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Acta Crystallogr Sect E Struct Rep Online. 2010 December 1; 66(Pt 12): m1597.
Published online 2010 November 20. doi:  10.1107/S1600536810046891
PMCID: PMC3011554

Triazidotris[μ-2-(2-pyridyl)ethanolato]dicobalt(II) acetonitrile monosolvate

Abstract

In the title compound, [Co2(C7H8NO)3(N3)3]·CH3CN, the two CoII ions in the dinuclear complex have different coordination environments, both in a distorted octa­hedral geometry. One CoII atom is coordinated by three O atoms from the three 2-hy­droxy­ethyl­pyridine (HEP) bridging ligands, two N atoms from two HEP ligands and one azido ligand, while the other CoII atom is coordinated by the same three O atoms, one N atom from an HEP ligand and two azido ligands. Weak inter­molecular C—H(...)N hydrogen bonds link the dinuclear complexes into corrugated layers parallel to the bc plane. These layers are further packed with the formation of channels propagating in [010] and filled with the disordered [in a ratio 0.691 (13):0.309 (13)] acetonitrile solvate mol­ecules.

Related literature

For the crystal structures of cobalt complexes with related ligands, see: Lah et al. (2006 [triangle]); Cheng & Wei (2002 [triangle]). For general background to mol­ecules functioning as nanoscale magnets, see: Sanudo et al. (2003 [triangle]); Sessoli et al. (1993 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1597-scheme1.jpg

Experimental

Crystal data

  • [Co2(C7H8NO)3(N3)3]·C2H3N
  • M r = 651.44
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1597-efi1.jpg
  • a = 10.8612 (11) Å
  • b = 10.9177 (12) Å
  • c = 13.3809 (14) Å
  • α = 90.299 (1)°
  • β = 112.659 (2)°
  • γ = 97.311 (1)°
  • V = 1449.8 (3) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.19 mm−1
  • T = 298 K
  • 0.28 × 0.23 × 0.11 mm

Data collection

  • Bruker SMART 1000 CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996) [triangle] T min = 0.731, T max = 0.880
  • 7657 measured reflections
  • 5044 independent reflections
  • 3337 reflections with I > 2σ(I)
  • R int = 0.025

Refinement

  • R[F 2 > 2σ(F 2)] = 0.041
  • wR(F 2) = 0.098
  • S = 1.00
  • 5044 reflections
  • 399 parameters
  • H-atom parameters constrained
  • Δρmax = 0.45 e Å−3
  • Δρmin = −0.27 e Å−3

Data collection: APEX2 (Bruker, 2006 [triangle]); cell refinement: SAINT (Bruker, 2006 [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
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810046891/cv2795sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810046891/cv2795Isup2.hkl

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

Acknowledgments

This work was supported by the National Natural Science Foundation of China (grant Nos. 20671048 and 21041002)

supplementary crystallographic information

Comment

Many present and future specialized applications of magnets require monodisperse, nanoscale magnetic particles, and the discovery that individual molecules can function as nanoscale magnets was thus a significant development (Sanudo et al., 2003; Sessoli et al., 1993). We have synthesized the title compound, and characterized it by X-ray diffraction and elemental analysis which is reported in this paper.

In the title compound, (I) (Fig. 1), [Co2(C7H9NO)3(N3)3].CH3CN, two Co(II) ions in the dinuclear complex have different coordination environments both having distorted octahedral geometry. The bond lengths and angles in (I) are normal and correspond to those observed in related complexes (Lah et al., 2006; Cheng et al., 2002). Weak intermolecular C—H···N hydrogen bonds (Table 1) link the dinuclear complexes into corrugated layers parallel to bc plane. These layers are further packed with the formation of channels propagated in direction [010] and filled with the disordered [in a ratio 0.691 (13):0.309 (13)] acetonitrile solvate molecules.

Experimental

A mixtutre of solutions of CoCl2.6H2O(1 mmol, 238 mg) in methanol (10 ml) and acetonitrile (10 ml) was added Pyridine-2-ethanol(2 mmol, 246 mg) in 5 ml methanol, NaN3(2 mmol, 130 mg) and terramethylammonium hydroide(0.4 mmol, 165 mg, 25% solution in water), then stirred for 6 h. The resulting red solution was filtrated and was allowed to stand at room temperature for about three week, whereupon brown block crystal suitable for X-ray diffraction analysis was obtained.

Refinement

All H atoms were placed in geometrically calculated positions, with C—H = 0.93–0.96 Å, and allowed to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(Cmethyl).

Figures

Fig. 1.
The molecular structure of (I) showing the atomic numbering and 30% probability displacement ellipsoids. The disordered solvent molecule and H atoms omitted for clarity.

Crystal data

[Co2(C7H8NO)3(N3)3]·C2H3NZ = 2
Mr = 651.44F(000) = 668
Triclinic, P1Dx = 1.492 Mg m3
a = 10.8612 (11) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.9177 (12) ÅCell parameters from 2225 reflections
c = 13.3809 (14) Åθ = 2.6–25.2°
α = 90.299 (1)°µ = 1.19 mm1
β = 112.659 (2)°T = 298 K
γ = 97.311 (1)°Block, brown
V = 1449.8 (3) Å30.28 × 0.23 × 0.11 mm

Data collection

Bruker SMART 1000 CCD diffractometer5044 independent reflections
Radiation source: fine-focus sealed tube3337 reflections with I > 2σ(I)
graphiteRint = 0.025
phi and ω scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.731, Tmax = 0.880k = −12→12
7657 measured reflectionsl = −15→9

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.0388P)2] where P = (Fo2 + 2Fc2)/3
5044 reflections(Δ/σ)max = 0.001
399 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = −0.27 e Å3

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

xyzUiso*/UeqOcc. (<1)
Co10.79597 (5)0.73623 (4)0.18322 (4)0.03535 (16)
Co20.78387 (5)0.97181 (5)0.19775 (4)0.03735 (16)
N10.7998 (3)0.6546 (3)0.0525 (2)0.0396 (8)
N20.9332 (3)0.6468 (3)0.2842 (3)0.0401 (8)
N30.6333 (3)1.0413 (3)0.2150 (3)0.0428 (8)
N40.6574 (3)0.6080 (3)0.1861 (3)0.0461 (9)
N50.6549 (3)0.5761 (3)0.2696 (3)0.0536 (10)
N60.6448 (5)0.5410 (5)0.3463 (4)0.1064 (19)
N70.9149 (4)1.0879 (3)0.3095 (3)0.0505 (9)
N81.0220 (4)1.1180 (3)0.3044 (3)0.0544 (10)
N91.1266 (5)1.1512 (4)0.3049 (4)0.0926 (16)
N100.7804 (3)1.0773 (3)0.0821 (3)0.0482 (9)
N110.7882 (3)1.1876 (3)0.0911 (3)0.0435 (8)
N120.7913 (4)1.2946 (3)0.0908 (3)0.0645 (11)
N130.6698 (14)0.2524 (18)0.6694 (12)0.215 (8)0.691 (13)
N13'0.438 (6)0.163 (9)0.532 (5)0.22 (4)0.309 (13)
O10.9186 (2)0.8804 (2)0.1873 (2)0.0387 (6)
O20.7787 (2)0.8383 (2)0.29203 (19)0.0385 (6)
O30.6765 (2)0.8409 (2)0.09277 (19)0.0367 (6)
C10.9670 (4)0.8961 (4)0.1030 (3)0.0487 (11)
H1A1.03900.96530.12260.058*
H1B0.89490.91360.03670.058*
C21.0189 (4)0.7779 (4)0.0853 (4)0.0510 (11)
H2A1.07820.79570.04680.061*
H2B1.07070.74770.15500.061*
C30.9046 (4)0.6799 (4)0.0213 (3)0.0443 (10)
C40.9015 (4)0.6213 (4)−0.0721 (4)0.0590 (13)
H40.97370.6394−0.09310.071*
C50.7932 (5)0.5369 (4)−0.1338 (4)0.0652 (14)
H50.79260.4961−0.19520.078*
C60.6867 (4)0.5140 (4)−0.1037 (3)0.0537 (12)
H60.61110.4589−0.14520.064*
C70.6926 (4)0.5737 (3)−0.0106 (3)0.0459 (10)
H70.61950.55760.00960.055*
C80.8700 (4)0.8420 (4)0.4023 (3)0.0478 (11)
H8A0.83600.77790.43870.057*
H8B0.87290.92110.43730.057*
C91.0126 (4)0.8245 (4)0.4169 (3)0.0496 (11)
H9A1.04360.88300.37440.059*
H9B1.07190.84220.49250.059*
C101.0212 (4)0.6958 (4)0.3828 (3)0.0436 (10)
C111.1134 (4)0.6259 (4)0.4510 (4)0.0595 (12)
H111.17430.66050.51830.071*
C121.1163 (5)0.5073 (4)0.4211 (4)0.0647 (13)
H121.17950.46130.46680.078*
C131.0252 (5)0.4571 (4)0.3231 (4)0.0585 (12)
H131.02420.37580.30140.070*
C140.9345 (4)0.5285 (4)0.2565 (3)0.0483 (11)
H140.87180.49360.18990.058*
C150.5349 (3)0.8193 (4)0.0590 (3)0.0429 (10)
H15A0.50280.73450.02980.052*
H15B0.49510.87300.00120.052*
C160.4873 (4)0.8415 (4)0.1497 (3)0.0475 (10)
H16A0.39190.81080.12470.057*
H16B0.53460.79470.21080.057*
C170.5096 (4)0.9748 (4)0.1869 (3)0.0476 (10)
C180.4030 (5)1.0300 (5)0.1920 (4)0.0644 (13)
H180.31870.98330.17350.077*
C190.4218 (5)1.1530 (5)0.2244 (4)0.0764 (15)
H190.35051.19070.22620.092*
C200.5477 (5)1.2189 (5)0.2539 (4)0.0714 (14)
H200.56391.30180.27750.086*
C210.6496 (5)1.1608 (4)0.2481 (3)0.0531 (11)
H210.73461.20660.26810.064*
C220.577 (2)0.270 (3)0.600 (2)0.221 (13)0.691 (13)
C230.481 (3)0.328 (3)0.5030 (18)0.287 (14)0.691 (13)
H23A0.48620.41410.52040.430*0.691 (13)
H23B0.39110.28740.48530.430*0.691 (13)
H23C0.50600.31840.44210.430*0.691 (13)
C22'0.414 (11)0.059 (12)0.509 (7)0.27 (7)0.309 (13)
C23'0.394 (6)−0.068 (7)0.459 (5)0.28 (5)0.309 (13)
H23D0.3369−0.12240.48450.419*0.309 (13)
H23E0.4800−0.09700.48000.419*0.309 (13)
H23F0.3532−0.06650.38190.419*0.309 (13)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0370 (3)0.0337 (3)0.0329 (3)0.0039 (2)0.0113 (3)−0.0013 (2)
Co20.0417 (3)0.0345 (3)0.0354 (3)0.0051 (2)0.0146 (3)−0.0005 (2)
N10.0397 (19)0.0374 (19)0.0384 (19)0.0072 (15)0.0111 (17)−0.0022 (15)
N20.046 (2)0.0364 (19)0.0380 (19)0.0086 (15)0.0156 (17)0.0027 (15)
N30.051 (2)0.041 (2)0.040 (2)0.0118 (16)0.0202 (18)0.0026 (16)
N40.051 (2)0.046 (2)0.039 (2)−0.0019 (17)0.0179 (18)0.0028 (17)
N50.051 (2)0.053 (2)0.049 (2)−0.0040 (18)0.014 (2)0.008 (2)
N60.101 (4)0.136 (4)0.057 (3)−0.034 (3)0.019 (3)0.023 (3)
N70.054 (2)0.048 (2)0.046 (2)0.0016 (18)0.018 (2)−0.0076 (17)
N80.058 (3)0.042 (2)0.056 (2)0.004 (2)0.015 (2)−0.0057 (18)
N90.065 (3)0.089 (3)0.120 (4)−0.013 (3)0.038 (3)−0.019 (3)
N100.063 (2)0.040 (2)0.045 (2)0.0055 (17)0.0249 (19)0.0029 (17)
N110.039 (2)0.044 (2)0.044 (2)0.0024 (17)0.0138 (17)0.0017 (17)
N120.075 (3)0.044 (2)0.068 (3)−0.002 (2)0.023 (2)0.006 (2)
N130.127 (11)0.38 (2)0.143 (12)−0.007 (13)0.069 (10)0.085 (14)
N13'0.13 (4)0.43 (12)0.12 (3)0.03 (5)0.07 (3)0.03 (6)
O10.0394 (15)0.0389 (15)0.0370 (15)0.0034 (12)0.0148 (13)−0.0042 (12)
O20.0452 (16)0.0384 (15)0.0325 (15)0.0070 (12)0.0154 (13)0.0014 (12)
O30.0375 (15)0.0366 (14)0.0355 (14)0.0041 (11)0.0139 (13)−0.0006 (12)
C10.051 (3)0.049 (3)0.049 (3)−0.004 (2)0.026 (2)−0.003 (2)
C20.046 (2)0.056 (3)0.055 (3)0.003 (2)0.025 (2)−0.007 (2)
C30.041 (2)0.047 (3)0.048 (3)0.0094 (19)0.019 (2)−0.003 (2)
C40.057 (3)0.068 (3)0.057 (3)0.000 (2)0.031 (3)−0.014 (3)
C50.070 (3)0.072 (3)0.053 (3)0.002 (3)0.025 (3)−0.021 (3)
C60.053 (3)0.054 (3)0.047 (3)−0.001 (2)0.013 (2)−0.012 (2)
C70.042 (2)0.044 (2)0.043 (2)0.0028 (19)0.008 (2)−0.004 (2)
C80.063 (3)0.047 (3)0.030 (2)0.008 (2)0.014 (2)−0.0031 (19)
C90.055 (3)0.048 (3)0.035 (2)0.005 (2)0.007 (2)−0.004 (2)
C100.042 (2)0.048 (3)0.038 (2)0.004 (2)0.013 (2)0.001 (2)
C110.059 (3)0.065 (3)0.045 (3)0.014 (2)0.009 (2)0.003 (2)
C120.065 (3)0.066 (3)0.055 (3)0.031 (3)0.008 (3)0.015 (3)
C130.069 (3)0.047 (3)0.063 (3)0.022 (2)0.025 (3)0.007 (2)
C140.054 (3)0.044 (3)0.047 (3)0.011 (2)0.018 (2)0.002 (2)
C150.035 (2)0.046 (2)0.042 (2)0.0081 (18)0.007 (2)−0.0011 (19)
C160.039 (2)0.051 (3)0.051 (3)0.007 (2)0.016 (2)0.004 (2)
C170.049 (3)0.054 (3)0.044 (3)0.014 (2)0.020 (2)0.005 (2)
C180.055 (3)0.070 (3)0.074 (3)0.016 (2)0.029 (3)−0.004 (3)
C190.068 (4)0.082 (4)0.087 (4)0.032 (3)0.033 (3)−0.008 (3)
C200.086 (4)0.060 (3)0.074 (4)0.025 (3)0.033 (3)−0.009 (3)
C210.065 (3)0.047 (3)0.052 (3)0.014 (2)0.025 (2)−0.003 (2)
C220.126 (17)0.43 (4)0.123 (15)0.03 (2)0.067 (13)0.03 (2)
C230.20 (2)0.50 (5)0.19 (2)0.05 (3)0.11 (2)−0.03 (3)
C22'0.18 (7)0.4 (2)0.16 (7)0.04 (11)0.03 (5)0.04 (10)
C23'0.21 (6)0.42 (13)0.16 (6)0.01 (8)0.03 (5)0.14 (7)

Geometric parameters (Å, °)

Co1—O31.907 (3)C5—H50.9300
Co1—O21.909 (2)C6—C71.378 (5)
Co1—O11.914 (2)C6—H60.9300
Co1—N41.933 (3)C7—H70.9300
Co1—N21.958 (3)C8—C91.522 (5)
Co1—N11.977 (3)C8—H8A0.9700
Co1—Co22.6020 (7)C8—H8B0.9700
Co2—O31.916 (2)C9—C101.500 (5)
Co2—O11.920 (2)C9—H9A0.9700
Co2—N101.926 (3)C9—H9B0.9700
Co2—N71.936 (3)C10—C111.384 (6)
Co2—O21.942 (2)C11—C121.362 (6)
Co2—N31.977 (3)C11—H110.9300
N1—C71.349 (4)C12—C131.361 (6)
N1—C31.353 (4)C12—H120.9300
N2—C141.345 (5)C13—C141.378 (6)
N2—C101.353 (5)C13—H130.9300
N3—C211.343 (5)C14—H140.9300
N3—C171.354 (5)C15—C161.520 (5)
N4—N51.181 (5)C15—H15A0.9700
N5—N61.137 (5)C15—H15B0.9700
N7—N81.196 (5)C16—C171.495 (5)
N8—N91.145 (5)C16—H16A0.9700
N10—N111.199 (4)C16—H16B0.9700
N11—N121.163 (4)C17—C181.396 (5)
N13—C221.12 (2)C18—C191.374 (6)
N13'—C22'1.15 (12)C18—H180.9300
O1—C11.419 (4)C19—C201.369 (6)
O2—C81.423 (4)C19—H190.9300
O3—C151.413 (4)C20—C211.370 (6)
C1—C21.526 (5)C20—H200.9300
C1—H1A0.9700C21—H210.9300
C1—H1B0.9700C22—C231.51 (3)
C2—C31.501 (5)C23—H23A0.9600
C2—H2A0.9700C23—H23B0.9600
C2—H2B0.9700C23—H23C0.9600
C3—C41.388 (5)C22'—C23'1.49 (9)
C4—C51.371 (6)C23'—H23D0.9600
C4—H40.9300C23'—H23E0.9600
C5—C61.360 (6)C23'—H23F0.9600
O3—Co1—O280.44 (10)N1—C3—C4120.1 (4)
O3—Co1—O178.49 (10)N1—C3—C2118.8 (3)
O2—Co1—O179.33 (10)C4—C3—C2121.0 (4)
O3—Co1—N496.18 (13)C5—C4—C3120.9 (4)
O2—Co1—N492.87 (12)C5—C4—H4119.6
O1—Co1—N4171.13 (12)C3—C4—H4119.6
O3—Co1—N2173.19 (11)C6—C5—C4118.8 (4)
O2—Co1—N295.74 (12)C6—C5—H5120.6
O1—Co1—N295.31 (12)C4—C5—H5120.6
N4—Co1—N289.60 (14)C5—C6—C7119.0 (4)
O3—Co1—N189.39 (12)C5—C6—H6120.5
O2—Co1—N1169.41 (12)C7—C6—H6120.5
O1—Co1—N195.88 (12)N1—C7—C6122.9 (4)
N4—Co1—N191.11 (13)N1—C7—H7118.6
N2—Co1—N194.10 (13)C6—C7—H7118.6
O3—Co1—Co247.24 (7)O2—C8—C9113.9 (3)
O2—Co1—Co248.03 (7)O2—C8—H8A108.8
O1—Co1—Co247.35 (7)C9—C8—H8A108.8
N4—Co1—Co2123.97 (10)O2—C8—H8B108.8
N2—Co1—Co2126.20 (9)C9—C8—H8B108.8
N1—Co1—Co2122.12 (9)H8A—C8—H8B107.7
O3—Co2—O178.13 (10)C10—C9—C8112.4 (3)
O3—Co2—N1089.75 (12)C10—C9—H9A109.1
O1—Co2—N1095.34 (13)C8—C9—H9A109.1
O3—Co2—N7170.94 (13)C10—C9—H9B109.1
O1—Co2—N793.18 (13)C8—C9—H9B109.1
N10—Co2—N793.66 (15)H9A—C9—H9B107.9
O3—Co2—O279.39 (10)N2—C10—C11120.0 (4)
O1—Co2—O278.37 (10)N2—C10—C9118.5 (4)
N10—Co2—O2168.33 (12)C11—C10—C9121.5 (4)
N7—Co2—O296.48 (13)C12—C11—C10121.0 (4)
O3—Co2—N396.99 (12)C12—C11—H11119.5
O1—Co2—N3170.99 (12)C10—C11—H11119.5
N10—Co2—N392.19 (14)C13—C12—C11118.9 (4)
N7—Co2—N391.28 (14)C13—C12—H12120.6
O2—Co2—N393.36 (12)C11—C12—H12120.6
O3—Co2—Co146.96 (7)C12—C13—C14119.1 (4)
O1—Co2—Co147.16 (7)C12—C13—H13120.5
N10—Co2—Co1121.82 (10)C14—C13—H13120.5
N7—Co2—Co1124.69 (11)N2—C14—C13122.4 (4)
O2—Co2—Co146.96 (7)N2—C14—H14118.8
N3—Co2—Co1124.18 (10)C13—C14—H14118.8
C7—N1—C3118.3 (3)O3—C15—C16113.4 (3)
C7—N1—Co1119.3 (3)O3—C15—H15A108.9
C3—N1—Co1122.4 (2)C16—C15—H15A108.9
C14—N2—C10118.6 (4)O3—C15—H15B108.9
C14—N2—Co1118.1 (3)C16—C15—H15B108.9
C10—N2—Co1123.2 (3)H15A—C15—H15B107.7
C21—N3—C17118.0 (3)C17—C16—C15113.2 (3)
C21—N3—Co2119.7 (3)C17—C16—H16A108.9
C17—N3—Co2122.1 (3)C15—C16—H16A108.9
N5—N4—Co1120.4 (3)C17—C16—H16B108.9
N6—N5—N4175.6 (5)C15—C16—H16B108.9
N8—N7—Co2118.0 (3)H16A—C16—H16B107.7
N9—N8—N7176.0 (5)N3—C17—C18120.4 (4)
N11—N10—Co2122.8 (3)N3—C17—C16119.7 (3)
N12—N11—N10174.5 (4)C18—C17—C16119.9 (4)
C1—O1—Co1119.9 (2)C19—C18—C17120.4 (4)
C1—O1—Co2122.1 (2)C19—C18—H18119.8
Co1—O1—Co285.49 (10)C17—C18—H18119.8
C8—O2—Co1121.3 (2)C20—C19—C18118.6 (4)
C8—O2—Co2122.7 (2)C20—C19—H19120.7
Co1—O2—Co285.01 (10)C18—C19—H19120.7
C15—O3—Co1124.3 (2)C19—C20—C21119.0 (4)
C15—O3—Co2121.4 (2)C19—C20—H20120.5
Co1—O3—Co285.80 (10)C21—C20—H20120.5
O1—C1—C2108.9 (3)N3—C21—C20123.6 (4)
O1—C1—H1A109.9N3—C21—H21118.2
C2—C1—H1A109.9C20—C21—H21118.2
O1—C1—H1B109.9N13—C22—C23162 (3)
C2—C1—H1B109.9N13'—C22'—C23'167 (10)
H1A—C1—H1B108.3C22'—C23'—H23D109.5
C3—C2—C1111.0 (3)C22'—C23'—H23E109.5
C3—C2—H2A109.4H23D—C23'—H23E109.5
C1—C2—H2A109.4C22'—C23'—H23F109.4
C3—C2—H2B109.4H23D—C23'—H23F109.5
C1—C2—H2B109.4H23E—C23'—H23F109.5
H2A—C2—H2B108.0
O2—Co1—Co2—O3−121.83 (14)N10—Co2—O1—C1−6.8 (3)
O1—Co1—Co2—O3118.84 (14)N7—Co2—O1—C1−100.7 (3)
N4—Co1—Co2—O3−63.50 (16)O2—Co2—O1—C1163.3 (3)
N2—Co1—Co2—O3177.63 (15)N3—Co2—O1—C1139.7 (7)
N1—Co1—Co2—O353.28 (14)Co1—Co2—O1—C1122.7 (3)
O3—Co1—Co2—O1−118.84 (14)O3—Co2—O1—Co1−40.86 (10)
O2—Co1—Co2—O1119.33 (14)N10—Co2—O1—Co1−129.47 (12)
N4—Co1—Co2—O1177.66 (16)N7—Co2—O1—Co1136.55 (13)
N2—Co1—Co2—O158.79 (15)O2—Co2—O1—Co140.58 (9)
N1—Co1—Co2—O1−65.56 (15)N3—Co2—O1—Co117.0 (8)
O3—Co1—Co2—N10−54.07 (15)O3—Co1—O2—C8−164.8 (3)
O2—Co1—Co2—N10−175.90 (16)O1—Co1—O2—C8−84.8 (3)
O1—Co1—Co2—N1064.77 (16)N4—Co1—O2—C899.4 (3)
N4—Co1—Co2—N10−117.57 (17)N2—Co1—O2—C89.5 (3)
N2—Co1—Co2—N10123.56 (16)N1—Co1—O2—C8−148.7 (6)
N1—Co1—Co2—N10−0.79 (16)Co2—Co1—O2—C8−125.6 (3)
O3—Co1—Co2—N7−175.47 (16)O3—Co1—O2—Co2−39.24 (9)
O2—Co1—Co2—N762.70 (16)O1—Co1—O2—Co240.73 (10)
O1—Co1—Co2—N7−56.63 (17)N4—Co1—O2—Co2−135.03 (12)
N4—Co1—Co2—N7121.03 (18)N2—Co1—O2—Co2135.08 (11)
N2—Co1—Co2—N72.16 (17)N1—Co1—O2—Co2−23.1 (7)
N1—Co1—Co2—N7−122.19 (17)O3—Co2—O2—C8163.5 (3)
O3—Co1—Co2—O2121.83 (14)O1—Co2—O2—C883.6 (3)
O1—Co1—Co2—O2−119.33 (14)N10—Co2—O2—C8141.8 (6)
N4—Co1—Co2—O258.33 (16)N7—Co2—O2—C8−8.4 (3)
N2—Co1—Co2—O2−60.54 (15)N3—Co2—O2—C8−100.0 (3)
N1—Co1—Co2—O2175.11 (14)Co1—Co2—O2—C8124.3 (3)
O3—Co1—Co2—N364.34 (15)O3—Co2—O2—Co139.18 (9)
O2—Co1—Co2—N3−57.50 (15)O1—Co2—O2—Co1−40.74 (9)
O1—Co1—Co2—N3−176.82 (15)N10—Co2—O2—Co117.5 (7)
N4—Co1—Co2—N30.84 (17)N7—Co2—O2—Co1−132.67 (12)
N2—Co1—Co2—N3−118.03 (16)N3—Co2—O2—Co1135.66 (12)
N1—Co1—Co2—N3117.62 (16)O2—Co1—O3—C15−85.8 (2)
O3—Co1—N1—C7−75.3 (3)O1—Co1—O3—C15−166.7 (3)
O2—Co1—N1—C7−91.2 (7)N4—Co1—O3—C156.1 (3)
O1—Co1—N1—C7−153.7 (3)N2—Co1—O3—C15−142.0 (9)
N4—Co1—N1—C720.9 (3)N1—Co1—O3—C1597.2 (3)
N2—Co1—N1—C7110.5 (3)Co2—Co1—O3—C15−125.6 (3)
Co2—Co1—N1—C7−111.4 (3)O2—Co1—O3—Co239.83 (9)
O3—Co1—N1—C3102.3 (3)O1—Co1—O3—Co2−41.11 (9)
O2—Co1—N1—C386.4 (7)N4—Co1—O3—Co2131.71 (12)
O1—Co1—N1—C323.9 (3)N2—Co1—O3—Co2−16.4 (10)
N4—Co1—N1—C3−161.5 (3)N1—Co1—O3—Co2−137.24 (11)
N2—Co1—N1—C3−71.9 (3)O1—Co2—O3—C15169.1 (3)
Co2—Co1—N1—C366.2 (3)N10—Co2—O3—C15−95.4 (3)
O3—Co1—N2—C14−156.3 (9)N7—Co2—O3—C15152.4 (8)
O2—Co1—N2—C14148.3 (3)O2—Co2—O3—C1588.9 (3)
O1—Co1—N2—C14−132.0 (3)N3—Co2—O3—C15−3.2 (3)
N4—Co1—N2—C1455.4 (3)Co1—Co2—O3—C15128.1 (3)
N1—Co1—N2—C14−35.7 (3)O1—Co2—O3—Co141.02 (10)
Co2—Co1—N2—C14−171.2 (2)N10—Co2—O3—Co1136.53 (12)
O3—Co1—N2—C1027.7 (11)N7—Co2—O3—Co124.4 (8)
O2—Co1—N2—C10−27.7 (3)O2—Co2—O3—Co1−39.18 (9)
O1—Co1—N2—C1052.0 (3)N3—Co2—O3—Co1−131.30 (11)
N4—Co1—N2—C10−120.6 (3)Co1—O1—C1—C2−49.8 (4)
N1—Co1—N2—C10148.3 (3)Co2—O1—C1—C2−154.5 (2)
Co2—Co1—N2—C1012.8 (3)O1—C1—C2—C378.0 (4)
O3—Co2—N3—C21−154.7 (3)C7—N1—C3—C4−1.5 (6)
O1—Co2—N3—C21148.7 (7)Co1—N1—C3—C4−179.1 (3)
N10—Co2—N3—C21−64.7 (3)C7—N1—C3—C2174.6 (4)
N7—Co2—N3—C2129.0 (3)Co1—N1—C3—C2−3.0 (5)
O2—Co2—N3—C21125.6 (3)C1—C2—C3—N1−49.4 (5)
Co1—Co2—N3—C21163.7 (3)C1—C2—C3—C4126.7 (4)
O3—Co2—N3—C1720.4 (3)N1—C3—C4—C5−0.2 (7)
O1—Co2—N3—C17−36.2 (10)C2—C3—C4—C5−176.2 (4)
N10—Co2—N3—C17110.4 (3)C3—C4—C5—C61.8 (7)
N7—Co2—N3—C17−155.9 (3)C4—C5—C6—C7−1.7 (7)
O2—Co2—N3—C17−59.3 (3)C3—N1—C7—C61.6 (6)
Co1—Co2—N3—C17−21.2 (4)Co1—N1—C7—C6179.3 (3)
O3—Co1—N4—N5−125.1 (3)C5—C6—C7—N10.0 (7)
O2—Co1—N4—N5−44.4 (3)Co1—O2—C8—C932.7 (4)
O1—Co1—N4—N5−72.5 (10)Co2—O2—C8—C9−72.9 (4)
N2—Co1—N4—N551.4 (3)O2—C8—C9—C10−68.6 (5)
N1—Co1—N4—N5145.4 (3)C14—N2—C10—C112.4 (6)
Co2—Co1—N4—N5−83.7 (4)Co1—N2—C10—C11178.4 (3)
Co1—N4—N5—N6172 (7)C14—N2—C10—C9−175.4 (3)
O3—Co2—N7—N852.6 (10)Co1—N2—C10—C90.6 (5)
O1—Co2—N7—N836.3 (3)C8—C9—C10—N250.3 (5)
N10—Co2—N7—N8−59.3 (4)C8—C9—C10—C11−127.5 (4)
O2—Co2—N7—N8114.9 (3)N2—C10—C11—C12−0.7 (6)
N3—Co2—N7—N8−151.6 (3)C9—C10—C11—C12177.0 (4)
Co1—Co2—N7—N874.1 (4)C10—C11—C12—C13−1.0 (7)
Co2—N7—N8—N9179 (100)C11—C12—C13—C141.1 (7)
O3—Co2—N10—N11151.3 (3)C10—N2—C14—C13−2.4 (6)
O1—Co2—N10—N11−130.7 (3)Co1—N2—C14—C13−178.6 (3)
N7—Co2—N10—N11−37.2 (3)C12—C13—C14—N20.6 (6)
O2—Co2—N10—N11172.6 (5)Co1—O3—C15—C1671.6 (4)
N3—Co2—N10—N1154.3 (3)Co2—O3—C15—C16−36.6 (4)
Co1—Co2—N10—N11−172.5 (3)O3—C15—C16—C1769.0 (4)
Co2—N10—N11—N12−161 (4)C21—N3—C17—C180.3 (6)
O3—Co1—O1—C1−83.7 (3)Co2—N3—C17—C18−174.8 (3)
O2—Co1—O1—C1−166.0 (3)C21—N3—C17—C16180.0 (4)
N4—Co1—O1—C1−137.4 (8)Co2—N3—C17—C164.9 (5)
N2—Co1—O1—C199.1 (3)C15—C16—C17—N3−51.8 (5)
N1—Co1—O1—C14.5 (3)C15—C16—C17—C18127.9 (4)
Co2—Co1—O1—C1−124.7 (3)N3—C17—C18—C190.8 (7)
O3—Co1—O1—Co241.02 (9)C16—C17—C18—C19−178.9 (4)
O2—Co1—O1—Co2−41.27 (10)C17—C18—C19—C20−1.6 (8)
N4—Co1—O1—Co2−12.7 (9)C18—C19—C20—C211.3 (8)
N2—Co1—O1—Co2−136.12 (11)C17—N3—C21—C20−0.7 (6)
N1—Co1—O1—Co2129.19 (11)Co2—N3—C21—C20174.6 (4)
O3—Co2—O1—C181.9 (3)C19—C20—C21—N3−0.2 (8)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C6A—H6A1···N2Bi0.972.423.382 (3)169
C8A—H8A2···N1Aii0.962.573.384 (4)142

Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y, −z+2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV2795).

References

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  • Lah, N., Leban, I. & Clerac, R. (2006). Eur. J. Inorg. Chem. pp. 4888–4894.
  • Sanudo, E. C., Brechin, E. K., Boskovic, C., Wernsdorfer, W., Yoo, J., Yamaguchi, A., Concolino, T. R., Hendrickson, D. N. & Christou, G. (2003). Polyhedron, 22, 2267–2271.
  • Sessoli, R., Tsai, H.-L., Schake, A. R., Wang, S., Vincent, J. B., Folting, K., Gatteschi, D., Christou, G. & Hendrickson, D. N. (1993). J. Am. Chem. Soc.115, 1804–1816.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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