metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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Di­ethano­laminium cyclo-octa-μ2-fluoro-hexa­deca-μ2-tri­methyl­acetato-κ32O:O′-hepta­chromium(III)nickel(II) eth­yl acetate 0.5-solvate

aDepartment of Chemistry, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C, Denmark, and bSchool of Chemistry, The University of Manchester, Oxford Road, Manchester M13 9PL, England
*Correspondence e-mail: kre@chem.au.dk

(Received 3 May 2005; accepted 21 June 2005; online 13 July 2005)

The title compound, [N(C2H4OH)2H2][Cr7NiF8(C5H9O2)16]·0.5C4H8O2, is a heterometallic wheel templated by a protonated amino alcohol. It consists of an octa­gon of metal centres, with each edge of the octa­gon bridged by a single F anion and two carboxyl­ate groups. Each metal atom is octa­hedrally coordinated. The protonated amine mol­ecule protrudes through the cavity of the ring, while a solvent eth­yl acetate mol­ecule fills up the vacant space between the ring anions. It appears that the one equivalent of Ni atoms is unevenly distributed among the eight metal sites.

Comment

Our recent report (Larsen, McInnes et al., 2003[Larsen, F. K., McInnes, E. J. L., El Mkami, H., Overgaard, J., Piligkos, S., Rajaraman, G., Rentschler, E., Smith, A. A., Smith, G. M., Boote, V., Jennings, M., Timco G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 101-105.]) of a series of octa­nuclear {Cr7M} heterometallic wheel-type complexes with the general formula [NR2H2][Cr7MF8(O2CCMe3)16] was the first report of anti-ferromagnetically coupled cyclic mol­ecules that have a non-diamagnetic ground state. There has been considerable inter­est in such mol­ecules for applications as diverse as olefin polymerization catalysis (Lassahn et al., 2004[Lassahn, P.-G., Lozan, V., Timco, G. A., Christian, P., Janiak C. & Winpenny, R. E. P. (2004). J. Catal. 222, 260-267.]), magnetic cooling (Affronte et al., 2004[Affronte, M., Ghirri, A., Carretta, S., Amoretti, G., Piligkos, S., Timco, G. A. & Winpenny, R. E. P. (2004). Appl. Phys. Lett. 84, 3468-3470.]) and quantum computing (Meier et al., 2003[Meier, F., Levy, J. & Loss, D. (2003). Phys. Rev. Lett. 90, 047901-1.]). They were synthesized using a secondary ammonium cation, [NR2H2]+, which is a protonated alk­yl-chain secondary amine with R = CH3(CH2)n (e.g. n = 0–7). It acts as a template in the reaction of CrF3·4H2O with pivalic acid in the presence of a second divalent metal cation (M2+ = Ni, Co, Mn, Fe, Zn or Cd). This procedure gives {Cr7M} ring compounds in good yield (Larsen, Overgaard et al., 2003[Larsen, F. K., Overgaard, J., Parsons, S., Rentschler, E., Smith, A. A., Timco, G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 5978-5981.]; Larsen, McInnes et al., 2003[Larsen, F. K., McInnes, E. J. L., El Mkami, H., Overgaard, J., Piligkos, S., Rajaraman, G., Rentschler, E., Smith, A. A., Smith, G. M., Boote, V., Jennings, M., Timco G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 101-105.]). In each case, the amines are found to be hydrogen-bonded at the centre of the metal ring. The protonated N atoms are not involved in the packing of the mol­ecules in the crystal structure, because they are accommodated completely in the cavity (void) of the wheels. However, it was found that the choice of R can influence the packing of the rings in the crystal structure, regardless of the solvent used for crystallization. For example, both short and very long alk­yl chains lead to packing where the octa­nuclear wheels are coplanar (generally tetra­gonal or orthorhombic crystals), but for inter­mediate chain lengths (Et or nPr), monoclinic crystals are found, where the rings pack with an angle of ca 50° between the mean planes of neighbouring rings (Larsen, Overgaard et al., 2003[Larsen, F. K., Overgaard, J., Parsons, S., Rentschler, E., Smith, A. A., Timco, G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 5978-5981.]).

The purpose of this paper is to extend further our studies of heterometallic wheels, by the preparation and structural characterization of the new title complex, [N(CH2CH2OH)2H2][Cr7NiF8(O2CCMe3)16][C4H8O2]0.5, (I)[link]. Using a protonated secondary amino alcohol as a template, we wished to investigate the influence of the alcohol group on the accommodation of the amine group in the void of the wheel, and also how the –OH group might influence the packing of the anionic rings in the crystal structure. A further goal was to obtain a complex for the synthesis of further polymetallic cage complexes, using the two OH groups of the diethano­lamine to bind to further metal centres.

[Scheme 1]

For five of the 16 bridging pivalate groups in (I)[link], two possible positions were located and refined for the tert-but­yl meth­yl groups. The occupation factors for the major component of these five disordered pivalate groups, of which two are on either face, while one is on the edge of the circular ring mol­ecule, are in the range 0.521 (10)–0.592 (9). For all pivalate groups, a restraint was imposed in order to maintain tetra­hedral coordination of the CMe3 groups, and a common C—C bond length was restrained to 1.521 (1) Å.

Compound (I)[link] was crystallized from an eth­yl acetate solution and a mol­ecule of eth­yl acetate is incorporated in the crystal structure. It is situated near a centre of symmetry and is disordered over two positions, with two of the atom positions coinciding. The protonated ethano­lamine mol­ecule appears to be disordered over three orientations in the void of the octa­gonal ring, with one major [0.444 (5)] and two minor [0.251 (5) and 0.302 (5)] orientations. The amine N atom of the main component sits significantly closer to one side of the ring than the other. The N⋯F distances vary systematically around the ring: N1⋯F1 = 3.104 (3), N1⋯F2 = 3.408 (3), N1⋯F3 = 3.730 (3), N1⋯F4 = 3.829 (3), N1⋯F5 = 3.557 (3), N1⋯F6 = 3.215 (3), N1⋯F7 = 2.878 (3) and N1⋯F8 = 2.855 (3) Å.

In the final cycles of refinement, all Cr/Ni atoms were refined using Cr scattering factors. The metal atoms on the side of the ring with the shorter N⋯F separations tend to have smaller values for their equivalent isotropic displacement parameters: Ueq(Cr1) = 0.0238 (1), Ueq(Cr2) = 0.0281 (1), Ueq(Cr3) = 0.0286 (1), Ueq(Cr4) = 0.0308 (1), Ueq(Cr5) = 0.0234 (1), Ueq(Cr6) = 0.0222 (1), Ueq(Cr7) = 0.0238 (1) and Ueq(Cr8) = 0.0257 (1) Å2. Since Ni has four more electrons than Cr, it is conceivable that the Cr atoms with lower Ueq values may have greater Ni occupancy, so there is an indication of an uneven distribution of Ni around the ring.

The O atoms of the ethano­lamine mol­ecule are found to have short distances to the same F atoms which are involved in the shortest N⋯F separation [O2A⋯F1 = 2.952 (3) and O2B⋯F8 = 2.933 (3) Å]. The minor disorder components of the ethano­lammonium cation show short N⋯F distances to other F atoms than found for the major component and of similar lengths: N1C⋯F1 = 2.721 (3), N1C⋯F2 = 2.922 (3) and N1C⋯F8 = 2.939 (3) Å, and N1E⋯F6 = 2.837 (3), N1E⋯F7 = 2.940 (3) and N1E⋯F5 = 3.084 (3) Å.

[Figure 1]
Figure 1
A view of (I)[link], showing 50% displacement ellipsoids, with selected atoms labelled. Only one orientation is shown for the disorder components. Colour key: Cr/Ni green, F pink, O red, C grey, N blue. H atoms have been omitted.

Experimental

Compound (I)[link] was synthesized in approximately 65% yield in a similar way to the analogues reported earlier (Larsen, Overgaard et al., 2003[Larsen, F. K., Overgaard, J., Parsons, S., Rentschler, E., Smith, A. A., Timco, G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 5978-5981.]), except that the amine used was diethano­lamine and the product was crystallized from eth­yl acetate. Elemental analysis (dried sample), calculated for C84H156Cr7F8N1Ni1O34: Cr 15.83, Ni 2.55, C 43.89, H 6.84, N 0.61%; found: Cr 15.28, Ni 2.72, C 43.89, H 7.00, N 0.62%. ES–MS (2 THF/MeOH m/z): −2191 [Cr7NiF8(O2CCMe3)16], 2298 [M], 2321 [M+Na]+.

Crystal data
  • (C4H12NO2)[Cr7NiF8(C5H9O2)16]·0.5C4H8O2

  • Mr = 2342.85

  • Monoclinic, P 21 /c

  • a = 24.9892 (15) Å

  • b = 16.6220 (9) Å

  • c = 30.8299 (19) Å

  • β = 110.506 (3)°

  • V = 11994.4 (12) Å3

  • Z = 4

  • Dx = 1.294 Mg m−3

  • Mo Kα radiation

  • Cell parameters from 9946 reflections

  • θ = 2.2–31.0°

  • μ = 0.78 mm−1

  • T = 100 (2) K

  • Block, green

  • 0.38 × 0.3 × 0.25 mm

Data collection
  • Bruker X8 APEX-II diffractometer

  • φ and ω scans

  • Absorption correction: multi-scan(SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.])Tmin = 0.723, Tmax = 0.823

  • 209153 measured reflections

  • 38517 independent reflections

  • 28754 reflections with I > 2σ(I)

  • Rint = 0.035

  • θmax = 31.1°

  • h = −36 → 35

  • k = −23 → 24

  • l = −44 → 44

Refinement
  • Refinement on F2

  • R[F2 > 2σ(F2)] = 0.091

  • wR(F2) = 0.258

  • S = 1.04

  • 38517 reflections

  • 1066 parameters

  • H-atom parameters constrained

  • w = 1/[σ2(Fo2) + (0.1134P)2 + 52.1149P] where P = (Fo2 + 2Fc2)/3

  • (Δ/σ)max = 0.006

  • Δρmax = 2.10 e Å−3

  • Δρmin = −1.17 e Å−3

Meth­yl H atoms were located in idealized positions, with C—H = 0.98 Å, and refined as riding, with the constraint Uiso(H) = 1.5Uiso(C). N-bound H atoms were located in idealized positions, with N—H = 0.92 Å, and refined as riding, with the constraint Uiso(H) = 1.2Uiso(N). The highest difference peak is 0.39 Å from H20C and the deepest difference hole is 0.51 Å from C28.

Data collection: APEX-II (Bruker–Nonius, 2004[Bruker-Nonius (2004). APEX-II and SAINT-Plus (Version 7.06a). Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker–Nonius, 2004[Bruker-Nonius (2004). APEX-II and SAINT-Plus (Version 7.06a). Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.]); molecular graphics: SHELXL97; software used to prepare material for publication: enCIFer (Version 1.1; Allen et al., 2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]) and WinGX (Version 1.70.00; Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supporting information


Comment top

Our recent report (Larsen et al., 2003) Please specify unique reference of a series of octanuclear {Cr7M} heterometallic wheel-type complexes with the general formula [NR2H2][Cr7MF8(O2CCMe3)16] was the first report of anti-ferromagnetically coupled cyclic molecules that have a non-diamagnetic ground state. There has been considerable interest in such molecules for applications as diverse as olefin polymerization catalysis (Lassahn et al., 2004), magnetic cooling (Affronte et al., 2004) and quantum computing (Meier et al., 2003). They were synthesized using an ammonia cation, [NR2H2]+, which is a protonated alkyl-chain secondary amine with R = CH3(CH2)n (e.g. n = 0–7). It acts as a template in the reaction of CrF3·4H2O with pivalic acid in the presence of a second divalent metal cation (M2+ = Ni, Co, Mn, Fe, Zn or Cd). This procedure gives {Cr7M} ring compounds in good yield (Larsen, Overgaard et al., 2003; Larsen, McInnes et al., 2003). In each case, the amines are found to be hydrogen-bonded at the centre of the metal ring. The protonated N atoms are not involved in the packing of the molecules in the crystal lattice, because they are accommodated completely in the cavity (void) of the wheels. However, it was found that the choice of R can influence the packing of the rings in the crystal lattice, regardless of the solvent used for crystallization. For example, both short and very long alkyl chains lead to packing where the octanuclear wheels are coplanar (generally tetragonal or orthorhombic crystals), but for intermediate chain lengths (Et or nPr), monoclinic crystals are found, where the rings pack with an angle of ca 50° between the mean planes of neighbouring rings (Larsen, Overgaard et al., 2003).

The purpose of this paper is to extend further our studies of heterometallic wheels, by the preparation and structural characterization of the title new complex, [N(CH2CH2OH)2H2][Cr7NiF8(O2CCMe3)16][C4H8O2]0.5, (I). Using as a template a protonated secondary amino alcohol, we wished to investigate the influence of the alcohol group on the accommodation of the amine group in the void of the wheel and also how the –OH group might influence the packing of the ring molecules in the crystal lattice. A further goal was to obtain a complex for the synthesis of further polymetallic cage complexes, using the two OH groups of the diethanolamine to bind to further metal centres.

For five of the 16 bridging pivalate groups in (I), two possible positions were located and refined for the tert-butyl methyl groups. The occupation factors for the major component of these five disordered pivalate groups, of which two are on either face, while one is on the edge of the circular ring molecule, are in the range 0.521 (10)–0.592 (9). For all pivalate groups, a constraint was imposed in order to maintain tetrahedral coordination of the CMe3 moieties, and a common C—C bond length was restrained to 1.521 (1) Å.

Compound (I) was crystallized from an ethyl acetate solution and a molecule of ethyl acetate is incorporated in the crystal structure. It is situated near a centre of symmetry and is disordered over two positions, with two of the atom positions coinciding. The ethanolamine molecule appears to be disordered over three orientations in the void of the octagonal ring, with one major [0.444 (5)] and two minor [0.251 (5) and 0.302 (5)] orientations. The amine N atom of the main component sits significantly closer to one side of the ring than the other. The N—F distances vary systematically around the ring: N1—F1 = 3.104 (3), N1—F2 = 3.408 (3), N1—F3 = 3.730 (3), N1—F4 = 3.829 (3), N1—F5 = 3.557 (3), N1—F6 = 3.215 (3), N1—F7 = 2.878 (3) and N1—F8 = 2.855 (3) Å.

In the final cycles of refinement, all Cr/Ni atoms were refined using Cr scattering factors. The metal atoms on the side of the ring with the shorter N—F separations tend to have smaller values for their equivalent isotropic displacement parameters: Ueq(Cr1) = 0.0238 (1), Ueq(Cr2) = 0.0281 (1), Ueq(Cr3) = 0.0286 (1), Ueq(Cr4) = 0.0308 (1), Ueq(Cr5) = 0.0234 (1), Ueq(Cr6) = 0.0222 (1), Ueq(Cr7) = 0.0238 (1) and Ueq(Cr8) = 0.0257 (1) Å2. Since Ni has four more electrons than Cr, it is conceivable that the Cr atoms with lower Ueq values may have greater Ni occupancy, so there is indication of an uneven distribution of Ni around the ring.

The O atoms of the ethanolamine molecule are found to have short distances to the same F atoms which are involved in the shortest N—F separation [O2A—F1 = 2.952 (3) and O2B—F8 = 2.933 (3) Å]. The minor disorder components of the ethanolammonium cation show short N—F distances to other F atoms than found for the major component and of similar lengths: N1C—F1 = 2.721 (3), N1C—F2 = 2.922 (3) and N1C—F8 = 2.939 (3) Å, and N1E—F6 = 2.837 (3), N1E—F7 = 2.940 (3) and N1E—F5 = 3.084 (3) Å.

Experimental top

Compound (I) was synthesized in approximately 65% yield in a similar way to the analogues reported earlier (Larsen, Overgaard et al., 2003), except that the amine used was diethanolamine and the product was crystallized from ethyl acetate. Elemental analysis (dried sample), calculated for C84H156Cr7F8N1Ni1O34: Cr 15.83, Ni 2.55, C 43.89, H 6.84, N 0.61%; found: Cr 15.28, Ni 2.72, C 43.89, H 7.00, N 0.62%. ES–MS (2 THF/MeOH m/z): -2191 [Cr7NiF8(O2CCMe3) 16], 2298 [M-], 2321 [M+Na]+.

Refinement top

Methyl H atoms were located in idealized positions, with C—H = 0.98 Å, and refined as riding, with the constraint Uiso(H) = 1.5Uiso(C). N-bound H atoms were located in idealized positions, with N—H = 0.92 Å, and refined as riding, with the constraint Uiso(H) = 1.2Uiso(N). Please check added text. The highest difference peak is 0.39 Å from H20C and the deepest difference hole is 0.51 Å from C28.

Computing details top

Data collection: SMART (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: enCIFer (Version 1.1; Allen et al., 2004) and WinGX (Version 1.70.00; Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of (I), showing 50% displacement ellipsoids, with selected atoms labelled. Only one orientation is shown for the disorder components. Colour key: Cr/Ni green, F pink, O red, C grey, N blue.
Diethanolaminium cyclo-octa-µ2-fluoro-hexadeca-µ2-trimethylacetato-κ2O:O'- heptachromium(III)nickel(II) ethyl acetate 0.5-solvate top
Crystal data top
(C4H12NO2)[Cr7NiF8(C5H9O2)16]·0.5C4H8O2F(000) = 4908
Mr = 2342.85Dx = 1.294 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9946 reflections
a = 24.9892 (15) Åθ = 2.2–31.0°
b = 16.6220 (9) ŵ = 0.78 mm1
c = 30.8299 (19) ÅT = 100 K
β = 110.506 (3)°Block, green
V = 11994.4 (12) Å30.38 × 0.3 × 0.25 mm
Z = 4
Data collection top
Bruker X8 APEX-II
diffractometer
38517 independent reflections
Radiation source: fine-focus sealed tube28754 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 83.33 pixels mm-1θmax = 31.1°, θmin = 2.5°
ϕ and ω scansh = 3635
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 2324
Tmin = 0.723, Tmax = 0.823l = 4444
209153 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.091Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.258H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.1134P)2 + 52.1149P]
where P = (Fo2 + 2Fc2)/3
38517 reflections(Δ/σ)max = 0.006
1066 parametersΔρmax = 2.10 e Å3
141 restraintsΔρmin = 1.17 e Å3
Crystal data top
(C4H12NO2)[Cr7NiF8(C5H9O2)16]·0.5C4H8O2V = 11994.4 (12) Å3
Mr = 2342.85Z = 4
Monoclinic, P21/cMo Kα radiation
a = 24.9892 (15) ŵ = 0.78 mm1
b = 16.6220 (9) ÅT = 100 K
c = 30.8299 (19) Å0.38 × 0.3 × 0.25 mm
β = 110.506 (3)°
Data collection top
Bruker X8 APEX-II
diffractometer
38517 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
28754 reflections with I > 2σ(I)
Tmin = 0.723, Tmax = 0.823Rint = 0.035
209153 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.091141 restraints
wR(F2) = 0.258H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.1134P)2 + 52.1149P]
where P = (Fo2 + 2Fc2)/3
38517 reflectionsΔρmax = 2.10 e Å3
1066 parametersΔρmin = 1.17 e Å3
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cr10.24845 (2)0.30732 (3)0.53149 (2)0.02378 (12)
Cr20.17266 (3)0.23451 (4)0.59513 (2)0.02810 (13)
Cr30.12131 (3)0.31986 (4)0.67277 (2)0.02856 (13)
Cr40.15764 (3)0.48148 (4)0.74459 (2)0.03080 (14)
Cr50.22740 (2)0.65434 (3)0.740880 (19)0.02338 (12)
Cr60.32644 (2)0.70831 (3)0.694543 (19)0.02222 (11)
Cr70.35228 (2)0.64380 (4)0.599364 (19)0.02382 (12)
Cr80.33790 (2)0.46585 (4)0.543084 (19)0.02571 (12)
F10.19865 (10)0.32329 (14)0.56776 (9)0.0325 (5)
F20.18121 (10)0.30385 (14)0.64808 (8)0.0319 (5)
F30.14510 (10)0.43013 (13)0.68579 (8)0.0302 (5)
F40.21990 (10)0.53930 (14)0.73597 (8)0.0303 (5)
F50.25624 (9)0.65394 (13)0.69092 (7)0.0270 (4)
F60.33767 (10)0.62235 (13)0.65650 (7)0.0283 (4)
F70.30798 (10)0.54933 (16)0.57288 (8)0.0333 (5)
F80.29877 (11)0.38951 (15)0.56946 (8)0.0346 (5)
O110.19584 (14)0.2266 (2)0.49306 (11)0.0409 (7)
O120.16241 (13)0.16393 (19)0.54221 (12)0.0398 (7)
O130.29402 (13)0.22558 (19)0.57568 (12)0.0398 (7)
O140.25123 (14)0.1987 (2)0.62736 (12)0.0426 (7)
O210.14561 (14)0.14517 (18)0.62421 (12)0.0391 (7)
O220.09468 (14)0.20917 (18)0.66065 (11)0.0374 (6)
O230.09225 (12)0.26815 (18)0.56420 (10)0.0323 (6)
O240.06884 (12)0.35197 (18)0.61191 (10)0.0338 (6)
O310.05925 (14)0.3370 (2)0.69615 (11)0.0390 (7)
O320.09342 (15)0.4260 (2)0.75357 (11)0.0423 (8)
O330.17371 (15)0.28622 (19)0.73370 (10)0.0411 (7)
O340.21066 (16)0.3958 (2)0.77585 (11)0.0438 (8)
O410.17130 (15)0.5347 (2)0.80388 (10)0.0419 (7)
O420.19833 (12)0.65794 (17)0.79206 (9)0.0291 (5)
O430.10292 (12)0.56438 (18)0.71131 (10)0.0338 (6)
O440.15052 (12)0.66674 (19)0.69496 (10)0.0329 (6)
O510.23345 (12)0.77042 (16)0.74569 (10)0.0304 (5)
O520.31486 (12)0.79640 (16)0.73316 (10)0.0303 (5)
O530.30420 (11)0.64100 (16)0.78710 (9)0.0261 (5)
O540.36780 (12)0.64591 (18)0.75064 (9)0.0303 (5)
O610.39856 (12)0.75736 (18)0.69798 (10)0.0329 (6)
O620.39842 (12)0.73888 (18)0.62611 (10)0.0315 (6)
O630.28298 (12)0.77293 (16)0.64041 (9)0.0294 (5)
O640.28194 (12)0.70839 (19)0.57637 (10)0.0343 (6)
O710.36455 (14)0.6663 (2)0.54189 (10)0.0378 (7)
O720.37709 (13)0.5440 (2)0.51640 (10)0.0391 (7)
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C1C0.2744 (12)0.4412 (13)0.6770 (15)0.0521 (18)*0.251 (4)
H1C10.29160.49450.68790.063*0.251 (4)
H1C20.25200.42480.69640.063*0.251 (4)
N1C0.2365 (8)0.4472 (12)0.6285 (6)0.0456 (17)*0.251 (4)
H1C30.25890.43870.61080.055*0.251 (4)
H1C40.21180.40420.62320.055*0.251 (4)
C1D0.2050 (13)0.5106 (14)0.6111 (10)0.0521 (18)*0.251 (4)
H1D10.22040.52540.58660.063*0.251 (4)
H1D20.22260.55000.63620.063*0.251 (4)
C2D0.1492 (10)0.5433 (9)0.5920 (8)0.0533 (15)*0.251 (4)
H2D10.13240.53210.55840.064*0.251 (4)
H2D20.12380.52100.60750.064*0.251 (4)
O2D0.1574 (8)0.6220 (9)0.6000 (7)0.0651 (13)*0.251 (4)
O2E0.3730 (6)0.4797 (9)0.7166 (5)0.0651 (13)*0.302 (5)
C2E0.3278 (7)0.4363 (11)0.7159 (7)0.0533 (15)*0.302 (5)
H2E10.32030.44530.74500.064*0.302 (5)
H2E20.33630.37840.71410.064*0.302 (5)
C1E0.2824 (8)0.4551 (15)0.6808 (12)0.0521 (18)*0.302 (5)
H1E10.26740.40040.67080.063*0.302 (5)
H1E20.25800.47540.69770.063*0.302 (5)
N1E0.2587 (7)0.4936 (10)0.6413 (6)0.0456 (17)*0.302 (5)
H1E30.26620.46160.61980.055*0.302 (5)
H1E40.28100.53870.64410.055*0.302 (5)
C1F0.1998 (12)0.5223 (13)0.6177 (7)0.0521 (18)*0.302 (5)
H1F10.17520.48960.63000.063*0.302 (5)
H1F20.19850.57800.62880.063*0.302 (5)
C2F0.1720 (13)0.5244 (10)0.5688 (8)0.0533 (15)*0.302 (5)
H2F10.18760.48290.55340.064*0.302 (5)
H2F20.13030.51630.56000.064*0.302 (5)
O2F0.1839 (7)0.5984 (8)0.5579 (5)0.0651 (13)*0.302 (5)
O990.4693 (4)0.5143 (7)0.9913 (4)0.164 (4)*
C990.4441 (9)0.5166 (7)1.0299 (7)0.181 (7)*
O980.4767 (11)0.4978 (13)1.0601 (10)0.192 (10)*0.50
C980.3844 (10)0.5449 (15)1.0045 (9)0.129 (8)*0.50
H98A0.36600.50910.97820.194*0.50
H98B0.38540.59980.99320.194*0.50
H98C0.36270.54431.02550.194*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0180 (2)0.0254 (3)0.0247 (3)0.00061 (19)0.00350 (19)0.0014 (2)
Cr20.0238 (3)0.0240 (3)0.0340 (3)0.0023 (2)0.0072 (2)0.0009 (2)
Cr30.0337 (3)0.0261 (3)0.0229 (3)0.0072 (2)0.0061 (2)0.0003 (2)
Cr40.0382 (3)0.0297 (3)0.0224 (3)0.0123 (2)0.0080 (2)0.0024 (2)
Cr50.0227 (2)0.0247 (3)0.0194 (2)0.00281 (19)0.00320 (19)0.00213 (19)
Cr60.0235 (2)0.0214 (2)0.0192 (2)0.00308 (19)0.00432 (19)0.00107 (18)
Cr70.0211 (2)0.0301 (3)0.0197 (2)0.0060 (2)0.00641 (19)0.0007 (2)
Cr80.0200 (2)0.0357 (3)0.0199 (2)0.0056 (2)0.00509 (19)0.0050 (2)
F10.0266 (10)0.0292 (11)0.0396 (13)0.0005 (9)0.0090 (9)0.0003 (9)
F20.0301 (11)0.0327 (11)0.0278 (11)0.0046 (9)0.0039 (9)0.0011 (9)
F30.0387 (12)0.0251 (10)0.0237 (10)0.0068 (9)0.0072 (9)0.0003 (8)
F40.0339 (11)0.0281 (11)0.0251 (10)0.0056 (9)0.0055 (9)0.0013 (8)
F50.0266 (10)0.0293 (10)0.0215 (9)0.0049 (8)0.0039 (8)0.0025 (8)
F60.0332 (11)0.0287 (10)0.0232 (10)0.0046 (9)0.0099 (8)0.0026 (8)
F70.0298 (11)0.0448 (13)0.0250 (10)0.0113 (10)0.0093 (9)0.0041 (9)
F80.0388 (13)0.0334 (12)0.0257 (11)0.0041 (10)0.0037 (9)0.0006 (9)
O110.0400 (16)0.0384 (16)0.0396 (16)0.0095 (13)0.0080 (13)0.0114 (13)
O120.0341 (15)0.0307 (14)0.0542 (19)0.0060 (12)0.0149 (14)0.0086 (13)
O130.0276 (14)0.0365 (15)0.0490 (18)0.0057 (11)0.0056 (13)0.0100 (13)
O140.0369 (16)0.0389 (17)0.0452 (18)0.0025 (13)0.0059 (14)0.0119 (14)
O210.0398 (16)0.0281 (14)0.0512 (19)0.0024 (12)0.0184 (14)0.0049 (13)
O220.0458 (17)0.0290 (14)0.0391 (16)0.0100 (12)0.0170 (13)0.0015 (12)
O230.0269 (13)0.0353 (14)0.0330 (14)0.0033 (11)0.0084 (11)0.0051 (11)
O240.0310 (14)0.0352 (14)0.0298 (14)0.0022 (11)0.0040 (11)0.0052 (11)
O310.0446 (17)0.0399 (16)0.0356 (15)0.0147 (13)0.0178 (13)0.0095 (12)
O320.0535 (19)0.0455 (18)0.0318 (15)0.0232 (15)0.0199 (14)0.0101 (13)
O330.0556 (19)0.0310 (14)0.0274 (14)0.0081 (13)0.0031 (13)0.0060 (11)
O340.057 (2)0.0355 (16)0.0273 (14)0.0120 (14)0.0002 (13)0.0053 (12)
O410.058 (2)0.0424 (17)0.0265 (14)0.0203 (15)0.0162 (14)0.0070 (12)
O420.0320 (13)0.0316 (13)0.0240 (12)0.0042 (10)0.0099 (10)0.0009 (10)
O430.0296 (13)0.0365 (15)0.0343 (14)0.0055 (11)0.0096 (11)0.0053 (12)
O440.0260 (13)0.0401 (15)0.0268 (13)0.0020 (11)0.0018 (10)0.0059 (11)
O510.0307 (13)0.0234 (12)0.0339 (14)0.0001 (10)0.0073 (11)0.0024 (10)
O520.0312 (13)0.0257 (12)0.0318 (13)0.0043 (10)0.0083 (11)0.0027 (10)
O530.0237 (11)0.0307 (13)0.0204 (11)0.0023 (9)0.0032 (9)0.0018 (9)
O540.0298 (13)0.0378 (14)0.0208 (11)0.0038 (11)0.0058 (10)0.0034 (10)
O610.0297 (13)0.0359 (14)0.0299 (13)0.0078 (11)0.0065 (11)0.0013 (11)
O620.0281 (13)0.0339 (14)0.0308 (13)0.0096 (11)0.0083 (11)0.0022 (11)
O630.0301 (13)0.0271 (12)0.0272 (12)0.0004 (10)0.0056 (10)0.0061 (10)
O640.0304 (14)0.0440 (16)0.0237 (12)0.0013 (12)0.0036 (11)0.0030 (11)
O710.0395 (16)0.0469 (17)0.0304 (14)0.0072 (13)0.0164 (12)0.0059 (12)
O720.0303 (14)0.060 (2)0.0301 (14)0.0110 (13)0.0147 (12)0.0077 (13)
O730.0218 (12)0.0435 (16)0.0286 (13)0.0050 (11)0.0060 (10)0.0013 (11)
O740.0350 (16)0.0436 (18)0.0416 (17)0.0045 (13)0.0073 (13)0.0041 (14)
O810.0248 (13)0.0529 (19)0.0423 (17)0.0023 (12)0.0090 (12)0.0165 (14)
O820.0274 (14)0.0489 (18)0.0422 (17)0.0003 (12)0.0091 (12)0.0115 (14)
O830.0321 (14)0.0429 (16)0.0231 (12)0.0047 (12)0.0076 (11)0.0022 (11)
O840.0227 (13)0.0508 (18)0.0375 (16)0.0020 (12)0.0016 (11)0.0089 (13)
C110.0240 (17)0.0305 (18)0.044 (2)0.0014 (14)0.0014 (16)0.0079 (16)
C120.046 (3)0.041 (3)0.069 (4)0.008 (2)0.016 (2)0.026 (2)
C160.0255 (17)0.0224 (17)0.061 (3)0.0016 (13)0.0029 (18)0.0101 (17)
C170.045 (3)0.049 (3)0.090 (5)0.017 (2)0.002 (3)0.036 (3)
C210.039 (2)0.0261 (17)0.042 (2)0.0062 (15)0.0112 (18)0.0054 (15)
C220.065 (3)0.028 (2)0.076 (4)0.012 (2)0.037 (3)0.002 (2)
C260.0280 (17)0.0311 (18)0.0261 (16)0.0017 (14)0.0049 (14)0.0001 (13)
C270.036 (2)0.062 (3)0.035 (2)0.012 (2)0.0039 (18)0.014 (2)
C310.048 (2)0.040 (2)0.0307 (19)0.0153 (19)0.0169 (18)0.0042 (16)
C320.057 (3)0.056 (3)0.038 (2)0.023 (2)0.029 (2)0.012 (2)
C360.057 (3)0.036 (2)0.0241 (18)0.0062 (19)0.0021 (18)0.0082 (15)
C370.079 (4)0.045 (3)0.043 (3)0.003 (3)0.012 (3)0.014 (2)
C410.0334 (19)0.039 (2)0.0219 (16)0.0104 (15)0.0061 (14)0.0023 (14)
C420.054 (3)0.039 (2)0.0268 (18)0.0122 (19)0.0151 (18)0.0052 (16)
C460.0245 (16)0.0366 (19)0.0244 (16)0.0004 (14)0.0063 (13)0.0091 (14)
C470.0261 (19)0.048 (3)0.046 (2)0.0070 (17)0.0007 (17)0.011 (2)
C510.0306 (17)0.0242 (15)0.0230 (15)0.0002 (13)0.0049 (13)0.0017 (12)
C520.049 (3)0.030 (2)0.051 (3)0.0029 (18)0.021 (2)0.0084 (18)
C560.0275 (16)0.0227 (15)0.0204 (14)0.0010 (12)0.0017 (12)0.0005 (11)
C570.0284 (17)0.041 (2)0.0244 (17)0.0059 (15)0.0017 (14)0.0084 (15)
C610.0260 (16)0.0231 (15)0.0336 (18)0.0057 (12)0.0069 (14)0.0023 (13)
C620.035 (2)0.038 (2)0.051 (3)0.0161 (18)0.0104 (19)0.0024 (19)
C660.0251 (16)0.0284 (17)0.0301 (17)0.0042 (13)0.0056 (13)0.0072 (13)
C670.063 (3)0.039 (2)0.042 (3)0.003 (2)0.012 (2)0.012 (2)
C710.0283 (18)0.058 (3)0.0250 (17)0.0134 (18)0.0087 (14)0.0006 (17)
C720.050 (3)0.083 (4)0.033 (2)0.025 (3)0.021 (2)0.002 (2)
C760.0231 (16)0.041 (2)0.0253 (16)0.0029 (14)0.0056 (13)0.0001 (14)
C770.0220 (17)0.049 (3)0.050 (3)0.0013 (17)0.0003 (17)0.001 (2)
C810.0274 (18)0.045 (2)0.0302 (18)0.0038 (16)0.0069 (15)0.0043 (16)
C820.034 (2)0.056 (3)0.041 (2)0.0109 (19)0.0133 (18)0.009 (2)
C860.0248 (16)0.0371 (19)0.0230 (15)0.0017 (14)0.0063 (13)0.0026 (14)
C870.039 (2)0.051 (3)0.035 (2)0.0108 (19)0.0019 (18)0.0066 (19)
Geometric parameters (Å, º) top
Cr1—F81.946 (2)C49—H49A0.9800
Cr1—O841.957 (3)C49—H49B0.9800
Cr1—O111.960 (3)C49—H49C0.9800
Cr1—F11.961 (3)C50—H50A0.9800
Cr1—O821.965 (3)C50—H50B0.9800
Cr1—O131.978 (3)C50—H50C0.9800
Cr2—F11.922 (2)C51—C521.515 (5)
Cr2—F21.948 (2)C52—C551.511 (3)
Cr2—O121.952 (3)C52—C541.516 (3)
Cr2—O141.957 (3)C52—C531.525 (3)
Cr2—O211.972 (3)C53—H53A0.9800
Cr2—O231.979 (3)C53—H53B0.9800
Cr3—F21.921 (3)C53—H53C0.9800
Cr3—F31.925 (2)C54—H54A0.9800
Cr3—O311.946 (3)C54—H54B0.9800
Cr3—O221.948 (3)C54—H54C0.9800
Cr3—O241.950 (3)C55—H55A0.9800
Cr3—O331.958 (3)C55—H55B0.9800
Cr4—F41.925 (2)C55—H55C0.9800
Cr4—F31.927 (2)C56—C571.517 (5)
Cr4—O411.950 (3)C57—C581.513 (3)
Cr4—O321.953 (3)C57—C59B1.515 (3)
Cr4—O341.954 (4)C57—C60B1.519 (3)
Cr4—O431.959 (3)C57—C591.521 (3)
Cr5—F51.916 (2)C57—C601.526 (3)
Cr5—F41.922 (2)C57—C58B1.528 (3)
Cr5—O511.937 (3)C58—H58A0.9800
Cr5—O421.956 (3)C58—H58B0.9800
Cr5—O441.958 (3)C58—H58C0.9800
Cr5—O531.961 (3)C59—H59A0.9800
Cr6—F61.931 (2)C59—H59B0.9800
Cr6—F51.941 (2)C59—H59C0.9800
Cr6—O611.947 (3)C60—H60A0.9800
Cr6—O631.962 (3)C60—H60B0.9800
Cr6—O541.971 (3)C60—H60C0.9800
Cr6—O521.971 (3)C58B—H58D0.9800
Cr7—F71.930 (2)C58B—H58E0.9800
Cr7—O711.938 (3)C58B—H58F0.9800
Cr7—F61.953 (2)C59B—H59D0.9800
Cr7—O731.959 (3)C59B—H59E0.9800
Cr7—O621.960 (3)C59B—H59F0.9800
Cr7—O641.968 (3)C60B—H60D0.9800
Cr8—F81.945 (3)C60B—H60E0.9800
Cr8—F71.952 (3)C60B—H60F0.9800
Cr8—O811.962 (3)C61—C621.520 (5)
Cr8—O831.971 (3)C62—C631.515 (3)
Cr8—O721.972 (3)C62—C651.518 (3)
Cr8—O741.979 (3)C62—C641.519 (3)
O11—C111.238 (6)C63—H63A0.9800
O12—C111.262 (6)C63—H63B0.9800
O13—C161.264 (6)C63—H63C0.9800
O14—C161.263 (6)C64—H64A0.9800
O21—C211.249 (6)C64—H64B0.9800
O22—C211.264 (6)C64—H64C0.9800
O23—C261.257 (5)C65—H65A0.9800
O24—C261.270 (5)C65—H65B0.9800
O31—C311.256 (5)C65—H65C0.9800
O32—C311.258 (5)C66—C671.532 (5)
O33—C361.269 (5)C67—C691.514 (3)
O34—C361.244 (6)C67—C69B1.517 (3)
O41—C411.262 (5)C67—C681.521 (3)
O42—C411.245 (5)C67—C70B1.521 (3)
O43—C461.257 (5)C67—C68B1.525 (3)
O44—C461.258 (5)C67—C701.532 (3)
O51—C511.266 (5)C68—H68A0.9800
O52—C511.260 (5)C68—H68B0.9800
O53—C561.263 (5)C68—H68C0.9800
O54—C561.263 (5)C69—H69A0.9800
O61—C611.264 (5)C69—H69B0.9800
O62—C611.251 (5)C69—H69C0.9800
O63—C661.262 (5)C70—H70A0.9800
O64—C661.255 (5)C70—H70B0.9800
O71—C711.250 (6)C70—H70C0.9800
O72—C711.267 (6)C68B—H68D0.9800
O73—C761.252 (5)C68B—H68E0.9800
O74—C761.263 (5)C68B—H68F0.9800
O81—C811.261 (6)C69B—H69D0.9800
O82—C811.261 (5)C69B—H69E0.9800
O83—C861.264 (5)C69B—H69F0.9800
O84—C861.259 (5)C70B—H70D0.9800
C11—C121.519 (6)C70B—H70E0.9800
C12—C151.507 (3)C70B—H70F0.9800
C12—C14B1.516 (3)C71—C721.536 (6)
C12—C141.521 (3)C72—C741.512 (3)
C12—C131.522 (3)C72—C731.518 (3)
C12—C13B1.526 (3)C72—C751.522 (3)
C12—C15B1.529 (3)C73—H73A0.9800
C13—H13A0.9800C73—H73B0.9800
C13—H13B0.9800C73—H73C0.9800
C13—H13C0.9800C74—H74A0.9800
C14—H14A0.9800C74—H74B0.9800
C14—H14B0.9800C74—H74C0.9800
C14—H14C0.9800C75—H75A0.9800
C15—H15A0.9800C75—H75B0.9800
C15—H15B0.9800C75—H75C0.9800
C15—H15C0.9800C76—C771.517 (5)
C13B—H13D0.9800C77—C781.518 (3)
C13B—H13E0.9800C77—C791.518 (3)
C13B—H13F0.9800C77—C801.518 (3)
C14B—H14D0.9800C78—H78A0.9800
C14B—H14E0.9800C78—H78B0.9800
C14B—H14F0.9800C78—H78C0.9800
C15B—H15D0.9800C79—H79A0.9800
C15B—H15E0.9800C79—H79B0.9800
C15B—H15F0.9800C79—H79C0.9800
C16—C171.534 (6)C80—H80A0.9800
C17—C201.511 (3)C80—H80B0.9800
C17—C19A1.517 (3)C80—H80C0.9800
C17—C18A1.522 (3)C81—C821.515 (6)
C17—C191.526 (3)C82—C841.515 (3)
C17—C20A1.530 (3)C82—C831.518 (3)
C17—C181.534 (3)C82—C851.517 (3)
C18—H18A0.9800C83—H83A0.9800
C18—H18B0.9800C83—H83B0.9800
C18—H18C0.9800C83—H83C0.9800
C19—H19A0.9800C84—H84A0.9800
C19—H19B0.9800C84—H84B0.9800
C19—H19C0.9800C84—H84C0.9800
C20—H20A0.9800C85—H85A0.9800
C20—H20B0.9800C85—H85B0.9800
C20—H20C0.9800C85—H85C0.9800
C18A—H18D0.9800C86—C871.521 (5)
C18A—H18E0.9800C87—C891.510 (3)
C18A—H18F0.9800C87—C88B1.519 (3)
C19A—H19D0.9800C87—C901.520 (3)
C19A—H19E0.9800C87—C881.524 (3)
C19A—H19F0.9800C87—C90B1.527 (3)
C20A—H20D0.9800C87—C89B1.528 (3)
C20A—H20E0.9800C88—H88A0.9800
C20A—H20F0.9800C88—H88B0.9800
C21—C221.512 (6)C88—H88C0.9800
C22—C251.517 (3)C89—H89A0.9800
C22—C241.517 (3)C89—H89B0.9800
C22—C231.524 (3)C89—H89C0.9800
C23—H23A0.9800C90—H90A0.9800
C23—H23B0.9800C90—H90B0.9800
C23—H23C0.9800C90—H90C0.9800
C24—H24A0.9800C88B—H88D0.9800
C24—H24B0.9800C88B—H88E0.9800
C24—H24C0.9800C88B—H88F0.9800
C25—H25A0.9800C89B—H89D0.9800
C25—H25B0.9800C89B—H89E0.9800
C25—H25C0.9800C89B—H89F0.9800
C26—C271.517 (5)C90B—H90D0.9800
C27—C301.516 (3)C90B—H90E0.9800
C27—C281.520 (3)C90B—H90F0.9800
C27—C291.525 (3)O2A—C2A1.334 (6)
C28—H28A0.9800C2A—C1A1.65 (2)
C28—H28B0.9800C2A—H2A10.9900
C28—H28C0.9800C2A—H2A20.9900
C29—H29A0.9800C1A—N11.372 (18)
C29—H29B0.9800C1A—H1A10.9900
C29—H29C0.9800C1A—H1A20.9900
C30—H30A0.9800N1—C1B1.401 (19)
C30—H30B0.9800N1—H1A0.9200
C30—H30C0.9800N1—H1B0.9200
C31—C321.516 (6)C1B—C2B1.410 (19)
C32—C331.517 (3)C1B—H1B10.9900
C32—C341.517 (3)C1B—H1B20.9900
C32—C351.520 (3)C2B—O2B1.333 (6)
C33—H33A0.9800C2B—H2B10.9900
C33—H33B0.9800C2B—H2B20.9900
C33—H33C0.9800O2C—C2C1.334 (6)
C34—H34A0.9800C2C—C1C1.49 (3)
C34—H34B0.9800C2C—H2C10.9900
C34—H34C0.9800C2C—H2C20.9900
C35—H35A0.9800C1C—N1C1.47 (4)
C35—H35B0.9800C1C—H1C10.9900
C35—H35C0.9800C1C—H1C20.9900
C36—C371.520 (6)N1C—C1D1.31 (3)
C37—C391.518 (3)N1C—H1C30.9200
C37—C401.519 (3)N1C—H1C40.9200
C37—C381.523 (3)C1D—C2D1.42 (3)
C38—H38A0.9800C1D—H1D10.9900
C38—H38B0.9800C1D—H1D20.9900
C38—H38C0.9800C2D—O2D1.335 (6)
C39—H39A0.9800C2D—H2D10.9900
C39—H39B0.9800C2D—H2D20.9900
C39—H39C0.9800O2E—C2E1.334 (6)
C40—H40A0.9800C2E—C1E1.30 (3)
C40—H40B0.9800C2E—H2E10.9900
C40—H40C0.9800C2E—H2E20.9900
C41—C421.529 (5)C1E—N1E1.32 (4)
C42—C431.517 (3)C1E—H1E10.9900
C42—C451.517 (3)C1E—H1E20.9900
C42—C441.519 (3)N1E—C1F1.48 (3)
C43—H43A0.9800N1E—H1E30.9200
C43—H43B0.9800N1E—H1E40.9200
C43—H43C0.9800C1F—C2F1.42 (3)
C44—H44A0.9800C1F—H1F10.9900
C44—H44B0.9800C1F—H1F20.9900
C44—H44C0.9800C2F—O2F1.335 (6)
C45—H45A0.9800C2F—H2F10.9900
C45—H45B0.9800C2F—H2F20.9900
C45—H45C0.9800O99—O99i1.515 (19)
C46—C471.518 (5)O99—C991.53 (2)
C47—C491.515 (3)C99—O981.05 (3)
C47—C481.517 (3)C99—C981.497 (16)
C47—C501.521 (3)C98—H98A0.9800
C48—H48A0.9800C98—H98B0.9800
C48—H48B0.9800C98—H98C0.9800
C48—H48C0.9800
F8—Cr1—O8490.89 (12)H48B—C48—H48C109.5
F8—Cr1—O11178.32 (13)C47—C49—H49A109.5
O84—Cr1—O1187.90 (14)C47—C49—H49B109.5
F8—Cr1—F188.13 (11)H49A—C49—H49B109.5
O84—Cr1—F189.34 (12)C47—C49—H49C109.5
O11—Cr1—F190.69 (13)H49A—C49—H49C109.5
F8—Cr1—O8292.85 (12)H49B—C49—H49C109.5
O84—Cr1—O8292.44 (15)C47—C50—H50A109.5
O11—Cr1—O8288.37 (14)C47—C50—H50B109.5
F1—Cr1—O82177.95 (13)H50A—C50—H50B109.5
F8—Cr1—O1388.46 (12)C47—C50—H50C109.5
O84—Cr1—O13178.86 (14)H50A—C50—H50C109.5
O11—Cr1—O1392.77 (14)H50B—C50—H50C109.5
F1—Cr1—O1391.57 (13)O52—C51—O51125.1 (3)
O82—Cr1—O1386.67 (15)O52—C51—C52118.4 (3)
F1—Cr2—F287.65 (11)O51—C51—C52116.4 (3)
F1—Cr2—O1293.44 (13)C55—C52—C51110.5 (4)
F2—Cr2—O12178.61 (12)C55—C52—C54110.7 (3)
F1—Cr2—O1491.33 (12)C51—C52—C54111.3 (4)
F2—Cr2—O1487.62 (13)C55—C52—C53109.7 (3)
O12—Cr2—O1493.21 (15)C51—C52—C53105.6 (4)
F1—Cr2—O21178.68 (13)C54—C52—C53108.9 (2)
F2—Cr2—O2191.09 (12)C52—C53—H53A109.5
O12—Cr2—O2187.81 (14)C52—C53—H53B109.5
O14—Cr2—O2189.02 (14)H53A—C53—H53B109.5
F1—Cr2—O2390.78 (11)C52—C53—H53C109.5
F2—Cr2—O2391.81 (11)H53A—C53—H53C109.5
O12—Cr2—O2387.31 (13)H53B—C53—H53C109.5
O14—Cr2—O23177.78 (14)C52—C54—H54A109.5
O21—Cr2—O2388.85 (13)C52—C54—H54B109.5
F2—Cr3—F389.30 (10)H54A—C54—H54B109.5
F2—Cr3—O31178.45 (13)C52—C54—H54C109.5
F3—Cr3—O3190.64 (12)H54A—C54—H54C109.5
F2—Cr3—O2293.12 (12)H54B—C54—H54C109.5
F3—Cr3—O22177.58 (13)C52—C55—H55A109.5
O31—Cr3—O2286.94 (14)C52—C55—H55B109.5
F2—Cr3—O2490.64 (12)H55A—C55—H55B109.5
F3—Cr3—O2489.68 (11)C52—C55—H55C109.5
O31—Cr3—O2487.81 (14)H55A—C55—H55C109.5
O22—Cr3—O2490.26 (13)H55B—C55—H55C109.5
F2—Cr3—O3389.34 (13)O54—C56—O53125.5 (3)
F3—Cr3—O3391.03 (11)O54—C56—C57117.2 (3)
O31—Cr3—O3392.21 (15)O53—C56—C57117.3 (3)
O22—Cr3—O3389.03 (13)C58—C57—C59B133.7 (7)
O24—Cr3—O33179.29 (14)C58—C57—C56110.4 (4)
F4—Cr4—F387.95 (10)C59B—C57—C56115.0 (6)
F4—Cr4—O4191.05 (12)C58—C57—C60B56.7 (5)
F3—Cr4—O41178.99 (13)C59B—C57—C60B110.0 (3)
F4—Cr4—O32178.23 (14)C56—C57—C60B113.4 (6)
F3—Cr4—O3293.05 (12)C58—C57—C59109.9 (3)
O41—Cr4—O3287.95 (13)C59B—C57—C5943.9 (5)
F4—Cr4—O3489.47 (13)C56—C57—C59111.9 (4)
F3—Cr4—O3490.00 (12)C60B—C57—C59134.5 (7)
O41—Cr4—O3490.15 (15)C58—C57—C60109.5 (3)
O32—Cr4—O3491.99 (16)C59B—C57—C6066.1 (5)
F4—Cr4—O4391.49 (11)C56—C57—C60106.1 (5)
F3—Cr4—O4388.01 (11)C60B—C57—C6053.9 (5)
O41—Cr4—O4391.86 (14)C59—C57—C60108.9 (3)
O32—Cr4—O4387.08 (15)C58—C57—C58B53.0 (5)
O34—Cr4—O43177.75 (13)C59B—C57—C58B109.2 (3)
F5—Cr5—F489.26 (10)C56—C57—C58B99.7 (6)
F5—Cr5—O5191.36 (11)C60B—C57—C58B108.9 (3)
F4—Cr5—O51178.91 (12)C59—C57—C58B66.7 (5)
F5—Cr5—O42178.42 (11)C60—C57—C58B153.2 (7)
F4—Cr5—O4292.32 (11)C57—C58—H58A109.5
O51—Cr5—O4287.07 (12)C57—C58—H58B109.5
F5—Cr5—O4488.23 (11)H58A—C58—H58B109.5
F4—Cr5—O4490.22 (12)C57—C58—H58C109.5
O51—Cr5—O4488.91 (12)H58A—C58—H58C109.5
O42—Cr5—O4491.86 (12)H58B—C58—H58C109.5
F5—Cr5—O5392.05 (10)C57—C59—H59A109.5
F4—Cr5—O5389.34 (11)C57—C59—H59B109.5
O51—Cr5—O5391.53 (12)H59A—C59—H59B109.5
O42—Cr5—O5387.87 (11)C57—C59—H59C109.5
O44—Cr5—O53179.47 (13)H59A—C59—H59C109.5
F6—Cr6—F586.63 (10)H59B—C59—H59C109.5
F6—Cr6—O6190.81 (11)C57—C60—H60A109.5
F5—Cr6—O61177.00 (12)C57—C60—H60B109.5
F6—Cr6—O6392.48 (11)H60A—C60—H60B109.5
F5—Cr6—O6389.21 (10)C57—C60—H60C109.5
O61—Cr6—O6392.47 (12)H60A—C60—H60C109.5
F6—Cr6—O5490.03 (11)H60B—C60—H60C109.5
F5—Cr6—O5489.48 (11)C57—C58B—H58D109.5
O61—Cr6—O5488.95 (12)C57—C58B—H58E109.5
O63—Cr6—O54177.09 (13)H58D—C58B—H58E109.5
F6—Cr6—O52179.75 (13)C57—C58B—H58F109.5
F5—Cr6—O5293.41 (11)H58D—C58B—H58F109.5
O61—Cr6—O5289.15 (12)H58E—C58B—H58F109.5
O63—Cr6—O5287.28 (12)C57—C59B—H59D109.5
O54—Cr6—O5290.21 (12)C57—C59B—H59E109.5
F7—Cr7—O7191.22 (12)H59D—C59B—H59E109.5
F7—Cr7—F688.42 (10)C57—C59B—H59F109.5
O71—Cr7—F6178.33 (12)H59D—C59B—H59F109.5
F7—Cr7—O7392.68 (12)H59E—C59B—H59F109.5
O71—Cr7—O7392.56 (13)C57—C60B—H60D109.5
F6—Cr7—O7389.08 (11)C57—C60B—H60E109.5
F7—Cr7—O62179.01 (12)H60D—C60B—H60E109.5
O71—Cr7—O6288.31 (13)C57—C60B—H60F109.5
F6—Cr7—O6292.07 (11)H60D—C60B—H60F109.5
O73—Cr7—O6286.46 (12)H60E—C60B—H60F109.5
F7—Cr7—O6489.08 (12)O62—C61—O61125.5 (3)
O71—Cr7—O6488.42 (13)O62—C61—C62117.2 (3)
F6—Cr7—O6489.94 (11)O61—C61—C62117.3 (3)
O73—Cr7—O64177.96 (13)C63—C62—C65109.9 (3)
O62—Cr7—O6491.79 (13)C63—C62—C64109.9 (2)
F8—Cr8—F786.30 (10)C65—C62—C64109.8 (3)
F8—Cr8—O8191.31 (13)C63—C62—C61109.8 (4)
F7—Cr8—O81176.36 (13)C65—C62—C61105.3 (4)
F8—Cr8—O8393.02 (11)C64—C62—C61112.1 (4)
F7—Cr8—O8389.89 (11)C62—C63—H63A109.5
O81—Cr8—O8392.97 (13)C62—C63—H63B109.5
F8—Cr8—O72179.48 (13)H63A—C63—H63B109.5
F7—Cr8—O7293.22 (12)C62—C63—H63C109.5
O81—Cr8—O7289.18 (15)H63A—C63—H63C109.5
O83—Cr8—O7286.77 (13)H63B—C63—H63C109.5
F8—Cr8—O7488.01 (13)C62—C64—H64A109.5
F7—Cr8—O7489.88 (13)C62—C64—H64B109.5
O81—Cr8—O7487.29 (14)H64A—C64—H64B109.5
O83—Cr8—O74178.93 (15)C62—C64—H64C109.5
O72—Cr8—O7492.20 (14)H64A—C64—H64C109.5
Cr2—F1—Cr1121.73 (12)H64B—C64—H64C109.5
Cr3—F2—Cr2122.83 (12)C62—C65—H65A109.5
Cr3—F3—Cr4123.65 (12)C62—C65—H65B109.5
Cr5—F4—Cr4123.17 (13)H65A—C65—H65B109.5
Cr5—F5—Cr6122.62 (11)C62—C65—H65C109.5
Cr6—F6—Cr7121.72 (11)H65A—C65—H65C109.5
Cr7—F7—Cr8121.34 (12)H65B—C65—H65C109.5
Cr1—F8—Cr8121.33 (12)O64—C66—O63125.6 (4)
C11—O11—Cr1131.0 (3)O64—C66—C67119.6 (4)
C11—O12—Cr2133.8 (3)O63—C66—C67114.8 (4)
C16—O13—Cr1135.0 (3)C69—C67—C69B118.4 (9)
C16—O14—Cr2129.3 (3)C69—C67—C68110.1 (3)
C21—O21—Cr2128.6 (3)C69B—C67—C6862.6 (9)
C21—O22—Cr3135.5 (3)C69—C67—C70B28.2 (7)
C26—O23—Cr2135.6 (3)C69B—C67—C70B109.7 (3)
C26—O24—Cr3126.8 (3)C68—C67—C70B132.7 (8)
C31—O31—Cr3132.1 (3)C69—C67—C68B80.8 (7)
C31—O32—Cr4133.8 (3)C69B—C67—C68B109.4 (3)
C36—O33—Cr3135.0 (3)C68—C67—C68B47.6 (9)
C36—O34—Cr4130.6 (3)C70B—C67—C68B108.9 (3)
C41—O41—Cr4129.9 (3)C69—C67—C70109.1 (3)
C41—O42—Cr5135.4 (3)C69B—C67—C7046.2 (10)
C46—O43—Cr4134.6 (3)C68—C67—C70108.3 (3)
C46—O44—Cr5130.1 (3)C70B—C67—C7084.1 (7)
C51—O51—Cr5129.6 (3)C68B—C67—C70155.5 (10)
C51—O52—Cr6133.9 (3)C69—C67—C66112.8 (5)
C56—O53—Cr5135.1 (2)C69B—C67—C66127.4 (10)
C56—O54—Cr6128.5 (2)C68—C67—C66109.9 (5)
C61—O61—Cr6129.0 (3)C70B—C67—C66109.6 (7)
C61—O62—Cr7134.0 (3)C68B—C67—C6689.1 (11)
C66—O63—Cr6135.1 (3)C70—C67—C66106.3 (5)
C66—O64—Cr7128.3 (3)C67—C68—H68A109.5
C71—O71—Cr7130.3 (3)C67—C68—H68B109.5
C71—O72—Cr8132.8 (3)H68A—C68—H68B109.5
C76—O73—Cr7135.3 (3)C67—C68—H68C109.5
C76—O74—Cr8128.3 (3)H68A—C68—H68C109.5
C81—O81—Cr8130.2 (3)H68B—C68—H68C109.5
C81—O82—Cr1133.3 (3)C67—C69—H69A109.5
C86—O83—Cr8134.6 (3)C67—C69—H69B109.5
C86—O84—Cr1130.3 (3)H69A—C69—H69B109.5
O11—C11—O12126.0 (4)C67—C69—H69C109.5
O11—C11—C12117.5 (4)H69A—C69—H69C109.5
O12—C11—C12116.4 (4)H69B—C69—H69C109.5
C15—C12—C14B129.1 (8)C67—C70—H70A109.5
C15—C12—C11113.9 (6)C67—C70—H70B109.5
C14B—C12—C11117.0 (7)H70A—C70—H70B109.5
C15—C12—C14110.4 (3)C67—C70—H70C109.5
C14B—C12—C1454.6 (6)H70A—C70—H70C109.5
C11—C12—C14103.4 (6)H70B—C70—H70C109.5
C15—C12—C13110.3 (3)C67—C68B—H68D109.5
C14B—C12—C1354.6 (6)C67—C68B—H68E109.5
C11—C12—C13109.6 (6)H68D—C68B—H68E109.5
C14—C12—C13109.1 (3)C67—C68B—H68F109.5
C15—C12—C13B58.3 (7)H68D—C68B—H68F109.5
C14B—C12—C13B109.4 (3)H68E—C68B—H68F109.5
C11—C12—C13B105.4 (8)C67—C69B—H69D109.5
C14—C12—C13B151.2 (8)C67—C69B—H69E109.5
C13—C12—C13B59.3 (6)H69D—C69B—H69E109.5
C15—C12—C15B50.4 (7)C67—C69B—H69F109.5
C14B—C12—C15B109.1 (3)H69D—C69B—H69F109.5
C11—C12—C15B107.3 (8)H69E—C69B—H69F109.5
C14—C12—C15B63.5 (6)C67—C70B—H70D109.5
C13—C12—C15B143.0 (8)C67—C70B—H70E109.5
C13B—C12—C15B108.4 (3)H70D—C70B—H70E109.5
C12—C13—H13A109.5C67—C70B—H70F109.5
C12—C13—H13B109.5H70D—C70B—H70F109.5
H13A—C13—H13B109.5H70E—C70B—H70F109.5
C12—C13—H13C109.5O71—C71—O72125.9 (4)
H13A—C13—H13C109.5O71—C71—C72113.9 (4)
H13B—C13—H13C109.5O72—C71—C72120.2 (4)
C12—C14—H14A109.5C74—C72—C73110.1 (3)
C12—C14—H14B109.5C74—C72—C75109.8 (3)
H14A—C14—H14B109.5C73—C72—C75109.2 (3)
C12—C14—H14C109.5C74—C72—C71110.7 (5)
H14A—C14—H14C109.5C73—C72—C71110.1 (4)
H14B—C14—H14C109.5C75—C72—C71106.9 (4)
C12—C15—H15A109.5C72—C73—H73A109.5
C12—C15—H15B109.5C72—C73—H73B109.5
H15A—C15—H15B109.5H73A—C73—H73B109.5
C12—C15—H15C109.5C72—C73—H73C109.5
H15A—C15—H15C109.5H73A—C73—H73C109.5
H15B—C15—H15C109.5H73B—C73—H73C109.5
C12—C13B—H13D109.5C72—C74—H74A109.5
C12—C13B—H13E109.5C72—C74—H74B109.5
H13D—C13B—H13E109.5H74A—C74—H74B109.5
C12—C13B—H13F109.5C72—C74—H74C109.5
H13D—C13B—H13F109.5H74A—C74—H74C109.5
H13E—C13B—H13F109.5H74B—C74—H74C109.5
C12—C14B—H14D109.5C72—C75—H75A109.5
C12—C14B—H14E109.5C72—C75—H75B109.5
H14D—C14B—H14E109.5H75A—C75—H75B109.5
C12—C14B—H14F109.5C72—C75—H75C109.5
H14D—C14B—H14F109.5H75A—C75—H75C109.5
H14E—C14B—H14F109.5H75B—C75—H75C109.5
C12—C15B—H15D109.5O73—C76—O74125.6 (4)
C12—C15B—H15E109.5O73—C76—C77116.9 (3)
H15D—C15B—H15E109.5O74—C76—C77117.4 (4)
C12—C15B—H15F109.5C78—C77—C79109.9 (2)
H15D—C15B—H15F109.5C78—C77—C80109.9 (2)
H15E—C15B—H15F109.5C79—C77—C80109.7 (2)
O14—C16—O13126.1 (4)C78—C77—C76106.8 (4)
O14—C16—C17119.4 (4)C79—C77—C76108.4 (4)
O13—C16—C17114.4 (4)C80—C77—C76112.1 (3)
C20—C17—C19A119.4 (11)C77—C78—H78A109.5
C20—C17—C18A65.1 (7)C77—C78—H78B109.5
C19A—C17—C18A109.6 (3)H78A—C78—H78B109.5
C20—C17—C19109.9 (3)C77—C78—H78C109.5
C19A—C17—C1944.1 (7)H78A—C78—H78C109.5
C18A—C17—C19149.4 (9)H78B—C78—H78C109.5
C20—C17—C20A43.5 (7)C77—C79—H79A109.5
C19A—C17—C20A109.1 (3)C77—C79—H79B109.5
C18A—C17—C20A108.4 (3)H79A—C79—H79B109.5
C19—C17—C20A75.4 (7)C77—C79—H79C109.5
C20—C17—C18109.3 (3)H79A—C79—H79C109.5
C19A—C17—C1864.0 (7)H79B—C79—H79C109.5
C18A—C17—C1852.4 (7)C77—C80—H80A109.5
C19—C17—C18107.8 (3)C77—C80—H80B109.5
C20A—C17—C18147.2 (8)H80A—C80—H80B109.5
C20—C17—C16114.7 (7)C77—C80—H80C109.5
C19A—C17—C16124.6 (10)H80A—C80—H80C109.5
C18A—C17—C16102.5 (8)H80B—C80—H80C109.5
C19—C17—C16106.5 (5)O81—C81—O82125.7 (4)
C20A—C17—C16101.5 (8)O81—C81—C82116.2 (4)
C18—C17—C16108.4 (6)O82—C81—C82118.1 (4)
C17—C18—H18A109.5C84—C82—C81110.4 (4)
C17—C18—H18B109.5C84—C82—C83110.0 (2)
H18A—C18—H18B109.5C81—C82—C83107.6 (3)
C17—C18—H18C109.5C84—C82—C85110.1 (2)
H18A—C18—H18C109.5C81—C82—C85108.7 (4)
H18B—C18—H18C109.5C83—C82—C85110.0 (2)
C17—C19—H19A109.5C82—C83—H83A109.5
C17—C19—H19B109.5C82—C83—H83B109.5
H19A—C19—H19B109.5H83A—C83—H83B109.5
C17—C19—H19C109.5C82—C83—H83C109.5
H19A—C19—H19C109.5H83A—C83—H83C109.5
H19B—C19—H19C109.5H83B—C83—H83C109.5
C17—C20—H20A109.5C82—C84—H84A109.5
C17—C20—H20B109.5C82—C84—H84B109.5
H20A—C20—H20B109.5H84A—C84—H84B109.5
C17—C20—H20C109.5C82—C84—H84C109.5
H20A—C20—H20C109.5H84A—C84—H84C109.5
H20B—C20—H20C109.5H84B—C84—H84C109.5
C17—C18A—H18D109.5C82—C85—H85A109.5
C17—C18A—H18E109.5C82—C85—H85B109.5
H18D—C18A—H18E109.5H85A—C85—H85B109.5
C17—C18A—H18F109.5C82—C85—H85C109.5
H18D—C18A—H18F109.5H85A—C85—H85C109.5
H18E—C18A—H18F109.5H85B—C85—H85C109.5
C17—C19A—H19D109.5O84—C86—O83125.7 (4)
C17—C19A—H19E109.5O84—C86—C87117.3 (3)
H19D—C19A—H19E109.5O83—C86—C87117.0 (4)
C17—C19A—H19F109.5C89—C87—C88B123.3 (8)
H19D—C19A—H19F109.5C89—C87—C90110.3 (3)
H19E—C19A—H19F109.5C88B—C87—C9070.9 (6)
C17—C20A—H20D109.5C89—C87—C86114.1 (5)
C17—C20A—H20E109.5C88B—C87—C86119.7 (7)
H20D—C20A—H20E109.5C90—C87—C86106.3 (5)
C17—C20A—H20F109.5C89—C87—C88109.9 (3)
H20D—C20A—H20F109.5C88B—C87—C8838.1 (6)
H20E—C20A—H20F109.5C90—C87—C88109.0 (3)
O21—C21—O22126.0 (4)C86—C87—C88107.1 (5)
O21—C21—C22119.0 (4)C89—C87—C90B73.1 (5)
O22—C21—C22115.0 (4)C88B—C87—C90B109.1 (3)
C21—C22—C25107.6 (4)C90—C87—C90B43.1 (5)
C21—C22—C24111.1 (4)C86—C87—C90B103.4 (7)
C25—C22—C24110.0 (3)C88—C87—C90B144.2 (7)
C21—C22—C23109.4 (4)C89—C87—C89B35.2 (5)
C25—C22—C23109.4 (3)C88B—C87—C89B109.0 (3)
C24—C22—C23109.3 (3)C90—C87—C89B140.8 (7)
C22—C23—H23A109.5C86—C87—C89B106.8 (6)
C22—C23—H23B109.5C88—C87—C89B80.4 (6)
H23A—C23—H23B109.5C90B—C87—C89B108.3 (3)
C22—C23—H23C109.5C87—C88—H88A109.5
H23A—C23—H23C109.5C87—C88—H88B109.5
H23B—C23—H23C109.5H88A—C88—H88B109.5
C22—C24—H24A109.5C87—C88—H88C109.5
C22—C24—H24B109.5H88A—C88—H88C109.5
H24A—C24—H24B109.5H88B—C88—H88C109.5
C22—C24—H24C109.5C87—C89—H89A109.5
H24A—C24—H24C109.5C87—C89—H89B109.5
H24B—C24—H24C109.5H89A—C89—H89B109.5
C22—C25—H25A109.5C87—C89—H89C109.5
C22—C25—H25B109.5H89A—C89—H89C109.5
H25A—C25—H25B109.5H89B—C89—H89C109.5
C22—C25—H25C109.5C87—C90—H90A109.5
H25A—C25—H25C109.5C87—C90—H90B109.5
H25B—C25—H25C109.5H90A—C90—H90B109.5
O23—C26—O24125.6 (4)C87—C90—H90C109.5
O23—C26—C27118.6 (3)H90A—C90—H90C109.5
O24—C26—C27115.8 (3)H90B—C90—H90C109.5
C30—C27—C26108.3 (4)C87—C88B—H88D109.5
C30—C27—C28109.8 (3)C87—C88B—H88E109.5
C26—C27—C28111.8 (4)H88D—C88B—H88E109.5
C30—C27—C29109.5 (3)C87—C88B—H88F109.5
C26—C27—C29108.4 (4)H88D—C88B—H88F109.5
C28—C27—C29109.0 (3)H88E—C88B—H88F109.5
C27—C28—H28A109.5C87—C89B—H89D109.5
C27—C28—H28B109.5C87—C89B—H89E109.5
H28A—C28—H28B109.5H89D—C89B—H89E109.5
C27—C28—H28C109.5C87—C89B—H89F109.5
H28A—C28—H28C109.5H89D—C89B—H89F109.5
H28B—C28—H28C109.5H89E—C89B—H89F109.5
C27—C29—H29A109.5C87—C90B—H90D109.5
C27—C29—H29B109.5C87—C90B—H90E109.5
H29A—C29—H29B109.5H90D—C90B—H90E109.5
C27—C29—H29C109.5C87—C90B—H90F109.5
H29A—C29—H29C109.5H90D—C90B—H90F109.5
H29B—C29—H29C109.5H90E—C90B—H90F109.5
C27—C30—H30A109.5O2A—C2A—C1A94.3 (9)
C27—C30—H30B109.5O2A—C2A—H2A1112.9
H30A—C30—H30B109.5C1A—C2A—H2A1112.9
C27—C30—H30C109.5O2A—C2A—H2A2112.9
H30A—C30—H30C109.5C1A—C2A—H2A2112.9
H30B—C30—H30C109.5H2A1—C2A—H2A2110.3
O31—C31—O32125.4 (4)N1—C1A—C2A111.8 (13)
O31—C31—C32117.0 (4)N1—C1A—H1A1109.3
O32—C31—C32117.6 (4)C2A—C1A—H1A1109.3
C31—C32—C33110.8 (4)N1—C1A—H1A2109.3
C31—C32—C34109.9 (4)C2A—C1A—H1A2109.3
C33—C32—C34110.2 (2)H1A1—C1A—H1A2107.9
C31—C32—C35106.5 (4)C1A—N1—C1B129.0 (12)
C33—C32—C35109.6 (3)C1A—N1—H1A105.0
C34—C32—C35109.7 (3)C1B—N1—H1A105.0
C32—C33—H33A109.5C1A—N1—H1B105.0
C32—C33—H33B109.5C1B—N1—H1B105.0
H33A—C33—H33B109.5H1A—N1—H1B105.9
C32—C33—H33C109.5N1—C1B—C2B136.6 (14)
H33A—C33—H33C109.5N1—C1B—H1B1103.0
H33B—C33—H33C109.5C2B—C1B—H1B1103.0
C32—C34—H34A109.5N1—C1B—H1B2103.0
C32—C34—H34B109.5C2B—C1B—H1B2103.0
H34A—C34—H34B109.5H1B1—C1B—H1B2105.1
C32—C34—H34C109.5O2B—C2B—C1B106.1 (11)
H34A—C34—H34C109.5O2B—C2B—H2B1110.5
H34B—C34—H34C109.5C1B—C2B—H2B1110.5
C32—C35—H35A109.5O2B—C2B—H2B2110.5
C32—C35—H35B109.5C1B—C2B—H2B2110.5
H35A—C35—H35B109.5H2B1—C2B—H2B2108.7
C32—C35—H35C109.5O2C—C2C—C1C101.2 (18)
H35A—C35—H35C109.5O2C—C2C—H2C1111.5
H35B—C35—H35C109.5C1C—C2C—H2C1111.5
O34—C36—O33126.1 (4)O2C—C2C—H2C2111.5
O34—C36—C37116.8 (4)C1C—C2C—H2C2111.5
O33—C36—C37117.1 (4)H2C1—C2C—H2C2109.3
C39—C37—C40109.9 (3)C2C—C1C—N1C111 (3)
C39—C37—C36112.6 (6)C2C—C1C—H1C1109.5
C40—C37—C36109.7 (4)N1C—C1C—H1C1109.5
C39—C37—C38109.3 (3)C2C—C1C—H1C2109.5
C40—C37—C38109.4 (3)N1C—C1C—H1C2109.5
C36—C37—C38105.9 (5)H1C1—C1C—H1C2108.1
C37—C38—H38A109.5C1D—N1C—C1C124 (2)
C37—C38—H38B109.5C1D—N1C—H1C3106.4
H38A—C38—H38B109.5C1C—N1C—H1C3106.4
C37—C38—H38C109.5C1D—N1C—H1C4106.4
H38A—C38—H38C109.5C1C—N1C—H1C4106.4
H38B—C38—H38C109.5H1C3—N1C—H1C4106.5
C37—C39—H39A109.5N1C—C1D—C2D147 (3)
C37—C39—H39B109.5N1C—C1D—H1D1100.1
H39A—C39—H39B109.5C2D—C1D—H1D1100.1
C37—C39—H39C109.5N1C—C1D—H1D2100.1
H39A—C39—H39C109.5C2D—C1D—H1D2100.1
H39B—C39—H39C109.5H1D1—C1D—H1D2104.2
C37—C40—H40A109.5O2D—C2D—C1D103.5 (18)
C37—C40—H40B109.5O2D—C2D—H2D1111.1
H40A—C40—H40B109.5C1D—C2D—H2D1111.1
C37—C40—H40C109.5O2D—C2D—H2D2111.1
H40A—C40—H40C109.5C1D—C2D—H2D2111.1
H40B—C40—H40C109.5H2D1—C2D—H2D2109.0
O42—C41—O41125.3 (4)O2E—C2E—C1E111.8 (18)
O42—C41—C42118.1 (3)O2E—C2E—H2E1109.3
O41—C41—C42116.6 (3)C1E—C2E—H2E1109.3
C43—C42—C45110.0 (2)O2E—C2E—H2E2109.3
C43—C42—C44109.6 (2)C1E—C2E—H2E2109.3
C45—C42—C44109.7 (2)H2E1—C2E—H2E2107.9
C43—C42—C41109.2 (3)N1E—C1E—C2E150 (3)
C45—C42—C41106.9 (4)N1E—C1E—H1E199.3
C44—C42—C41111.4 (4)C2E—C1E—H1E199.3
C42—C43—H43A109.5N1E—C1E—H1E299.3
C42—C43—H43B109.5C2E—C1E—H1E299.3
H43A—C43—H43B109.5H1E1—C1E—H1E2104.0
C42—C43—H43C109.5C1E—N1E—C1F131.4 (19)
H43A—C43—H43C109.5C1E—N1E—H1E3104.4
H43B—C43—H43C109.5C1F—N1E—H1E3104.4
C42—C44—H44A109.5C1E—N1E—H1E4104.4
C42—C44—H44B109.5C1F—N1E—H1E4104.4
H44A—C44—H44B109.5H1E3—N1E—H1E4105.6
C42—C44—H44C109.5C2F—C1F—N1E124 (2)
H44A—C44—H44C109.5C2F—C1F—H1F1106.2
H44B—C44—H44C109.5N1E—C1F—H1F1106.2
C42—C45—H45A109.5C2F—C1F—H1F2106.2
C42—C45—H45B109.5N1E—C1F—H1F2106.2
H45A—C45—H45B109.5H1F1—C1F—H1F2106.4
C42—C45—H45C109.5O2F—C2F—C1F102.7 (16)
H45A—C45—H45C109.5O2F—C2F—H2F1111.2
H45B—C45—H45C109.5C1F—C2F—H2F1111.2
O43—C46—O44125.2 (4)O2F—C2F—H2F2111.2
O43—C46—C47117.1 (3)C1F—C2F—H2F2111.2
O44—C46—C47117.7 (4)H2F1—C2F—H2F2109.1
C49—C47—C48110.2 (3)O99i—O99—C99112.0 (14)
C49—C47—C46107.2 (4)O98—C99—C98152 (3)
C48—C47—C46111.5 (4)O98—C99—O99106 (2)
C49—C47—C50109.7 (3)C98—C99—O99102.0 (17)
C48—C47—C50109.4 (2)C99—C98—H98A109.5
C46—C47—C50108.8 (4)C99—C98—H98B109.5
C47—C48—H48A109.5H98A—C98—H98B109.5
C47—C48—H48B109.5C99—C98—H98C109.5
H48A—C48—H48B109.5H98A—C98—H98C109.5
C47—C48—H48C109.5H98B—C98—H98C109.5
H48A—C48—H48C109.5
F2—Cr2—F1—Cr1142.52 (15)O83—Cr8—O81—C8156.9 (4)
O12—Cr2—F1—Cr138.35 (16)O72—Cr8—O81—C81143.7 (4)
O14—Cr2—F1—Cr154.95 (17)O74—Cr8—O81—C81124.1 (4)
O21—Cr2—F1—Cr1160 (6)F8—Cr1—O82—C817.1 (4)
O23—Cr2—F1—Cr1125.70 (15)O84—Cr1—O82—C8198.1 (4)
F8—Cr1—F1—Cr2129.30 (15)O11—Cr1—O82—C81174.1 (4)
O84—Cr1—F1—Cr2139.79 (16)F1—Cr1—O82—C81111 (3)
O11—Cr1—F1—Cr251.89 (17)O13—Cr1—O82—C8181.2 (4)
O82—Cr1—F1—Cr211 (3)F8—Cr8—O83—C861.6 (4)
O13—Cr1—F1—Cr240.90 (16)F7—Cr8—O83—C8687.9 (4)
F3—Cr3—F2—Cr2144.00 (15)O81—Cr8—O83—C8689.8 (4)
O31—Cr3—F2—Cr256 (5)O72—Cr8—O83—C86178.9 (4)
O22—Cr3—F2—Cr235.97 (17)O74—Cr8—O83—C86166 (8)
O24—Cr3—F2—Cr254.32 (16)F8—Cr1—O84—C8643.7 (4)
O33—Cr3—F2—Cr2124.96 (16)O11—Cr1—O84—C86137.5 (4)
F1—Cr2—F2—Cr3128.26 (15)F1—Cr1—O84—C86131.8 (4)
O12—Cr2—F2—Cr313 (6)O82—Cr1—O84—C8649.2 (4)
O14—Cr2—F2—Cr3140.31 (16)O13—Cr1—O84—C8611 (8)
O21—Cr2—F2—Cr351.34 (16)Cr1—O11—C11—O127.0 (7)
O23—Cr2—F2—Cr337.55 (16)Cr1—O11—C11—C12170.9 (3)
F2—Cr3—F3—Cr4131.21 (15)Cr2—O12—C11—O1121.3 (7)
O31—Cr3—F3—Cr450.34 (17)Cr2—O12—C11—C12160.8 (3)
O22—Cr3—F3—Cr450 (3)O11—C11—C12—C1550.2 (6)
O24—Cr3—F3—Cr4138.15 (17)O12—C11—C12—C15131.7 (5)
O33—Cr3—F3—Cr441.88 (18)O11—C11—C12—C14B126.4 (7)
F4—Cr4—F3—Cr3143.88 (16)O12—C11—C12—C14B51.6 (7)
O41—Cr4—F3—Cr3153 (9)O11—C11—C12—C1469.5 (6)
O32—Cr4—F3—Cr337.58 (18)O12—C11—C12—C14108.5 (5)
O34—Cr4—F3—Cr354.41 (17)O11—C11—C12—C13174.2 (5)
O43—Cr4—F3—Cr3124.55 (16)O12—C11—C12—C137.7 (6)
F5—Cr5—F4—Cr4142.77 (14)O11—C11—C12—C13B111.9 (7)
O51—Cr5—F4—Cr418 (6)O12—C11—C12—C13B70.1 (7)
O42—Cr5—F4—Cr437.33 (15)O11—C11—C12—C15B3.5 (7)
O44—Cr5—F4—Cr454.54 (15)O12—C11—C12—C15B174.6 (6)
O53—Cr5—F4—Cr4125.16 (15)Cr2—O14—C16—O1311.2 (7)
F3—Cr4—F4—Cr5127.87 (14)Cr2—O14—C16—C17166.0 (3)
O41—Cr4—F4—Cr551.98 (17)Cr1—O13—C16—O1416.1 (7)
O32—Cr4—F4—Cr54 (4)Cr1—O13—C16—C17166.5 (3)
O34—Cr4—F4—Cr5142.11 (16)O14—C16—C17—C206.8 (7)
O43—Cr4—F4—Cr539.92 (15)O13—C16—C17—C20170.8 (5)
F4—Cr5—F5—Cr6129.51 (14)O14—C16—C17—C19A160.2 (9)
O51—Cr5—F5—Cr651.38 (15)O13—C16—C17—C19A22.2 (10)
O42—Cr5—F5—Cr647 (4)O14—C16—C17—C18A74.9 (8)
O44—Cr5—F5—Cr6140.25 (15)O13—C16—C17—C18A102.7 (8)
O53—Cr5—F5—Cr640.20 (15)O14—C16—C17—C19115.1 (5)
F6—Cr6—F5—Cr5146.17 (14)O13—C16—C17—C1967.3 (6)
O61—Cr6—F5—Cr5115 (2)O14—C16—C17—C20A37.1 (8)
O63—Cr6—F5—Cr5121.30 (15)O13—C16—C17—C20A145.3 (7)
O54—Cr6—F5—Cr556.11 (15)O14—C16—C17—C18129.1 (5)
O52—Cr6—F5—Cr534.07 (15)O13—C16—C17—C1848.5 (6)
F5—Cr6—F6—Cr7127.31 (14)Cr2—O21—C21—O2218.2 (7)
O61—Cr6—F6—Cr754.26 (15)Cr2—O21—C21—C22162.8 (3)
O63—Cr6—F6—Cr738.25 (15)Cr3—O22—C21—O2112.7 (8)
O54—Cr6—F6—Cr7143.21 (15)Cr3—O22—C21—C22166.4 (3)
O52—Cr6—F6—Cr726 (25)O21—C21—C22—C25118.0 (4)
F7—Cr7—F6—Cr6144.23 (14)O22—C21—C22—C2562.8 (5)
O71—Cr7—F6—Cr667 (4)O21—C21—C22—C242.6 (6)
O73—Cr7—F6—Cr6123.06 (15)O22—C21—C22—C24176.6 (4)
O62—Cr7—F6—Cr636.63 (15)O21—C21—C22—C23123.3 (4)
O64—Cr7—F6—Cr655.15 (15)O22—C21—C22—C2355.8 (5)
O71—Cr7—F7—Cr853.04 (17)Cr2—O23—C26—O241.5 (7)
F6—Cr7—F7—Cr8128.59 (15)Cr2—O23—C26—C27179.6 (3)
O73—Cr7—F7—Cr839.58 (16)Cr3—O24—C26—O2330.2 (6)
O62—Cr7—F7—Cr89 (7)Cr3—O24—C26—C27148.0 (3)
O64—Cr7—F7—Cr8141.44 (15)O23—C26—C27—C30115.8 (4)
F8—Cr8—F7—Cr7143.50 (15)O24—C26—C27—C3065.9 (4)
O81—Cr8—F7—Cr794.5 (18)O23—C26—C27—C285.3 (5)
O83—Cr8—F7—Cr7123.46 (16)O24—C26—C27—C28172.9 (4)
O72—Cr8—F7—Cr736.70 (16)O23—C26—C27—C29125.5 (4)
O74—Cr8—F7—Cr755.50 (17)O24—C26—C27—C2952.8 (5)
O84—Cr1—F8—Cr853.43 (17)Cr3—O31—C31—O326.8 (8)
O11—Cr1—F8—Cr897 (5)Cr3—O31—C31—C32174.6 (3)
F1—Cr1—F8—Cr8142.74 (16)Cr4—O32—C31—O3120.2 (8)
O82—Cr1—F8—Cr839.06 (18)Cr4—O32—C31—C32158.4 (3)
O13—Cr1—F8—Cr8125.64 (17)O31—C31—C32—C3323.0 (5)
F7—Cr8—F8—Cr1129.53 (16)O32—C31—C32—C33158.3 (4)
O81—Cr8—F8—Cr153.22 (17)O31—C31—C32—C34145.0 (4)
O83—Cr8—F8—Cr139.83 (17)O32—C31—C32—C3436.3 (5)
O72—Cr8—F8—Cr1107 (15)O31—C31—C32—C3596.2 (5)
O74—Cr8—F8—Cr1140.46 (18)O32—C31—C32—C3582.5 (5)
F8—Cr1—O11—C1184 (5)Cr4—O34—C36—O339.5 (8)
O84—Cr1—O11—C11128.0 (4)Cr4—O34—C36—C37167.6 (3)
F1—Cr1—O11—C1138.6 (4)Cr3—O33—C36—O3415.7 (9)
O82—Cr1—O11—C11139.5 (4)Cr3—O33—C36—C37167.2 (4)
O13—Cr1—O11—C1153.0 (4)O34—C36—C37—C39165.8 (5)
F1—Cr2—O12—C113.6 (4)O33—C36—C37—C3916.9 (6)
F2—Cr2—O12—C11138 (5)O34—C36—C37—C4043.0 (6)
O14—Cr2—O12—C1195.1 (4)O33—C36—C37—C40139.6 (5)
O21—Cr2—O12—C11176.0 (4)O34—C36—C37—C3874.9 (6)
O23—Cr2—O12—C1187.0 (4)O33—C36—C37—C38102.5 (5)
F8—Cr1—O13—C1687.8 (4)Cr5—O42—C41—O4119.0 (7)
O84—Cr1—O13—C16143 (8)Cr5—O42—C41—C42160.5 (3)
O11—Cr1—O13—C1691.0 (4)Cr4—O41—C41—O4210.8 (7)
F1—Cr1—O13—C160.3 (4)Cr4—O41—C41—C42169.7 (3)
O82—Cr1—O13—C16179.2 (4)O42—C41—C42—C43130.1 (4)
F1—Cr2—O14—C1641.6 (4)O41—C41—C42—C4350.3 (5)
F2—Cr2—O14—C16129.2 (4)O42—C41—C42—C45111.0 (4)
O12—Cr2—O14—C1651.9 (4)O41—C41—C42—C4568.6 (4)
O21—Cr2—O14—C16139.7 (4)O42—C41—C42—C448.9 (5)
O23—Cr2—O14—C16156 (4)O41—C41—C42—C44171.5 (4)
F1—Cr2—O21—C2127 (6)Cr4—O43—C46—O4424.4 (6)
F2—Cr2—O21—C2144.3 (4)Cr4—O43—C46—C47154.3 (3)
O12—Cr2—O21—C21134.9 (4)Cr5—O44—C46—O435.4 (6)
O14—Cr2—O21—C21131.9 (4)Cr5—O44—C46—C47176.0 (3)
O23—Cr2—O21—C2147.5 (4)O43—C46—C47—C4972.4 (4)
F2—Cr3—O22—C212.6 (4)O44—C46—C47—C49106.4 (4)
F3—Cr3—O22—C21178 (100)O43—C46—C47—C48166.9 (3)
O31—Cr3—O22—C21178.9 (4)O44—C46—C47—C4814.3 (5)
O24—Cr3—O22—C2193.3 (4)O43—C46—C47—C5046.1 (4)
O33—Cr3—O22—C2186.7 (4)O44—C46—C47—C50135.1 (4)
F1—Cr2—O23—C2690.0 (4)Cr6—O52—C51—O5116.1 (6)
F2—Cr2—O23—C262.3 (4)Cr6—O52—C51—C52168.6 (3)
O12—Cr2—O23—C26176.6 (4)Cr5—O51—C51—O5218.7 (6)
O14—Cr2—O23—C2673 (4)Cr5—O51—C51—C52156.6 (3)
O21—Cr2—O23—C2688.7 (4)O52—C51—C52—C5541.0 (5)
F2—Cr3—O24—C2651.9 (3)O51—C51—C52—C55143.3 (4)
F3—Cr3—O24—C26141.2 (3)O52—C51—C52—C54164.5 (3)
O31—Cr3—O24—C26128.2 (4)O51—C51—C52—C5419.8 (5)
O22—Cr3—O24—C2641.2 (4)O52—C51—C52—C5377.5 (4)
O33—Cr3—O24—C2637 (12)O51—C51—C52—C5398.2 (4)
F2—Cr3—O31—C31125 (4)Cr6—O54—C56—O5318.0 (5)
F3—Cr3—O31—C3137.1 (4)Cr6—O54—C56—C57161.5 (3)
O22—Cr3—O31—C31142.9 (4)Cr5—O53—C56—O5413.8 (6)
O24—Cr3—O31—C31126.7 (4)Cr5—O53—C56—C57166.7 (3)
O33—Cr3—O31—C3154.0 (4)O54—C56—C57—C58130.2 (4)
F4—Cr4—O32—C31121 (4)O53—C56—C57—C5849.4 (5)
F3—Cr4—O32—C313.6 (5)O54—C56—C57—C59B40.4 (6)
O41—Cr4—O32—C31176.2 (5)O53—C56—C57—C59B140.0 (6)
O34—Cr4—O32—C3193.7 (5)O54—C56—C57—C60B168.2 (6)
O43—Cr4—O32—C3184.3 (5)O53—C56—C57—C60B12.2 (6)
F2—Cr3—O33—C3690.3 (5)O54—C56—C57—C597.5 (5)
F3—Cr3—O33—C361.0 (5)O53—C56—C57—C59172.1 (4)
O31—Cr3—O33—C3689.7 (5)O54—C56—C57—C60111.2 (4)
O22—Cr3—O33—C36176.6 (5)O53—C56—C57—C6069.3 (4)
O24—Cr3—O33—C36179 (100)O54—C56—C57—C58B76.2 (6)
F4—Cr4—O34—C36126.6 (5)O53—C56—C57—C58B103.4 (6)
F3—Cr4—O34—C3638.6 (5)Cr7—O62—C61—O6127.8 (6)
O41—Cr4—O34—C36142.4 (5)Cr7—O62—C61—C62153.7 (3)
O32—Cr4—O34—C3654.4 (5)Cr6—O61—C61—O627.7 (6)
O43—Cr4—O34—C3611 (4)Cr6—O61—C61—C62170.8 (3)
F4—Cr4—O41—C4140.5 (4)O62—C61—C62—C63138.2 (4)
F3—Cr4—O41—C4132 (9)O61—C61—C62—C6343.2 (5)
O32—Cr4—O41—C41138.0 (4)O62—C61—C62—C65103.5 (4)
O34—Cr4—O41—C41130.0 (4)O61—C61—C62—C6575.1 (4)
O43—Cr4—O41—C4151.0 (4)O62—C61—C62—C6415.8 (5)
F5—Cr5—O42—C41172 (34)O61—C61—C62—C64165.6 (4)
F4—Cr5—O42—C414.5 (4)Cr7—O64—C66—O6319.2 (6)
O51—Cr5—O42—C41176.4 (4)Cr7—O64—C66—C67161.0 (3)
O44—Cr5—O42—C4194.8 (4)Cr6—O63—C66—O6414.7 (6)
O53—Cr5—O42—C4184.8 (4)Cr6—O63—C66—C67165.2 (3)
F4—Cr4—O43—C465.8 (4)O64—C66—C67—C693.3 (5)
F3—Cr4—O43—C4682.1 (4)O63—C66—C67—C69176.8 (4)
O41—Cr4—O43—C4696.9 (4)O64—C66—C67—C69B163.0 (12)
O32—Cr4—O43—C46175.2 (4)O63—C66—C67—C69B16.8 (12)
O34—Cr4—O43—C46110 (4)O64—C66—C67—C68126.7 (4)
F5—Cr5—O44—C46128.1 (4)O63—C66—C67—C6853.4 (5)
F4—Cr5—O44—C4638.8 (4)O64—C66—C67—C70B26.8 (8)
O51—Cr5—O44—C46140.6 (4)O63—C66—C67—C70B153.1 (8)
O42—Cr5—O44—C4653.5 (4)O64—C66—C67—C68B83.0 (9)
O53—Cr5—O44—C466 (17)O63—C66—C67—C68B97.1 (8)
F5—Cr5—O51—C5147.1 (3)O64—C66—C67—C70116.2 (4)
F4—Cr5—O51—C51172 (100)O63—C66—C67—C7063.7 (5)
O42—Cr5—O51—C51132.8 (3)Cr7—O71—C71—O729.9 (7)
O44—Cr5—O51—C51135.3 (3)Cr7—O71—C71—C72173.9 (3)
O53—Cr5—O51—C5145.0 (3)Cr8—O72—C71—O7123.0 (7)
F6—Cr6—O52—C5195 (25)Cr8—O72—C71—C72153.0 (3)
F5—Cr6—O52—C516.7 (4)O71—C71—C72—C74162.8 (4)
O61—Cr6—O52—C51174.8 (4)O72—C71—C72—C7420.7 (5)
O63—Cr6—O52—C5182.3 (4)O71—C71—C72—C7340.9 (5)
O54—Cr6—O52—C5196.2 (4)O72—C71—C72—C73142.6 (4)
F5—Cr5—O53—C561.8 (3)O71—C71—C72—C7577.6 (4)
F4—Cr5—O53—C5687.4 (3)O72—C71—C72—C7598.8 (5)
O51—Cr5—O53—C5693.2 (4)Cr7—O73—C76—O7414.4 (7)
O42—Cr5—O53—C56179.8 (4)Cr7—O73—C76—C77168.4 (3)
O44—Cr5—O53—C56121 (16)Cr8—O74—C76—O7317.8 (7)
F6—Cr6—O54—C56133.0 (3)Cr8—O74—C76—C77159.5 (3)
F5—Cr6—O54—C5646.4 (3)O73—C76—C77—C7866.8 (4)
O61—Cr6—O54—C56136.2 (3)O74—C76—C77—C78110.7 (4)
O63—Cr6—O54—C5617 (3)O73—C76—C77—C7951.6 (4)
O52—Cr6—O54—C5647.1 (3)O74—C76—C77—C79131.0 (4)
F6—Cr6—O61—C6142.9 (3)O73—C76—C77—C80172.8 (3)
F5—Cr6—O61—C6174 (2)O74—C76—C77—C809.7 (5)
O63—Cr6—O61—C6149.6 (4)Cr8—O81—C81—O820.2 (7)
O54—Cr6—O61—C61132.9 (3)Cr8—O81—C81—C82179.5 (3)
O52—Cr6—O61—C61136.9 (3)Cr1—O82—C81—O8128.9 (7)
F7—Cr7—O62—C61108 (7)Cr1—O82—C81—C82150.7 (3)
O71—Cr7—O62—C61170.7 (4)O81—C81—C82—C84179.1 (4)
F6—Cr7—O62—C6110.9 (4)O82—C81—C82—C841.2 (5)
O73—Cr7—O62—C6178.1 (4)O81—C81—C82—C8360.8 (5)
O64—Cr7—O62—C61100.9 (4)O82—C81—C82—C83118.8 (4)
F6—Cr6—O63—C663.6 (4)O81—C81—C82—C8558.2 (5)
F5—Cr6—O63—C6683.0 (4)O82—C81—C82—C85122.1 (4)
O61—Cr6—O63—C6694.5 (4)Cr1—O84—C86—O8316.2 (6)
O54—Cr6—O63—C66146 (2)Cr1—O84—C86—C87162.2 (3)
O52—Cr6—O63—C66176.4 (4)Cr8—O83—C86—O8411.4 (7)
F7—Cr7—O64—C66136.3 (3)Cr8—O83—C86—C87170.2 (3)
O71—Cr7—O64—C66132.5 (3)O84—C86—C87—C898.8 (6)
F6—Cr7—O64—C6647.9 (3)O83—C86—C87—C89172.6 (5)
O73—Cr7—O64—C6614 (4)O84—C86—C87—C88B170.1 (7)
O62—Cr7—O64—C6644.2 (3)O83—C86—C87—C88B11.4 (8)
F7—Cr7—O71—C7143.1 (4)O84—C86—C87—C90113.0 (5)
F6—Cr7—O71—C71121 (4)O83—C86—C87—C9065.6 (5)
O73—Cr7—O71—C7149.6 (4)O84—C86—C87—C88130.6 (5)
O62—Cr7—O71—C71136.0 (4)O83—C86—C87—C8850.8 (5)
O64—Cr7—O71—C71132.2 (4)O84—C86—C87—C90B68.4 (7)
F8—Cr8—O72—C7116 (15)O83—C86—C87—C90B110.1 (6)
F7—Cr8—O72—C717.3 (4)O84—C86—C87—C89B45.7 (7)
O81—Cr8—O72—C71175.5 (4)O83—C86—C87—C89B135.7 (6)
O83—Cr8—O72—C7182.5 (4)O2A—C2A—C1A—N1115.2 (15)
O74—Cr8—O72—C7197.3 (4)C2A—C1A—N1—C1B172.7 (15)
F7—Cr7—O73—C762.2 (4)C1A—N1—C1B—C2B166.7 (17)
O71—Cr7—O73—C7693.5 (4)N1—C1B—C2B—O2B64 (3)
F6—Cr7—O73—C7686.2 (4)O2C—C2C—C1C—N1C107 (2)
O62—Cr7—O73—C76178.3 (4)C2C—C1C—N1C—C1D157 (2)
O64—Cr7—O73—C76148 (4)C1C—N1C—C1D—C2D113 (5)
F8—Cr8—O74—C76133.0 (4)N1C—C1D—C2D—O2D156 (4)
F7—Cr8—O74—C7646.7 (4)O2E—C2E—C1E—N1E10 (6)
O81—Cr8—O74—C76135.6 (4)C2E—C1E—N1E—C1F156 (4)
O83—Cr8—O74—C7631 (9)C1E—N1E—C1F—C2F146 (2)
O72—Cr8—O74—C7646.5 (4)N1E—C1F—C2F—O2F92 (3)
F8—Cr8—O81—C8136.2 (4)O99i—O99—C99—O980.7 (14)
F7—Cr8—O81—C8185.0 (18)O99i—O99—C99—C98179.2 (14)
Symmetry code: (i) x+1, y+1, z+2.

Experimental details

Crystal data
Chemical formula(C4H12NO2)[Cr7NiF8(C5H9O2)16]·0.5C4H8O2
Mr2342.85
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)24.9892 (15), 16.6220 (9), 30.8299 (19)
β (°) 110.506 (3)
V3)11994.4 (12)
Z4
Radiation typeMo Kα
µ (mm1)0.78
Crystal size (mm)0.38 × 0.3 × 0.25
Data collection
DiffractometerBruker X8 APEX-II
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.723, 0.823
No. of measured, independent and
observed [I > 2σ(I)] reflections
209153, 38517, 28754
Rint0.035
(sin θ/λ)max1)0.727
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.091, 0.258, 1.04
No. of reflections38517
No. of parameters1066
No. of restraints141
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.1134P)2 + 52.1149P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.10, 1.17

Computer programs: SMART (Bruker, 2004), SAINT-Plus (Bruker, 2004), SAINT-Plus, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97, enCIFer (Version 1.1; Allen et al., 2004) and WinGX (Version 1.70.00; Farrugia, 1999).

 

Acknowledgements

This work was supported by the INTAS (03–51-4532) and the EPSRC (UK).

References

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First citationLarsen, F. K., Overgaard, J., Parsons, S., Rentschler, E., Smith, A. A., Timco, G. A. & Winpenny, R. E. P. (2003). Angew. Chem. Int. Ed. 42, 5978–5981. Web of Science CSD CrossRef CAS
First citationLassahn, P.-G., Lozan, V., Timco, G. A., Christian, P., Janiak C. & Winpenny, R. E. P. (2004). J. Catal. 222, 260–267.
First citationMeier, F., Levy, J. & Loss, D. (2003). Phys. Rev. Lett. 90, 047901–1. Web of Science CrossRef PubMed
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
First citationSheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.

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