#------------------------------------------------------------------------------ #$Date: 2023-05-06 13:44:56 +0300 (Sat, 06 May 2023) $ #$Revision: 283578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/27/2022716.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_2022716 loop_ _publ_author_name 'Vinaya, ?' 'Basavaraju, Yeriyur B.' 'Yathirajan, Hemmige S.' 'Parkin, Sean' _publ_section_title ; Syntheses and crystal structures of four 4-(4-meth-oxy-phen-yl)piperazin-1-ium salts: tri-fluoro-acetate, 2,3,4,5,6-penta-fluoro-benzoate, 4-iodo-benzoate, and a polymorph with 4-methyl-benzoate. ; _journal_coeditor_code VM2279 _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 380 _journal_page_last 385 _journal_paper_doi 10.1107/S2056989023002529 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C11 H17 N2 O +, C8 H7 O2 -, H2 O' _chemical_formula_moiety 'C11 H17 N2 O +, C8 H7 O2 -, H2 O' _chemical_formula_sum 'C19 H26 N2 O4' _chemical_formula_weight 346.42 _chemical_name_systematic ; 4-(4-Methoxyphenyl)piperazin-1-ium 4-methylbenzoate monohydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXL-2019/2 and CIFFIX' _cell_angle_alpha 80.190(6) _cell_angle_beta 86.089(5) _cell_angle_gamma 82.843(6) _cell_formula_units_Z 2 _cell_length_a 6.1481(13) _cell_length_b 7.3467(12) _cell_length_c 19.980(4) _cell_measurement_reflns_used 9904 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.83 _cell_volume 881.3(3) _computing_cell_refinement ; APEX3 (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; APEX3 (Bruker, 2016) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2020) ; _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 90.0(2) _diffrn_detector_area_resol_mean 7.41 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _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 0.0411 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 23917 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.590 _diffrn_reflns_theta_min 2.071 _diffrn_source microsource _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description plate _exptl_crystal_F_000 372 _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.191 _refine_diff_density_min -0.180 _refine_ls_extinction_coef 0.0038(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2019/2 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 245 _refine_ls_number_reflns 4059 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0381 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+0.3732P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.0799 _reflns_number_gt 3137 _reflns_number_total 4059 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2279sup1.cif _cod_data_source_block IV _cod_depositor_comments 'Adding full bibliography for 2022713--2022716.cif.' _cod_database_code 2022716 _cod_database_fobs_code 2022716 _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 0.974 _shelx_estimated_absorpt_t_max 0.998 _shelx_hkl_file ; -1 0 0 54.4988 2.52989 2 -1 0 0 52.6740 2.39977 2 -1 0 0 54.3397 2.02221 4 -1 0 0 53.5633 2.04525 5 -1 0 0 52.9121 2.07808 5 1 0 0 55.3514 2.52181 2 1 0 0 53.6109 2.38476 2 1 0 0 54.7233 1.98097 4 1 0 0 53.5360 1.99711 5 1 0 0 54.1356 1.96200 5 -2 0 0 17.3089 1.60638 5 -2 0 0 16.2967 1.62008 5 -2 0 0 16.8890 2.02788 2 -2 0 0 18.1147 1.55058 4 -2 0 0 17.9523 2.04693 2 2 0 0 15.5917 1.37365 5 2 0 0 18.3062 1.45576 5 2 0 0 17.5124 1.99620 2 2 0 0 17.5734 1.50204 4 2 0 0 19.1335 1.97528 2 -3 0 0 47.7951 3.81861 4 -3 0 0 51.8712 3.16000 5 -3 0 0 49.4273 3.54506 2 3 0 0 51.1059 3.55954 2 3 0 0 56.4345 2.94331 4 3 0 0 50.9887 2.58304 5 3 0 0 51.8487 2.63127 5 3 0 0 52.3207 3.58151 2 -4 0 0 3.84574 1.49238 2 -4 0 0 3.98675 1.37016 5 -4 0 0 6.38869 1.78466 5 -4 0 0 2.08589 1.48955 2 -4 0 0 4.68659 1.20676 4 4 0 0 2.63385 1.52027 2 4 0 0 4.53668 1.26365 4 4 0 0 5.22874 1.21115 5 4 0 0 4.83649 1.98591 2 4 0 0 5.83962 1.61168 5 -5 0 0 5.87801 1.79292 5 -5 0 0 2.17032 1.63363 2 -5 0 0 2.95999 1.31570 4 -5 0 0 3.56117 1.79364 2 5 0 0 2.77763 0.98729 5 5 0 0 1.38894 1.64936 2 5 0 0 6.62428 2.44245 2 5 0 0 1.68568 0.78323 5 -6 0 0 36.6375 4.45942 2 -6 0 0 36.6735 4.48126 2 6 0 0 31.3411 4.19177 2 -7 0 0 21.1506 4.38535 2 -7 0 0 19.6432 4.32768 2 -7 0 0 16.3312 3.92448 5 7 -1 0 1.26482 2.35232 2 -7 1 0 1.52222 1.70985 5 -7 1 0 3.44996 2.28203 2 -7 1 0 0.00844 2.59100 2 6 -1 0 -0.8678 1.47446 2 -6 1 0 1.29882 1.44103 2 -6 1 0 0.88101 1.64605 2 -6 1 0 1.14947 1.43113 5 -6 1 0 0.89811 1.35921 4 5 -1 0 12.0277 2.53888 2 -5 1 0 4.82866 1.96345 5 -5 1 0 6.60252 1.78549 5 -5 1 0 10.0337 1.94058 4 -5 1 0 6.40140 2.09105 2 -5 1 0 8.53461 2.23663 2 4 -1 0 4.29599 1.61782 2 4 -1 0 5.66201 1.63852 2 -4 1 0 5.59582 1.40138 5 -4 1 0 4.89554 1.70025 2 -4 1 0 5.45459 1.45542 5 -4 1 0 4.81975 1.60749 2 -4 1 0 3.28887 1.14455 4 3 -1 0 18.4153 2.06090 2 3 -1 0 12.1653 1.75290 2 -3 1 0 14.7925 2.97186 2 -3 1 0 17.5731 1.62983 5 -3 1 0 14.3045 1.51584 4 -3 1 0 13.3827 1.51643 5 -3 1 0 15.6553 1.95543 2 2 -1 0 701.030 18.5417 2 -2 1 0 689.644 18.6582 2 -2 1 0 706.973 17.7572 5 -2 1 0 737.713 18.1343 4 -2 1 0 718.973 18.6702 2 1 -1 0 2471.70 58.6377 2 -1 1 0 2459.55 58.6473 2 0 -1 0 5.45036 0.73348 2 0 -1 0 6.13443 0.51569 3 0 -1 0 5.89434 0.83296 4 0 1 0 5.89533 0.82641 2 0 1 0 5.24125 0.74388 2 0 1 0 5.09174 0.77201 4 0 1 0 6.24538 0.55479 3 -1 -1 0 5530.25 138.015 1 1 1 0 5498.82 138.078 1 -2 -1 0 13.7116 1.72411 5 -2 -1 0 16.2388 2.14324 2 -2 -1 0 14.4412 2.15357 2 -2 -1 0 12.9381 1.57444 4 -2 -1 0 14.7731 1.70739 5 2 1 0 13.8330 1.64475 5 2 1 0 11.2348 2.04718 2 2 1 0 15.5028 2.11072 2 2 1 0 13.1110 1.52809 5 2 1 0 14.6380 1.63774 4 -3 -1 0 165.514 7.15859 5 -3 -1 0 161.450 7.19422 2 -3 -1 0 161.351 6.62992 5 -3 -1 0 165.008 6.39559 4 -3 -1 0 160.295 7.23076 2 3 1 0 160.643 6.20804 5 3 1 0 164.988 6.20176 4 3 1 0 148.906 6.98372 2 3 1 0 160.541 7.10736 2 3 1 0 161.488 6.22162 5 -4 -1 0 23.7250 2.71504 5 -4 -1 0 24.6290 3.27312 2 -4 -1 0 25.5755 2.52681 4 -4 -1 0 24.1790 2.72895 5 4 1 0 26.7831 2.50487 4 4 1 0 25.0783 2.36695 5 4 1 0 24.9046 2.34478 5 4 1 0 18.4164 2.92061 2 4 1 0 28.7583 3.26424 2 -5 -1 0 11.3881 2.30582 5 -5 -1 0 8.18280 2.20067 5 -5 -1 0 4.35416 2.13445 2 -5 -1 0 11.5582 2.93921 2 5 1 0 8.50899 2.47040 2 5 1 0 7.00614 1.65399 5 5 1 0 7.12159 2.64010 2 5 1 0 9.69711 2.01871 4 5 1 0 8.66676 1.86047 5 -6 -1 0 1.71825 2.18359 2 -6 -1 0 2.25142 1.79102 5 -6 -1 0 6.08761 2.45140 2 6 1 0 2.90931 1.58978 4 6 1 0 2.64512 1.28118 5 6 1 0 2.90610 1.94449 2 -7 -1 0 10.9575 3.16612 2 -7 -1 0 2.12869 2.42233 2 7 1 0 8.62759 3.36880 2 7 1 0 5.11112 1.56483 5 7 1 0 6.45288 1.61771 5 7 -2 0 -3.0646 2.60906 2 -7 2 0 4.58782 2.26175 2 -7 2 0 -0.3876 2.01457 2 -7 2 0 1.05483 1.80444 5 6 -2 0 9.60040 2.45060 2 -6 2 0 1.83733 1.73145 4 -6 2 0 4.76630 1.99835 2 -6 2 0 9.26263 2.09040 5 -6 2 0 4.14392 1.86034 5 -6 2 0 3.61940 1.99431 2 -5 2 0 10.7437 1.95098 4 -5 2 0 10.6987 2.32120 2 -5 2 0 12.7366 2.17296 5 -5 2 0 14.0650 2.62795 2 -5 2 0 13.1568 2.20051 5 4 -2 0 20.0651 2.22588 2 -4 2 0 23.3161 2.18465 5 -4 2 0 20.5730 2.33738 2 -4 2 0 17.8680 2.60525 5 -4 2 0 21.4729 2.46562 2 -4 2 0 19.3410 1.97243 4 3 -2 0 52.0746 2.81213 2 3 -2 0 51.2215 2.72625 2 -3 2 0 50.0150 2.90006 2 -3 2 0 50.2132 3.02976 2 -3 2 0 50.9141 2.64979 4 2 -2 0 1.44134 0.60636 2 2 -2 0 0.91413 0.49964 2 -2 2 0 0.45352 0.57381 2 -2 2 0 0.70284 0.54013 2 -1 2 0 945.083 23.5247 4 0 -2 0 9999.99 236.965 1 0 2 0 9743.58 237.242 1 -1 -2 0 214.809 6.37708 5 -1 -2 0 219.473 6.01084 3 -1 -2 0 217.751 6.51041 5 -1 -2 0 215.760 7.49935 2 -1 -2 0 216.181 7.35671 4 -1 -2 0 213.000 7.17456 2 1 2 0 212.515 6.72052 5 1 2 0 213.258 6.86482 5 1 2 0 216.287 7.10855 4 1 2 0 215.177 7.28312 2 1 2 0 214.784 7.54308 2 -2 -2 0 50.7996 3.72720 2 -2 -2 0 56.1384 3.55662 5 -2 -2 0 52.9684 3.10340 3 -2 -2 0 51.0807 3.75839 2 -2 -2 0 54.8287 3.28835 5 2 2 0 59.7243 3.37353 5 2 2 0 56.7132 3.75986 2 2 2 0 56.6204 3.31398 4 2 2 0 56.1433 3.84689 2 -3 -2 0 113.479 6.25288 2 -3 -2 0 125.990 6.43480 2 -3 -2 0 114.505 5.60079 5 -3 -2 0 117.492 5.60849 4 3 2 0 119.697 5.46824 5 3 2 0 110.134 5.34596 5 3 2 0 120.923 6.19872 2 3 2 0 117.337 6.32301 2 3 2 0 118.854 5.48845 4 -4 -2 0 28.3452 3.15264 5 -4 -2 0 29.7944 3.64416 2 -4 -2 0 32.3553 3.09809 4 -4 -2 0 29.4474 3.61606 2 4 2 0 32.9539 2.95466 5 4 2 0 30.9388 2.87511 5 4 2 0 29.3187 3.44236 2 4 2 0 35.6730 3.05449 4 4 2 0 28.6888 3.76930 2 -5 -2 0 21.4457 3.52837 2 -5 -2 0 19.8190 2.96056 4 -5 -2 0 18.2950 3.58265 2 5 2 0 15.7323 3.28855 2 5 2 0 21.5064 2.75905 5 5 2 0 18.7225 2.58919 5 5 2 0 19.1421 2.70134 4 5 2 0 21.8291 4.29522 2 -6 -2 0 66.9561 6.29071 2 6 2 0 65.3565 4.61883 5 6 2 0 63.4421 5.90217 2 -7 -2 0 -0.1545 2.19901 2 7 2 0 -0.4514 1.64963 4 7 2 0 -1.2852 1.18875 5 7 2 0 -1.0919 1.88242 2 -7 3 0 3.69513 2.30936 5 -7 3 0 2.66520 2.11589 2 6 -3 0 1.77842 1.88076 2 -6 3 0 -1.2192 1.64152 4 -6 3 0 2.88796 1.74043 5 -6 3 0 1.44093 2.01670 5 -6 3 0 2.41817 1.66670 2 -6 3 0 3.44984 2.00876 2 5 -3 0 9.29438 1.97767 2 -5 3 0 7.34374 1.76253 4 -5 3 0 5.38901 1.68717 2 -5 3 0 7.16211 1.90975 2 -5 3 0 7.41784 1.84211 5 -5 3 0 5.10680 1.59936 5 4 -3 0 8.02339 1.62700 2 4 -3 0 13.2914 1.75738 2 -4 3 0 12.3261 1.85301 2 -4 3 0 14.6199 1.67452 4 -4 3 0 12.8510 1.74130 2 -3 3 0 9.42325 1.37492 2 -3 3 0 11.5173 1.35476 2 -2 3 0 903.718 23.1720 4 -1 3 0 237.757 7.52583 4 -1 3 0 244.314 7.46898 3 0 -3 0 5.89641 1.25754 4 0 -3 0 4.78141 0.99367 2 0 -3 0 6.17629 1.02176 2 0 3 0 3.39107 1.09029 2 0 3 0 5.47119 1.13935 2 0 3 0 4.52952 1.16758 4 0 3 0 4.87294 0.76634 3 -1 -3 0 1197.66 28.6306 5 -1 -3 0 1178.38 29.0676 5 -1 -3 0 1145.83 30.4353 2 -1 -3 0 1163.99 30.6791 2 -1 -3 0 1195.73 28.3292 3 -1 -3 0 1189.90 30.7980 4 1 3 0 1185.66 30.6198 4 1 3 0 1170.66 29.9687 5 1 3 0 1144.43 29.6715 5 1 3 0 1160.98 30.5048 2 1 3 0 1119.78 30.6001 2 -2 -3 0 0.32650 0.91111 5 -2 -3 0 0.96054 1.13486 2 -2 -3 0 -0.1295 0.74593 5 -2 -3 0 0.14031 0.68670 3 -2 -3 0 0.13383 0.89440 2 -2 -3 0 0.97713 0.99955 4 2 3 0 0.16220 0.80707 5 2 3 0 -0.9185 0.91216 2 2 3 0 0.87005 0.81466 5 -3 -3 0 23.3699 2.56187 5 -3 -3 0 24.1428 3.10872 2 -3 -3 0 36.4349 3.14282 5 -3 -3 0 30.2013 2.63737 3 -3 -3 0 33.4589 3.47717 2 -3 -3 0 23.6566 2.63562 4 3 3 0 26.4063 3.24394 2 3 3 0 30.4946 2.84622 5 3 3 0 35.2410 3.55115 2 3 3 0 30.9125 2.89670 4 3 3 0 26.5398 2.58463 5 -4 -3 0 31.0775 3.23618 3 -4 -3 0 38.4639 4.09347 2 -4 -3 0 35.6848 4.01988 2 -4 -3 0 32.0021 3.35494 5 4 3 0 32.4957 3.97140 2 4 3 0 29.1666 3.62595 5 4 3 0 26.7404 3.62883 2 4 3 0 28.9306 3.17668 5 4 3 0 28.2510 3.13263 4 -5 -3 0 42.0631 4.66134 3 -5 -3 0 41.5120 4.44046 5 -5 -3 0 49.7777 5.96081 2 -5 -3 0 40.7975 4.99107 2 5 3 0 42.5339 4.80192 2 5 3 0 44.4817 4.16174 4 5 3 0 39.2777 5.19500 2 5 3 0 43.6933 3.94514 5 -6 -3 0 14.3024 3.92415 2 -6 -3 0 13.7488 3.33663 5 6 3 0 9.61789 3.52948 2 6 3 0 12.6791 2.77010 4 6 3 0 15.7267 3.42006 5 -7 -3 0 10.6984 3.39228 2 -7 -3 0 16.0360 3.90583 5 7 3 0 9.09824 2.60256 5 7 3 0 15.2344 3.18837 4 -6 4 0 6.99136 2.32668 5 -6 4 0 9.11074 3.29362 5 -6 4 0 11.8358 2.32216 2 -5 4 0 85.3602 4.49300 2 -5 4 0 80.5518 4.73699 4 -4 4 0 29.9627 2.48650 4 -3 4 0 19.5456 2.04219 4 -2 4 0 95.5106 4.25024 4 -2 4 0 94.8670 4.78943 3 -1 4 0 883.783 23.4804 4 -1 4 0 879.016 22.7812 3 0 -4 0 33.4194 2.26122 2 0 -4 0 40.0062 2.20001 2 0 -4 0 37.5643 2.71879 4 0 4 0 36.1099 2.61398 2 0 4 0 36.4934 1.73185 3 0 4 0 33.3405 2.64362 4 0 4 0 34.5175 2.45820 2 -1 -4 0 584.174 16.8989 2 -1 -4 0 570.033 17.0719 4 -1 -4 0 564.425 16.6764 2 1 4 0 570.489 16.1073 5 1 4 0 579.124 17.1710 2 1 4 0 581.710 16.1605 5 1 4 0 582.498 16.8633 2 -2 -4 0 1.22180 0.96726 5 -2 -4 0 0.20086 1.18256 2 -2 -4 0 2.02832 1.10709 4 -2 -4 0 1.02875 1.25367 2 -2 -4 0 1.47691 0.87454 5 -2 -4 0 1.68725 0.77990 3 2 4 0 1.03183 1.13244 4 2 4 0 1.35131 1.29526 2 2 4 0 0.71178 1.45964 2 2 4 0 1.75200 1.06482 5 -3 -4 0 22.7175 3.24047 2 -3 -4 0 21.0028 3.28944 2 -3 -4 0 24.9043 2.70711 5 -3 -4 0 25.0227 2.94525 4 -3 -4 0 21.9651 2.57749 3 -3 -4 0 21.7303 2.67088 5 3 4 0 21.8304 2.62285 5 3 4 0 25.1095 2.92163 4 3 4 0 22.5915 2.79433 5 3 4 0 19.2715 3.33680 2 3 4 0 25.6342 3.26822 2 -4 -4 0 3.33647 1.67943 5 -4 -4 0 4.78312 1.82253 5 -4 -4 0 4.14375 1.76447 4 -4 -4 0 4.06820 2.10922 2 -4 -4 0 4.92244 2.12596 2 -4 -4 0 3.95052 1.50621 3 4 4 0 5.66535 2.03750 2 4 4 0 8.12920 2.47620 2 4 4 0 2.61939 1.30826 5 4 4 0 4.18359 1.56322 4 4 4 0 3.60113 1.73409 5 -5 -4 0 32.5116 4.16470 3 -5 -4 0 31.0634 4.83085 2 -5 -4 0 32.3590 4.17042 5 5 4 0 25.4990 5.24499 2 5 4 0 32.6152 4.54332 2 5 4 0 35.5993 6.00252 4 -6 -4 0 30.5498 4.39406 5 -6 -4 0 32.4405 5.45784 2 6 4 0 28.0340 5.60427 2 6 4 0 30.8146 3.91880 4 6 4 0 31.5314 3.93741 5 -7 -4 0 25.4867 4.52252 5 -7 -4 0 20.3791 5.36893 2 7 4 0 17.7406 4.73156 2 7 4 0 18.4076 3.39868 4 7 4 0 18.3468 3.49546 5 -6 5 0 13.8990 3.28158 5 -6 5 0 17.6360 3.32169 4 -6 5 0 18.3315 4.96372 3 -5 5 0 -0.4632 2.10377 3 -5 5 0 -0.6852 1.40897 4 -5 5 0 2.98400 1.31798 4 -4 5 0 56.4251 3.53250 4 -4 5 0 62.9052 5.69206 3 -4 5 0 58.8541 4.02640 4 -3 5 0 164.129 7.79044 4 -3 5 0 187.744 8.71530 3 -1 5 0 7.56822 1.48404 3 0 -5 0 28.3381 2.69627 4 0 -5 0 30.4418 2.30115 2 0 -5 0 26.4802 2.06413 2 0 5 0 29.0353 2.22386 2 0 5 0 26.9802 2.39227 2 0 5 0 31.0724 2.80089 4 -1 -5 0 39.6264 3.18978 2 -1 -5 0 40.2271 3.46923 4 -1 -5 0 39.6044 3.42503 2 1 5 0 40.2584 3.23743 2 1 5 0 31.7275 2.81931 5 1 5 0 40.7364 3.39450 2 1 5 0 40.1375 3.44658 4 -2 -5 0 88.1784 3.82234 5 -2 -5 0 88.6903 5.46441 2 -2 -5 0 90.1377 3.38841 3 -2 -5 0 91.5465 5.41369 4 2 5 0 94.3421 5.19640 5 2 5 0 88.6783 5.41681 2 2 5 0 98.7433 5.57208 4 2 5 0 91.2814 5.70979 2 -3 -5 0 42.1821 3.67053 3 -3 -5 0 45.2975 4.03666 4 -3 -5 0 45.2451 3.64139 5 -3 -5 0 45.9873 3.62442 5 -3 -5 0 46.3318 4.67553 2 -3 -5 0 42.3431 4.67083 2 3 5 0 51.9489 4.44308 4 3 5 0 44.9364 4.14117 5 3 5 0 46.4193 4.39105 2 3 5 0 46.4547 3.93732 5 3 5 0 56.6955 4.93677 2 -4 -5 0 20.0590 2.78578 3 -4 -5 0 14.9313 3.10748 5 -4 -5 0 14.1741 2.85598 5 4 5 0 15.9306 3.46332 2 4 5 0 16.9919 3.40081 2 4 5 0 16.8569 3.01498 4 4 5 0 17.0121 3.10598 5 -5 -5 0 32.7464 4.15074 3 -5 -5 0 36.1907 5.15317 2 5 5 0 28.8853 4.15964 5 5 5 0 37.8679 4.69734 2 5 5 0 36.6670 4.11404 4 -6 -5 0 -2.2832 1.63391 5 -6 -5 0 3.92496 2.90945 2 6 5 0 2.67789 2.47277 2 6 5 0 2.38892 1.75812 4 6 5 0 -0.8198 1.57001 5 -7 -5 0 29.4242 6.53196 2 7 5 0 26.6256 5.39633 2 7 5 0 24.4133 4.74066 4 -5 6 0 64.1665 5.16343 4 -5 6 0 63.4720 8.11400 3 -4 6 0 2.40714 2.00180 4 -4 6 0 3.48561 2.11075 3 -3 6 0 23.5113 3.04629 4 -3 6 0 23.7261 3.61123 3 -2 6 0 92.1464 5.21931 4 -2 6 0 84.4341 5.17963 3 -1 6 0 126.226 5.07726 3 -1 6 0 130.606 6.34610 4 0 -6 0 49.2555 2.93224 2 0 -6 0 48.6409 3.14267 2 0 -6 0 50.1860 3.94461 4 0 6 0 57.2178 4.23575 4 0 6 0 46.4995 3.32942 2 0 6 0 60.9528 3.37245 2 -1 -6 0 16.5890 2.60914 2 -1 -6 0 15.8203 2.82192 2 1 6 0 13.7145 2.33150 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1.88991 5 3 2 23 -2.0483 2.38927 2 3 2 23 1.70118 2.35162 3 3 2 23 0.66287 2.99382 4 -4 -2 -23 34.3002 4.76351 5 4 2 23 29.7131 4.93395 3 4 2 23 35.5388 5.36481 2 4 2 23 34.5010 5.95466 5 2 -3 -23 8.16799 3.24019 2 -2 3 23 4.54462 3.74080 3 -2 3 23 3.39528 5.01864 2 1 -3 -23 4.22947 3.22199 2 1 -3 -23 4.64968 2.23523 5 -1 3 23 5.54701 2.90487 4 -1 3 23 7.18031 2.81062 2 -1 3 23 3.74594 2.66224 3 -1 3 23 7.10875 2.78861 2 -1 3 23 6.71856 3.14888 5 0 -3 -23 1.73097 2.97277 2 0 -3 -23 2.05455 2.29868 5 0 3 23 7.67018 2.92551 2 0 3 23 5.12151 2.19928 5 0 3 23 0.88995 2.69854 3 0 3 23 5.99534 2.60330 4 -1 -3 -23 1.70794 1.73655 5 -1 -3 -23 3.82688 2.73725 2 1 3 23 4.95017 2.60516 3 1 3 23 3.59082 2.28481 5 1 3 23 1.78971 2.89976 2 1 3 23 3.08317 2.57558 4 -2 -3 -23 -1.4102 2.39035 2 -2 -3 -23 3.88890 2.27160 5 2 3 23 5.72715 2.71375 5 2 3 23 3.28745 2.83121 4 2 3 23 7.83367 3.21044 3 2 3 23 4.19940 3.19902 2 3 3 23 43.4193 5.85473 2 3 3 23 42.8430 5.66493 5 3 3 23 41.9865 4.62726 4 -4 -3 -23 40.6964 7.27457 5 4 3 23 46.7702 5.14831 5 4 3 23 43.0058 5.41070 4 4 3 23 47.3409 5.28036 3 4 3 23 44.5278 7.01238 2 2 -4 -23 3.06245 2.81023 2 -2 4 23 -2.2006 1.97362 2 -2 4 23 2.50794 2.32258 3 -2 4 23 1.49144 2.08218 4 1 -4 -23 0.75536 3.23234 2 -1 4 23 0.25319 2.80603 4 -1 4 23 -0.7111 1.98326 5 0 -4 -23 3.02631 3.46563 2 0 -4 -23 8.13634 2.44291 5 0 4 23 10.8027 3.44749 3 0 4 23 9.04806 3.28765 4 0 4 23 9.96594 3.43142 2 0 4 23 7.55951 2.95386 5 -1 -4 -23 -0.6329 1.85381 5 -1 -4 -23 3.90583 2.77103 2 1 4 23 2.59039 2.66486 3 1 4 23 3.47983 2.60218 2 1 4 23 -2.9208 2.25539 5 1 4 23 -0.6989 2.25609 4 -2 -4 -23 2.67023 2.30255 5 2 4 23 1.52611 5.20182 3 2 4 23 1.62014 2.94786 2 2 4 23 5.47952 2.73966 5 2 4 23 5.48675 2.69668 4 -3 -4 -23 11.2710 3.14439 5 -3 -4 -23 5.44725 3.99800 2 3 4 23 5.69688 4.15440 2 3 4 23 7.83566 3.53154 3 3 4 23 12.6156 3.03686 4 3 4 23 10.3086 3.31636 5 -1 5 23 -0.0550 2.30737 3 -1 5 23 0.89205 1.96699 2 -1 5 23 1.70898 2.22526 4 0 -5 -23 69.8115 6.78418 2 0 5 23 71.6699 7.28446 3 0 5 23 72.5903 7.05786 5 -1 -5 -23 7.22657 3.90908 2 1 5 23 1.23410 4.10555 3 1 5 23 7.83730 3.80409 4 1 5 23 3.56091 3.54317 2 -2 -5 -23 3.05299 3.53429 5 -2 -5 -23 -2.3387 2.63704 2 2 5 23 3.11479 2.33014 4 2 5 23 1.82400 2.54172 2 2 5 23 -0.4985 2.84615 3 2 5 23 0.93519 2.33946 5 -3 -5 -23 -1.6329 2.75369 2 3 5 23 2.82970 2.43201 4 0 2 -24 44.4856 7.11103 2 0 -2 24 41.4070 6.09348 2 0 -2 24 38.2593 5.72053 3 0 -2 24 40.0659 4.60357 5 1 -2 24 8.71638 3.22832 4 1 1 -24 7.42858 3.64022 2 -1 -1 24 10.6224 2.93678 3 -1 -1 24 12.3943 3.96214 5 -1 -1 24 6.19713 3.60873 2 0 1 -24 4.77427 2.78794 2 0 -1 24 4.08889 2.66653 3 0 -1 24 -2.4027 2.19737 5 -1 1 -24 47.7187 5.33287 2 1 -1 24 46.0742 5.24909 3 1 -1 24 40.9816 4.76343 5 1 -1 24 40.9050 6.16137 2 1 -1 24 44.0577 4.60837 4 -2 1 -24 1.85220 2.52309 5 2 -1 24 4.84239 3.17780 3 2 -1 24 3.40631 3.66964 2 2 -1 24 0.21427 2.85830 5 2 -1 24 3.96510 2.72548 4 2 0 -24 5.50835 2.04971 5 2 0 -24 6.56113 2.43392 2 -2 0 24 5.00625 2.37993 5 -2 0 24 4.02961 3.22092 3 1 0 -24 28.2651 3.58687 5 1 0 -24 34.5201 4.94730 2 -1 0 24 25.3214 4.61168 2 -1 0 24 25.9466 4.52147 3 -1 0 24 22.5715 5.19288 5 0 0 24 64.2771 5.61529 5 0 0 24 74.9750 6.34156 3 1 0 24 14.1280 4.18345 2 1 0 24 11.9667 3.87146 3 1 0 24 23.2544 3.95883 5 1 0 24 14.6790 4.41510 4 -2 0 -24 1.69112 2.55379 2 2 0 24 0.47134 2.59330 2 2 0 24 0.38576 2.21742 5 2 0 24 -0.9523 1.97816 4 2 0 24 -2.2771 2.30989 3 -3 0 -24 -4.1936 2.11396 2 -3 0 -24 -3.5116 1.50926 5 3 0 24 -7.1770 2.43111 2 3 0 24 -1.2344 2.12188 5 3 0 24 -2.1700 1.89538 4 2 -1 -24 14.5518 2.90219 5 2 -1 -24 12.8073 4.18096 2 -2 1 24 10.1445 3.37667 5 -2 1 24 11.2149 4.41940 2 1 -1 -24 49.2456 5.63350 2 1 -1 -24 47.9828 4.27741 5 -1 1 24 49.2465 5.26025 2 -1 1 24 55.3739 5.76205 3 -1 1 24 41.4847 6.45714 5 0 1 24 22.8531 4.26523 5 0 1 24 24.2370 4.47894 4 0 1 24 34.6545 4.75962 3 -1 -1 -24 12.1950 3.67523 2 -1 -1 -24 25.3275 3.60362 5 1 1 24 13.6099 3.44119 5 1 1 24 22.2607 4.50247 2 1 1 24 17.2704 3.21175 4 1 1 24 32.1487 4.71834 3 -2 -1 -24 1.20167 3.01099 2 -2 -1 -24 2.24002 1.89339 5 2 1 24 8.63496 2.74999 2 2 1 24 2.00342 2.93792 4 2 1 24 3.57103 2.45587 5 2 1 24 -0.0682 2.25557 3 -3 -1 -24 26.3107 4.66076 5 3 1 24 19.4674 4.46852 5 3 1 24 25.8356 5.03308 2 3 1 24 27.4909 4.37958 4 2 -2 -24 0.85777 3.50340 2 -2 2 24 3.23057 3.26754 3 -2 2 24 3.96180 2.56084 5 -2 2 24 3.35743 3.01168 2 1 -2 -24 52.8507 6.87417 2 1 -2 -24 67.5952 4.82834 5 0 -2 -24 37.6225 4.97861 2 0 -2 -24 30.9776 3.84622 5 0 2 24 45.4876 5.27085 3 0 2 24 30.1514 4.58114 4 0 2 24 29.1939 4.60192 5 -1 -2 -24 24.8170 3.63141 5 -1 -2 -24 20.5849 4.38112 2 1 2 24 27.8843 4.53689 3 1 2 24 15.7009 4.23289 2 1 2 24 22.2333 3.90816 5 1 2 24 21.1178 4.41836 4 -2 -2 -24 -3.6831 2.18317 2 -2 -2 -24 3.18653 2.01267 5 2 2 24 -1.8473 2.13304 4 2 2 24 -3.0906 2.15770 3 2 2 24 3.68245 2.26453 5 2 2 24 3.93855 2.73046 2 -3 -2 -24 -1.6169 2.28278 2 -3 -2 -24 0.06351 3.99562 5 3 2 24 0.26641 2.72565 4 3 2 24 -1.1426 2.32000 3 3 2 24 2.08841 3.41676 2 2 -3 -24 -0.5398 2.71793 2 -2 3 24 0.52450 3.14799 3 -2 3 24 -0.3157 1.85506 5 -1 3 24 92.8824 12.0676 3 0 -3 -24 37.7390 4.40264 5 0 3 24 45.5870 5.76825 3 0 3 24 46.3668 5.63422 2 0 3 24 53.6759 5.83430 5 -1 -3 -24 0.36882 3.72379 2 -1 -3 -24 10.2713 2.67961 5 1 3 24 4.10996 2.90846 4 1 3 24 8.83231 3.55533 2 1 3 24 13.4924 3.43039 3 1 3 24 13.9671 4.28076 5 -2 -3 -24 6.23396 3.26237 2 -2 -3 -24 6.75862 2.31820 5 2 3 24 0.40635 3.18192 2 2 3 24 7.95601 2.56861 4 -3 -3 -24 1.45417 1.88620 5 -3 -3 -24 5.52800 3.24578 2 3 3 24 -0.1477 2.50585 3 3 3 24 3.59040 2.16551 4 3 3 24 -0.4593 2.13131 5 3 3 24 0.27042 2.31325 2 1 -4 -24 -1.1362 2.87574 2 -1 4 24 7.19752 3.21288 2 -1 4 24 9.04567 3.27020 4 -1 4 24 9.52714 2.82028 5 -1 4 24 8.19091 4.09333 3 0 4 24 72.0632 6.85316 5 0 4 24 64.2459 6.55974 4 -1 -4 -24 -0.6120 2.07033 5 -1 -4 -24 -2.4596 2.68462 2 1 4 24 -1.2082 2.39392 3 1 4 24 -2.6071 2.09996 4 -2 -4 -24 1.65752 3.70346 2 -2 -4 -24 3.01529 1.82175 5 2 4 24 3.22856 2.51037 5 2 4 24 -0.1860 3.22675 2 2 4 24 1.82922 3.18487 3 2 4 24 3.25542 2.61477 4 -3 -4 -24 1.39534 3.81193 2 0 5 24 -1.7102 2.24258 4 -1 -5 -24 40.6180 7.08230 2 1 5 24 39.7252 6.53144 2 1 5 24 43.7908 5.44977 3 1 0 -25 4.32876 2.61497 5 1 0 -25 3.07395 3.28631 2 -1 0 25 -0.2395 2.10102 5 -1 0 25 2.11593 3.47346 3 -1 0 25 4.28533 3.31836 2 0 0 -25 10.5862 3.44091 5 0 0 -25 8.24670 3.85383 2 0 0 25 15.4795 3.77729 4 0 0 25 16.5990 4.47842 3 -1 0 -25 8.98798 3.04924 5 -1 0 -25 6.11267 3.34261 2 1 0 25 9.30326 2.99495 3 1 0 25 6.27521 3.53462 2 1 0 25 8.17817 3.42255 4 1 0 25 2.33735 3.20617 5 2 0 25 17.6183 3.39148 4 2 0 25 22.3649 3.93134 5 1 -1 -25 -1.2111 2.32146 2 1 -1 -25 1.69509 1.76713 5 -1 1 25 -1.1054 2.28047 5 0 -1 -25 0.52911 2.98086 2 0 -1 -25 4.22195 2.36534 5 0 1 25 -0.8336 2.54997 3 0 1 25 2.42218 3.48857 2 0 1 25 0.37393 2.88125 4 -1 -1 -25 0.53181 1.71553 5 -1 -1 -25 0.91888 2.26674 2 1 1 25 0.31038 2.47981 2 1 1 25 -0.6426 2.16324 4 1 1 25 -3.5070 2.44234 3 -2 -1 -25 0.17488 3.20133 2 2 1 25 3.04703 3.49913 2 2 1 25 -2.1908 2.00006 4 1 -2 -25 18.1394 3.65012 5 1 -2 -25 14.2903 4.20547 2 -1 2 25 14.3104 3.95060 5 -1 2 25 12.7576 3.61150 4 -1 2 25 17.0400 4.07505 3 0 -2 -25 2.27296 2.45208 2 0 -2 -25 -1.0717 1.70412 5 0 2 25 -2.6185 2.01999 5 0 2 25 -0.6088 3.18304 2 0 2 25 1.73079 2.23425 4 -1 -2 -25 5.18857 2.59221 5 -1 -2 -25 1.44704 3.41934 2 1 2 25 6.71037 3.52404 5 1 2 25 -0.0150 2.07631 4 1 2 25 5.22770 3.63013 2 -2 -2 -25 3.81501 3.33692 2 -2 -2 -25 4.29383 2.10113 5 2 2 25 5.34792 3.00544 2 2 2 25 4.74254 2.53164 5 2 2 25 -0.5490 2.11405 4 2 2 25 4.06528 3.58641 3 1 -3 -25 21.0800 4.70907 2 1 -3 -25 25.3678 5.18849 5 -1 3 25 25.7316 4.71780 3 -1 3 25 28.1482 5.00836 4 -1 3 25 25.6638 4.53499 2 -1 3 25 23.5061 4.04904 5 0 -3 -25 14.5010 2.90189 5 0 3 25 4.18389 3.39487 2 0 3 25 11.1887 4.02454 3 0 3 25 10.7267 3.45134 4 0 3 25 2.69852 3.02457 5 -1 -3 -25 0.02362 2.19454 5 -1 -3 -25 2.92961 2.95813 2 1 3 25 1.24275 2.85699 5 1 3 25 -1.2562 2.12042 4 1 3 25 2.55692 4.57821 2 1 3 25 0.37558 3.35172 3 -2 -3 -25 2.09302 2.67595 2 -2 -3 -25 1.10798 1.73995 5 2 3 25 -2.1237 1.96220 5 2 3 25 -1.6707 2.24014 3 2 3 25 0.86726 3.06697 4 0 4 25 2.16069 2.30193 4 -1 -4 -25 0.21827 2.47287 5 1 4 25 -1.5512 2.14995 2 1 4 25 0.97336 2.54178 3 1 4 25 2.69136 2.70364 4 1 4 25 -1.1362 1.78416 5 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 72623 _shelx_res_file ; TITL m22270 : space group P1bar m22270.res created by SHELXL-2019/2 at 17:55:48 on 27-Feb-2023 CELL 0.71073 6.1481 7.3467 19.9801 80.190 86.089 82.843 ZERR 2 0.0013 0.0012 0.0040 0.006 0.005 0.006 LATT 1 SFAC C H N O UNIT 38 52 4 8 TEMP -183 SIZE 0.29 0.21 0.02 REM FORM plate REM COLR colourless L.S. 10 BOND $H LIST 4 ACTA CONF REM Instructions for potential hydrogen bonds HTAB N1 O2 EQIV $1 -x+1, -y+2, -z+1 HTAB N1 O1W_$1 HTAB C1 O1W HTAB C2 O3_$1 EQIV $2 -x, -y+1, -z+1 HTAB C4 O2_$2 EQIV $3 x-1, y, z HTAB C4 O1W_$3 HTAB O1W O3 EQIV $4 x+1, y, z HTAB O1W O2_$4 HTAB REM Relative twist of benzene and piperazinium rings: MPLA C1 C2 C3 C4 MPLA C5 C6 C7 C8 C9 C10 REM Out of planarity of methoxy group: RTAB tors C9 C8 O1 C11 MPLA 7 C5 C6 C7 C8 C9 C10 O1 C11 REM Out of planarity of N2: RTAB angl C2 N2 C3 RTAB angl C3 N2 C5 RTAB angl C5 N2 C2 REM Planarity of anion: MPLA C12 O2 O3 MPLA C13 C14 C15 C16 C17 C18 REM FMAP 2 PLAN 20 WGHT 0.012400 0.373200 EXTI 0.003793 FVAR 0.65064 N1 3 0.238870 0.747868 0.543555 11.00000 0.02021 0.01975 = 0.01779 -0.00259 -0.00132 -0.00366 H1A 2 0.202785 0.727005 0.496118 11.00000 0.04230 H1B 2 0.271181 0.871185 0.538454 11.00000 0.03324 N2 3 0.284440 0.653895 0.688841 11.00000 0.01485 0.02335 = 0.01566 -0.00378 -0.00073 -0.00212 C1 1 0.427270 0.618874 0.572710 11.00000 0.01915 0.02249 = 0.01873 -0.00455 -0.00033 -0.00063 AFIX 23 H1C 2 0.558241 0.630796 0.541287 11.00000 -1.20000 H1D 2 0.392248 0.489067 0.578218 11.00000 -1.20000 AFIX 0 C2 1 0.476031 0.663146 0.640909 11.00000 0.01619 0.02437 = 0.01841 -0.00345 0.00059 -0.00327 AFIX 23 H2A 2 0.598899 0.573865 0.660243 11.00000 -1.20000 H2B 2 0.522549 0.789461 0.634542 11.00000 -1.20000 AFIX 0 C3 1 0.088722 0.767108 0.660092 11.00000 0.01557 0.02759 = 0.01987 -0.00371 -0.00082 -0.00124 AFIX 23 H3A 2 0.108509 0.900258 0.656176 11.00000 -1.20000 H3B 2 -0.039758 0.743193 0.691596 11.00000 -1.20000 AFIX 0 C4 1 0.042654 0.727296 0.590891 11.00000 0.01746 0.02774 = 0.02076 -0.00265 -0.00093 -0.00373 AFIX 23 H4A 2 0.002660 0.599190 0.595399 11.00000 -1.20000 H4B 2 -0.082879 0.814471 0.572187 11.00000 -1.20000 AFIX 0 C5 1 0.324635 0.680518 0.755656 11.00000 0.01979 0.01875 = 0.01660 -0.00203 0.00012 -0.00469 C6 1 0.528454 0.624812 0.783502 11.00000 0.01881 0.02976 = 0.01966 -0.00590 0.00089 -0.00165 AFIX 43 H6 2 0.644111 0.569862 0.756838 11.00000 -1.20000 AFIX 0 C7 1 0.568011 0.647154 0.849227 11.00000 0.01913 0.03584 = 0.02139 -0.00429 -0.00414 -0.00259 AFIX 43 H7 2 0.709269 0.608607 0.866686 11.00000 -1.20000 AFIX 0 C8 1 0.402060 0.725237 0.888931 11.00000 0.02692 0.03032 = 0.01603 -0.00591 -0.00093 -0.00558 C9 1 0.197080 0.777371 0.862815 11.00000 0.02495 0.03621 = 0.02098 -0.00918 0.00241 0.00078 AFIX 43 H9 2 0.080563 0.827557 0.890402 11.00000 -1.20000 AFIX 0 C10 1 0.158825 0.757709 0.797257 11.00000 0.01973 0.03342 = 0.02241 -0.00636 -0.00203 -0.00022 AFIX 43 H10 2 0.017294 0.797357 0.780137 11.00000 -1.20000 AFIX 0 O1 4 0.421456 0.758520 0.954107 11.00000 0.02885 0.05445 = 0.01989 -0.01377 -0.00441 -0.00101 C11 1 0.632198 0.713601 0.982039 11.00000 0.03193 0.06641 = 0.02269 -0.01352 -0.00607 -0.00792 AFIX 137 H11A 2 0.623438 0.740327 1.028619 11.00000 -1.50000 H11B 2 0.737047 0.788298 0.954254 11.00000 -1.50000 H11C 2 0.681120 0.581268 0.982463 11.00000 -1.50000 AFIX 0 REM Anion O2 4 0.122345 0.711505 0.417004 11.00000 0.02609 0.02702 = 0.01941 -0.00441 -0.00177 -0.00234 O3 4 0.399695 0.876628 0.379689 11.00000 0.03241 0.03650 = 0.03102 -0.00586 -0.01147 -0.01216 C12 1 0.241286 0.795663 0.369754 11.00000 0.02069 0.01714 = 0.02426 -0.00612 -0.00515 0.00246 C13 1 0.188238 0.795387 0.297438 11.00000 0.01874 0.01847 = 0.01980 -0.00452 -0.00254 0.00084 C14 1 0.330219 0.862500 0.244106 11.00000 0.01763 0.02364 = 0.02828 -0.00590 -0.00148 -0.00365 AFIX 43 H14 2 0.457991 0.912589 0.253423 11.00000 -1.20000 AFIX 0 C15 1 0.285475 0.856383 0.177330 11.00000 0.02412 0.03072 = 0.02179 -0.00319 0.00290 -0.00305 AFIX 43 H15 2 0.384517 0.901179 0.141471 11.00000 -1.20000 AFIX 0 C16 1 0.098630 0.785989 0.162023 11.00000 0.02655 0.02607 = 0.01955 -0.00548 -0.00326 0.00092 C17 1 -0.044801 0.722761 0.215579 11.00000 0.02159 0.02344 = 0.02437 -0.00606 -0.00476 -0.00338 AFIX 43 H17 2 -0.174944 0.676288 0.206177 11.00000 -1.20000 AFIX 0 C18 1 -0.000362 0.726705 0.282263 11.00000 0.01941 0.01955 = 0.02098 -0.00273 -0.00064 -0.00198 AFIX 43 H18 2 -0.099671 0.682046 0.318066 11.00000 -1.20000 AFIX 0 C19 1 0.047416 0.778927 0.089860 11.00000 0.03969 0.04503 = 0.02232 -0.00803 -0.00379 -0.00434 AFIX 137 H19A 2 -0.003498 0.658960 0.087676 11.00000 -1.50000 H19B 2 0.179989 0.793648 0.060251 11.00000 -1.50000 H19C 2 -0.067539 0.879581 0.074736 11.00000 -1.50000 AFIX 0 O1W 4 0.721073 0.874924 0.461150 11.00000 0.02293 0.02603 = 0.02449 -0.00452 -0.00430 -0.00455 H1W 2 0.599661 0.873859 0.432783 11.00000 0.06245 H2W 2 0.849635 0.813123 0.442906 11.00000 0.06040 HKLF 4 REM m22270 : space group P1bar REM wR2 = 0.0799, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0381 for 3137 Fo > 4sig(Fo) and 0.0595 for all 4059 data REM 245 parameters refined using 0 restraints END WGHT 0.0124 0.3732 REM Instructions for potential hydrogen bonds HTAB N1 O2 HTAB N1 O1W_$1 HTAB C1 O1W HTAB C2 O3_$1 HTAB C4 O2_$2 HTAB C4 O1W_$3 HTAB O1W O3 HTAB O1W O2_$4 REM Highest difference peak 0.191, deepest hole -0.180, 1-sigma level 0.040 Q1 1 0.2193 0.8728 0.2720 11.00000 0.05 0.19 Q2 1 0.4357 0.7360 0.7487 11.00000 0.05 0.19 Q3 1 0.0597 0.7825 0.1311 11.00000 0.05 0.18 Q4 1 0.5550 0.6602 0.8126 11.00000 0.05 0.17 Q5 1 0.2567 0.9238 0.4208 11.00000 0.05 0.17 Q6 1 0.2021 0.8055 0.3309 11.00000 0.05 0.17 Q7 1 0.1243 0.7448 0.2917 11.00000 0.05 0.17 Q8 1 0.2940 0.7790 0.2735 11.00000 0.05 0.17 Q9 1 0.2535 0.7455 0.7722 11.00000 0.05 0.16 Q10 1 0.3088 0.6795 0.7177 11.00000 0.05 0.16 Q11 1 0.0675 0.7336 0.1929 11.00000 0.05 0.15 Q12 1 0.3186 0.8342 0.2136 11.00000 0.05 0.15 Q13 1 0.4760 0.7399 0.8560 11.00000 0.05 0.15 Q14 1 0.0761 0.8905 0.6713 11.00000 0.05 0.15 Q15 1 -0.1976 0.7329 0.3705 11.00000 0.05 0.15 Q16 1 0.0787 0.8008 0.2854 11.00000 0.05 0.15 Q17 1 0.2276 0.7644 0.1697 11.00000 0.05 0.15 Q18 1 0.5843 0.8615 1.0388 11.00000 0.05 0.15 Q19 1 0.4221 0.6567 0.7727 11.00000 0.05 0.15 Q20 1 0.4769 0.6447 0.8728 11.00000 0.05 0.15 ; _shelx_res_checksum 13087 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N1 0.23887(18) 0.74787(16) 0.54355(5) 0.0192(2) Uani d 1 . . H H1A 0.203(3) 0.727(2) 0.4961(9) 0.042(5) Uiso d 1 . . H H1B 0.271(3) 0.871(2) 0.5385(8) 0.033(4) Uiso d 1 . . N N2 0.28444(17) 0.65390(15) 0.68884(5) 0.0179(2) Uani d 1 . . C C1 0.4273(2) 0.61887(18) 0.57271(6) 0.0202(3) Uani d 1 . . H H1C 0.558241 0.630796 0.541287 0.024 Uiso calc 1 . . H H1D 0.392248 0.489067 0.578218 0.024 Uiso calc 1 . . C C2 0.4760(2) 0.66315(19) 0.64091(6) 0.0196(3) Uani d 1 . . H H2A 0.598899 0.573865 0.660243 0.024 Uiso calc 1 . . H H2B 0.522549 0.789461 0.634542 0.024 Uiso calc 1 . . C C3 0.0887(2) 0.76711(19) 0.66009(6) 0.0211(3) Uani d 1 . . H H3A 0.108509 0.900258 0.656176 0.025 Uiso calc 1 . . H H3B -0.039758 0.743193 0.691596 0.025 Uiso calc 1 . . C C4 0.0427(2) 0.7273(2) 0.59089(6) 0.0220(3) Uani d 1 . . H H4A 0.002660 0.599190 0.595399 0.026 Uiso calc 1 . . H H4B -0.082879 0.814471 0.572187 0.026 Uiso calc 1 . . C C5 0.3246(2) 0.68052(18) 0.75566(6) 0.0183(3) Uani d 1 . . C C6 0.5285(2) 0.62481(19) 0.78350(6) 0.0227(3) Uani d 1 . . H H6 0.644111 0.569862 0.756838 0.027 Uiso calc 1 . . C C7 0.5680(2) 0.6472(2) 0.84923(7) 0.0254(3) Uani d 1 . . H H7 0.709269 0.608607 0.866686 0.030 Uiso calc 1 . . C C8 0.4021(2) 0.7252(2) 0.88893(6) 0.0240(3) Uani d 1 . . C C9 0.1971(2) 0.7774(2) 0.86282(7) 0.0274(3) Uani d 1 . . H H9 0.080563 0.827557 0.890402 0.033 Uiso calc 1 . . C C10 0.1588(2) 0.7577(2) 0.79726(7) 0.0252(3) Uani d 1 . . H H10 0.017294 0.797357 0.780137 0.030 Uiso calc 1 . . O O1 0.42146(17) 0.75852(16) 0.95411(5) 0.0337(3) Uani d 1 . . C C11 0.6322(3) 0.7136(3) 0.98204(7) 0.0392(4) Uani d 1 . . H H11A 0.623438 0.740327 1.028619 0.059 Uiso calc 1 . . H H11B 0.737047 0.788298 0.954254 0.059 Uiso calc 1 . . H H11C 0.681120 0.581268 0.982463 0.059 Uiso calc 1 . . O O2 0.12234(15) 0.71150(13) 0.41700(4) 0.0241(2) Uani d 1 . . O O3 0.39970(17) 0.87663(14) 0.37969(5) 0.0321(3) Uani d 1 . . C C12 0.2413(2) 0.79566(18) 0.36975(7) 0.0206(3) Uani d 1 . . C C13 0.1882(2) 0.79539(18) 0.29744(6) 0.0190(3) Uani d 1 . . C C14 0.3302(2) 0.86250(19) 0.24411(7) 0.0229(3) Uani d 1 . . H H14 0.457991 0.912589 0.253423 0.027 Uiso calc 1 . . C C15 0.2855(2) 0.8564(2) 0.17733(7) 0.0259(3) Uani d 1 . . H H15 0.384517 0.901179 0.141471 0.031 Uiso calc 1 . . C C16 0.0986(2) 0.78599(19) 0.16202(7) 0.0241(3) Uani d 1 . . C C17 -0.0448(2) 0.72276(19) 0.21558(7) 0.0226(3) Uani d 1 . . H H17 -0.174944 0.676288 0.206177 0.027 Uiso calc 1 . . C C18 -0.0004(2) 0.72670(18) 0.28226(6) 0.0201(3) Uani d 1 . . H H18 -0.099671 0.682046 0.318066 0.024 Uiso calc 1 . . C C19 0.0474(3) 0.7789(2) 0.08986(7) 0.0353(4) Uani d 1 . . H H19A -0.003498 0.658960 0.087676 0.053 Uiso calc 1 . . H H19B 0.179989 0.793648 0.060251 0.053 Uiso calc 1 . . H H19C -0.067539 0.879581 0.074736 0.053 Uiso calc 1 . . O O1W 0.72107(18) 0.87492(14) 0.46115(5) 0.0241(2) Uani d 1 . . H H1W 0.600(3) 0.874(3) 0.4328(10) 0.062(6) Uiso d 1 . . H H2W 0.850(3) 0.813(3) 0.4429(10) 0.060(6) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0202(6) 0.0197(6) 0.0178(6) -0.0037(5) -0.0013(4) -0.0026(4) N2 0.0149(5) 0.0234(6) 0.0157(5) -0.0021(4) -0.0007(4) -0.0038(4) C1 0.0192(7) 0.0225(7) 0.0187(6) -0.0006(5) -0.0003(5) -0.0045(5) C2 0.0162(6) 0.0244(7) 0.0184(6) -0.0033(5) 0.0006(5) -0.0034(5) C3 0.0156(6) 0.0276(7) 0.0199(7) -0.0012(6) -0.0008(5) -0.0037(5) C4 0.0175(7) 0.0277(7) 0.0208(7) -0.0037(6) -0.0009(5) -0.0026(5) C5 0.0198(7) 0.0187(7) 0.0166(6) -0.0047(5) 0.0001(5) -0.0020(5) C6 0.0188(7) 0.0298(8) 0.0197(7) -0.0016(6) 0.0009(5) -0.0059(5) C7 0.0191(7) 0.0358(8) 0.0214(7) -0.0026(6) -0.0041(5) -0.0043(6) C8 0.0269(8) 0.0303(8) 0.0160(6) -0.0056(6) -0.0009(5) -0.0059(5) C9 0.0250(7) 0.0362(9) 0.0210(7) 0.0008(6) 0.0024(6) -0.0092(6) C10 0.0197(7) 0.0334(8) 0.0224(7) -0.0002(6) -0.0020(5) -0.0064(6) O1 0.0288(6) 0.0545(7) 0.0199(5) -0.0010(5) -0.0044(4) -0.0138(5) C11 0.0319(9) 0.0664(12) 0.0227(8) -0.0079(8) -0.0061(6) -0.0135(7) O2 0.0261(5) 0.0270(5) 0.0194(5) -0.0023(4) -0.0018(4) -0.0044(4) O3 0.0324(6) 0.0365(6) 0.0310(6) -0.0122(5) -0.0115(5) -0.0059(4) C12 0.0207(7) 0.0171(7) 0.0243(7) 0.0025(5) -0.0051(5) -0.0061(5) C13 0.0187(6) 0.0185(7) 0.0198(6) 0.0008(5) -0.0025(5) -0.0045(5) C14 0.0176(7) 0.0236(7) 0.0283(7) -0.0037(6) -0.0015(5) -0.0059(6) C15 0.0241(7) 0.0307(8) 0.0218(7) -0.0031(6) 0.0029(5) -0.0032(6) C16 0.0266(7) 0.0261(7) 0.0195(7) 0.0009(6) -0.0033(5) -0.0055(5) C17 0.0216(7) 0.0234(7) 0.0244(7) -0.0034(6) -0.0048(5) -0.0061(5) C18 0.0194(7) 0.0195(7) 0.0210(7) -0.0020(5) -0.0006(5) -0.0027(5) C19 0.0397(9) 0.0450(10) 0.0223(7) -0.0043(8) -0.0038(7) -0.0080(7) O1W 0.0229(5) 0.0260(5) 0.0245(5) -0.0045(4) -0.0043(4) -0.0045(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' 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 N1 C4 . . 109.09(10) ? C1 N1 H1A . . 113.3(9) ? C4 N1 H1A . . 109.7(9) ? C1 N1 H1B . . 109.9(10) ? C4 N1 H1B . . 108.5(10) ? H1A N1 H1B . . 106.2(13) ? C5 N2 C3 . . 114.15(10) ? C5 N2 C2 . . 114.57(10) ? C3 N2 C2 . . 112.07(10) ? N1 C1 C2 . . 110.21(11) ? N1 C1 H1C . . 109.6 ? C2 C1 H1C . . 109.6 ? N1 C1 H1D . . 109.6 ? C2 C1 H1D . . 109.6 ? H1C C1 H1D . . 108.1 ? N2 C2 C1 . . 111.90(10) ? N2 C2 H2A . . 109.2 ? C1 C2 H2A . . 109.2 ? N2 C2 H2B . . 109.2 ? C1 C2 H2B . . 109.2 ? H2A C2 H2B . . 107.9 ? N2 C3 C4 . . 112.90(11) ? N2 C3 H3A . . 109.0 ? C4 C3 H3A . . 109.0 ? N2 C3 H3B . . 109.0 ? C4 C3 H3B . . 109.0 ? H3A C3 H3B . . 107.8 ? N1 C4 C3 . . 110.50(11) ? N1 C4 H4A . . 109.5 ? C3 C4 H4A . . 109.5 ? N1 C4 H4B . . 109.5 ? C3 C4 H4B . . 109.5 ? H4A C4 H4B . . 108.1 ? C6 C5 C10 . . 116.85(12) ? C6 C5 N2 . . 121.63(12) ? C10 C5 N2 . . 121.48(12) ? C5 C6 C7 . . 122.01(13) ? C5 C6 H6 . . 119.0 ? C7 C6 H6 . . 119.0 ? C8 C7 C6 . . 119.92(13) ? C8 C7 H7 . . 120.0 ? C6 C7 H7 . . 120.0 ? C7 C8 O1 . . 125.52(12) ? C7 C8 C9 . . 118.96(12) ? O1 C8 C9 . . 115.52(12) ? C10 C9 C8 . . 121.06(13) ? C10 C9 H9 . . 119.5 ? C8 C9 H9 . . 119.5 ? C9 C10 C5 . . 121.16(13) ? C9 C10 H10 . . 119.4 ? C5 C10 H10 . . 119.4 ? C8 O1 C11 . . 117.39(11) ? O1 C11 H11A . . 109.5 ? O1 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? O1 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? O3 C12 O2 . . 124.23(12) ? O3 C12 C13 . . 117.92(12) ? O2 C12 C13 . . 117.85(11) ? C18 C13 C14 . . 118.71(12) ? C18 C13 C12 . . 121.19(11) ? C14 C13 C12 . . 120.10(12) ? C15 C14 C13 . . 120.20(12) ? C15 C14 H14 . . 119.9 ? C13 C14 H14 . . 119.9 ? C16 C15 C14 . . 121.25(13) ? C16 C15 H15 . . 119.4 ? C14 C15 H15 . . 119.4 ? C15 C16 C17 . . 118.16(12) ? C15 C16 C19 . . 121.89(13) ? C17 C16 C19 . . 119.95(13) ? C18 C17 C16 . . 120.95(12) ? C18 C17 H17 . . 119.5 ? C16 C17 H17 . . 119.5 ? C17 C18 C13 . . 120.71(12) ? C17 C18 H18 . . 119.6 ? C13 C18 H18 . . 119.6 ? C16 C19 H19A . . 109.5 ? C16 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C16 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? H1W O1W H2W . . 109.5(16) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C1 . 1.4864(17) ? N1 C4 . 1.4879(17) ? N1 H1A . 1.028(17) ? N1 H1B . 0.939(16) ? N2 C5 . 1.4239(16) ? N2 C3 . 1.4669(16) ? N2 C2 . 1.4674(16) ? C1 C2 . 1.5111(17) ? C1 H1C . 0.9900 ? C1 H1D . 0.9900 ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 C4 . 1.5131(18) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 C6 . 1.3918(18) ? C5 C10 . 1.3974(18) ? C6 C7 . 1.3920(18) ? C6 H6 . 0.9500 ? C7 C8 . 1.3777(19) ? C7 H7 . 0.9500 ? C8 O1 . 1.3809(16) ? C8 C9 . 1.381(2) ? C9 C10 . 1.3809(19) ? C9 H9 . 0.9500 ? C10 H10 . 0.9500 ? O1 C11 . 1.4242(18) ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? O2 C12 . 1.2759(16) ? O3 C12 . 1.2461(16) ? C12 C13 . 1.5032(18) ? C13 C18 . 1.3917(18) ? C13 C14 . 1.3935(18) ? C14 C15 . 1.3897(19) ? C14 H14 . 0.9500 ? C15 C16 . 1.3894(19) ? C15 H15 . 0.9500 ? C16 C17 . 1.3937(19) ? C16 C19 . 1.5074(19) ? C17 C18 . 1.3840(18) ? C17 H17 . 0.9500 ? C18 H18 . 0.9500 ? C19 H19A . 0.9800 ? C19 H19B . 0.9800 ? C19 H19C . 0.9800 ? O1W H1W . 0.97(2) ? O1W H2W . 0.94(2) ? 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 O2 . 1.028(17) 1.714(17) 2.7391(15) 174.1(15) yes N1 H1B O1W 2_676 0.939(16) 1.873(17) 2.7977(16) 167.8(14) yes C1 H1C O1W . 0.99 2.46 3.2617(17) 138 yes C2 H2B O3 2_676 0.99 2.52 3.5088(17) 174 yes C4 H4A O2 2_566 0.99 2.55 3.5294(17) 169 yes C4 H4B O1W 1_455 0.99 2.54 3.3184(17) 135 yes O1W H1W O3 . 0.97(2) 1.67(2) 2.6418(14) 176.5(18) yes O1W H2W O2 1_655 0.94(2) 1.83(2) 2.7626(15) 170.5(17) 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 C4 N1 C1 C2 . . . . -59.83(13) ? C5 N2 C2 C1 . . . . 175.50(11) ? C3 N2 C2 C1 . . . . -52.38(14) ? N1 C1 C2 N2 . . . . 57.29(14) ? C5 N2 C3 C4 . . . . -176.52(11) ? C2 N2 C3 C4 . . . . 51.15(14) ? C1 N1 C4 C3 . . . . 58.20(14) ? N2 C3 C4 N1 . . . . -54.40(15) ? C3 N2 C5 C6 . . . . -162.71(12) ? C2 N2 C5 C6 . . . . -31.58(17) ? C3 N2 C5 C10 . . . . 19.66(17) ? C2 N2 C5 C10 . . . . 150.78(12) ? C10 C5 C6 C7 . . . . -1.0(2) ? N2 C5 C6 C7 . . . . -178.78(12) ? C5 C6 C7 C8 . . . . 0.5(2) ? C6 C7 C8 O1 . . . . -178.52(13) ? C6 C7 C8 C9 . . . . 1.1(2) ? C7 C8 C9 C10 . . . . -2.0(2) ? O1 C8 C9 C10 . . . . 177.58(13) ? C8 C9 C10 C5 . . . . 1.5(2) ? C6 C5 C10 C9 . . . . 0.1(2) ? N2 C5 C10 C9 . . . . 177.80(13) ? C7 C8 O1 C11 . . . . 2.0(2) ? C9 C8 O1 C11 . . . . -177.61(14) ? O3 C12 C13 C18 . . . . -172.58(12) ? O2 C12 C13 C18 . . . . 8.03(18) ? O3 C12 C13 C14 . . . . 8.23(19) ? O2 C12 C13 C14 . . . . -171.15(12) ? C18 C13 C14 C15 . . . . -1.47(19) ? C12 C13 C14 C15 . . . . 177.74(12) ? C13 C14 C15 C16 . . . . 0.8(2) ? C14 C15 C16 C17 . . . . 0.6(2) ? C14 C15 C16 C19 . . . . 179.81(14) ? C15 C16 C17 C18 . . . . -1.2(2) ? C19 C16 C17 C18 . . . . 179.54(13) ? C16 C17 C18 C13 . . . . 0.5(2) ? C14 C13 C18 C17 . . . . 0.85(19) ? C12 C13 C18 C17 . . . . -178.35(12) ?