#------------------------------------------------------------------------------
#$Date: 2022-11-10 03:46:29 +0100 (Thu, 10 Nov 2022) $
#$Revision: 279170 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022693.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_2022693
loop_
_publ_author_name
'Felczak, Aleksandra'
'Kalinowska-Lis, Urszula'
'Kusz, Joachim'
'Checi\'nska, Lilianna'
_publ_section_title
;
Zwitterionic versus neutral molecules of fluoroquinolones: crystal
structure of danofloxacin dihydrate
;
_journal_coeditor_code VP3026
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229622010300
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration rmad
_chemical_formula_iupac 'C19 H20 F N3 O3, 2H2 O'
_chemical_formula_moiety 'C19 H20 F N3 O3, 2(H2 O)'
_chemical_formula_sum 'C19 H24 F N3 O5'
_chemical_formula_weight 393.41
_chemical_name_common
;
Danofloxacin dihydrate
;
_chemical_name_systematic
'(1S,4S)-5-(3-Carboxylato-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2-methyl-2,5-diazabicyclo[2.2.1]heptan-2-ium dihydrate'
_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 mixed
_atom_sites_solution_primary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.1687(4)
_cell_length_b 10.6689(7)
_cell_length_c 23.4887(15)
_cell_measurement_reflns_used 3993
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.2110
_cell_measurement_theta_min 3.5150
_cell_volume 1796.47(19)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0403
_diffrn_reflns_av_unetI/netI 0.0487
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 9878
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.299
_diffrn_reflns_theta_min 3.424
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.113
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.15465
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.455
_exptl_crystal_description needle(x)2610
_exptl_crystal_F_000 832
_exptl_crystal_size_max 0.262
_exptl_crystal_size_mid 0.105
_exptl_crystal_size_min 0.055
_refine_diff_density_max 0.444
_refine_diff_density_min -0.248
_refine_ls_abs_structure_details
;
Flack x determined using 1169 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.1(5)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 274
_refine_ls_number_reflns 4050
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.006
_refine_ls_R_factor_all 0.0539
_refine_ls_R_factor_gt 0.0426
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1038
_refine_ls_wR_factor_ref 0.1081
_reflns_number_gt 3470
_reflns_number_total 4050
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vp3026sup1.cif
_cod_data_source_block DFX-Mo
_cod_database_code 2022693
_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
;
0 2 0 153.345 4.98038 2
0 3 0 0.02012 0.29945 2
0 4 0 1.02896 0.36583 2
0 5 0-0.06707 0.39031 2
0 6 0 49.2728 1.85183 2
0 7 0 0.12983 0.48675 2
0 8 0 7.17051 0.56920 1
0 8 0 7.00343 0.75878 2
0 9 0-0.49259 0.71693 2
0 9 0-0.11148 0.45835 1
0 10 0 0.82698 0.80409 2
0 10 0 1.12919 0.53527 1
0 11 0-0.25603 0.55613 1
0 11 0 0.53006 0.84992 2
0 12 0 35.9386 1.83074 2
0 12 0 36.8733 1.60607 1
0 13 0 0.16757 0.64345 1
0 13 0-0.74522 1.05160 2
0 14 0 2.54752 1.16465 2
0 2 -1 125.144 4.08933 2
0 3 -1 58.6533 2.01511 2
0 4 -1 316.214 10.4273 2
0 4 1 325.574 10.4129 2
0 5 -1 0.01181 0.38994 2
0 5 1 0.97952 0.37696 2
0 6 -1 8.77089 0.64318 2
0 6 1 8.47841 0.60082 2
0 7 1 64.5535 2.39164 2
0 7 1 66.5080 2.31538 1
0 7 -1 62.9763 2.40424 2
0 8 1 52.6604 1.97874 1
0 8 -1 51.5403 1.99102 1
0 8 1 55.6557 2.10413 2
0 8 -1 54.9380 2.09920 2
0 9 1 24.5062 1.28374 2
0 9 1 25.9089 1.14333 1
0 9 -1 24.3004 1.14136 1
0 9 -1 25.9424 1.30915 2
0 10 1 10.3238 0.98860 2
0 10 -1 10.2163 0.77695 1
0 10 -1 10.2038 1.00815 2
0 10 1 10.3118 0.74365 1
0 11 1 2.11917 0.57272 1
0 11 -1 2.63434 0.59315 1
0 11 1 3.09779 0.89492 2
0 11 -1 2.58662 0.90079 2
0 12 1 1.92055 0.61116 1
0 12 1 1.57524 0.97691 2
0 12 -1 0.81040 0.64860 1
0 12 -1 1.90847 0.97576 2
0 13 -1 5.37873 0.77342 1
0 13 -1 3.56868 1.09067 2
0 13 1 5.54803 1.11095 2
0 13 1 5.03705 0.73556 1
0 14 -1-0.78361 1.15108 2
0 14 1-2.03499 1.18064 2
0 2 -2 21.9356 0.84132 2
0 3 -2 110.127 3.66823 2
0 4 -2 36.7253 1.38615 2
0 5 -2 165.575 5.64243 2
0 5 2 172.759 5.60558 2
0 6 2 2.04883 0.32914 1
0 6 2 2.23854 0.46883 2
0 6 -2 3.07461 0.52768 2
0 7 -2 20.4134 1.05421 2
0 7 2 21.4827 1.03509 2
0 7 2 22.1090 0.93929 1
0 8 2 18.3731 0.86962 1
0 8 2 19.0790 1.02937 2
0 8 -2 18.3449 1.04520 2
0 9 2 5.36605 0.79131 2
0 9 -2 5.51231 0.80218 2
0 9 -2 4.72615 0.59569 1
0 9 2 5.75252 0.55480 1
0 10 -2 36.3526 1.66675 2
0 10 -2 32.7141 1.46419 1
0 10 2 33.2782 1.61019 2
0 10 2 34.7932 1.42595 1
0 11 2 4.84963 0.61206 1
0 11 -2 5.21058 0.70495 1
0 11 2 4.55095 0.92983 2
0 11 -2 4.72187 0.93771 2
0 12 2 7.69534 1.06186 2
0 12 -2 6.87046 1.06027 2
0 12 2 6.69619 0.70834 1
0 12 -2 5.81645 0.75482 1
0 13 2 0.63995 0.63686 1
0 13 -2 0.61204 1.03132 2
0 13 -2 0.19870 0.70780 1
0 13 2 2.26494 1.05349 2
0 14 -2 11.4597 1.34743 2
0 14 2 12.7562 1.37912 2
0 2 -3 210.567 6.66247 2
0 2 3 202.765 6.59200 1
0 3 -3 92.2013 3.18905 2
0 3 3 96.1045 3.11009 1
0 4 3 2.02645 0.24145 1
0 4 -3 1.71654 0.41542 2
0 5 -3 119.827 4.10406 2
0 5 3 121.572 4.01115 1
0 6 -3 2.33087 0.47608 2
0 6 3 2.64712 0.45339 2
0 6 3 2.58931 0.34026 1
0 7 3 0.13168 0.46376 2
0 7 3-0.02271 0.31956 1
0 7 -3-0.49594 0.52650 2
0 8 -3 40.3518 1.74422 2
0 8 3 43.4002 1.71460 2
0 8 3 41.9562 1.59443 1
0 9 -3 33.9735 1.55147 2
0 9 3 31.9124 1.50353 2
0 9 -3 32.7155 1.38457 1
0 9 3 30.9211 1.31140 1
0 10 3 12.3621 1.06080 2
0 10 -3 12.1959 0.85554 1
0 10 3 13.5472 0.78590 1
0 10 -3 12.4914 1.05768 2
0 11 3 0.72287 0.50181 1
0 11 3-0.23932 0.84178 2
0 11 -3 0.56030 0.56534 1
0 11 -3 0.33733 0.85132 2
0 12 3 2.71391 0.98517 2
0 12 -3 1.79424 0.98395 2
0 12 -3 2.30477 0.68426 1
0 12 3 2.61411 0.58512 1
0 13 3 6.06477 1.12687 2
0 13 -3 6.29972 1.13309 2
0 13 -3 4.91640 0.80476 1
0 13 3 4.54498 0.71252 1
0 14 3 7.48561 0.82960 1
0 14 3 7.79282 1.30453 2
0 14 -3 6.10413 1.20844 2
0 0 -4 199.068 6.43801 3
0 1 -4 20.7101 0.76189 2
0 2 -4 5.96956 0.42133 2
0 2 4 5.95162 0.24215 1
0 3 4 69.6729 2.29938 1
0 3 -4 70.2585 2.41207 2
0 4 4 27.2675 0.98035 1
0 4 -4 26.9737 1.10489 2
0 5 -4 59.1151 2.18745 2
0 5 4 61.1999 2.07180 1
0 6 4 0.76069 0.27056 1
0 6 4 0.34024 0.39762 2
0 6 -4 0.15333 0.46154 2
0 7 -4 30.0566 1.33320 2
0 7 4 31.9794 1.29294 2
0 7 4 28.9821 1.16677 1
0 8 4 2.04533 0.59218 2
0 8 4 1.70058 0.38600 1
0 8 -4 1.17432 0.63607 2
0 9 4 70.3180 2.51870 1
0 9 4 74.2900 2.69043 2
0 9 -4 70.6210 2.71760 2
0 9 -4 69.3092 2.60674 1
0 10 4 1.65575 0.46540 1
0 10 -4 0.73313 0.55323 1
0 10 4 1.05337 0.76980 2
0 10 -4 1.29129 0.81142 2
0 11 4 0.65709 0.81131 2
0 11 4 0.64043 0.47145 1
0 11 -4 0.02029 0.58517 1
0 11 -4 0.68928 0.88073 2
0 12 -4 0.21503 0.65691 1
0 12 -4 1.66511 0.95867 2
0 12 4-0.28238 0.52765 1
0 12 4 0.79884 0.92345 2
0 13 -4 10.9773 1.27412 2
0 13 -4 12.7161 1.01168 1
0 13 4 12.8518 1.26832 2
0 13 4 13.3448 0.88125 1
0 14 4 31.9034 1.51481 1
0 14 4 34.7947 1.92150 2
0 0 -5 0.30958 0.26311 3
0 1 -5 54.7060 1.73007 3
0 -1 -5 45.8842 1.78279 3
0 2 -5 14.0606 0.64110 2
0 2 5 13.5760 0.46804 1
0 3 -5 78.4845 2.60980 2
0 3 5 74.9957 2.47827 1
0 4 5 21.0099 0.77664 1
0 4 -5 22.2776 0.95280 2
0 5 5 43.7173 1.50636 1
0 5 -5 41.7465 1.65648 2
0 6 5 1.20082 0.25524 1
0 6 -5 0.55698 0.48374 2
0 7 5 21.4160 0.86926 1
0 7 5 20.8603 0.99283 2
0 7 -5 19.8012 1.06610 2
0 8 5 11.8032 0.63876 1
0 8 5 12.3768 0.82235 2
0 8 -5 12.7683 0.90619 2
0 9 5 61.6163 2.23294 1
0 9 -5 59.1106 2.32747 1
0 9 -5 64.2061 2.46943 2
0 9 5 65.6738 2.40014 2
0 10 5 24.9880 1.12071 1
0 10 -5 26.2862 1.42299 2
0 10 5 28.0659 1.39508 2
0 10 -5 24.9693 1.22596 1
0 11 5 2.59409 0.85181 2
0 11 -5 2.10917 0.90070 2
0 11 5 2.37350 0.49593 1
0 11 -5 1.50348 0.58934 1
0 12 5 2.36114 0.53939 1
0 12 5 3.72515 0.96180 2
0 12 -5 1.90330 0.70127 1
0 12 -5 2.24383 0.95730 2
0 13 -5-0.59352 1.00942 2
0 13 5 0.34062 0.57322 1
0 13 -5-0.18525 0.72506 1
0 13 5 1.02980 1.03610 2
0 14 5-0.40306 0.66572 1
0 0 -6 260.257 8.42982 3
0 -1 6 22.9892 0.85187 2
0 -1 -6 19.8149 0.88992 3
0 1 -6 21.6019 0.81358 3
0 2 -6 22.9078 0.88302 2
0 2 6 21.6516 0.72023 1
0 3 6 56.3960 1.86855 1
0 3 -6 59.2986 2.03047 2
0 4 -6 1.62201 0.43377 2
0 4 6 2.18329 0.19251 1
0 5 6 5.40073 0.31368 1
0 5 -6 5.32196 0.55097 2
0 6 6 1.66528 0.25273 1
0 6 -6 2.15436 0.51026 2
0 7 6 50.7268 1.81298 1
0 7 6 53.7258 1.93142 2
0 7 -6 50.3452 2.01088 2
0 8 6 4.37418 0.40402 1
0 8 -6 3.25713 0.69563 2
0 8 6 4.53696 0.60742 2
0 9 6 0.91063 0.36628 1
0 9 -6 1.35924 0.72673 2
0 9 6 0.20118 0.64919 2
0 10 6 0.52881 0.40359 1
0 10 6 0.44203 0.74223 2
0 10 -6-0.30072 0.80099 2
0 10 -6 0.36923 0.54203 1
0 11 6 4.32883 0.86472 2
0 11 -6 2.63753 0.94007 2
0 11 6 3.19331 0.50927 1
0 11 -6 3.78686 0.64894 1
0 12 6 2.47607 0.53496 1
0 12 6 3.11162 0.96684 2
0 12 -6 3.28444 0.98307 2
0 12 -6 2.18745 0.70195 1
0 13 -6 6.96586 1.11623 2
0 13 6 5.23366 0.66588 1
0 13 6 3.52399 1.08844 2
0 13 -6 5.92262 0.85410 1
0 0 -7 0.15224 0.31994 3
0 -1 -7 6.58383 0.53312 3
0 1 -7 7.28387 0.42761 3
0 -1 7 7.28775 0.45435 2
0 2 7 176.957 5.73196 1
0 -2 7 193.318 5.88399 2
0 -2 -7 177.626 5.74183 1
0 2 -7 185.842 5.86964 2
0 3 7 2.07528 0.13960 1
0 3 -7 1.72264 0.40738 2
0 4 7 37.7032 1.28318 1
0 4 -7 39.1413 1.48972 2
0 5 7 3.95661 0.25996 1
0 5 -7 4.22151 0.53402 2
0 6 7 11.4382 0.50400 1
0 6 -7 10.7878 0.74891 2
0 7 7 12.2884 0.57925 1
0 7 7 12.5976 0.72475 2
0 7 -7 12.8599 0.84721 2
0 8 7-0.06132 0.53151 2
0 8 7 0.12778 0.28959 1
0 8 -7 0.10445 0.62762 2
0 9 7 18.8891 0.86073 1
0 9 -7 20.4184 1.19047 2
0 9 7 19.5387 1.09344 2
0 10 7 2.13009 0.77124 2
0 10 -7 1.35811 0.83097 2
0 10 7 1.89105 0.40616 1
0 10 -7 1.54610 0.58709 1
0 11 -7 0.59668 0.86607 2
0 11 7 0.67844 0.43158 1
0 11 -7 0.27459 0.59204 1
0 11 7 0.50819 0.81872 2
0 12 7 0.80198 0.48228 1
0 12 7 0.75791 0.92291 2
0 12 -7 0.88418 0.94280 2
0 12 -7 0.84191 0.66477 1
0 13 7 0.33126 1.08739 3
0 13 7 1.31612 1.03021 2
0 13 7 0.60588 0.54030 1
0 13 -7 0.77997 0.72479 1
0 0 -8 122.506 4.07006 3
0 1 -8 5.60063 0.43363 3
0 -1 8 5.68117 0.42990 2
0 -1 -8 5.73127 0.20646 1
0 -1 -8 5.82724 0.52029 3
0 -2 -8 1.05401 0.10448 1
0 -2 8 0.80619 0.39159 2
0 2 -8 0.79248 0.31966 3
0 2 8 1.27735 0.40883 3
0 3 -8 118.522 3.78581 2
0 3 8 110.682 3.60391 1
0 4 8 29.0250 0.98373 1
0 4 -8 27.9816 1.20537 2
0 5 -8 1.52147 0.49782 2
0 5 8 1.94243 0.18943 1
0 6 -8-0.13974 0.51371 2
0 6 8 0.27105 0.19462 1
0 7 8 13.7901 0.59966 1
0 7 -8 12.7542 0.88108 2
0 8 8 0.51204 0.27800 1
0 8 -8-0.87497 0.68941 2
0 8 8 0.01492 0.51234 2
0 9 8 70.1168 2.52587 2
0 9 8 65.5085 2.34004 1
0 9 -8 67.2950 2.63238 2
0 10 -8 15.9380 1.14026 2
0 10 8 15.2410 0.76197 1
0 10 8 16.4957 1.07414 2
0 10 -8 16.2269 0.95240 1
0 11 -8 8.82025 1.05047 2
0 11 8 8.17087 0.95455 2
0 11 -8 8.57250 0.80601 1
0 11 8 7.82918 0.59787 1
0 12 8 1.71960 0.49235 1
0 12 -8 1.47261 0.70086 1
0 12 8 1.63562 0.97746 3
0 12 -8 0.51568 0.94277 2
0 12 8 1.27076 0.92246 2
0 13 8 1.13703 0.51487 1
0 13 8-0.28468 1.03870 3
0 0 -9-0.14330 0.39088 3
0 -1 9 21.5573 0.84497 2
0 1 -9 21.4669 0.86067 3
0 -1 -9 18.6001 0.91646 3
0 -1 -9 19.9294 0.66069 1
0 2 -9 414.226 12.3762 3
0 -2 -9 376.492 12.2576 1
0 -2 9 393.212 12.4203 2
0 3 9 139.619 4.49303 1
0 4 9 5.42467 0.24487 1
0 4 -9 6.36933 0.55041 2
0 5 -9 17.7934 0.91505 2
0 5 9 16.5327 0.61780 1
0 6 9 28.3009 1.01893 1
0 6 -9 30.1679 1.28854 2
0 -6 9 27.5210 1.30235 2
0 7 9 1.29115 0.23633 1
0 7 -9 1.69763 0.62875 2
0 8 -9 3.35886 0.70476 2
0 8 9 2.54455 0.55383 2
0 8 9 3.31022 0.33171 1
0 9 -9 14.3906 1.05500 2
0 9 9 13.2150 0.89770 2
0 9 9 12.9715 0.64968 1
0 10 -9 2.13406 0.59190 1
0 10 9 2.73874 0.40360 1
0 10 9 3.17223 0.75933 2
0 10 -9 3.09120 0.84565 2
0 11 9 1.62106 0.97510 3
0 11 9 0.87552 0.81599 2
0 11 -9 1.35184 0.63784 1
0 11 9 1.57491 0.41067 1
0 11 -9 1.70769 0.88080 2
0 12 -9 3.38712 0.72938 1
0 12 9 4.84923 0.96973 2
0 12 9 3.58141 0.51348 1
0 12 9 1.93311 1.00181 3
0 13 9 3.11343 0.54764 1
0 13 9 2.14987 1.04037 3
0 0 -10 3.15453 0.45752 3
0 -1 10 62.4138 2.11937 2
0 -1 -10 59.4829 2.18751 3
0 1 -10 67.0194 2.14371 3
0 -1 -10 60.0576 1.95981 1
0 -2 10 78.9799 2.75986 2
0 2 -10 87.2220 2.72882 3
0 -2 -10 79.0920 2.57463 1
0 3 10 0.08680 0.07524 1
0 4 -10 1.89128 0.45594 2
0 4 10 1.00144 0.11761 1
0 5 -10 200.297 6.20748 2
0 5 10 181.015 5.95088 1
0 6 -10 12.9633 0.85169 2
0 -6 10 12.4548 0.87055 2
0 6 10 12.8351 0.92839 3
0 6 10 13.4266 0.52984 1
0 7 10 3.44970 0.28187 1
0 7 -10 3.60894 0.66310 2
0 7 10 3.31204 0.75086 3
0 8 10 1.47436 0.52064 2
0 8 10 1.35899 0.27786 1
0 8 -10 2.19709 0.68928 2
0 8 10 2.07178 0.85324 3
0 9 -10 2.50423 0.77705 2
0 9 10 1.47602 0.31373 1
0 9 10 1.45257 0.60638 2
0 9 10 1.93034 0.95531 3
0 10 10 4.03654 0.75557 2
0 10 -10 4.45508 0.66824 1
0 10 10 4.01261 0.42397 1
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-9 0 0-0.51029 1.16980 3
-9 -1 0 23.3908 1.55065 3
-9 -2 0 20.7175 1.45578 3
-9 -3 0 1.84443 0.99967 3
-9 -4 0 4.83069 1.07310 3
-9 -4 1 3.43829 1.02484 3
-9 -3 1 2.61485 0.98239 3
-9 -2 1 3.90637 1.05214 3
-9 -1 1 0.41873 1.08815 3
-9 0 -1 2.59347 1.22743 3
-9 0 1 1.22287 1.10628 3
-9 -1 -1 0.85376 1.08974 3
-9 -2 -1 6.08328 1.14146 3
-9 -3 -1 2.90452 1.02470 3
-9 -4 -1 4.46441 1.07941 3
-9 -3 2-0.22596 0.93749 3
-9 -2 2 0.58643 0.92993 3
-9 -1 2 7.04998 1.05501 3
-9 0 2 3.63751 1.08637 3
-9 -1 -2 7.41411 1.24787 3
-9 -2 -2-0.49767 1.09707 3
-9 -3 -2-0.13412 1.00619 3
-9 -4 -2 6.26711 1.17880 3
-9 -3 3 1.10260 0.88912 3
-9 -2 3 2.71865 0.90734 3
-9 -1 3 3.12443 0.94814 3
-9 0 3-0.17683 1.01491 3
-9 -1 -3 4.21112 1.20472 3
-9 -2 -3 1.22110 1.11741 3
-9 -3 -3 0.14010 1.05186 3
-9 -4 -3 10.1811 1.27701 3
-9 -2 4 1.48854 0.85553 3
-9 -1 4 1.21323 0.85971 3
-9 0 4 0.99931 0.95954 3
-9 -3 -4-0.02929 1.11254 3
-9 -4 -4 5.41407 1.23123 3
-9 -2 5 1.28576 0.84165 3
-9 -1 5 6.91975 0.95471 3
-9 0 5 6.38914 1.05516 3
-9 -1 6 4.77237 0.90215 3
-9 0 6 6.21141 1.01918 3
-9 -1 7 2.18307 0.80583 3
-9 0 7 2.51148 0.91319 3
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 36373
_shelx_res_file
;
TITL danofloxacin-Mo
shelx.res
created by SHELXL-2018/3 at 18:37:02 on 30-Sep-2022
CELL 0.71073 7.1687 10.6689 23.4887 90.000 90.000 90.000
ZERR 4.00 0.0004 0.0007 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 F N O
UNIT 76 96 4 12 20
MERG 2
OMIT 2 0 0
OMIT 8 3 1
DFIX 0.82 0.01 O27 H27A O27 H27B
EQIV $1 x-1/2, -y+1/2, -z+1
HTAB N20 O26_$1
HTAB O27 O26
EQIV $2 -x+1, y-1/2, -z+3/2
HTAB O27 O24_$2
HTAB O28 O24
EQIV $3 x, y+1, z
HTAB O28 O27_$3
FMAP 2
PLAN 5
ACTA
BOND $H
CONF
L.S. 8
TEMP -173.00
WGHT 0.073100
FVAR 0.21717
N1 4 0.625587 0.531974 0.512276 11.00000 0.01586 0.01009 =
0.01635 0.00107 0.00084 0.00042
C2 1 0.617681 0.569857 0.567081 11.00000 0.01218 0.01286 =
0.02013 -0.00193 0.00057 -0.00044
AFIX 43
H2 2 0.599788 0.656652 0.574276 11.00000 -1.20000
AFIX 0
C3 1 0.633731 0.491536 0.612905 11.00000 0.01008 0.01440 =
0.01812 -0.00312 0.00019 0.00025
C4 1 0.654580 0.359041 0.603829 11.00000 0.00866 0.01556 =
0.01883 -0.00050 -0.00023 -0.00025
C5 1 0.649894 0.318941 0.544861 11.00000 0.01033 0.01088 =
0.01648 0.00069 -0.00061 0.00007
C6 1 0.659652 0.190404 0.531313 11.00000 0.01276 0.01219 =
0.01768 0.00330 -0.00055 -0.00100
AFIX 43
H6 2 0.659635 0.129618 0.560868 11.00000 -1.20000
AFIX 0
C7 1 0.669009 0.153587 0.476489 11.00000 0.01635 0.00805 =
0.02041 -0.00106 -0.00174 0.00052
C8 1 0.675155 0.238493 0.429800 11.00000 0.00953 0.01401 =
0.01677 -0.00154 0.00018 -0.00054
C9 1 0.659030 0.365514 0.443207 11.00000 0.01273 0.01201 =
0.01679 0.00160 -0.00001 0.00033
AFIX 43
H9 2 0.657696 0.425771 0.413432 11.00000 -1.20000
AFIX 0
C10 1 0.644873 0.405353 0.499488 11.00000 0.01080 0.01087 =
0.01762 -0.00032 0.00056 0.00021
C11 1 0.615482 0.620776 0.464940 11.00000 0.02165 0.00986 =
0.01528 0.00220 0.00106 -0.00050
AFIX 13
H11 2 0.728748 0.624920 0.440161 11.00000 -1.20000
AFIX 0
C12 1 0.510647 0.740310 0.471322 11.00000 0.02838 0.01420 =
0.02731 0.00207 0.00256 0.00531
AFIX 23
H12A 2 0.560422 0.815493 0.451842 11.00000 -1.20000
H12B 2 0.449367 0.756900 0.508334 11.00000 -1.20000
AFIX 0
C13 1 0.432729 0.636721 0.434888 11.00000 0.02292 0.01717 =
0.02344 0.00609 -0.00293 0.00003
AFIX 23
H13A 2 0.323952 0.589593 0.449588 11.00000 -1.20000
H13B 2 0.435057 0.648213 0.393071 11.00000 -1.20000
AFIX 0
N14 4 0.709289 0.197301 0.375661 11.00000 0.01589 0.00959 =
0.01692 -0.00004 0.00011 -0.00058
C15 1 0.734467 0.285055 0.328040 11.00000 0.01355 0.01170 =
0.01688 0.00061 0.00232 -0.00144
AFIX 13
H15 2 0.822428 0.355648 0.336022 11.00000 -1.20000
AFIX 0
C16 1 0.798303 0.196222 0.281028 11.00000 0.01270 0.01449 =
0.01762 -0.00091 0.00149 -0.00127
AFIX 23
H16A 2 0.804532 0.236739 0.243158 11.00000 -1.20000
H16B 2 0.917492 0.153580 0.289865 11.00000 -1.20000
AFIX 0
C17 1 0.629178 0.111622 0.288052 11.00000 0.01330 0.01315 =
0.01685 -0.00175 0.00057 0.00337
AFIX 13
H17 2 0.625929 0.038087 0.261672 11.00000 -1.20000
AFIX 0
C18 1 0.637471 0.077704 0.351328 11.00000 0.01541 0.01007 =
0.01750 -0.00252 0.00056 0.00037
AFIX 23
H18A 2 0.512575 0.056574 0.366538 11.00000 -1.20000
H18B 2 0.724078 0.007168 0.358492 11.00000 -1.20000
AFIX 0
C19 1 0.543889 0.325755 0.305789 11.00000 0.01581 0.00948 =
0.01855 -0.00131 0.00048 -0.00090
AFIX 23
H19A 2 0.555589 0.391756 0.276379 11.00000 -1.20000
H19B 2 0.462960 0.356468 0.336962 11.00000 -1.20000
AFIX 0
N20 4 0.469643 0.203456 0.280519 11.00000 0.01259 0.01333 =
0.01717 -0.00054 0.00150 -0.00083
C21 1 0.408765 0.217321 0.220521 11.00000 0.01900 0.02154 =
0.01764 0.00081 -0.00230 0.00011
AFIX 137
H21A 2 0.513152 0.248092 0.197491 11.00000 -1.50000
H21B 2 0.305277 0.277177 0.218524 11.00000 -1.50000
H21C 2 0.367629 0.135857 0.205893 11.00000 -1.50000
AFIX 0
F22 3 0.683883 0.029332 0.464360 11.00000 0.03253 0.00829 =
0.02016 -0.00088 -0.00122 0.00204
C23 1 0.626537 0.545685 0.672355 11.00000 0.01728 0.01131 =
0.01560 -0.00061 0.00093 -0.00373
O24 5 0.501255 0.625257 0.682477 11.00000 0.02013 0.02181 =
0.02518 -0.00733 -0.00338 0.00745
O25 5 0.741923 0.506160 0.707746 11.00000 0.02696 0.02145 =
0.02256 -0.00324 -0.00653 0.00561
O26 5 0.678195 0.280761 0.643399 11.00000 0.01598 0.01493 =
0.01579 0.00072 -0.00153 0.00022
O27 5 0.618333 0.055949 0.702538 11.00000 0.02145 0.02127 =
0.02811 0.00839 0.00388 0.00312
O28 5 0.458824 0.863059 0.630478 11.00000 0.03583 0.03377 =
0.03256 0.00650 -0.00828 -0.00352
H20 2 0.371541 0.178653 0.302854 11.00000 0.00813
H27A 2 0.620607 0.122179 0.683490 11.00000 0.06002
H27B 2 0.571004 0.071315 0.734399 11.00000 0.01794
H28A 2 0.474509 0.797691 0.650850 11.00000 0.05473
H28B 2 0.502532 0.917734 0.650515 11.00000 0.03930
HKLF 4
REM danofloxacin-Mo
REM wR2 = 0.1081, GooF = S = 1.006, Restrained GooF = 1.006 for all data
REM R1 = 0.0426 for 3470 Fo > 4sig(Fo) and 0.0539 for all 4050 data
REM 274 parameters refined using 2 restraints
END
WGHT 0.0706 0.0000
REM Highest difference peak 0.444, deepest hole -0.248, 1-sigma level 0.061
Q1 1 0.6422 0.3385 0.5722 11.00000 0.05 0.44
Q2 1 0.6228 0.0961 0.3203 11.00000 0.05 0.43
Q3 1 0.6260 0.5203 0.6394 11.00000 0.05 0.42
Q4 1 0.7034 0.1825 0.5004 11.00000 0.05 0.38
Q5 1 0.4391 0.2093 0.2490 11.00000 0.05 0.35
;
_shelx_res_checksum 15429
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
N N1 0.6256(3) 0.53197(17) 0.51228(8) 0.0141(4) Uani d 1 . .
C C2 0.6177(3) 0.5699(2) 0.56708(10) 0.0151(5) Uani d 1 . .
H H2 0.599788 0.656652 0.574276 0.018 Uiso calc 1 . .
C C3 0.6337(3) 0.4915(2) 0.61290(9) 0.0142(5) Uani d 1 . .
C C4 0.6546(3) 0.3590(2) 0.60383(10) 0.0144(5) Uani d 1 . .
C C5 0.6499(3) 0.3189(2) 0.54486(9) 0.0126(5) Uani d 1 . .
C C6 0.6597(3) 0.1904(2) 0.53131(10) 0.0142(5) Uani d 1 . .
H H6 0.659635 0.129618 0.560868 0.017 Uiso calc 1 . .
C C7 0.6690(3) 0.1536(2) 0.47649(10) 0.0149(5) Uani d 1 . .
C C8 0.6752(3) 0.2385(2) 0.42980(9) 0.0134(5) Uani d 1 . .
C C9 0.6590(3) 0.3655(2) 0.44321(9) 0.0138(5) Uani d 1 . .
H H9 0.657696 0.425771 0.413432 0.017 Uiso calc 1 . .
C C10 0.6449(3) 0.4054(2) 0.49949(9) 0.0131(5) Uani d 1 . .
C C11 0.6155(4) 0.6208(2) 0.46494(10) 0.0156(5) Uani d 1 . .
H H11 0.728748 0.624920 0.440161 0.019 Uiso calc 1 . .
C C12 0.5106(4) 0.7403(2) 0.47132(11) 0.0233(6) Uani d 1 . .
H H12A 0.560422 0.815493 0.451842 0.028 Uiso calc 1 . .
H H12B 0.449367 0.756900 0.508334 0.028 Uiso calc 1 . .
C C13 0.4327(4) 0.6367(2) 0.43489(11) 0.0212(5) Uani d 1 . .
H H13A 0.323952 0.589593 0.449588 0.025 Uiso calc 1 . .
H H13B 0.435057 0.648213 0.393071 0.025 Uiso calc 1 . .
N N14 0.7093(3) 0.19730(18) 0.37566(8) 0.0141(4) Uani d 1 . .
C C15 0.7345(3) 0.2851(2) 0.32804(9) 0.0140(5) Uani d 1 . .
H H15 0.822428 0.355648 0.336022 0.017 Uiso calc 1 . .
C C16 0.7983(3) 0.1962(2) 0.28103(9) 0.0149(5) Uani d 1 . .
H H16A 0.804532 0.236739 0.243158 0.018 Uiso calc 1 . .
H H16B 0.917492 0.153580 0.289865 0.018 Uiso calc 1 . .
C C17 0.6292(3) 0.1116(2) 0.28805(10) 0.0144(5) Uani d 1 . .
H H17 0.625929 0.038087 0.261672 0.017 Uiso calc 1 . .
C C18 0.6375(3) 0.0777(2) 0.35133(9) 0.0143(5) Uani d 1 . .
H H18A 0.512575 0.056574 0.366538 0.017 Uiso calc 1 . .
H H18B 0.724078 0.007168 0.358492 0.017 Uiso calc 1 . .
C C19 0.5439(3) 0.3258(2) 0.30579(10) 0.0146(5) Uani d 1 . .
H H19A 0.555589 0.391756 0.276379 0.018 Uiso calc 1 . .
H H19B 0.462960 0.356468 0.336962 0.018 Uiso calc 1 . .
N N20 0.4696(3) 0.20346(19) 0.28052(8) 0.0144(4) Uani d 1 . .
C C21 0.4088(4) 0.2173(2) 0.22052(10) 0.0194(5) Uani d 1 . .
H H21A 0.513152 0.248092 0.197491 0.029 Uiso calc 1 . .
H H21B 0.305277 0.277177 0.218524 0.029 Uiso calc 1 . .
H H21C 0.367629 0.135857 0.205893 0.029 Uiso calc 1 . .
F F22 0.6839(2) 0.02933(12) 0.46436(6) 0.0203(3) Uani d 1 . .
C C23 0.6265(3) 0.5457(2) 0.67236(9) 0.0147(5) Uani d 1 . .
O O24 0.5013(2) 0.62526(18) 0.68248(7) 0.0224(4) Uani d 1 . .
O O25 0.7419(3) 0.50616(17) 0.70775(7) 0.0237(4) Uani d 1 . .
O O26 0.6782(2) 0.28076(16) 0.64340(6) 0.0156(4) Uani d 1 . .
O O27 0.6183(3) 0.05595(17) 0.70254(8) 0.0236(4) Uani d 1 . .
O O28 0.4588(3) 0.8631(3) 0.63048(9) 0.0341(5) Uani d 1 . .
H H20 0.372(4) 0.179(2) 0.3029(11) 0.008(6) Uiso d 1 . .
H H27A 0.621(6) 0.122(2) 0.6835(14) 0.060(13) Uiso d 1 . .
H H27B 0.571(4) 0.071(3) 0.7344(8) 0.018(7) Uiso d 1 . .
H H28A 0.475(6) 0.798(5) 0.6509(17) 0.055(12) Uiso d 1 . .
H H28B 0.503(5) 0.918(4) 0.6505(16) 0.039(11) Uiso 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
N1 0.0159(10) 0.0101(9) 0.0164(9) 0.0004(8) 0.0008(8) 0.0011(7)
C2 0.0122(11) 0.0129(10) 0.0201(11) -0.0004(9) 0.0006(9) -0.0019(9)
C3 0.0101(11) 0.0144(10) 0.0181(11) 0.0003(9) 0.0002(9) -0.0031(9)
C4 0.0087(11) 0.0156(11) 0.0188(11) -0.0003(9) -0.0002(9) -0.0005(9)
C5 0.0103(11) 0.0109(10) 0.0165(11) 0.0001(9) -0.0006(8) 0.0007(8)
C6 0.0128(11) 0.0122(10) 0.0177(10) -0.0010(9) -0.0006(9) 0.0033(9)
C7 0.0164(12) 0.0081(10) 0.0204(11) 0.0005(9) -0.0017(9) -0.0011(9)
C8 0.0095(11) 0.0140(10) 0.0168(10) -0.0005(9) 0.0002(8) -0.0015(9)
C9 0.0127(11) 0.0120(10) 0.0168(10) 0.0003(9) 0.0000(9) 0.0016(9)
C10 0.0108(11) 0.0109(10) 0.0176(11) 0.0002(9) 0.0006(9) -0.0003(8)
C11 0.0217(12) 0.0099(10) 0.0153(10) -0.0005(10) 0.0011(9) 0.0022(9)
C12 0.0284(15) 0.0142(11) 0.0273(13) 0.0053(11) 0.0026(11) 0.0021(10)
C13 0.0229(13) 0.0172(12) 0.0234(12) 0.0000(10) -0.0029(10) 0.0061(10)
N14 0.0159(10) 0.0096(8) 0.0169(9) -0.0006(8) 0.0001(8) 0.0000(8)
C15 0.0136(11) 0.0117(10) 0.0169(11) -0.0014(9) 0.0023(9) 0.0006(9)
C16 0.0127(11) 0.0145(10) 0.0176(11) -0.0013(10) 0.0015(9) -0.0009(9)
C17 0.0133(11) 0.0131(10) 0.0168(10) 0.0034(9) 0.0006(9) -0.0017(9)
C18 0.0154(11) 0.0101(10) 0.0175(11) 0.0004(9) 0.0006(9) -0.0025(8)
C19 0.0158(12) 0.0095(10) 0.0185(11) -0.0009(9) 0.0005(9) -0.0013(8)
N20 0.0126(10) 0.0133(9) 0.0172(9) -0.0008(8) 0.0015(8) -0.0005(8)
C21 0.0190(13) 0.0215(12) 0.0176(11) 0.0001(10) -0.0023(9) 0.0008(10)
F22 0.0325(9) 0.0083(6) 0.0202(7) 0.0020(6) -0.0012(6) -0.0009(5)
C23 0.0173(12) 0.0113(10) 0.0156(10) -0.0037(10) 0.0009(9) -0.0006(8)
O24 0.0201(10) 0.0218(9) 0.0252(9) 0.0074(8) -0.0034(7) -0.0073(7)
O25 0.0270(10) 0.0214(9) 0.0226(9) 0.0056(8) -0.0065(8) -0.0032(8)
O26 0.0160(9) 0.0149(8) 0.0158(8) 0.0002(7) -0.0015(6) 0.0007(6)
O27 0.0215(10) 0.0213(9) 0.0281(10) 0.0031(8) 0.0039(8) 0.0084(8)
O28 0.0358(12) 0.0338(12) 0.0326(11) -0.0035(10) -0.0083(10) 0.0065(11)
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -12 -21 0.0198
0 11 23 0.0349
1 13 14 0.0363
10 0 0 0.1245
-1 -14 -14 0.0231
10 -1 -1 0.1247
-10 4 4 0.1313
1 14 14 0.0384
-8 0 -20 0.1079
2 13 14 0.0399
0 -14 -9 0.0258
-3 4 -5 0.1180
2 -1 5 0.1152
-3 -11 20 0.0595
1 -2 -33 0.0111
2 12 19 0.0347
-1 -2 33 0.0517
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
C2 N1 C10 . . 120.05(18) ?
C2 N1 C11 . . 121.92(19) ?
C10 N1 C11 . . 118.03(19) ?
N1 C2 C3 . . 124.3(2) ?
N1 C2 H2 . . 117.8 ?
C3 C2 H2 . . 117.8 ?
C2 C3 C4 . . 119.5(2) ?
C2 C3 C23 . . 119.4(2) ?
C4 C3 C23 . . 121.1(2) ?
O26 C4 C3 . . 123.8(2) ?
O26 C4 C5 . . 120.8(2) ?
C3 C4 C5 . . 115.43(19) ?
C10 C5 C6 . . 117.8(2) ?
C10 C5 C4 . . 122.0(2) ?
C6 C5 C4 . . 120.1(2) ?
C7 C6 C5 . . 120.1(2) ?
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C6 C7 F22 . . 119.2(2) ?
C6 C7 C8 . . 123.5(2) ?
F22 C7 C8 . . 117.2(2) ?
N14 C8 C9 . . 122.4(2) ?
N14 C8 C7 . . 121.2(2) ?
C9 C8 C7 . . 116.2(2) ?
C10 C9 C8 . . 121.1(2) ?
C10 C9 H9 . . 119.4 ?
C8 C9 H9 . . 119.4 ?
N1 C10 C9 . . 120.6(2) ?
N1 C10 C5 . . 118.3(2) ?
C9 C10 C5 . . 121.1(2) ?
N1 C11 C12 . . 120.2(2) ?
N1 C11 C13 . . 118.4(2) ?
C12 C11 C13 . . 60.55(17) ?
N1 C11 H11 . . 115.5 ?
C12 C11 H11 . . 115.5 ?
C13 C11 H11 . . 115.5 ?
C11 C12 C13 . . 60.05(16) ?
C11 C12 H12A . . 117.8 ?
C13 C12 H12A . . 117.8 ?
C11 C12 H12B . . 117.8 ?
C13 C12 H12B . . 117.8 ?
H12A C12 H12B . . 114.9 ?
C11 C13 C12 . . 59.40(16) ?
C11 C13 H13A . . 117.8 ?
C12 C13 H13A . . 117.8 ?
C11 C13 H13B . . 117.8 ?
C12 C13 H13B . . 117.8 ?
H13A C13 H13B . . 115.0 ?
C8 N14 C15 . . 121.66(19) ?
C8 N14 C18 . . 124.76(19) ?
C15 N14 C18 . . 107.22(17) ?
N14 C15 C19 . . 109.39(18) ?
N14 C15 C16 . . 101.07(18) ?
C19 C15 C16 . . 101.39(18) ?
N14 C15 H15 . . 114.5 ?
C19 C15 H15 . . 114.5 ?
C16 C15 H15 . . 114.5 ?
C17 C16 C15 . . 92.93(17) ?
C17 C16 H16A . . 113.1 ?
C15 C16 H16A . . 113.1 ?
C17 C16 H16B . . 113.1 ?
C15 C16 H16B . . 113.1 ?
H16A C16 H16B . . 110.5 ?
N20 C17 C16 . . 101.84(18) ?
N20 C17 C18 . . 107.18(17) ?
C16 C17 C18 . . 102.40(18) ?
N20 C17 H17 . . 114.6 ?
C16 C17 H17 . . 114.6 ?
C18 C17 H17 . . 114.6 ?
N14 C18 C17 . . 100.57(17) ?
N14 C18 H18A . . 111.7 ?
C17 C18 H18A . . 111.7 ?
N14 C18 H18B . . 111.7 ?
C17 C18 H18B . . 111.7 ?
H18A C18 H18B . . 109.4 ?
C15 C19 N20 . . 101.64(17) ?
C15 C19 H19A . . 111.4 ?
N20 C19 H19A . . 111.4 ?
C15 C19 H19B . . 111.4 ?
N20 C19 H19B . . 111.4 ?
H19A C19 H19B . . 109.3 ?
C21 N20 C17 . . 113.41(18) ?
C21 N20 C19 . . 112.72(19) ?
C17 N20 C19 . . 104.10(17) ?
C21 N20 H20 . . 110.3(16) ?
C17 N20 H20 . . 109.0(17) ?
C19 N20 H20 . . 106.9(16) ?
N20 C21 H21A . . 109.5 ?
N20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
N20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
O25 C23 O24 . . 125.2(2) ?
O25 C23 C3 . . 117.7(2) ?
O24 C23 C3 . . 117.2(2) ?
H27A O27 H27B . . 109(3) ?
H28A O28 H28B . . 102(4) ?
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
N1 C2 . 1.350(3) ?
N1 C10 . 1.391(3) ?
N1 C11 . 1.463(3) ?
C2 C3 . 1.367(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.437(3) ?
C3 C23 . 1.512(3) ?
C4 O26 . 1.261(3) ?
C4 C5 . 1.450(3) ?
C5 C10 . 1.410(3) ?
C5 C6 . 1.410(3) ?
C6 C7 . 1.348(3) ?
C6 H6 . 0.9500 ?
C7 F22 . 1.360(2) ?
C7 C8 . 1.423(3) ?
C8 N14 . 1.368(3) ?
C8 C9 . 1.396(3) ?
C9 C10 . 1.392(3) ?
C9 H9 . 0.9500 ?
C11 C12 . 1.488(3) ?
C11 C13 . 1.498(4) ?
C11 H11 . 1.0000 ?
C12 C13 . 1.505(4) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
N14 C15 . 1.470(3) ?
N14 C18 . 1.490(3) ?
C15 C19 . 1.526(3) ?
C15 C16 . 1.525(3) ?
C15 H15 . 1.0000 ?
C16 C17 . 1.520(3) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 N20 . 1.516(3) ?
C17 C18 . 1.531(3) ?
C17 H17 . 1.0000 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 N20 . 1.529(3) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
N20 C21 . 1.483(3) ?
N20 H20 . 0.92(3) ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C23 O25 . 1.246(3) ?
C23 O24 . 1.259(3) ?
O27 H27A . 0.837(13) ?
O27 H27B . 0.838(12) ?
O28 H28A . 0.85(5) ?
O28 H28B . 0.81(4) ?
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
N20 H20 O26 4_456 0.92(3) 1.92(3) 2.754(3) 150(2) yes
N20 H20 O25 4_456 0.92(3) 2.20(2) 2.782(3) 121(2) yes
O27 H27A O26 . 0.837(13) 1.980(16) 2.805(2) 169(4) yes
O27 H27B O24 3_646 0.838(12) 2.100(14) 2.929(3) 170(3) yes
O28 H28A O24 . 0.85(5) 1.99(5) 2.832(3) 167(4) yes
O28 H28B O27 1_565 0.81(4) 2.09(4) 2.900(3) 179(4) 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
C10 N1 C2 C3 . . . . 2.3(4) ?
C11 N1 C2 C3 . . . . -177.3(2) ?
N1 C2 C3 C4 . . . . -2.1(4) ?
N1 C2 C3 C23 . . . . 178.7(2) ?
C2 C3 C4 O26 . . . . 176.9(2) ?
C23 C3 C4 O26 . . . . -4.0(4) ?
C2 C3 C4 C5 . . . . -2.2(3) ?
C23 C3 C4 C5 . . . . 177.0(2) ?
O26 C4 C5 C10 . . . . -172.7(2) ?
C3 C4 C5 C10 . . . . 6.4(3) ?
O26 C4 C5 C6 . . . . 4.1(3) ?
C3 C4 C5 C6 . . . . -176.8(2) ?
C10 C5 C6 C7 . . . . 1.8(3) ?
C4 C5 C6 C7 . . . . -175.2(2) ?
C5 C6 C7 F22 . . . . 178.1(2) ?
C5 C6 C7 C8 . . . . 1.9(4) ?
C6 C7 C8 N14 . . . . 171.3(2) ?
F22 C7 C8 N14 . . . . -5.0(3) ?
C6 C7 C8 C9 . . . . -3.9(4) ?
F22 C7 C8 C9 . . . . 179.8(2) ?
N14 C8 C9 C10 . . . . -172.8(2) ?
C7 C8 C9 C10 . . . . 2.3(4) ?
C2 N1 C10 C9 . . . . -178.0(2) ?
C11 N1 C10 C9 . . . . 1.7(3) ?
C2 N1 C10 C5 . . . . 1.9(3) ?
C11 N1 C10 C5 . . . . -178.4(2) ?
C8 C9 C10 N1 . . . . -178.9(2) ?
C8 C9 C10 C5 . . . . 1.2(4) ?
C6 C5 C10 N1 . . . . 176.8(2) ?
C4 C5 C10 N1 . . . . -6.3(3) ?
C6 C5 C10 C9 . . . . -3.3(3) ?
C4 C5 C10 C9 . . . . 173.6(2) ?
C2 N1 C11 C12 . . . . -29.2(3) ?
C10 N1 C11 C12 . . . . 151.1(2) ?
C2 N1 C11 C13 . . . . -99.8(3) ?
C10 N1 C11 C13 . . . . 80.5(3) ?
N1 C11 C12 C13 . . . . -107.6(2) ?
N1 C11 C13 C12 . . . . 110.6(2) ?
C9 C8 N14 C15 . . . . 1.1(4) ?
C7 C8 N14 C15 . . . . -173.8(2) ?
C9 C8 N14 C18 . . . . -147.3(2) ?
C7 C8 N14 C18 . . . . 37.8(3) ?
C8 N14 C15 C19 . . . . -82.3(3) ?
C18 N14 C15 C19 . . . . 70.9(2) ?
C8 N14 C15 C16 . . . . 171.3(2) ?
C18 N14 C15 C16 . . . . -35.5(2) ?
N14 C15 C16 C17 . . . . 54.55(19) ?
C19 C15 C16 C17 . . . . -58.06(19) ?
C15 C16 C17 N20 . . . . 55.49(18) ?
C15 C16 C17 C18 . . . . -55.30(19) ?
C8 N14 C18 C17 . . . . 152.3(2) ?
C15 N14 C18 C17 . . . . 0.2(2) ?
N20 C17 C18 N14 . . . . -71.2(2) ?
C16 C17 C18 N14 . . . . 35.5(2) ?
N14 C15 C19 N20 . . . . -67.2(2) ?
C16 C15 C19 N20 . . . . 39.0(2) ?
C16 C17 N20 C21 . . . . 89.4(2) ?
C18 C17 N20 C21 . . . . -163.5(2) ?
C16 C17 N20 C19 . . . . -33.5(2) ?
C18 C17 N20 C19 . . . . 73.7(2) ?
C15 C19 N20 C21 . . . . -126.7(2) ?
C15 C19 N20 C17 . . . . -3.3(2) ?
C2 C3 C23 O25 . . . . -136.5(2) ?
C4 C3 C23 O25 . . . . 44.4(3) ?
C2 C3 C23 O24 . . . . 45.1(3) ?
C4 C3 C23 O24 . . . . -134.1(2) ?
_cod_database_fobs_code 2022693