Literature DB >> 21201648

catena-Poly[[aqua-(pyrazino[2,3-f][1,10]phenanthroline-κN,N)cobalt(II)]-μ-pyrazine-2,3-dicarboxyl-ato-κNO:O].

Zhan-Lin Xu1, Xiu-Ying Li, Guang-Bo Che, Lu Lu, Chun-Hui Xu.   

Abstract

In the title compound, [Co(C(6)H(2)N(2)O(4))(C(14)H(8)N(4))(H(2)O)](n), the Co atom is bonded to one N,N'-bidentate pyrazino[2,3-f][1,10]phenanthroline (Pyphen) ligand, one N,O-bidentate pyrazine-2,3-dicarboxyl-ate (PZDC) dianion and one water mol-ecule in a distorted octa-hedral mer-CoN(3)O(3) geometry. The Co(II) atoms are bridged by the PZDC dianions, forming an infinite one-dimensional chain running along the b axis. Adjacent chains pack together through π-π stacking inter-actions [centroid-centroid separations = 3.498 (4) and 3.528 (4) Å], and O-H⋯O and O-H⋯N hydrogen bonds involving the water mol-ecule complete the structure.

Entities:  

Year:  2008        PMID： 21201648      PMCID： PMC2960716          DOI： 10.1107/S1600536808027177

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


Related literature

For related structures, see: Che et al. (2008 ▶); Liu et al. (2008 ▶). For the synthesis of the ligand, see: Che et al. (2006 ▶).

Experimental

Crystal data

[Co(C6H2N2O4)(C14H8N4)(H2O)] M = 475.29 Triclinic, a = 6.8430 (14) Å b = 7.4455 (15) Å c = 17.454 (4) Å α = 93.64 (3)° β = 95.99 (3)° γ = 97.61 (3)° V = 873.9 (3) Å3 Z = 2 Mo Kα radiation μ = 1.04 mm−1 T = 292 (2) K 0.41 × 0.33 × 0.19 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T min = 0.672, T max = 0.823 7576 measured reflections 3434 independent reflections 1541 reflections with I > 2σ(I) R int = 0.114

Refinement

R[F 2 > 2σ(F 2)] = 0.070 wR(F 2) = 0.161 S = 0.92 3434 reflections 297 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.45 e Å−3 Δρmin = −0.65 e Å−3 Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); 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: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808027177/hb2775sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808027177/hb2775Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C6H2N2O4)(C14H8N4)(H2O)]Z = 2
Mr = 475.29F000 = 482
Triclinic, P1Dx = 1.806 Mg m−3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 6.8430 (14) ÅCell parameters from 2411 reflections
b = 7.4455 (15) Åθ = 2.4–26.0º
c = 17.454 (4) ŵ = 1.04 mm−1
α = 93.64 (3)ºT = 292 (2) K
β = 95.99 (3)ºBlock, yellow
γ = 97.61 (3)º0.41 × 0.33 × 0.19 mm
V = 873.9 (3) Å3
Bruker SMART CCD diffractometer3434 independent reflections
Radiation source: fine-focus sealed tube1541 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.114
T = 292(2) Kθmax = 26.1º
ω scansθmin = 2.4º
Absorption correction: multi-scan(SADABS; Bruker, 2002)h = −8→8
Tmin = 0.672, Tmax = 0.823k = −9→9
7576 measured reflectionsl = −20→21
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap and geom
R[F2 > 2σ(F2)] = 0.070H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.161  w = 1/[σ2(Fo2) + (0.0488P)2] where P = (Fo2 + 2Fc2)/3
S = 0.92(Δ/σ)max < 0.001
3434 reflectionsΔρmax = 0.45 e Å−3
297 parametersΔρmin = −0.65 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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
C10.1297 (9)−0.2248 (9)0.7468 (4)0.0382 (19)
H10.0668−0.21190.79120.046*
C20.0341 (10)−0.3449 (9)0.6867 (4)0.042 (2)
H2−0.0854−0.41600.69180.050*
C30.1202 (10)−0.3567 (9)0.6187 (4)0.0378 (18)
H30.0554−0.43050.57610.045*
C40.3067 (10)−0.2560 (9)0.6148 (4)0.0334 (17)
C50.4113 (10)−0.2614 (9)0.5466 (4)0.0309 (17)
C60.4200 (11)−0.3667 (10)0.4217 (4)0.047 (2)
H60.3620−0.43520.37670.057*
C70.6080 (12)−0.2729 (10)0.4227 (4)0.046 (2)
H70.6723−0.28170.37850.056*
C80.6015 (10)−0.1635 (9)0.5474 (4)0.0377 (19)
C90.6942 (9)−0.0530 (9)0.6161 (4)0.0307 (17)
C100.8851 (10)0.0455 (9)0.6205 (4)0.0368 (18)
H100.95840.04320.57850.044*
C110.9615 (10)0.1464 (9)0.6892 (4)0.0383 (19)
H111.08590.21620.69390.046*
C120.8503 (10)0.1414 (9)0.7502 (4)0.0390 (19)
H120.90550.20660.79630.047*
C130.5930 (9)−0.0467 (8)0.6809 (4)0.0306 (17)
C140.3934 (9)−0.1466 (8)0.6793 (4)0.0283 (16)
C150.6273 (9)0.4436 (8)0.8808 (3)0.0243 (15)
C160.7009 (9)0.6013 (9)0.9285 (4)0.0287 (16)
C170.7670 (9)0.4280 (10)1.0288 (4)0.0352 (18)
H170.81130.41791.08040.042*
C180.7034 (9)0.2695 (9)0.9810 (4)0.0314 (17)
H180.71190.15681.00020.038*
C190.5404 (10)0.4446 (10)0.7980 (4)0.0346 (18)
C200.7100 (11)0.7927 (9)0.9014 (4)0.0329 (17)
N10.3064 (8)−0.1266 (7)0.7451 (3)0.0311 (14)
N20.6678 (8)0.0493 (7)0.7479 (3)0.0328 (14)
N30.3191 (8)−0.3632 (7)0.4820 (3)0.0376 (15)
N40.7025 (8)−0.1691 (8)0.4849 (3)0.0386 (15)
N50.6314 (7)0.2789 (7)0.9087 (3)0.0292 (14)
N60.7668 (7)0.5927 (7)1.0039 (3)0.0321 (14)
O10.4150 (7)0.3020 (6)0.7750 (2)0.0389 (12)
O20.5959 (7)0.5679 (7)0.7600 (3)0.0494 (14)
O1W0.2264 (8)0.0860 (8)0.8973 (3)0.0411 (14)
O30.5474 (7)0.8538 (6)0.8915 (3)0.0368 (12)
O40.8788 (7)0.8715 (7)0.8956 (3)0.0536 (15)
Co0.46559 (14)0.06529 (13)0.83165 (5)0.0332 (3)
HW1A0.113 (11)0.005 (10)0.905 (4)0.06 (3)*
HW1B0.200 (10)0.182 (10)0.910 (4)0.05 (3)*
U11U22U33U12U13U23
C10.029 (4)0.047 (5)0.037 (5)−0.004 (4)0.011 (3)0.000 (4)
C20.040 (4)0.046 (5)0.034 (5)−0.016 (4)0.010 (4)−0.001 (4)
C30.038 (4)0.037 (5)0.034 (5)−0.001 (4)−0.004 (4)−0.006 (4)
C40.034 (4)0.027 (4)0.038 (4)−0.001 (3)0.004 (3)−0.002 (3)
C50.040 (4)0.032 (4)0.021 (4)0.008 (3)0.001 (3)0.004 (3)
C60.051 (5)0.064 (6)0.025 (4)0.002 (4)0.009 (4)−0.008 (4)
C70.059 (6)0.051 (6)0.032 (5)0.014 (4)0.012 (4)0.001 (4)
C80.036 (4)0.030 (4)0.053 (5)0.008 (4)0.024 (4)0.011 (4)
C90.031 (4)0.036 (5)0.024 (4)0.003 (3)0.004 (3)−0.001 (3)
C100.032 (4)0.034 (5)0.046 (5)0.006 (3)0.009 (4)0.005 (4)
C110.032 (4)0.039 (5)0.044 (5)−0.003 (3)0.016 (4)0.008 (4)
C120.039 (5)0.038 (5)0.040 (5)0.003 (4)0.002 (4)0.011 (4)
C130.038 (4)0.022 (4)0.030 (4)0.001 (3)−0.003 (3)0.000 (3)
C140.034 (4)0.015 (4)0.034 (4)−0.001 (3)0.000 (3)0.002 (3)
C150.030 (4)0.020 (4)0.025 (4)0.007 (3)0.004 (3)0.005 (3)
C160.025 (4)0.030 (4)0.031 (4)0.001 (3)0.008 (3)0.003 (3)
C170.039 (4)0.039 (5)0.027 (4)0.004 (4)0.001 (3)0.005 (4)
C180.033 (4)0.026 (4)0.038 (5)0.004 (3)0.012 (3)0.012 (3)
C190.039 (4)0.032 (5)0.035 (5)0.006 (4)0.013 (4)−0.001 (4)
C200.036 (4)0.030 (5)0.031 (4)−0.005 (4)0.010 (4)−0.001 (3)
N10.030 (3)0.026 (3)0.037 (4)0.002 (3)0.006 (3)0.000 (3)
N20.035 (3)0.030 (3)0.032 (4)−0.006 (3)0.009 (3)0.000 (3)
N30.044 (4)0.038 (4)0.029 (4)0.004 (3)0.003 (3)0.001 (3)
N40.041 (4)0.045 (4)0.032 (4)0.006 (3)0.013 (3)0.004 (3)
N50.026 (3)0.035 (4)0.030 (4)0.007 (3)0.009 (3)0.011 (3)
N60.028 (3)0.029 (4)0.038 (4)−0.003 (3)0.011 (3)0.002 (3)
O10.050 (3)0.032 (3)0.030 (3)−0.003 (2)−0.003 (2)0.001 (2)
O20.063 (4)0.041 (4)0.043 (3)−0.002 (3)0.008 (3)0.007 (3)
O1W0.035 (3)0.030 (4)0.055 (4)−0.009 (3)0.015 (3)−0.009 (3)
O30.036 (3)0.033 (3)0.045 (3)0.006 (2)0.014 (2)0.009 (2)
O40.042 (3)0.050 (4)0.064 (4)−0.017 (3)0.009 (3)0.009 (3)
Co0.0347 (6)0.0307 (6)0.0323 (6)−0.0037 (4)0.0069 (4)0.0004 (4)
C1—N11.332 (7)C13—N21.345 (8)
C1—C21.383 (9)C13—C141.463 (9)
C1—H10.9300C14—N11.357 (7)
C2—C31.381 (8)C15—N51.351 (7)
C2—H20.9300C15—C161.399 (8)
C3—C41.403 (9)C15—C191.504 (9)
C3—H30.9300C16—N61.353 (8)
C4—C141.378 (8)C16—C201.525 (9)
C4—C51.453 (9)C17—N61.328 (8)
C5—N31.364 (8)C17—C181.393 (8)
C5—C81.403 (9)C17—H170.9300
C6—N31.318 (8)C18—N51.315 (8)
C6—C71.378 (9)C18—H180.9300
C6—H60.9300C19—O21.211 (7)
C7—N41.345 (8)C19—O11.288 (7)
C7—H70.9300C20—O41.242 (7)
C8—N41.353 (8)C20—O31.257 (8)
C8—C91.446 (9)Co—N12.116 (5)
C9—C131.389 (8)Co—N22.124 (5)
C9—C101.403 (9)Co—N52.135 (5)
C10—C111.389 (9)Co—O3i2.050 (5)
C10—H100.9300Co—O1W2.110 (5)
C11—C121.370 (8)Co—O12.125 (5)
C11—H110.9300O1W—HW1A0.95 (7)
C12—N21.338 (8)O1W—HW1B0.78 (7)
C12—H120.9300O3—Coii2.050 (5)
N1—C1—C2124.0 (7)N6—C16—C20115.1 (6)
N1—C1—H1118.0C15—C16—C20123.7 (6)
C2—C1—H1118.0N6—C17—C18122.7 (6)
C3—C2—C1118.5 (6)N6—C17—H17118.6
C3—C2—H2120.7C18—C17—H17118.6
C1—C2—H2120.7N5—C18—C17120.2 (6)
C2—C3—C4119.1 (6)N5—C18—H18119.9
C2—C3—H3120.5C17—C18—H18119.9
C4—C3—H3120.5O2—C19—O1127.2 (7)
C14—C4—C3117.7 (6)O2—C19—C15120.0 (7)
C14—C4—C5119.0 (6)O1—C19—C15112.7 (6)
C3—C4—C5123.4 (6)O4—C20—O3128.2 (7)
N3—C5—C8121.2 (6)O4—C20—C16115.6 (7)
N3—C5—C4118.2 (6)O3—C20—C16116.1 (6)
C8—C5—C4120.6 (6)C1—N1—C14116.6 (6)
N3—C6—C7122.6 (7)C1—N1—Co127.8 (5)
N3—C6—H6118.7C14—N1—Co115.5 (4)
C7—C6—H6118.7C12—N2—C13116.6 (6)
N4—C7—C6122.8 (7)C12—N2—Co127.5 (5)
N4—C7—H7118.6C13—N2—Co115.3 (4)
C6—C7—H7118.6C6—N3—C5116.3 (6)
N4—C8—C5121.5 (7)C7—N4—C8115.6 (6)
N4—C8—C9118.3 (6)C18—N5—C15119.2 (6)
C5—C8—C9120.2 (6)C18—N5—Co127.6 (5)
C13—C9—C10118.4 (6)C15—N5—Co112.2 (4)
C13—C9—C8119.1 (6)C17—N6—C16116.7 (6)
C10—C9—C8122.6 (6)C19—O1—Co114.9 (4)
C11—C10—C9118.1 (6)Co—O1W—HW1A134 (4)
C11—C10—H10121.0Co—O1W—HW1B120 (6)
C9—C10—H10121.0HW1A—O1W—HW1B104 (7)
C12—C11—C10118.9 (7)C20—O3—Coii131.4 (4)
C12—C11—H11120.6O3i—Co—O1W91.3 (2)
C10—C11—H11120.6O3i—Co—N188.77 (19)
N2—C12—C11124.5 (7)O1W—Co—N196.0 (2)
N2—C12—H12117.7O3i—Co—N296.21 (19)
C11—C12—H12117.7O1W—Co—N2169.4 (2)
N2—C13—C9123.6 (6)N1—Co—N276.8 (2)
N2—C13—C14115.9 (6)O3i—Co—O1173.06 (19)
C9—C13—C14120.5 (6)O1W—Co—O191.9 (2)
N1—C14—C4123.9 (6)N1—Co—O196.98 (19)
N1—C14—C13115.5 (6)N2—Co—O181.41 (19)
C4—C14—C13120.6 (6)O3i—Co—N596.8 (2)
N5—C15—C16119.9 (6)O1W—Co—N587.2 (2)
N5—C15—C19116.4 (6)N1—Co—N5173.5 (2)
C16—C15—C19123.7 (6)N2—Co—N599.2 (2)
N6—C16—C15121.2 (6)O1—Co—N577.22 (19)
D—H···AD—HH···AD···AD—H···A
O1W—HW1A···O4iii0.95 (7)1.76 (7)2.680 (7)164 (6)
O1W—HW1B···N6iv0.78 (7)2.15 (7)2.851 (8)149 (7)
Table 1

Selected bond lengths (Å)

Co—N12.116 (5)
Co—N22.124 (5)
Co—N52.135 (5)
Co—O3i2.050 (5)
Co—O1W2.110 (5)
Co—O12.125 (5)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—HW1A⋯O4ii0.95 (7)1.76 (7)2.680 (7)164 (6)
O1W—HW1B⋯N6iii0.78 (7)2.15 (7)2.851 (8)149 (7)

Symmetry codes: (ii) ; (iii) .

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1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
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1.  Poly[[(N,N-dimethyl-formamide-κO)(μ(3)-pyrazine-2,3-dicarboxyl-ato-κN,O:O:O)copper(II)] monohydrate].

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