The present study of the title compound, [Co(C
3H
8N
2O
2)
3](NO
3)
2, probably represents a correction to that reported by Zhang, Song, Zhang, Ma & Yu [
Z. Naturforsch. Teil B (2005),
60, 505–510] with a doubled
a axis. As modelled here, there are four independent cations, each built up around a
fac-CoN
3O
3 octahedron, and eight anions in the asymmetric unit. Two of the cations show disorder in one of their ethyl side chains in ratios of 0.712 (10):0.288 (10) and 0.612 (7):0.388 (8). Numerous cation-to-anion N—H
O hydrogen bonds, many of which are bifurcated, help to establish the crystal packing.
Supporting information
CCDC reference: 672666
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.004 Å
- Disorder in main residue
- R factor = 0.037
- wR factor = 0.091
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact O133 .. C34 .. 2.71 Ang.
| Author Response: this is discussed in the text of the paper
|
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.59 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.88 Ratio
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.66 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.91 Ratio
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.59 Ratio
PLAT221_ALERT_4_C Large Solvent/Anion O Ueq(max)/Ueq(min) ... 3.42 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.55 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.58 Ratio
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.68 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O26
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N131
PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc.
PLAT430_ALERT_2_C Short Inter D...A Contact O111 .. O122 .. 2.89 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O163 .. C11 .. 2.93 Ang.
| Author Response: this is discussed in the text of the paper
|
PLAT432_ALERT_2_C Short Inter X...Y Contact C29A .. C18B .. 3.13 Ang.
| Author Response: this is discussed in the text of the paper
|
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11A .. O171 .. 2.64 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H13E .. O163 .. 2.64 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H15D .. O163 .. 2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H23E .. O112 .. 2.64 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H31A .. O101 .. 2.63 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H31B .. O133 .. 2.61 Ang.
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 32.90 Deg.
C18A -O16 -C18B 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 34.70 Deg.
C28B -O26 -C28A 1.555 1.555 1.555
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
25 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
12 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
9 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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).
tris(ethyl carbazate-
κ2N,
O)cobalt(II) dinitrate
top
Crystal data top
[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 | |
Data collection top
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 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)] = 0.037 | 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 |
Crystal data top
[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)° | |
Data collection top
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 | |
Refinement top
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 | |
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 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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) | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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) |
Hydrogen-bond geometry (Å, º) top
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 |
Selected bond lengths (Å) topCo1—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) |
Hydrogen-bond geometry (Å, º) top
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.