Insights into crystallization mechanism: a synchrotron study of polymorphism in a cobalt acetate cluster compound

Burley, J.C.; Prior, T.J.

doi:10.1107/S0108270105041570

metal-organic compounds

STRUCTURAL
CHEMISTRY

ISSN: 2053-2296

Volume 62| Part 2| February 2006| Pages m63-m66

doi:10.1107/S0108270105041570

Insights into crystallization mechanism: a synchrotron study of polymorphism in a cobalt acetate cluster compound

Jonathan C. Burley ^a ^* and Timothy J. Prior ^b

^aUniversity Chemical Laboratory, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, England, and ^bSynchrotron Radiation Department, Daresbury Laboratory, Warrington, Cheshire WA4 4AD, England
^*Correspondence e-mail: jb442@hermes.cam.ac.uk

(Received 7 December 2005; accepted 12 December 2005; online 21 January 2006)

The structure of the title compound, di-μ₃-acetato-1κ²O,O′:2κO′;2κO:3κ²O,O′-di-μ₂-acetato-1κO:2κO′;2κO:3κO′-octapyridyl-1κ³N,2κ²N,3κ³N-tricobalt(II) bis(hexafluorophosphate), [Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂, consists of divalent multinuclear cations in which three Co^II ions are bridged by four μ₂-acetate groups. The Co^II ions are arranged in an approximately linear manner. The bridging acetates adopt two distinct coordination geometries: one pair bridges via a single O atom and the other pair employs both O atoms. The coordination octahedron around each Co^II ion is completed by three pyridine molecules for the two outer Co^II ions and by two for the inner ion. Charge is balanced by two PF₆⁻ anions. Single-crystal synchrotron X-ray studies indicate the existence of two polymorphs, both triclinic, which are distinguished primarily by differences in the relative orientations of the multinuclear cations, which in form 1 are tilted with respect to each other, but in form 2 are co-parallel as a result of the central Co atom lying on an inversion centre. The results of the structural studies allow an insight into the crystallization mechanism and resultant polymorphism. They suggest that a (bidentate carboxyl)C—O⋯H—C(pyridine) interaction exists in solution. For form 1, crystallized from pyridine, the interaction is not structure determining, as it is satisfied by interactions between solvent and solute. For form 2, crystallized from CH₂Cl₂, the interaction is between a bound acetate carboxyl group on one cation and a bound pyridine on another and is thus structure directing.

Comment

Multinuclear transition metal complexes have been intensively studied over a number of years, with interest driven by structural similarities to active sites in biological systems (Hagen et al., 1993 ), fundamental magnetism studies (Chudnovsky, 1996 ) and possible use as supramolecular building blocks (Yaghi et al., 2003 ). During the course of investigations into possible complexes formed by Co^II, pyridine and acetate derivatives, the title compound, (I), was isolated as two polymorphs (Figs. 1 and 2). Examination of the refined crystal structures allows postulation of a crystal nucleation mechanism which is consistent both with the synthetic conditions and the existence of the two polymorphic forms.

Both polymorphs adopt the space group P $[\overline{1}]$ , form 1 with Z = 4 and form 2 with Z = 1. The cations in both forms adopt essentially identical molecular structures and are formed by three Co^II ions arranged in an approximately linear manner. The cations possess an approximate (form 1) or an exact (form 2) crystallographic centre of symmetry located at the central Co^II ion. For octahedral coordination about Co^II, there are 18 coordination sites available for the ligands. The three Co^II ions are linked by four bridging acetate groups, which adopt two distinct coordination modes. One pair of acetates bridges in a syn–syn manner, with each O atom coordinated to a single Co^II ion, thus occupying a total of four coordination sites. The other pair of acetates adopts a syn–anti configuration, with one O atom acting as a μ₂-bridge and the other coordinated to a single Co^II ion. This pair of acetates therefore occupies a total of six coordination sites. The coordination modes adopted by the acetate groups lead to the central Co^II ion being surrounded by four O atoms, arranged in an approximately square-planar manner; for form 2, the O—Co—O angles deviate from 90° by 1.56 (15)°. The terminal Co^II ions are surrounded by three O atoms, which are not regularly spaced; for form 2, the O4—Co2—O3 angle is 60.7 (1)°, whereas O2—Co2—O3 is 101.4 (1)°. The remaining eight available metal-coordination sites are occupied by pyridines, two of which bind along the molecular axis and six of which bind perpendicular to the molecular axis. The lack of an exact molecular centre of symmetry in form 1 is manifested primarily in the lengths of the trans bonds about the central Co^II ion, Co2—O2 and Co2—O7 (formed by the acetate μ₂-O atom), which are 2.154 (2) and 2.134 (2) Å, respectively; each pair of bond lengths is identical by symmetry in form 2. In form 1, half of the PF₆⁻ groups exhibit a significant degree of rotational disorder about the central P atom; the occupancies, constrained to sum to unity, refined to 0.565 (5):0.435 (5) and 0.600 (4):0.400 (4) for the major and minor components of P2 and P4, respectively. However, in form 2 there is no evidence in difference Fourier maps for disorder of the PF₆⁻ units.

In terms of crystal packing, for both polymorphs the cations and anions adopt an arrangement in which layers are formed in the ab plane. It should be noted that a description of the structure as layered is for convenience and does not reflect the presence of any obvious specific intralayer interactions. The two forms are very similar. In fact, viewed along [100] and [ $[\overline{1}]$ 00], the two structures may practically be superimposed (Fig. 3a and 3b). However, when the two forms are viewed in a projection achieved by rotating by 90° about the normal to 001, a significant difference becomes clear. In form 2, the layers are formed by cations which have Co⋯Co⋯Co molecular axes co-parallel (Fig. 3d). However, in form 1 the two distinct trimers are not arranged with their axes co-parallel (Fig. 3c).

The only notable non-ionic interaction in either polymorph is the short C—O⋯H—C distance (carboxyl–pyridine) of 2.56 Å between cations in form 2 (Fig. 4). This can be compared with the sum of the van der Waals radii (2.72 Å; Bondi, 1964 ; Rowland & Taylor, 1996 ) and the average of the intramolecular C—O⋯H—C(pyridine) distances (2.62 Å). Thus, in form 2 the intermolecular C—O⋯H—C distance is 0.15 Å shorter than the sum of the van der Waals radii, and 0.03 Å shorter than the corresponding mean intramolecular distance. The equivalent distance in form 1 is 3.13 Å, which is 0.41 Å greater than sum of the van der Waals radii and 0.54 Å longer than the corresponding distance in form 2. These short C—O⋯H—C interactions in form 2 form a linear network of cations which runs along the a axis. Given the generally accepted correlation between intermolecular distance and interaction strength, it seems reasonable that this interaction has the potential to be chemically important and structure directing.

The presence of this short contact in form 2 and its absence in form 1 are consistent with a crystal nucleation mechanism in which the intermolecular C—O⋯H—C interaction occurs between a bridging acetate of one cation and pyridine. For form 1, crystallized from pyridine, the interaction is between the cations and the solvent molecules, whereas for form 2, crystallized from CH₂Cl₂, the interaction is between a bound pyridine on one cation and a bridging acetate on a neighbouring cation, and is thus structure-directing.

Form 1 has a slightly lower volume per formula unit than form 2 [1375.98 (13) versus 1379.3 (8) Å³], and thus packing considerations suggest that form 1 has the lower lattice energy, although the difference may be slight. Furthermore, the disorder in the PF₆⁻ groups suggests that form 1 should also be favoured on entropic grounds. That form 2 has been isolated despite the apparent greater stability of form 1 in terms of both lattice energy and lattice entropy is consistent with our argument above that the pyridine-H⋯O—C interaction is of some importance in stabilizing this form, both kinetically in the crystallization of both forms, and thermodynamically in the stability of form 2.

In conclusion, structural studies of the two polymorphic forms of (I) have provided an insight into the crystal nucleation mechanism for this compound and the reason for the existence of two polymorphs.

Figure 1
The molecular structure of form 1 of compound (I)

. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. Both disorder components of the PF₆⁻ ions are shown.

Figure 2
The molecular structure of form 2 of compound (I)

. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. [Symmetry code: (i) 1-x, 1-y, 1-z.]

Figure 3
Packing diagrams (PLATON; Spek, 2003

) of the two polymorphic forms of (I)

. (a) Projection view of form 1 along 100, (b) projection view of form 2 along $[\overline{1}]$ 00, (c) projection view of form 1 rotated 90° about the normal to 001 and (d) projection of form 2 rotated 90° to the 001 normal.

Figure 4
Intermolecular interactions in form 2 of (I)

; these are absent in form 1 (PLATON; Spek, 2003

Experimental

A solution of Co(OAc)₂·4H₂O (0.5 g), pyridine (10 ml) and acetic anydride (5 ml) were warmed to 323 K and stirred for approximately 4 h. Two molar equivalents of NH₄PF₆ were added, and a pink solid was precipitated on addition of excess hexane. Pink transparent crystals of form 1 of (I) were grown by slow cooling of a saturated solution in pyridine. Crystals of form 2 of (I) were obtained by recrystallization from dichloromethane. The crystals are air-stable for several months.

Compound (I), polymorph 1

Crystal data

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂
M_r = 1335.71
Triclinic, $[P \overline 1]$
a = 10.7354 (6) Å
b = 22.1257 (12) Å
c = 23.6103 (13) Å
α = 99.380 (1)°
β = 95.008 (1)°
γ = 92.238 (1)°
V = 5503.9 (5) Å³
Z = 4
D_x = 1.612 Mg m⁻³
Synchrotron radiation
λ = 0.84610 Å
Cell parameters from 38731 reflections
θ = 3.6–31.6°
μ = 1.05 mm⁻¹
T = 120 (2) K
Plate, pink
0.25 × 0.1 × 0.05 mm

Data collection

Bruker D8 diffractometer
ω rotation scans with narrow frames
Absorption correction: multi-scan(SADABS; Bruker, 2004 )T_min = 0.463, T_max = 0.949
38731 measured reflections
21108 independent reflections
17966 reflections with I > 2σ(I)
R_int = 0.030
θ_max = 31.6°
h = 0 → 13
k = −27 → 27
l = −29 → 28

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.056
wR(F²) = 0.152
S = 1.05
21108 reflections
1432 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0871P)² + 8.495P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max = 0.002
Δρ_max = 1.48 e Å⁻³
Δρ_min = −1.46 e Å⁻³

Compound (I), polymorph 2

Crystal data

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂
M_r = 1335.71
Triclinic, $[P \overline 1]$
a = 10.688 (4) Å
b = 11.839 (4) Å
c = 12.480 (4) Å
α = 98.149 (5)°
β = 103.605 (5)°
γ = 111.722 (5)°
V = 1379.3 (8) Å³
Z = 1
D_x = 1.608 Mg m⁻³
Synchrotron radiation
λ = 0.67110 Å
Cell parameters from 3499 reflections
θ = 3.0–26.9°
μ = 1.05 mm⁻¹
T = 120 (2) K
Needle, pink
0.1 × 0.02 × 0.02 mm

Data collection

Bruker D8 diffractometer
ω rotation scans with narrow frames
Absorption correction: multi-scan(SADABS; Bruker, 2004)T_min = 0.207, T_max = 1
11698 measured reflections
5565 independent reflections
3897 reflections with I > 2σ(I)
R_int = 0.052
θ_max = 24.8°
h = −13 → 13
k = −14 → 14
l = −15 → 15

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.072
wR(F²) = 0.214
S = 1.03
5565 reflections
369 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.1413P)² + 0.0662P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max < 0.001
Δρ_max = 1.29 e Å⁻³
Δρ_min = −0.84 e Å⁻³

Pyridine H atoms were placed in idealized positions, with C—H = 0.93 Å, and refined as riding, with U_iso(H) = 1.2U_eq(C). Methyl H atom were also placed in idealized positions, with C—H = 0.96 Å, and refined with U_iso(H) = 1.5U_eq(C). For form 2, the highest difference peak is located 1.04 Å from atom H2B and the deepest hole is 0.82 Å from atom Co1. A number of difference peaks with density greater than 1 e Å⁻³ were present and are due to the quality of the crystal employed, which was the best available.

For both compounds, data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Version 1.64; Farrugia, 1999 ) and PLATON (Spek, 2003 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, II, global. DOI: 10.1107/S0108270105041570/fa1176sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S0108270105041570/fa1176Isup2.hkl

Structure factors: contains datablock II. DOI: 10.1107/S0108270105041570/fa1176IIsup3.hkl

Comment top

Multinuclear transition metal complexes have been intensively studied over a number of years, with interest driven by structural similarities to active sites in biological systems (Hagen et al., 1993), fundamental magnetism studies (Chudnovsky, 1996) and possible use as supramolecular building blocks (Yaghi et al., 2003). During the course of investigations into possible complexes formed by Co^II, pyridine and acetate derivatives, the title compound, (I), was isolated as two polymorphs (Figs. 1 and 2). Examination of the refined crystal structures allows postulation of a crystal nucleation mechanism which is consistent both with the synthetic conditions and the existence of the two polymorphic forms.

Both polymorphs adopt the space group P1, form 1 with Z = 4 and form 2 with Z = 1. The cations in both forms adopt essentially identical molecular structures and are formed by three Co^II ions arranged in an approximately linear manner. The cations possess an approximate (form 1) or an exact (form 2) crystallographic centre of symmetry located at the central Co^II ion. For octahedral coordination about Co^II, there are 18 coordination sites available for the ligands. The three Co^II ions are linked by four bridging acetate groups, which adopt two distinct coordination modes. One pair of acetates bridges in a syn–syn manner, with each O atom coordinated to a single Co^II ion, thus occupying a total of four coordination sites. The other pair of acetates adopts a syn–anti configuration, with one O atom acting as a µ₂-bridge and the other coordinated to a single Co^II ion. This pair of acetates therefore occupies a total of six coordination sites. The coordination modes adopted by the acetate groups lead to the central Co^II ion being surrounded by four O atoms, arranged in an approximately square-planar manner; for form 2, the O—Co—O angles deviate from 90° by 1.56 (15)°. The terminal Co^II ions are surrounded by three O atoms, which are not regularly spaced; for form 2, the O4—Co2—O3 angle is 60.7 (1)°, whereas the O2—Co2—O3 angle is 101.4 (1)°. The remaining eight available metal-coordination sites are occupied by pyridine molecules, two of which bind along the molecular axis and six of which bind perpendicular to the molecular axis. The lack of an exact molecular centre of symmetry in form 1 is manifested primarily in the lengths of the trans bonds about the central Co^II ion, Co2—O2 and Co2—O7 (formed by the µ₂-bridging O atom of the acetate), which are 2.154 (2) and 2.134 (2) Å, respectively; each pair of bond lengths is identical by symmetry in form 2. In form 1, half of the PF₆⁻ groups exhibit a significant degree of rotational disorder about the central P atom; the occupancies, constrained to sum to unity, refined to 0.565 (5):0.435 (5) and 0.600 (4):0.400 (4) for the major and minor components of P2 and P4, respectively. However, in form 2 there is no evidence in difference Fourier maps for disorder of the PF₆⁻ units.

In terms of crystal packing, for both polymorphs the cations and anions adopt an arrangement in which layers are formed in the ab plane. It should be noted that a description of the structure as layered is for convenience and does not reflect the presence of any obvious specific intralayer interactions. The two forms are very similar. In fact, viewed along [100] and [100], the two structures may practically be superimposed (Fig. 3a and 3b). However, when the two forms are viewed in a projection achieved by rotating by 90° about the normal to 001, a significant difference becomes clear. In form 2, the layers are formed by cations which have Co···Co···Co molecular axes co-parallel (Fig. 3d). However, in form 1 the two distinct trimers are not arranged with their axes co-parallel (Fig. 3c).

The only notable non-ionic interaction in either polymorph is the short C—O···H—C distance (carboxyl···pyridine) of 2.56 Å between cations in form 2 (Fig. 4). This can be compared with the sum of the van der Waals radii (2.72 Å; Reference?) and the average of the intramolecular C—O···H—C(pyridine) distances (2.62 Å). Thus, in form 2 the intermolecular C—O···H—C distance is 0.15 Å shorter than the sum of the van der Waals radii, and 0.03 Å shorter than the corresponding mean intramolecular distance. The equivalent distance in form 1 is 3.13 Å, which is 0.41 Å greater than sum of the van der Waals radii and 0.54 Å longer than the corresponding distance in form 2. These short C—O···H—C interactions in form 2 form a linear network of cations which runs along the a axis. Given the generally accepted correlation between intermolecular distance and interaction strength, it seems reasonable that this interaction has the potential to be chemically important and structure-directing.

The presence of this short contact in form 2 and its absence in form 1 are consistent with a crystal nucleation mechanism in which the intermolecular C—O···H—C interaction occurs between a bridging acetate of one cation and pyridine. For form 1, crystallized from pyridine, the interaction is between the cations and the solvent molecules, whereas for form 2, crystallized from CH₂Cl₂, the interaction is between a bound pyridine on one cation and a bridging acetate on a neighbouring cation, and is thus structure-directing.

Form 1 has a slightly lower volume per formula unit than form 2 [1375.98 (13) versus 1379.3 (8) Å³], and thus packing considerations suggest that form 1 has the lower lattice energy, although the difference may be slight. Furthermore, the disorder in the PF₆⁻ groups suggests that form 1 should also be favoured on entropic grounds. That form 2 has been isolated despite the apparent greater stability of form 1 in terms of both lattice energy and lattice entropy is consistent with our argument above that the py-H···O—C interaction is of some importance in stabilizing this form, both kinetically in the crystallization of both forms, and thermodynamically in the stability of form 2.

Experimental top

Computing details top

For both compounds, data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Version 1.64; Farrugia, 1999) and PLATON (Spek, 2003); software used to prepare material for publication: SHEXLX97.

Figures top

	Fig. 1. The molecular structure of form 1 of compound (I). Displacement ellipsoids are drawn at the ?? probability level and H atoms are shown as small spheres of arbitrary radii. Both disorder components of the PF₆⁻ ions are shown.
	Fig. 2. The molecular structure of form 2 of compound (I). Displacement ellipsoids are drawn at the ?? probability level and H atoms are shown as small spheres of arbitrary radii.
	Fig. 3. Packing diagrams (PLATON; Spek, 2003) of the two polymorphic forms of (I). (a) Projection view of form 1 along 100. (b) Projection view of form 2 along 100. (c) Projection view of form 1 rotated 90° about the normal to 001. (d) Projection of form 2 rotated 90° to the 001 normal.
	Fig. 4. Intermolecular interactions in form 2 of (I), absent in form 1. (PLATON; Spek, 2003).

(I) di-µ₃-acetato-1κ²O,O':2κO';2κO:3κ²O,O'-di-µ₂-acetato- 1κO:2κO';2κO:3κO'-octapyridyl-1κ³N,2κ²N,3κ³N-tricobalt(II) bis(hexafluorophosphate) top

Crystal data top

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂	Z = 4
M_r = 1335.71	F(000) = 2716
Triclinic, P1	D_x = 1.612 Mg m⁻³
Hall symbol: -P 1	Synchrotron radiation, λ = 0.84610 Å
a = 10.7354 (6) Å	Cell parameters from 38731 reflections
b = 22.1257 (12) Å	θ = 3.6–31.6°
c = 23.6103 (13) Å	µ = 1.05 mm⁻¹
α = 99.380 (1)°	T = 120 K
β = 95.008 (1)°	Plate, pink
γ = 92.238 (1)°	0.25 × 0.1 × 0.05 mm
V = 5503.9 (5) Å³

Data collection top

Bruker D8 diffractometer	21108 independent reflections
Radiation source: Daresbury SRS Station 16.2SMX	17966 reflections with I > 2σ(I)
Silicon 111 monochromator	R_int = 0.030
ω rotation with narrow frames scans	θ_max = 31.6°, θ_min = 3.6°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = 0→13
T_min = 0.463, T_max = 0.949	k = −27→27
38731 measured reflections	l = −29→28

Refinement top

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)] = 0.056	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.152	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0871P)² + 8.495P] where P = (F_o² + 2F_c²)/3
21108 reflections	(Δ/σ)_max = 0.002
1432 parameters	Δρ_max = 1.48 e Å⁻³
66 restraints	Δρ_min = −1.46 e Å⁻³

Crystal data top

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂	γ = 92.238 (1)°
M_r = 1335.71	V = 5503.9 (5) Å³
Triclinic, P1	Z = 4
a = 10.7354 (6) Å	Synchrotron radiation, λ = 0.84610 Å
b = 22.1257 (12) Å	µ = 1.05 mm⁻¹
c = 23.6103 (13) Å	T = 120 K
α = 99.380 (1)°	0.25 × 0.1 × 0.05 mm
β = 95.008 (1)°

Data collection top

Bruker D8 diffractometer	21108 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	17966 reflections with I > 2σ(I)
T_min = 0.463, T_max = 0.949	R_int = 0.030
38731 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.056	66 restraints
wR(F²) = 0.152	H-atom parameters constrained
S = 1.05	Δρ_max = 1.48 e Å⁻³
21108 reflections	Δρ_min = −1.46 e Å⁻³
1432 parameters

Special details top

Experimental. A correction to account for decay of the synchrotron beam with time and crystal absorption is applied within the program SAINT v7.0 using a multi-scan method based on equivalents. Ratio of minimum to maximum apparent transmission: 0.487966

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.64029 (4)	1.034157 (18)	0.206669 (18)	0.01183 (11)
C1	0.4323 (3)	0.99007 (14)	0.22652 (13)	0.0134 (6)
O1	0.4445 (2)	1.04186 (10)	0.21098 (10)	0.0170 (5)
O2	0.5304 (2)	0.96107 (9)	0.23618 (9)	0.0137 (4)
C2	0.3048 (3)	0.96341 (15)	0.23191 (17)	0.0216 (7)
H2A	0.2510	0.9959	0.2436	0.032*
H2B	0.3102	0.9368	0.2602	0.032*
H2C	0.2711	0.9404	0.1954	0.032*
C3	0.8504 (3)	0.95504 (13)	0.23090 (13)	0.0119 (6)
O3	0.8156 (2)	1.00660 (10)	0.21999 (10)	0.0173 (5)
O4	0.7788 (2)	0.90986 (10)	0.23319 (10)	0.0156 (5)
C4	0.9886 (3)	0.94904 (16)	0.24188 (17)	0.0220 (7)
H4A	1.0054	0.9310	0.2759	0.033*
H4B	1.0309	0.9889	0.2473	0.033*
H4C	1.0180	0.9234	0.2095	0.033*
Co2	0.60728 (4)	0.875518 (16)	0.249667 (17)	0.00939 (10)
C5	0.3643 (3)	0.79420 (14)	0.26379 (13)	0.0124 (6)
C6	0.2259 (3)	0.79898 (15)	0.24861 (16)	0.0207 (7)
H6A	0.1928	0.8271	0.2783	0.031*
H6B	0.1838	0.7593	0.2453	0.031*
H6C	0.2130	0.8136	0.2126	0.031*
O5	0.4346 (2)	0.84106 (9)	0.26495 (10)	0.0151 (5)
O6	0.3994 (2)	0.74296 (10)	0.27435 (10)	0.0167 (5)
Co3	0.57472 (4)	0.718275 (18)	0.293467 (19)	0.01227 (11)
C7	0.7847 (3)	0.76370 (14)	0.27602 (14)	0.0147 (6)
O7	0.6849 (2)	0.79162 (9)	0.26488 (9)	0.0132 (4)
O8	0.7735 (2)	0.71371 (10)	0.29431 (10)	0.0184 (5)
C8	0.9116 (3)	0.79016 (15)	0.26857 (16)	0.0193 (7)
H8A	0.9421	0.8184	0.3027	0.029*
H8B	0.9059	0.8114	0.2361	0.029*
H8C	0.9681	0.7577	0.2620	0.029*
Co4	0.09639 (4)	0.526541 (18)	0.203858 (19)	0.01364 (11)
C1B	−0.1125 (3)	0.44947 (13)	0.23402 (13)	0.0129 (6)
O9	−0.0791 (2)	0.49328 (10)	0.20959 (10)	0.0183 (5)
O10	−0.0445 (2)	0.40756 (10)	0.24609 (10)	0.0167 (5)
C2B	−0.2451 (3)	0.44746 (15)	0.25030 (16)	0.0204 (7)
H2B1	−0.2975	0.4216	0.2202	0.031*
H2B2	−0.2749	0.4882	0.2555	0.031*
H2B3	−0.2473	0.4313	0.2856	0.031*
C3B	0.3079 (3)	0.49299 (14)	0.23584 (14)	0.0144 (6)
O11	0.2939 (2)	0.54147 (10)	0.21480 (10)	0.0197 (5)
O12	0.2102 (2)	0.46110 (9)	0.24275 (9)	0.0136 (4)
Co5	0.13078 (4)	0.374367 (16)	0.255211 (17)	0.01001 (10)
C4B	0.4369 (3)	0.47353 (15)	0.25081 (15)	0.0179 (7)
H4B1	0.4730	0.4572	0.2161	0.027*
H4B2	0.4326	0.4426	0.2749	0.027*
H4B3	0.4880	0.5083	0.2711	0.027*
C5B	0.3725 (3)	0.29689 (14)	0.27036 (13)	0.0129 (6)
O13	0.3055 (2)	0.34083 (10)	0.26578 (10)	0.0157 (5)
O14	0.3395 (2)	0.24821 (10)	0.28834 (10)	0.0187 (5)
C6B	0.5037 (3)	0.30122 (15)	0.25271 (16)	0.0199 (7)
H6B1	0.5027	0.3185	0.2179	0.030*
H6B2	0.5356	0.2610	0.2462	0.030*
H6B3	0.5563	0.3270	0.2828	0.030*
C7B	−0.0485 (3)	0.25472 (14)	0.27163 (14)	0.0138 (6)
O15	0.0495 (2)	0.28717 (9)	0.26547 (9)	0.0135 (4)
O16	−0.0356 (2)	0.20490 (10)	0.28958 (10)	0.0181 (5)
C8B	−0.1774 (3)	0.27556 (15)	0.25751 (15)	0.0197 (7)
H8B1	−0.2272	0.2425	0.2336	0.030*
H8B2	−0.1715	0.3098	0.2374	0.030*
H8B3	−0.2158	0.2877	0.2925	0.030*
Co6	0.16304 (4)	0.218051 (18)	0.297719 (19)	0.01354 (11)
N1	0.6694 (3)	1.09403 (12)	0.29038 (12)	0.0156 (6)
C10	0.7448 (3)	1.08051 (16)	0.33458 (15)	0.0214 (7)
H10	0.7843	1.0436	0.3295	0.026*
C11	0.7664 (4)	1.11902 (17)	0.38736 (16)	0.0267 (8)
H11	0.8180	1.1076	0.4171	0.032*
C12	0.7104 (3)	1.17453 (16)	0.39534 (15)	0.0229 (7)
H12	0.7247	1.2014	0.4301	0.027*
C13	0.6327 (3)	1.18908 (16)	0.35032 (15)	0.0228 (7)
H13	0.5932	1.2260	0.3542	0.027*
C14	0.6147 (3)	1.14737 (15)	0.29909 (14)	0.0177 (7)
H14	0.5615	1.1573	0.2692	0.021*
N2	0.6693 (3)	1.10945 (12)	0.16380 (12)	0.0176 (6)
C20	0.5760 (3)	1.14450 (15)	0.14927 (15)	0.0191 (7)
H20	0.4977	1.1379	0.1619	0.023*
C21	0.5915 (4)	1.18989 (16)	0.11640 (15)	0.0238 (8)
H21	0.5254	1.2138	0.1078	0.029*
C22	0.7073 (4)	1.19931 (17)	0.09628 (17)	0.0298 (9)
H22	0.7200	1.2294	0.0738	0.036*
C23	0.8030 (4)	1.16302 (18)	0.11045 (19)	0.0353 (10)
H23	0.8812	1.1678	0.0971	0.042*
C24	0.7806 (4)	1.11943 (17)	0.14484 (17)	0.0276 (8)
H24	0.8462	1.0960	0.1552	0.033*
N3	0.6107 (3)	0.98007 (12)	0.12006 (12)	0.0188 (6)
C30	0.7076 (4)	0.95715 (17)	0.09347 (16)	0.0283 (8)
H30	0.7867	0.9630	0.1136	0.034*
C31	0.6969 (5)	0.9254 (2)	0.03793 (17)	0.0404 (11)
H31	0.7671	0.9104	0.0211	0.049*
C32	0.5798 (5)	0.91630 (19)	0.00766 (17)	0.0379 (10)
H32	0.5697	0.8953	−0.0300	0.045*
C33	0.4786 (4)	0.93884 (19)	0.03420 (17)	0.0352 (10)
H33	0.3986	0.9330	0.0150	0.042*
C34	0.4977 (4)	0.97040 (17)	0.09003 (16)	0.0254 (8)
H34	0.4287	0.9857	0.1077	0.031*
N4	0.5706 (2)	0.83412 (11)	0.16099 (11)	0.0135 (5)
C40	0.6631 (3)	0.80825 (15)	0.13249 (15)	0.0201 (7)
H40	0.7441	0.8132	0.1507	0.024*
C41	0.6439 (4)	0.77484 (18)	0.07787 (16)	0.0281 (8)
H41	0.7105	0.7570	0.0600	0.034*
C42	0.5241 (4)	0.76788 (16)	0.04954 (16)	0.0261 (8)
H42	0.5088	0.7455	0.0125	0.031*
C43	0.4283 (3)	0.79503 (16)	0.07780 (15)	0.0243 (8)
H43	0.3469	0.7915	0.0601	0.029*
C44	0.4553 (3)	0.82776 (14)	0.13311 (14)	0.0174 (7)
H44	0.3904	0.8462	0.1518	0.021*
N5	0.6445 (3)	0.91542 (11)	0.33868 (11)	0.0133 (5)
C50	0.7613 (3)	0.92810 (14)	0.36475 (14)	0.0169 (7)
H50	0.8283	0.9150	0.3443	0.020*
C51	0.7865 (4)	0.95976 (15)	0.42070 (15)	0.0240 (8)
H51	0.8686	0.9679	0.4372	0.029*
C52	0.6873 (4)	0.97887 (16)	0.45144 (16)	0.0279 (8)
H52	0.7014	1.0009	0.4887	0.033*
C53	0.5661 (4)	0.96455 (18)	0.42549 (16)	0.0301 (9)
H53	0.4976	0.9759	0.4455	0.036*
C54	0.5490 (3)	0.93309 (15)	0.36944 (15)	0.0210 (7)
H54	0.4676	0.9238	0.3523	0.025*
N6	0.5812 (3)	0.77322 (12)	0.37940 (12)	0.0183 (6)
C60	0.6886 (3)	0.79493 (15)	0.41063 (15)	0.0221 (7)
H60	0.7628	0.7904	0.3931	0.027*
C61	0.6951 (4)	0.82359 (17)	0.46723 (17)	0.0312 (9)
H61	0.7717	0.8383	0.4871	0.037*
C62	0.5861 (5)	0.83010 (19)	0.49394 (17)	0.0372 (10)
H62	0.5879	0.8489	0.5323	0.045*
C63	0.4743 (4)	0.80825 (19)	0.46270 (17)	0.0342 (9)
H63	0.3993	0.8118	0.4797	0.041*
C64	0.4756 (4)	0.78111 (17)	0.40589 (16)	0.0254 (8)
H64	0.3996	0.7676	0.3848	0.030*
N7	0.5610 (3)	0.64194 (12)	0.33681 (12)	0.0169 (6)
C70	0.6616 (3)	0.61235 (14)	0.35300 (14)	0.0176 (7)
H70	0.7388	0.6231	0.3413	0.021*
C71	0.6549 (4)	0.56678 (16)	0.38618 (15)	0.0230 (8)
H71	0.7261	0.5466	0.3958	0.028*
C72	0.5421 (4)	0.55153 (16)	0.40491 (16)	0.0281 (8)
H72	0.5361	0.5213	0.4278	0.034*
C73	0.4374 (4)	0.58179 (17)	0.38913 (18)	0.0317 (9)
H73	0.3600	0.5726	0.4015	0.038*
C74	0.4506 (3)	0.62631 (16)	0.35437 (17)	0.0247 (8)
H74	0.3801	0.6460	0.3429	0.030*
N8	0.5590 (3)	0.65853 (12)	0.20988 (12)	0.0151 (6)
C80	0.4867 (3)	0.67054 (15)	0.16423 (15)	0.0205 (7)
H80	0.4430	0.7062	0.1684	0.025*
C81	0.4740 (4)	0.63220 (17)	0.11103 (15)	0.0253 (8)
H81	0.4234	0.6424	0.0804	0.030*
C82	0.5375 (4)	0.57858 (16)	0.10415 (16)	0.0251 (8)
H82	0.5304	0.5520	0.0690	0.030*
C83	0.6204 (3)	0.60688 (15)	0.20244 (15)	0.0197 (7)
H83	0.6718	0.5980	0.2335	0.024*
C84	0.6120 (4)	0.56576 (15)	0.15116 (16)	0.0244 (8)
H84	0.6557	0.5301	0.1483	0.029*
N9	0.0908 (3)	0.58077 (12)	0.28926 (12)	0.0177 (6)
C90	0.1301 (4)	0.64008 (16)	0.29995 (17)	0.0272 (8)
H90	0.1573	0.6576	0.2697	0.033*
C91	0.1324 (4)	0.67637 (18)	0.3531 (2)	0.0372 (10)
H91	0.1582	0.7177	0.3583	0.045*
C92	0.0958 (4)	0.6504 (2)	0.3985 (2)	0.0403 (11)
H92	0.0983	0.6736	0.4352	0.048*
C93	0.0548 (4)	0.5887 (2)	0.38863 (17)	0.0357 (10)
H93	0.0292	0.5699	0.4185	0.043*
C94	0.0530 (4)	0.55635 (16)	0.33356 (15)	0.0250 (8)
H94	0.0241	0.5154	0.3268	0.030*
N10	0.0464 (3)	0.60424 (12)	0.16674 (12)	0.0181 (6)
C100	−0.0690 (3)	0.62454 (16)	0.17023 (16)	0.0238 (8)
H100	−0.1251	0.6043	0.1896	0.029*
C101	−0.1080 (4)	0.67438 (16)	0.14619 (16)	0.0286 (8)
H101	−0.1893	0.6869	0.1489	0.034*
C102	−0.0255 (4)	0.70520 (16)	0.11835 (17)	0.0308 (9)
H102	−0.0491	0.7394	0.1027	0.037*
C103	0.0931 (4)	0.68435 (17)	0.11410 (17)	0.0311 (9)
H103	0.1504	0.7040	0.0949	0.037*
C104	0.1265 (4)	0.63355 (16)	0.13878 (17)	0.0265 (8)
H104	0.2067	0.6196	0.1357	0.032*
N11	0.1078 (3)	0.47981 (12)	0.11672 (12)	0.0198 (6)
C110	0.2116 (4)	0.48432 (17)	0.08896 (16)	0.0272 (8)
H110	0.2844	0.5031	0.1098	0.033*
C111	0.2141 (4)	0.46223 (18)	0.03102 (18)	0.0354 (10)
H111	0.2873	0.4662	0.0132	0.043*
C112	0.1066 (5)	0.43401 (19)	−0.00042 (18)	0.0387 (10)
H112	0.1057	0.4194	−0.0397	0.046*
C113	0.0006 (4)	0.42797 (18)	0.02784 (17)	0.0336 (9)
H113	−0.0723	0.4082	0.0081	0.040*
C114	0.0042 (4)	0.45177 (16)	0.08590 (16)	0.0246 (8)
H114	−0.0680	0.4482	0.1044	0.029*
N12	0.1262 (3)	0.34018 (11)	0.16499 (11)	0.0142 (5)
C120	0.2300 (3)	0.34169 (15)	0.13692 (15)	0.0186 (7)
H120	0.3031	0.3611	0.1568	0.022*
C121	0.2323 (4)	0.31545 (16)	0.07961 (15)	0.0248 (8)
H121	0.3054	0.3173	0.0614	0.030*
C122	0.1235 (4)	0.28642 (18)	0.04992 (16)	0.0297 (9)
H122	0.1227	0.2674	0.0117	0.036*
C123	0.0162 (4)	0.28624 (16)	0.07824 (15)	0.0254 (8)
H123	−0.0585	0.2681	0.0589	0.031*
C124	0.0209 (3)	0.31308 (15)	0.13523 (15)	0.0190 (7)
H124	−0.0518	0.3124	0.1539	0.023*
N13	0.1375 (3)	0.40690 (11)	0.34613 (12)	0.0148 (5)
C130	0.2432 (3)	0.43372 (14)	0.37597 (15)	0.0181 (7)
H130	0.3149	0.4357	0.3568	0.022*
C131	0.2500 (3)	0.45857 (16)	0.43403 (15)	0.0232 (8)
H131	0.3246	0.4771	0.4532	0.028*
C132	0.1448 (4)	0.45545 (16)	0.46280 (15)	0.0254 (8)
H132	0.1469	0.4723	0.5016	0.030*
C133	0.0351 (3)	0.42685 (16)	0.43320 (15)	0.0233 (7)
H133	−0.0368	0.4232	0.4519	0.028*
C134	0.0358 (3)	0.40386 (14)	0.37514 (14)	0.0182 (7)
H134	−0.0380	0.3853	0.3551	0.022*
N14	0.1631 (3)	0.26328 (13)	0.38604 (12)	0.0198 (6)
C140	0.2669 (4)	0.29216 (15)	0.41598 (15)	0.0221 (7)
H140	0.3365	0.2982	0.3963	0.027*
C141	0.2748 (4)	0.31326 (17)	0.47482 (17)	0.0300 (9)
H141	0.3475	0.3337	0.4940	0.036*
C142	0.1727 (4)	0.30335 (19)	0.50437 (17)	0.0353 (10)
H142	0.1756	0.3166	0.5439	0.042*
C143	0.0659 (5)	0.27326 (19)	0.47396 (18)	0.0377 (10)
H143	−0.0039	0.2656	0.4929	0.045*
C144	0.0642 (4)	0.25485 (17)	0.41560 (17)	0.0289 (8)
H144	−0.0089	0.2356	0.3955	0.035*
N15	0.2004 (3)	0.13772 (12)	0.33321 (12)	0.0178 (6)
C150	0.3150 (3)	0.11684 (16)	0.33394 (16)	0.0232 (8)
H150	0.3755	0.1371	0.3169	0.028*
C151	0.3490 (4)	0.06649 (17)	0.35868 (17)	0.0291 (8)
H151	0.4305	0.0537	0.3589	0.035*
C152	0.2586 (4)	0.03587 (16)	0.38303 (16)	0.0292 (9)
H152	0.2777	0.0016	0.3996	0.035*
C153	0.1401 (4)	0.05685 (18)	0.38242 (18)	0.0335 (9)
H153	0.0779	0.0370	0.3988	0.040*
C154	0.1135 (4)	0.10793 (17)	0.35725 (19)	0.0315 (9)
H154	0.0328	0.1219	0.3571	0.038*
N16	0.1571 (3)	0.16418 (12)	0.21137 (12)	0.0175 (6)
C160	0.2093 (4)	0.18347 (16)	0.16753 (16)	0.0248 (8)
H160	0.2478	0.2227	0.1736	0.030*
C161	0.2084 (4)	0.14774 (18)	0.11370 (17)	0.0325 (9)
H161	0.2448	0.1629	0.0842	0.039*
C162	0.1525 (4)	0.08894 (18)	0.10426 (17)	0.0324 (9)
H162	0.1513	0.0638	0.0686	0.039*
C163	0.1019 (3)	0.10761 (15)	0.20130 (16)	0.0236 (8)
H163	0.0638	0.0938	0.2311	0.028*
C164	0.0986 (4)	0.06875 (16)	0.14916 (17)	0.0288 (9)
H164	0.0606	0.0295	0.1444	0.035*
P1	0.88486 (9)	0.13150 (4)	0.56716 (4)	0.0238 (2)
F1	1.0168 (2)	0.16826 (13)	0.58152 (12)	0.0523 (7)
F2	0.9375 (3)	0.08779 (18)	0.51542 (13)	0.0796 (12)
F3	0.9312 (3)	0.08648 (11)	0.61017 (12)	0.0461 (7)
F4	0.7521 (2)	0.09423 (10)	0.55402 (13)	0.0508 (8)
F5	0.8301 (3)	0.17430 (11)	0.61873 (10)	0.0431 (6)
F6	0.8402 (2)	0.17718 (13)	0.52466 (11)	0.0491 (7)
P2	0.65490 (9)	0.37860 (4)	0.43452 (4)	0.0265 (2)
F10	0.5672 (2)	0.42200 (12)	0.47243 (11)	0.0450 (6)
F7	0.7323 (5)	0.3402 (2)	0.3874 (2)	0.0428 (4)*	0.565 (5)
F8	0.7571 (5)	0.3747 (2)	0.4846 (2)	0.0428 (4)*	0.565 (5)
F9	0.5748 (5)	0.3199 (2)	0.4407 (2)	0.0428 (4)*	0.565 (5)
F11	0.5525 (4)	0.3899 (3)	0.38080 (19)	0.0428 (4)*	0.565 (5)
F12	0.7273 (5)	0.4414 (2)	0.4237 (2)	0.0428 (4)*	0.565 (5)
F7B	0.7569 (6)	0.3323 (3)	0.4081 (3)	0.0428 (4)*	0.435 (5)
F8B	0.7567 (6)	0.3948 (3)	0.4918 (3)	0.0428 (4)*	0.435 (5)
F9B	0.6046 (6)	0.3228 (3)	0.4667 (3)	0.0428 (4)*	0.435 (5)
F11B	0.5565 (6)	0.3590 (3)	0.3831 (3)	0.0428 (4)*	0.435 (5)
F12B	0.7173 (7)	0.4308 (3)	0.4080 (3)	0.0428 (4)*	0.435 (5)
P3	0.61714 (9)	0.37994 (4)	0.07085 (4)	0.0221 (2)
F13	0.6866 (2)	0.34074 (11)	0.02128 (10)	0.0385 (6)
F14	0.7324 (2)	0.37176 (14)	0.11620 (11)	0.0521 (7)
F15	0.5503 (2)	0.31830 (10)	0.08343 (11)	0.0376 (6)
F16	0.5471 (3)	0.41810 (11)	0.12085 (11)	0.0423 (6)
F17	0.5020 (2)	0.38578 (13)	0.02535 (10)	0.0458 (7)
F18	0.6838 (3)	0.44119 (12)	0.05854 (14)	0.0626 (9)
P4	0.06571 (9)	0.86950 (4)	0.06303 (4)	0.0223 (2)
F19	0.1253 (5)	0.8097 (2)	0.0306 (2)	0.0447 (4)*	0.600 (4)
F20	0.1049 (5)	0.8470 (2)	0.12424 (17)	0.0447 (4)*	0.600 (4)
F21	−0.0644 (4)	0.8311 (2)	0.0587 (2)	0.0447 (4)*	0.600 (4)
F22	0.0071 (5)	0.9274 (2)	0.0997 (2)	0.0447 (4)*	0.600 (4)
F23	0.0262 (5)	0.8922 (2)	0.00514 (18)	0.0447 (4)*	0.600 (4)
F24	0.1970 (4)	0.9078 (2)	0.0721 (2)	0.0447 (4)*	0.600 (4)
F19B	0.1043 (7)	0.7992 (3)	0.0442 (3)	0.0447 (4)*	0.400 (4)
F20B	0.1468 (7)	0.8674 (3)	0.1209 (2)	0.0447 (4)*	0.400 (4)
F21B	−0.0604 (6)	0.8395 (3)	0.0828 (3)	0.0447 (4)*	0.400 (4)
F22B	0.0139 (7)	0.9351 (3)	0.0789 (3)	0.0447 (4)*	0.400 (4)
F23B	−0.0120 (6)	0.8647 (3)	0.0000 (2)	0.0447 (4)*	0.400 (4)
F24B	0.1869 (6)	0.8958 (3)	0.0389 (3)	0.0447 (4)*	0.400 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0103 (2)	0.0075 (2)	0.0199 (2)	0.00214 (15)	−0.00011 (16)	0.00900 (16)
C1	0.0123 (15)	0.0108 (15)	0.0176 (16)	0.0025 (12)	−0.0017 (12)	0.0047 (12)
O1	0.0143 (11)	0.0121 (11)	0.0273 (13)	0.0030 (9)	−0.0004 (9)	0.0123 (9)
O2	0.0118 (11)	0.0086 (10)	0.0225 (12)	0.0028 (8)	0.0008 (9)	0.0077 (9)
C2	0.0115 (16)	0.0145 (16)	0.040 (2)	0.0017 (13)	−0.0004 (14)	0.0105 (14)
C3	0.0095 (15)	0.0098 (14)	0.0173 (15)	0.0011 (11)	0.0004 (12)	0.0056 (12)
O3	0.0119 (11)	0.0116 (11)	0.0305 (13)	0.0010 (9)	−0.0001 (9)	0.0108 (9)
O4	0.0100 (11)	0.0111 (11)	0.0268 (13)	−0.0006 (9)	−0.0001 (9)	0.0079 (9)
C4	0.0081 (16)	0.0181 (17)	0.041 (2)	−0.0021 (13)	−0.0038 (14)	0.0133 (15)
Co2	0.0084 (2)	0.00418 (19)	0.0163 (2)	0.00018 (15)	−0.00162 (16)	0.00532 (16)
C5	0.0093 (15)	0.0114 (14)	0.0181 (16)	0.0028 (12)	0.0021 (12)	0.0066 (12)
C6	0.0115 (16)	0.0163 (16)	0.035 (2)	−0.0009 (13)	−0.0033 (14)	0.0113 (14)
O5	0.0107 (11)	0.0102 (10)	0.0258 (12)	−0.0008 (8)	−0.0003 (9)	0.0080 (9)
O6	0.0120 (11)	0.0096 (10)	0.0299 (13)	0.0015 (9)	−0.0011 (9)	0.0086 (9)
Co3	0.0100 (2)	0.0070 (2)	0.0216 (2)	0.00147 (15)	−0.00033 (16)	0.00854 (16)
C7	0.0143 (16)	0.0100 (14)	0.0197 (16)	0.0017 (12)	−0.0013 (12)	0.0034 (12)
O7	0.0110 (11)	0.0076 (10)	0.0228 (12)	0.0032 (8)	0.0007 (9)	0.0080 (8)
O8	0.0150 (12)	0.0127 (11)	0.0309 (13)	0.0018 (9)	0.0003 (10)	0.0145 (10)
C8	0.0126 (16)	0.0131 (15)	0.034 (2)	0.0005 (12)	−0.0005 (14)	0.0095 (14)
Co4	0.0126 (2)	0.0085 (2)	0.0217 (2)	0.00040 (16)	−0.00088 (17)	0.00924 (16)
C1B	0.0120 (15)	0.0082 (14)	0.0176 (16)	0.0011 (11)	−0.0025 (12)	0.0019 (12)
O9	0.0160 (12)	0.0139 (11)	0.0276 (13)	−0.0005 (9)	−0.0006 (10)	0.0131 (9)
O10	0.0094 (11)	0.0116 (11)	0.0308 (13)	0.0035 (9)	−0.0004 (9)	0.0092 (9)
C2B	0.0149 (17)	0.0167 (16)	0.0316 (19)	0.0038 (13)	0.0033 (14)	0.0091 (14)
C3B	0.0146 (16)	0.0105 (14)	0.0179 (16)	−0.0009 (12)	−0.0002 (12)	0.0028 (12)
O11	0.0184 (12)	0.0124 (11)	0.0311 (13)	−0.0009 (9)	0.0004 (10)	0.0133 (10)
O12	0.0109 (11)	0.0076 (10)	0.0236 (12)	0.0003 (8)	0.0004 (9)	0.0066 (8)
Co5	0.0086 (2)	0.00394 (19)	0.0184 (2)	0.00091 (15)	−0.00121 (16)	0.00565 (16)
C4B	0.0137 (16)	0.0142 (15)	0.0263 (18)	0.0010 (12)	−0.0008 (13)	0.0064 (13)
C5B	0.0128 (15)	0.0103 (14)	0.0157 (15)	−0.0017 (12)	−0.0007 (12)	0.0041 (12)
O13	0.0089 (11)	0.0118 (10)	0.0281 (13)	0.0048 (8)	0.0007 (9)	0.0080 (9)
O14	0.0149 (12)	0.0118 (11)	0.0320 (13)	0.0004 (9)	0.0008 (10)	0.0120 (10)
C6B	0.0126 (16)	0.0159 (16)	0.034 (2)	0.0029 (13)	0.0034 (14)	0.0113 (14)
C7B	0.0139 (16)	0.0092 (14)	0.0190 (16)	−0.0002 (12)	0.0006 (12)	0.0048 (12)
O15	0.0111 (11)	0.0070 (10)	0.0238 (12)	−0.0009 (8)	−0.0015 (9)	0.0082 (9)
O16	0.0151 (12)	0.0114 (11)	0.0300 (13)	−0.0004 (9)	0.0015 (10)	0.0110 (9)
C8B	0.0124 (16)	0.0164 (16)	0.0316 (19)	−0.0008 (13)	0.0008 (14)	0.0090 (14)
Co6	0.0128 (2)	0.0071 (2)	0.0226 (2)	0.00051 (16)	−0.00019 (17)	0.00901 (17)
N1	0.0162 (14)	0.0117 (13)	0.0206 (14)	−0.0009 (11)	−0.0004 (11)	0.0090 (11)
C10	0.0234 (18)	0.0178 (16)	0.0252 (18)	0.0051 (14)	−0.0023 (14)	0.0113 (14)
C11	0.030 (2)	0.0273 (19)	0.0230 (19)	0.0028 (16)	−0.0055 (15)	0.0101 (15)
C12	0.0264 (19)	0.0205 (17)	0.0212 (18)	−0.0041 (14)	0.0005 (14)	0.0040 (14)
C13	0.029 (2)	0.0142 (16)	0.0267 (19)	0.0046 (14)	0.0024 (15)	0.0087 (14)
C14	0.0178 (17)	0.0145 (15)	0.0223 (17)	0.0031 (13)	−0.0022 (13)	0.0092 (13)
N2	0.0198 (15)	0.0124 (13)	0.0226 (15)	−0.0009 (11)	0.0015 (11)	0.0093 (11)
C20	0.0192 (17)	0.0155 (16)	0.0254 (18)	0.0016 (13)	−0.0019 (14)	0.0137 (13)
C21	0.029 (2)	0.0174 (17)	0.0274 (19)	0.0034 (15)	−0.0028 (15)	0.0131 (14)
C22	0.040 (2)	0.0193 (18)	0.035 (2)	−0.0004 (16)	0.0073 (18)	0.0196 (16)
C23	0.035 (2)	0.027 (2)	0.053 (3)	0.0048 (17)	0.020 (2)	0.0248 (19)
C24	0.0224 (19)	0.0216 (18)	0.045 (2)	0.0038 (15)	0.0075 (16)	0.0206 (16)
N3	0.0244 (16)	0.0116 (13)	0.0218 (15)	0.0005 (11)	−0.0006 (12)	0.0084 (11)
C30	0.032 (2)	0.031 (2)	0.0244 (19)	0.0138 (17)	0.0014 (16)	0.0102 (16)
C31	0.053 (3)	0.045 (3)	0.025 (2)	0.028 (2)	0.0049 (19)	0.0082 (18)
C32	0.059 (3)	0.029 (2)	0.024 (2)	0.008 (2)	−0.0022 (19)	−0.0004 (16)
C33	0.041 (2)	0.035 (2)	0.027 (2)	−0.0124 (19)	−0.0113 (18)	0.0092 (17)
C34	0.026 (2)	0.0264 (19)	0.0241 (19)	−0.0040 (15)	0.0007 (15)	0.0080 (15)
N4	0.0140 (13)	0.0077 (12)	0.0192 (14)	0.0000 (10)	−0.0018 (11)	0.0059 (10)
C40	0.0147 (17)	0.0191 (17)	0.0254 (18)	−0.0003 (13)	−0.0008 (13)	0.0023 (14)
C41	0.027 (2)	0.029 (2)	0.027 (2)	0.0062 (16)	0.0011 (15)	−0.0004 (15)
C42	0.035 (2)	0.0205 (18)	0.0211 (18)	−0.0019 (15)	−0.0038 (15)	0.0011 (14)
C43	0.0229 (19)	0.0238 (18)	0.0246 (19)	−0.0022 (15)	−0.0107 (15)	0.0072 (14)
C44	0.0164 (16)	0.0143 (15)	0.0226 (17)	0.0040 (13)	−0.0009 (13)	0.0077 (13)
N5	0.0163 (14)	0.0064 (12)	0.0174 (14)	0.0031 (10)	−0.0041 (11)	0.0049 (10)
C50	0.0156 (16)	0.0133 (15)	0.0222 (17)	−0.0006 (12)	−0.0040 (13)	0.0072 (13)
C51	0.027 (2)	0.0175 (17)	0.0258 (19)	−0.0049 (14)	−0.0122 (15)	0.0089 (14)
C52	0.044 (2)	0.0205 (18)	0.0178 (18)	0.0053 (16)	−0.0034 (16)	0.0005 (14)
C53	0.029 (2)	0.034 (2)	0.026 (2)	0.0141 (17)	−0.0013 (16)	0.0009 (16)
C54	0.0197 (18)	0.0208 (17)	0.0222 (18)	0.0080 (14)	−0.0035 (14)	0.0044 (14)
N6	0.0200 (15)	0.0123 (13)	0.0241 (15)	0.0005 (11)	0.0015 (12)	0.0078 (11)
C60	0.0238 (19)	0.0161 (16)	0.0268 (19)	−0.0023 (14)	−0.0004 (14)	0.0070 (14)
C61	0.038 (2)	0.0226 (19)	0.031 (2)	−0.0027 (17)	−0.0091 (17)	0.0063 (16)
C62	0.059 (3)	0.030 (2)	0.023 (2)	0.010 (2)	−0.0003 (19)	0.0026 (16)
C63	0.038 (2)	0.036 (2)	0.033 (2)	0.0111 (18)	0.0107 (18)	0.0096 (17)
C64	0.0223 (19)	0.0281 (19)	0.0274 (19)	0.0050 (15)	0.0035 (15)	0.0081 (15)
N7	0.0195 (15)	0.0115 (13)	0.0217 (14)	0.0002 (11)	−0.0002 (11)	0.0099 (11)
C70	0.0187 (17)	0.0113 (15)	0.0242 (17)	0.0005 (12)	−0.0030 (13)	0.0100 (13)
C71	0.029 (2)	0.0172 (17)	0.0240 (18)	0.0027 (14)	−0.0038 (15)	0.0099 (14)
C72	0.041 (2)	0.0188 (18)	0.029 (2)	−0.0014 (16)	0.0057 (17)	0.0163 (15)
C73	0.032 (2)	0.0223 (19)	0.048 (2)	0.0020 (16)	0.0169 (18)	0.0182 (17)
C74	0.0211 (18)	0.0173 (17)	0.040 (2)	0.0048 (14)	0.0071 (16)	0.0147 (15)
N8	0.0143 (14)	0.0114 (13)	0.0207 (14)	−0.0009 (10)	−0.0002 (11)	0.0079 (11)
C80	0.0206 (18)	0.0174 (16)	0.0254 (18)	0.0054 (14)	−0.0011 (14)	0.0098 (14)
C81	0.027 (2)	0.0285 (19)	0.0207 (18)	0.0011 (15)	−0.0039 (15)	0.0078 (15)
C82	0.032 (2)	0.0173 (17)	0.0242 (19)	−0.0066 (15)	0.0035 (15)	−0.0001 (14)
C83	0.0213 (18)	0.0132 (16)	0.0255 (18)	0.0033 (13)	−0.0011 (14)	0.0075 (13)
C84	0.035 (2)	0.0110 (16)	0.0287 (19)	0.0035 (14)	0.0059 (16)	0.0043 (14)
N9	0.0175 (14)	0.0114 (13)	0.0241 (15)	0.0032 (11)	−0.0032 (11)	0.0051 (11)
C90	0.030 (2)	0.0140 (17)	0.037 (2)	−0.0017 (15)	−0.0087 (16)	0.0078 (15)
C91	0.039 (2)	0.0169 (18)	0.050 (3)	0.0075 (17)	−0.012 (2)	−0.0045 (17)
C92	0.040 (3)	0.034 (2)	0.041 (2)	0.0142 (19)	−0.001 (2)	−0.0135 (19)
C93	0.044 (3)	0.038 (2)	0.026 (2)	0.0056 (19)	0.0035 (18)	0.0059 (17)
C94	0.031 (2)	0.0180 (17)	0.0268 (19)	0.0019 (15)	−0.0005 (15)	0.0063 (14)
N10	0.0224 (15)	0.0095 (13)	0.0245 (15)	0.0015 (11)	−0.0019 (12)	0.0114 (11)
C100	0.0251 (19)	0.0205 (17)	0.0285 (19)	0.0076 (15)	0.0016 (15)	0.0113 (15)
C101	0.035 (2)	0.0198 (18)	0.034 (2)	0.0114 (16)	−0.0017 (17)	0.0137 (15)
C102	0.049 (3)	0.0140 (17)	0.030 (2)	0.0043 (16)	−0.0088 (18)	0.0117 (15)
C103	0.042 (2)	0.0198 (18)	0.035 (2)	−0.0065 (17)	0.0005 (18)	0.0174 (16)
C104	0.0246 (19)	0.0185 (17)	0.039 (2)	−0.0028 (15)	0.0002 (16)	0.0154 (16)
N11	0.0252 (16)	0.0139 (13)	0.0227 (15)	0.0015 (12)	0.0015 (12)	0.0106 (11)
C110	0.030 (2)	0.0243 (19)	0.031 (2)	0.0003 (16)	0.0078 (16)	0.0119 (15)
C111	0.048 (3)	0.029 (2)	0.034 (2)	0.0061 (19)	0.0173 (19)	0.0107 (17)
C112	0.061 (3)	0.030 (2)	0.026 (2)	0.005 (2)	0.006 (2)	0.0050 (17)
C113	0.046 (3)	0.024 (2)	0.030 (2)	−0.0018 (18)	−0.0057 (18)	0.0053 (16)
C114	0.030 (2)	0.0177 (17)	0.0263 (19)	0.0014 (15)	−0.0011 (15)	0.0058 (14)
N12	0.0159 (14)	0.0082 (12)	0.0186 (14)	0.0006 (10)	0.0002 (11)	0.0038 (10)
C120	0.0178 (17)	0.0159 (16)	0.0235 (18)	−0.0006 (13)	0.0016 (13)	0.0079 (13)
C121	0.0254 (19)	0.0260 (19)	0.0252 (19)	0.0008 (15)	0.0074 (15)	0.0085 (15)
C122	0.041 (2)	0.027 (2)	0.0195 (18)	−0.0039 (17)	0.0037 (16)	0.0020 (15)
C123	0.031 (2)	0.0201 (17)	0.0234 (19)	−0.0091 (15)	−0.0046 (15)	0.0040 (14)
C124	0.0186 (17)	0.0162 (16)	0.0224 (17)	−0.0047 (13)	−0.0007 (13)	0.0068 (13)
N13	0.0169 (14)	0.0069 (12)	0.0209 (14)	0.0004 (10)	0.0002 (11)	0.0041 (10)
C130	0.0163 (17)	0.0133 (15)	0.0253 (18)	−0.0020 (13)	−0.0017 (13)	0.0077 (13)
C131	0.0233 (19)	0.0184 (17)	0.0274 (19)	−0.0046 (14)	−0.0060 (15)	0.0081 (14)
C132	0.036 (2)	0.0202 (17)	0.0194 (18)	−0.0010 (15)	0.0008 (15)	0.0029 (14)
C133	0.0234 (19)	0.0220 (18)	0.0255 (19)	0.0013 (14)	0.0063 (15)	0.0046 (14)
C134	0.0166 (17)	0.0141 (15)	0.0245 (18)	0.0001 (13)	0.0008 (13)	0.0054 (13)
N14	0.0235 (16)	0.0137 (13)	0.0237 (15)	0.0006 (11)	0.0005 (12)	0.0090 (11)
C140	0.0276 (19)	0.0124 (16)	0.0270 (19)	0.0009 (14)	−0.0032 (15)	0.0085 (13)
C141	0.037 (2)	0.0208 (18)	0.031 (2)	−0.0007 (16)	−0.0088 (17)	0.0063 (15)
C142	0.050 (3)	0.031 (2)	0.024 (2)	0.0021 (19)	−0.0001 (18)	0.0039 (16)
C143	0.051 (3)	0.032 (2)	0.032 (2)	−0.003 (2)	0.014 (2)	0.0037 (17)
C144	0.033 (2)	0.0243 (19)	0.031 (2)	−0.0048 (16)	0.0054 (17)	0.0096 (16)
N15	0.0216 (15)	0.0104 (13)	0.0239 (15)	0.0017 (11)	0.0012 (12)	0.0110 (11)
C150	0.0249 (19)	0.0170 (17)	0.030 (2)	0.0059 (14)	0.0017 (15)	0.0108 (14)
C151	0.033 (2)	0.0220 (18)	0.035 (2)	0.0099 (16)	−0.0003 (17)	0.0134 (16)
C152	0.049 (3)	0.0171 (17)	0.0242 (19)	0.0082 (17)	−0.0033 (17)	0.0143 (15)
C153	0.043 (2)	0.0216 (19)	0.044 (2)	0.0022 (17)	0.0137 (19)	0.0236 (17)
C154	0.025 (2)	0.0242 (19)	0.053 (3)	0.0065 (16)	0.0095 (18)	0.0249 (18)
N16	0.0170 (14)	0.0107 (13)	0.0257 (15)	0.0025 (11)	−0.0021 (11)	0.0075 (11)
C160	0.028 (2)	0.0175 (17)	0.031 (2)	0.0003 (15)	0.0010 (16)	0.0093 (15)
C161	0.043 (2)	0.030 (2)	0.026 (2)	0.0016 (18)	0.0058 (17)	0.0078 (16)
C162	0.041 (2)	0.026 (2)	0.029 (2)	0.0076 (17)	−0.0043 (18)	0.0011 (16)
C163	0.0270 (19)	0.0137 (16)	0.031 (2)	−0.0022 (14)	−0.0024 (15)	0.0085 (14)
C164	0.037 (2)	0.0133 (17)	0.034 (2)	−0.0002 (15)	−0.0102 (17)	0.0029 (15)
P1	0.0272 (5)	0.0186 (4)	0.0237 (5)	0.0019 (4)	−0.0075 (4)	0.0030 (4)
F1	0.0328 (14)	0.0671 (18)	0.0595 (17)	−0.0170 (13)	−0.0141 (12)	0.0320 (15)
F2	0.070 (2)	0.113 (3)	0.0451 (17)	0.057 (2)	−0.0120 (15)	−0.0227 (18)
F3	0.0456 (16)	0.0345 (13)	0.0606 (17)	0.0053 (12)	−0.0128 (13)	0.0237 (12)
F4	0.0385 (15)	0.0222 (12)	0.084 (2)	−0.0087 (11)	−0.0259 (14)	0.0034 (12)
F5	0.0581 (17)	0.0325 (13)	0.0373 (14)	0.0114 (12)	0.0052 (12)	−0.0009 (11)
F6	0.0383 (15)	0.0687 (18)	0.0493 (16)	0.0053 (13)	−0.0037 (12)	0.0399 (14)
P2	0.0267 (5)	0.0211 (5)	0.0292 (5)	−0.0039 (4)	0.0029 (4)	−0.0022 (4)
F10	0.0461 (16)	0.0439 (15)	0.0477 (15)	0.0156 (12)	0.0144 (12)	0.0073 (12)
P3	0.0276 (5)	0.0140 (4)	0.0243 (5)	−0.0012 (4)	0.0008 (4)	0.0030 (3)
F13	0.0341 (13)	0.0411 (14)	0.0373 (13)	0.0107 (11)	0.0034 (11)	−0.0047 (11)
F14	0.0348 (15)	0.075 (2)	0.0396 (15)	−0.0048 (14)	−0.0139 (12)	0.0006 (13)
F15	0.0386 (14)	0.0213 (11)	0.0548 (15)	−0.0028 (10)	0.0002 (11)	0.0152 (10)
F16	0.0551 (17)	0.0303 (13)	0.0400 (14)	0.0007 (12)	0.0174 (12)	−0.0052 (10)
F17	0.0451 (15)	0.0664 (18)	0.0325 (13)	0.0304 (14)	0.0025 (11)	0.0220 (12)
F18	0.078 (2)	0.0277 (14)	0.089 (2)	−0.0079 (14)	0.0428 (18)	0.0141 (14)
P4	0.0216 (5)	0.0177 (4)	0.0272 (5)	0.0021 (4)	−0.0032 (4)	0.0049 (4)

Geometric parameters (Å, º) top

Co1—O3	2.016 (2)	C62—H62	0.9300
Co1—N2	2.112 (3)	C63—C64	1.379 (5)
Co1—O1	2.125 (2)	C63—H63	0.9300
Co1—N1	2.183 (3)	C64—H64	0.9300
Co1—N3	2.185 (3)	N7—C74	1.341 (5)
Co1—O2	2.203 (2)	N7—C70	1.343 (4)
Co1—C1	2.513 (3)	C70—C71	1.377 (5)
C1—O1	1.264 (4)	C70—H70	0.9300
C1—O2	1.277 (4)	C71—C72	1.374 (5)
C1—C2	1.494 (4)	C71—H71	0.9300
O2—Co2	2.154 (2)	C72—C73	1.385 (5)
C2—H2A	0.9600	C72—H72	0.9300
C2—H2B	0.9600	C73—C74	1.392 (5)
C2—H2C	0.9600	C73—H73	0.9300
C3—O4	1.248 (4)	C74—H74	0.9300
C3—O3	1.272 (4)	N8—C83	1.336 (4)
C3—C4	1.499 (4)	N8—C80	1.341 (4)
O4—Co2	2.057 (2)	C80—C81	1.389 (5)
C4—H4A	0.9600	C80—H80	0.9300
C4—H4B	0.9600	C81—C82	1.385 (5)
C4—H4C	0.9600	C81—H81	0.9300
Co2—O5	2.060 (2)	C82—C84	1.385 (5)
Co2—O7	2.134 (2)	C82—H82	0.9300
Co2—N5	2.139 (3)	C83—C84	1.385 (5)
Co2—N4	2.140 (3)	C83—H83	0.9300
C5—O5	1.253 (4)	C84—H84	0.9300
C5—O6	1.264 (4)	N9—C94	1.338 (5)
C5—C6	1.510 (4)	N9—C90	1.339 (4)
C6—H6A	0.9600	C90—C91	1.373 (6)
C6—H6B	0.9600	C90—H90	0.9300
C6—H6C	0.9600	C91—C92	1.376 (7)
O6—Co3	2.014 (2)	C91—H91	0.9300
Co3—N7	2.119 (3)	C92—C93	1.394 (6)
Co3—O8	2.138 (2)	C92—H92	0.9300
Co3—N8	2.178 (3)	C93—C94	1.377 (5)
Co3—N6	2.183 (3)	C93—H93	0.9300
Co3—O7	2.199 (2)	C94—H94	0.9300
C7—O8	1.257 (4)	N10—C104	1.338 (5)
C7—O7	1.286 (4)	N10—C100	1.339 (5)
C7—C8	1.497 (4)	C100—C101	1.383 (5)
C8—H8A	0.9600	C100—H100	0.9300
C8—H8B	0.9600	C101—C102	1.372 (6)
C8—H8C	0.9600	C101—H101	0.9300
Co4—O9	2.019 (2)	C102—C103	1.377 (6)
Co4—O11	2.119 (2)	C102—H102	0.9300
Co4—N10	2.120 (3)	C103—C104	1.393 (5)
Co4—N11	2.163 (3)	C103—H103	0.9300
Co4—N9	2.179 (3)	C104—H104	0.9300
Co4—O12	2.193 (2)	N11—C114	1.345 (5)
Co4—C3B	2.509 (3)	N11—C110	1.350 (5)
C1B—O10	1.256 (4)	C110—C111	1.379 (5)
C1B—O9	1.262 (4)	C110—H110	0.9300
C1B—C2B	1.507 (4)	C111—C112	1.385 (6)
O10—Co5	2.053 (2)	C111—H111	0.9300
C2B—H2B1	0.9600	C112—C113	1.381 (6)
C2B—H2B2	0.9600	C112—H112	0.9300
C2B—H2B3	0.9600	C113—C114	1.383 (5)
C3B—O11	1.262 (4)	C113—H113	0.9300
C3B—O12	1.278 (4)	C114—H114	0.9300
C3B—C4B	1.496 (4)	N12—C124	1.342 (4)
O12—Co5	2.144 (2)	N12—C120	1.347 (4)
Co5—O13	2.054 (2)	C120—C121	1.385 (5)
Co5—N12	2.137 (3)	C120—H120	0.9300
Co5—N13	2.144 (3)	C121—C122	1.386 (5)
Co5—O15	2.145 (2)	C121—H121	0.9300
C4B—H4B1	0.9600	C122—C123	1.381 (6)
C4B—H4B2	0.9600	C122—H122	0.9300
C4B—H4B3	0.9600	C123—C124	1.375 (5)
C5B—O13	1.245 (4)	C123—H123	0.9300
C5B—O14	1.269 (4)	C124—H124	0.9300
C5B—C6B	1.507 (4)	N13—C134	1.344 (4)
O14—Co6	2.026 (2)	N13—C130	1.344 (4)
C6B—H6B1	0.9600	C130—C131	1.386 (5)
C6B—H6B2	0.9600	C130—H130	0.9300
C6B—H6B3	0.9600	C131—C132	1.373 (5)
C7B—O16	1.252 (4)	C131—H131	0.9300
C7B—O15	1.282 (4)	C132—C133	1.388 (5)
C7B—C8B	1.503 (4)	C132—H132	0.9300
C7B—Co6	2.501 (3)	C133—C134	1.383 (5)
O15—Co6	2.183 (2)	C133—H133	0.9300
O16—Co6	2.129 (2)	C134—H134	0.9300
C8B—H8B1	0.9600	N14—C144	1.344 (5)
C8B—H8B2	0.9600	N14—C140	1.345 (5)
C8B—H8B3	0.9600	C140—C141	1.386 (5)
Co6—N15	2.122 (3)	C140—H140	0.9300
Co6—N14	2.161 (3)	C141—C142	1.378 (6)
Co6—N16	2.182 (3)	C141—H141	0.9300
N1—C14	1.332 (4)	C142—C143	1.384 (6)
N1—C10	1.345 (4)	C142—H142	0.9300
C10—C11	1.386 (5)	C143—C144	1.370 (6)
C10—H10	0.9300	C143—H143	0.9300
C11—C12	1.381 (5)	C144—H144	0.9300
C11—H11	0.9300	N15—C150	1.331 (5)
C12—C13	1.381 (5)	N15—C154	1.339 (5)
C12—H12	0.9300	C150—C151	1.386 (5)
C13—C14	1.390 (5)	C150—H150	0.9300
C13—H13	0.9300	C151—C152	1.380 (6)
C14—H14	0.9300	C151—H151	0.9300
N2—C24	1.335 (5)	C152—C153	1.371 (6)
N2—C20	1.345 (4)	C152—H152	0.9300
C20—C21	1.379 (5)	C153—C154	1.388 (5)
C20—H20	0.9300	C153—H153	0.9300
C21—C22	1.389 (6)	C154—H154	0.9300
C21—H21	0.9300	N16—C160	1.339 (5)
C22—C23	1.380 (6)	N16—C163	1.340 (4)
C22—H22	0.9300	C160—C161	1.382 (5)
C23—C24	1.385 (5)	C160—H160	0.9300
C23—H23	0.9300	C161—C162	1.387 (6)
C24—H24	0.9300	C161—H161	0.9300
N3—C30	1.337 (5)	C162—C164	1.378 (6)
N3—C34	1.342 (5)	C162—H162	0.9300
C30—C31	1.376 (5)	C163—C164	1.379 (5)
C30—H30	0.9300	C163—H163	0.9300
C31—C32	1.381 (6)	C164—H164	0.9300
C31—H31	0.9300	P1—F5	1.587 (2)
C32—C33	1.371 (6)	P1—F1	1.587 (3)
C32—H32	0.9300	P1—F2	1.589 (3)
C33—C34	1.382 (5)	P1—F6	1.595 (2)
C33—H33	0.9300	P1—F3	1.597 (2)
C34—H34	0.9300	P1—F4	1.598 (3)
N4—C44	1.341 (4)	P2—F11B	1.533 (6)
N4—C40	1.342 (4)	P2—F8	1.557 (4)
C40—C41	1.372 (5)	P2—F12B	1.557 (7)
C40—H40	0.9300	P2—F9	1.564 (4)
C41—C42	1.388 (5)	P2—F10	1.596 (2)
C41—H41	0.9300	P2—F7	1.600 (4)
C42—C43	1.379 (5)	P2—F7B	1.624 (5)
C42—H42	0.9300	P2—F12	1.632 (5)
C43—C44	1.387 (5)	P2—F8B	1.645 (5)
C43—H43	0.9300	P2—F9B	1.649 (5)
C44—H44	0.9300	P2—F11	1.662 (4)
N5—C54	1.342 (4)	P3—F18	1.588 (3)
N5—C50	1.346 (4)	P3—F17	1.589 (3)
C50—C51	1.389 (5)	P3—F13	1.597 (2)
C50—H50	0.9300	P3—F16	1.598 (2)
C51—C52	1.381 (6)	P3—F15	1.599 (2)
C51—H51	0.9300	P3—F14	1.600 (3)
C52—C53	1.391 (6)	P4—F23	1.562 (4)
C52—H52	0.9300	P4—F20B	1.564 (5)
C53—C54	1.385 (5)	P4—F22B	1.574 (5)
C53—H53	0.9300	P4—F24B	1.592 (5)
C54—H54	0.9300	P4—F21	1.593 (4)
N6—C60	1.341 (4)	P4—F24	1.596 (4)
N6—C64	1.345 (5)	P4—F19	1.602 (4)
C60—C61	1.377 (5)	P4—F22	1.608 (4)
C60—H60	0.9300	P4—F21B	1.623 (5)
C61—C62	1.378 (6)	P4—F19B	1.627 (5)
C61—H61	0.9300	P4—F23B	1.627 (5)
C62—C63	1.380 (6)	P4—F20	1.631 (4)

O3—Co1—N2	102.10 (10)	C51—C52—H52	120.7
O3—Co1—O1	160.92 (9)	C53—C52—H52	120.7
N2—Co1—O1	96.73 (10)	C54—C53—C52	119.1 (4)
O3—Co1—N1	88.61 (10)	C54—C53—H53	120.5
N2—Co1—N1	90.96 (10)	C52—C53—H53	120.5
O1—Co1—N1	88.01 (10)	N5—C54—C53	122.9 (3)
O3—Co1—N3	92.98 (10)	N5—C54—H54	118.5
N2—Co1—N3	85.05 (10)	C53—C54—H54	118.5
O1—Co1—N3	91.68 (10)	C60—N6—C64	116.7 (3)
N1—Co1—N3	175.94 (10)	C60—N6—Co3	122.9 (2)
O3—Co1—O2	101.10 (8)	C64—N6—Co3	120.1 (2)
N2—Co1—O2	155.93 (10)	N6—C60—C61	123.5 (4)
O1—Co1—O2	60.63 (8)	N6—C60—H60	118.2
N1—Co1—O2	95.94 (9)	C61—C60—H60	118.2
N3—Co1—O2	87.43 (9)	C60—C61—C62	118.9 (4)
O3—Co1—C1	131.56 (9)	C60—C61—H61	120.5
N2—Co1—C1	126.19 (11)	C62—C61—H61	120.5
O1—Co1—C1	30.18 (9)	C61—C62—C63	118.7 (4)
N1—Co1—C1	93.66 (10)	C61—C62—H62	120.7
N3—Co1—C1	88.09 (11)	C63—C62—H62	120.7
O2—Co1—C1	30.52 (9)	C64—C63—C62	118.8 (4)
O1—C1—O2	118.7 (3)	C64—C63—H63	120.6
O1—C1—C2	119.9 (3)	C62—C63—H63	120.6
O2—C1—C2	121.4 (3)	N6—C64—C63	123.4 (4)
O1—C1—Co1	57.65 (16)	N6—C64—H64	118.3
O2—C1—Co1	61.20 (16)	C63—C64—H64	118.3
C2—C1—Co1	174.2 (2)	C74—N7—C70	118.0 (3)
C1—O1—Co1	92.17 (18)	C74—N7—Co3	119.2 (2)
C1—O2—Co2	147.3 (2)	C70—N7—Co3	122.5 (2)
C1—O2—Co1	88.28 (18)	N7—C70—C71	122.7 (3)
Co2—O2—Co1	122.57 (10)	N7—C70—H70	118.7
C1—C2—H2A	109.5	C71—C70—H70	118.7
C1—C2—H2B	109.5	C72—C71—C70	119.3 (3)
H2A—C2—H2B	109.5	C72—C71—H71	120.4
C1—C2—H2C	109.5	C70—C71—H71	120.4
H2A—C2—H2C	109.5	C71—C72—C73	119.0 (3)
H2B—C2—H2C	109.5	C71—C72—H72	120.5
O4—C3—O3	125.2 (3)	C73—C72—H72	120.5
O4—C3—C4	118.3 (3)	C72—C73—C74	118.5 (4)
O3—C3—C4	116.5 (3)	C72—C73—H73	120.8
C3—O3—Co1	128.7 (2)	C74—C73—H73	120.8
C3—O4—Co2	149.2 (2)	N7—C74—C73	122.6 (3)
C3—C4—H4A	109.5	N7—C74—H74	118.7
C3—C4—H4B	109.5	C73—C74—H74	118.7
H4A—C4—H4B	109.5	C83—N8—C80	116.9 (3)
C3—C4—H4C	109.5	C83—N8—Co3	120.5 (2)
H4A—C4—H4C	109.5	C80—N8—Co3	122.6 (2)
H4B—C4—H4C	109.5	N8—C80—C81	123.1 (3)
O4—Co2—O5	179.18 (9)	N8—C80—H80	118.4
O4—Co2—O7	91.29 (8)	C81—C80—H80	118.4
O5—Co2—O7	89.02 (8)	C82—C81—C80	119.3 (3)
O4—Co2—N5	90.20 (10)	C82—C81—H81	120.4
O5—Co2—N5	90.55 (10)	C80—C81—H81	120.4
O7—Co2—N5	91.66 (9)	C84—C82—C81	117.9 (3)
O4—Co2—N4	90.06 (10)	C84—C82—H82	121.0
O5—Co2—N4	89.19 (10)	C81—C82—H82	121.0
O7—Co2—N4	87.41 (9)	N8—C83—C84	123.8 (3)
N5—Co2—N4	179.04 (9)	N8—C83—H83	118.1
O4—Co2—O2	88.54 (8)	C84—C83—H83	118.1
O5—Co2—O2	91.17 (8)	C82—C84—C83	119.0 (3)
O7—Co2—O2	178.77 (8)	C82—C84—H84	120.5
N5—Co2—O2	87.13 (9)	C83—C84—H84	120.5
N4—Co2—O2	93.81 (9)	C94—N9—C90	117.1 (3)
O5—C5—O6	125.6 (3)	C94—N9—Co4	122.2 (2)
O5—C5—C6	117.6 (3)	C90—N9—Co4	120.7 (3)
O6—C5—C6	116.8 (3)	N9—C90—C91	123.6 (4)
C5—C6—H6A	109.5	N9—C90—H90	118.2
C5—C6—H6B	109.5	C91—C90—H90	118.2
H6A—C6—H6B	109.5	C90—C91—C92	118.7 (4)
C5—C6—H6C	109.5	C90—C91—H91	120.7
H6A—C6—H6C	109.5	C92—C91—H91	120.7
H6B—C6—H6C	109.5	C91—C92—C93	118.9 (4)
C5—O5—Co2	146.7 (2)	C91—C92—H92	120.6
C5—O6—Co3	128.4 (2)	C93—C92—H92	120.6
O6—Co3—N7	107.47 (10)	C94—C93—C92	118.3 (4)
O6—Co3—O8	160.29 (9)	C94—C93—H93	120.8
N7—Co3—O8	91.90 (10)	C92—C93—H93	120.9
O6—Co3—N8	88.16 (10)	N9—C94—C93	123.4 (3)
N7—Co3—N8	91.41 (10)	N9—C94—H94	118.3
O8—Co3—N8	87.75 (10)	C93—C94—H94	118.3
O6—Co3—N6	90.64 (10)	C104—N10—C100	118.3 (3)
N7—Co3—N6	85.04 (10)	C104—N10—Co4	121.9 (2)
O8—Co3—N6	94.72 (10)	C100—N10—Co4	119.7 (2)
N8—Co3—N6	175.73 (10)	N10—C100—C101	122.6 (4)
O6—Co3—O7	100.76 (8)	N10—C100—H100	118.7
N7—Co3—O7	151.33 (10)	C101—C100—H100	118.7
O8—Co3—O7	60.39 (8)	C102—C101—C100	119.3 (4)
N8—Co3—O7	94.45 (9)	C102—C101—H101	120.4
N6—Co3—O7	89.81 (9)	C100—C101—H101	120.4
O8—C7—O7	118.2 (3)	C101—C102—C103	118.6 (3)
O8—C7—C8	120.4 (3)	C101—C102—H102	120.7
O7—C7—C8	121.4 (3)	C103—C102—H102	120.7
C7—O7—Co2	146.7 (2)	C102—C103—C104	119.5 (4)
C7—O7—Co3	88.92 (18)	C102—C103—H103	120.3
Co2—O7—Co3	122.52 (10)	C104—C103—H103	120.3
C7—O8—Co3	92.45 (19)	N10—C104—C103	121.8 (4)
C7—C8—H8A	109.5	N10—C104—H104	119.1
C7—C8—H8B	109.5	C103—C104—H104	119.1
H8A—C8—H8B	109.5	C114—N11—C110	117.6 (3)
C7—C8—H8C	109.5	C114—N11—Co4	119.6 (2)
H8A—C8—H8C	109.5	C110—N11—Co4	122.2 (2)
H8B—C8—H8C	109.5	N11—C110—C111	122.7 (4)
O9—Co4—O11	162.22 (9)	N11—C110—H110	118.7
O9—Co4—N10	97.29 (10)	C111—C110—H110	118.7
O11—Co4—N10	100.03 (10)	C110—C111—C112	119.3 (4)
O9—Co4—N11	95.05 (10)	C110—C111—H111	120.4
O11—Co4—N11	89.96 (10)	C112—C111—H111	120.4
N10—Co4—N11	86.60 (11)	C113—C112—C111	118.5 (4)
O9—Co4—N9	88.22 (10)	C113—C112—H112	120.7
O11—Co4—N9	88.00 (10)	C111—C112—H112	120.7
N10—Co4—N9	89.34 (10)	C112—C113—C114	119.1 (4)
N11—Co4—N9	175.08 (10)	C112—C113—H113	120.4
O9—Co4—O12	101.79 (8)	C114—C113—H113	120.4
O11—Co4—O12	60.79 (8)	N11—C114—C113	122.8 (4)
N10—Co4—O12	160.80 (10)	N11—C114—H114	118.6
N11—Co4—O12	93.71 (9)	C113—C114—H114	118.6
N9—Co4—O12	89.20 (9)	C124—N12—C120	117.8 (3)
O9—Co4—C3B	132.38 (9)	C124—N12—Co5	120.7 (2)
O11—Co4—C3B	30.18 (9)	C120—N12—Co5	121.4 (2)
N10—Co4—C3B	130.21 (11)	N12—C120—C121	122.7 (3)
N11—Co4—C3B	91.42 (11)	N12—C120—H120	118.7
N9—Co4—C3B	89.07 (10)	C121—C120—H120	118.7
O12—Co4—C3B	30.62 (9)	C120—C121—C122	118.7 (3)
O10—C1B—O9	125.5 (3)	C120—C121—H121	120.6
O10—C1B—C2B	117.3 (3)	C122—C121—H121	120.6
O9—C1B—C2B	117.2 (3)	C123—C122—C121	118.6 (3)
C1B—O9—Co4	128.2 (2)	C123—C122—H122	120.7
C1B—O10—Co5	149.1 (2)	C121—C122—H122	120.7
C1B—C2B—H2B1	109.5	C124—C123—C122	119.5 (3)
C1B—C2B—H2B2	109.5	C124—C123—H123	120.3
H2B1—C2B—H2B2	109.5	C122—C123—H123	120.3
C1B—C2B—H2B3	109.5	N12—C124—C123	122.6 (3)
H2B1—C2B—H2B3	109.5	N12—C124—H124	118.7
H2B2—C2B—H2B3	109.5	C123—C124—H124	118.7
O11—C3B—O12	118.5 (3)	C134—N13—C130	117.2 (3)
O11—C3B—C4B	119.8 (3)	C134—N13—Co5	121.8 (2)
O12—C3B—C4B	121.7 (3)	C130—N13—Co5	120.9 (2)
O11—C3B—Co4	57.59 (16)	N13—C130—C131	123.0 (3)
O12—C3B—Co4	60.92 (16)	N13—C130—H130	118.5
C4B—C3B—Co4	175.9 (2)	C131—C130—H130	118.5
C3B—O11—Co4	92.23 (19)	C132—C131—C130	118.9 (3)
C3B—O12—Co5	147.8 (2)	C132—C131—H131	120.5
C3B—O12—Co4	88.46 (17)	C130—C131—H131	120.5
Co5—O12—Co4	121.30 (10)	C131—C132—C133	119.2 (3)
O10—Co5—O13	178.96 (9)	C131—C132—H132	120.4
O10—Co5—N12	92.36 (10)	C133—C132—H132	120.4
O13—Co5—N12	88.51 (10)	C134—C133—C132	118.2 (3)
O10—Co5—O12	89.30 (8)	C134—C133—H133	120.9
O13—Co5—O12	91.26 (8)	C132—C133—H133	120.9
N12—Co5—O12	90.64 (9)	N13—C134—C133	123.4 (3)
O10—Co5—N13	88.66 (10)	N13—C134—H134	118.3
O13—Co5—N13	90.46 (10)	C133—C134—H134	118.3
N12—Co5—N13	178.72 (10)	C144—N14—C140	117.3 (3)
O12—Co5—N13	90.15 (9)	C144—N14—Co6	120.0 (2)
O10—Co5—O15	90.23 (8)	C140—N14—Co6	121.9 (2)
O13—Co5—O15	89.23 (8)	N14—C140—C141	122.9 (4)
N12—Co5—O15	88.05 (9)	N14—C140—H140	118.5
O12—Co5—O15	178.58 (8)	C141—C140—H140	118.5
N13—Co5—O15	91.17 (9)	C142—C141—C140	118.8 (4)
C3B—C4B—H4B1	109.5	C142—C141—H141	120.6
C3B—C4B—H4B2	109.5	C140—C141—H141	120.6
H4B1—C4B—H4B2	109.5	C141—C142—C143	118.6 (4)
C3B—C4B—H4B3	109.5	C141—C142—H142	120.7
H4B1—C4B—H4B3	109.5	C143—C142—H142	120.7
H4B2—C4B—H4B3	109.5	C144—C143—C142	119.3 (4)
O13—C5B—O14	125.5 (3)	C144—C143—H143	120.4
O13—C5B—C6B	117.6 (3)	C142—C143—H143	120.4
O14—C5B—C6B	116.8 (3)	N14—C144—C143	123.1 (4)
C5B—O13—Co5	149.7 (2)	N14—C144—H144	118.5
C5B—O14—Co6	127.2 (2)	C143—C144—H144	118.5
C5B—C6B—H6B1	109.5	C150—N15—C154	117.9 (3)
C5B—C6B—H6B2	109.5	C150—N15—Co6	119.7 (2)
H6B1—C6B—H6B2	109.5	C154—N15—Co6	122.4 (2)
C5B—C6B—H6B3	109.5	N15—C150—C151	123.5 (4)
H6B1—C6B—H6B3	109.5	N15—C150—H150	118.3
H6B2—C6B—H6B3	109.5	C151—C150—H150	118.3
O16—C7B—O15	119.0 (3)	C152—C151—C150	118.2 (4)
O16—C7B—C8B	119.9 (3)	C152—C151—H151	120.9
O15—C7B—C8B	121.0 (3)	C150—C151—H151	120.9
O16—C7B—Co6	58.29 (16)	C153—C152—C151	118.9 (3)
O15—C7B—Co6	60.76 (15)	C153—C152—H152	120.6
C8B—C7B—Co6	178.0 (2)	C151—C152—H152	120.6
C7B—O15—Co5	148.4 (2)	C152—C153—C154	119.6 (4)
C7B—O15—Co6	88.41 (17)	C152—C153—H153	120.2
Co5—O15—Co6	121.45 (10)	C154—C153—H153	120.2
C7B—O16—Co6	91.69 (19)	N15—C154—C153	122.0 (4)
C7B—C8B—H8B1	109.5	N15—C154—H154	119.0
C7B—C8B—H8B2	109.5	C153—C154—H154	119.0
H8B1—C8B—H8B2	109.5	C160—N16—C163	117.2 (3)
C7B—C8B—H8B3	109.5	C160—N16—Co6	123.8 (2)
H8B1—C8B—H8B3	109.5	C163—N16—Co6	119.0 (2)
H8B2—C8B—H8B3	109.5	N16—C160—C161	122.9 (3)
O14—Co6—N15	100.42 (10)	N16—C160—H160	118.5
O14—Co6—O16	162.49 (9)	C161—C160—H160	118.5
N15—Co6—O16	96.29 (10)	C160—C161—C162	119.1 (4)
O14—Co6—N14	95.28 (11)	C160—C161—H161	120.4
N15—Co6—N14	85.65 (11)	C162—C161—H161	120.4
O16—Co6—N14	91.14 (10)	C164—C162—C161	118.3 (4)
O14—Co6—N16	88.19 (10)	C164—C162—H162	120.9
N15—Co6—N16	89.42 (10)	C161—C162—H162	120.9
O16—Co6—N16	86.79 (10)	N16—C163—C164	123.5 (4)
N14—Co6—N16	174.41 (10)	N16—C163—H163	118.2
O14—Co6—O15	102.54 (8)	C164—C163—H163	118.2
N15—Co6—O15	157.04 (10)	C162—C164—C163	119.0 (3)
O16—Co6—O15	60.85 (8)	C162—C164—H164	120.5
N14—Co6—O15	92.24 (9)	C163—C164—H164	120.5
N16—Co6—O15	91.28 (9)	F5—P1—F1	90.70 (16)
O14—Co6—C7B	133.21 (9)	F5—P1—F2	178.9 (2)
N15—Co6—C7B	126.26 (11)	F1—P1—F2	90.34 (19)
O16—Co6—C7B	30.02 (9)	F5—P1—F6	89.73 (15)
N14—Co6—C7B	91.56 (11)	F1—P1—F6	90.52 (15)
N16—Co6—C7B	89.24 (10)	F2—P1—F6	90.49 (18)
O15—Co6—C7B	30.83 (9)	F5—P1—F3	90.02 (14)
C14—N1—C10	116.9 (3)	F1—P1—F3	88.68 (14)
C14—N1—Co1	120.5 (2)	F2—P1—F3	89.78 (17)
C10—N1—Co1	122.7 (2)	F6—P1—F3	179.15 (16)
N1—C10—C11	123.0 (3)	F5—P1—F4	88.64 (16)
N1—C10—H10	118.5	F1—P1—F4	178.83 (16)
C11—C10—H10	118.5	F2—P1—F4	90.32 (18)
C12—C11—C10	119.3 (3)	F6—P1—F4	90.44 (15)
C12—C11—H11	120.4	F3—P1—F4	90.37 (14)
C10—C11—H11	120.4	F11B—P2—F12B	94.6 (3)
C13—C12—C11	118.3 (3)	F8—P2—F9	96.6 (3)
C13—C12—H12	120.8	F8—P2—F10	96.1 (2)
C11—C12—H12	120.8	F9—P2—F10	91.8 (2)
C12—C13—C14	118.6 (3)	F8—P2—F7	92.8 (3)
C12—C13—H13	120.7	F9—P2—F7	91.6 (3)
C14—C13—H13	120.7	F10—P2—F7	170.1 (2)
N1—C14—C13	123.9 (3)	F11B—P2—F7B	93.8 (3)
N1—C14—H14	118.1	F12B—P2—F7B	89.4 (4)
C13—C14—H14	118.1	F9—P2—F7B	86.5 (3)
C24—N2—C20	117.7 (3)	F8—P2—F12	88.9 (3)
C24—N2—Co1	119.5 (2)	F9—P2—F12	174.4 (3)
C20—N2—Co1	122.5 (2)	F10—P2—F12	86.7 (2)
N2—C20—C21	122.7 (3)	F7—P2—F12	89.1 (3)
N2—C20—H20	118.6	F11B—P2—F8B	175.5 (3)
C21—C20—H20	118.6	F12B—P2—F8B	89.9 (3)
C20—C21—C22	119.1 (3)	F7B—P2—F8B	85.6 (3)
C20—C21—H21	120.5	F11B—P2—F9B	91.3 (3)
C22—C21—H21	120.5	F12B—P2—F9B	173.4 (4)
C23—C22—C21	118.5 (3)	F7B—P2—F9B	87.2 (3)
C23—C22—H22	120.8	F8—P2—F11	174.0 (3)
C21—C22—H22	120.8	F9—P2—F11	89.3 (3)
C22—C23—C24	118.9 (4)	F10—P2—F11	82.8 (2)
C22—C23—H23	120.6	F7—P2—F11	88.0 (2)
C24—C23—H23	120.6	F7B—P2—F11	108.3 (3)
N2—C24—C23	123.1 (4)	F12—P2—F11	85.2 (3)
N2—C24—H24	118.4	F8B—P2—F11	159.0 (3)
C23—C24—H24	118.4	F9B—P2—F11	111.5 (3)
C30—N3—C34	116.7 (3)	F18—P3—F17	91.27 (18)
C30—N3—Co1	120.4 (2)	F18—P3—F13	90.18 (15)
C34—N3—Co1	122.8 (2)	F17—P3—F13	90.13 (13)
N3—C30—C31	123.6 (4)	F18—P3—F16	90.78 (14)
N3—C30—H30	118.2	F17—P3—F16	90.11 (14)
C31—C30—H30	118.2	F13—P3—F16	179.01 (15)
C30—C31—C32	118.7 (4)	F18—P3—F15	179.8 (2)
C30—C31—H31	120.6	F17—P3—F15	88.90 (14)
C32—C31—H31	120.6	F13—P3—F15	89.88 (14)
C33—C32—C31	118.8 (4)	F16—P3—F15	89.16 (14)
C33—C32—H32	120.6	F18—P3—F14	90.28 (18)
C31—C32—H32	120.6	F17—P3—F14	178.19 (16)
C32—C33—C34	118.8 (4)	F13—P3—F14	88.94 (14)
C32—C33—H33	120.6	F16—P3—F14	90.80 (15)
C34—C33—H33	120.6	F15—P3—F14	89.55 (15)
N3—C34—C33	123.4 (4)	F20B—P4—F22B	98.7 (4)
N3—C34—H34	118.3	F20B—P4—F24B	88.5 (4)
C33—C34—H34	118.3	F22B—P4—F24B	92.9 (4)
C44—N4—C40	117.1 (3)	F23—P4—F21	90.7 (2)
C44—N4—Co2	122.8 (2)	F23—P4—F24	93.0 (2)
C40—N4—Co2	119.9 (2)	F21—P4—F24	176.1 (2)
N4—C40—C41	123.2 (3)	F23—P4—F19	92.5 (2)
N4—C40—H40	118.4	F21—P4—F19	89.1 (2)
C41—C40—H40	118.4	F24—P4—F19	92.2 (2)
C40—C41—C42	119.3 (4)	F23—P4—F22	91.6 (2)
C40—C41—H41	120.3	F21—P4—F22	90.2 (3)
C42—C41—H41	120.3	F24—P4—F22	88.3 (2)
C43—C42—C41	118.2 (3)	F19—P4—F22	175.9 (2)
C43—C42—H42	120.9	F20B—P4—F21B	94.8 (4)
C41—C42—H42	120.9	F22B—P4—F21B	89.5 (4)
C42—C43—C44	118.9 (3)	F24B—P4—F21B	175.6 (4)
C42—C43—H43	120.6	F20B—P4—F19B	85.3 (4)
C44—C43—H43	120.6	F22B—P4—F19B	174.0 (4)
N4—C44—C43	123.2 (3)	F24B—P4—F19B	91.6 (4)
N4—C44—H44	118.4	F21B—P4—F19B	85.8 (4)
C43—C44—H44	118.4	F20B—P4—F23B	173.7 (4)
C54—N5—C50	117.5 (3)	F22B—P4—F23B	87.5 (4)
C54—N5—Co2	119.5 (2)	F24B—P4—F23B	90.4 (4)
C50—N5—Co2	122.8 (2)	F21B—P4—F23B	86.1 (4)
N5—C50—C51	123.1 (3)	F19B—P4—F23B	88.5 (4)
N5—C50—H50	118.4	F23—P4—F20	178.7 (2)
C51—C50—H50	118.4	F21—P4—F20	89.0 (2)
C52—C51—C50	118.8 (3)	F24—P4—F20	87.3 (2)
C52—C51—H51	120.6	F19—P4—F20	88.8 (2)
C50—C51—H51	120.6	F22—P4—F20	87.1 (2)
C51—C52—C53	118.6 (3)

(II) top

Crystal data top

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂	Z = 1
M_r = 1335.71	F(000) = 679
Triclinic, P1	D_x = 1.608 Mg m⁻³
Hall symbol: -P 1	Synchrotron radiation, λ = 0.67110 Å
a = 10.688 (4) Å	Cell parameters from 3499 reflections
b = 11.839 (4) Å	θ = 3.0–26.9°
c = 12.480 (4) Å	µ = 1.05 mm⁻¹
α = 98.149 (5)°	T = 120 K
β = 103.605 (5)°	Needle, pink
γ = 111.722 (5)°	0.1 × 0.02 × 0.02 mm
V = 1379.3 (8) Å³

Data collection top

Bruker D8 diffractometer	5565 independent reflections
Radiation source: Daresbury SRS Station 9.8	3897 reflections with I > 2σ(I)
Silicon 111 monochromator	R_int = 0.052
ω rotation with narrow frames scans	θ_max = 24.8°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −13→13
T_min = 0.207, T_max = 1	k = −14→14
11698 measured reflections	l = −15→15

Refinement top

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)] = 0.072	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.214	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.1413P)² + 0.0662P] where P = (F_o² + 2F_c²)/3
5565 reflections	(Δ/σ)_max < 0.001
369 parameters	Δρ_max = 1.29 e Å⁻³
0 restraints	Δρ_min = −0.84 e Å⁻³

Crystal data top

[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂	γ = 111.722 (5)°
M_r = 1335.71	V = 1379.3 (8) Å³
Triclinic, P1	Z = 1
a = 10.688 (4) Å	Synchrotron radiation, λ = 0.67110 Å
b = 11.839 (4) Å	µ = 1.05 mm⁻¹
c = 12.480 (4) Å	T = 120 K
α = 98.149 (5)°	0.1 × 0.02 × 0.02 mm
β = 103.605 (5)°

Data collection top

Bruker D8 diffractometer	5565 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	3897 reflections with I > 2σ(I)
T_min = 0.207, T_max = 1	R_int = 0.052
11698 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.072	0 restraints
wR(F²) = 0.214	H-atom parameters constrained
S = 1.03	Δρ_max = 1.29 e Å⁻³
5565 reflections	Δρ_min = −0.84 e Å⁻³
369 parameters

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.0000	0.0000	0.0000	0.0251 (3)
O1	−0.0951 (4)	0.1167 (3)	0.0320 (3)	0.0316 (8)
O2	0.0088 (4)	0.3256 (3)	0.0552 (3)	0.0371 (9)
C1	−0.0998 (6)	0.2202 (5)	0.0310 (4)	0.0314 (11)
C2	−0.2417 (6)	0.2246 (6)	0.0035 (5)	0.0418 (13)
H2A	−0.3048	0.1624	−0.0683	0.063*
H2B	−0.2308	0.3087	−0.0041	0.063*
H2C	−0.2824	0.2055	0.0649	0.063*
Co2	0.21063 (7)	0.35336 (6)	0.07863 (6)	0.0318 (2)
O3	0.1867 (4)	0.1623 (3)	0.0132 (3)	0.0311 (8)
O4	0.3916 (4)	0.3243 (3)	0.0648 (3)	0.0356 (8)
C3	0.3190 (5)	0.2063 (5)	0.0248 (4)	0.0313 (11)
C4	0.3864 (6)	0.1229 (5)	−0.0078 (5)	0.0369 (12)
H4A	0.3133	0.0372	−0.0436	0.055*
H4B	0.4544	0.1230	0.0603	0.055*
H4C	0.4359	0.1536	−0.0618	0.055*
N1	0.0725 (4)	0.0084 (4)	0.1758 (4)	0.0297 (9)
C10	−0.0119 (6)	0.0034 (6)	0.2405 (5)	0.0398 (13)
H10	−0.1013	0.0044	0.2084	0.048*
C11	0.0264 (7)	−0.0031 (7)	0.3525 (5)	0.0539 (17)
H11	−0.0374	−0.0086	0.3953	0.065*
C12	0.1550 (7)	−0.0015 (7)	0.4014 (5)	0.0493 (16)
H12	0.1820	−0.0067	0.4781	0.059*
C13	0.2456 (6)	0.0077 (5)	0.3370 (5)	0.0374 (12)
H13	0.3371	0.0106	0.3689	0.045*
C14	0.2003 (5)	0.0124 (5)	0.2257 (4)	0.0299 (11)
H14	0.2630	0.0189	0.1818	0.036*
N2	0.1892 (5)	0.3914 (4)	−0.0887 (4)	0.0338 (10)
C20	0.2854 (6)	0.4924 (5)	−0.1048 (5)	0.0375 (12)
H20	0.3695	0.5428	−0.0432	0.045*
C21	0.2687 (7)	0.5273 (5)	−0.2069 (5)	0.0409 (13)
H21	0.3398	0.6001	−0.2147	0.049*
C22	0.1481 (7)	0.4553 (6)	−0.2962 (5)	0.0450 (14)
H22	0.1324	0.4783	−0.3664	0.054*
C23	0.0502 (7)	0.3487 (7)	−0.2819 (5)	0.0567 (18)
H23	−0.0328	0.2950	−0.3432	0.068*
C24	0.0739 (7)	0.3211 (6)	−0.1784 (5)	0.0495 (16)
H24	0.0046	0.2479	−0.1695	0.059*
N3	0.3173 (5)	0.5473 (4)	0.1667 (4)	0.0371 (10)
C30	0.4553 (7)	0.6139 (5)	0.1883 (5)	0.0413 (13)
H30	0.5053	0.5776	0.1521	0.050*
C31	0.5305 (7)	0.7337 (6)	0.2608 (5)	0.0491 (16)
H31	0.6286	0.7794	0.2715	0.059*
C32	0.4595 (8)	0.7850 (6)	0.3171 (6)	0.0509 (16)
H32	0.5086	0.8655	0.3695	0.061*
C33	0.3181 (8)	0.7184 (6)	0.2963 (6)	0.0566 (17)
H33	0.2668	0.7520	0.3335	0.068*
C34	0.2496 (7)	0.6006 (6)	0.2202 (6)	0.0498 (15)
H34	0.1504	0.5556	0.2051	0.060*
N4	0.2392 (5)	0.3279 (4)	0.2510 (4)	0.0401 (11)
C40	0.3638 (7)	0.3365 (5)	0.3152 (5)	0.0451 (14)
H40	0.4333	0.3376	0.2794	0.054*
C41	0.3959 (8)	0.3436 (7)	0.4293 (6)	0.0555 (17)
H41	0.4855	0.3493	0.4712	0.067*
C42	0.2966 (9)	0.3426 (7)	0.4829 (6)	0.066 (2)
H42	0.3175	0.3505	0.5626	0.079*
C43	0.1672 (9)	0.3301 (8)	0.4184 (6)	0.070 (2)
H43	0.0952	0.3260	0.4521	0.084*
C44	0.1434 (7)	0.3235 (6)	0.3042 (5)	0.0521 (16)
H44	0.0534	0.3155	0.2604	0.063*
P1	0.69698 (16)	0.16469 (15)	0.35473 (13)	0.0398 (4)
F1	0.6597 (7)	0.2811 (5)	0.3789 (5)	0.0922 (17)
F2	0.5529 (5)	0.0923 (6)	0.2524 (4)	0.0865 (16)
F3	0.7788 (5)	0.2235 (4)	0.2704 (4)	0.0707 (12)
F4	0.7324 (4)	0.0456 (4)	0.3302 (3)	0.0585 (10)
F5	0.8387 (5)	0.2319 (4)	0.4577 (3)	0.0755 (13)
F6	0.6166 (4)	0.1054 (3)	0.4400 (3)	0.0474 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0219 (5)	0.0304 (5)	0.0264 (5)	0.0100 (4)	0.0148 (4)	0.0076 (4)
O1	0.0296 (19)	0.0335 (19)	0.037 (2)	0.0135 (16)	0.0185 (16)	0.0097 (15)
O2	0.034 (2)	0.038 (2)	0.047 (2)	0.0157 (17)	0.0240 (18)	0.0146 (17)
C1	0.033 (3)	0.042 (3)	0.024 (2)	0.018 (2)	0.015 (2)	0.008 (2)
C2	0.040 (3)	0.046 (3)	0.045 (3)	0.022 (3)	0.017 (3)	0.011 (3)
Co2	0.0306 (4)	0.0302 (4)	0.0327 (4)	0.0079 (3)	0.0165 (3)	0.0050 (3)
O3	0.0268 (19)	0.0376 (19)	0.0306 (19)	0.0096 (15)	0.0179 (15)	0.0096 (15)
O4	0.0246 (18)	0.038 (2)	0.038 (2)	0.0040 (16)	0.0142 (16)	0.0075 (16)
C3	0.027 (3)	0.041 (3)	0.024 (2)	0.010 (2)	0.012 (2)	0.011 (2)
C4	0.029 (3)	0.048 (3)	0.042 (3)	0.017 (2)	0.020 (2)	0.015 (3)
N1	0.028 (2)	0.031 (2)	0.030 (2)	0.0095 (18)	0.0156 (18)	0.0064 (18)
C10	0.039 (3)	0.062 (4)	0.032 (3)	0.028 (3)	0.020 (2)	0.017 (3)
C11	0.047 (4)	0.096 (5)	0.035 (3)	0.038 (4)	0.026 (3)	0.021 (3)
C12	0.051 (4)	0.079 (5)	0.031 (3)	0.035 (4)	0.020 (3)	0.020 (3)
C13	0.032 (3)	0.045 (3)	0.031 (3)	0.014 (2)	0.009 (2)	0.005 (2)
C14	0.024 (2)	0.032 (3)	0.034 (3)	0.010 (2)	0.013 (2)	0.007 (2)
N2	0.032 (2)	0.031 (2)	0.038 (3)	0.0105 (19)	0.017 (2)	0.0071 (19)
C20	0.035 (3)	0.036 (3)	0.041 (3)	0.010 (2)	0.021 (3)	0.007 (2)
C21	0.049 (4)	0.041 (3)	0.034 (3)	0.015 (3)	0.020 (3)	0.008 (2)
C22	0.051 (4)	0.054 (4)	0.040 (3)	0.026 (3)	0.024 (3)	0.019 (3)
C23	0.045 (4)	0.069 (4)	0.034 (3)	0.004 (3)	0.011 (3)	0.005 (3)
C24	0.043 (3)	0.046 (3)	0.039 (3)	0.000 (3)	0.014 (3)	0.001 (3)
N3	0.037 (3)	0.034 (2)	0.034 (2)	0.007 (2)	0.014 (2)	0.0037 (19)
C30	0.046 (3)	0.038 (3)	0.036 (3)	0.014 (3)	0.013 (3)	0.008 (2)
C31	0.046 (4)	0.038 (3)	0.043 (3)	0.002 (3)	0.008 (3)	0.003 (3)
C32	0.066 (5)	0.033 (3)	0.045 (4)	0.015 (3)	0.016 (3)	0.004 (3)
C33	0.068 (5)	0.046 (4)	0.058 (4)	0.026 (3)	0.028 (4)	0.002 (3)
C34	0.049 (4)	0.045 (3)	0.051 (4)	0.016 (3)	0.023 (3)	0.001 (3)
N4	0.040 (3)	0.034 (2)	0.038 (3)	0.006 (2)	0.017 (2)	0.005 (2)
C40	0.052 (4)	0.041 (3)	0.037 (3)	0.013 (3)	0.018 (3)	0.005 (3)
C41	0.067 (5)	0.064 (4)	0.037 (3)	0.029 (4)	0.017 (3)	0.013 (3)
C42	0.080 (6)	0.073 (5)	0.039 (4)	0.024 (4)	0.025 (4)	0.010 (3)
C43	0.060 (5)	0.097 (6)	0.036 (4)	0.013 (4)	0.028 (4)	0.001 (4)
C44	0.048 (4)	0.065 (4)	0.037 (3)	0.013 (3)	0.023 (3)	0.005 (3)
P1	0.0408 (9)	0.0527 (9)	0.0337 (8)	0.0205 (7)	0.0200 (7)	0.0171 (7)
F1	0.145 (5)	0.087 (3)	0.117 (4)	0.080 (4)	0.094 (4)	0.060 (3)
F2	0.054 (3)	0.157 (5)	0.044 (2)	0.043 (3)	0.010 (2)	0.021 (3)
F3	0.086 (3)	0.093 (3)	0.068 (3)	0.044 (3)	0.057 (3)	0.049 (2)
F4	0.068 (3)	0.061 (2)	0.062 (2)	0.033 (2)	0.038 (2)	0.0168 (19)
F5	0.051 (2)	0.083 (3)	0.049 (2)	−0.009 (2)	0.0092 (19)	0.000 (2)
F6	0.046 (2)	0.059 (2)	0.0417 (19)	0.0172 (17)	0.0269 (16)	0.0154 (16)

Geometric parameters (Å, º) top

Co1—O1	2.044 (3)	C21—C22	1.368 (9)
Co1—N1	2.122 (4)	C21—H21	0.9500
Co1—O3	2.150 (3)	C22—C23	1.377 (9)
O1—C1	1.246 (6)	C22—H22	0.9500
O2—C1	1.285 (7)	C23—C24	1.366 (9)
O2—Co2	1.999 (4)	C23—H23	0.9500
C1—C2	1.496 (7)	C24—H24	0.9500
C2—H2A	0.9800	N3—C30	1.328 (8)
C2—H2B	0.9800	N3—C34	1.347 (8)
C2—H2C	0.9800	C30—C31	1.389 (8)
Co2—O4	2.126 (4)	C30—H30	0.9500
Co2—N3	2.130 (5)	C31—C32	1.382 (10)
Co2—N2	2.176 (5)	C31—H31	0.9500
Co2—N4	2.181 (5)	C32—C33	1.360 (10)
Co2—O3	2.190 (4)	C32—H32	0.9500
O3—C3	1.276 (6)	C33—C34	1.387 (9)
O4—C3	1.273 (6)	C33—H33	0.9500
C3—C4	1.487 (8)	C34—H34	0.9500
C4—H4A	0.9800	N4—C44	1.335 (8)
C4—H4B	0.9800	N4—C40	1.341 (8)
C4—H4C	0.9800	C40—C41	1.367 (9)
N1—C10	1.337 (7)	C40—H40	0.9500
N1—C14	1.341 (6)	C41—C42	1.378 (10)
C10—C11	1.382 (8)	C41—H41	0.9500
C10—H10	0.9500	C42—C43	1.368 (11)
C11—C12	1.359 (9)	C42—H42	0.9500
C11—H11	0.9500	C43—C44	1.374 (9)
C12—C13	1.381 (8)	C43—H43	0.9500
C12—H12	0.9500	C44—H44	0.9500
C13—C14	1.376 (7)	P1—F5	1.575 (4)
C13—H13	0.9500	P1—F1	1.579 (5)
C14—H14	0.9500	P1—F2	1.589 (5)
N2—C20	1.335 (7)	P1—F3	1.596 (4)
N2—C24	1.338 (8)	P1—F4	1.598 (4)
C20—C21	1.387 (8)	P1—F6	1.599 (3)
C20—H20	0.9500

O1—Co1—O1ⁱ	180.0 (2)	C13—C14—H14	118.1
O1—Co1—N1ⁱ	88.44 (15)	C20—N2—C24	116.6 (5)
O1ⁱ—Co1—N1ⁱ	91.56 (15)	C20—N2—Co2	121.4 (4)
O1—Co1—N1	91.56 (15)	C24—N2—Co2	121.9 (4)
O1ⁱ—Co1—N1	88.44 (15)	N2—C20—C21	123.2 (6)
N1ⁱ—Co1—N1	180.00 (8)	N2—C20—H20	118.4
O1—Co1—O3	88.62 (14)	C21—C20—H20	118.4
O1ⁱ—Co1—O3	91.38 (14)	C22—C21—C20	118.9 (5)
N1ⁱ—Co1—O3	87.68 (14)	C22—C21—H21	120.6
N1—Co1—O3	92.32 (14)	C20—C21—H21	120.6
O1—Co1—O3ⁱ	91.38 (14)	C21—C22—C23	118.4 (6)
O1ⁱ—Co1—O3ⁱ	88.62 (14)	C21—C22—H22	120.8
N1ⁱ—Co1—O3ⁱ	92.32 (14)	C23—C22—H22	120.8
N1—Co1—O3ⁱ	87.68 (14)	C24—C23—C22	119.2 (6)
O3—Co1—O3ⁱ	180.0 (3)	C24—C23—H23	120.4
C1—O1—Co1	148.0 (3)	C22—C23—H23	120.4
C1—O2—Co2	127.5 (3)	N2—C24—C23	123.7 (6)
O1—C1—O2	125.1 (5)	N2—C24—H24	118.2
O1—C1—C2	118.3 (5)	C23—C24—H24	118.2
O2—C1—C2	116.6 (5)	C30—N3—C34	116.9 (5)
C1—C2—H2A	109.5	C30—N3—Co2	122.9 (4)
C1—C2—H2B	109.5	C34—N3—Co2	119.2 (4)
H2A—C2—H2B	109.5	N3—C30—C31	123.5 (6)
C1—C2—H2C	109.5	N3—C30—H30	118.2
H2A—C2—H2C	109.5	C31—C30—H30	118.2
H2B—C2—H2C	109.5	C32—C31—C30	118.5 (6)
O2—Co2—O4	161.20 (15)	C32—C31—H31	120.8
O2—Co2—N3	100.56 (17)	C30—C31—H31	120.8
O4—Co2—N3	97.84 (17)	C33—C32—C31	118.9 (6)
O2—Co2—N2	88.23 (16)	C33—C32—H32	120.5
O4—Co2—N2	86.76 (15)	C31—C32—H32	120.5
N3—Co2—N2	93.59 (17)	C32—C33—C34	119.2 (6)
O2—Co2—N4	92.53 (17)	C32—C33—H33	120.4
O4—Co2—N4	93.60 (17)	C34—C33—H33	120.4
N3—Co2—N4	82.83 (17)	N3—C34—C33	123.0 (6)
N2—Co2—N4	176.41 (17)	N3—C34—H34	118.5
O2—Co2—O3	101.43 (14)	C33—C34—H34	118.5
O4—Co2—O3	60.72 (13)	C44—N4—C40	116.3 (6)
N3—Co2—O3	157.39 (16)	C44—N4—Co2	121.8 (5)
N2—Co2—O3	92.30 (15)	C40—N4—Co2	121.0 (4)
N4—Co2—O3	90.99 (15)	N4—C40—C41	123.4 (6)
C3—O3—Co1	146.3 (3)	N4—C40—H40	118.3
C3—O3—Co2	89.3 (3)	C41—C40—H40	118.3
Co1—O3—Co2	121.64 (16)	C40—C41—C42	119.1 (7)
C3—O4—Co2	92.2 (3)	C40—C41—H41	120.4
O4—C3—O3	117.8 (5)	C42—C41—H41	120.4
O4—C3—C4	120.9 (5)	C43—C42—C41	118.4 (7)
O3—C3—C4	121.3 (5)	C43—C42—H42	120.8
C3—C4—H4A	109.5	C41—C42—H42	120.8
C3—C4—H4B	109.5	C42—C43—C44	118.8 (7)
H4A—C4—H4B	109.5	C42—C43—H43	120.6
C3—C4—H4C	109.5	C44—C43—H43	120.6
H4A—C4—H4C	109.5	N4—C44—C43	123.9 (7)
H4B—C4—H4C	109.5	N4—C44—H44	118.1
C10—N1—C14	117.0 (5)	C43—C44—H44	118.1
C10—N1—Co1	120.5 (4)	F5—P1—F1	91.1 (3)
C14—N1—Co1	122.4 (3)	F5—P1—F2	177.9 (3)
N1—C10—C11	122.3 (5)	F1—P1—F2	90.4 (3)
N1—C10—H10	118.9	F5—P1—F3	90.4 (3)
C11—C10—H10	118.9	F1—P1—F3	90.8 (2)
C12—C11—C10	120.1 (6)	F2—P1—F3	91.0 (3)
C12—C11—H11	119.9	F5—P1—F4	89.5 (3)
C10—C11—H11	119.9	F1—P1—F4	179.2 (3)
C11—C12—C13	118.5 (6)	F2—P1—F4	89.0 (3)
C11—C12—H12	120.8	F3—P1—F4	89.8 (2)
C13—C12—H12	120.8	F5—P1—F6	89.1 (2)
C14—C13—C12	118.4 (5)	F1—P1—F6	89.7 (2)
C14—C13—H13	120.8	F2—P1—F6	89.5 (2)
C12—C13—H13	120.8	F3—P1—F6	179.3 (2)
N1—C14—C13	123.7 (5)	F4—P1—F6	89.7 (2)
N1—C14—H14	118.1

Symmetry code: (i) −x, −y, −z.

Experimental details

	(I)	(II)
Crystal data
Chemical formula	[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂	[Co₃(C₂H₃O₂)₄(C₅H₅N)₈](PF₆)₂
M_r	1335.71	1335.71
Crystal system, space group	Triclinic, P1	Triclinic, P1
Temperature (K)	120	120
a, b, c (Å)	10.7354 (6), 22.1257 (12), 23.6103 (13)	10.688 (4), 11.839 (4), 12.480 (4)
α, β, γ (°)	99.380 (1), 95.008 (1), 92.238 (1)	98.149 (5), 103.605 (5), 111.722 (5)
V (Å³)	5503.9 (5)	1379.3 (8)
Z	4	1
Radiation type	Synchrotron, λ = 0.84610 Å	Synchrotron, λ = 0.67110 Å
µ (mm⁻¹)	1.05	1.05
Crystal size (mm)	0.25 × 0.1 × 0.05	0.1 × 0.02 × 0.02

Data collection
Diffractometer	Bruker D8 diffractometer	Bruker D8 diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.463, 0.949	0.207, 1
No. of measured, independent and observed [I > 2σ(I)] reflections	38731, 21108, 17966	11698, 5565, 3897
R_int	0.030	0.052
(sin θ/λ)_max (Å⁻¹)	0.620	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.056, 0.152, 1.05	0.072, 0.214, 1.03
No. of reflections	21108	5565
No. of parameters	1432	369
No. of restraints	66	0
H-atom treatment	H-atom parameters constrained	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.48, −1.46	1.29, −0.84

Computer programs: APEX2 (Bruker, 2004), APEX2, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), WinGX (Version 1.64; Farrugia, 1999) and PLATON (Spek, 2003), SHEXLX97.

Acknowledgements

JB thanks Jesus College, Cambridge University, for a Junior Research Fellowship.

References

Bondi, A. (1964). J. Phys. Chem. 68, 441–452. Web of Science CrossRef CAS Google Scholar
Bruker (2004). APEX2, including SAINT (Version 7.0) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chudnovsky, E. M. (1996). Science, 274, 938–939. CrossRef CAS Web of Science Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Hagen, K. S., Lachicotte, R., Kitaygorodskiy, A. & Elbouadili, A. (1993). Angew. Chem. Int. Ed. Engl. 32, 1321–1324. CSD CrossRef Web of Science Google Scholar
Rowland, R. S. & Taylor, R. (1996). J. Phys. Chem. 100, 7384–7391. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany. Google Scholar
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yaghi, O. M., O'Keeffe, M., Ockwig, N., Chae, H. K. & Eddaoudi, M. (2003). Nature (London), 423, 705–714. CrossRef PubMed CAS Google Scholar

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STRUCTURAL
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ISSN: 2053-2296

Volume 62| Part 2| February 2006| Pages m63-m66

doi:10.1107/S0108270105041570

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

Insights into crystallization mechanism: a synchrotron study of polymorphism in a cobalt acetate cluster compound

Comment

Experimental

Compound (I), polymorph 1

Crystal data

Data collection

Refinement

Compound (I), polymorph 2

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds