Literature DB >> 21201321

Bis{μ-2-[(2-oxidobenzyl-idene)amino-meth-yl]phenolato-κO,N,O'}bis-[(pyridine-κN)zinc(II)].

Chun Yang1, Ou-Yang Yan, Qing-Lun Wang, Dai-Zheng Liao.   

Abstract

In the title centrosymmetric zinc(II) complex, [Zn(2)(C(4)H(13)NO(2))(2)(C(6)H(5)N)(2)], each Zn(II) atom is coordinated by two 2-[(2-oxidobenzyl-idene)amino-meth-yl]phenolate (L) ligands and one pyridine (py) mol-ecule in a distorted trigonal-bipyramidal geometry. Each L ligand behaves as a tridentate ligand and provides a phenolate oxygen bridge which links the two Zn(II) atoms. The ZnL(py) units are linked by π-π inter-actions between adjacent pyridine mol-ecules, with a centroid-centroid distance of 3.724 Å, resulting in a two-dimensional structure.

Entities:  

Year:  2008        PMID： 21201321      PMCID： PMC2960381          DOI： 10.1107/S1600536808000962

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


Related literature

For the biochemical and catalytic activity of zinc(II) complexes, see: Marco et al. (2004 ▶); Kim et al. (2000 ▶). ZnII ions in phenoxide-bridged dinuclear complexes provide flexible coordination numbers, see: Atakol et al. (1999 ▶); Huang et al. (2006 ▶). For the preparation of H2 L, see: Moustafa (2003 ▶).

Experimental

Crystal data

[Zn2(C14H13NO2)2(C5H5N)2] M = 739.42 Monoclinic, a = 10.145 (6) Å b = 13.806 (8) Å c = 12.671 (8) Å β = 102.063 (10)° V = 1735.5 (18) Å3 Z = 2 Mo Kα radiation μ = 1.43 mm−1 T = 294 (2) K 0.20 × 0.18 × 0.12 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.693, T max = 1.000 (expected range = 0.584–0.843) 9656 measured reflections 3561 independent reflections 2440 reflections with I > 2σ(I) R int = 0.056

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.084 S = 1.00 3561 reflections 217 parameters H-atom parameters constrained Δρmax = 0.40 e Å−3 Δρmin = −0.32 e Å−3 Data collection: SMART-NT (Bruker, 1998 ▶); cell refinement: SAINT-NT (Bruker, 1998 ▶); data reduction: SAINT-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL-NT (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL-NT. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000962/at2532sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000962/at2532Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn2(C14H13NO2)2(C5H5N)2]F000 = 760
Mr = 739.42Dx = 1.415 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2807 reflections
a = 10.145 (6) Åθ = 2.5–24.3º
b = 13.806 (8) ŵ = 1.43 mm−1
c = 12.671 (8) ÅT = 294 (2) K
β = 102.063 (10)ºBlock, yellow
V = 1735.5 (18) Å30.20 × 0.18 × 0.12 mm
Z = 2
Bruker SMART APEX CCD area-detector diffractometer3561 independent reflections
Radiation source: fine-focus sealed tube2440 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.056
T = 294(2) Kθmax = 26.5º
φ and ω scansθmin = 2.1º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.693, Tmax = 1.000k = −17→14
9656 measured reflectionsl = −15→14
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.084  w = 1/[σ2(Fo2) + (0.0341P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
3561 reflectionsΔρmax = 0.40 e Å−3
217 parametersΔρmin = −0.32 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
Zn10.60866 (3)1.08479 (2)0.49115 (2)0.03166 (11)
O10.46079 (18)1.05680 (13)0.56701 (14)0.0360 (5)
O20.3413 (2)0.78111 (13)0.45886 (14)0.0444 (5)
N10.4099 (2)0.87742 (16)0.66733 (16)0.0326 (5)
N20.7965 (2)1.02458 (17)0.57069 (17)0.0356 (6)
C10.4150 (3)1.09767 (19)0.6492 (2)0.0330 (6)
C20.3621 (3)1.1911 (2)0.6419 (2)0.0422 (7)
H20.36111.22780.58020.051*
C30.3106 (3)1.2300 (2)0.7263 (3)0.0531 (9)
H30.27401.29200.72010.064*
C40.3136 (3)1.1771 (2)0.8189 (3)0.0550 (9)
H40.27991.20350.87540.066*
C50.3670 (3)1.0849 (2)0.8273 (2)0.0492 (8)
H50.36951.04970.89030.059*
C60.4171 (3)1.0433 (2)0.7438 (2)0.0351 (7)
C70.4791 (3)0.9441 (2)0.7531 (2)0.0429 (7)
H7A0.57320.94940.74890.051*
H7B0.47530.91700.82300.051*
C80.3665 (3)0.7963 (2)0.6971 (2)0.0351 (7)
H80.37920.78590.77100.042*
C90.3000 (3)0.7197 (2)0.6279 (2)0.0340 (6)
C100.2446 (3)0.6435 (2)0.6794 (2)0.0503 (8)
H100.25110.64650.75360.060*
C110.1821 (4)0.5660 (2)0.6240 (3)0.0643 (10)
H110.14600.51700.65970.077*
C120.1733 (4)0.5613 (2)0.5133 (3)0.0640 (10)
H120.13080.50870.47450.077*
C130.2264 (3)0.6333 (2)0.4608 (2)0.0552 (9)
H130.21910.62810.38660.066*
C140.2920 (3)0.7152 (2)0.5145 (2)0.0365 (7)
C150.9071 (3)1.0806 (2)0.5933 (2)0.0446 (7)
H150.89911.14620.57620.054*
C161.0325 (3)1.0443 (3)0.6410 (2)0.0561 (9)
H161.10731.08490.65580.067*
C171.0448 (3)0.9487 (3)0.6659 (3)0.0607 (10)
H171.12870.92290.69700.073*
C180.9335 (3)0.8906 (3)0.6452 (3)0.0603 (9)
H180.94010.82510.66300.072*
C190.8101 (3)0.9309 (2)0.5970 (2)0.0461 (8)
H190.73430.89130.58260.055*
U11U22U33U12U13U23
Zn10.02991 (19)0.03587 (19)0.03086 (18)−0.00479 (15)0.01014 (13)−0.00201 (15)
O10.0333 (11)0.0390 (11)0.0407 (11)−0.0073 (8)0.0192 (9)−0.0102 (9)
O20.0649 (14)0.0390 (12)0.0338 (10)−0.0139 (10)0.0206 (10)−0.0039 (9)
N10.0330 (13)0.0348 (13)0.0293 (12)0.0030 (10)0.0044 (10)−0.0020 (10)
N20.0286 (13)0.0446 (15)0.0342 (13)−0.0056 (11)0.0076 (10)−0.0026 (11)
C10.0239 (14)0.0372 (16)0.0392 (16)−0.0080 (12)0.0096 (12)−0.0133 (13)
C20.0455 (19)0.0363 (17)0.0480 (18)−0.0079 (14)0.0171 (14)−0.0074 (14)
C30.051 (2)0.0375 (18)0.073 (2)0.0010 (15)0.0197 (18)−0.0152 (17)
C40.060 (2)0.055 (2)0.059 (2)−0.0088 (17)0.0321 (18)−0.0267 (18)
C50.056 (2)0.056 (2)0.0395 (17)−0.0135 (17)0.0188 (15)−0.0146 (16)
C60.0332 (16)0.0377 (16)0.0336 (15)−0.0057 (13)0.0050 (12)−0.0114 (13)
C70.0418 (18)0.0504 (18)0.0330 (15)0.0001 (14)0.0000 (13)−0.0070 (14)
C80.0325 (16)0.0437 (18)0.0291 (14)0.0082 (13)0.0064 (12)0.0048 (13)
C90.0332 (16)0.0392 (16)0.0306 (14)0.0015 (13)0.0086 (12)0.0030 (13)
C100.057 (2)0.056 (2)0.0392 (17)−0.0067 (17)0.0138 (15)0.0105 (16)
C110.073 (3)0.060 (2)0.064 (2)−0.0266 (19)0.026 (2)0.0044 (19)
C120.079 (3)0.054 (2)0.064 (2)−0.0310 (19)0.025 (2)−0.0107 (18)
C130.075 (2)0.053 (2)0.0420 (18)−0.0196 (18)0.0224 (17)−0.0087 (16)
C140.0387 (17)0.0359 (16)0.0376 (16)−0.0031 (13)0.0142 (13)−0.0022 (13)
C150.0351 (17)0.054 (2)0.0463 (17)−0.0098 (15)0.0123 (14)−0.0063 (15)
C160.0306 (18)0.086 (3)0.050 (2)−0.0117 (17)0.0054 (15)−0.008 (2)
C170.0317 (19)0.098 (3)0.051 (2)0.0096 (19)0.0062 (15)0.012 (2)
C180.052 (2)0.067 (2)0.062 (2)0.0123 (18)0.0121 (17)0.0219 (18)
C190.0376 (18)0.053 (2)0.0483 (18)−0.0027 (15)0.0095 (14)0.0083 (15)
Zn1—O11.9814 (19)C6—C71.501 (4)
Zn1—O2i1.988 (2)C7—H7A0.9700
Zn1—N1i2.045 (2)C7—H7B0.9700
Zn1—N22.129 (2)C8—C91.448 (4)
Zn1—O1i2.155 (2)C8—H80.9300
O1—C11.349 (3)C9—C101.415 (4)
O1—Zn1i2.155 (2)C9—C141.423 (4)
O2—C141.313 (3)C10—C111.362 (4)
O2—Zn1i1.988 (2)C10—H100.9300
N1—C81.288 (3)C11—C121.389 (4)
N1—C71.484 (3)C11—H110.9300
N1—Zn1i2.045 (2)C12—C131.368 (4)
N2—C191.335 (3)C12—H120.9300
N2—C151.344 (3)C13—C141.413 (4)
C1—C21.394 (4)C13—H130.9300
C1—C61.411 (4)C15—C161.383 (4)
C2—C31.392 (4)C15—H150.9300
C2—H20.9300C16—C171.357 (5)
C3—C41.376 (4)C16—H160.9300
C3—H30.9300C17—C181.366 (5)
C4—C51.379 (4)C17—H170.9300
C4—H40.9300C18—C191.390 (4)
C5—C61.389 (4)C18—H180.9300
C5—H50.9300C19—H190.9300
O1—Zn1—O2i101.29 (8)C6—C7—H7A109.1
O1—Zn1—N1i127.04 (8)N1—C7—H7B109.1
O2i—Zn1—N1i92.31 (8)C6—C7—H7B109.1
O1—Zn1—N2112.80 (9)H7A—C7—H7B107.8
O2i—Zn1—N293.97 (9)N1—C8—C9127.0 (3)
N1i—Zn1—N2117.01 (8)N1—C8—H8116.5
O1—Zn1—O1i76.26 (8)C9—C8—H8116.5
O2i—Zn1—O1i175.72 (8)C10—C9—C14119.2 (3)
N1i—Zn1—O1i86.51 (8)C10—C9—C8116.3 (2)
N2—Zn1—O1i90.23 (8)C14—C9—C8124.4 (2)
C1—O1—Zn1135.25 (16)C11—C10—C9122.3 (3)
C1—O1—Zn1i120.19 (15)C11—C10—H10118.9
Zn1—O1—Zn1i103.74 (8)C9—C10—H10118.9
C14—O2—Zn1i125.11 (17)C10—C11—C12118.8 (3)
C8—N1—C7117.6 (2)C10—C11—H11120.6
C8—N1—Zn1i122.84 (19)C12—C11—H11120.6
C7—N1—Zn1i119.56 (18)C13—C12—C11120.6 (3)
C19—N2—C15117.8 (3)C13—C12—H12119.7
C19—N2—Zn1122.13 (19)C11—C12—H12119.7
C15—N2—Zn1120.0 (2)C12—C13—C14122.7 (3)
O1—C1—C2121.8 (2)C12—C13—H13118.6
O1—C1—C6119.1 (2)C14—C13—H13118.6
C2—C1—C6119.1 (2)O2—C14—C13119.3 (2)
C3—C2—C1120.5 (3)O2—C14—C9124.3 (2)
C3—C2—H2119.8C13—C14—C9116.4 (3)
C1—C2—H2119.8N2—C15—C16122.3 (3)
C4—C3—C2120.4 (3)N2—C15—H15118.8
C4—C3—H3119.8C16—C15—H15118.8
C2—C3—H3119.8C17—C16—C15119.1 (3)
C3—C4—C5119.6 (3)C17—C16—H16120.5
C3—C4—H4120.2C15—C16—H16120.5
C5—C4—H4120.2C16—C17—C18119.6 (3)
C4—C5—C6121.5 (3)C16—C17—H17120.2
C4—C5—H5119.2C18—C17—H17120.2
C6—C5—H5119.2C17—C18—C19118.8 (3)
C5—C6—C1119.0 (3)C17—C18—H18120.6
C5—C6—C7122.1 (3)C19—C18—H18120.6
C1—C6—C7118.9 (2)N2—C19—C18122.3 (3)
N1—C7—C6112.5 (2)N2—C19—H19118.8
N1—C7—H7A109.1C18—C19—H19118.8
O2i—Zn1—O1—C1−14.5 (3)C2—C1—C6—C7−177.7 (2)
N1i—Zn1—O1—C1−116.1 (2)C8—N1—C7—C6−125.5 (3)
N2—Zn1—O1—C184.8 (3)Zn1i—N1—C7—C656.0 (3)
O1i—Zn1—O1—C1169.1 (3)C5—C6—C7—N1122.3 (3)
O2i—Zn1—O1—Zn1i176.41 (8)C1—C6—C7—N1−60.5 (3)
N1i—Zn1—O1—Zn1i74.75 (12)C7—N1—C8—C9−178.2 (2)
N2—Zn1—O1—Zn1i−84.36 (10)Zn1i—N1—C8—C90.3 (4)
O1i—Zn1—O1—Zn1i0.0N1—C8—C9—C10−171.4 (3)
O1—Zn1—N2—C1953.3 (2)N1—C8—C9—C1411.1 (4)
O2i—Zn1—N2—C19157.3 (2)C14—C9—C10—C11−0.8 (5)
N1i—Zn1—N2—C19−108.1 (2)C8—C9—C10—C11−178.5 (3)
O1i—Zn1—N2—C19−21.9 (2)C9—C10—C11—C120.4 (5)
O1—Zn1—N2—C15−128.6 (2)C10—C11—C12—C130.0 (6)
O2i—Zn1—N2—C15−24.6 (2)C11—C12—C13—C14−0.1 (6)
N1i—Zn1—N2—C1570.0 (2)Zn1i—O2—C14—C13162.6 (2)
O1i—Zn1—N2—C15156.2 (2)Zn1i—O2—C14—C9−17.7 (4)
Zn1—O1—C1—C263.6 (4)C12—C13—C14—O2179.6 (3)
Zn1i—O1—C1—C2−128.6 (2)C12—C13—C14—C9−0.2 (5)
Zn1—O1—C1—C6−118.3 (2)C10—C9—C14—O2−179.1 (3)
Zn1i—O1—C1—C649.4 (3)C8—C9—C14—O2−1.6 (4)
O1—C1—C2—C3177.4 (3)C10—C9—C14—C130.6 (4)
C6—C1—C2—C3−0.6 (4)C8—C9—C14—C13178.1 (3)
C1—C2—C3—C41.1 (5)C19—N2—C15—C160.8 (4)
C2—C3—C4—C5−0.5 (5)Zn1—N2—C15—C16−177.4 (2)
C3—C4—C5—C6−0.6 (5)N2—C15—C16—C170.1 (5)
C4—C5—C6—C11.0 (4)C15—C16—C17—C18−1.1 (5)
C4—C5—C6—C7178.2 (3)C16—C17—C18—C191.1 (5)
O1—C1—C6—C5−178.5 (2)C15—N2—C19—C18−0.7 (4)
C2—C1—C6—C5−0.4 (4)Zn1—N2—C19—C18177.5 (2)
O1—C1—C6—C74.2 (4)C17—C18—C19—N2−0.3 (5)
  2 in total

1.  Isolation of a Pyridinium Alkoxy Ion Bridged Dimeric Zinc Complex for the Coupling Reactions of CO(2) and Epoxides This work was supported by the Ministry of Science and Technology. We thank Dr. Young-A Lee, KIST, for the X-ray crystallographic analysis.

Authors: 
Journal:  Angew Chem Int Ed Engl       Date:  2000-11-17       Impact factor: 15.336

2.  A short history of SHELX.

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

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