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

Dao-Peng Zhang; Nai-Chang Tian; Xiao-Mei Zhang

doi:10.1107/S1600536810015758

. 2010 May 8;66(Pt 6):m614. doi: 10.1107/S1600536810015758

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

Dao-Peng Zhang ^a, Nai-Chang Tian ^a, Xiao-Mei Zhang ^a,^*

PMCID: PMC2979601 PMID: 21579273

Abstract

In the title complex, [Co(NCO)₂(C₁₂H₈N₂)₂], the Co^II 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 ▶); He et al. (2004 ▶); Yin (2007 ▶).

Experimental

Crystal data

[Co(CNO)₂(C₁₂H₈N₂)₂]
M _r = 503.38
Orthorhombic,
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 ▶) 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
Δρ_max = 0.70 e Å⁻³
Δρ_min = −0.62 e Å⁻³

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.

Supplementary Material

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

e-66-0m614-sup1.cif^{(14.1KB, cif)}

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

e-66-0m614-Isup2.hkl^{(93.1KB, hkl)}

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

Table 1. Selected bond lengths (Å).

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

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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 Co^II 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—N_phen and Co—N_isocyanate 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%.

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
M_r = 503.38	D_x = 1.556 Mg m⁻³
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2ab	Cell parameters from 1231 reflections
a = 13.2317 (8) Å	θ = 2.6–27.0°
b = 9.7095 (6) Å	µ = 0.84 mm⁻¹
c = 16.7265 (10) Å	T = 293 K
V = 2148.9 (2) Å³	Block, orange-yellow
Z = 4	0.27 × 0.25 × 0.18 mm

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Data collection

Bruker APEXII CCD diffractometer	1890 independent reflections
Radiation source: fine-focus sealed tube	1553 reflections with I > 2σ(I)
graphite	R_int = 0.023
φ and ω scans	θ_max = 25.0°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→15
T_min = 0.805, T_max = 0.864	k = −7→11
9949 measured reflections	l = −19→19

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Refinement

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.144	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0851P)² + 1.8714P] where P = (F_o² + 2F_c²)/3
1890 reflections	(Δ/σ)_max = 0.001
159 parameters	Δρ_max = 0.70 e Å⁻³
0 restraints	Δρ_min = −0.62 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Co1	0.5000	0.18820 (5)	0.7500	0.0357 (2)
O1	0.3547 (3)	0.4750 (4)	0.9117 (2)	0.1113 (12)
N1	0.34514 (17)	0.1463 (3)	0.71529 (15)	0.0407 (6)
N2	0.51307 (17)	0.0223 (3)	0.65894 (15)	0.0402 (6)
N3	0.4590 (2)	0.3270 (3)	0.83709 (18)	0.0551 (7)
C1	0.2633 (3)	0.2026 (4)	0.7466 (2)	0.0519 (9)
H1	0.2713	0.2725	0.7841	0.062*
C2	0.1656 (3)	0.1624 (4)	0.7262 (3)	0.0636 (10)
H2	0.1099	0.2033	0.7503	0.076*
C3	0.1531 (3)	0.0611 (4)	0.6696 (3)	0.0694 (11)
H3	0.0886	0.0323	0.6553	0.083*
C4	0.2379 (2)	0.0016 (3)	0.6335 (2)	0.0507 (8)
C5	0.2324 (3)	−0.1020 (4)	0.5729 (3)	0.0721 (11)
H5	0.1695	−0.1280	0.5532	0.086*
C6	0.3168 (3)	−0.1634 (4)	0.5432 (2)	0.0705 (11)
H6	0.3108	−0.2326	0.5050	0.085*
C7	0.4141 (3)	−0.1225 (4)	0.5701 (2)	0.0581 (9)
C8	0.5032 (3)	−0.1852 (5)	0.5447 (3)	0.0720 (14)
H8	0.5003	−0.2574	0.5082	0.086*
C9	0.5947 (3)	−0.1417 (5)	0.5727 (2)	0.0759 (12)
H9	0.6545	−0.1807	0.5542	0.091*
C10	0.5961 (3)	−0.0358 (4)	0.6307 (2)	0.0548 (8)
H10	0.6583	−0.0057	0.6499	0.066*
C11	0.4227 (2)	−0.0189 (3)	0.62939 (17)	0.0402 (7)
C12	0.3333 (2)	0.0450 (3)	0.65996 (17)	0.0410 (7)
C13	0.4114 (3)	0.4017 (4)	0.8731 (2)	0.0548 (8)

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Atomic displacement parameters (Å²)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0293 (4)	0.0381 (4)	0.0396 (4)	0.000	−0.0021 (2)	0.000
O1	0.112 (3)	0.117 (3)	0.105 (3)	0.031 (2)	0.026 (2)	−0.026 (2)
N1	0.0337 (13)	0.0439 (13)	0.0446 (14)	−0.0007 (11)	−0.0062 (11)	0.0051 (11)
N2	0.0395 (13)	0.0402 (14)	0.0409 (13)	0.0017 (10)	−0.0029 (10)	−0.0013 (11)
N3	0.0524 (17)	0.0535 (16)	0.0593 (17)	0.0016 (13)	0.0047 (15)	−0.0093 (14)
C1	0.0381 (19)	0.055 (2)	0.062 (2)	0.0014 (15)	−0.0010 (13)	−0.0053 (15)
C2	0.0308 (17)	0.068 (2)	0.092 (3)	−0.0021 (16)	0.0034 (18)	0.002 (2)
C3	0.0423 (19)	0.071 (2)	0.095 (3)	−0.0157 (18)	−0.0190 (19)	0.004 (2)
C4	0.0464 (18)	0.0461 (17)	0.0598 (19)	−0.0053 (14)	−0.0155 (15)	0.0057 (15)
C5	0.065 (2)	0.071 (2)	0.080 (3)	−0.020 (2)	−0.032 (2)	−0.004 (2)
C6	0.080 (3)	0.064 (2)	0.067 (2)	−0.015 (2)	−0.021 (2)	−0.0126 (19)
C7	0.070 (2)	0.058 (2)	0.0467 (18)	−0.0031 (18)	−0.0113 (17)	−0.0070 (16)
C8	0.073 (3)	0.081 (3)	0.062 (3)	0.0094 (19)	−0.0093 (18)	−0.032 (2)
C9	0.073 (3)	0.095 (3)	0.060 (2)	0.021 (2)	0.000 (2)	−0.030 (2)
C10	0.0512 (19)	0.060 (2)	0.0529 (19)	0.0070 (16)	−0.0040 (15)	−0.0139 (16)
C11	0.0435 (16)	0.0374 (15)	0.0398 (15)	−0.0038 (12)	−0.0097 (13)	0.0058 (12)
C12	0.0440 (16)	0.0365 (14)	0.0426 (15)	−0.0042 (12)	−0.0106 (13)	0.0112 (12)
C13	0.055 (2)	0.0567 (19)	0.0525 (19)	0.0017 (17)	0.0092 (16)	−0.0045 (16)

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Geometric parameters (Å, °)

Co1—N1	2.168 (2)	C4—C12	1.403 (4)
Co1—N2	2.223 (3)	C4—C5	1.430 (5)
Co1—N3	2.058 (3)	C5—C6	1.360 (6)
O1—C13	1.220 (4)	C5—H5	0.9300
N1—C1	1.321 (5)	C6—C7	1.420 (5)
N1—C12	1.359 (4)	C6—H6	0.9300
N2—C10	1.322 (4)	C7—C8	1.394 (5)
N2—C11	1.354 (4)	C7—C11	1.418 (5)
N3—C13	1.133 (4)	C8—C9	1.365 (6)
C1—C2	1.393 (5)	C8—H8	0.9300
C1—H1	0.9300	C9—C10	1.414 (5)
C2—C3	1.374 (6)	C9—H9	0.9300
C2—H2	0.9300	C10—H10	0.9300
C3—C4	1.399 (5)	C11—C12	1.430 (4)
C3—H3	0.9300

N3ⁱ—Co1—N3	98.13 (17)	C4—C3—H3	120.1
N3ⁱ—Co1—N1	100.52 (11)	C3—C4—C12	117.5 (3)
N3—Co1—N1	93.64 (11)	C3—C4—C5	123.8 (3)
N3ⁱ—Co1—N1ⁱ	93.64 (11)	C12—C4—C5	118.7 (3)
N3—Co1—N1ⁱ	100.52 (11)	C6—C5—C4	121.7 (3)
N1—Co1—N1ⁱ	158.36 (13)	C6—C5—H5	119.2
N3ⁱ—Co1—N2	88.23 (11)	C4—C5—H5	119.2
N3—Co1—N2	168.55 (10)	C5—C6—C7	120.4 (4)
N1—Co1—N2	75.76 (9)	C5—C6—H6	119.8
N1ⁱ—Co1—N2	88.51 (9)	C7—C6—H6	119.8
N3ⁱ—Co1—N2ⁱ	168.55 (10)	C8—C7—C11	117.1 (3)
N3—Co1—N2ⁱ	88.23 (11)	C8—C7—C6	123.3 (3)
N1—Co1—N2ⁱ	88.51 (9)	C11—C7—C6	119.5 (4)
N1ⁱ—Co1—N2ⁱ	75.76 (9)	C9—C8—C7	120.7 (4)
N2—Co1—N2ⁱ	87.17 (13)	C9—C8—H8	119.6
C1—N1—C12	118.3 (3)	C7—C8—H8	119.6
C1—N1—Co1	126.2 (2)	C8—C9—C10	118.2 (4)
C12—N1—Co1	115.26 (19)	C8—C9—H9	120.9
C10—N2—C11	118.5 (3)	C10—C9—H9	120.9
C10—N2—Co1	128.2 (2)	N2—C10—C9	123.0 (3)
C11—N2—Co1	113.28 (19)	N2—C10—H10	118.5
C13—N3—Co1	160.3 (3)	C9—C10—H10	118.5
N1—C1—C2	123.2 (3)	N2—C11—C7	122.4 (3)
N1—C1—H1	118.4	N2—C11—C12	118.1 (3)
C2—C1—H1	118.4	C7—C11—C12	119.5 (3)
C3—C2—C1	118.7 (4)	N1—C12—C4	122.4 (3)
C3—C2—H2	120.6	N1—C12—C11	117.5 (2)
C1—C2—H2	120.6	C4—C12—C11	120.1 (3)
C2—C3—C4	119.8 (3)	N3—C13—O1	175.3 (4)
C2—C3—H3	120.1

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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. [DOI] [PubMed]
Yin, G.-Q. (2007). Acta Cryst. E63, m1542–m1543.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

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

e-66-0m614-sup1.cif^{(14.1KB, cif)}

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

e-66-0m614-Isup2.hkl^{(93.1KB, hkl)}

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

[bb1] Bruker (2007). APEX2 and SAINT-Plus Bruker AXS Inc., Madison, Wisconsin, USA.

[bb2] Cheng, Y.-Q. & Hu, M.-L. (2003). Z. Kristallogr. New Cryst. Struct.218, 95–96.

[bb3] He, X., Lu, C.-Z., Yu, Y.-Q., Chen, S.-M., Wu, X.-Y. & Yan, Y. (2004). Z. Anorg. Allg. Chem.630, 1131–1135.

[bb4] Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.

[bb5] Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]

[bb6] Yin, G.-Q. (2007). Acta Cryst. E63, m1542–m1543.

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

Dao-Peng Zhang

Nai-Chang Tian

Xiao-Mei Zhang

Abstract

Related literature

Experimental

Crystal data

Data collection

Refinement

Supplementary Material

Table 1. Selected bond lengths (Å).

Acknowledgments

supplementary crystallographic information

Comment

Experimental

Refinement

Figures

Fig. 1.

Crystal data

Data collection

Refinement

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

Atomic displacement parameters (Å²)

Geometric parameters (Å, °)

Footnotes

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

Cite

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PERMALINK

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

Dao-Peng Zhang

Nai-Chang Tian

Xiao-Mei Zhang

Abstract

Related literature

Experimental

Crystal data

Data collection

Refinement

Supplementary Material

Table 1. Selected bond lengths (Å).

Acknowledgments

supplementary crystallographic information

Comment

Experimental

Refinement

Figures

Fig. 1.

Crystal data

Data collection

Refinement

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

Atomic displacement parameters (Å2)

Geometric parameters (Å, °)

Footnotes

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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

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

Atomic displacement parameters (Å²)