Di-μ-azido-κ4N1:N1-bis­[(1,10-phen­anthroline-κ2N,N′)(thio­cyanato-κN)lead(II)]

Mohammadnezhad, G.; Ghanbarpour, A.R.; Amini, M.M.; Ng, S.W.

doi:10.1107/S1600536810032125

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 9| September 2010| Page m1120

https://doi.org/10.1107/S1600536810032125

Open

access

Di-μ-azido-κ⁴N¹:N¹-bis[(1,10-phenanthroline-κ²N,N′)(thiocyanato-κN)lead(II)]

Gholamhossein Mohammadnezhad,^a Ali Reza Ghanbarpour,^a Mostafa M. Amini ^a and Seik Weng Ng ^b ^*

^aDepartment of Chemistry, General Campus, Shahid Beheshti University, Tehran 1983963113, Iran, and ^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 3 August 2010; accepted 10 August 2010; online 18 August 2010)

In the centrosymmetric binuclear title compound, [Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄], the N-donor atoms of one N-heterocycle and the N-donor atom of a thiocyanate anion along with the sterically active lone-pair electrons comprise an approximate square; a plane through three atoms of this square is twisted slightly with respect to the square made up of the other four atoms (two from the other N-heterocycle and one each from the bridging azide anions) at a dihedral angle of 18.7 (1)°. The Pb^II atom is in a Ψ-square-antiprismaic coordination.

Related literature

For related structures, see: Engelhardt et al. (1989 ); Zhu et al. (2008 ).

Experimental

Crystal data

[Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄]
M_r = 1335.42
Triclinic, $[P \overline 1]$
a = 10.3412 (6) Å
b = 10.8327 (6) Å
c = 11.4178 (6) Å
α = 89.923 (1)°
β = 72.080 (1)°
γ = 65.273 (1)°
V = 1093.35 (10) Å³
Z = 1
Mo Kα radiation
μ = 7.85 mm⁻¹
T = 100 K
0.25 × 0.15 × 0.15 mm

Data collection

Bruker SMART APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.244, T_max = 0.386
10523 measured reflections
5002 independent reflections
4783 reflections with I > 2σ(I)
R_int = 0.021

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.061
S = 1.09
5002 reflections
316 parameters
H-atom parameters constrained
Δρ_max = 1.23 e Å⁻³
Δρ_min = −1.38 e Å⁻³

Data collection: APEX2 (Bruker, 2009 ); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810032125/ci5151sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810032125/ci5151Isup2.hkl

checkCIF report

Comment top

Relative to the (1,10-phenanthroline)lead(II) species, the azide counterion can function as a bridging unit through only one nitrogen atom only or through two end nitrogen atoms. In fact, an example is known in which the anion functions in both bridging modes (Zhu et al., 2008). Similarly, an example is known in which the thiocyanate anion functions in dual bridging modes (Engelhardt et al., 1989). The title compound (Scheme I) is a centrosymmetric dinuclear lead(II) compound having the azide and thiocyanate anions behaving only in one type of bonding interaction; the azide bridges through only one nitrogen atom but the thiocyanate anion is unidentate (Fig. 1). The nitrogen donor-atoms of one 1,10-phenanthroline ligand, the nitrogen donor-atom of a thiocyanate along with the sterically active lone-pair electrons comprise an approximate square (Fig. 2); the three atoms of this square is slightly twisted with respect to the square made up by the other four atoms (two from the other 1,10-phenanthroline and one each from the bridging azide anions) at a dihedral angle of 18.7 (1)°. Obviously, the tilt arises from the presence of the lone pair. The lead atom is displaced by 1.044 (3) Å with respect to the three-atom plane and is displaced in the opposite direction by 1.548 (1) Å with respect to the four atom plane. The geometry of the lead atom is better regarded as showing Ψ-square antiprismatic coordination.

Related literature top

For related structures, see: Engelhardt et al. (1989); Zhu et al. (2008).

Experimental top

Potassium thiocyanate (0.5 mmol, 0.09 g), sodium azide (0.03 g, 0.05 mmol) and 1,10-phenanthroline (2 mmol, 0.36 g) were loaded into one arm of a U-shaped glass tube. Lead(II) acetate (0.38 g, 1 mmol) and sodium nitrite (0.07 g, 1 mmol) were loaded into the other. Methanol was added to both arms. The ligand-containing arm was immersed in an oil bath at 333 K whereas the other arm was kept at ambient temperature. Crystals were collected after 10 days.

Structure description top

For related structures, see: Engelhardt et al. (1989); Zhu et al. (2008).

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Displacement ellipsoid plot (Barbour, 2001) of centrosymmetric [Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄] at the 70% probability level. H atoms are drawn as spheres of arbitrary radius. Symmetry-related (1 - x, 1 - y, 1 - z) atoms are not labeled.
	Fig. 2. The square environment of the Pb atom.

Di-µ-azido-κ⁴N¹:N¹-bis[(1,10-phenanthroline- κ²N,N')(thiocyanato-κN)lead(II)] top

Crystal data top

[Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄]	Z = 1
M_r = 1335.42	F(000) = 642
Triclinic, P1	D_x = 2.034 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.3412 (6) Å	Cell parameters from 8054 reflections
b = 10.8327 (6) Å	θ = 2.3–28.3°
c = 11.4178 (6) Å	µ = 7.85 mm⁻¹
α = 89.923 (1)°	T = 100 K
β = 72.080 (1)°	Prism, colourless
γ = 65.273 (1)°	0.25 × 0.15 × 0.15 mm
V = 1093.35 (10) Å³

Data collection top

Bruker SMART APEXII area-detector diffractometer	5002 independent reflections
Radiation source: fine-focus sealed tube	4783 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
ω scans	θ_max = 27.5°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→13
T_min = 0.244, T_max = 0.386	k = −14→13
10523 measured reflections	l = −14→14

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) = 0.061	H-atom parameters constrained
S = 1.09	w = 1/[σ²(F_o²) + (0.041P)²] where P = (F_o² + 2F_c²)/3
5002 reflections	(Δ/σ)_max = 0.001
316 parameters	Δρ_max = 1.23 e Å⁻³
0 restraints	Δρ_min = −1.38 e Å⁻³

Crystal data top

[Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄]	γ = 65.273 (1)°
M_r = 1335.42	V = 1093.35 (10) Å³
Triclinic, P1	Z = 1
a = 10.3412 (6) Å	Mo Kα radiation
b = 10.8327 (6) Å	µ = 7.85 mm⁻¹
c = 11.4178 (6) Å	T = 100 K
α = 89.923 (1)°	0.25 × 0.15 × 0.15 mm
β = 72.080 (1)°

Data collection top

Bruker SMART APEXII area-detector diffractometer	5002 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	4783 reflections with I > 2σ(I)
T_min = 0.244, T_max = 0.386	R_int = 0.021
10523 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	0 restraints
wR(F²) = 0.061	H-atom parameters constrained
S = 1.09	Δρ_max = 1.23 e Å⁻³
5002 reflections	Δρ_min = −1.38 e Å⁻³
316 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pb1	0.451831 (12)	0.668463 (11)	0.618902 (10)	0.00916 (5)
S1	−0.09428 (10)	0.84240 (11)	0.95648 (9)	0.0222 (2)
N1	0.3623 (3)	0.8343 (3)	0.4496 (3)	0.0121 (6)
N2	0.6474 (3)	0.7683 (3)	0.4566 (3)	0.0114 (6)
N3	0.4103 (3)	0.4959 (3)	0.7794 (3)	0.0120 (6)
N4	0.6519 (3)	0.5550 (3)	0.7575 (3)	0.0120 (6)
N5	0.6529 (3)	0.4519 (3)	0.4832 (3)	0.0123 (6)
N6	0.7855 (3)	0.4215 (3)	0.4627 (3)	0.0126 (6)
N7	0.9113 (4)	0.3913 (3)	0.4423 (3)	0.0233 (7)
N8	0.1509 (3)	0.8079 (3)	0.7442 (3)	0.0192 (6)
C1	0.4430 (4)	0.8968 (3)	0.3809 (3)	0.0105 (6)
C2	0.2277 (4)	0.8640 (4)	0.4419 (4)	0.0155 (7)
H2	0.1709	0.8205	0.4904	0.019*
C3	0.1637 (4)	0.9559 (4)	0.3663 (3)	0.0142 (7)
H3	0.0672	0.9724	0.3631	0.017*
C4	0.2422 (4)	1.0207 (4)	0.2979 (3)	0.0151 (7)
H4	0.2006	1.0841	0.2468	0.018*
C5	0.3852 (4)	0.9931 (4)	0.3035 (3)	0.0124 (6)
C6	0.4768 (4)	1.0539 (3)	0.2299 (3)	0.0137 (7)
H6	0.4386	1.1174	0.1775	0.016*
C7	0.6157 (4)	1.0224 (4)	0.2339 (3)	0.0135 (7)
H7	0.6738	1.0641	0.1844	0.016*
C8	0.6776 (4)	0.9273 (3)	0.3113 (3)	0.0120 (6)
C9	0.8244 (4)	0.8902 (4)	0.3146 (3)	0.0141 (7)
H9	0.8849	0.9309	0.2670	0.017*
C10	0.8783 (4)	0.7946 (4)	0.3876 (3)	0.0151 (7)
H10	0.9766	0.7682	0.3915	0.018*
C11	0.7866 (4)	0.7369 (4)	0.4559 (3)	0.0138 (7)
H11	0.8263	0.6703	0.5054	0.017*
C12	0.5929 (4)	0.8631 (3)	0.3841 (3)	0.0098 (6)
C13	0.5152 (4)	0.4199 (4)	0.8317 (3)	0.0115 (6)
C14	0.2921 (4)	0.4702 (4)	0.7950 (3)	0.0141 (7)
H14	0.2183	0.5243	0.7597	0.017*
C15	0.2702 (4)	0.3671 (4)	0.8612 (3)	0.0133 (7)
H15	0.1833	0.3527	0.8706	0.016*
C16	0.3759 (4)	0.2880 (4)	0.9118 (3)	0.0136 (7)
H16	0.3639	0.2172	0.9563	0.016*
C17	0.5034 (4)	0.3128 (3)	0.8971 (3)	0.0113 (6)
C18	0.6175 (4)	0.2330 (4)	0.9489 (3)	0.0145 (7)
H18	0.6107	0.1584	0.9898	0.017*
C19	0.7349 (4)	0.2629 (4)	0.9401 (3)	0.0142 (7)
H19	0.8093	0.2095	0.9752	0.017*
C20	0.7469 (4)	0.3743 (4)	0.8785 (3)	0.0125 (7)
C21	0.8638 (4)	0.4121 (4)	0.8715 (3)	0.0145 (7)
H21	0.9364	0.3640	0.9100	0.017*
C22	0.8727 (4)	0.5168 (4)	0.8102 (3)	0.0150 (7)
H22	0.9505	0.5435	0.8057	0.018*
C23	0.7647 (4)	0.5852 (4)	0.7531 (3)	0.0139 (7)
H23	0.7732	0.6573	0.7089	0.017*
C24	0.6409 (4)	0.4512 (3)	0.8211 (3)	0.0102 (6)
C25	0.0496 (4)	0.8222 (4)	0.8327 (3)	0.0142 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.00832 (7)	0.01057 (7)	0.00924 (8)	−0.00546 (5)	−0.00197 (5)	0.00214 (5)
S1	0.0135 (4)	0.0343 (5)	0.0161 (5)	−0.0093 (4)	−0.0034 (4)	0.0113 (4)
N1	0.0106 (13)	0.0119 (14)	0.0143 (14)	−0.0061 (11)	−0.0032 (11)	0.0025 (11)
N2	0.0114 (13)	0.0113 (14)	0.0117 (14)	−0.0057 (11)	−0.0030 (11)	0.0027 (11)
N3	0.0125 (13)	0.0134 (14)	0.0113 (14)	−0.0069 (11)	−0.0040 (11)	0.0053 (11)
N4	0.0122 (13)	0.0137 (14)	0.0096 (14)	−0.0071 (11)	−0.0010 (11)	0.0016 (11)
N5	0.0106 (13)	0.0121 (14)	0.0144 (14)	−0.0064 (11)	−0.0023 (11)	0.0008 (11)
N6	0.0145 (14)	0.0113 (14)	0.0143 (15)	−0.0075 (11)	−0.0055 (12)	0.0026 (11)
N7	0.0137 (15)	0.0235 (17)	0.034 (2)	−0.0092 (13)	−0.0084 (14)	0.0047 (15)
N8	0.0147 (15)	0.0193 (16)	0.0184 (16)	−0.0066 (13)	−0.0002 (13)	0.0012 (13)
C1	0.0117 (15)	0.0119 (16)	0.0044 (14)	−0.0051 (13)	0.0016 (12)	−0.0017 (12)
C2	0.0154 (16)	0.0155 (18)	0.0184 (18)	−0.0087 (14)	−0.0069 (14)	0.0040 (14)
C3	0.0108 (15)	0.0165 (17)	0.0145 (17)	−0.0050 (14)	−0.0047 (13)	0.0010 (14)
C4	0.0159 (17)	0.0148 (17)	0.0142 (17)	−0.0049 (14)	−0.0073 (14)	0.0030 (14)
C5	0.0131 (15)	0.0112 (16)	0.0104 (16)	−0.0046 (13)	−0.0019 (13)	−0.0002 (13)
C6	0.0158 (16)	0.0100 (16)	0.0118 (16)	−0.0036 (13)	−0.0029 (13)	0.0023 (13)
C7	0.0152 (16)	0.0137 (16)	0.0091 (16)	−0.0086 (13)	0.0021 (13)	0.0001 (13)
C8	0.0121 (15)	0.0098 (16)	0.0107 (16)	−0.0045 (13)	0.0002 (13)	−0.0021 (13)
C9	0.0134 (16)	0.0115 (16)	0.0160 (17)	−0.0075 (13)	−0.0003 (13)	−0.0009 (13)
C10	0.0109 (15)	0.0179 (18)	0.0142 (17)	−0.0048 (14)	−0.0034 (13)	−0.0014 (14)
C11	0.0120 (15)	0.0138 (17)	0.0136 (17)	−0.0052 (13)	−0.0025 (13)	0.0008 (13)
C12	0.0103 (15)	0.0103 (15)	0.0057 (15)	−0.0043 (12)	0.0012 (12)	−0.0007 (12)
C13	0.0110 (15)	0.0127 (16)	0.0093 (16)	−0.0042 (13)	−0.0028 (12)	−0.0004 (13)
C14	0.0138 (16)	0.0175 (17)	0.0138 (17)	−0.0080 (14)	−0.0068 (13)	0.0038 (14)
C15	0.0120 (15)	0.0181 (17)	0.0114 (16)	−0.0108 (14)	0.0001 (13)	−0.0003 (13)
C16	0.0159 (16)	0.0131 (16)	0.0075 (16)	−0.0069 (14)	0.0023 (13)	−0.0009 (13)
C17	0.0136 (15)	0.0105 (16)	0.0053 (15)	−0.0039 (13)	0.0006 (12)	−0.0022 (12)
C18	0.0161 (16)	0.0130 (17)	0.0112 (16)	−0.0047 (14)	−0.0031 (13)	0.0037 (13)
C19	0.0140 (16)	0.0143 (17)	0.0125 (16)	−0.0043 (13)	−0.0047 (13)	0.0027 (13)
C20	0.0123 (16)	0.0148 (17)	0.0069 (15)	−0.0040 (13)	−0.0016 (13)	−0.0025 (13)
C21	0.0120 (15)	0.0172 (17)	0.0122 (16)	−0.0039 (13)	−0.0050 (13)	−0.0004 (13)
C22	0.0100 (15)	0.0227 (19)	0.0120 (16)	−0.0094 (14)	0.0000 (13)	−0.0008 (14)
C23	0.0118 (15)	0.0165 (17)	0.0115 (16)	−0.0077 (13)	0.0004 (13)	0.0006 (13)
C24	0.0100 (15)	0.0120 (16)	0.0061 (15)	−0.0043 (13)	−0.0003 (12)	−0.0009 (12)
C25	0.0127 (16)	0.0134 (17)	0.0163 (17)	−0.0048 (13)	−0.0059 (14)	0.0043 (13)

Geometric parameters (Å, º) top

Pb1—N5	2.485 (3)	C6—H6	0.95
Pb1—N5ⁱ	2.489 (3)	C7—C8	1.430 (5)
Pb1—N3	2.687 (3)	C7—H7	0.95
Pb1—N8	2.711 (3)	C8—C12	1.415 (5)
Pb1—N1	2.742 (3)	C8—C9	1.412 (5)
Pb1—N4	2.860 (3)	C9—C10	1.370 (5)
Pb1—N2	2.865 (3)	C9—H9	0.95
S1—C25	1.641 (4)	C10—C11	1.392 (5)
N1—C2	1.324 (4)	C10—H10	0.95
N1—C1	1.356 (4)	C11—H11	0.95
N2—C11	1.331 (4)	C13—C17	1.407 (5)
N2—C12	1.364 (4)	C13—C24	1.446 (5)
N3—C14	1.324 (4)	C14—C15	1.404 (5)
N3—C13	1.364 (4)	C14—H14	0.95
N4—C23	1.325 (4)	C15—C16	1.366 (5)
N4—C24	1.363 (4)	C15—H15	0.95
N5—N6	1.211 (4)	C16—C17	1.413 (5)
N5—Pb1ⁱ	2.489 (3)	C16—H16	0.95
N6—N7	1.145 (4)	C17—C18	1.437 (5)
N8—C25	1.164 (5)	C18—C19	1.358 (5)
C1—C5	1.423 (5)	C18—H18	0.95
C1—C12	1.448 (5)	C19—C20	1.427 (5)
C2—C3	1.404 (5)	C19—H19	0.95
C2—H2	0.95	C20—C21	1.412 (5)
C3—C4	1.359 (5)	C20—C24	1.415 (5)
C3—H3	0.95	C21—C22	1.353 (5)
C4—C5	1.403 (5)	C21—H21	0.95
C4—H4	0.95	C22—C23	1.405 (5)
C5—C6	1.439 (5)	C22—H22	0.95
C6—C7	1.347 (5)	C23—H23	0.95

N5—Pb1—N5ⁱ	67.99 (11)	C6—C7—C8	121.3 (3)
N5—Pb1—N3	82.92 (9)	C6—C7—H7	119.3
N5ⁱ—Pb1—N3	77.99 (9)	C8—C7—H7	119.3
N5—Pb1—N8	144.35 (10)	C12—C8—C9	118.0 (3)
N5ⁱ—Pb1—N8	78.18 (10)	C12—C8—C7	119.8 (3)
N3—Pb1—N8	79.30 (9)	C9—C8—C7	122.2 (3)
N5—Pb1—N1	102.42 (9)	C10—C9—C8	118.9 (3)
N5ⁱ—Pb1—N1	76.63 (9)	C10—C9—H9	120.5
N3—Pb1—N1	149.70 (8)	C8—C9—H9	120.5
N8—Pb1—N1	79.54 (9)	C9—C10—C11	119.0 (3)
N5—Pb1—N4	76.52 (9)	C9—C10—H10	120.5
N5ⁱ—Pb1—N4	127.42 (9)	C11—C10—H10	120.5
N3—Pb1—N4	59.80 (8)	N2—C11—C10	124.6 (3)
N8—Pb1—N4	118.75 (9)	N2—C11—H11	117.7
N1—Pb1—N4	150.49 (8)	C10—C11—H11	117.7
N5—Pb1—N2	79.06 (9)	N2—C12—C8	122.6 (3)
N5ⁱ—Pb1—N2	116.13 (9)	N2—C12—C1	118.0 (3)
N3—Pb1—N2	150.03 (8)	C8—C12—C1	119.4 (3)
N8—Pb1—N2	127.96 (9)	N3—C13—C17	121.7 (3)
N1—Pb1—N2	58.79 (8)	N3—C13—C24	119.2 (3)
N4—Pb1—N2	92.59 (8)	C17—C13—C24	119.0 (3)
C2—N1—C1	118.1 (3)	N3—C14—C15	123.3 (3)
C2—N1—Pb1	118.2 (2)	N3—C14—H14	118.3
C1—N1—Pb1	123.5 (2)	C15—C14—H14	118.3
C11—N2—C12	116.9 (3)	C16—C15—C14	118.9 (3)
C11—N2—Pb1	123.4 (2)	C16—C15—H15	120.5
C12—N2—Pb1	119.4 (2)	C14—C15—H15	120.5
C14—N3—C13	118.5 (3)	C15—C16—C17	119.2 (3)
C14—N3—Pb1	117.9 (2)	C15—C16—H16	120.4
C13—N3—Pb1	123.0 (2)	C17—C16—H16	120.4
C23—N4—C24	117.7 (3)	C16—C17—C13	118.3 (3)
C23—N4—Pb1	124.6 (2)	C16—C17—C18	121.4 (3)
C24—N4—Pb1	117.2 (2)	C13—C17—C18	120.3 (3)
N6—N5—Pb1	121.1 (2)	C19—C18—C17	120.8 (3)
N6—N5—Pb1ⁱ	126.5 (2)	C19—C18—H18	119.6
Pb1—N5—Pb1ⁱ	112.01 (11)	C17—C18—H18	119.6
N7—N6—N5	179.1 (4)	C18—C19—C20	120.2 (3)
C25—N8—Pb1	147.1 (3)	C18—C19—H19	119.9
N1—C1—C5	121.6 (3)	C20—C19—H19	119.9
N1—C1—C12	119.4 (3)	C21—C20—C24	117.3 (3)
C5—C1—C12	119.0 (3)	C21—C20—C19	122.0 (3)
N1—C2—C3	123.8 (3)	C24—C20—C19	120.7 (3)
N1—C2—H2	118.1	C22—C21—C20	120.1 (3)
C3—C2—H2	118.1	C22—C21—H21	120.0
C4—C3—C2	118.9 (3)	C20—C21—H21	120.0
C4—C3—H3	120.5	C21—C22—C23	118.7 (3)
C2—C3—H3	120.5	C21—C22—H22	120.6
C3—C4—C5	119.3 (3)	C23—C22—H22	120.6
C3—C4—H4	120.4	N4—C23—C22	123.8 (3)
C5—C4—H4	120.4	N4—C23—H23	118.1
C4—C5—C1	118.3 (3)	C22—C23—H23	118.1
C4—C5—C6	122.2 (3)	N4—C24—C20	122.4 (3)
C1—C5—C6	119.5 (3)	N4—C24—C13	118.8 (3)
C7—C6—C5	121.1 (3)	C20—C24—C13	118.8 (3)
C7—C6—H6	119.5	N8—C25—S1	179.4 (3)
C5—C6—H6	119.5

N5—Pb1—N1—C2	109.1 (3)	C1—N1—C2—C3	0.3 (5)
N5ⁱ—Pb1—N1—C2	45.6 (3)	Pb1—N1—C2—C3	174.9 (3)
N3—Pb1—N1—C2	11.8 (4)	N1—C2—C3—C4	−1.1 (6)
N8—Pb1—N1—C2	−34.6 (3)	C2—C3—C4—C5	0.7 (5)
N4—Pb1—N1—C2	−166.4 (2)	C3—C4—C5—C1	0.3 (5)
N2—Pb1—N1—C2	178.0 (3)	C3—C4—C5—C6	177.5 (3)
N5—Pb1—N1—C1	−76.6 (3)	N1—C1—C5—C4	−1.1 (5)
N5ⁱ—Pb1—N1—C1	−140.1 (3)	C12—C1—C5—C4	177.6 (3)
N3—Pb1—N1—C1	−173.9 (2)	N1—C1—C5—C6	−178.4 (3)
N8—Pb1—N1—C1	139.7 (3)	C12—C1—C5—C6	0.4 (5)
N4—Pb1—N1—C1	7.9 (4)	C4—C5—C6—C7	−177.9 (3)
N2—Pb1—N1—C1	−7.8 (2)	C1—C5—C6—C7	−0.7 (5)
N5—Pb1—N2—C11	−67.0 (3)	C5—C6—C7—C8	0.0 (5)
N5ⁱ—Pb1—N2—C11	−125.6 (3)	C6—C7—C8—C12	0.9 (5)
N3—Pb1—N2—C11	−12.9 (4)	C6—C7—C8—C9	178.4 (3)
N8—Pb1—N2—C11	139.0 (3)	C12—C8—C9—C10	−0.1 (5)
N1—Pb1—N2—C11	−178.9 (3)	C7—C8—C9—C10	−177.6 (3)
N4—Pb1—N2—C11	8.8 (3)	C8—C9—C10—C11	0.2 (5)
N5—Pb1—N2—C12	119.5 (2)	C12—N2—C11—C10	0.6 (5)
N5ⁱ—Pb1—N2—C12	60.9 (3)	Pb1—N2—C11—C10	−173.1 (3)
N3—Pb1—N2—C12	173.6 (2)	C9—C10—C11—N2	−0.4 (6)
N8—Pb1—N2—C12	−34.5 (3)	C11—N2—C12—C8	−0.5 (5)
N1—Pb1—N2—C12	7.6 (2)	Pb1—N2—C12—C8	173.4 (2)
N4—Pb1—N2—C12	−164.7 (2)	C11—N2—C12—C1	178.6 (3)
N5—Pb1—N3—C14	−104.1 (3)	Pb1—N2—C12—C1	−7.5 (4)
N5ⁱ—Pb1—N3—C14	−35.1 (3)	C9—C8—C12—N2	0.3 (5)
N8—Pb1—N3—C14	44.9 (3)	C7—C8—C12—N2	177.8 (3)
N1—Pb1—N3—C14	−1.5 (4)	C9—C8—C12—C1	−178.8 (3)
N4—Pb1—N3—C14	177.4 (3)	C7—C8—C12—C1	−1.2 (5)
N2—Pb1—N3—C14	−157.3 (2)	N1—C1—C12—N2	0.3 (5)
N5—Pb1—N3—C13	66.6 (3)	C5—C1—C12—N2	−178.5 (3)
N5ⁱ—Pb1—N3—C13	135.5 (3)	N1—C1—C12—C8	179.4 (3)
N8—Pb1—N3—C13	−144.4 (3)	C5—C1—C12—C8	0.6 (5)
N1—Pb1—N3—C13	169.2 (2)	C14—N3—C13—C17	2.3 (5)
N4—Pb1—N3—C13	−11.9 (2)	Pb1—N3—C13—C17	−168.3 (2)
N2—Pb1—N3—C13	13.4 (4)	C14—N3—C13—C24	−176.8 (3)
N5—Pb1—N4—C23	93.2 (3)	Pb1—N3—C13—C24	12.6 (4)
N5ⁱ—Pb1—N4—C23	141.3 (3)	C13—N3—C14—C15	−1.0 (5)
N3—Pb1—N4—C23	−177.2 (3)	Pb1—N3—C14—C15	170.1 (3)
N8—Pb1—N4—C23	−121.5 (3)	N3—C14—C15—C16	−0.4 (6)
N1—Pb1—N4—C23	1.8 (4)	C14—C15—C16—C17	0.5 (5)
N2—Pb1—N4—C23	15.1 (3)	C15—C16—C17—C13	0.8 (5)
N5—Pb1—N4—C24	−78.8 (2)	C15—C16—C17—C18	179.7 (3)
N5ⁱ—Pb1—N4—C24	−30.8 (3)	N3—C13—C17—C16	−2.2 (5)
N3—Pb1—N4—C24	10.8 (2)	C24—C13—C17—C16	176.9 (3)
N8—Pb1—N4—C24	66.4 (2)	N3—C13—C17—C18	178.8 (3)
N1—Pb1—N4—C24	−170.3 (2)	C24—C13—C17—C18	−2.1 (5)
N2—Pb1—N4—C24	−156.9 (2)	C16—C17—C18—C19	−176.2 (3)
N5ⁱ—Pb1—N5—N6	173.0 (3)	C13—C17—C18—C19	2.7 (5)
N3—Pb1—N5—N6	−107.1 (3)	C17—C18—C19—C20	−0.3 (5)
N8—Pb1—N5—N6	−167.5 (2)	C18—C19—C20—C21	177.5 (3)
N1—Pb1—N5—N6	103.1 (3)	C18—C19—C20—C24	−2.7 (5)
N4—Pb1—N5—N6	−46.6 (3)	C24—C20—C21—C22	−1.0 (5)
N2—Pb1—N5—N6	48.8 (3)	C19—C20—C21—C22	178.8 (3)
N5ⁱ—Pb1—N5—Pb1ⁱ	0.0	C20—C21—C22—C23	−0.6 (5)
N3—Pb1—N5—Pb1ⁱ	79.87 (12)	C24—N4—C23—C22	−0.1 (5)
N8—Pb1—N5—Pb1ⁱ	19.5 (2)	Pb1—N4—C23—C22	−172.1 (3)
N1—Pb1—N5—Pb1ⁱ	−69.85 (12)	C21—C22—C23—N4	1.2 (5)
N4—Pb1—N5—Pb1ⁱ	140.43 (13)	C23—N4—C24—C20	−1.6 (5)
N2—Pb1—N5—Pb1ⁱ	−124.19 (12)	Pb1—N4—C24—C20	171.0 (2)
N5—Pb1—N8—C25	79.2 (6)	C23—N4—C24—C13	177.5 (3)
N5ⁱ—Pb1—N8—C25	97.7 (5)	Pb1—N4—C24—C13	−9.9 (4)
N3—Pb1—N8—C25	17.8 (5)	C21—C20—C24—N4	2.2 (5)
N1—Pb1—N8—C25	176.0 (5)	C19—C20—C24—N4	−177.6 (3)
N4—Pb1—N8—C25	−28.7 (6)	C21—C20—C24—C13	−176.9 (3)
N2—Pb1—N8—C25	−148.3 (5)	C19—C20—C24—C13	3.3 (5)
C2—N1—C1—C5	0.8 (5)	N3—C13—C24—N4	−0.9 (5)
Pb1—N1—C1—C5	−173.5 (2)	C17—C13—C24—N4	180.0 (3)
C2—N1—C1—C12	−177.9 (3)	N3—C13—C24—C20	178.3 (3)
Pb1—N1—C1—C12	7.8 (4)	C17—C13—C24—C20	−0.9 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Pb₂(N₃)₂(NCS)₂(C₁₂H₈N₂)₄]
M_r	1335.42
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	10.3412 (6), 10.8327 (6), 11.4178 (6)
α, β, γ (°)	89.923 (1), 72.080 (1), 65.273 (1)
V (Å³)	1093.35 (10)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	7.85
Crystal size (mm)	0.25 × 0.15 × 0.15

Data collection
Diffractometer	Bruker SMART APEXII area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.244, 0.386
No. of measured, independent and observed [I > 2σ(I)] reflections	10523, 5002, 4783
R_int	0.021
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.061, 1.09
No. of reflections	5002
No. of parameters	316
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.23, −1.38

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Acknowledgements

The authors thank Shahid Beheshti University and the University of Malaya for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Engelhardt, L. M., Furphy, B. M., Harrowfield, J. M., Patrick, J. M., Skelton, B. W. & White, A. H. (1989). J. Chem. Soc. Dalton Trans. pp. 595–599. CSD CrossRef Web of Science Google Scholar
Sheldrick, G. M. (1996). 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
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhu, L. H., Zeng, M. H., Shen, X. C. & Ng, S. W. (2008). Main Group Met. Chem. 30, 103–104. 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.