Literature DB >> 22589816

Poly[tetra-aqua-bis-(μ(3)-oxalato-κ(5)O(1),O(2):O(1'):O(1'),O(2'))(μ(2)-oxalato-κ(4)O(1),O(2):O(1'),O(2'))dipraseodymium(III)].

Cheng-Jun Hao1, Hui Xie.   

Abstract

In the title complex, [Pr(2)(C(2)O(4))(3)(H(2)O)(4)](n), the two independent Pr(III) ions are both nine-coordinated in a distorted monocapped square-anti-prismatic geometry by seven O atoms from four oxalate ligands and two water mol-ecules. The Pr(III) ions are bridged by the oxalate ligands, forming a layer parallel to (001). O-H⋯O hydrogen bonds connect the layers.

Entities:  

Year:  2012        PMID： 22589816      PMCID： PMC3343842          DOI： 10.1107/S1600536812011014

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


Related literature

For the structures and potential applications of lanthanide complexes, see: Ma et al. (2001 ▶); Shibasaki & Yoshikawa (2002 ▶); Song et al. (2012 ▶).

Experimental

Crystal data

[Pr2(C2O4)3(H2O)4] M = 617.94 Orthorhombic, a = 8.6358 (17) Å b = 9.5356 (19) Å c = 16.885 (3) Å V = 1390.4 (5) Å3 Z = 4 Mo Kα radiation μ = 7.02 mm−1 T = 293 K 0.23 × 0.22 × 0.20 mm

Data collection

Rigaku Mercury CCD diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2002 ▶) T min = 0.295, T max = 0.334 13654 measured reflections 3181 independent reflections 2826 reflections with I > 2σ(I) R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.029 wR(F 2) = 0.072 S = 1.04 3181 reflections 217 parameters H-atom parameters constrained Δρmax = 1.34 e Å−3 Δρmin = −1.44 e Å−3 Absolute structure: Flack (1983 ▶), 1344 Friedel pairs Flack parameter: 0.49 (3) Data collection: CrystalClear (Rigaku, 2002 ▶); cell refinement: CrystalClear; 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: ORTEPII (Johnson, 1976 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812011014/hy2521sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812011014/hy2521Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pr2(C2O4)3(H2O)4]F(000) = 1160
Mr = 617.94Dx = 2.952 Mg m−3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 3600 reflections
a = 8.6358 (17) Åθ = 1.4–28.0°
b = 9.5356 (19) ŵ = 7.02 mm−1
c = 16.885 (3) ÅT = 293 K
V = 1390.4 (5) Å3Block, green
Z = 40.23 × 0.22 × 0.20 mm
Rigaku Mercury CCD diffractometer3181 independent reflections
Radiation source: fine-focus sealed tube2826 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ω scansθmax = 27.4°, θmin = 3.2°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2002)h = −9→11
Tmin = 0.295, Tmax = 0.334k = −12→12
13654 measured reflectionsl = −21→21
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.029H-atom parameters constrained
wR(F2) = 0.072w = 1/[σ2(Fo2) + (0.0284P)2 + 3.201P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
3181 reflectionsΔρmax = 1.34 e Å−3
217 parametersΔρmin = −1.44 e Å−3
0 restraintsAbsolute structure: Flack (1983), 1344 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.49 (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
Pr10.37510 (4)0.75389 (2)0.143154 (14)0.01214 (9)
Pr2−0.12589 (4)0.26126 (3)0.137142 (14)0.01185 (8)
O10.3263 (5)0.4984 (4)0.1336 (3)0.0245 (10)
O20.1023 (5)0.6852 (4)0.1081 (2)0.0220 (9)
O30.1479 (5)0.3304 (5)0.1473 (3)0.0383 (12)
O4−0.0761 (5)0.5159 (5)0.1102 (3)0.0236 (10)
O50.5734 (5)0.8913 (4)0.0744 (2)0.0220 (9)
O60.4832 (5)0.9677 (5)0.2184 (2)0.0221 (9)
O70.6490 (5)1.1490 (4)0.2172 (2)0.0209 (9)
O80.7467 (5)1.0643 (5)0.0716 (3)0.0255 (10)
O90.0572 (5)0.0999 (5)0.0683 (2)0.0205 (9)
O10−0.0198 (5)0.0560 (4)0.2191 (2)0.0230 (9)
O110.1596 (4)−0.1155 (4)0.2289 (2)0.0186 (9)
O120.2521 (5)−0.0484 (4)0.0791 (2)0.0219 (9)
O1W0.4097 (7)0.6778 (5)0.0052 (2)0.0361 (14)
H1W0.47470.7253−0.02150.054*
H2W0.35610.6140−0.01680.054*
O2W0.6418 (6)0.6597 (5)0.1743 (3)0.0357 (11)
H3W0.70100.65990.13410.053*
H4W0.63690.59500.20880.053*
O3W−0.1196 (7)0.3125 (5)−0.0081 (2)0.0296 (10)
H5W−0.14470.3960−0.02000.044*
H6W−0.15670.2530−0.04040.044*
O4W−0.3828 (6)0.3679 (5)0.0986 (2)0.0303 (10)
H7W−0.44430.40930.13040.045*
H8W−0.41200.38340.05130.045*
C10.1907 (7)0.4536 (6)0.1341 (4)0.0214 (13)
C20.0597 (7)0.5610 (6)0.1160 (3)0.0196 (12)
C30.6393 (7)0.9949 (6)0.1035 (3)0.0160 (12)
C40.5861 (6)1.0398 (6)0.1870 (3)0.0169 (12)
C50.1355 (7)0.0127 (5)0.1057 (3)0.0164 (11)
C60.0863 (6)−0.0190 (6)0.1925 (3)0.0166 (12)
U11U22U33U12U13U23
Pr10.01379 (15)0.00894 (14)0.01370 (14)−0.00143 (13)0.00092 (11)0.00098 (9)
Pr20.01324 (15)0.00861 (13)0.01371 (14)−0.00137 (13)0.00076 (12)−0.00112 (9)
O10.025 (2)0.013 (2)0.035 (2)−0.0023 (16)−0.001 (2)0.0004 (18)
O20.019 (2)0.019 (2)0.028 (2)−0.0007 (18)−0.0038 (19)0.0043 (16)
O30.018 (2)0.0103 (19)0.086 (4)−0.0033 (18)−0.005 (2)0.009 (2)
O40.022 (2)0.018 (2)0.031 (2)−0.0029 (16)−0.0023 (19)0.0017 (18)
O50.030 (2)0.015 (2)0.020 (2)−0.0103 (17)0.0063 (18)−0.0088 (17)
O60.025 (2)0.025 (2)0.0165 (18)−0.0139 (18)0.0081 (18)−0.0051 (18)
O70.028 (2)0.0162 (19)0.0188 (18)−0.0058 (17)0.0033 (19)−0.0052 (15)
O80.030 (2)0.022 (3)0.024 (2)−0.0126 (19)0.010 (2)−0.0098 (19)
O90.025 (2)0.020 (2)0.0162 (19)0.0110 (18)0.0016 (18)0.0036 (17)
O100.027 (2)0.024 (2)0.019 (2)0.0093 (18)0.0056 (19)0.0051 (19)
O110.021 (2)0.019 (2)0.0155 (18)0.0023 (16)−0.0005 (17)0.0045 (15)
O120.027 (2)0.017 (2)0.022 (2)0.0088 (18)0.0093 (18)0.0092 (18)
O1W0.056 (4)0.027 (3)0.025 (2)−0.023 (2)0.016 (2)−0.0094 (17)
O2W0.030 (3)0.030 (3)0.046 (3)0.008 (2)0.003 (3)0.006 (2)
O3W0.046 (3)0.020 (2)0.024 (2)0.007 (3)0.002 (2)0.0062 (15)
O4W0.027 (2)0.038 (3)0.027 (2)0.008 (2)−0.001 (2)0.0004 (17)
C10.022 (3)0.013 (3)0.029 (3)−0.003 (2)0.002 (3)0.000 (3)
C20.027 (3)0.018 (3)0.014 (3)−0.001 (2)0.000 (2)−0.001 (2)
C30.016 (3)0.015 (3)0.017 (3)0.002 (3)0.004 (3)−0.0010 (18)
C40.021 (3)0.014 (3)0.015 (3)−0.001 (2)−0.001 (2)−0.002 (2)
C50.022 (3)0.009 (3)0.018 (3)0.000 (3)0.000 (3)0.0023 (18)
C60.020 (3)0.016 (3)0.014 (2)−0.001 (2)−0.002 (2)0.002 (2)
Pr1—O12i2.419 (4)O4—C21.253 (7)
Pr1—O52.449 (4)O5—C31.241 (6)
Pr1—O1W2.458 (4)O6—C41.242 (7)
Pr1—O12.478 (4)O7—C41.281 (7)
Pr1—O22.516 (4)O8—C31.261 (7)
Pr1—O2W2.527 (5)O9—C51.244 (7)
Pr1—O7ii2.570 (4)O10—C61.247 (7)
Pr1—O62.578 (4)O11—C61.275 (7)
Pr1—O11i2.666 (4)O12—C51.247 (7)
Pr2—O8iii2.442 (4)O1W—H1W0.8500
Pr2—O32.460 (4)O1W—H2W0.8501
Pr2—O92.494 (4)O2W—H3W0.8500
Pr2—O3W2.501 (4)O2W—H4W0.8500
Pr2—O42.508 (4)O3W—H5W0.8500
Pr2—O4W2.526 (5)O3W—H6W0.8499
Pr2—O11iv2.565 (4)O4W—H7W0.8511
Pr2—O102.566 (4)O4W—H8W0.8513
Pr2—O7iii2.598 (4)C1—C21.556 (9)
O1—C11.247 (7)C3—C41.544 (7)
O2—C21.247 (7)C5—C61.555 (8)
O3—C11.252 (7)
O12i—Pr1—O571.23 (15)O9—Pr2—O1063.55 (13)
O12i—Pr1—O1W81.93 (16)O3W—Pr2—O10132.08 (14)
O5—Pr1—O1W67.89 (15)O4—Pr2—O10140.82 (14)
O12i—Pr1—O1131.49 (15)O4W—Pr2—O10139.42 (14)
O5—Pr1—O1127.89 (14)O11iv—Pr2—O1085.07 (13)
O1W—Pr1—O170.66 (15)O8iii—Pr2—O7iii65.29 (13)
O12i—Pr1—O271.72 (14)O3—Pr2—O7iii142.48 (15)
O5—Pr1—O2133.05 (13)O9—Pr2—O7iii117.55 (13)
O1W—Pr1—O279.30 (16)O3W—Pr2—O7iii127.34 (15)
O1—Pr1—O264.51 (14)O4—Pr2—O7iii128.43 (13)
O12i—Pr1—O2W140.37 (15)O4W—Pr2—O7iii69.05 (14)
O5—Pr1—O2W69.61 (15)O11iv—Pr2—O7iii69.21 (11)
O1W—Pr1—O2W88.94 (17)O10—Pr2—O7iii70.88 (13)
O1—Pr1—O2W79.57 (15)C1—O1—Pr1119.7 (4)
O2—Pr1—O2W144.08 (15)C2—O2—Pr1119.9 (4)
O12i—Pr1—O7ii132.68 (13)C1—O3—Pr2121.5 (4)
O5—Pr1—O7ii134.42 (14)C2—O4—Pr2118.6 (4)
O1W—Pr1—O7ii139.87 (15)C3—O5—Pr1123.9 (4)
O1—Pr1—O7ii70.32 (14)C4—O6—Pr1119.1 (3)
O2—Pr1—O7ii92.21 (13)C4—O7—Pr1v130.3 (3)
O2W—Pr1—O7ii75.20 (14)C4—O7—Pr2vi116.5 (3)
O12i—Pr1—O676.29 (15)Pr1v—O7—Pr2vi112.19 (14)
O5—Pr1—O663.73 (12)C3—O8—Pr2vi122.8 (3)
O1W—Pr1—O6131.05 (14)C5—O9—Pr2121.3 (4)
O1—Pr1—O6150.63 (14)C6—O10—Pr2120.4 (3)
O2—Pr1—O6131.37 (13)C6—O11—Pr2vii134.4 (3)
O2W—Pr1—O681.29 (14)C6—O11—Pr1viii114.9 (3)
O7ii—Pr1—O683.38 (13)Pr2vii—O11—Pr1viii110.13 (14)
O12i—Pr1—O11i64.69 (12)C5—O12—Pr1viii123.9 (3)
O5—Pr1—O11i119.72 (13)Pr1—O1W—H1W115.2
O1W—Pr1—O11i137.50 (16)Pr1—O1W—H2W124.0
O1—Pr1—O11i112.07 (13)H1W—O1W—H2W120.6
O2—Pr1—O11i66.14 (12)Pr1—O2W—H3W112.4
O2W—Pr1—O11i133.55 (12)Pr1—O2W—H4W110.8
O7ii—Pr1—O11i68.09 (12)H3W—O2W—H4W125.4
O6—Pr1—O11i67.40 (12)Pr2—O3W—H5W114.3
O8iii—Pr2—O3132.12 (15)Pr2—O3W—H6W119.4
O8iii—Pr2—O966.40 (15)H5W—O3W—H6W112.1
O3—Pr2—O965.72 (15)Pr2—O4W—H7W124.9
O8iii—Pr2—O3W73.46 (15)Pr2—O4W—H8W124.9
O3—Pr2—O3W89.72 (18)H7W—O4W—H8W109.1
O9—Pr2—O3W69.50 (14)O1—C1—O3126.9 (6)
O8iii—Pr2—O4137.69 (15)O1—C1—C2117.2 (5)
O3—Pr2—O465.69 (14)O3—C1—C2116.0 (5)
O9—Pr2—O4113.85 (14)O2—C2—O4126.4 (6)
O3W—Pr2—O468.22 (15)O2—C2—C1115.6 (5)
O8iii—Pr2—O4W78.30 (16)O4—C2—C1118.0 (5)
O3—Pr2—O4W138.94 (15)O5—C3—O8125.9 (5)
O9—Pr2—O4W133.26 (13)O5—C3—C4116.5 (5)
O3W—Pr2—O4W71.82 (15)O8—C3—C4117.6 (5)
O4—Pr2—O4W73.38 (14)O6—C4—O7125.7 (5)
O8iii—Pr2—O11iv134.49 (13)O6—C4—C3116.7 (5)
O3—Pr2—O11iv85.69 (15)O7—C4—C3117.6 (5)
O9—Pr2—O11iv139.96 (13)O9—C5—O12124.6 (5)
O3W—Pr2—O11iv141.03 (13)O9—C5—C6117.4 (5)
O4—Pr2—O11iv74.70 (14)O12—C5—C6118.0 (5)
O4W—Pr2—O11iv86.72 (13)O10—C6—O11127.2 (5)
O8iii—Pr2—O1079.57 (15)O10—C6—C5115.4 (5)
O3—Pr2—O1079.85 (14)O11—C6—C5117.3 (5)
O12i—Pr1—O1—C1−43.6 (5)O4W—Pr2—O9—C5−146.9 (4)
O5—Pr1—O1—C1−141.8 (4)O11iv—Pr2—O9—C529.4 (5)
O1W—Pr1—O1—C1−103.0 (5)O10—Pr2—O9—C5−12.7 (4)
O2—Pr1—O1—C1−15.9 (4)O7iii—Pr2—O9—C5−60.5 (5)
O2W—Pr1—O1—C1164.5 (5)O8iii—Pr2—O10—C677.6 (4)
O7ii—Pr1—O1—C186.6 (5)O3—Pr2—O10—C6−58.9 (4)
O6—Pr1—O1—C1114.3 (5)O9—Pr2—O10—C68.9 (4)
O11i—Pr1—O1—C131.5 (5)O3W—Pr2—O10—C621.4 (5)
O12i—Pr1—O2—C2171.5 (4)O4—Pr2—O10—C6−87.1 (5)
O5—Pr1—O2—C2132.1 (4)O4W—Pr2—O10—C6135.4 (4)
O1W—Pr1—O2—C286.6 (4)O11iv—Pr2—O10—C6−145.4 (4)
O1—Pr1—O2—C213.0 (4)O7iii—Pr2—O10—C6144.9 (5)
O2W—Pr1—O2—C213.6 (5)Pr1—O1—C1—O3−163.0 (6)
O7ii—Pr1—O2—C2−53.9 (4)Pr1—O1—C1—C217.5 (7)
O6—Pr1—O2—C2−137.1 (4)Pr2—O3—C1—O1−176.1 (5)
O11i—Pr1—O2—C2−118.8 (4)Pr2—O3—C1—C23.5 (8)
O8iii—Pr2—O3—C1132.1 (5)Pr1—O2—C2—O4170.7 (5)
O9—Pr2—O3—C1132.4 (6)Pr1—O2—C2—C1−9.8 (7)
O3W—Pr2—O3—C164.9 (5)Pr2—O4—C2—O2−176.5 (5)
O4—Pr2—O3—C1−1.2 (5)Pr2—O4—C2—C14.0 (7)
O4W—Pr2—O3—C13.6 (6)O1—C1—C2—O2−5.0 (8)
O11iv—Pr2—O3—C1−76.4 (5)O3—C1—C2—O2175.4 (6)
O10—Pr2—O3—C1−162.1 (5)O1—C1—C2—O4174.6 (5)
O7iii—Pr2—O3—C1−123.3 (5)O3—C1—C2—O4−5.0 (9)
O8iii—Pr2—O4—C2−128.4 (4)Pr1—O5—C3—O8176.5 (5)
O3—Pr2—O4—C2−1.8 (4)Pr1—O5—C3—C4−2.1 (7)
O9—Pr2—O4—C2−47.9 (5)Pr2vi—O8—C3—O5−177.6 (5)
O3W—Pr2—O4—C2−101.8 (5)Pr2vi—O8—C3—C41.0 (7)
O4W—Pr2—O4—C2−178.4 (5)Pr1—O6—C4—O7179.3 (4)
O11iv—Pr2—O4—C290.4 (4)Pr1—O6—C4—C30.9 (6)
O10—Pr2—O4—C228.9 (5)Pr1v—O7—C4—O68.5 (9)
O7iii—Pr2—O4—C2137.0 (4)Pr2vi—O7—C4—O6175.9 (5)
O12i—Pr1—O5—C385.5 (5)Pr1v—O7—C4—C3−173.1 (3)
O1W—Pr1—O5—C3174.2 (5)Pr2vi—O7—C4—C3−5.7 (6)
O1—Pr1—O5—C3−146.1 (4)O5—C3—C4—O60.7 (8)
O2—Pr1—O5—C3125.0 (4)O8—C3—C4—O6−178.0 (6)
O2W—Pr1—O5—C3−88.3 (5)O5—C3—C4—O7−177.8 (6)
O7ii—Pr1—O5—C3−46.6 (5)O8—C3—C4—O73.4 (8)
O6—Pr1—O5—C31.8 (4)Pr2—O9—C5—O12−163.2 (4)
O11i—Pr1—O5—C341.0 (5)Pr2—O9—C5—C615.3 (7)
O12i—Pr1—O6—C4−76.9 (4)Pr1viii—O12—C5—O9−168.6 (4)
O5—Pr1—O6—C4−1.3 (4)Pr1viii—O12—C5—C612.9 (7)
O1W—Pr1—O6—C4−10.7 (5)Pr2—O10—C6—O11173.1 (4)
O1—Pr1—O6—C4120.0 (4)Pr2—O10—C6—C5−5.4 (7)
O2—Pr1—O6—C4−126.7 (4)Pr2vii—O11—C6—O109.0 (9)
O2W—Pr1—O6—C470.2 (4)Pr1viii—O11—C6—O10179.4 (5)
O7ii—Pr1—O6—C4146.1 (4)Pr2vii—O11—C6—C5−172.6 (3)
O11i—Pr1—O6—C4−144.9 (4)Pr1viii—O11—C6—C5−2.2 (6)
O8iii—Pr2—O9—C5−102.6 (5)O9—C5—C6—O10−6.3 (8)
O3—Pr2—O9—C577.7 (4)O12—C5—C6—O10172.3 (5)
O3W—Pr2—O9—C5177.1 (5)O9—C5—C6—O11175.1 (5)
O4—Pr2—O9—C5123.9 (4)O12—C5—C6—O11−6.4 (8)
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O2ix0.852.022.852 (6)166
O1W—H2W···O8x0.852.152.998 (6)173
O2W—H3W···O4xi0.852.402.998 (6)128
O2W—H4W···O6ii0.852.012.792 (6)152
O3W—H5W···O12xii0.851.972.780 (6)158
O3W—H6W···O3xii0.852.603.379 (7)154
O4W—H7W···O1xiii0.852.162.865 (6)140
O4W—H8W···O9xii0.852.042.882 (6)169
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1W⋯O2i0.852.022.852 (6)166
O1W—H2W⋯O8ii0.852.152.998 (6)173
O2W—H3W⋯O4iii0.852.402.998 (6)128
O2W—H4W⋯O6iv0.852.012.792 (6)152
O3W—H5W⋯O12v0.851.972.780 (6)158
O3W—H6W⋯O3v0.852.603.379 (7)154
O4W—H7W⋯O1vi0.852.162.865 (6)140
O4W—H8W⋯O9v0.852.042.882 (6)169

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

  3 in total

1.  Lanthanide complexes in multifunctional asymmetric catalysis.

Authors:  Masakatsu Shibasaki; Naoki Yoshikawa
Journal:  Chem Rev       Date:  2002-06       Impact factor: 60.622

2.  A short history of SHELX.

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

3.  Cyano-Bridged 4f-3d Coordination Polymers with a Unique Two-Dimensional Topological Architecture and Unusual Magnetic Behavior.

Authors:  Bao-Qing Ma; Song Gao; Gang Su; Guang-Xian Xu
Journal:  Angew Chem Int Ed Engl       Date:  2001-01-19       Impact factor: 15.336
  3 in total

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