#------------------------------------------------------------------------------ #$Date: 2018-01-13 08:37:19 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205192 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548684.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_1548684 loop_ _publ_author_name 'Mohamed Abdelahi, Mohamed Mokhtar' 'El Bakri, Youness' 'Benchidmi, Mohammed' 'Essassi, El Mokhtar' 'Mague, Joel T.' _publ_section_title ; 3-Bromo-6-nitro-1-(prop-2-en-1-yl)-1H-indazole ; _journal_coeditor_code HB4194 _journal_issue 1 _journal_name_full IUCrData _journal_page_first x171837 _journal_paper_doi 10.1107/S2414314617018375 _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C10 H8 Br N3 O2' _chemical_formula_moiety 'C10 H8 Br N3 O2' _chemical_formula_sum 'C10 H8 Br N3 O2' _chemical_formula_weight 282.10 _chemical_name_systematic ; 3-Bromo-6-nitro-1-(prop-2-en-1-yl)-1H-indazole ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 95.086(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.5971(4) _cell_length_b 9.9501(5) _cell_length_c 28.5690(13) _cell_measurement_reflns_used 7120 _cell_measurement_temperature 150.(2) _cell_measurement_theta_max 72.1909 _cell_measurement_theta_min 3.1059 _cell_volume 2151.08(18) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.865 _diffrn_measured_fraction_theta_max 0.852 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 7880 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 72.284 _diffrn_reflns_theta_min 3.106 _exptl_absorpt_coefficient_mu 5.144 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Sheldrick, 2009) ; _exptl_crystal_colour 'pale orange' _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.252 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.040 _refine_diff_density_max 1.300 _refine_diff_density_min -1.219 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 7639 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.191 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0792 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+28.3909P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2135 _refine_ls_wR_factor_ref 0.2174 _reflns_number_gt 7050 _reflns_number_total 7639 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb4194sup1.cif _cod_data_source_block I _cod_database_code 1548684 _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 0.357 _shelx_estimated_absorpt_t_max 0.821 _shelx_hkl_file ; -2 0 1 2580.46 172.327 -2 2 0 0 2580.46 172.327 1 2 0 -1 2264.78 171.907 -2 -2 0 0 2264.78 171.907 1 3 0 -2 3.45359 2.57777 -2 -3 0 0 3.45359 2.57777 1 -3 0 2 7.90437 1.75553 -2 3 0 0 7.90437 1.75553 1 -4 0 3 5.18091 3.56590 -2 4 0 0 5.18091 3.56590 1 -4 0 3 17.4649 3.64963 -2 4 0 0 17.4649 3.64963 1 6 0 -4 290.864 21.1261 -2 -6 0 0 290.864 21.1261 1 -6 0 4 283.908 19.9634 -2 6 0 0 283.908 19.9634 1 -6 0 4 285.409 20.3021 -2 6 0 0 285.409 20.3021 1 -9 0 6 1.37861 4.14387 -2 9 0 0 1.37861 4.14387 1 0 1 0 0.24247 0.33282 -2 0 -1 0 0.24247 0.33282 1 0 -1 0 0.14053 0.28625 -2 0 1 0 0.14053 0.28625 1 -1 -1 0 42.4391 3.57193 1 1 -1 0 53.6134 3.63194 1 1 -1 0 21.1782 2.06283 2 1 1 0 23.6950 2.01763 2 -1 1 0 26.6585 2.06502 2 -1 1 0 48.3116 3.60291 1 1 1 0 45.4436 3.56135 1 -2 1 1 1299.81 87.2397 -2 2 -1 0 1299.81 87.2397 1 -2 -1 0 125.358 9.20347 1 -2 -1 1 1296.14 87.2570 -2 2 1 0 1296.14 87.2570 1 2 -1 -1 1081.78 87.1148 -2 -2 1 0 1081.78 87.1148 1 -3 1 2 209.945 14.1042 -2 3 -1 0 209.945 14.1042 1 3 1 -2 171.736 14.1898 -2 -3 -1 0 171.736 14.1898 1 -3 -1 2 191.625 13.9468 -2 3 1 0 191.625 13.9468 1 -3 -1 2 198.007 14.1091 -2 3 1 0 198.007 14.1091 1 -4 1 3 170.388 12.3928 -2 4 -1 0 170.388 12.3928 1 4 1 -3 169.184 12.6840 -2 -4 -1 0 169.184 12.6840 1 -4 1 3 154.256 12.5251 -2 4 -1 0 154.256 12.5251 1 6 1 -4 150.585 10.7275 -2 -6 -1 0 150.585 10.7275 1 -6 1 4 123.363 10.4187 -2 6 -1 0 123.363 10.4187 1 -6 1 4 112.917 10.9922 -2 6 -1 0 112.917 10.9922 1 -6 1 4 133.510 10.6178 -2 6 -1 0 133.510 10.6178 1 -6 1 4 121.564 11.7515 -2 6 -1 0 121.564 11.7515 1 -6 -1 4 149.242 12.5373 -2 6 1 0 149.242 12.5373 1 -6 -1 4 112.830 13.5029 -2 6 1 0 112.830 13.5029 1 -6 -1 4 133.486 10.2845 -2 6 1 0 133.486 10.2845 1 6 -1 -4 133.250 10.6215 -2 -6 1 0 133.250 10.6215 1 -6 -1 4 133.838 10.6692 -2 6 1 0 133.838 10.6692 1 7 -1 -5 179.595 14.5365 -2 -7 1 0 179.595 14.5365 1 -9 1 6 24.0437 6.81988 -2 9 -1 0 24.0437 6.81988 1 -9 1 6 25.2793 5.39365 -2 9 -1 0 25.2793 5.39365 1 0 2 0 424.589 34.0094 -2 0 -2 0 424.589 34.0094 1 0 -2 0 529.352 34.1319 -2 0 2 0 529.352 34.1319 1 -1 -2 0 1121.10 88.5465 1 -1 -2 0 777.608 51.8249 2 1 -2 0 776.324 51.7936 2 1 2 0 629.565 51.7410 2 -1 -2 1 1841.72 130.848 -2 1 2 0 1841.72 130.848 1 -1 2 0 1193.28 88.6073 1 -1 2 0 1430.05 88.6616 1 -2 -2 1 1019.38 72.5921 -2 2 2 0 1019.38 72.5921 1 -3 2 2 129.704 10.1624 -2 3 -2 0 129.704 10.1624 1 -3 2 2 141.874 10.2681 -2 3 -2 0 141.874 10.2681 1 3 2 -2 132.170 10.1323 -2 -3 -2 0 132.170 10.1323 1 -3 -2 2 144.557 10.3829 -2 3 2 0 144.557 10.3829 1 -4 2 3 356.148 23.8596 -2 4 -2 0 356.148 23.8596 1 -4 2 3 304.924 22.5244 -2 4 -2 0 304.924 22.5244 1 -5 2 3 523.376 37.3156 -2 5 -2 0 523.376 37.3156 1 -6 2 4 105.750 9.83761 -2 6 -2 0 105.750 9.83761 1 -6 2 4 106.803 9.77394 -2 6 -2 0 106.803 9.77394 1 -6 2 4 116.538 9.06139 -2 6 -2 0 116.538 9.06139 1 -6 -2 4 116.864 9.21369 -2 6 2 0 116.864 9.21369 1 -6 -2 4 104.506 11.1131 -2 6 2 0 104.506 11.1131 1 -6 -2 4 101.033 11.7772 -2 6 2 0 101.033 11.7772 1 -7 2 5 25.7902 6.00885 -2 7 -2 0 25.7902 6.00885 1 -9 2 6 39.1111 5.08899 -2 9 -2 0 39.1111 5.08899 1 -9 2 6 27.5328 5.76627 -2 9 -2 0 27.5328 5.76627 1 -9 -2 6 47.6253 5.38758 -2 9 2 0 47.6253 5.38758 1 0 -3 0 -0.2331 0.74787 -2 0 3 0 -0.2331 0.74787 1 1 -3 -1 241.387 17.5607 -2 -1 3 0 241.387 17.5607 1 2 3 -1 536.650 41.0768 -2 -2 -3 0 536.650 41.0768 1 2 -3 -1 652.180 41.8464 -2 -2 3 0 652.180 41.8464 1 -2 -3 1 562.140 41.8614 -2 2 3 0 562.140 41.8614 1 -3 3 2 73.9609 6.49191 -2 3 -3 0 73.9609 6.49191 1 3 3 -2 90.3771 6.40944 -2 -3 -3 0 90.3771 6.40944 1 -3 -3 2 75.7391 6.54821 -2 3 3 0 75.7391 6.54821 1 3 -3 -2 71.5662 6.26128 -2 -3 3 0 71.5662 6.26128 1 -4 3 3 107.389 9.98006 -2 4 -3 0 107.389 9.98006 1 -5 3 3 398.453 28.7499 -2 5 -3 0 398.453 28.7499 1 -6 3 4 301.904 23.4325 -2 6 -3 0 301.904 23.4325 1 -6 3 4 338.503 21.8333 -2 6 -3 0 338.503 21.8333 1 6 3 -4 312.665 23.4220 -2 -6 -3 0 312.665 23.4220 1 -6 -3 4 320.164 21.9547 -2 6 3 0 320.164 21.9547 1 -9 3 6 -1.8713 2.50124 -2 9 -3 0 -1.8713 2.50124 1 -9 -3 6 9.12512 4.96018 -2 9 3 0 9.12512 4.96018 1 0 -4 0 434.306 31.4531 -2 0 4 0 434.306 31.4531 1 1 4 -1 374.476 27.6850 -2 -1 -4 0 374.476 27.6850 1 -1 -4 1 404.590 28.2948 -2 1 4 0 404.590 28.2948 1 2 4 -1 766.413 55.7825 -2 -2 -4 0 766.413 55.7825 1 2 -4 -1 829.541 56.8474 -2 -2 4 0 829.541 56.8474 1 -2 -4 1 785.029 56.9409 -2 2 4 0 785.029 56.9409 1 -3 4 2 626.366 46.6442 -2 3 -4 0 626.366 46.6442 1 3 -4 -2 673.603 47.4979 -2 -3 4 0 673.603 47.4979 1 -3 -4 2 682.261 47.7755 -2 3 4 0 682.261 47.7755 1 6 4 -4 32.9731 9.11360 -2 -6 -4 0 32.9731 9.11360 1 -6 4 4 28.5077 9.35348 -2 6 -4 0 28.5077 9.35348 1 6 4 -4 31.7398 7.96997 -2 -6 -4 0 31.7398 7.96997 1 -6 4 4 35.7629 7.92316 -2 6 -4 0 35.7629 7.92316 1 -6 4 4 29.6262 6.50169 -2 6 -4 0 29.6262 6.50169 1 0 5 0 1.38853 2.75681 -2 0 -5 0 1.38853 2.75681 1 0 -5 0 -0.2394 1.56637 -2 0 5 0 -0.2394 1.56637 1 -2 -5 1 2.89190 5.08704 -2 2 5 0 2.89190 5.08704 1 2 -5 -1 1.07182 4.43930 -2 -2 5 0 1.07182 4.43930 1 3 5 -2 9.81804 3.48599 -2 -3 -5 0 9.81804 3.48599 1 -3 -5 2 14.6089 5.99837 -2 3 5 0 14.6089 5.99837 1 3 -5 -2 7.30053 3.17400 -2 -3 5 0 7.30053 3.17400 1 -6 5 4 46.2215 10.1425 -2 6 -5 0 46.2215 10.1425 1 6 5 -4 49.8806 8.03788 -2 -6 -5 0 49.8806 8.03788 1 6 5 -4 43.6006 7.63624 -2 -6 -5 0 43.6006 7.63624 1 0 -6 0 77.3937 7.30927 -2 0 6 0 77.3937 7.30927 1 1 -6 -1 170.170 14.1657 -2 -1 6 0 170.170 14.1657 1 -1 -6 1 174.810 14.4077 -2 1 6 0 174.810 14.4077 1 2 -6 -1 839.944 60.6556 -2 -2 6 0 839.944 60.6556 1 -2 -6 1 837.244 61.0171 -2 2 6 0 837.244 61.0171 1 3 6 -2 716.557 45.7668 -2 -3 -6 0 716.557 45.7668 1 -3 6 2 627.460 42.0111 -2 3 -6 0 627.460 42.0111 1 3 6 -2 594.389 46.4378 -2 -3 -6 0 594.389 46.4378 1 -3 6 2 630.957 45.6559 -2 3 -6 0 630.957 45.6559 1 6 6 -4 116.586 10.8814 -2 -6 -6 0 116.586 10.8814 1 0 7 0 0.67568 3.63551 -2 0 -7 0 0.67568 3.63551 1 0 7 0 -0.2826 3.06431 -2 0 -7 0 -0.2826 3.06431 1 1 7 -1 371.723 25.4342 -2 -1 -7 0 371.723 25.4342 1 -1 7 1 372.553 25.1685 -2 1 -7 0 372.553 25.1685 1 2 7 -1 26.5451 8.45722 -2 -2 -7 0 26.5451 8.45722 1 3 7 -2 292.833 20.4736 -2 -3 -7 0 292.833 20.4736 1 -3 7 2 257.775 18.7478 -2 3 -7 0 257.775 18.7478 1 6 7 -4 43.3538 6.13787 -2 -6 -7 0 43.3538 6.13787 1 0 8 0 146.207 11.8113 -2 0 -8 0 146.207 11.8113 1 0 8 0 139.540 10.6845 -2 0 -8 0 139.540 10.6845 1 -1 8 1 84.5526 7.78126 -2 1 -8 0 84.5526 7.78126 1 1 8 -1 62.7921 8.17695 -2 -1 -8 0 62.7921 8.17695 1 2 8 -1 149.046 12.4457 -2 -2 -8 0 149.046 12.4457 1 -3 8 2 268.989 18.6365 -2 3 -8 0 268.989 18.6365 1 3 8 -2 277.438 20.5212 -2 -3 -8 0 277.438 20.5212 1 0 9 0 -1.4043 2.62121 -2 0 -9 0 -1.4043 2.62121 1 1 9 -1 293.901 20.4117 -2 -1 -9 0 293.901 20.4117 1 1 9 -1 208.872 15.9114 -2 1 9 0 208.872 15.9114 -2 -1 -9 0 208.872 15.9114 1 2 9 -1 46.5040 5.94703 -2 -2 -9 0 46.5040 5.94703 1 2 9 -1 49.0291 6.60334 -2 -2 -9 0 49.0291 6.60334 1 -2 9 0 320.290 26.4039 -2 2 -9 0 320.290 26.4039 1 -3 9 2 106.647 8.16636 -2 3 -9 0 106.647 8.16636 1 3 9 -2 102.036 10.4285 -2 -3 -9 0 102.036 10.4285 1 0 10 0 718.972 46.8328 -2 0 -10 0 718.972 46.8328 1 1 10 -1 7.00167 5.42454 -2 -1 -10 0 7.00167 5.42454 1 2 10 -1 1.96336 6.67808 -2 -2 -10 0 1.96336 6.67808 1 -3 10 2 19.6910 3.58857 -2 3 -10 0 19.6910 3.58857 1 3 10 -2 24.0649 6.90835 -2 -3 -10 0 24.0649 6.90835 1 0 11 0 0.46872 2.25950 -2 0 -11 0 0.46872 2.25950 1 0 11 -1 7.40528 7.63665 -2 0 -11 0 7.40528 7.63665 1 1 11 -1 43.2611 4.70173 -2 -1 -11 0 43.2611 4.70173 1 0 12 0 11.1865 2.89764 -2 0 -12 0 11.1865 2.89764 1 -1 12 1 42.2421 3.78119 -2 1 -12 0 42.2421 3.78119 1 2 12 0 20.4560 4.17246 2 -9 0 5 84.8713 8.52454 -2 9 0 -1 84.8713 8.52454 1 -9 0 5 83.0813 8.00488 -2 9 0 -1 83.0813 8.00488 1 -6 0 3 29.3891 7.66758 -2 6 0 -1 29.3891 7.66758 1 6 0 -3 12.5217 4.48713 -2 -6 0 1 12.5217 4.48713 1 -6 0 3 22.3602 6.08508 -2 6 0 -1 22.3602 6.08508 1 -6 0 3 16.3270 5.84224 -2 6 0 -1 16.3270 5.84224 1 -5 0 2 367.992 24.8085 -2 5 0 -1 367.992 24.8085 1 -4 0 2 30.1680 4.27957 -2 4 0 -1 30.1680 4.27957 1 -4 0 2 29.4408 4.72337 -2 4 0 -1 29.4408 4.72337 1 -3 0 1 238.187 17.3230 -2 3 0 -1 238.187 17.3230 1 2 0 0 1155.36 89.9936 -2 -2 0 1 1155.36 89.9936 1 -2 0 0 1377.75 90.1797 -2 2 0 -1 1377.75 90.1797 1 1 0 -1 45.6045 3.45287 1 1 0 0 59.0683 4.49098 -2 -1 0 1 59.0683 4.49098 1 -1 0 -1 448.256 32.5255 1 1 0 1 469.151 32.5222 1 -2 0 2 890.369 62.8663 -2 2 0 1 890.369 62.8663 1 2 0 -2 872.669 62.7675 -2 -2 0 -1 872.669 62.7675 1 2 0 1 42.3469 3.84732 2 -3 0 3 185.554 12.7054 -2 3 0 1 185.554 12.7054 1 -3 0 3 164.964 12.6354 -2 3 0 1 164.964 12.6354 1 3 0 -3 172.723 12.8249 -2 -3 0 -1 172.723 12.8249 1 -4 0 -1 8.01119 2.57525 2 -6 0 5 4.00384 3.28813 -2 6 0 1 4.00384 3.28813 1 6 0 -5 10.8063 4.54423 -2 -6 0 -1 10.8063 4.54423 1 -6 0 5 3.98165 3.20045 -2 6 0 1 3.98165 3.20045 1 -9 0 7 19.4586 5.54169 -2 9 0 1 19.4586 5.54169 1 -9 0 7 12.1768 4.69790 -2 9 0 1 12.1768 4.69790 1 -9 1 5 21.0415 7.61992 -2 9 -1 -1 21.0415 7.61992 1 -9 -1 5 9.16273 3.08954 -2 9 1 -1 9.16273 3.08954 1 7 -1 -4 86.7872 9.21301 -2 -7 1 1 86.7872 9.21301 1 6 1 -3 8.25301 3.67614 -2 -6 -1 1 8.25301 3.67614 1 -6 1 3 2.46498 3.15343 -2 6 -1 -1 2.46498 3.15343 1 -6 1 3 15.5425 4.98301 -2 6 -1 -1 15.5425 4.98301 1 -6 -1 3 18.0770 5.45064 -2 6 1 -1 18.0770 5.45064 1 -6 -1 3 6.95845 3.21305 -2 6 1 -1 6.95845 3.21305 1 -6 -1 3 12.1234 3.73168 -2 6 1 -1 12.1234 3.73168 1 -5 1 2 23.6131 6.22764 -2 5 -1 -1 23.6131 6.22764 1 -5 1 2 19.6901 4.97698 -2 5 -1 -1 19.6901 4.97698 1 -4 1 2 125.322 10.0156 -2 4 -1 -1 125.322 10.0156 1 4 1 -2 129.482 10.1711 -2 -4 -1 1 129.482 10.1711 1 -4 1 2 127.674 10.5871 -2 4 -1 -1 127.674 10.5871 1 -4 -1 2 137.650 10.8330 -2 4 1 -1 137.650 10.8330 1 -3 1 1 750.387 50.6134 -2 3 -1 -1 750.387 50.6134 1 3 1 -1 649.110 49.7207 -2 -3 -1 1 649.110 49.7207 1 -3 -1 1 757.742 50.6518 -2 3 1 -1 757.742 50.6518 1 -3 -1 1 677.309 49.7201 -2 3 1 -1 677.309 49.7201 1 2 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203.977 16.5191 1 4 5 6 190.184 17.2799 -2 -4 -5 9 190.184 17.2799 1 -3 5 -7 85.5834 8.74983 -2 3 -5 -9 85.5834 8.74983 1 -2 -5 -8 521.471 38.3398 -2 2 5 -9 521.471 38.3398 1 2 -5 8 517.040 38.5321 -2 -2 5 9 517.040 38.5321 1 1 5 8 714.294 48.3380 -2 -1 -5 9 714.294 48.3380 1 1 -5 8 628.177 49.5861 -2 -1 5 9 628.177 49.5861 1 -1 -5 -8 705.754 49.4879 -2 1 5 -9 705.754 49.4879 1 0 5 9 40.2941 3.89761 -2 0 -5 9 40.2941 3.89761 1 0 -5 -9 35.8053 4.50350 -2 0 5 -9 35.8053 4.50350 1 0 -5 9 36.6133 5.36050 -2 0 5 9 36.6133 5.36050 1 -1 5 10 1010.27 68.6936 -2 1 -5 9 1010.27 68.6936 1 1 -5 -10 966.268 69.9524 -2 -1 5 -9 966.268 69.9524 1 -1 -5 10 950.325 70.5676 -2 1 5 9 950.325 70.5676 1 -2 5 10 618.353 43.9172 -2 2 -5 9 618.353 43.9172 1 3 5 -11 98.6780 9.31072 -2 -3 -5 -9 98.6780 9.31072 1 -3 5 11 110.839 10.1802 -2 3 -5 9 110.839 10.1802 1 -6 5 13 6.03361 3.17668 -2 6 -5 9 6.03361 3.17668 1 -6 6 -5 127.933 13.8295 -2 6 -6 -9 127.933 13.8295 1 -5 6 -6 139.577 12.4749 -2 5 -6 -9 139.577 12.4749 1 5 6 6 160.817 13.9951 -2 -5 -6 9 160.817 13.9951 1 4 6 6 128.074 10.5346 -2 -4 -6 9 128.074 10.5346 1 3 6 7 18.8998 5.96888 -2 -3 -6 9 18.8998 5.96888 1 3 6 7 11.2757 7.16425 -2 -3 -6 9 11.2757 7.16425 1 -3 6 -7 12.2247 4.27129 -2 3 -6 -9 12.2247 4.27129 1 -2 6 -8 21.1570 8.19033 -2 2 -6 -9 21.1570 8.19033 1 2 6 8 44.1222 10.1807 -2 -2 -6 9 44.1222 10.1807 1 2 6 8 28.5295 7.10495 -2 -2 -6 9 28.5295 7.10495 1 0 -6 -9 797.915 56.7168 -2 0 6 -9 797.915 56.7168 1 0 -6 9 770.474 57.0185 -2 0 6 9 770.474 57.0185 1 -1 6 10 419.215 27.6173 -2 1 -6 9 419.215 27.6173 1 1 -6 -10 421.876 31.1848 -2 -1 6 -9 421.876 31.1848 1 -1 -6 10 398.434 33.0492 -2 1 6 9 398.434 33.0492 1 -2 6 10 101.365 9.80484 -2 2 -6 9 101.365 9.80484 1 3 6 -11 51.0172 6.58366 -2 -3 -6 -9 51.0172 6.58366 1 -3 -6 11 55.6898 9.24894 -2 3 6 9 55.6898 9.24894 1 4 6 -12 97.6610 11.4764 -2 -4 -6 -9 97.6610 11.4764 1 -6 6 13 28.3663 6.35540 -2 6 -6 9 28.3663 6.35540 1 -6 6 13 15.5885 6.25635 -2 6 -6 9 15.5885 6.25635 1 6 6 -13 21.7208 7.02338 -2 -6 -6 -9 21.7208 7.02338 1 6 7 5 121.270 10.4700 -2 -6 -7 9 121.270 10.4700 1 -5 7 -6 5.38499 6.61047 -2 5 -7 -9 5.38499 6.61047 1 -4 7 -6 24.5847 6.46808 -2 4 -7 -9 24.5847 6.46808 1 4 7 6 14.9731 7.81045 -2 -4 -7 9 14.9731 7.81045 1 -3 7 -7 141.228 10.7622 -2 3 -7 -9 141.228 10.7622 1 3 7 7 140.071 11.2040 -2 -3 -7 9 140.071 11.2040 1 -2 7 -8 287.563 19.2620 -2 2 -7 -9 287.563 19.2620 1 2 7 8 252.735 21.6277 -2 -2 -7 9 252.735 21.6277 1 2 7 8 274.835 19.0880 -2 -2 -7 9 274.835 19.0880 1 -1 7 -8 163.020 13.3922 -2 1 -7 -9 163.020 13.3922 1 1 7 8 175.114 13.2114 -2 -1 -7 9 175.114 13.2114 1 1 7 8 154.291 12.6779 -2 -1 -7 9 154.291 12.6779 1 1 7 8 182.152 14.7657 -2 -1 -7 9 182.152 14.7657 1 0 7 9 2.56425 2.77462 -2 0 -7 9 2.56425 2.77462 1 0 7 9 -2.5478 3.63434 -2 0 -7 9 -2.5478 3.63434 1 0 7 -9 3.86384 3.76628 -2 0 -7 -9 3.86384 3.76628 1 0 7 9 6.79507 4.85835 -2 0 -7 9 6.79507 4.85835 1 -1 7 10 66.2711 6.92621 -2 1 -7 9 66.2711 6.92621 1 1 7 -10 47.3676 10.5143 -2 -1 -7 -9 47.3676 10.5143 1 -2 7 10 417.502 28.0235 -2 2 -7 9 417.502 28.0235 1 -3 7 11 65.8530 7.63467 -2 3 -7 9 65.8530 7.63467 1 -3 7 11 78.5811 7.37986 -2 3 -7 9 78.5811 7.37986 1 5 -7 9 23.4313 5.54172 1 -5 8 -6 19.1750 6.07740 -2 5 -8 -9 19.1750 6.07740 1 -4 8 -6 44.3863 7.15649 -2 4 -8 -9 44.3863 7.15649 1 4 8 6 66.9105 8.45450 -2 -4 -8 9 66.9105 8.45450 1 -3 8 -7 37.5569 5.19212 -2 3 -8 -9 37.5569 5.19212 1 3 8 7 34.4492 5.49864 -2 -3 -8 9 34.4492 5.49864 1 -2 8 -8 110.362 9.57848 -2 2 -8 -9 110.362 9.57848 1 2 8 8 94.9220 9.06317 -2 -2 -8 9 94.9220 9.06317 1 1 8 8 505.730 36.9412 -2 -1 -8 9 505.730 36.9412 1 0 8 9 120.586 9.32893 -2 0 -8 9 120.586 9.32893 1 0 8 -9 123.202 10.2506 -2 0 -8 -9 123.202 10.2506 1 1 8 -10 111.879 11.8668 -2 -1 -8 -9 111.879 11.8668 1 -3 8 11 8.17523 3.06694 -2 3 -8 9 8.17523 3.06694 1 -3 8 11 12.1943 5.32356 -2 3 -8 9 12.1943 5.32356 1 -3 -8 11 9.61378 5.40521 -2 3 8 9 9.61378 5.40521 1 4 9 6 62.2587 7.50413 -2 -4 -9 9 62.2587 7.50413 1 -4 9 -6 69.2505 6.76577 -2 4 -9 -9 69.2505 6.76577 1 -3 9 -7 39.9859 4.95599 -2 3 -9 -9 39.9859 4.95599 1 3 9 7 35.8501 6.10555 -2 -3 -9 9 35.8501 6.10555 1 0 9 -9 6.19253 3.24204 -2 0 -9 -9 6.19253 3.24204 1 0 9 9 8.05359 2.75728 -2 0 -9 9 8.05359 2.75728 1 0 9 9 16.3174 5.09657 -2 0 -9 9 16.3174 5.09657 1 1 9 -10 168.467 13.8405 -2 -1 -9 -9 168.467 13.8405 1 -3 9 11 4.32500 3.64352 -2 3 -9 9 4.32500 3.64352 1 -3 9 11 6.34439 6.37968 -2 3 -9 9 6.34439 6.37968 1 -4 10 -6 0.57189 3.89725 -2 4 -10 -9 0.57189 3.89725 1 3 10 7 203.844 15.6656 -2 -3 -10 9 203.844 15.6656 1 1 10 8 34.5496 4.94384 -2 -1 -10 9 34.5496 4.94384 1 0 10 9 14.2638 5.30661 -2 0 -10 9 14.2638 5.30661 1 0 10 9 13.0655 3.04984 -2 0 -10 9 13.0655 3.04984 1 0 10 9 12.9619 4.46137 -2 0 -10 9 12.9619 4.46137 1 0 10 -9 15.1108 4.80553 -2 0 -10 -9 15.1108 4.80553 1 1 10 -10 17.8293 7.04367 -2 -1 -10 -9 17.8293 7.04367 1 -2 10 10 52.6147 5.21685 -2 2 -10 9 52.6147 5.21685 1 -3 10 11 94.4582 7.12235 -2 3 -10 9 94.4582 7.12235 1 3 11 7 15.8149 3.26067 -2 -3 -11 9 15.8149 3.26067 1 -3 11 -7 15.8181 2.90654 -2 3 -11 -9 15.8181 2.90654 1 0 11 -9 0.13958 3.41645 -2 0 -11 -9 0.13958 3.41645 1 0 11 9 4.09415 2.84071 -2 0 -11 9 4.09415 2.84071 1 -9 0 -4 -1.7030 2.42850 -2 9 0 -10 -1.7030 2.42850 1 -9 0 -4 0.60126 3.90190 -2 9 0 -10 0.60126 3.90190 1 -6 0 -6 277.247 18.9392 -2 6 0 -10 277.247 18.9392 1 -5 0 -7 20.1538 7.70428 -2 5 0 -10 20.1538 7.70428 1 -5 0 -7 -2.1380 8.83705 -2 5 0 -10 -2.1380 8.83705 1 -4 0 -7 157.341 14.3049 -2 4 0 -10 157.341 14.3049 1 -4 0 -7 176.989 12.8585 -2 4 0 -10 176.989 12.8585 1 -3 0 -8 64.6921 6.20432 -2 3 0 -10 64.6921 6.20432 1 -1 0 10 58.1625 4.50628 2 0 0 -10 473.194 33.9613 -2 0 0 -10 473.194 33.9613 1 1 0 10 3.54439 1.56980 1 1 0 -11 38.2337 3.72615 -2 -1 0 -10 38.2337 3.72615 1 2 0 10 1716.49 119.989 1 -3 0 12 91.2936 7.24251 -2 3 0 10 91.2936 7.24251 1 -3 0 12 89.3060 7.16457 -2 3 0 10 89.3060 7.16457 1 -6 0 14 493.128 32.5962 -2 6 0 10 493.128 32.5962 1 -6 0 14 445.847 31.4424 -2 6 0 10 445.847 31.4424 1 -8 0 15 30.6128 8.07528 -2 8 0 10 30.6128 8.07528 1 -9 1 -4 11.0831 4.10951 -2 9 -1 -10 11.0831 4.10951 1 -9 -1 -4 13.1104 4.15940 -2 9 1 -10 13.1104 4.15940 1 -9 -1 -4 17.7537 4.37252 -2 9 1 -10 17.7537 4.37252 1 -6 1 -6 155.955 11.9524 -2 6 -1 -10 155.955 11.9524 1 -5 1 -7 168.855 15.4547 -2 5 -1 -10 168.855 15.4547 1 -5 1 -7 180.435 14.6134 -2 5 -1 -10 180.435 14.6134 1 -5 1 -7 204.915 13.8688 -2 5 -1 -10 204.915 13.8688 1 -5 -1 -7 190.431 15.2610 -2 5 1 -10 190.431 15.2610 1 -5 -1 -7 185.517 14.9639 -2 5 1 -10 185.517 14.9639 1 -4 1 -7 324.122 22.7415 -2 4 -1 -10 324.122 22.7415 1 -4 1 -7 342.913 25.6983 -2 4 -1 -10 342.913 25.6983 1 -4 -1 -7 309.494 22.9054 -2 4 1 -10 309.494 22.9054 1 -4 -1 -7 362.358 25.6247 -2 4 1 -10 362.358 25.6247 1 3 1 8 16.5399 3.94495 -2 -3 -1 10 16.5399 3.94495 1 1 -1 -10 1878.70 134.008 1 -1 1 10 1029.97 73.1585 2 0 1 -10 364.944 26.2222 -2 0 -1 -10 364.944 26.2222 1 0 -1 -10 361.393 26.1378 -2 0 1 -10 361.393 26.1378 1 -1 1 11 626.470 43.4655 -2 1 -1 10 626.470 43.4655 1 1 1 -11 649.159 43.5260 -2 -1 -1 -10 649.159 43.5260 1 -1 1 -10 524.623 37.4295 1 -1 -1 11 548.501 43.4208 -2 1 1 10 548.501 43.4208 1 -2 1 11 1212.90 85.0083 -2 2 -1 10 1212.90 85.0083 1 -2 -1 12 1226.79 85.9297 -2 2 1 10 1226.79 85.9297 1 -3 1 12 13.3851 3.84138 -2 3 -1 10 13.3851 3.84138 1 -3 -1 12 3.11428 3.27938 -2 3 1 10 3.11428 3.27938 1 -3 -1 12 9.67099 2.99182 -2 3 1 10 9.67099 2.99182 1 -4 -1 13 133.084 10.7055 -2 4 1 10 133.084 10.7055 1 -5 1 13 102.553 8.97612 -2 5 -1 10 102.553 8.97612 1 5 -1 10 59.6144 6.24875 1 -5 -1 13 119.115 9.36098 -2 5 1 10 119.115 9.36098 1 -6 1 14 121.803 9.48374 -2 6 -1 10 121.803 9.48374 1 -6 1 14 97.5322 11.1774 -2 6 -1 10 97.5322 11.1774 1 -6 1 14 100.154 11.2556 -2 6 -1 10 100.154 11.2556 1 -6 -1 14 127.960 9.64313 -2 6 1 10 127.960 9.64313 1 -6 -1 14 116.901 11.7835 -2 6 1 10 116.901 11.7835 1 -8 1 15 132.381 11.1489 -2 8 -1 10 132.381 11.1489 1 -8 -1 15 122.933 12.3031 -2 8 1 10 122.933 12.3031 1 -9 2 -4 3.00192 3.00041 -2 9 -2 -10 3.00192 3.00041 1 -9 2 -4 9.90355 4.08145 -2 9 -2 -10 9.90355 4.08145 1 6 2 6 15.3149 5.65037 -2 -6 -2 10 15.3149 5.65037 1 -6 2 -6 25.7210 6.15678 -2 6 -2 -10 25.7210 6.15678 1 -6 2 -6 22.1340 5.16338 -2 6 -2 -10 22.1340 5.16338 1 -6 -2 -6 16.4371 5.23098 -2 6 2 -10 16.4371 5.23098 1 -6 -2 -6 23.3647 6.49465 -2 6 2 -10 23.3647 6.49465 1 5 2 7 74.2104 8.69769 -2 -5 -2 10 74.2104 8.69769 1 -5 2 -7 90.5581 11.5504 -2 5 -2 -10 90.5581 11.5504 1 -5 2 -7 95.6546 8.54622 -2 5 -2 -10 95.6546 8.54622 1 -5 -2 -7 105.658 10.3201 -2 5 2 -10 105.658 10.3201 1 -5 -2 -7 80.3540 10.8606 -2 5 2 -10 80.3540 10.8606 1 -4 2 -7 83.3247 11.5628 -2 4 -2 -10 83.3247 11.5628 1 -4 2 -7 85.3463 8.22011 -2 4 -2 -10 85.3463 8.22011 1 -4 -2 -7 93.0426 10.4426 -2 4 2 -10 93.0426 10.4426 1 -4 -2 -7 78.8248 9.23860 -2 4 2 -10 78.8248 9.23860 1 3 2 8 58.4535 5.15388 -2 -3 -2 10 58.4535 5.15388 1 -3 2 -8 45.8957 5.80283 -2 3 -2 -10 45.8957 5.80283 1 -3 2 -8 50.7117 6.66059 -2 3 -2 -10 50.7117 6.66059 1 -3 -2 -8 59.2234 5.72709 -2 3 2 -10 59.2234 5.72709 1 -2 -2 10 58.9636 4.97022 1 -1 2 -9 2007.66 142.820 -2 1 -2 -10 2007.66 142.820 1 0 2 -10 2.37456 1.33437 -2 0 -2 -10 2.37456 1.33437 1 0 -2 -10 4.25533 1.57275 -2 0 2 -10 4.25533 1.57275 1 -1 2 11 903.144 66.1211 -2 1 -2 10 903.144 66.1211 1 1 -2 -11 986.120 67.1349 -2 -1 2 -10 986.120 67.1349 1 -1 -2 11 936.811 67.2776 -2 1 2 10 936.811 67.2776 1 -2 2 11 941.037 58.4896 -2 2 -2 10 941.037 58.4896 1 -2 -2 12 891.904 62.7243 -2 2 2 10 891.904 62.7243 1 2 2 10 226.954 16.3878 2 2 -2 -11 718.604 59.0523 -2 -2 2 -10 718.604 59.0523 1 -3 2 12 117.779 8.94258 -2 3 -2 10 117.779 8.94258 1 -3 -2 12 114.809 9.13427 -2 3 2 10 114.809 9.13427 1 4 2 -12 515.633 37.1818 -2 -4 -2 -10 515.633 37.1818 1 -5 2 13 134.366 10.4204 -2 5 -2 10 134.366 10.4204 1 6 2 -14 148.333 12.9736 -2 -6 -2 -10 148.333 12.9736 1 -6 2 14 156.633 11.9580 -2 6 -2 10 156.633 11.9580 1 -6 2 14 155.682 13.2497 -2 6 -2 10 155.682 13.2497 1 -6 -2 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32 2.08646 3.73235 -2 3 -1 30 2.08646 3.73235 1 -3 -1 32 2.69254 3.07352 -2 3 1 30 2.69254 3.07352 1 -4 -1 -30 1.50601 1.93883 2 -4 1 -30 -0.1302 1.97756 2 5 -2 -30 12.0268 3.06957 1 5 2 27 3.35929 4.47175 -2 -5 -2 30 3.35929 4.47175 1 5 2 -30 5.50527 2.54992 1 4 -2 -30 7.78354 3.14488 1 4 -2 27 11.5683 4.34893 -2 -4 2 30 11.5683 4.34893 1 4 2 -30 4.50414 2.40539 1 3 2 28 20.5913 4.79451 -2 -3 -2 30 20.5913 4.79451 1 3 2 28 21.7732 5.00779 -2 -3 -2 30 21.7732 5.00779 1 3 -2 28 16.9892 3.71692 -2 -3 2 30 16.9892 3.71692 1 3 -2 28 13.2592 4.54527 -2 -3 2 30 13.2592 4.54527 1 2 2 29 43.5245 5.87497 -2 -2 -2 30 43.5245 5.87497 1 2 -2 -30 21.0160 4.36071 1 2 2 -30 29.2367 4.44983 1 1 2 29 103.275 8.62852 -2 -1 -2 30 103.275 8.62852 1 1 2 29 96.4385 9.31939 -2 -1 -2 30 96.4385 9.31939 1 1 -2 -30 66.2031 6.83854 1 1 2 -30 76.0653 6.10026 1 0 2 30 111.530 8.88919 -2 0 -2 30 111.530 8.88919 1 0 2 30 118.193 9.60095 -2 0 -2 30 118.193 9.60095 1 0 -2 -30 108.998 9.08661 -2 0 2 -30 108.998 9.08661 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14.4909 1 1 -3 30 16.2646 5.22341 2 -1 -3 -30 15.3105 3.42481 2 -1 -3 31 25.0768 6.61458 -2 1 3 30 25.0768 6.61458 1 -2 -3 -30 10.0535 2.99076 2 -2 -3 31 9.49098 5.95510 -2 2 3 30 9.49098 5.95510 1 -2 3 -30 2.02228 2.59519 2 4 -4 -30 31.0005 3.60947 1 4 -4 27 37.3715 4.15180 -2 -4 4 30 37.3715 4.15180 1 4 4 -30 34.6291 3.59813 1 3 -4 28 12.3990 3.78004 -2 -3 4 30 12.3990 3.78004 1 2 -4 -30 44.4847 4.63779 1 2 -4 29 36.9327 6.69610 -2 -2 4 30 36.9327 6.69610 1 2 -4 29 39.9397 5.27496 -2 -2 4 30 39.9397 5.27496 1 2 4 -30 31.4016 4.17281 1 1 -4 -30 83.8435 7.80872 1 1 4 -30 97.9796 7.00611 1 1 -4 29 119.768 9.48862 -2 -1 4 30 119.768 9.48862 1 0 4 30 28.7776 4.72303 -2 0 -4 30 28.7776 4.72303 1 0 -4 30 24.3376 5.01391 -2 0 4 30 24.3376 5.01391 1 0 -4 30 25.4897 5.61162 -2 0 4 30 25.4897 5.61162 1 0 -4 -30 31.0493 4.31761 -2 0 4 -30 31.0493 4.31761 1 -1 -4 -30 49.2157 4.64016 2 -1 -4 31 75.7125 8.64117 -2 1 4 30 75.7125 8.64117 1 -1 4 -30 52.1161 7.62696 2 2 -4 30 8.20556 3.52273 2 -2 4 -30 9.14069 3.36639 2 -3 4 32 107.248 7.87591 -2 3 -4 30 107.248 7.87591 1 3 5 28 6.35250 2.89272 -2 -3 -5 30 6.35250 2.89272 1 -3 5 -28 9.46404 3.07241 -2 3 -5 -30 9.46404 3.07241 1 2 -5 -30 84.1882 7.58502 1 2 5 -30 95.3297 6.68095 1 1 5 -30 65.9731 5.41470 1 1 -5 29 106.707 8.41919 -2 -1 5 30 106.707 8.41919 1 0 5 30 18.1229 4.30958 -2 0 -5 30 18.1229 4.30958 1 0 -5 30 18.9709 3.90367 -2 0 5 30 18.9709 3.90367 1 -1 -5 -30 8.16801 2.87776 2 -2 5 31 12.9251 3.95870 -2 2 -5 30 12.9251 3.95870 1 -2 -5 -30 2.81189 1.67976 2 2 -5 30 1.07920 1.80450 2 -2 5 -30 -0.3083 2.59996 2 2 -6 -30 33.2140 3.76295 1 2 6 29 25.5025 4.05411 -2 -2 -6 30 25.5025 4.05411 1 -2 6 30 28.9090 3.25032 1 2 6 -30 27.0745 3.07787 1 1 6 29 23.3728 4.18226 -2 -1 -6 30 23.3728 4.18226 1 1 6 -30 16.9155 3.02863 1 1 -6 29 26.4512 4.26584 -2 -1 6 30 26.4512 4.26584 1 0 6 30 8.72012 2.68512 -2 0 -6 30 8.72012 2.68512 1 0 -6 30 6.19226 1.85912 -2 0 6 30 6.19226 1.85912 1 1 -6 30 14.0252 2.89549 1 -1 -6 -30 14.6244 2.84422 2 1 6 30 12.4403 2.83771 2 5 0 -31 14.2477 3.18998 1 4 0 28 20.7096 5.46529 -2 -4 0 31 20.7096 5.46529 1 4 0 -31 2.44109 2.83944 1 3 0 29 100.987 8.40269 -2 -3 0 31 100.987 8.40269 1 3 0 29 127.387 8.70774 -2 -3 0 31 127.387 8.70774 1 2 0 -31 36.7274 4.31312 1 2 0 30 68.5149 7.76313 -2 -2 0 31 68.5149 7.76313 1 1 0 -31 12.3589 4.08581 1 1 0 30 41.6525 7.22586 -2 -1 0 31 41.6525 7.22586 1 0 0 -31 0.63636 6.61320 -2 0 0 -31 0.63636 6.61320 1 0 0 31 9.49527 6.14517 -2 0 0 31 9.49527 6.14517 1 0 0 31 5.56839 3.35835 -2 0 0 31 5.56839 3.35835 1 -1 0 -31 2.70770 2.82739 2 -2 0 32 9.64772 5.58454 -2 2 0 31 9.64772 5.58454 1 -2 0 -31 3.55391 2.30048 2 5 -1 -31 1.81622 2.27065 1 5 1 -31 2.99432 2.42745 1 4 -1 -31 11.5580 3.67550 1 4 -1 28 14.5682 4.80127 -2 -4 1 31 14.5682 4.80127 1 4 1 -31 14.0983 3.12477 1 3 1 29 9.83801 4.04681 -2 -3 -1 31 9.83801 4.04681 1 3 1 29 9.42961 3.30033 -2 -3 -1 31 9.42961 3.30033 1 2 -1 -31 166.043 11.9285 1 2 1 30 210.934 15.0094 -2 -2 -1 31 210.934 15.0094 1 2 1 -31 174.875 11.8452 1 1 -1 -31 67.7248 6.40758 1 1 1 30 87.0714 8.27851 -2 -1 -1 31 87.0714 8.27851 1 1 1 -31 68.7080 5.94069 1 0 1 31 69.1277 6.66089 -2 0 -1 31 69.1277 6.66089 1 0 1 31 71.8558 6.80671 -2 0 -1 31 71.8558 6.80671 1 0 -1 31 67.8080 9.29122 -2 0 1 31 67.8080 9.29122 1 0 -1 -31 70.1206 6.85354 -2 0 1 -31 70.1206 6.85354 1 -1 -1 -31 55.8823 5.07548 2 -1 1 32 74.9474 7.86240 -2 1 -1 31 74.9474 7.86240 1 -1 1 -31 46.9786 5.51294 2 -2 -1 -31 18.3417 3.58679 2 -2 1 32 50.1447 6.76623 -2 2 -1 31 50.1447 6.76623 1 -2 -1 32 45.7598 6.52504 -2 2 1 31 45.7598 6.52504 1 -2 1 -31 19.0884 3.57308 2 -3 1 33 69.2963 6.68041 -2 3 -1 31 69.2963 6.68041 1 -3 -1 33 67.9166 5.67506 -2 3 1 31 67.9166 5.67506 1 4 -2 -31 69.4398 5.99724 1 4 -2 28 83.2534 7.04165 -2 -4 2 31 83.2534 7.04165 1 4 2 -31 83.5442 6.00769 1 3 2 29 0.59163 2.20270 -2 -3 -2 31 0.59163 2.20270 1 3 -2 29 -1.8254 2.54299 -2 -3 2 31 -1.8254 2.54299 1 -2 -2 31 71.5541 6.51275 1 2 -2 -31 60.0989 5.83044 1 2 2 -31 66.8834 5.62949 1 1 -2 -31 77.2413 7.08766 1 1 2 -31 83.5696 6.47950 1 0 2 31 25.8198 5.88566 -2 0 -2 31 25.8198 5.88566 1 0 -2 -31 39.9205 5.06844 -2 0 2 -31 39.9205 5.06844 1 0 -2 31 37.9494 5.51211 -2 0 2 31 37.9494 5.51211 1 -1 2 32 16.9836 7.22461 -2 1 -2 31 16.9836 7.22461 1 -1 2 32 15.2326 5.63730 -2 1 -2 31 15.2326 5.63730 1 -1 -2 -31 12.5699 3.52636 2 -1 2 -31 6.17678 3.21491 2 -2 2 32 26.9600 5.32592 -2 2 -2 31 26.9600 5.32592 1 -2 -2 -31 20.0062 3.20138 2 -2 -2 32 28.9773 5.96867 -2 2 2 31 28.9773 5.96867 1 -2 2 -31 14.4586 3.50657 2 -3 2 33 35.0051 4.67302 -2 3 -2 31 35.0051 4.67302 1 4 -3 -31 46.9240 4.28010 1 4 3 -31 47.0865 4.20823 1 3 -3 29 32.4514 3.93802 -2 -3 3 31 32.4514 3.93802 1 3 -3 29 36.0459 4.19393 -2 -3 3 31 36.0459 4.19393 1 2 -3 -31 24.2994 4.01991 1 2 -3 30 17.5110 5.10957 -2 -2 3 31 17.5110 5.10957 1 2 3 -31 23.6229 3.49652 1 1 -3 -31 11.8503 4.86244 1 1 -3 30 21.0719 6.62426 -2 -1 3 31 21.0719 6.62426 1 1 3 -31 21.8418 3.54031 1 -1 3 31 19.6384 4.52547 1 0 3 31 101.102 7.58958 -2 0 -3 31 101.102 7.58958 1 0 -3 31 78.9115 8.10268 -2 0 3 31 78.9115 8.10268 1 0 -3 31 103.370 8.05724 -2 0 3 31 103.370 8.05724 1 0 -3 -31 100.740 7.61831 -2 0 3 -31 100.740 7.61831 1 -1 -3 32 17.3410 6.13164 -2 1 3 31 17.3410 6.13164 1 -1 3 -31 10.1818 5.09871 2 -2 -3 -31 18.2514 3.15037 2 -2 -3 32 45.0524 7.17916 -2 2 3 31 45.0524 7.17916 1 -2 3 -31 15.3082 3.52523 2 3 -4 29 32.8852 3.50555 -2 -3 4 31 32.8852 3.50555 1 2 -4 -31 10.9625 3.57140 1 -2 4 31 9.97207 4.29643 1 1 -4 -31 50.9786 5.81783 1 1 -4 30 74.1208 8.89819 -2 -1 4 31 74.1208 8.89819 1 1 4 -31 45.5191 4.42926 1 0 4 31 157.950 11.2609 -2 0 -4 31 157.950 11.2609 1 0 -4 31 153.432 11.6467 -2 0 4 31 153.432 11.6467 1 -1 -4 -31 63.2757 5.26076 2 -1 -4 32 37.3136 5.85723 -2 1 4 31 37.3136 5.85723 1 2 -4 31 21.4645 3.98244 2 -2 -4 -31 18.0980 2.76888 2 -2 4 -31 14.5014 3.71580 2 3 -5 -31 6.45176 2.11122 1 2 5 30 1.67315 3.54577 -2 -2 -5 31 1.67315 3.54577 1 2 -5 -31 5.59884 2.58316 1 -2 5 31 2.98346 1.57464 1 2 5 -31 5.75484 2.37344 1 1 5 -31 12.9149 2.93631 1 0 5 31 16.3879 3.11772 -2 0 -5 31 16.3879 3.11772 1 0 -5 31 16.4933 3.61132 -2 0 5 31 16.4933 3.61132 1 -1 -5 -31 86.8233 6.44892 2 -1 5 32 192.615 13.3141 -2 1 -5 31 192.615 13.3141 1 4 0 -32 28.9961 3.52778 1 3 0 30 3.76974 2.87526 -2 -3 0 32 3.76974 2.87526 1 2 0 31 1.26033 5.95794 -2 -2 0 32 1.26033 5.95794 1 2 0 -32 13.0332 3.46123 1 1 0 -32 6.17105 2.84134 1 1 0 31 5.66600 6.34902 -2 -1 0 32 5.66600 6.34902 1 0 0 32 399.125 26.6631 -2 0 0 32 399.125 26.6631 1 -1 0 -32 9.83296 4.10129 2 -1 0 33 8.83684 6.01688 -2 1 0 32 8.83684 6.01688 1 2 0 32 43.1760 5.75233 2 -2 0 -32 41.2805 4.65096 2 -2 0 33 103.736 9.00894 -2 2 0 32 103.736 9.00894 1 4 1 29 55.3402 5.66931 -2 -4 -1 32 55.3402 5.66931 1 -4 1 32 1.69514 2.28090 2 4 1 -32 21.4983 3.08268 1 3 1 30 3.69820 2.99989 -2 -3 -1 32 3.69820 2.99989 1 3 -1 30 1.08834 2.52718 -2 -3 1 32 1.08834 2.52718 1 2 1 31 28.9991 6.57281 -2 -2 -1 32 28.9991 6.57281 1 2 -1 -32 11.3406 3.42505 1 2 -1 31 25.3875 5.29853 -2 -2 1 32 25.3875 5.29853 1 1 -1 -32 95.5306 7.87796 1 1 1 31 126.934 10.1457 -2 -1 -1 32 126.934 10.1457 1 1 1 -32 91.3281 7.63090 1 -1 1 32 115.973 8.22417 1 0 1 32 47.8248 5.88408 -2 0 -1 32 47.8248 5.88408 1 0 1 32 46.8428 5.63105 -2 0 -1 32 46.8428 5.63105 1 0 -1 32 46.3144 5.72886 -2 0 1 32 46.3144 5.72886 1 -1 1 33 13.4427 6.31123 -2 1 -1 32 13.4427 6.31123 1 -1 -1 33 15.2160 5.61828 -2 1 1 32 15.2160 5.61828 1 -1 1 -32 9.94230 4.14869 2 2 -1 32 28.2729 4.76011 2 -2 1 -32 42.5171 4.27247 2 -2 -1 33 92.7625 8.29418 -2 2 1 32 92.7625 8.29418 1 4 -2 -32 1.93586 1.99028 1 4 2 29 12.4978 3.92415 -2 -4 -2 32 12.4978 3.92415 1 4 2 -32 -1.7930 1.99207 1 3 2 30 0.94727 1.75570 -2 -3 -2 32 0.94727 1.75570 1 3 -2 30 -2.0632 2.29155 -2 -3 2 32 -2.0632 2.29155 1 2 -2 -32 16.0913 3.61515 1 2 -2 31 41.4989 5.92862 -2 -2 2 32 41.4989 5.92862 1 2 2 -32 19.8913 3.23973 1 1 2 31 17.8548 5.21678 -2 -1 -2 32 17.8548 5.21678 1 1 2 -32 13.3952 3.37309 1 1 -2 31 27.9149 5.72541 -2 -1 2 32 27.9149 5.72541 1 0 2 32 26.6257 4.43811 -2 0 -2 32 26.6257 4.43811 1 0 2 32 23.2203 6.26194 -2 0 -2 32 23.2203 6.26194 1 0 -2 32 28.3751 4.78621 -2 0 2 32 28.3751 4.78621 1 -1 -2 -32 91.0466 6.77481 2 -1 -2 33 185.249 13.4578 -2 1 2 32 185.249 13.4578 1 -1 2 -32 80.2207 7.16246 2 -2 -2 -32 8.92992 2.85539 2 -2 2 -32 10.6642 3.28388 2 3 3 30 91.3699 7.00522 -2 -3 -3 32 91.3699 7.00522 1 3 -3 30 103.048 8.34334 -2 -3 3 32 103.048 8.34334 1 2 -3 -32 26.1183 4.56746 1 2 -3 31 39.1313 5.90476 -2 -2 3 32 39.1313 5.90476 1 2 3 -32 30.8114 3.59710 1 1 -3 -32 7.33366 3.74702 1 1 3 -32 7.62876 2.41975 1 1 -3 31 28.0312 6.96042 -2 -1 3 32 28.0312 6.96042 1 0 3 32 34.3161 4.50119 -2 0 -3 32 34.3161 4.50119 1 0 -3 32 36.2188 5.23700 -2 0 3 32 36.2188 5.23700 1 -1 -3 -32 27.6881 3.65567 2 -2 -3 -32 18.6752 2.89966 2 -2 3 33 45.4217 5.21970 -2 2 -3 32 45.4217 5.21970 1 -2 3 -32 13.8764 3.58947 2 3 4 30 40.6102 4.05236 -2 -3 -4 32 40.6102 4.05236 1 -3 4 -30 40.3939 3.99018 -2 3 -4 -32 40.3939 3.99018 1 -3 -4 -30 42.3515 3.57452 -2 3 4 -32 42.3515 3.57452 1 2 -4 -32 64.1127 5.52648 1 -2 -4 32 26.3421 4.44750 2 -2 4 32 60.7385 5.69164 1 2 4 -32 65.3890 4.99494 1 1 4 -32 87.4459 6.54852 1 1 -4 31 114.155 9.25197 -2 -1 4 32 114.155 9.25197 1 0 4 32 0.76572 1.76382 -2 0 -4 32 0.76572 1.76382 1 0 -4 32 0.72986 4.26874 -2 0 4 32 0.72986 4.26874 1 -1 4 33 18.9296 4.48077 -2 1 -4 32 18.9296 4.48077 1 -1 -4 -32 12.7093 3.26362 2 1 5 31 92.5901 7.28587 -2 -1 -5 32 92.5901 7.28587 1 1 5 -32 38.6142 4.05005 1 0 5 32 40.8366 3.77104 -2 0 -5 32 40.8366 3.77104 1 4 0 -33 1.63342 1.88983 1 2 0 -33 10.6201 3.20524 1 -2 0 33 11.5097 4.10231 1 1 0 -33 20.5534 4.73546 1 1 0 32 29.5150 6.92288 -2 -1 0 33 29.5150 6.92288 1 0 0 33 2.85823 3.19807 -2 0 0 33 2.85823 3.19807 1 -1 0 -33 2.81443 2.96277 2 -2 0 -33 0.02761 2.26396 2 3 1 31 21.9323 3.99996 -2 -3 -1 33 21.9323 3.99996 1 3 -1 31 26.2305 4.06689 -2 -3 1 33 26.2305 4.06689 1 2 -1 -33 84.1668 6.52676 1 -2 1 33 88.6686 6.89038 1 2 1 -33 81.6726 6.39679 1 1 -1 -33 12.5888 3.26746 1 1 -1 32 30.4571 6.76785 -2 -1 1 33 30.4571 6.76785 1 1 1 -33 9.47260 3.73685 1 0 -1 33 24.4104 4.50063 -2 0 1 33 24.4104 4.50063 1 1 -1 33 19.2836 4.32574 1 -1 -1 -33 24.2428 3.95512 2 -1 1 -33 20.5890 4.41328 2 -2 -1 -33 6.63430 2.04398 2 -2 1 -33 7.37884 2.34078 2 3 2 31 14.9203 3.39863 -2 -3 -2 33 14.9203 3.39863 1 -3 2 -31 18.6340 3.04070 -2 3 -2 -33 18.6340 3.04070 1 -3 -2 -31 18.2726 2.81530 -2 3 2 -33 18.2726 2.81530 1 2 -2 -33 21.5627 3.53054 1 2 2 -33 18.2036 3.71108 1 1 -2 -33 23.7072 4.72284 1 1 -2 32 79.7891 8.09277 -2 -1 2 33 79.7891 8.09277 1 1 2 -33 20.6123 3.64118 1 0 -2 33 52.5253 5.45254 -2 0 2 33 52.5253 5.45254 1 -1 -2 -33 3.11872 2.50793 2 -1 2 34 3.83983 4.78462 -2 1 -2 33 3.83983 4.78462 1 2 -2 33 59.9708 6.83114 1 -2 -2 -33 33.3754 3.47413 2 2 2 33 29.5680 4.19507 2 -3 3 -31 31.9657 3.66797 -2 3 -3 -33 31.9657 3.66797 1 3 3 31 37.7248 3.76189 -2 -3 -3 33 37.7248 3.76189 1 -3 -3 -31 36.3997 3.42319 -2 3 3 -33 36.3997 3.42319 1 2 -3 -33 12.8961 3.53527 1 2 3 32 30.7899 4.96877 -2 -2 -3 33 30.7899 4.96877 1 2 3 -33 15.0320 2.81322 1 1 3 -33 42.9311 4.35663 1 -1 -3 -33 15.7054 3.74105 2 -1 3 34 39.0725 5.14395 -2 1 -3 33 39.0725 5.14395 1 1 4 32 35.6018 4.74404 -2 -1 -4 33 35.6018 4.74404 1 1 4 -33 38.7207 4.41056 1 0 4 33 7.13896 2.69989 -2 0 -4 33 7.13896 2.69989 1 -3 0 -32 3.28752 2.55141 -2 3 0 -34 3.28752 2.55141 1 1 0 -34 2.69036 2.98004 1 -3 1 -32 19.4107 2.95990 -2 3 -1 -34 19.4107 2.95990 1 -3 -1 -32 25.0568 2.91293 -2 3 1 -34 25.0568 2.91293 1 2 -1 -34 7.01549 3.03742 1 -2 -1 34 12.4807 4.16987 1 -2 1 34 4.97877 3.38451 2 2 1 -34 10.3742 2.89649 1 1 -1 -34 58.9805 7.94035 1 1 1 33 83.6741 8.05787 -2 -1 -1 34 83.6741 8.05787 1 1 1 -34 41.4956 4.69999 1 -1 1 34 34.8764 5.30094 2 0 -1 34 14.8963 4.94849 -2 0 1 34 14.8963 4.94849 1 2 -2 -34 86.7109 6.39306 1 -2 -2 34 84.5651 6.29692 1 -2 2 34 52.1923 5.20584 2 2 2 -34 78.4768 6.13978 1 1 2 33 29.9016 5.51618 -2 -1 -2 34 29.9016 5.51618 1 1 2 -34 15.1236 3.70897 1 0 2 34 19.2342 3.57170 -2 0 -2 34 19.2342 3.57170 1 1 3 33 54.2574 5.82493 -2 -1 -3 34 54.2574 5.82493 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 78813 _shelx_res_file ; TITL jtm859_4_a.res in P2(1)/n jtm859_5.res created by SHELXL-2016/6 at 08:42:11 on 16-Oct-2017 REM Old TITL jtm859_4 in P2(1) REM SHELXT solution in P2(1)/n REM R1 0.244, Rweak 0.070, Alpha 0.148, Orientation as input REM Formula found by SHELXT: C23 Br2 N4 O4 CELL 1.54178 7.5971 9.9501 28.5690 90.000 95.086 90.000 ZERR 8.000 0.0004 0.0005 0.0013 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H BR N O UNIT 80 64 8 24 16 TEMP -123 SIZE 0.04 0.085 0.252 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 CONF EQIV $1 -x+1/2, y-1/2, -z+1/2 HTAB C4 O1_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C9 Br1_$2 EQIV $3 -x+3/2, y-1/2, -z+1/2 EQIV $4 -x+3/2, y+1/2, -z+1/2 HTAB C18 Br1_$4 HTAB C18 O4_$3 ACTA 136 WGHT 0.053500 28.390900 BASF 0.32874 FVAR 0.35181 BR1 3 0.566981 0.145432 0.473799 11.00000 0.06873 0.03635 = 0.02937 0.00506 0.00516 0.00460 O1 5 0.418935 0.460896 0.221306 11.00000 0.07087 0.05053 = 0.03350 0.00712 0.00560 0.00787 O2 5 0.273015 0.275217 0.216570 11.00000 0.07625 0.07099 = 0.03248 -0.00835 -0.01727 -0.01426 N1 4 0.648185 0.461835 0.396833 11.00000 0.03819 0.02655 = 0.02272 -0.00615 0.00429 -0.00679 N2 4 0.661406 0.391022 0.437366 11.00000 0.03420 0.03731 = 0.02907 -0.00118 0.00471 0.00461 N3 4 0.365593 0.354813 0.238266 11.00000 0.03036 0.03805 = 0.03310 0.00379 0.00219 0.00574 C1 1 0.581919 0.276750 0.427404 11.00000 0.04249 0.02342 = 0.02662 -0.00049 0.00285 0.00948 C2 1 0.513349 0.265793 0.380220 11.00000 0.02143 0.02456 = 0.03541 -0.00357 0.01424 0.00325 C3 1 0.421508 0.171996 0.351377 11.00000 0.02805 0.01724 = 0.03757 -0.00159 0.00221 0.00493 AFIX 43 H3 2 0.391544 0.087488 0.363954 11.00000 -1.20000 AFIX 0 C4 1 0.374749 0.199503 0.305993 11.00000 0.01884 0.02303 = 0.03220 -0.00750 0.00397 -0.00658 AFIX 43 H4 2 0.312848 0.134651 0.286457 11.00000 -1.20000 AFIX 0 C5 1 0.418664 0.326707 0.287344 11.00000 0.02030 0.02044 = 0.03277 -0.00273 0.00522 0.00178 C6 1 0.509780 0.425677 0.313398 11.00000 0.01931 0.02135 = 0.03803 -0.00044 0.00336 0.00838 AFIX 43 H6 2 0.540098 0.509440 0.300322 11.00000 -1.20000 AFIX 0 C7 1 0.554386 0.391990 0.361290 11.00000 0.01035 0.02705 = 0.03014 -0.00620 0.00365 0.00855 C8 1 0.703030 0.603759 0.396864 11.00000 0.04231 0.02935 = 0.03469 -0.00818 0.00160 -0.01155 AFIX 23 H8A 2 0.816224 0.613203 0.416593 11.00000 -1.20000 H8B 2 0.724045 0.630139 0.364414 11.00000 -1.20000 AFIX 0 C9 1 0.574867 0.694732 0.414155 11.00000 0.03661 0.02432 = 0.02991 -0.00463 0.00428 0.00451 AFIX 43 H9 2 0.537239 0.676754 0.444368 11.00000 -1.20000 AFIX 0 C10 1 0.507732 0.797740 0.392075 11.00000 0.04136 0.03900 = 0.05278 0.00896 0.00473 0.00026 AFIX 93 H10A 2 0.541706 0.819364 0.361763 11.00000 -1.20000 H10B 2 0.424128 0.852263 0.406066 11.00000 -1.20000 AFIX 0 BR2 3 0.294787 0.942365 0.029963 11.00000 0.03710 0.03423 = 0.02877 0.00485 -0.00417 -0.00087 O3 5 0.729675 0.734697 0.279147 11.00000 0.05773 0.04466 = 0.02764 0.00726 -0.00476 0.02163 O4 5 0.646162 0.937528 0.287737 11.00000 0.07007 0.04053 = 0.03090 -0.01237 -0.00066 -0.00537 N4 4 0.522660 0.648228 0.105054 11.00000 0.03708 0.02950 = 0.02789 -0.00124 -0.00290 -0.00078 N5 4 0.444425 0.701579 0.065272 11.00000 0.03763 0.03856 = 0.01961 -0.00184 -0.00069 -0.00065 N6 4 0.659049 0.837251 0.263874 11.00000 0.03165 0.03884 = 0.02483 0.00788 -0.00572 -0.00056 C11 1 0.399900 0.827781 0.075400 11.00000 0.02151 0.03635 = 0.02418 -0.00053 -0.00258 -0.01443 C12 1 0.449362 0.858717 0.123728 11.00000 0.02838 0.03017 = 0.02998 0.00643 -0.00048 -0.00262 C13 1 0.432497 0.970697 0.152751 11.00000 0.03043 0.02426 = 0.03296 0.00295 0.00016 -0.00215 AFIX 43 H13 2 0.374507 1.050083 0.141120 11.00000 -1.20000 AFIX 0 C14 1 0.501367 0.961723 0.197665 11.00000 0.02441 0.02784 = 0.03696 0.00078 0.00406 -0.01154 AFIX 43 H14 2 0.494502 1.036167 0.218244 11.00000 -1.20000 AFIX 0 C15 1 0.584229 0.841023 0.214260 11.00000 0.03652 0.03877 = 0.01794 0.00427 0.00198 -0.00471 C16 1 0.598739 0.729381 0.187879 11.00000 0.02934 0.02631 = 0.02541 0.00838 0.00095 -0.00486 AFIX 43 H16 2 0.652562 0.649426 0.200420 11.00000 -1.20000 AFIX 0 C17 1 0.529510 0.739008 0.140954 11.00000 0.02650 0.02076 = 0.03043 -0.00659 0.00485 -0.00950 C18 1 0.597532 0.513573 0.104383 11.00000 0.04352 0.02832 = 0.03306 -0.00549 0.00442 -0.00327 AFIX 23 H18A 2 0.673729 0.507640 0.078086 11.00000 -1.20000 H18B 2 0.673545 0.499252 0.133934 11.00000 -1.20000 AFIX 0 C19 1 0.468170 0.407348 0.099368 11.00000 0.05014 0.03365 = 0.04808 -0.00600 0.00242 0.00203 AFIX 43 H19 2 0.392167 0.395215 0.123703 11.00000 -1.20000 AFIX 0 C20 1 0.449981 0.327028 0.063182 11.00000 0.05315 0.04119 = 0.05511 -0.01360 -0.01753 0.00492 AFIX 93 H20A 2 0.524262 0.336954 0.038349 11.00000 -1.20000 H20B 2 0.362454 0.258601 0.061658 11.00000 -1.20000 AFIX 0 HKLF 5 REM jtm859_4_a.res in P2(1)/n REM R1 = 0.0792 for 7050 Fo > 4sig(Fo) and 0.0852 for all 7639 data REM 290 parameters refined using 0 restraints END WGHT 0.0535 28.3774 REM Highest difference peak 1.300, deepest hole -1.219, 1-sigma level 0.196 Q1 1 0.6857 0.4471 0.4657 11.00000 0.05 1.30 Q2 1 0.4272 0.6457 0.0255 11.00000 0.05 1.05 Q3 1 0.4358 0.2654 0.4717 11.00000 0.05 0.88 Q4 1 0.4860 0.2086 0.4465 11.00000 0.05 0.85 Q5 1 0.7149 0.1511 0.4731 11.00000 0.05 0.84 ; _shelx_res_checksum 99405 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Br Br1 0.5670(2) 0.14543(15) 0.47380(4) 0.0448(5) Uani d 1 O O1 0.4189(17) 0.4609(11) 0.2213(3) 0.052(3) Uani d 1 O O2 0.2730(18) 0.2752(12) 0.2166(3) 0.061(3) Uani d 1 N N1 0.6482(14) 0.4618(10) 0.3968(3) 0.029(3) Uani d 1 N N2 0.6614(15) 0.3910(11) 0.4374(3) 0.033(3) Uani d 1 N N3 0.3656(16) 0.3548(12) 0.2383(3) 0.034(3) Uani d 1 C C1 0.582(2) 0.2767(12) 0.4274(4) 0.031(3) Uani d 1 C C2 0.5133(18) 0.2658(12) 0.3802(4) 0.026(3) Uani d 1 C C3 0.4215(18) 0.1720(13) 0.3514(4) 0.028(3) Uani d 1 H H3 0.391544 0.087488 0.363954 0.033 Uiso calc 1 C C4 0.3747(17) 0.1995(12) 0.3060(4) 0.025(3) Uani d 1 H H4 0.312848 0.134651 0.286457 0.030 Uiso calc 1 C C5 0.4187(16) 0.3267(13) 0.2873(4) 0.024(3) Uani d 1 C C6 0.5098(16) 0.4257(12) 0.3134(4) 0.026(3) Uani d 1 H H6 0.540098 0.509440 0.300322 0.031 Uiso calc 1 C C7 0.5544(15) 0.3920(12) 0.3613(4) 0.022(3) Uani d 1 C C8 0.703(2) 0.6038(13) 0.3969(4) 0.036(3) Uani d 1 H H8A 0.816224 0.613203 0.416593 0.043 Uiso calc 1 H H8B 0.724045 0.630139 0.364414 0.043 Uiso calc 1 C C9 0.5749(19) 0.6947(12) 0.4142(4) 0.030(3) Uani d 1 H H9 0.537239 0.676754 0.444368 0.036 Uiso calc 1 C C10 0.508(2) 0.7977(14) 0.3921(5) 0.044(4) Uani d 1 H H10A 0.541706 0.819364 0.361763 0.053 Uiso calc 1 H H10B 0.424128 0.852263 0.406066 0.053 Uiso calc 1 Br Br2 0.29479(19) 0.94236(14) 0.02996(4) 0.0338(4) Uani d 1 O O3 0.7297(14) 0.7347(10) 0.2791(3) 0.044(3) Uani d 1 O O4 0.6462(16) 0.9375(10) 0.2877(3) 0.047(3) Uani d 1 N N4 0.5227(15) 0.6482(11) 0.1051(3) 0.032(3) Uani d 1 N N5 0.4444(16) 0.7016(11) 0.0653(3) 0.032(3) Uani d 1 N N6 0.6590(16) 0.8373(12) 0.2639(3) 0.032(3) Uani d 1 C C11 0.3999(17) 0.8278(14) 0.0754(4) 0.028(3) Uani d 1 C C12 0.4494(18) 0.8587(13) 0.1237(4) 0.030(3) Uani d 1 C C13 0.4325(18) 0.9707(13) 0.1528(4) 0.029(3) Uani d 1 H H13 0.374507 1.050083 0.141120 0.035 Uiso calc 1 C C14 0.5014(17) 0.9617(13) 0.1977(4) 0.030(3) Uani d 1 H H14 0.494502 1.036167 0.218244 0.036 Uiso calc 1 C C15 0.5842(18) 0.8410(14) 0.2143(4) 0.031(3) Uani d 1 C C16 0.5987(18) 0.7294(13) 0.1879(4) 0.027(3) Uani d 1 H H16 0.652562 0.649426 0.200420 0.033 Uiso calc 1 C C17 0.5295(18) 0.7390(12) 0.1410(4) 0.026(3) Uani d 1 C C18 0.598(2) 0.5136(13) 0.1044(4) 0.035(3) Uani d 1 H H18A 0.673729 0.507640 0.078086 0.042 Uiso calc 1 H H18B 0.673545 0.499252 0.133934 0.042 Uiso calc 1 C C19 0.468(2) 0.4073(14) 0.0994(5) 0.044(4) Uani d 1 H H19 0.392167 0.395215 0.123703 0.053 Uiso calc 1 C C20 0.450(2) 0.3270(16) 0.0632(5) 0.051(4) Uani d 1 H H20A 0.524262 0.336954 0.038349 0.061 Uiso calc 1 H H20B 0.362454 0.258601 0.061658 0.061 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0687(11) 0.0364(8) 0.0294(6) 0.0046(9) 0.0052(8) 0.0051(5) O1 0.071(8) 0.051(7) 0.033(4) 0.008(6) 0.006(5) 0.007(4) O2 0.076(9) 0.071(8) 0.032(5) -0.014(8) -0.017(6) -0.008(5) N1 0.038(7) 0.027(6) 0.023(4) -0.007(6) 0.004(4) -0.006(4) N2 0.034(7) 0.037(7) 0.029(5) 0.005(6) 0.005(5) -0.001(4) N3 0.030(6) 0.038(7) 0.033(5) 0.006(7) 0.002(5) 0.004(5) C1 0.042(8) 0.023(7) 0.027(5) 0.009(7) 0.003(6) 0.000(5) C2 0.021(6) 0.025(6) 0.035(6) 0.003(7) 0.014(5) -0.004(5) C3 0.028(7) 0.017(6) 0.038(6) 0.005(6) 0.002(6) -0.002(5) C4 0.019(6) 0.023(6) 0.032(5) -0.007(6) 0.004(5) -0.008(4) C5 0.020(7) 0.020(6) 0.033(6) 0.002(6) 0.005(5) -0.003(5) C6 0.019(7) 0.021(6) 0.038(6) 0.008(6) 0.003(5) 0.000(5) C7 0.010(6) 0.027(6) 0.030(5) 0.009(6) 0.004(5) -0.006(4) C8 0.042(9) 0.029(7) 0.035(6) -0.012(7) 0.002(6) -0.008(5) C9 0.037(8) 0.024(6) 0.030(5) 0.005(7) 0.004(6) -0.005(5) C10 0.041(9) 0.039(9) 0.053(8) 0.000(8) 0.005(8) 0.009(6) Br2 0.0371(7) 0.0342(7) 0.0288(5) -0.0009(7) -0.0042(6) 0.0048(5) O3 0.058(7) 0.045(6) 0.028(4) 0.022(6) -0.005(5) 0.007(4) O4 0.070(7) 0.041(6) 0.031(4) -0.005(6) -0.001(5) -0.012(4) N4 0.037(7) 0.030(6) 0.028(5) -0.001(6) -0.003(4) -0.001(4) N5 0.038(7) 0.039(6) 0.020(4) -0.001(6) -0.001(5) -0.002(4) N6 0.032(7) 0.039(7) 0.025(4) -0.001(6) -0.006(5) 0.008(5) C11 0.022(6) 0.036(8) 0.024(5) -0.014(7) -0.003(5) -0.001(5) C12 0.028(7) 0.030(7) 0.030(5) -0.003(7) 0.000(5) 0.006(5) C13 0.030(7) 0.024(6) 0.033(6) -0.002(7) 0.000(5) 0.003(5) C14 0.024(7) 0.028(7) 0.037(6) -0.012(7) 0.004(5) 0.001(5) C15 0.037(8) 0.039(8) 0.018(5) -0.005(7) 0.002(5) 0.004(5) C16 0.029(7) 0.026(6) 0.025(5) -0.005(7) 0.001(5) 0.008(5) C17 0.026(7) 0.021(6) 0.030(5) -0.010(6) 0.005(5) -0.007(5) C18 0.044(9) 0.028(7) 0.033(6) -0.003(7) 0.004(6) -0.005(5) C19 0.050(10) 0.034(8) 0.048(7) 0.002(8) 0.002(7) -0.006(6) C20 0.053(10) 0.041(8) 0.055(8) 0.005(10) -0.018(8) -0.014(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 N2 N1 C7 111.3(10) N2 N1 C8 120.0(9) C7 N1 C8 127.8(10) C1 N2 N1 105.6(9) O2 N3 O1 123.9(11) O2 N3 C5 118.3(11) O1 N3 C5 117.9(11) N2 C1 C2 113.6(11) N2 C1 Br1 120.6(9) C2 C1 Br1 125.8(10) C3 C2 C1 138.1(12) C3 C2 C7 119.1(11) C1 C2 C7 102.9(11) C4 C3 C2 120.8(12) C4 C3 H3 119.6 C2 C3 H3 119.6 C3 C4 C5 119.5(11) C3 C4 H4 120.3 C5 C4 H4 120.3 C6 C5 C4 123.7(11) C6 C5 N3 117.8(11) C4 C5 N3 118.6(11) C5 C6 C7 114.6(11) C5 C6 H6 122.7 C7 C6 H6 122.7 N1 C7 C2 106.5(10) N1 C7 C6 131.0(11) C2 C7 C6 122.5(11) C9 C8 N1 113.6(12) C9 C8 H8A 108.8 N1 C8 H8A 108.8 C9 C8 H8B 108.8 N1 C8 H8B 108.8 H8A C8 H8B 107.7 C10 C9 C8 125.5(13) C10 C9 H9 117.2 C8 C9 H9 117.2 C9 C10 H10A 120.0 C9 C10 H10B 120.0 H10A C10 H10B 120.0 N5 N4 C17 111.0(10) N5 N4 C18 119.7(9) C17 N4 C18 129.1(10) C11 N5 N4 106.8(9) O3 N6 O4 122.8(10) O3 N6 C15 119.0(11) O4 N6 C15 118.2(11) N5 C11 C12 111.1(11) N5 C11 Br2 121.8(8) C12 C11 Br2 127.1(10) C13 C12 C17 121.7(10) C13 C12 C11 135.4(12) C17 C12 C11 102.9(11) C14 C13 C12 117.6(12) C14 C13 H13 121.2 C12 C13 H13 121.2 C13 C14 C15 119.9(12) C13 C14 H14 120.0 C15 C14 H14 120.0 C16 C15 C14 124.4(10) C16 C15 N6 118.0(12) C14 C15 N6 117.6(11) C15 C16 C17 115.8(12) C15 C16 H16 122.1 C17 C16 H16 122.1 N4 C17 C16 131.4(12) N4 C17 C12 108.1(10) C16 C17 C12 120.5(11) C19 C18 N4 114.3(12) C19 C18 H18A 108.7 N4 C18 H18A 108.7 C19 C18 H18B 108.7 N4 C18 H18B 108.7 H18A C18 H18B 107.6 C20 C19 C18 123.5(16) C20 C19 H19 118.3 C18 C19 H19 118.3 C19 C20 H20A 120.0 C19 C20 H20B 120.0 H20A C20 H20B 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C1 1.872(12) O1 N3 1.244(15) O2 N3 1.195(15) N1 N2 1.352(13) N1 C7 1.376(14) N1 C8 1.472(16) N2 C1 1.307(16) N3 C5 1.451(15) C1 C2 1.406(17) C2 C3 1.391(18) C2 C7 1.413(17) C3 C4 1.342(16) C3 H3 0.9500 C4 C5 1.424(17) C4 H4 0.9500 C5 C6 1.383(17) C6 C7 1.420(15) C6 H6 0.9500 C8 C9 1.448(19) C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.285(18) C9 H9 0.9500 C10 H10A 0.9500 C10 H10B 0.9500 Br2 C11 1.854(12) O3 N6 1.216(14) O4 N6 1.217(14) N4 N5 1.344(14) N4 C17 1.364(15) N4 C18 1.456(17) N5 C11 1.339(17) N6 C15 1.480(13) C11 C12 1.432(15) C12 C13 1.402(17) C12 C17 1.407(18) C13 C14 1.345(16) C13 H13 0.9500 C14 C15 1.418(19) C14 H14 0.9500 C15 C16 1.352(18) C16 C17 1.399(16) C16 H16 0.9500 C18 C19 1.44(2) C18 H18A 0.9900 C18 H18B 0.9900 C19 C20 1.304(19) C19 H19 0.9500 C20 H20A 0.9500 C20 H20B 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C4 H4 O1 2_545 0.95 2.46 3.304(16) 147 C18 H18B O4 2_645 0.99 2.59 3.578(16) 174 C9 H9 Br1 3_666 0.95 3.09 3.814(11) 134 C18 H18A Br1 2_655 0.99 2.91 3.770(14) 146 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 C7 N1 N2 C1 1.8(14) C8 N1 N2 C1 171.7(12) N1 N2 C1 C2 0.3(15) N1 N2 C1 Br1 -179.8(9) N2 C1 C2 C3 179.7(15) Br1 C1 C2 C3 0(3) N2 C1 C2 C7 -2.0(16) Br1 C1 C2 C7 178.0(10) C1 C2 C3 C4 179.1(16) C7 C2 C3 C4 1.1(19) C2 C3 C4 C5 0(2) C3 C4 C5 C6 1(2) C3 C4 C5 N3 -179.5(12) O2 N3 C5 C6 -173.3(12) O1 N3 C5 C6 6.5(17) O2 N3 C5 C4 6.8(18) O1 N3 C5 C4 -173.4(12) C4 C5 C6 C7 -1.2(18) N3 C5 C6 C7 178.9(10) N2 N1 C7 C2 -3.0(13) C8 N1 C7 C2 -172.0(12) N2 N1 C7 C6 -179.2(12) C8 N1 C7 C6 12(2) C3 C2 C7 N1 -178.4(11) C1 C2 C7 N1 2.9(13) C3 C2 C7 C6 -1.8(18) C1 C2 C7 C6 179.5(12) C5 C6 C7 N1 177.5(12) C5 C6 C7 C2 1.8(17) N2 N1 C8 C9 -77.9(15) C7 N1 C8 C9 90.1(14) N1 C8 C9 C10 -125.4(16) C17 N4 N5 C11 -0.1(15) C18 N4 N5 C11 -175.7(12) N4 N5 C11 C12 -0.4(15) N4 N5 C11 Br2 177.7(9) N5 C11 C12 C13 -178.5(15) Br2 C11 C12 C13 3(2) N5 C11 C12 C17 0.7(15) Br2 C11 C12 C17 -177.3(10) C17 C12 C13 C14 2(2) C11 C12 C13 C14 -178.6(14) C12 C13 C14 C15 -1(2) C13 C14 C15 C16 -1(2) C13 C14 C15 N6 179.5(12) O3 N6 C15 C16 -0.3(18) O4 N6 C15 C16 -180.0(13) O3 N6 C15 C14 179.4(12) O4 N6 C15 C14 -0.2(18) C14 C15 C16 C17 2(2) N6 C15 C16 C17 -178.6(11) N5 N4 C17 C16 -179.5(14) C18 N4 C17 C16 -4(2) N5 N4 C17 C12 0.6(15) C18 N4 C17 C12 175.6(13) C15 C16 C17 N4 179.5(13) C15 C16 C17 C12 -1(2) C13 C12 C17 N4 178.6(12) C11 C12 C17 N4 -0.8(14) C13 C12 C17 C16 -1(2) C11 C12 C17 C16 179.3(13) N5 N4 C18 C19 -71.9(15) C17 N4 C18 C19 113.4(15) N4 C18 C19 C20 116.0(16) _cod_database_fobs_code 1548684