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In the title complex, [Co(C4H4O5)(C6H6N4S2)(H2O)]·H2O, the CoII atom has a distorted octahedral coordination geometry, formed by one tridentate oxydiacetate, one bidentate diaminobithiazole and one coordinated water molecule. The CoII atom lies on a crystallographic twofold axis, resulting in disorder of the oxydiacetate dianion and the coordinated water. In the crystal structure, parallel thiazole rings are separated by 3.343 (4) Å, allowing π–π stacking interactions to occur.
Supporting information
CCDC reference: 236021
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.022
- wR factor = 0.060
- Data-to-parameter ratio = 10.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT301_ALERT_3_B Main Residue Disorder ......................... 30.00 Perc.
Alert level C
PLAT322_ALERT_2_C Check Hybridisation of S1 in Main Residue . ?
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1985); 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).
Aqua(2,2'-diamino-4,4-bi-1,3-thiazole-
κ2N,
N')(oxydiacetato-
κ3O,
O',
O'')cobalt(II) monohydrate
top
Crystal data top
[Co(C4H4O5)(C6H6N4S2)(H2O)]·H2O | F(000) = 868 |
Mr = 425.32 | Dx = 1.786 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 20 reflections |
a = 8.1393 (16) Å | θ = 9.5–12.2° |
b = 22.855 (2) Å | µ = 1.39 mm−1 |
c = 8.6530 (19) Å | T = 295 K |
β = 100.633 (16)° | Prism, red |
V = 1582.1 (5) Å3 | 0.52 × 0.48 × 0.30 mm |
Z = 4 | |
Data collection top
Rigaku AFC-7S diffractometer | 1414 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.011 |
Graphite monochromator | θmax = 26.0°, θmin = 2.7° |
ω/2θ scans | h = 0→10 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→28 |
Tmin = 0.48, Tmax = 0.66 | l = −10→10 |
1669 measured reflections | 3 standard reflections every 150 reflections |
1558 independent reflections | intensity decay: 0.2% |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0288P)2 + 1.5071P] where P = (Fo2 + 2Fc2)/3 |
1558 reflections | (Δ/σ)max < 0.001 |
155 parameters | Δρmax = 0.27 e Å−3 |
0 restraints | Δρmin = −0.35 e Å−3 |
Special details top
Experimental. The structure was tried to solved and refined with the Cc space group,
the same disordered structure was obtained. The structure refinement with the
Cc space group was converged to R = 0.022, wiht unreasonable
anisotropic thermal parameters for some non-H atoms. |
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 | Occ. (<1) |
Co | 0.5000 | 0.132657 (13) | 0.2500 | 0.02483 (11) | |
S1 | 0.80998 (7) | −0.01499 (3) | 0.07028 (7) | 0.05005 (16) | |
O1 | 0.2925 (6) | 0.1546 (2) | 0.0860 (5) | 0.0352 (9) | 0.50 |
O2 | 0.0692 (3) | 0.21094 (12) | 0.0158 (3) | 0.0410 (6) | 0.50 |
O3 | 0.381 (2) | 0.2003 (7) | 0.352 (2) | 0.037 (4) | 0.50 |
O4 | 0.6589 (5) | 0.1535 (2) | 0.4579 (5) | 0.0319 (9) | 0.50 |
O5 | 0.7184 (3) | 0.20943 (12) | 0.6698 (3) | 0.0409 (6) | 0.50 |
O6 | 0.640 (2) | 0.2000 (5) | 0.131 (2) | 0.0200 (13) | 0.50 |
O1W | 1.0000 | 0.13508 (9) | 0.7500 | 0.0522 (5) | |
N2 | 0.8264 (3) | 0.10194 (9) | 0.0379 (3) | 0.0592 (5) | |
N3 | 0.62451 (18) | 0.06227 (6) | 0.16776 (16) | 0.0299 (3) | |
C2 | 0.7501 (2) | 0.05681 (9) | 0.0926 (2) | 0.0372 (4) | |
C4 | 0.5702 (2) | 0.00758 (7) | 0.2083 (2) | 0.0311 (4) | |
C5 | 0.6547 (3) | −0.03818 (9) | 0.1656 (2) | 0.0420 (5) | |
H5 | 0.6321 | −0.0771 | 0.1849 | 0.050* | |
C11 | 0.1972 (4) | 0.19572 (15) | 0.1092 (4) | 0.0291 (7) | 0.50 |
C12 | 0.2416 (4) | 0.23044 (15) | 0.2611 (4) | 0.0309 (7) | 0.50 |
C13 | 0.4667 (4) | 0.22895 (15) | 0.4932 (4) | 0.0314 (7) | 0.50 |
C14 | 0.6261 (4) | 0.19466 (14) | 0.5436 (4) | 0.0273 (7) | 0.50 |
H1 | 0.9365 | 0.1586 | 0.6843 | 0.050* | |
H2A | 0.7858 | 0.1367 | 0.0446 | 0.050* | |
H2B | 0.8903 | 0.0987 | −0.0275 | 0.050* | |
H12A | 0.2825 | 0.2662 | 0.2476 | 0.050* | 0.50 |
H12B | 0.1434 | 0.2363 | 0.3181 | 0.050* | 0.50 |
H13A | 0.4811 | 0.2656 | 0.4564 | 0.050* | 0.50 |
H13B | 0.4026 | 0.2307 | 0.5736 | 0.050* | 0.50 |
H6A | 0.5815 | 0.2193 | 0.0544 | 0.050* | 0.50 |
H6B | 0.7132 | 0.2177 | 0.1930 | 0.050* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.02576 (18) | 0.02146 (17) | 0.02661 (18) | 0.000 | 0.00311 (12) | 0.000 |
S1 | 0.0468 (3) | 0.0508 (3) | 0.0544 (3) | 0.0197 (2) | 0.0142 (2) | −0.0066 (2) |
O1 | 0.039 (3) | 0.0347 (17) | 0.030 (2) | 0.0029 (18) | 0.0002 (14) | −0.0023 (16) |
O2 | 0.0318 (14) | 0.0437 (15) | 0.0421 (14) | 0.0007 (11) | −0.0072 (11) | 0.0082 (12) |
O3 | 0.032 (6) | 0.046 (4) | 0.035 (5) | 0.007 (3) | 0.009 (3) | −0.005 (2) |
O4 | 0.033 (2) | 0.0280 (15) | 0.033 (2) | 0.0044 (15) | −0.0007 (14) | −0.0018 (16) |
O5 | 0.0406 (15) | 0.0452 (15) | 0.0323 (13) | −0.0001 (12) | −0.0057 (11) | −0.0057 (12) |
O6 | 0.016 (3) | 0.020 (3) | 0.023 (3) | −0.0044 (16) | 0.001 (3) | 0.0045 (17) |
O1W | 0.0474 (12) | 0.0418 (12) | 0.0655 (14) | 0.000 | 0.0056 (11) | 0.000 |
N2 | 0.0601 (12) | 0.0548 (12) | 0.0751 (13) | −0.0068 (10) | 0.0447 (11) | −0.0038 (10) |
N3 | 0.0305 (7) | 0.0290 (7) | 0.0306 (7) | 0.0015 (6) | 0.0067 (6) | −0.0003 (6) |
C2 | 0.0333 (10) | 0.0410 (10) | 0.0376 (10) | 0.0038 (8) | 0.0075 (8) | −0.0053 (8) |
C4 | 0.0388 (10) | 0.0262 (8) | 0.0271 (8) | 0.0035 (7) | 0.0025 (7) | 0.0007 (7) |
C5 | 0.0541 (12) | 0.0301 (9) | 0.0413 (10) | 0.0097 (8) | 0.0075 (9) | −0.0002 (8) |
C11 | 0.0267 (17) | 0.0285 (17) | 0.0301 (17) | −0.0050 (14) | 0.0001 (13) | 0.0083 (14) |
C12 | 0.0292 (17) | 0.0289 (17) | 0.0335 (17) | 0.0061 (14) | 0.0029 (14) | 0.0063 (14) |
C13 | 0.0301 (18) | 0.0298 (17) | 0.0330 (17) | 0.0000 (14) | 0.0022 (14) | −0.0066 (14) |
C14 | 0.0294 (17) | 0.0266 (16) | 0.0253 (15) | −0.0049 (13) | 0.0037 (13) | 0.0027 (13) |
Geometric parameters (Å, º) top
Co—O1 | 2.057 (5) | O1W—H1 | 0.878 |
Co—O4 | 2.068 (5) | N2—C2 | 1.335 (3) |
Co—N3 | 2.0946 (15) | N2—H2A | 0.866 |
Co—O3 | 2.105 (19) | N2—H2B | 0.839 |
Co—O6 | 2.274 (18) | N3—C2 | 1.315 (2) |
S1—C5 | 1.716 (2) | N3—C4 | 1.392 (2) |
S1—C2 | 1.733 (2) | C4—C5 | 1.341 (3) |
O1—C11 | 1.258 (6) | C5—H5 | 0.930 |
O2—C11 | 1.244 (4) | C11—C12 | 1.521 (5) |
O3—C12 | 1.434 (17) | C12—H12A | 0.898 |
O3—C13 | 1.443 (17) | C12—H12B | 1.023 |
O4—C14 | 1.256 (6) | C13—C14 | 1.510 (5) |
O5—C14 | 1.252 (4) | C13—H13A | 0.912 |
O6—H6A | 0.860 | C13—H13B | 0.944 |
O6—H6B | 0.830 | | |
| | | |
O1—Co—O4 | 147.73 (9) | N3—C2—N2 | 123.86 (18) |
O1—Co—N3 | 109.87 (13) | N3—C2—S1 | 113.92 (15) |
O4—Co—N3 | 102.05 (12) | N2—C2—S1 | 122.21 (15) |
O1—Co—O3 | 74.3 (5) | C5—C4—N3 | 115.34 (17) |
O4—Co—O3 | 74.1 (5) | C4—C5—S1 | 110.64 (15) |
N3—Co—O3 | 175.0 (5) | C4—C5—H5 | 124.7 |
O1—Co—O6 | 86.4 (4) | S1—C5—H5 | 124.7 |
O4—Co—O6 | 87.3 (4) | O2—C11—O1 | 124.9 (4) |
N3—Co—O6 | 92.9 (5) | O2—C11—C12 | 116.9 (3) |
O3—Co—O6 | 90.09 (15) | O1—C11—C12 | 118.2 (3) |
C5—S1—C2 | 89.51 (9) | O3—C12—C11 | 105.3 (8) |
C11—O1—Co | 121.6 (3) | O3—C12—H12A | 103.5 |
C12—O3—C13 | 117.2 (12) | C11—C12—H12A | 113.4 |
C12—O3—Co | 119.9 (11) | O3—C12—H12B | 114.0 |
C13—O3—Co | 120.1 (11) | C11—C12—H12B | 113.8 |
C14—O4—Co | 121.3 (3) | H12A—C12—H12B | 106.6 |
Co—O6—H6A | 116.2 | O3—C13—C14 | 105.3 (8) |
Co—O6—H6B | 113.1 | O3—C13—H13A | 101.2 |
H6A—O6—H6B | 118.6 | C14—C13—H13A | 114.7 |
C2—N2—H2A | 118.5 | O3—C13—H13B | 113.3 |
C2—N2—H2B | 123.9 | C14—C13—H13B | 111.8 |
H2A—N2—H2B | 114.7 | H13A—C13—H13B | 110.1 |
C2—N3—C4 | 110.58 (15) | O5—C14—O4 | 123.9 (4) |
C2—N3—Co | 135.23 (13) | O5—C14—C13 | 117.2 (3) |
C4—N3—Co | 114.07 (11) | O4—C14—C13 | 118.9 (3) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1···O5 | 0.88 | 2.11 | 2.835 (3) | 140 |
O1W—H1···O2i | 0.88 | 2.10 | 2.852 (3) | 144 |
N2—H2A···O6 | 0.87 | 2.09 | 2.903 (14) | 155 |
N2—H2A···O3i | 0.87 | 2.28 | 3.067 (16) | 151 |
N2—H2B···O1Wii | 0.84 | 2.41 | 3.174 (3) | 151 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x, y, z−1. |
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