Dichlorido{μ-6,6′-dimeth­oxy-2,2′-[o-phenyl­enebis(nitrilo­methyl­idyne)]diphenolato}(dimethyl sulfoxide)lead(II)zinc(II) N,N-dimethyl­formamide solvate

Wang, H.; Zhang, D.; Tian, L.; Zhang, L.-F.

doi:10.1107/S1600536808034338

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 11| November 2008| Page m1460

doi:10.1107/S1600536808034338

Open

access

Dichlorido{μ-6,6′-dimethoxy-2,2′-[o-phenylenebis(nitrilomethylidyne)]diphenolato}(dimethyl sulfoxide)lead(II)zinc(II) N,N-dimethylformamide solvate

Hailong Wang,^a Daopeng Zhang,^a Laijin Tian ^a and Li-Fang Zhang ^a ^*

^aSchool of Chemistry & Chemical Technology, Shandong University, Jinan 250100, People's Republic of China
^*Correspondence e-mail: Zhanglf@sdu.edu.cn

(Received 8 October 2008; accepted 21 October 2008; online 25 October 2008)

In the heterodinuclear complex of the title compound, [PbZn(C₂₂H₁₈N₂O₄)Cl₂(C₂H₆OS)]·C₃H₇NO, the Zn^II atom is coordinated in a distorted square-pyramidal geometry by two N atoms and two O atoms from the diphenolate ligand, and one Cl atom which occupies the apical position. The Pb^II atom is coordinated in a distorted octahedral geometry by the four O atoms of the diphenolate ligand, one O atom from the dimethyl sulfoxide molecule and one Cl atom. The dimethyl sulfoxide molecule is disordered over two positions, with site occupancies of 0.576 (2) and 0.424 (2).

Related literature

For general background, see: Karlin (1993 ); Ni et al. (2005 ); Ward (2007 ). For a related structure, see: Korupoju et al. (2000 ). For related literature on the preparative method, see: Lo et al. (2004 ); Sui et al. (2007 ).

Experimental

Crystal data

[PbZn(C₂₂H₁₈N₂O₄)Cl₂(C₂H₆OS)]·C₃H₇NO
M_r = 869.07
Monoclinic, P 2₁ /c
a = 15.2850 (7) Å
b = 18.8433 (8) Å
c = 10.7343 (5) Å
β = 94.771 (1)°
V = 3081.0 (2) Å³
Z = 4
Mo Kα radiation
μ = 6.52 mm⁻¹
T = 295 (2) K
0.2 × 0.15 × 0.1 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.343, T_max = 0.518
18055 measured reflections
6997 independent reflections
4923 reflections with I > 2σ(I)
R_int = 0.039

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.073
S = 0.99
6997 reflections
387 parameters
28 restraints
H-atom parameters constrained
Δρ_max = 0.75 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Table 1
Selected bond lengths (Å)

Zn1—N1	2.070 (4)
Zn1—N2	2.077 (3)
Zn1—O3	2.028 (3)
Zn1—O2	2.014 (3)
Zn1—Cl2	2.2686 (14)
Pb1—O1	2.791 (4)
Pb1—O2	2.476 (3)
Pb1—O3	2.420 (3)
Pb1—O4	2.667 (3)
Pb1—O5	2.741 (5)
Pb1—O5′	2.746 (7)
Pb1—Cl1	2.6088 (15)

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808034338/is2345sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808034338/is2345Isup2.hkl

checkCIF report

Comment top

Heterometallic dinuclear complexes have been intensively studied owing to their unique physical and chemical properties (Ward, 2007; Ni et al., 2005). In addition, these compounds exist at the active sites of many metalloenzymes and play important roles in biological systems (Karlin, 1993). Whereas, it is necessary to further widen the system of application of heterometallic compounds. Herein, a novel heterometallic binuclear Zn^IIPb^II compound has been obtained by step-by-step method and its structure is depicted.

As shown in Fig. 1, the title compound is a binuclear neutral complex with a slightly distorted planar configuration. Each Zn^II atom is coordinated in a square-pyramidal geometry with the basal square formed by two N atoms and two O atoms from the L ligand, and with the apical position occupied by terminal Cl atom. The coordination environment of each Pb^II atom is in a distorted octahedral geometry composed of four O atoms from the ligand, one Cl atom and one O atom of the DMSO molecule. The Zn^II atom and the Pb^II atom are connected via two bridging O atoms of the ligand. The bond lengths of Zn—O, Zn—N and Zn—Cl are normal (Korupoju et al., 2000).

Related literature top

For general background, see: Karlin (1993); Ni et al. (2005); Ward (2007). For a related structure, see: Korupoju et al. (2000). For related literature on the preparative method, see: Lo et al. (2004); Sui et al. (2007).

Experimental top

The H₂L ligand and the complex ZnL were synthesized according to the previous literatures (Lo et al., 2004; Sui et al., 2007). The title compound was obtained by allowing the mixture of ZnL (0.088 g, 0.2 mmol) and PbCl₂.2H₂O (0.063 g, 0.2 mmol) being refluxed in a DMF and DMSO (1:1) solution, cooled down to room temperature, then filtered. Yellow single crystals suitable for X-ray diffraction were obtained via slow evaporation of the filtrate at room temperature.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. A view of (I) with the unique atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level, all hydrogen atoms are omitted for clarity. Only one conpoment of the disordered DMSO molecule is shown.

Dichlorido-1κCl,2κCl-{µ-6,6'-dimethoxy-2,2'-[o- phenylenebis(nitrilomethylidyne)]diphenolato- 1κ⁴O¹,N,N',O^1':2κ⁴O,O',O'',O''}(dimethyl sulfoxide-2κO)lead(II)zinc(II) N,N-dimethylformamide solvate top

Crystal data top

[PbZn(C₂₂H₁₈N₂O₄)Cl₂(C₂H₆OS)]·C₃H₇NO	F(000) = 1696
M_r = 869.07	D_x = 1.874 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P2ybc	Cell parameters from 5739 reflections
a = 15.2850 (7) Å	θ = 1.7–27.5°
b = 18.8433 (8) Å	µ = 6.52 mm⁻¹
c = 10.7343 (5) Å	T = 295 K
β = 94.771 (1)°	Block, yellow
V = 3081.0 (2) Å³	0.2 × 0.15 × 0.1 mm
Z = 4

Data collection top

Bruker APEX CCD area-detector diffractometer	6997 independent reflections
Radiation source: fine-focus sealed tube	4923 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.039
ω scans	θ_max = 27.5°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −19→15
T_min = 0.343, T_max = 0.518	k = −23→24
18055 measured reflections	l = −13→12

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.073	H-atom parameters constrained
S = 0.99	w = 1/[σ²(F_o²) + (0.0296P)²] where P = (F_o² + 2F_c²)/3
6997 reflections	(Δ/σ)_max = 0.001
387 parameters	Δρ_max = 0.75 e Å⁻³
28 restraints	Δρ_min = −0.61 e Å⁻³

Crystal data top

[PbZn(C₂₂H₁₈N₂O₄)Cl₂(C₂H₆OS)]·C₃H₇NO	V = 3081.0 (2) Å³
M_r = 869.07	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 15.2850 (7) Å	µ = 6.52 mm⁻¹
b = 18.8433 (8) Å	T = 295 K
c = 10.7343 (5) Å	0.2 × 0.15 × 0.1 mm
β = 94.771 (1)°

Data collection top

Bruker APEX CCD area-detector diffractometer	6997 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	4923 reflections with I > 2σ(I)
T_min = 0.343, T_max = 0.518	R_int = 0.039
18055 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	28 restraints
wR(F²) = 0.073	H-atom parameters constrained
S = 0.99	Δρ_max = 0.75 e Å⁻³
6997 reflections	Δρ_min = −0.61 e Å⁻³
387 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)
C1	0.9922 (4)	0.5643 (3)	−0.2068 (8)	0.092 (2)
H1A	1.0047	0.6013	−0.1464	0.138*
H1B	0.9834	0.5848	−0.2888	0.138*
H1C	1.0406	0.5318	−0.2041	0.138*
C2	0.8849 (3)	0.4724 (3)	−0.2534 (5)	0.0464 (12)
C3	0.9128 (4)	0.4565 (3)	−0.3684 (5)	0.0594 (15)
H3	0.9561	0.4841	−0.4004	0.071*
C4	0.8775 (4)	0.4007 (3)	−0.4364 (5)	0.0615 (16)
H4	0.8966	0.3910	−0.5147	0.074*
C5	0.8147 (3)	0.3591 (3)	−0.3907 (5)	0.0535 (14)
H5	0.7913	0.3212	−0.4380	0.064*
C6	0.7850 (3)	0.3730 (2)	−0.2721 (4)	0.0384 (11)
C7	0.8183 (3)	0.4316 (2)	−0.2022 (4)	0.0396 (11)
C8	0.7195 (3)	0.3250 (2)	−0.2308 (4)	0.0387 (11)
H8	0.6966	0.2912	−0.2876	0.046*
C9	0.6238 (3)	0.2772 (2)	−0.0917 (4)	0.0340 (10)
C10	0.6124 (3)	0.2101 (2)	−0.1400 (4)	0.0458 (12)
H10	0.6504	0.1929	−0.1964	0.055*
C11	0.5449 (3)	0.1680 (3)	−0.1049 (5)	0.0503 (13)
H11	0.5370	0.1227	−0.1386	0.060*
C12	0.4890 (3)	0.1927 (3)	−0.0202 (5)	0.0497 (13)
H12	0.4429	0.1643	0.0018	0.060*
C13	0.5009 (3)	0.2587 (2)	0.0317 (4)	0.0440 (12)
H13	0.4636	0.2747	0.0898	0.053*
C14	0.5687 (3)	0.3017 (2)	−0.0023 (4)	0.0338 (10)
C15	0.5294 (3)	0.4084 (2)	0.0968 (4)	0.0329 (10)
H15	0.4743	0.3883	0.1023	0.040*
C16	0.5433 (3)	0.4791 (2)	0.1456 (4)	0.0333 (10)
C17	0.4754 (3)	0.5081 (3)	0.2123 (4)	0.0414 (12)
H17	0.4262	0.4807	0.2241	0.050*
C18	0.4806 (3)	0.5746 (3)	0.2589 (5)	0.0493 (13)
H18	0.4371	0.5916	0.3067	0.059*
C19	0.5518 (3)	0.6180 (2)	0.2349 (4)	0.0429 (12)
H19	0.5542	0.6645	0.2638	0.051*
C20	0.6174 (3)	0.5923 (2)	0.1696 (4)	0.0377 (11)
C25	0.7952 (4)	0.5309 (4)	0.3414 (6)	0.0688 (17)
H25	0.7753	0.4877	0.3083	0.083*
C23	0.7891 (5)	0.6193 (4)	0.4986 (6)	0.105 (3)
H23A	0.7556	0.6292	0.5683	0.158*
H23B	0.7822	0.6575	0.4395	0.158*
H23C	0.8500	0.6145	0.5274	0.158*
C24	0.6895 (4)	0.5155 (4)	0.4933 (6)	0.092 (2)
H24A	0.6710	0.5410	0.5639	0.138*
H24B	0.7109	0.4696	0.5197	0.138*
H24C	0.6406	0.5101	0.4318	0.138*
C21	0.6168 (3)	0.5213 (2)	0.1249 (4)	0.0343 (10)
C22	0.6974 (4)	0.7029 (3)	0.1830 (6)	0.0630 (16)
H22A	0.7504	0.7230	0.1565	0.095*
H22C	0.6992	0.7041	0.2726	0.095*
H22B	0.6479	0.7298	0.1483	0.095*
N1	0.6903 (2)	0.32535 (18)	−0.1215 (3)	0.0351 (9)
N2	0.5875 (2)	0.37078 (18)	0.0461 (3)	0.0337 (8)
N3	0.7585 (3)	0.5545 (3)	0.4398 (5)	0.0637 (13)
O3	0.6844 (2)	0.49968 (15)	0.0660 (3)	0.0412 (8)
O2	0.7936 (2)	0.45072 (16)	−0.0930 (3)	0.0452 (8)
O1	0.9148 (2)	0.52743 (19)	−0.1786 (4)	0.0606 (10)
O6	0.8536 (3)	0.5608 (3)	0.2891 (5)	0.0903 (15)
O4	0.6892 (2)	0.63108 (17)	0.1411 (3)	0.0521 (9)
Zn1	0.71596 (3)	0.39911 (3)	0.01970 (5)	0.03524 (13)
Pb1	0.805850 (13)	0.569995 (10)	0.003745 (18)	0.04440 (7)
Cl1	0.70822 (10)	0.63063 (8)	−0.17678 (14)	0.0672 (4)
Cl2	0.80237 (8)	0.34936 (7)	0.17826 (12)	0.0528 (3)
C27	0.9574 (13)	0.7236 (9)	0.2609 (7)	0.098 (3)	0.576 (2)
H27A	0.9198	0.7548	0.3027	0.147*	0.576 (2)
H27B	1.0163	0.7271	0.2992	0.147*	0.576 (2)
H27C	0.9371	0.6756	0.2672	0.147*	0.576 (2)
C26	1.0639 (6)	0.7110 (7)	0.087 (2)	0.074 (3)	0.576 (2)
H26A	1.0806	0.7151	0.0031	0.111*	0.576 (2)
H26B	1.0632	0.6618	0.1104	0.111*	0.576 (2)
H26C	1.1055	0.7360	0.1429	0.111*	0.576 (2)
S1	0.95576 (17)	0.74864 (13)	0.0961 (2)	0.0599 (5)	0.576 (2)
O5	0.8885 (11)	0.6987 (5)	0.0345 (17)	0.073 (5)	0.576 (2)
C27'	0.9400 (18)	0.7406 (10)	0.2440 (14)	0.098 (3)	0.424 (2)
H27D	0.9102	0.7137	0.3036	0.147*	0.424 (2)
H27E	0.8995	0.7731	0.2012	0.147*	0.424 (2)
H27F	0.9874	0.7667	0.2867	0.147*	0.424 (2)
C26'	1.0592 (10)	0.7461 (8)	0.080 (3)	0.074 (3)	0.424 (2)
H26D	1.0844	0.7296	0.0062	0.111*	0.424 (2)
H26E	1.1050	0.7539	0.1452	0.111*	0.424 (2)
H26F	1.0282	0.7897	0.0618	0.111*	0.424 (2)
S1'	0.9837 (2)	0.68004 (18)	0.1302 (3)	0.0599 (5)	0.424 (2)
O5'	0.9125 (17)	0.6873 (8)	0.027 (2)	0.073 (5)	0.424 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.073 (5)	0.080 (5)	0.129 (7)	−0.032 (4)	0.042 (4)	−0.012 (4)
C2	0.045 (3)	0.039 (3)	0.057 (3)	0.002 (2)	0.016 (3)	0.007 (3)
C3	0.063 (4)	0.057 (3)	0.064 (4)	0.002 (3)	0.036 (3)	0.008 (3)
C4	0.078 (4)	0.063 (4)	0.049 (3)	−0.003 (3)	0.037 (3)	−0.001 (3)
C5	0.061 (4)	0.057 (3)	0.044 (3)	0.004 (3)	0.019 (3)	−0.004 (3)
C6	0.045 (3)	0.036 (3)	0.035 (3)	0.005 (2)	0.008 (2)	0.002 (2)
C7	0.040 (3)	0.041 (3)	0.039 (3)	0.010 (2)	0.010 (2)	0.007 (2)
C8	0.042 (3)	0.035 (3)	0.039 (3)	0.006 (2)	0.004 (2)	−0.003 (2)
C9	0.040 (3)	0.029 (2)	0.033 (3)	−0.005 (2)	0.002 (2)	−0.0033 (19)
C10	0.065 (3)	0.035 (3)	0.039 (3)	−0.004 (2)	0.010 (2)	−0.005 (2)
C11	0.077 (4)	0.029 (3)	0.045 (3)	−0.011 (3)	0.004 (3)	−0.008 (2)
C12	0.057 (3)	0.047 (3)	0.046 (3)	−0.019 (3)	0.008 (3)	−0.004 (2)
C13	0.052 (3)	0.041 (3)	0.040 (3)	−0.009 (2)	0.010 (2)	0.001 (2)
C14	0.038 (3)	0.033 (2)	0.031 (2)	−0.006 (2)	0.004 (2)	0.0015 (19)
C15	0.033 (3)	0.035 (2)	0.031 (2)	−0.0024 (19)	0.0039 (19)	0.0039 (19)
C16	0.040 (3)	0.030 (2)	0.030 (2)	0.005 (2)	0.003 (2)	−0.0005 (19)
C17	0.043 (3)	0.045 (3)	0.036 (3)	0.007 (2)	0.004 (2)	0.001 (2)
C18	0.049 (3)	0.050 (3)	0.048 (3)	0.015 (3)	0.004 (2)	−0.010 (3)
C19	0.057 (3)	0.033 (3)	0.038 (3)	0.011 (2)	0.001 (2)	−0.004 (2)
C20	0.048 (3)	0.030 (2)	0.034 (3)	0.001 (2)	−0.001 (2)	0.000 (2)
C25	0.079 (5)	0.074 (4)	0.052 (4)	0.005 (4)	−0.002 (3)	−0.002 (3)
C23	0.150 (7)	0.088 (6)	0.076 (5)	−0.002 (5)	0.007 (5)	−0.013 (4)
C24	0.075 (5)	0.100 (6)	0.103 (6)	0.013 (4)	0.018 (4)	0.044 (5)
C21	0.045 (3)	0.032 (3)	0.026 (2)	0.004 (2)	0.004 (2)	0.0034 (19)
C22	0.073 (4)	0.033 (3)	0.083 (4)	−0.004 (3)	0.004 (3)	−0.012 (3)
N1	0.039 (2)	0.031 (2)	0.036 (2)	0.0011 (17)	0.0061 (17)	−0.0043 (17)
N2	0.042 (2)	0.029 (2)	0.031 (2)	−0.0039 (17)	0.0049 (17)	−0.0003 (16)
N3	0.074 (3)	0.067 (3)	0.050 (3)	0.005 (3)	0.003 (3)	0.007 (3)
O3	0.045 (2)	0.0313 (17)	0.049 (2)	−0.0054 (14)	0.0186 (15)	−0.0070 (15)
O2	0.057 (2)	0.0389 (19)	0.043 (2)	−0.0104 (15)	0.0244 (16)	−0.0070 (15)
O1	0.052 (2)	0.056 (2)	0.077 (3)	−0.0158 (19)	0.0308 (19)	−0.002 (2)
O6	0.084 (3)	0.107 (4)	0.084 (3)	0.009 (3)	0.027 (3)	0.005 (3)
O4	0.066 (2)	0.0349 (19)	0.057 (2)	−0.0089 (17)	0.0159 (18)	−0.0100 (17)
Zn1	0.0403 (3)	0.0300 (3)	0.0366 (3)	−0.0041 (2)	0.0101 (2)	−0.0017 (2)
Pb1	0.04989 (13)	0.04072 (11)	0.04396 (12)	−0.01222 (9)	0.01203 (8)	−0.00356 (9)
Cl1	0.0783 (10)	0.0622 (9)	0.0613 (9)	−0.0068 (8)	0.0069 (7)	0.0132 (7)
Cl2	0.0503 (8)	0.0548 (8)	0.0523 (8)	−0.0035 (6)	−0.0015 (6)	0.0091 (6)
C27	0.103 (4)	0.106 (4)	0.083 (4)	−0.004 (3)	0.006 (3)	−0.001 (3)
C26	0.058 (5)	0.074 (11)	0.085 (6)	0.017 (7)	−0.017 (4)	0.003 (11)
S1	0.0670 (14)	0.0486 (11)	0.0625 (13)	−0.0105 (10)	−0.0049 (10)	0.0059 (10)
O5	0.057 (10)	0.099 (5)	0.063 (3)	−0.039 (6)	0.007 (6)	−0.021 (4)
C27'	0.103 (4)	0.106 (4)	0.083 (4)	−0.004 (3)	0.006 (3)	−0.001 (3)
C26'	0.058 (5)	0.074 (11)	0.085 (6)	0.017 (7)	−0.017 (4)	0.003 (11)
S1'	0.0670 (14)	0.0486 (11)	0.0625 (13)	−0.0105 (10)	−0.0049 (10)	0.0059 (10)
O5'	0.057 (10)	0.099 (5)	0.063 (3)	−0.039 (6)	0.007 (6)	−0.021 (4)

Geometric parameters (Å, º) top

C1—O1	1.427 (6)	C25—H25	0.9300
C1—H1A	0.9600	C23—N3	1.436 (8)
C1—H1B	0.9600	C23—H23A	0.9600
C1—H1C	0.9600	C23—H23B	0.9600
C2—O1	1.367 (6)	C23—H23C	0.9600
C2—C3	1.372 (7)	C24—N3	1.443 (7)
C2—C7	1.422 (6)	C24—H24A	0.9600
C3—C4	1.365 (8)	C24—H24B	0.9600
C3—H3	0.9300	C24—H24C	0.9600
C4—C5	1.362 (7)	C21—O3	1.319 (5)
C4—H4	0.9300	C22—O4	1.428 (5)
C5—C6	1.412 (6)	C22—H22A	0.9600
C5—H5	0.9300	C22—H22C	0.9600
C6—C7	1.406 (6)	C22—H22B	0.9600
C6—C8	1.446 (6)	Zn1—N1	2.070 (4)
C7—O2	1.312 (5)	Zn1—N2	2.077 (3)
C8—N1	1.290 (5)	Zn1—O3	2.028 (3)
C8—H8	0.9300	Zn1—O2	2.014 (3)
C9—C10	1.372 (6)	Zn1—Cl2	2.2686 (14)
C9—C14	1.406 (6)	Pb1—O1	2.791 (4)
C9—N1	1.419 (5)	Pb1—O2	2.476 (3)
C10—C11	1.379 (6)	Pb1—O3	2.420 (3)
C10—H10	0.9300	Pb1—O4	2.667 (3)
C11—C12	1.379 (7)	Pb1—O5	2.741 (5)
C11—H11	0.9300	Pb1—O5'	2.746 (7)
C12—C13	1.369 (6)	Pb1—Cl1	2.6088 (15)
C12—H12	0.9300	C27—S1	1.829 (6)
C13—C14	1.388 (6)	C27—H27A	0.9600
C13—H13	0.9300	C27—H27B	0.9600
C14—N2	1.422 (5)	C27—H27C	0.9600
C15—N2	1.292 (5)	C26—S1	1.809 (6)
C15—C16	1.441 (6)	C26—H26A	0.9600
C15—H15	0.9300	C26—H26B	0.9600
C16—C21	1.409 (6)	C26—H26C	0.9600
C16—C17	1.418 (6)	S1—O5	1.506 (5)
C17—C18	1.349 (6)	C27'—S1'	1.838 (7)
C17—H17	0.9300	C27'—H27D	0.9600
C18—C19	1.402 (7)	C27'—H27E	0.9600
C18—H18	0.9300	C27'—H27F	0.9600
C19—C20	1.359 (6)	C26'—S1'	1.809 (6)
C19—H19	0.9300	C26'—H26D	0.9600
C20—O4	1.375 (5)	C26'—H26E	0.9600
C20—C21	1.421 (6)	C26'—H26F	0.9600
C25—O6	1.230 (7)	S1'—O5'	1.492 (7)
C25—N3	1.314 (7)

O1—C1—H1A	109.5	H24A—C24—H24C	109.5
O1—C1—H1B	109.5	H24B—C24—H24C	109.5
H1A—C1—H1B	109.5	O3—C21—C16	124.6 (4)
O1—C1—H1C	109.5	O3—C21—C20	118.0 (4)
H1A—C1—H1C	109.5	C16—C21—C20	117.4 (4)
H1B—C1—H1C	109.5	O4—C22—H22A	109.5
O1—C2—C3	125.5 (5)	O4—C22—H22C	109.5
O1—C2—C7	113.5 (4)	H22A—C22—H22C	109.5
C3—C2—C7	121.0 (5)	O4—C22—H22B	109.5
C4—C3—C2	120.7 (5)	H22A—C22—H22B	109.5
C4—C3—H3	119.6	H22C—C22—H22B	109.5
C2—C3—H3	119.6	C8—N1—C9	120.7 (4)
C5—C4—C3	120.6 (5)	C8—N1—Zn1	127.6 (3)
C5—C4—H4	119.7	C9—N1—Zn1	111.1 (3)
C3—C4—H4	119.7	C15—N2—C14	122.1 (4)
C4—C5—C6	120.5 (5)	C15—N2—Zn1	127.4 (3)
C4—C5—H5	119.8	C14—N2—Zn1	110.5 (3)
C6—C5—H5	119.8	C25—N3—C23	119.7 (6)
C7—C6—C5	119.8 (4)	C25—N3—C24	121.6 (6)
C7—C6—C8	123.9 (4)	C23—N3—C24	118.7 (6)
C5—C6—C8	116.3 (4)	C21—O3—Zn1	128.2 (3)
O2—C7—C6	125.0 (4)	C21—O3—Pb1	127.8 (3)
O2—C7—C2	117.8 (4)	Zn1—O3—Pb1	103.89 (12)
C6—C7—C2	117.2 (4)	C7—O2—Zn1	129.2 (3)
N1—C8—C6	125.2 (4)	C7—O2—Pb1	127.3 (3)
N1—C8—H8	117.4	Zn1—O2—Pb1	102.38 (12)
C6—C8—H8	117.4	C2—O1—C1	119.2 (4)
C10—C9—C14	119.8 (4)	C20—O4—C22	118.9 (4)
C10—C9—N1	125.1 (4)	C20—O4—Pb1	118.5 (3)
C14—C9—N1	115.1 (4)	C22—O4—Pb1	122.6 (3)
C9—C10—C11	120.0 (5)	O2—Zn1—O3	81.97 (12)
C9—C10—H10	120.0	O2—Zn1—N1	88.26 (13)
C11—C10—H10	120.0	O3—Zn1—N1	140.59 (14)
C10—C11—C12	120.3 (4)	O2—Zn1—N2	144.80 (14)
C10—C11—H11	119.8	O3—Zn1—N2	87.68 (13)
C12—C11—H11	119.8	N1—Zn1—N2	78.68 (14)
C13—C12—C11	120.4 (5)	O2—Zn1—Cl2	108.35 (10)
C13—C12—H12	119.8	O3—Zn1—Cl2	109.75 (10)
C11—C12—H12	119.8	N1—Zn1—Cl2	109.57 (11)
C12—C13—C14	120.1 (4)	N2—Zn1—Cl2	106.82 (10)
C12—C13—H13	120.0	O3—Pb1—O2	65.53 (10)
C14—C13—H13	120.0	O3—Pb1—Cl1	92.31 (8)
C13—C14—C9	119.3 (4)	O2—Pb1—Cl1	93.86 (9)
C13—C14—N2	124.8 (4)	O3—Pb1—O4	61.32 (10)
C9—C14—N2	115.8 (4)	O2—Pb1—O4	126.34 (10)
N2—C15—C16	125.1 (4)	Cl1—Pb1—O4	81.62 (8)
N2—C15—H15	117.5	O3—Pb1—O5	143.8 (5)
C16—C15—H15	117.5	O2—Pb1—O5	150.6 (5)
C21—C16—C17	119.3 (4)	Cl1—Pb1—O5	86.06 (18)
C21—C16—C15	124.0 (4)	O4—Pb1—O5	82.8 (5)
C17—C16—C15	116.6 (4)	O3—Pb1—O5'	151.5 (8)
C18—C17—C16	121.5 (5)	O2—Pb1—O5'	142.5 (8)
C18—C17—H17	119.3	Cl1—Pb1—O5'	90.82 (17)
C16—C17—H17	119.3	O4—Pb1—O5'	91.2 (8)
C17—C18—C19	119.7 (5)	O5—Pb1—O5'	9.1 (12)
C17—C18—H18	120.1	O5—S1—C26	109.0 (10)
C19—C18—H18	120.1	O5—S1—C27	102.6 (9)
C20—C19—C18	120.2 (4)	C26—S1—C27	90.6 (8)
C20—C19—H19	119.9	S1—O5—Pb1	153.7 (5)
C18—C19—H19	119.9	S1'—C27'—H27D	109.5
C19—C20—O4	124.2 (4)	S1'—C27'—H27E	109.5
C19—C20—C21	121.8 (4)	H27D—C27'—H27E	109.5
O4—C20—C21	114.0 (4)	S1'—C27'—H27F	109.5
O6—C25—N3	125.9 (6)	H27D—C27'—H27F	109.5
O6—C25—H25	117.0	H27E—C27'—H27F	109.5
N3—C25—H25	117.0	S1'—C26'—H26D	109.5
N3—C23—H23A	109.5	S1'—C26'—H26E	109.5
N3—C23—H23B	109.5	H26D—C26'—H26E	109.5
H23A—C23—H23B	109.5	S1'—C26'—H26F	109.5
N3—C23—H23C	109.5	H26D—C26'—H26F	109.5
H23A—C23—H23C	109.5	H26E—C26'—H26F	109.5
H23B—C23—H23C	109.5	O5'—S1'—C26'	99.2 (11)
N3—C24—H24A	109.5	O5'—S1'—C27'	98.7 (16)
N3—C24—H24B	109.5	C26'—S1'—C27'	92.7 (12)
H24A—C24—H24B	109.5	S1'—O5'—Pb1	112.7 (5)
N3—C24—H24C	109.5

Experimental details

Crystal data
Chemical formula	[PbZn(C₂₂H₁₈N₂O₄)Cl₂(C₂H₆OS)]·C₃H₇NO
M_r	869.07
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	295
a, b, c (Å)	15.2850 (7), 18.8433 (8), 10.7343 (5)
β (°)	94.771 (1)
V (Å³)	3081.0 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	6.52
Crystal size (mm)	0.2 × 0.15 × 0.1

Data collection
Diffractometer	Bruker APEX CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.343, 0.518
No. of measured, independent and observed [I > 2σ(I)] reflections	18055, 6997, 4923
R_int	0.039
(sin θ/λ)_max (Å⁻¹)	0.651

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.073, 0.99
No. of reflections	6997
No. of parameters	387
No. of restraints	28
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.75, −0.61

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Zn1—N1	2.070 (4)	Pb1—O2	2.476 (3)
Zn1—N2	2.077 (3)	Pb1—O3	2.420 (3)
Zn1—O3	2.028 (3)	Pb1—O4	2.667 (3)
Zn1—O2	2.014 (3)	Pb1—O5	2.741 (5)
Zn1—Cl2	2.2686 (14)	Pb1—O5'	2.746 (7)
Pb1—O1	2.791 (4)	Pb1—Cl1	2.6088 (15)

Acknowledgements

This work was supported by the Natural Science Foundation of China and the Post-Doctoral Innovation Project of Shandong Province.

References

Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Karlin, K. D. (1993). Science, 261, 701–708. CrossRef CAS PubMed Web of Science Google Scholar
Korupoju, S. R., Mangayarkarasi, N., Ameerunisha, S., Valente, E. J. & Zacharias, P. S. (2000). J. Chem. Soc. Dalton Trans. pp. 2845–2852. Web of Science CSD CrossRef Google Scholar
Lo, W.-K., Wong, W.-K., Guo, J., Wong, W.-Y., Li, K.-F. & Cheah, K. W. (2004). Inorg. Chim. Acta, 357, 4510–4521. Web of Science CSD CrossRef CAS Google Scholar
Ni, Z. H., Kou, H.-Z., Zhao, Y.-H., Zheng, L., Wang, R.-J., Cui, A.-L. & Sato, O. (2005). Inorg. Chem. 44, 2050–2059. Web of Science CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sui, Y., Sui, Y.-H., Luo, Q.-Y. & Wang, Y.-D. (2007). Acta Cryst. E63, m2277–m2278. CrossRef IUCr Journals Google Scholar
Ward, M. D. (2007). Coord. Chem. Rev. 251, 1663–1677. Web of Science CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.