Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827019901673X/bk1502sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827019901673X/bk1502Isup2.hkl |
CCDC reference: 144612
Compound (I) was prepared according to the method of Parker et al. (1985). A crystal suitable for X-ray diffraction was grown from an acetone-water solution in the dark under aerobic conditions.
The hydrogen-bonding H atoms H1, H1WA and H1WB were located from a difference Fourier map and refined isotropically. The terminal methyl group of the hexyl ligand was found to be disordered over two positions, C17 and C17'. These two atoms refined to occupancies of 0.30 (5) and 0.70 (5), respectively.
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1995); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of the cation of (I) showing 30% probability displacement ellipsoids. H atoms are drawn as spheres of arbitrary radii. |
[Co(C11H19N4O2)(C6H13)H2O]ClO4 | Dx = 1.385 Mg m−3 |
Mr = 500.86 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 34 reflections |
Hall symbol: -R 3 | θ = 5.3–14.8° |
a = 42.064 (6) Å | µ = 0.87 mm−1 |
c = 7.052 (3) Å | T = 293 K |
V = 10806 (5) Å3 | Prism, red |
Z = 18 | 0.8 × 0.4 × 0.4 mm |
F(000) = 4752 |
Siemens P4 diffractometer | 2891 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.032 |
Graphite monochromator | θmax = 25°, θmin = 1.9° |
2θ/ω scans | h = −1→47 |
Absorption correction: empirical (using intensity measurements) via ψ-scan (north et al., 1968) ? | k = −50→1 |
Tmin = 0.687, Tmax = 0.707 | l = 0→8 |
4691 measured reflections | 3 standard reflections every 97 reflections |
4077 independent reflections | intensity decay: 6.0% |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.183 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Calculated w = 1/[σ2(Fo2) + (0.0828P)2 + 52.947P] where P = (Fo2 + 2Fc2)/3 |
4077 reflections | (Δ/σ)max = 0.001 |
298 parameters | Δρmax = 0.69 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Co(C11H19N4O2)(C6H13)H2O]ClO4 | Z = 18 |
Mr = 500.86 | Mo Kα radiation |
Trigonal, R3 | µ = 0.87 mm−1 |
a = 42.064 (6) Å | T = 293 K |
c = 7.052 (3) Å | 0.8 × 0.4 × 0.4 mm |
V = 10806 (5) Å3 |
Siemens P4 diffractometer | 2891 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) via ψ-scan (north et al., 1968) ? | Rint = 0.032 |
Tmin = 0.687, Tmax = 0.707 | 3 standard reflections every 97 reflections |
4691 measured reflections | intensity decay: 6.0% |
4077 independent reflections |
R[F2 > 2σ(F2)] = 0.064 | 0 restraints |
wR(F2) = 0.183 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.69 e Å−3 |
4077 reflections | Δρmin = −0.41 e Å−3 |
298 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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R factor obs 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. Hydrogen atoms attached to the carbon atoms were placed at their calculated position using Hadd command, and refined using riding model. Hydrogen atom of attached to the oxygen atoms were found from DIFMAP and refined isotropically The –CH3 group of the axial ligand were refined disordered, the s.o.f were refined using the free variable. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.589231 (17) | 0.091116 (17) | 0.22658 (8) | 0.0447 (2) | |
O1W | 0.54829 (13) | 0.04825 (13) | 0.3922 (6) | 0.0621 (11) | |
N1 | 0.62390 (11) | 0.09447 (12) | 0.4060 (6) | 0.0546 (11) | |
N2 | 0.60220 (11) | 0.05793 (11) | 0.1102 (6) | 0.0506 (10) | |
N3 | 0.55259 (11) | 0.08704 (12) | 0.0516 (5) | 0.0511 (10) | |
N4 | 0.57586 (13) | 0.12233 (12) | 0.3486 (6) | 0.0564 (11) | |
O1 | 0.63312 (12) | 0.11598 (12) | 0.5592 (5) | 0.0744 (12) | |
O2 | 0.59103 (13) | 0.13940 (12) | 0.5107 (6) | 0.0774 (12) | |
C1 | 0.66323 (16) | 0.07027 (19) | 0.5210 (9) | 0.0769 (18) | |
H1A | 0.6668 | 0.0859 | 0.6278 | 0.115* | |
H1B | 0.6865 | 0.0776 | 0.4620 | 0.115* | |
H1C | 0.6524 | 0.0453 | 0.5629 | 0.115* | |
C2 | 0.63805 (14) | 0.07353 (15) | 0.3800 (8) | 0.0562 (13) | |
C3 | 0.62570 (14) | 0.05296 (15) | 0.2041 (8) | 0.0569 (13) | |
C4 | 0.63967 (17) | 0.02781 (18) | 0.1457 (11) | 0.0807 (19) | |
H4A | 0.6202 | 0.0062 | 0.0873 | 0.121* | |
H4B | 0.6483 | 0.0209 | 0.2554 | 0.121* | |
H4C | 0.6594 | 0.0402 | 0.0570 | 0.121* | |
C5 | 0.58713 (17) | 0.03999 (18) | −0.0719 (8) | 0.0720 (17) | |
H5A | 0.5873 | 0.0170 | −0.0775 | 0.086* | |
H5B | 0.6025 | 0.0556 | −0.1739 | 0.086* | |
C6 | 0.54836 (16) | 0.03247 (16) | −0.0994 (8) | 0.0699 (16) | |
H6A | 0.5381 | 0.0171 | −0.2106 | 0.084* | |
H6B | 0.5338 | 0.0186 | 0.0089 | 0.084* | |
C7 | 0.54427 (17) | 0.06582 (17) | −0.1228 (8) | 0.0674 (15) | |
H7A | 0.5606 | 0.0812 | −0.2224 | 0.081* | |
H7B | 0.5193 | 0.0581 | −0.1613 | 0.081* | |
C8 | 0.50644 (19) | 0.1055 (2) | −0.0171 (11) | 0.095 (2) | |
H8A | 0.5130 | 0.1084 | −0.1489 | 0.142* | |
H8B | 0.5034 | 0.1256 | 0.0233 | 0.142* | |
H8C | 0.4839 | 0.0829 | 0.0009 | 0.142* | |
C9 | 0.53642 (14) | 0.10505 (15) | 0.0981 (8) | 0.0587 (13) | |
C10 | 0.54928 (16) | 0.12543 (16) | 0.2748 (8) | 0.0620 (14) | |
C11 | 0.5342 (2) | 0.1471 (2) | 0.3658 (12) | 0.101 (2) | |
H11A | 0.5447 | 0.1548 | 0.4898 | 0.151* | |
H11B | 0.5080 | 0.1322 | 0.3765 | 0.151* | |
H11C | 0.5401 | 0.1683 | 0.2897 | 0.151* | |
C12 | 0.62900 (15) | 0.13266 (16) | 0.0737 (9) | 0.0672 (15) | |
H12A | 0.6514 | 0.1425 | 0.1473 | 0.081* | |
H12B | 0.6328 | 0.1218 | −0.0394 | 0.081* | |
C13 | 0.6255 (2) | 0.16350 (19) | 0.0125 (10) | 0.089 (2) | |
H13A | 0.6250 | 0.1766 | 0.1248 | 0.106* | |
H13B | 0.6018 | 0.1539 | −0.0491 | 0.106* | |
C14 | 0.65371 (18) | 0.19045 (17) | −0.1172 (10) | 0.0795 (18) | |
H14A | 0.6575 | 0.1770 | −0.2181 | 0.095* | |
H14B | 0.6766 | 0.2036 | −0.0475 | 0.095* | |
C15 | 0.6458 (3) | 0.2181 (2) | −0.2059 (13) | 0.126 (3) | |
H15A | 0.6202 | 0.2053 | −0.2432 | 0.151* | |
H15B | 0.6485 | 0.2354 | −0.1075 | 0.151* | |
C16 | 0.6667 (3) | 0.2392 (3) | −0.3664 (17) | 0.150 (4) | |
H16C | 0.6623 | 0.2233 | −0.4730 | 0.180* | 0.69 (5) |
H16D | 0.6921 | 0.2500 | −0.3318 | 0.180* | 0.69 (5) |
H16A | 0.6762 | 0.2252 | −0.4276 | 0.180* | 0.31 (5) |
H16B | 0.6872 | 0.2614 | −0.3196 | 0.180* | 0.31 (5) |
C17 | 0.648 (2) | 0.243 (2) | −0.516 (6) | 0.26 (4) | 0.31 (5) |
H17A | 0.6363 | 0.2228 | −0.6057 | 0.389* | 0.31 (5) |
H17B | 0.6301 | 0.2461 | −0.4522 | 0.389* | 0.31 (5) |
H17C | 0.6650 | 0.2646 | −0.5824 | 0.389* | 0.31 (5) |
C17' | 0.6593 (6) | 0.2693 (9) | −0.431 (5) | 0.184 (17) | 0.69 (5) |
H17D | 0.6711 | 0.2892 | −0.3429 | 0.276* | 0.69 (5) |
H17E | 0.6681 | 0.2780 | −0.5569 | 0.276* | 0.69 (5) |
H17F | 0.6333 | 0.2595 | −0.4267 | 0.276* | 0.69 (5) |
Cl1 | 0.54919 (4) | −0.03783 (4) | 0.4772 (2) | 0.0605 (4) | |
O11 | 0.58291 (12) | −0.01126 (13) | 0.5568 (7) | 0.0908 (14) | |
O12 | 0.54105 (18) | −0.02117 (14) | 0.3261 (9) | 0.131 (2) | |
O13 | 0.55118 (16) | −0.06784 (15) | 0.4145 (9) | 0.120 (2) | |
O14 | 0.52138 (17) | −0.0487 (2) | 0.6123 (11) | 0.149 (3) | |
H1WA | 0.5486 (17) | 0.0298 (18) | 0.379 (9) | 0.07 (2)* | |
H1WB | 0.529 (2) | 0.045 (2) | 0.401 (11) | 0.10 (3)* | |
H1 | 0.615 (2) | 0.1293 (19) | 0.551 (10) | 0.11 (2)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0455 (4) | 0.0516 (4) | 0.0358 (4) | 0.0234 (3) | 0.0002 (3) | −0.0040 (3) |
O1W | 0.059 (3) | 0.065 (3) | 0.064 (3) | 0.032 (2) | 0.016 (2) | 0.010 (2) |
N1 | 0.051 (2) | 0.061 (3) | 0.042 (2) | 0.021 (2) | −0.0047 (18) | −0.005 (2) |
N2 | 0.047 (2) | 0.055 (2) | 0.045 (2) | 0.021 (2) | 0.0063 (18) | −0.0083 (19) |
N3 | 0.047 (2) | 0.060 (3) | 0.040 (2) | 0.023 (2) | −0.0011 (18) | 0.0030 (19) |
N4 | 0.070 (3) | 0.057 (3) | 0.044 (2) | 0.033 (2) | 0.005 (2) | −0.004 (2) |
O1 | 0.083 (3) | 0.090 (3) | 0.050 (2) | 0.044 (3) | −0.021 (2) | −0.019 (2) |
O2 | 0.103 (3) | 0.079 (3) | 0.054 (2) | 0.048 (3) | −0.007 (2) | −0.024 (2) |
C1 | 0.055 (3) | 0.096 (5) | 0.079 (4) | 0.038 (3) | −0.001 (3) | 0.016 (4) |
C2 | 0.043 (3) | 0.063 (3) | 0.056 (3) | 0.022 (3) | 0.001 (2) | 0.007 (3) |
C3 | 0.047 (3) | 0.061 (3) | 0.063 (3) | 0.026 (3) | 0.011 (3) | 0.004 (3) |
C4 | 0.069 (4) | 0.077 (4) | 0.111 (5) | 0.048 (4) | 0.013 (4) | 0.000 (4) |
C5 | 0.078 (4) | 0.086 (4) | 0.055 (3) | 0.043 (4) | 0.000 (3) | −0.025 (3) |
C6 | 0.072 (4) | 0.071 (4) | 0.051 (3) | 0.024 (3) | −0.005 (3) | −0.022 (3) |
C7 | 0.065 (4) | 0.081 (4) | 0.051 (3) | 0.032 (3) | −0.012 (3) | −0.009 (3) |
C8 | 0.084 (5) | 0.095 (5) | 0.121 (6) | 0.057 (4) | −0.013 (4) | 0.015 (4) |
C9 | 0.052 (3) | 0.065 (3) | 0.063 (3) | 0.033 (3) | 0.005 (3) | 0.012 (3) |
C10 | 0.070 (4) | 0.061 (3) | 0.062 (3) | 0.039 (3) | 0.015 (3) | 0.006 (3) |
C11 | 0.112 (6) | 0.112 (6) | 0.118 (6) | 0.086 (5) | 0.023 (5) | 0.003 (5) |
C12 | 0.048 (3) | 0.072 (4) | 0.073 (4) | 0.023 (3) | 0.006 (3) | 0.015 (3) |
C13 | 0.096 (5) | 0.081 (5) | 0.087 (5) | 0.042 (4) | 0.032 (4) | 0.034 (4) |
C14 | 0.074 (4) | 0.066 (4) | 0.081 (4) | 0.023 (3) | 0.014 (3) | 0.010 (3) |
C15 | 0.131 (8) | 0.102 (6) | 0.118 (7) | 0.039 (6) | 0.033 (6) | 0.041 (5) |
C16 | 0.152 (10) | 0.132 (9) | 0.142 (9) | 0.053 (7) | 0.028 (8) | 0.053 (7) |
C17 | 0.56 (12) | 0.16 (5) | 0.11 (3) | 0.21 (7) | −0.08 (5) | −0.03 (3) |
C17' | 0.22 (2) | 0.14 (2) | 0.20 (3) | 0.095 (17) | 0.030 (17) | 0.11 (2) |
Cl1 | 0.0539 (8) | 0.0567 (8) | 0.0736 (9) | 0.0297 (6) | −0.0053 (6) | 0.0006 (7) |
O11 | 0.077 (3) | 0.090 (3) | 0.096 (3) | 0.035 (3) | −0.021 (3) | −0.018 (3) |
O12 | 0.152 (5) | 0.084 (4) | 0.145 (5) | 0.050 (4) | −0.079 (4) | −0.002 (3) |
O13 | 0.131 (5) | 0.095 (4) | 0.158 (5) | 0.074 (4) | −0.038 (4) | −0.041 (4) |
O14 | 0.101 (4) | 0.146 (6) | 0.179 (7) | 0.045 (4) | 0.062 (4) | 0.028 (5) |
Co1—N1 | 1.882 (4) | C3—C4 | 1.502 (8) |
Co1—N2 | 1.919 (4) | C5—C6 | 1.510 (8) |
Co1—N3 | 1.914 (4) | C6—C7 | 1.506 (8) |
Co1—N4 | 1.876 (4) | C8—C9 | 1.509 (8) |
Co1—C12 | 2.023 (5) | C9—C10 | 1.454 (8) |
Co1—O1W | 2.116 (4) | C10—C11 | 1.492 (8) |
N1—O1 | 1.337 (5) | C12—C13 | 1.444 (8) |
N1—C2 | 1.299 (7) | C13—C14 | 1.479 (8) |
N2—C3 | 1.291 (6) | C14—C15 | 1.499 (11) |
N2—C5 | 1.464 (7) | C15—C16 | 1.435 (12) |
N3—C7 | 1.455 (7) | C16—C17 | 1.36 (5) |
N3—C9 | 1.289 (7) | C16—C17' | 1.52 (2) |
N4—O2 | 1.330 (5) | Cl1—O13 | 1.379 (5) |
N4—C10 | 1.298 (7) | Cl1—O14 | 1.396 (6) |
C1—C2 | 1.508 (7) | Cl1—O12 | 1.409 (5) |
C2—C3 | 1.452 (8) | Cl1—O11 | 1.411 (4) |
N4—Co1—N1 | 97.5 (2) | N1—C2—C1 | 123.3 (5) |
N4—Co1—N3 | 81.31 (19) | C3—C2—C1 | 124.6 (5) |
N1—Co1—N3 | 177.83 (17) | N2—C3—C2 | 114.6 (5) |
N4—Co1—N2 | 177.75 (18) | N2—C3—C4 | 125.1 (5) |
N1—Co1—N2 | 81.39 (19) | C2—C3—C4 | 120.3 (5) |
N3—Co1—N2 | 99.68 (18) | N2—C5—C6 | 111.4 (4) |
N4—Co1—C12 | 92.7 (2) | C7—C6—C5 | 115.7 (5) |
N1—Co1—C12 | 91.1 (2) | N3—C7—C6 | 112.0 (5) |
N3—Co1—C12 | 90.8 (2) | N3—C9—C10 | 114.5 (5) |
N2—Co1—C12 | 89.3 (2) | N3—C9—C8 | 124.1 (6) |
N4—Co1—O1W | 86.7 (2) | C10—C9—C8 | 121.4 (5) |
N1—Co1—O1W | 87.86 (19) | N4—C10—C9 | 111.7 (5) |
N3—Co1—O1W | 90.23 (18) | N4—C10—C11 | 122.7 (6) |
N2—Co1—O1W | 91.29 (19) | C9—C10—C11 | 125.6 (6) |
C12—Co1—O1W | 178.7 (2) | C13—C12—Co1 | 121.6 (4) |
C2—N1—O1 | 119.8 (4) | C12—C13—C14 | 118.0 (6) |
C2—N1—Co1 | 117.1 (4) | C13—C14—C15 | 116.6 (6) |
O1—N1—Co1 | 123.1 (4) | C16—C15—C14 | 120.1 (9) |
C3—N2—C5 | 122.4 (5) | C17—C16—C15 | 118 (4) |
C3—N2—Co1 | 114.7 (4) | C17—C16—C17' | 46.7 (19) |
C5—N2—Co1 | 122.9 (4) | C15—C16—C17' | 115.7 (14) |
C9—N3—C7 | 122.7 (5) | O13—Cl1—O14 | 110.0 (4) |
C9—N3—Co1 | 114.9 (4) | O13—Cl1—O12 | 110.7 (4) |
C7—N3—Co1 | 122.4 (4) | O14—Cl1—O12 | 107.9 (5) |
C10—N4—O2 | 119.7 (5) | O13—Cl1—O11 | 110.8 (3) |
C10—N4—Co1 | 117.4 (4) | O14—Cl1—O11 | 109.5 (4) |
O2—N4—Co1 | 122.7 (4) | O12—Cl1—O11 | 107.8 (3) |
N1—C2—C3 | 112.1 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 1.15 (9) | 1.31 (9) | 2.443 (8) | 167 (8) |
O1W—H1WA···O12 | 0.79 (7) | 2.04 (7) | 2.819 (8) | 171 (8) |
O1W—H1WB···O14i | 0.75 (9) | 2.20 (9) | 2.940 (10) | 166 (8) |
Symmetry code: (i) −x+1, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C11H19N4O2)(C6H13)H2O]ClO4 |
Mr | 500.86 |
Crystal system, space group | Trigonal, R3 |
Temperature (K) | 293 |
a, c (Å) | 42.064 (6), 7.052 (3) |
V (Å3) | 10806 (5) |
Z | 18 |
Radiation type | Mo Kα |
µ (mm−1) | 0.87 |
Crystal size (mm) | 0.8 × 0.4 × 0.4 |
Data collection | |
Diffractometer | Siemens P4 diffractometer |
Absorption correction | Empirical (using intensity measurements) via ψ-scan (North et al., 1968) |
Tmin, Tmax | 0.687, 0.707 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4691, 4077, 2891 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.064, 0.183, 1.03 |
No. of reflections | 4077 |
No. of parameters | 298 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Calculated w = 1/[σ2(Fo2) + (0.0828P)2 + 52.947P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.69, −0.41 |
Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Sheldrick, 1995), SHELXTL.
Co1—N1 | 1.882 (4) | N1—C2 | 1.299 (7) |
Co1—N2 | 1.919 (4) | N2—C3 | 1.291 (6) |
Co1—N3 | 1.914 (4) | N2—C5 | 1.464 (7) |
Co1—N4 | 1.876 (4) | N3—C7 | 1.455 (7) |
Co1—C12 | 2.023 (5) | N3—C9 | 1.289 (7) |
Co1—O1W | 2.116 (4) | N4—O2 | 1.330 (5) |
N1—O1 | 1.337 (5) | N4—C10 | 1.298 (7) |
N4—Co1—N1 | 97.5 (2) | N3—Co1—C12 | 90.8 (2) |
N4—Co1—N3 | 81.31 (19) | N2—Co1—C12 | 89.3 (2) |
N1—Co1—N3 | 177.83 (17) | N4—Co1—O1W | 86.7 (2) |
N4—Co1—N2 | 177.75 (18) | N1—Co1—O1W | 87.86 (19) |
N1—Co1—N2 | 81.39 (19) | N3—Co1—O1W | 90.23 (18) |
N3—Co1—N2 | 99.68 (18) | N2—Co1—O1W | 91.29 (19) |
N4—Co1—C12 | 92.7 (2) | C12—Co1—O1W | 178.7 (2) |
N1—Co1—C12 | 91.1 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 1.15 (9) | 1.31 (9) | 2.443 (8) | 167 (8) |
O1W—H1WA···O12 | 0.79 (7) | 2.04 (7) | 2.819 (8) | 171 (8) |
O1W—H1WB···O14i | 0.75 (9) | 2.20 (9) | 2.940 (10) | 166 (8) |
Symmetry code: (i) −x+1, −y, −z+1. |
Costa-type organocobalt complexes, [LCo(DO)(DOH)pnR]X, where L = neutral base, (DO)(DOH)pn = 3,3'-(propane-1,3-diyldinitrilo)bis(butan-2-one)dioximato, R = alkyl and X = anion group (PF6-, ClO4- etc.), exhibit many interesting properties and have been examined in detail as coenzyme B12 models (Randaccio et al., 1989). However, only a few structures of (aqua)alkyl costa-type complexes (R = CH3, X = PF6-, etc.) are available (Marzilli et al., 1985) and we report here the structural data on a new such compound with R = n-C6H13, (I). \scheme
An ORTEP plot (Johnson, 1965) of the cation in (I), with the atom-numbering scheme, is shown in Fig. 1. The Co exhibits a distorted octahedral stereochemistry and the (DH)(DOH)pn ligand occupies four equatorial positions. The four equatorial N atoms are coplanar within 0.01 (4) Å, and the Co is displaced by 0.033 (1) Å from this mean plane toward the axial alkyl group. The two chemically equivalent halves of the equatorial macrocycle, with the exclusion of C6, are approximately planar. These planes have a dihedral angle of 8.5 (2)° and bend toward the axial water group. The position of the central atom of the propylene bridge appears to be determined mainly by the interaction with the axial ligands (Parker et al., 1985). Other bond lengths and angles are in agreement with those in related compounds (Zangrando, Parker, Bresciani-Pahor et al., 1987; Zangrando, Parker & Mezzetti, 1987; Parker et al., 1985).
The oxime H atom takes part in a short intramolecular hydrogen bond linking oxime O atoms O1 and O2. The H atoms of the water molecule form O—H···O hydrogen bonds with perchlorate O atoms. Details of the hydrogen bonding are in Table 2.