#------------------------------------------------------------------------------ #$Date: 2022-07-27 03:06:56 +0100 (Wed, 27 Jul 2022) $ #$Revision: 276956 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244132.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_2244132 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-nitrophenyl)piperazin-1-ium benzoate monohydrate and 4-(4-nitrophenyl)piperazin-1-ium 2-carboxy-4,6-dinitrophenolate ; _journal_coeditor_code HB8030 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022007472 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C10 H14 N3 O2 +, C7 H3 N2 O7 -' _chemical_formula_moiety 'C10 H14 N3 O2 +, C7 H3 N2 O7 -' _chemical_formula_sum 'C17 H17 N5 O9' _chemical_formula_weight 435.35 _chemical_name_systematic ; 4-(4-Nitrophenyl)piperazin-1-ium 2-carboxy-4,6-dinitrophenolate ; _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 90.426(2) _cell_angle_beta 105.2730(10) _cell_angle_gamma 98.538(2) _cell_formula_units_Z 2 _cell_length_a 7.9599(4) _cell_length_b 8.5391(4) _cell_length_c 14.2227(5) _cell_measurement_reflns_used 4212 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.510 _cell_measurement_theta_min 2.415 _cell_volume 921.15(7) _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 90(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_unetI/netI 0.0243 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 38287 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.510 _diffrn_reflns_theta_min 2.415 _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 0.130 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.570 _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.276 _refine_diff_density_min -0.180 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 4212 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0293 _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^)+(0.0290P)^2^+0.3527P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.0772 _reflns_number_gt 3662 _reflns_number_total 4212 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8030sup1.cif _cod_data_source_block II _cod_database_code 2244132 _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 0.972 _shelx_estimated_absorpt_t_max 0.985 _shelx_hkl_file ; -3 0 0 3378.74 145.032 2 -3 0 0 3574.56 145.169 2 -3 0 0 3160.74 150.259 3 -3 0 0 3369.75 144.641 5 -3 0 0 3292.08 145.104 6 3 0 0 3595.67 145.629 6 3 0 0 3209.63 147.005 6 3 0 0 3326.88 143.842 5 3 0 0 3379.07 144.632 5 3 0 0 3485.20 145.274 2 3 0 0 3319.17 144.768 2 3 0 0 3278.81 146.414 3 -4 0 0 126.262 9.64250 2 -4 0 0 131.251 9.85724 5 -4 0 0 137.917 9.27211 5 -4 0 0 145.001 10.4509 6 -4 0 0 123.578 10.6541 3 -4 0 0 123.379 9.72368 6 4 0 0 124.436 9.85759 6 4 0 0 131.282 11.2681 3 4 0 0 122.796 9.46346 2 4 0 0 124.763 9.78105 2 4 0 0 128.836 9.73853 6 4 0 0 119.009 8.61579 5 4 0 0 131.904 9.56649 5 -5 0 0 10.2622 3.23889 2 -5 0 0 11.0945 3.63554 6 -5 0 0 2.22095 2.95374 6 -5 0 0 8.69754 3.68985 3 -5 0 0 8.20392 3.88385 5 -5 0 0 9.65760 2.99299 5 -5 0 0 4.94097 3.34040 2 5 0 0 4.92417 2.93669 5 5 0 0 5.89844 3.28633 6 5 0 0 7.66235 3.43243 6 5 0 0 14.9190 3.58456 5 5 0 0 10.6949 4.49834 3 5 0 0 7.15525 3.43347 2 5 0 0 16.2618 4.48636 2 -6 0 0 59.8209 7.98163 2 -6 0 0 64.0660 8.16971 2 -6 0 0 61.7926 8.28400 6 -6 0 0 63.8860 9.21762 3 -6 0 0 49.0977 7.83240 5 -6 0 0 61.3059 7.09978 5 -6 0 0 53.6478 7.33026 4 -6 0 0 52.6430 7.80230 6 6 0 0 62.0437 7.78851 5 6 0 0 61.5309 9.08245 2 6 0 0 66.1234 9.27466 3 6 0 0 42.9515 8.12198 2 6 0 0 58.0838 8.22072 6 6 0 0 56.0999 8.13101 6 -7 0 0 214.572 18.0280 6 -7 0 0 221.884 16.2601 4 -7 0 0 249.641 18.6520 2 -7 0 0 204.148 17.6885 2 -7 0 0 236.680 18.8046 6 7 0 0 195.624 17.9137 2 7 0 0 241.815 19.4299 6 7 0 0 224.368 16.7597 5 -8 0 0 13.2307 5.55069 2 -8 0 0 4.52173 4.86912 6 -8 0 0 -2.2305 3.46456 5 -8 0 0 4.46858 3.52332 4 -8 0 0 -0.0033 6.20417 6 -8 0 0 3.28531 6.32040 2 8 0 0 6.46389 6.38798 6 8 0 0 7.38132 6.01784 2 -9 0 0 72.6369 12.4321 4 -9 0 0 106.221 15.1080 2 -9 0 0 87.3119 14.0807 5 -9 0 0 67.0042 14.4579 6 -9 0 0 84.1493 14.7287 6 9 0 0 67.7190 12.8904 5 9 0 0 55.9242 13.9746 6 9 -1 0 22.8773 7.75073 2 9 -1 0 1.39516 7.59842 6 9 -1 0 12.7625 6.61528 5 -9 1 0 10.6975 8.38013 2 -9 1 0 8.53524 6.14239 4 -9 1 0 12.9805 7.97848 6 -9 1 0 3.52672 8.34028 6 -9 1 0 23.1072 8.47188 5 8 -1 0 5.56451 5.08061 5 8 -1 0 4.62231 4.80224 2 8 -1 0 3.97039 5.70306 6 -8 1 0 0.65355 5.15580 4 -8 1 0 6.14753 5.04594 2 -8 1 0 -4.4419 6.61609 6 -8 1 0 4.37167 5.14448 2 -8 1 0 3.42842 4.63854 6 -8 1 0 -2.0598 4.40305 5 7 -1 0 5.05013 4.38867 5 7 -1 0 1.77759 4.19608 2 7 -1 0 7.99146 4.67097 6 7 -1 0 1.14494 3.65096 5 -7 1 0 1.08382 3.18258 4 -7 1 0 8.02518 4.49985 6 -7 1 0 1.05295 3.40958 2 -7 1 0 5.24219 4.35516 2 -7 1 0 1.43944 3.96559 6 -7 1 0 -0.6302 3.50477 5 6 -1 0 547.835 30.3930 2 6 -1 0 480.193 28.4246 2 6 -1 0 545.336 28.6371 5 6 -1 0 487.373 31.4772 6 6 -1 0 508.935 26.7797 5 6 -1 0 513.968 30.3040 6 -6 1 0 498.008 30.0673 2 -6 1 0 503.037 30.3951 6 -6 1 0 500.161 28.3382 4 -6 1 0 460.965 30.4991 3 -6 1 0 543.664 28.9817 2 -6 1 0 501.229 27.9974 5 -6 1 0 530.174 28.6591 5 5 -1 0 746.845 39.0859 6 5 -1 0 807.482 37.3490 2 5 -1 0 756.823 35.9477 5 5 -1 0 864.766 39.2427 2 5 -1 0 742.254 37.3661 5 5 -1 0 719.535 37.6231 6 -5 1 0 761.985 39.9493 3 -5 1 0 772.716 36.8863 5 -5 1 0 606.547 37.4342 2 -5 1 0 763.541 37.5330 4 -5 1 0 736.597 37.5137 2 -5 1 0 718.796 38.8592 6 -5 1 0 701.784 37.6070 6 -5 1 0 730.213 37.2532 5 4 -1 0 63.0630 5.45450 5 4 -1 0 71.4647 6.94568 2 4 -1 0 64.5890 6.81360 6 4 -1 0 63.4309 6.38405 5 4 -1 0 57.4867 6.23740 2 4 -1 0 65.5488 6.43788 6 -4 1 0 70.8860 7.08828 6 -4 1 0 60.1836 6.59704 2 -4 1 0 59.5752 6.09804 5 -4 1 0 58.8286 6.06556 2 -4 1 0 60.4573 5.74895 5 -4 1 0 70.6814 7.61343 3 -4 1 0 56.0958 5.97779 4 -4 1 0 69.1534 6.62784 6 3 -1 0 1186.12 57.1949 6 3 -1 0 1317.05 55.8504 5 3 -1 0 1289.49 56.0400 5 3 -1 0 1307.10 57.4801 6 3 -1 0 1284.19 58.0404 2 3 -1 0 1191.66 56.9687 2 -3 1 0 1264.73 57.0552 5 -3 1 0 1313.62 59.2025 3 -3 1 0 1297.30 55.7188 5 -3 1 0 1233.17 57.0783 4 -3 1 0 1151.48 57.5592 2 -3 1 0 1246.95 57.2918 2 -3 1 0 1244.92 57.4750 6 -3 1 0 1318.19 56.9733 6 2 -1 0 2094.88 91.1958 2 2 -1 0 2006.70 90.0919 5 2 -1 0 1939.91 91.1875 6 2 -1 0 2101.25 88.3087 6 2 -1 0 2110.98 90.9126 4 2 -1 0 2015.33 91.5795 2 2 -1 0 1944.78 90.7946 5 -2 1 0 2103.13 88.0977 2 -2 1 0 2163.12 86.9056 4 -2 1 0 2122.16 90.5850 5 -2 1 0 2013.00 91.1888 2 -2 1 0 2090.38 88.7233 3 -2 1 0 2137.59 87.1511 6 -2 1 0 1924.91 90.7036 5 -2 1 0 2136.50 87.5751 6 1 -1 0 1198.71 57.8863 6 1 -1 0 1210.57 57.5421 4 1 -1 0 1297.89 57.3862 5 1 -1 0 1421.63 55.1517 6 1 -1 0 1312.76 55.0253 2 1 -1 0 1301.19 57.0449 5 1 -1 0 1347.43 58.1987 2 -1 1 0 1273.34 57.9123 2 -1 1 0 1259.65 58.0273 2 -1 1 0 1312.70 55.5400 6 -1 1 0 1300.99 55.2589 4 -1 1 0 1298.55 54.6870 5 -1 1 0 1293.32 55.6886 6 0 -1 0 2222.75 97.6744 2 0 -1 0 2120.83 97.0663 5 0 1 0 2242.75 95.6133 3 0 1 0 2372.06 94.2551 6 -1 -1 0 3431.67 151.635 1 1 1 0 3529.91 152.259 1 -3 -1 0 2575.55 109.145 5 -3 -1 0 2661.27 109.257 2 -3 -1 0 2434.27 111.515 2 -3 -1 0 2459.04 110.363 3 -3 -1 0 2539.00 109.368 6 -3 -1 0 2585.38 109.974 6 3 1 0 2443.36 111.725 6 3 1 0 2453.22 110.341 5 3 1 0 2507.09 109.353 6 3 1 0 2513.95 108.643 5 3 1 0 2455.97 110.685 2 3 1 0 2608.68 109.246 2 3 1 0 2325.75 112.050 3 -4 -1 0 254.064 16.2924 5 -4 -1 0 256.575 16.7663 6 -4 -1 0 268.668 16.2145 2 -4 -1 0 255.132 16.4849 2 -4 -1 0 250.884 16.4045 6 -4 -1 0 274.714 17.7261 3 -4 -1 0 273.541 15.3464 5 4 1 0 271.249 16.9112 6 4 1 0 261.304 15.8398 5 4 1 0 300.927 17.0921 6 4 1 0 273.186 15.6176 5 4 1 0 273.502 16.4174 2 4 1 0 258.936 16.5196 2 4 1 0 256.639 17.4276 3 -5 -1 0 155.162 11.8190 2 -5 -1 0 141.418 12.0943 2 -5 -1 0 130.910 11.7026 5 -5 -1 0 143.638 10.9906 5 -5 -1 0 155.188 13.2512 3 -5 -1 0 155.616 12.2266 6 -5 -1 0 144.547 12.4669 6 5 1 0 141.025 11.3189 5 5 1 0 159.045 13.4141 3 5 1 0 150.638 12.0393 6 5 1 0 129.111 11.6428 2 5 1 0 143.918 12.0468 2 5 1 0 147.719 11.2698 5 5 1 0 135.549 12.1937 6 -6 -1 0 349.717 22.0416 6 -6 -1 0 307.268 20.4842 6 -6 -1 0 294.893 18.6676 5 -6 -1 0 270.016 20.0363 5 -6 -1 0 281.762 21.6168 3 -6 -1 0 281.977 20.9898 2 -6 -1 0 314.238 20.3001 2 6 1 0 306.780 20.4047 2 6 1 0 285.378 18.8563 5 6 1 0 296.543 22.1282 3 6 1 0 271.818 20.4537 6 6 1 0 328.321 19.7463 5 6 1 0 276.486 20.2005 2 -7 -1 0 45.0616 9.37469 6 -7 -1 0 28.2188 7.57606 2 -7 -1 0 21.7992 6.71808 6 -7 -1 0 28.3437 6.15544 5 -7 -1 0 31.2864 7.06331 2 7 1 0 31.1035 7.42363 6 7 1 0 29.4893 6.43888 5 7 1 0 32.7435 7.12137 2 7 1 0 22.3514 6.76582 3 -8 -1 0 196.928 23.0358 6 -8 -1 0 171.603 17.6051 6 -8 -1 0 185.898 15.8148 5 -8 -1 0 181.738 15.4988 4 -8 -1 0 191.400 17.7007 2 8 1 0 187.723 20.1112 3 8 1 0 168.245 17.6674 2 8 1 0 171.066 17.8871 6 8 1 0 173.138 15.5840 5 -9 -1 0 5.72798 5.20277 5 -9 -1 0 -1.1513 6.03819 6 -9 -1 0 4.89251 6.22066 4 -9 -1 0 19.9115 7.68142 2 9 1 0 -0.4363 7.55057 3 9 1 0 -10.129 7.50388 2 9 1 0 9.03295 7.60173 6 9 1 0 -1.7776 6.82759 5 9 -2 0 237.508 24.3661 2 9 -2 0 282.607 26.4358 6 9 -2 0 290.812 21.9861 5 -9 2 0 292.011 26.0424 6 -9 2 0 322.630 24.2739 5 -9 2 0 249.265 22.2030 4 -9 2 0 255.653 24.1502 6 8 -2 0 -5.9156 5.79305 2 8 -2 0 -1.1000 4.83732 5 8 -2 0 9.50433 7.20668 6 -8 2 0 11.7189 6.58745 2 -8 2 0 -8.8298 6.05672 6 -8 2 0 4.90626 4.64697 4 -8 2 0 10.5451 5.93452 5 -8 2 0 12.3780 6.79030 6 -8 2 0 2.56063 4.82182 2 7 -2 0 44.6613 9.49190 6 7 -2 0 23.7791 5.62415 5 7 -2 0 38.4554 7.26243 5 7 -2 0 27.7480 7.89719 2 -7 2 0 33.3944 8.43852 6 -7 2 0 40.7245 8.85100 2 -7 2 0 27.0730 6.44433 6 -7 2 0 45.6440 7.94305 5 -7 2 0 30.3509 6.75880 2 -7 2 0 34.5460 7.15511 4 6 -2 0 307.908 21.1801 2 6 -2 0 291.214 18.6690 2 6 -2 0 274.865 20.6171 6 6 -2 0 217.714 17.8994 6 6 -2 0 283.807 16.7827 5 6 -2 0 270.232 18.2749 5 -6 2 0 341.055 19.9132 4 -6 2 0 290.418 18.5294 5 -6 2 0 262.964 20.3712 3 -6 2 0 238.498 18.2733 6 -6 2 0 324.699 21.5139 6 -6 2 0 258.128 19.8358 2 -6 2 0 260.532 18.3330 2 -6 2 0 285.761 18.7889 5 5 -2 0 40.8933 6.10419 5 5 -2 0 38.8903 6.13669 6 5 -2 0 32.9139 6.32713 6 5 -2 0 37.1927 5.60642 2 5 -2 0 32.7486 6.06974 2 -5 2 0 42.1488 6.38974 5 -5 2 0 41.4134 6.17297 2 -5 2 0 41.5273 6.16765 4 -5 2 0 31.0518 5.09772 5 -5 2 0 26.9391 5.16291 2 -5 2 0 24.6480 5.95314 3 -5 2 0 38.7622 5.66534 6 -5 2 0 37.1832 6.28024 6 4 -2 0 509.405 28.2393 6 4 -2 0 551.959 26.4979 5 4 -2 0 490.283 26.4688 6 4 -2 0 483.437 24.5291 5 4 -2 0 514.080 26.2084 2 4 -2 0 496.143 27.8092 2 -4 2 0 512.000 26.7694 6 -4 2 0 500.722 26.5336 2 -4 2 0 513.894 25.8990 5 -4 2 0 551.932 26.4060 5 -4 2 0 518.343 28.3016 3 -4 2 0 471.093 27.4336 2 -4 2 0 484.250 30.4851 6 -4 2 0 459.331 28.3787 4 3 -2 0 222.986 10.9055 5 3 -2 0 198.274 11.8597 5 3 -2 0 210.178 12.2097 2 3 -2 0 204.273 13.7969 6 3 -2 0 180.519 12.5752 2 3 -2 0 178.962 12.7279 6 -3 2 0 179.917 11.9951 4 -3 2 0 170.831 11.4348 5 -3 2 0 179.109 11.2244 5 -3 2 0 178.303 11.7577 2 -3 2 0 191.320 12.7716 2 -3 2 0 200.229 12.3285 6 -3 2 0 170.072 12.5945 6 2 -2 0 66.0289 5.68933 4 2 -2 0 73.1713 6.43069 2 2 -2 0 51.5853 5.33485 2 2 -2 0 75.4973 6.46933 6 2 -2 0 61.5629 5.26310 5 2 -2 0 65.8101 5.89316 6 2 -2 0 70.8695 4.90656 5 -2 2 0 62.7142 5.72111 2 -2 2 0 67.2562 5.95118 6 -2 2 0 70.7067 5.49524 5 -2 2 0 64.4567 5.82228 4 -2 2 0 60.7309 6.02661 2 -2 2 0 70.6445 6.52073 6 -2 2 0 66.1670 5.31479 5 1 -2 0 3677.17 145.093 2 1 -2 0 3040.65 145.810 5 1 -2 0 3423.43 146.287 5 1 -2 0 3076.51 146.827 4 1 -2 0 3306.53 147.839 6 1 -2 0 3391.37 148.162 6 1 -2 0 3625.26 147.908 2 -1 2 0 3451.47 147.757 2 -1 2 0 3325.58 148.138 6 -1 2 0 3363.67 147.916 6 -1 2 0 3635.66 146.864 5 -1 2 0 3677.08 148.292 2 -1 2 0 3358.97 146.370 5 0 -2 0 1336.68 60.8986 6 0 -2 0 1384.36 59.7135 4 0 -2 0 1284.47 60.6531 2 0 -2 0 1380.28 60.7693 3 0 -2 0 1377.32 59.0779 5 0 -2 0 1388.44 60.4037 6 0 -2 0 1296.16 59.6305 5 0 -2 0 1377.15 60.0884 2 0 2 0 1389.56 59.9882 5 0 2 0 1330.54 60.7225 2 0 2 0 1289.97 60.8072 6 0 2 0 1239.63 59.0870 5 0 2 0 1339.51 61.0027 6 0 2 0 1391.66 58.7675 4 0 2 0 1207.23 60.3818 2 0 2 0 1423.14 59.2596 3 -1 -2 0 6623.84 302.433 1 1 2 0 7194.23 297.763 1 -2 -2 0 751.601 35.7048 6 -2 -2 0 789.979 36.5840 3 -2 -2 0 701.525 36.6096 2 -2 -2 0 737.468 35.8105 5 -2 -2 0 732.525 34.8416 5 -2 -2 0 746.142 35.7040 4 -2 -2 0 816.500 35.7980 2 -2 -2 0 754.008 36.5359 6 2 2 0 768.110 35.8547 6 2 2 0 735.151 36.7513 6 2 2 0 652.052 36.2670 2 2 2 0 737.596 35.4135 2 2 2 0 747.923 36.0279 3 2 2 0 749.016 35.0264 5 2 2 0 718.487 35.2672 5 -3 -2 0 4311.75 177.070 2 -3 -2 0 4203.49 176.928 6 -3 -2 0 4062.31 175.811 4 -3 -2 0 3760.20 174.956 5 -3 -2 0 4308.81 175.364 2 -3 -2 0 3921.18 175.198 6 -3 -2 0 4111.46 176.752 3 -3 -2 0 4047.72 175.162 5 3 2 0 4233.97 174.958 5 3 2 0 3633.70 175.333 5 3 2 0 3951.89 175.032 2 3 2 0 4272.46 176.577 3 3 2 0 3675.37 177.052 2 3 2 0 4096.56 175.538 6 -4 -2 0 896.851 46.5531 3 -4 -2 0 874.830 45.3034 5 -4 -2 0 972.774 46.1972 4 -4 -2 0 890.603 46.3868 6 -4 -2 0 972.121 45.5778 6 -4 -2 0 814.898 45.6362 2 -4 -2 0 975.469 45.1634 2 4 2 0 931.631 46.5473 3 4 2 0 987.129 44.7960 5 4 2 0 882.335 45.8976 2 4 2 0 944.509 45.4396 6 4 2 0 875.531 46.4472 6 4 2 0 941.254 44.3664 5 -5 -2 0 15.6275 3.84922 5 -5 -2 0 12.0681 5.75478 5 -5 -2 0 18.2392 4.62491 6 -5 -2 0 18.0129 5.16081 6 -5 -2 0 12.7430 4.57230 2 -5 -2 0 13.6346 4.20081 2 5 2 0 13.2413 4.88820 6 5 2 0 21.8647 5.45850 5 5 2 0 20.6861 6.18576 3 5 2 0 14.5105 4.92098 2 5 2 0 18.4880 4.52271 2 5 2 0 20.8178 4.86581 5 5 2 0 13.8715 5.05501 6 -6 -2 0 3.97131 4.48956 6 -6 -2 0 9.53152 5.73427 2 -6 -2 0 -3.2131 1.98991 5 -6 -2 0 0.50920 3.37942 6 -6 -2 0 -0.2580 2.49517 2 6 2 0 9.79959 4.49768 5 6 2 0 5.42655 4.07401 3 6 2 0 2.55157 4.48507 2 6 2 0 3.07586 3.50628 6 6 2 0 1.04685 3.56340 2 -7 -2 0 127.821 13.8694 6 -7 -2 0 132.282 15.8757 2 -7 -2 0 140.333 16.0792 6 -7 -2 0 140.754 12.9446 5 7 2 0 128.922 14.1961 6 7 2 0 126.163 13.5581 2 7 2 0 146.835 15.4170 5 7 2 0 143.235 15.9711 3 -8 -2 0 70.5807 10.3041 5 -8 -2 0 45.3077 11.9225 6 -8 -2 0 72.4218 11.2841 2 -8 -2 0 55.2654 11.1208 6 8 2 0 69.3611 11.4131 6 8 2 0 48.8168 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506.357 30.0406 4 -2 6 -3 444.723 28.9795 6 -2 6 -3 441.724 28.5490 2 -2 6 -3 461.298 27.9072 2 -2 6 -3 450.764 30.9245 3 2 -6 3 393.686 32.1993 6 2 -6 3 418.296 27.6849 6 2 -6 3 425.573 27.7989 2 2 -6 3 454.188 27.1446 2 2 -6 3 470.593 27.7605 4 2 -6 3 455.406 20.1864 5 2 -6 3 464.261 20.0933 5 -3 6 -3 116.081 11.0017 5 -3 6 -3 112.652 13.4425 4 -3 6 -3 135.853 15.1816 3 -3 6 -3 100.696 11.5683 2 -3 6 -3 119.458 13.3380 6 -3 6 -3 108.355 11.3384 6 -3 6 -3 138.479 12.3487 5 3 -6 3 94.4086 12.3907 2 3 -6 3 121.019 11.7750 6 3 -6 3 105.342 11.3651 2 3 -6 3 124.452 11.9670 4 -4 6 -3 114.910 11.6249 5 -4 6 -3 110.191 11.8289 2 -4 6 -3 119.530 13.4285 6 -4 6 -3 107.631 13.5251 2 -4 6 -3 111.127 13.4087 4 -4 6 -3 104.070 11.0950 6 4 -6 3 88.4378 12.1461 6 4 -6 3 103.658 13.5902 2 -5 6 -3 347.960 24.0951 5 -5 6 -3 402.475 28.3646 6 -5 6 -3 352.812 24.4432 5 -5 6 -3 375.641 23.7761 6 -5 6 -3 348.489 27.0266 4 -5 6 -3 346.552 26.6509 2 -5 6 -3 351.353 23.7150 2 5 -6 3 361.724 27.3194 6 5 -6 3 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-6 -11 126.293 17.2260 2 3 -6 -11 118.546 18.2861 6 3 -6 -11 125.449 18.8578 6 3 -6 -11 99.4827 14.0614 5 -3 6 11 149.678 18.6643 2 -3 6 11 119.071 6.72988 3 -3 6 11 141.173 13.2924 5 -3 6 11 113.075 12.3354 5 -3 6 11 134.882 18.5139 6 -3 6 11 114.539 6.68086 3 2 -6 -11 -10.412 8.99912 2 2 -6 -11 0.60629 5.94466 5 2 -6 -11 3.91874 6.43935 6 2 -6 -11 6.22944 6.64183 2 2 -6 -11 8.02491 9.28710 6 -2 6 11 12.3616 6.79838 4 -2 6 11 0.01391 5.46897 5 -2 6 11 -3.6305 6.12219 2 -2 6 11 0.10753 4.29830 5 -2 6 11 -1.0179 6.52279 6 1 -6 -11 250.875 21.6389 5 1 -6 -11 274.465 30.3060 6 1 -6 -11 244.615 27.1963 2 1 -6 -11 248.649 24.7441 6 1 -6 -11 218.145 22.5839 2 -1 6 11 252.942 17.3470 5 -1 6 11 243.299 20.1623 5 -1 6 11 234.570 25.3160 6 -1 6 11 228.158 23.9068 2 0 -6 -11 346.566 25.7044 5 0 -6 -11 333.753 29.4875 2 0 -6 -11 309.403 27.5533 6 0 -6 -11 363.000 27.9798 2 0 -6 -11 275.884 28.6627 6 0 6 11 334.450 27.1699 2 0 6 11 330.466 20.6350 5 0 6 11 359.497 28.3735 6 -1 -6 -11 -3.1229 10.3854 2 -1 -6 -11 5.20758 5.65289 5 -1 -6 -11 -2.2600 10.1053 6 -1 -6 -11 2.17728 7.06493 2 -1 -6 -11 4.04111 7.67266 6 1 6 11 -6.1288 7.59542 6 1 6 11 9.53468 4.89538 5 1 6 11 -0.0963 3.55960 3 1 6 11 15.4505 8.31033 2 -2 -6 -11 142.830 17.5057 6 -2 -6 -11 97.8830 14.7633 2 -2 -6 -11 118.387 14.6983 5 -2 -6 -11 79.6320 19.4494 6 -2 -6 -11 103.913 12.5645 3 2 6 11 106.575 15.3767 2 2 6 11 110.438 15.7417 6 2 6 11 107.950 10.4698 5 -3 -6 -11 97.8403 13.4961 5 -3 -6 -11 88.1030 14.4606 2 -3 -6 -11 106.701 15.4382 6 3 6 11 102.677 16.7331 2 3 6 11 92.0948 16.9821 6 7 -7 -11 91.1352 15.7104 5 7 -7 -11 88.8049 20.0482 6 -7 7 11 88.1868 17.8591 2 -7 7 11 108.019 14.6468 4 -7 7 11 77.9964 16.5416 5 6 -7 -11 14.0651 9.55383 5 6 -7 -11 8.15520 10.8531 6 6 -7 -11 12.4692 10.3599 2 6 -7 -11 22.5184 11.1510 6 -6 7 11 15.8821 7.60229 4 -6 7 11 -2.9535 7.18140 5 -6 7 11 12.7839 11.8748 2 -6 7 11 21.5384 8.13488 3 -6 7 11 27.0818 13.0156 6 5 -7 -11 180.677 20.1980 5 5 -7 -11 206.240 24.2301 2 5 -7 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3 -6 8 11 120.304 16.8818 4 -6 8 11 123.722 25.5376 6 -6 8 11 125.625 23.0670 2 -6 8 11 114.258 20.0705 5 5 -8 -11 399.170 36.0842 6 5 -8 -11 332.398 27.6132 5 5 -8 -11 322.219 32.7724 2 -5 8 11 323.303 33.1885 2 -5 8 11 326.632 28.0209 4 -5 8 11 317.568 38.2471 6 -5 8 11 316.603 22.3361 3 -5 8 11 329.113 27.0583 5 4 -8 -11 41.3412 13.5099 6 4 -8 -11 27.0623 17.7815 6 4 -8 -11 33.2105 13.8774 2 -4 8 11 32.0816 12.9340 6 -4 8 11 35.9453 11.2212 4 -4 8 11 30.7995 11.9409 2 -4 8 11 29.1755 7.38153 3 -4 8 11 39.5876 10.0535 5 3 -8 -11 1100.39 61.1098 5 3 -8 -11 934.105 60.3217 6 3 -8 -11 916.462 60.8572 6 -3 8 11 815.115 47.9894 3 -3 8 11 904.640 43.6673 3 -3 8 11 1013.91 61.4819 6 2 -8 -11 3.60418 8.81334 5 2 -8 -11 1.65685 8.01766 2 2 -8 -11 0.70989 10.4236 6 -2 8 11 7.86452 3.52679 3 -2 8 11 -12.627 7.31391 5 -2 8 11 -6.5236 6.67234 4 -2 8 11 -6.4974 8.08187 2 -2 8 11 2.10838 9.02550 6 1 -8 -11 -16.720 9.19946 6 1 -8 -11 19.6647 19.1245 6 -1 8 11 6.51018 6.51954 5 -1 8 11 -2.0705 3.59983 3 -1 8 11 -5.2810 9.12211 6 -1 8 11 12.0182 9.89952 2 0 -8 -11 38.1566 11.2575 5 0 -8 -11 23.9706 14.5190 6 0 -8 -11 41.9492 12.5107 2 0 8 11 47.2474 14.7868 6 0 8 11 58.3829 10.2216 5 0 8 11 53.5176 16.2002 2 3 8 -12 153.491 13.3900 6 3 8 -12 169.114 17.3115 5 3 8 -12 108.567 19.7067 3 3 8 -12 159.991 15.3891 4 3 8 -12 167.949 13.6748 2 3 8 -12 149.719 18.6604 6 2 8 -12 24.0371 8.52547 6 2 8 -12 28.4248 5.46141 2 2 8 -12 26.3723 8.63320 4 2 8 -12 30.9617 8.30334 5 2 8 -12 13.7958 7.78096 2 2 8 -12 25.7904 5.25707 6 2 8 -12 21.2872 11.5789 3 1 8 -12 16.2832 4.00863 6 1 8 -12 14.4120 10.4830 3 1 8 -12 6.04616 9.47905 4 1 8 -12 14.1892 6.07004 2 1 8 -12 15.3585 3.86194 2 1 8 -12 11.7011 6.12920 6 0 8 -12 203.189 12.1662 2 0 8 -12 231.587 24.7153 3 0 8 -12 212.918 13.7222 2 0 8 -12 213.523 11.9645 6 0 8 -12 184.568 20.6699 4 0 8 -12 227.883 19.1982 5 -1 8 -12 -2.0352 6.24116 4 -1 8 -12 -1.6174 8.39949 3 -1 8 -12 -11.579 6.67593 5 5 7 -12 -10.493 7.27092 3 5 7 -12 3.98830 5.05280 6 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5.75368 6 4 4 -12 18.0561 5.21575 5 4 4 -12 24.8289 5.10086 2 -4 -4 12 9.59072 5.59956 6 -4 -4 12 38.2734 6.58512 2 3 4 -12 207.848 14.8137 6 3 4 -12 186.317 10.6219 4 3 4 -12 219.164 13.3355 2 3 4 -12 213.134 18.0949 3 3 4 -12 202.629 13.8083 5 3 4 -12 180.018 13.9972 6 3 4 -12 187.865 13.6943 2 3 4 -12 220.145 12.6498 5 -3 -4 12 196.594 13.0898 6 -3 -4 12 208.112 12.9067 2 -3 -4 12 186.595 13.3870 2 2 4 -12 234.795 19.2587 3 2 4 -12 215.548 14.8522 4 2 4 -12 227.361 13.7043 5 2 4 -12 227.218 12.3369 6 2 4 -12 225.104 12.4422 5 2 4 -12 217.841 13.0541 2 2 4 -12 231.356 12.4583 2 2 4 -12 235.967 13.0346 6 1 4 -12 10.2180 4.63208 4 1 4 -12 21.0502 2.93838 5 1 4 -12 14.0519 5.72484 3 0 4 -12 349.889 26.3516 3 0 4 -12 355.532 23.0657 4 -1 4 -12 205.082 17.1914 4 -1 4 -12 223.729 20.1577 3 -2 4 -12 265.125 20.9366 4 -2 4 -12 288.435 13.5515 5 -2 4 -12 289.303 24.5772 3 -2 4 -12 306.900 14.2229 5 -3 4 -12 7.74431 5.96141 4 -3 4 -12 5.72063 3.43118 5 -3 4 -12 2.60527 7.30466 3 -4 4 -12 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-17 7.10320 5.82344 3 4 3 -17 8.59030 3.49585 2 4 3 -17 8.82907 3.49889 2 4 3 -17 1.65901 2.96163 6 3 3 -17 28.8796 5.78617 5 3 3 -17 37.3133 7.90073 3 2 3 -17 11.1887 5.43222 3 2 3 -17 -0.2176 3.71388 5 1 3 -17 95.5791 10.9038 4 1 3 -17 108.753 7.07846 5 1 3 -17 116.515 12.3525 3 0 3 -17 66.6833 11.3457 4 5 2 -17 4.11479 4.78856 2 5 2 -17 11.5272 5.33828 3 5 2 -17 -5.2519 5.16130 6 5 2 -17 6.95094 4.87227 6 5 2 -17 6.40825 5.13558 2 5 2 -17 5.61320 5.92426 5 4 2 -17 399.206 24.8404 3 4 2 -17 395.540 23.1146 2 4 2 -17 398.764 22.6916 6 4 2 -17 407.831 20.3140 6 4 2 -17 393.020 23.8029 5 4 2 -17 346.777 24.6199 5 3 2 -17 253.779 17.8565 5 3 2 -17 263.858 17.8015 3 3 2 -17 255.551 16.3528 5 2 2 -17 494.537 27.7155 4 2 2 -17 470.760 27.0445 5 2 2 -17 504.863 25.2378 5 2 2 -17 515.747 26.8427 4 2 2 -17 494.069 27.6693 3 1 2 -17 19.5988 5.70427 4 1 2 -17 15.1409 5.68343 5 1 2 -17 10.7544 4.06056 5 1 2 -17 10.3786 8.00463 4 1 2 -17 14.9140 5.84469 3 0 2 -17 -4.6619 4.57163 3 0 2 -17 -1.0452 3.33424 5 0 2 -17 -11.887 4.76575 4 -1 2 -17 22.4328 6.75454 3 -1 2 -17 19.2649 6.56955 4 6 1 -17 181.791 14.9964 6 6 1 -17 197.528 16.5732 5 6 1 -17 160.002 16.1896 3 6 1 -17 175.567 20.2720 6 5 1 -17 7.57027 5.40523 5 5 1 -17 4.76478 4.00485 2 5 1 -17 0.59763 4.31298 6 5 1 -17 16.4334 6.19225 6 5 1 -17 2.16296 5.09107 3 5 1 -17 -5.1245 5.47617 2 4 1 -17 175.957 13.6953 5 4 1 -17 160.820 14.1787 2 4 1 -17 182.875 15.9914 5 4 1 -17 159.149 12.9751 3 4 1 -17 161.064 14.0518 6 4 1 -17 165.571 11.3338 2 4 1 -17 156.878 11.8229 6 3 1 -17 62.2058 6.88407 3 3 1 -17 59.3098 7.46828 4 3 1 -17 53.5822 8.69555 5 3 1 -17 59.0347 5.58933 2 3 1 -17 62.4933 9.70753 5 3 1 -17 63.2369 5.51263 6 3 1 -17 51.9892 6.02358 4 2 1 -17 154.485 14.7658 4 2 1 -17 172.092 12.7478 5 2 1 -17 156.986 14.3790 5 2 1 -17 170.324 12.8139 4 2 1 -17 164.623 10.4940 3 1 1 -17 88.1821 13.1572 4 1 1 -17 42.8313 5.56681 3 1 1 -17 48.0309 7.02529 5 1 1 -17 42.9438 8.38593 5 1 1 -17 42.8673 7.55816 4 1 1 -17 37.8532 5.99373 3 0 1 -17 32.4903 6.22591 4 0 1 -17 31.0306 5.56585 3 0 1 -17 34.6039 6.12582 5 -1 1 -17 284.303 20.7031 4 -1 1 -17 286.862 20.3766 3 -1 1 -17 320.054 18.2091 5 6 0 -17 25.0041 9.91356 6 6 0 -17 22.0093 8.23118 5 6 0 -17 24.3957 6.84346 3 6 0 -17 31.1799 7.67546 6 5 0 -17 2.34714 5.80590 2 5 0 -17 10.2051 4.27703 2 5 0 -17 6.06605 6.11050 5 5 0 -17 5.29371 5.88967 6 5 0 -17 2.32061 4.17484 3 4 0 -17 109.700 9.62396 6 4 0 -17 119.740 12.9842 6 4 0 -17 115.644 9.81326 2 4 0 -17 104.549 13.6160 5 4 0 -17 114.767 13.3957 2 -4 0 17 106.925 13.3848 2 3 0 -17 110.906 8.83824 6 3 0 -17 129.443 11.7236 5 3 0 -17 115.142 9.01523 2 3 0 -17 126.430 11.1259 6 3 0 -17 124.308 11.8378 4 3 0 -17 120.415 11.0344 2 3 0 -17 110.798 9.90053 4 2 0 -17 50.4477 7.12231 4 2 0 -17 40.7364 5.39914 2 2 0 -17 37.1980 9.47343 4 2 0 -17 37.8425 4.65145 6 2 0 -17 41.5135 3.91602 6 2 0 -17 40.0017 9.27448 5 2 0 -17 38.1288 4.48678 2 2 0 -17 37.4984 7.31892 5 1 0 -17 138.243 15.9346 5 1 0 -17 134.720 13.4453 5 1 0 -17 157.952 12.3324 4 0 0 -17 2.30298 5.12580 4 0 0 -17 -2.5930 4.41378 5 -1 0 -17 412.194 26.0471 4 -1 0 -17 414.227 33.8287 5 6 -1 -17 304.220 24.5515 5 6 -1 -17 316.221 27.7336 6 6 -1 -17 288.882 24.0174 6 6 -1 -17 320.205 30.6395 2 5 -1 -17 82.1724 10.5745 6 5 -1 -17 66.9343 10.0527 2 5 -1 -17 62.7272 11.0888 5 5 -1 -17 86.2032 13.7805 2 4 -1 -17 8.98842 6.21878 6 4 -1 -17 -4.4358 5.23762 2 4 -1 -17 7.91008 5.10447 5 4 -1 -17 5.28604 2.71786 4 4 -1 -17 3.35035 4.12293 4 4 -1 -17 3.20123 3.66789 2 -4 1 17 3.01889 9.97932 6 -4 1 17 -2.6198 7.78492 2 3 -1 -17 66.0522 10.1026 6 3 -1 -17 71.1434 11.3664 4 3 -1 -17 66.7379 7.89497 6 3 -1 -17 58.2199 9.75852 5 3 -1 -17 73.3431 8.20706 2 3 -1 -17 74.4668 10.2324 2 -3 1 17 59.2737 10.3133 6 2 -1 -17 10.4140 8.61414 5 2 -1 -17 3.41481 8.38687 4 2 -1 -17 3.88441 3.56448 2 2 -1 -17 3.08388 3.28339 6 2 -1 -17 2.12153 3.89074 6 2 -1 -17 -2.8907 4.90952 5 2 -1 -17 0.55191 3.69305 2 -2 1 17 1.61582 4.10922 2 1 -1 -17 57.9014 10.1362 5 1 -1 -17 61.1837 7.02095 2 1 -1 -17 57.5283 6.61239 6 1 -1 -17 55.1299 6.74443 2 1 -1 -17 47.5149 11.6180 5 1 -1 -17 59.3500 6.69806 6 0 -1 -17 19.1336 3.55108 6 0 -1 -17 24.0021 6.72703 5 0 -1 -17 15.6963 4.48901 6 0 -1 -17 15.6814 3.40247 2 -1 -1 -17 50.3443 6.07813 2 -1 -1 -17 48.6919 5.75805 6 -1 -1 -17 54.6708 7.33575 2 6 -2 -17 16.4337 7.77409 5 6 -2 -17 14.1951 9.93707 2 6 -2 -17 21.7439 8.72274 6 5 -2 -17 84.7690 15.1815 5 5 -2 -17 116.594 15.3026 2 5 -2 -17 98.6583 14.9364 6 5 -2 -17 90.8046 12.0009 6 4 -2 -17 66.6273 11.8808 2 4 -2 -17 55.4498 10.1818 5 4 -2 -17 55.2329 9.32306 6 4 -2 -17 57.8699 9.29146 2 4 -2 -17 52.5284 12.2952 6 4 -2 -17 59.9999 9.92346 4 -4 2 17 48.8815 12.9452 2 3 -2 -17 228.448 17.5617 6 3 -2 -17 231.193 19.7565 6 3 -2 -17 207.891 17.2352 2 3 -2 -17 236.791 19.3469 2 3 -2 -17 245.862 19.5683 5 -3 2 17 233.733 21.6355 6 -3 2 17 216.474 20.1749 2 2 -2 -17 182.043 15.9516 6 2 -2 -17 200.004 16.6211 6 2 -2 -17 190.542 18.9094 5 2 -2 -17 209.788 16.6752 2 2 -2 -17 203.650 15.1588 2 -2 2 17 167.429 19.7703 6 1 -2 -17 13.1864 5.61111 2 1 -2 -17 14.9066 6.14491 5 1 -2 -17 8.76869 5.92450 6 1 -2 -17 9.39653 4.58502 2 1 -2 -17 9.42811 4.68690 6 0 -2 -17 7.00866 3.90985 6 0 -2 -17 6.89392 3.48715 2 0 -2 -17 -11.516 5.34698 2 0 -2 -17 2.59602 5.33254 6 5 -3 -17 39.6925 10.0108 5 5 -3 -17 33.3503 11.5992 2 5 -3 -17 49.4621 11.3590 6 4 -3 -17 34.4902 10.0806 5 4 -3 -17 22.4666 10.0126 6 4 -3 -17 45.7977 9.14443 6 4 -3 -17 43.8448 10.0342 2 3 -3 -17 6.41179 6.43466 5 3 -3 -17 5.08908 5.53300 6 3 -3 -17 20.0679 10.9867 2 3 -3 -17 1.47678 6.68780 2 2 -3 -17 173.956 20.5325 2 2 -3 -17 203.605 17.8193 2 2 -3 -17 205.328 18.1923 6 2 -3 -17 200.385 18.5969 5 1 -3 -17 163.368 18.8648 6 1 -3 -17 182.991 16.2071 2 1 -3 -17 197.163 17.9180 5 1 -3 -17 188.685 16.1291 6 4 -4 -17 18.8615 11.5497 6 4 -4 -17 26.5004 9.81274 2 4 -4 -17 12.5886 9.53599 5 3 -4 -17 140.701 17.4374 2 3 -4 -17 159.591 17.6795 5 3 -4 -17 172.668 18.2810 6 2 -4 -17 239.404 21.8018 6 2 -4 -17 274.879 22.5849 2 2 -4 -17 275.099 22.3980 5 3 2 -18 19.6306 6.64491 3 3 2 -18 36.8643 6.75363 5 2 2 -18 6.10832 5.52180 4 2 2 -18 12.4117 5.35230 3 2 2 -18 3.33265 4.79702 5 1 2 -18 46.1254 8.21144 4 1 2 -18 49.4047 7.33285 3 4 1 -18 44.0446 5.75395 6 4 1 -18 50.5337 7.77219 3 4 1 -18 34.0673 7.08129 6 4 1 -18 50.8286 6.23590 2 4 1 -18 46.0180 7.95712 2 3 1 -18 32.9064 5.36845 4 3 1 -18 30.4586 6.18889 5 3 1 -18 33.2493 4.91279 3 2 1 -18 56.8142 9.25244 5 2 1 -18 63.4892 8.10299 4 1 1 -18 346.759 19.4185 5 1 1 -18 288.174 19.7899 4 4 0 -18 11.3377 6.67930 2 4 0 -18 9.17209 4.17960 6 4 0 -18 3.29679 5.49463 5 4 0 -18 13.7379 5.75189 6 4 0 -18 9.06965 4.19867 2 3 0 -18 94.7481 8.68056 2 3 0 -18 97.5290 8.61316 6 3 0 -18 90.1296 7.61803 2 3 0 -18 91.9335 11.1275 5 3 0 -18 92.4870 6.93784 6 2 0 -18 10.6487 5.26518 4 2 0 -18 21.6130 5.99186 5 1 0 -18 121.311 11.3678 4 1 0 -18 128.736 13.7707 5 4 -1 -18 122.505 17.4159 6 4 -1 -18 123.253 12.0197 6 4 -1 -18 125.713 15.7085 5 4 -1 -18 132.313 15.9897 2 4 -1 -18 117.623 8.56184 4 3 -1 -18 3.77925 4.09922 6 3 -1 -18 3.23534 6.98205 5 3 -1 -18 7.97767 4.68685 2 3 -1 -18 8.50962 5.61663 2 3 -1 -18 8.57524 5.90510 6 2 -1 -18 68.1393 9.10186 6 2 -1 -18 64.6435 7.55318 2 2 -1 -18 46.6064 7.93239 6 1 -1 -18 6.84832 3.54708 2 1 -1 -18 -1.8949 2.27882 6 1 -1 -18 1.06186 3.19100 2 4 -2 -18 79.5781 12.5876 6 4 -2 -18 77.7572 12.8077 5 4 -2 -18 94.9392 14.5002 2 3 -2 -18 303.483 22.3548 5 3 -2 -18 306.445 19.6277 6 3 -2 -18 315.665 22.3076 6 3 -2 -18 277.850 21.4348 2 2 -2 -18 90.1007 10.6727 6 2 -2 -18 81.3489 10.3208 2 2 -2 -18 90.4718 12.9758 5 2 -2 -18 88.5473 11.0236 6 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 56528 _shelx_res_file ; TITL hsy7 CELL 0.71073 7.9599 8.5391 14.2227 90.426 105.273 98.538 ZERR 2 0.0004 0.0004 0.0005 0.002 0.001 0.002 LATT 1 SFAC C H N O UNIT 34 34 10 18 TEMP -183 SIZE 0.22 0.18 0.12 OMIT -2 180.0 L.S. 20 ACTA BOND $H CONF HTAB LIST 4 FMAP 2 PLAN 20 WGHT 0.029000 0.352700 FVAR 1.35133 MOLE 1 N11 3 0.308831 0.103857 0.644052 11.00000 0.02304 0.01279 = 0.01455 -0.00027 0.00369 0.00398 H11 2 0.296729 0.183973 0.603988 11.00000 -1.20000 H12 2 0.279619 0.012945 0.605676 11.00000 -1.20000 C12 1 0.179152 0.103144 0.703397 11.00000 0.01775 0.01815 = 0.01982 -0.00333 0.00319 0.00374 AFIX 23 H12A 2 0.057929 0.073293 0.660768 11.00000 -1.20000 H12B 2 0.189046 0.210714 0.732785 11.00000 -1.20000 AFIX 0 C13 1 0.214035 -0.013890 0.783497 11.00000 0.01884 0.01914 = 0.01710 -0.00297 0.00514 -0.00083 AFIX 23 H13A 2 0.132145 -0.009185 0.824770 11.00000 -1.20000 H13B 2 0.193137 -0.122854 0.754076 11.00000 -1.20000 AFIX 0 N14 3 0.396249 0.024050 0.843555 11.00000 0.01842 0.01792 = 0.01424 -0.00175 0.00446 0.00154 C15 1 0.515613 0.004830 0.783253 11.00000 0.01947 0.01617 = 0.01589 -0.00122 0.00483 0.00449 AFIX 23 H15A 2 0.488413 -0.104343 0.753583 11.00000 -1.20000 H15B 2 0.638806 0.021470 0.824484 11.00000 -1.20000 AFIX 0 C16 1 0.496161 0.122990 0.703450 11.00000 0.01945 0.01574 = 0.01751 -0.00060 0.00656 0.00295 AFIX 23 H16A 2 0.533353 0.232191 0.732964 11.00000 -1.20000 H16B 2 0.572910 0.105473 0.661006 11.00000 -1.20000 AFIX 0 C141 1 0.442871 0.137098 0.919658 11.00000 0.02098 0.01318 = 0.01279 0.00281 0.00444 0.00319 C142 1 0.316386 0.183178 0.963228 11.00000 0.01631 0.02066 = 0.01765 0.00041 0.00299 0.00290 AFIX 43 H142 2 0.195465 0.140648 0.937005 11.00000 -1.20000 AFIX 0 C143 1 0.364981 0.288589 1.043002 11.00000 0.01915 0.01992 = 0.01729 0.00198 0.00633 0.00636 AFIX 43 H143 2 0.278309 0.317870 1.071662 11.00000 -1.20000 AFIX 0 C144 1 0.541374 0.351762 1.081256 11.00000 0.02180 0.01302 = 0.01326 0.00047 0.00394 0.00309 C145 1 0.668857 0.313624 1.038522 11.00000 0.01751 0.01676 = 0.01698 0.00148 0.00445 0.00121 AFIX 43 H145 2 0.788742 0.360085 1.063966 11.00000 -1.20000 AFIX 0 C146 1 0.620246 0.207935 0.958970 11.00000 0.01899 0.01756 = 0.01693 0.00113 0.00708 0.00312 AFIX 43 H146 2 0.707817 0.182053 0.929865 11.00000 -1.20000 AFIX 0 N144 3 0.592453 0.462902 1.164547 11.00000 0.02114 0.01500 = 0.01608 0.00126 0.00536 0.00329 O141 4 0.478593 0.492085 1.203787 11.00000 0.02405 0.02733 = 0.02293 -0.00614 0.00923 0.00576 O142 4 0.748047 0.524566 1.194104 11.00000 0.02129 0.02339 = 0.02297 -0.00566 0.00578 -0.00293 MOLE 2 C21 1 0.245321 0.436481 0.469513 11.00000 0.01883 0.01537 = 0.01616 -0.00035 0.00391 0.00135 C22 1 0.200942 0.593286 0.453553 11.00000 0.01827 0.01419 = 0.01716 -0.00169 0.00422 0.00144 C23 1 0.154717 0.650111 0.361608 11.00000 0.01558 0.01461 = 0.01871 -0.00005 0.00435 0.00238 AFIX 43 H23 2 0.130774 0.755656 0.353679 11.00000 -1.20000 AFIX 0 C24 1 0.142903 0.553949 0.280378 11.00000 0.01512 0.01889 = 0.01461 0.00113 0.00343 0.00178 C25 1 0.178068 0.400407 0.289983 11.00000 0.01430 0.01764 = 0.01744 -0.00416 0.00535 -0.00010 AFIX 43 H25 2 0.165646 0.333989 0.233912 11.00000 -1.20000 AFIX 0 C26 1 0.231340 0.345208 0.381989 11.00000 0.01641 0.01308 = 0.01962 -0.00128 0.00587 0.00244 O21 4 0.288976 0.386600 0.555802 11.00000 0.03942 0.01599 = 0.01512 0.00086 0.00436 0.00711 C27 1 0.209329 0.701604 0.537339 11.00000 0.02517 0.01581 = 0.01784 -0.00150 0.00508 0.00130 O271 4 0.164160 0.832524 0.525726 11.00000 0.03466 0.01532 = 0.02183 -0.00318 0.00460 0.00656 O272 4 0.268597 0.650932 0.625365 11.00000 0.05411 0.01775 = 0.01510 -0.00187 0.00514 0.00959 H272 2 0.288108 0.539641 0.614353 11.00000 -1.50000 N24 3 0.098238 0.617300 0.184206 11.00000 0.01405 0.02203 = 0.01681 0.00043 0.00428 0.00218 O241 4 0.084390 0.759797 0.179203 11.00000 0.02278 0.02064 = 0.02163 0.00496 0.00562 0.00537 O242 4 0.078729 0.528844 0.112419 11.00000 0.02243 0.02839 = 0.01507 -0.00383 0.00491 0.00225 N26 3 0.278417 0.186763 0.386887 11.00000 0.02075 0.01531 = 0.02086 -0.00074 0.00927 0.00313 O261 4 0.207185 0.092182 0.316727 11.00000 0.02666 0.01784 = 0.02851 -0.00865 0.00736 0.00232 O262 4 0.389984 0.153809 0.458786 11.00000 0.03288 0.02449 = 0.02256 0.00310 0.00610 0.01325 HKLF 4 REM hsy7 REM R1 = 0.0293 for 3662 Fo > 4sig(Fo) and 0.0363 for all 4212 data REM 289 parameters refined using 0 restraints END WGHT 0.0290 0.3527 REM Instructions for potential hydrogen bonds HTAB N11 O21 HTAB N11 O262 EQIV $1 x, y-1, z HTAB N11 O271_$1 EQIV $2 -x, -y, -z+1 HTAB C12 O261_$2 EQIV $3 -x+1, -y+1, -z+2 HTAB C12 O142_$3 HTAB C16 O141_$3 EQIV $4 -x+1, -y, -z+1 HTAB C16 O261_$4 EQIV $5 -x, -y+1, -z+1 HTAB C142 O241_$5 EQIV $6 x+1, y, z+1 HTAB C145 O242_$6 EQIV $7 -x+1, -y+1, -z+1 HTAB C146 O241_$7 HTAB O272 O21 REM Highest difference peak 0.276, deepest hole -0.180, 1-sigma level 0.038 Q1 1 0.4974 0.0596 0.7427 11.00000 0.05 0.28 Q2 1 0.1994 0.6368 0.4935 11.00000 0.05 0.27 Q3 1 0.2208 0.5205 0.4603 11.00000 0.05 0.26 Q4 1 0.5649 0.4000 1.1120 11.00000 0.05 0.25 Q5 1 0.1439 0.5963 0.3187 11.00000 0.05 0.23 Q6 1 0.2480 0.3867 0.4235 11.00000 0.05 0.23 Q7 1 0.5972 0.3344 1.0551 11.00000 0.05 0.22 Q8 1 0.1976 0.0423 0.7415 11.00000 0.05 0.22 Q9 1 0.1299 0.5857 0.2438 11.00000 0.05 0.22 Q10 1 0.4690 0.3030 1.0740 11.00000 0.05 0.21 Q11 1 0.5291 0.1759 0.9332 11.00000 0.05 0.21 Q12 1 0.1465 0.4797 0.2837 11.00000 0.05 0.21 Q13 1 0.4186 0.0900 0.8747 11.00000 0.05 0.19 Q14 1 0.6197 0.2832 0.9796 11.00000 0.05 0.19 Q15 1 0.2061 0.3748 0.3418 11.00000 0.05 0.19 Q16 1 0.2121 0.6248 0.4151 11.00000 0.05 0.19 Q17 1 0.3562 0.2405 1.0030 11.00000 0.05 0.18 Q18 1 0.3151 0.0106 0.8161 11.00000 0.05 0.17 Q19 1 0.3722 0.1431 0.9441 11.00000 0.05 0.17 Q20 1 0.2576 0.2826 0.3850 11.00000 0.05 0.17 ; _shelx_res_checksum 34436 _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 0.30883(12) 0.10386(11) 0.64405(7) 0.01693(19) Uani d 1 . . H H11 0.2967(17) 0.1840(17) 0.6040(10) 0.020 Uiso d 1 . . H H12 0.2796(17) 0.0129(17) 0.6057(10) 0.020 Uiso d 1 . . C C12 0.17915(14) 0.10314(13) 0.70340(8) 0.0188(2) Uani d 1 . . H H12A 0.0579 0.0733 0.6608 0.023 Uiso calc 1 . . H H12B 0.1890 0.2107 0.7328 0.023 Uiso calc 1 . . C C13 0.21403(14) -0.01389(13) 0.78350(8) 0.0187(2) Uani d 1 . . H H13A 0.1321 -0.0092 0.8248 0.022 Uiso calc 1 . . H H13B 0.1931 -0.1229 0.7541 0.022 Uiso calc 1 . . N N14 0.39625(12) 0.02405(11) 0.84356(6) 0.01699(19) Uani d 1 . . C C15 0.51561(14) 0.00483(13) 0.78325(8) 0.0170(2) Uani d 1 . . H H15A 0.4884 -0.1043 0.7536 0.020 Uiso calc 1 . . H H15B 0.6388 0.0215 0.8245 0.020 Uiso calc 1 . . C C16 0.49616(14) 0.12299(13) 0.70345(8) 0.0172(2) Uani d 1 . . H H16A 0.5334 0.2322 0.7330 0.021 Uiso calc 1 . . H H16B 0.5729 0.1055 0.6610 0.021 Uiso calc 1 . . C C141 0.44287(14) 0.13710(12) 0.91966(7) 0.0156(2) Uani d 1 . . C C142 0.31639(14) 0.18318(13) 0.96323(8) 0.0185(2) Uani d 1 . . H H142 0.1955 0.1406 0.9370 0.022 Uiso calc 1 . . C C143 0.36498(14) 0.28859(13) 1.04300(8) 0.0182(2) Uani d 1 . . H H143 0.2783 0.3179 1.0717 0.022 Uiso calc 1 . . C C144 0.54137(14) 0.35176(12) 1.08126(7) 0.0161(2) Uani d 1 . . C C145 0.66886(14) 0.31362(13) 1.03852(8) 0.0173(2) Uani d 1 . . H H145 0.7887 0.3601 1.0640 0.021 Uiso calc 1 . . C C146 0.62025(14) 0.20794(13) 0.95897(8) 0.0174(2) Uani d 1 . . H H146 0.7078 0.1821 0.9299 0.021 Uiso calc 1 . . N N144 0.59245(12) 0.46290(11) 1.16455(6) 0.01728(19) Uani d 1 . . O O141 0.47859(11) 0.49209(10) 1.20379(6) 0.02406(19) Uani d 1 . . O O142 0.74805(11) 0.52457(10) 1.19410(6) 0.02329(18) Uani d 1 . . C C21 0.24532(14) 0.43648(13) 0.46951(8) 0.0171(2) Uani d 1 . . C C22 0.20094(14) 0.59329(12) 0.45355(8) 0.0168(2) Uani d 1 . . C C23 0.15472(14) 0.65011(13) 0.36161(8) 0.0163(2) Uani d 1 . . H H23 0.1308 0.7557 0.3537 0.020 Uiso calc 1 . . C C24 0.14290(14) 0.55395(13) 0.28038(8) 0.0164(2) Uani d 1 . . C C25 0.17807(14) 0.40041(13) 0.28998(8) 0.0165(2) Uani d 1 . . H H25 0.1656 0.3340 0.2339 0.020 Uiso calc 1 . . C C26 0.23134(14) 0.34521(12) 0.38199(8) 0.0162(2) Uani d 1 . . O O21 0.28898(12) 0.38660(9) 0.55580(6) 0.02378(19) Uani d 1 . . C C27 0.20933(15) 0.70160(13) 0.53734(8) 0.0199(2) Uani d 1 . . O O271 0.16416(12) 0.83252(9) 0.52573(6) 0.02424(19) Uani d 1 . . O O272 0.26860(13) 0.65093(10) 0.62536(6) 0.0294(2) Uani d 1 . . H H272 0.288(2) 0.540(2) 0.6144(12) 0.044 Uiso d 1 . . N N24 0.09824(12) 0.61730(11) 0.18421(7) 0.01767(19) Uani d 1 . . O O241 0.08439(11) 0.75980(9) 0.17920(6) 0.02152(18) Uani d 1 . . O O242 0.07873(11) 0.52884(10) 0.11242(6) 0.02219(18) Uani d 1 . . N N26 0.27842(12) 0.18676(11) 0.38689(7) 0.01824(19) Uani d 1 . . O O261 0.20718(11) 0.09218(9) 0.31673(6) 0.02451(19) Uani d 1 . . O O262 0.38998(12) 0.15381(10) 0.45879(6) 0.02596(19) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N11 0.0230(5) 0.0128(4) 0.0146(4) 0.0040(4) 0.0037(4) -0.0003(4) C12 0.0177(5) 0.0181(5) 0.0198(5) 0.0037(4) 0.0032(4) -0.0033(4) C13 0.0188(5) 0.0191(5) 0.0171(5) -0.0008(4) 0.0051(4) -0.0030(4) N14 0.0184(4) 0.0179(4) 0.0142(4) 0.0015(4) 0.0045(3) -0.0018(3) C15 0.0195(5) 0.0162(5) 0.0159(5) 0.0045(4) 0.0048(4) -0.0012(4) C16 0.0194(5) 0.0157(5) 0.0175(5) 0.0030(4) 0.0066(4) -0.0006(4) C141 0.0210(5) 0.0132(5) 0.0128(5) 0.0032(4) 0.0044(4) 0.0028(4) C142 0.0163(5) 0.0207(5) 0.0176(5) 0.0029(4) 0.0030(4) 0.0004(4) C143 0.0192(5) 0.0199(5) 0.0173(5) 0.0064(4) 0.0063(4) 0.0020(4) C144 0.0218(5) 0.0130(5) 0.0133(5) 0.0031(4) 0.0039(4) 0.0005(4) C145 0.0175(5) 0.0168(5) 0.0170(5) 0.0012(4) 0.0045(4) 0.0015(4) C146 0.0190(5) 0.0176(5) 0.0169(5) 0.0031(4) 0.0071(4) 0.0011(4) N144 0.0211(5) 0.0150(4) 0.0161(4) 0.0033(4) 0.0054(4) 0.0013(3) O141 0.0240(4) 0.0273(4) 0.0229(4) 0.0058(3) 0.0092(3) -0.0061(3) O142 0.0213(4) 0.0234(4) 0.0230(4) -0.0029(3) 0.0058(3) -0.0057(3) C21 0.0188(5) 0.0154(5) 0.0162(5) 0.0013(4) 0.0039(4) -0.0003(4) C22 0.0183(5) 0.0142(5) 0.0172(5) 0.0014(4) 0.0042(4) -0.0017(4) C23 0.0156(5) 0.0146(5) 0.0187(5) 0.0024(4) 0.0043(4) -0.0001(4) C24 0.0151(5) 0.0189(5) 0.0146(5) 0.0018(4) 0.0034(4) 0.0011(4) C25 0.0143(5) 0.0176(5) 0.0174(5) -0.0001(4) 0.0054(4) -0.0042(4) C26 0.0164(5) 0.0131(5) 0.0196(5) 0.0024(4) 0.0059(4) -0.0013(4) O21 0.0394(5) 0.0160(4) 0.0151(4) 0.0071(3) 0.0044(3) 0.0009(3) C27 0.0252(6) 0.0158(5) 0.0178(5) 0.0013(4) 0.0051(4) -0.0015(4) O271 0.0347(5) 0.0153(4) 0.0218(4) 0.0066(3) 0.0046(3) -0.0032(3) O272 0.0541(6) 0.0178(4) 0.0151(4) 0.0096(4) 0.0051(4) -0.0019(3) N24 0.0141(4) 0.0220(5) 0.0168(4) 0.0022(4) 0.0043(3) 0.0004(4) O241 0.0228(4) 0.0206(4) 0.0216(4) 0.0054(3) 0.0056(3) 0.0050(3) O242 0.0224(4) 0.0284(4) 0.0151(4) 0.0022(3) 0.0049(3) -0.0038(3) N26 0.0207(5) 0.0153(4) 0.0209(5) 0.0031(4) 0.0093(4) -0.0007(4) O261 0.0267(4) 0.0178(4) 0.0285(4) 0.0023(3) 0.0074(3) -0.0087(3) O262 0.0329(5) 0.0245(4) 0.0226(4) 0.0132(4) 0.0061(3) 0.0031(3) 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 C16 N11 C12 . . 113.90(8) ? C16 N11 H11 . . 108.4(9) ? C12 N11 H11 . . 108.3(9) ? C16 N11 H12 . . 111.0(8) ? C12 N11 H12 . . 108.3(9) ? H11 N11 H12 . . 106.8(12) ? N11 C12 C13 . . 110.16(9) ? 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 . . 109.99(9) ? N14 C13 H13A . . 109.7 ? C12 C13 H13A . . 109.7 ? N14 C13 H13B . . 109.7 ? C12 C13 H13B . . 109.7 ? H13A C13 H13B . . 108.2 ? C141 N14 C15 . . 121.02(9) ? C141 N14 C13 . . 121.10(9) ? C15 N14 C13 . . 109.06(8) ? N14 C15 C16 . . 110.28(9) ? N14 C15 H15A . . 109.6 ? C16 C15 H15A . . 109.6 ? N14 C15 H15B . . 109.6 ? C16 C15 H15B . . 109.6 ? H15A C15 H15B . . 108.1 ? N11 C16 C15 . . 109.87(9) ? 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 ? N14 C141 C142 . . 121.47(10) ? N14 C141 C146 . . 121.20(10) ? C142 C141 C146 . . 117.30(10) ? C143 C142 C141 . . 121.27(10) ? C143 C142 H142 . . 119.4 ? C141 C142 H142 . . 119.4 ? C142 C143 C144 . . 119.59(10) ? C142 C143 H143 . . 120.2 ? C144 C143 H143 . . 120.2 ? C145 C144 C143 . . 120.87(10) ? C145 C144 N144 . . 119.43(10) ? C143 C144 N144 . . 119.67(10) ? C146 C145 C144 . . 119.48(10) ? C146 C145 H145 . . 120.3 ? C144 C145 H145 . . 120.3 ? C145 C146 C141 . . 121.42(10) ? C145 C146 H146 . . 119.3 ? C141 C146 H146 . . 119.3 ? O142 N144 O141 . . 122.45(9) ? O142 N144 C144 . . 118.77(9) ? O141 N144 C144 . . 118.78(9) ? O21 C21 C26 . . 124.86(10) ? O21 C21 C22 . . 120.75(9) ? C26 C21 C22 . . 114.38(9) ? C23 C22 C21 . . 121.89(10) ? C23 C22 C27 . . 117.59(10) ? C21 C22 C27 . . 120.49(10) ? C22 C23 C24 . . 120.26(10) ? C22 C23 H23 . . 119.9 ? C24 C23 H23 . . 119.9 ? C25 C24 C23 . . 120.99(10) ? C25 C24 N24 . . 119.55(9) ? C23 C24 N24 . . 119.43(10) ? C26 C25 C24 . . 118.95(10) ? C26 C25 H25 . . 120.5 ? C24 C25 H25 . . 120.5 ? C25 C26 C21 . . 123.45(10) ? C25 C26 N26 . . 115.98(9) ? C21 C26 N26 . . 120.55(9) ? O271 C27 O272 . . 121.14(10) ? O271 C27 C22 . . 121.85(10) ? O272 C27 C22 . . 117.01(10) ? C27 O272 H272 . . 105.0(10) ? O242 N24 O241 . . 123.40(9) ? O242 N24 C24 . . 118.92(9) ? O241 N24 C24 . . 117.67(9) ? O262 N26 O261 . . 122.85(9) ? O262 N26 C26 . . 119.17(9) ? O261 N26 C26 . . 117.95(9) ? 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 C16 . 1.4919(14) ? N11 C12 . 1.4951(14) ? N11 H11 . 0.894(14) ? N11 H12 . 0.910(14) ? C12 C13 . 1.5187(15) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 N14 . 1.4635(14) ? C13 H13A . 0.9900 ? C13 H13B . 0.9900 ? N14 C141 . 1.3812(13) ? N14 C15 . 1.4625(14) ? C15 C16 . 1.5169(15) ? C15 H15A . 0.9900 ? C15 H15B . 0.9900 ? C16 H16A . 0.9900 ? C16 H16B . 0.9900 ? C141 C142 . 1.4125(15) ? C141 C146 . 1.4133(15) ? C142 C143 . 1.3774(15) ? C142 H142 . 0.9500 ? C143 C144 . 1.3881(15) ? C143 H143 . 0.9500 ? C144 C145 . 1.3875(15) ? C144 N144 . 1.4437(13) ? C145 C146 . 1.3765(15) ? C145 H145 . 0.9500 ? C146 H146 . 0.9500 ? N144 O142 . 1.2315(12) ? N144 O141 . 1.2355(12) ? C21 O21 . 1.2788(13) ? C21 C26 . 1.4340(15) ? C21 C22 . 1.4394(15) ? C22 C23 . 1.3747(15) ? C22 C27 . 1.4844(15) ? C23 C24 . 1.3869(15) ? C23 H23 . 0.9500 ? C24 C25 . 1.3811(15) ? C24 N24 . 1.4498(13) ? C25 C26 . 1.3750(15) ? C25 H25 . 0.9500 ? C26 N26 . 1.4540(14) ? C27 O271 . 1.2236(14) ? C27 O272 . 1.3171(14) ? O272 H272 . 1.003(18) ? N24 O242 . 1.2277(12) ? N24 O241 . 1.2389(12) ? N26 O262 . 1.2303(12) ? N26 O261 . 1.2343(12) ? 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 O21 . 0.894(14) 1.869(14) 2.7356(12) 162.8(13) y N11 H11 O262 . 0.894(14) 2.396(14) 2.8937(13) 115.4(11) y N11 H12 O271 1_545 0.910(14) 1.874(14) 2.7668(12) 166.2(12) y O272 H272 O21 . 1.000(17) 1.549(17) 2.5020(12) 157.4(15) y C12 H12B O142 2_667 0.99 2.41 3.3921(14) 173 y C16 H16A O141 2_667 0.99 2.54 3.4906(14) 161 y C145 H145 O242 1_656 0.95 2.46 3.3927(15) 168 y C146 H146 O241 2_666 0.95 2.55 3.4227(15) 153 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 . . . . -50.40(12) ? N11 C12 C13 N14 . . . . 56.08(11) ? C12 C13 N14 C141 . . . . 84.07(12) ? C12 C13 N14 C15 . . . . -63.61(11) ? C141 N14 C15 C16 . . . . -83.73(12) ? C13 N14 C15 C16 . . . . 63.98(11) ? C12 N11 C16 C15 . . . . 50.41(11) ? N14 C15 C16 N11 . . . . -56.47(11) ? C15 N14 C141 C142 . . . . 164.67(10) ? C13 N14 C141 C142 . . . . 20.80(15) ? C15 N14 C141 C146 . . . . -17.23(15) ? C13 N14 C141 C146 . . . . -161.10(10) ? N14 C141 C142 C143 . . . . 175.90(10) ? C146 C141 C142 C143 . . . . -2.27(16) ? C141 C142 C143 C144 . . . . 0.36(16) ? C142 C143 C144 C145 . . . . 1.84(16) ? C142 C143 C144 N144 . . . . 179.67(10) ? C143 C144 C145 C146 . . . . -2.02(16) ? N144 C144 C145 C146 . . . . -179.86(10) ? C144 C145 C146 C141 . . . . 0.00(16) ? N14 C141 C146 C145 . . . . -176.08(10) ? C142 C141 C146 C145 . . . . 2.09(16) ? C145 C144 N144 O142 . . . . 1.91(15) ? C143 C144 N144 O142 . . . . -175.95(10) ? C145 C144 N144 O141 . . . . -177.77(10) ? C143 C144 N144 O141 . . . . 4.37(15) ? O21 C21 C22 C23 . . . . 179.56(10) ? C26 C21 C22 C23 . . . . -1.93(15) ? O21 C21 C22 C27 . . . . 1.51(16) ? C26 C21 C22 C27 . . . . -179.98(10) ? C21 C22 C23 C24 . . . . 2.55(16) ? C27 C22 C23 C24 . . . . -179.35(10) ? C22 C23 C24 C25 . . . . -0.39(16) ? C22 C23 C24 N24 . . . . -178.48(9) ? C23 C24 C25 C26 . . . . -2.25(16) ? N24 C24 C25 C26 . . . . 175.84(9) ? C24 C25 C26 C21 . . . . 2.85(16) ? C24 C25 C26 N26 . . . . -175.67(9) ? O21 C21 C26 C25 . . . . 177.64(10) ? C22 C21 C26 C25 . . . . -0.79(16) ? O21 C21 C26 N26 . . . . -3.90(17) ? C22 C21 C26 N26 . . . . 177.67(9) ? C23 C22 C27 O271 . . . . 5.49(17) ? C21 C22 C27 O271 . . . . -176.38(10) ? C23 C22 C27 O272 . . . . -174.21(10) ? C21 C22 C27 O272 . . . . 3.93(16) ? C25 C24 N24 O242 . . . . 5.79(14) ? C23 C24 N24 O242 . . . . -176.09(9) ? C25 C24 N24 O241 . . . . -173.14(9) ? C23 C24 N24 O241 . . . . 4.98(14) ? C25 C26 N26 O262 . . . . 150.18(10) ? C21 C26 N26 O262 . . . . -28.38(15) ? C25 C26 N26 O261 . . . . -27.86(14) ? C21 C26 N26 O261 . . . . 153.57(10) ? _cod_database_fobs_code 2244132