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In the title compound, [Pb(C7H4O3)]n, the PbII atom is coordinated by five O atoms from four salicylic acid ligands with Pb—O distances of 2.318 (16)–2.605 (15) Å. Each ligand acts in a pentadentate mode that leads to the formation of a two-dimensional polymeric network.
Supporting information
CCDC reference: 620779
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.030 Å
- R factor = 0.076
- wR factor = 0.214
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 30
Alert level C
DIFMN02_ALERT_2_C The minimum difference density is < -0.1*ZMAX*0.75
_refine_diff_density_min given = -6.508
Test value = -6.150
DIFMN03_ALERT_1_C The minimum difference density is < -0.1*ZMAX*0.75
The relevant atom site should be identified.
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 6.349
Test value = 6.150
DIFMX02_ALERT_1_C The maximum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 6.35 e/A
PLAT098_ALERT_2_C Minimum (Negative) Residual Density ............ -6.51 e/A
PLAT213_ALERT_2_C Atom C1 has ADP max/min Ratio ............. 3.20 oblat
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.02
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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, 1997); software used to prepare material for publication: SHELXTL.
Poly[µ-salicylato-lead(II)]
top
Crystal data top
[Pb(C7H4O3)] | F(000) = 608 |
Mr = 343.29 | Dx = 3.251 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2ybc | Cell parameters from 1807 reflections |
a = 5.8137 (18) Å | θ = 2.9–27.6° |
b = 18.890 (5) Å | µ = 24.00 mm−1 |
c = 6.8843 (18) Å | T = 298 K |
β = 111.906 (3)° | Block, orange |
V = 701.5 (3) Å3 | 0.36 × 0.12 × 0.10 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1210 independent reflections |
Radiation source: fine-focus sealed tube | 966 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.080 |
φ and ω scans | θmax = 25.0°, θmin = 3.4° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −6→6 |
Tmin = 0.04, Tmax = 0.09 | k = −15→22 |
3496 measured reflections | l = −8→8 |
Refinement top
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)] = 0.076 | H-atom parameters constrained |
wR(F2) = 0.214 | w = 1/[σ2(Fo2) + (0.1574P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max < 0.001 |
1210 reflections | Δρmax = 6.35 e Å−3 |
101 parameters | Δρmin = −6.51 e Å−3 |
240 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0063 (15) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pb1 | 0.15777 (11) | 0.54329 (4) | −0.17574 (10) | 0.0184 (5) | |
O1 | 0.745 (3) | 0.5405 (7) | 0.498 (3) | 0.032 (3) | |
O2 | 0.494 (3) | 0.5333 (7) | 0.165 (2) | 0.025 (3) | |
O3 | 0.004 (2) | 0.5627 (8) | 0.114 (2) | 0.025 (3) | |
C1 | 0.541 (4) | 0.5595 (12) | 0.348 (3) | 0.022 (3) | |
C2 | 0.366 (4) | 0.6075 (11) | 0.387 (3) | 0.024 (3) | |
C3 | 0.110 (4) | 0.6090 (11) | 0.261 (3) | 0.023 (3) | |
C4 | −0.035 (4) | 0.6605 (12) | 0.303 (3) | 0.026 (3) | |
H4 | −0.2045 | 0.6607 | 0.2245 | 0.032* | |
C5 | 0.062 (4) | 0.7122 (12) | 0.458 (3) | 0.030 (4) | |
H5 | −0.0418 | 0.7467 | 0.4769 | 0.037* | |
C6 | 0.319 (4) | 0.7121 (13) | 0.587 (4) | 0.034 (4) | |
H6 | 0.3891 | 0.7450 | 0.6936 | 0.041* | |
C7 | 0.460 (4) | 0.6585 (12) | 0.541 (3) | 0.028 (3) | |
H7 | 0.6286 | 0.6572 | 0.6207 | 0.033* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pb1 | 0.0078 (6) | 0.0190 (7) | 0.0211 (6) | −0.0003 (3) | −0.0028 (4) | 0.0011 (3) |
O1 | 0.014 (6) | 0.038 (7) | 0.028 (7) | 0.002 (5) | −0.008 (5) | 0.008 (5) |
O2 | 0.014 (5) | 0.026 (6) | 0.025 (6) | 0.011 (5) | −0.004 (5) | −0.003 (5) |
O3 | 0.009 (5) | 0.028 (6) | 0.031 (5) | 0.003 (5) | −0.002 (4) | −0.003 (5) |
C1 | 0.009 (5) | 0.020 (6) | 0.030 (6) | 0.007 (5) | −0.003 (5) | 0.005 (5) |
C2 | 0.018 (6) | 0.024 (6) | 0.025 (6) | 0.000 (5) | 0.003 (5) | −0.001 (5) |
C3 | 0.013 (5) | 0.022 (6) | 0.029 (6) | 0.000 (5) | 0.001 (5) | −0.002 (5) |
C4 | 0.014 (6) | 0.027 (7) | 0.035 (7) | 0.003 (6) | 0.006 (6) | 0.000 (6) |
C5 | 0.026 (7) | 0.022 (7) | 0.038 (7) | 0.002 (6) | 0.006 (6) | −0.006 (6) |
C6 | 0.028 (7) | 0.024 (7) | 0.039 (7) | −0.005 (6) | −0.001 (6) | −0.007 (7) |
C7 | 0.016 (6) | 0.029 (6) | 0.031 (6) | 0.002 (5) | 0.000 (5) | −0.002 (6) |
Geometric parameters (Å, º) top
Pb1—O3i | 2.318 (16) | C1—C2 | 1.46 (3) |
Pb1—O2 | 2.437 (15) | C2—C7 | 1.38 (3) |
Pb1—O2ii | 2.465 (14) | C2—C3 | 1.41 (3) |
Pb1—O3 | 2.499 (15) | C3—C4 | 1.39 (3) |
Pb1—O1iii | 2.605 (15) | C4—C5 | 1.40 (3) |
O1—C1 | 1.30 (2) | C4—H4 | 0.9300 |
O1—Pb1iv | 2.605 (15) | C5—C6 | 1.43 (3) |
O2—C1 | 1.28 (3) | C5—H5 | 0.9300 |
O2—Pb1ii | 2.465 (13) | C6—C7 | 1.41 (3) |
O3—C3 | 1.31 (3) | C6—H6 | 0.9300 |
O3—Pb1i | 2.318 (16) | C7—H7 | 0.9300 |
| | | |
O3i—Pb1—O2 | 89.5 (5) | O1—C1—C2 | 121 (2) |
O3i—Pb1—O2ii | 82.6 (5) | C7—C2—C3 | 118.5 (19) |
O2—Pb1—O2ii | 64.5 (6) | C7—C2—C1 | 118.2 (18) |
O3i—Pb1—O3 | 71.9 (6) | C3—C2—C1 | 122.9 (19) |
O2—Pb1—O3 | 69.0 (5) | O3—C3—C4 | 118.7 (18) |
O2ii—Pb1—O3 | 126.6 (5) | O3—C3—C2 | 123.2 (18) |
O3i—Pb1—O1iii | 80.4 (5) | C4—C3—C2 | 118 (2) |
O2—Pb1—O1iii | 168.2 (5) | C3—C4—C5 | 122.9 (19) |
O2ii—Pb1—O1iii | 119.7 (5) | C3—C4—H4 | 118.6 |
O3—Pb1—O1iii | 101.7 (5) | C5—C4—H4 | 118.6 |
C1—O1—Pb1iv | 162.6 (14) | C4—C5—C6 | 120 (2) |
C1—O2—Pb1 | 135.6 (12) | C4—C5—H5 | 119.8 |
C1—O2—Pb1ii | 108.9 (12) | C6—C5—H5 | 119.8 |
Pb1—O2—Pb1ii | 115.5 (6) | C7—C6—C5 | 115 (2) |
C3—O3—Pb1i | 122.9 (13) | C7—C6—H6 | 122.6 |
C3—O3—Pb1 | 120.7 (12) | C5—C6—H6 | 122.6 |
Pb1i—O3—Pb1 | 108.1 (6) | C2—C7—C6 | 125.3 (19) |
O2—C1—O1 | 118.3 (19) | C2—C7—H7 | 117.3 |
O2—C1—C2 | 120.9 (17) | C6—C7—H7 | 117.3 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z; (iii) x−1, y, z−1; (iv) x+1, y, z+1. |
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