In the title complex, [Zn(C7H11NO2)2](C7H4NO3S)2, the ZnII ion lies on a crystallographic inversion centre and possesses an octahedral geometry with two neutral 2-pyridylethanol (pyet) ligands and two coordinated water molecules. Pyet acts as an N,O-bidentate ligand, giving rise to a six-membered chelate ring. H atoms of the water molecules and the hydroxy group of pyet are involved in hydrogen bonding with amine-N, sulfonyl-O and carbonyl-O atoms of neighbouring saccharinate ions, creating a three-dimensional network.
Supporting information
CCDC reference: 189877
Key indicators
- Single-crystal X-ray study
- T = 133 K
- Mean (C-C) = 0.002 Å
- R factor = 0.024
- wR factor = 0.069
- Data-to-parameter ratio = 19.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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-(2-pyridyl)ethanol-
κ2N,
O]zinc(II)
disaccharinate
top
Crystal data top
[Zn(C7H11NO2)2](C7H4NO3S)2 | F(000) = 736 |
Mr = 712.05 | Dx = 1.623 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.8270 (6) Å | Cell parameters from 6687 reflections |
b = 8.7748 (6) Å | θ = 2.4–30.5° |
c = 19.1473 (10) Å | µ = 1.05 mm−1 |
β = 100.833 (3)° | T = 133 K |
V = 1456.63 (16) Å3 | Prism, colourless |
Z = 2 | 0.50 × 0.40 × 0.35 mm |
Data collection top
Bruker SMART 1000CCD diffractometer | 4267 independent reflections |
Radiation source: fine-focus sealed tube | 3997 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
Detector resolution: 8.192 pixels mm-1 | θmax = 30.0°, θmin = 2.2° |
ω and φ scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | k = −12→12 |
Tmin = 0.583, Tmax = 0.692 | l = −26→26 |
28712 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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.069 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0439P)2 + 0.4412P] where P = (Fo2 + 2Fc2)/3 |
4267 reflections | (Δ/σ)max = 0.001 |
217 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
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 | |
C11 | 0.34348 (13) | 0.00586 (12) | 0.31505 (6) | 0.0183 (2) | |
H11 | 0.2649 | −0.0346 | 0.2791 | 0.022* | |
C12 | 0.36602 (14) | 0.16249 (13) | 0.32376 (6) | 0.0212 (2) | |
H12 | 0.3011 | 0.2304 | 0.2931 | 0.025* | |
C13 | 0.48155 (14) | 0.22178 (13) | 0.37644 (7) | 0.0224 (2) | |
H13 | 0.4940 | 0.3290 | 0.3811 | 0.027* | |
C14 | 0.57929 (13) | 0.12521 (13) | 0.42247 (6) | 0.0204 (2) | |
H14 | 0.6588 | 0.1651 | 0.4582 | 0.025* | |
C15 | 0.55653 (12) | −0.03076 (12) | 0.41431 (6) | 0.01605 (19) | |
C16 | 0.44128 (12) | −0.08798 (12) | 0.36140 (5) | 0.01508 (18) | |
C21 | 0.64332 (12) | −0.15702 (12) | 0.45727 (5) | 0.01621 (19) | |
O21 | 0.74972 (9) | −0.13168 (10) | 0.50833 (4) | 0.02115 (16) | |
N1 | 0.59298 (11) | −0.29720 (10) | 0.43442 (5) | 0.01810 (18) | |
S1 | 0.45256 (3) | −0.28843 (3) | 0.367118 (13) | 0.01531 (6) | |
O1 | 0.49442 (11) | −0.35141 (10) | 0.30374 (4) | 0.02411 (17) | |
O2 | 0.31301 (10) | −0.35246 (10) | 0.38457 (5) | 0.02345 (17) | |
Zn1 | 0.5000 | 0.0000 | 0.0000 | 0.01274 (6) | |
O4 | 0.74133 (9) | −0.05092 (9) | 0.01568 (4) | 0.01741 (15) | |
H41 | 0.770 (2) | −0.080 (2) | −0.0212 (10) | 0.034 (4)* | |
H42 | 0.795 (2) | 0.026 (2) | 0.0283 (10) | 0.033 (5)* | |
N2 | 0.52929 (10) | 0.15812 (10) | 0.08444 (4) | 0.01406 (16) | |
C31 | 0.48669 (12) | 0.30354 (12) | 0.06918 (6) | 0.01687 (19) | |
H31 | 0.4457 | 0.3294 | 0.0212 | 0.020* | |
C32 | 0.49984 (13) | 0.41704 (13) | 0.12018 (6) | 0.0213 (2) | |
H32 | 0.4679 | 0.5183 | 0.1075 | 0.026* | |
C33 | 0.56068 (14) | 0.37954 (14) | 0.19011 (6) | 0.0228 (2) | |
H33 | 0.5731 | 0.4552 | 0.2262 | 0.027* | |
C34 | 0.60302 (13) | 0.22987 (13) | 0.20644 (6) | 0.0197 (2) | |
H34 | 0.6450 | 0.2021 | 0.2541 | 0.024* | |
C35 | 0.58406 (12) | 0.12024 (12) | 0.15302 (5) | 0.01534 (18) | |
C36 | 0.61561 (13) | −0.04526 (13) | 0.17048 (6) | 0.01827 (19) | |
H36A | 0.6485 | −0.0563 | 0.2226 | 0.022* | |
H36B | 0.7017 | −0.0800 | 0.1479 | 0.022* | |
C37 | 0.47581 (13) | −0.14697 (13) | 0.14553 (5) | 0.0189 (2) | |
H37A | 0.4878 | −0.2442 | 0.1722 | 0.023* | |
H37B | 0.3811 | −0.0959 | 0.1543 | 0.023* | |
O3 | 0.46346 (10) | −0.17624 (9) | 0.07100 (4) | 0.01736 (15) | |
H3 | 0.385 (2) | −0.230 (2) | 0.0552 (10) | 0.039 (5)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C11 | 0.0159 (5) | 0.0212 (5) | 0.0172 (5) | 0.0021 (4) | 0.0019 (4) | 0.0023 (3) |
C12 | 0.0207 (5) | 0.0204 (5) | 0.0226 (5) | 0.0049 (4) | 0.0044 (4) | 0.0054 (4) |
C13 | 0.0236 (5) | 0.0153 (5) | 0.0285 (6) | 0.0009 (4) | 0.0056 (4) | 0.0008 (4) |
C14 | 0.0190 (5) | 0.0178 (5) | 0.0237 (5) | 0.0005 (4) | 0.0021 (4) | −0.0016 (4) |
C15 | 0.0141 (4) | 0.0167 (4) | 0.0174 (5) | 0.0019 (4) | 0.0030 (4) | 0.0005 (4) |
C16 | 0.0142 (4) | 0.0155 (4) | 0.0159 (4) | 0.0013 (3) | 0.0035 (3) | 0.0010 (3) |
C21 | 0.0142 (4) | 0.0187 (5) | 0.0157 (4) | 0.0037 (4) | 0.0028 (3) | 0.0001 (4) |
O21 | 0.0178 (4) | 0.0244 (4) | 0.0191 (4) | 0.0042 (3) | −0.0021 (3) | −0.0014 (3) |
N1 | 0.0174 (4) | 0.0168 (4) | 0.0186 (4) | 0.0035 (3) | −0.0003 (3) | 0.0018 (3) |
S1 | 0.01516 (12) | 0.01458 (12) | 0.01589 (12) | 0.00073 (8) | 0.00212 (9) | 0.00030 (8) |
O1 | 0.0291 (4) | 0.0235 (4) | 0.0199 (4) | 0.0035 (3) | 0.0048 (3) | −0.0051 (3) |
O2 | 0.0189 (4) | 0.0238 (4) | 0.0275 (4) | −0.0038 (3) | 0.0037 (3) | 0.0053 (3) |
Zn1 | 0.01377 (9) | 0.01217 (9) | 0.01185 (9) | −0.00024 (5) | 0.00127 (6) | −0.00088 (5) |
O4 | 0.0151 (3) | 0.0166 (4) | 0.0200 (4) | −0.0010 (3) | 0.0020 (3) | −0.0029 (3) |
N2 | 0.0127 (4) | 0.0150 (4) | 0.0142 (4) | −0.0005 (3) | 0.0017 (3) | −0.0015 (3) |
C31 | 0.0154 (4) | 0.0161 (4) | 0.0187 (5) | 0.0004 (3) | 0.0020 (4) | −0.0016 (4) |
C32 | 0.0212 (5) | 0.0169 (5) | 0.0253 (5) | 0.0021 (4) | 0.0026 (4) | −0.0051 (4) |
C33 | 0.0221 (5) | 0.0222 (5) | 0.0232 (5) | 0.0007 (4) | 0.0017 (4) | −0.0097 (4) |
C34 | 0.0184 (5) | 0.0244 (5) | 0.0153 (5) | 0.0004 (4) | 0.0009 (4) | −0.0049 (4) |
C35 | 0.0125 (4) | 0.0181 (4) | 0.0149 (4) | −0.0007 (3) | 0.0014 (3) | −0.0018 (3) |
C36 | 0.0197 (5) | 0.0187 (5) | 0.0147 (4) | 0.0012 (4) | −0.0012 (4) | −0.0001 (4) |
C37 | 0.0244 (5) | 0.0182 (5) | 0.0143 (4) | −0.0034 (4) | 0.0037 (4) | 0.0009 (4) |
O3 | 0.0200 (4) | 0.0173 (3) | 0.0139 (3) | −0.0044 (3) | 0.0011 (3) | −0.0002 (3) |
Geometric parameters (Å, º) top
C11—C16 | 1.3867 (14) | C33—C34 | 1.3851 (17) |
C11—C12 | 1.3943 (15) | C34—C35 | 1.3911 (14) |
C12—C13 | 1.3934 (17) | C35—C36 | 1.5044 (15) |
C13—C14 | 1.3976 (16) | C36—C37 | 1.5251 (15) |
C14—C15 | 1.3878 (15) | C37—O3 | 1.4338 (12) |
C15—C16 | 1.3878 (14) | C11—H11 | 0.9500 |
C15—C21 | 1.5014 (14) | C12—H12 | 0.9500 |
C16—S1 | 1.7639 (11) | C13—H13 | 0.9500 |
C21—O21 | 1.2418 (13) | C14—H14 | 0.9500 |
C21—N1 | 1.3524 (14) | O4—H41 | 0.835 (19) |
N1—S1 | 1.6133 (9) | O4—H42 | 0.83 (2) |
S1—O1 | 1.4434 (8) | C31—H31 | 0.9500 |
S1—O2 | 1.4490 (9) | C32—H32 | 0.9500 |
Zn1—N2 | 2.1093 (9) | C33—H33 | 0.9500 |
Zn1—O3 | 2.1233 (8) | C34—H34 | 0.9500 |
Zn1—O4 | 2.1417 (8) | C36—H36A | 0.9900 |
N2—C31 | 1.3468 (13) | C36—H36B | 0.9900 |
N2—C35 | 1.3527 (13) | C37—H37A | 0.9900 |
C31—C32 | 1.3843 (15) | C37—H37B | 0.9900 |
C32—C33 | 1.3854 (17) | O3—H3 | 0.84 (2) |
| | | |
C16—C11—C12 | 116.81 (10) | C34—C33—C32 | 118.85 (10) |
C13—C12—C11 | 121.55 (10) | C33—C34—C35 | 119.97 (10) |
C12—C13—C14 | 120.75 (11) | N2—C35—C34 | 121.03 (10) |
C15—C14—C13 | 117.89 (10) | N2—C35—C36 | 118.05 (9) |
C16—C15—C14 | 120.65 (10) | C34—C35—C36 | 120.83 (9) |
C16—C15—C21 | 111.20 (9) | C35—C36—C37 | 112.97 (9) |
C14—C15—C21 | 128.16 (10) | O3—C37—C36 | 108.80 (9) |
C11—C16—C15 | 122.35 (10) | C37—O3—Zn1 | 120.96 (6) |
C11—C16—S1 | 130.76 (8) | C16—C11—H11 | 121.6 |
C15—C16—S1 | 106.88 (7) | C12—C11—H11 | 121.6 |
O21—C21—N1 | 124.85 (10) | C13—C12—H12 | 119.2 |
O21—C21—C15 | 122.13 (10) | C11—C12—H12 | 119.2 |
N1—C21—C15 | 113.02 (9) | C12—C13—H13 | 119.6 |
C21—N1—S1 | 111.80 (7) | C14—C13—H13 | 119.6 |
O1—S1—O2 | 114.11 (5) | C15—C14—H14 | 121.1 |
O1—S1—N1 | 111.95 (5) | C13—C14—H14 | 121.1 |
O2—S1—N1 | 110.86 (5) | Zn1—O4—H41 | 113.6 (12) |
O1—S1—C16 | 110.49 (5) | Zn1—O4—H42 | 111.8 (13) |
O2—S1—C16 | 111.13 (5) | H41—O4—H42 | 103.8 (18) |
N1—S1—C16 | 97.07 (5) | N2—C31—H31 | 118.5 |
N2i—Zn1—N2 | 180.00 (3) | C32—C31—H31 | 118.5 |
N2i—Zn1—O3 | 90.01 (3) | C31—C32—H32 | 120.8 |
N2—Zn1—O3 | 89.99 (3) | C33—C32—H32 | 120.8 |
N2i—Zn1—O3i | 89.99 (3) | C34—C33—H33 | 120.6 |
N2—Zn1—O3i | 90.01 (3) | C32—C33—H33 | 120.6 |
O3—Zn1—O3i | 180.00 (4) | C33—C34—H34 | 120.0 |
N2i—Zn1—O4 | 86.89 (3) | C35—C34—H34 | 120.0 |
N2—Zn1—O4 | 93.11 (3) | C35—C36—H36A | 109.0 |
O3—Zn1—O4 | 91.44 (3) | C37—C36—H36A | 109.0 |
O3i—Zn1—O4 | 88.56 (3) | C35—C36—H36B | 109.0 |
N2i—Zn1—O4i | 93.11 (3) | C37—C36—H36B | 109.0 |
N2—Zn1—O4i | 86.89 (3) | H36A—C36—H36B | 107.8 |
O3—Zn1—O4i | 88.56 (3) | O3—C37—H37A | 109.9 |
O3i—Zn1—O4i | 91.44 (3) | C36—C37—H37A | 109.9 |
O4—Zn1—O4i | 180.0 | O3—C37—H37B | 109.9 |
C31—N2—C35 | 118.54 (9) | C36—C37—H37B | 109.9 |
C31—N2—Zn1 | 117.90 (7) | H37A—C37—H37B | 108.3 |
C35—N2—Zn1 | 123.53 (7) | C37—O3—H3 | 111.1 (13) |
N2—C31—C32 | 123.06 (10) | Zn1—O3—H3 | 112.8 (13) |
C31—C32—C33 | 118.48 (10) | | |
| | | |
C16—C11—C12—C13 | 0.14 (18) | O3i—Zn1—N2—C31 | 30.78 (8) |
C11—C12—C13—C14 | 0.08 (19) | O4—Zn1—N2—C31 | 119.34 (8) |
C12—C13—C14—C15 | −0.53 (18) | O4i—Zn1—N2—C31 | −60.66 (8) |
C13—C14—C15—C16 | 0.77 (17) | O3—Zn1—N2—C35 | 28.76 (8) |
C13—C14—C15—C21 | −178.92 (11) | O3i—Zn1—N2—C35 | −151.24 (8) |
C12—C11—C16—C15 | 0.10 (17) | O4—Zn1—N2—C35 | −62.68 (8) |
C12—C11—C16—S1 | −178.91 (9) | O4i—Zn1—N2—C35 | 117.32 (8) |
C14—C15—C16—C11 | −0.57 (17) | C35—N2—C31—C32 | 1.63 (16) |
C21—C15—C16—C11 | 179.16 (10) | Zn1—N2—C31—C32 | 179.71 (8) |
C14—C15—C16—S1 | 178.65 (9) | N2—C31—C32—C33 | 0.48 (17) |
C21—C15—C16—S1 | −1.62 (11) | C31—C32—C33—C34 | −1.25 (17) |
C16—C15—C21—O21 | −178.64 (10) | C32—C33—C34—C35 | −0.03 (17) |
C14—C15—C21—O21 | 1.07 (18) | C31—N2—C35—C34 | −2.95 (15) |
C16—C15—C21—N1 | 1.25 (13) | Zn1—N2—C35—C34 | 179.09 (8) |
C14—C15—C21—N1 | −179.04 (11) | C31—N2—C35—C36 | 173.72 (9) |
O21—C21—N1—S1 | 179.72 (9) | Zn1—N2—C35—C36 | −4.25 (13) |
C15—C21—N1—S1 | −0.17 (12) | C33—C34—C35—N2 | 2.19 (17) |
C21—N1—S1—O1 | 114.78 (8) | C33—C34—C35—C36 | −174.38 (10) |
C21—N1—S1—O2 | −116.55 (8) | N2—C35—C36—C37 | −55.15 (13) |
C21—N1—S1—C16 | −0.70 (9) | C34—C35—C36—C37 | 121.52 (11) |
C11—C16—S1—O1 | 63.88 (12) | C35—C36—C37—O3 | 80.07 (11) |
C15—C16—S1—O1 | −115.25 (8) | C36—C37—O3—Zn1 | −42.05 (11) |
C11—C16—S1—O2 | −63.84 (12) | N2i—Zn1—O3—C37 | 176.71 (8) |
C15—C16—S1—O2 | 117.03 (8) | N2—Zn1—O3—C37 | −3.29 (8) |
C11—C16—S1—N1 | −179.48 (11) | O4—Zn1—O3—C37 | 89.82 (8) |
C15—C16—S1—N1 | 1.39 (8) | O4i—Zn1—O3—C37 | −90.18 (8) |
O3—Zn1—N2—C31 | −149.22 (8) | | |
Symmetry code: (i) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H41···O2ii | 0.835 (19) | 2.002 (19) | 2.8317 (12) | 173 (2) |
O4—H42···N1iii | 0.83 (2) | 1.90 (2) | 2.7355 (12) | 174 (2) |
O3—H3···O21iv | 0.84 (2) | 1.82 (2) | 2.6437 (11) | 165 (2) |
Symmetry codes: (ii) x+1/2, −y−1/2, z−1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y−1/2, z−1/2. |