Literature DB >> 21202796

Poly[[diaqua-tris[μ(4)-(p-phenyl-enedi-oxy)diacetato]didysprosium(III)] dihydrate].

Ya-Feng Li1, Dao-Wu Wang, Yuan-Rui Wang, Long Zhang.   

Abstract

The title dysprosium coordination polymer, {[Dy(2)(C(10)H(8)O(6))(3)(H(2)O)(2)]·2H(2)O}(n), was synthesized by reacting dysprosium(III) nitrate and the flexible ligand (p-phenyl-enedi-oxy)diacetic acid under hydro-thermal conditions. Each Dy(III) ion is coordinated by nine O atoms in a tricapped trigonal prismatic geometry. The DyO(9) polyhedra form layers parallel to the bc plane. The rigid benzene rings of the anions link the layers along the a axis, forming a three-dimensional framework.

Entities:  

Year:  2008        PMID： 21202796      PMCID： PMC2961875          DOI： 10.1107/S1600536808017649

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


Related literature

For related literature, see: Eddaoudi et al. (2001 ▶); Li & Han (2006 ▶); Michl (1995 ▶); Yaghi et al. (1998 ▶).

Experimental

Crystal data

[Dy2(C10H8O6)3(H2O)2]·2H2O M = 1069.56 Monoclinic, a = 12.080 (2) Å b = 16.615 (3) Å c = 8.8802 (18) Å β = 109.32 (3)° V = 1682.0 (6) Å3 Z = 2 Mo Kα radiation μ = 4.50 mm−1 T = 293 (2) K 0.19 × 0.16 × 0.13 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.437, T max = 0.548 16183 measured reflections 3838 independent reflections 3229 reflections with I > 2σ(I) R int = 0.043

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.059 S = 1.05 3838 reflections 256 parameters 6 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.83 e Å−3 Δρmin = −0.93 e Å−3 Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808017649/ci2601sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808017649/ci2601Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Dy2(C10H8O6)3(H2O)2]·2H2OF000 = 1040
Mr = 1069.56Dx = 2.112 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2000 reflections
a = 12.080 (2) Åθ = 3.0–27.5º
b = 16.615 (3) ŵ = 4.50 mm−1
c = 8.8802 (18) ÅT = 293 (2) K
β = 109.32 (3)ºBlock, grey yellow
V = 1682.0 (6) Å30.19 × 0.16 × 0.13 mm
Z = 2
Rigaku R-AXIS RAPID diffractometer3838 independent reflections
Radiation source: fine-focus sealed tube3229 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.043
Detector resolution: 10.00 pixels mm-1θmax = 27.5º
T = 293(2) Kθmin = 3.0º
ω scansh = −15→15
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)k = −21→21
Tmin = 0.437, Tmax = 0.548l = −11→11
16183 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.059  w = 1/[σ2(Fo2) + (0.0147P)2 + 5.1969P] where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.009
3838 reflectionsΔρmax = 0.83 e Å−3
256 parametersΔρmin = −0.93 e Å−3
6 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
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
Dy10.047406 (15)0.117791 (10)0.06685 (2)0.01642 (6)
O1−0.1292 (2)0.11347 (17)−0.1593 (3)0.0272 (7)
O1W−0.0933 (3)0.2099 (2)0.1170 (4)0.0492 (11)
H16A−0.051 (5)0.246 (3)0.161 (7)0.074*
H16B−0.145 (4)0.228 (3)0.046 (6)0.074*
O2−0.1802 (2)−0.01721 (17)−0.1976 (3)0.0255 (6)
O3−0.3483 (2)0.15102 (17)−0.3735 (3)0.0252 (6)
O4−0.7742 (2)0.21741 (16)−0.8419 (3)0.0214 (6)
O5−0.8998 (3)0.35594 (17)−1.1500 (3)0.0244 (6)
O6−0.9551 (3)0.23500 (18)−1.0955 (4)0.0335 (8)
O70.1721 (3)0.09109 (18)−0.0991 (4)0.0312 (7)
O80.0580 (3)−0.0133 (2)−0.1313 (4)0.0362 (8)
O90.3019 (3)0.0217 (2)−0.2669 (4)0.0417 (9)
C1−0.1940 (3)0.0565 (2)−0.2298 (5)0.0199 (8)
C2−0.3012 (3)0.0727 (2)−0.3743 (5)0.0245 (9)
H2A−0.28030.0664−0.47010.029*
H2B−0.36110.0331−0.37780.029*
C3−0.4522 (3)0.1666 (2)−0.4950 (5)0.0193 (8)
C4−0.5023 (3)0.1140 (2)−0.6214 (4)0.0211 (8)
H4−0.46500.0660−0.62860.025*
C5−0.5082 (4)0.2383 (3)−0.4866 (5)0.0254 (9)
H5−0.47420.2739−0.40330.030*
C6−0.6087 (3)0.1338 (2)−0.7369 (5)0.0216 (8)
H6−0.64180.0991−0.82220.026*
C7−0.6154 (4)0.2576 (3)−0.6023 (5)0.0242 (9)
H7−0.65300.3058−0.59670.029*
C8−0.6648 (3)0.2037 (2)−0.7256 (4)0.0176 (8)
C9−0.7965 (3)0.2992 (2)−0.9002 (5)0.0210 (8)
H9A−0.72550.3229−0.90920.025*
H9B−0.82220.3317−0.82720.025*
C10−0.8909 (3)0.2962 (2)−1.0620 (4)0.0179 (8)
C110.1401 (3)0.0239 (3)−0.1581 (5)0.0242 (9)
C120.1937 (4)−0.0131 (3)−0.2737 (6)0.0397 (12)
H12A0.2054−0.0702−0.25100.048*
H12B0.1389−0.0075−0.38120.048*
C130.3980 (4)0.0092 (3)−0.1300 (6)0.0340 (11)
C140.4975 (4)0.0529 (3)−0.1204 (6)0.0361 (11)
H140.49600.0887−0.20140.043*
C150.4008 (4)−0.0437 (3)−0.0085 (6)0.0357 (11)
H150.3342−0.0731−0.01350.043*
O2W−0.2446 (4)0.2835 (3)−0.1500 (5)0.0604 (12)
H17A−0.229 (6)0.258 (4)−0.219 (7)0.091*
H17B−0.303 (5)0.260 (4)−0.133 (8)0.091*
U11U22U33U12U13U23
Dy10.01428 (9)0.01573 (9)0.01598 (9)0.00025 (7)0.00061 (6)0.00046 (7)
O10.0256 (15)0.0200 (14)0.0229 (14)−0.0024 (12)−0.0097 (12)−0.0005 (12)
O1W0.044 (2)0.060 (3)0.0311 (19)0.0266 (19)−0.0044 (16)−0.0118 (18)
O20.0257 (15)0.0170 (14)0.0278 (15)0.0069 (11)0.0010 (13)0.0013 (12)
O30.0199 (14)0.0197 (14)0.0236 (14)0.0063 (11)−0.0093 (12)−0.0046 (12)
O40.0150 (13)0.0162 (14)0.0233 (14)−0.0012 (10)−0.0068 (11)0.0050 (11)
O50.0303 (15)0.0203 (14)0.0180 (13)−0.0027 (12)0.0018 (12)0.0078 (12)
O60.0304 (17)0.0256 (17)0.0284 (16)−0.0090 (13)−0.0118 (13)0.0125 (13)
O70.0436 (19)0.0238 (16)0.0336 (17)−0.0028 (14)0.0226 (15)−0.0064 (13)
O80.0270 (16)0.046 (2)0.0300 (16)−0.0127 (15)0.0015 (14)0.0092 (15)
O90.0338 (18)0.063 (2)0.0360 (18)0.0116 (17)0.0216 (16)0.0022 (17)
C10.0173 (18)0.022 (2)0.0179 (18)0.0061 (15)0.0022 (15)−0.0016 (16)
C20.021 (2)0.018 (2)0.026 (2)0.0061 (16)−0.0042 (17)−0.0026 (17)
C30.0142 (17)0.019 (2)0.0204 (18)0.0005 (14)0.0000 (15)0.0004 (15)
C40.0196 (18)0.0181 (19)0.0205 (18)0.0024 (16)−0.0003 (15)−0.0044 (16)
C50.023 (2)0.023 (2)0.021 (2)0.0029 (17)−0.0057 (17)−0.0077 (17)
C60.0202 (18)0.017 (2)0.0211 (19)−0.0009 (15)−0.0024 (16)−0.0027 (15)
C70.021 (2)0.020 (2)0.026 (2)0.0051 (16)0.0002 (17)−0.0025 (17)
C80.0128 (17)0.0201 (19)0.0166 (18)0.0003 (14)0.0003 (15)0.0046 (15)
C90.024 (2)0.0146 (19)0.0195 (19)0.0001 (15)0.0008 (16)0.0022 (15)
C100.0168 (18)0.0158 (19)0.0178 (18)0.0027 (14)0.0013 (15)0.0026 (15)
C110.020 (2)0.026 (2)0.027 (2)−0.0014 (16)0.0099 (17)0.0060 (18)
C120.036 (3)0.043 (3)0.043 (3)0.001 (2)0.017 (2)−0.014 (2)
C130.032 (2)0.036 (3)0.044 (3)0.011 (2)0.025 (2)−0.001 (2)
C140.043 (3)0.032 (3)0.047 (3)0.009 (2)0.032 (2)0.009 (2)
C150.033 (2)0.033 (3)0.050 (3)0.003 (2)0.026 (2)0.001 (2)
O2W0.055 (3)0.060 (3)0.051 (3)0.016 (2)−0.003 (2)−0.013 (2)
Dy1—O8i2.333 (3)C3—O31.382 (4)
Dy1—O2i2.341 (3)C3—C51.385 (5)
Dy1—O12.399 (3)C3—C41.392 (5)
Dy1—O6ii2.417 (3)C4—C61.392 (5)
Dy1—O5iii2.421 (3)C4—H40.93
Dy1—O1W2.435 (4)C5—C71.399 (5)
Dy1—O72.471 (3)C5—H50.93
Dy1—O4ii2.624 (3)C6—C81.366 (5)
Dy1—O82.830 (4)C6—H60.93
O1—C11.255 (5)C7—C81.387 (5)
O1W—H16A0.80 (3)C7—H70.93
O1W—H16B0.79 (3)C9—C101.512 (5)
O2—C11.256 (5)C9—H9A0.97
O3—C31.382 (4)C9—H9B0.97
O3—C21.421 (5)C11—C121.514 (6)
O4—C81.400 (4)C12—H12A0.97
O4—C91.448 (4)C12—H12B0.97
O5—C101.246 (5)C13—C141.382 (7)
O6—C101.253 (5)C13—C151.384 (7)
O7—C111.240 (5)C14—C15iv1.383 (7)
O8—C111.257 (5)C14—H140.93
O9—C131.391 (6)C15—C14iv1.383 (7)
O9—C121.413 (6)C15—H150.93
C1—C21.516 (5)O2W—H17A0.82 (3)
C2—H2A0.97O2W—H17B0.86 (3)
C2—H2B0.97
O8i—Dy1—O2i71.77 (11)O3—C2—C1113.0 (3)
O8i—Dy1—O177.10 (10)O3—C2—H2A109.0
O2i—Dy1—O1131.87 (10)C1—C2—H2A109.0
O8i—Dy1—O6ii147.73 (10)O3—C2—H2B109.0
O2i—Dy1—O6ii137.92 (11)C1—C2—H2B109.0
O1—Dy1—O6ii72.10 (10)H2A—C2—H2B107.8
O8i—Dy1—O5iii81.77 (11)O3—C3—C5116.9 (3)
O2i—Dy1—O5iii73.24 (10)O3—C3—C5116.9 (3)
O1—Dy1—O5iii136.95 (11)O3—C3—C4123.6 (3)
O6ii—Dy1—O5iii114.92 (10)O3—C3—C4123.6 (3)
O8i—Dy1—O1W87.26 (14)C5—C3—C4119.5 (3)
O2i—Dy1—O1W139.73 (12)C3—C4—C6119.7 (4)
O1—Dy1—O1W71.98 (11)C3—C4—H4120.1
O6ii—Dy1—O1W74.39 (14)C6—C4—H4120.1
O5iii—Dy1—O1W69.93 (11)C3—C5—C7120.5 (4)
O8i—Dy1—O7120.17 (11)C3—C5—H5119.7
O2i—Dy1—O773.43 (11)C7—C5—H5119.7
O1—Dy1—O792.54 (11)C8—C6—C4120.4 (4)
O6ii—Dy1—O771.26 (11)C8—C6—H6119.8
O5iii—Dy1—O7130.44 (10)C4—C6—H6119.8
O1W—Dy1—O7145.27 (13)C8—C7—C5119.0 (4)
O8i—Dy1—O4ii148.49 (9)C8—C7—H7120.5
O2i—Dy1—O4ii86.51 (9)C5—C7—H7120.5
O1—Dy1—O4ii133.60 (9)C6—C8—C7120.8 (3)
O6ii—Dy1—O4ii61.51 (9)C6—C8—O4117.0 (3)
O5iii—Dy1—O4ii70.01 (10)C7—C8—O4122.2 (3)
O1W—Dy1—O4ii95.66 (12)O4—C9—C10107.5 (3)
O7—Dy1—O4ii72.37 (10)O4—C9—H9A110.2
O8i—Dy1—O873.76 (13)C10—C9—H9A110.2
O2i—Dy1—O866.07 (10)O4—C9—H9B110.2
O1—Dy1—O870.55 (10)C10—C9—H9B110.2
O6ii—Dy1—O8104.10 (10)H9A—C9—H9B108.5
O5iii—Dy1—O8137.24 (9)O5—C10—O6125.5 (3)
O1W—Dy1—O8140.83 (11)O5—C10—C9116.8 (3)
O7—Dy1—O847.87 (9)O6—C10—C9117.8 (3)
O4ii—Dy1—O8118.45 (9)O7—C11—O8121.3 (4)
C1—O1—Dy1132.4 (2)O7—C11—C12120.6 (4)
Dy1—O1W—H16A101 (5)O8—C11—C12118.0 (4)
Dy1—O1W—H16B121 (5)O9—C12—C11113.7 (4)
H16A—O1W—H16B108 (4)O9—C12—H12A108.8
C1—O2—Dy1i145.7 (3)C11—C12—H12A108.8
C3—O3—C2115.4 (3)O9—C12—H12B108.8
C8—O4—C9115.7 (3)C11—C12—H12B108.8
C8—O4—Dy1v127.1 (2)H12A—C12—H12B107.7
C9—O4—Dy1v116.5 (2)C14—C13—C15119.3 (5)
C10—O5—Dy1vi137.2 (3)C14—C13—O9115.6 (4)
C10—O6—Dy1v128.9 (2)C15—C13—O9125.0 (5)
C11—O7—Dy1104.3 (3)C13—C14—C15iv120.6 (4)
C11—O8—Dy1i160.3 (3)C13—C14—H14119.7
C11—O8—Dy186.5 (3)C15iv—C14—H14119.7
Dy1i—O8—Dy1106.24 (12)C14iv—C15—C13120.0 (5)
C13—O9—C12118.0 (4)C14iv—C15—H15120.0
O1—C1—O2127.4 (3)C13—C15—H15120.0
O1—C1—C2120.3 (3)H17A—O2W—H17B108 (4)
O2—C1—C2112.2 (3)
O8i—Dy1—O1—C1−35.1 (4)C2—O3—C3—C5172.1 (4)
O2i—Dy1—O1—C115.4 (4)O3—O3—C3—C40.0 (3)
O6ii—Dy1—O1—C1154.7 (4)C2—O3—C3—C4−7.1 (6)
O5iii—Dy1—O1—C1−97.7 (4)O3—C3—C4—C6178.5 (4)
O1W—Dy1—O1—C1−126.4 (4)O3—C3—C4—C6178.5 (4)
O7—Dy1—O1—C185.3 (4)C5—C3—C4—C6−0.6 (6)
O4ii—Dy1—O1—C1153.2 (3)O3—C3—C5—C7−178.1 (4)
O8—Dy1—O1—C142.0 (4)O3—C3—C5—C7−178.1 (4)
O8i—Dy1—O7—C1114.8 (3)C4—C3—C5—C71.1 (7)
O2i—Dy1—O7—C1171.4 (3)C3—C4—C6—C8−0.9 (6)
O1—Dy1—O7—C11−61.7 (3)C3—C5—C7—C80.1 (7)
O6ii—Dy1—O7—C11−131.9 (3)C4—C6—C8—C72.1 (6)
O5iii—Dy1—O7—C11121.0 (3)C4—C6—C8—O4−176.8 (4)
O1W—Dy1—O7—C11−123.1 (3)C5—C7—C8—C6−1.6 (6)
O4ii—Dy1—O7—C11163.0 (3)C5—C7—C8—O4177.2 (4)
O8—Dy1—O7—C11−1.0 (2)C9—O4—C8—C6−139.9 (4)
O8i—Dy1—O8—C11−164.8 (3)Dy1v—O4—C8—C649.9 (5)
O2i—Dy1—O8—C11−87.9 (2)C9—O4—C8—C741.2 (5)
O1—Dy1—O8—C11113.5 (3)Dy1v—O4—C8—C7−129.0 (3)
O6ii—Dy1—O8—C1148.6 (2)C8—O4—C9—C10158.0 (3)
O5iii—Dy1—O8—C11−107.1 (3)Dy1v—O4—C9—C10−30.8 (4)
O1W—Dy1—O8—C11131.1 (3)Dy1vi—O5—C10—O6−34.7 (7)
O7—Dy1—O8—C111.0 (2)Dy1vi—O5—C10—C9146.8 (3)
O4ii—Dy1—O8—C11−16.3 (3)Dy1v—O6—C10—O5−177.4 (3)
O8i—Dy1—O8—Dy1i0.0Dy1v—O6—C10—C91.1 (6)
O2i—Dy1—O8—Dy1i76.87 (12)O4—C9—C10—O5−160.8 (3)
O1—Dy1—O8—Dy1i−81.74 (12)O4—C9—C10—O620.5 (5)
O6ii—Dy1—O8—Dy1i−146.60 (11)Dy1—O7—C11—O82.0 (5)
O5iii—Dy1—O8—Dy1i57.68 (18)Dy1—O7—C11—C12177.9 (3)
O1W—Dy1—O8—Dy1i−64.1 (2)Dy1i—O8—C11—O7−133.2 (8)
O7—Dy1—O8—Dy1i165.76 (18)Dy1—O8—C11—O7−1.7 (4)
O4ii—Dy1—O8—Dy1i148.44 (9)Dy1i—O8—C11—C1250.8 (10)
Dy1—O1—C1—O2−0.9 (7)Dy1—O8—C11—C12−177.7 (4)
Dy1—O1—C1—C2−179.0 (3)C13—O9—C12—C1168.3 (6)
Dy1i—O2—C1—O1−18.9 (8)O7—C11—C12—O918.6 (6)
Dy1i—O2—C1—C2159.4 (4)O8—C11—C12—O9−165.4 (4)
O3—O3—C2—C10.00 (8)C12—O9—C13—C14−172.0 (4)
C3—O3—C2—C1−174.5 (4)C12—O9—C13—C159.4 (7)
O1—C1—C2—O3−27.4 (6)C15—C13—C14—C15iv0.4 (8)
O2—C1—C2—O3154.2 (4)O9—C13—C14—C15iv−178.4 (4)
C2—O3—C3—O30(43)C14—C13—C15—C14iv−0.4 (8)
O3—O3—C3—C50.00 (12)O9—C13—C15—C14iv178.3 (4)
D—H···AD—HH···AD···AD—H···A
O1W—H16A···O6iii0.80 (3)2.11 (5)2.706 (4)131 (6)
O1W—H16B···O2W0.79 (3)1.98 (4)2.755 (6)166 (7)
O2W—H17A···O30.82 (3)2.41 (6)2.952 (5)125 (5)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H16A⋯O6i0.80 (3)2.11 (5)2.706 (4)131 (6)
O1W—H16B⋯O2W0.79 (3)1.98 (4)2.755 (6)166 (7)
O2W—H17A⋯O30.82 (3)2.41 (6)2.952 (5)125 (5)

Symmetry code: (i) .

  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.  Modular chemistry: secondary building units as a basis for the design of highly porous and robust metal-organic carboxylate frameworks.

Authors:  M Eddaoudi; D B Moler; H Li; B Chen; T M Reineke; M O'Keeffe; O M Yaghi
Journal:  Acc Chem Res       Date:  2001-04       Impact factor: 22.384
  2 in total

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