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The title compounds, [N-(2-aminoethyl)-1,3-propanediamine-κ3N]triazidocobalt(III), [Co(N3)3(C5H15N3)], [N-(2-aminoethyl)-N-methyl-1,3-propanediamine-κ3N]triazidocobalt(III), [Co(N3)3(C6H17N3)], [N-(2-aminopropyl)-1,3-propanediamine-κ3N]triazidocobalt(III), [Co(N3)3(C6H17N3)], and [N-(2-aminopropyl)-N-methyl-1,3-propanediamine-κ3N]triazidocobalt(III), [Co(N3)3(C7H19N3)], each consist of a CoIII atom, three azide ligands in a meridional configuration and a tridentate amine ligand, namely aepn [N-(2-aminoethyl)-1,3-propanediamine] or dpt [N-(3-aminopropyl)-1,3-propanediamine], or their N-methylated analogs.
Supporting information
CCDC references: 153881; 153882; 153883; 153884
For all compounds, data collection: CAD-4-PC (Enraf-Nonius, 1989); cell refinement: CAD-4-PC; data reduction: NRCVAX DATRD2 (Le Page & Gabe, 1979); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: ORTEPIII (Burnett & Johnson, 1996).
(I) Triazido[
N-(2-aminoethyl)-1,3-propanediamine]cobalt(III)
top
Crystal data top
[Co(C5H15N3)(N3)3] | F(000) = 624 |
Mr = 302.22 | Dx = 1.678 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.795 (4) Å | Cell parameters from 25 reflections |
b = 15.958 (5) Å | θ = 6.5–15.1° |
c = 8.903 (4) Å | µ = 1.44 mm−1 |
β = 106.78 (5)° | T = 293 K |
V = 1196.4 (9) Å3 | Brick, dark green |
Z = 4 | 0.49 × 0.20 × 0.18 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1370 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.042 |
Graphite monochromator | θmax = 26.0°, θmin = 2.6° |
ω–2θ scans | h = −10→10 |
Absorption correction: ψ scan (NRCVAX ABSORP; Gabe et al., 1989) | k = 0→19 |
Tmin = 0.456, Tmax = 0.771 | l = 0→10 |
2494 measured reflections | 3 standard reflections every 240 min |
2342 independent reflections | intensity decay: none |
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)] = 0.052 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.125 | All H-atom parameters refined |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0891P)2] where P = (Fo2 + 2Fc2)/3 |
2342 reflections | (Δ/σ)max < 0.001 |
223 parameters | Δρmax = 1.71 e Å−3 |
0 restraints | Δρmin = −0.71 e Å−3 |
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. |
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_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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co | 0.11705 (8) | 0.16988 (4) | 0.95819 (8) | 0.0206 (2) | |
N1 | 0.1679 (6) | 0.1724 (3) | 1.1869 (5) | 0.0269 (10) | |
H1N | 0.094 (7) | 0.187 (3) | 1.224 (6) | 0.020 (14)* | |
H2N | 0.247 (8) | 0.210 (4) | 1.215 (7) | 0.05 (2)* | |
N2 | 0.2206 (5) | 0.0591 (3) | 0.9848 (5) | 0.0235 (10) | |
H3N | 0.150 (7) | 0.031 (4) | 0.973 (6) | 0.023 (16)* | |
N3 | 0.0611 (6) | 0.1652 (3) | 0.7276 (5) | 0.0309 (11) | |
H4N | −0.037 (7) | 0.142 (4) | 0.708 (7) | 0.032 (17)* | |
H5N | 0.031 (6) | 0.216 (3) | 0.696 (6) | 0.017 (13)* | |
N4 | −0.0806 (5) | 0.1108 (3) | 0.9514 (6) | 0.0301 (10) | |
N5 | 0.0111 (5) | 0.2787 (3) | 0.9365 (6) | 0.0348 (12) | |
N6 | 0.3234 (5) | 0.2202 (3) | 0.9791 (5) | 0.0300 (10) | |
N7 | −0.2004 (5) | 0.1494 (3) | 0.9416 (5) | 0.0303 (11) | |
N8 | −0.3188 (6) | 0.1831 (3) | 0.9322 (7) | 0.0510 (15) | |
N9 | 0.0815 (6) | 0.3378 (3) | 1.0047 (6) | 0.0368 (11) | |
N10 | 0.1466 (8) | 0.3979 (4) | 1.0646 (8) | 0.069 (2) | |
N11 | 0.3414 (5) | 0.2718 (3) | 0.8867 (5) | 0.0306 (11) | |
N12 | 0.3667 (7) | 0.3216 (4) | 0.8051 (7) | 0.0500 (14) | |
C1 | 0.2242 (6) | 0.0875 (4) | 1.2498 (7) | 0.0291 (13) | |
H1C | 0.284 (7) | 0.088 (4) | 1.360 (7) | 0.038 (16)* | |
H2C | 0.136 (7) | 0.049 (4) | 1.247 (6) | 0.032 (15)* | |
C2 | 0.3197 (6) | 0.0532 (3) | 1.1517 (6) | 0.0285 (12) | |
H3C | 0.412 (6) | 0.094 (3) | 1.167 (5) | 0.020 (13)* | |
H4C | 0.3467 (6) | −0.006 (4) | 1.179 (6) | 0.029 (14)* | |
C3 | 0.3061 (7) | 0.0322 (4) | 0.8742 (7) | 0.0326 (13) | |
H5C | 0.385 (7) | 0.068 (4) | 0.888 (7) | 0.037 (17)* | |
H6C | 0.343 (6) | −0.027 (4) | 0.9023 (6) | 0.032 (15)* | |
C4 | 0.2061 (8) | 0.0371 (4) | 0.7051 (7) | 0.0373 (15) | |
H7C | 0.265 (7) | 0.024 (4) | 0.640 (8) | 0.046 (19)* | |
H8C | 0.121 (9) | 0.004 (5) | 0.692 (8) | 0.06 (2)* | |
C5 | 0.1650 (8) | 0.1248 (4) | 0.6468 (7) | 0.0378 (15) | |
H9C | 0.246 (7) | 0.156 (4) | 0.664 (7) | 0.027 (17)* | |
H10C | 0.114 (5) | 0.122 (3) | 0.540 (6) | 0.017 (13)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0204 (3) | 0.0128 (3) | 0.0274 (4) | 0.0010 (3) | 0.0051 (2) | −0.0006 (3) |
N1 | 0.031 (2) | 0.019 (2) | 0.033 (2) | −0.001 (2) | 0.013 (2) | −0.002 (2) |
N2 | 0.023 (2) | 0.016 (2) | 0.029 (2) | −0.002 (2) | 0.005 (2) | 0.000 (2) |
N3 | 0.041 (3) | 0.022 (3) | 0.027 (2) | 0.008 (2) | 0.004 (2) | 0.005 (2) |
N4 | 0.023 (2) | 0.017 (2) | 0.048 (3) | −0.002 (2) | 0.006 (2) | −0.004 (2) |
N5 | 0.033 (3) | 0.016 (2) | 0.051 (3) | 0.003 (2) | 0.006 (2) | −0.004 (2) |
N6 | 0.024 (2) | 0.029 (3) | 0.036 (2) | −0.005 (2) | 0.006 (2) | 0.005 (2) |
N7 | 0.025 (2) | 0.022 (2) | 0.042 (3) | −0.002 (2) | 0.005 (2) | 0.005 (2) |
N8 | 0.029 (3) | 0.044 (3) | 0.081 (4) | 0.012 (2) | 0.018 (3) | 0.018 (3) |
N9 | 0.047 (3) | 0.021 (3) | 0.042 (3) | 0.005 (2) | 0.012 (2) | 0.004 (2) |
N10 | 0.093 (5) | 0.027 (3) | 0.078 (5) | −0.008 (3) | 0.008 (4) | −0.017 (3) |
N11 | 0.025 (2) | 0.031 (3) | 0.034 (2) | −0.006 (2) | 0.005 (2) | −0.002 (2) |
N12 | 0.052 (3) | 0.051 (4) | 0.050 (3) | −0.008 (3) | 0.019 (3) | 0.016 (3) |
C1 | 0.029 (3) | 0.030 (3) | 0.028 (3) | −0.004 (2) | 0.007 (2) | 0.004 (2) |
C2 | 0.031 (3) | 0.017 (3) | 0.032 (3) | 0.001 (2) | 0.002 (2) | 0.003 (2) |
C3 | 0.033 (3) | 0.028 (3) | 0.038 (3) | 0.004 (3) | 0.013 (3) | −0.002 (3) |
C4 | 0.045 (4) | 0.032 (3) | 0.037 (3) | 0.009 (3) | 0.015 (3) | −0.005 (3) |
C5 | 0.045 (4) | 0.038 (4) | 0.029 (3) | 0.010 (3) | 0.009 (3) | −0.002 (3) |
Geometric parameters (Å, º) top
Co—N6 | 1.943 (4) | N6—N11 | 1.207 (6) |
Co—N5 | 1.954 (4) | N7—N8 | 1.153 (7) |
Co—N1 | 1.955 (5) | N9—N10 | 1.165 (7) |
Co—N4 | 1.963 (4) | N11—N12 | 1.141 (7) |
Co—N3 | 1.970 (5) | C1—C2 | 1.480 (8) |
Co—N2 | 1.971 (4) | C1—H1C | 0.97 (6) |
N1—C1 | 1.495 (7) | C1—H2C | 0.99 (6) |
N1—H1N | 0.85 (6) | C2—H3C | 1.01 (5) |
N1—H2N | 0.90 (7) | C2—H4C | 0.99 (6) |
N2—C3 | 1.466 (7) | C3—C4 | 1.510 (8) |
N2—C2 | 1.493 (7) | C3—H5C | 0.88 (6) |
N2—H3N | 0.74 (6) | C3—H6C | 1.01 (6) |
N3—C5 | 1.466 (8) | C4—C5 | 1.501 (9) |
N3—H4N | 0.91 (6) | C4—H7C | 0.91 (7) |
N3—H5N | 0.88 (5) | C4—H8C | 0.90 (7) |
N4—N7 | 1.202 (6) | C5—H9C | 0.84 (6) |
N5—N9 | 1.193 (6) | C5—H10C | 0.93 (5) |
| | | |
N6—Co—N5 | 92.7 (2) | N11—N6—Co | 121.3 (4) |
N6—Co—N1 | 88.0 (2) | N8—N7—N4 | 176.9 (6) |
N5—Co—N1 | 92.5 (2) | N10—N9—N5 | 176.5 (6) |
N6—Co—N4 | 174.5 (2) | N12—N11—N6 | 176.1 (5) |
N5—Co—N4 | 91.8 (2) | C2—C1—N1 | 107.3 (4) |
N1—Co—N4 | 88.6 (2) | C2—C1—H1C | 112 (3) |
N6—Co—N3 | 93.5 (2) | N1—C1—H1C | 113 (4) |
N5—Co—N3 | 87.8 (2) | C2—C1—H2C | 109 (3) |
N1—Co—N3 | 178.4 (2) | N1—C1—H2C | 112 (3) |
N4—Co—N3 | 89.8 (2) | H1C—C1—H2C | 103 (5) |
N6—Co—N2 | 88.4 (2) | C1—C2—N2 | 107.2 (4) |
N5—Co—N2 | 178.3 (2) | C1—C2—H3C | 105 (3) |
N1—Co—N2 | 86.2 (2) | N2—C2—H3C | 108 (4) |
N4—Co—N2 | 87.0 (2) | C1—C2—H4C | 110 (3) |
N3—Co—N2 | 93.4 (2) | N2—C2—H4C | 110 (3) |
C1—N1—Co | 108.8 (3) | H3C—C2—H4C | 117 (4) |
C1—N1—H1N | 108 (4) | N2—C3—C4 | 113.0 (5) |
Co—N1—H1N | 116 (4) | N2—C3—H5C | 104 (4) |
C1—N1—H2N | 111 (4) | C4—C3—H5C | 108 (4) |
Co—N1—H2N | 103 (4) | N2—C3—H6C | 107 (3) |
H1N—N1—H2N | 109 (6) | C4—C3—H6C | 110 (3) |
C3—N2—C2 | 112.6 (4) | H5C—C3—H6C | 114 (5) |
C3—N2—Co | 119.4 (4) | C5—C4—C3 | 113.9 (5) |
C2—N2—Co | 107.1 (3) | C5—C4—H7C | 97 (4) |
C3—N2—H3N | 107 (4) | C3—C4—H7C | 111 (4) |
C2—N2—H3N | 109 (4) | C5—C4—H8C | 114 (5) |
Co—N2—H3N | 101 (4) | C3—C4—H8C | 109 (4) |
C5—N3—Co | 121.7 (4) | H7C—C4—H8C | 112 (6) |
C5—N3—H4N | 115 (4) | N3—C5—C4 | 111.2 (6) |
Co—N3—H4N | 99 (4) | N3—C5—H9C | 105 (4) |
C5—N3—H5N | 115 (3) | C4—C5—H9C | 112 (4) |
Co—N3—H5N | 105 (3) | N3—C5—H10C | 109 (3) |
H4N—N3—H5N | 97 (5) | C4—C5—H10C | 108 (3) |
N7—N4—Co | 120.4 (4) | H9C—C5—H10C | 111 (5) |
N9—N5—Co | 119.3 (4) | | |
(II) Triazido[
N,
N-(2-aminoethyl)-methyl-1,3-propanediamine]cobalt(III)
top
Crystal data top
[Co(C6H17N3)(N3)3] | F(000) = 656 |
Mr = 316.25 | Dx = 1.616 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.560 (3) Å | Cell parameters from 25 reflections |
b = 9.404 (2) Å | θ = 8.1–12.7° |
c = 16.149 (4) Å | µ = 1.33 mm−1 |
β = 91.65 (3)° | T = 293 K |
V = 1299.5 (7) Å3 | Brick, dark green |
Z = 4 | 0.50 × 0.48 × 0.21 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1851 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.019 |
Graphite monochromator | θmax = 25.0°, θmin = 2.5° |
ω–2θ scans | h = −10→10 |
Absorption correction: ψ scan (NRCVAX ABSORP; Gabe et al., 1989) | k = 0→11 |
Tmin = 0.654, Tmax = 0.756 | l = 0→19 |
2357 measured reflections | 3 standard reflections every 240 min |
2278 independent reflections | intensity decay: none |
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)] = 0.022 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.057 | All H-atom parameters refined |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0364P)2 + 0.0998P] where P = (Fo2 + 2Fc2)/3 |
2278 reflections | (Δ/σ)max = −0.009 |
240 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.22 e Å−3 |
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. |
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_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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co | 0.03654 (3) | 0.21659 (3) | 0.129815 (14) | 0.02545 (9) | |
N1 | 0.1369 (2) | 0.1907 (2) | 0.23898 (11) | 0.0369 (4) | |
H1N | 0.228 (3) | 0.171 (3) | 0.2373 (15) | 0.047 (7)* | |
H2N | 0.125 (3) | 0.270 (3) | 0.2643 (16) | 0.054 (7)* | |
N2 | −0.1460 (2) | 0.1064 (2) | 0.17558 (9) | 0.0289 (3) | |
N3 | −0.0723 (2) | 0.2358 (2) | 0.02167 (10) | 0.0322 (4) | |
H3N | −0.022 (3) | 0.290 (3) | −0.0076 (15) | 0.049 (7)* | |
H4N | −0.066 (3) | 0.157 (3) | 0.0010 (14) | 0.045 (7)* | |
N4 | 0.1332 (2) | 0.0445 (2) | 0.08478 (10) | 0.0368 (4) | |
N5 | 0.2200 (2) | 0.3255 (2) | 0.09835 (12) | 0.0469 (5) | |
N6 | −0.0586 (2) | 0.3906 (2) | 0.17103 (10) | 0.0351 (4) | |
N7 | 0.2525 (2) | 0.0014 (2) | 0.11699 (10) | 0.0318 (4) | |
N8 | 0.3665 (2) | −0.0440 (2) | 0.14558 (12) | 0.0490 (5) | |
N9 | 0.2622 (2) | 0.3255 (2) | 0.02904 (12) | 0.0393 (4) | |
N10 | 0.3094 (3) | 0.3287 (3) | −0.03648 (14) | 0.0718 (7) | |
N11 | 0.0008 (2) | 0.5048 (2) | 0.16284 (10) | 0.0322 (4) | |
N12 | 0.0501 (2) | 0.6180 (2) | 0.15798 (13) | 0.0503 (5) | |
C1 | 0.0519 (3) | 0.0842 (3) | 0.28720 (14) | 0.0457 (5) | |
H1C | 0.087 (3) | −0.011 (3) | 0.2670 (15) | 0.052 (7)* | |
H2C | 0.067 (3) | 0.095 (3) | 0.3452 (16) | 0.065 (8)* | |
C2 | −0.1194 (3) | 0.1086 (3) | 0.26746 (12) | 0.0405 (5) | |
H3C | −0.151 (2) | 0.207 (2) | 0.2868 (12) | 0.034 (5)* | |
H4C | −0.183 (3) | 0.037 (3) | 0.2936 (14) | 0.045 (6)* | |
C3 | −0.3013 (2) | 0.1745 (3) | 0.15721 (14) | 0.0393 (5) | |
H5C | −0.301 (2) | 0.271 (2) | 0.1814 (13) | 0.035 (5)* | |
H6C | −0.379 (3) | 0.122 (3) | 0.1851 (14) | 0.049 (6)* | |
C4 | −0.3417 (3) | 0.1866 (3) | 0.06548 (15) | 0.0479 (6) | |
H7C | −0.339 (2) | 0.091 (3) | 0.0421 (13) | 0.037 (6)* | |
H8C | −0.443 (4) | 0.225 (3) | 0.0593 (17) | 0.068 (8)* | |
C5 | −0.2376 (3) | 0.2839 (3) | 0.01880 (14) | 0.0433 (5) | |
H9C | −0.236 (3) | 0.378 (3) | 0.0381 (15) | 0.051 (7)* | |
H10C | −0.270 (3) | 0.290 (3) | −0.0402 (16) | 0.053 (7)* | |
C6 | −0.1569 (3) | −0.0446 (2) | 0.1478 (2) | 0.0440 (5) | |
H11C | −0.160 (2) | −0.047 (2) | 0.0870 (13) | 0.037 (6)* | |
H12C | −0.063 (3) | −0.099 (3) | 0.1724 (14) | 0.053 (7)* | |
H13C | −0.257 (3) | −0.080 (3) | 0.1675 (15) | 0.061 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.02504 (14) | 0.02436 (14) | 0.02689 (14) | −0.00089 (10) | 0.00001 (9) | −0.00342 (10) |
N1 | 0.0338 (10) | 0.0421 (11) | 0.0343 (9) | 0.0041 (8) | −0.0069 (7) | −0.0096 (8) |
N2 | 0.0327 (8) | 0.0248 (8) | 0.0294 (8) | −0.0012 (6) | 0.0032 (6) | −0.0019 (6) |
N3 | 0.0347 (9) | 0.0322 (9) | 0.0298 (8) | 0.0014 (8) | 0.0008 (7) | 0.0004 (8) |
N4 | 0.0326 (9) | 0.0377 (9) | 0.0398 (9) | 0.0072 (7) | −0.0064 (7) | −0.0110 (7) |
N5 | 0.0408 (10) | 0.0514 (11) | 0.0492 (11) | −0.0148 (9) | 0.0145 (8) | −0.0162 (9) |
N6 | 0.0357 (9) | 0.0255 (9) | 0.0443 (10) | −0.0027 (7) | 0.0060 (7) | −0.0057 (7) |
N7 | 0.0350 (9) | 0.0293 (8) | 0.0312 (8) | −0.0012 (7) | 0.0031 (7) | −0.0039 (7) |
N8 | 0.0413 (10) | 0.0504 (12) | 0.0546 (12) | 0.0118 (9) | −0.0110 (9) | 0.0011 (9) |
N9 | 0.0295 (8) | 0.0369 (10) | 0.0515 (12) | −0.0027 (7) | 0.0027 (8) | 0.0025 (8) |
N10 | 0.073 (2) | 0.094 (2) | 0.0488 (13) | −0.0159 (14) | 0.0152 (12) | 0.0076 (12) |
N11 | 0.0346 (8) | 0.0304 (10) | 0.0315 (8) | 0.0036 (7) | −0.0007 (7) | −0.0005 (7) |
N12 | 0.0548 (12) | 0.0282 (10) | 0.0680 (13) | −0.0064 (8) | 0.0031 (10) | 0.0067 (9) |
C1 | 0.0572 (14) | 0.0503 (14) | 0.0294 (11) | 0.0084 (11) | −0.0047 (10) | 0.0048 (10) |
C2 | 0.0505 (12) | 0.0415 (12) | 0.0298 (10) | −0.0007 (10) | 0.0058 (9) | 0.0022 (9) |
C3 | 0.0277 (10) | 0.0456 (12) | 0.0450 (12) | −0.0029 (9) | 0.0056 (9) | −0.0022 (10) |
C4 | 0.0304 (11) | 0.064 (2) | 0.0483 (13) | 0.0036 (11) | −0.0063 (9) | −0.0027 (11) |
C5 | 0.0434 (12) | 0.0474 (14) | 0.0388 (12) | 0.0116 (10) | −0.0084 (9) | 0.0036 (10) |
C6 | 0.0558 (15) | 0.0285 (11) | 0.0484 (13) | −0.0102 (10) | 0.0112 (11) | −0.0049 (10) |
Geometric parameters (Å, º) top
Co—N6 | 1.953 (2) | N9—N10 | 1.144 (3) |
Co—N1 | 1.954 (2) | N11—N12 | 1.149 (2) |
Co—N5 | 1.955 (2) | C1—C2 | 1.509 (3) |
Co—N3 | 1.964 (2) | C1—H1C | 1.00 (3) |
Co—N4 | 1.966 (2) | C1—H2C | 0.95 (3) |
Co—N2 | 2.032 (2) | C2—H3C | 1.01 (2) |
N1—C1 | 1.474 (3) | C2—H4C | 0.97 (2) |
N1—H1N | 0.81 (3) | C3—C4 | 1.516 (3) |
N1—H2N | 0.86 (3) | C3—H5C | 0.99 (2) |
N2—C6 | 1.492 (3) | C3—H6C | 0.96 (2) |
N2—C2 | 1.495 (2) | C4—C5 | 1.496 (3) |
N2—C3 | 1.497 (3) | C4—H7C | 0.98 (2) |
N3—C5 | 1.485 (3) | C4—H8C | 0.94 (3) |
N3—H3N | 0.83 (3) | C5—H9C | 0.94 (3) |
N3—H4N | 0.82 (3) | C5—H10C | 0.99 (3) |
N4—N7 | 1.203 (2) | C6—H11C | 0.98 (2) |
N5—N9 | 1.186 (3) | C6—H12C | 1.02 (2) |
N6—N11 | 1.196 (2) | C6—H13C | 0.98 (3) |
N7—N8 | 1.150 (2) | | |
| | | |
N6—Co—N1 | 88.50 (8) | N12—N11—N6 | 175.5 (2) |
N6—Co—N5 | 89.73 (7) | N1—C1—C2 | 106.1 (2) |
N1—Co—N5 | 87.94 (9) | N1—C1—H1C | 105.9 (14) |
N6—Co—N3 | 91.97 (7) | C2—C1—H1C | 111.6 (13) |
N1—Co—N3 | 177.15 (8) | N1—C1—H2C | 112.9 (17) |
N5—Co—N3 | 94.87 (8) | C2—C1—H2C | 107.4 (16) |
N6—Co—N4 | 178.11 (7) | H1C—C1—H2C | 113 (2) |
N1—Co—N4 | 93.00 (8) | N2—C2—C1 | 109.1 (2) |
N5—Co—N4 | 89.17 (8) | N2—C2—H3C | 106.5 (11) |
N3—Co—N4 | 86.59 (7) | C1—C2—H3C | 109.7 (12) |
N6—Co—N2 | 88.32 (7) | N2—C2—H4C | 110.7 (13) |
N1—Co—N2 | 86.06 (7) | C1—C2—H4C | 110.9 (13) |
N5—Co—N2 | 173.73 (7) | H3C—C2—H4C | 109.9 (17) |
N3—Co—N2 | 91.15 (7) | N2—C3—C4 | 113.7 (2) |
N4—Co—N2 | 92.94 (7) | N2—C3—H5C | 108.9 (12) |
C1—N1—Co | 110.50 (13) | C4—C3—H5C | 108.3 (12) |
C1—N1—H1N | 110.6 (18) | N2—C3—H6C | 108.1 (14) |
Co—N1—H1N | 113.6 (17) | C4—C3—H6C | 111.0 (13) |
C1—N1—H2N | 105.7 (17) | H5C—C3—H6C | 106.6 (19) |
Co—N1—H2N | 105.4 (17) | C5—C4—C3 | 114.6 (2) |
H1N—N1—H2N | 111 (2) | C5—C4—H7C | 110.3 (13) |
C6—N2—C2 | 108.5 (2) | C3—C4—H7C | 107.5 (12) |
C6—N2—C3 | 107.4 (2) | C5—C4—H8C | 105.9 (17) |
C2—N2—C3 | 107.5 (2) | C3—C4—H8C | 108.4 (17) |
C6—N2—Co | 114.70 (13) | H7C—C4—H8C | 110 (2) |
C2—N2—Co | 104.92 (12) | N3—C5—C4 | 112.2 (2) |
C3—N2—Co | 113.44 (12) | N3—C5—H9C | 105.6 (15) |
C5—N3—Co | 118.88 (14) | C4—C5—H9C | 114.5 (15) |
C5—N3—H3N | 107.8 (17) | N3—C5—H10C | 106.7 (14) |
Co—N3—H3N | 108.9 (17) | C4—C5—H10C | 111.6 (14) |
C5—N3—H4N | 109.9 (17) | H9C—C5—H10C | 105.7 (19) |
Co—N3—H4N | 104.2 (16) | N2—C6—H11C | 108.8 (13) |
H3N—N3—H4N | 107 (2) | N2—C6—H12C | 108.3 (14) |
N7—N4—Co | 118.58 (13) | H11C—C6—H12C | 111.8 (18) |
N9—N5—Co | 120.93 (15) | N2—C6—H13C | 105.8 (15) |
N11—N6—Co | 122.11 (13) | H11C—C6—H13C | 108.8 (19) |
N8—N7—N4 | 177.4 (2) | H12C—C6—H13C | 113 (2) |
N10—N9—N5 | 176.7 (2) | | |
(III) Triazido[
N-(3-aminopropyl)-1,3-propanediamine]cobalt(III)
top
Crystal data top
[Co(C6H17N3)(N3)3] | F(000) = 656 |
Mr = 316.25 | Dx = 1.628 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.8040 (12) Å | Cell parameters from 25 reflections |
b = 9.286 (2) Å | θ = 7.9–12.8° |
c = 14.209 (2) Å | µ = 1.34 mm−1 |
β = 94.267 (14)° | T = 293 K |
V = 1290.1 (3) Å3 | Brick, dark green |
Z = 4 | 0.65 × 0.45 × 0.35 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1918 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 26.5°, θmin = 2.1° |
ω–2θ scans | h = −12→12 |
Absorption correction: ψ scan (NRCVAX ABSORP; Gabe et al., 1989) | k = 0→11 |
Tmin = 0.570, Tmax = 0.625 | l = 0→17 |
2777 measured reflections | 3 standard reflections every 240 min |
2664 independent reflections | intensity decay: none |
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)] = 0.025 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.060 | All H-atom parameters refined |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0326P)2] where P = (Fo2 + 2Fc2)/3 |
2664 reflections | (Δ/σ)max = 0.004 |
240 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.23 e Å−3 |
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. |
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_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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co | 0.64854 (3) | 0.19033 (3) | 0.90649 (2) | 0.02257 (9) | |
N1 | 0.6185 (2) | −0.0139 (2) | 0.87042 (14) | 0.0294 (4) | |
H1N | 0.572 (2) | −0.038 (3) | 0.9124 (16) | 0.033 (7)* | |
H2N | 0.564 (3) | −0.019 (3) | 0.8199 (19) | 0.053 (8)* | |
N2 | 0.8349 (2) | 0.2054 (2) | 0.85703 (12) | 0.0296 (4) | |
H3N | 0.811 (2) | 0.224 (2) | 0.7985 (17) | 0.033 (6)* | |
N3 | 0.6433 (2) | 0.3906 (2) | 0.95173 (14) | 0.0314 (4) | |
H4N | 0.587 (3) | 0.428 (3) | 0.9133 (18) | 0.040 (7)* | |
H5N | 0.603 (2) | 0.383 (2) | 1.0023 (17) | 0.028 (6)* | |
N4 | 0.5737 (2) | 0.2661 (2) | 0.78332 (11) | 0.0299 (4) | |
N5 | 0.4639 (2) | 0.1808 (2) | 0.95258 (13) | 0.0355 (4) | |
N6 | 0.7240 (2) | 0.1169 (2) | 1.02741 (13) | 0.0424 (5) | |
N7 | 0.5558 (2) | 0.1866 (2) | 0.71736 (11) | 0.0286 (4) | |
N8 | 0.5375 (2) | 0.1133 (2) | 0.65197 (14) | 0.0481 (5) | |
N9 | 0.3671 (2) | 0.1827 (2) | 0.89611 (14) | 0.0422 (5) | |
N10 | 0.2706 (2) | 0.1827 (3) | 0.8456 (2) | 0.0866 (10) | |
N11 | 0.7901 (2) | 0.1813 (2) | 1.08625 (12) | 0.0314 (4) | |
N12 | 0.8560 (2) | 0.2381 (3) | 1.14651 (13) | 0.0504 (6) | |
C1 | 0.7341 (3) | −0.1141 (3) | 0.8650 (2) | 0.0402 (6) | |
H1C | 0.698 (3) | −0.201 (3) | 0.8419 (18) | 0.049 (7)* | |
H2C | 0.774 (2) | −0.124 (3) | 0.9300 (18) | 0.043 (7)* | |
C2 | 0.8431 (3) | −0.0524 (3) | 0.8073 (2) | 0.0432 (6) | |
H3C | 0.807 (3) | −0.022 (3) | 0.7460 (18) | 0.043 (7)* | |
H4C | 0.905 (3) | −0.128 (3) | 0.7946 (19) | 0.062 (8)* | |
C3 | 0.9177 (2) | 0.0714 (3) | 0.8548 (2) | 0.0435 (6) | |
H5C | 1.002 (3) | 0.092 (3) | 0.8274 (17) | 0.047 (7)* | |
H6C | 0.946 (2) | 0.048 (3) | 0.9159 (18) | 0.046 (7)* | |
C4 | 0.9253 (2) | 0.3245 (3) | 0.8945 (2) | 0.0422 (6) | |
H7C | 1.003 (3) | 0.321 (3) | 0.8579 (18) | 0.047 (7)* | |
H8C | 0.954 (3) | 0.297 (3) | 0.9576 (18) | 0.046 (7)* | |
C5 | 0.8581 (3) | 0.4699 (3) | 0.8899 (2) | 0.0483 (7) | |
H9C | 0.925 (3) | 0.541 (3) | 0.8974 (18) | 0.052 (7)* | |
H10C | 0.809 (3) | 0.482 (3) | 0.8319 (19) | 0.048 (7)* | |
C6 | 0.7608 (3) | 0.4896 (3) | 0.9660 (2) | 0.0423 (6) | |
H11C | 0.807 (2) | 0.467 (3) | 1.0262 (17) | 0.046 (7)* | |
H12C | 0.723 (2) | 0.584 (3) | 0.9692 (16) | 0.044 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.02707 (14) | 0.02442 (14) | 0.01605 (13) | −0.00219 (13) | 0.00052 (9) | 0.00144 (12) |
N1 | 0.0342 (11) | 0.0297 (10) | 0.0243 (9) | −0.0019 (8) | 0.0018 (8) | −0.0006 (8) |
N2 | 0.0279 (9) | 0.0368 (10) | 0.0238 (9) | −0.0026 (8) | −0.0005 (7) | 0.0033 (8) |
N3 | 0.0447 (11) | 0.0282 (10) | 0.0210 (9) | 0.0010 (9) | 0.0013 (9) | 0.0021 (8) |
N4 | 0.0356 (10) | 0.0337 (10) | 0.0199 (8) | 0.0028 (8) | −0.0019 (7) | 0.0005 (8) |
N5 | 0.0337 (10) | 0.0429 (11) | 0.0312 (9) | −0.0028 (9) | 0.0109 (8) | −0.0015 (9) |
N6 | 0.0643 (14) | 0.0354 (11) | 0.0255 (9) | −0.0081 (10) | −0.0101 (9) | 0.0058 (9) |
N7 | 0.0285 (9) | 0.0349 (9) | 0.0219 (8) | −0.0042 (8) | −0.0007 (7) | 0.0076 (9) |
N8 | 0.0724 (15) | 0.0455 (12) | 0.0253 (10) | −0.0143 (11) | −0.0028 (9) | −0.0042 (10) |
N9 | 0.0338 (11) | 0.0466 (12) | 0.0478 (12) | 0.0004 (10) | 0.0128 (9) | 0.0178 (10) |
N10 | 0.0350 (13) | 0.138 (3) | 0.085 (2) | −0.006 (2) | −0.0066 (12) | 0.055 (2) |
N11 | 0.0325 (9) | 0.0391 (10) | 0.0226 (8) | 0.0100 (9) | 0.0021 (7) | 0.0050 (9) |
N12 | 0.0491 (13) | 0.0683 (15) | 0.0316 (11) | 0.0012 (11) | −0.0114 (9) | −0.0090 (10) |
C1 | 0.050 (2) | 0.0286 (13) | 0.0413 (14) | 0.0038 (11) | 0.0019 (11) | −0.0007 (11) |
C2 | 0.0435 (14) | 0.0440 (14) | 0.0428 (14) | 0.0120 (12) | 0.0086 (11) | −0.0066 (12) |
C3 | 0.0302 (13) | 0.052 (2) | 0.0480 (15) | 0.0071 (12) | 0.0030 (11) | 0.0036 (13) |
C4 | 0.0332 (12) | 0.054 (2) | 0.0392 (13) | −0.0175 (12) | 0.0010 (10) | 0.0010 (12) |
C5 | 0.057 (2) | 0.0398 (15) | 0.047 (2) | −0.0232 (13) | −0.0003 (13) | 0.0062 (12) |
C6 | 0.057 (2) | 0.0289 (13) | 0.0400 (14) | −0.0077 (11) | −0.0054 (12) | −0.0032 (11) |
Geometric parameters (Å, º) top
Co—N6 | 1.943 (2) | N9—N10 | 1.145 (3) |
Co—N3 | 1.970 (2) | N11—N12 | 1.160 (3) |
Co—N5 | 1.973 (2) | C1—C2 | 1.508 (3) |
Co—N4 | 1.976 (2) | C1—H1C | 0.93 (3) |
Co—N1 | 1.981 (2) | C1—H2C | 0.98 (2) |
Co—N2 | 2.010 (2) | C2—C3 | 1.497 (4) |
N1—C1 | 1.473 (3) | C2—H3C | 0.96 (2) |
N1—H1N | 0.81 (2) | C2—H4C | 0.95 (3) |
N1—H2N | 0.86 (3) | C3—H5C | 0.96 (3) |
N2—C3 | 1.487 (3) | C3—H6C | 0.92 (3) |
N2—C4 | 1.491 (3) | C4—C5 | 1.501 (4) |
N2—H3N | 0.86 (2) | C4—H7C | 0.96 (3) |
N3—C6 | 1.476 (3) | C4—H8C | 0.95 (3) |
N3—H4N | 0.82 (3) | C5—C6 | 1.505 (4) |
N3—H5N | 0.85 (2) | C5—H9C | 0.93 (3) |
N4—N7 | 1.196 (2) | C5—H10C | 0.93 (3) |
N5—N9 | 1.196 (3) | C6—H11C | 0.96 (2) |
N6—N11 | 1.182 (2) | C6—H12C | 0.95 (2) |
N7—N8 | 1.155 (2) | | |
| | | |
N6—Co—N3 | 93.46 (8) | N12—N11—N6 | 176.5 (2) |
N6—Co—N5 | 89.37 (8) | N1—C1—C2 | 111.6 (2) |
N3—Co—N5 | 83.53 (8) | N1—C1—H1C | 107.0 (15) |
N6—Co—N4 | 179.40 (8) | C2—C1—H1C | 113.9 (16) |
N3—Co—N4 | 86.32 (8) | N1—C1—H2C | 105.5 (14) |
N5—Co—N4 | 91.16 (8) | C2—C1—H2C | 107.3 (14) |
N6—Co—N1 | 86.11 (8) | H1C—C1—H2C | 111 (2) |
N3—Co—N1 | 168.96 (8) | C3—C2—C1 | 112.9 (2) |
N5—Co—N1 | 85.44 (8) | C3—C2—H3C | 108.6 (15) |
N4—Co—N1 | 94.22 (8) | C1—C2—H3C | 112.0 (15) |
N6—Co—N2 | 92.16 (8) | C3—C2—H4C | 110.9 (17) |
N3—Co—N2 | 95.43 (8) | C1—C2—H4C | 107.9 (17) |
N5—Co—N2 | 178.20 (8) | H3C—C2—H4C | 104 (2) |
N4—Co—N2 | 87.31 (7) | N2—C3—C2 | 113.7 (2) |
N1—Co—N2 | 95.61 (7) | N2—C3—H5C | 109.3 (15) |
C1—N1—Co | 121.23 (15) | C2—C3—H5C | 112.1 (14) |
C1—N1—H1N | 110.0 (16) | N2—C3—H6C | 108.0 (16) |
Co—N1—H1N | 98.9 (17) | C2—C3—H6C | 110.2 (16) |
C1—N1—H2N | 110.8 (18) | H5C—C3—H6C | 103 (2) |
Co—N1—H2N | 109.7 (18) | N2—C4—C5 | 113.9 (2) |
H1N—N1—H2N | 104 (2) | N2—C4—H7C | 104.8 (15) |
C3—N2—C4 | 108.5 (2) | C5—C4—H7C | 112.1 (14) |
C3—N2—Co | 117.47 (14) | N2—C4—H8C | 105.2 (15) |
C4—N2—Co | 117.26 (14) | C5—C4—H8C | 112.2 (15) |
C3—N2—H3N | 104.9 (15) | H7C—C4—H8C | 108 (2) |
C4—N2—H3N | 107.8 (15) | C4—C5—C6 | 112.2 (2) |
Co—N2—H3N | 99.2 (14) | C4—C5—H9C | 109.5 (16) |
C6—N3—Co | 126.4 (2) | C6—C5—H9C | 108.0 (16) |
C6—N3—H4N | 107.9 (17) | C4—C5—H10C | 110.1 (15) |
Co—N3—H4N | 102.1 (17) | C6—C5—H10C | 107.7 (16) |
C6—N3—H5N | 110.0 (15) | H9C—C5—H10C | 109 (2) |
Co—N3—H5N | 103.1 (15) | N3—C6—C5 | 110.9 (2) |
H4N—N3—H5N | 105 (2) | N3—C6—H11C | 107.5 (15) |
N7—N4—Co | 119.82 (14) | C5—C6—H11C | 109.4 (14) |
N9—N5—Co | 118.57 (14) | N3—C6—H12C | 106.1 (14) |
N11—N6—Co | 126.9 (2) | C5—C6—H12C | 114.6 (15) |
N8—N7—N4 | 178.0 (2) | H11C—C6—H12C | 108 (2) |
N10—N9—N5 | 176.6 (2) | | |
(IV) Triazido[3,3'-diamino-
N-methyldopropylamine]cobalt(III)
top
Crystal data top
[Co(C7H19N3)(N3)3] | Z = 2 |
Mr = 330.27 | F(000) = 344 |
Triclinic, P1 | Dx = 1.579 Mg m−3 |
a = 8.848 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.931 (2) Å | Cell parameters from 25 reflections |
c = 9.606 (3) Å | θ = 8.4–13.5° |
α = 105.98 (2)° | µ = 1.25 mm−1 |
β = 90.51 (4)° | T = 293 K |
γ = 106.99 (3)° | Polyhedra, dark green |
V = 694.6 (5) Å3 | 0.45 × 0.38 × 0.18 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 2066 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.0°, θmin = 2.2° |
ω–2θ scans | h = −10→10 |
Absorption correction: ψ scan (NRCVAX ABSORP; Gabe et al., 1989) | k = 0→10 |
Tmin = 0.666, Tmax = 0.799 | l = −11→10 |
2447 measured reflections | 3 standard reflections every 240 min |
2447 independent reflections | intensity decay: none |
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)] = 0.026 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.066 | All H-atom parameters refined |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0397P)2 + 0.1912P] where P = (Fo2 + 2Fc2)/3 |
2447 reflections | (Δ/σ)max = 0.024 |
257 parameters | Δρmax = 0.32 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
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. |
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_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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co | 0.12819 (3) | 0.78911 (3) | 0.77457 (3) | 0.02682 (10) | |
N1 | 0.0821 (2) | 0.5501 (2) | 0.7337 (2) | 0.0334 (4) | |
H1N | 0.040 (3) | 0.506 (3) | 0.647 (3) | 0.042 (7)* | |
H2N | 0.012 (3) | 0.518 (3) | 0.780 (3) | 0.043 (7)* | |
N2 | 0.3454 (2) | 0.8195 (2) | 0.6862 (2) | 0.0308 (4) | |
N3 | 0.1456 (2) | 1.0239 (2) | 0.8168 (3) | 0.0399 (5) | |
H3N | 0.105 (4) | 1.033 (4) | 0.740 (4) | 0.062 (9)* | |
H4N | 0.081 (4) | 1.037 (4) | 0.875 (3) | 0.062 (10)* | |
N4 | 0.0064 (2) | 0.7357 (2) | 0.5848 (2) | 0.0390 (4) | |
N5 | −0.0682 (2) | 0.7774 (3) | 0.8695 (2) | 0.0467 (5) | |
N6 | 0.2447 (2) | 0.8307 (2) | 0.9617 (2) | 0.0406 (4) | |
N7 | −0.0803 (2) | 0.8105 (2) | 0.5679 (2) | 0.0435 (5) | |
N8 | −0.1668 (3) | 0.8777 (3) | 0.5455 (3) | 0.0777 (8) | |
N9 | −0.1833 (2) | 0.6598 (3) | 0.8233 (2) | 0.0445 (5) | |
N10 | −0.2956 (3) | 0.5510 (3) | 0.7840 (3) | 0.0764 (8) | |
N11 | 0.1756 (2) | 0.7791 (2) | 1.0532 (2) | 0.0450 (5) | |
N12 | 0.1162 (4) | 0.7329 (4) | 1.1452 (3) | 0.0864 (9) | |
C1 | 0.2066 (3) | 0.4746 (3) | 0.7466 (3) | 0.0449 (6) | |
H1C | 0.250 (3) | 0.516 (3) | 0.848 (3) | 0.043 (7)* | |
H2C | 0.162 (3) | 0.361 (3) | 0.718 (3) | 0.040 (6)* | |
C2 | 0.3351 (3) | 0.5220 (3) | 0.6520 (4) | 0.0513 (7) | |
H3C | 0.406 (4) | 0.461 (4) | 0.659 (4) | 0.079 (10)* | |
H4C | 0.293 (3) | 0.496 (3) | 0.560 (3) | 0.046 (8)* | |
C3 | 0.4277 (3) | 0.7008 (3) | 0.7063 (3) | 0.0466 (6) | |
H5C | 0.461 (3) | 0.732 (3) | 0.808 (3) | 0.049 (7)* | |
H6C | 0.527 (4) | 0.729 (4) | 0.662 (3) | 0.067 (9)* | |
C4 | 0.4653 (3) | 0.9821 (3) | 0.7588 (3) | 0.0401 (5) | |
H7C | 0.493 (3) | 0.979 (3) | 0.853 (2) | 0.028 (5)* | |
H8C | 0.558 (3) | 0.987 (3) | 0.708 (3) | 0.048 (7)* | |
C5 | 0.4170 (3) | 1.1327 (3) | 0.7672 (3) | 0.0445 (6) | |
H9C | 0.508 (3) | 1.223 (4) | 0.797 (3) | 0.056 (8)* | |
H10C | 0.380 (3) | 1.131 (3) | 0.678 (3) | 0.046 (7)* | |
C6 | 0.2968 (3) | 1.1528 (3) | 0.8735 (3) | 0.0378 (5) | |
H11C | 0.332 (3) | 1.143 (3) | 0.960 (3) | 0.036 (6)* | |
H12C | 0.276 (3) | 1.259 (3) | 0.893 (3) | 0.041 (6)* | |
C7 | 0.3270 (3) | 0.8014 (4) | 0.5274 (3) | 0.0499 (6) | |
H13C | 0.255 (3) | 0.683 (4) | 0.476 (3) | 0.054 (8)* | |
H14C | 0.284 (3) | 0.887 (4) | 0.514 (3) | 0.057 (8)* | |
H15C | 0.429 (4) | 0.808 (4) | 0.494 (3) | 0.069 (9)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.0237 (2) | 0.0282 (2) | 0.0274 (2) | 0.00577 (11) | 0.00526 (10) | 0.00834 (11) |
N1 | 0.0311 (10) | 0.0321 (10) | 0.0366 (11) | 0.0054 (8) | 0.0064 (9) | 0.0138 (9) |
N2 | 0.0278 (9) | 0.0306 (9) | 0.0325 (9) | 0.0061 (7) | 0.0073 (7) | 0.0095 (7) |
N3 | 0.0343 (11) | 0.0330 (10) | 0.0496 (12) | 0.0099 (8) | 0.0053 (10) | 0.0078 (9) |
N4 | 0.0396 (10) | 0.0421 (11) | 0.0365 (10) | 0.0166 (9) | −0.0025 (8) | 0.0092 (8) |
N5 | 0.0290 (10) | 0.0457 (12) | 0.0495 (12) | 0.0007 (9) | 0.0144 (9) | −0.0004 (9) |
N6 | 0.0379 (10) | 0.0479 (11) | 0.0303 (9) | −0.0002 (9) | 0.0027 (8) | 0.0168 (9) |
N7 | 0.0398 (11) | 0.0388 (11) | 0.0483 (12) | 0.0112 (9) | −0.0074 (9) | 0.0085 (9) |
N8 | 0.071 (2) | 0.062 (2) | 0.102 (2) | 0.0338 (14) | −0.026 (2) | 0.0139 (15) |
N9 | 0.0303 (11) | 0.0465 (12) | 0.0527 (12) | 0.0134 (10) | 0.0127 (9) | 0.0061 (10) |
N10 | 0.0323 (12) | 0.0555 (15) | 0.115 (2) | 0.0014 (11) | 0.0108 (13) | −0.0038 (15) |
N11 | 0.0477 (12) | 0.0449 (11) | 0.0388 (11) | 0.0042 (9) | 0.0030 (9) | 0.0174 (9) |
N12 | 0.086 (2) | 0.114 (2) | 0.069 (2) | 0.010 (2) | 0.022 (2) | 0.064 (2) |
C1 | 0.0492 (14) | 0.0310 (12) | 0.056 (2) | 0.0122 (11) | −0.0051 (12) | 0.0156 (11) |
C2 | 0.0364 (13) | 0.0372 (13) | 0.077 (2) | 0.0139 (11) | 0.0059 (13) | 0.0087 (13) |
C3 | 0.0293 (12) | 0.0433 (14) | 0.067 (2) | 0.0145 (10) | 0.0073 (12) | 0.0124 (13) |
C4 | 0.0295 (12) | 0.0404 (13) | 0.0455 (14) | 0.0018 (10) | 0.0082 (10) | 0.0140 (11) |
C5 | 0.0431 (14) | 0.0345 (12) | 0.0508 (15) | 0.0003 (11) | 0.0091 (11) | 0.0166 (11) |
C6 | 0.0441 (13) | 0.0265 (11) | 0.0377 (12) | 0.0049 (10) | 0.0005 (10) | 0.0077 (9) |
C7 | 0.0461 (15) | 0.063 (2) | 0.0345 (13) | 0.0098 (14) | 0.0152 (11) | 0.0119 (12) |
Geometric parameters (Å, º) top
Co—N6 | 1.951 (2) | N11—N12 | 1.144 (3) |
Co—N5 | 1.958 (2) | C1—C2 | 1.499 (4) |
Co—N4 | 1.974 (2) | C1—H1C | 0.97 (3) |
Co—N1 | 1.976 (2) | C1—H2C | 0.93 (3) |
Co—N3 | 1.982 (2) | C2—C3 | 1.504 (4) |
Co—N2 | 2.083 (2) | C2—H3C | 0.96 (3) |
N1—C1 | 1.470 (3) | C2—H4C | 0.90 (3) |
N1—H1N | 0.84 (3) | C3—H5C | 0.95 (3) |
N1—H2N | 0.80 (3) | C3—H6C | 0.98 (3) |
N2—C7 | 1.492 (3) | C4—C5 | 1.509 (4) |
N2—C4 | 1.500 (3) | C4—H7C | 0.94 (2) |
N2—C3 | 1.501 (3) | C4—H8C | 0.95 (3) |
N3—C6 | 1.467 (3) | C5—C6 | 1.495 (3) |
N3—H3N | 0.85 (3) | C5—H9C | 0.93 (3) |
N3—H4N | 0.81 (3) | C5—H10C | 0.91 (3) |
N4—N7 | 1.192 (3) | C6—H11C | 0.92 (2) |
N5—N9 | 1.203 (3) | C6—H12C | 0.99 (3) |
N6—N11 | 1.195 (3) | C7—H13C | 1.04 (3) |
N7—N8 | 1.152 (3) | C7—H14C | 0.98 (3) |
N9—N10 | 1.140 (3) | C7—H15C | 0.95 (3) |
| | | |
N6—Co—N5 | 89.89 (9) | C2—C1—H1C | 109.6 (15) |
N6—Co—N4 | 177.20 (8) | N1—C1—H2C | 109.4 (15) |
N5—Co—N4 | 89.51 (9) | C2—C1—H2C | 109.3 (15) |
N6—Co—N1 | 91.86 (9) | H1C—C1—H2C | 111 (2) |
N5—Co—N1 | 90.01 (9) | C1—C2—C3 | 111.9 (2) |
N4—Co—N1 | 85.41 (9) | C1—C2—H3C | 106 (2) |
N6—Co—N3 | 90.99 (10) | C3—C2—H3C | 108 (2) |
N5—Co—N3 | 83.45 (10) | C1—C2—H4C | 110.1 (17) |
N4—Co—N3 | 91.65 (10) | C3—C2—H4C | 110.4 (17) |
N1—Co—N3 | 172.86 (8) | H3C—C2—H4C | 111 (3) |
N6—Co—N2 | 87.24 (8) | N2—C3—C2 | 116.8 (2) |
N5—Co—N2 | 175.41 (8) | N2—C3—H5C | 106.1 (16) |
N4—Co—N2 | 93.52 (8) | C2—C3—H5C | 111.2 (16) |
N1—Co—N2 | 93.66 (8) | N2—C3—H6C | 104.6 (18) |
N3—Co—N2 | 93.01 (8) | C2—C3—H6C | 113.2 (18) |
C1—N1—Co | 122.3 (2) | H5C—C3—H6C | 104 (2) |
C1—N1—H1N | 105.4 (17) | N2—C4—C5 | 117.2 (2) |
Co—N1—H1N | 107.7 (17) | N2—C4—H7C | 106.2 (14) |
C1—N1—H2N | 109.0 (19) | C5—C4—H7C | 110.5 (13) |
Co—N1—H2N | 108.2 (19) | N2—C4—H8C | 107.0 (16) |
H1N—N1—H2N | 102 (3) | C5—C4—H8C | 109.2 (16) |
C7—N2—C4 | 108.1 (2) | H7C—C4—H8C | 106 (2) |
C7—N2—C3 | 107.8 (2) | C6—C5—C4 | 111.9 (2) |
C4—N2—C3 | 102.6 (2) | C6—C5—H9C | 109.0 (17) |
C7—N2—Co | 111.6 (2) | C4—C5—H9C | 107.4 (17) |
C4—N2—Co | 113.10 (14) | C6—C5—H10C | 110.4 (17) |
C3—N2—Co | 113.11 (14) | C4—C5—H10C | 111.1 (17) |
C6—N3—Co | 121.5 (2) | H9C—C5—H10C | 107 (2) |
C6—N3—H3N | 112 (2) | N3—C6—C5 | 109.5 (2) |
Co—N3—H3N | 106 (2) | N3—C6—H11C | 109.0 (15) |
C6—N3—H4N | 109 (2) | C5—C6—H11C | 109.0 (15) |
Co—N3—H4N | 104 (2) | N3—C6—H12C | 107.5 (14) |
H3N—N3—H4N | 103 (3) | C5—C6—H12C | 113.4 (14) |
N7—N4—Co | 120.9 (2) | H11C—C6—H12C | 108 (2) |
N9—N5—Co | 119.6 (2) | N2—C7—H13C | 107.5 (15) |
N11—N6—Co | 118.8 (2) | N2—C7—H14C | 108.2 (16) |
N8—N7—N4 | 176.9 (3) | H13C—C7—H14C | 114 (2) |
N10—N9—N5 | 177.2 (2) | N2—C7—H15C | 106.3 (18) |
N12—N11—N6 | 176.6 (3) | H13C—C7—H15C | 106 (2) |
N1—C1—C2 | 110.4 (2) | H14C—C7—H15C | 114 (3) |
N1—C1—H1C | 106.8 (15) | | |
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