#------------------------------------------------------------------------------
#$Date: 2022-11-10 03:46:29 +0100 (Thu, 10 Nov 2022) $
#$Revision: 279170 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022694.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_2022694
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 7.1815(2)
_cell_length_b 10.6840(3)
_cell_length_c 23.5104(7)
_cell_measurement_reflns_used 5102
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 74.9670
_cell_measurement_theta_min 3.6660
_cell_volume 1803.89(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0452
_diffrn_reflns_av_unetI/netI 0.0423
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 10288
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.330
_diffrn_reflns_theta_min 3.760
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.945
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.50341
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.449
_exptl_crystal_description needle
_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 0.243
_refine_diff_density_min -0.340
_refine_ls_abs_structure_details
;
Flack x determined using 1277 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.05(14)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.097
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 274
_refine_ls_number_reflns 3612
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.097
_refine_ls_R_factor_all 0.0509
_refine_ls_R_factor_gt 0.0464
_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^)+(0.0787P)^2^+0.4590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1251
_refine_ls_wR_factor_ref 0.1308
_reflns_number_gt 3329
_reflns_number_total 3612
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vp3026sup1.cif
_cod_data_source_block DFX-Cu
_cod_database_code 2022694
_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 0 2 1845.61 75.2199 6
0 0 3 72.7328 13.1144 6
0 0 4 33557.0 1285.52 4
0 0 5 22.6862 28.3424 4
0 0 6 47171.0 1809.55 4
0 0 7 11.6096 32.3453 4
0 0 -7-2.07124 29.9851 1
0 0 -8 19618.1 785.626 1
0 0 8 20713.8 795.204 4
0 0 9-1.71016 32.1948 4
0 0 -9 5.33960 31.0239 1
0 0 10 701.588 64.2406 4
0 0 -10 631.483 57.7353 1
0 0 11 21.8419 36.2013 4
0 0 -11 50.1452 36.8390 1
0 0 12 97230.0 3656.29 4
0 0 -12 93517.0 3645.49 1
0 0 13-5.45997 37.0336 4
0 0 14 7151.72 336.229 4
0 0 15 3.93828 41.5259 14
0 0 15 6.48282 35.1465 4
0 0 16 1804.32 130.383 4
0 0 16 1693.67 114.362 14
0 0 17 37.0499 48.4765 14
0 0 19-52.3773 60.7109 14
0 0 19-67.4787 91.4834 15
0 0 20 3157.47 182.757 14
0 0 20 3117.38 272.093 15
0 0 21 39.1258 64.9510 14
0 0 21-39.2676 88.7797 15
0 0 22 715.747 87.1145 14
0 0 22 492.078 136.567 15
0 0 23 26.3762 61.2097 14
0 0 23 19.5961 81.8984 15
0 0 24-17.3028 61.8147 14
0 0 25-38.1499 57.4948 14
0 0 26 372.787 61.5344 14
0 0 27 24.5328 34.9391 17
0 0 27-13.3708 43.9059 14
0 0 28 7944.50 328.856 17
0 0 29 7.64075 20.9703 17
0 -1 0-2.48199 24.0756 5
0 -1 -1 73113.6 2775.92 1
0 -1 -2 52242.6 1990.55 1
0 -1 -3 23383.5 903.313 1
0 -1 -4 3211.43 155.700 1
0 -1 4 3782.32 157.787 4
0 -1 5 9184.06 348.506 4
0 -1 -5 7736.92 344.464 1
0 -1 -6 3320.43 169.263 1
0 -1 6 4081.39 174.188 4
0 1 -7 1005.30 54.8430 1
0 -1 -7 1107.52 77.2098 1
0 -1 8 1126.40 78.1138 4
0 1 -8 909.319 52.6874 1
0 -1 -8 986.753 74.8623 1
0 1 9 3491.16 167.251 4
0 -1 -9 3329.29 167.932 1
0 -1 9 3734.95 173.599 4
0 1 -9 3159.83 145.213 1
0 1 10 10317.6 428.340 4
0 -1 10 10776.1 435.012 4
0 -1 -10 9937.98 428.997 1
0 1 -10 9818.35 404.920 1
0 -1 11 7610.63 342.372 4
0 -1 -11 7365.47 339.854 1
0 1 11 7945.06 340.197 4
0 -1 12 5697.91 268.304 4
0 -1 -12 5327.83 265.384 1
0 1 12 5633.99 264.091 4
0 -1 -13 149.471 52.7247 1
0 1 13 101.741 41.7469 4
0 1 14 4701.51 240.269 4
0 1 15 246.125 55.5749 4
0 -1 15 244.882 51.2533 14
0 1 15 278.943 52.6485 14
0 1 16 37.8031 39.1613 4
0 1 16 40.2981 44.8595 14
0 -1 16 100.150 50.7201 14
0 1 17 1978.57 140.303 4
0 -1 17 1751.48 122.590 14
0 1 17 1956.99 125.880 14
0 -1 18 130.317 97.7460 15
0 -1 18 132.331 58.7126 14
0 1 18 174.641 56.5895 14
0 1 18 182.919 51.9319 4
0 1 19 3400.40 189.217 14
0 -1 19 3461.78 191.972 14
0 1 20 1481.96 181.427 15
0 -1 20 1483.25 198.182 15
0 -1 20 1543.34 121.929 14
0 1 20 1720.61 122.815 14
0 1 21-8.99589 82.1976 15
0 -1 21-2.78758 61.4280 14
0 1 21-21.6894 60.2662 14
0 -1 21 70.5751 93.0583 15
0 -1 22 374.859 79.4460 14
0 1 22 338.882 111.554 15
0 1 22 444.351 79.4119 14
0 -1 22 343.564 120.912 15
0 -1 23 189.296 98.0507 15
0 -1 23 100.845 64.5566 14
0 1 23-86.9015 96.0064 15
0 1 23 46.8899 59.5119 14
0 1 24 343.767 67.6954 14
0 1 25 41.8180 54.8991 14
0 -1 25 17.8118 55.9146 14
0 -1 26 963.062 75.3595 17
0 -1 26 1139.08 91.8073 14
0 1 26 1098.78 88.8654 14
0 -1 27 160.061 37.4389 17
0 1 27 238.277 49.9263 14
0 1 28 637.991 54.6628 17
0 -1 28 480.853 45.3893 17
0 1 28 650.439 57.3941 14
0 1 29 21.2422 22.5946 17
0 -1 29 20.7852 20.2231 10
0 -2 0 23803.6 930.847 1
0 -2 0 24879.9 954.328 5
0 -2 -1 20491.1 815.321 5
0 -2 -3 32484.8 1257.84 1
0 -2 -4 1062.14 74.9947 1
0 -2 -5 2313.00 124.529 1
0 -2 -6 3353.42 167.548 1
0 -2 -7 31136.6 1222.44 1
0 -2 -8 127.008 48.8856 1
0 -2 -9 68796.1 2656.56 1
0 -2 -10 14791.2 619.818 1
0 -2 -11 14382.0 610.892 1
0 2 12 1362.70 101.861 4
0 -2 -12 1292.73 110.765 1
0 2 13 15358.2 657.911 4
0 -2 -13 16165.9 677.313 1
0 2 14 1027.73 91.7731 4
0 -2 14 944.256 80.8965 14
0 2 15 7287.67 353.852 4
0 -2 15 7752.26 335.664 14
0 2 16 698.296 80.3428 4
0 -2 16 770.068 77.2100 14
0 2 16 745.617 75.8542 14
0 -2 16 730.831 59.7819 21
0 2 17 5287.51 278.630 4
0 2 17 5538.56 258.275 14
0 -2 17 5470.82 259.585 14
0 -2 17 5232.38 236.486 21
0 -2 18-21.1022 35.3063 21
0 -2 18 7.69262 53.3446 14
0 -2 18 9.29470 89.1559 15
0 2 18 24.3794 51.2146 14
0 2 18 26.1268 36.4592 4
0 -2 19 462.770 76.8935 14
0 2 19 496.693 74.6577 14
0 -2 19 523.500 134.627 15
0 2 20 6526.13 306.704 14
0 -2 20 5687.35 429.028 15
0 -2 20 6618.74 310.591 14
0 -2 21 830.773 80.1246 13
0 -2 21 1083.23 105.619 14
0 -2 21 1200.19 184.062 15
0 2 21 1275.53 107.224 14
0 2 22 1427.43 185.185 15
0 2 22 1938.19 130.824 14
0 -2 22 1717.87 220.657 15
0 -2 22 1668.05 129.491 14
0 -2 23 576.159 82.9325 14
0 2 23 507.315 77.7866 14
0 2 24 1399.36 106.443 14
0 -2 24 1213.92 105.705 14
0 -2 24 1196.37 87.6869 17
0 -2 25 115.469 56.3560 14
0 2 25 88.2767 54.2602 14
0 -2 25 55.5937 38.1184 17
0 2 26 103.684 51.1223 14
0 -2 26 126.316 37.1308 17
0 -2 27-4.85513 15.8828 17
0 2 28 2.28765 31.9535 14
0 -2 28-9.54297 23.0036 10
0 2 29 405.044 37.5534 17
0 -3 0 29.9438 35.4096 1
0 -3 0 59.7832 63.8519 5
0 -3 -1 9650.27 407.855 1
0 -3 -1 10448.3 436.306 5
0 -3 -2 17994.3 740.930 5
0 -3 -3 15922.1 663.033 5
0 -3 -4 11418.2 500.239 1
0 -3 4 13826.2 554.641 15
0 -3 -5 14218.8 586.371 1
0 -3 -6 9769.36 422.017 1
0 -3 -7 327.026 62.1180 1
0 -3 -8 20587.1 842.633 1
0 -3 -9 26200.9 1061.23 1
0 -3 -10 6.58636 52.1190 1
0 -3 -11 17.9446 52.7980 1
0 -3 -12 1267.31 120.409 1
0 -3 -13 534.125 88.4404 1
0 3 14 399.515 65.4110 4
0 -3 14 369.899 47.0605 21
0 3 15 1447.26 115.465 4
0 -3 15 1272.60 85.2160 21
0 3 16-3.70596 41.3378 4
0 -3 16 42.8915 37.3896 21
0 3 17 5794.83 281.624 14
0 -3 17 6043.77 266.608 21
0 3 17 6121.02 308.710 4
0 -3 17 6441.58 424.240 15
0 -3 18 278.089 118.090 15
0 3 18 258.098 64.5960 14
0 -3 18 279.864 49.9701 21
0 -3 19 6667.51 280.368 21
0 -3 19 5487.60 424.855 15
0 -3 19 5727.17 279.784 13
0 3 19 6676.07 299.771 14
0 3 20 52.3171 60.2609 14
0 -3 20 64.1709 40.1836 21
0 -3 20 67.4691 49.7102 13
0 -3 20 46.5154 104.091 15
0 3 21 1270.64 104.566 14
0 -3 21 1190.83 82.2021 21
0 -3 21 1220.32 108.622 14
0 -3 21 979.649 188.460 15
0 -3 21 937.051 86.4126 13
0 -3 22 64.7671 45.6822 13
0 3 22 110.443 59.5107 14
0 -3 22 49.8621 38.3932 17
0 -3 22 151.708 104.478 15
0 -3 22 160.294 67.8244 14
0 -3 23 427.384 77.3138 14
0 -3 23 362.064 52.1394 17
0 3 23 449.765 72.0494 14
0 -3 24 1253.07 87.6705 17
0 3 24 1843.83 115.088 14
0 3 25 1065.38 77.4304 14
0 -3 25 4.83674 17.3334 17
0 -3 26 102.313 37.0796 10
0 3 26 245.162 49.0418 14
0 3 27-11.5311 34.6001 14
0 -3 27 15.6253 23.8495 10
0 3 28 731.138 55.2723 17
0 3 28 754.885 52.7236 14
0 3 29 49.7414 19.7231 17
0 -4 0 179.359 83.9048 5
0 -4 -1 56256.5 2207.88 5
0 -4 -2 5896.22 279.721 1
0 -4 -2 6123.85 309.884 5
0 -4 2 6160.41 256.153 2
0 -4 2 6559.66 345.135 15
0 -4 -3 362.893 86.6461 5
0 -4 3 417.000 48.2377 2
0 -4 3 521.940 112.684 15
0 -4 4 4895.57 293.437 15
0 -4 4 4742.85 206.293 2
0 -4 -4 4975.73 268.969 5
0 -4 -5 3724.25 227.586 5
0 -4 -6 427.740 94.0325 5
0 -4 -6 307.276 68.5225 1
0 -4 -7 7249.92 346.993 1
0 -4 -8 4941.96 263.168 1
0 -4 -9 1015.23 111.439 1
0 -4 -10 212.066 72.8479 1
0 -4 -11 4793.88 272.267 1
0 -4 12 788.656 76.2703 14
0 -4 12 828.251 65.3833 21
0 -4 13 11280.3 448.118 14
0 -4 13 10241.4 431.785 13
0 -4 13 10229.8 430.526 21
0 -4 13 10259.2 419.734 16
0 -4 14 361.203 53.6222 21
0 -4 14 466.871 66.8665 14
0 -4 14 385.016 58.1079 13
0 -4 15 4262.60 186.750 16
0 4 15 3972.13 236.483 4
0 -4 15 3929.24 199.301 13
0 -4 15 4279.25 199.301 21
0 -4 15 4250.50 214.630 14
0 -4 16 6749.38 291.483 21
0 -4 16 6066.13 290.826 13
0 -4 16 6320.98 443.751 15
0 -4 16 6696.14 278.174 16
0 4 16 6844.57 338.242 4
0 -4 17 233.008 59.8634 13
0 -4 17 355.963 56.0613 21
0 4 17 263.860 60.8775 4
0 -4 17 224.847 127.539 15
0 4 18 157.891 59.2749 14
0 -4 18 71.5842 113.532 15
0 -4 18 152.854 49.9114 21
0 -4 18 184.119 57.6867 13
0 -4 19 6102.06 292.987 13
0 -4 19 6938.96 295.261 21
0 -4 19 6109.41 469.209 15
0 4 19 6652.07 307.812 14
0 -4 20 993.327 79.8711 21
0 -4 20 698.954 78.7134 13
0 4 20 944.053 93.4968 14
0 -4 20 709.233 172.476 15
0 -4 21 51.5670 44.7246 21
0 4 21 80.1631 57.3508 14
0 -4 21 83.8293 53.9751 13
0 -4 21 50.0135 104.536 15
0 -4 22 755.490 67.6752 21
0 4 22 816.984 83.3646 14
0 -4 22 568.174 69.3724 13
0 -4 23 351.208 51.3917 10
0 -4 23 270.243 46.9962 21
0 4 24 748.214 74.7552 14
0 -4 24 553.843 58.2909 10
0 4 25 1740.79 99.8255 14
0 -4 25 1166.42 77.9445 10
0 4 26 230.957 42.7711 14
0 4 28 123.111 26.1494 17
0 -5 0 37.3723 41.5394 2
0 -5 -1 125.659 85.7959 5
0 -5 -1 70.9325 44.1691 2
0 -5 1 143.238 45.9416 2
0 -5 -2 28884.8 1151.05 5
0 -5 2 27150.9 1069.01 2
0 -5 3 20143.3 793.231 2
0 -5 3 20296.6 910.026 15
0 -5 -3 20243.6 871.336 5
0 -5 -4 11399.5 516.199 5
0 -5 4 10378.2 431.382 2
0 -5 5 7495.08 319.017 2
0 -5 -5 7836.02 401.305 5
0 -5 -6 980.561 137.829 5
0 -5 -7 712.403 97.8173 1
0 -5 -8 338.919 102.283 5
0 -5 -9 2995.91 230.561 5
0 -5 10 30810.0 1126.95 13
0 -5 10 27860.4 1111.82 16
0 -5 -10 26135.4 1134.07 12
0 -5 10 29040.0 1122.51 21
0 -5 11 3079.40 149.186 16
0 -5 11 3437.93 164.520 13
0 -5 11 3227.69 160.233 21
0 -5 12 4299.35 198.978 9
0 -5 12 4577.91 211.554 13
0 -5 12 4325.50 208.477 21
0 -5 12 4411.90 195.487 16
0 -5 13 21.6096 42.7996 9
0 -5 13 41.9949 50.3446 13
0 -5 13 34.4668 29.0252 16
0 -5 13 14.6082 41.5725 21
0 -5 14 2717.57 150.183 13
0 -5 14 2998.58 150.753 21
0 -5 14 2569.38 137.106 9
0 -5 15 2983.39 142.044 16
0 -5 15 2885.45 155.618 21
0 -5 15 2580.57 289.536 15
0 -5 15 2638.36 155.195 13
0 -5 16 185.889 125.556 15
0 -5 16 214.670 60.5048 13
0 -5 16 229.029 57.5637 21
0 -5 16 209.918 42.2444 16
0 5 16 196.237 63.8829 4
0 -5 17 425.127 147.384 15
0 -5 17 310.475 68.9475 13
0 -5 17 479.437 64.9134 21
0 -5 18 430.522 74.4443 13
0 -5 18 427.996 58.9415 10
0 -5 18 537.488 163.478 15
0 5 18 584.102 75.9676 14
0 -5 -18 437.557 133.772 5
0 -5 18 661.749 71.7913 21
0 -5 19 1425.91 99.3319 21
0 5 19 1272.86 104.037 14
0 -5 19 1099.52 86.8913 10
0 -5 19 1118.74 100.745 13
0 -5 19 1391.31 221.469 15
0 -5 -19 969.379 173.662 5
0 5 20 564.950 73.1198 14
0 -5 20 377.271 55.4265 10
0 -5 20 504.680 66.2341 21
0 -5 20 342.483 139.649 15
0 -5 20 409.034 72.1332 13
0 -5 -20 467.888 130.391 5
0 -5 21 509.720 59.7314 10
0 -5 21 779.674 72.7683 21
0 5 21 795.750 82.4115 14
0 -5 21 674.443 77.2420 13
0 -5 22 396.995 65.1883 13
0 5 22 671.771 74.6581 14
0 -5 22 742.560 67.2338 21
0 -5 22 484.185 54.0375 10
0 -5 23 211.702 43.6520 21
0 5 24 179.306 47.4468 14
0 5 25 1218.65 78.8773 14
0 5 26 524.165 45.2900 14
0 5 27 836.947 53.8358 17
0 -6 0 7933.31 337.067 2
0 -6 1 1558.81 98.3915 2
0 -6 -1 1450.32 95.4327 2
0 -6 2 365.547 57.0391 2
0 -6 -2 385.030 57.5194 2
0 -6 -3 425.449 59.4852 2
0 -6 3 431.962 59.4971 2
0 -6 -3 366.426 102.700 5
0 -6 -4 12.5981 86.6368 5
0 -6 4 42.3264 47.6765 2
0 -6 -5 144.912 92.8066 5
0 -6 5 168.028 53.9402 2
0 -6 -6 293.130 103.981 5
0 -6 -7 2015.63 195.061 5
0 -6 7 1799.69 114.600 13
0 -6 7 1758.05 104.581 21
0 -6 7 1715.17 101.737 9
0 -6 8 80.1928 41.4195 21
0 -6 8 42.8958 42.7837 9
0 -6 8 41.7982 54.7155 13
0 -6 8 54.6015 30.8092 16
0 -6 -8-67.2107 97.0087 5
0 -6 9 4524.82 202.722 16
0 -6 9 4613.29 209.790 9
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8 -5 -7 65.4681 22.2734 8
-8 -5 7 14.9793 28.0717 11
8 -5 -8 24.7820 18.7645 8
8 -6 5 35.8989 13.7779 16
8 -6 4 207.617 21.6042 16
8 -6 2 14.3537 16.0963 16
8 -6 1 1035.24 52.0578 16
-8 -6 -1 946.128 62.1080 12
8 -6 0 599.771 38.2456 16
-8 -6 0 953.631 57.8675 12
8 -6 -1 922.422 47.1345 16
9 0 0 31.9820 14.3674 16
9 0 -1 64.5020 15.6078 16
9 0 -2 107.657 17.7525 16
9 0 -3 8.88336 14.0390 16
9 -1 1 157.632 20.4415 16
9 -1 0 1276.35 60.6551 16
9 -1 -1 253.120 25.6525 16
9 -1 -2 277.434 24.2771 16
9 -1 -3 166.775 18.7958 16
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 3668
_shelx_res_file
;
TITL danofloxacin-Cu
shelx.res
created by SHELXL-2018/3 at 14:40:55 on 05-Oct-2022
CELL 1.54184 7.1815 10.6840 23.5104 90.000 90.000 90.000
ZERR 4.00 0.0002 0.0003 0.0007 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 -6 7 5
OMIT -4 10 10
OMIT 2 0 20
OMIT 2 9 18
OMIT 4 3 23
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. 4
TEMP -173.00
WGHT 0.078700 0.459000
FVAR 2.97561
N1 4 0.625394 0.531750 0.512298 11.00000 0.02840 0.01843 =
0.02614 0.00104 0.00104 0.00022
C2 1 0.617700 0.569440 0.567134 11.00000 0.02620 0.02221 =
0.02774 -0.00153 0.00035 -0.00021
AFIX 43
H2 2 0.599820 0.656095 0.574361 11.00000 -1.20000
AFIX 0
C3 1 0.633879 0.491439 0.612773 11.00000 0.02574 0.01967 =
0.02769 -0.00221 0.00189 0.00031
C4 1 0.655308 0.358874 0.603774 11.00000 0.02034 0.02054 =
0.02867 0.00130 -0.00140 -0.00115
C5 1 0.649859 0.318944 0.544853 11.00000 0.02418 0.01896 =
0.02521 0.00017 -0.00135 -0.00052
C6 1 0.659793 0.190724 0.531104 11.00000 0.02497 0.01964 =
0.02850 0.00158 -0.00068 0.00020
AFIX 43
H6 2 0.659942 0.129849 0.560557 11.00000 -1.20000
AFIX 0
C7 1 0.669061 0.154269 0.476435 11.00000 0.02676 0.01312 =
0.03223 -0.00057 -0.00297 0.00176
C8 1 0.675562 0.238241 0.429877 11.00000 0.02048 0.02036 =
0.02687 0.00235 -0.00078 0.00094
C9 1 0.659372 0.365454 0.443139 11.00000 0.02306 0.02323 =
0.02938 0.00025 -0.00047 -0.00020
AFIX 43
H9 2 0.658102 0.425605 0.413382 11.00000 -1.20000
AFIX 0
C10 1 0.645046 0.405121 0.499611 11.00000 0.02261 0.01814 =
0.02697 -0.00084 -0.00014 -0.00097
C11 1 0.615276 0.620606 0.464790 11.00000 0.03494 0.01916 =
0.02638 0.00256 0.00094 -0.00056
AFIX 13
H11 2 0.728499 0.624941 0.440109 11.00000 -1.20000
AFIX 0
C12 1 0.510646 0.739747 0.471306 11.00000 0.04018 0.02497 =
0.03443 0.00144 0.00218 0.00530
AFIX 23
H12A 2 0.560349 0.814993 0.451982 11.00000 -1.20000
H12B 2 0.449241 0.755999 0.508276 11.00000 -1.20000
AFIX 0
C13 1 0.433432 0.636652 0.434775 11.00000 0.03467 0.02457 =
0.03872 0.00562 -0.00337 -0.00095
AFIX 23
H13A 2 0.324828 0.589415 0.449329 11.00000 -1.20000
H13B 2 0.435975 0.648430 0.393015 11.00000 -1.20000
AFIX 0
N14 4 0.709402 0.197281 0.375738 11.00000 0.02871 0.01876 =
0.02406 -0.00022 -0.00047 -0.00131
C15 1 0.734248 0.284802 0.328163 11.00000 0.02634 0.02033 =
0.02437 -0.00032 0.00061 -0.00222
AFIX 13
H15 2 0.821823 0.355452 0.336088 11.00000 -1.20000
AFIX 0
C16 1 0.797732 0.196280 0.281034 11.00000 0.02518 0.02369 =
0.02734 -0.00019 0.00079 0.00035
AFIX 23
H16A 2 0.803297 0.236896 0.243224 11.00000 -1.20000
H16B 2 0.917056 0.153966 0.289689 11.00000 -1.20000
AFIX 0
C17 1 0.629706 0.111329 0.288106 11.00000 0.02374 0.01884 =
0.03095 -0.00353 0.00253 0.00137
AFIX 13
H17 2 0.626496 0.037881 0.261759 11.00000 -1.20000
AFIX 0
C18 1 0.637522 0.078126 0.350858 11.00000 0.02618 0.01763 =
0.03083 -0.00276 -0.00138 -0.00055
AFIX 23
H18A 2 0.512655 0.057052 0.365913 11.00000 -1.20000
H18B 2 0.723614 0.007506 0.358047 11.00000 -1.20000
AFIX 0
C19 1 0.544089 0.324939 0.305999 11.00000 0.02731 0.01947 =
0.02985 -0.00132 0.00298 0.00148
AFIX 23
H19A 2 0.463229 0.355204 0.337206 11.00000 -1.20000
H19B 2 0.555539 0.391210 0.276776 11.00000 -1.20000
AFIX 0
N20 4 0.470061 0.203851 0.280549 11.00000 0.02448 0.02162 =
0.02798 -0.00150 0.00024 -0.00050
C21 1 0.408274 0.217501 0.220459 11.00000 0.03347 0.02882 =
0.02897 -0.00064 0.00016 -0.00039
AFIX 137
H21A 2 0.513645 0.244480 0.196981 11.00000 -1.50000
H21B 2 0.308762 0.280087 0.218309 11.00000 -1.50000
H21C 2 0.361719 0.136925 0.206512 11.00000 -1.50000
AFIX 0
F22 3 0.683931 0.029492 0.464370 11.00000 0.04505 0.01492 =
0.03071 -0.00228 -0.00146 0.00243
C23 1 0.626543 0.545835 0.672407 11.00000 0.02629 0.01964 =
0.02790 -0.00095 -0.00001 -0.00241
O24 5 0.501159 0.625715 0.682543 11.00000 0.03253 0.02950 =
0.03270 -0.00663 -0.00167 0.00742
O25 5 0.742088 0.506230 0.707672 11.00000 0.04010 0.02936 =
0.03072 -0.00322 -0.00642 0.00690
O26 5 0.678127 0.280831 0.643332 11.00000 0.02811 0.02256 =
0.02633 0.00067 -0.00152 -0.00053
O27 5 0.618340 0.055966 0.702653 11.00000 0.03438 0.02907 =
0.03605 0.00649 0.00226 0.00337
O28 5 0.459260 0.863016 0.630317 11.00000 0.04694 0.04108 =
0.03952 0.00560 -0.00862 -0.00197
H20 2 0.364422 0.179018 0.300950 11.00000 0.02797
H27A 2 0.627389 0.134766 0.683080 11.00000 0.07013
H27B 2 0.565405 0.071162 0.737143 11.00000 0.03786
H28A 2 0.479548 0.797433 0.651528 11.00000 0.05660
H28B 2 0.517326 0.917369 0.654202 11.00000 0.04737
HKLF 4
REM danofloxacin-Cu
REM wR2 = 0.1308, GooF = S = 1.097, Restrained GooF = 1.097 for all data
REM R1 = 0.0464 for 3329 Fo > 4sig(Fo) and 0.0509 for all 3612 data
REM 274 parameters refined using 0 restraints
END
WGHT 0.0786 0.4595
REM Highest difference peak 0.243, deepest hole -0.340, 1-sigma level 0.063
Q1 1 0.4623 0.0575 0.7017 11.00000 0.05 0.24
Q2 1 0.3175 0.8562 0.6168 11.00000 0.05 0.22
Q3 1 0.4886 0.6277 0.7215 11.00000 0.05 0.22
Q4 1 0.4629 0.4976 0.5996 11.00000 0.05 0.21
Q5 1 0.3660 0.6227 0.7111 11.00000 0.05 0.21
;
_shelx_res_checksum 44619
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 0.6254(4) 0.5318(2) 0.51230(11) 0.0243(5) Uani d 1 . .
C C2 0.6177(4) 0.5694(3) 0.56713(13) 0.0254(6) Uani d 1 . .
H H2 0.599820 0.656095 0.574361 0.030 Uiso calc 1 . .
C C3 0.6339(4) 0.4914(3) 0.61277(12) 0.0244(6) Uani d 1 . .
C C4 0.6553(4) 0.3589(3) 0.60377(13) 0.0232(6) Uani d 1 . .
C C5 0.6499(4) 0.3189(3) 0.54485(12) 0.0228(6) Uani d 1 . .
C C6 0.6598(4) 0.1907(3) 0.53110(13) 0.0244(6) Uani d 1 . .
H H6 0.659942 0.129849 0.560557 0.029 Uiso calc 1 . .
C C7 0.6691(4) 0.1543(3) 0.47643(13) 0.0240(6) Uani d 1 . .
C C8 0.6756(4) 0.2382(3) 0.42988(13) 0.0226(6) Uani d 1 . .
C C9 0.6594(4) 0.3655(3) 0.44314(13) 0.0252(6) Uani d 1 . .
H H9 0.658102 0.425605 0.413382 0.030 Uiso calc 1 . .
C C10 0.6450(4) 0.4051(3) 0.49961(13) 0.0226(6) Uani d 1 . .
C C11 0.6153(5) 0.6206(3) 0.46479(14) 0.0268(6) Uani d 1 . .
H H11 0.728499 0.624941 0.440109 0.032 Uiso calc 1 . .
C C12 0.5106(5) 0.7397(3) 0.47131(15) 0.0332(7) Uani d 1 . .
H H12A 0.560349 0.814993 0.451982 0.040 Uiso calc 1 . .
H H12B 0.449241 0.755999 0.508276 0.040 Uiso calc 1 . .
C C13 0.4334(5) 0.6367(3) 0.43477(16) 0.0327(7) Uani d 1 . .
H H13A 0.324828 0.589415 0.449329 0.039 Uiso calc 1 . .
H H13B 0.435975 0.648430 0.393015 0.039 Uiso calc 1 . .
N N14 0.7094(4) 0.1973(2) 0.37574(11) 0.0238(5) Uani d 1 . .
C C15 0.7342(4) 0.2848(3) 0.32816(12) 0.0237(6) Uani d 1 . .
H H15 0.821823 0.355452 0.336088 0.028 Uiso calc 1 . .
C C16 0.7977(4) 0.1963(3) 0.28103(13) 0.0254(6) Uani d 1 . .
H H16A 0.803297 0.236896 0.243224 0.030 Uiso calc 1 . .
H H16B 0.917056 0.153966 0.289689 0.030 Uiso calc 1 . .
C C17 0.6297(4) 0.1113(3) 0.28811(13) 0.0245(6) Uani d 1 . .
H H17 0.626496 0.037881 0.261759 0.029 Uiso calc 1 . .
C C18 0.6375(4) 0.0781(3) 0.35086(13) 0.0249(6) Uani d 1 . .
H H18A 0.512655 0.057052 0.365913 0.030 Uiso calc 1 . .
H H18B 0.723614 0.007506 0.358047 0.030 Uiso calc 1 . .
C C19 0.5441(4) 0.3249(3) 0.30600(14) 0.0255(6) Uani d 1 . .
H H19A 0.463229 0.355204 0.337206 0.031 Uiso calc 1 . .
H H19B 0.555539 0.391210 0.276776 0.031 Uiso calc 1 . .
N N20 0.4701(4) 0.2039(3) 0.28055(11) 0.0247(6) Uani d 1 . .
C C21 0.4083(5) 0.2175(3) 0.22046(13) 0.0304(7) Uani d 1 . .
H H21A 0.513645 0.244480 0.196981 0.046 Uiso calc 1 . .
H H21B 0.308762 0.280087 0.218309 0.046 Uiso calc 1 . .
H H21C 0.361719 0.136925 0.206512 0.046 Uiso calc 1 . .
F F22 0.6839(3) 0.02949(16) 0.46437(8) 0.0302(4) Uani d 1 . .
C C23 0.6265(4) 0.5458(3) 0.67241(13) 0.0246(6) Uani d 1 . .
O O24 0.5012(3) 0.6257(2) 0.68254(9) 0.0316(5) Uani d 1 . .
O O25 0.7421(3) 0.5062(2) 0.70767(10) 0.0334(5) Uani d 1 . .
O O26 0.6781(3) 0.2808(2) 0.64333(9) 0.0257(5) Uani d 1 . .
O O27 0.6183(3) 0.0560(2) 0.70265(11) 0.0332(5) Uani d 1 . .
O O28 0.4593(4) 0.8630(3) 0.63032(12) 0.0425(6) Uani d 1 . .
H H20 0.364(6) 0.179(4) 0.3010(16) 0.028(9) Uiso d 1 . .
H H27A 0.627(8) 0.135(6) 0.683(2) 0.070(17) Uiso d 1 . .
H H27B 0.565(6) 0.071(4) 0.7371(19) 0.038(11) Uiso d 1 . .
H H28A 0.480(7) 0.797(6) 0.652(2) 0.057(15) Uiso d 1 . .
H H28B 0.517(7) 0.917(5) 0.654(2) 0.047(13) 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 0.0284(12) 0.0184(13) 0.0261(12) 0.0002(11) 0.0010(10) 0.0010(10)
C2 0.0262(14) 0.0222(15) 0.0277(14) -0.0002(12) 0.0003(12) -0.0015(12)
C3 0.0257(14) 0.0197(14) 0.0277(14) 0.0003(12) 0.0019(12) -0.0022(11)
C4 0.0203(13) 0.0205(14) 0.0287(14) -0.0012(12) -0.0014(11) 0.0013(12)
C5 0.0242(14) 0.0190(14) 0.0252(14) -0.0005(12) -0.0014(11) 0.0002(11)
C6 0.0250(14) 0.0196(14) 0.0285(14) 0.0002(12) -0.0007(12) 0.0016(12)
C7 0.0268(14) 0.0131(13) 0.0322(15) 0.0018(11) -0.0030(12) -0.0006(11)
C8 0.0205(13) 0.0204(14) 0.0269(14) 0.0009(11) -0.0008(11) 0.0024(11)
C9 0.0231(14) 0.0232(15) 0.0294(15) -0.0002(12) -0.0005(11) 0.0003(12)
C10 0.0226(13) 0.0181(14) 0.0270(15) -0.0010(11) -0.0001(11) -0.0008(11)
C11 0.0349(16) 0.0192(15) 0.0264(14) -0.0006(13) 0.0009(13) 0.0026(12)
C12 0.0402(18) 0.0250(17) 0.0344(16) 0.0053(14) 0.0022(15) 0.0014(13)
C13 0.0347(17) 0.0246(17) 0.0387(17) -0.0009(14) -0.0034(14) 0.0056(14)
N14 0.0287(13) 0.0188(12) 0.0241(12) -0.0013(10) -0.0005(10) -0.0002(10)
C15 0.0263(14) 0.0203(14) 0.0244(14) -0.0022(12) 0.0006(11) -0.0003(12)
C16 0.0252(14) 0.0237(15) 0.0273(15) 0.0004(12) 0.0008(11) -0.0002(12)
C17 0.0237(14) 0.0188(14) 0.0310(15) 0.0014(12) 0.0025(12) -0.0035(12)
C18 0.0262(13) 0.0176(15) 0.0308(15) -0.0006(12) -0.0014(12) -0.0028(11)
C19 0.0273(15) 0.0195(15) 0.0299(15) 0.0015(12) 0.0030(12) -0.0013(11)
N20 0.0245(13) 0.0216(13) 0.0280(13) -0.0005(11) 0.0002(10) -0.0015(10)
C21 0.0335(17) 0.0288(17) 0.0290(16) -0.0004(14) 0.0002(13) -0.0006(13)
F22 0.0451(11) 0.0149(9) 0.0307(9) 0.0024(8) -0.0015(8) -0.0023(7)
C23 0.0263(14) 0.0196(14) 0.0279(14) -0.0024(12) 0.0000(12) -0.0010(12)
O24 0.0325(12) 0.0295(12) 0.0327(11) 0.0074(10) -0.0017(9) -0.0066(9)
O25 0.0401(13) 0.0294(12) 0.0307(11) 0.0069(10) -0.0064(10) -0.0032(10)
O26 0.0281(11) 0.0226(11) 0.0263(10) -0.0005(9) -0.0015(8) 0.0007(8)
O27 0.0344(12) 0.0291(12) 0.0360(13) 0.0034(10) 0.0023(10) 0.0065(10)
O28 0.0469(15) 0.0411(15) 0.0395(14) -0.0020(13) -0.0086(12) 0.0056(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
0 -5 10 0.0198
4 0 9 0.1079
-5 0 0 0.1245
-1 6 -7 0.0363
1 -1 -15 0.0517
0 5 -11 0.0349
0 6 -7 0.0384
-5 -1 1 0.1247
-1 6 -6 0.0399
0 -7 4 0.0258
1 2 2 0.1180
1 -5 -9 0.0595
-1 0 -2 0.1152
0 -1 15 0.0111
-1 6 -9 0.0347
0 -6 7 0.0231
4 2 -2 0.1313
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 . . 119.9(3) ?
C2 N1 C11 . . 122.1(3) ?
C10 N1 C11 . . 118.1(3) ?
N1 C2 C3 . . 124.4(3) ?
N1 C2 H2 . . 117.8 ?
C3 C2 H2 . . 117.8 ?
C2 C3 C4 . . 119.6(3) ?
C2 C3 C23 . . 119.3(3) ?
C4 C3 C23 . . 121.0(3) ?
O26 C4 C3 . . 123.8(3) ?
O26 C4 C5 . . 120.9(3) ?
C3 C4 C5 . . 115.3(3) ?
C10 C5 C6 . . 117.6(3) ?
C10 C5 C4 . . 122.0(3) ?
C6 C5 C4 . . 120.2(3) ?
C7 C6 C5 . . 120.2(3) ?
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C6 C7 F22 . . 119.0(3) ?
C6 C7 C8 . . 123.8(3) ?
F22 C7 C8 . . 117.1(3) ?
N14 C8 C9 . . 122.2(3) ?
N14 C8 C7 . . 121.5(3) ?
C9 C8 C7 . . 116.1(3) ?
C10 C9 C8 . . 120.8(3) ?
C10 C9 H9 . . 119.6 ?
C8 C9 H9 . . 119.6 ?
N1 C10 C9 . . 120.4(3) ?
N1 C10 C5 . . 118.4(3) ?
C9 C10 C5 . . 121.2(3) ?
N1 C11 C12 . . 120.0(3) ?
N1 C11 C13 . . 118.5(3) ?
C12 C11 C13 . . 60.6(2) ?
N1 C11 H11 . . 115.5 ?
C12 C11 H11 . . 115.5 ?
C13 C11 H11 . . 115.5 ?
C11 C12 C13 . . 60.0(2) ?
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 . . 59.4(2) ?
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 . . 121.8(2) ?
C8 N14 C18 . . 125.2(3) ?
C15 N14 C18 . . 106.6(2) ?
N14 C15 C19 . . 109.3(2) ?
N14 C15 C16 . . 101.2(2) ?
C19 C15 C16 . . 101.2(2) ?
N14 C15 H15 . . 114.5 ?
C19 C15 H15 . . 114.5 ?
C16 C15 H15 . . 114.5 ?
C17 C16 C15 . . 93.1(2) ?
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 ?
C18 C17 C16 . . 102.5(2) ?
C18 C17 N20 . . 107.0(2) ?
C16 C17 N20 . . 101.4(2) ?
C18 C17 H17 . . 114.8 ?
C16 C17 H17 . . 114.8 ?
N20 C17 H17 . . 114.8 ?
N14 C18 C17 . . 101.2(2) ?
N14 C18 H18A . . 111.5 ?
C17 C18 H18A . . 111.5 ?
N14 C18 H18B . . 111.5 ?
C17 C18 H18B . . 111.5 ?
H18A C18 H18B . . 109.3 ?
N20 C19 C15 . . 102.0(2) ?
N20 C19 H19A . . 111.4 ?
C15 C19 H19A . . 111.4 ?
N20 C19 H19B . . 111.4 ?
C15 C19 H19B . . 111.4 ?
H19A C19 H19B . . 109.2 ?
C21 N20 C19 . . 113.2(3) ?
C21 N20 C17 . . 113.5(2) ?
C19 N20 C17 . . 104.1(2) ?
C21 N20 H20 . . 106(2) ?
C19 N20 H20 . . 109(2) ?
C17 N20 H20 . . 111(2) ?
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 . . 125.3(3) ?
O25 C23 C3 . . 117.4(3) ?
O24 C23 C3 . . 117.2(3) ?
H27A O27 H27B . . 107(4) ?
H28A O28 H28B . . 95(5) ?
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 . 1.352(4) ?
N1 C10 . 1.393(4) ?
N1 C11 . 1.468(4) ?
C2 C3 . 1.364(4) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.440(4) ?
C3 C23 . 1.519(4) ?
C4 O26 . 1.260(4) ?
C4 C5 . 1.450(4) ?
C5 C10 . 1.407(4) ?
C5 C6 . 1.409(4) ?
C6 C7 . 1.345(4) ?
C6 H6 . 0.9500 ?
C7 F22 . 1.367(3) ?
C7 C8 . 1.416(4) ?
C8 N14 . 1.368(4) ?
C8 C9 . 1.399(4) ?
C9 C10 . 1.397(4) ?
C9 H9 . 0.9500 ?
C11 C12 . 1.486(5) ?
C11 C13 . 1.494(5) ?
C11 H11 . 1.0000 ?
C12 C13 . 1.503(5) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
N14 C15 . 1.469(4) ?
N14 C18 . 1.493(4) ?
C15 C19 . 1.523(4) ?
C15 C16 . 1.526(4) ?
C15 H15 . 1.0000 ?
C16 C17 . 1.519(4) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 C18 . 1.518(4) ?
C17 N20 . 1.524(4) ?
C17 H17 . 1.0000 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 N20 . 1.521(4) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
N20 C21 . 1.488(4) ?
N20 H20 . 0.94(4) ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C23 O25 . 1.247(4) ?
C23 O24 . 1.263(4) ?
O27 H27A . 0.96(6) ?
O27 H27B . 0.91(5) ?
O28 H28A . 0.87(6) ?
O28 H28B . 0.91(6) ?
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 0.94(4) 1.92(4) 2.761(3) 148(3) yes
N20 H20 O25 4_456 0.94(4) 2.17(4) 2.792(4) 123(3) yes
O27 H27A O26 . 0.96(6) 1.86(6) 2.811(3) 172(5) yes
O27 H27B O24 3_646 0.91(5) 2.03(5) 2.929(4) 168(4) yes
O28 H28A O24 . 0.87(6) 1.98(7) 2.833(4) 165(5) yes
O28 H28B O27 1_565 0.91(6) 2.00(6) 2.906(4) 172(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 . . . . 2.2(5) ?
C11 N1 C2 C3 . . . . -177.3(3) ?
N1 C2 C3 C4 . . . . -1.9(5) ?
N1 C2 C3 C23 . . . . 178.8(3) ?
C2 C3 C4 O26 . . . . 177.2(3) ?
C23 C3 C4 O26 . . . . -3.5(5) ?
C2 C3 C4 C5 . . . . -2.5(4) ?
C23 C3 C4 C5 . . . . 176.7(3) ?
O26 C4 C5 C10 . . . . -172.9(3) ?
C3 C4 C5 C10 . . . . 6.8(4) ?
O26 C4 C5 C6 . . . . 3.5(4) ?
C3 C4 C5 C6 . . . . -176.7(3) ?
C10 C5 C6 C7 . . . . 1.7(4) ?
C4 C5 C6 C7 . . . . -174.9(3) ?
C5 C6 C7 F22 . . . . 178.2(3) ?
C5 C6 C7 C8 . . . . 2.1(5) ?
C6 C7 C8 N14 . . . . 171.3(3) ?
F22 C7 C8 N14 . . . . -4.8(4) ?
C6 C7 C8 C9 . . . . -4.1(4) ?
F22 C7 C8 C9 . . . . 179.8(3) ?
N14 C8 C9 C10 . . . . -173.0(3) ?
C7 C8 C9 C10 . . . . 2.4(4) ?
C2 N1 C10 C9 . . . . -177.9(3) ?
C11 N1 C10 C9 . . . . 1.6(4) ?
C2 N1 C10 C5 . . . . 2.2(4) ?
C11 N1 C10 C5 . . . . -178.3(3) ?
C8 C9 C10 N1 . . . . -178.8(3) ?
C8 C9 C10 C5 . . . . 1.2(5) ?
C6 C5 C10 N1 . . . . 176.7(3) ?
C4 C5 C10 N1 . . . . -6.8(4) ?
C6 C5 C10 C9 . . . . -3.3(4) ?
C4 C5 C10 C9 . . . . 173.3(3) ?
C2 N1 C11 C12 . . . . -29.2(4) ?
C10 N1 C11 C12 . . . . 151.3(3) ?
C2 N1 C11 C13 . . . . -99.8(4) ?
C10 N1 C11 C13 . . . . 80.7(4) ?
N1 C11 C12 C13 . . . . -107.8(3) ?
N1 C11 C13 C12 . . . . 110.4(3) ?
C9 C8 N14 C15 . . . . 1.1(4) ?
C7 C8 N14 C15 . . . . -174.0(3) ?
C9 C8 N14 C18 . . . . -147.0(3) ?
C7 C8 N14 C18 . . . . 37.9(4) ?
C8 N14 C15 C19 . . . . -82.5(3) ?
C18 N14 C15 C19 . . . . 70.7(3) ?
C8 N14 C15 C16 . . . . 171.3(3) ?
C18 N14 C15 C16 . . . . -35.5(3) ?
N14 C15 C16 C17 . . . . 54.4(2) ?
C19 C15 C16 C17 . . . . -58.2(3) ?
C15 C16 C17 C18 . . . . -54.9(3) ?
C15 C16 C17 N20 . . . . 55.6(2) ?
C8 N14 C18 C17 . . . . 152.5(3) ?
C15 N14 C18 C17 . . . . 0.4(3) ?
C16 C17 C18 N14 . . . . 35.1(3) ?
N20 C17 C18 N14 . . . . -71.1(3) ?
N14 C15 C19 N20 . . . . -67.5(3) ?
C16 C15 C19 N20 . . . . 38.7(3) ?
C15 C19 N20 C21 . . . . -126.7(3) ?
C15 C19 N20 C17 . . . . -3.1(3) ?
C18 C17 N20 C21 . . . . -163.3(3) ?
C16 C17 N20 C21 . . . . 89.7(3) ?
C18 C17 N20 C19 . . . . 73.2(3) ?
C16 C17 N20 C19 . . . . -33.8(3) ?
C2 C3 C23 O25 . . . . -136.5(3) ?
C4 C3 C23 O25 . . . . 44.2(4) ?
C2 C3 C23 O24 . . . . 44.9(4) ?
C4 C3 C23 O24 . . . . -134.3(3) ?
_cod_database_fobs_code 2022694