Bis(μ-imino­diacetato)bis­[(2,2′-diamino-4,4′-bi-1,3-thia­zole)lead(II)] tetra­hydrate

Du, M.; Liu, B.-X.; Nie, J.-J.; Xu, D.-J.

doi:10.1107/S1600536810006926

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 3| March 2010| Pages m343-m344

doi:10.1107/S1600536810006926

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Bis(μ-iminodiacetato)bis[(2,2′-diamino-4,4′-bi-1,3-thiazole)lead(II)] tetrahydrate

Mei Du,^a ^* Bing-Xin Liu,^a Jing-Jing Nie ^b and Duan-Jun Xu ^b

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

(Received 16 February 2010; accepted 23 February 2010; online 27 February 2010)

In the crystal structure of the title compound, [Pb₂(C₄H₅NO₄)₂(C₆H₆N₄S₂)₂]·4H₂O, the dinuclear Pb^II complex molecule is centrosymmetric. The Pb atom is chelated by a tridentate iminodiacetate anion (IDA) and a diaminobithiazole (DABT) ligand, while a carboxylate O atom from an adjacent IDA anion further bridges the Pb atom with a longer Pb—O bond [2.892 (3) Å]. The lone-pair electrons of the Pb atom occupy an axial site in the Ψ-pentagonal-bipyramidal coordination polyhedron. The IDA anion displays a facial configuration: its chelating five-membered rings assume an envelope configuration. Within the DABT ligand, the two thiazole rings are twisted relative to each other, making a dihedral angle of 9.51 (17)°. Extensive N—H⋯O, O—H⋯O and weak C—H⋯O hydrogen bonding helps to stabilize the crystal structure.

Related literature

For the potential applications of metal complexes of diaminobithiazole in the field of biology, see: Waring (1981 ); Fisher et al. (1985 ). For Pb^II complexes with a similar coordination geometry, see: Lacouture et al. (2001 ); Jones et al. (1988 ). For a complex with a longer Pb—O bond distance [2.968 (4) Å], see: Inoue et al. (1993 ). For the dihedral angles between thiazole rings in diaminobithiazole complexes, see: Liu et al. (2006 ); Zhang et al. (2006 ).

Experimental

Crystal data

[Pb₂(C₄H₅NO₄)₂(C₆H₆N₄S₂)₂]·4H₂O
M_r = 1145.16
Triclinic, $[P \overline 1]$
a = 9.2241 (8) Å
b = 9.8526 (9) Å
c = 10.6380 (11) Å
α = 77.0732 (12)°
β = 67.4141 (15)°
γ = 69.0690 (12)°
V = 829.54 (14) Å³
Z = 1
Mo Kα radiation
μ = 10.46 mm⁻¹
T = 295 K
0.20 × 0.12 × 0.10 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.132, T_max = 0.350
5960 measured reflections
2878 independent reflections
2745 reflections with I > 2σ(I)
R_int = 0.021

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.048
S = 1.07
2878 reflections
244 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.54 e Å⁻³
Δρ_min = −0.70 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb—O1	2.546 (3)
Pb—O1ⁱ	2.892 (3)
Pb—O3	2.536 (3)
Pb—N1	2.593 (3)
Pb—N3	2.594 (3)
Pb—N5	2.402 (4)
Symmetry code: (i) -x+1, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯O3	0.86 (6)	2.05 (5)	2.880 (6)	162 (5)
N2—H2B⋯O1W	0.86 (3)	2.16 (4)	2.959 (6)	153 (6)
N4—H4A⋯O1	0.86 (5)	2.15 (5)	2.946 (5)	155 (5)
N4—H4B⋯O4ⁱⁱ	0.86 (3)	2.07 (5)	2.885 (7)	159 (6)
N5—H5N⋯O2W	0.87 (5)	2.01 (6)	2.809 (7)	153 (4)
O1W—H11⋯O2ⁱⁱⁱ	0.82 (2)	1.97 (2)	2.783 (6)	171 (5)
O1W—H12⋯O3^iv	0.82 (5)	2.11 (4)	2.819 (6)	144 (5)
O2W—H21⋯O1W^v	0.82 (7)	2.10 (7)	2.892 (7)	161 (6)
O2W—H22⋯O4^vi	0.82 (5)	1.95 (5)	2.766 (6)	168 (7)
C5—H5⋯O2^vii	0.93	2.56	3.476 (6)	167
Symmetry codes: (ii) x, y, z+1; (iii) x, y+1, z-1; (iv) -x+1, -y+2, -z; (v) -x+2, -y+2, -z; (vi) -x+2, -y+1, -z; (vii) x, 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/S1600536810006926/ng2733sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810006926/ng2733Isup2.hkl

checkCIF report

Comment top

Some metal complexes with 2,2'-diamino-4,4'-bi-1,3-thiazole (DABT) have shown the potential application in the biological field (Waring, 1981; Fisher et al., 1985). As a part of serial structural investigation of metal complexes with DABT, the title Pb^II complex was prepared in the laboratory and its X-ray structure is presented here.

The molecular structure of the title compound is shown in Fig. 1. The dinuclear Pb^II complex molecule is centro-symmetric. Each Pb atom is chelated by a tridentate iminodiacetate anion (IDA) and a diaminobithiazole (DABT) ligand, and one carboxyl O atom from the adjacent IDA anion further bridges the Pb atom. The lone-pair electrons of the Pb atom occupy an axial site in the distorted Ψ-pentagonal bipyramidal coordination geometry, which is similar to that found in Pb^II complexes reported previously (Lacouture et al., 2001; Jones et al., 1988). The longer Pb—O(bridge) bond distance (Table 1) is comparable to 2.968 (4) Å found in a related Pb complex (Inoue et al., 1993). The IDA displays a facial configuration, its both chelating five-membered rings assume the envelope configuration. Within the DABT ligand, the two thiazole rings are twisted to each other with a dihedral angle of 9.51 (17)°, it agrees with 14.7 (3) and 9.5 (2)° found in transition metal complexes of DABT (Liu et al., 2006; Zhang et al., 2006).

The extensive N—H···O, O—H···O and weak C—H···O hydrogen bonding helps to stabilize the crystal structure (Table 2).

Related literature top

For the potential applications of metal complexes of diaminobithiazole in the field of biology, see: Waring (1981); Fisher et al. (1985). For Pb^II complexes with a similar coordination geometry, see: Lacouture et al. (2001); Jones et al. (1988). For a complex with a longer Pb—O bond distance [2.968 (4) Å], see: Inoue et al. (1993). For the dihedral angles between thiazole rings in diaminobithiazole complexes, see: Liu et al. (2006); Zhang et al. (2006).

Experimental top

An aqueous solution (20 ml) containing DABT (0.20 g, 1 mmol) and Pb(NO₃)₂ (0.33 g, 1 mmol) was mixed with another aqueous solution (10 ml) of H₂IDA (0.13 g, 1 mmol) and NaOH (0.08 g, 2 mmol). The mixture was refluxed for 5 h. The solution was filtered after cooling to room temperature. Single crystals were obtained from the filtrate after one week.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); 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).

Figures top

Fig. 1. The dinuclear molecular structure with 30% probability displacement ellipsoids. Dashed lines indicate the hydrogen bonding [symmetric code: (i) -x,-y,1-z].

Bis(µ-iminodiacetato)bis[(2,2'-diamino-4,4'-bi-1,3-thiazole)lead(II)] tetrahydrate top

Crystal data top

[Pb₂(C₄H₅NO₄)₂(C₆H₆N₄S₂)₂]·4H₂O	Z = 1
M_r = 1145.16	F(000) = 544
Triclinic, P1	D_x = 2.292 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.2241 (8) Å	Cell parameters from 4336 reflections
b = 9.8526 (9) Å	θ = 2.1–24.6°
c = 10.6380 (11) Å	µ = 10.46 mm⁻¹
α = 77.0732 (12)°	T = 295 K
β = 67.4141 (15)°	Block, yellow
γ = 69.0690 (12)°	0.20 × 0.12 × 0.10 mm
V = 829.54 (14) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	2878 independent reflections
Radiation source: fine-focus sealed tube	2745 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
Detector resolution: 10.00 pixels mm^-1	θ_max = 25.0°, θ_min = 2.1°
ω scans	h = −10→10
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −11→11
T_min = 0.132, T_max = 0.350	l = −12→12
5960 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)] = 0.020	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ²(F_o²) + (0.019P)² + 0.7917P] where P = (F_o² + 2F_c²)/3
2878 reflections	(Δ/σ)_max = 0.001
244 parameters	Δρ_max = 0.54 e Å⁻³
9 restraints	Δρ_min = −0.70 e Å⁻³

Crystal data top

[Pb₂(C₄H₅NO₄)₂(C₆H₆N₄S₂)₂]·4H₂O	γ = 69.0690 (12)°
M_r = 1145.16	V = 829.54 (14) Å³
Triclinic, P1	Z = 1
a = 9.2241 (8) Å	Mo Kα radiation
b = 9.8526 (9) Å	µ = 10.46 mm⁻¹
c = 10.6380 (11) Å	T = 295 K
α = 77.0732 (12)°	0.20 × 0.12 × 0.10 mm
β = 67.4141 (15)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	2878 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2745 reflections with I > 2σ(I)
T_min = 0.132, T_max = 0.350	R_int = 0.021
5960 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	9 restraints
wR(F²) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	Δρ_max = 0.54 e Å⁻³
2878 reflections	Δρ_min = −0.70 e Å⁻³
244 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Pb	0.545731 (18)	0.724630 (15)	0.424338 (14)	0.02919 (7)
S1	0.85653 (18)	1.10157 (14)	0.16319 (14)	0.0551 (3)
S2	0.70556 (17)	0.84111 (15)	0.78711 (13)	0.0513 (3)
O1	0.6288 (4)	0.4760 (3)	0.5554 (3)	0.0400 (7)
O2	0.8401 (5)	0.2774 (4)	0.5652 (4)	0.0696 (11)
O3	0.5809 (4)	0.7154 (3)	0.1777 (3)	0.0431 (7)
O4	0.6770 (6)	0.5550 (4)	0.0268 (4)	0.0714 (12)
O1W	0.7380 (5)	1.1758 (4)	−0.1588 (4)	0.0577 (9)
O2W	1.0741 (5)	0.6671 (5)	0.1186 (5)	0.0717 (11)
N1	0.7119 (4)	0.9098 (4)	0.3108 (4)	0.0359 (8)
N2	0.7160 (6)	0.9566 (5)	0.0832 (4)	0.0541 (11)
N3	0.6755 (4)	0.7770 (4)	0.5787 (3)	0.0357 (8)
N4	0.5919 (6)	0.6270 (5)	0.7807 (4)	0.0563 (11)
N5	0.8084 (4)	0.5688 (4)	0.2998 (4)	0.0355 (8)
C1	0.7507 (5)	0.9781 (5)	0.1862 (4)	0.0382 (10)
C2	0.8435 (6)	1.0598 (5)	0.3335 (5)	0.0494 (12)
H2	0.8841	1.1027	0.3770	0.059*
C3	0.7666 (5)	0.9569 (5)	0.3947 (4)	0.0372 (10)
C4	0.6525 (6)	0.7362 (5)	0.7099 (4)	0.0399 (10)
C5	0.7564 (6)	0.9461 (5)	0.6339 (5)	0.0461 (11)
H5	0.7934	1.0262	0.6206	0.055*
C6	0.7354 (5)	0.8967 (4)	0.5350 (5)	0.0368 (10)
C11	0.7810 (6)	0.4004 (5)	0.5131 (4)	0.0370 (10)
C12	0.8948 (6)	0.4667 (5)	0.3912 (5)	0.0418 (10)
H12A	0.9443	0.5183	0.4229	0.050*
H12B	0.9827	0.3892	0.3400	0.050*
C13	0.7855 (6)	0.4939 (5)	0.2072 (4)	0.0408 (10)
H13A	0.7393	0.4162	0.2599	0.049*
H13B	0.8919	0.4499	0.1420	0.049*
C14	0.6733 (6)	0.5959 (5)	0.1303 (4)	0.0427 (11)
H11	0.768 (8)	1.197 (7)	−0.2418 (10)	0.080*
H12	0.6393 (18)	1.220 (6)	−0.132 (6)	0.080*
H21	1.124 (7)	0.724 (5)	0.113 (7)	0.080*
H22	1.147 (6)	0.594 (4)	0.086 (7)	0.080*
H2A	0.662 (6)	0.895 (5)	0.101 (6)	0.080*
H2B	0.751 (8)	0.997 (6)	0.001 (2)	0.080*
H4A	0.582 (7)	0.570 (5)	0.736 (5)	0.080*
H4B	0.595 (7)	0.598 (6)	0.862 (2)	0.080*
H5N	0.865 (6)	0.626 (5)	0.247 (5)	0.080*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb	0.03072 (10)	0.03010 (10)	0.02682 (10)	−0.00792 (7)	−0.01080 (7)	−0.00292 (6)
S1	0.0619 (9)	0.0475 (7)	0.0531 (7)	−0.0305 (6)	−0.0092 (6)	0.0054 (6)
S2	0.0594 (8)	0.0592 (8)	0.0430 (7)	−0.0105 (6)	−0.0248 (6)	−0.0183 (6)
O1	0.0430 (19)	0.0399 (17)	0.0384 (17)	−0.0150 (15)	−0.0159 (14)	0.0016 (13)
O2	0.070 (3)	0.051 (2)	0.064 (2)	−0.0008 (19)	−0.025 (2)	0.0136 (19)
O3	0.051 (2)	0.0448 (18)	0.0352 (16)	−0.0102 (15)	−0.0218 (15)	−0.0005 (14)
O4	0.110 (3)	0.068 (2)	0.049 (2)	−0.016 (2)	−0.046 (2)	−0.0134 (19)
O1W	0.063 (2)	0.059 (2)	0.054 (2)	−0.0169 (19)	−0.030 (2)	0.0050 (19)
O2W	0.062 (3)	0.076 (3)	0.074 (3)	−0.035 (2)	−0.002 (2)	−0.013 (2)
N1	0.040 (2)	0.0315 (18)	0.0362 (19)	−0.0136 (16)	−0.0107 (16)	−0.0017 (15)
N2	0.068 (3)	0.058 (3)	0.039 (2)	−0.030 (2)	−0.019 (2)	0.010 (2)
N3	0.038 (2)	0.041 (2)	0.0309 (18)	−0.0143 (16)	−0.0126 (16)	−0.0041 (15)
N4	0.081 (3)	0.066 (3)	0.032 (2)	−0.033 (3)	−0.026 (2)	0.007 (2)
N5	0.034 (2)	0.039 (2)	0.035 (2)	−0.0125 (16)	−0.0138 (16)	−0.0001 (16)
C1	0.038 (2)	0.033 (2)	0.037 (2)	−0.0107 (19)	−0.0072 (19)	−0.0009 (18)
C2	0.050 (3)	0.046 (3)	0.058 (3)	−0.024 (2)	−0.013 (2)	−0.010 (2)
C3	0.034 (2)	0.035 (2)	0.040 (2)	−0.0065 (19)	−0.0086 (19)	−0.0115 (19)
C4	0.043 (3)	0.047 (3)	0.032 (2)	−0.008 (2)	−0.015 (2)	−0.010 (2)
C5	0.052 (3)	0.044 (3)	0.051 (3)	−0.012 (2)	−0.024 (2)	−0.014 (2)
C6	0.033 (2)	0.034 (2)	0.045 (2)	−0.0053 (18)	−0.015 (2)	−0.0113 (19)
C11	0.043 (3)	0.038 (2)	0.034 (2)	−0.008 (2)	−0.021 (2)	−0.0024 (19)
C12	0.038 (3)	0.048 (3)	0.042 (2)	−0.012 (2)	−0.021 (2)	0.001 (2)
C13	0.049 (3)	0.040 (2)	0.036 (2)	−0.009 (2)	−0.019 (2)	−0.0080 (19)
C14	0.054 (3)	0.045 (3)	0.032 (2)	−0.020 (2)	−0.014 (2)	0.000 (2)

Geometric parameters (Å, º) top

Pb—O1	2.546 (3)	N2—H2A	0.86 (6)
Pb—O1ⁱ	2.892 (3)	N2—H2B	0.86 (3)
Pb—O3	2.536 (3)	N3—C4	1.318 (5)
Pb—N1	2.593 (3)	N3—C6	1.391 (5)
Pb—N3	2.594 (3)	N4—C4	1.335 (6)
Pb—N5	2.402 (4)	N4—H4A	0.86 (5)
S1—C2	1.732 (5)	N4—H4B	0.86 (3)
S1—C1	1.739 (4)	N5—C13	1.468 (5)
S2—C5	1.718 (5)	N5—C12	1.475 (5)
S2—C4	1.741 (4)	N5—H5N	0.86 (5)
O1—C11	1.283 (5)	C2—C3	1.348 (6)
O2—C11	1.237 (5)	C2—H2	0.9300
O3—C14	1.259 (5)	C3—C6	1.435 (6)
O4—C14	1.239 (5)	C5—C6	1.354 (6)
O1W—H11	0.819 (16)	C5—H5	0.9300
O1W—H12	0.82 (5)	C11—C12	1.509 (6)
O2W—H21	0.82 (7)	C12—H12A	0.9700
O2W—H22	0.82 (5)	C12—H12B	0.9700
N1—C1	1.321 (5)	C13—C14	1.513 (6)
N1—C3	1.403 (5)	C13—H13A	0.9700
N2—C1	1.331 (6)	C13—H13B	0.9700

N5—Pb—O3	66.12 (11)	N1—C1—S1	114.6 (3)
N5—Pb—O1	67.04 (11)	N2—C1—S1	120.7 (3)
O3—Pb—O1	114.56 (10)	C3—C2—S1	110.9 (4)
N5—Pb—N1	78.68 (11)	C3—C2—H2	124.5
O3—Pb—N1	81.95 (10)	S1—C2—H2	124.5
O1—Pb—N1	128.64 (10)	C2—C3—N1	115.0 (4)
N5—Pb—N3	90.68 (12)	C2—C3—C6	125.7 (4)
O3—Pb—N3	143.48 (11)	N1—C3—C6	119.3 (4)
O1—Pb—N3	77.56 (10)	N3—C4—N4	124.6 (4)
N1—Pb—N3	65.44 (11)	N3—C4—S2	113.7 (3)
C2—S1—C1	89.0 (2)	N4—C4—S2	121.7 (3)
C5—S2—C4	89.4 (2)	C6—C5—S2	111.0 (4)
C11—O1—Pb	116.9 (3)	C6—C5—H5	124.5
C14—O3—Pb	114.4 (3)	S2—C5—H5	124.5
H11—O1W—H12	105 (6)	C5—C6—N3	114.7 (4)
H21—O2W—H22	104 (6)	C5—C6—C3	126.4 (4)
C1—N1—C3	110.4 (4)	N3—C6—C3	119.0 (4)
C1—N1—Pb	132.4 (3)	O2—C11—O1	124.6 (4)
C3—N1—Pb	117.1 (3)	O2—C11—C12	118.1 (4)
C1—N2—H2A	116 (4)	O1—C11—C12	117.3 (4)
C1—N2—H2B	122 (4)	N5—C12—C11	112.3 (4)
H2A—N2—H2B	121 (6)	N5—C12—H12A	109.1
C4—N3—C6	111.2 (4)	C11—C12—H12A	109.1
C4—N3—Pb	128.8 (3)	N5—C12—H12B	109.1
C6—N3—Pb	116.8 (3)	C11—C12—H12B	109.1
C4—N4—H4A	118 (4)	H12A—C12—H12B	107.9
C4—N4—H4B	119 (4)	N5—C13—C14	112.6 (4)
H4A—N4—H4B	119 (6)	N5—C13—H13A	109.1
C13—N5—C12	112.7 (3)	C14—C13—H13A	109.1
C13—N5—Pb	109.0 (3)	N5—C13—H13B	109.1
C12—N5—Pb	112.3 (3)	C14—C13—H13B	109.1
C13—N5—H5N	105 (4)	H13A—C13—H13B	107.8
C12—N5—H5N	111 (4)	O4—C14—O3	124.8 (5)
Pb—N5—H5N	106 (4)	O4—C14—C13	117.8 (4)
N1—C1—N2	124.7 (4)	O3—C14—C13	117.4 (4)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O3	0.86 (6)	2.05 (5)	2.880 (6)	162 (5)
N2—H2B···O1W	0.86 (3)	2.16 (4)	2.959 (6)	153 (6)
N4—H4A···O1	0.86 (5)	2.15 (5)	2.946 (5)	155 (5)
N4—H4B···O4ⁱⁱ	0.86 (3)	2.07 (5)	2.885 (7)	159 (6)
N5—H5N···O2W	0.87 (5)	2.01 (6)	2.809 (7)	153 (4)
O1W—H11···O2ⁱⁱⁱ	0.82 (2)	1.97 (2)	2.783 (6)	171 (5)
O1W—H12···O3^iv	0.82 (5)	2.11 (4)	2.819 (6)	144 (5)
O2W—H21···O1W^v	0.82 (7)	2.10 (7)	2.892 (7)	161 (6)
O2W—H22···O4^vi	0.82 (5)	1.95 (5)	2.766 (6)	168 (7)
C5—H5···O2^vii	0.93	2.56	3.476 (6)	167

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

Experimental details

Crystal data
Chemical formula	[Pb₂(C₄H₅NO₄)₂(C₆H₆N₄S₂)₂]·4H₂O
M_r	1145.16
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	9.2241 (8), 9.8526 (9), 10.6380 (11)
α, β, γ (°)	77.0732 (12), 67.4141 (15), 69.0690 (12)
V (Å³)	829.54 (14)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	10.46
Crystal size (mm)	0.20 × 0.12 × 0.10

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.132, 0.350
No. of measured, independent and observed [I > 2σ(I)] reflections	5960, 2878, 2745
R_int	0.021
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.048, 1.07
No. of reflections	2878
No. of parameters	244
No. of restraints	9
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.54, −0.70

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

Selected bond lengths (Å) top

Pb—O1	2.546 (3)	Pb—N1	2.593 (3)
Pb—O1ⁱ	2.892 (3)	Pb—N3	2.594 (3)
Pb—O3	2.536 (3)	Pb—N5	2.402 (4)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O3	0.86 (6)	2.05 (5)	2.880 (6)	162 (5)
N2—H2B···O1W	0.86 (3)	2.16 (4)	2.959 (6)	153 (6)
N4—H4A···O1	0.86 (5)	2.15 (5)	2.946 (5)	155 (5)
N4—H4B···O4ⁱⁱ	0.86 (3)	2.07 (5)	2.885 (7)	159 (6)
N5—H5N···O2W	0.87 (5)	2.01 (6)	2.809 (7)	153 (4)
O1W—H11···O2ⁱⁱⁱ	0.819 (16)	1.97 (2)	2.783 (6)	171 (5)
O1W—H12···O3^iv	0.82 (5)	2.11 (4)	2.819 (6)	144 (5)
O2W—H21···O1W^v	0.82 (7)	2.10 (7)	2.892 (7)	161 (6)
O2W—H22···O4^vi	0.82 (5)	1.95 (5)	2.766 (6)	168 (7)
C5—H5···O2^vii	0.93	2.56	3.476 (6)	167

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

Acknowledgements

The project was supported by the ZIJIN project of Zhejiang University, China.

References

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Volume 66| Part 3| March 2010| Pages m343-m344

doi:10.1107/S1600536810006926

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Bis(μ-imino­di­acetato)bis­­[(2,2′-di­amino-4,4′-bi-1,3-thia­zole)lead(II)] tetra­hydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Bis(μ-iminodiacetato)bis[(2,2′-diamino-4,4′-bi-1,3-thiazole)lead(II)] tetrahydrate