#------------------------------------------------------------------------------
#$Date: 2024-11-09 03:46:57 +0100 (Sat, 09 Nov 2024) $
#$Revision: 295854 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023314.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_2023314
loop_
_publ_author_name
'Mohan Kumar, Thaluru M.'
'Bhaskar, Besagarahally L.'
'Priyanka, Prabhakar'
'Divakara, Thayamma R.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Crystal structure and Hirshfeld-surface analysis of an etoxazole
metabolite designated R13
;
_journal_coeditor_code NX2015
_journal_issue 12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024010600
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C21 H21 F2 N O2'
_chemical_formula_moiety 'C21 H21 F2 N O2'
_chemical_formula_sum 'C21 H21 F2 N O2'
_chemical_formula_weight 357.39
_chemical_name_systematic
;
4-(4-tert-Butyl-2-ethoxyphenyl)-2-(2,6-difluorophenyl)oxazole
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 93.0350(10)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 18.4793(6)
_cell_length_b 10.4036(3)
_cell_length_c 18.5669(7)
_cell_measurement_reflns_used 9910
_cell_measurement_temperature 100.0(2)
_cell_measurement_theta_max 27.53
_cell_measurement_theta_min 2.25
_cell_volume 3564.5(2)
_computing_cell_refinement
;
APEX5 (Bruker, 2023)
;
_computing_data_collection
;
APEX5 (Bruker, 2023)
;
_computing_data_reduction
;
APEX5 (Bruker, 2023)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0607
_diffrn_reflns_av_unetI/netI 0.0351
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 41370
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.525
_diffrn_reflns_theta_min 2.197
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.099
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.904
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.332
_exptl_crystal_description 'cut block'
_exptl_crystal_F_000 1504
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.190
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.258
_refine_diff_density_min -0.218
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 239
_refine_ls_number_reflns 4095
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.069
_refine_ls_R_factor_all 0.0388
_refine_ls_R_factor_gt 0.0325
_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^)+(0.0317P)^2^+1.7737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0798
_refine_ls_wR_factor_ref 0.0849
_reflns_number_gt 3558
_reflns_number_total 4095
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file nx2015.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 2023314
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.980
_shelx_estimated_absorpt_t_max 0.989
_shelx_hkl_file
;
4 0 0 2.10600 1.42984 1
4 0 0 4.77589 1.35998 3
4 0 0 2.51421 1.11755 4
4 0 0 4.80149 1.20459 5
-4 0 0 6.56870 1.40981 3
-4 0 0 2.82924 1.00548 4
-4 0 0 2.37764 1.65810 1
6 0 0 37.2837 5.99056 1
-6 0 0 47.2540 4.22226 4
-6 0 0 37.1676 5.78944 1
-6 0 0 49.0769 4.22180 3
6 0 0 43.2394 4.01502 5
8 0 0 383.526 25.2150 3
8 0 0 366.269 25.2774 4
8 0 0 368.695 25.0148 5
8 0 0 391.503 27.3412 1
-8 0 0 386.146 25.2266 3
-8 0 0 350.088 27.7527 1
-8 0 0 390.980 24.7040 4
10 0 0 72.7448 6.88149 3
10 0 0 68.0007 10.3730 1
-10 0 0 70.3955 6.77182 3
10 0 0 69.6440 6.64038 5
10 0 0 69.8318 9.49565 4
-10 0 0 76.0244 11.2434 1
-10 0 0 78.6417 6.93466 4
12 0 0 477.989 32.4492 3
-12 0 0 487.583 39.5083 1
12 0 0 462.077 32.2784 5
12 0 0 500.815 32.9551 4
12 0 0 498.029 36.9155 1
-12 0 0 456.621 32.1943 4
-12 0 0 492.340 32.4505 3
14 0 0 1246.71 81.1235 5
-14 0 0 1253.19 78.7430 4
14 0 0 1248.25 86.0755 1
14 0 0 1247.78 79.2344 3
14 0 0 1255.69 79.4959 4
-14 0 0 1279.61 79.0141 3
-14 0 0 1246.11 80.6710 4
16 0 0 1379.33 85.9975 4
-16 0 0 1316.27 84.7473 4
16 0 0 1351.87 85.8613 3
16 0 0 1313.98 85.3695 5
16 0 0 1361.47 91.2495 1
16 0 0 1289.02 85.5331 3
18 0 0 22.6040 5.70112 3
18 0 0 35.4576 9.87419 1
18 0 0 25.5605 5.71847 5
-18 0 0 23.8416 5.29392 4
18 0 0 20.9897 5.79219 3
-20 0 0 216.147 17.8885 4
20 0 0 230.569 24.4461 1
20 0 0 216.800 18.7310 3
20 0 0 213.924 23.6787 1
20 0 0 198.917 19.0570 3
22 0 0 37.8970 10.1956 1
22 0 0 27.1480 6.60104 3
-22 0 0 37.9626 7.00030 4
-1 -1 0 288.631 18.2186 5
-1 -1 0 277.653 19.3254 1
1 1 0 290.093 18.6823 1
1 1 0 282.539 18.6174 4
1 1 0 284.142 18.2133 5
-3 -1 0 376.245 24.8098 4
-3 -1 0 376.234 25.1318 1
3 1 0 377.064 25.3310 4
3 1 0 399.784 24.8843 1
3 1 0 374.637 25.0669 5
3 1 0 375.474 23.6984 3
-5 -1 0 702.748 44.0373 1
-5 -1 0 681.145 41.5776 3
5 1 0 619.727 41.3805 3
-5 1 0 636.121 42.3831 1
7 -1 0 152.562 12.2723 1
7 -1 0 156.068 10.3936 5
7 -1 0 152.423 10.8279 3
-7 -1 0 157.810 11.4202 3
7 -1 0 142.476 10.9242 4
-7 -1 0 142.421 14.2549 1
-7 -1 0 152.815 11.4022 4
7 1 0 147.500 11.9242 4
-7 1 0 152.430 12.6089 1
7 1 0 147.986 11.6223 5
7 1 0 152.777 14.3760 1
-7 1 0 155.400 10.8257 3
-7 1 0 157.948 11.0296 4
7 1 0 165.729 11.5649 3
9 -1 0 432.815 27.6220 3
-9 -1 0 416.169 28.3350 4
9 -1 0 428.198 27.6480 4
9 -1 0 429.622 30.0289 1
9 -1 0 437.132 27.4245 5
-9 -1 0 414.750 28.3492 3
-9 -1 0 391.486 31.8175 1
-9 1 0 456.838 27.5945 3
9 1 0 379.613 28.6100 3
-9 1 0 391.946 27.3182 4
9 1 0 406.851 31.8204 1
9 1 0 436.267 28.8221 4
9 1 0 449.793 28.4391 5
-9 1 0 416.656 30.0065 1
11 -1 0 632.964 41.0073 3
-11 -1 0 625.705 41.7689 4
-11 -1 0 608.495 46.5210 1
11 -1 0 603.078 45.0143 1
11 -1 0 644.306 41.1647 4
-11 -1 0 666.372 41.9777 3
-11 1 0 644.126 40.9033 4
-11 1 0 628.110 44.2297 1
11 1 0 651.855 41.9208 3
11 1 0 618.181 46.0561 1
11 1 0 608.506 42.5013 5
-11 1 0 678.355 41.0300 3
11 1 0 650.334 42.3669 4
13 -1 0 65.2329 8.17197 4
-13 -1 0 77.0121 9.15727 4
-13 -1 0 72.7789 9.04352 3
13 -1 0 77.0039 11.6168 1
13 -1 0 69.4566 7.25803 3
13 -1 0 67.2802 8.19988 5
-13 -1 0 71.8950 8.89905 4
-13 1 0 60.8526 10.4201 1
13 1 0 71.7597 9.49954 4
13 1 0 63.1862 8.76963 5
-13 1 0 83.1038 8.08897 4
13 1 0 70.6435 13.0925 1
-13 1 0 80.5883 7.21857 3
13 1 0 69.8291 9.03079 3
15 -1 0 15.1892 5.91782 1
15 -1 0 28.1284 5.56851 4
15 -1 0 35.9563 5.85972 5
15 -1 0 30.8999 5.48563 3
15 1 0 37.2667 7.26739 3
-15 1 0 30.9096 5.30520 3
15 1 0 21.8559 5.84970 4
15 1 0 36.4880 7.11619 3
-15 1 0 23.3684 4.66779 4
15 1 0 38.5360 9.83657 1
17 -1 0 279.043 22.3729 3
17 -1 0 303.756 22.7666 5
17 -1 0 280.508 26.2889 1
17 -1 0 303.698 22.8227 3
17 -1 0 316.665 22.5671 4
-17 1 0 285.064 21.8923 4
17 1 0 281.793 29.0642 1
17 1 0 295.351 23.5662 3
17 1 0 332.180 24.1393 3
17 1 0 290.368 23.5427 5
17 1 0 281.484 28.5200 1
19 -1 0 47.2279 8.53488 3
19 -1 0 44.9385 10.5051 1
-19 -1 0 68.1528 9.91613 4
19 -1 0 68.8591 9.22161 3
19 -1 0 51.9909 8.75287 5
19 1 0 98.9180 17.7229 1
19 1 0 61.6146 9.73454 3
19 1 0 52.5897 9.96016 3
-19 1 0 55.1152 7.71806 4
19 1 0 47.9642 13.1449 1
-21 -1 0 3.43488 2.94550 4
21 -1 0 2.69101 3.02269 3
21 -1 0 11.9740 5.97557 1
21 -1 0 3.95854 3.30573 3
-21 1 0 4.22018 2.84157 4
21 1 0 10.5027 4.78655 3
21 1 0 12.9044 6.70297 1
21 1 0 10.1744 4.86781 3
23 -1 0 3.41412 3.03410 1
23 -1 0 3.10154 2.86770 3
23 1 0 -1.2420 1.59459 1
23 1 0 3.83514 3.20870 5
23 1 0 -0.7825 2.47155 3
0 2 0 2920.19 180.753 2
2 -2 0 2024.18 137.720 2
-2 2 0 2212.71 130.815 2
2 2 0 2176.69 132.098 2
-4 -2 0 70.7629 6.72425 4
4 -2 0 72.8265 5.78288 1
4 -2 0 77.9016 5.17143 3
-4 -2 0 79.3664 6.38860 5
-4 -2 0 82.5967 6.52339 3
4 -2 0 77.5923 5.13391 4
-4 -2 0 71.8777 9.98648 1
4 2 0 71.9061 6.71915 4
4 2 0 71.0362 6.53604 3
4 2 0 83.8535 6.51873 5
4 2 0 76.9669 6.61094 5
-4 2 0 72.8353 5.11569 3
-4 2 0 72.2729 5.74111 1
4 2 0 80.2264 10.3018 1
-4 2 0 71.8884 5.16505 4
-6 -2 0 1403.43 87.5400 4
-8 -2 0 1599.50 112.832 1
-8 -2 0 1827.20 106.811 4
8 2 0 1746.60 113.026 1
-10 -2 0 42.2210 6.23012 4
-10 -2 0 41.1161 6.32650 3
10 -2 0 35.4624 6.01473 1
10 -2 0 39.2951 4.60574 3
-10 -2 0 39.1005 9.13891 1
10 -2 0 33.1807 4.25461 5
-10 2 0 44.7012 6.65109 1
-10 2 0 38.7042 3.92291 4
10 2 0 34.7704 5.80080 5
10 2 0 51.5779 7.14922 4
10 2 0 53.7583 10.4209 1
-12 -2 0 4.68717 2.69970 4
-12 -2 0 1.90355 2.22724 3
12 -2 0 4.33040 1.83491 4
12 -2 0 4.44611 1.84718 3
12 -2 0 1.32124 1.47269 5
-12 -2 0 1.50179 1.96959 4
12 -2 0 1.24284 1.94587 1
12 2 0 1.47023 2.20672 3
-12 2 0 5.01323 2.58247 1
12 2 0 6.18938 2.66680 5
12 2 0 2.25329 3.28124 1
-12 2 0 4.69726 1.61927 3
-12 2 0 1.70829 1.32301 4
12 2 0 4.32256 2.98586 4
14 -2 0 13.6705 3.24073 3
14 -2 0 4.63733 3.21281 1
-14 -2 0 6.60383 3.47118 4
-14 -2 0 9.81192 3.58638 4
14 -2 0 6.86412 2.44343 4
14 -2 0 8.39240 2.80943 5
-14 2 0 8.73373 2.56598 4
14 2 0 10.6718 4.15238 4
-14 2 0 11.0119 2.65674 4
14 2 0 7.49489 3.62057 3
14 2 0 13.5175 6.23876 1
14 2 0 9.37101 3.64924 3
14 2 0 10.2344 3.87759 5
-16 -2 0 947.133 62.8175 4
16 -2 0 910.357 61.4126 3
16 -2 0 960.381 60.3808 3
16 -2 0 899.072 61.7167 5
16 -2 0 946.295 64.9415 1
16 -2 0 987.330 60.6523 4
16 -2 0 939.359 65.1294 1
16 2 0 944.359 71.1846 1
16 2 0 990.155 69.6068 1
16 2 0 947.680 63.6122 3
16 2 0 960.563 63.2763 3
18 -2 0 18.3258 5.05733 5
-18 -2 0 18.8384 5.52946 4
18 -2 0 13.5974 6.50422 1
18 -2 0 19.8715 6.40808 1
18 -2 0 21.5766 4.72570 3
18 -2 0 19.3066 4.57956 3
18 2 0 13.7247 7.35233 1
18 2 0 12.7048 4.84370 3
-18 2 0 18.0315 3.95713 4
20 -2 0 77.1835 16.1377 1
20 -2 0 63.0348 12.0951 1
20 -2 0 60.4411 8.97008 3
20 -2 0 63.0201 9.26498 5
-20 -2 0 89.3594 14.8787 4
20 -2 0 75.1223 9.37262 3
20 2 0 74.0089 12.1876 5
20 2 0 77.2364 12.0532 3
20 2 0 52.3974 14.5766 1
20 2 0 70.8082 18.1981 1
-20 2 0 63.1258 8.16355 4
20 2 0 75.8443 11.6072 3
22 -2 0 12.6081 4.31318 3
22 -2 0 9.17090 4.83229 1
22 -2 0 12.6590 4.16559 3
22 2 0 9.14243 5.33197 5
22 2 0 21.9541 11.8290 1
22 2 0 6.01221 5.09307 3
-22 2 0 15.1724 4.50601 4
22 2 0 13.3214 5.40358 3
1 -3 0 988.716 64.3615 5
1 3 0 1067.39 65.2812 1
3 -3 0 4923.32 301.222 2
3 3 0 4825.64 300.660 2
-3 3 0 4843.86 301.562 2
3 3 0 4905.33 301.440 2
-5 -3 0 673.589 46.5607 3
-5 -3 0 745.134 45.8581 4
-5 -3 0 741.645 46.5667 5
5 3 0 705.452 47.0495 4
5 3 0 761.114 45.5587 5
5 3 0 693.274 50.4392 1
5 3 0 676.420 46.5627 3
-5 3 0 733.670 46.4606 1
5 3 0 742.427 46.3777 5
7 -3 0 24.1127 2.43975 3
7 -3 0 22.9302 3.43660 1
7 -3 0 25.7251 2.46921 4
-7 -3 0 21.1044 4.44971 4
-7 -3 0 33.2051 5.24265 5
-7 -3 0 26.4577 4.81993 3
7 -3 0 26.3901 2.16448 5
7 3 0 31.3594 5.07742 3
-7 3 0 26.4184 2.35627 3
7 3 0 34.1518 5.70399 5
-7 3 0 25.2709 3.50539 1
7 3 0 23.3556 6.91143 1
-7 3 0 24.0376 2.13718 4
7 3 0 30.0300 5.28073 4
7 3 0 26.3407 4.74163 5
9 -3 0 356.291 22.1070 3
9 -3 0 336.596 23.4397 1
-9 -3 0 362.155 24.7634 4
-9 -3 0 357.117 24.7664 3
-9 -3 0 367.058 25.0260 4
9 -3 0 345.819 22.0593 4
9 -3 0 351.405 21.9449 5
9 3 0 369.515 29.8354 1
-9 3 0 324.041 22.1094 4
-9 3 0 335.776 23.1683 1
9 3 0 333.749 24.9338 5
-9 3 0 347.500 21.8979 3
9 3 0 327.828 25.4081 4
9 3 0 343.428 24.4199 5
9 3 0 326.286 24.6163 3
11 -3 0 79.9135 6.94614 3
11 -3 0 94.0291 7.21485 5
11 -3 0 82.7665 6.99923 4
11 -3 0 90.5765 8.67123 1
-11 -3 0 88.7081 10.9960 3
-11 -3 0 66.5138 9.67721 4
-11 -3 0 100.376 9.84934 4
11 3 0 104.406 9.86703 5
-11 3 0 100.126 8.69727 1
11 3 0 105.936 12.3821 5
11 3 0 91.8733 11.7171 4
11 3 0 101.171 16.4894 1
11 3 0 96.8527 9.72645 3
11 3 0 76.4588 10.9176 3
-11 3 0 91.2307 6.74020 4
-11 3 0 89.3357 6.88714 3
13 -3 0 91.3506 7.81464 3
-13 -3 0 95.3460 11.4942 4
13 -3 0 80.3958 9.15213 1
13 -3 0 91.8498 7.45009 4
-13 -3 0 74.3265 10.6965 4
13 -3 0 86.1032 7.66991 5
13 3 0 82.3864 11.2061 5
-13 3 0 86.4967 7.11579 3
13 3 0 76.4172 15.0246 1
-13 3 0 94.4296 6.85271 4
13 3 0 107.049 17.7704 1
13 3 0 83.7227 11.9235 5
13 3 0 108.837 10.5436 3
-13 3 0 84.9260 7.02973 4
13 3 0 73.1065 11.1505 3
13 3 0 77.2238 11.1902 4
15 -3 0 195.397 17.6785 1
15 -3 0 212.357 15.5229 5
-15 -3 0 190.516 17.7525 4
15 -3 0 211.066 14.9510 3
15 -3 0 196.019 17.0856 1
15 -3 0 205.814 15.1572 4
-15 3 0 204.273 14.3812 4
15 3 0 238.253 28.9597 1
15 3 0 226.235 28.2371 1
15 3 0 188.959 17.7673 3
-15 3 0 203.059 14.1829 4
15 3 0 173.130 18.1529 3
15 3 0 228.232 19.2574 5
17 -3 0 439.213 33.0631 5
17 -3 0 486.681 31.3546 3
17 -3 0 447.436 35.6685 1
-17 -3 0 461.833 34.6102 4
17 -3 0 504.160 34.4215 1
-17 3 0 486.441 30.4663 4
17 3 0 461.678 36.0601 3
17 3 0 463.039 35.5313 5
17 3 0 475.286 38.4398 3
17 3 0 461.082 42.6618 1
17 3 0 487.803 42.3945 1
19 -3 0 17.6223 5.11198 5
19 -3 0 22.6982 6.03396 1
19 -3 0 24.2540 4.55231 3
-19 -3 0 9.25393 4.88392 4
19 -3 0 24.0419 4.64110 3
19 -3 0 23.7234 6.36678 1
19 3 0 34.7218 11.6186 1
-19 3 0 23.2647 3.71230 4
19 3 0 27.1367 7.38916 3
19 3 0 33.2430 11.7782 1
19 3 0 24.6419 7.53654 5
19 3 0 15.2703 5.85334 3
21 -3 0 2.11352 1.88585 3
21 -3 0 -0.7444 1.60269 3
21 -3 0 0.93547 2.06428 1
-21 -3 0 1.32910 2.87013 4
21 3 0 -3.3758 2.70650 5
21 3 0 -1.6656 2.91898 3
21 3 0 0.31441 3.77119 3
21 3 0 1.27654 3.36634 1
23 -3 0 30.2943 4.64712 3
23 3 0 29.1992 7.55574 5
23 3 0 23.4107 6.47727 3
0 4 0 2978.96 189.092 2
2 -4 0 13.9322 2.57956 4
2 -4 0 12.0645 2.57072 5
2 -4 0 11.3373 2.31093 5
-2 -4 0 9.87601 2.87233 4
-2 -4 0 14.8230 3.15890 4
-2 -4 0 18.3602 3.57164 5
2 4 0 14.5254 4.77578 1
-2 4 0 13.9205 2.60605 3
2 4 0 15.6317 3.11401 5
-2 4 0 17.1705 2.39322 5
2 4 0 14.0526 4.86448 1
2 4 0 16.8772 3.50061 5
-2 4 0 12.4037 2.68478 3
-2 4 0 14.9728 2.10553 5
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-3 -5 22 32.6696 8.66735 5
-3 -5 22 25.6498 10.4474 3
3 5 -22 40.6477 8.98746 4
-3 5 22 41.3048 16.2288 1
-3 5 22 31.7273 9.19312 3
1 -5 -22 36.8208 10.9190 4
1 -5 -22 14.9244 10.8570 1
-1 -5 22 33.2892 9.39610 5
-1 5 22 28.1653 9.70175 3
1 5 -22 21.7783 7.86596 4
-1 5 22 39.0169 13.9159 1
1 -5 22 109.252 16.3684 5
1 -5 22 109.122 21.5732 3
-1 -5 -22 107.571 18.8256 4
-1 -5 -22 109.044 24.5828 1
1 5 22 80.9225 18.5030 3
1 5 22 106.199 24.0800 1
1 5 22 108.224 16.2997 5
3 -5 22 3.03881 4.12325 3
3 5 22 -0.2095 2.82389 3
-8 0 23 -3.9947 1.99101 3
-8 0 23 2.76657 3.40480 5
-8 0 23 1.66692 4.15478 1
8 0 -23 0.42044 3.03456 4
8 0 -23 0.29186 3.53709 1
6 0 -23 -0.9723 2.66515 4
-6 0 23 7.21128 6.69556 1
6 0 -23 7.59965 6.68194 1
-4 0 23 5.65705 4.99512 1
-4 0 23 -5.9160 1.42443 3
-4 0 23 -0.9368 3.15877 5
4 0 -23 -0.6150 3.80086 1
4 0 -23 -1.1592 2.55925 4
2 0 -23 2.24486 5.63928 1
-2 0 23 0.41647 3.45225 5
-2 0 23 0.13233 3.76472 3
-2 0 23 5.95901 5.88183 1
2 0 -23 -2.1203 2.63919 4
0 0 -23 2.45164 3.10266 4
0 0 23 6.52865 6.00947 1
0 0 23 -2.0828 2.89506 3
0 0 23 -3.6571 2.27561 5
0 0 -23 5.43088 5.15806 1
-2 0 -23 5.43636 6.28059 1
2 0 23 1.72034 3.49144 5
-2 0 -23 -0.8108 2.62584 4
2 0 23 -0.8854 2.94054 3
2 0 23 -2.3259 2.23429 1
-4 0 -23 3.09950 3.74229 4
4 0 23 2.47420 4.76938 1
4 0 23 -2.9460 1.79602 5
-7 -1 23 1.24988 3.32740 1
7 -1 -23 -2.8709 2.27822 4
7 -1 -23 13.4764 8.66580 1
-7 -1 23 0.48379 3.92471 5
-7 1 23 -0.7310 2.24013 3
7 1 -23 7.64312 7.05739 1
-7 1 23 3.41213 4.11845 5
-7 1 23 6.28533 5.59528 1
7 1 -23 2.68408 4.02986 4
5 -1 -23 13.7490 10.3078 1
-5 -1 23 34.5789 14.3963 1
-5 -1 23 33.5881 9.74828 3
-5 -1 23 35.5164 9.60575 5
-5 1 23 31.1427 11.0830 5
-5 1 23 34.2496 13.8224 1
5 1 -23 29.4802 9.64032 4
-3 -1 23 7.28358 4.97213 5
3 -1 -23 6.81717 6.81424 1
-3 -1 23 8.33813 6.79493 1
3 -1 -23 8.14305 5.38572 4
-3 -1 23 4.62449 4.69783 3
3 1 -23 0.97779 4.26548 4
-3 1 23 3.58186 5.72200 3
-3 1 23 4.12240 5.21792 5
3 1 -23 3.58281 7.54642 1
-3 1 23 2.67956 5.82156 1
-1 -1 23 5.44018 4.82065 5
-1 -1 23 0.31911 3.81466 3
1 -1 -23 6.58822 6.25964 1
1 -1 -23 3.69485 4.30374 4
-1 -1 23 10.3005 7.71693 1
-1 1 23 -0.2730 3.52925 5
1 1 -23 5.45261 4.48682 4
-1 1 23 5.21279 4.69441 3
1 1 -23 4.29247 6.01919 1
-1 1 23 -1.0207 2.66747 1
1 -1 23 10.8278 7.90180 1
-1 -1 -23 3.07396 5.25269 1
-1 -1 -23 2.07311 4.00584 4
1 -1 23 6.80035 4.74810 3
1 -1 23 5.16455 4.24266 5
-1 1 -23 6.22019 5.06835 4
1 1 23 -2.5531 2.29714 3
-1 1 -23 7.10790 7.01313 1
1 1 23 8.15280 5.03947 5
1 1 23 1.72191 4.28835 1
3 -1 23 143.505 20.2979 3
3 -1 23 146.013 19.8819 5
-3 -1 -23 144.995 20.9214 4
-3 -1 -23 121.115 27.3856 1
3 -1 23 146.666 27.6483 1
3 1 23 143.171 30.2403 1
3 1 23 145.253 20.6716 5
-3 1 -23 146.331 18.8603 4
-3 1 -23 98.2659 32.0786 1
-5 -1 -23 47.4268 10.2426 4
5 -1 23 45.6630 13.0653 3
5 -1 23 48.2563 11.2627 5
5 1 23 44.8527 11.3173 3
-5 1 -23 34.9625 11.2027 4
-6 -2 23 6.35477 5.02026 1
-6 -2 23 1.08248 3.77376 3
6 -2 -23 -1.5841 3.22439 1
-6 -2 23 -0.0364 3.02645 5
6 -2 -23 1.28618 3.03572 4
6 2 -23 5.71752 4.53860 4
-6 2 23 -0.7934 2.85782 3
-6 2 23 9.02788 7.81327 1
-4 -2 23 22.8081 10.6034 1
-4 -2 23 4.57377 5.60267 5
4 -2 -23 12.0594 8.76459 1
4 -2 -23 13.1890 6.07710 4
-4 -2 23 7.21519 7.25605 3
-4 2 23 23.0138 7.82628 3
4 2 -23 11.8424 9.04600 1
-4 2 23 15.4841 9.17664 1
-4 2 23 12.1521 8.06752 5
4 2 -23 5.50001 5.90749 4
-2 -2 23 5.04245 5.11834 5
2 -2 -23 5.32019 5.43653 4
-2 -2 23 0.50846 4.53406 1
-2 -2 23 11.0387 5.27996 3
2 -2 -23 0.49346 4.74654 1
-2 2 23 -1.3983 2.85717 5
-2 2 23 8.15765 7.25879 1
2 2 -23 -1.4605 2.57844 1
2 2 -23 5.09258 5.24619 4
-2 2 23 -3.2635 2.20234 3
0 -2 23 130.015 16.6783 3
0 -2 -23 108.075 27.0085 1
0 -2 23 130.197 24.7244 1
0 -2 -23 127.552 20.0910 4
0 -2 23 125.042 17.6047 5
0 2 23 128.787 19.9302 5
0 2 23 107.895 18.7578 3
0 2 -23 109.836 26.6296 4
0 2 -23 128.299 28.3556 1
-2 -2 -23 73.6647 13.4437 4
-2 -2 -23 67.4476 21.4830 1
2 -2 23 49.6273 13.0535 3
2 -2 23 55.3031 12.6133 5
2 -2 23 72.5226 18.9607 1
-2 2 -23 54.9420 12.2261 4
2 2 23 70.6490 21.4317 1
4 -2 23 2.86225 3.27229 5
-4 -2 -23 3.11245 3.57735 4
4 2 23 10.3500 8.29715 1
4 2 23 -0.4297 2.40571 3
-5 -3 23 5.81761 5.74897 5
-5 -3 23 6.12845 7.80686 1
5 -3 -23 7.73964 6.46396 4
-5 -3 23 5.21896 5.59516 3
5 3 -23 6.44426 5.86726 4
-5 3 23 5.35853 5.52782 3
5 3 -23 7.84082 9.20694 1
-5 3 23 3.16440 5.65619 5
-5 3 23 -0.3368 2.99243 1
-3 -3 23 15.5447 9.69243 1
3 -3 -23 15.8758 9.71768 1
3 -3 -23 15.2461 6.38878 4
-3 -3 23 14.4139 8.67007 3
3 3 -23 13.5764 14.6681 1
-3 3 23 17.8542 9.14068 1
3 3 -23 27.2898 7.80850 4
-3 3 23 15.6331 5.87553 3
-1 -3 23 -1.2123 2.83478 1
1 -3 -23 10.3773 7.14109 1
-1 -3 23 -0.8957 3.33367 5
1 -3 -23 -0.1346 2.88159 4
-1 3 23 -1.2488 2.68021 3
-1 3 23 15.1125 8.90881 1
-1 -3 -23 0.77564 4.34462 1
-1 -3 -23 3.84997 4.19879 4
1 -3 23 -2.4950 2.62102 5
-1 3 -23 -0.0325 3.00320 4
1 3 23 0.72350 4.17872 1
1 3 23 -1.9219 1.98087 5
3 -3 23 35.1939 10.6596 5
3 -3 23 35.5601 11.1593 3
-3 -3 -23 34.7792 9.75653 4
-3 -3 -23 34.4017 16.8190 1
3 3 23 40.6158 9.47203 5
3 3 23 25.9534 9.64265 3
3 3 23 25.6649 14.5922 1
-2 -4 23 0.72455 3.17508 3
2 -4 -23 4.61688 5.74084 1
-2 4 23 1.10513 3.05591 1
-2 0 24 0.43541 4.79713 3
2 0 -24 1.27835 2.84565 4
-2 0 24 -0.1200 2.68636 5
-2 0 24 -0.0031 2.52701 1
2 0 -24 -0.1984 3.93462 1
0 0 24 8.19364 6.12356 3
0 0 -24 16.9037 6.24957 4
0 0 24 17.4788 8.47050 1
0 0 24 16.4213 7.67376 5
1 -1 -24 13.7469 5.91819 4
1 -1 -24 17.7282 10.3206 1
-1 -1 24 21.0148 6.57732 3
-1 1 24 12.2520 6.90961 3
1 1 -24 13.4634 7.04750 4
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 13296
_shelx_res_file
;
TITL m24167 : space group C2/c
m24167.res
created by SHELXL-2019/3 at 11:40:15 on 25-Oct-2024
CELL 0.71073 18.4793 10.4036 18.5669 90.000 93.035 90.000
ZERR 8 0.0006 0.0003 0.0007 0.000 0.001 0.000
LATT 7
SYMM -X, Y, 1/2-Z
SFAC C H F N O
UNIT 168 168 16 8 16
TEMP -173
SIZE 0.20 0.19 0.11
REM COLR colourless
REM FORM cut block
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for *potential* hydrogen bonds and close contacts:
HTAB C2 O2
EQIV $2 0.5-x, y-0.5, 0.5-z
RTAB dist N1 C19_$2
RTAB dist N1 H19_$2
RTAB angl N1 H19_$2 C19_$2
HTAB
REM Overlap of inversion-related oxazole rings = 3.3426(11)
EQIV $1 0.5-x, 1.5-y, 1-z
MPLA 5 N1 O1 C1 C2 C3 N1_$1 O1_$1 C1_$1 C2_$1 C3_$1
REM Angle between inversion-related (different) benzene rings = 11.56(6)
MPLA C4 C5 C6 C7 C8 C9
MPLA C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
REM Centroid-to-centroid distance of these rings via CENT/X in XP = 3.9439
REM RTAB dist X1a X1b
REM CONN 0 x1a x1b
REM X1A 2 10.334749 10.397460 10.538520 10.00000 10.04000
REM X1B 2 10.320921 10.594310 10.718801 10.00000 10.04000
REM Centroid to centroid SU estimation = 0.0011
RTAB D2CG C4 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
RTAB D2CG C5 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
RTAB D2CG C6 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
RTAB D2CG C7 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
RTAB D2CG C8 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
RTAB D2CG C9 C16_$1 C17_$1 C18_$1 C19_$1 C20_$1 C21_$1
REM Dihedrals: First is 24.91(5), second is 15.30(6) degrees.
MPLA N1 C1 O1 C2 C3
MPLA C16 C17 C18 C19 C20 C21
MPLA N1 C1 O1 C2 C3
MPLA C4 C5 C6 C7 C8 C9
MPLA C16 C17 C18 C19 C20 C21
REM Ethoxy torsions:
RTAB tors C4 C9 o2 C10
RTAB tors C9 O2 C10 C11
REM t-butyl torsion:
RTAB tors C13 C12 C7 C6
FMAP 2
PLAN 20
REM EXTI 0.000812 : not significant
WGHT 0.031700 1.773700
FVAR 0.43043
F1 3 0.312742 0.821346 0.325086 11.00000 0.01839 0.03274 =
0.03118 0.00802 0.00413 0.00396
F2 3 0.058895 0.817368 0.342052 11.00000 0.01787 0.04753 =
0.04287 0.01978 0.00194 -0.00162
O1 5 0.143156 0.714745 0.446349 11.00000 0.02039 0.02398 =
0.02187 0.00440 0.00357 0.00214
O2 5 0.195334 0.411636 0.583637 11.00000 0.01735 0.02465 =
0.02500 0.00678 0.00506 0.00198
N1 4 0.248484 0.641490 0.410104 11.00000 0.02171 0.01896 =
0.01942 0.00073 0.00167 0.00011
C1 1 0.195158 0.720026 0.397183 11.00000 0.01859 0.01912 =
0.01933 -0.00134 0.00196 -0.00165
C2 1 0.168110 0.623141 0.494721 11.00000 0.02253 0.02229 =
0.01993 0.00422 0.00199 0.00055
AFIX 43
H2 2 0.144270 0.596124 0.536213 11.00000 -1.20000
AFIX 0
C3 1 0.232184 0.577649 0.473643 11.00000 0.02079 0.01783 =
0.01813 -0.00047 0.00093 -0.00250
C4 1 0.283433 0.484599 0.506751 11.00000 0.02019 0.01764 =
0.01914 -0.00133 0.00083 0.00000
C5 1 0.354277 0.479789 0.484887 11.00000 0.02346 0.02077 =
0.02086 0.00197 0.00398 -0.00082
AFIX 43
H5 2 0.368284 0.535977 0.447771 11.00000 -1.20000
AFIX 0
C6 1 0.404835 0.395515 0.515680 11.00000 0.01842 0.02521 =
0.02545 0.00055 0.00363 0.00046
AFIX 43
H6 2 0.452820 0.395248 0.499675 11.00000 -1.20000
AFIX 0
C7 1 0.386190 0.310680 0.570092 11.00000 0.01969 0.01952 =
0.01950 -0.00279 0.00037 0.00094
C8 1 0.315196 0.313859 0.591917 11.00000 0.02109 0.01897 =
0.01904 0.00005 0.00183 -0.00040
AFIX 43
H8 2 0.301032 0.255850 0.628094 11.00000 -1.20000
AFIX 0
C9 1 0.264552 0.400298 0.561811 11.00000 0.01776 0.02011 =
0.01928 -0.00189 0.00195 -0.00101
C10 1 0.171458 0.323296 0.636870 11.00000 0.02167 0.02233 =
0.02275 0.00559 0.00256 -0.00111
AFIX 23
H10A 2 0.205099 0.324699 0.680171 11.00000 -1.20000
H10B 2 0.169803 0.234787 0.617268 11.00000 -1.20000
AFIX 0
C11 1 0.096814 0.365515 0.656046 11.00000 0.02244 0.03636 =
0.02972 0.01177 0.00486 0.00117
AFIX 137
H11A 2 0.063603 0.360211 0.613215 11.00000 -1.50000
H11B 2 0.098855 0.454391 0.673527 11.00000 -1.50000
H11C 2 0.079477 0.309378 0.693857 11.00000 -1.50000
AFIX 0
C12 1 0.443660 0.220035 0.604116 11.00000 0.01934 0.02389 =
0.02160 -0.00002 0.00079 0.00276
C13 1 0.412971 0.129463 0.659837 11.00000 0.02542 0.03156 =
0.02824 0.00785 0.00313 0.00723
AFIX 137
H13A 2 0.373991 0.077640 0.636764 11.00000 -1.50000
H13B 2 0.393756 0.180052 0.699046 11.00000 -1.50000
H13C 2 0.451514 0.072699 0.679385 11.00000 -1.50000
AFIX 0
C14 1 0.504596 0.300062 0.641390 11.00000 0.02394 0.03603 =
0.03368 -0.00085 -0.00530 0.00010
AFIX 137
H14A 2 0.525169 0.357895 0.606173 11.00000 -1.50000
H14B 2 0.542537 0.242579 0.661459 11.00000 -1.50000
H14C 2 0.484974 0.350789 0.680327 11.00000 -1.50000
AFIX 0
C15 1 0.475070 0.137233 0.545042 11.00000 0.02845 0.02874 =
0.02768 0.00007 0.00484 0.00840
AFIX 137
H15A 2 0.435806 0.090190 0.519134 11.00000 -1.50000
H15B 2 0.509964 0.075983 0.567013 11.00000 -1.50000
H15C 2 0.499521 0.192584 0.511211 11.00000 -1.50000
AFIX 0
C16 1 0.186373 0.813742 0.338519 11.00000 0.02179 0.01796 =
0.01792 -0.00106 0.00078 0.00007
C17 1 0.245769 0.862386 0.303699 11.00000 0.01876 0.02124 =
0.02095 -0.00245 0.00144 0.00230
C18 1 0.239927 0.951208 0.248730 11.00000 0.02490 0.02237 =
0.02116 -0.00049 0.00551 -0.00113
AFIX 43
H18 2 0.281992 0.981741 0.226916 11.00000 -1.20000
AFIX 0
C19 1 0.171944 0.995431 0.225671 11.00000 0.03045 0.02095 =
0.02094 0.00214 0.00099 0.00112
AFIX 43
H19 2 0.167056 1.057008 0.187945 11.00000 -1.20000
AFIX 0
C20 1 0.111084 0.949646 0.257759 11.00000 0.02325 0.02813 =
0.02763 0.00407 -0.00169 0.00367
AFIX 43
H20 2 0.064166 0.978656 0.241898 11.00000 -1.20000
AFIX 0
C21 1 0.119374 0.861748 0.312818 11.00000 0.01948 0.02545 =
0.02653 0.00235 0.00318 -0.00196
HKLF 4
REM m24167 : space group C2/c
REM wR2 = 0.0849, GooF = S = 1.069, Restrained GooF = 1.069 for all data
REM R1 = 0.0325 for 3558 Fo > 4sig(Fo) and 0.0388 for all 4095 data
REM 239 parameters refined using 0 restraints
END
WGHT 0.0317 1.7737
REM Instructions for potential hydrogen bonds
HTAB C2 O2
REM Highest difference peak 0.258, deepest hole -0.218, 1-sigma level 0.040
Q1 1 0.4152 0.2622 0.5870 11.00000 0.05 0.26
Q2 1 0.4274 0.1818 0.6273 11.00000 0.05 0.22
Q3 1 0.2536 0.5278 0.4857 11.00000 0.05 0.22
Q4 1 0.1874 0.7605 0.3647 11.00000 0.05 0.20
Q5 1 0.1270 0.6329 0.5325 11.00000 0.05 0.20
Q6 1 0.3755 0.4335 0.5045 11.00000 0.05 0.18
Q7 1 0.4560 0.1814 0.5780 11.00000 0.05 0.18
Q8 1 0.2398 0.9170 0.2831 11.00000 0.05 0.17
Q9 1 0.2154 0.6243 0.4956 11.00000 0.05 0.17
Q10 1 0.2709 0.4375 0.5261 11.00000 0.05 0.16
Q11 1 0.2394 0.6027 0.4429 11.00000 0.05 0.16
Q12 1 0.3145 0.4730 0.4919 11.00000 0.05 0.16
Q13 1 0.4672 0.2531 0.6199 11.00000 0.05 0.14
Q14 1 0.2878 0.3402 0.5641 11.00000 0.05 0.14
Q15 1 0.2109 0.8230 0.3166 11.00000 0.05 0.14
Q16 1 0.3977 0.3723 0.5503 11.00000 0.05 0.14
Q17 1 0.2638 0.6027 0.3771 11.00000 0.05 0.14
Q18 1 0.2376 0.7075 0.4161 11.00000 0.05 0.14
Q19 1 0.3890 0.3348 0.5278 11.00000 0.05 0.14
Q20 1 0.2039 0.6592 0.3881 11.00000 0.05 0.14
;
_shelx_res_checksum 4165
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F F1 0.31274(3) 0.82135(6) 0.32509(3) 0.02734(16) Uani d 1 . .
F F2 0.05890(3) 0.81737(7) 0.34205(4) 0.03608(19) Uani d 1 . .
O O1 0.14316(4) 0.71474(7) 0.44635(4) 0.02199(17) Uani d 1 . .
O O2 0.19533(4) 0.41164(7) 0.58364(4) 0.02220(17) Uani d 1 . .
N N1 0.24848(5) 0.64149(8) 0.41010(5) 0.02001(18) Uani d 1 . .
C C1 0.19516(5) 0.72003(9) 0.39718(5) 0.0190(2) Uani d 1 . .
C C2 0.16811(6) 0.62314(10) 0.49472(6) 0.0216(2) Uani d 1 . .
H H2 0.144270 0.596124 0.536213 0.026 Uiso calc 1 . .
C C3 0.23218(5) 0.57765(9) 0.47364(5) 0.0189(2) Uani d 1 . .
C C4 0.28343(5) 0.48460(9) 0.50675(5) 0.0190(2) Uani d 1 . .
C C5 0.35428(6) 0.47979(10) 0.48489(6) 0.0216(2) Uani d 1 . .
H H5 0.368284 0.535977 0.447771 0.026 Uiso calc 1 . .
C C6 0.40484(6) 0.39551(10) 0.51568(6) 0.0229(2) Uani d 1 . .
H H6 0.452820 0.395248 0.499675 0.028 Uiso calc 1 . .
C C7 0.38619(5) 0.31068(9) 0.57009(5) 0.0196(2) Uani d 1 . .
C C8 0.31520(5) 0.31386(9) 0.59192(5) 0.0197(2) Uani d 1 . .
H H8 0.301032 0.255850 0.628094 0.024 Uiso calc 1 . .
C C9 0.26455(5) 0.40030(9) 0.56181(5) 0.0190(2) Uani d 1 . .
C C10 0.17146(6) 0.32330(10) 0.63687(6) 0.0222(2) Uani d 1 . .
H H10A 0.205099 0.324699 0.680171 0.027 Uiso calc 1 . .
H H10B 0.169803 0.234787 0.617268 0.027 Uiso calc 1 . .
C C11 0.09681(6) 0.36551(12) 0.65605(6) 0.0294(3) Uani d 1 . .
H H11A 0.063603 0.360211 0.613215 0.044 Uiso calc 1 . .
H H11B 0.098855 0.454391 0.673527 0.044 Uiso calc 1 . .
H H11C 0.079477 0.309378 0.693857 0.044 Uiso calc 1 . .
C C12 0.44366(5) 0.22003(10) 0.60412(6) 0.0216(2) Uani d 1 . .
C C13 0.41297(6) 0.12946(11) 0.65984(6) 0.0283(2) Uani d 1 . .
H H13A 0.373991 0.077640 0.636764 0.043 Uiso calc 1 . .
H H13B 0.393756 0.180052 0.699046 0.043 Uiso calc 1 . .
H H13C 0.451514 0.072699 0.679385 0.043 Uiso calc 1 . .
C C14 0.50460(6) 0.30006(12) 0.64139(7) 0.0315(3) Uani d 1 . .
H H14A 0.525169 0.357895 0.606173 0.047 Uiso calc 1 . .
H H14B 0.542537 0.242579 0.661459 0.047 Uiso calc 1 . .
H H14C 0.484974 0.350789 0.680327 0.047 Uiso calc 1 . .
C C15 0.47507(6) 0.13723(11) 0.54504(6) 0.0282(2) Uani d 1 . .
H H15A 0.435806 0.090190 0.519134 0.042 Uiso calc 1 . .
H H15B 0.509964 0.075983 0.567013 0.042 Uiso calc 1 . .
H H15C 0.499521 0.192584 0.511211 0.042 Uiso calc 1 . .
C C16 0.18637(5) 0.81374(9) 0.33852(5) 0.0192(2) Uani d 1 . .
C C17 0.24577(5) 0.86239(10) 0.30370(5) 0.0203(2) Uani d 1 . .
C C18 0.23993(6) 0.95121(10) 0.24873(6) 0.0227(2) Uani d 1 . .
H H18 0.281992 0.981741 0.226916 0.027 Uiso calc 1 . .
C C19 0.17194(6) 0.99543(10) 0.22567(6) 0.0241(2) Uani d 1 . .
H H19 0.167056 1.057008 0.187945 0.029 Uiso calc 1 . .
C C20 0.11108(6) 0.94965(11) 0.25776(6) 0.0264(2) Uani d 1 . .
H H20 0.064166 0.978656 0.241898 0.032 Uiso calc 1 . .
C C21 0.11937(6) 0.86175(10) 0.31282(6) 0.0237(2) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
F1 0.0184(3) 0.0327(3) 0.0312(3) 0.0040(3) 0.0041(2) 0.0080(3)
F2 0.0179(3) 0.0475(4) 0.0429(4) -0.0016(3) 0.0019(3) 0.0198(3)
O1 0.0204(4) 0.0240(4) 0.0219(4) 0.0021(3) 0.0036(3) 0.0044(3)
O2 0.0174(3) 0.0247(4) 0.0250(4) 0.0020(3) 0.0051(3) 0.0068(3)
N1 0.0217(4) 0.0190(4) 0.0194(4) 0.0001(3) 0.0017(3) 0.0007(3)
C1 0.0186(5) 0.0191(5) 0.0193(5) -0.0016(4) 0.0020(4) -0.0013(4)
C2 0.0225(5) 0.0223(5) 0.0199(5) 0.0006(4) 0.0020(4) 0.0042(4)
C3 0.0208(5) 0.0178(4) 0.0181(5) -0.0025(4) 0.0009(4) -0.0005(4)
C4 0.0202(5) 0.0176(4) 0.0191(5) 0.0000(4) 0.0008(4) -0.0013(4)
C5 0.0235(5) 0.0208(5) 0.0209(5) -0.0008(4) 0.0040(4) 0.0020(4)
C6 0.0184(5) 0.0252(5) 0.0254(5) 0.0005(4) 0.0036(4) 0.0005(4)
C7 0.0197(5) 0.0195(5) 0.0195(5) 0.0009(4) 0.0004(4) -0.0028(4)
C8 0.0211(5) 0.0190(5) 0.0190(5) -0.0004(4) 0.0018(4) 0.0001(4)
C9 0.0178(5) 0.0201(5) 0.0193(5) -0.0010(4) 0.0019(4) -0.0019(4)
C10 0.0217(5) 0.0223(5) 0.0227(5) -0.0011(4) 0.0026(4) 0.0056(4)
C11 0.0224(5) 0.0364(6) 0.0297(6) 0.0012(5) 0.0049(4) 0.0118(5)
C12 0.0193(5) 0.0239(5) 0.0216(5) 0.0028(4) 0.0008(4) 0.0000(4)
C13 0.0254(5) 0.0316(6) 0.0282(6) 0.0072(5) 0.0031(4) 0.0078(5)
C14 0.0239(6) 0.0360(6) 0.0337(6) 0.0001(5) -0.0053(5) -0.0009(5)
C15 0.0284(6) 0.0287(6) 0.0277(6) 0.0084(5) 0.0048(4) 0.0001(4)
C16 0.0218(5) 0.0180(5) 0.0179(5) 0.0001(4) 0.0008(4) -0.0011(4)
C17 0.0188(5) 0.0212(5) 0.0210(5) 0.0023(4) 0.0014(4) -0.0025(4)
C18 0.0249(5) 0.0224(5) 0.0212(5) -0.0011(4) 0.0055(4) -0.0005(4)
C19 0.0305(6) 0.0210(5) 0.0209(5) 0.0011(4) 0.0010(4) 0.0021(4)
C20 0.0233(5) 0.0281(5) 0.0276(6) 0.0037(4) -0.0017(4) 0.0041(4)
C21 0.0195(5) 0.0255(5) 0.0265(5) -0.0020(4) 0.0032(4) 0.0023(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_geom_angle_publ_flag
C1 O1 C2 . . 104.02(8) ?
C9 O2 C10 . . 118.37(8) ?
C1 N1 C3 . . 105.08(8) ?
N1 C1 O1 . . 114.10(9) ?
N1 C1 C16 . . 127.75(9) ?
O1 C1 C16 . . 118.12(9) ?
C3 C2 O1 . . 108.82(9) ?
C3 C2 H2 . . 125.6 ?
O1 C2 H2 . . 125.6 ?
C2 C3 N1 . . 107.97(9) ?
C2 C3 C4 . . 131.74(9) ?
N1 C3 C4 . . 120.22(9) ?
C5 C4 C9 . . 117.61(9) ?
C5 C4 C3 . . 119.87(9) ?
C9 C4 C3 . . 122.51(9) ?
C6 C5 C4 . . 121.84(10) ?
C6 C5 H5 . . 119.1 ?
C4 C5 H5 . . 119.1 ?
C5 C6 C7 . . 120.80(10) ?
C5 C6 H6 . . 119.6 ?
C7 C6 H6 . . 119.6 ?
C8 C7 C6 . . 117.83(9) ?
C8 C7 C12 . . 122.52(9) ?
C6 C7 C12 . . 119.65(9) ?
C9 C8 C7 . . 121.41(9) ?
C9 C8 H8 . . 119.3 ?
C7 C8 H8 . . 119.3 ?
O2 C9 C8 . . 123.77(9) ?
O2 C9 C4 . . 115.73(9) ?
C8 C9 C4 . . 120.49(9) ?
O2 C10 C11 . . 107.11(8) ?
O2 C10 H10A . . 110.3 ?
C11 C10 H10A . . 110.3 ?
O2 C10 H10B . . 110.3 ?
C11 C10 H10B . . 110.3 ?
H10A C10 H10B . . 108.5 ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 C7 . . 112.60(8) ?
C13 C12 C15 . . 107.80(9) ?
C7 C12 C15 . . 109.36(8) ?
C13 C12 C14 . . 108.56(9) ?
C7 C12 C14 . . 109.15(9) ?
C15 C12 C14 . . 109.32(9) ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C12 C14 H14A . . 109.5 ?
C12 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C12 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C12 C15 H15A . . 109.5 ?
C12 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C12 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C21 C16 C17 . . 114.61(9) ?
C21 C16 C1 . . 123.64(9) ?
C17 C16 C1 . . 121.75(9) ?
F1 C17 C18 . . 117.73(9) ?
F1 C17 C16 . . 118.68(9) ?
C18 C17 C16 . . 123.59(10) ?
C17 C18 C19 . . 119.12(10) ?
C17 C18 H18 . . 120.4 ?
C19 C18 H18 . . 120.4 ?
C18 C19 C20 . . 119.80(10) ?
C18 C19 H19 . . 120.1 ?
C20 C19 H19 . . 120.1 ?
C21 C20 C19 . . 119.20(10) ?
C21 C20 H20 . . 120.4 ?
C19 C20 H20 . . 120.4 ?
F2 C21 C20 . . 117.70(9) ?
F2 C21 C16 . . 118.60(9) ?
C20 C21 C16 . . 123.68(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 C17 . 1.3489(12) ?
F2 C21 . 1.3495(12) ?
O1 C1 . 1.3611(12) ?
O1 C2 . 1.3725(12) ?
O2 C9 . 1.3671(12) ?
O2 C10 . 1.4361(12) ?
N1 C1 . 1.2927(13) ?
N1 C3 . 1.4004(13) ?
C1 C16 . 1.4644(14) ?
C2 C3 . 1.3521(14) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.4664(14) ?
C4 C5 . 1.3919(14) ?
C4 C9 . 1.4049(14) ?
C5 C6 . 1.3827(15) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.3983(14) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3938(14) ?
C7 C12 . 1.5314(14) ?
C8 C9 . 1.3934(14) ?
C8 H8 . 0.9500 ?
C10 C11 . 1.5081(15) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 C13 . 1.5303(15) ?
C12 C15 . 1.5328(15) ?
C12 C14 . 1.5355(15) ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
C16 C21 . 1.3955(15) ?
C16 C17 . 1.3978(14) ?
C17 C18 . 1.3768(14) ?
C18 C19 . 1.3843(15) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.3848(16) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.3741(15) ?
C20 H20 . 0.9500 ?
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
C2 H2 O2 . 0.95 2.29 2.7807(12) 111.1 no
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
C3 N1 C1 O1 . . . . -0.50(11) ?
C3 N1 C1 C16 . . . . 177.39(9) ?
C2 O1 C1 N1 . . . . 0.39(11) ?
C2 O1 C1 C16 . . . . -177.71(9) ?
C1 O1 C2 C3 . . . . -0.11(11) ?
O1 C2 C3 N1 . . . . -0.18(11) ?
O1 C2 C3 C4 . . . . 176.69(10) ?
C1 N1 C3 C2 . . . . 0.40(11) ?
C1 N1 C3 C4 . . . . -176.89(9) ?
C2 C3 C4 C5 . . . . -162.47(11) ?
N1 C3 C4 C5 . . . . 14.08(14) ?
C2 C3 C4 C9 . . . . 15.99(17) ?
N1 C3 C4 C9 . . . . -167.46(9) ?
C9 C4 C5 C6 . . . . 0.07(15) ?
C3 C4 C5 C6 . . . . 178.60(9) ?
C4 C5 C6 C7 . . . . 0.45(16) ?
C5 C6 C7 C8 . . . . 0.16(15) ?
C5 C6 C7 C12 . . . . -178.95(9) ?
C6 C7 C8 C9 . . . . -1.30(15) ?
C12 C7 C8 C9 . . . . 177.78(9) ?
C10 O2 C9 C8 . . . . -4.80(14) ?
C10 O2 C9 C4 . . . . 176.53(9) ?
C7 C8 C9 O2 . . . . -176.75(9) ?
C7 C8 C9 C4 . . . . 1.86(15) ?
C5 C4 C9 O2 . . . . 177.51(9) ?
C3 C4 C9 O2 . . . . -0.98(14) ?
C5 C4 C9 C8 . . . . -1.20(14) ?
C3 C4 C9 C8 . . . . -179.69(9) ?
C9 O2 C10 C11 . . . . 174.49(9) ?
C8 C7 C12 C13 . . . . 3.86(14) ?
C6 C7 C12 C13 . . . . -177.08(9) ?
C8 C7 C12 C15 . . . . 123.67(10) ?
C6 C7 C12 C15 . . . . -57.26(12) ?
C8 C7 C12 C14 . . . . -116.78(11) ?
C6 C7 C12 C14 . . . . 62.29(12) ?
N1 C1 C16 C21 . . . . 156.63(11) ?
O1 C1 C16 C21 . . . . -25.56(14) ?
N1 C1 C16 C17 . . . . -23.42(16) ?
O1 C1 C16 C17 . . . . 154.39(9) ?
C21 C16 C17 F1 . . . . 179.95(9) ?
C1 C16 C17 F1 . . . . -0.01(14) ?
C21 C16 C17 C18 . . . . 0.45(15) ?
C1 C16 C17 C18 . . . . -179.51(9) ?
F1 C17 C18 C19 . . . . -179.85(9) ?
C16 C17 C18 C19 . . . . -0.35(16) ?
C17 C18 C19 C20 . . . . -0.28(16) ?
C18 C19 C20 C21 . . . . 0.77(16) ?
C19 C20 C21 F2 . . . . -178.85(10) ?
C19 C20 C21 C16 . . . . -0.67(17) ?
C17 C16 C21 F2 . . . . 178.24(9) ?
C1 C16 C21 F2 . . . . -1.81(16) ?
C17 C16 C21 C20 . . . . 0.07(16) ?
C1 C16 C21 C20 . . . . -179.98(10) ?