Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801005086/ob6033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801005086/ob6033Isup2.hkl |
CCDC reference: 165628
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- Disorder in solvent or counterion
- R factor = 0.066
- wR factor = 0.189
- Data-to-parameter ratio = 12.6
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 44.00 Perc. PLAT_601 Alert C Structure Contains Solvent Accessible VOIDS of 49.00 A 3 PLAT_731 Alert C Bond Calc 0.85(3), Rep 0.849(10) .... 3.00 s.u-Ratio O1W -H1WB 1.555 1.555 PLAT_732 Alert C Angle Calc 110(4), Rep 109.8(18) .... 2.22 s.u-Ratio H1WA -O1W -H1WB 1.555 1.555 1.555 PLAT_735 Alert C D-H Calc 0.88(8), Rep 0.87(17) .... 2.12 s.u-Ratio O2 -H2 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.849(10) .... 3.00 s.u-Ratio O1W -H1WB 1.555 1.555 PLAT_737 Alert C D...A Calc 2.439(5), Rep 2.441(12) .... 2.40 s.u-Ratio O2 -O1 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
7 Alert Level C = Please check
The title compound was synthesized as described by 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 perchlorate anion shows an orientational disorder. The positional parameters of the O atoms were refined with Cl—O constrained to 1.43 (1) Å and O···O to 2.32 (2) Å. The site-occupation factor of the O11–O14 atoms was refined using a free variable as 0.729 (11) and that of the O11'–O14' atoms as 0.271 (11). The hydroxy and aqua H atoms were located from difference Fourier maps and were refined isotropically. The positional parameters of the other H atoms were calculated geometrically and were refined using a riding model.
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 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. ORTEP drawing of (I) with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Co(C5H11)(C11H19N4O2)(H2O)]ClO4 | F(000) = 1024 |
Mr = 486.84 | Dx = 1.433 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 17.761 (4) Å | Cell parameters from 60 reflections |
b = 6.6774 (13) Å | θ = 5.3–10.0° |
c = 19.173 (4) Å | µ = 0.92 mm−1 |
β = 96.91 (2)° | T = 293 K |
V = 2257.3 (8) Å3 | Prism, red |
Z = 4 | 0.55 × 0.30 × 0.30 mm |
Bruker P4 diffractometer | 2709 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.070 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
2θ/ω scans | h = −1→21 |
Absorption correction: ψ scan (North et al., 1968) | k = −1→7 |
Tmin = 0.641, Tmax = 0.759 | l = −22→22 |
5163 measured reflections | 3 standard reflections every 97 reflections |
3956 independent reflections | intensity decay: 9.7% |
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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.189 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.1023P)2 + 2.2665P] where P = (Fo2 + 2Fc2)/3 |
3956 reflections | (Δ/σ)max < 0.001 |
313 parameters | Δρmax = 0.56 e Å−3 |
59 restraints | Δρmin = −0.79 e Å−3 |
[Co(C5H11)(C11H19N4O2)(H2O)]ClO4 | V = 2257.3 (8) Å3 |
Mr = 486.84 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 17.761 (4) Å | µ = 0.92 mm−1 |
b = 6.6774 (13) Å | T = 293 K |
c = 19.173 (4) Å | 0.55 × 0.30 × 0.30 mm |
β = 96.91 (2)° |
Bruker P4 diffractometer | 2709 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.070 |
Tmin = 0.641, Tmax = 0.759 | 3 standard reflections every 97 reflections |
5163 measured reflections | intensity decay: 9.7% |
3956 independent reflections |
R[F2 > 2σ(F2)] = 0.066 | 59 restraints |
wR(F2) = 0.189 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.56 e Å−3 |
3956 reflections | Δρmin = −0.79 e Å−3 |
313 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 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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.21442 (3) | 1.25797 (10) | 0.45904 (3) | 0.0355 (2) | |
N1 | 0.2254 (2) | 1.4165 (6) | 0.3801 (2) | 0.0406 (10) | |
N2 | 0.1520 (2) | 1.1049 (6) | 0.3910 (2) | 0.0438 (10) | |
N3 | 0.2022 (3) | 1.1065 (7) | 0.5413 (2) | 0.0475 (11) | |
N4 | 0.2745 (2) | 1.4159 (7) | 0.5252 (2) | 0.0450 (10) | |
O1 | 0.2657 (2) | 1.5843 (5) | 0.3831 (2) | 0.0514 (9) | |
O2 | 0.3087 (2) | 1.5841 (6) | 0.5088 (2) | 0.0584 (11) | |
H2 | 0.298 (4) | 1.587 (10) | 0.463 (4) | 0.070* | |
C1 | 0.1845 (4) | 1.4823 (11) | 0.2565 (3) | 0.0722 (19) | |
H1A | 0.2079 | 1.6102 | 0.2668 | 0.108* | |
H1B | 0.1326 | 1.5013 | 0.2370 | 0.108* | |
H1C | 0.2112 | 1.4125 | 0.2232 | 0.108* | |
C2 | 0.1873 (3) | 1.3629 (9) | 0.3221 (3) | 0.0460 (13) | |
C3 | 0.1449 (3) | 1.1768 (9) | 0.3289 (3) | 0.0488 (13) | |
C4 | 0.0994 (4) | 1.0879 (12) | 0.2659 (4) | 0.082 (2) | |
H4A | 0.0743 | 0.9694 | 0.2794 | 0.123* | |
H4B | 0.1324 | 1.0540 | 0.2315 | 0.123* | |
H4C | 0.0623 | 1.1832 | 0.2462 | 0.123* | |
C5 | 0.1146 (4) | 0.9197 (9) | 0.4084 (4) | 0.0638 (17) | |
H5A | 0.1487 | 0.8076 | 0.4047 | 0.077* | |
H5B | 0.0698 | 0.8987 | 0.3750 | 0.077* | |
C6 | 0.0925 (3) | 0.9277 (9) | 0.4811 (4) | 0.0653 (18) | |
H6A | 0.0592 | 0.8155 | 0.4872 | 0.078* | |
H6B | 0.0637 | 1.0495 | 0.4859 | 0.078* | |
C7 | 0.1573 (4) | 0.9222 (9) | 0.5388 (4) | 0.0680 (18) | |
H7A | 0.1378 | 0.9036 | 0.5835 | 0.082* | |
H7B | 0.1897 | 0.8089 | 0.5315 | 0.082* | |
C8 | 0.2344 (5) | 1.0920 (14) | 0.6695 (3) | 0.088 (2) | |
H8A | 0.2202 | 0.9534 | 0.6650 | 0.132* | |
H8B | 0.1981 | 1.1628 | 0.6934 | 0.132* | |
H8C | 0.2837 | 1.1030 | 0.6959 | 0.132* | |
C9 | 0.2363 (3) | 1.1800 (10) | 0.5984 (3) | 0.0534 (15) | |
C10 | 0.2786 (3) | 1.3644 (10) | 0.5899 (3) | 0.0531 (14) | |
C11 | 0.3195 (5) | 1.4819 (13) | 0.6477 (4) | 0.087 (2) | |
H11A | 0.3535 | 1.5737 | 0.6289 | 0.131* | |
H11B | 0.3479 | 1.3930 | 0.6803 | 0.131* | |
H11C | 0.2837 | 1.5553 | 0.6714 | 0.131* | |
C12 | 0.3035 (3) | 1.0888 (8) | 0.4441 (3) | 0.0451 (12) | |
H12A | 0.3198 | 1.0193 | 0.4877 | 0.054* | |
H12B | 0.2865 | 0.9877 | 0.4094 | 0.054* | |
C13 | 0.3715 (3) | 1.1902 (9) | 0.4208 (3) | 0.0572 (15) | |
H13A | 0.3900 | 1.2906 | 0.4552 | 0.069* | |
H13B | 0.3568 | 1.2577 | 0.3764 | 0.069* | |
C14 | 0.4342 (3) | 1.0432 (11) | 0.4121 (3) | 0.0620 (17) | |
H14A | 0.4495 | 0.9795 | 0.4571 | 0.074* | |
H14B | 0.4144 | 0.9397 | 0.3795 | 0.074* | |
C15 | 0.5022 (4) | 1.1325 (15) | 0.3865 (4) | 0.095 (3) | |
H15A | 0.5231 | 1.2323 | 0.4201 | 0.114* | |
H15B | 0.4865 | 1.2010 | 0.3425 | 0.114* | |
C16 | 0.5640 (4) | 0.9850 (17) | 0.3750 (5) | 0.123 (4) | |
H16A | 0.6070 | 1.0560 | 0.3616 | 0.184* | |
H16B | 0.5455 | 0.8930 | 0.3384 | 0.184* | |
H16C | 0.5787 | 0.9124 | 0.4176 | 0.184* | |
Cl1 | −0.05350 (9) | 1.4968 (3) | 0.34438 (8) | 0.0691 (5) | |
O11 | −0.0698 (6) | 1.6479 (14) | 0.3937 (5) | 0.136 (4) | 0.729 (11) |
O12 | −0.0058 (7) | 1.5779 (19) | 0.3001 (5) | 0.134 (5) | 0.729 (11) |
O13 | −0.1226 (5) | 1.422 (2) | 0.3136 (8) | 0.156 (6) | 0.729 (11) |
O14 | −0.0111 (5) | 1.3465 (14) | 0.3873 (5) | 0.127 (4) | 0.729 (11) |
O1W | 0.1210 (2) | 1.4376 (6) | 0.4753 (2) | 0.0493 (9) | |
H1WA | 0.117 (3) | 1.415 (9) | 0.5183 (8) | 0.059* | |
H1WB | 0.0781 (15) | 1.424 (9) | 0.4510 (19) | 0.059* | |
O11' | −0.0731 (18) | 1.671 (3) | 0.3023 (14) | 0.164 (12) | 0.271 (11) |
O12' | −0.0883 (15) | 1.326 (3) | 0.3105 (14) | 0.145 (13) | 0.271 (11) |
O13' | −0.0645 (19) | 1.520 (5) | 0.4148 (7) | 0.183 (11) | 0.271 (11) |
O14' | 0.0262 (6) | 1.476 (4) | 0.3418 (15) | 0.135 (10) | 0.271 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0351 (4) | 0.0337 (4) | 0.0388 (4) | 0.0032 (3) | 0.0084 (2) | 0.0021 (3) |
N1 | 0.039 (2) | 0.036 (2) | 0.048 (2) | 0.0045 (19) | 0.0108 (19) | 0.0028 (19) |
N2 | 0.033 (2) | 0.035 (2) | 0.063 (3) | 0.0005 (18) | 0.0037 (19) | −0.004 (2) |
N3 | 0.049 (3) | 0.041 (2) | 0.056 (3) | 0.012 (2) | 0.021 (2) | 0.013 (2) |
N4 | 0.043 (2) | 0.047 (3) | 0.046 (3) | 0.005 (2) | 0.0076 (19) | −0.006 (2) |
O1 | 0.051 (2) | 0.041 (2) | 0.064 (2) | −0.0085 (17) | 0.0093 (18) | 0.0100 (18) |
O2 | 0.063 (3) | 0.047 (2) | 0.065 (2) | −0.011 (2) | 0.005 (2) | −0.009 (2) |
C1 | 0.077 (4) | 0.090 (5) | 0.048 (3) | 0.004 (4) | 0.003 (3) | 0.015 (3) |
C2 | 0.042 (3) | 0.054 (3) | 0.042 (3) | 0.005 (3) | 0.003 (2) | 0.007 (3) |
C3 | 0.039 (3) | 0.056 (3) | 0.049 (3) | 0.010 (3) | −0.002 (2) | −0.010 (3) |
C4 | 0.062 (4) | 0.095 (5) | 0.083 (5) | 0.001 (4) | −0.015 (4) | −0.023 (4) |
C5 | 0.053 (3) | 0.040 (3) | 0.099 (5) | −0.006 (3) | 0.011 (3) | −0.004 (3) |
C6 | 0.047 (3) | 0.041 (3) | 0.113 (5) | 0.000 (3) | 0.033 (4) | 0.012 (3) |
C7 | 0.079 (4) | 0.050 (4) | 0.082 (4) | 0.008 (3) | 0.036 (4) | 0.020 (3) |
C8 | 0.098 (5) | 0.117 (7) | 0.053 (4) | 0.033 (5) | 0.025 (4) | 0.026 (4) |
C9 | 0.057 (3) | 0.060 (4) | 0.046 (3) | 0.023 (3) | 0.018 (3) | 0.010 (3) |
C10 | 0.051 (3) | 0.067 (4) | 0.041 (3) | 0.018 (3) | 0.003 (2) | −0.005 (3) |
C11 | 0.098 (5) | 0.108 (6) | 0.053 (4) | 0.015 (5) | −0.004 (4) | −0.016 (4) |
C12 | 0.040 (3) | 0.049 (3) | 0.046 (3) | 0.008 (2) | 0.006 (2) | −0.001 (2) |
C13 | 0.043 (3) | 0.065 (4) | 0.066 (4) | 0.008 (3) | 0.018 (3) | −0.002 (3) |
C14 | 0.042 (3) | 0.100 (5) | 0.043 (3) | 0.016 (3) | −0.002 (2) | −0.006 (3) |
C15 | 0.056 (4) | 0.135 (8) | 0.101 (6) | 0.019 (5) | 0.036 (4) | 0.007 (6) |
C16 | 0.067 (5) | 0.212 (12) | 0.093 (6) | 0.050 (7) | 0.022 (4) | −0.010 (7) |
Cl1 | 0.0502 (8) | 0.1036 (14) | 0.0546 (9) | 0.0016 (9) | 0.0114 (7) | 0.0000 (9) |
O11 | 0.194 (10) | 0.113 (8) | 0.121 (8) | 0.051 (8) | 0.097 (7) | 0.013 (6) |
O12 | 0.150 (10) | 0.179 (12) | 0.083 (6) | −0.078 (9) | 0.054 (6) | −0.015 (6) |
O13 | 0.077 (7) | 0.190 (13) | 0.180 (10) | −0.040 (7) | −0.071 (7) | 0.061 (9) |
O14 | 0.077 (6) | 0.123 (7) | 0.174 (10) | 0.014 (6) | −0.017 (6) | 0.030 (7) |
O1W | 0.045 (2) | 0.044 (2) | 0.061 (2) | 0.0123 (18) | 0.0125 (17) | 0.002 (2) |
O11' | 0.15 (2) | 0.16 (2) | 0.18 (2) | 0.06 (2) | 0.01 (2) | 0.05 (2) |
O12' | 0.10 (2) | 0.20 (3) | 0.114 (18) | −0.09 (2) | −0.049 (17) | 0.02 (2) |
O13' | 0.28 (2) | 0.16 (2) | 0.122 (19) | 0.00 (2) | 0.073 (19) | 0.008 (18) |
O14' | 0.123 (17) | 0.15 (2) | 0.14 (2) | 0.041 (16) | 0.068 (16) | −0.023 (17) |
Co1—N1 | 1.876 (4) | Cl1—O14 | 1.450 (6) |
Co1—N4 | 1.880 (4) | O2—H2 | 0.87 (7) |
Co1—N2 | 1.905 (4) | C1—H1A | 0.9600 |
Co1—N3 | 1.908 (4) | C1—H1B | 0.9600 |
Co1—C12 | 1.993 (5) | C1—H1C | 0.9600 |
Co1—O1W | 2.100 (3) | C4—H4A | 0.9600 |
N1—C2 | 1.281 (7) | C4—H4B | 0.9600 |
N1—O1 | 1.327 (5) | C4—H4C | 0.9600 |
N2—C3 | 1.276 (7) | C5—H5A | 0.9700 |
N2—C5 | 1.461 (7) | C5—H5B | 0.9700 |
N3—C9 | 1.284 (7) | C6—H6A | 0.9700 |
N3—C7 | 1.464 (8) | C6—H6B | 0.9700 |
N4—C10 | 1.280 (7) | C7—H7A | 0.9700 |
N4—O2 | 1.332 (6) | C7—H7B | 0.9700 |
C1—C2 | 1.485 (8) | C8—H8A | 0.9600 |
C2—C3 | 1.467 (8) | C8—H8B | 0.9600 |
C3—C4 | 1.492 (8) | C8—H8C | 0.9600 |
C5—C6 | 1.496 (9) | C11—H11A | 0.9600 |
C6—C7 | 1.498 (9) | C11—H11B | 0.9600 |
C8—C9 | 1.488 (8) | C11—H11C | 0.9600 |
C9—C10 | 1.462 (9) | C12—H12A | 0.9700 |
C10—C11 | 1.475 (9) | C12—H12B | 0.9700 |
C12—C13 | 1.498 (7) | C13—H13A | 0.9700 |
C13—C14 | 1.509 (8) | C13—H13B | 0.9700 |
C14—C15 | 1.482 (9) | C14—H14A | 0.9700 |
C15—C16 | 1.511 (11) | C14—H14B | 0.9700 |
Cl1—O12 | 1.380 (6) | C15—H15A | 0.9700 |
Cl1—O13 | 1.391 (7) | C15—H15B | 0.9700 |
Cl1—O13' | 1.396 (9) | C16—H16A | 0.9600 |
Cl1—O12' | 1.416 (9) | C16—H16B | 0.9600 |
Cl1—O14' | 1.430 (9) | C16—H16C | 0.9600 |
Cl1—O11 | 1.436 (7) | O1W—H1WA | 0.850 (10) |
Cl1—O11' | 1.437 (9) | O1W—H1WB | 0.849 (10) |
N1—Co1—N4 | 97.0 (2) | O11—Cl1—O14 | 104.1 (6) |
N1—Co1—N2 | 81.86 (19) | O11'—Cl1—O14 | 162.7 (13) |
N4—Co1—N2 | 178.32 (19) | N4—O2—H2 | 102 (5) |
N1—Co1—N3 | 177.65 (18) | C2—C1—H1A | 109.5 |
N4—Co1—N3 | 81.4 (2) | C2—C1—H1B | 109.5 |
N2—Co1—N3 | 99.6 (2) | H1A—C1—H1B | 109.5 |
N1—Co1—C12 | 92.4 (2) | C2—C1—H1C | 109.5 |
N4—Co1—C12 | 91.1 (2) | H1A—C1—H1C | 109.5 |
N2—Co1—C12 | 90.2 (2) | H1B—C1—H1C | 109.5 |
N3—Co1—C12 | 89.4 (2) | C3—C4—H4A | 109.5 |
N1—Co1—O1W | 87.62 (16) | C3—C4—H4B | 109.5 |
N4—Co1—O1W | 88.50 (17) | H4A—C4—H4B | 109.5 |
N2—Co1—O1W | 90.19 (17) | C3—C4—H4C | 109.5 |
N3—Co1—O1W | 90.56 (17) | H4A—C4—H4C | 109.5 |
C12—Co1—O1W | 179.6 (2) | H4B—C4—H4C | 109.5 |
C2—N1—O1 | 119.9 (4) | N2—C5—H5A | 109.4 |
C2—N1—Co1 | 116.6 (4) | C6—C5—H5A | 109.4 |
O1—N1—Co1 | 123.3 (3) | N2—C5—H5B | 109.4 |
C3—N2—C5 | 122.3 (5) | C6—C5—H5B | 109.4 |
C3—N2—Co1 | 114.9 (4) | H5A—C5—H5B | 108.0 |
C5—N2—Co1 | 122.7 (4) | C5—C6—H6A | 108.5 |
C9—N3—C7 | 123.2 (5) | C7—C6—H6A | 108.5 |
C9—N3—Co1 | 114.5 (4) | C5—C6—H6B | 108.5 |
C7—N3—Co1 | 122.3 (4) | C7—C6—H6B | 108.5 |
C10—N4—O2 | 118.7 (5) | H6A—C6—H6B | 107.5 |
C10—N4—Co1 | 117.7 (4) | N3—C7—H7A | 109.3 |
O2—N4—Co1 | 123.5 (3) | C6—C7—H7A | 109.3 |
N1—C2—C3 | 112.5 (5) | N3—C7—H7B | 109.3 |
N1—C2—C1 | 123.1 (5) | C6—C7—H7B | 109.3 |
C3—C2—C1 | 124.4 (5) | H7A—C7—H7B | 107.9 |
N2—C3—C2 | 114.0 (5) | C9—C8—H8A | 109.5 |
N2—C3—C4 | 126.1 (6) | C9—C8—H8B | 109.5 |
C2—C3—C4 | 119.9 (6) | H8A—C8—H8B | 109.5 |
N2—C5—C6 | 111.2 (5) | C9—C8—H8C | 109.5 |
C5—C6—C7 | 115.0 (5) | H8A—C8—H8C | 109.5 |
N3—C7—C6 | 111.8 (5) | H8B—C8—H8C | 109.5 |
N3—C9—C10 | 115.0 (5) | C10—C11—H11A | 109.5 |
N3—C9—C8 | 124.8 (7) | C10—C11—H11B | 109.5 |
C10—C9—C8 | 120.3 (6) | H11A—C11—H11B | 109.5 |
N4—C10—C9 | 111.4 (5) | C10—C11—H11C | 109.5 |
N4—C10—C11 | 123.4 (6) | H11A—C11—H11C | 109.5 |
C9—C10—C11 | 125.2 (6) | H11B—C11—H11C | 109.5 |
C13—C12—Co1 | 118.0 (4) | C13—C12—H12A | 107.8 |
C12—C13—C14 | 111.8 (5) | Co1—C12—H12A | 107.8 |
C15—C14—C13 | 114.6 (6) | C13—C12—H12B | 107.8 |
C14—C15—C16 | 114.9 (8) | Co1—C12—H12B | 107.8 |
O12—Cl1—O13 | 117.2 (7) | H12A—C12—H12B | 107.2 |
O12—Cl1—O13' | 136.0 (14) | C12—C13—H13A | 109.3 |
O13—Cl1—O13' | 103.3 (16) | C14—C13—H13A | 109.3 |
O12—Cl1—O12' | 107.5 (13) | C12—C13—H13B | 109.3 |
O13—Cl1—O12' | 36.9 (12) | C14—C13—H13B | 109.3 |
O13'—Cl1—O12' | 115.3 (13) | H13A—C13—H13B | 107.9 |
O12—Cl1—O14' | 48.2 (10) | C15—C14—H14A | 108.6 |
O13—Cl1—O14' | 141.1 (12) | C13—C14—H14A | 108.6 |
O13'—Cl1—O14' | 107.4 (13) | C15—C14—H14B | 108.6 |
O12'—Cl1—O14' | 106.5 (12) | C13—C14—H14B | 108.6 |
O12—Cl1—O11 | 108.4 (6) | H14A—C14—H14B | 107.6 |
O13—Cl1—O11 | 107.2 (7) | C14—C15—H15A | 108.5 |
O13'—Cl1—O11 | 39.0 (12) | C16—C15—H15A | 108.5 |
O12'—Cl1—O11 | 139.1 (13) | C14—C15—H15B | 108.5 |
O14'—Cl1—O11 | 111.7 (11) | C16—C15—H15B | 108.5 |
O12—Cl1—O11' | 57.4 (11) | H15A—C15—H15B | 107.5 |
O13—Cl1—O11' | 85.0 (13) | C15—C16—H16A | 109.5 |
O13'—Cl1—O11' | 113.7 (13) | C15—C16—H16B | 109.5 |
O12'—Cl1—O11' | 109.4 (12) | H16A—C16—H16B | 109.5 |
O14'—Cl1—O11' | 103.5 (12) | C15—C16—H16C | 109.5 |
O11—Cl1—O11' | 75.3 (12) | H16A—C16—H16C | 109.5 |
O12—Cl1—O14 | 107.8 (7) | H16B—C16—H16C | 109.5 |
O13—Cl1—O14 | 111.2 (6) | Co1—O1W—H1WA | 102 (4) |
O13'—Cl1—O14 | 69.5 (13) | Co1—O1W—H1WB | 122 (4) |
O12'—Cl1—O14 | 82.6 (12) | H1WA—O1W—H1WB | 109.8 (18) |
O14'—Cl1—O14 | 60.2 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O11i | 0.85 (1) | 2.01 (2) | 2.830 (13) | 160 (4) |
O2—H2···O1 | 0.87 (17) | 1.57 (7) | 2.441 (12) | 170 (6) |
O1W—H1WB···O14 | 0.85 (1) | 1.95 (18) | 2.788 (14) | 168 (6) |
Symmetry code: (i) −x, −y+3, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C5H11)(C11H19N4O2)(H2O)]ClO4 |
Mr | 486.84 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 17.761 (4), 6.6774 (13), 19.173 (4) |
β (°) | 96.91 (2) |
V (Å3) | 2257.3 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.92 |
Crystal size (mm) | 0.55 × 0.30 × 0.30 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.641, 0.759 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5163, 3956, 2709 |
Rint | 0.070 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.066, 0.189, 1.04 |
No. of reflections | 3956 |
No. of parameters | 313 |
No. of restraints | 59 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.56, −0.79 |
Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Siemens, 1995), SHELXTL.
Co1—N1 | 1.876 (4) | N2—C3 | 1.276 (7) |
Co1—N4 | 1.880 (4) | N2—C5 | 1.461 (7) |
Co1—N2 | 1.905 (4) | N3—C9 | 1.284 (7) |
Co1—N3 | 1.908 (4) | N3—C7 | 1.464 (8) |
Co1—C12 | 1.993 (5) | N4—C10 | 1.280 (7) |
Co1—O1W | 2.100 (3) | N4—O2 | 1.332 (6) |
N1—C2 | 1.281 (7) | C5—C6 | 1.496 (9) |
N1—O1 | 1.327 (5) | C6—C7 | 1.498 (9) |
N1—Co1—N4 | 97.0 (2) | N3—Co1—C12 | 89.4 (2) |
N1—Co1—N2 | 81.86 (19) | N1—Co1—O1W | 87.62 (16) |
N4—Co1—N2 | 178.32 (19) | N4—Co1—O1W | 88.50 (17) |
N1—Co1—N3 | 177.65 (18) | N2—Co1—O1W | 90.19 (17) |
N4—Co1—N3 | 81.4 (2) | N3—Co1—O1W | 90.56 (17) |
N2—Co1—N3 | 99.6 (2) | C12—Co1—O1W | 179.6 (2) |
N1—Co1—C12 | 92.4 (2) | N2—C5—C6 | 111.2 (5) |
N4—Co1—C12 | 91.1 (2) | C5—C6—C7 | 115.0 (5) |
N2—Co1—C12 | 90.2 (2) | N3—C7—C6 | 111.8 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O11i | 0.850 (10) | 2.01 (2) | 2.830 (13) | 160 (4) |
O2—H2···O1 | 0.87 (17) | 1.57 (7) | 2.441 (12) | 170 (6) |
O1W—H1WB···O14 | 0.849 (10) | 1.95 (18) | 2.788 (14) | 168 (6) |
Symmetry code: (i) −x, −y+3, −z+1. |
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As important coenzyme B12 models, several Costa-type organocobalt complexes, [LCo(DO-DOH-pn)R]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- or ClO4- etc.), have been reported (Finke et al., 1983). But only a few structures are available, especially with aqua as the axial ligand (Randaccio et al., 1989). In this report, we describe the structure of the title compound, (I), with L = H2O and R = pentyl.
The Co atom has a distorted octahedral coordination with the R and H2O ligands in axial positions (Fig. 1). The four equatorial N atoms of the DO-DOH-pn ligand are coplanar within 0.004 Å, and the Co atom is displaced by 0.025 (6) Å from this mean plane towards the axial alkyl group. The two chemically equivalent halves of the equatorial macrocycle, with the exclusion of C6, have a dihedral angle of 6.3 (7)° and bend toward the aqua ligand. Compared with the complex having R = hexyl, which we have previously reported (Xiang et al., 2000), the Co—C bond length is slightly shorter. The Co—C bond lengths are 1.993 (5) and 2.022 (5) Å for R = pentyl and hexyl, respectively. Other bond lengths and angles agree with those in related compounds (Zagrando et al., 1987; Parker et al., 1985; Marzilli et al., 1985).