catena-Poly[[(1,10-phenanthroline-κN,N')lead(II)]-di-μ-nitrato-κO,O':O'';κO:O',O''-[(1,10-phenanthroline-κN,N')lead(II)]-bis-(μ-2,2,2-trichloro-acetato-κO:O')].

In the title Pb(II) complex, [Pb(2)(C(2)Cl(3)O(2))(2)(NO(3))(2)(C(12)H(8)N(2))(2)](n), the 1,10-phenanthroline ligand is chelating, the nitrate anion chelates one Pb(II) ion and simultaneously bridges a neighbouring Pb(II) ion via the third O atom, and the trichloro-acetate anion is bidentate, bridging two Pb(II) ions. The coordination geometry is based on a penta-gonal-bipramidal geometry defined by an N(2)O(5) donor set with no obvious stereochemical role for the lead-bound lone pair of electrons. The coordination polymer has a zigzag topology along [010] and comprises alternating eight-membered {PbONO}(2) and {PbOCO}(2) rings.

Related literature

On the stereochemical activity of lone pairs of electrons in PbII structures, see: Davidovich et al. (2009 ▶). For recent structural studies of mixed-ligand PbII compounds, see: Shahverdizadeh et al. (2008 ▶, 2011a ▶,b ▶). For specialized crystallization techniques, see: Harrowfield et al. (1996 ▶).

Experimental

Crystal data

[Pb2(C2Cl3O2)2(NO3)2(C12H8N2)2]

M = 1223.54

Triclinic,

a = 8.8852 (3) Å

b = 9.7465 (3) Å

c = 11.1570 (3) Å

α = 109.427 (3)°

β = 99.019 (3)°

γ = 106.199 (3)°

V = 841.13 (4) Å3

Z = 1

Mo Kα radiation

μ = 10.54 mm−1

T = 100 K

0.20 × 0.15 × 0.10 mm

Data collection

Agilent SuperNova Dual diffractometer with an Atlas detector

Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010 ▶) T min = 0.227, T max = 0.419

12671 measured reflections

3899 independent reflections

3740 reflections with I > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.017

wR(F 2) = 0.038

S = 0.99

3899 reflections

235 parameters

H-atom parameters constrained

Δρmax = 0.84 e Å−3

Δρmin = −0.97 e Å−3

Data collection: CrysAlis PRO (Agilent, 2010 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812003595/hg5168sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812003595/hg5168Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pb2(C2Cl3O2)2(NO3)2(C12H8N2)2]	Z = 1
Mr = 1223.54	F(000) = 572
Triclinic, P1	Dx = 2.415 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.8852 (3) Å	Cell parameters from 9962 reflections
b = 9.7465 (3) Å	θ = 2.4–27.5°
c = 11.1570 (3) Å	µ = 10.54 mm−1
α = 109.427 (3)°	T = 100 K
β = 99.019 (3)°	Prism, colourless
γ = 106.199 (3)°	0.20 × 0.15 × 0.10 mm
V = 841.13 (4) Å3

Agilent SuperNova Dual diffractometer with an Atlas detector	3899 independent reflections
Radiation source: SuperNova (Mo) X-ray Source	3740 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.029
Detector resolution: 10.4041 pixels mm-1	θmax = 27.6°, θmin = 2.4°
ω scan	h = −11→11
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010)	k = −12→12
Tmin = 0.227, Tmax = 0.419	l = −14→14
12671 measured reflections

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)] = 0.017	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.038	H-atom parameters constrained
S = 0.99	w = 1/[σ2(Fo2) + (0.0188P)2] where P = (Fo2 + 2Fc2)/3
3899 reflections	(Δ/σ)max = 0.001
235 parameters	Δρmax = 0.84 e Å−3
0 restraints	Δρmin = −0.97 e Å−3

	x	y	z	Uiso*/Ueq
Pb	0.526354 (11)	0.321866 (10)	0.619700 (8)	0.00914 (4)
Cl1	1.10668 (9)	0.71315 (9)	0.63924 (7)	0.02148 (16)
Cl2	0.92529 (9)	0.85568 (8)	0.80608 (7)	0.01891 (15)
Cl3	0.89253 (10)	0.85230 (9)	0.54481 (7)	0.02467 (17)
O1	0.7927 (2)	0.5079 (2)	0.66123 (18)	0.0146 (4)
O2	0.6722 (3)	0.5436 (2)	0.4883 (2)	0.0231 (5)
O3	0.6734 (2)	0.1262 (2)	0.54516 (18)	0.0148 (4)
O4	0.5454 (2)	0.1386 (2)	0.36793 (18)	0.0157 (4)
O5	0.6385 (3)	−0.0491 (2)	0.35098 (19)	0.0167 (4)
N1	0.5609 (3)	0.5650 (3)	0.8223 (2)	0.0112 (5)
N2	0.6794 (3)	0.3366 (3)	0.8360 (2)	0.0115 (5)
N3	0.6188 (3)	0.0712 (3)	0.4200 (2)	0.0115 (5)
C1	0.5074 (3)	0.6760 (3)	0.8136 (3)	0.0131 (6)
H1	0.4390	0.6586	0.7314	0.016*
C2	0.5473 (4)	0.8182 (3)	0.9205 (3)	0.0163 (6)
H2	0.5091	0.8964	0.9098	0.020*
C3	0.6421 (4)	0.8433 (3)	1.0406 (3)	0.0152 (6)
H3	0.6673	0.9378	1.1147	0.018*
C4	0.7023 (3)	0.7275 (3)	1.0538 (3)	0.0115 (5)
C5	0.6586 (3)	0.5890 (3)	0.9403 (3)	0.0111 (5)
C6	0.7343 (3)	0.2258 (3)	0.8442 (3)	0.0120 (5)
H6	0.7036	0.1326	0.7676	0.014*
C7	0.8356 (4)	0.2399 (3)	0.9606 (3)	0.0154 (6)
H7	0.8731	0.1580	0.9619	0.018*
C8	0.8803 (3)	0.3727 (3)	1.0725 (3)	0.0150 (6)
H8	0.9508	0.3849	1.1517	0.018*
C9	0.8205 (3)	0.4908 (3)	1.0688 (3)	0.0113 (5)
C10	0.7198 (3)	0.4687 (3)	0.9475 (2)	0.0098 (5)
C11	0.8037 (4)	0.7453 (3)	1.1749 (3)	0.0151 (6)
H11	0.8318	0.8382	1.2512	0.018*
C12	0.8606 (3)	0.6330 (3)	1.1830 (3)	0.0147 (6)
H12	0.9277	0.6478	1.2648	0.018*
C13	0.7796 (3)	0.5824 (3)	0.5894 (3)	0.0123 (6)
C14	0.9201 (3)	0.7446 (3)	0.6404 (3)	0.0142 (6)

	U11	U22	U33	U12	U13	U23
Pb	0.01030 (6)	0.00697 (6)	0.00857 (6)	0.00233 (4)	0.00028 (4)	0.00284 (4)
Cl1	0.0130 (3)	0.0269 (4)	0.0277 (4)	0.0043 (3)	0.0084 (3)	0.0157 (3)
Cl2	0.0239 (4)	0.0124 (3)	0.0149 (3)	0.0045 (3)	0.0009 (3)	0.0024 (3)
Cl3	0.0247 (4)	0.0209 (4)	0.0244 (4)	−0.0022 (3)	−0.0044 (3)	0.0178 (3)
O1	0.0157 (10)	0.0124 (10)	0.0149 (10)	0.0008 (8)	0.0043 (8)	0.0080 (8)
O2	0.0218 (12)	0.0128 (10)	0.0234 (11)	0.0013 (9)	−0.0097 (10)	0.0048 (9)
O3	0.0179 (11)	0.0173 (10)	0.0092 (9)	0.0073 (9)	0.0027 (8)	0.0047 (8)
O4	0.0187 (11)	0.0162 (10)	0.0154 (10)	0.0073 (9)	0.0038 (9)	0.0096 (8)
O5	0.0240 (11)	0.0096 (10)	0.0192 (10)	0.0078 (9)	0.0125 (9)	0.0043 (8)
N1	0.0115 (11)	0.0115 (11)	0.0106 (11)	0.0035 (9)	0.0022 (9)	0.0051 (9)
N2	0.0137 (12)	0.0088 (11)	0.0123 (11)	0.0039 (9)	0.0031 (10)	0.0046 (9)
N3	0.0120 (12)	0.0096 (11)	0.0135 (12)	0.0014 (9)	0.0063 (10)	0.0061 (9)
C1	0.0163 (14)	0.0149 (14)	0.0111 (13)	0.0092 (12)	0.0054 (11)	0.0053 (11)
C2	0.0230 (16)	0.0137 (14)	0.0165 (14)	0.0109 (12)	0.0077 (13)	0.0065 (11)
C3	0.0193 (15)	0.0109 (13)	0.0146 (14)	0.0046 (12)	0.0073 (12)	0.0033 (11)
C4	0.0130 (14)	0.0123 (13)	0.0107 (13)	0.0041 (11)	0.0055 (11)	0.0055 (10)
C5	0.0105 (13)	0.0116 (13)	0.0122 (13)	0.0013 (11)	0.0053 (11)	0.0069 (10)
C6	0.0144 (14)	0.0098 (13)	0.0111 (13)	0.0039 (11)	0.0027 (11)	0.0040 (10)
C7	0.0193 (15)	0.0144 (14)	0.0171 (14)	0.0081 (12)	0.0051 (12)	0.0101 (11)
C8	0.0170 (15)	0.0187 (15)	0.0131 (14)	0.0077 (12)	0.0035 (12)	0.0100 (11)
C9	0.0107 (13)	0.0125 (13)	0.0095 (13)	0.0025 (11)	0.0017 (11)	0.0047 (10)
C10	0.0096 (13)	0.0101 (13)	0.0101 (12)	0.0026 (10)	0.0041 (11)	0.0046 (10)
C11	0.0187 (15)	0.0121 (14)	0.0107 (13)	0.0036 (12)	0.0042 (12)	0.0015 (11)
C12	0.0125 (14)	0.0172 (14)	0.0095 (13)	0.0028 (11)	0.0003 (11)	0.0028 (11)
C13	0.0119 (14)	0.0110 (13)	0.0143 (14)	0.0045 (11)	0.0061 (12)	0.0038 (11)
C14	0.0124 (14)	0.0161 (14)	0.0145 (14)	0.0033 (11)	0.0018 (11)	0.0091 (11)

Pb—O1	2.410 (2)	C1—H1	0.9500
Pb—O2i	2.821 (2)	C2—C3	1.371 (4)
Pb—O3	2.591 (2)	C2—H2	0.9500
Pb—O4	2.844 (2)	C3—C4	1.415 (4)
Pb—O5ii	2.807 (2)	C3—H3	0.9500
Pb—N1	2.576 (2)	C4—C5	1.412 (4)
Pb—N2	2.515 (2)	C4—C11	1.429 (4)
Cl1—C14	1.770 (3)	C5—C10	1.442 (4)
Cl2—C14	1.790 (3)	C6—C7	1.401 (4)
Cl3—C14	1.762 (3)	C6—H6	0.9500
O1—C13	1.260 (3)	C7—C8	1.369 (4)
O2—C13	1.226 (3)	C7—H7	0.9500
O3—N3	1.272 (3)	C8—C9	1.405 (4)
O4—N3	1.252 (3)	C8—H8	0.9500
O5—N3	1.247 (3)	C9—C10	1.413 (4)
N1—C1	1.322 (3)	C9—C12	1.442 (4)
N1—C5	1.366 (3)	C11—C12	1.350 (4)
N2—C6	1.326 (3)	C11—H11	0.9500
N2—C10	1.368 (3)	C12—H12	0.9500
C1—C2	1.401 (4)	C13—C14	1.568 (4)
O1—Pb—N2	77.20 (7)	C2—C3—C4	119.6 (2)
O1—Pb—N1	73.51 (7)	C2—C3—H3	120.2
N2—Pb—N1	65.43 (7)	C4—C3—H3	120.2
O1—Pb—O3	82.13 (6)	C5—C4—C3	117.2 (2)
N2—Pb—O3	77.41 (6)	C5—C4—C11	119.6 (2)
N1—Pb—O3	138.96 (6)	C3—C4—C11	123.2 (2)
O1—Pb—O5ii	143.59 (6)	N1—C5—C4	122.1 (2)
N2—Pb—O5ii	72.82 (7)	N1—C5—C10	118.4 (2)
N1—Pb—O5ii	110.82 (6)	C4—C5—C10	119.5 (2)
O3—Pb—O5ii	71.66 (6)	N2—C6—C7	123.0 (2)
O1—Pb—O2i	100.42 (6)	N2—C6—H6	118.5
N2—Pb—O2i	142.33 (6)	C7—C6—H6	118.5
N1—Pb—O2i	77.74 (6)	C8—C7—C6	119.4 (3)
O3—Pb—O2i	140.08 (6)	C8—C7—H7	120.3
O5ii—Pb—O2i	115.93 (6)	C6—C7—H7	120.3
O1—Pb—O4	90.38 (6)	C7—C8—C9	119.2 (2)
N2—Pb—O4	124.31 (6)	C7—C8—H8	120.4
N1—Pb—O4	159.41 (7)	C9—C8—H8	120.4
O3—Pb—O4	46.99 (5)	C8—C9—C10	118.1 (2)
O5ii—Pb—O4	89.76 (5)	C8—C9—C12	122.3 (2)
O2i—Pb—O4	93.09 (6)	C10—C9—C12	119.6 (2)
C13—O1—Pb	107.77 (17)	N2—C10—C9	121.8 (2)
N3—O3—Pb	101.84 (14)	N2—C10—C5	118.8 (2)
N3—O4—Pb	90.19 (14)	C9—C10—C5	119.3 (2)
C1—N1—C5	118.9 (2)	C12—C11—C4	121.5 (2)
C1—N1—Pb	123.02 (17)	C12—C11—H11	119.3
C5—N1—Pb	117.39 (16)	C4—C11—H11	119.3
C6—N2—C10	118.3 (2)	C11—C12—C9	120.6 (3)
C6—N2—Pb	122.22 (17)	C11—C12—H12	119.7
C10—N2—Pb	119.21 (16)	C9—C12—H12	119.7
O5—N3—O4	121.0 (2)	O2—C13—O1	128.1 (3)
O5—N3—O3	119.6 (2)	O2—C13—C14	118.2 (2)
O4—N3—O3	119.4 (2)	O1—C13—C14	113.8 (2)
N1—C1—C2	122.7 (2)	C13—C14—Cl3	113.04 (19)
N1—C1—H1	118.6	C13—C14—Cl1	108.31 (18)
C2—C1—H1	118.6	Cl3—C14—Cl1	109.62 (15)
C3—C2—C1	119.3 (3)	C13—C14—Cl2	108.31 (19)
C3—C2—H2	120.4	Cl3—C14—Cl2	107.89 (15)
C1—C2—H2	120.4	Cl1—C14—Cl2	109.62 (14)
N2—Pb—O1—C13	−162.22 (17)	C5—N1—C1—C2	0.3 (4)
N1—Pb—O1—C13	−94.40 (17)	Pb—N1—C1—C2	−170.2 (2)
O3—Pb—O1—C13	118.98 (17)	N1—C1—C2—C3	−1.8 (5)
O5ii—Pb—O1—C13	162.70 (14)	C1—C2—C3—C4	2.0 (4)
O2i—Pb—O1—C13	−20.64 (17)	C2—C3—C4—C5	−0.8 (4)
O4—Pb—O1—C13	72.57 (17)	C2—C3—C4—C11	179.0 (3)
O1—Pb—O3—N3	−105.10 (16)	C1—N1—C5—C4	1.0 (4)
N2—Pb—O3—N3	176.34 (16)	Pb—N1—C5—C4	172.0 (2)
N1—Pb—O3—N3	−158.57 (14)	C1—N1—C5—C10	−178.3 (2)
O5ii—Pb—O3—N3	100.50 (16)	Pb—N1—C5—C10	−7.3 (3)
O2i—Pb—O3—N3	−8.3 (2)	C3—C4—C5—N1	−0.7 (4)
O4—Pb—O3—N3	−7.15 (13)	C11—C4—C5—N1	179.4 (3)
O1—Pb—O4—N3	85.95 (15)	C3—C4—C5—C10	178.5 (2)
N2—Pb—O4—N3	11.24 (17)	C11—C4—C5—C10	−1.3 (4)
N1—Pb—O4—N3	123.84 (19)	C10—N2—C6—C7	−2.0 (4)
O3—Pb—O4—N3	7.11 (13)	Pb—N2—C6—C7	172.4 (2)
O5ii—Pb—O4—N3	−57.64 (15)	N2—C6—C7—C8	0.6 (4)
O2i—Pb—O4—N3	−173.59 (15)	C6—C7—C8—C9	1.3 (4)
O1—Pb—N1—C1	94.8 (2)	C7—C8—C9—C10	−1.8 (4)
N2—Pb—N1—C1	177.9 (2)	C7—C8—C9—C12	179.2 (3)
O3—Pb—N1—C1	150.9 (2)	C6—N2—C10—C9	1.5 (4)
O5ii—Pb—N1—C1	−123.5 (2)	Pb—N2—C10—C9	−173.1 (2)
O2i—Pb—N1—C1	−10.2 (2)	C6—N2—C10—C5	−179.0 (2)
O4—Pb—N1—C1	54.9 (3)	Pb—N2—C10—C5	6.4 (3)
O1—Pb—N1—C5	−75.88 (19)	C8—C9—C10—N2	0.4 (4)
N2—Pb—N1—C5	7.30 (18)	C12—C9—C10—N2	179.4 (2)
O3—Pb—N1—C5	−19.8 (2)	C8—C9—C10—C5	−179.1 (2)
O5ii—Pb—N1—C5	65.9 (2)	C12—C9—C10—C5	−0.1 (4)
O2i—Pb—N1—C5	179.2 (2)	N1—C5—C10—N2	0.7 (4)
O4—Pb—N1—C5	−115.7 (2)	C4—C5—C10—N2	−178.6 (2)
O1—Pb—N2—C6	−103.8 (2)	N1—C5—C10—C9	−179.7 (2)
N1—Pb—N2—C6	178.6 (2)	C4—C5—C10—C9	1.0 (4)
O3—Pb—N2—C6	−19.2 (2)	C5—C4—C11—C12	0.7 (4)
O5ii—Pb—N2—C6	55.2 (2)	C3—C4—C11—C12	−179.1 (3)
O2i—Pb—N2—C6	165.63 (18)	C4—C11—C12—C9	0.1 (4)
O4—Pb—N2—C6	−22.3 (2)	C8—C9—C12—C11	178.5 (3)
O1—Pb—N2—C10	70.51 (19)	C10—C9—C12—C11	−0.4 (4)
N1—Pb—N2—C10	−7.01 (18)	Pb—O1—C13—O2	−21.3 (3)
O3—Pb—N2—C10	155.2 (2)	Pb—O1—C13—C14	158.09 (17)
O5ii—Pb—N2—C10	−130.4 (2)	O2—C13—C14—Cl3	3.3 (3)
O2i—Pb—N2—C10	−20.0 (3)	O1—C13—C14—Cl3	−176.12 (19)
O4—Pb—N2—C10	152.07 (17)	O2—C13—C14—Cl1	−118.3 (2)
Pb—O4—N3—O5	167.5 (2)	O1—C13—C14—Cl1	62.2 (3)
Pb—O4—N3—O3	−12.2 (2)	O2—C13—C14—Cl2	122.8 (2)
Pb—O3—N3—O5	−165.96 (19)	O1—C13—C14—Cl2	−56.6 (3)
Pb—O3—N3—O4	13.7 (3)

Table 1

Selected bond lengths (Å)

Pb—O1	2.410 (2)
Pb—O2i	2.821 (2)
Pb—O3	2.591 (2)
Pb—O4	2.844 (2)
Pb—O5ii	2.807 (2)
Pb—N1	2.576 (2)
Pb—N2	2.515 (2)

Symmetry codes: (i) ; (ii) .