Bis(2,2′-diamino-4,4′-bi-1,3-thia­zole-κ2N3,N3′)bis­(nitrato-κO)lead(II) dihydrate

Liu, B.-X.; Xu, D.-J.

doi:10.1107/S1600536809029638

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Pages m1002-m1003

doi:10.1107/S1600536809029638

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Bis(2,2′-diamino-4,4′-bi-1,3-thiazole-κ²N³,N^3′)bis(nitrato-κO)lead(II) dihydrate

Bing-Xin Liu ^a and Duan-Jun Xu ^b ^*

^aDepartment of Chemistry, Shanghai University, 200444 People's Republic of China, and ^bDepartment of Chemistry, Zhejiang University, Hangzhou, 310027, People's Republic of China
^*Correspondence e-mail: xudj@mail.hz.zj.cn

(Received 23 July 2009; accepted 24 July 2009; online 29 July 2009)

In the title compound, [Pb(NO₃)₂(C₆H₆N₄S₂)₂]·2H₂O, the Pb^II cation is N,N′-chelated by two 2,2′-diamino-4,4′-bi-1,3-thiazole (DABT) ligands and further is cis coordinated by two nitrate anions in a distorted PbN₄O₂ octahedral geometry. One of the uncoordinated water molecules is close to an inversion center and is disordered equally over two sites. Intramolecular N—H⋯N and N—H⋯O interactions are present. An extensive hydrogen-bonding network of types N—H⋯O, O—H⋯O, O—H⋯N and O—H⋯S consolidates the crystal structure.

Related literature

For the application of 2,2′-diamino-4,4′-bi-1,3-thiazole complexes as soft magnetic materials, see: Sun et al. (1997 ). For general background to the structures of complexes of 2,2′-diamino-4,4′-bi-1,3-thiazole, see: Liu et al. (2003 ). For Pb—N bond distances in 2,2′-diamino-4,4′-bi-1,3-thiazole complexes, see: Abedini et al. (2005 ); Liu et al. (2006 ). H atoms bonded to the disordered O atoms were placed in calculated positions, see: Nardelli (1999 )

Experimental

Crystal data

[Pb(NO₃)₂(C₆H₆N₄S₂)₂]·2H₂O
M_r = 1527.66
Triclinic, $[P \overline 1]$
a = 9.2387 (8) Å
b = 9.6962 (9) Å
c = 13.5636 (6) Å
α = 105.731 (4)°
β = 90.377 (3)°
γ = 97.072 (5)°
V = 1159.61 (16) Å³
Z = 1
Mo Kα radiation
μ = 7.70 mm⁻¹
T = 294 K
0.21 × 0.16 × 0.14 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.215, T_max = 0.340
6095 measured reflections
4012 independent reflections
3705 reflections with I > 2σ(I)
R_int = 0.015

Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.065
S = 1.08
4012 reflections
319 parameters
H-atom parameters constrained
Δρ_max = 0.83 e Å⁻³
Δρ_min = −0.46 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb—N1	2.656 (4)
Pb—N3	2.563 (4)
Pb—N5	2.535 (5)
Pb—N7	2.692 (4)
Pb—O1	2.704 (4)
Pb—O4	2.803 (5)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯O1	0.92	2.08	2.884 (8)	145
N2—H2B⋯O4ⁱ	0.90	2.33	3.209 (7)	165
N2—H2B⋯O6ⁱ	0.90	2.31	3.057 (7)	140
N4—H4A⋯N7	0.99	2.19	3.168 (7)	166
N4—H4B⋯O1Wⁱⁱ	0.88	2.29	3.015 (8)	141
N4—H4B⋯O2WAⁱⁱⁱ	0.88	2.26	2.98 (9)	140
N6—H6A⋯N1	0.93	2.22	3.119 (8)	160
N6—H6B⋯O2WA^iv	0.96	2.29	3.12 (10)	145
N6—H6B⋯O1W^iv	0.96	2.10	2.929 (10)	144
N8—H8A⋯O3^v	0.90	2.17	3.027 (7)	159
N8—H8B⋯O4	0.84	2.13	2.916 (7)	156
O1W—H1A⋯O3	0.85	1.94	2.782 (8)	168
O1W—H1B⋯O2WA	0.83	1.97	2.54 (9)	125
O1W—H1B⋯O2WB	0.83	2.14	2.93 (4)	160
O2WA—H2C⋯N4ⁱⁱⁱ	0.85	2.42	2.98 (9)	124
O2WA—H2D⋯O1W^vi	0.85	2.17	2.85 (9)	136
O2WB—H2E⋯S4ⁱⁱⁱ	0.85	2.27	3.09 (5)	164
O2WB—H2F⋯S3^vii	0.85	2.80	3.53 (5)	144
O2WB—H2F⋯N6^vii	0.85	1.91	2.67 (5)	148
Symmetry codes: (i) x+1, y, z; (ii) x-1, y-1, z; (iii) -x+1, -y+1, -z; (iv) x, y-1, z; (v) x-1, y, z; (vi) -x+2, -y+2, -z; (vii) -x+2, -y+1, -z.

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809029638/hk2747sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809029638/hk2747Isup2.hkl

checkCIF report

Comment top

Some metal complexes of 2,2'-diamino-4,4'-bi-1,3-thiazole (DABT) have shown potential application in the field of soft magnetic material (Sun et al., 1997). As part of the ongoing structural investigation of metal complexes with DABT ligand (Liu et al., 2003), the title Pb^II complex has recently been prepared and its crystal structure is reported herein.

In the title compound, the Pb^II cation is N,N'-chelated by two DABT ligands and further is cis-coordinated by two nitrate anions in a distorted PbN₄O₂ octahedral geometry (Fig. 1). The Pb—N bond distances (Table 1) are somewhat longer than those [2.527, 2.544 and 2.551 Å] found in other two Pb complexes with DABT ligand (Abedini et al. 2005; Liu et al. 2006). One of the lattice water molecules is close to an inversion center and is disordered equally over two sites. The extensive hydrogen bonding network of types N—H···O, O—H···O, O—H···N and O—H···S is present in the crystal structure.

Related literature top

For the application of 2,2'-diamino-4,4'-bi-1,3-thiazole complexes as soft magnetic materials, see: Sun et al. (1997). For general background to the structures of complexes of 2,2'-diamino-4,4'-bi-1,3-thiazole, see: Liu et al. (2003). For Pb—N bond distances in 2,2'-diamino-4,4'-bi-1,3-thiazole complexes, see: Abedini et al. (2005); Liu et al. (2006).

Experimental top

An aqueous solution (15 ml) of DABT (0.20 g, 1 mmol) and Pb(NO₃)₂ (0.33 g, 1 mmol) was refluxed for 4 h. The solution was filtered after cooling to room temperature. Yellow single crystals were obtained from the filtrate after 4 d.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002), and Nardelli (1999); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. The molecular structure of the title compound with 30% probability displacement ellipsoids (arbitrary spheres for H atoms); dashed lines indicate the hydrogen bonding.

Bis(2,2'-diamino-4,4'-bi-1,3-thiazole- κ²N³,N^3')bis(nitrato-κO)lead(II) dihydrate top

Crystal data top

[Pb(NO₃)₂(C₆H₆N₄S₂)₂]·2H₂O	Z = 1
M_r = 1527.66	F(000) = 736
Triclinic, P1	D_x = 2.187 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.2387 (8) Å	Cell parameters from 4246 reflections
b = 9.6962 (9) Å	θ = 2.2–25.0°
c = 13.5636 (6) Å	µ = 7.70 mm⁻¹
α = 105.731 (4)°	T = 294 K
β = 90.377 (3)°	Block, yellow
γ = 97.072 (5)°	0.21 × 0.16 × 0.14 mm
V = 1159.61 (16) Å³

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	4012 independent reflections
Radiation source: fine-focus sealed tube	3705 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.015
Detector resolution: 10.0 pixels mm^-1	θ_max = 25.0°, θ_min = 1.6°
ω scans	h = −9→10
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −9→11
T_min = 0.215, T_max = 0.340	l = −16→15
6095 measured reflections

Refinement top

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.065	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0293P)² + 1.6634P] where P = (F_o² + 2F_c²)/3
4012 reflections	(Δ/σ)_max = 0.004
319 parameters	Δρ_max = 0.83 e Å⁻³
0 restraints	Δρ_min = −0.46 e Å⁻³

Crystal data top

[Pb(NO₃)₂(C₆H₆N₄S₂)₂]·2H₂O	γ = 97.072 (5)°
M_r = 1527.66	V = 1159.61 (16) Å³
Triclinic, P1	Z = 1
a = 9.2387 (8) Å	Mo Kα radiation
b = 9.6962 (9) Å	µ = 7.70 mm⁻¹
c = 13.5636 (6) Å	T = 294 K
α = 105.731 (4)°	0.21 × 0.16 × 0.14 mm
β = 90.377 (3)°

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	4012 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	3705 reflections with I > 2σ(I)
T_min = 0.215, T_max = 0.340	R_int = 0.015
6095 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.065	H-atom parameters constrained
S = 1.08	Δρ_max = 0.83 e Å⁻³
4012 reflections	Δρ_min = −0.46 e Å⁻³
319 parameters

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	U_iso*/U_eq	Occ. (<1)
Pb	0.51296 (2)	0.384529 (19)	0.321343 (15)	0.03622 (8)
S1	0.86425 (18)	0.07481 (19)	0.43924 (14)	0.0634 (4)
S2	0.20076 (16)	−0.09836 (15)	0.28488 (12)	0.0527 (4)
S3	0.6251 (3)	0.1416 (2)	−0.04539 (14)	0.0887 (6)
S4	0.1267 (3)	0.5374 (2)	0.10337 (14)	0.0845 (6)
N1	0.6815 (5)	0.2053 (5)	0.3667 (3)	0.0462 (11)
N2	0.9129 (5)	0.3416 (6)	0.4149 (5)	0.0660 (15)
H2A	0.9059	0.4168	0.3862	0.079*
H2B	1.0104	0.3441	0.4233	0.079*
N3	0.3856 (4)	0.1266 (4)	0.2963 (3)	0.0395 (9)
N4	0.1501 (5)	0.1384 (5)	0.2314 (4)	0.0614 (14)
H4A	0.1852	0.2369	0.2254	0.074*
H4B	0.0971	0.0753	0.1816	0.074*
N5	0.5432 (6)	0.2735 (5)	0.1318 (3)	0.0537 (12)
N6	0.7467 (8)	0.1533 (8)	0.1351 (5)	0.101 (2)
H6A	0.7241	0.1444	0.2003	0.121*
H6B	0.8060	0.0773	0.1133	0.121*
N7	0.3075 (5)	0.4293 (5)	0.1959 (3)	0.0450 (10)
N8	0.1492 (5)	0.5684 (5)	0.3050 (4)	0.0566 (12)
H8A	0.0613	0.5979	0.3009	0.068*
H8B	0.1761	0.5443	0.3564	0.068*
N9	0.2813 (5)	0.3333 (5)	0.4915 (3)	0.0417 (10)
N10	0.7714 (5)	0.5968 (5)	0.2504 (4)	0.0499 (11)
O1	0.7860 (4)	0.4915 (5)	0.2859 (4)	0.0662 (12)
O2	0.6464 (4)	0.6191 (5)	0.2306 (3)	0.0637 (11)
O3	0.8811 (5)	0.6758 (5)	0.2381 (4)	0.0757 (13)
O4	0.2622 (5)	0.4100 (5)	0.4368 (4)	0.0767 (14)
O5	0.4074 (4)	0.3241 (4)	0.5214 (3)	0.0583 (10)
O6	0.1759 (5)	0.2579 (6)	0.5126 (4)	0.0799 (14)
C1	0.8164 (6)	0.2223 (6)	0.4046 (4)	0.0465 (13)
C2	0.6914 (7)	−0.0124 (7)	0.4019 (5)	0.0649 (17)
H2	0.6586	−0.1055	0.4053	0.078*
C3	0.6101 (6)	0.0701 (5)	0.3673 (4)	0.0417 (11)
C4	0.4582 (6)	0.0295 (5)	0.3302 (4)	0.0406 (11)
C5	0.3759 (6)	−0.0963 (6)	0.3282 (5)	0.0536 (14)
H5	0.4097	−0.1719	0.3476	0.064*
C6	0.2493 (6)	0.0720 (5)	0.2691 (4)	0.0433 (12)
C7	0.6410 (8)	0.1928 (7)	0.0868 (5)	0.0664 (17)
C8	0.4800 (9)	0.2367 (9)	−0.0394 (5)	0.082 (2)
H8	0.4276	0.2442	−0.0961	0.099*
C9	0.4521 (7)	0.2994 (6)	0.0586 (4)	0.0565 (15)
C10	0.3355 (7)	0.3902 (6)	0.0933 (4)	0.0528 (14)
C11	0.2503 (10)	0.4381 (8)	0.0331 (5)	0.084 (2)
H11	0.2573	0.4198	−0.0375	0.100*
C12	0.2007 (6)	0.5091 (6)	0.2119 (4)	0.0479 (13)
O1W	0.8919 (7)	0.9099 (6)	0.1556 (7)	0.143 (3)
H1A	0.8768	0.8420	0.1848	0.172*
H1B	0.9025	0.8687	0.0946	0.172*
O2WA	0.952 (12)	0.968 (9)	−0.012 (7)	0.46 (3)	0.50
H2C	0.8712	0.9381	−0.0459	0.553*	0.50
H2D	1.0193	0.9627	−0.0553	0.553*	0.50
O2WB	1.007 (6)	0.784 (5)	−0.045 (3)	0.46 (3)	0.50
H2E	0.9815	0.6950	−0.0507	0.553*	0.50
H2F	1.0980	0.7961	−0.0538	0.553*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb	0.03230 (12)	0.03302 (12)	0.04414 (12)	0.00269 (8)	0.00326 (8)	0.01255 (8)
S1	0.0507 (9)	0.0742 (11)	0.0805 (11)	0.0126 (8)	−0.0077 (8)	0.0450 (9)
S2	0.0488 (8)	0.0411 (7)	0.0670 (9)	−0.0075 (6)	0.0027 (7)	0.0187 (7)
S3	0.1077 (16)	0.1029 (15)	0.0530 (10)	0.0293 (13)	0.0292 (10)	0.0096 (10)
S4	0.1085 (16)	0.0875 (13)	0.0631 (11)	0.0429 (12)	−0.0244 (10)	0.0174 (9)
N1	0.038 (2)	0.045 (2)	0.060 (3)	0.010 (2)	0.002 (2)	0.021 (2)
N2	0.035 (3)	0.062 (3)	0.109 (5)	−0.001 (2)	−0.009 (3)	0.041 (3)
N3	0.038 (2)	0.036 (2)	0.045 (2)	0.0012 (18)	0.0018 (18)	0.0118 (18)
N4	0.047 (3)	0.051 (3)	0.091 (4)	−0.007 (2)	−0.019 (3)	0.033 (3)
N5	0.063 (3)	0.055 (3)	0.047 (3)	0.016 (2)	0.013 (2)	0.018 (2)
N6	0.114 (6)	0.131 (6)	0.068 (4)	0.079 (5)	0.023 (4)	0.017 (4)
N7	0.044 (3)	0.049 (3)	0.047 (3)	0.004 (2)	−0.002 (2)	0.022 (2)
N8	0.047 (3)	0.071 (3)	0.061 (3)	0.018 (2)	0.005 (2)	0.028 (3)
N9	0.035 (2)	0.052 (3)	0.038 (2)	0.001 (2)	0.0006 (18)	0.014 (2)
N10	0.047 (3)	0.053 (3)	0.053 (3)	0.005 (2)	0.005 (2)	0.020 (2)
O1	0.047 (2)	0.061 (3)	0.104 (4)	0.005 (2)	0.003 (2)	0.047 (3)
O2	0.050 (3)	0.075 (3)	0.076 (3)	0.013 (2)	−0.006 (2)	0.034 (2)
O3	0.054 (3)	0.075 (3)	0.113 (4)	−0.003 (2)	0.013 (3)	0.055 (3)
O4	0.069 (3)	0.078 (3)	0.112 (4)	0.033 (3)	0.034 (3)	0.064 (3)
O5	0.047 (2)	0.066 (3)	0.057 (2)	0.0002 (19)	−0.0071 (19)	0.012 (2)
O6	0.050 (3)	0.100 (4)	0.098 (4)	−0.015 (3)	−0.006 (2)	0.052 (3)
C1	0.039 (3)	0.055 (3)	0.053 (3)	0.011 (3)	0.004 (2)	0.024 (3)
C2	0.057 (4)	0.057 (4)	0.093 (5)	0.003 (3)	−0.007 (3)	0.042 (3)
C3	0.043 (3)	0.042 (3)	0.044 (3)	0.006 (2)	0.005 (2)	0.017 (2)
C4	0.041 (3)	0.037 (3)	0.045 (3)	0.006 (2)	0.008 (2)	0.013 (2)
C5	0.051 (3)	0.041 (3)	0.074 (4)	0.003 (3)	0.001 (3)	0.026 (3)
C6	0.046 (3)	0.038 (3)	0.042 (3)	−0.002 (2)	0.002 (2)	0.008 (2)
C7	0.075 (5)	0.069 (4)	0.055 (4)	0.022 (4)	0.014 (3)	0.012 (3)
C8	0.092 (6)	0.101 (6)	0.050 (4)	0.014 (5)	0.003 (4)	0.013 (4)
C9	0.068 (4)	0.055 (3)	0.046 (3)	−0.001 (3)	0.006 (3)	0.016 (3)
C10	0.068 (4)	0.045 (3)	0.045 (3)	0.006 (3)	−0.001 (3)	0.011 (2)
C11	0.123 (7)	0.090 (5)	0.044 (3)	0.032 (5)	−0.010 (4)	0.021 (3)
C12	0.048 (3)	0.042 (3)	0.055 (3)	−0.002 (3)	−0.010 (3)	0.020 (3)
O1W	0.117 (5)	0.087 (4)	0.240 (9)	−0.022 (4)	−0.075 (6)	0.087 (5)
O2WA	0.66 (8)	0.50 (7)	0.31 (4)	0.30 (6)	0.16 (4)	0.17 (4)
O2WB	0.66 (8)	0.50 (7)	0.31 (4)	0.30 (6)	0.16 (4)	0.17 (4)

Geometric parameters (Å, º) top

Pb—N1	2.656 (4)	N7—C12	1.311 (7)
Pb—N3	2.563 (4)	N7—C10	1.375 (7)
Pb—N5	2.535 (5)	N8—C12	1.354 (7)
Pb—N7	2.692 (4)	N8—H8A	0.8999
Pb—O1	2.704 (4)	N8—H8B	0.8393
Pb—O4	2.803 (5)	N9—O4	1.210 (6)
S1—C2	1.717 (7)	N9—O6	1.227 (6)
S1—C1	1.726 (5)	N9—O5	1.252 (5)
S2—C5	1.714 (6)	N10—O3	1.233 (6)
S2—C6	1.728 (5)	N10—O2	1.242 (6)
S3—C8	1.709 (8)	N10—O1	1.262 (6)
S3—C7	1.726 (7)	C2—C3	1.330 (7)
S4—C11	1.710 (8)	C2—H2	0.9300
S4—C12	1.720 (5)	C3—C4	1.458 (7)
N1—C1	1.319 (7)	C4—C5	1.349 (7)
N1—C3	1.395 (6)	C5—H5	0.9300
N2—C1	1.345 (7)	C8—C9	1.344 (9)
N2—H2A	0.9230	C8—H8	0.9300
N2—H2B	0.9039	C9—C10	1.474 (8)
N3—C6	1.313 (6)	C10—C11	1.338 (9)
N3—C4	1.390 (6)	C11—H11	0.9300
N4—C6	1.355 (7)	O1W—H1A	0.8534
N4—H4A	0.9949	O1W—H1B	0.8279
N4—H4B	0.8762	O2WA—O2WAⁱ	1.0 (2)
N5—C7	1.313 (8)	O2WA—H2C	0.8498
N5—C9	1.391 (8)	O2WA—H2D	0.8500
N6—C7	1.323 (9)	O2WB—H2E	0.8502
N6—H6A	0.9337	O2WB—H2F	0.8500
N6—H6B	0.9558

N5—Pb—N3	78.40 (14)	O3—N10—O1	119.2 (5)
N5—Pb—N1	90.14 (15)	O2—N10—O1	118.7 (5)
N3—Pb—N1	65.73 (13)	N10—O1—Pb	105.8 (3)
N5—Pb—N7	64.98 (15)	N1—C1—N2	124.6 (5)
N3—Pb—N7	89.39 (13)	N1—C1—S1	114.4 (4)
N1—Pb—N7	148.47 (14)	N2—C1—S1	121.0 (4)
N5—Pb—O1	75.24 (16)	C3—C2—S1	111.4 (5)
N3—Pb—O1	132.73 (13)	C3—C2—H2	124.3
N1—Pb—O1	75.77 (13)	S1—C2—H2	124.3
N7—Pb—O1	113.10 (13)	C2—C3—N1	115.0 (5)
C2—S1—C1	89.0 (3)	C2—C3—C4	125.6 (5)
C5—S2—C6	89.2 (3)	N1—C3—C4	119.4 (4)
C8—S3—C7	89.4 (3)	C5—C4—N3	114.7 (5)
C11—S4—C12	88.7 (3)	C5—C4—C3	125.5 (5)
C1—N1—C3	110.2 (4)	N3—C4—C3	119.7 (4)
C1—N1—Pb	133.5 (4)	C4—C5—S2	111.0 (4)
C3—N1—Pb	115.4 (3)	C4—C5—H5	124.5
C1—N2—H2A	127.5	S2—C5—H5	124.5
C1—N2—H2B	123.9	N3—C6—N4	125.3 (5)
H2A—N2—H2B	102.7	N3—C6—S2	114.5 (4)
C6—N3—C4	110.5 (4)	N4—C6—S2	120.2 (4)
C6—N3—Pb	130.0 (3)	N5—C7—N6	124.9 (6)
C4—N3—Pb	118.7 (3)	N5—C7—S3	114.5 (5)
C6—N4—H4A	115.8	N6—C7—S3	120.6 (5)
C6—N4—H4B	109.5	C9—C8—S3	110.7 (6)
H4A—N4—H4B	120.6	C9—C8—H8	124.7
C7—N5—C9	110.0 (5)	S3—C8—H8	124.7
C7—N5—Pb	129.2 (4)	C8—C9—N5	115.4 (6)
C9—N5—Pb	120.7 (4)	C8—C9—C10	126.0 (6)
C7—N6—H6A	114.4	N5—C9—C10	118.7 (5)
C7—N6—H6B	131.4	C11—C10—N7	115.5 (6)
H6A—N6—H6B	100.3	C11—C10—C9	125.7 (6)
C12—N7—C10	109.9 (5)	N7—C10—C9	118.8 (5)
C12—N7—Pb	132.8 (4)	C10—C11—S4	110.9 (5)
C10—N7—Pb	115.3 (3)	C10—C11—H11	124.5
C12—N8—H8A	112.9	S4—C11—H11	124.5
C12—N8—H8B	120.1	N7—C12—N8	124.8 (5)
H8A—N8—H8B	121.3	N7—C12—S4	115.0 (4)
O4—N9—O6	119.0 (5)	N8—C12—S4	120.3 (4)
O4—N9—O5	120.7 (5)	H1A—O1W—H1B	105.1
O6—N9—O5	120.1 (5)	H2C—O2WA—H2D	107.7
O3—N10—O2	122.1 (5)	H2E—O2WB—H2F	107.7

Symmetry code: (i) −x+2, −y+2, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O1	0.92	2.08	2.884 (8)	145
N2—H2B···O4ⁱⁱ	0.90	2.33	3.209 (7)	165
N2—H2B···O6ⁱⁱ	0.90	2.31	3.057 (7)	140
N4—H4A···N7	0.99	2.19	3.168 (7)	166
N4—H4B···O1Wⁱⁱⁱ	0.88	2.29	3.015 (8)	141
N4—H4B···O2WA^iv	0.88	2.26	2.98 (9)	140
N6—H6A···N1	0.93	2.22	3.119 (8)	160
N6—H6B···O2WA^v	0.96	2.29	3.12 (10)	145
N6—H6B···O1W^v	0.96	2.10	2.929 (10)	144
N8—H8A···O3^vi	0.90	2.17	3.027 (7)	159
N8—H8B···O4	0.84	2.13	2.916 (7)	156
O1W—H1A···O3	0.85	1.94	2.782 (8)	168
O1W—H1B···O2WA	0.83	1.97	2.54 (9)	125
O1W—H1B···O2WB	0.83	2.14	2.93 (4)	160
O2WA—H2C···N4^iv	0.85	2.42	2.98 (9)	124
O2WA—H2D···O1Wⁱ	0.85	2.17	2.85 (9)	136
O2WB—H2E···S4^iv	0.85	2.27	3.09 (5)	164
O2WB—H2F···S3^vii	0.85	2.80	3.53 (5)	144
O2WB—H2F···N6^vii	0.85	1.91	2.67 (5)	148

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

Experimental details

Crystal data
Chemical formula	[Pb(NO₃)₂(C₆H₆N₄S₂)₂]·2H₂O
M_r	1527.66
Crystal system, space group	Triclinic, P1
Temperature (K)	294
a, b, c (Å)	9.2387 (8), 9.6962 (9), 13.5636 (6)
α, β, γ (°)	105.731 (4), 90.377 (3), 97.072 (5)
V (Å³)	1159.61 (16)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	7.70
Crystal size (mm)	0.21 × 0.16 × 0.14

Data collection
Diffractometer	Rigaku R-AXIS RAPID IP diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.215, 0.340
No. of measured, independent and observed [I > 2σ(I)] reflections	6095, 4012, 3705
R_int	0.015
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.065, 1.08
No. of reflections	4012
No. of parameters	319
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.83, −0.46

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), and Nardelli (1999), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top

Pb—N1	2.656 (4)	Pb—N7	2.692 (4)
Pb—N3	2.563 (4)	Pb—O1	2.704 (4)
Pb—N5	2.535 (5)	Pb—O4	2.803 (5)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O1	0.92	2.08	2.884 (8)	145
N2—H2B···O4ⁱ	0.90	2.33	3.209 (7)	165
N2—H2B···O6ⁱ	0.90	2.31	3.057 (7)	140
N4—H4A···N7	0.99	2.19	3.168 (7)	166
N4—H4B···O1Wⁱⁱ	0.88	2.29	3.015 (8)	141
N4—H4B···O2WAⁱⁱⁱ	0.88	2.26	2.98 (9)	140
N6—H6A···N1	0.93	2.22	3.119 (8)	160
N6—H6B···O2WA^iv	0.96	2.29	3.12 (10)	145
N6—H6B···O1W^iv	0.96	2.10	2.929 (10)	144
N8—H8A···O3^v	0.90	2.17	3.027 (7)	159
N8—H8B···O4	0.84	2.13	2.916 (7)	156
O1W—H1A···O3	0.85	1.94	2.782 (8)	168
O1W—H1B···O2WA	0.83	1.97	2.54 (9)	125
O1W—H1B···O2WB	0.83	2.14	2.93 (4)	160
O2WA—H2C···N4ⁱⁱⁱ	0.85	2.42	2.98 (9)	124
O2WA—H2D···O1W^vi	0.85	2.17	2.85 (9)	136
O2WB—H2E···S4ⁱⁱⁱ	0.85	2.27	3.09 (5)	164
O2WB—H2F···S3^vii	0.85	2.80	3.53 (5)	144
O2WB—H2F···N6^vii	0.85	1.91	2.67 (5)	148

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

Acknowledgements

The project was supported by the Educational Development Foundation of Shanghai Educational Committee, China (grant No. AB0448).

References

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