Structural Evolution in a Series of Isomorphous Rare Earth Compounds as Response of Lanthanide Contraction
Abstract
:1. Introduction
2. Materials and Methods
2.1. Preparation
2.2. Spectroscopic Measurement and Elemental Analyses
2.3. Single Crystal X-ray Structure Determinations
3. Results and Discussion
3.1. Unit Cell Volumes and Lattice Parameters
3.2. Alignment of RE in the Coordination Polymer
3.3. RE Coordination
3.4. Coordination Modes of the Acetate Ligands
3.5. Hydrogen Bonds
3.6. Packing
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Ce | Pr | Nd | Pm | Sm | Eu | Gd | Tb | Dy | Ho | Er | Tm | Yb | Lu | |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Empirical formula | C4H23CeClO7 | C4H12ClO7Pr | C4H12ClNdO7 | C4H12ClO7Sm | C4H12ClEuO7 | C4H12ClGdO7 | C4H12ClO7Tb | C4H12ClDyO7 | C4H12ClHoO7 | C4H12ClErO7 | C4H12ClO7Tm | C4H12ClO7Yb | C4H12ClLuO7 | |
Formula weight [g/mol] | 347.71 | 348.50 | 351.83 | 357.94 | 359.55 | 364.84 | 366.51 | 370.09 | 372.52 | 374.85 | 376.52 | 380.63 | 382.56 | |
Temperature [K] | 100(2) | 100(2) | ||||||||||||
Crystal system | monoclinic | Monoclinic | ||||||||||||
Space group | P 21/n | P 21/n | ||||||||||||
a [Å] | 7.9625(3) | 7.9333(3) | 7.9059(3) | 7.8503(3) | 7.8412(2) | 7.8219(4) | 7.8003(2) | 7.8106(4) | 7.7993(3) | 7.7927(3) | 7.7747(2) | 7.7710(3) | 7.7668(3) | |
b [Å] | 7.9276(3) | 7.9139(3) | 7.9008(3) | 7.8844(3) | 7.8769(2) | 7.8592(4) | 7.8539(2) | 7.8433(4) | 7.8345(3) | 7.8301(5) | 7.8392(2) | 7.8224(3) | 7.8297(3) | |
b [Å] | 17.6973(6) | 17.6327(6) | 17.5852(7) | 17.5192(6) | 17.4901(5) | 17.4434(8) | 17.3942(5) | 17.3400(8) | 17.2564(7) | 17.1904(7) | 17.1517(5) | 17.1055(8) | 17.0618(7) | |
β | 99.122(2)° | 98.947 | 98.856(2) | 98.483(2) | 98.354(1)° | 98.265(2) | 98.075(2)° | 97.978(2)° | 97.881(2)° | 97.695(2) | 97.552(1) | 97.422(2) | 97.336(2) | |
Volume [Å3] | 1102.99(7) | 1093.57(7) | 1085.33(7) | 1072.49(7) | 1068.80(5) | 1061.18(9) | 1055.05(5) | 1051.98(9) | 1044.47(7) | 1039.47(7) | 1036.28(5) | 1031.09(7) | 1029.06(7) | |
Z,Z′,dcalc [g/mol] | 4, 1, 2.094 | 4, 1, 2.117 | 4, 1, 2.153 | 4, 1, 2.217 | 4, 1, 2.234 | 4, 1, 2.284 | 4, 1, 2.307 | 4, 1, 2.337 | 4, 1, 2.369 | 4, 1, 2.395 | 4, 1, 2.413 | 4, 1, 2.452 | 4, 1, 2.469 | |
μ [mm−1] | 4.373 | 4.703 | 5.034 | 5.728 | 6.122 | 6.509 | 6.960 | 7.361 | 7.835 | 8.335 | 8.823 | 9.333 | 9.857 | |
F(000) | 668 | 672 | 676 | 684 | 688 | 692 | 696 | 700 | 704 | 708 | 712 | 716 | 720 | |
2Ѳmax | 56° | 56° | ||||||||||||
Reflections collected | 101277 | 125986 | 122829 | 130814 | 79828 | 122742 | 126109 | 49237 | 133421 | 93.617 | 108715 | 70583 | 100183 | |
Reflections unique, Rint | 2664, 0.0460 | 2645, 0.0398 | 2621, 0.0566 | 2595, 0.0344 | 2587, 0.0399 | 2569, 0.0358 | 2551, 0.0517 | 2547, 0.0328 | 2528, 0.0358 | 2514, 0.0305 | 2504, 0.0397 | 2491, 0.0721 | 2490, 0.0653 | |
Data/restraints/parameters | 2664/0/125 | 2645/0/125 | 2621/0/125 | 2595/0/126 | 2587/0/125 | 2569/0/126 | 2551/0/125 | 2547/0/126 | 2528/0/126 | 2514/0/126 | 2504/0/125 | 2491/0/125 | 2490/0/125 | |
Goodness of fito n F2 | 1.224 | 1.101 | 1.062 | 1.133 | 1.094 | 1.090 | 1.054 | 1.184 | 1.176 | 1.409 | 1.132 | 1.061 | 1.034 | |
R1/wR2 [I > 2σ(I)] | 0.0177, 0.0355 | 0.0125, 0.0280 | 0.0122, 0.0270 | 0.0101, 0.0233 | 0.0131, 0.0327 | 0.0094, 0.0206 | 0.0108, 0.0245 | 0.0127, 0.0266 | 0.0103, 0.0234 | 0.0135, 0.0292 | 0.0108, 0.0240 | 0.0162, 0.0302 | 0.0119, 0.0264 | |
R1/wR2 [all data] | 0.0186, 0.0358 | 0.0134, 0.0283 | 0.0142, 0.0275 | 0.0105, 0.0235 | 0.0137, 0.0330 | 0.0100, 0.0208 | 0.0131, 0.0253 | 0.0131, 0.0267 | 0.0106, 0.0235 | 0.0135, 0.0292 | 0.0113, 0.0241 | 0.0217, 0.0318 | 0.0143, 0.0269 | |
Extinction coefficient | N/A | 0.00104(8) | N/A | 0.00122(7) | N/A | 0.0045(1) | 0.00185(8) | 0.00115(9) | N/A | |||||
±∆e[eÅ−3] | 0.532/−0.811 | 0.457/−0.609 | 0.387/−0.358 | 0.381/−0.528 | 0.470/−0.703 | 0.348/−0.474 | 0.486/−0.392 | 0.489/−0.652 | 0.364/−0.436 | 0.524/−0.603 | 0.386/−0.579 | 0.522/−0.480 | 0.365/−0.421 | |
CCDC number | 2260824 | 2260831 | 2260827 | 2260830 | 2260822 | 2260828 | 2260829 | 2260820 | 2260832 | 2260823 | 2260825 | 2260821 | 2206826 |
Ce | Pr | Nd | Pm | Sm | Eu | Gd | Tb | Dy | Ho | Er | Tm | Yb | Lu | |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Empirical formula | C4H23BrCeO7 | C4H12BrO7Pr | C4H12BrNdO7 | C4H12BrO7Sm | C4H12BrEuO7 | C4H12BrGdO7 | C4H12BrO7Tb | C4H12BrDyO7 | C4H12BrHoO7 | C4H12BrErO7 | C4H12BrO7Tm | C4H12BrO7Yb | C4H12BrLuO7 | |
Formula weight [g/mol] | 392.17 | 392.96 | 396.29 | 402.40 | 404.01 | 409.30 | 410.97 | 414.55 | 416.98 | 419.31 | 420.98 | 425.09 | 427.02 | |
Temperature [K] | 100(2) | 100(2) | ||||||||||||
Crystal system | monoclinic | Monoclinic | ||||||||||||
Space group | P 21/n | P 21/n | ||||||||||||
a [Å] | 7.9597(3) | 7.9293(3) | 7.9027(3) | 7.8473(3) | 7.8318(3) | 7.8191(2) | 7.7972(3) | 7.8038(3) | 7.8117(3) | 7.8069(3) | 7.7868(5) | 7.7854(3) | 7.7611(3) | |
b [Å] | 8.0442(3) | 8.0327(3) | 8.0349(3) | 8.0230(3) | 8.0121(3) | 8.0130(2) | 8.0263(3) | 8.0288(3) | 8.0361(4) | 8.0529(3) | 8.0675(5) | 8.0625(3) | 8.0702(3) | |
b [Å] | 18.0642(8) | 18.0186(6) | 17.9481(6) | 17.8722(7) | 17.8214(7) | 17.7804(6) | 17.7443(8) | 17.6550(7) | 17.5440(9) | 17.4494(7) | 17.3994(7) | 17.3573(7) | 17.2952(6) | |
β | 96.732(2)° | 96.533(2)° | 96.414(2)° | ° | 95.987(2)° | 95.972(2)° | 95.929(2)° | 95.862(2)° | 96.034(2)° | 96.096(3)° | 96.154(2)° | 96.154(2)° | 96.142(29)° | 96.098(2)° |
Volume [Å3] | 1148.67(8) | 1140.22(7) | 1132.52(7) | 1119.08(7) | 1112.21(7) | 1108.06(5) | 1104.68(8) | 1100.05(7) | 1095.11(9) | 1090.69(7) | 1086.73(11) | 1083.26(7) | 1077.13(7) | |
Z,Z′,dcalc [g/mol] | 4, 1, 2.268 | 4, 1, 2.289 | 4, 1, 2.324 | 4, 1, 2.388 | 4, 1, 2.413 | 4, 1, 2.453 | 4, 1, 2.471 | 4, 1, 2.503 | 4, 1, 2.529 | 4, 1, 2.544 | 4, 1, 2.573 | 4, 1, 2.606 | 4, 1, 2.633 | |
μ [mm−1] | 7.446 | 7.781 | 8.117 | 8.822 | 9.236 | 9.595 | 10.023 | 10.429 | 10.878 | 11.362 | 11.845 | 12.326 | 12.879 | |
F(000) | 740 | 744 | 748 | 756 | 760 | 764 | 768 | 772 | 776 | 780 | 784 | 788 | 792 | |
2Ѳmax | 56° | 56° | ||||||||||||
Reflections collected | 113305 | 92529 | 132337 | 1113760 | 118192 | 132199 | 124829 | 101683 | 102663 | 121.468 | 112602 | 120213 | 103545 | |
Reflections unique, Rint | 2770, 0.0572 | 2753, 0.0497 | 2735, 0.0553 | 2708, 0.0701 | 2696, 0.0516 | 2690, 0.0410 | 2683, 0.0459 | 2666, 0.0444 | 2655, 0.0734 | 2636, 0.0413 | 2626, 0.0488 | 2616, 0.0460 | 2596, 0.0753 | |
Data/restraints/parameters | 2770/0/125 | 2753/0/125 | 2735/0/125 | 2708/0/125 | 2696/0/125 | 2690/0/125 | 2683/0/125 | 2666/0/126 | 2655/0/125 | 2636/0/126 | 2626/0/125 | 2616/0/125 | 2596/0/125 | |
Goodness of fito n F2 | 1.071 | 1.078 | 1.051 | 1.084 | 1.100 | 1.134 | 1.122 | 1.118 | 1.049 | 1.182 | 1.083 | 1.073 | 1.054 | |
R1/wR2 [I>2σ(I)] | 0.0142, 0.0310 | 0.0141, 0.0295 | 0.0129, 0.0300 | 0.0150, 0.0305 | 0.0131, 0.0300 | 0.0155, 0.0403 | 0.0133, 0.0301 | 0.0129, 0.0321 | 0.148, 0.0336 | 0.0114, 0.0253 | 0.0118, 0.0265 | 0.0121, 0.0261 | 0.0184, 0.0417 | |
R1/wR2 [all data] | 0.0173, 0.0321 | 0.0175, 0.0305 | 0.0154, 0.0307 | 0.0201, 0.0321 | 0.0157, 0.0309 | 0.0168, 0.0410 | 0.0151, 0.0306 | 0.0140, 0.0325 | 0.196, 0.0353 | 0.0123, 0.0255 | 0.0141, 0.0272 | 0.0141, 0.0266 | 0.0233, 0.0437 | |
Extinction coefficient | N/A | N/A | 0.00126(9) | N/A | 0.00082(5) | N/A | ||||||||
±∆e[eÅ−3] | 0.368/−0.374 | 0.441/−0.499 | 0.402/−0.415 | 0.442/−0.443 | 0.408/−0.408 | 0.695/−0.977 | 0.554/−0.407 | 0.779/−0.601 | 0.508/−0.579 | 0.364/−0.467 | 0.383/−0.226 | 0.4607/−0.581 | 1.131/−1.209 | |
CCDC number | 2261207 | 2261199 | 2261203 | 2261208 | 2261206 | 2261205 | 2261209 | 2261200 | 2261198 | 2261201 | 2261202 | 2261204 | 2261210 |
RE | Ce | Pr | Nd | Pm | Sm | Eu | Gd | Tb | Dy | Ho | Er | Tm | Yb | Lu |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Hal = Cl | ||||||||||||||
RE(1)-O(11) | 2.422(2) | 2.404(1) | 2.390(1) | 2.351(1) | 2.341(1) | 2.325(1) | 2.294(1) | 2.274(1) | 2.252(1) | 2.232(2) | 2.218(1) | 2.201(2) | 2.193(1) | |
RE(1)-O(21) | 2.440(2) | 2.422(1) | 2.406(1) | 2.373(1) | 2.362(1) | 2.346(1) | 2.323(1) | 2.312(1) | 2.295(1) | 2.280(2) | 2.265(1) | 2.246(2) | 2.239(1) | |
RE(1)-O(2W) | 2.486(2) | 2.468(1) | 2.452(1) | 2.421(1) | 2.407(1) | 2.393(1) | 2.403(1) | 2.361(2) | 2.345(1) | 2.331(2) | 2.320(1) | 2.312(2) | 2.302(2) | |
RE(1)-O(3W) | 2.499(2) | 2.482(1) | 2.467(1) | 2.438(1) | 2.427(1) | 2.418(1) | 2.403(1) | 2.392(1) | 2.381(1) | 2.372(2) | 2.360(1) | 2.347(2) | 2.346(2) | |
RE(1)-O(1W) | 2.524(2) | 2.506(1) | 2.487(1) | 2.457(1) | 2.444(1) | 2.425(1) | 2.404(1) | 2.388(1) | 2.367(1) | 2.346(2) | 2.339(1) | 2.320(2) | 2.309(2) | |
RE(1)-O(12) 1 | 2.536(2) | 2.516(1) | 2.498(1) | 2.462(1) | 2.450(1) | 2.436(1) | 2.413(1) | 2.396(2) | 2.378(1) | 2.362(2) | 2.346(1) | 2.334(2) | 2.327(2) | |
RE(1)-O(22) 2 | 2.548(2) | 2.529(1) | 2.510(1) | 2.475(1) | 2.462(1) | 2.449(1) | 2.428(1) | 2.416(1) | 2.400(1) | 2.386(2) | 2.373(1) | 2.359(2) | 2.358(2) | |
RE(1)-O(21) 2 | 2.665(2) | 2.648(1) | 2.633(1) | 2.620(1) | 2.613(1) | 2.607(1) | 2.612(1) | 2.604(1) | 2.596(1) | 2.588(2) | 2.592(1) | 2.601(2) | 2.585(2) | |
RE(1)-O(11) 1 | 2.738(2) | 2.725(1) | 2.706(1) | 2.723(1) | 2.728(1) | 2.740(1) | 2.820(1) | 2.905(2) | 2.991(1) | 3.083(2) | 3.128(2) | 3.178(2) | 3.211(2) | |
Hal = Br | ||||||||||||||
RE(1)-O(11) | 2.417(1) | 2.401(1) | 2.388(1) | 2.349(2) | 2.338(1) | 2.324(2) | 2.294(2) | 2.269(1) | 2.248(2) | 2.229(1) | 2.216(2) | 2.201(2) | 2.188(2) | |
RE(1)-O(21) | 2.431(1) | 2.416(1) | 2.403(1) | 2.370(2) | 2.356(1) | 2.343(2) | 2.322(1) | 2.307(1) | 2.294(2) | 2.280(1) | 2.266(1) | 2.251(1) | 2.238(2) | |
RE(1)-O(2W) | 2.489(1) | 2.471(1) | 2.457(1) | 2.425(2) | 2.409(2) | 2.398(2) | 2.381(2) | 2.365(1) | 2.346(2) | 2.338(1) | 2.325(2) | 2.316(2) | 2.305(2) | |
RE(1)-O(3W) | 2.490(2) | 2.476(1) | 2.461(1) | 2.431(2) | 2.420(2) | 2.412(2) | 2.398(2) | 2.386(2) | 2.366(2) | 2.347(2) | 2.353(2) | 2.344(2) | 2.338(2) | |
RE(1)-O(1W) | 2.526(1) | 2.504(1) | 2.490(1) | 2.459(2) | 2.442(2) | 2.426(2) | 2.405(2) | 2.389(1) | 2.373(2) | 2.360(2) | 2.336(2) | 2.322(2) | 2.306(2) | |
RE(1)-O(12) 1 | 2.536(1) | 2.516(2) | 2.499(1) | 2.466(2) | 2.450(2) | 2.439(2) | 2.417(2) | 2.395(2) | 2.376(2) | 2.365(2) | 2.342(2) | 2.333(3) | 2.323(2) | |
RE(1)-O(22) 2 | 2.539(1) | 2.527(1) | 2.504(1) | 2.471(2) | 2.459(2) | 2.447(2) | 2.429(2) | 2.412(2) | 2.395(2) | 2.382(1) | 2.368(2) | 2.358(2) | 2.350(2) | |
RE(1)-O(21) 2 | 2.666(1) | 2.652(1) | 2.632(1) | 2.623(2) | 2.615(1) | 2.608(2) | 2.612(2) | 2.603(1) | 2.591(2) | 2.582(1) | 2.587(2) | 2.594(2) | 2.577(2) | |
RE(1)-O(11) 1 | 2.746(1) | 2.730(1) | 2.711(1) | 2.722(2) | 2.720(2) | 2.733(2) | 2.808(2) | 2.917(2) | 3.026(2) | 3.129(2) | 3.165(2) | 3.213(2) | 3.238(2) |
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Reuter, H.; Böltken, M.; Horstmann, M.; Haase, M. Structural Evolution in a Series of Isomorphous Rare Earth Compounds as Response of Lanthanide Contraction. Crystals 2023, 13, 1043. https://doi.org/10.3390/cryst13071043
Reuter H, Böltken M, Horstmann M, Haase M. Structural Evolution in a Series of Isomorphous Rare Earth Compounds as Response of Lanthanide Contraction. Crystals. 2023; 13(7):1043. https://doi.org/10.3390/cryst13071043
Chicago/Turabian StyleReuter, Hans, Marcel Böltken, Maik Horstmann, and Markus Haase. 2023. "Structural Evolution in a Series of Isomorphous Rare Earth Compounds as Response of Lanthanide Contraction" Crystals 13, no. 7: 1043. https://doi.org/10.3390/cryst13071043