Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680703454X/xu2294sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680703454X/xu2294Isup2.hkl |
CCDC reference: 657604
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.005 Å
- R factor = 0.041
- wR factor = 0.094
- Data-to-parameter ratio = 13.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O5W - H5WA ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT322_ALERT_2_C Check Hybridisation of S1 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of S2 in Main Residue . ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Co (2) 1.80
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 2 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For general background, see: Waring (1981); Fisher et al. (1985). For related structures, see: Liu & Xu (2004); Liu et al. (2004); Liu & Xu (2005); Luo et al. (2004); Wu et al. (2003).
An aqua solution (20 ml) containing DABT (0.20 g, 1 mmol) and CoCl2.6H2O (0.23 g, 1 mmol) was mixed with an aqueous solution (10 ml) of pyridine-2,3-dicarboxylic acid (0.17 g, 1 mmol) and NaOH (0.08 g, 2 mmol). The mixture was refluxed for 6 h. After cooling to room temperature the solution was filtered. Single crystals of the title compound were obtained from the filtrate after 3 d.
H atoms on carbon atoms were placed in calculated positions with C—H distances = 0.93 Å (aromatic), and were included in the final cycles of refinement in riding mode with Uiso(H) = 1.2Ueq(C). H atoms of amino groups and coordinated water molecule were located in a difference Fourier map and included in the structure factor calculations in riding mode with Uiso(H) = 1.2Ueq(N,O). H atoms of lattice water molecules were located in a difference Fourier map and refined as riding in their as-found relative positions, Uiso(H) = 1.5Ueq(O).
Transition metal complexes of 2,2'-diamino-4,4'-bi-1,3-thiazole (DABT) have shown biological activities such as the effective inhibitors of DNA synthesis of the tumor cells (Waring, 1981; Fisher et al., 1985). As part of serial structural investigation of metal complexes with DABT (Liu & Xu, 2004), the title CoII complex was recently prepared and its X-ray structure is presented here.
The molecular structure of the title compound is shown in Fig. 1. The complex of CoII has a distorted octahedral coordination geometry (Table 1) formed by one of DABT ligand, one of pyridine-2,3-dicarboxylate anion, one of coordinated water and one of adjacent pyridine-2,3-dicarboxylate anion.
Within the complex, the DABT molecule shows approximately coplanar configuration with the dihedral angle of 3.29 (19)° between thiazole rings defined by C1, C2, C3, S1, N1 and C4, C5, C6, S2, N3. This is compare to 4.57 (7)° found in [Mn(DABT)(oxydiacetate)] (Luo et al., 2004) and 6.52 (9)° found in [Cu(DABT)(oxydiacetato)] (Wu et al., 2003), but different from the 17.23 (7)° found in [Cr(C4H5NO4)(C6H6N4S2)(H2O)]Cl (Liu et al., 2004) and 20.02 (8)° in [Ni(DABT)(iminodiacetate)] (Liu & Xu, 2005). Bond lengths C6—N4 [1.334 (4) Å] and C3—N2 [1.326 (4) Å] imply the existence of electron delocalization between thiazole rings and amino groups.
Within the pyridine-2,3-dicarboxylate anion, one oxygen atom (O11) of one carboxyl group of the pyridine-2,3-dicarboxylate anion and the nitrogen atom (N11) of pyridine ring chelate to CoII atom and one oxygen atom (O13) of another carboxyl group of the pyridine-2,3-dicarboxylate anion chelates to another neighboring CoII atom to form the dimeric complex across an inversion centre. The dihedral angles between the pyridine ring and two carboxyl group plans are 5.84 (7) and 84.82 (11)° for the plan formed by C11, C16, O11, O12 and the plan formed by C12, C17, O13, O14 respectively. Otherwise, another uncoordinated oxygen atom (O12 and O14) hydrogen bonded to the lattice water within the complex (Fig. 1 and Table 2), which helps to stabilize the crystal structure.
For general background, see: Waring (1981); Fisher et al. (1985). For related structures, see: Liu & Xu (2004); Liu et al. (2004); Liu & Xu (2005); Luo et al. (2004); Wu et al. (2003).
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Co2(C7H3NO4)2(C6H6N4OS2)2(H2O)2]·10H2O | Z = 1 |
Mr = 1060.80 | F(000) = 546 |
Triclinic, P1 | Dx = 1.674 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1415 (12) Å | Cell parameters from 3550 reflections |
b = 11.2685 (17) Å | θ = 2.2–25.0° |
c = 12.0084 (18) Å | µ = 1.08 mm−1 |
α = 74.269 (2)° | T = 295 K |
β = 82.864 (2)° | Prism, red |
γ = 87.713 (2)° | 0.20 × 0.18 × 0.15 mm |
V = 1052.2 (3) Å3 |
Rigaku R-AXIS RAPID IP diffractometer | 3653 independent reflections |
Radiation source: fine-focus sealed tube | 2911 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
Detector resolution: 10.0 pixels mm-1 | θmax = 25.0°, θmin = 2.2° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −12→13 |
Tmin = 0.785, Tmax = 0.850 | l = −10→14 |
5510 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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0371P)2 + 0.1585P] where P = (Fo2 + 2Fc2)/3 |
3653 reflections | (Δ/σ)max = 0.001 |
280 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.35 e Å−3 |
[Co2(C7H3NO4)2(C6H6N4OS2)2(H2O)2]·10H2O | γ = 87.713 (2)° |
Mr = 1060.80 | V = 1052.2 (3) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.1415 (12) Å | Mo Kα radiation |
b = 11.2685 (17) Å | µ = 1.08 mm−1 |
c = 12.0084 (18) Å | T = 295 K |
α = 74.269 (2)° | 0.20 × 0.18 × 0.15 mm |
β = 82.864 (2)° |
Rigaku R-AXIS RAPID IP diffractometer | 3653 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2911 reflections with I > 2σ(I) |
Tmin = 0.785, Tmax = 0.850 | Rint = 0.024 |
5510 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.35 e Å−3 |
3653 reflections | Δρmin = −0.35 e Å−3 |
280 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 | ||
Co | 0.60678 (5) | 0.75306 (4) | 0.67792 (3) | 0.02432 (14) | |
O1 | 0.8327 (3) | 0.7076 (2) | 0.74704 (18) | 0.0352 (6) | |
H1A | 0.8672 | 0.7344 | 0.8051 | 0.042* | |
H1B | 0.8511 | 0.6202 | 0.7539 | 0.042* | |
O11 | 0.7251 (2) | 0.84018 (19) | 0.51418 (18) | 0.0283 (5) | |
O12 | 0.6872 (3) | 0.9176 (2) | 0.32782 (19) | 0.0430 (7) | |
O13 | 0.4141 (3) | 1.10459 (19) | 0.23638 (17) | 0.0310 (5) | |
O14 | 0.3918 (3) | 0.9300 (2) | 0.18751 (18) | 0.0346 (6) | |
O1W | 0.9293 (3) | 0.9688 (3) | 0.1480 (2) | 0.0643 (8) | |
H1WA | 0.8766 | 0.9545 | 0.2156 | 0.096* | |
H1WB | 0.8631 | 0.9621 | 0.1036 | 0.096* | |
O2W | 0.6777 (3) | 0.9173 (3) | 0.0296 (2) | 0.0668 (9) | |
H2WA | 0.6010 | 0.9136 | 0.0851 | 0.100* | |
H2WB | 0.6404 | 0.9555 | −0.0317 | 0.100* | |
O3W | 0.1478 (3) | 0.7661 (3) | 0.1589 (2) | 0.0578 (8) | |
H3WA | 0.0658 | 0.8144 | 0.1503 | 0.087* | |
H3WB | 0.2164 | 0.7997 | 0.1845 | 0.087* | |
O4W | 0.9238 (4) | 0.7896 (3) | 0.9211 (2) | 0.0692 (9) | |
H4WA | 0.8313 | 0.8099 | 0.9535 | 0.104* | |
H4WB | 0.9765 | 0.8543 | 0.8905 | 0.104* | |
O5W | 0.9981 (3) | 0.4713 (3) | 0.7438 (2) | 0.0580 (8) | |
H5WA | 1.0817 | 0.4715 | 0.7758 | 0.087* | |
H5WB | 0.9498 | 0.4013 | 0.7758 | 0.087* | |
N1 | 0.4475 (3) | 0.6361 (2) | 0.8125 (2) | 0.0277 (6) | |
N2 | 0.3392 (4) | 0.7576 (3) | 0.9341 (3) | 0.0496 (9) | |
H2A | 0.4010 | 0.8200 | 0.8967 | 0.060* | |
H2B | 0.2718 | 0.7646 | 0.9912 | 0.060* | |
N3 | 0.6356 (3) | 0.5797 (2) | 0.6344 (2) | 0.0292 (6) | |
N4 | 0.8368 (4) | 0.6102 (3) | 0.4712 (3) | 0.0466 (8) | |
H4A | 0.8628 | 0.6849 | 0.4660 | 0.056* | |
H4B | 0.8918 | 0.5762 | 0.4206 | 0.056* | |
N11 | 0.4028 (3) | 0.8234 (2) | 0.5804 (2) | 0.0244 (6) | |
S1 | 0.24658 (13) | 0.52066 (9) | 0.98787 (8) | 0.0504 (3) | |
S2 | 0.69105 (13) | 0.38950 (9) | 0.55697 (9) | 0.0494 (3) | |
C1 | 0.4354 (4) | 0.5161 (3) | 0.8048 (3) | 0.0318 (8) | |
C2 | 0.3348 (4) | 0.4416 (3) | 0.8901 (3) | 0.0461 (10) | |
H2 | 0.3153 | 0.3593 | 0.8958 | 0.055* | |
C3 | 0.3536 (4) | 0.6516 (3) | 0.9056 (3) | 0.0343 (8) | |
C4 | 0.5369 (4) | 0.4850 (3) | 0.7072 (3) | 0.0315 (8) | |
C5 | 0.5490 (5) | 0.3779 (3) | 0.6782 (3) | 0.0451 (10) | |
H5 | 0.4892 | 0.3073 | 0.7179 | 0.054* | |
C6 | 0.7259 (4) | 0.5416 (3) | 0.5516 (3) | 0.0347 (8) | |
C11 | 0.4513 (4) | 0.8779 (3) | 0.4665 (2) | 0.0219 (7) | |
C12 | 0.3387 (4) | 0.9247 (3) | 0.3874 (3) | 0.0225 (7) | |
C13 | 0.1700 (4) | 0.9115 (3) | 0.4278 (3) | 0.0287 (7) | |
H13 | 0.0912 | 0.9400 | 0.3768 | 0.034* | |
C14 | 0.1218 (4) | 0.8561 (3) | 0.5432 (3) | 0.0292 (8) | |
H14 | 0.0101 | 0.8466 | 0.5715 | 0.035* | |
C15 | 0.2420 (4) | 0.8144 (3) | 0.6168 (3) | 0.0294 (8) | |
H15 | 0.2086 | 0.7785 | 0.6953 | 0.035* | |
C16 | 0.6369 (4) | 0.8799 (3) | 0.4317 (3) | 0.0251 (7) | |
C17 | 0.3888 (4) | 0.9916 (3) | 0.2608 (3) | 0.0267 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.0253 (2) | 0.0238 (3) | 0.0231 (2) | −0.00139 (18) | −0.00092 (17) | −0.00574 (18) |
O1 | 0.0353 (13) | 0.0335 (14) | 0.0382 (14) | −0.0013 (10) | −0.0107 (10) | −0.0090 (11) |
O11 | 0.0217 (12) | 0.0335 (13) | 0.0282 (12) | −0.0005 (10) | −0.0003 (9) | −0.0071 (10) |
O12 | 0.0309 (14) | 0.0640 (18) | 0.0259 (13) | 0.0036 (12) | 0.0064 (10) | −0.0032 (12) |
O13 | 0.0436 (14) | 0.0247 (13) | 0.0244 (12) | −0.0022 (10) | −0.0013 (10) | −0.0070 (10) |
O14 | 0.0486 (15) | 0.0332 (14) | 0.0252 (12) | −0.0035 (11) | −0.0032 (10) | −0.0132 (10) |
O1W | 0.0445 (17) | 0.096 (2) | 0.0495 (18) | −0.0068 (16) | 0.0110 (13) | −0.0213 (16) |
O2W | 0.0565 (18) | 0.104 (3) | 0.0370 (16) | 0.0172 (17) | −0.0063 (13) | −0.0152 (16) |
O3W | 0.0556 (18) | 0.068 (2) | 0.0555 (18) | 0.0012 (15) | −0.0085 (14) | −0.0250 (15) |
O4W | 0.064 (2) | 0.079 (2) | 0.078 (2) | 0.0005 (17) | −0.0182 (16) | −0.0410 (18) |
O5W | 0.0528 (18) | 0.070 (2) | 0.0552 (18) | 0.0086 (15) | −0.0105 (14) | −0.0224 (15) |
N1 | 0.0281 (15) | 0.0266 (15) | 0.0251 (15) | 0.0004 (12) | −0.0002 (12) | −0.0030 (12) |
N2 | 0.057 (2) | 0.045 (2) | 0.0430 (19) | −0.0086 (16) | 0.0228 (16) | −0.0177 (16) |
N3 | 0.0276 (15) | 0.0267 (15) | 0.0347 (16) | 0.0009 (12) | −0.0036 (12) | −0.0107 (13) |
N4 | 0.050 (2) | 0.0421 (19) | 0.048 (2) | −0.0006 (15) | 0.0140 (16) | −0.0209 (16) |
N11 | 0.0244 (14) | 0.0229 (14) | 0.0249 (14) | −0.0020 (11) | 0.0007 (11) | −0.0057 (11) |
S1 | 0.0504 (6) | 0.0504 (6) | 0.0390 (6) | −0.0131 (5) | 0.0117 (5) | 0.0015 (5) |
S2 | 0.0630 (7) | 0.0339 (6) | 0.0588 (7) | 0.0044 (5) | −0.0069 (5) | −0.0261 (5) |
C1 | 0.0314 (19) | 0.0279 (19) | 0.0337 (19) | −0.0034 (15) | −0.0088 (15) | −0.0013 (15) |
C2 | 0.049 (2) | 0.033 (2) | 0.051 (2) | −0.0106 (18) | −0.0011 (19) | −0.0032 (18) |
C3 | 0.0319 (19) | 0.037 (2) | 0.0279 (19) | 0.0003 (16) | 0.0003 (15) | −0.0006 (16) |
C4 | 0.036 (2) | 0.0237 (18) | 0.036 (2) | 0.0004 (15) | −0.0118 (15) | −0.0067 (15) |
C5 | 0.056 (3) | 0.028 (2) | 0.053 (2) | −0.0035 (18) | −0.0084 (19) | −0.0115 (18) |
C6 | 0.038 (2) | 0.030 (2) | 0.042 (2) | 0.0078 (16) | −0.0081 (16) | −0.0182 (16) |
C11 | 0.0256 (17) | 0.0191 (16) | 0.0233 (17) | −0.0011 (13) | −0.0037 (13) | −0.0090 (13) |
C12 | 0.0271 (17) | 0.0187 (16) | 0.0241 (17) | 0.0005 (13) | −0.0022 (13) | −0.0103 (13) |
C13 | 0.0276 (18) | 0.0292 (19) | 0.0326 (19) | 0.0040 (14) | −0.0079 (14) | −0.0124 (15) |
C14 | 0.0216 (17) | 0.0306 (19) | 0.0352 (19) | −0.0021 (14) | 0.0032 (14) | −0.0111 (15) |
C15 | 0.0287 (18) | 0.0311 (19) | 0.0267 (18) | −0.0028 (14) | 0.0026 (14) | −0.0073 (14) |
C16 | 0.0267 (17) | 0.0217 (17) | 0.0282 (19) | −0.0007 (13) | 0.0004 (14) | −0.0101 (14) |
C17 | 0.0240 (17) | 0.030 (2) | 0.0266 (18) | 0.0013 (14) | −0.0055 (13) | −0.0071 (15) |
Co—O1 | 2.100 (2) | N2—H2B | 0.8421 |
Co—O11 | 2.077 (2) | N3—C6 | 1.319 (4) |
Co—O13i | 2.119 (2) | N3—C4 | 1.392 (4) |
Co—N1 | 2.119 (2) | N4—C6 | 1.334 (4) |
Co—N3 | 2.151 (3) | N4—H4A | 0.8603 |
Co—N11 | 2.152 (3) | N4—H4B | 0.8727 |
O1—H1A | 0.9091 | N11—C15 | 1.326 (4) |
O1—H1B | 0.9730 | N11—C11 | 1.354 (4) |
O11—C16 | 1.268 (4) | S1—C2 | 1.730 (4) |
O12—C16 | 1.226 (4) | S1—C3 | 1.735 (3) |
O13—C17 | 1.246 (4) | S2—C5 | 1.721 (4) |
O13—Coi | 2.119 (2) | S2—C6 | 1.731 (3) |
O14—C17 | 1.258 (4) | C1—C2 | 1.344 (4) |
O1W—H1WA | 0.8476 | C1—C4 | 1.462 (4) |
O1W—H1WB | 0.8222 | C2—H2 | 0.9300 |
O2W—H2WA | 0.8481 | C4—C5 | 1.342 (5) |
O2W—H2WB | 0.8324 | C5—H5 | 0.9300 |
O3W—H3WA | 0.8428 | C11—C12 | 1.388 (4) |
O3W—H3WB | 0.8205 | C11—C16 | 1.517 (4) |
O4W—H4WA | 0.8557 | C12—C13 | 1.398 (4) |
O4W—H4WB | 0.8309 | C12—C17 | 1.515 (4) |
O5W—H5WA | 0.8221 | C13—C14 | 1.371 (4) |
O5W—H5WB | 0.8637 | C13—H13 | 0.9300 |
N1—C3 | 1.322 (4) | C14—C15 | 1.383 (4) |
N1—C1 | 1.388 (4) | C14—H14 | 0.9300 |
N2—C3 | 1.326 (4) | C15—H15 | 0.9300 |
N2—H2A | 0.8659 | ||
O11—Co—O1 | 92.19 (8) | C5—S2—C6 | 89.78 (17) |
O11—Co—O13i | 102.79 (8) | C2—C1—N1 | 115.8 (3) |
O1—Co—O13i | 86.43 (9) | C2—C1—C4 | 127.8 (3) |
O11—Co—N1 | 161.66 (10) | N1—C1—C4 | 116.3 (3) |
O1—Co—N1 | 99.38 (9) | C1—C2—S1 | 110.3 (3) |
O13i—Co—N1 | 92.16 (9) | C1—C2—H2 | 124.9 |
O11—Co—N3 | 89.33 (9) | S1—C2—H2 | 124.9 |
O1—Co—N3 | 85.08 (9) | N1—C3—N2 | 123.7 (3) |
O13i—Co—N3 | 165.46 (9) | N1—C3—S1 | 114.1 (3) |
N1—Co—N3 | 77.62 (10) | N2—C3—S1 | 122.2 (3) |
O11—Co—N11 | 77.37 (8) | C5—C4—N3 | 115.4 (3) |
O1—Co—N11 | 169.15 (9) | C5—C4—C1 | 129.1 (3) |
O13i—Co—N11 | 92.97 (9) | N3—C4—C1 | 115.5 (3) |
N1—Co—N11 | 91.47 (9) | C4—C5—S2 | 110.4 (3) |
N3—Co—N11 | 97.56 (10) | C4—C5—H5 | 124.8 |
Co—O1—H1A | 125.8 | S2—C5—H5 | 124.8 |
Co—O1—H1B | 106.3 | N3—C6—N4 | 124.8 (3) |
H1A—O1—H1B | 114.7 | N3—C6—S2 | 113.6 (3) |
C16—O11—Co | 118.08 (19) | N4—C6—S2 | 121.6 (3) |
C17—O13—Coi | 138.2 (2) | N11—C11—C12 | 122.3 (3) |
H1WA—O1W—H1WB | 107.0 | N11—C11—C16 | 114.9 (3) |
H2WA—O2W—H2WB | 107.4 | C12—C11—C16 | 122.8 (3) |
H3WA—O3W—H3WB | 106.3 | C11—C12—C13 | 118.0 (3) |
H4WA—O4W—H4WB | 107.1 | C11—C12—C17 | 123.6 (3) |
H5WA—O5W—H5WB | 107.3 | C13—C12—C17 | 118.5 (3) |
C3—N1—C1 | 110.5 (3) | C14—C13—C12 | 119.5 (3) |
C3—N1—Co | 133.9 (2) | C14—C13—H13 | 120.3 |
C1—N1—Co | 115.6 (2) | C12—C13—H13 | 120.3 |
C3—N2—H2A | 121.2 | C13—C14—C15 | 118.9 (3) |
C3—N2—H2B | 120.2 | C13—C14—H14 | 120.6 |
H2A—N2—H2B | 118.5 | C15—C14—H14 | 120.6 |
C6—N3—C4 | 110.9 (3) | N11—C15—C14 | 122.9 (3) |
C6—N3—Co | 134.3 (2) | N11—C15—H15 | 118.5 |
C4—N3—Co | 114.8 (2) | C14—C15—H15 | 118.5 |
C6—N4—H4A | 125.9 | O12—C16—O11 | 126.4 (3) |
C6—N4—H4B | 118.0 | O12—C16—C11 | 117.7 (3) |
H4A—N4—H4B | 116.0 | O11—C16—C11 | 115.9 (3) |
C15—N11—C11 | 118.4 (3) | O13—C17—O14 | 124.9 (3) |
C15—N11—Co | 128.4 (2) | O13—C17—C12 | 117.7 (3) |
C11—N11—Co | 113.05 (19) | O14—C17—C12 | 117.2 (3) |
C2—S1—C3 | 89.32 (17) |
Symmetry code: (i) −x+1, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O4W | 0.91 | 1.79 | 2.694 (4) | 177 |
O1—H1B···O5W | 0.97 | 2.04 | 2.943 (4) | 153 |
N2—H2A···O13i | 0.87 | 2.08 | 2.853 (4) | 149 |
N2—H2B···O3Wii | 0.84 | 2.14 | 2.968 (4) | 167 |
N4—H4A···O11 | 0.86 | 2.21 | 2.869 (4) | 133 |
N4—H4B···O5Wiii | 0.87 | 2.25 | 3.105 (4) | 165 |
O1W—H1WA···O12 | 0.85 | 1.90 | 2.690 (3) | 156 |
O1W—H1WB···O2W | 0.82 | 1.99 | 2.796 (4) | 166 |
O2W—H2WA···O14 | 0.85 | 2.01 | 2.839 (3) | 167 |
O2W—H2WB···O14iv | 0.83 | 2.01 | 2.817 (3) | 165 |
O3W—H3WA···O1Wv | 0.84 | 2.02 | 2.823 (4) | 158 |
O3W—H3WB···O14 | 0.82 | 2.10 | 2.878 (4) | 159 |
O4W—H4WA···O2Wii | 0.86 | 2.01 | 2.814 (4) | 155 |
O4W—H4WB···O1Wvi | 0.83 | 2.08 | 2.884 (5) | 164 |
O5W—H5WB···O3Wvii | 0.86 | 1.99 | 2.854 (4) | 175 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) x, y, z+1; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+2, −z; (v) x−1, y, z; (vi) −x+2, −y+2, −z+1; (vii) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co2(C7H3NO4)2(C6H6N4OS2)2(H2O)2]·10H2O |
Mr | 1060.80 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 8.1415 (12), 11.2685 (17), 12.0084 (18) |
α, β, γ (°) | 74.269 (2), 82.864 (2), 87.713 (2) |
V (Å3) | 1052.2 (3) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.08 |
Crystal size (mm) | 0.20 × 0.18 × 0.15 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.785, 0.850 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5510, 3653, 2911 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.094, 1.06 |
No. of reflections | 3653 |
No. of parameters | 280 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.35, −0.35 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, CrystalStructure (Rigaku/MSC, 2002), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Co—O1 | 2.100 (2) | Co—N1 | 2.119 (2) |
Co—O11 | 2.077 (2) | Co—N3 | 2.151 (3) |
Co—O13i | 2.119 (2) | Co—N11 | 2.152 (3) |
Symmetry code: (i) −x+1, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O4W | 0.91 | 1.79 | 2.694 (4) | 177 |
O1—H1B···O5W | 0.97 | 2.04 | 2.943 (4) | 153 |
N2—H2A···O13i | 0.87 | 2.08 | 2.853 (4) | 149 |
N2—H2B···O3Wii | 0.84 | 2.14 | 2.968 (4) | 167 |
N4—H4A···O11 | 0.86 | 2.21 | 2.869 (4) | 133 |
N4—H4B···O5Wiii | 0.87 | 2.25 | 3.105 (4) | 165 |
O1W—H1WA···O12 | 0.85 | 1.90 | 2.690 (3) | 156 |
O1W—H1WB···O2W | 0.82 | 1.99 | 2.796 (4) | 166 |
O2W—H2WA···O14 | 0.85 | 2.01 | 2.839 (3) | 167 |
O2W—H2WB···O14iv | 0.83 | 2.01 | 2.817 (3) | 165 |
O3W—H3WA···O1Wv | 0.84 | 2.02 | 2.823 (4) | 158 |
O3W—H3WB···O14 | 0.82 | 2.10 | 2.878 (4) | 159 |
O4W—H4WA···O2Wii | 0.86 | 2.01 | 2.814 (4) | 155 |
O4W—H4WB···O1Wvi | 0.83 | 2.08 | 2.884 (5) | 164 |
O5W—H5WB···O3Wvii | 0.86 | 1.99 | 2.854 (4) | 175 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) x, y, z+1; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+2, −z; (v) x−1, y, z; (vi) −x+2, −y+2, −z+1; (vii) −x+1, −y+1, −z+1. |
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Transition metal complexes of 2,2'-diamino-4,4'-bi-1,3-thiazole (DABT) have shown biological activities such as the effective inhibitors of DNA synthesis of the tumor cells (Waring, 1981; Fisher et al., 1985). As part of serial structural investigation of metal complexes with DABT (Liu & Xu, 2004), the title CoII complex was recently prepared and its X-ray structure is presented here.
The molecular structure of the title compound is shown in Fig. 1. The complex of CoII has a distorted octahedral coordination geometry (Table 1) formed by one of DABT ligand, one of pyridine-2,3-dicarboxylate anion, one of coordinated water and one of adjacent pyridine-2,3-dicarboxylate anion.
Within the complex, the DABT molecule shows approximately coplanar configuration with the dihedral angle of 3.29 (19)° between thiazole rings defined by C1, C2, C3, S1, N1 and C4, C5, C6, S2, N3. This is compare to 4.57 (7)° found in [Mn(DABT)(oxydiacetate)] (Luo et al., 2004) and 6.52 (9)° found in [Cu(DABT)(oxydiacetato)] (Wu et al., 2003), but different from the 17.23 (7)° found in [Cr(C4H5NO4)(C6H6N4S2)(H2O)]Cl (Liu et al., 2004) and 20.02 (8)° in [Ni(DABT)(iminodiacetate)] (Liu & Xu, 2005). Bond lengths C6—N4 [1.334 (4) Å] and C3—N2 [1.326 (4) Å] imply the existence of electron delocalization between thiazole rings and amino groups.
Within the pyridine-2,3-dicarboxylate anion, one oxygen atom (O11) of one carboxyl group of the pyridine-2,3-dicarboxylate anion and the nitrogen atom (N11) of pyridine ring chelate to CoII atom and one oxygen atom (O13) of another carboxyl group of the pyridine-2,3-dicarboxylate anion chelates to another neighboring CoII atom to form the dimeric complex across an inversion centre. The dihedral angles between the pyridine ring and two carboxyl group plans are 5.84 (7) and 84.82 (11)° for the plan formed by C11, C16, O11, O12 and the plan formed by C12, C17, O13, O14 respectively. Otherwise, another uncoordinated oxygen atom (O12 and O14) hydrogen bonded to the lattice water within the complex (Fig. 1 and Table 2), which helps to stabilize the crystal structure.