Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801012909/bt6068sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801012909/bt6068Isup2.hkl |
CCDC reference: 172187
An aqueous solution (30 ml) of bis(2-pyridyl)amine (0.340 g, 2.0 mmol) was added slowly to an aqueous solution (30 ml) of Co(NO3)2·6H2O (0.290 g, 1.0 mmol) with vigorous stirring. The resulting solution was filtered off to remove impurities and then allowed to stand at room temperature. After two weeks, red crystals were harvested by slow evaporation of the solvent. Crystals were found to be stable to air and X-ray exposure.
H atoms bonded to C atoms were kept fixed at calculated positions with Uiso 20% larger than Ueq for the atoms to which they are attached. H atoms bonded to N atoms were located in difference Fourier maps and refined isotropically.
Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Co(NO3)(C10H9N3)2]NO3 | F(000) = 1076 |
Mr = 525.35 | Dx = 1.611 Mg m−3 Dm = 1.62 (1) Mg m−3 Dm measured by flotation in a mixture of carbon tetrachloride and bromoform |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 14084 reflections |
a = 17.191 (3) Å | θ = 2.5–25.8° |
b = 7.308 (1) Å | µ = 0.85 mm−1 |
c = 17.843 (5) Å | T = 293 K |
β = 104.94 (3)° | Irregular, red |
V = 2165.9 (8) Å3 | 0.42 × 0.20 × 0.08 mm |
Z = 4 |
Stoe IPDS diffractometer | 2598 reflections with I > 2σ(I) |
Radiation source: x-ray tube | Rint = 0.048 |
area detection scans | θmax = 25.8°, θmin = 2.5° |
Absorption correction: numerical (Stoe & Cie, 1998) | h = −21→20 |
Tmin = 0.815, Tmax = 0.934 | k = −8→8 |
14084 measured reflections | l = −21→21 |
4037 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.0787P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.079 | (Δ/σ)max = 0.002 |
S = 1.04 | Δρmax = 0.37 e Å−3 |
4037 reflections | Δρmin = −0.52 e Å−3 |
324 parameters |
[Co(NO3)(C10H9N3)2]NO3 | V = 2165.9 (8) Å3 |
Mr = 525.35 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 17.191 (3) Å | µ = 0.85 mm−1 |
b = 7.308 (1) Å | T = 293 K |
c = 17.843 (5) Å | 0.42 × 0.20 × 0.08 mm |
β = 104.94 (3)° |
Stoe IPDS diffractometer | 4037 independent reflections |
Absorption correction: numerical (Stoe & Cie, 1998) | 2598 reflections with I > 2σ(I) |
Tmin = 0.815, Tmax = 0.934 | Rint = 0.048 |
14084 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.079 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.37 e Å−3 |
4037 reflections | Δρmin = −0.52 e Å−3 |
324 parameters |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
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 _refine_ls_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. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.20807 (2) | 0.99836 (6) | 0.01758 (2) | 0.0231 (1) | |
O1 | 0.2401 (1) | 1.2047 (3) | 0.0839 (1) | 0.0302 (6) | |
O2 | 0.1241 (1) | 1.1759 (3) | 0.0011 (1) | 0.0296 (6) | |
O3 | 0.1475 (1) | 1.4308 (3) | 0.0765 (2) | 0.0323 (9) | |
N1 | 0.1688 (2) | 1.2848 (5) | 0.0557 (2) | 0.0330 (11) | |
N11 | 0.1649 (1) | 0.8898 (3) | 0.0972 (1) | 0.0269 (8) | |
N17 | 0.0453 (1) | 0.8077 (3) | 0.0059 (1) | 0.0290 (8) | |
N19 | 0.1497 (1) | 0.8211 (3) | −0.0577 (1) | 0.0261 (7) | |
N21 | 0.3049 (1) | 0.8520 (3) | 0.0485 (1) | 0.0261 (8) | |
N27 | 0.3826 (1) | 1.1069 (4) | 0.0343 (1) | 0.0297 (9) | |
N29 | 0.2556 (1) | 1.1244 (3) | −0.0551 (1) | 0.0255 (8) | |
C12 | 0.2081 (2) | 0.8977 (5) | 0.1727 (2) | 0.0368 (10) | |
C13 | 0.1765 (2) | 0.8552 (5) | 0.2326 (2) | 0.0473 (13) | |
C14 | 0.0959 (2) | 0.8044 (5) | 0.2165 (2) | 0.0470 (13) | |
C15 | 0.0516 (2) | 0.7920 (5) | 0.1415 (2) | 0.0381 (10) | |
C16 | 0.0886 (2) | 0.8306 (4) | 0.0820 (2) | 0.0284 (9) | |
C18 | 0.0741 (2) | 0.7710 (4) | −0.0574 (2) | 0.0266 (9) | |
C22 | 0.3014 (2) | 0.6730 (4) | 0.0668 (2) | 0.0306 (10) | |
C23 | 0.3682 (2) | 0.5742 (5) | 0.1019 (2) | 0.0357 (10) | |
C24 | 0.4425 (2) | 0.6627 (5) | 0.1216 (2) | 0.0370 (10) | |
C25 | 0.4471 (2) | 0.8403 (5) | 0.1008 (2) | 0.0362 (10) | |
C26 | 0.3775 (2) | 0.9325 (4) | 0.0612 (2) | 0.0258 (9) | |
C28 | 0.3323 (1) | 1.1815 (4) | −0.0317 (2) | 0.0257 (9) | |
C110 | 0.1778 (2) | 0.7693 (4) | −0.1193 (2) | 0.0331 (10) | |
C111 | 0.1311 (2) | 0.6805 (5) | −0.1822 (2) | 0.0401 (11) | |
C112 | 0.0522 (2) | 0.6377 (5) | −0.1830 (2) | 0.0459 (13) | |
C113 | 0.0239 (2) | 0.6816 (5) | −0.1205 (2) | 0.0398 (10) | |
C210 | 0.2102 (2) | 1.1864 (5) | −0.1250 (2) | 0.0333 (10) | |
C211 | 0.2393 (2) | 1.3035 (5) | −0.1703 (2) | 0.0404 (10) | |
C212 | 0.3161 (2) | 1.3741 (5) | −0.1421 (2) | 0.0408 (11) | |
C213 | 0.3628 (2) | 1.3141 (4) | −0.0724 (2) | 0.0339 (10) | |
O4 | 0.5396 (2) | 0.2615 (5) | 0.0725 (2) | 0.0773 (12) | |
O5 | 0.5563 (2) | 0.2595 (5) | 0.1949 (2) | 0.0912 (14) | |
O6 | 0.6385 (2) | 0.1193 (5) | 0.1469 (2) | 0.0789 (13) | |
N2 | 0.5787 (1) | 0.2134 (4) | 0.1384 (2) | 0.0421 (10) | |
H12 | 0.262 | 0.934 | 0.184 | 0.044* | |
H13 | 0.208 | 0.860 | 0.284 | 0.057* | |
H14 | 0.072 | 0.779 | 0.257 | 0.056* | |
H15 | −0.002 | 0.759 | 0.130 | 0.046* | |
H17 | −0.000 (2) | 0.784 (4) | −0.001 (2) | 0.027 (7)* | |
H22 | 0.252 | 0.615 | 0.055 | 0.037* | |
H23 | 0.364 | 0.450 | 0.112 | 0.043* | |
H24 | 0.488 | 0.601 | 0.149 | 0.044* | |
H25 | 0.497 | 0.900 | 0.113 | 0.043* | |
H27 | 0.429 (2) | 1.151 (5) | 0.045 (2) | 0.043 (9)* | |
H110 | 0.231 | 0.796 | −0.118 | 0.040* | |
H111 | 0.152 | 0.649 | −0.224 | 0.048* | |
H112 | 0.019 | 0.580 | −0.226 | 0.055* | |
H113 | −0.029 | 0.652 | −0.120 | 0.048* | |
H210 | 0.157 | 1.147 | −0.142 | 0.040* | |
H211 | 0.208 | 1.336 | −0.219 | 0.049* | |
H212 | 0.336 | 1.462 | −0.170 | 0.049* | |
H213 | 0.414 | 1.361 | −0.052 | 0.041* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0168 (2) | 0.0257 (2) | 0.0270 (2) | −0.0020 (2) | 0.0059 (1) | −0.0018 (2) |
O1 | 0.020 (1) | 0.034 (1) | 0.036 (1) | −0.006 (1) | 0.006 (1) | −0.008 (1) |
O2 | 0.019 (1) | 0.029 (1) | 0.039 (1) | −0.002 (1) | 0.004 (1) | −0.004 (1) |
O3 | 0.027 (1) | 0.025 (2) | 0.045 (2) | −0.000 (1) | 0.005 (1) | −0.002 (1) |
N1 | 0.024 (2) | 0.032 (2) | 0.043 (2) | −0.010 (2) | 0.005 (1) | −0.001 (2) |
N11 | 0.022 (1) | 0.031 (2) | 0.028 (1) | 0.001 (1) | 0.008 (1) | −0.002 (1) |
N17 | 0.016 (1) | 0.037 (2) | 0.035 (1) | −0.005 (1) | 0.008 (1) | −0.004 (1) |
N19 | 0.024 (1) | 0.027 (2) | 0.028 (1) | −0.001 (1) | 0.008 (1) | −0.002 (1) |
N21 | 0.022 (1) | 0.028 (2) | 0.029 (1) | −0.001 (1) | 0.007 (1) | 0.001 (1) |
N27 | 0.018 (1) | 0.032 (2) | 0.037 (1) | −0.005 (1) | 0.003 (1) | 0.003 (1) |
N29 | 0.021 (1) | 0.026 (2) | 0.030 (1) | 0.001 (1) | 0.007 (1) | −0.002 (1) |
C12 | 0.031 (2) | 0.048 (2) | 0.030 (2) | −0.001 (1) | 0.005 (1) | −0.003 (1) |
C13 | 0.049 (2) | 0.065 (3) | 0.028 (2) | −0.001 (2) | 0.011 (1) | 0.000 (2) |
C14 | 0.054 (2) | 0.058 (3) | 0.037 (2) | −0.008 (2) | 0.025 (2) | 0.001 (2) |
C15 | 0.032 (2) | 0.042 (2) | 0.045 (2) | −0.008 (1) | 0.020 (1) | −0.004 (2) |
C16 | 0.026 (1) | 0.024 (2) | 0.036 (2) | 0.000 (1) | 0.010 (1) | −0.001 (1) |
C18 | 0.023 (1) | 0.024 (2) | 0.032 (1) | −0.001 (1) | 0.005 (1) | 0.002 (1) |
C22 | 0.027 (1) | 0.029 (2) | 0.037 (2) | −0.005 (1) | 0.010 (1) | 0.001 (1) |
C23 | 0.041 (2) | 0.030 (2) | 0.039 (2) | 0.003 (1) | 0.015 (1) | 0.003 (1) |
C24 | 0.031 (2) | 0.039 (2) | 0.040 (2) | 0.010 (1) | 0.006 (1) | 0.009 (1) |
C25 | 0.023 (1) | 0.039 (2) | 0.044 (2) | 0.000 (1) | 0.003 (1) | 0.003 (1) |
C26 | 0.024 (1) | 0.026 (2) | 0.028 (1) | −0.002 (1) | 0.008 (1) | −0.002 (1) |
C28 | 0.021 (1) | 0.027 (2) | 0.030 (1) | −0.001 (1) | 0.009 (1) | −0.002 (1) |
C110 | 0.033 (2) | 0.033 (2) | 0.036 (2) | 0.001 (1) | 0.015 (1) | −0.002 (1) |
C111 | 0.050 (2) | 0.037 (2) | 0.034 (2) | −0.002 (2) | 0.013 (1) | −0.003 (1) |
C112 | 0.050 (2) | 0.046 (3) | 0.036 (2) | −0.011 (2) | 0.000 (1) | −0.012 (2) |
C113 | 0.030 (2) | 0.045 (2) | 0.041 (2) | −0.009 (1) | 0.005 (1) | −0.004 (2) |
C210 | 0.026 (1) | 0.038 (2) | 0.033 (2) | 0.002 (1) | 0.001 (1) | −0.002 (1) |
C211 | 0.047 (2) | 0.042 (2) | 0.030 (2) | 0.004 (2) | 0.007 (1) | 0.007 (1) |
C212 | 0.049 (2) | 0.037 (2) | 0.041 (2) | −0.002 (2) | 0.018 (1) | 0.010 (2) |
C213 | 0.029 (1) | 0.033 (2) | 0.047 (2) | −0.005 (1) | 0.014 (1) | −0.001 (1) |
O4 | 0.052 (2) | 0.106 (3) | 0.059 (2) | −0.028 (2) | −0.013 (1) | 0.032 (2) |
O5 | 0.081 (2) | 0.130 (3) | 0.077 (2) | 0.042 (2) | 0.047 (2) | 0.018 (2) |
O6 | 0.059 (2) | 0.102 (3) | 0.070 (2) | 0.035 (2) | 0.006 (1) | −0.020 (2) |
N2 | 0.027 (1) | 0.048 (2) | 0.049 (2) | −0.011 (1) | 0.005 (1) | 0.001 (1) |
Co1—O1 | 1.909 (2) | C15—C16 | 1.399 (4) |
Co1—O2 | 1.907 (2) | C18—C113 | 1.392 (4) |
Co1—N11 | 1.935 (2) | C22—C23 | 1.365 (4) |
Co1—N19 | 1.947 (2) | C23—C24 | 1.393 (4) |
Co1—N21 | 1.935 (2) | C24—C25 | 1.358 (5) |
Co1—N29 | 1.935 (2) | C25—C26 | 1.396 (4) |
O1—N1 | 1.335 (4) | C28—C213 | 1.392 (4) |
O2—N1 | 1.337 (4) | C110—C111 | 1.364 (4) |
O3—N1 | 1.216 (4) | C111—C112 | 1.390 (5) |
O4—N2 | 1.246 (4) | C112—C113 | 1.363 (4) |
O5—N2 | 1.215 (4) | C12—H12 | 0.93 |
O6—N2 | 1.213 (4) | C13—H13 | 0.93 |
N11—C16 | 1.341 (3) | C14—H14 | 0.93 |
N11—C12 | 1.361 (3) | C15—H15 | 0.93 |
N17—C16 | 1.379 (3) | C22—H22 | 0.93 |
N17—C18 | 1.373 (3) | C23—H23 | 0.93 |
N19—C18 | 1.351 (3) | C24—H24 | 0.93 |
N19—C110 | 1.364 (4) | C25—H25 | 0.93 |
N21—C22 | 1.353 (4) | C210—C211 | 1.359 (5) |
N21—C26 | 1.346 (3) | C110—H110 | 0.93 |
N27—C26 | 1.373 (4) | C211—C212 | 1.386 (5) |
N27—C28 | 1.381 (4) | C111—H111 | 0.93 |
N29—C210 | 1.366 (4) | C212—C213 | 1.367 (4) |
N29—C28 | 1.343 (3) | C112—H112 | 0.93 |
N17—H17 | 0.78 (3) | C113—H113 | 0.93 |
N27—H27 | 0.84 (3) | C210—H210 | 0.93 |
C12—C13 | 1.354 (4) | C211—H211 | 0.93 |
C13—C14 | 1.390 (5) | C212—H212 | 0.93 |
C14—C15 | 1.362 (4) | C213—H213 | 0.93 |
O1—Co1—O2 | 69.15 (9) | N21—C22—C23 | 122.5 (3) |
O1—Co1—N11 | 88.41 (9) | C22—C23—C24 | 118.6 (3) |
O1—Co1—N19 | 165.50 (9) | C23—C24—C25 | 119.3 (3) |
O1—Co1—N21 | 99.81 (9) | C24—C25—C26 | 119.8 (3) |
O1—Co1—N29 | 86.31 (9) | N27—C26—C25 | 120.1 (3) |
O2—Co1—N11 | 88.49 (9) | N21—C26—N27 | 119.1 (2) |
O2—Co1—N19 | 96.38 (9) | N21—C26—C25 | 120.8 (3) |
O2—Co1—N21 | 168.95 (9) | N27—C28—N29 | 119.4 (2) |
O2—Co1—N29 | 90.37 (9) | N27—C28—C213 | 118.9 (2) |
N11—Co1—N19 | 90.37 (9) | N29—C28—C213 | 121.7 (2) |
N11—Co1—N21 | 91.61 (9) | N19—C110—C111 | 122.7 (3) |
N11—Co1—N29 | 174.66 (9) | C110—C111—C112 | 118.7 (3) |
N19—Co1—N21 | 94.67 (9) | N11—C12—H12 | 119 |
N19—Co1—N29 | 94.94 (9) | C13—C12—H12 | 119 |
N21—Co1—N29 | 88.51 (9) | C111—C112—C113 | 119.5 (3) |
Co1—O1—N1 | 91.29 (18) | C12—C13—H13 | 121 |
Co1—O2—N1 | 91.28 (17) | C18—C113—C112 | 119.6 (3) |
O1—N1—O2 | 108.3 (3) | C14—C13—H13 | 121 |
O1—N1—O3 | 126.1 (3) | C15—C14—H14 | 120 |
O2—N1—O3 | 125.6 (3) | C13—C14—H14 | 120 |
Co1—N11—C12 | 119.65 (19) | C16—C15—H15 | 121 |
Co1—N11—C16 | 121.58 (18) | C14—C15—H15 | 121 |
C12—N11—C16 | 118.0 (2) | C23—C22—H22 | 119 |
C16—N17—C18 | 128.0 (2) | N21—C22—H22 | 119 |
Co1—N19—C18 | 120.2 (2) | C22—C23—H23 | 121 |
Co1—N19—C110 | 120.9 (2) | C24—C23—H23 | 121 |
C18—N19—C110 | 117.9 (2) | C25—C24—H24 | 120 |
Co1—N21—C22 | 121.0 (2) | C23—C24—H24 | 120 |
Co1—N21—C26 | 119.9 (2) | C26—C25—H25 | 120 |
C22—N21—C26 | 118.6 (2) | C24—C25—H25 | 120 |
C26—N27—C28 | 125.7 (3) | N29—C210—C211 | 122.7 (3) |
Co1—N29—C28 | 119.3 (2) | N19—C110—H110 | 119 |
Co1—N29—C210 | 121.9 (2) | C111—C110—H110 | 119 |
C28—N29—C210 | 117.7 (2) | C112—C111—H111 | 121 |
C18—N17—H17 | 113 (2) | C210—C211—C212 | 118.7 (3) |
C16—N17—H17 | 117 (2) | C110—C111—H111 | 121 |
C26—N27—H27 | 115 (2) | C113—C112—H112 | 120 |
C28—N27—H27 | 113 (2) | C211—C212—C213 | 119.5 (3) |
O4—N2—O6 | 120.7 (3) | C111—C112—H112 | 120 |
O4—N2—O5 | 119.7 (3) | C28—C213—C212 | 119.1 (3) |
O5—N2—O6 | 119.6 (3) | C18—C113—H113 | 120 |
N11—C12—C13 | 122.9 (3) | C112—C113—H113 | 120 |
C12—C13—C14 | 118.6 (3) | N29—C210—H210 | 119 |
C13—C14—C15 | 119.7 (3) | C211—C210—H210 | 119 |
C14—C15—C16 | 119.0 (3) | C212—C211—H211 | 121 |
N17—C16—C15 | 119.1 (2) | C210—C211—H211 | 121 |
N11—C16—C15 | 121.5 (2) | C211—C212—H212 | 120 |
N11—C16—N17 | 119.4 (2) | C213—C212—H212 | 120 |
N19—C18—C113 | 121.4 (2) | C28—C213—H213 | 120 |
N17—C18—C113 | 118.5 (2) | C212—C213—H213 | 121 |
N17—C18—N19 | 120.1 (2) | ||
O2—Co1—O1—N1 | 0.81 (16) | Co1—N11—C16—C15 | −165.0 (2) |
N11—Co1—O1—N1 | −88.18 (17) | C12—N11—C16—N17 | −175.0 (3) |
N21—Co1—O1—N1 | −179.55 (17) | C12—N11—C16—C15 | 5.2 (4) |
N29—Co1—O1—N1 | 92.61 (17) | C18—N17—C16—N11 | 26.6 (4) |
O1—Co1—O2—N1 | −0.80 (16) | C18—N17—C16—C15 | −153.6 (3) |
N11—Co1—O2—N1 | 88.07 (17) | C16—N17—C18—N19 | −25.7 (4) |
N19—Co1—O2—N1 | 178.27 (17) | C16—N17—C18—C113 | 154.2 (3) |
N29—Co1—O2—N1 | −86.72 (17) | Co1—N19—C18—N17 | −16.0 (3) |
O1—Co1—N11—C12 | −43.5 (2) | Co1—N19—C18—C113 | 164.1 (2) |
O1—Co1—N11—C16 | 126.5 (2) | C110—N19—C18—N17 | 175.1 (2) |
O2—Co1—N11—C12 | −112.7 (2) | C110—N19—C18—C113 | −4.8 (4) |
O2—Co1—N11—C16 | 57.3 (2) | Co1—N19—C110—C111 | −164.4 (2) |
N19—Co1—N11—C12 | 150.9 (2) | C18—N19—C110—C111 | 4.4 (4) |
N19—Co1—N11—C16 | −39.1 (2) | Co1—N21—C22—C23 | −168.0 (2) |
N21—Co1—N11—C12 | 56.3 (2) | C26—N21—C22—C23 | 4.1 (4) |
N21—Co1—N11—C16 | −133.8 (2) | Co1—N21—C26—N27 | −15.8 (3) |
O2—Co1—N19—C18 | −49.1 (2) | Co1—N21—C26—C25 | 164.6 (2) |
O2—Co1—N19—C110 | 119.4 (2) | C22—N21—C26—N27 | 172.1 (2) |
N11—Co1—N19—C18 | 39.4 (2) | C22—N21—C26—C25 | −7.6 (4) |
N11—Co1—N19—C110 | −152.1 (2) | C28—N27—C26—N21 | −31.7 (4) |
N21—Co1—N19—C18 | 131.0 (2) | C28—N27—C26—C25 | 148.0 (3) |
N21—Co1—N19—C110 | −60.4 (2) | C26—N27—C28—N29 | 30.2 (4) |
N29—Co1—N19—C18 | −140.1 (2) | C26—N27—C28—C213 | −149.6 (3) |
N29—Co1—N19—C110 | 28.5 (2) | Co1—N29—C28—N27 | 18.4 (3) |
O1—Co1—N21—C22 | 130.6 (2) | Co1—N29—C28—C213 | −161.8 (2) |
O1—Co1—N21—C26 | −41.3 (2) | C210—N29—C28—N27 | −173.1 (3) |
N11—Co1—N21—C22 | 41.9 (2) | C210—N29—C28—C213 | 6.8 (4) |
N11—Co1—N21—C26 | −130.0 (2) | Co1—N29—C210—C211 | 167.5 (3) |
N19—Co1—N21—C22 | −48.6 (2) | C28—N29—C210—C211 | −0.8 (5) |
N19—Co1—N21—C26 | 139.5 (2) | N11—C12—C13—C14 | −1.2 (5) |
N29—Co1—N21—C22 | −143.4 (2) | C12—C13—C14—C15 | 2.4 (5) |
N29—Co1—N21—C26 | 44.7 (2) | C13—C14—C15—C16 | 0.1 (6) |
O1—Co1—N29—C28 | 54.1 (2) | C14—C15—C16—N11 | −4.0 (5) |
O1—Co1—N29—C210 | −113.9 (2) | C14—C15—C16—N17 | 176.2 (3) |
O2—Co1—N29—C28 | 123.2 (2) | N17—C18—C113—C112 | −177.6 (3) |
O2—Co1—N29—C210 | −44.9 (2) | N19—C18—C113—C112 | 2.3 (5) |
N19—Co1—N29—C28 | −140.4 (2) | N21—C22—C23—C24 | 1.9 (4) |
N19—Co1—N29—C210 | 51.6 (2) | C22—C23—C24—C25 | −4.5 (4) |
N21—Co1—N29—C28 | −45.8 (2) | C23—C24—C25—C26 | 1.1 (4) |
N21—Co1—N29—C210 | 146.1 (2) | C24—C25—C26—N27 | −174.6 (3) |
Co1—O1—N1—O2 | −1.1 (2) | C24—C25—C26—N21 | 5.1 (4) |
Co1—O1—N1—O3 | 178.2 (3) | N29—C28—C213—C212 | −6.9 (4) |
Co1—O2—N1—O1 | 1.1 (2) | N27—C28—C213—C212 | 173.0 (3) |
Co1—O2—N1—O3 | −178.2 (3) | N29—C210—C211—C212 | −5.1 (5) |
Co1—N11—C12—C13 | 167.8 (3) | C210—C211—C212—C213 | 4.9 (5) |
C16—N11—C12—C13 | −2.6 (5) | C211—C212—C213—C28 | 0.8 (5) |
Co1—N11—C16—N17 | 14.8 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
N17—H17···O2i | 0.78 (3) | 2.15 (3) | 2.884 (3) | 157 (3) |
N27—H27···O4ii | 0.84 (3) | 2.00 (3) | 2.842 (4) | 179 (3) |
C13—H13···O1iii | 0.93 | 2.57 | 3.400 (4) | 149 |
C14—H14···O5iv | 0.93 | 2.57 | 3.404 (5) | 148 |
C22—H22···O3v | 0.93 | 2.35 | 3.224 (4) | 157 |
C110—H110···O6vi | 0.93 | 2.51 | 3.418 (4) | 167 |
C113—H113···O3i | 0.93 | 2.44 | 3.343 (4) | 163 |
C211—H211···O6vii | 0.93 | 2.40 | 3.324 (4) | 171 |
Symmetry codes: (i) −x, −y+2, −z; (ii) x, y+1, z; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x, y−1, z; (vi) −x+1, −y+1, −z; (vii) x−1/2, −y+3/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(NO3)(C10H9N3)2]NO3 |
Mr | 525.35 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 17.191 (3), 7.308 (1), 17.843 (5) |
β (°) | 104.94 (3) |
V (Å3) | 2165.9 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.85 |
Crystal size (mm) | 0.42 × 0.20 × 0.08 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Numerical (Stoe & Cie, 1998) |
Tmin, Tmax | 0.815, 0.934 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14084, 4037, 2598 |
Rint | 0.048 |
(sin θ/λ)max (Å−1) | 0.613 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.079, 1.04 |
No. of reflections | 4037 |
No. of parameters | 324 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.37, −0.52 |
Computer programs: IPDS Software (Stoe & Cie, 1998), IPDS Software, SIR92 (Altomare et al., 1993), SHELXL93 (Sheldrick, 1993), ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).
Co1—O1 | 1.909 (2) | O1—N1 | 1.335 (4) |
Co1—O2 | 1.907 (2) | O2—N1 | 1.337 (4) |
Co1—N11 | 1.935 (2) | O3—N1 | 1.216 (4) |
Co1—N19 | 1.947 (2) | O4—N2 | 1.246 (4) |
Co1—N21 | 1.935 (2) | O5—N2 | 1.215 (4) |
Co1—N29 | 1.935 (2) | O6—N2 | 1.213 (4) |
O1—Co1—O2 | 69.15 (9) | N11—Co1—N29 | 174.66 (9) |
O1—Co1—N11 | 88.41 (9) | N19—Co1—N21 | 94.67 (9) |
O1—Co1—N19 | 165.50 (9) | N19—Co1—N29 | 94.94 (9) |
O1—Co1—N21 | 99.81 (9) | N21—Co1—N29 | 88.51 (9) |
O1—Co1—N29 | 86.31 (9) | O1—N1—O2 | 108.3 (3) |
O2—Co1—N11 | 88.49 (9) | O1—N1—O3 | 126.1 (3) |
O2—Co1—N19 | 96.38 (9) | O2—N1—O3 | 125.6 (3) |
O2—Co1—N21 | 168.95 (9) | O4—N2—O6 | 120.7 (3) |
O2—Co1—N29 | 90.37 (9) | O4—N2—O5 | 119.7 (3) |
N11—Co1—N19 | 90.37 (9) | O5—N2—O6 | 119.6 (3) |
N11—Co1—N21 | 91.61 (9) |
D—H···A | D—H | H···A | D···A | D—H···A |
N17—H17···O2i | 0.78 (3) | 2.15 (3) | 2.884 (3) | 157 (3) |
N27—H27···O4ii | 0.84 (3) | 2.00 (3) | 2.842 (4) | 179 (3) |
C13—H13···O1iii | 0.93 | 2.57 | 3.400 (4) | 149 |
C14—H14···O5iv | 0.93 | 2.57 | 3.404 (5) | 148 |
C22—H22···O3v | 0.93 | 2.35 | 3.224 (4) | 157 |
C110—H110···O6vi | 0.93 | 2.51 | 3.418 (4) | 167 |
C113—H113···O3i | 0.93 | 2.44 | 3.343 (4) | 163 |
C211—H211···O6vii | 0.93 | 2.40 | 3.324 (4) | 171 |
Symmetry codes: (i) −x, −y+2, −z; (ii) x, y+1, z; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x, y−1, z; (vi) −x+1, −y+1, −z; (vii) x−1/2, −y+3/2, z−1/2. |
During our studies of first-row transition metal complexes with N-donor aromatic ligands (Castillo et al., 2001; Castillo et al., 2000), we have obtained the compound [bis(2-pyridyl)amine-N,N'](nitrato-O,O')cobalt(II) nitrate, (I).
Ligands containing aromatic nitrogen heterocycles play an important role in the molecular self-assembling process that leads to supramolecular architectures (Jones, 1998). The crystal structure of (I) comprises discrete [Co(NO3)(C10H9N3)2]+ cations and NO3- anions. The CoII centre is six-coordinated by four pyridinic N atoms of two bis(2-pyridyl)amine moieties and by two O atoms of a bidentate nitrate anion, as shown in Fig. 1. The bidentate bis(2-pyridyl)amine ligands chelate the CoII atom to form two six-membered coordination rings. The Co—N bond distances range from 1.935 (2) to 1.948 (2) Å. The pyridine rings in the same ligand are in the normal trans–trans mode (Du et al., 2001) and the dihedral angles are 27.7 (1) and 37.4 (1)°, respectively. The nitrate ligand is coordinated with two almost equivalent Co—O bond distances, 1.907 (2) and 1.908 (2) Å. The main distortion of the octahedral geometry is due to the small O—Co—O bite angle [69.15 (8)°] of the bidentate nitrate anion. The N—O bond distance involving the uncoordinated O atom of the nitrato ligand is significantly shorter than those for the coordinated O atoms, but is similar to ones of the nitrate anion.
In the crystal structure of (I), the cations and nitrate anions are held together by means of an extensive network of N—H···O and C—H···O hydrogen bonds (Fig. 2).