Literature DB >> 21579016

Hexaaqua-manganese(II) bis-{[N-(3-meth-oxy-2-oxidobenzyl-idene)glycylglycinato]copper(II)} hexa-hydrate.

Long-Wei Lei1, Yin-Zhi Jiang, Yang Zou.   

Abstract

The ligand N-(2-hydr-oxy-3-methoxy-benzyl-idene)glycylglycine (H(3)L), a Schiff base derived from glycylglycine and 3-methoxy-salicylaldehyde, was used in the synthesis of a new organic-inorganic coordination complex, [Mn(H(2)O)(6)][Cu(C(12)H(11)N(2)O(5))](2)·6H(2)O. The Mn(II) atom is located on an inversion center and is coordinated to six water mol-ecules in a slightly distorted octa-hedral geometry. The Cu(II) atom is chelated by the tetra-dentate Schiff base ligand in a distorted CuN(2)O(2) square-planar coordination. In the crystal structure, the complex [Mn(H(2)O)(6)](2+) cations and the [CuL](-) anions are arranged in columns parallel to the a axis and are held together by O-H⋯O hydrogen bonding. Additional hydrogen bonds of the same type further link the columns into a three-dimensional network.

Entities:  

Year:  2010        PMID： 21579016      PMCID： PMC2979099          DOI： 10.1107/S1600536810013061

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


Related literature

Transition metal complexes of salicylaldehyde–peptide- and salicylaldehyde–amino-acid-derived Schiff bases are suitable non-enzymatic models for pyridoxal amino acid systems, which are of considerable importance as key inter­mediates in metabolic reactions, see: Bkouche-Waksman et al. (1988 ▶); Wetmore et al. (2001 ▶); Zabinski & Toney (2001 ▶). For the preparation, structural characterization, spectroscopic and magnetic studies of Schiff base complexes derived from salicylaldehyde and amino acids, see: Ganguly et al. (2008 ▶) and references cited therein. For Schiff bases derived from simple peptides, see: Zou et al. (2003 ▶).

Experimental

Crystal data

[Mn(H2O)6][Cu(C12H11N2O5)]2·6H2O M = 924.67 Triclinic, a = 6.712 (1) Å b = 11.762 (2) Å c = 12.092 (2) Å α = 76.51 (1)° β = 83.90 (1)° γ = 80.37 (1)° V = 912.9 (3) Å3 Z = 1 Mo Kα radiation μ = 1.59 mm−1 T = 293 K 0.3 × 0.2 × 0.2 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2003 ▶) T min = 0.690, T max = 0.728 4571 measured reflections 3156 independent reflections 1625 reflections with I > 2σ(I) R int = 0.114

Refinement

R[F 2 > 2σ(F 2)] = 0.057 wR(F 2) = 0.129 S = 0.79 3156 reflections 246 parameters 114 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.74 e Å−3 Δρmin = −0.56 e Å−3 Data collection: SMART (Bruker, 2003 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810013061/wm2319sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810013061/wm2319Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mn(H2O)6][Cu(C12H11N2O5)]2·6H2OZ = 1
Mr = 924.67F(000) = 477
Triclinic, P1Dx = 1.682 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.712 (1) ÅCell parameters from 1625 reflections
b = 11.762 (2) Åθ = 1.7–25.0°
c = 12.092 (2) ŵ = 1.59 mm−1
α = 76.51 (1)°T = 293 K
β = 83.90 (1)°Block, violet-red
γ = 80.37 (1)°0.3 × 0.2 × 0.2 mm
V = 912.9 (3) Å3
Bruker SMART CCD diffractometer3156 independent reflections
Radiation source: fine-focus sealed tube1625 reflections with I > 2σ(I)
graphiteRint = 0.114
φ and ω scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2003)h = −7→7
Tmin = 0.690, Tmax = 0.728k = −12→13
4571 measured reflectionsl = −14→13
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 0.79w = 1/[σ2(Fo2) + (0.0082P)2] where P = (Fo2 + 2Fc2)/3
3156 reflections(Δ/σ)max < 0.001
246 parametersΔρmax = 0.74 e Å−3
114 restraintsΔρmin = −0.56 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Cu10.77185 (12)0.49742 (7)0.37778 (7)0.0309 (3)
C10.7114 (9)0.5700 (6)0.5897 (5)0.0359 (10)
C20.6755 (9)0.6598 (7)0.6508 (6)0.0396 (11)
C30.6653 (9)0.6330 (7)0.7685 (6)0.0407 (12)
H30.64210.69420.80710.049*
C40.6886 (9)0.5174 (6)0.8304 (6)0.0441 (13)
H40.67990.50070.90970.053*
C50.7244 (9)0.4286 (7)0.7730 (6)0.0430 (13)
H50.74060.35070.81430.052*
C60.7379 (9)0.4509 (6)0.6520 (5)0.0365 (11)
C70.7766 (9)0.3506 (6)0.6003 (5)0.0366 (12)
H70.78910.27610.64870.044*
C80.8340 (9)0.2463 (5)0.4483 (5)0.0332 (12)
H8A0.72530.19970.47580.040*
H8B0.95990.19920.47460.040*
C90.8469 (9)0.2797 (6)0.3194 (5)0.0311 (11)
C100.8264 (9)0.4476 (5)0.1580 (5)0.0283 (11)
H10A0.72420.42230.12210.034*
H10B0.95790.42450.12140.034*
C110.7866 (9)0.5805 (6)0.1443 (5)0.0296 (11)
C120.6232 (10)0.8684 (6)0.6400 (6)0.0542 (19)
H12A0.49730.86900.68570.081*
H12B0.62060.94120.58370.081*
H12C0.73250.86020.68780.081*
N10.7953 (7)0.3554 (5)0.4929 (4)0.0317 (10)
N20.8214 (7)0.3923 (4)0.2782 (4)0.0285 (10)
O10.6519 (6)0.7718 (4)0.5847 (4)0.0457 (11)
O20.7206 (6)0.6012 (4)0.4771 (4)0.0378 (10)
O30.8774 (6)0.1989 (4)0.2649 (4)0.0394 (12)
O40.7585 (6)0.6211 (3)0.2352 (3)0.0315 (10)
O50.7834 (6)0.6436 (4)0.0469 (4)0.0384 (11)
Mn10.50000.00000.00000.0327 (4)
O60.1953 (6)0.0535 (4)−0.0541 (4)0.0428 (13)
H6C0.15230.05030.01510.051*
H6B0.14850.1267−0.07060.051*
O70.5193 (6)0.1775 (4)0.0174 (4)0.0477 (13)
H7B0.40220.21080.03580.057*
H7C0.59450.16060.07300.057*
O80.3774 (6)−0.0518 (4)0.1787 (4)0.0572 (15)
H8D0.4634−0.04460.22240.069*
H8E0.2674−0.00660.18890.069*
O90.9213 (6)0.2144 (4)0.0353 (4)0.0465 (13)
H9D0.90920.20920.10700.056*
H9B0.82590.26170.00080.056*
O100.6740 (7)0.8222 (4)0.3246 (4)0.0500 (14)
H10F0.69940.76070.29710.060*
O11A0.0288 (7)0.0311 (4)0.7410 (4)0.0554 (15)
H11B0.11590.07000.75440.066*
H11C0.0589−0.03540.74540.066*
H10E0.662 (10)0.759 (6)0.387 (6)0.06 (2)*
U11U22U33U12U13U23
Cu10.0346 (5)0.0328 (5)0.0247 (5)−0.0031 (4)−0.0013 (4)−0.0065 (4)
C10.0277 (19)0.054 (2)0.029 (2)−0.0056 (18)−0.0004 (18)−0.0161 (19)
C20.029 (2)0.057 (2)0.036 (2)−0.005 (2)−0.0012 (19)−0.020 (2)
C30.029 (2)0.063 (3)0.034 (2)−0.005 (2)−0.001 (2)−0.022 (2)
C40.031 (2)0.069 (3)0.034 (2)−0.007 (2)0.000 (2)−0.017 (2)
C50.031 (2)0.066 (3)0.032 (2)−0.007 (2)0.001 (2)−0.011 (2)
C60.028 (2)0.055 (2)0.028 (2)−0.0085 (19)−0.0002 (18)−0.0124 (19)
C70.030 (2)0.050 (2)0.030 (2)−0.009 (2)0.000 (2)−0.006 (2)
C80.029 (2)0.039 (2)0.031 (2)−0.006 (2)−0.002 (2)−0.005 (2)
C90.027 (2)0.035 (2)0.031 (2)−0.006 (2)−0.0011 (19)−0.004 (2)
C100.024 (2)0.032 (2)0.027 (2)−0.003 (2)0.000 (2)−0.005 (2)
C110.025 (2)0.032 (2)0.029 (2)−0.002 (2)0.0010 (19)−0.0042 (19)
C120.053 (4)0.061 (4)0.058 (4)−0.006 (3)−0.004 (3)−0.033 (4)
N10.028 (2)0.041 (2)0.027 (2)−0.0088 (19)−0.0008 (19)−0.009 (2)
N20.024 (2)0.031 (2)0.029 (2)−0.0047 (19)−0.0009 (18)−0.0025 (19)
O10.041 (2)0.058 (3)0.044 (2)−0.005 (2)−0.0023 (19)−0.024 (2)
O20.035 (2)0.050 (2)0.030 (2)−0.0042 (19)−0.0017 (19)−0.013 (2)
O30.046 (3)0.035 (3)0.036 (3)−0.001 (2)−0.001 (2)−0.010 (2)
O40.034 (2)0.030 (2)0.029 (2)−0.0028 (18)0.0010 (18)−0.0058 (18)
O50.039 (3)0.039 (3)0.031 (2)0.000 (2)0.000 (2)−0.001 (2)
Mn10.0291 (9)0.0317 (9)0.0351 (9)−0.0001 (7)−0.0035 (7)−0.0055 (7)
O60.029 (3)0.052 (3)0.047 (3)0.005 (2)−0.007 (2)−0.016 (3)
O70.042 (3)0.038 (3)0.061 (3)0.007 (2)−0.016 (2)−0.011 (3)
O80.036 (3)0.084 (4)0.041 (3)0.004 (3)−0.001 (2)−0.001 (3)
O90.051 (3)0.048 (3)0.039 (3)0.006 (2)−0.011 (2)−0.013 (3)
O100.064 (4)0.034 (3)0.052 (4)−0.011 (3)−0.006 (3)−0.008 (3)
O11A0.050 (3)0.043 (3)0.074 (4)−0.010 (2)0.003 (3)−0.016 (3)
Cu1—O21.873 (4)C10—H10A0.9700
Cu1—N21.887 (5)C10—H10B0.9700
Cu1—N11.905 (5)C11—O51.237 (7)
Cu1—O41.979 (4)C11—O41.282 (7)
C1—O21.323 (7)C12—O11.424 (7)
C1—C21.400 (8)C12—H12A0.9600
C1—C61.418 (9)C12—H12B0.9600
C2—O11.366 (8)C12—H12C0.9600
C2—C31.382 (9)Mn1—O6i2.161 (4)
C3—C41.383 (9)Mn1—O62.161 (4)
C3—H30.9300Mn1—O7i2.173 (4)
C4—C51.360 (8)Mn1—O72.173 (4)
C4—H40.9300Mn1—O8i2.212 (4)
C5—C61.421 (9)Mn1—O82.212 (4)
C5—H50.9300O6—H6C0.8500
C6—C71.434 (8)O6—H6B0.8500
C7—N11.280 (7)O7—H7B0.8500
C7—H70.9300O7—H7C0.8499
C8—N11.479 (7)O8—H8D0.8499
C8—C91.513 (8)O8—H8E0.8499
C8—H8A0.9700O9—H9D0.8500
C8—H8B0.9700O9—H9B0.8500
C9—O31.256 (7)O10—H10F0.8500
C9—N21.290 (7)O10—H10E0.93 (7)
C10—N21.447 (7)O11A—H11B0.8495
C10—C111.513 (8)O11A—H11C0.7651
O2—Cu1—N2179.5 (2)O4—C11—C10117.6 (6)
O2—Cu1—N196.4 (2)O1—C12—H12A109.5
N2—Cu1—N183.4 (2)O1—C12—H12B109.5
O2—Cu1—O496.16 (18)H12A—C12—H12B109.5
N2—Cu1—O484.08 (19)O1—C12—H12C109.5
N1—Cu1—O4167.49 (18)H12A—C12—H12C109.5
O2—C1—C2118.0 (6)H12B—C12—H12C109.5
O2—C1—C6123.8 (6)C7—N1—C8121.0 (6)
C2—C1—C6118.2 (6)C7—N1—Cu1124.9 (5)
O1—C2—C3124.6 (6)C8—N1—Cu1114.1 (4)
O1—C2—C1114.6 (6)C9—N2—C10124.9 (5)
C3—C2—C1120.7 (7)C9—N2—Cu1119.8 (5)
C2—C3—C4121.7 (7)C10—N2—Cu1115.3 (4)
C2—C3—H3119.2C2—O1—C12118.2 (5)
C4—C3—H3119.2C1—O2—Cu1125.7 (4)
C5—C4—C3118.6 (7)C11—O4—Cu1114.0 (4)
C5—C4—H4120.7O6i—Mn1—O6180.0 (4)
C3—C4—H4120.7O6i—Mn1—O7i91.61 (16)
C4—C5—C6122.1 (7)O6—Mn1—O7i88.39 (16)
C4—C5—H5118.9O6i—Mn1—O788.39 (16)
C6—C5—H5118.9O6—Mn1—O791.61 (16)
C1—C6—C5118.6 (6)O7i—Mn1—O7180.0 (2)
C1—C6—C7124.0 (6)O6i—Mn1—O8i89.94 (16)
C5—C6—C7117.4 (6)O6—Mn1—O8i90.06 (16)
N1—C7—C6125.3 (7)O7i—Mn1—O8i92.27 (17)
N1—C7—H7117.4O7—Mn1—O8i87.73 (17)
C6—C7—H7117.4O6i—Mn1—O890.06 (16)
N1—C8—C9109.0 (5)O6—Mn1—O889.94 (16)
N1—C8—H8A109.9O7i—Mn1—O887.73 (17)
C9—C8—H8A109.9O7—Mn1—O892.27 (17)
N1—C8—H8B109.9O8i—Mn1—O8180.0 (4)
C9—C8—H8B109.9Mn1—O6—H6C89.0
H8A—C8—H8B108.3Mn1—O6—H6B119.0
O3—C9—N2127.5 (6)H6C—O6—H6B90.0
O3—C9—C8118.8 (5)Mn1—O7—H7B109.3
N2—C9—C8113.7 (6)Mn1—O7—H7C99.5
N2—C10—C11109.1 (5)H7B—O7—H7C110.9
N2—C10—H10A109.9Mn1—O8—H8D108.6
C11—C10—H10A109.9Mn1—O8—H8E109.3
N2—C10—H10B109.9H8D—O8—H8E109.5
C11—C10—H10B109.9H9D—O9—H9B112.9
H10A—C10—H10B108.3H10F—O10—H10E74.7
O5—C11—O4123.7 (6)H11B—O11A—H11C118.5
O5—C11—C10118.7 (5)
D—H···AD—HH···AD···AD—H···A
O11A—H11C···O3ii0.771.932.689 (6)172
O11A—H11B···O10iii0.852.062.786 (7)143
O10—H10F···O40.851.932.775 (6)180
O10—H10E···O20.93 (7)1.92 (7)2.805 (7)157 (6)
O9—H9D···O30.851.882.727 (6)179
O9—H9B···O70.852.402.842 (6)113
O8—H8E···O11Aiv0.852.122.786 (6)135
O8—H8D···O10v0.852.172.795 (7)130
O7—H7C···O90.852.352.842 (6)117
O7—H7B···O5vi0.852.062.702 (6)132
O6—H6B···O9vii0.852.172.739 (5)124
Table 1

Selected bond lengths (Å)

Cu1—O21.873 (4)
Cu1—N21.887 (5)
Cu1—N11.905 (5)
Cu1—O41.979 (4)
Mn1—O62.161 (4)
Mn1—O72.173 (4)
Mn1—O82.212 (4)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O11A—H11C⋯O3i0.771.932.689 (6)172
O11A—H11B⋯O10ii0.852.062.786 (7)143
O10—H10F⋯O40.851.932.775 (6)180
O10—H10E⋯O20.93 (7)1.92 (7)2.805 (7)157 (6)
O9—H9D⋯O30.851.882.727 (6)179
O9—H9B⋯O70.852.402.842 (6)113
O8—H8E⋯O11Aiii0.852.122.786 (6)135
O8—H8D⋯O10iv0.852.172.795 (7)130
O7—H7C⋯O90.852.352.842 (6)117
O7—H7B⋯O5v0.852.062.702 (6)132
O6—H6B⋯O9vi0.852.172.739 (5)124

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

  5 in total

1.  Enzyme catalysis of 1,2-amino shifts: the cooperative action of B6, B12, and aminomutases.

Authors:  S D Wetmore; D M Smith; L Radom
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2.  A short history of SHELX.

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

3.  Metal ion inhibition of nonenzymatic pyridoxal phosphate catalyzed decarboxylation and transamination.

Authors:  R F Zabinski; M D Toney
Journal:  J Am Chem Soc       Date:  2001-01-17       Impact factor: 15.419

4.  A novel molecular ladder structure of Cu(II)-Ba(II) coordination polymer exhibiting ferromagnetic coupling.

Authors:  Yang Zou; Wenlong Liu; Song Gao; Jingli Xie; Qingjin Meng
Journal:  Chem Commun (Camb)       Date:  2003-12-07       Impact factor: 6.222

5.  A model for vitamin B6--amino-acid-related metal complexes. Neutron diffraction study of aqua(N-salicylideneglycinato)copper(II) hemihydrate at 130 K.

Authors:  I Bkouche-Waksman; J M Barbe; A Kvick
Journal:  Acta Crystallogr B       Date:  1988-12-01
  5 in total

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