Between MOFs and mol­ecules: organolead(IV) compounds with chain structures

Organolead compounds are of inter­est mainly as catalysts and organolead halides have proved to be very efficient materials for solar cells. Two organolead(IV) di­methyl­arsinates, namely catena-poly[[tri­phenyl­lead(IV)]-μ-chlorido-[tri­phenyl­lead(IV)]-μ-di­methyl­arsinato-κ²O:O′], [Pb₂(C₆H₅)₆(C₂H₆AsO₂)Cl]_n or [(Ph₃Pb)₂Cl(O₂AsMe₂)], (1), and poly[chlorido­(μ₃-di­methyl­arsinato-κ³O:O,O′:O′)di­phenyl­lead(IV)], [Pb(C₆H₅)₂(C₂H₆AsO₂)Cl]_n or [(Ph₂ClPb)(O₂AsMe₂)], (2), together with the tri­phenyl­lead(IV) di­phenyl­phosphinate catena-poly[[tri­phenyl­lead(IV)]-μ-di­phenyl­phosphinato-κ²O:O′], [Pb(C₆H₅)₃(C₁₂H₁₀O₂P)]_n or [(Ph₃Pb)(O₂PPh₂)], (3), have been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and mass spectrometry. In (1), a chain structure was found with alternating chloride and Pb—O—As—O—Pb arsinate bridges between five-coordinate Pb^IV atoms. In (2), bidentate and chelate-like bonded di­methyl­arsinate ligands form double chains with heptacoordinated Pb^IV atoms. In (3), a pentacoordinated Pb^IV atom is connected by Pb—O—P—O—Pb phosphinate bridges to form a linear chain. Obviously, the steric demand of the phenyl ligands at Pb^IV reduces the possibility of inter­connections via polydentate ligands to one dimension only. Thus, no metal–organic frameworks (MOF) are formed but instead various chain structures are observed.

Computing details

For all structures, data collection: X-AREA (Stoe & Cie, 2013); cell refinement: X-AREA (Stoe & Cie, 2013); data reduction: X-AREA (Stoe & Cie, 2013). Program(s) used to solve structure: SHELXS97 (Sheldrick, 2008) for (1), (3); SIR2011 (Burla et al., 2012) for (2). Program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015) for (1), (3); SHELXL97 (Sheldrick, 2008) for (2). For all structures, molecular graphics: DIAMOND (Brandenburg, 2016).

catena-Poly[[triphenyllead(IV)]-µ-chlorido-[triphenyllead(IV)]-µ-dimethylarsinato-κ²O:O'] (1)

Crystal data

[Pb2(C6H5)6(C2H6AsO2)Cl]	Dx = 1.955 Mg m^−3
Mr = 1049.42	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbca	Cell parameters from 9292 reflections
a = 19.0566 (8) Å	θ = 2.0–26.1°
b = 15.5255 (10) Å	µ = 10.46 mm^−1
c = 24.0975 (14) Å	T = 153 K
V = 7129.6 (7) Å^3	Block, colourless
Z = 8	0.16 × 0.12 × 0.09 mm
F(000) = 3952

Data collection

Stoe IPDS 2 diffractometer	6273 independent reflections
Radiation source: fine-focus sealed tube	4712 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.076
Detector resolution: 6.7 pixels mm^-1	θmax = 25.0°, θmin = 1.9°
ω scans	h = −20→22
Absorption correction: gaussian (Coppens et al., 1965)	k = −18→18
Tmin = 0.383, Tmax = 0.585	l = −25→28
41656 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.040	H-atom parameters constrained
wR(F^2) = 0.079	w = 1/[σ^2(Fo^2) + (0.036P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
6273 reflections	Δρmax = 2.64 e Å^−3
325 parameters	Δρmin = −1.31 e Å^−3

Special details

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. All phenyl rings were refined as idealized rigid groups (AFIX 66)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.21533 (2)	0.25344 (2)	0.08898 (2)	0.02170 (8)
Pb2	0.24676 (2)	0.33066 (2)	0.31934 (2)	0.02138 (8)
As1	0.19577 (4)	0.12320 (5)	−0.03722 (4)	0.02216 (19)
Cl1	0.24679 (12)	0.29385 (13)	0.19868 (8)	0.0268 (4)
O1	0.2518 (3)	0.1413 (4)	−0.0892 (2)	0.0285 (13)
O2	0.1834 (3)	0.2131 (3)	−0.0004 (3)	0.0273 (13)
C1	0.3288 (2)	0.2547 (4)	0.0685 (2)	0.030 (2)
C2	0.3801 (3)	0.2420 (4)	0.10865 (18)	0.0283 (19)
H2	0.3669	0.2314	0.1461	0.034*
C3	0.4507 (2)	0.2448 (4)	0.0941 (2)	0.039 (2)
H3	0.4857	0.2361	0.1216	0.047*
C4	0.4699 (2)	0.2602 (4)	0.0394 (3)	0.041 (3)
H4	0.5181	0.2621	0.0294	0.049*
C5	0.4186 (3)	0.2730 (4)	−0.0008 (2)	0.043 (3)
H5	0.4318	0.2836	−0.0382	0.052*
C6	0.3481 (3)	0.2702 (4)	0.0137 (2)	0.035 (2)
H6	0.3130	0.2789	−0.0137	0.042*
C7	0.1587 (3)	0.1393 (3)	0.1192 (3)	0.0243 (19)
C8	0.1921 (2)	0.0757 (3)	0.1500 (3)	0.033 (2)
H8	0.2388	0.0843	0.1625	0.040*
C9	0.1570 (3)	−0.0003 (3)	0.1626 (3)	0.040 (3)
H9	0.1799	−0.0438	0.1837	0.048*
C10	0.0886 (3)	−0.0128 (3)	0.1443 (3)	0.045 (3)
H10	0.0647	−0.0648	0.1529	0.054*
C11	0.0552 (3)	0.0508 (4)	0.1135 (3)	0.047 (3)
H11	0.0084	0.0423	0.1010	0.057*
C12	0.0902 (3)	0.1269 (3)	0.1009 (3)	0.035 (2)
H12	0.0674	0.1703	0.0798	0.042*
C13	0.1551 (3)	0.3738 (3)	0.0779 (2)	0.0219 (18)
C14	0.1211 (3)	0.3876 (3)	0.0277 (2)	0.0252 (19)
H14	0.1237	0.3456	−0.0009	0.030*
C15	0.0832 (3)	0.4630 (3)	0.01919 (19)	0.029 (2)
H15	0.0600	0.4724	−0.0152	0.035*
C16	0.0793 (3)	0.5246 (3)	0.0610 (2)	0.031 (2)
H16	0.0534	0.5761	0.0551	0.038*
C17	0.1133 (3)	0.5108 (3)	0.1112 (2)	0.032 (2)
H17	0.1107	0.5528	0.1398	0.039*
C18	0.1512 (3)	0.4354 (3)	0.11970 (18)	0.027 (2)
H18	0.1744	0.4260	0.1540	0.033*
C19	0.1776 (3)	0.2159 (3)	0.3269 (2)	0.0244 (19)
C20	0.1786 (3)	0.1660 (4)	0.3748 (2)	0.035 (2)
H20	0.2085	0.1813	0.4047	0.042*
C21	0.1357 (3)	0.0938 (3)	0.3789 (2)	0.037 (2)
H21	0.1364	0.0598	0.4116	0.044*
C22	0.0919 (3)	0.0715 (3)	0.3351 (3)	0.036 (2)
H22	0.0626	0.0222	0.3379	0.043*
C23	0.0909 (3)	0.1214 (4)	0.2872 (2)	0.035 (2)
H23	0.0610	0.1061	0.2572	0.042*
C24	0.1338 (3)	0.1936 (3)	0.2831 (2)	0.030 (2)
H24	0.1331	0.2276	0.2503	0.036*
C25	0.36245 (19)	0.3285 (4)	0.3184 (2)	0.0241 (18)
C26	0.3991 (3)	0.3391 (4)	0.36779 (18)	0.0277 (19)
H26	0.3743	0.3488	0.4014	0.033*
C27	0.4719 (3)	0.3355 (4)	0.3680 (2)	0.034 (2)
H27	0.4970	0.3428	0.4018	0.041*
C28	0.50821 (19)	0.3213 (4)	0.3188 (2)	0.032 (2)
H28	0.5580	0.3189	0.3190	0.038*
C29	0.4716 (3)	0.3107 (4)	0.2694 (2)	0.032 (2)
H29	0.4964	0.3010	0.2358	0.039*
C30	0.3987 (3)	0.3143 (4)	0.26917 (18)	0.0255 (19)
H30	0.3737	0.3070	0.2354	0.031*
C31	0.1862 (3)	0.4447 (3)	0.2943 (3)	0.0227 (18)
C32	0.1144 (3)	0.4337 (3)	0.2871 (3)	0.031 (2)
H32	0.0936	0.3790	0.2937	0.037*
C33	0.0730 (2)	0.5026 (3)	0.2703 (3)	0.031 (2)
H33	0.0239	0.4951	0.2654	0.037*
C34	0.1034 (3)	0.5826 (3)	0.2607 (3)	0.034 (2)
H34	0.0751	0.6297	0.2492	0.040*
C35	0.1752 (3)	0.5937 (3)	0.2679 (3)	0.035 (2)
H35	0.1960	0.6484	0.2613	0.042*
C36	0.2166 (2)	0.5247 (3)	0.2847 (3)	0.031 (2)
H36	0.2657	0.5323	0.2897	0.037*
C37	0.2334 (5)	0.0304 (6)	0.0061 (4)	0.038 (2)
H37A	0.2019	0.0182	0.0372	0.046*
H37B	0.2797	0.0467	0.0203	0.046*
H37C	0.2378	−0.0210	−0.0172	0.046*
C38	0.1081 (5)	0.0862 (7)	−0.0660 (4)	0.038 (2)
H38A	0.0754	0.0758	−0.0353	0.045*
H38B	0.1146	0.0328	−0.0871	0.045*
H38C	0.0889	0.1308	−0.0905	0.045*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.02607 (15)	0.01689 (13)	0.02215 (16)	−0.00096 (13)	0.00054 (14)	−0.00002 (14)
Pb2	0.02182 (15)	0.02003 (14)	0.02229 (16)	−0.00047 (13)	−0.00117 (15)	0.00149 (12)
As1	0.0255 (4)	0.0188 (4)	0.0222 (5)	0.0005 (3)	0.0000 (4)	−0.0010 (3)
Cl1	0.0306 (11)	0.0259 (9)	0.0239 (11)	0.0011 (9)	−0.0014 (10)	−0.0007 (8)
O1	0.028 (3)	0.036 (3)	0.023 (3)	−0.001 (3)	0.002 (3)	−0.001 (2)
O2	0.039 (3)	0.019 (3)	0.024 (3)	0.003 (3)	0.000 (3)	−0.005 (2)
C1	0.038 (5)	0.016 (4)	0.036 (5)	0.000 (4)	−0.003 (4)	−0.009 (4)
C2	0.026 (4)	0.027 (4)	0.031 (5)	0.002 (4)	0.001 (4)	−0.002 (4)
C3	0.025 (5)	0.036 (5)	0.057 (7)	0.000 (4)	−0.006 (4)	−0.014 (5)
C4	0.031 (5)	0.032 (5)	0.060 (8)	−0.006 (4)	0.013 (5)	−0.021 (5)
C5	0.046 (6)	0.040 (6)	0.044 (7)	−0.013 (5)	0.012 (5)	−0.007 (5)
C6	0.037 (5)	0.034 (6)	0.034 (6)	−0.006 (4)	0.005 (4)	−0.001 (4)
C7	0.027 (5)	0.020 (4)	0.025 (5)	−0.003 (3)	0.008 (4)	0.003 (3)
C8	0.032 (5)	0.021 (4)	0.047 (6)	0.002 (4)	0.006 (4)	0.001 (4)
C9	0.053 (7)	0.025 (5)	0.043 (7)	0.003 (4)	0.005 (5)	0.012 (4)
C10	0.049 (7)	0.031 (5)	0.056 (8)	−0.019 (5)	0.005 (6)	−0.005 (5)
C11	0.036 (6)	0.043 (6)	0.063 (8)	−0.018 (5)	−0.005 (5)	0.005 (5)
C12	0.034 (5)	0.031 (5)	0.040 (6)	−0.003 (4)	−0.006 (5)	0.007 (4)
C13	0.023 (4)	0.019 (4)	0.024 (5)	0.000 (3)	0.004 (4)	0.001 (3)
C14	0.020 (4)	0.024 (4)	0.031 (5)	−0.004 (3)	−0.001 (4)	−0.005 (4)
C15	0.027 (5)	0.032 (5)	0.029 (6)	0.008 (4)	0.000 (4)	−0.003 (4)
C16	0.028 (5)	0.028 (5)	0.038 (6)	0.010 (4)	−0.006 (4)	0.000 (4)
C17	0.036 (6)	0.027 (5)	0.033 (6)	0.001 (4)	0.002 (5)	−0.003 (4)
C18	0.026 (5)	0.031 (5)	0.025 (5)	−0.002 (4)	0.006 (4)	−0.001 (4)
C19	0.020 (4)	0.023 (4)	0.030 (6)	−0.002 (3)	0.001 (4)	0.008 (4)
C20	0.048 (6)	0.033 (5)	0.024 (5)	−0.007 (5)	−0.001 (4)	−0.003 (4)
C21	0.059 (7)	0.024 (5)	0.028 (6)	−0.015 (4)	0.009 (5)	0.003 (4)
C22	0.036 (5)	0.024 (5)	0.047 (7)	−0.009 (4)	0.012 (5)	0.000 (4)
C23	0.027 (5)	0.031 (5)	0.046 (7)	−0.011 (4)	−0.008 (4)	−0.008 (4)
C24	0.028 (5)	0.030 (5)	0.032 (6)	0.000 (4)	−0.003 (4)	0.005 (4)
C25	0.035 (5)	0.016 (4)	0.022 (5)	−0.003 (3)	−0.004 (4)	0.003 (3)
C26	0.027 (5)	0.029 (5)	0.027 (5)	0.001 (4)	−0.001 (4)	−0.001 (4)
C27	0.029 (5)	0.039 (5)	0.034 (6)	−0.002 (4)	−0.009 (4)	0.004 (4)
C28	0.022 (4)	0.034 (5)	0.040 (6)	0.000 (4)	−0.001 (4)	0.005 (4)
C29	0.031 (5)	0.033 (5)	0.032 (6)	−0.008 (4)	0.007 (4)	−0.001 (4)
C30	0.027 (5)	0.022 (4)	0.027 (5)	−0.003 (3)	0.001 (4)	−0.001 (4)
C31	0.026 (5)	0.019 (4)	0.023 (5)	0.005 (3)	−0.004 (4)	−0.001 (3)
C32	0.032 (5)	0.021 (5)	0.038 (6)	0.006 (4)	0.000 (4)	0.001 (4)
C33	0.028 (5)	0.031 (5)	0.034 (6)	0.000 (4)	0.001 (4)	0.002 (4)
C34	0.036 (5)	0.022 (4)	0.042 (6)	0.009 (4)	−0.008 (4)	−0.001 (4)
C35	0.034 (5)	0.017 (4)	0.054 (7)	−0.003 (4)	−0.003 (5)	0.005 (4)
C36	0.024 (5)	0.032 (5)	0.038 (6)	0.001 (4)	−0.003 (4)	0.004 (4)
C37	0.040 (6)	0.041 (5)	0.033 (6)	0.008 (4)	0.004 (4)	0.012 (4)
C38	0.036 (6)	0.043 (6)	0.035 (6)	0.004 (5)	0.004 (4)	−0.011 (5)

Geometric parameters (Å, º)

Pb1—C7	2.199 (4)	C16—H16	0.9500
Pb1—C13	2.210 (4)	C17—C18	1.3900
Pb1—C1	2.219 (4)	C17—H17	0.9500
Pb1—O2	2.323 (6)	C18—H18	0.9500
Pb1—Cl1	2.782 (2)	C19—C20	1.3900
Pb2—C31	2.198 (4)	C19—C24	1.3900
Pb2—C25	2.205 (4)	C20—C21	1.3900
Pb2—C19	2.224 (4)	C20—H20	0.9500
Pb2—O1^i	2.248 (6)	C21—C22	1.3900
Pb2—Cl1	2.963 (2)	C21—H21	0.9500
As1—O1	1.670 (6)	C22—C23	1.3900
As1—O2	1.672 (5)	C22—H22	0.9500
As1—C38	1.898 (10)	C23—C24	1.3900
As1—C37	1.918 (9)	C23—H23	0.9500
O1—Pb2^ii	2.248 (6)	C24—H24	0.9500
C1—C2	1.3900	C25—C26	1.3900
C1—C6	1.3900	C25—C30	1.3900
C2—C3	1.3900	C26—C27	1.3900
C2—H2	0.9500	C26—H26	0.9500
C3—C4	1.3900	C27—C28	1.3900
C3—H3	0.9500	C27—H27	0.9500
C4—C5	1.3900	C28—C29	1.3900
C4—H4	0.9500	C28—H28	0.9500
C5—C6	1.3900	C29—C30	1.3900
C5—H5	0.9500	C29—H29	0.9500
C6—H6	0.9500	C30—H30	0.9500
C7—C8	1.3900	C31—C32	1.3900
C7—C12	1.3900	C31—C36	1.3900
C8—C9	1.3900	C32—C33	1.3900
C8—H8	0.9500	C32—H32	0.9500
C9—C10	1.3900	C33—C34	1.3900
C9—H9	0.9500	C33—H33	0.9500
C10—C11	1.3900	C34—C35	1.3900
C10—H10	0.9500	C34—H34	0.9500
C11—C12	1.3900	C35—C36	1.3900
C11—H11	0.9500	C35—H35	0.9500
C12—H12	0.9500	C36—H36	0.9500
C13—C14	1.3900	C37—H37A	0.9800
C13—C18	1.3900	C37—H37B	0.9800
C14—C15	1.3900	C37—H37C	0.9800
C14—H14	0.9500	C38—H38A	0.9800
C15—C16	1.3900	C38—H38B	0.9800
C15—H15	0.9500	C38—H38C	0.9800
C16—C17	1.3900
C7—Pb1—C13	117.8 (2)	C17—C16—H16	120.0
C7—Pb1—C1	124.0 (2)	C15—C16—H16	120.0
C13—Pb1—C1	118.2 (2)	C18—C17—C16	120.0
C7—Pb1—O2	87.8 (2)	C18—C17—H17	120.0
C13—Pb1—O2	88.86 (19)	C16—C17—H17	120.0
C1—Pb1—O2	92.9 (2)	C17—C18—C13	120.0
C7—Pb1—Cl1	88.44 (17)	C17—C18—H18	120.0
C13—Pb1—Cl1	92.05 (14)	C13—C18—H18	120.0
C1—Pb1—Cl1	89.98 (15)	C20—C19—C24	120.0
O2—Pb1—Cl1	176.11 (16)	C20—C19—Pb2	120.4 (3)
C31—Pb2—C25	122.3 (2)	C24—C19—Pb2	119.6 (3)
C31—Pb2—C19	110.9 (2)	C19—C20—C21	120.0
C25—Pb2—C19	125.5 (2)	C19—C20—H20	120.0
C31—Pb2—O1^i	97.8 (2)	C21—C20—H20	120.0
C25—Pb2—O1^i	88.3 (2)	C20—C21—C22	120.0
C19—Pb2—O1^i	95.7 (2)	C20—C21—H21	120.0
C31—Pb2—Cl1	83.49 (18)	C22—C21—H21	120.0
C25—Pb2—Cl1	89.22 (14)	C23—C22—C21	120.0
C19—Pb2—Cl1	85.75 (15)	C23—C22—H22	120.0
O1^i—Pb2—Cl1	177.54 (17)	C21—C22—H22	120.0
O1—As1—O2	110.4 (3)	C22—C23—C24	120.0
O1—As1—C38	109.9 (4)	C22—C23—H23	120.0
O2—As1—C38	108.9 (4)	C24—C23—H23	120.0
O1—As1—C37	107.2 (4)	C23—C24—C19	120.0
O2—As1—C37	113.0 (4)	C23—C24—H24	120.0
C38—As1—C37	107.5 (5)	C19—C24—H24	120.0
Pb1—Cl1—Pb2	167.35 (9)	C26—C25—C30	120.0
As1—O1—Pb2^ii	137.8 (4)	C26—C25—Pb2	119.4 (3)
As1—O2—Pb1	132.9 (3)	C30—C25—Pb2	120.6 (3)
C2—C1—C6	120.0	C27—C26—C25	120.0
C2—C1—Pb1	121.9 (3)	C27—C26—H26	120.0
C6—C1—Pb1	118.1 (3)	C25—C26—H26	120.0
C3—C2—C1	120.0	C28—C27—C26	120.0
C3—C2—H2	120.0	C28—C27—H27	120.0
C1—C2—H2	120.0	C26—C27—H27	120.0
C2—C3—C4	120.0	C27—C28—C29	120.0
C2—C3—H3	120.0	C27—C28—H28	120.0
C4—C3—H3	120.0	C29—C28—H28	120.0
C5—C4—C3	120.0	C30—C29—C28	120.0
C5—C4—H4	120.0	C30—C29—H29	120.0
C3—C4—H4	120.0	C28—C29—H29	120.0
C6—C5—C4	120.0	C29—C30—C25	120.0
C6—C5—H5	120.0	C29—C30—H30	120.0
C4—C5—H5	120.0	C25—C30—H30	120.0
C5—C6—C1	120.0	C32—C31—C36	120.0
C5—C6—H6	120.0	C32—C31—Pb2	116.9 (3)
C1—C6—H6	120.0	C36—C31—Pb2	123.1 (3)
C8—C7—C12	120.0	C31—C32—C33	120.0
C8—C7—Pb1	121.6 (3)	C31—C32—H32	120.0
C12—C7—Pb1	117.9 (3)	C33—C32—H32	120.0
C9—C8—C7	120.0	C32—C33—C34	120.0
C9—C8—H8	120.0	C32—C33—H33	120.0
C7—C8—H8	120.0	C34—C33—H33	120.0
C8—C9—C10	120.0	C35—C34—C33	120.0
C8—C9—H9	120.0	C35—C34—H34	120.0
C10—C9—H9	120.0	C33—C34—H34	120.0
C11—C10—C9	120.0	C34—C35—C36	120.0
C11—C10—H10	120.0	C34—C35—H35	120.0
C9—C10—H10	120.0	C36—C35—H35	120.0
C12—C11—C10	120.0	C35—C36—C31	120.0
C12—C11—H11	120.0	C35—C36—H36	120.0
C10—C11—H11	120.0	C31—C36—H36	120.0
C11—C12—C7	120.0	As1—C37—H37A	109.5
C11—C12—H12	120.0	As1—C37—H37B	109.5
C7—C12—H12	120.0	H37A—C37—H37B	109.5
C14—C13—C18	120.0	As1—C37—H37C	109.5
C14—C13—Pb1	118.5 (3)	H37A—C37—H37C	109.5
C18—C13—Pb1	121.5 (3)	H37B—C37—H37C	109.5
C13—C14—C15	120.0	As1—C38—H38A	109.5
C13—C14—H14	120.0	As1—C38—H38B	109.5
C15—C14—H14	120.0	H38A—C38—H38B	109.5
C16—C15—C14	120.0	As1—C38—H38C	109.5
C16—C15—H15	120.0	H38A—C38—H38C	109.5
C14—C15—H15	120.0	H38B—C38—H38C	109.5
C17—C16—C15	120.0

Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2.

Poly[chlorido(µ₃-dimethylarsinato-κ³O:O,O':O')diphenyllead(IV)] (2)

Crystal data

[Pb(C6H5)2(C2H6AsO2)Cl]	F(000) = 992
Mr = 533.83	Dx = 2.375 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 7.3822 (3) Å	Cell parameters from 14717 reflections
b = 19.9500 (7) Å	θ = 2.0–27.2°
c = 10.2878 (4) Å	µ = 13.67 mm^−1
β = 99.763 (3)°	T = 100 K
V = 1493.19 (10) Å^3	Needle, colourless
Z = 4	0.26 × 0.03 × 0.03 mm

Data collection

Stoe IPDS/2T diffractometer	2934 independent reflections
Radiation source: fine-focus sealed tube	2116 reflections with I > 2σ(I)
Detector resolution: 6.7 pixels mm^-1	Rint = 0.094
ω–scans	θmax = 26.0°, θmin = 2.3°
Absorption correction: gaussian (Coppens et al., 1965)	h = −9→9
Tmin = 0.183, Tmax = 0.727	k = −24→24
21245 measured reflections	l = −12→12

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.067	w = 1/[σ^2(Fo^2) + (0.030P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max < 0.001
2934 reflections	Δρmax = 1.60 e Å^−3
173 parameters	Δρmin = −1.43 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00158 (14)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.72935 (3)	0.01889 (2)	0.39198 (3)	0.02132 (11)
Cl1	0.6838 (2)	0.06690 (10)	0.14258 (19)	0.0276 (4)
As1	0.80432 (8)	−0.02385 (4)	0.71823 (7)	0.02082 (17)
O1	0.9474 (6)	−0.0265 (3)	0.6067 (5)	0.0233 (11)
O2	0.6000 (6)	−0.0103 (3)	0.6226 (5)	0.0254 (12)
C1	0.7357 (9)	0.1241 (3)	0.4576 (7)	0.0196 (15)
C2	0.6534 (9)	0.1432 (4)	0.5607 (8)	0.0256 (17)
H2	0.5920	0.1112	0.6061	0.031*
C3	0.6607 (10)	0.2101 (4)	0.5982 (9)	0.0303 (19)
H3	0.6047	0.2241	0.6703	0.036*
C4	0.7498 (10)	0.2567 (4)	0.5307 (8)	0.0295 (19)
H4	0.7560	0.3023	0.5574	0.035*
C5	0.8295 (10)	0.2366 (4)	0.4244 (9)	0.0294 (18)
H5	0.8886	0.2687	0.3777	0.035*
C6	0.8233 (10)	0.1696 (4)	0.3858 (8)	0.0245 (17)
H6	0.8770	0.1553	0.3129	0.029*
C7	0.7202 (9)	−0.0825 (4)	0.3123 (8)	0.0220 (16)
C8	0.6264 (9)	−0.0917 (4)	0.1841 (8)	0.0233 (16)
H8	0.5636	−0.0554	0.1365	0.028*
C9	0.6262 (10)	−0.1551 (4)	0.1269 (9)	0.0288 (18)
H9	0.5657	−0.1619	0.0388	0.035*
C10	0.7132 (10)	−0.2074 (4)	0.1978 (9)	0.032 (2)
H10	0.7115	−0.2506	0.1587	0.038*
C11	0.8025 (10)	−0.1982 (4)	0.3244 (10)	0.034 (2)
H11	0.8621	−0.2352	0.3720	0.041*
C12	0.8073 (10)	−0.1359 (4)	0.3841 (9)	0.0269 (18)
H12	0.8688	−0.1298	0.4721	0.032*
C13	0.8766 (10)	0.0463 (4)	0.8386 (9)	0.032 (2)
H13A	0.9964	0.0357	0.8916	0.048*
H13B	0.7852	0.0516	0.8967	0.048*
H13C	0.8858	0.0881	0.7901	0.048*
C14	0.8019 (10)	−0.1056 (5)	0.8132 (9)	0.0326 (19)
H14A	0.9222	−0.1126	0.8684	0.049*
H14B	0.7751	−0.1429	0.7509	0.049*
H14C	0.7071	−0.1034	0.8692	0.049*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.01614 (13)	0.02184 (15)	0.02556 (16)	−0.00021 (13)	0.00230 (9)	−0.00146 (16)
Cl1	0.0293 (9)	0.0273 (10)	0.0250 (10)	−0.0023 (8)	0.0017 (8)	0.0001 (8)
As1	0.0145 (3)	0.0260 (4)	0.0216 (4)	0.0001 (3)	0.0019 (3)	0.0008 (4)
O1	0.013 (2)	0.031 (3)	0.025 (3)	−0.002 (2)	0.0040 (18)	−0.005 (3)
O2	0.009 (2)	0.031 (3)	0.034 (3)	0.001 (2)	−0.0024 (19)	−0.003 (3)
C1	0.022 (3)	0.014 (3)	0.022 (4)	0.001 (3)	0.000 (3)	−0.010 (3)
C2	0.018 (3)	0.023 (4)	0.035 (5)	0.004 (3)	0.004 (3)	−0.009 (4)
C3	0.021 (4)	0.035 (5)	0.035 (5)	0.003 (3)	0.002 (3)	−0.005 (4)
C4	0.025 (4)	0.023 (4)	0.037 (5)	0.003 (3)	−0.004 (3)	−0.007 (4)
C5	0.027 (4)	0.028 (4)	0.033 (5)	0.000 (3)	0.003 (3)	0.003 (4)
C6	0.025 (4)	0.023 (4)	0.025 (4)	−0.003 (3)	0.001 (3)	−0.003 (3)
C7	0.017 (3)	0.015 (4)	0.032 (5)	−0.002 (3)	−0.002 (3)	0.000 (3)
C8	0.024 (3)	0.025 (4)	0.022 (4)	−0.005 (3)	0.006 (3)	0.003 (3)
C9	0.025 (4)	0.030 (4)	0.031 (5)	−0.005 (3)	0.003 (3)	−0.002 (4)
C10	0.025 (4)	0.025 (4)	0.044 (5)	0.001 (3)	0.000 (4)	−0.011 (4)
C11	0.024 (4)	0.024 (4)	0.051 (6)	0.004 (3)	0.000 (4)	−0.005 (4)
C12	0.019 (3)	0.031 (4)	0.029 (5)	0.002 (3)	−0.003 (3)	−0.001 (4)
C13	0.018 (3)	0.038 (5)	0.041 (5)	0.007 (3)	0.006 (3)	−0.001 (4)
C14	0.023 (4)	0.038 (5)	0.037 (5)	0.000 (3)	0.007 (3)	0.002 (4)

Geometric parameters (Å, º)

Pb1—C7	2.180 (7)	C5—C6	1.392 (11)
Pb1—C1	2.202 (7)	C5—H5	0.9500
Pb1—O1^i	2.389 (4)	C6—H6	0.9500
Pb1—O2^ii	2.416 (4)	C7—C12	1.390 (11)
Pb1—O1	2.662 (5)	C7—C8	1.394 (11)
Pb1—Cl1	2.706 (2)	C8—C9	1.394 (11)
As1—O2	1.678 (4)	C8—H8	0.9500
As1—O1	1.687 (5)	C9—C10	1.370 (12)
As1—C13	1.885 (9)	C9—H9	0.9500
As1—C14	1.902 (9)	C10—C11	1.368 (12)
O1—Pb1^i	2.389 (4)	C10—H10	0.9500
O2—Pb1^ii	2.416 (4)	C11—C12	1.385 (11)
C1—C2	1.363 (11)	C11—H11	0.9500
C1—C6	1.396 (11)	C12—H12	0.9500
C2—C3	1.389 (11)	C13—H13A	0.9800
C2—H2	0.9500	C13—H13B	0.9800
C3—C4	1.390 (12)	C13—H13C	0.9800
C3—H3	0.9500	C14—H14A	0.9800
C4—C5	1.386 (12)	C14—H14B	0.9800
C4—H4	0.9500	C14—H14C	0.9800
C7—Pb1—C1	175.8 (3)	C4—C5—C6	120.3 (8)
C7—Pb1—O1^i	91.6 (2)	C4—C5—H5	119.8
C1—Pb1—O1^i	88.2 (2)	C6—C5—H5	119.8
C7—Pb1—O2^ii	86.8 (2)	C5—C6—C1	118.0 (7)
C1—Pb1—O2^ii	93.2 (2)	C5—C6—H6	121.0
O1^i—Pb1—O2^ii	176.80 (18)	C1—C6—H6	121.0
C7—Pb1—O1	88.4 (2)	C12—C7—C8	120.9 (7)
C1—Pb1—O1	95.3 (2)	C12—C7—Pb1	122.0 (6)
O1^i—Pb1—O1	63.51 (19)	C8—C7—Pb1	117.2 (5)
O2^ii—Pb1—O1	119.20 (16)	C7—C8—C9	118.9 (7)
C7—Pb1—Cl1	88.9 (2)	C7—C8—H8	120.5
C1—Pb1—Cl1	86.9 (2)	C9—C8—H8	120.5
O1^i—Pb1—Cl1	86.92 (13)	C10—C9—C8	120.0 (8)
O2^ii—Pb1—Cl1	90.25 (13)	C10—C9—H9	120.0
O1—Pb1—Cl1	150.20 (10)	C8—C9—H9	120.0
O2—As1—O1	102.1 (2)	C11—C10—C9	120.7 (8)
O2—As1—C13	113.1 (3)	C11—C10—H10	119.6
O1—As1—C13	109.3 (3)	C9—C10—H10	119.6
O2—As1—C14	110.7 (3)	C10—C11—C12	121.0 (8)
O1—As1—C14	112.6 (3)	C10—C11—H11	119.5
C13—As1—C14	109.0 (4)	C12—C11—H11	119.5
As1—O1—Pb1^i	137.2 (3)	C11—C12—C7	118.5 (8)
As1—O1—Pb1	101.16 (19)	C11—C12—H12	120.7
Pb1^i—O1—Pb1	116.49 (19)	C7—C12—H12	120.7
As1—O2—Pb1^ii	145.1 (3)	As1—C13—H13A	109.5
C2—C1—C6	122.5 (7)	As1—C13—H13B	109.5
C2—C1—Pb1	121.0 (6)	H13A—C13—H13B	109.5
C6—C1—Pb1	116.5 (5)	As1—C13—H13C	109.5
C1—C2—C3	118.9 (8)	H13A—C13—H13C	109.5
C1—C2—H2	120.5	H13B—C13—H13C	109.5
C3—C2—H2	120.5	As1—C14—H14A	109.5
C2—C3—C4	120.2 (8)	As1—C14—H14B	109.5
C2—C3—H3	119.9	H14A—C14—H14B	109.5
C4—C3—H3	119.9	As1—C14—H14C	109.5
C5—C4—C3	120.1 (8)	H14A—C14—H14C	109.5
C5—C4—H4	120.0	H14B—C14—H14C	109.5
C3—C4—H4	120.0

Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+1, −y, −z+1.

catena-Poly[[triphenyllead(IV)]-µ-diphenylphosphinato-κ²O:O'] (3)

Crystal data

[Pb(C6H5)3(C12H10O2P)]	F(000) = 1272
Mr = 655.66	Dx = 1.740 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 13.8277 (8) Å	Cell parameters from 22205 reflections
b = 12.6242 (6) Å	θ = 1.9–27.1°
c = 14.4713 (8) Å	µ = 6.83 mm^−1
β = 97.717 (5)°	T = 100 K
V = 2503.3 (2) Å^3	Needle, colourless
Z = 4	0.11 × 0.04 × 0.02 mm

Data collection

Stoe IPDS/2T diffractometer	5316 independent reflections
Radiation source: fine-focus sealed tube	3301 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.095
Detector resolution: 6.7 pixels mm^-1	θmax = 26.9°, θmin = 1.9°
ω scans	h = −17→17
Absorption correction: gaussian (Coppens et al., 1965)	k = −15→15
Tmin = 0.376, Tmax = 0.917	l = −18→18
18698 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.101	H-atom parameters constrained
S = 0.91	w = 1/[σ^2(Fo^2) + (0.040P)^2] where P = (Fo^2 + 2Fc^2)/3
5316 reflections	(Δ/σ)max = 0.001
223 parameters	Δρmax = 2.58 e Å^−3
2 restraints	Δρmin = −2.17 e Å^−3

Special details

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. All phenyl rings refined using geometrical constraints (AFIX 66). Rotationally Disordered phenyl ring (C13—C18) refined with equal anisotropic displacement parameters for neighboring atoms. The occupations of both orientations were set 50:50% since refinement confirmed this ratio within the 3\s limit.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pb1	0.22665 (2)	0.84365 (2)	0.19550 (2)	0.03541 (10)
P1	0.15953 (16)	0.60620 (16)	0.31759 (15)	0.0343 (5)
O1	0.1699 (4)	0.6709 (4)	0.2329 (4)	0.0392 (13)
O2	0.2323 (4)	0.5195 (4)	0.3428 (4)	0.0399 (14)
C1	0.2631 (4)	0.7809 (4)	0.0635 (3)	0.038 (2)
C2	0.2790 (4)	0.8476 (3)	−0.0093 (3)	0.0361 (18)
H2	0.2700	0.9219	−0.0039	0.043*
C3	0.3081 (4)	0.8058 (4)	−0.0901 (3)	0.043 (2)
H3	0.3189	0.8515	−0.1398	0.052*
C4	0.3213 (4)	0.6972 (4)	−0.0980 (3)	0.049 (2)
H4	0.3411	0.6686	−0.1532	0.059*
C5	0.3054 (4)	0.6304 (3)	−0.0252 (4)	0.050 (2)
H5	0.3144	0.5562	−0.0306	0.060*
C6	0.2763 (4)	0.6722 (4)	0.0556 (3)	0.042 (2)
H6	0.2655	0.6266	0.1054	0.050*
C7	0.3428 (4)	0.8381 (4)	0.3127 (3)	0.0362 (18)
C8	0.4179 (5)	0.7649 (5)	0.3124 (4)	0.060 (3)
H8	0.4177	0.7172	0.2616	0.072*
C9	0.4932 (4)	0.7617 (5)	0.3863 (5)	0.075 (4)
H9	0.5446	0.7117	0.3860	0.090*
C10	0.4935 (4)	0.8316 (6)	0.4605 (4)	0.062 (3)
H10	0.5451	0.8294	0.5110	0.074*
C11	0.4185 (4)	0.9047 (5)	0.4609 (3)	0.052 (3)
H11	0.4187	0.9525	0.5116	0.062*
C12	0.3431 (4)	0.9080 (4)	0.3870 (4)	0.039 (2)
H12	0.2918	0.9580	0.3873	0.046*
C13A	0.0824 (5)	0.9098 (10)	0.2076 (9)	0.039 (2)*	0.5
C14A	0.0753 (5)	0.9735 (10)	0.2848 (8)	0.044 (3)*	0.5
H14A	0.1301	0.9819	0.3314	0.053*	0.5
C15A	−0.0118 (7)	1.0250 (9)	0.2937 (7)	0.044 (3)*	0.5
H15A	−0.0166	1.0686	0.3464	0.053*	0.5
C16A	−0.0919 (5)	1.0127 (9)	0.2255 (8)	0.041 (3)*	0.5
H16A	−0.1515	1.0479	0.2316	0.049*	0.5
C17A	−0.0849 (6)	0.9490 (9)	0.1484 (7)	0.044 (3)*	0.5
H17A	−0.1396	0.9406	0.1017	0.053*	0.5
C18A	0.0022 (7)	0.8975 (9)	0.1394 (7)	0.047 (3)*	0.5
H18A	0.0070	0.8540	0.0867	0.057*	0.5
C13B	0.0852 (5)	0.9165 (10)	0.1989 (9)	0.039 (2)*	0.5
C14B	0.0516 (7)	0.9464 (10)	0.2814 (7)	0.044 (3)*	0.5
H14B	0.0894	0.9313	0.3397	0.053*	0.5
C15B	−0.0374 (7)	0.9983 (9)	0.2786 (6)	0.044 (3)*	0.5
H15B	−0.0604	1.0187	0.3350	0.053*	0.5
C16B	−0.0927 (5)	1.0204 (9)	0.1934 (8)	0.041 (3)*	0.5
H16B	−0.1535	1.0559	0.1915	0.049*	0.5
C17B	−0.0591 (7)	0.9906 (9)	0.1109 (6)	0.044 (3)*	0.5
H17B	−0.0969	1.0057	0.0526	0.053*	0.5
C18B	0.0299 (7)	0.9387 (9)	0.1137 (7)	0.047 (3)*	0.5
H18B	0.0529	0.9183	0.0573	0.057*	0.5
C19	0.0383 (3)	0.5496 (4)	0.3019 (4)	0.0343 (18)
C20	0.0121 (4)	0.4842 (4)	0.3718 (3)	0.039 (2)
H20	0.0556	0.4747	0.4279	0.047*
C21	−0.0776 (4)	0.4328 (4)	0.3597 (4)	0.050 (2)
H21	−0.0954	0.3882	0.4074	0.060*
C22	−0.1411 (3)	0.4467 (5)	0.2776 (4)	0.051 (2)
H22	−0.2024	0.4116	0.2694	0.061*
C23	−0.1150 (4)	0.5120 (5)	0.2077 (3)	0.052 (3)
H23	−0.1584	0.5215	0.1517	0.063*
C24	−0.0253 (4)	0.5635 (4)	0.2199 (3)	0.043 (2)
H24	−0.0074	0.6081	0.1721	0.051*
C25	0.1655 (4)	0.6902 (4)	0.4197 (3)	0.036 (2)
C26	0.2498 (3)	0.6920 (4)	0.4838 (4)	0.043 (2)
H26	0.3042	0.6495	0.4740	0.052*
C27	0.2547 (3)	0.7561 (5)	0.5624 (3)	0.043 (2)
H27	0.3124	0.7574	0.6062	0.052*
C28	0.1752 (4)	0.8184 (4)	0.5768 (3)	0.047 (2)
H28	0.1785	0.8622	0.6305	0.056*
C29	0.0908 (4)	0.8165 (4)	0.5127 (4)	0.066 (3)
H29	0.0365	0.8591	0.5226	0.080*
C30	0.0860 (3)	0.7524 (4)	0.4341 (4)	0.056 (3)
H30	0.0283	0.7511	0.3903	0.067*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.04572 (18)	0.02277 (13)	0.03683 (16)	0.00280 (18)	0.00222 (11)	−0.00012 (17)
P1	0.0372 (12)	0.0240 (10)	0.0412 (12)	−0.0009 (9)	0.0034 (10)	0.0032 (9)
O1	0.049 (3)	0.024 (3)	0.047 (3)	0.002 (3)	0.017 (3)	0.007 (3)
O2	0.043 (3)	0.020 (3)	0.056 (4)	0.002 (2)	0.002 (3)	0.000 (3)
C1	0.042 (5)	0.025 (4)	0.045 (5)	−0.002 (4)	−0.004 (4)	0.002 (4)
C2	0.039 (4)	0.028 (4)	0.040 (4)	0.005 (4)	−0.002 (3)	−0.005 (4)
C3	0.046 (5)	0.042 (5)	0.041 (5)	0.004 (4)	0.005 (4)	0.010 (4)
C4	0.046 (5)	0.051 (5)	0.048 (5)	−0.003 (5)	0.000 (4)	−0.014 (5)
C5	0.055 (6)	0.033 (5)	0.063 (6)	−0.007 (4)	0.012 (5)	−0.010 (4)
C6	0.058 (5)	0.031 (5)	0.038 (4)	−0.003 (4)	0.012 (4)	0.001 (4)
C7	0.040 (4)	0.030 (4)	0.035 (4)	−0.003 (4)	−0.005 (3)	0.004 (4)
C8	0.063 (7)	0.062 (6)	0.055 (6)	0.034 (5)	0.010 (5)	0.000 (5)
C9	0.064 (7)	0.091 (9)	0.066 (7)	0.040 (7)	−0.003 (6)	0.019 (7)
C10	0.047 (6)	0.083 (8)	0.052 (6)	−0.009 (6)	−0.007 (5)	0.021 (6)
C11	0.048 (6)	0.063 (6)	0.041 (5)	−0.008 (5)	−0.006 (4)	0.005 (5)
C12	0.033 (5)	0.039 (5)	0.042 (5)	0.004 (4)	−0.002 (4)	−0.010 (4)
C19	0.039 (5)	0.028 (4)	0.036 (4)	−0.003 (4)	0.004 (4)	−0.001 (3)
C20	0.042 (5)	0.032 (4)	0.044 (5)	−0.004 (4)	0.006 (4)	−0.002 (4)
C21	0.058 (6)	0.034 (5)	0.056 (6)	−0.008 (4)	0.005 (5)	−0.004 (4)
C22	0.038 (5)	0.048 (6)	0.067 (6)	−0.009 (4)	0.008 (5)	−0.018 (5)
C23	0.044 (6)	0.062 (6)	0.050 (6)	0.003 (5)	−0.001 (4)	−0.012 (5)
C24	0.041 (5)	0.044 (5)	0.043 (5)	0.006 (4)	0.006 (4)	−0.001 (4)
C25	0.040 (5)	0.028 (4)	0.038 (4)	−0.004 (3)	−0.007 (4)	0.005 (3)
C26	0.041 (5)	0.050 (5)	0.038 (5)	0.002 (4)	0.002 (4)	0.007 (4)
C27	0.043 (5)	0.049 (5)	0.035 (5)	−0.006 (4)	−0.002 (4)	−0.005 (4)
C28	0.055 (6)	0.036 (5)	0.046 (5)	0.002 (4)	−0.003 (4)	−0.010 (4)
C29	0.060 (6)	0.048 (6)	0.085 (8)	0.020 (5)	−0.014 (6)	−0.023 (5)
C30	0.056 (6)	0.027 (4)	0.078 (7)	0.006 (4)	−0.011 (5)	−0.015 (5)

Geometric parameters (Å, º)

Pb1—C7	2.175 (4)	C16A—C17A	1.3900
Pb1—C13B	2.168 (4)	C16A—H16A	0.9500
Pb1—C13A	2.192 (4)	C17A—C18A	1.3900
Pb1—C1	2.189 (4)	C17A—H17A	0.9500
Pb1—O2^i	2.375 (5)	C18A—H18A	0.9500
Pb1—O1	2.404 (5)	C13B—C14B	1.3900
P1—O1	1.496 (6)	C13B—C18B	1.3900
P1—O2	1.499 (5)	C14B—C15B	1.3900
P1—C19	1.809 (4)	C14B—H14B	0.9500
P1—C25	1.811 (4)	C15B—C16B	1.3900
O2—Pb1^ii	2.375 (5)	C15B—H15B	0.9500
C1—C2	1.3900	C16B—C17B	1.3900
C1—C6	1.3900	C16B—H16B	0.9500
C2—C3	1.3900	C17B—C18B	1.3900
C2—H2	0.9500	C17B—H17B	0.9500
C3—C4	1.3900	C18B—H18B	0.9500
C3—H3	0.9500	C19—C20	1.3900
C4—C5	1.3900	C19—C24	1.3900
C4—H4	0.9500	C20—C21	1.3900
C5—C6	1.3900	C20—H20	0.9500
C5—H5	0.9500	C21—C22	1.3900
C6—H6	0.9500	C21—H21	0.9500
C7—C8	1.3900	C22—C23	1.3900
C7—C12	1.3900	C22—H22	0.9500
C8—C9	1.3900	C23—C24	1.3900
C8—H8	0.9500	C23—H23	0.9500
C9—C10	1.3900	C24—H24	0.9500
C9—H9	0.9500	C25—C26	1.3900
C10—C11	1.3900	C25—C30	1.3900
C10—H10	0.9500	C26—C27	1.3900
C11—C12	1.3900	C26—H26	0.9500
C11—H11	0.9500	C27—C28	1.3900
C12—H12	0.9500	C27—H27	0.9500
C13A—C14A	1.3900	C28—C29	1.3900
C13A—C18A	1.3900	C28—H28	0.9500
C14A—C15A	1.3900	C29—C30	1.3900
C14A—H14A	0.9500	C29—H29	0.9500
C15A—C16A	1.3900	C30—H30	0.9500
C15A—H15A	0.9500
C7—Pb1—C13B	124.7 (4)	C16A—C15A—H15A	120.0
C7—Pb1—C13A	122.3 (4)	C14A—C15A—H15A	120.0
C7—Pb1—C1	115.9 (2)	C15A—C16A—C17A	120.0
C13B—Pb1—C1	119.2 (4)	C15A—C16A—H16A	120.0
C13A—Pb1—C1	121.8 (4)	C17A—C16A—H16A	120.0
C7—Pb1—O2^i	92.2 (2)	C18A—C17A—C16A	120.0
C13B—Pb1—O2^i	81.6 (4)	C18A—C17A—H17A	120.0
C13A—Pb1—O2^i	84.9 (4)	C16A—C17A—H17A	120.0
C1—Pb1—O2^i	92.54 (19)	C17A—C18A—C13A	120.0
C7—Pb1—O1	91.4 (2)	C17A—C18A—H18A	120.0
C13B—Pb1—O1	93.3 (4)	C13A—C18A—H18A	120.0
C13A—Pb1—O1	90.0 (4)	C14B—C13B—C18B	120.0
C1—Pb1—O1	89.31 (18)	C14B—C13B—Pb1	122.8 (6)
O2^i—Pb1—O1	174.82 (18)	C18B—C13B—Pb1	117.1 (6)
O1—P1—O2	117.6 (4)	C15B—C14B—C13B	120.0
O1—P1—C19	107.6 (3)	C15B—C14B—H14B	120.0
O2—P1—C19	108.8 (3)	C13B—C14B—H14B	120.0
O1—P1—C25	110.5 (3)	C14B—C15B—C16B	120.0
O2—P1—C25	105.9 (3)	C14B—C15B—H15B	120.0
C19—P1—C25	105.9 (3)	C16B—C15B—H15B	120.0
P1—O1—Pb1	138.6 (3)	C15B—C16B—C17B	120.0
P1—O2—Pb1^ii	143.1 (3)	C15B—C16B—H16B	120.0
C2—C1—C6	120.0	C17B—C16B—H16B	120.0
C2—C1—Pb1	121.4 (3)	C16B—C17B—C18B	120.0
C6—C1—Pb1	118.5 (3)	C16B—C17B—H17B	120.0
C1—C2—C3	120.0	C18B—C17B—H17B	120.0
C1—C2—H2	120.0	C17B—C18B—C13B	120.0
C3—C2—H2	120.0	C17B—C18B—H18B	120.0
C4—C3—C2	120.0	C13B—C18B—H18B	120.0
C4—C3—H3	120.0	C20—C19—C24	120.0
C2—C3—H3	120.0	C20—C19—P1	118.1 (3)
C5—C4—C3	120.0	C24—C19—P1	121.8 (3)
C5—C4—H4	120.0	C21—C20—C19	120.0
C3—C4—H4	120.0	C21—C20—H20	120.0
C4—C5—C6	120.0	C19—C20—H20	120.0
C4—C5—H5	120.0	C22—C21—C20	120.0
C6—C5—H5	120.0	C22—C21—H21	120.0
C5—C6—C1	120.0	C20—C21—H21	120.0
C5—C6—H6	120.0	C23—C22—C21	120.0
C1—C6—H6	120.0	C23—C22—H22	120.0
C8—C7—C12	120.0	C21—C22—H22	120.0
C8—C7—Pb1	119.5 (3)	C22—C23—C24	120.0
C12—C7—Pb1	120.5 (3)	C22—C23—H23	120.0
C7—C8—C9	120.0	C24—C23—H23	120.0
C7—C8—H8	120.0	C23—C24—C19	120.0
C9—C8—H8	120.0	C23—C24—H24	120.0
C8—C9—C10	120.0	C19—C24—H24	120.0
C8—C9—H9	120.0	C26—C25—C30	120.0
C10—C9—H9	120.0	C26—C25—P1	119.8 (3)
C11—C10—C9	120.0	C30—C25—P1	120.2 (3)
C11—C10—H10	120.0	C25—C26—C27	120.0
C9—C10—H10	120.0	C25—C26—H26	120.0
C10—C11—C12	120.0	C27—C26—H26	120.0
C10—C11—H11	120.0	C28—C27—C26	120.0
C12—C11—H11	120.0	C28—C27—H27	120.0
C11—C12—C7	120.0	C26—C27—H27	120.0
C11—C12—H12	120.0	C29—C28—C27	120.0
C7—C12—H12	120.0	C29—C28—H28	120.0
C14A—C13A—C18A	120.0	C27—C28—H28	120.0
C14A—C13A—Pb1	116.6 (6)	C30—C29—C28	120.0
C18A—C13A—Pb1	123.2 (6)	C30—C29—H29	120.0
C13A—C14A—C15A	120.0	C28—C29—H29	120.0
C13A—C14A—H14A	120.0	C29—C30—C25	120.0
C15A—C14A—H14A	120.0	C29—C30—H30	120.0
C16A—C15A—C14A	120.0	C25—C30—H30	120.0

Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, −z+1/2.