Poly[μ-salicylato-lead(II)]

In the title compound, [Pb(C₇H₄O₃)]_n, the Pb^II 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.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](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

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Computing details

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)]

Crystal data

[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) Å^3	0.36 × 0.12 × 0.10 mm
Z = 4

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.076	H-atom parameters constrained
wR(F^2) = 0.214	w = 1/[σ^2(Fo^2) + (0.1574P)^2] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0063 (15)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Pb1—O3^i	2.318 (16)	C1—C2	1.46 (3)
Pb1—O2	2.437 (15)	C2—C7	1.38 (3)
Pb1—O2^ii	2.465 (14)	C2—C3	1.41 (3)
Pb1—O3	2.499 (15)	C3—C4	1.39 (3)
Pb1—O1^iii	2.605 (15)	C4—C5	1.40 (3)
O1—C1	1.30 (2)	C4—H4	0.9300
O1—Pb1^iv	2.605 (15)	C5—C6	1.43 (3)
O2—C1	1.28 (3)	C5—H5	0.9300
O2—Pb1^ii	2.465 (13)	C6—C7	1.41 (3)
O3—C3	1.31 (3)	C6—H6	0.9300
O3—Pb1^i	2.318 (16)	C7—H7	0.9300
O3^i—Pb1—O2	89.5 (5)	O1—C1—C2	121 (2)
O3^i—Pb1—O2^ii	82.6 (5)	C7—C2—C3	118.5 (19)
O2—Pb1—O2^ii	64.5 (6)	C7—C2—C1	118.2 (18)
O3^i—Pb1—O3	71.9 (6)	C3—C2—C1	122.9 (19)
O2—Pb1—O3	69.0 (5)	O3—C3—C4	118.7 (18)
O2^ii—Pb1—O3	126.6 (5)	O3—C3—C2	123.2 (18)
O3^i—Pb1—O1^iii	80.4 (5)	C4—C3—C2	118 (2)
O2—Pb1—O1^iii	168.2 (5)	C3—C4—C5	122.9 (19)
O2^ii—Pb1—O1^iii	119.7 (5)	C3—C4—H4	118.6
O3—Pb1—O1^iii	101.7 (5)	C5—C4—H4	118.6
C1—O1—Pb1^iv	162.6 (14)	C4—C5—C6	120 (2)
C1—O2—Pb1	135.6 (12)	C4—C5—H5	119.8
C1—O2—Pb1^ii	108.9 (12)	C6—C5—H5	119.8
Pb1—O2—Pb1^ii	115.5 (6)	C7—C6—C5	115 (2)
C3—O3—Pb1^i	122.9 (13)	C7—C6—H6	122.6
C3—O3—Pb1	120.7 (12)	C5—C6—H6	122.6
Pb1^i—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.