#------------------------------------------------------------------------------ #$Date: 2022-08-27 05:38:19 +0300 (Sat, 27 Aug 2022) $ #$Revision: 277424 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244152.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_2244152 loop_ _publ_author_name 'Shankara Prasad, Holehundi J.' Devaraju Vinaya 'Yathirajan, Hemmige S.' 'Parkin, Sean R.' 'Glidewell, Christopher' _publ_section_title ; Syntheses and crystal structures of 4-(4-methoxyphenyl)piperazin-1-ium 4-methylbenzoate monohydrate and bis[4-(4-methoxyphenyl)piperazin-1-ium] benzene-1,2-dicarboxylate ; _journal_coeditor_code ZL5034 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022008337 _journal_volume 78 _journal_year 2022 _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 dual _audit_creation_method SHELXL-2014 _cell_angle_alpha 86.695(2) _cell_angle_beta 83.654(2) _cell_angle_gamma 82.182(3) _cell_formula_units_Z 4 _cell_length_a 7.4141(5) _cell_length_b 12.3595(11) _cell_length_c 19.9917(17) _cell_measurement_reflns_used 8258 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 27.535 _cell_measurement_theta_min 1.917 _cell_volume 1802.1(3) _computing_cell_refinement ; APEX3 (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; APEX3 (Bruker, 2016) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture dual source' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 54020 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.535 _diffrn_reflns_theta_min 1.917 _diffrn_source microsource _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_correction_T_min 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.277 _exptl_crystal_description needle _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.297 _refine_diff_density_min -0.181 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 479 _refine_ls_number_reflns 8288 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0456 _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^)+(0.0586P)^2^+0.3838P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.1317 _reflns_number_gt 5772 _reflns_number_total 8288 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl5034sup1.cif _cod_data_source_block I _cod_database_code 2244152 _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 0.993 _shelx_hkl_file ; -1 0 0 -0.2659 0.30140 4 -3 0 0 13.4339 0.95031 2 -3 0 0 10.6167 1.82913 4 -3 0 0 12.7862 0.76854 2 -4 0 0 333.079 12.0514 4 -4 0 0 311.213 13.6085 3 -5 0 0 195.988 9.51375 4 -5 0 0 190.749 11.1706 3 -7 0 0 57.1451 6.03502 4 -7 0 0 66.8260 7.78344 3 -8 0 0 11.7764 4.91325 3 -8 0 0 10.6179 3.58646 4 -9 0 0 7.29934 4.59313 3 -9 0 0 2.48541 3.51621 4 -9 0 0 7.26700 1.43766 5 -9 0 0 6.54903 1.66416 5 -9 1 0 -1.3863 2.13788 5 -9 1 0 -7.2190 3.18967 3 -8 1 0 7.39864 1.39703 5 -8 1 0 6.21937 1.60983 5 -8 1 0 5.62072 3.48871 3 -8 1 0 10.3381 3.53305 4 -7 1 0 5.46734 2.68151 4 -7 1 0 7.93004 3.27627 3 -6 1 0 8.32402 3.13517 3 -6 1 0 12.4699 3.48930 4 -5 1 0 3.45114 1.60593 4 -5 1 0 1.66168 0.62278 2 -5 1 0 0.84988 0.66262 2 -5 1 0 0.13515 1.62169 3 4 -1 0 34.7702 1.41774 2 4 -1 0 34.2530 1.44053 2 -4 1 0 30.7564 3.74362 3 -4 1 0 40.3341 3.71177 4 -4 1 0 37.7776 2.62280 2 -4 1 0 35.4090 2.32607 2 3 -1 0 0.65582 0.57826 2 3 -1 0 0.06317 0.43143 2 3 -1 0 0.34151 0.78814 4 -3 1 0 -0.0590 0.56714 2 -3 1 0 -0.1608 0.63093 2 -3 1 0 0.33637 0.82122 4 2 -1 0 331.696 9.29848 2 2 -1 0 317.824 9.50898 2 2 -1 0 336.665 9.92925 4 -2 1 0 332.647 9.76232 2 -2 1 0 343.302 10.0163 4 -2 1 0 319.536 9.53655 2 1 -1 0 26.3746 1.70738 4 1 -1 0 24.6651 1.90728 2 -1 1 0 25.0457 1.95804 2 -1 1 0 26.3180 1.74692 4 -1 1 0 24.0714 1.30728 5 -1 1 0 23.8195 1.90225 2 -1 1 0 23.4682 1.15359 5 -1 -1 0 9.09736 1.09895 2 -1 -1 0 9.60634 1.13583 2 1 1 0 9.87711 1.05676 2 -2 -1 0 246.923 6.87455 2 -2 -1 0 248.071 6.73968 2 2 1 0 260.026 6.65722 2 2 1 0 247.882 6.29315 2 -3 -1 0 109.733 3.42891 2 -3 -1 0 113.765 3.22310 2 -4 -1 0 4.75613 1.66118 4 -4 -1 0 7.75018 2.82246 3 -5 -1 0 -0.4381 2.02130 3 -5 -1 0 -1.9359 1.04572 4 -6 -1 0 60.7595 7.31957 3 -6 -1 0 65.4500 6.05305 4 -7 -1 0 6.50588 2.98531 4 -7 -1 0 11.3533 4.36501 3 -8 -1 0 2.79384 2.87022 4 -8 -1 0 5.67453 3.83170 3 -9 -1 0 3.01135 4.27724 3 -9 -1 0 1.93893 2.81494 4 -9 2 0 3.54850 3.05190 5 -9 2 0 2.90374 3.50818 4 -9 2 0 7.12926 3.62342 3 -8 2 0 17.3543 4.35529 3 -8 2 0 5.20522 3.75192 3 -8 2 0 16.9547 2.80865 5 -8 2 0 19.7764 4.47345 4 -8 2 0 11.6581 2.99210 5 -7 2 0 0.33575 1.31967 5 -7 2 0 1.14688 2.12609 4 -7 2 0 -1.9307 2.00989 3 -7 2 0 -0.3672 2.33551 3 -7 2 0 -2.0657 1.05863 5 -6 2 0 29.7450 2.41407 2 -6 2 0 24.7281 4.04840 3 -6 2 0 26.0238 2.35990 5 -6 2 0 31.9998 2.19277 5 -6 2 0 27.2886 5.22734 4 -6 2 0 32.7757 2.29295 2 5 -2 0 282.021 8.22652 2 5 -2 0 298.273 8.11325 2 -5 2 0 289.462 12.1065 3 -5 2 0 283.516 7.82238 5 -5 2 0 291.148 8.26737 5 -5 2 0 280.680 9.64462 2 -5 2 0 298.515 12.2597 4 -5 2 0 297.177 10.3838 2 4 -2 0 625.535 18.7777 4 4 -2 0 614.954 16.4422 2 4 -2 0 611.383 17.0429 2 -4 2 0 567.500 18.0124 3 -4 2 0 620.562 17.5279 2 -4 2 0 604.417 14.4512 5 -4 2 0 621.186 18.8775 4 -4 2 0 608.125 18.0505 2 -4 2 0 600.116 14.8207 5 3 -2 0 4571.71 100.708 2 -3 2 0 4613.95 101.337 2 -3 2 0 4597.16 100.887 2 -3 2 0 4221.02 99.2037 3 -3 2 0 4478.27 97.7104 5 2 -2 0 639.370 17.2410 4 2 -2 0 662.180 18.4144 2 -2 2 0 634.620 16.4004 5 -2 2 0 627.996 15.7214 5 -2 2 0 641.913 18.3850 2 -2 2 0 651.831 18.3148 2 -2 2 0 613.482 15.0084 3 -2 2 0 655.119 17.6202 4 0 -2 0 310.138 10.4391 2 0 -2 0 319.829 10.5490 2 0 -2 0 312.119 10.0033 4 0 -2 0 295.412 9.28362 3 0 -2 0 311.111 9.74266 5 0 -2 0 314.556 9.27406 5 0 2 0 324.377 9.88613 5 0 2 0 323.171 9.27367 5 0 2 0 330.935 10.5974 2 0 2 0 317.907 10.5409 2 0 2 0 321.852 10.1292 4 -2 -2 0 101.626 3.05009 5 -2 -2 0 105.008 4.94175 2 -2 -2 0 105.939 2.91093 5 2 2 0 94.3454 4.48191 2 -3 -2 0 3194.01 70.6390 2 -3 -2 0 3267.97 71.0729 2 -3 -2 0 2888.22 76.7922 3 3 2 0 3215.79 69.7060 2 3 2 0 3300.39 70.3744 2 -4 -2 0 526.082 12.8758 2 -4 -2 0 469.914 19.9274 3 -4 -2 0 519.081 13.3752 2 -5 -2 0 51.8759 5.16913 4 -5 -2 0 43.4711 6.04267 3 -6 -2 0 -0.7457 1.84757 4 -6 -2 0 0.73043 2.26471 3 -7 -2 0 7.71363 3.92926 3 -7 -2 0 2.41831 2.25909 4 -8 -2 0 60.7809 7.04673 4 -8 -2 0 58.5515 8.92087 3 -9 -2 0 -0.2919 4.65942 3 -9 -2 0 -3.0469 2.84487 4 -9 3 0 12.9276 4.27846 4 -9 3 0 10.2911 4.39540 5 -9 3 0 13.6056 2.98063 3 -8 3 0 10.8754 2.78881 3 -8 3 0 1.82837 2.90306 5 -8 3 0 5.84865 2.76403 5 -8 3 0 2.96771 3.14926 4 -7 3 0 7.38944 2.48383 3 -7 3 0 12.5259 2.55574 5 -7 3 0 12.2634 2.89334 3 -7 3 0 1.79589 2.47272 5 -7 3 0 7.91709 3.13604 4 -7 3 0 10.4671 1.53905 2 6 -3 0 97.9137 3.94746 2 -6 3 0 93.9713 5.26545 5 -6 3 0 108.133 8.91314 4 -6 3 0 89.2432 5.75285 3 -6 3 0 92.9030 6.12487 3 -6 3 0 98.8743 6.09737 2 -6 3 0 98.0173 6.25209 5 -6 3 0 105.779 5.80573 2 5 -3 0 85.4740 6.29073 4 5 -3 0 94.4575 5.52224 2 5 -3 0 88.2160 4.97552 2 -5 3 0 106.783 6.99612 4 -5 3 0 82.9840 4.89742 3 -5 3 0 86.5297 5.40364 5 -5 3 0 81.9200 5.13991 3 -5 3 0 89.6734 4.75058 5 -5 3 0 96.8169 6.00473 2 -5 3 0 89.1998 6.21055 2 4 -3 0 273.787 10.9901 2 4 -3 0 277.992 10.9190 4 4 -3 0 262.453 10.3839 2 -4 3 0 246.798 10.8959 4 -4 3 0 252.923 9.68391 5 -4 3 0 273.695 11.2274 2 -4 3 0 256.896 8.36389 3 -4 3 0 254.525 8.77285 5 -4 3 0 272.010 11.4868 2 -4 3 0 250.077 8.66692 3 3 -3 0 487.020 16.5529 2 3 -3 0 506.958 15.5318 4 -3 3 0 500.898 11.8215 3 -3 3 0 489.488 16.6334 2 -3 3 0 493.482 16.9375 2 -3 3 0 479.168 13.8900 5 -3 3 0 497.438 16.0524 4 -3 3 0 446.911 12.0402 3 -3 3 0 492.545 15.0650 5 2 -3 0 70.3955 5.17345 2 2 -3 0 71.6978 5.32650 2 2 -3 0 73.1555 3.23057 5 2 -3 0 71.2506 4.41744 4 2 -3 0 74.6007 3.03152 5 -2 3 0 71.7754 4.59850 5 -2 3 0 76.2803 4.92072 4 -2 3 0 70.4544 5.28316 2 -2 3 0 67.7814 5.21414 2 -2 3 0 71.5982 4.07668 5 1 -3 0 185.786 7.39251 5 1 -3 0 175.037 7.46928 4 1 -3 0 181.173 5.45539 3 1 -3 0 182.417 8.63048 2 1 -3 0 179.908 6.71372 5 1 -3 0 179.765 8.54856 2 -1 3 0 166.906 7.64638 5 -1 3 0 175.542 7.77527 4 -1 3 0 187.795 8.74973 2 -1 3 0 195.560 8.94004 2 -1 3 0 168.389 6.92196 5 0 -3 0 87.5182 5.03251 5 0 -3 0 80.8772 4.43251 5 0 -3 0 70.6363 5.12321 2 0 -3 0 81.2527 5.40210 2 0 -3 0 84.0737 4.56356 3 0 -3 0 78.7671 4.97869 4 0 3 0 75.8705 4.24422 5 0 3 0 73.9226 5.16709 2 0 3 0 82.1673 4.93354 5 0 3 0 79.5540 5.05340 4 0 3 0 89.5237 5.68288 2 -1 -3 0 241.280 9.97322 2 -1 -3 0 265.358 10.4195 4 -1 -3 0 244.432 10.0475 2 -1 -3 0 250.101 9.14433 5 -1 -3 0 245.319 8.49950 5 -1 -3 0 224.542 10.0228 3 1 3 0 252.280 8.09960 5 1 3 0 269.521 10.2816 2 1 3 0 244.690 8.71231 5 1 3 0 248.219 10.0750 2 -2 -3 0 1651.87 39.3756 5 -2 -3 0 1574.71 43.9775 3 -2 -3 0 1664.82 38.4350 5 -2 -3 0 1625.90 41.3215 2 -2 -3 0 1702.20 41.6305 2 2 3 0 1726.70 41.6281 2 2 3 0 1726.24 36.4558 5 2 3 0 1675.49 41.0987 2 2 3 0 1702.63 36.3171 5 -3 -3 0 93.2997 5.42901 2 -3 -3 0 88.4418 5.16879 2 -3 -3 0 82.4067 7.06905 3 -3 -3 0 86.6826 3.34533 5 -3 -3 0 86.9899 3.74377 5 3 3 0 87.3152 4.82872 2 3 3 0 91.4780 5.13288 2 -4 -3 0 556.769 16.3941 2 -4 -3 0 519.712 21.9805 3 -4 -3 0 551.018 12.2349 5 -4 -3 0 550.439 15.8443 2 -4 -3 0 546.272 12.3220 5 4 3 0 562.070 15.3971 2 4 3 0 550.350 14.6899 2 -5 -3 0 3.30812 3.11438 3 -6 -3 0 22.2043 4.87877 4 -6 -3 0 18.9155 5.55432 3 -7 -3 0 -1.0502 2.21409 4 -7 -3 0 -3.3547 3.04742 3 -8 -3 0 2.01810 2.62069 4 -8 -3 0 1.78870 4.40418 3 -9 -3 0 7.02642 1.44914 5 -9 -3 0 17.5978 6.31524 3 -9 -3 0 11.6229 1.98216 5 -9 -3 0 2.83421 3.55675 4 -8 4 0 4.47541 3.30697 4 -8 4 0 5.04682 3.32588 5 -8 4 0 7.79521 3.08742 5 -7 4 0 7.38951 2.62055 2 -7 4 0 8.29780 1.47621 3 -7 4 0 9.10853 3.17433 5 -7 4 0 1.40510 2.51254 5 -7 4 0 8.35299 1.52011 3 -7 4 0 5.75935 3.10290 4 -7 4 0 5.74729 1.95323 2 6 -4 0 2.55668 2.92407 2 6 -4 0 4.72073 1.86445 2 -6 4 0 2.84095 2.07916 2 -6 4 0 4.41984 2.55284 4 -6 4 0 6.94900 2.61478 5 -6 4 0 4.90622 1.08072 3 -6 4 0 0.45447 1.91598 2 -6 4 0 2.75883 1.05181 3 5 -4 0 74.8979 5.56205 2 5 -4 0 68.8893 5.80324 4 5 -4 0 71.0996 6.09764 2 -5 4 0 69.2969 2.79340 3 -5 4 0 81.1677 5.46553 5 -5 4 0 80.3318 6.44779 2 -5 4 0 70.2309 6.36002 2 -5 4 0 78.8209 6.64545 4 -5 4 0 75.2306 2.77386 3 -5 4 0 76.2111 6.20116 5 4 -4 0 3.27591 2.21169 4 4 -4 0 7.25563 2.40522 2 -4 4 0 4.16869 2.37251 2 -4 4 0 3.36890 2.10810 5 -4 4 0 4.64620 1.89759 5 -4 4 0 3.19934 2.08928 2 -4 4 0 7.86158 2.62746 4 3 -4 0 1973.63 50.3180 2 3 -4 0 1792.38 49.9427 2 3 -4 0 1932.81 47.9279 4 -3 4 0 1867.95 50.6417 2 -3 4 0 2015.12 49.0999 5 -3 4 0 1958.13 50.7406 2 -3 4 0 1996.53 47.1460 5 -3 4 0 1984.92 49.3824 4 2 -4 0 2.74728 1.34514 5 2 -4 0 4.19345 1.87869 2 2 -4 0 11.5408 1.71143 5 2 -4 0 3.00122 1.55576 4 2 -4 0 7.97337 2.43426 2 -2 4 0 6.26711 2.02823 5 -2 4 0 5.57267 1.96617 4 -2 4 0 4.92694 2.14592 2 -2 4 0 7.18588 1.83596 5 -2 4 0 6.53212 2.40566 2 1 -4 0 2808.42 67.3635 2 1 -4 0 2720.76 67.1323 2 1 -4 0 2727.94 61.1966 3 1 -4 0 2740.48 63.0797 5 1 -4 0 2742.42 64.8733 4 1 -4 0 2698.82 64.3199 5 -1 4 0 2687.97 65.5170 4 -1 4 0 2738.44 67.1971 2 -1 4 0 2710.15 67.1506 2 -1 4 0 2691.12 63.7066 5 -1 4 0 2746.66 65.4147 5 0 -4 0 62.6189 4.53139 3 0 -4 0 65.2302 4.95791 5 0 -4 0 62.9998 4.98460 4 0 -4 0 62.1263 4.35238 5 0 -4 0 58.9389 5.22841 2 0 -4 0 77.6404 6.00636 2 0 4 0 63.9614 4.93049 5 0 4 0 72.1620 5.43558 4 0 4 0 64.8231 5.47164 2 0 4 0 63.1260 4.34426 5 0 4 0 71.3988 5.81361 2 -1 -4 0 316.436 12.0096 5 -1 -4 0 317.458 11.2623 5 -1 -4 0 308.853 12.9223 3 -1 -4 0 332.840 13.4201 2 -1 -4 0 319.451 13.0339 4 -1 -4 0 331.190 13.3715 2 1 4 0 323.598 13.2581 2 1 4 0 316.566 11.6543 5 1 4 0 309.194 12.9396 2 -2 -4 0 90.6301 6.29123 2 -2 -4 0 88.2718 5.40352 5 -2 -4 0 73.1711 6.49952 3 -2 -4 0 80.5607 4.72724 5 -2 -4 0 83.6699 6.02182 2 -2 -4 0 92.4598 6.78456 4 2 4 0 81.8156 4.21153 5 2 4 0 83.3975 3.77141 5 2 4 0 70.8969 5.57496 2 2 4 0 88.0496 6.25210 2 -3 -4 0 366.021 17.4198 3 -3 -4 0 414.987 15.0898 2 -3 -4 0 396.288 13.0817 5 -3 -4 0 415.583 14.9351 2 -3 -4 0 416.076 12.1958 5 3 4 0 396.305 14.2314 2 -4 -4 0 2.81284 2.45963 3 -4 -4 0 -0.0909 0.72168 5 -4 -4 0 -0.8420 1.10058 2 -4 -4 0 0.43694 1.22922 2 -4 -4 0 1.83018 1.12823 5 4 4 0 1.55337 1.18282 2 4 4 0 0.64474 1.15222 2 -5 -4 0 103.878 6.20334 2 -5 -4 0 110.902 5.04605 5 -5 -4 0 103.367 4.29883 5 -5 -4 0 101.108 5.73098 2 -5 -4 0 101.649 9.87656 3 5 4 0 105.677 5.29136 2 5 4 0 101.642 4.80370 2 -6 -4 0 36.0337 2.80532 2 -6 -4 0 37.4606 2.84007 5 -6 -4 0 35.6133 3.05003 2 -6 -4 0 39.5060 6.98559 3 -6 -4 0 33.8093 2.29760 5 -7 -4 0 12.0687 3.71460 4 -7 -4 0 0.85584 3.37510 3 -7 -4 0 7.95098 1.82104 5 -7 -4 0 6.21825 1.33141 5 -8 -4 0 40.7664 3.80178 5 -8 -4 0 41.3280 2.93808 5 -8 -4 0 43.7603 9.47870 3 -8 -4 0 42.8786 6.57618 4 -9 -4 0 44.8664 7.37862 4 -9 -4 0 43.2815 5.13442 5 -9 -4 0 44.5072 9.63032 3 -9 -4 0 52.6098 3.72838 5 -8 5 0 24.7328 3.52383 2 -8 5 0 20.4255 2.88833 2 -8 5 0 12.3064 4.97071 5 -8 5 0 23.8702 5.33728 5 -8 5 0 24.2045 5.64982 4 7 -5 0 1.95543 1.85631 2 -7 5 0 -1.8325 2.65901 4 -7 5 0 1.58288 2.29912 2 -7 5 0 -0.8470 2.09518 2 -7 5 0 -4.0561 2.32934 5 -7 5 0 5.14743 2.80264 5 6 -5 0 5.86811 2.95152 4 6 -5 0 0.99953 2.19519 2 6 -5 0 1.28068 1.81150 2 -6 5 0 5.20950 2.57039 5 -6 5 0 5.47586 2.95651 4 -6 5 0 -1.0216 2.09402 2 -6 5 0 -3.6253 1.75054 2 -6 5 0 4.00277 2.73587 5 5 -5 0 5.49939 2.27781 2 5 -5 0 2.97771 1.88403 4 5 -5 0 2.99166 2.32708 2 -5 5 0 2.84889 2.41613 2 -5 5 0 1.44063 1.94067 2 -5 5 0 5.14947 2.75417 5 -5 5 0 1.16140 1.92392 5 -5 5 0 1.95710 2.16510 4 4 -5 0 0.57021 1.74652 2 4 -5 0 2.64327 2.01544 2 4 -5 0 0.89505 1.64591 4 -4 5 0 -0.5743 1.56551 2 -4 5 0 0.26227 1.44043 4 -4 5 0 2.23427 1.96230 5 -4 5 0 4.10175 2.15522 2 -4 5 0 2.14948 1.71404 5 3 -5 0 16.4760 1.67238 5 3 -5 0 17.0246 1.61780 5 3 -5 0 13.3685 2.88195 4 3 -5 0 21.2283 3.76510 2 3 -5 0 20.0162 4.25433 2 -3 5 0 14.7770 3.51396 4 -3 5 0 18.5770 3.51452 5 -3 5 0 20.5279 4.32709 2 -3 5 0 11.4003 3.08870 2 -3 5 0 20.5550 4.09321 5 2 -5 0 4.94406 1.88900 5 2 -5 0 5.30925 0.77433 3 2 -5 0 2.26917 1.83541 2 2 -5 0 3.38900 1.95092 2 2 -5 0 5.27938 2.44406 4 2 -5 0 5.19041 1.61549 5 -2 5 0 8.87793 2.77180 2 -2 5 0 0.01693 1.56866 2 -2 5 0 5.54763 1.88744 5 -2 5 0 8.13763 2.80475 5 -2 5 0 3.79996 1.89683 4 1 -5 0 -0.4715 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20.0848 4 -3 -5 0 511.806 18.9641 2 -3 -5 0 497.122 18.5819 2 -3 -5 0 519.887 21.8611 3 -3 -5 0 475.105 16.8391 5 3 5 0 520.169 18.3863 2 3 5 0 511.668 18.7124 2 3 5 0 501.862 11.5362 5 -4 -5 0 105.960 5.69025 5 -4 -5 0 90.6193 6.84140 2 -4 -5 0 96.2035 9.34258 3 -4 -5 0 99.5674 6.32683 5 -4 -5 0 93.2245 7.05393 2 4 5 0 94.2168 6.45480 2 -5 -5 0 270.399 11.4932 2 -5 -5 0 241.933 9.22738 5 -5 -5 0 238.367 16.1692 3 -5 -5 0 248.181 10.4431 5 -5 -5 0 240.091 11.4655 2 5 5 0 238.122 9.96403 2 5 5 0 260.337 10.8913 2 -6 -5 0 18.0105 2.92372 5 -6 -5 0 16.2164 2.51426 5 -6 -5 0 26.1739 6.36797 3 -6 -5 0 15.8013 3.02694 2 -6 -5 0 20.7363 3.20285 2 6 5 0 17.6890 2.36236 2 6 5 0 15.1981 2.09821 2 -7 -5 0 2.78817 3.55815 3 -7 -5 0 2.21380 1.53636 5 -7 -5 0 0.90593 1.99264 5 -7 -5 0 1.29054 1.19428 2 -8 -5 0 4.64551 2.81511 5 -8 -5 0 9.36121 2.32296 5 -8 -5 0 1.57434 3.00909 4 -8 -5 0 3.33539 5.07022 3 -9 -5 0 36.6891 9.41392 3 -9 -5 0 50.3520 4.82618 5 -9 -5 0 67.9951 8.50517 4 -8 6 0 1.95552 2.32482 2 -8 6 0 3.81355 4.00925 4 -8 6 0 9.11265 4.07570 5 7 -6 0 25.9198 5.10163 2 -7 6 0 20.4579 4.44767 2 -7 6 0 24.5011 4.70201 2 -7 6 0 22.6273 5.82054 5 -7 6 0 26.4629 5.76145 4 6 -6 0 6.26986 3.14201 2 6 -6 0 15.2631 4.00947 4 -6 6 0 15.2335 4.85368 4 -6 6 0 21.7651 4.63330 5 -6 6 0 14.1682 4.78692 2 -6 6 0 13.6315 4.40092 5 -6 6 0 6.22514 3.73740 2 5 -6 0 -2.4646 2.29401 4 -5 6 0 -0.2857 2.86573 2 -5 6 0 6.47260 3.14781 4 -5 6 0 4.37136 3.05220 2 -5 6 0 5.97611 3.04336 5 -5 6 0 8.80476 3.03746 5 4 -6 0 -0.1088 1.96074 4 4 -6 0 5.66548 2.73854 2 4 -6 0 1.40744 2.14352 2 -4 6 0 0.47793 2.23802 4 -4 6 0 3.43203 2.44557 2 -4 6 0 4.63234 2.77375 5 -4 6 0 10.3434 3.42561 2 -4 6 0 4.73130 2.33610 5 3 -6 0 184.641 7.15775 5 3 -6 0 180.913 11.6969 2 3 -6 0 170.384 7.49871 5 3 -6 0 183.306 11.7272 2 3 -6 0 179.317 9.77205 4 -3 6 0 191.113 10.0661 5 -3 6 0 163.947 11.3741 2 -3 6 0 168.748 11.4431 2 -3 6 0 201.929 11.5315 5 2 -6 0 177.740 5.87801 3 2 -6 0 189.077 8.53316 5 2 -6 0 168.510 11.2888 2 2 -6 0 176.119 9.14200 5 2 -6 0 166.983 11.2727 2 2 -6 0 167.725 9.62075 4 -2 6 0 191.597 9.81560 5 -2 6 0 190.671 12.0264 2 -2 6 0 180.343 10.7753 4 -2 6 0 162.906 11.1563 2 -2 6 0 175.627 10.5751 5 1 -6 0 15.0206 2.25382 3 1 -6 0 18.1833 3.68035 5 1 -6 0 19.3614 4.66146 2 1 -6 0 17.3503 3.63590 4 1 -6 0 19.1203 4.30990 2 1 -6 0 16.6271 3.36355 5 -1 6 0 13.1890 3.95980 2 -1 6 0 17.6365 3.98841 5 -1 6 0 10.3546 3.44332 2 -1 6 0 14.5901 3.78514 4 -1 6 0 16.3507 3.34274 5 0 -6 0 171.440 10.1584 4 0 -6 0 168.396 9.00472 5 0 -6 0 161.596 9.66143 5 0 -6 0 166.854 10.9841 2 0 -6 0 167.347 9.10128 3 0 -6 0 170.912 11.0071 2 0 6 0 170.081 11.0975 2 0 6 0 137.245 11.7429 2 0 6 0 166.581 10.3827 4 0 6 0 151.628 8.51775 5 0 6 0 180.951 10.3804 5 -1 -6 0 564.325 21.4204 3 -1 -6 0 571.306 20.7874 5 -1 -6 0 583.541 22.7944 2 -1 -6 0 601.440 22.2298 4 -1 -6 0 580.230 22.6858 2 -1 -6 0 641.631 22.0192 5 1 6 0 571.939 24.6806 4 1 6 0 576.061 18.7967 5 1 6 0 621.784 20.9802 5 1 6 0 602.881 22.6922 2 1 6 0 586.238 22.7733 2 -2 -6 0 184.233 9.53850 5 -2 -6 0 186.546 10.3051 5 -2 -6 0 184.077 11.3326 4 -2 -6 0 187.183 11.8973 3 -2 -6 0 177.930 11.1059 2 -2 -6 0 180.937 11.3420 2 2 6 0 200.080 9.34328 5 2 6 0 167.607 10.7524 2 2 6 0 181.781 11.0045 2 -3 -6 0 49.6884 13.8664 1 3 6 0 37.3447 12.8772 1 -4 -6 0 66.7250 6.73512 2 -4 -6 0 73.7722 6.69643 2 -4 -6 0 82.9027 8.85214 3 -4 -6 0 78.2834 5.71901 5 -4 -6 0 70.4296 7.74313 4 -4 -6 0 64.5227 6.06657 5 4 6 0 66.4479 6.41849 2 4 6 0 68.1143 6.17399 2 -5 -6 0 314.358 13.7403 5 -5 -6 0 316.653 19.5753 3 -5 -6 0 318.978 17.8162 4 -5 -6 0 356.228 14.5423 5 -5 -6 0 346.097 15.4678 2 5 6 0 323.538 13.5974 2 5 6 0 320.263 14.1499 2 -6 -6 0 2.17774 3.59997 4 -6 -6 0 -4.6757 1.96809 5 -6 -6 0 2.23731 1.95120 2 -6 -6 0 2.25828 1.87535 2 -6 -6 0 2.68443 3.29855 3 6 6 0 0.81128 1.64547 2 6 6 0 -0.3066 1.71789 2 -7 -6 0 99.0121 6.38598 2 -7 -6 0 97.1431 7.57802 5 -7 -6 0 96.9816 11.9401 3 -7 -6 0 102.391 6.14546 2 -7 -6 0 85.5143 6.21892 5 -8 -6 0 4.34401 4.99770 3 -8 -6 0 4.92932 2.48532 5 -8 -6 0 11.4870 3.54215 5 -9 -6 0 -9.1884 5.18464 3 -9 -6 0 -0.3270 4.06491 4 7 -7 0 15.4109 4.45327 2 -7 7 0 20.1266 4.76829 2 -7 7 0 11.8761 5.18357 4 -7 7 0 4.94268 4.79980 5 -7 7 0 13.9394 4.65920 2 6 -7 0 44.5086 6.25988 4 6 -7 0 53.0867 6.38025 2 -6 7 0 50.6374 6.61174 5 -6 7 0 54.3245 7.13286 2 -6 7 0 57.0262 7.77849 5 -6 7 0 39.8561 6.22666 4 -6 7 0 39.5548 7.03688 2 5 -7 0 1.12454 2.57214 4 5 -7 0 -1.7958 2.08511 2 -5 7 0 -0.7048 2.84438 2 -5 7 0 1.08243 2.41971 4 -5 7 0 -3.8408 2.30579 5 -5 7 0 0.64587 2.80984 5 -5 7 0 -3.0046 2.18706 2 4 -7 0 71.6799 7.75818 2 4 -7 0 84.1722 10.0388 2 4 -7 0 93.4315 7.49544 4 -4 7 0 80.6441 7.16219 5 -4 7 0 92.0013 9.54235 2 -4 7 0 84.9941 8.20669 4 -4 7 0 75.2288 8.11418 5 -4 7 0 79.5685 8.28037 2 3 -7 0 73.3479 7.65933 5 3 -7 0 74.9098 8.50758 2 3 -7 0 71.3739 7.95897 2 3 -7 0 79.3632 6.82203 4 3 -7 0 80.2748 5.12013 5 -3 7 0 89.1474 8.24543 4 -3 7 0 75.3346 6.64574 5 -3 7 0 72.5051 7.72497 5 -3 7 0 88.9590 8.86391 2 -3 7 0 91.3638 9.00975 2 2 -7 0 18.8706 4.82231 2 2 -7 0 22.6478 3.42790 5 2 -7 0 28.7232 4.46460 4 2 -7 0 12.3664 4.21454 2 2 -7 0 13.7832 3.60522 5 2 -7 0 20.1011 2.05766 3 -2 7 0 21.1516 5.30745 2 -2 7 0 24.4186 3.87902 5 -2 7 0 19.4926 4.83301 2 -2 7 0 24.2394 5.08242 4 -2 7 0 21.8976 5.16679 5 1 -7 0 19.7587 4.96660 2 1 -7 0 24.6564 4.88685 5 1 -7 0 16.6988 3.66003 5 1 -7 0 17.9251 4.39210 4 1 -7 0 22.2604 3.00478 3 1 -7 0 23.1206 5.37249 2 -1 7 0 24.5208 5.06817 4 -1 7 0 25.7226 5.66516 2 -1 7 0 17.7792 3.82164 5 -1 7 0 31.2750 5.10539 5 -1 7 0 17.0302 4.65307 2 0 -7 0 0.53842 1.89499 5 0 -7 0 1.00039 1.57128 3 0 -7 0 1.21474 1.63053 4 0 -7 0 -1.2901 1.76494 2 0 -7 0 -2.1892 1.40229 2 0 -7 0 1.68532 1.77674 5 0 7 0 0.33375 1.30021 5 0 7 0 1.17479 2.13196 2 0 7 0 0.57337 1.83405 4 0 7 0 -1.5810 1.65057 5 -1 -7 0 46.9772 6.18997 2 -1 -7 0 31.6141 5.29552 2 -1 -7 0 35.9149 5.04259 3 -1 -7 0 32.2493 4.86659 4 -1 -7 0 36.0937 4.91049 5 -1 -7 0 40.5209 4.72251 5 1 7 0 40.4571 5.74828 2 1 7 0 36.9997 4.33078 5 1 7 0 30.4913 5.10684 4 1 7 0 32.6504 5.39948 2 1 7 0 38.7654 5.01340 5 -2 -7 0 35.5073 5.56934 2 -2 -7 0 29.9296 4.55552 4 -2 -7 0 33.3765 4.90110 5 -2 -7 0 25.6820 4.56223 2 -2 -7 0 33.5361 4.43103 5 -2 -7 0 20.4768 5.01297 3 2 7 0 31.1048 4.15399 5 2 7 0 37.0621 3.81246 5 2 7 0 24.9855 5.19614 2 2 7 0 28.9413 4.93046 2 -3 -7 0 29.6398 4.93512 2 -3 -7 0 33.7097 6.06546 3 -3 -7 0 28.1168 3.98537 5 -3 -7 0 22.1259 4.69922 5 -3 -7 0 23.1321 5.26509 4 -3 -7 0 17.6155 4.76562 2 3 7 0 20.4673 3.06066 5 3 7 0 22.5375 4.86237 2 3 7 0 24.6552 5.08041 2 3 7 0 22.4081 2.51191 5 -4 -7 0 43.1665 7.34187 3 -4 -7 0 56.1855 5.49914 5 -4 -7 0 41.6768 5.95251 2 -4 -7 0 55.0744 6.18276 5 -4 -7 0 64.0161 7.81310 4 -4 -7 0 45.7692 6.19041 2 4 7 0 47.8062 6.88779 2 4 7 0 48.7145 6.24635 2 -5 -7 0 241.363 13.1104 2 -5 -7 0 207.538 15.8073 3 -5 -7 0 217.451 12.0338 5 -5 -7 0 216.161 10.8874 5 -5 -7 0 182.561 13.9972 4 -5 -7 0 226.344 13.2049 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36.7183 6.40674 4 -4 8 0 28.0546 6.37090 2 -4 8 0 16.3026 4.59028 5 3 -8 0 43.8232 4.52152 5 3 -8 0 55.6925 7.65502 2 3 -8 0 45.8757 5.71961 4 3 -8 0 37.6610 7.60533 2 3 -8 0 41.8177 4.97512 5 -3 8 0 52.1282 7.51765 2 -3 8 0 53.1789 6.97689 5 -3 8 0 49.2493 7.49404 2 -3 8 0 51.8296 6.93048 4 2 -8 0 7.43872 3.67865 2 2 -8 0 8.93071 2.63847 5 2 -8 0 6.77910 3.74742 2 2 -8 0 7.10579 3.10520 4 2 -8 0 2.72324 2.74973 5 2 -8 0 8.12446 1.79119 3 -2 8 0 9.48147 3.80196 4 -2 8 0 2.88926 2.84394 2 -2 8 0 4.82303 3.19021 5 -2 8 0 4.26012 2.53387 5 -2 8 0 14.2281 4.92303 2 1 -8 0 -0.1805 2.60233 5 1 -8 0 0.27863 2.09630 4 1 -8 0 0.72681 2.40536 2 1 -8 0 -1.8031 2.44528 2 1 -8 0 0.15305 1.73451 5 1 -8 0 2.93159 1.84795 3 -1 8 0 -1.0946 1.91349 4 -1 8 0 1.20394 2.82724 2 -1 8 0 3.21349 2.42554 5 -1 8 0 0.42662 2.68214 2 -1 8 0 -2.5179 1.43954 5 0 -8 0 33.6796 4.85685 3 0 -8 0 54.5210 7.34652 2 0 -8 0 31.5470 5.25832 4 0 -8 0 35.0615 5.40353 5 0 -8 0 48.7895 6.81697 2 0 -8 0 40.1364 5.02927 5 0 8 0 33.7416 4.82773 5 0 8 0 42.6657 6.17388 2 0 8 0 41.0199 6.30723 4 0 8 0 46.8152 6.15045 5 0 8 0 42.3454 6.58659 2 -1 -8 0 46.9455 6.02654 3 -1 -8 0 52.3689 7.06093 2 -1 -8 0 47.0868 5.50229 5 -1 -8 0 48.3440 6.10000 5 -1 -8 0 37.5896 7.44887 2 -1 -8 0 47.8328 6.36541 4 1 8 0 51.3880 6.64383 2 1 8 0 33.8705 4.41535 5 1 8 0 38.8084 5.40491 5 -2 -8 0 153.564 11.7800 3 -2 -8 0 175.610 12.7908 2 -2 -8 0 187.820 10.8979 5 -2 -8 0 152.359 11.8309 2 -2 -8 0 182.980 12.5613 4 -2 -8 0 142.522 10.3337 5 2 8 0 157.208 12.1224 2 2 8 0 166.787 12.1347 2 2 8 0 156.895 8.62266 5 2 8 0 157.800 9.94049 5 -3 -8 0 27.6152 6.04463 2 -3 -8 0 25.3414 4.92645 5 -3 -8 0 26.7694 6.53010 3 -3 -8 0 35.6803 7.42593 4 -3 -8 0 21.8197 5.43567 2 -3 -8 0 26.2879 5.38310 5 3 8 0 21.1332 5.39768 2 3 8 0 24.0773 3.18431 5 3 8 0 28.0553 4.01321 5 -4 -8 0 33.1437 7.57457 3 -4 -8 0 34.8941 5.74688 2 -4 -8 0 37.0983 5.76301 5 -4 -8 0 26.1685 5.71846 2 -4 -8 0 22.8120 6.22125 4 -4 -8 0 34.3732 4.88178 5 4 8 0 34.7022 2.22323 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64.0767 8.39071 5 -1 0 24 67.1544 10.9263 3 -1 0 24 103.789 11.7435 4 -1 0 24 58.2768 10.3948 2 0 0 -24 75.6944 11.9369 2 0 0 -24 89.2081 9.63865 5 0 0 24 115.288 13.1558 2 0 0 24 106.057 12.8499 3 0 0 24 89.4449 10.9586 4 0 0 24 101.337 11.8425 5 -1 0 -24 245.713 15.4815 5 -1 0 -24 219.918 18.3570 2 1 0 24 203.551 18.0795 2 1 0 24 236.374 17.0835 5 1 0 24 257.479 20.6139 3 1 0 24 245.099 16.5615 4 -2 0 -24 18.0768 5.61178 5 -2 0 -24 17.8951 6.88394 2 2 0 24 19.9011 6.98622 3 2 0 24 20.2934 6.20564 5 2 0 24 11.7276 6.16939 2 2 0 24 7.42469 4.58739 4 -3 0 -24 286.808 26.0679 5 -3 0 -24 279.261 21.2901 2 3 0 24 268.760 16.3205 4 3 0 24 295.228 21.7318 2 -4 0 -24 65.9530 9.11222 5 -4 0 -24 63.8444 11.0659 2 4 0 24 57.5298 8.18616 4 4 0 24 83.4779 12.2428 2 4 0 24 54.9763 10.5106 5 2 -1 -24 7.36417 5.59301 2 -2 1 24 -2.4374 4.33393 3 -2 1 24 11.0146 5.55246 5 -2 1 24 2.08029 4.86501 2 1 -1 -24 2.75739 5.32823 2 1 -1 -24 13.7495 4.51956 5 -1 1 24 -1.4427 5.19913 3 -1 1 24 -1.4060 4.72477 2 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-3.9630 3.10824 5 0 2 24 0.58534 3.36890 3 0 2 24 2.55685 4.39109 4 0 2 24 -2.0728 4.16406 2 0 2 24 -3.4794 3.54653 5 -1 -2 -24 95.3784 12.8131 2 -1 -2 -24 107.915 10.4520 5 1 2 24 84.5931 10.7016 4 1 2 24 104.200 13.4699 2 1 2 24 79.9987 12.3223 3 1 2 24 107.002 12.5040 5 -2 -2 -24 29.6345 8.71687 2 -2 -2 -24 21.8419 5.87895 5 2 2 24 18.4373 7.98217 2 2 2 24 19.1210 6.59189 5 2 2 24 18.7665 5.94470 4 2 2 24 21.1300 7.74739 3 -3 -2 -24 46.3025 10.6139 2 -3 -2 -24 59.0959 8.39094 5 3 2 24 40.5286 9.29780 2 3 2 24 33.3468 7.40406 4 3 2 24 25.8665 7.64320 5 -4 -2 -24 30.2967 6.79610 5 4 2 24 22.7460 6.56651 4 4 2 24 32.9949 7.92756 5 4 2 24 21.1934 8.76690 2 2 -3 -24 -3.8899 6.76372 2 2 -3 -24 5.38799 4.26888 5 -2 3 24 0.00996 4.74235 3 -2 3 24 -2.4346 4.32493 4 -2 3 24 9.37245 5.51672 5 -2 3 24 9.57696 6.06200 2 1 -3 -24 9.65226 6.95978 2 1 -3 -24 19.7738 5.75525 5 -1 3 24 3.10607 4.54518 4 -1 3 24 10.0250 6.10166 5 -1 3 24 2.24457 4.93011 3 0 -3 -24 7.57204 5.49983 2 0 -3 -24 4.15708 3.71719 5 0 3 24 3.13152 4.73944 3 0 3 24 0.61557 4.54198 5 0 3 24 -0.8942 4.01502 4 0 3 24 -2.0492 4.96503 2 -1 -3 -24 -5.3898 3.18274 5 -1 -3 -24 1.96564 4.81282 2 1 3 24 0.79806 4.96218 3 1 3 24 -2.8220 3.73800 4 1 3 24 -1.6377 4.31564 5 1 3 24 3.49292 4.68955 2 -2 -3 -24 1.61394 4.82193 2 -2 -3 -24 1.53422 3.48972 5 2 3 24 -2.5847 3.73497 4 2 3 24 -9.8738 4.51679 2 2 3 24 -2.9064 4.38619 3 2 3 24 -0.2556 3.92935 5 -3 -3 -24 2.89699 3.78056 5 -3 -3 -24 -3.1007 3.10943 2 3 3 24 4.00040 4.31483 4 3 3 24 1.54015 5.03674 2 3 3 24 -8.1698 4.50628 5 -4 -3 -24 0.99957 3.95039 5 -4 -3 -24 4.53633 6.17301 2 4 3 24 4.67645 6.47551 2 4 3 24 13.0200 6.39827 5 4 3 24 3.09504 4.97515 4 -1 4 24 -2.4806 4.15441 4 -1 4 24 13.9939 6.02072 5 -1 4 24 4.19150 4.81934 3 -1 4 24 0.11243 4.77877 2 0 -4 -24 12.8177 5.10280 5 0 -4 -24 18.0440 7.79945 2 0 4 24 4.28414 6.29146 3 0 4 24 14.5395 6.48279 2 0 4 24 8.69152 5.80126 4 -1 -4 -24 9.69611 5.77139 2 -1 -4 -24 8.43028 5.44710 5 1 4 24 2.06129 4.99660 5 1 4 24 13.5735 6.13742 4 1 4 24 21.5565 7.08870 2 1 4 24 11.1498 6.14847 3 -2 -4 -24 2.08930 5.33649 2 -2 -4 -24 3.69806 4.17488 5 2 4 24 1.79108 4.86476 4 2 4 24 4.66563 5.25875 2 2 4 24 4.10826 5.39586 5 -3 -4 -24 13.4341 5.76643 2 3 4 24 23.0169 8.55955 2 3 4 24 8.65991 6.50099 5 3 4 24 26.5954 7.42830 4 -4 -4 -24 3.57523 5.75940 2 -4 -4 -24 10.5092 4.68945 5 4 4 24 3.92300 5.44074 5 4 4 24 1.16509 6.12493 2 1 -5 -24 24.1890 8.59894 2 1 -5 -24 7.01773 4.47142 5 -1 5 24 3.87794 5.49868 3 -1 5 24 21.5999 7.29403 5 -1 5 24 7.73083 5.88548 4 -1 5 24 6.81426 6.17288 2 0 -5 -24 -2.8558 3.81298 5 0 -5 -24 1.57204 6.73624 2 0 5 24 5.25387 4.85715 4 0 5 24 7.73631 5.27685 3 0 5 24 -2.1693 5.85511 2 0 5 24 2.41986 4.60089 5 -1 -5 -24 5.62684 5.98558 2 -1 -5 -24 -1.0799 4.16226 5 1 5 24 1.10463 4.88007 2 1 5 24 -1.7705 4.71644 4 -2 -5 -24 1.24799 3.89567 5 -2 -5 -24 -8.8905 4.83450 2 2 5 24 -0.5452 4.39925 4 2 5 24 -2.6219 5.55525 2 2 5 24 10.6374 6.51328 5 -3 -5 -24 -3.3416 3.77004 5 -3 -5 -24 -2.7034 4.68736 2 3 5 24 2.89695 5.98262 2 3 5 24 6.15878 4.49665 5 3 5 24 2.14164 5.01403 4 -4 -5 -24 -0.1016 3.38076 5 -4 -5 -24 -1.4003 5.36072 2 4 5 24 3.13369 6.27177 2 0 -6 -24 7.12182 6.91823 2 0 6 24 17.8231 7.06387 2 0 6 24 19.4122 7.86949 5 -1 -6 -24 29.9026 8.74272 2 -1 -6 -24 39.3836 8.32692 5 1 6 24 46.7771 10.5279 5 1 6 24 42.3731 9.23471 4 1 6 24 33.7764 10.1665 2 -2 -6 -24 10.2509 7.09366 2 2 6 24 19.6108 8.76452 2 2 6 24 14.3058 6.28132 4 -3 -6 -24 10.4775 8.89682 2 -3 -6 -24 9.35909 4.97139 5 3 6 24 11.4279 6.27268 5 3 6 24 17.1454 8.15390 2 3 6 24 4.11292 6.17491 4 0 3 -25 2.20353 4.28818 5 0 3 -25 4.85007 5.60161 2 0 -3 25 5.98222 4.50337 4 0 -3 25 -5.8071 4.78292 2 0 -3 25 -3.4924 3.67039 5 0 -3 25 -2.5054 4.40392 3 -1 3 -25 7.99398 6.60159 2 -1 3 -25 4.37855 4.06717 5 1 -3 25 -0.2075 5.67488 3 1 -3 25 0.76058 5.24838 2 1 -3 25 -1.3780 4.37974 4 1 -3 25 6.24584 5.55071 5 1 2 -25 3.26834 4.39326 5 1 2 -25 12.6997 6.99673 2 -1 -2 25 10.0875 5.97710 3 -1 -2 25 18.0392 6.80743 5 -1 -2 25 2.41185 4.80759 4 -1 -2 25 5.26976 5.08622 2 0 2 -25 8.96835 4.88200 5 0 2 -25 17.1194 7.22957 2 0 -2 25 -2.7977 4.79394 3 0 -2 25 18.8591 7.48679 4 0 -2 25 21.6901 6.83465 5 -1 2 -25 1.75941 5.17394 2 -1 2 -25 5.19902 4.33335 5 1 -2 25 1.38826 3.54832 3 1 -2 25 2.36885 4.03063 4 1 -2 25 0.78346 5.06191 2 1 -2 25 -2.5834 4.01416 5 -2 2 -25 109.298 13.9522 2 -2 2 -25 91.7273 12.1179 5 2 -2 25 79.9479 12.7271 3 2 -2 25 110.584 13.7562 2 1 1 -25 8.80447 6.50756 2 1 1 -25 1.93387 3.90953 5 -1 -1 25 3.53781 5.03226 2 -1 -1 25 5.56159 5.40230 4 -1 -1 25 -3.8325 4.48452 3 -1 -1 25 -0.7721 4.40705 5 0 1 -25 17.2841 5.59633 5 0 1 -25 6.80641 6.26682 2 0 -1 25 12.8623 5.42380 5 0 -1 25 11.0979 6.52476 3 0 -1 25 17.8794 6.01022 4 -1 1 -25 9.12859 5.45904 2 -1 1 -25 -0.9958 3.14354 5 1 -1 25 -0.8387 4.79744 4 1 -1 25 4.07245 5.47942 5 1 -1 25 -3.6631 5.11989 3 1 -1 25 5.64358 5.50849 2 -2 1 -25 -1.5648 4.81091 2 2 -1 25 2.71211 5.26554 3 2 -1 25 -4.5575 4.39953 2 2 -1 25 -1.9450 3.86842 4 -3 1 -25 4.65809 4.31298 5 3 -1 25 5.47829 4.45733 4 3 -1 25 1.59499 5.38069 2 3 -1 25 -2.5392 4.73456 5 3 -1 25 9.06423 6.40714 3 1 0 -25 11.3507 4.57771 5 1 0 -25 24.7687 8.83408 2 -1 0 25 12.2199 6.85626 3 -1 0 25 11.3546 5.44639 5 -1 0 25 17.5927 6.32938 2 -1 0 25 8.30896 5.81753 4 0 0 -25 77.1127 12.3459 2 0 0 -25 80.5523 9.34636 5 0 0 25 96.8469 12.9857 3 0 0 25 86.3318 13.1184 2 0 0 25 76.4896 10.9159 4 0 0 25 112.711 12.4306 5 -1 0 -25 -1.9091 3.89630 5 -1 0 -25 -0.6638 5.33735 2 1 0 25 -5.1235 3.67146 2 1 0 25 1.06307 5.16179 3 1 0 25 3.08935 3.99986 4 -2 0 -25 3.46587 5.05159 2 -2 0 -25 3.96276 4.45891 5 2 0 25 6.42915 4.85993 5 2 0 25 -2.2636 4.44309 3 2 0 25 9.65277 4.42629 4 2 0 25 4.59057 5.54047 2 -3 0 -25 14.9109 5.68648 5 -3 0 -25 12.6944 7.01201 2 3 0 25 7.93841 5.57497 2 3 0 25 5.96674 5.17472 4 3 0 25 14.1630 7.48304 3 3 0 25 13.5340 5.72870 5 1 -1 -25 3.69976 6.12458 2 1 -1 -25 8.12382 4.82103 5 -1 1 25 2.70801 5.11963 2 -1 1 25 10.6090 5.54070 5 -1 1 25 8.11185 4.82264 3 -1 1 25 12.8776 5.61041 4 0 -1 -25 3.92719 5.93228 2 0 -1 -25 0.76320 3.61138 5 0 1 25 1.86575 5.16613 2 0 1 25 5.89071 4.62134 4 0 1 25 -2.8233 4.21624 5 -1 -1 -25 7.04279 6.10266 2 -1 -1 -25 7.37983 5.12338 5 1 1 25 9.05071 5.49207 2 1 1 25 11.2205 5.15085 4 1 1 25 14.7472 7.97112 3 -2 -1 -25 -2.7484 3.49958 5 -2 -1 -25 0.19303 5.49174 2 2 1 25 -7.6786 3.96728 4 2 1 25 3.13366 5.29427 3 2 1 25 -4.6547 4.40062 2 2 1 25 7.20696 5.34285 5 -3 -1 -25 1.00045 4.40039 5 -3 -1 -25 5.87559 6.37414 2 3 1 25 -3.4411 5.76834 3 3 1 25 5.15018 5.64729 2 3 1 25 14.7280 6.20139 5 1 -2 -25 50.7762 10.9576 2 1 -2 -25 42.4707 7.88620 5 -1 2 25 47.5666 12.3192 3 -1 2 25 62.9291 9.93507 5 -1 2 25 47.4650 11.1785 2 0 -2 -25 41.5398 10.2833 2 0 -2 -25 41.5890 7.50890 5 0 2 25 34.4984 8.22719 5 0 2 25 38.2110 8.63186 4 0 2 25 29.1395 10.0436 2 -1 -2 -25 4.58247 4.41299 5 -1 -2 -25 0.29343 5.26297 2 1 2 25 5.38265 4.94904 4 1 2 25 2.08251 5.11534 2 1 2 25 8.38386 8.43487 3 -2 -2 -25 31.5233 6.99379 5 -2 -2 -25 15.7651 7.65919 2 2 2 25 31.8077 8.92227 3 2 2 25 24.9114 6.97030 4 2 2 25 23.4681 6.98376 5 2 2 25 32.9824 9.92408 2 -3 -2 -25 2.16073 5.26961 2 -3 -2 -25 -5.4226 4.23739 5 3 2 25 9.22766 6.12316 5 3 2 25 -6.4926 4.32338 4 3 2 25 7.76844 6.00029 2 1 -3 -25 20.3413 7.70104 2 1 -3 -25 22.0547 6.26235 5 -1 3 25 13.7402 7.32784 2 -1 3 25 37.4846 9.27971 4 -1 3 25 18.9126 6.58485 5 0 -3 -25 3.92429 4.65823 5 0 -3 -25 -7.2534 5.39554 2 0 3 25 8.15289 5.06099 5 0 3 25 12.0768 5.70293 4 -1 -3 -25 1.43786 3.94240 5 -1 -3 -25 4.46499 5.17431 2 1 3 25 2.15357 4.13823 4 1 3 25 3.22467 6.04899 2 1 3 25 1.04198 4.97824 5 1 3 25 3.06212 6.61100 3 -2 -3 -25 -0.2753 3.72453 5 -2 -3 -25 -10.115 4.56599 2 2 3 25 7.74326 5.35858 3 2 3 25 -7.7872 3.35700 2 2 3 25 6.79523 4.72779 4 -3 -3 -25 0.22169 4.05552 5 -3 -3 -25 -2.2547 5.66586 2 3 3 25 -2.0480 5.76147 2 3 3 25 6.01852 5.96322 5 3 3 25 4.18272 5.13351 4 0 -4 -25 81.2374 10.3963 5 0 -4 -25 89.9358 13.9833 2 0 4 25 82.8584 12.9273 5 0 4 25 86.5903 13.3181 2 0 4 25 76.9985 11.6561 4 -1 -4 -25 11.2778 5.01551 5 -1 -4 -25 6.45628 5.99885 2 1 4 25 8.13015 5.69885 4 1 4 25 -3.2205 5.51476 2 1 4 25 3.31271 5.42305 3 1 4 25 -3.7430 4.88049 5 -2 -4 -25 31.1585 10.1422 2 2 4 25 26.0674 9.82273 5 2 4 25 11.9445 6.75712 4 2 4 25 21.1304 8.21114 2 -3 -4 -25 7.44354 4.96255 5 3 4 25 3.94983 5.44931 4 3 4 25 1.28755 5.55371 2 3 4 25 -1.1193 5.97829 5 -1 -5 -25 8.47262 5.44102 5 -1 -5 -25 1.26568 5.84849 2 1 5 25 5.30649 5.92545 5 1 5 25 0.98021 5.16563 4 -2 -5 -25 -1.3249 4.24030 5 -2 -5 -25 3.72521 5.66548 2 2 5 25 3.28072 5.48570 5 2 5 25 3.99420 5.09947 4 2 5 25 -7.8493 5.10575 2 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 79165 _shelx_res_file ; TITL hsy10cg CELL 0.71073 7.4141 12.3595 19.9917 86.695 83.654 82.182 ZERR 4 0.0005 0.0011 0.0017 0.002 0.002 0.003 LATT 1 SFAC C H N O UNIT 76 104 8 16 TEMP -93 SIZE 0.30 0.18 0.08 OMIT -2 180.0 L.S. 20 ACTA BOND $H CONF HTAB LIST 4 FMAP 2 PLAN 20 MPLA 6 C141 > C147 MPLA 6 C241 > C247 WGHT 0.058600 0.383800 FVAR 0.73112 MOLE 1 N11 3 0.760964 0.620684 0.545663 11.00000 0.02812 0.03154 = 0.02091 -0.00476 -0.00218 -0.00480 H11 2 0.732709 0.604370 0.502557 11.00000 -1.20000 H12 2 0.880179 0.634952 0.539172 11.00000 -1.20000 C12 1 0.751806 0.523841 0.592812 11.00000 0.03876 0.02537 = 0.02896 -0.00653 -0.00171 -0.00340 AFIX 23 H12A 2 0.835897 0.461020 0.574218 11.00000 -1.20000 H12B 2 0.625994 0.503863 0.598071 11.00000 -1.20000 AFIX 0 C13 1 0.804662 0.548549 0.660751 11.00000 0.03968 0.02175 = 0.02542 -0.00143 -0.00392 0.00186 AFIX 23 H13A 2 0.792210 0.484515 0.692211 11.00000 -1.20000 H13B 2 0.934568 0.561206 0.655903 11.00000 -1.20000 AFIX 0 N14 3 0.690963 0.644487 0.689051 11.00000 0.02942 0.02138 = 0.02053 -0.00191 -0.00186 -0.00157 C15 1 0.695142 0.740043 0.642055 11.00000 0.03073 0.02186 = 0.02300 -0.00043 -0.00193 -0.00133 AFIX 23 H15A 2 0.820348 0.760961 0.635853 11.00000 -1.20000 H15B 2 0.611209 0.802356 0.661357 11.00000 -1.20000 AFIX 0 C16 1 0.638971 0.716577 0.574418 11.00000 0.03100 0.02811 = 0.02393 -0.00228 -0.00336 0.00085 AFIX 23 H16A 2 0.510476 0.701124 0.579844 11.00000 -1.20000 H16B 2 0.647190 0.781362 0.543265 11.00000 -1.20000 AFIX 0 C141 1 0.715492 0.664040 0.756638 11.00000 0.02630 0.02526 = 0.02173 0.00002 -0.00274 -0.00480 C142 1 0.827877 0.591601 0.795196 11.00000 0.04265 0.03264 = 0.02921 -0.00232 -0.00709 0.00584 AFIX 43 H142 2 0.897874 0.529444 0.775065 11.00000 -1.20000 AFIX 0 C143 1 0.838766 0.608980 0.862138 11.00000 0.05400 0.04176 = 0.03027 0.00084 -0.01437 0.00706 AFIX 43 H143 2 0.914449 0.557823 0.887565 11.00000 -1.20000 AFIX 0 C144 1 0.741584 0.699413 0.892783 11.00000 0.04871 0.04044 = 0.02280 -0.00297 -0.00851 -0.00578 C145 1 0.631848 0.772811 0.855312 11.00000 0.04221 0.03348 = 0.02777 -0.00738 -0.00414 0.00116 AFIX 43 H145 2 0.564903 0.835826 0.875493 11.00000 -1.20000 AFIX 0 C146 1 0.618906 0.754920 0.788253 11.00000 0.03397 0.03076 = 0.02438 -0.00240 -0.00700 0.00211 AFIX 43 H146 2 0.542078 0.806055 0.763241 11.00000 -1.20000 AFIX 0 O144 4 0.764863 0.708737 0.959505 11.00000 0.08815 0.05605 = 0.02602 -0.00794 -0.02072 0.00753 C147 1 0.680491 0.804451 0.990741 11.00000 0.11028 0.05331 = 0.02681 -0.01175 -0.01423 -0.00176 AFIX 137 H17A 2 0.727948 0.868110 0.967196 11.00000 -1.50000 H17B 2 0.706872 0.800862 1.037841 11.00000 -1.50000 H17C 2 0.547867 0.811072 0.988950 11.00000 -1.50000 AFIX 0 MOLE 2 N21 3 0.750643 0.114289 0.545766 11.00000 0.02617 0.03155 = 0.02204 -0.00470 -0.00284 -0.00383 H21 2 0.723067 0.097510 0.502572 11.00000 -1.20000 H22 2 0.867112 0.130046 0.541246 11.00000 -1.20000 C22 1 0.744412 0.017541 0.593390 11.00000 0.03705 0.02449 = 0.02862 -0.00557 -0.00378 -0.00335 AFIX 23 H22A 2 0.832080 -0.044325 0.575491 11.00000 -1.20000 H22B 2 0.620191 -0.004780 0.598160 11.00000 -1.20000 AFIX 0 C23 1 0.792763 0.045008 0.661520 11.00000 0.03621 0.02410 = 0.02590 -0.00185 -0.00449 0.00169 AFIX 23 H23A 2 0.782873 -0.018897 0.693285 11.00000 -1.20000 H23B 2 0.921247 0.060383 0.657141 11.00000 -1.20000 AFIX 0 N24 3 0.672391 0.140151 0.689042 11.00000 0.02744 0.02269 = 0.02135 -0.00149 -0.00337 -0.00186 C25 1 0.675581 0.234654 0.641432 11.00000 0.02759 0.02280 = 0.02548 -0.00116 -0.00182 0.00011 AFIX 23 H25A 2 0.799865 0.256936 0.635605 11.00000 -1.20000 H25B 2 0.589249 0.296681 0.659862 11.00000 -1.20000 AFIX 0 C26 1 0.623182 0.208455 0.573810 11.00000 0.02833 0.02953 = 0.02336 -0.00055 -0.00391 0.00065 AFIX 23 H26A 2 0.496260 0.190263 0.578998 11.00000 -1.20000 H26B 2 0.628340 0.273095 0.542361 11.00000 -1.20000 AFIX 0 C241 1 0.701631 0.160993 0.756119 11.00000 0.02384 0.02735 = 0.02364 -0.00218 -0.00208 -0.00350 C242 1 0.714609 0.076278 0.804888 11.00000 0.06975 0.03063 = 0.03067 0.00081 -0.01281 -0.01030 AFIX 43 H242 2 0.705323 0.004117 0.792910 11.00000 -1.20000 AFIX 0 C243 1 0.740610 0.094705 0.870120 11.00000 0.08665 0.04022 = 0.02999 0.00563 -0.01914 -0.00595 AFIX 43 H243 2 0.748474 0.035189 0.902385 11.00000 -1.20000 AFIX 0 C244 1 0.755423 0.198003 0.889412 11.00000 0.04634 0.04742 = 0.02387 -0.00635 -0.00868 -0.00076 C245 1 0.739118 0.283215 0.843038 11.00000 0.06651 0.03587 = 0.03201 -0.00953 -0.00922 -0.00756 AFIX 43 H245 2 0.745796 0.355343 0.855738 11.00000 -1.20000 AFIX 0 C246 1 0.712633 0.264241 0.776963 11.00000 0.06457 0.02887 = 0.02808 -0.00075 -0.00684 -0.00804 AFIX 43 H246 2 0.701793 0.324389 0.745218 11.00000 -1.20000 AFIX 0 O244 4 0.787418 0.206228 0.955434 11.00000 0.09569 0.06008 = 0.02939 -0.01071 -0.02457 0.00047 C247 1 0.803586 0.310745 0.977219 11.00000 0.10323 0.07215 = 0.04621 -0.02655 -0.03227 0.00218 AFIX 137 H27A 2 0.901494 0.341764 0.948572 11.00000 -1.50000 H27B 2 0.832788 0.304488 1.024027 11.00000 -1.50000 H27C 2 0.687704 0.358567 0.974188 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.754138 0.592373 0.303439 11.00000 0.02259 0.02813 = 0.02810 -0.00629 -0.00446 0.00107 C32 1 0.802719 0.664910 0.250842 11.00000 0.04305 0.02762 = 0.03616 -0.00139 -0.00802 -0.00414 AFIX 43 H32 2 0.851735 0.729002 0.259968 11.00000 -1.20000 AFIX 0 C33 1 0.779878 0.644000 0.185307 11.00000 0.05717 0.04154 = 0.03233 0.00473 -0.00886 -0.00561 AFIX 43 H33 2 0.812559 0.694608 0.149930 11.00000 -1.20000 AFIX 0 C34 1 0.710400 0.550898 0.170118 11.00000 0.03973 0.04955 = 0.03039 -0.00829 -0.00720 -0.00052 C35 1 0.667130 0.477466 0.222622 11.00000 0.03565 0.04401 = 0.03586 -0.01597 -0.00319 -0.01078 AFIX 43 H35 2 0.623080 0.411882 0.213193 11.00000 -1.20000 AFIX 0 C36 1 0.687101 0.498195 0.288648 11.00000 0.02913 0.03317 = 0.03057 -0.00620 0.00043 -0.00675 AFIX 43 H36 2 0.654592 0.447470 0.323981 11.00000 -1.20000 AFIX 0 C37 1 0.772048 0.617934 0.375035 11.00000 0.02623 0.02861 = 0.03144 -0.00974 -0.00748 0.00499 O31 4 0.694447 0.561443 0.421793 11.00000 0.04097 0.04019 = 0.02550 -0.00693 -0.00488 -0.00213 O32 4 0.860489 0.693328 0.384148 11.00000 0.05210 0.04765 = 0.04519 -0.01910 -0.00840 -0.01664 C38 1 0.682146 0.528578 0.098719 11.00000 0.07168 0.08167 = 0.03486 -0.01301 -0.01541 -0.00649 AFIX 137 H38A 2 0.637304 0.597159 0.075288 11.00000 -1.50000 H38B 2 0.592221 0.477170 0.099462 11.00000 -1.50000 H38C 2 0.798595 0.496934 0.075115 11.00000 -1.50000 AFIX 0 MOLE 4 C41 1 0.780876 0.092751 0.302540 11.00000 0.02277 0.02714 = 0.02773 -0.00463 -0.00649 -0.00040 C42 1 0.856349 0.161648 0.252945 11.00000 0.03237 0.02987 = 0.04327 -0.00117 -0.00600 -0.00605 AFIX 43 H42 2 0.901803 0.225164 0.265218 11.00000 -1.20000 AFIX 0 C43 1 0.865543 0.137941 0.185478 11.00000 0.04653 0.04453 = 0.03588 0.00744 0.00172 -0.00396 AFIX 43 H43 2 0.916484 0.186048 0.152039 11.00000 -1.20000 AFIX 0 C44 1 0.801974 0.045681 0.166078 11.00000 0.04736 0.04459 = 0.02816 -0.00391 -0.00555 0.00609 C45 1 0.727623 -0.023080 0.215808 11.00000 0.04461 0.03193 = 0.03365 -0.00941 -0.01190 -0.00036 AFIX 43 H45 2 0.683144 -0.086849 0.203422 11.00000 -1.20000 AFIX 0 C46 1 0.717182 -0.000194 0.283370 11.00000 0.03141 0.02808 = 0.02804 -0.00228 -0.00594 -0.00294 AFIX 43 H46 2 0.666142 -0.048412 0.316714 11.00000 -1.20000 AFIX 0 C47 1 0.771686 0.118217 0.375614 11.00000 0.02524 0.03134 = 0.03307 -0.01074 -0.00904 0.00307 O41 4 0.692948 0.056643 0.419298 11.00000 0.03981 0.04172 = 0.02602 -0.00619 -0.00630 -0.00149 O42 4 0.842429 0.198265 0.389472 11.00000 0.06308 0.05104 = 0.05158 -0.02393 -0.00904 -0.02110 C48 1 0.810152 0.019657 0.092755 11.00000 0.08757 0.07099 = 0.02960 -0.00812 -0.00633 0.00813 AFIX 137 H48A 2 0.852356 0.080476 0.064377 11.00000 -1.50000 H48B 2 0.688010 0.008699 0.082312 11.00000 -1.50000 H48C 2 0.895390 -0.047075 0.084043 11.00000 -1.50000 AFIX 0 MOLE 5 O51 4 0.878151 0.858629 0.461188 11.00000 0.03382 0.03341 = 0.03408 -0.00897 -0.00416 -0.00565 H51 2 0.813254 0.917536 0.444527 11.00000 -1.50000 H52 2 0.863770 0.802788 0.434676 11.00000 -1.50000 MOLE 6 O61 4 0.864705 0.361561 0.465710 11.00000 0.03633 0.03334 = 0.03403 -0.01040 -0.00341 -0.00663 H61 2 0.845311 0.305739 0.441217 11.00000 -1.50000 H62 2 0.797031 0.423445 0.449232 11.00000 -1.50000 HKLF 4 REM hsy10cg REM R1 = 0.0456 for 5772 Fo > 4sig(Fo) and 0.0727 for all 8288 data REM 479 parameters refined using 0 restraints END WGHT 0.0586 0.3838 REM Instructions for potential hydrogen bonds HTAB N11 O31 EQIV $1 -x+2, -y+1, -z+1 HTAB N11 O61_$1 HTAB C12 O61 HTAB C15 O42_$1 HTAB C16 O51 EQIV $2 -x+1, -y+1, -z+2 HTAB C147 O244_$2 HTAB N21 O41 HTAB N21 O42 HTAB N21 O51_$1 EQIV $3 x, y-1, z HTAB C22 O51_$3 EQIV $4 -x+1, -y, -z+1 HTAB C22 O41_$4 HTAB C25 O32_$1 HTAB C26 O61 EQIV $5 x, y+1, z HTAB O51 O41_$5 HTAB O51 O32 HTAB O61 O42 HTAB O61 O31 REM Highest difference peak 0.297, deepest hole -0.181, 1-sigma level 0.038 Q1 1 0.7809 0.5640 0.0605 11.00000 0.05 0.30 Q2 1 0.7672 0.0989 0.3380 11.00000 0.05 0.25 Q3 1 0.7663 0.5371 0.6254 11.00000 0.05 0.23 Q4 1 0.7669 0.5965 0.3374 11.00000 0.05 0.20 Q5 1 0.7428 0.0700 0.0623 11.00000 0.05 0.19 Q6 1 0.6646 0.7223 0.6085 11.00000 0.05 0.19 Q7 1 0.7611 0.0332 0.6276 11.00000 0.05 0.19 Q8 1 0.7232 0.6577 0.7208 11.00000 0.05 0.19 Q9 1 0.7397 0.5565 0.4591 11.00000 0.05 0.18 Q10 1 0.7033 0.1526 0.7207 11.00000 0.05 0.18 Q11 1 0.7163 0.4501 0.0881 11.00000 0.05 0.17 Q12 1 0.7454 -0.0157 0.2510 11.00000 0.05 0.17 Q13 1 0.7220 0.0289 0.1908 11.00000 0.05 0.17 Q14 1 0.7277 0.1010 0.6745 11.00000 0.05 0.17 Q15 1 0.6382 0.2169 0.6099 11.00000 0.05 0.16 Q16 1 0.6823 0.1189 0.7786 11.00000 0.05 0.16 Q17 1 0.6742 0.1815 0.6656 11.00000 0.05 0.16 Q18 1 0.7443 0.6330 0.8794 11.00000 0.05 0.16 Q19 1 0.7129 0.0664 0.4652 11.00000 0.05 0.15 Q20 1 0.7167 0.7423 0.8670 11.00000 0.05 0.15 ; _shelx_res_checksum 97417 _shelxl_version_number 2.014 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 N11 0.76096(16) 0.62068(10) 0.54566(6) 0.0267(3) Uani d 1 . . H H11 0.733(2) 0.6044(12) 0.5026(8) 0.032 Uiso d 1 . . H H12 0.880(2) 0.6350(12) 0.5392(7) 0.032 Uiso d 1 . . C C12 0.7518(2) 0.52384(11) 0.59281(7) 0.0310(3) Uani d 1 . . H H12A 0.8359 0.4610 0.5742 0.037 Uiso calc 1 . . H H12B 0.6260 0.5039 0.5981 0.037 Uiso calc 1 . . C C13 0.8047(2) 0.54855(11) 0.66075(7) 0.0294(3) Uani d 1 . . H H13A 0.7922 0.4845 0.6922 0.035 Uiso calc 1 . . H H13B 0.9346 0.5612 0.6559 0.035 Uiso calc 1 . . N N14 0.69096(14) 0.64449(9) 0.68905(5) 0.0240(2) Uani d 1 . . C C15 0.69514(18) 0.74004(10) 0.64205(6) 0.0255(3) Uani d 1 . . H H15A 0.8203 0.7610 0.6359 0.031 Uiso calc 1 . . H H15B 0.6112 0.8024 0.6614 0.031 Uiso calc 1 . . C C16 0.63897(18) 0.71658(11) 0.57442(6) 0.0280(3) Uani d 1 . . H H16A 0.5105 0.7011 0.5798 0.034 Uiso calc 1 . . H H16B 0.6472 0.7814 0.5433 0.034 Uiso calc 1 . . C C141 0.71549(17) 0.66404(11) 0.75664(6) 0.0243(3) Uani d 1 . . C C142 0.8279(2) 0.59160(12) 0.79520(7) 0.0355(3) Uani d 1 . . H H142 0.8979 0.5294 0.7751 0.043 Uiso calc 1 . . C C143 0.8388(2) 0.60898(14) 0.86214(7) 0.0426(4) Uani d 1 . . H H143 0.9144 0.5578 0.8876 0.051 Uiso calc 1 . . C C144 0.7416(2) 0.69941(13) 0.89278(7) 0.0369(3) Uani d 1 . . C C145 0.6318(2) 0.77281(12) 0.85531(7) 0.0348(3) Uani d 1 . . H H145 0.5649 0.8358 0.8755 0.042 Uiso calc 1 . . C C146 0.61891(19) 0.75492(12) 0.78825(7) 0.0299(3) Uani d 1 . . H H146 0.5421 0.8061 0.7632 0.036 Uiso calc 1 . . O O144 0.76486(19) 0.70874(10) 0.95950(5) 0.0570(4) Uani d 1 . . C C147 0.6805(3) 0.80445(16) 0.99074(8) 0.0634(6) Uani d 1 . . H H17A 0.7279 0.8681 0.9672 0.095 Uiso calc 1 . . H H17B 0.7069 0.8009 1.0378 0.095 Uiso calc 1 . . H H17C 0.5479 0.8111 0.9889 0.095 Uiso calc 1 . . N N21 0.75064(16) 0.11429(10) 0.54577(6) 0.0264(2) Uani d 1 . . H H21 0.723(2) 0.0975(12) 0.5026(8) 0.032 Uiso d 1 . . H H22 0.867(2) 0.1300(12) 0.5412(7) 0.032 Uiso d 1 . . C C22 0.7444(2) 0.01754(11) 0.59339(7) 0.0299(3) Uani d 1 . . H H22A 0.8321 -0.0443 0.5755 0.036 Uiso calc 1 . . H H22B 0.6202 -0.0048 0.5982 0.036 Uiso calc 1 . . C C23 0.79276(19) 0.04501(11) 0.66152(7) 0.0291(3) Uani d 1 . . H H23A 0.7829 -0.0189 0.6933 0.035 Uiso calc 1 . . H H23B 0.9212 0.0604 0.6571 0.035 Uiso calc 1 . . N N24 0.67239(14) 0.14015(9) 0.68904(5) 0.0239(2) Uani d 1 . . C C25 0.67558(18) 0.23465(11) 0.64143(6) 0.0257(3) Uani d 1 . . H H25A 0.7999 0.2569 0.6356 0.031 Uiso calc 1 . . H H25B 0.5892 0.2967 0.6599 0.031 Uiso calc 1 . . C C26 0.62318(18) 0.20845(11) 0.57381(6) 0.0274(3) Uani d 1 . . H H26A 0.4963 0.1903 0.5790 0.033 Uiso calc 1 . . H H26B 0.6283 0.2731 0.5424 0.033 Uiso calc 1 . . C C241 0.70163(17) 0.16099(11) 0.75612(6) 0.0249(3) Uani d 1 . . C C242 0.7146(2) 0.07628(13) 0.80489(7) 0.0428(4) Uani d 1 . . H H242 0.7053 0.0041 0.7929 0.051 Uiso calc 1 . . C C243 0.7406(3) 0.09470(14) 0.87012(8) 0.0518(5) Uani d 1 . . H H243 0.7485 0.0352 0.9024 0.062 Uiso calc 1 . . C C244 0.7554(2) 0.19800(14) 0.88941(7) 0.0391(4) Uani d 1 . . C C245 0.7391(2) 0.28321(14) 0.84304(8) 0.0441(4) Uani d 1 . . H H245 0.7458 0.3553 0.8557 0.053 Uiso calc 1 . . C C246 0.7126(2) 0.26424(13) 0.77696(7) 0.0402(4) Uani d 1 . . H H246 0.7018 0.3244 0.7452 0.048 Uiso calc 1 . . O O244 0.7874(2) 0.20623(11) 0.95543(6) 0.0610(4) Uani d 1 . . C C247 0.8036(3) 0.31074(18) 0.97722(10) 0.0723(7) Uani d 1 . . H H27A 0.9015 0.3418 0.9486 0.109 Uiso calc 1 . . H H27B 0.8328 0.3045 1.0240 0.109 Uiso calc 1 . . H H27C 0.6877 0.3586 0.9742 0.109 Uiso calc 1 . . C C31 0.75414(17) 0.59237(11) 0.30344(7) 0.0263(3) Uani d 1 . . C C32 0.8027(2) 0.66491(12) 0.25084(7) 0.0354(3) Uani d 1 . . H H32 0.8517 0.7290 0.2600 0.042 Uiso calc 1 . . C C33 0.7799(2) 0.64400(14) 0.18531(8) 0.0437(4) Uani d 1 . . H H33 0.8126 0.6946 0.1499 0.052 Uiso calc 1 . . C C34 0.7104(2) 0.55090(14) 0.17012(8) 0.0399(4) Uani d 1 . . C C35 0.6671(2) 0.47747(13) 0.22262(7) 0.0375(4) Uani d 1 . . H H35 0.6231 0.4119 0.2132 0.045 Uiso calc 1 . . C C36 0.68710(18) 0.49820(12) 0.28865(7) 0.0308(3) Uani d 1 . . H H36 0.6546 0.4475 0.3240 0.037 Uiso calc 1 . . C C37 0.77205(18) 0.61793(11) 0.37504(7) 0.0289(3) Uani d 1 . . O O31 0.69445(14) 0.56144(8) 0.42179(5) 0.0355(2) Uani d 1 . . O O32 0.86049(16) 0.69333(10) 0.38415(6) 0.0465(3) Uani d 1 . . C C38 0.6821(3) 0.52858(18) 0.09872(9) 0.0619(5) Uani d 1 . . H H38A 0.6373 0.5972 0.0753 0.093 Uiso calc 1 . . H H38B 0.5922 0.4772 0.0995 0.093 Uiso calc 1 . . H H38C 0.7986 0.4969 0.0751 0.093 Uiso calc 1 . . C C41 0.78088(17) 0.09275(11) 0.30254(7) 0.0257(3) Uani d 1 . . C C42 0.85635(19) 0.16165(12) 0.25294(8) 0.0348(3) Uani d 1 . . H H42 0.9018 0.2252 0.2652 0.042 Uiso calc 1 . . C C43 0.8655(2) 0.13794(14) 0.18548(8) 0.0433(4) Uani d 1 . . H H43 0.9165 0.1860 0.1520 0.052 Uiso calc 1 . . C C44 0.8020(2) 0.04568(14) 0.16608(7) 0.0409(4) Uani d 1 . . C C45 0.7276(2) -0.02308(13) 0.21581(7) 0.0363(3) Uani d 1 . . H H45 0.6831 -0.0868 0.2034 0.044 Uiso calc 1 . . C C46 0.71718(18) -0.00019(11) 0.28337(7) 0.0290(3) Uani d 1 . . H H46 0.6661 -0.0484 0.3167 0.035 Uiso calc 1 . . C C47 0.77169(18) 0.11822(12) 0.37561(7) 0.0297(3) Uani d 1 . . O O41 0.69295(14) 0.05664(9) 0.41930(5) 0.0358(2) Uani d 1 . . O O42 0.84243(17) 0.19826(10) 0.38947(6) 0.0529(3) Uani d 1 . . C C48 0.8102(3) 0.01966(18) 0.09276(8) 0.0642(6) Uani d 1 . . H H48A 0.8524 0.0805 0.0644 0.096 Uiso calc 1 . . H H48B 0.6880 0.0087 0.0823 0.096 Uiso calc 1 . . H H48C 0.8954 -0.0471 0.0840 0.096 Uiso calc 1 . . O O51 0.87815(14) 0.85863(9) 0.46119(5) 0.0333(2) Uani d 1 . . H H51 0.813(3) 0.9175(16) 0.4445(9) 0.050 Uiso d 1 . . H H52 0.864(2) 0.8028(15) 0.4347(9) 0.050 Uiso d 1 . . O O61 0.86471(14) 0.36156(9) 0.46571(5) 0.0340(2) Uani d 1 . . H H61 0.845(2) 0.3057(16) 0.4412(9) 0.051 Uiso d 1 . . H H62 0.797(3) 0.4234(16) 0.4492(9) 0.051 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 N11 0.0281(6) 0.0315(7) 0.0209(6) -0.0048(5) -0.0022(4) -0.0048(5) C12 0.0388(8) 0.0254(7) 0.0290(7) -0.0034(6) -0.0017(6) -0.0065(6) C13 0.0397(8) 0.0217(7) 0.0254(7) 0.0019(6) -0.0039(6) -0.0014(5) N14 0.0294(6) 0.0214(6) 0.0205(5) -0.0016(4) -0.0019(4) -0.0019(4) C15 0.0307(7) 0.0219(7) 0.0230(6) -0.0013(5) -0.0019(5) -0.0004(5) C16 0.0310(7) 0.0281(7) 0.0239(7) 0.0009(5) -0.0034(5) -0.0023(5) C141 0.0263(6) 0.0253(7) 0.0217(6) -0.0048(5) -0.0027(5) 0.0000(5) C142 0.0426(8) 0.0326(8) 0.0292(7) 0.0058(6) -0.0071(6) -0.0023(6) C143 0.0540(10) 0.0418(9) 0.0303(8) 0.0071(7) -0.0144(7) 0.0008(7) C144 0.0487(9) 0.0404(9) 0.0228(7) -0.0058(7) -0.0085(6) -0.0030(6) C145 0.0422(8) 0.0335(8) 0.0278(7) 0.0012(6) -0.0041(6) -0.0074(6) C146 0.0340(7) 0.0308(8) 0.0244(7) 0.0021(6) -0.0070(5) -0.0024(6) O144 0.0881(10) 0.0560(8) 0.0260(6) 0.0075(7) -0.0207(6) -0.0079(5) C147 0.1103(17) 0.0533(12) 0.0268(9) -0.0018(11) -0.0142(9) -0.0118(8) N21 0.0262(6) 0.0316(7) 0.0220(6) -0.0038(5) -0.0028(4) -0.0047(5) C22 0.0371(7) 0.0245(7) 0.0286(7) -0.0034(6) -0.0038(6) -0.0056(6) C23 0.0362(7) 0.0241(7) 0.0259(7) 0.0017(6) -0.0045(5) -0.0018(5) N24 0.0274(6) 0.0227(6) 0.0213(5) -0.0019(4) -0.0034(4) -0.0015(4) C25 0.0276(7) 0.0228(7) 0.0255(7) 0.0001(5) -0.0018(5) -0.0012(5) C26 0.0283(7) 0.0295(7) 0.0234(7) 0.0007(5) -0.0039(5) -0.0005(5) C241 0.0238(6) 0.0274(7) 0.0236(6) -0.0035(5) -0.0021(5) -0.0022(5) C242 0.0697(11) 0.0306(8) 0.0307(8) -0.0103(8) -0.0128(7) 0.0008(6) C243 0.0867(14) 0.0402(10) 0.0300(8) -0.0060(9) -0.0191(8) 0.0056(7) C244 0.0463(9) 0.0474(10) 0.0239(7) -0.0008(7) -0.0087(6) -0.0063(7) C245 0.0665(11) 0.0359(9) 0.0320(8) -0.0076(8) -0.0092(7) -0.0095(7) C246 0.0646(11) 0.0289(8) 0.0281(7) -0.0080(7) -0.0068(7) -0.0008(6) O244 0.0957(10) 0.0601(8) 0.0294(6) 0.0005(7) -0.0246(6) -0.0107(6) C247 0.1032(18) 0.0722(15) 0.0462(11) 0.0022(12) -0.0323(11) -0.0265(10) C31 0.0226(6) 0.0281(7) 0.0281(7) 0.0011(5) -0.0045(5) -0.0063(6) C32 0.0431(8) 0.0276(8) 0.0362(8) -0.0041(6) -0.0080(6) -0.0014(6) C33 0.0572(10) 0.0415(10) 0.0323(8) -0.0056(8) -0.0089(7) 0.0047(7) C34 0.0397(8) 0.0495(10) 0.0304(8) -0.0005(7) -0.0072(6) -0.0083(7) C35 0.0356(8) 0.0440(9) 0.0359(8) -0.0108(7) -0.0032(6) -0.0160(7) C36 0.0291(7) 0.0332(8) 0.0306(7) -0.0068(6) 0.0004(5) -0.0062(6) C37 0.0262(7) 0.0286(7) 0.0314(7) 0.0050(6) -0.0075(5) -0.0097(6) O31 0.0410(6) 0.0402(6) 0.0255(5) -0.0021(5) -0.0049(4) -0.0069(4) O32 0.0521(7) 0.0477(7) 0.0452(7) -0.0166(5) -0.0084(5) -0.0191(5) C38 0.0717(13) 0.0817(15) 0.0349(9) -0.0065(11) -0.0154(9) -0.0130(9) C41 0.0228(6) 0.0271(7) 0.0277(7) -0.0004(5) -0.0065(5) -0.0046(5) C42 0.0324(7) 0.0299(8) 0.0433(9) -0.0060(6) -0.0060(6) -0.0012(6) C43 0.0465(9) 0.0445(10) 0.0359(8) -0.0040(7) 0.0017(7) 0.0074(7) C44 0.0474(9) 0.0446(9) 0.0282(8) 0.0061(7) -0.0055(6) -0.0039(7) C45 0.0446(9) 0.0319(8) 0.0336(8) -0.0004(6) -0.0119(6) -0.0094(6) C46 0.0314(7) 0.0281(7) 0.0280(7) -0.0029(6) -0.0059(5) -0.0023(6) C47 0.0252(7) 0.0313(8) 0.0331(7) 0.0031(6) -0.0090(5) -0.0107(6) O41 0.0398(6) 0.0417(6) 0.0260(5) -0.0015(5) -0.0063(4) -0.0062(4) O42 0.0631(8) 0.0510(7) 0.0516(7) -0.0211(6) -0.0090(6) -0.0239(6) C48 0.0876(15) 0.0710(14) 0.0296(9) 0.0081(11) -0.0063(9) -0.0081(9) O51 0.0338(5) 0.0334(6) 0.0341(6) -0.0057(4) -0.0042(4) -0.0090(5) O61 0.0363(6) 0.0333(6) 0.0340(6) -0.0066(5) -0.0034(4) -0.0104(5) 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 C12 N11 C16 . . 109.88(10) ? C12 N11 H11 . . 110.3(9) ? C16 N11 H11 . . 112.7(9) ? C12 N11 H12 . . 108.3(10) ? C16 N11 H12 . . 110.4(9) ? H11 N11 H12 . . 105.1(13) ? N11 C12 C13 . . 110.18(11) ? N11 C12 H12A . . 109.6 ? C13 C12 H12A . . 109.6 ? N11 C12 H12B . . 109.6 ? C13 C12 H12B . . 109.6 ? H12A C12 H12B . . 108.1 ? N14 C13 C12 . . 112.02(11) ? N14 C13 H13A . . 109.2 ? C12 C13 H13A . . 109.2 ? N14 C13 H13B . . 109.2 ? C12 C13 H13B . . 109.2 ? H13A C13 H13B . . 107.9 ? C141 N14 C13 . . 115.21(10) ? C141 N14 C15 . . 115.05(10) ? C13 N14 C15 . . 111.21(10) ? N14 C15 C16 . . 111.37(11) ? N14 C15 H15A . . 109.4 ? C16 C15 H15A . . 109.4 ? N14 C15 H15B . . 109.4 ? C16 C15 H15B . . 109.4 ? H15A C15 H15B . . 108.0 ? N11 C16 C15 . . 109.93(11) ? N11 C16 H16A . . 109.7 ? C15 C16 H16A . . 109.7 ? N11 C16 H16B . . 109.7 ? C15 C16 H16B . . 109.7 ? H16A C16 H16B . . 108.2 ? C146 C141 C142 . . 117.13(12) ? C146 C141 N14 . . 120.41(11) ? C142 C141 N14 . . 122.38(12) ? C143 C142 C141 . . 120.97(13) ? C143 C142 H142 . . 119.5 ? C141 C142 H142 . . 119.5 ? C142 C143 C144 . . 121.15(14) ? C142 C143 H143 . . 119.4 ? C144 C143 H143 . . 119.4 ? O144 C144 C145 . . 125.25(14) ? O144 C144 C143 . . 115.95(13) ? C145 C144 C143 . . 118.79(13) ? C144 C145 C146 . . 120.21(13) ? C144 C145 H145 . . 119.9 ? C146 C145 H145 . . 119.9 ? C145 C146 C141 . . 121.74(13) ? C145 C146 H146 . . 119.1 ? C141 C146 H146 . . 119.1 ? C144 O144 C147 . . 117.49(13) ? O144 C147 H17A . . 109.5 ? O144 C147 H17B . . 109.5 ? H17A C147 H17B . . 109.5 ? O144 C147 H17C . . 109.5 ? H17A C147 H17C . . 109.5 ? H17B C147 H17C . . 109.5 ? C22 N21 C26 . . 109.64(10) ? C22 N21 H21 . . 110.7(9) ? C26 N21 H21 . . 111.8(9) ? C22 N21 H22 . . 106.9(10) ? C26 N21 H22 . . 110.2(10) ? H21 N21 H22 . . 107.5(13) ? N21 C22 C23 . . 109.97(11) ? N21 C22 H22A . . 109.7 ? C23 C22 H22A . . 109.7 ? N21 C22 H22B . . 109.7 ? C23 C22 H22B . . 109.7 ? H22A C22 H22B . . 108.2 ? N24 C23 C22 . . 112.03(11) ? N24 C23 H23A . . 109.2 ? C22 C23 H23A . . 109.2 ? N24 C23 H23B . . 109.2 ? C22 C23 H23B . . 109.2 ? H23A C23 H23B . . 107.9 ? C241 N24 C25 . . 114.88(10) ? C241 N24 C23 . . 113.35(10) ? C25 N24 C23 . . 110.62(10) ? N24 C25 C26 . . 111.20(11) ? N24 C25 H25A . . 109.4 ? C26 C25 H25A . . 109.4 ? N24 C25 H25B . . 109.4 ? C26 C25 H25B . . 109.4 ? H25A C25 H25B . . 108.0 ? N21 C26 C25 . . 110.03(10) ? N21 C26 H26A . . 109.7 ? C25 C26 H26A . . 109.7 ? N21 C26 H26B . . 109.7 ? C25 C26 H26B . . 109.7 ? H26A C26 H26B . . 108.2 ? C246 C241 C242 . . 116.53(13) ? C246 C241 N24 . . 123.04(12) ? C242 C241 N24 . . 120.40(12) ? C243 C242 C241 . . 121.40(15) ? C243 C242 H242 . . 119.3 ? C241 C242 H242 . . 119.3 ? C242 C243 C244 . . 121.06(15) ? C242 C243 H243 . . 119.5 ? C244 C243 H243 . . 119.5 ? C245 C244 C243 . . 118.89(14) ? C245 C244 O244 . . 125.06(15) ? C243 C244 O244 . . 116.05(14) ? C244 C245 C246 . . 119.87(15) ? C244 C245 H245 . . 120.1 ? C246 C245 H245 . . 120.1 ? C241 C246 C245 . . 122.22(14) ? C241 C246 H246 . . 118.9 ? C245 C246 H246 . . 118.9 ? C244 O244 C247 . . 117.82(14) ? O244 C247 H27A . . 109.5 ? O244 C247 H27B . . 109.5 ? H27A C247 H27B . . 109.5 ? O244 C247 H27C . . 109.5 ? H27A C247 H27C . . 109.5 ? H27B C247 H27C . . 109.5 ? C36 C31 C32 . . 118.79(13) ? C36 C31 C37 . . 121.27(12) ? C32 C31 C37 . . 119.93(13) ? C33 C32 C31 . . 120.19(14) ? C33 C32 H32 . . 119.9 ? C31 C32 H32 . . 119.9 ? C32 C33 C34 . . 121.44(15) ? C32 C33 H33 . . 119.3 ? C34 C33 H33 . . 119.3 ? C33 C34 C35 . . 118.01(14) ? C33 C34 C38 . . 121.66(16) ? C35 C34 C38 . . 120.33(16) ? C36 C35 C34 . . 121.09(14) ? C36 C35 H35 . . 119.5 ? C34 C35 H35 . . 119.5 ? C31 C36 C35 . . 120.44(14) ? C31 C36 H36 . . 119.8 ? C35 C36 H36 . . 119.8 ? O32 C37 O31 . . 124.57(13) ? O32 C37 C31 . . 117.82(13) ? O31 C37 C31 . . 117.61(12) ? C34 C38 H38A . . 109.5 ? C34 C38 H38B . . 109.5 ? H38A C38 H38B . . 109.5 ? C34 C38 H38C . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? C46 C41 C42 . . 118.81(12) ? C46 C41 C47 . . 121.00(12) ? C42 C41 C47 . . 120.18(12) ? C43 C42 C41 . . 120.21(14) ? C43 C42 H42 . . 119.9 ? C41 C42 H42 . . 119.9 ? C44 C43 C42 . . 121.24(15) ? C44 C43 H43 . . 119.4 ? C42 C43 H43 . . 119.4 ? C43 C44 C45 . . 118.30(14) ? C43 C44 C48 . . 121.61(16) ? C45 C44 C48 . . 120.08(16) ? C44 C45 C46 . . 121.03(14) ? C44 C45 H45 . . 119.5 ? C46 C45 H45 . . 119.5 ? C45 C46 C41 . . 120.40(13) ? C45 C46 H46 . . 119.8 ? C41 C46 H46 . . 119.8 ? O42 C47 O41 . . 123.97(13) ? O42 C47 C41 . . 117.63(14) ? O41 C47 C41 . . 118.40(12) ? C44 C48 H48A . . 109.5 ? C44 C48 H48B . . 109.5 ? H48A C48 H48B . . 109.5 ? C44 C48 H48C . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? H51 O51 H52 . . 105.5(16) ? H61 O61 H62 . . 106.6(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 N11 C12 . 1.4845(18) ? N11 C16 . 1.4917(17) ? N11 H11 . 0.948(16) ? N11 H12 . 0.918(16) ? C12 C13 . 1.5131(18) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 N14 . 1.4617(16) ? C13 H13A . 0.9900 ? C13 H13B . 0.9900 ? N14 C141 . 1.4216(16) ? N14 C15 . 1.4677(16) ? C15 C16 . 1.5128(18) ? C15 H15A . 0.9900 ? C15 H15B . 0.9900 ? C16 H16A . 0.9900 ? C16 H16B . 0.9900 ? C141 C146 . 1.3917(18) ? C141 C142 . 1.3963(19) ? C142 C143 . 1.380(2) ? C142 H142 . 0.9500 ? C143 C144 . 1.381(2) ? C143 H143 . 0.9500 ? C144 O144 . 1.3771(17) ? C144 C145 . 1.379(2) ? C145 C146 . 1.3870(19) ? C145 H145 . 0.9500 ? C146 H146 . 0.9500 ? O144 C147 . 1.406(2) ? C147 H17A . 0.9800 ? C147 H17B . 0.9800 ? C147 H17C . 0.9800 ? N21 C22 . 1.4874(18) ? N21 C26 . 1.4902(17) ? N21 H21 . 0.950(16) ? N21 H22 . 0.905(16) ? C22 C23 . 1.5144(18) ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? C23 N24 . 1.4706(16) ? C23 H23A . 0.9900 ? C23 H23B . 0.9900 ? N24 C241 . 1.4251(16) ? N24 C25 . 1.4646(16) ? C25 C26 . 1.5113(18) ? C25 H25A . 0.9900 ? C25 H25B . 0.9900 ? C26 H26A . 0.9900 ? C26 H26B . 0.9900 ? C241 C246 . 1.381(2) ? C241 C242 . 1.390(2) ? C242 C243 . 1.375(2) ? C242 H242 . 0.9500 ? C243 C244 . 1.377(2) ? C243 H243 . 0.9500 ? C244 C245 . 1.364(2) ? C244 O244 . 1.3784(17) ? C245 C246 . 1.394(2) ? C245 H245 . 0.9500 ? C246 H246 . 0.9500 ? O244 C247 . 1.411(2) ? C247 H27A . 0.9800 ? C247 H27B . 0.9800 ? C247 H27C . 0.9800 ? C31 C36 . 1.3852(19) ? C31 C32 . 1.391(2) ? C31 C37 . 1.5072(18) ? C32 C33 . 1.383(2) ? C32 H32 . 0.9500 ? C33 C34 . 1.385(2) ? C33 H33 . 0.9500 ? C34 C35 . 1.387(2) ? C34 C38 . 1.511(2) ? C35 C36 . 1.3865(19) ? C35 H35 . 0.9500 ? C36 H36 . 0.9500 ? C37 O32 . 1.2424(17) ? C37 O31 . 1.2678(17) ? C38 H38A . 0.9800 ? C38 H38B . 0.9800 ? C38 H38C . 0.9800 ? C41 C46 . 1.3885(19) ? C41 C42 . 1.390(2) ? C41 C47 . 1.5043(18) ? C42 C43 . 1.389(2) ? C42 H42 . 0.9500 ? C43 C44 . 1.382(2) ? C43 H43 . 0.9500 ? C44 C45 . 1.387(2) ? C44 C48 . 1.512(2) ? C45 C46 . 1.3876(19) ? C45 H45 . 0.9500 ? C46 H46 . 0.9500 ? C47 O42 . 1.2392(17) ? C47 O41 . 1.2705(18) ? C48 H48A . 0.9800 ? C48 H48B . 0.9800 ? C48 H48C . 0.9800 ? O51 H51 . 0.89(2) ? O51 H52 . 0.918(19) ? O61 H61 . 0.904(19) ? O61 H62 . 0.92(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 N11 H11 O31 . 0.946(16) 1.793(16) 2.7366(16) 174.5(13) y N11 H12 O61 2_766 0.917(15) 1.891(15) 2.7969(16) 169.2(13) y N21 H21 O41 . 0.949(16) 1.813(16) 2.7592(16) 174.1(14) y N21 H22 O51 2_766 0.904(15) 1.909(15) 2.8047(16) 170.9(13) y O51 H51 O41 1_565 0.89(2) 1.89(2) 2.7712(16) 170.0(18) y O51 H52 O32 . 0.918(18) 1.739(18) 2.6539(16) 174.3(15) y O61 H61 O42 . 0.906(19) 1.733(19) 2.6315(16) 171.2(15) y O61 H62 O31 . 0.92(2) 1.85(2) 2.7593(15) 169.1(19) y C22 H22B O41 2_656 0.99 2.56 3.5266(19) 167 y C142 H142 Cg1 2_766 0.95 2.83 3.5976(16) 138 y C146 H146 Cg2 2_666 0.95 2.73 3.5478(16) 145 y 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 C16 N11 C12 C13 . . . . -57.49(14) ? N11 C12 C13 N14 . . . . 56.22(15) ? C12 C13 N14 C141 . . . . 171.77(11) ? C12 C13 N14 C15 . . . . -55.02(15) ? C141 N14 C15 C16 . . . . -171.14(10) ? C13 N14 C15 C16 . . . . 55.58(14) ? C12 N11 C16 C15 . . . . 58.26(14) ? N14 C15 C16 N11 . . . . -57.35(14) ? C13 N14 C141 C146 . . . . 177.99(12) ? C15 N14 C141 C146 . . . . 46.58(16) ? C13 N14 C141 C142 . . . . -5.45(18) ? C15 N14 C141 C142 . . . . -136.85(14) ? C146 C141 C142 C143 . . . . 1.3(2) ? N14 C141 C142 C143 . . . . -175.37(14) ? C141 C142 C143 C144 . . . . -1.2(3) ? C142 C143 C144 O144 . . . . -179.29(15) ? C142 C143 C144 C145 . . . . 0.2(3) ? O144 C144 C145 C146 . . . . -179.99(15) ? C143 C144 C145 C146 . . . . 0.6(2) ? C144 C145 C146 C141 . . . . -0.4(2) ? C142 C141 C146 C145 . . . . -0.5(2) ? N14 C141 C146 C145 . . . . 176.20(13) ? C145 C144 O144 C147 . . . . -4.8(3) ? C143 C144 O144 C147 . . . . 174.67(17) ? C26 N21 C22 C23 . . . . -57.46(14) ? N21 C22 C23 N24 . . . . 56.44(15) ? C22 C23 N24 C241 . . . . 173.71(11) ? C22 C23 N24 C25 . . . . -55.59(14) ? C241 N24 C25 C26 . . . . -173.81(10) ? C23 N24 C25 C26 . . . . 56.30(13) ? C22 N21 C26 C25 . . . . 58.68(14) ? N24 C25 C26 N21 . . . . -58.38(14) ? C25 N24 C241 C246 . . . . 6.68(18) ? C23 N24 C241 C246 . . . . 135.22(14) ? C25 N24 C241 C242 . . . . -175.46(13) ? C23 N24 C241 C242 . . . . -46.92(17) ? C246 C241 C242 C243 . . . . -1.2(2) ? N24 C241 C242 C243 . . . . -179.21(15) ? C241 C242 C243 C244 . . . . -0.2(3) ? C242 C243 C244 C245 . . . . 1.7(3) ? C242 C243 C244 O244 . . . . -177.89(16) ? C243 C244 C245 C246 . . . . -1.6(3) ? O244 C244 C245 C246 . . . . 177.91(16) ? C242 C241 C246 C245 . . . . 1.3(2) ? N24 C241 C246 C245 . . . . 179.21(14) ? C244 C245 C246 C241 . . . . 0.1(3) ? C245 C244 O244 C247 . . . . 0.4(3) ? C243 C244 O244 C247 . . . . 179.97(18) ? C36 C31 C32 C33 . . . . 1.5(2) ? C37 C31 C32 C33 . . . . -177.47(13) ? C31 C32 C33 C34 . . . . -0.6(2) ? C32 C33 C34 C35 . . . . -1.2(2) ? C32 C33 C34 C38 . . . . 178.95(15) ? C33 C34 C35 C36 . . . . 2.1(2) ? C38 C34 C35 C36 . . . . -178.08(15) ? C32 C31 C36 C35 . . . . -0.7(2) ? C37 C31 C36 C35 . . . . 178.31(12) ? C34 C35 C36 C31 . . . . -1.1(2) ? C36 C31 C37 O32 . . . . 168.27(13) ? C32 C31 C37 O32 . . . . -12.75(19) ? C36 C31 C37 O31 . . . . -12.27(18) ? C32 C31 C37 O31 . . . . 166.71(13) ? C46 C41 C42 C43 . . . . 0.7(2) ? C47 C41 C42 C43 . . . . 179.74(13) ? C41 C42 C43 C44 . . . . -0.5(2) ? C42 C43 C44 C45 . . . . 0.2(2) ? C42 C43 C44 C48 . . . . 179.55(15) ? C43 C44 C45 C46 . . . . 0.0(2) ? C48 C44 C45 C46 . . . . -179.38(15) ? C44 C45 C46 C41 . . . . 0.2(2) ? C42 C41 C46 C45 . . . . -0.5(2) ? C47 C41 C46 C45 . . . . -179.56(12) ? C46 C41 C47 O42 . . . . 175.08(13) ? C42 C41 C47 O42 . . . . -3.96(19) ? C46 C41 C47 O41 . . . . -4.69(19) ? C42 C41 C47 O41 . . . . 176.28(12) ? _cod_database_fobs_code 2244152