Poly[[diaqua­(μ₄-3-sulfonatobenzoato)lead(II)] 4,4′-bipyridine]

The title compound, [Pb(C₇H₄O₅S)(H₂O)₂]·C₁₀H₈N₂, crystallizes as a two-dimensional coordination polymer. Double sheets are formed by Pb²⁺ ions which are connected by μ₄-bridging 3-sulfonatobenzoate groups. The coordination around the Pb atoms comprises three O atoms from carboxyl­ate groups, two O atoms from the sulfonate group and additionally two water mol­ecules. As a result of hydrogen bonds between 4,4′-bipyridine and water mol­ecules attached to Pb²⁺ the double layer structure is extended to give a three-dimensional supra­molecular architecture.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.019
• wR factor = 0.056
• Data-to-parameter ratio = 12.5

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)        4000 Deg.
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT731_ALERT_1_C Bond    Calc     0.84(4), Rep   0.841(19) ......       2.11 su-Ra
              O6   -H6      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.855(19) ......       2.11 su-Ra
              O6   -H5      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.84(5), Rep   0.844(19) ......       2.63 su-Ra
              O7   -H7      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.846(19) ......       2.11 su-Ra
              O7   -H8      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(4), Rep   0.842(19) ......       2.11 su-Ra
              O6   -H6      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.846(19) ......       2.11 su-Ra
              O7   -H8      1.555   1.555

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
PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............          1 Times

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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

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Computing details

Data collection: STADI-4 (Stoe & Cie, 1996); cell refinement: STADI-4; data reduction: STADI-4; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

Poly[[diaqua(µ₄-3-sulfonatobenzoato)lead(II)] 4,4'-bipyridine]

Crystal data

[Pb(C7H4O5S)(H2O)2]·C10H8N2	Z = 2
Mr = 599.57	F(000) = 572
Triclinic, P1	Dx = 2.080 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.178 (5) Å	Cell parameters from 24 reflections
b = 9.483 (4) Å	θ = 7.7–11.0°
c = 12.790 (6) Å	µ = 8.96 mm^−1
α = 89.19 (4)°	T = 293 K
β = 80.73 (4)°	Needle, colourless
γ = 78.05 (4)°	0.38 × 0.09 × 0.09 mm
V = 957.5 (9) Å^3

Data collection

Stoe Stadi-4 diffractometer	3236 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.031
Graphite monochromator	θmax = 25.0°, θmin = 1.6°
ω–2θ scans	h = −9→9
Absorption correction: ψ scan (X-RED32; Stoe & Cie, 1996)	k = −11→11
Tmin = 0.054, Tmax = 0.445	l = −15→15
6715 measured reflections	2 standard reflections every 60 min
3380 independent reflections	intensity decay: random variation +−5%

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)] = 0.019	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.056	w = 1/[σ^2(Fo^2) + (0.0311P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.19	(Δ/σ)max < 0.001
3380 reflections	Δρmax = 0.98 e Å^−3
270 parameters	Δρmin = −0.79 e Å^−3
6 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: 0.0110 (6)

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
C1	−0.2082 (5)	0.8695 (4)	0.8971 (3)	0.0272 (7)
C2	−0.1912 (5)	1.0093 (4)	0.8775 (3)	0.0289 (8)
H1	−0.0887	1.0356	0.8807	0.035*
C3	−0.3275 (5)	1.1109 (4)	0.8530 (3)	0.0268 (7)
C4	−0.4814 (5)	1.0731 (4)	0.8480 (3)	0.0323 (8)
H2	−0.5717	1.1412	0.8305	0.039*
C5	−0.4990 (5)	0.9339 (5)	0.8691 (3)	0.0357 (9)
H3	−0.6020	0.9081	0.8663	0.043*
C6	−0.3634 (5)	0.8310 (4)	0.8948 (3)	0.0326 (8)
H4	−0.3764	0.7374	0.9102	0.039*
C7	−0.0566 (5)	0.7582 (4)	0.9169 (3)	0.0310 (8)
C8	0.1887 (6)	1.0826 (5)	0.5183 (3)	0.0369 (9)
C9	0.1455 (7)	1.0637 (6)	0.6272 (4)	0.0488 (12)
H9	0.0655	1.1336	0.6685	0.059*
C10	0.2226 (8)	0.9409 (7)	0.6726 (4)	0.0568 (14)
H10	0.1924	0.9307	0.7451	0.068*
C11	0.3794 (7)	0.8532 (6)	0.5155 (4)	0.0525 (12)
H11	0.4609	0.7817	0.4768	0.063*
C12	0.3080 (7)	0.9717 (6)	0.4620 (4)	0.0453 (11)
H12	0.3392	0.9775	0.3892	0.054*
C13	0.1063 (6)	1.2131 (5)	0.4656 (3)	0.0372 (10)
C14	−0.0538 (6)	1.2910 (5)	0.5067 (3)	0.0424 (10)
H13	−0.1099	1.2663	0.5713	0.051*
C15	−0.1294 (6)	1.4050 (5)	0.4514 (4)	0.0468 (11)
H14	−0.2381	1.4539	0.4795	0.056*
C16	0.1007 (7)	1.3789 (6)	0.3226 (3)	0.0505 (12)
H15	0.1558	1.4100	0.2598	0.061*
C17	0.1860 (7)	1.2625 (5)	0.3714 (3)	0.0450 (11)
H16	0.2955	1.2172	0.3419	0.054*
N1	0.3383 (6)	0.8352 (5)	0.6193 (4)	0.0552 (11)
N2	−0.0555 (6)	1.4495 (4)	0.3597 (3)	0.0477 (10)
O1	0.0872 (4)	0.7877 (3)	0.8987 (3)	0.0461 (7)
O2	−0.0770 (4)	0.6341 (3)	0.9488 (3)	0.0420 (7)
O3	−0.4341 (4)	1.3750 (3)	0.9185 (2)	0.0398 (7)
O4	−0.3510 (5)	1.3319 (3)	0.7294 (2)	0.0487 (8)
O5	−0.1396 (4)	1.3006 (4)	0.8471 (3)	0.0538 (8)
O6	0.4130 (5)	0.6056 (4)	0.7615 (3)	0.0545 (9)
H6	0.402 (7)	0.668 (4)	0.714 (3)	0.060 (17)*
H5	0.484 (6)	0.531 (4)	0.735 (4)	0.064 (18)*
O7	0.1772 (4)	0.3802 (4)	0.8005 (2)	0.0416 (7)
H7	0.086 (5)	0.352 (7)	0.819 (4)	0.09 (2)*
H8	0.174 (6)	0.423 (6)	0.742 (3)	0.057 (16)*
S	−0.30985 (12)	1.29300 (10)	0.83358 (7)	0.0309 (2)
Pb	0.243824 (15)	0.539897 (14)	0.933755 (10)	0.02885 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0266 (19)	0.0212 (18)	0.0304 (17)	0.0007 (15)	−0.0027 (14)	0.0036 (14)
C2	0.0214 (18)	0.027 (2)	0.0369 (18)	−0.0021 (15)	−0.0028 (15)	−0.0001 (15)
C3	0.0268 (19)	0.0226 (19)	0.0283 (16)	0.0003 (15)	−0.0038 (15)	0.0018 (14)
C4	0.030 (2)	0.031 (2)	0.0345 (18)	−0.0006 (17)	−0.0082 (16)	0.0045 (15)
C5	0.031 (2)	0.034 (2)	0.043 (2)	−0.0071 (18)	−0.0088 (17)	0.0002 (17)
C6	0.036 (2)	0.027 (2)	0.0352 (18)	−0.0069 (18)	−0.0060 (16)	0.0037 (16)
C7	0.032 (2)	0.024 (2)	0.0325 (18)	0.0022 (17)	−0.0045 (16)	0.0045 (15)
C8	0.042 (2)	0.038 (2)	0.036 (2)	−0.017 (2)	−0.0103 (18)	0.0083 (17)
C9	0.054 (3)	0.058 (3)	0.034 (2)	−0.010 (3)	−0.008 (2)	0.010 (2)
C10	0.062 (3)	0.072 (4)	0.043 (2)	−0.021 (3)	−0.020 (2)	0.021 (3)
C11	0.051 (3)	0.043 (3)	0.066 (3)	−0.012 (2)	−0.014 (2)	0.005 (2)
C12	0.054 (3)	0.043 (3)	0.040 (2)	−0.014 (2)	−0.006 (2)	0.0041 (19)
C13	0.045 (3)	0.041 (2)	0.0309 (18)	−0.019 (2)	−0.0114 (18)	0.0023 (17)
C14	0.046 (3)	0.046 (3)	0.038 (2)	−0.019 (2)	−0.0057 (19)	0.0053 (19)
C15	0.044 (3)	0.046 (3)	0.053 (2)	−0.012 (2)	−0.012 (2)	0.002 (2)
C16	0.069 (4)	0.050 (3)	0.034 (2)	−0.018 (3)	−0.007 (2)	0.007 (2)
C17	0.054 (3)	0.044 (3)	0.034 (2)	−0.008 (2)	−0.002 (2)	0.0064 (18)
N1	0.060 (3)	0.053 (3)	0.061 (2)	−0.021 (2)	−0.025 (2)	0.022 (2)
N2	0.061 (3)	0.039 (2)	0.049 (2)	−0.014 (2)	−0.020 (2)	0.0062 (17)
O1	0.0273 (15)	0.0363 (17)	0.0702 (19)	−0.0005 (13)	−0.0038 (14)	0.0216 (15)
O2	0.0375 (16)	0.0268 (16)	0.0602 (17)	−0.0043 (13)	−0.0086 (14)	0.0175 (13)
O3	0.0415 (17)	0.0300 (16)	0.0413 (15)	0.0044 (14)	−0.0019 (13)	−0.0053 (12)
O4	0.071 (2)	0.0335 (17)	0.0364 (14)	−0.0017 (16)	−0.0045 (15)	0.0094 (12)
O5	0.0338 (17)	0.0342 (18)	0.094 (2)	−0.0098 (14)	−0.0102 (17)	0.0125 (17)
O6	0.054 (2)	0.038 (2)	0.059 (2)	0.0069 (18)	0.0040 (17)	0.0206 (17)
O7	0.0358 (17)	0.0441 (19)	0.0461 (17)	−0.0118 (15)	−0.0066 (14)	0.0067 (14)
S	0.0295 (5)	0.0208 (5)	0.0383 (5)	0.0010 (4)	−0.0022 (4)	0.0039 (4)
Pb	0.02344 (11)	0.02329 (11)	0.03851 (11)	−0.00113 (6)	−0.00640 (6)	0.00609 (6)

Geometric parameters (Å, º)

C1—C2	1.376 (5)	C13—C17	1.398 (6)
C1—C6	1.397 (5)	C14—C15	1.376 (7)
C1—C7	1.505 (5)	C14—H13	0.9300
C2—C3	1.389 (5)	C15—N2	1.335 (6)
C2—H1	0.9300	C15—H14	0.9300
C3—C4	1.390 (6)	C16—N2	1.329 (7)
C3—S	1.773 (4)	C16—C17	1.377 (7)
C4—C5	1.375 (6)	C16—H15	0.9300
C4—H2	0.9300	C17—H16	0.9300
C5—C6	1.396 (6)	Pb—O1	2.504 (3)
C5—H3	0.9300	Pb—O2	2.567 (4)
C6—H4	0.9300	Pb—O2^i	2.654 (3)
C7—O1	1.250 (5)	Pb—O3^ii	2.749 (4)
C7—O2	1.275 (5)	Pb—O3^iii	2.856 (3)
C8—C12	1.395 (7)	O2—Pb^i	2.654 (3)
C8—C9	1.400 (6)	O3—S	1.469 (3)
C8—C13	1.489 (6)	O3—Pb^iv	2.749 (4)
C9—C10	1.373 (8)	O4—S	1.451 (3)
C9—H9	0.9300	O5—S	1.447 (3)
C10—N1	1.335 (8)	Pb—O6	2.549 (4)
C10—H10	0.9300	O6—H6	0.841 (19)
C11—N1	1.334 (7)	O6—H5	0.855 (19)
C11—C12	1.380 (7)	Pb—O7	2.492 (3)
C11—H11	0.9300	O7—H7	0.844 (19)
C12—H12	0.9300	O7—H8	0.846 (19)
C13—C14	1.388 (7)	O3—Pb^iv	2.749 (4)
C2—C1—C6	120.0 (4)	N2—C16—H15	118.0
C2—C1—C7	119.4 (3)	C17—C16—H15	118.0
C6—C1—C7	120.6 (3)	C16—C17—C13	119.3 (5)
C1—C2—C3	119.8 (3)	C16—C17—H16	120.3
C1—C2—H1	120.1	C13—C17—H16	120.3
C3—C2—H1	120.1	C11—N1—C10	116.5 (5)
C2—C3—C4	120.7 (4)	C16—N2—C15	116.6 (4)
C2—C3—S	120.1 (3)	C7—O1—Pb	95.4 (2)
C4—C3—S	119.1 (3)	C7—O2—Pb	91.8 (2)
C5—C4—C3	119.4 (4)	C7—O2—Pb^i	152.7 (3)
C5—C4—H2	120.3	Pb—O2—Pb^i	110.41 (11)
C3—C4—H2	120.3	S—O3—Pb^iv	135.60 (17)
C4—C5—C6	120.5 (4)	Pb—O6—H6	139 (4)
C4—C5—H3	119.8	Pb—O6—H5	109 (3)
C6—C5—H3	119.8	H6—O6—H5	108 (3)
C5—C6—C1	119.5 (4)	Pb—O7—H7	114 (5)
C5—C6—H4	120.2	Pb—O7—H8	110 (4)
C1—C6—H4	120.2	H7—O7—H8	109 (3)
O1—C7—O2	121.3 (4)	O5—S—O4	114.8 (2)
O1—C7—C1	119.5 (4)	O5—S—O3	110.5 (2)
O2—C7—C1	119.3 (4)	O4—S—O3	112.0 (2)
C12—C8—C9	116.7 (5)	O5—S—C3	106.67 (19)
C12—C8—C13	122.2 (4)	O4—S—C3	107.18 (18)
C9—C8—C13	121.1 (4)	O3—S—C3	105.05 (18)
C10—C9—C8	119.3 (5)	O1—Pb—O2	51.41 (10)
C10—C9—H9	120.4	O1—Pb—O2^i	118.59 (11)
C8—C9—H9	120.4	O1—Pb—O3^ii	141.79 (10)
N1—C10—C9	124.3 (5)	O1—Pb—O3^iii	96.80 (11)
N1—C10—H10	117.9	O1—Pb—O6	76.72 (12)
C9—C10—H10	117.9	O1—Pb—O7	105.00 (11)
N1—C11—C12	123.9 (6)	O2—Pb—O2^i	69.59 (11)
N1—C11—H11	118.1	O2—Pb—O3^ii	166.11 (10)
C12—C11—H11	118.1	O2—Pb—O3^iii	121.90 (10)
C11—C12—C8	119.4 (5)	O2—Pb—O6	113.72 (12)
C11—C12—H12	120.3	O2—Pb—O7	79.65 (11)
C8—C12—H12	120.3	O2^i—Pb—O3^ii	98.79 (10)
C14—C13—C17	116.6 (4)	O2^i—Pb—O3^iii	100.95 (10)
C14—C13—C8	121.9 (4)	O2^i—Pb—O6	152.37 (12)
C17—C13—C8	121.5 (4)	O2^i—Pb—O7	76.48 (11)
C15—C14—C13	119.7 (4)	O3^ii—Pb—O3^iii	66.64 (11)
C15—C14—H13	120.1	O3^ii—Pb—O6	72.88 (11)
C13—C14—H13	120.1	O3^ii—Pb—O7	90.41 (11)
N2—C15—C14	123.7 (5)	O3^iii—Pb—O6	99.63 (12)
N2—C15—H14	118.1	O3^iii—Pb—O7	156.45 (10)
C14—C15—H14	118.1	O6—Pb—O7	77.27 (13)
N2—C16—C17	123.9 (5)
C6—C1—C2—C3	−1.5 (5)	O2—C7—O1—Pb	3.8 (4)
C7—C1—C2—C3	176.2 (3)	C1—C7—O1—Pb	−174.0 (3)
C1—C2—C3—C4	0.0 (5)	O1—C7—O2—Pb	−3.7 (4)
C1—C2—C3—S	177.1 (3)	C1—C7—O2—Pb	174.2 (3)
C2—C3—C4—C5	1.0 (5)	O1—C7—O2—Pb^i	141.7 (5)
S—C3—C4—C5	−176.2 (3)	C1—C7—O2—Pb^i	−40.5 (7)
C3—C4—C5—C6	−0.4 (6)	Pb^iv—O3—S—O5	145.2 (2)
C4—C5—C6—C1	−1.1 (6)	Pb^iv—O3—S—O4	15.9 (3)
C2—C1—C6—C5	2.0 (5)	Pb^iv—O3—S—C3	−100.1 (3)
C7—C1—C6—C5	−175.6 (3)	C2—C3—S—O5	0.8 (4)
C2—C1—C7—O1	−11.4 (5)	C4—C3—S—O5	178.0 (3)
C6—C1—C7—O1	166.3 (4)	C2—C3—S—O4	124.1 (3)
C2—C1—C7—O2	170.7 (3)	C4—C3—S—O4	−58.6 (3)
C6—C1—C7—O2	−11.6 (5)	C2—C3—S—O3	−116.5 (3)
C12—C8—C9—C10	0.9 (7)	C4—C3—S—O3	60.7 (3)
C13—C8—C9—C10	179.1 (5)	C7—O1—Pb—O7	61.1 (3)
C8—C9—C10—N1	−0.2 (9)	C7—O1—Pb—O6	133.8 (3)
N1—C11—C12—C8	1.7 (8)	C7—O1—Pb—O2	−2.1 (2)
C9—C8—C12—C11	−1.6 (7)	C7—O1—Pb—O2^i	−21.5 (3)
C13—C8—C12—C11	−179.8 (4)	C7—O1—Pb—O3^ii	171.7 (2)
C12—C8—C13—C14	152.5 (4)	C7—O1—Pb—O3^iii	−127.9 (2)
C9—C8—C13—C14	−25.5 (6)	C7—O2—Pb—O7	−116.8 (2)
C12—C8—C13—C17	−26.7 (6)	Pb^i—O2—Pb—O7	79.31 (13)
C9—C8—C13—C17	155.2 (4)	C7—O2—Pb—O1	2.0 (2)
C17—C13—C14—C15	3.7 (6)	Pb^i—O2—Pb—O1	−161.85 (19)
C8—C13—C14—C15	−175.6 (4)	C7—O2—Pb—O6	−45.8 (3)
C13—C14—C15—N2	−1.8 (7)	Pb^i—O2—Pb—O6	150.34 (13)
N2—C16—C17—C13	0.1 (8)	C7—O2—Pb—O2^i	163.9 (3)
C14—C13—C17—C16	−2.9 (6)	Pb^i—O2—Pb—O2^i	0.0
C8—C13—C17—C16	176.4 (4)	C7—O2—Pb—O3^ii	−161.7 (3)
C12—C11—N1—C10	−1.0 (8)	Pb^i—O2—Pb—O3^ii	34.4 (4)
C9—C10—N1—C11	0.2 (8)	C7—O2—Pb—O3^iii	73.5 (3)
C17—C16—N2—C15	1.9 (7)	Pb^i—O2—Pb—O3^iii	−90.41 (13)
C14—C15—N2—C16	−1.0 (7)

Symmetry codes: (i) −x, −y+1, −z+2; (ii) x+1, y−1, z; (iii) −x, −y+2, −z+2; (iv) x−1, y+1, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6···N1	0.84 (2)	2.02 (2)	2.849 (6)	170 (5)
O7—H8···N2^v	0.85 (2)	1.99 (3)	2.773 (5)	153 (5)

Symmetry code: (v) −x, −y+2, −z+1.