Two polymorph modifications of tris­(hexa­fluoro­acetyl­aceton­ato)iron(III) revealed: is that common for other trivalent metals?

Chang, J.; Defeo, J.N.; Wei, Z.; Dikarev, E.V.

doi:10.1107/S2053229624007575

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Two polymorph modifications of tris(hexafluoroacetylacetonato)iron(III) revealed: is that common for other trivalent metals?

J. Chang, J. N. Defeo, Z. Wei and E. V. Dikarev

A long-standing issue about the correct identification of an important starting reagent, iron(III) hexafluoroacetylacetonate, Fe(hfac)₃ (1), has been resolved. The tris-chelated mononuclear complex was found to crystallize in two polymorph modifications which can be assigned as the low-temperature (1-L) monoclinic P2₁/n and the high-temperature (1-H) trigonal P $\overline{3}$ . Low-temperature polymorph 1-L was found to transform to 1-H upon sublimation at 44 °C. Two modifications are clearly distinguished by powder X-ray diffraction (PXRD), single-crystal X-ray diffraction, differential scanning calorimetry (DSC), and melting-point measurements. On the other hand, the two forms share similar characteristics in direct analysis in real-time mass spectrometry (DART-MS), attenuated total reflection (ATR) spectroscopy, and some physical properties, such as color, volatility, sensitivity, and solubility. Analysis of the literature and some of our preliminary data strongly suggest that the appearance of two polymorph modifications for trivalent metal (both transition and main group) hexafluoroacetylacetonates is a common case for several largely used complexes not yet accounted for in the crystallographic databases.

Keywords: crystal structure; iron(III) hexafluoroacetylacetonate; tris-chelated; mononuclear complex; phase transformation; fluorinated β-diketonate; polymorph modification; octahedral complex.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229624007575/vx3007sup1.cif Contains datablocks 1-L, 1-H, global
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229624007575/vx30071-Lsup2.hkl Contains datablock 1-L
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229624007575/vx30071-Hsup3.hkl Contains datablock 1-H

CCDC references: 2364188; 2364187

Computing details top

Tris(1,1,1,5,5,5-hexafluoro-4-oxopent-2-en-2-olato)iron(III) (1-L) top

Crystal data top

[Fe(C₅HF₆O₂)₃]	F(000) = 1316
M_r = 677.02	D_x = 2.062 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 8.7659 (2) Å	Cell parameters from 21755 reflections
b = 12.9796 (3) Å	θ = 1.9–31.1°
c = 19.1759 (5) Å	µ = 0.88 mm⁻¹
β = 91.632 (2)°	T = 100 K
V = 2180.90 (9) Å³	Block, red
Z = 4	0.16 × 0.12 × 0.09 mm

Data collection top

Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector	5815 independent reflections
Radiation source: micro-focus sealed X-ray tube	5188 reflections with I > 2σ(I)
Mirror monochromator	R_int = 0.035
Detector resolution: 10.0000 pixels mm^-1	θ_max = 30.9°, θ_min = 1.9°
ω scans	h = −12→12
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2023)	k = −18→18
T_min = 0.807, T_max = 1.000	l = −26→21
29802 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.032	H-atom parameters constrained
wR(F²) = 0.080	w = 1/[σ²(F_o²) + (0.0337P)² + 1.5613P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.001
5815 reflections	Δρ_max = 0.71 e Å⁻³
437 parameters	Δρ_min = −0.49 e Å⁻³
340 restraints	Extinction correction: SHELXL2019 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: dual	Extinction coefficient: 0.0015 (2)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Fe1	0.46900 (2)	0.49202 (2)	0.72339 (2)	0.01693 (7)
O1	0.57997 (12)	0.55097 (8)	0.80610 (5)	0.0185 (2)
O2	0.27477 (12)	0.52851 (9)	0.77026 (6)	0.0204 (2)
O3	0.47272 (12)	0.62615 (8)	0.67298 (6)	0.0199 (2)
O4	0.35357 (13)	0.43511 (9)	0.64130 (6)	0.0231 (2)
O5	0.66633 (12)	0.44825 (8)	0.68348 (6)	0.0206 (2)
O6	0.46767 (12)	0.35703 (8)	0.77335 (6)	0.0208 (2)
C1	0.64970 (18)	0.57904 (13)	0.92318 (8)	0.0227 (3)
C2	0.52614 (17)	0.56446 (11)	0.86604 (8)	0.0173 (3)
C3	0.37466 (17)	0.56599 (12)	0.88408 (8)	0.0203 (3)
H3	0.348842	0.576705	0.931306	0.024*
C4	0.25941 (17)	0.55187 (11)	0.83328 (8)	0.0189 (3)
C5	0.09413 (18)	0.57213 (13)	0.85443 (9)	0.0242 (3)
C6	0.4270 (2)	0.76326 (14)	0.59627 (10)	0.0305 (4)
C7	0.41157 (17)	0.64876 (12)	0.61483 (8)	0.0200 (3)
C8	0.3346 (2)	0.58291 (14)	0.56906 (8)	0.0266 (3)
H8	0.294569	0.608734	0.525938	0.032*
C9	0.31523 (18)	0.47960 (13)	0.58556 (8)	0.0228 (3)
C11	0.89668 (18)	0.36581 (12)	0.66105 (9)	0.0236 (3)
C12	0.74973 (17)	0.37331 (11)	0.70213 (8)	0.0183 (3)
C13	0.71970 (17)	0.29929 (11)	0.75225 (8)	0.0200 (3)
H13	0.795415	0.249771	0.764805	0.024*
C14	0.57945 (17)	0.29747 (11)	0.78402 (7)	0.0172 (3)
C15	0.54919 (18)	0.21521 (12)	0.83934 (8)	0.0224 (3)
F1	0.75797 (11)	0.64274 (8)	0.90242 (5)	0.0283 (2)
F2	0.71521 (13)	0.48824 (9)	0.93766 (6)	0.0362 (3)
F3	0.59418 (12)	0.61549 (11)	0.98224 (5)	0.0388 (3)
F4	0.06344 (13)	0.67176 (9)	0.84624 (7)	0.0430 (3)
F5	0.07236 (12)	0.54738 (11)	0.92035 (6)	0.0395 (3)
F6	−0.00539 (12)	0.51973 (11)	0.81544 (7)	0.0427 (3)
F7	0.34009 (17)	0.81936 (9)	0.63729 (9)	0.0629 (4)
F8	0.38449 (18)	0.78312 (11)	0.53107 (8)	0.0616 (4)
F9	0.56915 (12)	0.79520 (8)	0.60523 (6)	0.0346 (2)
F13	0.86086 (13)	0.35067 (10)	0.59334 (6)	0.0416 (3)
F14	0.97807 (11)	0.45122 (8)	0.66567 (6)	0.0326 (2)
F15	0.98408 (13)	0.28783 (8)	0.68154 (7)	0.0399 (3)
F16	0.66232 (12)	0.14777 (8)	0.84594 (6)	0.0328 (2)
F17	0.53208 (17)	0.25995 (9)	0.90105 (5)	0.0442 (3)
F18	0.42170 (11)	0.16378 (8)	0.82345 (6)	0.0324 (2)
C10	0.237 (4)	0.410 (2)	0.5286 (13)	0.0315 (18)	0.395 (3)
F10	0.2012 (14)	0.3222 (13)	0.5514 (7)	0.047 (2)	0.395 (3)
F11	0.0996 (6)	0.4562 (7)	0.5074 (4)	0.0420 (14)	0.395 (3)
F12	0.3186 (7)	0.4093 (6)	0.4738 (3)	0.0524 (16)	0.395 (3)
C10X	0.268 (2)	0.405 (2)	0.5270 (13)	0.036 (2)	0.263 (3)
F10X	0.1355 (8)	0.3686 (7)	0.5421 (4)	0.0576 (18)	0.263 (3)
F11X	0.2545 (11)	0.4523 (5)	0.4649 (3)	0.0505 (17)	0.263 (3)
F12X	0.3659 (9)	0.3294 (5)	0.5210 (3)	0.0386 (14)	0.263 (3)
C10Y	0.240 (4)	0.407 (3)	0.5329 (14)	0.034 (2)	0.342 (3)
F10Y	0.1750 (16)	0.3215 (14)	0.5617 (8)	0.0313 (16)	0.342 (3)
F11Y	0.1430 (10)	0.4470 (7)	0.4898 (4)	0.054 (2)	0.342 (3)
F12Y	0.3533 (7)	0.3629 (6)	0.4936 (4)	0.0454 (18)	0.342 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.01857 (11)	0.01664 (11)	0.01548 (11)	0.00176 (8)	−0.00116 (8)	0.00129 (8)
O1	0.0159 (5)	0.0235 (5)	0.0162 (5)	0.0004 (4)	0.0001 (4)	0.0000 (4)
O2	0.0170 (5)	0.0234 (5)	0.0205 (5)	0.0030 (4)	−0.0020 (4)	0.0004 (4)
O3	0.0227 (5)	0.0181 (5)	0.0186 (5)	0.0012 (4)	−0.0027 (4)	0.0015 (4)
O4	0.0261 (6)	0.0223 (5)	0.0206 (5)	−0.0010 (4)	−0.0025 (4)	−0.0030 (4)
O5	0.0227 (5)	0.0182 (5)	0.0212 (5)	0.0023 (4)	0.0037 (4)	0.0029 (4)
O6	0.0202 (5)	0.0195 (5)	0.0228 (5)	0.0016 (4)	0.0019 (4)	0.0037 (4)
C1	0.0186 (7)	0.0317 (8)	0.0177 (7)	−0.0013 (6)	−0.0016 (6)	−0.0007 (6)
C2	0.0182 (7)	0.0168 (6)	0.0168 (6)	0.0003 (5)	−0.0018 (5)	0.0022 (5)
C3	0.0185 (7)	0.0252 (7)	0.0171 (7)	0.0006 (6)	0.0013 (6)	0.0021 (6)
C4	0.0166 (7)	0.0179 (7)	0.0222 (7)	0.0018 (5)	0.0007 (6)	0.0041 (6)
C5	0.0171 (7)	0.0298 (8)	0.0257 (8)	0.0030 (6)	0.0002 (6)	0.0027 (6)
C6	0.0268 (8)	0.0275 (8)	0.0370 (9)	0.0027 (7)	−0.0036 (7)	0.0130 (7)
C7	0.0164 (7)	0.0228 (7)	0.0209 (7)	0.0053 (5)	0.0020 (6)	0.0041 (6)
C8	0.0273 (8)	0.0340 (9)	0.0182 (7)	0.0007 (7)	−0.0054 (6)	0.0043 (7)
C9	0.0186 (7)	0.0314 (8)	0.0184 (7)	0.0009 (6)	0.0013 (6)	−0.0053 (6)
C11	0.0238 (8)	0.0178 (7)	0.0297 (8)	−0.0009 (6)	0.0069 (6)	−0.0006 (6)
C12	0.0188 (7)	0.0162 (6)	0.0198 (7)	−0.0011 (5)	0.0007 (5)	−0.0025 (5)
C13	0.0195 (7)	0.0173 (7)	0.0230 (7)	0.0006 (5)	−0.0005 (6)	0.0022 (6)
C14	0.0210 (7)	0.0142 (6)	0.0163 (6)	−0.0024 (5)	−0.0021 (5)	0.0000 (5)
C15	0.0263 (8)	0.0181 (7)	0.0227 (7)	−0.0006 (6)	0.0016 (6)	0.0045 (6)
F1	0.0192 (4)	0.0371 (6)	0.0283 (5)	−0.0070 (4)	−0.0025 (4)	−0.0038 (4)
F2	0.0330 (6)	0.0399 (6)	0.0348 (6)	0.0050 (5)	−0.0133 (5)	0.0109 (5)
F3	0.0255 (5)	0.0712 (8)	0.0197 (5)	−0.0047 (5)	0.0003 (4)	−0.0132 (5)
F4	0.0281 (5)	0.0334 (6)	0.0681 (8)	0.0142 (5)	0.0124 (5)	0.0098 (6)
F5	0.0215 (5)	0.0688 (8)	0.0285 (5)	0.0060 (5)	0.0074 (4)	0.0115 (5)
F6	0.0166 (5)	0.0646 (8)	0.0467 (7)	−0.0055 (5)	−0.0002 (5)	−0.0150 (6)
F7	0.0587 (8)	0.0234 (6)	0.1087 (13)	0.0136 (6)	0.0372 (9)	0.0086 (7)
F8	0.0736 (10)	0.0517 (8)	0.0574 (8)	−0.0152 (7)	−0.0357 (7)	0.0360 (7)
F9	0.0308 (5)	0.0285 (5)	0.0441 (6)	−0.0053 (4)	−0.0054 (5)	0.0125 (5)
F13	0.0390 (6)	0.0579 (8)	0.0285 (6)	−0.0093 (5)	0.0130 (5)	−0.0098 (5)
F14	0.0229 (5)	0.0208 (5)	0.0546 (7)	−0.0055 (4)	0.0088 (5)	−0.0041 (5)
F15	0.0326 (6)	0.0283 (5)	0.0599 (8)	0.0129 (4)	0.0203 (5)	0.0133 (5)
F16	0.0278 (5)	0.0264 (5)	0.0441 (6)	0.0030 (4)	−0.0004 (4)	0.0174 (5)
F17	0.0808 (9)	0.0331 (6)	0.0192 (5)	−0.0007 (6)	0.0093 (5)	0.0035 (4)
F18	0.0242 (5)	0.0256 (5)	0.0476 (6)	−0.0067 (4)	0.0026 (4)	0.0120 (5)
C10	0.030 (4)	0.047 (3)	0.018 (3)	−0.014 (3)	−0.002 (3)	−0.016 (3)
F10	0.059 (6)	0.041 (3)	0.040 (5)	−0.014 (4)	−0.012 (3)	−0.010 (3)
F11	0.0237 (19)	0.067 (3)	0.034 (3)	−0.0147 (19)	−0.0100 (15)	0.001 (2)
F12	0.037 (3)	0.092 (5)	0.029 (3)	−0.022 (3)	0.012 (2)	−0.032 (3)
C10X	0.035 (4)	0.045 (4)	0.027 (4)	−0.004 (4)	−0.001 (4)	−0.009 (3)
F10X	0.039 (3)	0.085 (5)	0.049 (4)	−0.029 (3)	0.011 (3)	−0.036 (3)
F11X	0.074 (5)	0.055 (3)	0.021 (2)	0.001 (3)	−0.018 (3)	−0.010 (2)
F12X	0.054 (3)	0.035 (3)	0.027 (3)	0.005 (2)	0.001 (3)	−0.017 (2)
C10Y	0.029 (4)	0.050 (4)	0.023 (4)	−0.008 (3)	0.009 (3)	−0.002 (3)
F10Y	0.030 (3)	0.035 (3)	0.029 (3)	−0.016 (2)	0.007 (2)	−0.009 (2)
F11Y	0.069 (5)	0.050 (3)	0.040 (4)	−0.003 (4)	−0.033 (3)	−0.008 (3)
F12Y	0.034 (3)	0.064 (5)	0.039 (4)	−0.013 (3)	0.022 (3)	−0.030 (3)

Geometric parameters (Å, º) top

Fe1—O1	1.9899 (11)	C7—C8	1.387 (2)
Fe1—O2	2.0045 (11)	C8—H8	0.9500
Fe1—O3	1.9921 (11)	C8—C9	1.389 (2)
Fe1—O4	1.9891 (11)	C9—C10	1.563 (9)
Fe1—O5	1.9939 (11)	C9—C10X	1.532 (13)
Fe1—O6	1.9971 (11)	C9—C10Y	1.518 (12)
O1—C2	1.2670 (18)	C11—C12	1.532 (2)
O2—C4	1.2568 (19)	C11—F13	1.342 (2)
O3—C7	1.2582 (18)	C11—F14	1.3199 (18)
O4—C9	1.252 (2)	C11—F15	1.3224 (19)
O5—C12	1.2624 (18)	C12—C13	1.389 (2)
O6—C14	1.2603 (18)	C13—H13	0.9500
C1—C2	1.530 (2)	C13—C14	1.388 (2)
C1—F1	1.3283 (19)	C14—C15	1.534 (2)
C1—F2	1.337 (2)	C15—F16	1.3261 (19)
C1—F3	1.3321 (19)	C15—F17	1.3303 (19)
C2—C3	1.382 (2)	C15—F18	1.3297 (19)
C3—H3	0.9500	C10—F10	1.26 (3)
C3—C4	1.395 (2)	C10—F11	1.39 (3)
C4—C5	1.538 (2)	C10—F12	1.29 (4)
C5—F4	1.329 (2)	C10X—F10X	1.29 (2)
C5—F5	1.3233 (19)	C10X—F11X	1.34 (3)
C5—F6	1.321 (2)	C10X—F12X	1.31 (2)
C6—C7	1.535 (2)	C10Y—F10Y	1.37 (3)
C6—F7	1.328 (2)	C10Y—F11Y	1.28 (4)
C6—F8	1.320 (2)	C10Y—F12Y	1.39 (4)
C6—F9	1.319 (2)

O1—Fe1—O2	87.36 (4)	C8—C7—C6	119.65 (15)
O1—Fe1—O3	92.08 (4)	C7—C8—H8	119.6
O1—Fe1—O5	90.33 (5)	C7—C8—C9	120.74 (15)
O1—Fe1—O6	87.96 (5)	C9—C8—H8	119.6
O3—Fe1—O2	92.11 (5)	O4—C9—C8	127.44 (15)
O3—Fe1—O5	92.08 (4)	O4—C9—C10	115.6 (11)
O3—Fe1—O6	179.29 (5)	O4—C9—C10X	113.2 (13)
O4—Fe1—O1	178.59 (5)	O4—C9—C10Y	112.5 (14)
O4—Fe1—O2	91.33 (5)	C8—C9—C10	117.0 (11)
O4—Fe1—O3	87.45 (5)	C8—C9—C10X	118.5 (12)
O4—Fe1—O5	91.02 (5)	C8—C9—C10Y	120.0 (14)
O4—Fe1—O6	92.53 (5)	F13—C11—C12	109.26 (13)
O5—Fe1—O2	175.27 (4)	F14—C11—C12	111.89 (13)
O5—Fe1—O6	87.20 (4)	F14—C11—F13	107.40 (14)
O6—Fe1—O2	88.60 (5)	F14—C11—F15	108.39 (14)
C2—O1—Fe1	126.15 (10)	F15—C11—C12	112.61 (13)
C4—O2—Fe1	127.14 (10)	F15—C11—F13	107.05 (14)
C7—O3—Fe1	128.42 (10)	O5—C12—C11	113.08 (13)
C9—O4—Fe1	128.49 (11)	O5—C12—C13	127.53 (14)
C12—O5—Fe1	127.77 (10)	C13—C12—C11	119.36 (13)
C14—O6—Fe1	126.94 (10)	C12—C13—H13	119.9
F1—C1—C2	111.07 (13)	C14—C13—C12	120.21 (14)
F1—C1—F2	107.74 (13)	C14—C13—H13	119.9
F1—C1—F3	108.38 (14)	O6—C14—C13	127.78 (14)
F2—C1—C2	109.31 (13)	O6—C14—C15	112.98 (13)
F3—C1—C2	112.60 (13)	C13—C14—C15	119.24 (13)
F3—C1—F2	107.56 (13)	F16—C15—C14	112.46 (13)
O1—C2—C1	113.10 (13)	F16—C15—F17	107.83 (14)
O1—C2—C3	127.91 (14)	F16—C15—F18	108.17 (13)
C3—C2—C1	118.99 (13)	F17—C15—C14	109.72 (13)
C2—C3—H3	119.8	F18—C15—C14	110.60 (13)
C2—C3—C4	120.35 (14)	F18—C15—F17	107.92 (14)
C4—C3—H3	119.8	F10—C10—C9	112.8 (18)
O2—C4—C3	127.42 (14)	F10—C10—F11	106 (2)
O2—C4—C5	114.98 (13)	F10—C10—F12	115 (2)
C3—C4—C5	117.52 (14)	F11—C10—C9	108.2 (18)
F4—C5—C4	108.92 (13)	F12—C10—C9	109.2 (19)
F5—C5—C4	111.89 (13)	F12—C10—F11	105.1 (18)
F5—C5—F4	108.35 (15)	F10X—C10X—C9	107.1 (13)
F6—C5—C4	111.99 (14)	F10X—C10X—F11X	108.2 (17)
F6—C5—F4	107.81 (14)	F10X—C10X—F12X	110 (2)
F6—C5—F5	107.74 (14)	F11X—C10X—C9	112.0 (18)
F7—C6—C7	109.72 (14)	F12X—C10X—C9	111.8 (15)
F8—C6—C7	112.59 (16)	F12X—C10X—F11X	107.7 (15)
F8—C6—F7	107.60 (16)	F10Y—C10Y—C9	114 (2)
F9—C6—C7	111.31 (13)	F10Y—C10Y—F12Y	101 (2)
F9—C6—F7	107.83 (17)	F11Y—C10Y—C9	117 (3)
F9—C6—F8	107.60 (15)	F11Y—C10Y—F10Y	108 (2)
O3—C7—C6	113.14 (14)	F11Y—C10Y—F12Y	106.8 (19)
O3—C7—C8	127.21 (15)	F12Y—C10Y—C9	108 (2)

Fe1—O1—C2—C1	162.11 (10)	C6—C7—C8—C9	−178.15 (15)
Fe1—O1—C2—C3	−17.1 (2)	C7—C8—C9—O4	4.1 (3)
Fe1—O2—C4—C3	5.6 (2)	C7—C8—C9—C10	−176.0 (16)
Fe1—O2—C4—C5	−177.78 (10)	C7—C8—C9—C10X	−164.4 (8)
Fe1—O3—C7—C6	174.55 (10)	C7—C8—C9—C10Y	−176.1 (19)
Fe1—O3—C7—C8	−4.8 (2)	C8—C9—C10—F10	−169.1 (19)
Fe1—O4—C9—C8	−5.1 (2)	C8—C9—C10—F11	−53 (2)
Fe1—O4—C9—C10	175.0 (16)	C8—C9—C10—F12	61 (2)
Fe1—O4—C9—C10X	163.9 (8)	C8—C9—C10X—F10X	−116.8 (18)
Fe1—O4—C9—C10Y	175.1 (17)	C8—C9—C10X—F11X	1.6 (17)
Fe1—O5—C12—C11	−177.80 (10)	C8—C9—C10X—F12X	122.6 (18)
Fe1—O5—C12—C13	4.3 (2)	C8—C9—C10Y—F10Y	−156 (2)
Fe1—O6—C14—C13	−14.7 (2)	C8—C9—C10Y—F11Y	−28 (4)
Fe1—O6—C14—C15	165.23 (10)	C8—C9—C10Y—F12Y	92 (2)
O1—C2—C3—C4	−0.2 (3)	C11—C12—C13—C14	−172.25 (14)
O2—C4—C5—F4	−90.73 (17)	C12—C13—C14—O6	0.1 (2)
O2—C4—C5—F5	149.50 (14)	C12—C13—C14—C15	−179.82 (14)
O2—C4—C5—F6	28.4 (2)	C13—C14—C15—F16	−5.4 (2)
O3—C7—C8—C9	1.2 (3)	C13—C14—C15—F17	114.61 (16)
O4—C9—C10—F10	11 (3)	C13—C14—C15—F18	−126.46 (15)
O4—C9—C10—F11	127.4 (15)	F1—C1—C2—O1	44.26 (18)
O4—C9—C10—F12	−118.7 (17)	F1—C1—C2—C3	−136.47 (15)
O4—C9—C10X—F10X	73.1 (19)	F2—C1—C2—O1	−74.49 (16)
O4—C9—C10X—F11X	−168.4 (11)	F2—C1—C2—C3	104.77 (16)
O4—C9—C10X—F12X	−47 (2)	F3—C1—C2—O1	166.02 (14)
O4—C9—C10Y—F10Y	23 (4)	F3—C1—C2—C3	−14.7 (2)
O4—C9—C10Y—F11Y	151 (2)	F7—C6—C7—O3	−70.26 (19)
O4—C9—C10Y—F12Y	−88 (2)	F7—C6—C7—C8	109.16 (19)
O5—C12—C13—C14	5.6 (2)	F8—C6—C7—O3	169.94 (15)
O6—C14—C15—F16	174.67 (13)	F8—C6—C7—C8	−10.6 (2)
O6—C14—C15—F17	−65.31 (17)	F9—C6—C7—O3	49.0 (2)
O6—C14—C15—F18	53.62 (18)	F9—C6—C7—C8	−131.56 (17)
C1—C2—C3—C4	−179.35 (14)	F13—C11—C12—O5	−61.96 (17)
C2—C3—C4—O2	6.4 (3)	F13—C11—C12—C13	116.16 (16)
C2—C3—C4—C5	−170.13 (14)	F14—C11—C12—O5	56.85 (18)
C3—C4—C5—F4	86.24 (17)	F14—C11—C12—C13	−125.03 (16)
C3—C4—C5—F5	−33.5 (2)	F15—C11—C12—O5	179.23 (14)
C3—C4—C5—F6	−154.61 (15)	F15—C11—C12—C13	−2.7 (2)

Tris(1,1,1,5,5,5-hexafluoro-4-oxopent-2-en-2-olato)iron(III) (1-H) top

Crystal data top

[Fe(C₅HF₆O₂)₃]	D_x = 2.026 Mg m⁻³
M_r = 677.02	Synchrotron radiation, λ = 0.41329 Å
Trigonal, P3	Cell parameters from 9909 reflections
a = 18.1141 (4) Å	θ = 2.4–21.1°
c = 11.7136 (3) Å	µ = 0.21 mm⁻¹
V = 3328.54 (17) Å³	T = 100 K
Z = 6	Block, red
F(000) = 1974	0.15 × 0.12 × 0.09 mm

Data collection top

Huber 4-circle diffractometer	9816 independent reflections
Radiation source: synchrotron	9201 reflections with I > 2σ(I)
Si(111) & Si(311) monochromator	R_int = 0.048
Detector resolution: 30 pixels mm^-1	θ_max = 21.4°, θ_min = 1.0°
φ scans	h = −24→25
Absorption correction: multi-scan (SADABS; Bruker, 2018)	k = −25→31
T_min = 0.853, T_max = 1.000	l = −17→20
44621 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.032	H-atom parameters constrained
wR(F²) = 0.084	w = 1/[σ²(F_o²) + (0.0325P)² + 0.8379P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.002
9816 reflections	Δρ_max = 0.42 e Å⁻³
419 parameters	Δρ_min = −0.87 e Å⁻³
66 restraints	Extinction correction: SHELXL2019 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: dual	Extinction coefficient: 0.0612 (18)

Special details top

Refinement. Refined as a 2-component twin.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Fe1	1.000000	1.000000	0.71400 (2)	0.01654 (5)
Fe2	0.666667	0.333333	0.51162 (2)	0.01865 (5)
Fe3	0.333333	0.666667	0.93886 (2)	0.02110 (6)
O1	0.89940 (5)	0.92050 (5)	0.62066 (7)	0.01976 (14)
O2	0.97128 (5)	0.89995 (5)	0.81556 (7)	0.02078 (14)
O3	0.61280 (6)	0.38529 (6)	0.41847 (7)	0.02248 (14)
O4	0.56364 (5)	0.28567 (6)	0.61197 (7)	0.02412 (15)
O5	0.28244 (6)	0.56081 (5)	0.84457 (7)	0.02463 (15)
O6	0.38193 (7)	0.61141 (7)	1.03795 (7)	0.02682 (16)
C1	0.76554 (7)	0.80956 (8)	0.56148 (10)	0.02247 (19)
C2	0.83980 (7)	0.84721 (7)	0.64728 (9)	0.01791 (16)
C3	0.83466 (7)	0.79900 (7)	0.74320 (9)	0.02029 (18)
H3	0.784606	0.745835	0.757020	0.024*
C4	0.90328 (7)	0.82924 (7)	0.81852 (8)	0.01883 (17)
C5	0.90137 (8)	0.77069 (7)	0.91514 (9)	0.0236 (2)
C6	0.53188 (10)	0.44576 (10)	0.35758 (11)	0.0300 (3)
C7	0.54744 (7)	0.39018 (7)	0.44150 (9)	0.01997 (18)
C8	0.49062 (8)	0.35176 (8)	0.53137 (9)	0.02246 (19)
H8	0.443465	0.360613	0.540069	0.027*
C9	0.50280 (7)	0.30028 (8)	0.60868 (9)	0.02141 (19)
C12	0.28010 (8)	0.49139 (7)	0.86520 (9)	0.02183 (19)
C13	0.32037 (8)	0.47359 (8)	0.95365 (9)	0.0242 (2)
H13	0.314621	0.418651	0.959664	0.029*
C14	0.36896 (8)	0.53643 (8)	1.03300 (9)	0.02281 (19)
C15	0.41563 (10)	0.51552 (11)	1.12642 (11)	0.0325 (3)
F1	0.79368 (6)	0.82446 (7)	0.45473 (7)	0.0376 (2)
F2	0.71822 (7)	0.84609 (8)	0.57490 (9)	0.0427 (2)
F3	0.71500 (7)	0.72637 (6)	0.57427 (10)	0.0483 (3)
F4	0.95881 (7)	0.74648 (6)	0.89470 (7)	0.03534 (19)
F5	0.82540 (6)	0.70044 (6)	0.92495 (8)	0.0385 (2)
F6	0.92051 (6)	0.81077 (5)	1.01509 (6)	0.02827 (16)
F7	0.59348 (8)	0.52668 (7)	0.36801 (12)	0.0514 (3)
F8	0.53281 (9)	0.42204 (9)	0.25058 (7)	0.0491 (3)
F9	0.45868 (7)	0.44381 (8)	0.37561 (8)	0.0422 (2)
F16	0.49857 (7)	0.55425 (10)	1.10301 (10)	0.0514 (3)
F17	0.38688 (9)	0.43233 (7)	1.13467 (9)	0.0509 (3)
F18	0.40698 (8)	0.54366 (7)	1.22734 (7)	0.0415 (2)
C10	0.43433 (9)	0.25160 (11)	0.69967 (11)	0.0335 (3)
F10	0.3909 (6)	0.1711 (4)	0.6730 (6)	0.0654 (14)	0.75 (3)
F11	0.3809 (6)	0.2822 (9)	0.7073 (7)	0.0672 (17)	0.75 (3)
F12	0.4692 (5)	0.2603 (5)	0.8012 (4)	0.0390 (11)	0.75 (3)
F10X	0.4049 (10)	0.1657 (7)	0.6835 (17)	0.043 (3)	0.25 (3)
F11X	0.3675 (7)	0.2612 (10)	0.6983 (16)	0.038 (2)	0.25 (3)
F12X	0.4670 (12)	0.2644 (15)	0.8049 (12)	0.039 (4)	0.25 (3)
C11	0.22338 (9)	0.41848 (8)	0.78326 (11)	0.0308 (3)
F13	0.1407 (5)	0.3902 (10)	0.8150 (7)	0.062 (2)	0.53 (5)
F14	0.2364 (11)	0.3541 (7)	0.7912 (14)	0.054 (2)	0.53 (5)
F15	0.2347 (11)	0.4497 (8)	0.6776 (5)	0.0340 (13)	0.53 (5)
F13X	0.1446 (5)	0.3774 (7)	0.8169 (5)	0.0414 (16)	0.47 (5)
F14X	0.2486 (7)	0.3602 (7)	0.7731 (10)	0.0356 (14)	0.47 (5)
F15X	0.2222 (15)	0.4436 (10)	0.6786 (8)	0.042 (3)	0.47 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.01379 (7)	0.01379 (7)	0.02205 (10)	0.00689 (3)	0.000	0.000
Fe2	0.01576 (7)	0.01576 (7)	0.02441 (11)	0.00788 (4)	0.000	0.000
Fe3	0.01905 (8)	0.01905 (8)	0.02521 (11)	0.00952 (4)	0.000	0.000
O1	0.0163 (3)	0.0171 (3)	0.0237 (3)	0.0067 (3)	−0.0016 (3)	0.0021 (3)
O2	0.0197 (3)	0.0170 (3)	0.0244 (3)	0.0083 (3)	−0.0033 (3)	0.0008 (3)
O3	0.0225 (4)	0.0228 (4)	0.0256 (3)	0.0139 (3)	0.0047 (3)	0.0057 (3)
O4	0.0190 (3)	0.0243 (4)	0.0276 (3)	0.0098 (3)	0.0030 (3)	0.0083 (3)
O5	0.0252 (4)	0.0197 (3)	0.0273 (3)	0.0099 (3)	−0.0077 (3)	−0.0006 (3)
O6	0.0285 (4)	0.0268 (4)	0.0286 (3)	0.0164 (3)	−0.0097 (3)	−0.0062 (3)
C1	0.0162 (4)	0.0232 (5)	0.0239 (4)	0.0068 (4)	−0.0021 (3)	0.0015 (4)
C2	0.0155 (4)	0.0166 (4)	0.0208 (4)	0.0074 (3)	−0.0014 (3)	−0.0013 (3)
C3	0.0193 (4)	0.0165 (4)	0.0213 (4)	0.0061 (4)	−0.0005 (3)	0.0011 (3)
C4	0.0218 (5)	0.0166 (4)	0.0189 (3)	0.0102 (4)	0.0000 (3)	−0.0003 (3)
C5	0.0299 (6)	0.0186 (4)	0.0205 (4)	0.0107 (4)	−0.0023 (4)	0.0006 (3)
C6	0.0377 (7)	0.0363 (7)	0.0274 (5)	0.0271 (6)	0.0029 (4)	0.0064 (5)
C7	0.0222 (5)	0.0202 (4)	0.0200 (4)	0.0125 (4)	−0.0010 (3)	−0.0002 (3)
C8	0.0197 (5)	0.0292 (5)	0.0211 (4)	0.0143 (4)	−0.0001 (3)	−0.0009 (4)
C9	0.0159 (4)	0.0245 (5)	0.0194 (4)	0.0068 (4)	0.0008 (3)	0.0010 (3)
C12	0.0215 (5)	0.0188 (4)	0.0213 (4)	0.0071 (4)	−0.0027 (3)	0.0008 (3)
C13	0.0291 (6)	0.0221 (5)	0.0218 (4)	0.0132 (4)	−0.0034 (4)	0.0014 (4)
C14	0.0229 (5)	0.0281 (5)	0.0205 (4)	0.0151 (4)	−0.0032 (3)	−0.0006 (4)
C15	0.0395 (7)	0.0412 (7)	0.0270 (5)	0.0278 (6)	−0.0127 (5)	−0.0073 (5)
F1	0.0264 (4)	0.0510 (6)	0.0214 (3)	0.0088 (4)	−0.0025 (3)	−0.0056 (3)
F2	0.0311 (4)	0.0616 (7)	0.0485 (5)	0.0330 (5)	−0.0119 (4)	−0.0118 (5)
F3	0.0373 (5)	0.0248 (4)	0.0562 (6)	−0.0044 (4)	−0.0257 (4)	0.0084 (4)
F4	0.0544 (6)	0.0365 (4)	0.0314 (4)	0.0349 (5)	0.0004 (4)	0.0037 (3)
F5	0.0397 (5)	0.0235 (4)	0.0326 (4)	0.0010 (3)	−0.0060 (3)	0.0105 (3)
F6	0.0365 (4)	0.0294 (4)	0.0184 (3)	0.0161 (3)	−0.0027 (3)	−0.0016 (2)
F7	0.0539 (7)	0.0316 (5)	0.0736 (7)	0.0250 (5)	0.0042 (6)	0.0185 (5)
F8	0.0804 (8)	0.0763 (8)	0.0223 (3)	0.0628 (8)	0.0049 (4)	0.0094 (4)
F9	0.0467 (6)	0.0638 (7)	0.0391 (4)	0.0448 (5)	0.0029 (4)	0.0113 (4)
F16	0.0390 (6)	0.0806 (9)	0.0494 (6)	0.0409 (6)	−0.0147 (4)	−0.0076 (5)
F17	0.0812 (9)	0.0436 (6)	0.0433 (5)	0.0428 (6)	−0.0288 (5)	−0.0067 (4)
F18	0.0609 (7)	0.0532 (6)	0.0224 (3)	0.0375 (5)	−0.0125 (4)	−0.0063 (3)
C10	0.0213 (5)	0.0445 (8)	0.0252 (5)	0.0092 (5)	0.0044 (4)	0.0076 (5)
F10	0.042 (2)	0.051 (2)	0.0433 (11)	−0.0210 (13)	0.0068 (14)	0.0037 (15)
F11	0.041 (2)	0.122 (5)	0.053 (2)	0.052 (3)	0.0277 (18)	0.041 (3)
F12	0.038 (2)	0.052 (2)	0.0236 (16)	0.0195 (17)	0.0078 (12)	0.0118 (14)
F10X	0.037 (5)	0.024 (3)	0.059 (7)	0.008 (4)	0.024 (5)	0.012 (3)
F11X	0.014 (3)	0.059 (5)	0.035 (3)	0.014 (3)	0.010 (2)	0.010 (3)
F12X	0.025 (5)	0.056 (7)	0.017 (4)	0.006 (5)	−0.004 (3)	0.001 (4)
C11	0.0353 (7)	0.0193 (5)	0.0298 (5)	0.0077 (5)	−0.0107 (5)	−0.0007 (4)
F13	0.0289 (17)	0.041 (3)	0.089 (4)	−0.0027 (16)	−0.0170 (19)	−0.018 (2)
F14	0.096 (5)	0.0239 (17)	0.037 (3)	0.026 (3)	−0.025 (3)	−0.0060 (19)
F15	0.046 (3)	0.0241 (17)	0.0214 (16)	0.0097 (17)	−0.0106 (18)	−0.0024 (11)
F13X	0.0328 (19)	0.031 (2)	0.040 (3)	0.0009 (14)	−0.0032 (14)	−0.0002 (14)
F14X	0.058 (3)	0.0233 (17)	0.030 (2)	0.0233 (16)	−0.0156 (18)	−0.0048 (14)
F15X	0.059 (6)	0.026 (3)	0.035 (3)	0.015 (3)	−0.027 (3)	−0.0035 (15)

Geometric parameters (Å, º) top

Fe1—O1	1.9914 (8)	C5—F4	1.3373 (16)
Fe1—O1ⁱ	1.9914 (8)	C5—F5	1.3323 (15)
Fe1—O1ⁱⁱ	1.9914 (8)	C5—F6	1.3289 (13)
Fe1—O2	2.0070 (8)	C6—C7	1.5307 (16)
Fe1—O2ⁱⁱ	2.0070 (8)	C6—F7	1.332 (2)
Fe1—O2ⁱ	2.0069 (8)	C6—F8	1.3277 (16)
Fe2—O3ⁱⁱⁱ	1.9866 (8)	C6—F9	1.3257 (17)
Fe2—O3^iv	1.9866 (8)	C7—C8	1.3912 (16)
Fe2—O3	1.9866 (8)	C8—H8	0.9500
Fe2—O4ⁱⁱⁱ	1.9997 (8)	C8—C9	1.3944 (16)
Fe2—O4	1.9997 (8)	C9—C10	1.5357 (17)
Fe2—O4^iv	1.9997 (8)	C12—C13	1.3945 (16)
Fe3—O5	1.9948 (9)	C12—C11	1.5376 (17)
Fe3—O5^v	1.9948 (9)	C13—H13	0.9500
Fe3—O5^vi	1.9948 (9)	C13—C14	1.3901 (17)
Fe3—O6^vi	2.0012 (9)	C14—C15	1.5414 (17)
Fe3—O6	2.0012 (9)	C15—F16	1.331 (2)
Fe3—O6^v	2.0012 (9)	C15—F17	1.3291 (19)
O1—C2	1.2618 (13)	C15—F18	1.3273 (16)
O2—C4	1.2575 (14)	C10—F10	1.302 (6)
O3—C7	1.2597 (14)	C10—F11	1.337 (6)
O4—C9	1.2561 (15)	C10—F12	1.319 (4)
O5—C12	1.2602 (15)	C10—F10X	1.383 (10)
O6—C14	1.2587 (16)	C10—F11X	1.307 (11)
C1—C2	1.5387 (15)	C10—F12X	1.337 (10)
C1—F1	1.3261 (14)	C11—F13	1.371 (9)
C1—F2	1.3283 (16)	C11—F14	1.303 (8)
C1—F3	1.3234 (15)	C11—F15	1.333 (7)
C2—C3	1.3972 (15)	C11—F13X	1.298 (7)
C3—H3	0.9500	C11—F14X	1.349 (7)
C3—C4	1.3938 (15)	C11—F15X	1.312 (9)
C4—C5	1.5395 (15)

O1—Fe1—O1ⁱ	92.74 (3)	O2—C4—C3	127.57 (10)
O1—Fe1—O1ⁱⁱ	92.74 (3)	O2—C4—C5	113.27 (9)
O1ⁱ—Fe1—O1ⁱⁱ	92.74 (3)	C3—C4—C5	119.09 (10)
O1ⁱ—Fe1—O2	175.07 (3)	F4—C5—C4	109.94 (10)
O1ⁱⁱ—Fe1—O2ⁱⁱ	86.68 (3)	F5—C5—C4	112.21 (10)
O1—Fe1—O2ⁱⁱ	175.07 (3)	F5—C5—F4	107.68 (11)
O1ⁱⁱ—Fe1—O2	92.17 (3)	F6—C5—C4	111.19 (9)
O1—Fe1—O2ⁱ	92.17 (3)	F6—C5—F4	107.67 (10)
O1ⁱ—Fe1—O2ⁱⁱ	92.17 (3)	F6—C5—F5	107.98 (10)
O1ⁱ—Fe1—O2ⁱ	86.69 (3)	F7—C6—C7	109.67 (11)
O1ⁱⁱ—Fe1—O2ⁱ	175.07 (3)	F8—C6—C7	110.93 (11)
O1—Fe1—O2	86.68 (3)	F8—C6—F7	107.67 (13)
O2ⁱ—Fe1—O2ⁱⁱ	88.45 (4)	F9—C6—C7	113.01 (11)
O2ⁱ—Fe1—O2	88.45 (4)	F9—C6—F7	106.93 (12)
O2—Fe1—O2ⁱⁱ	88.45 (4)	F9—C6—F8	108.42 (12)
O3ⁱⁱⁱ—Fe2—O3^iv	92.73 (3)	O3—C7—C6	113.41 (10)
O3ⁱⁱⁱ—Fe2—O3	92.73 (3)	O3—C7—C8	127.82 (10)
O3^iv—Fe2—O3	92.73 (3)	C8—C7—C6	118.77 (11)
O3^iv—Fe2—O4	176.31 (4)	C7—C8—H8	120.0
O3—Fe2—O4^iv	90.95 (4)	C7—C8—C9	120.06 (11)
O3ⁱⁱⁱ—Fe2—O4^iv	176.31 (4)	C9—C8—H8	120.0
O3—Fe2—O4	87.36 (4)	O4—C9—C8	127.58 (10)
O3ⁱⁱⁱ—Fe2—O4ⁱⁱⁱ	87.36 (4)	O4—C9—C10	113.55 (11)
O3^iv—Fe2—O4^iv	87.36 (4)	C8—C9—C10	118.83 (11)
O3^iv—Fe2—O4ⁱⁱⁱ	90.95 (4)	O5—C12—C13	127.78 (11)
O3—Fe2—O4ⁱⁱⁱ	176.31 (4)	O5—C12—C11	114.33 (10)
O3ⁱⁱⁱ—Fe2—O4	90.95 (4)	C13—C12—C11	117.87 (11)
O4ⁱⁱⁱ—Fe2—O4^iv	88.95 (4)	C12—C13—H13	120.1
O4ⁱⁱⁱ—Fe2—O4	88.95 (4)	C14—C13—C12	119.84 (11)
O4—Fe2—O4^iv	88.95 (4)	C14—C13—H13	120.1
O5^vi—Fe3—O5	92.30 (3)	O6—C14—C13	127.93 (11)
O5^vi—Fe3—O5^v	92.30 (3)	O6—C14—C15	113.77 (11)
O5—Fe3—O5^v	92.30 (3)	C13—C14—C15	118.29 (12)
O5—Fe3—O6^vi	90.99 (4)	F16—C15—C14	109.73 (13)
O5^v—Fe3—O6	90.99 (4)	F17—C15—C14	112.22 (12)
O5^vi—Fe3—O6	176.66 (4)	F17—C15—F16	108.17 (13)
O5^v—Fe3—O6^vi	176.66 (4)	F18—C15—C14	110.69 (11)
O5^vi—Fe3—O6^v	90.99 (4)	F18—C15—F16	107.46 (13)
O5—Fe3—O6	87.01 (4)	F18—C15—F17	108.42 (13)
O5—Fe3—O6^v	176.66 (4)	F10—C10—C9	109.8 (3)
O5^v—Fe3—O6^v	87.01 (4)	F10—C10—F11	108.8 (4)
O5^vi—Fe3—O6^vi	87.00 (4)	F10—C10—F12	109.6 (6)
O6^v—Fe3—O6	89.74 (4)	F11—C10—C9	110.7 (4)
O6^v—Fe3—O6^vi	89.74 (4)	F12—C10—C9	110.9 (3)
O6^vi—Fe3—O6	89.74 (4)	F12—C10—F11	107.0 (6)
C2—O1—Fe1	128.12 (7)	F10X—C10—C9	107.3 (7)
C4—O2—Fe1	128.00 (7)	F11X—C10—C9	116.8 (8)
C7—O3—Fe2	128.11 (7)	F11X—C10—F10X	106.7 (8)
C9—O4—Fe2	128.22 (8)	F11X—C10—F12X	110.3 (15)
C12—O5—Fe3	128.45 (7)	F12X—C10—C9	112.4 (9)
C14—O6—Fe3	128.43 (8)	F12X—C10—F10X	102.1 (14)
F1—C1—C2	111.33 (9)	F13—C11—C12	106.7 (5)
F1—C1—F2	106.76 (11)	F14—C11—C12	112.4 (5)
F2—C1—C2	109.92 (10)	F14—C11—F13	107.4 (7)
F3—C1—C2	112.61 (10)	F14—C11—F15	112.8 (10)
F3—C1—F1	108.37 (11)	F15—C11—C12	108.7 (6)
F3—C1—F2	107.61 (11)	F15—C11—F13	108.5 (8)
O1—C2—C1	113.79 (9)	F13X—C11—C12	112.0 (4)
O1—C2—C3	127.66 (10)	F13X—C11—F14X	106.5 (7)
C3—C2—C1	118.55 (10)	F13X—C11—F15X	106.2 (10)
C2—C3—H3	120.1	F14X—C11—C12	112.6 (5)
C4—C3—C2	119.72 (10)	F15X—C11—C12	113.9 (8)
C4—C3—H3	120.1	F15X—C11—F14X	105.1 (8)

Fe1—O1—C2—C1	171.13 (7)	C3—C4—C5—F4	109.87 (12)
Fe1—O1—C2—C3	−8.62 (17)	C3—C4—C5—F5	−9.94 (15)
Fe1—O2—C4—C3	8.13 (17)	C3—C4—C5—F6	−130.99 (11)
Fe1—O2—C4—C5	−174.91 (7)	C6—C7—C8—C9	179.53 (11)
Fe2—O3—C7—C6	171.79 (9)	C7—C8—C9—O4	3.6 (2)
Fe2—O3—C7—C8	−8.30 (19)	C7—C8—C9—C10	−173.93 (12)
Fe2—O4—C9—C8	2.16 (19)	C8—C9—C10—F10	105.5 (6)
Fe2—O4—C9—C10	179.82 (9)	C8—C9—C10—F11	−14.6 (7)
Fe3—O5—C12—C13	−7.4 (2)	C8—C9—C10—F12	−133.2 (5)
Fe3—O5—C12—C11	170.74 (9)	C8—C9—C10—F10X	120.1 (9)
Fe3—O6—C14—C13	3.3 (2)	C8—C9—C10—F11X	0.5 (7)
Fe3—O6—C14—C15	−178.22 (9)	C8—C9—C10—F12X	−128.5 (15)
O1—C2—C3—C4	−4.25 (18)	C12—C13—C14—O6	1.0 (2)
O2—C4—C5—F4	−67.38 (12)	C12—C13—C14—C15	−177.39 (12)
O2—C4—C5—F5	172.82 (10)	C13—C12—C11—F13	102.2 (8)
O2—C4—C5—F6	51.76 (14)	C13—C12—C11—F14	−15.4 (11)
O3—C7—C8—C9	−0.4 (2)	C13—C12—C11—F15	−141.0 (7)
O4—C9—C10—F10	−72.3 (6)	C13—C12—C11—F13X	91.4 (6)
O4—C9—C10—F11	167.5 (6)	C13—C12—C11—F14X	−28.6 (6)
O4—C9—C10—F12	48.9 (5)	C13—C12—C11—F15X	−148.2 (10)
O4—C9—C10—F10X	−57.8 (9)	C13—C14—C15—F16	105.36 (15)
O4—C9—C10—F11X	−177.4 (7)	C13—C14—C15—F17	−14.92 (19)
O4—C9—C10—F12X	53.7 (15)	C13—C14—C15—F18	−136.20 (13)
O5—C12—C13—C14	1.1 (2)	F1—C1—C2—O1	41.99 (14)
O5—C12—C11—F13	−76.1 (8)	F1—C1—C2—C3	−138.24 (11)
O5—C12—C11—F14	166.3 (11)	F2—C1—C2—O1	−76.10 (13)
O5—C12—C11—F15	40.7 (7)	F2—C1—C2—C3	103.68 (13)
O5—C12—C11—F13X	−86.9 (6)	F3—C1—C2—O1	163.93 (11)
O5—C12—C11—F14X	153.1 (6)	F3—C1—C2—C3	−16.29 (16)
O5—C12—C11—F15X	33.5 (10)	F7—C6—C7—O3	−67.09 (14)
O6—C14—C15—F16	−73.28 (15)	F7—C6—C7—C8	112.99 (14)
O6—C14—C15—F17	166.44 (13)	F8—C6—C7—O3	51.71 (17)
O6—C14—C15—F18	45.16 (18)	F8—C6—C7—C8	−128.21 (13)
C1—C2—C3—C4	176.01 (10)	F9—C6—C7—O3	173.72 (12)
C2—C3—C4—O2	4.45 (18)	F9—C6—C7—C8	−6.20 (18)
C2—C3—C4—C5	−172.36 (10)	C11—C12—C13—C14	−176.92 (12)

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

Selected bond lengths and angles (Å, °) for 1-L and 1-H. top

	1-L		1-H
Fe1—O1	1.9899 (11)	Fe1—O1	1.9914 (8)
Fe1—O2	2.0045 (11)	Fe1—O2	2.0070 (8)
Fe1—O3	1.9921 (11)	Fe2—O3	1.9866 (8)
Fe1—O4	1.9891 (11)	Fe2—O4	1.9997 (8)
Fe1—O5	1.9939 (11)	Fe3—O5	1.9948 (9)
Fe1—O6	1.9971 (11)	Fe3—O6	2.0012 (9)

O1—Fe1—O2	87.36 (4)	O1—Fe1—O1ⁱ	92.74 (3)
O1—Fe1—O3	92.08 (5)	O1—Fe1—O2	86.68 (3)
O1—Fe1—O4	178.59 (5)	O1—Fe1—O2ⁱ	92.17 (3)
O1—Fe1—O5	90.33 (5)	O1—Fe1—O2ⁱⁱ	175.07 (3)
O1—Fe1—O6	87.96 (5)	O2—Fe1—O2ⁱ	88.45 (4)
O2—Fe1—O3	92.11 (5)	O3—Fe2—O3ⁱⁱⁱ	92.73 (3)
O2—Fe1—O4	91.33 (5)	O3—Fe2—O4	87.36 (4)
O2—Fe1—O5	175.27 (4)	O4—Fe2—O3ⁱⁱⁱ	90.95 (4)
O2—Fe1—O6	88.60 (5)	O4—Fe2—O3^iv	176.31 (4)
O3—Fe1—O4	87.45 (5)	O4—Fe2—O4ⁱⁱⁱ	88.95 (4)
O3—Fe1—O5	92.08 (4)	O5—Fe3—O5^v	92.30 (3)
O3—Fe1—O6	179.29 (5)	O5—Fe3—O6	87.01 (4)
O4—Fe1—O5	91.02 (5)	O5—Fe3—O6^v	176.66 (4)
O4—Fe1—O6	92.53 (5)	O5—Fe3—O6^vi	90.99 (4)
O5—Fe1—O6	87.20 (4)	O6—Fe3—O6^v	89.74 (4)

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

Assignment of ions detected in the positive-mode DART-MS spectra of 1-L and 1-H (hfac = C₅H₁O₂F₆). top

1-L
Ions	Measured, m/z	Calculated, m/z	Δ	% Base
[Fe(hfac)₂]⁺	469.9241	469.9110	0.0131	18.51
[Fe(hfac)₂·H₂O]⁺	487.9358	487.9216	0.0142	100.00
[Fe(hfac)₂·2H₂O]⁺	505.9463	505.9322	0.0141	10.6568
[Fe(hfac)₃·NH₄]⁺	694.9616	694.9335	0.0281	4.6383

1-H
[Fe(hfac)₂]⁺	469.9065	469.9110	0.0045	35.96
[Fe(hfac)₂·H₂O]⁺	487.9194	487.9216	0.0022	100.00
[Fe(hfac)₂·2H₂O]⁺	505.9279	505.9322	0.0043	4.03
[Fe(hfac)₃·NH₄]⁺	694.9329	694.9335	0.0006	4.07

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Two polymorph modifications of tris­(hexa­fluoro­acetyl­aceton­ato)iron(III) revealed: is that common for other trivalent metals?

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Two polymorph modifications of tris(hexafluoroacetylacetonato)iron(III) revealed: is that common for other trivalent metals?