



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810013802/pk2239sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536810013802/pk2239Isup2.hkl |
CCDC reference: 777873
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean
(C-C) = 0.005 Å
- R factor = 0.055
- wR factor = 0.103
- Data-to-parameter ratio = 16.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.01 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C24 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 9 PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT480_ALERT_4_C Long H...A H-Bond Reported H5 .. S2 .. 3.02 Ang. PLAT481_ALERT_4_C Long D...A H-Bond Reported O5 .. S2 .. 3.86 Ang. PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 2
Alert level G PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 11.67
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 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 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
0.1 mmol Co(CH3COO)2.3H2O, 0.2 mmol sulfadiazine, ethanol (2.2 ml), water (0.2 ml) and pyridine (0.2 ml) were placed in a Pyrex tube (ca 25 cm). The tube was frozen with liquid N2, evacuated under vacuum, sealed with a torch and heated at 353 K for three days to give red-brown block-shaped crystals, with a yield of 70%.
The water H were found in a difference Fourier map and refined freely. Other H atoms were treated as riding, with C—H distances of 0.95 Å,N—H distances of 0.88 Å, were refined as riding with Uiso(H) = 1.2Ueq(C,N).
The title compound consists of [Co(C11H11N4O4S2] and half a lattice water molecule and is isostructural with trans-[Ni(sdz)2(py)2] (where sdz = sulfadiazine anion and py = pyridine)(Wang et al., 2009), the title cobalt(II) complex has six-coordinate distorted octahedral geometry and contains two bidentate N-coordinated sulfadiazinate anion and two pyridine molecules occupying the trans sites. One water molecule lies on a 2-fold rotation axis. The coordination mode of sulfadiazine is similar to its cobalt(II) complex (Ajibade et al., 2006) and copper(II) complex (Brown et al., 1987), but different from Zn(sdz)2 (Yuan et al., 2001), polymeric Cd(II) complex (Wang et al. 2005), and its copper complex (Hossain et al. 2006). The Co—N bond distances involving the sulfonamide atoms N3, N7, the pyrimido atoms N1, N5, and the pyridine atoms N9, N10, are very similar, at 2.132 (2), 2.091 (2), 2.124 (2), 2.168 (2), 2.196 (2), 2.193 (2) Å, respectively. The tetrahedral coordination at S is distorted, as is also found in the neutral sulfadiazine molecule. A three dimensional network is generated by N—H···O and O—H···O hydrogen bonds involving the complex and water molecules.
For mono ligand sulfadiazine–metal complexes, see: Yuan et al. (2001); Wang et al. (2005). For mixed ligand sulfadiazine–metal complexes, see: Ajibade et al. (2006); Brown et al. (1987); Hossain et al. (2006); Wang et al. (2009).
Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear (Rigaku, 1999); data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[Co(C10H9N4O2S)2(C5H5N)2]·0.5H2O | F(000) = 2992 |
Mr = 724.68 | Dx = 1.534 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -C 2yc | Cell parameters from 11616 reflections |
a = 39.618 (4) Å | θ = 3.0–27.5° |
b = 11.2407 (9) Å | µ = 0.74 mm−1 |
c = 14.5673 (13) Å | T = 193 K |
β = 104.648 (2)° | Block, red-brown |
V = 6276.4 (10) Å3 | 0.44 × 0.15 × 0.12 mm |
Z = 8 |
Rigaku Mercury diffractometer | 7188 independent reflections |
Radiation source: fine-focus sealed tube | 6038 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 7.31 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −51→51 |
Absorption correction: multi-scan (REQAB; Jacobson, 1998) | k = −12→14 |
Tmin = 0.738, Tmax = 0.917 | l = −18→15 |
34520 measured reflections |
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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | w = 1/[σ2(Fo2) + (0.027P)2 + 11.6654P] where P = (Fo2 + 2Fc2)/3 |
7188 reflections | (Δ/σ)max = 0.001 |
434 parameters | Δρmax = 0.36 e Å−3 |
0 restraints | Δρmin = −0.52 e Å−3 |
[Co(C10H9N4O2S)2(C5H5N)2]·0.5H2O | V = 6276.4 (10) Å3 |
Mr = 724.68 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 39.618 (4) Å | µ = 0.74 mm−1 |
b = 11.2407 (9) Å | T = 193 K |
c = 14.5673 (13) Å | 0.44 × 0.15 × 0.12 mm |
β = 104.648 (2)° |
Rigaku Mercury diffractometer | 7188 independent reflections |
Absorption correction: multi-scan (REQAB; Jacobson, 1998) | 6038 reflections with I > 2σ(I) |
Tmin = 0.738, Tmax = 0.917 | Rint = 0.051 |
34520 measured reflections |
R[F2 > 2σ(F2)] = 0.055 | 0 restraints |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | w = 1/[σ2(Fo2) + (0.027P)2 + 11.6654P] where P = (Fo2 + 2Fc2)/3 |
7188 reflections | Δρmax = 0.36 e Å−3 |
434 parameters | Δρmin = −0.52 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 | ||
Co1 | 0.376102 (9) | 0.51879 (3) | 0.36763 (2) | 0.02249 (10) | |
S1 | 0.316541 (17) | 0.74751 (6) | 0.38330 (4) | 0.02182 (14) | |
S2 | 0.428760 (18) | 0.28343 (6) | 0.33767 (4) | 0.02344 (15) | |
O1 | 0.34287 (5) | 0.78002 (16) | 0.46799 (12) | 0.0283 (4) | |
O2 | 0.28292 (5) | 0.71697 (16) | 0.39809 (13) | 0.0278 (4) | |
O3 | 0.40112 (5) | 0.26443 (17) | 0.25308 (13) | 0.0339 (5) | |
O4 | 0.46383 (5) | 0.28960 (17) | 0.32502 (14) | 0.0327 (5) | |
O5 | 0.5000 | 0.1180 (3) | 0.2500 | 0.0491 (9) | |
N1 | 0.34102 (6) | 0.50839 (19) | 0.23097 (15) | 0.0232 (5) | |
N2 | 0.28923 (6) | 0.6275 (2) | 0.18964 (16) | 0.0284 (5) | |
N3 | 0.33361 (6) | 0.64112 (19) | 0.33688 (15) | 0.0230 (5) | |
N4 | 0.29295 (8) | 1.1427 (3) | 0.1053 (2) | 0.0640 (10) | |
H4A | 0.3103 | 1.1712 | 0.0844 | 0.077* | |
H4B | 0.2718 | 1.1724 | 0.0845 | 0.077* | |
N5 | 0.41670 (6) | 0.53040 (19) | 0.49884 (15) | 0.0235 (5) | |
N6 | 0.46858 (6) | 0.4129 (2) | 0.51736 (16) | 0.0274 (5) | |
N7 | 0.41832 (5) | 0.40206 (18) | 0.38452 (14) | 0.0212 (5) | |
N8 | 0.42558 (9) | −0.0979 (2) | 0.6145 (2) | 0.0587 (9) | |
H8A | 0.4058 | −0.1331 | 0.6145 | 0.070* | |
H8B | 0.4449 | −0.1194 | 0.6557 | 0.070* | |
N9 | 0.34589 (6) | 0.3841 (2) | 0.42168 (16) | 0.0274 (5) | |
N10 | 0.40774 (6) | 0.65618 (19) | 0.32242 (15) | 0.0239 (5) | |
C1 | 0.31931 (7) | 0.5951 (2) | 0.24867 (18) | 0.0229 (5) | |
C2 | 0.33096 (8) | 0.4491 (2) | 0.14931 (19) | 0.0298 (6) | |
H2 | 0.3454 | 0.3875 | 0.1357 | 0.036* | |
C3 | 0.30007 (8) | 0.4755 (3) | 0.0844 (2) | 0.0339 (7) | |
H3 | 0.2927 | 0.4334 | 0.0262 | 0.041* | |
C4 | 0.28045 (8) | 0.5663 (3) | 0.1082 (2) | 0.0344 (7) | |
H4 | 0.2593 | 0.5868 | 0.0638 | 0.041* | |
C5 | 0.30980 (7) | 0.8664 (2) | 0.30240 (18) | 0.0239 (6) | |
C6 | 0.27690 (8) | 0.9142 (3) | 0.2684 (2) | 0.0373 (7) | |
H6 | 0.2579 | 0.8836 | 0.2900 | 0.045* | |
C7 | 0.27134 (8) | 1.0056 (3) | 0.2037 (2) | 0.0443 (8) | |
H7 | 0.2486 | 1.0378 | 0.1813 | 0.053* | |
C8 | 0.29878 (8) | 1.0518 (3) | 0.1703 (2) | 0.0342 (7) | |
C9 | 0.33169 (8) | 1.0030 (3) | 0.2045 (2) | 0.0348 (7) | |
H9 | 0.3507 | 1.0330 | 0.1827 | 0.042* | |
C10 | 0.33721 (7) | 0.9114 (3) | 0.2697 (2) | 0.0318 (6) | |
H10 | 0.3599 | 0.8789 | 0.2924 | 0.038* | |
C11 | 0.43653 (7) | 0.4463 (2) | 0.47028 (17) | 0.0224 (5) | |
C12 | 0.43111 (8) | 0.5883 (2) | 0.57944 (19) | 0.0296 (6) | |
H12 | 0.4181 | 0.6479 | 0.6014 | 0.036* | |
C13 | 0.46446 (8) | 0.5632 (3) | 0.6311 (2) | 0.0353 (7) | |
H13 | 0.4750 | 0.6054 | 0.6876 | 0.042* | |
C14 | 0.48192 (7) | 0.4741 (3) | 0.5973 (2) | 0.0335 (7) | |
H14 | 0.5048 | 0.4549 | 0.6329 | 0.040* | |
C15 | 0.42831 (7) | 0.1675 (2) | 0.41761 (18) | 0.0235 (5) | |
C16 | 0.45886 (7) | 0.1330 (2) | 0.48288 (19) | 0.0267 (6) | |
H16 | 0.4804 | 0.1699 | 0.4823 | 0.032* | |
C17 | 0.45791 (8) | 0.0452 (2) | 0.5484 (2) | 0.0336 (7) | |
H17 | 0.4788 | 0.0216 | 0.5926 | 0.040* | |
C18 | 0.42632 (9) | −0.0092 (3) | 0.5502 (2) | 0.0376 (7) | |
C19 | 0.39586 (9) | 0.0261 (3) | 0.4843 (2) | 0.0381 (7) | |
H19 | 0.3743 | −0.0107 | 0.4845 | 0.046* | |
C20 | 0.39676 (8) | 0.1139 (2) | 0.4190 (2) | 0.0311 (6) | |
H20 | 0.3759 | 0.1379 | 0.3748 | 0.037* | |
C21 | 0.35814 (8) | 0.3409 (3) | 0.5089 (2) | 0.0326 (7) | |
H21 | 0.3788 | 0.3751 | 0.5475 | 0.039* | |
C22 | 0.34273 (8) | 0.2498 (3) | 0.5466 (2) | 0.0389 (7) | |
H22 | 0.3526 | 0.2225 | 0.6094 | 0.047* | |
C23 | 0.31292 (9) | 0.1993 (3) | 0.4922 (3) | 0.0495 (9) | |
H23 | 0.3017 | 0.1359 | 0.5161 | 0.059* | |
C24 | 0.29964 (10) | 0.2425 (4) | 0.4023 (3) | 0.0661 (12) | |
H24 | 0.2790 | 0.2096 | 0.3626 | 0.079* | |
C25 | 0.31661 (9) | 0.3340 (3) | 0.3703 (2) | 0.0515 (9) | |
H25 | 0.3070 | 0.3635 | 0.3081 | 0.062* | |
C26 | 0.41834 (8) | 0.6433 (3) | 0.2431 (2) | 0.0336 (7) | |
H26 | 0.4118 | 0.5732 | 0.2064 | 0.040* | |
C27 | 0.43829 (9) | 0.7266 (3) | 0.2117 (2) | 0.0426 (8) | |
H27 | 0.4450 | 0.7142 | 0.1542 | 0.051* | |
C28 | 0.44845 (8) | 0.8276 (3) | 0.2641 (2) | 0.0359 (7) | |
H28 | 0.4623 | 0.8860 | 0.2438 | 0.043* | |
C29 | 0.43811 (8) | 0.8426 (3) | 0.3469 (2) | 0.0346 (7) | |
H29 | 0.4448 | 0.9113 | 0.3852 | 0.041* | |
C30 | 0.41771 (8) | 0.7553 (2) | 0.3730 (2) | 0.0307 (6) | |
H30 | 0.4104 | 0.7662 | 0.4297 | 0.037* | |
H5 | 0.5105 (11) | 0.168 (4) | 0.219 (3) | 0.082 (15)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0261 (2) | 0.02007 (19) | 0.02013 (18) | 0.00081 (14) | 0.00363 (14) | −0.00073 (14) |
S1 | 0.0264 (3) | 0.0205 (3) | 0.0191 (3) | −0.0007 (3) | 0.0067 (3) | −0.0014 (2) |
S2 | 0.0288 (4) | 0.0227 (3) | 0.0198 (3) | 0.0009 (3) | 0.0078 (3) | −0.0013 (2) |
O1 | 0.0332 (11) | 0.0287 (10) | 0.0203 (9) | −0.0015 (8) | 0.0018 (8) | −0.0045 (8) |
O2 | 0.0289 (10) | 0.0292 (10) | 0.0283 (10) | −0.0026 (8) | 0.0126 (8) | 0.0016 (8) |
O3 | 0.0420 (12) | 0.0340 (11) | 0.0222 (10) | 0.0031 (9) | 0.0015 (9) | −0.0070 (8) |
O4 | 0.0334 (11) | 0.0361 (12) | 0.0338 (11) | 0.0020 (9) | 0.0182 (9) | 0.0035 (9) |
O5 | 0.070 (3) | 0.0337 (19) | 0.054 (2) | 0.000 | 0.034 (2) | 0.000 |
N1 | 0.0275 (12) | 0.0222 (11) | 0.0201 (11) | 0.0008 (9) | 0.0064 (9) | −0.0005 (9) |
N2 | 0.0277 (12) | 0.0318 (13) | 0.0233 (12) | 0.0029 (10) | 0.0017 (10) | −0.0038 (10) |
N3 | 0.0259 (12) | 0.0223 (12) | 0.0195 (11) | 0.0035 (9) | 0.0035 (9) | −0.0014 (9) |
N4 | 0.0510 (19) | 0.072 (2) | 0.075 (2) | 0.0204 (16) | 0.0289 (17) | 0.0521 (19) |
N5 | 0.0290 (12) | 0.0236 (12) | 0.0182 (11) | −0.0032 (9) | 0.0064 (9) | −0.0018 (9) |
N6 | 0.0228 (12) | 0.0341 (13) | 0.0235 (12) | −0.0022 (10) | 0.0028 (9) | 0.0009 (10) |
N7 | 0.0240 (12) | 0.0194 (11) | 0.0191 (11) | −0.0002 (8) | 0.0033 (9) | −0.0022 (8) |
N8 | 0.089 (3) | 0.0385 (17) | 0.0559 (19) | −0.0041 (16) | 0.0324 (18) | 0.0179 (14) |
N9 | 0.0274 (12) | 0.0271 (13) | 0.0289 (12) | 0.0007 (9) | 0.0092 (10) | 0.0007 (10) |
N10 | 0.0273 (12) | 0.0226 (12) | 0.0214 (11) | 0.0050 (9) | 0.0052 (9) | 0.0018 (9) |
C1 | 0.0263 (14) | 0.0207 (13) | 0.0222 (13) | −0.0023 (10) | 0.0071 (11) | 0.0017 (10) |
C2 | 0.0361 (16) | 0.0270 (15) | 0.0286 (15) | 0.0002 (12) | 0.0126 (13) | −0.0068 (12) |
C3 | 0.0321 (16) | 0.0412 (17) | 0.0257 (14) | −0.0037 (13) | 0.0026 (12) | −0.0109 (13) |
C4 | 0.0295 (16) | 0.0438 (18) | 0.0266 (15) | 0.0023 (13) | 0.0010 (12) | −0.0039 (13) |
C5 | 0.0282 (14) | 0.0221 (14) | 0.0211 (13) | 0.0010 (11) | 0.0058 (11) | 0.0005 (10) |
C6 | 0.0324 (16) | 0.0361 (17) | 0.0483 (19) | 0.0067 (13) | 0.0192 (15) | 0.0154 (14) |
C7 | 0.0334 (17) | 0.047 (2) | 0.056 (2) | 0.0150 (14) | 0.0176 (15) | 0.0235 (16) |
C8 | 0.0379 (17) | 0.0331 (16) | 0.0338 (16) | 0.0054 (13) | 0.0135 (13) | 0.0102 (13) |
C9 | 0.0321 (16) | 0.0403 (18) | 0.0347 (16) | −0.0015 (13) | 0.0133 (13) | 0.0103 (13) |
C10 | 0.0256 (15) | 0.0366 (17) | 0.0329 (16) | 0.0025 (12) | 0.0068 (12) | 0.0068 (13) |
C11 | 0.0270 (14) | 0.0214 (13) | 0.0196 (12) | −0.0045 (10) | 0.0075 (11) | 0.0014 (10) |
C12 | 0.0392 (17) | 0.0283 (15) | 0.0237 (14) | −0.0078 (12) | 0.0124 (12) | −0.0038 (11) |
C13 | 0.0368 (17) | 0.0457 (18) | 0.0219 (14) | −0.0129 (14) | 0.0045 (13) | −0.0094 (13) |
C14 | 0.0250 (15) | 0.0484 (18) | 0.0240 (14) | −0.0066 (13) | 0.0005 (12) | 0.0008 (13) |
C15 | 0.0296 (14) | 0.0183 (13) | 0.0241 (13) | 0.0004 (10) | 0.0094 (11) | −0.0022 (10) |
C16 | 0.0327 (15) | 0.0227 (14) | 0.0261 (14) | −0.0010 (11) | 0.0099 (12) | −0.0024 (11) |
C17 | 0.0467 (19) | 0.0267 (15) | 0.0267 (15) | 0.0021 (13) | 0.0078 (13) | −0.0005 (12) |
C18 | 0.061 (2) | 0.0236 (15) | 0.0347 (17) | 0.0010 (14) | 0.0249 (16) | −0.0014 (12) |
C19 | 0.0451 (19) | 0.0239 (15) | 0.054 (2) | −0.0077 (13) | 0.0279 (16) | −0.0054 (14) |
C20 | 0.0302 (15) | 0.0237 (14) | 0.0411 (17) | −0.0003 (11) | 0.0120 (13) | −0.0040 (12) |
C21 | 0.0344 (16) | 0.0353 (17) | 0.0283 (15) | −0.0069 (13) | 0.0083 (13) | 0.0007 (12) |
C22 | 0.0427 (18) | 0.0438 (18) | 0.0321 (16) | −0.0025 (14) | 0.0130 (14) | 0.0088 (14) |
C23 | 0.048 (2) | 0.050 (2) | 0.050 (2) | −0.0153 (16) | 0.0130 (17) | 0.0136 (17) |
C24 | 0.054 (2) | 0.082 (3) | 0.053 (2) | −0.042 (2) | −0.0043 (19) | 0.023 (2) |
C25 | 0.040 (2) | 0.068 (2) | 0.0388 (19) | −0.0234 (17) | −0.0046 (15) | 0.0137 (17) |
C26 | 0.0466 (19) | 0.0306 (16) | 0.0249 (15) | −0.0012 (13) | 0.0116 (13) | −0.0042 (12) |
C27 | 0.062 (2) | 0.0409 (19) | 0.0319 (17) | −0.0024 (16) | 0.0254 (16) | −0.0008 (14) |
C28 | 0.0407 (18) | 0.0327 (16) | 0.0383 (17) | −0.0059 (13) | 0.0174 (14) | 0.0024 (13) |
C29 | 0.0436 (18) | 0.0268 (16) | 0.0346 (16) | −0.0079 (13) | 0.0123 (14) | −0.0055 (12) |
C30 | 0.0416 (17) | 0.0259 (15) | 0.0271 (15) | −0.0017 (12) | 0.0135 (13) | −0.0041 (11) |
Co1—N7 | 2.091 (2) | C6—C7 | 1.374 (4) |
Co1—N1 | 2.124 (2) | C6—H6 | 0.9500 |
Co1—N3 | 2.132 (2) | C7—C8 | 1.398 (4) |
Co1—N5 | 2.168 (2) | C7—H7 | 0.9500 |
Co1—N10 | 2.193 (2) | C8—C9 | 1.386 (4) |
Co1—N9 | 2.196 (2) | C9—C10 | 1.381 (4) |
S1—O2 | 1.4436 (19) | C9—H9 | 0.9500 |
S1—O1 | 1.4466 (19) | C10—H10 | 0.9500 |
S1—N3 | 1.605 (2) | C12—C13 | 1.375 (4) |
S1—C5 | 1.757 (3) | C12—H12 | 0.9500 |
S2—O3 | 1.443 (2) | C13—C14 | 1.376 (4) |
S2—O4 | 1.449 (2) | C13—H13 | 0.9500 |
S2—N7 | 1.599 (2) | C14—H14 | 0.9500 |
S2—C15 | 1.751 (3) | C15—C16 | 1.392 (4) |
O5—H5 | 0.89 (4) | C15—C20 | 1.392 (4) |
N1—C2 | 1.334 (3) | C16—C17 | 1.380 (4) |
N1—C1 | 1.366 (3) | C16—H16 | 0.9500 |
N2—C1 | 1.332 (3) | C17—C18 | 1.399 (4) |
N2—C4 | 1.339 (3) | C17—H17 | 0.9500 |
N3—C1 | 1.368 (3) | C18—C19 | 1.396 (5) |
N4—C8 | 1.373 (4) | C19—C20 | 1.378 (4) |
N4—H4A | 0.8800 | C19—H19 | 0.9500 |
N4—H4B | 0.8800 | C20—H20 | 0.9500 |
N5—C12 | 1.338 (3) | C21—C22 | 1.376 (4) |
N5—C11 | 1.360 (3) | C21—H21 | 0.9500 |
N6—C11 | 1.335 (3) | C22—C23 | 1.368 (5) |
N6—C14 | 1.342 (3) | C22—H22 | 0.9500 |
N7—C11 | 1.368 (3) | C23—C24 | 1.372 (5) |
N8—C18 | 1.373 (4) | C23—H23 | 0.9500 |
N8—H8A | 0.8800 | C24—C25 | 1.373 (5) |
N8—H8B | 0.8800 | C24—H24 | 0.9500 |
N9—C21 | 1.332 (4) | C25—H25 | 0.9500 |
N9—C25 | 1.335 (4) | C26—C27 | 1.376 (4) |
N10—C26 | 1.334 (3) | C26—H26 | 0.9500 |
N10—C30 | 1.339 (3) | C27—C28 | 1.371 (4) |
C2—C3 | 1.376 (4) | C27—H27 | 0.9500 |
C2—H2 | 0.9500 | C28—C29 | 1.379 (4) |
C3—C4 | 1.379 (4) | C28—H28 | 0.9500 |
C3—H3 | 0.9500 | C29—C30 | 1.385 (4) |
C4—H4 | 0.9500 | C29—H29 | 0.9500 |
C5—C6 | 1.380 (4) | C30—H30 | 0.9500 |
C5—C10 | 1.386 (4) | ||
N7—Co1—N1 | 112.97 (8) | C6—C7—H7 | 119.6 |
N7—Co1—N3 | 174.43 (8) | C8—C7—H7 | 119.6 |
N1—Co1—N3 | 62.84 (8) | N4—C8—C9 | 121.4 (3) |
N7—Co1—N5 | 62.69 (8) | N4—C8—C7 | 120.4 (3) |
N1—Co1—N5 | 173.41 (8) | C9—C8—C7 | 118.2 (3) |
N3—Co1—N5 | 121.11 (8) | C10—C9—C8 | 120.9 (3) |
N7—Co1—N10 | 88.64 (8) | C10—C9—H9 | 119.6 |
N1—Co1—N10 | 92.61 (8) | C8—C9—H9 | 119.6 |
N3—Co1—N10 | 87.91 (8) | C9—C10—C5 | 120.4 (3) |
N5—Co1—N10 | 82.50 (8) | C9—C10—H10 | 119.8 |
N7—Co1—N9 | 91.00 (8) | C5—C10—H10 | 119.8 |
N1—Co1—N9 | 90.65 (8) | N6—C11—N5 | 125.9 (2) |
N3—Co1—N9 | 92.70 (8) | N6—C11—N7 | 125.5 (2) |
N5—Co1—N9 | 94.33 (8) | N5—C11—N7 | 108.6 (2) |
N10—Co1—N9 | 176.60 (8) | N5—C12—C13 | 121.3 (3) |
O2—S1—O1 | 115.23 (11) | N5—C12—H12 | 119.4 |
O2—S1—N3 | 112.88 (11) | C13—C12—H12 | 119.4 |
O1—S1—N3 | 104.94 (11) | C12—C13—C14 | 117.0 (3) |
O2—S1—C5 | 106.95 (12) | C12—C13—H13 | 121.5 |
O1—S1—C5 | 109.53 (12) | C14—C13—H13 | 121.5 |
N3—S1—C5 | 107.05 (12) | N6—C14—C13 | 124.1 (3) |
O3—S2—O4 | 116.35 (12) | N6—C14—H14 | 117.9 |
O3—S2—N7 | 105.41 (11) | C13—C14—H14 | 117.9 |
O4—S2—N7 | 111.97 (12) | C16—C15—C20 | 119.9 (3) |
O3—S2—C15 | 108.95 (12) | C16—C15—S2 | 120.6 (2) |
O4—S2—C15 | 106.96 (12) | C20—C15—S2 | 119.5 (2) |
N7—S2—C15 | 106.82 (11) | C17—C16—C15 | 120.0 (3) |
C2—N1—C1 | 117.7 (2) | C17—C16—H16 | 120.0 |
C2—N1—Co1 | 147.23 (19) | C15—C16—H16 | 120.0 |
C1—N1—Co1 | 94.47 (15) | C16—C17—C18 | 120.4 (3) |
C1—N2—C4 | 114.9 (2) | C16—C17—H17 | 119.8 |
C1—N3—S1 | 123.99 (18) | C18—C17—H17 | 119.8 |
C1—N3—Co1 | 94.06 (15) | N8—C18—C19 | 120.7 (3) |
S1—N3—Co1 | 141.87 (13) | N8—C18—C17 | 120.2 (3) |
C8—N4—H4A | 120.0 | C19—C18—C17 | 119.0 (3) |
C8—N4—H4B | 120.0 | C20—C19—C18 | 120.6 (3) |
H4A—N4—H4B | 120.0 | C20—C19—H19 | 119.7 |
C12—N5—C11 | 117.1 (2) | C18—C19—H19 | 119.7 |
C12—N5—Co1 | 149.3 (2) | C19—C20—C15 | 120.0 (3) |
C11—N5—Co1 | 92.62 (15) | C19—C20—H20 | 120.0 |
C11—N6—C14 | 114.6 (2) | C15—C20—H20 | 120.0 |
C11—N7—S2 | 123.98 (18) | N9—C21—C22 | 124.1 (3) |
C11—N7—Co1 | 95.79 (16) | N9—C21—H21 | 117.9 |
S2—N7—Co1 | 139.33 (12) | C22—C21—H21 | 117.9 |
C18—N8—H8A | 120.0 | C23—C22—C21 | 118.9 (3) |
C18—N8—H8B | 120.0 | C23—C22—H22 | 120.6 |
H8A—N8—H8B | 120.0 | C21—C22—H22 | 120.6 |
C21—N9—C25 | 115.9 (3) | C22—C23—C24 | 118.2 (3) |
C21—N9—Co1 | 119.55 (19) | C22—C23—H23 | 120.9 |
C25—N9—Co1 | 124.4 (2) | C24—C23—H23 | 120.9 |
C26—N10—C30 | 117.0 (2) | C23—C24—C25 | 119.1 (3) |
C26—N10—Co1 | 120.87 (18) | C23—C24—H24 | 120.4 |
C30—N10—Co1 | 122.14 (18) | C25—C24—H24 | 120.4 |
N2—C1—N1 | 125.2 (2) | N9—C25—C24 | 123.8 (3) |
N2—C1—N3 | 126.4 (2) | N9—C25—H25 | 118.1 |
N1—C1—N3 | 108.4 (2) | C24—C25—H25 | 118.1 |
N1—C2—C3 | 121.2 (3) | N10—C26—C27 | 123.2 (3) |
N1—C2—H2 | 119.4 | N10—C26—H26 | 118.4 |
C3—C2—H2 | 119.4 | C27—C26—H26 | 118.4 |
C2—C3—C4 | 116.6 (3) | C28—C27—C26 | 119.4 (3) |
C2—C3—H3 | 121.7 | C28—C27—H27 | 120.3 |
C4—C3—H3 | 121.7 | C26—C27—H27 | 120.3 |
N2—C4—C3 | 124.5 (3) | C27—C28—C29 | 118.6 (3) |
N2—C4—H4 | 117.8 | C27—C28—H28 | 120.7 |
C3—C4—H4 | 117.8 | C29—C28—H28 | 120.7 |
C6—C5—C10 | 119.0 (3) | C28—C29—C30 | 118.5 (3) |
C6—C5—S1 | 120.4 (2) | C28—C29—H29 | 120.8 |
C10—C5—S1 | 120.5 (2) | C30—C29—H29 | 120.8 |
C7—C6—C5 | 120.7 (3) | N10—C30—C29 | 123.4 (3) |
C7—C6—H6 | 119.7 | N10—C30—H30 | 118.3 |
C5—C6—H6 | 119.7 | C29—C30—H30 | 118.3 |
C6—C7—C8 | 120.8 (3) | ||
N7—Co1—N1—C2 | 12.2 (4) | Co1—N3—C1—N1 | −4.2 (2) |
N3—Co1—N1—C2 | −171.9 (4) | C1—N1—C2—C3 | 1.1 (4) |
N10—Co1—N1—C2 | 101.8 (3) | Co1—N1—C2—C3 | 168.7 (2) |
N9—Co1—N1—C2 | −79.2 (3) | N1—C2—C3—C4 | 0.4 (4) |
N7—Co1—N1—C1 | −178.81 (14) | C1—N2—C4—C3 | 0.4 (4) |
N3—Co1—N1—C1 | −2.87 (14) | C2—C3—C4—N2 | −1.1 (5) |
N10—Co1—N1—C1 | −89.18 (15) | O2—S1—C5—C6 | 1.9 (3) |
N9—Co1—N1—C1 | 89.83 (15) | O1—S1—C5—C6 | −123.6 (2) |
O2—S1—N3—C1 | 63.1 (2) | N3—S1—C5—C6 | 123.1 (2) |
O1—S1—N3—C1 | −170.7 (2) | O2—S1—C5—C10 | −176.3 (2) |
C5—S1—N3—C1 | −54.3 (2) | O1—S1—C5—C10 | 58.2 (3) |
O2—S1—N3—Co1 | −112.6 (2) | N3—S1—C5—C10 | −55.0 (3) |
O1—S1—N3—Co1 | 13.6 (2) | C10—C5—C6—C7 | −0.5 (5) |
C5—S1—N3—Co1 | 130.0 (2) | S1—C5—C6—C7 | −178.7 (3) |
N1—Co1—N3—C1 | 2.87 (14) | C5—C6—C7—C8 | 0.4 (5) |
N5—Co1—N3—C1 | 176.82 (14) | C6—C7—C8—N4 | 179.7 (3) |
N10—Co1—N3—C1 | 96.88 (15) | C6—C7—C8—C9 | −0.1 (5) |
N9—Co1—N3—C1 | −86.47 (16) | N4—C8—C9—C10 | −179.8 (3) |
N1—Co1—N3—S1 | 179.3 (2) | C7—C8—C9—C10 | −0.1 (5) |
N5—Co1—N3—S1 | −6.7 (2) | C8—C9—C10—C5 | −0.1 (5) |
N10—Co1—N3—S1 | −86.7 (2) | C6—C5—C10—C9 | 0.3 (4) |
N9—Co1—N3—S1 | 90.0 (2) | S1—C5—C10—C9 | 178.5 (2) |
N7—Co1—N5—C12 | 169.1 (4) | C14—N6—C11—N5 | −3.2 (4) |
N3—Co1—N5—C12 | −6.3 (4) | C14—N6—C11—N7 | 176.1 (2) |
N10—Co1—N5—C12 | 76.7 (4) | C12—N5—C11—N6 | 2.9 (4) |
N9—Co1—N5—C12 | −102.0 (4) | Co1—N5—C11—N6 | 174.8 (2) |
N7—Co1—N5—C11 | 3.19 (14) | C12—N5—C11—N7 | −176.5 (2) |
N3—Co1—N5—C11 | −172.13 (14) | Co1—N5—C11—N7 | −4.6 (2) |
N10—Co1—N5—C11 | −89.16 (15) | S2—N7—C11—N6 | 14.3 (4) |
N9—Co1—N5—C11 | 92.08 (15) | Co1—N7—C11—N6 | −174.6 (2) |
O3—S2—N7—C11 | 174.9 (2) | S2—N7—C11—N5 | −166.26 (17) |
O4—S2—N7—C11 | −57.6 (2) | Co1—N7—C11—N5 | 4.8 (2) |
C15—S2—N7—C11 | 59.1 (2) | C11—N5—C12—C13 | −0.3 (4) |
O3—S2—N7—Co1 | 8.7 (2) | Co1—N5—C12—C13 | −164.4 (3) |
O4—S2—N7—Co1 | 136.13 (18) | N5—C12—C13—C14 | −1.5 (4) |
C15—S2—N7—Co1 | −107.1 (2) | C11—N6—C14—C13 | 1.2 (4) |
N1—Co1—N7—C11 | 171.33 (14) | C12—C13—C14—N6 | 1.0 (4) |
N5—Co1—N7—C11 | −3.19 (14) | O3—S2—C15—C16 | 151.9 (2) |
N10—Co1—N7—C11 | 79.07 (15) | O4—S2—C15—C16 | 25.3 (2) |
N9—Co1—N7—C11 | −97.55 (15) | N7—S2—C15—C16 | −94.7 (2) |
N1—Co1—N7—S2 | −20.1 (2) | O3—S2—C15—C20 | −31.5 (2) |
N5—Co1—N7—S2 | 165.4 (2) | O4—S2—C15—C20 | −158.0 (2) |
N10—Co1—N7—S2 | −112.37 (19) | N7—S2—C15—C20 | 81.9 (2) |
N9—Co1—N7—S2 | 71.01 (19) | C20—C15—C16—C17 | 0.4 (4) |
N7—Co1—N9—C21 | 59.8 (2) | S2—C15—C16—C17 | 177.0 (2) |
N1—Co1—N9—C21 | 172.8 (2) | C15—C16—C17—C18 | −0.4 (4) |
N3—Co1—N9—C21 | −124.3 (2) | C16—C17—C18—N8 | 178.9 (3) |
N5—Co1—N9—C21 | −2.9 (2) | C16—C17—C18—C19 | 0.4 (4) |
N7—Co1—N9—C25 | −114.9 (3) | N8—C18—C19—C20 | −179.1 (3) |
N1—Co1—N9—C25 | −1.9 (3) | C17—C18—C19—C20 | −0.5 (4) |
N3—Co1—N9—C25 | 60.9 (3) | C18—C19—C20—C15 | 0.6 (4) |
N5—Co1—N9—C25 | −177.6 (3) | C16—C15—C20—C19 | −0.6 (4) |
N7—Co1—N10—C26 | 64.3 (2) | S2—C15—C20—C19 | −177.2 (2) |
N1—Co1—N10—C26 | −48.6 (2) | C25—N9—C21—C22 | 0.6 (5) |
N3—Co1—N10—C26 | −111.3 (2) | Co1—N9—C21—C22 | −174.6 (2) |
N5—Co1—N10—C26 | 127.0 (2) | N9—C21—C22—C23 | 0.0 (5) |
N7—Co1—N10—C30 | −114.7 (2) | C21—C22—C23—C24 | −0.4 (6) |
N1—Co1—N10—C30 | 132.3 (2) | C22—C23—C24—C25 | 0.1 (6) |
N3—Co1—N10—C30 | 69.6 (2) | C21—N9—C25—C24 | −0.9 (6) |
N5—Co1—N10—C30 | −52.1 (2) | Co1—N9—C25—C24 | 174.0 (3) |
C4—N2—C1—N1 | 1.2 (4) | C23—C24—C25—N9 | 0.6 (7) |
C4—N2—C1—N3 | −178.2 (3) | C30—N10—C26—C27 | −0.7 (4) |
C2—N1—C1—N2 | −1.9 (4) | Co1—N10—C26—C27 | −179.8 (2) |
Co1—N1—C1—N2 | −175.3 (2) | N10—C26—C27—C28 | 0.9 (5) |
C2—N1—C1—N3 | 177.5 (2) | C26—C27—C28—C29 | −0.3 (5) |
Co1—N1—C1—N3 | 4.2 (2) | C27—C28—C29—C30 | −0.4 (5) |
S1—N3—C1—N2 | −2.1 (4) | C26—N10—C30—C29 | −0.1 (4) |
Co1—N3—C1—N2 | 175.3 (2) | Co1—N10—C30—C29 | 179.0 (2) |
S1—N3—C1—N1 | 178.46 (17) | C28—C29—C30—N10 | 0.7 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O1i | 0.88 | 2.44 | 3.266 (3) | 157 |
N4—H4B···O2ii | 0.88 | 2.30 | 3.108 (4) | 152 |
N8—H8A···O3iii | 0.88 | 2.54 | 3.084 (3) | 120 |
N8—H8B···O5iv | 0.88 | 2.26 | 3.114 (4) | 162 |
O5—H5···O4v | 0.89 (4) | 1.91 (4) | 2.785 (3) | 169 (4) |
Symmetry codes: (i) x, −y+2, z−1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x, −y, z+1/2; (iv) −x+1, −y, −z+1; (v) −x+1, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C10H9N4O2S)2(C5H5N)2]·0.5H2O |
Mr | 724.68 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 193 |
a, b, c (Å) | 39.618 (4), 11.2407 (9), 14.5673 (13) |
β (°) | 104.648 (2) |
V (Å3) | 6276.4 (10) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.74 |
Crystal size (mm) | 0.44 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Rigaku Mercury |
Absorption correction | Multi-scan (REQAB; Jacobson, 1998) |
Tmin, Tmax | 0.738, 0.917 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34520, 7188, 6038 |
Rint | 0.051 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.055, 0.103, 1.18 |
No. of reflections | 7188 |
No. of parameters | 434 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + (0.027P)2 + 11.6654P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.36, −0.52 |
Computer programs: CrystalClear (Rigaku, 1999), CrystalStructure (Rigaku/MSC & Rigaku, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O1i | 0.88 | 2.44 | 3.266 (3) | 156.9 |
N4—H4B···O2ii | 0.88 | 2.30 | 3.108 (4) | 152.2 |
N8—H8A···O3iii | 0.88 | 2.54 | 3.084 (3) | 120.3 |
N8—H8B···O5iv | 0.88 | 2.26 | 3.114 (4) | 162.1 |
O5—H5···O4v | 0.89 (4) | 1.91 (4) | 2.785 (3) | 169 (4) |
Symmetry codes: (i) x, −y+2, z−1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x, −y, z+1/2; (iv) −x+1, −y, −z+1; (v) −x+1, y, −z+1/2. |
The title compound consists of [Co(C11H11N4O4S2] and half a lattice water molecule and is isostructural with trans-[Ni(sdz)2(py)2] (where sdz = sulfadiazine anion and py = pyridine)(Wang et al., 2009), the title cobalt(II) complex has six-coordinate distorted octahedral geometry and contains two bidentate N-coordinated sulfadiazinate anion and two pyridine molecules occupying the trans sites. One water molecule lies on a 2-fold rotation axis. The coordination mode of sulfadiazine is similar to its cobalt(II) complex (Ajibade et al., 2006) and copper(II) complex (Brown et al., 1987), but different from Zn(sdz)2 (Yuan et al., 2001), polymeric Cd(II) complex (Wang et al. 2005), and its copper complex (Hossain et al. 2006). The Co—N bond distances involving the sulfonamide atoms N3, N7, the pyrimido atoms N1, N5, and the pyridine atoms N9, N10, are very similar, at 2.132 (2), 2.091 (2), 2.124 (2), 2.168 (2), 2.196 (2), 2.193 (2) Å, respectively. The tetrahedral coordination at S is distorted, as is also found in the neutral sulfadiazine molecule. A three dimensional network is generated by N—H···O and O—H···O hydrogen bonds involving the complex and water molecules.