Literature DB >> 24454049

Bis(μ-hydroxido-κ(2) O:O)bis[bis(5-car-boxy-pyridine-2-carboxyl-ato-κ(2) N,O (2))iron(III)] dihydrate.

Wenhai Cao1.   

Abstract

The complete binuclear complex in [Fe2(C7H4NO4)4(OH)2]·2H2O, is generated by the application twofold symmetry. The Fe(III) atom is coordinated by the O atoms of two bridging hydroxyl groups and by two N and two O atoms from two pyridine-2,5-di-carboxyl-ato ligands, forming a distorted octa-hedral geometry. The Fe⋯Fe separation within the dinuclear complex is 3.0657 (4) Å. In the crystal, O-H⋯O and C-H⋯O hydrogen-bonding inter-actions connect the mol-ecules into a three-dimensional supra-molecular network.

Entities:  

Year:  2013        PMID： 24454049      PMCID： PMC3884273          DOI： 10.1107/S1600536813029449

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


Related literature

For background to the coordination modes of the pyridine-2,5-di­carboxyl­ate ligand, see: Zhang et al. (2005 ▶, 2006 ▶); Liang et al. (2000 ▶); Wibowo et al. (2011 ▶). For iron complexes of the pyridine-2,5-di­carboxyl­ate ligand, see: Shi et al. (2011 ▶); Xu et al. (2004 ▶); Gao et al. (2005 ▶).

Experimental

Crystal data

[Fe2(C7H4NO4)4(OH)2]·2H2O M = 846.20 Monoclinic, a = 7.6130 (7) Å b = 14.2716 (14) Å c = 16.2594 (13) Å β = 114.556 (4)° V = 1606.8 (3) Å3 Z = 2 Mo Kα radiation μ = 1.00 mm−1 T = 298 K 0.28 × 0.25 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.767, T max = 0.825 11029 measured reflections 3972 independent reflections 3224 reflections with I > 2σ(I) R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.035 wR(F 2) = 0.096 S = 1.01 3972 reflections 244 parameters H-atom parameters constrained Δρmax = 0.37 e Å−3 Δρmin = −0.47 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; 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 datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S1600536813029449/rz5089sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813029449/rz5089Isup2.hkl 968712 Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Fe2(C7H4NO4)4(OH)2]·2H2OF(000) = 860
Mr = 846.20Dx = 1.749 Mg m−3
Monoclinic, P2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ycCell parameters from 3376 reflections
a = 7.6130 (7) Åθ = 2.8–27.8°
b = 14.2716 (14) ŵ = 1.00 mm−1
c = 16.2594 (13) ÅT = 298 K
β = 114.556 (4)°Rod, green
V = 1606.8 (3) Å30.28 × 0.25 × 0.20 mm
Z = 2
Bruker APEXII CCD diffractometer3972 independent reflections
Radiation source: fine-focus sealed tube3224 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 28.3°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −10→9
Tmin = 0.767, Tmax = 0.825k = −19→15
11029 measured reflectionsl = −21→21
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0446P)2 + 0.9967P] where P = (Fo2 + 2Fc2)/3
3972 reflections(Δ/σ)max < 0.001
244 parametersΔρmax = 0.37 e Å−3
0 restraintsΔρmin = −0.47 e Å−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
Fe10.80977 (4)0.202541 (19)0.164770 (19)0.02479 (10)
O10.7658 (2)0.21500 (10)0.03507 (10)0.0320 (3)
C10.7583 (3)0.37700 (14)0.06158 (13)0.0276 (4)
O20.7390 (3)0.30988 (11)−0.07630 (11)0.0422 (4)
C20.7485 (3)0.46928 (15)0.03644 (15)0.0364 (5)
H20.74590.4859−0.01940.044*
N30.7556 (2)0.05572 (11)0.14087 (12)0.0270 (4)
C30.7427 (4)0.53720 (16)0.09617 (16)0.0384 (5)
H30.73560.60030.08080.046*
O30.7248 (4)0.66606 (13)0.22363 (14)0.0732 (7)
O40.7493 (4)0.55104 (13)0.31845 (12)0.0619 (6)
H40.74320.59810.34920.093*
C40.7476 (3)0.51062 (14)0.17838 (14)0.0311 (4)
O50.5359 (2)0.19337 (10)0.14846 (11)0.0346 (3)
N50.7678 (2)0.35085 (12)0.14291 (11)0.0264 (3)
C50.7609 (3)0.41600 (14)0.20041 (14)0.0302 (4)
H50.76510.39780.25610.036*
O60.2935 (2)0.09752 (13)0.13321 (15)0.0517 (5)
C60.7553 (3)0.29598 (14)0.00125 (14)0.0281 (4)
O70.8655 (3)−0.25246 (13)0.07024 (15)0.0579 (5)
C70.7401 (4)0.58513 (16)0.24209 (16)0.0378 (5)
O81.1183 (3)−0.15856 (12)0.13517 (14)0.0515 (5)
H81.1783−0.20460.13090.077*
C80.5788 (3)0.03170 (15)0.13346 (15)0.0308 (4)
O90.9102 (2)0.20283 (10)0.29588 (10)0.0295 (3)
H9A0.84740.18070.32460.044*
C90.5143 (4)−0.05918 (16)0.12100 (19)0.0442 (6)
H90.3921−0.07380.11720.053*
C100.6332 (3)−0.12806 (16)0.11428 (18)0.0435 (6)
H100.5931−0.19030.10650.052*
O100.2618 (4)0.34823 (19)0.09961 (18)0.0971 (9)
H10A0.26830.29040.11760.146*
H10B0.19970.32790.04400.146*
C110.8133 (3)−0.10417 (15)0.11911 (15)0.0322 (4)
C120.8722 (3)−0.01115 (14)0.13374 (14)0.0288 (4)
H120.99450.00500.13870.035*
C130.4555 (3)0.11238 (16)0.13878 (15)0.0333 (5)
C140.9348 (4)−0.17947 (15)0.10565 (17)0.0376 (5)
U11U22U33U12U13U23
Fe10.03269 (17)0.01681 (15)0.02696 (16)0.00018 (11)0.01447 (12)0.00000 (11)
O10.0489 (9)0.0203 (7)0.0281 (7)−0.0003 (6)0.0173 (7)−0.0018 (6)
C10.0343 (10)0.0215 (9)0.0284 (10)0.0000 (8)0.0144 (8)−0.0006 (8)
O20.0745 (12)0.0278 (8)0.0328 (8)0.0048 (7)0.0309 (8)0.0031 (6)
C20.0549 (14)0.0255 (11)0.0331 (11)0.0019 (9)0.0224 (10)0.0029 (9)
N30.0325 (9)0.0200 (8)0.0313 (8)−0.0020 (7)0.0162 (7)−0.0021 (7)
C30.0579 (14)0.0200 (10)0.0414 (12)0.0024 (9)0.0247 (11)0.0012 (9)
O30.150 (2)0.0244 (9)0.0644 (13)0.0098 (11)0.0631 (15)−0.0020 (9)
O40.1225 (18)0.0296 (10)0.0442 (10)0.0052 (10)0.0452 (12)−0.0055 (8)
C40.0381 (11)0.0210 (10)0.0339 (11)0.0019 (8)0.0146 (9)−0.0026 (8)
O50.0332 (8)0.0254 (8)0.0474 (9)0.0016 (6)0.0189 (7)−0.0015 (6)
N50.0342 (9)0.0195 (8)0.0274 (8)0.0024 (7)0.0149 (7)0.0011 (6)
C50.0399 (11)0.0241 (10)0.0285 (10)0.0023 (8)0.0163 (9)−0.0009 (8)
O60.0397 (9)0.0413 (10)0.0850 (14)−0.0057 (8)0.0370 (9)−0.0127 (10)
C60.0339 (10)0.0232 (10)0.0295 (10)0.0004 (8)0.0156 (8)−0.0005 (8)
O70.0709 (13)0.0267 (9)0.0846 (14)−0.0100 (8)0.0409 (11)−0.0218 (9)
C70.0531 (14)0.0255 (11)0.0384 (12)0.0043 (9)0.0226 (11)−0.0029 (9)
O80.0502 (10)0.0285 (9)0.0842 (14)0.0002 (8)0.0364 (10)−0.0146 (9)
C80.0354 (11)0.0247 (10)0.0371 (11)−0.0025 (8)0.0197 (9)−0.0021 (9)
O90.0327 (7)0.0322 (8)0.0277 (7)−0.0008 (6)0.0168 (6)0.0009 (6)
C90.0399 (13)0.0293 (12)0.0702 (17)−0.0096 (10)0.0295 (12)−0.0064 (11)
C100.0444 (13)0.0235 (11)0.0650 (16)−0.0095 (9)0.0250 (12)−0.0078 (11)
O100.141 (3)0.0694 (18)0.0912 (19)0.0195 (17)0.0580 (18)−0.0053 (15)
C110.0399 (11)0.0216 (10)0.0360 (11)−0.0012 (8)0.0167 (9)−0.0026 (9)
C120.0337 (10)0.0214 (10)0.0342 (10)0.0000 (8)0.0170 (9)−0.0007 (8)
C130.0341 (11)0.0315 (11)0.0383 (11)0.0001 (9)0.0190 (9)−0.0029 (9)
C140.0506 (14)0.0219 (10)0.0468 (13)−0.0033 (9)0.0268 (11)−0.0038 (9)
Fe1—O91.9427 (15)C4—C71.502 (3)
Fe1—O9i1.9543 (15)O5—C131.287 (3)
Fe1—O51.9937 (15)N5—C51.335 (3)
Fe1—O12.0011 (15)C5—H50.9300
Fe1—N32.1397 (17)O6—C131.217 (3)
Fe1—N52.1480 (17)O7—C141.201 (3)
O1—C61.268 (2)O8—C141.309 (3)
C1—N51.347 (3)O8—H80.8200
C1—C21.372 (3)C8—C91.372 (3)
C1—C61.510 (3)C8—C131.511 (3)
O2—C61.231 (2)O9—Fe1i1.9543 (15)
C2—C31.386 (3)O9—H9A0.8554
C2—H20.9300C9—C101.371 (3)
N3—C121.340 (3)C9—H90.9300
N3—C81.345 (3)C10—C111.383 (3)
C3—C41.375 (3)C10—H100.9300
C3—H30.9300O10—H10A0.8695
O3—C71.187 (3)O10—H10B0.8773
O4—C71.308 (3)C11—C121.390 (3)
O4—H40.8500C11—C141.492 (3)
C4—C51.390 (3)C12—H120.9300
O9—Fe1—O9i76.25 (7)N5—C5—C4121.07 (19)
O9—Fe1—O593.39 (6)N5—C5—H5119.5
O9i—Fe1—O5169.02 (6)C4—C5—H5119.5
O9—Fe1—O1166.74 (6)O2—C6—O1123.53 (19)
O9i—Fe1—O191.53 (6)O2—C6—C1120.67 (18)
O5—Fe1—O199.10 (7)O1—C6—C1115.78 (18)
O9—Fe1—N399.19 (6)O3—C7—O4124.3 (2)
O9i—Fe1—N399.39 (6)O3—C7—C4122.8 (2)
O5—Fe1—N378.44 (6)O4—C7—C4112.89 (19)
O1—Fe1—N387.73 (6)C14—O8—H8109.5
O9—Fe1—N598.23 (6)N3—C8—C9122.5 (2)
O9i—Fe1—N596.84 (6)N3—C8—C13115.04 (18)
O5—Fe1—N588.13 (6)C9—C8—C13122.4 (2)
O1—Fe1—N577.87 (6)Fe1—O9—Fe1i103.75 (7)
N3—Fe1—N5158.55 (7)Fe1—O9—H9A122.9
C6—O1—Fe1119.39 (13)Fe1i—O9—H9A127.0
N5—C1—C2122.20 (19)C10—C9—C8118.8 (2)
N5—C1—C6113.94 (17)C10—C9—H9120.6
C2—C1—C6123.85 (19)C8—C9—H9120.6
C1—C2—C3118.4 (2)C9—C10—C11119.4 (2)
C1—C2—H2120.8C9—C10—H10120.3
C3—C2—H2120.8C11—C10—H10120.3
C12—N3—C8118.98 (17)H10A—O10—H10B87.9
C12—N3—Fe1128.94 (14)C10—C11—C12119.1 (2)
C8—N3—Fe1112.08 (13)C10—C11—C14118.3 (2)
C4—C3—C2119.5 (2)C12—C11—C14122.5 (2)
C4—C3—H3120.3N3—C12—C11121.13 (19)
C2—C3—H3120.3N3—C12—H12119.4
C7—O4—H4105.7C11—C12—H12119.4
C3—C4—C5119.2 (2)O6—C13—O5125.6 (2)
C3—C4—C7118.80 (19)O6—C13—C8119.8 (2)
C5—C4—C7122.0 (2)O5—C13—C8114.59 (18)
C13—O5—Fe1119.57 (13)O7—C14—O8124.2 (2)
C5—N5—C1119.53 (17)O7—C14—C11121.3 (2)
C5—N5—Fe1128.09 (14)O8—C14—C11114.47 (19)
C1—N5—Fe1112.28 (13)
O9—Fe1—O1—C6−66.9 (3)C3—C4—C5—N5−0.4 (3)
O9i—Fe1—O1—C6−89.41 (16)C7—C4—C5—N5−179.9 (2)
O5—Fe1—O1—C693.34 (16)Fe1—O1—C6—O2175.93 (17)
N3—Fe1—O1—C6171.25 (16)Fe1—O1—C6—C1−5.7 (2)
N5—Fe1—O1—C67.26 (16)N5—C1—C6—O2177.1 (2)
N5—C1—C2—C3−1.9 (3)C2—C1—C6—O2−1.7 (3)
C6—C1—C2—C3176.8 (2)N5—C1—C6—O1−1.3 (3)
O9—Fe1—N3—C12−91.72 (18)C2—C1—C6—O1179.9 (2)
O9i—Fe1—N3—C12−14.28 (18)C3—C4—C7—O32.1 (4)
O5—Fe1—N3—C12176.66 (19)C5—C4—C7—O3−178.5 (3)
O1—Fe1—N3—C1276.90 (18)C3—C4—C7—O4−178.8 (2)
N5—Fe1—N3—C12124.4 (2)C5—C4—C7—O40.7 (3)
O9—Fe1—N3—C887.60 (15)C12—N3—C8—C91.6 (3)
O9i—Fe1—N3—C8165.05 (14)Fe1—N3—C8—C9−177.8 (2)
O5—Fe1—N3—C8−4.01 (14)C12—N3—C8—C13−177.72 (18)
O1—Fe1—N3—C8−103.78 (15)Fe1—N3—C8—C132.9 (2)
N5—Fe1—N3—C8−56.3 (2)O9i—Fe1—O9—Fe1i−0.25 (9)
C1—C2—C3—C40.2 (4)O5—Fe1—O9—Fe1i176.08 (6)
C2—C3—C4—C50.9 (4)O1—Fe1—O9—Fe1i−23.5 (3)
C2—C3—C4—C7−179.6 (2)N3—Fe1—O9—Fe1i97.25 (7)
O9—Fe1—O5—C13−93.78 (17)N5—Fe1—O9—Fe1i−95.32 (7)
O9i—Fe1—O5—C13−74.7 (4)N3—C8—C9—C10−1.1 (4)
O1—Fe1—O5—C1390.68 (17)C13—C8—C9—C10178.1 (2)
N3—Fe1—O5—C134.91 (16)C8—C9—C10—C11−0.8 (4)
N5—Fe1—O5—C13168.08 (17)C9—C10—C11—C122.2 (4)
C2—C1—N5—C52.4 (3)C9—C10—C11—C14−176.1 (2)
C6—C1—N5—C5−176.44 (18)C8—N3—C12—C11−0.1 (3)
C2—C1—N5—Fe1−174.31 (18)Fe1—N3—C12—C11179.16 (15)
C6—C1—N5—Fe16.9 (2)C10—C11—C12—N3−1.7 (3)
O9—Fe1—N5—C5−16.69 (18)C14—C11—C12—N3176.5 (2)
O9i—Fe1—N5—C5−93.71 (18)Fe1—O5—C13—O6175.8 (2)
O5—Fe1—N5—C576.46 (18)Fe1—O5—C13—C8−4.7 (3)
O1—Fe1—N5—C5176.19 (19)N3—C8—C13—O6−179.6 (2)
N3—Fe1—N5—C5127.3 (2)C9—C8—C13—O61.1 (4)
O9—Fe1—N5—C1159.65 (14)N3—C8—C13—O50.9 (3)
O9i—Fe1—N5—C182.63 (14)C9—C8—C13—O5−178.4 (2)
O5—Fe1—N5—C1−107.19 (14)C10—C11—C14—O718.1 (4)
O1—Fe1—N5—C1−7.47 (14)C12—C11—C14—O7−160.1 (2)
N3—Fe1—N5—C1−56.3 (2)C10—C11—C14—O8−162.0 (2)
C1—N5—C5—C4−1.2 (3)C12—C11—C14—O819.8 (3)
Fe1—N5—C5—C4174.93 (15)
D—H···AD—HH···AD···AD—H···A
O8—H8···O2ii0.821.982.761 (2)160
O4—H4···O2iii0.851.802.643 (2)175
O9—H9A···O6iv0.861.912.735 (2)162
O10—H10A···O50.872.342.914 (3)124
O10—H10B···O7v0.882.022.865 (3)161
C3—H3···O7vi0.932.363.223 (3)155
C5—H5···O10iv0.932.543.465 (3)174
C9—H9···O8vii0.932.533.425 (3)162
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O8—H8⋯O2i 0.821.982.761 (2)160
O4—H4⋯O2ii 0.851.802.643 (2)175
O9—H9A⋯O6iii 0.861.912.735 (2)162
O10—H10A⋯O50.872.342.914 (3)124
O10—H10B⋯O7iv 0.882.022.865 (3)161
C3—H3⋯O7v 0.932.363.223 (3)155
C5—H5⋯O10iii 0.932.543.465 (3)174
C9—H9⋯O8vi 0.932.533.425 (3)162

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

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Authors: 
Journal:  Angew Chem Int Ed Engl       Date:  2000-09-15       Impact factor: 15.336

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