catena-Poly[μ-aqua-2:1′κ2O:O-aqua-2κO-(2-fluoro­benzoato-1κ2O,O′)(μ2-2-fluoro­benzoato-2′:1κ2O:O′)bis­(μ3-2-fluoro­benzoato)-2′:1:2κ4O:O,O′:O′;1:2:1′κ5F,O:O,O′:O′-dilead(II)]

Zhang, B.-S.

doi:10.1107/S1600536808022678

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 8| August 2008| Pages m1055-m1056

doi:10.1107/S1600536808022678

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catena-Poly[μ-aqua-2:1′κ²O:O-aqua-2κO-(2-fluorobenzoato-1κ²O,O′)(μ₂-2-fluorobenzoato-2′:1κ²O:O′)bis(μ₃-2-fluorobenzoato)-2′:1:2κ⁴O:O,O′:O′;1:2:1′κ⁵F,O:O,O′:O′-dilead(II)]

Bi-Song Zhang ^a ^*

^aCollege of Materials Science and Chemical Engineering, Jinhua College of Professions and Technology, Jinhua, Zhejiang 321017, People's Republic of China
^*Correspondence e-mail: zbs_jy@163.com

(Received 4 July 2008; accepted 18 July 2008; online 23 July 2008)

In the title compound, [Pb₂(C₇H₄FO₂)₄(H₂O)₂]_n, one Pb^II atom is coordinated by seven O atoms and one F atom from five 2-fluorobenzoate ligands, and the other Pb^II 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 ); Xiao & Morsali (2007 ); Zhang (2004 , 2005 , 2006a ,b ,c ); Zhang et al. (2005 ); Zhu et al. (1999 ).

Experimental

Crystal data

[Pb₂(C₇H₄FO₂)₄(H₂O)₂]
M_r = 1006.84
Triclinic, $[P \overline 1]$
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 ) 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[F² > 2σ(F²)] = 0.037
wR(F²) = 0.094
S = 1.03
6646 reflections
397 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 3.74 e Å⁻³
Δρ_min = −2.48 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O4	2.480 (6)
Pb1—O2	2.489 (5)
Pb1—O1	2.551 (6)
Pb1—O8	2.574 (5)
Pb1—O9	2.621 (6)
Pb1—O3	2.642 (6)
Pb1—O6ⁱ	2.766 (6)
Pb1—F3ⁱⁱ	2.856 (8)
Pb2—O2	2.517 (5)
Pb2—O7	2.534 (6)
Pb2—O5	2.592 (6)
Pb2—O10	2.599 (6)
Pb2—O8	2.603 (5)
Pb2—O9ⁱⁱ	2.670 (6)
Pb2—O7ⁱⁱⁱ	2.999 (6)
Pb2—O1ⁱⁱ	2.804 (5)
Symmetry codes: (i) -x+1, -y, -z; (ii) x+1, y, z; (iii) -x+2, -y, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O6ⁱ	0.82	2.15	2.881 (8)	148
O7—H7B⋯O5ⁱⁱⁱ	0.82	2.66	3.360 (8)	144
O10—H10A⋯O3ⁱⁱ	0.82	2.07	2.892 (8)	174
O10—H10B⋯O4	0.82	2.22	2.856 (8)	135
O10—H10B⋯F2	0.82	2.44	3.161 (13)	147
C19—H19⋯O3^iv	0.93	2.56	3.364 (13)	145
Symmetry codes: (i) -x+1, -y, -z; (ii) x+1, y, z; (iii) -x+2, -y, -z; (iv) -x, -y, -z+1.

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; 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: SHELXL97.

Supporting information

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

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

checkCIF report

Comment top

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 Pb^II 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).

Related literature top

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

Experimental top

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.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); 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: SHELXL97 (Sheldrick, 2008).

Figures top

	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, -z; (ii) 1 + x, y, z; (iii) 2 - x, -y, -z.]
	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.]

catena-Poly[µ-aqua-2:1'κ²O:O-aqua-2κO-(2-fluorobenzoato- 1κ²O,O')(µ₂-2-fluorobenzoato- 2':1κ²O:O')bis(µ₃-2-fluorobenzoato)- 2':1:2κ⁴O:O,O':O';1:2:1'κ⁵F,O:O,O':O'-dilead(II)] top

Crystal data top

[Pb₂(C₇H₄FO₂)₄(H₂O)₂]	Z = 2
M_r = 1006.84	F(000) = 936
Triclinic, P1	D_x = 2.312 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.1016 (14) Å	Cell parameters from 14100 reflections
b = 14.794 (3) Å	θ = 3.0–27.5°
c = 15.096 (3) Å	µ = 11.71 mm⁻¹
α = 111.56 (3)°	T = 290 K
β = 95.32 (3)°	Block, colorless
γ = 97.31 (3)°	0.44 × 0.19 × 0.13 mm
V = 1446.2 (6) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	6646 independent reflections
Radiation source: rotating anode	5329 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.028
Detector resolution: 10 pixels mm^-1	θ_max = 27.5°, θ_min = 3.0°
ω scans	h = −8→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −19→18
T_min = 0.082, T_max = 0.223	l = −19→19
14182 measured reflections

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0382P)² + 11.3431P] where P = (F_o² + 2F_c²)/3
6646 reflections	(Δ/σ)_max = 0.001
397 parameters	Δρ_max = 3.74 e Å⁻³
3 restraints	Δρ_min = −2.48 e Å⁻³

Crystal data top

[Pb₂(C₇H₄FO₂)₄(H₂O)₂]	γ = 97.31 (3)°
M_r = 1006.84	V = 1446.2 (6) Å³
Triclinic, P1	Z = 2
a = 7.1016 (14) Å	Mo Kα radiation
b = 14.794 (3) Å	µ = 11.71 mm⁻¹
c = 15.096 (3) Å	T = 290 K
α = 111.56 (3)°	0.44 × 0.19 × 0.13 mm
β = 95.32 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	6646 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	5329 reflections with I > 2σ(I)
T_min = 0.082, T_max = 0.223	R_int = 0.028
14182 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	3 restraints
wR(F²) = 0.094	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0382P)² + 11.3431P] where P = (F_o² + 2F_c²)/3
6646 reflections	Δρ_max = 3.74 e Å⁻³
397 parameters	Δρ_min = −2.48 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Pb1	0.50250 (4)	0.06503 (2)	0.265288 (19)	0.02816 (8)
Pb2	0.99101 (4)	0.11234 (2)	0.13887 (2)	0.03456 (9)
F1	0.8986 (13)	0.3238 (6)	0.1926 (7)	0.106 (3)
F2	0.9276 (14)	0.3801 (7)	0.5078 (9)	0.145 (4)
F3	−0.3272 (8)	−0.0400 (6)	0.3676 (5)	0.0707 (19)
F4	1.0244 (18)	0.2764 (11)	−0.0872 (11)	0.180 (6)
O1	0.3833 (7)	0.1887 (4)	0.2019 (4)	0.0382 (12)
O2	0.6657 (7)	0.1535 (4)	0.1739 (4)	0.0343 (12)
O3	0.3924 (8)	0.2018 (4)	0.4107 (4)	0.0424 (13)
O4	0.6947 (8)	0.2189 (4)	0.3891 (4)	0.0417 (13)
O5	0.8814 (9)	0.1620 (5)	−0.0029 (5)	0.0533 (17)
O6	0.5976 (8)	0.0707 (4)	−0.0775 (4)	0.0377 (12)
O7	0.7609 (8)	−0.0319 (4)	0.0120 (4)	0.0425 (13)
H7A	0.6855	−0.0566	0.0382	0.064*
H7B	0.8141	−0.0784	−0.0152	0.064*
O8	0.8336 (8)	0.0170 (5)	0.2355 (4)	0.0442 (14)
O9	0.1307 (8)	0.0018 (5)	0.2258 (4)	0.0427 (14)
O10	1.0501 (8)	0.2362 (5)	0.3173 (4)	0.0490 (15)
H10A	1.1424	0.2256	0.3465	0.073*
H10B	0.9746	0.2651	0.3505	0.073*
C1	0.5762 (13)	0.2909 (6)	0.1437 (6)	0.0391 (18)
C2	0.7517 (15)	0.3433 (7)	0.1545 (8)	0.053 (2)
C3	0.790 (2)	0.4252 (8)	0.1307 (11)	0.086 (4)
H3	0.9146	0.4587	0.1389	0.103*
C4	0.635 (3)	0.4537 (10)	0.0945 (11)	0.097 (5)
H4	0.6530	0.5102	0.0807	0.117*
C5	0.455 (2)	0.4012 (10)	0.0783 (10)	0.082 (4)
H5	0.3580	0.4227	0.0496	0.098*
C6	0.396 (3)	0.3144 (9)	0.1011 (7)	0.105 (6)
H6	0.2716	0.2803	0.0912	0.126*
C7	0.5377 (11)	0.2061 (6)	0.1744 (5)	0.0306 (15)
C8	0.5995 (12)	0.3522 (6)	0.5128 (6)	0.0380 (17)
C9	0.4447 (16)	0.3912 (8)	0.5579 (7)	0.056 (2)
H9	0.3217	0.3540	0.5411	0.067*
C10	0.482 (2)	0.4869 (8)	0.6279 (8)	0.074 (4)
H10	0.3817	0.5141	0.6570	0.089*
C11	0.660 (2)	0.5406 (8)	0.6543 (9)	0.077 (4)
H11	0.6803	0.6037	0.7021	0.093*
C12	0.814 (2)	0.5043 (8)	0.6121 (8)	0.075 (4)
H12	0.9369	0.5418	0.6296	0.090*
C13	0.7761 (15)	0.4092 (8)	0.5425 (8)	0.058 (2)
C14	0.5595 (11)	0.2510 (6)	0.4324 (5)	0.0328 (16)
C15	−0.0168 (12)	−0.0643 (6)	0.3273 (6)	0.0349 (16)
C16	0.1421 (14)	−0.1041 (7)	0.3439 (8)	0.054 (2)
H16	0.2446	−0.0985	0.3111	0.064*
C17	0.1563 (18)	−0.1518 (9)	0.4069 (9)	0.073 (3)
H17	0.2674	−0.1756	0.4181	0.087*
C18	0.0000 (17)	−0.1632 (8)	0.4532 (8)	0.065 (3)
H18	0.0045	−0.1968	0.4945	0.078*
C19	−0.1581 (15)	−0.1259 (8)	0.4385 (7)	0.057 (3)
H19	−0.2618	−0.1333	0.4701	0.068*
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)
C22	0.7003 (14)	0.2145 (6)	−0.1082 (6)	0.046 (2)
C23	0.849 (2)	0.2749 (9)	−0.1202 (9)	0.072 (3)
C24	0.828 (3)	0.3368 (10)	−0.1663 (12)	0.108 (6)
H24	0.9346	0.3763	−0.1729	0.129*
C25	0.650 (3)	0.3397 (10)	−0.2026 (11)	0.113 (7)
H25	0.6327	0.3816	−0.2348	0.136*
C26	0.491 (2)	0.2812 (9)	−0.1926 (9)	0.088 (4)
H26	0.3698	0.2864	−0.2180	0.105*
C27	0.501 (3)	0.2134 (9)	−0.1455 (8)	0.101 (6)
H27	0.3952	0.1736	−0.1392	0.121*
C28	0.7316 (12)	0.1442 (6)	−0.0584 (6)	0.0389 (18)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02153 (14)	0.03441 (15)	0.03085 (15)	0.00615 (10)	0.00427 (10)	0.01469 (12)
Pb2	0.02253 (14)	0.05183 (19)	0.03065 (16)	0.00657 (12)	0.00338 (11)	0.01749 (14)
F1	0.098 (6)	0.095 (6)	0.116 (7)	−0.014 (5)	0.001 (5)	0.045 (5)
F2	0.087 (6)	0.111 (7)	0.172 (10)	−0.004 (5)	0.023 (7)	−0.014 (7)
F3	0.039 (3)	0.129 (6)	0.083 (4)	0.034 (3)	0.027 (3)	0.075 (4)
F4	0.120 (9)	0.226 (14)	0.235 (15)	−0.030 (9)	0.001 (10)	0.162 (13)
O1	0.025 (3)	0.051 (3)	0.044 (3)	0.008 (2)	0.009 (2)	0.023 (3)
O2	0.028 (3)	0.042 (3)	0.042 (3)	0.011 (2)	0.011 (2)	0.024 (3)
O3	0.031 (3)	0.049 (3)	0.038 (3)	0.002 (3)	0.006 (2)	0.008 (3)
O4	0.031 (3)	0.046 (3)	0.037 (3)	0.006 (2)	0.007 (2)	0.003 (3)
O5	0.042 (4)	0.074 (4)	0.047 (4)	−0.009 (3)	−0.009 (3)	0.037 (3)
O6	0.031 (3)	0.041 (3)	0.040 (3)	0.000 (2)	0.003 (2)	0.018 (3)
O7	0.036 (3)	0.041 (3)	0.046 (3)	0.006 (3)	0.008 (3)	0.013 (3)
O8	0.026 (3)	0.071 (4)	0.055 (4)	0.019 (3)	0.015 (3)	0.041 (3)
O9	0.028 (3)	0.055 (4)	0.055 (4)	0.010 (3)	0.011 (3)	0.031 (3)
O10	0.033 (3)	0.064 (4)	0.043 (3)	0.011 (3)	0.005 (3)	0.013 (3)
C1	0.053 (5)	0.034 (4)	0.036 (4)	0.019 (4)	0.018 (4)	0.014 (3)
C2	0.052 (6)	0.049 (5)	0.055 (6)	0.005 (4)	0.004 (5)	0.018 (5)
C3	0.111 (11)	0.047 (6)	0.111 (11)	0.003 (7)	0.049 (9)	0.039 (7)
C4	0.162 (16)	0.062 (8)	0.105 (11)	0.047 (10)	0.049 (11)	0.059 (8)
C5	0.125 (12)	0.069 (8)	0.077 (9)	0.052 (8)	0.024 (8)	0.044 (7)
C6	0.240 (19)	0.079 (8)	0.039 (6)	0.116 (11)	0.046 (8)	0.039 (6)
C7	0.031 (4)	0.038 (4)	0.022 (3)	0.006 (3)	0.004 (3)	0.010 (3)
C8	0.044 (5)	0.043 (4)	0.028 (4)	0.011 (4)	0.004 (3)	0.014 (3)
C9	0.063 (6)	0.059 (6)	0.045 (5)	0.016 (5)	0.016 (5)	0.014 (5)
C10	0.109 (10)	0.053 (6)	0.057 (7)	0.034 (7)	0.035 (7)	0.005 (5)
C11	0.126 (12)	0.041 (6)	0.053 (7)	0.011 (7)	0.020 (7)	0.004 (5)
C12	0.092 (9)	0.049 (6)	0.053 (7)	−0.018 (6)	0.006 (6)	−0.004 (5)
C13	0.054 (6)	0.063 (6)	0.055 (6)	0.014 (5)	0.016 (5)	0.018 (5)
C14	0.034 (4)	0.039 (4)	0.022 (3)	0.004 (3)	0.000 (3)	0.010 (3)
C15	0.039 (4)	0.038 (4)	0.030 (4)	0.010 (3)	0.003 (3)	0.015 (3)
C16	0.047 (5)	0.065 (6)	0.066 (6)	0.023 (5)	0.017 (5)	0.039 (5)
C17	0.074 (8)	0.090 (9)	0.083 (8)	0.038 (7)	0.009 (6)	0.059 (7)
C18	0.071 (7)	0.077 (7)	0.066 (7)	0.016 (6)	0.007 (6)	0.051 (6)
C19	0.054 (6)	0.074 (7)	0.054 (6)	0.004 (5)	0.007 (5)	0.039 (5)
C20	0.036 (4)	0.056 (5)	0.042 (5)	0.010 (4)	0.006 (4)	0.025 (4)
C21	0.025 (4)	0.031 (4)	0.034 (4)	0.005 (3)	0.006 (3)	0.015 (3)
C22	0.062 (6)	0.035 (4)	0.038 (5)	−0.005 (4)	0.006 (4)	0.015 (4)
C23	0.078 (9)	0.070 (7)	0.069 (8)	−0.010 (6)	−0.001 (6)	0.037 (6)
C24	0.141 (15)	0.075 (9)	0.111 (12)	−0.036 (9)	−0.004 (11)	0.065 (9)
C25	0.21 (2)	0.060 (8)	0.079 (10)	0.023 (11)	−0.002 (12)	0.043 (8)
C26	0.138 (13)	0.053 (7)	0.068 (8)	0.037 (8)	−0.017 (8)	0.019 (6)
C27	0.191 (15)	0.058 (7)	0.041 (6)	0.079 (9)	−0.037 (7)	0.000 (5)
C28	0.040 (4)	0.047 (5)	0.034 (4)	0.006 (4)	0.005 (3)	0.021 (4)

Geometric parameters (Å, º) top

Pb1—O4	2.480 (6)	C4—C5	1.36 (2)
Pb1—O2	2.489 (5)	C4—H4	0.9300
Pb1—O1	2.551 (6)	C5—C6	1.469 (18)
Pb1—O8	2.574 (5)	C5—H5	0.9300
Pb1—O9	2.621 (6)	C6—H6	0.9300
Pb1—O3	2.642 (6)	C8—C13	1.354 (13)
Pb1—O6ⁱ	2.766 (6)	C8—C9	1.420 (12)
Pb1—F3ⁱⁱ	2.856 (8)	C8—C14	1.513 (11)
Pb2—O2	2.517 (5)	C9—C10	1.394 (14)
Pb2—O7	2.534 (6)	C9—H9	0.9300
Pb2—O5	2.592 (6)	C10—C11	1.344 (18)
Pb2—O10	2.599 (6)	C10—H10	0.9300
Pb2—O8	2.603 (5)	C11—C12	1.385 (18)
Pb2—O9ⁱⁱ	2.670 (6)	C11—H11	0.9300
Pb2—O7ⁱⁱⁱ	2.999 (6)	C12—C13	1.386 (14)
Pb2—O1ⁱⁱ	2.804 (5)	C12—H12	0.9300
F1—C2	1.261 (13)	C15—C16	1.381 (12)
F2—C13	1.294 (13)	C15—C20	1.389 (11)
F3—C20	1.351 (10)	C15—C21	1.502 (10)
F4—C23	1.290 (17)	C16—C17	1.381 (13)
O1—C7	1.239 (9)	C16—H16	0.9300
O2—C7	1.269 (9)	C17—C18	1.390 (16)
O3—C14	1.256 (9)	C17—H17	0.9300
O4—C14	1.256 (9)	C18—C19	1.347 (15)
O5—C28	1.227 (10)	C18—H18	0.9300
O6—C28	1.276 (10)	C19—C20	1.366 (12)
O7—H7A	0.8200	C19—H19	0.9300
O7—H7B	0.8200	C21—O8^iv	1.243 (9)
O8—C21ⁱⁱ	1.243 (9)	C22—C23	1.366 (14)
O9—C21	1.247 (9)	C22—C27	1.467 (17)
O9—Pb2^iv	2.670 (6)	C22—C28	1.517 (11)
O10—H10A	0.8200	C23—C24	1.353 (17)
O10—H10B	0.8200	C24—C25	1.35 (2)
C1—C2	1.344 (13)	C24—H24	0.9300
C1—C7	1.491 (10)	C25—C26	1.39 (2)
C1—C6	1.515 (17)	C25—H25	0.9300
C2—C3	1.386 (14)	C26—C27	1.433 (16)
C3—C4	1.37 (2)	C26—H26	0.9300
C3—H3	0.9300	C27—H27	0.9300

O4—Pb1—O2	74.52 (19)	C1—C2—C3	125.1 (11)
O4—Pb1—O1	81.3 (2)	C4—C3—C2	116.2 (13)
O2—Pb1—O1	51.13 (16)	C4—C3—H3	121.9
O4—Pb1—O8	83.7 (2)	C2—C3—H3	121.9
O2—Pb1—O8	68.63 (17)	C5—C4—C3	121.3 (11)
O1—Pb1—O8	119.76 (17)	C5—C4—H4	119.3
O4—Pb1—O9	130.77 (18)	C3—C4—H4	119.3
O2—Pb1—O9	120.83 (18)	C4—C5—C6	127.4 (13)
O1—Pb1—O9	77.90 (17)	C4—C5—H5	116.3
O8—Pb1—O9	145.0 (2)	C6—C5—H5	116.3
O4—Pb1—O3	50.68 (17)	C5—C6—C1	107.1 (14)
O2—Pb1—O3	106.06 (18)	C5—C6—H6	126.4
O1—Pb1—O3	72.71 (19)	C1—C6—H6	126.4
O8—Pb1—O3	131.93 (19)	O1—C7—O2	120.4 (7)
O9—Pb1—O3	80.51 (19)	O1—C7—C1	120.1 (7)
O6ⁱ—Pb1—F3ⁱⁱ	104.7 (2)	O2—C7—C1	119.6 (6)
O1—Pb1—O6ⁱ	85.90 (18)	C13—C8—C9	117.9 (9)
O2—Pb1—O6ⁱ	77.99 (18)	C13—C8—C14	123.1 (8)
O9—Pb1—O6ⁱ	69.51 (17)	C9—C8—C14	119.0 (8)
O8—Pb1—O6ⁱ	81.25 (18)	C10—C9—C8	118.2 (11)
O3—Pb1—O6ⁱ	146.29 (17)	C10—C9—H9	120.9
O4—Pb1—O6ⁱ	151.93 (18)	C8—C9—H9	120.9
O4—Pb1—F3ⁱⁱ	87.7 (2)	C11—C10—C9	121.4 (11)
O1—Pb1—F3ⁱⁱ	168.8 (2)	C11—C10—H10	119.3
O3—Pb1—F3ⁱⁱ	99.11 (19)	C9—C10—H10	119.3
O9—Pb1—F3ⁱⁱ	108.72 (18)	C10—C11—C12	121.7 (10)
O2—Pb1—F3ⁱⁱ	127.0 (2)	C10—C11—H11	119.2
O8—Pb1—F3ⁱⁱ	59.89 (19)	C12—C11—H11	119.2
O2—Pb2—O7	76.62 (18)	C11—C12—C13	116.6 (11)
O2—Pb2—O5	78.46 (19)	C11—C12—H12	121.7
O7—Pb2—O5	71.2 (2)	C13—C12—H12	121.7
O2—Pb2—O10	75.17 (18)	F2—C13—C8	123.0 (10)
O7—Pb2—O10	144.72 (19)	F2—C13—C12	112.9 (11)
O5—Pb2—O10	122.4 (2)	C8—C13—C12	124.1 (10)
O2—Pb2—O8	67.75 (17)	O4—C14—O3	122.0 (7)
O7—Pb2—O8	75.8 (2)	O4—C14—C8	118.9 (7)
O5—Pb2—O8	137.09 (18)	O3—C14—C8	119.1 (7)
O10—Pb2—O8	74.2 (2)	C16—C15—C20	115.2 (7)
O2—Pb2—O9ⁱⁱ	115.50 (16)	C16—C15—C21	120.1 (7)
O7—Pb2—O9ⁱⁱ	93.94 (19)	C20—C15—C21	124.7 (7)
O5—Pb2—O9ⁱⁱ	157.3 (2)	C17—C16—C15	123.2 (9)
O10—Pb2—O9ⁱⁱ	79.6 (2)	C17—C16—H16	118.4
O8—Pb2—O9ⁱⁱ	48.39 (16)	C15—C16—H16	118.4
O2—Pb2—O1ⁱⁱ	141.13 (16)	C16—C17—C18	118.2 (10)
O5—Pb2—O1ⁱⁱ	108.21 (19)	C16—C17—H17	120.9
O7—Pb2—O1ⁱⁱ	142.21 (17)	C18—C17—H17	120.9
O8—Pb2—O1ⁱⁱ	114.69 (18)	C19—C18—C17	120.3 (9)
O9—Pb2—O1ⁱⁱ	150.98 (13)	C19—C18—H18	119.8
O10—Pb2—O1ⁱⁱ	69.09 (17)	C17—C18—H18	119.8
O7ⁱⁱⁱ—Pb2—O1ⁱⁱ	66.45 (15)	C18—C19—C20	120.0 (10)
O2—Pb2—O7ⁱⁱⁱ	146.84 (16)	C18—C19—H19	120.0
O5—Pb2—O7ⁱⁱⁱ	73.48 (19)	C20—C19—H19	120.0
O7—Pb2—O7ⁱⁱⁱ	77.86 (17)	F3—C20—C19	116.8 (8)
O8—Pb2—O7ⁱⁱⁱ	125.04 (17)	F3—C20—C15	120.2 (7)
O9—Pb2—O7ⁱⁱⁱ	138.80 (13)	C19—C20—C15	123.0 (8)
O10—Pb2—O7ⁱⁱⁱ	135.54 (17)	O8^iv—C21—O9	120.6 (7)
C7—O1—Pb1	92.7 (5)	O8^iv—C21—C15	121.9 (6)
C7—O2—Pb1	94.9 (4)	O9—C21—C15	117.5 (7)
C7—O2—Pb2	150.1 (5)	C23—C22—C27	121.0 (11)
Pb1—O2—Pb2	114.7 (2)	C23—C22—C28	122.1 (10)
C14—O3—Pb1	89.7 (4)	C27—C22—C28	116.9 (9)
C14—O4—Pb1	97.4 (5)	F4—C23—C24	114.8 (13)
C28—O5—Pb2	135.0 (5)	F4—C23—C22	121.2 (11)
Pb2—O7—H7A	109.5	C24—C23—C22	124.0 (14)
Pb2—O7—H7B	112.5	C25—C24—C23	118.3 (14)
H7A—O7—H7B	101.3	C25—C24—H24	120.8
C21—O8—Pb1ⁱⁱ	171.78 (14)	C23—C24—H24	120.8
C21—O8—Pb2ⁱⁱ	169.90 (14)	C24—C25—C26	121.1 (12)
Pb1—O8—Pb2	109.0 (2)	C24—C25—H25	119.4
C21—O9—Pb1	146.2 (5)	C26—C25—H25	119.4
C21^iv—O9—Pb2	161.84 (13)	C25—C26—C27	123.8 (15)
Pb1^iv—O9—Pb2	152.03 (16)	C25—C26—H26	118.1
Pb2—O10—H10A	109.5	C27—C26—H26	118.1
Pb2—O10—H10B	129.8	C26—C27—C22	111.7 (15)
H10A—O10—H10B	115.8	C26—C27—H27	124.1
C2—C1—C7	123.9 (8)	C22—C27—H27	124.1
C2—C1—C6	122.7 (10)	O5—C28—O6	125.0 (8)
C7—C1—C6	113.3 (9)	O5—C28—C22	118.3 (8)
F1—C2—C1	121.4 (9)	O6—C28—C22	116.7 (7)
F1—C2—C3	113.4 (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, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O6ⁱ	0.82	2.15	2.881 (8)	148
O7—H7B···O5ⁱⁱⁱ	0.82	2.66	3.360 (8)	144
O10—H10A···O3ⁱⁱ	0.82	2.07	2.892 (8)	174
O10—H10B···O4	0.82	2.22	2.856 (8)	135
O10—H10B···F2	0.82	2.44	3.161 (13)	147
C19—H19···O3^v	0.93	2.56	3.364 (13)	145

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

Experimental details

Crystal data
Chemical formula	[Pb₂(C₇H₄FO₂)₄(H₂O)₂]
M_r	1006.84
Crystal system, space group	Triclinic, P1
Temperature (K)	290
a, b, c (Å)	7.1016 (14), 14.794 (3), 15.096 (3)
α, β, γ (°)	111.56 (3), 95.32 (3), 97.31 (3)
V (Å³)	1446.2 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	11.71
Crystal size (mm)	0.44 × 0.19 × 0.13

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.082, 0.223
No. of measured, independent and observed [I > 2σ(I)] reflections	14182, 6646, 5329
R_int	0.028
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.094, 1.03
No. of reflections	6646
No. of parameters	397
No. of restraints	3
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0382P)² + 11.3431P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	3.74, −2.48

Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Pb1—O4	2.480 (6)	Pb2—O2	2.517 (5)
Pb1—O2	2.489 (5)	Pb2—O7	2.534 (6)
Pb1—O1	2.551 (6)	Pb2—O5	2.592 (6)
Pb1—O8	2.574 (5)	Pb2—O10	2.599 (6)
Pb1—O9	2.621 (6)	Pb2—O8	2.603 (5)
Pb1—O3	2.642 (6)	Pb2—O9ⁱⁱ	2.670 (6)
Pb1—O6ⁱ	2.766 (6)	Pb2—O7ⁱⁱⁱ	2.999 (6)
Pb1—F3ⁱⁱ	2.856 (8)	Pb2—O1ⁱⁱ	2.804 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O6ⁱ	0.82	2.15	2.881 (8)	148
O7—H7B···O5ⁱⁱⁱ	0.82	2.66	3.360 (8)	144
O10—H10A···O3ⁱⁱ	0.82	2.07	2.892 (8)	174
O10—H10B···O4	0.82	2.22	2.856 (8)	135
O10—H10B···F2	0.82	2.44	3.161 (13)	147
C19—H19···O3^iv	0.93	2.56	3.364 (13)	145

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

Acknowledgements

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

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Morsali, A. & Mahjoub, A. R. (2005). Solid State Sci. 7, 1429–1437. Web of Science CSD CrossRef CAS Google Scholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Xiao, H.-P. & Morsali, A. (2007). Solid State Sci. 9, 155–158. Web of Science CSD CrossRef CAS Google Scholar
Zhang, B.-S. (2004). Z. Kristallogr. New Cryst. Struct. 219, 483–484. CAS Google Scholar
Zhang, B.-S. (2005). Z. Kristallogr. New Cryst. Struct. 220, 73–74. CAS Google Scholar
Zhang, B.-S. (2006a). Acta Cryst. E62, m2645–m2647. Web of Science CSD CrossRef IUCr Journals Google Scholar
Zhang, B.-S. (2006b). Z. Kristallogr. New Cryst. Struct. 221, 191–194. CAS Google Scholar
Zhang, B.-S. (2006c). Z. Kristallogr. New Cryst. Struct. 221, 355–356. CAS Google Scholar
Zhang, B.-S., Zhu, X.-C., Yu, Y.-Y., Chen, L., Chen, Z.-B. & Hu, Y.-M. (2005). Z. Kristallogr. New Cryst. Struct. 220, 211–212. CAS Google Scholar
Zhu, H.-G., Xu, Y., Yu, Z., Wu, Q.-J., Fun, H.-K. & You, X.-Z. (1999). Polyhedron, 18, 3491–3495. Web of Science CSD CrossRef CAS Google Scholar

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