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In the crystal structure of the title compound, {[Cd(C8H4O4)(C6H6N4S2)2]·H2O}n, the CdII ion is located on a twofold axis, and is coordinated by two diaminobithiazole ligands and two terephthalate dianions in a distorted octahedral geometry. The terephthalate dianion, located on an inversion centre, bridges the CdII ions to form polymeric chains.
Supporting information
CCDC reference: 618293
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.008 Å
- R factor = 0.046
- wR factor = 0.103
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S2
PLAT322_ALERT_2_C Check Hybridisation of S1 in Main Residue . ?
PLAT322_ALERT_2_C Check Hybridisation of S2 in Main Residue . ?
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 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
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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; 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).
catena-Poly[[[bis(2,2'-diamino-4,4'-bi-1,3-thiazole-
κ2N,
N')cadmium(II)]-µ- terephthalato-
κ2O:
O']
monohydrate]
top
Crystal data top
[Cd(C8H4O4)(C6H6N4S2)2]·H2O | F(000) = 1384 |
Mr = 691.06 | Dx = 1.721 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1519 reflections |
a = 9.4657 (14) Å | θ = 2.4–20.9° |
b = 16.749 (3) Å | µ = 1.18 mm−1 |
c = 17.181 (3) Å | T = 295 K |
β = 101.714 (2)° | Prism, yellow |
V = 2667.2 (8) Å3 | 0.25 × 0.16 × 0.13 mm |
Z = 4 | |
Data collection top
Bruker APEXII diffractometer | 2359 independent reflections |
Radiation source: fine-focus sealed tube | 1755 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.065 |
φ and ω scans | θmax = 25.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −11→11 |
Tmin = 0.780, Tmax = 0.860 | k = −19→17 |
6709 measured reflections | l = −18→20 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.046 | H-atom parameters constrained |
wR(F2) = 0.103 | w = 1/[σ2(Fo2) + (0.0437P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
2359 reflections | Δρmax = 0.67 e Å−3 |
174 parameters | Δρmin = −0.98 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0015 (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 | |
Cd | 0.5000 | 0.57839 (3) | 0.2500 | 0.0315 (2) | |
N1 | 0.3738 (4) | 0.5464 (3) | 0.3522 (2) | 0.0360 (10) | |
N2 | 0.1907 (5) | 0.6434 (3) | 0.3466 (3) | 0.0544 (13) | |
H2A | 0.2133 | 0.6628 | 0.3037 | 0.050* | |
H2B | 0.1024 | 0.6588 | 0.3508 | 0.050* | |
N3 | 0.6339 (4) | 0.4804 (3) | 0.3357 (2) | 0.0373 (11) | |
N4 | 0.8564 (5) | 0.4684 (3) | 0.2965 (3) | 0.0535 (13) | |
H4A | 0.9304 | 0.4388 | 0.3033 | 0.050* | |
H4B | 0.8678 | 0.5189 | 0.3001 | 0.050* | |
O1 | 0.6595 (4) | 0.6791 (2) | 0.29369 (19) | 0.0405 (9) | |
O2 | 0.8835 (4) | 0.6381 (2) | 0.3454 (2) | 0.0527 (11) | |
S1 | 0.18941 (17) | 0.51355 (12) | 0.43969 (9) | 0.0631 (5) | |
S2 | 0.75036 (19) | 0.34167 (11) | 0.36213 (13) | 0.0797 (6) | |
C1 | 0.4148 (6) | 0.4742 (3) | 0.3896 (3) | 0.0460 (15) | |
C2 | 0.3296 (6) | 0.4483 (4) | 0.4383 (4) | 0.0631 (18) | |
H2 | 0.3446 | 0.4012 | 0.4675 | 0.076* | |
C3 | 0.2547 (5) | 0.5739 (4) | 0.3725 (3) | 0.0409 (13) | |
C4 | 0.5436 (6) | 0.4346 (4) | 0.3726 (3) | 0.0501 (15) | |
C5 | 0.5883 (7) | 0.3600 (4) | 0.3898 (5) | 0.077 (2) | |
H5 | 0.5384 | 0.3226 | 0.4137 | 0.092* | |
C6 | 0.7483 (6) | 0.4396 (3) | 0.3281 (3) | 0.0467 (15) | |
C7 | 0.7590 (5) | 0.7127 (3) | 0.4279 (3) | 0.0340 (12) | |
C8 | 0.8780 (5) | 0.7154 (3) | 0.4902 (3) | 0.0397 (13) | |
H8 | 0.9643 | 0.6920 | 0.4842 | 0.048* | |
C9 | 0.6303 (5) | 0.7476 (3) | 0.4387 (3) | 0.0369 (13) | |
H9 | 0.5492 | 0.7459 | 0.3978 | 0.044* | |
C10 | 0.7692 (6) | 0.6734 (3) | 0.3503 (3) | 0.0378 (13) | |
O1W | 0.5000 | 0.8252 (3) | 0.2500 | 0.0496 (14) | |
H1W | 0.5664 | 0.7886 | 0.2722 | 0.074* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd | 0.0288 (3) | 0.0308 (4) | 0.0374 (3) | 0.000 | 0.0122 (2) | 0.000 |
N1 | 0.033 (2) | 0.037 (3) | 0.041 (2) | 0.000 (2) | 0.015 (2) | 0.005 (2) |
N2 | 0.054 (3) | 0.057 (4) | 0.060 (3) | 0.023 (3) | 0.032 (3) | 0.017 (3) |
N3 | 0.037 (2) | 0.031 (3) | 0.047 (3) | 0.000 (2) | 0.017 (2) | 0.009 (2) |
N4 | 0.042 (3) | 0.041 (3) | 0.084 (4) | 0.012 (2) | 0.028 (3) | 0.006 (3) |
O1 | 0.040 (2) | 0.039 (2) | 0.042 (2) | −0.0039 (18) | 0.0053 (17) | −0.0029 (17) |
O2 | 0.039 (2) | 0.063 (3) | 0.059 (2) | 0.008 (2) | 0.0175 (19) | −0.019 (2) |
S1 | 0.0510 (9) | 0.0819 (13) | 0.0659 (11) | 0.0035 (9) | 0.0345 (8) | 0.0225 (9) |
S2 | 0.0639 (11) | 0.0470 (11) | 0.1365 (17) | 0.0209 (9) | 0.0399 (11) | 0.0333 (11) |
C1 | 0.041 (3) | 0.045 (4) | 0.053 (3) | −0.003 (3) | 0.012 (3) | 0.014 (3) |
C2 | 0.052 (4) | 0.063 (4) | 0.080 (4) | 0.008 (3) | 0.027 (3) | 0.036 (4) |
C3 | 0.033 (3) | 0.052 (4) | 0.040 (3) | −0.001 (3) | 0.013 (2) | 0.002 (3) |
C4 | 0.037 (3) | 0.049 (4) | 0.067 (4) | 0.005 (3) | 0.016 (3) | 0.019 (3) |
C5 | 0.062 (4) | 0.047 (4) | 0.133 (6) | 0.012 (3) | 0.048 (4) | 0.042 (4) |
C6 | 0.041 (3) | 0.036 (4) | 0.064 (4) | 0.009 (3) | 0.015 (3) | 0.003 (3) |
C7 | 0.035 (3) | 0.029 (3) | 0.038 (3) | −0.005 (2) | 0.009 (2) | 0.001 (2) |
C8 | 0.029 (3) | 0.046 (4) | 0.045 (3) | 0.006 (3) | 0.010 (2) | 0.005 (3) |
C9 | 0.030 (3) | 0.044 (4) | 0.036 (3) | 0.001 (3) | 0.006 (2) | −0.001 (3) |
C10 | 0.036 (3) | 0.032 (3) | 0.048 (3) | −0.008 (3) | 0.013 (3) | −0.001 (3) |
O1W | 0.049 (3) | 0.033 (3) | 0.067 (4) | 0.000 | 0.012 (3) | 0.000 |
Geometric parameters (Å, º) top
Cd—O1 | 2.286 (3) | S1—C2 | 1.723 (6) |
Cd—O1i | 2.286 (3) | S1—C3 | 1.739 (5) |
Cd—N1i | 2.376 (4) | S2—C5 | 1.723 (6) |
Cd—N1 | 2.376 (4) | S2—C6 | 1.741 (6) |
Cd—N3i | 2.389 (4) | C1—C2 | 1.347 (7) |
Cd—N3 | 2.389 (4) | C1—C4 | 1.469 (7) |
N1—C3 | 1.329 (6) | C2—H2 | 0.9300 |
N1—C1 | 1.387 (6) | C4—C5 | 1.333 (8) |
N2—C3 | 1.345 (7) | C5—H5 | 0.9300 |
N2—H2A | 0.8711 | C7—C8 | 1.388 (6) |
N2—H2B | 0.8919 | C7—C9 | 1.397 (6) |
N3—C6 | 1.310 (6) | C7—C10 | 1.507 (7) |
N3—C4 | 1.393 (6) | C8—C9ii | 1.387 (7) |
N4—C6 | 1.341 (7) | C8—H8 | 0.9300 |
N4—H4A | 0.8469 | C9—C8ii | 1.387 (7) |
N4—H4B | 0.8538 | C9—H9 | 0.9300 |
O1—C10 | 1.273 (6) | O1W—H1W | 0.9044 |
O2—C10 | 1.251 (6) | | |
| | | |
O1—Cd—O1i | 84.95 (18) | C2—C1—N1 | 115.1 (5) |
O1—Cd—N1i | 90.66 (13) | C2—C1—C4 | 127.2 (5) |
O1i—Cd—N1i | 108.73 (13) | N1—C1—C4 | 117.8 (5) |
O1—Cd—N1 | 108.73 (13) | C1—C2—S1 | 111.3 (5) |
O1i—Cd—N1 | 90.66 (13) | C1—C2—H2 | 124.3 |
N1i—Cd—N1 | 153.9 (2) | S1—C2—H2 | 124.3 |
O1—Cd—N3i | 160.27 (13) | N1—C3—N2 | 124.2 (5) |
O1i—Cd—N3i | 94.13 (13) | N1—C3—S1 | 114.1 (4) |
N1i—Cd—N3i | 70.92 (14) | N2—C3—S1 | 121.7 (4) |
N1—Cd—N3i | 90.98 (14) | C5—C4—N3 | 114.8 (5) |
O1—Cd—N3 | 94.13 (13) | C5—C4—C1 | 128.2 (5) |
O1i—Cd—N3 | 160.27 (13) | N3—C4—C1 | 116.9 (5) |
N1i—Cd—N3 | 90.98 (14) | C4—C5—S2 | 111.5 (5) |
N1—Cd—N3 | 70.92 (14) | C4—C5—H5 | 124.2 |
N3i—Cd—N3 | 93.2 (2) | S2—C5—H5 | 124.2 |
C3—N1—C1 | 110.6 (4) | N3—C6—N4 | 124.6 (5) |
C3—N1—Cd | 134.2 (3) | N3—C6—S2 | 114.3 (4) |
C1—N1—Cd | 113.8 (3) | N4—C6—S2 | 121.2 (4) |
C3—N2—H2A | 115.6 | C8—C7—C9 | 118.5 (4) |
C3—N2—H2B | 126.1 | C8—C7—C10 | 120.6 (5) |
H2A—N2—H2B | 110.8 | C9—C7—C10 | 121.0 (4) |
C6—N3—C4 | 110.8 (5) | C9ii—C8—C7 | 120.8 (5) |
C6—N3—Cd | 130.0 (4) | C9ii—C8—H8 | 119.6 |
C4—N3—Cd | 111.1 (3) | C7—C8—H8 | 119.6 |
C6—N4—H4A | 114.3 | C8ii—C9—C7 | 120.8 (4) |
C6—N4—H4B | 115.0 | C8ii—C9—H9 | 119.6 |
H4A—N4—H4B | 118.8 | C7—C9—H9 | 119.6 |
H1W—O1W—H1W | 94.74 | O2—C10—O1 | 124.5 (5) |
C10—O1—Cd | 125.3 (3) | O2—C10—C7 | 118.5 (5) |
C2—S1—C3 | 88.9 (3) | O1—C10—C7 | 117.0 (5) |
C5—S2—C6 | 88.6 (3) | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+3/2, −y+3/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O1 | 0.90 | 2.04 | 2.893 (6) | 158 |
N2—H2A···O1i | 0.87 | 2.27 | 3.093 (6) | 158 |
N2—H2B···O2iii | 0.89 | 2.08 | 2.905 (6) | 153 |
N4—H4A···O1Wiv | 0.85 | 2.27 | 2.946 (6) | 137 |
N4—H4B···O2 | 0.85 | 2.14 | 2.960 (6) | 162 |
Symmetry codes: (i) −x+1, y, −z+1/2; (iii) x−1, y, z; (iv) x+1/2, y−1/2, z. |
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