#------------------------------------------------------------------------------ #$Date: 2024-05-15 04:58:38 +0300 (Wed, 15 May 2024) $ #$Revision: 291856 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023126.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_2023126 loop_ _publ_author_name 'Zeller, Matthias' 'Parent, Stephan' 'Schultheiss, Nate' _publ_section_title ; Structural characterization and comparative analysis of polymorphic forms of psilocin (4-hydroxy-N,N-dimethyltryptamine) ; _journal_coeditor_code HB8096 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024004201 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C12 H16 N2 O' _chemical_formula_sum 'C12 H16 N2 O' _chemical_formula_weight 204.27 _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 _atom_sites_solution_primary isomor _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 90.807(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.6228(5) _cell_length_b 8.4984(4) _cell_length_c 12.5073(5) _cell_measurement_reflns_used 7001 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 30.1709 _cell_measurement_theta_min 3.0699 _cell_volume 1129.01(9) _computing_cell_refinement ; SAINT V8.40B (Bruker, 2020) ; _computing_data_collection ; Apex4 v2022.10-0 (Bruker, 2022) ; _computing_data_reduction ; SAINT V8.40B (Bruker, 2020) ; _computing_publication_material 'publCIF (Westrip, 2013)' _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015b), ShelXle Rev1580 (H\"ubschle et al., 2011) ; _computing_structure_solution 'isomorphous replacement' _diffrn_ambient_temperature 300(2) _diffrn_detector_area_resol_mean 7.4074 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three circle diffractometer' _diffrn_measurement_device_type 'Bruker AXS D8 Quest' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'Triumph curved graphite crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 34680 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.226 _diffrn_reflns_theta_min 2.898 _diffrn_source 'fine focus sealed tube X-ray source' _diffrn_source_current '30 mA' _diffrn_source_voltage '50 kV' _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS 2016/2; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.202 _exptl_crystal_description plate _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.213 _refine_diff_density_min -0.192 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 146 _refine_ls_number_reflns 4323 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0523 _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^)+(0.0782P)^2^+0.1036P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1459 _refine_ls_wR_factor_ref 0.1715 _reflns_number_gt 2421 _reflns_number_total 4323 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8096.cif _cod_data_source_block Form_I_300K _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2023126 _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 0.967 _shelx_estimated_absorpt_t_max 0.995 _shelx_hkl_file ; 1 0 0 -0.8959 0.40401 4 -1 0 0 0.09271 0.29497 3 -1 0 0 -0.0752 0.35982 2 3 0 0 174.096 10.1276 1 -3 0 0 180.076 4.84581 4 3 0 0 184.203 4.86759 4 3 0 0 180.246 4.95695 2 -3 0 0 184.127 4.74229 3 -3 0 0 188.401 4.97879 2 -3 0 0 181.562 9.91736 1 4 0 0 101.272 3.25213 2 -4 0 0 95.2544 8.41192 1 -4 0 0 88.7993 3.25648 2 4 0 0 89.3786 8.94457 1 -4 0 0 87.2108 3.03104 4 4 0 0 94.6899 3.06790 4 -4 0 0 89.9760 2.82918 3 5 0 0 9871.81 247.284 1 -5 0 0 9999.99 247.122 1 6 0 0 12.4819 1.73117 2 -6 0 0 9.34713 1.50694 3 -6 0 0 10.6456 1.61878 4 6 0 0 7.86561 5.56539 1 -6 0 0 12.1972 1.79218 2 6 0 0 10.2283 1.51489 4 -6 0 0 8.28267 5.16722 1 7 0 0 585.302 27.4884 1 -7 0 0 597.012 15.0955 3 7 0 0 601.330 15.2561 4 -7 0 0 614.942 15.4515 2 -7 0 0 603.477 15.2906 4 -7 0 0 631.409 27.4111 1 7 0 0 594.015 15.3955 2 8 0 0 156.724 5.46779 4 8 0 0 163.652 15.8831 1 -8 0 0 162.314 5.12006 3 -8 0 0 171.086 14.7872 1 8 0 0 174.756 5.67804 2 -8 0 0 168.674 5.73133 2 -8 0 0 177.291 5.57921 4 -9 0 0 94.5786 3.91995 3 -9 0 0 97.2235 4.76291 2 -9 0 0 105.137 13.3227 1 -9 0 0 92.7807 4.45322 4 9 0 0 89.5877 4.60947 2 9 0 0 102.656 14.9856 1 9 0 0 101.570 4.51544 4 -10 0 0 258.220 8.17822 2 10 0 0 267.077 7.85640 4 10 0 0 232.102 8.03024 2 -10 0 0 243.823 7.75539 4 10 0 0 229.450 21.3870 1 -10 0 0 225.465 20.8002 1 -10 0 0 248.193 7.43835 3 -11 0 0 11.8744 2.67103 4 -11 0 0 13.3211 2.89043 2 11 0 0 9.05637 2.42292 4 -11 0 0 -3.1111 7.17608 1 -11 0 0 5.83214 7.79430 1 -11 0 0 12.2879 2.36767 3 -12 0 0 3.71034 8.48148 1 -12 0 0 4.19665 2.34896 3 12 0 0 3.62342 2.42327 4 -12 0 0 -1.5767 7.98079 1 -12 0 0 3.55129 2.75736 2 -13 0 0 -0.9585 8.60633 1 -13 0 0 -4.9124 7.94576 1 -13 0 0 -2.8037 2.88543 2 13 0 0 -2.2389 2.58754 4 -13 0 0 -1.0971 2.51192 3 -14 0 0 8.64890 13.0753 1 -14 0 0 10.6660 3.51409 2 -14 0 0 7.80006 2.93272 3 -14 0 0 -13.185 10.5988 1 14 0 0 12.6644 3.20926 4 -15 0 0 -3.4068 14.4144 1 15 0 0 8.38183 3.15963 4 -15 0 0 10.9255 3.71111 2 -15 0 0 12.8175 3.36767 3 -15 0 0 -10.777 14.1076 1 -16 0 0 -1.8854 3.56786 2 -16 0 0 1.16753 2.99308 3 16 0 0 1.66310 3.25459 4 0 1 0 0.99877 0.37685 4 -1 -1 0 1053.48 27.0492 1 1 -1 0 1050.06 26.3621 1 -1 1 0 971.835 26.0710 1 -2 -1 0 474.857 15.6806 1 2 -1 0 468.106 14.9250 1 -2 -1 0 450.535 11.0249 4 -2 -1 0 434.430 10.9909 2 2 1 0 433.528 10.9953 2 2 1 0 456.894 15.5806 1 -2 1 0 450.339 14.6684 1 -2 1 0 435.643 10.8532 3 3 -1 0 792.031 25.1756 1 -3 -1 0 817.885 25.7866 1 -3 1 0 812.046 24.9686 1 3 1 0 764.011 25.3401 1 4 -1 0 111.680 3.35326 4 4 -1 0 111.286 3.61946 2 4 -1 0 126.127 9.51379 1 -4 -1 0 109.465 3.67985 2 -4 -1 0 122.456 9.48555 1 -4 -1 0 109.718 3.57644 4 -4 1 0 113.976 8.96084 1 4 1 0 103.139 3.60680 2 -4 1 0 111.646 3.23377 3 -4 1 0 112.416 3.58397 2 4 1 0 117.899 9.23238 1 -4 1 0 106.144 3.34844 4 4 1 0 108.175 3.61872 4 5 -1 0 41.9461 2.70435 2 5 -1 0 47.2739 2.41470 4 -5 -1 0 42.4104 2.65227 4 -5 -1 0 51.8673 7.67478 1 5 -1 0 45.7673 7.07028 1 -5 -1 0 43.7398 2.79053 2 5 1 0 48.2268 7.50909 1 -5 1 0 45.4061 6.82413 1 -5 1 0 46.3850 2.37514 4 5 1 0 44.2415 2.63870 2 -5 1 0 49.8559 2.18960 3 -5 1 0 55.7868 2.80762 2 5 1 0 45.1299 2.72025 4 -6 -1 0 65.5968 3.07243 4 6 -1 0 60.1076 3.11747 2 6 -1 0 64.8166 9.24322 1 -6 -1 0 70.1141 3.26159 2 -6 -1 0 62.1705 2.66334 3 -6 -1 0 55.9734 8.72814 1 6 -1 0 68.7366 2.75181 4 -6 1 0 62.8327 2.80795 4 -6 1 0 67.6878 3.12159 2 6 1 0 58.7857 8.93168 1 6 1 0 64.0974 2.99008 4 -6 1 0 66.8539 8.54623 1 -6 1 0 61.6656 2.53935 3 6 1 0 62.7014 3.09262 2 7 -1 0 167.564 5.35694 2 -7 -1 0 174.343 14.8958 1 -7 -1 0 158.597 4.88774 3 7 -1 0 182.953 14.3993 1 -7 -1 0 156.811 5.32493 4 7 -1 0 163.429 4.99392 4 -7 -1 0 141.644 5.28799 2 -7 1 0 181.004 13.6556 1 -7 1 0 165.018 5.09102 4 -7 1 0 156.560 4.81420 3 7 1 0 157.006 5.25622 2 7 1 0 183.920 15.3115 1 -7 1 0 170.441 5.38141 2 7 1 0 157.610 5.24925 4 8 -1 0 48.6772 9.98549 1 -8 -1 0 46.0181 9.13316 1 -8 -1 0 54.2067 3.38985 4 8 -1 0 47.8547 3.49137 2 -8 -1 0 48.2181 2.89091 3 -8 -1 0 50.3356 3.59679 2 8 -1 0 51.7120 3.13856 4 -8 1 0 49.5634 2.71666 3 8 1 0 40.4352 3.41033 2 -8 1 0 47.2071 3.01834 4 -8 1 0 45.8226 3.40485 2 8 1 0 44.1181 9.00779 1 8 1 0 59.1841 3.27868 4 -8 1 0 60.6487 10.4029 1 -9 -1 0 98.0342 13.1913 1 9 -1 0 95.7903 4.22160 4 -9 -1 0 98.7776 4.70537 2 9 -1 0 77.3275 12.3576 1 9 -1 0 92.7663 4.69538 2 -9 -1 0 96.4556 4.17965 3 -9 -1 0 99.8650 4.80784 4 -9 1 0 99.0033 4.75995 2 -9 1 0 94.2079 4.27014 4 9 1 0 106.098 4.60138 2 9 1 0 100.562 4.43911 4 -9 1 0 98.5635 3.96491 3 -9 1 0 93.4351 13.4456 1 10 -1 0 -2.4840 2.01535 4 -10 -1 0 4.76188 2.30947 3 10 -1 0 -0.1803 2.47802 2 -10 -1 0 -0.6616 2.41638 4 10 -1 0 8.59141 7.64079 1 -10 -1 0 3.94633 2.55883 2 -10 -1 0 -1.6981 6.32376 1 -10 1 0 2.94958 2.08844 3 -10 1 0 5.47160 2.54127 2 -10 1 0 3.55512 6.06497 1 10 1 0 0.93166 2.37458 2 10 1 0 0.18705 2.25107 4 -10 1 0 -0.6266 2.13486 4 11 -1 0 34.2579 2.90051 4 -11 -1 0 30.2525 3.18514 4 -11 -1 0 36.2768 10.6574 1 11 -1 0 17.4882 9.69609 1 -11 -1 0 42.2193 10.8350 1 -11 -1 0 26.1288 2.89006 3 -11 -1 0 30.6838 3.31955 2 -11 1 0 29.3796 2.96317 4 11 1 0 34.1541 3.12506 4 -11 1 0 36.7530 9.88910 1 -11 1 0 36.1683 2.91858 3 -11 1 0 31.9502 3.31899 2 -11 1 0 46.7934 11.1976 1 -12 -1 0 2.60487 8.52503 1 -12 -1 0 2.03160 2.86995 2 -12 -1 0 -5.1053 7.25892 1 12 -1 0 -1.0235 2.30971 4 -12 -1 0 -0.1474 2.52101 3 -12 1 0 0.69548 2.37003 3 12 1 0 -2.0944 2.44571 4 -12 1 0 0.70194 2.47404 4 -12 1 0 3.58942 2.86764 2 -12 1 0 6.98666 9.10301 1 -12 1 0 -3.4975 5.99760 1 -13 -1 0 13.2028 10.2149 1 -13 -1 0 8.30940 3.23967 2 13 -1 0 6.12476 2.59772 4 -13 -1 0 6.25931 2.71761 3 -13 -1 0 25.3132 12.0086 1 -13 1 0 4.85660 8.72847 1 -13 1 0 1.86717 3.07671 2 13 1 0 7.69372 2.89152 4 -13 1 0 14.3956 9.18031 1 -13 1 0 9.71555 2.79647 3 -14 -1 0 22.9794 12.8439 1 -14 -1 0 36.3883 3.61863 3 -14 -1 0 28.6537 3.97301 2 -14 -1 0 32.3548 13.2625 1 14 -1 0 40.8064 3.74812 4 14 1 0 31.4715 3.72024 4 -14 1 0 30.5639 4.01235 2 -14 1 0 26.8935 3.35067 3 -14 1 0 18.0590 11.4528 1 -14 1 0 25.3336 12.1145 1 -15 -1 0 1.22337 3.07050 3 15 -1 0 0.34329 2.75573 4 -15 -1 0 14.7968 15.6628 1 -15 -1 0 -2.8390 3.30871 2 -15 -1 0 18.7765 14.5606 1 15 1 0 -4.1328 2.99923 4 -15 1 0 -10.611 14.4262 1 -15 1 0 -3.8230 3.26218 2 -15 1 0 1.38133 2.76740 3 -16 -1 0 -15.254 31.4157 1 -16 -1 0 3.77503 3.71444 2 16 -1 0 7.87231 3.32443 4 -16 -1 0 -3.1119 3.11813 3 -16 1 0 4.00373 3.17693 3 -16 1 0 5.30453 3.70397 2 16 1 0 0.50417 3.46741 4 1 -2 0 2777.33 68.5799 1 -1 2 0 2850.91 67.7702 1 -2 -2 0 8.70901 1.19679 2 2 -2 0 11.7155 0.85118 4 -2 -2 0 6.86767 3.01284 1 2 -2 0 16.4188 2.93435 1 2 -2 0 13.1120 1.18151 2 -2 -2 0 12.3303 1.26389 4 -2 2 0 15.4376 1.27003 2 2 2 0 15.1044 1.30974 3 -2 2 0 13.8344 2.72382 1 2 2 0 14.1011 1.26013 4 2 2 0 12.4994 1.21040 2 -2 2 0 15.1543 1.21112 3 -3 -2 0 529.489 13.1842 4 3 -2 0 525.063 12.9076 4 -3 -2 0 512.409 13.1426 2 -3 -2 0 544.782 19.8002 1 3 -2 0 534.552 18.4869 1 3 -2 0 517.098 13.1064 2 3 2 0 551.425 13.2151 4 -3 2 0 514.196 12.9055 4 3 2 0 545.027 13.1741 2 -3 2 0 529.235 13.1349 2 -3 2 0 528.206 12.9510 3 -3 2 0 546.942 18.1859 1 -4 -2 0 140.813 4.38945 2 4 -2 0 134.481 3.95066 4 4 -2 0 141.431 4.29682 2 -4 -2 0 145.916 4.36280 4 -4 -2 0 142.905 10.7409 1 4 -2 0 144.251 10.0581 1 4 2 0 142.858 4.36111 4 -4 2 0 131.507 4.23641 2 -4 2 0 138.493 3.92135 4 4 2 0 141.423 4.32764 2 -4 2 0 138.418 3.91263 3 -4 2 0 137.723 9.48542 1 5 -2 0 81.6081 2.91479 4 -5 -2 0 77.7205 3.30518 2 -5 -2 0 72.3657 9.33722 1 5 -2 0 75.4857 3.21841 2 5 -2 0 69.4014 8.04349 1 -5 -2 0 73.6761 3.34735 4 -5 2 0 80.8247 2.79815 4 -5 2 0 71.9410 8.23800 1 -5 2 0 81.3644 3.16910 2 5 2 0 76.3568 3.16212 2 -5 2 0 77.7041 2.69616 3 5 2 0 73.2819 3.29853 4 -6 -2 0 3.15129 4.40170 1 6 -2 0 0.30141 1.19983 4 -6 -2 0 1.33778 1.65544 2 6 -2 0 0.30907 1.52148 2 -6 -2 0 0.13090 1.54745 4 6 -2 0 -1.3956 4.00918 1 -6 2 0 -0.9851 1.48873 2 -6 2 0 -0.1322 3.18409 1 -6 2 0 2.21280 1.17257 4 -6 2 0 -1.6151 1.13682 3 6 2 0 0.78181 1.52472 2 6 2 0 1.48534 1.51209 4 -7 -2 0 1.74853 1.82449 4 7 -2 0 11.5104 5.91105 1 -7 -2 0 4.45956 1.86012 2 7 -2 0 3.85658 1.80227 2 -7 -2 0 -0.3675 4.73234 1 7 -2 0 4.34185 1.50204 4 -7 2 0 2.91647 1.76251 2 -7 2 0 2.96843 4.73532 1 -7 2 0 2.37007 1.39543 4 -7 2 0 3.16217 1.46028 3 7 2 0 4.12158 1.75266 2 7 2 0 3.17617 1.76798 4 -8 -2 0 27.0324 2.57586 2 8 -2 0 27.9240 2.52610 2 -8 -2 0 20.1990 2.45342 4 8 -2 0 17.0266 7.18223 1 -8 -2 0 17.1175 6.88565 1 -8 2 0 20.1982 6.57457 1 -8 2 0 28.3784 2.48285 2 -8 2 0 24.9551 2.26707 3 8 2 0 21.6565 2.38558 2 -8 2 0 26.7353 2.09820 4 8 2 0 22.2251 2.42058 4 -9 -2 0 33.6322 3.05122 2 -9 -2 0 36.4957 2.87204 3 -9 -2 0 39.5436 10.0252 1 9 -2 0 29.3759 2.40182 4 -9 -2 0 27.2693 2.89971 4 9 -2 0 25.3568 8.41909 1 9 -2 0 32.3225 2.97075 2 9 2 0 31.2302 2.87895 2 -9 2 0 25.5049 7.87816 1 -9 2 0 31.3135 2.69223 3 9 2 0 36.3220 2.96918 4 -9 2 0 34.1637 2.93280 2 -9 2 0 34.3576 2.51860 4 10 -2 0 119.234 16.4810 1 10 -2 0 124.462 5.68298 2 -10 -2 0 126.630 17.6022 1 -10 -2 0 137.056 5.26209 3 -10 -2 0 121.181 5.93036 4 10 -2 0 134.516 5.14725 4 -10 -2 0 131.124 5.73473 2 -10 2 0 128.863 4.83955 3 10 2 0 129.031 5.61613 2 -10 2 0 132.466 16.1419 1 -10 2 0 134.600 5.83505 2 -10 2 0 129.414 5.09192 4 -10 2 0 141.703 16.1198 1 10 2 0 124.923 5.51453 4 -11 -2 0 7.75319 2.64608 3 11 -2 0 6.79775 2.33367 4 -11 -2 0 -4.3229 7.06079 1 -11 -2 0 10.6610 2.85833 2 11 -2 0 -2.1879 7.08873 1 -11 -2 0 5.09462 8.92901 1 -11 2 0 7.66431 2.23900 3 11 2 0 4.83479 2.61294 4 -11 2 0 6.39631 2.36705 4 -11 2 0 12.4682 8.41267 1 -11 2 0 12.5265 2.85910 2 -11 2 0 7.62501 6.87129 1 -12 -2 0 13.4004 3.22845 2 -12 -2 0 18.5576 11.1835 1 -12 -2 0 14.8410 10.9813 1 -12 -2 0 17.4333 2.97564 3 12 -2 0 18.6937 2.63256 4 -12 2 0 11.7329 2.63217 4 -12 2 0 12.9691 3.14726 2 -12 2 0 15.4127 9.20699 1 12 2 0 14.6513 3.11044 4 -12 2 0 2.47603 8.27785 1 -12 2 0 12.4244 2.52766 3 -13 -2 0 4.71660 2.90215 3 -13 -2 0 10.8038 3.31825 2 -13 -2 0 -1.3635 10.1015 1 -13 -2 0 -1.8512 8.88336 1 13 -2 0 9.91218 2.56255 4 -13 2 0 7.20519 9.55812 1 -13 2 0 6.53178 3.22546 2 13 2 0 3.52722 3.09964 4 -13 2 0 6.71241 2.70203 3 -13 2 0 -8.4378 7.38703 1 -14 -2 0 5.12878 3.41198 2 14 -2 0 10.0888 2.86088 4 -14 -2 0 15.8853 12.1951 1 -14 -2 0 35.4065 13.6923 1 -14 -2 0 8.21332 3.07120 3 -14 2 0 9.44974 10.8872 1 -14 2 0 8.98414 2.87138 3 -14 2 0 -13.779 9.67743 1 -14 2 0 9.03014 3.49749 2 14 2 0 8.97735 3.38617 4 -15 -2 0 -28.841 14.1268 1 -15 -2 0 -3.8425 3.02952 3 15 -2 0 2.54798 2.69635 4 -15 -2 0 6.05892 3.55511 2 -15 -2 0 4.77011 15.7118 1 15 2 0 0.18223 3.31791 4 -15 2 0 -0.1880 2.71366 3 -15 2 0 6.08935 3.58279 2 -15 2 0 -10.487 14.8479 1 16 -2 0 0.23651 2.78927 4 -16 -2 0 -4.1257 3.52792 2 -16 -2 0 1.20726 23.2473 1 -16 -2 0 0.10175 3.42607 3 -16 2 0 -0.6737 3.70305 2 16 2 0 2.79435 3.53148 4 -16 2 0 -1.1994 2.83804 3 0 -3 0 3.42292 1.60219 1 0 -3 0 1.79417 0.90250 4 0 3 0 1.17018 1.13631 3 0 3 0 -0.4358 1.00311 4 1 -3 0 1534.30 38.6330 1 2 -3 0 139.791 6.93480 1 -2 -3 0 123.743 4.00615 2 -2 -3 0 140.606 8.25966 1 2 -3 0 131.113 3.66365 4 2 -3 0 132.831 4.01010 2 -2 -3 0 139.281 4.03928 4 2 3 0 131.485 3.95698 3 -2 3 0 135.532 5.69672 1 2 3 0 133.226 4.05131 4 -2 3 0 133.065 3.79944 3 -2 3 0 127.019 4.02736 2 3 -3 0 77.8092 2.48414 4 -3 -3 0 80.3584 3.14364 4 3 -3 0 81.1599 2.94635 2 -3 -3 0 81.8573 3.13691 2 -3 -3 0 83.4156 7.80274 1 3 -3 0 85.0579 6.65354 1 3 3 0 76.0398 2.99388 2 -3 3 0 76.5948 5.95700 1 3 3 0 73.7805 3.12229 4 -3 3 0 77.8722 3.06397 2 3 3 0 82.2531 2.93399 3 -3 3 0 77.5962 2.63731 3 -4 -3 0 132.914 10.4912 1 4 -3 0 136.440 3.82772 4 -4 -3 0 139.124 4.37016 2 4 -3 0 149.828 9.91407 1 -4 -3 0 129.257 4.44577 4 4 -3 0 136.879 4.26052 2 4 3 0 130.352 4.40244 4 -4 3 0 132.267 3.90914 3 -4 3 0 127.185 3.83038 4 -4 3 0 136.325 4.38280 2 -4 3 0 150.697 9.20278 1 4 3 0 129.602 4.35464 2 5 -3 0 120.679 3.67210 4 -5 -3 0 122.797 4.21383 4 -5 -3 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2.54825 4 -2 1 -19 -12.584 21.1453 1 -2 1 -19 -0.6606 3.39473 3 1 2 -19 29.8129 23.7376 1 0 -2 -19 0.48197 3.25998 4 0 -2 -19 0.26968 2.32228 3 0 2 -19 0.44495 2.65864 4 0 2 -19 -1.1844 3.05397 3 0 2 -19 -31.432 31.2995 1 -1 -2 -19 -1.3976 2.52033 3 -1 2 -19 1.94633 3.18434 3 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6629 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71069 10.626 8.503 12.520 90.009 90.784 90.004 ) ; _shelx_hkl_checksum 23871 _shelx_res_file ; TITL 57_30_03_2_0m.res in P2(1)/c 57_30_03_2_1m.res created by SHELXL-2019/3 at 09:12:15 on 02-Jun-2023 REM Old TITL 57_30_03_2_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.194, Rweak 0.010, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C12 N2 O CELL 0.71073 10.6228 8.4984 12.5073 90.0000 90.8071 90.0000 ZERR 4.000 0.0005 0.0004 0.0005 0.0000 0.0024 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 48 64 8 4 OMIT 1 0 0 TEMP 26.850 SIZE 0.43 0.29 0.06 L.S. 10 BOND $H ACTA CONF HTAB EQIV $1 -x+1, -y+1, -z+1 HTAB O1 N2_$1 EQIV $2 x, -y+1/2, z-1/2 HTAB N1 O1_$2 LIST 4 FMAP 2 PLAN 20 WGHT 0.078200 0.103600 FVAR 1.38694 O1 4 0.699926 0.474380 0.468702 11.00000 0.07108 0.05238 = 0.04504 -0.00479 0.02122 -0.00884 H1O 2 0.731268 0.587706 0.481004 11.00000 0.10258 N1 3 0.644545 0.137441 0.181509 11.00000 0.08676 0.07412 = 0.05085 -0.01907 0.01227 0.01185 H1N 2 0.650809 0.095243 0.114425 11.00000 0.09339 N2 3 0.253125 0.228038 0.491408 11.00000 0.04983 0.05782 = 0.05823 -0.00463 0.00872 -0.00521 C1 1 0.474040 0.241810 0.428106 11.00000 0.05495 0.05729 = 0.05024 -0.00693 0.00998 -0.00065 AFIX 23 H1A 2 0.473533 0.351254 0.450111 11.00000 -1.20000 H1B 2 0.507116 0.180151 0.487413 11.00000 -1.20000 AFIX 0 C5 1 0.542459 0.129652 0.246711 11.00000 0.07202 0.06310 = 0.05683 -0.01614 0.00530 0.00261 AFIX 43 H5 2 0.471156 0.068880 0.233330 11.00000 -1.20000 AFIX 0 C6 1 0.559991 0.223969 0.334525 11.00000 0.05672 0.04732 = 0.04675 -0.00348 0.00799 0.00747 C7 1 0.681085 0.297213 0.321254 11.00000 0.05464 0.04562 = 0.03926 0.00272 0.01147 0.01325 C8 1 0.750130 0.411044 0.378250 11.00000 0.05377 0.05039 = 0.04122 0.00605 0.01278 0.00768 C9 1 0.865705 0.457222 0.339993 11.00000 0.05585 0.07191 = 0.06345 0.00375 0.01694 0.00072 AFIX 43 H9 2 0.913117 0.531082 0.377831 11.00000 -1.20000 AFIX 0 C10 1 0.912622 0.394150 0.244710 11.00000 0.05828 0.09341 = 0.07088 0.01034 0.02809 0.01348 AFIX 43 H10 2 0.990900 0.427232 0.221063 11.00000 -1.20000 AFIX 0 C11 1 0.847287 0.286332 0.185970 11.00000 0.07215 0.08557 = 0.05570 0.00078 0.02784 0.02399 AFIX 43 H11 2 0.879046 0.245610 0.122822 11.00000 -1.20000 AFIX 0 C12 1 0.730340 0.239271 0.224519 11.00000 0.06694 0.05869 = 0.04488 -0.00034 0.01418 0.01903 C2 1 0.341002 0.190717 0.404458 11.00000 0.05891 0.06638 = 0.06089 -0.01701 0.00821 -0.00418 AFIX 23 H2A 2 0.311821 0.241790 0.339330 11.00000 -1.20000 H2B 2 0.340035 0.078053 0.392046 11.00000 -1.20000 AFIX 0 C3 1 0.123074 0.204000 0.454680 11.00000 0.05229 0.14881 = 0.11166 -0.05490 0.00412 -0.00962 AFIX 137 H3A 2 0.105329 0.272151 0.395138 11.00000 -1.50000 H3B 2 0.066678 0.227621 0.511797 11.00000 -1.50000 H3C 2 0.111940 0.096468 0.433020 11.00000 -1.50000 AFIX 0 C4 1 0.277897 0.135095 0.587868 11.00000 0.09785 0.08734 = 0.09398 0.03598 0.02883 0.00322 AFIX 137 H4A 2 0.263611 0.025763 0.572681 11.00000 -1.50000 H4B 2 0.222611 0.168533 0.643515 11.00000 -1.50000 H4C 2 0.363726 0.149990 0.610712 11.00000 -1.50000 REM ##### REM ##### AFIX 0 HKLF 4 REM 57_30_03_2_0m.res in P2(1)/c REM wR2 = 0.1715, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0523 for 2421 Fo > 4sig(Fo) and 0.0971 for all 4323 data REM 146 parameters refined using 0 restraints END WGHT 0.0786 0.1027 REM Instructions for potential hydrogen bonds HTAB O1 N2_$1 HTAB N1 O1_$2 HTAB C1 O1 HTAB C1 O1_$1 REM Highest difference peak 0.213, deepest hole -0.192, 1-sigma level 0.031 Q1 1 0.7064 0.2709 0.2745 11.00000 0.05 0.21 Q2 1 0.6248 0.2696 0.3388 11.00000 0.05 0.21 Q3 1 0.7956 0.2610 0.2242 11.00000 0.05 0.20 Q4 1 0.7218 0.3345 0.3562 11.00000 0.05 0.17 Q5 1 0.2366 0.1082 0.5297 11.00000 0.05 0.17 Q6 1 0.5245 0.2278 0.3851 11.00000 0.05 0.16 Q7 1 0.2964 0.2185 0.4609 11.00000 0.05 0.16 Q8 1 0.5568 0.1468 0.3117 11.00000 0.05 0.15 Q9 1 0.8992 0.2987 0.2410 11.00000 0.05 0.14 Q10 1 0.8149 0.4256 0.3759 11.00000 0.05 0.13 Q11 1 0.5003 0.2663 0.5031 11.00000 0.05 0.13 Q12 1 0.2573 0.3132 0.5010 11.00000 0.05 0.12 Q13 1 0.0608 0.2602 0.4937 11.00000 0.05 0.12 Q14 1 0.6399 0.4493 0.5051 11.00000 0.05 0.12 Q15 1 0.5241 0.2171 0.2747 11.00000 0.05 0.12 Q16 1 0.0574 0.3139 0.4702 11.00000 0.05 0.12 Q17 1 0.1039 0.1741 0.3833 11.00000 0.05 0.12 Q18 1 0.8762 0.4374 0.2821 11.00000 0.05 0.11 Q19 1 0.6595 0.3193 0.3099 11.00000 0.05 0.11 Q20 1 0.0642 0.1957 0.5265 11.00000 0.05 0.11 ; _shelx_res_checksum 9452 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 O O1 0.69993(9) 0.47438(10) 0.46870(6) 0.0560(2) Uani d 1 . . H H1O 0.7313(19) 0.588(3) 0.4810(15) 0.103(6) Uiso d 1 . . N N1 0.64455(13) 0.13744(16) 0.18151(10) 0.0705(4) Uani d 1 . . H H1N 0.6508(18) 0.095(2) 0.1144(16) 0.093(6) Uiso d 1 . . N N2 0.25313(10) 0.22804(13) 0.49141(9) 0.0552(3) Uani d 1 . . C C1 0.47404(11) 0.24181(16) 0.42811(10) 0.0541(3) Uani d 1 . . H H1A 0.473533 0.351254 0.450111 0.065 Uiso calc 1 . . H H1B 0.507116 0.180151 0.487413 0.065 Uiso calc 1 . . C C5 0.54246(14) 0.12965(17) 0.24671(11) 0.0639(4) Uani d 1 . . H H5 0.471156 0.068880 0.233330 0.077 Uiso calc 1 . . C C6 0.55999(12) 0.22397(14) 0.33453(9) 0.0502(3) Uani d 1 . . C C7 0.68108(11) 0.29721(13) 0.32125(8) 0.0464(3) Uani d 1 . . C C8 0.75013(11) 0.41104(14) 0.37825(9) 0.0483(3) Uani d 1 . . C C9 0.86570(13) 0.45722(18) 0.33999(12) 0.0636(3) Uani d 1 . . H H9 0.913117 0.531082 0.377831 0.076 Uiso calc 1 . . C C10 0.91262(14) 0.3942(2) 0.24471(13) 0.0739(4) Uani d 1 . . H H10 0.990900 0.427232 0.221063 0.089 Uiso calc 1 . . C C11 0.84729(15) 0.2863(2) 0.18597(12) 0.0709(4) Uani d 1 . . H H11 0.879046 0.245610 0.122822 0.085 Uiso calc 1 . . C C12 0.73034(13) 0.23927(16) 0.22452(10) 0.0567(3) Uani d 1 . . C C2 0.34100(13) 0.19072(18) 0.40446(11) 0.0620(3) Uani d 1 . . H H2A 0.311821 0.241790 0.339330 0.074 Uiso calc 1 . . H H2B 0.340035 0.078053 0.392046 0.074 Uiso calc 1 . . C C3 0.12307(15) 0.2040(3) 0.45468(18) 0.1042(7) Uani d 1 . . H H3A 0.105329 0.272151 0.395138 0.156 Uiso calc 1 . . H H3B 0.066678 0.227621 0.511797 0.156 Uiso calc 1 . . H H3C 0.111940 0.096468 0.433020 0.156 Uiso calc 1 . . C C4 0.27790(19) 0.1351(2) 0.58787(15) 0.0928(6) Uani d 1 . . H H4A 0.263611 0.025763 0.572681 0.139 Uiso calc 1 . . H H4B 0.222611 0.168533 0.643515 0.139 Uiso calc 1 . . H H4C 0.363726 0.149990 0.610712 0.139 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0711(6) 0.0524(5) 0.0450(4) -0.0088(4) 0.0212(4) -0.0048(3) N1 0.0868(9) 0.0741(8) 0.0509(6) 0.0118(6) 0.0123(6) -0.0191(6) N2 0.0498(5) 0.0578(6) 0.0582(6) -0.0052(4) 0.0087(4) -0.0046(5) C1 0.0550(7) 0.0573(7) 0.0502(6) -0.0007(5) 0.0100(5) -0.0069(5) C5 0.0720(8) 0.0631(8) 0.0568(7) 0.0026(6) 0.0053(6) -0.0161(6) C6 0.0567(6) 0.0473(6) 0.0467(6) 0.0075(5) 0.0080(5) -0.0035(5) C7 0.0546(6) 0.0456(5) 0.0393(5) 0.0132(5) 0.0115(4) 0.0027(4) C8 0.0538(6) 0.0504(6) 0.0412(5) 0.0077(5) 0.0128(4) 0.0061(4) C9 0.0558(7) 0.0719(8) 0.0635(8) 0.0007(6) 0.0169(6) 0.0038(6) C10 0.0583(8) 0.0934(11) 0.0709(9) 0.0135(7) 0.0281(7) 0.0103(8) C11 0.0722(9) 0.0856(10) 0.0557(7) 0.0240(8) 0.0278(6) 0.0008(7) C12 0.0669(7) 0.0587(7) 0.0449(6) 0.0190(6) 0.0142(5) -0.0003(5) C2 0.0589(7) 0.0664(8) 0.0609(7) -0.0042(6) 0.0082(6) -0.0170(6) C3 0.0523(8) 0.1488(19) 0.1117(15) -0.0096(10) 0.0041(9) -0.0549(14) C4 0.0979(13) 0.0873(12) 0.0940(12) 0.0032(10) 0.0288(10) 0.0360(10) 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' 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 C8 O1 H1O . . 111.3(11) ? C12 N1 C5 . . 109.09(11) ? C12 N1 H1N . . 123.6(12) ? C5 N1 H1N . . 126.6(12) ? C4 N2 C3 . . 109.96(15) ? C4 N2 C2 . . 112.52(12) ? C3 N2 C2 . . 110.01(12) ? C6 C1 C2 . . 113.42(11) ? C6 C1 H1A . . 108.9 ? C2 C1 H1A . . 108.9 ? C6 C1 H1B . . 108.9 ? C2 C1 H1B . . 108.9 ? H1A C1 H1B . . 107.7 ? N1 C5 C6 . . 110.47(13) ? N1 C5 H5 . . 124.8 ? C6 C5 H5 . . 124.8 ? C5 C6 C7 . . 105.78(11) ? C5 C6 C1 . . 127.32(12) ? C7 C6 C1 . . 126.84(11) ? C8 C7 C12 . . 118.56(11) ? C8 C7 C6 . . 134.49(10) ? C12 C7 C6 . . 106.86(11) ? O1 C8 C9 . . 122.25(12) ? O1 C8 C7 . . 118.99(10) ? C9 C8 C7 . . 118.75(11) ? C8 C9 C10 . . 120.89(15) ? C8 C9 H9 . . 119.6 ? C10 C9 H9 . . 119.6 ? C11 C10 C9 . . 122.10(13) ? C11 C10 H10 . . 118.9 ? C9 C10 H10 . . 118.9 ? C10 C11 C12 . . 117.14(12) ? C10 C11 H11 . . 121.4 ? C12 C11 H11 . . 121.4 ? N1 C12 C11 . . 129.70(13) ? N1 C12 C7 . . 107.80(12) ? C11 C12 C7 . . 122.50(14) ? N2 C2 C1 . . 113.26(11) ? N2 C2 H2A . . 108.9 ? C1 C2 H2A . . 108.9 ? N2 C2 H2B . . 108.9 ? C1 C2 H2B . . 108.9 ? H2A C2 H2B . . 107.7 ? N2 C3 H3A . . 109.5 ? N2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? N2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? N2 C4 H4A . . 109.5 ? N2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? N2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? 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 O1 C8 . 1.3678(13) ? O1 H1O . 1.03(2) ? N1 C12 . 1.362(2) ? N1 C5 . 1.3676(19) ? N1 H1N . 0.92(2) ? N2 C4 . 1.463(2) ? N2 C3 . 1.4640(19) ? N2 C2 . 1.4776(16) ? C1 C6 . 1.5022(15) ? C1 C2 . 1.5038(18) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C5 C6 . 1.3703(17) ? C5 H5 . 0.9300 ? C6 C7 . 1.4407(17) ? C7 C8 . 1.4026(18) ? C7 C12 . 1.4135(15) ? C8 C9 . 1.3809(17) ? C9 C10 . 1.405(2) ? C9 H9 . 0.9300 ? C10 C11 . 1.359(2) ? C10 H10 . 0.9300 ? C11 C12 . 1.397(2) ? C11 H11 . 0.9300 ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1O N2 3_666 1.03(2) 1.61(2) 2.6242(14) 166.6(18) yes N1 H1N O1 4_565 0.92(2) 1.99(2) 2.8944(14) 167.9(18) 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 C12 N1 C5 C6 . . . . -0.99(17) ? N1 C5 C6 C7 . . . . 1.03(15) ? N1 C5 C6 C1 . . . . -176.28(12) ? C2 C1 C6 C5 . . . . -20.34(19) ? C2 C1 C6 C7 . . . . 162.90(12) ? C5 C6 C7 C8 . . . . 175.62(13) ? C1 C6 C7 C8 . . . . -7.1(2) ? C5 C6 C7 C12 . . . . -0.69(13) ? C1 C6 C7 C12 . . . . 176.64(11) ? C12 C7 C8 O1 . . . . 176.31(10) ? C6 C7 C8 O1 . . . . 0.3(2) ? C12 C7 C8 C9 . . . . -2.62(17) ? C6 C7 C8 C9 . . . . -178.60(13) ? O1 C8 C9 C10 . . . . -177.63(12) ? C7 C8 C9 C10 . . . . 1.3(2) ? C8 C9 C10 C11 . . . . 0.2(2) ? C9 C10 C11 C12 . . . . -0.3(2) ? C5 N1 C12 C11 . . . . -179.00(15) ? C5 N1 C12 C7 . . . . 0.52(15) ? C10 C11 C12 N1 . . . . 178.25(14) ? C10 C11 C12 C7 . . . . -1.2(2) ? C8 C7 C12 N1 . . . . -176.89(11) ? C6 C7 C12 N1 . . . . 0.12(14) ? C8 C7 C12 C11 . . . . 2.67(19) ? C6 C7 C12 C11 . . . . 179.68(12) ? C4 N2 C2 C1 . . . . -68.20(16) ? C3 N2 C2 C1 . . . . 168.82(15) ? C6 C1 C2 N2 . . . . -172.27(11) ?