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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]-κ
3O1,
O2:
O1′-sodium], [Na(C
8H
6FO
3)(H
2O)
2]
n, (I), and isotypic poly[μ
5-[2-(4-fluorophenoxy)acetato]-κ
5O1,
O2:
O1,
O1′:
O1′:
O1′:
O1′-potassium], [K(C
8H
6FO
3)]
n, (II), and poly[μ
5-[2-(4-fluorophenoxy)acetato]-κ
5O1,
O2:
O1,
O1′:
O1′:
O1′:
O1′-rubidium], [Rb(C
8H
6FO
3)]
n, (III), have been determined and their coordination polymeric structures described. In the structure of (I), the very distorted octahedral NaO
6 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 μ
2-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
MO
7 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 μ
3-O-atom bridges, generating cyclic links with short
MM 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
CCDC references: 1577305; 1577304; 1577303
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 = 228.15 | Dx = 1.541 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 797 reflections |
a = 5.4784 (5) Å | θ = 3.5–25.4° |
b = 5.9139 (6) Å | µ = 0.17 mm−1 |
c = 30.379 (3) Å | T = 200 K |
β = 92.540 (7)° | Plate, colourless |
V = 983.27 (17) Å3 | 0.30 × 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 source | 1385 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.5° |
ω scans | h = −3→6 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2014) | k = −5→7 |
Tmin = 0.883, Tmax = 0.990 | l = −37→29 |
3173 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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.143 | H-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 parameters | Δρmax = 0.26 e Å−3 |
0 restraints | Δρmin = −0.30 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Na1 | 0.5911 (2) | 0.5972 (2) | 0.55378 (4) | 0.0299 (4) | |
F4 | −0.2056 (3) | 0.5094 (4) | 0.73896 (7) | 0.0517 (8) | |
O1W | 0.7177 (3) | 0.6601 (4) | 0.48056 (7) | 0.0311 (7) | |
O2W | 0.2745 (4) | 0.8641 (4) | 0.53340 (7) | 0.0322 (7) | |
O11 | 0.4988 (4) | 0.3523 (4) | 0.62005 (7) | 0.0321 (7) | |
O13 | 0.8176 (4) | 0.2708 (4) | 0.55680 (7) | 0.0318 (7) | |
O14 | 0.8542 (4) | −0.0913 (4) | 0.57744 (7) | 0.0303 (7) | |
C1 | 0.3259 (5) | 0.3815 (5) | 0.65147 (10) | 0.0274 (10) | |
C2 | 0.3028 (6) | 0.2441 (6) | 0.68762 (11) | 0.0347 (11) | |
C3 | 0.1228 (6) | 0.2868 (6) | 0.71733 (11) | 0.0364 (11) | |
C4 | −0.0280 (5) | 0.4681 (6) | 0.70971 (11) | 0.0358 (11) | |
C5 | −0.0101 (6) | 0.6078 (6) | 0.67394 (12) | 0.0423 (11) | |
C6 | 0.1697 (6) | 0.5643 (6) | 0.64466 (11) | 0.0363 (11) | |
C12 | 0.6249 (6) | 0.1416 (5) | 0.62169 (10) | 0.0304 (10) | |
C13 | 0.7776 (5) | 0.1081 (6) | 0.58167 (10) | 0.0263 (10) | |
H2 | 0.41040 | 0.11960 | 0.69230 | 0.0420* | |
H3 | 0.10500 | 0.19250 | 0.74230 | 0.0440* | |
H5 | −0.11890 | 0.73150 | 0.66940 | 0.0510* | |
H6 | 0.18660 | 0.65960 | 0.61980 | 0.0440* | |
H11W | 0.69230 | 0.79650 | 0.47700 | 0.0470* | |
H12W | 0.86350 | 0.62110 | 0.46890 | 0.0470* | |
H21W | 0.15090 | 0.87260 | 0.54620 | 0.0480* | |
H22W | 0.23830 | 0.82210 | 0.50520 | 0.0480* | |
H121 | 0.50470 | 0.01700 | 0.62320 | 0.0360* | |
H122 | 0.73250 | 0.13550 | 0.64870 | 0.0360* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0294 (6) | 0.0191 (7) | 0.0413 (8) | 0.0015 (5) | 0.0042 (5) | 0.0018 (6) |
F4 | 0.0406 (11) | 0.0556 (15) | 0.0608 (14) | 0.0050 (10) | 0.0226 (9) | −0.0113 (12) |
O1W | 0.0280 (11) | 0.0222 (12) | 0.0436 (14) | 0.0004 (9) | 0.0067 (9) | 0.0016 (11) |
O2W | 0.0294 (11) | 0.0287 (13) | 0.0390 (13) | 0.0022 (9) | 0.0063 (9) | −0.0018 (11) |
O11 | 0.0354 (12) | 0.0245 (13) | 0.0371 (13) | 0.0102 (9) | 0.0094 (9) | 0.0056 (10) |
O13 | 0.0289 (11) | 0.0260 (13) | 0.0410 (14) | 0.0074 (9) | 0.0073 (9) | 0.0064 (11) |
O14 | 0.0314 (11) | 0.0205 (12) | 0.0395 (13) | 0.0050 (9) | 0.0063 (9) | −0.0022 (10) |
C1 | 0.0268 (15) | 0.0261 (17) | 0.0293 (18) | 0.0045 (13) | 0.0020 (12) | −0.0029 (15) |
C2 | 0.0324 (17) | 0.035 (2) | 0.037 (2) | 0.0101 (14) | 0.0043 (13) | 0.0030 (16) |
C3 | 0.0363 (18) | 0.038 (2) | 0.035 (2) | 0.0036 (15) | 0.0044 (14) | 0.0025 (16) |
C4 | 0.0300 (18) | 0.040 (2) | 0.038 (2) | 0.0004 (15) | 0.0082 (14) | −0.0113 (17) |
C5 | 0.0402 (19) | 0.035 (2) | 0.052 (2) | 0.0123 (17) | 0.0041 (16) | −0.0035 (19) |
C6 | 0.0388 (18) | 0.031 (2) | 0.039 (2) | 0.0081 (15) | 0.0015 (14) | 0.0063 (16) |
C12 | 0.0349 (17) | 0.0195 (17) | 0.0370 (19) | 0.0072 (13) | 0.0049 (13) | 0.0022 (14) |
C13 | 0.0227 (15) | 0.0236 (18) | 0.0321 (18) | 0.0019 (13) | −0.0028 (12) | 0.0000 (14) |
Geometric parameters (Å, º) top
Na1—O1W | 2.388 (2) | O2W—H22W | 0.9100 |
Na1—O2W | 2.406 (3) | C1—C2 | 1.377 (5) |
Na1—O11 | 2.549 (3) | C1—C6 | 1.389 (4) |
Na1—O13 | 2.294 (3) | C2—C3 | 1.389 (5) |
Na1—O14i | 2.428 (3) | C3—C4 | 1.367 (5) |
Na1—O1Wii | 2.472 (2) | C4—C5 | 1.372 (5) |
F4—C4 | 1.368 (4) | C5—C6 | 1.380 (5) |
O11—C1 | 1.385 (4) | C12—C13 | 1.519 (4) |
O11—C12 | 1.425 (4) | C2—H2 | 0.9500 |
O13—C13 | 1.249 (4) | C3—H3 | 0.9500 |
O14—C13 | 1.260 (4) | C5—H5 | 0.9500 |
O1W—H11W | 0.8200 | C6—H6 | 0.9500 |
O1W—H12W | 0.9200 | C12—H121 | 0.9900 |
O2W—H21W | 0.8000 | C12—H122 | 0.9900 |
| | | |
O1W—Na1—O2W | 83.91 (8) | Na1—O2W—H21W | 122.00 |
O1W—Na1—O11 | 154.17 (9) | O11—C1—C2 | 124.5 (3) |
O1W—Na1—O13 | 89.39 (9) | O11—C1—C6 | 115.5 (3) |
O1W—Na1—O14i | 87.96 (8) | C2—C1—C6 | 120.0 (3) |
O1W—Na1—O1Wii | 85.66 (8) | C1—C2—C3 | 120.3 (3) |
O2W—Na1—O11 | 114.21 (8) | C2—C3—C4 | 118.3 (3) |
O2W—Na1—O13 | 160.86 (10) | F4—C4—C3 | 118.2 (3) |
O2W—Na1—O14i | 89.44 (9) | C3—C4—C5 | 122.9 (3) |
O1Wii—Na1—O2W | 79.81 (8) | F4—C4—C5 | 119.0 (3) |
O11—Na1—O13 | 67.43 (8) | C4—C5—C6 | 118.4 (3) |
O11—Na1—O14i | 109.47 (8) | C1—C6—C5 | 120.1 (3) |
O1Wii—Na1—O11 | 80.07 (8) | O11—C12—C13 | 111.7 (2) |
O13—Na1—O14i | 108.27 (9) | O13—C13—C12 | 120.1 (3) |
O1Wii—Na1—O13 | 81.82 (8) | O14—C13—C12 | 113.7 (3) |
O1Wii—Na1—O14i | 168.02 (9) | O13—C13—O14 | 126.2 (3) |
Na1—O1W—Na1ii | 94.34 (8) | C1—C2—H2 | 120.00 |
Na1—O11—C1 | 129.73 (18) | C3—C2—H2 | 120.00 |
Na1—O11—C12 | 114.32 (17) | C2—C3—H3 | 121.00 |
C1—O11—C12 | 115.5 (2) | C4—C3—H3 | 121.00 |
Na1—O13—C13 | 124.3 (2) | C4—C5—H5 | 121.00 |
Na1iii—O14—C13 | 122.97 (19) | C6—C5—H5 | 121.00 |
Na1—O1W—H12W | 128.00 | C1—C6—H6 | 120.00 |
H11W—O1W—H12W | 110.00 | C5—C6—H6 | 120.00 |
Na1ii—O1W—H11W | 116.00 | O11—C12—H121 | 109.00 |
Na1ii—O1W—H12W | 106.00 | O11—C12—H122 | 109.00 |
Na1—O1W—H11W | 103.00 | C13—C12—H121 | 109.00 |
Na1—O2W—H22W | 101.00 | C13—C12—H122 | 109.00 |
H21W—O2W—H22W | 109.00 | H121—C12—H122 | 108.00 |
| | | |
O2W—Na1—O1W—Na1ii | −80.20 (8) | O11—Na1—O1Wii—Na1ii | −158.39 (9) |
O11—Na1—O1W—Na1ii | 56.4 (2) | O13—Na1—O1Wii—Na1ii | −90.01 (9) |
O13—Na1—O1W—Na1ii | 81.85 (9) | Na1—O11—C1—C2 | −175.8 (2) |
O14i—Na1—O1W—Na1ii | −169.85 (8) | Na1—O11—C1—C6 | 4.1 (4) |
O1Wii—Na1—O1W—Na1ii | 0.02 (12) | C12—O11—C1—C2 | 12.6 (4) |
O1W—Na1—O11—C1 | −147.6 (2) | C12—O11—C1—C6 | −167.6 (3) |
O1W—Na1—O11—C12 | 24.2 (3) | Na1—O11—C12—C13 | −2.8 (3) |
O2W—Na1—O11—C1 | −16.1 (3) | C1—O11—C12—C13 | 170.2 (2) |
O2W—Na1—O11—C12 | 155.62 (18) | Na1—O13—C13—O14 | 161.6 (2) |
O13—Na1—O11—C1 | −175.3 (2) | Na1—O13—C13—C12 | −18.9 (4) |
O13—Na1—O11—C12 | −3.59 (18) | Na1iii—O14—C13—O13 | −107.3 (3) |
O14i—Na1—O11—C1 | 82.4 (2) | Na1iii—O14—C13—C12 | 73.1 (3) |
O14i—Na1—O11—C12 | −105.91 (19) | O11—C1—C2—C3 | −179.8 (3) |
O1Wii—Na1—O11—C1 | −90.1 (2) | C6—C1—C2—C3 | 0.3 (5) |
O1Wii—Na1—O11—C12 | 81.61 (19) | O11—C1—C6—C5 | 179.7 (3) |
O1W—Na1—O13—C13 | −156.1 (2) | C2—C1—C6—C5 | −0.4 (5) |
O11—Na1—O13—C13 | 12.2 (2) | C1—C2—C3—C4 | −0.3 (5) |
O14i—Na1—O13—C13 | 116.2 (2) | C2—C3—C4—F4 | 179.8 (3) |
O1Wii—Na1—O13—C13 | −70.4 (2) | C2—C3—C4—C5 | 0.5 (5) |
O1W—Na1—O14i—C13i | 95.5 (2) | F4—C4—C5—C6 | −180.0 (3) |
O2W—Na1—O14i—C13i | 11.6 (2) | C3—C4—C5—C6 | −0.7 (5) |
O11—Na1—O14i—C13i | −104.0 (2) | C4—C5—C6—C1 | 0.6 (5) |
O13—Na1—O14i—C13i | −175.8 (2) | O11—C12—C13—O13 | 13.2 (4) |
O1W—Na1—O1Wii—Na1ii | 0.00 (7) | O11—C12—C13—O14 | −167.2 (2) |
O2W—Na1—O1Wii—Na1ii | 84.58 (8) | | |
Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y+1, −z+1; (iii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11W···O2Wiv | 0.82 | 2.04 | 2.846 (3) | 165 |
O1W—H12W···O13v | 0.92 | 2.05 | 2.862 (3) | 147 |
O2W—H21W···O14vi | 0.80 | 1.93 | 2.727 (3) | 177 |
O2W—H22W···O13ii | 0.91 | 1.97 | 2.877 (3) | 176 |
C3—H3···F4vii | 0.95 | 2.53 | 3.154 (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) x−1, y+1, z; (vii) −x−1/2, y−1/2, −z+3/2. |
Poly[µ
5-[2-(4-fluorophenoxy)acetato]-
κ5O1,
O2:
O1,
O1':
O1':
O1':
O1'-potassium] (II)
top
Crystal data top
[K(C8H6FO3)] | F(000) = 424 |
Mr = 208.23 | Dx = 1.647 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 802 reflections |
a = 18.3542 (15) Å | θ = 4.4–27.8° |
b = 6.9466 (8) Å | µ = 0.62 mm−1 |
c = 6.5969 (5) Å | T = 200 K |
β = 92.995 (7)° | Plate, colourless |
V = 839.94 (13) Å3 | 0.30 × 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 source | 1354 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.1° |
ω scans | h = −22→22 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2014) | k = −8→8 |
Tmin = 0.896, Tmax = 0.990 | l = −7→8 |
1647 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)] = 0.081 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.199 | H-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 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −0.64 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
K1 | 0.56245 (6) | 0.47997 (19) | 0.24806 (18) | 0.0289 (4) | |
F4 | 0.9737 (2) | 0.4952 (7) | 0.1957 (6) | 0.0564 (14) | |
O11 | 0.7007 (2) | 0.4839 (7) | 0.4894 (6) | 0.0339 (13) | |
O13 | 0.5763 (2) | 0.3954 (6) | 0.6505 (6) | 0.0330 (14) | |
O14 | 0.5884 (2) | 0.6318 (7) | 0.8797 (6) | 0.0340 (13) | |
C1 | 0.7706 (3) | 0.4988 (9) | 0.4222 (8) | 0.0309 (19) | |
C2 | 0.8274 (3) | 0.5930 (10) | 0.5270 (9) | 0.0340 (19) | |
C3 | 0.8966 (3) | 0.5907 (11) | 0.4485 (9) | 0.0396 (19) | |
C4 | 0.9064 (3) | 0.4968 (11) | 0.2703 (10) | 0.0406 (19) | |
C5 | 0.8507 (4) | 0.4057 (10) | 0.1637 (10) | 0.040 (2) | |
C6 | 0.7815 (3) | 0.4059 (10) | 0.2397 (9) | 0.0373 (19) | |
C12 | 0.6873 (3) | 0.5768 (10) | 0.6755 (8) | 0.0310 (19) | |
C13 | 0.6105 (3) | 0.5301 (9) | 0.7406 (8) | 0.0294 (19) | |
H2 | 0.81950 | 0.65830 | 0.65040 | 0.0410* | |
H3 | 0.93640 | 0.65370 | 0.51840 | 0.0480* | |
H5 | 0.85910 | 0.34310 | 0.03910 | 0.0490* | |
H6 | 0.74210 | 0.34310 | 0.16770 | 0.0450* | |
H121 | 0.69250 | 0.71770 | 0.65930 | 0.0370* | |
H122 | 0.72370 | 0.53360 | 0.78190 | 0.0370* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0266 (6) | 0.0432 (8) | 0.0167 (6) | 0.0012 (6) | 0.0008 (4) | −0.0015 (6) |
F4 | 0.036 (2) | 0.090 (3) | 0.045 (2) | 0.008 (2) | 0.0202 (17) | 0.004 (2) |
O11 | 0.0231 (19) | 0.058 (3) | 0.0207 (19) | −0.0021 (19) | 0.0022 (15) | −0.008 (2) |
O13 | 0.031 (2) | 0.046 (3) | 0.022 (2) | −0.0031 (19) | 0.0019 (16) | −0.002 (2) |
O14 | 0.033 (2) | 0.055 (3) | 0.0146 (18) | 0.002 (2) | 0.0073 (16) | −0.004 (2) |
C1 | 0.026 (3) | 0.049 (4) | 0.018 (3) | 0.006 (3) | 0.003 (2) | 0.002 (3) |
C2 | 0.026 (3) | 0.052 (4) | 0.024 (3) | 0.001 (3) | 0.002 (2) | −0.005 (3) |
C3 | 0.029 (3) | 0.065 (4) | 0.025 (3) | 0.002 (3) | 0.003 (2) | 0.003 (3) |
C4 | 0.030 (3) | 0.058 (4) | 0.034 (3) | 0.012 (3) | 0.005 (3) | 0.008 (3) |
C5 | 0.045 (4) | 0.053 (4) | 0.024 (3) | 0.010 (3) | 0.009 (3) | −0.005 (3) |
C6 | 0.030 (3) | 0.054 (4) | 0.027 (3) | 0.000 (3) | −0.006 (2) | −0.010 (3) |
C12 | 0.025 (3) | 0.053 (4) | 0.015 (3) | −0.001 (3) | 0.001 (2) | −0.003 (3) |
C13 | 0.025 (3) | 0.046 (4) | 0.017 (3) | 0.002 (3) | −0.002 (2) | 0.008 (3) |
Geometric parameters (Å, º) top
K1—O11 | 2.924 (4) | C1—C6 | 1.390 (8) |
K1—O13 | 2.718 (4) | C2—C3 | 1.397 (8) |
K1—O14i | 2.714 (4) | C3—C4 | 1.365 (9) |
K1—O13ii | 2.804 (4) | C4—C5 | 1.366 (9) |
K1—O14ii | 2.956 (4) | C5—C6 | 1.390 (9) |
K1—O13iii | 2.701 (4) | C12—C13 | 1.530 (8) |
K1—O14iv | 2.866 (5) | C2—H2 | 0.9500 |
F4—C4 | 1.353 (7) | C3—H3 | 0.9500 |
O11—C1 | 1.383 (7) | C5—H5 | 0.9500 |
O11—C12 | 1.420 (7) | C6—H6 | 0.9500 |
O13—C13 | 1.259 (7) | C12—H121 | 0.9900 |
O14—C13 | 1.243 (7) | C12—H122 | 0.9900 |
C1—C2 | 1.385 (8) | | |
| | | |
O11—K1—O13 | 55.67 (11) | K1vii—O14—C13 | 111.5 (4) |
O11—K1—O14i | 107.22 (12) | K1vi—O14—K1ii | 87.00 (12) |
O11—K1—O13ii | 129.81 (12) | K1vi—O14—K1vii | 127.08 (16) |
O11—K1—O14ii | 158.59 (13) | K1ii—O14—K1vii | 91.29 (12) |
O11—K1—O13iii | 92.81 (13) | O11—C1—C2 | 124.2 (5) |
O11—K1—O14iv | 72.57 (13) | O11—C1—C6 | 114.9 (5) |
O13—K1—O14i | 161.22 (13) | C2—C1—C6 | 120.9 (5) |
O13—K1—O13ii | 82.73 (12) | C1—C2—C3 | 119.0 (6) |
O13—K1—O14ii | 105.08 (12) | C2—C3—C4 | 119.2 (6) |
O13—K1—O13iii | 91.08 (13) | F4—C4—C3 | 118.8 (5) |
O13—K1—O14iv | 84.37 (12) | F4—C4—C5 | 118.8 (6) |
O13ii—K1—O14i | 107.33 (12) | C3—C4—C5 | 122.4 (6) |
O14i—K1—O14ii | 93.00 (12) | C4—C5—C6 | 119.2 (6) |
O13iii—K1—O14i | 97.97 (14) | C1—C6—C5 | 119.3 (6) |
O14i—K1—O14iv | 82.61 (13) | O11—C12—C13 | 110.5 (5) |
O13ii—K1—O14ii | 45.58 (12) | O13—C13—O14 | 126.7 (5) |
O13ii—K1—O13iii | 116.93 (12) | O13—C13—C12 | 118.0 (5) |
O13ii—K1—O14iv | 77.04 (12) | O14—C13—C12 | 115.3 (5) |
O13iii—K1—O14ii | 77.11 (12) | C1—C2—H2 | 121.00 |
O14ii—K1—O14iv | 118.17 (13) | C3—C2—H2 | 120.00 |
O13iii—K1—O14iv | 164.71 (12) | C2—C3—H3 | 120.00 |
K1—O11—C1 | 128.3 (3) | C4—C3—H3 | 120.00 |
K1—O11—C12 | 106.9 (3) | C4—C5—H5 | 120.00 |
C1—O11—C12 | 116.7 (4) | C6—C5—H5 | 120.00 |
K1—O13—C13 | 108.6 (3) | C1—C6—H6 | 120.00 |
K1—O13—K1ii | 97.28 (12) | C5—C6—H6 | 120.00 |
K1—O13—K1v | 115.87 (15) | O11—C12—H121 | 110.00 |
K1ii—O13—C13 | 95.4 (3) | O11—C12—H122 | 110.00 |
K1v—O13—C13 | 131.0 (4) | C13—C12—H121 | 110.00 |
K1ii—O13—K1v | 98.24 (13) | C13—C12—H122 | 110.00 |
K1vi—O14—C13 | 121.3 (4) | H121—C12—H122 | 108.00 |
K1ii—O14—C13 | 88.7 (3) | | |
| | | |
O13—K1—O11—C1 | 169.5 (5) | O13vii—K1vii—O14—C13 | −158.7 (4) |
O14i—K1—O11—C1 | −19.1 (5) | O14iii—K1v—O13—C13 | −133.5 (4) |
O13ii—K1—O11—C1 | −150.8 (4) | O11vi—K1vi—O14—C13 | 86.2 (4) |
O14ii—K1—O11—C1 | 141.0 (5) | O13v—K1vi—O14—C13 | −9.2 (4) |
O13iii—K1—O11—C1 | 80.1 (5) | O14vii—K1vi—O14—C13 | 155.3 (4) |
O14iv—K1—O11—C1 | −95.4 (5) | O13—K1ii—O14—C13 | 10.0 (3) |
O13—K1—O11—C12 | −43.7 (3) | O11v—K1v—O13—K1 | 127.46 (15) |
O14i—K1—O11—C12 | 127.6 (4) | O13v—K1v—O13—K1 | −176.86 (15) |
O13ii—K1—O11—C12 | −4.0 (4) | O11vii—K1vii—O14—C13 | −103.0 (4) |
O14ii—K1—O11—C12 | −72.3 (5) | O11v—K1v—O13—C13 | −25.7 (5) |
O13iii—K1—O11—C12 | −133.1 (4) | O13v—K1v—O13—C13 | 30.0 (5) |
O14iv—K1—O11—C12 | 51.4 (4) | O14viii—K1vii—O14—C13 | 97.2 (4) |
O14—K1ii—O13—C13 | −9.9 (3) | O14iv—K1vii—O14—C13 | 7.7 (4) |
O13viii—K1ii—O13—C13 | 22.1 (4) | K1—O11—C1—C6 | −36.0 (7) |
O11ii—K1ii—O13—C13 | 141.8 (3) | C12—O11—C1—C6 | 180.0 (5) |
O13ii—K1ii—O13—C13 | 109.6 (3) | K1—O11—C1—C2 | 145.8 (5) |
O14—K1ii—O13—K1v | 122.9 (2) | K1—O11—C12—C13 | 34.7 (5) |
O14iii—K1v—O13—K1 | 19.64 (16) | C12—O11—C1—C2 | 1.8 (9) |
O11—K1—O13—C13 | 52.1 (3) | C1—O11—C12—C13 | −174.1 (5) |
O13ii—K1—O13—C13 | −98.3 (4) | K1v—O13—C13—C12 | 95.5 (6) |
O14ii—K1—O13—C13 | −138.3 (3) | K1ii—O13—C13—O14 | 21.3 (6) |
O13iii—K1—O13—C13 | 144.7 (4) | K1—O13—C13—O14 | 120.9 (6) |
O14iv—K1—O13—C13 | −20.7 (3) | K1—O13—C13—C12 | −59.1 (5) |
O11—K1—O13—K1ii | 150.32 (19) | K1ii—O13—C13—C12 | −158.7 (4) |
O13ii—K1—O13—K1ii | 0.00 (13) | K1v—O13—C13—O14 | −84.6 (7) |
O14ii—K1—O13—K1ii | −40.08 (16) | K1vii—O14—C13—C12 | 69.1 (5) |
O13iii—K1—O13—K1ii | −117.02 (13) | K1vi—O14—C13—O13 | 65.6 (7) |
O14iv—K1—O13—K1ii | 77.61 (13) | K1vi—O14—C13—C12 | −114.4 (5) |
O11—K1—O13—K1v | −106.83 (19) | K1ii—O14—C13—O13 | −20.1 (6) |
O13ii—K1—O13—K1v | 102.85 (16) | K1ii—O14—C13—C12 | 159.9 (4) |
O14ii—K1—O13—K1v | 62.77 (17) | K1vii—O14—C13—O13 | −110.9 (6) |
O13iii—K1—O13—K1v | −14.17 (15) | O11—C1—C2—C3 | 177.0 (6) |
O14iv—K1—O13—K1v | −179.54 (16) | C6—C1—C2—C3 | −1.1 (10) |
O13viii—K1ii—O14—C13 | −141.1 (4) | O11—C1—C6—C5 | −177.3 (6) |
O11ii—K1ii—O14—C13 | −77.6 (5) | C2—C1—C6—C5 | 0.9 (10) |
O13ii—K1ii—O14—C13 | −53.5 (4) | C1—C2—C3—C4 | 0.4 (10) |
O13—K1ii—O14—K1vi | −111.5 (2) | C2—C3—C4—F4 | −179.9 (6) |
O13—K1ii—O14—K1vii | 121.46 (18) | C2—C3—C4—C5 | 0.6 (11) |
O13viii—K1vii—O14—C13 | 117.5 (4) | F4—C4—C5—C6 | 179.7 (6) |
O14—K1ii—O13—K1 | −119.5 (2) | C3—C4—C5—C6 | −0.8 (11) |
O13viii—K1ii—O13—K1 | −87.51 (15) | C4—C5—C6—C1 | 0.0 (10) |
O11ii—K1ii—O13—K1 | 32.2 (2) | O11—C12—C13—O13 | 13.0 (7) |
O13ii—K1ii—O13—K1 | 0.00 (13) | O11—C12—C13—O14 | −167.0 (5) |
Symmetry codes: (i) x, y, z−1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z−1/2; (iv) x, −y+3/2, z−1/2; (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[µ
5-[2-(4-fluorophenoxy)acetato]-
κ5O1,
O2:
O1,
O1':
O1':
O1':
O1'-rubidium] (III)
top
Crystal data top
[Rb(C8H6FO3)] | F(000) = 496 |
Mr = 254.60 | Dx = 1.915 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1154 reflections |
a = 18.0011 (16) Å | θ = 3.4–28.0° |
b = 7.1625 (4) Å | µ = 5.59 mm−1 |
c = 6.8548 (4) Å | T = 200 K |
β = 91.995 (7)° | Plate, colourless |
V = 883.27 (11) Å3 | 0.35 × 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 source | 1315 reflections with I > 2]s(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 16.07 pixels mm-1 | θmax = 26.0°, θmin = 3.4° |
ω scans | h = −22→15 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2014) | k = −8→8 |
Tmin = 0.42, Tmax = 0.98 | l = −6→8 |
3411 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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H-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 parameters | Δρmax = 1.17 e Å−3 |
0 restraints | Δρmin = −0.64 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Rb1 | 0.56818 (3) | 0.47364 (7) | 0.24428 (7) | 0.0324 (2) | |
F4 | 0.9883 (2) | 0.5090 (5) | 0.1990 (5) | 0.0584 (16) | |
O11 | 0.7111 (2) | 0.4808 (5) | 0.4986 (5) | 0.0350 (12) | |
O13 | 0.5819 (2) | 0.4066 (5) | 0.6572 (5) | 0.0389 (14) | |
O14 | 0.5951 (2) | 0.6396 (5) | 0.8734 (5) | 0.0352 (14) | |
C1 | 0.7813 (3) | 0.4990 (6) | 0.4306 (7) | 0.0304 (19) | |
C2 | 0.8368 (4) | 0.6086 (7) | 0.5143 (8) | 0.0374 (19) | |
C3 | 0.9064 (4) | 0.6096 (8) | 0.4355 (8) | 0.040 (2) | |
C4 | 0.9192 (3) | 0.5044 (8) | 0.2744 (8) | 0.040 (2) | |
C5 | 0.8652 (4) | 0.3972 (8) | 0.1876 (8) | 0.044 (2) | |
C6 | 0.7954 (4) | 0.3956 (7) | 0.2643 (8) | 0.0384 (19) | |
C12 | 0.6952 (3) | 0.5806 (7) | 0.6728 (7) | 0.0321 (19) | |
C13 | 0.6176 (4) | 0.5380 (7) | 0.7386 (8) | 0.0323 (19) | |
H2 | 0.82720 | 0.68290 | 0.62550 | 0.0450* | |
H3 | 0.94520 | 0.68320 | 0.49330 | 0.0480* | |
H5 | 0.87540 | 0.32460 | 0.07570 | 0.0520* | |
H6 | 0.75690 | 0.32350 | 0.20330 | 0.0460* | |
H11 | 0.69980 | 0.71630 | 0.64880 | 0.0380* | |
H12 | 0.73180 | 0.54590 | 0.77750 | 0.0380* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rb1 | 0.0407 (4) | 0.0287 (3) | 0.0277 (3) | −0.0011 (2) | 0.0006 (2) | 0.0002 (2) |
F4 | 0.044 (3) | 0.086 (3) | 0.046 (2) | 0.009 (2) | 0.0113 (18) | 0.0016 (18) |
O11 | 0.032 (2) | 0.039 (2) | 0.034 (2) | −0.0015 (18) | 0.0004 (17) | −0.0097 (16) |
O13 | 0.047 (3) | 0.031 (2) | 0.039 (2) | −0.0084 (18) | 0.0066 (19) | −0.0007 (17) |
O14 | 0.045 (3) | 0.033 (2) | 0.028 (2) | 0.0004 (18) | 0.0072 (18) | −0.0026 (16) |
C1 | 0.036 (4) | 0.030 (3) | 0.025 (3) | 0.004 (3) | 0.000 (2) | 0.001 (2) |
C2 | 0.039 (4) | 0.040 (3) | 0.033 (3) | 0.001 (3) | −0.001 (3) | −0.005 (2) |
C3 | 0.034 (4) | 0.051 (4) | 0.035 (3) | −0.003 (3) | −0.001 (3) | −0.001 (3) |
C4 | 0.035 (4) | 0.048 (4) | 0.038 (3) | 0.010 (3) | 0.004 (3) | 0.008 (3) |
C5 | 0.054 (5) | 0.042 (3) | 0.035 (3) | 0.008 (3) | 0.006 (3) | −0.008 (3) |
C6 | 0.045 (4) | 0.033 (3) | 0.037 (3) | 0.000 (3) | 0.000 (3) | −0.005 (2) |
C12 | 0.037 (4) | 0.027 (3) | 0.032 (3) | −0.001 (2) | −0.001 (3) | −0.009 (2) |
C13 | 0.044 (4) | 0.024 (3) | 0.029 (3) | 0.003 (3) | 0.004 (2) | 0.008 (2) |
Geometric parameters (Å, º) top
Rb1—O11 | 3.058 (4) | C1—C6 | 1.390 (7) |
Rb1—O13 | 2.873 (3) | C2—C3 | 1.382 (10) |
Rb1—O14i | 2.863 (4) | C3—C4 | 1.363 (8) |
Rb1—O13ii | 2.936 (4) | C4—C5 | 1.360 (8) |
Rb1—O14ii | 3.128 (4) | C5—C6 | 1.379 (10) |
Rb1—O13iii | 2.801 (4) | C12—C13 | 1.514 (9) |
Rb1—O14iv | 2.943 (4) | C2—H2 | 0.9500 |
F4—C4 | 1.364 (6) | C3—H3 | 0.9500 |
O11—C1 | 1.368 (6) | C5—H5 | 0.9500 |
O11—C12 | 1.429 (6) | C6—H6 | 0.9500 |
O13—C13 | 1.259 (7) | C12—H11 | 0.9900 |
O14—C13 | 1.254 (7) | C12—H12 | 0.9900 |
C1—C2 | 1.380 (8) | | |
| | | |
O11—Rb1—O13 | 53.08 (10) | Rb1vii—O14—C13 | 112.2 (3) |
O11—Rb1—O14i | 109.53 (10) | Rb1vi—O14—Rb1ii | 86.26 (9) |
O11—Rb1—O13ii | 128.81 (10) | Rb1vi—O14—Rb1vii | 128.80 (13) |
O11—Rb1—O14ii | 156.34 (9) | Rb1ii—O14—Rb1vii | 91.32 (10) |
O11—Rb1—O13iii | 93.39 (10) | O11—C1—C2 | 125.2 (5) |
O11—Rb1—O14iv | 71.72 (10) | O11—C1—C6 | 115.2 (5) |
O13—Rb1—O14i | 158.88 (10) | C2—C1—C6 | 119.6 (5) |
O13—Rb1—O13ii | 82.56 (10) | C1—C2—C3 | 119.6 (5) |
O13—Rb1—O14ii | 104.98 (10) | C2—C3—C4 | 119.7 (6) |
O13—Rb1—O13iii | 92.42 (10) | F4—C4—C3 | 118.4 (5) |
O13—Rb1—O14iv | 81.57 (10) | F4—C4—C5 | 119.7 (5) |
O13ii—Rb1—O14i | 105.58 (10) | C3—C4—C5 | 121.9 (6) |
O14i—Rb1—O14ii | 93.74 (10) | C4—C5—C6 | 119.0 (5) |
O13iii—Rb1—O14i | 101.28 (10) | C1—C6—C5 | 120.2 (6) |
O14i—Rb1—O14iv | 81.09 (10) | O11—C12—C13 | 111.2 (4) |
O13ii—Rb1—O14ii | 43.20 (9) | O13—C13—O14 | 126.0 (6) |
O13ii—Rb1—O13iii | 114.95 (10) | O13—C13—C12 | 118.7 (5) |
O13ii—Rb1—O14iv | 78.41 (10) | O14—C13—C12 | 115.3 (5) |
O13iii—Rb1—O14ii | 77.40 (10) | C1—C2—H2 | 120.00 |
O14ii—Rb1—O14iv | 117.71 (10) | C3—C2—H2 | 120.00 |
O13iii—Rb1—O14iv | 164.69 (10) | C2—C3—H3 | 120.00 |
Rb1—O11—C1 | 125.2 (3) | C4—C3—H3 | 120.00 |
Rb1—O11—C12 | 107.2 (3) | C4—C5—H5 | 120.00 |
C1—O11—C12 | 116.8 (4) | C6—C5—H5 | 121.00 |
Rb1—O13—C13 | 109.7 (3) | C1—C6—H6 | 120.00 |
Rb1—O13—Rb1ii | 97.45 (11) | C5—C6—H6 | 120.00 |
Rb1—O13—Rb1v | 111.55 (12) | O11—C12—H11 | 109.00 |
Rb1ii—O13—C13 | 98.0 (4) | O11—C12—H12 | 109.00 |
Rb1v—O13—C13 | 132.8 (3) | C13—C12—H11 | 109.00 |
Rb1ii—O13—Rb1v | 98.42 (11) | C13—C12—H12 | 109.00 |
Rb1vi—O14—C13 | 118.8 (3) | H11—C12—H12 | 108.00 |
Rb1ii—O14—C13 | 89.1 (4) | | |
| | | |
O13—Rb1—O11—C1 | 173.2 (4) | O13—Rb1—O14ii—C13ii | 51.2 (3) |
O13—Rb1—O11—C12 | −44.0 (3) | O11—Rb1—O13iii—Rb1iii | −129.02 (12) |
O14i—Rb1—O11—C1 | −20.5 (3) | O11—Rb1—O13iii—C13iii | 20.3 (5) |
O14i—Rb1—O11—C12 | 122.3 (3) | O13—Rb1—O13iii—Rb1iii | 177.83 (13) |
O13ii—Rb1—O11—C1 | −151.1 (3) | O13—Rb1—O13iii—C13iii | −32.9 (5) |
O13ii—Rb1—O11—C12 | −8.4 (3) | O11—Rb1—O14iv—C13iv | 106.0 (4) |
O14ii—Rb1—O11—C1 | 148.6 (3) | O11—Rb1—O14iv—Rb1vii | −78.18 (16) |
O14ii—Rb1—O11—C12 | −68.7 (4) | O13—Rb1—O14iv—C13iv | 159.8 (4) |
O13iii—Rb1—O11—C1 | 82.7 (3) | O13—Rb1—O14iv—Rb1vii | −24.38 (16) |
O13iii—Rb1—O11—C12 | −134.5 (3) | Rb1—O11—C1—C2 | 138.1 (4) |
O14iv—Rb1—O11—C1 | −93.6 (3) | Rb1—O11—C1—C6 | −42.2 (5) |
O14iv—Rb1—O11—C12 | 49.1 (3) | C12—O11—C1—C2 | −1.5 (7) |
O11—Rb1—O13—C13 | 51.4 (4) | C12—O11—C1—C6 | 178.2 (4) |
O11—Rb1—O13—Rb1ii | 152.73 (16) | Rb1—O11—C12—C13 | 37.4 (4) |
O11—Rb1—O13—Rb1v | −105.13 (16) | C1—O11—C12—C13 | −176.3 (4) |
O14i—Rb1—O13—C13 | 13.1 (5) | Rb1—O13—C13—O14 | 122.7 (5) |
O14i—Rb1—O13—Rb1ii | 114.4 (3) | Rb1—O13—C13—C12 | −57.8 (5) |
O14i—Rb1—O13—Rb1v | −143.5 (2) | Rb1ii—O13—C13—O14 | 21.8 (6) |
O13ii—Rb1—O13—C13 | −101.3 (4) | Rb1ii—O13—C13—C12 | −158.7 (4) |
O13ii—Rb1—O13—Rb1ii | 0.00 (10) | Rb1v—O13—C13—O14 | −87.6 (7) |
O13ii—Rb1—O13—Rb1v | 102.14 (13) | Rb1v—O13—C13—C12 | 91.9 (5) |
O14ii—Rb1—O13—C13 | −138.5 (4) | Rb1vi—O14—C13—O13 | 65.0 (7) |
O14ii—Rb1—O13—Rb1ii | −37.25 (12) | Rb1vi—O14—C13—C12 | −114.5 (4) |
O14ii—Rb1—O13—Rb1v | 64.90 (14) | Rb1ii—O14—C13—O13 | −20.2 (6) |
O13iii—Rb1—O13—C13 | 143.9 (4) | Rb1ii—O14—C13—C12 | 160.3 (4) |
O13iii—Rb1—O13—Rb1ii | −114.85 (11) | Rb1vii—O14—C13—O13 | −111.3 (5) |
O13iii—Rb1—O13—Rb1v | −12.71 (13) | Rb1vii—O14—C13—C12 | 69.2 (5) |
O14iv—Rb1—O13—C13 | −22.0 (4) | O11—C1—C2—C3 | 177.6 (5) |
O14iv—Rb1—O13—Rb1ii | 79.31 (11) | C6—C1—C2—C3 | −2.1 (8) |
O14iv—Rb1—O13—Rb1v | −178.55 (14) | O11—C1—C6—C5 | −177.3 (5) |
O11—Rb1—O14i—C13i | 88.7 (4) | C2—C1—C6—C5 | 2.4 (8) |
O11—Rb1—O14i—Rb1iv | −95.68 (16) | C1—C2—C3—C4 | 0.9 (8) |
O13—Rb1—O14i—C13i | 120.5 (5) | C2—C3—C4—F4 | 179.6 (5) |
O13—Rb1—O14i—Rb1iv | −64.0 (4) | C2—C3—C4—C5 | 0.0 (9) |
O11—Rb1—O13ii—Rb1ii | −28.05 (16) | F4—C4—C5—C6 | −179.3 (5) |
O11—Rb1—O13ii—C13ii | −139.2 (3) | C3—C4—C5—C6 | 0.3 (9) |
O13—Rb1—O13ii—Rb1ii | 0.00 (10) | C4—C5—C6—C1 | −1.5 (8) |
O13—Rb1—O13ii—C13ii | −111.2 (3) | O11—C12—C13—O13 | 10.4 (7) |
O11—Rb1—O14ii—C13ii | 71.3 (4) | O11—C12—C13—O14 | −170.1 (4) |
Symmetry codes: (i) x, y, z−1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z−1/2; (iv) x, −y+3/2, z−1/2; (v) x, −y+1/2, z+1/2; (vi) x, y, z+1; (vii) x, −y+3/2, z+1/2. |
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