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Acta Crystallogr Sect E Struct Rep Online. 2008 December 1; 64(Pt 12): m1538.
Published online 2008 November 13. doi:  10.1107/S1600536808036611
PMCID: PMC2959989

Tris(phenanthroline-κ2 N,N′)cobalt(II) tetra­fluoridoborate acetonitrile solvate

Abstract

In the crystal structure of the title compound, [Co(C12H8N2)3](BF4)2·CH3CN, the mol­ecular packing involves dimers of distorted octahedrally coordinated cations which are held together by one π–π [centroid–centroid = 3.542 (4) Å] and two C—H(...)π inter­actions [2.573 (4) Å] resulting in a P4AE (Parallel Fourfold Aryl Embrace) motif. The anions are found in aryl boxes formed from the phenanthroline ligands.

Related literature

For other [Co(phen)3]2+ complexes, see: Boys et al. (1984 [triangle]); Geraghty et al. (1999 [triangle]); Russell et al. (2001 [triangle]); Tershansy et al. (2005 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1538-scheme1.jpg

Experimental

Crystal data

  • [Co(C12H8N2)3](BF4)2·C2H3N
  • M r = 814.22
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1538-efi1.jpg
  • a = 18.0443 (2) Å
  • b = 9.36230 (10) Å
  • c = 22.0702 (2) Å
  • β = 107.3610 (10)°
  • V = 3558.60 (6) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.56 mm−1
  • T = 150 (2) K
  • 0.32 × 0.28 × 0.12 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1997 [triangle]) T min = 0.840, T max = 0.935
  • 56541 measured reflections
  • 6276 independent reflections
  • 5268 reflections with I > 2σ(I)
  • R int = 0.046

Refinement

  • R[F 2 > 2σ(F 2)] = 0.072
  • wR(F 2) = 0.213
  • S = 1.03
  • 6276 reflections
  • 501 parameters
  • H-atom parameters constrained
  • Δρmax = 2.96 e Å−3
  • Δρmin = −0.94 e Å−3

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1997 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808036611/at2665sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808036611/at2665Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors gratefully acknowledge the Thailand Research fund for supporting this work (grant No. RMU5080029).

supplementary crystallographic information

Comment

The reaction of anhydrous cobalt(II) chloride with AgBF4 in the presence of phenanthroline yields the coordination compound tris(phenanthroline)cobalt(II) tetrafluoroborate (1), [Co(phen)3][BF4]2.MeCN. Crystals were grown by allowing ether to diffuse into a concentrated solution of the complex in MeCN. The title complex crystallizes in the space group P21/n in contrast to the related compound [Co(phen)3][BF4]2.H2O.EtOH which crystallizes in P1 (Russell et al., 2001). The structure of (1) is shown in Fig. 1 while important bond lengths and angles are given in Table 1. The cobalt centre is octahedrally coordinated with Co—N bond lengths and N—Co—N angles for the chelating phenanthroline ligands essentially identical to those reported for other [Co(phen)3]2+ complexes (Boys et al., 1984; Geraghty et al., 1999; Russell et al., 2001; Tershansy et al., 2005).

The crystal lattice of (1) contains dimers of [Co(phen)3]2+ cations in which there is a P4AE (Parallel Fourfold Aryl Embrace) motif involving one π–π [centroid···centroid 3.542 (4) Å] and two C—H···π interactions between the phenanthroline ligands as shown in Fig. 2 (Cg1 is the centroid of the ring C31–C35; Russell et al., 2001). The offset between the central aryl ring of the two phenanthroline ligands is 6.443 (3) Å and indicative of overlap of a single aryl ring (Russell et al., 2001). The dimers found in (1) are isolated from each other unlike in the structure of [Co(phen)3][BF4]2.H2O.EtOH where a further P4AE interaction results in formation of a zig-zag chain. A further difference is that the anions are not found in hydrophilic channels between chains of the cations but rather in aryl boxes formed from six phenanthroline ligands. This difference is presumeably the result of a lack of suitable hydrogen bonding solvent in the current structure.

Experimental

Cobalt(II) chloride (130 mg, 1 mmol) was suspended in MeCN (20 ml). AgBF4 (389 mg, 2 mmol) was then added resulting in precipitation of a white solid. The solution was filtered through celite to remove AgCl and phenanthroline (541 mg, 3 mmol) was added giving an orange solution. The volume of the solution was reduced in vacuo to ca. 10 ml and then layered with Et2O (60 ml). After two days yellow crystals formed (602 mg, 74%) Analysis calculated for C38H27N7B2F8Co: C 56.06, H 3.34, N 12.04%; found: C 56.27, H 3.40, N 12.41%. ESI+ MS: (m/z) Anal. Calc. 814.22; found: [M]+ 814.19.

Refinement

Hydrogen atoms were placed geometrically and refined with a riding model and with Uiso constrained to be 1.2 (aromatic CH) or 1.5 (Me) times Ueq of the carrier atom.

Figures

Fig. 1.
The molecular structure of (1) showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.
Fig. 2.
The molecular packing in (1) showing the C—H···π and π–π interactions which make up the P4AE structural motif. Only selected H atoms are labelled for clarity. [Symmetry codes:(i) -x, -y, ...

Crystal data

[Co(C12H8N2)3](BF4)2·C2H3NF000 = 1652
Mr = 814.22Dx = 1.520 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9965 reflections
a = 18.0443 (2) Åθ = 2.4–24.8º
b = 9.36230 (10) ŵ = 0.57 mm1
c = 22.0702 (2) ÅT = 150 (2) K
β = 107.3610 (10)ºPlate, yellow
V = 3558.60 (6) Å30.32 × 0.28 × 0.12 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer6276 independent reflections
Radiation source: fine-focus sealed tube5268 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.046
Detector resolution: 100 pixels mm-1θmax = 25.0º
T = 150(2) Kθmin = 1.3º
[var phi] and ω scansh = −21→21
Absorption correction: multi-scan(SADABS; Bruker, 1997)k = −11→11
Tmin = 0.840, Tmax = 0.935l = −26→26
56541 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.072H-atom parameters constrained
wR(F2) = 0.213  w = 1/[σ2(Fo2) + (0.1194P)2 + 14.1582P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
6276 reflectionsΔρmax = 2.96 e Å3
501 parametersΔρmin = −0.94 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

Special details

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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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 andgoodness of fit S are based on F2, conventional R-factors R are basedon F, with F set to zero for negative F2. The threshold expression ofF2 > σ(F2) is used only for calculating R-factors(gt) etc. and isnot relevant to the choice of reflections for refinement. R-factors basedon 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)

xyzUiso*/Ueq
Co10.22845 (3)0.04969 (6)0.47231 (3)0.0198 (2)
N10.1221 (2)−0.0494 (4)0.47236 (17)0.0223 (8)
N20.1549 (2)0.1052 (4)0.38050 (17)0.0233 (8)
N30.2689 (2)−0.1362 (4)0.43523 (17)0.0235 (8)
N40.3331 (2)0.1259 (4)0.45860 (17)0.0232 (8)
N50.2832 (2)0.0047 (4)0.57022 (17)0.0235 (8)
N60.20568 (19)0.2398 (4)0.51664 (17)0.0216 (8)
C10.1066 (3)−0.1261 (5)0.5179 (2)0.0252 (9)
H10.1448−0.13430.55680.030*
C20.0356 (3)−0.1949 (5)0.5099 (2)0.0289 (10)
H20.0267−0.24740.54280.035*
C3−0.0204 (3)−0.1836 (5)0.4530 (2)0.0313 (11)
H3−0.0675−0.23070.44650.038*
C4−0.0075 (2)−0.1013 (5)0.4041 (2)0.0278 (10)
C5−0.0641 (3)−0.0811 (6)0.3436 (2)0.0339 (11)
H5−0.1121−0.12580.33510.041*
C6−0.0489 (3)0.0016 (6)0.2988 (2)0.0365 (12)
H6−0.08720.01540.26040.044*
C70.0253 (3)0.0685 (5)0.3093 (2)0.0289 (10)
C80.0446 (3)0.1556 (6)0.2640 (2)0.0348 (11)
H80.00810.17390.22500.042*
C90.1171 (3)0.2124 (6)0.2777 (2)0.0349 (11)
H90.13030.27010.24820.042*
C100.1712 (3)0.1839 (5)0.3359 (2)0.0290 (10)
H100.22100.22130.34400.035*
C110.0829 (2)0.0478 (5)0.3671 (2)0.0237 (9)
C120.0656 (2)−0.0368 (5)0.4164 (2)0.0234 (9)
C130.2350 (3)−0.2627 (5)0.4210 (2)0.0312 (10)
H130.1877−0.27850.42880.037*
C140.2679 (3)−0.3736 (5)0.3948 (2)0.0379 (12)
H140.2419−0.46000.38430.046*
C150.3377 (3)−0.3543 (6)0.3847 (2)0.0375 (12)
H150.3605−0.42820.36850.045*
C160.3749 (3)−0.2222 (5)0.3990 (2)0.0319 (11)
C170.4484 (3)−0.1899 (7)0.3889 (2)0.0408 (13)
H170.4745−0.26130.37420.049*
C180.4802 (3)−0.0585 (7)0.4003 (3)0.0430 (14)
H180.5273−0.04090.39270.052*
C190.4429 (3)0.0541 (6)0.4237 (2)0.0331 (11)
C200.4724 (3)0.1939 (6)0.4353 (2)0.0393 (12)
H200.51860.21800.42740.047*
C210.4328 (3)0.2934 (6)0.4580 (2)0.0374 (12)
H210.45210.38590.46590.045*
C220.3631 (3)0.2568 (5)0.4695 (2)0.0288 (10)
H220.33680.32610.48520.035*
C230.3720 (2)0.0255 (5)0.4363 (2)0.0242 (9)
C240.3377 (2)−0.1148 (5)0.42359 (19)0.0238 (9)
C250.3210 (3)−0.1131 (5)0.5963 (2)0.0315 (10)
H250.3253−0.18840.57010.038*
C260.3545 (3)−0.1271 (7)0.6623 (3)0.0437 (14)
H260.3812−0.20990.67920.052*
C270.3477 (3)−0.0184 (7)0.7013 (3)0.0437 (14)
H270.3696−0.02690.74500.052*
C280.3075 (3)0.1062 (6)0.6756 (2)0.0333 (11)
C290.2966 (3)0.2253 (6)0.7135 (2)0.0405 (13)
H290.31750.22150.75740.049*
C300.2569 (3)0.3414 (6)0.6863 (2)0.0383 (12)
H300.25060.41670.71180.046*
C310.2242 (3)0.3520 (5)0.6191 (2)0.0301 (10)
C320.1828 (3)0.4708 (5)0.5884 (3)0.0370 (12)
H320.17490.54860.61200.044*
C330.1537 (3)0.4724 (5)0.5234 (3)0.0369 (12)
H330.12580.55070.50250.044*
C340.1667 (3)0.3550 (5)0.4893 (2)0.0271 (10)
H340.14710.35720.44520.033*
C350.2344 (2)0.2377 (5)0.5808 (2)0.0235 (9)
C360.2759 (2)0.1130 (5)0.6095 (2)0.0244 (9)
B10.5917 (3)0.4996 (7)0.3923 (3)0.0366 (13)
B20.4925 (4)1.0025 (7)0.1490 (4)0.0475 (17)
F10.5174 (3)0.4621 (5)0.3646 (2)0.0922 (17)
F20.6209 (3)0.4429 (4)0.45093 (17)0.0689 (12)
F30.60229 (15)0.6448 (3)0.39024 (15)0.0399 (7)
F40.6351 (3)0.4370 (5)0.3547 (2)0.0865 (15)
F50.4886 (3)0.9846 (5)0.2141 (2)0.0738 (12)
F60.5557 (2)1.0845 (4)0.15558 (16)0.0625 (11)
F70.4259 (2)1.0742 (5)0.1195 (2)0.0742 (13)
F80.4948 (3)0.8703 (4)0.1273 (2)0.0852 (14)
C1S0.9015 (5)0.2643 (9)0.7541 (3)0.079 (2)
H1S10.89860.36100.76770.118*
H1S20.90170.26400.71060.118*
H1S30.94820.22050.78020.118*
C2S0.8353 (5)0.1856 (8)0.7595 (4)0.072 (2)
N1S0.7831 (5)0.1217 (10)0.7631 (4)0.098 (2)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0168 (3)0.0217 (3)0.0215 (3)−0.0008 (2)0.0067 (2)−0.0004 (2)
N10.0199 (17)0.0226 (18)0.0255 (19)−0.0003 (14)0.0086 (15)−0.0029 (14)
N20.0244 (18)0.0242 (18)0.0228 (19)−0.0015 (15)0.0094 (15)−0.0027 (15)
N30.0224 (18)0.0256 (19)0.0237 (19)0.0007 (15)0.0086 (15)−0.0003 (15)
N40.0196 (17)0.028 (2)0.0206 (18)−0.0017 (15)0.0048 (14)0.0022 (15)
N50.0180 (17)0.0275 (19)0.0243 (19)0.0005 (15)0.0055 (14)0.0053 (15)
N60.0198 (17)0.0225 (18)0.0239 (19)−0.0019 (14)0.0085 (14)−0.0003 (14)
C10.024 (2)0.025 (2)0.029 (2)0.0014 (18)0.0118 (18)0.0010 (18)
C20.030 (2)0.027 (2)0.037 (3)−0.0012 (19)0.020 (2)−0.0002 (19)
C30.023 (2)0.026 (2)0.049 (3)−0.0038 (18)0.016 (2)−0.005 (2)
C40.019 (2)0.029 (2)0.038 (3)0.0007 (18)0.0127 (19)−0.008 (2)
C50.019 (2)0.040 (3)0.039 (3)−0.001 (2)0.003 (2)−0.008 (2)
C60.025 (2)0.041 (3)0.036 (3)0.001 (2)−0.003 (2)−0.007 (2)
C70.027 (2)0.031 (2)0.027 (2)0.0050 (19)0.0053 (19)−0.0032 (19)
C80.037 (3)0.040 (3)0.023 (2)0.005 (2)0.003 (2)−0.002 (2)
C90.042 (3)0.039 (3)0.024 (2)−0.001 (2)0.012 (2)0.002 (2)
C100.031 (2)0.031 (2)0.026 (2)−0.003 (2)0.0093 (19)−0.0006 (19)
C110.021 (2)0.024 (2)0.025 (2)0.0012 (17)0.0064 (18)−0.0034 (17)
C120.020 (2)0.024 (2)0.027 (2)0.0009 (17)0.0081 (18)−0.0053 (17)
C130.035 (3)0.027 (2)0.034 (3)−0.001 (2)0.013 (2)−0.0016 (19)
C140.052 (3)0.025 (2)0.034 (3)0.002 (2)0.009 (2)−0.004 (2)
C150.046 (3)0.037 (3)0.032 (3)0.015 (2)0.016 (2)−0.002 (2)
C160.033 (2)0.041 (3)0.021 (2)0.012 (2)0.0076 (19)0.001 (2)
C170.030 (3)0.066 (4)0.030 (3)0.012 (3)0.014 (2)−0.006 (2)
C180.027 (2)0.073 (4)0.035 (3)0.003 (3)0.019 (2)−0.004 (3)
C190.022 (2)0.056 (3)0.022 (2)−0.002 (2)0.0085 (19)0.005 (2)
C200.024 (2)0.062 (3)0.033 (3)−0.015 (2)0.011 (2)0.004 (2)
C210.033 (3)0.042 (3)0.034 (3)−0.016 (2)0.006 (2)0.002 (2)
C220.028 (2)0.031 (2)0.025 (2)−0.0075 (19)0.0041 (18)0.0014 (19)
C230.020 (2)0.035 (2)0.016 (2)0.0003 (18)0.0035 (16)0.0008 (17)
C240.024 (2)0.032 (2)0.015 (2)0.0033 (18)0.0057 (16)0.0008 (17)
C250.023 (2)0.036 (3)0.036 (3)0.004 (2)0.010 (2)0.008 (2)
C260.031 (3)0.056 (3)0.043 (3)0.009 (2)0.007 (2)0.023 (3)
C270.030 (3)0.068 (4)0.030 (3)0.002 (3)0.004 (2)0.016 (3)
C280.024 (2)0.052 (3)0.022 (2)−0.008 (2)0.0049 (19)0.006 (2)
C290.040 (3)0.064 (4)0.018 (2)−0.014 (3)0.009 (2)−0.007 (2)
C300.040 (3)0.045 (3)0.034 (3)−0.011 (2)0.017 (2)−0.014 (2)
C310.029 (2)0.034 (3)0.032 (3)−0.010 (2)0.015 (2)−0.011 (2)
C320.042 (3)0.026 (2)0.051 (3)−0.005 (2)0.026 (3)−0.012 (2)
C330.045 (3)0.027 (3)0.045 (3)0.004 (2)0.023 (2)0.001 (2)
C340.027 (2)0.027 (2)0.030 (2)0.0017 (18)0.0120 (19)0.0040 (18)
C350.018 (2)0.028 (2)0.026 (2)−0.0055 (17)0.0089 (17)−0.0021 (18)
C360.0172 (19)0.033 (2)0.023 (2)−0.0053 (18)0.0060 (17)0.0001 (18)
B10.035 (3)0.042 (3)0.032 (3)−0.010 (3)0.008 (2)0.001 (3)
B20.034 (3)0.035 (3)0.061 (4)−0.006 (3)−0.004 (3)0.006 (3)
F10.066 (3)0.086 (3)0.096 (3)−0.043 (2)−0.020 (2)0.043 (3)
F20.096 (3)0.051 (2)0.040 (2)0.005 (2)−0.0088 (19)0.0005 (16)
F30.0271 (14)0.0351 (16)0.060 (2)−0.0011 (12)0.0168 (13)0.0045 (14)
F40.129 (4)0.062 (3)0.089 (3)−0.011 (3)0.066 (3)−0.017 (2)
F50.078 (3)0.089 (3)0.059 (2)−0.013 (2)0.027 (2)0.001 (2)
F60.055 (2)0.075 (2)0.043 (2)−0.0238 (18)−0.0066 (16)0.0258 (18)
F70.0396 (19)0.105 (3)0.069 (3)0.012 (2)0.0018 (18)−0.033 (2)
F80.132 (4)0.048 (2)0.091 (3)0.007 (2)0.057 (3)−0.008 (2)
C1S0.116 (7)0.074 (5)0.045 (4)0.001 (5)0.023 (4)0.008 (4)
C2S0.094 (6)0.059 (4)0.080 (5)0.030 (4)0.051 (5)0.024 (4)

Geometric parameters (Å, °)

Co1—N42.123 (4)C17—C181.349 (8)
Co1—N22.129 (4)C17—H170.9300
Co1—N62.129 (4)C18—C191.428 (8)
Co1—N12.131 (3)C18—H180.9300
Co1—N52.133 (4)C19—C201.407 (8)
Co1—N32.142 (4)C19—C231.413 (6)
N1—C11.331 (6)C20—C211.357 (8)
N1—C121.353 (6)C20—H200.9300
N2—C101.331 (6)C21—C221.398 (7)
N2—C111.355 (6)C21—H210.9300
N3—C131.327 (6)C22—H220.9300
N3—C241.355 (6)C23—C241.444 (7)
N4—C221.332 (6)C25—C261.406 (7)
N4—C231.351 (6)C25—H250.9300
N5—C251.334 (6)C26—C271.362 (9)
N5—C361.366 (6)C26—H260.9300
N6—C341.331 (6)C27—C281.401 (8)
N6—C351.356 (6)C27—H270.9300
C1—C21.398 (6)C28—C361.400 (6)
C1—H10.9300C28—C291.441 (8)
C2—C31.361 (7)C29—C301.342 (8)
C2—H20.9300C29—H290.9300
C3—C41.400 (7)C30—C311.428 (7)
C3—H30.9300C30—H300.9300
C4—C121.401 (6)C31—C321.396 (7)
C4—C51.432 (7)C31—C351.409 (6)
C5—C61.346 (8)C32—C331.373 (8)
C5—H50.9300C32—H320.9300
C6—C71.432 (7)C33—C341.392 (7)
C6—H60.9300C33—H330.9300
C7—C111.399 (6)C34—H340.9300
C7—C81.413 (7)C35—C361.429 (6)
C8—C91.359 (7)B1—F11.344 (7)
C8—H80.9300B1—F21.351 (7)
C9—C101.388 (7)B1—F31.376 (7)
C9—H90.9300B1—F41.426 (8)
C10—H100.9300B2—F81.333 (8)
C11—C121.451 (6)B2—F61.346 (7)
C13—C141.405 (7)B2—F71.360 (7)
C13—H130.9300B2—F51.468 (9)
C14—C151.353 (8)C1S—C2S1.438 (12)
C14—H140.9300C1S—H1S10.9600
C15—C161.398 (8)C1S—H1S20.9600
C15—H150.9300C1S—H1S30.9600
C16—C241.405 (6)C2S—N1S1.139 (11)
C16—C171.440 (7)
N4—Co1—N296.35 (14)C24—C16—C17118.5 (5)
N4—Co1—N694.96 (14)C18—C17—C16121.5 (5)
N2—Co1—N694.71 (14)C18—C17—H17119.3
N4—Co1—N1170.19 (14)C16—C17—H17119.3
N2—Co1—N178.55 (14)C17—C18—C19121.4 (5)
N6—Co1—N193.82 (13)C17—C18—H18119.3
N4—Co1—N592.75 (13)C19—C18—H18119.3
N2—Co1—N5168.89 (14)C20—C19—C23117.1 (5)
N6—Co1—N578.11 (14)C20—C19—C18124.0 (5)
N1—Co1—N593.34 (14)C23—C19—C18118.9 (5)
N4—Co1—N378.43 (14)C21—C20—C19119.6 (4)
N2—Co1—N391.24 (14)C21—C20—H20120.2
N6—Co1—N3171.57 (13)C19—C20—H20120.2
N1—Co1—N393.21 (13)C20—C21—C22120.0 (5)
N5—Co1—N396.84 (14)C20—C21—H21120.0
C1—N1—C12117.8 (4)C22—C21—H21120.0
C1—N1—Co1128.9 (3)N4—C22—C21122.1 (5)
C12—N1—Co1113.2 (3)N4—C22—H22118.9
C10—N2—C11117.9 (4)C21—C22—H22118.9
C10—N2—Co1128.8 (3)N4—C23—C19122.6 (4)
C11—N2—Co1113.3 (3)N4—C23—C24117.7 (4)
C13—N3—C24118.1 (4)C19—C23—C24119.7 (4)
C13—N3—Co1129.0 (3)N3—C24—C16122.6 (4)
C24—N3—Co1112.9 (3)N3—C24—C23117.5 (4)
C22—N4—C23118.6 (4)C16—C24—C23119.9 (4)
C22—N4—Co1127.9 (3)N5—C25—C26122.1 (5)
C23—N4—Co1113.5 (3)N5—C25—H25119.0
C25—N5—C36118.2 (4)C26—C25—H25119.0
C25—N5—Co1128.6 (3)C27—C26—C25119.5 (5)
C36—N5—Co1113.2 (3)C27—C26—H26120.2
C34—N6—C35118.1 (4)C25—C26—H26120.2
C34—N6—Co1128.1 (3)C26—C27—C28120.0 (5)
C35—N6—Co1113.7 (3)C26—C27—H27120.0
N1—C1—C2123.0 (4)C28—C27—H27120.0
N1—C1—H1118.5C36—C28—C27117.4 (5)
C2—C1—H1118.5C36—C28—C29119.1 (5)
C3—C2—C1118.7 (4)C27—C28—C29123.6 (5)
C3—C2—H2120.6C30—C29—C28120.9 (5)
C1—C2—H2120.6C30—C29—H29119.5
C2—C3—C4120.4 (4)C28—C29—H29119.5
C2—C3—H3119.8C29—C30—C31121.4 (5)
C4—C3—H3119.8C29—C30—H30119.3
C3—C4—C12116.9 (4)C31—C30—H30119.3
C3—C4—C5123.7 (4)C32—C31—C35117.5 (4)
C12—C4—C5119.4 (4)C32—C31—C30123.6 (5)
C6—C5—C4121.1 (4)C35—C31—C30118.8 (5)
C6—C5—H5119.5C33—C32—C31119.8 (4)
C4—C5—H5119.5C33—C32—H32120.1
C5—C6—C7121.2 (4)C31—C32—H32120.1
C5—C6—H6119.4C32—C33—C34119.0 (5)
C7—C6—H6119.4C32—C33—H33120.5
C11—C7—C8116.9 (4)C34—C33—H33120.5
C11—C7—C6119.3 (4)N6—C34—C33123.1 (4)
C8—C7—C6123.7 (4)N6—C34—H34118.4
C9—C8—C7119.5 (4)C33—C34—H34118.4
C9—C8—H8120.2N6—C35—C31122.5 (4)
C7—C8—H8120.2N6—C35—C36117.5 (4)
C8—C9—C10119.7 (5)C31—C35—C36120.0 (4)
C8—C9—H9120.1N5—C36—C28122.8 (4)
C10—C9—H9120.1N5—C36—C35117.5 (4)
N2—C10—C9122.7 (4)C28—C36—C35119.7 (4)
N2—C10—H10118.6F1—B1—F2112.6 (5)
C9—C10—H10118.6F1—B1—F3111.9 (5)
N2—C11—C7123.1 (4)F2—B1—F3113.7 (5)
N2—C11—C12117.4 (4)F1—B1—F4105.9 (5)
C7—C11—C12119.5 (4)F2—B1—F4105.7 (5)
N1—C12—C4123.2 (4)F3—B1—F4106.3 (4)
N1—C12—C11117.4 (4)F8—B2—F6116.8 (6)
C4—C12—C11119.4 (4)F8—B2—F7113.9 (5)
N3—C13—C14122.3 (5)F6—B2—F7111.6 (5)
N3—C13—H13118.8F8—B2—F5105.2 (5)
C14—C13—H13118.8F6—B2—F5104.2 (5)
C15—C14—C13119.9 (5)F7—B2—F5103.5 (6)
C15—C14—H14120.1C2S—C1S—H1S1109.5
C13—C14—H14120.1C2S—C1S—H1S2109.5
C14—C15—C16119.3 (5)H1S1—C1S—H1S2109.5
C14—C15—H15120.4C2S—C1S—H1S3109.5
C16—C15—H15120.4H1S1—C1S—H1S3109.5
C15—C16—C24117.8 (4)H1S2—C1S—H1S3109.5
C15—C16—C17123.6 (5)N1S—C2S—C1S178.8 (10)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: AT2665).

References

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