Literature DB >> 21754309

Poly[tetra-kis(μ(4)-4,6-dimethyl-5-nitro-benzene-1,3-dicarboxyl-ato-κO:O:O:O)bis-(pyridine-κN)dizinc].

Qing-Yu Ma1, Rui-Fang Guan, Guo-Zhong Li.   

Abstract

In the title complex, [Zn(2)(C(10)H(7)NO(6))(2)(C(5)H(5)N)(2)](n), the repeat unit is a centrosymmetic tetra-carboxyl-ato-O,O'-bridged dimer in which each Zn(II) atom is five-coordinated by four O atoms from different dianionic 4,6-dimethyl-5-nitro-iso-phthalate ligands [Zn-O = 2.0283 (18)-2.0540 (19) Å] and one N atom from a pyridine mol-ecule [Zn-N = 2.030 (2) Å] in the axial site of a slightly distorted square-pyramidal coordination sphere. The Zn⋯Zn separation is 2.9750 (6) Å. The complex dimers are extended into a two-dimensional polymeric structure parallel to (100) through bridges provided by the second carboxyl-ate group of the ligand.

Entities:  

Year:  2011        PMID： 21754309      PMCID： PMC3089336          DOI： 10.1107/S1600536811013092

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


Related literature

For the structure of a similar but discrete tetra-carboxyl­ato-bridged Zn2 dimer, see: Yu et al. (2011 ▶).

Experimental

Crystal data

[Zn(C10H7NO6)(C5H5N)] M = 381.64 Monoclinic, a = 10.2947 (9) Å b = 11.8526 (10) Å c = 12.8501 (11) Å β = 97.933 (2)° V = 1553.0 (2) Å3 Z = 4 Mo Kα radiation μ = 1.62 mm−1 T = 298 K 0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.824, T max = 0.879 8899 measured reflections 3525 independent reflections 2750 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.033 wR(F 2) = 0.081 S = 1.03 3525 reflections 217 parameters H-atom parameters constrained Δρmax = 0.43 e Å−3 Δρmin = −0.43 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); 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 global, I. DOI: 10.1107/S1600536811013092/zs2089sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811013092/zs2089Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Zn(C10H7NO6)(C5H5N)]F(000) = 776
Mr = 381.64Dx = 1.632 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2968 reflections
a = 10.2947 (9) Åθ = 2.3–26.1°
b = 11.8526 (10) ŵ = 1.62 mm−1
c = 12.8501 (11) ÅT = 298 K
β = 97.933 (2)°Rod, colourless
V = 1553.0 (2) Å30.12 × 0.10 × 0.08 mm
Z = 4
Bruker APEXII CCD area-detector diffractometer3525 independent reflections
Radiation source: fine-focus sealed tube2750 reflections with I > 2σ(I)
graphiteRint = 0.029
φ and ω scansθmax = 27.7°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −8→13
Tmin = 0.824, Tmax = 0.879k = −15→15
8899 measured reflectionsl = −16→16
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0353P)2 + 0.6981P] where P = (Fo2 + 2Fc2)/3
3525 reflections(Δ/σ)max = 0.001
217 parametersΔρmax = 0.43 e Å−3
0 restraintsΔρmin = −0.43 e Å−3
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles
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*/UeqOcc. (<1)
Zn10.63668 (3)−0.03544 (2)0.53898 (2)0.0233 (1)
O10.65410 (19)0.13708 (16)0.54695 (18)0.0546 (8)
O20.4496 (2)0.18909 (15)0.49411 (17)0.0508 (7)
O30.55390 (18)−0.03094 (18)0.67374 (14)0.0454 (7)
O40.6491 (2)−0.02213 (19)0.38329 (14)0.0499 (7)
O50.7497 (2)0.62087 (19)0.42547 (16)0.0600 (8)
O60.9095 (2)0.5865 (2)0.5453 (2)0.0703 (10)
N10.7959 (2)0.57613 (18)0.50579 (17)0.0352 (7)
N20.8232 (2)−0.07998 (17)0.59645 (16)0.0298 (6)
C10.5998 (2)0.32743 (18)0.56737 (17)0.0245 (7)
C20.6751 (2)0.39863 (19)0.51257 (17)0.0253 (7)
C30.7112 (2)0.50127 (19)0.56086 (18)0.0258 (7)
C40.6795 (2)0.53868 (18)0.65714 (17)0.0253 (7)
C50.5997 (2)0.46553 (19)0.70674 (17)0.0235 (6)
C60.5600 (2)0.36307 (19)0.66100 (17)0.0260 (7)
C70.5647 (3)0.2080 (2)0.53197 (18)0.0283 (7)
C80.7134 (3)0.3664 (2)0.4076 (2)0.0382 (9)
C90.7241 (3)0.6519 (2)0.7019 (2)0.0416 (9)
C100.5618 (2)0.48883 (19)0.81384 (17)0.0259 (7)
C110.9056 (3)−0.1198 (3)0.5336 (2)0.0455 (10)
C121.0338 (3)−0.1460 (3)0.5712 (3)0.0625 (14)
C131.0764 (3)−0.1350 (3)0.6760 (3)0.0739 (15)
C140.9916 (4)−0.0970 (4)0.7408 (3)0.0817 (14)
C150.8655 (3)−0.0695 (3)0.6982 (2)0.0559 (11)
H6A0.505200.316800.694000.0310*
H8A0.678900.293000.387900.0570*0.500
H8B0.807200.365100.412300.0570*0.500
H8C0.678300.420600.355700.0570*0.500
H8D0.764100.426100.382700.0570*0.500
H8E0.635800.354100.358300.0570*0.500
H8F0.764600.298500.414900.0570*0.500
H9A0.692500.662600.768100.0620*0.500
H9B0.690000.710400.654100.0620*0.500
H9C0.818200.654900.712200.0620*0.500
H9D0.774700.689300.654800.0620*0.500
H9E0.777100.641500.768800.0620*0.500
H9F0.648900.697000.710800.0620*0.500
H11A0.87570−0.130000.462600.0550*
H12A1.09060−0.170900.525800.0750*
H13A1.16230−0.153200.703000.0890*
H14A1.01850−0.089800.812600.0980*
H15A0.80810−0.042700.742300.0670*
U11U22U33U12U13U23
Zn10.0253 (2)0.0240 (2)0.0210 (1)0.0011 (1)0.0044 (1)0.0003 (1)
O10.0406 (12)0.0231 (10)0.0991 (18)0.0015 (9)0.0057 (12)−0.0082 (10)
O20.0471 (12)0.0278 (10)0.0708 (14)−0.0077 (9)−0.0156 (10)−0.0060 (9)
O30.0346 (10)0.0791 (15)0.0245 (9)0.0051 (10)0.0108 (8)0.0017 (9)
O40.0510 (12)0.0788 (15)0.0218 (9)0.0216 (11)0.0114 (9)0.0125 (9)
O50.0789 (16)0.0588 (14)0.0439 (12)−0.0111 (12)0.0142 (11)0.0230 (11)
O60.0460 (14)0.0838 (18)0.0819 (18)−0.0243 (13)0.0113 (13)0.0200 (15)
N10.0456 (14)0.0298 (11)0.0338 (12)−0.0076 (10)0.0185 (10)−0.0013 (9)
N20.0285 (11)0.0286 (10)0.0324 (11)0.0014 (9)0.0047 (9)−0.0001 (9)
C10.0281 (12)0.0225 (11)0.0229 (11)−0.0012 (9)0.0036 (9)−0.0028 (9)
C20.0302 (12)0.0246 (12)0.0220 (11)0.0007 (10)0.0064 (9)−0.0024 (9)
C30.0298 (13)0.0227 (11)0.0261 (12)−0.0020 (9)0.0077 (10)0.0036 (9)
C40.0317 (13)0.0204 (11)0.0239 (11)−0.0007 (10)0.0043 (9)−0.0005 (9)
C50.0278 (12)0.0243 (11)0.0189 (10)0.0017 (10)0.0047 (9)−0.0002 (9)
C60.0303 (13)0.0243 (12)0.0244 (12)−0.0048 (9)0.0079 (10)0.0010 (9)
C70.0412 (15)0.0237 (12)0.0215 (11)−0.0049 (11)0.0100 (10)−0.0010 (9)
C80.0552 (18)0.0334 (14)0.0293 (13)0.0001 (12)0.0171 (12)−0.0026 (11)
C90.0616 (19)0.0268 (13)0.0390 (15)−0.0123 (13)0.0160 (14)−0.0078 (11)
C100.0355 (14)0.0236 (12)0.0195 (11)0.0024 (10)0.0075 (10)0.0011 (9)
C110.0412 (17)0.0514 (18)0.0456 (16)0.0133 (14)0.0122 (13)0.0050 (14)
C120.0423 (19)0.066 (2)0.083 (3)0.0198 (16)0.0219 (18)0.004 (2)
C130.0309 (18)0.073 (3)0.111 (3)0.0081 (17)−0.0148 (19)−0.020 (2)
C140.053 (2)0.110 (3)0.071 (2)0.023 (2)−0.0308 (19)−0.039 (2)
C150.0443 (18)0.074 (2)0.0458 (18)0.0131 (16)−0.0064 (14)−0.0239 (16)
Zn1—O12.0540 (19)C5—C101.507 (3)
Zn1—O32.0336 (18)C11—C121.377 (4)
Zn1—O42.0283 (18)C12—C131.364 (5)
Zn1—N22.030 (2)C13—C141.363 (5)
Zn1—O2i2.0450 (19)C14—C151.377 (5)
O1—C71.242 (3)C6—H6A0.9300
O2—C71.238 (4)C8—H8A0.9600
O3—C10ii1.246 (3)C8—H8B0.9600
O4—C10iii1.240 (3)C8—H8C0.9600
O5—N11.199 (3)C8—H8D0.9600
O6—N11.215 (3)C8—H8E0.9600
N1—C31.490 (3)C8—H8F0.9600
N2—C111.336 (4)C9—H9A0.9600
N2—C151.326 (3)C9—H9B0.9600
C1—C21.400 (3)C9—H9C0.9600
C1—C61.389 (3)C9—H9D0.9600
C1—C71.515 (3)C9—H9E0.9600
C2—C31.393 (3)C9—H9F0.9600
C2—C81.506 (3)C11—H11A0.9300
C3—C41.395 (3)C12—H12A0.9300
C4—C51.406 (3)C13—H13A0.9300
C4—C91.507 (3)C14—H14A0.9300
C5—C61.386 (3)C15—H15A0.9300
O1—Zn1—O388.59 (9)N2—C11—C12121.7 (3)
O1—Zn1—O487.41 (9)C11—C12—C13119.1 (3)
O1—Zn1—N299.73 (8)C12—C13—C14119.3 (3)
O1—Zn1—O2i158.34 (8)C13—C14—C15118.9 (3)
O3—Zn1—O4158.24 (8)N2—C15—C14122.2 (3)
O3—Zn1—N2100.58 (8)C1—C6—H6A119.00
O2i—Zn1—O388.82 (8)C5—C6—H6A119.00
O4—Zn1—N2101.18 (8)C2—C8—H8A109.00
O2i—Zn1—O487.07 (9)C2—C8—H8B109.00
O2i—Zn1—N2101.89 (8)C2—C8—H8C109.00
Zn1—O1—C7127.48 (18)C2—C8—H8D109.00
Zn1i—O2—C7127.43 (17)C2—C8—H8E109.00
Zn1—O3—C10ii129.39 (16)C2—C8—H8F109.00
Zn1—O4—C10iii126.61 (17)H8A—C8—H8B110.00
O5—N1—O6124.0 (2)H8A—C8—H8C109.00
O5—N1—C3118.9 (2)H8B—C8—H8C109.00
O6—N1—C3117.0 (2)H8D—C8—H8E109.00
Zn1—N2—C11121.32 (17)H8D—C8—H8F110.00
Zn1—N2—C15120.00 (19)H8E—C8—H8F109.00
C11—N2—C15118.7 (2)C4—C9—H9A109.00
C2—C1—C6120.2 (2)C4—C9—H9B109.00
C2—C1—C7122.5 (2)C4—C9—H9C110.00
C6—C1—C7117.2 (2)C4—C9—H9D110.00
C1—C2—C3115.8 (2)C4—C9—H9E109.00
C1—C2—C8122.0 (2)C4—C9—H9F109.00
C3—C2—C8122.3 (2)H9A—C9—H9B109.00
N1—C3—C2116.51 (19)H9A—C9—H9C109.00
N1—C3—C4117.13 (19)H9B—C9—H9C110.00
C2—C3—C4126.3 (2)H9D—C9—H9E109.00
C3—C4—C5115.4 (2)H9D—C9—H9F110.00
C3—C4—C9121.7 (2)H9E—C9—H9F109.00
C5—C4—C9122.9 (2)N2—C11—H11A119.00
C4—C5—C6120.3 (2)C12—C11—H11A119.00
C4—C5—C10122.8 (2)C11—C12—H12A120.00
C6—C5—C10116.71 (19)C13—C12—H12A120.00
C1—C6—C5121.9 (2)C12—C13—H13A120.00
O1—C7—O2126.0 (2)C14—C13—H13A120.00
O1—C7—C1116.4 (2)C13—C14—H14A121.00
O2—C7—C1117.6 (2)C15—C14—H14A121.00
O3iv—C10—C5117.08 (19)N2—C15—H15A119.00
O4v—C10—C5117.53 (19)C14—C15—H15A119.00
O3iv—C10—O4v125.3 (2)
O3—Zn1—O1—C7−70.9 (2)C15—N2—C11—C12−2.4 (5)
O4—Zn1—O1—C787.7 (2)C11—N2—C15—C140.8 (5)
N2—Zn1—O1—C7−171.4 (2)Zn1—N2—C11—C12177.4 (3)
O2i—Zn1—O1—C712.3 (4)Zn1—N2—C15—C14−179.1 (3)
O1—Zn1—O3—C10ii82.6 (2)C2—C1—C6—C5−4.3 (3)
O4—Zn1—O3—C10ii3.2 (4)C2—C1—C7—O174.4 (3)
N2—Zn1—O3—C10ii−177.8 (2)C7—C1—C2—C87.3 (3)
O2i—Zn1—O3—C10ii−75.9 (2)C7—C1—C6—C5172.4 (2)
O1—Zn1—O4—C10iii−75.2 (2)C6—C1—C2—C33.3 (3)
O3—Zn1—O4—C10iii4.4 (4)C6—C1—C7—O275.5 (3)
N2—Zn1—O4—C10iii−174.7 (2)C7—C1—C2—C3−173.3 (2)
O2i—Zn1—O4—C10iii83.8 (2)C6—C1—C2—C8−176.2 (2)
O1—Zn1—N2—C11−106.3 (2)C6—C1—C7—O1−102.3 (3)
O1—Zn1—N2—C1573.6 (2)C2—C1—C7—O2−107.9 (3)
O3—Zn1—N2—C11163.4 (2)C8—C2—C3—C4179.4 (2)
O3—Zn1—N2—C15−16.8 (2)C8—C2—C3—N1−2.9 (3)
O4—Zn1—N2—C11−17.0 (2)C1—C2—C3—C40.0 (3)
O4—Zn1—N2—C15162.8 (2)C1—C2—C3—N1177.59 (19)
O2i—Zn1—N2—C1172.3 (2)N1—C3—C4—C92.4 (3)
O2i—Zn1—N2—C15−107.8 (2)C2—C3—C4—C5−2.2 (3)
O1—Zn1—O2i—C7i−3.3 (4)C2—C3—C4—C9−180.0 (2)
O3—Zn1—O2i—C7i79.9 (2)N1—C3—C4—C5−179.84 (19)
O4—Zn1—O2i—C7i−78.7 (2)C3—C4—C5—C61.3 (3)
N2—Zn1—O2i—C7i−179.5 (2)C9—C4—C5—C6179.0 (2)
Zn1—O1—C7—O2−11.5 (4)C3—C4—C5—C10176.5 (2)
Zn1—O1—C7—C1166.09 (17)C9—C4—C5—C10−5.8 (3)
Zn1i—O2—C7—O18.2 (4)C10—C5—C6—C1−173.6 (2)
Zn1i—O2—C7—C1−169.35 (16)C4—C5—C10—O3iv138.0 (2)
Zn1—O3—C10ii—C5ii169.14 (16)C4—C5—C10—O4v−44.5 (3)
Zn1—O3—C10ii—O4i−8.1 (4)C6—C5—C10—O3iv−46.6 (3)
Zn1—O4—C10iii—O3i−8.2 (4)C6—C5—C10—O4v130.9 (2)
Zn1—O4—C10iii—C5iii169.07 (16)C4—C5—C6—C11.9 (3)
O6—N1—C3—C2−108.6 (3)N2—C11—C12—C132.5 (5)
O5—N1—C3—C4−111.8 (3)C11—C12—C13—C14−0.8 (6)
O6—N1—C3—C469.3 (3)C12—C13—C14—C15−0.8 (6)
O5—N1—C3—C270.4 (3)C13—C14—C15—N20.8 (6)
  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.  Tetra-kis-(μ-benzoato-κO:O')bis{[4-(di-methyl-amino)-pyridine-κN]zinc(II)}.

Authors:  Zhe-Yin Yu; Kun-Hua Lin; Fei-Fei Zhang; Min Shao; Ming Li
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15
  2 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.