The crystal structures of [18]aneN6H2K[Co(CN)6].4H2O [potassium dihydrogen hexacyanocobaltate-1,4,7,10,13,16-hexaazacyclooctadecane-water (1/1/4)], [16]aneN4H2K[Co(CN)6] [potassium dihydrogen hexacyanocobaltate-1,5,9,13-tetraazacyclohexadecane (1/1)] and [12]aneN4H3[Co(CN)6].2H2O [trihydrogen hexacyanocobaltate-1,4,7,10-tetraazacyclododecane-water (1/1/2)] have been determined. For these supercomplexes, the [Co(CN)6]3- binding with protonated polyammonium macrocycles is dominant in the binding competition between K+ and [Co(CN)6]3-. It is suggested that the binding of [Co(CN)6]3- with protonated polyammonium macrocycles is independent of the cavity size of the macrocycle, whereas that of K+ is size-match selective. For [18]aneN6H2K[Co(CN)6].4H2O, the formation of a two-dimensional lamella may be derived from a chain-like arrangement of four-, five- and eight-membered rings in the network through the mutual balance between electrostatic and hydrogen-bonding interactions. [16]aneN4H2K[Co(CN)6] is a novel example demonstrating the anchoring of cobalticyanide through hydrogen-bonding interactions inside a zeolite-type cavity in the three-dimensional network formed by K+ and the macrocycles through Coulombic interactions. Also, a three-dimensional network was formed mainly through hydrogen-bonding interactions between [Co(CN)6]3-, protonated macrocycles and water molecules in [12]aneN4H3[Co(CN)6].2H2O.
Supporting information
| Crystallographic Information File (CIF) Contains datablocks 1, 2, 3, global |
| Structure factor file (CIF format) Contains datablock 1 |
| Structure factor file (CIF format) Contains datablock 2 |
| Structure factor file (CIF format) Contains datablock 3 |
CCDC references: 131771; 131772; 131773
Data collection: Siemens XSCANS ver. 2.10b for (1), (3); MSC/AFC Diffractometer Control for (2). Cell refinement: Siemens XSCANS ver. 2.10b for (1), (3); MSC/AFC Diffractometer Control for (2). Data reduction: Siemens XSCANS ver. 2.10b for (1), (3); MSC/AFC Diffractometer Control for (2). For all compounds, program(s) used to solve structure: SHELXS86 (Sheldrick, 1990). Program(s) used to refine structure: SHELXL93 (Sheldrick, 1993) for (1); SHELXTL-PC (Sheldrick, 1990) for (2), (3). For all compounds, molecular graphics: SHELXTL-PC (Sheldrick, 1990).
Crystal data top
KH2[Co(CN)6](C12H30N6).4(H2O) | Z = 2 |
Mr = 586.65 | F(000) = 620 |
Triclinic, P1 | Dx = 1.324 Mg m−3 |
a = 10.125 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.133 (2) Å | Cell parameters from 25 reflections |
c = 15.014 (2) Å | θ = 5–15° |
α = 73.78 (1)° | µ = 0.77 mm−1 |
β = 71.68 (1)° | T = 293 K |
γ = 68.87 (2)° | Plate, colorless |
V = 1472.0 (6) Å3 | 0.30 × 0.30 × 0.10 mm |
Data collection top
Siemens P4 diffractometer | 3032 reflections with > 4σ(F) |
Radiation source: fine-focus sealed tube | Rint = 0.034 |
Graphite monochromator | θmax = 24.0°, θmin = 1.5° |
ω scans | h = 0→11 |
Absorption correction: empirical | k = −11→12 |
Tmin = 0.833, Tmax = 0.946 | l = −16→17 |
4910 measured reflections | 3 standard reflections every 100 reflections |
4617 independent reflections | intensity decay: −1.3% |
Refinement top
Refinement on F | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.059 | H-atom parameters not defined? |
wR(F2) = 0.075 | Calculated w = 1/[σ2(Fo) + 0.0005Fo2] |
3023 reflections | (Δ/σ)max = 0.001 |
325 parameters | Δρmax = 0.36 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
Primary atom site location: structure-invariant direct methods | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.2607 (1) | 0.2764 (1) | 0.2894 (1) | 0.025 (1) | |
C1 | 0.1670 (7) | 0.1451 (6) | 0.3620 (4) | 0.035 (3) | |
N1 | 0.1076 (6) | 0.0702 (5) | 0.4054 (4) | 0.048 (3) | |
C2 | 0.3494 (7) | 0.4107 (6) | 0.2223 (4) | 0.038 (3) | |
N2 | 0.3998 (7) | 0.4926 (6) | 0.1854 (4) | 0.061 (3) | |
C3 | 0.0782 (7) | 0.4080 (6) | 0.3063 (4) | 0.036 (3) | |
N3 | −0.0325 (7) | 0.4876 (6) | 0.3142 (4) | 0.054 (3) | |
C4 | 0.2940 (7) | 0.2896 (6) | 0.4040 (5) | 0.037 (3) | |
N4 | 0.3185 (7) | 0.2939 (6) | 0.4724 (4) | 0.054 (3) | |
C5 | 0.4467 (7) | 0.1490 (6) | 0.2665 (4) | 0.035 (3) | |
N5 | 0.5575 (6) | 0.0730 (6) | 0.2514 (4) | 0.050 (3) | |
C6 | 0.2325 (7) | 0.2547 (6) | 0.1756 (5) | 0.038 (3) | |
N6 | 0.2167 (7) | 0.2382 (6) | 0.1083 (4) | 0.061 (3) | |
K1 | −0.0057 (2) | −0.0181 (2) | 0.1273 (1) | 0.056 (1) | |
N11 | −0.2878 (5) | 0.1178 (5) | 0.0404 (4) | 0.039 (2) | |
H11M | −0.1964 | 0.1003 | 0.0034 | 0.050* | |
H11N | −0.2855 | 0.0906 | 0.1024 | 0.050* | 0.5 |
N12 | −0.1567 (6) | 0.3214 (5) | −0.0442 (4) | 0.045 (3) | |
H12M | −0.1919 | 0.3493 | −0.0969 | 0.050* | |
N13 | 0.1399 (5) | 0.1870 (5) | −0.0389 (3) | 0.036 (2) | |
H13M | 0.1504 | 0.1848 | 0.0201 | 0.050* | |
H13N | 0.0752 | 0.1494 | −0.0491 | 0.050* | 0.5 |
C11 | −0.3514 (7) | 0.0193 (6) | 0.0349 (5) | 0.043 (3) | |
H11A | −0.3322 | 0.0144 | −0.0310 | 0.060* | |
H11B | −0.4552 | 0.0487 | 0.0589 | 0.060* | |
C12 | −0.3747 (7) | 0.2553 (6) | 0.0151 (5) | 0.047 (3) | |
H12A | −0.4701 | 0.2709 | 0.0573 | 0.060* | |
H12B | −0.3850 | 0.2713 | −0.0490 | 0.060* | |
C13 | −0.2992 (8) | 0.3453 (7) | 0.0214 (5) | 0.050 (3) | |
H13A | −0.3567 | 0.4351 | 0.0073 | 0.060* | |
H13B | −0.2857 | 0.3278 | 0.0848 | 0.060* | |
C14 | −0.0642 (7) | 0.3888 (6) | −0.0356 (5) | 0.048 (3) | |
H14A | −0.0682 | 0.3776 | 0.0309 | 0.060* | |
H14B | −0.0962 | 0.4809 | −0.0609 | 0.060* | |
C15 | 0.0901 (8) | 0.3273 (6) | −0.0866 (5) | 0.046 (3) | |
H15A | 0.0925 | 0.3316 | −0.1518 | 0.060* | |
H15B | 0.1538 | 0.3732 | −0.0859 | 0.060* | |
C16 | 0.2899 (7) | 0.1173 (6) | −0.0884 (4) | 0.041 (3) | |
H16A | 0.3534 | 0.1688 | −0.0984 | 0.060* | |
H16B | 0.2868 | 0.1098 | −0.1498 | 0.060* | |
N21 | 0.1576 (6) | −0.3043 (5) | 0.4705 (4) | 0.050 (3) | |
H21M | 0.1216 | −0.3646 | 0.5156 | 0.060* | |
N22 | −0.0101 (7) | −0.1100 (5) | 0.3476 (4) | 0.049 (3) | |
H22M | 0.0417 | −0.0901 | 0.3773 | 0.060* | |
N23 | −0.2200 (6) | 0.1586 (5) | 0.4304 (4) | 0.043 (3) | |
H23M | −0.1322 | 0.1403 | 0.4422 | 0.050* | |
H23N | −0.3041 | 0.1493 | 0.4709 | 0.050* | |
C21 | 0.2979 (8) | −0.3494 (7) | 0.4924 (6) | 0.057 (4) | |
H21A | 0.3355 | −0.4431 | 0.5000 | 0.080* | |
H21B | 0.3640 | −0.3122 | 0.4402 | 0.080* | |
C22 | 0.1608 (9) | −0.3290 (7) | 0.3774 (5) | 0.061 (4) | |
H22A | 0.2365 | −0.3001 | 0.3285 | 0.080* | |
H22B | 0.1804 | −0.4209 | 0.3806 | 0.080* | |
C23 | 0.0202 (8) | −0.2534 (6) | 0.3533 (5) | 0.054 (4) | |
H23A | −0.0551 | −0.2829 | 0.4022 | 0.080* | |
H23B | 0.0186 | −0.2674 | 0.2934 | 0.080* | |
C24 | −0.1668 (8) | −0.0391 (7) | 0.3622 (5) | 0.050 (4) | |
H24A | −0.2034 | −0.0627 | 0.3199 | 0.080* | |
H24B | −0.2166 | −0.0667 | 0.4265 | 0.080* | |
C25 | −0.2009 (9) | 0.1085 (7) | 0.3438 (5) | 0.052 (4) | |
H25A | −0.2880 | 0.1499 | 0.3206 | 0.080* | |
H25B | −0.1218 | 0.1320 | 0.2951 | 0.080* | |
C26 | −0.2851 (8) | 0.3060 (7) | 0.4179 (5) | 0.055 (4) | |
H26A | −0.3797 | 0.3314 | 0.4053 | 0.080* | |
H26B | −0.2242 | 0.3473 | 0.3646 | 0.080* | |
O1W | 0.5410 (6) | 0.0953 (7) | 0.5561 (4) | 0.109 (4) | |
H1WA | 0.4748 | 0.1553 | 0.5318 | 0.100* | |
H1WB | 0.5514 | 0.0486 | 0.5168 | 0.100* | |
O2W | 0.5361 (7) | 0.6723 (7) | 0.2006 (5) | 0.115 (5) | |
H2WA | 0.4972 | 0.6191 | 0.1956 | 0.120* | |
H2WB | 0.4752 | 0.7100 | 0.2456 | 0.120* | |
O3W | −0.3176 (6) | 0.6593 (6) | 0.3319 (4) | 0.097 (4) | |
H3WA | −0.2313 | 0.6072 | 0.3261 | 0.100* | |
H3WB | −0.3374 | 0.6901 | 0.3819 | 0.100* | |
O4W | 0.3133 (9) | 0.9111 (7) | 0.2125 (6) | 0.142 (6) | |
H4WA | 0.2233 | 0.9258 | 0.2404 | 0.150* | |
H4WB | 0.3860 | 0.8558 | 0.2328 | 0.150* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.026 (1) | 0.026 (1) | 0.023 (1) | −0.004 (1) | −0.005 (1) | −0.010 (1) |
C1 | 0.028 (4) | 0.034 (4) | 0.041 (4) | −0.007 (3) | −0.014 (3) | −0.003 (3) |
N1 | 0.045 (4) | 0.042 (3) | 0.062 (4) | 0.001 (3) | −0.013 (3) | −0.027 (3) |
C2 | 0.045 (4) | 0.040 (4) | 0.030 (4) | −0.009 (3) | −0.003 (3) | −0.017 (4) |
N2 | 0.072 (5) | 0.060 (4) | 0.046 (4) | −0.03 (3) | 0.003 (3) | −0.036 (4) |
C3 | 0.038 (4) | 0.030 (4) | 0.043 (4) | −0.004 (3) | −0.009 (3) | −0.017 (3) |
N3 | 0.045 (4) | 0.044 (4) | 0.067 (4) | −0.010 (3) | −0.016 (3) | −0.004 (3) |
C4 | 0.036 (4) | 0.034 (4) | 0.040 (4) | −0.006 (3) | −0.005 (3) | −0.013 (3) |
N4 | 0.061 (4) | 0.068 (4) | 0.036 (4) | −0.016 (3) | −0.013 (3) | −0.017 (3) |
C5 | 0.042 (4) | 0.042 (4) | 0.024 (3) | −0.006 (3) | −0.010 (3) | −0.016 (4) |
N5 | 0.035 (4) | 0.060 (4) | 0.048 (4) | −0.015 (3) | −0.016 (3) | 0.004 (3) |
C6 | 0.040 (4) | 0.040 (4) | 0.036 (4) | −0.005 (3) | −0.014 (3) | −0.009 (3) |
N6 | 0.086 (5) | 0.060 (4) | 0.051 (4) | −0.012 (3) | −0.033 (4) | −0.022 (4) |
K1 | 0.059 (1) | 0.069 (1) | 0.040 (1) | −0.007 (1) | −0.008 (1) | −0.024 (1) |
N11 | 0.031 (3) | 0.046 (3) | 0.039 (3) | −0.003 (3) | −0.010 (2) | −0.012 (3) |
N12 | 0.046 (4) | 0.042 (3) | 0.045 (3) | −0.008 (3) | −0.012 (3) | −0.010 (3) |
N13 | 0.040 (3) | 0.037 (3) | 0.038 (3) | −0.006 (2) | −0.011 (3) | −0.019 (3) |
C11 | 0.029 (4) | 0.053 (4) | 0.046 (4) | −0.011 (3) | −0.007 (3) | −0.012 (3) |
C12 | 0.032 (4) | 0.039 (4) | 0.060 (5) | −0.006 (3) | −0.008 (3) | −0.004 (3) |
C13 | 0.053 (5) | 0.040 (4) | 0.046 (4) | −0.013 (3) | −0.003 (4) | −0.006 (4) |
C14 | 0.053 (5) | 0.028 (4) | 0.066 (5) | −0.006 (3) | −0.019 (4) | −0.014 (3) |
C15 | 0.058 (5) | 0.039 (4) | 0.044 (4) | 0.000 (3) | −0.011 (4) | −0.025 (4) |
C16 | 0.036 (4) | 0.052 (4) | 0.039 (4) | −0.012 (3) | −0.001 (3) | −0.023 (3) |
N21 | 0.055 (4) | 0.046 (3) | 0.055 (4) | −0.015 (3) | −0.010 (3) | −0.021 (3) |
N22 | 0.065 (4) | 0.040 (3) | 0.058 (4) | −0.008 (3) | −0.029 (3) | −0.023 (3) |
N23 | 0.036 (3) | 0.052 (4) | 0.047 (3) | −0.004 (3) | −0.017 (3) | −0.018 (3) |
C21 | 0.048 (5) | 0.048 (4) | 0.077 (6) | −0.023 (4) | −0.009 (4) | −0.012 (4) |
C22 | 0.077 (6) | 0.048 (5) | 0.063 (5) | −0.027 (4) | −0.005 (4) | −0.021 (4) |
C23 | 0.073 (6) | 0.046 (4) | 0.053 (5) | −0.012 (4) | −0.022 (4) | −0.022 (4) |
C24 | 0.072 (5) | 0.054 (5) | 0.039 (4) | −0.03 (3) | −0.021 (4) | −0.031 (4) |
C25 | 0.076 (5) | 0.061 (5) | 0.036 (4) | −0.003 (3) | −0.025 (4) | −0.034 (4) |
C26 | 0.053 (5) | 0.044 (4) | 0.066 (5) | 0.001 (4) | −0.020 (4) | −0.016 (4) |
O1W | 0.063 (4) | 0.129 (6) | 0.105 (5) | 0.050 (4) | −0.033 (4) | −0.036 (4) |
O2W | 0.116 (6) | 0.113 (6) | 0.141 (6) | 0.004 (5) | −0.033 (5) | −0.083 (5) |
O3W | 0.069 (4) | 0.114 (5) | 0.089 (4) | −0.046 (4) | −0.021 (4) | 0.016 (4) |
O4W | 0.153 (8) | 0.115 (6) | 0.164 (8) | −0.020 (6) | −0.063 (6) | −0.029 (6) |
Geometric parameters (Å, º) top
Co1—C1 | 1.920 (7) | N11—K1i | 3.298 (5) |
Co1—C2 | 1.901 (7) | N12—C13 | 1.449 (8) |
Co1—C3 | 1.894 (6) | N12—C14 | 1.447 (11) |
Co1—C4 | 1.909 (8) | N13—C15 | 1.496 (7) |
Co1—C5 | 1.902 (6) | N13—C16 | 1.492 (7) |
Co1—C6 | 1.909 (8) | N13—K1i | 3.393 (7) |
C1—N1 | 1.137 (9) | C11—C16i | 1.514 (8) |
C2—N2 | 1.129 (10) | C12—C13 | 1.500 (13) |
C3—N3 | 1.147 (8) | C14—C15 | 1.505 (9) |
C4—N4 | 1.146 (11) | C16—C11i | 1.514 (8) |
C5—N5 | 1.135 (8) | N21—C21 | 1.437 (11) |
C6—N6 | 1.143 (11) | N21—C22 | 1.486 (11) |
K1—N11 | 3.205 (6) | N22—C23 | 1.496 (9) |
K1—N13 | 3.247 (5) | N22—C24 | 1.471 (9) |
K1—N22 | 3.168 (6) | N23—C25 | 1.486 (10) |
K1—C24 | 3.369 (7) | N23—C26 | 1.513 (8) |
K1—K1i | 3.699 (4) | C21—C26ii | 1.508 (13) |
K1—N11i | 3.298 (5) | C22—C23 | 1.469 (11) |
K1—N13i | 3.393 (7) | C24—C25 | 1.513 (10) |
N11—C11 | 1.489 (11) | C26—C21ii | 1.508 (13) |
N11—C12 | 1.475 (7) | | |
| | | |
N22···N1 | 3.089 (9) | N23···N1 | 3.030 (9) |
O2W···N2 | 2.898 (9) | O3W···N3 | 2.807 (9) |
O1W···N4 | 2.860 (9) | N11iii···N5 | 3.049 (9) |
N13···N6 | 2.814 (9) | O1W···N23iii | 2.745 (9) |
O2W···O4W | 2.807 (9) | O2W···O3Wiii | 2.761 (9) |
| | | |
C1—Co1—C2 | 177.3 (3) | N13—K1—N13i | 112.3 (1) |
C1—Co1—C3 | 90.1 (3) | N22—K1—N13i | 115.5 (2) |
C2—Co1—C3 | 88.4 (3) | C24—K1—N13i | 107.3 (2) |
C1—Co1—C4 | 89.1 (3) | K1i—K1—N13i | 54.3 (1) |
C2—Co1—C4 | 88.8 (3) | N11i—K1—N13i | 82.4 (1) |
C3—Co1—C4 | 92.3 (3) | K1—N11—C11 | 111.8 (3) |
C1—Co1—C5 | 92.2 (3) | K1—N11—C12 | 133.5 (5) |
C2—Co1—C5 | 89.4 (3) | C11—N11—C12 | 114.4 (6) |
C3—Co1—C5 | 177.3 (2) | K1—N11—K1i | 69.3 (1) |
C4—Co1—C5 | 89.2 (3) | C11—N11—K1i | 92.1 (3) |
C1—Co1—C6 | 89.6 (3) | C12—N11—K1i | 114.0 (3) |
C2—Co1—C6 | 92.6 (3) | C13—N12—C14 | 114.7 (6) |
C3—Co1—C6 | 90.0 (3) | K1—N13—C15 | 136.8 (3) |
C4—Co1—C6 | 177.3 (2) | K1—N13—C16 | 110.4 (3) |
C5—Co1—C6 | 88.5 (3) | C15—N13—C16 | 112.2 (4) |
Co1—C1—N1 | 177.9 (5) | K1—N13—K1i | 67.7 (1) |
Co1—C2—N2 | 177.4 (6) | C15—N13—K1i | 106.2 (5) |
Co1—C3—N3 | 178.1 (7) | C16—N13—K1i | 88.9 (4) |
Co1—C4—N4 | 177.5 (5) | N11—C11—C16i | 114.0 (6) |
Co1—C5—N5 | 178.9 (6) | N11—C12—C13 | 109.7 (6) |
Co1—C6—N6 | 178.2 (6) | N12—C13—C12 | 109.1 (6) |
N11—K1—N13 | 86.1 (1) | N12—C14—C15 | 108.6 (6) |
N11—K1—N22 | 125.4 (1) | N13—C15—C14 | 109.0 (5) |
N13—K1—N22 | 131.7 (2) | N13—C16—C11i | 113.5 (5) |
N11—K1—C24 | 99.9 (2) | C21—N21—C22 | 114.1 (6) |
N13—K1—C24 | 136.1 (2) | K1—N22—C23 | 97.7 (4) |
N22—K1—C24 | 25.8 (2) | K1—N22—C24 | 84.8 (4) |
N11—K1—K1i | 56.5 (1) | C23—N22—C24 | 112.1 (6) |
N13—K1—K1i | 58.0 (1) | C25—N23—C26 | 112.5 (5) |
N22—K1—K1i | 168.2 (1) | N21—C21—C26i | 109.7 (6) |
C24—K1—K1i | 154.8 (2) | N21—C22—C23 | 108.7 (6) |
N11—K1—N11i | 110.7 (1) | N22—C23—C22 | 111.0 (8) |
N13—K1—N11i | 58.1 (1) | K1—C24—N22 | 69.5 (3) |
N22—K1—N11i | 122.3 (1) | K1—C24—C25 | 86.2 (3) |
C24—K1—N11i | 147.9 (2) | N22—C24—C25 | 113.9 (7) |
K1B—K1—N11i | 54.2 (1) | N23—C25—C24 | 112.7 (5) |
N11—K1—N13i | 57.6 (1) | N23—C26—C21i | 109.3 (6) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y, −z+1; (iii) x+1, y, z. |
Crystal data top
KH2[Co(CN)6](C12H28N4) | F(000) = 1016 |
Mr = 484.55 | Dx = 1.363 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 10.675 (2) Å | θ = 5–15° |
b = 10.516 (2) Å | µ = 0.93 mm−1 |
c = 21.051 (4) Å | T = 293 K |
β = 91.89 (3)° | Block, yellow |
V = 2361.9 (8) Å3 | 0.35 × 0.30 × 0.22 mm |
Z = 4 | |
Data collection top
Rigaku AFC7R diffractometer | 3133 reflections with > 4σ(F) |
Radiation source: Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA | Rint = 0.021 |
Graphite monochromator | θmax = 27.5°, θmin = 1.9° |
ω scans | h = 0→13 |
Absorption correction: empirical | k = 0→13 |
Tmin = 0.942, Tmax = 1.000 | l = −27→27 |
5713 measured reflections | 3 standard reflections every 150 reflections |
5425 independent reflections | intensity decay: −1.7% |
Refinement top
Refinement on F | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.049 | H-atom parameters not defined? |
wR(F2) = 0.063 | Calculated w = 1/[σ2(Fo) + 0.0002Fo2] |
3133 reflections | (Δ/σ)max = 0.082 |
272 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
Primary atom site location: structure-invariant direct methods | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
K1 | 0.1883 (1) | 0.4827 (1) | −0.1228 (1) | 0.050 (1) | |
Co1 | 0.2773 (1) | 0.7967 (1) | 0.1154 (1) | 0.024 (1) | |
C1 | 0.2340 (3) | 0.6309 (3) | 0.0861 (2) | 0.034 (1) | |
N1 | 0.2133 (3) | 0.5307 (3) | 0.0676 (2) | 0.054 (1) | |
C2 | 0.2784 (3) | 0.7396 (3) | 0.2007 (2) | 0.030 (1) | |
N2 | 0.2797 (3) | 0.7090 (3) | 0.2528 (2) | 0.043 (1) | |
C3 | 0.3258 (3) | 0.9590 (3) | 0.1457 (2) | 0.031 (1) | |
N3 | 0.3537 (3) | 1.0568 (3) | 0.1662 (2) | 0.050 (1) | |
C4 | 0.2689 (3) | 0.8551 (3) | 0.0294 (2) | 0.032 (1) | |
N4 | 0.2573 (3) | 0.8862 (3) | −0.0228 (2) | 0.043 (1) | |
C5 | 0.4495 (3) | 0.7521 (3) | 0.1106 (2) | 0.032 (1) | |
N5 | 0.5526 (3) | 0.7239 (3) | 0.1106 (2) | 0.050 (1) | |
C6 | 0.1073 (3) | 0.8442 (3) | 0.1248 (2) | 0.031 (1) | |
N6 | 0.0073 (3) | 0.8767 (3) | 0.1333 (2) | 0.039 (1) | |
N7 | 0.2863 (3) | 0.3083 (3) | −0.0036 (2) | 0.031 (1) | |
H(7) | 0.2496 | 0.3735 | 0.0163 | 0.050* | |
H(7N) | 0.3238 | 0.3241 | −0.0405 | 0.050* | 0.5 |
N8 | −0.0723 (3) | 0.2521 (3) | 0.1003 (2) | 0.039 (1) | |
H(8) | −0.1264 | 0.1966 | 0.0818 | 0.050* | |
H(8N) | −0.1253 | 0.3173 | 0.1060 | 0.050* | 0.5 |
N9 | 0.1996 (3) | 0.2945 (3) | 0.2989 (2) | 0.037 (1) | |
H(9) | 0.2369 | 0.2500 | 0.3308 | 0.050* | |
H(9N) | 0.1315 | 0.3148 | 0.3208 | 0.050* | 0.5 |
N10 | 0.5733 (3) | 0.3938 (3) | 0.1733 (2) | 0.039 (1) | |
H(10) | 0.6145 | 0.4637 | 0.1608 | 0.050* | |
H(10N) | 0.6226 | 0.3490 | 0.2006 | 0.050* | 0.5 |
C7 | 0.1846 (3) | 0.2164 (3) | −0.0234 (2) | 0.035 (1) | |
H(7A) | 0.2233 | 0.1414 | −0.0399 | 0.100* | |
H(7B) | 0.1345 | 0.2538 | −0.0572 | 0.100* | |
C8 | 0.0981 (3) | 0.1784 (3) | 0.0293 (2) | 0.034 (1) | |
H(8A) | 0.1481 | 0.1482 | 0.0649 | 0.100* | |
H(8B) | 0.0441 | 0.1105 | 0.0151 | 0.100* | |
C9 | 0.0189 (3) | 0.2885 (3) | 0.0505 (2) | 0.037 (1) | |
H(9A) | 0.0730 | 0.3539 | 0.0675 | 0.100* | |
H(9B) | −0.0260 | 0.3226 | 0.0141 | 0.100* | |
C10 | −0.0193 (3) | 0.1949 (3) | 0.1598 (2) | 0.042 (1) | |
H(10A) | 0.0311 | 0.1226 | 0.1496 | 0.100* | |
H(10B) | −0.0862 | 0.1658 | 0.1855 | 0.100* | |
C11 | 0.0614 (3) | 0.2887 (3) | 0.1987 (2) | 0.042 (1) | |
H(11A) | 0.0097 | 0.3523 | 0.2174 | 0.100* | |
H(11B) | 0.1201 | 0.3298 | 0.1718 | 0.100* | |
C12 | 0.1301 (3) | 0.2131 (3) | 0.2505 (2) | 0.042 (1) | |
H(12A) | 0.0705 | 0.1608 | 0.2715 | 0.100* | |
H(12B) | 0.1889 | 0.1577 | 0.2308 | 0.100* | |
C13 | 0.2822 (3) | 0.3959 (3) | 0.2744 (2) | 0.037 (1) | |
H(13A) | 0.3186 | 0.4436 | 0.3092 | 0.100* | |
H(13B) | 0.2326 | 0.4530 | 0.2484 | 0.100* | |
C14 | 0.3870 (3) | 0.3410 (3) | 0.2350 (2) | 0.036 (1) | |
H(14A) | 0.3513 | 0.2857 | 0.2030 | 0.100* | |
H(14B) | 0.4427 | 0.2919 | 0.2620 | 0.100* | |
C15 | 0.4606 (3) | 0.4460 (3) | 0.2040 (2) | 0.037 (1) | |
H(15A) | 0.4078 | 0.4870 | 0.1724 | 0.100* | |
H(15B) | 0.4850 | 0.5081 | 0.2354 | 0.100* | |
C16 | 0.5530 (3) | 0.2978 (3) | 0.1215 (2) | 0.039 (1) | |
H(16A) | 0.5089 | 0.2265 | 0.1385 | 0.100* | |
H(16B) | 0.6326 | 0.2681 | 0.1076 | 0.100* | |
C17 | 0.4772 (3) | 0.3494 (3) | 0.0643 (2) | 0.043 (1) | |
H(17A) | 0.5310 | 0.3653 | 0.0295 | 0.100* | |
H(17B) | 0.4385 | 0.4281 | 0.0760 | 0.100* | |
C18 | 0.3773 (3) | 0.2554 (3) | 0.0448 (2) | 0.048 (1) | |
H(18A) | 0.4167 | 0.1815 | 0.0276 | 0.100* | |
H(18B) | 0.3330 | 0.2298 | 0.0817 | 0.100* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K(1) | 0.050 (1) | 0.039 (1) | 0.061 (1) | 0.003 (1) | 0.008 (1) | 0.001 (1) |
Co(1) | 0.025 (1) | 0.021 (1) | 0.027 (1) | −0.005 (1) | 0.002 (1) | 0.000 (1) |
C(1) | 0.032 (1) | 0.033 (1) | 0.036 (1) | −0.007 (1) | −0.003 (1) | 0.001 (1) |
N(1) | 0.051 (1) | 0.036 (1) | 0.074 (1) | −0.021 (1) | −0.001 (1) | 0.000 (1) |
C(2) | 0.027 (1) | 0.025 (1) | 0.039 (1) | −0.005 (1) | 0.002 (1) | −0.003 (1) |
N(2) | 0.045 (1) | 0.047 (1) | 0.038 (1) | 0.005 (1) | 0.002 (1) | −0.003 (1) |
C(3) | 0.034 (1) | 0.030 (1) | 0.029 (1) | 0.004 (1) | 0.004 (1) | −0.001 (1) |
N(3) | 0.065 (1) | 0.031 (1) | 0.055 (1) | −0.011 (1) | 0.003 (1) | −0.009 (1) |
C(4) | 0.028 (1) | 0.028 (1) | 0.039 (1) | −0.010 (1) | 0.001 (1) | −0.001 (1) |
N(4) | 0.052 (1) | 0.047 (1) | 0.030 (1) | −0.001 (1) | 0.001 (1) | −0.002 (1) |
C(5) | 0.037 (1) | 0.034 (1) | 0.026 (1) | −0.005 (1) | 0.005 (1) | 0.003 (1) |
N(5) | 0.036 (1) | 0.068 (1) | 0.046 (1) | −0.004 (1) | 0.006 (1) | 0.015 (1) |
C(6) | 0.033 (1) | 0.026 (1) | 0.032 (1) | 0.000 (1) | 0.001 (1) | −0.002 (1) |
N(6) | 0.028 (1) | 0.041 (1) | 0.047 (1) | −0.002 (1) | 0.008 (1) | 0.000 (1) |
N(7) | 0.036 (1) | 0.031 (1) | 0.025 (1) | −0.002 (1) | 0.002 (1) | −0.005 (1) |
N(8) | 0.028 (1) | 0.037 (1) | 0.051 (1) | −0.009 (1) | 0.002 (1) | −0.005 (1) |
N(9) | 0.039 (1) | 0.041 (1) | 0.031 (1) | 0.008 (1) | 0.009 (1) | 0.008 (1) |
N(10) | 0.031 (1) | 0.048 (1) | 0.038 (1) | −0.002 (1) | 0.002 (1) | −0.008 (1) |
C(7) | 0.040 (1) | 0.033 (1) | 0.033 (1) | −0.007 (1) | 0.000 (1) | −0.007 (1) |
C(8) | 0.035 (1) | 0.025 (1) | 0.042 (1) | 0.004 (1) | 0.005 (1) | −0.004 (1) |
C(9) | 0.035 (1) | 0.033 (1) | 0.041 (1) | 0.004 (1) | 0.000 (1) | −0.001 (1) |
C(10) | 0.047 (1) | 0.032 (1) | 0.048 (1) | −0.006 (1) | 0.014 (1) | −0.008 (1) |
C(11) | 0.048 (1) | 0.034 (1) | 0.045 (1) | −0.001 (1) | −0.001 (1) | 0.001 (1) |
C(12) | 0.049 (1) | 0.036 (1) | 0.043 (1) | 0.004 (1) | 0.010 (1) | 0.003 (1) |
C(13) | 0.039 (1) | 0.037 (1) | 0.036 (1) | −0.004 (1) | 0.004 (1) | 0.000 (1) |
C(14) | 0.034 (1) | 0.034 (1) | 0.041 (1) | −0.002 (1) | 0.007 (1) | 0.003 (1) |
C(15) | 0.042 (1) | 0.035 (1) | 0.035 (1) | −0.003 (1) | 0.004 (1) | −0.005 (1) |
C(16) | 0.031 (1) | 0.045 (1) | 0.042 (1) | −0.011 (1) | 0.000 (1) | 0.002 (1) |
C(17) | 0.043 (1) | 0.044 (1) | 0.042 (1) | 0.002 (1) | −0.003 (1) | −0.004 (1) |
C(18) | 0.049 (1) | 0.043 (1) | 0.051 (1) | 0.009 (1) | −0.016 (1) | −0.006 (1) |
Geometric parameters (Å, º) top
K1—N7 | 3.252 (3) | N7—C7 | 1.502 (5) |
K1—C7 | 3.497 (4) | N7—C18 | 1.493 (5) |
K1—N8i | 3.095 (3) | N8—C9 | 1.503 (5) |
K1—N9ii | 3.352 (3) | N8—C10 | 1.486 (5) |
K1—N10iii | 3.077 (3) | N9—C12 | 1.508 (5) |
Co1—C1 | 1.901 (4) | N9—C13 | 1.487 (5) |
Co1—C2 | 1.894 (4) | N10—C15 | 1.490 (5) |
Co1—C3 | 1.889 (3) | N10—C16 | 1.496 (5) |
Co1—C4 | 1.910 (4) | C7—C8 | 1.520 (5) |
Co1—C5 | 1.903 (3) | C8—C9 | 1.510 (5) |
Co1—C6 | 1.899 (3) | C10—C11 | 1.529 (5) |
C1—N1 | 1.142 (5) | C11—C12 | 1.518 (6) |
C2—N2 | 1.143 (5) | C13—C14 | 1.527 (5) |
C3—N3 | 1.151 (5) | C14—C15 | 1.516 (5) |
C4—N4 | 1.150 (5) | C16—C17 | 1.529 (6) |
C5—N5 | 1.140 (5) | C17—C18 | 1.502 (5) |
C6—N6 | 1.140 (5) | | |
| | | |
N1···N7 | 2.899 (6) | N2···N10v | 2.916 (6) |
N4···N8i | 2.909 (6) | N5···N7iii | 2.898 (6) |
N6···N9iv | 2.806 (6) | | |
| | | |
N7—K1—N8i | 120.6 (1) | Co1—C6—N6 | 176.2 (4) |
N7—K1—N9ii | 82.7 (1) | K1—N7—C7 | 86.5 (2) |
N8i—K1—N9ii | 151.7 (1) | K1—N7—C18 | 157.3 (2) |
N7—K1—N10iii | 104.8 (1) | C7—N7—C18 | 113.4 (3) |
N8i—K1—N10iii | 90.7 (1) | C9—N8—C10 | 117.0 (3) |
N9ii—K1—N10iii | 98.8 (1) | C9—N8—K1i | 98.6 (2) |
C1—Co1—C2 | 90.6 (2) | C10—N8—K1i | 112.2 (2) |
C1—Co1—C3 | 177.9 (1) | C12—N9—C13 | 117.2 (3) |
C2—Co1—C3 | 88.4 (2) | C12—N9—K1vi | 79.3 (2) |
C1—Co1—C4 | 89.2 (2) | C13—N9—K1vi | 145.7 (2) |
C2—Co1—C4 | 177.7 (1) | C15—N10—C16 | 117.7 (3) |
C3—Co1—C4 | 91.9 (2) | C15—N10—K1iii | 133.1 (2) |
C1—Co1—C5 | 89.0 (1) | C16—N10—K1iii | 97.8 (2) |
C2—Co1—C5 | 89.8 (2) | N7—C7—C8 | 114.7 (3) |
C3—Co1—C5 | 89.2 (1) | C7—C8—C9 | 112.0 (3) |
C4—Co1—C5 | 92.6 (2) | N8—C9—C8 | 113.1 (3) |
C1—Co1—C6 | 93.0 (1) | N8—C10—C11 | 112.5 (3) |
C2—Co1—C6 | 87.7 (2) | C10—C11—C12 | 107.2 (3) |
C3—Co1—C6 | 88.8 (1) | N9—C12—C11 | 113.8 (3) |
C4—Co1—C6 | 90.0 (2) | N9—C13—C14 | 111.7 (3) |
C5—Co1—C6 | 176.8 (2) | C13—C14—C15 | 111.0 (3) |
Co1—C1—N1 | 176.9 (3) | N10—C15—C14 | 110.9 (3) |
Co1—C2—N2 | 177.9 (3) | N10—C16—C17 | 113.2 (3) |
Co1—C3—N3 | 177.6 (4) | C16—C17—C18 | 109.5 (3) |
Co1—C4—N4 | 175.9 (3) | N7—C18—C17 | 112.4 (3) |
Co1—C5—N5 | 176.9 (4) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) x, −y+1/2, z−1/2; (iii) −x+1, −y+1, −z; (iv) −x, y+1/2, −z+1/2; (v) −x+1, y+1/2, −z+1/2; (vi) x, −y+1/2, z+1/2. |
Crystal data top
H3[Co(CN)6](C8H20N4)·2(H2O) | Z = 1 |
Mr = 426.37 | F(000) = 224 |
Triclinic, P1 | Dx = 1.423 Mg m−3 |
a = 7.635 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.202 (5) Å | Cell parameters from 25 reflections |
c = 9.442 (3) Å | θ = 5–15° |
α = 109.08 (1)° | µ = 0.89 mm−1 |
β = 103.46 (1)° | T = 293 K |
γ = 107.03 (1)° | Plate, colorless |
V = 497.7 (4) Å3 | 0.30 × 0.30 × 0.08 mm |
Data collection top
Siemens P4 diffractometer | 2015 reflections with > 4σ(F) |
Radiation source: fine-focus sealed tube | Rint = 0.187 |
Graphite monochromator | θmax = 27.5°, θmin = 2.5° |
ω scans | h = 0→9 |
Absorption correction: empirical | k = −9→9 |
Tmin = 0.851, Tmax = 1.000 | l = −12→11 |
2375 measured reflections | 3 standard reflections every 100 reflections |
2374 independent reflections | intensity decay: −1.5% |
Refinement top
Refinement on F | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | One H atom on O2W, and the acidic H atoms of the macrocycle can not be
located from differential map |
R[F2 > 2σ(F2)] = 0.061 | Calculated w = 1/[σ2(Fo) + 0.002(Fo2)] |
wR(F2) = 0.082 | (Δ/σ)max = 0.150 |
2015 reflections | Δρmax = 0.85 e Å−3 |
242 parameters | Δρmin = −0.47 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.10 (5) |
Secondary atom site location: difference Fourier map | |
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. One H atom on O2W, and the acdic H atoms of the macrocycle can not be
located from differential map. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.019 (1) | |
C1 | −0.1068 (3) | −0.2125 (3) | 0.0482 (3) | 0.034 (1) | |
C2 | 0.2135 (3) | 0.1290 (3) | 0.2041 (3) | 0.031 (1) | |
C3 | 0.0837 (3) | 0.2040 (3) | −0.0433 (3) | 0.032 (1) | |
C4 | −0.1921 (3) | −0.1299 (3) | −0.2050 (3) | 0.029 (1) | |
C5 | −0.1527 (3) | 0.1068 (3) | 0.0987 (3) | 0.036 (1) | |
C6 | 0.1643 (3) | −0.1085 (3) | −0.0755 (3) | 0.033 (1) | |
N1 | −0.1506 (3) | −0.3420 (3) | 0.0647 (3) | 0.066 (1) | |
N2 | 0.3225 (3) | 0.1964 (3) | 0.3223 (3) | 0.057 (1) | |
N3 | 0.1400 (3) | 0.3316 (3) | −0.0799 (3) | 0.071 (1) | |
N4 | −0.3315 (3) | −0.2175 (3) | −0.3367 (3) | 0.051 (1) | |
N5 | −0.2505 (3) | 0.1810 (3) | 0.1454 (3) | 0.098 (1) | |
N6 | 0.2563 (3) | −0.1745 (3) | −0.1367 (3) | 0.090 (1) | |
N7 | −0.2931 (3) | 0.2971 (3) | −0.1851 (3) | 0.031 (1) | |
H7A | −0.2061 | 0.2938 | −0.1044 | 0.080* | |
N8 | −0.6327 (3) | −0.0621 (3) | −0.4367 (3) | 0.073 (1) | |
H8A | −0.5160 | −0.0714 | −0.4098 | 0.080* | |
N9 | −0.5935 (3) | −0.3615 (3) | −0.6614 (3) | 0.033 (1) | |
N10 | −0.3752 (3) | 0.0608 (3) | −0.5720 (3) | 0.062 (1) | |
H10A | −0.4926 | 0.0691 | −0.5878 | 0.080* | |
C7 | −0.4834 (3) | 0.2559 (3) | −0.2048 (3) | 0.086 (1) | |
H7B | −0.4999 | 0.3722 | −0.1826 | 0.080* | |
H7C | −0.4989 | 0.2224 | −0.1187 | 0.080* | |
C8 | −0.6565 (3) | 0.1117 (3) | −0.3447 (3) | 0.046 (1) | |
H8B | −0.7687 | 0.0758 | −0.3147 | 0.080* | |
H8C | −0.6848 | 0.1680 | −0.4170 | 0.080* | |
C9 | −0.7954 (3) | −0.2089 (3) | −0.5633 (3) | 0.033 (1) | |
H9A | −0.8389 | −0.1623 | −0.6397 | 0.080* | |
H9B | −0.8971 | −0.2389 | −0.5208 | 0.080* | |
C10 | −0.7823 (3) | −0.3874 (3) | −0.6521 (3) | 0.073 (1) | |
H10B | −0.8114 | −0.4692 | −0.6000 | 0.080* | |
H10C | −0.8791 | −0.4487 | −0.7590 | 0.080* | |
C11 | −0.5384 (3) | −0.2647 (3) | −0.7836 (3) | 0.082 (1) | |
H11A | −0.6410 | −0.2302 | −0.8274 | 0.080* | |
H11B | −0.5182 | −0.3487 | −0.8703 | 0.080* | |
C12 | −0.3536 (3) | −0.0938 (3) | −0.6700 (3) | 0.053 (1) | |
H12A | −0.2700 | −0.1295 | −0.6044 | 0.080* | |
H12B | −0.2879 | −0.0567 | −0.7366 | 0.080* | |
C13 | −0.1861 (3) | 0.2185 (3) | −0.4356 (3) | 0.041 (1) | |
H13A | −0.1024 | 0.2835 | −0.4787 | 0.080* | |
H13B | −0.1154 | 0.1645 | −0.3801 | 0.080* | |
C14 | −0.2347 (3) | 0.3568 (3) | −0.3220 (3) | 0.091 (1) | |
H14A | −0.1222 | 0.4749 | −0.2690 | 0.080* | |
H14B | −0.3409 | 0.3764 | −0.3816 | 0.080* | |
O1W | −0.3372 (3) | −0.5152 (3) | −0.7439 (3) | 0.072 (1) | |
H1WA | −0.2781 | −0.4841 | −0.6449 | 0.050* | |
H1WB | −0.2639 | −0.4716 | −0.7896 | 0.050* | |
O2W | 0.2737 (3) | −0.5132 (3) | −0.3581 (3) | 0.099 (1) | |
H2WA | 0.3354 | −0.4539 | −0.2570 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.021 (1) | 0.018 (1) | 0.019 (1) | 0.009 (1) | 0.005 (1) | 0.008 (1) |
C1 | 0.055 (1) | 0.028 (1) | 0.015 (1) | 0.013 (1) | 0.015 (1) | 0.005 (1) |
C2 | 0.027 (1) | 0.043 (1) | 0.024 (1) | 0.019 (1) | 0.001 (1) | 0.019 (1) |
C3 | 0.041 (1) | 0.019 (1) | 0.022 (1) | 0.001 (1) | 0.008 (1) | 0.005 (1) |
C4 | 0.033 (1) | 0.015 (1) | 0.033 (1) | 0.001 (1) | 0.011 (1) | 0.014 (1) |
C5 | 0.044 (1) | 0.031 (1) | 0.020 (1) | −0.002 (1) | 0.007 (1) | 0.017 (1) |
C6 | 0.026 (1) | 0.045 (1) | 0.026 (1) | 0.007 (1) | 0.008 (1) | 0.021 (1) |
N1 | 0.100 (1) | 0.027 (1) | 0.045 (1) | 0.014 (1) | 0.030 (1) | −0.008 (1) |
N2 | 0.050 (1) | 0.041 (1) | 0.053 (1) | 0.005 (1) | −0.012 (1) | 0.022 (1) |
N3 | 0.113 (1) | 0.030 (1) | 0.020 (1) | 0.010 (1) | −0.013 (1) | −0.007 (1) |
N4 | 0.054 (1) | 0.061 (1) | 0.014 (1) | −0.005 (1) | −0.011 (1) | 0.031 (1) |
N5 | 0.038 (1) | 0.074 (1) | 0.109 (1) | −0.033 (1) | 0.011 (1) | 0.017 (1) |
N6 | 0.064 (1) | 0.122 (1) | 0.062 (1) | −0.007 (1) | 0.021 (1) | 0.063 (1) |
N7 | 0.035 (1) | 0.033 (1) | 0.021 (1) | 0.012 (1) | 0.004 (1) | 0.015 (1) |
N8 | 0.011 (1) | 0.044 (1) | 0.127 (1) | 0.034 (1) | −0.019 (1) | 0.001 (1) |
N9 | 0.030 (1) | 0.035 (1) | 0.029 (1) | 0.009 (1) | 0.005 (1) | 0.014 (1) |
N10 | 0.61 (1) | 0.008 (1) | 0.071 (1) | −0.005 (1) | −0.032 (1) | 0.019 (1) |
C7 | 0.056 (1) | 0.044 (1) | 0.111 (1) | 0.037 (1) | −0.035 (1) | 0.003 (1) |
C8 | 0.046 (1) | 0.048 (1) | 0.026 (1) | 0.003 (1) | 0.013 (1) | 0.010 (1) |
C9 | 0.042 (1) | 0.026 (1) | 0.030 (1) | 0.010 (1) | 0.015 (1) | 0.012 (1) |
C10 | 0.012 (1) | 0.006 (1) | 0.135 (1) | −0.013 (1) | −0.019 (1) | 0.004 (1) |
C11 | 0.106 (1) | 0.022 (1) | 0.066 (1) | 0.013 (1) | −0.042 (1) | 0.020 (1) |
C12 | 0.051 (1) | 0.052 (1) | 0.031 (1) | 0.002 (1) | 0.025 (1) | −0.003 (1) |
C13 | 0.010 (1) | 0.054 (1) | 0.039 (1) | 0.016 (1) | −0.001 (1) | −0.002 (1) |
C14 | 0.092 (1) | 0.022 (1) | 0.099 (1) | −0.002 (1) | 0.004 (1) | −0.001 (1) |
O1W | 0.098 (1) | 0.058 (1) | 0.118 (1) | 0.058 (1) | 0.080 (1) | 0.054 (1) |
O2W | 0.110 (1) | 0.065 (1) | 0.154 (1) | 0.046 (1) | 0.092 (1) | 0.046 (1) |
Geometric parameters (Å, º) top
Co1—C1 | 1.942 (3) | N7—C7 | 1.344 (3) |
Co1—C2 | 1.919 (2) | N7—C14 | 1.632 (4) |
Co1—C3 | 1.822 (3) | N8—C8 | 1.495 (3) |
Co1—C4 | 1.857 (2) | N8—C9 | 1.383 (2) |
Co1—C5 | 1.889 (3) | N9—C10 | 1.423 (3) |
Co1—C6 | 1.879 (3) | N9—C11 | 1.663 (4) |
C1—N1 | 1.090 (4) | N10—C12 | 1.385 (3) |
C2—N2 | 1.068 (3) | N10—C13 | 1.539 (2) |
C3—N3 | 1.200 (4) | C7—C8 | 1.463 (2) |
C4—N4 | 1.244 (3) | C9—C10 | 1.476 (3) |
C5—N5 | 1.169 (4) | C11—C12 | 1.503 (2) |
C6—N6 | 1.152 (4) | C13—C14 | 1.487 (3) |
| | | |
O1W···N9 | 2.745 (8) | O1Wii···N9 | 2.707 (8) |
O2W···N6 | 2.942 (8) | O1Wiii···N9 | 3.001 (8) |
N7···N1i | 2.804 (8) | N8···N4 | 3.049 (8) |
N9···N4 | 2.862 (8) | N10iv···N2 | 2.952 (8) |
| | | |
C1—Co1—C2 | 91.2 (1) | Co1—C3—N3 | 176.1 (2) |
C1—Co1—C3 | 175.4 (1) | Co1—C4—N4 | 175.1 (2) |
C2—Co1—C3 | 90.3 (1) | Co1—C5—N5 | 171.7 (3) |
C1—Co1—C4 | 89.8 (1) | Co1—C6—N6 | 172.9 (2) |
C2—Co1—C4 | 175.3 (1) | C7—N7—C14 | 112.9 (2) |
C3—Co1—C4 | 89.1 (1) | C8—N8—C9 | 118.1 (2) |
C1—Co1—C5 | 87.5 (1) | C10—N9—C11 | 115.3 (2) |
C2—Co1—C5 | 89.0 (1) | C12—N10—C13 | 116.0 (2) |
C3—Co1—C5 | 88.3 (1) | N7—C7—C8 | 127.9 (2) |
C4—Co1—C5 | 95.6 (1) | N8—C8—C7 | 115.5 (2) |
C1—Co1—C6 | 88.6 (1) | N8—C9—C10 | 120.2 (2) |
C2—Co1—C6 | 85.5 (1) | N9—C10—C9 | 113.0 (2) |
C3—Co1—C6 | 95.8 (1) | N9—C11—C12 | 101.4 (2) |
C4—Co1—C6 | 89.9 (1) | N10—C12—C11 | 117.1 (2) |
C5—Co1—C6 | 173.2 (1) | N10—C13—C14 | 110.3 (2) |
Co1—C1—N1 | 169.7 (2) | N7—C14—C13 | 114.5 (2) |
Co1—C2—N2 | 174.7 (3) | | |
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z+1; (iii) x, y, z+1; (iv) x+1, y, z+1. |