Literature DB >> 21580850

catena-Poly[[bis-(3,5-dicarboxy-benzo-ato)cobalt(II)]-μ-4,4'-bipyridine].

Chun-Sheng Ling, Qiu-Xia Han.   

Abstract

In the title compound, [Co(C(9)H(5)O(6))(2)(C(10)H(8)N(2))](n), the asymmetric unit consists of one n class="Chemical">Co(2+) ion with site symmetry 2, one mono-deprotonated 1,3,5-benzene-tricarboxylic acid anion and one-half of a 4,4'-bipyridine (4,4'-bipy) mol-ecule, in which two N and two C atoms have site symmetry 2. In the crystal structure, the Co(2+) centre is coordinated by four O atoms from two bidentate carboxyl-ate groups of two anions and two N atoms of two 4,4'-bipy mol-ecules, resulting in infinite chains propagating in [010]. The cobalt coordination is distorted trans-CoO(4)N(2) octa-hedral and inter-chain O-H⋯O hydrogen bonds complete the structure.

Entities:  

Year:  2008        PMID： 21580850      PMCID： PMC2959783          DOI： 10.1107/S1600536808032558

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


Related literature

For background, see: Feller et al. (2007 ▶); Brown et al. (2008 ▶).

Experimental

Crystal data

[Co(C9H5O6)2(C10n class="Species">H8N2)] M = 633.37 Monoclinic, a = 10.6682 (7) Å b = 11.0490 (7) Å c = 22.6563 (14) Å β = 101.401 (1)° V = 2617.9 (3) Å3 Z = 4 Mo Kα radiation μ = 0.73 mm−1 T = 293 (2) K 0.18 × 0.15 × 0.13 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2001 ▶) T min = 0.880, T max = 0.911 7123 measured reflections 2579 independent reflections 2051 reflections with I > 2σ(I) R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.038 wR(F 2) = 0.098 S = 1.02 2579 reflections 197 parameters 7 restraints H-atom parameters constrained Δρmax = 0.30 e Å−3 Δρmin = −0.73 e Å−3 Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAIn class="Chemical">NT-Plus); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2003 ▶); software used to prepare material for publication: PLATON. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808032558/hb2815sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808032558/hb2815Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C9H5O6)2(C10H8N2)]F(000) = 1292
Mr = 633.37Dx = 1.607 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1750 reflections
a = 10.6682 (7) Åθ = 2.7–25.9°
b = 11.0490 (7) ŵ = 0.73 mm−1
c = 22.6563 (14) ÅT = 293 K
β = 101.401 (1)°Block, purple
V = 2617.9 (3) Å30.18 × 0.15 × 0.13 mm
Z = 4
Bruker SMART CCD diffractometer2579 independent reflections
Radiation source: fine-focus sealed tube2051 reflections with I > 2σ(I)
graphiteRint = 0.031
ω scansθmax = 26.0°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)h = −13→13
Tmin = 0.880, Tmax = 0.911k = −13→13
7123 measured reflectionsl = −27→15
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: difmap and geom
wR(F2) = 0.098H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0508P)2 + 1.9201P] where P = (Fo2 + 2Fc2)/3
2579 reflections(Δ/σ)max = 0.001
197 parametersΔρmax = 0.31 e Å−3
7 restraintsΔρmin = −0.73 e Å−3
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
Co10.50000.64801 (3)0.25000.01788 (9)
O10.60733 (12)0.64666 (13)0.18575 (6)0.0280 (3)
O20.40351 (13)0.65638 (14)0.14327 (6)0.0347 (4)
O30.30786 (17)0.7752 (2)−0.06851 (8)0.0661 (6)
H30.25230.7863−0.09820.099*
O40.39825 (18)0.6736 (2)−0.13349 (8)0.0692 (6)
O50.85792 (15)0.55679 (17)−0.04477 (7)0.0509 (5)
H50.92870.5390−0.04390.076*
O60.91135 (16)0.5199 (2)0.05406 (8)0.0591 (6)
N10.50000.4678 (2)0.25000.0232 (4)
N20.5000−0.1726 (2)0.25000.0274 (6)
C10.55508 (19)0.64578 (18)0.07857 (9)0.0281 (5)
C20.67509 (19)0.60572 (19)0.07160 (9)0.0298 (5)
H20.73600.58430.10530.036*
C30.70461 (19)0.5975 (2)0.01464 (10)0.0306 (5)
C40.6137 (2)0.6293 (2)−0.03605 (10)0.0338 (5)
H40.63260.6222−0.07420.041*
C50.4946 (2)0.6717 (2)−0.02928 (10)0.0329 (5)
C60.4664 (2)0.6797 (2)0.02785 (10)0.0327 (5)
H60.38670.70840.03220.039*
C70.51892 (19)0.65013 (18)0.13895 (9)0.0265 (5)
C80.8332 (2)0.5551 (2)0.00808 (10)0.0362 (6)
C90.3971 (2)0.7059 (2)−0.08302 (10)0.0392 (6)
C100.4034 (2)0.40519 (19)0.21766 (10)0.0321 (5)
H100.33560.44770.19470.039*
C110.3993 (2)0.28136 (19)0.21669 (10)0.0330 (5)
H110.32950.24140.19380.040*
C120.50000.2156 (3)0.25000.0284 (7)
C130.50000.0812 (3)0.25000.0269 (7)
C140.38822 (19)0.01470 (19)0.23157 (10)0.0333 (5)
H140.31080.05470.21920.040*
C150.3916 (2)−0.1093 (2)0.23148 (10)0.0328 (5)
H150.3158−0.15140.21810.039*
U11U22U33U12U13U23
Co10.02150 (17)0.01328 (16)0.01973 (17)0.0000.00619 (13)0.000
O10.0246 (6)0.0345 (8)0.0250 (7)0.0022 (6)0.0052 (5)0.0008 (6)
O20.0252 (7)0.0480 (9)0.0314 (8)0.0040 (7)0.0071 (6)0.0026 (7)
O30.0446 (10)0.1163 (17)0.0354 (10)0.0378 (11)0.0033 (8)0.0035 (10)
O40.0557 (11)0.1214 (18)0.0293 (10)0.0270 (12)0.0052 (8)−0.0022 (10)
O50.0367 (8)0.0734 (12)0.0478 (10)0.0152 (8)0.0210 (7)0.0025 (9)
O60.0376 (9)0.0938 (15)0.0466 (10)0.0261 (9)0.0100 (8)0.0094 (10)
N10.0263 (7)0.0191 (7)0.0246 (7)0.0000.0062 (6)0.000
N20.0268 (12)0.0246 (13)0.0313 (13)0.0000.0072 (10)0.000
C10.0268 (10)0.0300 (10)0.0276 (10)0.0007 (9)0.0057 (8)−0.0005 (9)
C20.0250 (10)0.0327 (11)0.0308 (11)0.0034 (9)0.0030 (9)0.0013 (9)
C30.0254 (10)0.0333 (11)0.0335 (11)0.0015 (9)0.0070 (9)−0.0025 (9)
C40.0294 (10)0.0441 (13)0.0296 (11)0.0011 (10)0.0097 (9)−0.0015 (10)
C50.0289 (11)0.0410 (13)0.0288 (11)0.0011 (9)0.0054 (9)0.0003 (9)
C60.0256 (10)0.0413 (12)0.0320 (12)0.0031 (9)0.0071 (9)−0.0010 (10)
C70.0259 (10)0.0244 (10)0.0291 (10)0.0014 (8)0.0050 (8)0.0002 (9)
C80.0297 (11)0.0435 (13)0.0369 (13)0.0022 (10)0.0100 (10)−0.0008 (10)
C90.0292 (11)0.0614 (15)0.0284 (12)0.0044 (11)0.0092 (9)0.0027 (11)
C100.0317 (11)0.0265 (11)0.0370 (12)0.0027 (9)0.0042 (9)0.0031 (9)
C110.0310 (11)0.0271 (11)0.0391 (12)−0.0005 (9)0.0030 (9)−0.0002 (9)
C120.0267 (14)0.0246 (15)0.0354 (16)0.0000.0096 (12)0.000
C130.0270 (14)0.0238 (15)0.0300 (16)0.0000.0057 (12)0.000
C140.0246 (10)0.0265 (11)0.0464 (13)0.0007 (9)0.0015 (10)0.0022 (10)
C150.0241 (10)0.0276 (11)0.0456 (13)−0.0015 (9)0.0044 (10)0.0006 (10)
Co1—N2i1.982 (2)C1—C71.494 (3)
Co1—N11.992 (2)C2—C31.390 (3)
Co1—O1ii2.0221 (14)C2—H20.9300
Co1—O12.0221 (14)C3—C41.393 (3)
Co1—O2ii2.4354 (13)C3—C81.485 (3)
Co1—O22.4354 (13)C4—C51.391 (3)
O1—C71.273 (2)C4—H40.9300
O2—C71.256 (2)C5—C61.389 (3)
O3—C91.314 (3)C5—C91.485 (3)
O3—H30.8127C6—H60.9300
O4—C91.200 (3)C10—C111.369 (3)
O5—C81.276 (3)C10—H100.9300
O5—H50.7761C11—C121.390 (3)
O6—C81.260 (3)C11—H110.9300
N1—C101.333 (2)C12—C11ii1.390 (3)
N1—C10ii1.333 (2)C12—C131.485 (4)
N2—C15ii1.346 (2)C13—C141.392 (2)
N2—C151.346 (2)C13—C14ii1.392 (2)
N2—Co1iii1.982 (2)C14—C151.371 (3)
C1—C61.388 (3)C14—H140.9300
C1—C21.393 (3)C15—H150.9300
N2i—Co1—N1180.0C1—C6—C5121.1 (2)
N2i—Co1—O1ii90.42 (4)C1—C6—H6119.5
N1—Co1—O1ii89.58 (4)C5—C6—H6119.5
N2i—Co1—O190.42 (4)O2—C7—O1120.87 (19)
N1—Co1—O189.58 (4)O2—C7—C1120.51 (18)
O1ii—Co1—O1179.16 (8)O1—C7—C1118.62 (17)
C7—O1—Co199.65 (12)O6—C8—O5123.7 (2)
C9—O3—H3109.1O6—C8—C3119.2 (2)
C8—O5—H5110.6O5—C8—C3117.11 (19)
C10—N1—C10ii117.5 (2)O4—C9—O3123.8 (2)
C10—N1—Co1121.23 (12)O4—C9—C5124.6 (2)
C10ii—N1—Co1121.23 (12)O3—C9—C5111.60 (19)
C15ii—N2—C15117.4 (2)N1—C10—C11123.1 (2)
C15ii—N2—Co1iii121.30 (12)N1—C10—H10118.5
C15—N2—Co1iii121.30 (12)C11—C10—H10118.5
C6—C1—C2118.9 (2)C10—C11—C12119.7 (2)
C6—C1—C7119.49 (18)C10—C11—H11120.2
C2—C1—C7121.58 (18)C12—C11—H11120.2
C3—C2—C1120.52 (19)C11ii—C12—C11116.9 (3)
C3—C2—H2119.7C11ii—C12—C13121.54 (13)
C1—C2—H2119.7C11—C12—C13121.54 (13)
C2—C3—C4120.00 (19)C14—C13—C14ii116.3 (3)
C2—C3—C8119.79 (18)C14—C13—C12121.83 (13)
C4—C3—C8120.2 (2)C14ii—C13—C12121.83 (13)
C5—C4—C3119.7 (2)C15—C14—C13120.4 (2)
C5—C4—H4120.1C15—C14—H14119.8
C3—C4—H4120.1C13—C14—H14119.8
C6—C5—C4119.72 (19)N2—C15—C14122.7 (2)
C6—C5—C9120.1 (2)N2—C15—H15118.7
C4—C5—C9120.2 (2)C14—C15—H15118.7
N2i—Co1—O1—C7−88.18 (11)C6—C1—C7—O1−163.76 (19)
N1—Co1—O1—C791.82 (11)C2—C1—C7—O117.7 (3)
O1ii—Co1—O1—C791.82 (12)C2—C3—C8—O64.3 (3)
N2i—Co1—N1—C10−141 (22)C4—C3—C8—O6−175.8 (2)
O1ii—Co1—N1—C1083.93 (12)C2—C3—C8—O5−175.6 (2)
O1—Co1—N1—C10−96.07 (12)C4—C3—C8—O54.3 (3)
N2i—Co1—N1—C10ii39 (23)C6—C5—C9—O4−159.5 (3)
O1ii—Co1—N1—C10ii−96.07 (12)C4—C5—C9—O419.2 (4)
O1—Co1—N1—C10ii83.93 (12)C6—C5—C9—O319.8 (3)
C6—C1—C2—C3−1.3 (3)C4—C5—C9—O3−161.5 (2)
C7—C1—C2—C3177.20 (19)C10ii—N1—C10—C110.39 (16)
C1—C2—C3—C4−0.1 (3)Co1—N1—C10—C11−179.61 (16)
C1—C2—C3—C8179.8 (2)N1—C10—C11—C12−0.8 (3)
C2—C3—C4—C51.4 (3)C10—C11—C12—C11ii0.37 (15)
C8—C3—C4—C5−178.4 (2)C10—C11—C12—C13−179.63 (15)
C3—C4—C5—C6−1.3 (3)C11ii—C12—C13—C14161.59 (15)
C3—C4—C5—C9180.0 (2)C11—C12—C13—C14−18.41 (15)
C2—C1—C6—C51.5 (3)C11ii—C12—C13—C14ii−18.41 (15)
C7—C1—C6—C5−177.08 (19)C11—C12—C13—C14ii161.59 (15)
C4—C5—C6—C1−0.2 (3)C14ii—C13—C14—C15−0.70 (16)
C9—C5—C6—C1178.6 (2)C12—C13—C14—C15179.30 (16)
Co1—O1—C7—O21.9 (2)C15ii—N2—C15—C14−0.74 (16)
Co1—O1—C7—C1−177.68 (15)Co1iii—N2—C15—C14179.26 (16)
C6—C1—C7—O216.6 (3)C13—C14—C15—N21.5 (3)
C2—C1—C7—O2−161.9 (2)
D—H···AD—HH···AD···AD—H···A
O3—H3···O2iv0.811.882.648 (2)157
O5—H5···O6v0.781.882.651 (2)170
Table 1

Selected bond lengths (Å)

Co1—N2i1.982 (2)
Co1—N11.992 (2)
Co1—O12.0221 (14)
Co1—O22.4354 (13)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O3—H3⋯O2ii0.811.882.648 (2)157
O5—H5⋯O6iii0.781.882.651 (2)170

Symmetry codes: (ii) ; (iii) .

  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Two coordination polymers created via in situ ligand synthesis involving C-N and C-C bond formation.

Authors:  Russell K Feller; Paul M Forster; Fred Wudl; Anthony K Cheetham
Journal:  Inorg Chem       Date:  2007-09-14       Impact factor: 5.165
  2 in total

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