Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The structures of the sodium, potassium and rubidium complex salts of (4-fluoro­phen­oxy)acetic acid (PFPA), namely poly[μ-aqua-aqua-μ-[2-(4-fluoro­phen­oxy)acetato]-κ3O1,O2:O1′-sodium], [Na(C8H6FO3)(H2O)2]n, (I), and iso­typic poly[μ5-[2-(4-fluoro­phen­oxy)acetato]-κ5O1,O2:O1,O1′:O1′:O1′:O1′-potassium], [K(C8H6FO3)]n, (II), and poly[μ5-[2-(4-fluoro­phen­oxy)acetato]-κ5O1,O2:O1,O1′:O1′:O1′:O1′-rubidium], [Rb(C8H6FO3)]n, (III), have been determined and their coordination polymeric structures described. In the structure of (I), the very distorted octa­hedral NaO6 coordination polyhedron comprises two bidentate chelating O-atom donors (carboxyl­ate and phen­oxy) of the PFPA ligand and three O-atom donors from water mol­ecules, one mono­dentate and the other μ2-bridging between inversion-related Na centres in a cyclic manner. A bridging carboxyl­ate donor generates two-dimensional polymer layers lying parallel to (001), in which intra­layer water O—H...O hydrogen-bonding associations are also present. Structures (II) and (III) are isotypic, each having an irregular MO7 stereochemistry, with the primary metal–ligand bidentate chelate similar to that in (I) and extended into a two-dimensional polymeric layered structure, lying parallel to (100), through five additional bridging carboxyl­ate O atoms. Two of these bonds are from an O,O′-bidentate chelate inter­action and the other three are from μ3-O-atom bridges, generating cyclic links with short M...M separations [3.9064 (17) Å for (II) and 4.1001 (8) for (III)], the shortest being a centrosymmetric four-membered cyclic link. In the crystals of (I)–(III), intra­layer C—H...F inter­actions are present, but no π–π ring inter­actions are found.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617014103/cu3118sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617014103/cu3118Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617014103/cu3118IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617014103/cu3118IIIsup4.hkl
Contains datablock III

cml

Chemical Markup Language (CML) file https://doi.org/10.1107/S2053229617014103/cu3118Isup5.cml
Supplementary material

cml

Chemical Markup Language (CML) file https://doi.org/10.1107/S2053229617014103/cu3118IIsup6.cml
Supplementary material

cml

Chemical Markup Language (CML) file https://doi.org/10.1107/S2053229617014103/cu3118IIIsup7.cml
Supplementary material

CCDC references: 1577305; 1577304; 1577303

Computing details top

For all structures, data collection: CrysAlis PRO (Rigaku OD, 2014); cell refinement: CrysAlis PRO (Rigaku OD, 2014); data reduction: CrysAlis PRO (Rigaku OD, 2014). Program(s) used to solve structure: SIR92 (Altomare et al., 1993) for (I), (III); SHELXS97 (Sheldrick, 2008) for (II). For all structures, program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).

Poly[µ-aqua-aqua-µ-[2-(4-fluorophenoxy)acetato]-κ3O1,O2:O1'-sodium] (I) top
Crystal data top
[Na(C8H6FO3)(H2O)2]F(000) = 472
Mr = 228.15Dx = 1.541 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 797 reflections
a = 5.4784 (5) Åθ = 3.5–25.4°
b = 5.9139 (6) ŵ = 0.17 mm1
c = 30.379 (3) ÅT = 200 K
β = 92.540 (7)°Plate, colourless
V = 983.27 (17) Å30.30 × 0.30 × 0.03 mm
Z = 4
Data collection top
Oxford Diffraction Gemini-S CCD-detector
diffractometer
1918 independent reflections
Radiation source: Enhance (Mo) X-ray source1385 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 16.077 pixels mm-1θmax = 26.0°, θmin = 3.5°
ω scansh = 36
Absorption correction: multi-scan
(CrysAlis PRO; Rigaku OD, 2014)
k = 57
Tmin = 0.883, Tmax = 0.990l = 3729
3173 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.064Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0577P)2]
where P = (Fo2 + 2Fc2)/3
1918 reflections(Δ/σ)max < 0.001
138 parametersΔρmax = 0.26 e Å3
0 restraintsΔρmin = 0.30 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Na10.5911 (2)0.5972 (2)0.55378 (4)0.0299 (4)
F40.2056 (3)0.5094 (4)0.73896 (7)0.0517 (8)
O1W0.7177 (3)0.6601 (4)0.48056 (7)0.0311 (7)
O2W0.2745 (4)0.8641 (4)0.53340 (7)0.0322 (7)
O110.4988 (4)0.3523 (4)0.62005 (7)0.0321 (7)
O130.8176 (4)0.2708 (4)0.55680 (7)0.0318 (7)
O140.8542 (4)0.0913 (4)0.57744 (7)0.0303 (7)
C10.3259 (5)0.3815 (5)0.65147 (10)0.0274 (10)
C20.3028 (6)0.2441 (6)0.68762 (11)0.0347 (11)
C30.1228 (6)0.2868 (6)0.71733 (11)0.0364 (11)
C40.0280 (5)0.4681 (6)0.70971 (11)0.0358 (11)
C50.0101 (6)0.6078 (6)0.67394 (12)0.0423 (11)
C60.1697 (6)0.5643 (6)0.64466 (11)0.0363 (11)
C120.6249 (6)0.1416 (5)0.62169 (10)0.0304 (10)
C130.7776 (5)0.1081 (6)0.58167 (10)0.0263 (10)
H20.410400.119600.692300.0420*
H30.105000.192500.742300.0440*
H50.118900.731500.669400.0510*
H60.186600.659600.619800.0440*
H11W0.692300.796500.477000.0470*
H12W0.863500.621100.468900.0470*
H21W0.150900.872600.546200.0480*
H22W0.238300.822100.505200.0480*
H1210.504700.017000.623200.0360*
H1220.732500.135500.648700.0360*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0294 (6)0.0191 (7)0.0413 (8)0.0015 (5)0.0042 (5)0.0018 (6)
F40.0406 (11)0.0556 (15)0.0608 (14)0.0050 (10)0.0226 (9)0.0113 (12)
O1W0.0280 (11)0.0222 (12)0.0436 (14)0.0004 (9)0.0067 (9)0.0016 (11)
O2W0.0294 (11)0.0287 (13)0.0390 (13)0.0022 (9)0.0063 (9)0.0018 (11)
O110.0354 (12)0.0245 (13)0.0371 (13)0.0102 (9)0.0094 (9)0.0056 (10)
O130.0289 (11)0.0260 (13)0.0410 (14)0.0074 (9)0.0073 (9)0.0064 (11)
O140.0314 (11)0.0205 (12)0.0395 (13)0.0050 (9)0.0063 (9)0.0022 (10)
C10.0268 (15)0.0261 (17)0.0293 (18)0.0045 (13)0.0020 (12)0.0029 (15)
C20.0324 (17)0.035 (2)0.037 (2)0.0101 (14)0.0043 (13)0.0030 (16)
C30.0363 (18)0.038 (2)0.035 (2)0.0036 (15)0.0044 (14)0.0025 (16)
C40.0300 (18)0.040 (2)0.038 (2)0.0004 (15)0.0082 (14)0.0113 (17)
C50.0402 (19)0.035 (2)0.052 (2)0.0123 (17)0.0041 (16)0.0035 (19)
C60.0388 (18)0.031 (2)0.039 (2)0.0081 (15)0.0015 (14)0.0063 (16)
C120.0349 (17)0.0195 (17)0.0370 (19)0.0072 (13)0.0049 (13)0.0022 (14)
C130.0227 (15)0.0236 (18)0.0321 (18)0.0019 (13)0.0028 (12)0.0000 (14)
Geometric parameters (Å, º) top
Na1—O1W2.388 (2)O2W—H22W0.9100
Na1—O2W2.406 (3)C1—C21.377 (5)
Na1—O112.549 (3)C1—C61.389 (4)
Na1—O132.294 (3)C2—C31.389 (5)
Na1—O14i2.428 (3)C3—C41.367 (5)
Na1—O1Wii2.472 (2)C4—C51.372 (5)
F4—C41.368 (4)C5—C61.380 (5)
O11—C11.385 (4)C12—C131.519 (4)
O11—C121.425 (4)C2—H20.9500
O13—C131.249 (4)C3—H30.9500
O14—C131.260 (4)C5—H50.9500
O1W—H11W0.8200C6—H60.9500
O1W—H12W0.9200C12—H1210.9900
O2W—H21W0.8000C12—H1220.9900
O1W—Na1—O2W83.91 (8)Na1—O2W—H21W122.00
O1W—Na1—O11154.17 (9)O11—C1—C2124.5 (3)
O1W—Na1—O1389.39 (9)O11—C1—C6115.5 (3)
O1W—Na1—O14i87.96 (8)C2—C1—C6120.0 (3)
O1W—Na1—O1Wii85.66 (8)C1—C2—C3120.3 (3)
O2W—Na1—O11114.21 (8)C2—C3—C4118.3 (3)
O2W—Na1—O13160.86 (10)F4—C4—C3118.2 (3)
O2W—Na1—O14i89.44 (9)C3—C4—C5122.9 (3)
O1Wii—Na1—O2W79.81 (8)F4—C4—C5119.0 (3)
O11—Na1—O1367.43 (8)C4—C5—C6118.4 (3)
O11—Na1—O14i109.47 (8)C1—C6—C5120.1 (3)
O1Wii—Na1—O1180.07 (8)O11—C12—C13111.7 (2)
O13—Na1—O14i108.27 (9)O13—C13—C12120.1 (3)
O1Wii—Na1—O1381.82 (8)O14—C13—C12113.7 (3)
O1Wii—Na1—O14i168.02 (9)O13—C13—O14126.2 (3)
Na1—O1W—Na1ii94.34 (8)C1—C2—H2120.00
Na1—O11—C1129.73 (18)C3—C2—H2120.00
Na1—O11—C12114.32 (17)C2—C3—H3121.00
C1—O11—C12115.5 (2)C4—C3—H3121.00
Na1—O13—C13124.3 (2)C4—C5—H5121.00
Na1iii—O14—C13122.97 (19)C6—C5—H5121.00
Na1—O1W—H12W128.00C1—C6—H6120.00
H11W—O1W—H12W110.00C5—C6—H6120.00
Na1ii—O1W—H11W116.00O11—C12—H121109.00
Na1ii—O1W—H12W106.00O11—C12—H122109.00
Na1—O1W—H11W103.00C13—C12—H121109.00
Na1—O2W—H22W101.00C13—C12—H122109.00
H21W—O2W—H22W109.00H121—C12—H122108.00
O2W—Na1—O1W—Na1ii80.20 (8)O11—Na1—O1Wii—Na1ii158.39 (9)
O11—Na1—O1W—Na1ii56.4 (2)O13—Na1—O1Wii—Na1ii90.01 (9)
O13—Na1—O1W—Na1ii81.85 (9)Na1—O11—C1—C2175.8 (2)
O14i—Na1—O1W—Na1ii169.85 (8)Na1—O11—C1—C64.1 (4)
O1Wii—Na1—O1W—Na1ii0.02 (12)C12—O11—C1—C212.6 (4)
O1W—Na1—O11—C1147.6 (2)C12—O11—C1—C6167.6 (3)
O1W—Na1—O11—C1224.2 (3)Na1—O11—C12—C132.8 (3)
O2W—Na1—O11—C116.1 (3)C1—O11—C12—C13170.2 (2)
O2W—Na1—O11—C12155.62 (18)Na1—O13—C13—O14161.6 (2)
O13—Na1—O11—C1175.3 (2)Na1—O13—C13—C1218.9 (4)
O13—Na1—O11—C123.59 (18)Na1iii—O14—C13—O13107.3 (3)
O14i—Na1—O11—C182.4 (2)Na1iii—O14—C13—C1273.1 (3)
O14i—Na1—O11—C12105.91 (19)O11—C1—C2—C3179.8 (3)
O1Wii—Na1—O11—C190.1 (2)C6—C1—C2—C30.3 (5)
O1Wii—Na1—O11—C1281.61 (19)O11—C1—C6—C5179.7 (3)
O1W—Na1—O13—C13156.1 (2)C2—C1—C6—C50.4 (5)
O11—Na1—O13—C1312.2 (2)C1—C2—C3—C40.3 (5)
O14i—Na1—O13—C13116.2 (2)C2—C3—C4—F4179.8 (3)
O1Wii—Na1—O13—C1370.4 (2)C2—C3—C4—C50.5 (5)
O1W—Na1—O14i—C13i95.5 (2)F4—C4—C5—C6180.0 (3)
O2W—Na1—O14i—C13i11.6 (2)C3—C4—C5—C60.7 (5)
O11—Na1—O14i—C13i104.0 (2)C4—C5—C6—C10.6 (5)
O13—Na1—O14i—C13i175.8 (2)O11—C12—C13—O1313.2 (4)
O1W—Na1—O1Wii—Na1ii0.00 (7)O11—C12—C13—O14167.2 (2)
O2W—Na1—O1Wii—Na1ii84.58 (8)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1, z+1; (iii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11W···O2Wiv0.822.042.846 (3)165
O1W—H12W···O13v0.922.052.862 (3)147
O2W—H21W···O14vi0.801.932.727 (3)177
O2W—H22W···O13ii0.911.972.877 (3)176
C3—H3···F4vii0.952.533.154 (4)123
Symmetry codes: (ii) x+1, y+1, z+1; (iv) x+1, y+2, z+1; (v) x+2, y+1, z+1; (vi) x1, y+1, z; (vii) x1/2, y1/2, z+3/2.
Poly[µ5-[2-(4-fluorophenoxy)acetato]-κ5O1,O2:O1,O1':O1':O1':O1'-potassium] (II) top
Crystal data top
[K(C8H6FO3)]F(000) = 424
Mr = 208.23Dx = 1.647 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 802 reflections
a = 18.3542 (15) Åθ = 4.4–27.8°
b = 6.9466 (8) ŵ = 0.62 mm1
c = 6.5969 (5) ÅT = 200 K
β = 92.995 (7)°Plate, colourless
V = 839.94 (13) Å30.30 × 0.16 × 0.08 mm
Z = 4
Data collection top
Oxford Diffraction Gemini-S CCD-detector
diffractometer
1647 independent reflections
Radiation source: Enhance (Mo) X-ray source1354 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 16.077 pixels mm-1θmax = 26.0°, θmin = 3.1°
ω scansh = 2222
Absorption correction: multi-scan
(CrysAlis PRO; Rigaku OD, 2014)
k = 88
Tmin = 0.896, Tmax = 0.990l = 78
1647 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.081Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.199H-atom parameters constrained
S = 1.20 w = 1/[σ2(Fo2) + (0.0535P)2 + 3.5272P]
where P = (Fo2 + 2Fc2)/3
1647 reflections(Δ/σ)max < 0.001
119 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = 0.64 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.56245 (6)0.47997 (19)0.24806 (18)0.0289 (4)
F40.9737 (2)0.4952 (7)0.1957 (6)0.0564 (14)
O110.7007 (2)0.4839 (7)0.4894 (6)0.0339 (13)
O130.5763 (2)0.3954 (6)0.6505 (6)0.0330 (14)
O140.5884 (2)0.6318 (7)0.8797 (6)0.0340 (13)
C10.7706 (3)0.4988 (9)0.4222 (8)0.0309 (19)
C20.8274 (3)0.5930 (10)0.5270 (9)0.0340 (19)
C30.8966 (3)0.5907 (11)0.4485 (9)0.0396 (19)
C40.9064 (3)0.4968 (11)0.2703 (10)0.0406 (19)
C50.8507 (4)0.4057 (10)0.1637 (10)0.040 (2)
C60.7815 (3)0.4059 (10)0.2397 (9)0.0373 (19)
C120.6873 (3)0.5768 (10)0.6755 (8)0.0310 (19)
C130.6105 (3)0.5301 (9)0.7406 (8)0.0294 (19)
H20.819500.658300.650400.0410*
H30.936400.653700.518400.0480*
H50.859100.343100.039100.0490*
H60.742100.343100.167700.0450*
H1210.692500.717700.659300.0370*
H1220.723700.533600.781900.0370*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0266 (6)0.0432 (8)0.0167 (6)0.0012 (6)0.0008 (4)0.0015 (6)
F40.036 (2)0.090 (3)0.045 (2)0.008 (2)0.0202 (17)0.004 (2)
O110.0231 (19)0.058 (3)0.0207 (19)0.0021 (19)0.0022 (15)0.008 (2)
O130.031 (2)0.046 (3)0.022 (2)0.0031 (19)0.0019 (16)0.002 (2)
O140.033 (2)0.055 (3)0.0146 (18)0.002 (2)0.0073 (16)0.004 (2)
C10.026 (3)0.049 (4)0.018 (3)0.006 (3)0.003 (2)0.002 (3)
C20.026 (3)0.052 (4)0.024 (3)0.001 (3)0.002 (2)0.005 (3)
C30.029 (3)0.065 (4)0.025 (3)0.002 (3)0.003 (2)0.003 (3)
C40.030 (3)0.058 (4)0.034 (3)0.012 (3)0.005 (3)0.008 (3)
C50.045 (4)0.053 (4)0.024 (3)0.010 (3)0.009 (3)0.005 (3)
C60.030 (3)0.054 (4)0.027 (3)0.000 (3)0.006 (2)0.010 (3)
C120.025 (3)0.053 (4)0.015 (3)0.001 (3)0.001 (2)0.003 (3)
C130.025 (3)0.046 (4)0.017 (3)0.002 (3)0.002 (2)0.008 (3)
Geometric parameters (Å, º) top
K1—O112.924 (4)C1—C61.390 (8)
K1—O132.718 (4)C2—C31.397 (8)
K1—O14i2.714 (4)C3—C41.365 (9)
K1—O13ii2.804 (4)C4—C51.366 (9)
K1—O14ii2.956 (4)C5—C61.390 (9)
K1—O13iii2.701 (4)C12—C131.530 (8)
K1—O14iv2.866 (5)C2—H20.9500
F4—C41.353 (7)C3—H30.9500
O11—C11.383 (7)C5—H50.9500
O11—C121.420 (7)C6—H60.9500
O13—C131.259 (7)C12—H1210.9900
O14—C131.243 (7)C12—H1220.9900
C1—C21.385 (8)
O11—K1—O1355.67 (11)K1vii—O14—C13111.5 (4)
O11—K1—O14i107.22 (12)K1vi—O14—K1ii87.00 (12)
O11—K1—O13ii129.81 (12)K1vi—O14—K1vii127.08 (16)
O11—K1—O14ii158.59 (13)K1ii—O14—K1vii91.29 (12)
O11—K1—O13iii92.81 (13)O11—C1—C2124.2 (5)
O11—K1—O14iv72.57 (13)O11—C1—C6114.9 (5)
O13—K1—O14i161.22 (13)C2—C1—C6120.9 (5)
O13—K1—O13ii82.73 (12)C1—C2—C3119.0 (6)
O13—K1—O14ii105.08 (12)C2—C3—C4119.2 (6)
O13—K1—O13iii91.08 (13)F4—C4—C3118.8 (5)
O13—K1—O14iv84.37 (12)F4—C4—C5118.8 (6)
O13ii—K1—O14i107.33 (12)C3—C4—C5122.4 (6)
O14i—K1—O14ii93.00 (12)C4—C5—C6119.2 (6)
O13iii—K1—O14i97.97 (14)C1—C6—C5119.3 (6)
O14i—K1—O14iv82.61 (13)O11—C12—C13110.5 (5)
O13ii—K1—O14ii45.58 (12)O13—C13—O14126.7 (5)
O13ii—K1—O13iii116.93 (12)O13—C13—C12118.0 (5)
O13ii—K1—O14iv77.04 (12)O14—C13—C12115.3 (5)
O13iii—K1—O14ii77.11 (12)C1—C2—H2121.00
O14ii—K1—O14iv118.17 (13)C3—C2—H2120.00
O13iii—K1—O14iv164.71 (12)C2—C3—H3120.00
K1—O11—C1128.3 (3)C4—C3—H3120.00
K1—O11—C12106.9 (3)C4—C5—H5120.00
C1—O11—C12116.7 (4)C6—C5—H5120.00
K1—O13—C13108.6 (3)C1—C6—H6120.00
K1—O13—K1ii97.28 (12)C5—C6—H6120.00
K1—O13—K1v115.87 (15)O11—C12—H121110.00
K1ii—O13—C1395.4 (3)O11—C12—H122110.00
K1v—O13—C13131.0 (4)C13—C12—H121110.00
K1ii—O13—K1v98.24 (13)C13—C12—H122110.00
K1vi—O14—C13121.3 (4)H121—C12—H122108.00
K1ii—O14—C1388.7 (3)
O13—K1—O11—C1169.5 (5)O13vii—K1vii—O14—C13158.7 (4)
O14i—K1—O11—C119.1 (5)O14iii—K1v—O13—C13133.5 (4)
O13ii—K1—O11—C1150.8 (4)O11vi—K1vi—O14—C1386.2 (4)
O14ii—K1—O11—C1141.0 (5)O13v—K1vi—O14—C139.2 (4)
O13iii—K1—O11—C180.1 (5)O14vii—K1vi—O14—C13155.3 (4)
O14iv—K1—O11—C195.4 (5)O13—K1ii—O14—C1310.0 (3)
O13—K1—O11—C1243.7 (3)O11v—K1v—O13—K1127.46 (15)
O14i—K1—O11—C12127.6 (4)O13v—K1v—O13—K1176.86 (15)
O13ii—K1—O11—C124.0 (4)O11vii—K1vii—O14—C13103.0 (4)
O14ii—K1—O11—C1272.3 (5)O11v—K1v—O13—C1325.7 (5)
O13iii—K1—O11—C12133.1 (4)O13v—K1v—O13—C1330.0 (5)
O14iv—K1—O11—C1251.4 (4)O14viii—K1vii—O14—C1397.2 (4)
O14—K1ii—O13—C139.9 (3)O14iv—K1vii—O14—C137.7 (4)
O13viii—K1ii—O13—C1322.1 (4)K1—O11—C1—C636.0 (7)
O11ii—K1ii—O13—C13141.8 (3)C12—O11—C1—C6180.0 (5)
O13ii—K1ii—O13—C13109.6 (3)K1—O11—C1—C2145.8 (5)
O14—K1ii—O13—K1v122.9 (2)K1—O11—C12—C1334.7 (5)
O14iii—K1v—O13—K119.64 (16)C12—O11—C1—C21.8 (9)
O11—K1—O13—C1352.1 (3)C1—O11—C12—C13174.1 (5)
O13ii—K1—O13—C1398.3 (4)K1v—O13—C13—C1295.5 (6)
O14ii—K1—O13—C13138.3 (3)K1ii—O13—C13—O1421.3 (6)
O13iii—K1—O13—C13144.7 (4)K1—O13—C13—O14120.9 (6)
O14iv—K1—O13—C1320.7 (3)K1—O13—C13—C1259.1 (5)
O11—K1—O13—K1ii150.32 (19)K1ii—O13—C13—C12158.7 (4)
O13ii—K1—O13—K1ii0.00 (13)K1v—O13—C13—O1484.6 (7)
O14ii—K1—O13—K1ii40.08 (16)K1vii—O14—C13—C1269.1 (5)
O13iii—K1—O13—K1ii117.02 (13)K1vi—O14—C13—O1365.6 (7)
O14iv—K1—O13—K1ii77.61 (13)K1vi—O14—C13—C12114.4 (5)
O11—K1—O13—K1v106.83 (19)K1ii—O14—C13—O1320.1 (6)
O13ii—K1—O13—K1v102.85 (16)K1ii—O14—C13—C12159.9 (4)
O14ii—K1—O13—K1v62.77 (17)K1vii—O14—C13—O13110.9 (6)
O13iii—K1—O13—K1v14.17 (15)O11—C1—C2—C3177.0 (6)
O14iv—K1—O13—K1v179.54 (16)C6—C1—C2—C31.1 (10)
O13viii—K1ii—O14—C13141.1 (4)O11—C1—C6—C5177.3 (6)
O11ii—K1ii—O14—C1377.6 (5)C2—C1—C6—C50.9 (10)
O13ii—K1ii—O14—C1353.5 (4)C1—C2—C3—C40.4 (10)
O13—K1ii—O14—K1vi111.5 (2)C2—C3—C4—F4179.9 (6)
O13—K1ii—O14—K1vii121.46 (18)C2—C3—C4—C50.6 (11)
O13viii—K1vii—O14—C13117.5 (4)F4—C4—C5—C6179.7 (6)
O14—K1ii—O13—K1119.5 (2)C3—C4—C5—C60.8 (11)
O13viii—K1ii—O13—K187.51 (15)C4—C5—C6—C10.0 (10)
O11ii—K1ii—O13—K132.2 (2)O11—C12—C13—O1313.0 (7)
O13ii—K1ii—O13—K10.00 (13)O11—C12—C13—O14167.0 (5)
Symmetry codes: (i) x, y, z1; (ii) x+1, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x, y+3/2, z1/2; (v) x, y+1/2, z+1/2; (vi) x, y, z+1; (vii) x, y+3/2, z+1/2; (viii) x+1, y+1/2, z+3/2.
Poly[µ5-[2-(4-fluorophenoxy)acetato]-κ5O1,O2:O1,O1':O1':O1':O1'-rubidium] (III) top
Crystal data top
[Rb(C8H6FO3)]F(000) = 496
Mr = 254.60Dx = 1.915 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1154 reflections
a = 18.0011 (16) Åθ = 3.4–28.0°
b = 7.1625 (4) ŵ = 5.59 mm1
c = 6.8548 (4) ÅT = 200 K
β = 91.995 (7)°Plate, colourless
V = 883.27 (11) Å30.35 × 0.30 × 0.03 mm
Z = 4
Data collection top
Oxford Diffraction Gemini-S CCD-detector
diffractometer
1735 independent reflections
Radiation source: Enhance (Mo) X-ray source1315 reflections with I > 2]s(I)
Graphite monochromatorRint = 0.051
Detector resolution: 16.07 pixels mm-1θmax = 26.0°, θmin = 3.4°
ω scansh = 2215
Absorption correction: multi-scan
(CrysAlis PRO; Rigaku OD, 2014)
k = 88
Tmin = 0.42, Tmax = 0.98l = 68
3411 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H-atom parameters constrained
S = 0.97 w = 1/[σ2(Fo2) + (0.0365P)2]
where P = (Fo2 + 2Fc2)/3
1735 reflections(Δ/σ)max = 0.001
118 parametersΔρmax = 1.17 e Å3
0 restraintsΔρmin = 0.64 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rb10.56818 (3)0.47364 (7)0.24428 (7)0.0324 (2)
F40.9883 (2)0.5090 (5)0.1990 (5)0.0584 (16)
O110.7111 (2)0.4808 (5)0.4986 (5)0.0350 (12)
O130.5819 (2)0.4066 (5)0.6572 (5)0.0389 (14)
O140.5951 (2)0.6396 (5)0.8734 (5)0.0352 (14)
C10.7813 (3)0.4990 (6)0.4306 (7)0.0304 (19)
C20.8368 (4)0.6086 (7)0.5143 (8)0.0374 (19)
C30.9064 (4)0.6096 (8)0.4355 (8)0.040 (2)
C40.9192 (3)0.5044 (8)0.2744 (8)0.040 (2)
C50.8652 (4)0.3972 (8)0.1876 (8)0.044 (2)
C60.7954 (4)0.3956 (7)0.2643 (8)0.0384 (19)
C120.6952 (3)0.5806 (7)0.6728 (7)0.0321 (19)
C130.6176 (4)0.5380 (7)0.7386 (8)0.0323 (19)
H20.827200.682900.625500.0450*
H30.945200.683200.493300.0480*
H50.875400.324600.075700.0520*
H60.756900.323500.203300.0460*
H110.699800.716300.648800.0380*
H120.731800.545900.777500.0380*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0407 (4)0.0287 (3)0.0277 (3)0.0011 (2)0.0006 (2)0.0002 (2)
F40.044 (3)0.086 (3)0.046 (2)0.009 (2)0.0113 (18)0.0016 (18)
O110.032 (2)0.039 (2)0.034 (2)0.0015 (18)0.0004 (17)0.0097 (16)
O130.047 (3)0.031 (2)0.039 (2)0.0084 (18)0.0066 (19)0.0007 (17)
O140.045 (3)0.033 (2)0.028 (2)0.0004 (18)0.0072 (18)0.0026 (16)
C10.036 (4)0.030 (3)0.025 (3)0.004 (3)0.000 (2)0.001 (2)
C20.039 (4)0.040 (3)0.033 (3)0.001 (3)0.001 (3)0.005 (2)
C30.034 (4)0.051 (4)0.035 (3)0.003 (3)0.001 (3)0.001 (3)
C40.035 (4)0.048 (4)0.038 (3)0.010 (3)0.004 (3)0.008 (3)
C50.054 (5)0.042 (3)0.035 (3)0.008 (3)0.006 (3)0.008 (3)
C60.045 (4)0.033 (3)0.037 (3)0.000 (3)0.000 (3)0.005 (2)
C120.037 (4)0.027 (3)0.032 (3)0.001 (2)0.001 (3)0.009 (2)
C130.044 (4)0.024 (3)0.029 (3)0.003 (3)0.004 (2)0.008 (2)
Geometric parameters (Å, º) top
Rb1—O113.058 (4)C1—C61.390 (7)
Rb1—O132.873 (3)C2—C31.382 (10)
Rb1—O14i2.863 (4)C3—C41.363 (8)
Rb1—O13ii2.936 (4)C4—C51.360 (8)
Rb1—O14ii3.128 (4)C5—C61.379 (10)
Rb1—O13iii2.801 (4)C12—C131.514 (9)
Rb1—O14iv2.943 (4)C2—H20.9500
F4—C41.364 (6)C3—H30.9500
O11—C11.368 (6)C5—H50.9500
O11—C121.429 (6)C6—H60.9500
O13—C131.259 (7)C12—H110.9900
O14—C131.254 (7)C12—H120.9900
C1—C21.380 (8)
O11—Rb1—O1353.08 (10)Rb1vii—O14—C13112.2 (3)
O11—Rb1—O14i109.53 (10)Rb1vi—O14—Rb1ii86.26 (9)
O11—Rb1—O13ii128.81 (10)Rb1vi—O14—Rb1vii128.80 (13)
O11—Rb1—O14ii156.34 (9)Rb1ii—O14—Rb1vii91.32 (10)
O11—Rb1—O13iii93.39 (10)O11—C1—C2125.2 (5)
O11—Rb1—O14iv71.72 (10)O11—C1—C6115.2 (5)
O13—Rb1—O14i158.88 (10)C2—C1—C6119.6 (5)
O13—Rb1—O13ii82.56 (10)C1—C2—C3119.6 (5)
O13—Rb1—O14ii104.98 (10)C2—C3—C4119.7 (6)
O13—Rb1—O13iii92.42 (10)F4—C4—C3118.4 (5)
O13—Rb1—O14iv81.57 (10)F4—C4—C5119.7 (5)
O13ii—Rb1—O14i105.58 (10)C3—C4—C5121.9 (6)
O14i—Rb1—O14ii93.74 (10)C4—C5—C6119.0 (5)
O13iii—Rb1—O14i101.28 (10)C1—C6—C5120.2 (6)
O14i—Rb1—O14iv81.09 (10)O11—C12—C13111.2 (4)
O13ii—Rb1—O14ii43.20 (9)O13—C13—O14126.0 (6)
O13ii—Rb1—O13iii114.95 (10)O13—C13—C12118.7 (5)
O13ii—Rb1—O14iv78.41 (10)O14—C13—C12115.3 (5)
O13iii—Rb1—O14ii77.40 (10)C1—C2—H2120.00
O14ii—Rb1—O14iv117.71 (10)C3—C2—H2120.00
O13iii—Rb1—O14iv164.69 (10)C2—C3—H3120.00
Rb1—O11—C1125.2 (3)C4—C3—H3120.00
Rb1—O11—C12107.2 (3)C4—C5—H5120.00
C1—O11—C12116.8 (4)C6—C5—H5121.00
Rb1—O13—C13109.7 (3)C1—C6—H6120.00
Rb1—O13—Rb1ii97.45 (11)C5—C6—H6120.00
Rb1—O13—Rb1v111.55 (12)O11—C12—H11109.00
Rb1ii—O13—C1398.0 (4)O11—C12—H12109.00
Rb1v—O13—C13132.8 (3)C13—C12—H11109.00
Rb1ii—O13—Rb1v98.42 (11)C13—C12—H12109.00
Rb1vi—O14—C13118.8 (3)H11—C12—H12108.00
Rb1ii—O14—C1389.1 (4)
O13—Rb1—O11—C1173.2 (4)O13—Rb1—O14ii—C13ii51.2 (3)
O13—Rb1—O11—C1244.0 (3)O11—Rb1—O13iii—Rb1iii129.02 (12)
O14i—Rb1—O11—C120.5 (3)O11—Rb1—O13iii—C13iii20.3 (5)
O14i—Rb1—O11—C12122.3 (3)O13—Rb1—O13iii—Rb1iii177.83 (13)
O13ii—Rb1—O11—C1151.1 (3)O13—Rb1—O13iii—C13iii32.9 (5)
O13ii—Rb1—O11—C128.4 (3)O11—Rb1—O14iv—C13iv106.0 (4)
O14ii—Rb1—O11—C1148.6 (3)O11—Rb1—O14iv—Rb1vii78.18 (16)
O14ii—Rb1—O11—C1268.7 (4)O13—Rb1—O14iv—C13iv159.8 (4)
O13iii—Rb1—O11—C182.7 (3)O13—Rb1—O14iv—Rb1vii24.38 (16)
O13iii—Rb1—O11—C12134.5 (3)Rb1—O11—C1—C2138.1 (4)
O14iv—Rb1—O11—C193.6 (3)Rb1—O11—C1—C642.2 (5)
O14iv—Rb1—O11—C1249.1 (3)C12—O11—C1—C21.5 (7)
O11—Rb1—O13—C1351.4 (4)C12—O11—C1—C6178.2 (4)
O11—Rb1—O13—Rb1ii152.73 (16)Rb1—O11—C12—C1337.4 (4)
O11—Rb1—O13—Rb1v105.13 (16)C1—O11—C12—C13176.3 (4)
O14i—Rb1—O13—C1313.1 (5)Rb1—O13—C13—O14122.7 (5)
O14i—Rb1—O13—Rb1ii114.4 (3)Rb1—O13—C13—C1257.8 (5)
O14i—Rb1—O13—Rb1v143.5 (2)Rb1ii—O13—C13—O1421.8 (6)
O13ii—Rb1—O13—C13101.3 (4)Rb1ii—O13—C13—C12158.7 (4)
O13ii—Rb1—O13—Rb1ii0.00 (10)Rb1v—O13—C13—O1487.6 (7)
O13ii—Rb1—O13—Rb1v102.14 (13)Rb1v—O13—C13—C1291.9 (5)
O14ii—Rb1—O13—C13138.5 (4)Rb1vi—O14—C13—O1365.0 (7)
O14ii—Rb1—O13—Rb1ii37.25 (12)Rb1vi—O14—C13—C12114.5 (4)
O14ii—Rb1—O13—Rb1v64.90 (14)Rb1ii—O14—C13—O1320.2 (6)
O13iii—Rb1—O13—C13143.9 (4)Rb1ii—O14—C13—C12160.3 (4)
O13iii—Rb1—O13—Rb1ii114.85 (11)Rb1vii—O14—C13—O13111.3 (5)
O13iii—Rb1—O13—Rb1v12.71 (13)Rb1vii—O14—C13—C1269.2 (5)
O14iv—Rb1—O13—C1322.0 (4)O11—C1—C2—C3177.6 (5)
O14iv—Rb1—O13—Rb1ii79.31 (11)C6—C1—C2—C32.1 (8)
O14iv—Rb1—O13—Rb1v178.55 (14)O11—C1—C6—C5177.3 (5)
O11—Rb1—O14i—C13i88.7 (4)C2—C1—C6—C52.4 (8)
O11—Rb1—O14i—Rb1iv95.68 (16)C1—C2—C3—C40.9 (8)
O13—Rb1—O14i—C13i120.5 (5)C2—C3—C4—F4179.6 (5)
O13—Rb1—O14i—Rb1iv64.0 (4)C2—C3—C4—C50.0 (9)
O11—Rb1—O13ii—Rb1ii28.05 (16)F4—C4—C5—C6179.3 (5)
O11—Rb1—O13ii—C13ii139.2 (3)C3—C4—C5—C60.3 (9)
O13—Rb1—O13ii—Rb1ii0.00 (10)C4—C5—C6—C11.5 (8)
O13—Rb1—O13ii—C13ii111.2 (3)O11—C12—C13—O1310.4 (7)
O11—Rb1—O14ii—C13ii71.3 (4)O11—C12—C13—O14170.1 (4)
Symmetry codes: (i) x, y, z1; (ii) x+1, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x, y+3/2, z1/2; (v) x, y+1/2, z+1/2; (vi) x, y, z+1; (vii) x, y+3/2, z+1/2.
 

Subscribe to Acta Crystallographica Section C: Structural Chemistry

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds