Literature DB >> 24427006

Tetra-kis(μ-2-phenyl-acetato-κ(2) O:O')bis-{[4-(di-methyl-amino)-pyridine-κN (1)]cobalt(II)}.

Meriem Benslimane1, Yasmine Kheira Redjel1, Georges Dénès2, Hocine Merazig1.   

Abstract

The title compound, [Co2(C8H7O2)4(C7H10N2)2], crystallizes as a centrosymmetric dimer containing two Co(II) atoms bridged by four bidentate phenyl-acetate ligands in syn-syn bridging modes. Each Co(II) atom is five-coordinated by four O atoms from four different carboxyl-ate ligands and the ring N atom of a 4-(di-methyl-amino)-pyridine unit, generating a distorted square-pyramidal geometry in which the four O atoms form the basal plane and the N atom occupies the axial position. In the crystal, C-H⋯O inter-actions link the dinuclear complex mol-ecules into a three-dimensional network.

Entities:  

Year:  2013        PMID: 24427006      PMCID: PMC3884428          DOI: 10.1107/S1600536813023258

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For properties of the 4-(di­methyl­amino)­pyridine ligand as a homogeneous catalyst, see: Satgé et al. (2004 ▶). For transition metal complexes of 4-(di­methyl­amino)­pyridine which exhibit luminescence properties, see: Araki et al. (2005 ▶). For biological and magnetic properties of carb­oxy­lic acid complexes of cobalt(II), see: Cotton et al. (1999 ▶). For related centrosymmetric dinuclear cobalt(II) complexes bridged by carboxyl­ates, see: Cui et al. (1999 ▶); Catterick & Thornton (1977 ▶).

Experimental

Crystal data

[Co2(C8H7O2)4(C7H10N2)2] M = 902.74 Triclinic, a = 8.107 (5) Å b = 11.043 (5) Å c = 12.573 (5) Å α = 99.766 (5)° β = 101.878 (5)° γ = 105.335 (5)° V = 1031.9 (9) Å3 Z = 1 Mo Kα radiation μ = 0.86 mm−1 T = 150 K 0.15 × 0.10 × 0.01 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2012 ▶) T min = 0.902, T max = 0.991 9238 measured reflections 3645 independent reflections 3352 reflections with I > 2σ(I)) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.060 S = 1.05 3645 reflections 271 parameters H-atom parameters constrained Δρmax = 0.25 e Å−3 Δρmin = −0.24 e Å−3 Data collection: APEX2 (Bruker, 2012 ▶); cell refinement: SAINT (Bruker, 2012 ▶); data reduction: SAINT; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ▶) and ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536813023258/lr2113sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813023258/lr2113Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co2(C8H7O2)4(C7H10N2)2]Z = 1
Mr = 902.74F(000) = 470
Triclinic, P1Dx = 1.453 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.107 (5) ÅCell parameters from 4872 reflections
b = 11.043 (5) Åθ = 2.3–25°
c = 12.573 (5) ŵ = 0.86 mm1
α = 99.766 (5)°T = 150 K
β = 101.878 (5)°Box, blue
γ = 105.335 (5)°0.15 × 0.1 × 0.01 mm
V = 1031.9 (9) Å3
Bruker APEXII CCD diffractometer3645 independent reflections
Radiation source: fine-focus sealed tube3352 reflections with I > 2σ(I))
Graphite monochromatorRint = 0.019
ω and φ scansθmax = 25.0°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Bruker, 2012)h = −9→9
Tmin = 0.902, Tmax = 0.991k = −13→13
9238 measured reflectionsl = −14→14
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.025w = 1/[σ2(Fo2) + (0.0206P)2 + 0.6871P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.060(Δ/σ)max < 0.001
S = 1.05Δρmax = 0.25 e Å3
3645 reflectionsΔρmin = −0.24 e Å3
271 parameters
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.
xyzUiso*/Ueq
Co10.56888 (3)0.01135 (2)0.114253 (18)0.01603 (8)
O10.70384 (17)0.18802 (11)0.09742 (10)0.0256 (3)
O30.75242 (16)−0.06983 (12)0.07678 (10)0.0241 (3)
O20.59969 (17)0.17191 (12)−0.08452 (10)0.0248 (3)
O40.64516 (17)−0.08060 (13)−0.10383 (10)0.0277 (3)
N10.7414 (2)0.15583 (15)0.63408 (12)0.0259 (3)
N20.64381 (19)0.06270 (13)0.28539 (11)0.0178 (3)
C100.7997 (2)0.46694 (16)0.12315 (14)0.0192 (4)
C30.7158 (2)−0.00546 (16)0.34964 (14)0.0197 (4)
H30.7415−0.07640.31390.024*
C110.7164 (3)0.55861 (17)0.10444 (16)0.0256 (4)
H110.66610.55990.03130.031*
C10.7158 (2)0.12779 (17)0.52207 (14)0.0195 (4)
C180.8183 (2)−0.25048 (16)−0.17600 (14)0.0181 (4)
C130.7818 (3)0.64805 (18)0.30092 (16)0.0302 (4)
H130.77660.70850.36030.036*
C170.8651 (2)−0.18185 (17)−0.05447 (14)0.0205 (4)
H17A0.9855−0.1236−0.03380.025*
H17B0.8624−0.2454−0.00970.025*
C230.9124 (2)−0.20046 (17)−0.24739 (15)0.0222 (4)
H231.0052−0.1233−0.22020.027*
C20.7540 (2)0.02208 (17)0.46401 (14)0.0216 (4)
H20.8051−0.02890.50330.026*
C190.6790 (2)−0.36483 (17)−0.21909 (15)0.0245 (4)
H190.6135−0.399−0.17240.029*
C90.8102 (3)0.37074 (16)0.02588 (15)0.0236 (4)
H9A0.93240.37170.03580.028*
H9B0.77540.3982−0.04240.028*
C140.8655 (3)0.55707 (19)0.32101 (16)0.0311 (4)
H140.91630.55630.39420.037*
C40.6139 (2)0.16674 (17)0.34079 (14)0.0228 (4)
H40.5680.21790.2990.027*
C150.8741 (2)0.46726 (18)0.23306 (15)0.0267 (4)
H150.93030.40630.24760.032*
C50.6466 (2)0.20198 (17)0.45452 (15)0.0246 (4)
H50.62310.27530.48760.029*
C220.8696 (3)−0.26441 (19)−0.35918 (15)0.0274 (4)
H220.934−0.23−0.40620.033*
C160.7435 (2)−0.10501 (16)−0.02568 (14)0.0180 (4)
C200.6361 (3)−0.42857 (18)−0.33028 (16)0.0291 (4)
H200.5425−0.5053−0.35790.035*
C120.7061 (3)0.64871 (18)0.19226 (17)0.0322 (5)
H120.64870.70910.1780.039*
C80.6943 (2)0.23260 (16)0.01192 (14)0.0186 (4)
C70.8177 (3)0.0810 (2)0.70317 (16)0.0328 (5)
H7A0.82560.11520.78020.049*
H7B0.93410.08580.69460.049*
H7C0.7438−0.00760.68040.049*
C210.7319 (3)−0.37875 (19)−0.40079 (15)0.0292 (4)
H210.7037−0.4219−0.47560.035*
C60.6940 (3)0.2633 (2)0.68950 (16)0.0353 (5)
H6A0.7210.26930.76860.053*
H6B0.56940.24930.66110.053*
H6C0.76010.34210.67540.053*
U11U22U33U12U13U23
Co10.02007 (13)0.01633 (13)0.01213 (12)0.00678 (9)0.00475 (9)0.00211 (9)
O10.0329 (7)0.0188 (6)0.0213 (7)0.0030 (5)0.0044 (6)0.0066 (5)
O30.0262 (7)0.0258 (7)0.0218 (7)0.0115 (5)0.0093 (5)0.0010 (5)
O20.0293 (7)0.0213 (6)0.0190 (6)0.0020 (5)0.0056 (6)0.0022 (5)
O40.0278 (7)0.0354 (8)0.0261 (7)0.0202 (6)0.0074 (6)0.0073 (6)
N10.0366 (9)0.0275 (8)0.0140 (7)0.0111 (7)0.0067 (7)0.0044 (6)
N20.0212 (7)0.0178 (7)0.0146 (7)0.0072 (6)0.0048 (6)0.0029 (6)
C100.0187 (9)0.0152 (8)0.0212 (9)0.0001 (7)0.0075 (7)0.0034 (7)
C30.0234 (9)0.0163 (8)0.0209 (9)0.0086 (7)0.0065 (7)0.0030 (7)
C110.0319 (10)0.0201 (9)0.0238 (9)0.0060 (8)0.0054 (8)0.0080 (8)
C10.0196 (9)0.0213 (9)0.0160 (8)0.0035 (7)0.0054 (7)0.0040 (7)
C180.0181 (8)0.0187 (9)0.0209 (9)0.0111 (7)0.0059 (7)0.0041 (7)
C130.0418 (12)0.0204 (9)0.0283 (10)0.0084 (9)0.0156 (9)0.0003 (8)
C170.0190 (9)0.0212 (9)0.0213 (9)0.0081 (7)0.0052 (7)0.0023 (7)
C230.0182 (9)0.0231 (9)0.0252 (9)0.0068 (7)0.0047 (7)0.0066 (8)
C20.0265 (10)0.0217 (9)0.0196 (9)0.0109 (8)0.0055 (7)0.0085 (7)
C190.0248 (10)0.0238 (9)0.0256 (10)0.0062 (8)0.0090 (8)0.0068 (8)
C90.0301 (10)0.0185 (9)0.0221 (9)0.0041 (8)0.0114 (8)0.0047 (7)
C140.0390 (12)0.0316 (11)0.0200 (9)0.0107 (9)0.0046 (9)0.0034 (8)
C40.0330 (10)0.0216 (9)0.0180 (9)0.0151 (8)0.0061 (8)0.0057 (7)
C150.0289 (10)0.0255 (10)0.0270 (10)0.0132 (8)0.0043 (8)0.0059 (8)
C50.0346 (11)0.0213 (9)0.0199 (9)0.0144 (8)0.0069 (8)0.0016 (7)
C220.0283 (10)0.0366 (11)0.0224 (10)0.0131 (9)0.0097 (8)0.0117 (8)
C160.0165 (8)0.0139 (8)0.0234 (9)0.0029 (7)0.0081 (7)0.0030 (7)
C200.0277 (10)0.0222 (9)0.0285 (10)0.0035 (8)0.0000 (8)−0.0017 (8)
C120.0420 (12)0.0205 (10)0.0393 (12)0.0154 (9)0.0124 (10)0.0098 (9)
C80.0189 (9)0.0179 (9)0.0208 (9)0.0070 (7)0.0089 (7)0.0026 (7)
C70.0410 (12)0.0410 (12)0.0191 (10)0.0146 (10)0.0071 (9)0.0124 (9)
C210.0347 (11)0.0350 (11)0.0169 (9)0.0160 (9)0.0022 (8)0.0006 (8)
C60.0547 (14)0.0327 (11)0.0196 (10)0.0140 (10)0.0148 (9)0.0022 (8)
Co1—O32.0224 (15)C13—H130.93
Co1—O12.0382 (14)C17—C161.519 (2)
Co1—O2i2.0429 (15)C17—H17A0.97
Co1—N22.0460 (16)C17—H17B0.97
Co1—O4i2.0628 (16)C23—C221.388 (3)
Co1—Co1i2.8020 (12)C23—H230.93
O1—C81.253 (2)C2—H20.93
O3—C161.262 (2)C19—C201.381 (3)
O2—C81.256 (2)C19—H190.93
O2—Co1i2.0429 (15)C9—C81.524 (2)
O4—C161.247 (2)C9—H9A0.97
O4—Co1i2.0628 (16)C9—H9B0.97
N1—C11.349 (2)C14—C151.381 (3)
N1—C61.453 (2)C14—H140.93
N1—C71.454 (2)C4—C51.366 (2)
N2—C31.343 (2)C4—H40.93
N2—C41.345 (2)C15—H150.93
C10—C111.383 (3)C5—H50.93
C10—C151.388 (3)C22—C211.380 (3)
C10—C91.510 (2)C22—H220.93
C3—C21.369 (2)C20—C211.384 (3)
C3—H30.93C20—H200.93
C11—C121.387 (3)C12—H120.93
C11—H110.93C7—H7A0.96
C1—C21.410 (2)C7—H7B0.96
C1—C51.411 (2)C7—H7C0.96
C18—C231.386 (2)C21—H210.93
C18—C191.388 (3)C6—H6A0.96
C18—C171.506 (2)C6—H6B0.96
C13—C121.380 (3)C6—H6C0.96
C13—C141.382 (3)
O3—Co1—O193.27 (6)C3—C2—H2120.1
O3—Co1—O2i87.33 (6)C1—C2—H2120.1
O1—Co1—O2i163.77 (5)C20—C19—C18120.91 (17)
O3—Co1—N2102.92 (6)C20—C19—H19119.5
O1—Co1—N294.29 (5)C18—C19—H19119.5
O2i—Co1—N2101.39 (5)C10—C9—C8114.21 (14)
O3—Co1—O4i163.73 (5)C10—C9—H9A108.7
O1—Co1—O4i85.64 (6)C8—C9—H9A108.7
O2i—Co1—O4i89.27 (7)C10—C9—H9B108.7
N2—Co1—O4i93.35 (5)C8—C9—H9B108.7
O3—Co1—Co1i89.34 (4)H9A—C9—H9B107.6
O1—Co1—Co1i79.04 (4)C15—C14—C13120.40 (18)
O2i—Co1—Co1i84.75 (4)C15—C14—H14119.8
N2—Co1—Co1i166.44 (4)C13—C14—H14119.8
O4i—Co1—Co1i74.50 (4)N2—C4—C5124.16 (16)
C8—O1—Co1129.17 (11)N2—C4—H4117.9
C16—O3—Co1116.62 (11)C5—C4—H4117.9
C8—O2—Co1i121.65 (11)C14—C15—C10120.78 (17)
C16—O4—Co1i133.30 (12)C14—C15—H15119.6
C1—N1—C6120.56 (16)C10—C15—H15119.6
C1—N1—C7121.55 (16)C4—C5—C1120.39 (16)
C6—N1—C7117.89 (15)C4—C5—H5119.8
C3—N2—C4115.61 (15)C1—C5—H5119.8
C3—N2—Co1124.00 (11)C21—C22—C23120.28 (18)
C4—N2—Co1120.31 (11)C21—C22—H22119.9
C11—C10—C15118.12 (17)C23—C22—H22119.9
C11—C10—C9120.35 (16)O4—C16—O3125.35 (16)
C15—C10—C9121.52 (16)O4—C16—C17118.12 (15)
N2—C3—C2124.67 (16)O3—C16—C17116.52 (15)
N2—C3—H3117.7C19—C20—C21120.23 (18)
C2—C3—H3117.7C19—C20—H20119.9
C10—C11—C12121.52 (18)C21—C20—H20119.9
C10—C11—H11119.2C13—C12—C11119.52 (18)
C12—C11—H11119.2C13—C12—H12120.2
N1—C1—C2122.71 (16)C11—C12—H12120.2
N1—C1—C5122.05 (16)O1—C8—O2125.30 (16)
C2—C1—C5115.23 (16)O1—C8—C9117.19 (15)
C23—C18—C19118.53 (16)O2—C8—C9117.50 (15)
C23—C18—C17120.81 (16)N1—C7—H7A109.5
C19—C18—C17120.66 (16)N1—C7—H7B109.5
C12—C13—C14119.66 (18)H7A—C7—H7B109.5
C12—C13—H13120.2N1—C7—H7C109.5
C14—C13—H13120.2H7A—C7—H7C109.5
C18—C17—C16114.52 (14)H7B—C7—H7C109.5
C18—C17—H17A108.6C22—C21—C20119.40 (17)
C16—C17—H17A108.6C22—C21—H21120.3
C18—C17—H17B108.6C20—C21—H21120.3
C16—C17—H17B108.6N1—C6—H6A109.5
H17A—C17—H17B107.6N1—C6—H6B109.5
C18—C23—C22120.65 (17)H6A—C6—H6B109.5
C18—C23—H23119.7N1—C6—H6C109.5
C22—C23—H23119.7H6A—C6—H6C109.5
C3—C2—C1119.85 (16)H6B—C6—H6C109.5
D—H···AD—HH···AD···AD—H···A
C6—H6A···O2ii0.962.533.337 (3)142
C23—H23···O3iii0.932.583.469 (3)159
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A DA D—H⋯A
C6—H6A⋯O2i 0.962.533.337 (3)142
C23—H23⋯O3ii 0.932.583.469 (3)159

Symmetry codes: (i) ; (ii) .

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