#------------------------------------------------------------------------------
#$Date: 2023-05-06 12:44:56 +0200 (Sat, 06 May 2023) $
#$Revision: 283578 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022713.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_2022713
loop_
_publ_author_name
'Vinaya, ?'
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Syntheses and crystal structures of four
4-(4-meth-oxy-phen-yl)piperazin-1-ium salts: tri-fluoro-acetate,
2,3,4,5,6-penta-fluoro-benzoate, 4-iodo-benzoate, and a polymorph with
4-methyl-benzoate.
;
_journal_coeditor_code VM2279
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 380
_journal_page_last 385
_journal_paper_doi 10.1107/S2056989023002529
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C11 H17 N2 O +, C2 F3 O2 -'
_chemical_formula_moiety 'C11 H17 N2 O +, C2 F3 O2 -'
_chemical_formula_sum 'C13 H17 F3 N2 O3'
_chemical_formula_weight 306.28
_chemical_name_systematic
;
4-(4-Methoxyphenyl)piperazin-1-ium 2,2,2-trifluoroacetate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 16.2967(9)
_cell_length_b 6.0887(2)
_cell_length_c 28.4139(15)
_cell_measurement_reflns_used 9961
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.53
_cell_measurement_theta_min 2.50
_cell_volume 2819.4(2)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008),
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0381
_diffrn_reflns_av_unetI/netI 0.0228
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -36
_diffrn_reflns_number 26032
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.569
_diffrn_reflns_theta_min 1.902
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.128
_exptl_absorpt_correction_T_max 0.958
_exptl_absorpt_correction_T_min 0.847
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.443
_exptl_crystal_description 'solvent-rounded block'
_exptl_crystal_F_000 1280
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.180
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.388
_refine_diff_density_min -0.218
_refine_ls_extinction_coef 0.0023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 200
_refine_ls_number_reflns 3243
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.049
_refine_ls_R_factor_all 0.0403
_refine_ls_R_factor_gt 0.0336
_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^)+(0.0351P)^2^+1.3982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0825
_refine_ls_wR_factor_ref 0.0871
_reflns_number_gt 2802
_reflns_number_total 3243
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2279sup1.cif
_cod_data_source_block I
_cod_depositor_comments
'Adding full bibliography for 2022713--2022716.cif.'
_cod_database_code 2022713
_cod_database_fobs_code 2022713
_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 0.970
_shelx_estimated_absorpt_t_max 0.986
_shelx_hkl_file
;
1 0 0 0.99333 0.60081 2
-1 0 0 0.65688 0.49693 2
-2 0 0 9431.66 291.349 1
-3 0 0 0.88041 1.07991 2
3 0 0 -1.1669 0.69539 2
4 0 0 145.636 7.69194 2
-4 0 0 136.552 7.82182 2
-4 0 0 139.595 7.62331 4
-5 0 0 1.24796 0.73972 3
-5 0 0 2.80997 1.62882 4
5 0 0 1.25241 1.57201 2
-6 0 0 7.02774 1.51105 3
-6 0 0 10.2461 2.75903 4
6 0 0 13.1994 3.08674 2
7 0 0 -0.3603 2.38865 2
-7 0 0 1.18911 2.37230 4
-1 -1 0 0.99542 0.28687 3
1 -1 0 0.67759 0.57784 4
-1 -1 0 0.10327 0.51206 2
-1 1 0 0.63322 0.51333 4
-1 -1 0 1.15861 0.33225 3
1 1 0 0.51251 0.62305 2
1 -1 0 0.54060 0.58153 2
-1 1 0 0.02585 0.44103 2
-2 1 0 0.01797 0.54804 4
2 -1 0 0.68293 0.68235 2
2 1 0 0.41801 0.75315 2
-2 1 0 0.81024 0.67189 2
-2 -1 0 -1.0391 0.52018 2
3 -1 0 0.26273 1.00236 2
-3 -1 0 0.04675 0.21029 3
-3 -1 0 -0.4601 0.92402 2
-3 1 0 0.05119 0.87711 4
-3 1 0 0.87557 1.13825 2
3 1 0 0.84958 1.00338 2
-3 -1 0 0.41182 0.24370 3
4 -1 0 2.35372 1.28017 2
-4 1 0 0.08051 1.56175 2
-4 -1 0 0.39108 1.36358 2
-4 -1 0 0.30592 0.49591 3
-4 -1 0 -0.0416 0.47344 3
-4 1 0 -0.4123 1.06965 4
4 1 0 0.71445 1.17209 2
-5 1 0 0.23396 0.46180 3
-5 1 0 -0.1929 0.41650 3
-5 1 0 0.78454 1.55107 4
-5 -1 0 0.00948 0.69998 3
-5 -1 0 -0.8029 1.29877 4
5 1 0 0.05352 1.67681 2
-5 -1 0 0.92016 0.87297 3
5 -1 0 -2.2823 1.36335 2
-6 -1 0 -0.9073 1.47457 4
-6 -1 0 -1.0808 1.01955 3
-6 1 0 2.56693 1.92751 4
-6 -1 0 0.30153 1.11749 3
-6 1 0 0.57192 0.88067 3
6 -1 0 0.46896 1.72568 2
7 1 0 1.45014 2.46938 2
7 -1 0 -0.0471 2.31392 2
-7 1 0 -2.2368 2.28717 4
-7 -1 0 0.52745 2.50917 4
0 2 0 253.901 8.82659 4
0 2 0 236.007 8.71779 3
0 -2 0 267.182 8.82776 3
0 -2 0 275.306 8.85491 4
-2 -2 0 13.4525 1.14555 3
2 2 0 15.1009 1.87260 2
-2 2 0 11.5917 1.49305 4
-2 -2 0 14.8256 1.81335 2
2 -2 0 15.8049 1.76452 2
-2 2 0 13.1244 1.55936 2
2 -2 0 13.7874 1.60536 4
-2 -2 0 14.9737 1.24348 3
-3 -2 0 1126.42 37.8915 2
-3 2 0 1095.64 37.2041 4
-3 2 0 1132.93 37.5258 2
3 -2 0 1156.56 37.3048 2
-3 -2 0 1155.69 35.6407 3
3 2 0 1122.82 37.8301 2
4 -2 0 37.4448 3.56757 2
-4 2 0 40.4768 3.62916 4
-4 -2 0 35.5920 2.29779 3
4 2 0 37.7841 3.70351 2
-4 -2 0 36.1342 2.50136 3
-4 2 0 38.1383 3.85380 2
-4 -2 0 31.5688 3.81406 2
5 2 0 5.03203 2.20017 2
-5 -2 0 2.97241 1.12009 3
-5 2 0 0.62831 1.51468 4
-5 2 0 1.69065 0.48543 3
5 -2 0 -0.0239 1.53119 2
-5 -2 0 2.22138 1.07787 3
-5 2 0 3.08126 0.54761 3
-6 -2 0 -0.9546 1.39249 3
-6 2 0 7.31617 2.56107 4
-6 -2 0 4.16501 1.91585 4
6 -2 0 1.57575 1.80056 2
-6 2 0 -0.5282 0.77122 3
6 2 0 -1.0249 1.59898 2
-6 -2 0 1.32948 1.28474 3
-7 -2 0 28.7069 5.30456 4
7 -2 0 32.0419 4.60756 2
-7 2 0 35.3272 4.65277 4
7 2 0 21.0780 4.42466 2
0 -3 0 0.38234 0.64488 3
0 -3 0 -0.1622 0.61806 4
0 3 0 -0.1431 0.60538 4
-1 -3 0 0.44444 0.63368 3
1 3 0 0.87117 0.81607 4
1 3 0 -0.5271 0.61435 2
-1 3 0 -0.0952 0.40769 3
-1 -3 0 0.02131 0.45748 4
-1 3 0 0.58515 0.59007 4
-1 -3 0 0.03326 0.61261 2
1 -3 0 1.60496 0.71527 4
-2 3 0 -1.0697 0.41694 4
-2 -3 0 0.20095 0.68833 2
2 3 0 1.97257 0.42429 3
-2 -3 0 0.42150 0.64447 3
-2 3 0 -0.5866 0.62594 2
-2 -3 0 -1.0581 0.51208 4
2 3 0 0.41687 0.27481 3
2 3 0 0.59743 0.97857 2
-3 -3 0 -1.2098 0.94774 2
-3 3 0 -0.2797 0.86872 2
3 -3 0 1.19387 1.05686 2
-3 3 0 -0.4271 0.86479 4
-3 -3 0 1.43279 1.28251 4
-3 -3 0 0.38260 0.66493 3
3 3 0 -1.4843 1.11932 2
-3 -3 0 -0.3881 0.63854 3
-4 -3 0 -0.2205 0.81550 3
-4 -3 0 -0.4077 0.74615 3
-4 3 0 -0.2629 1.23974 4
-4 3 0 0.31429 1.43029 2
4 3 0 1.12747 1.42248 2
4 -3 0 -0.1323 1.20898 2
-4 -3 0 -0.2879 1.64696 2
-5 -3 0 0.50660 1.19856 3
-5 -3 0 1.16921 1.13128 3
-5 3 0 -2.0061 1.11362 4
5 -3 0 3.73880 1.71475 2
5 3 0 -1.3183 1.42522 2
6 3 0 0.42207 1.78920 2
-6 -3 0 0.16128 1.55802 3
-6 3 0 -1.4080 1.65702 4
-6 -3 0 -1.0276 1.26768 3
6 -3 0 0.16445 1.80633 2
-6 3 0 -1.8474 0.81643 3
-7 -3 0 -2.7266 2.57500 4
-7 3 0 0.66482 2.23671 4
7 3 0 5.03395 2.91826 2
-1 4 0 1719.17 54.2250 4
1 4 0 1764.52 54.2127 3
-1 -4 0 1852.84 54.9623 4
-1 4 0 1573.42 53.7985 3
1 4 0 1646.86 54.7842 4
1 -4 0 1713.38 54.1418 4
-1 -4 0 1805.59 54.6747 2
2 -4 0 126.043 5.98974 4
2 4 0 127.178 6.54816 2
-2 4 0 127.998 5.09918 3
-2 4 0 122.537 5.83162 4
-2 -4 0 120.973 6.29315 2
-2 4 0 116.320 5.83149 2
-2 -4 0 127.445 5.90405 3
-2 -4 0 120.694 6.40639 4
-3 -4 0 80.2890 5.61799 4
3 -4 0 84.5113 5.15766 4
-3 4 0 87.8504 5.09909 4
-3 4 0 90.7265 5.36777 2
3 4 0 92.7535 5.84966 2
-3 4 0 79.9514 3.35232 3
-3 -4 0 85.9663 4.75243 3
-3 -4 0 78.8713 5.54800 2
4 4 0 39.7331 4.23153 2
-4 -4 0 38.0257 4.40262 4
-4 -4 0 45.7041 3.53959 3
-4 -4 0 43.1575 4.35653 2
-4 4 0 41.6735 2.01478 3
-4 4 0 43.9567 4.11389 2
-4 4 0 37.6290 3.67510 4
5 4 0 8.24797 2.97211 2
-5 4 0 9.58333 2.49483 4
-5 -4 0 8.43165 1.99204 3
-6 4 0 62.9949 5.70373 4
-6 -4 0 61.5744 5.00737 3
-6 4 0 61.6771 3.68407 3
6 4 0 70.7106 6.58252 2
7 4 0 188.407 11.7366 2
-7 4 0 186.793 11.0805 4
0 5 0 2.77587 1.11800 3
0 -5 0 1.18709 0.84979 4
0 -5 0 1.33648 0.95112 3
0 5 0 2.06366 1.06264 4
1 5 0 -0.1480 0.76978 3
-1 -5 0 0.63573 0.83510 4
1 -5 0 0.47249 0.77504 4
-1 -5 0 0.06856 0.90190 3
1 5 0 0.80007 0.77418 4
1 5 0 -0.0255 0.85080 2
-1 5 0 0.50838 0.77858 4
-1 5 0 0.05067 0.69749 3
2 5 0 -0.2849 1.03547 2
-2 5 0 0.29578 0.73033 4
-2 5 0 0.86580 0.74058 3
-2 -5 0 1.34948 1.08580 2
-2 -5 0 1.47343 1.14267 4
2 -5 0 -0.3588 0.80968 4
-2 5 0 1.10616 1.14648 2
2 5 0 0.41865 0.76560 3
2 5 0 2.53951 0.97644 3
-2 -5 0 -1.1622 0.66454 3
3 5 0 -0.9788 0.99000 2
3 -5 0 -0.8425 0.93863 4
-3 -5 0 0.36676 1.26934 4
-3 -5 0 0.13488 1.28802 2
-3 5 0 -1.3645 0.94194 2
-3 5 0 -0.4192 0.57975 3
-3 5 0 -0.8380 0.76509 4
-3 -5 0 -1.4708 0.78865 3
-4 5 0 0.80744 1.54988 2
-4 5 0 -2.0583 0.94453 4
-4 -5 0 0.63053 1.12154 3
-4 5 0 -0.6366 0.60202 3
-5 5 0 -0.0654 1.47676 4
-5 -5 0 -2.1350 1.18097 3
5 5 0 2.27912 1.72854 2
-5 5 0 -0.8026 0.81355 3
6 5 0 0.04574 2.20791 2
-6 5 0 -0.3673 1.74705 4
-6 5 0 0.55024 1.11419 3
-6 -5 0 1.55489 1.65247 3
7 5 0 3.21460 2.87480 2
-7 -5 0 2.55961 2.30552 3
-7 5 0 2.17485 2.63702 4
0 6 0 353.961 13.5189 3
0 6 0 364.195 13.8101 4
0 -6 0 340.593 13.3710 4
0 -6 0 348.151 13.4443 3
-1 6 0 3790.27 117.540 3
-2 -6 0 306.498 13.2110 4
-2 -6 0 301.436 12.6712 3
2 6 0 310.358 11.9348 3
-2 6 0 319.984 12.5851 4
2 -6 0 320.785 12.5022 4
2 6 0 304.058 13.2572 2
-2 -6 0 330.364 13.1329 2
-2 6 0 317.434 11.9821 3
2 6 0 311.049 13.5284 4
3 6 0 84.6126 5.07053 3
-3 6 0 78.5730 4.32398 3
3 -6 0 77.5882 5.20746 4
3 6 0 82.7780 3.96991 3
-3 -6 0 84.9701 5.37652 3
-3 6 0 81.5523 5.18209 4
3 6 0 88.5003 6.14055 2
-3 -6 0 74.1698 5.75920 4
-3 6 0 68.7580 5.02788 2
-3 -6 0 85.8674 5.84718 2
-4 6 0 393.866 16.0562 4
4 6 0 390.883 17.3133 2
-4 6 0 377.341 14.1439 3
-4 -6 0 417.723 16.2647 3
-5 6 0 33.5024 3.86245 4
5 6 0 37.7480 4.69842 2
-5 6 0 36.4844 2.94886 3
-6 -6 0 10.7163 2.84073 3
6 6 0 11.0272 3.41093 2
-6 6 0 6.96708 2.45198 4
-6 6 0 12.4677 2.24492 3
7 6 0 2.76983 2.91703 2
-7 -6 0 -0.3208 2.36814 3
-7 6 0 3.19218 2.74477 4
0 -7 0 2.07914 1.18940 3
0 -7 0 -0.7233 0.95978 4
0 7 0 0.49987 0.82002 4
0 7 0 1.28808 1.13360 3
1 7 0 0.33803 1.16951 4
1 7 0 -0.1863 0.74692 2
-1 7 0 -1.1988 0.68292 3
-1 -7 0 -0.9588 0.62204 4
-1 7 0 -1.3693 0.81085 4
1 7 0 1.74706 1.11544 3
-1 -7 0 -0.1989 0.98815 3
1 -7 0 -0.1423 0.78511 4
-2 7 0 0.76585 1.04441 4
-2 -7 0 -1.0498 0.99383 4
2 -7 0 -0.2562 0.90774 4
-2 7 0 0.22716 0.88138 3
2 7 0 -0.1856 0.93753 2
2 7 0 -1.5228 1.00862 4
-2 -7 0 0.01916 1.00526 3
2 7 0 -0.6244 0.88690 3
-2 -7 0 -0.5830 1.02534 2
-3 7 0 0.78676 1.33183 2
-3 -7 0 -0.4201 1.15597 3
-3 7 0 1.34259 1.29189 4
3 -7 0 -1.7990 1.03509 4
3 7 0 0.33377 0.82301 3
-3 7 0 -0.9627 0.97049 3
3 7 0 -0.8882 1.21332 2
3 7 0 -0.7550 0.72257 3
-4 7 0 -0.2826 1.36522 4
4 7 0 -0.8232 1.33815 2
-4 7 0 -0.2963 1.06040 3
5 7 0 -1.0946 2.10941 2
-5 -7 0 1.03777 1.76923 3
-5 7 0 1.32799 1.25002 3
-5 7 0 -0.2644 1.44501 4
-6 7 0 3.28770 1.84002 3
-6 7 0 4.70737 2.45705 4
-6 -7 0 0.05589 1.89293 3
-7 -7 0 -1.9175 2.62533 3
7 7 0 2.31692 3.15822 2
0 8 0 1.95035 1.25550 4
0 -8 0 1.36763 1.03458 4
0 -8 0 3.26222 1.54240 3
0 8 0 2.24455 1.44411 3
-1 -8 0 1071.53 36.1904 3
-1 -8 0 1035.76 36.0449 4
1 8 0 1082.66 35.8140 3
1 -8 0 1010.20 35.3107 4
1 8 0 1073.89 36.6607 4
1 8 0 1059.44 36.2982 2
-1 8 0 999.925 35.6564 4
2 -8 0 305.484 12.4544 4
2 8 0 296.441 13.6269 4
-2 8 0 290.360 12.1921 3
-2 -8 0 275.977 12.9816 4
-2 -8 0 290.779 12.9358 3
2 8 0 281.826 13.2026 2
-2 8 0 269.955 12.3388 4
3 8 0 156.563 7.39438 3
3 8 0 159.583 9.55174 2
-3 8 0 169.199 8.79823 4
3 8 0 171.371 7.49406 3
-3 8 0 165.095 8.08576 3
-4 -8 0 75.5171 6.13150 3
4 8 0 73.4156 6.56454 2
-4 8 0 58.3409 6.93378 3
-4 8 0 77.3416 5.79415 4
-5 -8 0 46.6559 5.12861 3
-5 8 0 45.2838 4.89879 4
5 8 0 36.9408 5.59645 2
-5 8 0 39.5219 3.94400 3
-6 -8 0 52.2498 5.89204 3
6 8 0 38.5104 5.67246 2
-6 8 0 45.7840 5.02574 4
-6 8 0 38.0082 5.95865 3
7 8 0 23.3758 5.53125 2
-7 8 0 27.7653 5.19744 4
0 9 0 3.91227 1.78834 4
0 -9 0 5.40977 1.91937 3
0 -9 0 2.10235 1.44758 4
0 9 0 2.31495 1.41979 3
1 9 0 -0.5403 0.87035 2
1 -9 0 -0.4660 1.13451 4
-1 -9 0 -1.7251 1.07142 3
-1 -9 0 -0.3287 1.22933 4
1 9 0 2.00683 1.48514 3
1 9 0 1.71243 1.42216 4
-1 9 0 1.00767 1.44490 3
-1 9 0 0.31797 1.37572 4
2 9 0 0.24364 1.55362 4
2 -9 0 0.22564 1.16346 4
2 9 0 1.23417 1.64378 2
-2 9 0 -0.4439 1.29869 3
2 9 0 -1.7898 1.08171 3
-2 -9 0 -1.6541 1.36584 3
-2 9 0 0.99420 1.38743 4
3 9 0 -0.9565 1.26405 3
-3 9 0 0.30094 1.33960 3
-3 -9 0 1.20770 1.46320 3
3 9 0 -0.1205 1.84468 2
-3 9 0 1.03039 1.43660 4
3 9 0 -1.3047 1.11362 3
-4 9 0 -0.3356 1.52161 3
-4 9 0 0.26764 1.44280 4
4 9 0 -4.1521 1.51735 2
-4 -9 0 3.43983 2.02006 3
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;
_shelx_hkl_checksum 5088
_shelx_res_file
;
TITL m22264 : space group Pbca
m22264.res
created by SHELXL-2019/2 at 16:57:21 on 27-Feb-2023
CELL 0.71073 16.2967 6.0887 28.4139 90.000 90.000 90.000
ZERR 8 0.0009 0.0002 0.0015 0.000 0.000 0.000
LATT 1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H N O F
UNIT 104 136 16 24 24
TEMP -183
SIZE 0.24 0.18 0.11
REM FORM solvent-rounded block
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds
HTAB N1 O2
EQIV $1 x, y+1, z
HTAB N1 O3_$1
EQIV $2 -x+1, y-1/2, -z+3/2
HTAB C3 O1_$2
EQIV $3 -x+1, -y, -z+1
HTAB C4 F1_$3
EQIV $4 -x+1, -y+1, -z+1
HTAB C4 O2_$4
EQIV $5 -x+3/2, -y+1, z+1/2
HTAB C11 F3_$5
HTAB
REM Relative twist of benzene and piperazinium rings:
MPLA C1 C2 C3 C4
MPLA C5 C6 C7 C8 C9 C10
REM Out of planarity of methoxy group:
RTAB tors C9 C8 O1 C11
MPLA 7 C5 C6 C7 C8 C9 C10 O1 C11
REM Out of planarity of N2:
RTAB angl C2 N2 C3
RTAB angl C3 N2 C5
RTAB angl C5 N2 C2
REM Geometry of anion:
MPLA C12 O2 O3
MPLA C12 C13 F3
REM
FMAP 2
PLAN 20
WGHT 0.035100 1.398200
EXTI 0.002334
FVAR 0.51187
O1 4 0.643476 0.881384 0.847407 11.00000 0.01883 0.02161 =
0.01240 -0.00238 -0.00007 -0.00110
N1 3 0.578798 0.573509 0.562199 11.00000 0.01804 0.01378 =
0.01242 0.00002 -0.00115 0.00075
H1A 2 0.574610 0.487097 0.535013 11.00000 0.02888
H1B 2 0.568006 0.712968 0.553547 11.00000 0.02263
N2 3 0.617705 0.600175 0.660374 11.00000 0.01480 0.02021 =
0.01141 0.00021 -0.00082 -0.00267
C1 1 0.664838 0.563875 0.579439 11.00000 0.01563 0.02319 =
0.01497 0.00000 -0.00011 0.00220
AFIX 23
H1C 2 0.702091 0.626714 0.555436 11.00000 -1.20000
H1D 2 0.680835 0.408985 0.584747 11.00000 -1.20000
AFIX 0
C2 1 0.672965 0.692114 0.625120 11.00000 0.01465 0.02306 =
0.01377 0.00108 0.00016 -0.00259
AFIX 23
H2A 2 0.730261 0.684243 0.636575 11.00000 -1.20000
H2B 2 0.659190 0.848350 0.619580 11.00000 -1.20000
AFIX 0
C3 1 0.532552 0.619246 0.643896 11.00000 0.01448 0.02523 =
0.01407 -0.00134 -0.00081 -0.00230
AFIX 23
H3A 2 0.519051 0.775947 0.638751 11.00000 -1.20000
H3B 2 0.494967 0.561212 0.668281 11.00000 -1.20000
AFIX 0
C4 1 0.520251 0.493507 0.598610 11.00000 0.01776 0.02277 =
0.01368 -0.00022 -0.00095 -0.00439
AFIX 23
H4A 2 0.529255 0.334880 0.604256 11.00000 -1.20000
H4B 2 0.463242 0.513595 0.587369 11.00000 -1.20000
AFIX 0
C5 1 0.627494 0.681736 0.707303 11.00000 0.01510 0.01844 =
0.01281 0.00034 -0.00150 0.00014
C6 1 0.673646 0.865682 0.718512 11.00000 0.01947 0.02178 =
0.01467 0.00241 0.00042 -0.00478
AFIX 43
H6 2 0.700715 0.944071 0.694126 11.00000 -1.20000
AFIX 0
C7 1 0.681137 0.938167 0.765066 11.00000 0.01991 0.01882 =
0.01693 -0.00084 -0.00193 -0.00503
AFIX 43
H7 2 0.713564 1.063514 0.772171 11.00000 -1.20000
AFIX 0
C8 1 0.641066 0.826303 0.800677 11.00000 0.01454 0.01860 =
0.01304 -0.00094 -0.00162 0.00282
C9 1 0.594538 0.640500 0.789818 11.00000 0.01693 0.02090 =
0.01501 0.00273 0.00073 -0.00205
AFIX 43
H9 2 0.567039 0.563175 0.814201 11.00000 -1.20000
AFIX 0
C10 1 0.588212 0.568294 0.743833 11.00000 0.01911 0.01846 =
0.01703 0.00017 -0.00125 -0.00436
AFIX 43
H10 2 0.556949 0.440604 0.736930 11.00000 -1.20000
AFIX 0
C11 1 0.688479 1.074161 0.859628 11.00000 0.02340 0.02345 =
0.01805 -0.00473 -0.00225 -0.00252
AFIX 137
H11A 2 0.683518 1.100895 0.893519 11.00000 -1.50000
H11B 2 0.666423 1.200190 0.842301 11.00000 -1.50000
H11C 2 0.746404 1.053795 0.851455 11.00000 -1.50000
AFIX 0
F1 5 0.620027 -0.250219 0.467953 11.00000 0.04369 0.01279 =
0.02179 -0.00198 0.00566 0.00065
F2 5 0.600562 0.009734 0.418587 11.00000 0.07764 0.02543 =
0.01345 -0.00110 0.00243 0.00965
F3 5 0.711969 -0.002555 0.458759 11.00000 0.02684 0.04612 =
0.07250 -0.02510 0.02455 -0.00872
O2 4 0.574753 0.296127 0.487718 11.00000 0.03414 0.01611 =
0.01743 -0.00135 -0.00321 0.00534
O3 4 0.592308 0.025712 0.540046 11.00000 0.05515 0.01754 =
0.01440 0.00088 0.00360 0.00275
C12 1 0.594529 0.108568 0.500370 11.00000 0.01551 0.01437 =
0.01544 -0.00184 -0.00012 -0.00204
C13 1 0.631124 -0.035776 0.460904 11.00000 0.02466 0.01553 =
0.01918 0.00021 0.00538 -0.00198
HKLF 4 1 0 1 0 1 0 0 0 0 -1
REM m22264 : space group Pbca
REM wR2 = 0.0871, GooF = S = 1.049, Restrained GooF = 1.049 for all data
REM R1 = 0.0336 for 2802 Fo > 4sig(Fo) and 0.0403 for all 3243 data
REM 200 parameters refined using 0 restraints
END
WGHT 0.0351 1.3981
REM Instructions for potential hydrogen bonds
HTAB N1 O2
HTAB N1 O3_$1
HTAB C3 O1_$2
HTAB C4 F1_$3
HTAB C4 O2_$4
HTAB C11 F3_$5
REM Highest difference peak 0.388, deepest hole -0.218, 1-sigma level 0.041
Q1 1 0.6067 0.0261 0.4795 11.00000 0.05 0.39
Q2 1 0.6637 0.6368 0.6005 11.00000 0.05 0.30
Q3 1 0.5287 0.5541 0.6206 11.00000 0.05 0.27
Q4 1 0.5956 0.6036 0.7673 11.00000 0.05 0.25
Q5 1 0.6162 0.6138 0.7275 11.00000 0.05 0.25
Q6 1 0.6508 0.8818 0.7827 11.00000 0.05 0.24
Q7 1 0.6692 0.9084 0.7399 11.00000 0.05 0.24
Q8 1 0.6264 0.7276 0.7940 11.00000 0.05 0.24
Q9 1 0.6435 0.6432 0.6417 11.00000 0.05 0.23
Q10 1 0.6217 0.6480 0.6828 11.00000 0.05 0.23
Q11 1 0.6592 0.7444 0.7136 11.00000 0.05 0.22
Q12 1 0.5766 0.5940 0.6526 11.00000 0.05 0.21
Q13 1 0.6451 0.8648 0.8208 11.00000 0.05 0.20
Q14 1 0.6230 0.5705 0.5719 11.00000 0.05 0.19
Q15 1 0.6439 0.0339 0.4307 11.00000 0.05 0.18
Q16 1 0.5774 0.0439 0.5207 11.00000 0.05 0.17
Q17 1 0.5455 0.5418 0.5798 11.00000 0.05 0.15
Q18 1 0.6339 0.4783 0.6564 11.00000 0.05 0.14
Q19 1 0.5483 0.2244 0.4977 11.00000 0.05 0.14
Q20 1 0.6824 0.8330 0.6186 11.00000 0.05 0.14
;
_shelx_res_checksum 90033
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
O O1 0.64348(5) 0.88138(14) 0.84741(3) 0.01761(19) Uani d 1 . .
N N1 0.57880(6) 0.57351(17) 0.56220(3) 0.0147(2) Uani d 1 . .
H H1A 0.5746(10) 0.487(3) 0.5350(6) 0.029(4) Uiso d 1 . .
H H1B 0.5680(9) 0.713(3) 0.5535(5) 0.023(4) Uiso d 1 . .
N N2 0.61770(6) 0.60018(16) 0.66037(3) 0.0155(2) Uani d 1 . .
C C1 0.66484(7) 0.5639(2) 0.57944(4) 0.0179(2) Uani d 1 . .
H H1C 0.702091 0.626714 0.555436 0.022 Uiso calc 1 . .
H H1D 0.680835 0.408985 0.584747 0.022 Uiso calc 1 . .
C C2 0.67297(7) 0.6921(2) 0.62512(4) 0.0172(2) Uani d 1 . .
H H2A 0.730261 0.684243 0.636575 0.021 Uiso calc 1 . .
H H2B 0.659190 0.848350 0.619580 0.021 Uiso calc 1 . .
C C3 0.53255(7) 0.6192(2) 0.64390(4) 0.0179(2) Uani d 1 . .
H H3A 0.519051 0.775947 0.638751 0.022 Uiso calc 1 . .
H H3B 0.494967 0.561212 0.668281 0.022 Uiso calc 1 . .
C C4 0.52025(7) 0.4935(2) 0.59861(4) 0.0181(2) Uani d 1 . .
H H4A 0.529255 0.334880 0.604256 0.022 Uiso calc 1 . .
H H4B 0.463242 0.513595 0.587369 0.022 Uiso calc 1 . .
C C5 0.62749(7) 0.68174(19) 0.70730(4) 0.0155(2) Uani d 1 . .
C C6 0.67365(7) 0.8657(2) 0.71851(4) 0.0186(3) Uani d 1 . .
H H6 0.700715 0.944071 0.694126 0.022 Uiso calc 1 . .
C C7 0.68114(7) 0.9382(2) 0.76507(4) 0.0186(2) Uani d 1 . .
H H7 0.713564 1.063514 0.772171 0.022 Uiso calc 1 . .
C C8 0.64107(7) 0.82630(19) 0.80068(4) 0.0154(2) Uani d 1 . .
C C9 0.59454(7) 0.6405(2) 0.78982(4) 0.0176(2) Uani d 1 . .
H H9 0.567039 0.563175 0.814201 0.021 Uiso calc 1 . .
C C10 0.58821(7) 0.5683(2) 0.74383(4) 0.0182(2) Uani d 1 . .
H H10 0.556949 0.440604 0.736930 0.022 Uiso calc 1 . .
C C11 0.68848(8) 1.0742(2) 0.85963(4) 0.0216(3) Uani d 1 . .
H H11A 0.683518 1.100895 0.893519 0.032 Uiso calc 1 . .
H H11B 0.666423 1.200190 0.842301 0.032 Uiso calc 1 . .
H H11C 0.746404 1.053795 0.851455 0.032 Uiso calc 1 . .
F F1 0.62003(5) -0.25022(11) 0.46795(3) 0.02609(19) Uani d 1 . .
F F2 0.60056(6) 0.00973(14) 0.41859(3) 0.0388(2) Uani d 1 . .
F F3 0.71197(5) -0.00256(16) 0.45876(4) 0.0485(3) Uani d 1 . .
O O2 0.57475(6) 0.29613(14) 0.48772(3) 0.0226(2) Uani d 1 . .
O O3 0.59231(7) 0.02571(15) 0.54005(3) 0.0290(2) Uani d 1 . .
C C12 0.59453(7) 0.10857(19) 0.50037(4) 0.0151(2) Uani d 1 . .
C C13 0.63112(8) -0.0358(2) 0.46090(4) 0.0198(3) Uani d 1 . .
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
O1 0.0188(4) 0.0216(4) 0.0124(4) -0.0011(3) -0.0001(3) -0.0024(3)
N1 0.0180(5) 0.0138(5) 0.0124(4) 0.0007(4) -0.0012(4) 0.0000(4)
N2 0.0148(5) 0.0202(5) 0.0114(4) -0.0027(4) -0.0008(3) 0.0002(4)
C1 0.0156(5) 0.0232(6) 0.0150(5) 0.0022(5) -0.0001(4) 0.0000(4)
C2 0.0146(5) 0.0231(6) 0.0138(5) -0.0026(4) 0.0002(4) 0.0011(4)
C3 0.0145(5) 0.0252(6) 0.0141(5) -0.0023(4) -0.0008(4) -0.0013(4)
C4 0.0178(5) 0.0228(6) 0.0137(5) -0.0044(5) -0.0009(4) -0.0002(4)
C5 0.0151(5) 0.0184(5) 0.0128(5) 0.0001(4) -0.0015(4) 0.0003(4)
C6 0.0195(6) 0.0218(6) 0.0147(5) -0.0048(5) 0.0004(4) 0.0024(4)
C7 0.0199(6) 0.0188(6) 0.0169(5) -0.0050(5) -0.0019(4) -0.0008(4)
C8 0.0145(5) 0.0186(6) 0.0130(5) 0.0028(4) -0.0016(4) -0.0009(4)
C9 0.0169(5) 0.0209(6) 0.0150(5) -0.0020(5) 0.0007(4) 0.0027(4)
C10 0.0191(6) 0.0185(6) 0.0170(5) -0.0044(5) -0.0012(4) 0.0002(4)
C11 0.0234(6) 0.0235(6) 0.0181(5) -0.0025(5) -0.0022(5) -0.0047(5)
F1 0.0437(5) 0.0128(4) 0.0218(4) 0.0006(3) 0.0057(3) -0.0020(3)
F2 0.0776(7) 0.0254(4) 0.0134(4) 0.0096(4) 0.0024(4) -0.0011(3)
F3 0.0268(5) 0.0461(6) 0.0725(7) -0.0087(4) 0.0245(4) -0.0251(5)
O2 0.0341(5) 0.0161(4) 0.0174(4) 0.0053(4) -0.0032(4) -0.0013(3)
O3 0.0552(7) 0.0175(4) 0.0144(4) 0.0027(4) 0.0036(4) 0.0009(3)
C12 0.0155(5) 0.0144(5) 0.0154(5) -0.0020(4) -0.0001(4) -0.0018(4)
C13 0.0247(6) 0.0155(6) 0.0192(6) -0.0020(5) 0.0054(5) 0.0002(4)
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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
C8 O1 C11 . . 116.87(9) ?
C1 N1 C4 . . 111.25(9) ?
C1 N1 H1A . . 108.6(10) ?
C4 N1 H1A . . 110.0(10) ?
C1 N1 H1B . . 108.1(9) ?
C4 N1 H1B . . 111.9(9) ?
H1A N1 H1B . . 106.9(13) ?
C5 N2 C2 . . 115.95(9) ?
C5 N2 C3 . . 112.00(9) ?
C2 N2 C3 . . 109.51(9) ?
N1 C1 C2 . . 110.07(9) ?
N1 C1 H1C . . 109.6 ?
C2 C1 H1C . . 109.6 ?
N1 C1 H1D . . 109.6 ?
C2 C1 H1D . . 109.6 ?
H1C C1 H1D . . 108.2 ?
N2 C2 C1 . . 109.59(9) ?
N2 C2 H2A . . 109.8 ?
C1 C2 H2A . . 109.8 ?
N2 C2 H2B . . 109.8 ?
C1 C2 H2B . . 109.8 ?
H2A C2 H2B . . 108.2 ?
N2 C3 C4 . . 110.90(9) ?
N2 C3 H3A . . 109.5 ?
C4 C3 H3A . . 109.5 ?
N2 C3 H3B . . 109.5 ?
C4 C3 H3B . . 109.5 ?
H3A C3 H3B . . 108.0 ?
N1 C4 C3 . . 109.93(9) ?
N1 C4 H4A . . 109.7 ?
C3 C4 H4A . . 109.7 ?
N1 C4 H4B . . 109.7 ?
C3 C4 H4B . . 109.7 ?
H4A C4 H4B . . 108.2 ?
C6 C5 C10 . . 118.42(10) ?
C6 C5 N2 . . 123.69(10) ?
C10 C5 N2 . . 117.90(10) ?
C5 C6 C7 . . 121.28(11) ?
C5 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
C8 C7 C6 . . 119.65(11) ?
C8 C7 H7 . . 120.2 ?
C6 C7 H7 . . 120.2 ?
O1 C8 C7 . . 125.08(11) ?
O1 C8 C9 . . 115.34(10) ?
C7 C8 C9 . . 119.57(10) ?
C10 C9 C8 . . 120.46(11) ?
C10 C9 H9 . . 119.8 ?
C8 C9 H9 . . 119.8 ?
C9 C10 C5 . . 120.61(11) ?
C9 C10 H10 . . 119.7 ?
C5 C10 H10 . . 119.7 ?
O1 C11 H11A . . 109.5 ?
O1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
O1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O3 C12 O2 . . 129.27(11) ?
O3 C12 C13 . . 116.19(10) ?
O2 C12 C13 . . 114.45(10) ?
F2 C13 F1 . . 106.79(10) ?
F2 C13 F3 . . 107.26(11) ?
F1 C13 F3 . . 106.81(11) ?
F2 C13 C12 . . 113.14(10) ?
F1 C13 C12 . . 113.32(9) ?
F3 C13 C12 . . 109.16(10) ?
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
O1 C8 . 1.3701(13) ?
O1 C11 . 1.4269(15) ?
N1 C1 . 1.4864(15) ?
N1 C4 . 1.4893(14) ?
N1 H1A . 0.937(16) ?
N1 H1B . 0.901(16) ?
N2 C5 . 1.4318(14) ?
N2 C2 . 1.4587(14) ?
N2 C3 . 1.4692(14) ?
C1 C2 . 1.5205(16) ?
C1 H1C . 0.9900 ?
C1 H1D . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.5106(15) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.3862(16) ?
C5 C10 . 1.4015(16) ?
C6 C7 . 1.3998(16) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3835(16) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.3964(17) ?
C9 C10 . 1.3824(16) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
F1 C13 . 1.3333(14) ?
F2 C13 . 1.3306(14) ?
F3 C13 . 1.3343(15) ?
O2 C12 . 1.2399(14) ?
O3 C12 . 1.2356(14) ?
C12 C13 . 1.5445(16) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A O2 . 0.937(16) 1.777(16) 2.7084(13) 172.1(15) yes
N1 H1B O3 1_565 0.901(16) 1.982(16) 2.8329(14) 156.7(13) yes
C3 H3B O1 3_646 0.99 2.55 3.2230(14) 125 yes
C4 H4B F1 5_656 0.99 2.62 3.3162(14) 127 yes
C4 H4B O2 5_666 0.99 2.51 3.1709(14) 124 yes
C11 H11A F3 2_665 0.98 2.59 3.2796(15) 128 yes
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
C4 N1 C1 C2 . . . . -55.67(12) ?
C5 N2 C2 C1 . . . . 170.74(9) ?
C3 N2 C2 C1 . . . . -61.35(12) ?
N1 C1 C2 N2 . . . . 58.98(12) ?
C5 N2 C3 C4 . . . . -168.97(9) ?
C2 N2 C3 C4 . . . . 60.94(12) ?
C1 N1 C4 C3 . . . . 54.44(12) ?
N2 C3 C4 N1 . . . . -56.90(12) ?
C2 N2 C5 C6 . . . . 12.65(16) ?
C3 N2 C5 C6 . . . . -114.02(12) ?
C2 N2 C5 C10 . . . . -167.21(10) ?
C3 N2 C5 C10 . . . . 66.12(13) ?
C10 C5 C6 C7 . . . . -0.13(18) ?
N2 C5 C6 C7 . . . . -179.99(11) ?
C5 C6 C7 C8 . . . . -0.78(18) ?
C11 O1 C8 C7 . . . . 2.48(16) ?
C11 O1 C8 C9 . . . . -178.21(10) ?
C6 C7 C8 O1 . . . . -179.82(11) ?
C6 C7 C8 C9 . . . . 0.89(18) ?
O1 C8 C9 C10 . . . . -179.47(10) ?
C7 C8 C9 C10 . . . . -0.12(18) ?
C8 C9 C10 C5 . . . . -0.80(18) ?
C6 C5 C10 C9 . . . . 0.91(18) ?
N2 C5 C10 C9 . . . . -179.22(11) ?
O3 C12 C13 F2 . . . . 151.49(11) ?
O2 C12 C13 F2 . . . . -31.49(15) ?
O3 C12 C13 F1 . . . . 29.73(16) ?
O2 C12 C13 F1 . . . . -153.24(11) ?
O3 C12 C13 F3 . . . . -89.16(13) ?
O2 C12 C13 F3 . . . . 87.86(13) ?