Poly[(3,5-dinitro­benzoato)-μ3-triazolato-cobalt(II)]

Qi, X.-L.

doi:10.1107/S160053680804155X

metal-organic compounds

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Volume 65| Part 1| January 2009| Page m47

doi:10.1107/S160053680804155X

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Poly[(3,5-dinitrobenzoato)-μ₃-triazolato-cobalt(II)]

Xu-Liang Qi ^a ^*

^aLiaocheng Vocational and Technical College, Liaocheng, Shandong, People's Republic of China
^*Correspondence e-mail: q200801@sina.com

(Received 30 November 2008; accepted 8 December 2008; online 13 December 2008)

The title compound, [Co(C₂H₂N₃)(C₇H₃N₂O₆)]_n, was obtained by the reaction of CoCl₂, triazole and 3,5-dinitrobenzoic acid in a 1:1:1 ratio. The Co centre is in a distorted tetrahedral coordination by three N atoms of three different triazole ligands and one O atom of the 3,5-dinitrobenzoate anion.

Related literature

For background, see: Park et al. (2006 ).

Experimental

Crystal data

[Co(C₂H₂N₃)(C₇H₃N₂O₆)]
M_r = 338.11
Monoclinic, P 2₁ /c
a = 11.326 (2) Å
b = 9.4043 (19) Å
c = 10.696 (2) Å
β = 91.22 (3)°
V = 1139.0 (4) Å³
Z = 4
Mo Kα radiation
μ = 1.55 mm⁻¹
T = 296 (2) K
0.14 × 0.12 × 0.10 mm

Data collection

Bruker SMART 1K CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) T_min = 0.812, T_max = 0.861
10929 measured reflections
2602 independent reflections
2256 reflections with I > 2σ(I)
R_int = 0.041

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.060
S = 1.03
2602 reflections
190 parameters
H-atom parameters constrained
Δρ_max = 0.33 e Å⁻³
Δρ_min = −0.36 e Å⁻³

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; 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: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680804155X/bt2826sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680804155X/bt2826Isup2.hkl

checkCIF report

Comment top

The asymmetric unit of the title compound is shown in Fig. 1. Co is four-coordinated by one O atom of a 3,5-dinitrobenzoic acid anion and three triazole N atoms in a tetrahedral geometry. The Co—O/N bond lengths of 1.9510 (13)–2.0396 (16)Å are in the normal range. The triazole and 3,5-dinitrobenzoic acid ligands adopt tridentate and monodentate coordinating modes, respectively. As shown in Figs. 2a and 2b, cobalt ions are connected by triazole ligands to generate a two-dimensional net with the 3,5-dinitrobenzoic acid ligands stacking out of this net. There is not obvious supramolecular interaction between the two-dimensional nets.

Related literature top

For background? a related structure? see: Park et al. (2006).

Experimental top

CoCl₂ (1.0 mmol), 3,5-dinitrobenzoic acid (1 mmol), and triazole (1 mmol) were dissolved in water (10 ml). The solution was heated in a 25 ml Teflon lined reaction vessel at 433 K for ca 3 days and then cooled to room temperature. Purple crystals were obtained in a yield of 85%.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART (Bruker, 2001); data reduction: SAINT (Bruker, 2001); 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: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. An ORTEP view of the asymmetric unit with 50% displacement ellipsoids for non-H atoms. Symmetry codes: (A) -x,y - 1/2,-z + 1/2; (B) x,-y + 1/2,z + 1/2.
	Fig. 2. View of the two-dimensional net.

Poly[(3,5-dinitrobenzoato)-µ₃-triazolato-cobalt(II)] top

Crystal data top

[Co(C₂H₂N₃)(C₇H₃N₂O₆)]	F(000) = 676
M_r = 338.11	D_x = 1.972 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.326 (2) Å	Cell parameters from 8661 reflections
b = 9.4043 (19) Å	θ = 3.4–27.5°
c = 10.696 (2) Å	µ = 1.55 mm⁻¹
β = 91.22 (3)°	T = 296 K
V = 1139.0 (4) Å³	Block, red
Z = 4	0.14 × 0.12 × 0.10 mm

Data collection top

Bruker SMART 1K CCD area-detector diffractometer	2602 independent reflections
Radiation source: rotating anode	2256 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
ω scans	θ_max = 27.5°, θ_min = 3.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −14→14
T_min = 0.812, T_max = 0.861	k = −12→12
10929 measured reflections	l = −13→13

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.060	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0193P)² + 0.8847P] where P = (F_o² + 2F_c²)/3
2602 reflections	(Δ/σ)_max = 0.001
190 parameters	Δρ_max = 0.33 e Å⁻³
0 restraints	Δρ_min = −0.36 e Å⁻³

Crystal data top

[Co(C₂H₂N₃)(C₇H₃N₂O₆)]	V = 1139.0 (4) Å³
M_r = 338.11	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.326 (2) Å	µ = 1.55 mm⁻¹
b = 9.4043 (19) Å	T = 296 K
c = 10.696 (2) Å	0.14 × 0.12 × 0.10 mm
β = 91.22 (3)°

Data collection top

Bruker SMART 1K CCD area-detector diffractometer	2602 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	2256 reflections with I > 2σ(I)
T_min = 0.812, T_max = 0.861	R_int = 0.041
10929 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.060	H-atom parameters constrained
S = 1.03	Δρ_max = 0.33 e Å⁻³
2602 reflections	Δρ_min = −0.36 e Å⁻³
190 parameters

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

	x	y	z	U_iso*/U_eq
C1	−0.01347 (15)	0.35028 (19)	0.25548 (18)	0.0159 (4)
H1	−0.0595	0.3768	0.3226	0.019*
C2	0.10642 (16)	0.24145 (19)	0.14215 (18)	0.0176 (4)
H2	0.1617	0.1761	0.1145	0.021*
C3	0.32087 (15)	0.02322 (19)	0.30024 (19)	0.0187 (4)
C4	0.45442 (15)	0.03032 (19)	0.29392 (19)	0.0174 (4)
C5	0.51022 (16)	−0.0334 (2)	0.19406 (19)	0.0186 (4)
H5	0.4668	−0.0830	0.1335	0.022*
C6	0.52033 (16)	0.1050 (2)	0.38296 (19)	0.0181 (4)
H6	0.4838	0.1486	0.4499	0.022*
C7	0.64177 (16)	0.1134 (2)	0.37020 (19)	0.0185 (4)
C8	0.70035 (16)	0.0510 (2)	0.27338 (19)	0.0199 (4)
H8	0.7819	0.0574	0.2668	0.024*
C9	0.63179 (16)	−0.0217 (2)	0.18643 (19)	0.0195 (4)
Co1	0.10473 (2)	0.09672 (2)	0.39456 (2)	0.01158 (8)
N1	0.05927 (13)	0.23721 (15)	0.25698 (14)	0.0148 (3)
N2	0.06612 (12)	0.34762 (16)	0.07340 (14)	0.0142 (3)
N3	−0.01218 (12)	0.41947 (15)	0.14790 (14)	0.0140 (3)
N4	0.69050 (14)	−0.08206 (18)	0.07799 (17)	0.0236 (4)
N5	0.71165 (14)	0.19524 (18)	0.46234 (16)	0.0217 (4)
O1	0.27667 (11)	0.08348 (14)	0.39657 (14)	0.0209 (3)
O2	0.26354 (12)	−0.03470 (16)	0.21590 (14)	0.0270 (3)
O3	0.79840 (13)	−0.0720 (2)	0.07570 (16)	0.0399 (4)
O4	0.63013 (13)	−0.13889 (16)	−0.00391 (14)	0.0277 (3)
O5	0.65828 (13)	0.25969 (17)	0.54211 (16)	0.0339 (4)
O6	0.81961 (12)	0.19449 (16)	0.45430 (15)	0.0296 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0157 (8)	0.0187 (8)	0.0137 (9)	0.0024 (7)	0.0040 (7)	0.0001 (7)
C2	0.0198 (9)	0.0189 (9)	0.0144 (9)	0.0055 (7)	0.0045 (7)	0.0008 (7)
C3	0.0146 (8)	0.0190 (9)	0.0226 (10)	0.0003 (7)	0.0033 (7)	0.0074 (8)
C4	0.0144 (8)	0.0176 (8)	0.0202 (10)	0.0012 (7)	0.0023 (7)	0.0035 (8)
C5	0.0176 (8)	0.0192 (9)	0.0190 (10)	0.0008 (7)	0.0001 (7)	0.0011 (8)
C6	0.0161 (8)	0.0188 (9)	0.0194 (10)	0.0029 (7)	0.0027 (7)	0.0019 (8)
C7	0.0155 (8)	0.0205 (9)	0.0194 (10)	0.0001 (7)	−0.0015 (7)	0.0034 (8)
C8	0.0135 (8)	0.0246 (9)	0.0217 (10)	0.0032 (8)	0.0020 (7)	0.0050 (8)
C9	0.0188 (9)	0.0214 (9)	0.0184 (10)	0.0058 (8)	0.0044 (7)	0.0024 (8)
Co1	0.01125 (12)	0.01384 (12)	0.00973 (13)	−0.00079 (9)	0.00236 (8)	0.00031 (9)
N1	0.0168 (7)	0.0157 (7)	0.0120 (8)	0.0016 (6)	0.0038 (6)	0.0011 (6)
N2	0.0142 (7)	0.0166 (7)	0.0120 (8)	0.0020 (6)	0.0036 (6)	−0.0009 (6)
N3	0.0129 (7)	0.0174 (7)	0.0117 (8)	0.0025 (6)	0.0036 (6)	−0.0008 (6)
N4	0.0217 (8)	0.0280 (9)	0.0211 (9)	0.0074 (7)	0.0047 (7)	0.0026 (7)
N5	0.0196 (8)	0.0230 (8)	0.0225 (9)	−0.0005 (7)	−0.0021 (7)	0.0034 (7)
O1	0.0128 (6)	0.0242 (7)	0.0260 (8)	0.0001 (5)	0.0055 (5)	−0.0001 (6)
O2	0.0178 (6)	0.0368 (8)	0.0265 (8)	−0.0064 (6)	−0.0004 (6)	0.0003 (7)
O3	0.0182 (7)	0.0697 (12)	0.0321 (10)	0.0115 (8)	0.0057 (6)	−0.0112 (9)
O4	0.0324 (8)	0.0299 (7)	0.0210 (8)	0.0010 (6)	0.0032 (6)	−0.0035 (6)
O5	0.0308 (8)	0.0380 (9)	0.0329 (9)	0.0016 (7)	−0.0004 (7)	−0.0153 (7)
O6	0.0157 (6)	0.0387 (8)	0.0343 (9)	−0.0033 (6)	−0.0041 (6)	0.0045 (7)

Geometric parameters (Å, º) top

C1—N3	1.322 (2)	C7—N5	1.469 (3)
C1—N1	1.345 (2)	C8—C9	1.380 (3)
C1—H1	0.9300	C8—H8	0.9300
C2—N2	1.316 (2)	C9—N4	1.464 (3)
C2—N1	1.350 (2)	Co1—O1	1.9510 (13)
C2—H2	0.9300	Co1—N3ⁱ	2.0158 (15)
C3—O2	1.228 (2)	Co1—N1	2.0356 (16)
C3—O1	1.287 (2)	Co1—N2ⁱⁱ	2.0396 (16)
C3—C4	1.517 (2)	N2—N3	1.381 (2)
C4—C6	1.388 (3)	N2—Co1ⁱⁱⁱ	2.0396 (16)
C4—C5	1.389 (3)	N3—Co1^iv	2.0158 (15)
C5—C9	1.385 (3)	N4—O4	1.223 (2)
C5—H5	0.9300	N4—O3	1.227 (2)
C6—C7	1.387 (3)	N5—O5	1.218 (2)
C6—H6	0.9300	N5—O6	1.228 (2)
C7—C8	1.373 (3)

N3—C1—N1	112.41 (16)	C8—C9—N4	117.87 (16)
N3—C1—H1	123.8	C5—C9—N4	118.99 (18)
N1—C1—H1	123.8	O1—Co1—N3ⁱ	117.64 (6)
N2—C2—N1	113.05 (16)	O1—Co1—N1	106.65 (6)
N2—C2—H2	123.5	N3ⁱ—Co1—N1	104.57 (6)
N1—C2—H2	123.5	O1—Co1—N2ⁱⁱ	103.88 (7)
O2—C3—O1	125.11 (17)	N3ⁱ—Co1—N2ⁱⁱ	107.62 (6)
O2—C3—C4	119.94 (18)	N1—Co1—N2ⁱⁱ	117.09 (6)
O1—C3—C4	114.94 (17)	C1—N1—C2	102.70 (15)
C6—C4—C5	119.94 (17)	C1—N1—Co1	131.85 (13)
C6—C4—C3	120.92 (17)	C2—N1—Co1	125.30 (12)
C5—C4—C3	119.07 (17)	C2—N2—N3	105.55 (15)
C9—C5—C4	118.70 (18)	C2—N2—Co1ⁱⁱⁱ	129.80 (12)
C9—C5—H5	120.7	N3—N2—Co1ⁱⁱⁱ	124.66 (11)
C4—C5—H5	120.7	C1—N3—N2	106.29 (14)
C7—C6—C4	118.76 (18)	C1—N3—Co1^iv	125.99 (12)
C7—C6—H6	120.6	N2—N3—Co1^iv	127.71 (12)
C4—C6—H6	120.6	O4—N4—O3	124.17 (18)
C8—C7—C6	123.08 (18)	O4—N4—C9	118.73 (16)
C8—C7—N5	117.89 (17)	O3—N4—C9	117.10 (17)
C6—C7—N5	119.01 (18)	O5—N5—O6	124.19 (18)
C7—C8—C9	116.48 (17)	O5—N5—C7	117.56 (16)
C7—C8—H8	121.8	O6—N5—C7	118.25 (17)
C9—C8—H8	121.8	C3—O1—Co1	115.13 (12)
C8—C9—C5	123.05 (18)

O2—C3—C4—C6	174.83 (18)	N3ⁱ—Co1—N1—C2	−81.85 (15)
O1—C3—C4—C6	−3.9 (3)	N2ⁱⁱ—Co1—N1—C2	159.19 (14)
O2—C3—C4—C5	−2.1 (3)	N1—C2—N2—N3	0.6 (2)
O1—C3—C4—C5	179.20 (17)	N1—C2—N2—Co1ⁱⁱⁱ	−179.28 (12)
C6—C4—C5—C9	0.6 (3)	N1—C1—N3—N2	0.1 (2)
C3—C4—C5—C9	177.53 (16)	N1—C1—N3—Co1^iv	−178.75 (11)
C5—C4—C6—C7	−0.4 (3)	C2—N2—N3—C1	−0.41 (18)
C3—C4—C6—C7	−177.31 (17)	Co1ⁱⁱⁱ—N2—N3—C1	179.45 (12)
C4—C6—C7—C8	−0.1 (3)	C2—N2—N3—Co1^iv	178.44 (12)
C4—C6—C7—N5	178.47 (17)	Co1ⁱⁱⁱ—N2—N3—Co1^iv	−1.7 (2)
C6—C7—C8—C9	0.4 (3)	C8—C9—N4—O4	−175.39 (17)
N5—C7—C8—C9	−178.19 (16)	C5—C9—N4—O4	1.3 (3)
C7—C8—C9—C5	−0.2 (3)	C8—C9—N4—O3	4.7 (3)
C7—C8—C9—N4	176.34 (17)	C5—C9—N4—O3	−178.66 (18)
C4—C5—C9—C8	−0.3 (3)	C8—C7—N5—O5	174.23 (18)
C4—C5—C9—N4	−176.77 (17)	C6—C7—N5—O5	−4.4 (3)
N3—C1—N1—C2	0.2 (2)	C8—C7—N5—O6	−5.8 (3)
N3—C1—N1—Co1	175.77 (12)	C6—C7—N5—O6	175.59 (17)
N2—C2—N1—C1	−0.5 (2)	O2—C3—O1—Co1	−6.3 (2)
N2—C2—N1—Co1	−176.45 (12)	C4—C3—O1—Co1	172.33 (11)
O1—Co1—N1—C1	−131.24 (16)	N3ⁱ—Co1—O1—C3	48.42 (14)
N3ⁱ—Co1—N1—C1	103.46 (16)	N1—Co1—O1—C3	−68.51 (13)
N2ⁱⁱ—Co1—N1—C1	−15.50 (18)	N2ⁱⁱ—Co1—O1—C3	167.19 (12)
O1—Co1—N1—C2	43.46 (16)

Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2; (iv) −x, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Co(C₂H₂N₃)(C₇H₃N₂O₆)]
M_r	338.11
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	11.326 (2), 9.4043 (19), 10.696 (2)
β (°)	91.22 (3)
V (Å³)	1139.0 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.55
Crystal size (mm)	0.14 × 0.12 × 0.10

Data collection
Diffractometer	Bruker SMART 1K CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.812, 0.861
No. of measured, independent and observed [I > 2σ(I)] reflections	10929, 2602, 2256
R_int	0.041
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.060, 1.03
No. of reflections	2602
No. of parameters	190
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.33, −0.36

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

References

Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Park, H., Moureau, D. M. & Parise, J. B. (2006). Chem. Mater. 18, 525–531. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar