Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807022519/rz2137sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807022519/rz2137Isup2.hkl |
CCDC reference: 641963
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.030
- wR factor = 0.073
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H2W .. H4W .. 1.94 Ang. PLAT420_ALERT_2_B D-H Without Acceptor O1W - H2W ... ?
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pr1 PLAT245_ALERT_2_C U(iso) H1W Smaller than U(eq) O1W by ... 0.03 AngSq PLAT245_ALERT_2_C U(iso) H2W Smaller than U(eq) O1W by ... 0.03 AngSq PLAT245_ALERT_2_C U(iso) H3W Smaller than U(eq) O2W by ... 0.04 AngSq PLAT245_ALERT_2_C U(iso) H4W Smaller than U(eq) O2W by ... 0.04 AngSq PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.15 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Pr1 (3) 3.16 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
A mixture of Pr(NO3)3 (0.5 mmol), (p-phenylenedioxy)diacetic acid (0.75 mmol), NaOH (1.5 mmol) and H2O (10 ml) was placed in a 20 ml Teflon reactor, which was heated at 433 K for three days and then cooled to room temperature at a rate of 10 K h-1. Crystals were obtained after washing with water and drying in air.
Carbon-bound H atoms were placed at calculated positions and were treated as riding on the parent C atoms with C—H = 0.93 Å, and with Uiso(H) = 1.2 Ueq(C). Water H atoms were tentatively located in difference Fourier maps and were refined with distance restraints of O–H = 0.82 or 0.85 Å and H···H = 1.29 or 1.39 Å, each within a standard deviation of 0.01 Å.
Molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000; Choi & Jeon, 2003). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. As a building block, (p-phenylenedioxy)diacetic acid (1,4-BDOA) is an excellent candidate for the construction of supramolecular complexes (Qiu et al., 2006). Recently, we obtained the title novel coordination polymer, (I), by the reaction of praseodymium nitrate, (p-phenylenedioxy)diacetic acid in alkaline aqueous solution, and its crystal structure is reported here.
In (I), each PrIII ion is coordinated by nine oxygen atoms, eight from four 1,4-BDOA2- ligands and one from a water molecule (Fig. 1). The coordination environment around the PrIII ion can be described as a tri-capped-trigonal prismatic geometry with O—Pr—O bond angles ranging from 47.76 (8) to 149.67 (8) Å. Pairs of Pr ions are bridged by the dianionic ligands at a distance of 4.188 (3) Å to form helical chains which are further cross-linked by the ligands into a three-dimensional supramolecular network (Fig. 2) with channels running along the c axis hosting the uncoordinated water molecules. The crystal structure is stabilized by intermolecular O—H···O hydrogen bonding interactions.
For related literature, see: Choi & Jeon (2003); Qiu et al. (2006); Tao et al. (2000).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.
[Pr2(C10H8O6)3(H2O)2]·2H2O | F(000) = 1012 |
Mr = 1026.38 | Dx = 1.959 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3500 reflections |
a = 12.1685 (3) Å | θ = 1.7–28.0° |
b = 16.9339 (4) Å | µ = 2.86 mm−1 |
c = 8.9299 (2) Å | T = 293 K |
β = 108.956 (1)° | Block, colourless |
V = 1740.30 (7) Å3 | 0.18 × 0.15 × 0.12 mm |
Z = 2 |
Bruker APEXII area-detector diffractometer | 4182 independent reflections |
Radiation source: fine-focus sealed tube | 3381 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
φ and ω scans | θmax = 28.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→16 |
Tmin = 0.607, Tmax = 0.715 | k = −17→22 |
14677 measured reflections | l = −11→11 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0304P)2 + 2.8471P] where P = (Fo2 + 2Fc2)/3 |
4182 reflections | (Δ/σ)max = 0.001 |
244 parameters | Δρmax = 0.62 e Å−3 |
6 restraints | Δρmin = −0.81 e Å−3 |
[Pr2(C10H8O6)3(H2O)2]·2H2O | V = 1740.30 (7) Å3 |
Mr = 1026.38 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.1685 (3) Å | µ = 2.86 mm−1 |
b = 16.9339 (4) Å | T = 293 K |
c = 8.9299 (2) Å | 0.18 × 0.15 × 0.12 mm |
β = 108.956 (1)° |
Bruker APEXII area-detector diffractometer | 4182 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3381 reflections with I > 2σ(I) |
Tmin = 0.607, Tmax = 0.715 | Rint = 0.036 |
14677 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 6 restraints |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.62 e Å−3 |
4182 reflections | Δρmin = −0.81 e Å−3 |
244 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 | ||
C1 | 0.3882 (3) | 0.2982 (2) | 1.0544 (4) | 0.0214 (7) | |
C2 | 0.2921 (3) | 0.2998 (2) | 0.8969 (4) | 0.0230 (8) | |
H2A | 0.2219 | 0.3214 | 0.9097 | 0.028* | |
H2B | 0.3144 | 0.3329 | 0.8229 | 0.028* | |
C3 | 0.1633 (3) | 0.2069 (2) | 0.7228 (4) | 0.0198 (7) | |
C4 | 0.1125 (3) | 0.2595 (2) | 0.6019 (5) | 0.0274 (8) | |
H4 | 0.1479 | 0.3077 | 0.5967 | 0.033* | |
C5 | 0.0081 (3) | 0.2397 (2) | 0.4888 (5) | 0.0289 (9) | |
H5 | −0.0268 | 0.2749 | 0.4075 | 0.035* | |
C6 | −0.0447 (3) | 0.1683 (2) | 0.4949 (4) | 0.0218 (8) | |
C7 | 0.0062 (3) | 0.1167 (2) | 0.6184 (4) | 0.0262 (8) | |
H7 | −0.0295 | 0.0687 | 0.6244 | 0.031* | |
C8 | 0.1099 (3) | 0.1363 (2) | 0.7325 (4) | 0.0240 (8) | |
H8 | 0.1437 | 0.1019 | 0.8159 | 0.029* | |
C9 | −0.1944 (3) | 0.0758 (2) | 0.3755 (4) | 0.0270 (8) | |
H9A | −0.2151 | 0.0695 | 0.4709 | 0.032* | |
H9B | −0.1353 | 0.0369 | 0.3781 | 0.032* | |
C10 | −0.3006 (3) | 0.0605 (2) | 0.2326 (4) | 0.0227 (8) | |
C11 | 0.3538 (3) | 0.0272 (2) | 1.1574 (4) | 0.0254 (8) | |
C12 | 0.3027 (4) | −0.0132 (3) | 1.2703 (5) | 0.0414 (11) | |
H12A | 0.2934 | −0.0690 | 1.2443 | 0.050* | |
H12B | 0.3569 | −0.0086 | 1.3770 | 0.050* | |
C13 | 0.1003 (4) | 0.0075 (3) | 1.1304 (5) | 0.0352 (10) | |
C14 | 0.0010 (4) | 0.0502 (3) | 1.1204 (5) | 0.0368 (10) | |
H14 | 0.0016 | 0.0842 | 1.2024 | 0.044* | |
C15 | 0.0980 (4) | −0.0433 (3) | 1.0079 (5) | 0.0377 (10) | |
H15 | 0.1636 | −0.0727 | 1.0126 | 0.045* | |
O1 | 0.4518 (3) | 0.23847 (17) | 1.0882 (3) | 0.0385 (8) | |
O2 | 0.3992 (2) | 0.35833 (16) | 1.1385 (3) | 0.0284 (6) | |
O3 | 0.2716 (2) | 0.22057 (15) | 0.8373 (3) | 0.0241 (6) | |
O4 | −0.1475 (2) | 0.15296 (16) | 0.3742 (3) | 0.0272 (6) | |
O5 | −0.3176 (2) | −0.01103 (16) | 0.2027 (3) | 0.0281 (6) | |
O6 | −0.3610 (2) | 0.11699 (16) | 0.1607 (3) | 0.0312 (6) | |
O7 | 0.3150 (2) | 0.09148 (16) | 1.0965 (3) | 0.0318 (6) | |
O8 | 0.4394 (2) | −0.00571 (16) | 1.1333 (3) | 0.0282 (6) | |
O9 | 0.1936 (3) | 0.0180 (2) | 1.2671 (3) | 0.0414 (8) | |
O1W | 0.6001 (3) | 0.2096 (2) | 0.8741 (4) | 0.0525 (10) | |
O2W | 0.7480 (3) | 0.2822 (2) | 0.1433 (4) | 0.0648 (11) | |
Pr1 | 0.451486 (16) | 0.116370 (11) | 0.92970 (2) | 0.01832 (7) | |
H1W | 0.6202 | 0.2263 | 0.7986 | 0.022* | |
H2W | 0.5562 | 0.2409 | 0.8926 | 0.022* | |
H3W | 0.7894 | 0.2456 | 0.1300 | 0.022* | |
H4W | 0.6805 | 0.2807 | 0.0727 | 0.022* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0247 (19) | 0.019 (2) | 0.0184 (16) | 0.0007 (15) | 0.0038 (14) | 0.0004 (15) |
C2 | 0.027 (2) | 0.0151 (19) | 0.0206 (17) | −0.0004 (15) | −0.0008 (15) | −0.0047 (14) |
C3 | 0.0137 (16) | 0.0204 (19) | 0.0200 (16) | 0.0001 (14) | −0.0021 (13) | −0.0060 (14) |
C4 | 0.023 (2) | 0.021 (2) | 0.031 (2) | −0.0068 (16) | −0.0009 (16) | 0.0024 (16) |
C5 | 0.023 (2) | 0.026 (2) | 0.0268 (19) | −0.0029 (17) | −0.0073 (16) | 0.0071 (16) |
C6 | 0.0156 (17) | 0.022 (2) | 0.0199 (16) | −0.0023 (15) | −0.0047 (13) | −0.0043 (15) |
C7 | 0.0225 (19) | 0.023 (2) | 0.0248 (18) | −0.0062 (16) | −0.0034 (15) | 0.0009 (16) |
C8 | 0.0203 (18) | 0.022 (2) | 0.0217 (17) | −0.0001 (15) | −0.0038 (14) | 0.0033 (15) |
C9 | 0.0236 (19) | 0.020 (2) | 0.0262 (19) | −0.0056 (16) | −0.0076 (15) | 0.0021 (16) |
C10 | 0.0204 (18) | 0.025 (2) | 0.0185 (17) | −0.0065 (16) | 0.0009 (14) | 0.0007 (15) |
C11 | 0.0240 (19) | 0.027 (2) | 0.0238 (18) | −0.0021 (16) | 0.0052 (15) | −0.0027 (16) |
C12 | 0.040 (3) | 0.044 (3) | 0.042 (2) | 0.001 (2) | 0.016 (2) | 0.018 (2) |
C13 | 0.037 (2) | 0.033 (3) | 0.043 (2) | −0.007 (2) | 0.024 (2) | 0.005 (2) |
C14 | 0.042 (3) | 0.031 (2) | 0.047 (3) | −0.007 (2) | 0.028 (2) | −0.007 (2) |
C15 | 0.036 (2) | 0.031 (3) | 0.056 (3) | 0.0017 (19) | 0.028 (2) | 0.002 (2) |
O1 | 0.0356 (17) | 0.0254 (17) | 0.0343 (16) | 0.0095 (13) | −0.0166 (13) | −0.0140 (13) |
O2 | 0.0379 (16) | 0.0199 (15) | 0.0197 (12) | 0.0014 (12) | −0.0012 (11) | −0.0079 (11) |
O3 | 0.0192 (13) | 0.0168 (14) | 0.0249 (13) | −0.0007 (10) | −0.0084 (10) | −0.0051 (10) |
O4 | 0.0201 (13) | 0.0207 (15) | 0.0271 (13) | −0.0082 (11) | −0.0110 (11) | 0.0041 (11) |
O5 | 0.0237 (14) | 0.0196 (15) | 0.0321 (14) | −0.0063 (11) | −0.0032 (12) | −0.0030 (11) |
O6 | 0.0239 (14) | 0.0246 (16) | 0.0300 (14) | −0.0006 (12) | −0.0122 (12) | 0.0044 (12) |
O7 | 0.0388 (16) | 0.0234 (15) | 0.0392 (16) | 0.0103 (13) | 0.0208 (13) | 0.0093 (13) |
O8 | 0.0252 (14) | 0.0282 (16) | 0.0279 (14) | 0.0072 (12) | 0.0039 (12) | 0.0005 (12) |
O9 | 0.0360 (17) | 0.055 (2) | 0.0406 (17) | −0.0066 (15) | 0.0231 (15) | 0.0001 (15) |
O1W | 0.050 (2) | 0.065 (3) | 0.0345 (17) | −0.0256 (18) | 0.0027 (15) | 0.0144 (16) |
O2W | 0.053 (2) | 0.067 (3) | 0.056 (2) | −0.012 (2) | −0.0079 (18) | 0.011 (2) |
Pr1 | 0.01760 (11) | 0.01524 (11) | 0.01758 (10) | −0.00029 (8) | −0.00054 (7) | 0.00020 (8) |
C1—O2 | 1.246 (4) | C12—H12A | 0.9700 |
C1—O1 | 1.250 (4) | C12—H12B | 0.9700 |
C1—C2 | 1.509 (5) | C13—O9 | 1.383 (5) |
C2—O3 | 1.435 (4) | C13—C15 | 1.385 (6) |
C2—H2A | 0.9700 | C13—C14 | 1.385 (6) |
C2—H2B | 0.9700 | C14—C15i | 1.372 (6) |
C3—C8 | 1.377 (5) | C14—H14 | 0.9300 |
C3—C4 | 1.382 (5) | C15—C14i | 1.372 (6) |
C3—O3 | 1.400 (4) | C15—H15 | 0.9300 |
C4—C5 | 1.382 (5) | O1—Pr1 | 2.505 (3) |
C4—H4 | 0.9300 | O2—Pr1ii | 2.505 (2) |
C5—C6 | 1.378 (5) | O3—Pr1 | 2.723 (2) |
C5—H5 | 0.9300 | O5—Pr1iii | 2.446 (3) |
C6—O4 | 1.385 (4) | O6—Pr1iv | 2.531 (3) |
C6—C7 | 1.386 (5) | O7—Pr1 | 2.600 (3) |
C7—C8 | 1.380 (5) | O8—Pr1v | 2.465 (3) |
C7—H7 | 0.9300 | O8—Pr1 | 2.788 (3) |
C8—H8 | 0.9300 | O1W—Pr1 | 2.568 (3) |
C9—O4 | 1.427 (4) | O1W—H1W | 0.8374 |
C9—C10 | 1.514 (5) | O1W—H2W | 0.8059 |
C9—H9A | 0.9700 | O2W—H3W | 0.8319 |
C9—H9B | 0.9700 | O2W—H4W | 0.8582 |
C10—O5 | 1.244 (4) | Pr1—O5iii | 2.446 (3) |
C10—O6 | 1.249 (4) | Pr1—O8v | 2.465 (3) |
C11—O7 | 1.241 (5) | Pr1—O2vi | 2.505 (2) |
C11—O8 | 1.260 (4) | Pr1—O6vii | 2.531 (3) |
C11—C12 | 1.510 (5) | Pr1—H2W | 2.5404 |
C12—O9 | 1.420 (5) | ||
O2—C1—O1 | 125.3 (3) | C2—O3—Pr1 | 117.86 (19) |
O2—C1—C2 | 116.5 (3) | C6—O4—C9 | 115.3 (3) |
O1—C1—C2 | 118.1 (3) | C10—O5—Pr1iii | 148.5 (2) |
O3—C2—C1 | 108.5 (3) | C10—O6—Pr1iv | 129.8 (2) |
O3—C2—H2A | 110.0 | C11—O7—Pr1 | 99.8 (2) |
C1—C2—H2A | 110.0 | C11—O8—Pr1v | 155.7 (3) |
O3—C2—H2B | 110.0 | C11—O8—Pr1 | 90.3 (2) |
C1—C2—H2B | 110.0 | Pr1v—O8—Pr1 | 105.58 (9) |
H2A—C2—H2B | 108.4 | C13—O9—C12 | 117.6 (3) |
C8—C3—C4 | 120.6 (3) | Pr1—O1W—H1W | 140.5 |
C8—C3—O3 | 116.7 (3) | Pr1—O1W—H2W | 79.0 |
C4—C3—O3 | 122.7 (3) | H1W—O1W—H2W | 109.3 |
C3—C4—C5 | 119.0 (4) | H3W—O2W—H4W | 110.7 |
C3—C4—H4 | 120.5 | O5iii—Pr1—O8v | 70.05 (9) |
C5—C4—H4 | 120.5 | O5iii—Pr1—O1 | 138.91 (10) |
C6—C5—C4 | 120.9 (3) | O8v—Pr1—O1 | 148.69 (9) |
C6—C5—H5 | 119.5 | O5iii—Pr1—O2vi | 73.65 (9) |
C4—C5—H5 | 119.5 | O8v—Pr1—O2vi | 82.36 (9) |
C5—C6—O4 | 116.7 (3) | O1—Pr1—O2vi | 113.49 (9) |
C5—C6—C7 | 119.4 (3) | O5iii—Pr1—O6vii | 132.82 (9) |
O4—C6—C7 | 123.9 (3) | O8v—Pr1—O6vii | 77.26 (9) |
C8—C7—C6 | 120.0 (4) | O1—Pr1—O6vii | 72.56 (9) |
C8—C7—H7 | 120.0 | O2vi—Pr1—O6vii | 134.67 (10) |
C6—C7—H7 | 120.0 | O5iii—Pr1—O1W | 139.07 (10) |
C3—C8—C7 | 120.0 (3) | O8v—Pr1—O1W | 87.60 (11) |
C3—C8—H8 | 120.0 | O1—Pr1—O1W | 74.31 (12) |
C7—C8—H8 | 120.0 | O2vi—Pr1—O1W | 69.60 (9) |
O4—C9—C10 | 112.6 (3) | O6vii—Pr1—O1W | 69.51 (10) |
O4—C9—H9A | 109.1 | O5iii—Pr1—O7 | 73.11 (9) |
C10—C9—H9A | 109.1 | O8v—Pr1—O7 | 119.94 (9) |
O4—C9—H9B | 109.1 | O1—Pr1—O7 | 72.20 (10) |
C10—C9—H9B | 109.1 | O2vi—Pr1—O7 | 128.92 (9) |
H9A—C9—H9B | 107.8 | O6vii—Pr1—O7 | 96.22 (9) |
O5—C10—O6 | 127.3 (3) | O1W—Pr1—O7 | 146.24 (11) |
O5—C10—C9 | 112.6 (3) | O5iii—Pr1—O3 | 88.99 (8) |
O6—C10—C9 | 120.0 (3) | O8v—Pr1—O3 | 149.67 (8) |
O7—C11—O8 | 122.1 (4) | O1—Pr1—O3 | 59.33 (8) |
O7—C11—C12 | 120.6 (4) | O2vi—Pr1—O3 | 70.52 (8) |
O8—C11—C12 | 117.2 (4) | O6vii—Pr1—O3 | 131.89 (8) |
O9—C12—C11 | 113.8 (4) | O1W—Pr1—O3 | 95.18 (10) |
O9—C12—H12A | 108.8 | O7—Pr1—O3 | 71.23 (8) |
C11—C12—H12A | 108.8 | O5iii—Pr1—O8 | 66.83 (8) |
O9—C12—H12B | 108.8 | O8v—Pr1—O8 | 74.42 (9) |
C11—C12—H12B | 108.8 | O1—Pr1—O8 | 103.55 (9) |
H12A—C12—H12B | 107.7 | O2vi—Pr1—O8 | 138.96 (8) |
O9—C13—C15 | 125.3 (4) | O6vii—Pr1—O8 | 72.30 (8) |
O9—C13—C14 | 116.0 (4) | O1W—Pr1—O8 | 140.50 (9) |
C15—C13—C14 | 118.7 (4) | O7—Pr1—O8 | 47.76 (8) |
C15i—C14—C13 | 121.4 (4) | O3—Pr1—O8 | 118.08 (8) |
C15i—C14—H14 | 119.3 | O5iii—Pr1—H2W | 145.7 |
C13—C14—H14 | 119.3 | O8v—Pr1—H2W | 105.7 |
C14i—C15—C13 | 119.9 (4) | O1—Pr1—H2W | 58.7 |
C14i—C15—H15 | 120.1 | O2vi—Pr1—H2W | 72.0 |
C13—C15—H15 | 120.1 | O6vii—Pr1—H2W | 75.2 |
C1—O1—Pr1 | 130.1 (2) | O1W—Pr1—H2W | 18.1 |
C1—O2—Pr1ii | 135.0 (2) | O7—Pr1—H2W | 130.5 |
C3—O3—C2 | 115.8 (3) | O3—Pr1—H2W | 79.1 |
C3—O3—Pr1 | 126.0 (2) | O8—Pr1—H2W | 146.6 |
Symmetry codes: (i) −x, −y, −z+2; (ii) x, −y+1/2, z+1/2; (iii) −x, −y, −z+1; (iv) x−1, y, z−1; (v) −x+1, −y, −z+2; (vi) x, −y+1/2, z−1/2; (vii) x+1, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O2Wii | 0.84 | 2.40 | 3.149 (5) | 149 |
O1W—H2W···O1 | 0.81 | 2.47 | 3.064 (5) | 131 |
O2W—H3W···O4viii | 0.83 | 2.59 | 2.992 (5) | 111 |
O2W—H4W···O1Wix | 0.86 | 2.10 | 2.778 (5) | 135 |
Symmetry codes: (ii) x, −y+1/2, z+1/2; (viii) x+1, y, z; (ix) x, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Pr2(C10H8O6)3(H2O)2]·2H2O |
Mr | 1026.38 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 12.1685 (3), 16.9339 (4), 8.9299 (2) |
β (°) | 108.956 (1) |
V (Å3) | 1740.30 (7) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.86 |
Crystal size (mm) | 0.18 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.607, 0.715 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14677, 4182, 3381 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.661 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.073, 1.03 |
No. of reflections | 4182 |
No. of parameters | 244 |
No. of restraints | 6 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.62, −0.81 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2004), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O2Wi | 0.84 | 2.40 | 3.149 (5) | 149.2 |
O1W—H2W···O1 | 0.81 | 2.47 | 3.064 (5) | 131.4 |
O2W—H3W···O4ii | 0.83 | 2.59 | 2.992 (5) | 111.0 |
O2W—H4W···O1Wiii | 0.86 | 2.10 | 2.778 (5) | 135.1 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x+1, y, z; (iii) x, y, z−1. |
Molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000; Choi & Jeon, 2003). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. As a building block, (p-phenylenedioxy)diacetic acid (1,4-BDOA) is an excellent candidate for the construction of supramolecular complexes (Qiu et al., 2006). Recently, we obtained the title novel coordination polymer, (I), by the reaction of praseodymium nitrate, (p-phenylenedioxy)diacetic acid in alkaline aqueous solution, and its crystal structure is reported here.
In (I), each PrIII ion is coordinated by nine oxygen atoms, eight from four 1,4-BDOA2- ligands and one from a water molecule (Fig. 1). The coordination environment around the PrIII ion can be described as a tri-capped-trigonal prismatic geometry with O—Pr—O bond angles ranging from 47.76 (8) to 149.67 (8) Å. Pairs of Pr ions are bridged by the dianionic ligands at a distance of 4.188 (3) Å to form helical chains which are further cross-linked by the ligands into a three-dimensional supramolecular network (Fig. 2) with channels running along the c axis hosting the uncoordinated water molecules. The crystal structure is stabilized by intermolecular O—H···O hydrogen bonding interactions.