#------------------------------------------------------------------------------
#$Date: 2025-04-05 13:40:53 +0200 (Sat, 05 Apr 2025) $
#$Revision: 299190 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023409.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_2023409
loop_
_publ_author_name
'Mewis, Ryan E.'
'Hulme, Matthew C.'
'Marron, Jack'
'Langley, Stuart K.'
'Sutcliffe, Oliver B.'
'Benjamin, Sophie L.'
_publ_section_title
;
Synthesis and crystal structures of five fluorinated diphenidine
derivatives.
;
_journal_coeditor_code EE2011
_journal_issue 'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 229
_journal_page_last 234
_journal_paper_doi 10.1107/S2056989025001288
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C18 H22 F2 N +, Cl -'
_chemical_formula_moiety 'C18 H22 F2 N +, Cl -'
_chemical_formula_sum 'C18 H22 Cl F2 N'
_chemical_formula_weight 325.81
_chemical_name_systematic
;
tert-Butyl[1-(2,6-difluorophenyl)-2-phenylethyl]azanium chloride
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 105.044(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.3115(6)
_cell_length_b 10.5400(5)
_cell_length_c 14.8039(7)
_cell_measurement_reflns_used 8922
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 26.21
_cell_measurement_theta_min 3.01
_cell_volume 1704.48(15)
_computing_cell_refinement 'CrysAlisPro (Agilent, 2014)'
_computing_data_collection 'CrysAlisPro (Agilent, 2014)'
_computing_data_reduction 'CrysAlisPro (Agilent, 2014)'
_computing_molecular_graphics
;
X-SEED (Barbour, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur'
_diffrn_measurement_method 'scans in phi and omega'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0362
_diffrn_reflns_av_unetI/netI 0.0556
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 7223
_diffrn_reflns_theta_full 24.998
_diffrn_reflns_theta_max 24.998
_diffrn_reflns_theta_min 3.259
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.240
_exptl_absorpt_correction_T_max 0.976
_exptl_absorpt_correction_T_min 0.944
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.270
_exptl_crystal_description Block
_exptl_crystal_F_000 688
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.218
_refine_diff_density_min -0.250
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3008
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.055
_refine_ls_R_factor_all 0.0704
_refine_ls_R_factor_gt 0.0488
_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^)+(0.0303P)^2^+0.5824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0877
_refine_ls_wR_factor_ref 0.0954
_reflns_number_gt 2343
_reflns_number_total 3008
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ee2011.cif
_cod_data_source_block III
_cod_depositor_comments
'Adding full bibliography for 2023405--2023409.cif.'
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023409
_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 -3 25.3348 11.7072 3
0 0 -4 3208.88 68.4317 3
0 0 4 3105.94 66.8556 3
0 0 5 1.61232 10.9089 3
0 0 5 16.4802 22.2265 2
0 0 -5-3.83046 13.3815 3
0 0 -5 5.77539 29.9742 4
0 0 -6 2781.28 78.8184 3
0 0 6 2940.91 110.422 2
0 0 -6 2938.77 129.446 4
0 0 6 2783.71 77.1499 3
0 0 -7 3.14239 30.8876 4
0 0 7 15.0923 15.2857 3
0 0 7 41.7528 24.1094 2
0 0 -7-5.39060 13.9523 3
0 0 -8 8279.67 156.051 3
0 0 8 9253.93 156.639 3
0 0 -8 8425.03 251.907 4
0 0 8 8797.07 220.956 2
0 0 9 18.5884 24.0281 2
0 0 -9 22.2812 31.4989 4
0 0 9 7.01875 12.8753 3
0 0 9 13.7810 6.75868 5
0 0 -9 21.6938 15.2904 3
0 0 10 326.417 36.3661 3
0 0 -10 370.901 37.2727 3
0 0 -10 298.508 62.2235 4
0 0 11 11.4633 14.3826 3
0 0 -11-1.48931 31.1780 4
0 0 12 40.5343 16.4358 3
0 0 -12 57.4374 50.4203 4
0 0 -13 25.5918 33.9297 4
0 0 -14-12.0800 43.9305 4
0 0 -15 2.98038 38.6139 4
0 0 -16 558.912 109.394 4
0 0 -17 24.1806 42.5800 4
0 1 -2 38.4498 19.4546 2
0 -1 -2 24.7263 15.9462 4
0 1 -2 38.1677 15.3539 3
0 1 -3 25402.3 212.450 3
0 -1 -3 24797.4 271.284 4
0 1 4 841.231 36.8241 3
0 -1 -4 924.972 64.1987 4
0 1 -4 898.880 46.1803 3
0 -1 4 796.437 44.8486 3
0 -1 -5 1382.50 84.4723 4
0 1 -5 1206.88 54.9347 3
0 -1 5 1268.78 58.5916 3
0 1 5 1337.68 49.3102 3
0 1 6 833.941 41.3563 3
0 1 -6 767.353 48.3824 3
0 -1 -6 809.124 76.5131 4
0 -1 6 829.279 50.8857 3
0 -1 -7 2145.53 122.694 4
0 1 -7 2015.35 78.8700 3
0 1 7 2079.92 68.9935 3
0 1 7 2076.84 93.9611 2
0 -1 7 2029.96 106.171 2
0 -1 7 1898.97 79.1140 3
0 1 8 47.3452 14.9949 3
0 -1 -8 73.4160 42.5134 4
0 1 8 50.0329 26.5462 2
0 1 -8 42.7721 19.4819 3
0 -1 8 35.2166 16.7423 3
0 -1 8 84.1597 35.5397 2
0 1 -9 296.056 37.2569 3
0 -1 9 271.657 34.3965 3
0 1 9 203.812 38.7603 2
0 -1 -9 348.582 61.2759 4
0 1 9 285.368 29.3551 3
0 1 10 253.461 45.5261 2
0 1 -10 252.656 35.8684 3
0 -1 -10 254.653 60.1656 4
0 1 -10 188.580 51.9367 4
0 1 10 196.777 26.2103 3
0 1 11 1022.32 57.6003 3
0 1 -11 1091.72 114.382 4
0 -1 -11 1064.72 114.257 4
0 1 -11 1086.33 70.1841 3
0 1 12 2213.39 83.1685 3
0 1 -12 2002.69 159.899 4
0 1 -12 2228.16 102.081 3
0 -1 -12 1953.40 158.346 4
0 -1 -13-36.3133 51.8537 4
0 1 -13 38.1469 21.0751 3
0 1 -13 60.1128 45.1705 4
0 -1 -14 1639.80 159.656 4
0 1 -14 1815.95 165.346 4
0 -1 -15 177.712 73.6634 4
0 1 -15 124.749 72.7330 4
0 1 -16 107.440 65.3175 4
0 -1 -16 195.520 71.0555 4
0 -1 -17 101.763 56.5006 4
0 1 -17 180.161 76.1097 4
0 2 0 10711.8 131.709 2
0 2 -1 2193.02 71.0406 2
0 2 -2 8241.10 152.140 2
0 -2 -2 8236.32 153.580 4
0 2 -3 12174.7 186.678 3
0 2 -3 12518.8 208.076 2
0 -2 -3 12124.0 208.559 4
0 2 -4 266.344 34.7698 3
0 -2 -4 285.269 45.4690 4
0 2 -4 306.251 45.3672 2
0 -2 -5 577.173 33.3267 5
0 2 -5 543.288 46.3540 3
0 -2 -5 598.298 60.6327 4
0 2 -6 556.669 47.7183 3
0 2 6 577.923 40.0378 3
0 -2 -6 595.776 32.2249 5
0 -2 -6 543.774 68.0011 4
0 2 -7 1637.70 81.6069 3
0 -2 -7 1804.88 116.446 4
0 2 7 1728.05 68.8352 3
0 2 -8 726.489 58.0719 3
0 -2 -8 629.560 74.4998 4
0 2 8 661.334 43.7500 3
0 2 8 682.432 54.4775 2
0 -2 -9 316.618 60.5240 4
0 2 -9 299.272 41.5230 3
0 2 9 352.828 43.4064 2
0 2 9 319.543 31.0288 3
0 2 10 18.3415 13.7368 3
0 2 10 37.7655 20.8291 2
0 -2 -10-18.5526 32.3303 4
0 2 -10 38.1258 23.2292 3
0 2 11 602.830 63.1463 2
0 2 11 570.322 42.4322 3
0 -2 -11 549.021 85.4475 4
0 2 -11 584.417 57.4112 3
0 2 12 18.7222 11.5585 3
0 -2 -12 29.9002 45.0947 4
0 2 -12 55.5890 24.8970 3
0 2 -12 33.7631 45.7652 4
0 2 -13 468.748 89.0805 4
0 2 -13 521.367 56.2385 3
0 -2 -13 465.066 96.0117 4
0 2 -14 385.482 85.0655 4
0 -2 -14 380.770 84.3733 4
0 -2 -15 216.541 66.0412 4
0 2 -15 240.457 72.5495 4
0 2 -16 87.6257 68.2910 4
0 -2 -16 69.0583 50.0932 4
0 -2 -17 69.7702 71.3467 4
0 2 -17 31.3574 49.4648 4
0 3 0 0.09962 20.2395 2
0 3 -1 15250.9 214.350 2
0 3 1 15618.0 159.438 1
0 3 1 15354.3 173.342 2
0 -3 1 15625.9 216.459 2
0 3 -2 10523.2 195.971 2
0 -3 -2 10576.0 131.601 1
0 -3 -3 847.143 64.9515 4
0 3 -3 776.137 61.7372 2
0 3 -4 18959.7 283.415 3
0 3 -4 18759.2 304.479 2
0 -3 -4 18437.7 304.801 4
0 -3 -5 28.2823 32.3558 4
0 3 -5 53.3502 28.6765 3
0 3 -5-3.74240 29.6081 2
0 3 -6-14.0180 22.8942 3
0 -3 -6-23.7749 32.4891 4
0 -3 -7 3501.01 167.250 4
0 -3 -7 3775.74 99.9201 5
0 3 -7 3737.15 138.249 3
0 3 -8 2408.32 113.643 3
0 3 8 2461.76 95.0573 3
0 -3 -8 2356.01 76.3323 5
0 -3 -8 2295.91 142.248 4
0 3 9 51.6466 20.1800 2
0 3 9 69.1235 20.0940 3
0 -3 -9 60.9683 37.1598 4
0 3 -9 52.3021 27.8167 3
0 3 10 314.745 41.6918 2
0 3 -10 330.641 47.8932 3
0 -3 -10 299.786 62.6891 4
0 3 10 396.082 40.1979 3
0 -3 -11 492.978 81.0617 4
0 3 11 473.578 42.6534 3
0 3 -11 517.410 58.8439 3
0 3 11 439.992 52.7224 2
0 3 12-13.5811 15.0559 2
0 3 -12 27.0756 25.7384 3
0 -3 -13 780.526 112.801 4
0 3 -13 857.235 77.6836 3
0 -3 -14 77.2270 45.1403 4
0 3 -14 57.8818 43.1596 4
0 -3 -15 626.424 112.003 4
0 3 -15 646.523 115.826 4
0 -3 -16 325.482 91.2092 4
0 3 -16 249.345 87.9767 4
0 -3 -17 483.088 112.879 4
0 3 -17 472.315 99.6110 4
0 4 0 25425.4 286.534 2
0 4 1 128.781 24.4772 2
0 -4 1 118.533 29.5103 2
0 4 1 115.212 21.7960 1
0 4 -1 115.045 33.4007 2
0 4 -2 7293.72 180.974 2
0 -4 2 7132.37 180.284 2
0 4 2 7231.83 129.321 2
0 4 -3 1523.36 93.1463 2
0 -4 -3 1357.86 55.6531 1
0 4 -4 3638.66 141.729 3
0 -4 -4 3480.20 95.1156 1
0 -4 -4 3596.35 148.015 4
0 4 -4 3598.93 148.279 2
0 4 -5 4257.44 158.223 3
0 -4 -5 4545.29 175.891 4
0 4 -5 4386.58 169.491 2
0 4 -6 891.056 76.5108 3
0 -4 -6 934.398 88.8148 4
0 -4 -7 1213.44 102.918 4
0 4 -7 1147.90 85.9957 3
0 4 -8 5538.22 189.836 3
0 -4 -8 5865.94 148.276 5
0 -4 -8 5573.16 228.334 4
0 4 -9 9.22362 21.7817 3
0 -4 -9 77.2506 45.0005 4
0 -4 -9 8.11103 13.1115 5
0 4 9-10.1711 16.5504 3
0 4 10 4356.08 135.504 2
0 4 10 4378.93 141.887 3
0 4 -10 4273.74 174.461 3
0 -4 -10 4229.52 220.775 4
0 -4 -11 63.7658 47.6553 4
0 4 -11 78.0452 33.9316 3
0 4 11 69.5843 22.1692 3
0 4 11 82.3911 24.5803 2
0 -4 -12 907.458 118.982 4
0 4 -12 1167.95 96.1716 3
0 -4 -13 447.940 93.5733 4
0 4 -13 458.268 65.5720 3
0 -4 -14 667.952 113.870 4
0 -4 -15 348.191 93.4109 4
0 -4 -16 1120.09 151.179 4
0 4 -16 681.368 120.881 4
0 4 -17 91.4274 66.7431 4
0 -4 -17 365.813 110.684 4
0 5 0-13.0756 21.5560 2
0 5 1 594.304 49.3540 2
0 5 -1 515.921 55.2014 2
0 5 1 599.582 43.9761 1
0 5 2 13.2933 17.2166 2
0 5 2 27.3516 16.0178 1
0 -5 2 3.24505 18.8531 2
0 5 -2-19.3841 30.1505 2
0 -5 3 1684.90 101.236 2
0 5 -3 1797.40 108.225 2
0 5 3 1780.05 68.8329 2
0 -5 -4 5291.91 121.131 1
0 5 -4 5140.91 186.227 3
0 5 -4 5563.13 193.127 2
0 5 -5 1032.86 93.0069 2
0 5 -5 1159.85 91.9879 3
0 -5 -5 1180.08 100.044 4
0 -5 -5 1112.67 60.9196 1
0 5 -6 942.810 87.9980 3
0 -5 -6 1038.70 97.7372 4
0 -5 -7 1269.34 109.842 4
0 5 -7 1126.63 94.5322 3
0 5 -8 891.824 86.9268 3
0 -5 -8 714.363 88.8019 4
0 5 -9 3.97264 26.4619 3
0 -5 -9 49.3753 21.7741 5
0 -5 -9 38.3265 43.0599 4
0 5 -10 65.8924 35.7549 3
0 -5 -10 12.8538 41.4802 4
0 5 10 71.7408 20.2671 2
0 -5 -11 80.9391 46.7308 4
0 5 -11 77.9839 40.3537 3
0 5 -12 376.143 63.0563 3
0 -5 -12 347.865 84.0901 4
0 -5 -13 35.7577 45.2460 4
0 5 -13 92.3590 39.6519 3
0 -5 -14 731.038 121.626 4
0 5 -14 720.088 86.9256 3
0 -5 -15 64.4917 62.7375 4
0 -5 -16-10.3386 53.1514 4
0 6 0 2811.51 120.926 2
0 6 -1 53.4312 30.0031 2
0 6 1 6.22885 18.9059 2
0 6 1-2.65240 15.5929 1
0 6 2 68.0956 18.9234 1
0 6 -2 53.4367 33.5251 2
0 6 2 79.9207 23.2905 2
0 6 -3 742.381 74.0436 2
0 6 3 925.578 57.7968 2
0 6 -4 40.9576 30.0356 3
0 6 -4 65.6191 40.1963 2
0 6 4 27.8952 15.7712 2
0 6 -5 1138.59 100.487 3
0 6 5 1166.88 55.9531 2
0 6 -5 1374.84 113.447 2
0 -6 -6 549.566 46.4669 1
0 6 -6 523.650 71.9782 3
0 -6 -7 830.133 97.9007 4
0 6 -7 766.234 87.3159 3
0 -6 -7 869.451 62.0106 1
0 6 -8 1424.27 116.782 3
0 -6 -8 1528.07 131.764 4
0 6 -9 24.5602 30.6251 3
0 -6 -9 10.9842 38.9897 4
0 -6 -9-5.53077 19.2589 5
0 6 -10 866.671 95.6248 3
0 -6 -10 1063.62 121.799 4
0 -6 -11 547.353 93.5415 4
0 6 -11 685.195 86.3788 3
0 -6 -12 70.9664 48.7026 4
0 6 -12 8.36449 32.6579 3
0 6 -13 448.575 75.3715 3
0 -6 -13 281.266 72.3155 4
0 -6 -14 181.197 66.7448 4
0 6 -14 172.318 54.0568 3
0 -6 -15 14.7874 47.6301 4
0 -6 -16 42.7933 49.0558 4
0 7 0 51.8254 31.4445 2
0 7 1 7133.54 194.351 2
0 7 -1 6986.66 214.258 2
0 7 1 6838.17 170.060 1
0 7 -2 312.978 49.2624 2
0 7 2 474.544 45.5500 1
0 7 2 397.446 46.5058 2
0 7 3 2053.97 92.3985 2
0 7 -3 1938.58 126.502 2
0 7 4 388.558 40.6908 2
0 7 -4 453.386 72.3386 2
0 7 -4 285.364 59.5582 3
0 7 5 22.7216 15.2962 2
0 7 -5 34.9774 39.9839 2
0 7 -5 24.6460 36.6380 3
0 7 6 4248.35 106.385 2
0 7 -6 3830.58 196.864 3
0 -7 -7 1844.16 88.2443 1
0 7 -7 1798.80 137.179 3
0 7 7 1818.25 63.8810 2
0 7 8 1227.52 48.0752 2
0 7 -8 1321.96 118.894 3
0 7 -9 141.467 46.7584 3
0 -7 -10-6.20645 35.0309 4
0 7 -10-2.81992 34.7628 3
0 -7 -11 1155.95 137.832 4
0 7 -11 1126.71 115.941 3
0 -7 -12-33.9995 54.5129 4
0 7 -12 29.4601 41.6778 3
0 -7 -13 31.6505 49.6638 4
0 7 -13 50.2874 41.0331 3
0 7 -14 109.806 46.0252 3
0 -7 -14 11.6266 50.2313 4
0 -7 -15 779.934 137.247 4
0 8 0 770.345 77.8787 2
0 8 -1 1371.23 102.760 2
0 8 1 1524.20 87.7300 1
0 8 1 1458.02 96.7678 2
0 8 -2 24.4695 31.9128 2
0 8 2 78.9471 25.3961 1
0 8 2 65.4794 26.8521 2
0 8 -3 2844.54 159.954 2
0 8 3 2506.04 112.210 2
0 8 -4 254.227 64.0411 2
0 8 4 324.329 41.1980 2
0 8 -4 285.241 63.8275 3
0 8 -5 818.091 98.2646 3
0 8 5 799.100 55.8179 2
0 8 6 4354.33 115.628 2
0 8 -6 4329.95 224.381 3
0 8 7 1054.80 50.1782 2
0 8 -7 938.660 108.705 3
0 8 -8 1429.24 132.466 3
0 8 -9-24.3849 33.3098 3
0 8 -10 294.368 70.2011 3
0 8 -11 29.6915 33.5773 3
0 8 -12 276.640 68.5532 3
0 -8 -13 352.995 93.7248 4
0 8 -13 321.999 78.1090 3
0 8 -14 162.644 59.3071 3
0 -8 -14 145.528 74.7181 4
0 9 0 18.0579 18.7884 1
0 9 0 26.9905 33.3327 2
0 9 1 450.257 62.0621 2
0 9 1 475.435 54.1148 1
0 9 -1 383.973 60.8189 2
0 9 2 532.537 53.7171 1
0 9 -2 559.990 75.7644 2
0 9 2 463.772 57.1757 2
0 9 -3 85.4017 42.9032 2
0 9 3 127.195 32.8690 2
0 9 4 58.1017 22.0273 2
0 9 -4 23.2171 37.4083 3
0 9 -4 24.3975 46.6258 2
0 9 -5 828.234 106.000 3
0 9 5 1072.66 68.7311 2
0 9 -6 884.542 112.180 3
0 9 -7 136.535 53.1194 3
0 9 -8 633.546 98.0488 3
0 9 -9-31.5621 47.5094 3
0 9 -10-7.08317 36.4342 3
0 9 -11 376.728 85.8042 3
0 9 -12-36.8554 34.9988 3
0 9 -13 28.1073 52.6907 3
0 10 0 6248.41 205.674 1
0 10 0 6511.42 241.608 2
0 10 1 165.322 46.3327 2
0 10 -1 140.602 47.5703 2
0 10 1 133.108 33.2374 1
0 10 -2 190.659 56.9258 2
0 10 2 131.557 36.3834 2
0 10 -3 2052.99 169.065 3
0 10 3 1991.32 115.511 2
0 10 -4 229.072 73.0156 3
0 10 4 278.598 46.2950 2
0 10 -5 838.165 117.859 3
0 10 -6 1411.80 148.656 3
0 10 -7 3.74248 42.8357 3
0 10 -8 230.823 68.3075 3
0 10 -9 90.4653 59.1239 3
0 10 -10 27.9976 38.1697 3
0 10 -11 390.775 87.8806 3
0 10 -12 86.5319 59.3673 3
0 10 -13 42.6823 43.3068 3
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12 1 -4 449.697 93.5441 5
12 -1 -3 402.832 94.0702 5
12 1 -3 470.033 104.553 5
12 -1 -2 58.4492 51.2276 5
12 1 -2 163.435 67.8030 5
12 -1 -1 344.725 94.1154 5
12 1 -1 254.211 81.4125 5
12 1 0 196.039 68.7985 5
12 -1 0 342.886 85.5545 5
12 1 1 97.4556 65.6844 5
12 -1 1 123.150 71.1445 5
12 -1 2 900.862 135.642 5
12 1 2 678.269 114.768 5
12 -1 3 300.110 85.1568 5
12 1 3 117.203 64.6722 5
12 -1 4 109.268 60.9352 5
12 1 4 77.3242 64.4664 5
12 -1 5 196.730 73.3057 5
12 1 5 154.229 61.5007 5
12 -1 6 53.7140 55.2136 5
12 1 6 119.451 66.2889 5
12 1 7 56.4969 45.3976 5
12 2 -15 1393.83 156.995 2
12 2 -15 1677.57 170.605 1
12 2 -14 11.9704 34.7508 2
12 2 -14 62.7691 50.5395 1
12 2 -13 656.874 106.170 1
12 2 -12 575.974 97.3106 1
12 -2 -12 538.621 89.5926 5
12 -2 -11 185.635 60.0329 5
12 2 -11 100.583 60.6493 1
12 -2 -10 178.675 61.7079 5
12 2 -10 145.320 54.9224 1
12 2 -10 149.987 56.9324 5
12 -2 -9 554.599 98.9167 5
12 2 -9 741.467 113.798 5
12 -2 -8 256.174 67.4615 5
12 2 -8 247.971 68.6845 5
12 -2 -7 268.718 74.5732 5
12 2 -7 433.432 94.2755 5
12 -2 -6 351.070 84.1186 5
12 2 -6 470.010 92.8254 5
12 -2 -5 109.233 57.2412 5
12 2 -5 41.6390 51.7727 5
-12 2 4 221.412 67.5404 3
12 2 -4 162.820 73.2550 5
-12 2 3 523.836 96.5449 3
12 2 -3 493.105 101.819 5
-12 2 2 75.9670 44.0019 3
12 2 -2 164.609 67.1878 5
-12 2 1 1010.23 134.951 3
12 2 -1 1024.83 138.799 5
-12 2 0 254.766 79.2691 3
12 2 0 134.903 69.3026 5
-12 2 -1 2041.66 186.438 3
12 2 1 2080.56 197.326 5
-12 2 -2 194.631 77.7718 3
12 2 2 144.914 67.7425 5
-12 2 -3 738.345 121.352 3
12 2 3 733.782 118.455 5
-12 2 -4 23.0827 60.3642 3
12 2 4 51.3431 73.0976 5
12 -2 5 90.5583 61.7459 5
-12 2 -5-42.4469 43.5992 3
12 2 5 85.0664 61.1661 5
12 -2 6 160.977 75.2455 5
12 2 6 49.8612 47.8793 5
12 2 7 484.700 101.395 5
12 3 -15 451.650 98.9359 2
12 3 -14 387.923 86.9877 1
12 3 -14 474.543 97.8146 2
12 3 -13 249.396 80.7775 2
12 3 -13 57.3561 45.2156 1
12 3 -12 45.9801 39.7454 1
12 -3 -11 576.877 97.8491 5
12 3 -11 747.389 113.826 1
12 -3 -10 113.797 51.1102 5
12 3 -10 115.937 52.5334 1
12 -3 -9 57.1475 53.1698 5
12 3 -9 33.0197 44.2103 1
12 -3 -8 763.262 114.554 5
-12 3 7 287.226 67.0559 3
12 3 -7 238.351 80.6763 5
-12 3 6 63.7673 54.2186 3
12 3 -6 46.6634 52.0853 5
-12 3 5 1131.29 129.049 3
12 3 -5 1243.23 147.218 5
-12 3 4 0.43524 38.2266 3
12 3 -4 124.756 57.7993 5
-12 3 3 371.865 84.5556 3
12 3 -3 477.315 97.5392 5
-12 3 2 373.263 88.3723 3
12 3 -2 328.306 91.8949 5
-12 3 1 1563.36 163.142 3
12 3 -1 1812.71 180.425 5
-12 3 0 128.739 58.3716 3
12 3 0 166.608 80.5199 5
-12 3 -1 22.1193 56.3927 3
12 3 1 34.8587 47.7291 5
-12 3 -2 67.6583 61.8903 3
12 3 2-40.3781 47.0835 5
-12 3 -3 127.808 61.0104 3
12 3 3 95.6069 53.1432 5
-12 3 -4 79.4434 63.8940 3
12 3 4-16.7685 46.7528 5
12 3 5 68.0030 57.1854 5
12 3 6 71.2415 60.1775 5
12 4 -13 469.923 102.237 2
12 4 -13 258.685 70.9665 1
12 4 -12 775.094 120.070 1
12 -4 -11 7.63216 37.4849 5
12 4 -11 315.687 76.4785 1
12 4 -10 220.083 74.3883 1
12 4 -9 42.6264 58.1971 1
-12 4 9 3.75403 32.0675 3
-12 4 8 64.1483 42.0929 3
-12 4 7-2.16578 33.2206 3
-12 4 6 275.064 72.4167 3
-12 4 5 188.433 58.8277 3
-12 4 4 575.969 98.1365 3
-12 4 3 265.906 86.2281 3
12 4 -3 201.423 81.0613 5
-12 4 2 179.314 65.3241 3
12 4 -2 93.8514 63.0704 5
-12 4 1-7.37411 45.6561 3
12 4 -1 14.9598 45.7603 5
-12 4 0-48.5605 54.8548 3
12 4 0 43.8263 49.6574 5
-12 4 -1 100.444 67.2803 3
12 4 1 149.600 84.9378 5
-12 4 -2 468.322 96.0448 3
12 4 2 601.817 113.115 5
-12 4 -3 135.467 80.3318 3
12 4 3 9.77477 50.5329 5
12 4 4 383.091 97.6101 5
12 4 5 521.915 110.350 5
12 5 -11 165.760 72.6603 1
12 5 -10 215.695 76.2451 1
12 5 -9 44.3687 46.2532 1
-12 5 9 47.4260 40.7788 3
-12 5 8 1100.92 124.434 3
12 5 -8 995.274 136.108 1
-12 5 7-40.2955 39.5445 3
-12 5 6 234.799 66.0022 3
-12 5 5 163.986 67.0552 3
-12 5 4 38.0041 45.3196 3
-12 5 3 213.246 63.0244 3
-12 5 2 21.1094 43.8360 3
-12 5 1-9.37465 52.4426 3
-12 5 0 279.039 78.1892 3
-12 5 -1 161.559 64.7661 3
-12 5 -2 1912.22 198.470 3
12 6 -9 1398.37 162.651 1
12 6 -8 140.164 62.5604 1
-12 6 8 45.6450 45.6220 3
-12 6 7 1603.20 155.233 3
-12 6 6 501.851 89.1553 3
-12 6 5 206.086 66.9659 3
-12 6 4 247.699 79.5843 3
-12 6 3-3.85536 44.6434 3
-12 6 2 339.973 92.0458 3
-12 6 1 304.837 93.6643 3
-12 6 0 84.6858 68.6189 3
-12 6 -1 636.700 119.160 3
-12 7 8 168.937 58.1739 3
-12 7 7 132.103 60.2869 3
-12 7 6 29.0506 35.8896 3
-12 7 5 752.855 119.411 3
-12 7 4 223.038 77.0116 3
-12 7 3-22.6613 35.4423 3
-12 7 2 80.9400 52.1190 3
-12 7 1 58.5826 52.1836 3
-12 8 7-66.9378 47.6819 3
-12 8 6 129.056 57.6395 3
-12 8 5 192.187 71.0034 3
-12 8 4 414.328 93.3350 3
-12 9 7-7.60507 47.1077 3
13 0 -12 69.9316 49.9398 5
13 0 -11 67.0448 60.3769 5
13 0 -10 661.996 111.843 5
13 0 -9 61.0676 56.8451 5
13 0 -8 211.103 73.4014 5
13 0 -7 127.527 69.5818 5
13 0 -6-25.0100 37.3840 5
13 0 -5 94.3989 63.8617 5
13 0 -4 786.938 121.972 5
13 0 -3-41.8619 56.2387 5
13 0 -2 496.159 104.958 5
13 0 -1 30.0895 45.9429 5
13 0 0 14.3156 61.8199 5
13 0 1 21.3797 61.8078 5
13 0 2 77.3306 62.2903 5
13 0 3 27.7138 52.7991 5
13 1 -14 577.299 102.139 1
13 1 -13 72.1202 44.4204 1
13 -1 -12 17.8190 34.9813 5
13 1 -11 310.426 79.3954 5
13 -1 -11 444.428 90.9774 5
13 1 -10 160.521 68.2812 5
13 -1 -10 165.413 62.5045 5
13 1 -9 123.370 57.9336 5
13 -1 -9 90.7048 57.1939 5
13 -1 -8 338.890 86.3547 5
13 1 -8 403.837 90.0082 5
13 -1 -7 102.222 59.4932 5
13 1 -7 73.2353 48.8562 5
13 -1 -6 58.1129 62.7659 5
13 1 -6 43.5838 62.3050 5
13 -1 -5 150.162 71.0984 5
13 1 -5 10.6619 44.0507 5
13 -1 -4 122.801 63.2379 5
13 1 -4 483.161 110.005 5
13 -1 -3 205.005 78.4749 5
13 1 -3 170.891 62.3893 5
13 -1 -2 108.100 82.4786 5
13 1 -2 91.8825 79.0309 5
13 -1 -1 49.6973 50.8126 5
13 1 -1 11.9693 38.8343 5
13 -1 0 171.821 75.8501 5
13 1 0 276.621 88.1100 5
13 -1 1 58.3209 50.0994 5
13 1 1 79.5693 57.7648 5
13 -1 2 219.991 86.7954 5
13 1 2 88.6006 53.4467 5
13 -1 3 167.330 69.0205 5
13 1 3 113.678 58.1468 5
13 2 -14 2.88748 48.9796 2
13 2 -14 99.8816 54.6047 1
13 2 -13-50.4034 40.0452 1
13 2 -12 41.7121 35.3168 1
13 -2 -11 162.508 69.0249 5
13 -2 -10 93.5291 58.8569 5
13 2 -10 34.1386 53.5476 5
13 -2 -9 29.4418 50.3878 5
13 2 -9 149.977 69.8708 5
13 -2 -8 119.150 55.5001 5
13 2 -8 216.589 70.0242 5
13 -2 -7 363.448 94.4507 5
13 2 -7 172.191 68.3809 5
13 -2 -6 71.4920 58.2498 5
13 2 -6 136.377 74.4334 5
13 -2 -5 446.998 97.6857 5
13 2 -5 363.613 88.9304 5
13 -2 -4 62.2567 51.7884 5
13 2 -4 73.8731 61.3594 5
13 -2 -3 87.0071 62.6004 5
13 2 -3 7.21235 48.3301 5
13 -2 -2 201.655 76.1778 5
13 2 -2 322.571 86.9383 5
13 -2 -1 586.090 115.492 5
-13 2 1 573.090 109.112 3
13 2 -1 593.365 120.769 5
13 -2 0 64.3202 66.0314 5
-13 2 0 21.2027 55.1524 3
13 2 0 149.802 80.7638 5
13 -2 1 240.155 77.3112 5
-13 2 -1 270.570 74.6151 3
13 2 1 476.223 108.645 5
13 -2 2 41.6708 55.2378 5
-13 2 -2 84.3242 53.1689 3
13 2 2 161.937 73.8568 5
13 3 -12 97.3164 57.0472 1
13 -3 -11 1172.69 143.241 5
13 3 -11 1176.41 144.141 1
13 -3 -10 253.745 73.6966 5
13 -3 -9 163.700 63.7274 5
13 -3 -8 183.564 73.7787 5
13 -3 -7-62.2440 43.1748 5
13 3 -7 69.0836 53.3196 5
-13 3 6 416.355 88.4591 3
13 3 -6 163.199 76.5658 5
-13 3 5 18.3061 41.8997 3
13 3 -5 69.5478 64.5744 5
-13 3 4 269.314 73.9750 3
13 3 -4 180.573 66.3369 5
-13 3 3 146.968 69.7570 3
13 3 -3 157.917 77.9068 5
-13 3 2 104.362 62.1704 3
13 3 -2 170.075 69.4254 5
-13 3 1-52.9578 49.7051 3
13 3 -1 157.551 78.7311 5
-13 3 0 113.279 70.1381 3
13 3 0 267.102 93.6103 5
-13 3 -1 24.2292 53.3102 3
13 3 1 33.5703 59.5552 5
13 -4 -11 60.9188 51.2984 5
13 4 -10 250.755 74.8791 1
13 -4 -10 194.357 70.7545 5
13 -4 -9 76.1788 44.8595 5
-13 4 8 27.3637 36.3741 3
-13 4 7 117.020 56.0141 3
-13 4 6 147.462 66.7384 3
-13 4 5 398.977 86.2007 3
-13 4 4 330.076 83.3049 3
-13 4 3 19.5136 43.9258 3
13 4 -3 167.397 79.6297 5
-13 4 2 199.488 76.3431 3
13 4 -2 249.532 82.6491 5
-13 4 1 209.565 79.5208 3
13 4 -1 244.819 92.7633 5
-13 4 0 177.318 65.6145 3
13 4 0 10.6282 67.5863 5
-13 5 8 16.7160 30.0181 3
-13 5 7 32.5198 48.3673 3
-13 5 6 208.549 68.6319 3
-13 5 5 23.9466 45.9555 3
-13 5 4 617.375 109.522 3
-13 5 3 231.159 77.1062 3
-13 5 2 133.079 72.0367 3
-13 5 1 140.824 76.2717 3
-13 6 8 60.1745 38.9765 3
-13 6 7 290.313 80.9258 3
-13 6 6 96.0602 59.9268 3
-13 6 5 225.861 71.7785 3
-13 6 4 117.734 72.9005 3
-13 6 3 545.465 106.271 3
-13 7 7-56.0193 52.1213 3
-13 7 6 120.939 54.6833 3
-13 7 5 218.847 76.1396 3
14 0 -11 8.50833 41.0662 5
14 0 -10 333.163 85.4072 5
14 0 -9 5.33549 44.7221 5
14 0 -8 54.8322 48.4667 5
14 0 -7 48.9281 55.5967 5
14 0 -6 324.680 94.0636 5
14 0 -5 36.9600 62.6786 5
14 0 -4 123.300 77.0024 5
14 0 -3 58.1192 56.1162 5
14 1 -11 89.3689 63.7720 5
14 -1 -11 150.247 66.5438 5
14 1 -10 675.316 121.119 5
14 -1 -10 758.298 127.923 5
14 1 -9 88.2364 65.6015 5
14 -1 -9 82.8569 66.3061 5
14 1 -8 140.542 69.6593 5
14 -1 -8 146.341 63.0447 5
14 -1 -7-15.4376 46.2089 5
14 1 -7 54.0790 63.5415 5
14 -1 -6 441.645 102.413 5
14 1 -6 379.046 98.7661 5
14 -1 -5 8.60894 55.0774 5
14 1 -5 47.5906 44.9333 5
14 -1 -4 309.044 89.4378 5
14 1 -4 130.329 84.5261 5
14 -1 -3 197.822 77.6257 5
14 1 -3 177.610 80.6400 5
14 -2 -11-11.4640 47.1348 5
14 2 -10 68.4588 53.6627 5
14 -2 -10 83.4596 57.2297 5
14 -2 -9 77.9688 65.7152 5
14 2 -9 151.130 69.6158 5
14 -2 -8 121.005 69.5154 5
14 2 -8 69.4442 52.7060 5
14 -2 -7 150.340 70.7494 5
14 2 -7 67.8251 55.3933 5
14 -2 -6 28.2758 52.4512 5
14 2 -6 60.2812 66.7702 5
14 -2 -5 39.3952 60.2901 5
14 2 -5 164.614 86.4200 5
14 -2 -4 257.557 81.3224 5
14 2 -4 230.239 79.7589 5
14 -3 -11 167.710 67.2047 5
14 -3 -10 239.485 74.9212 5
14 -3 -9 929.350 142.828 5
14 -3 -8 31.2426 44.7935 5
14 -3 -7 475.068 111.521 5
14 3 -7 214.269 86.1970 5
14 -3 -6 68.4133 68.7312 5
14 -3 -5 213.145 99.1427 5
-14 3 3 80.5733 57.6517 3
14 -4 -10 199.313 73.3002 5
14 -4 -9 95.8367 60.3484 5
14 -4 -8 376.879 101.286 5
-14 4 6 175.368 65.5268 3
-14 4 5 159.728 74.6333 3
-14 4 4-13.1900 42.6633 3
-14 5 7 51.3997 49.4463 3
-14 5 6 79.1543 51.0366 3
-14 5 5 105.125 54.9680 3
-14 6 7 27.1461 34.7084 3
0 0 0 0.00 0.00 0
TITL OS-3-a in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 11.311491 10.539971 14.803916 90.0000 105.0436 90.0000
ZERR 5.00 0.000584 0.000467 0.000670 0.0000 0.0047 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N F
UNIT 90.00 105.00 5.00 10.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 13919
_shelx_res_file
;
REM reset to P21/c #14
REM
REM
REM
REM OS-3-a in P21/c #14
REM R1 = 0.0586 for 2786 Fo > 4sig(Fo) and 0.0882 for all 3759 data
REM 202 parameters refined using 0 restraints
REM Highest difference peak 0.273, deepest hole -0.244, 1-sigma level 0.055
REM OS-3-a in P21/c #14
REM wR2 = 0.0943, GooF = S = 1.057, Restrained GooF = 1.057 for all data
REM R1 = 0.0491 for 2343 Fo > 4sig(Fo) and 0.0706 for all 3008 data
REM 202 parameters refined using 0 restraints
REM Highest difference peak 0.219, deepest hole -0.246, 1-sigma level 0.047
TITL OS-3-a in P21/c #14
C:\Users\stula\Desktop\OS5-II~1\OS5.res
created by SHELXL-2018/3 at 10:25:23 on 29-Jan-2025
CELL 0.71073 11.3115 10.5400 14.8039 90.000 105.044 90.000
ZERR 4.0000 0.0006 0.0005 0.0007 0.000 0.005 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H CL F N
UNIT 72 88 4 8 4
MERG 2
OMIT -2 50
SHEL 7.00 0.77
FMAP 2
GRID
PLAN 5
TEMP -100
BOND $H
HTAB N1 CL1
HTAB N1 CL1_$1
EQIV $1 1-X, 2-Y, -Z
L.S. 20
ACTA
WGHT 0.030300 0.582400
FVAR 1.57038
CL1 3 0.390367 1.139815 0.055849 11.00000 0.03052 0.01863 =
0.02607 0.00235 0.01148 0.00416
F1 4 0.098566 0.740338 0.101061 11.00000 0.02961 0.03638 =
0.04187 0.00090 0.02016 0.00014
F2 4 0.399937 0.601872 -0.041669 11.00000 0.03834 0.02761 =
0.03629 0.00038 0.01904 0.00649
N1 5 0.418204 0.845748 0.066644 11.00000 0.02221 0.01323 =
0.01720 0.00113 0.00626 0.00094
C1 1 0.595095 0.888857 0.195953 11.00000 0.02478 0.02860 =
0.02047 0.00373 0.00210 -0.00096
AFIX 137
H1C 2 0.648652 0.862937 0.156776 11.00000 -1.50000
H1D 2 0.636607 0.873592 0.261856 11.00000 -1.50000
H1E 2 0.576024 0.979356 0.186458 11.00000 -1.50000
AFIX 0
C2 1 0.390388 0.851796 0.227614 11.00000 0.03019 0.03200 =
0.01858 -0.00080 0.00813 -0.00250
AFIX 137
H2A 2 0.367671 0.941068 0.215264 11.00000 -1.50000
H2B 2 0.431267 0.840815 0.294127 11.00000 -1.50000
H2C 2 0.316581 0.799009 0.211062 11.00000 -1.50000
AFIX 0
C3 1 0.506913 0.671568 0.180503 11.00000 0.03291 0.02316 =
0.02049 0.00607 0.00214 0.00242
AFIX 137
H3A 2 0.430789 0.622529 0.168216 11.00000 -1.50000
H3B 2 0.555718 0.655092 0.244475 11.00000 -1.50000
H3C 2 0.553596 0.646429 0.136139 11.00000 -1.50000
AFIX 0
C4 1 0.476885 0.812153 0.169149 11.00000 0.02130 0.02096 =
0.01422 0.00349 0.00205 0.00025
C5 1 0.286381 0.813997 0.020290 11.00000 0.01979 0.01682 =
0.01957 0.00061 0.00560 0.00248
AFIX 13
H5 2 0.234618 0.867019 0.050999 11.00000 -1.20000
AFIX 0
C6 1 0.252682 0.677700 0.030349 11.00000 0.01974 0.01912 =
0.01507 0.00198 0.00192 0.00009
C7 1 0.159624 0.644801 0.071467 11.00000 0.02069 0.02521 =
0.02254 0.00102 0.00295 0.00066
C8 1 0.127290 0.521872 0.084814 11.00000 0.03022 0.03399 =
0.03168 0.00747 0.00514 -0.01005
AFIX 43
H8 2 0.064723 0.504267 0.115178 11.00000 -1.20000
AFIX 0
C9 1 0.187441 0.424973 0.053280 11.00000 0.04286 0.02147 =
0.03384 0.00694 -0.00315 -0.01131
AFIX 43
H9 2 0.166274 0.339447 0.061977 11.00000 -1.20000
AFIX 0
C10 1 0.278413 0.450636 0.009044 11.00000 0.03891 0.01816 =
0.03155 -0.00054 -0.00034 0.00241
AFIX 43
H10 2 0.319903 0.384076 -0.013306 11.00000 -1.20000
AFIX 0
C11 1 0.306771 0.575093 -0.001510 11.00000 0.02640 0.02420 =
0.01978 0.00191 0.00612 0.00086
C12 1 0.260038 0.857286 -0.081928 11.00000 0.02275 0.02093 =
0.01970 0.00407 0.00471 0.00039
AFIX 23
H12A 2 0.290438 0.944996 -0.084222 11.00000 -1.20000
H12B 2 0.304422 0.801691 -0.115937 11.00000 -1.20000
AFIX 0
C13 1 0.124742 0.852940 -0.129478 11.00000 0.02407 0.02125 =
0.01707 0.00545 0.00586 -0.00028
C14 1 0.048861 0.949340 -0.114996 11.00000 0.03258 0.02724 =
0.03468 -0.00439 -0.00051 0.00427
AFIX 43
H14 2 0.082380 1.018435 -0.075390 11.00000 -1.20000
AFIX 0
C15 1 -0.075199 0.946252 -0.157512 11.00000 0.03264 0.04591 =
0.05128 -0.00130 0.00472 0.01660
AFIX 43
H15 2 -0.126360 1.013158 -0.147073 11.00000 -1.20000
AFIX 0
C16 1 -0.125009 0.846538 -0.214984 11.00000 0.02259 0.05221 =
0.04568 0.00007 0.00152 0.00008
AFIX 43
H16 2 -0.210343 0.844521 -0.244199 11.00000 -1.20000
AFIX 0
C17 1 -0.050876 0.750339 -0.229782 11.00000 0.03560 0.04078 =
0.03046 -0.01058 0.00241 -0.00995
AFIX 43
H17 2 -0.084782 0.681460 -0.269479 11.00000 -1.20000
AFIX 0
C18 1 0.073844 0.753298 -0.186838 11.00000 0.02721 0.02802 =
0.02776 -0.00183 0.00862 0.00146
AFIX 43
H18 2 0.124631 0.685936 -0.197099 11.00000 -1.20000
AFIX 0
H1A 2 0.422693 0.932662 0.064769 11.00000 0.02014
H1B 2 0.470892 0.817806 0.030199 11.00000 0.03328
HKLF 4
REM OS-3-a in P21/c #14
REM wR2 = 0.0954, GooF = S = 1.055, Restrained GooF = 1.055 for all data
REM R1 = 0.0488 for 2343 Fo > 4sig(Fo) and 0.0704 for all 3008 data
REM 210 parameters refined using 0 restraints
END
WGHT 0.0265 0.6363
REM Highest difference peak 0.218, deepest hole -0.250, 1-sigma level 0.047
Q1 1 0.4019 1.0770 -0.0043 11.00000 0.05 0.22
Q2 1 0.1046 0.8283 -0.1837 11.00000 0.05 0.21
Q3 1 0.3095 0.6407 0.0457 11.00000 0.05 0.20
Q4 1 0.4179 0.8534 0.1837 11.00000 0.05 0.19
Q5 1 0.4405 0.8150 0.1244 11.00000 0.05 0.19
;
_shelx_res_checksum 60970
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cl Cl1 0.39037(5) 1.13981(5) 0.05585(4) 0.02430(17) Uani d 1 . .
F F1 0.09857(12) 0.74034(14) 0.10106(9) 0.0339(4) Uani d 1 . .
F F2 0.39994(13) 0.60187(13) -0.04167(9) 0.0323(4) Uani d 1 . .
N N1 0.41820(17) 0.84575(19) 0.06664(12) 0.0173(4) Uani d 1 . .
C C1 0.5951(2) 0.8889(2) 0.19595(15) 0.0253(6) Uani d 1 . .
H H1C 0.648652 0.862937 0.156776 0.038 Uiso calc 1 . .
H H1D 0.636607 0.873592 0.261856 0.038 Uiso calc 1 . .
H H1E 0.576024 0.979356 0.186458 0.038 Uiso calc 1 . .
C C2 0.3904(2) 0.8518(2) 0.22761(15) 0.0266(6) Uani d 1 . .
H H2A 0.367671 0.941068 0.215264 0.040 Uiso calc 1 . .
H H2B 0.431267 0.840815 0.294127 0.040 Uiso calc 1 . .
H H2C 0.316581 0.799009 0.211062 0.040 Uiso calc 1 . .
C C3 0.5069(2) 0.6716(2) 0.18050(15) 0.0264(6) Uani d 1 . .
H H3A 0.430789 0.622529 0.168216 0.040 Uiso calc 1 . .
H H3B 0.555718 0.655092 0.244475 0.040 Uiso calc 1 . .
H H3C 0.553596 0.646429 0.136139 0.040 Uiso calc 1 . .
C C4 0.4769(2) 0.8122(2) 0.16915(14) 0.0193(5) Uani d 1 . .
C C5 0.2864(2) 0.8140(2) 0.02029(14) 0.0186(5) Uani d 1 . .
H H5 0.234618 0.867019 0.050999 0.022 Uiso calc 1 . .
C C6 0.2527(2) 0.6777(2) 0.03035(14) 0.0185(5) Uani d 1 . .
C C7 0.1596(2) 0.6448(2) 0.07147(15) 0.0233(5) Uani d 1 . .
C C8 0.1273(2) 0.5219(3) 0.08481(17) 0.0325(6) Uani d 1 . .
H H8 0.064723 0.504267 0.115178 0.039 Uiso calc 1 . .
C C9 0.1874(2) 0.4250(3) 0.05328(17) 0.0352(7) Uani d 1 . .
H H9 0.166274 0.339447 0.061977 0.042 Uiso calc 1 . .
C C10 0.2784(2) 0.4506(2) 0.00904(17) 0.0313(6) Uani d 1 . .
H H10 0.319903 0.384076 -0.013306 0.038 Uiso calc 1 . .
C C11 0.3068(2) 0.5751(2) -0.00151(15) 0.0234(6) Uani d 1 . .
C C12 0.2600(2) 0.8573(2) -0.08193(14) 0.0213(5) Uani d 1 . .
H H12A 0.290438 0.944996 -0.084222 0.026 Uiso calc 1 . .
H H12B 0.304422 0.801691 -0.115937 0.026 Uiso calc 1 . .
C C13 0.1247(2) 0.8529(2) -0.12948(14) 0.0207(5) Uani d 1 . .
C C14 0.0489(2) 0.9493(3) -0.11500(17) 0.0332(6) Uani d 1 . .
H H14 0.082380 1.018435 -0.075390 0.040 Uiso calc 1 . .
C C15 -0.0752(3) 0.9463(3) -0.15751(19) 0.0444(8) Uani d 1 . .
H H15 -0.126360 1.013158 -0.147073 0.053 Uiso calc 1 . .
C C16 -0.1250(2) 0.8465(3) -0.21498(19) 0.0415(7) Uani d 1 . .
H H16 -0.210343 0.844521 -0.244199 0.050 Uiso calc 1 . .
C C17 -0.0509(2) 0.7503(3) -0.22978(17) 0.0368(7) Uani d 1 . .
H H17 -0.084782 0.681460 -0.269479 0.044 Uiso calc 1 . .
C C18 0.0738(2) 0.7533(2) -0.18684(15) 0.0274(6) Uani d 1 . .
H H18 0.124631 0.685936 -0.197099 0.033 Uiso calc 1 . .
H H1A 0.423(2) 0.933(2) 0.0648(15) 0.020(6) Uiso d 1 . .
H H1B 0.471(2) 0.818(2) 0.0302(16) 0.033(7) 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
Cl1 0.0305(3) 0.0186(3) 0.0261(3) 0.0042(3) 0.0115(2) 0.0024(3)
F1 0.0296(8) 0.0364(9) 0.0419(8) 0.0001(7) 0.0202(7) 0.0009(7)
F2 0.0383(9) 0.0276(8) 0.0363(8) 0.0065(7) 0.0190(7) 0.0004(7)
N1 0.0222(11) 0.0132(11) 0.0172(10) 0.0009(10) 0.0063(8) 0.0011(9)
C1 0.0248(14) 0.0286(15) 0.0205(12) -0.0010(12) 0.0021(10) 0.0037(11)
C2 0.0302(14) 0.0320(15) 0.0186(12) -0.0025(13) 0.0081(10) -0.0008(11)
C3 0.0329(15) 0.0232(14) 0.0205(12) 0.0024(12) 0.0021(10) 0.0061(11)
C4 0.0213(13) 0.0210(12) 0.0142(11) 0.0003(11) 0.0021(9) 0.0035(10)
C5 0.0198(13) 0.0168(12) 0.0196(12) 0.0025(11) 0.0056(9) 0.0006(10)
C6 0.0197(13) 0.0191(12) 0.0151(11) 0.0001(11) 0.0019(9) 0.0020(10)
C7 0.0207(13) 0.0252(14) 0.0225(12) 0.0007(12) 0.0029(10) 0.0010(11)
C8 0.0302(15) 0.0340(16) 0.0317(14) -0.0100(13) 0.0051(11) 0.0075(13)
C9 0.0429(17) 0.0215(15) 0.0338(15) -0.0113(14) -0.0031(12) 0.0069(12)
C10 0.0389(16) 0.0182(13) 0.0315(14) 0.0024(13) -0.0003(12) -0.0005(12)
C11 0.0264(14) 0.0242(14) 0.0198(12) 0.0009(12) 0.0061(10) 0.0019(11)
C12 0.0228(13) 0.0209(13) 0.0197(11) 0.0004(11) 0.0047(9) 0.0041(11)
C13 0.0241(13) 0.0213(13) 0.0171(11) -0.0003(12) 0.0059(9) 0.0054(11)
C14 0.0326(16) 0.0272(15) 0.0347(14) 0.0043(13) -0.0005(12) -0.0044(12)
C15 0.0326(17) 0.0459(19) 0.0513(18) 0.0166(15) 0.0047(13) -0.0013(16)
C16 0.0226(15) 0.052(2) 0.0457(16) 0.0001(15) 0.0015(12) 0.0001(16)
C17 0.0356(17) 0.0408(17) 0.0305(14) -0.0099(15) 0.0024(12) -0.0106(13)
C18 0.0272(15) 0.0280(15) 0.0278(13) 0.0015(12) 0.0086(11) -0.0018(12)
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'
Cl Cl 0.1484 0.1585 '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'
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
C5 N1 C4 . . 121.50(16) ?
C5 N1 H1A . . 105.3(14) ?
C4 N1 H1A . . 104.3(14) ?
C5 N1 H1B . . 111.4(14) ?
C4 N1 H1B . . 108.5(15) ?
H1A N1 H1B . . 104.2(19) ?
C4 C1 H1C . . 109.5 ?
C4 C1 H1D . . 109.5 ?
H1C C1 H1D . . 109.5 ?
C4 C1 H1E . . 109.5 ?
H1C C1 H1E . . 109.5 ?
H1D C1 H1E . . 109.5 ?
C4 C2 H2A . . 109.5 ?
C4 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
C4 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
C4 C3 H3A . . 109.5 ?
C4 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C4 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C3 C4 C2 . . 111.26(19) ?
C3 C4 C1 . . 109.42(19) ?
C2 C4 C1 . . 110.85(19) ?
C3 C4 N1 . . 111.22(18) ?
C2 C4 N1 . . 108.81(18) ?
C1 C4 N1 . . 105.11(17) ?
C6 C5 N1 . . 114.40(18) ?
C6 C5 C12 . . 113.12(18) ?
N1 C5 C12 . . 107.39(16) ?
C6 C5 H5 . . 107.2 ?
N1 C5 H5 . . 107.2 ?
C12 C5 H5 . . 107.2 ?
C11 C6 C7 . . 114.0(2) ?
C11 C6 C5 . . 124.53(19) ?
C7 C6 C5 . . 121.5(2) ?
F1 C7 C8 . . 118.5(2) ?
F1 C7 C6 . . 117.6(2) ?
C8 C7 C6 . . 123.9(2) ?
C9 C8 C7 . . 118.6(2) ?
C9 C8 H8 . . 120.7 ?
C7 C8 H8 . . 120.7 ?
C8 C9 C10 . . 120.7(2) ?
C8 C9 H9 . . 119.6 ?
C10 C9 H9 . . 119.6 ?
C11 C10 C9 . . 117.8(2) ?
C11 C10 H10 . . 121.1 ?
C9 C10 H10 . . 121.1 ?
F2 C11 C10 . . 118.5(2) ?
F2 C11 C6 . . 116.5(2) ?
C10 C11 C6 . . 124.9(2) ?
C13 C12 C5 . . 111.39(17) ?
C13 C12 H12A . . 109.4 ?
C5 C12 H12A . . 109.4 ?
C13 C12 H12B . . 109.4 ?
C5 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108.0 ?
C18 C13 C14 . . 118.6(2) ?
C18 C13 C12 . . 121.4(2) ?
C14 C13 C12 . . 120.0(2) ?
C15 C14 C13 . . 120.7(3) ?
C15 C14 H14 . . 119.7 ?
C13 C14 H14 . . 119.7 ?
C16 C15 C14 . . 120.2(3) ?
C16 C15 H15 . . 119.9 ?
C14 C15 H15 . . 119.9 ?
C17 C16 C15 . . 119.6(3) ?
C17 C16 H16 . . 120.2 ?
C15 C16 H16 . . 120.2 ?
C16 C17 C18 . . 120.1(3) ?
C16 C17 H17 . . 119.9 ?
C18 C17 H17 . . 119.9 ?
C13 C18 C17 . . 120.7(2) ?
C13 C18 H18 . . 119.6 ?
C17 C18 H18 . . 119.6 ?
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 C7 . 1.356(3) ?
F2 C11 . 1.367(2) ?
N1 C5 . 1.508(3) ?
N1 C4 . 1.532(3) ?
N1 H1A . 0.92(2) ?
N1 H1B . 0.95(2) ?
C1 C4 . 1.524(3) ?
C1 H1C . 0.9800 ?
C1 H1D . 0.9800 ?
C1 H1E . 0.9800 ?
C2 C4 . 1.523(3) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 C4 . 1.520(3) ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C5 C6 . 1.504(3) ?
C5 C12 . 1.534(3) ?
C5 H5 . 1.0000 ?
C6 C11 . 1.384(3) ?
C6 C7 . 1.390(3) ?
C7 C8 . 1.374(3) ?
C8 C9 . 1.374(4) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.382(4) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.369(3) ?
C10 H10 . 0.9500 ?
C12 C13 . 1.510(3) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C18 . 1.379(3) ?
C13 C14 . 1.382(3) ?
C14 C15 . 1.381(4) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.377(4) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.369(4) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.389(3) ?
C17 H17 . 0.9500 ?
C18 H18 . 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
N1 H1A Cl1 . 0.92(2) 2.21(3) 3.115(2) 167.7(19) yes
N1 H1B Cl1 3_675 0.95(2) 2.31(2) 3.1684(19) 151(2) yes