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Acta Crystallogr Sect E Struct Rep Online. 2008 August 1; 64(Pt 8): m1055–m1056.
Published online 2008 July 23. doi:  10.1107/S1600536808022678
PMCID: PMC2961970

catena-Poly[μ-aqua-2:1′κ2 O:O-aqua-2κO-(2-fluoro­benzoato-1κ2 O,O′)(μ2-2-fluoro­benzoato-2′:1κ2 O:O′)bis­(μ3-2-fluoro­benzoato)-2′:1:2κ4 O:O,O′:O′;1:2:1′κ5 F,O:O,O′:O′-dilead(II)]

Abstract

In the title compound, [Pb2(C7H4FO2)4(H2O)2]n, one PbII atom is coordinated by seven O atoms and one F atom from five 2-fluoro­benzoate ligands, and the other PbII atom is coordinated by five O atoms from four 2-fluoro­benzoate ligands and three water mol­ecules, resulting in distorted PbO7F and PbO8 polyhedra. The 2-fluoro­benzoate ligands bridge Pb atoms, giving rise to a one-dimensional chain structure extending along the [100] direction. The polymeric chains are connected via C—H(...)O hydrogen bonds and π–π inter­actions, with an inter­planar distance of 3.46 (1) Å. An intramolecular O—H(...)F interaction is also present.

Related literature

For related literature, see: Morsali & Mahjoub (2005 [triangle]); Xiao & Morsali (2007 [triangle]); Zhang (2004 [triangle], 2005 [triangle], 2006a [triangle],b [triangle],c [triangle]); Zhang et al. (2005 [triangle]); Zhu et al. (1999 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1055-scheme1.jpg

Experimental

Crystal data

  • [Pb2(C7H4FO2)4(H2O)2]
  • M r = 1006.84
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1055-efi1.jpg
  • a = 7.1016 (14) Å
  • b = 14.794 (3) Å
  • c = 15.096 (3) Å
  • α = 111.56 (3)°
  • β = 95.32 (3)°
  • γ = 97.31 (3)°
  • V = 1446.2 (6) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 11.71 mm−1
  • T = 290 (2) K
  • 0.44 × 0.19 × 0.13 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.082, T max = 0.223
  • 14182 measured reflections
  • 6646 independent reflections
  • 5329 reflections with I > 2σ(I)
  • R int = 0.028

Refinement

  • R[F 2 > 2σ(F 2)] = 0.037
  • wR(F 2) = 0.094
  • S = 1.03
  • 6646 reflections
  • 397 parameters
  • 3 restraints
  • H-atom parameters constrained
  • Δρmax = 3.74 e Å−3
  • Δρmin = −2.48 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 [triangle]); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808022678/hy2143sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808022678/hy2143Isup2.hkl

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

Acknowledgments

The author gratefully acknowledges financial support from the Education Office of Zhejiang Province (grant No. 20051316).

supplementary crystallographic information

Comment

We have studied the metal complexes of halogen-substituted benzoic acid (X–C6H4COOH; X = F, Cl, Br and I) (Zhang, 2004, 2005; Zhang et al., 2005; Zhang, 2006a,b,c). The related crystal structures can be found, such as [Pb(phen)n(NO2)X] (phen = 1,10-phenanthroline; X = CH3COO-, NCS- and ClO4-) (Morsali & Mahjoub, 2005), [Pb3(bpy)(H2O)5(sip)2].0.5bpy.2H2O (sip = 5-sulfoisophthalate; bpy = 2,2'-bipyridine) (Xiao & Morsali, 2007) and PbI2(L) (L = bpy, phen) (Zhu et al., 1999). We report here the synthesis and structure of the title compound, a new one-dimensional PbII coordination polymer.

In the title compound, the Pb1 atom is coordinated by seven O atoms and one F atom from five 2-fluorobenzoate ligands to complete a significantly distorted PbO7F polyhedron. The Pb1—O bond lengths are in the range of 2.480 (6) to 2.766 (6) Å and the Pb1—F bond length is 2.856 (8)Å (Table 1). The Pb2 atom is coordinated by five O atoms from four 2-fluorobenzoate ligands and three water molecules to complete a significantly distorted PbO8 polyhedron. The Pb2—O bond lengths are in the range of 2.517 (5) to 2.999 (6)Å (Table 1). The 2-fluorobenzoate ligands bridge the Pb atoms, giving rise to a one-dimensional chain structure extending along the [100] direction (Fig. 2). There are intrachain O—H···O hydrogen bonds between the coordinated water molecules and the carboxylate O atoms of the 2-fluorobenzoate ligands (Table 2). The polymeric chains are connected via C—H···O hydrogen bonds and π–π stacking interactions between the benzene rings, with an interplanar distance of 3.46 (1) Å, into a two-dimensional supramolecular structure (Fig. 3).

Experimental

Freshly prepared PbCO3 (0.140 g, 0.52 mmol), 2-fluorobenzoic acid (0.035 g, 0.25 mmol) in CH3OH/H2O (15 ml; 1:2 v/v) were mixed and stirred for ca 2 h. Subsequently, the resulting suspension was heated in a 23 ml Teflon-lined stainless steel autoclave at 423 K for 5 d. After the autoclave was cooled to room temperature, the solid was filtered off. The resulting colorless filtrate was allowed to stand at room temperature for one month, affording colorless block crystals suitable for X-ray analysis.

Refinement

C-bound H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93Å and Uiso(H) = 1.2Ueq(C). H atoms of water molecules were located on a difference Fourier map and fixed with O—H = 0.82Å and Uiso(H) = 1.5Ueq(O). The highest residual electron density was 0.78Å from atom Pb2 and the deepest hole 0.71Å from atom Pb2.

Figures

Fig. 1.
The asymmetric unit of the title compound, together with symmetry-related atoms to complete the coordination units. Displacement ellipsoids are drawn at the 35% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) 1 - x, -y, ...
Fig. 2.
View of one-dimensional chain structure extending along the [100] direction.
Fig. 3.
The C—H···O hydrogen bonds (dashed lines) and the π–π stacking interactions in the title compound. [Symmetry code: (iv) -x, -y, 1 - z.]

Crystal data

[Pb2(C7H4FO2)4(H2O)2]Z = 2
Mr = 1006.84F000 = 936
Triclinic, P1Dx = 2.312 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 7.1016 (14) ÅCell parameters from 14100 reflections
b = 14.794 (3) Åθ = 3.0–27.5º
c = 15.096 (3) ŵ = 11.71 mm1
α = 111.56 (3)ºT = 290 (2) K
β = 95.32 (3)ºBlock, colorless
γ = 97.31 (3)º0.44 × 0.19 × 0.13 mm
V = 1446.2 (6) Å3

Data collection

Rigaku R-AXIS RAPID diffractometer6646 independent reflections
Radiation source: rotating anode5329 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.028
Detector resolution: 10 pixels mm-1θmax = 27.5º
T = 290(2) Kθmin = 3.0º
ω scansh = −8→9
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)k = −19→18
Tmin = 0.082, Tmax = 0.223l = −19→19
14182 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.038H-atom parameters constrained
wR(F2) = 0.094  w = 1/[σ2(Fo2) + (0.0382P)2 + 11.3431P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
6646 reflectionsΔρmax = 3.74 e Å3
397 parametersΔρmin = −2.48 e Å3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

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

xyzUiso*/Ueq
Pb10.50250 (4)0.06503 (2)0.265288 (19)0.02816 (8)
Pb20.99101 (4)0.11234 (2)0.13887 (2)0.03456 (9)
F10.8986 (13)0.3238 (6)0.1926 (7)0.106 (3)
F20.9276 (14)0.3801 (7)0.5078 (9)0.145 (4)
F3−0.3272 (8)−0.0400 (6)0.3676 (5)0.0707 (19)
F41.0244 (18)0.2764 (11)−0.0872 (11)0.180 (6)
O10.3833 (7)0.1887 (4)0.2019 (4)0.0382 (12)
O20.6657 (7)0.1535 (4)0.1739 (4)0.0343 (12)
O30.3924 (8)0.2018 (4)0.4107 (4)0.0424 (13)
O40.6947 (8)0.2189 (4)0.3891 (4)0.0417 (13)
O50.8814 (9)0.1620 (5)−0.0029 (5)0.0533 (17)
O60.5976 (8)0.0707 (4)−0.0775 (4)0.0377 (12)
O70.7609 (8)−0.0319 (4)0.0120 (4)0.0425 (13)
H7A0.6855−0.05660.03820.064*
H7B0.8141−0.0784−0.01520.064*
O80.8336 (8)0.0170 (5)0.2355 (4)0.0442 (14)
O90.1307 (8)0.0018 (5)0.2258 (4)0.0427 (14)
O101.0501 (8)0.2362 (5)0.3173 (4)0.0490 (15)
H10A1.14240.22560.34650.073*
H10B0.97460.26510.35050.073*
C10.5762 (13)0.2909 (6)0.1437 (6)0.0391 (18)
C20.7517 (15)0.3433 (7)0.1545 (8)0.053 (2)
C30.790 (2)0.4252 (8)0.1307 (11)0.086 (4)
H30.91460.45870.13890.103*
C40.635 (3)0.4537 (10)0.0945 (11)0.097 (5)
H40.65300.51020.08070.117*
C50.455 (2)0.4012 (10)0.0783 (10)0.082 (4)
H50.35800.42270.04960.098*
C60.396 (3)0.3144 (9)0.1011 (7)0.105 (6)
H60.27160.28030.09120.126*
C70.5377 (11)0.2061 (6)0.1744 (5)0.0306 (15)
C80.5995 (12)0.3522 (6)0.5128 (6)0.0380 (17)
C90.4447 (16)0.3912 (8)0.5579 (7)0.056 (2)
H90.32170.35400.54110.067*
C100.482 (2)0.4869 (8)0.6279 (8)0.074 (4)
H100.38170.51410.65700.089*
C110.660 (2)0.5406 (8)0.6543 (9)0.077 (4)
H110.68030.60370.70210.093*
C120.814 (2)0.5043 (8)0.6121 (8)0.075 (4)
H120.93690.54180.62960.090*
C130.7761 (15)0.4092 (8)0.5425 (8)0.058 (2)
C140.5595 (11)0.2510 (6)0.4324 (5)0.0328 (16)
C15−0.0168 (12)−0.0643 (6)0.3273 (6)0.0349 (16)
C160.1421 (14)−0.1041 (7)0.3439 (8)0.054 (2)
H160.2446−0.09850.31110.064*
C170.1563 (18)−0.1518 (9)0.4069 (9)0.073 (3)
H170.2674−0.17560.41810.087*
C180.0000 (17)−0.1632 (8)0.4532 (8)0.065 (3)
H180.0045−0.19680.49450.078*
C19−0.1581 (15)−0.1259 (8)0.4385 (7)0.057 (3)
H19−0.2618−0.13330.47010.068*
C20−0.1660 (12)−0.0773 (7)0.3773 (6)0.0426 (19)
C21−0.0202 (10)−0.0121 (5)0.2587 (5)0.0292 (15)
C220.7003 (14)0.2145 (6)−0.1082 (6)0.046 (2)
C230.849 (2)0.2749 (9)−0.1202 (9)0.072 (3)
C240.828 (3)0.3368 (10)−0.1663 (12)0.108 (6)
H240.93460.3763−0.17290.129*
C250.650 (3)0.3397 (10)−0.2026 (11)0.113 (7)
H250.63270.3816−0.23480.136*
C260.491 (2)0.2812 (9)−0.1926 (9)0.088 (4)
H260.36980.2864−0.21800.105*
C270.501 (3)0.2134 (9)−0.1455 (8)0.101 (6)
H270.39520.1736−0.13920.121*
C280.7316 (12)0.1442 (6)−0.0584 (6)0.0389 (18)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pb10.02153 (14)0.03441 (15)0.03085 (15)0.00615 (10)0.00427 (10)0.01469 (12)
Pb20.02253 (14)0.05183 (19)0.03065 (16)0.00657 (12)0.00338 (11)0.01749 (14)
F10.098 (6)0.095 (6)0.116 (7)−0.014 (5)0.001 (5)0.045 (5)
F20.087 (6)0.111 (7)0.172 (10)−0.004 (5)0.023 (7)−0.014 (7)
F30.039 (3)0.129 (6)0.083 (4)0.034 (3)0.027 (3)0.075 (4)
F40.120 (9)0.226 (14)0.235 (15)−0.030 (9)0.001 (10)0.162 (13)
O10.025 (3)0.051 (3)0.044 (3)0.008 (2)0.009 (2)0.023 (3)
O20.028 (3)0.042 (3)0.042 (3)0.011 (2)0.011 (2)0.024 (3)
O30.031 (3)0.049 (3)0.038 (3)0.002 (3)0.006 (2)0.008 (3)
O40.031 (3)0.046 (3)0.037 (3)0.006 (2)0.007 (2)0.003 (3)
O50.042 (4)0.074 (4)0.047 (4)−0.009 (3)−0.009 (3)0.037 (3)
O60.031 (3)0.041 (3)0.040 (3)0.000 (2)0.003 (2)0.018 (3)
O70.036 (3)0.041 (3)0.046 (3)0.006 (3)0.008 (3)0.013 (3)
O80.026 (3)0.071 (4)0.055 (4)0.019 (3)0.015 (3)0.041 (3)
O90.028 (3)0.055 (4)0.055 (4)0.010 (3)0.011 (3)0.031 (3)
O100.033 (3)0.064 (4)0.043 (3)0.011 (3)0.005 (3)0.013 (3)
C10.053 (5)0.034 (4)0.036 (4)0.019 (4)0.018 (4)0.014 (3)
C20.052 (6)0.049 (5)0.055 (6)0.005 (4)0.004 (5)0.018 (5)
C30.111 (11)0.047 (6)0.111 (11)0.003 (7)0.049 (9)0.039 (7)
C40.162 (16)0.062 (8)0.105 (11)0.047 (10)0.049 (11)0.059 (8)
C50.125 (12)0.069 (8)0.077 (9)0.052 (8)0.024 (8)0.044 (7)
C60.240 (19)0.079 (8)0.039 (6)0.116 (11)0.046 (8)0.039 (6)
C70.031 (4)0.038 (4)0.022 (3)0.006 (3)0.004 (3)0.010 (3)
C80.044 (5)0.043 (4)0.028 (4)0.011 (4)0.004 (3)0.014 (3)
C90.063 (6)0.059 (6)0.045 (5)0.016 (5)0.016 (5)0.014 (5)
C100.109 (10)0.053 (6)0.057 (7)0.034 (7)0.035 (7)0.005 (5)
C110.126 (12)0.041 (6)0.053 (7)0.011 (7)0.020 (7)0.004 (5)
C120.092 (9)0.049 (6)0.053 (7)−0.018 (6)0.006 (6)−0.004 (5)
C130.054 (6)0.063 (6)0.055 (6)0.014 (5)0.016 (5)0.018 (5)
C140.034 (4)0.039 (4)0.022 (3)0.004 (3)0.000 (3)0.010 (3)
C150.039 (4)0.038 (4)0.030 (4)0.010 (3)0.003 (3)0.015 (3)
C160.047 (5)0.065 (6)0.066 (6)0.023 (5)0.017 (5)0.039 (5)
C170.074 (8)0.090 (9)0.083 (8)0.038 (7)0.009 (6)0.059 (7)
C180.071 (7)0.077 (7)0.066 (7)0.016 (6)0.007 (6)0.051 (6)
C190.054 (6)0.074 (7)0.054 (6)0.004 (5)0.007 (5)0.039 (5)
C200.036 (4)0.056 (5)0.042 (5)0.010 (4)0.006 (4)0.025 (4)
C210.025 (4)0.031 (4)0.034 (4)0.005 (3)0.006 (3)0.015 (3)
C220.062 (6)0.035 (4)0.038 (5)−0.005 (4)0.006 (4)0.015 (4)
C230.078 (9)0.070 (7)0.069 (8)−0.010 (6)−0.001 (6)0.037 (6)
C240.141 (15)0.075 (9)0.111 (12)−0.036 (9)−0.004 (11)0.065 (9)
C250.21 (2)0.060 (8)0.079 (10)0.023 (11)−0.002 (12)0.043 (8)
C260.138 (13)0.053 (7)0.068 (8)0.037 (8)−0.017 (8)0.019 (6)
C270.191 (15)0.058 (7)0.041 (6)0.079 (9)−0.037 (7)0.000 (5)
C280.040 (4)0.047 (5)0.034 (4)0.006 (4)0.005 (3)0.021 (4)

Geometric parameters (Å, °)

Pb1—O42.480 (6)C4—C51.36 (2)
Pb1—O22.489 (5)C4—H40.9300
Pb1—O12.551 (6)C5—C61.469 (18)
Pb1—O82.574 (5)C5—H50.9300
Pb1—O92.621 (6)C6—H60.9300
Pb1—O32.642 (6)C8—C131.354 (13)
Pb1—O6i2.766 (6)C8—C91.420 (12)
Pb1—F3ii2.856 (8)C8—C141.513 (11)
Pb2—O22.517 (5)C9—C101.394 (14)
Pb2—O72.534 (6)C9—H90.9300
Pb2—O52.592 (6)C10—C111.344 (18)
Pb2—O102.599 (6)C10—H100.9300
Pb2—O82.603 (5)C11—C121.385 (18)
Pb2—O9ii2.670 (6)C11—H110.9300
Pb2—O7iii2.999 (6)C12—C131.386 (14)
Pb2—O1ii2.804 (5)C12—H120.9300
F1—C21.261 (13)C15—C161.381 (12)
F2—C131.294 (13)C15—C201.389 (11)
F3—C201.351 (10)C15—C211.502 (10)
F4—C231.290 (17)C16—C171.381 (13)
O1—C71.239 (9)C16—H160.9300
O2—C71.269 (9)C17—C181.390 (16)
O3—C141.256 (9)C17—H170.9300
O4—C141.256 (9)C18—C191.347 (15)
O5—C281.227 (10)C18—H180.9300
O6—C281.276 (10)C19—C201.366 (12)
O7—H7A0.8200C19—H190.9300
O7—H7B0.8200C21—O8iv1.243 (9)
O8—C21ii1.243 (9)C22—C231.366 (14)
O9—C211.247 (9)C22—C271.467 (17)
O9—Pb2iv2.670 (6)C22—C281.517 (11)
O10—H10A0.8200C23—C241.353 (17)
O10—H10B0.8200C24—C251.35 (2)
C1—C21.344 (13)C24—H240.9300
C1—C71.491 (10)C25—C261.39 (2)
C1—C61.515 (17)C25—H250.9300
C2—C31.386 (14)C26—C271.433 (16)
C3—C41.37 (2)C26—H260.9300
C3—H30.9300C27—H270.9300
O4—Pb1—O274.52 (19)C1—C2—C3125.1 (11)
O4—Pb1—O181.3 (2)C4—C3—C2116.2 (13)
O2—Pb1—O151.13 (16)C4—C3—H3121.9
O4—Pb1—O883.7 (2)C2—C3—H3121.9
O2—Pb1—O868.63 (17)C5—C4—C3121.3 (11)
O1—Pb1—O8119.76 (17)C5—C4—H4119.3
O4—Pb1—O9130.77 (18)C3—C4—H4119.3
O2—Pb1—O9120.83 (18)C4—C5—C6127.4 (13)
O1—Pb1—O977.90 (17)C4—C5—H5116.3
O8—Pb1—O9145.0 (2)C6—C5—H5116.3
O4—Pb1—O350.68 (17)C5—C6—C1107.1 (14)
O2—Pb1—O3106.06 (18)C5—C6—H6126.4
O1—Pb1—O372.71 (19)C1—C6—H6126.4
O8—Pb1—O3131.93 (19)O1—C7—O2120.4 (7)
O9—Pb1—O380.51 (19)O1—C7—C1120.1 (7)
O6i—Pb1—F3ii104.7 (2)O2—C7—C1119.6 (6)
O1—Pb1—O6i85.90 (18)C13—C8—C9117.9 (9)
O2—Pb1—O6i77.99 (18)C13—C8—C14123.1 (8)
O9—Pb1—O6i69.51 (17)C9—C8—C14119.0 (8)
O8—Pb1—O6i81.25 (18)C10—C9—C8118.2 (11)
O3—Pb1—O6i146.29 (17)C10—C9—H9120.9
O4—Pb1—O6i151.93 (18)C8—C9—H9120.9
O4—Pb1—F3ii87.65 (20)C11—C10—C9121.4 (11)
O1—Pb1—F3ii168.83 (21)C11—C10—H10119.3
O3—Pb1—F3ii99.11 (19)C9—C10—H10119.3
O9—Pb1—F3ii108.72 (18)C10—C11—C12121.7 (10)
O2—Pb1—F3ii126.98 (22)C10—C11—H11119.2
O8—Pb1—F3ii59.89 (19)C12—C11—H11119.2
O2—Pb2—O776.62 (18)C11—C12—C13116.6 (11)
O2—Pb2—O578.46 (19)C11—C12—H12121.7
O7—Pb2—O571.2 (2)C13—C12—H12121.7
O2—Pb2—O1075.17 (18)F2—C13—C8123.0 (10)
O7—Pb2—O10144.72 (19)F2—C13—C12112.9 (11)
O5—Pb2—O10122.4 (2)C8—C13—C12124.1 (10)
O2—Pb2—O867.75 (17)O4—C14—O3122.0 (7)
O7—Pb2—O875.8 (2)O4—C14—C8118.9 (7)
O5—Pb2—O8137.09 (18)O3—C14—C8119.1 (7)
O10—Pb2—O874.2 (2)C16—C15—C20115.2 (7)
O2—Pb2—O9ii115.50 (16)C16—C15—C21120.1 (7)
O7—Pb2—O9ii93.94 (19)C20—C15—C21124.7 (7)
O5—Pb2—O9ii157.3 (2)C17—C16—C15123.2 (9)
O10—Pb2—O9ii79.6 (2)C17—C16—H16118.4
O8—Pb2—O9ii48.39 (16)C15—C16—H16118.4
O2—Pb2—O1ii141.13 (16)C16—C17—C18118.2 (10)
O5—Pb2—O1ii108.21 (19)C16—C17—H17120.9
O7—Pb2—O1ii142.21 (17)C18—C17—H17120.9
O8—Pb2—O1ii114.69 (18)C19—C18—C17120.3 (9)
O9—Pb2—O1ii150.98 (13)C19—C18—H18119.8
O10—Pb2—O1ii69.09 (17)C17—C18—H18119.8
O7iii—Pb2—O1ii66.45 (15)C18—C19—C20120.0 (10)
O2—Pb2—O7iii146.84 (16)C18—C19—H19120.0
O5—Pb2—O7iii73.48 (19)C20—C19—H19120.0
O7—Pb2—O7iii77.86 (17)F3—C20—C19116.8 (8)
O8—Pb2—O7iii125.04 (17)F3—C20—C15120.2 (7)
O9—Pb2—O7iii138.80 (13)C19—C20—C15123.0 (8)
O10—Pb2—O7iii135.54 (17)O8iv—C21—O9120.6 (7)
C7—O1—Pb192.7 (5)O8iv—C21—C15121.9 (6)
C7—O2—Pb194.9 (4)O9—C21—C15117.5 (7)
C7—O2—Pb2150.1 (5)C23—C22—C27121.0 (11)
Pb1—O2—Pb2114.7 (2)C23—C22—C28122.1 (10)
C14—O3—Pb189.7 (4)C27—C22—C28116.9 (9)
C14—O4—Pb197.4 (5)F4—C23—C24114.8 (13)
C28—O5—Pb2135.0 (5)F4—C23—C22121.2 (11)
Pb2—O7—H7A109.5C24—C23—C22124.0 (14)
Pb2—O7—H7B112.5C25—C24—C23118.3 (14)
H7A—O7—H7B101.3C25—C24—H24120.8
C21—O8—Pb1ii171.78 (14)C23—C24—H24120.8
C21—O8—Pb2ii169.90 (14)C24—C25—C26121.1 (12)
Pb1—O8—Pb2109.0 (2)C24—C25—H25119.4
C21—O9—Pb1146.2 (5)C26—C25—H25119.4
C21iv—O9—Pb2161.84 (13)C25—C26—C27123.8 (15)
Pb1iv—O9—Pb2152.03 (16)C25—C26—H26118.1
Pb2—O10—H10A109.5C27—C26—H26118.1
Pb2—O10—H10B129.8C26—C27—C22111.7 (15)
H10A—O10—H10B115.8C26—C27—H27124.1
C2—C1—C7123.9 (8)C22—C27—H27124.1
C2—C1—C6122.7 (10)O5—C28—O6125.0 (8)
C7—C1—C6113.3 (9)O5—C28—C22118.3 (8)
F1—C2—C1121.4 (9)O6—C28—C22116.7 (7)
F1—C2—C3113.4 (11)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O7—H7A···O6i0.822.152.881 (8)148
O7—H7B···O5iii0.822.663.360 (8)144
O10—H10A···O3ii0.822.072.892 (8)174
O10—H10B···O40.822.222.856 (8)135
O10—H10B···F20.822.443.161 (13)147
C19—H19···O3v0.932.563.364 (13)145

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2143).

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