In the crystal structure of mononuclear [Co(SCN)
2(
L)
2(H
2O)
2]·2H
2O [
L is 2,5-bis(4-pyridyl)-1,3,4-thiadiazole, C
12H
8N
4S], the Co
II atom exists in an octahedral environment composed of two N atoms of the SCN
- groups and two aqua ligands, along with the two N atoms from two monodentate
L ligands that are positioned
trans to each other. Hydrogen-bonding interactions between the mononuclear units and uncoordinated water molecules result in a two-dimensional supramolecular network structure. The Co atom lies on a special position of
site symmetry.
Supporting information
CCDC reference: 236020
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.040
- wR factor = 0.102
- Data-to-parameter ratio = 13.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O2W - H2WA ... ?
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT230_ALERT_2_C Hirshfeld Test Diff for S2 - C13 = 5.74 su
PLAT322_ALERT_2_C Check Hybridisation of S1 in Main Residue . ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 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
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXL97.
Diaquabis[2,5-bis(4-pyridyl)-1,3,4-thiadiazole]dithiocyanatocobalt(II) dihydrate
top
Crystal data top
[Co(SCN)2(C12H8N4S)2(H2O)2]·2H2O | Z = 1 |
Mr = 727.76 | F(000) = 373 |
Triclinic, P1 | Dx = 1.572 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.0566 (5) Å | Cell parameters from 674 reflections |
b = 8.3022 (6) Å | θ = 2.3–24.2° |
c = 14.8495 (10) Å | µ = 0.88 mm−1 |
α = 104.593 (2)° | T = 293 K |
β = 93.149 (1)° | Block, red |
γ = 112.148 (1)° | 0.38 × 0.32 × 0.22 mm |
V = 768.79 (9) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2695 independent reflections |
Radiation source: fine-focus sealed tube | 2126 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
φ and ω scans | θmax = 25.0°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→8 |
Tmin = 0.731, Tmax = 0.830 | k = −9→9 |
4193 measured reflections | l = −17→14 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.102 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0535P)2] where P = (Fo2 + 2Fc2)/3 |
2695 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.46 e Å−3 |
4 restraints | Δρmin = −0.28 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 0.5000 | 1.0000 | 0.02668 (18) | |
S1 | 1.03704 (13) | 0.72056 (13) | 0.59599 (6) | 0.0425 (2) | |
N1 | 0.5995 (4) | 0.5615 (3) | 0.87210 (16) | 0.0307 (6) | |
N2 | 0.6742 (4) | 0.7078 (4) | 0.55877 (19) | 0.0449 (7) | |
N3 | 0.7680 (4) | 0.7419 (4) | 0.48311 (18) | 0.0438 (7) | |
N4 | 1.3531 (4) | 0.8726 (4) | 0.28936 (19) | 0.0459 (7) | |
C1 | 0.4732 (5) | 0.5800 (4) | 0.8084 (2) | 0.0383 (8) | |
H1A | 0.3399 | 0.5636 | 0.8198 | 0.046* | |
C2 | 0.5292 (5) | 0.6217 (5) | 0.7272 (2) | 0.0421 (8) | |
H2A | 0.4346 | 0.6300 | 0.6843 | 0.050* | |
C3 | 0.7294 (5) | 0.6512 (4) | 0.7102 (2) | 0.0330 (7) | |
C4 | 0.8613 (5) | 0.6356 (4) | 0.7760 (2) | 0.0393 (8) | |
H4A | 0.9973 | 0.6565 | 0.7677 | 0.047* | |
C5 | 0.7902 (5) | 0.5888 (4) | 0.8541 (2) | 0.0373 (7) | |
H5A | 0.8805 | 0.5756 | 0.8968 | 0.045* | |
C6 | 0.7939 (5) | 0.6923 (4) | 0.6230 (2) | 0.0348 (7) | |
C7 | 0.9566 (5) | 0.7504 (4) | 0.4915 (2) | 0.0342 (7) | |
C8 | 1.0933 (5) | 0.7870 (4) | 0.4207 (2) | 0.0341 (7) | |
C9 | 1.0238 (5) | 0.8181 (5) | 0.3403 (2) | 0.0430 (8) | |
H9A | 0.8895 | 0.8107 | 0.3288 | 0.052* | |
C10 | 1.1601 (5) | 0.8607 (5) | 0.2771 (2) | 0.0481 (9) | |
H10A | 1.1131 | 0.8820 | 0.2233 | 0.058* | |
C11 | 1.4152 (5) | 0.8367 (5) | 0.3655 (2) | 0.0468 (9) | |
H11A | 1.5487 | 0.8409 | 0.3741 | 0.056* | |
C12 | 1.2925 (5) | 0.7936 (4) | 0.4320 (2) | 0.0418 (8) | |
H12A | 1.3428 | 0.7692 | 0.4840 | 0.050* | |
S2 | 0.79008 (13) | 0.05595 (11) | 0.96369 (6) | 0.0425 (2) | |
O1W | 0.2488 (3) | 0.2691 (3) | 0.91010 (15) | 0.0401 (5) | |
H1WA | 0.1397 | 0.2341 | 0.9360 | 0.060* | |
H1WB | 0.2678 | 0.1725 | 0.8817 | 0.060* | |
N5 | 0.6827 (4) | 0.3541 (4) | 0.99392 (19) | 0.0376 (6) | |
C13 | 0.7278 (4) | 0.2311 (4) | 0.9808 (2) | 0.0298 (7) | |
O2W | 0.3285 (4) | −0.0224 (3) | 0.81157 (17) | 0.0555 (7) | |
H2WB | 0.4332 | 0.0305 | 0.7852 | 0.083* | |
H2WA | 0.3718 | −0.0612 | 0.8546 | 0.083* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0281 (3) | 0.0289 (3) | 0.0290 (3) | 0.0147 (2) | 0.0103 (2) | 0.0124 (2) |
S1 | 0.0442 (5) | 0.0630 (6) | 0.0332 (5) | 0.0275 (4) | 0.0149 (4) | 0.0247 (4) |
N1 | 0.0341 (14) | 0.0330 (14) | 0.0291 (14) | 0.0156 (11) | 0.0098 (11) | 0.0117 (11) |
N2 | 0.0427 (16) | 0.0628 (19) | 0.0364 (16) | 0.0220 (14) | 0.0127 (13) | 0.0241 (14) |
N3 | 0.0418 (16) | 0.0621 (19) | 0.0329 (15) | 0.0211 (14) | 0.0116 (12) | 0.0216 (14) |
N4 | 0.0462 (17) | 0.0570 (18) | 0.0383 (17) | 0.0209 (14) | 0.0172 (13) | 0.0182 (14) |
C1 | 0.0343 (17) | 0.052 (2) | 0.0361 (18) | 0.0209 (15) | 0.0124 (14) | 0.0180 (16) |
C2 | 0.0424 (18) | 0.058 (2) | 0.0354 (19) | 0.0253 (16) | 0.0109 (15) | 0.0202 (17) |
C3 | 0.0389 (17) | 0.0287 (16) | 0.0304 (17) | 0.0116 (13) | 0.0104 (13) | 0.0091 (13) |
C4 | 0.0318 (16) | 0.053 (2) | 0.0340 (18) | 0.0132 (15) | 0.0113 (14) | 0.0191 (16) |
C5 | 0.0338 (17) | 0.0473 (19) | 0.0323 (17) | 0.0148 (14) | 0.0055 (13) | 0.0171 (15) |
C6 | 0.0379 (17) | 0.0368 (17) | 0.0325 (17) | 0.0150 (14) | 0.0120 (14) | 0.0139 (14) |
C7 | 0.0429 (18) | 0.0371 (17) | 0.0270 (16) | 0.0178 (14) | 0.0073 (13) | 0.0138 (14) |
C8 | 0.0411 (18) | 0.0328 (17) | 0.0275 (16) | 0.0132 (14) | 0.0096 (13) | 0.0095 (14) |
C9 | 0.0393 (18) | 0.062 (2) | 0.0348 (19) | 0.0227 (16) | 0.0126 (14) | 0.0213 (17) |
C10 | 0.048 (2) | 0.070 (2) | 0.0330 (19) | 0.0253 (18) | 0.0112 (15) | 0.0235 (18) |
C11 | 0.0355 (18) | 0.061 (2) | 0.047 (2) | 0.0210 (16) | 0.0145 (16) | 0.0162 (18) |
C12 | 0.0453 (19) | 0.051 (2) | 0.0338 (18) | 0.0215 (16) | 0.0072 (15) | 0.0175 (16) |
S2 | 0.0438 (5) | 0.0370 (5) | 0.0594 (6) | 0.0239 (4) | 0.0170 (4) | 0.0217 (4) |
O1W | 0.0336 (11) | 0.0381 (12) | 0.0426 (13) | 0.0091 (10) | 0.0116 (10) | 0.0089 (10) |
N5 | 0.0414 (15) | 0.0427 (15) | 0.0432 (16) | 0.0281 (13) | 0.0156 (12) | 0.0180 (13) |
C13 | 0.0257 (15) | 0.0367 (17) | 0.0292 (16) | 0.0114 (13) | 0.0095 (12) | 0.0142 (14) |
O2W | 0.0523 (15) | 0.0572 (16) | 0.0451 (15) | 0.0111 (12) | 0.0152 (12) | 0.0110 (12) |
Geometric parameters (Å, º) top
Co1—N1 | 2.174 (2) | C3—C6 | 1.474 (4) |
Co1—N5 | 2.067 (2) | C4—C5 | 1.375 (4) |
Co1—O1W | 2.118 (2) | C4—H4A | 0.9300 |
Co1—N5i | 2.067 (2) | C5—H5A | 0.9300 |
Co1—O1Wi | 2.118 (2) | C7—C8 | 1.476 (4) |
Co1—N1i | 2.174 (2) | C8—C12 | 1.385 (5) |
S1—C6 | 1.726 (3) | C8—C9 | 1.386 (4) |
S1—C7 | 1.730 (3) | C9—C10 | 1.393 (4) |
N1—C5 | 1.332 (4) | C9—H9A | 0.9300 |
N1—C1 | 1.340 (4) | C10—H10A | 0.9300 |
N2—C6 | 1.302 (4) | C11—C12 | 1.376 (4) |
N2—N3 | 1.372 (4) | C11—H11A | 0.9300 |
N3—C7 | 1.303 (4) | C12—H12A | 0.9300 |
N4—C10 | 1.327 (4) | S2—C13 | 1.637 (3) |
N4—C11 | 1.331 (4) | O1W—H1WA | 0.8635 |
C1—C2 | 1.375 (4) | O1W—H1WB | 0.8691 |
C1—H1A | 0.9300 | N5—C13 | 1.155 (4) |
C2—C3 | 1.389 (4) | O2W—H2WB | 0.8749 |
C2—H2A | 0.9300 | O2W—H2WA | 0.8722 |
C3—C4 | 1.375 (4) | | |
| | | |
N1i—Co1—N1 | 180 | C5—C4—H4A | 120.3 |
N1—Co1—N5 | 88.71 (10) | C3—C4—H4A | 120.3 |
N1—Co1—N5i | 91.29 (10) | N1—C5—C4 | 123.8 (3) |
N1—Co1—O1w | 86.49 (8) | N1—C5—H5A | 118.1 |
N1—Co1—O1wi | 93.51 (9) | C4—C5—H5A | 118.1 |
N1i—Co1—N5 | 91.29 (10) | N2—C6—C3 | 123.8 (3) |
N1i—Co1—N5i | 88.71 (10) | N2—C6—S1 | 113.7 (2) |
N1i—Co1—O1w | 93.51 (9) | C3—C6—S1 | 122.4 (2) |
N1i—Co1—O1wi | 86.49 (8) | N3—C7—C8 | 124.0 (3) |
N5—Co1—N5i | 180 | N3—C7—S1 | 113.6 (2) |
N5—Co1—O1w | 91.13 (10) | C8—C7—S1 | 122.4 (2) |
N5—Co1—O1wi | 88.87 (10) | C12—C8—C9 | 118.0 (3) |
N5i—Co1—O1w | 88.87 (10) | C12—C8—C7 | 122.2 (3) |
N5i—Co1—O1wi | 91.13 (10) | C9—C8—C7 | 119.8 (3) |
O1w—Co1—O1wi | 180 | C8—C9—C10 | 118.4 (3) |
C6—S1—C7 | 87.05 (15) | C8—C9—H9A | 120.8 |
C5—N1—C1 | 116.3 (3) | C10—C9—H9A | 120.8 |
C5—N1—Co1 | 122.24 (19) | N4—C10—C9 | 123.6 (3) |
C1—N1—Co1 | 121.4 (2) | N4—C10—H10A | 118.2 |
C6—N2—N3 | 112.8 (3) | C9—C10—H10A | 118.2 |
C7—N3—N2 | 112.7 (3) | N4—C11—C12 | 123.6 (3) |
C10—N4—C11 | 117.2 (3) | N4—C11—H11A | 118.2 |
N1—C1—C2 | 123.8 (3) | C12—C11—H11A | 118.2 |
N1—C1—H1A | 118.1 | C11—C12—C8 | 119.2 (3) |
C2—C1—H1A | 118.1 | C11—C12—H12A | 120.4 |
C1—C2—C3 | 118.8 (3) | C8—C12—H12A | 120.4 |
C1—C2—H2A | 120.6 | Co1—O1W—H1WA | 113.4 |
C3—C2—H2A | 120.6 | Co1—O1W—H1WB | 119.9 |
C4—C3—C2 | 117.7 (3) | H1WA—O1W—H1WB | 107.4 |
C4—C3—C6 | 121.8 (3) | C13—N5—Co1 | 159.7 (3) |
C2—C3—C6 | 120.5 (3) | N5—C13—S2 | 179.1 (3) |
C5—C4—C3 | 119.4 (3) | H2WB—O2W—H2WA | 108.9 |
| | | |
N5—Co1—N1—C5 | −35.1 (2) | C2—C3—C6—S1 | −177.2 (2) |
N5i—Co1—N1—C5 | 144.9 (2) | C7—S1—C6—N2 | −0.9 (3) |
O1Wi—Co1—N1—C5 | 53.7 (2) | C7—S1—C6—C3 | 178.1 (3) |
O1W—Co1—N1—C5 | −126.3 (2) | N2—N3—C7—C8 | −179.4 (3) |
N5—Co1—N1—C1 | 147.2 (2) | N2—N3—C7—S1 | −1.0 (4) |
N5i—Co1—N1—C1 | −32.8 (2) | C6—S1—C7—N3 | 1.1 (3) |
O1Wi—Co1—N1—C1 | −124.0 (2) | C6—S1—C7—C8 | 179.5 (3) |
O1W—Co1—N1—C1 | 56.0 (2) | N3—C7—C8—C12 | −179.5 (3) |
C6—N2—N3—C7 | 0.3 (4) | S1—C7—C8—C12 | 2.3 (4) |
C5—N1—C1—C2 | 1.1 (5) | N3—C7—C8—C9 | 1.2 (5) |
Co1—N1—C1—C2 | 178.9 (3) | S1—C7—C8—C9 | −177.0 (3) |
N1—C1—C2—C3 | −1.6 (5) | C12—C8—C9—C10 | −2.3 (5) |
C1—C2—C3—C4 | 0.4 (5) | C7—C8—C9—C10 | 177.0 (3) |
C1—C2—C3—C6 | 178.7 (3) | C11—N4—C10—C9 | 1.8 (5) |
C2—C3—C4—C5 | 1.2 (5) | C8—C9—C10—N4 | 0.3 (6) |
C6—C3—C4—C5 | −177.0 (3) | C10—N4—C11—C12 | −1.9 (5) |
C1—N1—C5—C4 | 0.7 (5) | N4—C11—C12—C8 | −0.2 (5) |
Co1—N1—C5—C4 | −177.1 (3) | C9—C8—C12—C11 | 2.3 (5) |
C3—C4—C5—N1 | −1.8 (5) | C7—C8—C12—C11 | −177.0 (3) |
N3—N2—C6—C3 | −178.4 (3) | O1Wi—Co1—N5—C13 | 163.5 (7) |
N3—N2—C6—S1 | 0.6 (4) | O1W—Co1—N5—C13 | −16.5 (7) |
C4—C3—C6—N2 | 179.9 (3) | N1i—Co1—N5—C13 | 77.0 (7) |
C2—C3—C6—N2 | 1.7 (5) | N1—Co1—N5—C13 | −103.0 (7) |
C4—C3—C6—S1 | 1.0 (4) | | |
Symmetry code: (i) −x+1, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1wa···S2ii | 0.86 | 2.47 | 3.304 (3) | 162 |
O1w—H1wb···O2w | 0.87 | 1.90 | 2.766 (3) | 174 |
O2w—H2wb···N4iii | 0.88 | 1.97 | 2.836 (4) | 173 |
Symmetry codes: (ii) x−1, y, z; (iii) −x+2, −y+1, −z+1. |