research communications
η)-cycloheptadienyl][(1,2,3-η)-cycloheptatrienyl]cobalt(I)
of (18-crown-6)potassium(I) [(1,2,3,4,5-aDepartment of Chemistry, 120 Trustee Road, University of Rochester, Rochester, NY 14627, USA, and bDepartment of Chemistry, 207 Pleasant Street SE, University of Minnesota, Minneapolis, MN 55455, USA
*Correspondence e-mail: brennessel@chem.rochester.edu
The reaction of bis(anthracene)cobaltate(−I) with excess cycloheptatriene, C7H8, resulted in a new 18-electron cobaltate containing two different seven-membered ring ligands, based on single-crystal X-ray diffraction. The of this structure contains two independent cation–anion pairs of the title complex, [K(18-crown-6)][Co(η3-C7H7)(η5-C7H9)], where 18-crown-6 stands for 1,4,7,10,13,16-hexaoxacyclooctadecane (C12H24O6), in general positions and well separated. Each (18-crown-6)potassium cation is in contact with the η3-coordinating ligand of one cobaltate complex. Each η3-coordinating ligand behaves as an allylic anion whose exo-diene moiety is bent away from the allylic plane, and thus is not involved directly in the bonding. The metal-coordinating portions of the anionic η5 ligands are planar and one of these ligands is modeled as disordered over two positions, with occupancy ratio 0.699 (5):0.301 (5), such that one orientation is rotated by one carbon atom with respect to the other. The diffraction intensities were integrated according to non-merohedral [-1 0 0/0 -1 0/0.064 0 1], a 180° rotation about axis [001], and the masses of the twin domains refined to equal amounts. As both ligands are formally coordinated as anions, the cobalt atom is best considered to be CoI. This compound is of interest as the first to possess cycloheptatrienyl and cycloheptadienyl ligands in an anionic metal complex.
Keywords: crystal structure; 18-crown-6; hexaoxacyclooctadecane; cycloheptadienyl; cycloheptatrienyl; cobalt(I).
CCDC reference: 1049452
1. Chemical context
To date there is only one η6-C7H8)2 (Green & Walker, 1989), presumably because such molecules tend to isomerize. In the case of this zirconium species, room-temperature syntheses produced a mixture of it and its hydrogen-migrated isomer Zr(η7-C7H7)(η5-C7H9). For the titanium analog, although the homoleptic CHT complex was initially observed by NMR, no crystals were obtained, and it readily isomerized. Metal vapor co-condensation reactions of titanium and iron with CHT also led to the isomerized forms (Timms & Turney, 1976; Blackborow et al., 1976). Co-condensation of molybdenum atoms with CHT resulted in Mo(η6-C7H8)2, which could be isolated at room temperature, but was observed to isomerize to Mo(η7-C7H7)(η5-C7H9) with a half-life of ca 200 h (Green et al., 1989).
reported of a homoleptic cycloheptatriene (CHT) transition metal complex, Zr(Given the tendency for homoleptic CHT complexes to isomerize, we decided to investigate whether this would occur in the late transition metal low-valent cobalt system. The 18-electron anionic precursor bis(anthracene)cobaltate(−I) was chosen because it had been demonstrated that the anthracene ligands are quite labile (Brennessel et al., 2002; Brennessel & Ellis, 2012). Under an argon atmosphere, excess CHT was introduced dropwise to a cold tetrahydrofuran solution of bis(anthracene)cobaltate(−I). Red–brown single crystals of the isolated product suitable for an X-ray diffraction experiment revealed a new 18-electron cobalt complex anion containing two different cyclic ligands, [Co(η3-C7H7)(η5-C7H9)]−, which confirmed that isomerization had occurred and that both anthracene ligands had been displaced. As no spectroscopy had been performed, it is unknown if an anionic intermediate like `[Co(η-C7H8)2]−' was initially formed, and if formed, whether it had any lifetime in cold and/or room-temperature solutions.
2. Structural commentary
There are two independent contact ion pairs of [K(18-crown-6)][Co(η3-C7H7)(η5-C7H9)], (I), in the (Figs. 1 and 2). The potassium cations are complexed by 18-crown-6 cyclic and are in contact with carbon atoms of the η3-coordinating ligands of the cobalt anions, with K⋯C distances ranging from 3.207 (3) to 3.538 (4) Å. The longest K⋯C distance is well within the sum of the van der Waals radii for potassium and carbon of 4.45 Å (Bondi, 1964). The C7H7 ligands are bonded η3 to the cobalt atoms, and their Co—C and C C bond lengths are consistent with their formulations as anionic allylic ligands with exo-diene moieties, i.e., η3-cycloheptatrienyl ligands (see Table 1). Especially noteworthy are the lengths of the double bonds in the exo-diene portions, which are normal for C=C bonds and show that the exo-diene moieties are independent of the allylic coordination to the metal centers. The Co—C bond lengths have the typical long–short–long pattern seen in other η3-cycloheptatrienyl transition metal species (Table 2), and the exo-diene portions of these ligands are essentially planar and are bent away from the plane of the allylic regions by 28.0 (4) and 27.2 (4)°, for anions containing Co1 and Co2, respectively. Interestingly, the tropylium cation (CHT+) also has the formula C7H7; however, tropylium as a ligand is aromatic, and thus planar and with similar C C bond lengths. The η5-coordinating ligands are essentially planar in their cobalt-bonded regions with r.m.s. deviations from planarity of 0.050 and 0.051 Å for planes C8–C12 and C22–C26, respectively (see Figs. 1 and 2).
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With cobalt bound to three (`allyl') and five (`pentadienyl') carbon atoms of the seven-membered rings as described above, it is thought best to consider the cobalt atom as formally CoI with two anionic ligands. Extended Hückel MO calculations on [Fe(η3-C7H7)(CO)3]− (Hofmann, 1978), whose structure has been reported (Sepp et al., 1978), not only demonstrated that there is a preference for the metal to bind through the η3-allylic region of the ligand rather than through the diene segment, but showed that there is more charge localization on the ring for the former conformation over the latter.
The exact mechanism of isomerization has not been determined for (I), including whether the hydrogen transfer is intra- or intermolecular. In one DFT study on selected early transition metal complexes, the mechanism for hydrogen migration was determined to be intramolecular, and a metal hydride intermediate was predicted to be favored over a direct ligand-to-ligand transfer (Herbert et al., 2004). The same conclusion was reached in kinetic studies on similar molybdenum complexes (Green et al., 1989). If these studies can be extended to the cobalt system, then it could be proposed that the hydrogen migration occurs via a `[CoH(η-C7H7)(η-C7H8)]−' intermediate.
3. Database survey
As mentioned above, there is exactly one homoleptic CHT structure in the Cambridge Structural Database to date (CSD, Version 5.36, update No. 1, November 2014; Groom & Allen, 2014), namely Zr(η6-C7H8)2 (Green & Walker, 1989). All others have been structurally characterized after isomerization, including (I). There are 23 structures containing an η5-cycloheptadienyl ligand, but only 12 structures containing an η3-cycloheptatrienyl ligand bonded to a single metal atom. Of the latter, just three are anionic; they are of the form [AsPh4][M(CO)3(η3-C7H7)], M = Fe (Sepp et al., 1978) and M = Ru, Os (Astley et al., 1990). (I) is the first example of an anionic transition metal complex containing both cycloheptadienyl and cycloheptatrienyl ligands to be reported.
4. Synthesis and crystallization
All operations were performed under an atmosphere of 99.5% argon further purified by passage through columns of activated BASF catalyst and molecular sieves. Standard Schlenk techniques were employed for all reactions with a double manifold vacuum (0.01 Torr) line. Solutions were transferred via stainless steel double-ended needles (cannulas) and glass-covered magnetic stir bars were employed. Cycloheptatriene was distilled from Na/K alloy.
Excess cycloheptatriene was added dropwise to a deep pinkish-red solution of [K(18-crown-6)(THF)2][Co(η4-C14H10)2] (0.500 g, 0.579 mmol; Brennessel et al., 2002; Brennessel & Ellis, 2012) in THF (50 ml, 195 K). The solution was slowly warmed to room temperature, at which point it was deep yellowish brown. After the solvent was removed in vacuo and heptane (70 ml) was added, the slurry was filtered. The product was washed with pentane (20 ml) and dried in vacuo, yielding a blackish-gray solid [0.292 g, 92%, based on cobalt and using the formulation of (I)]. This product was only characterized by single-crystal X-ray diffraction. Red–brown blocks were grown from a pentane-layered THF solution at 273 K.
5. Refinement
Crystal data, data collection and structure . The stalled at R1 = 0.19, at which point the structure was examined for (Parsons et al., 2003). Non-merohedral was identified and the data were re-integrated accordingly. Application of [ 0 0 / 0 0 / 0.064 0 1], a 180° rotation about direction [001], reduced the R1 residual to its final value of 0.043 (Table 3). The mass ratio of the twin components refined to 0.5040 (7):0.4960 (7).
details are summarized in Table 3
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The η5-coordinating ligand C8–C14 is modeled as disordered over two positions with site occupancy ratio 0.699 (5):0.301 (5), such that the ethyl linkage is shifted by one carbon atom (see Fig. 4). Analogous bond lengths and angles between the two positions of the disordered ring were heavily restrained to be similar. Anisotropic displacement parameters for pairs of proximal atoms from the two components of the disorder were constrained to be equivalent (Sheldrick, 2015).
H-atom positions of ring-ligand carbon atoms, except those in the minor component of the disorder, were located in a difference map and refined freely. All other H atoms were placed geometrically and treated as riding atoms: methine and sp2, C—H = 1.00 Å, and methylene, C—H = 0.99 Å, with Uiso(H) = 1.2Ueq(C).
Supporting information
CCDC reference: 1049452
10.1107/S2056989015003151/bh2504sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S2056989015003151/bh2504Isup2.hkl
To date there is only one η6-C7H8)2 (Green & Walker, 1989), presumably because such molecules tend to isomerize. In the case of this zirconium species, room-temperature syntheses produced a mixture of it and its hydrogen-migrated isomer Zr(η7-C7H7)(η5-C7H9). For the titanium analog, although the homoleptic CHT complex was initially observed by NMR, no crystals were obtained, and it readily isomerized. Metal–vapor co-condensation reactions of titanium and iron with CHT also led to the isomerized forms (Timms & Turney, 1976; Blackborow et al., 1976). Co-condensation of molybdenum atoms with CHT resulted in Mo(η6-C7H8)2, which could be isolated at room temperature, but was observed to isomerize to Mo(η7-C7H7)(η5-C7H9) with a half-life of ca 200 hours (Green et al., 1989).
reported of a homoleptic cycloheptatriene (CHT) transition metal complex, Zr(Given the tendency for homoleptic CHT complexes to isomerize, we decided to investigate whether this would occur in the late transition metal low-valent cobalt system. The 18-electron anionic precursor bis(anthracene)cobaltate(-I) was chosen because it had been demonstrated that the anthracene ligands are quite labile (Brennessel et al., 2002; Brennessel & Ellis, 2012). Under an argon atmosphere, excess CHT was introduced dropwise to a cold tetrahydrofuran solution of bis(anthracene)cobaltate(-I). Red–brown single crystals of the isolated product suitable for an X-ray diffraction experiment revealed a new 18-electron cobalt complex anion containing two different cyclic ligands, [Co(η3-C7H7)(η5-C7H9)]-, which confirmed that isomerization had occurred and that both anthracene ligands had been displaced. As no spectroscopy had been performed, it is unknown if an anionic intermediate like `[Co(η-C7H8)2]-' was initially formed, and if formed, whether it had any lifetime in cold and/or room-temperature solutions.
There are two independent contact ion pairs of [K(18-crown-6)][Co(η3-C7H7)(η5-C7H9)], (I), in the (Figs. 1 and 2). The potassium cations are complexed by 18-crown-6 cyclic and are in contact with carbon atoms of the η3-coordinating ligands of the cobalt anions, with K···C distances ranging from 3.207 (3) to 3.538 (4) Å. The longest K···C distance is well within the sum of the van der Waals radii for potassium and carbon of 4.45 Å (Bondi, 1964). The C7H7 ligands are bonded η3 to the cobalt centers, and their Co—C and C≐C bond lengths are consistent with their formulations as anionic allylic ligands with exo-diene moieties, i.e., η3-cycloheptatrienyl ligands (see Table 1). Especially noteworthy are the lengths of the double bonds in the exo-diene portions, which are normal for C═C bonds and show that the exo-diene moieties are independent of the allylic coordination to the metal centers. The Co—C bond lengths have the typical long–short–long pattern seen in other η3-cycloheptatrienyl transition metal species (Table 2), and the exo-diene portions of these ligands are essentially planar and are bent away from the plane of the allylic regions by 28.0 (4) and 27.2 (4)°, for anions containing Co1 and Co2, respectively. Interestingly, the tropylium cation (CHT+) also has the formula C7H7; however, tropylium as a ligand is aromatic, and thus planar and with similar C≐C bond lengths. The η5-coordinating ligands are essentially planar in their cobalt-bonded regions with r.m.s. deviations from planarity of 0.050 and 0.051 Å for planes C8–C12 and C22–C26, respectively (see Figs. 1 and 2).
With cobalt bound to three (`allyl') and five (`pentadienyl') carbon atoms of the seven-membered rings as described above, it is thought best to consider the cobalt center as formally CoI with two anionic ligands. Extended Hückel MO calculations on [Fe(η3-C7H7)(CO)3]- (Hofmann, 1978), whose structure has been reported (Sepp et al., 1978), not only demonstrated that there is a preference for the metal to bind through the η3-allylic region of the ligand rather than through the diene segment, but showed that there is more charge localization on the ring for the former conformation over the latter.
The exact mechanism of isomerization has not been determined for (I), including whether the hydrogen transfer is intra- or intermolecular. In one DFT study on selected early transition metal complexes, the mechanism for hydrogen migration was determined to be intramolecular, and a metal hydride intermediate was predicted to be favored over a direct ligand-to-ligand transfer (Herbert et al., 2004). The same conclusion was reached in kinetic studies on similar molybdenum complexes (Green et al., 1989). If these studies can be extended to the cobalt system, then it could be proposed that the hydrogen migration occurs via a `[CoH(η-C7H7)(η-C7H8)]-' intermediate.
As mentioned above, there is exactly one homoleptic CHT structure in the Cambridge Structural Database to date (CSD, Version 5.36, update No. 1, November 2014; Groom & Allen, 2014), namely Zr(η6-C7H8)2 (Green & Walker, 1989). All others have been structurally characterized after isomerization, including (I). There are 23 structures containing an η5-cycloheptadienyl ligand, but only 12 structures containing an η3-cycloheptatrienyl ligand bonded to a single metal center. Of the latter, just three are anionic; they are of the form [AsPh4][M(CO)3(η3-C7H7)], M = Fe (Sepp et al., 1978) and M = Ru, Os (Astley et al., 1990). (I) is the first example of an anionic transition metal complex containing both cycloheptadienyl and cycloheptatrienyl ligands to be reported.
All operations were performed under an atmosphere of 99.5% argon further purified by passage through columns of activated BASF catalyst and molecular sieves. Standard Schlenk techniques were employed for all reactions with a double manifold vacuum (0.01 Torr) line. Solutions were transferred via stainless steel double-ended needles (cannulas) and glass-covered magnetic stir bars were employed. Cycloheptatriene was distilled from Na/K alloy.
Excess cycloheptatriene was added dropwise to a deep pinkish-red solution of [K(18-crown-6)(THF)2][Co(η4-C14H10)2] (0.500 g, 0.579 mmol; Brennessel et al., 2002; Brennessel & Ellis, 2012) in THF (50 ml, 195 K). The solution was slowly warmed to room temperature, at which point it was deep yellowish brown. After the solvent was removed in vacuo and heptane (70 ml) was added, the slurry was filtered. The product was washed with pentane (20 ml) and dried in vacuo, yielding a blackish-gray solid [0.292 g, 92%, based on cobalt and using the formulation of (I)]. This product was only characterized by single-crystal X-ray diffraction. Red–brown blocks were grown from a pentane-layered THF solution at 273 K.
Crystal data, data collection and structure 1 0 0 / 0 1 0 / 0.064 0 1], a 180° rotation about [001], reduced the R1 residual to its final value of 0.043 (Table 3). The mass ratio of the twin components refined to 0.5040 (7):0.4960 (7).
details are summarized in Table 3. The stalled at R1 = 0.19, at which point the structure was examined for (Parsons et al., 2003). Non-merohedral was discovered and the data were re-integrated accordingly. Application of [The η5-coordinating ligand C8–C14 is modeled as disordered over two positions with site occupancy ratio 0.699 (5):0.301 (5), such that the ethyl linkage is shifted by one carbon atom (see Fig. 4). Analogous bond lengths and angles between the two positions of the disordered ring were heavily restrained to be similar. Anisotropic displacement parameters for pairs of proximal atoms from the two components of the disorder were constrained to be equivalent (Sheldrick, 2015).
H-atom positions of ring-ligand carbon atoms, except those in the minor component of the disorder, were located in a difference map and refined freely. All other H atoms were placed geometrically and treated as riding atoms: methine and sp2, C—H = 1.00 Å, and methylene, C—H = 0.99 Å, with Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 2003); cell
SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2015); software used to prepare material for publication: SHELXTL (Sheldrick, 2015).Fig. 1. Structure of the first independent molecule of (I), with displacement ellipsoids shown at the 50% probability level. H atoms have been omitted. Thin lines indicate the primarily electrostatic interactions between the K atom and the crown ether and η3 ring. | |
Fig. 2. Structure of the second independent molecule of (I), with displacement ellipsoids shown at the 50% probability level. H atoms and the minor component of the disordered ring have been omitted. Thin lines indicate the primarily electrostatic interactions between the K atom and the crown ether and η3 ring. | |
Fig. 3. Numbering scheme used for the η3-cycloheptatrienyl ligands in Table 3. | |
Fig. 4. View of the ring ligand disorder. Displacement ellipsoids are shown at the 50% probability level and H atoms have been omitted. The numbering scheme of the minor component of the disorder was chosen to show the mirror-like symmetry that allows both orientations to fit within essentially the same volume. |
[K(C12H24O6)][Co(C7H7)(C7H9)] | F(000) = 2320 |
Mr = 546.61 | Dx = 1.377 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.3925 (19) Å | Cell parameters from 3984 reflections |
b = 17.225 (2) Å | θ = 2.4–27.4° |
c = 18.678 (2) Å | µ = 0.85 mm−1 |
β = 91.6077 (19)° | T = 173 K |
V = 5271.8 (11) Å3 | Block, red-brown |
Z = 8 | 0.32 × 0.24 × 0.16 mm |
Siemens SMART CCD platform diffractometer | 9117 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.055 |
ω scans | θmax = 27.5°, θmin = 1.2° |
Absorption correction: multi-scan (TWINABS; Sheldrick, 2012) | h = −21→21 |
Tmin = 0.612, Tmax = 0.746 | k = 0→22 |
85092 measured reflections | l = 0→24 |
12058 independent reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: mixed |
wR(F2) = 0.084 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0271P)2 + 2.3296P] where P = (Fo2 + 2Fc2)/3 |
12058 reflections | (Δ/σ)max = 0.001 |
728 parameters | Δρmax = 0.46 e Å−3 |
45 restraints | Δρmin = −0.47 e Å−3 |
[K(C12H24O6)][Co(C7H7)(C7H9)] | V = 5271.8 (11) Å3 |
Mr = 546.61 | Z = 8 |
Monoclinic, P21/c | Mo Kα radiation |
a = 16.3925 (19) Å | µ = 0.85 mm−1 |
b = 17.225 (2) Å | T = 173 K |
c = 18.678 (2) Å | 0.32 × 0.24 × 0.16 mm |
β = 91.6077 (19)° |
Siemens SMART CCD platform diffractometer | 12058 independent reflections |
Absorption correction: multi-scan (TWINABS; Sheldrick, 2012) | 9117 reflections with I > 2σ(I) |
Tmin = 0.612, Tmax = 0.746 | Rint = 0.055 |
85092 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 45 restraints |
wR(F2) = 0.084 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 0.46 e Å−3 |
12058 reflections | Δρmin = −0.47 e Å−3 |
728 parameters |
Refinement. The structure was integrated and refined as a non-merohedral twin (Parsons et al., 2003). Application of twin law [-1 0 0 / 0 - 1 0 / 0.064 0 1], a 180° rotation about reciprocal lattice [001], reduced the R residual from 19.0% to its final value of 4.3%. The mass ratio of the twin components refined to 0.5039 (7):0.4961 (7). The η5-coordinating ligand C8—C14 is modeled as disordered over two positions, 0.697 (5):0.303 (5), such that the ethyl linkage is shifted by one carbon atom. Analogous bond lengths and angles between the two positions of the disordered ring were heavily restrained to be similar. Anisotropic displacement parameters for pairs of proximal atoms from the two components of the disorder were constrained to be equivalent. H atom positions of ring-ligand carbon atoms, except those in the minor component of the disorder, were refined freely. All other H atoms were placed geometrically and treated as riding atoms: methine and sp2, C—H = 1.00 Å, and methylene, C—H = 0.99 Å, with Uiso(H) = 1.2Ueq(C). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.08386 (3) | 0.87509 (2) | 0.59699 (2) | 0.02870 (10) | |
C1 | 0.1495 (3) | 0.8446 (2) | 0.5119 (2) | 0.0510 (11) | |
H1 | 0.172 (3) | 0.881 (2) | 0.489 (2) | 0.078 (14)* | |
C2 | 0.0624 (3) | 0.8404 (2) | 0.50036 (18) | 0.0433 (9) | |
H2 | 0.035 (2) | 0.867 (2) | 0.469 (2) | 0.059 (12)* | |
C3 | 0.0169 (2) | 0.7864 (2) | 0.54050 (18) | 0.0394 (8) | |
H3 | −0.039 (2) | 0.787 (2) | 0.5341 (19) | 0.051 (11)* | |
C4 | 0.0432 (2) | 0.7125 (2) | 0.56839 (19) | 0.0443 (9) | |
H4 | −0.005 (2) | 0.688 (2) | 0.592 (2) | 0.079 (13)* | |
C5 | 0.1172 (3) | 0.6777 (2) | 0.56901 (19) | 0.0500 (10) | |
H5 | 0.124 (2) | 0.626 (2) | 0.590 (2) | 0.076 (13)* | |
C6 | 0.1922 (3) | 0.7098 (3) | 0.5507 (2) | 0.0585 (12) | |
H6 | 0.242 (3) | 0.675 (2) | 0.561 (2) | 0.088 (15)* | |
C7 | 0.2057 (2) | 0.7831 (3) | 0.5275 (2) | 0.0596 (12) | |
H7 | 0.265 (3) | 0.800 (2) | 0.522 (2) | 0.079 (13)* | |
C8 | 0.15714 (18) | 0.88005 (18) | 0.69126 (16) | 0.0293 (7) | |
H8 | 0.1933 (18) | 0.8412 (17) | 0.7021 (15) | 0.031 (8)* | |
C9 | 0.0752 (2) | 0.86626 (19) | 0.70514 (16) | 0.0326 (7) | |
H9 | 0.0561 (17) | 0.8191 (17) | 0.7215 (15) | 0.030 (8)* | |
C10 | 0.0139 (2) | 0.9175 (2) | 0.67898 (17) | 0.0364 (8) | |
H10 | −0.0423 (19) | 0.9061 (16) | 0.6853 (15) | 0.029 (8)* | |
C11 | 0.0287 (2) | 0.97567 (19) | 0.62694 (19) | 0.0391 (8) | |
H11 | −0.019 (2) | 0.9961 (18) | 0.6036 (17) | 0.047 (9)* | |
C12 | 0.1052 (2) | 0.99269 (17) | 0.59661 (18) | 0.0357 (7) | |
H12 | 0.101 (2) | 1.0225 (19) | 0.5523 (18) | 0.051 (10)* | |
C13 | 0.1851 (2) | 1.00884 (19) | 0.63506 (18) | 0.0360 (8) | |
H13A | 0.1932 (18) | 1.0645 (18) | 0.6471 (15) | 0.034 (8)* | |
H13B | 0.229 (2) | 0.9996 (19) | 0.604 (2) | 0.056 (11)* | |
C14 | 0.1941 (2) | 0.95999 (19) | 0.70173 (18) | 0.0330 (7) | |
H14A | 0.1658 (17) | 0.9837 (16) | 0.7411 (15) | 0.029 (8)* | |
H14B | 0.2494 (18) | 0.9562 (16) | 0.7172 (14) | 0.024 (7)* | |
Co2 | 0.39803 (2) | 0.38636 (2) | 0.59565 (2) | 0.03271 (10) | |
C15 | 0.3302 (2) | 0.3197 (2) | 0.52922 (19) | 0.0440 (9) | |
H15 | 0.276 (2) | 0.333 (2) | 0.518 (2) | 0.067 (12)* | |
C16 | 0.3926 (3) | 0.3615 (2) | 0.49555 (17) | 0.0451 (9) | |
H16 | 0.381 (2) | 0.402 (2) | 0.4625 (18) | 0.054 (10)* | |
C17 | 0.4764 (2) | 0.3482 (2) | 0.50970 (19) | 0.0438 (9) | |
H17 | 0.519 (2) | 0.3912 (19) | 0.4897 (18) | 0.056 (10)* | |
C18 | 0.5157 (2) | 0.2777 (2) | 0.52637 (19) | 0.0439 (9) | |
H18 | 0.579 (2) | 0.280 (2) | 0.525 (2) | 0.069 (12)* | |
C19 | 0.4846 (2) | 0.2077 (2) | 0.54489 (18) | 0.0455 (9) | |
H19 | 0.527 (2) | 0.162 (2) | 0.5528 (17) | 0.057 (11)* | |
C20 | 0.4028 (3) | 0.1907 (2) | 0.55977 (19) | 0.0480 (9) | |
H20 | 0.392 (2) | 0.1417 (19) | 0.5780 (17) | 0.044 (9)* | |
C21 | 0.3370 (3) | 0.2401 (3) | 0.5569 (2) | 0.0549 (11) | |
H21 | 0.291 (2) | 0.224 (2) | 0.572 (2) | 0.063 (13)* | |
C22 | 0.3724 (5) | 0.5020 (8) | 0.6053 (8) | 0.0308 (11) | 0.699 (5) |
H22 | 0.3723 | 0.5303 | 0.5585 | 0.037* | 0.699 (5) |
C23 | 0.4523 (5) | 0.4885 (7) | 0.6346 (8) | 0.031 (2) | 0.699 (5) |
H23 | 0.4942 | 0.5245 | 0.6242 | 0.038* | 0.699 (5) |
C24 | 0.4724 (5) | 0.4234 (9) | 0.6786 (8) | 0.0380 (13) | 0.699 (5) |
H24 | 0.5286 | 0.4150 | 0.6900 | 0.046* | 0.699 (5) |
C25 | 0.4159 (4) | 0.3698 (5) | 0.7071 (4) | 0.0332 (15) | 0.699 (5) |
H25 | 0.4345 | 0.3271 | 0.7352 | 0.040* | 0.699 (5) |
C26 | 0.3307 (3) | 0.3810 (3) | 0.6927 (3) | 0.0344 (11) | 0.699 (5) |
H26 | 0.2949 | 0.3346 | 0.6986 | 0.041* | 0.699 (5) |
C27 | 0.2936 (6) | 0.4589 (6) | 0.7100 (3) | 0.0303 (12) | 0.699 (5) |
H27A | 0.3241 | 0.4825 | 0.7510 | 0.036* | 0.699 (5) |
H27B | 0.2363 | 0.4515 | 0.7240 | 0.036* | 0.699 (5) |
C28 | 0.2960 (3) | 0.5137 (3) | 0.6455 (3) | 0.0335 (10) | 0.699 (5) |
H28A | 0.2481 | 0.5038 | 0.6133 | 0.040* | 0.699 (5) |
H28B | 0.2931 | 0.5681 | 0.6621 | 0.040* | 0.699 (5) |
C22' | 0.4013 (10) | 0.3665 (13) | 0.6930 (10) | 0.0332 (15) | 0.301 (5) |
H22' | 0.4212 | 0.3132 | 0.7056 | 0.040* | 0.301 (5) |
C23' | 0.4652 (10) | 0.422 (2) | 0.6851 (19) | 0.0380 (13) | 0.301 (5) |
H23' | 0.5118 | 0.4215 | 0.7165 | 0.046* | 0.301 (5) |
C24' | 0.4570 (11) | 0.4773 (19) | 0.629 (2) | 0.031 (2) | 0.301 (5) |
H24' | 0.5062 | 0.4977 | 0.6105 | 0.038* | 0.301 (5) |
C25' | 0.3825 (11) | 0.506 (2) | 0.5966 (19) | 0.0308 (11) | 0.301 (5) |
H25' | 0.3834 | 0.5452 | 0.5613 | 0.037* | 0.301 (5) |
C26' | 0.3069 (6) | 0.4736 (6) | 0.6182 (5) | 0.0335 (10) | 0.301 (5) |
H26C | 0.2592 | 0.4781 | 0.5839 | 0.040* | 0.301 (5) |
C27' | 0.2893 (16) | 0.4648 (14) | 0.6962 (8) | 0.0303 (12) | 0.301 (5) |
H27C | 0.2297 | 0.4678 | 0.7028 | 0.036* | 0.301 (5) |
H27D | 0.3154 | 0.5078 | 0.7236 | 0.036* | 0.301 (5) |
C28' | 0.3216 (8) | 0.3867 (7) | 0.7254 (6) | 0.0344 (11) | 0.301 (5) |
H28C | 0.3287 | 0.3899 | 0.7781 | 0.041* | 0.301 (5) |
H28D | 0.2812 | 0.3454 | 0.7142 | 0.041* | 0.301 (5) |
K1 | 0.11102 (4) | 0.69805 (3) | 0.39075 (3) | 0.02821 (14) | |
O1 | 0.21703 (13) | 0.79524 (13) | 0.31156 (12) | 0.0361 (5) | |
C29 | 0.1870 (2) | 0.87284 (18) | 0.3082 (2) | 0.0439 (8) | |
H29A | 0.2247 | 0.9058 | 0.2809 | 0.053* | |
H29B | 0.1834 | 0.8944 | 0.3571 | 0.053* | |
C30 | 0.1046 (2) | 0.87240 (18) | 0.27208 (18) | 0.0433 (8) | |
H30A | 0.0854 | 0.9263 | 0.2641 | 0.052* | |
H30B | 0.1071 | 0.8461 | 0.2251 | 0.052* | |
O2 | 0.05022 (13) | 0.83223 (12) | 0.31708 (10) | 0.0332 (5) | |
C31 | −0.0317 (2) | 0.83326 (19) | 0.28937 (18) | 0.0409 (8) | |
H31A | −0.0343 | 0.8096 | 0.2410 | 0.049* | |
H31B | −0.0515 | 0.8874 | 0.2854 | 0.049* | |
C32 | −0.08384 (19) | 0.78852 (18) | 0.33875 (18) | 0.0405 (8) | |
H32A | −0.0788 | 0.8103 | 0.3877 | 0.049* | |
H32B | −0.1417 | 0.7919 | 0.3225 | 0.049* | |
O3 | −0.05789 (12) | 0.71010 (13) | 0.33890 (12) | 0.0378 (5) | |
C33 | −0.10669 (19) | 0.6611 (2) | 0.38195 (18) | 0.0422 (8) | |
H33A | −0.1649 | 0.6653 | 0.3667 | 0.051* | |
H33B | −0.1012 | 0.6766 | 0.4329 | 0.051* | |
C34 | −0.0775 (2) | 0.5799 (2) | 0.37251 (19) | 0.0447 (9) | |
H34A | −0.1157 | 0.5431 | 0.3948 | 0.054* | |
H34B | −0.0749 | 0.5674 | 0.3209 | 0.054* | |
O4 | 0.00127 (13) | 0.57276 (11) | 0.40546 (13) | 0.0388 (5) | |
C35 | 0.0343 (2) | 0.49680 (19) | 0.3986 (2) | 0.0513 (10) | |
H35A | 0.0403 | 0.4840 | 0.3473 | 0.062* | |
H35B | −0.0028 | 0.4583 | 0.4197 | 0.062* | |
C36 | 0.1150 (2) | 0.49405 (19) | 0.4361 (2) | 0.0499 (10) | |
H36A | 0.1102 | 0.5144 | 0.4854 | 0.060* | |
H36B | 0.1342 | 0.4396 | 0.4393 | 0.060* | |
O5 | 0.17146 (13) | 0.53887 (12) | 0.39880 (12) | 0.0364 (5) | |
C37 | 0.2495 (2) | 0.5416 (2) | 0.43407 (18) | 0.0426 (9) | |
H37A | 0.2700 | 0.4883 | 0.4426 | 0.051* | |
H37B | 0.2453 | 0.5679 | 0.4809 | 0.051* | |
C38 | 0.3067 (2) | 0.5849 (2) | 0.38815 (18) | 0.0414 (8) | |
H38A | 0.3626 | 0.5832 | 0.4095 | 0.050* | |
H38B | 0.3077 | 0.5612 | 0.3399 | 0.050* | |
O6 | 0.27920 (13) | 0.66290 (12) | 0.38309 (12) | 0.0362 (5) | |
C39 | 0.32695 (19) | 0.7087 (2) | 0.33672 (18) | 0.0407 (8) | |
H39A | 0.3208 | 0.6896 | 0.2869 | 0.049* | |
H39B | 0.3853 | 0.7056 | 0.3515 | 0.049* | |
C40 | 0.29782 (19) | 0.7908 (2) | 0.34127 (18) | 0.0407 (8) | |
H40A | 0.2984 | 0.8079 | 0.3919 | 0.049* | |
H40B | 0.3344 | 0.8254 | 0.3145 | 0.049* | |
K2 | 0.39810 (4) | 0.20452 (3) | 0.38877 (3) | 0.02898 (14) | |
O7 | 0.45283 (14) | 0.33192 (12) | 0.30801 (11) | 0.0368 (5) | |
C41 | 0.3973 (2) | 0.3681 (2) | 0.25962 (19) | 0.0485 (9) | |
H41A | 0.3914 | 0.3367 | 0.2153 | 0.058* | |
H41B | 0.4177 | 0.4201 | 0.2466 | 0.058* | |
C42 | 0.3170 (2) | 0.37518 (19) | 0.2941 (2) | 0.0476 (9) | |
H42A | 0.3236 | 0.4036 | 0.3400 | 0.057* | |
H42B | 0.2786 | 0.4047 | 0.2625 | 0.057* | |
O8 | 0.28521 (13) | 0.29987 (12) | 0.30686 (12) | 0.0380 (5) | |
C43 | 0.20880 (19) | 0.3019 (2) | 0.34089 (19) | 0.0425 (9) | |
H43A | 0.1704 | 0.3360 | 0.3137 | 0.051* | |
H43B | 0.2159 | 0.3229 | 0.3900 | 0.051* | |
C44 | 0.17541 (19) | 0.2215 (2) | 0.34377 (19) | 0.0450 (9) | |
H44A | 0.1190 | 0.2226 | 0.3613 | 0.054* | |
H44B | 0.1743 | 0.1981 | 0.2954 | 0.054* | |
O9 | 0.22655 (13) | 0.17710 (13) | 0.39114 (12) | 0.0390 (5) | |
C45 | 0.1980 (2) | 0.0998 (2) | 0.4002 (2) | 0.0471 (9) | |
H45A | 0.1895 | 0.0747 | 0.3529 | 0.056* | |
H45B | 0.1452 | 0.1003 | 0.4248 | 0.056* | |
C46 | 0.2594 (2) | 0.0557 (2) | 0.44361 (19) | 0.0460 (9) | |
H46A | 0.2707 | 0.0826 | 0.4897 | 0.055* | |
H46B | 0.2385 | 0.0031 | 0.4540 | 0.055* | |
O10 | 0.33194 (13) | 0.05044 (12) | 0.40421 (12) | 0.0372 (5) | |
C47 | 0.3896 (2) | −0.00261 (18) | 0.4340 (2) | 0.0499 (10) | |
H47A | 0.3662 | −0.0556 | 0.4345 | 0.060* | |
H47B | 0.4042 | 0.0124 | 0.4839 | 0.060* | |
C48 | 0.4635 (2) | −0.00123 (19) | 0.3895 (2) | 0.0508 (10) | |
H48A | 0.5010 | −0.0437 | 0.4042 | 0.061* | |
H48B | 0.4477 | −0.0086 | 0.3384 | 0.061* | |
O11 | 0.50257 (13) | 0.07131 (11) | 0.39930 (12) | 0.0369 (5) | |
C49 | 0.5787 (2) | 0.0755 (2) | 0.36519 (19) | 0.0452 (9) | |
H49A | 0.5716 | 0.0619 | 0.3139 | 0.054* | |
H49B | 0.6176 | 0.0381 | 0.3876 | 0.054* | |
C50 | 0.61118 (19) | 0.1558 (2) | 0.37255 (19) | 0.0449 (9) | |
H50A | 0.6114 | 0.1720 | 0.4234 | 0.054* | |
H50B | 0.6679 | 0.1580 | 0.3557 | 0.054* | |
O12 | 0.56028 (12) | 0.20619 (13) | 0.33055 (12) | 0.0370 (5) | |
C51 | 0.5866 (2) | 0.2849 (2) | 0.33212 (19) | 0.0451 (9) | |
H51A | 0.6443 | 0.2884 | 0.3181 | 0.054* | |
H51B | 0.5822 | 0.3063 | 0.3811 | 0.054* | |
C52 | 0.5337 (2) | 0.3295 (2) | 0.28107 (18) | 0.0430 (9) | |
H52A | 0.5551 | 0.3828 | 0.2759 | 0.052* | |
H52B | 0.5330 | 0.3042 | 0.2334 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0393 (2) | 0.02537 (19) | 0.02133 (19) | −0.00096 (19) | −0.00152 (18) | −0.00292 (16) |
C1 | 0.077 (3) | 0.050 (2) | 0.0272 (19) | −0.034 (2) | 0.0239 (19) | −0.0144 (17) |
C2 | 0.074 (3) | 0.0300 (18) | 0.0251 (17) | 0.0044 (19) | −0.0124 (18) | −0.0030 (14) |
C3 | 0.0346 (18) | 0.049 (2) | 0.0348 (18) | 0.0014 (17) | −0.0005 (15) | −0.0142 (15) |
C4 | 0.060 (2) | 0.0315 (18) | 0.042 (2) | −0.0090 (18) | 0.0182 (18) | −0.0024 (15) |
C5 | 0.081 (3) | 0.0335 (19) | 0.0358 (19) | 0.016 (2) | 0.002 (2) | −0.0059 (15) |
C6 | 0.054 (2) | 0.080 (3) | 0.041 (2) | 0.019 (3) | −0.0118 (19) | −0.026 (2) |
C7 | 0.037 (2) | 0.097 (4) | 0.045 (2) | −0.016 (2) | 0.0044 (18) | −0.038 (2) |
C8 | 0.0373 (16) | 0.0262 (17) | 0.0244 (16) | 0.0058 (15) | −0.0027 (13) | 0.0016 (12) |
C9 | 0.0414 (18) | 0.0349 (17) | 0.0219 (15) | −0.0082 (15) | 0.0068 (14) | −0.0005 (13) |
C10 | 0.0299 (17) | 0.0422 (19) | 0.0370 (19) | −0.0042 (15) | −0.0006 (15) | −0.0148 (16) |
C11 | 0.0356 (18) | 0.0309 (18) | 0.050 (2) | 0.0050 (15) | −0.0118 (16) | −0.0138 (15) |
C12 | 0.050 (2) | 0.0246 (14) | 0.0324 (17) | −0.0010 (15) | −0.0049 (16) | −0.0002 (14) |
C13 | 0.0433 (19) | 0.0273 (18) | 0.0374 (19) | −0.0060 (15) | 0.0036 (16) | 0.0005 (14) |
C14 | 0.0305 (17) | 0.0375 (18) | 0.0309 (18) | −0.0008 (15) | −0.0013 (14) | −0.0076 (14) |
Co2 | 0.0306 (2) | 0.0312 (2) | 0.0362 (2) | 0.00488 (19) | −0.00151 (19) | −0.01252 (18) |
C15 | 0.0350 (18) | 0.056 (2) | 0.041 (2) | 0.0139 (17) | −0.0100 (16) | −0.0203 (18) |
C16 | 0.069 (3) | 0.0418 (19) | 0.0245 (16) | 0.020 (2) | 0.0061 (17) | 0.0050 (14) |
C17 | 0.055 (2) | 0.0360 (19) | 0.041 (2) | 0.0036 (18) | 0.0107 (18) | −0.0036 (16) |
C18 | 0.044 (2) | 0.048 (2) | 0.0394 (19) | 0.0062 (18) | −0.0088 (17) | −0.0044 (16) |
C19 | 0.057 (2) | 0.041 (2) | 0.0379 (19) | 0.0158 (19) | −0.0108 (17) | −0.0020 (15) |
C20 | 0.079 (3) | 0.0316 (18) | 0.0331 (18) | 0.004 (2) | 0.0024 (19) | −0.0010 (14) |
C21 | 0.057 (3) | 0.071 (3) | 0.038 (2) | −0.002 (2) | 0.0151 (19) | −0.009 (2) |
C22 | 0.039 (3) | 0.027 (2) | 0.027 (4) | 0.000 (2) | 0.001 (2) | −0.0030 (18) |
C23 | 0.0296 (18) | 0.027 (4) | 0.037 (3) | −0.004 (2) | −0.0002 (18) | −0.014 (3) |
C24 | 0.029 (2) | 0.051 (2) | 0.034 (3) | 0.013 (2) | −0.003 (2) | −0.013 (2) |
C25 | 0.048 (3) | 0.0353 (19) | 0.015 (3) | 0.018 (3) | −0.014 (2) | −0.008 (2) |
C26 | 0.044 (2) | 0.035 (2) | 0.024 (3) | −0.0001 (19) | 0.002 (3) | −0.002 (3) |
C27 | 0.0300 (19) | 0.036 (2) | 0.025 (3) | 0.0070 (16) | 0.002 (3) | −0.004 (3) |
C28 | 0.033 (2) | 0.024 (2) | 0.043 (3) | 0.008 (2) | −0.003 (2) | −0.0027 (18) |
C22' | 0.048 (3) | 0.0353 (19) | 0.015 (3) | 0.018 (3) | −0.014 (2) | −0.008 (2) |
C23' | 0.029 (2) | 0.051 (2) | 0.034 (3) | 0.013 (2) | −0.003 (2) | −0.013 (2) |
C24' | 0.0296 (18) | 0.027 (4) | 0.037 (3) | −0.004 (2) | −0.0002 (18) | −0.014 (3) |
C25' | 0.039 (3) | 0.027 (2) | 0.027 (4) | 0.000 (2) | 0.001 (2) | −0.0030 (18) |
C26' | 0.033 (2) | 0.024 (2) | 0.043 (3) | 0.008 (2) | −0.003 (2) | −0.0027 (18) |
C27' | 0.0300 (19) | 0.036 (2) | 0.025 (3) | 0.0070 (16) | 0.002 (3) | −0.004 (3) |
C28' | 0.044 (2) | 0.035 (2) | 0.024 (3) | −0.0001 (19) | 0.002 (3) | −0.002 (3) |
K1 | 0.0271 (3) | 0.0252 (3) | 0.0322 (4) | −0.0006 (3) | −0.0016 (3) | 0.0035 (3) |
O1 | 0.0371 (12) | 0.0336 (12) | 0.0376 (13) | −0.0071 (10) | 0.0006 (10) | 0.0006 (10) |
C29 | 0.060 (2) | 0.0255 (17) | 0.047 (2) | −0.0121 (17) | 0.0115 (17) | 0.0086 (15) |
C30 | 0.063 (2) | 0.0337 (18) | 0.0334 (17) | 0.0069 (18) | 0.0004 (17) | 0.0099 (14) |
O2 | 0.0384 (12) | 0.0314 (12) | 0.0294 (12) | 0.0044 (10) | −0.0043 (9) | 0.0045 (9) |
C31 | 0.048 (2) | 0.0359 (18) | 0.0375 (19) | 0.0170 (16) | −0.0203 (16) | −0.0051 (15) |
C32 | 0.0334 (17) | 0.046 (2) | 0.0422 (19) | 0.0128 (16) | −0.0044 (15) | −0.0109 (16) |
O3 | 0.0303 (11) | 0.0411 (13) | 0.0421 (13) | 0.0051 (10) | 0.0023 (10) | −0.0026 (11) |
C33 | 0.0238 (16) | 0.063 (2) | 0.0398 (19) | −0.0076 (16) | −0.0015 (14) | 0.0025 (16) |
C34 | 0.0392 (19) | 0.054 (2) | 0.0405 (19) | −0.0227 (18) | 0.0011 (16) | 0.0024 (16) |
O4 | 0.0400 (12) | 0.0293 (11) | 0.0470 (13) | −0.0078 (10) | 0.0013 (11) | −0.0035 (11) |
C35 | 0.058 (2) | 0.0286 (17) | 0.069 (3) | −0.0108 (17) | 0.026 (2) | −0.0085 (19) |
C36 | 0.065 (2) | 0.0269 (17) | 0.059 (2) | 0.0092 (18) | 0.024 (2) | 0.0113 (16) |
O5 | 0.0420 (13) | 0.0352 (12) | 0.0321 (12) | 0.0052 (10) | 0.0036 (10) | 0.0062 (10) |
C37 | 0.055 (2) | 0.0396 (19) | 0.0325 (18) | 0.0239 (17) | −0.0056 (16) | 0.0003 (15) |
C38 | 0.0344 (18) | 0.050 (2) | 0.0397 (19) | 0.0196 (16) | −0.0059 (15) | −0.0092 (16) |
O6 | 0.0281 (11) | 0.0430 (13) | 0.0377 (13) | 0.0047 (10) | 0.0047 (10) | −0.0008 (10) |
C39 | 0.0262 (16) | 0.062 (2) | 0.0341 (18) | −0.0014 (16) | 0.0058 (13) | −0.0067 (17) |
C40 | 0.0323 (17) | 0.053 (2) | 0.0370 (19) | −0.0142 (17) | 0.0071 (14) | −0.0057 (17) |
K2 | 0.0277 (3) | 0.0263 (3) | 0.0329 (4) | 0.0028 (3) | 0.0007 (3) | 0.0054 (3) |
O7 | 0.0481 (13) | 0.0332 (12) | 0.0294 (12) | −0.0045 (10) | 0.0067 (10) | 0.0041 (10) |
C41 | 0.068 (2) | 0.0327 (17) | 0.044 (2) | −0.0093 (19) | −0.0025 (19) | 0.0153 (15) |
C42 | 0.067 (2) | 0.0256 (18) | 0.049 (2) | 0.0151 (18) | −0.0116 (19) | 0.0085 (15) |
O8 | 0.0407 (12) | 0.0324 (12) | 0.0408 (14) | 0.0103 (11) | 0.0019 (10) | 0.0003 (10) |
C43 | 0.0360 (17) | 0.048 (2) | 0.043 (2) | 0.0218 (17) | −0.0104 (15) | −0.0078 (17) |
C44 | 0.0229 (16) | 0.071 (3) | 0.041 (2) | 0.0118 (16) | −0.0020 (14) | −0.0047 (18) |
O9 | 0.0272 (11) | 0.0472 (13) | 0.0423 (14) | −0.0015 (10) | −0.0025 (10) | 0.0040 (11) |
C45 | 0.0318 (17) | 0.065 (2) | 0.045 (2) | −0.0154 (17) | 0.0060 (16) | −0.0024 (19) |
C46 | 0.054 (2) | 0.042 (2) | 0.042 (2) | −0.0183 (18) | 0.0070 (17) | 0.0099 (16) |
O10 | 0.0398 (12) | 0.0356 (12) | 0.0360 (12) | −0.0014 (10) | −0.0010 (10) | 0.0122 (11) |
C47 | 0.065 (2) | 0.0254 (17) | 0.058 (2) | −0.0029 (18) | −0.020 (2) | 0.0122 (15) |
C48 | 0.056 (2) | 0.0241 (17) | 0.071 (3) | 0.0156 (17) | −0.016 (2) | −0.0060 (17) |
O11 | 0.0375 (12) | 0.0332 (12) | 0.0399 (12) | 0.0094 (10) | −0.0002 (10) | −0.0050 (11) |
C49 | 0.043 (2) | 0.053 (2) | 0.0396 (19) | 0.0237 (18) | −0.0013 (17) | −0.0009 (16) |
C50 | 0.0219 (16) | 0.074 (3) | 0.0387 (19) | 0.0068 (17) | −0.0033 (14) | −0.0057 (17) |
O12 | 0.0270 (11) | 0.0403 (12) | 0.0434 (13) | −0.0053 (10) | −0.0060 (9) | −0.0035 (10) |
C51 | 0.0370 (18) | 0.054 (2) | 0.044 (2) | −0.0175 (17) | 0.0068 (16) | −0.0136 (17) |
C52 | 0.053 (2) | 0.0366 (19) | 0.040 (2) | −0.0177 (17) | 0.0147 (17) | −0.0064 (16) |
Co1—C2 | 1.924 (3) | C26'—H26C | 1.0000 |
Co1—C1 | 2.014 (4) | C27'—C28' | 1.538 (15) |
Co1—C9 | 2.035 (3) | C27'—H27C | 0.9900 |
Co1—C11 | 2.040 (3) | C27'—H27D | 0.9900 |
Co1—C12 | 2.055 (3) | C28'—H28C | 0.9900 |
Co1—C10 | 2.072 (3) | C28'—H28D | 0.9900 |
Co1—C8 | 2.105 (3) | K1—O4 | 2.828 (2) |
Co1—C3 | 2.142 (3) | K1—O6 | 2.830 (2) |
C1—C7 | 1.430 (6) | K1—O2 | 2.855 (2) |
C1—C2 | 1.439 (6) | K1—O1 | 2.856 (2) |
C1—K1 | 3.436 (4) | K1—O3 | 2.915 (2) |
C1—H1 | 0.85 (4) | K1—O5 | 2.918 (2) |
C2—C3 | 1.420 (5) | O1—C40 | 1.424 (4) |
C2—K1 | 3.307 (3) | O1—C29 | 1.425 (4) |
C2—H2 | 0.85 (4) | C29—C30 | 1.493 (5) |
C3—C4 | 1.437 (5) | C29—H29A | 0.9900 |
C3—H3 | 0.91 (4) | C29—H29B | 0.9900 |
C4—C5 | 1.353 (5) | C30—O2 | 1.422 (4) |
C4—K1 | 3.538 (4) | C30—H30A | 0.9900 |
C4—H4 | 1.01 (4) | C30—H30B | 0.9900 |
C5—C6 | 1.398 (6) | O2—C31 | 1.426 (4) |
C5—K1 | 3.346 (4) | C31—C32 | 1.489 (5) |
C5—H5 | 0.98 (4) | C31—H31A | 0.9900 |
C6—C7 | 1.354 (6) | C31—H31B | 0.9900 |
C6—K1 | 3.242 (4) | C32—O3 | 1.416 (3) |
C6—H6 | 1.04 (4) | C32—H32A | 0.9900 |
C7—K1 | 3.295 (4) | C32—H32B | 0.9900 |
C7—H7 | 1.03 (4) | O3—C33 | 1.427 (4) |
C8—C9 | 1.395 (4) | C33—C34 | 1.491 (5) |
C8—C14 | 1.515 (4) | C33—H33A | 0.9900 |
C8—H8 | 0.91 (3) | C33—H33B | 0.9900 |
C9—C10 | 1.415 (5) | C34—O4 | 1.419 (4) |
C9—H9 | 0.93 (3) | C34—H34A | 0.9900 |
C10—C11 | 1.421 (5) | C34—H34B | 0.9900 |
C10—H10 | 0.95 (3) | O4—C35 | 1.423 (4) |
C11—C12 | 1.421 (5) | C35—C36 | 1.480 (5) |
C11—H11 | 0.95 (3) | C35—H35A | 0.9900 |
C12—C13 | 1.502 (5) | C35—H35B | 0.9900 |
C12—H12 | 0.97 (3) | C36—O5 | 1.406 (4) |
C13—C14 | 1.507 (5) | C36—H36A | 0.9900 |
C13—H13A | 0.99 (3) | C36—H36B | 0.9900 |
C13—H13B | 0.95 (4) | O5—C37 | 1.423 (4) |
C14—H14A | 0.97 (3) | C37—C38 | 1.489 (5) |
C14—H14B | 0.95 (3) | C37—H37A | 0.9900 |
Co2—C22' | 1.850 (18) | C37—H37B | 0.9900 |
Co2—C16 | 1.918 (3) | C38—O6 | 1.419 (4) |
Co2—C24' | 1.93 (3) | C38—H38A | 0.9900 |
Co2—C15 | 2.005 (4) | C38—H38B | 0.9900 |
Co2—C22 | 2.045 (15) | O6—C39 | 1.423 (4) |
Co2—C24 | 2.046 (13) | C39—C40 | 1.496 (4) |
Co2—C23' | 2.07 (3) | C39—H39A | 0.9900 |
Co2—C25' | 2.07 (3) | C39—H39B | 0.9900 |
Co2—C23 | 2.092 (13) | C40—H40A | 0.9900 |
Co2—C25 | 2.113 (7) | C40—H40B | 0.9900 |
Co2—C26 | 2.150 (5) | K2—O7 | 2.823 (2) |
Co2—C26' | 2.167 (10) | K2—O9 | 2.853 (2) |
C15—C16 | 1.413 (5) | K2—O11 | 2.867 (2) |
C15—C21 | 1.468 (6) | K2—O8 | 2.882 (2) |
C15—K2 | 3.496 (3) | K2—O10 | 2.885 (2) |
C15—H15 | 0.94 (4) | K2—O12 | 2.901 (2) |
C16—C17 | 1.410 (5) | O7—C41 | 1.410 (4) |
C16—K2 | 3.362 (4) | O7—C52 | 1.432 (4) |
C16—H16 | 0.95 (3) | C41—C42 | 1.487 (5) |
C17—C18 | 1.404 (5) | C41—H41A | 0.9900 |
C17—H17 | 1.09 (4) | C41—H41B | 0.9900 |
C18—C19 | 1.358 (5) | C42—O8 | 1.420 (4) |
C18—K2 | 3.411 (4) | C42—H42A | 0.9900 |
C18—H18 | 1.03 (4) | C42—H42B | 0.9900 |
C19—C20 | 1.408 (6) | O8—C43 | 1.421 (4) |
C19—K2 | 3.207 (3) | C43—C44 | 1.490 (5) |
C19—H19 | 1.05 (4) | C43—H43A | 0.9900 |
C20—C21 | 1.375 (6) | C43—H43B | 0.9900 |
C20—K2 | 3.201 (4) | C44—O9 | 1.425 (4) |
C20—H20 | 0.93 (3) | C44—H44A | 0.9900 |
C21—K2 | 3.379 (4) | C44—H44B | 0.9900 |
C21—H21 | 0.85 (4) | O9—C45 | 1.424 (4) |
C22—C23 | 1.425 (7) | C45—C46 | 1.484 (5) |
C22—C28 | 1.491 (9) | C45—H45A | 0.9900 |
C22—H22 | 1.0000 | C45—H45B | 0.9900 |
C23—C24 | 1.424 (6) | C46—O10 | 1.419 (4) |
C23—H23 | 0.9500 | C46—H46A | 0.9900 |
C24—C25 | 1.421 (6) | C46—H46B | 0.9900 |
C24—H24 | 0.9500 | O10—C47 | 1.418 (4) |
C25—C26 | 1.428 (7) | C47—C48 | 1.488 (5) |
C25—H25 | 0.9500 | C47—H47A | 0.9900 |
C26—C27 | 1.511 (8) | C47—H47B | 0.9900 |
C26—H26 | 1.0000 | C48—O11 | 1.414 (4) |
C27—C28 | 1.532 (10) | C48—H48A | 0.9900 |
C27—H27A | 0.9900 | C48—H48B | 0.9900 |
C27—H27B | 0.9900 | O11—C49 | 1.419 (4) |
C28—H28A | 0.9900 | C49—C50 | 1.487 (5) |
C28—H28B | 0.9900 | C49—H49A | 0.9900 |
C22'—C23' | 1.424 (10) | C49—H49B | 0.9900 |
C22'—C28' | 1.497 (11) | C50—O12 | 1.424 (4) |
C22'—H22' | 1.0000 | C50—H50A | 0.9900 |
C23'—C24' | 1.428 (9) | C50—H50B | 0.9900 |
C23'—H23' | 0.9500 | O12—C51 | 1.422 (4) |
C24'—C25' | 1.430 (9) | C51—C52 | 1.485 (5) |
C24'—H24' | 0.9500 | C51—H51A | 0.9900 |
C25'—C26' | 1.424 (10) | C51—H51B | 0.9900 |
C25'—H25' | 0.9500 | C52—H52A | 0.9900 |
C26'—C27' | 1.502 (10) | C52—H52B | 0.9900 |
C2—Co1—C1 | 42.78 (16) | O1—K1—O3 | 111.86 (7) |
C2—Co1—C9 | 153.16 (15) | O4—K1—O5 | 59.59 (6) |
C1—Co1—C9 | 144.86 (17) | O6—K1—O5 | 58.11 (6) |
C2—Co1—C11 | 116.74 (15) | O2—K1—O5 | 154.03 (7) |
C1—Co1—C11 | 133.54 (17) | O1—K1—O5 | 111.53 (6) |
C9—Co1—C11 | 75.37 (14) | O3—K1—O5 | 113.71 (6) |
C2—Co1—C12 | 109.21 (14) | O4—K1—C6 | 101.77 (11) |
C1—Co1—C12 | 99.20 (15) | O6—K1—C6 | 71.64 (9) |
C9—Co1—C12 | 95.37 (14) | O2—K1—C6 | 121.46 (10) |
C11—Co1—C12 | 40.60 (13) | O1—K1—C6 | 101.57 (11) |
C2—Co1—C10 | 135.42 (16) | O3—K1—C6 | 131.52 (9) |
C1—Co1—C10 | 173.91 (17) | O5—K1—C6 | 83.19 (10) |
C9—Co1—C10 | 40.30 (13) | O4—K1—C7 | 123.43 (10) |
C11—Co1—C10 | 40.43 (14) | O6—K1—C7 | 72.30 (9) |
C12—Co1—C10 | 75.68 (14) | O2—K1—C7 | 99.46 (11) |
C2—Co1—C8 | 151.90 (15) | O1—K1—C7 | 81.99 (10) |
C1—Co1—C8 | 111.47 (16) | O3—K1—C7 | 130.41 (9) |
C9—Co1—C8 | 39.34 (12) | O5—K1—C7 | 103.05 (11) |
C11—Co1—C8 | 89.04 (13) | C6—K1—C7 | 23.89 (11) |
C12—Co1—C8 | 82.53 (13) | O4—K1—C2 | 109.94 (9) |
C10—Co1—C8 | 71.48 (13) | O6—K1—C2 | 116.23 (9) |
C2—Co1—C3 | 40.45 (15) | O2—K1—C2 | 67.10 (7) |
C1—Co1—C3 | 72.70 (14) | O1—K1—C2 | 92.66 (8) |
C9—Co1—C3 | 112.76 (14) | O3—K1—C2 | 84.82 (8) |
C11—Co1—C3 | 121.05 (13) | O5—K1—C2 | 138.81 (8) |
C12—Co1—C3 | 141.81 (14) | C6—K1—C2 | 58.85 (10) |
C10—Co1—C3 | 109.20 (13) | C7—K1—C2 | 46.11 (11) |
C8—Co1—C3 | 135.52 (13) | O4—K1—C5 | 79.94 (9) |
C7—C1—C2 | 128.7 (4) | O6—K1—C5 | 91.46 (9) |
C7—C1—Co1 | 112.8 (3) | O2—K1—C5 | 124.37 (8) |
C2—C1—Co1 | 65.3 (2) | O1—K1—C5 | 125.07 (9) |
C7—C1—K1 | 72.2 (2) | O3—K1—C5 | 109.88 (9) |
C2—C1—K1 | 72.7 (2) | O5—K1—C5 | 81.36 (8) |
Co1—C1—K1 | 128.27 (15) | C6—K1—C5 | 24.44 (10) |
C7—C1—H1 | 111 (3) | C7—K1—C5 | 43.50 (11) |
C2—C1—H1 | 114 (3) | C2—K1—C5 | 57.50 (9) |
Co1—C1—H1 | 117 (3) | O4—K1—C1 | 127.02 (8) |
K1—C1—H1 | 107 (3) | O6—K1—C1 | 91.69 (9) |
C3—C2—C1 | 119.1 (4) | O2—K1—C1 | 77.15 (9) |
C3—C2—Co1 | 78.0 (2) | O1—K1—C1 | 78.89 (8) |
C1—C2—Co1 | 71.9 (2) | O3—K1—C1 | 108.74 (9) |
C3—C2—K1 | 88.8 (2) | O5—K1—C1 | 126.92 (10) |
C1—C2—K1 | 82.8 (2) | C6—K1—C1 | 44.31 (12) |
Co1—C2—K1 | 140.36 (17) | C7—K1—C1 | 24.41 (11) |
C3—C2—H2 | 116 (3) | C2—K1—C1 | 24.54 (10) |
C1—C2—H2 | 125 (3) | C5—K1—C1 | 54.68 (9) |
Co1—C2—H2 | 123 (3) | O4—K1—C4 | 75.23 (8) |
K1—C2—H2 | 96 (2) | O6—K1—C4 | 113.25 (8) |
C2—C3—C4 | 128.0 (3) | O2—K1—C4 | 106.28 (8) |
C2—C3—Co1 | 61.50 (19) | O1—K1—C4 | 131.02 (7) |
C4—C3—Co1 | 108.0 (2) | O3—K1—C4 | 89.20 (8) |
C2—C3—H3 | 117 (2) | O5—K1—C4 | 97.64 (7) |
C4—C3—H3 | 111 (2) | C6—K1—C4 | 42.52 (10) |
Co1—C3—H3 | 123 (2) | C7—K1—C4 | 52.78 (10) |
C5—C4—C3 | 130.9 (4) | C2—K1—C4 | 43.91 (8) |
C5—C4—K1 | 70.8 (2) | C5—K1—C4 | 22.45 (9) |
C3—C4—K1 | 79.7 (2) | C1—K1—C4 | 52.22 (8) |
C5—C4—H4 | 121 (2) | C40—O1—C29 | 112.5 (3) |
C3—C4—H4 | 108 (2) | C40—O1—K1 | 109.87 (18) |
K1—C4—H4 | 131 (2) | C29—O1—K1 | 111.03 (17) |
C4—C5—C6 | 128.1 (4) | O1—C29—C30 | 108.8 (3) |
C4—C5—K1 | 86.7 (2) | O1—C29—H29A | 109.9 |
C6—C5—K1 | 73.6 (2) | C30—C29—H29A | 109.9 |
C4—C5—H5 | 119 (2) | O1—C29—H29B | 109.9 |
C6—C5—H5 | 112 (2) | C30—C29—H29B | 109.9 |
K1—C5—H5 | 120 (2) | H29A—C29—H29B | 108.3 |
C7—C6—C5 | 126.8 (4) | O2—C30—C29 | 108.1 (2) |
C7—C6—K1 | 80.2 (2) | O2—C30—H30A | 110.1 |
C5—C6—K1 | 82.0 (2) | C29—C30—H30A | 110.1 |
C7—C6—H6 | 118 (2) | O2—C30—H30B | 110.1 |
C5—C6—H6 | 115 (2) | C29—C30—H30B | 110.1 |
K1—C6—H6 | 116 (2) | H30A—C30—H30B | 108.4 |
C6—C7—C1 | 130.2 (4) | C30—O2—C31 | 112.3 (2) |
C6—C7—K1 | 75.9 (2) | C30—O2—K1 | 117.54 (18) |
C1—C7—K1 | 83.3 (2) | C31—O2—K1 | 119.83 (19) |
C6—C7—H7 | 117 (2) | O2—C31—C32 | 108.6 (3) |
C1—C7—H7 | 112 (2) | O2—C31—H31A | 110.0 |
K1—C7—H7 | 119 (2) | C32—C31—H31A | 110.0 |
C9—C8—C14 | 121.0 (3) | O2—C31—H31B | 110.0 |
C9—C8—Co1 | 67.60 (18) | C32—C31—H31B | 110.0 |
C14—C8—Co1 | 111.2 (2) | H31A—C31—H31B | 108.3 |
C9—C8—H8 | 117.1 (18) | O3—C32—C31 | 108.5 (3) |
C14—C8—H8 | 112.5 (19) | O3—C32—H32A | 110.0 |
Co1—C8—H8 | 120.5 (18) | C31—C32—H32A | 110.0 |
C8—C9—C10 | 120.6 (3) | O3—C32—H32B | 110.0 |
C8—C9—Co1 | 73.07 (18) | C31—C32—H32B | 110.0 |
C10—C9—Co1 | 71.29 (18) | H32A—C32—H32B | 108.4 |
C8—C9—H9 | 123.2 (18) | C32—O3—C33 | 113.1 (2) |
C10—C9—H9 | 114.6 (18) | C32—O3—K1 | 110.55 (17) |
Co1—C9—H9 | 115.3 (17) | C33—O3—K1 | 108.24 (17) |
C9—C10—C11 | 122.9 (3) | O3—C33—C34 | 107.5 (3) |
C9—C10—Co1 | 68.42 (18) | O3—C33—H33A | 110.2 |
C11—C10—Co1 | 68.56 (19) | C34—C33—H33A | 110.2 |
C9—C10—H10 | 120.6 (18) | O3—C33—H33B | 110.2 |
C11—C10—H10 | 114.5 (17) | C34—C33—H33B | 110.2 |
Co1—C10—H10 | 125.2 (17) | H33A—C33—H33B | 108.5 |
C12—C11—C10 | 126.0 (3) | O4—C34—C33 | 108.7 (3) |
C12—C11—Co1 | 70.29 (18) | O4—C34—H34A | 109.9 |
C10—C11—Co1 | 71.00 (19) | C33—C34—H34A | 109.9 |
C12—C11—H11 | 118 (2) | O4—C34—H34B | 109.9 |
C10—C11—H11 | 115 (2) | C33—C34—H34B | 109.9 |
Co1—C11—H11 | 124 (2) | H34A—C34—H34B | 108.3 |
C11—C12—C13 | 128.0 (3) | C34—O4—C35 | 112.5 (3) |
C11—C12—Co1 | 69.12 (18) | C34—O4—K1 | 117.73 (18) |
C13—C12—Co1 | 109.1 (2) | C35—O4—K1 | 116.62 (18) |
C11—C12—H12 | 114 (2) | O4—C35—C36 | 108.9 (3) |
C13—C12—H12 | 110 (2) | O4—C35—H35A | 109.9 |
Co1—C12—H12 | 121.0 (19) | C36—C35—H35A | 109.9 |
C12—C13—C14 | 110.9 (3) | O4—C35—H35B | 109.9 |
C12—C13—H13A | 113.4 (18) | C36—C35—H35B | 109.9 |
C14—C13—H13A | 110.0 (17) | H35A—C35—H35B | 108.3 |
C12—C13—H13B | 110 (2) | O5—C36—C35 | 109.8 (3) |
C14—C13—H13B | 111 (2) | O5—C36—H36A | 109.7 |
H13A—C13—H13B | 102 (3) | C35—C36—H36A | 109.7 |
C13—C14—C8 | 111.8 (3) | O5—C36—H36B | 109.7 |
C13—C14—H14A | 110.7 (17) | C35—C36—H36B | 109.7 |
C8—C14—H14A | 106.4 (17) | H36A—C36—H36B | 108.2 |
C13—C14—H14B | 111.2 (17) | C36—O5—C37 | 112.6 (3) |
C8—C14—H14B | 110.7 (17) | C36—O5—K1 | 108.31 (17) |
H14A—C14—H14B | 106 (2) | C37—O5—K1 | 106.98 (18) |
C22'—Co2—C16 | 156.4 (7) | O5—C37—C38 | 108.8 (3) |
C22'—Co2—C24' | 80.5 (9) | O5—C37—H37A | 109.9 |
C16—Co2—C24' | 120.1 (10) | C38—C37—H37A | 109.9 |
C22'—Co2—C15 | 120.2 (8) | O5—C37—H37B | 109.9 |
C16—Co2—C15 | 42.17 (16) | C38—C37—H37B | 109.9 |
C24'—Co2—C15 | 157.8 (8) | H37A—C37—H37B | 108.3 |
C16—Co2—C22 | 107.4 (4) | O6—C38—C37 | 108.0 (3) |
C15—Co2—C22 | 120.0 (4) | O6—C38—H38A | 110.1 |
C16—Co2—C24 | 144.9 (4) | C37—C38—H38A | 110.1 |
C15—Co2—C24 | 162.9 (4) | O6—C38—H38B | 110.1 |
C22—Co2—C24 | 75.5 (5) | C37—C38—H38B | 110.1 |
C22'—Co2—C23' | 42.2 (6) | H38A—C38—H38B | 108.4 |
C16—Co2—C23' | 149.7 (7) | C38—O6—C39 | 112.7 (2) |
C24'—Co2—C23' | 41.7 (6) | C38—O6—K1 | 120.47 (18) |
C15—Co2—C23' | 160.5 (8) | C39—O6—K1 | 117.74 (17) |
C22'—Co2—C25' | 100.1 (10) | O6—C39—C40 | 107.9 (3) |
C16—Co2—C25' | 103.2 (10) | O6—C39—H39A | 110.1 |
C24'—Co2—C25' | 41.7 (6) | C40—C39—H39A | 110.1 |
C15—Co2—C25' | 120.5 (9) | O6—C39—H39B | 110.1 |
C23'—Co2—C25' | 76.3 (12) | C40—C39—H39B | 110.1 |
C16—Co2—C23 | 122.3 (4) | H39A—C39—H39B | 108.4 |
C15—Co2—C23 | 156.9 (3) | O1—C40—C39 | 108.9 (3) |
C22—Co2—C23 | 40.3 (3) | O1—C40—H40A | 109.9 |
C24—Co2—C23 | 40.2 (3) | C39—C40—H40A | 109.9 |
C16—Co2—C25 | 158.6 (2) | O1—C40—H40B | 109.9 |
C15—Co2—C25 | 126.2 (3) | C39—C40—H40B | 109.9 |
C22—Co2—C25 | 93.9 (4) | H40A—C40—H40B | 108.3 |
C24—Co2—C25 | 39.9 (2) | O7—K2—O9 | 117.72 (7) |
C23—Co2—C25 | 74.1 (3) | O7—K2—O11 | 117.43 (7) |
C16—Co2—C26 | 143.25 (19) | O9—K2—O11 | 116.98 (7) |
C15—Co2—C26 | 102.01 (18) | O7—K2—O8 | 58.82 (6) |
C22—Co2—C26 | 81.7 (3) | O9—K2—O8 | 58.94 (6) |
C24—Co2—C26 | 71.6 (3) | O11—K2—O8 | 150.02 (7) |
C23—Co2—C26 | 88.1 (3) | O7—K2—O10 | 153.45 (7) |
C25—Co2—C26 | 39.13 (19) | O9—K2—O10 | 58.17 (6) |
C22'—Co2—C26' | 86.5 (5) | O11—K2—O10 | 58.82 (6) |
C16—Co2—C26' | 109.3 (3) | O8—K2—O10 | 109.87 (7) |
C24'—Co2—C26' | 73.6 (8) | O7—K2—O12 | 58.92 (6) |
C15—Co2—C26' | 98.3 (3) | O9—K2—O12 | 157.17 (7) |
C23'—Co2—C26' | 89.6 (9) | O11—K2—O12 | 58.77 (6) |
C25'—Co2—C26' | 39.2 (4) | O8—K2—O12 | 112.15 (7) |
C16—C15—C21 | 125.7 (3) | O10—K2—O12 | 113.44 (7) |
C16—C15—Co2 | 65.6 (2) | O7—K2—C20 | 126.27 (8) |
C21—C15—Co2 | 106.4 (3) | O9—K2—C20 | 88.19 (10) |
C16—C15—K2 | 72.9 (2) | O11—K2—C20 | 82.78 (8) |
C21—C15—K2 | 73.3 (2) | O8—K2—C20 | 124.69 (9) |
Co2—C15—K2 | 127.35 (15) | O10—K2—C20 | 80.25 (8) |
C16—C15—H15 | 118 (2) | O12—K2—C20 | 112.20 (9) |
C21—C15—H15 | 112 (2) | O7—K2—C19 | 109.48 (9) |
Co2—C15—H15 | 120 (2) | O9—K2—C19 | 113.56 (9) |
K2—C15—H15 | 107 (2) | O11—K2—C19 | 72.73 (8) |
C17—C16—C15 | 123.2 (3) | O8—K2—C19 | 137.22 (8) |
C17—C16—Co2 | 80.5 (2) | O10—K2—C19 | 94.75 (8) |
C15—C16—Co2 | 72.2 (2) | O12—K2—C19 | 87.36 (8) |
C17—C16—K2 | 86.5 (2) | C20—K2—C19 | 25.38 (10) |
C15—C16—K2 | 83.5 (2) | O7—K2—C16 | 72.91 (8) |
Co2—C16—K2 | 139.18 (16) | O9—K2—C16 | 94.65 (9) |
C17—C16—H16 | 115 (2) | O11—K2—C16 | 128.96 (8) |
C15—C16—H16 | 122 (2) | O8—K2—C16 | 80.16 (8) |
Co2—C16—H16 | 118 (2) | O10—K2—C16 | 131.61 (8) |
K2—C16—H16 | 102 (2) | O12—K2—C16 | 104.74 (8) |
C18—C17—C16 | 128.3 (4) | C20—K2—C16 | 57.88 (9) |
C18—C17—Co2 | 111.9 (3) | C19—K2—C16 | 57.69 (9) |
C16—C17—Co2 | 59.95 (19) | O7—K2—C21 | 117.55 (9) |
C18—C17—H17 | 111.9 (18) | O9—K2—C21 | 72.39 (9) |
C16—C17—H17 | 116.8 (18) | O11—K2—C21 | 105.88 (9) |
Co2—C17—H17 | 116.1 (18) | O8—K2—C21 | 100.79 (9) |
C19—C18—C17 | 130.6 (4) | O10—K2—C21 | 87.24 (9) |
C19—C18—K2 | 69.9 (2) | O12—K2—C21 | 130.20 (9) |
C17—C18—K2 | 84.6 (2) | C20—K2—C21 | 23.92 (10) |
C19—C18—H18 | 115 (2) | C19—K2—C21 | 44.53 (10) |
C17—C18—H18 | 114 (2) | C16—K2—C21 | 44.71 (10) |
K2—C18—H18 | 123 (2) | O7—K2—C18 | 86.21 (8) |
C18—C19—C20 | 126.9 (4) | O9—K2—C18 | 125.87 (8) |
C18—C19—K2 | 86.7 (2) | O11—K2—C18 | 85.43 (8) |
C20—C19—K2 | 77.1 (2) | O8—K2—C18 | 122.02 (8) |
C18—C19—H19 | 116.7 (19) | O10—K2—C18 | 118.10 (8) |
C20—C19—H19 | 116.1 (19) | O12—K2—C18 | 76.96 (8) |
K2—C19—H19 | 112.7 (18) | C20—K2—C18 | 43.81 (10) |
C21—C20—C19 | 128.0 (4) | C19—K2—C18 | 23.42 (9) |
C21—C20—K2 | 85.3 (2) | C16—K2—C18 | 43.92 (9) |
C19—C20—K2 | 77.5 (2) | C21—K2—C18 | 53.75 (10) |
C21—C20—H20 | 114 (2) | O7—K2—C15 | 94.16 (8) |
C19—C20—H20 | 117 (2) | O9—K2—C15 | 75.37 (8) |
K2—C20—H20 | 116 (2) | O11—K2—C15 | 127.23 (8) |
C20—C21—C15 | 130.0 (4) | O8—K2—C15 | 82.05 (8) |
C20—C21—K2 | 70.8 (2) | O10—K2—C15 | 108.57 (8) |
C15—C21—K2 | 82.2 (2) | O12—K2—C15 | 126.18 (8) |
C20—C21—H21 | 119 (3) | C20—K2—C15 | 44.99 (9) |
C15—C21—H21 | 111 (3) | C19—K2—C15 | 56.64 (9) |
K2—C21—H21 | 122 (3) | C16—K2—C15 | 23.68 (9) |
C23—C22—C28 | 127.2 (10) | C21—K2—C15 | 24.58 (10) |
C23—C22—Co2 | 71.6 (7) | C18—K2—C15 | 53.83 (9) |
C28—C22—Co2 | 110.7 (6) | C41—O7—C52 | 112.1 (3) |
C23—C22—H22 | 113.2 | C41—O7—K2 | 118.45 (18) |
C28—C22—H22 | 113.2 | C52—O7—K2 | 118.42 (19) |
Co2—C22—H22 | 113.2 | O7—C41—C42 | 108.8 (3) |
C24—C23—C22 | 123.1 (8) | O7—C41—H41A | 109.9 |
C24—C23—Co2 | 68.2 (7) | C42—C41—H41A | 109.9 |
C22—C23—Co2 | 68.1 (7) | O7—C41—H41B | 109.9 |
C24—C23—H23 | 118.4 | C42—C41—H41B | 109.9 |
C22—C23—H23 | 118.4 | H41A—C41—H41B | 108.3 |
Co2—C23—H23 | 141.4 | O8—C42—C41 | 109.3 (3) |
C25—C24—C23 | 125.8 (8) | O8—C42—H42A | 109.8 |
C25—C24—Co2 | 72.5 (5) | C41—C42—H42A | 109.8 |
C23—C24—Co2 | 71.6 (7) | O8—C42—H42B | 109.8 |
C25—C24—H24 | 117.1 | C41—C42—H42B | 109.8 |
C23—C24—H24 | 117.1 | H42A—C42—H42B | 108.3 |
Co2—C24—H24 | 132.5 | C42—O8—C43 | 112.6 (3) |
C24—C25—C26 | 119.1 (6) | C42—O8—K2 | 112.13 (18) |
C24—C25—Co2 | 67.5 (6) | C43—O8—K2 | 109.72 (18) |
C26—C25—Co2 | 71.9 (4) | O8—C43—C44 | 108.8 (3) |
C24—C25—H25 | 120.5 | O8—C43—H43A | 109.9 |
C26—C25—H25 | 120.5 | C44—C43—H43A | 109.9 |
Co2—C25—H25 | 133.2 | O8—C43—H43B | 109.9 |
C25—C26—C27 | 118.5 (6) | C44—C43—H43B | 109.9 |
C25—C26—Co2 | 69.0 (4) | H43A—C43—H43B | 108.3 |
C27—C26—Co2 | 111.2 (4) | O9—C44—C43 | 108.1 (3) |
C25—C26—H26 | 116.4 | O9—C44—H44A | 110.1 |
C27—C26—H26 | 116.4 | C43—C44—H44A | 110.1 |
Co2—C26—H26 | 116.4 | O9—C44—H44B | 110.1 |
C26—C27—C28 | 111.1 (4) | C43—C44—H44B | 110.1 |
C26—C27—H27A | 109.4 | H44A—C44—H44B | 108.4 |
C28—C27—H27A | 109.4 | C45—O9—C44 | 112.8 (3) |
C26—C27—H27B | 109.4 | C45—O9—K2 | 118.99 (18) |
C28—C27—H27B | 109.4 | C44—O9—K2 | 117.67 (18) |
H27A—C27—H27B | 108.0 | O9—C45—C46 | 108.8 (3) |
C22—C28—C27 | 110.7 (5) | O9—C45—H45A | 109.9 |
C22—C28—H28A | 109.5 | C46—C45—H45A | 109.9 |
C27—C28—H28A | 109.5 | O9—C45—H45B | 109.9 |
C22—C28—H28B | 109.5 | C46—C45—H45B | 109.9 |
C27—C28—H28B | 109.5 | H45A—C45—H45B | 108.3 |
H28A—C28—H28B | 108.1 | O10—C46—C45 | 108.4 (3) |
C23'—C22'—C28' | 122.7 (15) | O10—C46—H46A | 110.0 |
C23'—C22'—Co2 | 77.1 (15) | C45—C46—H46A | 110.0 |
C28'—C22'—Co2 | 110.6 (9) | O10—C46—H46B | 110.0 |
C23'—C22'—H22' | 113.6 | C45—C46—H46B | 110.0 |
C28'—C22'—H22' | 113.6 | H46A—C46—H46B | 108.4 |
Co2—C22'—H22' | 113.6 | C47—O10—C46 | 113.4 (3) |
C22'—C23'—C24' | 118.0 (16) | C47—O10—K2 | 112.57 (18) |
C22'—C23'—Co2 | 60.7 (12) | C46—O10—K2 | 108.41 (18) |
C24'—C23'—Co2 | 64.1 (16) | O10—C47—C48 | 108.3 (3) |
C22'—C23'—H23' | 121.0 | O10—C47—H47A | 110.0 |
C24'—C23'—H23' | 121.0 | C48—C47—H47A | 110.0 |
Co2—C23'—H23' | 154.0 | O10—C47—H47B | 110.0 |
C23'—C24'—C25' | 126.8 (17) | C48—C47—H47B | 110.0 |
C23'—C24'—Co2 | 74.2 (16) | H47A—C47—H47B | 108.4 |
C25'—C24'—Co2 | 74.2 (18) | O11—C48—C47 | 108.4 (3) |
C23'—C24'—H24' | 116.6 | O11—C48—H48A | 110.0 |
C25'—C24'—H24' | 116.6 | C47—C48—H48A | 110.0 |
Co2—C24'—H24' | 127.4 | O11—C48—H48B | 110.0 |
C26'—C25'—C24' | 119.3 (12) | C47—C48—H48B | 110.0 |
C26'—C25'—Co2 | 74.1 (13) | H48A—C48—H48B | 108.4 |
C24'—C25'—Co2 | 64.1 (16) | C48—O11—C49 | 112.8 (3) |
C26'—C25'—H25' | 120.3 | C48—O11—K2 | 115.52 (18) |
C24'—C25'—H25' | 120.3 | C49—O11—K2 | 117.40 (18) |
Co2—C25'—H25' | 134.7 | O11—C49—C50 | 108.8 (3) |
C25'—C26'—C27' | 120.4 (14) | O11—C49—H49A | 109.9 |
C25'—C26'—Co2 | 66.7 (15) | C50—C49—H49A | 109.9 |
C27'—C26'—Co2 | 105.7 (6) | O11—C49—H49B | 109.9 |
C25'—C26'—H26C | 117.4 | C50—C49—H49B | 109.9 |
C27'—C26'—H26C | 117.4 | H49A—C49—H49B | 108.3 |
Co2—C26'—H26C | 117.4 | O12—C50—C49 | 108.3 (3) |
C26'—C27'—C28' | 111.0 (9) | O12—C50—H50A | 110.0 |
C26'—C27'—H27C | 109.4 | C49—C50—H50A | 110.0 |
C28'—C27'—H27C | 109.4 | O12—C50—H50B | 110.0 |
C26'—C27'—H27D | 109.4 | C49—C50—H50B | 110.0 |
C28'—C27'—H27D | 109.4 | H50A—C50—H50B | 108.4 |
H27C—C27'—H27D | 108.0 | C51—O12—C50 | 113.4 (2) |
C22'—C28'—C27' | 110.8 (9) | C51—O12—K2 | 106.40 (18) |
C22'—C28'—H28C | 109.5 | C50—O12—K2 | 108.45 (18) |
C27'—C28'—H28C | 109.5 | O12—C51—C52 | 108.0 (3) |
C22'—C28'—H28D | 109.5 | O12—C51—H51A | 110.1 |
C27'—C28'—H28D | 109.5 | C52—C51—H51A | 110.1 |
H28C—C28'—H28D | 108.1 | O12—C51—H51B | 110.1 |
O4—K1—O6 | 117.70 (7) | C52—C51—H51B | 110.1 |
O4—K1—O2 | 116.76 (7) | H51A—C51—H51B | 108.4 |
O6—K1—O2 | 118.44 (7) | O7—C52—C51 | 108.6 (3) |
O4—K1—O1 | 153.61 (7) | O7—C52—H52A | 110.0 |
O6—K1—O1 | 59.43 (6) | C51—C52—H52A | 110.0 |
O2—K1—O1 | 59.01 (6) | O7—C52—H52B | 110.0 |
O4—K1—O3 | 59.05 (7) | C51—C52—H52B | 110.0 |
O6—K1—O3 | 156.35 (7) | H52A—C52—H52B | 108.3 |
O2—K1—O3 | 57.77 (6) | ||
C7—C1—C2—C3 | 35.8 (6) | C23—C22—C28—C27 | −39.7 (14) |
Co1—C1—C2—C3 | −64.5 (3) | Co2—C22—C28—C27 | 42.5 (9) |
K1—C1—C2—C3 | 84.6 (3) | C26—C27—C28—C22 | −36.4 (9) |
C7—C1—C2—Co1 | 100.3 (4) | C16—Co2—C22'—C23' | 133.2 (13) |
K1—C1—C2—Co1 | 149.06 (12) | C24'—Co2—C22'—C23' | −19.4 (15) |
C7—C1—C2—K1 | −48.8 (4) | C15—Co2—C22'—C23' | 169.2 (13) |
Co1—C1—C2—K1 | −149.06 (12) | C25'—Co2—C22'—C23' | −56.4 (14) |
C1—C2—C3—C4 | −30.0 (5) | C26'—Co2—C22'—C23' | −93.3 (13) |
Co1—C2—C3—C4 | −91.3 (3) | C16—Co2—C22'—C28' | −106.4 (12) |
K1—C2—C3—C4 | 51.1 (4) | C24'—Co2—C22'—C28' | 101.0 (13) |
C1—C2—C3—Co1 | 61.3 (3) | C15—Co2—C22'—C28' | −70.5 (14) |
K1—C2—C3—Co1 | 142.33 (15) | C23'—Co2—C22'—C28' | 120.4 (15) |
C2—C3—C4—C5 | 5.5 (6) | C25'—Co2—C22'—C28' | 64.0 (13) |
Co1—C3—C4—C5 | −62.0 (5) | C26'—Co2—C22'—C28' | 27.0 (13) |
C2—C3—C4—K1 | −47.6 (3) | C28'—C22'—C23'—C24' | −76 (4) |
Co1—C3—C4—K1 | −115.13 (16) | Co2—C22'—C23'—C24' | 30 (3) |
C3—C4—C5—C6 | 9.7 (7) | C28'—C22'—C23'—Co2 | −106.4 (14) |
K1—C4—C5—C6 | 66.2 (4) | C22'—C23'—C24'—C25' | 27 (6) |
C3—C4—C5—K1 | −56.5 (4) | Co2—C23'—C24'—C25' | 56 (4) |
C4—C5—C6—C7 | −0.9 (6) | C22'—C23'—C24'—Co2 | −29 (3) |
K1—C5—C6—C7 | 71.3 (4) | C23'—C24'—C25'—C26' | −4 (6) |
C4—C5—C6—K1 | −72.2 (4) | Co2—C24'—C25'—C26' | 52 (3) |
C5—C6—C7—C1 | −3.8 (7) | C23'—C24'—C25'—Co2 | −56 (4) |
K1—C6—C7—C1 | 68.4 (4) | C24'—C25'—C26'—C27' | 48 (4) |
C5—C6—C7—K1 | −72.1 (4) | Co2—C25'—C26'—C27' | 95.1 (14) |
C2—C1—C7—C6 | −16.2 (7) | C24'—C25'—C26'—Co2 | −47 (3) |
Co1—C1—C7—C6 | 59.6 (5) | C25'—C26'—C27'—C28' | −87.4 (19) |
K1—C1—C7—C6 | −65.2 (4) | Co2—C26'—C27'—C28' | −16 (2) |
C2—C1—C7—K1 | 49.0 (4) | C23'—C22'—C28'—C27' | 44 (2) |
Co1—C1—C7—K1 | 124.8 (2) | Co2—C22'—C28'—C27' | −43 (2) |
C14—C8—C9—C10 | 46.8 (4) | C26'—C27'—C28'—C22' | 38 (2) |
Co1—C8—C9—C10 | −55.3 (3) | C40—O1—C29—C30 | 176.3 (3) |
C14—C8—C9—Co1 | 102.1 (3) | K1—O1—C29—C30 | −60.1 (3) |
C8—C9—C10—C11 | 12.5 (5) | O1—C29—C30—O2 | 66.3 (3) |
Co1—C9—C10—C11 | −43.7 (3) | C29—C30—O2—C31 | 176.0 (3) |
C8—C9—C10—Co1 | 56.1 (3) | C29—C30—O2—K1 | −38.9 (3) |
C9—C10—C11—C12 | −2.7 (5) | C30—O2—C31—C32 | 178.7 (3) |
Co1—C10—C11—C12 | −46.3 (3) | K1—O2—C31—C32 | 34.5 (3) |
C9—C10—C11—Co1 | 43.6 (3) | O2—C31—C32—O3 | −64.0 (3) |
C10—C11—C12—C13 | −51.8 (5) | C31—C32—O3—C33 | −177.0 (2) |
Co1—C11—C12—C13 | −98.4 (3) | C31—C32—O3—K1 | 61.4 (3) |
C10—C11—C12—Co1 | 46.6 (3) | C32—O3—C33—C34 | 175.3 (3) |
C11—C12—C13—C14 | 36.0 (5) | K1—O3—C33—C34 | −61.9 (3) |
Co1—C12—C13—C14 | −42.0 (3) | O3—C33—C34—O4 | 69.3 (3) |
C12—C13—C14—C8 | 35.9 (4) | C33—C34—O4—C35 | −179.6 (3) |
C9—C8—C14—C13 | −88.9 (4) | C33—C34—O4—K1 | −39.5 (3) |
Co1—C8—C14—C13 | −13.0 (3) | C34—O4—C35—C36 | −178.3 (3) |
C21—C15—C16—C17 | −27.8 (6) | K1—O4—C35—C36 | 41.2 (4) |
Co2—C15—C16—C17 | 65.4 (3) | O4—C35—C36—O5 | −69.5 (4) |
K2—C15—C16—C17 | −81.4 (3) | C35—C36—O5—C37 | 177.2 (3) |
C21—C15—C16—Co2 | −93.2 (4) | C35—C36—O5—K1 | 59.1 (3) |
K2—C15—C16—Co2 | −146.80 (12) | C36—O5—C37—C38 | 175.7 (3) |
C21—C15—C16—K2 | 53.6 (3) | K1—O5—C37—C38 | −65.5 (3) |
Co2—C15—C16—K2 | 146.80 (12) | O5—C37—C38—O6 | 65.2 (3) |
C15—C16—C17—C18 | 33.9 (6) | C37—C38—O6—C39 | −176.5 (3) |
Co2—C16—C17—C18 | 95.2 (4) | C37—C38—O6—K1 | −30.2 (3) |
K2—C16—C17—C18 | −45.9 (4) | C38—O6—C39—C40 | −174.4 (3) |
C15—C16—C17—Co2 | −61.4 (3) | K1—O6—C39—C40 | 38.2 (3) |
K2—C16—C17—Co2 | −141.17 (13) | C29—O1—C40—C39 | −175.0 (3) |
C16—C17—C18—C19 | −12.3 (7) | K1—O1—C40—C39 | 60.8 (3) |
Co2—C17—C18—C19 | 55.9 (5) | O6—C39—C40—O1 | −66.8 (3) |
C16—C17—C18—K2 | 45.2 (4) | C52—O7—C41—C42 | −174.6 (3) |
Co2—C17—C18—K2 | 113.49 (19) | K2—O7—C41—C42 | 41.9 (3) |
C17—C18—C19—C20 | −7.6 (6) | O7—C41—C42—O8 | −64.5 (4) |
K2—C18—C19—C20 | −71.2 (3) | C41—C42—O8—C43 | 179.1 (3) |
C17—C18—C19—K2 | 63.5 (4) | C41—C42—O8—K2 | 54.8 (3) |
C18—C19—C20—C21 | 2.0 (6) | C42—O8—C43—C44 | 173.0 (3) |
K2—C19—C20—C21 | −73.8 (4) | K2—O8—C43—C44 | −61.4 (3) |
C18—C19—C20—K2 | 75.8 (4) | O8—C43—C44—O9 | 67.3 (3) |
C19—C20—C21—C15 | 9.0 (7) | C43—C44—O9—C45 | 177.5 (3) |
K2—C20—C21—C15 | −61.2 (4) | C43—C44—O9—K2 | −38.1 (3) |
C19—C20—C21—K2 | 70.2 (4) | C44—O9—C45—C46 | 173.8 (3) |
C16—C15—C21—C20 | 3.2 (7) | K2—O9—C45—C46 | 29.9 (3) |
Co2—C15—C21—C20 | −68.2 (5) | O9—C45—C46—O10 | −64.5 (4) |
K2—C15—C21—C20 | 56.6 (4) | C45—C46—O10—C47 | −168.7 (3) |
C16—C15—C21—K2 | −53.5 (3) | C45—C46—O10—K2 | 65.5 (3) |
Co2—C15—C21—K2 | −124.89 (17) | C46—O10—C47—C48 | −178.3 (3) |
C28—C22—C23—C24 | 60 (2) | K2—O10—C47—C48 | −54.8 (3) |
Co2—C22—C23—C24 | −42.2 (14) | O10—C47—C48—O11 | 69.0 (3) |
C28—C22—C23—Co2 | 102.4 (11) | C47—C48—O11—C49 | 173.5 (3) |
C22—C23—C24—C25 | −9 (3) | C47—C48—O11—K2 | −47.5 (3) |
Co2—C23—C24—C25 | −51.0 (13) | C48—O11—C49—C50 | 174.7 (3) |
C22—C23—C24—Co2 | 42.2 (14) | K2—O11—C49—C50 | 36.6 (3) |
C23—C24—C25—C26 | −1.4 (19) | O11—C49—C50—O12 | −68.3 (3) |
Co2—C24—C25—C26 | −52.0 (8) | C49—C50—O12—C51 | −178.6 (3) |
C23—C24—C25—Co2 | 50.6 (13) | C49—C50—O12—K2 | 63.4 (3) |
C24—C25—C26—C27 | −53.4 (11) | C50—O12—C51—C52 | 174.5 (3) |
Co2—C25—C26—C27 | −103.4 (5) | K2—O12—C51—C52 | −66.4 (3) |
C24—C25—C26—Co2 | 50.0 (9) | C41—O7—C52—C51 | −175.3 (3) |
C25—C26—C27—C28 | 91.0 (9) | K2—O7—C52—C51 | −31.7 (3) |
Co2—C26—C27—C28 | 14.1 (9) | O12—C51—C52—O7 | 67.4 (3) |
Co1—C2 | 1.924 (3) | Co2—C16 | 1.918 (3) |
Co1—C1 | 2.014 (4) | Co2—C15 | 2.005 (4) |
Co1—C9 | 2.035 (3) | Co2—C22 | 2.045 (15) |
Co1—C11 | 2.040 (3) | Co2—C24 | 2.046 (13) |
Co1—C12 | 2.055 (3) | Co2—C23 | 2.092 (13) |
Co1—C10 | 2.072 (3) | Co2—C25 | 2.113 (7) |
Co1—C8 | 2.105 (3) | Co2—C26 | 2.150 (5) |
Co1—C3 | 2.142 (3) | C15—C16 | 1.413 (5) |
C1—C7 | 1.430 (6) | C15—C21 | 1.468 (6) |
C1—C2 | 1.439 (6) | C15—K2 | 3.496 (3) |
C1—K1 | 3.436 (4) | C16—C17 | 1.410 (5) |
C2—C3 | 1.420 (5) | C16—K2 | 3.362 (4) |
C2—K1 | 3.307 (3) | C17—C18 | 1.404 (5) |
C3—C4 | 1.437 (5) | C18—C19 | 1.358 (5) |
C4—C5 | 1.353 (5) | C18—K2 | 3.411 (4) |
C4—K1 | 3.538 (4) | C19—C20 | 1.408 (6) |
C5—C6 | 1.398 (6) | C19—K2 | 3.207 (3) |
C5—K1 | 3.346 (4) | C20—C21 | 1.375 (6) |
C6—C7 | 1.354 (6) | C20—K2 | 3.201 (4) |
C6—K1 | 3.242 (4) | C21—K2 | 3.379 (4) |
C7—K1 | 3.295 (4) | C22—C23 | 1.425 (7) |
C8—C9 | 1.395 (4) | C22—C28 | 1.491 (9) |
C8—C14 | 1.515 (4) | C23—C24 | 1.424 (6) |
C9—C10 | 1.415 (5) | C24—C25 | 1.421 (6) |
C10—C11 | 1.421 (5) | C25—C26 | 1.428 (7) |
C11—C12 | 1.421 (5) | C26—C27 | 1.511 (8) |
C12—C13 | 1.502 (5) | C27—C28 | 1.532 (10) |
C13—C14 | 1.507 (5) |
Bond | (I)a | (I)b | NEFYIIc | SEKJOHd | SEKJIBe |
M—C1 | 2.014 (4) | 2.005 (4) | 2.287 (5) | 2.252 (7) | 2.244 (5) |
M—C2 | 1.924 (3) | 1.918 (3) | 2.147 (6) | 2.113 (7) | 2.124 (5) |
M—C3 | 2.142 (3) | 2.186 (4) | 2.213 (6) | 2.230 (7) | 2.244 (5) |
C1—C2 | 1.439 (6) | 1.413 (5) | 1.388 (8) | 1.425 (11) | 1.439 (8) |
C2—C3 | 1.420 (5) | 1.410 (5) | 1.420 (8) | 1.432 (10) | 1.448 (8) |
C3—C4 | 1.437 (5) | 1.404 (5) | 1.446 (11) | 1.468 (10) | 1.459 (8) |
C4—C5 | 1.353 (5) | 1.358 (5) | 1.349 (12) | 1.350 (10) | 1.348 (8) |
C5—C6 | 1.398 (6) | 1.408 (6) | 1.419 (10) | 1.429 (12) | 1.438 (9) |
C6—C7 | 1.354 (6) | 1.375 (6) | 1.338 (8) | 1.358 (11) | 1.342 (9) |
C7—C1 | 1.430 (6) | 1.468 (6) | 1.461 (8) | 1.462 (10) | 1.455 (8) |
Fold angle | 28.0 (4) | 27.2 (4) | 29.6 | 35.8 | 37.1 |
Notes: (a) (I), ring C1–C7; (b) (I), ring C15–C21; (c) [Pd(η3-C7H7)(PPh3)2][BF4] (Murahashi et al., 2012); (d) [AsPh4][Ru(η3-C7H7)(CO)3] (Astley et al., 1990); (e) [AsPh4][Os(η3-C7H7)(CO)3] (Astley et al., 1990). |
Experimental details
Crystal data | |
Chemical formula | [K(C12H24O6)][Co(C7H7)(C7H9)] |
Mr | 546.61 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 173 |
a, b, c (Å) | 16.3925 (19), 17.225 (2), 18.678 (2) |
β (°) | 91.6077 (19) |
V (Å3) | 5271.8 (11) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.85 |
Crystal size (mm) | 0.32 × 0.24 × 0.16 |
Data collection | |
Diffractometer | Siemens SMART CCD platform diffractometer |
Absorption correction | Multi-scan (TWINABS; Sheldrick, 2012) |
Tmin, Tmax | 0.612, 0.746 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 85092, 12058, 9117 |
Rint | 0.055 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.084, 1.00 |
No. of reflections | 12058 |
No. of parameters | 728 |
No. of restraints | 45 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.46, −0.47 |
Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SIR97 (Altomare et al., 1999), SHELXL2014 (Sheldrick, 2015), SHELXTL (Sheldrick, 2015).
Acknowledgements
This research has been supported by the US National Science Foundation and the donors of the Petroleum Research Fund, administered by the American Chemical Society. The authors thank Dr Victor G. Young Jr for supplying the original data for re-integration with the latest software.
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