metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Bis(iso­cyanato-κN)bis­­(1,10-phenanthroline-κ2N,N′)cobalt(II)

aSchool of Chemistry & Chemical Technology, Shandong University, Jinan 250100, People's Republic of China
*Correspondence e-mail: sdzhangxm@126.com

(Received 22 April 2010; accepted 28 April 2010; online 8 May 2010)

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[Cheng, Y.-Q. & Hu, M.-L. (2003). Z. Kristallogr. New Cryst. Struct. 218, 95-96.]); He et al. (2004[He, X., Lu, C.-Z., Yu, Y.-Q., Chen, S.-M., Wu, X.-Y. & Yan, Y. (2004). Z. Anorg. Allg. Chem. 630, 1131-1135.]); Yin (2007[Yin, G.-Q. (2007). Acta Cryst. E63, m1542-m1543.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(CNO)2(C12H8N2)2]

  • Mr = 503.38

  • Orthorhombic, P b c n

  • 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[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.805, Tmax = 0.864

  • 9949 measured reflections

  • 1890 independent reflections

  • 1553 reflections with I > 2σ(I)

  • Rint = 0.023

Refinement
  • R[F2 > 2σ(F2)] = 0.044

  • wR(F2) = 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

Table 1
Selected bond lengths (Å)

Co1—N1 2.168 (2)
Co1—N2 2.223 (3)
Co1—N3 2.058 (3)

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

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).

Related literature top

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

Experimental top

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 top

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

Structure description top

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).

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

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); 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).

Figures top
[Figure 1] 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.]
Bis(isocyanato-κN)bis(1,10-phenanthroline- κ2N,N')cobalt(II) top
Crystal data top
[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 top
Bruker APEXII CCD
diffractometer
1890 independent reflections
Radiation source: fine-focus sealed tube1553 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1515
Tmin = 0.805, Tmax = 0.864k = 711
9949 measured reflectionsl = 1919
Refinement top
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 = 1.06 w = 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
Crystal data top
[Co(CNO)2(C12H8N2)2]V = 2148.9 (2) Å3
Mr = 503.38Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 13.2317 (8) ŵ = 0.84 mm1
b = 9.7095 (6) ÅT = 293 K
c = 16.7265 (10) Å0.27 × 0.25 × 0.18 mm
Data collection top
Bruker APEXII CCD
diffractometer
1890 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
1553 reflections with I > 2σ(I)
Tmin = 0.805, Tmax = 0.864Rint = 0.023
9949 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.144H-atom parameters constrained
S = 1.06Δρmax = 0.70 e Å3
1890 reflectionsΔρmin = 0.62 e Å3
159 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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)
H50.16950.12800.55320.086*
C60.3168 (3)0.1634 (4)0.5432 (2)0.0705 (11)
H60.31080.23260.50500.085*
C70.4141 (3)0.1225 (4)0.5701 (2)0.0581 (9)
C80.5032 (3)0.1852 (5)0.5447 (3)0.0720 (14)
H80.50030.25740.50820.086*
C90.5947 (3)0.1417 (5)0.5727 (2)0.0759 (12)
H90.65450.18070.55420.091*
C100.5961 (3)0.0358 (4)0.6307 (2)0.0548 (8)
H100.65830.00570.64990.066*
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) top
U11U22U33U12U13U23
Co10.0293 (4)0.0381 (4)0.0396 (4)0.0000.0021 (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, º) top
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 code: (i) x+1, y, z+3/2.

Experimental details

Crystal data
Chemical formula[Co(CNO)2(C12H8N2)2]
Mr503.38
Crystal system, space groupOrthorhombic, Pbcn
Temperature (K)293
a, b, c (Å)13.2317 (8), 9.7095 (6), 16.7265 (10)
V3)2148.9 (2)
Z4
Radiation typeMo Kα
µ (mm1)0.84
Crystal size (mm)0.27 × 0.25 × 0.18
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.805, 0.864
No. of measured, independent and
observed [I > 2σ(I)] reflections
9949, 1890, 1553
Rint0.023
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.144, 1.06
No. of reflections1890
No. of parameters159
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.70, 0.62

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Co1—N12.168 (2)Co1—N32.058 (3)
Co1—N22.223 (3)
 

Acknowledgements

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

References

First citationBruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationCheng, Y.-Q. & Hu, M.-L. (2003). Z. Kristallogr. New Cryst. Struct. 218, 95–96.  CAS Google Scholar
First citationHe, X., Lu, C.-Z., Yu, Y.-Q., Chen, S.-M., Wu, X.-Y. & Yan, Y. (2004). Z. Anorg. Allg. Chem. 630, 1131–1135.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationYin, G.-Q. (2007). Acta Cryst. E63, m1542–m1543.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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