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Acta Cryst. (2007). E63, m3028-m3029    [ doi:10.1107/S1600536807055584 ]

Redetermination of tris(ethyl carbazate-[kappa]2N,O)cobalt(II) dinitrate

K. Srinivasan, S. Govindarajan and W. T. A. Harrison

Abstract top

The present study of the title compound, [Co(C3H8N2O2)3](NO3)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-CoN3O3 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.

Comment top

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.

Related literature top

For the previous determination of the structure, see: Zhang et al. (2005). For background, see: Indira et al. (1993).

Experimental top

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.

Refinement top

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).

Computing details top

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).

Figures top
[Figure 1] Fig. 1. View of the Co3-containing complex cation in (I) shoiwng 50% displacement ellipsoids (arbitrary spheres for the H atoms). The C-bound H atoms are omitted for clarity.
[Figure 2] Fig. 2. Unit cell packing in (I) viewed down [010] with H atoms and minor disorder components omitted for clarity.
tris(ethyl carbazate-κ2N,O)cobalt(II) dinitrate top
Crystal data top
[Co(C3H8N2O2)3](NO3)2F000 = 4112
Mr = 495.29Dx = 1.626 Mg m−3
Monoclinic, P21/nMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 19276 reflections
a = 28.0291 (6) Åθ = 2.9–27.5º
b = 8.6245 (2) ŵ = 0.92 mm−1
c = 35.6763 (7) ÅT = 120 (2) K
β = 110.2445 (5)ºBlock, pink
V = 8091.5 (3) Å30.44 × 0.40 × 0.28 mm
Z = 16
Data collection top
Nonius KappaCCD
diffractometer		18519 independent reflections
Radiation source: fine-focus sealed tube14049 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.049
T = 120(2) Kθmax = 27.5º
ω and φ scansθmin = 2.9º
Absorption correction: multi-scan
(SADABS; Bruker, 2003)		h = −36→36
Tmin = 0.687, Tmax = 0.784k = −10→11
86674 measured reflectionsl = −46→46
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.091  w = 1/[σ2(Fo2) + (0.0347P)2 + 4.8866P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.003
18519 reflectionsΔρmax = 0.60 e Å−3
1128 parametersΔρmin = −0.53 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Co(C3H8N2O2)3](NO3)2V = 8091.5 (3) Å3
Mr = 495.29Z = 16
Monoclinic, P21/nMo Kα
a = 28.0291 (6) ŵ = 0.92 mm−1
b = 8.6245 (2) ÅT = 120 (2) K
c = 35.6763 (7) Å0.44 × 0.40 × 0.28 mm
β = 110.2445 (5)º
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 = 0.784Rint = 0.049
86674 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0371128 parameters
wR(F2) = 0.091H-atom parameters constrained
S = 1.04Δρmax = 0.60 e Å−3
18519 reflectionsΔρmin = −0.53 e Å−3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement 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
xyzUiso*/UeqOcc. (<1)
Co10.378517 (10)0.22555 (3)0.109456 (8)0.01724 (7)
C110.43324 (8)0.5019 (2)0.13542 (7)0.0232 (5)
C120.49470 (10)0.6426 (3)0.11677 (9)0.0451 (7)
H12A0.50160.54110.10670.054*
H12B0.52770.69310.13120.054*
C130.46476 (12)0.7405 (4)0.08305 (9)0.0523 (8)
H13A0.48450.76060.06560.078*
H13B0.45680.83900.09320.078*
H13C0.43310.68700.06790.078*
N110.36718 (6)0.3885 (2)0.15178 (5)0.0209 (4)
H11A0.33700.44080.14050.025*
H11B0.36640.33740.17420.025*
N120.40882 (6)0.4933 (2)0.16183 (5)0.0220 (4)
H120.41800.54890.18390.026*
O110.42745 (5)0.40812 (17)0.10801 (4)0.0234 (3)
O120.46638 (6)0.61959 (19)0.14385 (5)0.0357 (4)
C140.34850 (8)0.1177 (2)0.03016 (6)0.0202 (4)
C150.37987 (9)−0.0675 (3)−0.00506 (7)0.0314 (5)
H15A0.3648−0.1400−0.02760.038*
H15B0.3904−0.12850.02000.038*
C160.42593 (10)0.0086 (3)−0.00952 (9)0.0456 (7)
H16A0.4504−0.0712−0.01040.068*
H16B0.44160.07760.01320.068*
H16C0.41570.0688−0.03430.068*
N130.31313 (7)0.3000 (2)0.06174 (5)0.0212 (4)
H13D0.28440.28650.06830.025*
H13E0.31590.40350.05650.025*
N140.30982 (7)0.2100 (2)0.02783 (5)0.0241 (4)
H140.28290.21510.00590.029*
O130.38688 (5)0.10170 (17)0.06084 (4)0.0219 (3)
O140.34184 (6)0.04539 (18)−0.00426 (4)0.0264 (3)
C170.42888 (8)−0.0037 (3)0.16649 (6)0.0237 (5)
C18A0.51489 (11)−0.0781 (6)0.20164 (14)0.0274 (12)0.712 (10)
H18A0.52240.02320.19180.033*0.712 (10)
H18B0.5265−0.16160.18780.033*0.712 (10)
C19A0.5410 (2)−0.0904 (9)0.24591 (15)0.0488 (16)0.712 (10)
H19A0.5779−0.08960.25220.073*0.712 (10)
H19B0.5310−0.18740.25550.073*0.712 (10)
H19C0.5312−0.00240.25900.073*0.712 (10)
C18B0.5134 (3)−0.0007 (14)0.2175 (3)0.023 (3)0.288 (10)
H18C0.52680.05200.19850.028*0.288 (10)
H18D0.50850.07650.23630.028*0.288 (10)
C19B0.5477 (6)−0.1283 (17)0.2390 (4)0.031 (3)*0.288 (10)
H19D0.5816−0.08630.25340.046*0.288 (10)
H19E0.5500−0.20630.21970.046*0.288 (10)
H19F0.5341−0.17630.25810.046*0.288 (10)
N150.34325 (6)0.03124 (19)0.12700 (5)0.0185 (4)
H15C0.31990.06530.13800.022*
H15D0.3266−0.02900.10510.022*
N160.38162 (6)−0.0566 (2)0.15541 (5)0.0221 (4)
H160.3744−0.14320.16530.026*
O150.44102 (5)0.11584 (18)0.15282 (5)0.0293 (4)
O160.46121 (6)−0.0928 (2)0.19427 (5)0.0350 (4)
Co20.661707 (10)0.76084 (3)0.155900 (8)0.01657 (7)
C210.66557 (8)0.6839 (2)0.08018 (6)0.0198 (4)
C220.62819 (9)0.4910 (3)0.03125 (7)0.0316 (5)
H22A0.62760.42970.05460.038*
H22B0.64120.42350.01450.038*
C230.57506 (11)0.5427 (3)0.00744 (8)0.0499 (7)
H23A0.55350.4516−0.00250.075*
H23B0.57570.6060−0.01520.075*
H23C0.56140.60400.02450.075*
N210.70996 (7)0.8665 (2)0.12868 (5)0.0210 (4)
H21A0.70320.97100.12540.025*
H21B0.74350.85380.14460.025*
N220.70081 (7)0.7952 (2)0.09118 (5)0.0237 (4)
H220.71770.82320.07560.028*
O210.63925 (5)0.64307 (16)0.10010 (4)0.0201 (3)
O220.66203 (6)0.62304 (17)0.04504 (4)0.0266 (3)
C240.60653 (8)1.0327 (2)0.15778 (6)0.0202 (4)
C250.53594 (8)1.1650 (3)0.11072 (7)0.0299 (5)
H25A0.50421.21160.11200.036*
H25B0.52761.06150.09810.036*
C260.55730 (10)1.2659 (3)0.08614 (7)0.0361 (6)
H26A0.53151.28190.05970.054*
H26B0.58711.21550.08320.054*
H26C0.56721.36620.09940.054*
N230.68026 (6)0.9259 (2)0.20469 (5)0.0207 (4)
H23D0.68280.87630.22810.025*
H23E0.71080.97340.20790.025*
N240.64041 (7)1.0370 (2)0.19474 (5)0.0210 (4)
H240.63821.10590.21230.025*
O230.60516 (5)0.93140 (17)0.13296 (4)0.0220 (3)
O240.57298 (6)1.14897 (19)0.15107 (5)0.0301 (4)
C270.63903 (8)0.5134 (3)0.19850 (7)0.0260 (5)
C28A0.5735 (2)0.4775 (7)0.22683 (19)0.0322 (13)0.612 (7)
H28A0.58350.49550.25590.039*0.612 (7)
H28B0.56130.57640.21270.039*0.612 (7)
C29A0.53289 (15)0.3553 (5)0.21343 (12)0.0339 (13)0.612 (7)
H29A0.50250.39080.21860.051*0.612 (7)
H29B0.54530.25910.22820.051*0.612 (7)
H29C0.52430.33650.18480.051*0.612 (7)
C28B0.5622 (3)0.4169 (10)0.2051 (3)0.048 (2)0.388 (7)
H28C0.54500.45710.17780.058*0.388 (7)
H28D0.54790.31440.20810.058*0.388 (7)
C29B0.5609 (4)0.5253 (13)0.2354 (3)0.057 (3)0.388 (7)
H29D0.52550.54610.23270.086*0.388 (7)
H29E0.57730.62230.23230.086*0.388 (7)
H29F0.57890.48140.26190.086*0.388 (7)
N250.71077 (6)0.5678 (2)0.18181 (5)0.0203 (4)
H25C0.71770.51270.16220.024*
H25D0.74100.60280.19990.024*
N260.68546 (6)0.4719 (2)0.20128 (5)0.0227 (4)
H260.70000.38870.21460.027*
O250.61747 (5)0.63310 (18)0.18129 (5)0.0263 (3)
O260.61803 (7)0.4136 (2)0.21639 (6)0.0535 (6)
Co30.861768 (10)0.23284 (3)0.102066 (8)0.01656 (7)
C310.92004 (8)0.0164 (2)0.15870 (6)0.0201 (4)
C321.00754 (8)−0.0041 (3)0.19841 (7)0.0286 (5)
H32A1.01070.07820.21850.034*
H32B1.01550.04110.17570.034*
C331.04293 (9)−0.1347 (3)0.21655 (7)0.0328 (6)
H33A1.0778−0.09540.22740.049*
H33B1.0406−0.21290.19610.049*
H33C1.0336−0.18160.23810.049*
N310.83223 (6)0.03374 (19)0.12312 (5)0.0190 (4)
H31A0.81040.06450.13590.023*
H31B0.8147−0.02920.10200.023*
N320.87400 (6)−0.0467 (2)0.14988 (5)0.0239 (4)
H320.8698−0.13570.16040.029*
O310.92832 (5)0.14003 (16)0.14449 (4)0.0210 (3)
O320.95605 (6)−0.06886 (18)0.18456 (5)0.0290 (4)
C340.91254 (7)0.5176 (2)0.11969 (6)0.0185 (4)
C350.95894 (9)0.6621 (3)0.08829 (7)0.0277 (5)
H35A0.93030.65790.06250.033*
H35B0.98310.57800.08870.033*
C360.98499 (12)0.8170 (3)0.09326 (8)0.0489 (8)
H36A0.99800.83330.07140.073*
H36B1.01330.81950.11880.073*
H36C0.96060.89910.09280.073*
N330.85559 (6)0.39863 (19)0.14547 (5)0.0185 (4)
H33D0.82440.44710.13640.022*
H33E0.85930.35020.16930.022*
N340.89534 (6)0.5077 (2)0.15053 (5)0.0185 (4)
H340.90780.56470.17220.022*
O330.90476 (5)0.41820 (16)0.09329 (4)0.0202 (3)
O340.94035 (6)0.64404 (17)0.12149 (4)0.0239 (3)
C370.82773 (8)0.1031 (2)0.02534 (6)0.0187 (4)
C380.85617 (9)−0.1023 (3)−0.00621 (7)0.0303 (5)
H38A0.8389−0.1896−0.02370.036*
H38B0.8710−0.14220.02140.036*
C390.89794 (12)−0.0420 (4)−0.01941 (9)0.0538 (8)
H39A0.9215−0.1264−0.01900.081*
H39B0.91630.0405−0.00120.081*
H39C0.8833−0.0006−0.04660.081*
N350.79322 (6)0.2941 (2)0.05538 (5)0.0193 (4)
H35C0.76590.28340.06380.023*
H35D0.79460.39550.04780.023*
N360.78822 (7)0.1928 (2)0.02297 (5)0.0203 (4)
H360.76000.18940.00210.024*
O350.86768 (5)0.09820 (16)0.05461 (4)0.0210 (3)
O360.81902 (6)0.01782 (17)−0.00770 (4)0.0242 (3)
Co40.169396 (10)0.75473 (3)0.153429 (8)0.01597 (6)
C410.11708 (8)1.0333 (2)0.15505 (6)0.0182 (4)
C420.05033 (8)1.1801 (3)0.10802 (7)0.0281 (5)
H42A0.01531.19670.10790.034*
H42B0.05011.08930.09100.034*
C430.06818 (10)1.3211 (3)0.09203 (8)0.0358 (6)
H43A0.04491.34250.06490.054*
H43B0.10251.30270.09150.054*
H43C0.06881.41020.10920.054*
N410.18798 (7)0.91604 (19)0.20300 (5)0.0202 (4)
H41A0.18840.86590.22590.024*
H41B0.21950.95900.20750.024*
N420.15002 (7)1.0330 (2)0.19243 (5)0.0208 (4)
H420.14831.10280.20990.025*
O410.11619 (5)0.93343 (16)0.12992 (4)0.0190 (3)
O420.08458 (6)1.15162 (17)0.14867 (4)0.0269 (3)
C440.14550 (7)0.5096 (2)0.19671 (6)0.0170 (4)
C450.07985 (8)0.4684 (3)0.22343 (7)0.0265 (5)
H45A0.08370.57960.23080.032*
H45B0.07570.41020.24600.032*
C460.03322 (9)0.4472 (3)0.18709 (8)0.0345 (6)
H46A0.00330.48290.19290.052*
H46B0.02920.33720.17980.052*
H46C0.03670.50760.16490.052*
N430.21539 (6)0.55428 (19)0.17677 (5)0.0192 (4)
H43D0.22050.49990.15630.023*
H43E0.24660.58420.19450.023*
N440.19016 (6)0.4594 (2)0.19640 (5)0.0199 (4)
H440.20340.37160.20780.024*
O430.12486 (5)0.63135 (16)0.18029 (4)0.0188 (3)
O440.12563 (5)0.41468 (17)0.21669 (5)0.0251 (3)
C470.17398 (8)0.6915 (2)0.07687 (6)0.0194 (4)
C480.13050 (9)0.5236 (3)0.02327 (7)0.0325 (6)
H48A0.13080.44970.04460.039*
H48B0.13940.46560.00270.039*
C490.07804 (10)0.5910 (3)0.00489 (8)0.0441 (7)
H49A0.05340.5070−0.00540.066*
H49B0.07720.6603−0.01710.066*
H49C0.06930.64950.02520.066*
N450.22220 (6)0.8546 (2)0.12932 (5)0.0199 (4)
H45C0.21830.96060.12770.024*
H45D0.25490.83240.14550.024*
N460.21268 (7)0.7915 (2)0.09073 (5)0.0230 (4)
H460.23150.81720.07640.028*
O450.14707 (5)0.64853 (16)0.09604 (4)0.0201 (3)
O460.16830 (6)0.64395 (18)0.04004 (4)0.0273 (4)
N1010.71481 (6)0.2698 (2)0.11364 (5)0.0216 (4)
O1010.72087 (6)0.16852 (17)0.08997 (5)0.0281 (4)
O1020.73847 (6)0.39666 (17)0.11777 (5)0.0300 (4)
O1030.68603 (6)0.24390 (19)0.13268 (5)0.0342 (4)
N1110.79002 (6)0.1855 (2)0.20916 (5)0.0192 (4)
O1110.75882 (6)0.20017 (18)0.22718 (4)0.0253 (3)
O1120.78583 (6)0.07391 (19)0.18579 (5)0.0312 (4)
O1130.82537 (6)0.2811 (2)0.21539 (5)0.0358 (4)
N1210.83351 (7)0.6941 (2)0.20478 (5)0.0222 (4)
O1210.80825 (6)0.71321 (18)0.16828 (4)0.0302 (4)
O1220.81160 (6)0.68252 (19)0.22976 (4)0.0270 (4)
O1230.88088 (6)0.6874 (2)0.21545 (5)0.0369 (4)
N1310.79525 (7)0.7141 (2)0.05358 (5)0.0228 (4)
O1310.77184 (5)0.84304 (16)0.04915 (4)0.0218 (3)
O1320.78612 (6)0.62343 (18)0.02471 (4)0.0308 (4)
O1330.82550 (9)0.6800 (3)0.08622 (6)0.0746 (8)
N1410.29539 (6)0.1812 (2)0.21059 (5)0.0187 (4)
O1410.26319 (5)0.19033 (18)0.22794 (4)0.0241 (3)
O1420.32952 (7)0.2818 (2)0.21749 (5)0.0359 (4)
O1430.29348 (6)0.07125 (19)0.18752 (5)0.0316 (4)
N1510.22660 (6)0.2607 (2)0.11169 (5)0.0217 (4)
O1510.23779 (6)0.15584 (17)0.09150 (4)0.0266 (3)
O1520.24698 (6)0.39237 (18)0.11406 (5)0.0314 (4)
O1530.19592 (6)0.2345 (2)0.12905 (5)0.0362 (4)
N1610.31379 (7)0.7123 (2)0.05965 (5)0.0202 (4)
O1610.29207 (5)0.84470 (16)0.05366 (4)0.0216 (3)
O1620.30895 (7)0.62641 (18)0.03041 (5)0.0334 (4)
O1630.33890 (7)0.6712 (2)0.09410 (5)0.0398 (4)
N1710.34031 (6)0.6733 (2)0.21102 (5)0.0186 (4)
O1710.32225 (6)0.70080 (17)0.17398 (4)0.0228 (3)
O1720.38704 (5)0.64911 (18)0.22713 (5)0.0272 (4)
O1730.31158 (5)0.66930 (18)0.23114 (4)0.0239 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01957 (14)0.01827 (15)0.01411 (13)0.00035 (11)0.00613 (11)0.00113 (11)
C110.0215 (11)0.0184 (11)0.0289 (12)0.0006 (9)0.0078 (9)0.0016 (9)
C120.0348 (14)0.0362 (16)0.068 (2)−0.0076 (12)0.0232 (14)0.0034 (14)
C130.0545 (18)0.053 (2)0.0514 (18)0.0023 (15)0.0207 (15)0.0042 (15)
N110.0217 (9)0.0231 (10)0.0188 (9)0.0009 (7)0.0085 (7)0.0004 (7)
N120.0227 (9)0.0226 (10)0.0184 (9)−0.0007 (7)0.0043 (7)−0.0057 (8)
O110.0271 (8)0.0197 (8)0.0278 (8)0.0004 (6)0.0150 (7)−0.0004 (7)
O120.0350 (9)0.0259 (9)0.0472 (11)−0.0083 (7)0.0156 (8)−0.0043 (8)
C140.0284 (11)0.0191 (11)0.0146 (10)−0.0015 (9)0.0095 (9)0.0003 (8)
C150.0426 (14)0.0243 (13)0.0277 (13)0.0080 (10)0.0126 (11)−0.0060 (10)
C160.0452 (16)0.0494 (18)0.0501 (17)0.0040 (13)0.0266 (14)−0.0125 (14)
N130.0273 (9)0.0207 (9)0.0163 (9)0.0050 (7)0.0086 (7)0.0004 (7)
N140.0278 (10)0.0284 (10)0.0129 (8)0.0076 (8)0.0030 (7)−0.0017 (8)
O130.0247 (8)0.0234 (8)0.0168 (7)0.0039 (6)0.0063 (6)−0.0015 (6)
O140.0341 (9)0.0275 (9)0.0172 (7)0.0061 (7)0.0085 (7)−0.0039 (6)
C170.0202 (10)0.0308 (13)0.0212 (11)0.0040 (9)0.0087 (9)0.0080 (10)
C18A0.0170 (16)0.031 (3)0.032 (2)0.0015 (14)0.0066 (14)0.0084 (19)
C19A0.034 (3)0.086 (5)0.023 (2)−0.015 (3)0.005 (2)−0.004 (3)
C18B0.016 (4)0.027 (6)0.024 (5)0.002 (3)0.004 (3)0.003 (4)
N150.0179 (8)0.0198 (9)0.0169 (9)0.0009 (7)0.0049 (7)−0.0006 (7)
N160.0209 (9)0.0186 (9)0.0260 (10)−0.0001 (7)0.0073 (8)0.0073 (8)
O150.0204 (8)0.0339 (9)0.0309 (9)−0.0030 (7)0.0053 (7)0.0184 (7)
O160.0201 (8)0.0429 (10)0.0404 (10)0.0052 (7)0.0085 (7)0.0253 (8)
Co20.01984 (13)0.01599 (15)0.01447 (13)−0.00063 (11)0.00670 (11)0.00120 (11)
C210.0254 (11)0.0186 (11)0.0151 (10)0.0022 (8)0.0066 (9)0.0006 (8)
C220.0488 (15)0.0228 (12)0.0281 (13)−0.0093 (11)0.0195 (11)−0.0088 (10)
C230.0536 (18)0.0495 (18)0.0370 (16)−0.0132 (14)0.0034 (13)−0.0070 (14)
N210.0263 (9)0.0189 (9)0.0176 (9)−0.0046 (7)0.0071 (7)−0.0005 (7)
N220.0319 (10)0.0252 (10)0.0181 (9)−0.0085 (8)0.0139 (8)−0.0024 (8)
O210.0248 (8)0.0195 (8)0.0176 (7)−0.0040 (6)0.0093 (6)−0.0019 (6)
O220.0416 (9)0.0231 (8)0.0204 (8)−0.0070 (7)0.0174 (7)−0.0054 (7)
C240.0231 (11)0.0212 (11)0.0205 (11)0.0018 (9)0.0130 (9)0.0036 (9)
C250.0248 (12)0.0350 (14)0.0286 (12)0.0097 (10)0.0074 (10)0.0053 (11)
C260.0399 (14)0.0395 (15)0.0305 (13)0.0094 (12)0.0144 (11)0.0105 (11)
N230.0239 (9)0.0209 (9)0.0166 (9)−0.0006 (7)0.0058 (7)0.0025 (7)
N240.0292 (10)0.0189 (9)0.0166 (9)0.0037 (7)0.0098 (7)−0.0022 (7)
O230.0249 (8)0.0224 (8)0.0175 (7)0.0039 (6)0.0057 (6)0.0002 (6)
O240.0347 (9)0.0323 (9)0.0258 (8)0.0136 (7)0.0139 (7)0.0023 (7)
C270.0262 (11)0.0255 (12)0.0263 (12)−0.0016 (9)0.0091 (9)0.0097 (10)
C28A0.037 (3)0.023 (3)0.046 (3)−0.002 (2)0.026 (3)0.006 (2)
C29A0.025 (2)0.046 (3)0.030 (2)0.0026 (19)0.0090 (17)0.0064 (19)
C28B0.048 (5)0.030 (5)0.074 (7)−0.009 (4)0.032 (5)0.005 (4)
C29B0.071 (7)0.057 (7)0.056 (6)0.029 (5)0.038 (5)0.027 (5)
N250.0202 (9)0.0184 (9)0.0237 (9)−0.0016 (7)0.0092 (7)0.0023 (7)
N260.0240 (9)0.0181 (9)0.0261 (10)−0.0004 (7)0.0087 (8)0.0091 (8)
O250.0229 (8)0.0273 (9)0.0316 (9)0.0030 (6)0.0131 (7)0.0133 (7)
O260.0350 (10)0.0508 (12)0.0836 (15)0.0073 (9)0.0318 (10)0.0436 (11)
Co30.01981 (14)0.01586 (15)0.01406 (13)−0.00134 (11)0.00592 (11)−0.00030 (11)
C310.0242 (11)0.0177 (11)0.0210 (11)0.0031 (8)0.0112 (9)0.0008 (9)
C320.0232 (11)0.0263 (13)0.0364 (13)0.0019 (9)0.0105 (10)0.0029 (11)
C330.0281 (12)0.0290 (13)0.0385 (14)0.0047 (10)0.0080 (11)0.0036 (11)
N310.0192 (9)0.0170 (9)0.0218 (9)−0.0017 (7)0.0083 (7)−0.0024 (7)
N320.0228 (9)0.0165 (9)0.0338 (11)0.0016 (7)0.0114 (8)0.0106 (8)
O310.0218 (7)0.0174 (8)0.0230 (8)−0.0014 (6)0.0069 (6)0.0045 (6)
O320.0230 (8)0.0228 (8)0.0405 (10)0.0044 (6)0.0102 (7)0.0129 (7)
C340.0184 (10)0.0177 (11)0.0179 (10)−0.0009 (8)0.0044 (8)0.0021 (8)
C350.0322 (12)0.0294 (13)0.0249 (12)−0.0066 (10)0.0143 (10)−0.0018 (10)
C360.067 (2)0.0451 (17)0.0442 (16)−0.0283 (15)0.0321 (15)−0.0064 (14)
N330.0190 (9)0.0198 (9)0.0175 (9)−0.0005 (7)0.0073 (7)0.0001 (7)
N340.0207 (9)0.0196 (9)0.0151 (8)−0.0043 (7)0.0060 (7)−0.0039 (7)
O330.0271 (8)0.0171 (8)0.0185 (7)−0.0030 (6)0.0106 (6)−0.0023 (6)
O340.0301 (8)0.0211 (8)0.0238 (8)−0.0081 (6)0.0134 (7)−0.0030 (6)
C370.0279 (11)0.0140 (10)0.0159 (10)−0.0005 (8)0.0098 (9)0.0019 (8)
C380.0444 (14)0.0210 (12)0.0224 (12)0.0116 (10)0.0076 (10)−0.0051 (9)
C390.066 (2)0.0546 (19)0.0579 (19)0.0287 (16)0.0427 (17)0.0135 (15)
N350.0253 (9)0.0170 (9)0.0158 (9)0.0012 (7)0.0075 (7)−0.0023 (7)
N360.0268 (9)0.0194 (9)0.0124 (8)0.0020 (7)0.0037 (7)−0.0020 (7)
O350.0242 (8)0.0211 (8)0.0165 (7)0.0015 (6)0.0058 (6)−0.0020 (6)
O360.0343 (8)0.0216 (8)0.0156 (7)0.0056 (7)0.0073 (6)−0.0033 (6)
Co40.01871 (13)0.01439 (14)0.01511 (13)−0.00110 (11)0.00620 (10)0.00028 (11)
C410.0229 (10)0.0155 (11)0.0195 (10)−0.0011 (8)0.0113 (9)0.0016 (8)
C420.0270 (12)0.0254 (12)0.0272 (12)0.0035 (9)0.0033 (10)0.0038 (10)
C430.0398 (14)0.0334 (14)0.0353 (14)−0.0003 (11)0.0144 (12)0.0069 (11)
N410.0251 (9)0.0184 (9)0.0151 (8)−0.0022 (7)0.0045 (7)0.0022 (7)
N420.0294 (10)0.0174 (9)0.0158 (9)0.0024 (7)0.0082 (7)−0.0015 (7)
O410.0227 (7)0.0165 (7)0.0161 (7)0.0007 (6)0.0046 (6)−0.0012 (6)
O420.0320 (9)0.0224 (8)0.0251 (8)0.0077 (7)0.0083 (7)0.0000 (7)
C440.0220 (10)0.0149 (10)0.0136 (9)−0.0015 (8)0.0056 (8)−0.0002 (8)
C450.0306 (12)0.0251 (12)0.0313 (12)0.0074 (10)0.0202 (10)0.0103 (10)
C460.0279 (12)0.0335 (14)0.0456 (15)−0.0024 (10)0.0172 (11)0.0005 (12)
N430.0164 (8)0.0188 (9)0.0229 (9)−0.0025 (7)0.0076 (7)0.0004 (7)
N440.0197 (9)0.0144 (9)0.0256 (9)0.0021 (7)0.0079 (7)0.0058 (7)
O430.0207 (7)0.0153 (7)0.0223 (7)0.0026 (6)0.0098 (6)0.0037 (6)
O440.0262 (8)0.0223 (8)0.0320 (9)0.0065 (6)0.0165 (7)0.0109 (7)
C470.0260 (11)0.0146 (10)0.0185 (10)0.0017 (8)0.0089 (9)0.0014 (8)
C480.0501 (15)0.0251 (13)0.0299 (13)−0.0159 (11)0.0235 (12)−0.0142 (10)
C490.0446 (16)0.0543 (18)0.0306 (14)−0.0140 (14)0.0093 (12)−0.0127 (13)
N450.0215 (9)0.0202 (9)0.0168 (9)−0.0043 (7)0.0051 (7)−0.0002 (7)
N460.0272 (10)0.0261 (10)0.0200 (9)−0.0076 (8)0.0135 (8)−0.0017 (8)
O450.0244 (8)0.0197 (8)0.0184 (7)−0.0039 (6)0.0102 (6)−0.0022 (6)
O460.0390 (9)0.0257 (9)0.0227 (8)−0.0103 (7)0.0175 (7)−0.0076 (7)
N1010.0186 (9)0.0213 (10)0.0221 (9)0.0010 (7)0.0036 (7)0.0032 (8)
O1010.0393 (9)0.0202 (8)0.0258 (8)−0.0026 (7)0.0127 (7)−0.0041 (7)
O1020.0286 (8)0.0193 (8)0.0440 (10)−0.0059 (7)0.0150 (8)−0.0070 (7)
O1030.0349 (9)0.0356 (10)0.0398 (10)−0.0036 (8)0.0228 (8)0.0024 (8)
N1110.0209 (9)0.0216 (10)0.0143 (8)0.0002 (7)0.0051 (7)−0.0002 (7)
O1110.0265 (8)0.0320 (9)0.0222 (8)0.0034 (7)0.0145 (7)0.0000 (7)
O1120.0393 (9)0.0294 (9)0.0262 (8)−0.0013 (7)0.0130 (7)−0.0135 (7)
O1130.0379 (10)0.0431 (11)0.0301 (9)−0.0222 (8)0.0164 (8)−0.0077 (8)
N1210.0283 (10)0.0165 (9)0.0255 (10)−0.0026 (7)0.0142 (8)−0.0016 (8)
O1210.0461 (10)0.0280 (9)0.0185 (8)0.0046 (7)0.0136 (7)0.0045 (7)
O1220.0283 (8)0.0366 (9)0.0201 (8)−0.0070 (7)0.0136 (7)0.0014 (7)
O1230.0242 (9)0.0488 (11)0.0411 (10)−0.0059 (8)0.0154 (8)−0.0184 (9)
N1310.0255 (9)0.0242 (10)0.0180 (9)0.0040 (8)0.0066 (8)0.0015 (8)
O1310.0254 (8)0.0154 (8)0.0249 (8)0.0017 (6)0.0091 (6)0.0040 (6)
O1320.0447 (10)0.0223 (9)0.0217 (8)0.0014 (7)0.0067 (7)−0.0039 (7)
O1330.0900 (17)0.0707 (15)0.0281 (11)0.0559 (13)−0.0240 (10)−0.0135 (10)
N1410.0210 (9)0.0200 (9)0.0140 (8)0.0010 (7)0.0045 (7)−0.0004 (7)
O1410.0264 (8)0.0287 (9)0.0214 (8)0.0017 (7)0.0135 (6)−0.0008 (7)
O1420.0413 (10)0.0381 (10)0.0332 (9)−0.0223 (8)0.0193 (8)−0.0081 (8)
O1430.0399 (9)0.0294 (9)0.0274 (9)0.0006 (7)0.0143 (7)−0.0142 (7)
N1510.0185 (8)0.0210 (10)0.0230 (9)−0.0002 (7)0.0039 (7)0.0024 (8)
O1510.0333 (9)0.0206 (8)0.0263 (8)0.0001 (7)0.0109 (7)−0.0049 (7)
O1520.0359 (9)0.0189 (8)0.0461 (10)−0.0046 (7)0.0226 (8)−0.0044 (7)
O1530.0350 (9)0.0375 (10)0.0450 (11)−0.0077 (8)0.0251 (8)−0.0014 (8)
N1610.0249 (9)0.0199 (9)0.0176 (9)0.0018 (7)0.0094 (7)0.0007 (7)
O1610.0263 (8)0.0163 (8)0.0206 (8)0.0040 (6)0.0062 (6)−0.0006 (6)
O1620.0542 (11)0.0238 (9)0.0220 (8)0.0071 (8)0.0130 (8)−0.0060 (7)
O1630.0557 (11)0.0338 (10)0.0195 (8)0.0171 (9)−0.0002 (8)0.0043 (7)
N1710.0213 (9)0.0169 (9)0.0180 (9)−0.0040 (7)0.0073 (7)−0.0002 (7)
O1710.0301 (8)0.0249 (8)0.0159 (7)0.0016 (6)0.0110 (6)0.0056 (6)
O1720.0189 (8)0.0310 (9)0.0282 (8)−0.0003 (7)0.0036 (6)−0.0057 (7)
O1730.0251 (8)0.0311 (9)0.0185 (7)−0.0063 (7)0.0114 (6)−0.0001 (7)
Geometric parameters (Å, °) top
Co1—O112.1005 (15)Co3—N332.1582 (16)
Co1—O152.1172 (15)C31—O311.237 (2)
Co1—O132.1179 (14)C31—O321.329 (2)
Co1—N132.1236 (17)C31—N321.334 (3)
Co1—N152.1460 (17)C32—O321.465 (3)
Co1—N112.1649 (17)C32—C331.492 (3)
C11—O111.236 (3)C32—H32A0.9900
C11—O121.338 (3)C32—H32B0.9900
C11—N121.345 (3)C33—H33A0.9800
C12—O121.461 (3)C33—H33B0.9800
C12—C131.471 (4)C33—H33C0.9800
C12—H12A0.9900N31—N321.411 (2)
C12—H12B0.9900N31—H31A0.9200
C13—H13A0.9800N31—H31B0.9200
C13—H13B0.9800N32—H320.8800
C13—H13C0.9800C34—O331.236 (2)
N11—N121.421 (2)C34—O341.329 (2)
N11—H11A0.9200C34—N341.348 (2)
N11—H11B0.9200C35—O341.458 (2)
N12—H120.8800C35—C361.503 (3)
C14—O131.249 (2)C35—H35A0.9900
C14—N141.324 (3)C35—H35B0.9900
C14—O141.332 (2)C36—H36A0.9800
C15—O141.451 (3)C36—H36B0.9800
C15—C161.505 (3)C36—H36C0.9800
C15—H15A0.9900N33—N341.421 (2)
C15—H15B0.9900N33—H33D0.9200
C16—H16A0.9800N33—H33E0.9200
C16—H16B0.9800N34—H340.8800
C16—H16C0.9800C37—O351.240 (2)
N13—N141.413 (2)C37—N361.329 (3)
N13—H13D0.9200C37—O361.338 (2)
N13—H13E0.9200C38—O361.457 (2)
N14—H140.8800C38—C391.498 (4)
C17—O151.238 (3)C38—H38A0.9900
C17—N161.326 (3)C38—H38B0.9900
C17—O161.331 (2)C39—H39A0.9800
C18A—O161.441 (3)C39—H39B0.9800
C18A—C19A1.497 (7)C39—H39C0.9800
C18A—H18A0.9900N35—N361.417 (2)
C18A—H18B0.9900N35—H35C0.9200
C19A—H19A0.9800N35—H35D0.9200
C19A—H19B0.9800N36—H360.8800
C19A—H19C0.9800Co4—O412.1063 (14)
C18B—C19B1.488 (17)Co4—O432.1064 (14)
C18B—O161.619 (9)Co4—O452.1297 (14)
C18B—H18C0.9900Co4—N452.1338 (16)
C18B—H18D0.9900Co4—N432.1450 (17)
C19B—H19D0.9800Co4—N412.1671 (17)
C19B—H19E0.9800C41—O411.237 (2)
C19B—H19F0.9800C41—N421.334 (3)
N15—N161.416 (2)C41—O421.334 (2)
N15—H15C0.9200C42—O421.457 (3)
N15—H15D0.9200C42—C431.501 (3)
N16—H160.8800C42—H42A0.9900
Co2—O252.0853 (14)C42—H42B0.9900
Co2—O232.1090 (14)C43—H43A0.9800
Co2—N212.1240 (17)C43—H43B0.9800
Co2—O212.1270 (14)C43—H43C0.9800
Co2—N252.1534 (17)N41—N421.420 (2)
Co2—N232.1678 (17)N41—H41A0.9200
C21—O211.239 (2)N41—H41B0.9200
C21—O221.331 (2)N42—H420.8800
C21—N221.335 (3)C44—O431.243 (2)
C22—O221.455 (3)C44—O441.328 (2)
C22—C231.504 (4)C44—N441.328 (3)
C22—H22A0.9900C45—O441.460 (2)
C22—H22B0.9900C45—C461.500 (3)
C23—H23A0.9800C45—H45A0.9900
C23—H23B0.9800C45—H45B0.9900
C23—H23C0.9800C46—H46A0.9800
N21—N221.413 (2)C46—H46B0.9800
N21—H21A0.9200C46—H46C0.9800
N21—H21B0.9200N43—N441.415 (2)
N22—H220.8800N43—H43D0.9200
C24—O231.235 (2)N43—H43E0.9200
C24—N241.332 (3)N44—H440.8800
C24—O241.338 (2)C47—O451.237 (2)
C25—O241.461 (3)C47—O461.332 (2)
C25—C261.499 (3)C47—N461.340 (3)
C25—H25A0.9900C48—O461.456 (3)
C25—H25B0.9900C48—C491.504 (4)
C26—H26A0.9800C48—H48A0.9900
C26—H26B0.9800C48—H48B0.9900
C26—H26C0.9800C49—H49A0.9800
N23—N241.421 (2)C49—H49B0.9800
N23—H23D0.9200C49—H49C0.9800
N23—H23E0.9200N45—N461.417 (2)
N24—H240.8800N45—H45C0.9200
C27—O251.246 (3)N45—H45D0.9200
C27—N261.320 (3)N46—H460.8800
C27—O261.324 (3)N101—O1031.241 (2)
C28A—C29A1.502 (7)N101—O1021.261 (2)
C28A—O261.524 (6)N101—O1011.267 (2)
C28A—H28A0.9900N111—O1131.248 (2)
C28A—H28B0.9900N111—O1121.252 (2)
C29A—H29A0.9800N111—O1111.258 (2)
C29A—H29B0.9800N121—O1221.249 (2)
C29A—H29C0.9800N121—O1231.250 (2)
C28B—C29B1.440 (14)N121—O1211.260 (2)
C28B—O261.476 (8)N131—O1331.216 (2)
C28B—H28C0.9900N131—O1321.247 (2)
C28B—H28D0.9900N131—O1311.273 (2)
C29B—H29D0.9800N141—O1431.245 (2)
C29B—H29E0.9800N141—O1421.251 (2)
C29B—H29F0.9800N141—O1411.261 (2)
N25—N261.418 (2)N151—O1531.242 (2)
N25—H25C0.9200N151—O1521.261 (2)
N25—H25D0.9200N151—O1511.261 (2)
N26—H260.8800N161—O1631.238 (2)
Co3—O332.0896 (14)N161—O1621.248 (2)
Co3—O352.1062 (14)N161—O1611.277 (2)
Co3—O312.1112 (14)N171—O1731.251 (2)
Co3—N352.1285 (17)N171—O1721.252 (2)
Co3—N312.1515 (16)N171—O1711.263 (2)
O11—Co1—O1588.32 (6)O35—Co3—N3189.28 (6)
O11—Co1—O1395.73 (6)O31—Co3—N3178.37 (6)
O15—Co1—O1394.30 (6)N35—Co3—N3196.84 (7)
O11—Co1—N1398.24 (6)O33—Co3—N3378.13 (6)
O15—Co1—N13170.86 (7)O35—Co3—N33171.95 (6)
O13—Co1—N1378.78 (6)O31—Co3—N3390.41 (6)
O11—Co1—N15164.39 (6)N35—Co3—N3397.01 (6)
O15—Co1—N1577.65 (6)N31—Co3—N3398.17 (6)
O13—Co1—N1592.16 (6)O31—C31—O32123.81 (19)
N13—Co1—N1596.49 (7)O31—C31—N32123.95 (19)
O11—Co1—N1177.60 (6)O32—C31—N32112.24 (18)
O15—Co1—N1193.69 (7)O32—C32—C33106.73 (18)
O13—Co1—N11169.43 (6)O32—C32—H32A110.4
N13—Co1—N1193.93 (6)C33—C32—H32A110.4
N15—Co1—N1196.30 (6)O32—C32—H32B110.4
O11—C11—O12124.4 (2)C33—C32—H32B110.4
O11—C11—N12123.98 (19)H32A—C32—H32B108.6
O12—C11—N12111.50 (19)C32—C33—H33A109.5
O12—C12—C13109.4 (2)C32—C33—H33B109.5
O12—C12—H12A109.8H33A—C33—H33B109.5
C13—C12—H12A109.8C32—C33—H33C109.5
O12—C12—H12B109.8H33A—C33—H33C109.5
C13—C12—H12B109.8H33B—C33—H33C109.5
H12A—C12—H12B108.2N32—N31—Co3107.42 (11)
C12—C13—H13A109.5N32—N31—H31A110.2
C12—C13—H13B109.5Co3—N31—H31A110.2
H13A—C13—H13B109.5N32—N31—H31B110.2
C12—C13—H13C109.5Co3—N31—H31B110.2
H13A—C13—H13C109.5H31A—N31—H31B108.5
H13B—C13—H13C109.5C31—N32—N31117.87 (17)
N12—N11—Co1106.45 (11)C31—N32—H32121.1
N12—N11—H11A110.4N31—N32—H32121.1
Co1—N11—H11A110.4C31—O31—Co3112.10 (13)
N12—N11—H11B110.4C31—O32—C32116.51 (17)
Co1—N11—H11B110.4O33—C34—O34123.49 (18)
H11A—N11—H11B108.6O33—C34—N34124.04 (18)
C11—N12—N11115.54 (17)O34—C34—N34112.44 (17)
C11—N12—H12122.2O34—C35—C36107.14 (18)
N11—N12—H12122.2O34—C35—H35A110.3
C11—O11—Co1112.30 (13)C36—C35—H35A110.3
C11—O12—C12116.64 (19)O34—C35—H35B110.3
O13—C14—N14124.03 (19)C36—C35—H35B110.3
O13—C14—O14124.05 (19)H35A—C35—H35B108.5
N14—C14—O14111.92 (18)C35—C36—H36A109.5
O14—C15—C16111.8 (2)C35—C36—H36B109.5
O14—C15—H15A109.2H36A—C36—H36B109.5
C16—C15—H15A109.2C35—C36—H36C109.5
O14—C15—H15B109.2H36A—C36—H36C109.5
C16—C15—H15B109.2H36B—C36—H36C109.5
H15A—C15—H15B107.9N34—N33—Co3106.00 (11)
C15—C16—H16A109.5N34—N33—H33D110.5
C15—C16—H16B109.5Co3—N33—H33D110.5
H16A—C16—H16B109.5N34—N33—H33E110.5
C15—C16—H16C109.5Co3—N33—H33E110.5
H16A—C16—H16C109.5H33D—N33—H33E108.7
H16B—C16—H16C109.5C34—N34—N33115.09 (16)
N14—N13—Co1107.63 (12)C34—N34—H34122.5
N14—N13—H13D110.2N33—N34—H34122.5
Co1—N13—H13D110.2C34—O33—Co3112.04 (13)
N14—N13—H13E110.2C34—O34—C35114.64 (16)
Co1—N13—H13E110.2O35—C37—N36124.28 (18)
H13D—N13—H13E108.5O35—C37—O36124.02 (18)
C14—N14—N13117.82 (17)N36—C37—O36111.71 (17)
C14—N14—H14121.1O36—C38—C39111.58 (19)
N13—N14—H14121.1O36—C38—H38A109.3
C14—O13—Co1110.88 (13)C39—C38—H38A109.3
C14—O14—C15117.57 (17)O36—C38—H38B109.3
O15—C17—N16123.5 (2)C39—C38—H38B109.3
O15—C17—O16124.41 (19)H38A—C38—H38B108.0
N16—C17—O16112.09 (19)C38—C39—H39A109.5
O16—C18A—C19A106.6 (4)C38—C39—H39B109.5
O16—C18A—H18A110.4H39A—C39—H39B109.5
C19A—C18A—H18A110.4C38—C39—H39C109.5
O16—C18A—H18B110.4H39A—C39—H39C109.5
C19A—C18A—H18B110.4H39B—C39—H39C109.5
H18A—C18A—H18B108.6N36—N35—Co3107.03 (12)
C19B—C18B—O16102.1 (9)N36—N35—H35C110.3
C19B—C18B—H18C111.3Co3—N35—H35C110.3
O16—C18B—H18C111.3N36—N35—H35D110.3
C19B—C18B—H18D111.3Co3—N35—H35D110.3
O16—C18B—H18D111.3H35C—N35—H35D108.6
H18C—C18B—H18D109.2C37—N36—N35117.52 (16)
C18B—C19B—H19D109.5C37—N36—H36121.2
C18B—C19B—H19E109.5N35—N36—H36121.2
H19D—C19B—H19E109.5C37—O35—Co3111.03 (13)
C18B—C19B—H19F109.5C37—O36—C38116.65 (16)
H19D—C19B—H19F109.5O41—Co4—O4395.82 (5)
H19E—C19B—H19F109.5O41—Co4—O4590.00 (5)
N16—N15—Co1108.32 (11)O43—Co4—O45101.36 (5)
N16—N15—H15C110.0O41—Co4—N4592.21 (6)
Co1—N15—H15C110.0O43—Co4—N45171.97 (6)
N16—N15—H15D110.0O45—Co4—N4578.47 (6)
Co1—N15—H15D110.0O41—Co4—N43172.67 (6)
H15C—N15—H15D108.4O43—Co4—N4377.72 (6)
C17—N16—N15117.57 (17)O45—Co4—N4387.92 (6)
C17—N16—H16121.2N45—Co4—N4394.26 (6)
N15—N16—H16121.2O41—Co4—N4178.01 (6)
C17—O15—Co1112.92 (13)O43—Co4—N4188.05 (6)
C17—O16—C18A118.95 (19)O45—Co4—N41165.52 (6)
C17—O16—C18B111.1 (3)N45—Co4—N4193.75 (6)
C18A—O16—C18B32.9 (3)N43—Co4—N41104.96 (6)
O25—Co2—O2393.27 (6)O41—C41—N42123.83 (19)
O25—Co2—N21173.50 (7)O41—C41—O42124.59 (19)
O23—Co2—N2192.03 (6)N42—C41—O42111.56 (17)
O25—Co2—O2197.26 (6)O42—C42—C43108.87 (19)
O23—Co2—O2191.76 (6)O42—C42—H42A109.9
N21—Co2—O2178.81 (6)C43—C42—H42A109.9
O25—Co2—N2578.02 (6)O42—C42—H42B109.9
O23—Co2—N25171.23 (6)C43—C42—H42B109.9
N21—Co2—N2596.59 (7)H42A—C42—H42B108.3
O21—Co2—N2588.33 (6)C42—C43—H43A109.5
O25—Co2—N2390.66 (6)C42—C43—H43B109.5
O23—Co2—N2378.05 (6)H43A—C43—H43B109.5
N21—Co2—N2394.11 (7)C42—C43—H43C109.5
O21—Co2—N23167.46 (6)H43A—C43—H43C109.5
N25—Co2—N23102.87 (7)H43B—C43—H43C109.5
O21—C21—O22124.25 (19)N42—N41—Co4107.05 (11)
O21—C21—N22124.23 (19)N42—N41—H41A110.3
O22—C21—N22111.52 (18)Co4—N41—H41A110.3
O22—C22—C23111.2 (2)N42—N41—H41B110.3
O22—C22—H22A109.4Co4—N41—H41B110.3
C23—C22—H22A109.4H41A—N41—H41B108.6
O22—C22—H22B109.4C41—N42—N41117.56 (16)
C23—C22—H22B109.4C41—N42—H42121.2
H22A—C22—H22B108.0N41—N42—H42121.2
C22—C23—H23A109.5C41—O41—Co4112.77 (13)
C22—C23—H23B109.5C41—O42—C42118.33 (17)
H23A—C23—H23B109.5O43—C44—O44124.08 (18)
C22—C23—H23C109.5O43—C44—N44123.88 (18)
H23A—C23—H23C109.5O44—C44—N44112.04 (17)
H23B—C23—H23C109.5O44—C45—C46111.80 (18)
N22—N21—Co2108.10 (12)O44—C45—H45A109.3
N22—N21—H21A110.1C46—C45—H45A109.3
Co2—N21—H21A110.1O44—C45—H45B109.3
N22—N21—H21B110.1C46—C45—H45B109.3
Co2—N21—H21B110.1H45A—C45—H45B107.9
H21A—N21—H21B108.4C45—C46—H46A109.5
C21—N22—N21117.67 (16)C45—C46—H46B109.5
C21—N22—H22121.2H46A—C46—H46B109.5
N21—N22—H22121.2C45—C46—H46C109.5
C21—O21—Co2111.03 (13)H46A—C46—H46C109.5
C21—O22—C22117.05 (16)H46B—C46—H46C109.5
O23—C24—N24124.32 (19)N44—N43—Co4108.77 (11)
O23—C24—O24123.81 (19)N44—N43—H43D109.9
N24—C24—O24111.84 (18)Co4—N43—H43D109.9
O24—C25—C26109.86 (19)N44—N43—H43E109.9
O24—C25—H25A109.7Co4—N43—H43E109.9
C26—C25—H25A109.7H43D—N43—H43E108.3
O24—C25—H25B109.7C44—N44—N43116.73 (16)
C26—C25—H25B109.7C44—N44—H44121.6
H25A—C25—H25B108.2N43—N44—H44121.6
C25—C26—H26A109.5C44—O43—Co4112.87 (12)
C25—C26—H26B109.5C44—O44—C45116.64 (16)
H26A—C26—H26B109.5O45—C47—O46124.43 (19)
C25—C26—H26C109.5O45—C47—N46124.01 (19)
H26A—C26—H26C109.5O46—C47—N46111.57 (18)
H26B—C26—H26C109.5O46—C48—C49111.5 (2)
N24—N23—Co2107.04 (11)O46—C48—H48A109.3
N24—N23—H23D110.3C49—C48—H48A109.3
Co2—N23—H23D110.3O46—C48—H48B109.3
N24—N23—H23E110.3C49—C48—H48B109.3
Co2—N23—H23E110.3H48A—C48—H48B108.0
H23D—N23—H23E108.6C48—C49—H49A109.5
C24—N24—N23117.26 (16)C48—C49—H49B109.5
C24—N24—H24121.4H49A—C49—H49B109.5
N23—N24—H24121.4C48—C49—H49C109.5
C24—O23—Co2112.50 (13)H49A—C49—H49C109.5
C24—O24—C25117.56 (17)H49B—C49—H49C109.5
O25—C27—N26124.0 (2)N46—N45—Co4108.25 (11)
O25—C27—O26123.7 (2)N46—N45—H45C110.0
N26—C27—O26112.28 (19)Co4—N45—H45C110.0
C29A—C28A—O26105.3 (4)N46—N45—H45D110.0
C29A—C28A—H28A110.7Co4—N45—H45D110.0
O26—C28A—H28A110.7H45C—N45—H45D108.4
C29A—C28A—H28B110.7C47—N46—N45117.52 (16)
O26—C28A—H28B110.7C47—N46—H46121.2
H28A—C28A—H28B108.8N45—N46—H46121.2
C29B—C28B—O2696.2 (7)C47—O45—Co4111.73 (13)
C29B—C28B—H28C112.5C47—O46—C48116.51 (16)
O26—C28B—H28C112.5O103—N101—O102120.49 (18)
C29B—C28B—H28D112.5O103—N101—O101120.18 (18)
O26—C28B—H28D112.5O102—N101—O101119.32 (17)
H28C—C28B—H28D110.0O113—N111—O112120.81 (17)
N26—N25—Co2107.93 (12)O113—N111—O111119.44 (17)
N26—N25—H25C110.1O112—N111—O111119.74 (17)
Co2—N25—H25C110.1O122—N121—O123120.79 (18)
N26—N25—H25D110.1O122—N121—O121120.60 (18)
Co2—N25—H25D110.1O123—N121—O121118.61 (18)
H25C—N25—H25D108.4O133—N131—O132121.02 (19)
C27—N26—N25116.92 (17)O133—N131—O131119.27 (18)
C27—N26—H26121.5O132—N131—O131119.70 (17)
N25—N26—H26121.5O143—N141—O142120.88 (17)
C27—O25—Co2113.10 (13)O143—N141—O141119.85 (17)
C27—O26—C28B117.6 (4)O142—N141—O141119.26 (17)
C27—O26—C28A114.9 (3)O153—N151—O152120.41 (18)
C28B—O26—C28A34.7 (4)O153—N151—O151120.42 (18)
O33—Co3—O3595.25 (5)O152—N151—O151119.17 (17)
O33—Co3—O3189.16 (5)O163—N161—O162121.33 (18)
O35—Co3—O3194.10 (5)O163—N161—O161119.76 (17)
O33—Co3—N3595.97 (6)O162—N161—O161118.91 (17)
O35—Co3—N3578.98 (6)O173—N171—O172120.72 (17)
O31—Co3—N35171.71 (6)O173—N171—O171120.05 (16)
O33—Co3—N31167.01 (6)O172—N171—O171119.23 (16)
O11—Co1—N11—N12−16.86 (11)O25—C27—O26—C28A−19.3 (4)
O15—Co1—N11—N1270.60 (12)N26—C27—O26—C28A160.2 (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—C28A3.3 (6)
N15—Co1—N11—N12148.57 (12)C29A—C28A—O26—C27133.8 (3)
O11—C11—N12—N11−13.1 (3)C29A—C28A—O26—C28B30.7 (6)
O12—C11—N12—N11170.23 (16)O33—Co3—N31—N32−20.7 (3)
Co1—N11—N12—C1121.0 (2)O35—Co3—N31—N3289.93 (12)
O12—C11—O11—Co1172.74 (16)O31—Co3—N31—N32−4.40 (12)
N12—C11—O11—Co1−3.6 (3)N35—Co3—N31—N32168.74 (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—C11104.05 (15)O32—C31—N32—N31179.09 (17)
N15—Co1—O11—C11−56.5 (3)Co3—N31—N32—C314.4 (2)
N11—Co1—O11—C1111.81 (14)O32—C31—O31—Co3176.67 (16)
O11—C11—O12—C124.3 (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—C1186.4 (3)O35—Co3—O31—C31−84.10 (14)
O11—Co1—N13—N14102.08 (13)N31—Co3—O31—C314.32 (14)
O13—Co1—N13—N147.83 (12)N33—Co3—O31—C31102.58 (14)
N15—Co1—N13—N14−83.09 (13)O31—C31—O32—C324.2 (3)
N11—Co1—N13—N14−179.90 (13)N32—C31—O32—C32−175.75 (18)
O13—C14—N14—N132.4 (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—N3471.73 (12)
N14—C14—O13—Co15.1 (3)N35—Co3—N33—N34−111.98 (12)
O14—C14—O13—Co1−175.76 (16)N31—Co3—N33—N34150.03 (11)
O11—Co1—O13—C14−104.45 (14)O33—C34—N34—N33−17.1 (3)
O15—Co1—O13—C14166.81 (14)O34—C34—N34—N33164.95 (16)
N13—Co1—O13—C14−7.15 (14)Co3—N33—N34—C3423.07 (19)
N15—Co1—O13—C1489.04 (14)O34—C34—O33—Co3177.68 (15)
N11—Co1—O13—C14−54.2 (4)N34—C34—O33—Co30.0 (2)
O13—C14—O14—C154.9 (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—C34106.29 (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—C3410.36 (13)
O13—Co1—N15—N1691.97 (12)O33—C34—O34—C353.4 (3)
N13—Co1—N15—N16170.92 (12)N34—C34—O34—C35−178.67 (17)
N11—Co1—N15—N16−94.38 (13)C36—C35—O34—C34174.7 (2)
O15—C17—N16—N15−1.3 (3)O33—Co3—N35—N36103.27 (12)
O16—C17—N16—N15177.74 (17)O35—Co3—N35—N369.06 (12)
Co1—N15—N16—C172.4 (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—N352.9 (3)
O11—Co1—O15—C17174.60 (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—C171.49 (15)N36—C37—O35—Co35.8 (2)
N11—Co1—O15—C1797.14 (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—C18A163.1 (3)O31—Co3—O35—C37167.13 (13)
O15—C17—O16—C18B17.6 (6)N35—Co3—O35—C37−8.27 (13)
N16—C17—O16—C18B−161.5 (5)N31—Co3—O35—C3788.85 (14)
C19A—C18A—O16—C17140.5 (4)O35—C37—O36—C388.9 (3)
C19A—C18A—O16—C18B56.0 (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—N427.45 (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—N4242.1 (3)
N25—Co2—N21—N2284.79 (13)N45—Co4—N41—N4298.91 (12)
N23—Co2—N21—N22−171.73 (13)N43—Co4—N41—N42−165.67 (11)
O21—C21—N22—N212.6 (3)O41—C41—N42—N413.9 (3)
O22—C21—N22—N21−177.79 (17)O42—C41—N42—N41−177.95 (16)
Co2—N21—N22—C210.8 (2)Co4—N41—N42—C41−8.5 (2)
O22—C21—O21—Co2175.97 (16)N42—C41—O41—Co43.5 (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—C4180.55 (14)
O23—Co2—O21—C2195.22 (14)O45—Co4—O41—C41−178.03 (13)
N21—Co2—O21—C213.50 (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—C2160.0 (3)O41—C41—O42—C42−9.6 (3)
O21—C21—O22—C22−5.7 (3)N42—C41—O42—C42172.28 (17)
N22—C21—O22—C22174.70 (18)C43—C42—O42—C41−106.3 (2)
C23—C22—O22—C2189.1 (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—N247.55 (11)N45—Co4—N43—N44179.03 (12)
N21—Co2—N23—N2498.75 (12)N41—Co4—N43—N4483.99 (13)
O21—Co2—N23—N2443.7 (3)O43—C44—N44—N431.4 (3)
N25—Co2—N23—N24−163.52 (12)O44—C44—N44—N43−178.36 (16)
O23—C24—N24—N236.2 (3)Co4—N43—N44—C44−0.1 (2)
O24—C24—N24—N23−175.75 (16)O44—C44—O43—Co4177.82 (15)
Co2—N23—N24—C24−9.6 (2)N44—C44—O43—Co4−2.0 (2)
N24—C24—O23—Co21.4 (3)O41—Co4—O43—C44177.81 (13)
O24—C24—O23—Co2−176.45 (15)O45—Co4—O43—C4486.64 (13)
O25—Co2—O23—C2484.79 (14)N43—Co4—O43—C441.32 (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—C45172.22 (17)
O23—C24—O24—C25−6.5 (3)C46—C45—O44—C4479.3 (2)
N24—C24—O24—C25175.49 (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—N4685.79 (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—N2686.45 (13)O46—C47—N46—N45178.43 (17)
O25—C27—N26—N25−2.8 (3)Co4—N45—N46—C471.9 (2)
O26—C27—N26—N25177.69 (19)O46—C47—O45—Co4−179.68 (16)
Co2—N25—N26—C272.6 (2)N46—C47—O45—Co40.5 (3)
N26—C27—O25—Co21.3 (3)O41—Co4—O45—C4792.72 (14)
O26—C27—O25—Co2−179.3 (2)O43—Co4—O45—C47−171.34 (14)
O23—Co2—O25—C27179.18 (16)N45—Co4—O45—C470.47 (14)
O21—Co2—O25—C2786.99 (16)N43—Co4—O45—C47−94.30 (14)
N25—Co2—O25—C270.26 (16)N41—Co4—O45—C4758.9 (3)
N23—Co2—O25—C27−102.76 (16)O45—C47—O46—C48−5.5 (3)
O25—C27—O26—C28B19.5 (6)N46—C47—O46—C48174.34 (18)
N26—C27—O26—C28B−161.0 (5)C49—C48—O46—C4784.0 (2)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N11—H11A···O1520.922.403.166 (2)140
N11—H11A···O1630.922.603.111 (2)116
N11—H11A···O1710.922.643.188 (2)119
N11—H11B···O1420.922.193.028 (2)151
N12—H12···O1720.882.192.931 (2)141
N13—H13D···O1510.922.102.947 (2)153
N13—H13D···O1520.922.403.155 (2)139
N13—H13E···O1620.922.123.016 (2)166
N13—H13E···O1630.922.643.395 (3)140
N14—H14···O131i0.882.092.939 (2)161
N14—H14···O132i0.882.333.053 (2)140
N15—H15C···O1430.922.142.968 (2)149
N15—H15C···O1510.922.452.984 (2)117
N15—H15D···O161ii0.922.062.982 (2)176
N15—H15D···O163ii0.922.663.307 (2)128
N16—H16···O171ii0.882.092.889 (2)151
N21—H21A···O101iii0.922.283.013 (2)137
N21—H21A···O103iii0.922.433.336 (2)167
N21—H21B···O1210.922.102.939 (2)151
N21—H21B···O112iii0.922.442.979 (2)117
N22—H22···O1310.882.052.907 (2)164
N23—H23D···O113iv0.922.263.166 (2)169
N23—H23D···O111iv0.922.393.121 (2)136
N23—H23E···O111iii0.922.343.141 (2)146
N23—H23E···O112iii0.922.643.496 (2)156
N24—H24···O122iv0.882.162.852 (2)135
N25—H25C···O1020.922.123.038 (2)176
N25—H25C···O1030.922.573.243 (2)130
N25—H25D···O1220.922.022.924 (2)169
N26—H26···O1110.882.253.043 (2)150
N31—H31A···O1120.922.122.970 (2)153
N31—H31A···O1010.922.633.152 (2)116
N31—H31B···O131ii0.922.163.073 (2)175
N31—H31B···O133ii0.922.613.303 (3)133
N32—H32···O121ii0.882.262.992 (2)141
N32—H32···O123ii0.882.423.234 (3)154
N33—H33D···O1020.922.313.083 (2)142
N33—H33E···O1130.922.253.071 (2)149
N34—H34···O1230.882.212.929 (2)139
N35—H35C···O1010.922.062.922 (2)155
N35—H35C···O1020.922.503.233 (2)136
N35—H35D···O1320.922.113.025 (2)171
N36—H36···O161i0.882.042.896 (2)164
N36—H36···O162i0.882.463.144 (2)135
N41—H41A···O141v0.922.303.066 (2)140
N41—H41A···O142v0.922.363.255 (2)165
N41—H41B···O141iii0.922.323.088 (2)141
N41—H41B···O143iii0.922.603.460 (2)156
N42—H42···O173v0.882.092.818 (2)139
N43—H43D···O1520.922.113.018 (2)169
N43—H43D···O1530.922.493.187 (2)133
N43—H43E···O1730.921.982.898 (2)175
N44—H44···O1410.882.223.041 (2)155
N45—H45C···O151iii0.922.303.028 (2)136
N45—H45C···O153iii0.922.453.358 (2)169
N45—H45D···O1710.922.133.012 (2)159
N46—H46···O1610.882.132.991 (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.
Table 1
Selected geometric parameters (Å) top
Co1—O112.1005 (15)Co3—O332.0896 (14)
Co1—O152.1172 (15)Co3—O352.1062 (14)
Co1—O132.1179 (14)Co3—O312.1112 (14)
Co1—N132.1236 (17)Co3—N352.1285 (17)
Co1—N152.1460 (17)Co3—N312.1515 (16)
Co1—N112.1649 (17)Co3—N332.1582 (16)
Co2—O252.0853 (14)Co4—O412.1063 (14)
Co2—O232.1090 (14)Co4—O432.1064 (14)
Co2—N212.1240 (17)Co4—O452.1297 (14)
Co2—O212.1270 (14)Co4—N452.1338 (16)
Co2—N252.1534 (17)Co4—N432.1450 (17)
Co2—N232.1678 (17)Co4—N412.1671 (17)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N11—H11A···O1520.922.403.166 (2)140
N11—H11A···O1630.922.603.111 (2)116
N11—H11A···O1710.922.643.188 (2)119
N11—H11B···O1420.922.193.028 (2)151
N12—H12···O1720.882.192.931 (2)141
N13—H13D···O1510.922.102.947 (2)153
N13—H13D···O1520.922.403.155 (2)139
N13—H13E···O1620.922.123.016 (2)166
N13—H13E···O1630.922.643.395 (3)140
N14—H14···O131i0.882.092.939 (2)161
N14—H14···O132i0.882.333.053 (2)140
N15—H15C···O1430.922.142.968 (2)149
N15—H15C···O1510.922.452.984 (2)117
N15—H15D···O161ii0.922.062.982 (2)176
N15—H15D···O163ii0.922.663.307 (2)128
N16—H16···O171ii0.882.092.889 (2)151
N21—H21A···O101iii0.922.283.013 (2)137
N21—H21A···O103iii0.922.433.336 (2)167
N21—H21B···O1210.922.102.939 (2)151
N21—H21B···O112iii0.922.442.979 (2)117
N22—H22···O1310.882.052.907 (2)164
N23—H23D···O113iv0.922.263.166 (2)169
N23—H23D···O111iv0.922.393.121 (2)136
N23—H23E···O111iii0.922.343.141 (2)146
N23—H23E···O112iii0.922.643.496 (2)156
N24—H24···O122iv0.882.162.852 (2)135
N25—H25C···O1020.922.123.038 (2)176
N25—H25C···O1030.922.573.243 (2)130
N25—H25D···O1220.922.022.924 (2)169
N26—H26···O1110.882.253.043 (2)150
N31—H31A···O1120.922.122.970 (2)153
N31—H31A···O1010.922.633.152 (2)116
N31—H31B···O131ii0.922.163.073 (2)175
N31—H31B···O133ii0.922.613.303 (3)133
N32—H32···O121ii0.882.262.992 (2)141
N32—H32···O123ii0.882.423.234 (3)154
N33—H33D···O1020.922.313.083 (2)142
N33—H33E···O1130.922.253.071 (2)149
N34—H34···O1230.882.212.929 (2)139
N35—H35C···O1010.922.062.922 (2)155
N35—H35C···O1020.922.503.233 (2)136
N35—H35D···O1320.922.113.025 (2)171
N36—H36···O161i0.882.042.896 (2)164
N36—H36···O162i0.882.463.144 (2)135
N41—H41A···O141v0.922.303.066 (2)140
N41—H41A···O142v0.922.363.255 (2)165
N41—H41B···O141iii0.922.323.088 (2)141
N41—H41B···O143iii0.922.603.460 (2)156
N42—H42···O173v0.882.092.818 (2)139
N43—H43D···O1520.922.113.018 (2)169
N43—H43D···O1530.922.493.187 (2)133
N43—H43E···O1730.921.982.898 (2)175
N44—H44···O1410.882.223.041 (2)155
N45—H45C···O151iii0.922.303.028 (2)136
N45—H45C···O153iii0.922.453.358 (2)169
N45—H45D···O1710.922.133.012 (2)159
N46—H46···O1610.882.132.991 (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.
references
References top

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Bruker (2003). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565–?.

Indira, A., Babu, A. M., Bellad, S. B., Sridhar, M. A., Shashidhara Prasad, J. & Prout, C. K. (1993). Curr. Sci. 64, 247–252.

Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.

Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Zhang, T.-L., Song, J.-C., Zhang, J.-G., Ma, G.-X. & Yu, K.-B. (2005). Z. Naturforsch. Teil B, 60, 505–510.