Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807053743/hb2602sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807053743/hb2602Isup2.hkl |
CCDC reference: 672583
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.036
- wR factor = 0.061
- Data-to-parameter ratio = 16.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4
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 Pb1 (2) 2.05
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
A mixture of Pb(NO3)2 (1 mmol), H2fum (1 mmol) and L (1 mmol) were dissolved in 12 ml distilled water, followed by addition of triethylamine until the pH value of the system was adjusted to about 5.8. The resulting solution was sealed in a 23-ml Teflon-lined stainless steel autoclave and heated at 450 K for 10 days under autogenous pressure. Afterwards, the reaction system was slowly cooled to room temperature. Colourless blocks 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).
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).
[Pb(C4H2O4)(C24H16N2)] | Z = 2 |
Mr = 653.63 | F(000) = 628 |
Triclinic, P1 | Dx = 1.880 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.3044 (17) Å | Cell parameters from 10181 reflections |
b = 11.021 (2) Å | θ = 3.0–27.5° |
c = 12.746 (3) Å | µ = 7.35 mm−1 |
α = 89.35 (3)° | T = 293 K |
β = 86.73 (3)° | Block, colorless |
γ = 82.49 (3)° | 0.18 × 0.16 × 0.15 mm |
V = 1154.7 (4) Å3 |
Rigaku R-AXIS RAPID diffractometer | 5231 independent reflections |
Radiation source: rotating anode | 4411 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scan | h = −10→10 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −14→14 |
Tmin = 0.254, Tmax = 0.333 | l = −16→14 |
11422 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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0096P)2 + 1.8148P] where P = (Fo2 + 2Fc2)/3 |
5231 reflections | (Δ/σ)max = 0.002 |
316 parameters | Δρmax = 0.77 e Å−3 |
0 restraints | Δρmin = −0.70 e Å−3 |
[Pb(C4H2O4)(C24H16N2)] | γ = 82.49 (3)° |
Mr = 653.63 | V = 1154.7 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.3044 (17) Å | Mo Kα radiation |
b = 11.021 (2) Å | µ = 7.35 mm−1 |
c = 12.746 (3) Å | T = 293 K |
α = 89.35 (3)° | 0.18 × 0.16 × 0.15 mm |
β = 86.73 (3)° |
Rigaku R-AXIS RAPID diffractometer | 5231 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4411 reflections with I > 2σ(I) |
Tmin = 0.254, Tmax = 0.333 | Rint = 0.041 |
11422 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.77 e Å−3 |
5231 reflections | Δρmin = −0.70 e Å−3 |
316 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 | 0.4593 (6) | 0.0099 (5) | 0.3502 (4) | 0.0427 (12) | |
C2 | 0.4835 (6) | −0.0340 (4) | 0.4607 (4) | 0.0432 (12) | |
H2 | 0.4744 | −0.1158 | 0.4750 | 0.052* | |
C3 | 0.1800 (6) | 0.0473 (4) | 0.0722 (4) | 0.0401 (12) | |
C4 | 0.0161 (6) | 0.0255 (4) | 0.0441 (4) | 0.0419 (12) | |
H4 | −0.0706 | 0.0494 | 0.0920 | 0.050* | |
C5 | 0.2750 (6) | 0.3741 (4) | 0.3041 (4) | 0.0400 (12) | |
H5 | 0.2981 | 0.3115 | 0.3526 | 0.048* | |
C6 | 0.1994 (7) | 0.4868 (4) | 0.3407 (4) | 0.0429 (12) | |
H6 | 0.1737 | 0.4979 | 0.4122 | 0.051* | |
C7 | 0.1623 (6) | 0.5819 (4) | 0.2720 (4) | 0.0384 (11) | |
C8 | 0.2041 (6) | 0.5598 (4) | 0.1626 (4) | 0.0377 (11) | |
C9 | 0.2769 (6) | 0.4420 (4) | 0.1324 (4) | 0.0342 (11) | |
C10 | 0.3062 (6) | 0.4128 (4) | 0.0226 (4) | 0.0356 (11) | |
C11 | 0.3919 (7) | 0.2663 (4) | −0.1023 (4) | 0.0492 (14) | |
H11 | 0.4357 | 0.1865 | −0.1197 | 0.059* | |
C12 | 0.3552 (7) | 0.3488 (4) | −0.1829 (4) | 0.0470 (13) | |
H12 | 0.3729 | 0.3224 | −0.2522 | 0.056* | |
C13 | 0.2933 (6) | 0.4686 (4) | −0.1631 (4) | 0.0382 (11) | |
C14 | 0.2685 (6) | 0.5034 (4) | −0.0553 (4) | 0.0362 (11) | |
C15 | 0.2079 (7) | 0.6242 (4) | −0.0196 (4) | 0.0513 (15) | |
H15 | 0.1918 | 0.6868 | −0.0690 | 0.062* | |
C16 | 0.1732 (7) | 0.6510 (4) | 0.0830 (4) | 0.0517 (15) | |
H16 | 0.1285 | 0.7300 | 0.1022 | 0.062* | |
C17 | 0.2590 (6) | 0.5552 (4) | −0.2513 (4) | 0.0372 (11) | |
C18 | 0.3689 (6) | 0.5503 (5) | −0.3385 (4) | 0.0447 (13) | |
H18 | 0.4610 | 0.4922 | −0.3403 | 0.054* | |
C19 | 0.3443 (8) | 0.6296 (5) | −0.4222 (4) | 0.0549 (15) | |
H19 | 0.4189 | 0.6241 | −0.4798 | 0.066* | |
C20 | 0.2103 (7) | 0.7165 (5) | −0.4208 (4) | 0.0511 (14) | |
H20 | 0.1956 | 0.7715 | −0.4763 | 0.061* | |
C21 | 0.0971 (7) | 0.7223 (5) | −0.3369 (4) | 0.0497 (14) | |
H21 | 0.0047 | 0.7800 | −0.3367 | 0.060* | |
C22 | 0.1207 (6) | 0.6426 (4) | −0.2533 (4) | 0.0441 (12) | |
H22 | 0.0435 | 0.6470 | −0.1972 | 0.053* | |
C23 | 0.0785 (6) | 0.7009 (4) | 0.3128 (4) | 0.0387 (11) | |
C24 | 0.1379 (7) | 0.8109 (4) | 0.2931 (4) | 0.0446 (13) | |
H24 | 0.2331 | 0.8126 | 0.2513 | 0.054* | |
C25 | 0.0570 (8) | 0.9177 (5) | 0.3352 (5) | 0.0553 (16) | |
H25 | 0.0978 | 0.9913 | 0.3217 | 0.066* | |
C26 | −0.0836 (8) | 0.9160 (5) | 0.3970 (5) | 0.0584 (16) | |
H26 | −0.1388 | 0.9888 | 0.4242 | 0.070* | |
C27 | −0.1433 (7) | 0.8071 (5) | 0.4188 (5) | 0.0572 (16) | |
H27 | −0.2372 | 0.8059 | 0.4621 | 0.069* | |
C28 | −0.0632 (6) | 0.6999 (4) | 0.3762 (4) | 0.0454 (13) | |
H28 | −0.1043 | 0.6264 | 0.3900 | 0.054* | |
N1 | 0.3158 (5) | 0.3512 (3) | 0.2036 (3) | 0.0363 (9) | |
N2 | 0.3676 (5) | 0.2954 (3) | −0.0021 (3) | 0.0416 (10) | |
O1 | 0.4253 (6) | 0.1240 (3) | 0.3391 (3) | 0.0647 (12) | |
O2 | 0.4774 (5) | −0.0635 (3) | 0.2768 (3) | 0.0553 (10) | |
O3 | 0.1859 (4) | 0.1193 (3) | 0.1493 (3) | 0.0448 (9) | |
O4 | 0.3050 (5) | −0.0021 (3) | 0.0238 (3) | 0.0571 (10) | |
Pb1 | 0.46035 (2) | 0.137456 (17) | 0.147460 (15) | 0.03580 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.046 (3) | 0.047 (3) | 0.032 (3) | 0.007 (2) | −0.004 (2) | 0.000 (2) |
C2 | 0.049 (3) | 0.034 (3) | 0.043 (3) | 0.006 (2) | 0.000 (3) | 0.002 (2) |
C3 | 0.045 (3) | 0.037 (3) | 0.039 (3) | −0.007 (2) | −0.002 (2) | 0.001 (2) |
C4 | 0.038 (3) | 0.046 (3) | 0.041 (3) | −0.006 (2) | −0.002 (2) | −0.009 (2) |
C5 | 0.058 (3) | 0.033 (2) | 0.029 (3) | −0.005 (2) | −0.005 (2) | −0.001 (2) |
C6 | 0.059 (3) | 0.039 (3) | 0.028 (3) | −0.001 (2) | −0.001 (2) | −0.008 (2) |
C7 | 0.048 (3) | 0.031 (2) | 0.037 (3) | −0.007 (2) | −0.001 (2) | −0.006 (2) |
C8 | 0.049 (3) | 0.033 (2) | 0.030 (3) | −0.004 (2) | −0.001 (2) | −0.004 (2) |
C9 | 0.040 (3) | 0.032 (2) | 0.031 (3) | −0.004 (2) | −0.004 (2) | −0.0037 (19) |
C10 | 0.043 (3) | 0.033 (2) | 0.031 (3) | −0.005 (2) | −0.003 (2) | −0.0052 (19) |
C11 | 0.075 (4) | 0.034 (3) | 0.035 (3) | 0.005 (3) | 0.002 (3) | −0.006 (2) |
C12 | 0.069 (4) | 0.043 (3) | 0.027 (3) | −0.002 (3) | 0.002 (3) | −0.008 (2) |
C13 | 0.045 (3) | 0.036 (2) | 0.034 (3) | −0.006 (2) | −0.001 (2) | −0.001 (2) |
C14 | 0.046 (3) | 0.033 (2) | 0.029 (3) | −0.003 (2) | 0.000 (2) | −0.0039 (19) |
C15 | 0.084 (4) | 0.033 (3) | 0.034 (3) | 0.001 (3) | 0.003 (3) | 0.001 (2) |
C16 | 0.082 (4) | 0.029 (2) | 0.041 (3) | 0.003 (3) | −0.007 (3) | −0.002 (2) |
C17 | 0.045 (3) | 0.039 (3) | 0.030 (3) | −0.012 (2) | −0.003 (2) | −0.003 (2) |
C18 | 0.046 (3) | 0.052 (3) | 0.034 (3) | −0.003 (2) | 0.004 (2) | −0.003 (2) |
C19 | 0.069 (4) | 0.064 (4) | 0.033 (3) | −0.015 (3) | 0.005 (3) | −0.002 (3) |
C20 | 0.073 (4) | 0.049 (3) | 0.034 (3) | −0.015 (3) | −0.009 (3) | 0.005 (2) |
C21 | 0.054 (4) | 0.046 (3) | 0.048 (4) | −0.001 (3) | −0.010 (3) | 0.005 (2) |
C22 | 0.046 (3) | 0.046 (3) | 0.039 (3) | 0.000 (2) | −0.002 (2) | −0.005 (2) |
C23 | 0.050 (3) | 0.039 (3) | 0.026 (3) | −0.001 (2) | −0.004 (2) | −0.008 (2) |
C24 | 0.064 (4) | 0.036 (3) | 0.034 (3) | −0.009 (3) | 0.006 (3) | −0.005 (2) |
C25 | 0.080 (4) | 0.031 (3) | 0.053 (4) | −0.003 (3) | 0.004 (3) | −0.008 (2) |
C26 | 0.071 (4) | 0.041 (3) | 0.059 (4) | 0.012 (3) | −0.001 (3) | −0.015 (3) |
C27 | 0.054 (4) | 0.055 (3) | 0.058 (4) | 0.006 (3) | 0.011 (3) | −0.004 (3) |
C28 | 0.052 (3) | 0.036 (3) | 0.049 (3) | −0.007 (2) | −0.002 (3) | −0.003 (2) |
N1 | 0.048 (2) | 0.0306 (19) | 0.030 (2) | −0.0017 (18) | −0.0039 (18) | −0.0042 (16) |
N2 | 0.058 (3) | 0.034 (2) | 0.031 (2) | 0.0030 (19) | −0.004 (2) | −0.0079 (17) |
O1 | 0.104 (3) | 0.046 (2) | 0.036 (2) | 0.020 (2) | −0.007 (2) | −0.0002 (17) |
O2 | 0.077 (3) | 0.045 (2) | 0.043 (2) | −0.0011 (19) | −0.007 (2) | −0.0109 (17) |
O3 | 0.050 (2) | 0.048 (2) | 0.037 (2) | −0.0123 (17) | −0.0021 (17) | −0.0103 (16) |
O4 | 0.043 (2) | 0.065 (2) | 0.063 (3) | −0.0025 (19) | −0.003 (2) | −0.022 (2) |
Pb1 | 0.03826 (11) | 0.03501 (10) | 0.03301 (10) | 0.00104 (7) | −0.00548 (7) | −0.00209 (7) |
C1—O2 | 1.234 (6) | C15—C16 | 1.351 (7) |
C1—O1 | 1.260 (6) | C15—H15 | 0.9300 |
C1—C2 | 1.499 (7) | C16—H16 | 0.9300 |
C2—C2i | 1.321 (10) | C17—C18 | 1.394 (6) |
C2—H2 | 0.9300 | C17—C22 | 1.400 (7) |
C3—O4 | 1.242 (6) | C18—C19 | 1.379 (7) |
C3—O3 | 1.277 (6) | C18—H18 | 0.9300 |
C3—C4 | 1.477 (7) | C19—C20 | 1.370 (8) |
C4—C4ii | 1.319 (10) | C19—H19 | 0.9300 |
C4—H4 | 0.9300 | C20—C21 | 1.378 (7) |
C5—N1 | 1.324 (6) | C20—H20 | 0.9300 |
C5—C6 | 1.390 (6) | C21—C22 | 1.380 (7) |
C5—H5 | 0.9300 | C21—H21 | 0.9300 |
C6—C7 | 1.373 (7) | C22—H22 | 0.9300 |
C6—H6 | 0.9300 | C23—C24 | 1.382 (7) |
C7—C8 | 1.433 (6) | C23—C28 | 1.391 (7) |
C7—C23 | 1.487 (6) | C24—C25 | 1.375 (7) |
C8—C9 | 1.407 (6) | C24—H24 | 0.9300 |
C8—C16 | 1.430 (7) | C25—C26 | 1.373 (8) |
C9—N1 | 1.363 (6) | C25—H25 | 0.9300 |
C9—C10 | 1.439 (6) | C26—C27 | 1.377 (8) |
C10—N2 | 1.361 (6) | C26—H26 | 0.9300 |
C10—C14 | 1.419 (6) | C27—C28 | 1.379 (7) |
C11—N2 | 1.318 (6) | C27—H27 | 0.9300 |
C11—C12 | 1.385 (7) | C28—H28 | 0.9300 |
C11—H11 | 0.9300 | Pb1—N1 | 2.590 (4) |
C12—C13 | 1.374 (6) | Pb1—N2 | 2.645 (4) |
C12—H12 | 0.9300 | Pb1—O1 | 2.449 (4) |
C13—C14 | 1.426 (6) | Pb1—O2 | 2.740 (4) |
C13—C17 | 1.483 (6) | Pb1—O3 | 2.313 (3) |
C14—C15 | 1.431 (6) | Pb1—O4 | 2.705 (4) |
O2—C1—O1 | 124.1 (5) | C20—C19—H19 | 119.9 |
O2—C1—C2 | 120.2 (4) | C18—C19—H19 | 119.9 |
O1—C1—C2 | 115.6 (4) | C19—C20—C21 | 120.0 (5) |
C2i—C2—C1 | 125.3 (6) | C19—C20—H20 | 120.0 |
C2i—C2—H2 | 117.3 | C21—C20—H20 | 120.0 |
C1—C2—H2 | 117.3 | C20—C21—C22 | 120.1 (5) |
O4—C3—O3 | 121.9 (5) | C20—C21—H21 | 120.0 |
O4—C3—C4 | 121.8 (5) | C22—C21—H21 | 120.0 |
O3—C3—C4 | 116.3 (4) | C21—C22—C17 | 121.1 (5) |
C4ii—C4—C3 | 124.6 (6) | C21—C22—H22 | 119.4 |
C4ii—C4—H4 | 117.7 | C17—C22—H22 | 119.4 |
C3—C4—H4 | 117.7 | C24—C23—C28 | 119.1 (4) |
N1—C5—C6 | 123.4 (4) | C24—C23—C7 | 123.0 (5) |
N1—C5—H5 | 118.3 | C28—C23—C7 | 117.9 (4) |
C6—C5—H5 | 118.3 | C25—C24—C23 | 120.3 (5) |
C7—C6—C5 | 120.4 (5) | C25—C24—H24 | 119.8 |
C7—C6—H6 | 119.8 | C23—C24—H24 | 119.8 |
C5—C6—H6 | 119.8 | C26—C25—C24 | 120.3 (5) |
C6—C7—C8 | 117.5 (4) | C26—C25—H25 | 119.9 |
C6—C7—C23 | 119.5 (4) | C24—C25—H25 | 119.9 |
C8—C7—C23 | 123.0 (4) | C25—C26—C27 | 120.2 (5) |
C9—C8—C16 | 118.7 (4) | C25—C26—H26 | 119.9 |
C9—C8—C7 | 118.1 (4) | C27—C26—H26 | 119.9 |
C16—C8—C7 | 123.1 (4) | C26—C27—C28 | 119.7 (5) |
N1—C9—C8 | 122.4 (4) | C26—C27—H27 | 120.2 |
N1—C9—C10 | 117.8 (4) | C28—C27—H27 | 120.2 |
C8—C9—C10 | 119.7 (4) | C27—C28—C23 | 120.4 (5) |
N2—C10—C14 | 122.3 (4) | C27—C28—H28 | 119.8 |
N2—C10—C9 | 117.2 (4) | C23—C28—H28 | 119.8 |
C14—C10—C9 | 120.5 (4) | C5—N1—C9 | 118.1 (4) |
N2—C11—C12 | 123.1 (5) | C5—N1—Pb1 | 119.9 (3) |
N2—C11—H11 | 118.5 | C9—N1—Pb1 | 122.0 (3) |
C12—C11—H11 | 118.5 | C11—N2—C10 | 118.1 (4) |
C13—C12—C11 | 121.6 (5) | C11—N2—Pb1 | 121.4 (3) |
C13—C12—H12 | 119.2 | C10—N2—Pb1 | 120.3 (3) |
C11—C12—H12 | 119.2 | C1—O1—Pb1 | 99.2 (3) |
C12—C13—C14 | 116.6 (4) | C1—O2—Pb1 | 86.1 (3) |
C12—C13—C17 | 120.1 (4) | C3—O3—Pb1 | 102.0 (3) |
C14—C13—C17 | 123.3 (4) | C3—O4—Pb1 | 84.5 (3) |
C10—C14—C13 | 118.4 (4) | O3—Pb1—O1 | 85.17 (14) |
C10—C14—C15 | 117.1 (4) | O3—Pb1—N1 | 75.35 (12) |
C13—C14—C15 | 124.5 (4) | O1—Pb1—N1 | 75.70 (12) |
C16—C15—C14 | 122.6 (5) | O3—Pb1—N2 | 79.49 (13) |
C16—C15—H15 | 118.7 | O1—Pb1—N2 | 137.38 (12) |
C14—C15—H15 | 118.7 | N1—Pb1—N2 | 62.03 (12) |
C15—C16—C8 | 121.0 (5) | O3—Pb1—O4 | 51.31 (11) |
C15—C16—H16 | 119.5 | O1—Pb1—O4 | 120.44 (14) |
C8—C16—H16 | 119.5 | N1—Pb1—O4 | 118.64 (12) |
C18—C17—C22 | 117.1 (5) | N2—Pb1—O4 | 78.77 (12) |
C18—C17—C13 | 119.0 (5) | O3—Pb1—O2 | 84.60 (12) |
C22—C17—C13 | 123.8 (4) | O1—Pb1—O2 | 49.85 (11) |
C19—C18—C17 | 121.5 (5) | N1—Pb1—O2 | 123.32 (11) |
C19—C18—H18 | 119.2 | N2—Pb1—O2 | 161.17 (12) |
C17—C18—H18 | 119.2 | O4—Pb1—O2 | 83.44 (12) |
C20—C19—C18 | 120.1 (5) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Pb(C4H2O4)(C24H16N2)] |
Mr | 653.63 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.3044 (17), 11.021 (2), 12.746 (3) |
α, β, γ (°) | 89.35 (3), 86.73 (3), 82.49 (3) |
V (Å3) | 1154.7 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 7.35 |
Crystal size (mm) | 0.18 × 0.16 × 0.15 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.254, 0.333 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11422, 5231, 4411 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.061, 1.06 |
No. of reflections | 5231 |
No. of parameters | 316 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.77, −0.70 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
Pb1—N1 | 2.590 (4) | Pb1—O2 | 2.740 (4) |
Pb1—N2 | 2.645 (4) | Pb1—O3 | 2.313 (3) |
Pb1—O1 | 2.449 (4) | Pb1—O4 | 2.705 (4) |
Metal cations with an s2 electron configuration have important applications in electroluminescent devices or organic light-emitting diode technology (Fan & Zhu, 2006). Among them, the PbII coordination polymers have received much attention due to their interesting network topologies and properties (Yang et al., 2007). Herein, we present a new Pb(II) coordination polymer, namely the title compound, (I), [Pb(fum)(L)], where fum = the fumarate dianion and L = 4,7-diphenyl-1,10-phenanthroline.
In compound (I) the PbII atom is six-coordinated by four carboxylate O atoms from two different fum ligands and two N atoms from one L ligand (Table 1, Fig. 1). The resulting PbN2O6 polyhedron is irregular, perhaps caused, in part, by the stereochemical activity of the Pb lone pair of electrons. There are two fum half-molecules in the asymmetric unit, both being completed by inversion symmetry. The neighboring PbII atoms are linked by the fum dianions to form a chain structure and the L ligands are decorded on both sides of the chains (Fig. 2). Furthermore, π-π interactions [minimum centroid-centroid separation = 3.462 (3) Å]. between L ligands in neighboring chains yields a two-dimensional supramolecular layer structure (Fig. 3).