catena-Poly[(2,2′-diamino-4,4′-bi-1,3-thia­zole-κ²N,N′)lead(II)]-di-μ-isonicotintato-κ⁴O:O′]

In the polymeric title compound, [Pb(C₆H₄NO₂)₂C₆H₆N₄S₂)]_n, the Pb^II ion is located on a twofold axis and coordinated by one N,N′-bidentate diamino­bithia­zole (DABT) ligand and four O-monodentate isonicotinate anions in a very distorted cis-PbN₂O₄ octa­hedral geometry. The carboxyl­ate group of the isonicotinate anion bridges two Pb^II ions, forming a polymeric chain. The complete DABT mol­ecule is generated by twofold symmetry; its two thia­zole rings are twisted with a dihedral angle of 9.5 (2)°. There are no π–π stacking inter­actions in the title compound, but N—H...O and N—H...N hydrogen bonds help to stabilize the structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.026
• wR factor = 0.060
• Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for         Pb

Alert level C
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         S1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C4
PLAT322_ALERT_2_C Check Hybridisation of  S1     in Main Residue .          ?

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 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
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

catena-Poly[-(2,2'-diamino-4,4'-bi-1,3-thiazole-κ²N,N')lead(II)]-di-µ- isonicotintato-κ⁴O:O']

Crystal data

[Pb(C6H4NO2)2(C6H6N4S2)]	F(000) = 1240
Mr = 649.66	Dx = 2.106 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1988 reflections
a = 25.430 (3) Å	θ = 2.2–25.0°
b = 10.7493 (19) Å	µ = 8.48 mm^−1
c = 7.7480 (12) Å	T = 295 K
β = 104.715 (12)°	Prism, yellow
V = 2048.5 (6) Å^3	0.12 × 0.10 × 0.10 mm
Z = 4

Data collection

Bruker APEX-2 diffractometer	2077 independent reflections
Radiation source: fine-focus sealed tube	1939 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
φ and ω scans	θmax = 26.2°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −20→31
Tmin = 0.355, Tmax = 0.430	k = −13→13
5814 measured reflections	l = −9→9

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.060	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0262P)^2 + 4.0444P] where P = (Fo^2 + 2Fc^2)/3
2077 reflections	(Δ/σ)max = 0.001
142 parameters	Δρmax = 0.71 e Å^−3
0 restraints	Δρmin = −0.65 e Å^−3

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
Pb	0.5000	0.865740 (19)	0.7500	0.03979 (10)
S1	0.38522 (8)	0.49828 (16)	0.4639 (2)	0.0875 (6)
N1	0.45246 (17)	0.6677 (4)	0.6127 (6)	0.0544 (11)
N2	0.37555 (19)	0.7414 (5)	0.3984 (8)	0.0848 (16)
H2A	0.3863	0.8174	0.4127	0.102*
H2B	0.3454	0.7234	0.3229	0.102*
N3	0.7642 (2)	0.8307 (6)	0.7004 (8)	0.0826 (17)
O1	0.56095 (18)	0.8354 (4)	0.5445 (7)	0.0965 (16)
O2	0.58305 (17)	1.0251 (4)	0.4677 (8)	0.117 (2)
C1	0.4055 (2)	0.6517 (5)	0.4929 (9)	0.0634 (15)
C2	0.4437 (3)	0.4543 (5)	0.6163 (9)	0.079 (2)
H2	0.4531	0.3724	0.6483	0.095*
C3	0.4745 (2)	0.5543 (4)	0.6841 (7)	0.0579 (14)
C4	0.5942 (2)	0.9174 (6)	0.5240 (9)	0.0683 (16)
C5	0.6535 (2)	0.8832 (4)	0.5808 (6)	0.0459 (11)
C6	0.69237 (19)	0.9533 (5)	0.5281 (7)	0.0525 (12)
H6	0.6822	1.0204	0.4511	0.063*
C7	0.7458 (2)	0.9224 (6)	0.5913 (8)	0.0692 (15)
H7	0.7712	0.9704	0.5536	0.083*
C8	0.7267 (3)	0.7636 (6)	0.7494 (8)	0.083 (2)
H8	0.7385	0.6975	0.8269	0.100*
C9	0.6712 (3)	0.7848 (4)	0.6938 (7)	0.0608 (14)
H9	0.6468	0.7340	0.7317	0.073*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb	0.02339 (13)	0.02956 (13)	0.06173 (18)	0.000	0.00216 (10)	0.000
S1	0.1103 (14)	0.0813 (11)	0.0854 (11)	−0.0638 (10)	0.0514 (11)	−0.0409 (9)
N1	0.043 (2)	0.038 (2)	0.085 (3)	−0.0111 (18)	0.022 (2)	−0.015 (2)
N2	0.043 (3)	0.084 (4)	0.113 (4)	−0.012 (3)	−0.006 (3)	−0.024 (3)
N3	0.060 (3)	0.079 (4)	0.091 (4)	0.028 (3)	−0.014 (3)	−0.016 (3)
O1	0.058 (3)	0.094 (3)	0.149 (5)	−0.037 (2)	0.046 (3)	−0.052 (3)
O2	0.054 (3)	0.063 (3)	0.194 (6)	0.015 (2)	−0.045 (3)	−0.020 (3)
C1	0.047 (3)	0.065 (3)	0.085 (4)	−0.023 (3)	0.029 (3)	−0.030 (3)
C2	0.119 (6)	0.041 (3)	0.102 (5)	−0.026 (3)	0.073 (5)	−0.018 (3)
C3	0.069 (3)	0.041 (2)	0.080 (4)	−0.010 (2)	0.047 (3)	−0.012 (2)
C4	0.041 (3)	0.059 (3)	0.095 (4)	0.001 (3)	0.000 (3)	−0.027 (3)
C5	0.040 (3)	0.040 (2)	0.054 (3)	0.0006 (19)	0.005 (2)	−0.0058 (19)
C6	0.042 (3)	0.053 (3)	0.060 (3)	0.001 (2)	0.009 (2)	0.012 (2)
C7	0.044 (3)	0.077 (4)	0.086 (4)	−0.004 (3)	0.015 (3)	−0.008 (3)
C8	0.118 (6)	0.052 (3)	0.063 (4)	0.035 (4)	−0.007 (4)	0.006 (3)
C9	0.083 (4)	0.035 (2)	0.067 (3)	0.000 (3)	0.025 (3)	−0.001 (2)

Geometric parameters (Å, º)

Pb—N1	2.544 (4)	C4—O1	1.259 (7)
Pb—N1^i	2.544 (4)	C4—O2	1.244 (8)
Pb—O1	2.510 (4)	C2—C3	1.354 (7)
Pb—O1^i	2.510 (4)	C2—H2	0.9300
Pb—O2^ii	2.622 (4)	C3—C3^i	1.433 (12)
Pb—O2^iii	2.622 (4)	C4—C5	1.504 (7)
S1—C2	1.714 (8)	C5—C9	1.374 (7)
S1—C1	1.726 (5)	C5—C6	1.385 (6)
N1—C1	1.324 (7)	C6—C7	1.364 (7)
N1—C3	1.396 (7)	C6—H6	0.9300
N2—C1	1.327 (8)	C7—H7	0.9300
N2—H2A	0.8600	C8—C9	1.385 (9)
N2—H2B	0.8600	C8—H8	0.9300
N3—C7	1.305 (8)	C9—H9	0.9300
N3—C8	1.325 (9)
O1^i—Pb—O1	165.1 (2)	N1—C1—S1	113.7 (5)
O1^i—Pb—N1	81.49 (16)	N2—C1—S1	120.8 (5)
O1—Pb—N1	86.01 (13)	C3—C2—S1	111.3 (5)
O1^i—Pb—N1^i	86.01 (13)	C3—C2—H2	124.3
O1—Pb—N1^i	81.49 (16)	S1—C2—H2	124.3
N1—Pb—N1^i	66.4 (2)	C2—C3—N1	113.9 (6)
O1^i—Pb—O2^iii	100.2 (2)	C2—C3—C3^i	127.3 (4)
O1—Pb—O2^iii	86.55 (18)	N1—C3—C3^i	118.8 (3)
N1—Pb—O2^iii	149.69 (14)	O2—C4—O1	126.5 (6)
N1^i—Pb—O2^iii	83.46 (14)	O2—C4—C5	116.9 (5)
O1^i—Pb—O2^ii	86.55 (18)	O1—C4—C5	116.6 (6)
O1—Pb—O2^ii	100.2 (2)	C9—C5—C6	117.6 (5)
N1—Pb—O2^ii	83.46 (14)	C9—C5—C4	121.1 (5)
N1^i—Pb—O2^ii	149.69 (14)	C6—C5—C4	121.2 (5)
O2^iii—Pb—O2^ii	126.8 (2)	C7—C6—C5	118.9 (5)
C2—S1—C1	89.7 (3)	C7—C6—H6	120.6
C1—N1—C3	111.4 (4)	C5—C6—H6	120.6
C1—N1—Pb	130.5 (4)	N3—C7—C6	125.1 (6)
C3—N1—Pb	117.7 (3)	N3—C7—H7	117.4
C1—N2—H2A	120.0	C6—C7—H7	117.4
C1—N2—H2B	120.0	N3—C8—C9	124.8 (5)
H2A—N2—H2B	120.0	N3—C8—H8	117.6
C7—N3—C8	115.6 (5)	C9—C8—H8	117.6
C4—O1—Pb	122.2 (4)	C5—C9—C8	117.9 (5)
C4—O2—Pb^ii	135.8 (4)	C5—C9—H9	121.0
N1—C1—N2	125.6 (5)	C8—C9—H9	121.0

Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1, −y+2, −z+1; (iii) x, −y+2, z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O2^ii	0.86	1.99	2.816 (7)	160
N2—H2B···N3^iv	0.86	2.12	2.961 (8)	164

Symmetry codes: (ii) −x+1, −y+2, −z+1; (iv) x−1/2, −y+3/2, z−1/2.