In the title complex, [Co(NCO)
2(C
10H
8N
2)
2], the Co atom is coordinated by four N atoms from two 2,2′-bipyridyl ligands and two N atoms from two cyanate anions in a distorted octahedral geometry. The Co atom lies on a twofold rotation axis. The average Co—N bond length is 2.126 (7) Å. Weak intermolecular C—H

O interactions lead to the formation of a three-dimensional network.
Supporting information
CCDC reference: 684452
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean
(C-C) = 0.005 Å
- R factor = 0.040
- wR factor = 0.078
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C1
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for N1 - C1 .. 5.03 su
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
1 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
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
CoCl2.6H2O(0.0476 g 0.2 mmol) was dissolved in 10 ml MeOH, the solution was
then added to an aqueous solution of 2,2'-bipyridyl(0.0316 g 0.2 mmol). The
reaction mixture was stirred for 10 minutes until the solution color became
red. NaOCN(0.0130 g 0.2 mmol) was added to the reaction mixture. The mixture
was filtered and red single crystals were obtained by slow evaporation of the
mother liquid for three weeks at room temperature. Elemental analysis for
C22H16Co N6S2 calculated: C 58.03, H 3.54, N 18.45%; found: C 58.23, H
3.23, N 18.30%.
All H atoms were placed geometrically and treated as riding on their parent
atoms with C—H 0.93 Å (2,2'-bipyridyl) [Uiso(H) =
1.2Ueq(C)].
Data collection: SMART (Siemens, 1996); cell refinement: SMART (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Crystal data top
[Co(NCO)2(C10H8N2)2] | F(000) = 932 |
Mr = 455.34 | Dx = 1.434 Mg m−3 |
Orthorhombic, Pbcn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2n2ab | Cell parameters from 1484 reflections |
a = 14.148 (12) Å | θ = 2.5–20.8° |
b = 9.774 (8) Å | µ = 0.85 mm−1 |
c = 15.253 (13) Å | T = 298 K |
V = 2109 (3) Å3 | Plate, red |
Z = 4 | 0.30 × 0.25 × 0.06 mm |
Data collection top
Bruker Smart 1000 diffractometer | 1870 independent reflections |
Radiation source: fine-focus sealed tube | 1009 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.078 |
ϕ & ω scans | θmax = 25.0°, θmin = 2.5° |
Absorption correction: multi-scan [SADABS; Sheldrick, 1996) | h = −16→14 |
Tmin = 0.786, Tmax = 0.951 | k = −11→9 |
10457 measured reflections | l = −18→17 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0386P)2 + 2.2714P] where P = (Fo2 + 2Fc2)/3 |
1870 reflections | (Δ/σ)max = 0.001 |
141 parameters | Δρmax = 0.25 e Å−3 |
0 restraints | Δρmin = −0.30 e Å−3 |
Crystal data top
[Co(NCO)2(C10H8N2)2] | V = 2109 (3) Å3 |
Mr = 455.34 | Z = 4 |
Orthorhombic, Pbcn | Mo Kα radiation |
a = 14.148 (12) Å | µ = 0.85 mm−1 |
b = 9.774 (8) Å | T = 298 K |
c = 15.253 (13) Å | 0.30 × 0.25 × 0.06 mm |
Data collection top
Bruker Smart 1000 diffractometer | 1870 independent reflections |
Absorption correction: multi-scan [SADABS; Sheldrick, 1996) | 1009 reflections with I > 2σ(I) |
Tmin = 0.786, Tmax = 0.951 | Rint = 0.078 |
10457 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.25 e Å−3 |
1870 reflections | Δρmin = −0.30 e Å−3 |
141 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 1.02936 (6) | 0.7500 | 0.0514 (2) | |
N1 | 0.45099 (19) | 1.1668 (3) | 0.6615 (2) | 0.0780 (10) | |
N2 | 0.42837 (17) | 0.8651 (2) | 0.68223 (17) | 0.0525 (7) | |
N3 | 0.36432 (16) | 1.0105 (3) | 0.81603 (17) | 0.0538 (7) | |
O1 | 0.4129 (2) | 1.3351 (3) | 0.5593 (2) | 0.1331 (13) | |
C1 | 0.4337 (2) | 1.2469 (5) | 0.6118 (3) | 0.0737 (12) | |
C2 | 0.3390 (2) | 0.8363 (3) | 0.7088 (2) | 0.0501 (8) | |
C3 | 0.2898 (2) | 0.7277 (4) | 0.6735 (2) | 0.0655 (10) | |
H3 | 0.2289 | 0.7081 | 0.6927 | 0.079* | |
C4 | 0.3309 (3) | 0.6491 (4) | 0.6103 (3) | 0.0802 (12) | |
H4 | 0.2983 | 0.5754 | 0.5863 | 0.096* | |
C5 | 0.4205 (3) | 0.6794 (4) | 0.5821 (2) | 0.0738 (11) | |
H5 | 0.4496 | 0.6275 | 0.5388 | 0.089* | |
C6 | 0.4657 (2) | 0.7879 (4) | 0.6196 (2) | 0.0669 (10) | |
H6 | 0.5263 | 0.8090 | 0.6002 | 0.080* | |
C7 | 0.3019 (2) | 0.9245 (3) | 0.7788 (2) | 0.0511 (9) | |
C8 | 0.2077 (2) | 0.9216 (3) | 0.8059 (3) | 0.0676 (10) | |
H8 | 0.1645 | 0.8642 | 0.7784 | 0.081* | |
C9 | 0.1797 (3) | 1.0036 (4) | 0.8731 (3) | 0.0808 (13) | |
H9 | 0.1172 | 1.0020 | 0.8921 | 0.097* | |
C10 | 0.2434 (3) | 1.0881 (4) | 0.9122 (2) | 0.0804 (12) | |
H10 | 0.2256 | 1.1444 | 0.9585 | 0.096* | |
C11 | 0.3354 (2) | 1.0883 (3) | 0.8814 (2) | 0.0685 (10) | |
H11 | 0.3790 | 1.1460 | 0.9082 | 0.082* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0391 (3) | 0.0536 (4) | 0.0615 (4) | 0.000 | 0.0011 (3) | 0.000 |
N1 | 0.064 (2) | 0.078 (2) | 0.092 (3) | 0.0116 (17) | 0.0007 (18) | 0.0301 (19) |
N2 | 0.0402 (15) | 0.0601 (19) | 0.0573 (19) | 0.0020 (13) | 0.0000 (14) | −0.0038 (14) |
N3 | 0.0457 (15) | 0.0555 (19) | 0.0603 (19) | 0.0050 (14) | 0.0027 (14) | −0.0032 (14) |
O1 | 0.115 (2) | 0.152 (3) | 0.133 (3) | 0.055 (2) | 0.025 (2) | 0.070 (2) |
C1 | 0.052 (2) | 0.090 (4) | 0.079 (3) | 0.020 (2) | 0.018 (2) | 0.012 (2) |
C2 | 0.0385 (19) | 0.056 (2) | 0.056 (2) | −0.0010 (17) | −0.0047 (17) | 0.0121 (17) |
C3 | 0.051 (2) | 0.070 (3) | 0.076 (3) | −0.011 (2) | −0.0061 (19) | 0.004 (2) |
C4 | 0.087 (3) | 0.077 (3) | 0.077 (3) | −0.020 (2) | −0.011 (2) | −0.012 (2) |
C5 | 0.074 (3) | 0.074 (3) | 0.072 (3) | 0.001 (2) | 0.001 (2) | −0.019 (2) |
C6 | 0.053 (2) | 0.079 (3) | 0.069 (3) | −0.0057 (19) | −0.0008 (19) | −0.009 (2) |
C7 | 0.0420 (19) | 0.047 (2) | 0.064 (3) | 0.0030 (16) | 0.0052 (16) | 0.0113 (16) |
C8 | 0.046 (2) | 0.071 (3) | 0.086 (3) | −0.0028 (18) | 0.009 (2) | 0.010 (2) |
C9 | 0.053 (2) | 0.092 (4) | 0.097 (3) | 0.012 (2) | 0.028 (2) | 0.016 (3) |
C10 | 0.079 (3) | 0.077 (3) | 0.086 (3) | 0.014 (2) | 0.033 (3) | 0.002 (2) |
C11 | 0.062 (2) | 0.066 (3) | 0.078 (3) | 0.0021 (19) | 0.013 (2) | −0.009 (2) |
Geometric parameters (Å, º) top
Co1—N1i | 2.027 (3) | C3—H3 | 0.9300 |
Co1—N1 | 2.027 (3) | C4—C5 | 1.371 (4) |
Co1—N2 | 2.162 (3) | C4—H4 | 0.9300 |
Co1—N2i | 2.162 (3) | C5—C6 | 1.364 (4) |
Co1—N3 | 2.176 (3) | C5—H5 | 0.9300 |
Co1—N3i | 2.176 (3) | C6—H6 | 0.9300 |
N1—C1 | 1.117 (4) | C7—C8 | 1.396 (4) |
N2—C6 | 1.327 (4) | C8—C9 | 1.360 (4) |
N2—C2 | 1.358 (3) | C8—H8 | 0.9300 |
N3—C11 | 1.319 (4) | C9—C10 | 1.361 (5) |
N3—C7 | 1.345 (3) | C9—H9 | 0.9300 |
O1—C1 | 1.213 (4) | C10—C11 | 1.384 (4) |
C2—C3 | 1.378 (4) | C10—H10 | 0.9300 |
C2—C7 | 1.469 (4) | C11—H11 | 0.9300 |
C3—C4 | 1.363 (4) | | |
| | | |
N1i—Co1—N1 | 97.0 (2) | C4—C3—H3 | 120.2 |
N1i—Co1—N2 | 166.18 (11) | C2—C3—H3 | 120.2 |
N1—Co1—N2 | 90.76 (12) | C3—C4—C5 | 119.6 (4) |
N1i—Co1—N2i | 90.76 (12) | C3—C4—H4 | 120.2 |
N1—Co1—N2i | 166.18 (11) | C5—C4—H4 | 120.2 |
N2—Co1—N2i | 84.07 (14) | C6—C5—C4 | 118.1 (4) |
N1i—Co1—N3 | 92.83 (12) | C6—C5—H5 | 121.0 |
N1—Co1—N3 | 93.59 (11) | C4—C5—H5 | 121.0 |
N2—Co1—N3 | 75.22 (11) | N2—C6—C5 | 123.8 (3) |
N2i—Co1—N3 | 97.44 (10) | N2—C6—H6 | 118.1 |
N1i—Co1—N3i | 93.59 (11) | C5—C6—H6 | 118.1 |
N1—Co1—N3i | 92.83 (12) | N3—C7—C8 | 121.0 (3) |
N2—Co1—N3i | 97.44 (10) | N3—C7—C2 | 116.1 (3) |
N2i—Co1—N3i | 75.22 (11) | C8—C7—C2 | 123.0 (3) |
N3—Co1—N3i | 170.29 (13) | C9—C8—C7 | 119.3 (3) |
C1—N1—Co1 | 172.6 (3) | C9—C8—H8 | 120.3 |
C6—N2—C2 | 117.9 (3) | C7—C8—H8 | 120.3 |
C6—N2—Co1 | 125.4 (2) | C8—C9—C10 | 119.7 (3) |
C2—N2—Co1 | 116.6 (2) | C8—C9—H9 | 120.2 |
C11—N3—C7 | 118.4 (3) | C10—C9—H9 | 120.2 |
C11—N3—Co1 | 125.1 (2) | C9—C10—C11 | 118.4 (4) |
C7—N3—Co1 | 115.9 (2) | C9—C10—H10 | 120.8 |
N1—C1—O1 | 178.3 (5) | C11—C10—H10 | 120.8 |
N2—C2—C3 | 120.9 (3) | N3—C11—C10 | 123.2 (3) |
N2—C2—C7 | 115.3 (3) | N3—C11—H11 | 118.4 |
C3—C2—C7 | 123.7 (3) | C10—C11—H11 | 118.4 |
C4—C3—C2 | 119.6 (3) | | |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···O1ii | 0.93 | 2.50 | 3.236 (5) | 137 |
C5—H5···O1iii | 0.93 | 2.48 | 3.198 (5) | 134 |
Symmetry codes: (ii) −x+1/2, −y+5/2, z+1/2; (iii) −x+1, −y+2, −z+1. |
Experimental details
Crystal data |
Chemical formula | [Co(NCO)2(C10H8N2)2] |
Mr | 455.34 |
Crystal system, space group | Orthorhombic, Pbcn |
Temperature (K) | 298 |
a, b, c (Å) | 14.148 (12), 9.774 (8), 15.253 (13) |
V (Å3) | 2109 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.85 |
Crystal size (mm) | 0.30 × 0.25 × 0.06 |
|
Data collection |
Diffractometer | Bruker Smart 1000 diffractometer |
Absorption correction | Multi-scan [SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.786, 0.951 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10457, 1870, 1009 |
Rint | 0.078 |
(sin θ/λ)max (Å−1) | 0.595 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.078, 1.00 |
No. of reflections | 1870 |
No. of parameters | 141 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.25, −0.30 |
Selected geometric parameters (Å, º) topCo1—N1i | 2.027 (3) | Co1—N2i | 2.162 (3) |
Co1—N1 | 2.027 (3) | Co1—N3 | 2.176 (3) |
Co1—N2 | 2.162 (3) | Co1—N3i | 2.176 (3) |
| | | |
N1i—Co1—N1 | 97.0 (2) | N2—Co1—N3 | 75.22 (11) |
N1i—Co1—N2 | 166.18 (11) | N2i—Co1—N3 | 97.44 (10) |
N1—Co1—N2 | 90.76 (12) | N1i—Co1—N3i | 93.59 (11) |
N1i—Co1—N2i | 90.76 (12) | N1—Co1—N3i | 92.83 (12) |
N1—Co1—N2i | 166.18 (11) | N2—Co1—N3i | 97.44 (10) |
N2—Co1—N2i | 84.07 (14) | N2i—Co1—N3i | 75.22 (11) |
N1i—Co1—N3 | 92.83 (12) | N3—Co1—N3i | 170.29 (13) |
N1—Co1—N3 | 93.59 (11) | | |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C10—H10···O1ii | 0.93 | 2.50 | 3.236 (5) | 136.7 |
C5—H5···O1iii | 0.93 | 2.48 | 3.198 (5) | 134.1 |
Symmetry codes: (ii) −x+1/2, −y+5/2, z+1/2; (iii) −x+1, −y+2, −z+1. |
Organometallic Co derivatives are applied as catalysts in polymerization reactions of polar olefins and for the elucidation of the hypothetical mechanism of these polymerization reactions (Milani et al., 2003). In recent years the synthesis of the without bridge bonding mononucleate complexs was used to find out the information to design the multidimensional structure complexes, so the homologic ligands complex [Co(2,2'-bipy)2(N3)2].Cl.2H2O was reported(Tang et al., 2004). In this paper, Co(C10H8N2)2(NCO)2 was synthesized by the reaction of CoCl2.6H2O, 2,2'-bipyridyl and NaOCN at room temperature and the structure of the resulting complex is presented here (Fig. 1).
The Co atom lies on a special position (Wyckoff position 4c, site symmetry 2). It is formed by coordination of two 2,2'-bipyridyls ligands and two cyanate anions. The coordination gemotry of the central Co atom is distorted octahedral with four N atoms from two 2,2'-bipyridyls and two N atoms from two cyanate anions. The equatorial plane consists of N1, N2, N3 and N3iwith an average bond length of 2.135 (3) Å. The apical positions are occupied by a cyanate anion and a N atom from a 2,2'-bipyridyl with the bond length 2.027 (3) Å 2.162 (3) Å, respectively. The distances Co—N(2,2'-bipyridyl) in the title complex are significantly longer (2.176 (3) Å and 2.162 (3) Å) than those in the comparable bond length (1.950 (3) Å and 1.954 (3) Å, Tang et al.(2004)). The complexes arrange into a three-dimensional network via weak intermolecular C—H···O interactions (H···O distances: 2.499 (3) Å and 2.481 (4) Å; C···O distances: 3.417 (5) Å and 3.084 (7) Å)..