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Acta Crystallogr Sect E Struct Rep Online. 2010 June 1; 66(Pt 6): m614.
Published online 2010 May 8. doi:  10.1107/S1600536810015758
PMCID: PMC2979601

Bis(isocyanato-κN)bis­(1,10-phenanthroline-κ2 N,N′)cobalt(II)

Abstract

In the title complex, [Co(NCO)2(C12H8N2)2], the CoII atom, lying on a twofold rotation axis, is coordinated in a distorted octa­hedral environment by four N atoms from two chelating phenanthroline ligands and two N atoms from two isocyanate ligands in cis positions.

Related literature

For related structures, see: Cheng & Hu (2003 [triangle]); He et al. (2004 [triangle]); Yin (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m614-scheme1.jpg

Experimental

Crystal data

  • [Co(CNO)2(C12H8N2)2]
  • M r = 503.38
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m614-efi1.jpg
  • a = 13.2317 (8) Å
  • b = 9.7095 (6) Å
  • c = 16.7265 (10) Å
  • V = 2148.9 (2) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.84 mm−1
  • T = 293 K
  • 0.27 × 0.25 × 0.18 mm

Data collection

  • Bruker APEXII CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.805, T max = 0.864
  • 9949 measured reflections
  • 1890 independent reflections
  • 1553 reflections with I > 2σ(I)
  • R int = 0.023

Refinement

  • R[F 2 > 2σ(F 2)] = 0.044
  • wR(F 2) = 0.144
  • S = 1.06
  • 1890 reflections
  • 159 parameters
  • H-atom parameters constrained
  • Δρmax = 0.70 e Å−3
  • Δρmin = −0.62 e Å−3

Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT-Plus (Bruker, 2007 [triangle]); data reduction: SAINT-Plus (Bruker, 2007 [triangle]); 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 bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810015758/hy2302sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810015758/hy2302Isup2.hkl

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

Acknowledgments

Financial support from the Natural Science Foundation of Shandong Province (grant No. Q2008B01) and the Independent Innovation Foundation of SDU is gratefully acknowledged.

supplementary crystallographic information

Comment

As has been known for a very long time, 1,10-phenanthroline (phen) is a good bidentate chelating ligand, and has been widely introduced into the transition metal complexes. Here, we present a new six-coordinated cobalt(II) complex based on phen.

The molecular structure of the title compound is shown in Fig. 1. The coordination geometry of the CoII ion is distorted octahedral, in which four positions are occupied by four N atoms of two chelating phen ligands and the other two occupied by two N atoms of two isocyanate ligands at a cis position. The Co—Nphen and Co—Nisocyanate bond lengths are 2.168 (2), 2.223 (3) and 2.058 (3) Å (Table 1), respectively, which are all comparable to those found in other bis(phen)cobalt(II) complexes (Cheng & Hu, 2003; He et al., 2004; Yin, 2007).

Experimental

To a solution of 1,10-phenanthroline monohydrate (39.6 mg, 0.2 mmol) dissolved in methanol (15 ml) was added Co(ClO4)2.6H2O (36.6 mg, 0.1 mmol). The mixture was stirred for 5 min before NaNCO (13 mg, 0.2 mmol) was added. After the stirring process was continued for an additional 5 min, the mixture was filtered, and the filtrate was allowed to slow evaporate to afford orange-yellow crystals suitable for X-ray diffraction with a yield about 55%.

Refinement

H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 Å and with Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. H atoms are omitted for clarity. [Symmetry code: (i) 1-x, y, 3/2-z.]

Crystal data

[Co(CNO)2(C12H8N2)2]F(000) = 1028
Mr = 503.38Dx = 1.556 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 1231 reflections
a = 13.2317 (8) Åθ = 2.6–27.0°
b = 9.7095 (6) ŵ = 0.84 mm1
c = 16.7265 (10) ÅT = 293 K
V = 2148.9 (2) Å3Block, orange-yellow
Z = 40.27 × 0.25 × 0.18 mm

Data collection

Bruker APEXII CCD diffractometer1890 independent reflections
Radiation source: fine-focus sealed tube1553 reflections with I > 2σ(I)
graphiteRint = 0.023
[var phi] and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −15→15
Tmin = 0.805, Tmax = 0.864k = −7→11
9949 measured reflectionsl = −19→19

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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.144H-atom parameters constrained
S = 1.06w = 1/[σ2(Fo2) + (0.0851P)2 + 1.8714P] where P = (Fo2 + 2Fc2)/3
1890 reflections(Δ/σ)max = 0.001
159 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = −0.62 e Å3

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

xyzUiso*/Ueq
Co10.50000.18820 (5)0.75000.0357 (2)
O10.3547 (3)0.4750 (4)0.9117 (2)0.1113 (12)
N10.34514 (17)0.1463 (3)0.71529 (15)0.0407 (6)
N20.51307 (17)0.0223 (3)0.65894 (15)0.0402 (6)
N30.4590 (2)0.3270 (3)0.83709 (18)0.0551 (7)
C10.2633 (3)0.2026 (4)0.7466 (2)0.0519 (9)
H10.27130.27250.78410.062*
C20.1656 (3)0.1624 (4)0.7262 (3)0.0636 (10)
H20.10990.20330.75030.076*
C30.1531 (3)0.0611 (4)0.6696 (3)0.0694 (11)
H30.08860.03230.65530.083*
C40.2379 (2)0.0016 (3)0.6335 (2)0.0507 (8)
C50.2324 (3)−0.1020 (4)0.5729 (3)0.0721 (11)
H50.1695−0.12800.55320.086*
C60.3168 (3)−0.1634 (4)0.5432 (2)0.0705 (11)
H60.3108−0.23260.50500.085*
C70.4141 (3)−0.1225 (4)0.5701 (2)0.0581 (9)
C80.5032 (3)−0.1852 (5)0.5447 (3)0.0720 (14)
H80.5003−0.25740.50820.086*
C90.5947 (3)−0.1417 (5)0.5727 (2)0.0759 (12)
H90.6545−0.18070.55420.091*
C100.5961 (3)−0.0358 (4)0.6307 (2)0.0548 (8)
H100.6583−0.00570.64990.066*
C110.4227 (2)−0.0189 (3)0.62939 (17)0.0402 (7)
C120.3333 (2)0.0450 (3)0.65996 (17)0.0410 (7)
C130.4114 (3)0.4017 (4)0.8731 (2)0.0548 (8)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0293 (4)0.0381 (4)0.0396 (4)0.000−0.0021 (2)0.000
O10.112 (3)0.117 (3)0.105 (3)0.031 (2)0.026 (2)−0.026 (2)
N10.0337 (13)0.0439 (13)0.0446 (14)−0.0007 (11)−0.0062 (11)0.0051 (11)
N20.0395 (13)0.0402 (14)0.0409 (13)0.0017 (10)−0.0029 (10)−0.0013 (11)
N30.0524 (17)0.0535 (16)0.0593 (17)0.0016 (13)0.0047 (15)−0.0093 (14)
C10.0381 (19)0.055 (2)0.062 (2)0.0014 (15)−0.0010 (13)−0.0053 (15)
C20.0308 (17)0.068 (2)0.092 (3)−0.0021 (16)0.0034 (18)0.002 (2)
C30.0423 (19)0.071 (2)0.095 (3)−0.0157 (18)−0.0190 (19)0.004 (2)
C40.0464 (18)0.0461 (17)0.0598 (19)−0.0053 (14)−0.0155 (15)0.0057 (15)
C50.065 (2)0.071 (2)0.080 (3)−0.020 (2)−0.032 (2)−0.004 (2)
C60.080 (3)0.064 (2)0.067 (2)−0.015 (2)−0.021 (2)−0.0126 (19)
C70.070 (2)0.058 (2)0.0467 (18)−0.0031 (18)−0.0113 (17)−0.0070 (16)
C80.073 (3)0.081 (3)0.062 (3)0.0094 (19)−0.0093 (18)−0.032 (2)
C90.073 (3)0.095 (3)0.060 (2)0.021 (2)0.000 (2)−0.030 (2)
C100.0512 (19)0.060 (2)0.0529 (19)0.0070 (16)−0.0040 (15)−0.0139 (16)
C110.0435 (16)0.0374 (15)0.0398 (15)−0.0038 (12)−0.0097 (13)0.0058 (12)
C120.0440 (16)0.0365 (14)0.0426 (15)−0.0042 (12)−0.0106 (13)0.0112 (12)
C130.055 (2)0.0567 (19)0.0525 (19)0.0017 (17)0.0092 (16)−0.0045 (16)

Geometric parameters (Å, °)

Co1—N12.168 (2)C4—C121.403 (4)
Co1—N22.223 (3)C4—C51.430 (5)
Co1—N32.058 (3)C5—C61.360 (6)
O1—C131.220 (4)C5—H50.9300
N1—C11.321 (5)C6—C71.420 (5)
N1—C121.359 (4)C6—H60.9300
N2—C101.322 (4)C7—C81.394 (5)
N2—C111.354 (4)C7—C111.418 (5)
N3—C131.133 (4)C8—C91.365 (6)
C1—C21.393 (5)C8—H80.9300
C1—H10.9300C9—C101.414 (5)
C2—C31.374 (6)C9—H90.9300
C2—H20.9300C10—H100.9300
C3—C41.399 (5)C11—C121.430 (4)
C3—H30.9300
N3i—Co1—N398.13 (17)C4—C3—H3120.1
N3i—Co1—N1100.52 (11)C3—C4—C12117.5 (3)
N3—Co1—N193.64 (11)C3—C4—C5123.8 (3)
N3i—Co1—N1i93.64 (11)C12—C4—C5118.7 (3)
N3—Co1—N1i100.52 (11)C6—C5—C4121.7 (3)
N1—Co1—N1i158.36 (13)C6—C5—H5119.2
N3i—Co1—N288.23 (11)C4—C5—H5119.2
N3—Co1—N2168.55 (10)C5—C6—C7120.4 (4)
N1—Co1—N275.76 (9)C5—C6—H6119.8
N1i—Co1—N288.51 (9)C7—C6—H6119.8
N3i—Co1—N2i168.55 (10)C8—C7—C11117.1 (3)
N3—Co1—N2i88.23 (11)C8—C7—C6123.3 (3)
N1—Co1—N2i88.51 (9)C11—C7—C6119.5 (4)
N1i—Co1—N2i75.76 (9)C9—C8—C7120.7 (4)
N2—Co1—N2i87.17 (13)C9—C8—H8119.6
C1—N1—C12118.3 (3)C7—C8—H8119.6
C1—N1—Co1126.2 (2)C8—C9—C10118.2 (4)
C12—N1—Co1115.26 (19)C8—C9—H9120.9
C10—N2—C11118.5 (3)C10—C9—H9120.9
C10—N2—Co1128.2 (2)N2—C10—C9123.0 (3)
C11—N2—Co1113.28 (19)N2—C10—H10118.5
C13—N3—Co1160.3 (3)C9—C10—H10118.5
N1—C1—C2123.2 (3)N2—C11—C7122.4 (3)
N1—C1—H1118.4N2—C11—C12118.1 (3)
C2—C1—H1118.4C7—C11—C12119.5 (3)
C3—C2—C1118.7 (4)N1—C12—C4122.4 (3)
C3—C2—H2120.6N1—C12—C11117.5 (2)
C1—C2—H2120.6C4—C12—C11120.1 (3)
C2—C3—C4119.8 (3)N3—C13—O1175.3 (4)
C2—C3—H3120.1

Symmetry codes: (i) −x+1, y, −z+3/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2302).

References

  • Bruker (2007). APEX2 and SAINT-Plus Bruker AXS Inc., Madison, Wisconsin, USA.
  • Cheng, Y.-Q. & Hu, M.-L. (2003). Z. Kristallogr. New Cryst. Struct.218, 95–96.
  • He, X., Lu, C.-Z., Yu, Y.-Q., Chen, S.-M., Wu, X.-Y. & Yan, Y. (2004). Z. Anorg. Allg. Chem.630, 1131–1135.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Yin, G.-Q. (2007). Acta Cryst. E63, m1542–m1543.

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