Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807055584/tk2213sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807055584/tk2213Isup2.hkl |
CCDC reference: 672666
Ethyl carbazate (0.208 g, 0.002 mol) was added to an aqueous solution (25 ml) containing formic acid (85%, 0.08 ml). To this solution was added cobalt nitrate hexahydrate (0.291 g, 0.001 mol) dissolved in doubly distilled water (50 ml). The resulting pink solution was concentrated over a water bath to about 15 ml and kept for crystallization at room temperature. Pink blocks of (I) obtained after a week were separated and washed with ethanol and air dried.
The C18/C19 and C28/C29 ethyl side chains of the ligands are disordered in 0.712 (10):0.288 (10) and 0.612 (7):0.388 (8) ratios, respectively. The H atoms were geometrically placed (N—H = 0.88–0.92 Å, C—H = 0.98–0.99 Å) and refined as riding with Uiso(H) = 1.2Ueq(N,C) or 1.5Ueq(methyl C).
Data collection: COLLECT (Nonius, 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO (Otwinowski & Minor 1997), HKL SCALEPACK (Otwinowski & Minor 1997) and SORTAV (Blessing 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Co(C3H8N2O2)3](NO3)2 | F(000) = 4112 |
Mr = 495.29 | Dx = 1.626 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 19276 reflections |
a = 28.0291 (6) Å | θ = 2.9–27.5° |
b = 8.6245 (2) Å | µ = 0.92 mm−1 |
c = 35.6763 (7) Å | T = 120 K |
β = 110.2445 (5)° | Block, pink |
V = 8091.5 (3) Å3 | 0.44 × 0.40 × 0.28 mm |
Z = 16 |
Nonius KappaCCD diffractometer | 18519 independent reflections |
Radiation source: fine-focus sealed tube | 14049 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
ω and ϕ scans | θmax = 27.5°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2003) | h = −36→36 |
Tmin = 0.687, Tmax = 0.784 | k = −10→11 |
86674 measured reflections | l = −46→46 |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0347P)2 + 4.8866P] where P = (Fo2 + 2Fc2)/3 |
18519 reflections | (Δ/σ)max = 0.003 |
1128 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
[Co(C3H8N2O2)3](NO3)2 | V = 8091.5 (3) Å3 |
Mr = 495.29 | Z = 16 |
Monoclinic, P21/n | Mo Kα radiation |
a = 28.0291 (6) Å | µ = 0.92 mm−1 |
b = 8.6245 (2) Å | T = 120 K |
c = 35.6763 (7) Å | 0.44 × 0.40 × 0.28 mm |
β = 110.2445 (5)° |
Nonius KappaCCD diffractometer | 18519 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2003) | 14049 reflections with I > 2σ(I) |
Tmin = 0.687, Tmax = 0.784 | Rint = 0.049 |
86674 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.60 e Å−3 |
18519 reflections | Δρmin = −0.53 e Å−3 |
1128 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 | 0.378517 (10) | 0.22555 (3) | 0.109456 (8) | 0.01724 (7) | |
C11 | 0.43324 (8) | 0.5019 (2) | 0.13542 (7) | 0.0232 (5) | |
C12 | 0.49470 (10) | 0.6426 (3) | 0.11677 (9) | 0.0451 (7) | |
H12A | 0.5016 | 0.5411 | 0.1067 | 0.054* | |
H12B | 0.5277 | 0.6931 | 0.1312 | 0.054* | |
C13 | 0.46476 (12) | 0.7405 (4) | 0.08305 (9) | 0.0523 (8) | |
H13A | 0.4845 | 0.7606 | 0.0656 | 0.078* | |
H13B | 0.4568 | 0.8390 | 0.0932 | 0.078* | |
H13C | 0.4331 | 0.6870 | 0.0679 | 0.078* | |
N11 | 0.36718 (6) | 0.3885 (2) | 0.15178 (5) | 0.0209 (4) | |
H11A | 0.3370 | 0.4408 | 0.1405 | 0.025* | |
H11B | 0.3664 | 0.3374 | 0.1742 | 0.025* | |
N12 | 0.40882 (6) | 0.4933 (2) | 0.16183 (5) | 0.0220 (4) | |
H12 | 0.4180 | 0.5489 | 0.1839 | 0.026* | |
O11 | 0.42745 (5) | 0.40812 (17) | 0.10801 (4) | 0.0234 (3) | |
O12 | 0.46638 (6) | 0.61959 (19) | 0.14385 (5) | 0.0357 (4) | |
C14 | 0.34850 (8) | 0.1177 (2) | 0.03016 (6) | 0.0202 (4) | |
C15 | 0.37987 (9) | −0.0675 (3) | −0.00506 (7) | 0.0314 (5) | |
H15A | 0.3648 | −0.1400 | −0.0276 | 0.038* | |
H15B | 0.3904 | −0.1285 | 0.0200 | 0.038* | |
C16 | 0.42593 (10) | 0.0086 (3) | −0.00952 (9) | 0.0456 (7) | |
H16A | 0.4504 | −0.0712 | −0.0104 | 0.068* | |
H16B | 0.4416 | 0.0776 | 0.0132 | 0.068* | |
H16C | 0.4157 | 0.0688 | −0.0343 | 0.068* | |
N13 | 0.31313 (7) | 0.3000 (2) | 0.06174 (5) | 0.0212 (4) | |
H13D | 0.2844 | 0.2865 | 0.0683 | 0.025* | |
H13E | 0.3159 | 0.4035 | 0.0565 | 0.025* | |
N14 | 0.30982 (7) | 0.2100 (2) | 0.02783 (5) | 0.0241 (4) | |
H14 | 0.2829 | 0.2151 | 0.0059 | 0.029* | |
O13 | 0.38688 (5) | 0.10170 (17) | 0.06084 (4) | 0.0219 (3) | |
O14 | 0.34184 (6) | 0.04539 (18) | −0.00426 (4) | 0.0264 (3) | |
C17 | 0.42888 (8) | −0.0037 (3) | 0.16649 (6) | 0.0237 (5) | |
C18A | 0.51489 (11) | −0.0781 (6) | 0.20164 (14) | 0.0274 (12) | 0.712 (10) |
H18A | 0.5224 | 0.0232 | 0.1918 | 0.033* | 0.712 (10) |
H18B | 0.5265 | −0.1616 | 0.1878 | 0.033* | 0.712 (10) |
C19A | 0.5410 (2) | −0.0904 (9) | 0.24591 (15) | 0.0488 (16) | 0.712 (10) |
H19A | 0.5779 | −0.0896 | 0.2522 | 0.073* | 0.712 (10) |
H19B | 0.5310 | −0.1874 | 0.2555 | 0.073* | 0.712 (10) |
H19C | 0.5312 | −0.0024 | 0.2590 | 0.073* | 0.712 (10) |
C18B | 0.5134 (3) | −0.0007 (14) | 0.2175 (3) | 0.023 (3) | 0.288 (10) |
H18C | 0.5268 | 0.0520 | 0.1985 | 0.028* | 0.288 (10) |
H18D | 0.5085 | 0.0765 | 0.2363 | 0.028* | 0.288 (10) |
C19B | 0.5477 (6) | −0.1283 (17) | 0.2390 (4) | 0.031 (3)* | 0.288 (10) |
H19D | 0.5816 | −0.0863 | 0.2534 | 0.046* | 0.288 (10) |
H19E | 0.5500 | −0.2063 | 0.2197 | 0.046* | 0.288 (10) |
H19F | 0.5341 | −0.1763 | 0.2581 | 0.046* | 0.288 (10) |
N15 | 0.34325 (6) | 0.03124 (19) | 0.12700 (5) | 0.0185 (4) | |
H15C | 0.3199 | 0.0653 | 0.1380 | 0.022* | |
H15D | 0.3266 | −0.0290 | 0.1051 | 0.022* | |
N16 | 0.38162 (6) | −0.0566 (2) | 0.15541 (5) | 0.0221 (4) | |
H16 | 0.3744 | −0.1432 | 0.1653 | 0.026* | |
O15 | 0.44102 (5) | 0.11584 (18) | 0.15282 (5) | 0.0293 (4) | |
O16 | 0.46121 (6) | −0.0928 (2) | 0.19427 (5) | 0.0350 (4) | |
Co2 | 0.661707 (10) | 0.76084 (3) | 0.155900 (8) | 0.01657 (7) | |
C21 | 0.66557 (8) | 0.6839 (2) | 0.08018 (6) | 0.0198 (4) | |
C22 | 0.62819 (9) | 0.4910 (3) | 0.03125 (7) | 0.0316 (5) | |
H22A | 0.6276 | 0.4297 | 0.0546 | 0.038* | |
H22B | 0.6412 | 0.4235 | 0.0145 | 0.038* | |
C23 | 0.57506 (11) | 0.5427 (3) | 0.00744 (8) | 0.0499 (7) | |
H23A | 0.5535 | 0.4516 | −0.0025 | 0.075* | |
H23B | 0.5757 | 0.6060 | −0.0152 | 0.075* | |
H23C | 0.5614 | 0.6040 | 0.0245 | 0.075* | |
N21 | 0.70996 (7) | 0.8665 (2) | 0.12868 (5) | 0.0210 (4) | |
H21A | 0.7032 | 0.9710 | 0.1254 | 0.025* | |
H21B | 0.7435 | 0.8538 | 0.1446 | 0.025* | |
N22 | 0.70081 (7) | 0.7952 (2) | 0.09118 (5) | 0.0237 (4) | |
H22 | 0.7177 | 0.8232 | 0.0756 | 0.028* | |
O21 | 0.63925 (5) | 0.64307 (16) | 0.10010 (4) | 0.0201 (3) | |
O22 | 0.66203 (6) | 0.62304 (17) | 0.04504 (4) | 0.0266 (3) | |
C24 | 0.60653 (8) | 1.0327 (2) | 0.15778 (6) | 0.0202 (4) | |
C25 | 0.53594 (8) | 1.1650 (3) | 0.11072 (7) | 0.0299 (5) | |
H25A | 0.5042 | 1.2116 | 0.1120 | 0.036* | |
H25B | 0.5276 | 1.0615 | 0.0981 | 0.036* | |
C26 | 0.55730 (10) | 1.2659 (3) | 0.08614 (7) | 0.0361 (6) | |
H26A | 0.5315 | 1.2819 | 0.0597 | 0.054* | |
H26B | 0.5871 | 1.2155 | 0.0832 | 0.054* | |
H26C | 0.5672 | 1.3662 | 0.0994 | 0.054* | |
N23 | 0.68026 (6) | 0.9259 (2) | 0.20469 (5) | 0.0207 (4) | |
H23D | 0.6828 | 0.8763 | 0.2281 | 0.025* | |
H23E | 0.7108 | 0.9734 | 0.2079 | 0.025* | |
N24 | 0.64041 (7) | 1.0370 (2) | 0.19474 (5) | 0.0210 (4) | |
H24 | 0.6382 | 1.1059 | 0.2123 | 0.025* | |
O23 | 0.60516 (5) | 0.93140 (17) | 0.13296 (4) | 0.0220 (3) | |
O24 | 0.57298 (6) | 1.14897 (19) | 0.15107 (5) | 0.0301 (4) | |
C27 | 0.63903 (8) | 0.5134 (3) | 0.19850 (7) | 0.0260 (5) | |
C28A | 0.5735 (2) | 0.4775 (7) | 0.22683 (19) | 0.0322 (13) | 0.612 (7) |
H28A | 0.5835 | 0.4955 | 0.2559 | 0.039* | 0.612 (7) |
H28B | 0.5613 | 0.5764 | 0.2127 | 0.039* | 0.612 (7) |
C29A | 0.53289 (15) | 0.3553 (5) | 0.21343 (12) | 0.0339 (13) | 0.612 (7) |
H29A | 0.5025 | 0.3908 | 0.2186 | 0.051* | 0.612 (7) |
H29B | 0.5453 | 0.2591 | 0.2282 | 0.051* | 0.612 (7) |
H29C | 0.5243 | 0.3365 | 0.1848 | 0.051* | 0.612 (7) |
C28B | 0.5622 (3) | 0.4169 (10) | 0.2051 (3) | 0.048 (2) | 0.388 (7) |
H28C | 0.5450 | 0.4571 | 0.1778 | 0.058* | 0.388 (7) |
H28D | 0.5479 | 0.3144 | 0.2081 | 0.058* | 0.388 (7) |
C29B | 0.5609 (4) | 0.5253 (13) | 0.2354 (3) | 0.057 (3) | 0.388 (7) |
H29D | 0.5255 | 0.5461 | 0.2327 | 0.086* | 0.388 (7) |
H29E | 0.5773 | 0.6223 | 0.2323 | 0.086* | 0.388 (7) |
H29F | 0.5789 | 0.4814 | 0.2619 | 0.086* | 0.388 (7) |
N25 | 0.71077 (6) | 0.5678 (2) | 0.18181 (5) | 0.0203 (4) | |
H25C | 0.7177 | 0.5127 | 0.1622 | 0.024* | |
H25D | 0.7410 | 0.6028 | 0.1999 | 0.024* | |
N26 | 0.68546 (6) | 0.4719 (2) | 0.20128 (5) | 0.0227 (4) | |
H26 | 0.7000 | 0.3887 | 0.2146 | 0.027* | |
O25 | 0.61747 (5) | 0.63310 (18) | 0.18129 (5) | 0.0263 (3) | |
O26 | 0.61803 (7) | 0.4136 (2) | 0.21639 (6) | 0.0535 (6) | |
Co3 | 0.861768 (10) | 0.23284 (3) | 0.102066 (8) | 0.01656 (7) | |
C31 | 0.92004 (8) | 0.0164 (2) | 0.15870 (6) | 0.0201 (4) | |
C32 | 1.00754 (8) | −0.0041 (3) | 0.19841 (7) | 0.0286 (5) | |
H32A | 1.0107 | 0.0782 | 0.2185 | 0.034* | |
H32B | 1.0155 | 0.0411 | 0.1757 | 0.034* | |
C33 | 1.04293 (9) | −0.1347 (3) | 0.21655 (7) | 0.0328 (6) | |
H33A | 1.0778 | −0.0954 | 0.2274 | 0.049* | |
H33B | 1.0406 | −0.2129 | 0.1961 | 0.049* | |
H33C | 1.0336 | −0.1816 | 0.2381 | 0.049* | |
N31 | 0.83223 (6) | 0.03374 (19) | 0.12312 (5) | 0.0190 (4) | |
H31A | 0.8104 | 0.0645 | 0.1359 | 0.023* | |
H31B | 0.8147 | −0.0292 | 0.1020 | 0.023* | |
N32 | 0.87400 (6) | −0.0467 (2) | 0.14988 (5) | 0.0239 (4) | |
H32 | 0.8698 | −0.1357 | 0.1604 | 0.029* | |
O31 | 0.92832 (5) | 0.14003 (16) | 0.14449 (4) | 0.0210 (3) | |
O32 | 0.95605 (6) | −0.06886 (18) | 0.18456 (5) | 0.0290 (4) | |
C34 | 0.91254 (7) | 0.5176 (2) | 0.11969 (6) | 0.0185 (4) | |
C35 | 0.95894 (9) | 0.6621 (3) | 0.08829 (7) | 0.0277 (5) | |
H35A | 0.9303 | 0.6579 | 0.0625 | 0.033* | |
H35B | 0.9831 | 0.5780 | 0.0887 | 0.033* | |
C36 | 0.98499 (12) | 0.8170 (3) | 0.09326 (8) | 0.0489 (8) | |
H36A | 0.9980 | 0.8333 | 0.0714 | 0.073* | |
H36B | 1.0133 | 0.8195 | 0.1188 | 0.073* | |
H36C | 0.9606 | 0.8991 | 0.0928 | 0.073* | |
N33 | 0.85559 (6) | 0.39863 (19) | 0.14547 (5) | 0.0185 (4) | |
H33D | 0.8244 | 0.4471 | 0.1364 | 0.022* | |
H33E | 0.8593 | 0.3502 | 0.1693 | 0.022* | |
N34 | 0.89534 (6) | 0.5077 (2) | 0.15053 (5) | 0.0185 (4) | |
H34 | 0.9078 | 0.5647 | 0.1722 | 0.022* | |
O33 | 0.90476 (5) | 0.41820 (16) | 0.09329 (4) | 0.0202 (3) | |
O34 | 0.94035 (6) | 0.64404 (17) | 0.12149 (4) | 0.0239 (3) | |
C37 | 0.82773 (8) | 0.1031 (2) | 0.02534 (6) | 0.0187 (4) | |
C38 | 0.85617 (9) | −0.1023 (3) | −0.00621 (7) | 0.0303 (5) | |
H38A | 0.8389 | −0.1896 | −0.0237 | 0.036* | |
H38B | 0.8710 | −0.1422 | 0.0214 | 0.036* | |
C39 | 0.89794 (12) | −0.0420 (4) | −0.01941 (9) | 0.0538 (8) | |
H39A | 0.9215 | −0.1264 | −0.0190 | 0.081* | |
H39B | 0.9163 | 0.0405 | −0.0012 | 0.081* | |
H39C | 0.8833 | −0.0006 | −0.0466 | 0.081* | |
N35 | 0.79322 (6) | 0.2941 (2) | 0.05538 (5) | 0.0193 (4) | |
H35C | 0.7659 | 0.2834 | 0.0638 | 0.023* | |
H35D | 0.7946 | 0.3955 | 0.0478 | 0.023* | |
N36 | 0.78822 (7) | 0.1928 (2) | 0.02297 (5) | 0.0203 (4) | |
H36 | 0.7600 | 0.1894 | 0.0021 | 0.024* | |
O35 | 0.86768 (5) | 0.09820 (16) | 0.05461 (4) | 0.0210 (3) | |
O36 | 0.81902 (6) | 0.01782 (17) | −0.00770 (4) | 0.0242 (3) | |
Co4 | 0.169396 (10) | 0.75473 (3) | 0.153429 (8) | 0.01597 (6) | |
C41 | 0.11708 (8) | 1.0333 (2) | 0.15505 (6) | 0.0182 (4) | |
C42 | 0.05033 (8) | 1.1801 (3) | 0.10802 (7) | 0.0281 (5) | |
H42A | 0.0153 | 1.1967 | 0.1079 | 0.034* | |
H42B | 0.0501 | 1.0893 | 0.0910 | 0.034* | |
C43 | 0.06818 (10) | 1.3211 (3) | 0.09203 (8) | 0.0358 (6) | |
H43A | 0.0449 | 1.3425 | 0.0649 | 0.054* | |
H43B | 0.1025 | 1.3027 | 0.0915 | 0.054* | |
H43C | 0.0688 | 1.4102 | 0.1092 | 0.054* | |
N41 | 0.18798 (7) | 0.91604 (19) | 0.20300 (5) | 0.0202 (4) | |
H41A | 0.1884 | 0.8659 | 0.2259 | 0.024* | |
H41B | 0.2195 | 0.9590 | 0.2075 | 0.024* | |
N42 | 0.15002 (7) | 1.0330 (2) | 0.19243 (5) | 0.0208 (4) | |
H42 | 0.1483 | 1.1028 | 0.2099 | 0.025* | |
O41 | 0.11619 (5) | 0.93343 (16) | 0.12992 (4) | 0.0190 (3) | |
O42 | 0.08458 (6) | 1.15162 (17) | 0.14867 (4) | 0.0269 (3) | |
C44 | 0.14550 (7) | 0.5096 (2) | 0.19671 (6) | 0.0170 (4) | |
C45 | 0.07985 (8) | 0.4684 (3) | 0.22343 (7) | 0.0265 (5) | |
H45A | 0.0837 | 0.5796 | 0.2308 | 0.032* | |
H45B | 0.0757 | 0.4102 | 0.2460 | 0.032* | |
C46 | 0.03322 (9) | 0.4472 (3) | 0.18709 (8) | 0.0345 (6) | |
H46A | 0.0033 | 0.4829 | 0.1929 | 0.052* | |
H46B | 0.0292 | 0.3372 | 0.1798 | 0.052* | |
H46C | 0.0367 | 0.5076 | 0.1649 | 0.052* | |
N43 | 0.21539 (6) | 0.55428 (19) | 0.17677 (5) | 0.0192 (4) | |
H43D | 0.2205 | 0.4999 | 0.1563 | 0.023* | |
H43E | 0.2466 | 0.5842 | 0.1945 | 0.023* | |
N44 | 0.19016 (6) | 0.4594 (2) | 0.19640 (5) | 0.0199 (4) | |
H44 | 0.2034 | 0.3716 | 0.2078 | 0.024* | |
O43 | 0.12486 (5) | 0.63135 (16) | 0.18029 (4) | 0.0188 (3) | |
O44 | 0.12563 (5) | 0.41468 (17) | 0.21669 (5) | 0.0251 (3) | |
C47 | 0.17398 (8) | 0.6915 (2) | 0.07687 (6) | 0.0194 (4) | |
C48 | 0.13050 (9) | 0.5236 (3) | 0.02327 (7) | 0.0325 (6) | |
H48A | 0.1308 | 0.4497 | 0.0446 | 0.039* | |
H48B | 0.1394 | 0.4656 | 0.0027 | 0.039* | |
C49 | 0.07804 (10) | 0.5910 (3) | 0.00489 (8) | 0.0441 (7) | |
H49A | 0.0534 | 0.5070 | −0.0054 | 0.066* | |
H49B | 0.0772 | 0.6603 | −0.0171 | 0.066* | |
H49C | 0.0693 | 0.6495 | 0.0252 | 0.066* | |
N45 | 0.22220 (6) | 0.8546 (2) | 0.12932 (5) | 0.0199 (4) | |
H45C | 0.2183 | 0.9606 | 0.1277 | 0.024* | |
H45D | 0.2549 | 0.8324 | 0.1455 | 0.024* | |
N46 | 0.21268 (7) | 0.7915 (2) | 0.09073 (5) | 0.0230 (4) | |
H46 | 0.2315 | 0.8172 | 0.0764 | 0.028* | |
O45 | 0.14707 (5) | 0.64853 (16) | 0.09604 (4) | 0.0201 (3) | |
O46 | 0.16830 (6) | 0.64395 (18) | 0.04004 (4) | 0.0273 (4) | |
N101 | 0.71481 (6) | 0.2698 (2) | 0.11364 (5) | 0.0216 (4) | |
O101 | 0.72087 (6) | 0.16852 (17) | 0.08997 (5) | 0.0281 (4) | |
O102 | 0.73847 (6) | 0.39666 (17) | 0.11777 (5) | 0.0300 (4) | |
O103 | 0.68603 (6) | 0.24390 (19) | 0.13268 (5) | 0.0342 (4) | |
N111 | 0.79002 (6) | 0.1855 (2) | 0.20916 (5) | 0.0192 (4) | |
O111 | 0.75882 (6) | 0.20017 (18) | 0.22718 (4) | 0.0253 (3) | |
O112 | 0.78583 (6) | 0.07391 (19) | 0.18579 (5) | 0.0312 (4) | |
O113 | 0.82537 (6) | 0.2811 (2) | 0.21539 (5) | 0.0358 (4) | |
N121 | 0.83351 (7) | 0.6941 (2) | 0.20478 (5) | 0.0222 (4) | |
O121 | 0.80825 (6) | 0.71321 (18) | 0.16828 (4) | 0.0302 (4) | |
O122 | 0.81160 (6) | 0.68252 (19) | 0.22976 (4) | 0.0270 (4) | |
O123 | 0.88088 (6) | 0.6874 (2) | 0.21545 (5) | 0.0369 (4) | |
N131 | 0.79525 (7) | 0.7141 (2) | 0.05358 (5) | 0.0228 (4) | |
O131 | 0.77184 (5) | 0.84304 (16) | 0.04915 (4) | 0.0218 (3) | |
O132 | 0.78612 (6) | 0.62343 (18) | 0.02471 (4) | 0.0308 (4) | |
O133 | 0.82550 (9) | 0.6800 (3) | 0.08622 (6) | 0.0746 (8) | |
N141 | 0.29539 (6) | 0.1812 (2) | 0.21059 (5) | 0.0187 (4) | |
O141 | 0.26319 (5) | 0.19033 (18) | 0.22794 (4) | 0.0241 (3) | |
O142 | 0.32952 (7) | 0.2818 (2) | 0.21749 (5) | 0.0359 (4) | |
O143 | 0.29348 (6) | 0.07125 (19) | 0.18752 (5) | 0.0316 (4) | |
N151 | 0.22660 (6) | 0.2607 (2) | 0.11169 (5) | 0.0217 (4) | |
O151 | 0.23779 (6) | 0.15584 (17) | 0.09150 (4) | 0.0266 (3) | |
O152 | 0.24698 (6) | 0.39237 (18) | 0.11406 (5) | 0.0314 (4) | |
O153 | 0.19592 (6) | 0.2345 (2) | 0.12905 (5) | 0.0362 (4) | |
N161 | 0.31379 (7) | 0.7123 (2) | 0.05965 (5) | 0.0202 (4) | |
O161 | 0.29207 (5) | 0.84470 (16) | 0.05366 (4) | 0.0216 (3) | |
O162 | 0.30895 (7) | 0.62641 (18) | 0.03041 (5) | 0.0334 (4) | |
O163 | 0.33890 (7) | 0.6712 (2) | 0.09410 (5) | 0.0398 (4) | |
N171 | 0.34031 (6) | 0.6733 (2) | 0.21102 (5) | 0.0186 (4) | |
O171 | 0.32225 (6) | 0.70080 (17) | 0.17398 (4) | 0.0228 (3) | |
O172 | 0.38704 (5) | 0.64911 (18) | 0.22713 (5) | 0.0272 (4) | |
O173 | 0.31158 (5) | 0.66930 (18) | 0.23114 (4) | 0.0239 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.01957 (14) | 0.01827 (15) | 0.01411 (13) | 0.00035 (11) | 0.00613 (11) | 0.00113 (11) |
C11 | 0.0215 (11) | 0.0184 (11) | 0.0289 (12) | 0.0006 (9) | 0.0078 (9) | 0.0016 (9) |
C12 | 0.0348 (14) | 0.0362 (16) | 0.068 (2) | −0.0076 (12) | 0.0232 (14) | 0.0034 (14) |
C13 | 0.0545 (18) | 0.053 (2) | 0.0514 (18) | 0.0023 (15) | 0.0207 (15) | 0.0042 (15) |
N11 | 0.0217 (9) | 0.0231 (10) | 0.0188 (9) | 0.0009 (7) | 0.0085 (7) | 0.0004 (7) |
N12 | 0.0227 (9) | 0.0226 (10) | 0.0184 (9) | −0.0007 (7) | 0.0043 (7) | −0.0057 (8) |
O11 | 0.0271 (8) | 0.0197 (8) | 0.0278 (8) | 0.0004 (6) | 0.0150 (7) | −0.0004 (7) |
O12 | 0.0350 (9) | 0.0259 (9) | 0.0472 (11) | −0.0083 (7) | 0.0156 (8) | −0.0043 (8) |
C14 | 0.0284 (11) | 0.0191 (11) | 0.0146 (10) | −0.0015 (9) | 0.0095 (9) | 0.0003 (8) |
C15 | 0.0426 (14) | 0.0243 (13) | 0.0277 (13) | 0.0080 (10) | 0.0126 (11) | −0.0060 (10) |
C16 | 0.0452 (16) | 0.0494 (18) | 0.0501 (17) | 0.0040 (13) | 0.0266 (14) | −0.0125 (14) |
N13 | 0.0273 (9) | 0.0207 (9) | 0.0163 (9) | 0.0050 (7) | 0.0086 (7) | 0.0004 (7) |
N14 | 0.0278 (10) | 0.0284 (10) | 0.0129 (8) | 0.0076 (8) | 0.0030 (7) | −0.0017 (8) |
O13 | 0.0247 (8) | 0.0234 (8) | 0.0168 (7) | 0.0039 (6) | 0.0063 (6) | −0.0015 (6) |
O14 | 0.0341 (9) | 0.0275 (9) | 0.0172 (7) | 0.0061 (7) | 0.0085 (7) | −0.0039 (6) |
C17 | 0.0202 (10) | 0.0308 (13) | 0.0212 (11) | 0.0040 (9) | 0.0087 (9) | 0.0080 (10) |
C18A | 0.0170 (16) | 0.031 (3) | 0.032 (2) | 0.0015 (14) | 0.0066 (14) | 0.0084 (19) |
C19A | 0.034 (3) | 0.086 (5) | 0.023 (2) | −0.015 (3) | 0.005 (2) | −0.004 (3) |
C18B | 0.016 (4) | 0.027 (6) | 0.024 (5) | 0.002 (3) | 0.004 (3) | 0.003 (4) |
N15 | 0.0179 (8) | 0.0198 (9) | 0.0169 (9) | 0.0009 (7) | 0.0049 (7) | −0.0006 (7) |
N16 | 0.0209 (9) | 0.0186 (9) | 0.0260 (10) | −0.0001 (7) | 0.0073 (8) | 0.0073 (8) |
O15 | 0.0204 (8) | 0.0339 (9) | 0.0309 (9) | −0.0030 (7) | 0.0053 (7) | 0.0184 (7) |
O16 | 0.0201 (8) | 0.0429 (10) | 0.0404 (10) | 0.0052 (7) | 0.0085 (7) | 0.0253 (8) |
Co2 | 0.01984 (13) | 0.01599 (15) | 0.01447 (13) | −0.00063 (11) | 0.00670 (11) | 0.00120 (11) |
C21 | 0.0254 (11) | 0.0186 (11) | 0.0151 (10) | 0.0022 (8) | 0.0066 (9) | 0.0006 (8) |
C22 | 0.0488 (15) | 0.0228 (12) | 0.0281 (13) | −0.0093 (11) | 0.0195 (11) | −0.0088 (10) |
C23 | 0.0536 (18) | 0.0495 (18) | 0.0370 (16) | −0.0132 (14) | 0.0034 (13) | −0.0070 (14) |
N21 | 0.0263 (9) | 0.0189 (9) | 0.0176 (9) | −0.0046 (7) | 0.0071 (7) | −0.0005 (7) |
N22 | 0.0319 (10) | 0.0252 (10) | 0.0181 (9) | −0.0085 (8) | 0.0139 (8) | −0.0024 (8) |
O21 | 0.0248 (8) | 0.0195 (8) | 0.0176 (7) | −0.0040 (6) | 0.0093 (6) | −0.0019 (6) |
O22 | 0.0416 (9) | 0.0231 (8) | 0.0204 (8) | −0.0070 (7) | 0.0174 (7) | −0.0054 (7) |
C24 | 0.0231 (11) | 0.0212 (11) | 0.0205 (11) | 0.0018 (9) | 0.0130 (9) | 0.0036 (9) |
C25 | 0.0248 (12) | 0.0350 (14) | 0.0286 (12) | 0.0097 (10) | 0.0074 (10) | 0.0053 (11) |
C26 | 0.0399 (14) | 0.0395 (15) | 0.0305 (13) | 0.0094 (12) | 0.0144 (11) | 0.0105 (11) |
N23 | 0.0239 (9) | 0.0209 (9) | 0.0166 (9) | −0.0006 (7) | 0.0058 (7) | 0.0025 (7) |
N24 | 0.0292 (10) | 0.0189 (9) | 0.0166 (9) | 0.0037 (7) | 0.0098 (7) | −0.0022 (7) |
O23 | 0.0249 (8) | 0.0224 (8) | 0.0175 (7) | 0.0039 (6) | 0.0057 (6) | 0.0002 (6) |
O24 | 0.0347 (9) | 0.0323 (9) | 0.0258 (8) | 0.0136 (7) | 0.0139 (7) | 0.0023 (7) |
C27 | 0.0262 (11) | 0.0255 (12) | 0.0263 (12) | −0.0016 (9) | 0.0091 (9) | 0.0097 (10) |
C28A | 0.037 (3) | 0.023 (3) | 0.046 (3) | −0.002 (2) | 0.026 (3) | 0.006 (2) |
C29A | 0.025 (2) | 0.046 (3) | 0.030 (2) | 0.0026 (19) | 0.0090 (17) | 0.0064 (19) |
C28B | 0.048 (5) | 0.030 (5) | 0.074 (7) | −0.009 (4) | 0.032 (5) | 0.005 (4) |
C29B | 0.071 (7) | 0.057 (7) | 0.056 (6) | 0.029 (5) | 0.038 (5) | 0.027 (5) |
N25 | 0.0202 (9) | 0.0184 (9) | 0.0237 (9) | −0.0016 (7) | 0.0092 (7) | 0.0023 (7) |
N26 | 0.0240 (9) | 0.0181 (9) | 0.0261 (10) | −0.0004 (7) | 0.0087 (8) | 0.0091 (8) |
O25 | 0.0229 (8) | 0.0273 (9) | 0.0316 (9) | 0.0030 (6) | 0.0131 (7) | 0.0133 (7) |
O26 | 0.0350 (10) | 0.0508 (12) | 0.0836 (15) | 0.0073 (9) | 0.0318 (10) | 0.0436 (11) |
Co3 | 0.01981 (14) | 0.01586 (15) | 0.01406 (13) | −0.00134 (11) | 0.00592 (11) | −0.00030 (11) |
C31 | 0.0242 (11) | 0.0177 (11) | 0.0210 (11) | 0.0031 (8) | 0.0112 (9) | 0.0008 (9) |
C32 | 0.0232 (11) | 0.0263 (13) | 0.0364 (13) | 0.0019 (9) | 0.0105 (10) | 0.0029 (11) |
C33 | 0.0281 (12) | 0.0290 (13) | 0.0385 (14) | 0.0047 (10) | 0.0080 (11) | 0.0036 (11) |
N31 | 0.0192 (9) | 0.0170 (9) | 0.0218 (9) | −0.0017 (7) | 0.0083 (7) | −0.0024 (7) |
N32 | 0.0228 (9) | 0.0165 (9) | 0.0338 (11) | 0.0016 (7) | 0.0114 (8) | 0.0106 (8) |
O31 | 0.0218 (7) | 0.0174 (8) | 0.0230 (8) | −0.0014 (6) | 0.0069 (6) | 0.0045 (6) |
O32 | 0.0230 (8) | 0.0228 (8) | 0.0405 (10) | 0.0044 (6) | 0.0102 (7) | 0.0129 (7) |
C34 | 0.0184 (10) | 0.0177 (11) | 0.0179 (10) | −0.0009 (8) | 0.0044 (8) | 0.0021 (8) |
C35 | 0.0322 (12) | 0.0294 (13) | 0.0249 (12) | −0.0066 (10) | 0.0143 (10) | −0.0018 (10) |
C36 | 0.067 (2) | 0.0451 (17) | 0.0442 (16) | −0.0283 (15) | 0.0321 (15) | −0.0064 (14) |
N33 | 0.0190 (9) | 0.0198 (9) | 0.0175 (9) | −0.0005 (7) | 0.0073 (7) | 0.0001 (7) |
N34 | 0.0207 (9) | 0.0196 (9) | 0.0151 (8) | −0.0043 (7) | 0.0060 (7) | −0.0039 (7) |
O33 | 0.0271 (8) | 0.0171 (8) | 0.0185 (7) | −0.0030 (6) | 0.0106 (6) | −0.0023 (6) |
O34 | 0.0301 (8) | 0.0211 (8) | 0.0238 (8) | −0.0081 (6) | 0.0134 (7) | −0.0030 (6) |
C37 | 0.0279 (11) | 0.0140 (10) | 0.0159 (10) | −0.0005 (8) | 0.0098 (9) | 0.0019 (8) |
C38 | 0.0444 (14) | 0.0210 (12) | 0.0224 (12) | 0.0116 (10) | 0.0076 (10) | −0.0051 (9) |
C39 | 0.066 (2) | 0.0546 (19) | 0.0579 (19) | 0.0287 (16) | 0.0427 (17) | 0.0135 (15) |
N35 | 0.0253 (9) | 0.0170 (9) | 0.0158 (9) | 0.0012 (7) | 0.0075 (7) | −0.0023 (7) |
N36 | 0.0268 (9) | 0.0194 (9) | 0.0124 (8) | 0.0020 (7) | 0.0037 (7) | −0.0020 (7) |
O35 | 0.0242 (8) | 0.0211 (8) | 0.0165 (7) | 0.0015 (6) | 0.0058 (6) | −0.0020 (6) |
O36 | 0.0343 (8) | 0.0216 (8) | 0.0156 (7) | 0.0056 (7) | 0.0073 (6) | −0.0033 (6) |
Co4 | 0.01871 (13) | 0.01439 (14) | 0.01511 (13) | −0.00110 (11) | 0.00620 (10) | 0.00028 (11) |
C41 | 0.0229 (10) | 0.0155 (11) | 0.0195 (10) | −0.0011 (8) | 0.0113 (9) | 0.0016 (8) |
C42 | 0.0270 (12) | 0.0254 (12) | 0.0272 (12) | 0.0035 (9) | 0.0033 (10) | 0.0038 (10) |
C43 | 0.0398 (14) | 0.0334 (14) | 0.0353 (14) | −0.0003 (11) | 0.0144 (12) | 0.0069 (11) |
N41 | 0.0251 (9) | 0.0184 (9) | 0.0151 (8) | −0.0022 (7) | 0.0045 (7) | 0.0022 (7) |
N42 | 0.0294 (10) | 0.0174 (9) | 0.0158 (9) | 0.0024 (7) | 0.0082 (7) | −0.0015 (7) |
O41 | 0.0227 (7) | 0.0165 (7) | 0.0161 (7) | 0.0007 (6) | 0.0046 (6) | −0.0012 (6) |
O42 | 0.0320 (9) | 0.0224 (8) | 0.0251 (8) | 0.0077 (7) | 0.0083 (7) | 0.0000 (7) |
C44 | 0.0220 (10) | 0.0149 (10) | 0.0136 (9) | −0.0015 (8) | 0.0056 (8) | −0.0002 (8) |
C45 | 0.0306 (12) | 0.0251 (12) | 0.0313 (12) | 0.0074 (10) | 0.0202 (10) | 0.0103 (10) |
C46 | 0.0279 (12) | 0.0335 (14) | 0.0456 (15) | −0.0024 (10) | 0.0172 (11) | 0.0005 (12) |
N43 | 0.0164 (8) | 0.0188 (9) | 0.0229 (9) | −0.0025 (7) | 0.0076 (7) | 0.0004 (7) |
N44 | 0.0197 (9) | 0.0144 (9) | 0.0256 (9) | 0.0021 (7) | 0.0079 (7) | 0.0058 (7) |
O43 | 0.0207 (7) | 0.0153 (7) | 0.0223 (7) | 0.0026 (6) | 0.0098 (6) | 0.0037 (6) |
O44 | 0.0262 (8) | 0.0223 (8) | 0.0320 (9) | 0.0065 (6) | 0.0165 (7) | 0.0109 (7) |
C47 | 0.0260 (11) | 0.0146 (10) | 0.0185 (10) | 0.0017 (8) | 0.0089 (9) | 0.0014 (8) |
C48 | 0.0501 (15) | 0.0251 (13) | 0.0299 (13) | −0.0159 (11) | 0.0235 (12) | −0.0142 (10) |
C49 | 0.0446 (16) | 0.0543 (18) | 0.0306 (14) | −0.0140 (14) | 0.0093 (12) | −0.0127 (13) |
N45 | 0.0215 (9) | 0.0202 (9) | 0.0168 (9) | −0.0043 (7) | 0.0051 (7) | −0.0002 (7) |
N46 | 0.0272 (10) | 0.0261 (10) | 0.0200 (9) | −0.0076 (8) | 0.0135 (8) | −0.0017 (8) |
O45 | 0.0244 (8) | 0.0197 (8) | 0.0184 (7) | −0.0039 (6) | 0.0102 (6) | −0.0022 (6) |
O46 | 0.0390 (9) | 0.0257 (9) | 0.0227 (8) | −0.0103 (7) | 0.0175 (7) | −0.0076 (7) |
N101 | 0.0186 (9) | 0.0213 (10) | 0.0221 (9) | 0.0010 (7) | 0.0036 (7) | 0.0032 (8) |
O101 | 0.0393 (9) | 0.0202 (8) | 0.0258 (8) | −0.0026 (7) | 0.0127 (7) | −0.0041 (7) |
O102 | 0.0286 (8) | 0.0193 (8) | 0.0440 (10) | −0.0059 (7) | 0.0150 (8) | −0.0070 (7) |
O103 | 0.0349 (9) | 0.0356 (10) | 0.0398 (10) | −0.0036 (8) | 0.0228 (8) | 0.0024 (8) |
N111 | 0.0209 (9) | 0.0216 (10) | 0.0143 (8) | 0.0002 (7) | 0.0051 (7) | −0.0002 (7) |
O111 | 0.0265 (8) | 0.0320 (9) | 0.0222 (8) | 0.0034 (7) | 0.0145 (7) | 0.0000 (7) |
O112 | 0.0393 (9) | 0.0294 (9) | 0.0262 (8) | −0.0013 (7) | 0.0130 (7) | −0.0135 (7) |
O113 | 0.0379 (10) | 0.0431 (11) | 0.0301 (9) | −0.0222 (8) | 0.0164 (8) | −0.0077 (8) |
N121 | 0.0283 (10) | 0.0165 (9) | 0.0255 (10) | −0.0026 (7) | 0.0142 (8) | −0.0016 (8) |
O121 | 0.0461 (10) | 0.0280 (9) | 0.0185 (8) | 0.0046 (7) | 0.0136 (7) | 0.0045 (7) |
O122 | 0.0283 (8) | 0.0366 (9) | 0.0201 (8) | −0.0070 (7) | 0.0136 (7) | 0.0014 (7) |
O123 | 0.0242 (9) | 0.0488 (11) | 0.0411 (10) | −0.0059 (8) | 0.0154 (8) | −0.0184 (9) |
N131 | 0.0255 (9) | 0.0242 (10) | 0.0180 (9) | 0.0040 (8) | 0.0066 (8) | 0.0015 (8) |
O131 | 0.0254 (8) | 0.0154 (8) | 0.0249 (8) | 0.0017 (6) | 0.0091 (6) | 0.0040 (6) |
O132 | 0.0447 (10) | 0.0223 (9) | 0.0217 (8) | 0.0014 (7) | 0.0067 (7) | −0.0039 (7) |
O133 | 0.0900 (17) | 0.0707 (15) | 0.0281 (11) | 0.0559 (13) | −0.0240 (10) | −0.0135 (10) |
N141 | 0.0210 (9) | 0.0200 (9) | 0.0140 (8) | 0.0010 (7) | 0.0045 (7) | −0.0004 (7) |
O141 | 0.0264 (8) | 0.0287 (9) | 0.0214 (8) | 0.0017 (7) | 0.0135 (6) | −0.0008 (7) |
O142 | 0.0413 (10) | 0.0381 (10) | 0.0332 (9) | −0.0223 (8) | 0.0193 (8) | −0.0081 (8) |
O143 | 0.0399 (9) | 0.0294 (9) | 0.0274 (9) | 0.0006 (7) | 0.0143 (7) | −0.0142 (7) |
N151 | 0.0185 (8) | 0.0210 (10) | 0.0230 (9) | −0.0002 (7) | 0.0039 (7) | 0.0024 (8) |
O151 | 0.0333 (9) | 0.0206 (8) | 0.0263 (8) | 0.0001 (7) | 0.0109 (7) | −0.0049 (7) |
O152 | 0.0359 (9) | 0.0189 (8) | 0.0461 (10) | −0.0046 (7) | 0.0226 (8) | −0.0044 (7) |
O153 | 0.0350 (9) | 0.0375 (10) | 0.0450 (11) | −0.0077 (8) | 0.0251 (8) | −0.0014 (8) |
N161 | 0.0249 (9) | 0.0199 (9) | 0.0176 (9) | 0.0018 (7) | 0.0094 (7) | 0.0007 (7) |
O161 | 0.0263 (8) | 0.0163 (8) | 0.0206 (8) | 0.0040 (6) | 0.0062 (6) | −0.0006 (6) |
O162 | 0.0542 (11) | 0.0238 (9) | 0.0220 (8) | 0.0071 (8) | 0.0130 (8) | −0.0060 (7) |
O163 | 0.0557 (11) | 0.0338 (10) | 0.0195 (8) | 0.0171 (9) | −0.0002 (8) | 0.0043 (7) |
N171 | 0.0213 (9) | 0.0169 (9) | 0.0180 (9) | −0.0040 (7) | 0.0073 (7) | −0.0002 (7) |
O171 | 0.0301 (8) | 0.0249 (8) | 0.0159 (7) | 0.0016 (6) | 0.0110 (6) | 0.0056 (6) |
O172 | 0.0189 (8) | 0.0310 (9) | 0.0282 (8) | −0.0003 (7) | 0.0036 (6) | −0.0057 (7) |
O173 | 0.0251 (8) | 0.0311 (9) | 0.0185 (7) | −0.0063 (7) | 0.0114 (6) | −0.0001 (7) |
Co1—O11 | 2.1005 (15) | Co3—N33 | 2.1582 (16) |
Co1—O15 | 2.1172 (15) | C31—O31 | 1.237 (2) |
Co1—O13 | 2.1179 (14) | C31—O32 | 1.329 (2) |
Co1—N13 | 2.1236 (17) | C31—N32 | 1.334 (3) |
Co1—N15 | 2.1460 (17) | C32—O32 | 1.465 (3) |
Co1—N11 | 2.1649 (17) | C32—C33 | 1.492 (3) |
C11—O11 | 1.236 (3) | C32—H32A | 0.9900 |
C11—O12 | 1.338 (3) | C32—H32B | 0.9900 |
C11—N12 | 1.345 (3) | C33—H33A | 0.9800 |
C12—O12 | 1.461 (3) | C33—H33B | 0.9800 |
C12—C13 | 1.471 (4) | C33—H33C | 0.9800 |
C12—H12A | 0.9900 | N31—N32 | 1.411 (2) |
C12—H12B | 0.9900 | N31—H31A | 0.9200 |
C13—H13A | 0.9800 | N31—H31B | 0.9200 |
C13—H13B | 0.9800 | N32—H32 | 0.8800 |
C13—H13C | 0.9800 | C34—O33 | 1.236 (2) |
N11—N12 | 1.421 (2) | C34—O34 | 1.329 (2) |
N11—H11A | 0.9200 | C34—N34 | 1.348 (2) |
N11—H11B | 0.9200 | C35—O34 | 1.458 (2) |
N12—H12 | 0.8800 | C35—C36 | 1.503 (3) |
C14—O13 | 1.249 (2) | C35—H35A | 0.9900 |
C14—N14 | 1.324 (3) | C35—H35B | 0.9900 |
C14—O14 | 1.332 (2) | C36—H36A | 0.9800 |
C15—O14 | 1.451 (3) | C36—H36B | 0.9800 |
C15—C16 | 1.505 (3) | C36—H36C | 0.9800 |
C15—H15A | 0.9900 | N33—N34 | 1.421 (2) |
C15—H15B | 0.9900 | N33—H33D | 0.9200 |
C16—H16A | 0.9800 | N33—H33E | 0.9200 |
C16—H16B | 0.9800 | N34—H34 | 0.8800 |
C16—H16C | 0.9800 | C37—O35 | 1.240 (2) |
N13—N14 | 1.413 (2) | C37—N36 | 1.329 (3) |
N13—H13D | 0.9200 | C37—O36 | 1.338 (2) |
N13—H13E | 0.9200 | C38—O36 | 1.457 (2) |
N14—H14 | 0.8800 | C38—C39 | 1.498 (4) |
C17—O15 | 1.238 (3) | C38—H38A | 0.9900 |
C17—N16 | 1.326 (3) | C38—H38B | 0.9900 |
C17—O16 | 1.331 (2) | C39—H39A | 0.9800 |
C18A—O16 | 1.441 (3) | C39—H39B | 0.9800 |
C18A—C19A | 1.497 (7) | C39—H39C | 0.9800 |
C18A—H18A | 0.9900 | N35—N36 | 1.417 (2) |
C18A—H18B | 0.9900 | N35—H35C | 0.9200 |
C19A—H19A | 0.9800 | N35—H35D | 0.9200 |
C19A—H19B | 0.9800 | N36—H36 | 0.8800 |
C19A—H19C | 0.9800 | Co4—O41 | 2.1063 (14) |
C18B—C19B | 1.488 (17) | Co4—O43 | 2.1064 (14) |
C18B—O16 | 1.619 (9) | Co4—O45 | 2.1297 (14) |
C18B—H18C | 0.9900 | Co4—N45 | 2.1338 (16) |
C18B—H18D | 0.9900 | Co4—N43 | 2.1450 (17) |
C19B—H19D | 0.9800 | Co4—N41 | 2.1671 (17) |
C19B—H19E | 0.9800 | C41—O41 | 1.237 (2) |
C19B—H19F | 0.9800 | C41—N42 | 1.334 (3) |
N15—N16 | 1.416 (2) | C41—O42 | 1.334 (2) |
N15—H15C | 0.9200 | C42—O42 | 1.457 (3) |
N15—H15D | 0.9200 | C42—C43 | 1.501 (3) |
N16—H16 | 0.8800 | C42—H42A | 0.9900 |
Co2—O25 | 2.0853 (14) | C42—H42B | 0.9900 |
Co2—O23 | 2.1090 (14) | C43—H43A | 0.9800 |
Co2—N21 | 2.1240 (17) | C43—H43B | 0.9800 |
Co2—O21 | 2.1270 (14) | C43—H43C | 0.9800 |
Co2—N25 | 2.1534 (17) | N41—N42 | 1.420 (2) |
Co2—N23 | 2.1678 (17) | N41—H41A | 0.9200 |
C21—O21 | 1.239 (2) | N41—H41B | 0.9200 |
C21—O22 | 1.331 (2) | N42—H42 | 0.8800 |
C21—N22 | 1.335 (3) | C44—O43 | 1.243 (2) |
C22—O22 | 1.455 (3) | C44—O44 | 1.328 (2) |
C22—C23 | 1.504 (4) | C44—N44 | 1.328 (3) |
C22—H22A | 0.9900 | C45—O44 | 1.460 (2) |
C22—H22B | 0.9900 | C45—C46 | 1.500 (3) |
C23—H23A | 0.9800 | C45—H45A | 0.9900 |
C23—H23B | 0.9800 | C45—H45B | 0.9900 |
C23—H23C | 0.9800 | C46—H46A | 0.9800 |
N21—N22 | 1.413 (2) | C46—H46B | 0.9800 |
N21—H21A | 0.9200 | C46—H46C | 0.9800 |
N21—H21B | 0.9200 | N43—N44 | 1.415 (2) |
N22—H22 | 0.8800 | N43—H43D | 0.9200 |
C24—O23 | 1.235 (2) | N43—H43E | 0.9200 |
C24—N24 | 1.332 (3) | N44—H44 | 0.8800 |
C24—O24 | 1.338 (2) | C47—O45 | 1.237 (2) |
C25—O24 | 1.461 (3) | C47—O46 | 1.332 (2) |
C25—C26 | 1.499 (3) | C47—N46 | 1.340 (3) |
C25—H25A | 0.9900 | C48—O46 | 1.456 (3) |
C25—H25B | 0.9900 | C48—C49 | 1.504 (4) |
C26—H26A | 0.9800 | C48—H48A | 0.9900 |
C26—H26B | 0.9800 | C48—H48B | 0.9900 |
C26—H26C | 0.9800 | C49—H49A | 0.9800 |
N23—N24 | 1.421 (2) | C49—H49B | 0.9800 |
N23—H23D | 0.9200 | C49—H49C | 0.9800 |
N23—H23E | 0.9200 | N45—N46 | 1.417 (2) |
N24—H24 | 0.8800 | N45—H45C | 0.9200 |
C27—O25 | 1.246 (3) | N45—H45D | 0.9200 |
C27—N26 | 1.320 (3) | N46—H46 | 0.8800 |
C27—O26 | 1.324 (3) | N101—O103 | 1.241 (2) |
C28A—C29A | 1.502 (7) | N101—O102 | 1.261 (2) |
C28A—O26 | 1.524 (6) | N101—O101 | 1.267 (2) |
C28A—H28A | 0.9900 | N111—O113 | 1.248 (2) |
C28A—H28B | 0.9900 | N111—O112 | 1.252 (2) |
C29A—H29A | 0.9800 | N111—O111 | 1.258 (2) |
C29A—H29B | 0.9800 | N121—O122 | 1.249 (2) |
C29A—H29C | 0.9800 | N121—O123 | 1.250 (2) |
C28B—C29B | 1.440 (14) | N121—O121 | 1.260 (2) |
C28B—O26 | 1.476 (8) | N131—O133 | 1.216 (2) |
C28B—H28C | 0.9900 | N131—O132 | 1.247 (2) |
C28B—H28D | 0.9900 | N131—O131 | 1.273 (2) |
C29B—H29D | 0.9800 | N141—O143 | 1.245 (2) |
C29B—H29E | 0.9800 | N141—O142 | 1.251 (2) |
C29B—H29F | 0.9800 | N141—O141 | 1.261 (2) |
N25—N26 | 1.418 (2) | N151—O153 | 1.242 (2) |
N25—H25C | 0.9200 | N151—O152 | 1.261 (2) |
N25—H25D | 0.9200 | N151—O151 | 1.261 (2) |
N26—H26 | 0.8800 | N161—O163 | 1.238 (2) |
Co3—O33 | 2.0896 (14) | N161—O162 | 1.248 (2) |
Co3—O35 | 2.1062 (14) | N161—O161 | 1.277 (2) |
Co3—O31 | 2.1112 (14) | N171—O173 | 1.251 (2) |
Co3—N35 | 2.1285 (17) | N171—O172 | 1.252 (2) |
Co3—N31 | 2.1515 (16) | N171—O171 | 1.263 (2) |
O11—Co1—O15 | 88.32 (6) | O35—Co3—N31 | 89.28 (6) |
O11—Co1—O13 | 95.73 (6) | O31—Co3—N31 | 78.37 (6) |
O15—Co1—O13 | 94.30 (6) | N35—Co3—N31 | 96.84 (7) |
O11—Co1—N13 | 98.24 (6) | O33—Co3—N33 | 78.13 (6) |
O15—Co1—N13 | 170.86 (7) | O35—Co3—N33 | 171.95 (6) |
O13—Co1—N13 | 78.78 (6) | O31—Co3—N33 | 90.41 (6) |
O11—Co1—N15 | 164.39 (6) | N35—Co3—N33 | 97.01 (6) |
O15—Co1—N15 | 77.65 (6) | N31—Co3—N33 | 98.17 (6) |
O13—Co1—N15 | 92.16 (6) | O31—C31—O32 | 123.81 (19) |
N13—Co1—N15 | 96.49 (7) | O31—C31—N32 | 123.95 (19) |
O11—Co1—N11 | 77.60 (6) | O32—C31—N32 | 112.24 (18) |
O15—Co1—N11 | 93.69 (7) | O32—C32—C33 | 106.73 (18) |
O13—Co1—N11 | 169.43 (6) | O32—C32—H32A | 110.4 |
N13—Co1—N11 | 93.93 (6) | C33—C32—H32A | 110.4 |
N15—Co1—N11 | 96.30 (6) | O32—C32—H32B | 110.4 |
O11—C11—O12 | 124.4 (2) | C33—C32—H32B | 110.4 |
O11—C11—N12 | 123.98 (19) | H32A—C32—H32B | 108.6 |
O12—C11—N12 | 111.50 (19) | C32—C33—H33A | 109.5 |
O12—C12—C13 | 109.4 (2) | C32—C33—H33B | 109.5 |
O12—C12—H12A | 109.8 | H33A—C33—H33B | 109.5 |
C13—C12—H12A | 109.8 | C32—C33—H33C | 109.5 |
O12—C12—H12B | 109.8 | H33A—C33—H33C | 109.5 |
C13—C12—H12B | 109.8 | H33B—C33—H33C | 109.5 |
H12A—C12—H12B | 108.2 | N32—N31—Co3 | 107.42 (11) |
C12—C13—H13A | 109.5 | N32—N31—H31A | 110.2 |
C12—C13—H13B | 109.5 | Co3—N31—H31A | 110.2 |
H13A—C13—H13B | 109.5 | N32—N31—H31B | 110.2 |
C12—C13—H13C | 109.5 | Co3—N31—H31B | 110.2 |
H13A—C13—H13C | 109.5 | H31A—N31—H31B | 108.5 |
H13B—C13—H13C | 109.5 | C31—N32—N31 | 117.87 (17) |
N12—N11—Co1 | 106.45 (11) | C31—N32—H32 | 121.1 |
N12—N11—H11A | 110.4 | N31—N32—H32 | 121.1 |
Co1—N11—H11A | 110.4 | C31—O31—Co3 | 112.10 (13) |
N12—N11—H11B | 110.4 | C31—O32—C32 | 116.51 (17) |
Co1—N11—H11B | 110.4 | O33—C34—O34 | 123.49 (18) |
H11A—N11—H11B | 108.6 | O33—C34—N34 | 124.04 (18) |
C11—N12—N11 | 115.54 (17) | O34—C34—N34 | 112.44 (17) |
C11—N12—H12 | 122.2 | O34—C35—C36 | 107.14 (18) |
N11—N12—H12 | 122.2 | O34—C35—H35A | 110.3 |
C11—O11—Co1 | 112.30 (13) | C36—C35—H35A | 110.3 |
C11—O12—C12 | 116.64 (19) | O34—C35—H35B | 110.3 |
O13—C14—N14 | 124.03 (19) | C36—C35—H35B | 110.3 |
O13—C14—O14 | 124.05 (19) | H35A—C35—H35B | 108.5 |
N14—C14—O14 | 111.92 (18) | C35—C36—H36A | 109.5 |
O14—C15—C16 | 111.8 (2) | C35—C36—H36B | 109.5 |
O14—C15—H15A | 109.2 | H36A—C36—H36B | 109.5 |
C16—C15—H15A | 109.2 | C35—C36—H36C | 109.5 |
O14—C15—H15B | 109.2 | H36A—C36—H36C | 109.5 |
C16—C15—H15B | 109.2 | H36B—C36—H36C | 109.5 |
H15A—C15—H15B | 107.9 | N34—N33—Co3 | 106.00 (11) |
C15—C16—H16A | 109.5 | N34—N33—H33D | 110.5 |
C15—C16—H16B | 109.5 | Co3—N33—H33D | 110.5 |
H16A—C16—H16B | 109.5 | N34—N33—H33E | 110.5 |
C15—C16—H16C | 109.5 | Co3—N33—H33E | 110.5 |
H16A—C16—H16C | 109.5 | H33D—N33—H33E | 108.7 |
H16B—C16—H16C | 109.5 | C34—N34—N33 | 115.09 (16) |
N14—N13—Co1 | 107.63 (12) | C34—N34—H34 | 122.5 |
N14—N13—H13D | 110.2 | N33—N34—H34 | 122.5 |
Co1—N13—H13D | 110.2 | C34—O33—Co3 | 112.04 (13) |
N14—N13—H13E | 110.2 | C34—O34—C35 | 114.64 (16) |
Co1—N13—H13E | 110.2 | O35—C37—N36 | 124.28 (18) |
H13D—N13—H13E | 108.5 | O35—C37—O36 | 124.02 (18) |
C14—N14—N13 | 117.82 (17) | N36—C37—O36 | 111.71 (17) |
C14—N14—H14 | 121.1 | O36—C38—C39 | 111.58 (19) |
N13—N14—H14 | 121.1 | O36—C38—H38A | 109.3 |
C14—O13—Co1 | 110.88 (13) | C39—C38—H38A | 109.3 |
C14—O14—C15 | 117.57 (17) | O36—C38—H38B | 109.3 |
O15—C17—N16 | 123.5 (2) | C39—C38—H38B | 109.3 |
O15—C17—O16 | 124.41 (19) | H38A—C38—H38B | 108.0 |
N16—C17—O16 | 112.09 (19) | C38—C39—H39A | 109.5 |
O16—C18A—C19A | 106.6 (4) | C38—C39—H39B | 109.5 |
O16—C18A—H18A | 110.4 | H39A—C39—H39B | 109.5 |
C19A—C18A—H18A | 110.4 | C38—C39—H39C | 109.5 |
O16—C18A—H18B | 110.4 | H39A—C39—H39C | 109.5 |
C19A—C18A—H18B | 110.4 | H39B—C39—H39C | 109.5 |
H18A—C18A—H18B | 108.6 | N36—N35—Co3 | 107.03 (12) |
C19B—C18B—O16 | 102.1 (9) | N36—N35—H35C | 110.3 |
C19B—C18B—H18C | 111.3 | Co3—N35—H35C | 110.3 |
O16—C18B—H18C | 111.3 | N36—N35—H35D | 110.3 |
C19B—C18B—H18D | 111.3 | Co3—N35—H35D | 110.3 |
O16—C18B—H18D | 111.3 | H35C—N35—H35D | 108.6 |
H18C—C18B—H18D | 109.2 | C37—N36—N35 | 117.52 (16) |
C18B—C19B—H19D | 109.5 | C37—N36—H36 | 121.2 |
C18B—C19B—H19E | 109.5 | N35—N36—H36 | 121.2 |
H19D—C19B—H19E | 109.5 | C37—O35—Co3 | 111.03 (13) |
C18B—C19B—H19F | 109.5 | C37—O36—C38 | 116.65 (16) |
H19D—C19B—H19F | 109.5 | O41—Co4—O43 | 95.82 (5) |
H19E—C19B—H19F | 109.5 | O41—Co4—O45 | 90.00 (5) |
N16—N15—Co1 | 108.32 (11) | O43—Co4—O45 | 101.36 (5) |
N16—N15—H15C | 110.0 | O41—Co4—N45 | 92.21 (6) |
Co1—N15—H15C | 110.0 | O43—Co4—N45 | 171.97 (6) |
N16—N15—H15D | 110.0 | O45—Co4—N45 | 78.47 (6) |
Co1—N15—H15D | 110.0 | O41—Co4—N43 | 172.67 (6) |
H15C—N15—H15D | 108.4 | O43—Co4—N43 | 77.72 (6) |
C17—N16—N15 | 117.57 (17) | O45—Co4—N43 | 87.92 (6) |
C17—N16—H16 | 121.2 | N45—Co4—N43 | 94.26 (6) |
N15—N16—H16 | 121.2 | O41—Co4—N41 | 78.01 (6) |
C17—O15—Co1 | 112.92 (13) | O43—Co4—N41 | 88.05 (6) |
C17—O16—C18A | 118.95 (19) | O45—Co4—N41 | 165.52 (6) |
C17—O16—C18B | 111.1 (3) | N45—Co4—N41 | 93.75 (6) |
C18A—O16—C18B | 32.9 (3) | N43—Co4—N41 | 104.96 (6) |
O25—Co2—O23 | 93.27 (6) | O41—C41—N42 | 123.83 (19) |
O25—Co2—N21 | 173.50 (7) | O41—C41—O42 | 124.59 (19) |
O23—Co2—N21 | 92.03 (6) | N42—C41—O42 | 111.56 (17) |
O25—Co2—O21 | 97.26 (6) | O42—C42—C43 | 108.87 (19) |
O23—Co2—O21 | 91.76 (6) | O42—C42—H42A | 109.9 |
N21—Co2—O21 | 78.81 (6) | C43—C42—H42A | 109.9 |
O25—Co2—N25 | 78.02 (6) | O42—C42—H42B | 109.9 |
O23—Co2—N25 | 171.23 (6) | C43—C42—H42B | 109.9 |
N21—Co2—N25 | 96.59 (7) | H42A—C42—H42B | 108.3 |
O21—Co2—N25 | 88.33 (6) | C42—C43—H43A | 109.5 |
O25—Co2—N23 | 90.66 (6) | C42—C43—H43B | 109.5 |
O23—Co2—N23 | 78.05 (6) | H43A—C43—H43B | 109.5 |
N21—Co2—N23 | 94.11 (7) | C42—C43—H43C | 109.5 |
O21—Co2—N23 | 167.46 (6) | H43A—C43—H43C | 109.5 |
N25—Co2—N23 | 102.87 (7) | H43B—C43—H43C | 109.5 |
O21—C21—O22 | 124.25 (19) | N42—N41—Co4 | 107.05 (11) |
O21—C21—N22 | 124.23 (19) | N42—N41—H41A | 110.3 |
O22—C21—N22 | 111.52 (18) | Co4—N41—H41A | 110.3 |
O22—C22—C23 | 111.2 (2) | N42—N41—H41B | 110.3 |
O22—C22—H22A | 109.4 | Co4—N41—H41B | 110.3 |
C23—C22—H22A | 109.4 | H41A—N41—H41B | 108.6 |
O22—C22—H22B | 109.4 | C41—N42—N41 | 117.56 (16) |
C23—C22—H22B | 109.4 | C41—N42—H42 | 121.2 |
H22A—C22—H22B | 108.0 | N41—N42—H42 | 121.2 |
C22—C23—H23A | 109.5 | C41—O41—Co4 | 112.77 (13) |
C22—C23—H23B | 109.5 | C41—O42—C42 | 118.33 (17) |
H23A—C23—H23B | 109.5 | O43—C44—O44 | 124.08 (18) |
C22—C23—H23C | 109.5 | O43—C44—N44 | 123.88 (18) |
H23A—C23—H23C | 109.5 | O44—C44—N44 | 112.04 (17) |
H23B—C23—H23C | 109.5 | O44—C45—C46 | 111.80 (18) |
N22—N21—Co2 | 108.10 (12) | O44—C45—H45A | 109.3 |
N22—N21—H21A | 110.1 | C46—C45—H45A | 109.3 |
Co2—N21—H21A | 110.1 | O44—C45—H45B | 109.3 |
N22—N21—H21B | 110.1 | C46—C45—H45B | 109.3 |
Co2—N21—H21B | 110.1 | H45A—C45—H45B | 107.9 |
H21A—N21—H21B | 108.4 | C45—C46—H46A | 109.5 |
C21—N22—N21 | 117.67 (16) | C45—C46—H46B | 109.5 |
C21—N22—H22 | 121.2 | H46A—C46—H46B | 109.5 |
N21—N22—H22 | 121.2 | C45—C46—H46C | 109.5 |
C21—O21—Co2 | 111.03 (13) | H46A—C46—H46C | 109.5 |
C21—O22—C22 | 117.05 (16) | H46B—C46—H46C | 109.5 |
O23—C24—N24 | 124.32 (19) | N44—N43—Co4 | 108.77 (11) |
O23—C24—O24 | 123.81 (19) | N44—N43—H43D | 109.9 |
N24—C24—O24 | 111.84 (18) | Co4—N43—H43D | 109.9 |
O24—C25—C26 | 109.86 (19) | N44—N43—H43E | 109.9 |
O24—C25—H25A | 109.7 | Co4—N43—H43E | 109.9 |
C26—C25—H25A | 109.7 | H43D—N43—H43E | 108.3 |
O24—C25—H25B | 109.7 | C44—N44—N43 | 116.73 (16) |
C26—C25—H25B | 109.7 | C44—N44—H44 | 121.6 |
H25A—C25—H25B | 108.2 | N43—N44—H44 | 121.6 |
C25—C26—H26A | 109.5 | C44—O43—Co4 | 112.87 (12) |
C25—C26—H26B | 109.5 | C44—O44—C45 | 116.64 (16) |
H26A—C26—H26B | 109.5 | O45—C47—O46 | 124.43 (19) |
C25—C26—H26C | 109.5 | O45—C47—N46 | 124.01 (19) |
H26A—C26—H26C | 109.5 | O46—C47—N46 | 111.57 (18) |
H26B—C26—H26C | 109.5 | O46—C48—C49 | 111.5 (2) |
N24—N23—Co2 | 107.04 (11) | O46—C48—H48A | 109.3 |
N24—N23—H23D | 110.3 | C49—C48—H48A | 109.3 |
Co2—N23—H23D | 110.3 | O46—C48—H48B | 109.3 |
N24—N23—H23E | 110.3 | C49—C48—H48B | 109.3 |
Co2—N23—H23E | 110.3 | H48A—C48—H48B | 108.0 |
H23D—N23—H23E | 108.6 | C48—C49—H49A | 109.5 |
C24—N24—N23 | 117.26 (16) | C48—C49—H49B | 109.5 |
C24—N24—H24 | 121.4 | H49A—C49—H49B | 109.5 |
N23—N24—H24 | 121.4 | C48—C49—H49C | 109.5 |
C24—O23—Co2 | 112.50 (13) | H49A—C49—H49C | 109.5 |
C24—O24—C25 | 117.56 (17) | H49B—C49—H49C | 109.5 |
O25—C27—N26 | 124.0 (2) | N46—N45—Co4 | 108.25 (11) |
O25—C27—O26 | 123.7 (2) | N46—N45—H45C | 110.0 |
N26—C27—O26 | 112.28 (19) | Co4—N45—H45C | 110.0 |
C29A—C28A—O26 | 105.3 (4) | N46—N45—H45D | 110.0 |
C29A—C28A—H28A | 110.7 | Co4—N45—H45D | 110.0 |
O26—C28A—H28A | 110.7 | H45C—N45—H45D | 108.4 |
C29A—C28A—H28B | 110.7 | C47—N46—N45 | 117.52 (16) |
O26—C28A—H28B | 110.7 | C47—N46—H46 | 121.2 |
H28A—C28A—H28B | 108.8 | N45—N46—H46 | 121.2 |
C29B—C28B—O26 | 96.2 (7) | C47—O45—Co4 | 111.73 (13) |
C29B—C28B—H28C | 112.5 | C47—O46—C48 | 116.51 (16) |
O26—C28B—H28C | 112.5 | O103—N101—O102 | 120.49 (18) |
C29B—C28B—H28D | 112.5 | O103—N101—O101 | 120.18 (18) |
O26—C28B—H28D | 112.5 | O102—N101—O101 | 119.32 (17) |
H28C—C28B—H28D | 110.0 | O113—N111—O112 | 120.81 (17) |
N26—N25—Co2 | 107.93 (12) | O113—N111—O111 | 119.44 (17) |
N26—N25—H25C | 110.1 | O112—N111—O111 | 119.74 (17) |
Co2—N25—H25C | 110.1 | O122—N121—O123 | 120.79 (18) |
N26—N25—H25D | 110.1 | O122—N121—O121 | 120.60 (18) |
Co2—N25—H25D | 110.1 | O123—N121—O121 | 118.61 (18) |
H25C—N25—H25D | 108.4 | O133—N131—O132 | 121.02 (19) |
C27—N26—N25 | 116.92 (17) | O133—N131—O131 | 119.27 (18) |
C27—N26—H26 | 121.5 | O132—N131—O131 | 119.70 (17) |
N25—N26—H26 | 121.5 | O143—N141—O142 | 120.88 (17) |
C27—O25—Co2 | 113.10 (13) | O143—N141—O141 | 119.85 (17) |
C27—O26—C28B | 117.6 (4) | O142—N141—O141 | 119.26 (17) |
C27—O26—C28A | 114.9 (3) | O153—N151—O152 | 120.41 (18) |
C28B—O26—C28A | 34.7 (4) | O153—N151—O151 | 120.42 (18) |
O33—Co3—O35 | 95.25 (5) | O152—N151—O151 | 119.17 (17) |
O33—Co3—O31 | 89.16 (5) | O163—N161—O162 | 121.33 (18) |
O35—Co3—O31 | 94.10 (5) | O163—N161—O161 | 119.76 (17) |
O33—Co3—N35 | 95.97 (6) | O162—N161—O161 | 118.91 (17) |
O35—Co3—N35 | 78.98 (6) | O173—N171—O172 | 120.72 (17) |
O31—Co3—N35 | 171.71 (6) | O173—N171—O171 | 120.05 (16) |
O33—Co3—N31 | 167.01 (6) | O172—N171—O171 | 119.23 (16) |
O11—Co1—N11—N12 | −16.86 (11) | O25—C27—O26—C28A | −19.3 (4) |
O15—Co1—N11—N12 | 70.60 (12) | N26—C27—O26—C28A | 160.2 (3) |
O13—Co1—N11—N12 | −68.5 (4) | C29B—C28B—O26—C27 | −91.4 (7) |
N13—Co1—N11—N12 | −114.45 (12) | C29B—C28B—O26—C28A | 3.3 (6) |
N15—Co1—N11—N12 | 148.57 (12) | C29A—C28A—O26—C27 | 133.8 (3) |
O11—C11—N12—N11 | −13.1 (3) | C29A—C28A—O26—C28B | 30.7 (6) |
O12—C11—N12—N11 | 170.23 (16) | O33—Co3—N31—N32 | −20.7 (3) |
Co1—N11—N12—C11 | 21.0 (2) | O35—Co3—N31—N32 | 89.93 (12) |
O12—C11—O11—Co1 | 172.74 (16) | O31—Co3—N31—N32 | −4.40 (12) |
N12—C11—O11—Co1 | −3.6 (3) | N35—Co3—N31—N32 | 168.74 (12) |
O15—Co1—O11—C11 | −82.34 (15) | N33—Co3—N31—N32 | −93.13 (13) |
O13—Co1—O11—C11 | −176.49 (14) | O31—C31—N32—N31 | −0.8 (3) |
N13—Co1—O11—C11 | 104.05 (15) | O32—C31—N32—N31 | 179.09 (17) |
N15—Co1—O11—C11 | −56.5 (3) | Co3—N31—N32—C31 | 4.4 (2) |
N11—Co1—O11—C11 | 11.81 (14) | O32—C31—O31—Co3 | 176.67 (16) |
O11—C11—O12—C12 | 4.3 (3) | N32—C31—O31—Co3 | −3.4 (3) |
N12—C11—O12—C12 | −178.97 (19) | O33—Co3—O31—C31 | −179.30 (14) |
C13—C12—O12—C11 | 86.4 (3) | O35—Co3—O31—C31 | −84.10 (14) |
O11—Co1—N13—N14 | 102.08 (13) | N31—Co3—O31—C31 | 4.32 (14) |
O13—Co1—N13—N14 | 7.83 (12) | N33—Co3—O31—C31 | 102.58 (14) |
N15—Co1—N13—N14 | −83.09 (13) | O31—C31—O32—C32 | 4.2 (3) |
N11—Co1—N13—N14 | −179.90 (13) | N32—C31—O32—C32 | −175.75 (18) |
O13—C14—N14—N13 | 2.4 (3) | C33—C32—O32—C31 | −163.38 (19) |
O14—C14—N14—N13 | −176.86 (17) | O33—Co3—N33—N34 | −17.32 (11) |
Co1—N13—N14—C14 | −8.2 (2) | O31—Co3—N33—N34 | 71.73 (12) |
N14—C14—O13—Co1 | 5.1 (3) | N35—Co3—N33—N34 | −111.98 (12) |
O14—C14—O13—Co1 | −175.76 (16) | N31—Co3—N33—N34 | 150.03 (11) |
O11—Co1—O13—C14 | −104.45 (14) | O33—C34—N34—N33 | −17.1 (3) |
O15—Co1—O13—C14 | 166.81 (14) | O34—C34—N34—N33 | 164.95 (16) |
N13—Co1—O13—C14 | −7.15 (14) | Co3—N33—N34—C34 | 23.07 (19) |
N15—Co1—O13—C14 | 89.04 (14) | O34—C34—O33—Co3 | 177.68 (15) |
N11—Co1—O13—C14 | −54.2 (4) | N34—C34—O33—Co3 | 0.0 (2) |
O13—C14—O14—C15 | 4.9 (3) | O35—Co3—O33—C34 | −174.28 (13) |
N14—C14—O14—C15 | −175.89 (18) | O31—Co3—O33—C34 | −80.24 (14) |
C16—C15—O14—C14 | −80.9 (2) | N35—Co3—O33—C34 | 106.29 (14) |
O11—Co1—N15—N16 | −28.4 (3) | N31—Co3—O33—C34 | −64.3 (3) |
O15—Co1—N15—N16 | −1.97 (12) | N33—Co3—O33—C34 | 10.36 (13) |
O13—Co1—N15—N16 | 91.97 (12) | O33—C34—O34—C35 | 3.4 (3) |
N13—Co1—N15—N16 | 170.92 (12) | N34—C34—O34—C35 | −178.67 (17) |
N11—Co1—N15—N16 | −94.38 (13) | C36—C35—O34—C34 | 174.7 (2) |
O15—C17—N16—N15 | −1.3 (3) | O33—Co3—N35—N36 | 103.27 (12) |
O16—C17—N16—N15 | 177.74 (17) | O35—Co3—N35—N36 | 9.06 (12) |
Co1—N15—N16—C17 | 2.4 (2) | N31—Co3—N35—N36 | −78.86 (12) |
N16—C17—O15—Co1 | −0.6 (3) | N33—Co3—N35—N36 | −178.01 (12) |
O16—C17—O15—Co1 | −179.56 (17) | O35—C37—N36—N35 | 2.9 (3) |
O11—Co1—O15—C17 | 174.60 (16) | O36—C37—N36—N35 | −177.45 (16) |
O13—Co1—O15—C17 | −89.78 (16) | Co3—N35—N36—C37 | −9.5 (2) |
N15—Co1—O15—C17 | 1.49 (15) | N36—C37—O35—Co3 | 5.8 (2) |
N11—Co1—O15—C17 | 97.14 (16) | O36—C37—O35—Co3 | −173.81 (15) |
O15—C17—O16—C18A | −17.9 (4) | O33—Co3—O35—C37 | −103.34 (14) |
N16—C17—O16—C18A | 163.1 (3) | O31—Co3—O35—C37 | 167.13 (13) |
O15—C17—O16—C18B | 17.6 (6) | N35—Co3—O35—C37 | −8.27 (13) |
N16—C17—O16—C18B | −161.5 (5) | N31—Co3—O35—C37 | 88.85 (14) |
C19A—C18A—O16—C17 | 140.5 (4) | O35—C37—O36—C38 | 8.9 (3) |
C19A—C18A—O16—C18B | 56.0 (7) | N36—C37—O36—C38 | −170.72 (17) |
C19B—C18B—O16—C17 | −166.6 (8) | C39—C38—O36—C37 | −89.8 (2) |
C19B—C18B—O16—C18A | −55.6 (9) | O41—Co4—N41—N42 | 7.45 (11) |
O23—Co2—N21—N22 | −93.57 (13) | O43—Co4—N41—N42 | −88.92 (12) |
O21—Co2—N21—N22 | −2.18 (12) | O45—Co4—N41—N42 | 42.1 (3) |
N25—Co2—N21—N22 | 84.79 (13) | N45—Co4—N41—N42 | 98.91 (12) |
N23—Co2—N21—N22 | −171.73 (13) | N43—Co4—N41—N42 | −165.67 (11) |
O21—C21—N22—N21 | 2.6 (3) | O41—C41—N42—N41 | 3.9 (3) |
O22—C21—N22—N21 | −177.79 (17) | O42—C41—N42—N41 | −177.95 (16) |
Co2—N21—N22—C21 | 0.8 (2) | Co4—N41—N42—C41 | −8.5 (2) |
O22—C21—O21—Co2 | 175.97 (16) | N42—C41—O41—Co4 | 3.5 (2) |
N22—C21—O21—Co2 | −4.5 (3) | O42—C41—O41—Co4 | −174.43 (15) |
O25—Co2—O21—C21 | −171.25 (14) | O43—Co4—O41—C41 | 80.55 (14) |
O23—Co2—O21—C21 | 95.22 (14) | O45—Co4—O41—C41 | −178.03 (13) |
N21—Co2—O21—C21 | 3.50 (14) | N45—Co4—O41—C41 | −99.58 (14) |
N25—Co2—O21—C21 | −93.55 (14) | N41—Co4—O41—C41 | −6.21 (13) |
N23—Co2—O21—C21 | 60.0 (3) | O41—C41—O42—C42 | −9.6 (3) |
O21—C21—O22—C22 | −5.7 (3) | N42—C41—O42—C42 | 172.28 (17) |
N22—C21—O22—C22 | 174.70 (18) | C43—C42—O42—C41 | −106.3 (2) |
C23—C22—O22—C21 | 89.1 (2) | O43—Co4—N43—N44 | −0.61 (12) |
O25—Co2—N23—N24 | −85.66 (12) | O45—Co4—N43—N44 | −102.70 (12) |
O23—Co2—N23—N24 | 7.55 (11) | N45—Co4—N43—N44 | 179.03 (12) |
N21—Co2—N23—N24 | 98.75 (12) | N41—Co4—N43—N44 | 83.99 (13) |
O21—Co2—N23—N24 | 43.7 (3) | O43—C44—N44—N43 | 1.4 (3) |
N25—Co2—N23—N24 | −163.52 (12) | O44—C44—N44—N43 | −178.36 (16) |
O23—C24—N24—N23 | 6.2 (3) | Co4—N43—N44—C44 | −0.1 (2) |
O24—C24—N24—N23 | −175.75 (16) | O44—C44—O43—Co4 | 177.82 (15) |
Co2—N23—N24—C24 | −9.6 (2) | N44—C44—O43—Co4 | −2.0 (2) |
N24—C24—O23—Co2 | 1.4 (3) | O41—Co4—O43—C44 | 177.81 (13) |
O24—C24—O23—Co2 | −176.45 (15) | O45—Co4—O43—C44 | 86.64 (13) |
O25—Co2—O23—C24 | 84.79 (14) | N43—Co4—O43—C44 | 1.32 (13) |
N21—Co2—O23—C24 | −98.98 (14) | N41—Co4—O43—C44 | −104.45 (14) |
O21—Co2—O23—C24 | −177.84 (14) | O43—C44—O44—C45 | −7.6 (3) |
N23—Co2—O23—C24 | −5.20 (14) | N44—C44—O44—C45 | 172.22 (17) |
O23—C24—O24—C25 | −6.5 (3) | C46—C45—O44—C44 | 79.3 (2) |
N24—C24—O24—C25 | 175.49 (18) | O41—Co4—N45—N46 | −90.76 (13) |
C26—C25—O24—C24 | −88.9 (2) | O45—Co4—N45—N46 | −1.21 (12) |
O25—Co2—N25—N26 | −1.47 (12) | N43—Co4—N45—N46 | 85.79 (13) |
N21—Co2—N25—N26 | −177.79 (12) | N41—Co4—N45—N46 | −168.88 (13) |
O21—Co2—N25—N26 | −99.25 (13) | O45—C47—N46—N45 | −1.7 (3) |
N23—Co2—N25—N26 | 86.45 (13) | O46—C47—N46—N45 | 178.43 (17) |
O25—C27—N26—N25 | −2.8 (3) | Co4—N45—N46—C47 | 1.9 (2) |
O26—C27—N26—N25 | 177.69 (19) | O46—C47—O45—Co4 | −179.68 (16) |
Co2—N25—N26—C27 | 2.6 (2) | N46—C47—O45—Co4 | 0.5 (3) |
N26—C27—O25—Co2 | 1.3 (3) | O41—Co4—O45—C47 | 92.72 (14) |
O26—C27—O25—Co2 | −179.3 (2) | O43—Co4—O45—C47 | −171.34 (14) |
O23—Co2—O25—C27 | 179.18 (16) | N45—Co4—O45—C47 | 0.47 (14) |
O21—Co2—O25—C27 | 86.99 (16) | N43—Co4—O45—C47 | −94.30 (14) |
N25—Co2—O25—C27 | 0.26 (16) | N41—Co4—O45—C47 | 58.9 (3) |
N23—Co2—O25—C27 | −102.76 (16) | O45—C47—O46—C48 | −5.5 (3) |
O25—C27—O26—C28B | 19.5 (6) | N46—C47—O46—C48 | 174.34 (18) |
N26—C27—O26—C28B | −161.0 (5) | C49—C48—O46—C47 | 84.0 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N11—H11A···O152 | 0.92 | 2.40 | 3.166 (2) | 140 |
N11—H11A···O163 | 0.92 | 2.60 | 3.111 (2) | 116 |
N11—H11A···O171 | 0.92 | 2.64 | 3.188 (2) | 119 |
N11—H11B···O142 | 0.92 | 2.19 | 3.028 (2) | 151 |
N12—H12···O172 | 0.88 | 2.19 | 2.931 (2) | 141 |
N13—H13D···O151 | 0.92 | 2.10 | 2.947 (2) | 153 |
N13—H13D···O152 | 0.92 | 2.40 | 3.155 (2) | 139 |
N13—H13E···O162 | 0.92 | 2.12 | 3.016 (2) | 166 |
N13—H13E···O163 | 0.92 | 2.64 | 3.395 (3) | 140 |
N14—H14···O131i | 0.88 | 2.09 | 2.939 (2) | 161 |
N14—H14···O132i | 0.88 | 2.33 | 3.053 (2) | 140 |
N15—H15C···O143 | 0.92 | 2.14 | 2.968 (2) | 149 |
N15—H15C···O151 | 0.92 | 2.45 | 2.984 (2) | 117 |
N15—H15D···O161ii | 0.92 | 2.06 | 2.982 (2) | 176 |
N15—H15D···O163ii | 0.92 | 2.66 | 3.307 (2) | 128 |
N16—H16···O171ii | 0.88 | 2.09 | 2.889 (2) | 151 |
N21—H21A···O101iii | 0.92 | 2.28 | 3.013 (2) | 137 |
N21—H21A···O103iii | 0.92 | 2.43 | 3.336 (2) | 167 |
N21—H21B···O121 | 0.92 | 2.10 | 2.939 (2) | 151 |
N21—H21B···O112iii | 0.92 | 2.44 | 2.979 (2) | 117 |
N22—H22···O131 | 0.88 | 2.05 | 2.907 (2) | 164 |
N23—H23D···O113iv | 0.92 | 2.26 | 3.166 (2) | 169 |
N23—H23D···O111iv | 0.92 | 2.39 | 3.121 (2) | 136 |
N23—H23E···O111iii | 0.92 | 2.34 | 3.141 (2) | 146 |
N23—H23E···O112iii | 0.92 | 2.64 | 3.496 (2) | 156 |
N24—H24···O122iv | 0.88 | 2.16 | 2.852 (2) | 135 |
N25—H25C···O102 | 0.92 | 2.12 | 3.038 (2) | 176 |
N25—H25C···O103 | 0.92 | 2.57 | 3.243 (2) | 130 |
N25—H25D···O122 | 0.92 | 2.02 | 2.924 (2) | 169 |
N26—H26···O111 | 0.88 | 2.25 | 3.043 (2) | 150 |
N31—H31A···O112 | 0.92 | 2.12 | 2.970 (2) | 153 |
N31—H31A···O101 | 0.92 | 2.63 | 3.152 (2) | 116 |
N31—H31B···O131ii | 0.92 | 2.16 | 3.073 (2) | 175 |
N31—H31B···O133ii | 0.92 | 2.61 | 3.303 (3) | 133 |
N32—H32···O121ii | 0.88 | 2.26 | 2.992 (2) | 141 |
N32—H32···O123ii | 0.88 | 2.42 | 3.234 (3) | 154 |
N33—H33D···O102 | 0.92 | 2.31 | 3.083 (2) | 142 |
N33—H33E···O113 | 0.92 | 2.25 | 3.071 (2) | 149 |
N34—H34···O123 | 0.88 | 2.21 | 2.929 (2) | 139 |
N35—H35C···O101 | 0.92 | 2.06 | 2.922 (2) | 155 |
N35—H35C···O102 | 0.92 | 2.50 | 3.233 (2) | 136 |
N35—H35D···O132 | 0.92 | 2.11 | 3.025 (2) | 171 |
N36—H36···O161i | 0.88 | 2.04 | 2.896 (2) | 164 |
N36—H36···O162i | 0.88 | 2.46 | 3.144 (2) | 135 |
N41—H41A···O141v | 0.92 | 2.30 | 3.066 (2) | 140 |
N41—H41A···O142v | 0.92 | 2.36 | 3.255 (2) | 165 |
N41—H41B···O141iii | 0.92 | 2.32 | 3.088 (2) | 141 |
N41—H41B···O143iii | 0.92 | 2.60 | 3.460 (2) | 156 |
N42—H42···O173v | 0.88 | 2.09 | 2.818 (2) | 139 |
N43—H43D···O152 | 0.92 | 2.11 | 3.018 (2) | 169 |
N43—H43D···O153 | 0.92 | 2.49 | 3.187 (2) | 133 |
N43—H43E···O173 | 0.92 | 1.98 | 2.898 (2) | 175 |
N44—H44···O141 | 0.88 | 2.22 | 3.041 (2) | 155 |
N45—H45C···O151iii | 0.92 | 2.30 | 3.028 (2) | 136 |
N45—H45C···O153iii | 0.92 | 2.45 | 3.358 (2) | 169 |
N45—H45D···O171 | 0.92 | 2.13 | 3.012 (2) | 159 |
N46—H46···O161 | 0.88 | 2.13 | 2.991 (2) | 165 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, y−1, z; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C3H8N2O2)3](NO3)2 |
Mr | 495.29 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 120 |
a, b, c (Å) | 28.0291 (6), 8.6245 (2), 35.6763 (7) |
β (°) | 110.2445 (5) |
V (Å3) | 8091.5 (3) |
Z | 16 |
Radiation type | Mo Kα |
µ (mm−1) | 0.92 |
Crystal size (mm) | 0.44 × 0.40 × 0.28 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2003) |
Tmin, Tmax | 0.687, 0.784 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 86674, 18519, 14049 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.091, 1.04 |
No. of reflections | 18519 |
No. of parameters | 1128 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.60, −0.53 |
Computer programs: COLLECT (Nonius, 1998), HKL SCALEPACK (Otwinowski & Minor 1997), HKL DENZO (Otwinowski & Minor 1997), HKL SCALEPACK (Otwinowski & Minor 1997) and SORTAV (Blessing 1995), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997).
Co1—O11 | 2.1005 (15) | Co3—O33 | 2.0896 (14) |
Co1—O15 | 2.1172 (15) | Co3—O35 | 2.1062 (14) |
Co1—O13 | 2.1179 (14) | Co3—O31 | 2.1112 (14) |
Co1—N13 | 2.1236 (17) | Co3—N35 | 2.1285 (17) |
Co1—N15 | 2.1460 (17) | Co3—N31 | 2.1515 (16) |
Co1—N11 | 2.1649 (17) | Co3—N33 | 2.1582 (16) |
Co2—O25 | 2.0853 (14) | Co4—O41 | 2.1063 (14) |
Co2—O23 | 2.1090 (14) | Co4—O43 | 2.1064 (14) |
Co2—N21 | 2.1240 (17) | Co4—O45 | 2.1297 (14) |
Co2—O21 | 2.1270 (14) | Co4—N45 | 2.1338 (16) |
Co2—N25 | 2.1534 (17) | Co4—N43 | 2.1450 (17) |
Co2—N23 | 2.1678 (17) | Co4—N41 | 2.1671 (17) |
D—H···A | D—H | H···A | D···A | D—H···A |
N11—H11A···O152 | 0.92 | 2.40 | 3.166 (2) | 140 |
N11—H11A···O163 | 0.92 | 2.60 | 3.111 (2) | 116 |
N11—H11A···O171 | 0.92 | 2.64 | 3.188 (2) | 119 |
N11—H11B···O142 | 0.92 | 2.19 | 3.028 (2) | 151 |
N12—H12···O172 | 0.88 | 2.19 | 2.931 (2) | 141 |
N13—H13D···O151 | 0.92 | 2.10 | 2.947 (2) | 153 |
N13—H13D···O152 | 0.92 | 2.40 | 3.155 (2) | 139 |
N13—H13E···O162 | 0.92 | 2.12 | 3.016 (2) | 166 |
N13—H13E···O163 | 0.92 | 2.64 | 3.395 (3) | 140 |
N14—H14···O131i | 0.88 | 2.09 | 2.939 (2) | 161 |
N14—H14···O132i | 0.88 | 2.33 | 3.053 (2) | 140 |
N15—H15C···O143 | 0.92 | 2.14 | 2.968 (2) | 149 |
N15—H15C···O151 | 0.92 | 2.45 | 2.984 (2) | 117 |
N15—H15D···O161ii | 0.92 | 2.06 | 2.982 (2) | 176 |
N15—H15D···O163ii | 0.92 | 2.66 | 3.307 (2) | 128 |
N16—H16···O171ii | 0.88 | 2.09 | 2.889 (2) | 151 |
N21—H21A···O101iii | 0.92 | 2.28 | 3.013 (2) | 137 |
N21—H21A···O103iii | 0.92 | 2.43 | 3.336 (2) | 167 |
N21—H21B···O121 | 0.92 | 2.10 | 2.939 (2) | 151 |
N21—H21B···O112iii | 0.92 | 2.44 | 2.979 (2) | 117 |
N22—H22···O131 | 0.88 | 2.05 | 2.907 (2) | 164 |
N23—H23D···O113iv | 0.92 | 2.26 | 3.166 (2) | 169 |
N23—H23D···O111iv | 0.92 | 2.39 | 3.121 (2) | 136 |
N23—H23E···O111iii | 0.92 | 2.34 | 3.141 (2) | 146 |
N23—H23E···O112iii | 0.92 | 2.64 | 3.496 (2) | 156 |
N24—H24···O122iv | 0.88 | 2.16 | 2.852 (2) | 135 |
N25—H25C···O102 | 0.92 | 2.12 | 3.038 (2) | 176 |
N25—H25C···O103 | 0.92 | 2.57 | 3.243 (2) | 130 |
N25—H25D···O122 | 0.92 | 2.02 | 2.924 (2) | 169 |
N26—H26···O111 | 0.88 | 2.25 | 3.043 (2) | 150 |
N31—H31A···O112 | 0.92 | 2.12 | 2.970 (2) | 153 |
N31—H31A···O101 | 0.92 | 2.63 | 3.152 (2) | 116 |
N31—H31B···O131ii | 0.92 | 2.16 | 3.073 (2) | 175 |
N31—H31B···O133ii | 0.92 | 2.61 | 3.303 (3) | 133 |
N32—H32···O121ii | 0.88 | 2.26 | 2.992 (2) | 141 |
N32—H32···O123ii | 0.88 | 2.42 | 3.234 (3) | 154 |
N33—H33D···O102 | 0.92 | 2.31 | 3.083 (2) | 142 |
N33—H33E···O113 | 0.92 | 2.25 | 3.071 (2) | 149 |
N34—H34···O123 | 0.88 | 2.21 | 2.929 (2) | 139 |
N35—H35C···O101 | 0.92 | 2.06 | 2.922 (2) | 155 |
N35—H35C···O102 | 0.92 | 2.50 | 3.233 (2) | 136 |
N35—H35D···O132 | 0.92 | 2.11 | 3.025 (2) | 171 |
N36—H36···O161i | 0.88 | 2.04 | 2.896 (2) | 164 |
N36—H36···O162i | 0.88 | 2.46 | 3.144 (2) | 135 |
N41—H41A···O141v | 0.92 | 2.30 | 3.066 (2) | 140 |
N41—H41A···O142v | 0.92 | 2.36 | 3.255 (2) | 165 |
N41—H41B···O141iii | 0.92 | 2.32 | 3.088 (2) | 141 |
N41—H41B···O143iii | 0.92 | 2.60 | 3.460 (2) | 156 |
N42—H42···O173v | 0.88 | 2.09 | 2.818 (2) | 139 |
N43—H43D···O152 | 0.92 | 2.11 | 3.018 (2) | 169 |
N43—H43D···O153 | 0.92 | 2.49 | 3.187 (2) | 133 |
N43—H43E···O173 | 0.92 | 1.98 | 2.898 (2) | 175 |
N44—H44···O141 | 0.88 | 2.22 | 3.041 (2) | 155 |
N45—H45C···O151iii | 0.92 | 2.30 | 3.028 (2) | 136 |
N45—H45C···O153iii | 0.92 | 2.45 | 3.358 (2) | 169 |
N45—H45D···O171 | 0.92 | 2.13 | 3.012 (2) | 159 |
N46—H46···O161 | 0.88 | 2.13 | 2.991 (2) | 165 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x, y−1, z; (iii) x, y+1, z; (iv) −x+3/2, y+1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2. |
The title compound, (I), was recently described by Zhang et al. (2005). We inadvertantly prepared the same material, and report here its structure. The cell described here has a doubled a axis and doubled volume compared to the Zhang unit cell and its aymmetric unit contains four [Co(C3H8N2O2)3]2+ cations and eight nitrate anions, compared to two cations and four anions in the Zhang model in the same space group. It is notable that both the cations showed disorder in the Zhang model, and visual comparison of the two structures suggest that they are closely related. It seems that the previous unit cell may have been too small. However, in such a complex system, it is possible that the present structure and the Zhang structure are actually polymorphs, perhaps with different hydrogen bonding motifs.
The four complex cations in (I) are similar (Fig. 1) and are each built up around a slightly distorted fac-CoN3O3 octahedral core (Table 1). In every case, a five-membered –Co—N—N—C—O– chelate ring arises for the twelve distinct N,O-bidentate ligands. In the Co1 and Co2-containing cations, one of the ethyl-carbazate ligands shows disorder of its ethyl side chains.
One feature of the crystal of (I) is a very short nitro-O133···C34 contact of 2.706 (3) Å. The displacement ellipsoid of O133 is suggestive of disorder, but attempts to model this feature with split-site atom schemes were not successful. There is some literature precedent for short O···C contacts arising from nitro groups. For example, in (C14H22N2O)2.CuCl(NO3)3 (Indira et al., 1993), an intermolecular nitro-O···C separation of 2.680 (5) Å occurs, which is even shorter than the value reported here.
The crystal packing for (I) is consolidated by a large number of cation-to-anion N—H···O hydrogen bonds (Table 2), a number of which are bifurcated. This helps to generate a structure (Fig. 2) in which [010] columns of cation are present, with the nitrate anions occupying the space between the columns. It is notable that the cores of the columns appear to be made up of the hydrophobic ethyl side chains of the ligands.