metal-organic compounds
The title compound, [Co(C17H16N2O2)(NCS)(H2O)], is a mononuclear cobalt(III) complex whose Co atom is coordinated by two N atoms and two O atoms of the Schiff base ligand, the N atom of the isothiocyanate anion, and a water molecule in a distorted octahedral configuration. The molecules are linked by intermolecular O—HO hydrogen bonds to form chains parallel to b.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031307/ng6068sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031307/ng6068Isup2.hkl |
CCDC reference: 262234
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Bruker, 1997b); software used to prepare material for publication: SHELXTL.
Aqua{2,2'-[propane-1,3-
diylbis(nitrilomethylidyne)]diphenolato}(thiocyanato)cobalt(III) top
Crystal data top
[Co(C17H16N2O2)(NCS)(H2O)] | F(000) = 856 |
Mr = 415.34 | Dx = 1.505 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2671 reflections |
a = 12.7882 (10) Å | θ = 3.0–24.7° |
b = 6.9977 (5) Å | µ = 1.07 mm−1 |
c = 21.3137 (17) Å | T = 295 K |
β = 105.994 (1)° | Block, brown |
V = 1833.5 (2) Å3 | 0.27 × 0.24 × 0.18 mm |
Z = 4 |
Data collection top
Bruker APEX area-detector diffractometer | 3784 independent reflections |
Radiation source: fine-focus sealed tube | 2944 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 26.5°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→16 |
Tmin = 0.761, Tmax = 0.830 | k = −8→8 |
10267 measured reflections | l = −26→23 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.161 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.085P)2 + 1.0593P] where P = (Fo2 + 2Fc2)/3 |
3784 reflections | (Δ/σ)max = 0.001 |
243 parameters | Δρmax = 0.98 e Å−3 |
3 restraints | Δρmin = −0.30 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Co1 | 0.90457 (4) | 0.90108 (7) | 0.83078 (2) | 0.0429 (2) | |
S1 | 1.25988 (11) | 0.6876 (2) | 0.91453 (8) | 0.0859 (5) | |
O1 | 0.8044 (2) | 0.7184 (4) | 0.84916 (13) | 0.0532 (7) | |
O2 | 0.9097 (2) | 0.7594 (4) | 0.75326 (12) | 0.0446 (6) | |
O3 | 0.7741 (2) | 1.0572 (5) | 0.77181 (13) | 0.0637 (8) | |
N1 | 0.8817 (3) | 1.0730 (4) | 0.90909 (15) | 0.0480 (8) | |
N2 | 1.0047 (2) | 1.1097 (4) | 0.80271 (15) | 0.0439 (7) | |
N3 | 1.0443 (3) | 0.7843 (4) | 0.88804 (16) | 0.0496 (8) | |
C1 | 0.7408 (3) | 0.8692 (6) | 0.93198 (18) | 0.0533 (10) | |
C2 | 0.7395 (3) | 0.7184 (6) | 0.88902 (17) | 0.0486 (9) | |
C3 | 0.6697 (4) | 0.5665 (8) | 0.8862 (2) | 0.0666 (13) | |
H3 | 0.6697 | 0.4651 | 0.8581 | 0.080* | |
C4 | 0.5989 (4) | 0.5651 (10) | 0.9256 (2) | 0.0868 (18) | |
H4 | 0.5517 | 0.4626 | 0.9234 | 0.104* | |
C5 | 0.5981 (5) | 0.7118 (11) | 0.9675 (2) | 0.093 (2) | |
H5 | 0.5501 | 0.7095 | 0.9932 | 0.112* | |
C6 | 0.6677 (4) | 0.8625 (9) | 0.9717 (2) | 0.0753 (14) | |
H6 | 0.6673 | 0.9616 | 1.0007 | 0.090* | |
C7 | 0.8111 (3) | 1.0325 (6) | 0.93987 (18) | 0.0515 (10) | |
H7 | 0.8048 | 1.1205 | 0.9713 | 0.062* | |
C8 | 0.9434 (5) | 1.2555 (6) | 0.9303 (2) | 0.0713 (13) | |
H8A | 0.8948 | 1.3623 | 0.9147 | 0.086* | |
H8B | 0.9649 | 1.2604 | 0.9776 | 0.086* | |
C9 | 1.0411 (4) | 1.2798 (6) | 0.9073 (2) | 0.0654 (12) | |
H9A | 1.0885 | 1.1709 | 0.9217 | 0.078* | |
H9B | 1.0797 | 1.3928 | 0.9278 | 0.078* | |
C10 | 1.0194 (4) | 1.2991 (5) | 0.8346 (2) | 0.0601 (11) | |
H10A | 0.9545 | 1.3754 | 0.8174 | 0.072* | |
H10B | 1.0800 | 1.3645 | 0.8248 | 0.072* | |
C11 | 1.0643 (3) | 1.0707 (6) | 0.76511 (19) | 0.0498 (9) | |
H11 | 1.1111 | 1.1667 | 0.7593 | 0.060* | |
C12 | 1.0670 (3) | 0.8938 (6) | 0.73061 (17) | 0.0463 (9) | |
C13 | 0.9910 (3) | 0.7467 (5) | 0.72519 (16) | 0.0413 (8) | |
C14 | 0.9985 (3) | 0.5848 (6) | 0.68852 (19) | 0.0565 (10) | |
H14 | 0.9491 | 0.4853 | 0.6852 | 0.068* | |
C15 | 1.0800 (4) | 0.5725 (8) | 0.6570 (2) | 0.0702 (13) | |
H15 | 1.0841 | 0.4644 | 0.6324 | 0.084* | |
C16 | 1.1537 (4) | 0.7148 (9) | 0.6614 (2) | 0.0724 (14) | |
H16 | 1.2079 | 0.7037 | 0.6402 | 0.087* | |
C17 | 1.1478 (3) | 0.8742 (7) | 0.6971 (2) | 0.0614 (11) | |
H17 | 1.1980 | 0.9720 | 0.6996 | 0.074* | |
C18 | 1.1332 (4) | 0.7462 (5) | 0.89764 (17) | 0.0469 (9) | |
H3A | 0.772 (3) | 1.083 (6) | 0.7303 (8) | 0.059 (13)* | |
H3B | 0.715 (2) | 1.102 (6) | 0.7814 (18) | 0.074 (15)* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0448 (3) | 0.0407 (3) | 0.0425 (3) | −0.0018 (2) | 0.0108 (2) | −0.0002 (2) |
S1 | 0.0573 (8) | 0.0940 (10) | 0.1057 (11) | 0.0065 (7) | 0.0214 (7) | −0.0200 (8) |
O1 | 0.0583 (17) | 0.0551 (16) | 0.0519 (15) | −0.0172 (13) | 0.0247 (13) | −0.0098 (12) |
O2 | 0.0423 (14) | 0.0482 (14) | 0.0445 (13) | −0.0075 (11) | 0.0137 (11) | −0.0071 (11) |
O3 | 0.0527 (18) | 0.097 (2) | 0.0425 (15) | 0.0334 (16) | 0.0146 (13) | 0.0150 (15) |
N1 | 0.062 (2) | 0.0377 (16) | 0.0424 (16) | 0.0027 (14) | 0.0119 (15) | 0.0002 (13) |
N2 | 0.0475 (18) | 0.0352 (16) | 0.0464 (17) | −0.0038 (13) | 0.0085 (14) | 0.0051 (13) |
N3 | 0.054 (2) | 0.0374 (17) | 0.0511 (18) | 0.0062 (15) | 0.0049 (16) | 0.0045 (14) |
C1 | 0.049 (2) | 0.072 (3) | 0.0364 (19) | 0.003 (2) | 0.0073 (16) | 0.0044 (18) |
C2 | 0.045 (2) | 0.069 (3) | 0.0312 (17) | −0.0037 (18) | 0.0093 (15) | 0.0044 (17) |
C3 | 0.065 (3) | 0.088 (3) | 0.047 (2) | −0.032 (2) | 0.015 (2) | −0.008 (2) |
C4 | 0.075 (3) | 0.132 (5) | 0.055 (3) | −0.051 (3) | 0.022 (2) | 0.001 (3) |
C5 | 0.074 (4) | 0.157 (6) | 0.058 (3) | −0.025 (4) | 0.035 (3) | −0.008 (3) |
C6 | 0.073 (3) | 0.108 (4) | 0.052 (3) | −0.001 (3) | 0.029 (2) | −0.007 (3) |
C7 | 0.065 (3) | 0.055 (2) | 0.0356 (19) | 0.010 (2) | 0.0160 (18) | −0.0019 (17) |
C8 | 0.112 (4) | 0.044 (2) | 0.065 (3) | −0.016 (2) | 0.036 (3) | −0.015 (2) |
C9 | 0.091 (3) | 0.038 (2) | 0.059 (3) | −0.016 (2) | 0.006 (2) | −0.0057 (18) |
C10 | 0.079 (3) | 0.033 (2) | 0.068 (3) | −0.0084 (19) | 0.020 (2) | 0.0023 (18) |
C11 | 0.043 (2) | 0.053 (2) | 0.051 (2) | −0.0109 (17) | 0.0082 (17) | 0.0116 (18) |
C12 | 0.038 (2) | 0.060 (2) | 0.0398 (19) | 0.0010 (17) | 0.0080 (15) | 0.0065 (17) |
C13 | 0.0382 (19) | 0.051 (2) | 0.0343 (17) | 0.0015 (16) | 0.0097 (14) | 0.0017 (15) |
C14 | 0.057 (3) | 0.062 (3) | 0.050 (2) | 0.001 (2) | 0.0156 (18) | −0.0079 (19) |
C15 | 0.065 (3) | 0.087 (4) | 0.061 (3) | 0.013 (3) | 0.022 (2) | −0.017 (2) |
C16 | 0.048 (3) | 0.116 (4) | 0.059 (3) | 0.010 (3) | 0.022 (2) | −0.007 (3) |
C17 | 0.040 (2) | 0.089 (3) | 0.058 (2) | −0.007 (2) | 0.0181 (19) | 0.002 (2) |
C18 | 0.069 (3) | 0.0304 (18) | 0.0395 (19) | −0.0073 (17) | 0.0129 (18) | −0.0036 (14) |
Geometric parameters (Å, º) top
Co1—O1 | 1.925 (3) | C5—C6 | 1.367 (8) |
Co1—O2 | 1.944 (2) | C5—H5 | 0.9300 |
Co1—N3 | 2.037 (3) | C6—H6 | 0.9300 |
Co1—O3 | 2.098 (3) | C7—H7 | 0.9300 |
Co1—N2 | 2.133 (3) | C8—C9 | 1.473 (7) |
Co1—N1 | 2.142 (3) | C8—H8A | 0.9700 |
S1—C18 | 1.613 (5) | C8—H8B | 0.9700 |
O1—C2 | 1.341 (4) | C9—C10 | 1.502 (6) |
O2—C13 | 1.338 (4) | C9—H9A | 0.9700 |
O3—H3A | 0.895 (10) | C9—H9B | 0.9700 |
O3—H3B | 0.891 (10) | C10—H10A | 0.9700 |
N1—C7 | 1.285 (5) | C10—H10B | 0.9700 |
N1—C8 | 1.503 (5) | C11—C12 | 1.445 (6) |
N2—C11 | 1.279 (5) | C11—H11 | 0.9300 |
N2—C10 | 1.477 (5) | C12—C13 | 1.398 (5) |
N3—C18 | 1.129 (5) | C12—C17 | 1.415 (5) |
C1—C2 | 1.394 (6) | C13—C14 | 1.395 (5) |
C1—C6 | 1.424 (6) | C14—C15 | 1.389 (6) |
C1—C7 | 1.435 (6) | C14—H14 | 0.9300 |
C2—C3 | 1.379 (6) | C15—C16 | 1.357 (7) |
C3—C4 | 1.394 (6) | C15—H15 | 0.9300 |
C3—H3 | 0.9300 | C16—C17 | 1.365 (7) |
C4—C5 | 1.362 (8) | C16—H16 | 0.9300 |
C4—H4 | 0.9300 | C17—H17 | 0.9300 |
O1—Co1—O2 | 90.83 (11) | C1—C6—H6 | 119.7 |
O1—Co1—N3 | 97.77 (13) | N1—C7—C1 | 128.4 (4) |
O2—Co1—N3 | 94.30 (12) | N1—C7—H7 | 115.8 |
O1—Co1—O3 | 90.20 (13) | C1—C7—H7 | 115.8 |
O2—Co1—O3 | 87.94 (11) | C9—C8—N1 | 114.9 (4) |
N3—Co1—O3 | 171.68 (14) | C9—C8—H8A | 108.5 |
O1—Co1—N2 | 174.92 (11) | N1—C8—H8A | 108.5 |
O2—Co1—N2 | 86.98 (11) | C9—C8—H8B | 108.5 |
N3—Co1—N2 | 86.98 (13) | N1—C8—H8B | 108.5 |
O3—Co1—N2 | 85.14 (13) | H8A—C8—H8B | 107.5 |
O1—Co1—N1 | 88.45 (12) | C8—C9—C10 | 115.0 (4) |
O2—Co1—N1 | 173.17 (11) | C8—C9—H9A | 108.5 |
N3—Co1—N1 | 92.53 (13) | C10—C9—H9A | 108.5 |
O3—Co1—N1 | 85.27 (12) | C8—C9—H9B | 108.5 |
N2—Co1—N1 | 93.18 (12) | C10—C9—H9B | 108.5 |
C2—O1—Co1 | 133.8 (3) | H9A—C9—H9B | 107.5 |
C13—O2—Co1 | 128.8 (2) | N2—C10—C9 | 111.0 (3) |
Co1—O3—H3A | 120 (2) | N2—C10—H10A | 109.4 |
Co1—O3—H3B | 129 (2) | C9—C10—H10A | 109.4 |
H3A—O3—H3B | 111 (2) | N2—C10—H10B | 109.4 |
C7—N1—C8 | 114.7 (3) | C9—C10—H10B | 109.4 |
C7—N1—Co1 | 122.7 (3) | H10A—C10—H10B | 108.0 |
C8—N1—Co1 | 122.6 (3) | N2—C11—C12 | 127.1 (3) |
C11—N2—C10 | 117.2 (3) | N2—C11—H11 | 116.4 |
C11—N2—Co1 | 122.5 (3) | C12—C11—H11 | 116.4 |
C10—N2—Co1 | 119.7 (3) | C13—C12—C17 | 118.3 (4) |
C18—N3—Co1 | 151.2 (3) | C13—C12—C11 | 124.0 (3) |
C2—C1—C6 | 118.3 (4) | C17—C12—C11 | 117.5 (4) |
C2—C1—C7 | 125.0 (4) | O2—C13—C14 | 119.1 (3) |
C6—C1—C7 | 116.7 (4) | O2—C13—C12 | 121.5 (3) |
O1—C2—C3 | 118.6 (4) | C14—C13—C12 | 119.4 (4) |
O1—C2—C1 | 121.2 (4) | C15—C14—C13 | 119.9 (4) |
C3—C2—C1 | 120.1 (4) | C15—C14—H14 | 120.1 |
C2—C3—C4 | 120.0 (5) | C13—C14—H14 | 120.1 |
C2—C3—H3 | 120.0 | C16—C15—C14 | 121.4 (5) |
C4—C3—H3 | 120.0 | C16—C15—H15 | 119.3 |
C5—C4—C3 | 120.8 (5) | C14—C15—H15 | 119.3 |
C5—C4—H4 | 119.6 | C15—C16—C17 | 119.6 (4) |
C3—C4—H4 | 119.6 | C15—C16—H16 | 120.2 |
C4—C5—C6 | 120.2 (5) | C17—C16—H16 | 120.2 |
C4—C5—H5 | 119.9 | C16—C17—C12 | 121.4 (4) |
C6—C5—H5 | 119.9 | C16—C17—H17 | 119.3 |
C5—C6—C1 | 120.6 (5) | C12—C17—H17 | 119.3 |
C5—C6—H6 | 119.7 | N3—C18—S1 | 177.4 (4) |
O2—Co1—O1—C2 | −165.8 (3) | O1—C2—C3—C4 | −178.1 (4) |
N3—Co1—O1—C2 | 99.7 (3) | C1—C2—C3—C4 | 1.1 (7) |
O3—Co1—O1—C2 | −77.9 (3) | C2—C3—C4—C5 | −0.4 (8) |
N1—Co1—O1—C2 | 7.4 (3) | C3—C4—C5—C6 | −0.5 (9) |
O1—Co1—O2—C13 | −150.9 (3) | C4—C5—C6—C1 | 0.7 (9) |
N3—Co1—O2—C13 | −53.0 (3) | C2—C1—C6—C5 | 0.0 (7) |
O3—Co1—O2—C13 | 118.9 (3) | C7—C1—C6—C5 | −179.8 (5) |
N2—Co1—O2—C13 | 33.7 (3) | C8—N1—C7—C1 | −179.1 (4) |
O1—Co1—N1—C7 | −6.4 (3) | Co1—N1—C7—C1 | 3.6 (6) |
N3—Co1—N1—C7 | −104.1 (3) | C2—C1—C7—N1 | 1.9 (7) |
O3—Co1—N1—C7 | 83.9 (3) | C6—C1—C7—N1 | −178.4 (4) |
N2—Co1—N1—C7 | 168.7 (3) | C7—N1—C8—C9 | 165.9 (4) |
O1—Co1—N1—C8 | 176.5 (3) | Co1—N1—C8—C9 | −16.8 (5) |
N3—Co1—N1—C8 | 78.8 (3) | N1—C8—C9—C10 | 65.3 (5) |
O3—Co1—N1—C8 | −93.2 (3) | C11—N2—C10—C9 | −126.3 (4) |
N2—Co1—N1—C8 | −8.4 (3) | Co1—N2—C10—C9 | 45.0 (5) |
O2—Co1—N2—C11 | −22.3 (3) | C8—C9—C10—N2 | −82.2 (5) |
N3—Co1—N2—C11 | 72.1 (3) | C10—N2—C11—C12 | 177.8 (4) |
O3—Co1—N2—C11 | −110.5 (3) | Co1—N2—C11—C12 | 6.8 (5) |
N1—Co1—N2—C11 | 164.5 (3) | N2—C11—C12—C13 | 10.6 (6) |
O2—Co1—N2—C10 | 166.9 (3) | N2—C11—C12—C17 | −173.3 (4) |
N3—Co1—N2—C10 | −98.6 (3) | Co1—O2—C13—C14 | 153.6 (3) |
O3—Co1—N2—C10 | 78.7 (3) | Co1—O2—C13—C12 | −27.9 (5) |
N1—Co1—N2—C10 | −6.3 (3) | C17—C12—C13—O2 | −177.2 (3) |
O1—Co1—N3—C18 | 142.8 (6) | C11—C12—C13—O2 | −1.1 (5) |
O2—Co1—N3—C18 | 51.4 (6) | C17—C12—C13—C14 | 1.4 (5) |
N2—Co1—N3—C18 | −35.3 (6) | C11—C12—C13—C14 | 177.4 (4) |
N1—Co1—N3—C18 | −128.4 (6) | O2—C13—C14—C15 | 177.6 (4) |
Co1—O1—C2—C3 | 174.6 (3) | C12—C13—C14—C15 | −1.0 (6) |
Co1—O1—C2—C1 | −4.5 (6) | C13—C14—C15—C16 | 0.5 (7) |
C6—C1—C2—O1 | 178.3 (4) | C14—C15—C16—C17 | −0.4 (8) |
C7—C1—C2—O1 | −2.0 (6) | C15—C16—C17—C12 | 0.8 (7) |
C6—C1—C2—C3 | −0.8 (6) | C13—C12—C17—C16 | −1.3 (6) |
C7—C1—C2—C3 | 178.9 (4) | C11—C12—C17—C16 | −177.6 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···O1i | 0.90 (1) | 1.95 (2) | 2.739 (4) | 146 (3) |
O3—H3B···O2i | 0.89 (1) | 1.91 (3) | 2.669 (4) | 142 (3) |
Symmetry code: (i) −x+3/2, y+1/2, −z+3/2. |