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The title compound, [Co(C29H29N5)2](NO3)2, contains a six-coordinate high-spin CoII ion with approximate local D2d symmetry. The bond lengths and angles at cobalt undergo only small changes between the two temperatures, which confirms that the CoII ion does not undergo a spin-state transition over this temperature range.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102023296/bm1518sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102023296/bm1518Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102023296/bm1518IIsup3.hkl
Contains datablock II

CCDC references: 205297; 205298

Comment top

We have recently reported a synthetic and structural study of a series of complexes [Co(LR)2]2+ [R is H, iPr, Ph or mesityl (Mes); Holland et al., 2001]. As part of this study, we described the crystal structure of [Co(LMes)2](ClO4)2·2CH3NO2, which we obtained at 150 K to prevent desolvation of the crystals. Unfortunately, it was not possible to interpret this structure meaningfully because, although the complex is in a high-spin form at 290 K, in the absence of variable-temperature magnetic data, it was unclear whether the Co ion had undergone a spin-state transition upon cooling (see e.g. Figgis et al., 1983; Gaspar et al., 2001). We now report structure determinations of the title unsolvated salt [Co(LMes)2](NO3)2, (I), at 290 K and 150 K, which are intended to address this ambiguity. \sch

Compound (I) crystallizes in the orthorhombic space group Pca21, with one complex dication and two anions per asymmetric unit, all lying on general positions. The CoII ion has a distorted octahedral stereochemistry with approximate D2 d local symmetry, which resembles those of other [M(LR)2]2+ (M is Fe, Co, Ni, Cu or Zn) complexes that we have characterized crystallographically (Solanki et al., 1998, 2001; Halcrow et al., 2000; Holland et al., 2001, 2002). As in these other compounds, the coordination sphere at Co in (I) is substantially distorted from an ideal octahedron by the restricted bite angle of the LMes ligand; the average of the four angles N2—Co1—N9, N2—Co1—N23, N36—Co1—N43 and N2—Co1—N57 is 77.09 (13)° at 150 K, compared with the ideal octahedral angle of 90°. While five of the six Co—N bonds in (I) are identical at the two temperatures to within experimental error, the Co1—N36 bond is 0.013 (2) Å longer at 150 K than at 290 K. This cannot reflect the existence of a partial spin-state transition upon cooling, since that would give rise to a shortening of this bond at lower temperature (Figgis et al., 1983; Holland et al., 2001), the opposite trend to that observed. Hence, the origin of this effect is uncertain, although librational shortening of the Co—N bonds at 290 K may contribute to it. All N—Co—N angles are identical in the two structures to within three s.u.s, except for N9—Co1—N57, which is 0.44 (8)° larger at 150 K than at 290 K, and N23—Co1—N57, which has contracted by 0.63 (8)° in the low-temperature structure. The significance of these small differences is also unclear.

The effective magnetic moment of (I) at 290 K is 4.2 µB, which is identical, within experimental error, to that exhibited by [Co(LMes)2](ClO4)2 (Holland et al., 2001), and is consistent with (I) being completely high-spin at this temperature (O'Connor, 1982). The almost identical molecular structures of (I) at 290 K and 150 K also demonstrate that (I) is still in a high-spin state at 150 K. That being the case, it is interesting that all the Co—N bonds in (I) are shorter than the corresponding bonds in [Co(LMes)2](ClO4)2·2CH3NO2 at 150 K, by between 0.017 (2) and 0.035 (2) Å. Despite this, the Co—N distances in (I) are within the range previously observed for high-spin CoII complexes with a hexa-nitrogen donor set (tabulated in Holland et al., 2001). In particular, the Co—N(pyridine) bond lengths, which are the most sensitive to the spin state of a CoII ion in this type of complex (Figgis et al., 1983), are within the range expected from a high-spin CoII compound. Hence, this study emphasizes that the coordination sphere in six-coordinate high-spin CoII complexes is rather plastic, and that structural data can only be related to the spin state in these compounds with care (Holland et al., 2001).

Experimental top

A mixture of Co(NO3)2·6H2O (0.16 g, 0.55 mmol) and LMes (0.50 g, 1.11 mmol) in MeCN (50 ml) was stirred at 323 K until all the solid had dissolved. The resultant orange solution was filtered, and then concentrated in vacuo until orange-yellow microcrystals began to form. After overnight storage of the mixture at 243 K, the product was filtered, washed with Et2O and dried in vacuo. Diffusion of Et2O vapour into a dilute MeCN solution of the sparingly soluble complex yielded small, strongly diffracting rectangular prisms of (I). The same crystal was used for data collection at both 290 K and 150 K.

Refinement top

At both temperatures, one of the two nitrate ions was disordered and was modelled over three orientations. At 290 K, these were refined with occupancies of 0.40, 0.30 and 0.30, the latter two orientations sharing a common N atom. At 150 K, three distinct partial NO3 moieties were detected, with occupancies of 0.40, 0.40 and 0.20. The N—O distances within the disordered anion at 290 K were restrained to 1.25 (1) Å, and non-bonded O···O distances within a given disorder orientation to 2.17 (1) Å. At 150 K, corresponding restraints of 1.26 (1) and 2.18 (1) Å, respectively, were applied. At both temperatures, all non-H atoms with occupancy >0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The torsion angles of all the CH3 groups in the molecule were allowed to refine freely except that, at both temperatures, antibumping restraints were applied to individual H atoms attached to atoms C21 and C53, and to C35 and C55. Even with these restraints, there is one abnormally short intermolecular H···H contact of H11···H35Ci 2.06–2.10 Å [symmetry code: (i) x, y − 1, z]. Introduction of additional antibumping restraints between H11 and the C35i methyl group prevented the refinements from converging, so these were omitted from the final models. However, for this reason, the refined methyl group torsions on C35 at the two temperatures probably do not correspond to the `true' equilibrium positions. The fixed C—H distances were as follows: at 290 K, CH(aryl) = 0.93 and CH(methyl) = 0.96 Å; at 150 K, CH(aryl) = 0.95 and CH(methyl) = 0.98 Å. At both temperatures, the H-atom Uiso parameters were fixed at 1.2Ueq(C) for CH(aryl), and 1.5Ueq(C) for CH(methyl). The Flack parameters (Flack, 1983) were calculated using 5661 (290 K) and 5773 (150 K) Friedel pairs.

Computing details top

For both compounds, data collection: COLLECT (Nonius, 1999); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995); software used to prepare material for publication: local program.

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of the [Co(LMes)2]2+ dication in (I) at 150 K, with 35% probability displacement ellipsoids, showing the atom-numbering scheme employed. H atoms have been omitted for clarity.
(I) Bis{2,6-bis[3-(2,4,6-trimethylphenyl)pyrazol- 1-yl-κN2]pyridine-κN}cobalt(II) dinitrate top
Crystal data top
[Co(C29H29N5)2](NO3)2Dx = 1.329 Mg m3
Mr = 1078.09Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21Cell parameters from 59607 reflections
a = 22.3350 (1) Åθ = 2.6–27.5°
b = 10.9094 (2) ŵ = 0.38 mm1
c = 22.1061 (2) ÅT = 290 K
V = 5386.40 (11) Å3Rectangular prism, orange
Z = 40.45 × 0.35 × 0.28 mm
F(000) = 2260
Data collection top
Nonius KappaCCD area-detector
diffractometer
11975 independent reflections
Radiation source: fine-focus sealed tube10665 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 2.6°
type of scansh = 2927
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
k = 1214
Tmin = 0.847, Tmax = 0.901l = 2828
59607 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.037 w = 1/[σ2(Fo2) + (0.061P)2 + 0.6652P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.104(Δ/σ)max = 0.001
S = 1.04Δρmax = 0.26 e Å3
11975 reflectionsΔρmin = 0.28 e Å3
721 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
21 restraintsExtinction coefficient: 0.0083 (8)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.004 (9)
Crystal data top
[Co(C29H29N5)2](NO3)2V = 5386.40 (11) Å3
Mr = 1078.09Z = 4
Orthorhombic, Pca21Mo Kα radiation
a = 22.3350 (1) ŵ = 0.38 mm1
b = 10.9094 (2) ÅT = 290 K
c = 22.1061 (2) Å0.45 × 0.35 × 0.28 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
11975 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
10665 reflections with I > 2σ(I)
Tmin = 0.847, Tmax = 0.901Rint = 0.046
59607 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.104Δρmax = 0.26 e Å3
S = 1.04Δρmin = 0.28 e Å3
11975 reflectionsAbsolute structure: Flack (1983)
721 parametersAbsolute structure parameter: 0.004 (9)
21 restraints
Special details top

Experimental. Detector set at 30 mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings

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.

One nitrate anion is disordered over three orientations: N74A—O77A, occupancy 0.30 N74A, O75B—O77B, occupancy 0.30 (i.e N74A has total occupancy 0.60) N74C—O77C, occupancy 0.40. A ttempts to refine a distinct N atom for disorder orientation 'B' were unsuccessful. The N—O distances within the disordered anion were restrained to 1.25 (2) Å, and non-bonded O···O distances within a given disorder orientation to 2.17 (2) Å. All non-H atoms with occupancy >0.5 were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The torsions of all the methyl groups were allowed to refine freely, except that anti-bumping restraints were applied to H35A and H55A, and to H21B and H53B, to prevent abnormally short intramolecular H···H contacts in the final model. Even with these restraints, there is one abnormally short intermolecular H···H contact of H11···H35Ci 2.10 Å (related by x, y − 1, z). Introduction of additional antibumping restraints between H11 and the C35i methyl group prevented the refinement from converging, so that these were omitted from the final model. However, for this reason the refined methyl group torsion on C35 probably does not correspond to the 'true' equilibrium position.

The Flack parameters was calculated using 5661 Friedel pairs.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.607489 (10)0.76851 (2)0.680880 (14)0.03987 (8)
N20.57191 (8)0.74731 (15)0.76390 (8)0.0446 (4)
C30.55530 (10)0.6364 (2)0.78252 (10)0.0489 (4)
C40.53254 (11)0.6152 (2)0.83960 (11)0.0580 (5)
H40.52170.53700.85240.070*
C50.52679 (11)0.7160 (2)0.87670 (11)0.0594 (5)
H50.51170.70530.91560.071*
C60.54270 (10)0.8327 (2)0.85814 (11)0.0554 (5)
H60.53800.90060.88320.066*
C70.56580 (9)0.84295 (19)0.80055 (10)0.0456 (4)
N80.56316 (9)0.54573 (17)0.73743 (9)0.0564 (4)
N90.58487 (7)0.57989 (14)0.68215 (9)0.0483 (3)
C100.58058 (13)0.4814 (2)0.64692 (12)0.0646 (6)
C110.5552 (2)0.3850 (2)0.68054 (18)0.1089 (14)
H110.54680.30650.66650.131*
C120.54517 (19)0.4278 (3)0.73672 (16)0.0948 (11)
H120.52890.38420.76890.114*
C130.59768 (12)0.4863 (2)0.58140 (11)0.0600 (6)
C140.65777 (13)0.4790 (2)0.56409 (12)0.0635 (6)
C150.67262 (13)0.4905 (3)0.50323 (13)0.0678 (7)
H150.71260.48560.49180.081*
C160.62930 (13)0.5090 (3)0.45922 (12)0.0678 (6)
C170.57040 (13)0.5119 (3)0.47714 (13)0.0715 (7)
H170.54090.52250.44790.086*
C180.55331 (12)0.4996 (3)0.53682 (13)0.0695 (7)
C190.70679 (16)0.4563 (3)0.60912 (15)0.0844 (9)
H19A0.70430.37350.62360.127*
H19B0.70250.51190.64250.127*
H19C0.74490.46900.59010.127*
C200.64758 (18)0.5258 (4)0.39392 (14)0.0957 (11)
H20A0.61320.51590.36830.144*
H20B0.67730.46580.38350.144*
H20C0.66390.60650.38850.144*
C210.48794 (15)0.5013 (5)0.55272 (19)0.1132 (15)
H21A0.46450.49250.51660.170*
H21B0.47830.57760.57200.170*
H21C0.47920.43480.57980.170*
N220.58671 (8)0.95299 (16)0.77437 (8)0.0468 (4)
N230.61361 (7)0.94846 (16)0.71854 (8)0.0434 (3)
C240.63490 (9)1.06095 (19)0.70766 (11)0.0488 (4)
C250.62093 (13)1.1370 (2)0.75783 (13)0.0624 (6)
H250.63051.21950.76200.075*
C260.59119 (12)1.0673 (2)0.79821 (12)0.0608 (6)
H260.57651.09270.83550.073*
C270.67046 (9)1.09025 (18)0.65231 (11)0.0496 (4)
C280.73324 (10)1.0974 (2)0.65716 (12)0.0581 (5)
C290.76674 (11)1.1237 (3)0.60657 (15)0.0692 (7)
H290.80821.12720.61030.083*
C300.74159 (12)1.1450 (3)0.55046 (14)0.0714 (7)
C310.67956 (12)1.1402 (2)0.54673 (12)0.0624 (6)
H310.66141.15580.50960.075*
C320.64328 (10)1.1130 (2)0.59637 (11)0.0531 (5)
C330.76527 (12)1.0772 (3)0.71653 (14)0.0752 (8)
H33A0.76860.99080.72420.113*
H33B0.74301.11520.74860.113*
H33C0.80461.11260.71450.113*
C340.77911 (17)1.1722 (5)0.4957 (2)0.1076 (13)
H34A0.81051.22830.50640.161*
H34B0.75451.20820.46480.161*
H34C0.79641.09750.48080.161*
C350.57717 (10)1.1124 (2)0.58626 (13)0.0629 (6)
H35A0.55851.05880.61510.094*
H35B0.56881.08410.54600.094*
H35C0.56181.19400.59120.094*
N360.64243 (7)0.79238 (16)0.59803 (8)0.0437 (3)
C370.60653 (8)0.8124 (2)0.55128 (10)0.0450 (4)
C380.62794 (10)0.8306 (2)0.49313 (10)0.0547 (5)
H380.60230.84240.46050.066*
C390.68920 (12)0.8302 (3)0.48635 (11)0.0625 (6)
H390.70520.84210.44790.075*
C400.72801 (10)0.8129 (3)0.53452 (11)0.0583 (5)
H400.76930.81550.52960.070*
C410.70184 (9)0.79158 (19)0.59044 (10)0.0462 (4)
N420.54538 (8)0.81694 (17)0.56736 (8)0.0462 (4)
N430.53080 (7)0.81276 (15)0.62770 (8)0.0442 (3)
C440.47234 (9)0.8388 (2)0.63077 (10)0.0517 (5)
C450.44993 (10)0.8589 (3)0.57238 (12)0.0673 (7)
H450.41060.87780.56230.081*
C460.49617 (10)0.8457 (3)0.53343 (11)0.0602 (6)
H460.49480.85460.49160.072*
C470.44206 (8)0.8464 (2)0.69096 (11)0.0546 (5)
C480.41866 (12)0.7403 (2)0.71846 (14)0.0637 (6)
C490.39602 (13)0.7501 (3)0.77725 (16)0.0747 (8)
H490.38210.67970.79630.090*
C500.39348 (11)0.8585 (3)0.80785 (13)0.0720 (7)
C510.41353 (11)0.9626 (3)0.77896 (13)0.0683 (6)
H510.41131.03740.79900.082*
C520.43717 (9)0.9590 (2)0.72048 (11)0.0585 (5)
C530.41764 (16)0.6195 (3)0.6862 (2)0.0937 (10)
H53A0.39810.55950.71110.141*
H53B0.45790.59370.67800.141*
H53C0.39620.62790.64880.141*
C540.36962 (19)0.8661 (5)0.87150 (16)0.1073 (12)
H54A0.37610.78940.89170.161*
H54B0.32750.88360.87040.161*
H54C0.39000.93020.89290.161*
C550.45633 (12)1.0771 (3)0.69217 (17)0.0799 (8)
H55A0.49751.09270.70190.120*
H55B0.43191.14260.70740.120*
H55C0.45191.07170.64910.120*
N560.73330 (8)0.76534 (17)0.64401 (9)0.0493 (4)
N570.70164 (7)0.73378 (15)0.69457 (8)0.0462 (4)
C580.74179 (9)0.7006 (2)0.73604 (11)0.0542 (5)
C590.80006 (11)0.7140 (3)0.71203 (14)0.0674 (7)
H590.83600.69860.73190.081*
C600.79328 (11)0.7540 (3)0.65399 (13)0.0616 (6)
H600.82370.77030.62650.074*
C610.72196 (9)0.6563 (2)0.79660 (11)0.0558 (5)
C620.71531 (12)0.5299 (3)0.80706 (13)0.0663 (6)
C630.69156 (14)0.4917 (3)0.86212 (17)0.0809 (9)
H630.68590.40830.86870.097*
C640.67597 (13)0.5735 (4)0.90752 (15)0.0829 (9)
C650.68537 (12)0.6981 (3)0.89752 (13)0.0737 (7)
H650.67580.75440.92760.088*
C660.70900 (11)0.7393 (3)0.84285 (12)0.0619 (6)
C670.7346 (2)0.4340 (3)0.76170 (17)0.0933 (10)
H67A0.75160.36530.78260.140*
H67B0.76390.46850.73490.140*
H67C0.70040.40740.73880.140*
C680.6485 (2)0.5272 (6)0.9655 (2)0.1256 (17)
H68A0.62260.45920.95680.188*
H68B0.62570.59170.98410.188*
H68C0.67960.50120.99260.188*
C690.72050 (15)0.8746 (3)0.83585 (14)0.0756 (7)
H69A0.70450.91750.87020.113*
H69B0.70150.90360.79960.113*
H69C0.76280.88890.83330.113*
N700.51618 (19)0.7544 (3)0.36273 (14)0.0915 (9)
O710.52326 (14)0.8553 (2)0.38852 (10)0.0991 (8)
O720.5505 (2)0.7169 (4)0.3250 (2)0.1495 (14)
O730.47080 (19)0.6941 (3)0.37401 (18)0.1396 (13)
N74A0.59323 (14)0.8685 (5)1.0120 (2)0.0738 (14)0.60
O75A0.6265 (3)0.9284 (7)0.9786 (4)0.083 (2)*0.30
O76A0.6201 (4)0.7880 (9)1.0457 (4)0.106 (3)*0.30
O77A0.5393 (2)0.8447 (9)1.0021 (4)0.0541 (15)*0.30
O75B0.6308 (3)0.8734 (9)1.0520 (4)0.091 (2)*0.30
O76B0.5459 (4)0.8113 (11)1.0125 (5)0.111 (4)*0.30
O77B0.6003 (4)0.9536 (8)0.9694 (4)0.104 (3)*0.30
N74C0.5932 (5)0.8383 (15)1.0211 (8)0.182 (8)*0.40
O75C0.5873 (6)0.7684 (10)1.0657 (6)0.170 (4)*0.40
O76C0.6388 (4)0.9051 (9)1.0220 (5)0.135 (3)*0.40
O77C0.5468 (3)0.8841 (8)0.9965 (4)0.098 (3)*0.40
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.04282 (12)0.04065 (12)0.03614 (12)0.00026 (8)0.00090 (11)0.00076 (14)
N20.0495 (9)0.0424 (9)0.0421 (9)0.0018 (6)0.0021 (7)0.0010 (7)
C30.0550 (11)0.0476 (11)0.0441 (11)0.0023 (8)0.0029 (8)0.0019 (8)
C40.0689 (13)0.0573 (13)0.0479 (12)0.0014 (10)0.0089 (10)0.0065 (10)
C50.0660 (13)0.0679 (15)0.0444 (12)0.0016 (10)0.0084 (10)0.0035 (10)
C60.0610 (12)0.0610 (13)0.0441 (11)0.0039 (10)0.0042 (9)0.0076 (9)
C70.0462 (10)0.0472 (11)0.0435 (10)0.0025 (8)0.0014 (8)0.0019 (8)
N80.0748 (12)0.0430 (9)0.0513 (10)0.0026 (8)0.0116 (9)0.0031 (8)
N90.0606 (8)0.0423 (7)0.0419 (8)0.0001 (6)0.0015 (9)0.0017 (9)
C100.0906 (17)0.0439 (12)0.0595 (15)0.0054 (11)0.0113 (13)0.0050 (10)
C110.204 (4)0.0410 (12)0.0815 (19)0.0303 (17)0.047 (3)0.0130 (16)
C120.163 (3)0.0423 (13)0.0789 (19)0.0194 (16)0.040 (2)0.0010 (13)
C130.0827 (15)0.0448 (12)0.0526 (13)0.0061 (10)0.0093 (11)0.0139 (10)
C140.0822 (16)0.0506 (12)0.0575 (13)0.0088 (11)0.0024 (12)0.0078 (10)
C150.0741 (16)0.0705 (16)0.0588 (15)0.0054 (12)0.0058 (12)0.0097 (12)
C160.0819 (16)0.0675 (16)0.0539 (14)0.0007 (13)0.0024 (13)0.0111 (12)
C170.0778 (16)0.0779 (17)0.0588 (15)0.0048 (13)0.0102 (13)0.0200 (13)
C180.0739 (15)0.0669 (15)0.0678 (16)0.0102 (12)0.0073 (13)0.0265 (13)
C190.100 (2)0.086 (2)0.0679 (18)0.0235 (17)0.0134 (16)0.0090 (15)
C200.107 (3)0.123 (3)0.0574 (18)0.006 (2)0.0064 (16)0.0076 (18)
C210.0744 (19)0.167 (4)0.098 (3)0.027 (2)0.0113 (18)0.047 (3)
N220.0523 (9)0.0439 (9)0.0443 (9)0.0004 (7)0.0008 (7)0.0070 (7)
N230.0468 (8)0.0422 (9)0.0411 (9)0.0008 (6)0.0024 (6)0.0021 (7)
C240.0498 (10)0.0408 (10)0.0558 (11)0.0010 (8)0.0078 (9)0.0013 (8)
C250.0757 (15)0.0421 (12)0.0693 (16)0.0052 (10)0.0022 (12)0.0114 (11)
C260.0733 (14)0.0495 (12)0.0594 (14)0.0025 (10)0.0007 (12)0.0158 (10)
C270.0503 (10)0.0378 (10)0.0607 (12)0.0031 (8)0.0041 (9)0.0026 (8)
C280.0518 (11)0.0501 (12)0.0724 (15)0.0038 (9)0.0059 (10)0.0078 (10)
C290.0506 (12)0.0694 (16)0.0877 (19)0.0018 (10)0.0004 (12)0.0148 (14)
C300.0665 (15)0.0687 (16)0.0790 (18)0.0042 (11)0.0119 (13)0.0123 (13)
C310.0689 (14)0.0596 (13)0.0587 (14)0.0015 (10)0.0029 (11)0.0061 (11)
C320.0560 (11)0.0407 (11)0.0626 (13)0.0013 (8)0.0054 (10)0.0028 (9)
C330.0595 (14)0.086 (2)0.0805 (19)0.0064 (13)0.0158 (13)0.0154 (16)
C340.089 (2)0.136 (4)0.098 (3)0.001 (2)0.025 (2)0.035 (2)
C350.0575 (12)0.0622 (14)0.0689 (16)0.0004 (10)0.0089 (11)0.0005 (12)
N360.0459 (8)0.0446 (9)0.0406 (8)0.0012 (6)0.0020 (7)0.0006 (7)
C370.0485 (10)0.0444 (10)0.0419 (10)0.0018 (7)0.0001 (8)0.0046 (8)
C380.0573 (11)0.0664 (14)0.0402 (10)0.0024 (10)0.0014 (9)0.0005 (9)
C390.0668 (13)0.0777 (16)0.0429 (12)0.0027 (12)0.0113 (10)0.0036 (11)
C400.0525 (11)0.0714 (15)0.0511 (12)0.0013 (11)0.0112 (9)0.0036 (11)
C410.0466 (10)0.0478 (10)0.0441 (10)0.0017 (7)0.0025 (8)0.0013 (8)
N420.0465 (8)0.0542 (10)0.0380 (8)0.0033 (7)0.0022 (7)0.0014 (7)
N430.0452 (8)0.0487 (9)0.0386 (9)0.0023 (6)0.0004 (6)0.0003 (7)
C440.0434 (10)0.0596 (12)0.0522 (12)0.0010 (8)0.0009 (8)0.0053 (10)
C450.0449 (11)0.099 (2)0.0577 (14)0.0010 (11)0.0074 (10)0.0089 (13)
C460.0518 (11)0.0809 (16)0.0479 (12)0.0038 (10)0.0100 (10)0.0051 (11)
C470.0402 (9)0.0693 (13)0.0541 (14)0.0052 (8)0.0000 (9)0.0056 (10)
C480.0542 (13)0.0727 (16)0.0642 (15)0.0040 (10)0.0096 (11)0.0075 (12)
C490.0649 (16)0.091 (2)0.0683 (19)0.0079 (12)0.0129 (13)0.0175 (15)
C500.0589 (14)0.103 (2)0.0543 (14)0.0112 (13)0.0061 (11)0.0011 (15)
C510.0539 (12)0.0849 (18)0.0661 (16)0.0062 (12)0.0023 (11)0.0088 (13)
C520.0435 (10)0.0731 (15)0.0589 (14)0.0061 (9)0.0006 (9)0.0015 (11)
C530.104 (2)0.0738 (17)0.103 (2)0.0111 (14)0.035 (2)0.001 (2)
C540.109 (3)0.147 (4)0.066 (2)0.013 (2)0.0246 (19)0.006 (2)
C550.0778 (16)0.0675 (15)0.094 (2)0.0045 (12)0.0165 (16)0.0025 (15)
N560.0434 (9)0.0560 (10)0.0485 (10)0.0017 (7)0.0015 (7)0.0045 (8)
N570.0455 (8)0.0478 (9)0.0452 (11)0.0023 (6)0.0003 (7)0.0021 (7)
C580.0480 (10)0.0590 (12)0.0556 (13)0.0036 (9)0.0083 (10)0.0043 (10)
C590.0441 (11)0.0891 (19)0.0689 (17)0.0063 (11)0.0045 (11)0.0116 (14)
C600.0418 (11)0.0784 (16)0.0647 (15)0.0019 (10)0.0045 (10)0.0072 (12)
C610.0485 (10)0.0647 (14)0.0543 (12)0.0024 (9)0.0096 (9)0.0097 (10)
C620.0634 (13)0.0716 (16)0.0639 (15)0.0015 (11)0.0141 (12)0.0152 (12)
C630.0764 (17)0.084 (2)0.083 (2)0.0054 (14)0.0101 (15)0.0322 (17)
C640.0628 (15)0.113 (2)0.0732 (19)0.0058 (15)0.0049 (13)0.0332 (18)
C650.0589 (13)0.104 (2)0.0587 (15)0.0137 (14)0.0018 (11)0.0101 (14)
C660.0533 (12)0.0770 (16)0.0553 (13)0.0066 (11)0.0102 (10)0.0092 (11)
C670.130 (3)0.070 (2)0.079 (2)0.0036 (18)0.017 (2)0.0070 (16)
C680.099 (3)0.172 (4)0.105 (3)0.018 (3)0.038 (2)0.061 (3)
C690.0882 (18)0.0721 (17)0.0665 (17)0.0042 (14)0.0181 (14)0.0012 (14)
N700.140 (3)0.0681 (16)0.0661 (16)0.0111 (17)0.0375 (18)0.0001 (13)
O710.154 (2)0.0782 (14)0.0655 (13)0.0208 (14)0.0310 (14)0.0047 (11)
O720.163 (3)0.135 (3)0.151 (3)0.041 (2)0.015 (3)0.034 (3)
O730.195 (4)0.0941 (19)0.130 (3)0.048 (2)0.031 (3)0.0052 (18)
N74A0.0384 (15)0.102 (3)0.081 (3)0.0166 (17)0.0128 (17)0.050 (2)
Geometric parameters (Å, º) top
Co1—N22.0132 (18)C37—N421.412 (3)
Co1—N92.1190 (15)C38—C391.376 (3)
Co1—N232.1368 (17)C38—H380.9300
Co1—N362.0077 (17)C39—C401.386 (4)
Co1—N432.1327 (17)C39—H390.9300
Co1—N572.1581 (16)C40—C411.387 (3)
N2—C71.328 (3)C40—H400.9300
N2—C31.331 (3)C41—N561.406 (3)
C3—C41.380 (3)N42—C461.367 (3)
C3—N81.415 (3)N42—N431.374 (2)
C4—C51.378 (4)N43—C441.338 (3)
C4—H40.9300C44—C451.402 (3)
C5—C61.384 (4)C44—C471.495 (3)
C5—H50.9300C45—C461.352 (4)
C6—C71.378 (3)C45—H450.9300
C6—H60.9300C46—H460.9300
C7—N221.412 (3)C47—C521.395 (3)
N8—C121.348 (3)C47—C481.409 (3)
N8—N91.366 (3)C48—C491.399 (4)
N9—C101.330 (3)C48—C531.498 (4)
C10—C111.407 (4)C49—C501.363 (5)
C10—C131.499 (3)C49—H490.9300
C11—C121.345 (5)C50—C511.378 (5)
C11—H110.9300C50—C541.507 (4)
C12—H120.9300C51—C521.397 (4)
C13—C141.398 (4)C51—H510.9300
C13—C181.405 (4)C52—C551.495 (4)
C14—C151.391 (4)C53—H53A0.9600
C14—C191.500 (4)C53—H53B0.9600
C15—C161.387 (4)C53—H53C0.9600
C15—H150.9300C54—H54A0.9600
C16—C171.374 (4)C54—H54B0.9600
C16—C201.512 (4)C54—H54C0.9600
C17—C181.380 (4)C55—H55A0.9600
C17—H170.9300C55—H55B0.9600
C18—C211.502 (4)C55—H55C0.9600
C19—H19A0.9600N56—C601.363 (3)
C19—H19B0.9600N56—N571.366 (2)
C19—H19C0.9600N57—C581.332 (3)
C20—H20A0.9600C58—C591.413 (4)
C20—H20B0.9600C58—C611.490 (3)
C20—H20C0.9600C59—C601.363 (4)
C21—H21A0.9600C59—H590.9300
C21—H21B0.9600C60—H600.9300
C21—H21C0.9600C61—C661.396 (4)
N22—C261.357 (3)C61—C621.407 (4)
N22—N231.373 (2)C62—C631.391 (4)
N23—C241.338 (3)C62—C671.511 (5)
C24—C251.419 (3)C63—C641.388 (5)
C24—C271.493 (3)C63—H630.9300
C25—C261.348 (4)C64—C651.393 (5)
C25—H250.9300C64—C681.509 (5)
C26—H260.9300C65—C661.393 (4)
C27—C321.400 (3)C65—H650.9300
C27—C281.408 (3)C66—C691.506 (4)
C28—C291.376 (4)C67—H67A0.9600
C28—C331.511 (4)C67—H67B0.9600
C29—C301.381 (4)C67—H67C0.9600
C29—H290.9300C68—H68A0.9600
C30—C311.389 (4)C68—H68B0.9600
C30—C341.502 (4)C68—H68C0.9600
C31—C321.396 (4)C69—H69A0.9600
C31—H310.9300C69—H69B0.9600
C32—C351.493 (3)C69—H69C0.9600
C33—H33A0.9600N70—O721.204 (5)
C33—H33B0.9600N70—O731.234 (5)
C33—H33C0.9600N70—O711.249 (4)
C34—H34A0.9600N74A—O75A1.234 (7)
C34—H34B0.9600N74A—O77A1.251 (6)
C34—H34C0.9600N74A—O76A1.298 (8)
C35—H35A0.9600N74A—O75B1.220 (6)
C35—H35B0.9600N74A—O76B1.227 (7)
C35—H35C0.9600N74A—O77B1.332 (7)
N36—C371.326 (3)N74C—O75C1.253 (9)
N36—C411.338 (3)N74C—O76C1.253 (9)
C37—C381.386 (3)N74C—O77C1.272 (9)
N2—Co1—N977.42 (7)H35B—C35—H35C109.5
N2—Co1—N2377.03 (7)C37—N36—C41120.21 (18)
N2—Co1—N36179.08 (7)C37—N36—Co1119.81 (13)
N2—Co1—N43102.21 (7)C41—N36—Co1119.95 (14)
N2—Co1—N57103.69 (7)N36—C37—C38122.54 (18)
N9—Co1—N36103.34 (7)N36—C37—N42113.23 (18)
N9—Co1—N23154.45 (7)C38—C37—N42124.20 (19)
N9—Co1—N4392.04 (7)C39—C38—C37116.3 (2)
N9—Co1—N5793.44 (6)C39—C38—H38121.8
N23—Co1—N36102.20 (7)C37—C38—H38121.8
N23—Co1—N4393.34 (6)C38—C39—C40122.6 (2)
N23—Co1—N5792.54 (6)C38—C39—H39118.7
N36—Co1—N4377.29 (7)C40—C39—H39118.7
N36—Co1—N5776.81 (6)C39—C40—C41116.4 (2)
N43—Co1—N57154.10 (6)C39—C40—H40121.8
C7—N2—C3119.80 (19)C41—C40—H40121.8
C7—N2—Co1120.43 (14)N36—C41—C40121.9 (2)
C3—N2—Co1119.76 (14)N36—C41—N56113.03 (18)
N2—C3—C4122.5 (2)C40—C41—N56125.04 (18)
N2—C3—N8112.52 (19)C46—N42—N43110.48 (18)
C4—C3—N8124.9 (2)C46—N42—C37130.4 (2)
C5—C4—C3116.4 (2)N43—N42—C37118.19 (16)
C5—C4—H4121.8C44—N43—N42105.87 (17)
C3—C4—H4121.8C44—N43—Co1143.50 (15)
C4—C5—C6122.3 (2)N42—N43—Co1110.63 (12)
C4—C5—H5118.9N43—C44—C45109.6 (2)
C6—C5—H5118.9N43—C44—C47119.90 (19)
C7—C6—C5116.4 (2)C45—C44—C47130.49 (19)
C7—C6—H6121.8C46—C45—C44107.3 (2)
C5—C6—H6121.8C46—C45—H45126.4
N2—C7—C6122.6 (2)C44—C45—H45126.4
N2—C7—N22112.57 (19)C45—C46—N42106.8 (2)
C6—C7—N22124.8 (2)C45—C46—H46126.6
C12—N8—N9110.8 (2)N42—C46—H46126.6
C12—N8—C3129.7 (2)C52—C47—C48119.5 (2)
N9—N8—C3118.91 (17)C52—C47—C44120.1 (2)
C10—N9—N8106.14 (18)C48—C47—C44120.4 (2)
C10—N9—Co1142.51 (17)C49—C48—C47118.2 (3)
N8—N9—Co1111.18 (13)C49—C48—C53120.3 (3)
N9—C10—C11108.9 (2)C47—C48—C53121.6 (3)
N9—C10—C13121.3 (2)C50—C49—C48122.9 (3)
C11—C10—C13129.7 (2)C50—C49—H49118.6
C12—C11—C10107.2 (2)C48—C49—H49118.6
C12—C11—H11126.4C49—C50—C51118.1 (3)
C10—C11—H11126.4C49—C50—C54121.8 (3)
C11—C12—N8107.0 (3)C51—C50—C54120.1 (3)
C11—C12—H12126.5C50—C51—C52121.9 (3)
N8—C12—H12126.5C50—C51—H51119.1
C14—C13—C18119.4 (2)C52—C51—H51119.1
C14—C13—C10120.5 (2)C47—C52—C51119.2 (2)
C18—C13—C10120.1 (2)C47—C52—C55122.7 (2)
C15—C14—C13119.3 (2)C51—C52—C55118.1 (3)
C15—C14—C19118.8 (3)C48—C53—H53A109.5
C13—C14—C19121.9 (3)C48—C53—H53B109.5
C16—C15—C14121.7 (3)H53A—C53—H53B109.5
C16—C15—H15119.2C48—C53—H53C109.5
C14—C15—H15119.2H53A—C53—H53C109.5
C17—C16—C15118.0 (3)H53B—C53—H53C109.5
C17—C16—C20122.1 (3)C50—C54—H54A109.5
C15—C16—C20120.0 (3)C50—C54—H54B109.5
C16—C17—C18122.6 (3)H54A—C54—H54B109.5
C16—C17—H17118.7C50—C54—H54C109.5
C18—C17—H17118.7H54A—C54—H54C109.5
C17—C18—C13119.0 (3)H54B—C54—H54C109.5
C17—C18—C21119.4 (3)C52—C55—H55A109.5
C13—C18—C21121.5 (3)C52—C55—H55B109.5
C14—C19—H19A109.5H55A—C55—H55B109.5
C14—C19—H19B109.5C52—C55—H55C109.5
H19A—C19—H19B109.5H55A—C55—H55C109.5
C14—C19—H19C109.5H55B—C55—H55C109.5
H19A—C19—H19C109.5C60—N56—N57110.67 (19)
H19B—C19—H19C109.5C60—N56—C41130.2 (2)
C16—C20—H20A109.5N57—N56—C41118.78 (15)
C16—C20—H20B109.5C58—N57—N56106.44 (17)
H20A—C20—H20B109.5C58—N57—Co1143.11 (15)
C16—C20—H20C109.5N56—N57—Co1110.20 (12)
H20A—C20—H20C109.5N57—C58—C59109.5 (2)
H20B—C20—H20C109.5N57—C58—C61120.40 (19)
C18—C21—H21A109.5C59—C58—C61130.1 (2)
C18—C21—H21B109.5C60—C59—C58106.5 (2)
H21A—C21—H21B109.5C60—C59—H59126.7
C18—C21—H21C109.5C58—C59—H59126.7
H21A—C21—H21C109.5C59—C60—N56106.9 (2)
H21B—C21—H21C109.5C59—C60—H60126.6
C26—N22—N23110.47 (19)N56—C60—H60126.6
C26—N22—C7130.2 (2)C66—C61—C62119.6 (2)
N23—N22—C7118.84 (16)C66—C61—C58120.6 (2)
C24—N23—N22106.50 (17)C62—C61—C58119.8 (2)
C24—N23—Co1142.70 (15)C63—C62—C61118.5 (3)
N22—N23—Co1110.80 (12)C63—C62—C67118.8 (3)
N23—C24—C25108.5 (2)C61—C62—C67122.6 (3)
N23—C24—C27122.18 (19)C64—C63—C62122.4 (3)
C25—C24—C27129.2 (2)C64—C63—H63118.8
C26—C25—C24107.2 (2)C62—C63—H63118.8
C26—C25—H25126.4C63—C64—C65118.4 (3)
C24—C25—H25126.4C63—C64—C68120.1 (4)
C25—C26—N22107.3 (2)C65—C64—C68121.6 (4)
C25—C26—H26126.4C66—C65—C64120.6 (3)
N22—C26—H26126.4C66—C65—H65119.7
C32—C27—C28119.3 (2)C64—C65—H65119.7
C32—C27—C24122.08 (18)C65—C66—C61120.3 (3)
C28—C27—C24118.6 (2)C65—C66—C69118.0 (3)
C29—C28—C27119.4 (2)C61—C66—C69121.6 (2)
C29—C28—C33118.6 (2)C62—C67—H67A109.5
C27—C28—C33122.0 (2)C62—C67—H67B109.5
C28—C29—C30122.9 (2)H67A—C67—H67B109.5
C28—C29—H29118.5C62—C67—H67C109.5
C30—C29—H29118.5H67A—C67—H67C109.5
C29—C30—C31116.9 (2)H67B—C67—H67C109.5
C29—C30—C34122.0 (3)C64—C68—H68A109.5
C31—C30—C34121.1 (3)C64—C68—H68B109.5
C30—C31—C32122.7 (2)H68A—C68—H68B109.5
C30—C31—H31118.6C64—C68—H68C109.5
C32—C31—H31118.6H68A—C68—H68C109.5
C31—C32—C27118.7 (2)H68B—C68—H68C109.5
C31—C32—C35117.2 (2)C66—C69—H69A109.5
C27—C32—C35124.1 (2)C66—C69—H69B109.5
C28—C33—H33A109.5H69A—C69—H69B109.5
C28—C33—H33B109.5C66—C69—H69C109.5
H33A—C33—H33B109.5H69A—C69—H69C109.5
C28—C33—H33C109.5H69B—C69—H69C109.5
H33A—C33—H33C109.5O72—N70—O73118.8 (4)
H33B—C33—H33C109.5O72—N70—O71122.3 (4)
C30—C34—H34A109.5O73—N70—O71118.8 (4)
C30—C34—H34B109.5O75A—N74A—O77A125.8 (6)
H34A—C34—H34B109.5O75A—N74A—O76A115.0 (6)
C30—C34—H34C109.5O77A—N74A—O76A113.9 (7)
H34A—C34—H34C109.5O75B—N74A—O76B127.5 (7)
H34B—C34—H34C109.5O75B—N74A—O77B113.6 (6)
C32—C35—H35A109.5O76B—N74A—O77B117.6 (6)
C32—C35—H35B109.5O75C—N74C—O76C115.3 (10)
H35A—C35—H35B109.5O75C—N74C—O77C119.4 (11)
C32—C35—H35C109.5O76C—N74C—O77C116.1 (10)
H35A—C35—H35C109.5
(II) Bis{2,6-bis[3-(2,4,6-trimethylphenyl)pyrazol- 1-yl-κN2]pyridine-κN}cobalt(II) dinitrate top
Crystal data top
[Co(C29H29N5)2](NO3)2Dx = 1.358 Mg m3
Mr = 1078.09Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21Cell parameters from 86435 reflections
a = 22.1974 (2) Åθ = 2.6–27.5°
b = 10.7761 (1) ŵ = 0.39 mm1
c = 22.0365 (1) ÅT = 150 K
V = 5271.16 (7) Å3Rectangular prism, orange
Z = 40.45 × 0.35 × 0.28 mm
F(000) = 2260
Data collection top
Nonius KappaCCD area-detector
diffractometer
11941 independent reflections
Radiation source: fine-focus sealed tube11339 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 2.6°
type of scansh = 2828
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
k = 1313
Tmin = 0.844, Tmax = 0.899l = 2728
86435 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.037 w = 1/[σ2(Fo2) + (0.0591P)2 + 1.4056P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.099(Δ/σ)max = 0.001
S = 1.06Δρmax = 0.68 e Å3
11941 reflectionsΔρmin = 0.35 e Å3
720 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
20 restraintsExtinction coefficient: 0.0124 (9)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack, 1983
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.001 (8)
Crystal data top
[Co(C29H29N5)2](NO3)2V = 5271.16 (7) Å3
Mr = 1078.09Z = 4
Orthorhombic, Pca21Mo Kα radiation
a = 22.1974 (2) ŵ = 0.39 mm1
b = 10.7761 (1) ÅT = 150 K
c = 22.0365 (1) Å0.45 × 0.35 × 0.28 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
11941 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
11339 reflections with I > 2σ(I)
Tmin = 0.844, Tmax = 0.899Rint = 0.052
86435 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.099Δρmax = 0.68 e Å3
S = 1.06Δρmin = 0.35 e Å3
11941 reflectionsAbsolute structure: Flack, 1983
720 parametersAbsolute structure parameter: 0.001 (8)
20 restraints
Special details top

Experimental. Detector set at 30 mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings

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.

One nitrate anion is disordered over three orientations: N74A—O77A, occupancy 0.40 N74B—O77B, occupancy 0.40 N74C—O77C, occupancy 0.20. The N—O distances within the disordered anion were restrained to 1.26 (1) Å, and non-bonded O···O distances within a given disorder orientation to 2.18 (1) Å. All non-H atoms except the disordered anion were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The torsions of all the methyl groups were allowed to refine freely, except that anti-bumping restraints were applied to H21B and H53B, and to H35A and H55C, to prevent abnormally short H···H contacts in the final model. Even with these restraints, there is one abnormally short intermolecular H···H contact of H11···H35Ci = 2.06 Å (related by x, y − 1, z). Introduction of additional antibumping restraints between H11 and the C35i methyl group prevented the refinement from converging, so that these were omitted from the final model. However, for this reason the refined methyl group torsion on C35 probably does not correspond to the 'true' equilibrium position.

The Flack parameter was calculated using 5773 Friedel pairs.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.607483 (10)0.76975 (2)0.680922 (13)0.02464 (7)
N20.57123 (7)0.74756 (15)0.76429 (8)0.0281 (3)
C30.55503 (9)0.63473 (18)0.78297 (9)0.0301 (4)
C40.53155 (10)0.6123 (2)0.84023 (9)0.0352 (4)
H40.52060.53130.85320.042*
C50.52497 (10)0.7152 (2)0.87759 (9)0.0357 (4)
H50.50920.70400.91730.043*
C60.54073 (9)0.83395 (19)0.85877 (9)0.0331 (4)
H60.53530.90430.88420.040*
C70.56472 (8)0.84434 (18)0.80124 (9)0.0281 (4)
N80.56351 (8)0.54347 (15)0.73779 (8)0.0345 (4)
N90.58603 (7)0.57828 (14)0.68231 (8)0.0297 (3)
C100.58181 (11)0.4787 (2)0.64691 (10)0.0409 (5)
C110.55647 (15)0.3800 (2)0.68013 (15)0.0638 (8)
H110.54880.29840.66570.077*
C120.54501 (15)0.4237 (2)0.73680 (13)0.0576 (7)
H120.52740.37890.76940.069*
C130.59955 (10)0.48487 (19)0.58112 (10)0.0357 (4)
C140.66054 (10)0.48227 (19)0.56414 (10)0.0368 (4)
C150.67532 (11)0.4956 (2)0.50319 (10)0.0393 (5)
H150.71650.49350.49160.047*
C160.63138 (11)0.5121 (2)0.45859 (10)0.0394 (5)
C170.57203 (11)0.5102 (2)0.47650 (11)0.0445 (5)
H170.54160.51940.44650.053*
C180.55488 (11)0.4955 (2)0.53677 (11)0.0448 (5)
C190.70979 (12)0.4623 (3)0.60964 (11)0.0494 (6)
H19A0.70760.37720.62530.074*
H19B0.70500.52100.64320.074*
H19C0.74900.47540.59020.074*
C200.64952 (14)0.5315 (3)0.39335 (11)0.0545 (6)
H20A0.61350.53210.36770.082*
H20B0.67630.46420.38060.082*
H20C0.67060.61110.38940.082*
C210.48908 (13)0.4904 (4)0.55213 (15)0.0800 (12)
H21A0.46750.44430.52050.120*
H21B0.47300.57490.55470.120*
H21C0.48370.44860.59130.120*
N220.58580 (7)0.95625 (15)0.77489 (7)0.0287 (3)
N230.61243 (7)0.95166 (15)0.71863 (7)0.0271 (3)
C240.63397 (8)1.06557 (18)0.70815 (9)0.0302 (4)
C250.62097 (11)1.1421 (2)0.75897 (11)0.0387 (5)
H250.63131.22710.76360.046*
C260.59097 (10)1.0707 (2)0.79975 (10)0.0369 (4)
H260.57641.09610.83830.044*
C270.66972 (8)1.09596 (17)0.65263 (9)0.0303 (4)
C280.73288 (9)1.10644 (18)0.65803 (10)0.0341 (4)
C290.76708 (9)1.1349 (2)0.60707 (11)0.0400 (5)
H290.80961.14070.61110.048*
C300.74144 (11)1.1551 (2)0.55075 (11)0.0419 (5)
C310.67913 (10)1.1464 (2)0.54624 (10)0.0383 (4)
H310.66071.16130.50800.046*
C320.64259 (9)1.11676 (18)0.59568 (10)0.0332 (4)
C330.76537 (10)1.0852 (2)0.71726 (11)0.0432 (5)
H33A0.77140.99600.72340.065*
H33B0.74131.11890.75070.065*
H33C0.80461.12700.71610.065*
C340.77921 (13)1.1854 (3)0.49596 (14)0.0605 (7)
H34A0.80861.24960.50650.091*
H34B0.75321.21560.46330.091*
H34C0.80041.11060.48240.091*
C350.57606 (9)1.1107 (2)0.58448 (10)0.0380 (4)
H35A0.55731.05580.61450.057*
H35B0.56861.07840.54360.057*
H35C0.55881.19410.58800.057*
N360.64347 (7)0.79509 (15)0.59762 (7)0.0271 (3)
C370.60724 (8)0.81419 (18)0.55053 (9)0.0281 (4)
C380.62918 (9)0.8346 (2)0.49242 (9)0.0334 (4)
H380.60300.84580.45870.040*
C390.69119 (10)0.8379 (2)0.48616 (9)0.0379 (4)
H390.70790.85250.44710.045*
C400.72998 (9)0.8205 (2)0.53495 (9)0.0341 (4)
H400.77250.82430.53040.041*
C410.70324 (8)0.79730 (18)0.59060 (9)0.0284 (4)
N420.54568 (7)0.81622 (16)0.56628 (7)0.0289 (3)
N430.53070 (7)0.81183 (15)0.62690 (7)0.0283 (3)
C440.47155 (9)0.83587 (19)0.62977 (9)0.0328 (4)
C450.44863 (10)0.8535 (2)0.57075 (10)0.0414 (5)
H450.40800.87020.56000.050*
C460.49620 (9)0.8421 (2)0.53201 (10)0.0371 (4)
H460.49500.85060.48910.044*
C470.44084 (8)0.84210 (19)0.69011 (9)0.0338 (4)
C480.41819 (10)0.7339 (2)0.71740 (11)0.0392 (5)
C490.39541 (10)0.7422 (3)0.77652 (12)0.0445 (5)
H490.38120.66890.79570.053*
C500.39285 (9)0.8527 (3)0.80795 (10)0.0431 (5)
C510.41233 (10)0.9592 (2)0.77899 (10)0.0405 (5)
H510.40961.03630.79970.049*
C520.43600 (9)0.9571 (2)0.72006 (10)0.0357 (4)
C530.41821 (13)0.6117 (2)0.68511 (15)0.0551 (6)
H53A0.40020.54830.71130.083*
H53B0.45970.58820.67520.083*
H53C0.39470.61860.64760.083*
C540.36921 (14)0.8583 (3)0.87202 (12)0.0610 (7)
H54A0.37930.78120.89330.091*
H54B0.32540.86870.87120.091*
H54C0.38760.92870.89330.091*
C550.45583 (10)1.0768 (2)0.69173 (12)0.0449 (5)
H55A0.43101.14490.70730.067*
H55B0.45121.07150.64760.067*
H55C0.49821.09220.70180.067*
N560.73443 (7)0.77133 (15)0.64470 (8)0.0295 (3)
N570.70228 (7)0.73903 (15)0.69539 (7)0.0286 (3)
C580.74248 (9)0.70686 (19)0.73734 (9)0.0326 (4)
C590.80142 (10)0.7207 (2)0.71390 (11)0.0387 (5)
H590.83820.70520.73460.046*
C600.79488 (10)0.7607 (2)0.65539 (11)0.0367 (4)
H600.82640.77790.62750.044*
C610.72184 (9)0.6618 (2)0.79812 (9)0.0345 (4)
C620.71419 (10)0.5345 (2)0.80860 (11)0.0424 (5)
C630.68995 (11)0.4961 (3)0.86429 (13)0.0517 (6)
H630.68380.41000.87120.062*
C640.67487 (11)0.5793 (3)0.90920 (12)0.0549 (7)
C650.68519 (10)0.7055 (3)0.89887 (11)0.0473 (5)
H650.67590.76370.92990.057*
C660.70876 (10)0.7479 (2)0.84414 (10)0.0386 (5)
C670.73200 (15)0.4374 (2)0.76289 (13)0.0566 (7)
H67A0.69680.41420.73860.085*
H67B0.74740.36410.78410.085*
H67C0.76340.47080.73620.085*
C680.64717 (16)0.5360 (5)0.96787 (17)0.0824 (12)
H68A0.62130.46410.96000.124*
H68B0.62310.60320.98550.124*
H68C0.67910.51250.99630.124*
C690.72065 (12)0.8842 (2)0.83607 (11)0.0439 (5)
H69A0.70370.93000.87050.066*
H69B0.70180.91290.79840.066*
H69C0.76420.89860.83410.066*
N700.51919 (13)0.75660 (19)0.36134 (10)0.0542 (6)
O710.52663 (9)0.85955 (16)0.38760 (8)0.0525 (4)
O720.55433 (14)0.7221 (3)0.32174 (13)0.0835 (8)
O730.47400 (13)0.6926 (2)0.37436 (11)0.0805 (8)
N74A0.5923 (2)0.8629 (6)1.0099 (3)0.0338 (14)*0.40
O75A0.6257 (2)0.9362 (5)0.9804 (2)0.0557 (12)*0.40
O76A0.6165 (2)0.7954 (6)1.0479 (3)0.0628 (13)*0.40
O77A0.5372 (2)0.8588 (7)0.9998 (3)0.0338 (13)*0.40
N74B0.5933 (2)0.8979 (5)1.0041 (2)0.0318 (12)*0.40
O75B0.6296 (3)0.8728 (7)1.0473 (3)0.0668 (15)*0.40
O76B0.5439 (3)0.8336 (6)1.0060 (3)0.059 (2)*0.40
O77B0.6062 (2)0.9703 (5)0.9640 (2)0.0522 (11)*0.40
N74C0.5882 (5)0.8510 (12)1.0266 (6)0.059 (4)*0.20
O75C0.5813 (7)0.7676 (13)1.0650 (7)0.103 (5)*0.20
O76C0.6370 (4)0.9143 (12)1.0287 (6)0.072 (3)*0.20
O77C0.5447 (4)0.8923 (10)0.9950 (5)0.045 (3)*0.20
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02629 (11)0.02474 (12)0.02291 (11)0.00012 (8)0.00073 (10)0.00009 (11)
N20.0291 (7)0.0279 (8)0.0271 (8)0.0006 (6)0.0020 (6)0.0001 (6)
C30.0336 (9)0.0282 (9)0.0286 (9)0.0027 (7)0.0024 (7)0.0009 (7)
C40.0412 (10)0.0344 (10)0.0299 (9)0.0018 (8)0.0054 (8)0.0036 (8)
C50.0362 (10)0.0429 (11)0.0280 (9)0.0020 (8)0.0038 (8)0.0012 (8)
C60.0329 (9)0.0361 (10)0.0302 (9)0.0039 (8)0.0004 (8)0.0037 (8)
C70.0273 (8)0.0287 (9)0.0285 (9)0.0026 (7)0.0007 (7)0.0020 (7)
N80.0452 (9)0.0267 (8)0.0315 (8)0.0009 (7)0.0093 (7)0.0019 (6)
N90.0349 (7)0.0286 (7)0.0257 (7)0.0014 (6)0.0024 (8)0.0007 (7)
C100.0554 (13)0.0289 (10)0.0384 (11)0.0019 (9)0.0104 (10)0.0033 (8)
C110.109 (2)0.0281 (10)0.0545 (14)0.0149 (12)0.0323 (17)0.0090 (12)
C120.095 (2)0.0263 (10)0.0517 (14)0.0101 (12)0.0278 (14)0.0012 (10)
C130.0481 (11)0.0265 (9)0.0324 (10)0.0038 (8)0.0058 (8)0.0076 (8)
C140.0457 (11)0.0287 (9)0.0360 (10)0.0048 (8)0.0012 (9)0.0033 (8)
C150.0447 (11)0.0388 (11)0.0343 (10)0.0040 (9)0.0050 (9)0.0032 (9)
C160.0482 (12)0.0375 (11)0.0326 (10)0.0017 (9)0.0005 (9)0.0059 (8)
C170.0437 (12)0.0506 (13)0.0392 (11)0.0035 (10)0.0051 (10)0.0152 (10)
C180.0432 (11)0.0480 (12)0.0433 (12)0.0074 (10)0.0047 (10)0.0186 (10)
C190.0578 (14)0.0523 (14)0.0380 (12)0.0164 (11)0.0055 (11)0.0021 (10)
C200.0627 (16)0.0663 (17)0.0345 (12)0.0000 (13)0.0008 (11)0.0026 (12)
C210.0423 (14)0.141 (3)0.0571 (18)0.0179 (17)0.0059 (13)0.038 (2)
N220.0298 (7)0.0269 (8)0.0294 (8)0.0001 (6)0.0013 (6)0.0050 (6)
N230.0270 (7)0.0273 (8)0.0270 (7)0.0006 (6)0.0007 (6)0.0005 (6)
C240.0278 (8)0.0263 (9)0.0365 (9)0.0011 (7)0.0045 (8)0.0006 (7)
C250.0429 (11)0.0282 (10)0.0449 (12)0.0038 (8)0.0012 (9)0.0072 (8)
C260.0416 (10)0.0299 (10)0.0391 (11)0.0007 (8)0.0008 (9)0.0105 (8)
C270.0295 (9)0.0233 (8)0.0381 (10)0.0018 (7)0.0029 (8)0.0027 (7)
C280.0313 (9)0.0281 (9)0.0431 (10)0.0020 (7)0.0024 (8)0.0033 (8)
C290.0324 (9)0.0375 (11)0.0501 (12)0.0019 (8)0.0033 (9)0.0066 (9)
C300.0424 (11)0.0378 (11)0.0453 (12)0.0016 (9)0.0056 (9)0.0058 (9)
C310.0442 (11)0.0353 (10)0.0355 (10)0.0002 (8)0.0040 (9)0.0019 (8)
C320.0354 (9)0.0251 (9)0.0390 (10)0.0003 (7)0.0034 (8)0.0007 (8)
C330.0337 (10)0.0476 (13)0.0483 (13)0.0045 (9)0.0074 (9)0.0071 (10)
C340.0551 (15)0.0708 (18)0.0557 (16)0.0037 (14)0.0114 (12)0.0155 (14)
C350.0353 (10)0.0352 (10)0.0434 (11)0.0008 (8)0.0068 (9)0.0011 (9)
N360.0284 (7)0.0269 (7)0.0259 (7)0.0010 (6)0.0014 (6)0.0007 (6)
C370.0299 (9)0.0258 (9)0.0285 (9)0.0012 (7)0.0005 (7)0.0034 (7)
C380.0370 (10)0.0368 (10)0.0264 (9)0.0023 (8)0.0010 (8)0.0002 (7)
C390.0421 (11)0.0421 (11)0.0295 (9)0.0019 (9)0.0060 (8)0.0014 (8)
C400.0335 (9)0.0375 (11)0.0311 (9)0.0022 (8)0.0059 (8)0.0030 (8)
C410.0287 (8)0.0278 (8)0.0286 (9)0.0001 (7)0.0004 (7)0.0022 (7)
N420.0302 (8)0.0332 (8)0.0234 (7)0.0034 (6)0.0008 (6)0.0009 (6)
N430.0284 (7)0.0308 (8)0.0255 (8)0.0010 (6)0.0015 (6)0.0003 (6)
C440.0271 (8)0.0374 (10)0.0338 (10)0.0013 (7)0.0010 (7)0.0024 (8)
C450.0290 (9)0.0586 (14)0.0365 (11)0.0037 (9)0.0051 (8)0.0063 (10)
C460.0329 (9)0.0489 (12)0.0294 (9)0.0055 (8)0.0056 (8)0.0027 (8)
C470.0250 (8)0.0426 (10)0.0338 (11)0.0027 (7)0.0005 (7)0.0042 (8)
C480.0331 (10)0.0442 (12)0.0402 (12)0.0001 (8)0.0047 (9)0.0058 (9)
C490.0394 (12)0.0526 (14)0.0415 (13)0.0050 (9)0.0076 (9)0.0114 (10)
C500.0336 (10)0.0638 (15)0.0319 (11)0.0069 (9)0.0034 (8)0.0032 (10)
C510.0325 (9)0.0509 (12)0.0380 (11)0.0055 (9)0.0006 (9)0.0029 (9)
C520.0268 (9)0.0440 (11)0.0365 (10)0.0041 (8)0.0006 (8)0.0033 (8)
C530.0643 (14)0.0455 (12)0.0554 (14)0.0077 (10)0.0173 (14)0.0002 (13)
C540.0595 (16)0.085 (2)0.0383 (13)0.0085 (14)0.0121 (12)0.0059 (13)
C550.0412 (10)0.0410 (11)0.0527 (15)0.0030 (9)0.0073 (10)0.0027 (10)
N560.0267 (7)0.0324 (8)0.0294 (8)0.0008 (6)0.0020 (6)0.0018 (6)
N570.0281 (7)0.0298 (8)0.0281 (9)0.0012 (6)0.0004 (6)0.0017 (6)
C580.0321 (9)0.0325 (9)0.0331 (10)0.0016 (8)0.0047 (8)0.0027 (8)
C590.0270 (9)0.0473 (13)0.0417 (12)0.0025 (8)0.0017 (8)0.0053 (9)
C600.0278 (9)0.0417 (11)0.0405 (11)0.0003 (8)0.0028 (9)0.0037 (9)
C610.0283 (9)0.0421 (11)0.0331 (10)0.0002 (8)0.0035 (8)0.0078 (8)
C620.0380 (10)0.0453 (12)0.0438 (12)0.0038 (9)0.0105 (9)0.0127 (9)
C630.0418 (12)0.0587 (15)0.0547 (14)0.0043 (11)0.0050 (11)0.0256 (13)
C640.0352 (11)0.0808 (19)0.0487 (14)0.0067 (11)0.0058 (10)0.0276 (13)
C650.0326 (10)0.0742 (16)0.0350 (11)0.0104 (11)0.0017 (9)0.0061 (11)
C660.0301 (10)0.0525 (12)0.0331 (10)0.0045 (9)0.0047 (8)0.0056 (9)
C670.0810 (19)0.0390 (13)0.0499 (14)0.0063 (12)0.0112 (14)0.0063 (11)
C680.0573 (17)0.119 (3)0.071 (2)0.0193 (19)0.0248 (16)0.048 (2)
C690.0479 (12)0.0469 (12)0.0368 (11)0.0053 (10)0.0082 (10)0.0035 (10)
N700.0860 (17)0.0379 (11)0.0387 (11)0.0078 (10)0.0246 (12)0.0001 (8)
O710.0796 (13)0.0426 (9)0.0351 (8)0.0100 (8)0.0165 (8)0.0031 (7)
O720.0990 (19)0.0764 (16)0.0753 (16)0.0301 (14)0.0128 (14)0.0190 (13)
O730.126 (2)0.0449 (11)0.0709 (15)0.0322 (13)0.0262 (14)0.0072 (10)
Geometric parameters (Å, º) top
Co1—N22.0199 (17)C37—N421.410 (2)
Co1—N92.1177 (15)C38—C391.384 (3)
Co1—N232.1320 (17)C38—H380.9500
Co1—N362.0206 (16)C39—C401.390 (3)
Co1—N432.1279 (16)C39—H390.9500
Co1—N572.1538 (16)C40—C411.385 (3)
N2—C71.331 (3)C40—H400.9500
N2—C31.333 (2)C41—N561.407 (3)
C3—C41.386 (3)N42—C461.362 (3)
C3—N81.412 (3)N42—N431.377 (2)
C4—C51.388 (3)N43—C441.340 (2)
C4—H40.9500C44—C451.410 (3)
C5—C61.390 (3)C44—C471.496 (3)
C5—H50.9500C45—C461.363 (3)
C6—C71.380 (3)C45—H450.9500
C6—H60.9500C46—H460.9500
C7—N221.418 (3)C47—C481.405 (3)
N8—C121.355 (3)C47—C521.408 (3)
N8—N91.373 (2)C48—C491.400 (4)
N9—C101.330 (3)C48—C531.497 (3)
C10—C111.408 (3)C49—C501.379 (4)
C10—C131.504 (3)C49—H490.9500
C11—C121.359 (4)C50—C511.382 (4)
C11—H110.9500C50—C541.508 (3)
C12—H120.9500C51—C521.401 (3)
C13—C181.397 (3)C51—H510.9500
C13—C141.405 (3)C52—C551.499 (3)
C14—C151.390 (3)C53—H53A0.9800
C14—C191.499 (3)C53—H53B0.9800
C15—C161.396 (3)C53—H53C0.9800
C15—H150.9500C54—H54A0.9800
C16—C171.375 (3)C54—H54B0.9800
C16—C201.508 (3)C54—H54C0.9800
C17—C181.391 (3)C55—H55A0.9800
C17—H170.9500C55—H55B0.9800
C18—C211.500 (4)C55—H55C0.9800
C19—H19A0.9800N56—C601.367 (3)
C19—H19B0.9800N56—N571.370 (2)
C19—H19C0.9800N57—C581.331 (3)
C20—H20A0.9800C58—C591.415 (3)
C20—H20B0.9800C58—C611.496 (3)
C20—H20C0.9800C59—C601.367 (3)
C21—H21A0.9800C59—H590.9500
C21—H21B0.9800C60—H600.9500
C21—H21C0.9800C61—C621.402 (3)
N22—C261.354 (3)C61—C661.404 (3)
N22—N231.374 (2)C62—C631.403 (4)
N23—C241.337 (2)C62—C671.505 (4)
C24—C251.420 (3)C63—C641.377 (4)
C24—C271.495 (3)C63—H630.9500
C25—C261.358 (3)C64—C651.398 (4)
C25—H250.9500C64—C681.506 (4)
C26—H260.9500C65—C661.392 (3)
C27—C321.410 (3)C65—H650.9500
C27—C281.411 (3)C66—C691.503 (3)
C28—C291.390 (3)C67—H67A0.9800
C28—C331.509 (3)C67—H67B0.9800
C29—C301.383 (3)C67—H67C0.9800
C29—H290.9500C68—H68A0.9800
C30—C311.390 (3)C68—H68B0.9800
C30—C341.505 (4)C68—H68C0.9800
C31—C321.395 (3)C69—H69A0.9800
C31—H310.9500C69—H69B0.9800
C32—C351.499 (3)C69—H69C0.9800
C33—H33A0.9800N70—O721.228 (4)
C33—H33B0.9800N70—O731.250 (4)
C33—H33C0.9800N70—O711.262 (3)
C34—H34A0.9800N74A—O76A1.231 (7)
C34—H34B0.9800N74A—O77A1.243 (6)
C34—H34C0.9800N74A—O75A1.265 (7)
C35—H35A0.9800N74B—O77B1.213 (6)
C35—H35B0.9800N74B—O75B1.275 (6)
C35—H35C0.9800N74B—O76B1.299 (6)
N36—C371.329 (3)N74C—O75C1.243 (9)
N36—C411.336 (2)N74C—O77C1.271 (8)
C37—C381.388 (3)N74C—O76C1.281 (9)
N2—Co1—N977.41 (7)H35B—C35—H35C109.5
N2—Co1—N2376.99 (6)C37—N36—C41120.53 (17)
N2—Co1—N36179.02 (7)C37—N36—Co1119.41 (12)
N2—Co1—N43102.41 (6)C41—N36—Co1120.02 (13)
N2—Co1—N57103.68 (6)N36—C37—C38122.18 (17)
N9—Co1—N23154.39 (6)N36—C37—N42113.38 (17)
N9—Co1—N36103.52 (7)C38—C37—N42124.40 (18)
N9—Co1—N4392.04 (6)C39—C38—C37116.43 (18)
N9—Co1—N5793.88 (6)C39—C38—H38121.8
N23—Co1—N36102.09 (6)C37—C38—H38121.8
N23—Co1—N4393.63 (6)C38—C39—C40122.39 (19)
N23—Co1—N5791.91 (6)C38—C39—H39118.8
N36—Co1—N4377.27 (6)C40—C39—H39118.8
N36—Co1—N5776.64 (6)C41—C40—C39116.33 (18)
N43—Co1—N57153.91 (6)C41—C40—H40121.8
C7—N2—C3119.77 (17)C39—C40—H40121.8
C7—N2—Co1120.46 (13)N36—C41—C40122.10 (18)
C3—N2—Co1119.75 (13)N36—C41—N56112.77 (16)
N2—C3—C4122.76 (18)C40—C41—N56125.12 (17)
N2—C3—N8112.43 (17)C46—N42—N43110.49 (16)
C4—C3—N8124.79 (18)C46—N42—C37130.41 (17)
C3—C4—C5116.13 (19)N43—N42—C37118.18 (15)
C3—C4—H4121.9C44—N43—N42106.01 (15)
C5—C4—H4121.9C44—N43—Co1143.10 (14)
C4—C5—C6122.10 (19)N42—N43—Co1110.88 (11)
C4—C5—H5118.9N43—C44—C45109.65 (18)
C6—C5—H5118.9N43—C44—C47119.82 (17)
C7—C6—C5116.49 (19)C45—C44—C47130.52 (18)
C7—C6—H6121.8C46—C45—C44106.62 (18)
C5—C6—H6121.8C46—C45—H45126.7
N2—C7—C6122.72 (18)C44—C45—H45126.7
N2—C7—N22112.33 (17)N42—C46—C45107.22 (19)
C6—C7—N22124.94 (18)N42—C46—H46126.4
C12—N8—N9110.87 (18)C45—C46—H46126.4
C12—N8—C3129.39 (19)C48—C47—C52120.16 (19)
N9—N8—C3119.09 (15)C48—C47—C44120.42 (19)
C10—N9—N8106.03 (16)C52—C47—C44119.40 (18)
C10—N9—Co1142.52 (15)C49—C48—C47118.3 (2)
N8—N9—Co1111.15 (12)C49—C48—C53119.9 (2)
N9—C10—C11109.4 (2)C47—C48—C53121.8 (2)
N9—C10—C13120.74 (19)C50—C49—C48122.5 (2)
C11—C10—C13129.7 (2)C50—C49—H49118.7
C12—C11—C10106.9 (2)C48—C49—H49118.7
C12—C11—H11126.5C49—C50—C51118.2 (2)
C10—C11—H11126.5C49—C50—C54121.3 (3)
N8—C12—C11106.8 (2)C51—C50—C54120.5 (3)
N8—C12—H12126.6C50—C51—C52122.1 (2)
C11—C12—H12126.6C50—C51—H51118.9
C18—C13—C14120.0 (2)C52—C51—H51118.9
C18—C13—C10119.5 (2)C51—C52—C47118.5 (2)
C14—C13—C10120.6 (2)C51—C52—C55118.8 (2)
C15—C14—C13118.9 (2)C47—C52—C55122.65 (19)
C15—C14—C19119.3 (2)C48—C53—H53A109.5
C13—C14—C19121.8 (2)C48—C53—H53B109.5
C14—C15—C16121.9 (2)H53A—C53—H53B109.5
C14—C15—H15119.0C48—C53—H53C109.5
C16—C15—H15119.0H53A—C53—H53C109.5
C17—C16—C15117.7 (2)H53B—C53—H53C109.5
C17—C16—C20122.1 (2)C50—C54—H54A109.5
C15—C16—C20120.2 (2)C50—C54—H54B109.5
C16—C17—C18122.6 (2)H54A—C54—H54B109.5
C16—C17—H17118.7C50—C54—H54C109.5
C18—C17—H17118.7H54A—C54—H54C109.5
C17—C18—C13118.9 (2)H54B—C54—H54C109.5
C17—C18—C21119.1 (2)C52—C55—H55A109.5
C13—C18—C21122.0 (2)C52—C55—H55B109.5
C14—C19—H19A109.5H55A—C55—H55B109.5
C14—C19—H19B109.5C52—C55—H55C109.5
H19A—C19—H19B109.5H55A—C55—H55C109.5
C14—C19—H19C109.5H55B—C55—H55C109.5
H19A—C19—H19C109.5C60—N56—N57110.45 (16)
H19B—C19—H19C109.5C60—N56—C41130.22 (18)
C16—C20—H20A109.5N57—N56—C41119.01 (15)
C16—C20—H20B109.5C58—N57—N56106.45 (16)
H20A—C20—H20B109.5C58—N57—Co1142.93 (14)
C16—C20—H20C109.5N56—N57—Co1110.44 (11)
H20A—C20—H20C109.5N57—C58—C59109.82 (18)
H20B—C20—H20C109.5N57—C58—C61120.07 (17)
C18—C21—H21A109.5C59—C58—C61130.10 (18)
C18—C21—H21B109.5C60—C59—C58106.22 (19)
H21A—C21—H21B109.5C60—C59—H59126.9
C18—C21—H21C109.5C58—C59—H59126.9
H21A—C21—H21C109.5N56—C60—C59107.05 (19)
H21B—C21—H21C109.5N56—C60—H60126.5
C26—N22—N23111.18 (17)C59—C60—H60126.5
C26—N22—C7129.54 (17)C62—C61—C66120.2 (2)
N23—N22—C7118.74 (15)C62—C61—C58120.1 (2)
C24—N23—N22106.05 (15)C66—C61—C58119.71 (19)
C24—N23—Co1142.66 (14)C61—C62—C63118.7 (2)
N22—N23—Co1111.25 (11)C61—C62—C67122.6 (2)
N23—C24—C25108.91 (18)C63—C62—C67118.7 (2)
N23—C24—C27122.15 (17)C64—C63—C62122.0 (3)
C25—C24—C27128.77 (18)C64—C63—H63119.0
C26—C25—C24107.00 (19)C62—C63—H63119.0
C26—C25—H25126.5C63—C64—C65118.5 (2)
C24—C25—H25126.5C63—C64—C68120.9 (3)
N22—C26—C25106.85 (19)C65—C64—C68120.6 (3)
N22—C26—H26126.6C66—C65—C64121.5 (3)
C25—C26—H26126.6C66—C65—H65119.3
C32—C27—C28119.12 (19)C64—C65—H65119.3
C32—C27—C24122.45 (16)C65—C66—C61119.1 (2)
C28—C27—C24118.42 (18)C65—C66—C69119.3 (2)
C29—C28—C27119.5 (2)C61—C66—C69121.6 (2)
C29—C28—C33118.12 (18)C62—C67—H67A109.5
C27—C28—C33122.39 (19)C62—C67—H67B109.5
C30—C29—C28122.36 (19)H67A—C67—H67B109.5
C30—C29—H29118.8C62—C67—H67C109.5
C28—C29—H29118.8H67A—C67—H67C109.5
C29—C30—C31117.6 (2)H67B—C67—H67C109.5
C29—C30—C34121.7 (2)C64—C68—H68A109.5
C31—C30—C34120.8 (2)C64—C68—H68B109.5
C30—C31—C32122.5 (2)H68A—C68—H68B109.5
C30—C31—H31118.7C64—C68—H68C109.5
C32—C31—H31118.7H68A—C68—H68C109.5
C31—C32—C27118.89 (18)H68B—C68—H68C109.5
C31—C32—C35117.01 (19)C66—C69—H69A109.5
C27—C32—C35124.10 (19)C66—C69—H69B109.5
C28—C33—H33A109.5H69A—C69—H69B109.5
C28—C33—H33B109.5C66—C69—H69C109.5
H33A—C33—H33B109.5H69A—C69—H69C109.5
C28—C33—H33C109.5H69B—C69—H69C109.5
H33A—C33—H33C109.5O72—N70—O73120.4 (3)
H33B—C33—H33C109.5O72—N70—O71120.6 (3)
C30—C34—H34A109.5O73—N70—O71119.0 (3)
C30—C34—H34B109.5O76A—N74A—O77A122.1 (7)
H34A—C34—H34B109.5O76A—N74A—O75A117.5 (5)
C30—C34—H34C109.5O77A—N74A—O75A120.4 (6)
H34A—C34—H34C109.5O77B—N74B—O75B122.2 (5)
H34B—C34—H34C109.5O77B—N74B—O76B124.3 (5)
C32—C35—H35A109.5O75B—N74B—O76B113.4 (6)
C32—C35—H35B109.5O75C—N74C—O77C122.2 (9)
H35A—C35—H35B109.5O75C—N74C—O76C117.7 (9)
C32—C35—H35C109.5O77C—N74C—O76C118.3 (9)
H35A—C35—H35C109.5

Experimental details

(I)(II)
Crystal data
Chemical formula[Co(C29H29N5)2](NO3)2[Co(C29H29N5)2](NO3)2
Mr1078.091078.09
Crystal system, space groupOrthorhombic, Pca21Orthorhombic, Pca21
Temperature (K)290150
a, b, c (Å)22.3350 (1), 10.9094 (2), 22.1061 (2)22.1974 (2), 10.7761 (1), 22.0365 (1)
V3)5386.40 (11)5271.16 (7)
Z44
Radiation typeMo KαMo Kα
µ (mm1)0.380.39
Crystal size (mm)0.45 × 0.35 × 0.280.45 × 0.35 × 0.28
Data collection
DiffractometerNonius KappaCCD area-detector
diffractometer
Nonius KappaCCD area-detector
diffractometer
Absorption correctionMulti-scan
(SORTAV; Blessing, 1995)
Multi-scan
(SORTAV; Blessing, 1995)
Tmin, Tmax0.847, 0.9010.844, 0.899
No. of measured, independent and
observed [I > 2σ(I)] reflections
59607, 11975, 10665 86435, 11941, 11339
Rint0.0460.052
(sin θ/λ)max1)0.6500.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.104, 1.04 0.037, 0.099, 1.06
No. of reflections1197511941
No. of parameters721720
No. of restraints2120
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.26, 0.280.68, 0.35
Absolute structureFlack (1983)Flack, 1983
Absolute structure parameter0.004 (9)0.001 (8)

Computer programs: COLLECT (Nonius, 1999), DENZO-SMN (Otwinowski & Minor, 1997), DENZO-SMN, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEX (McArdle, 1995), local program.

Selected geometric parameters (Å, º) for (I) top
Co1—N22.0132 (18)Co1—N362.0077 (17)
Co1—N92.1190 (15)Co1—N432.1327 (17)
Co1—N232.1368 (17)Co1—N572.1581 (16)
N2—Co1—N977.42 (7)N9—Co1—N5793.44 (6)
N2—Co1—N2377.03 (7)N23—Co1—N36102.20 (7)
N2—Co1—N36179.08 (7)N23—Co1—N4393.34 (6)
N2—Co1—N43102.21 (7)N23—Co1—N5792.54 (6)
N2—Co1—N57103.69 (7)N36—Co1—N4377.29 (7)
N9—Co1—N36103.34 (7)N36—Co1—N5776.81 (6)
N9—Co1—N23154.45 (7)N43—Co1—N57154.10 (6)
N9—Co1—N4392.04 (7)
Selected geometric parameters (Å, º) for (II) top
Co1—N22.0199 (17)Co1—N362.0206 (16)
Co1—N92.1177 (15)Co1—N432.1279 (16)
Co1—N232.1320 (17)Co1—N572.1538 (16)
N2—Co1—N977.41 (7)N9—Co1—N5793.88 (6)
N2—Co1—N2376.99 (6)N23—Co1—N36102.09 (6)
N2—Co1—N36179.02 (7)N23—Co1—N4393.63 (6)
N2—Co1—N43102.41 (6)N23—Co1—N5791.91 (6)
N2—Co1—N57103.68 (6)N36—Co1—N4377.27 (6)
N9—Co1—N23154.39 (6)N36—Co1—N5776.64 (6)
N9—Co1—N36103.52 (7)N43—Co1—N57153.91 (6)
N9—Co1—N4392.04 (6)
 

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