Literature DB >> 21201013

catena-Poly[[(2,2'-bipyridine-κN,N')nickel(II)]-μ-oxalato-κO,O:O,O].

Sheng Li, Xing-Lian Yan, Shou-Bin Wang, Yuan-Fang Ma.   

Abstract

The title compound, [Ni(C(2)O(4))(C(10)H(8)N(2))](n), is isostructural with its Mn(II), Fe(II), Cu(II) and Zn(II) analogues. Each Ni(II) atom is chelated by two oxalate ligands and one 2,2'-bipyridine, forming a slightly distorted octa-hedral geometry. Oxlate acts as a bridge to link neighbouring pairs of Ni(II) cations, forming a one-dimensional wave-like chain. The crystal showed partial inversion twinning.

Entities:  

Year:  2008        PMID： 21201013      PMCID： PMC2959270          DOI： 10.1107/S1600536808028389

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


Related literature

For related literature, see: Hong & Do (1997 ▶); Eddaoudi et al. (2001 ▶); Liang et al. (2004 ▶); Shi et al. (2005 ▶). For the isostructural MnII, FeII, CuII and ZnII complexes, see: Li et al. (2006 ▶); Deguenon et al. (1990 ▶); Fun et al. (1999 ▶); Luo et al. (2001 ▶); Yu et al. (2006 ▶); Lin et al. (2006 ▶).

Experimental

Crystal data

[Ni(C2O4)(C10H8N2)] M = 302.91 Orthorhombic, a = 9.6486 (14) Å b = 9.2627 (14) Å c = 13.883 (2) Å V = 1240.7 (3) Å3 Z = 4 Mo Kα radiation μ = 1.57 mm−1 T = 296 (2) K 0.12 × 0.10 × 0.06 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.834, T max = 0.912 6146 measured reflections 2114 independent reflections 1810 reflections with I > 2σ(I) R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.047 wR(F 2) = 0.154 S = 1.00 2114 reflections 173 parameters 1 restraint H-atom parameters constrained Δρmax = 0.44 e Å−3 Δρmin = −0.43 e Å−3 Absolute structure: Flack (1983 ▶), 971 Friedel pairs Flack parameter: 0.20 (3) Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; 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 I, global. DOI: 10.1107/S1600536808028389/cf2213sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808028389/cf2213Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ni(C2O4)(C10H8N2)]F(000) = 616
Mr = 302.91Dx = 1.622 Mg m−3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 1779 reflections
a = 9.6486 (14) Åθ = 2.6–21.5°
b = 9.2627 (14) ŵ = 1.57 mm−1
c = 13.883 (2) ÅT = 296 K
V = 1240.7 (3) Å3Block, green
Z = 40.12 × 0.10 × 0.06 mm
Bruker APEXII CCD area-detector diffractometer2114 independent reflections
Radiation source: fine-focus sealed tube1810 reflections with I > 2σ(I)
graphiteRint = 0.030
φ and ω scansθmax = 25.1°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −11→5
Tmin = 0.834, Tmax = 0.912k = −11→11
6146 measured reflectionsl = −16→16
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.154w = 1/[σ2(Fo2) + (0.118P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
2114 reflectionsΔρmax = 0.44 e Å−3
173 parametersΔρmin = −0.44 e Å−3
1 restraintAbsolute structure: Flack (1983), 971 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.20 (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
Ni10.88396 (7)1.09402 (7)0.25107 (8)0.04352 (14)
O11.0093 (4)1.2363 (5)0.1613 (3)0.0503 (11)
O21.0673 (4)1.1297 (4)0.3368 (3)0.0415 (9)
O30.7686 (4)1.2511 (5)0.3347 (3)0.0452 (10)
O40.7033 (4)1.1389 (4)0.1640 (3)0.0416 (9)
N10.8006 (5)0.9059 (5)0.3352 (4)0.0401 (11)
N20.9510 (5)0.8925 (5)0.1747 (4)0.0395 (11)
C11.1555 (6)1.2124 (6)0.3004 (4)0.0380 (12)
C21.1199 (4)1.2745 (6)0.1993 (4)0.0305 (12)
C30.7196 (8)0.9174 (8)0.4115 (5)0.0535 (17)
H30.69641.00990.43200.064*
C40.6668 (8)0.8030 (10)0.4630 (5)0.070 (2)
H40.61060.81630.51680.084*
C50.7033 (9)0.6629 (9)0.4291 (6)0.073 (2)
H50.67280.58090.46130.087*
C60.7820 (8)0.6507 (7)0.3504 (6)0.0633 (19)
H60.80540.55980.32690.076*
C70.8286 (6)0.7736 (6)0.3038 (4)0.0405 (13)
C80.9159 (6)0.7661 (7)0.2154 (4)0.0408 (13)
C90.9646 (9)0.6356 (7)0.1766 (6)0.0627 (19)
H90.94470.54840.20670.075*
C101.0418 (10)0.6383 (10)0.0936 (7)0.081 (3)
H101.07130.55190.06630.097*
C111.0758 (8)0.7647 (9)0.0510 (5)0.066 (2)
H111.12920.7669−0.00480.080*
C121.0277 (8)0.8924 (8)0.0937 (5)0.0601 (19)
H121.04950.98020.06510.072*
U11U22U33U12U13U23
Ni10.0387 (2)0.0456 (2)0.0463 (2)0.0000 (2)−0.0004 (3)0.0045 (3)
O10.042 (2)0.065 (3)0.044 (3)−0.012 (2)−0.0101 (19)0.022 (2)
O20.0384 (19)0.052 (2)0.034 (2)−0.0078 (19)−0.0056 (16)0.0150 (18)
O30.039 (2)0.061 (2)0.036 (2)0.0098 (19)−0.0144 (18)−0.0128 (19)
O40.042 (2)0.048 (2)0.035 (2)−0.0017 (18)−0.0036 (17)−0.0095 (18)
N10.043 (3)0.045 (3)0.032 (2)−0.0063 (18)0.006 (2)−0.0005 (19)
N20.045 (3)0.038 (2)0.036 (3)0.0049 (19)0.008 (2)0.002 (2)
C10.038 (3)0.036 (3)0.040 (3)0.007 (3)−0.004 (3)0.004 (3)
C20.028 (3)0.034 (3)0.029 (3)−0.002 (2)−0.0031 (19)0.005 (2)
C30.062 (4)0.058 (4)0.041 (4)−0.005 (3)0.016 (3)0.005 (3)
C40.068 (4)0.098 (6)0.043 (4)−0.024 (5)0.015 (4)0.011 (4)
C50.087 (5)0.071 (5)0.060 (4)−0.034 (4)0.011 (4)0.021 (4)
C60.088 (5)0.039 (3)0.063 (4)−0.022 (3)0.004 (4)−0.002 (3)
C70.040 (3)0.045 (3)0.037 (3)−0.008 (3)0.000 (3)0.005 (2)
C80.045 (3)0.046 (3)0.031 (3)0.008 (3)0.000 (3)−0.005 (2)
C90.089 (5)0.041 (3)0.058 (4)0.012 (3)−0.002 (4)0.005 (3)
C100.096 (7)0.073 (5)0.073 (5)0.040 (5)0.009 (5)−0.017 (5)
C110.091 (5)0.070 (5)0.037 (4)0.028 (4)0.012 (4)0.003 (3)
C120.069 (5)0.064 (4)0.047 (4)0.023 (3)0.014 (3)0.012 (3)
Ni1—O42.162 (4)C3—C41.376 (10)
Ni1—O22.157 (4)C3—H30.930
Ni1—O12.180 (4)C4—C51.425 (13)
Ni1—O32.169 (4)C4—H40.930
Ni1—N22.242 (5)C5—C61.335 (12)
Ni1—N12.246 (5)C5—H50.930
O1—C21.242 (6)C6—C71.385 (9)
O2—C11.251 (7)C6—H60.930
O3—C1i1.238 (6)C7—C81.491 (8)
O4—C2i1.237 (6)C8—C91.404 (9)
N1—C31.322 (8)C9—C101.372 (12)
N1—C71.328 (7)C9—H90.930
N2—C81.343 (8)C10—C111.353 (13)
N2—C121.346 (9)C10—H100.930
C1—O3ii1.238 (6)C11—C121.402 (10)
C1—C21.554 (6)C11—H110.930
C2—O4ii1.237 (6)C12—H120.930
O4—Ni1—O2160.07 (14)N1—C3—C4125.0 (7)
O4—Ni1—O190.65 (14)N1—C3—H3117.5
O2—Ni1—O176.55 (13)C4—C3—H3117.5
O4—Ni1—O375.90 (14)C3—C4—C5115.9 (7)
O2—Ni1—O391.31 (15)C3—C4—H4122.0
O1—Ni1—O3100.66 (17)C5—C4—H4122.0
O4—Ni1—N297.39 (17)C6—C5—C4119.3 (7)
O2—Ni1—N298.72 (18)C6—C5—H5120.4
O1—Ni1—N294.20 (18)C4—C5—H5120.4
O3—Ni1—N2163.69 (17)C5—C6—C7119.8 (7)
O4—Ni1—N198.71 (17)C5—C6—H6120.1
O2—Ni1—N197.23 (17)C7—C6—H6120.1
O1—Ni1—N1164.72 (18)N1—C7—C6122.7 (6)
O3—Ni1—N193.35 (18)N1—C7—C8115.3 (5)
N2—Ni1—N172.74 (17)C6—C7—C8122.0 (6)
C2—O1—Ni1114.0 (3)N2—C8—C9120.3 (6)
C1—O2—Ni1115.4 (4)N2—C8—C7116.6 (5)
C1i—O3—Ni1115.4 (3)C9—C8—C7123.0 (6)
C2i—O4—Ni1115.3 (3)C8—C9—C10119.2 (7)
C3—N1—C7117.2 (5)C8—C9—H9120.4
C3—N1—Ni1124.5 (4)C10—C9—H9120.4
C7—N1—Ni1118.2 (4)C11—C10—C9121.0 (7)
C8—N2—C12119.3 (5)C11—C10—H10119.5
C8—N2—Ni1117.0 (4)C9—C10—H10119.5
C12—N2—Ni1123.7 (4)C10—C11—C12117.7 (7)
O2—C1—O3ii127.7 (5)C10—C11—H11121.2
O2—C1—C2116.2 (5)C12—C11—H11121.2
O3ii—C1—C2116.2 (5)N2—C12—C11122.4 (7)
O4ii—C2—O1125.1 (5)N2—C12—H12118.8
O4ii—C2—C1117.0 (4)C11—C12—H12118.8
O1—C2—C1117.8 (4)
O4—Ni1—O1—C2162.4 (4)O1—Ni1—N2—C12−7.8 (6)
O2—Ni1—O1—C2−2.1 (4)O3—Ni1—N2—C12147.8 (6)
O3—Ni1—O1—C286.7 (4)N1—Ni1—N2—C12−179.8 (6)
N2—Ni1—O1—C2−100.1 (4)Ni1—O2—C1—O3ii−179.5 (5)
N1—Ni1—O1—C2−69.5 (8)Ni1—O2—C1—C2−0.7 (6)
O4—Ni1—O2—C1−49.9 (7)Ni1—O1—C2—O4ii−175.8 (5)
O1—Ni1—O2—C11.4 (4)Ni1—O1—C2—C12.5 (6)
O3—Ni1—O2—C1−99.2 (4)O2—C1—C2—O4ii177.1 (6)
N2—Ni1—O2—C193.7 (4)O3ii—C1—C2—O4ii−3.9 (7)
N1—Ni1—O2—C1167.2 (4)O2—C1—C2—O1−1.3 (7)
O4—Ni1—O3—C1i3.6 (4)O3ii—C1—C2—O1177.7 (6)
O2—Ni1—O3—C1i168.2 (4)C7—N1—C3—C42.7 (11)
O1—Ni1—O3—C1i91.6 (4)Ni1—N1—C3—C4179.3 (6)
N2—Ni1—O3—C1i−63.7 (8)N1—C3—C4—C5−0.5 (11)
N1—Ni1—O3—C1i−94.5 (4)C3—C4—C5—C6−1.4 (12)
O2—Ni1—O4—C2i−52.8 (7)C4—C5—C6—C71.0 (12)
O1—Ni1—O4—C2i−102.2 (4)C3—N1—C7—C6−3.1 (9)
O3—Ni1—O4—C2i−1.3 (4)Ni1—N1—C7—C6−179.9 (5)
N2—Ni1—O4—C2i163.5 (4)C3—N1—C7—C8177.8 (6)
N1—Ni1—O4—C2i89.9 (4)Ni1—N1—C7—C80.9 (6)
O4—Ni1—N1—C3−80.8 (6)C5—C6—C7—N11.3 (11)
O2—Ni1—N1—C387.1 (6)C5—C6—C7—C8−179.6 (7)
O1—Ni1—N1—C3152.0 (6)C12—N2—C8—C93.2 (9)
O3—Ni1—N1—C3−4.6 (6)Ni1—N2—C8—C9−174.3 (5)
N2—Ni1—N1—C3−175.9 (6)C12—N2—C8—C7−178.8 (6)
O4—Ni1—N1—C795.7 (4)Ni1—N2—C8—C73.6 (7)
O2—Ni1—N1—C7−96.3 (4)N1—C7—C8—N2−3.0 (7)
O1—Ni1—N1—C7−31.5 (9)C6—C7—C8—N2177.8 (6)
O3—Ni1—N1—C7171.9 (4)N1—C7—C8—C9174.9 (6)
N2—Ni1—N1—C70.6 (4)C6—C7—C8—C9−4.3 (9)
O4—Ni1—N2—C8−99.2 (5)N2—C8—C9—C10−3.7 (11)
O2—Ni1—N2—C892.6 (4)C7—C8—C9—C10178.5 (7)
O1—Ni1—N2—C8169.6 (4)C8—C9—C10—C112.4 (13)
O3—Ni1—N2—C8−34.7 (9)C9—C10—C11—C12−0.9 (13)
N1—Ni1—N2—C8−2.3 (4)C8—N2—C12—C11−1.7 (11)
O4—Ni1—N2—C1283.4 (6)Ni1—N2—C12—C11175.7 (6)
O2—Ni1—N2—C12−84.9 (6)C10—C11—C12—N20.4 (12)
  4 in total

1.  A Magnetically Coupled Three-Dimensional (Terephthalato)manganese(II) Network.

Authors:  Chang Seop Hong; Youngkyu Do
Journal:  Inorg Chem       Date:  1997-12-03       Impact factor: 5.165

2.  Porous metal-organic polyhedra: 25 A cuboctahedron constructed from 12 Cu2(CO2)4 paddle-wheel building blocks.

Authors:  M Eddaoudi; J Kim; J B Wachter; H K Chae; M O'Keeffe; O M Yaghi
Journal:  J Am Chem Soc       Date:  2001-05-09       Impact factor: 15.419

3.  A coordination pi-pi framework exhibits spontaneous magnetization.

Authors:  Lu-Lin Li; Kuan-Jiuh Lin; Chin-Jun Ho; Chia-Pin Sun; Hung-Duen Yang
Journal:  Chem Commun (Camb)       Date:  2006-02-10       Impact factor: 6.222

4.  A short history of SHELX.

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

1.  Retraction of articles.

Authors: 
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-06-13
  1 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.