research communications
Trinuclear nickel coordination complexes of phenanthrene-9,10-dione dioxime
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*Correspondence e-mail: acowley@cm.utexas.edu
A trinuclear nickel complex of phenanthrene-9,10-dione dioxime (H2pqd), namely bis[μ2-9,10-bis(oxidoimino)phenanthrene]bis[μ2-10-(oxidoimino)phenanthrene-9-one oxime](phenanthrene-9,10-dione dioxime)trinickel(II) toluene disolvate, [Ni3(C14H8N2O2)2(C14H9N2O2)2(C14H10N2O2)]·2C7H8, has been isolated and its determined. This complex features three independent NiII atoms that are arranged in a triangular fashion along with five supporting ligands. There are two square-planar NiII atoms and a third pseudo-octahedral NiII atom. While the square-planar NiII atoms are stacked, there are no ligand bridges between them. Each square-planar NiII atom, however, bridges with the pseudo-octahedral NiII atom through Ni—N—O—Ni and Ni—O—Ni bonds. A fluoridoboration reaction of the proton-bridged species gave the analogous complex bis(μ2-bis{[10-(oxidoimino)-9,10-dihydrophenanthren-9-ylidene]amino}difluoridoborato)(phenanthrene-9,10-dione dioxime)trinickel(II) dichloromethane trisolvate, [Ni3(C28H16BF2N4O2)4(C14H10N2O2)]·3CH2Cl2, which shows the same binding structure, but features a widened Ni—Ni interaction between the square-planar NiII atoms. The proton-bridged complex completes the macrocyclic coordination around the square-planar NiII atoms by means of an O—H⋯O hydrogen bond. Both compounds feature O—H⋯N hydrogen bonds between the oxime and the N atoms attached to square-planar nickel atom. The nickel units show no direct interaction with their nearest neighbors in the extended lattice. Two π-stacking interactions between adjacent molecules are found: one with a centroid–centroid distance of 3.886 (2) Å and the other with a centroid–centroid distance of 4.256 (3) Å. In the latter case, although not aromatic, the distance to the centroid of the central phenanthrene ring is shorter, with a distance of 3.528 (3) Å. Toluene molecules occupy the solvent channels that are oriented along the c axis. In the fluoridoboronate structure, the solvent (DCM) was too badly disordered to be modelled, so its contribution was removed using SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18].
Keywords: crystal structure; nickel; H2pqd; α–β dioxime; trinuclear; hydrogen bonding.
1. Chemical context
Oxime functional groups can coordinate to transition metal ions in a variety of ways, due to the presence of both nitrogen and oxygen donors. On account of the multitude of possible coordinations, these ligands, and particularly α–β dioximes, have the capability of forming bridging multinuclear complexes with many transition metals, including nickel (Chaudhuri, 2003). From the standpoint of single-molecule magnets, these multi-nuclear complexes play an important role due to their ability to facilitate spin-frustration in magnetic transition-metal clusters (Aromí & Brechin, 2006). Other nickel polynuclear compounds supported by oxime ligands have been reported (Jiang et al., 2005; Biswas et al., 2009).
Phenanthrenequinone dioxime (pqdH2) is an α–β dioxime ligand that incorporates a constrained ring system. Similar to other dioximes, however, it exists as three separate (E–E, E–Z, and Z–Z), as confirmed by – Interestingly, although this compound was synthesized over 100 years ago (Schmidt & Söll, 1907), no coordination complexes of this ligand have been structurally characterized to date.
2. Structural commentary
Fig. 1 shows the structure of [Ni3(H2pqd)(Hpqd)2(pqd)2], (1). This complex consists of three NiII atoms in a triangular arrangement, two of which are in a square-planar coordination environment, while the third is in a pseudo-octahedral coordination environment. The square-planar NiII atoms (Ni1 and Ni2) consist of one N,N-coordinating and one N,O-coordinating ligand. These ligands form bridges with the pseudo-octahedral NiII atom (Ni3) by means of their oxime O atoms. This arrangement permits the formation of Ni—N—O—Ni and Ni—O—Ni bridges between each square-planar NiII atom and the pseudo-octahedral NiII atom.
The structural features of the core ligation sphere warrant special attention. The Nisp—Nisp distance is 3.3657 (9) Å, a distance that precludes the presence of any metal–metal bonding. However, the distances between each of these nickel moieties and the pseudo-octahedral NiII atom are nearly identical [Nisp—Nioct = 3.2697 (7), 3.2674 (7) Å]. The pseudo-octahedral nickel geometry deviates significantly from a perfect octahedral symmetry [O2—Ni3—O8 = 160.00 (9), O4—Ni3—N10 = 164.8 (1), N9—Ni3—O6 = 165.5 (1)°].
Fig. 2 shows the complete coordination geometry of the compound [Ni3(pqdH2)(pqdBF2)2(pqd)2], (2). The physical arrangement of the ligation sphere directly mimics that of (1). In this case, however, the steric bulk of the BF2 groups forces an expansion of the stacked square-planar nickel units, resulting in an Nisp—Nisp distance of 3.592 (1) Å. The distances between these units and the pseudo-octahedral NiII atom, however, remain similar [Nisp—Nioct = 3.274 (1), 3.255 (1) Å]. Overall, the entire structure retains all the other structural features that are present in the proton-bridged compound.
The phenanthrene backbones show pronounced twisting between their aromatic rings, which precludes conjugation across this unit. For the proton-bridged complex, the angle between mean planes within a single phenanthrene backbone ranges from 9.24 (19)° (between C45–C50 and C51–C56) to 15.44 (13)° (between C59–C64 and C65–C70). For the BF2-bridged complex, there is a wider range of angles, with 5.2 (4)° (between C31–C36 and C37–C42) being the smallest, and 17.5 (3)° (between C59–C64 and C65–C70) being the largest.
3. Supramolecular features
The proton-bridged complex completes the macrocyclic coordination around the square-planar NiII atoms by means of hydrogen bonds. Furthermore, the ligand that coordinates the pseudo-octahedral NiII atom features hydrogen-bonding interactions (Table 1) between the oxime hydroxy groups and the ligands of the square-planar NiII atoms. The nickel units show no direct interaction with their nearest neighbors in the extended lattice. Some π-stacking between adjacent molecules is, however, evident (Fig. 3). Two interactions were found, one with a centroid–centroid distance of 3.886 (2) Å (symmetry code: 1 − x, − + y, − z) and the other with a centroid–centroid distance of 4.256 (3) Å (symmetry code: −x, −y, 2 − z). In the latter case, although not aromatic, the distance to the centroid of the central ring of phenanthrene is shorter, with a distance of 3.528 (3) Å. Toluene molecules occupy the solvent channels that are oriented along the c axis.
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The BF2-bridged complex completes the macrocyclic coordination around the square-planar NiII atoms by means of covalent O—B—O bonds. However, the hydrogen-bonding interactions (Table 2) that lock the pseudo-octahedral NiII atom remain in place. The nickel units show no direct interaction with their nearest neighbors in the extended lattice. A solvent channel oriented along the c axis is also evident (Fig. 4). However, the extreme disorder of the solvent does not permit the determination of a suitable model.
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4. Synthesis and crystallization
The parent ligand, pqdH2 (0.75 g; 3.1 mmol), was dissolved in 100 ml of ethanol, to which nickel(II) acetate (0.33 g, 1.3 mmol) was added. A red precipitate began to form after approximately 30 min. The solution was then allowed to stir for 1 h, followed by cooling in a freezer and filtration of the crude product (yield: 272 mg, 0.2 mmol, 32%). The resulting product was dissolved in DMF solution and layered with toluene, resulting in the formation of crystals of [Ni3(H2pqd)(Hpqd)2(pqd)2] after a period of 3–4 d. The crystals grew as red blocks with an consisting of a complete [Ni3(H2pqd)(Hpqd)2(pqd)2] molecule and two toluene solvent molecules.
The foregoing complex is stable enough to undergo a fluoridoboration reaction with boron trifluoride, thereby affording the compound [Ni3(H2pqd)(BF2pqd)2(pqd)2]. [Ni3(H2pqd)(Hpqd)2(pqd)2] was diluted in diethyl ether, thereby creating a slurry. One ml of 1.0 molar BF3–OEt2 (in ether) was then added and the mixture was allowed to react overnight. The resulting precipitate was then filtered off and washed thoroughly with EtOH and Et2O. The resulting precipitate was then dissolved in dichloromethane (DCM) and filtered through Celite (yield: 43 mg, 30 µmol, 79%). Subsequently, a crop of red block-shaped crystals was grown by solvent evaporation over a period of one day.
5. Refinement
Crystal data, data collection and structure . In proton-bridged structure (1), atoms H1A, H2A and H4A were found by assignment of difference map peaks and refined isotropically without geometrical constraints. The proton H3A was initially placed with the SHELXL HFIX 147 command (refinement on rotation) on O9, but was refined freely. Four distinct hydrogen-bonding interactions were evident in the trinuclear cluster. Finally, there were two O—H—O interactions between an oxime and oximato of each [Ni(Hpqd)(pqd)]− unit that could not be resolved due to rapid conversion to [Ni(pqd)(Hpqd)]−. All the restraints that are reported were included for the modelling of the disordered toluene solvent molecules.
details are summarized in Table 3In the case of BF2-bridged structure (2), atoms H1A and H2A were affixed to O9 and O10, respectively. They were then refined isotropically without rotational constraints. The SQUEEZE routine (Spek, 2015) as implemented in PLATON (Spek, 2009) was used to remove the electron density of three solvent DCM molecules per (calculated: 134 e−; 593 Å3).
Supporting information
https://doi.org/10.1107/S2056989016004023/pk2575sup1.cif
contains datablocks global, 1, 2. DOI:Structure factors: contains datablock 1. DOI: https://doi.org/10.1107/S2056989016004023/pk25751sup3.hkl
Structure factors: contains datablock 2. DOI: https://doi.org/10.1107/S2056989016004023/pk25752sup2.hkl
Data collection: CrystalClear (Rigaku Inc, 2008) for (1); CrysAlis PRO (Agilent, 2014) for (2). Cell
CrystalClear (Rigaku Inc, 2008) for (1); CrysAlis PRO (Agilent, 2014) for (2). Data reduction: CrystalClear (Rigaku Inc, 2008) for (1); CrysAlis PRO (Agilent, 2014) for (2). Program(s) used to solve structure: SIR2004 (Burla et al., 2005) for (1); OLEX2 (Dolomanov et al., 2009) for (2). For both compounds, program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: Mercury (Macrae et al., 2006); software used to prepare material for publication: publCIF (Westrip, 2010) and WinGX (Farrugia, 1999).[Ni3(C14H8N2O2)2(C14H9N2O2)2(C14H10N2O2)]·2C7H8 | F(000) = 3192 |
Mr = 1545.55 | Dx = 1.546 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71069 Å |
a = 15.973 (3) Å | Cell parameters from 20424 reflections |
b = 18.639 (3) Å | θ = 1.3–31.1° |
c = 22.785 (4) Å | µ = 0.92 mm−1 |
β = 101.757 (4)° | T = 100 K |
V = 6641.1 (19) Å3 | Block, red |
Z = 4 | 0.16 × 0.11 × 0.11 mm |
Rigaku Saturn724+ (2x2 bin mode) diffractometer | 15260 independent reflections |
Radiation source: Sealed Tube | 13993 reflections with I > 2σ(I) |
Detector resolution: 28.5714 pixels mm-1 | Rint = 0.054 |
dtprofit.ref scans | θmax = 27.5°, θmin = 1.8° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −20→20 |
Tmin = 0.799, Tmax = 1.000 | k = −24→24 |
79592 measured reflections | l = −29→29 |
Refinement on F2 | 291 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.151 | w = 1/[σ2(Fo2) + (0.0495P)2 + 7.4732P] where P = (Fo2 + 2Fc2)/3 |
S = 1.21 | (Δ/σ)max = 0.001 |
15260 reflections | Δρmax = 0.56 e Å−3 |
1046 parameters | Δρmin = −0.68 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.3573 (2) | 0.26380 (17) | 0.77353 (15) | 0.0300 (7) | |
C2 | 0.4143 (2) | 0.20289 (17) | 0.79218 (14) | 0.0287 (6) | |
C3 | 0.5058 (2) | 0.21463 (17) | 0.81436 (14) | 0.0289 (7) | |
C4 | 0.5622 (2) | 0.15956 (19) | 0.83987 (15) | 0.0341 (7) | |
H4 | 0.5433 | 0.1123 | 0.8376 | 0.041* | |
C5 | 0.6447 (2) | 0.1749 (2) | 0.86803 (16) | 0.0392 (8) | |
H5 | 0.6811 | 0.1381 | 0.8850 | 0.047* | |
C6 | 0.6738 (2) | 0.2450 (2) | 0.87123 (17) | 0.0423 (9) | |
H6 | 0.7292 | 0.2554 | 0.8913 | 0.051* | |
C7 | 0.6209 (2) | 0.2991 (2) | 0.84477 (17) | 0.0412 (8) | |
H7 | 0.6418 | 0.3458 | 0.8465 | 0.049* | |
C8 | 0.5364 (2) | 0.28614 (18) | 0.81521 (15) | 0.0318 (7) | |
C9 | 0.4809 (2) | 0.34500 (17) | 0.78633 (15) | 0.0306 (7) | |
C10 | 0.5151 (2) | 0.41244 (19) | 0.77676 (16) | 0.0371 (8) | |
H10 | 0.5735 | 0.4200 | 0.7897 | 0.045* | |
C11 | 0.4652 (2) | 0.46755 (19) | 0.74890 (17) | 0.0403 (8) | |
H11 | 0.4897 | 0.5119 | 0.7442 | 0.048* | |
C12 | 0.3783 (2) | 0.45710 (18) | 0.72779 (17) | 0.0388 (8) | |
H12 | 0.3445 | 0.4941 | 0.7085 | 0.047* | |
C13 | 0.3423 (2) | 0.39116 (17) | 0.73569 (16) | 0.0334 (7) | |
H13 | 0.2841 | 0.3841 | 0.7212 | 0.040* | |
C14 | 0.3922 (2) | 0.33465 (16) | 0.76530 (15) | 0.0294 (7) | |
C15 | 0.3654 (2) | 0.24577 (17) | 0.93609 (14) | 0.0292 (7) | |
C16 | 0.4342 (2) | 0.19229 (17) | 0.94884 (14) | 0.0283 (6) | |
C17 | 0.5203 (2) | 0.21590 (17) | 0.98016 (14) | 0.0293 (7) | |
C18 | 0.5819 (2) | 0.16511 (18) | 1.00548 (14) | 0.0327 (7) | |
H18 | 0.5684 | 0.1165 | 1.0024 | 0.039* | |
C19 | 0.6622 (2) | 0.1864 (2) | 1.03489 (15) | 0.0364 (8) | |
H19 | 0.7032 | 0.1524 | 1.0507 | 0.044* | |
C20 | 0.6815 (2) | 0.2591 (2) | 1.04065 (17) | 0.0410 (8) | |
H20 | 0.7354 | 0.2738 | 1.0606 | 0.049* | |
C21 | 0.6211 (2) | 0.3092 (2) | 1.01689 (16) | 0.0396 (8) | |
H21 | 0.6345 | 0.3577 | 1.0218 | 0.048* | |
C22 | 0.5392 (2) | 0.28906 (18) | 0.98522 (14) | 0.0317 (7) | |
C23 | 0.4766 (2) | 0.34208 (17) | 0.95560 (15) | 0.0317 (7) | |
C24 | 0.4995 (2) | 0.41366 (19) | 0.94928 (17) | 0.0386 (8) | |
H24 | 0.5548 | 0.4282 | 0.9663 | 0.046* | |
C25 | 0.4432 (3) | 0.4633 (2) | 0.91884 (18) | 0.0428 (9) | |
H25 | 0.4599 | 0.5108 | 0.9166 | 0.051* | |
C26 | 0.3618 (2) | 0.44223 (19) | 0.89172 (17) | 0.0408 (8) | |
H26 | 0.3242 | 0.4751 | 0.8696 | 0.049* | |
C27 | 0.3360 (2) | 0.37214 (18) | 0.89741 (16) | 0.0363 (8) | |
H27 | 0.2809 | 0.3585 | 0.8790 | 0.044* | |
C28 | 0.3911 (2) | 0.32129 (17) | 0.93032 (15) | 0.0312 (7) | |
C29 | 0.0764 (2) | 0.10264 (17) | 0.76379 (14) | 0.0291 (7) | |
C30 | 0.1064 (2) | 0.03055 (17) | 0.75287 (15) | 0.0309 (7) | |
C31 | 0.0435 (2) | −0.02258 (18) | 0.72335 (15) | 0.0346 (7) | |
C32 | 0.0685 (2) | −0.0803 (2) | 0.69200 (18) | 0.0429 (9) | |
H32 | 0.1254 | −0.0851 | 0.6889 | 0.051* | |
C33 | 0.0088 (3) | −0.1305 (2) | 0.6655 (2) | 0.0529 (10) | |
H33 | 0.0255 | −0.1689 | 0.6445 | 0.064* | |
C34 | −0.0749 (3) | −0.1236 (2) | 0.6701 (2) | 0.0539 (11) | |
H34 | −0.1146 | −0.1579 | 0.6526 | 0.065* | |
C35 | −0.1009 (2) | −0.0668 (2) | 0.70016 (19) | 0.0472 (9) | |
H35 | −0.1581 | −0.0628 | 0.7026 | 0.057* | |
C36 | −0.0422 (2) | −0.01423 (19) | 0.72739 (16) | 0.0366 (8) | |
C37 | −0.0676 (2) | 0.0483 (2) | 0.75883 (16) | 0.0360 (8) | |
C38 | −0.1479 (2) | 0.0511 (2) | 0.77467 (18) | 0.0434 (9) | |
H38 | −0.1845 | 0.0120 | 0.7661 | 0.052* | |
C39 | −0.1741 (2) | 0.1100 (2) | 0.80252 (18) | 0.0462 (9) | |
H39 | −0.2275 | 0.1102 | 0.8127 | 0.055* | |
C40 | −0.1214 (2) | 0.1683 (2) | 0.81519 (18) | 0.0450 (9) | |
H40 | −0.1397 | 0.2086 | 0.8331 | 0.054* | |
C41 | −0.0410 (2) | 0.1676 (2) | 0.80142 (17) | 0.0393 (8) | |
H41 | −0.0054 | 0.2072 | 0.8109 | 0.047* | |
C42 | −0.0122 (2) | 0.10822 (18) | 0.77336 (15) | 0.0323 (7) | |
C43 | 0.0836 (2) | 0.08681 (19) | 0.92655 (15) | 0.0345 (7) | |
C44 | 0.1243 (2) | 0.02254 (19) | 0.90908 (15) | 0.0346 (7) | |
C45 | 0.0739 (2) | −0.04203 (19) | 0.89031 (16) | 0.0378 (8) | |
C46 | 0.1065 (3) | −0.1008 (2) | 0.86405 (17) | 0.0433 (9) | |
H46 | 0.1639 | −0.1016 | 0.8616 | 0.052* | |
C47 | 0.0542 (3) | −0.1577 (2) | 0.8417 (2) | 0.0555 (11) | |
H47 | 0.0760 | −0.1960 | 0.8233 | 0.067* | |
C48 | −0.0306 (3) | −0.1576 (3) | 0.8468 (2) | 0.0633 (13) | |
H48 | −0.0655 | −0.1963 | 0.8323 | 0.076* | |
C49 | −0.0636 (3) | −0.1003 (2) | 0.8731 (2) | 0.0535 (11) | |
H49 | −0.1209 | −0.1011 | 0.8758 | 0.064* | |
C50 | −0.0134 (2) | −0.0412 (2) | 0.89578 (16) | 0.0424 (9) | |
C51 | −0.0494 (2) | 0.0194 (2) | 0.92335 (16) | 0.0408 (9) | |
C52 | −0.1321 (3) | 0.0157 (2) | 0.93653 (19) | 0.0505 (10) | |
H52 | −0.1643 | −0.0258 | 0.9266 | 0.061* | |
C53 | −0.1662 (2) | 0.0706 (3) | 0.96312 (19) | 0.0524 (11) | |
H53 | −0.2208 | 0.0661 | 0.9712 | 0.063* | |
C54 | −0.1207 (2) | 0.1331 (3) | 0.97825 (18) | 0.0507 (10) | |
H54 | −0.1443 | 0.1706 | 0.9964 | 0.061* | |
C55 | −0.0392 (2) | 0.1395 (2) | 0.96614 (17) | 0.0430 (9) | |
H55 | −0.0084 | 0.1816 | 0.9762 | 0.052* | |
C56 | −0.0028 (2) | 0.0833 (2) | 0.93893 (15) | 0.0379 (8) | |
C57 | 0.4778 (2) | −0.09599 (17) | 0.87975 (15) | 0.0311 (7) | |
C58 | 0.4046 (2) | −0.13101 (17) | 0.83829 (15) | 0.0305 (7) | |
C59 | 0.4055 (2) | −0.20914 (17) | 0.83084 (14) | 0.0320 (7) | |
C60 | 0.3314 (2) | −0.24949 (19) | 0.80879 (17) | 0.0412 (8) | |
H60 | 0.2797 | −0.2260 | 0.7955 | 0.049* | |
C61 | 0.3342 (3) | −0.3230 (2) | 0.80656 (19) | 0.0508 (10) | |
H61 | 0.2842 | −0.3488 | 0.7931 | 0.061* | |
C62 | 0.4101 (3) | −0.3585 (2) | 0.82407 (19) | 0.0534 (11) | |
H62 | 0.4120 | −0.4082 | 0.8214 | 0.064* | |
C63 | 0.4839 (3) | −0.3203 (2) | 0.84575 (19) | 0.0487 (10) | |
H63 | 0.5352 | −0.3449 | 0.8576 | 0.058* | |
C64 | 0.4835 (2) | −0.24541 (18) | 0.85028 (16) | 0.0367 (8) | |
C65 | 0.5628 (2) | −0.20611 (19) | 0.87678 (16) | 0.0367 (8) | |
C66 | 0.6421 (2) | −0.2409 (2) | 0.88592 (18) | 0.0453 (9) | |
H66 | 0.6448 | −0.2878 | 0.8724 | 0.054* | |
C67 | 0.7154 (3) | −0.2078 (2) | 0.91426 (19) | 0.0483 (10) | |
H67 | 0.7673 | −0.2321 | 0.9199 | 0.058* | |
C68 | 0.7123 (2) | −0.1384 (2) | 0.93455 (18) | 0.0441 (9) | |
H68 | 0.7622 | −0.1167 | 0.9550 | 0.053* | |
C69 | 0.6367 (2) | −0.10049 (19) | 0.92512 (16) | 0.0372 (8) | |
H69 | 0.6360 | −0.0534 | 0.9384 | 0.045* | |
C70 | 0.5598 (2) | −0.13368 (18) | 0.89503 (15) | 0.0321 (7) | |
C71 | 0.1134 (3) | 0.1368 (4) | 0.5502 (3) | 0.100 (2) | |
H71A | 0.0755 | 0.1011 | 0.5291 | 0.150* | |
H71B | 0.1188 | 0.1755 | 0.5235 | 0.150* | |
H71C | 0.0906 | 0.1547 | 0.5832 | 0.150* | |
C72 | 0.2006 (3) | 0.1037 (3) | 0.5736 (2) | 0.0596 (12) | |
C73 | 0.2598 (3) | 0.0972 (2) | 0.5371 (2) | 0.0513 (10) | |
H73 | 0.2466 | 0.1145 | 0.4980 | 0.062* | |
C74 | 0.3375 (3) | 0.0656 (2) | 0.55792 (19) | 0.0501 (10) | |
H74 | 0.3767 | 0.0618 | 0.5330 | 0.060* | |
C75 | 0.3582 (3) | 0.0391 (2) | 0.61574 (19) | 0.0502 (10) | |
H75 | 0.4106 | 0.0167 | 0.6294 | 0.060* | |
C76 | 0.3013 (3) | 0.0460 (3) | 0.6527 (2) | 0.0634 (13) | |
H76 | 0.3150 | 0.0287 | 0.6917 | 0.076* | |
C77 | 0.2235 (3) | 0.0787 (3) | 0.6320 (2) | 0.0722 (15) | |
H77 | 0.1857 | 0.0842 | 0.6578 | 0.087* | |
C78 | −0.1860 (5) | 0.0902 (4) | 0.4357 (4) | 0.087 (2) | 0.66 |
H78A | −0.1443 | 0.0585 | 0.4248 | 0.131* | 0.66 |
H78B | −0.1928 | 0.1314 | 0.4099 | 0.131* | 0.66 |
H78C | −0.2397 | 0.0656 | 0.4315 | 0.131* | 0.66 |
C79 | −0.1572 (3) | 0.1133 (3) | 0.4982 (3) | 0.0727 (19) | 0.66 |
C80 | −0.1792 (5) | 0.0748 (4) | 0.5449 (3) | 0.080 (2) | 0.66 |
H80 | −0.2124 | 0.0336 | 0.5364 | 0.096* | 0.66 |
C81 | −0.1524 (6) | 0.0964 (5) | 0.6039 (4) | 0.086 (3) | 0.66 |
H81 | −0.1681 | 0.0703 | 0.6348 | 0.103* | 0.66 |
C82 | −0.1021 (6) | 0.1574 (5) | 0.6167 (3) | 0.082 (3) | 0.66 |
H82 | −0.0833 | 0.1721 | 0.6562 | 0.098* | 0.66 |
C83 | −0.0800 (5) | 0.1963 (4) | 0.5703 (3) | 0.083 (2) | 0.66 |
H83 | −0.0466 | 0.2373 | 0.5789 | 0.100* | 0.66 |
C84 | −0.1068 (4) | 0.1750 (3) | 0.5113 (3) | 0.0769 (19) | 0.66 |
H84 | −0.0916 | 0.2015 | 0.4805 | 0.092* | 0.66 |
C78A | −0.1035 (9) | 0.1587 (8) | 0.4495 (6) | 0.078 (4) | 0.34 |
H78D | −0.0889 | 0.2087 | 0.4523 | 0.118* | 0.34 |
H78E | −0.1505 | 0.1513 | 0.4163 | 0.118* | 0.34 |
H78F | −0.0551 | 0.1314 | 0.4433 | 0.118* | 0.34 |
C79A | −0.1290 (7) | 0.1344 (6) | 0.5073 (7) | 0.080 (3) | 0.34 |
C81A | −0.2097 (10) | 0.0579 (9) | 0.5603 (8) | 0.082 (3) | 0.34 |
H81A | −0.2488 | 0.0208 | 0.5596 | 0.098* | 0.34 |
C80A | −0.1873 (8) | 0.0791 (7) | 0.5038 (8) | 0.079 (3) | 0.34 |
H80A | −0.2108 | 0.0567 | 0.4677 | 0.094* | 0.34 |
C82A | −0.1790 (13) | 0.0872 (12) | 0.6100 (11) | 0.082 (3) | 0.34 |
H82A | −0.1962 | 0.0714 | 0.6444 | 0.098* | 0.34 |
C83A | −0.1209 (15) | 0.1416 (12) | 0.6139 (7) | 0.082 (3) | 0.34 |
H83A | −0.0979 | 0.1629 | 0.6505 | 0.099* | 0.34 |
C84A | −0.0965 (12) | 0.1648 (9) | 0.5594 (6) | 0.081 (2) | 0.34 |
H84A | −0.0572 | 0.2019 | 0.5609 | 0.097* | 0.34 |
N1 | 0.27646 (17) | 0.24607 (14) | 0.76671 (13) | 0.0330 (6) | |
N2 | 0.37143 (17) | 0.14219 (14) | 0.79170 (13) | 0.0302 (6) | |
N3 | 0.28561 (17) | 0.22388 (14) | 0.93075 (12) | 0.0312 (6) | |
N4 | 0.42751 (17) | 0.12499 (14) | 0.93553 (12) | 0.0307 (6) | |
N5 | 0.13044 (18) | 0.15645 (14) | 0.76514 (14) | 0.0337 (6) | |
N6 | 0.18439 (17) | 0.00730 (14) | 0.76635 (13) | 0.0308 (6) | |
N7 | 0.13358 (18) | 0.14323 (15) | 0.93093 (13) | 0.0345 (6) | |
N8 | 0.20644 (18) | 0.03278 (15) | 0.90921 (13) | 0.0330 (6) | |
N9 | 0.45806 (17) | −0.03173 (14) | 0.89580 (12) | 0.0301 (6) | |
N10 | 0.34564 (17) | −0.08566 (14) | 0.81453 (13) | 0.0329 (6) | |
O1 | 0.21502 (15) | 0.29635 (12) | 0.75199 (13) | 0.0424 (6) | |
O2 | 0.41168 (14) | 0.07989 (11) | 0.80519 (11) | 0.0333 (5) | |
O3 | 0.22535 (15) | 0.27495 (13) | 0.92507 (12) | 0.0399 (6) | |
O4 | 0.34924 (14) | 0.09770 (12) | 0.91047 (11) | 0.0342 (5) | |
O5 | 0.09813 (16) | 0.22254 (13) | 0.76779 (14) | 0.0454 (7) | |
O6 | 0.24766 (14) | 0.05433 (12) | 0.79020 (11) | 0.0331 (5) | |
O7 | 0.10615 (16) | 0.20776 (14) | 0.94544 (13) | 0.0445 (6) | |
O8 | 0.25669 (15) | −0.02059 (12) | 0.89833 (11) | 0.0361 (5) | |
O9 | 0.52088 (17) | 0.00669 (14) | 0.93202 (12) | 0.0404 (6) | |
O10 | 0.27559 (16) | −0.11284 (13) | 0.77446 (12) | 0.0395 (6) | |
Ni1 | 0.25135 (3) | 0.14989 (2) | 0.77620 (2) | 0.03005 (11) | |
Ni2 | 0.24612 (3) | 0.12803 (2) | 0.92204 (2) | 0.03014 (11) | |
Ni3 | 0.34675 (3) | 0.01380 (2) | 0.85238 (2) | 0.02978 (11) | |
H1A | 0.149 (4) | 0.262 (3) | 0.761 (3) | 0.10 (2)* | |
H2A | 0.166 (3) | 0.244 (3) | 0.935 (2) | 0.081 (16)* | |
H3A | 0.488 (4) | 0.043 (3) | 0.933 (3) | 0.09 (2)* | |
H4A | 0.233 (3) | −0.070 (3) | 0.770 (2) | 0.095 (18)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0263 (16) | 0.0267 (15) | 0.0376 (17) | −0.0007 (13) | 0.0076 (13) | 0.0027 (13) |
C2 | 0.0271 (16) | 0.0272 (15) | 0.0329 (16) | 0.0010 (13) | 0.0088 (13) | 0.0019 (13) |
C3 | 0.0274 (16) | 0.0301 (16) | 0.0318 (16) | −0.0026 (13) | 0.0120 (13) | −0.0014 (13) |
C4 | 0.0296 (17) | 0.0359 (18) | 0.0379 (18) | 0.0044 (14) | 0.0095 (14) | 0.0015 (14) |
C5 | 0.0292 (18) | 0.047 (2) | 0.0414 (19) | 0.0061 (16) | 0.0076 (15) | 0.0005 (16) |
C6 | 0.0243 (17) | 0.055 (2) | 0.046 (2) | −0.0013 (16) | 0.0035 (15) | −0.0013 (18) |
C7 | 0.0321 (19) | 0.045 (2) | 0.046 (2) | −0.0098 (16) | 0.0084 (15) | −0.0027 (17) |
C8 | 0.0286 (17) | 0.0349 (17) | 0.0343 (17) | −0.0010 (14) | 0.0122 (13) | −0.0019 (14) |
C9 | 0.0319 (17) | 0.0291 (16) | 0.0334 (16) | −0.0043 (13) | 0.0125 (13) | −0.0049 (13) |
C10 | 0.0361 (19) | 0.0343 (18) | 0.0448 (19) | −0.0093 (15) | 0.0173 (15) | −0.0043 (15) |
C11 | 0.049 (2) | 0.0278 (17) | 0.048 (2) | −0.0082 (16) | 0.0199 (17) | 0.0011 (15) |
C12 | 0.048 (2) | 0.0265 (16) | 0.046 (2) | 0.0013 (15) | 0.0182 (17) | 0.0047 (15) |
C13 | 0.0344 (18) | 0.0274 (16) | 0.0396 (18) | 0.0021 (14) | 0.0104 (14) | 0.0029 (14) |
C14 | 0.0313 (17) | 0.0237 (15) | 0.0354 (16) | −0.0018 (13) | 0.0118 (13) | 0.0005 (13) |
C15 | 0.0300 (17) | 0.0285 (16) | 0.0298 (15) | −0.0013 (13) | 0.0080 (13) | −0.0011 (13) |
C16 | 0.0288 (16) | 0.0261 (15) | 0.0309 (15) | −0.0018 (13) | 0.0081 (13) | −0.0004 (12) |
C17 | 0.0282 (16) | 0.0318 (16) | 0.0285 (15) | −0.0034 (13) | 0.0072 (12) | −0.0013 (13) |
C18 | 0.0335 (18) | 0.0324 (17) | 0.0321 (16) | −0.0039 (14) | 0.0062 (14) | −0.0003 (14) |
C19 | 0.0315 (18) | 0.043 (2) | 0.0338 (17) | 0.0031 (15) | 0.0052 (14) | 0.0020 (15) |
C20 | 0.0312 (18) | 0.049 (2) | 0.0400 (19) | −0.0079 (16) | −0.0001 (15) | −0.0026 (16) |
C21 | 0.039 (2) | 0.0372 (19) | 0.0425 (19) | −0.0116 (16) | 0.0077 (16) | −0.0027 (16) |
C22 | 0.0322 (17) | 0.0329 (17) | 0.0312 (16) | −0.0055 (14) | 0.0095 (13) | −0.0022 (13) |
C23 | 0.0345 (18) | 0.0299 (16) | 0.0328 (16) | −0.0010 (14) | 0.0116 (14) | −0.0016 (13) |
C24 | 0.040 (2) | 0.0316 (17) | 0.047 (2) | −0.0064 (15) | 0.0132 (16) | −0.0014 (15) |
C25 | 0.053 (2) | 0.0287 (17) | 0.050 (2) | −0.0040 (16) | 0.0183 (18) | −0.0005 (16) |
C26 | 0.048 (2) | 0.0298 (17) | 0.046 (2) | 0.0042 (16) | 0.0131 (17) | 0.0056 (15) |
C27 | 0.039 (2) | 0.0315 (17) | 0.0391 (18) | 0.0016 (15) | 0.0109 (15) | 0.0002 (14) |
C28 | 0.0335 (17) | 0.0283 (16) | 0.0341 (17) | −0.0011 (14) | 0.0123 (14) | −0.0011 (13) |
C29 | 0.0243 (16) | 0.0294 (16) | 0.0328 (16) | 0.0010 (13) | 0.0043 (12) | 0.0051 (13) |
C30 | 0.0267 (16) | 0.0299 (16) | 0.0355 (17) | −0.0019 (13) | 0.0053 (13) | 0.0030 (13) |
C31 | 0.0344 (18) | 0.0314 (17) | 0.0359 (17) | −0.0036 (14) | 0.0026 (14) | 0.0023 (14) |
C32 | 0.037 (2) | 0.041 (2) | 0.048 (2) | −0.0034 (16) | 0.0033 (16) | −0.0064 (17) |
C33 | 0.050 (3) | 0.040 (2) | 0.064 (3) | −0.0043 (19) | 0.001 (2) | −0.0108 (19) |
C34 | 0.047 (2) | 0.042 (2) | 0.065 (3) | −0.0139 (19) | −0.006 (2) | −0.003 (2) |
C35 | 0.034 (2) | 0.043 (2) | 0.060 (2) | −0.0075 (17) | −0.0004 (17) | 0.0005 (19) |
C36 | 0.0312 (18) | 0.0355 (18) | 0.0403 (19) | −0.0055 (14) | 0.0007 (14) | 0.0057 (15) |
C37 | 0.0289 (17) | 0.0405 (19) | 0.0374 (18) | −0.0029 (15) | 0.0040 (14) | 0.0083 (15) |
C38 | 0.0283 (18) | 0.052 (2) | 0.049 (2) | −0.0044 (16) | 0.0051 (16) | 0.0110 (18) |
C39 | 0.0297 (19) | 0.063 (3) | 0.048 (2) | 0.0074 (18) | 0.0115 (16) | 0.0120 (19) |
C40 | 0.033 (2) | 0.057 (2) | 0.047 (2) | 0.0098 (18) | 0.0127 (16) | 0.0050 (18) |
C41 | 0.0339 (19) | 0.0388 (19) | 0.046 (2) | 0.0010 (15) | 0.0088 (15) | −0.0008 (16) |
C42 | 0.0255 (16) | 0.0349 (17) | 0.0357 (17) | 0.0006 (13) | 0.0043 (13) | 0.0063 (14) |
C43 | 0.0300 (17) | 0.0390 (18) | 0.0344 (17) | −0.0011 (14) | 0.0059 (13) | 0.0044 (14) |
C44 | 0.0328 (18) | 0.0368 (18) | 0.0328 (17) | −0.0041 (14) | 0.0035 (14) | 0.0078 (14) |
C45 | 0.038 (2) | 0.0362 (18) | 0.0372 (18) | −0.0071 (15) | 0.0031 (15) | 0.0051 (15) |
C46 | 0.043 (2) | 0.041 (2) | 0.044 (2) | −0.0107 (17) | 0.0031 (16) | 0.0024 (16) |
C47 | 0.063 (3) | 0.044 (2) | 0.058 (3) | −0.017 (2) | 0.008 (2) | −0.005 (2) |
C48 | 0.056 (3) | 0.058 (3) | 0.071 (3) | −0.030 (2) | 0.001 (2) | −0.004 (2) |
C49 | 0.043 (2) | 0.054 (3) | 0.060 (3) | −0.017 (2) | 0.0017 (19) | 0.002 (2) |
C50 | 0.038 (2) | 0.047 (2) | 0.0387 (19) | −0.0151 (17) | 0.0003 (15) | 0.0102 (17) |
C51 | 0.0311 (19) | 0.053 (2) | 0.0361 (18) | −0.0055 (16) | 0.0019 (14) | 0.0130 (16) |
C52 | 0.037 (2) | 0.064 (3) | 0.049 (2) | −0.0115 (19) | 0.0057 (17) | 0.016 (2) |
C53 | 0.030 (2) | 0.078 (3) | 0.051 (2) | 0.002 (2) | 0.0115 (17) | 0.019 (2) |
C54 | 0.035 (2) | 0.074 (3) | 0.046 (2) | 0.005 (2) | 0.0135 (17) | 0.011 (2) |
C55 | 0.0318 (19) | 0.054 (2) | 0.045 (2) | 0.0010 (17) | 0.0108 (16) | 0.0073 (18) |
C56 | 0.0281 (17) | 0.050 (2) | 0.0341 (17) | −0.0037 (16) | 0.0025 (14) | 0.0097 (16) |
C57 | 0.0320 (17) | 0.0263 (15) | 0.0364 (17) | 0.0007 (13) | 0.0102 (14) | 0.0033 (13) |
C58 | 0.0323 (17) | 0.0262 (15) | 0.0341 (16) | 0.0016 (13) | 0.0095 (13) | 0.0031 (13) |
C59 | 0.0381 (18) | 0.0273 (16) | 0.0303 (16) | 0.0003 (14) | 0.0061 (14) | 0.0001 (13) |
C60 | 0.042 (2) | 0.0313 (18) | 0.048 (2) | −0.0002 (15) | 0.0036 (16) | 0.0007 (16) |
C61 | 0.065 (3) | 0.0309 (19) | 0.050 (2) | −0.0080 (19) | −0.003 (2) | −0.0026 (17) |
C62 | 0.076 (3) | 0.0271 (18) | 0.053 (2) | 0.0001 (19) | 0.003 (2) | −0.0054 (17) |
C63 | 0.058 (3) | 0.0330 (19) | 0.053 (2) | 0.0136 (18) | 0.0061 (19) | 0.0004 (17) |
C64 | 0.047 (2) | 0.0299 (17) | 0.0355 (18) | 0.0032 (15) | 0.0124 (15) | 0.0008 (14) |
C65 | 0.0396 (19) | 0.0345 (18) | 0.0382 (18) | 0.0070 (15) | 0.0130 (15) | 0.0062 (15) |
C66 | 0.045 (2) | 0.039 (2) | 0.054 (2) | 0.0106 (17) | 0.0135 (18) | 0.0073 (17) |
C67 | 0.038 (2) | 0.047 (2) | 0.060 (2) | 0.0133 (18) | 0.0112 (18) | 0.0134 (19) |
C68 | 0.0332 (19) | 0.047 (2) | 0.050 (2) | 0.0003 (16) | 0.0055 (16) | 0.0147 (18) |
C69 | 0.0358 (19) | 0.0345 (18) | 0.0411 (19) | 0.0052 (15) | 0.0074 (15) | 0.0093 (15) |
C70 | 0.0312 (17) | 0.0303 (16) | 0.0356 (17) | 0.0021 (14) | 0.0085 (14) | 0.0062 (14) |
C71 | 0.055 (3) | 0.108 (5) | 0.138 (6) | 0.015 (3) | 0.025 (4) | 0.052 (4) |
C72 | 0.047 (3) | 0.054 (3) | 0.080 (3) | 0.000 (2) | 0.019 (2) | 0.015 (2) |
C73 | 0.055 (3) | 0.052 (2) | 0.050 (2) | −0.001 (2) | 0.0157 (19) | 0.0116 (19) |
C74 | 0.059 (3) | 0.045 (2) | 0.053 (2) | 0.000 (2) | 0.026 (2) | −0.0001 (19) |
C75 | 0.054 (3) | 0.045 (2) | 0.053 (2) | 0.0034 (19) | 0.014 (2) | 0.0046 (19) |
C76 | 0.070 (3) | 0.074 (3) | 0.052 (3) | 0.018 (3) | 0.025 (2) | 0.016 (2) |
C77 | 0.075 (3) | 0.083 (4) | 0.071 (3) | 0.017 (3) | 0.045 (3) | 0.020 (3) |
C78 | 0.110 (6) | 0.077 (5) | 0.074 (5) | −0.002 (5) | 0.018 (5) | −0.001 (4) |
C79 | 0.081 (4) | 0.068 (4) | 0.068 (3) | 0.006 (4) | 0.014 (3) | −0.012 (3) |
C80 | 0.100 (5) | 0.069 (4) | 0.067 (4) | 0.005 (4) | 0.006 (4) | −0.005 (3) |
C81 | 0.105 (5) | 0.069 (4) | 0.075 (4) | 0.007 (4) | −0.001 (4) | 0.004 (4) |
C82 | 0.097 (5) | 0.070 (5) | 0.069 (4) | 0.009 (4) | −0.005 (4) | −0.009 (3) |
C83 | 0.088 (4) | 0.078 (5) | 0.080 (4) | 0.007 (4) | 0.007 (4) | −0.015 (4) |
C84 | 0.080 (4) | 0.075 (4) | 0.076 (4) | 0.010 (4) | 0.018 (4) | −0.010 (4) |
C78A | 0.087 (8) | 0.089 (8) | 0.067 (7) | 0.002 (7) | 0.035 (6) | 0.000 (7) |
C79A | 0.090 (5) | 0.074 (5) | 0.074 (4) | 0.010 (4) | 0.015 (4) | −0.008 (4) |
C81A | 0.098 (6) | 0.074 (6) | 0.070 (5) | 0.002 (5) | 0.010 (5) | −0.003 (5) |
C80A | 0.093 (6) | 0.070 (5) | 0.072 (5) | 0.001 (5) | 0.014 (5) | −0.005 (5) |
C82A | 0.097 (6) | 0.072 (5) | 0.071 (5) | 0.007 (5) | 0.004 (5) | 0.000 (4) |
C83A | 0.095 (6) | 0.074 (5) | 0.071 (4) | 0.006 (5) | −0.003 (5) | −0.005 (5) |
C84A | 0.090 (5) | 0.074 (5) | 0.075 (4) | 0.008 (4) | 0.007 (4) | −0.009 (4) |
N1 | 0.0260 (14) | 0.0272 (14) | 0.0453 (16) | 0.0056 (11) | 0.0061 (12) | 0.0058 (12) |
N2 | 0.0292 (14) | 0.0235 (13) | 0.0386 (15) | 0.0031 (11) | 0.0087 (12) | 0.0020 (11) |
N3 | 0.0283 (14) | 0.0289 (14) | 0.0366 (15) | 0.0044 (11) | 0.0072 (11) | 0.0010 (11) |
N4 | 0.0267 (14) | 0.0288 (13) | 0.0366 (14) | −0.0035 (11) | 0.0064 (11) | −0.0041 (11) |
N5 | 0.0284 (15) | 0.0259 (13) | 0.0478 (17) | 0.0024 (11) | 0.0104 (12) | 0.0030 (12) |
N6 | 0.0275 (14) | 0.0251 (13) | 0.0394 (15) | −0.0040 (11) | 0.0060 (12) | 0.0006 (11) |
N7 | 0.0304 (15) | 0.0345 (15) | 0.0379 (15) | −0.0016 (12) | 0.0058 (12) | 0.0002 (12) |
N8 | 0.0307 (15) | 0.0301 (14) | 0.0389 (15) | −0.0007 (12) | 0.0084 (12) | 0.0027 (12) |
N9 | 0.0279 (14) | 0.0247 (13) | 0.0365 (14) | −0.0019 (11) | 0.0034 (11) | 0.0023 (11) |
N10 | 0.0294 (15) | 0.0264 (13) | 0.0415 (16) | −0.0013 (11) | 0.0039 (12) | −0.0017 (12) |
O1 | 0.0271 (13) | 0.0255 (12) | 0.0740 (19) | 0.0064 (10) | 0.0091 (12) | 0.0141 (12) |
O2 | 0.0295 (12) | 0.0231 (11) | 0.0480 (14) | 0.0047 (9) | 0.0098 (10) | 0.0017 (10) |
O3 | 0.0292 (13) | 0.0282 (12) | 0.0627 (17) | 0.0058 (10) | 0.0104 (11) | 0.0020 (11) |
O4 | 0.0255 (12) | 0.0296 (12) | 0.0474 (14) | −0.0045 (9) | 0.0072 (10) | −0.0069 (10) |
O5 | 0.0288 (13) | 0.0255 (12) | 0.084 (2) | 0.0048 (10) | 0.0163 (13) | 0.0077 (13) |
O6 | 0.0249 (12) | 0.0255 (11) | 0.0468 (14) | −0.0039 (9) | 0.0021 (10) | 0.0009 (10) |
O7 | 0.0333 (14) | 0.0368 (14) | 0.0663 (18) | 0.0036 (11) | 0.0169 (12) | −0.0043 (13) |
O8 | 0.0344 (13) | 0.0292 (12) | 0.0449 (14) | −0.0010 (10) | 0.0087 (11) | 0.0005 (10) |
O9 | 0.0337 (14) | 0.0317 (13) | 0.0506 (15) | −0.0002 (11) | −0.0038 (11) | −0.0058 (11) |
O10 | 0.0349 (14) | 0.0309 (12) | 0.0471 (15) | 0.0019 (11) | −0.0049 (11) | −0.0071 (11) |
Ni1 | 0.0237 (2) | 0.0232 (2) | 0.0434 (2) | 0.00088 (16) | 0.00702 (17) | 0.00455 (17) |
Ni2 | 0.0251 (2) | 0.0275 (2) | 0.0382 (2) | −0.00170 (16) | 0.00718 (17) | −0.00033 (17) |
Ni3 | 0.0274 (2) | 0.0223 (2) | 0.0386 (2) | 0.00040 (16) | 0.00435 (17) | 0.00011 (17) |
C1—N1 | 1.310 (4) | C55—H55 | 0.9300 |
C1—C14 | 1.461 (4) | C57—N9 | 1.310 (4) |
C1—C2 | 1.464 (4) | C57—C70 | 1.465 (5) |
C2—N2 | 1.322 (4) | C57—C58 | 1.495 (5) |
C2—C3 | 1.462 (4) | C58—N10 | 1.299 (4) |
C3—C4 | 1.410 (5) | C58—C59 | 1.467 (4) |
C3—C8 | 1.418 (4) | C59—C60 | 1.406 (5) |
C4—C5 | 1.373 (5) | C59—C64 | 1.408 (5) |
C4—H4 | 0.9300 | C60—C61 | 1.372 (5) |
C5—C6 | 1.383 (5) | C60—H60 | 0.9300 |
C5—H5 | 0.9300 | C61—C62 | 1.368 (6) |
C6—C7 | 1.374 (5) | C61—H61 | 0.9300 |
C6—H6 | 0.9300 | C62—C63 | 1.380 (6) |
C7—C8 | 1.400 (5) | C62—H62 | 0.9300 |
C7—H7 | 0.9300 | C63—C64 | 1.399 (5) |
C8—C9 | 1.479 (5) | C63—H63 | 0.9300 |
C9—C10 | 1.406 (4) | C64—C65 | 1.481 (5) |
C9—C14 | 1.412 (5) | C65—C66 | 1.400 (5) |
C10—C11 | 1.373 (5) | C65—C70 | 1.416 (5) |
C10—H10 | 0.9300 | C66—C67 | 1.364 (6) |
C11—C12 | 1.387 (5) | C66—H66 | 0.9300 |
C11—H11 | 0.9300 | C67—C68 | 1.379 (6) |
C12—C13 | 1.384 (5) | C67—H67 | 0.9300 |
C12—H12 | 0.9300 | C68—C69 | 1.378 (5) |
C13—C14 | 1.408 (4) | C68—H68 | 0.9300 |
C13—H13 | 0.9300 | C69—C70 | 1.420 (5) |
C15—N3 | 1.321 (4) | C69—H69 | 0.9300 |
C15—C16 | 1.468 (4) | C71—C72 | 1.517 (7) |
C15—C28 | 1.479 (4) | C71—H71A | 0.9600 |
C16—N4 | 1.290 (4) | C71—H71B | 0.9600 |
C16—C17 | 1.481 (4) | C71—H71C | 0.9600 |
C17—C22 | 1.396 (4) | C72—C73 | 1.387 (6) |
C17—C18 | 1.401 (5) | C72—C77 | 1.388 (7) |
C18—C19 | 1.380 (5) | C73—C74 | 1.369 (6) |
C18—H18 | 0.9300 | C73—H73 | 0.9300 |
C19—C20 | 1.390 (5) | C74—C75 | 1.382 (6) |
C19—H19 | 0.9300 | C74—H74 | 0.9300 |
C20—C21 | 1.372 (5) | C75—C76 | 1.365 (6) |
C20—H20 | 0.9300 | C75—H75 | 0.9300 |
C21—C22 | 1.410 (5) | C76—C77 | 1.377 (7) |
C21—H21 | 0.9300 | C76—H76 | 0.9300 |
C22—C23 | 1.469 (5) | C77—H77 | 0.9300 |
C23—C24 | 1.399 (5) | C78—C79 | 1.470 (10) |
C23—C28 | 1.424 (5) | C78—H78A | 0.9600 |
C24—C25 | 1.376 (5) | C78—H78B | 0.9600 |
C24—H24 | 0.9300 | C78—H78C | 0.9600 |
C25—C26 | 1.378 (5) | C79—C80 | 1.386 (6) |
C25—H25 | 0.9300 | C79—C84 | 1.401 (6) |
C26—C27 | 1.384 (5) | C80—C81 | 1.386 (7) |
C26—H26 | 0.9300 | C80—H80 | 0.9300 |
C27—C28 | 1.402 (5) | C81—C82 | 1.390 (7) |
C27—H27 | 0.9300 | C81—H81 | 0.9300 |
C29—N5 | 1.319 (4) | C82—C83 | 1.386 (7) |
C29—C30 | 1.465 (4) | C82—H82 | 0.9300 |
C29—C42 | 1.479 (4) | C83—C84 | 1.384 (6) |
C30—N6 | 1.295 (4) | C83—H83 | 0.9300 |
C30—C31 | 1.472 (5) | C84—H84 | 0.9300 |
C31—C32 | 1.394 (5) | C78A—C79A | 1.523 (18) |
C31—C36 | 1.399 (5) | C78A—H78D | 0.9600 |
C32—C33 | 1.384 (5) | C78A—H78E | 0.9600 |
C32—H32 | 0.9300 | C78A—H78F | 0.9600 |
C33—C34 | 1.367 (6) | C79A—C84A | 1.32 (2) |
C33—H33 | 0.9300 | C79A—C80A | 1.382 (8) |
C34—C35 | 1.372 (6) | C81A—C82A | 1.26 (3) |
C34—H34 | 0.9300 | C81A—C80A | 1.46 (2) |
C35—C36 | 1.410 (5) | C81A—H81A | 0.9300 |
C35—H35 | 0.9300 | C80A—H80A | 0.9300 |
C36—C37 | 1.469 (5) | C82A—C83A | 1.36 (3) |
C37—C38 | 1.403 (5) | C82A—H82A | 0.9300 |
C37—C42 | 1.420 (5) | C83A—C84A | 1.44 (2) |
C38—C39 | 1.375 (6) | C83A—H83A | 0.9300 |
C38—H38 | 0.9300 | C84A—H84A | 0.9300 |
C39—C40 | 1.370 (6) | N1—O1 | 1.349 (3) |
C39—H39 | 0.9300 | N1—Ni1 | 1.859 (3) |
C40—C41 | 1.382 (5) | N2—O2 | 1.333 (3) |
C40—H40 | 0.9300 | N2—Ni1 | 1.884 (3) |
C41—C42 | 1.401 (5) | N3—O3 | 1.341 (3) |
C41—H41 | 0.9300 | N3—Ni2 | 1.892 (3) |
C43—N7 | 1.311 (4) | N4—O4 | 1.363 (3) |
C43—C44 | 1.457 (5) | N5—O5 | 1.342 (3) |
C43—C56 | 1.465 (5) | N5—Ni1 | 1.900 (3) |
C44—N8 | 1.325 (4) | N6—O6 | 1.364 (3) |
C44—C45 | 1.463 (5) | N7—O7 | 1.344 (4) |
C45—C46 | 1.399 (5) | N7—Ni2 | 1.871 (3) |
C45—C50 | 1.425 (5) | N8—O8 | 1.333 (4) |
C46—C47 | 1.381 (5) | N8—Ni2 | 1.888 (3) |
C46—H46 | 0.9300 | N9—O9 | 1.365 (4) |
C47—C48 | 1.383 (6) | N9—Ni3 | 2.035 (3) |
C47—H47 | 0.9300 | N10—O10 | 1.388 (4) |
C48—C49 | 1.381 (7) | N10—Ni3 | 2.043 (3) |
C48—H48 | 0.9300 | O1—H1A | 1.29 (6) |
C49—C50 | 1.399 (5) | O2—Ni3 | 2.050 (2) |
C49—H49 | 0.9300 | O3—H2A | 1.17 (5) |
C50—C51 | 1.465 (6) | O4—Ni2 | 1.811 (2) |
C51—C56 | 1.411 (5) | O4—Ni3 | 2.044 (2) |
C51—C52 | 1.416 (5) | O5—H1A | 1.13 (6) |
C52—C53 | 1.359 (6) | O6—Ni1 | 1.813 (2) |
C52—H52 | 0.9300 | O6—Ni3 | 2.042 (2) |
C53—C54 | 1.378 (6) | O7—H2A | 1.24 (6) |
C53—H53 | 0.9300 | O8—Ni3 | 2.047 (2) |
C54—C55 | 1.389 (5) | O9—H3A | 0.85 (6) |
C54—H54 | 0.9300 | O10—H4A | 1.04 (6) |
C55—C56 | 1.402 (5) | ||
N1—C1—C14 | 127.3 (3) | C60—C59—C58 | 123.0 (3) |
N1—C1—C2 | 112.3 (3) | C64—C59—C58 | 118.0 (3) |
C14—C1—C2 | 120.4 (3) | C61—C60—C59 | 121.1 (4) |
N2—C2—C3 | 127.7 (3) | C61—C60—H60 | 119.5 |
N2—C2—C1 | 111.7 (3) | C59—C60—H60 | 119.5 |
C3—C2—C1 | 120.3 (3) | C62—C61—C60 | 120.4 (4) |
C4—C3—C8 | 119.3 (3) | C62—C61—H61 | 119.8 |
C4—C3—C2 | 122.9 (3) | C60—C61—H61 | 119.8 |
C8—C3—C2 | 117.5 (3) | C61—C62—C63 | 119.8 (4) |
C5—C4—C3 | 120.8 (3) | C61—C62—H62 | 120.1 |
C5—C4—H4 | 119.6 | C63—C62—H62 | 120.1 |
C3—C4—H4 | 119.6 | C62—C63—C64 | 121.7 (4) |
C4—C5—C6 | 120.1 (3) | C62—C63—H63 | 119.2 |
C4—C5—H5 | 120.0 | C64—C63—H63 | 119.2 |
C6—C5—H5 | 120.0 | C63—C64—C59 | 118.2 (3) |
C7—C6—C5 | 120.0 (3) | C63—C64—C65 | 120.5 (3) |
C7—C6—H6 | 120.0 | C59—C64—C65 | 121.3 (3) |
C5—C6—H6 | 120.0 | C66—C65—C70 | 118.8 (3) |
C6—C7—C8 | 122.1 (4) | C66—C65—C64 | 120.2 (3) |
C6—C7—H7 | 119.0 | C70—C65—C64 | 120.9 (3) |
C8—C7—H7 | 119.0 | C67—C66—C65 | 121.6 (4) |
C7—C8—C3 | 117.6 (3) | C67—C66—H66 | 119.2 |
C7—C8—C9 | 121.2 (3) | C65—C66—H66 | 119.2 |
C3—C8—C9 | 121.2 (3) | C66—C67—C68 | 119.8 (4) |
C10—C9—C14 | 117.7 (3) | C66—C67—H67 | 120.1 |
C10—C9—C8 | 121.0 (3) | C68—C67—H67 | 120.1 |
C14—C9—C8 | 121.3 (3) | C69—C68—C67 | 121.3 (4) |
C11—C10—C9 | 122.2 (3) | C69—C68—H68 | 119.3 |
C11—C10—H10 | 118.9 | C67—C68—H68 | 119.3 |
C9—C10—H10 | 118.9 | C68—C69—C70 | 119.7 (3) |
C10—C11—C12 | 120.0 (3) | C68—C69—H69 | 120.1 |
C10—C11—H11 | 120.0 | C70—C69—H69 | 120.1 |
C12—C11—H11 | 120.0 | C65—C70—C69 | 118.7 (3) |
C13—C12—C11 | 119.5 (3) | C65—C70—C57 | 118.0 (3) |
C13—C12—H12 | 120.2 | C69—C70—C57 | 123.3 (3) |
C11—C12—H12 | 120.2 | C72—C71—H71A | 109.5 |
C12—C13—C14 | 121.1 (3) | C72—C71—H71B | 109.5 |
C12—C13—H13 | 119.4 | H71A—C71—H71B | 109.5 |
C14—C13—H13 | 119.4 | C72—C71—H71C | 109.5 |
C13—C14—C9 | 119.4 (3) | H71A—C71—H71C | 109.5 |
C13—C14—C1 | 122.9 (3) | H71B—C71—H71C | 109.5 |
C9—C14—C1 | 117.6 (3) | C73—C72—C77 | 117.9 (4) |
N3—C15—C16 | 118.6 (3) | C73—C72—C71 | 121.0 (5) |
N3—C15—C28 | 124.4 (3) | C77—C72—C71 | 121.2 (5) |
C16—C15—C28 | 117.0 (3) | C74—C73—C72 | 120.7 (4) |
N4—C16—C15 | 126.2 (3) | C74—C73—H73 | 119.7 |
N4—C16—C17 | 115.3 (3) | C72—C73—H73 | 119.7 |
C15—C16—C17 | 118.5 (3) | C73—C74—C75 | 120.6 (4) |
C22—C17—C18 | 120.3 (3) | C73—C74—H74 | 119.7 |
C22—C17—C16 | 119.6 (3) | C75—C74—H74 | 119.7 |
C18—C17—C16 | 120.1 (3) | C76—C75—C74 | 119.6 (4) |
C19—C18—C17 | 120.7 (3) | C76—C75—H75 | 120.2 |
C19—C18—H18 | 119.6 | C74—C75—H75 | 120.2 |
C17—C18—H18 | 119.6 | C75—C76—C77 | 119.9 (4) |
C18—C19—C20 | 119.5 (3) | C75—C76—H76 | 120.0 |
C18—C19—H19 | 120.3 | C77—C76—H76 | 120.0 |
C20—C19—H19 | 120.3 | C76—C77—C72 | 121.3 (4) |
C21—C20—C19 | 120.2 (3) | C76—C77—H77 | 119.3 |
C21—C20—H20 | 119.9 | C72—C77—H77 | 119.3 |
C19—C20—H20 | 119.9 | C79—C78—H78A | 109.5 |
C20—C21—C22 | 121.7 (3) | C79—C78—H78B | 109.5 |
C20—C21—H21 | 119.2 | H78A—C78—H78B | 109.5 |
C22—C21—H21 | 119.2 | C79—C78—H78C | 109.5 |
C17—C22—C21 | 117.7 (3) | H78A—C78—H78C | 109.5 |
C17—C22—C23 | 120.3 (3) | H78B—C78—H78C | 109.5 |
C21—C22—C23 | 122.0 (3) | C80—C79—C84 | 119.1 (5) |
C24—C23—C28 | 117.8 (3) | C80—C79—C78 | 121.0 (5) |
C24—C23—C22 | 121.4 (3) | C84—C79—C78 | 119.9 (5) |
C28—C23—C22 | 120.7 (3) | C81—C80—C79 | 121.2 (5) |
C25—C24—C23 | 122.4 (3) | C81—C80—H80 | 119.4 |
C25—C24—H24 | 118.8 | C79—C80—H80 | 119.4 |
C23—C24—H24 | 118.8 | C80—C81—C82 | 119.5 (5) |
C24—C25—C26 | 119.6 (3) | C80—C81—H81 | 120.2 |
C24—C25—H25 | 120.2 | C82—C81—H81 | 120.2 |
C26—C25—H25 | 120.2 | C83—C82—C81 | 119.6 (5) |
C25—C26—C27 | 119.9 (4) | C83—C82—H82 | 120.2 |
C25—C26—H26 | 120.0 | C81—C82—H82 | 120.2 |
C27—C26—H26 | 120.0 | C84—C83—C82 | 121.0 (5) |
C26—C27—C28 | 121.5 (3) | C84—C83—H83 | 119.5 |
C26—C27—H27 | 119.3 | C82—C83—H83 | 119.5 |
C28—C27—H27 | 119.3 | C83—C84—C79 | 119.5 (5) |
C27—C28—C23 | 118.6 (3) | C83—C84—H84 | 120.2 |
C27—C28—C15 | 122.4 (3) | C79—C84—H84 | 120.2 |
C23—C28—C15 | 118.9 (3) | C79A—C78A—H78D | 109.5 |
N5—C29—C30 | 117.8 (3) | C79A—C78A—H78E | 109.5 |
N5—C29—C42 | 125.7 (3) | H78D—C78A—H78E | 109.5 |
C30—C29—C42 | 116.4 (3) | C79A—C78A—H78F | 109.5 |
N6—C30—C29 | 126.8 (3) | H78D—C78A—H78F | 109.5 |
N6—C30—C31 | 114.6 (3) | H78E—C78A—H78F | 109.5 |
C29—C30—C31 | 118.6 (3) | C84A—C79A—C80A | 120.4 (17) |
C32—C31—C36 | 120.4 (3) | C84A—C79A—C78A | 121.6 (11) |
C32—C31—C30 | 120.9 (3) | C80A—C79A—C78A | 117.9 (12) |
C36—C31—C30 | 118.7 (3) | C82A—C81A—C80A | 123.7 (16) |
C33—C32—C31 | 120.1 (4) | C82A—C81A—H81A | 118.2 |
C33—C32—H32 | 120.0 | C80A—C81A—H81A | 118.2 |
C31—C32—H32 | 120.0 | C79A—C80A—C81A | 115.9 (14) |
C34—C33—C32 | 120.1 (4) | C79A—C80A—H80A | 122.1 |
C34—C33—H33 | 119.9 | C81A—C80A—H80A | 122.1 |
C32—C33—H33 | 119.9 | C81A—C82A—C83A | 121 (2) |
C33—C34—C35 | 120.7 (4) | C81A—C82A—H82A | 119.5 |
C33—C34—H34 | 119.7 | C83A—C82A—H82A | 119.5 |
C35—C34—H34 | 119.7 | C82A—C83A—C84A | 117.8 (17) |
C34—C35—C36 | 121.0 (4) | C82A—C83A—H83A | 121.1 |
C34—C35—H35 | 119.5 | C84A—C83A—H83A | 121.1 |
C36—C35—H35 | 119.5 | C79A—C84A—C83A | 121.3 (18) |
C31—C36—C35 | 117.8 (3) | C79A—C84A—H84A | 119.3 |
C31—C36—C37 | 119.5 (3) | C83A—C84A—H84A | 119.3 |
C35—C36—C37 | 122.8 (3) | C1—N1—O1 | 120.2 (3) |
C38—C37—C42 | 118.0 (3) | C1—N1—Ni1 | 117.4 (2) |
C38—C37—C36 | 120.8 (3) | O1—N1—Ni1 | 122.4 (2) |
C42—C37—C36 | 121.1 (3) | C2—N2—O2 | 121.3 (3) |
C39—C38—C37 | 121.9 (4) | C2—N2—Ni1 | 116.3 (2) |
C39—C38—H38 | 119.1 | O2—N2—Ni1 | 122.3 (2) |
C37—C38—H38 | 119.1 | C15—N3—O3 | 116.8 (3) |
C40—C39—C38 | 120.0 (4) | C15—N3—Ni2 | 126.6 (2) |
C40—C39—H39 | 120.0 | O3—N3—Ni2 | 116.3 (2) |
C38—C39—H39 | 120.0 | C16—N4—O4 | 119.1 (3) |
C39—C40—C41 | 120.2 (4) | C29—N5—O5 | 116.3 (3) |
C39—C40—H40 | 119.9 | C29—N5—Ni1 | 126.6 (2) |
C41—C40—H40 | 119.9 | O5—N5—Ni1 | 116.3 (2) |
C40—C41—C42 | 121.2 (4) | C30—N6—O6 | 118.6 (3) |
C40—C41—H41 | 119.4 | C43—N7—O7 | 120.8 (3) |
C42—C41—H41 | 119.4 | C43—N7—Ni2 | 117.0 (2) |
C41—C42—C37 | 118.7 (3) | O7—N7—Ni2 | 122.0 (2) |
C41—C42—C29 | 122.4 (3) | C44—N8—O8 | 121.7 (3) |
C37—C42—C29 | 118.6 (3) | C44—N8—Ni2 | 115.9 (2) |
N7—C43—C44 | 112.4 (3) | O8—N8—Ni2 | 122.3 (2) |
N7—C43—C56 | 127.1 (3) | C57—N9—O9 | 117.4 (3) |
C44—C43—C56 | 120.4 (3) | C57—N9—Ni3 | 118.8 (2) |
N8—C44—C43 | 112.2 (3) | O9—N9—Ni3 | 122.5 (2) |
N8—C44—C45 | 127.3 (3) | C58—N10—O10 | 117.1 (3) |
C43—C44—C45 | 120.4 (3) | C58—N10—Ni3 | 118.1 (2) |
C46—C45—C50 | 120.2 (3) | O10—N10—Ni3 | 123.1 (2) |
C46—C45—C44 | 122.5 (3) | N1—O1—H1A | 101 (3) |
C50—C45—C44 | 117.1 (3) | N2—O2—Ni3 | 111.88 (18) |
C47—C46—C45 | 120.6 (4) | N3—O3—H2A | 103 (2) |
C47—C46—H46 | 119.7 | N4—O4—Ni2 | 127.34 (19) |
C45—C46—H46 | 119.7 | N4—O4—Ni3 | 116.88 (18) |
C46—C47—C48 | 119.8 (4) | Ni2—O4—Ni3 | 115.78 (11) |
C46—C47—H47 | 120.1 | N5—O5—H1A | 107 (3) |
C48—C47—H47 | 120.1 | N6—O6—Ni1 | 127.55 (19) |
C49—C48—C47 | 120.4 (4) | N6—O6—Ni3 | 116.43 (18) |
C49—C48—H48 | 119.8 | Ni1—O6—Ni3 | 115.93 (11) |
C47—C48—H48 | 119.8 | N7—O7—H2A | 98 (2) |
C48—C49—C50 | 121.9 (4) | N8—O8—Ni3 | 111.97 (18) |
C48—C49—H49 | 119.0 | N9—O9—H3A | 93 (4) |
C50—C49—H49 | 119.0 | N10—O10—H4A | 102 (3) |
C49—C50—C45 | 117.1 (4) | O6—Ni1—N1 | 169.58 (11) |
C49—C50—C51 | 121.4 (4) | O6—Ni1—N2 | 87.73 (10) |
C45—C50—C51 | 121.5 (3) | N1—Ni1—N2 | 81.94 (11) |
C56—C51—C52 | 117.1 (4) | O6—Ni1—N5 | 91.03 (11) |
C56—C51—C50 | 121.7 (3) | N1—Ni1—N5 | 99.21 (12) |
C52—C51—C50 | 121.2 (4) | N2—Ni1—N5 | 176.81 (12) |
C53—C52—C51 | 122.3 (4) | O4—Ni2—N7 | 170.22 (11) |
C53—C52—H52 | 118.9 | O4—Ni2—N8 | 88.31 (11) |
C51—C52—H52 | 118.9 | N7—Ni2—N8 | 81.93 (12) |
C52—C53—C54 | 120.6 (4) | O4—Ni2—N3 | 90.94 (11) |
C52—C53—H53 | 119.7 | N7—Ni2—N3 | 98.79 (12) |
C54—C53—H53 | 119.7 | N8—Ni2—N3 | 177.16 (12) |
C53—C54—C55 | 119.4 (4) | N9—Ni3—O6 | 165.53 (11) |
C53—C54—H54 | 120.3 | N9—Ni3—N10 | 76.02 (11) |
C55—C54—H54 | 120.3 | O6—Ni3—N10 | 95.97 (10) |
C54—C55—C56 | 120.9 (4) | N9—Ni3—O4 | 96.00 (10) |
C54—C55—H55 | 119.5 | O6—Ni3—O4 | 94.37 (10) |
C56—C55—H55 | 119.5 | N10—Ni3—O4 | 164.78 (11) |
C55—C56—C51 | 119.8 (3) | N9—Ni3—O8 | 104.85 (10) |
C55—C56—C43 | 123.0 (3) | O6—Ni3—O8 | 86.82 (10) |
C51—C56—C43 | 117.3 (3) | N10—Ni3—O8 | 89.16 (10) |
N9—C57—C70 | 128.8 (3) | O4—Ni3—O8 | 80.29 (9) |
N9—C57—C58 | 112.0 (3) | N9—Ni3—O2 | 91.16 (10) |
C70—C57—C58 | 119.2 (3) | O6—Ni3—O2 | 79.47 (9) |
N10—C58—C59 | 128.4 (3) | N10—Ni3—O2 | 106.60 (10) |
N10—C58—C57 | 112.7 (3) | O4—Ni3—O2 | 86.25 (9) |
C59—C58—C57 | 118.8 (3) | O8—Ni3—O2 | 159.99 (9) |
C60—C59—C64 | 118.8 (3) | ||
N1—C1—C2—N2 | 6.8 (4) | C50—C51—C56—C43 | −0.1 (5) |
C14—C1—C2—N2 | −174.0 (3) | N7—C43—C56—C55 | −9.7 (6) |
N1—C1—C2—C3 | −166.9 (3) | C44—C43—C56—C55 | 168.1 (3) |
C14—C1—C2—C3 | 12.4 (5) | N7—C43—C56—C51 | 171.5 (3) |
N2—C2—C3—C4 | −0.7 (5) | C44—C43—C56—C51 | −10.7 (5) |
C1—C2—C3—C4 | 171.9 (3) | N9—C57—C58—N10 | 16.8 (4) |
N2—C2—C3—C8 | −174.4 (3) | C70—C57—C58—N10 | −160.8 (3) |
C1—C2—C3—C8 | −1.8 (4) | N9—C57—C58—C59 | −161.1 (3) |
C8—C3—C4—C5 | 3.3 (5) | C70—C57—C58—C59 | 21.3 (4) |
C2—C3—C4—C5 | −170.3 (3) | N10—C58—C59—C60 | −17.7 (6) |
C3—C4—C5—C6 | −0.6 (5) | C57—C58—C59—C60 | 159.9 (3) |
C4—C5—C6—C7 | −1.8 (6) | N10—C58—C59—C64 | 166.4 (3) |
C5—C6—C7—C8 | 1.4 (6) | C57—C58—C59—C64 | −16.0 (5) |
C6—C7—C8—C3 | 1.3 (5) | C64—C59—C60—C61 | 0.6 (6) |
C6—C7—C8—C9 | −179.2 (3) | C58—C59—C60—C61 | −175.3 (4) |
C4—C3—C8—C7 | −3.6 (5) | C59—C60—C61—C62 | −2.1 (6) |
C2—C3—C8—C7 | 170.4 (3) | C60—C61—C62—C63 | 1.9 (7) |
C4—C3—C8—C9 | 176.9 (3) | C61—C62—C63—C64 | −0.2 (7) |
C2—C3—C8—C9 | −9.1 (4) | C62—C63—C64—C59 | −1.3 (6) |
C7—C8—C9—C10 | 13.2 (5) | C62—C63—C64—C65 | 176.6 (4) |
C3—C8—C9—C10 | −167.3 (3) | C60—C59—C64—C63 | 1.1 (5) |
C7—C8—C9—C14 | −169.4 (3) | C58—C59—C64—C63 | 177.2 (3) |
C3—C8—C9—C14 | 10.1 (5) | C60—C59—C64—C65 | −176.9 (3) |
C14—C9—C10—C11 | 1.0 (5) | C58—C59—C64—C65 | −0.8 (5) |
C8—C9—C10—C11 | 178.6 (3) | C63—C64—C65—C66 | 13.5 (5) |
C9—C10—C11—C12 | −1.6 (6) | C59—C64—C65—C66 | −168.6 (3) |
C10—C11—C12—C13 | 0.8 (5) | C63—C64—C65—C70 | −164.5 (3) |
C11—C12—C13—C14 | 0.6 (5) | C59—C64—C65—C70 | 13.4 (5) |
C12—C13—C14—C9 | −1.2 (5) | C70—C65—C66—C67 | 3.0 (6) |
C12—C13—C14—C1 | −178.7 (3) | C64—C65—C66—C67 | −175.1 (4) |
C10—C9—C14—C13 | 0.4 (5) | C65—C66—C67—C68 | −0.1 (6) |
C8—C9—C14—C13 | −177.2 (3) | C66—C67—C68—C69 | −2.1 (6) |
C10—C9—C14—C1 | 178.0 (3) | C67—C68—C69—C70 | 1.3 (6) |
C8—C9—C14—C1 | 0.5 (5) | C66—C65—C70—C69 | −3.7 (5) |
N1—C1—C14—C13 | −14.7 (5) | C64—C65—C70—C69 | 174.3 (3) |
C2—C1—C14—C13 | 166.2 (3) | C66—C65—C70—C57 | 174.0 (3) |
N1—C1—C14—C9 | 167.7 (3) | C64—C65—C70—C57 | −7.9 (5) |
C2—C1—C14—C9 | −11.4 (5) | C68—C69—C70—C65 | 1.6 (5) |
N3—C15—C16—N4 | 26.0 (5) | C68—C69—C70—C57 | −176.0 (3) |
C28—C15—C16—N4 | −154.2 (3) | N9—C57—C70—C65 | 173.9 (3) |
N3—C15—C16—C17 | −153.7 (3) | C58—C57—C70—C65 | −9.0 (5) |
C28—C15—C16—C17 | 26.0 (4) | N9—C57—C70—C69 | −8.5 (6) |
N4—C16—C17—C22 | 166.5 (3) | C58—C57—C70—C69 | 168.6 (3) |
C15—C16—C17—C22 | −13.8 (4) | C77—C72—C73—C74 | 1.6 (7) |
N4—C16—C17—C18 | −14.7 (4) | C71—C72—C73—C74 | −178.3 (5) |
C15—C16—C17—C18 | 165.1 (3) | C72—C73—C74—C75 | 0.3 (7) |
C22—C17—C18—C19 | −1.0 (5) | C73—C74—C75—C76 | −1.4 (7) |
C16—C17—C18—C19 | −179.9 (3) | C74—C75—C76—C77 | 0.5 (8) |
C17—C18—C19—C20 | 1.6 (5) | C75—C76—C77—C72 | 1.5 (9) |
C18—C19—C20—C21 | −0.4 (5) | C73—C72—C77—C76 | −2.5 (8) |
C19—C20—C21—C22 | −1.3 (6) | C71—C72—C77—C76 | 177.3 (6) |
C18—C17—C22—C21 | −0.6 (5) | C84—C79—C80—C81 | 0.2 (4) |
C16—C17—C22—C21 | 178.2 (3) | C78—C79—C80—C81 | −179.8 (3) |
C18—C17—C22—C23 | 176.3 (3) | C79—C80—C81—C82 | −0.6 (6) |
C16—C17—C22—C23 | −4.9 (5) | C80—C81—C82—C83 | 0.7 (7) |
C20—C21—C22—C17 | 1.8 (5) | C81—C82—C83—C84 | −0.4 (8) |
C20—C21—C22—C23 | −175.1 (3) | C82—C83—C84—C79 | 0.1 (7) |
C17—C22—C23—C24 | −166.6 (3) | C80—C79—C84—C83 | 0.0 (5) |
C21—C22—C23—C24 | 10.2 (5) | C78—C79—C84—C83 | −180.0 (3) |
C17—C22—C23—C28 | 11.0 (5) | C84A—C79A—C80A—C81A | 0.3 (6) |
C21—C22—C23—C28 | −172.2 (3) | C78A—C79A—C80A—C81A | −179.9 (2) |
C28—C23—C24—C25 | −1.3 (5) | C82A—C81A—C80A—C79A | 0.0 (6) |
C22—C23—C24—C25 | 176.4 (3) | C80A—C81A—C82A—C83A | −0.5 (7) |
C23—C24—C25—C26 | −2.0 (6) | C81A—C82A—C83A—C84A | 0.5 (8) |
C24—C25—C26—C27 | 2.8 (6) | C80A—C79A—C84A—C83A | −0.2 (7) |
C25—C26—C27—C28 | −0.1 (6) | C78A—C79A—C84A—C83A | 180.0 (4) |
C26—C27—C28—C23 | −3.3 (5) | C82A—C83A—C84A—C79A | −0.2 (8) |
C26—C27—C28—C15 | −178.9 (3) | C14—C1—N1—O1 | −1.9 (5) |
C24—C23—C28—C27 | 3.9 (5) | C2—C1—N1—O1 | 177.3 (3) |
C22—C23—C28—C27 | −173.8 (3) | C14—C1—N1—Ni1 | 176.6 (3) |
C24—C23—C28—C15 | 179.6 (3) | C2—C1—N1—Ni1 | −4.2 (4) |
C22—C23—C28—C15 | 1.9 (5) | C3—C2—N2—O2 | −9.3 (5) |
N3—C15—C28—C27 | −24.8 (5) | C1—C2—N2—O2 | 177.6 (3) |
C16—C15—C28—C27 | 155.5 (3) | C3—C2—N2—Ni1 | 166.7 (3) |
N3—C15—C28—C23 | 159.6 (3) | C1—C2—N2—Ni1 | −6.4 (4) |
C16—C15—C28—C23 | −20.1 (4) | C16—C15—N3—O3 | 173.6 (3) |
N5—C29—C30—N6 | 28.4 (5) | C28—C15—N3—O3 | −6.2 (5) |
C42—C29—C30—N6 | −150.6 (3) | C16—C15—N3—Ni2 | −13.4 (4) |
N5—C29—C30—C31 | −151.3 (3) | C28—C15—N3—Ni2 | 166.8 (2) |
C42—C29—C30—C31 | 29.7 (4) | C15—C16—N4—O4 | −4.3 (5) |
N6—C30—C31—C32 | −24.0 (5) | C17—C16—N4—O4 | 175.4 (3) |
C29—C30—C31—C32 | 155.8 (3) | C30—C29—N5—O5 | 172.0 (3) |
N6—C30—C31—C36 | 155.9 (3) | C42—C29—N5—O5 | −9.0 (5) |
C29—C30—C31—C36 | −24.4 (5) | C30—C29—N5—Ni1 | −18.5 (4) |
C36—C31—C32—C33 | −1.1 (6) | C42—C29—N5—Ni1 | 160.5 (3) |
C30—C31—C32—C33 | 178.8 (4) | C29—C30—N6—O6 | −4.0 (5) |
C31—C32—C33—C34 | −0.1 (7) | C31—C30—N6—O6 | 175.7 (3) |
C32—C33—C34—C35 | 0.8 (7) | C44—C43—N7—O7 | 178.7 (3) |
C33—C34—C35—C36 | −0.3 (7) | C56—C43—N7—O7 | −3.4 (5) |
C32—C31—C36—C35 | 1.5 (5) | C44—C43—N7—Ni2 | −6.0 (4) |
C30—C31—C36—C35 | −178.3 (3) | C56—C43—N7—Ni2 | 172.0 (3) |
C32—C31—C36—C37 | −177.9 (3) | C43—C44—N8—O8 | 175.6 (3) |
C30—C31—C36—C37 | 2.3 (5) | C45—C44—N8—O8 | −8.5 (5) |
C34—C35—C36—C31 | −0.8 (6) | C43—C44—N8—Ni2 | −7.2 (4) |
C34—C35—C36—C37 | 178.5 (4) | C45—C44—N8—Ni2 | 168.7 (3) |
C31—C36—C37—C38 | −166.6 (3) | C70—C57—N9—O9 | −0.4 (5) |
C35—C36—C37—C38 | 14.1 (5) | C58—C57—N9—O9 | −177.7 (3) |
C31—C36—C37—C42 | 14.3 (5) | C70—C57—N9—Ni3 | 166.5 (3) |
C35—C36—C37—C42 | −165.1 (3) | C58—C57—N9—Ni3 | −10.8 (4) |
C42—C37—C38—C39 | 1.1 (5) | C59—C58—N10—O10 | −3.5 (5) |
C36—C37—C38—C39 | −178.0 (3) | C57—C58—N10—O10 | 178.9 (3) |
C37—C38—C39—C40 | 0.4 (6) | C59—C58—N10—Ni3 | 162.1 (3) |
C38—C39—C40—C41 | −1.6 (6) | C57—C58—N10—Ni3 | −15.6 (4) |
C39—C40—C41—C42 | 1.2 (6) | C2—N2—O2—Ni3 | 143.0 (3) |
C40—C41—C42—C37 | 0.3 (5) | Ni1—N2—O2—Ni3 | −32.7 (3) |
C40—C41—C42—C29 | −173.5 (3) | C16—N4—O4—Ni2 | −30.5 (4) |
C38—C37—C42—C41 | −1.5 (5) | C16—N4—O4—Ni3 | 148.7 (2) |
C36—C37—C42—C41 | 177.7 (3) | C30—N6—O6—Ni1 | −30.9 (4) |
C38—C37—C42—C29 | 172.6 (3) | C30—N6—O6—Ni3 | 145.4 (2) |
C36—C37—C42—C29 | −8.3 (5) | C44—N8—O8—Ni3 | 145.0 (3) |
N5—C29—C42—C41 | −18.5 (5) | Ni2—N8—O8—Ni3 | −32.1 (3) |
C30—C29—C42—C41 | 160.4 (3) | N6—O6—Ni1—N1 | −158.8 (6) |
N5—C29—C42—C37 | 167.6 (3) | Ni3—O6—Ni1—N1 | 24.9 (7) |
C30—C29—C42—C37 | −13.4 (4) | N6—O6—Ni1—N2 | −151.0 (3) |
N7—C43—C44—N8 | 8.4 (4) | Ni3—O6—Ni1—N2 | 32.64 (14) |
C56—C43—C44—N8 | −169.7 (3) | N6—O6—Ni1—N5 | 31.9 (3) |
N7—C43—C44—C45 | −167.8 (3) | Ni3—O6—Ni1—N5 | −144.41 (14) |
C56—C43—C44—C45 | 14.1 (5) | C1—N1—Ni1—O6 | 8.5 (8) |
N8—C44—C45—C46 | −6.1 (6) | O1—N1—Ni1—O6 | −173.0 (6) |
C43—C44—C45—C46 | 169.4 (3) | C1—N1—Ni1—N2 | 0.7 (3) |
N8—C44—C45—C50 | 178.3 (3) | O1—N1—Ni1—N2 | 179.1 (3) |
C43—C44—C45—C50 | −6.2 (5) | C1—N1—Ni1—N5 | 177.7 (3) |
C50—C45—C46—C47 | 1.8 (6) | O1—N1—Ni1—N5 | −3.9 (3) |
C44—C45—C46—C47 | −173.7 (4) | C2—N2—Ni1—O6 | −175.1 (2) |
C45—C46—C47—C48 | −1.8 (6) | O2—N2—Ni1—O6 | 0.8 (2) |
C46—C47—C48—C49 | 1.1 (7) | C2—N2—Ni1—N1 | 3.5 (2) |
C47—C48—C49—C50 | −0.4 (7) | O2—N2—Ni1—N1 | 179.4 (3) |
C48—C49—C50—C45 | 0.4 (6) | C29—N5—Ni1—O6 | −5.9 (3) |
C48—C49—C50—C51 | 179.7 (4) | O5—N5—Ni1—O6 | 163.6 (3) |
C46—C45—C50—C49 | −1.0 (5) | C29—N5—Ni1—N1 | 176.0 (3) |
C44—C45—C50—C49 | 174.6 (3) | O5—N5—Ni1—N1 | −14.5 (3) |
C46—C45—C50—C51 | 179.7 (3) | N4—O4—Ni2—N8 | −149.4 (3) |
C44—C45—C50—C51 | −4.7 (5) | Ni3—O4—Ni2—N8 | 31.36 (14) |
C49—C50—C51—C56 | −171.2 (4) | N4—O4—Ni2—N3 | 33.3 (3) |
C45—C50—C51—C56 | 8.0 (5) | Ni3—O4—Ni2—N3 | −145.90 (14) |
C49—C50—C51—C52 | 9.9 (6) | C43—N7—Ni2—N8 | 1.8 (3) |
C45—C50—C51—C52 | −170.8 (3) | O7—N7—Ni2—N8 | 177.1 (3) |
C56—C51—C52—C53 | −0.1 (6) | C43—N7—Ni2—N3 | 179.0 (3) |
C50—C51—C52—C53 | 178.7 (4) | O7—N7—Ni2—N3 | −5.7 (3) |
C51—C52—C53—C54 | 0.2 (6) | C44—N8—Ni2—O4 | −176.1 (3) |
C52—C53—C54—C55 | −0.1 (6) | O8—N8—Ni2—O4 | 1.1 (2) |
C53—C54—C55—C56 | −0.1 (6) | C44—N8—Ni2—N7 | 3.3 (2) |
C54—C55—C56—C51 | 0.2 (5) | O8—N8—Ni2—N7 | −179.5 (3) |
C54—C55—C56—C43 | −178.5 (3) | C15—N3—Ni2—O4 | −10.2 (3) |
C52—C51—C56—C55 | −0.1 (5) | O3—N3—Ni2—O4 | 162.8 (2) |
C50—C51—C56—C55 | −179.0 (3) | C15—N3—Ni2—N7 | 170.8 (3) |
C52—C51—C56—C43 | 178.7 (3) | O3—N3—Ni2—N7 | −16.1 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O5 | 1.29 (6) | 1.13 (6) | 2.405 (4) | 169 (6) |
O3—H2A···O7 | 1.17 (5) | 1.23 (5) | 2.402 (4) | 176 (5) |
O9—H3A···N4 | 0.86 (6) | 1.82 (6) | 2.672 (4) | 175 (7) |
O10—H4A···N6 | 1.04 (5) | 1.63 (5) | 2.657 (4) | 168 (4) |
[Ni3(C28H16BF2N4O4)2(C14H10N2O2)]·3CH2Cl2 | F(000) = 2968 |
Mr = 1456.88 | Dx = 1.473 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54184 Å |
a = 15.6414 (8) Å | Cell parameters from 25728 reflections |
b = 30.8358 (11) Å | θ = 3.4–76.5° |
c = 14.7380 (8) Å | µ = 1.67 mm−1 |
β = 112.411 (6)° | T = 100 K |
V = 6571.5 (6) Å3 | Block, red |
Z = 4 | 0.29 × 0.07 × 0.04 mm |
Agilent SuperNova Dual Source diffractometer with an Atlas detector | 13041 independent reflections |
Radiation source: sealed X-ray tube | 8782 reflections with I > 2σ(I) |
Detector resolution: 5.2940 pixels mm-1 | Rint = 0.060 |
ω scans | θmax = 75.0°, θmin = 3.4° |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | h = −19→19 |
Tmin = 0.303, Tmax = 1.000 | k = −26→38 |
25337 measured reflections | l = −18→18 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.077 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.226 | w = 1/[σ2(Fo2) + (0.108P)2 + 8.2009P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.006 |
13041 reflections | Δρmax = 1.16 e Å−3 |
896 parameters | Δρmin = −0.83 e Å−3 |
Experimental. CrysAlisPro. (Agilent, 2014). Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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. Three molecules of what appeared to be dichloromethane were found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). |
x | y | z | Uiso*/Ueq | ||
C1 | 0.3411 (3) | 0.33690 (15) | 0.7321 (4) | 0.0323 (10) | |
C2 | 0.4326 (3) | 0.33998 (16) | 0.7254 (4) | 0.0336 (11) | |
C3 | 0.4765 (4) | 0.29952 (16) | 0.7127 (4) | 0.0347 (11) | |
C4 | 0.5720 (4) | 0.29722 (18) | 0.7393 (4) | 0.0423 (12) | |
H4 | 0.6093 | 0.3220 | 0.7661 | 0.051* | |
C5 | 0.6130 (4) | 0.25876 (18) | 0.7267 (5) | 0.0499 (14) | |
H5 | 0.6781 | 0.2571 | 0.7446 | 0.060* | |
C6 | 0.5574 (4) | 0.22266 (18) | 0.6875 (5) | 0.0498 (15) | |
H6 | 0.5847 | 0.1963 | 0.6785 | 0.060* | |
C7 | 0.4637 (4) | 0.22483 (17) | 0.6619 (4) | 0.0460 (14) | |
H7 | 0.4274 | 0.1997 | 0.6361 | 0.055* | |
C8 | 0.4198 (4) | 0.26291 (15) | 0.6727 (4) | 0.0362 (11) | |
C9 | 0.3201 (4) | 0.26641 (15) | 0.6448 (4) | 0.0357 (11) | |
C10 | 0.2594 (4) | 0.23476 (16) | 0.5841 (4) | 0.0394 (12) | |
H10 | 0.2844 | 0.2106 | 0.5627 | 0.047* | |
C11 | 0.1655 (4) | 0.23823 (18) | 0.5555 (4) | 0.0438 (13) | |
H11 | 0.1267 | 0.2162 | 0.5158 | 0.053* | |
C12 | 0.1264 (4) | 0.27305 (18) | 0.5831 (4) | 0.0422 (12) | |
H12 | 0.0611 | 0.2754 | 0.5620 | 0.051* | |
C13 | 0.1837 (4) | 0.30485 (16) | 0.6426 (4) | 0.0361 (11) | |
H13 | 0.1571 | 0.3291 | 0.6619 | 0.043* | |
C14 | 0.2797 (4) | 0.30177 (15) | 0.6744 (4) | 0.0336 (11) | |
C15 | 0.2126 (3) | 0.36498 (16) | 0.4672 (3) | 0.0310 (10) | |
C16 | 0.3085 (3) | 0.37760 (15) | 0.4870 (3) | 0.0295 (10) | |
C17 | 0.3700 (3) | 0.34790 (16) | 0.4634 (3) | 0.0304 (10) | |
C18 | 0.4630 (3) | 0.35767 (17) | 0.4827 (4) | 0.0352 (11) | |
H18 | 0.4869 | 0.3853 | 0.5083 | 0.042* | |
C19 | 0.5208 (4) | 0.32743 (18) | 0.4649 (4) | 0.0442 (13) | |
H19 | 0.5832 | 0.3346 | 0.4770 | 0.053* | |
C20 | 0.4864 (4) | 0.28685 (19) | 0.4294 (4) | 0.0472 (14) | |
H20 | 0.5261 | 0.2657 | 0.4196 | 0.057* | |
C21 | 0.3950 (4) | 0.27698 (18) | 0.4081 (4) | 0.0423 (12) | |
H21 | 0.3725 | 0.2491 | 0.3827 | 0.051* | |
C22 | 0.3341 (3) | 0.30700 (16) | 0.4230 (4) | 0.0330 (10) | |
C23 | 0.2352 (4) | 0.29719 (16) | 0.3911 (4) | 0.0335 (10) | |
C24 | 0.1973 (4) | 0.25910 (18) | 0.3381 (4) | 0.0423 (12) | |
H24 | 0.2378 | 0.2386 | 0.3275 | 0.051* | |
C25 | 0.1044 (4) | 0.25044 (19) | 0.3013 (4) | 0.0464 (13) | |
H25 | 0.0816 | 0.2242 | 0.2667 | 0.056* | |
C26 | 0.0436 (4) | 0.28018 (19) | 0.3149 (4) | 0.0455 (13) | |
H26 | −0.0211 | 0.2750 | 0.2874 | 0.055* | |
C27 | 0.0781 (4) | 0.31762 (18) | 0.3690 (4) | 0.0380 (11) | |
H27 | 0.0365 | 0.3376 | 0.3794 | 0.046* | |
C28 | 0.1730 (3) | 0.32636 (16) | 0.4084 (4) | 0.0341 (11) | |
C29 | 0.3296 (3) | 0.47670 (15) | 0.9399 (4) | 0.0325 (10) | |
C30 | 0.3915 (3) | 0.50074 (15) | 0.9040 (3) | 0.0316 (10) | |
C31 | 0.4137 (3) | 0.54622 (15) | 0.9300 (3) | 0.0322 (10) | |
C32 | 0.4728 (4) | 0.57048 (16) | 0.8987 (4) | 0.0386 (12) | |
H32 | 0.4988 | 0.5573 | 0.8569 | 0.046* | |
C33 | 0.4942 (4) | 0.61279 (17) | 0.9267 (4) | 0.0448 (13) | |
H33 | 0.5354 | 0.6284 | 0.9053 | 0.054* | |
C34 | 0.4558 (5) | 0.63252 (18) | 0.9862 (5) | 0.0557 (17) | |
H34 | 0.4704 | 0.6618 | 1.0061 | 0.067* | |
C35 | 0.3969 (4) | 0.60974 (17) | 1.0163 (4) | 0.0454 (14) | |
H35 | 0.3712 | 0.6239 | 1.0573 | 0.055* | |
C36 | 0.3721 (4) | 0.56675 (16) | 0.9903 (3) | 0.0340 (11) | |
C37 | 0.3088 (4) | 0.54261 (16) | 1.0242 (4) | 0.0360 (11) | |
C38 | 0.2666 (4) | 0.56390 (18) | 1.0798 (4) | 0.0418 (13) | |
H38 | 0.2772 | 0.5941 | 1.0922 | 0.050* | |
C39 | 0.2105 (4) | 0.5425 (2) | 1.1168 (4) | 0.0497 (15) | |
H39 | 0.1828 | 0.5579 | 1.1545 | 0.060* | |
C40 | 0.1938 (4) | 0.4987 (2) | 1.0998 (4) | 0.0443 (13) | |
H40 | 0.1552 | 0.4838 | 1.1261 | 0.053* | |
C41 | 0.2339 (4) | 0.47662 (17) | 1.0439 (4) | 0.0372 (11) | |
H41 | 0.2230 | 0.4464 | 1.0326 | 0.045* | |
C42 | 0.2897 (4) | 0.49811 (16) | 1.0043 (3) | 0.0355 (11) | |
C43 | 0.1661 (3) | 0.49600 (19) | 0.6807 (4) | 0.0400 (12) | |
C44 | 0.2317 (3) | 0.52960 (18) | 0.6755 (4) | 0.0392 (12) | |
C45 | 0.2153 (4) | 0.5756 (2) | 0.6941 (4) | 0.0511 (16) | |
C46 | 0.2581 (4) | 0.6091 (2) | 0.6633 (5) | 0.0581 (18) | |
H46 | 0.2979 | 0.6023 | 0.6301 | 0.070* | |
C47 | 0.2434 (5) | 0.6522 (2) | 0.6804 (7) | 0.077 (3) | |
H47 | 0.2730 | 0.6749 | 0.6597 | 0.093* | |
C48 | 0.1844 (5) | 0.6615 (3) | 0.7286 (7) | 0.094 (3) | |
H48 | 0.1729 | 0.6908 | 0.7403 | 0.112* | |
C49 | 0.1427 (5) | 0.6285 (3) | 0.7595 (6) | 0.083 (3) | |
H49 | 0.1032 | 0.6356 | 0.7928 | 0.100* | |
C50 | 0.1571 (4) | 0.5845 (2) | 0.7429 (5) | 0.061 (2) | |
C51 | 0.1151 (4) | 0.5488 (3) | 0.7768 (4) | 0.062 (2) | |
C52 | 0.0734 (5) | 0.5578 (3) | 0.8439 (5) | 0.073 (2) | |
H52 | 0.0721 | 0.5866 | 0.8658 | 0.088* | |
C53 | 0.0348 (5) | 0.5250 (4) | 0.8776 (5) | 0.088 (3) | |
H53 | 0.0047 | 0.5317 | 0.9209 | 0.105* | |
C54 | 0.0385 (4) | 0.4820 (4) | 0.8502 (5) | 0.077 (3) | |
H54 | 0.0127 | 0.4596 | 0.8761 | 0.093* | |
C55 | 0.0804 (4) | 0.4722 (3) | 0.7841 (4) | 0.0604 (19) | |
H55 | 0.0838 | 0.4430 | 0.7650 | 0.072* | |
C56 | 0.1175 (4) | 0.5059 (2) | 0.7462 (4) | 0.0500 (16) | |
C57 | 0.6326 (3) | 0.48466 (16) | 0.6652 (4) | 0.0315 (10) | |
C58 | 0.5935 (3) | 0.52870 (16) | 0.6698 (3) | 0.0315 (10) | |
C59 | 0.6591 (3) | 0.56487 (15) | 0.7051 (3) | 0.0304 (10) | |
C60 | 0.6390 (4) | 0.60134 (17) | 0.7479 (4) | 0.0395 (12) | |
H60 | 0.5788 | 0.6050 | 0.7481 | 0.047* | |
C61 | 0.7056 (4) | 0.63235 (18) | 0.7902 (5) | 0.0463 (13) | |
H61 | 0.6915 | 0.6570 | 0.8207 | 0.056* | |
C62 | 0.7926 (4) | 0.62788 (17) | 0.7885 (4) | 0.0436 (13) | |
H62 | 0.8380 | 0.6496 | 0.8171 | 0.052* | |
C63 | 0.8141 (4) | 0.59185 (17) | 0.7452 (4) | 0.0363 (11) | |
H63 | 0.8743 | 0.5889 | 0.7446 | 0.044* | |
C64 | 0.7473 (3) | 0.55957 (15) | 0.7021 (3) | 0.0298 (10) | |
C65 | 0.7705 (3) | 0.52067 (16) | 0.6569 (3) | 0.0320 (10) | |
C66 | 0.8480 (3) | 0.51969 (17) | 0.6315 (4) | 0.0346 (11) | |
H66 | 0.8867 | 0.5445 | 0.6430 | 0.041* | |
C67 | 0.8690 (3) | 0.48300 (19) | 0.5900 (4) | 0.0390 (12) | |
H67 | 0.9216 | 0.4828 | 0.5728 | 0.047* | |
C68 | 0.8134 (4) | 0.44667 (18) | 0.5735 (4) | 0.0409 (12) | |
H68 | 0.8281 | 0.4215 | 0.5450 | 0.049* | |
C69 | 0.7366 (3) | 0.44671 (18) | 0.5982 (4) | 0.0389 (12) | |
H69 | 0.6988 | 0.4216 | 0.5867 | 0.047* | |
C70 | 0.7146 (3) | 0.48316 (16) | 0.6398 (4) | 0.0332 (11) | |
N1 | 0.3219 (3) | 0.36493 (12) | 0.7882 (3) | 0.0321 (9) | |
N2 | 0.4789 (3) | 0.37504 (13) | 0.7289 (3) | 0.0339 (9) | |
N3 | 0.1712 (3) | 0.39220 (13) | 0.5053 (3) | 0.0316 (9) | |
N4 | 0.3296 (3) | 0.41530 (13) | 0.5315 (3) | 0.0290 (8) | |
N5 | 0.3158 (3) | 0.43671 (13) | 0.9063 (3) | 0.0337 (9) | |
N6 | 0.4215 (3) | 0.47684 (11) | 0.8493 (3) | 0.0288 (8) | |
N7 | 0.1558 (3) | 0.46191 (15) | 0.6258 (3) | 0.0364 (10) | |
N8 | 0.3047 (3) | 0.52333 (14) | 0.6565 (3) | 0.0359 (9) | |
N9 | 0.5880 (3) | 0.45401 (13) | 0.6849 (3) | 0.0346 (9) | |
N10 | 0.5047 (3) | 0.52610 (13) | 0.6498 (3) | 0.0378 (10) | |
O1 | 0.2406 (3) | 0.35856 (11) | 0.8007 (3) | 0.0397 (8) | |
O2 | 0.4437 (2) | 0.41270 (10) | 0.7481 (3) | 0.0329 (7) | |
O3 | 0.0833 (2) | 0.38339 (12) | 0.4931 (3) | 0.0436 (9) | |
O4 | 0.4102 (2) | 0.43359 (11) | 0.5495 (2) | 0.0319 (7) | |
O5 | 0.2580 (3) | 0.41112 (11) | 0.9310 (3) | 0.0422 (9) | |
O6 | 0.4795 (2) | 0.49203 (10) | 0.8119 (3) | 0.0324 (7) | |
O7 | 0.0898 (3) | 0.43277 (13) | 0.6260 (3) | 0.0448 (9) | |
O8 | 0.3220 (2) | 0.48291 (11) | 0.6323 (3) | 0.0347 (8) | |
O9 | 0.6191 (2) | 0.41229 (11) | 0.6839 (3) | 0.0373 (8) | |
H1A | 0.582 (4) | 0.3945 (14) | 0.694 (5) | 0.056* | |
O10 | 0.4608 (3) | 0.56409 (12) | 0.6526 (3) | 0.0463 (9) | |
H2A | 0.395 (5) | 0.5572 (5) | 0.654 (5) | 0.069* | |
Ni1 | 0.37718 (6) | 0.41976 (2) | 0.82564 (6) | 0.0306 (2) | |
Ni2 | 0.23963 (5) | 0.44031 (3) | 0.57163 (6) | 0.0301 (2) | |
Ni3 | 0.45817 (5) | 0.46682 (2) | 0.67739 (6) | 0.0277 (2) | |
F1 | 0.3252 (3) | 0.34124 (11) | 0.9649 (3) | 0.0556 (9) | |
F2 | 0.1678 (3) | 0.35125 (12) | 0.9084 (3) | 0.0601 (10) | |
F3 | −0.0369 (2) | 0.39118 (12) | 0.5394 (3) | 0.0613 (10) | |
F4 | 0.0009 (2) | 0.44772 (11) | 0.4612 (3) | 0.0506 (8) | |
B1 | 0.2493 (5) | 0.3650 (2) | 0.9034 (6) | 0.0486 (16) | |
B2 | 0.0335 (4) | 0.4143 (2) | 0.5275 (6) | 0.0437 (15) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.044 (3) | 0.021 (2) | 0.029 (2) | 0.0022 (19) | 0.011 (2) | 0.0065 (19) |
C2 | 0.042 (3) | 0.026 (2) | 0.030 (3) | 0.002 (2) | 0.011 (2) | 0.004 (2) |
C3 | 0.052 (3) | 0.023 (2) | 0.028 (2) | 0.003 (2) | 0.014 (2) | 0.000 (2) |
C4 | 0.051 (3) | 0.030 (3) | 0.042 (3) | 0.005 (2) | 0.013 (2) | −0.002 (2) |
C5 | 0.058 (3) | 0.035 (3) | 0.052 (4) | 0.010 (3) | 0.015 (3) | −0.004 (3) |
C6 | 0.064 (4) | 0.029 (3) | 0.055 (4) | 0.017 (3) | 0.022 (3) | −0.001 (3) |
C7 | 0.068 (4) | 0.024 (3) | 0.038 (3) | 0.001 (2) | 0.012 (3) | −0.002 (2) |
C8 | 0.061 (3) | 0.016 (2) | 0.029 (3) | 0.001 (2) | 0.015 (2) | 0.0017 (19) |
C9 | 0.058 (3) | 0.020 (2) | 0.028 (2) | −0.002 (2) | 0.014 (2) | 0.006 (2) |
C10 | 0.065 (3) | 0.019 (2) | 0.032 (3) | −0.006 (2) | 0.016 (2) | 0.002 (2) |
C11 | 0.059 (3) | 0.033 (3) | 0.035 (3) | −0.016 (2) | 0.014 (2) | 0.001 (2) |
C12 | 0.054 (3) | 0.036 (3) | 0.036 (3) | −0.010 (2) | 0.015 (2) | 0.002 (2) |
C13 | 0.049 (3) | 0.028 (3) | 0.031 (3) | −0.005 (2) | 0.015 (2) | 0.003 (2) |
C14 | 0.049 (3) | 0.023 (2) | 0.024 (2) | −0.006 (2) | 0.010 (2) | 0.0060 (19) |
C15 | 0.036 (2) | 0.032 (3) | 0.023 (2) | 0.0051 (19) | 0.0079 (18) | 0.006 (2) |
C16 | 0.041 (2) | 0.026 (2) | 0.025 (2) | 0.0059 (19) | 0.0159 (19) | 0.0028 (19) |
C17 | 0.041 (2) | 0.029 (2) | 0.022 (2) | 0.0046 (19) | 0.0133 (19) | 0.0010 (19) |
C18 | 0.039 (2) | 0.034 (3) | 0.032 (3) | 0.001 (2) | 0.013 (2) | −0.002 (2) |
C19 | 0.041 (3) | 0.041 (3) | 0.049 (3) | 0.006 (2) | 0.016 (2) | −0.007 (3) |
C20 | 0.050 (3) | 0.041 (3) | 0.050 (3) | 0.011 (2) | 0.018 (3) | −0.010 (3) |
C21 | 0.048 (3) | 0.033 (3) | 0.044 (3) | 0.001 (2) | 0.015 (2) | −0.010 (2) |
C22 | 0.045 (3) | 0.030 (3) | 0.025 (2) | 0.002 (2) | 0.015 (2) | −0.002 (2) |
C23 | 0.048 (3) | 0.029 (3) | 0.026 (2) | 0.000 (2) | 0.016 (2) | 0.003 (2) |
C24 | 0.054 (3) | 0.038 (3) | 0.040 (3) | −0.005 (2) | 0.023 (3) | −0.009 (2) |
C25 | 0.061 (3) | 0.042 (3) | 0.038 (3) | −0.013 (3) | 0.021 (3) | −0.014 (3) |
C26 | 0.050 (3) | 0.049 (3) | 0.033 (3) | −0.011 (3) | 0.012 (2) | −0.005 (3) |
C27 | 0.043 (3) | 0.037 (3) | 0.033 (3) | 0.002 (2) | 0.013 (2) | 0.004 (2) |
C28 | 0.042 (3) | 0.029 (2) | 0.028 (2) | 0.002 (2) | 0.010 (2) | 0.008 (2) |
C29 | 0.045 (3) | 0.023 (2) | 0.026 (2) | 0.0069 (19) | 0.011 (2) | 0.0031 (19) |
C30 | 0.042 (2) | 0.024 (2) | 0.025 (2) | 0.0043 (19) | 0.0094 (19) | 0.0014 (19) |
C31 | 0.048 (3) | 0.021 (2) | 0.021 (2) | 0.0047 (19) | 0.0066 (19) | 0.0026 (19) |
C32 | 0.058 (3) | 0.025 (2) | 0.030 (3) | 0.006 (2) | 0.014 (2) | −0.001 (2) |
C33 | 0.072 (4) | 0.023 (3) | 0.039 (3) | −0.004 (2) | 0.021 (3) | −0.001 (2) |
C34 | 0.095 (5) | 0.020 (3) | 0.051 (4) | −0.003 (3) | 0.027 (3) | −0.009 (3) |
C35 | 0.075 (4) | 0.028 (3) | 0.033 (3) | 0.006 (3) | 0.020 (3) | −0.006 (2) |
C36 | 0.050 (3) | 0.024 (2) | 0.023 (2) | 0.003 (2) | 0.009 (2) | −0.0012 (19) |
C37 | 0.045 (3) | 0.032 (3) | 0.021 (2) | 0.009 (2) | 0.002 (2) | 0.001 (2) |
C38 | 0.053 (3) | 0.038 (3) | 0.028 (3) | 0.009 (2) | 0.008 (2) | −0.009 (2) |
C39 | 0.065 (4) | 0.054 (4) | 0.030 (3) | 0.014 (3) | 0.018 (3) | −0.008 (3) |
C40 | 0.054 (3) | 0.054 (4) | 0.023 (2) | 0.011 (3) | 0.011 (2) | 0.004 (2) |
C41 | 0.046 (3) | 0.031 (3) | 0.033 (3) | 0.004 (2) | 0.013 (2) | 0.004 (2) |
C42 | 0.052 (3) | 0.028 (3) | 0.019 (2) | 0.010 (2) | 0.006 (2) | 0.0008 (19) |
C43 | 0.032 (2) | 0.056 (3) | 0.026 (2) | 0.014 (2) | 0.0044 (19) | −0.007 (2) |
C44 | 0.032 (2) | 0.046 (3) | 0.031 (3) | 0.011 (2) | 0.003 (2) | −0.010 (2) |
C45 | 0.036 (3) | 0.057 (4) | 0.045 (3) | 0.017 (3) | −0.002 (2) | −0.021 (3) |
C46 | 0.043 (3) | 0.039 (3) | 0.074 (5) | 0.008 (2) | 0.002 (3) | −0.024 (3) |
C47 | 0.052 (4) | 0.056 (4) | 0.103 (6) | 0.009 (3) | 0.006 (4) | −0.036 (4) |
C48 | 0.054 (4) | 0.070 (5) | 0.123 (8) | 0.019 (4) | −0.005 (4) | −0.062 (5) |
C49 | 0.053 (4) | 0.093 (6) | 0.082 (6) | 0.024 (4) | 0.001 (4) | −0.048 (5) |
C50 | 0.037 (3) | 0.080 (5) | 0.048 (4) | 0.018 (3) | −0.003 (3) | −0.034 (4) |
C51 | 0.043 (3) | 0.104 (6) | 0.028 (3) | 0.023 (3) | 0.002 (2) | −0.024 (3) |
C52 | 0.045 (3) | 0.129 (7) | 0.036 (3) | 0.022 (4) | 0.005 (3) | −0.028 (4) |
C53 | 0.041 (3) | 0.186 (11) | 0.031 (3) | 0.028 (5) | 0.007 (3) | −0.022 (5) |
C54 | 0.045 (3) | 0.155 (9) | 0.028 (3) | 0.007 (4) | 0.009 (3) | −0.001 (4) |
C55 | 0.037 (3) | 0.115 (6) | 0.025 (3) | 0.006 (3) | 0.007 (2) | −0.010 (3) |
C56 | 0.031 (2) | 0.087 (5) | 0.027 (3) | 0.013 (3) | 0.006 (2) | −0.012 (3) |
C57 | 0.034 (2) | 0.031 (3) | 0.027 (2) | 0.0035 (19) | 0.0096 (19) | −0.003 (2) |
C58 | 0.037 (2) | 0.034 (3) | 0.026 (2) | 0.000 (2) | 0.0141 (19) | −0.002 (2) |
C59 | 0.041 (2) | 0.027 (2) | 0.025 (2) | 0.0019 (19) | 0.0137 (19) | 0.0026 (19) |
C60 | 0.054 (3) | 0.032 (3) | 0.037 (3) | −0.002 (2) | 0.023 (2) | 0.001 (2) |
C61 | 0.065 (4) | 0.031 (3) | 0.048 (3) | 0.000 (3) | 0.028 (3) | −0.007 (3) |
C62 | 0.061 (3) | 0.027 (3) | 0.042 (3) | −0.012 (2) | 0.018 (3) | −0.004 (2) |
C63 | 0.044 (3) | 0.034 (3) | 0.030 (3) | −0.004 (2) | 0.012 (2) | 0.005 (2) |
C64 | 0.041 (2) | 0.028 (2) | 0.018 (2) | 0.0001 (19) | 0.0091 (18) | 0.0051 (19) |
C65 | 0.041 (2) | 0.031 (3) | 0.022 (2) | 0.001 (2) | 0.0104 (19) | 0.0010 (19) |
C66 | 0.037 (2) | 0.037 (3) | 0.028 (2) | 0.000 (2) | 0.0108 (19) | 0.006 (2) |
C67 | 0.033 (2) | 0.052 (3) | 0.031 (3) | 0.009 (2) | 0.011 (2) | 0.005 (2) |
C68 | 0.044 (3) | 0.042 (3) | 0.038 (3) | 0.002 (2) | 0.017 (2) | −0.011 (2) |
C69 | 0.039 (3) | 0.041 (3) | 0.036 (3) | −0.004 (2) | 0.013 (2) | −0.009 (2) |
C70 | 0.032 (2) | 0.034 (3) | 0.030 (2) | −0.0023 (19) | 0.0083 (19) | −0.003 (2) |
N1 | 0.042 (2) | 0.0176 (18) | 0.039 (2) | −0.0029 (16) | 0.0183 (18) | 0.0038 (17) |
N2 | 0.047 (2) | 0.020 (2) | 0.034 (2) | 0.0032 (17) | 0.0156 (18) | −0.0009 (17) |
N3 | 0.0329 (19) | 0.029 (2) | 0.032 (2) | −0.0009 (16) | 0.0119 (17) | 0.0026 (17) |
N4 | 0.0354 (19) | 0.027 (2) | 0.026 (2) | 0.0023 (16) | 0.0130 (16) | 0.0018 (16) |
N5 | 0.053 (2) | 0.0196 (19) | 0.032 (2) | 0.0056 (17) | 0.0206 (19) | 0.0067 (17) |
N6 | 0.038 (2) | 0.0146 (17) | 0.032 (2) | −0.0032 (15) | 0.0109 (16) | 0.0013 (16) |
N7 | 0.034 (2) | 0.046 (3) | 0.029 (2) | 0.0027 (18) | 0.0125 (17) | 0.0015 (19) |
N8 | 0.038 (2) | 0.032 (2) | 0.033 (2) | 0.0069 (17) | 0.0086 (17) | −0.0043 (18) |
N9 | 0.042 (2) | 0.027 (2) | 0.036 (2) | −0.0039 (17) | 0.0156 (18) | −0.0092 (18) |
N10 | 0.052 (2) | 0.025 (2) | 0.040 (2) | 0.0038 (18) | 0.021 (2) | −0.0010 (19) |
O1 | 0.049 (2) | 0.0295 (18) | 0.046 (2) | −0.0043 (15) | 0.0243 (17) | −0.0047 (16) |
O2 | 0.055 (2) | 0.0144 (15) | 0.0378 (19) | 0.0011 (13) | 0.0274 (16) | 0.0017 (14) |
O3 | 0.0344 (18) | 0.039 (2) | 0.058 (2) | −0.0016 (15) | 0.0185 (17) | −0.0068 (19) |
O4 | 0.0332 (16) | 0.0310 (17) | 0.0326 (18) | −0.0019 (13) | 0.0137 (14) | −0.0042 (15) |
O5 | 0.064 (2) | 0.0268 (18) | 0.047 (2) | −0.0021 (16) | 0.034 (2) | 0.0006 (17) |
O6 | 0.0429 (18) | 0.0201 (15) | 0.0347 (18) | −0.0032 (13) | 0.0155 (15) | −0.0033 (14) |
O7 | 0.043 (2) | 0.054 (2) | 0.043 (2) | −0.0077 (17) | 0.0235 (17) | −0.0037 (19) |
O8 | 0.0345 (16) | 0.0273 (17) | 0.041 (2) | 0.0049 (13) | 0.0123 (15) | −0.0044 (15) |
O9 | 0.0384 (18) | 0.0263 (17) | 0.048 (2) | 0.0018 (14) | 0.0167 (16) | −0.0074 (16) |
O10 | 0.057 (2) | 0.0255 (18) | 0.059 (3) | 0.0003 (16) | 0.025 (2) | 0.0035 (18) |
Ni1 | 0.0451 (5) | 0.0169 (4) | 0.0317 (4) | 0.0006 (3) | 0.0168 (4) | 0.0009 (3) |
Ni2 | 0.0342 (4) | 0.0274 (4) | 0.0293 (4) | 0.0031 (3) | 0.0127 (3) | −0.0014 (3) |
Ni3 | 0.0348 (4) | 0.0182 (4) | 0.0311 (4) | 0.0013 (3) | 0.0137 (3) | 0.0008 (3) |
F1 | 0.071 (2) | 0.0393 (18) | 0.058 (2) | 0.0011 (16) | 0.0272 (18) | 0.0146 (16) |
F2 | 0.072 (2) | 0.048 (2) | 0.072 (3) | −0.0111 (17) | 0.041 (2) | −0.0011 (19) |
F3 | 0.053 (2) | 0.056 (2) | 0.083 (3) | −0.0035 (16) | 0.0350 (19) | −0.004 (2) |
F4 | 0.0507 (18) | 0.0436 (19) | 0.049 (2) | 0.0051 (15) | 0.0097 (15) | −0.0025 (16) |
B1 | 0.061 (4) | 0.037 (4) | 0.051 (4) | −0.002 (3) | 0.025 (3) | −0.001 (3) |
B2 | 0.045 (3) | 0.035 (3) | 0.059 (4) | −0.005 (3) | 0.028 (3) | −0.003 (3) |
C1—N1 | 1.307 (6) | C44—C45 | 1.485 (8) |
C1—C2 | 1.475 (7) | C45—C50 | 1.385 (9) |
C1—C14 | 1.482 (7) | C45—C46 | 1.399 (10) |
C2—N2 | 1.291 (6) | C46—C47 | 1.388 (9) |
C2—C3 | 1.470 (7) | C46—H46 | 0.9500 |
C3—C4 | 1.394 (7) | C47—C48 | 1.392 (12) |
C3—C8 | 1.418 (7) | C47—H47 | 0.9500 |
C4—C5 | 1.394 (7) | C48—C49 | 1.375 (14) |
C4—H4 | 0.9500 | C48—H48 | 0.9500 |
C5—C6 | 1.396 (9) | C49—C50 | 1.413 (10) |
C5—H5 | 0.9500 | C49—H49 | 0.9500 |
C6—C7 | 1.367 (8) | C50—C51 | 1.464 (11) |
C6—H6 | 0.9500 | C51—C52 | 1.403 (9) |
C7—C8 | 1.400 (7) | C51—C56 | 1.405 (10) |
C7—H7 | 0.9500 | C52—C53 | 1.364 (13) |
C8—C9 | 1.458 (8) | C52—H52 | 0.9500 |
C9—C14 | 1.410 (7) | C53—C54 | 1.395 (13) |
C9—C10 | 1.417 (7) | C53—H53 | 0.9500 |
C10—C11 | 1.369 (8) | C54—C55 | 1.399 (9) |
C10—H10 | 0.9500 | C54—H54 | 0.9500 |
C11—C12 | 1.372 (8) | C55—C56 | 1.404 (10) |
C11—H11 | 0.9500 | C55—H55 | 0.9500 |
C12—C13 | 1.391 (7) | C57—N9 | 1.273 (6) |
C12—H12 | 0.9500 | C57—C70 | 1.466 (7) |
C13—C14 | 1.395 (7) | C57—C58 | 1.502 (7) |
C13—H13 | 0.9500 | C58—N10 | 1.308 (6) |
C15—N3 | 1.309 (6) | C58—C59 | 1.470 (7) |
C15—C28 | 1.464 (7) | C59—C60 | 1.383 (7) |
C15—C16 | 1.467 (7) | C59—C64 | 1.407 (7) |
C16—N4 | 1.314 (6) | C60—C61 | 1.376 (8) |
C16—C17 | 1.464 (6) | C60—H60 | 0.9500 |
C17—C18 | 1.404 (7) | C61—C62 | 1.377 (8) |
C17—C22 | 1.416 (7) | C61—H61 | 0.9500 |
C18—C19 | 1.391 (7) | C62—C63 | 1.385 (8) |
C18—H18 | 0.9500 | C62—H62 | 0.9500 |
C19—C20 | 1.384 (8) | C63—C64 | 1.407 (7) |
C19—H19 | 0.9500 | C63—H63 | 0.9500 |
C20—C21 | 1.376 (8) | C64—C65 | 1.483 (7) |
C20—H20 | 0.9500 | C65—C66 | 1.398 (7) |
C21—C22 | 1.404 (7) | C65—C70 | 1.414 (7) |
C21—H21 | 0.9500 | C66—C67 | 1.384 (7) |
C22—C23 | 1.465 (7) | C66—H66 | 0.9500 |
C23—C24 | 1.410 (7) | C67—C68 | 1.381 (8) |
C23—C28 | 1.418 (7) | C67—H67 | 0.9500 |
C24—C25 | 1.370 (8) | C68—C69 | 1.382 (7) |
C24—H24 | 0.9500 | C68—H68 | 0.9500 |
C25—C26 | 1.389 (8) | C69—C70 | 1.385 (7) |
C25—H25 | 0.9500 | C69—H69 | 0.9500 |
C26—C27 | 1.390 (8) | N1—O1 | 1.367 (5) |
C26—H26 | 0.9500 | N1—Ni1 | 1.883 (4) |
C27—C28 | 1.399 (7) | N2—O2 | 1.360 (5) |
C27—H27 | 0.9500 | N3—O3 | 1.346 (5) |
C29—N5 | 1.315 (6) | N3—Ni2 | 1.872 (4) |
C29—C30 | 1.469 (7) | N4—O4 | 1.312 (5) |
C29—C42 | 1.476 (7) | N4—Ni2 | 1.887 (4) |
C30—N6 | 1.304 (6) | N5—O5 | 1.350 (5) |
C30—C31 | 1.460 (7) | N5—Ni1 | 1.865 (4) |
C31—C32 | 1.398 (8) | N6—O6 | 1.314 (5) |
C31—C36 | 1.432 (7) | N6—Ni1 | 1.875 (4) |
C32—C33 | 1.371 (7) | N7—O7 | 1.370 (6) |
C32—H32 | 0.9500 | N7—Ni2 | 1.897 (4) |
C33—C34 | 1.379 (8) | N8—O8 | 1.352 (5) |
C33—H33 | 0.9500 | N9—O9 | 1.378 (5) |
C34—C35 | 1.361 (9) | N9—Ni3 | 2.029 (4) |
C34—H34 | 0.9500 | N10—O10 | 1.367 (5) |
C35—C36 | 1.393 (7) | N10—Ni3 | 2.064 (4) |
C35—H35 | 0.9500 | O1—B1 | 1.480 (8) |
C36—C37 | 1.470 (8) | O2—Ni1 | 1.829 (3) |
C37—C38 | 1.397 (7) | O2—Ni3 | 2.025 (3) |
C37—C42 | 1.411 (7) | O3—B2 | 1.440 (7) |
C38—C39 | 1.368 (9) | O4—Ni3 | 2.022 (3) |
C38—H38 | 0.9500 | O5—B1 | 1.471 (8) |
C39—C40 | 1.379 (9) | O6—Ni3 | 2.036 (3) |
C39—H39 | 0.9500 | O7—B2 | 1.493 (8) |
C40—C41 | 1.390 (8) | O8—Ni2 | 1.819 (3) |
C40—H40 | 0.9500 | O8—Ni3 | 2.036 (3) |
C41—C42 | 1.389 (8) | O9—H1A | 0.85 (7) |
C41—H41 | 0.9500 | O10—H2A | 1.06 (7) |
C43—N7 | 1.298 (7) | F1—B1 | 1.395 (8) |
C43—C56 | 1.471 (7) | F2—B1 | 1.372 (8) |
C43—C44 | 1.481 (8) | F3—B2 | 1.378 (7) |
C44—N8 | 1.290 (7) | F4—B2 | 1.377 (8) |
N1—C1—C2 | 117.6 (4) | C48—C49—H49 | 119.1 |
N1—C1—C14 | 126.3 (5) | C50—C49—H49 | 119.1 |
C2—C1—C14 | 116.2 (4) | C45—C50—C49 | 117.4 (8) |
N2—C2—C3 | 115.7 (5) | C45—C50—C51 | 119.8 (6) |
N2—C2—C1 | 126.5 (4) | C49—C50—C51 | 122.8 (7) |
C3—C2—C1 | 117.8 (4) | C52—C51—C56 | 119.2 (8) |
C4—C3—C8 | 120.7 (5) | C52—C51—C50 | 118.9 (7) |
C4—C3—C2 | 120.7 (5) | C56—C51—C50 | 121.9 (6) |
C8—C3—C2 | 118.7 (5) | C53—C52—C51 | 120.0 (8) |
C3—C4—C5 | 120.3 (5) | C53—C52—H52 | 120.0 |
C3—C4—H4 | 119.9 | C51—C52—H52 | 120.0 |
C5—C4—H4 | 119.9 | C52—C53—C54 | 121.7 (7) |
C4—C5—C6 | 119.2 (6) | C52—C53—H53 | 119.1 |
C4—C5—H5 | 120.4 | C54—C53—H53 | 119.1 |
C6—C5—H5 | 120.4 | C53—C54—C55 | 119.2 (9) |
C7—C6—C5 | 120.6 (5) | C53—C54—H54 | 120.4 |
C7—C6—H6 | 119.7 | C55—C54—H54 | 120.4 |
C5—C6—H6 | 119.7 | C54—C55—C56 | 119.5 (8) |
C6—C7—C8 | 122.0 (5) | C54—C55—H55 | 120.2 |
C6—C7—H7 | 119.0 | C56—C55—H55 | 120.2 |
C8—C7—H7 | 119.0 | C55—C56—C51 | 120.2 (6) |
C7—C8—C3 | 117.3 (5) | C55—C56—C43 | 120.3 (6) |
C7—C8—C9 | 123.3 (5) | C51—C56—C43 | 119.3 (6) |
C3—C8—C9 | 119.4 (4) | N9—C57—C70 | 130.1 (5) |
C14—C9—C10 | 117.2 (5) | N9—C57—C58 | 113.1 (4) |
C14—C9—C8 | 121.8 (4) | C70—C57—C58 | 116.8 (4) |
C10—C9—C8 | 121.0 (5) | N10—C58—C59 | 131.6 (4) |
C11—C10—C9 | 121.5 (5) | N10—C58—C57 | 110.5 (4) |
C11—C10—H10 | 119.3 | C59—C58—C57 | 117.4 (4) |
C9—C10—H10 | 119.3 | C60—C59—C64 | 120.4 (5) |
C10—C11—C12 | 121.1 (5) | C60—C59—C58 | 121.9 (4) |
C10—C11—H11 | 119.4 | C64—C59—C58 | 117.5 (4) |
C12—C11—H11 | 119.4 | C61—C60—C59 | 120.5 (5) |
C11—C12—C13 | 119.0 (5) | C61—C60—H60 | 119.8 |
C11—C12—H12 | 120.5 | C59—C60—H60 | 119.8 |
C13—C12—H12 | 120.5 | C60—C61—C62 | 120.3 (5) |
C12—C13—C14 | 121.1 (5) | C60—C61—H61 | 119.8 |
C12—C13—H13 | 119.5 | C62—C61—H61 | 119.8 |
C14—C13—H13 | 119.5 | C61—C62—C63 | 120.3 (5) |
C13—C14—C9 | 120.0 (5) | C61—C62—H62 | 119.9 |
C13—C14—C1 | 121.5 (5) | C63—C62—H62 | 119.9 |
C9—C14—C1 | 118.3 (5) | C62—C63—C64 | 120.4 (5) |
N3—C15—C28 | 127.5 (5) | C62—C63—H63 | 119.8 |
N3—C15—C16 | 112.3 (4) | C64—C63—H63 | 119.8 |
C28—C15—C16 | 120.1 (4) | C59—C64—C63 | 118.1 (5) |
N4—C16—C17 | 127.5 (4) | C59—C64—C65 | 121.3 (4) |
N4—C16—C15 | 112.2 (4) | C63—C64—C65 | 120.6 (4) |
C17—C16—C15 | 120.2 (4) | C66—C65—C70 | 118.4 (5) |
C18—C17—C22 | 119.4 (4) | C66—C65—C64 | 121.5 (4) |
C18—C17—C16 | 122.8 (5) | C70—C65—C64 | 120.0 (4) |
C22—C17—C16 | 117.7 (4) | C67—C66—C65 | 120.8 (5) |
C19—C18—C17 | 121.0 (5) | C67—C66—H66 | 119.6 |
C19—C18—H18 | 119.5 | C65—C66—H66 | 119.6 |
C17—C18—H18 | 119.5 | C68—C67—C66 | 120.1 (5) |
C20—C19—C18 | 119.4 (5) | C68—C67—H67 | 119.9 |
C20—C19—H19 | 120.3 | C66—C67—H67 | 119.9 |
C18—C19—H19 | 120.3 | C67—C68—C69 | 120.3 (5) |
C21—C20—C19 | 120.4 (5) | C67—C68—H68 | 119.9 |
C21—C20—H20 | 119.8 | C69—C68—H68 | 119.9 |
C19—C20—H20 | 119.8 | C68—C69—C70 | 120.4 (5) |
C20—C21—C22 | 121.8 (5) | C68—C69—H69 | 119.8 |
C20—C21—H21 | 119.1 | C70—C69—H69 | 119.8 |
C22—C21—H21 | 119.1 | C69—C70—C65 | 120.0 (5) |
C21—C22—C17 | 117.9 (5) | C69—C70—C57 | 121.9 (4) |
C21—C22—C23 | 120.6 (5) | C65—C70—C57 | 118.1 (4) |
C17—C22—C23 | 121.3 (4) | C1—N1—O1 | 116.1 (4) |
C24—C23—C28 | 117.1 (5) | C1—N1—Ni1 | 126.1 (3) |
C24—C23—C22 | 121.3 (5) | O1—N1—Ni1 | 115.8 (3) |
C28—C23—C22 | 121.6 (5) | C2—N2—O2 | 117.3 (4) |
C25—C24—C23 | 122.7 (5) | C15—N3—O3 | 117.4 (4) |
C25—C24—H24 | 118.6 | C15—N3—Ni2 | 117.0 (3) |
C23—C24—H24 | 118.6 | O3—N3—Ni2 | 125.6 (3) |
C24—C25—C26 | 119.7 (5) | O4—N4—C16 | 121.4 (4) |
C24—C25—H25 | 120.2 | O4—N4—Ni2 | 122.3 (3) |
C26—C25—H25 | 120.2 | C16—N4—Ni2 | 116.2 (3) |
C25—C26—C27 | 119.6 (5) | C29—N5—O5 | 118.5 (4) |
C25—C26—H26 | 120.2 | C29—N5—Ni1 | 116.9 (4) |
C27—C26—H26 | 120.2 | O5—N5—Ni1 | 124.6 (3) |
C26—C27—C28 | 121.1 (5) | C30—N6—O6 | 121.7 (4) |
C26—C27—H27 | 119.5 | C30—N6—Ni1 | 116.8 (3) |
C28—C27—H27 | 119.5 | O6—N6—Ni1 | 121.5 (3) |
C27—C28—C23 | 119.7 (5) | C43—N7—O7 | 116.4 (4) |
C27—C28—C15 | 123.0 (5) | C43—N7—Ni2 | 127.2 (4) |
C23—C28—C15 | 117.3 (4) | O7—N7—Ni2 | 114.4 (3) |
N5—C29—C30 | 112.0 (4) | C44—N8—O8 | 118.6 (4) |
N5—C29—C42 | 127.8 (5) | C57—N9—O9 | 117.6 (4) |
C30—C29—C42 | 120.3 (4) | C57—N9—Ni3 | 117.9 (3) |
N6—C30—C31 | 126.9 (5) | O9—N9—Ni3 | 122.1 (3) |
N6—C30—C29 | 112.3 (4) | C58—N10—O10 | 116.3 (4) |
C31—C30—C29 | 120.9 (4) | C58—N10—Ni3 | 115.7 (3) |
C32—C31—C36 | 118.8 (4) | O10—N10—Ni3 | 122.3 (3) |
C32—C31—C30 | 123.2 (5) | N1—O1—B1 | 113.0 (4) |
C36—C31—C30 | 118.0 (5) | N2—O2—Ni1 | 127.1 (3) |
C33—C32—C31 | 121.8 (5) | N2—O2—Ni3 | 117.6 (3) |
C33—C32—H32 | 119.1 | Ni1—O2—Ni3 | 115.17 (16) |
C31—C32—H32 | 119.1 | N3—O3—B2 | 118.8 (4) |
C32—C33—C34 | 119.7 (6) | N4—O4—Ni3 | 113.1 (3) |
C32—C33—H33 | 120.1 | N5—O5—B1 | 119.5 (4) |
C34—C33—H33 | 120.1 | N6—O6—Ni3 | 112.9 (3) |
C35—C34—C33 | 119.5 (5) | N7—O7—B2 | 114.4 (4) |
C35—C34—H34 | 120.2 | N8—O8—Ni2 | 128.3 (3) |
C33—C34—H34 | 120.2 | N8—O8—Ni3 | 115.4 (3) |
C34—C35—C36 | 123.6 (5) | Ni2—O8—Ni3 | 116.21 (17) |
C34—C35—H35 | 118.2 | N9—O9—H1A | 109.5 |
C36—C35—H35 | 118.2 | N10—O10—H2A | 109.5 |
C35—C36—C31 | 116.6 (5) | O2—Ni1—N5 | 170.30 (16) |
C35—C36—C37 | 122.7 (5) | O2—Ni1—N6 | 88.27 (16) |
C31—C36—C37 | 120.7 (4) | N5—Ni1—N6 | 82.07 (18) |
C38—C37—C42 | 118.0 (5) | O2—Ni1—N1 | 90.96 (16) |
C38—C37—C36 | 119.4 (5) | N5—Ni1—N1 | 98.53 (18) |
C42—C37—C36 | 122.6 (5) | N6—Ni1—N1 | 173.25 (18) |
C39—C38—C37 | 121.8 (5) | O8—Ni2—N3 | 170.42 (16) |
C39—C38—H38 | 119.1 | O8—Ni2—N4 | 88.60 (16) |
C37—C38—H38 | 119.1 | N3—Ni2—N4 | 81.88 (17) |
C38—C39—C40 | 120.3 (5) | O8—Ni2—N7 | 90.78 (17) |
C38—C39—H39 | 119.8 | N3—Ni2—N7 | 98.56 (19) |
C40—C39—H39 | 119.8 | N4—Ni2—N7 | 173.36 (18) |
C39—C40—C41 | 119.4 (6) | O4—Ni3—O2 | 89.28 (14) |
C39—C40—H40 | 120.3 | O4—Ni3—N9 | 87.74 (15) |
C41—C40—H40 | 120.3 | O2—Ni3—N9 | 96.72 (16) |
C42—C41—C40 | 120.9 (5) | O4—Ni3—O6 | 165.12 (14) |
C42—C41—H41 | 119.6 | O2—Ni3—O6 | 79.77 (13) |
C40—C41—H41 | 119.6 | N9—Ni3—O6 | 103.43 (16) |
C41—C42—C37 | 119.6 (5) | O4—Ni3—O8 | 81.29 (14) |
C41—C42—C29 | 123.0 (5) | O2—Ni3—O8 | 93.48 (15) |
C37—C42—C29 | 117.4 (5) | N9—Ni3—O8 | 164.91 (17) |
N7—C43—C56 | 127.1 (6) | O6—Ni3—O8 | 89.28 (14) |
N7—C43—C44 | 117.3 (5) | O4—Ni3—N10 | 107.36 (16) |
C56—C43—C44 | 115.5 (5) | O2—Ni3—N10 | 161.43 (17) |
N8—C44—C43 | 126.5 (5) | N9—Ni3—N10 | 76.28 (17) |
N8—C44—C45 | 114.4 (5) | O6—Ni3—N10 | 85.12 (16) |
C43—C44—C45 | 119.1 (5) | O8—Ni3—N10 | 97.08 (16) |
C50—C45—C46 | 120.8 (6) | F2—B1—F1 | 112.4 (5) |
C50—C45—C44 | 118.7 (7) | F2—B1—O5 | 105.9 (5) |
C46—C45—C44 | 120.5 (5) | F1—B1—O5 | 111.2 (5) |
C47—C46—C45 | 121.0 (7) | F2—B1—O1 | 106.8 (5) |
C47—C46—H46 | 119.5 | F1—B1—O1 | 108.5 (5) |
C45—C46—H46 | 119.5 | O5—B1—O1 | 112.0 (5) |
C46—C47—C48 | 118.5 (9) | F4—B2—F3 | 112.3 (5) |
C46—C47—H47 | 120.7 | F4—B2—O3 | 110.4 (5) |
C48—C47—H47 | 120.7 | F3—B2—O3 | 105.4 (5) |
C49—C48—C47 | 120.5 (7) | F4—B2—O7 | 109.1 (5) |
C49—C48—H48 | 119.7 | F3—B2—O7 | 106.1 (5) |
C47—C48—H48 | 119.7 | O3—B2—O7 | 113.4 (5) |
C48—C49—C50 | 121.7 (8) | ||
N1—C1—C2—N2 | −33.6 (7) | C54—C55—C56—C43 | 176.8 (5) |
C14—C1—C2—N2 | 146.8 (5) | C52—C51—C56—C55 | −1.5 (8) |
N1—C1—C2—C3 | 146.9 (5) | C50—C51—C56—C55 | 176.8 (5) |
C14—C1—C2—C3 | −32.8 (6) | C52—C51—C56—C43 | −176.3 (5) |
N2—C2—C3—C4 | 22.9 (7) | C50—C51—C56—C43 | 2.0 (8) |
C1—C2—C3—C4 | −157.5 (5) | N7—C43—C56—C55 | 24.5 (8) |
N2—C2—C3—C8 | −157.1 (5) | C44—C43—C56—C55 | −157.4 (5) |
C1—C2—C3—C8 | 22.6 (7) | N7—C43—C56—C51 | −160.7 (5) |
C8—C3—C4—C5 | 0.1 (8) | C44—C43—C56—C51 | 17.4 (7) |
C2—C3—C4—C5 | −179.8 (5) | N9—C57—C58—N10 | −28.2 (6) |
C3—C4—C5—C6 | −0.2 (9) | C70—C57—C58—N10 | 152.2 (4) |
C4—C5—C6—C7 | −0.2 (10) | N9—C57—C58—C59 | 145.3 (4) |
C5—C6—C7—C8 | 0.7 (10) | C70—C57—C58—C59 | −34.4 (6) |
C6—C7—C8—C3 | −0.7 (8) | N10—C58—C59—C60 | 17.3 (8) |
C6—C7—C8—C9 | 179.0 (5) | C57—C58—C59—C60 | −154.5 (5) |
C4—C3—C8—C7 | 0.3 (8) | N10—C58—C59—C64 | −168.3 (5) |
C2—C3—C8—C7 | −179.7 (5) | C57—C58—C59—C64 | 19.9 (6) |
C4—C3—C8—C9 | −179.5 (5) | C64—C59—C60—C61 | −1.7 (8) |
C2—C3—C8—C9 | 0.5 (7) | C58—C59—C60—C61 | 172.6 (5) |
C7—C8—C9—C14 | 166.8 (5) | C59—C60—C61—C62 | 1.4 (9) |
C3—C8—C9—C14 | −13.4 (7) | C60—C61—C62—C63 | −0.8 (9) |
C7—C8—C9—C10 | −15.0 (8) | C61—C62—C63—C64 | 0.3 (8) |
C3—C8—C9—C10 | 164.8 (5) | C60—C59—C64—C63 | 1.2 (7) |
C14—C9—C10—C11 | −0.2 (7) | C58—C59—C64—C63 | −173.3 (4) |
C8—C9—C10—C11 | −178.5 (5) | C60—C59—C64—C65 | 179.8 (4) |
C9—C10—C11—C12 | 1.3 (8) | C58—C59—C64—C65 | 5.3 (6) |
C10—C11—C12—C13 | −1.1 (8) | C62—C63—C64—C59 | −0.6 (7) |
C11—C12—C13—C14 | −0.1 (8) | C62—C63—C64—C65 | −179.2 (5) |
C12—C13—C14—C9 | 1.2 (7) | C59—C64—C65—C66 | 164.0 (5) |
C12—C13—C14—C1 | 175.8 (5) | C63—C64—C65—C66 | −17.5 (7) |
C10—C9—C14—C13 | −1.0 (7) | C59—C64—C65—C70 | −17.0 (7) |
C8—C9—C14—C13 | 177.2 (5) | C63—C64—C65—C70 | 161.6 (5) |
C10—C9—C14—C1 | −175.8 (4) | C70—C65—C66—C67 | 0.5 (7) |
C8—C9—C14—C1 | 2.5 (7) | C64—C65—C66—C67 | 179.6 (4) |
N1—C1—C14—C13 | 26.0 (7) | C65—C66—C67—C68 | −0.3 (8) |
C2—C1—C14—C13 | −154.4 (5) | C66—C67—C68—C69 | 0.0 (8) |
N1—C1—C14—C9 | −159.3 (5) | C67—C68—C69—C70 | 0.0 (8) |
C2—C1—C14—C9 | 20.3 (6) | C68—C69—C70—C65 | 0.2 (8) |
N3—C15—C16—N4 | −5.2 (6) | C68—C69—C70—C57 | 178.7 (5) |
C28—C15—C16—N4 | 173.2 (4) | C66—C65—C70—C69 | −0.5 (7) |
N3—C15—C16—C17 | 170.7 (4) | C64—C65—C70—C69 | −179.5 (4) |
C28—C15—C16—C17 | −10.9 (7) | C66—C65—C70—C57 | −179.1 (4) |
N4—C16—C17—C18 | −3.1 (8) | C64—C65—C70—C57 | 1.9 (7) |
C15—C16—C17—C18 | −178.4 (4) | N9—C57—C70—C69 | 24.8 (8) |
N4—C16—C17—C22 | 174.2 (5) | C58—C57—C70—C69 | −155.6 (5) |
C15—C16—C17—C22 | −1.0 (7) | N9—C57—C70—C65 | −156.6 (5) |
C22—C17—C18—C19 | −1.5 (8) | C58—C57—C70—C65 | 23.0 (6) |
C16—C17—C18—C19 | 175.9 (5) | C2—C1—N1—O1 | −173.7 (4) |
C17—C18—C19—C20 | −1.3 (9) | C14—C1—N1—O1 | 6.0 (7) |
C18—C19—C20—C21 | 2.5 (9) | C2—C1—N1—Ni1 | 23.2 (6) |
C19—C20—C21—C22 | −1.1 (9) | C14—C1—N1—Ni1 | −157.2 (4) |
C20—C21—C22—C17 | −1.7 (8) | C3—C2—N2—O2 | −175.1 (4) |
C20—C21—C22—C23 | 174.2 (5) | C1—C2—N2—O2 | 5.3 (7) |
C18—C17—C22—C21 | 2.9 (7) | C28—C15—N3—O3 | 2.9 (7) |
C16—C17—C22—C21 | −174.6 (5) | C16—C15—N3—O3 | −178.9 (4) |
C18—C17—C22—C23 | −172.9 (4) | C28—C15—N3—Ni2 | −176.9 (4) |
C16—C17—C22—C23 | 9.6 (7) | C16—C15—N3—Ni2 | 1.4 (5) |
C21—C22—C23—C24 | −5.0 (8) | C17—C16—N4—O4 | 9.2 (7) |
C17—C22—C23—C24 | 170.7 (5) | C15—C16—N4—O4 | −175.3 (4) |
C21—C22—C23—C28 | 177.8 (5) | C17—C16—N4—Ni2 | −168.8 (4) |
C17—C22—C23—C28 | −6.6 (7) | C15—C16—N4—Ni2 | 6.8 (5) |
C28—C23—C24—C25 | 2.0 (8) | C30—C29—N5—O5 | −178.1 (4) |
C22—C23—C24—C25 | −175.3 (5) | C42—C29—N5—O5 | 0.8 (8) |
C23—C24—C25—C26 | 0.8 (9) | C30—C29—N5—Ni1 | 1.0 (5) |
C24—C25—C26—C27 | −2.5 (9) | C42—C29—N5—Ni1 | 179.9 (4) |
C25—C26—C27—C28 | 1.4 (8) | C31—C30—N6—O6 | 1.7 (7) |
C26—C27—C28—C23 | 1.5 (8) | C29—C30—N6—O6 | −178.3 (4) |
C26—C27—C28—C15 | −178.9 (5) | C31—C30—N6—Ni1 | −178.0 (4) |
C24—C23—C28—C27 | −3.1 (7) | C29—C30—N6—Ni1 | 2.0 (5) |
C22—C23—C28—C27 | 174.2 (5) | C56—C43—N7—O7 | 2.8 (8) |
C24—C23—C28—C15 | 177.3 (5) | C44—C43—N7—O7 | −175.3 (4) |
C22—C23—C28—C15 | −5.4 (7) | C56—C43—N7—Ni2 | −160.1 (4) |
N3—C15—C28—C27 | 12.4 (8) | C44—C43—N7—Ni2 | 21.8 (7) |
C16—C15—C28—C27 | −165.7 (5) | C43—C44—N8—O8 | 4.6 (8) |
N3—C15—C28—C23 | −168.0 (5) | C45—C44—N8—O8 | −175.8 (4) |
C16—C15—C28—C23 | 13.9 (7) | C70—C57—N9—O9 | 0.4 (8) |
N5—C29—C30—N6 | −1.9 (6) | C58—C57—N9—O9 | −179.2 (4) |
C42—C29—C30—N6 | 179.1 (4) | C70—C57—N9—Ni3 | −162.4 (4) |
N5—C29—C30—C31 | 178.1 (4) | C58—C57—N9—Ni3 | 18.0 (5) |
C42—C29—C30—C31 | −0.9 (7) | C59—C58—N10—O10 | 7.1 (8) |
N6—C30—C31—C32 | −0.6 (8) | C57—C58—N10—O10 | 179.3 (4) |
C29—C30—C31—C32 | 179.4 (5) | C59—C58—N10—Ni3 | −147.0 (4) |
N6—C30—C31—C36 | 179.1 (5) | C57—C58—N10—Ni3 | 25.2 (5) |
C29—C30—C31—C36 | −0.9 (7) | C1—N1—O1—B1 | 137.4 (5) |
C36—C31—C32—C33 | 2.2 (8) | Ni1—N1—O1—B1 | −57.6 (5) |
C30—C31—C32—C33 | −178.1 (5) | C2—N2—O2—Ni1 | 32.8 (6) |
C31—C32—C33—C34 | −1.0 (9) | C2—N2—O2—Ni3 | −142.9 (4) |
C32—C33—C34—C35 | −0.1 (10) | C15—N3—O3—B2 | −175.3 (5) |
C33—C34—C35—C36 | 0.0 (10) | Ni2—N3—O3—B2 | 4.4 (7) |
C34—C35—C36—C31 | 1.2 (8) | C16—N4—O4—Ni3 | −145.0 (4) |
C34—C35—C36—C37 | 179.5 (6) | Ni2—N4—O4—Ni3 | 32.9 (4) |
C32—C31—C36—C35 | −2.2 (7) | C29—N5—O5—B1 | −173.4 (5) |
C30—C31—C36—C35 | 178.1 (5) | Ni1—N5—O5—B1 | 7.6 (7) |
C32—C31—C36—C37 | 179.4 (4) | C30—N6—O6—Ni3 | −146.0 (4) |
C30—C31—C36—C37 | −0.3 (7) | Ni1—N6—O6—Ni3 | 33.6 (4) |
C35—C36—C37—C38 | 4.1 (7) | C43—N7—O7—B2 | 139.1 (5) |
C31—C36—C37—C38 | −177.6 (4) | Ni2—N7—O7—B2 | −55.7 (5) |
C35—C36—C37—C42 | −174.7 (5) | C44—N8—O8—Ni2 | 29.2 (6) |
C31—C36—C37—C42 | 3.6 (7) | C44—N8—O8—Ni3 | −146.7 (4) |
C42—C37—C38—C39 | 1.9 (8) | N2—O2—Ni1—N6 | 152.7 (4) |
C36—C37—C38—C39 | −177.0 (5) | Ni3—O2—Ni1—N6 | −31.5 (2) |
C37—C38—C39—C40 | −0.1 (9) | N2—O2—Ni1—N1 | −34.0 (4) |
C38—C39—C40—C41 | −0.6 (8) | Ni3—O2—Ni1—N1 | 141.8 (2) |
C39—C40—C41—C42 | −0.6 (8) | C29—N5—Ni1—N6 | 0.0 (4) |
C40—C41—C42—C37 | 2.4 (8) | O5—N5—Ni1—N6 | 179.0 (4) |
C40—C41—C42—C29 | −176.4 (5) | C29—N5—Ni1—N1 | −173.2 (4) |
C38—C37—C42—C41 | −3.0 (7) | O5—N5—Ni1—N1 | 5.8 (4) |
C36—C37—C42—C41 | 175.8 (4) | C30—N6—Ni1—O2 | 177.9 (4) |
C38—C37—C42—C29 | 175.9 (4) | O6—N6—Ni1—O2 | −1.7 (3) |
C36—C37—C42—C29 | −5.2 (7) | C30—N6—Ni1—N5 | −1.2 (4) |
N5—C29—C42—C41 | 4.0 (8) | O6—N6—Ni1—N5 | 179.1 (4) |
C30—C29—C42—C41 | −177.2 (4) | C1—N1—Ni1—O2 | 4.2 (4) |
N5—C29—C42—C37 | −174.9 (5) | O1—N1—Ni1—O2 | −159.1 (3) |
C30—C29—C42—C37 | 3.9 (7) | C1—N1—Ni1—N5 | −177.8 (4) |
N7—C43—C44—N8 | −29.8 (8) | O1—N1—Ni1—N5 | 19.0 (4) |
C56—C43—C44—N8 | 151.8 (5) | N8—O8—Ni2—N4 | 157.2 (4) |
N7—C43—C44—C45 | 150.5 (5) | Ni3—O8—Ni2—N4 | −27.0 (2) |
C56—C43—C44—C45 | −27.8 (7) | N8—O8—Ni2—N7 | −29.5 (4) |
N8—C44—C45—C50 | −161.0 (5) | Ni3—O8—Ni2—N7 | 146.4 (2) |
C43—C44—C45—C50 | 18.7 (7) | C15—N3—Ni2—N4 | 1.7 (4) |
N8—C44—C45—C46 | 18.7 (8) | O3—N3—Ni2—N4 | −178.0 (4) |
C43—C44—C45—C46 | −161.6 (5) | C15—N3—Ni2—N7 | −171.6 (4) |
C50—C45—C46—C47 | −0.2 (9) | O3—N3—Ni2—N7 | 8.7 (4) |
C44—C45—C46—C47 | −179.9 (6) | O4—N4—Ni2—O8 | −3.9 (3) |
C45—C46—C47—C48 | −0.4 (11) | C16—N4—Ni2—O8 | 174.1 (4) |
C46—C47—C48—C49 | 0.8 (12) | O4—N4—Ni2—N3 | 177.1 (4) |
C47—C48—C49—C50 | −0.6 (12) | C16—N4—Ni2—N3 | −4.9 (3) |
C46—C45—C50—C49 | 0.4 (9) | C43—N7—Ni2—O8 | 2.3 (5) |
C44—C45—C50—C49 | −179.9 (5) | O7—N7—Ni2—O8 | −161.0 (3) |
C46—C45—C50—C51 | −178.3 (5) | C43—N7—Ni2—N3 | −179.8 (5) |
C44—C45—C50—C51 | 1.4 (8) | O7—N7—Ni2—N3 | 16.9 (4) |
C48—C49—C50—C45 | 0.0 (10) | N5—O5—B1—F2 | −161.0 (5) |
C48—C49—C50—C51 | 178.7 (7) | N5—O5—B1—F1 | 76.6 (7) |
C45—C50—C51—C52 | 166.2 (5) | N5—O5—B1—O1 | −45.0 (7) |
C49—C50—C51—C52 | −12.4 (9) | N1—O1—B1—F2 | −170.9 (4) |
C45—C50—C51—C56 | −12.1 (8) | N1—O1—B1—F1 | −49.6 (6) |
C49—C50—C51—C56 | 169.3 (6) | N1—O1—B1—O5 | 73.6 (6) |
C56—C51—C52—C53 | −0.8 (9) | N3—O3—B2—F4 | 80.1 (6) |
C50—C51—C52—C53 | −179.1 (6) | N3—O3—B2—F3 | −158.4 (5) |
C51—C52—C53—C54 | 2.5 (10) | N3—O3—B2—O7 | −42.7 (7) |
C52—C53—C54—C55 | −1.9 (10) | N7—O7—B2—F4 | −50.1 (6) |
C53—C54—C55—C56 | −0.4 (9) | N7—O7—B2—F3 | −171.4 (4) |
C54—C55—C56—C51 | 2.1 (8) | N7—O7—B2—O3 | 73.4 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H1A···N2 | 0.85 | 1.96 | 2.771 (6) | 158 |
O10—H2A···N8 | 1.06 | 1.77 | 2.765 (6) | 155 |
Acknowledgements
The data were collected using instrumentation purchased with funds provided by the National Science Foundation (grant No. 0741973). The chemistry was supported by the Robert A. Welch Foundation (grant F-0003).
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