Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807050702/hb2579sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807050702/hb2579Isup2.hkl |
CCDC reference: 667184
A mixture of Pb(NO3)2 (1 mmol), 1,4-H2NDC (1 mmol) and L (1 mmol) were dissolved in 15 ml distilled water, followed by addition of triethylamine until the pH value of the system was adjusted to about 6. The resulting solution was sealed in a 23-ml Teflon-lined stainless steel autoclave and heated at 453 K for 7 days under autogenous pressure. Afterwards, the reaction system was slowly cooled to room temperature. Colourless slabs and plates of (I) were collected.
All the H atoms were generated geometrically (C—H = 0.93 Å) and refined as riding with Uiso(H)= 1.2Ueq(C).
Lead(II), with its large radius, flexible coordination environment, and variable stereochemical activity, provides unique opportunities for formation of unusual coordination polymer network topologies with interesting properties (Fan & Zhu, 2006; 2007). Herein, we present a new Pb(II) coordination polymer, namely the title compound, (I), [Pb2(1,4-NDC)2(L)], where L= 1,10-phenanthroline and 1,4-NDC =naphthalene-1,4-dicarboxylate.
Selected bond lengthes and angles are listed in Table 1. In compound (I) there exist two 1,4-NDC dianions, one L ligand and two crystallographically independent Pb(II) atoms (Fig. 1). Pb1 is six-coordinated by six carboxylate O atoms from four 1,4-NDC ligands, and its lone pair of electrons appears to be stereochemically active. Atom Pb2 is also six-coordinated, by two N atoms from one chelating L ligand, and four carboxylate O atoms from three 1,4-NDC ligands, while the lone pair of electrons completes its environment. The 1,4-NDC dianions link neighboring Pb(II) atoms to generate a layer structure and the L ligands are located on both sides of the layers (Fig. 2). Moreover, the neighboring layers interact through π-π forces between L and 1,4-NDC ligands, forming a three-dimensional supramolecular structure.
For studies on related lead(II) carboxylates, see Fan & Zhu (2006) and (2007).
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Pb2(C12H6O4)2(C12H8N2)] | F(000) = 956 |
Mr = 1022.92 | Dx = 2.276 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 14193 reflections |
a = 7.063 (3) Å | θ = 3.0–27.5° |
b = 14.602 (5) Å | µ = 11.33 mm−1 |
c = 14.526 (5) Å | T = 293 K |
β = 94.922 (5)° | Slab, colourless |
V = 1492.6 (10) Å3 | 0.29 × 0.15 × 0.09 mm |
Z = 2 |
Rigaku R-AXIS RAPID diffractometer | 6786 independent reflections |
Radiation source: rotating anode | 6429 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −9→7 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −18→18 |
Tmin = 0.141, Tmax = 0.368 | l = −18→18 |
14649 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.046 | w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3 |
S = 0.91 | (Δ/σ)max = 0.001 |
6786 reflections | Δρmax = 0.60 e Å−3 |
433 parameters | Δρmin = −1.06 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 3232 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.011 (5) |
[Pb2(C12H6O4)2(C12H8N2)] | V = 1492.6 (10) Å3 |
Mr = 1022.92 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 7.063 (3) Å | µ = 11.33 mm−1 |
b = 14.602 (5) Å | T = 293 K |
c = 14.526 (5) Å | 0.29 × 0.15 × 0.09 mm |
β = 94.922 (5)° |
Rigaku R-AXIS RAPID diffractometer | 6786 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 6429 reflections with I > 2σ(I) |
Tmin = 0.141, Tmax = 0.368 | Rint = 0.036 |
14649 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.046 | Δρmax = 0.60 e Å−3 |
S = 0.91 | Δρmin = −1.06 e Å−3 |
6786 reflections | Absolute structure: Flack (1983), 3232 Friedel pairs |
433 parameters | Absolute structure parameter: −0.011 (5) |
1 restraint |
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 | 0.8600 (7) | −0.3121 (4) | 0.8347 (4) | 0.0310 (11) | |
C2 | 0.8383 (7) | −0.3959 (3) | 0.8940 (4) | 0.0262 (11) | |
C3 | 0.6962 (7) | −0.3962 (4) | 0.9510 (4) | 0.0375 (12) | |
H3 | 0.6189 | −0.3448 | 0.9524 | 0.045* | |
C4 | 0.6608 (8) | −0.4704 (4) | 1.0076 (4) | 0.0396 (13) | |
H4 | 0.5589 | −0.4686 | 1.0441 | 0.048* | |
C5 | 0.7767 (7) | −0.5462 (3) | 1.0094 (4) | 0.0339 (12) | |
C6 | 0.9682 (7) | −0.4729 (3) | 0.8950 (3) | 0.0254 (10) | |
C7 | 1.1281 (7) | −0.4789 (3) | 0.8432 (4) | 0.0349 (11) | |
H7 | 1.1488 | −0.4335 | 0.8004 | 0.042* | |
C8 | 1.2530 (8) | −0.5502 (3) | 0.8549 (5) | 0.0453 (15) | |
H8 | 1.3593 | −0.5514 | 0.8213 | 0.054* | |
C9 | 1.2242 (8) | −0.6206 (4) | 0.9159 (4) | 0.0447 (14) | |
H9 | 1.3119 | −0.6681 | 0.9238 | 0.054* | |
C10 | 1.0669 (8) | −0.6206 (3) | 0.9645 (4) | 0.0435 (13) | |
H10 | 1.0460 | −0.6695 | 1.0033 | 0.052* | |
C13 | 0.3703 (7) | −0.1061 (3) | 0.6647 (4) | 0.0242 (10) | |
C14 | 0.3748 (6) | −0.0248 (3) | 0.6024 (3) | 0.0212 (9) | |
C15 | 0.4044 (6) | −0.0375 (3) | 0.5120 (4) | 0.0289 (10) | |
H16 | 0.4243 | −0.0962 | 0.4900 | 0.035* | |
C16 | 0.4051 (7) | 0.0378 (3) | 0.4518 (4) | 0.0305 (11) | |
H17 | 0.4309 | 0.0285 | 0.3908 | 0.037* | |
C17 | 0.3689 (6) | 0.1242 (3) | 0.4810 (4) | 0.0273 (10) | |
C20 | 0.3402 (6) | 0.1398 (3) | 0.5757 (3) | 0.0242 (10) | |
C24 | 0.3427 (6) | 0.0644 (3) | 0.6368 (4) | 0.0251 (10) | |
C23 | 0.3107 (7) | 0.0790 (3) | 0.7304 (4) | 0.0320 (11) | |
H23 | 0.3109 | 0.0291 | 0.7702 | 0.038* | |
C19 | 0.3103 (7) | 0.2291 (3) | 0.6133 (4) | 0.0351 (12) | |
H13 | 0.3100 | 0.2802 | 0.5751 | 0.042* | |
C21 | 0.2826 (8) | 0.2399 (4) | 0.7039 (4) | 0.0438 (13) | |
H21 | 0.2652 | 0.2985 | 0.7268 | 0.053* | |
C31 | 0.7904 (8) | 0.2644 (4) | 0.6450 (6) | 0.056 (2) | |
H31 | 0.7716 | 0.3260 | 0.6578 | 0.067* | |
C32 | 0.8171 (8) | 0.2400 (4) | 0.5597 (5) | 0.0478 (15) | |
H32 | 0.8174 | 0.2846 | 0.5140 | 0.057* | |
C27 | 0.8455 (7) | 0.1461 (4) | 0.5359 (5) | 0.0411 (14) | |
C26 | 0.8780 (7) | 0.1184 (4) | 0.4484 (4) | 0.0460 (14) | |
H26 | 0.8808 | 0.1618 | 0.4017 | 0.055* | |
C28 | 0.8420 (6) | 0.0786 (3) | 0.6056 (4) | 0.0327 (12) | |
C29 | 0.8154 (7) | 0.1041 (3) | 0.6991 (4) | 0.0313 (11) | |
C35 | 0.7991 (8) | 0.0630 (4) | 0.8511 (4) | 0.0467 (14) | |
H35 | 0.8008 | 0.0178 | 0.8963 | 0.056* | |
C36 | 0.8966 (7) | −0.0346 (4) | 0.4998 (4) | 0.0423 (13) | |
H36 | 0.9139 | −0.0962 | 0.4864 | 0.051* | |
C18 | 0.3599 (8) | 0.1990 (3) | 0.4078 (4) | 0.0370 (12) | |
C30 | 0.7893 (8) | 0.1983 (4) | 0.7199 (5) | 0.0459 (16) | |
C12 | 0.7355 (8) | −0.6235 (3) | 1.0724 (4) | 0.0381 (12) | |
C22 | 0.2796 (8) | 0.1646 (4) | 0.7639 (4) | 0.0425 (13) | |
H22 | 0.2568 | 0.1729 | 0.8255 | 0.051* | |
C34 | 0.7771 (10) | 0.1539 (5) | 0.8771 (5) | 0.0610 (19) | |
H34 | 0.7673 | 0.1689 | 0.9388 | 0.073* | |
C11 | 0.9371 (7) | −0.5482 (3) | 0.9567 (4) | 0.0280 (11) | |
C25 | 0.9060 (8) | 0.0290 (5) | 0.4290 (5) | 0.0552 (17) | |
H25 | 0.9309 | 0.0105 | 0.3700 | 0.066* | |
C33 | 0.7700 (10) | 0.2208 (4) | 0.8114 (6) | 0.0587 (19) | |
H33 | 0.7522 | 0.2815 | 0.8279 | 0.070* | |
N1 | 0.8641 (5) | −0.0117 (3) | 0.5859 (3) | 0.0305 (9) | |
N2 | 0.8177 (6) | 0.0382 (3) | 0.7636 (3) | 0.0348 (10) | |
O1 | 0.9883 (6) | −0.3066 (3) | 0.7806 (4) | 0.0512 (12) | |
O2 | 0.7379 (5) | −0.2472 (2) | 0.8418 (3) | 0.0323 (8) | |
O3 | 0.5033 (4) | −0.1186 (2) | 0.7271 (3) | 0.0312 (8) | |
O4 | 0.2304 (4) | −0.1607 (2) | 0.6549 (2) | 0.0297 (8) | |
O5 | 0.4507 (6) | 0.1824 (3) | 0.3387 (3) | 0.0577 (12) | |
O6 | 0.2628 (6) | 0.2688 (2) | 0.4181 (3) | 0.0498 (11) | |
O7 | 0.8192 (7) | −0.6248 (3) | 1.1507 (3) | 0.0593 (12) | |
O8 | 0.6205 (9) | −0.6829 (4) | 1.0446 (4) | 0.102 (2) | |
Pb1 | 0.38951 (3) | −0.256319 (9) | 0.794522 (12) | 0.02560 (5) | |
Pb2 | 0.86603 (2) | −0.137997 (11) | 0.714247 (12) | 0.02589 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.028 (2) | 0.036 (3) | 0.028 (3) | −0.005 (2) | 0.002 (2) | 0.008 (2) |
C2 | 0.028 (2) | 0.026 (2) | 0.025 (3) | −0.0022 (19) | 0.002 (2) | 0.008 (2) |
C3 | 0.044 (3) | 0.041 (3) | 0.028 (3) | 0.013 (2) | 0.007 (2) | 0.011 (2) |
C4 | 0.040 (3) | 0.051 (3) | 0.030 (3) | 0.004 (2) | 0.014 (2) | 0.011 (3) |
C5 | 0.043 (3) | 0.039 (3) | 0.019 (3) | −0.003 (2) | −0.003 (2) | 0.010 (2) |
C6 | 0.030 (2) | 0.024 (2) | 0.022 (3) | 0.0012 (18) | −0.001 (2) | 0.0037 (19) |
C7 | 0.044 (3) | 0.028 (2) | 0.035 (3) | −0.002 (2) | 0.014 (2) | 0.003 (2) |
C8 | 0.046 (3) | 0.035 (3) | 0.057 (4) | 0.003 (2) | 0.013 (3) | −0.005 (3) |
C9 | 0.050 (3) | 0.038 (3) | 0.045 (4) | 0.017 (2) | 0.000 (3) | 0.000 (3) |
C10 | 0.059 (3) | 0.034 (3) | 0.036 (3) | 0.007 (2) | −0.003 (3) | 0.008 (2) |
C13 | 0.030 (2) | 0.020 (2) | 0.024 (3) | 0.0000 (18) | 0.011 (2) | 0.0026 (19) |
C14 | 0.0170 (19) | 0.022 (2) | 0.025 (2) | −0.0028 (16) | 0.0033 (18) | −0.0021 (19) |
C15 | 0.029 (2) | 0.028 (2) | 0.029 (3) | 0.0007 (19) | 0.002 (2) | −0.002 (2) |
C16 | 0.032 (2) | 0.035 (2) | 0.025 (3) | 0.002 (2) | 0.005 (2) | 0.005 (2) |
C17 | 0.023 (2) | 0.026 (2) | 0.032 (3) | −0.0041 (18) | 0.004 (2) | 0.009 (2) |
C20 | 0.023 (2) | 0.026 (2) | 0.023 (2) | −0.0007 (17) | 0.0015 (19) | 0.0041 (19) |
C24 | 0.022 (2) | 0.026 (2) | 0.028 (3) | −0.0006 (18) | 0.002 (2) | 0.001 (2) |
C23 | 0.037 (3) | 0.032 (2) | 0.028 (3) | 0.003 (2) | 0.011 (2) | 0.008 (2) |
C19 | 0.040 (3) | 0.021 (2) | 0.044 (3) | 0.0028 (19) | 0.002 (2) | 0.008 (2) |
C21 | 0.055 (3) | 0.029 (2) | 0.047 (3) | 0.008 (3) | 0.004 (3) | −0.008 (3) |
C31 | 0.046 (3) | 0.026 (3) | 0.093 (6) | 0.000 (2) | −0.012 (4) | 0.015 (3) |
C32 | 0.040 (3) | 0.033 (3) | 0.069 (5) | −0.001 (2) | −0.006 (3) | 0.023 (3) |
C27 | 0.019 (2) | 0.041 (3) | 0.063 (4) | 0.001 (2) | −0.001 (3) | 0.020 (3) |
C26 | 0.033 (3) | 0.063 (4) | 0.042 (4) | 0.004 (3) | 0.007 (3) | 0.029 (3) |
C28 | 0.022 (2) | 0.033 (2) | 0.043 (3) | 0.0004 (19) | 0.000 (2) | 0.008 (2) |
C29 | 0.027 (2) | 0.022 (2) | 0.044 (3) | −0.0011 (18) | −0.004 (2) | 0.004 (2) |
C35 | 0.051 (3) | 0.055 (3) | 0.033 (3) | 0.001 (3) | 0.001 (3) | −0.001 (3) |
C36 | 0.035 (3) | 0.054 (3) | 0.038 (3) | 0.005 (2) | 0.008 (2) | 0.006 (3) |
C18 | 0.047 (3) | 0.034 (3) | 0.030 (3) | −0.012 (2) | 0.001 (3) | 0.008 (2) |
C30 | 0.036 (3) | 0.031 (3) | 0.068 (5) | 0.003 (2) | −0.010 (3) | −0.001 (3) |
C12 | 0.045 (3) | 0.033 (3) | 0.037 (3) | −0.001 (2) | 0.006 (2) | 0.012 (2) |
C22 | 0.057 (3) | 0.041 (3) | 0.030 (3) | 0.003 (3) | 0.008 (3) | −0.005 (3) |
C34 | 0.062 (4) | 0.069 (4) | 0.049 (4) | 0.010 (3) | −0.011 (3) | −0.023 (4) |
C11 | 0.036 (3) | 0.024 (2) | 0.023 (3) | −0.003 (2) | −0.002 (2) | 0.008 (2) |
C25 | 0.039 (3) | 0.090 (5) | 0.038 (4) | 0.011 (3) | 0.013 (3) | 0.015 (4) |
C33 | 0.065 (4) | 0.039 (3) | 0.069 (5) | 0.005 (3) | −0.012 (4) | −0.017 (3) |
N1 | 0.0249 (19) | 0.028 (2) | 0.038 (3) | 0.0016 (16) | −0.0030 (19) | 0.0051 (19) |
N2 | 0.036 (2) | 0.033 (2) | 0.035 (3) | 0.0005 (17) | −0.003 (2) | 0.002 (2) |
O1 | 0.052 (2) | 0.039 (2) | 0.066 (3) | 0.0082 (19) | 0.027 (2) | 0.028 (2) |
O2 | 0.0352 (17) | 0.0233 (16) | 0.038 (2) | 0.0018 (14) | −0.0003 (15) | 0.0073 (16) |
O3 | 0.0340 (17) | 0.0242 (16) | 0.034 (2) | −0.0008 (13) | −0.0019 (15) | 0.0047 (15) |
O4 | 0.0290 (17) | 0.0328 (18) | 0.0279 (19) | −0.0069 (13) | 0.0045 (15) | 0.0033 (15) |
O5 | 0.081 (3) | 0.050 (2) | 0.046 (3) | 0.002 (2) | 0.027 (3) | 0.022 (2) |
O6 | 0.069 (3) | 0.034 (2) | 0.046 (3) | 0.0107 (19) | 0.000 (2) | 0.0143 (18) |
O7 | 0.090 (3) | 0.052 (3) | 0.034 (2) | −0.015 (2) | −0.007 (2) | 0.014 (2) |
O8 | 0.121 (5) | 0.100 (4) | 0.076 (4) | −0.071 (4) | −0.050 (4) | 0.056 (3) |
Pb1 | 0.03473 (10) | 0.02015 (8) | 0.02271 (9) | 0.00014 (7) | 0.00705 (7) | 0.00040 (8) |
Pb2 | 0.02927 (9) | 0.02153 (8) | 0.02683 (10) | −0.00054 (7) | 0.00221 (7) | 0.00271 (8) |
C1—O1 | 1.252 (7) | C31—C32 | 1.319 (10) |
C1—O2 | 1.291 (6) | C31—C30 | 1.454 (9) |
C1—C2 | 1.512 (7) | C31—H31 | 0.9300 |
C2—C3 | 1.355 (7) | C32—C27 | 1.432 (8) |
C2—C6 | 1.450 (7) | C32—H32 | 0.9300 |
C3—C4 | 1.396 (7) | C27—C26 | 1.372 (9) |
C3—H3 | 0.9300 | C27—C28 | 1.413 (7) |
C4—C5 | 1.375 (7) | C26—C25 | 1.354 (9) |
C4—H4 | 0.9300 | C26—H26 | 0.9300 |
C5—C11 | 1.420 (7) | C28—N1 | 1.362 (6) |
C5—C12 | 1.498 (7) | C28—C29 | 1.436 (8) |
C6—C7 | 1.412 (7) | C29—N2 | 1.341 (7) |
C6—C11 | 1.447 (6) | C29—C30 | 1.425 (7) |
C7—C8 | 1.365 (7) | C35—N2 | 1.339 (8) |
C7—H7 | 0.9300 | C35—C34 | 1.392 (8) |
C8—C9 | 1.383 (8) | C35—H35 | 0.9300 |
C8—H8 | 0.9300 | C36—N1 | 1.333 (7) |
C9—C10 | 1.366 (9) | C36—C25 | 1.391 (9) |
C9—H9 | 0.9300 | C36—H36 | 0.9300 |
C10—C11 | 1.397 (7) | C18—O6 | 1.245 (6) |
C10—H10 | 0.9300 | C18—O5 | 1.261 (7) |
C13—O3 | 1.261 (6) | C30—C33 | 1.386 (10) |
C13—O4 | 1.268 (6) | C12—O8 | 1.232 (7) |
C13—C14 | 1.495 (6) | C12—O7 | 1.236 (7) |
C14—C15 | 1.359 (7) | C22—H22 | 0.9300 |
C14—C24 | 1.420 (6) | C34—C33 | 1.364 (10) |
C15—C16 | 1.406 (7) | C34—H34 | 0.9300 |
C15—H16 | 0.9300 | C25—H25 | 0.9300 |
C16—C17 | 1.362 (7) | C33—H33 | 0.9300 |
C16—H17 | 0.9300 | Pb2—N1 | 2.622 (4) |
C17—C20 | 1.426 (7) | Pb2—N2 | 2.701 (4) |
C17—C18 | 1.522 (7) | Pb2—O1 | 2.756 (4) |
C20—C24 | 1.413 (6) | Pb2—O2 | 2.661 (4) |
C20—C19 | 1.436 (6) | Pb2—O3 | 2.600 (4) |
C24—C23 | 1.415 (7) | Pb2—O6i | 2.464 (4) |
C23—C22 | 1.366 (7) | Pb1—O2 | 2.501 (4) |
C23—H23 | 0.9300 | Pb1—O3 | 2.405 (3) |
C19—C21 | 1.356 (8) | Pb1—O4 | 2.633 (3) |
C19—H13 | 0.9300 | Pb1—O5i | 2.488 (4) |
C21—C22 | 1.404 (8) | Pb1—O7ii | 2.588 (4) |
C21—H21 | 0.9300 | Pb1—O8ii | 2.577 (5) |
O1—C1—O2 | 121.8 (5) | N2—C35—C34 | 122.5 (6) |
O1—C1—C2 | 121.6 (4) | N2—C35—H35 | 118.7 |
O2—C1—C2 | 116.6 (4) | C34—C35—H35 | 118.7 |
C3—C2—C6 | 119.5 (4) | N1—C36—C25 | 123.3 (6) |
C3—C2—C1 | 117.9 (4) | N1—C36—H36 | 118.4 |
C6—C2—C1 | 122.6 (4) | C25—C36—H36 | 118.4 |
C2—C3—C4 | 122.8 (5) | O6—C18—O5 | 125.2 (5) |
C2—C3—H3 | 118.6 | O6—C18—C17 | 119.6 (5) |
C4—C3—H3 | 118.6 | O5—C18—C17 | 115.2 (5) |
C5—C4—C3 | 120.0 (5) | C33—C30—C29 | 117.2 (6) |
C5—C4—H4 | 120.0 | C33—C30—C31 | 124.6 (6) |
C3—C4—H4 | 120.0 | C29—C30—C31 | 118.2 (6) |
C4—C5—C11 | 120.5 (5) | O8—C12—O7 | 122.7 (5) |
C4—C5—C12 | 118.1 (5) | O8—C12—C5 | 119.2 (5) |
C11—C5—C12 | 121.2 (4) | O7—C12—C5 | 118.1 (5) |
C7—C6—C11 | 117.0 (4) | C23—C22—C21 | 118.9 (5) |
C7—C6—C2 | 125.2 (4) | C23—C22—H22 | 120.5 |
C11—C6—C2 | 117.8 (4) | C21—C22—H22 | 120.5 |
C8—C7—C6 | 121.2 (5) | C33—C34—C35 | 119.4 (7) |
C8—C7—H7 | 119.4 | C33—C34—H34 | 120.3 |
C6—C7—H7 | 119.4 | C35—C34—H34 | 120.3 |
C7—C8—C9 | 121.2 (6) | C10—C11—C5 | 121.4 (5) |
C7—C8—H8 | 119.4 | C10—C11—C6 | 119.4 (5) |
C9—C8—H8 | 119.4 | C5—C11—C6 | 119.2 (4) |
C10—C9—C8 | 120.0 (5) | C26—C25—C36 | 118.2 (6) |
C10—C9—H9 | 120.0 | C26—C25—H25 | 120.9 |
C8—C9—H9 | 120.0 | C36—C25—H25 | 120.9 |
C9—C10—C11 | 121.1 (5) | C34—C33—C30 | 120.1 (6) |
C9—C10—H10 | 119.5 | C34—C33—H33 | 120.0 |
C11—C10—H10 | 119.5 | C30—C33—H33 | 120.0 |
O3—C13—O4 | 121.0 (4) | C36—N1—C28 | 118.2 (5) |
O3—C13—C14 | 119.8 (4) | C36—N1—Pb2 | 120.0 (3) |
O4—C13—C14 | 119.2 (4) | C28—N1—Pb2 | 121.7 (4) |
C15—C14—C24 | 120.5 (5) | C35—N2—C29 | 118.3 (5) |
C15—C14—C13 | 119.3 (4) | C35—N2—Pb2 | 122.3 (4) |
C24—C14—C13 | 120.2 (4) | C29—N2—Pb2 | 119.4 (4) |
C14—C15—C16 | 120.2 (4) | C1—O1—Pb2 | 93.1 (3) |
C14—C15—H16 | 119.9 | C1—O2—Pb1 | 125.9 (3) |
C16—C15—H16 | 119.9 | C1—O2—Pb2 | 96.6 (3) |
C17—C16—C15 | 121.3 (5) | Pb1—O2—Pb2 | 103.08 (12) |
C17—C16—H17 | 119.3 | C13—O3—Pb1 | 99.2 (3) |
C15—C16—H17 | 119.3 | C13—O3—Pb2 | 130.0 (3) |
C16—C17—C20 | 119.6 (4) | Pb1—O3—Pb2 | 107.69 (11) |
C16—C17—C18 | 116.4 (5) | C13—O4—Pb1 | 88.3 (3) |
C20—C17—C18 | 124.0 (4) | C18—O5—Pb1iii | 147.8 (4) |
C24—C20—C17 | 119.1 (4) | C18—O6—Pb2iii | 121.9 (4) |
C24—C20—C19 | 117.6 (5) | C12—O7—Pb1iv | 93.1 (3) |
C17—C20—C19 | 123.3 (4) | C12—O8—Pb1iv | 93.7 (4) |
C20—C24—C23 | 119.4 (4) | O3—Pb1—O5i | 78.12 (14) |
C20—C24—C14 | 119.2 (5) | O3—Pb1—O2 | 73.26 (11) |
C23—C24—C14 | 121.4 (4) | O5i—Pb1—O2 | 74.42 (14) |
C22—C23—C24 | 121.6 (5) | O3—Pb1—O8ii | 93.29 (19) |
C22—C23—H23 | 119.2 | O5i—Pb1—O8ii | 154.69 (18) |
C24—C23—H23 | 119.2 | O2—Pb1—O8ii | 80.32 (17) |
C21—C19—C20 | 120.8 (5) | O3—Pb1—O7ii | 73.96 (14) |
C21—C19—H13 | 119.6 | O5i—Pb1—O7ii | 144.51 (15) |
C20—C19—H13 | 119.6 | O2—Pb1—O7ii | 116.68 (13) |
C19—C21—C22 | 121.5 (5) | O8ii—Pb1—O7ii | 49.58 (14) |
C19—C21—H21 | 119.2 | O3—Pb1—O4 | 51.57 (10) |
C22—C21—H21 | 119.2 | O5i—Pb1—O4 | 77.52 (14) |
C32—C31—C30 | 122.3 (6) | O2—Pb1—O4 | 121.87 (10) |
C32—C31—H31 | 118.8 | O8ii—Pb1—O4 | 115.74 (14) |
C30—C31—H31 | 118.8 | O7ii—Pb1—O4 | 68.07 (13) |
C31—C32—C27 | 121.3 (6) | O6i—Pb2—O3 | 79.40 (14) |
C31—C32—H32 | 119.4 | O6i—Pb2—N1 | 81.63 (14) |
C27—C32—H32 | 119.4 | O3—Pb2—N1 | 91.69 (11) |
C26—C27—C28 | 118.2 (5) | O6i—Pb2—O2 | 95.01 (13) |
C26—C27—C32 | 122.9 (6) | O3—Pb2—O2 | 67.62 (10) |
C28—C27—C32 | 118.9 (6) | N1—Pb2—O2 | 159.28 (11) |
C25—C26—C27 | 121.1 (6) | O6i—Pb2—N2 | 133.35 (14) |
C25—C26—H26 | 119.5 | O3—Pb2—N2 | 74.31 (11) |
C27—C26—H26 | 119.5 | N1—Pb2—N2 | 61.68 (14) |
N1—C28—C27 | 121.0 (5) | O2—Pb2—N2 | 109.14 (13) |
N1—C28—C29 | 118.4 (5) | O6i—Pb2—O1 | 82.13 (15) |
C27—C28—C29 | 120.6 (5) | O3—Pb2—O1 | 110.68 (10) |
N2—C29—C30 | 122.5 (6) | N1—Pb2—O1 | 149.26 (13) |
N2—C29—C28 | 118.8 (4) | O2—Pb2—O1 | 48.41 (11) |
C30—C29—C28 | 118.7 (5) | N2—Pb2—O1 | 143.27 (15) |
Symmetry codes: (i) −x+1, y−1/2, −z+1; (ii) −x+1, y+1/2, −z+2; (iii) −x+1, y+1/2, −z+1; (iv) −x+1, y−1/2, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Pb2(C12H6O4)2(C12H8N2)] |
Mr | 1022.92 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 293 |
a, b, c (Å) | 7.063 (3), 14.602 (5), 14.526 (5) |
β (°) | 94.922 (5) |
V (Å3) | 1492.6 (10) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 11.33 |
Crystal size (mm) | 0.29 × 0.15 × 0.09 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.141, 0.368 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14649, 6786, 6429 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.046, 0.91 |
No. of reflections | 6786 |
No. of parameters | 433 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.60, −1.06 |
Absolute structure | Flack (1983), 3232 Friedel pairs |
Absolute structure parameter | −0.011 (5) |
Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
Pb2—N1 | 2.622 (4) | Pb1—O2 | 2.501 (4) |
Pb2—N2 | 2.701 (4) | Pb1—O3 | 2.405 (3) |
Pb2—O1 | 2.756 (4) | Pb1—O4 | 2.633 (3) |
Pb2—O2 | 2.661 (4) | Pb1—O5i | 2.488 (4) |
Pb2—O3 | 2.600 (4) | Pb1—O7ii | 2.588 (4) |
Pb2—O6i | 2.464 (4) | Pb1—O8ii | 2.577 (5) |
Symmetry codes: (i) −x+1, y−1/2, −z+1; (ii) −x+1, y+1/2, −z+2. |
Lead(II), with its large radius, flexible coordination environment, and variable stereochemical activity, provides unique opportunities for formation of unusual coordination polymer network topologies with interesting properties (Fan & Zhu, 2006; 2007). Herein, we present a new Pb(II) coordination polymer, namely the title compound, (I), [Pb2(1,4-NDC)2(L)], where L= 1,10-phenanthroline and 1,4-NDC =naphthalene-1,4-dicarboxylate.
Selected bond lengthes and angles are listed in Table 1. In compound (I) there exist two 1,4-NDC dianions, one L ligand and two crystallographically independent Pb(II) atoms (Fig. 1). Pb1 is six-coordinated by six carboxylate O atoms from four 1,4-NDC ligands, and its lone pair of electrons appears to be stereochemically active. Atom Pb2 is also six-coordinated, by two N atoms from one chelating L ligand, and four carboxylate O atoms from three 1,4-NDC ligands, while the lone pair of electrons completes its environment. The 1,4-NDC dianions link neighboring Pb(II) atoms to generate a layer structure and the L ligands are located on both sides of the layers (Fig. 2). Moreover, the neighboring layers interact through π-π forces between L and 1,4-NDC ligands, forming a three-dimensional supramolecular structure.