metal-organic compounds
Poly[diaquatris(μ4-1,3-phenylenediacetato)dineodymium(III)]
aSchool of Chemistry and Biology Engineering, Taiyuan University of Science and Technology, Taiyuan 030021, People's Republic of China, and bKey Laboratory of Nonferrous Metal Chemistry and Resources Utilization of Gansu Province, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000, People's Republic of China
*Correspondence e-mail: zqgao2008@163.com
In the title coordination polymer, [Nd2(C10H8O4)3(H2O)2]n, each of the two NdIII ions is nine-coordinated by eight O atoms from six different 2,2′-(m-phenylene)diacetate (pda) bivalent anions and by one O atom from a water molecule, forming a distorted tricapped trigonal–prismatic coordination geometry. Eight NdIII ions and 12 pda ligands form a large [Nd8(pda)12] ring, and four NdIII ions and six pda ligands form a small [Nd4(pda)6] ring. These rings are further connected by the coordination interactions of pda ligands and NdIII, generating a three-dimensional supramolecular framework.
Related literature
For the isotypic Ce analogue, see: Gao et al. (2011). For the structures and properties of lanthanide coordination compounds, see: Xiao et al. (2008); Lv et al. (2010). For bond lengths and angles in other complexes with nine-coordinate NdIII, see: Xiao et al. (2008); Wang et al. (2009).
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 1997); cell SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
10.1107/S1600536811006817/wm2461sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536811006817/wm2461Isup2.hkl
To a solution of neodymium nitrate hexahydrate (0.088 g, 0.2 mmol) in water (5 ml) was added an aqueous solution (5 ml) of the ligand (0.058 g, 0.3 mmol) and a drop of triethylamine. The reactants were sealed in a 25-ml Teflon-lined stainless-steel Parr bomb. The bomb was heated at 433 K for 3 d. Upon cooling, the solution yielded single crystals of the title complex in ca 75% yield. Anal./calc. for C30H28Nd2O14: C, 39.99; H, 3.13; found: C, 40.43; H, 3.47.
The H atoms of the water molecules were located in a difference Fourier map and were refined with distance constraints of O–H = 0.83 (5) Å. The C-bound H atoms were placed in geometrically idealized positions, with C–H = 0.93 and 0.97 Å for aryl and methylene H-atoms, respectively, and constrained to ride on their respective parent atoms, with Uiso(H) = 1.2 Ueq(C).
Data collection: SMART (Bruker, 1997); cell
SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).[Nd2(C10H8O4)3(H2O)2] | Z = 2 |
Mr = 901.00 | F(000) = 880 |
Triclinic, P1 | Dx = 2.028 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.4846 (13) Å | Cell parameters from 5315 reflections |
b = 11.9660 (16) Å | θ = 1.7–25.3° |
c = 12.3514 (16) Å | µ = 3.55 mm−1 |
α = 105.619 (5)° | T = 296 K |
β = 97.202 (5)° | Block, colorless |
γ = 92.625 (6)° | 0.24 × 0.22 × 0.20 mm |
V = 1475.5 (3) Å3 |
Bruker SMART CCD diffractometer | 5315 independent reflections |
Radiation source: fine-focus sealed tube | 4806 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.013 |
Detector resolution: 0 pixels mm-1 | θmax = 25.3°, θmin = 1.7° |
ϕ and ω scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | k = −12→14 |
Tmin = 0.516, Tmax = 0.580 | l = −14→14 |
7865 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0265P)2 + 1.487P] where P = (Fo2 + 2Fc2)/3 |
5315 reflections | (Δ/σ)max = 0.001 |
415 parameters | Δρmax = 0.64 e Å−3 |
3 restraints | Δρmin = −0.76 e Å−3 |
[Nd2(C10H8O4)3(H2O)2] | γ = 92.625 (6)° |
Mr = 901.00 | V = 1475.5 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.4846 (13) Å | Mo Kα radiation |
b = 11.9660 (16) Å | µ = 3.55 mm−1 |
c = 12.3514 (16) Å | T = 296 K |
α = 105.619 (5)° | 0.24 × 0.22 × 0.20 mm |
β = 97.202 (5)° |
Bruker SMART CCD diffractometer | 5315 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | 4806 reflections with I > 2σ(I) |
Tmin = 0.516, Tmax = 0.580 | Rint = 0.013 |
7865 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 3 restraints |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.64 e Å−3 |
5315 reflections | Δρmin = −0.76 e Å−3 |
415 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Nd1 | 0.029517 (16) | 0.026539 (14) | 0.183517 (13) | 0.01602 (6) | |
Nd2 | 0.306439 (16) | 0.036922 (15) | 0.455279 (14) | 0.01818 (6) | |
C1 | 0.0706 (3) | 0.8190 (3) | 0.2608 (3) | 0.0194 (7) | |
C2 | 0.1023 (4) | 0.7042 (3) | 0.2819 (3) | 0.0314 (9) | |
H2A | 0.1766 | 0.6787 | 0.2453 | 0.038* | |
H2B | 0.1270 | 0.7169 | 0.3629 | 0.038* | |
C3 | −0.0041 (4) | 0.6073 (3) | 0.2411 (3) | 0.0244 (8) | |
C4 | −0.1173 (4) | 0.6146 (3) | 0.2887 (3) | 0.0340 (9) | |
H4 | −0.1275 | 0.6802 | 0.3468 | 0.041* | |
C5 | −0.2149 (4) | 0.5267 (3) | 0.2516 (4) | 0.0368 (9) | |
H5 | −0.2897 | 0.5324 | 0.2853 | 0.044* | |
C6 | −0.2021 (4) | 0.4299 (3) | 0.1643 (3) | 0.0330 (9) | |
H6 | −0.2691 | 0.3714 | 0.1383 | 0.040* | |
C7 | −0.0910 (4) | 0.4192 (3) | 0.1154 (3) | 0.0265 (8) | |
C8 | 0.0082 (4) | 0.5078 (3) | 0.1549 (3) | 0.0252 (8) | |
H8 | 0.0843 | 0.5002 | 0.1230 | 0.030* | |
C9 | −0.0755 (4) | 0.3102 (3) | 0.0240 (3) | 0.0326 (9) | |
H9A | −0.1557 | 0.2884 | −0.0279 | 0.039* | |
H9B | −0.0092 | 0.3272 | −0.0188 | 0.039* | |
C10 | −0.0404 (3) | 0.2088 (3) | 0.0679 (3) | 0.0220 (7) | |
C11 | −0.2153 (3) | 0.7492 (3) | 0.5878 (3) | 0.0243 (7) | |
C12 | −0.1546 (4) | 0.6428 (3) | 0.6052 (4) | 0.0475 (12) | |
H12A | −0.0771 | 0.6353 | 0.5692 | 0.057* | |
H12B | −0.1280 | 0.6558 | 0.6860 | 0.057* | |
C13 | −0.2359 (4) | 0.5289 (3) | 0.5614 (3) | 0.0322 (9) | |
C14 | −0.3482 (4) | 0.5093 (3) | 0.6035 (3) | 0.0393 (10) | |
H14 | −0.3755 | 0.5681 | 0.6597 | 0.047* | |
C15 | −0.4198 (4) | 0.4044 (3) | 0.5636 (3) | 0.0334 (9) | |
H15 | −0.4955 | 0.3927 | 0.5924 | 0.040* | |
C16 | −0.3801 (3) | 0.3155 (3) | 0.4805 (3) | 0.0280 (8) | |
H16 | −0.4301 | 0.2449 | 0.4526 | 0.034* | |
C17 | −0.2661 (3) | 0.3315 (3) | 0.4388 (3) | 0.0232 (7) | |
C18 | −0.1952 (3) | 0.4387 (3) | 0.4794 (3) | 0.0258 (8) | |
H18 | −0.1190 | 0.4506 | 0.4512 | 0.031* | |
C19 | −0.2165 (3) | 0.2365 (3) | 0.3508 (3) | 0.0257 (8) | |
H19A | −0.1419 | 0.2690 | 0.3271 | 0.031* | |
H19B | −0.2825 | 0.2110 | 0.2848 | 0.031* | |
C20 | −0.1792 (3) | 0.1314 (3) | 0.3893 (3) | 0.0194 (7) | |
C21 | 0.4696 (3) | 0.1360 (3) | −0.3232 (3) | 0.0249 (8) | |
C22 | 0.5520 (3) | 0.2052 (3) | −0.2133 (3) | 0.0289 (8) | |
H22A | 0.6237 | 0.1609 | −0.1973 | 0.035* | |
H22B | 0.5873 | 0.2772 | −0.2238 | 0.035* | |
C23 | 0.4804 (3) | 0.2339 (3) | −0.1121 (3) | 0.0272 (8) | |
C24 | 0.3884 (5) | 0.3138 (4) | −0.1054 (4) | 0.0496 (12) | |
H24 | 0.3733 | 0.3507 | −0.1626 | 0.060* | |
H1W | −0.2406 | 0.0218 | 0.0635 | 0.060* | |
H2W | −0.2406 | −0.0802 | 0.1125 | 0.060* | |
H4W | 0.1094 | 0.0990 | 0.6110 | 0.060* | |
H3W | 0.0294 | 0.0896 | 0.5035 | 0.060* | |
C25 | 0.3193 (5) | 0.3397 (4) | −0.0164 (4) | 0.0574 (14) | |
H25 | 0.2561 | 0.3919 | −0.0146 | 0.069* | |
C26 | 0.3432 (4) | 0.2885 (4) | 0.0707 (3) | 0.0409 (10) | |
H26 | 0.2972 | 0.3075 | 0.1319 | 0.049* | |
C27 | 0.4349 (3) | 0.2093 (3) | 0.0676 (3) | 0.0270 (8) | |
C28 | 0.5025 (3) | 0.1825 (3) | −0.0248 (3) | 0.0261 (8) | |
H28 | 0.5641 | 0.1286 | −0.0278 | 0.031* | |
C29 | 0.4652 (4) | 0.1561 (4) | 0.1644 (3) | 0.0348 (9) | |
H29A | 0.5015 | 0.2183 | 0.2310 | 0.042* | |
H29B | 0.5324 | 0.1040 | 0.1459 | 0.042* | |
C30 | 0.3579 (3) | 0.0892 (3) | 0.1978 (3) | 0.0242 (7) | |
O1 | 0.1566 (2) | 0.9053 (2) | 0.2968 (2) | 0.0274 (5) | |
O2 | −0.0342 (2) | 0.8302 (2) | 0.2080 (2) | 0.0284 (6) | |
O3 | −0.0371 (3) | 0.10987 (19) | −0.0009 (2) | 0.0300 (6) | |
O4 | −0.0146 (3) | 0.2218 (2) | 0.1716 (2) | 0.0346 (6) | |
O5 | −0.1595 (2) | 0.84733 (19) | 0.64899 (19) | 0.0252 (5) | |
O6 | −0.3093 (2) | 0.7452 (2) | 0.5148 (2) | 0.0312 (6) | |
O7 | −0.0998 (2) | 0.0686 (2) | 0.3388 (2) | 0.0274 (5) | |
O8 | −0.2271 (3) | 0.1114 (2) | 0.4695 (2) | 0.0365 (6) | |
O9 | 0.5273 (2) | 0.1006 (2) | −0.41110 (18) | 0.0243 (5) | |
O10 | 0.3524 (3) | 0.1179 (3) | −0.3299 (2) | 0.0445 (7) | |
O11 | 0.3881 (2) | 0.0619 (2) | 0.2879 (2) | 0.0300 (6) | |
O12 | 0.2492 (2) | 0.0633 (2) | 0.1359 (2) | 0.0308 (6) | |
O13 | −0.2057 (2) | −0.0221 (2) | 0.1036 (2) | 0.0355 (6) | |
O14 | 0.1067 (2) | 0.1022 (2) | 0.5416 (2) | 0.0334 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.02272 (10) | 0.01120 (9) | 0.01384 (9) | 0.00192 (7) | 0.00258 (7) | 0.00292 (7) |
Nd2 | 0.02183 (10) | 0.01863 (10) | 0.01494 (10) | 0.00167 (7) | 0.00283 (7) | 0.00602 (7) |
C1 | 0.0306 (18) | 0.0139 (16) | 0.0136 (15) | 0.0028 (14) | 0.0065 (14) | 0.0017 (13) |
C2 | 0.043 (2) | 0.0156 (18) | 0.037 (2) | 0.0046 (15) | −0.0013 (17) | 0.0105 (16) |
C3 | 0.038 (2) | 0.0119 (16) | 0.0242 (18) | 0.0036 (14) | 0.0010 (15) | 0.0084 (14) |
C4 | 0.060 (3) | 0.0161 (18) | 0.029 (2) | 0.0100 (17) | 0.0159 (19) | 0.0066 (15) |
C5 | 0.044 (2) | 0.030 (2) | 0.046 (2) | 0.0107 (18) | 0.0183 (19) | 0.0189 (19) |
C6 | 0.041 (2) | 0.0188 (19) | 0.040 (2) | −0.0011 (16) | −0.0013 (18) | 0.0131 (17) |
C7 | 0.045 (2) | 0.0113 (17) | 0.0229 (18) | 0.0071 (15) | −0.0007 (16) | 0.0063 (14) |
C8 | 0.037 (2) | 0.0177 (17) | 0.0242 (17) | 0.0095 (15) | 0.0074 (15) | 0.0093 (14) |
C9 | 0.057 (3) | 0.0178 (18) | 0.0218 (18) | 0.0051 (17) | 0.0011 (17) | 0.0055 (15) |
C10 | 0.0297 (18) | 0.0129 (17) | 0.0227 (18) | 0.0016 (13) | 0.0054 (14) | 0.0032 (14) |
C11 | 0.0265 (18) | 0.0175 (18) | 0.0254 (18) | −0.0028 (14) | 0.0044 (15) | 0.0005 (14) |
C12 | 0.039 (2) | 0.016 (2) | 0.073 (3) | 0.0030 (17) | −0.018 (2) | −0.0002 (19) |
C13 | 0.034 (2) | 0.0155 (18) | 0.041 (2) | 0.0040 (15) | −0.0102 (17) | 0.0048 (16) |
C14 | 0.048 (3) | 0.029 (2) | 0.036 (2) | 0.0154 (19) | 0.0028 (19) | −0.0006 (17) |
C15 | 0.032 (2) | 0.030 (2) | 0.039 (2) | 0.0066 (16) | 0.0131 (17) | 0.0079 (17) |
C16 | 0.0314 (19) | 0.0191 (18) | 0.033 (2) | 0.0000 (15) | 0.0033 (16) | 0.0077 (15) |
C17 | 0.0307 (19) | 0.0192 (17) | 0.0210 (17) | 0.0042 (14) | 0.0007 (14) | 0.0087 (14) |
C18 | 0.0224 (17) | 0.0199 (18) | 0.035 (2) | 0.0017 (14) | −0.0010 (15) | 0.0103 (15) |
C19 | 0.0315 (19) | 0.0219 (18) | 0.0252 (18) | 0.0034 (15) | 0.0049 (15) | 0.0082 (15) |
C20 | 0.0236 (17) | 0.0151 (16) | 0.0167 (16) | −0.0015 (13) | 0.0018 (13) | 0.0007 (13) |
C21 | 0.0294 (19) | 0.030 (2) | 0.0158 (17) | 0.0037 (15) | 0.0031 (14) | 0.0064 (15) |
C22 | 0.0305 (19) | 0.035 (2) | 0.0192 (18) | 0.0000 (16) | 0.0027 (15) | 0.0038 (16) |
C23 | 0.033 (2) | 0.030 (2) | 0.0161 (17) | −0.0001 (15) | 0.0021 (15) | 0.0036 (15) |
C24 | 0.069 (3) | 0.055 (3) | 0.039 (2) | 0.029 (2) | 0.026 (2) | 0.026 (2) |
C25 | 0.077 (3) | 0.063 (3) | 0.050 (3) | 0.043 (3) | 0.037 (3) | 0.027 (2) |
C26 | 0.056 (3) | 0.040 (2) | 0.030 (2) | 0.010 (2) | 0.0212 (19) | 0.0081 (18) |
C27 | 0.0319 (19) | 0.0269 (19) | 0.0227 (18) | −0.0050 (15) | 0.0032 (15) | 0.0094 (15) |
C28 | 0.0246 (18) | 0.0267 (19) | 0.0253 (18) | −0.0011 (14) | 0.0007 (15) | 0.0060 (15) |
C29 | 0.030 (2) | 0.047 (2) | 0.030 (2) | −0.0072 (17) | 0.0004 (16) | 0.0188 (18) |
C30 | 0.0282 (19) | 0.0257 (19) | 0.0193 (17) | 0.0035 (15) | 0.0082 (15) | 0.0046 (15) |
O1 | 0.0361 (14) | 0.0165 (12) | 0.0282 (13) | −0.0012 (10) | −0.0038 (11) | 0.0079 (10) |
O2 | 0.0297 (13) | 0.0205 (13) | 0.0363 (14) | 0.0001 (10) | −0.0006 (11) | 0.0126 (11) |
O3 | 0.0495 (16) | 0.0138 (12) | 0.0258 (13) | 0.0040 (11) | 0.0117 (12) | 0.0010 (10) |
O4 | 0.0642 (19) | 0.0190 (13) | 0.0199 (13) | 0.0106 (12) | −0.0007 (12) | 0.0060 (10) |
O5 | 0.0326 (13) | 0.0158 (12) | 0.0228 (12) | 0.0005 (10) | −0.0011 (10) | 0.0001 (10) |
O6 | 0.0322 (14) | 0.0198 (13) | 0.0356 (14) | −0.0023 (10) | −0.0064 (12) | 0.0035 (11) |
O7 | 0.0340 (14) | 0.0250 (13) | 0.0264 (13) | 0.0103 (11) | 0.0121 (11) | 0.0080 (11) |
O8 | 0.0593 (18) | 0.0261 (14) | 0.0353 (15) | 0.0142 (13) | 0.0287 (14) | 0.0160 (12) |
O9 | 0.0316 (13) | 0.0260 (13) | 0.0162 (11) | 0.0074 (10) | 0.0064 (10) | 0.0050 (10) |
O10 | 0.0263 (15) | 0.073 (2) | 0.0265 (14) | −0.0010 (14) | 0.0021 (12) | 0.0016 (14) |
O11 | 0.0310 (14) | 0.0403 (15) | 0.0247 (13) | 0.0063 (11) | 0.0083 (11) | 0.0165 (12) |
O12 | 0.0262 (13) | 0.0424 (16) | 0.0236 (13) | −0.0044 (11) | 0.0031 (11) | 0.0100 (12) |
O13 | 0.0298 (14) | 0.0386 (16) | 0.0362 (15) | −0.0043 (12) | −0.0032 (12) | 0.0119 (12) |
O14 | 0.0334 (14) | 0.0384 (16) | 0.0316 (14) | 0.0090 (12) | 0.0078 (11) | 0.0129 (12) |
Nd1—O3i | 2.415 (2) | C15—C16 | 1.384 (5) |
Nd1—O5ii | 2.416 (2) | C15—H15 | 0.9300 |
Nd1—O4 | 2.441 (2) | C16—C17 | 1.384 (5) |
Nd1—O7 | 2.442 (2) | C16—H16 | 0.9300 |
Nd1—O12 | 2.496 (2) | C17—C18 | 1.387 (5) |
Nd1—O13 | 2.519 (2) | C17—C19 | 1.508 (5) |
Nd1—O2iii | 2.520 (2) | C18—H18 | 0.9300 |
Nd1—O1iii | 2.576 (2) | C19—C20 | 1.510 (5) |
Nd1—O3 | 2.749 (2) | C19—H19A | 0.9700 |
Nd2—O8iv | 2.377 (2) | C19—H19B | 0.9700 |
Nd2—O11 | 2.418 (2) | C20—O8 | 1.239 (4) |
Nd2—O9v | 2.462 (2) | C20—O7 | 1.257 (4) |
Nd2—O1iii | 2.475 (2) | C21—O10 | 1.227 (4) |
Nd2—O14 | 2.529 (3) | C21—O9 | 1.290 (4) |
Nd2—O6ii | 2.531 (2) | C21—C22 | 1.519 (5) |
Nd2—O10vi | 2.542 (3) | C21—Nd2vii | 2.952 (3) |
Nd2—O5ii | 2.571 (2) | C22—C23 | 1.506 (5) |
Nd2—O9vi | 2.621 (2) | C22—H22A | 0.9700 |
C1—O2 | 1.237 (4) | C22—H22B | 0.9700 |
C1—O1 | 1.282 (4) | C23—C28 | 1.380 (5) |
C1—C2 | 1.510 (4) | C23—C24 | 1.383 (5) |
C2—C3 | 1.506 (5) | C24—C25 | 1.366 (6) |
C2—H2A | 0.9700 | C24—H24 | 0.9300 |
C2—H2B | 0.9700 | C25—C26 | 1.377 (6) |
C3—C4 | 1.385 (5) | C25—H25 | 0.9300 |
C3—C8 | 1.392 (5) | C26—C27 | 1.377 (5) |
C4—C5 | 1.374 (6) | C26—H26 | 0.9300 |
C4—H4 | 0.9300 | C27—C28 | 1.391 (5) |
C5—C6 | 1.378 (5) | C27—C29 | 1.507 (5) |
C5—H5 | 0.9300 | C28—H28 | 0.9300 |
C6—C7 | 1.373 (5) | C29—C30 | 1.512 (5) |
C6—H6 | 0.9300 | C29—H29A | 0.9700 |
C7—C8 | 1.392 (5) | C29—H29B | 0.9700 |
C7—C9 | 1.508 (5) | C30—O11 | 1.251 (4) |
C8—H8 | 0.9300 | C30—O12 | 1.266 (4) |
C9—C10 | 1.499 (5) | O1—Nd2viii | 2.475 (2) |
C9—H9A | 0.9700 | O1—Nd1viii | 2.576 (2) |
C9—H9B | 0.9700 | O2—Nd1viii | 2.520 (2) |
C10—O4 | 1.241 (4) | O3—Nd1i | 2.415 (2) |
C10—O3 | 1.263 (4) | O5—Nd1ii | 2.416 (2) |
C11—O6 | 1.239 (4) | O5—Nd2ii | 2.571 (2) |
C11—O5 | 1.281 (4) | O6—Nd2ii | 2.531 (2) |
C11—C12 | 1.503 (5) | O8—Nd2iv | 2.377 (2) |
C12—C13 | 1.502 (5) | O9—Nd2v | 2.462 (2) |
C12—H12A | 0.9700 | O9—Nd2vii | 2.621 (2) |
C12—H12B | 0.9700 | O10—Nd2vii | 2.542 (3) |
C13—C14 | 1.381 (6) | O13—H1W | 0.8758 |
C13—C18 | 1.391 (5) | O13—H2W | 0.8110 |
C14—C15 | 1.367 (6) | O14—H4W | 0.8644 |
C14—H14 | 0.9300 | O14—H3W | 0.8693 |
O3i—Nd1—O5ii | 144.23 (9) | C7—C9—H9B | 108.7 |
O3i—Nd1—O4 | 113.33 (8) | H9A—C9—H9B | 107.6 |
O5ii—Nd1—O4 | 76.46 (8) | O4—C10—O3 | 119.9 (3) |
O3i—Nd1—O7 | 141.44 (8) | O4—C10—C9 | 120.3 (3) |
O5ii—Nd1—O7 | 71.16 (8) | O3—C10—C9 | 119.9 (3) |
O4—Nd1—O7 | 84.45 (8) | O6—C11—O5 | 120.5 (3) |
O3i—Nd1—O12 | 74.32 (8) | O6—C11—C12 | 123.3 (3) |
O5ii—Nd1—O12 | 71.68 (8) | O5—C11—C12 | 116.0 (3) |
O4—Nd1—O12 | 88.05 (9) | C13—C12—C11 | 117.0 (3) |
O7—Nd1—O12 | 142.83 (8) | C13—C12—H12A | 108.0 |
O3i—Nd1—O13 | 77.43 (9) | C11—C12—H12A | 108.0 |
O5ii—Nd1—O13 | 138.26 (8) | C13—C12—H12B | 108.0 |
O4—Nd1—O13 | 83.71 (9) | C11—C12—H12B | 108.0 |
O7—Nd1—O13 | 70.65 (8) | H12A—C12—H12B | 107.3 |
O12—Nd1—O13 | 144.46 (8) | C14—C13—C18 | 118.6 (3) |
O3i—Nd1—O2iii | 75.03 (8) | C14—C13—C12 | 121.8 (4) |
O5ii—Nd1—O2iii | 112.51 (8) | C18—C13—C12 | 119.6 (4) |
O4—Nd1—O2iii | 153.02 (9) | C15—C14—C13 | 120.8 (4) |
O7—Nd1—O2iii | 75.35 (8) | C15—C14—H14 | 119.6 |
O12—Nd1—O2iii | 118.83 (8) | C13—C14—H14 | 119.6 |
O13—Nd1—O2iii | 72.90 (8) | C14—C15—C16 | 120.4 (4) |
O3i—Nd1—O1iii | 94.43 (8) | C14—C15—H15 | 119.8 |
O5ii—Nd1—O1iii | 69.57 (8) | C16—C15—H15 | 119.8 |
O4—Nd1—O1iii | 146.02 (8) | C15—C16—C17 | 120.1 (3) |
O7—Nd1—O1iii | 85.44 (8) | C15—C16—H16 | 119.9 |
O12—Nd1—O1iii | 80.76 (8) | C17—C16—H16 | 119.9 |
O13—Nd1—O1iii | 122.85 (8) | C16—C17—C18 | 118.8 (3) |
O2iii—Nd1—O1iii | 50.71 (7) | C16—C17—C19 | 122.3 (3) |
O3i—Nd1—O3 | 64.78 (9) | C18—C17—C19 | 118.9 (3) |
O5ii—Nd1—O3 | 119.11 (7) | C17—C18—C13 | 121.2 (3) |
O4—Nd1—O3 | 48.91 (7) | C17—C18—H18 | 119.4 |
O7—Nd1—O3 | 119.10 (8) | C13—C18—H18 | 119.4 |
O12—Nd1—O3 | 80.67 (8) | C17—C19—C20 | 115.1 (3) |
O13—Nd1—O3 | 67.92 (8) | C17—C19—H19A | 108.5 |
O2iii—Nd1—O3 | 128.34 (7) | C20—C19—H19A | 108.5 |
O1iii—Nd1—O3 | 155.25 (8) | C17—C19—H19B | 108.5 |
O8iv—Nd2—O11 | 140.87 (9) | C20—C19—H19B | 108.5 |
O8iv—Nd2—O9v | 80.82 (8) | H19A—C19—H19B | 107.5 |
O11—Nd2—O9v | 72.33 (8) | O8—C20—O7 | 123.0 (3) |
O8iv—Nd2—O1iii | 74.90 (9) | O8—C20—C19 | 118.7 (3) |
O11—Nd2—O1iii | 76.48 (8) | O7—C20—C19 | 118.3 (3) |
O9v—Nd2—O1iii | 88.60 (8) | O10—C21—O9 | 120.9 (3) |
O8iv—Nd2—O14 | 71.83 (9) | O10—C21—C22 | 121.8 (3) |
O11—Nd2—O14 | 131.77 (8) | O9—C21—C22 | 117.3 (3) |
O9v—Nd2—O14 | 152.59 (8) | C23—C22—C21 | 114.1 (3) |
O1iii—Nd2—O14 | 85.98 (8) | C23—C22—H22A | 108.7 |
O8iv—Nd2—O6ii | 140.58 (9) | C21—C22—H22A | 108.7 |
O11—Nd2—O6ii | 77.47 (9) | C23—C22—H22B | 108.7 |
O9v—Nd2—O6ii | 132.09 (8) | C21—C22—H22B | 108.7 |
O1iii—Nd2—O6ii | 119.41 (8) | H22A—C22—H22B | 107.6 |
O14—Nd2—O6ii | 72.89 (9) | C28—C23—C24 | 118.0 (3) |
O8iv—Nd2—O10vi | 73.99 (10) | C28—C23—C22 | 122.3 (3) |
O11—Nd2—O10vi | 139.31 (9) | C24—C23—C22 | 119.7 (3) |
O9v—Nd2—O10vi | 103.61 (8) | C25—C24—C23 | 121.3 (4) |
O1iii—Nd2—O10vi | 144.10 (9) | C25—C24—H24 | 119.4 |
O14—Nd2—O10vi | 67.60 (8) | C23—C24—H24 | 119.4 |
O6ii—Nd2—O10vi | 76.78 (9) | C24—C25—C26 | 120.1 (4) |
O8iv—Nd2—O5ii | 123.39 (9) | C24—C25—H25 | 120.0 |
O11—Nd2—O5ii | 67.91 (8) | C26—C25—H25 | 120.0 |
O9v—Nd2—O5ii | 137.67 (7) | C25—C26—C27 | 120.4 (4) |
O1iii—Nd2—O5ii | 68.79 (7) | C25—C26—H26 | 119.8 |
O14—Nd2—O5ii | 63.87 (8) | C27—C26—H26 | 119.8 |
O6ii—Nd2—O5ii | 50.79 (7) | C26—C27—C28 | 118.7 (3) |
O10vi—Nd2—O5ii | 115.78 (9) | C26—C27—C29 | 120.8 (3) |
O8iv—Nd2—O9vi | 99.49 (9) | C28—C27—C29 | 120.5 (3) |
O11—Nd2—O9vi | 94.98 (8) | C23—C28—C27 | 121.6 (3) |
O9v—Nd2—O9vi | 65.88 (9) | C23—C28—H28 | 119.2 |
O1iii—Nd2—O9vi | 154.47 (8) | C27—C28—H28 | 119.2 |
O14—Nd2—O9vi | 116.39 (8) | C27—C29—C30 | 119.0 (3) |
O6ii—Nd2—O9vi | 80.98 (7) | C27—C29—H29A | 107.6 |
O10vi—Nd2—O9vi | 50.17 (8) | C30—C29—H29A | 107.6 |
O5ii—Nd2—O9vi | 130.65 (7) | C27—C29—H29B | 107.6 |
O2—C1—O1 | 120.1 (3) | C30—C29—H29B | 107.6 |
O2—C1—C2 | 121.6 (3) | H29A—C29—H29B | 107.0 |
O1—C1—C2 | 118.3 (3) | O11—C30—O12 | 125.0 (3) |
C3—C2—C1 | 115.8 (3) | O11—C30—C29 | 114.2 (3) |
C3—C2—H2A | 108.3 | O12—C30—C29 | 120.8 (3) |
C1—C2—H2A | 108.3 | C1—O1—Nd2viii | 149.4 (2) |
C3—C2—H2B | 108.3 | C1—O1—Nd1viii | 92.21 (19) |
C1—C2—H2B | 108.3 | Nd2viii—O1—Nd1viii | 109.46 (8) |
H2A—C2—H2B | 107.4 | C1—O2—Nd1viii | 96.0 (2) |
C4—C3—C8 | 118.0 (3) | C10—O3—Nd1i | 155.9 (2) |
C4—C3—C2 | 120.9 (3) | C10—O3—Nd1 | 87.89 (19) |
C8—C3—C2 | 121.1 (3) | Nd1i—O3—Nd1 | 115.22 (9) |
C5—C4—C3 | 121.1 (4) | C10—O4—Nd1 | 103.32 (19) |
C5—C4—H4 | 119.4 | C11—O5—Nd1ii | 153.8 (2) |
C3—C4—H4 | 119.4 | C11—O5—Nd2ii | 92.8 (2) |
C4—C5—C6 | 120.1 (4) | Nd1ii—O5—Nd2ii | 111.55 (9) |
C4—C5—H5 | 120.0 | C11—O6—Nd2ii | 95.8 (2) |
C6—C5—H5 | 120.0 | C20—O7—Nd1 | 147.9 (2) |
C7—C6—C5 | 120.5 (4) | C20—O8—Nd2iv | 144.9 (2) |
C7—C6—H6 | 119.7 | C21—O9—Nd2v | 132.8 (2) |
C5—C6—H6 | 119.7 | C21—O9—Nd2vii | 91.54 (19) |
C6—C7—C8 | 119.0 (3) | Nd2v—O9—Nd2vii | 114.12 (8) |
C6—C7—C9 | 120.0 (3) | C21—O10—Nd2vii | 96.9 (2) |
C8—C7—C9 | 120.9 (3) | C30—O11—Nd2 | 143.5 (2) |
C7—C8—C3 | 121.3 (3) | C30—O12—Nd1 | 131.1 (2) |
C7—C8—H8 | 119.4 | Nd1—O13—H1W | 116.9 |
C3—C8—H8 | 119.4 | Nd1—O13—H2W | 117.1 |
C10—C9—C7 | 114.1 (3) | H1W—O13—H2W | 125.7 |
C10—C9—H9A | 108.7 | Nd2—O14—H4W | 113.5 |
C7—C9—H9A | 108.7 | Nd2—O14—H3W | 123.7 |
C10—C9—H9B | 108.7 | H4W—O14—H3W | 113.8 |
O2—C1—C2—C3 | −3.6 (5) | O1iii—Nd1—O3—C10 | −137.8 (2) |
O1—C1—C2—C3 | 178.0 (3) | C1iii—Nd1—O3—C10 | 171.40 (19) |
C1—C2—C3—C4 | −65.1 (5) | O3i—Nd1—O3—Nd1i | 0.0 |
C1—C2—C3—C8 | 115.0 (4) | O5ii—Nd1—O3—Nd1i | 139.84 (10) |
C8—C3—C4—C5 | −0.4 (5) | O4—Nd1—O3—Nd1i | 172.57 (17) |
C2—C3—C4—C5 | 179.8 (3) | O7—Nd1—O3—Nd1i | −136.64 (10) |
C3—C4—C5—C6 | −1.1 (6) | O12—Nd1—O3—Nd1i | 76.98 (11) |
C4—C5—C6—C7 | 1.4 (6) | O13—Nd1—O3—Nd1i | −86.07 (11) |
C5—C6—C7—C8 | −0.2 (5) | O2iii—Nd1—O3—Nd1i | −42.57 (15) |
C5—C6—C7—C9 | 176.9 (3) | O1iii—Nd1—O3—Nd1i | 35.2 (2) |
C6—C7—C8—C3 | −1.3 (5) | C1iii—Nd1—O3—Nd1i | −15.6 (2) |
C9—C7—C8—C3 | −178.4 (3) | O3—C10—O4—Nd1 | −0.8 (4) |
C4—C3—C8—C7 | 1.6 (5) | C9—C10—O4—Nd1 | 179.2 (3) |
C2—C3—C8—C7 | −178.6 (3) | O3i—Nd1—O4—C10 | 7.8 (3) |
C6—C7—C9—C10 | −78.4 (4) | O5ii—Nd1—O4—C10 | 151.4 (2) |
C8—C7—C9—C10 | 98.7 (4) | O7—Nd1—O4—C10 | −136.7 (2) |
C7—C9—C10—O4 | −6.9 (5) | O12—Nd1—O4—C10 | 79.8 (2) |
C7—C9—C10—O3 | 173.1 (3) | O13—Nd1—O4—C10 | −65.6 (2) |
O6—C11—C12—C13 | −21.0 (6) | O2iii—Nd1—O4—C10 | −95.4 (3) |
O5—C11—C12—C13 | 162.9 (4) | O1iii—Nd1—O4—C10 | 150.0 (2) |
C11—C12—C13—C14 | −62.9 (6) | O3—Nd1—O4—C10 | 0.4 (2) |
C11—C12—C13—C18 | 119.6 (4) | C1iii—Nd1—O4—C10 | −162.0 (3) |
C18—C13—C14—C15 | −1.6 (6) | O6—C11—O5—Nd1ii | 156.4 (4) |
C12—C13—C14—C15 | −179.1 (4) | C12—C11—O5—Nd1ii | −27.5 (7) |
C13—C14—C15—C16 | 0.5 (6) | O6—C11—O5—Nd2ii | −2.8 (3) |
C14—C15—C16—C17 | 1.3 (6) | C12—C11—O5—Nd2ii | 173.3 (3) |
C15—C16—C17—C18 | −1.9 (5) | O5—C11—O6—Nd2ii | 2.9 (4) |
C15—C16—C17—C19 | 178.2 (3) | C12—C11—O6—Nd2ii | −173.0 (4) |
C16—C17—C18—C13 | 0.8 (5) | O8—C20—O7—Nd1 | 175.1 (3) |
C19—C17—C18—C13 | −179.3 (3) | C19—C20—O7—Nd1 | −5.4 (6) |
C14—C13—C18—C17 | 0.9 (5) | O3i—Nd1—O7—C20 | −105.2 (4) |
C12—C13—C18—C17 | 178.5 (3) | O5ii—Nd1—O7—C20 | 93.5 (4) |
C16—C17—C19—C20 | −65.2 (4) | O4—Nd1—O7—C20 | 15.9 (4) |
C18—C17—C19—C20 | 114.9 (4) | O12—Nd1—O7—C20 | 95.2 (4) |
C17—C19—C20—O8 | 22.9 (5) | O13—Nd1—O7—C20 | −69.4 (4) |
C17—C19—C20—O7 | −156.6 (3) | O2iii—Nd1—O7—C20 | −146.1 (4) |
O10—C21—C22—C23 | 8.0 (5) | O1iii—Nd1—O7—C20 | 163.4 (4) |
O9—C21—C22—C23 | −174.6 (3) | O3—Nd1—O7—C20 | −20.0 (4) |
C21—C22—C23—C28 | 109.6 (4) | C1iii—Nd1—O7—C20 | −170.7 (4) |
C21—C22—C23—C24 | −70.0 (5) | O7—C20—O8—Nd2iv | −36.4 (6) |
C28—C23—C24—C25 | −1.3 (7) | C19—C20—O8—Nd2iv | 144.1 (3) |
C22—C23—C24—C25 | 178.3 (4) | O10—C21—O9—Nd2v | −118.1 (3) |
C23—C24—C25—C26 | 2.0 (8) | C22—C21—O9—Nd2v | 64.4 (4) |
C24—C25—C26—C27 | −1.3 (8) | O10—C21—O9—Nd2vii | 7.5 (4) |
C25—C26—C27—C28 | 0.1 (6) | C22—C21—O9—Nd2vii | −170.0 (3) |
C25—C26—C27—C29 | 177.8 (4) | O9—C21—O10—Nd2vii | −7.8 (4) |
C24—C23—C28—C27 | 0.1 (6) | C22—C21—O10—Nd2vii | 169.6 (3) |
C22—C23—C28—C27 | −179.5 (3) | O12—C30—O11—Nd2 | −36.9 (6) |
C26—C27—C28—C23 | 0.5 (5) | C29—C30—O11—Nd2 | 144.4 (3) |
C29—C27—C28—C23 | −177.2 (3) | O8iv—Nd2—O11—C30 | 100.6 (4) |
C26—C27—C29—C30 | 58.1 (5) | O9v—Nd2—O11—C30 | 149.5 (4) |
C28—C27—C29—C30 | −124.2 (4) | O1iii—Nd2—O11—C30 | 56.7 (4) |
C27—C29—C30—O11 | −170.9 (3) | O14—Nd2—O11—C30 | −15.2 (4) |
C27—C29—C30—O12 | 10.4 (5) | O6ii—Nd2—O11—C30 | −68.1 (4) |
O2—C1—O1—Nd2viii | 126.3 (4) | O10vi—Nd2—O11—C30 | −120.0 (4) |
C2—C1—O1—Nd2viii | −55.3 (6) | O5ii—Nd2—O11—C30 | −15.6 (4) |
O2—C1—O1—Nd1viii | −9.9 (3) | O9vi—Nd2—O11—C30 | −147.7 (4) |
C2—C1—O1—Nd1viii | 168.6 (3) | C11ii—Nd2—O11—C30 | −43.0 (4) |
O1—C1—O2—Nd1viii | 10.1 (3) | C21vi—Nd2—O11—C30 | −134.6 (4) |
C2—C1—O2—Nd1viii | −168.2 (3) | O11—C30—O12—Nd1 | 27.9 (5) |
O4—C10—O3—Nd1i | −163.6 (4) | C29—C30—O12—Nd1 | −153.5 (3) |
C9—C10—O3—Nd1i | 16.4 (8) | O3i—Nd1—O12—C30 | −142.6 (3) |
O4—C10—O3—Nd1 | 0.7 (3) | O5ii—Nd1—O12—C30 | 26.1 (3) |
C9—C10—O3—Nd1 | −179.3 (3) | O4—Nd1—O12—C30 | 102.4 (3) |
O3i—Nd1—O3—C10 | −173.0 (3) | O7—Nd1—O12—C30 | 24.3 (4) |
O5ii—Nd1—O3—C10 | −33.2 (2) | O13—Nd1—O12—C30 | 178.8 (3) |
O4—Nd1—O3—C10 | −0.43 (19) | O2iii—Nd1—O12—C30 | −80.1 (3) |
O7—Nd1—O3—C10 | 50.4 (2) | O1iii—Nd1—O12—C30 | −45.4 (3) |
O12—Nd1—O3—C10 | −96.0 (2) | O3—Nd1—O12—C30 | 151.1 (3) |
O13—Nd1—O3—C10 | 100.9 (2) | C1iii—Nd1—O12—C30 | −63.8 (3) |
O2iii—Nd1—O3—C10 | 144.43 (19) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z+1; (iii) x, y−1, z; (iv) −x, −y, −z+1; (v) −x+1, −y, −z; (vi) x, y, z+1; (vii) x, y, z−1; (viii) x, y+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O13—H1W···O12i | 0.88 | 2.39 | 2.838 (3) | 112 |
O14—H4W···O7iv | 0.86 | 2.26 | 2.829 (3) | 124 |
O14—H4W···O2ii | 0.86 | 2.41 | 3.177 (4) | 148 |
O14—H3W···O7 | 0.87 | 2.25 | 3.024 (3) | 149 |
O14—H3W···O14iv | 0.87 | 2.53 | 3.100 (5) | 123 |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z+1; (iv) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Nd2(C10H8O4)3(H2O)2] |
Mr | 901.00 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 10.4846 (13), 11.9660 (16), 12.3514 (16) |
α, β, γ (°) | 105.619 (5), 97.202 (5), 92.625 (6) |
V (Å3) | 1475.5 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.55 |
Crystal size (mm) | 0.24 × 0.22 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1997) |
Tmin, Tmax | 0.516, 0.580 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7865, 5315, 4806 |
Rint | 0.013 |
(sin θ/λ)max (Å−1) | 0.601 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.054, 1.03 |
No. of reflections | 5315 |
No. of parameters | 415 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.64, −0.76 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).
D—H···A | D—H | H···A | D···A | D—H···A |
O13—H1W···O12i | 0.88 | 2.39 | 2.838 (3) | 112 |
O14—H4W···O7ii | 0.86 | 2.26 | 2.829 (3) | 124 |
O14—H4W···O2iii | 0.86 | 2.41 | 3.177 (4) | 148 |
O14—H3W···O7 | 0.87 | 2.25 | 3.024 (3) | 149 |
O14—H3W···O14ii | 0.87 | 2.53 | 3.100 (5) | 123 |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y, −z+1; (iii) −x, −y+1, −z+1. |
References
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (1997). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
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Lanthanide coordination polymers have shown versatile structural architectures, accompanied with desirable properties, like luminescence, magnetism, catalysis, gas adsorption and separation (Xiao et al., 2008; Lv et al., 2010). In order to extend our investigations in this field, we chose 1,3-phenylendiacetic acid (pda) as a functional ligand and synthesized the lanthanide coordination polymer [Nd2(pda)3(H2O)2]n, the structure of which is reported here.
The title compound is isotypic with its Ce analogue (Gao et al., 2011). The asymmetric unit of the title complex (Fig. 1) contains two crystallographically unique NdIII ions, three pda ligands, and two coordinated water molecules. Both Nd1 and Nd2 are nine-coordinated within a distorted tricapped trigonal-prismatic geometry. The nine coordination sites are occupied by one O atom from a water molecule and eight O atoms from six different pda anions. The Nd—O bond lengths in the title complex are in the range 2.377 (2)–2.749 (2) Å, which is comparable to those reported for other Nd complexes with oxygen environment around the central metal (Xiao et al., 2008; Wang et al., 2009). The pda ligands adopt two coordination modes, viz. µ4-hexadentate and µ4-pentadentate. Eight NdIII ions and twelve pda ligands form a large [Nd8(pda)12] ring, whereas four NdIII ions and six pda ligands form a small [Nd4(pda)6] ring (Fig. 2). These rings are further connected by the coordination interactions of pda ligands and NdIII to generate a three-dimensional supramolecular framework (Fig. 2).