Literature DB >> 21202787

Poly[[triaqua-tri-μ(5)-tartrato-dilanthanum(III)] dihydrate].

Liu Shi-Zhu1.   

Abstract

In the title polymer, {[La(2)(C(4)H(4)O(6))(3)(H(2)O)(3)]·2H(2)O}(n), two symmetry-independent La(III) ions are nine-coordinated and display a distorted monocapped square-anti-prismatic geometry. One is coordinated by seven O atoms from four tartrate ligands and two water mol-ecules, the other by eight O atoms from five tartrate ligands and one water mol-ecule. The three tartrate ligands in the asymmetric unit act identically as μ(5)-ligands, which link lanthanum centres to form a three-dimensional coordination framework. An extensive network of hydrogen bonds is observed in the crystal structure, involving two uncoordinated water mol-ecules, one of which is disordered over two positions, with occupancies of 0.550 (13) and 0.450 (13).

Entities:  

Year:  2008        PMID: 21202787      PMCID: PMC2961792          DOI: 10.1107/S160053680801756X

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


Related literature

For related literature, see: Yaghi et al. (1998 ▶, 2003 ▶); Serre et al. (2004 ▶); James et al. (2003 ▶).

Experimental

Crystal data

[La2(C4H4O6)3(H2O)3]·2H2O M = 812.12 Monoclinic, a = 12.6271 (2) Å b = 12.9273 (2) Å c = 16.6556 (3) Å β = 127.801 (1)° V = 2148.22 (6) Å3 Z = 4 Mo Kα radiation μ = 4.04 mm−1 T = 296 (2) K 0.25 × 0.21 × 0.18 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.372, T max = 0.480 19115 measured reflections 3771 independent reflections 3226 reflections with I > 2σ(I) R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.057 S = 1.05 3771 reflections 344 parameters H-atom parameters constrained Δρmax = 0.87 e Å−3 Δρmin = −0.65 e Å−3 Data collection: SMART (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); 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 datablocks I, global. DOI: 10.1107/S160053680801756X/bh2174sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680801756X/bh2174Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[La2(C4H4O6)3(H2O)3]·2H2OF000 = 1568
Mr = 812.12Dx = 2.511 Mg m3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 15678 reflections
a = 12.6271 (2) Åθ = 1.4–28.0º
b = 12.9273 (2) ŵ = 4.04 mm1
c = 16.6556 (3) ÅT = 296 (2) K
β = 127.801 (1)ºBlock, colourless
V = 2148.22 (6) Å30.25 × 0.21 × 0.18 mm
Z = 4
Bruker APEXII area-detector diffractometer3771 independent reflections
Radiation source: fine-focus sealed tube3226 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.047
T = 296(2) Kθmax = 25.2º
φ and ω scansθmin = 2.0º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −15→15
Tmin = 0.372, Tmax = 0.480k = −15→14
19115 measured reflectionsl = −19→19
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.057  w = 1/[σ2(Fo2) + (0.0203P)2 + 3.8165P] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
3771 reflectionsΔρmax = 0.87 e Å3
344 parametersΔρmin = −0.65 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
xyzUiso*/UeqOcc. (<1)
C1−0.0900 (4)0.9566 (4)0.5698 (3)0.0155 (10)
C2−0.1083 (4)0.8523 (4)0.5199 (3)0.0177 (10)
H2−0.02950.84160.52240.021*
C3−0.2308 (4)0.8455 (4)0.4086 (3)0.0176 (10)
H3−0.24320.91360.37820.021*
C4−0.2140 (4)0.7672 (4)0.3482 (3)0.0174 (10)
C50.0357 (5)1.0235 (4)0.9197 (3)0.0183 (10)
C60.1840 (4)0.9984 (4)0.9767 (3)0.0184 (10)
H60.22491.05870.96970.022*
C70.2635 (4)0.9782 (3)1.0918 (3)0.0165 (10)
H70.23331.02651.11930.020*
C80.4144 (4)0.9950 (4)1.1463 (3)0.0172 (10)
C90.2706 (4)0.7265 (4)0.8239 (3)0.0171 (10)
C100.2636 (4)0.6536 (4)0.8918 (3)0.0152 (10)
H100.24240.58410.86230.018*
C110.3977 (4)0.6497 (3)0.9974 (3)0.0150 (10)
H110.46870.64460.98990.018*
C120.4096 (4)0.5570 (3)1.0589 (3)0.0137 (10)
La1−0.02226 (2)0.81431 (2)0.77118 (2)0.01422 (8)
La2−0.54797 (2)0.73846 (2)0.22545 (2)0.01381 (8)
O1−0.0471 (3)0.9566 (3)0.6612 (2)0.0248 (8)
O2−0.1144 (3)1.0376 (2)0.5208 (2)0.0207 (7)
O3−0.1053 (3)0.7743 (2)0.5816 (2)0.0221 (7)
H3A−0.06610.72670.57760.033*
O4−0.3519 (3)0.8206 (2)0.3936 (2)0.0184 (7)
H4−0.36500.86450.42220.028*
O5−0.3178 (3)0.7172 (2)0.2791 (2)0.0221 (8)
O6−0.1040 (3)0.7609 (3)0.3649 (2)0.0232 (8)
O7−0.0495 (3)0.9637 (3)0.8484 (2)0.0255 (8)
O80.0074 (3)1.1045 (2)0.9438 (3)0.0226 (8)
O90.1947 (3)0.9140 (3)0.9266 (3)0.0294 (8)
H90.23720.87030.97100.044*
O100.2457 (3)0.8752 (2)1.1112 (2)0.0237 (8)
H10A0.17140.87111.09730.036*
O110.4892 (3)0.9167 (2)1.1844 (2)0.0214 (7)
O120.4517 (3)1.0853 (2)1.1460 (2)0.0213 (7)
O130.1759 (3)0.7910 (3)0.7713 (3)0.0256 (8)
O140.3687 (3)0.7181 (3)0.8235 (2)0.0235 (8)
O150.1587 (3)0.6864 (2)0.8953 (2)0.0197 (7)
H150.14380.64270.92280.030*
O160.4191 (3)0.7419 (2)1.0529 (2)0.0212 (7)
H160.45260.78321.03700.032*
O170.4440 (3)0.5724 (2)1.1455 (2)0.0238 (8)
O180.3836 (3)0.4696 (2)1.0164 (2)0.0194 (7)
O1W−0.2694 (3)0.8479 (3)0.6519 (3)0.0322 (9)
H1W−0.30290.84250.68090.048*
H2W−0.30740.89670.61290.048*
O2W−0.1015 (3)0.6276 (3)0.7134 (2)0.0307 (8)
H4W−0.17750.61380.69320.046*
H3W−0.05430.58150.75430.046*
O3W−0.7660 (3)0.6479 (3)0.1489 (3)0.0363 (10)
H6W−0.80760.64210.17150.054*
H5W−0.80250.60850.10040.054*
O5W0.6940 (6)0.5141 (5)0.6746 (7)0.139 (3)
H10W0.65040.56180.63120.208*
H9W0.64460.49370.69000.208*
O4WA0.4665 (13)0.9039 (8)0.9799 (8)0.056 (5)0.450 (13)
H4WA0.43040.84940.98180.084*0.450 (13)
H4WB0.48770.88890.94170.084*0.450 (13)
O4WB0.5902 (11)0.8436 (8)1.0338 (7)0.072 (4)0.550 (13)
H4WC0.58540.82950.98180.108*0.550 (13)
H4WD0.54000.89611.01690.108*0.550 (13)
U11U22U33U12U13U23
C10.008 (2)0.020 (3)0.017 (3)−0.0002 (18)0.008 (2)0.000 (2)
C20.018 (2)0.019 (3)0.019 (2)−0.0007 (19)0.013 (2)0.001 (2)
C30.014 (2)0.018 (3)0.019 (3)−0.0001 (18)0.010 (2)−0.001 (2)
C40.018 (3)0.020 (3)0.016 (2)−0.0001 (19)0.011 (2)0.002 (2)
C50.026 (3)0.015 (3)0.017 (2)0.000 (2)0.015 (2)0.005 (2)
C60.023 (2)0.016 (3)0.018 (2)−0.0038 (19)0.013 (2)−0.003 (2)
C70.025 (3)0.010 (2)0.019 (2)0.0028 (19)0.015 (2)0.003 (2)
C80.025 (3)0.015 (3)0.013 (2)0.000 (2)0.012 (2)−0.002 (2)
C90.019 (3)0.020 (3)0.013 (2)−0.0007 (19)0.010 (2)−0.001 (2)
C100.015 (2)0.015 (3)0.020 (2)0.0020 (18)0.013 (2)0.0033 (19)
C110.020 (2)0.014 (2)0.016 (2)0.0004 (18)0.013 (2)−0.0021 (19)
C120.010 (2)0.016 (3)0.018 (2)0.0019 (18)0.0102 (19)−0.002 (2)
La10.01520 (14)0.01340 (16)0.01582 (14)0.00137 (10)0.01041 (12)0.00210 (11)
La20.01507 (14)0.01329 (15)0.01485 (14)−0.00060 (10)0.01008 (12)−0.00145 (11)
O10.035 (2)0.024 (2)0.0153 (18)−0.0022 (15)0.0153 (16)−0.0006 (15)
O20.0321 (19)0.0115 (18)0.0204 (18)0.0018 (14)0.0170 (16)0.0048 (14)
O30.0296 (19)0.0142 (18)0.0211 (18)0.0049 (14)0.0148 (16)0.0042 (14)
O40.0148 (16)0.0217 (19)0.0211 (18)−0.0020 (13)0.0123 (14)−0.0078 (14)
O50.0188 (18)0.027 (2)0.0230 (18)−0.0058 (14)0.0140 (15)−0.0108 (15)
O60.0202 (18)0.031 (2)0.0234 (19)−0.0026 (14)0.0158 (15)−0.0061 (15)
O70.0218 (18)0.025 (2)0.0244 (19)−0.0017 (14)0.0116 (16)−0.0084 (16)
O80.0267 (18)0.0119 (18)0.034 (2)−0.0001 (14)0.0208 (16)−0.0045 (15)
O90.0268 (19)0.033 (2)0.0237 (19)0.0059 (15)0.0129 (16)−0.0087 (16)
O100.0199 (17)0.0202 (19)0.033 (2)0.0000 (14)0.0170 (16)0.0073 (16)
O110.0196 (17)0.0160 (18)0.0259 (18)−0.0002 (14)0.0126 (15)0.0017 (15)
O120.0273 (18)0.0150 (19)0.0174 (17)−0.0051 (14)0.0115 (15)−0.0027 (14)
O130.0247 (19)0.031 (2)0.028 (2)0.0126 (15)0.0197 (16)0.0147 (16)
O140.0207 (18)0.033 (2)0.0245 (19)0.0064 (15)0.0181 (16)0.0072 (16)
O150.0174 (17)0.0201 (19)0.0271 (19)0.0030 (13)0.0164 (15)0.0106 (15)
O160.0309 (19)0.0135 (18)0.0235 (18)−0.0071 (14)0.0189 (16)−0.0049 (14)
O170.037 (2)0.0175 (19)0.0171 (18)0.0001 (15)0.0166 (16)0.0003 (15)
O180.0267 (18)0.0165 (19)0.0195 (17)−0.0007 (14)0.0164 (15)−0.0011 (14)
O1W0.0219 (19)0.051 (2)0.028 (2)0.0068 (16)0.0173 (16)0.0164 (18)
O2W0.035 (2)0.022 (2)0.0256 (19)−0.0047 (16)0.0143 (17)−0.0026 (16)
O3W0.027 (2)0.052 (3)0.039 (2)−0.0224 (17)0.0246 (18)−0.0308 (19)
O5W0.117 (5)0.100 (5)0.255 (10)0.012 (4)0.142 (6)0.041 (6)
O4WA0.103 (11)0.045 (7)0.053 (7)−0.036 (7)0.064 (8)−0.019 (5)
O4WB0.090 (9)0.075 (8)0.056 (6)−0.033 (7)0.047 (6)0.005 (5)
C1—O21.245 (5)La1—O2W2.563 (3)
C1—O11.266 (5)La1—O92.679 (3)
C1—C21.525 (6)La1—O32.698 (3)
C2—O31.424 (5)La2—O52.478 (3)
C2—C31.524 (6)La2—O14ii2.488 (3)
C2—H20.9800La2—O17iii2.496 (3)
C3—O41.427 (5)La2—O3W2.505 (3)
C3—C41.531 (6)La2—O11iii2.529 (3)
C3—H30.9800La2—O42.569 (3)
C4—O61.241 (5)La2—O12iv2.606 (3)
C4—O51.269 (5)La2—O16iii2.641 (3)
C5—O81.249 (5)La2—O10iii2.730 (3)
C5—O71.265 (5)O3—H3A0.8187
C5—C61.527 (6)O4—H40.8211
C6—O91.430 (5)O6—La1v2.534 (3)
C6—C71.547 (6)O9—H90.8167
C6—H60.9800O10—La2vi2.730 (3)
C7—O101.420 (5)O10—H10A0.8180
C7—C81.543 (6)O11—La2vi2.529 (3)
C7—H70.9800O12—La2vii2.606 (3)
C8—O111.258 (5)O14—La2viii2.488 (3)
C8—O121.260 (5)O15—H150.8188
C9—O141.249 (5)O16—La2vi2.641 (3)
C9—O131.268 (5)O16—H160.8184
C9—C101.516 (6)O17—La2vi2.496 (3)
C10—O151.426 (5)O1W—H1W0.8167
C10—C111.520 (6)O1W—H2W0.8174
C10—H100.9800O2W—H4W0.8180
C11—O161.429 (5)O2W—H3W0.8220
C11—C121.523 (6)O3W—H6W0.8155
C11—H110.9800O3W—H5W0.8177
C12—O171.241 (5)O5W—H10W0.8468
C12—O181.265 (5)O5W—H9W0.8478
La1—O72.458 (3)O4WA—H4WA0.8498
La1—O12.476 (3)O4WA—H4WB0.8499
La1—O1W2.505 (3)O4WA—H4WD0.7409
La1—O132.519 (3)O4WB—H4WC0.8505
La1—O6i2.534 (3)O4WB—H4WD0.8503
La1—O152.537 (3)
O2—C1—O1122.7 (4)O1—La1—O359.64 (10)
O2—C1—C2119.5 (4)O1W—La1—O372.73 (10)
O1—C1—C2117.8 (4)O13—La1—O369.61 (10)
O3—C2—C3113.3 (4)O6i—La1—O3129.38 (10)
O3—C2—C1107.7 (4)O15—La1—O3109.80 (10)
C3—C2—C1114.6 (4)O2W—La1—O366.30 (10)
O3—C2—H2106.9O9—La1—O3131.08 (10)
C3—C2—H2106.9O5—La2—O14ii131.51 (10)
C1—C2—H2106.9O5—La2—O17iii75.65 (10)
O4—C3—C2113.9 (4)O14ii—La2—O17iii130.47 (10)
O4—C3—C4107.5 (4)O5—La2—O3W144.32 (11)
C2—C3—C4113.1 (4)O14ii—La2—O3W70.40 (10)
O4—C3—H3107.3O17iii—La2—O3W69.74 (11)
C2—C3—H3107.3O5—La2—O11iii80.05 (10)
C4—C3—H3107.3O14ii—La2—O11iii101.25 (11)
O6—C4—O5124.2 (4)O17iii—La2—O11iii126.38 (10)
O6—C4—C3118.9 (4)O3W—La2—O11iii128.09 (11)
O5—C4—C3116.8 (4)O5—La2—O461.24 (9)
O8—C5—O7124.6 (4)O14ii—La2—O472.79 (10)
O8—C5—C6117.5 (4)O17iii—La2—O4129.34 (10)
O7—C5—C6117.8 (4)O3W—La2—O4140.56 (10)
O9—C6—C5108.5 (4)O11iii—La2—O472.77 (10)
O9—C6—C7111.8 (4)O5—La2—O12iv76.47 (10)
C5—C6—C7115.0 (4)O14ii—La2—O12iv78.72 (10)
O9—C6—H6107.0O17iii—La2—O12iv68.33 (10)
C5—C6—H6107.0O3W—La2—O12iv82.92 (11)
C7—C6—H6107.0O11iii—La2—O12iv147.59 (10)
O10—C7—C8108.0 (3)O4—La2—O12iv76.44 (10)
O10—C7—C6111.6 (4)O5—La2—O16iii76.20 (10)
C8—C7—C6109.6 (3)O14ii—La2—O16iii149.60 (10)
O10—C7—H7109.2O17iii—La2—O16iii60.38 (10)
C8—C7—H7109.2O3W—La2—O16iii93.63 (10)
C6—C7—H7109.2O11iii—La2—O16iii67.75 (10)
O11—C8—O12125.4 (4)O4—La2—O16iii125.67 (9)
O11—C8—C7117.3 (4)O12iv—La2—O16iii126.16 (9)
O12—C8—C7117.2 (4)O5—La2—O10iii136.93 (10)
O14—C9—O13124.9 (4)O14ii—La2—O10iii72.81 (10)
O14—C9—C10117.5 (4)O17iii—La2—O10iii118.40 (10)
O13—C9—C10117.6 (4)O3W—La2—O10iii70.51 (11)
O15—C10—C9109.0 (3)O11iii—La2—O10iii58.50 (9)
O15—C10—C11111.5 (4)O4—La2—O10iii111.26 (10)
C9—C10—C11110.6 (4)O12iv—La2—O10iii146.07 (9)
O15—C10—H10108.6O16iii—La2—O10iii77.54 (10)
C9—C10—H10108.6C1—O1—La1131.0 (3)
C11—C10—H10108.6C2—O3—La1121.9 (3)
O16—C11—C10110.8 (4)C2—O3—H3A103.0
O16—C11—C12108.7 (3)La1—O3—H3A114.7
C10—C11—C12112.6 (4)C3—O4—La2119.8 (2)
O16—C11—H11108.2C3—O4—H4108.6
C10—C11—H11108.2La2—O4—H4121.1
C12—C11—H11108.2C4—O5—La2127.0 (3)
O17—C12—O18125.4 (4)C4—O6—La1v135.2 (3)
O17—C12—C11118.4 (4)C5—O7—La1131.3 (3)
O18—C12—C11116.2 (4)C6—O9—La1121.6 (2)
O7—La1—O178.94 (11)C6—O9—H9104.2
O7—La1—O1W76.88 (11)La1—O9—H9104.9
O1—La1—O1W75.70 (11)C7—O10—La2vi123.3 (2)
O7—La1—O13123.42 (11)C7—O10—H10A108.1
O1—La1—O1376.42 (10)La2vi—O10—H10A126.4
O1W—La1—O13140.85 (11)C8—O11—La2vi131.4 (3)
O7—La1—O6i74.88 (11)C8—O12—La2vii133.4 (3)
O1—La1—O6i145.67 (10)C9—O13—La1126.5 (3)
O1W—La1—O6i77.03 (10)C9—O14—La2viii143.6 (3)
O13—La1—O6i137.11 (10)C10—O15—La1123.8 (2)
O7—La1—O15115.51 (10)C10—O15—H15110.8
O1—La1—O15136.82 (10)La1—O15—H15120.3
O1W—La1—O15145.22 (10)C11—O16—La2vi122.1 (2)
O13—La1—O1561.51 (10)C11—O16—H16105.4
O6i—La1—O1575.61 (10)La2vi—O16—H16126.4
O7—La1—O2W142.04 (11)C12—O17—La2vi128.9 (3)
O1—La1—O2W125.34 (11)La1—O1W—H1W111.2
O1W—La1—O2W81.70 (12)La1—O1W—H2W127.1
O13—La1—O2W92.68 (11)H1W—O1W—H2W105.8
O6i—La1—O2W69.95 (11)La1—O2W—H4W116.7
O15—La1—O2W69.01 (10)La1—O2W—H3W117.0
O7—La1—O960.31 (10)H4W—O2W—H3W104.7
O1—La1—O987.05 (11)La2—O3W—H6W128.7
O1W—La1—O9136.24 (11)La2—O3W—H5W124.9
O13—La1—O968.26 (11)H6W—O3W—H5W105.5
O6i—La1—O998.66 (11)H10W—O5W—H9W105.7
O15—La1—O969.45 (10)H4WA—O4WA—H4WB105.2
O2W—La1—O9138.45 (11)H4WA—O4WA—H4WD106.4
O7—La1—O3133.15 (10)H4WC—O4WB—H4WD105.1
D—H···AD—HH···AD···AD—H···A
O3—H3A···O8iv0.821.872.677 (4)169
O4—H4···O18vii0.821.802.619 (4)174
O9—H9···O160.822.463.177 (5)147
O10—H10A···O8ix0.821.942.745 (4)167
O15—H15···O2iv0.821.822.632 (4)175
O16—H16···O4WA0.821.892.667 (9)158
O16—H16···O4WB0.821.942.708 (9)157
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O3—H3A⋯O8i0.821.872.677 (4)169
O4—H4⋯O18ii0.821.802.619 (4)174
O9—H9⋯O160.822.463.177 (5)147
O10—H10A⋯O8iii0.821.942.745 (4)167
O15—H15⋯O2i0.821.822.632 (4)175
O16—H16⋯O4WA0.821.892.667 (9)158
O16—H16⋯O4WB0.821.942.708 (9)157

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

  3 in total

1.  Reticular synthesis and the design of new materials.

Authors:  Omar M Yaghi; Michael O'Keeffe; Nathan W Ockwig; Hee K Chae; Mohamed Eddaoudi; Jaheon Kim
Journal:  Nature       Date:  2003-06-12       Impact factor: 49.962

2.  A short history of SHELX.

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

Review 3.  Metal-organic frameworks.

Authors:  Stuart L James
Journal:  Chem Soc Rev       Date:  2003-09       Impact factor: 54.564

  3 in total

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