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In the title compound, [Co
2O
2(C
10H
8N
2)
2](ClO
4)
2, the binuclear complex cation has 2/
m symmetry, and the perchlorate ion has mirror symmetry. The Co
III atoms are coordinated by two N atoms of the 2,2′-bipyridine ligand and two bridging O atoms in a square-planar geometry. The Co
Co distance in the complex is 2.8784 (19) Å.
Supporting information
CCDC reference: 605142
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.008 Å
- R factor = 0.072
- wR factor = 0.162
- Data-to-parameter ratio = 16.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N2 .. 6.35 su
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXTL.
Bis(2,2'-bipyridine)-bis(oxo)dicobalt(III) diperchlorate
top
Crystal data top
[Co2(C10H8N2)2O2](ClO4)2 | F(000) = 664 |
Mr = 661.13 | Dx = 1.823 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 8119 reflections |
a = 13.646 (5) Å | θ = 2.1–28.4° |
b = 15.289 (6) Å | µ = 1.66 mm−1 |
c = 6.309 (2) Å | T = 298 K |
β = 113.798 (6)° | Block, blue |
V = 1204.4 (8) Å3 | 0.24 × 0.16 × 0.08 mm |
Z = 2 | |
Data collection top
Bruker Apex CCD diffractometer | 1567 independent reflections |
Radiation source: fine-focus sealed tube | 1301 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
ω scan | θmax = 28.4°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −18→18 |
Tmin = 0.691, Tmax = 0.878 | k = −20→20 |
8119 measured reflections | l = −8→8 |
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) = 0.162 | H-atom parameters constrained |
S = 1.24 | w = 1/[σ2(Fo2) + (0.0622P)2 + 2.5649P] where P = (Fo2 + 2Fc2)/3 |
1567 reflections | (Δ/σ)max < 0.001 |
93 parameters | Δρmax = 0.66 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. The maximum residual electron-density is 0.66 e Å-3 at 0.84 Å from Co1 and
the minimum one -0.53 e Å-3 at 0.73 Å from Co1. 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 | Uiso*/Ueq | |
Co1 | 0.5000 | 0.40587 (5) | 1.0000 | 0.0367 (3) | |
Cl1 | 0.25142 (15) | 0.0000 | 0.9369 (3) | 0.0506 (5) | |
O1 | 0.5469 (5) | 0.5000 | 1.2227 (9) | 0.0583 (14) | |
O2 | 0.3624 (5) | 0.0000 | 1.0917 (10) | 0.0717 (17) | |
O3 | 0.2005 (4) | 0.0769 (2) | 0.9759 (8) | 0.0677 (12) | |
O4 | 0.2422 (5) | 0.0000 | 0.6999 (9) | 0.0654 (16) | |
C1 | 0.4675 (4) | 0.2261 (3) | 0.8730 (8) | 0.0400 (10) | |
N2 | 0.4466 (3) | 0.3071 (3) | 0.7763 (7) | 0.0452 (10) | |
C3 | 0.3898 (4) | 0.3138 (4) | 0.5449 (9) | 0.0522 (13) | |
H3 | 0.3751 | 0.3690 | 0.4774 | 0.063* | |
C4 | 0.3532 (4) | 0.2413 (4) | 0.4068 (9) | 0.0551 (14) | |
H4 | 0.3150 | 0.2476 | 0.2479 | 0.066* | |
C5 | 0.3734 (5) | 0.1592 (4) | 0.5049 (10) | 0.0583 (14) | |
H5 | 0.3480 | 0.1097 | 0.4137 | 0.070* | |
C6 | 0.4321 (4) | 0.1517 (4) | 0.7412 (9) | 0.0508 (12) | |
H6 | 0.4475 | 0.0968 | 0.8104 | 0.061* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0443 (5) | 0.0231 (4) | 0.0354 (5) | 0.000 | 0.0086 (4) | 0.000 |
Cl1 | 0.0511 (10) | 0.0448 (10) | 0.0419 (9) | 0.000 | 0.0043 (8) | 0.000 |
O1 | 0.073 (4) | 0.039 (3) | 0.046 (3) | 0.000 | 0.005 (3) | 0.000 |
O2 | 0.054 (3) | 0.076 (4) | 0.059 (4) | 0.000 | −0.004 (3) | 0.000 |
O3 | 0.074 (3) | 0.045 (2) | 0.078 (3) | 0.0068 (19) | 0.024 (2) | −0.0074 (19) |
O4 | 0.079 (4) | 0.064 (4) | 0.040 (3) | 0.000 | 0.010 (3) | 0.000 |
C1 | 0.043 (3) | 0.039 (3) | 0.035 (2) | 0.003 (2) | 0.013 (2) | 0.0007 (18) |
N2 | 0.051 (2) | 0.040 (2) | 0.039 (2) | 0.0022 (18) | 0.0129 (19) | 0.0016 (17) |
C3 | 0.060 (3) | 0.051 (3) | 0.038 (3) | 0.009 (2) | 0.012 (2) | 0.007 (2) |
C4 | 0.050 (3) | 0.068 (4) | 0.035 (3) | −0.001 (3) | 0.005 (2) | −0.006 (2) |
C5 | 0.057 (3) | 0.053 (3) | 0.056 (3) | −0.005 (3) | 0.014 (3) | −0.013 (3) |
C6 | 0.056 (3) | 0.039 (3) | 0.052 (3) | 0.000 (2) | 0.016 (2) | −0.006 (2) |
Geometric parameters (Å, º) top
Co1—O1 | 1.931 (3) | C1—C6 | 1.377 (6) |
Co1—O1i | 1.931 (3) | C1—C1ii | 1.486 (9) |
Co1—N2 | 1.994 (4) | N2—C3 | 1.353 (6) |
Co1—N2ii | 1.994 (4) | C3—C4 | 1.373 (8) |
Co1—Co1i | 2.8784 (19) | C3—H3 | 0.9300 |
Cl1—O2 | 1.433 (6) | C4—C5 | 1.376 (8) |
Cl1—O3iii | 1.437 (4) | C4—H4 | 0.9300 |
Cl1—O3 | 1.437 (4) | C5—C6 | 1.384 (7) |
Cl1—O4 | 1.450 (6) | C5—H5 | 0.9300 |
C1—N2 | 1.359 (6) | C6—H6 | 0.9300 |
| | | |
O1—Co1—O1i | 83.6 (2) | N2—C1—C1ii | 114.2 (2) |
O1—Co1—N2 | 177.3 (2) | C6—C1—C1ii | 124.2 (3) |
O1i—Co1—N2 | 97.50 (16) | C3—N2—C1 | 118.6 (4) |
O1—Co1—N2ii | 97.50 (16) | C3—N2—Co1 | 126.4 (4) |
O1i—Co1—N2ii | 177.3 (2) | C1—N2—Co1 | 115.0 (3) |
N2—Co1—N2ii | 81.5 (2) | N2—C3—C4 | 121.8 (5) |
O1—Co1—Co1i | 41.81 (11) | N2—C3—H3 | 119.1 |
O1i—Co1—Co1i | 41.81 (11) | C4—C3—H3 | 119.1 |
N2—Co1—Co1i | 139.25 (11) | C3—C4—C5 | 119.7 (5) |
N2ii—Co1—Co1i | 139.25 (11) | C3—C4—H4 | 120.2 |
O2—Cl1—O3iii | 109.6 (2) | C5—C4—H4 | 120.2 |
O2—Cl1—O3 | 109.6 (2) | C4—C5—C6 | 119.0 (5) |
O3iii—Cl1—O3 | 109.9 (4) | C4—C5—H5 | 120.5 |
O2—Cl1—O4 | 109.3 (4) | C6—C5—H5 | 120.5 |
O3iii—Cl1—O4 | 109.3 (2) | C1—C6—C5 | 119.4 (5) |
O3—Cl1—O4 | 109.3 (2) | C1—C6—H6 | 120.3 |
Co1—O1—Co1i | 96.4 (2) | C5—C6—H6 | 120.3 |
N2—C1—C6 | 121.5 (4) | | |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+1, y, −z+2; (iii) x, −y, z. |
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