Literature DB >> 21200498

catena-Poly[[aqua-copper(II)]-μ-[(S)-N-(2-hydroxy-benz-yl)-l-aspartato]].

Lei Zhang1, Bai-Wang Sun.   

Abstract

The title compound, [Cu(C(11)H(11)NO(5))(H(2)O)](n), was obtained by the reaction of Cu(NO(3))(2) and the homochiral organic ligand (S)-N-(2-hydroxy-benz-yl)-l-aspartic acid (S-H(3)sasp). The Cu(II) ion has a distorted square-pyramidal geometry and is coordinated by one N atom and three O atoms from the organic ligand and one O atom from a water mol-ecule. The carboxyl O atoms of the ligands bridge the Cu atoms to form an infinite one-dimensional zigzag chain. Inter-molecular hydrogen bonds link these chains into a two-dimensional arrangement.

Entities:  

Year:  2007        PMID： 21200498      PMCID： PMC2915087          DOI： 10.1107/S1600536807046922

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


Related literature

For related literature, see: Yang et al. (2004 ▶); Lü et al. (2005 ▶); Sreenivasulu & Vittal (2004 ▶); Sreenivasulu et al. (2005 ▶); Wang et al. (2006 ▶).

Experimental

Crystal data

[Cu(C11H11NO5)(H2O)] M = 318.77 Monoclinic, a = 5.9107 (13) Å b = 8.826 (2) Å c = 11.903 (3) Å β = 93.787 (19)° V = 619.6 (3) Å3 Z = 2 Mo Kα radiation μ = 1.79 mm−1 T = 293 (2) K 0.2 × 0.2 × 0.2 mm

Data collection

Rigaku Mercury2 diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T min = 0.690, T max = 0.703 6500 measured reflections 2934 independent reflections 2532 reflections with I > 2σ(I) R int = 0.058

Refinement

R[F 2 > 2σ(F 2)] = 0.041 wR(F 2) = 0.079 S = 0.99 2934 reflections 172 parameters 1 restraint H-atom parameters constrained Δρmax = 0.48 e Å−3 Δρmin = −0.41 e Å−3 Absolute structure: Flack (1983 ▶), 1355 Friedel pairs Flack parameter: 0.064 (16) Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Sheldrick, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807046922/pk2047sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807046922/pk2047Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu(C11H11NO5)(H2O)]F000 = 326
Mr = 318.77Dx = 1.709 Mg m−3
Monoclinic, P21Mo Kα radiation λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 1876 reflections
a = 5.9107 (13) Åθ = 3.4–27.5º
b = 8.826 (2) ŵ = 1.79 mm−1
c = 11.903 (3) ÅT = 293 (2) K
β = 93.787 (19)ºPrism, colourless
V = 619.6 (3) Å30.2 × 0.2 × 0.2 mm
Z = 2
Rigaku Mercury2 (2x2 bin mode) diffractometer2934 independent reflections
Radiation source: fine-focus sealed tube2532 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.058
Detector resolution: 13.6612 pixels mm-1θmax = 27.9º
T = 293(2) Kθmin = 2.9º
ω scansh = −7→7
Absorption correction: multi-scan(CrystalClear; Rigaku, 2005)k = −11→11
Tmin = 0.690, Tmax = 0.703l = −15→15
6500 measured reflections
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.041  w = 1/[σ2(Fo2) + (0.0135P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.079(Δ/σ)max = 0.001
S = 0.99Δρmax = 0.48 e Å−3
2934 reflectionsΔρmin = −0.41 e Å−3
172 parametersExtinction correction: none
1 restraintAbsolute structure: Flack (1983), 1355 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.064 (16)
Secondary atom site location: difference Fourier map
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 > 2σ(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
Cu10.10776 (6)0.12114 (6)0.91119 (3)0.02344 (12)
O2−0.2062 (4)0.0614 (3)0.8604 (2)0.0281 (6)
O1W0.4293 (4)0.1802 (3)0.9514 (2)0.0474 (9)
H1WA0.51390.13010.91410.071*
H1WB0.46890.26970.96840.071*
N10.1790 (5)0.0507 (3)0.7580 (2)0.0202 (6)
H1B0.32410.00250.77020.024*
O10.0408 (5)0.3744 (3)0.8257 (2)0.0410 (7)
H1A0.01570.45580.85570.061*
C80.0087 (6)−0.0670 (4)0.7261 (3)0.0212 (8)
H8A−0.0121−0.07150.64380.025*
O3−0.3920 (4)−0.0856 (3)0.7316 (3)0.0415 (8)
C6−0.0171 (7)0.2611 (4)0.6464 (3)0.0285 (9)
C9−0.2184 (6)−0.0274 (4)0.7737 (3)0.0226 (8)
C1−0.0879 (7)0.3633 (5)0.7264 (3)0.0309 (9)
C2−0.2846 (7)0.4502 (5)0.7032 (4)0.0408 (11)
H2A−0.33370.51720.75680.049*
C5−0.1454 (8)0.2473 (5)0.5451 (3)0.0393 (12)
H5A−0.10140.17820.49180.047*
C70.1977 (7)0.1710 (4)0.6726 (3)0.0312 (9)
H7A0.24260.12500.60350.037*
H7B0.31730.24030.69870.037*
C3−0.4050 (8)0.4350 (6)0.6000 (4)0.0506 (13)
H3A−0.53340.49380.58350.061*
C100.0854 (6)−0.2238 (4)0.7707 (3)0.0239 (8)
H10A−0.0131−0.30080.73580.029*
H10B0.2382−0.24340.74930.029*
C110.0808 (6)−0.2362 (4)0.8979 (3)0.0238 (8)
C4−0.3354 (9)0.3333 (6)0.5220 (4)0.0505 (13)
H4A−0.41770.32290.45310.061*
O5−0.0374 (4)−0.3461 (3)0.9343 (2)0.0297 (7)
O40.1842 (5)−0.1414 (3)0.9602 (2)0.0350 (7)
U11U22U33U12U13U23
Cu10.01864 (19)0.0292 (2)0.0225 (2)−0.0011 (2)0.00118 (15)−0.0045 (2)
O20.0185 (13)0.0362 (14)0.0302 (14)−0.0005 (11)0.0067 (11)−0.0075 (12)
O1W0.0204 (15)0.061 (2)0.060 (2)−0.0040 (13)0.0016 (14)−0.0351 (17)
N10.0182 (15)0.0212 (14)0.0213 (15)−0.0010 (12)0.0014 (12)−0.0015 (13)
O10.0457 (18)0.0356 (16)0.0408 (17)0.0072 (14)−0.0029 (15)−0.0119 (14)
C80.0221 (19)0.0250 (18)0.0167 (17)−0.0038 (16)0.0027 (15)−0.0007 (15)
O30.0161 (14)0.054 (2)0.0540 (19)−0.0037 (13)−0.0015 (13)−0.0196 (15)
C60.039 (2)0.0231 (19)0.024 (2)−0.0066 (17)0.0083 (18)0.0059 (16)
C90.0185 (18)0.028 (2)0.0207 (18)0.0008 (15)−0.0036 (15)0.0019 (15)
C10.034 (2)0.024 (2)0.034 (2)−0.0066 (18)0.0044 (19)0.0021 (18)
C20.038 (2)0.027 (2)0.057 (3)−0.002 (2)0.003 (2)0.001 (2)
C50.060 (3)0.038 (3)0.020 (2)−0.010 (2)0.002 (2)0.0048 (19)
C70.036 (2)0.026 (2)0.033 (2)−0.0079 (16)0.0151 (18)0.0016 (15)
C30.036 (3)0.039 (2)0.077 (4)−0.006 (2)0.000 (3)0.028 (3)
C100.024 (2)0.0228 (18)0.0253 (19)−0.0027 (16)0.0057 (16)−0.0012 (16)
C110.027 (2)0.0228 (18)0.0220 (19)0.0082 (16)0.0042 (17)0.0037 (15)
C40.059 (3)0.055 (3)0.035 (3)−0.018 (3)−0.014 (2)0.024 (2)
O50.0316 (14)0.0326 (19)0.0252 (13)−0.0070 (12)0.0045 (11)0.0059 (11)
O40.0492 (18)0.0286 (15)0.0255 (14)−0.0088 (15)−0.0093 (13)0.0005 (12)
Cu1—O5i1.934 (2)C6—C11.395 (6)
Cu1—O21.985 (3)C6—C71.513 (5)
Cu1—N11.998 (3)C1—C21.405 (6)
Cu1—O1W1.998 (3)C2—C31.385 (6)
Cu1—O42.424 (3)C2—H2A0.9300
O2—C91.294 (4)C5—C41.368 (7)
O1W—H1WA0.8200C5—H5A0.9300
O1W—H1WB0.8442C7—H7A0.9700
N1—C81.479 (4)C7—H7B0.9700
N1—C71.479 (4)C3—C41.374 (7)
N1—H1B0.9600C3—H3A0.9300
O1—C11.366 (4)C10—C111.520 (5)
O1—H1A0.8200C10—H10A0.9700
C8—C91.532 (5)C10—H10B0.9700
C8—C101.540 (5)C11—O41.250 (5)
C8—H8A0.9800C11—O51.287 (4)
O3—C91.225 (4)C4—H4A0.9300
C6—C51.387 (6)O5—Cu1ii1.934 (2)
O5i—Cu1—O294.24 (11)O1—C1—C6117.5 (4)
O5i—Cu1—N1170.47 (11)O1—C1—C2122.5 (4)
O2—Cu1—N183.59 (12)C6—C1—C2120.1 (4)
O5i—Cu1—O1W89.66 (11)C3—C2—C1119.4 (4)
O2—Cu1—O1W176.09 (11)C3—C2—H2A120.3
N1—Cu1—O1W92.61 (12)C1—C2—H2A120.3
O5i—Cu1—O487.84 (10)C4—C5—C6121.4 (4)
O2—Cu1—O488.57 (10)C4—C5—H5A119.3
N1—Cu1—O482.84 (11)C6—C5—H5A119.3
O1W—Cu1—O491.87 (11)N1—C7—C6114.7 (3)
C9—O2—Cu1113.9 (2)N1—C7—H7A108.6
Cu1—O1W—H1WA109.5C6—C7—H7A108.6
Cu1—O1W—H1WB123.1N1—C7—H7B108.6
H1WA—O1W—H1WB117.7C6—C7—H7B108.6
C8—N1—C7114.1 (3)H7A—C7—H7B107.6
C8—N1—Cu1105.8 (2)C4—C3—C2120.2 (4)
C7—N1—Cu1115.7 (2)C4—C3—H3A119.9
C8—N1—H1B108.3C2—C3—H3A119.9
C7—N1—H1B108.4C11—C10—C8112.6 (3)
Cu1—N1—H1B103.9C11—C10—H10A109.1
C1—O1—H1A109.5C8—C10—H10A109.1
N1—C8—C9110.1 (3)C11—C10—H10B109.1
N1—C8—C10111.3 (3)C8—C10—H10B109.1
C9—C8—C10108.8 (3)H10A—C10—H10B107.8
N1—C8—H8A108.9O4—C11—O5124.0 (3)
C9—C8—H8A108.9O4—C11—C10120.2 (3)
C10—C8—H8A108.9O5—C11—C10115.8 (3)
C5—C6—C1118.6 (4)C5—C4—C3120.3 (4)
C5—C6—C7122.4 (4)C5—C4—H4A119.8
C1—C6—C7119.0 (4)C3—C4—H4A119.8
O3—C9—O2125.6 (3)C11—O5—Cu1ii126.0 (2)
O3—C9—C8118.9 (3)C11—O4—Cu1114.9 (2)
O2—C9—C8115.4 (3)
O5i—Cu1—O2—C9−153.3 (2)O1—C1—C2—C3179.0 (4)
N1—Cu1—O2—C917.3 (2)C6—C1—C2—C3−1.0 (6)
O4—Cu1—O2—C9−65.6 (2)C1—C6—C5—C41.2 (6)
O2—Cu1—N1—C8−28.4 (2)C7—C6—C5—C4−178.0 (4)
O1W—Cu1—N1—C8152.5 (2)C8—N1—C7—C660.9 (4)
O4—Cu1—N1—C861.0 (2)Cu1—N1—C7—C6−62.2 (4)
O2—Cu1—N1—C799.0 (3)C5—C6—C7—N1−108.9 (4)
O1W—Cu1—N1—C7−80.0 (3)C1—C6—C7—N171.9 (4)
O4—Cu1—N1—C7−171.6 (3)C1—C2—C3—C41.5 (6)
C7—N1—C8—C9−93.8 (3)N1—C8—C10—C1170.4 (4)
Cu1—N1—C8—C934.5 (3)C9—C8—C10—C11−51.0 (4)
C7—N1—C8—C10145.4 (3)C8—C10—C11—O4−54.0 (5)
Cu1—N1—C8—C10−86.2 (3)C8—C10—C11—O5124.7 (3)
Cu1—O2—C9—O3175.6 (3)C6—C5—C4—C3−0.7 (6)
Cu1—O2—C9—C8−1.0 (4)C2—C3—C4—C5−0.6 (6)
N1—C8—C9—O3159.8 (3)O4—C11—O5—Cu1ii6.6 (5)
C10—C8—C9—O3−78.0 (4)C10—C11—O5—Cu1ii−172.1 (2)
N1—C8—C9—O2−23.4 (4)O5—C11—O4—Cu1−128.6 (3)
C10—C8—C9—O298.9 (3)C10—C11—O4—Cu150.0 (4)
C5—C6—C1—O1179.7 (3)O5i—Cu1—O4—C11127.5 (3)
C7—C6—C1—O1−1.1 (5)O2—Cu1—O4—C1133.2 (3)
C5—C6—C1—C2−0.3 (6)N1—Cu1—O4—C11−50.5 (3)
C7—C6—C1—C2178.9 (3)O1W—Cu1—O4—C11−142.9 (3)
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2iii0.821.912.688 (3)158
O1W—H1WB···O4iv0.842.302.913 (4)129
N1—H1B···O3iii0.961.932.843 (4)158
O1—H1A···O5v0.822.022.837 (4)178
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1WA⋯O2i0.821.912.688 (3)158
O1W—H1WB⋯O4ii0.842.302.913 (4)129
N1—H1B⋯O3i0.961.932.843 (4)158
O1—H1A⋯O5iii0.822.022.837 (4)178

Symmetry codes: (i) ; (ii) ; (iii) .

  1 in total

1.  Helix inside a Helix: encapsulation of hydrogen-bonded water molecules in a staircase coordination polymer.

Authors:  Bellam Sreenivasulu; Jagadese J Vittal
Journal:  Angew Chem Int Ed Engl       Date:  2004-11-05       Impact factor: 15.336
  1 in total

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