#------------------------------------------------------------------------------
#$Date: 2024-08-20 04:46:22 +0300 (Tue, 20 Aug 2024) $
#$Revision: 294174 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312581.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312581
loop_
_publ_author_name
'Chang, Joyce'
'Defeo, Julianna N.'
'Wei, Zheng'
'Dikarev, Evgeny V.'
_publ_section_title
;
Two polymorph modifications of tris(hexafluoroacetylacetonato)iron(III)
revealed: is that common for other trivalent metals?
;
_journal_coeditor_code VX3007
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624007575
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Fe (C5 H1 F6 O2)3]'
_chemical_formula_moiety 'C15 H3 F18 Fe O6'
_chemical_formula_sum 'C15 H3 F18 Fe O6'
_chemical_formula_weight 677.02
_chemical_name_common
;
Tris(hexafluoroacetylacetonato)iron(III)
;
_chemical_name_systematic
;
Tris(1,1,1,5,5,5-hexafluoro-4-oxopent-2-en-2-olato)iron(III)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_cell_angle_alpha 90
_cell_angle_beta 91.632(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.7659(2)
_cell_length_b 12.9796(3)
_cell_length_c 19.1759(5)
_cell_measurement_reflns_used 21755
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 31.0790
_cell_measurement_theta_min 1.8960
_cell_volume 2180.91(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0348
_diffrn_reflns_av_unetI/netI 0.0232
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 29802
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.930
_diffrn_reflns_theta_min 1.895
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.878
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80658
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2023)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.062
_exptl_crystal_description block
_exptl_crystal_F_000 1316
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.711
_refine_diff_density_min -0.487
_refine_ls_extinction_coef 0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 5815
_refine_ls_number_restraints 340
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0368
_refine_ls_R_factor_gt 0.0320
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.5613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0780
_refine_ls_wR_factor_ref 0.0801
_reflns_number_gt 5188
_reflns_number_total 5815
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vx3007sup1.cif
_cod_data_source_block 1-L
_cod_original_cell_volume 2180.90(9)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2312581
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.872
_shelx_estimated_absorpt_t_max 0.925
_shelx_hkl_file
;
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12 1 -6 296.778 67.3394 4
12 1 -5 1839.23 138.585 4
12 1 -4 12.2939 43.9863 4
12 2 -7-15.0802 59.9374 4
12 2 -6 71.9533 63.7583 4
12 2 -5 102.711 55.4376 4
12 2 -4 200.754 61.8453 4
12 3 -6 819.103 104.903 4
12 3 -5 4460.42 238.600 4
12 3 -4 162.482 58.0251 4
12 3 -3 449.799 74.8831 4
12 4 -5-7.45655 60.7855 4
12 4 -4-64.1245 80.1158 4
12 4 -3 291.444 67.2546 4
-12 5 4 406.066 75.2282 2
-12 6 2 116.326 54.9984 2
0 0 0 0.00 0.00 0
TITL str3060_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 8.765871 12.979619 19.175859 90.0000 91.6316 90.0000
ZERR 31.00 0.000216 0.000310 0.000458 0.0000 0.0024 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H O F Fe
UNIT 31.00 31.00 31.00 31.00 31.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 2828
_shelx_res_file
;
TITL
1-l.res
created by SHELXL-2019/3 at 12:26:27 on 10-Jul-2024
CELL 0.71073 8.765871 12.979619 19.175859 90 91.6316 90
ZERR 4 0.000216 0.00031 0.000458 0 0.0024 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F Fe O
UNIT 60 12 72 4 24
SADI C9 C10 C9 C10X C9 C10Y
RIGU C10 F10 F11 F12 F11X C10X F12X F10X F11Y C10Y F12Y F10Y
SIMU 0.01 0.02 2 C10 F10 F11 F12 F11X C10X F12X F10X F11Y C10Y F12Y F10Y
SUMP 1 0 1 2 1 3 1 4
L.S. 120
PLAN 5
SIZE 0.09 0.12 0.16
TEMP -173(2)
CONF
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.033700 1.561300
EXTI 0.001506
FVAR 1.90187 0.39520 0.26324 0.34157
FE1 4 0.468998 0.492016 0.723387 11.00000 0.01857 0.01664 =
0.01548 0.00129 -0.00116 0.00176
O1 5 0.579974 0.550971 0.806101 11.00000 0.01592 0.02346 =
0.01618 -0.00001 0.00008 0.00041
O2 5 0.274774 0.528515 0.770262 11.00000 0.01696 0.02343 =
0.02054 0.00042 -0.00204 0.00295
O3 5 0.472724 0.626154 0.672982 11.00000 0.02275 0.01813 =
0.01861 0.00149 -0.00275 0.00122
O4 5 0.353571 0.435109 0.641299 11.00000 0.02606 0.02232 =
0.02065 -0.00301 -0.00254 -0.00101
O5 5 0.666329 0.448255 0.683482 11.00000 0.02269 0.01820 =
0.02118 0.00288 0.00373 0.00233
O6 5 0.467669 0.357033 0.773352 11.00000 0.02017 0.01953 =
0.02284 0.00368 0.00195 0.00163
C1 1 0.649703 0.579044 0.923185 11.00000 0.01863 0.03171 =
0.01765 -0.00073 -0.00158 -0.00127
C2 1 0.526139 0.564462 0.866041 11.00000 0.01824 0.01677 =
0.01677 0.00218 -0.00182 0.00027
C3 1 0.374658 0.565987 0.884075 11.00000 0.01848 0.02520 =
0.01714 0.00215 0.00128 0.00060
AFIX 43
H3 2 0.348842 0.576705 0.931306 11.00000 -1.20000
AFIX 0
C4 1 0.259410 0.551867 0.833278 11.00000 0.01657 0.01792 =
0.02216 0.00406 0.00073 0.00183
C5 1 0.094133 0.572134 0.854427 11.00000 0.01710 0.02982 =
0.02572 0.00274 0.00015 0.00299
C6 1 0.427049 0.763265 0.596267 11.00000 0.02678 0.02747 =
0.03696 0.01304 -0.00365 0.00272
C7 1 0.411565 0.648758 0.614825 11.00000 0.01644 0.02276 =
0.02091 0.00410 0.00201 0.00531
C8 1 0.334560 0.582911 0.569061 11.00000 0.02731 0.03404 =
0.01821 0.00425 -0.00540 0.00068
AFIX 43
H8 2 0.294569 0.608734 0.525938 11.00000 -1.20000
AFIX 0
C9 1 0.315229 0.479598 0.585557 11.00000 0.01859 0.03139 =
0.01842 -0.00526 0.00131 0.00087
C11 1 0.896680 0.365812 0.661050 11.00000 0.02377 0.01778 =
0.02974 -0.00057 0.00690 -0.00087
C12 1 0.749730 0.373315 0.702128 11.00000 0.01878 0.01620 =
0.01981 -0.00248 0.00072 -0.00110
C13 1 0.719702 0.299291 0.752249 11.00000 0.01951 0.01729 =
0.02302 0.00222 -0.00048 0.00060
AFIX 43
H13 2 0.795415 0.249771 0.764805 11.00000 -1.20000
AFIX 0
C14 1 0.579453 0.297470 0.784024 11.00000 0.02101 0.01418 =
0.01632 0.00005 -0.00214 -0.00241
C15 1 0.549193 0.215208 0.839345 11.00000 0.02627 0.01811 =
0.02274 0.00450 0.00164 -0.00061
F1 3 0.757971 0.642742 0.902422 11.00000 0.01922 0.03707 =
0.02833 -0.00377 -0.00252 -0.00696
F2 3 0.715208 0.488236 0.937665 11.00000 0.03304 0.03993 =
0.03480 0.01092 -0.01327 0.00497
F3 3 0.594184 0.615488 0.982242 11.00000 0.02548 0.07123 =
0.01967 -0.01320 0.00032 -0.00467
F4 3 0.063441 0.671759 0.846236 11.00000 0.02810 0.03335 =
0.06806 0.00985 0.01243 0.01417
F5 3 0.072364 0.547382 0.920346 11.00000 0.02155 0.06882 =
0.02855 0.01149 0.00743 0.00601
F6 3 -0.005390 0.519729 0.815441 11.00000 0.01662 0.06462 =
0.04671 -0.01499 -0.00016 -0.00554
F7 3 0.340087 0.819360 0.637289 11.00000 0.05871 0.02340 =
0.10865 0.00862 0.03721 0.01361
F8 3 0.384491 0.783121 0.531074 11.00000 0.07356 0.05169 =
0.05744 0.03604 -0.03566 -0.01524
F9 3 0.569153 0.795203 0.605231 11.00000 0.03080 0.02851 =
0.04414 0.01246 -0.00536 -0.00527
F13 3 0.860860 0.350675 0.593342 11.00000 0.03898 0.05794 =
0.02846 -0.00981 0.01297 -0.00928
F14 3 0.978069 0.451221 0.665669 11.00000 0.02287 0.02077 =
0.05457 -0.00415 0.00882 -0.00546
F15 3 0.984083 0.287834 0.681541 11.00000 0.03264 0.02827 =
0.05986 0.01325 0.02029 0.01288
F16 3 0.662324 0.147769 0.845943 11.00000 0.02780 0.02638 =
0.04415 0.01736 -0.00043 0.00301
F17 3 0.532075 0.259949 0.901047 11.00000 0.08084 0.03311 =
0.01916 0.00352 0.00926 -0.00071
F18 3 0.421705 0.163779 0.823454 11.00000 0.02424 0.02559 =
0.04759 0.01197 0.00257 -0.00673
PART 1
C10 1 0.236698 0.409879 0.528600 21.00000 0.02977 0.04704 =
0.01754 -0.01633 -0.00161 -0.01430
F10 3 0.201154 0.322167 0.551430 21.00000 0.05937 0.04095 =
0.03953 -0.01004 -0.01201 -0.01424
F11 3 0.099575 0.456180 0.507398 21.00000 0.02374 0.06739 =
0.03432 0.00080 -0.00999 -0.01466
F12 3 0.318555 0.409321 0.473843 21.00000 0.03653 0.09239 =
0.02882 -0.03159 0.01216 -0.02211
PART 2
C10X 1 0.267593 0.404899 0.527016 31.00000 0.03462 0.04540 =
0.02662 -0.00850 -0.00082 -0.00423
F10X 3 0.135517 0.368614 0.542090 31.00000 0.03942 0.08504 =
0.04882 -0.03619 0.01141 -0.02890
F11X 3 0.254548 0.452303 0.464933 31.00000 0.07425 0.05496 =
0.02126 -0.01010 -0.01825 0.00099
F12X 3 0.365898 0.329398 0.520999 31.00000 0.05364 0.03545 =
0.02679 -0.01657 0.00113 0.00544
PART 3
C10Y 1 0.239567 0.407126 0.532927 41.00000 0.02894 0.04984 =
0.02327 -0.00204 0.00901 -0.00830
F10Y 3 0.175005 0.321532 0.561691 41.00000 0.03021 0.03531 =
0.02872 -0.00884 0.00712 -0.01647
F11Y 3 0.143036 0.447014 0.489838 41.00000 0.06921 0.04953 =
0.04047 -0.00799 -0.03272 -0.00305
F12Y 3 0.353312 0.362873 0.493605 41.00000 0.03396 0.06415 =
0.03937 -0.03036 0.02173 -0.01282
HKLF 4
REM
REM wR2 = 0.0801, GooF = S = 1.052, Restrained GooF = 1.047 for all data
REM R1 = 0.0320 for 5188 Fo > 4sig(Fo) and 0.0368 for all 5815 data
REM 437 parameters refined using 340 restraints
END
WGHT 0.0336 1.5640
REM Highest difference peak 0.711, deepest hole -0.487, 1-sigma level 0.059
Q1 1 1.0208 0.3136 0.7182 11.00000 0.05 0.71
Q2 1 0.9166 0.3124 0.6196 11.00000 0.05 0.68
Q3 1 0.3386 0.8048 0.5918 11.00000 0.05 0.57
Q4 1 0.4591 0.7393 0.5113 11.00000 0.05 0.52
Q5 1 0.5672 0.2594 0.8127 11.00000 0.05 0.46
;
_shelx_res_checksum 77162
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.46900(2) 0.49202(2) 0.72339(2) 0.01693(7) Uani d 1 . .
O O1 0.57997(12) 0.55097(8) 0.80610(5) 0.0185(2) Uani d 1 . .
O O2 0.27477(12) 0.52851(9) 0.77026(6) 0.0204(2) Uani d 1 . .
O O3 0.47272(12) 0.62615(8) 0.67298(6) 0.0199(2) Uani d 1 . .
O O4 0.35357(13) 0.43511(9) 0.64130(6) 0.0231(2) Uani d 1 . .
O O5 0.66633(12) 0.44825(8) 0.68348(6) 0.0206(2) Uani d 1 . .
O O6 0.46767(12) 0.35703(8) 0.77335(6) 0.0208(2) Uani d 1 . .
C C1 0.64970(18) 0.57904(13) 0.92318(8) 0.0227(3) Uani d 1 . .
C C2 0.52614(17) 0.56446(11) 0.86604(8) 0.0173(3) Uani d 1 . .
C C3 0.37466(17) 0.56599(12) 0.88408(8) 0.0203(3) Uani d 1 . .
H H3 0.348842 0.576705 0.931306 0.024 Uiso calc 1 . .
C C4 0.25941(17) 0.55187(11) 0.83328(8) 0.0189(3) Uani d 1 . .
C C5 0.09413(18) 0.57213(13) 0.85443(9) 0.0242(3) Uani d 1 . .
C C6 0.4270(2) 0.76326(14) 0.59627(10) 0.0305(4) Uani d 1 . .
C C7 0.41157(17) 0.64876(12) 0.61483(8) 0.0200(3) Uani d 1 . .
C C8 0.3346(2) 0.58291(14) 0.56906(8) 0.0266(3) Uani d 1 . .
H H8 0.294569 0.608734 0.525938 0.032 Uiso calc 1 . .
C C9 0.31523(18) 0.47960(13) 0.58556(8) 0.0228(3) Uani d 1 . .
C C11 0.89668(18) 0.36581(12) 0.66105(9) 0.0236(3) Uani d 1 . .
C C12 0.74973(17) 0.37331(11) 0.70213(8) 0.0183(3) Uani d 1 . .
C C13 0.71970(17) 0.29929(11) 0.75225(8) 0.0200(3) Uani d 1 . .
H H13 0.795415 0.249771 0.764805 0.024 Uiso calc 1 . .
C C14 0.57945(17) 0.29747(11) 0.78402(7) 0.0172(3) Uani d 1 . .
C C15 0.54919(18) 0.21521(12) 0.83934(8) 0.0224(3) Uani d 1 . .
F F1 0.75797(11) 0.64274(8) 0.90242(5) 0.0283(2) Uani d 1 . .
F F2 0.71521(13) 0.48824(9) 0.93766(6) 0.0362(3) Uani d 1 . .
F F3 0.59418(12) 0.61549(11) 0.98224(5) 0.0388(3) Uani d 1 . .
F F4 0.06344(13) 0.67176(9) 0.84624(7) 0.0430(3) Uani d 1 . .
F F5 0.07236(12) 0.54738(11) 0.92035(6) 0.0395(3) Uani d 1 . .
F F6 -0.00539(12) 0.51973(11) 0.81544(7) 0.0427(3) Uani d 1 . .
F F7 0.34009(17) 0.81936(9) 0.63729(9) 0.0629(4) Uani d 1 . .
F F8 0.38449(18) 0.78312(11) 0.53107(8) 0.0616(4) Uani d 1 . .
F F9 0.56915(12) 0.79520(8) 0.60523(6) 0.0346(2) Uani d 1 . .
F F13 0.86086(13) 0.35067(10) 0.59334(6) 0.0416(3) Uani d 1 . .
F F14 0.97807(11) 0.45122(8) 0.66567(6) 0.0326(2) Uani d 1 . .
F F15 0.98408(13) 0.28783(8) 0.68154(7) 0.0399(3) Uani d 1 . .
F F16 0.66232(12) 0.14777(8) 0.84594(6) 0.0328(2) Uani d 1 . .
F F17 0.53208(17) 0.25995(9) 0.90105(5) 0.0442(3) Uani d 1 . .
F F18 0.42170(11) 0.16378(8) 0.82345(6) 0.0324(2) Uani d 1 . .
C C10 0.237(4) 0.410(2) 0.5286(13) 0.0315(18) Uani d 0.395(3) A 1
F F10 0.2012(14) 0.3222(13) 0.5514(7) 0.047(2) Uani d 0.395(3) A 1
F F11 0.0996(6) 0.4562(7) 0.5074(4) 0.0420(14) Uani d 0.395(3) A 1
F F12 0.3186(7) 0.4093(6) 0.4738(3) 0.0524(16) Uani d 0.395(3) A 1
C C10X 0.268(2) 0.405(2) 0.5270(13) 0.036(2) Uani d 0.263(3) A 2
F F10X 0.1355(8) 0.3686(7) 0.5421(4) 0.0576(18) Uani d 0.263(3) A 2
F F11X 0.2545(11) 0.4523(5) 0.4649(3) 0.0505(17) Uani d 0.263(3) A 2
F F12X 0.3659(9) 0.3294(5) 0.5210(3) 0.0386(14) Uani d 0.263(3) A 2
C C10Y 0.240(4) 0.407(3) 0.5329(14) 0.034(2) Uani d 0.342(3) A 3
F F10Y 0.1750(16) 0.3215(14) 0.5617(8) 0.0313(16) Uani d 0.342(3) A 3
F F11Y 0.1430(10) 0.4470(7) 0.4898(4) 0.054(2) Uani d 0.342(3) A 3
F F12Y 0.3533(7) 0.3629(6) 0.4936(4) 0.0454(18) Uani d 0.342(3) A 3
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
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)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Fe1 O2 . . 87.36(4) ?
O1 Fe1 O3 . . 92.08(4) ?
O1 Fe1 O5 . . 90.33(5) ?
O1 Fe1 O6 . . 87.96(5) ?
O3 Fe1 O2 . . 92.11(5) ?
O3 Fe1 O5 . . 92.08(4) ?
O3 Fe1 O6 . . 179.29(5) ?
O4 Fe1 O1 . . 178.59(5) ?
O4 Fe1 O2 . . 91.33(5) ?
O4 Fe1 O3 . . 87.45(5) ?
O4 Fe1 O5 . . 91.02(5) ?
O4 Fe1 O6 . . 92.53(5) ?
O5 Fe1 O2 . . 175.27(4) ?
O5 Fe1 O6 . . 87.20(4) ?
O6 Fe1 O2 . . 88.60(5) ?
C2 O1 Fe1 . . 126.15(10) ?
C4 O2 Fe1 . . 127.14(10) ?
C7 O3 Fe1 . . 128.42(10) ?
C9 O4 Fe1 . . 128.49(11) ?
C12 O5 Fe1 . . 127.77(10) ?
C14 O6 Fe1 . . 126.94(10) ?
F1 C1 C2 . . 111.07(13) ?
F1 C1 F2 . . 107.74(13) ?
F1 C1 F3 . . 108.38(14) ?
F2 C1 C2 . . 109.31(13) ?
F3 C1 C2 . . 112.60(13) ?
F3 C1 F2 . . 107.56(13) ?
O1 C2 C1 . . 113.10(13) ?
O1 C2 C3 . . 127.91(14) ?
C3 C2 C1 . . 118.99(13) ?
C2 C3 H3 . . 119.8 ?
C2 C3 C4 . . 120.35(14) ?
C4 C3 H3 . . 119.8 ?
O2 C4 C3 . . 127.42(14) ?
O2 C4 C5 . . 114.98(13) ?
C3 C4 C5 . . 117.52(14) ?
F4 C5 C4 . . 108.92(13) ?
F5 C5 C4 . . 111.89(13) ?
F5 C5 F4 . . 108.35(15) ?
F6 C5 C4 . . 111.99(14) ?
F6 C5 F4 . . 107.81(14) ?
F6 C5 F5 . . 107.74(14) ?
F7 C6 C7 . . 109.72(14) ?
F8 C6 C7 . . 112.59(16) ?
F8 C6 F7 . . 107.60(16) ?
F9 C6 C7 . . 111.31(13) ?
F9 C6 F7 . . 107.83(17) ?
F9 C6 F8 . . 107.60(15) ?
O3 C7 C6 . . 113.14(14) ?
O3 C7 C8 . . 127.21(15) ?
C8 C7 C6 . . 119.65(15) ?
C7 C8 H8 . . 119.6 ?
C7 C8 C9 . . 120.74(15) ?
C9 C8 H8 . . 119.6 ?
O4 C9 C8 . . 127.44(15) ?
O4 C9 C10 . . 115.6(11) ?
O4 C9 C10X . . 113.2(13) ?
O4 C9 C10Y . . 112.5(14) ?
C8 C9 C10 . . 117.0(11) ?
C8 C9 C10X . . 118.5(12) ?
C8 C9 C10Y . . 120.0(14) ?
F13 C11 C12 . . 109.26(13) ?
F14 C11 C12 . . 111.89(13) ?
F14 C11 F13 . . 107.40(14) ?
F14 C11 F15 . . 108.39(14) ?
F15 C11 C12 . . 112.61(13) ?
F15 C11 F13 . . 107.05(14) ?
O5 C12 C11 . . 113.08(13) ?
O5 C12 C13 . . 127.53(14) ?
C13 C12 C11 . . 119.36(13) ?
C12 C13 H13 . . 119.9 ?
C14 C13 C12 . . 120.21(14) ?
C14 C13 H13 . . 119.9 ?
O6 C14 C13 . . 127.78(14) ?
O6 C14 C15 . . 112.98(13) ?
C13 C14 C15 . . 119.24(13) ?
F16 C15 C14 . . 112.46(13) ?
F16 C15 F17 . . 107.83(14) ?
F16 C15 F18 . . 108.17(13) ?
F17 C15 C14 . . 109.72(13) ?
F18 C15 C14 . . 110.60(13) ?
F18 C15 F17 . . 107.92(14) ?
F10 C10 C9 . . 112.8(18) ?
F10 C10 F11 . . 106(2) ?
F10 C10 F12 . . 115(2) ?
F11 C10 C9 . . 108.2(18) ?
F12 C10 C9 . . 109.2(19) ?
F12 C10 F11 . . 105.1(18) ?
F10X C10X C9 . . 107.1(13) ?
F10X C10X F11X . . 108.2(17) ?
F10X C10X F12X . . 110(2) ?
F11X C10X C9 . . 112.0(18) ?
F12X C10X C9 . . 111.8(15) ?
F12X C10X F11X . . 107.7(15) ?
F10Y C10Y C9 . . 114(2) ?
F10Y C10Y F12Y . . 101(2) ?
F11Y C10Y C9 . . 117(3) ?
F11Y C10Y F10Y . . 108(2) ?
F11Y C10Y F12Y . . 106.8(19) ?
F12Y C10Y C9 . . 108(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O1 . 1.9899(11) ?
Fe1 O2 . 2.0045(11) ?
Fe1 O3 . 1.9921(11) ?
Fe1 O4 . 1.9891(11) ?
Fe1 O5 . 1.9939(11) ?
Fe1 O6 . 1.9971(11) ?
O1 C2 . 1.2670(18) ?
O2 C4 . 1.2568(19) ?
O3 C7 . 1.2582(18) ?
O4 C9 . 1.252(2) ?
O5 C12 . 1.2624(18) ?
O6 C14 . 1.2603(18) ?
C1 C2 . 1.530(2) ?
C1 F1 . 1.3283(19) ?
C1 F2 . 1.337(2) ?
C1 F3 . 1.3321(19) ?
C2 C3 . 1.382(2) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.395(2) ?
C4 C5 . 1.538(2) ?
C5 F4 . 1.329(2) ?
C5 F5 . 1.3233(19) ?
C5 F6 . 1.321(2) ?
C6 C7 . 1.535(2) ?
C6 F7 . 1.328(2) ?
C6 F8 . 1.320(2) ?
C6 F9 . 1.319(2) ?
C7 C8 . 1.387(2) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.389(2) ?
C9 C10 . 1.563(9) ?
C9 C10X . 1.532(13) ?
C9 C10Y . 1.518(12) ?
C11 C12 . 1.532(2) ?
C11 F13 . 1.342(2) ?
C11 F14 . 1.3199(18) ?
C11 F15 . 1.3224(19) ?
C12 C13 . 1.389(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.388(2) ?
C14 C15 . 1.534(2) ?
C15 F16 . 1.3261(19) ?
C15 F17 . 1.3303(19) ?
C15 F18 . 1.3297(19) ?
C10 F10 . 1.26(3) ?
C10 F11 . 1.39(3) ?
C10 F12 . 1.29(4) ?
C10X F10X . 1.29(2) ?
C10X F11X . 1.34(3) ?
C10X F12X . 1.31(2) ?
C10Y F10Y . 1.37(3) ?
C10Y F11Y . 1.28(4) ?
C10Y F12Y . 1.39(4) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Fe1 O1 C2 C1 . . . . 162.11(10) ?
Fe1 O1 C2 C3 . . . . -17.1(2) ?
Fe1 O2 C4 C3 . . . . 5.6(2) ?
Fe1 O2 C4 C5 . . . . -177.78(10) ?
Fe1 O3 C7 C6 . . . . 174.55(10) ?
Fe1 O3 C7 C8 . . . . -4.8(2) ?
Fe1 O4 C9 C8 . . . . -5.1(2) ?
Fe1 O4 C9 C10 . . . . 175.0(16) ?
Fe1 O4 C9 C10X . . . . 163.9(8) ?
Fe1 O4 C9 C10Y . . . . 175.1(17) ?
Fe1 O5 C12 C11 . . . . -177.80(10) ?
Fe1 O5 C12 C13 . . . . 4.3(2) ?
Fe1 O6 C14 C13 . . . . -14.7(2) ?
Fe1 O6 C14 C15 . . . . 165.23(10) ?
O1 C2 C3 C4 . . . . -0.2(3) ?
O2 C4 C5 F4 . . . . -90.73(17) ?
O2 C4 C5 F5 . . . . 149.50(14) ?
O2 C4 C5 F6 . . . . 28.4(2) ?
O3 C7 C8 C9 . . . . 1.2(3) ?
O4 C9 C10 F10 . . . . 11(3) ?
O4 C9 C10 F11 . . . . 127.4(15) ?
O4 C9 C10 F12 . . . . -118.7(17) ?
O4 C9 C10X F10X . . . . 73.1(19) ?
O4 C9 C10X F11X . . . . -168.4(11) ?
O4 C9 C10X F12X . . . . -47(2) ?
O4 C9 C10Y F10Y . . . . 23(4) ?
O4 C9 C10Y F11Y . . . . 151(2) ?
O4 C9 C10Y F12Y . . . . -88(2) ?
O5 C12 C13 C14 . . . . 5.6(2) ?
O6 C14 C15 F16 . . . . 174.67(13) ?
O6 C14 C15 F17 . . . . -65.31(17) ?
O6 C14 C15 F18 . . . . 53.62(18) ?
C1 C2 C3 C4 . . . . -179.35(14) ?
C2 C3 C4 O2 . . . . 6.4(3) ?
C2 C3 C4 C5 . . . . -170.13(14) ?
C3 C4 C5 F4 . . . . 86.24(17) ?
C3 C4 C5 F5 . . . . -33.5(2) ?
C3 C4 C5 F6 . . . . -154.61(15) ?
C6 C7 C8 C9 . . . . -178.15(15) ?
C7 C8 C9 O4 . . . . 4.1(3) ?
C7 C8 C9 C10 . . . . -176.0(16) ?
C7 C8 C9 C10X . . . . -164.4(8) ?
C7 C8 C9 C10Y . . . . -176.1(19) ?
C8 C9 C10 F10 . . . . -169.1(19) ?
C8 C9 C10 F11 . . . . -53(2) ?
C8 C9 C10 F12 . . . . 61(2) ?
C8 C9 C10X F10X . . . . -116.8(18) ?
C8 C9 C10X F11X . . . . 1.6(17) ?
C8 C9 C10X F12X . . . . 122.6(18) ?
C8 C9 C10Y F10Y . . . . -156(2) ?
C8 C9 C10Y F11Y . . . . -28(4) ?
C8 C9 C10Y F12Y . . . . 92(2) ?
C11 C12 C13 C14 . . . . -172.25(14) ?
C12 C13 C14 O6 . . . . 0.1(2) ?
C12 C13 C14 C15 . . . . -179.82(14) ?
C13 C14 C15 F16 . . . . -5.4(2) ?
C13 C14 C15 F17 . . . . 114.61(16) ?
C13 C14 C15 F18 . . . . -126.46(15) ?
F1 C1 C2 O1 . . . . 44.26(18) ?
F1 C1 C2 C3 . . . . -136.47(15) ?
F2 C1 C2 O1 . . . . -74.49(16) ?
F2 C1 C2 C3 . . . . 104.77(16) ?
F3 C1 C2 O1 . . . . 166.02(14) ?
F3 C1 C2 C3 . . . . -14.7(2) ?
F7 C6 C7 O3 . . . . -70.26(19) ?
F7 C6 C7 C8 . . . . 109.16(19) ?
F8 C6 C7 O3 . . . . 169.94(15) ?
F8 C6 C7 C8 . . . . -10.6(2) ?
F9 C6 C7 O3 . . . . 49.0(2) ?
F9 C6 C7 C8 . . . . -131.56(17) ?
F13 C11 C12 O5 . . . . -61.96(17) ?
F13 C11 C12 C13 . . . . 116.16(16) ?
F14 C11 C12 O5 . . . . 56.85(18) ?
F14 C11 C12 C13 . . . . -125.03(16) ?
F15 C11 C12 O5 . . . . 179.23(14) ?
F15 C11 C12 C13 . . . . -2.7(2) ?
_cod_database_fobs_code 2312581