Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110032026/sq3261sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270110032026/sq3261Isup2.hkl |
CCDC reference: 796062
For related literature, see: Batten (2001); Batten & Robson (1998); Carlucci et al. (2003); Eddaoudi et al. (2001); Kong et al. (2009); Long et al. (2002); O'Keeffe et al. (2008); Ockwig et al. (2005); Qiao et al. (2008, 2009); Wang et al. (2008, 2009, 2010); Yang et al. (2007, 2008).
A mixture of Pb(NO3)2 (0.5 mmol), 1,4-H2bdc (0.5 mmol) and L (1 mmol) was dissolved in distilled water (12 ml). The resulting solution was stirred for about 2 h at room temperature, sealed in a 23 ml Teflon-lined stainless steel autoclave and heated at 468 K for 7 d under autogenous pressure. Afterwards, the reaction system was slowly cooled to room temperature. Pale-yellow block crystals of (I) suitable for single-crystal X-ray diffraction analysis were collected from the final reaction system by filtration, washed several times with distilled water and dried in air at ambient temperature (yield 35% based on PbII).
All H atoms were positioned geometrically, with N—H = 0.86 Å and C—H = 0.93 Å, and refined as riding, with Uiso(H) = 1.2Ueq(carrier).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).
[Pb2(C8H4O4)2(C18H11N5)2] | Z = 2 |
Mr = 1337.24 | F(000) = 1280 |
Triclinic, P1 | Dx = 1.932 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.9066 (7) Å | Cell parameters from 7984 reflections |
b = 15.0537 (10) Å | θ = 1.4–25.0° |
c = 15.0663 (10) Å | µ = 7.38 mm−1 |
α = 75.890 (1)° | T = 293 K |
β = 74.199 (1)° | Block, pale yellow |
γ = 81.399 (1)° | 0.27 × 0.22 × 0.16 mm |
V = 2299.2 (3) Å3 |
Bruker APEX diffractometer | 7984 independent reflections |
Radiation source: fine-focus sealed tube | 6315 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→11 |
Tmin = 0.56, Tmax = 0.77 | k = −17→17 |
12743 measured reflections | l = −17→10 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.070 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0361P)2] where P = (Fo2 + 2Fc2)/3 |
7984 reflections | (Δ/σ)max = 0.001 |
649 parameters | Δρmax = 1.27 e Å−3 |
0 restraints | Δρmin = −0.60 e Å−3 |
[Pb2(C8H4O4)2(C18H11N5)2] | γ = 81.399 (1)° |
Mr = 1337.24 | V = 2299.2 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.9066 (7) Å | Mo Kα radiation |
b = 15.0537 (10) Å | µ = 7.38 mm−1 |
c = 15.0663 (10) Å | T = 293 K |
α = 75.890 (1)° | 0.27 × 0.22 × 0.16 mm |
β = 74.199 (1)° |
Bruker APEX diffractometer | 7984 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 6315 reflections with I > 2σ(I) |
Tmin = 0.56, Tmax = 0.77 | Rint = 0.021 |
12743 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.070 | H-atom parameters constrained |
S = 0.98 | Δρmax = 1.27 e Å−3 |
7984 reflections | Δρmin = −0.60 e Å−3 |
649 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | −0.0251 (5) | −0.5031 (4) | 0.1199 (5) | 0.056 (2) | |
H1 | −0.1107 | −0.4984 | 0.1189 | 0.068* | |
C2 | 0.0497 (6) | −0.5853 (4) | 0.1164 (5) | 0.0542 (19) | |
H2 | 0.0117 | −0.6354 | 0.1133 | 0.065* | |
C3 | 0.5529 (5) | −0.6300 (4) | 0.1037 (5) | 0.0421 (15) | |
H3 | 0.5981 | −0.6856 | 0.0936 | 0.051* | |
C4 | 0.6187 (6) | −0.5625 (4) | 0.1133 (5) | 0.0496 (17) | |
H4 | 0.7055 | −0.5740 | 0.1114 | 0.060* | |
C5 | 0.3520 (5) | −0.3785 (4) | 0.1311 (4) | 0.0326 (13) | |
C6 | 0.5561 (5) | −0.4790 (4) | 0.1255 (4) | 0.0405 (15) | |
H6 | 0.5992 | −0.4329 | 0.1319 | 0.049* | |
C7 | 0.4255 (5) | −0.4646 (4) | 0.1280 (4) | 0.0303 (12) | |
C8 | 0.3639 (5) | −0.5372 (3) | 0.1207 (4) | 0.0326 (13) | |
C9 | 0.2264 (5) | −0.5242 (4) | 0.1224 (4) | 0.0354 (14) | |
C10 | 0.0289 (5) | −0.4286 (4) | 0.1251 (5) | 0.0509 (18) | |
H10 | −0.0197 | −0.3725 | 0.1270 | 0.061* | |
C11 | 0.1565 (5) | −0.4374 (4) | 0.1275 (4) | 0.0358 (14) | |
C12 | 0.2814 (5) | −0.2343 (4) | 0.1295 (4) | 0.0354 (14) | |
C13 | 0.2237 (5) | −0.3646 (4) | 0.1315 (4) | 0.0361 (14) | |
C14 | 0.1904 (6) | 0.0174 (5) | 0.1066 (7) | 0.081 (3) | |
H14 | 0.1188 | 0.0580 | 0.0995 | 0.097* | |
C15 | 0.1827 (6) | −0.0745 (4) | 0.1131 (6) | 0.071 (3) | |
H15 | 0.1078 | −0.0944 | 0.1094 | 0.085* | |
C16 | 0.2843 (5) | −0.1363 (4) | 0.1251 (4) | 0.0364 (14) | |
C17 | 0.3904 (6) | −0.1014 (4) | 0.1298 (6) | 0.064 (2) | |
H17 | 0.4625 | −0.1408 | 0.1384 | 0.077* | |
C18 | 0.3913 (7) | −0.0089 (4) | 0.1219 (6) | 0.066 (2) | |
H18 | 0.4653 | 0.0124 | 0.1253 | 0.080* | |
C19 | 0.4661 (6) | 0.3605 (4) | 0.3762 (6) | 0.063 (2) | |
H19 | 0.5056 | 0.3015 | 0.3743 | 0.075* | |
C20 | 0.5390 (6) | 0.4270 (4) | 0.3804 (5) | 0.056 (2) | |
H20 | 0.6244 | 0.4122 | 0.3819 | 0.068* | |
C21 | 0.4835 (6) | 0.5143 (4) | 0.3824 (5) | 0.0501 (17) | |
H21 | 0.5309 | 0.5600 | 0.3842 | 0.060* | |
C22 | 0.3544 (5) | 0.5340 (4) | 0.3816 (4) | 0.0359 (14) | |
C23 | 0.2859 (5) | 0.4631 (4) | 0.3776 (4) | 0.0341 (13) | |
C24 | 0.1508 (5) | 0.4784 (4) | 0.3774 (4) | 0.0332 (13) | |
C25 | −0.0320 (6) | 0.4220 (4) | 0.3747 (4) | 0.0462 (16) | |
H25 | −0.0734 | 0.3732 | 0.3723 | 0.055* | |
C26 | −0.1034 (6) | 0.5060 (4) | 0.3787 (5) | 0.0462 (16) | |
H26 | −0.1895 | 0.5128 | 0.3786 | 0.055* | |
C27 | −0.0450 (5) | 0.5784 (4) | 0.3829 (4) | 0.0430 (15) | |
H27 | −0.0908 | 0.6354 | 0.3857 | 0.052* | |
C28 | 0.0842 (5) | 0.5657 (4) | 0.3830 (4) | 0.0351 (14) | |
C29 | 0.1567 (5) | 0.6355 (4) | 0.3881 (4) | 0.0331 (13) | |
C30 | 0.2842 (5) | 0.6228 (4) | 0.3857 (4) | 0.0339 (13) | |
C31 | 0.2258 (5) | 0.7624 (4) | 0.3964 (4) | 0.0350 (14) | |
C32 | 0.2231 (5) | 0.8591 (4) | 0.3999 (4) | 0.0352 (13) | |
C33 | 0.1126 (6) | 0.9170 (4) | 0.4012 (5) | 0.0473 (17) | |
H33 | 0.0375 | 0.8946 | 0.4015 | 0.057* | |
C34 | 0.3305 (6) | 0.8973 (4) | 0.4005 (5) | 0.0496 (18) | |
H34 | 0.4076 | 0.8611 | 0.3999 | 0.060* | |
C35 | 0.1139 (6) | 1.0081 (4) | 0.4020 (5) | 0.0473 (16) | |
H35 | 0.0381 | 1.0459 | 0.4027 | 0.057* | |
C36 | 0.3231 (6) | 0.9892 (4) | 0.4019 (5) | 0.0496 (17) | |
H36 | 0.3963 | 1.0132 | 0.4030 | 0.060* | |
C37 | 0.2574 (5) | 0.2445 (4) | −0.0805 (4) | 0.0342 (13) | |
C38 | 0.2548 (5) | 0.2308 (4) | −0.1743 (4) | 0.0326 (13) | |
C39 | 0.1502 (5) | 0.1949 (4) | −0.1841 (4) | 0.0455 (16) | |
H39 | 0.0821 | 0.1800 | −0.1320 | 0.055* | |
C40 | 0.1469 (6) | 0.1813 (4) | −0.2709 (4) | 0.0467 (16) | |
H40 | 0.0764 | 0.1576 | −0.2770 | 0.056* | |
C41 | 0.2485 (5) | 0.2030 (4) | −0.3489 (4) | 0.0312 (13) | |
C42 | 0.2449 (6) | 0.1920 (4) | −0.4448 (4) | 0.0371 (14) | |
C43 | 0.3515 (5) | 0.2412 (4) | −0.3402 (4) | 0.0408 (15) | |
H43 | 0.4186 | 0.2579 | −0.3926 | 0.049* | |
C44 | 0.3536 (5) | 0.2544 (4) | −0.2528 (4) | 0.0406 (15) | |
H44 | 0.4230 | 0.2797 | −0.2469 | 0.049* | |
C45 | 0.5348 (5) | 0.1564 (4) | 0.1885 (5) | 0.0363 (14) | |
C46 | 0.6565 (5) | 0.1580 (3) | 0.2175 (4) | 0.0304 (12) | |
C47 | 0.7718 (5) | 0.1719 (4) | 0.1486 (4) | 0.0371 (14) | |
H47 | 0.7752 | 0.1725 | 0.0861 | 0.044* | |
C48 | 0.8801 (5) | 0.1848 (4) | 0.1727 (4) | 0.0349 (13) | |
H48 | 0.9560 | 0.1946 | 0.1264 | 0.042* | |
C49 | 0.8762 (5) | 0.1830 (3) | 0.2657 (4) | 0.0319 (13) | |
C50 | 0.7636 (5) | 0.1664 (4) | 0.3343 (4) | 0.0384 (14) | |
H50 | 0.7609 | 0.1640 | 0.3971 | 0.046* | |
C51 | 0.6545 (5) | 0.1534 (4) | 0.3101 (4) | 0.0405 (14) | |
H51 | 0.5796 | 0.1414 | 0.3568 | 0.049* | |
C52 | 0.9942 (5) | 0.1986 (4) | 0.2921 (4) | 0.0351 (14) | |
N1 | 0.4282 (4) | −0.6191 (3) | 0.1082 (4) | 0.0374 (12) | |
N2 | 0.1725 (4) | −0.5971 (3) | 0.1170 (4) | 0.0414 (13) | |
N3 | 0.3858 (4) | −0.2950 (3) | 0.1310 (3) | 0.0357 (11) | |
H3A | 0.4601 | −0.2831 | 0.1318 | 0.043* | |
N4 | 0.1786 (4) | −0.2735 (3) | 0.1305 (4) | 0.0365 (12) | |
N9 | 0.2942 (5) | 0.0511 (3) | 0.1098 (4) | 0.0500 (14) | |
N10 | 0.2168 (5) | 1.0452 (3) | 0.4017 (3) | 0.0406 (12) | |
O1 | 0.3628 (4) | 0.2633 (3) | −0.0702 (3) | 0.0470 (11) | |
O2 | 0.1613 (4) | 0.2351 (3) | −0.0135 (3) | 0.0476 (11) | |
O3 | 0.1348 (3) | 0.2068 (3) | −0.4647 (3) | 0.0391 (10) | |
O4 | 0.3458 (4) | 0.1743 (3) | −0.5021 (3) | 0.0439 (10) | |
O5 | 0.4314 (4) | 0.1563 (3) | 0.2500 (3) | 0.0502 (11) | |
O6 | 0.5416 (3) | 0.1629 (3) | 0.1023 (3) | 0.0403 (10) | |
O7 | 1.0982 (4) | 0.1948 (3) | 0.2319 (3) | 0.0588 (13) | |
O8 | 0.9841 (4) | 0.2119 (3) | 0.3734 (3) | 0.0415 (10) | |
N5 | 0.0910 (4) | 0.4067 (3) | 0.3739 (3) | 0.0366 (11) | |
N6 | 0.3432 (4) | 0.3761 (3) | 0.3748 (4) | 0.0455 (13) | |
N7 | 0.3281 (4) | 0.7025 (3) | 0.3900 (3) | 0.0371 (12) | |
N8 | 0.1199 (4) | 0.7250 (3) | 0.3949 (3) | 0.0361 (12) | |
H8A | 0.0444 | 0.7525 | 0.3976 | 0.043* | |
Pb1 | 0.306872 (18) | 0.228293 (14) | 0.106810 (15) | 0.03121 (7) | |
Pb2 | 0.216110 (19) | 0.227339 (14) | 0.365684 (15) | 0.03315 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.026 (3) | 0.050 (4) | 0.104 (6) | −0.008 (3) | −0.021 (4) | −0.028 (4) |
C2 | 0.036 (4) | 0.039 (4) | 0.100 (6) | −0.007 (3) | −0.022 (4) | −0.029 (4) |
C3 | 0.033 (3) | 0.026 (3) | 0.066 (4) | −0.002 (3) | −0.017 (3) | −0.003 (3) |
C4 | 0.028 (3) | 0.049 (4) | 0.075 (5) | −0.003 (3) | −0.019 (3) | −0.011 (4) |
C5 | 0.034 (3) | 0.025 (3) | 0.042 (4) | −0.009 (2) | −0.008 (3) | −0.011 (3) |
C6 | 0.035 (3) | 0.033 (3) | 0.057 (4) | −0.011 (3) | −0.017 (3) | −0.004 (3) |
C7 | 0.031 (3) | 0.027 (3) | 0.037 (3) | −0.008 (2) | −0.010 (3) | −0.008 (3) |
C8 | 0.035 (3) | 0.019 (3) | 0.045 (4) | −0.006 (2) | −0.012 (3) | −0.005 (3) |
C9 | 0.038 (3) | 0.027 (3) | 0.044 (4) | −0.005 (3) | −0.014 (3) | −0.007 (3) |
C10 | 0.034 (3) | 0.039 (4) | 0.085 (5) | −0.002 (3) | −0.013 (3) | −0.026 (4) |
C11 | 0.034 (3) | 0.026 (3) | 0.048 (4) | −0.005 (2) | −0.009 (3) | −0.010 (3) |
C12 | 0.035 (3) | 0.027 (3) | 0.047 (4) | −0.008 (3) | −0.008 (3) | −0.012 (3) |
C13 | 0.032 (3) | 0.029 (3) | 0.046 (4) | −0.006 (2) | −0.001 (3) | −0.015 (3) |
C14 | 0.041 (4) | 0.033 (4) | 0.173 (9) | 0.004 (3) | −0.024 (5) | −0.036 (5) |
C15 | 0.039 (4) | 0.036 (4) | 0.149 (8) | −0.007 (3) | −0.027 (5) | −0.033 (5) |
C16 | 0.037 (3) | 0.023 (3) | 0.050 (4) | −0.006 (3) | −0.004 (3) | −0.014 (3) |
C17 | 0.056 (4) | 0.029 (4) | 0.126 (7) | −0.002 (3) | −0.047 (5) | −0.028 (4) |
C18 | 0.059 (5) | 0.037 (4) | 0.122 (7) | −0.004 (3) | −0.041 (5) | −0.034 (4) |
C19 | 0.041 (4) | 0.037 (4) | 0.115 (7) | 0.007 (3) | −0.017 (4) | −0.034 (4) |
C20 | 0.033 (3) | 0.037 (4) | 0.101 (6) | 0.004 (3) | −0.016 (4) | −0.024 (4) |
C21 | 0.036 (3) | 0.040 (4) | 0.076 (5) | −0.009 (3) | −0.009 (3) | −0.018 (4) |
C22 | 0.033 (3) | 0.031 (3) | 0.044 (4) | −0.004 (3) | −0.002 (3) | −0.016 (3) |
C23 | 0.039 (3) | 0.029 (3) | 0.035 (3) | −0.008 (3) | −0.004 (3) | −0.013 (3) |
C24 | 0.038 (3) | 0.029 (3) | 0.035 (3) | −0.004 (3) | −0.006 (3) | −0.014 (3) |
C25 | 0.054 (4) | 0.035 (4) | 0.056 (4) | −0.016 (3) | −0.016 (3) | −0.012 (3) |
C26 | 0.035 (3) | 0.044 (4) | 0.068 (5) | −0.004 (3) | −0.018 (3) | −0.021 (3) |
C27 | 0.041 (3) | 0.030 (3) | 0.064 (4) | 0.001 (3) | −0.022 (3) | −0.015 (3) |
C28 | 0.036 (3) | 0.035 (3) | 0.037 (3) | −0.007 (3) | −0.002 (3) | −0.017 (3) |
C29 | 0.032 (3) | 0.027 (3) | 0.039 (3) | −0.009 (2) | −0.004 (3) | −0.009 (3) |
C30 | 0.038 (3) | 0.028 (3) | 0.038 (3) | −0.008 (3) | −0.006 (3) | −0.013 (3) |
C31 | 0.039 (3) | 0.024 (3) | 0.044 (4) | −0.009 (3) | −0.003 (3) | −0.013 (3) |
C32 | 0.044 (3) | 0.029 (3) | 0.033 (3) | −0.007 (3) | −0.004 (3) | −0.010 (3) |
C33 | 0.044 (4) | 0.029 (3) | 0.073 (5) | −0.014 (3) | −0.014 (3) | −0.011 (3) |
C34 | 0.033 (3) | 0.028 (3) | 0.089 (5) | −0.003 (3) | −0.011 (3) | −0.019 (3) |
C35 | 0.045 (4) | 0.028 (3) | 0.067 (5) | −0.004 (3) | −0.010 (3) | −0.010 (3) |
C36 | 0.044 (4) | 0.039 (4) | 0.071 (5) | −0.016 (3) | −0.007 (3) | −0.022 (3) |
C37 | 0.030 (3) | 0.032 (3) | 0.041 (4) | −0.005 (2) | −0.010 (3) | −0.007 (3) |
C38 | 0.030 (3) | 0.037 (3) | 0.037 (3) | −0.006 (2) | −0.014 (3) | −0.012 (3) |
C39 | 0.029 (3) | 0.071 (5) | 0.037 (4) | −0.017 (3) | −0.001 (3) | −0.012 (3) |
C40 | 0.039 (3) | 0.072 (5) | 0.039 (4) | −0.021 (3) | −0.014 (3) | −0.016 (3) |
C41 | 0.031 (3) | 0.028 (3) | 0.039 (3) | 0.001 (2) | −0.014 (3) | −0.009 (3) |
C42 | 0.040 (4) | 0.030 (3) | 0.047 (4) | −0.008 (3) | −0.017 (3) | −0.009 (3) |
C43 | 0.033 (3) | 0.049 (4) | 0.038 (4) | −0.005 (3) | −0.005 (3) | −0.008 (3) |
C44 | 0.035 (3) | 0.052 (4) | 0.041 (4) | −0.012 (3) | −0.011 (3) | −0.014 (3) |
C45 | 0.035 (3) | 0.024 (3) | 0.051 (4) | −0.005 (2) | −0.014 (3) | −0.005 (3) |
C46 | 0.028 (3) | 0.026 (3) | 0.039 (3) | −0.003 (2) | −0.013 (3) | −0.005 (3) |
C47 | 0.038 (3) | 0.043 (4) | 0.034 (3) | 0.001 (3) | −0.012 (3) | −0.013 (3) |
C48 | 0.024 (3) | 0.040 (3) | 0.038 (3) | −0.006 (2) | −0.001 (3) | −0.007 (3) |
C49 | 0.030 (3) | 0.025 (3) | 0.040 (3) | −0.005 (2) | −0.012 (3) | −0.002 (3) |
C50 | 0.040 (3) | 0.044 (4) | 0.031 (3) | −0.003 (3) | −0.009 (3) | −0.009 (3) |
C51 | 0.030 (3) | 0.048 (4) | 0.042 (4) | −0.014 (3) | −0.004 (3) | −0.006 (3) |
C52 | 0.036 (3) | 0.027 (3) | 0.045 (4) | −0.003 (2) | −0.016 (3) | −0.005 (3) |
N1 | 0.036 (3) | 0.027 (3) | 0.053 (3) | −0.006 (2) | −0.016 (2) | −0.008 (2) |
N2 | 0.037 (3) | 0.026 (3) | 0.068 (4) | −0.003 (2) | −0.020 (3) | −0.014 (3) |
N3 | 0.034 (3) | 0.033 (3) | 0.045 (3) | −0.013 (2) | −0.008 (2) | −0.013 (2) |
N4 | 0.032 (3) | 0.024 (2) | 0.056 (3) | −0.004 (2) | −0.007 (2) | −0.017 (2) |
N9 | 0.047 (3) | 0.031 (3) | 0.079 (4) | −0.009 (2) | −0.015 (3) | −0.023 (3) |
N10 | 0.045 (3) | 0.029 (3) | 0.044 (3) | −0.008 (2) | −0.003 (2) | −0.007 (2) |
O1 | 0.039 (2) | 0.068 (3) | 0.044 (3) | −0.018 (2) | −0.011 (2) | −0.021 (2) |
O2 | 0.034 (2) | 0.077 (3) | 0.037 (2) | −0.015 (2) | −0.004 (2) | −0.021 (2) |
O3 | 0.033 (2) | 0.051 (3) | 0.038 (2) | −0.0044 (19) | −0.0090 (19) | −0.019 (2) |
O4 | 0.035 (2) | 0.058 (3) | 0.040 (3) | 0.000 (2) | −0.005 (2) | −0.023 (2) |
O5 | 0.028 (2) | 0.070 (3) | 0.050 (3) | −0.006 (2) | −0.007 (2) | −0.008 (2) |
O6 | 0.036 (2) | 0.042 (2) | 0.050 (3) | −0.0034 (18) | −0.017 (2) | −0.017 (2) |
O7 | 0.037 (3) | 0.094 (4) | 0.047 (3) | −0.019 (2) | −0.007 (2) | −0.014 (3) |
O8 | 0.040 (2) | 0.043 (2) | 0.048 (3) | −0.0073 (19) | −0.016 (2) | −0.015 (2) |
N5 | 0.037 (3) | 0.029 (3) | 0.049 (3) | −0.008 (2) | −0.013 (2) | −0.011 (2) |
N6 | 0.034 (3) | 0.027 (3) | 0.077 (4) | −0.001 (2) | −0.010 (3) | −0.019 (3) |
N7 | 0.034 (3) | 0.028 (3) | 0.050 (3) | −0.006 (2) | −0.005 (2) | −0.014 (2) |
N8 | 0.036 (3) | 0.024 (2) | 0.051 (3) | −0.003 (2) | −0.010 (2) | −0.015 (2) |
Pb1 | 0.03078 (12) | 0.03135 (13) | 0.03598 (14) | −0.00628 (9) | −0.01026 (10) | −0.01111 (10) |
Pb2 | 0.03446 (13) | 0.03374 (13) | 0.03622 (14) | −0.00678 (10) | −0.01022 (10) | −0.01278 (10) |
C1—C10 | 1.369 (7) | C31—C32 | 1.465 (7) |
C1—C2 | 1.381 (8) | C32—C33 | 1.376 (8) |
C1—H1 | 0.9300 | C32—C34 | 1.383 (8) |
C2—N2 | 1.326 (7) | C33—C35 | 1.377 (8) |
C2—H2 | 0.9300 | C33—H33 | 0.9300 |
C3—N1 | 1.330 (7) | C34—C36 | 1.379 (8) |
C3—C4 | 1.383 (8) | C34—H34 | 0.9300 |
C3—H3 | 0.9300 | C35—N10 | 1.324 (7) |
C4—C6 | 1.367 (8) | C35—H35 | 0.9300 |
C4—H4 | 0.9300 | C36—N10 | 1.328 (7) |
C5—N3 | 1.362 (6) | C36—H36 | 0.9300 |
C5—C13 | 1.381 (7) | C37—O2 | 1.240 (7) |
C5—C7 | 1.422 (7) | C37—O1 | 1.281 (6) |
C6—C7 | 1.399 (7) | C37—C38 | 1.485 (8) |
C6—H6 | 0.9300 | C38—C44 | 1.379 (8) |
C7—C8 | 1.407 (7) | C38—C39 | 1.388 (7) |
C8—N1 | 1.354 (7) | C39—C40 | 1.383 (8) |
C8—C9 | 1.477 (7) | C39—H39 | 0.9300 |
C9—N2 | 1.350 (6) | C40—C41 | 1.389 (8) |
C9—C11 | 1.418 (7) | C40—H40 | 0.9300 |
C10—C11 | 1.388 (7) | C41—C43 | 1.385 (7) |
C10—H10 | 0.9300 | C41—C42 | 1.505 (8) |
C11—C13 | 1.428 (7) | C42—O4 | 1.239 (7) |
C12—N4 | 1.338 (6) | C42—O3 | 1.290 (6) |
C12—N3 | 1.351 (6) | C42—Pb2i | 2.870 (6) |
C12—C16 | 1.466 (7) | C43—C44 | 1.385 (8) |
C13—N4 | 1.384 (7) | C43—H43 | 0.9300 |
C14—N9 | 1.325 (8) | C44—H44 | 0.9300 |
C14—C15 | 1.377 (8) | C45—O5 | 1.249 (7) |
C14—H14 | 0.9300 | C45—O6 | 1.261 (7) |
C15—C16 | 1.358 (8) | C45—C46 | 1.511 (7) |
C15—H15 | 0.9300 | C46—C51 | 1.374 (8) |
C16—C17 | 1.365 (8) | C46—C47 | 1.401 (8) |
C17—C18 | 1.369 (8) | C47—C48 | 1.379 (7) |
C17—H17 | 0.9300 | C47—H47 | 0.9300 |
C18—N9 | 1.308 (8) | C48—C49 | 1.384 (7) |
C18—H18 | 0.9300 | C48—H48 | 0.9300 |
C19—N6 | 1.331 (7) | C49—C50 | 1.383 (8) |
C19—C20 | 1.391 (8) | C49—C52 | 1.511 (7) |
C19—H19 | 0.9300 | C50—C51 | 1.389 (7) |
C20—C21 | 1.367 (8) | C50—H50 | 0.9300 |
C20—H20 | 0.9300 | C51—H51 | 0.9300 |
C21—C22 | 1.398 (8) | C52—O7 | 1.249 (7) |
C21—H21 | 0.9300 | C52—O8 | 1.260 (7) |
C22—C23 | 1.411 (7) | N3—H3A | 0.8600 |
C22—C30 | 1.444 (7) | Pb1—O1 | 2.508 (4) |
C23—N6 | 1.370 (7) | Pb1—O2 | 2.691 (4) |
C23—C24 | 1.458 (7) | Pb1—O5 | 2.772 (4) |
C24—N5 | 1.360 (6) | Pb1—O6 | 2.591 (4) |
C24—C28 | 1.413 (7) | Pb1—O7ii | 2.555 (4) |
C25—N5 | 1.324 (7) | Pb1—N1iii | 2.824 (4) |
C25—C26 | 1.387 (8) | Pb1—N2iii | 2.829 (4) |
C25—H25 | 0.9300 | Pb1—N9 | 2.681 (5) |
C26—C27 | 1.363 (7) | Pb2—O3iv | 2.424 (4) |
C26—H26 | 0.9300 | Pb2—O4iv | 2.651 (4) |
C27—C28 | 1.394 (7) | Pb2—O5 | 2.761 (4) |
C27—H27 | 0.9300 | Pb2—O7ii | 2.836 (4) |
C28—C29 | 1.433 (7) | Pb2—O8ii | 2.545 (4) |
C29—N8 | 1.367 (6) | Pb2—N5 | 2.853 (4) |
C29—C30 | 1.367 (7) | Pb2—N6 | 2.852 (4) |
C30—N7 | 1.378 (6) | Pb2—N10v | 2.662 (5) |
C31—N7 | 1.323 (7) | N8—H8A | 0.8600 |
C31—N8 | 1.367 (6) | ||
C10—C1—C2 | 118.9 (5) | C41—C42—Pb2i | 163.3 (4) |
C10—C1—H1 | 120.6 | C44—C43—C41 | 119.4 (6) |
C2—C1—H1 | 120.6 | C44—C43—H43 | 120.3 |
N2—C2—C1 | 124.0 (5) | C41—C43—H43 | 120.3 |
N2—C2—H2 | 118.0 | C38—C44—C43 | 121.3 (5) |
C1—C2—H2 | 118.0 | C38—C44—H44 | 119.3 |
N1—C3—C4 | 123.2 (5) | C43—C44—H44 | 119.3 |
N1—C3—H3 | 118.4 | O5—C45—O6 | 123.2 (5) |
C4—C3—H3 | 118.4 | O5—C45—C46 | 118.2 (5) |
C6—C4—C3 | 119.9 (5) | O6—C45—C46 | 118.3 (5) |
C6—C4—H4 | 120.0 | C51—C46—C47 | 118.9 (5) |
C3—C4—H4 | 120.0 | C51—C46—C45 | 120.9 (5) |
N3—C5—C13 | 105.5 (5) | C47—C46—C45 | 120.0 (5) |
N3—C5—C7 | 131.0 (5) | C48—C47—C46 | 120.6 (5) |
C13—C5—C7 | 123.5 (5) | C48—C47—H47 | 119.7 |
C4—C6—C7 | 118.3 (5) | C46—C47—H47 | 119.7 |
C4—C6—H6 | 120.9 | C47—C48—C49 | 120.1 (5) |
C7—C6—H6 | 120.9 | C47—C48—H48 | 119.9 |
C6—C7—C8 | 118.8 (5) | C49—C48—H48 | 119.9 |
C6—C7—C5 | 124.0 (5) | C50—C49—C48 | 119.5 (5) |
C8—C7—C5 | 117.1 (5) | C50—C49—C52 | 120.3 (5) |
N1—C8—C7 | 121.8 (5) | C48—C49—C52 | 120.3 (5) |
N1—C8—C9 | 117.9 (5) | C49—C50—C51 | 120.4 (5) |
C7—C8—C9 | 120.2 (5) | C49—C50—H50 | 119.8 |
N2—C9—C11 | 122.3 (5) | C51—C50—H50 | 119.8 |
N2—C9—C8 | 117.2 (5) | C46—C51—C50 | 120.5 (5) |
C11—C9—C8 | 120.4 (5) | C46—C51—H51 | 119.8 |
C1—C10—C11 | 119.5 (6) | C50—C51—H51 | 119.8 |
C1—C10—H10 | 120.2 | O7—C52—O8 | 123.5 (5) |
C11—C10—H10 | 120.2 | O7—C52—C49 | 117.1 (5) |
C10—C11—C9 | 117.7 (5) | O8—C52—C49 | 119.3 (5) |
C10—C11—C13 | 124.7 (5) | C3—N1—C8 | 118.0 (5) |
C9—C11—C13 | 117.6 (5) | C2—N2—C9 | 117.5 (5) |
N4—C12—N3 | 112.6 (4) | C12—N3—C5 | 107.6 (4) |
N4—C12—C16 | 124.9 (5) | C12—N3—H3A | 126.2 |
N3—C12—C16 | 122.5 (5) | C5—N3—H3A | 126.2 |
C5—C13—N4 | 110.8 (5) | C12—N4—C13 | 103.6 (4) |
C5—C13—C11 | 121.1 (5) | C18—N9—C14 | 116.0 (5) |
N4—C13—C11 | 128.0 (5) | C18—N9—Pb1 | 119.9 (4) |
N9—C14—C15 | 123.5 (6) | C14—N9—Pb1 | 123.9 (4) |
N9—C14—H14 | 118.3 | C35—N10—C36 | 116.6 (5) |
C15—C14—H14 | 118.3 | C35—N10—Pb2iii | 119.6 (4) |
C16—C15—C14 | 120.1 (6) | C36—N10—Pb2iii | 122.5 (4) |
C16—C15—H15 | 120.0 | C37—O1—Pb1 | 97.5 (3) |
C14—C15—H15 | 120.0 | C37—O2—Pb1 | 89.9 (3) |
C15—C16—C17 | 116.2 (5) | C42—O3—Pb2i | 96.4 (3) |
C15—C16—C12 | 121.8 (5) | C42—O4—Pb2i | 87.2 (3) |
C17—C16—C12 | 122.0 (5) | C45—O5—Pb2 | 157.8 (4) |
C16—C17—C18 | 120.4 (6) | C45—O5—Pb1 | 88.6 (3) |
C16—C17—H17 | 119.8 | Pb2—O5—Pb1 | 85.34 (11) |
C18—C17—H17 | 119.8 | C45—O6—Pb1 | 96.8 (3) |
N9—C18—C17 | 123.8 (6) | C52—O7—Pb1vi | 166.2 (4) |
N9—C18—H18 | 118.1 | C52—O8—Pb2vi | 100.9 (3) |
C17—C18—H18 | 118.1 | C25—N5—C24 | 117.5 (5) |
N6—C19—C20 | 123.9 (6) | C25—N5—Pb2 | 119.0 (4) |
N6—C19—H19 | 118.0 | C24—N5—Pb2 | 123.5 (3) |
C20—C19—H19 | 118.0 | C19—N6—C23 | 117.6 (5) |
C21—C20—C19 | 119.2 (6) | C19—N6—Pb2 | 118.2 (4) |
C21—C20—H20 | 120.4 | C23—N6—Pb2 | 124.2 (3) |
C19—C20—H20 | 120.4 | C31—N7—C30 | 104.4 (4) |
C20—C21—C22 | 119.0 (5) | C29—N8—C31 | 107.1 (4) |
C20—C21—H21 | 120.5 | C29—N8—H8A | 126.5 |
C22—C21—H21 | 120.5 | C31—N8—H8A | 126.5 |
C21—C22—C23 | 118.9 (5) | O1—Pb1—O7ii | 132.98 (13) |
C21—C22—C30 | 124.3 (5) | O1—Pb1—O6 | 89.16 (13) |
C23—C22—C30 | 116.9 (5) | O7ii—Pb1—O6 | 131.70 (14) |
N6—C23—C22 | 121.5 (5) | O1—Pb1—N9 | 90.13 (15) |
N6—C23—C24 | 116.7 (5) | O7ii—Pb1—N9 | 78.78 (16) |
C22—C23—C24 | 121.9 (5) | O6—Pb1—N9 | 78.89 (14) |
N5—C24—C28 | 121.5 (5) | O1—Pb1—O2 | 49.80 (12) |
N5—C24—C23 | 118.6 (5) | O7ii—Pb1—O2 | 83.23 (12) |
C28—C24—C23 | 119.9 (5) | O6—Pb1—O2 | 130.95 (12) |
N5—C25—C26 | 124.4 (5) | N9—Pb1—O2 | 76.17 (15) |
N5—C25—H25 | 117.8 | O1—Pb1—O5 | 137.61 (12) |
C26—C25—H25 | 117.8 | O7ii—Pb1—O5 | 86.88 (12) |
C27—C26—C25 | 118.8 (5) | O6—Pb1—O5 | 48.49 (12) |
C27—C26—H26 | 120.6 | N9—Pb1—O5 | 83.81 (15) |
C25—C26—H26 | 120.6 | O2—Pb1—O5 | 159.04 (13) |
C26—C27—C28 | 119.1 (5) | O1—Pb1—N1iii | 91.40 (13) |
C26—C27—H27 | 120.5 | O7ii—Pb1—N1iii | 117.17 (15) |
C28—C27—H27 | 120.5 | O6—Pb1—N1iii | 76.11 (12) |
C27—C28—C24 | 118.7 (5) | N9—Pb1—N1iii | 154.93 (14) |
C27—C28—C29 | 124.7 (5) | O2—Pb1—N1iii | 122.69 (13) |
C24—C28—C29 | 116.5 (5) | O5—Pb1—N1iii | 78.27 (13) |
N8—C29—C30 | 105.6 (5) | O1—Pb1—N2iii | 93.17 (14) |
N8—C29—C28 | 130.3 (5) | O7ii—Pb1—N2iii | 75.12 (15) |
C30—C29—C28 | 124.1 (5) | O6—Pb1—N2iii | 133.84 (12) |
C29—C30—N7 | 111.0 (5) | N9—Pb1—N2iii | 147.09 (14) |
C29—C30—C22 | 120.6 (5) | O2—Pb1—N2iii | 81.14 (13) |
N7—C30—C22 | 128.3 (5) | O5—Pb1—N2iii | 114.08 (13) |
N7—C31—N8 | 111.9 (4) | N1iii—Pb1—N2iii | 57.75 (13) |
N7—C31—C32 | 125.8 (5) | O3iv—Pb2—O8ii | 82.40 (13) |
N8—C31—C32 | 122.2 (5) | O3iv—Pb2—O4iv | 51.73 (12) |
C33—C32—C34 | 116.7 (5) | O8ii—Pb2—O4iv | 130.42 (13) |
C33—C32—C31 | 121.0 (5) | O3iv—Pb2—N10v | 83.64 (14) |
C34—C32—C31 | 122.3 (5) | O8ii—Pb2—N10v | 79.47 (14) |
C32—C33—C35 | 119.7 (6) | O4iv—Pb2—N10v | 77.92 (14) |
C32—C33—H33 | 120.2 | O3iv—Pb2—O5 | 134.04 (12) |
C35—C33—H33 | 120.2 | O8ii—Pb2—O5 | 126.98 (12) |
C36—C34—C32 | 119.9 (6) | O4iv—Pb2—O5 | 85.16 (12) |
C36—C34—H34 | 120.1 | N10v—Pb2—O5 | 70.88 (14) |
C32—C34—H34 | 120.1 | O3iv—Pb2—O7ii | 128.71 (12) |
N10—C35—C33 | 123.8 (6) | O8ii—Pb2—O7ii | 48.15 (12) |
N10—C35—H35 | 118.1 | O4iv—Pb2—O7ii | 153.24 (13) |
C33—C35—H35 | 118.1 | N10v—Pb2—O7ii | 75.75 (15) |
N10—C36—C34 | 123.3 (5) | O5—Pb2—O7ii | 81.85 (12) |
N10—C36—H36 | 118.3 | O3iv—Pb2—N6 | 86.80 (14) |
C34—C36—H36 | 118.3 | O8ii—Pb2—N6 | 132.49 (13) |
O2—C37—O1 | 121.1 (5) | O4iv—Pb2—N6 | 69.75 (14) |
O2—C37—C38 | 120.8 (5) | N10v—Pb2—N6 | 144.92 (15) |
O1—C37—C38 | 118.1 (5) | O5—Pb2—N6 | 92.72 (13) |
C44—C38—C39 | 119.0 (5) | O7ii—Pb2—N6 | 133.96 (15) |
C44—C38—C37 | 121.3 (5) | O3iv—Pb2—N5 | 80.93 (13) |
C39—C38—C37 | 119.7 (5) | O8ii—Pb2—N5 | 75.59 (12) |
C40—C39—C38 | 120.3 (6) | O4iv—Pb2—N5 | 109.41 (12) |
C40—C39—H39 | 119.8 | N10v—Pb2—N5 | 152.12 (14) |
C38—C39—H39 | 119.8 | O5—Pb2—N5 | 135.25 (13) |
C39—C40—C41 | 120.2 (5) | O7ii—Pb2—N5 | 96.20 (13) |
C39—C40—H40 | 119.9 | N6—Pb2—N5 | 57.02 (13) |
C41—C40—H40 | 119.9 | O3iv—Pb2—C42iv | 26.53 (14) |
C43—C41—C40 | 119.7 (5) | O8ii—Pb2—C42iv | 108.23 (15) |
C43—C41—C42 | 119.0 (5) | O4iv—Pb2—C42iv | 25.55 (13) |
C40—C41—C42 | 121.1 (5) | N10v—Pb2—C42iv | 82.83 (15) |
O4—C42—O3 | 123.0 (5) | O5—Pb2—C42iv | 110.32 (15) |
O4—C42—C41 | 119.8 (5) | O7ii—Pb2—C42iv | 150.37 (14) |
O3—C42—C41 | 117.0 (5) | N6—Pb2—C42iv | 73.97 (16) |
O4—C42—Pb2i | 67.3 (3) | N5—Pb2—C42iv | 93.25 (15) |
O3—C42—Pb2i | 57.1 (3) |
Symmetry codes: (i) x, y, z−1; (ii) x−1, y, z; (iii) x, y+1, z; (iv) x, y, z+1; (v) x, y−1, z; (vi) x+1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3A···O1vii | 0.86 | 1.93 | 2.720 (6) | 151 |
N8—H8A···O3viii | 0.86 | 2.02 | 2.822 (6) | 155 |
Symmetry codes: (vii) −x+1, −y, −z; (viii) −x, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Pb2(C8H4O4)2(C18H11N5)2] |
Mr | 1337.24 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 10.9066 (7), 15.0537 (10), 15.0663 (10) |
α, β, γ (°) | 75.890 (1), 74.199 (1), 81.399 (1) |
V (Å3) | 2299.2 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 7.38 |
Crystal size (mm) | 0.27 × 0.22 × 0.16 |
Data collection | |
Diffractometer | Bruker APEX diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.56, 0.77 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12743, 7984, 6315 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.070, 0.98 |
No. of reflections | 7984 |
No. of parameters | 649 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.27, −0.60 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008), publCIF (Westrip, 2010).
Pb1—O1 | 2.508 (4) | Pb2—O3iii | 2.424 (4) |
Pb1—O2 | 2.691 (4) | Pb2—O4iii | 2.651 (4) |
Pb1—O5 | 2.772 (4) | Pb2—O5 | 2.761 (4) |
Pb1—O6 | 2.591 (4) | Pb2—O7i | 2.836 (4) |
Pb1—O7i | 2.555 (4) | Pb2—O8i | 2.545 (4) |
Pb1—N1ii | 2.824 (4) | Pb2—N5 | 2.853 (4) |
Pb1—N2ii | 2.829 (4) | Pb2—N6 | 2.852 (4) |
Pb1—N9 | 2.681 (5) | Pb2—N10iv | 2.662 (5) |
Symmetry codes: (i) x−1, y, z; (ii) x, y+1, z; (iii) x, y, z+1; (iv) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3A···O1v | 0.86 | 1.93 | 2.720 (6) | 151.2 |
N8—H8A···O3vi | 0.86 | 2.02 | 2.822 (6) | 154.5 |
Symmetry codes: (v) −x+1, −y, −z; (vi) −x, −y+1, −z. |
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The design and synthesis of coordination polymers with infinite three-dimensional framework structures has been an area of rapid growth in recent years, owing to the potential of these polymers in various applications such as catalysis, electrical conductivity, host–guest chemistry and magnetism (Ockwig et al., 2005; O'Keeffe et al., 2008; Yang et al., 2008). In this regard, a great many coordination polymers with mineral topologies, including CdSO4 (cds), NbO (nbo), Pt3O4 (pto), pyrite (pyr), quartz (qtz), rutile (rto), diamond (diaz) and sodalite (sod), have provided experimental examples of these theoretical topologies (Batten, 2001; Batten & Robson, 1998; Carlucci et al., 2003). As a result, the design and construction of diverse topological networks has received much attention (Eddaoudi et al., 2001). The topologies of coordination polymers can often be controlled and modified by the coordination geometry preferred by the metal ion and the chemical structure of the organic ligand (Long et al., 2002). It is well known that careful selection of a suitable organic ligand with certain features is helpful for constructing coordination polymers with desirable properties. So far, the combination of bridging carboxylates, 1,10-phenanthroline-like (phen-like) chelating ligands and metal ions has generated many interesting coordination architectures (Wang et al., 2008; Qiao et al., 2008; Kong et al., 2009). Unfortunately, owing to the termination effect of chelating phen-like ligands, such coordination polymers containing both polycarboxylates and phen-like ligands are usually only one- or two-dimensional (Wang et al., 2009, 2010; Qiao et al., 2009). High-dimensional complexes based on dicarboxylate and phen-like ligands have rarely been reported (Yang et al., 2007). Here, we have selected the benzene-1,4-dicarboxylate dianion (1,4-bdc) as an organic linker and 6-(pyridin-4-yl)-5H-cyclopenta[f][1,10]phenanthroline (L) as an N-donor ligand, generating a new two-fold interpenetrating coordination polymer with α-Po topology, [Pb2(L)2(1,4-bdc)2]n, (I).
The asymmetric unit of (I) contains two PbII atoms, two 1,4-bdc dianions and two L ligands (Fig. 1). Each PbII atom is eight-coordinated by three N atoms from two different L ligands and five carboxylate O atoms from three different 1,4-bdc dianions. The Pb—O distances (Table 1) are comparable with those observed for [Pb(eedb)(L')(DMF)] (eedb is 4,4'-ethylenedibenzoate, L' is pyrazino[2,3-f][1,10]phenanthroline and DMF is dimethylformamide) (Qiao et al., 2009). The two independent 1,4-bdc dianions show different coordination modes. For convenience, the 1,4-bdc anions containing atoms O1–O4 and O5–O8 are designated 1,4-bdc1 and 1,4-bdc2, respectively. Each 1,4-bdc1 anion coordinates to two PbII atoms in a chelating bis-bidentate mode. Carboxylate atoms O1 and O2 chelate Pb1, while atoms O3 and O4 chelate Pb2v [symmetry code: (v) x, y, z - 1]. Each carboxylate group of the 1,4-bdc2 anion connects two PbII atoms in a chelating-bridging tridentate mode to form a dimer. Carboxylate atoms O5 and O6 chelate Pb1, while atom O5 bridges simultaneously to Pb2. The other O atoms, O7 and O8, chelate Pb2vi, while atom O7 bridges simultaneously to Pb1vi [symmetry code: (vi) 1 + x, y, z]. The distance between the PbII atoms in the dinuclear unit is 3.751 (3) Å.
Neighbouring dinuclear units are connected together by the aromatic backbone of both 1,4-bdc dianions and the L ligands. Each dinuclear PbII unit is surrounded by eight organic ligands: four bridging 1,4-bdc dianions and four bridging L ligands. Although each dinuclear PbII unit is ligated by eight bridging ligands, it is almost [Please check rephrasing] linked to six nearest neighbours, because two pairs of L ligands form two `double bridges' (Fig. 2). Each dinuclear unit therefore acts as a six-connecting node, and the overall three-dimensional framework topology is that of α-polonium (Fig. 2).
The most striking feature of (I) is that two identical three-dimensional single α-polonium nets are interlocked with each other, thus leading directly to the formation of a twofold interpenetrated three-dimensional α-Po architecture (Fig. 3).
There are strong N—H···O hydrogen bonds between the N atoms of the L ligands and the carboxylate O atoms of the 1,4-bdc ligands within different α-Po nets (Table 2). Each α-Po net is hydrogen-bonded to its neighbour through these hydrogen bonds, which further consolidates the twofold interpenetrated framework.
To date, although a number of α-Po frameworks have been reported, we are not aware of any other example of a PbII coordination polymer with this motif (O'Keeffe et al., 2008; Wang et al., 2010). As far as we know, only one α-Po framework based on a 1,10-phen-like ligand, [Cd(1,4-ndc)(L'')]n (L'' is pyrazino[2,3-f][1,10]phenanthroline and 1,4-ndc is naphthalene-1,4-dicarboxylate), has been reported so far (Qiao et al., 2008). In that structure, four CdII atoms are bridged by the carboxylate groups of the 1,4-ndc ligands to form tetranuclear cadmium carboxylate clusters. These tetranuclear cadmium carboxylate clusters are further connected together by the aromatic backbone of the dicarboxylate ligands to generate a three-dimensional non-interpenetrating α-Po net.
Notably, although the very recently reported compound {[Pb(L)(1,4-bdc)].2H2O}n (Wang et al., 2010) is constructed from the same mixed organic ligands and PbII atoms, its structure is entirely different from that of (I). In that compound, each carboxylate group of the 1,4-bdc anion chelates one PbII atom in a bidentate mode. All 1,4-bdc anions assume one kind of coordination mode, namely bridging bis(bidentate). Adjacent PbII atoms are bridged by 1,4-bdc dianions to form a one-dimensional zigzag chain. The L ligands are attached on both sides of the chains in chelating modes. Clearly, the topological difference between (I) and the previously reported compound is mainly attributed to the different coordination modes of the 1,4-bdc dianions and the L ligands. The water molecules are not coordinated to any of the metal atoms, and are in the voids between the chains. It should be pointed out that the previously reported compound was synthesized at 443 K, while (I) was prepared at 468 K in the presence of PbII, 1,4-bdc and L. Thus, the synthesis of the two structures can apparently be controlled through variation of the reaction temperature.