Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807041487/im2029sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807041487/im2029Isup2.hkl |
CCDC reference: 660175
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.004 Å
- R factor = 0.028
- wR factor = 0.056
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O2 .. 10.98 su
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT230_ALERT_2_C Hirshfeld Test Diff for S1 - C10 .. 5.05 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O3 .. 5.54 su PLAT390_ALERT_3_C Deviating Methyl C9 X-C-H Bond Angle ...... 102.00 Deg.
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1 (2) 2.09
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related literature, see: Carcelli et al. (1999); Chen, Zhou, Liang et al. (2004); Chen, Zhou, Li et al. (2004); Kaur et al. (2002); Zhong et al. (2007); Zhou et al. (2004).
H-Pysc (1.0 mmol) and Cd(Ac)2 × 4H2O (0.5 mmol) were dissolved in a water-ethanol mixture (1:1 v/v; 16 ml) at 353 K. After stirring for ca 2 hrs, 10 ml of a solution containing 1.0 mmol (NH4)SCN was added, then the mixture was further stirred for another 2 hrs. The resulting solution was filtered and the filtrate allowed to standing at room temperature. Well shaped colorless crystals suitable for X-rays diffraction were obtained in 58% yield after two weeks.
Hydrogen atoms bound to carbon atoms and nitrogen atoms were positioned geometrically and refined using a riding model, with C—H = 0.93 Å, N—H = 0.86 Å, and Uiso(H) = 1.2Ueq(C or N). Water Hydrogen atoms were located in difference maps and constrained to ride at the as-found O—H distances (0.89 Å), with Uiso(H) = 1.5Ueq(O).
Crystal structures and properties of metal complexes based on pyridine-2-carbaldehyde semicarbazone (H-Pysc), owing to their antimicrobial, cytotoxic and antioxidant activities, have been reported in numerous papers (Zhou et al., 2004; Kaur et al., 2002; Carcelli et al., 1999; Zhong et al., 2007) in last several years. Herein, we report the synthesis and crystal structure of the title compound, (I).
Compound (I) is composed of one [Cd(HPysc)(SCN)(Ac)(H2O)] unit and one lattice water. The Cd atom in compound (I) is seven-coordinated (Fig. 1) by one S atom (from thiocyanate), two N atoms (from H-Pysc ligand) and four O atoms (one from the coordinated water molecule, one from H-Pysc ligand, and two from the acetate anion), forming a slightly distorted pentagonal bipyramidal geometry (Table 1). S1 and O1W occupy the apical positions of the coordination polyhedron. Similar to the corresponding nickel(II) complex (Zhou et al., 2004), the H-Pysc ligand is planar and utilizes its pyridyl N atom, amide O atom and imine N atom for metal coordination. This is in contrast to the highly related ligand pyridine-3-carbaldehyde-semicarbazone in it's cobalt(II) (Chen, Zhou, Liang et al., 2004) and nickel(II) (Chen, Zhou, Li et al., 2004) complexes, in which only the pyridyl N atoms bind to the metal ions. The acetate anion acts as a bidentate chelating ligand leading to two short C—O distances (O(2)—C(8) 1.261 (3) Å, O(3)—C(8) 1.260 (3) Å).
The molecules are connected by intermolecular hydrogen bonding interactions and π - π stacking interactions to form a three-dimensional supramolecular network. The coordinated water molecules (O1W) act as hydrogen bond donor sites towards the thiocyanate S1 atoms and acetate O3 atoms to form O—H···Si and O—H···Oii hydrogen bonds, respectively [symmetry codes i=x, 1/2 - y, 1/2 + z; ii = 1 - x, -y, 1 - z]. The uncoordinated water molecules (O2W) also act as a H atom donors, the accepters being the thiocyanate N5 atoms and acetate O2 atoms, respectively, forming O—H···Niii and O—H···Oi hydrogen bonds [symmetry codes iii=x, 3/2 - y, 1/2 + z]. In addition, the O1W atoms and semicarbazone O1 atoms accept H atoms from N4 to form N—H···Ov and N—H···Oiv hydrogen bonds [symmetry codes iv = 1 - x, 1 - y, 1 - z; v = x, 1 + y, z] (Table 2, Fig. 2).
For related literature, see: Carcelli et al. (1999); Chen, Zhou, Liang et al. (2004); Chen, Zhou, Li et al. (2004); Kaur et al. (2002); Zhong et al. (2007); Zhou et al. (2004).
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
[Cd(C2H3O2)(NCS)(C7H8N4O)(H2O)]·H2O | Z = 4 |
Mr = 429.73 | F(000) = 856 |
Monoclinic, P21/c | Dx = 1.814 Mg m−3 |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 14.767 (1) Å | θ = 2.8–28.4° |
b = 7.7345 (7) Å | µ = 1.55 mm−1 |
c = 13.964 (1) Å | T = 173 K |
β = 99.340 (1)° | Block, colourless |
V = 1573.7 (3) Å3 | 0.35 × 0.28 × 0.22 mm |
Bruker SMART APEXII CCD diffractometer | 3919 independent reflections |
Radiation source: fine-focus sealed tube | 2921 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.072 |
ω scans | θmax = 28.4°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −19→19 |
Tmin = 0.601, Tmax = 0.718 | k = −9→10 |
14208 measured reflections | l = −18→18 |
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) = 0.056 | H-atom parameters constrained |
S = 0.93 | w = 1/[σ2(Fo2) + (0.0183P)2] where P = (Fo2 + 2Fc2)/3 |
3919 reflections | (Δ/σ)max = 0.001 |
199 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.63 e Å−3 |
[Cd(C2H3O2)(NCS)(C7H8N4O)(H2O)]·H2O | V = 1573.7 (3) Å3 |
Mr = 429.73 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.767 (1) Å | µ = 1.55 mm−1 |
b = 7.7345 (7) Å | T = 173 K |
c = 13.964 (1) Å | 0.35 × 0.28 × 0.22 mm |
β = 99.340 (1)° |
Bruker SMART APEXII CCD diffractometer | 3919 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2921 reflections with I > 2σ(I) |
Tmin = 0.601, Tmax = 0.718 | Rint = 0.072 |
14208 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.056 | H-atom parameters constrained |
S = 0.93 | Δρmax = 0.48 e Å−3 |
3919 reflections | Δρmin = −0.63 e Å−3 |
199 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 | ||
Cd1 | 0.688818 (11) | 0.12412 (2) | 0.472629 (12) | 0.02909 (6) | |
S1 | 0.72697 (6) | 0.26945 (11) | 0.30933 (5) | 0.0539 (2) | |
O1 | 0.59934 (11) | 0.3712 (2) | 0.50308 (13) | 0.0371 (4) | |
N1 | 0.83695 (13) | 0.0190 (3) | 0.54372 (14) | 0.0336 (5) | |
O3 | 0.54727 (11) | −0.0111 (2) | 0.39860 (11) | 0.0369 (4) | |
O1W | 0.63610 (11) | 0.0075 (2) | 0.61140 (11) | 0.0330 (4) | |
O2 | 0.67697 (12) | −0.1351 (2) | 0.38194 (14) | 0.0451 (5) | |
C8 | 0.59050 (17) | −0.1326 (3) | 0.36624 (17) | 0.0331 (5) | |
N3 | 0.73204 (13) | 0.4873 (3) | 0.58458 (14) | 0.0341 (5) | |
H3A | 0.7617 | 0.5745 | 0.6121 | 0.041* | |
N2 | 0.77331 (13) | 0.3339 (3) | 0.57216 (14) | 0.0303 (5) | |
N4 | 0.59726 (15) | 0.6374 (3) | 0.56943 (16) | 0.0416 (5) | |
H4A | 0.5394 | 0.6496 | 0.5494 | 0.050* | |
H4B | 0.6278 | 0.7186 | 0.6021 | 0.050* | |
C7 | 0.63933 (17) | 0.4936 (3) | 0.54996 (17) | 0.0313 (5) | |
C6 | 0.85542 (17) | 0.3042 (3) | 0.61182 (18) | 0.0359 (6) | |
H6 | 0.8905 | 0.3889 | 0.6477 | 0.043* | |
C1 | 0.86846 (18) | −0.1400 (4) | 0.5326 (2) | 0.0422 (7) | |
H1 | 0.8304 | −0.2183 | 0.4948 | 0.051* | |
C5 | 0.89292 (16) | 0.1320 (3) | 0.59916 (17) | 0.0347 (6) | |
N5 | 0.8725 (2) | 0.5003 (4) | 0.3657 (2) | 0.0673 (8) | |
C9 | 0.5393 (2) | −0.2757 (4) | 0.3088 (2) | 0.0486 (7) | |
C2 | 0.95532 (19) | −0.1941 (4) | 0.5746 (2) | 0.0495 (8) | |
H2 | 0.9748 | −0.3064 | 0.5657 | 0.059* | |
C4 | 0.98095 (18) | 0.0857 (4) | 0.6424 (2) | 0.0468 (7) | |
H4 | 1.0185 | 0.1654 | 0.6797 | 0.056* | |
C10 | 0.8116 (2) | 0.4066 (4) | 0.3455 (2) | 0.0478 (7) | |
C3 | 1.0120 (2) | −0.0781 (4) | 0.6296 (2) | 0.0521 (8) | |
H3 | 1.0709 | −0.1105 | 0.6580 | 0.062* | |
O2W | 0.79164 (14) | 0.6935 (3) | 0.74484 (15) | 0.0604 (6) | |
H9C | 0.4875 | −0.3189 | 0.3348 | 0.091* | |
H9B | 0.5195 | −0.2523 | 0.2396 | 0.091* | |
H9A | 0.5857 | −0.3653 | 0.3135 | 0.091* | |
H2B | 0.7535 | 0.6609 | 0.7848 | 0.091* | |
H1B | 0.5745 | 0.0123 | 0.6070 | 0.091* | |
H1A | 0.6617 | 0.0540 | 0.6679 | 0.091* | |
H2A | 0.8207 | 0.7926 | 0.7617 | 0.091* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02724 (9) | 0.02820 (10) | 0.03121 (10) | 0.00117 (8) | 0.00290 (6) | −0.00288 (8) |
S1 | 0.0649 (5) | 0.0621 (5) | 0.0335 (4) | −0.0032 (4) | 0.0041 (3) | 0.0104 (4) |
O1 | 0.0324 (9) | 0.0285 (9) | 0.0484 (11) | 0.0034 (8) | 0.0007 (8) | −0.0104 (9) |
N1 | 0.0293 (11) | 0.0400 (13) | 0.0316 (12) | 0.0045 (10) | 0.0054 (9) | 0.0037 (10) |
O3 | 0.0344 (10) | 0.0398 (11) | 0.0361 (10) | −0.0003 (8) | 0.0043 (8) | −0.0082 (8) |
O1W | 0.0320 (9) | 0.0350 (10) | 0.0318 (9) | −0.0012 (8) | 0.0047 (7) | −0.0025 (8) |
O2 | 0.0356 (10) | 0.0459 (12) | 0.0537 (12) | −0.0028 (9) | 0.0068 (8) | −0.0107 (10) |
C8 | 0.0378 (13) | 0.0347 (14) | 0.0269 (12) | −0.0052 (12) | 0.0058 (10) | 0.0005 (12) |
N3 | 0.0334 (11) | 0.0265 (12) | 0.0410 (13) | −0.0023 (9) | 0.0020 (9) | −0.0086 (9) |
N2 | 0.0315 (11) | 0.0307 (12) | 0.0292 (11) | 0.0011 (9) | 0.0065 (9) | −0.0010 (9) |
N4 | 0.0398 (12) | 0.0303 (12) | 0.0532 (14) | 0.0053 (10) | 0.0030 (10) | −0.0113 (11) |
C7 | 0.0357 (13) | 0.0293 (14) | 0.0291 (13) | 0.0011 (11) | 0.0056 (10) | 0.0021 (11) |
C6 | 0.0330 (13) | 0.0428 (16) | 0.0304 (14) | −0.0021 (12) | 0.0007 (11) | −0.0068 (12) |
C1 | 0.0393 (14) | 0.0395 (17) | 0.0490 (17) | 0.0081 (13) | 0.0108 (12) | 0.0035 (13) |
C5 | 0.0289 (12) | 0.0450 (16) | 0.0304 (13) | 0.0022 (12) | 0.0054 (10) | 0.0037 (12) |
N5 | 0.0597 (17) | 0.0463 (17) | 0.096 (2) | 0.0005 (15) | 0.0134 (16) | 0.0116 (16) |
C9 | 0.0502 (17) | 0.0477 (18) | 0.0483 (18) | −0.0103 (15) | 0.0092 (14) | −0.0194 (14) |
C2 | 0.0474 (17) | 0.0512 (18) | 0.0519 (18) | 0.0213 (15) | 0.0141 (15) | 0.0142 (15) |
C4 | 0.0337 (14) | 0.067 (2) | 0.0368 (16) | 0.0091 (14) | −0.0014 (12) | 0.0015 (14) |
C10 | 0.0564 (19) | 0.0404 (18) | 0.0489 (18) | 0.0171 (15) | 0.0150 (15) | 0.0139 (14) |
C3 | 0.0358 (15) | 0.074 (2) | 0.0447 (17) | 0.0203 (15) | 0.0013 (13) | 0.0126 (16) |
O2W | 0.0694 (14) | 0.0664 (15) | 0.0482 (12) | −0.0270 (12) | 0.0179 (11) | −0.0203 (11) |
Cd1—N2 | 2.357 (2) | N2—C6 | 1.269 (3) |
Cd1—O2 | 2.3629 (18) | N4—C7 | 1.323 (3) |
Cd1—O1W | 2.3800 (15) | N4—H4A | 0.8600 |
Cd1—N1 | 2.393 (2) | N4—H4B | 0.8600 |
Cd1—O1 | 2.4000 (16) | C6—C5 | 1.464 (4) |
Cd1—O3 | 2.4146 (16) | C6—H6 | 0.9300 |
Cd1—S1 | 2.6829 (8) | C1—C2 | 1.386 (4) |
Cd1—C8 | 2.749 (3) | C1—H1 | 0.9300 |
S1—C10 | 1.655 (4) | C5—C4 | 1.388 (4) |
O1—C7 | 1.244 (3) | N5—C10 | 1.154 (4) |
N1—C1 | 1.332 (3) | C9—H9C | 0.9582 |
N1—C5 | 1.356 (3) | C9—H9B | 0.9803 |
O3—C8 | 1.260 (3) | C9—H9A | 0.9695 |
O1W—H1B | 0.9021 | C2—C3 | 1.374 (4) |
O1W—H1A | 0.8926 | C2—H2 | 0.9300 |
O2—C8 | 1.260 (3) | C4—C3 | 1.369 (4) |
C8—C9 | 1.497 (4) | C4—H4 | 0.9300 |
N3—N2 | 1.358 (3) | C3—H3 | 0.9300 |
N3—C7 | 1.377 (3) | O2W—H2B | 0.8910 |
N3—H3A | 0.8600 | O2W—H2A | 0.8910 |
N2—Cd1—O2 | 152.38 (7) | O2—C8—Cd1 | 59.06 (13) |
N2—Cd1—O1W | 89.57 (6) | O3—C8—Cd1 | 61.41 (12) |
O2—Cd1—O1W | 96.27 (6) | C9—C8—Cd1 | 178.4 (2) |
N2—Cd1—N1 | 68.20 (7) | N2—N3—C7 | 115.3 (2) |
O2—Cd1—N1 | 85.24 (7) | N2—N3—H3A | 122.4 |
O1W—Cd1—N1 | 86.06 (6) | C7—N3—H3A | 122.4 |
N2—Cd1—O1 | 66.52 (6) | C6—N2—N3 | 121.3 (2) |
O2—Cd1—O1 | 140.86 (6) | C6—N2—Cd1 | 120.63 (17) |
O1W—Cd1—O1 | 83.98 (6) | N3—N2—Cd1 | 118.12 (14) |
N1—Cd1—O1 | 133.60 (7) | C7—N4—H4A | 120.0 |
N2—Cd1—O3 | 152.75 (6) | C7—N4—H4B | 120.0 |
O2—Cd1—O3 | 54.50 (6) | H4A—N4—H4B | 120.0 |
O1W—Cd1—O3 | 79.02 (5) | O1—C7—N4 | 123.3 (2) |
N1—Cd1—O3 | 134.41 (7) | O1—C7—N3 | 121.2 (2) |
O1—Cd1—O3 | 87.56 (6) | N4—C7—N3 | 115.5 (2) |
N2—Cd1—S1 | 92.79 (5) | N2—C6—C5 | 117.7 (2) |
O2—Cd1—S1 | 84.69 (5) | N2—C6—H6 | 121.1 |
O1W—Cd1—S1 | 172.92 (4) | C5—C6—H6 | 121.1 |
N1—Cd1—S1 | 101.01 (5) | N1—C1—C2 | 123.1 (3) |
O1—Cd1—S1 | 90.84 (5) | N1—C1—H1 | 118.5 |
O3—Cd1—S1 | 95.98 (4) | C2—C1—H1 | 118.5 |
N2—Cd1—C8 | 176.58 (7) | N1—C5—C4 | 121.5 (3) |
O2—Cd1—C8 | 27.22 (7) | N1—C5—C6 | 116.6 (2) |
O1W—Cd1—C8 | 87.27 (6) | C4—C5—C6 | 121.9 (3) |
N1—Cd1—C8 | 110.22 (8) | C8—C9—H9C | 114.8 |
O1—Cd1—C8 | 114.40 (7) | C8—C9—H9B | 115.8 |
O3—Cd1—C8 | 27.28 (6) | H9C—C9—H9B | 108.0 |
S1—Cd1—C8 | 90.50 (5) | C8—C9—H9A | 101.7 |
C10—S1—Cd1 | 105.18 (10) | H9C—C9—H9A | 108.9 |
C7—O1—Cd1 | 118.10 (15) | H9B—C9—H9A | 107.1 |
C1—N1—C5 | 118.0 (2) | C3—C2—C1 | 118.5 (3) |
C1—N1—Cd1 | 125.32 (18) | C3—C2—H2 | 120.7 |
C5—N1—Cd1 | 116.69 (16) | C1—C2—H2 | 120.7 |
C8—O3—Cd1 | 91.31 (14) | C3—C4—C5 | 119.5 (3) |
Cd1—O1W—H1B | 112.9 | C3—C4—H4 | 120.3 |
Cd1—O1W—H1A | 114.8 | C5—C4—H4 | 120.3 |
H1B—O1W—H1A | 108.8 | N5—C10—S1 | 176.0 (3) |
C8—O2—Cd1 | 93.72 (15) | C4—C3—C2 | 119.4 (3) |
O2—C8—O3 | 120.5 (2) | C4—C3—H3 | 120.3 |
O2—C8—C9 | 119.4 (2) | C2—C3—H3 | 120.3 |
O3—C8—C9 | 120.1 (2) | H2B—O2W—H2A | 113.8 |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···S1i | 0.89 | 2.46 | 3.348 (2) | 170 |
O1W—H1B···O3ii | 0.90 | 1.79 | 2.689 (2) | 177 |
O2W—H2A···N5iii | 0.89 | 2.21 | 3.038 (4) | 154 |
O2W—H2B···O2i | 0.89 | 1.91 | 2.791 (3) | 169 |
N3—H3A···O2W | 0.86 | 2.05 | 2.773 (3) | 141 |
N4—H4A···O1iv | 0.86 | 2.07 | 2.916 (3) | 169 |
N4—H4B···O1Wv | 0.86 | 2.24 | 2.959 (3) | 141 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, −y, −z+1; (iii) x, −y+3/2, z+1/2; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C2H3O2)(NCS)(C7H8N4O)(H2O)]·H2O |
Mr | 429.73 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 173 |
a, b, c (Å) | 14.767 (1), 7.7345 (7), 13.964 (1) |
β (°) | 99.340 (1) |
V (Å3) | 1573.7 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.55 |
Crystal size (mm) | 0.35 × 0.28 × 0.22 |
Data collection | |
Diffractometer | Bruker SMART APEXII CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.601, 0.718 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14208, 3919, 2921 |
Rint | 0.072 |
(sin θ/λ)max (Å−1) | 0.668 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.056, 0.93 |
No. of reflections | 3919 |
No. of parameters | 199 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.48, −0.63 |
Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···S1i | 0.89 | 2.46 | 3.348 (2) | 170 |
O1W—H1B···O3ii | 0.90 | 1.79 | 2.689 (2) | 177 |
O2W—H2A···N5iii | 0.89 | 2.21 | 3.038 (4) | 154 |
O2W—H2B···O2i | 0.89 | 1.91 | 2.791 (3) | 169 |
N3—H3A···O2W | 0.86 | 2.05 | 2.773 (3) | 141 |
N4—H4A···O1iv | 0.86 | 2.07 | 2.916 (3) | 169 |
N4—H4B···O1Wv | 0.86 | 2.24 | 2.959 (3) | 141 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, −y, −z+1; (iii) x, −y+3/2, z+1/2; (iv) −x+1, −y+1, −z+1; (v) x, y+1, z. |
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Crystal structures and properties of metal complexes based on pyridine-2-carbaldehyde semicarbazone (H-Pysc), owing to their antimicrobial, cytotoxic and antioxidant activities, have been reported in numerous papers (Zhou et al., 2004; Kaur et al., 2002; Carcelli et al., 1999; Zhong et al., 2007) in last several years. Herein, we report the synthesis and crystal structure of the title compound, (I).
Compound (I) is composed of one [Cd(HPysc)(SCN)(Ac)(H2O)] unit and one lattice water. The Cd atom in compound (I) is seven-coordinated (Fig. 1) by one S atom (from thiocyanate), two N atoms (from H-Pysc ligand) and four O atoms (one from the coordinated water molecule, one from H-Pysc ligand, and two from the acetate anion), forming a slightly distorted pentagonal bipyramidal geometry (Table 1). S1 and O1W occupy the apical positions of the coordination polyhedron. Similar to the corresponding nickel(II) complex (Zhou et al., 2004), the H-Pysc ligand is planar and utilizes its pyridyl N atom, amide O atom and imine N atom for metal coordination. This is in contrast to the highly related ligand pyridine-3-carbaldehyde-semicarbazone in it's cobalt(II) (Chen, Zhou, Liang et al., 2004) and nickel(II) (Chen, Zhou, Li et al., 2004) complexes, in which only the pyridyl N atoms bind to the metal ions. The acetate anion acts as a bidentate chelating ligand leading to two short C—O distances (O(2)—C(8) 1.261 (3) Å, O(3)—C(8) 1.260 (3) Å).
The molecules are connected by intermolecular hydrogen bonding interactions and π - π stacking interactions to form a three-dimensional supramolecular network. The coordinated water molecules (O1W) act as hydrogen bond donor sites towards the thiocyanate S1 atoms and acetate O3 atoms to form O—H···Si and O—H···Oii hydrogen bonds, respectively [symmetry codes i=x, 1/2 - y, 1/2 + z; ii = 1 - x, -y, 1 - z]. The uncoordinated water molecules (O2W) also act as a H atom donors, the accepters being the thiocyanate N5 atoms and acetate O2 atoms, respectively, forming O—H···Niii and O—H···Oi hydrogen bonds [symmetry codes iii=x, 3/2 - y, 1/2 + z]. In addition, the O1W atoms and semicarbazone O1 atoms accept H atoms from N4 to form N—H···Ov and N—H···Oiv hydrogen bonds [symmetry codes iv = 1 - x, 1 - y, 1 - z; v = x, 1 + y, z] (Table 2, Fig. 2).