#------------------------------------------------------------------------------
#$Date: 2025-12-28 17:37:21 +0100 (Sun, 28 Dec 2025) $
#$Revision: 304188 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023543.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_2023543
loop_
_publ_author_name
'Patel, Bhumi C.'
'Modi, Krunal M.'
'Reddy, J. Prakasha'
_publ_contact_author_address
;
School of Applied Material Sciences
Central University of Gujarat
Vadodara, India
;
_publ_contact_author_email j.prakashareddy@cug.ac.in
_publ_contact_author_name 'Prakasha Reddy'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of anhydrous salt of
levofloxacin and 4-methylbenzoic acid
;
_journal_coeditor_code EE2021
_journal_date_accepted 2025-11-11
_journal_date_recd_electronic 2025-09-24
_journal_issue 12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1149
_journal_page_last 1152
_journal_paper_category GO
_journal_paper_doi 10.1107/S2056989025010047
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration rm
_chemical_formula_iupac 'C18 H21 F N3 O4 +, C8 H7 O2 -'
_chemical_formula_moiety 'C18 H21 F N3 O4 +, C8 H7 O2 -'
_chemical_formula_sum 'C26 H28 F N3 O6'
_chemical_formula_weight 497.51
_chemical_name_common
;
Levofloxacinium 4-methylbenzoate
;
_chemical_name_systematic
'4-{11-Carboxy-7-fluoro-2-methyl-10-oxo-4-oxa-1-azatricyclo[7.3.1.0^{5,13}^]trideca-5,7,9(13),11-tetraen-6-yl}-1-methylpiperazin-1-ium 4-methylbenzoate'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.1788(10)
_cell_length_b 13.0274(13)
_cell_length_c 25.979(3)
_cell_measurement_reflns_used 3952
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.5
_cell_volume 2429.6(5)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker SMART APEXII CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1157
_diffrn_reflns_av_unetI/netI 0.1198
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 17036
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.235
_diffrn_reflns_theta_min 1.749
_diffrn_source 'fine-focus sealed xray tube'
_exptl_absorpt_coefficient_mu 0.102
_exptl_absorpt_correction_T_max 0.7455
_exptl_absorpt_correction_T_min 0.5745
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'clear whiteish colourless'
_exptl_crystal_density_diffrn 1.360
_exptl_crystal_description irregular
_exptl_crystal_F_000 1048
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.23
_refine_diff_density_max 0.228
_refine_diff_density_min -0.173
_refine_ls_abs_structure_details
;
Flack x determined using 707 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.02(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.001
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 330
_refine_ls_number_reflns 5409
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.000
_refine_ls_R_factor_all 0.1617
_refine_ls_R_factor_gt 0.0601
_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^)+(0.0526P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1291
_refine_ls_wR_factor_ref 0.1767
_reflns_number_gt 2456
_reflns_number_total 5409
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ee2021sup1.cif
_cod_data_source_block I
_cod_database_code 2023543
_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_hkl_file
;
-1 0 0 0.64 0.67
1 0 0 -0.23 0.54
-2 0 0 5235.50 451.04
2 0 0 5163.15 450.99
-3 0 0 0.26 1.64
3 0 0 -0.42 1.38
-4 0 0 56.45 9.44
4 0 0 70.03 10.05
-5 0 0 3.84 2.50
5 0 0 0.49 3.23
-6 0 0 594.61 56.96
-7 0 0 5.31 4.24
8 0 0 19.67 10.19
9 0 0 0.45 5.18
9 -1 0 -4.57 5.28
8 -1 0 13.50 6.50
7 -1 0 -1.73 4.26
-7 1 0 -3.33 3.31
-6 1 0 15.63 4.45
-5 1 0 10.92 4.57
4 -1 0 1095.01 107.99
-4 1 0 1324.96 108.87
3 -1 0 0.59 1.80
-3 1 0 0.92 1.62
2 -1 0 2114.45 179.92
-2 1 0 2000.20 179.96
1 -1 0 273.00 24.31
-1 1 0 248.19 23.70
-1 -1 0 280.39 25.24
1 1 0 285.81 25.32
-2 -1 0 2609.94 222.16
2 1 0 2493.58 222.22
-3 -1 0 0.08 1.30
3 1 0 1.45 1.74
-4 -1 0 1084.99 97.76
4 1 0 1092.51 98.02
-5 -1 0 12.77 4.45
5 1 0 -0.30 2.93
-6 -1 0 16.24 4.72
-7 -1 0 -0.22 3.30
9 1 0 -10.97 5.60
9 -2 0 2.38 6.28
8 -2 0 3.62 4.64
7 -2 0 -9.87 3.71
-7 2 0 7.62 4.46
6 -2 0 4.85 5.22
-6 2 0 8.29 3.17
5 -2 0 14.21 6.86
-5 2 0 16.77 5.52
4 -2 0 0.63 2.19
4 -2 0 0.80 4.33
-4 2 0 3.29 2.81
3 -2 0 97.66 11.45
3 -2 0 107.11 13.16
-3 2 0 85.40 11.18
2 -2 0 11.04 3.76
2 -2 0 15.33 3.47
-2 2 0 18.73 3.45
1 -2 0 17.04 3.31
1 -2 0 13.00 2.60
-1 2 0 15.92 2.90
0 -2 0 160.05 14.63
0 -2 0 163.48 14.91
0 -2 0 161.22 14.32
0 2 0 176.85 15.00
0 2 0 151.15 14.34
-1 -2 0 18.37 2.28
-1 -2 0 15.03 3.24
1 2 0 18.39 3.38
1 2 0 15.15 2.29
-2 -2 0 15.26 2.65
2 2 0 11.78 2.67
-3 -2 0 91.66 10.36
3 2 0 92.39 10.47
-4 -2 0 -0.45 1.71
4 2 0 0.00 2.36
-5 -2 0 12.68 3.70
5 2 0 15.01 4.39
-6 -2 0 7.77 3.30
-7 -2 0 3.19 3.38
9 -3 0 -1.95 4.84
8 -3 0 1.26 5.66
7 -3 0 4.22 4.31
-7 3 0 -2.07 3.94
6 -3 0 28.68 9.18
-6 3 0 23.29 6.82
5 -3 0 8.91 4.81
-5 3 0 2.60 3.13
4 -3 0 34.54 8.97
4 -3 0 32.60 6.48
-4 3 0 20.42 5.72
3 -3 0 2.25 1.67
3 -3 0 2.45 2.41
-3 3 0 1.83 1.70
2 -3 0 38.02 7.11
2 -3 0 33.52 5.47
-2 3 0 27.85 5.43
1 -3 0 71.07 7.59
1 -3 0 63.81 7.25
-1 3 0 58.85 7.36
0 -3 0 -0.75 1.07
0 -3 0 0.27 0.76
0 -3 0 0.07 0.39
0 3 0 0.38 0.51
-1 -3 0 72.66 7.92
-1 -3 0 58.12 6.48
1 3 0 78.84 6.75
-2 -3 0 26.11 3.86
2 3 0 28.57 4.14
-3 -3 0 1.19 1.37
3 3 0 1.73 1.67
-4 -3 0 26.83 4.76
4 3 0 20.65 5.05
-5 -3 0 9.82 3.15
5 3 0 6.72 3.55
-6 -3 0 29.79 6.04
-7 -3 0 5.73 3.78
8 -4 0 -2.27 3.97
7 -4 0 -2.74 3.65
-7 4 0 4.02 5.29
6 -4 0 13.25 7.34
-6 4 0 17.83 6.40
5 -4 0 10.32 5.26
-5 4 0 17.65 5.80
4 -4 0 1.77 3.27
4 -4 0 0.77 2.86
-4 4 0 2.70 2.23
3 -4 0 29.90 7.02
3 -4 0 21.73 5.25
-3 4 0 32.61 6.26
2 -4 0 96.56 11.03
2 -4 0 100.34 11.62
-2 4 0 92.86 11.21
1 -4 0 71.35 8.30
1 -4 0 59.59 7.66
1 -4 0 83.47 7.43
-1 4 0 61.57 7.82
0 -4 0 11.31 2.67
0 -4 0 6.52 1.95
0 -4 0 9.21 1.53
0 4 0 12.74 1.88
-1 -4 0 85.89 9.03
-1 -4 0 71.47 7.22
1 4 0 76.78 7.41
-2 -4 0 110.44 12.65
-2 -4 0 98.05 10.55
2 4 0 128.39 11.25
-3 -4 0 29.06 4.34
3 4 0 27.20 4.88
-4 -4 0 3.50 2.00
4 4 0 2.07 2.55
-5 -4 0 16.02 3.95
5 4 0 3.30 3.70
-6 -4 0 18.00 4.63
8 -5 0 1.15 4.86
7 -5 0 -4.28 5.49
6 -5 0 -2.99 3.52
-6 5 0 -0.54 3.80
5 -5 0 47.42 11.71
-5 5 0 50.11 10.44
4 -5 0 6.57 3.52
4 -5 0 -0.65 2.97
-4 5 0 -1.69 2.35
3 -5 0 186.63 20.75
3 -5 0 157.53 19.00
-3 5 0 211.11 20.52
2 -5 0 378.94 35.72
2 -5 0 386.71 35.07
-2 5 0 342.00 35.09
1 -5 0 748.16 66.90
1 -5 0 707.34 65.28
1 -5 0 775.38 66.45
0 -5 0 -0.34 0.89
0 -5 0 0.60 0.50
0 -5 0 -0.95 0.86
0 5 0 0.78 0.76
-1 -5 0 750.33 66.06
-1 -5 0 724.68 63.84
-1 -5 0 721.41 63.97
-2 -5 0 327.47 33.16
-2 -5 0 355.30 30.40
2 5 0 333.72 30.84
-3 -5 0 191.60 18.13
3 5 0 193.72 19.02
-4 -5 0 3.15 1.88
4 5 0 4.75 2.41
-5 -5 0 57.89 7.24
5 5 0 39.72 8.06
-6 -5 0 -0.63 2.02
8 -6 0 8.13 7.31
7 -6 0 16.05 8.66
6 -6 0 2.45 4.28
-6 6 0 4.51 3.56
5 -6 0 112.80 18.87
-5 6 0 83.66 14.21
4 -6 0 -0.43 1.66
3 -6 0 40.29 7.23
3 -6 0 41.85 8.34
-3 6 0 34.65 7.02
2 -6 0 12.54 4.12
2 -6 0 11.37 3.04
2 -6 0 8.33 2.50
-2 6 0 18.24 4.22
1 -6 0 61.16 7.93
1 -6 0 68.99 6.51
1 -6 0 40.26 7.12
0 -6 0 6.48 1.99
0 -6 0 6.80 1.38
0 -6 0 7.45 2.56
0 6 0 4.76 1.52
-1 -6 0 63.74 8.16
-1 -6 0 61.81 5.84
-1 -6 0 51.91 5.92
1 6 0 57.32 6.03
-2 -6 0 16.69 5.16
-2 -6 0 9.74 1.56
2 6 0 10.84 2.33
-3 -6 0 45.55 4.84
3 6 0 39.60 6.02
-4 -6 0 -0.13 1.29
4 6 0 -0.28 2.38
-5 -6 0 106.90 10.55
5 6 0 73.69 12.44
8 -7 0 -6.59 4.48
7 -7 0 6.65 5.21
6 -7 0 1.92 3.02
5 -7 0 1.03 3.62
4 -7 0 -1.25 1.40
-4 7 0 -1.81 2.48
3 -7 0 -0.77 1.43
3 -7 0 1.82 1.58
3 -7 0 -2.86 2.48
-3 7 0 -3.65 1.84
2 -7 0 154.77 15.38
2 -7 0 162.46 17.55
2 -7 0 143.35 16.50
1 -7 0 29.48 5.11
1 -7 0 27.53 3.78
1 -7 0 48.17 7.53
0 -7 0 0.24 0.57
0 -7 0 -1.00 1.21
0 -7 0 -1.19 1.18
0 7 0 -1.43 0.78
-1 -7 0 32.35 3.82
-1 -7 0 28.06 6.11
-1 -7 0 31.62 3.58
1 7 0 33.80 4.05
-2 -7 0 145.24 16.89
2 7 0 142.67 13.93
3 7 0 1.43 1.47
4 7 0 0.51 2.17
8 -8 0 -5.18 3.80
7 -8 0 -1.41 5.36
6 -8 0 -0.40 3.29
5 -8 0 2.44 3.11
4 -8 0 1.80 3.33
3 -8 0 19.07 3.93
3 -8 0 22.38 6.41
3 -8 0 19.55 5.28
2 -8 0 10.36 3.91
2 -8 0 17.98 4.47
2 -8 0 16.43 3.30
1 -8 0 8.62 1.98
1 -8 0 5.89 3.32
1 -8 0 4.24 2.63
0 -8 0 41.18 5.33
0 -8 0 41.60 4.49
0 -8 0 37.97 7.70
0 8 0 33.02 5.28
-1 -8 0 4.46 1.09
-1 -8 0 3.19 1.16
-1 -8 0 8.00 3.79
1 8 0 4.16 1.60
-2 -8 0 17.98 5.16
2 8 0 14.49 2.84
-3 -8 0 19.38 5.79
3 8 0 17.32 3.58
4 8 0 4.21 2.25
7 -9 0 5.57 5.54
6 -9 0 -0.55 3.74
5 -9 0 5.11 3.51
4 -9 0 2.45 3.54
4 -9 0 0.48 2.14
3 -9 0 0.34 1.99
3 -9 0 2.01 1.39
3 -9 0 1.58 3.31
2 -9 0 27.54 4.62
2 -9 0 32.11 7.54
2 -9 0 38.05 7.03
1 -9 0 26.52 4.25
1 -9 0 42.49 6.48
1 -9 0 39.89 7.74
0 -9 0 2.16 1.87
0 -9 0 -0.14 1.24
0 9 0 4.52 2.00
-1 -9 0 34.21 7.64
1 9 0 27.59 4.50
-2 -9 0 19.78 6.17
2 9 0 24.88 4.00
-3 -9 0 0.47 2.75
3 9 0 0.51 1.59
4 9 0 -0.64 2.18
7 -10 0 -1.89 6.45
6 -10 0 43.06 8.71
6 -10 0 37.84 11.22
5 -10 0 2.63 3.23
5 -10 0 -2.04 2.32
4 -10 0 6.12 2.88
4 -10 0 9.35 4.41
3 -10 0 -7.58 3.80
3 -10 0 1.83 2.14
3 -10 0 -1.33 1.37
2 -10 0 85.29 12.30
2 -10 0 91.03 9.77
2 -10 0 87.32 12.51
1 -10 0 45.27 9.15
1 -10 0 34.84 6.42
1 -10 0 43.44 4.98
0 -10 0 55.36 6.49
0 -10 0 50.24 5.48
0 -10 0 44.76 9.00
0 10 0 40.56 6.70
-1 -10 0 39.41 9.11
1 10 0 36.37 5.64
-2 -10 0 74.21 13.33
2 10 0 68.76 8.07
-3 -10 0 -0.06 2.81
3 10 0 2.85 1.78
4 10 0 12.50 3.37
6 -11 0 5.77 5.39
6 -11 0 3.46 3.50
5 -11 0 -0.57 2.98
5 -11 0 1.29 2.66
4 -11 0 188.64 23.57
4 -11 0 189.36 20.05
3 -11 0 12.85 6.12
3 -11 0 13.58 3.06
2 -11 0 518.91 43.34
2 -11 0 426.76 44.79
2 -11 0 460.74 47.06
1 -11 0 3.83 1.31
1 -11 0 2.10 2.70
1 -11 0 -5.44 2.45
0 -11 0 3.95 1.36
0 -11 0 -0.13 1.96
0 -11 0 4.76 4.66
0 11 0 5.17 2.66
-1 -11 0 1.17 2.26
1 11 0 -1.30 1.87
-2 -11 0 423.22 44.84
2 11 0 445.99 40.28
-3 -11 0 24.89 7.99
3 11 0 21.90 4.04
6 -12 0 3.22 5.37
6 -12 0 3.45 4.25
5 -12 0 0.78 3.78
5 -12 0 -0.73 2.99
4 -12 0 4.70 3.09
4 -12 0 -1.11 1.94
3 -12 0 14.57 6.28
3 -12 0 23.56 4.49
2 -12 0 113.11 14.93
2 -12 0 135.10 17.39
2 -12 0 138.98 13.48
1 -12 0 -2.00 2.00
1 -12 0 -1.56 0.87
1 -12 0 -7.52 2.14
0 -12 0 4.20 1.76
0 -12 0 7.29 4.27
0 -12 0 8.23 1.61
-1 -12 0 -0.43 3.32
-2 -12 0 128.15 17.59
-3 -12 0 11.98 7.13
5 -13 0 -2.33 3.05
5 -13 0 -0.31 3.58
4 -13 0 -9.03 3.43
4 -13 0 -4.29 1.93
3 -13 0 2.46 1.77
3 -13 0 -0.93 3.10
2 -13 0 20.59 5.16
2 -13 0 7.95 4.35
2 -13 0 9.84 2.68
1 -13 0 4.56 3.20
1 -13 0 1.76 3.61
1 -13 0 2.10 1.30
0 -13 0 -0.34 3.25
-1 -13 0 -2.13 2.21
-2 -13 0 9.26 4.53
-3 -13 0 3.28 3.87
5 -14 0 0.27 4.17
5 -14 0 3.29 3.85
4 -14 0 -2.65 2.34
4 -14 0 5.32 4.53
3 -14 0 6.91 3.53
3 -14 0 4.17 1.95
2 -14 0 -13.15 4.31
2 -14 0 -1.46 3.42
2 -14 0 -0.22 1.70
1 -14 0 9.74 2.06
1 -14 0 8.19 3.35
1 -14 0 7.32 4.09
0 -14 0 9.82 4.98
-1 -14 0 9.33 4.78
-2 -14 0 3.54 4.50
-3 -14 0 7.50 6.11
4 -15 0 0.29 3.95
4 -15 0 -0.57 2.17
3 -15 0 2.29 3.93
3 -15 0 -0.03 2.08
2 -15 0 -0.75 2.00
2 -15 0 -16.32 4.93
2 -15 0 -3.73 2.74
1 -15 0 -0.79 4.10
0 -15 0 1.16 3.18
-1 -15 0 2.92 4.98
-2 -15 0 1.36 3.57
-3 -15 0 1.26 3.00
2 -16 0 4.80 2.45
2 -16 0 7.20 5.49
1 -16 0 4.61 3.88
0 -16 0 6.44 3.71
-1 -16 0 -2.59 2.95
-2 -16 0 -3.53 3.79
-2 -16 1 4.22 4.33
-1 -16 1 3.35 3.89
0 -16 1 -1.23 3.48
1 -16 1 10.35 4.60
2 -16 1 4.34 4.35
2 -16 1 7.03 2.29
-3 -15 1 4.53 5.06
-2 -15 1 4.59 4.55
-1 -15 1 0.87 4.08
0 -15 1 0.33 2.39
1 -15 1 0.06 3.42
2 -15 1 4.02 4.24
2 -15 1 7.25 4.62
3 -15 1 5.50 3.71
3 -15 1 10.28 3.07
4 -15 1 -4.04 2.86
4 -15 1 -3.69 2.47
-3 -14 1 -2.35 2.82
-2 -14 1 2.74 3.78
-1 -14 1 -0.55 3.50
0 -14 1 -0.11 2.17
1 -14 1 -1.27 1.19
1 -14 1 0.18 3.31
1 -14 1 -2.87 1.72
2 -14 1 4.12 4.95
2 -14 1 0.15 1.31
2 -14 1 -3.74 3.72
3 -14 1 0.65 2.66
3 -14 1 -2.93 1.72
4 -14 1 1.62 2.70
4 -14 1 -1.26 2.22
5 -14 1 4.10 5.52
5 -14 1 -0.05 2.73
-3 -13 1 4.53 4.48
-2 -13 1 0.91 2.66
-1 -13 1 12.73 5.65
0 -13 1 0.52 2.27
1 -13 1 20.00 3.07
1 -13 1 21.57 6.94
1 -13 1 17.00 3.93
2 -13 1 6.37 4.02
2 -13 1 1.32 2.68
2 -13 1 0.44 1.46
3 -13 1 3.96 3.86
3 -13 1 1.82 1.78
4 -13 1 -0.18 2.10
4 -13 1 -2.54 3.62
5 -13 1 1.28 2.84
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-2 -6 -29 6.35 5.20
-3 -6 -29 -3.86 4.43
2 -7 -29 1.33 3.87
1 -7 -29 0.64 3.89
0 -7 -29 11.12 4.60
-1 -7 -29 7.16 5.38
-2 -7 -29 5.21 4.56
1 -8 -29 10.35 4.42
0 -8 -29 1.60 4.32
-1 -8 -29 10.10 4.88
1 7 -30 -2.82 4.01
0 7 -30 4.24 5.33
-1 7 -30 1.20 5.00
1 -7 30 -7.08 4.70
2 6 -30 -0.67 3.81
1 6 -30 -1.98 3.39
0 6 -30 4.82 4.69
-1 6 -30 6.47 4.90
1 -6 30 2.54 4.38
-2 6 -30 4.27 5.50
2 -6 30 -4.14 6.33
2 5 -30 1.29 3.15
1 5 -30 1.37 3.53
0 5 -30 -1.33 3.79
-1 5 -30 -5.35 4.30
1 -5 30 5.31 4.68
-2 5 -30 -5.83 4.83
2 -5 30 -0.40 6.62
-3 5 -30 -0.23 6.16
3 4 -30 0.67 2.68
2 4 -30 1.31 2.97
1 4 -30 0.44 3.52
0 4 -30 -1.13 3.18
0 -4 30 1.60 3.76
-1 4 -30 -11.19 3.32
1 -4 30 -4.68 5.52
-2 4 -30 -7.79 4.49
2 -4 30 -1.63 6.41
-3 4 -30 -5.41 4.37
3 -4 30 -13.09 6.26
3 3 -30 4.13 2.80
2 3 -30 1.29 2.96
1 3 -30 0.63 2.92
0 3 -30 -6.27 3.40
0 -3 30 -12.89 3.92
-1 3 -30 1.92 4.37
1 -3 30 4.49 6.27
-2 3 -30 6.58 5.65
-3 3 -30 -4.88 5.58
3 -3 30 0.95 6.81
3 2 -30 -2.26 2.78
2 2 -30 2.39 3.30
1 2 -30 -1.91 2.82
0 2 -30 -5.97 2.64
0 -2 30 -9.86 5.15
-1 2 -30 4.22 3.72
1 -2 30 -4.83 3.67
-2 2 -30 -8.99 4.55
-3 2 -30 6.58 5.53
3 1 -30 -1.07 2.35
2 1 -30 -1.33 2.50
1 1 -30 2.20 3.21
0 1 -30 -3.59 3.40
-1 1 -30 -2.19 3.17
-2 1 -30 4.45 3.52
-3 1 -30 -11.79 4.36
-4 1 -30 5.41 5.88
3 0 -30 -2.56 2.94
2 0 -30 0.00 2.91
1 0 -30 -0.57 2.70
0 0 -30 1.99 3.98
-1 0 -30 1.02 3.22
-2 0 -30 3.95 3.77
-3 0 -30 11.80 6.05
-4 0 -30 0.21 4.93
3 -1 -30 0.54 3.17
2 -1 -30 0.15 2.05
1 -1 -30 0.28 3.04
0 -1 -30 3.70 3.41
-1 -1 -30 6.01 4.09
-2 -1 -30 7.32 4.48
-3 -1 -30 10.11 6.04
-4 -1 -30 -1.12 5.89
3 -2 -30 0.30 2.70
2 -2 -30 2.51 3.09
1 -2 -30 -2.30 3.41
0 -2 -30 4.96 3.59
-1 -2 -30 -8.67 3.63
-2 -2 -30 -1.17 2.96
-3 -2 -30 5.12 6.29
3 -3 -30 5.83 3.45
2 -3 -30 2.53 2.74
1 -3 -30 1.61 3.13
0 -3 -30 -9.04 3.10
-1 -3 -30 0.95 3.63
-2 -3 -30 0.21 4.79
-3 -3 -30 0.06 5.50
3 -4 -30 2.62 3.15
2 -4 -30 4.35 3.51
1 -4 -30 -1.01 2.90
0 -4 -30 -2.79 3.18
-1 -4 -30 -3.66 3.77
-2 -4 -30 3.36 3.19
-3 -4 -30 -4.26 5.30
2 -5 -30 -0.60 3.01
1 -5 -30 -2.38 2.86
0 -5 -30 -0.46 4.10
-1 -5 -30 9.28 3.41
-2 -5 -30 3.62 4.34
2 -6 -30 2.08 3.51
1 -6 -30 1.56 3.58
-1 -6 -30 5.54 3.45
-2 -6 -30 4.66 5.33
1 -7 -30 4.59 3.49
0 -7 -30 5.38 4.06
-1 -7 -30 3.93 4.43
0 6 -31 11.49 5.25
-1 6 -31 -0.50 5.10
1 5 -31 1.17 3.80
0 5 -31 -7.52 3.46
-1 5 -31 -2.09 4.93
1 -5 31 6.19 5.77
-2 5 -31 2.31 5.22
2 4 -31 11.40 4.44
1 4 -31 0.13 3.76
0 4 -31 -2.14 3.61
-1 4 -31 -9.02 3.47
1 -4 31 -0.12 6.27
-2 4 -31 -4.89 4.72
2 -4 31 -9.05 8.01
2 3 -31 3.89 3.07
1 3 -31 9.09 3.90
0 3 -31 -0.47 2.99
0 -3 31 -6.81 4.49
-1 3 -31 3.28 4.21
1 -3 31 -0.97 6.38
-2 3 -31 -1.38 4.88
2 -3 31 -2.86 7.96
-3 3 -31 3.89 6.73
3 2 -31 0.64 3.40
2 2 -31 -4.40 3.07
1 2 -31 -5.39 2.64
0 2 -31 1.08 3.55
0 -2 31 -4.40 5.58
-1 2 -31 -9.90 3.18
-2 2 -31 -1.30 4.93
-3 2 -31 -1.16 5.46
3 1 -31 1.05 3.50
2 1 -31 6.34 3.30
1 1 -31 1.17 2.79
0 1 -31 1.51 3.90
-1 1 -31 -2.45 3.15
-2 1 -31 6.14 5.34
-3 1 -31 -10.31 4.38
3 0 -31 -4.77 2.58
2 0 -31 3.57 2.91
1 0 -31 1.47 3.32
0 0 -31 0.73 3.49
-1 0 -31 -0.92 4.10
-2 0 -31 -8.23 2.87
-3 0 -31 3.84 5.51
3 -1 -31 -3.12 2.96
2 -1 -31 -0.05 3.30
1 -1 -31 -4.14 3.38
0 -1 -31 0.41 3.60
-1 -1 -31 -2.70 2.89
-2 -1 -31 -0.64 4.44
-3 -1 -31 3.89 6.54
3 -2 -31 -3.81 2.73
2 -2 -31 -3.13 2.65
1 -2 -31 -3.66 3.07
0 -2 -31 3.05 3.20
-1 -2 -31 -3.24 2.91
-2 -2 -31 1.31 3.97
-3 -2 -31 -7.44 4.71
2 -3 -31 0.23 2.85
1 -3 -31 3.97 3.96
0 -3 -31 2.98 3.44
-1 -3 -31 -5.55 3.51
-2 -3 -31 -7.43 4.34
2 -4 -31 7.87 4.66
1 -4 -31 -2.10 2.88
0 -4 -31 16.13 5.92
-1 -4 -31 -0.74 3.98
-2 -4 -31 5.27 5.08
1 -5 -31 -0.11 3.03
0 -5 -31 -0.28 4.22
-1 -5 -31 8.62 5.24
0 -6 -31 11.75 4.70
1 4 -32 -5.48 4.15
0 4 -32 9.66 4.99
-1 4 -32 3.90 4.99
1 -4 32 4.98 7.16
1 3 -32 3.06 4.85
0 3 -32 4.21 3.93
-1 3 -32 5.06 4.27
1 -3 32 -9.48 6.75
-2 3 -32 5.99 6.13
2 2 -32 -2.33 3.89
1 2 -32 -3.55 3.43
0 2 -32 -3.17 4.00
0 -2 32 -7.62 6.29
-1 2 -32 -1.64 4.25
1 -2 32 5.11 6.97
-2 2 -32 -0.20 4.77
2 1 -32 -9.72 2.79
1 1 -32 -0.68 3.79
0 1 -32 -3.58 3.94
-1 1 -32 10.75 4.45
-2 1 -32 4.93 5.89
2 0 -32 -0.18 3.71
1 0 -32 0.16 3.90
0 0 -32 -5.47 2.89
-1 0 -32 5.76 4.28
-2 0 -32 0.54 3.47
2 -1 -32 0.14 2.85
1 -1 -32 4.75 3.74
0 -1 -32 -0.42 4.30
-1 -1 -32 -2.65 4.29
-2 -1 -32 1.15 4.24
2 -2 -32 -2.70 3.35
1 -2 -32 2.64 3.17
0 -2 -32 -6.67 3.19
-1 -2 -32 8.11 4.29
-2 -2 -32 -4.36 4.47
1 -3 -32 6.82 4.39
0 -3 -32 -0.86 3.22
-1 -3 -32 2.01 4.66
-2 -3 -32 4.18 5.16
1 -4 -32 -2.80 3.54
0 -4 -32 0.59 4.41
-1 -4 -32 0.01 4.80
0 2 -33 -5.69 3.98
1 1 -33 -7.19 3.62
0 1 -33 -1.66 4.03
0 -1 33 -18.41 7.57
-1 1 -33 1.82 4.18
1 0 -33 -10.65 3.67
0 0 -33 2.99 3.93
-1 0 -33 -1.63 4.64
1 -1 -33 8.47 4.50
0 -1 -33 -1.45 4.79
-1 -1 -33 4.88 4.42
0 -2 -33 3.77 3.41
0 0 0 0.00 0.00
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7455
_exptl_absorpt_correction_T_min 0.5745
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71073 7.188 13.050 26.022 90.033 89.848 89.911
)
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 90271
_shelx_res_file
;
TITL k_a_a.res in P2(1)2(1)2(1)
k_a.res
created by SHELXL-2019/3 at 12:24:07 on 29-Jul-2025
REM Old TITL K_a.res in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1): R1 0.192, Rweak 0.024, Alpha 0.004
REM 0.914 for 26 systematic absences, Orientation as input
REM Flack x = -0.121 ( 1.414 ) from 775 Parsons' quotients
REM Formula found by SHELXT: C28 F N3 O4
CELL 0.71073 7.1788 13.0274 25.9791 90 90 90
ZERR 40 0.001 0.0013 0.0029 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H F N O
UNIT 104 112 4 12 24
L.S. 5
PLAN 1
TEMP 0
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.052600
EXTI 0.007483
FVAR 0.40773
F1 3 0.384590 0.425393 0.486009 11.00000 0.12430 0.05512 =
0.07236 -0.02096 0.02048 -0.00895
O4 5 0.440858 0.627879 0.635987 11.00000 0.09848 0.04529 =
0.05256 -0.00137 -0.00725 0.00193
O3 5 0.405509 0.785963 0.418642 11.00000 0.07942 0.07933 =
0.04821 0.00364 0.00316 -0.00113
N1 4 0.433080 0.804932 0.575367 11.00000 0.05984 0.04355 =
0.04868 -0.00108 -0.00414 -0.00025
O5 5 0.504948 0.197337 0.691627 11.00000 0.09612 0.04973 =
0.09698 -0.00439 -0.02522 0.01511
O2 5 0.410648 0.979427 0.414991 11.00000 0.10216 0.07703 =
0.06591 0.01972 -0.00637 -0.01477
AFIX 147
H2 2 0.412608 0.918689 0.406726 11.00000 -1.50000
AFIX 0
O6 5 0.505104 0.048830 0.650684 11.00000 0.11866 0.05676 =
0.12657 -0.01853 -0.06465 0.01175
N3 4 0.267737 0.239300 0.618491 11.00000 0.06773 0.04384 =
0.06608 -0.00079 -0.01102 0.00058
AFIX 13
H3 2 0.351504 0.221625 0.646927 11.00000 -1.20000
AFIX 0
N2 4 0.416179 0.435040 0.592144 11.00000 0.09722 0.04184 =
0.07359 0.00470 0.03142 0.01348
O1 5 0.422419 1.069556 0.486475 11.00000 0.13773 0.05155 =
0.08342 0.00939 -0.00590 0.00020
C3 1 0.414996 0.792221 0.467298 11.00000 0.03881 0.06451 =
0.05530 0.00260 -0.00062 0.00070
C2 1 0.421647 0.887335 0.493511 11.00000 0.04397 0.04906 =
0.05996 0.00409 -0.00260 0.00115
C4 1 0.417032 0.700531 0.499112 11.00000 0.04051 0.04976 =
0.05423 -0.00231 0.00124 -0.00020
C7 1 0.416147 0.522840 0.561792 11.00000 0.05775 0.04108 =
0.06009 -0.00017 0.00783 0.00393
C9 1 0.422531 0.708496 0.552831 11.00000 0.04960 0.04273 =
0.04829 -0.00210 -0.00173 0.00211
C8 1 0.427562 0.620401 0.583830 11.00000 0.05568 0.04834 =
0.04742 -0.00083 0.00260 0.00561
C10 1 0.432682 0.889460 0.546186 11.00000 0.05241 0.04641 =
0.06504 0.00199 -0.00840 0.00270
AFIX 43
H10 2 0.440276 0.952924 0.562442 11.00000 -1.20000
AFIX 0
C11 1 0.430830 0.813683 0.631855 11.00000 0.07419 0.04772 =
0.04540 -0.00636 -0.00498 -0.00299
AFIX 13
H11 2 0.502388 0.874645 0.641728 11.00000 -1.20000
AFIX 0
C6 1 0.404652 0.519748 0.508176 11.00000 0.06503 0.04853 =
0.05964 -0.01439 0.00769 -0.00082
C16 1 0.170522 0.336449 0.632118 11.00000 0.06421 0.04860 =
0.06602 0.00081 -0.00149 0.00956
AFIX 23
H16A 2 0.101626 0.326800 0.663871 11.00000 -1.20000
H16B 2 0.082101 0.353582 0.605224 11.00000 -1.20000
AFIX 0
C22 1 0.736742 0.076759 0.713115 11.00000 0.06407 0.04745 =
0.05807 -0.00010 -0.01144 0.00082
C5 1 0.408342 0.602915 0.477220 11.00000 0.06022 0.05918 =
0.05269 -0.00764 0.00304 0.00186
AFIX 43
H5 2 0.405122 0.595200 0.441643 11.00000 -1.20000
AFIX 0
C1 1 0.418113 0.987128 0.465747 11.00000 0.06641 0.06276 =
0.06616 0.01482 -0.00560 -0.00236
C25 1 1.064893 0.014645 0.764328 11.00000 0.05917 0.06989 =
0.05360 -0.00350 -0.00742 0.00317
C23 1 0.790587 -0.025730 0.715709 11.00000 0.08206 0.04781 =
0.08022 -0.00742 -0.02881 0.00025
AFIX 43
H23 2 0.717649 -0.075398 0.699742 11.00000 -1.20000
AFIX 0
C21 1 0.568509 0.108564 0.682927 11.00000 0.07943 0.05112 =
0.07286 0.00020 -0.01234 -0.00808
C17 1 0.306787 0.424007 0.638708 11.00000 0.08388 0.04733 =
0.05724 0.00066 0.00391 0.00506
AFIX 23
H17A 2 0.239637 0.487146 0.645588 11.00000 -1.20000
H17B 2 0.388308 0.410274 0.667678 11.00000 -1.20000
AFIX 0
C13 1 0.526664 0.720332 0.653384 11.00000 0.08745 0.05398 =
0.05013 0.00252 -0.01242 -0.00114
AFIX 23
H13A 2 0.656407 0.720735 0.642957 11.00000 -1.20000
H13B 2 0.522493 0.722761 0.690684 11.00000 -1.20000
AFIX 0
C24 1 0.950227 -0.055257 0.741523 11.00000 0.07816 0.05460 =
0.06432 -0.00442 -0.00154 0.00622
AFIX 43
H24 2 0.980162 -0.124614 0.743378 11.00000 -1.20000
AFIX 0
C15 1 0.382802 0.253375 0.571390 11.00000 0.09267 0.05173 =
0.07598 -0.00769 0.00953 0.00877
AFIX 23
H15A 2 0.302064 0.266210 0.542151 11.00000 -1.20000
H15B 2 0.452586 0.191077 0.564583 11.00000 -1.20000
AFIX 0
C27 1 0.848363 0.146791 0.737583 11.00000 0.08959 0.05069 =
0.08313 -0.01032 -0.01802 0.00226
AFIX 43
H27 2 0.815831 0.215889 0.737288 11.00000 -1.20000
AFIX 0
C26 1 1.009264 0.115906 0.762785 11.00000 0.09126 0.06252 =
0.10154 -0.01544 -0.02894 -0.00365
AFIX 43
H26 2 1.081991 0.165116 0.779177 11.00000 -1.20000
AFIX 0
C14 1 0.515431 0.341685 0.577812 11.00000 0.09062 0.04510 =
0.09221 -0.00233 0.02514 0.01048
AFIX 23
H14A 2 0.606069 0.325097 0.604224 11.00000 -1.20000
H14B 2 0.581967 0.352980 0.545812 11.00000 -1.20000
AFIX 0
C12 1 0.233378 0.826410 0.650786 11.00000 0.09955 0.08060 =
0.05981 -0.00446 0.01116 0.01439
AFIX 137
H12A 2 0.178361 0.885510 0.634783 11.00000 -1.50000
H12B 2 0.233870 0.835415 0.687461 11.00000 -1.50000
H12C 2 0.162330 0.766401 0.642152 11.00000 -1.50000
AFIX 0
C28 1 1.243443 -0.017597 0.789433 11.00000 0.06886 0.09695 =
0.08322 -0.01093 -0.01932 0.00938
AFIX 137
H28A 2 1.255020 -0.090935 0.787757 11.00000 -1.50000
H28B 2 1.243211 0.003861 0.824784 11.00000 -1.50000
H28C 2 1.346502 0.013623 0.771844 11.00000 -1.50000
AFIX 0
C18 1 0.133164 0.154054 0.612120 11.00000 0.08865 0.06251 =
0.10782 -0.01011 -0.01930 -0.01506
AFIX 137
H18A 2 0.071686 0.141200 0.644297 11.00000 -1.50000
H18B 2 0.198158 0.093334 0.601357 11.00000 -1.50000
H18C 2 0.042429 0.172378 0.586578 11.00000 -1.50000
AFIX 0
HKLF 4
REM k_a_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1767, GooF = S = 1.000, Restrained GooF = 1.000 for all data
REM R1 = 0.0601 for 2456 Fo > 4sig(Fo) and 0.1617 for all 5409 data
REM 330 parameters refined using 0 restraints
END
WGHT 0.0523 0.0000
REM Highest difference peak 0.228, deepest hole -0.173, 1-sigma level 0.047
Q1 1 0.4218 0.7022 0.5293 11.00000 0.05 0.23
;
_shelx_res_checksum 54685
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'
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
F F1 0.3846(6) 0.4254(2) 0.48601(11) 0.0839(13) Uani d 1 . .
O O4 0.4409(7) 0.6279(2) 0.63599(12) 0.0654(13) Uani d 1 . .
O O3 0.4055(6) 0.7860(3) 0.41864(13) 0.0690(12) Uani d 1 . .
N N1 0.4331(7) 0.8049(3) 0.57537(14) 0.0507(12) Uani d 1 . .
O O5 0.5049(7) 0.1973(2) 0.69163(16) 0.0809(14) Uani d 1 . .
O O2 0.4106(8) 0.9794(3) 0.41499(15) 0.0817(14) Uani d 1 . .
H H2 0.412608 0.918689 0.406726 0.123 Uiso calc 1 . .
O O6 0.5051(8) 0.0488(3) 0.65068(18) 0.1007(18) Uani d 1 . .
N N3 0.2677(7) 0.2393(3) 0.61849(16) 0.0592(14) Uani d 1 . .
H H3 0.351504 0.221625 0.646927 0.071 Uiso calc 1 . .
N N2 0.4162(8) 0.4350(3) 0.59214(17) 0.0709(16) Uani d 1 . .
O O1 0.4224(8) 1.0696(3) 0.48648(15) 0.0909(17) Uani d 1 . .
C C3 0.4150(8) 0.7922(4) 0.46730(19) 0.0529(14) Uani d 1 . .
C C2 0.4216(8) 0.8873(3) 0.49351(19) 0.0510(14) Uani d 1 . .
C C4 0.4170(8) 0.7005(3) 0.49911(19) 0.0482(13) Uani d 1 . .
C C7 0.4161(9) 0.5228(3) 0.5618(2) 0.0530(15) Uani d 1 . .
C C9 0.4225(8) 0.7085(3) 0.55283(17) 0.0469(13) Uani d 1 . .
C C8 0.4276(8) 0.6204(3) 0.58383(17) 0.0505(14) Uani d 1 . .
C C10 0.4327(8) 0.8895(4) 0.54619(19) 0.0546(15) Uani d 1 . .
H H10 0.440276 0.952924 0.562442 0.066 Uiso calc 1 . .
C C11 0.4308(10) 0.8137(3) 0.63186(17) 0.0558(16) Uani d 1 . .
H H11 0.502388 0.874645 0.641728 0.067 Uiso calc 1 . .
C C6 0.4047(9) 0.5197(4) 0.5082(2) 0.0577(16) Uani d 1 . .
C C16 0.1705(9) 0.3364(3) 0.6321(2) 0.0596(16) Uani d 1 . .
H H16A 0.101626 0.326800 0.663871 0.072 Uiso calc 1 . .
H H16B 0.082101 0.353582 0.605224 0.072 Uiso calc 1 . .
C C22 0.7367(9) 0.0768(4) 0.71312(19) 0.0565(16) Uani d 1 . .
C C5 0.4083(9) 0.6029(4) 0.4772(2) 0.0574(16) Uani d 1 . .
H H5 0.405122 0.595200 0.441643 0.069 Uiso calc 1 . .
C C1 0.4181(10) 0.9871(4) 0.4657(2) 0.0651(18) Uani d 1 . .
C C25 1.0649(9) 0.0146(4) 0.7643(2) 0.0609(16) Uani d 1 . .
C C23 0.7906(10) -0.0257(4) 0.7157(2) 0.0700(19) Uani d 1 . .
H H23 0.717649 -0.075398 0.699742 0.084 Uiso calc 1 . .
C C21 0.5685(10) 0.1086(4) 0.6829(2) 0.0678(18) Uani d 1 . .
C C17 0.3068(10) 0.4240(4) 0.63871(19) 0.0628(17) Uani d 1 . .
H H17A 0.239637 0.487146 0.645588 0.075 Uiso calc 1 . .
H H17B 0.388308 0.410274 0.667678 0.075 Uiso calc 1 . .
C C13 0.5267(10) 0.7203(3) 0.65338(19) 0.0639(17) Uani d 1 . .
H H13A 0.656407 0.720735 0.642957 0.077 Uiso calc 1 . .
H H13B 0.522493 0.722761 0.690684 0.077 Uiso calc 1 . .
C C24 0.9502(10) -0.0553(4) 0.7415(2) 0.0657(18) Uani d 1 . .
H H24 0.980162 -0.124614 0.743378 0.079 Uiso calc 1 . .
C C15 0.3828(10) 0.2534(4) 0.5714(2) 0.073(2) Uani d 1 . .
H H15A 0.302064 0.266210 0.542151 0.088 Uiso calc 1 . .
H H15B 0.452586 0.191077 0.564583 0.088 Uiso calc 1 . .
C C27 0.8484(11) 0.1468(4) 0.7376(2) 0.074(2) Uani d 1 . .
H H27 0.815831 0.215889 0.737288 0.089 Uiso calc 1 . .
C C26 1.0093(12) 0.1159(4) 0.7628(2) 0.085(2) Uani d 1 . .
H H26 1.081991 0.165116 0.779177 0.102 Uiso calc 1 . .
C C14 0.5154(10) 0.3417(4) 0.5778(2) 0.076(2) Uani d 1 . .
H H14A 0.606069 0.325097 0.604224 0.091 Uiso calc 1 . .
H H14B 0.581967 0.352980 0.545812 0.091 Uiso calc 1 . .
C C12 0.2334(11) 0.8264(4) 0.6508(2) 0.080(2) Uani d 1 . .
H H12A 0.178361 0.885510 0.634783 0.120 Uiso calc 1 . .
H H12B 0.233870 0.835415 0.687461 0.120 Uiso calc 1 . .
H H12C 0.162330 0.766401 0.642152 0.120 Uiso calc 1 . .
C C28 1.2434(10) -0.0176(5) 0.7894(2) 0.083(2) Uani d 1 . .
H H28A 1.255020 -0.090935 0.787757 0.125 Uiso calc 1 . .
H H28B 1.243211 0.003861 0.824784 0.125 Uiso calc 1 . .
H H28C 1.346502 0.013623 0.771844 0.125 Uiso calc 1 . .
C C18 0.1332(11) 0.1541(4) 0.6121(3) 0.086(2) Uani d 1 . .
H H18A 0.071686 0.141200 0.644297 0.129 Uiso calc 1 . .
H H18B 0.198158 0.093334 0.601357 0.129 Uiso calc 1 . .
H H18C 0.042429 0.172378 0.586578 0.129 Uiso calc 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
F1 0.124(4) 0.0551(17) 0.072(2) -0.009(2) 0.020(2) -0.0210(15)
O4 0.098(4) 0.0453(17) 0.053(2) 0.002(2) -0.007(2) -0.0014(15)
O3 0.079(3) 0.079(2) 0.048(2) -0.001(3) 0.003(2) 0.0036(18)
N1 0.060(4) 0.044(2) 0.049(2) 0.000(2) -0.004(2) -0.0011(17)
O5 0.096(4) 0.050(2) 0.097(3) 0.015(2) -0.025(3) -0.0044(19)
O2 0.102(4) 0.077(2) 0.066(3) -0.015(3) -0.006(3) 0.020(2)
O6 0.119(5) 0.057(2) 0.127(4) 0.012(2) -0.065(4) -0.019(2)
N3 0.068(4) 0.044(2) 0.066(3) 0.001(2) -0.011(3) -0.0008(19)
N2 0.097(5) 0.042(2) 0.074(3) 0.013(3) 0.031(3) 0.005(2)
O1 0.138(5) 0.052(2) 0.083(3) 0.000(3) -0.006(3) 0.009(2)
C3 0.039(4) 0.065(3) 0.055(3) 0.001(3) -0.001(3) 0.003(2)
C2 0.044(4) 0.049(3) 0.060(3) 0.001(3) -0.003(3) 0.004(2)
C4 0.041(4) 0.050(3) 0.054(3) 0.000(3) 0.001(3) -0.002(2)
C7 0.058(4) 0.041(2) 0.060(3) 0.004(3) 0.008(3) 0.000(2)
C9 0.050(4) 0.043(2) 0.048(3) 0.002(3) -0.002(3) -0.002(2)
C8 0.056(4) 0.048(2) 0.047(3) 0.006(3) 0.003(3) -0.001(2)
C10 0.052(4) 0.046(3) 0.065(3) 0.003(3) -0.008(3) 0.002(2)
C11 0.074(5) 0.048(3) 0.045(3) -0.003(3) -0.005(3) -0.006(2)
C6 0.065(5) 0.049(3) 0.060(4) -0.001(3) 0.008(3) -0.014(3)
C16 0.064(5) 0.049(3) 0.066(3) 0.010(3) -0.001(3) 0.001(3)
C22 0.064(5) 0.047(3) 0.058(3) 0.001(3) -0.011(3) 0.000(2)
C5 0.060(5) 0.059(3) 0.053(3) 0.002(3) 0.003(3) -0.008(2)
C1 0.066(5) 0.063(3) 0.066(4) -0.002(4) -0.006(4) 0.015(3)
C25 0.059(5) 0.070(3) 0.054(3) 0.003(3) -0.007(3) -0.004(3)
C23 0.082(6) 0.048(3) 0.080(4) 0.000(3) -0.029(4) -0.007(3)
C21 0.079(6) 0.051(3) 0.073(4) -0.008(4) -0.012(4) 0.000(3)
C17 0.084(5) 0.047(3) 0.057(3) 0.005(3) 0.004(3) 0.001(3)
C13 0.087(5) 0.054(3) 0.050(3) -0.001(3) -0.012(3) 0.003(2)
C24 0.078(6) 0.055(3) 0.064(3) 0.006(3) -0.002(4) -0.004(3)
C15 0.093(6) 0.052(3) 0.076(4) 0.009(3) 0.010(4) -0.008(3)
C27 0.090(6) 0.051(3) 0.083(4) 0.002(4) -0.018(4) -0.010(3)
C26 0.091(6) 0.063(3) 0.102(5) -0.004(4) -0.029(5) -0.015(3)
C14 0.091(6) 0.045(3) 0.092(4) 0.010(3) 0.025(4) -0.002(3)
C12 0.100(7) 0.081(4) 0.060(4) 0.014(4) 0.011(4) -0.004(3)
C28 0.069(6) 0.097(4) 0.083(4) 0.009(4) -0.019(4) -0.011(3)
C18 0.089(6) 0.063(3) 0.108(5) -0.015(4) -0.019(4) -0.010(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'
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'
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
C8 O4 C13 . . 114.0(4)
C9 N1 C11 . . 119.3(4)
C10 N1 C9 . . 120.4(4)
C10 N1 C11 . . 120.1(4)
C1 O2 H2 . . 109.5
C16 N3 H3 . . 108.0
C15 N3 H3 . . 108.0
C15 N3 C16 . . 110.6(4)
C18 N3 H3 . . 108.0
C18 N3 C16 . . 111.0(5)
C18 N3 C15 . . 111.3(4)
C7 N2 C17 . . 123.7(4)
C7 N2 C14 . . 122.8(4)
C17 N2 C14 . . 113.3(4)
O3 C3 C2 . . 122.5(4)
O3 C3 C4 . . 121.0(4)
C2 C3 C4 . . 116.5(4)
C3 C2 C1 . . 122.1(5)
C10 C2 C3 . . 120.0(4)
C10 C2 C1 . . 117.9(4)
C9 C4 C3 . . 120.4(4)
C5 C4 C3 . . 121.2(5)
C5 C4 C9 . . 118.4(4)
N2 C7 C8 . . 121.1(4)
N2 C7 C6 . . 122.9(4)
C6 C7 C8 . . 116.0(4)
N1 C9 C4 . . 119.3(4)
N1 C9 C8 . . 119.8(4)
C4 C9 C8 . . 120.8(4)
O4 C8 C7 . . 118.5(4)
O4 C8 C9 . . 121.0(4)
C7 C8 C9 . . 120.5(4)
N1 C10 C2 . . 123.3(4)
N1 C10 H10 . . 118.3
C2 C10 H10 . . 118.3
N1 C11 H11 . . 108.5
N1 C11 C13 . . 107.6(4)
N1 C11 C12 . . 110.1(5)
C13 C11 H11 . . 108.5
C13 C11 C12 . . 113.4(5)
C12 C11 H11 . . 108.5
F1 C6 C7 . . 116.9(4)
C5 C6 F1 . . 118.3(4)
C5 C6 C7 . . 124.8(4)
N3 C16 H16A . . 109.3
N3 C16 H16B . . 109.3
N3 C16 C17 . . 111.4(5)
H16A C16 H16B . . 108.0
C17 C16 H16A . . 109.3
C17 C16 H16B . . 109.3
C23 C22 C21 . . 121.0(5)
C27 C22 C23 . . 117.0(6)
C27 C22 C21 . . 122.0(5)
C4 C5 H5 . . 120.3
C6 C5 C4 . . 119.3(5)
C6 C5 H5 . . 120.3
O2 C1 C2 . . 114.7(5)
O1 C1 O2 . . 121.0(5)
O1 C1 C2 . . 124.3(5)
C24 C25 C26 . . 116.8(6)
C24 C25 C28 . . 121.2(5)
C26 C25 C28 . . 121.9(6)
C22 C23 H23 . . 119.3
C24 C23 C22 . . 121.4(5)
C24 C23 H23 . . 119.3
O5 C21 C22 . . 116.8(5)
O6 C21 O5 . . 124.5(6)
O6 C21 C22 . . 118.7(5)
N2 C17 C16 . . 109.3(4)
N2 C17 H17A . . 109.8
N2 C17 H17B . . 109.8
C16 C17 H17A . . 109.8
C16 C17 H17B . . 109.8
H17A C17 H17B . . 108.3
O4 C13 C11 . . 111.5(4)
O4 C13 H13A . . 109.3
O4 C13 H13B . . 109.3
C11 C13 H13A . . 109.3
C11 C13 H13B . . 109.3
H13A C13 H13B . . 108.0
C25 C24 C23 . . 121.7(5)
C25 C24 H24 . . 119.1
C23 C24 H24 . . 119.1
N3 C15 H15A . . 109.5
N3 C15 H15B . . 109.5
N3 C15 C14 . . 110.8(4)
H15A C15 H15B . . 108.1
C14 C15 H15A . . 109.5
C14 C15 H15B . . 109.5
C22 C27 H27 . . 119.6
C22 C27 C26 . . 120.8(5)
C26 C27 H27 . . 119.6
C25 C26 C27 . . 122.2(6)
C25 C26 H26 . . 118.9
C27 C26 H26 . . 118.9
N2 C14 C15 . . 110.9(5)
N2 C14 H14A . . 109.5
N2 C14 H14B . . 109.5
C15 C14 H14A . . 109.5
C15 C14 H14B . . 109.5
H14A C14 H14B . . 108.0
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12B . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
C25 C28 H28A . . 109.5
C25 C28 H28B . . 109.5
C25 C28 H28C . . 109.5
H28A C28 H28B . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
N3 C18 H18A . . 109.5
N3 C18 H18B . . 109.5
N3 C18 H18C . . 109.5
H18A C18 H18B . . 109.5
H18A C18 H18C . . 109.5
H18B C18 H18C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
F1 C6 . 1.365(5)
O4 C8 . 1.362(5)
O4 C13 . 1.426(6)
O3 C3 . 1.269(6)
N1 C9 . 1.388(6)
N1 C10 . 1.337(6)
N1 C11 . 1.472(6)
O5 C21 . 1.264(6)
O2 H2 . 0.8200
O2 C1 . 1.323(6)
O6 C21 . 1.231(6)
N3 H3 . 0.9800
N3 C16 . 1.488(6)
N3 C15 . 1.488(7)
N3 C18 . 1.481(7)
N2 C7 . 1.389(6)
N2 C17 . 1.449(7)
N2 C14 . 1.458(6)
O1 C1 . 1.202(6)
C3 C2 . 1.415(6)
C3 C4 . 1.453(6)
C2 C10 . 1.371(6)
C2 C1 . 1.487(7)
C4 C9 . 1.400(7)
C4 C5 . 1.394(6)
C7 C8 . 1.396(6)
C7 C6 . 1.396(7)
C9 C8 . 1.402(6)
C10 H10 . 0.9300
C11 H11 . 0.9800
C11 C13 . 1.505(7)
C11 C12 . 1.509(9)
C6 C5 . 1.350(7)
C16 H16A . 0.9700
C16 H16B . 0.9700
C16 C17 . 1.512(8)
C22 C23 . 1.392(7)
C22 C21 . 1.498(8)
C22 C27 . 1.371(8)
C5 H5 . 0.9300
C25 C24 . 1.363(7)
C25 C26 . 1.379(8)
C25 C28 . 1.498(8)
C23 H23 . 0.9300
C23 C24 . 1.382(9)
C17 H17A . 0.9700
C17 H17B . 0.9700
C13 H13A . 0.9700
C13 H13B . 0.9700
C24 H24 . 0.9300
C15 H15A . 0.9700
C15 H15B . 0.9700
C15 C14 . 1.503(8)
C27 H27 . 0.9300
C27 C26 . 1.387(9)
C26 H26 . 0.9300
C14 H14A . 0.9700
C14 H14B . 0.9700
C12 H12A . 0.9600
C12 H12B . 0.9600
C12 H12C . 0.9600
C28 H28A . 0.9600
C28 H28B . 0.9600
C28 H28C . 0.9600
C18 H18A . 0.9600
C18 H18B . 0.9600
C18 H18C . 0.9600
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
O2 H2 O3 . 0.82 1.76 2.522(6) 155
N3 H3 O5 . 0.98 1.63 2.610(6) 175
N3 H3 O6 . 0.98 2.51 3.125(6) 121
C11 H11 O6 1_565 0.98 2.28 3.147(6) 147
C12 H12C O3 4_466 0.96 2.52 3.308(8) 139
C13 H13A O3 4_566 0.97 2.40 3.302(8) 154
C14 H14B F1 . 0.97 2.30 2.785(6) 110
C15 H15B O1 1_545 0.97 2.58 3.268(7) 128
C16 H16B O2 4_466 0.97 2.55 3.277(7) 131
C18 H18C F1 4_456 0.96 2.54 3.279(8) 134
C28 H28B O2 2_665 0.96 2.60 3.481(7) 153
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
F1 C6 C5 C4 . . . . 176.0(5)
O3 C3 C2 C10 . . . . -179.7(6)
O3 C3 C2 C1 . . . . 0.0(10)
O3 C3 C4 C9 . . . . -178.3(6)
O3 C3 C4 C5 . . . . -0.1(9)
N1 C9 C8 O4 . . . . 0.7(9)
N1 C9 C8 C7 . . . . 179.7(6)
N1 C11 C13 O4 . . . . -56.6(6)
N3 C16 C17 N2 . . . . 56.2(6)
N3 C15 C14 N2 . . . . -54.6(6)
N2 C7 C8 O4 . . . . 0.7(9)
N2 C7 C8 C9 . . . . -178.3(6)
N2 C7 C6 F1 . . . . 2.9(10)
N2 C7 C6 C5 . . . . -178.5(6)
C3 C2 C10 N1 . . . . -1.7(10)
C3 C2 C1 O2 . . . . -0.8(9)
C3 C2 C1 O1 . . . . 179.6(7)
C3 C4 C9 N1 . . . . -2.4(9)
C3 C4 C9 C8 . . . . -179.0(5)
C3 C4 C5 C6 . . . . -177.9(6)
C2 C3 C4 C9 . . . . 0.9(9)
C2 C3 C4 C5 . . . . 179.1(6)
C4 C3 C2 C10 . . . . 1.1(9)
C4 C3 C2 C1 . . . . -179.2(6)
C4 C9 C8 O4 . . . . 177.2(5)
C4 C9 C8 C7 . . . . -3.8(9)
C7 N2 C17 C16 . . . . 118.4(6)
C7 N2 C14 C15 . . . . -118.4(6)
C7 C6 C5 C4 . . . . -2.6(10)
C9 N1 C10 C2 . . . . 0.2(9)
C9 N1 C11 C13 . . . . 32.8(8)
C9 N1 C11 C12 . . . . -91.2(6)
C9 C4 C5 C6 . . . . 0.3(9)
C8 O4 C13 C11 . . . . 54.5(6)
C8 C7 C6 F1 . . . . -177.0(5)
C8 C7 C6 C5 . . . . 1.6(10)
C10 N1 C9 C4 . . . . 1.9(9)
C10 N1 C9 C8 . . . . 178.5(5)
C10 N1 C11 C13 . . . . -151.6(5)
C10 N1 C11 C12 . . . . 84.3(6)
C10 C2 C1 O2 . . . . 178.9(6)
C10 C2 C1 O1 . . . . -0.8(10)
C11 N1 C9 C4 . . . . 177.4(5)
C11 N1 C9 C8 . . . . -6.0(9)
C11 N1 C10 C2 . . . . -175.3(6)
C6 C7 C8 O4 . . . . -179.4(5)
C6 C7 C8 C9 . . . . 1.6(9)
C16 N3 C15 C14 . . . . 54.8(6)
C22 C23 C24 C25 . . . . -1.9(10)
C22 C27 C26 C25 . . . . 0.3(10)
C5 C4 C9 N1 . . . . 179.4(5)
C5 C4 C9 C8 . . . . 2.8(9)
C1 C2 C10 N1 . . . . 178.6(6)
C23 C22 C21 O5 . . . . 164.6(6)
C23 C22 C21 O6 . . . . -17.5(9)
C23 C22 C27 C26 . . . . 1.2(9)
C21 C22 C23 C24 . . . . 177.0(6)
C21 C22 C27 C26 . . . . -176.2(6)
C17 N2 C7 C8 . . . . 44.6(9)
C17 N2 C7 C6 . . . . -135.3(6)
C17 N2 C14 C15 . . . . 57.0(7)
C13 O4 C8 C7 . . . . 155.4(5)
C13 O4 C8 C9 . . . . -25.6(8)
C24 C25 C26 C27 . . . . -2.5(10)
C15 N3 C16 C17 . . . . -56.0(6)
C27 C22 C23 C24 . . . . -0.4(9)
C27 C22 C21 O5 . . . . -18.1(8)
C27 C22 C21 O6 . . . . 159.9(6)
C26 C25 C24 C23 . . . . 3.3(9)
C14 N2 C7 C8 . . . . -140.5(6)
C14 N2 C7 C6 . . . . 39.6(10)
C14 N2 C17 C16 . . . . -57.0(7)
C12 C11 C13 O4 . . . . 65.4(6)
C28 C25 C24 C23 . . . . -176.2(6)
C28 C25 C26 C27 . . . . 177.0(6)
C18 N3 C16 C17 . . . . 180.0(4)
C18 N3 C15 C14 . . . . 178.6(5)
_cod_database_fobs_code 2023543