Poly[tetrakis(μ-1,1,1,3,3,3-hexafluoropropan-2-olato)iron(II)dipotassium].

The title compound, [K2Fe{OCH(CF3)2}4] n , was formed from the reaction of potassium hexa-fluoro-isopropoxide with iron(II) chloride in toluene. The Fe(II) atom has a highly distorted tetra-hedral coordination environment. All four of the non-equivalent hexa-fluoro-isoprop-oxy O atoms link the Fe(II) atoms to one of the K(+) atoms in an alternating chain of Fe-O-K-O fused four-membered rings, with K-Fe distances of 3.715 (2) and 3.717 (2) Å. This K(+) atom is also bridged to eight of the F atoms. The other K(+) atom is bonded to only two of the O atoms, but has seven short K⋯F contacts, one of which links the chains into a three-dimensional arrangement. Weak hydrogen bonding between the lone H atoms on the hexa-fluoro-isoprop-oxy groups and F atoms is also present. The crystal studied was refined as an inversion twin.

Related literature

For alkali or alkaline earth metal fluoro­alkoxides with short F—A distances, see: Zheng et al. (2009 ▶); Yamashita et al. (2005 ▶); Bernhardt et al. (2007 ▶); Purdy & George (1991 ▶, 1994 ▶); Samuels et al. (1993 ▶); Purdy et al. (1991 ▶). For iron(II) fluoro­alkoxides, see: Konefal et al. (1986 ▶); Cantalupo et al. (2010 ▶, 2012 ▶).

Experimental

Crystal data

[FeK2(C3HF6O)4]

M = 802.20

Orthorhombic,

a = 9.7368 (2) Å

b = 13.4345 (4) Å

c = 18.3933 (4) Å

V = 2406.02 (10) Å3

Z = 4

Cu Kα radiation

μ = 10.15 mm−1

T = 123 K

0.43 × 0.21 × 0.17 mm

Data collection

Agilent Xcalibur (Ruby, Gemini) diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012 ▶) T min = 0.254, T max = 1.000

16099 measured reflections

4923 independent reflections

4190 reflections with I > 2σ(I)

R int = 0.100

Refinement

R[F 2 > 2σ(F 2)] = 0.068

wR(F 2) = 0.182

S = 1.02

4923 reflections

389 parameters

144 restraints

H-atom parameters constrained

Δρmax = 1.63 e Å−3

Δρmin = −1.29 e Å−3

Absolute structure: Refined as an inversion twin

Absolute structure parameter: 0.205 (11)

Data collection: CrysAlis PRO (Agilent, 2012 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S1600536813034946/nk2215sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813034946/nk2215Isup2.hkl

CCDC reference:

Additional supporting information: crystallographic information; 3D view; checkCIF report

[FeK2(C3HF6O)4]	Dx = 2.215 Mg m−3
Mr = 802.20	Cu Kα radiation, λ = 1.54184 Å
Orthorhombic, P212121	Cell parameters from 8115 reflections
a = 9.7368 (2) Å	θ = 3.3–75.5°
b = 13.4345 (4) Å	µ = 10.15 mm−1
c = 18.3933 (4) Å	T = 123 K
V = 2406.02 (10) Å3	Prism, colorless
Z = 4	0.43 × 0.21 × 0.17 mm
F(000) = 1552

Agilent Xcalibur (Ruby, Gemini) diffractometer	4923 independent reflections
Radiation source: Enhance (Cu) X-ray Source	4190 reflections with I > 2σ(I)
Detector resolution: 10.5081 pixels mm-1	Rint = 0.100
ω scans	θmax = 75.7°, θmin = 4.1°
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	h = −12→8
Tmin = 0.254, Tmax = 1.000	k = −16→16
16099 measured reflections	l = −22→17

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.068	w = 1/[σ2(Fo2) + (0.1306P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.182	(Δ/σ)max < 0.001
S = 1.02	Δρmax = 1.63 e Å−3
4923 reflections	Δρmin = −1.29 e Å−3
389 parameters	Absolute structure: Refined as an inversion twin
144 restraints	Absolute structure parameter: 0.205 (11)

Experimental. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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

Refinement. Refined as a 2-component inversion twin. The structure was a racemic twin with a BASF component of 0.20906. In spite of the fact that the data was collected at -150 ° C the CF3 groups had some problems. Disorder was looked at without success but the best solution was to restrain using ISOR compound for some (but not all) F's.

	x	y	z	Uiso*/Ueq
Fe	0.41997 (13)	0.23850 (10)	0.28502 (6)	0.0109 (3)
K1	0.41988 (19)	0.48834 (14)	0.19850 (9)	0.0162 (4)
K2	0.69671 (19)	0.23877 (16)	0.16065 (9)	0.0196 (4)
O1A	0.6217 (6)	0.1993 (5)	0.2983 (3)	0.0152 (12)
C1A	0.6962 (9)	0.2291 (6)	0.3584 (4)	0.0145 (16)
H1AA	0.6995	0.3035	0.3588	0.017*
C2A	0.6316 (10)	0.1946 (7)	0.4284 (5)	0.0186 (18)
C3A	0.8423 (10)	0.1903 (8)	0.3490 (5)	0.024 (2)
F1A	0.6251 (7)	0.0950 (4)	0.4340 (3)	0.0284 (14)
F2A	0.6983 (7)	0.2266 (5)	0.4876 (3)	0.0347 (15)
F3A	0.5028 (6)	0.2283 (5)	0.4341 (3)	0.0272 (13)
F4A	0.8480 (7)	0.0916 (5)	0.3445 (4)	0.0320 (14)
F5A	0.9267 (7)	0.2178 (6)	0.4034 (4)	0.0449 (18)
F6A	0.8971 (6)	0.2258 (6)	0.2876 (4)	0.0378 (16)
O1B	0.3535 (7)	0.1029 (5)	0.2980 (4)	0.0181 (13)
C1B	0.2276 (9)	0.0657 (7)	0.3165 (5)	0.0170 (18)
H1BA	0.1580	0.1204	0.3163	0.020*
C2B	0.1877 (11)	−0.0141 (8)	0.2603 (5)	0.025 (2)
C3B	0.2342 (11)	0.0183 (8)	0.3922 (6)	0.026 (2)
F1B	0.1707 (8)	0.0271 (6)	0.1949 (3)	0.0406 (17)
F2B	0.0739 (8)	−0.0631 (6)	0.2766 (4)	0.047 (2)
F3B	0.2873 (7)	−0.0833 (5)	0.2517 (3)	0.0323 (14)
F4B	0.1165 (8)	−0.0222 (6)	0.4141 (4)	0.0458 (19)
F5B	0.3307 (8)	−0.0548 (5)	0.3957 (3)	0.0351 (15)
F6B	0.2697 (9)	0.0858 (6)	0.4414 (4)	0.0445 (19)
O1C	0.4260 (6)	0.2752 (4)	0.1770 (3)	0.0139 (11)
C1C	0.3268 (9)	0.2457 (7)	0.1284 (4)	0.0144 (16)
H1CA	0.3238	0.1713	0.1277	0.017*
C2C	0.1858 (9)	0.2841 (7)	0.1495 (5)	0.0175 (17)
C3C	0.3700 (10)	0.2821 (7)	0.0534 (5)	0.0177 (18)
F1C	0.1787 (6)	0.3837 (5)	0.1504 (3)	0.0304 (14)
F2C	0.1552 (6)	0.2545 (5)	0.2178 (3)	0.0260 (12)
F3C	0.0838 (6)	0.2516 (6)	0.1074 (3)	0.0341 (14)
F4C	0.3812 (7)	0.3802 (5)	0.0496 (3)	0.0325 (15)
F5C	0.4927 (6)	0.2443 (5)	0.0362 (3)	0.0295 (13)
F6C	0.2830 (7)	0.2540 (6)	0.0002 (3)	0.0342 (14)
O1D	0.3927 (7)	0.3754 (5)	0.3173 (3)	0.0165 (12)
C1D	0.3404 (10)	0.4119 (7)	0.3802 (5)	0.0171 (18)
H1DA	0.3309	0.3563	0.4160	0.020*
C2D	0.4377 (10)	0.4903 (8)	0.4112 (5)	0.023 (2)
C3D	0.1970 (12)	0.4569 (8)	0.3651 (5)	0.024 (2)
F1D	0.2019 (6)	0.5245 (5)	0.3110 (3)	0.0318 (14)
F2D	0.1412 (7)	0.5024 (6)	0.4213 (3)	0.0421 (19)
F3D	0.1113 (7)	0.3866 (6)	0.3436 (4)	0.0391 (17)
F4D	0.4577 (7)	0.5661 (5)	0.3630 (4)	0.0351 (15)
F5D	0.3921 (8)	0.5317 (6)	0.4723 (4)	0.046 (2)
F6D	0.5606 (7)	0.4520 (6)	0.4243 (4)	0.0359 (16)

	U11	U22	U33	U12	U13	U23
Fe	0.0062 (5)	0.0223 (7)	0.0041 (5)	0.0004 (5)	−0.0009 (4)	0.0011 (5)
K1	0.0121 (8)	0.0246 (9)	0.0119 (7)	−0.0017 (7)	0.0010 (7)	0.0019 (6)
K2	0.0133 (8)	0.0323 (10)	0.0134 (7)	0.0013 (8)	0.0029 (7)	0.0011 (7)
O1A	0.010 (2)	0.024 (3)	0.011 (2)	0.003 (2)	−0.002 (2)	0.002 (2)
C1A	0.014 (2)	0.0158 (19)	0.0142 (19)	−0.0003 (13)	−0.0017 (13)	0.0004 (13)
C2A	0.018 (3)	0.023 (3)	0.015 (3)	0.000 (3)	−0.006 (3)	−0.002 (3)
C3A	0.015 (4)	0.040 (5)	0.017 (4)	−0.001 (4)	−0.009 (4)	0.000 (4)
F1A	0.041 (4)	0.031 (3)	0.014 (2)	0.001 (3)	−0.003 (2)	0.003 (2)
F2A	0.041 (3)	0.050 (4)	0.012 (2)	0.001 (3)	−0.016 (2)	−0.002 (2)
F3A	0.022 (3)	0.048 (4)	0.012 (2)	0.010 (3)	0.005 (2)	0.002 (2)
F4A	0.019 (3)	0.039 (4)	0.038 (3)	0.009 (3)	−0.004 (3)	−0.002 (3)
F5A	0.021 (3)	0.069 (4)	0.045 (4)	−0.002 (3)	−0.023 (3)	−0.010 (3)
F6A	0.012 (3)	0.062 (4)	0.039 (4)	−0.001 (3)	0.009 (2)	0.008 (3)
O1B	0.010 (2)	0.021 (3)	0.023 (3)	−0.001 (2)	0.004 (2)	0.000 (2)
C1B	0.013 (3)	0.021 (3)	0.017 (3)	0.002 (3)	0.004 (3)	0.001 (3)
C2B	0.020 (5)	0.033 (5)	0.021 (4)	−0.006 (4)	0.000 (4)	0.003 (4)
C3B	0.023 (4)	0.032 (4)	0.022 (3)	−0.001 (3)	0.008 (3)	−0.004 (3)
F1B	0.042 (4)	0.060 (4)	0.019 (3)	−0.006 (3)	−0.013 (3)	0.005 (3)
F2B	0.026 (4)	0.073 (5)	0.042 (4)	−0.031 (4)	0.008 (3)	−0.011 (3)
F3B	0.035 (4)	0.036 (3)	0.026 (3)	0.003 (3)	−0.002 (3)	−0.009 (3)
F4B	0.030 (4)	0.075 (5)	0.033 (3)	−0.017 (3)	0.017 (3)	0.008 (3)
F5B	0.036 (4)	0.046 (4)	0.022 (3)	0.008 (3)	0.000 (3)	0.007 (3)
F6B	0.049 (5)	0.063 (5)	0.022 (3)	−0.004 (4)	0.006 (3)	−0.016 (3)
O1C	0.0133 (16)	0.0168 (16)	0.0114 (15)	0.0003 (12)	−0.0011 (12)	0.0006 (12)
C1C	0.014 (3)	0.020 (3)	0.009 (3)	0.001 (3)	−0.002 (2)	0.001 (3)
C2C	0.011 (3)	0.029 (3)	0.013 (3)	0.000 (3)	0.001 (3)	−0.002 (3)
C3C	0.014 (3)	0.027 (3)	0.012 (3)	0.002 (3)	−0.002 (3)	0.002 (3)
F1C	0.017 (3)	0.042 (3)	0.032 (3)	0.009 (3)	0.005 (2)	0.004 (3)
F2C	0.016 (2)	0.048 (3)	0.014 (2)	0.001 (2)	0.0067 (19)	0.004 (2)
F3C	0.014 (2)	0.064 (4)	0.025 (3)	−0.004 (3)	−0.007 (2)	−0.008 (3)
F4C	0.037 (4)	0.046 (4)	0.014 (2)	0.002 (3)	0.000 (2)	0.010 (2)
F5C	0.024 (2)	0.048 (3)	0.017 (2)	0.007 (2)	0.0095 (19)	0.002 (2)
F6C	0.033 (3)	0.055 (3)	0.014 (2)	−0.003 (3)	−0.009 (2)	−0.002 (2)
O1D	0.0175 (17)	0.0181 (16)	0.0141 (16)	0.0006 (12)	0.0022 (12)	−0.0007 (12)
C1D	0.014 (3)	0.024 (3)	0.013 (3)	0.000 (3)	0.000 (3)	0.001 (3)
C2D	0.021 (5)	0.037 (6)	0.012 (4)	0.004 (4)	−0.003 (3)	−0.004 (4)
C3D	0.024 (4)	0.031 (4)	0.018 (3)	−0.001 (3)	0.004 (3)	0.000 (3)
F1D	0.023 (3)	0.052 (4)	0.021 (3)	0.006 (3)	0.000 (2)	0.011 (3)
F2D	0.028 (3)	0.082 (5)	0.016 (3)	0.021 (4)	0.005 (2)	−0.012 (3)
F3D	0.020 (3)	0.066 (5)	0.032 (3)	−0.010 (3)	−0.001 (3)	−0.003 (3)
F4D	0.029 (4)	0.035 (4)	0.041 (4)	−0.010 (3)	−0.006 (3)	0.003 (3)
F5D	0.034 (4)	0.076 (5)	0.026 (3)	0.001 (4)	−0.001 (3)	−0.031 (3)
F6D	0.020 (3)	0.054 (4)	0.035 (3)	0.005 (3)	−0.015 (3)	−0.006 (3)

Fe—O1B	1.948 (6)	F1A—K1i	2.861 (6)
Fe—O1D	1.950 (6)	F4A—K1i	3.058 (7)
Fe—O1C	2.047 (6)	O1B—C1B	1.367 (11)
Fe—O1A	2.048 (6)	O1B—K1i	2.692 (7)
Fe—K2	3.535 (2)	C1B—C3B	1.532 (13)
Fe—K1	3.715 (2)	C1B—C2B	1.540 (13)
Fe—K1i	3.717 (2)	C1B—H1BA	1.0000
K1—O1D	2.674 (6)	C2B—F2B	1.323 (12)
K1—O1Bii	2.692 (7)	C2B—F1B	1.335 (11)
K1—F1Aii	2.861 (6)	C2B—F3B	1.353 (13)
K1—O1Aii	2.863 (7)	C3B—F6B	1.326 (13)
K1—F1C	2.877 (7)	C3B—F4B	1.331 (12)
K1—O1C	2.891 (6)	C3B—F5B	1.361 (13)
K1—F1D	3.003 (6)	F3B—K2i	2.888 (7)
K1—F5Bii	3.039 (7)	F3B—K1i	3.145 (7)
K1—F4Aii	3.058 (7)	F5B—K2i	2.973 (7)
K1—F4C	3.123 (6)	F5B—K1i	3.039 (7)
K1—F3Bii	3.145 (7)	O1C—C1C	1.375 (10)
K1—F4D	3.221 (7)	C1C—C2C	1.517 (12)
K2—O1A	2.689 (6)	C1C—C3C	1.522 (11)
K2—O1C	2.698 (7)	C1C—H1CA	1.0000
K2—F4Di	2.798 (8)	C2C—F3C	1.334 (11)
K2—F3Bii	2.888 (7)	C2C—F1C	1.340 (12)
K2—F5Bii	2.973 (7)	C2C—F2C	1.349 (10)
K2—F5C	3.032 (6)	C3C—F4C	1.324 (12)
K2—F6A	3.048 (7)	C3C—F5C	1.336 (11)
K2—F6Ciii	3.077 (6)	C3C—F6C	1.349 (10)
K2—F1Di	3.088 (7)	F6C—K2iv	3.077 (6)
K2—K1i	4.395 (3)	O1D—C1D	1.356 (10)
O1A—C1A	1.381 (10)	C1D—C2D	1.528 (13)
O1A—K1i	2.863 (6)	C1D—C3D	1.547 (14)
C1A—C2A	1.507 (12)	C1D—H1DA	1.0000
C1A—C3A	1.524 (13)	C2D—F6D	1.325 (12)
C1A—H1AA	1.0000	C2D—F5D	1.330 (11)
C2A—F3A	1.337 (12)	C2D—F4D	1.365 (12)
C2A—F2A	1.338 (10)	C3D—F2D	1.319 (11)
C2A—F1A	1.344 (12)	C3D—F3D	1.321 (13)
C3A—F4A	1.330 (13)	C3D—F1D	1.348 (11)
C3A—F6A	1.337 (12)	F1D—K2ii	3.088 (7)
C3A—F5A	1.347 (11)	F4D—K2ii	2.798 (8)
O1B—Fe—O1D	143.0 (3)	F1Di—K2—Fe	97.66 (13)
O1B—Fe—O1C	110.7 (3)	O1A—K2—K1	80.40 (13)
O1D—Fe—O1C	94.1 (2)	O1C—K2—K1	40.37 (13)
O1B—Fe—O1A	93.6 (3)	F4Di—K2—K1	109.28 (15)
O1D—Fe—O1A	109.7 (3)	F3Bii—K2—K1	46.14 (14)
O1C—Fe—O1A	98.7 (2)	F5Bii—K2—K1	44.14 (14)
O1B—Fe—K2	109.49 (19)	F5C—K2—K1	72.34 (13)
O1D—Fe—K2	107.45 (19)	F6A—K2—K1	108.52 (14)
O1C—Fe—K2	49.45 (18)	F6Ciii—K2—K1	107.35 (15)
O1A—Fe—K2	49.21 (17)	F1Di—K2—K1	152.62 (13)
O1B—Fe—K1	153.8 (2)	Fe—K2—K1	54.96 (4)
O1D—Fe—K1	43.83 (18)	O1A—K2—K1i	39.07 (14)
O1C—Fe—K1	50.70 (17)	O1C—K2—K1i	79.67 (13)
O1A—Fe—K1	106.50 (18)	F4Di—K2—K1i	47.01 (15)
K2—Fe—K1	73.86 (5)	F3Bii—K2—K1i	108.57 (13)
O1B—Fe—K1i	44.28 (19)	F5Bii—K2—K1i	153.69 (15)
O1D—Fe—K1i	152.21 (19)	F5C—K2—K1i	107.12 (14)
O1C—Fe—K1i	106.55 (17)	F6A—K2—K1i	70.74 (13)
O1A—Fe—K1i	49.86 (18)	F6Ciii—K2—K1i	131.40 (15)
K2—Fe—K1i	74.57 (5)	F1Di—K2—K1i	43.05 (12)
K1—Fe—K1i	148.42 (4)	Fe—K2—K1i	54.61 (4)
O1D—K1—O1Bii	112.7 (2)	K1—K2—K1i	109.57 (4)
O1D—K1—F1Aii	164.9 (2)	C1A—O1A—Fe	121.7 (5)
O1Bii—K1—F1Aii	81.9 (2)	C1A—O1A—K2	123.6 (5)
O1D—K1—O1Aii	122.10 (19)	Fe—O1A—K2	95.6 (2)
O1Bii—K1—O1Aii	63.20 (18)	C1A—O1A—K1i	110.2 (5)
F1Aii—K1—O1Aii	60.00 (17)	Fe—O1A—K1i	97.0 (2)
O1D—K1—F1C	83.88 (19)	K2—O1A—K1i	104.6 (2)
O1Bii—K1—F1C	163.0 (2)	O1A—C1A—C2A	112.0 (7)
F1Aii—K1—F1C	81.81 (19)	O1A—C1A—C3A	107.5 (7)
O1Aii—K1—F1C	112.00 (19)	C2A—C1A—C3A	112.4 (8)
O1D—K1—O1C	63.35 (18)	O1A—C1A—H1AA	108.3
O1Bii—K1—O1C	123.56 (19)	C2A—C1A—H1AA	108.3
F1Aii—K1—O1C	112.51 (17)	C3A—C1A—H1AA	108.3
O1Aii—K1—O1C	170.39 (18)	F3A—C2A—F2A	106.5 (8)
F1C—K1—O1C	59.39 (18)	F3A—C2A—F1A	106.7 (8)
O1D—K1—F1D	57.24 (18)	F2A—C2A—F1A	106.3 (7)
O1Bii—K1—F1D	118.1 (2)	F3A—C2A—C1A	110.7 (8)
F1Aii—K1—F1D	113.43 (19)	F2A—C2A—C1A	113.2 (8)
O1Aii—K1—F1D	74.11 (18)	F1A—C2A—C1A	113.1 (8)
F1C—K1—F1D	73.39 (18)	F4A—C3A—F6A	106.6 (9)
O1C—K1—F1D	105.59 (19)	F4A—C3A—F5A	107.1 (8)
O1D—K1—F5Bii	115.9 (2)	F6A—C3A—F5A	106.6 (8)
O1Bii—K1—F5Bii	57.84 (19)	F4A—C3A—C1A	112.7 (8)
F1Aii—K1—F5Bii	74.45 (19)	F6A—C3A—C1A	110.3 (8)
O1Aii—K1—F5Bii	108.25 (19)	F5A—C3A—C1A	113.0 (8)
F1C—K1—F5Bii	112.55 (18)	C2A—F1A—K1i	116.1 (5)
O1C—K1—F5Bii	73.54 (18)	C3A—F4A—K1i	115.7 (6)
F1D—K1—F5Bii	171.23 (18)	C3A—F6A—K2	114.3 (5)
O1D—K1—F4Aii	112.61 (19)	C1B—O1B—Fe	132.1 (6)
O1Bii—K1—F4Aii	116.48 (19)	C1B—O1B—K1i	121.3 (5)
F1Aii—K1—F4Aii	54.69 (19)	Fe—O1B—K1i	105.4 (3)
O1Aii—K1—F4Aii	55.65 (17)	O1B—C1B—C3B	110.0 (7)
F1C—K1—F4Aii	56.36 (17)	O1B—C1B—C2B	108.3 (7)
O1C—K1—F4Aii	115.57 (18)	C3B—C1B—C2B	109.3 (8)
F1D—K1—F4Aii	60.14 (17)	O1B—C1B—H1BA	109.7
F5Bii—K1—F4Aii	128.35 (19)	C3B—C1B—H1BA	109.7
O1D—K1—F4C	116.14 (18)	C2B—C1B—H1BA	109.7
O1Bii—K1—F4C	112.7 (2)	F2B—C2B—F1B	107.9 (9)
F1Aii—K1—F4C	57.82 (16)	F2B—C2B—F3B	106.6 (9)
O1Aii—K1—F4C	117.47 (17)	F1B—C2B—F3B	105.5 (8)
F1C—K1—F4C	53.42 (18)	F2B—C2B—C1B	113.9 (8)
O1C—K1—F4C	54.68 (16)	F1B—C2B—C1B	110.3 (8)
F1D—K1—F4C	126.43 (19)	F3B—C2B—C1B	112.1 (8)
F5Bii—K1—F4C	60.50 (18)	F6B—C3B—F4B	107.3 (8)
F4Aii—K1—F4C	83.19 (19)	F6B—C3B—F5B	106.3 (9)
O1D—K1—F3Bii	71.22 (18)	F4B—C3B—F5B	106.5 (9)
O1Bii—K1—F3Bii	54.89 (18)	F6B—C3B—C1B	110.3 (9)
F1Aii—K1—F3Bii	122.69 (19)	F4B—C3B—C1B	114.2 (9)
O1Aii—K1—F3Bii	115.15 (17)	F5B—C3B—C1B	111.8 (8)
F1C—K1—F3Bii	132.85 (19)	C2B—F3B—K2i	122.8 (6)
O1C—K1—F3Bii	73.62 (18)	C2B—F3B—K1i	114.0 (6)
F1D—K1—F3Bii	119.30 (17)	K2i—F3B—K1i	92.40 (19)
F5Bii—K1—F3Bii	51.94 (17)	C3B—F5B—K2i	126.5 (6)
F4Aii—K1—F3Bii	170.79 (18)	C3B—F5B—K1i	112.8 (6)
F4C—K1—F3Bii	102.85 (19)	K2i—F5B—K1i	92.91 (19)
O1D—K1—F4D	55.11 (18)	C1C—O1C—Fe	122.8 (5)
O1Bii—K1—F4D	72.43 (19)	C1C—O1C—K2	124.2 (5)
F1Aii—K1—F4D	130.92 (18)	Fe—O1C—K2	95.3 (2)
O1Aii—K1—F4D	71.10 (18)	C1C—O1C—K1	111.1 (5)
F1C—K1—F4D	122.75 (18)	Fe—O1C—K1	96.1 (2)
O1C—K1—F4D	116.56 (17)	K2—O1C—K1	102.4 (2)
F1D—K1—F4D	51.80 (18)	O1C—C1C—C2C	111.8 (7)
F5Bii—K1—F4D	120.40 (19)	O1C—C1C—C3C	107.6 (7)
F4Aii—K1—F4D	101.14 (19)	C2C—C1C—C3C	111.9 (7)
F4C—K1—F4D	171.16 (18)	O1C—C1C—H1CA	108.5
F3Bii—K1—F4D	73.87 (18)	C2C—C1C—H1CA	108.5
O1A—K2—O1C	70.43 (17)	C3C—C1C—H1CA	108.5
O1A—K2—F4Di	80.6 (2)	F3C—C2C—F1C	107.1 (8)
O1C—K2—F4Di	69.08 (19)	F3C—C2C—F2C	106.3 (7)
O1A—K2—F3Bii	69.64 (18)	F1C—C2C—F2C	105.8 (7)
O1C—K2—F3Bii	80.8 (2)	F3C—C2C—C1C	114.5 (7)
F4Di—K2—F3Bii	143.3 (2)	F1C—C2C—C1C	112.9 (8)
O1A—K2—F5Bii	119.22 (19)	F2C—C2C—C1C	109.8 (7)
O1C—K2—F5Bii	77.4 (2)	F4C—C3C—F5C	107.0 (8)
F4Di—K2—F5Bii	132.1 (2)	F4C—C3C—F6C	106.9 (8)
F3Bii—K2—F5Bii	55.06 (17)	F5C—C3C—F6C	106.5 (7)
O1A—K2—F5C	122.54 (18)	F4C—C3C—C1C	113.0 (7)
O1C—K2—F5C	55.93 (17)	F5C—C3C—C1C	109.9 (7)
F4Di—K2—F5C	63.32 (19)	F6C—C3C—C1C	113.2 (8)
F3Bii—K2—F5C	115.89 (19)	C2C—F1C—K1	116.7 (5)
F5Bii—K2—F5C	69.82 (18)	C3C—F4C—K1	115.3 (5)
O1A—K2—F6A	56.03 (17)	C3C—F5C—K2	114.6 (5)
O1C—K2—F6A	123.39 (17)	C3C—F6C—K2iv	149.4 (6)
F4Di—K2—F6A	114.6 (2)	C1D—O1D—Fe	130.7 (6)
F3Bii—K2—F6A	65.49 (19)	C1D—O1D—K1	121.9 (5)
F5Bii—K2—F6A	112.2 (2)	Fe—O1D—K1	105.8 (2)
F5C—K2—F6A	177.8 (2)	O1D—C1D—C2D	109.6 (8)
O1A—K2—F6Ciii	170.4 (2)	O1D—C1D—C3D	109.1 (7)
O1C—K2—F6Ciii	111.62 (18)	C2D—C1D—C3D	110.9 (8)
F4Di—K2—F6Ciii	91.4 (2)	O1D—C1D—H1DA	109.1
F3Bii—K2—F6Ciii	119.7 (2)	C2D—C1D—H1DA	109.1
F5Bii—K2—F6Ciii	70.11 (19)	C3D—C1D—H1DA	109.1
F5C—K2—F6Ciii	56.78 (16)	F6D—C2D—F5D	108.1 (8)
F6A—K2—F6Ciii	124.30 (18)	F6D—C2D—F4D	106.2 (8)
O1A—K2—F1Di	75.14 (17)	F5D—C2D—F4D	106.5 (9)
O1C—K2—F1Di	117.56 (18)	F6D—C2D—C1D	111.1 (9)
F4Di—K2—F1Di	54.91 (17)	F5D—C2D—C1D	113.4 (9)
F3Bii—K2—F1Di	131.32 (18)	F4D—C2D—C1D	111.1 (7)
F5Bii—K2—F1Di	163.23 (19)	F2D—C3D—F3D	107.8 (9)
F5C—K2—F1Di	111.10 (18)	F2D—C3D—F1D	106.4 (8)
F6A—K2—F1Di	67.20 (18)	F3D—C3D—F1D	106.5 (8)
F6Ciii—K2—F1Di	96.01 (18)	F2D—C3D—C1D	114.3 (8)
O1A—K2—Fe	35.22 (13)	F3D—C3D—C1D	110.1 (8)
O1C—K2—Fe	35.22 (12)	F1D—C3D—C1D	111.4 (8)
F4Di—K2—Fe	71.94 (15)	C3D—F1D—K1	115.1 (6)
F3Bii—K2—Fe	71.37 (14)	C3D—F1D—K2ii	121.0 (6)
F5Bii—K2—Fe	99.10 (15)	K1—F1D—K2ii	92.36 (18)
F5C—K2—Fe	89.38 (11)	C2D—F4D—K2ii	130.0 (6)
F6A—K2—Fe	89.56 (12)	C2D—F4D—K1	110.6 (5)
F6Ciii—K2—Fe	146.14 (14)	K2ii—F4D—K1	93.5 (2)
Fe—O1A—C1A—C2A	58.2 (9)	K1—O1C—C1C—C2C	−52.8 (8)
K2—O1A—C1A—C2A	−178.7 (5)	Fe—O1C—C1C—C3C	−177.0 (5)
K1i—O1A—C1A—C2A	−54.1 (8)	K2—O1C—C1C—C3C	−52.3 (8)
Fe—O1A—C1A—C3A	−177.8 (6)	K1—O1C—C1C—C3C	70.5 (7)
K2—O1A—C1A—C3A	−54.7 (8)	O1C—C1C—C2C—F3C	−175.2 (7)
K1i—O1A—C1A—C3A	69.8 (7)	C3C—C1C—C2C—F3C	64.0 (10)
O1A—C1A—C2A—F3A	−57.5 (10)	O1C—C1C—C2C—F1C	61.9 (10)
C3A—C1A—C2A—F3A	−178.7 (8)	C3C—C1C—C2C—F1C	−58.9 (10)
O1A—C1A—C2A—F2A	−177.0 (7)	O1C—C1C—C2C—F2C	−55.9 (10)
C3A—C1A—C2A—F2A	61.8 (10)	C3C—C1C—C2C—F2C	−176.7 (7)
O1A—C1A—C2A—F1A	62.1 (10)	O1C—C1C—C3C—F4C	−60.8 (10)
C3A—C1A—C2A—F1A	−59.1 (11)	C2C—C1C—C3C—F4C	62.4 (10)
O1A—C1A—C3A—F4A	−60.4 (10)	O1C—C1C—C3C—F5C	58.6 (9)
C2A—C1A—C3A—F4A	63.3 (10)	C2C—C1C—C3C—F5C	−178.2 (8)
O1A—C1A—C3A—F6A	58.6 (10)	O1C—C1C—C3C—F6C	177.5 (8)
C2A—C1A—C3A—F6A	−177.7 (8)	C2C—C1C—C3C—F6C	−59.3 (10)
O1A—C1A—C3A—F5A	177.9 (8)	F3C—C2C—F1C—K1	−162.6 (5)
C2A—C1A—C3A—F5A	−58.4 (11)	F2C—C2C—F1C—K1	84.4 (7)
F3A—C2A—F1A—K1i	87.7 (7)	C1C—C2C—F1C—K1	−35.7 (8)
F2A—C2A—F1A—K1i	−159.0 (5)	F5C—C3C—F4C—K1	−100.1 (6)
C1A—C2A—F1A—K1i	−34.2 (10)	F6C—C3C—F4C—K1	146.1 (5)
F6A—C3A—F4A—K1i	−100.7 (7)	C1C—C3C—F4C—K1	20.9 (9)
F5A—C3A—F4A—K1i	145.5 (6)	F4C—C3C—F5C—K2	82.7 (7)
C1A—C3A—F4A—K1i	20.5 (9)	F6C—C3C—F5C—K2	−163.3 (5)
F4A—C3A—F6A—K2	84.6 (8)	C1C—C3C—F5C—K2	−40.3 (9)
F5A—C3A—F6A—K2	−161.2 (6)	F4C—C3C—F6C—K2iv	50.4 (15)
C1A—C3A—F6A—K2	−38.1 (9)	F5C—C3C—F6C—K2iv	−63.7 (14)
Fe—O1B—C1B—C3B	−111.6 (8)	C1C—C3C—F6C—K2iv	175.4 (8)
K1i—O1B—C1B—C3B	54.1 (9)	Fe—O1D—C1D—C2D	130.2 (7)
Fe—O1B—C1B—C2B	129.0 (7)	K1—O1D—C1D—C2D	−66.0 (9)
K1i—O1B—C1B—C2B	−65.4 (8)	Fe—O1D—C1D—C3D	−108.2 (8)
O1B—C1B—C2B—F2B	173.4 (8)	K1—O1D—C1D—C3D	55.6 (9)
C3B—C1B—C2B—F2B	53.6 (11)	O1D—C1D—C2D—F6D	−59.5 (10)
O1B—C1B—C2B—F1B	−65.1 (10)	C3D—C1D—C2D—F6D	179.9 (7)
C3B—C1B—C2B—F1B	175.1 (8)	O1D—C1D—C2D—F5D	178.5 (8)
O1B—C1B—C2B—F3B	52.2 (10)	C3D—C1D—C2D—F5D	58.0 (11)
C3B—C1B—C2B—F3B	−67.6 (10)	O1D—C1D—C2D—F4D	58.5 (10)
O1B—C1B—C3B—F6B	60.7 (10)	C3D—C1D—C2D—F4D	−62.0 (10)
C2B—C1B—C3B—F6B	179.4 (9)	O1D—C1D—C3D—F2D	−174.5 (9)
O1B—C1B—C3B—F4B	−178.5 (8)	C2D—C1D—C3D—F2D	−53.7 (11)
C2B—C1B—C3B—F4B	−59.7 (11)	O1D—C1D—C3D—F3D	64.0 (10)
O1B—C1B—C3B—F5B	−57.4 (11)	C2D—C1D—C3D—F3D	−175.2 (7)
C2B—C1B—C3B—F5B	61.4 (11)	O1D—C1D—C3D—F1D	−53.9 (10)
F2B—C2B—F3B—K2i	−36.4 (10)	C2D—C1D—C3D—F1D	66.9 (10)
F1B—C2B—F3B—K2i	−151.0 (5)	F2D—C3D—F1D—K1	154.9 (6)
C1B—C2B—F3B—K2i	88.9 (8)	F3D—C3D—F1D—K1	−90.3 (8)
F2B—C2B—F3B—K1i	−146.4 (6)	C1D—C3D—F1D—K1	29.8 (9)
F1B—C2B—F3B—K1i	99.1 (7)	F2D—C3D—F1D—K2ii	45.4 (10)
C1B—C2B—F3B—K1i	−21.1 (9)	F3D—C3D—F1D—K2ii	160.2 (5)
F6B—C3B—F5B—K2i	161.5 (6)	C1D—C3D—F1D—K2ii	−79.8 (8)
F4B—C3B—F5B—K2i	47.3 (10)	F6D—C2D—F4D—K2ii	−153.1 (5)
C1B—C3B—F5B—K2i	−78.1 (9)	F5D—C2D—F4D—K2ii	−38.1 (11)
F6B—C3B—F5B—K1i	−86.2 (8)	C1D—C2D—F4D—K2ii	85.9 (9)
F4B—C3B—F5B—K1i	159.6 (6)	F6D—C2D—F4D—K1	93.2 (7)
C1B—C3B—F5B—K1i	34.2 (9)	F5D—C2D—F4D—K1	−151.8 (6)
Fe—O1C—C1C—C2C	59.7 (9)	C1D—C2D—F4D—K1	−27.8 (9)
K2—O1C—C1C—C2C	−175.5 (5)

D—H···A	D—H	H···A	D···A	D—H···A
C1A—H1AA···F3Bii	1.00	2.54	3.236 (10)	126
C1B—H1BA···F2C	1.00	2.56	3.199 (11)	122
C1C—H1CA···F4Di	1.00	2.56	3.201 (11)	122
C1D—H1DA···F2Av	1.00	2.46	3.361 (11)	150
C1D—H1DA···F3A	1.00	2.42	3.093 (11)	124

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1A—H1AA⋯F3B i	1.00	2.54	3.236 (10)	126
C1B—H1BA⋯F2C	1.00	2.56	3.199 (11)	122
C1C—H1CA⋯F4D ii	1.00	2.56	3.201 (11)	122
C1D—H1DA⋯F2A iii	1.00	2.46	3.361 (11)	150
C1D—H1DA⋯F3A	1.00	2.42	3.093 (11)	124

Symmetry codes: (i) ; (ii) ; (iii) .