#------------------------------------------------------------------------------ #$Date: 2023-01-25 10:34:33 +0200 (Wed, 25 Jan 2023) $ #$Revision: 280578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243844.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_2243844 loop_ _publ_author_name 'Moon, Dohyun' 'Jeon, Sunghwan' 'Lim, Woo Taik' 'Ryoo, Keon Sang' 'Choi, Jong-Ha' _publ_section_title ; Crystal structure of diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) (3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) tetrabromide dihydrate, [Cu(C~22~H~44~N~4~)(H~2~O)~2~][Cu(C~22~H~44~N~4~)]Br~4~·2H~2~O ; _journal_coeditor_code WM5611 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 677 _journal_page_last 680 _journal_paper_doi 10.1107/S205698902100551X _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Cu (C22 H44 N4)] Br2, 2H2 O' _chemical_formula_moiety 'C22 H44 Cu N4 2+, 2(Br -), 2(H2 O)' _chemical_formula_sum 'C22 H48 Br2 Cu N4 O2' _chemical_formula_weight 624.00 _chemical_name_systematic 'Diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) (3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) tetrabromide dihydrate' _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 _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 97.02(3) _cell_angle_beta 92.91(3) _cell_angle_gamma 111.31(3) _cell_formula_units_Z 2 _cell_length_a 8.0800(16) _cell_length_b 10.380(2) _cell_length_c 17.511(4) _cell_measurement_reflns_used 74723 _cell_measurement_temperature 220(2) _cell_measurement_theta_max 33.679 _cell_measurement_theta_min 0.350 _cell_volume 1350.8(6) _computing_cell_refinement ; HKL3000sm (Otwinowski et al., 2003) ; _computing_data_collection ; PAL BL2D-SMDC (Shin et al., 2016) ; _computing_data_reduction ; HKL3000sm (Otwinowski et al., 2003) ; _computing_molecular_graphics ; DIAMOND 4 (Putz & Brandenburg, 2014) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 220(2) _diffrn_measured_fraction_theta_full 0.954 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'Rayonix MX225HS CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.610 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_unetI/netI 0.0341 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 14201 _diffrn_reflns_theta_full 21.469 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 1.828 _diffrn_source 'PLSII 2D bending magnet' _exptl_absorpt_coefficient_mu 2.532 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; (HKL3000sm Scalepack; Otwinowski et al., 2003) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.534 _exptl_crystal_description octahedron _exptl_crystal_F_000 646 _exptl_crystal_size_max 0.075 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_min 0.069 _refine_diff_density_max 0.831 _refine_diff_density_min -1.030 _refine_ls_extinction_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/3 (Sheldrick 2018) ; _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 7233 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0561 _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^)+(0.0966P)^2^+0.5261P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1655 _refine_ls_wR_factor_ref 0.1762 _reflns_number_gt 5311 _reflns_number_total 7233 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5611sup1.cif _cod_data_source_block I _cod_depositor_comments ; 2023-01-25 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C44 H96 Br4 Cu2 N8 O4' _cod_original_formula_weight 1248.00 _cod_original_formula_moiety 'C22 H48 Cu N4 O2 2+, C22 H44 Cu N4 2+, 4(Br -), 2(H2 O)' _cod_original_formula_iupac '[Cu (C22 H44 N4) (H2 O)2] [Cu (C22 H44 N4)] Br4, 2H2 O' _cod_original_formula_units_Z 1 _cod_original_cell_volume 1350.8(5) _cod_database_code 2243844 _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 0.833 _shelx_estimated_absorpt_t_max 0.845 _shelx_hkl_file ; 0 0 218820.50 443.513 1 0 0 -217068.30 566.469 1 0 0 3 605.742 17.4997 1 0 0 -3 533.902 26.7394 1 0 0 4 9871.05 255.115 1 0 0 -4 9266.02 200.909 1 0 0 5 20.0999 1.79748 1 0 0 -5 20.3267 1.85628 1 0 0 6 1664.22 39.5799 1 0 0 -6 1546.56 37.279 1 0 0 7 3436.89 71.5252 1 0 0 -7 3323.42 69.6162 1 0 0 8 2056.61 48.0795 1 0 0 -8 2045.43 47.5555 1 0 0 9 1395.99 32.8295 1 0 0 -9 1369.10 33.1049 1 0 0 10 4105.31 86.9901 1 0 0 -10 3973.62 98.1493 1 0 0 11 1216.34 29.7321 1 0 0 -11 1188.36 34.1012 1 0 0 12 1194.45 30.8141 1 0 0 -12 1158.47 29.5122 1 0 0 13 1232.84 29.2821 1 0 0 -13 1223.01 28.5868 1 0 0 14 1014.48 25.7062 1 0 0 -14 1015.94 24.7821 1 0 0 15 10.4844 5.28598 1 0 0 -15 14.7635 4.97954 1 0 0 16 846.035 24.1509 1 0 0 -16 853.894 21.943 1 0 0 17 377.538 14.792 1 0 0 -17 388.739 14.6634 1 0 0 18 602.742 19.2262 1 0 0 -18 602.174 17.5232 1 0 0 19 21.0871 6.58205 1 0 0 -19 16.0563 6.22271 1 0 0 20 13.2463 6.594 1 0 0 -20 9.16666 6.36921 1 0 0 21 26.5428 6.99764 1 0 0 -21 37.8597 6.80461 1 0 0 22 28.4338 7.48762 1 0 0 -22 19.0463 7.21622 1 0 0 23-6.14316 7.29913 1 0 0 -23-2.77433 7.40647 1 0 1 -24 70.4595 7.95122 1 0 -1 24 62.8783 8.2438 1 0 1 -23 0.91923 7.21915 1 0 -1 23 0.15849 7.27462 1 0 1 -22 61.4162 6.84381 1 0 -1 22 73.1993 7.05284 1 0 1 -21-2.53692 6.32268 1 0 -1 21 9.37013 6.27555 1 0 1 -20 73.702 8.15916 1 0 -1 20 77.2793 8.37968 1 0 1 -19 44.228 6.01032 1 0 -1 19 35.6652 5.59641 1 0 1 -18 229.74 11.0702 1 0 -1 18 233.134 10.6299 1 0 1 -17 149.564 8.55739 1 0 -1 17 149.769 10.4113 1 0 1 -16 398.339 13.5039 1 0 -1 16 415.691 17.847 1 0 1 -15 185.278 8.67599 1 0 -1 15 172.712 10.1094 1 0 1 -14 175.554 9.56156 1 0 -1 14 159.921 9.22917 1 0 1 -13 566.963 18.5066 1 0 -1 13 584.642 19.267 1 0 1 -12 4.14411 5.41837 1 0 -1 12 0.97508 5.79511 1 0 1 -11 2380.03 71.8421 1 0 -1 11 2421.77 60.6839 1 0 1 -10 2251.80 102.037 1 0 -1 10 2244.70 58.8252 1 0 1 -9 110.374 11.4926 1 0 -1 9 128.907 6.842 1 0 1 -824720.70 496.822 1 0 -1 824596.70 611.594 1 0 1 -7 4280.63 120.265 1 0 -1 7 4362.60 100.264 1 0 1 -6 940.086 27.7754 1 0 -1 6 948.504 28.4373 1 0 1 -5 2415.03 50.9049 1 0 -1 5 2469.78 59.3336 1 0 1 -4 842.965 21.1908 1 0 -1 4 893.297 21.5575 1 0 1 -3 59.5799 2.61195 1 0 -1 3 63.6692 2.66526 1 0 1 -2 29.5463 1.43102 1 0 -1 2 30.0666 1.74477 1 0 1 -1 141.837 3.68867 1 0 -1 1 144.803 3.96799 1 0 1 016245.90 521.755 1 0 -1 014015.20 455.302 1 0 1 1 47.3086 2.01273 1 0 -1 -1 40.0571 2.14441 1 0 1 229848.50 692.304 1 0 -1 -226152.60 620.643 1 0 1 3 6892.98 177.463 1 0 -1 -3 6726.78 140.046 1 0 1 4 597.282 15.8605 1 0 -1 -4 567.853 15.2515 1 0 1 5 3677.94 72.5897 1 0 -1 -5 3551.27 70.697 1 0 1 6 10.4889 2.34136 1 0 -1 -6 11.0743 2.21863 1 0 1 7 97.3271 4.80204 1 0 -1 -7 99.9589 4.87078 1 0 1 8 228.02 9.26803 1 0 -1 -8 230.081 10.3138 1 0 1 9 2694.27 57.8328 1 0 -1 -9 2576.23 64.3823 1 0 1 10 3387.56 72.5463 1 0 -1 -10 3236.53 81.4338 1 0 1 11 302.66 10.5911 1 0 -1 -11 303.244 10.1326 1 0 1 12 460.196 14.8699 1 0 -1 -12 444.545 14.3917 1 0 1 13 219.132 9.48433 1 0 -1 -13 223.337 9.01712 1 0 1 14 528.615 16.1754 1 0 -1 -14 503.656 15.9455 1 0 1 15 195.745 9.83622 1 0 -1 -15 188.068 8.95719 1 0 1 16 624.061 20.2828 1 0 -1 -16 613.962 19.2421 1 0 1 17 48.5214 6.92732 1 0 -1 -17 47.0556 5.9334 1 0 1 18 462.804 18.1978 1 0 -1 -18 493.704 17.5546 1 0 1 19 42.4461 7.19652 1 0 -1 -19 41.5968 7.01773 1 0 1 20 29.3226 6.99539 1 0 -1 -20 33.5591 6.76477 1 0 1 21 38.6043 8.08867 1 0 -1 -21 40.0523 7.46455 1 0 1 22 4.8329 5.25933 1 0 -1 -22 1.9064 5.9366 1 0 1 23 11.7127 8.20506 1 0 -1 -23 11.5364 7.96711 1 0 2 -24 20.7868 11.4127 1 0 -2 24 24.3041 7.89529 1 0 2 -23 20.2989 9.82403 1 0 -2 23 11.6912 7.21307 1 0 2 -22 17.873 6.61119 1 0 -2 22 13.9215 5.44854 1 0 2 -21 41.4947 9.21846 1 0 -2 21 38.1334 7.19395 1 0 2 -20 60.462 7.05592 1 0 -2 20 56.4634 6.94328 1 0 2 -19 185.436 9.35849 1 0 -2 19 183.387 8.72099 1 0 2 -18 135.688 9.71206 1 0 -2 18 135.508 8.54553 1 0 2 -17 20.8971 9.35175 1 0 -2 17 14.8454 6.11904 1 0 2 -16 321.333 13.0311 1 0 -2 16 317.976 12.2783 1 0 2 -15 568.829 18.6034 1 0 -2 15 583.392 18.3908 1 0 2 -14 73.4741 5.87224 1 0 -2 14 70.2482 6.39713 1 0 2 -13 247.44 14.2316 1 0 -2 13 246.688 10.6626 1 0 2 -12 130.316 10.2875 1 0 -2 12 139.485 6.97534 1 0 2 -11 285.393 10.5661 1 0 -2 11 287.108 10.2018 1 0 2 -10 24.0062 3.86829 1 0 -2 10 21.5859 3.76486 1 0 2 -9 186.126 7.57577 1 0 -2 9 193.425 7.50645 1 0 2 -814866.60 268.323 1 0 -2 815347.30 275.162 1 0 2 -7 171.038 6.65467 1 0 -2 7 182.345 6.77189 1 0 2 -617435.80 355.305 1 0 -2 617808.90 360.562 1 0 2 -5 446.91 12.2865 1 0 -2 5 459.431 12.1191 1 0 2 -4 1673.50 35.813 1 0 -2 4 1692.85 35.813 1 0 2 -3 182.767 5.29497 1 0 -2 3 191.345 5.5259 1 0 2 -2 7436.78 148.696 1 0 -2 2 7470.38 152.048 1 0 2 -1 13.182 0.7902 1 0 -2 1 13.7926 0.85306 1 0 2 0 1298.69 35.8104 1 0 -2 0 1335.26 37.6468 1 0 2 1 2911.91 108.542 1 0 -2 -1 2870.02 74.1761 1 0 2 2 8024.59 197.533 1 0 -2 -2 8554.45 170.23 1 0 2 3 7.85333 1.29751 1 0 -2 -3 6.20462 1.42433 1 0 2 4 2882.03 57.245 1 0 -2 -4 2815.31 56.2831 1 0 2 5 4028.36 109.171 1 0 -2 -5 4003.81 88.8311 1 0 2 6 612.343 16.7287 1 0 -2 -6 586.467 16.1353 1 0 2 7 1334.52 30.7349 1 0 -2 -7 1297.22 29.9531 1 0 2 8 215.448 12.6122 1 0 -2 -8 209.941 8.37532 1 0 2 9 3213.58 66.8328 1 0 -2 -9 3178.96 65.2564 1 0 2 10 4815.20 112.22 1 0 -2 -10 4707.80 94.4077 1 0 2 11 893.579 23.3286 1 0 -2 -11 854.682 21.9894 1 0 2 12 557.085 17.6394 1 0 -2 -12 546.822 16.9029 1 0 2 13 644.499 18.3601 1 0 -2 -13 639.72 17.6276 1 0 2 14 680.245 20.0134 1 0 -2 -14 686.074 19.7666 1 0 2 15 74.3598 7.5912 1 0 -2 -15 79.9002 6.54883 1 0 2 16 104.745 7.29747 1 0 -2 -16 92.1252 7.006 1 0 2 17-4.16719 6.62869 1 0 -2 -17 10.2035 6.42442 1 0 2 18 396.491 16.8958 1 0 -2 -18 405.412 15.2931 1 0 2 19 54.8602 7.51974 1 0 -2 -19 62.6003 8.05228 1 0 2 20 107.709 9.63391 1 0 -2 -20 85.74 9.57193 1 0 2 21 2.70194 7.16145 1 0 -2 -21-1.93246 6.98657 1 0 2 22 5.94141 7.97565 1 0 -2 -22 4.07744 7.46485 1 0 2 23 -8.4762 9.00231 1 0 -2 -23 5.89437 8.80745 1 0 3 -24 1.04867 6.69983 1 0 -3 24-2.46354 6.59164 1 0 3 -23 5.9924 7.22477 1 0 -3 23 0.78564 7.69461 1 0 3 -22 43.0766 6.12257 1 0 -3 22 46.2585 6.17535 1 0 3 -21 2.7857 5.54078 1 0 -3 21 2.96172 6.21425 1 0 3 -20 71.4567 8.32853 1 0 -3 20 76.0545 7.51715 1 0 3 -19 172.725 8.95388 1 0 -3 19 158.946 8.7273 1 0 3 -18 154.582 8.42783 1 0 -3 18 153.074 7.88381 1 0 3 -17 79.3054 6.61116 1 0 -3 17 89.0372 7.00005 1 0 3 -16 205.959 9.48266 1 0 -3 16 202.788 8.87055 1 0 3 -15 346.67 13.1727 1 0 -3 15 356.943 12.3218 1 0 3 -14 551.053 15.0984 1 0 -3 14 532.313 14.5456 1 0 3 -13 485.387 16.379 1 0 -3 13 472.033 14.399 1 0 3 -12 5.4461 5.89628 1 0 -3 12 11.7926 4.6226 1 0 3 -11 106.08 5.87534 1 0 -3 11 100.356 5.35693 1 0 3 -10 527.706 14.9258 1 0 -3 10 526.845 15.0623 1 0 3 -9 421.416 12.6479 1 0 -3 9 415.909 12.445 1 0 3 -8 150.955 6.47619 1 0 -3 8 155.067 7.40415 1 0 3 -7 188.368 6.88899 1 0 -3 7 192.402 7.78428 1 0 3 -6 7953.20 144.383 1 0 -3 6 8020.73 167.664 1 0 3 -5 100.407 3.8387 1 0 -3 5 102.183 4.20643 1 0 3 -4 6679.90 163.753 1 0 -3 4 6535.99 225.011 1 0 3 -3 3198.05 68.4202 1 0 -3 3 3110.20 69.4551 1 0 3 -2 46.5799 1.97232 1 0 -3 2 45.732 1.97232 1 0 3 -1 874.382 19.8645 1 0 -3 1 966.518 18.8937 1 0 3 0 1482.24 40.0961 1 0 -3 0 1450.99 40.6953 1 0 3 1 5637.93 137.765 1 0 -3 -1 5725.10 140.533 1 0 3 2 4938.93 121.25 1 0 -3 -2 5113.29 127.963 1 0 3 3 2815.04 61.1505 1 0 -3 -3 2705.18 73.2499 1 0 3 4 2225.25 63.9533 1 0 -3 -4 2361.43 47.2877 1 0 3 5 18.3949 2.45266 1 0 -3 -5 16.2327 2.45266 1 0 3 6 1419.12 46.1647 1 0 -3 -6 1400.18 37.3489 1 0 3 7 407.429 11.8151 1 0 -3 -7 409.054 11.8151 1 0 3 8 706.474 21.8116 1 0 -3 -8 684.182 18.7542 1 0 3 9 769.85 23.1962 1 0 -3 -9 753.213 19.5431 1 0 3 10 2588.40 79.5181 1 0 -3 -10 2580.97 55.1098 1 0 3 11 489.656 14.9291 1 0 -3 -11 446.959 13.6151 1 0 3 12 950.068 26.1589 1 0 -3 -12 986.542 26.0711 1 0 3 13 20.2351 5.97772 1 0 -3 -13 19.0965 5.80445 1 0 3 14 -0.6504 6.29926 1 0 -3 -14 1.14422 5.56454 1 0 3 15 16.3652 6.84007 1 0 -3 -15 19.548 5.74056 1 0 3 16 32.667 7.1528 1 0 -3 -16 35.246 6.74501 1 0 3 17 44.0972 7.71544 1 0 -3 -17 34.4999 7.42272 1 0 3 18 133.896 12.8041 1 0 -3 -18 128.051 9.46387 1 0 3 19 5.5842 6.91104 1 0 -3 -19 0.13364 6.97786 1 0 3 20 56.0448 9.7112 1 0 -3 -20 55.4752 9.07624 1 0 3 21 49.1095 8.64146 1 0 -3 -21 33.0785 8.64146 1 0 3 22 6.45893 9.06638 1 0 -3 -22 9.53413 7.20534 1 0 4 -23 5.22358 7.15708 1 0 -4 23 13.6437 5.48865 1 0 4 -22 27.3573 6.25439 1 0 -4 22 36.7994 5.94394 1 0 4 -21 13.6276 6.7527 1 0 -4 21 21.7018 6.04993 1 0 4 -20 72.9434 6.81943 1 0 -4 20 64.0536 6.87474 1 0 4 -19 4.74258 6.17947 1 0 -4 19 0.90533 6.0715 1 0 4 -18 10.6813 5.89981 1 0 -4 18 11.6411 6.19921 1 0 4 -17 222.024 11.2275 1 0 -4 17 208.701 9.86152 1 0 4 -16 923.396 26.2308 1 0 -4 16 886.19 20.7726 1 0 4 -15 137.978 7.95486 1 0 -4 15 142.709 7.95486 1 0 4 -14 1671.55 36.2803 1 0 -4 14 1629.63 35.4393 1 0 4 -13 81.1101 7.602 1 0 -4 13 71.4478 5.7621 1 0 4 -12 315.906 12.4783 1 0 -4 12 313.155 10.2488 1 0 4 -11 75.494 6.74289 1 0 -4 11 75.1194 5.46483 1 0 4 -10 629.845 16.9268 1 0 -4 10 639.787 16.7861 1 0 4 -9 234.371 8.22612 1 0 -4 9 228.048 7.94064 1 0 4 -8 30.0242 3.32572 1 0 -4 8 30.6523 3.18158 1 0 4 -7 211.067 7.54062 1 0 -4 7 214.822 7.41009 1 0 -4 6 3721.71 147.128 1 0 4 -5 13.8715 1.88583 1 0 -4 5 11.9274 2.08024 1 0 4 -413656.80 451.406 1 0 -4 413381.00 446.723 1 0 4 -3 2460.74 88.9202 1 0 -4 3 2293.48 61.4092 1 0 4 -2 6666.81 220.757 1 0 -4 2 5970.53 144.397 1 0 4 -1 4931.91 173.416 1 0 -4 1 4823.97 121.198 1 0 4 0 12.7817 2.14409 1 0 -4 0 15.9823 1.93693 1 0 4 1 128.848 5.68494 1 0 -4 -1 148.634 3.34533 1 0 4 2 485.52 15.3586 1 0 -4 -2 502.781 12.743 1 0 4 3 6446.08 156.833 1 0 -4 -3 6621.49 161.942 1 0 4 4 1650.66 46.0525 1 0 -4 -4 1653.08 38.9562 1 0 4 5 187.368 6.12804 1 0 -4 -5 197.82 6.52115 1 0 4 6 129.011 5.16662 1 0 -4 -6 130.995 5.40416 1 0 4 7 301.646 9.42988 1 0 -4 -7 298.788 9.34437 1 0 4 8 474.822 12.964 1 0 -4 -8 470.04 13.0518 1 0 4 9 736.783 18.6893 1 0 -4 -9 729.192 18.4196 1 0 4 10 2029.03 43.9315 1 0 -4 -10 2012.92 49.48 1 0 4 11 14.4641 5.97744 1 0 -4 -11 11.2061 5.26803 1 0 4 12 1582.59 53.9172 1 0 -4 -12 1625.59 42.8308 1 0 4 13 390.233 14.2306 1 0 -4 -13 407.435 14.2306 1 0 4 14 351.922 13.6614 1 0 -4 -14 323.879 13.2396 1 0 4 15 27.3856 6.7125 1 0 -4 -15 18.1261 6.62919 1 0 4 16 8.91052 7.21923 1 0 -4 -16 10.1024 6.64033 1 0 4 17 41.9466 7.91301 1 0 -4 -17 46.244 7.62074 1 0 4 18 12.3984 7.66975 1 0 -4 -18 8.7194 7.37875 1 0 4 19 4.06097 7.53456 1 0 -4 -19 3.61537 7.40291 1 0 4 20 102.96 10.3851 1 0 -4 -20 90.8241 10.041 1 0 4 21 5.73149 8.91332 1 0 -4 -21 4.94131 8.77635 1 0 5 -23 0.38755 7.41184 1 0 -5 23 8.17886 7.62983 1 0 5 -22 38.2276 7.39988 1 0 -5 22 25.8301 7.29946 1 0 5 -21 18.9155 6.57493 1 0 -5 21 20.4108 6.81388 1 0 5 -20 58.9153 8.38258 1 0 -5 20 57.2783 7.84483 1 0 5 -19 11.2269 5.41931 1 0 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2415.42 48.1733 1 4 -4 6 1676.66 35.00 1 -4 4 -6 1664.31 35.00 1 4 -4 7 2462.53 49.1179 1 -4 4 -7 2443.12 48.3006 1 4 -4 8 2411.77 49.2314 1 -4 4 -8 2443.32 48.5983 1 4 -4 9 302.861 9.2328 1 -4 4 -9 306.74 9.1639 1 4 -4 10 4019.38 74.0649 1 -4 4 -10 3958.73 70.9376 1 4 -4 11 286.428 8.99841 1 -4 4 -11 287.505 9.19596 1 4 -4 12 155.093 7.47377 1 -4 4 -12 157.36 7.07322 1 4 -4 13 4.67876 4.35345 1 -4 4 -13 13.8545 4.42042 1 4 -4 14 32.4319 5.55075 1 -4 4 -14 34.2327 5.43008 1 4 -4 15 20.4346 5.22705 1 -4 4 -15 15.6365 5.28066 1 4 -4 16 42.3009 5.78621 1 -4 4 -16 51.2028 7.61794 1 4 -4 17 2.14653 4.67812 1 -4 4 -17 3.12148 5.25981 1 4 -4 18 176.99 9.28418 1 -4 4 -18 177.092 9.55192 1 4 -4 19 1.74333 5.27587 1 -4 4 -19 5.06943 6.10931 1 4 -4 20 122.051 10.3227 1 -4 4 -20 135.94 10.9952 1 4 -4 21 11.4805 8.58545 1 -4 4 -21 5.40622 5.50605 1 4 -4 22 28.971 10.1134 1 -4 4 -22 24.2036 7.86413 1 4 -3 -22 41.1211 7.08099 1 -4 3 22 46.8887 7.63133 1 4 -3 -21 8.21048 5.57693 1 -4 3 21 6.89371 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6.25477 1 6 -6 -15 13.5338 5.01674 1 -6 6 15 19.2052 5.01674 1 6 -6 -14 158.86 8.78503 1 -6 6 14 165.633 8.69636 1 6 -6 -13 48.3134 5.28678 1 -6 6 13 50.4197 5.71224 1 6 -6 -12 1.38296 3.97066 1 -6 6 12 4.48392 4.21303 1 6 -6 -11 31.2224 4.40009 1 -6 6 11 27.9351 4.34918 1 6 -6 -10 13.9359 3.57464 1 -6 6 10 13.107 3.61904 1 6 -6 -9 340.583 9.72493 1 -6 6 9 344.533 9.87512 1 6 -6 -8 474.625 13.6091 1 -6 6 8 493.218 17.4312 1 6 -6 -7 5.34583 3.07558 1 -6 6 7 3.48974 3.02189 1 6 -6 -6 1786.37 50.7613 1 -6 6 6 1947.05 52.7779 1 6 -6 -5 28.5535 2.72012 1 -6 6 5 26.4163 2.66572 1 6 -6 -4 849.004 25.4533 1 6 -6 -3 115.874 4.32242 1 -6 6 3 112.085 4.32242 1 6 -6 -2 105.683 4.82133 1 -6 6 2 100.838 3.80507 1 6 -6 -1 160.32 6.05266 1 -6 6 1 158.303 5.13487 1 6 -6 0 66.8814 4.21237 1 -6 6 0 69.9651 4.75283 1 6 -6 1 475.76 12.9456 1 -6 6 -1 467.726 13.2171 1 6 -6 2 1860.91 50.6877 1 6 -6 4 2667.00 68.5519 1 -6 6 -4 2815.59 70.6191 1 6 -6 5 733.596 24.6242 1 6 -6 6 115.902 4.77486 1 -6 6 -6 111.74 4.66059 1 6 -6 7 381.894 12.3797 1 -6 6 -7 370.715 10.0198 1 6 -6 8 1.08328 3.42902 1 -6 6 -8 2.29687 2.85073 1 6 -6 9 40.7051 4.34565 1 -6 6 -9 40.0496 4.12716 1 6 -6 10 369.444 12.0226 1 -6 6 -10 386.581 12.3508 1 6 -6 11 422.19 12.6711 1 -6 6 -11 439.841 13.0415 1 6 -6 12 99.9307 6.37937 1 -6 6 -12 110.033 5.90826 1 6 -6 13 2.87378 4.51056 1 -6 6 -13 5.56654 4.25411 1 6 -6 14 21.991 4.82317 1 -6 6 -14 26.4098 4.87463 1 6 -6 15 20.1559 4.94755 1 -6 6 -15 28.9969 4.38826 1 6 -6 16 36.5206 5.03273 1 -6 6 -16 41.0831 4.94148 1 6 -6 17 20.0594 5.72136 1 -6 6 -17 20.4819 5.62439 1 6 -6 18 86.6964 8.17001 1 -6 6 -18 98.0194 8.78675 1 6 -6 19 4.09445 5.90083 1 -6 6 -19 6.7438 5.75207 1 6 -5 -19 1.76724 4.74263 1 -6 5 19 9.04183 7.93008 1 6 -5 -18 5.57933 4.73321 1 -6 5 18 7.24613 4.91134 1 6 -5 -17 51.2239 4.85104 1 -6 5 17 51.8318 4.85104 1 6 -5 -16 91.0445 6.27602 1 -6 5 16 90.0104 6.27602 1 6 -5 -15-0.27256 4.587 1 -6 5 15 2.14725 3.9754 1 6 -5 -14 184.822 8.82247 1 -6 5 14 187.179 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4.09071 1 -10 9 0 24.6416 4.90476 1 10 -9 1 37.076 4.03 1 -10 9 -1 42.2405 4.16861 1 10 -9 2 39.6885 3.93388 1 -10 9 -2 53.1666 6.03196 1 10 -9 3 35.6759 7.66211 1 -10 9 -3 31.1116 4.61579 1 10 -9 4 86.3825 5.35067 1 -10 9 -4 86.7838 6.66262 1 10 -9 5 3.58309 4.61124 1 -10 9 -5-1.34687 4.21026 1 10 -9 6 46.6179 3.92847 1 -10 9 -6 49.2728 3.68198 1 10 -9 7 2.96587 3.3661 1 -10 9 -7 3.10441 3.46873 1 10 -8 -9-1.40794 3.42971 1 -10 8 9 3.06433 2.78177 1 10 -8 -8 19.1976 3.55565 1 -10 8 8 14.8561 3.29045 1 10 -8 -7 29.1028 3.65705 1 -10 8 7 21.6598 3.55299 1 10 -8 -6 1.41038 3.28087 1 -10 8 6-0.86523 2.75573 1 10 -8 -5 39.6573 3.75477 1 -10 8 5 36.1397 3.44692 1 10 -8 -4 28.0603 3.37457 1 -10 8 4 29.8214 3.23714 1 10 -8 -3 26.6882 4.60107 1 -10 8 3 29.5863 4.81137 1 10 -8 -1 156.999 12.3573 1 10 -8 0 34.818 9.52382 1 -10 8 0 46.1161 11.3346 1 10 -8 1 2.52934 3.25724 1 -10 8 -1-0.25136 3.0949 1 10 -8 2 8.54499 2.46167 1 -10 8 -2 6.44024 3.26473 1 10 -8 3 30.5038 3.69934 1 -10 8 -3 37.2719 3.90953 1 10 -8 4 18.3982 3.62603 1 -10 8 -4 17.8254 3.41057 1 10 -8 5 8.06521 3.13997 1 -10 8 -5 4.44217 2.96144 1 -10 8 -6 157.217 16.5218 1 10 -8 7 -1.0523 2.77471 1 -10 8 -7-0.90571 3.09407 1 10 -8 8 24.9746 4.14238 1 -10 8 -8 22.6105 3.7135 1 10 -7 -10 9.8809 3.6968 1 -10 7 10 17.4891 3.23348 1 10 -7 -9 42.4668 4.16351 1 -10 7 9 52.536 3.73042 1 10 -7 -8 12.8939 3.60016 1 -10 7 8 13.0282 3.26202 1 10 -7 -7-0.10054 3.16198 1 -10 7 7-1.68907 2.87042 1 10 -7 -6 -1.5703 3.1965 1 -10 7 6-2.10898 3.03896 1 10 -7 -5 173.73 9.0945 1 -10 7 5 154.252 8.74531 1 10 -7 -4-2.29203 3.22543 1 -10 7 4 0.52893 3.17357 1 -10 7 3 56.1532 6.63396 1 10 -7 -2 120.381 10.6096 1 10 -7 -1 81.683 5.44695 1 -10 7 1 86.1743 5.19743 1 10 -7 0 39.0092 4.33495 1 -10 7 0 42.239 5.44538 1 10 -7 1 31.2003 3.91948 1 -10 7 -1 47.4895 5.39397 1 10 -7 2 12.7948 3.67332 1 -10 7 -2 14.2039 3.52811 1 10 -7 3-3.38891 3.2596 1 -10 7 -3-1.92343 3.15185 1 10 -7 4 9.06712 3.04034 1 -10 7 -4 2.38268 3.07808 1 10 -7 5 -0.7866 3.15177 1 -10 7 -5-1.11524 2.81773 1 10 -7 6 30.4455 4.40623 1 -10 7 -6 36.8262 4.00273 1 10 -7 7-0.25776 3.28649 1 -10 7 -7-1.33178 3.21131 1 10 -7 8 61.9715 4.70188 1 -10 7 -8 70.3191 4.53568 1 10 -7 9 1.14677 3.59037 1 -10 7 -9 4.8068 4.06194 1 10 -6 -11 0.06849 2.9256 1 -10 6 11 2.26025 2.36299 1 10 -6 -10 16.9202 3.14105 1 -10 6 10 12.3519 2.55334 1 10 -6 -9 79.8057 4.55048 1 -10 6 9 67.9225 4.44558 1 10 -6 -8 4.84433 3.18067 1 -10 6 8 9.38525 3.05931 1 10 -6 -7 34.9115 3.88133 1 -10 6 7 29.1868 3.28735 1 10 -6 -6 1.00568 3.29697 1 -10 6 6-1.28561 2.85634 1 10 -6 -5 12.3367 3.29922 1 -10 6 5 10.4799 2.85338 1 10 -6 -4 2.74163 5.96583 1 -10 6 4 7.82187 5.65826 1 10 -6 -1 29.8038 5.29409 1 10 -6 0 240.869 13.865 1 10 -6 2-3.30855 4.64193 1 -10 6 -2 1.37211 3.15917 1 10 -6 3 7.03299 4.69236 1 -10 6 -3 1.56412 3.01731 1 10 -6 4 44.5941 5.13074 1 -10 6 -4 30.4957 4.32004 1 10 -6 5-2.45394 3.32003 1 -10 6 -5 0.96048 2.9425 1 10 -6 6 0.07763 3.05539 1 -10 6 -6-1.30312 3.12748 1 10 -6 7 0.33762 3.23785 1 -10 6 -7 0.18818 3.08287 1 10 -6 8 60.9262 4.33648 1 -10 6 -8 68.7374 5.66781 1 10 -6 9 0.298 3.5815 1 -10 6 -9-1.63347 2.73717 1 10 -5 -11 25.7432 5.13076 1 -10 5 11 20.5081 3.83441 1 10 -5 -10 22.3718 4.50753 1 -10 5 10 25.9095 3.07537 1 10 -5 -9 5.79991 4.84768 1 -10 5 9 11.4725 2.59697 1 10 -5 -8 43.8551 5.12236 1 -10 5 8 43.349 3.66621 1 10 -5 -7 101.681 6.88627 1 -10 5 7 91.7471 4.51928 1 10 -5 -6 1.24759 3.17472 1 -10 5 6 1.42278 2.95705 1 10 -5 -5 18.6797 3.74884 1 -10 5 5 26.1773 3.45302 1 10 -5 -4 1.45909 3.14685 1 -10 5 4 1.86742 2.96174 1 10 -5 -3 25.2041 5.08706 1 -10 5 3 28.7221 4.09608 1 10 -5 -2 65.2423 10.6216 1 -10 5 2 53.1303 9.32033 1 10 -5 -1 82.0863 6.65398 1 -10 5 1 92.2693 7.85461 1 10 -5 0 510.814 25.9189 1 10 -5 2 87.7939 5.36067 1 -10 5 -2 103.802 6.7037 1 10 -5 3-2.04686 5.45831 1 -10 5 -3-2.00673 4.1912 1 10 -5 4 8.08101 3.61262 1 -10 5 -4 9.93614 3.2393 1 10 -5 5 9.43358 3.24028 1 -10 5 -5 11.5995 3.36093 1 10 -5 6 10.6533 3.51282 1 -10 5 -6 11.2732 3.39229 1 10 -5 7 8.06193 3.38636 1 -10 5 -7 6.2341 3.35198 1 10 -5 8 30.984 4.10032 1 -10 5 -8 33.3115 4.10032 1 10 -5 9 28.6164 4.24962 1 -10 5 -9 34.3625 4.32958 1 10 -4 -11 14.4304 3.84067 1 -10 4 11 13.9642 3.02998 1 10 -4 -10 60.6365 4.13419 1 -10 4 10 56.9902 4.03148 1 10 -4 -9 25.4072 3.98779 1 -10 4 9 21.7738 3.41959 1 10 -4 -7 13.5231 3.38212 1 -10 4 7 9.22688 3.29071 1 10 -4 -6 29.0891 3.84288 1 -10 4 6 24.0835 3.54266 1 10 -4 -5 37.5668 4.34699 1 -10 4 5 37.2069 4.08672 1 10 -4 -4 25.7331 3.98485 1 -10 4 4 22.7361 3.64249 1 10 -4 -3 6.06306 4.65384 1 -10 4 3 2.1252 3.13097 1 10 -4 -2 33.6334 3.65468 1 -10 4 2 30.6223 3.43632 1 10 -4 -1 19.1523 5.87916 1 -10 4 1 21.5202 6.03586 1 10 -4 0 134.85 5.57266 1 -10 4 0 154.202 6.44485 1 10 -4 1 7.11569 3.70817 1 10 -4 3 4.14813 5.90379 1 -10 4 -3 4.8742 7.50472 1 10 -4 4 44.8627 4.31865 1 -10 4 -4 42.5542 3.75198 1 10 -4 5 23.8173 4.077 1 -10 4 -5 17.4064 3.65319 1 10 -4 6-1.92685 3.65087 1 -10 4 -6 1.43768 3.44805 1 10 -4 7 0.2442 3.60345 1 -10 4 -7 2.00125 3.44263 1 10 -4 8-1.71816 4.06057 1 -10 4 -8 8.68594 3.69791 1 10 -4 9-0.78986 3.97898 1 -10 4 -9 6.76426 3.50981 1 10 -3 -11 -2.435 3.03726 1 -10 3 11 2.92823 2.64786 1 10 -3 -10 4.13722 3.38356 1 -10 3 10 5.22818 3.31505 1 10 -3 -9 16.8065 3.73418 1 -10 3 9 15.7297 3.2788 1 10 -3 -8 50.8961 6.39199 1 -10 3 8 38.9513 5.48196 1 10 -3 -7 4.93278 3.67464 1 -10 3 7-2.33337 3.20354 1 10 -3 -6 184.169 8.84643 1 -10 3 6 177.988 13.2527 1 10 -3 -5 1.18489 3.30853 1 -10 3 5-3.56039 2.87922 1 10 -3 -4 9.69578 3.47398 1 -10 3 4 5.606 3.16028 1 10 -3 -3-0.35924 4.90571 1 -10 3 3 2.32035 3.1625 1 10 -3 -2 40.2245 4.23353 1 -10 3 2 38.5848 3.82807 1 10 -3 -1 2.82756 5.20295 1 -10 3 1 8.27769 4.61211 1 10 -3 0-2.52602 6.00158 1 -10 3 0 0.20695 4.03555 1 10 -3 1 26.002 8.92706 1 -10 3 -1 19.2039 9.67559 1 10 -3 2 102.821 7.19883 1 10 -3 3 7.23117 4.91174 1 -10 3 -3 13.4267 4.06831 1 10 -3 4 82.3382 4.80063 1 -10 3 -4 80.6282 4.71357 1 10 -3 5 10.0466 2.91936 1 -10 3 -5 0.46685 3.55428 1 10 -3 6 6.09124 3.04251 1 -10 3 -6 5.30728 3.12962 1 10 -3 7 25.2313 5.74088 1 -10 3 -7 25.2313 4.92075 1 10 -3 8-0.29774 4.23658 1 -10 3 -8 0.82498 4.19316 1 10 -2 -11 6.19111 3.57899 1 -10 2 11 7.69749 3.5042 1 10 -2 -10 10.478 3.85462 1 -10 2 10 6.10767 3.37686 1 10 -2 -9 3.54776 3.51461 1 -10 2 9-3.96222 3.07804 1 10 -2 -8 1.85745 3.501 1 -10 2 8-0.15197 3.06197 1 10 -2 -7 2.99845 4.19095 1 -10 2 7 2.49393 4.03616 1 10 -2 -6 124.208 6.26907 1 -10 2 6 127.903 6.22821 1 10 -2 -5-4.34096 3.27205 1 -10 2 5 2.90387 2.66633 1 10 -2 -4 148.92 6.99488 1 -10 2 4 143.772 6.64483 1 10 -2 -3 0.37371 5.70363 1 -10 2 3-2.57919 5.95481 1 10 -2 -2 3.21075 3.58958 1 -10 2 2 6.29107 3.33495 1 10 -2 -1 2.86013 5.42482 1 -10 2 1 4.76479 4.07962 1 10 -2 0 7.74961 5.15794 1 -10 2 0 6.77773 4.167 1 10 -2 1 4.33151 5.11964 1 -10 2 -1 3.09485 4.07521 1 10 -2 2 4.93522 3.90302 1 -10 2 -2 7.91571 3.33531 1 10 -2 3 13.0429 3.96733 1 -10 2 -3 14.4756 3.74692 1 10 -2 4 14.7385 4.21935 1 -10 2 -4 15.5577 3.84228 1 10 -2 5 6.98993 4.04817 1 -10 2 -5 14.0905 4.36057 1 10 -2 6-3.66914 4.04646 1 -10 2 -6 0.3513 3.66914 1 10 -2 7 5.05448 4.04098 1 -10 2 -7 1.83209 3.48876 1 10 -1 -10 0.53298 3.68037 1 -10 1 10-0.89765 3.3157 1 10 -1 -9 4.02458 3.67014 1 -10 1 9 0.62312 2.72116 1 10 -1 -8 4.06355 3.90614 1 -10 1 8 1.52748 3.48638 1 10 -1 -7 3.81765 3.81765 1 -10 1 7 2.70566 3.35383 1 10 -1 -6 8.57307 3.81362 1 -10 1 6 7.93645 3.41953 1 10 -1 -5-0.63006 7.36918 1 -10 1 5-4.00888 6.30056 1 -10 1 4 136.743 17.4575 1 10 -1 -3 3.43116 13.3349 1 -10 1 3-7.57795 6.33839 1 10 -1 -2 52.8739 4.64933 1 -10 1 2 48.8147 4.42886 1 10 -1 -1 22.9082 5.66956 1 -10 1 1 23.4666 4.75639 1 10 -1 0-0.49826 3.0693 1 -10 1 0 5.12879 4.17877 1 10 -1 1 9.66155 3.41943 1 -10 1 -1 0.36206 4.62628 1 10 -1 2-2.98448 3.53141 1 -10 1 -2 6.28631 4.70629 1 10 -1 3 14.1608 3.59618 1 -10 1 -3 6.82596 4.01008 1 10 -1 4 12.3289 3.78985 1 -10 1 -4 5.47725 3.8851 1 10 -1 5 9.94919 5.02567 1 -10 1 -5 15.5333 4.16763 1 10 -1 6 9.67069 3.70222 1 -10 1 -6 13.0939 4.165 1 10 0 -9-1.22628 3.8447 1 -10 0 9-0.04147 3.26415 1 10 0 -8 0.08466 3.61612 1 -10 0 8 0.6168 3.45285 1 10 0 -7 4.63719 3.77891 1 -10 0 7 3.35903 3.52574 1 10 0 -6 2.35745 4.34931 1 -10 0 6 1.26697 3.34077 1 10 0 -5 7.07931 3.80006 1 -10 0 5 4.91887 3.45285 1 10 0 -4 21.9544 4.252 1 -10 0 4 22.092 4.00959 1 10 0 -3 34.9102 7.59265 1 -10 0 3 33.397 4.87289 1 10 0 -2 128.019 16.2436 1 10 0 -1 12.5754 7.7704 1 -10 0 1 10.4955 8.23717 1 10 0 0 11.2078 5.8261 1 -10 0 0 14.3465 5.8261 1 10 0 1 1.97646 7.66756 1 -10 0 -1 14.7464 5.36169 1 10 0 2 3.21097 4.48831 1 -10 0 -2 7.24057 5.25047 1 10 0 3 4.79199 4.33831 1 -10 0 -3-0.38279 3.99805 1 10 0 4 12.4825 4.46867 1 -10 0 -4 7.94273 4.41894 1 10 1 -6 3.51178 4.00225 1 -10 -1 6 1.75262 3.55755 1 10 1 -5-1.15494 4.08567 1 -10 -1 5 3.26453 3.63171 1 10 1 -4 0.46288 4.28165 1 -10 -1 4-5.80644 3.93449 1 10 1 -3 12.5985 6.5002 1 -10 -1 3 34.573 6.5002 1 10 1 -2 41.3044 6.55548 1 -10 -1 2 42.9592 7.13287 1 10 1 -1 17.4688 6.45353 1 -10 -1 1 10.9153 5.41126 1 10 1 0 40.7578 8.71473 1 -10 -1 0 32.4907 6.42594 1 10 1 1 3.11732 6.3366 1 -10 -1 -1 3.46692 6.93385 1 11 -7 -3 1.12539 3.34815 1 -11 7 3-2.75977 4.22138 1 11 -7 -2 0.65384 3.08575 1 -11 7 2-0.59269 2.99167 1 11 -7 -1 2.54219 3.03927 1 -11 7 1 2.25341 3.01086 1 11 -7 0 12.0039 3.15568 1 -11 7 0 14.7693 3.02716 1 11 -7 1 4.19256 3.20298 1 -11 7 -1 5.13433 2.27555 1 11 -7 2-5.32924 4.89274 1 -11 7 -2 3.18028 4.02451 1 11 -6 -5 37.7346 5.53485 1 -11 6 5 44.3539 3.81196 1 11 -6 -4 13.3878 3.97746 1 -11 6 4 5.91168 2.61214 1 11 -6 -3 66.4707 5.74096 1 -11 6 3 62.6817 4.32486 1 11 -6 -2 15.8216 10.7375 1 -11 6 2 13.8053 4.92014 1 11 -6 -1 4.11031 3.35238 1 -11 6 1 4.52328 3.09002 1 11 -6 0 0.26396 3.24083 1 -11 6 0 1.37845 2.85956 1 11 -6 1 8.49816 3.12418 1 -11 6 -1 5.62451 2.70664 1 11 -6 2 1.76032 3.50091 1 -11 6 -2 1.97727 3.30368 1 11 -6 3 6.33384 3.95062 1 -11 6 -3 2.58595 2.99139 1 11 -5 -5 23.2885 3.55101 1 -11 5 5 22.355 3.32005 1 11 -5 -4 6.00273 3.68725 1 -11 5 4 0.64697 2.54411 1 11 -5 -3 59.2375 5.17929 1 -11 5 3 64.7313 5.27757 1 11 -5 -2 10.4337 4.98875 1 -11 5 2 13.1612 5.67804 1 11 -5 -1 28.6928 3.88902 1 -11 5 1 31.602 4.3489 1 11 -5 0 5.40497 5.33451 1 -11 5 0 8.97808 3.77945 1 11 -5 1 1.46237 3.09677 1 -11 5 -1-0.34409 2.88931 1 11 -5 2 2.28151 3.33334 1 -11 5 -2-1.19411 3.16058 1 11 -5 3-1.90614 3.51667 1 -11 5 -3-0.55553 2.98153 1 11 -4 -5-1.12694 3.10897 1 -11 4 5-0.43496 2.38733 1 11 -4 -4 10.3694 4.93209 1 -11 4 4 13.8909 3.89165 1 11 -4 -3 39.8805 5.99851 1 -11 4 3 36.9217 4.24347 1 11 -4 -2-0.88376 6.75335 1 -11 4 2-2.29369 11.7545 1 11 -4 -1 87.6597 5.60659 1 -11 4 1 83.228 4.69449 1 11 -4 0 6.01649 7.34022 1 -11 4 0 7.51672 4.5526 1 11 -4 1 16.1672 5.43085 1 -11 4 -1 20.6216 4.75721 1 11 -4 2 5.31383 3.7244 1 -11 4 -2-2.03006 3.2995 1 11 -3 -4 0.48929 3.45079 1 -11 3 4-0.45324 3.15207 1 11 -3 -3-1.71998 3.45561 1 -11 3 3 2.58519 3.11682 1 11 -3 -2-0.70066 6.24797 1 -11 3 2 9.11382 6.64308 1 11 -3 -1 84.2915 5.31208 1 -11 3 1 81.1808 6.6308 1 11 -3 0-2.69564 5.611 1 -11 3 0 1.29155 5.17155 1 0 0 0 0.00 0.00 1 ; _shelx_hkl_checksum 85368 _shelx_res_file ; TITL S200v in P-1 S200v.res created by SHELXL-2018/3 at 11:48:19 on 06-May-2021 CELL 0.61000 8.0800 10.3800 17.5110 97.016 92.908 111.308 ZERR 1.000 0.0016 0.0021 0.0035 0.030 0.030 0.030 LATT 1 SFAC C H N O CU BR DISP C 0.0019 0.0011 8.51 DISP H 0.0000 0.0000 0.66 DISP N 0.0040 0.0024 13.80 DISP O 0.0074 0.0043 22.01 DISP Cu 0.3373 0.9674 3402.11 DISP Br 0.0842 1.9122 6690.80 UNIT 44 96 8 4 2 4 ACTA OMIT -3 50 TEMP -53.15 SIZE 0.075 0.074 0.069 L.S. 10 BOND $H LIST 4 FMAP -2 PLAN -10 CONF WPDB EQIV $1 -x, -y+1, -z+1 EQIV $2 -x+1, -y+1, -z+2 EQIV $3 -x+1, -y+1, -z+1 EQIV $4 x-1, y, z EQIV $5 x+1, y, z HTAB O1 Br1_$3 HTAB O1 Br1 HTAB N1 Br1 HTAB N2 O1 HTAB C10 O1_$1 HTAB O2 Br2_$2 HTAB O2 Br2_$5 HTAB N3 Br2 HTAB N4 O2_$4 MERG 2 WGHT 0.096600 0.526100 EXTI 0.012603 FVAR 1.06422 CU1 5 0.000000 0.500000 0.500000 10.50000 0.05397 0.03925 = 0.04398 0.00506 0.00016 0.00982 BR1 6 0.402547 0.309724 0.581523 11.00000 0.06737 0.08170 = 0.10763 0.03862 0.02372 0.03627 DFIX 0.96 0.01 O1 H1O1 O1 H2O1 DANG 1.55 0.02 H1O1 H2O1 O1 4 0.239273 0.414943 0.434174 11.00000 0.06711 0.06716 = 0.07464 0.00646 0.00136 0.02225 H1O1 2 0.344785 0.480657 0.418272 11.00000 -1.50000 H2O1 2 0.279025 0.363848 0.468219 11.00000 -1.50000 N1 3 0.090717 0.472209 0.603694 11.00000 0.05032 0.04275 = 0.04532 0.00530 0.00223 0.01114 AFIX 13 H1 2 0.186408 0.435706 0.594109 11.00000 -1.20000 AFIX 0 N2 3 0.192030 0.695247 0.500698 11.00000 0.04968 0.03958 = 0.04640 0.00533 0.00123 0.01158 AFIX 13 H2 2 0.294565 0.675493 0.481196 11.00000 -1.20000 AFIX 0 C1 1 -0.133425 0.240648 0.562092 11.00000 0.05012 0.04053 = 0.05057 0.00843 0.00322 0.01384 AFIX 13 H1A 2 -0.035569 0.211837 0.544820 11.00000 -1.20000 AFIX 0 C2 1 -0.281368 0.112481 0.582680 11.00000 0.05319 0.04490 = 0.06329 0.01276 0.00337 0.01128 AFIX 23 H2A 2 -0.386524 0.135435 0.592531 11.00000 -1.20000 H2B 2 -0.315628 0.036372 0.538885 11.00000 -1.20000 AFIX 0 C3 1 -0.220379 0.063978 0.654135 11.00000 0.06166 0.05107 = 0.06959 0.01897 -0.00137 0.00868 AFIX 23 H3A 2 -0.123680 0.031181 0.642501 11.00000 -1.20000 H3B 2 -0.319937 -0.014341 0.668053 11.00000 -1.20000 AFIX 0 C4 1 -0.155056 0.183440 0.722154 11.00000 0.07422 0.05481 = 0.05671 0.01833 -0.00018 0.00876 AFIX 23 H4A 2 -0.252788 0.214278 0.734951 11.00000 -1.20000 H4B 2 -0.117270 0.150539 0.767590 11.00000 -1.20000 AFIX 0 C5 1 0.000385 0.305255 0.701789 11.00000 0.06651 0.04870 = 0.05134 0.01154 -0.00241 0.01105 AFIX 23 H5A 2 0.099526 0.275150 0.690634 11.00000 -1.20000 H5B 2 0.041854 0.380993 0.745878 11.00000 -1.20000 AFIX 0 C6 1 -0.056539 0.358694 0.631252 11.00000 0.05038 0.04644 = 0.04650 0.00733 0.00330 0.01289 AFIX 13 H6 2 -0.150780 0.394678 0.644934 11.00000 -1.20000 AFIX 0 C7 1 0.170675 0.599644 0.662057 11.00000 0.06647 0.04713 = 0.04361 0.00412 -0.00145 0.01170 AFIX 23 H7A 2 0.214645 0.575159 0.709233 11.00000 -1.20000 H7B 2 0.078680 0.636960 0.675206 11.00000 -1.20000 AFIX 0 C8 1 0.323773 0.711394 0.632660 11.00000 0.05436 0.04781 = 0.05257 0.00646 -0.00269 0.01009 AFIX 23 H8A 2 0.399793 0.666842 0.608126 11.00000 -1.20000 H8B 2 0.395973 0.778503 0.677232 11.00000 -1.20000 AFIX 0 C9 1 0.270336 0.792065 0.575141 11.00000 0.05110 0.04362 = 0.05076 0.00545 0.00060 0.00832 AFIX 13 H9 2 0.381547 0.865674 0.564382 11.00000 -1.20000 AFIX 0 C10 1 0.148560 0.865007 0.604717 11.00000 0.06261 0.05148 = 0.05326 0.00065 0.00142 0.01949 AFIX 23 H10A 2 0.032181 0.794226 0.610545 11.00000 -1.20000 H10B 2 0.129807 0.920869 0.566305 11.00000 -1.20000 AFIX 0 C11 1 0.223747 0.960358 0.682238 11.00000 0.07272 0.05892 = 0.05589 -0.00659 0.00047 0.01628 AFIX 137 H11A 2 0.145410 1.009367 0.696510 11.00000 -1.50000 H11B 2 0.341660 1.027751 0.677616 11.00000 -1.50000 H11C 2 0.231823 0.904385 0.721720 11.00000 -1.50000 AFIX 0 CU2 5 0.500000 0.500000 1.000000 10.50000 0.05121 0.04118 = 0.04493 0.00316 0.00363 0.01234 BR2 6 0.164729 0.611720 0.883988 11.00000 0.07099 0.09287 = 0.07067 -0.00158 0.00245 0.03959 DFIX 0.96 0.01 O2 H1O2 O2 H2O2 DANG 1.55 0.02 H1O2 H2O2 O2 4 0.962676 0.306913 0.945999 11.00000 0.07758 0.10639 = 0.08266 0.00701 0.01218 0.03984 H1O2 2 0.919238 0.327480 0.994239 11.00000 -1.50000 H2O2 2 1.006509 0.393655 0.925311 11.00000 -1.50000 N3 3 0.497604 0.488307 0.884098 11.00000 0.05401 0.04352 = 0.04650 0.00310 0.00271 0.01385 AFIX 13 H3 2 0.399068 0.517512 0.867864 11.00000 -1.20000 AFIX 0 N4 3 0.316034 0.305055 0.997393 11.00000 0.05226 0.04168 = 0.04668 0.00327 0.00251 0.01235 AFIX 13 H4 2 0.199482 0.313754 0.986331 11.00000 -1.20000 AFIX 0 C12 1 0.685051 0.731123 0.922540 11.00000 0.05489 0.04493 = 0.04603 0.00691 0.00704 0.01482 AFIX 13 H12 2 0.580177 0.756481 0.911901 11.00000 -1.20000 AFIX 0 C13 1 0.852242 0.853523 0.910719 11.00000 0.05962 0.04888 = 0.05864 0.00746 0.00791 0.01062 AFIX 23 H13A 2 0.958363 0.832878 0.923957 11.00000 -1.20000 H13B 2 0.859883 0.937737 0.945190 11.00000 -1.20000 AFIX 0 C14 1 0.847994 0.880140 0.826948 11.00000 0.07365 0.05353 = 0.05764 0.01359 0.01605 0.01715 AFIX 23 H14A 2 0.749448 0.910964 0.815617 11.00000 -1.20000 H14B 2 0.959670 0.955208 0.819902 11.00000 -1.20000 AFIX 0 C15 1 0.824236 0.749234 0.770753 11.00000 0.07405 0.05774 = 0.05330 0.00993 0.01565 0.01942 AFIX 23 H15A 2 0.814854 0.768115 0.717548 11.00000 -1.20000 H15B 2 0.929007 0.724031 0.778255 11.00000 -1.20000 AFIX 0 C16 1 0.657372 0.627870 0.783153 11.00000 0.07168 0.05645 = 0.04693 0.00625 0.00790 0.01709 AFIX 23 H16A 2 0.647929 0.543645 0.748224 11.00000 -1.20000 H16B 2 0.551606 0.649503 0.770759 11.00000 -1.20000 AFIX 0 C17 1 0.662987 0.600111 0.866665 11.00000 0.05566 0.04325 = 0.04974 0.00506 0.00496 0.01475 AFIX 13 H17 2 0.766123 0.572793 0.877565 11.00000 -1.20000 AFIX 0 C18 1 0.459854 0.351217 0.834777 11.00000 0.06811 0.04793 = 0.04771 0.00023 0.00708 0.01361 AFIX 23 H18A 2 0.563868 0.324513 0.840387 11.00000 -1.20000 H18B 2 0.439538 0.360527 0.780421 11.00000 -1.20000 AFIX 0 C19 1 0.297786 0.237690 0.856739 11.00000 0.06318 0.04654 = 0.04822 0.00046 0.00073 0.01134 AFIX 23 H19A 2 0.265388 0.154862 0.817165 11.00000 -1.20000 H19B 2 0.197839 0.269899 0.855880 11.00000 -1.20000 AFIX 0 C20 1 0.319952 0.194544 0.935102 11.00000 0.06190 0.04233 = 0.04913 -0.00023 0.00191 0.01197 AFIX 13 H20 2 0.215684 0.108375 0.937994 11.00000 -1.20000 AFIX 0 C21 1 0.486849 0.161317 0.947471 11.00000 0.08410 0.06506 = 0.05637 0.00246 0.00529 0.03832 AFIX 23 H21A 2 0.489639 0.129926 0.997909 11.00000 -1.20000 H21B 2 0.592161 0.247111 0.948683 11.00000 -1.20000 AFIX 0 C22 1 0.497977 0.048743 0.884864 11.00000 0.11395 0.07608 = 0.06568 0.00539 0.01441 0.05482 AFIX 137 H22A 2 0.603614 0.028795 0.897506 11.00000 -1.50000 H22B 2 0.504835 0.081991 0.835259 11.00000 -1.50000 H22C 2 0.392525 -0.035806 0.882202 11.00000 -1.50000 AFIX 0 HKLF 4 REM S200v in P-1 REM wR2 = 0.1762, GooF = S = 1.105, Restrained GooF = 1.105 for all data REM R1 = 0.0561 for 5311 Fo > 4sig(Fo) and 0.0721 for all 7233 data REM 298 parameters refined using 6 restraints END WGHT 0.0966 0.5261 REM Highest difference peak 0.831, deepest hole -1.030, 1-sigma level 0.095 Q1 1 0.4561 0.3622 0.6216 11.00000 0.05 -1.03 Q2 1 0.5173 0.5592 1.0306 11.00000 0.05 -0.85 Q3 1 -0.0642 0.4472 0.4630 11.00000 0.05 -0.85 Q4 1 0.4589 0.4492 1.0266 11.00000 0.05 -0.83 Q5 1 0.1657 0.6011 0.9313 11.00000 0.05 0.83 Q6 1 0.3867 0.2969 0.5320 11.00000 0.05 0.83 Q7 1 0.1921 0.6640 0.8564 11.00000 0.05 -0.78 Q8 1 0.0463 0.5502 0.4727 11.00000 0.05 -0.77 Q9 1 0.1002 0.4903 0.4971 11.00000 0.05 0.74 Q10 1 0.0701 0.6285 0.8880 11.00000 0.05 0.71 ; _shelx_res_checksum 52545 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 Cu Cu1 0.000000 0.500000 0.500000 0.04817(16) Uani d 1 . . Br Br1 0.40255(6) 0.30972(5) 0.58152(3) 0.08044(18) Uani d 1 . . O O1 0.2393(4) 0.4149(3) 0.43417(19) 0.0710(7) Uani d 1 . . H H1O1 0.345(4) 0.481(5) 0.418(3) 0.107 Uiso d 1 . . H H2O1 0.279(6) 0.364(5) 0.468(3) 0.107 Uiso d 1 . . N N1 0.0907(4) 0.4722(3) 0.60369(15) 0.0481(6) Uani d 1 . . H H1 0.186408 0.435706 0.594109 0.058 Uiso calc 1 . . N N2 0.1920(4) 0.6952(3) 0.50070(15) 0.0469(6) Uani d 1 . . H H2 0.294565 0.675493 0.481196 0.056 Uiso calc 1 . . C C1 -0.1334(4) 0.2406(3) 0.56209(19) 0.0479(6) Uani d 1 . . H H1A -0.035569 0.211837 0.544820 0.057 Uiso calc 1 . . C C2 -0.2814(5) 0.1125(4) 0.5827(2) 0.0555(8) Uani d 1 . . H H2A -0.386524 0.135435 0.592531 0.067 Uiso calc 1 . . H H2B -0.315628 0.036372 0.538885 0.067 Uiso calc 1 . . C C3 -0.2204(6) 0.0640(4) 0.6541(2) 0.0637(9) Uani d 1 . . H H3A -0.123680 0.031181 0.642501 0.076 Uiso calc 1 . . H H3B -0.319937 -0.014341 0.668053 0.076 Uiso calc 1 . . C C4 -0.1551(6) 0.1834(4) 0.7222(2) 0.0656(10) Uani d 1 . . H H4A -0.252788 0.214278 0.734951 0.079 Uiso calc 1 . . H H4B -0.117270 0.150539 0.767590 0.079 Uiso calc 1 . . C C5 0.0004(5) 0.3053(4) 0.7018(2) 0.0584(8) Uani d 1 . . H H5A 0.099526 0.275150 0.690634 0.070 Uiso calc 1 . . H H5B 0.041854 0.380993 0.745878 0.070 Uiso calc 1 . . C C6 -0.0565(4) 0.3587(4) 0.63125(19) 0.0493(7) Uani d 1 . . H H6 -0.150780 0.394678 0.644934 0.059 Uiso calc 1 . . C C7 0.1707(5) 0.5996(4) 0.66206(19) 0.0556(8) Uani d 1 . . H H7A 0.214645 0.575159 0.709233 0.067 Uiso calc 1 . . H H7B 0.078680 0.636960 0.675206 0.067 Uiso calc 1 . . C C8 0.3238(5) 0.7114(4) 0.6327(2) 0.0545(8) Uani d 1 . . H H8A 0.399793 0.666842 0.608126 0.065 Uiso calc 1 . . H H8B 0.395973 0.778503 0.677232 0.065 Uiso calc 1 . . C C9 0.2703(5) 0.7921(4) 0.57514(19) 0.0515(7) Uani d 1 . . H H9 0.381547 0.865674 0.564382 0.062 Uiso calc 1 . . C C10 0.1486(5) 0.8650(4) 0.6047(2) 0.0571(8) Uani d 1 . . H H10A 0.032181 0.794226 0.610545 0.069 Uiso calc 1 . . H H10B 0.129807 0.920869 0.566305 0.069 Uiso calc 1 . . C C11 0.2237(6) 0.9604(4) 0.6822(2) 0.0664(10) Uani d 1 . . H H11A 0.145410 1.009367 0.696510 0.100 Uiso calc 1 . . H H11B 0.341660 1.027751 0.677616 0.100 Uiso calc 1 . . H H11C 0.231823 0.904385 0.721720 0.100 Uiso calc 1 . . Cu Cu2 0.500000 0.500000 1.000000 0.04751(16) Uani d 1 . . Br Br2 0.16473(6) 0.61172(5) 0.88399(3) 0.07704(17) Uani d 1 . . O O2 0.9627(5) 0.3069(4) 0.9460(2) 0.0878(10) Uani d 1 . . H H1O2 0.919(9) 0.327(6) 0.994(2) 0.132 Uiso d 1 . . H H2O2 1.007(9) 0.394(3) 0.925(3) 0.132 Uiso d 1 . . N N3 0.4976(4) 0.4883(3) 0.88410(16) 0.0497(6) Uani d 1 . . H H3 0.399068 0.517512 0.867864 0.060 Uiso calc 1 . . N N4 0.3160(4) 0.3051(3) 0.99739(15) 0.0487(6) Uani d 1 . . H H4 0.199482 0.313754 0.986331 0.058 Uiso calc 1 . . C C12 0.6851(5) 0.7311(4) 0.92254(19) 0.0496(7) Uani d 1 . . H H12 0.580177 0.756481 0.911901 0.060 Uiso calc 1 . . C C13 0.8522(5) 0.8535(4) 0.9107(2) 0.0584(8) Uani d 1 . . H H13A 0.958363 0.832878 0.923957 0.070 Uiso calc 1 . . H H13B 0.859883 0.937737 0.945190 0.070 Uiso calc 1 . . C C14 0.8480(6) 0.8801(4) 0.8269(2) 0.0627(9) Uani d 1 . . H H14A 0.749448 0.910964 0.815617 0.075 Uiso calc 1 . . H H14B 0.959670 0.955208 0.819902 0.075 Uiso calc 1 . . C C15 0.8242(6) 0.7492(4) 0.7708(2) 0.0627(9) Uani d 1 . . H H15A 0.814854 0.768115 0.717548 0.075 Uiso calc 1 . . H H15B 0.929007 0.724031 0.778255 0.075 Uiso calc 1 . . C C16 0.6574(5) 0.6279(4) 0.7832(2) 0.0604(9) Uani d 1 . . H H16A 0.647929 0.543645 0.748224 0.072 Uiso calc 1 . . H H16B 0.551606 0.649503 0.770759 0.072 Uiso calc 1 . . C C17 0.6630(5) 0.6001(4) 0.8667(2) 0.0508(7) Uani d 1 . . H H17 0.766123 0.572793 0.877565 0.061 Uiso calc 1 . . C C18 0.4599(5) 0.3512(4) 0.8348(2) 0.0574(8) Uani d 1 . . H H18A 0.563868 0.324513 0.840387 0.069 Uiso calc 1 . . H H18B 0.439538 0.360527 0.780421 0.069 Uiso calc 1 . . C C19 0.2978(5) 0.2377(4) 0.8567(2) 0.0560(8) Uani d 1 . . H H19A 0.265388 0.154862 0.817165 0.067 Uiso calc 1 . . H H19B 0.197839 0.269899 0.855880 0.067 Uiso calc 1 . . C C20 0.3200(5) 0.1945(4) 0.9351(2) 0.0540(7) Uani d 1 . . H H20 0.215684 0.108375 0.937994 0.065 Uiso calc 1 . . C C21 0.4868(6) 0.1613(5) 0.9475(2) 0.0662(10) Uani d 1 . . H H21A 0.489639 0.129926 0.997909 0.079 Uiso calc 1 . . H H21B 0.592161 0.247111 0.948683 0.079 Uiso calc 1 . . C C22 0.4980(8) 0.0487(5) 0.8849(3) 0.0800(13) Uani d 1 . . H H22A 0.603614 0.028795 0.897506 0.120 Uiso calc 1 . . H H22B 0.504835 0.081991 0.835259 0.120 Uiso calc 1 . . H H22C 0.392525 -0.035806 0.882202 0.120 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 Cu1 0.0540(3) 0.0392(3) 0.0440(3) 0.0098(2) 0.0002(2) 0.0051(2) Br1 0.0674(3) 0.0817(3) 0.1076(4) 0.0363(2) 0.0237(2) 0.0386(3) O1 0.0671(16) 0.0672(19) 0.0746(19) 0.0222(15) 0.0014(13) 0.0065(14) N1 0.0503(14) 0.0427(15) 0.0453(13) 0.0111(12) 0.0022(10) 0.0053(11) N2 0.0497(13) 0.0396(14) 0.0464(14) 0.0116(11) 0.0012(10) 0.0053(10) C1 0.0501(16) 0.0405(17) 0.0506(17) 0.0138(13) 0.0032(12) 0.0084(12) C2 0.0532(18) 0.0449(19) 0.063(2) 0.0113(15) 0.0034(14) 0.0128(15) C3 0.062(2) 0.051(2) 0.070(2) 0.0087(17) -0.0014(17) 0.0190(17) C4 0.074(2) 0.055(2) 0.057(2) 0.0088(19) -0.0002(17) 0.0183(17) C5 0.067(2) 0.049(2) 0.0513(18) 0.0111(17) -0.0024(15) 0.0115(15) C6 0.0504(16) 0.0464(18) 0.0465(16) 0.0129(14) 0.0033(12) 0.0073(13) C7 0.066(2) 0.0471(19) 0.0436(16) 0.0117(16) -0.0014(14) 0.0041(13) C8 0.0544(17) 0.048(2) 0.0526(18) 0.0101(15) -0.0027(13) 0.0065(14) C9 0.0511(16) 0.0436(18) 0.0508(17) 0.0083(14) 0.0006(13) 0.0055(13) C10 0.063(2) 0.051(2) 0.0533(19) 0.0195(17) 0.0014(14) 0.0007(15) C11 0.073(2) 0.059(2) 0.056(2) 0.0163(19) 0.0005(17) -0.0066(17) Cu2 0.0512(3) 0.0412(3) 0.0449(3) 0.0123(2) 0.0036(2) 0.0032(2) Br2 0.0710(3) 0.0929(4) 0.0707(3) 0.0396(3) 0.00245(19) -0.0016(2) O2 0.078(2) 0.106(3) 0.083(2) 0.040(2) 0.0122(16) 0.0070(19) N3 0.0540(14) 0.0435(15) 0.0465(14) 0.0139(12) 0.0027(11) 0.0031(11) N4 0.0523(14) 0.0417(15) 0.0467(14) 0.0123(12) 0.0025(11) 0.0033(11) C12 0.0549(17) 0.0449(18) 0.0460(16) 0.0148(14) 0.0070(12) 0.0069(13) C13 0.0596(19) 0.049(2) 0.059(2) 0.0106(16) 0.0079(15) 0.0075(15) C14 0.074(2) 0.054(2) 0.058(2) 0.0171(18) 0.0160(17) 0.0136(16) C15 0.074(2) 0.058(2) 0.0533(19) 0.0194(19) 0.0157(16) 0.0099(16) C16 0.072(2) 0.056(2) 0.0469(18) 0.0171(18) 0.0079(15) 0.0062(15) C17 0.0557(17) 0.0433(18) 0.0497(17) 0.0148(15) 0.0050(13) 0.0051(13) C18 0.068(2) 0.048(2) 0.0477(17) 0.0136(17) 0.0071(14) 0.0002(14) C19 0.063(2) 0.047(2) 0.0482(17) 0.0113(16) 0.0007(14) 0.0005(14) C20 0.0619(19) 0.0423(18) 0.0491(17) 0.0120(15) 0.0019(14) -0.0002(13) C21 0.084(3) 0.065(2) 0.056(2) 0.038(2) 0.0053(18) 0.0025(17) C22 0.114(4) 0.076(3) 0.066(3) 0.055(3) 0.014(2) 0.005(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0019 0.0011 '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 0.0040 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0074 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3373 0.9674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br 0.0842 1.9122 '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 N1 Cu1 N1 2_566 . 180.00(7) ? N1 Cu1 N2 2_566 2_566 95.47(11) ? N1 Cu1 N2 . 2_566 84.53(11) ? N1 Cu1 N2 2_566 . 84.53(11) ? N1 Cu1 N2 . . 95.47(11) ? N2 Cu1 N2 2_566 . 180.0 ? H1O1 O1 H2O1 . . 106(2) ? C7 N1 C6 . . 113.3(3) ? C7 N1 Cu1 . . 116.0(2) ? C6 N1 Cu1 . . 107.52(19) ? C7 N1 H1 . . 106.5 ? C6 N1 H1 . . 106.5 ? Cu1 N1 H1 . . 106.5 ? C1 N2 C9 2_566 . 115.1(3) ? C1 N2 Cu1 2_566 . 107.68(19) ? C9 N2 Cu1 . . 120.8(2) ? C1 N2 H2 2_566 . 103.7 ? C9 N2 H2 . . 103.7 ? Cu1 N2 H2 . . 103.7 ? N2 C1 C2 2_566 . 113.8(3) ? N2 C1 C6 2_566 . 105.7(3) ? C2 C1 C6 . . 112.5(3) ? N2 C1 H1A 2_566 . 108.2 ? C2 C1 H1A . . 108.2 ? C6 C1 H1A . . 108.2 ? C3 C2 C1 . . 111.2(3) ? C3 C2 H2A . . 109.4 ? C1 C2 H2A . . 109.4 ? C3 C2 H2B . . 109.4 ? C1 C2 H2B . . 109.4 ? H2A C2 H2B . . 108.0 ? C2 C3 C4 . . 110.6(3) ? C2 C3 H3A . . 109.5 ? C4 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? C4 C3 H3B . . 109.5 ? H3A C3 H3B . . 108.1 ? C5 C4 C3 . . 110.2(3) ? C5 C4 H4A . . 109.6 ? C3 C4 H4A . . 109.6 ? C5 C4 H4B . . 109.6 ? C3 C4 H4B . . 109.6 ? H4A C4 H4B . . 108.1 ? C4 C5 C6 . . 110.4(3) ? C4 C5 H5A . . 109.6 ? C6 C5 H5A . . 109.6 ? C4 C5 H5B . . 109.6 ? C6 C5 H5B . . 109.6 ? H5A C5 H5B . . 108.1 ? N1 C6 C5 . . 114.2(3) ? N1 C6 C1 . . 106.3(3) ? C5 C6 C1 . . 111.3(3) ? N1 C6 H6 . . 108.3 ? C5 C6 H6 . . 108.3 ? C1 C6 H6 . . 108.3 ? N1 C7 C8 . . 111.7(3) ? N1 C7 H7A . . 109.3 ? C8 C7 H7A . . 109.3 ? N1 C7 H7B . . 109.3 ? C8 C7 H7B . . 109.3 ? H7A C7 H7B . . 107.9 ? C7 C8 C9 . . 115.8(3) ? C7 C8 H8A . . 108.3 ? C9 C8 H8A . . 108.3 ? C7 C8 H8B . . 108.3 ? C9 C8 H8B . . 108.3 ? H8A C8 H8B . . 107.4 ? N2 C9 C10 . . 112.3(3) ? N2 C9 C8 . . 108.6(3) ? C10 C9 C8 . . 114.4(3) ? N2 C9 H9 . . 107.1 ? C10 C9 H9 . . 107.1 ? C8 C9 H9 . . 107.1 ? C9 C10 C11 . . 112.9(3) ? C9 C10 H10A . . 109.0 ? C11 C10 H10A . . 109.0 ? C9 C10 H10B . . 109.0 ? C11 C10 H10B . . 109.0 ? H10A C10 H10B . . 107.8 ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N3 Cu2 N3 . 2_667 180.0 ? N3 Cu2 N4 . . 95.18(12) ? N3 Cu2 N4 2_667 . 84.82(12) ? N3 Cu2 N4 . 2_667 84.82(12) ? N3 Cu2 N4 2_667 2_667 95.18(12) ? N4 Cu2 N4 . 2_667 180.0 ? H1O2 O2 H2O2 . . 106(2) ? C18 N3 C17 . . 112.5(3) ? C18 N3 Cu2 . . 120.2(2) ? C17 N3 Cu2 . . 108.2(2) ? C18 N3 H3 . . 104.8 ? C17 N3 H3 . . 104.8 ? Cu2 N3 H3 . . 104.8 ? C20 N4 C12 . 2_667 115.3(3) ? C20 N4 Cu2 . . 117.0(2) ? C12 N4 Cu2 2_667 . 108.3(2) ? C20 N4 H4 . . 105.0 ? C12 N4 H4 2_667 . 105.0 ? Cu2 N4 H4 . . 105.0 ? N4 C12 C17 2_667 . 107.6(3) ? N4 C12 C13 2_667 . 113.6(3) ? C17 C12 C13 . . 111.0(3) ? N4 C12 H12 2_667 . 108.1 ? C17 C12 H12 . . 108.1 ? C13 C12 H12 . . 108.1 ? C12 C13 C14 . . 110.7(3) ? C12 C13 H13A . . 109.5 ? C14 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? C14 C13 H13B . . 109.5 ? H13A C13 H13B . . 108.1 ? C15 C14 C13 . . 111.5(3) ? C15 C14 H14A . . 109.3 ? C13 C14 H14A . . 109.3 ? C15 C14 H14B . . 109.3 ? C13 C14 H14B . . 109.3 ? H14A C14 H14B . . 108.0 ? C16 C15 C14 . . 110.8(3) ? C16 C15 H15A . . 109.5 ? C14 C15 H15A . . 109.5 ? C16 C15 H15B . . 109.5 ? C14 C15 H15B . . 109.5 ? H15A C15 H15B . . 108.1 ? C15 C16 C17 . . 111.0(3) ? C15 C16 H16A . . 109.4 ? C17 C16 H16A . . 109.4 ? C15 C16 H16B . . 109.4 ? C17 C16 H16B . . 109.4 ? H16A C16 H16B . . 108.0 ? N3 C17 C12 . . 106.1(3) ? N3 C17 C16 . . 113.7(3) ? C12 C17 C16 . . 110.6(3) ? N3 C17 H17 . . 108.7 ? C12 C17 H17 . . 108.7 ? C16 C17 H17 . . 108.7 ? N3 C18 C19 . . 111.5(3) ? N3 C18 H18A . . 109.3 ? C19 C18 H18A . . 109.3 ? N3 C18 H18B . . 109.3 ? C19 C18 H18B . . 109.3 ? H18A C18 H18B . . 108.0 ? C18 C19 C20 . . 115.6(3) ? C18 C19 H19A . . 108.4 ? C20 C19 H19A . . 108.4 ? C18 C19 H19B . . 108.4 ? C20 C19 H19B . . 108.4 ? H19A C19 H19B . . 107.4 ? N4 C20 C19 . . 109.5(3) ? N4 C20 C21 . . 111.4(3) ? C19 C20 C21 . . 113.2(3) ? N4 C20 H20 . . 107.5 ? C19 C20 H20 . . 107.5 ? C21 C20 H20 . . 107.5 ? C20 C21 C22 . . 113.5(4) ? C20 C21 H21A . . 108.9 ? C22 C21 H21A . . 108.9 ? C20 C21 H21B . . 108.9 ? C22 C21 H21B . . 108.9 ? H21A C21 H21B . . 107.7 ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 N1 2_566 2.016(3) ? Cu1 N1 . 2.016(3) ? Cu1 N2 2_566 2.055(3) ? Cu1 N2 . 2.055(3) ? Cu1 O1 . 2.658(4) ? O1 H1O1 . 0.958(10) ? O1 H2O1 . 0.960(10) ? N1 C7 . 1.481(4) ? N1 C6 . 1.488(4) ? N1 H1 . 0.9900 ? N2 C1 2_566 1.494(4) ? N2 C9 . 1.498(4) ? N2 H2 . 0.9900 ? C1 C2 . 1.528(5) ? C1 C6 . 1.537(5) ? C1 H1A . 0.9900 ? C2 C3 . 1.528(5) ? C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C3 C4 . 1.528(6) ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C4 C5 . 1.518(5) ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C5 C6 . 1.530(5) ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C6 H6 . 0.9900 ? C7 C8 . 1.519(5) ? C7 H7A . 0.9800 ? C7 H7B . 0.9800 ? C8 C9 . 1.525(5) ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C9 C10 . 1.519(5) ? C9 H9 . 0.9900 ? C10 C11 . 1.531(5) ? C10 H10A . 0.9800 ? C10 H10B . 0.9800 ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C11 H11C . 0.9700 ? Cu2 N3 . 2.017(3) ? Cu2 N3 2_667 2.017(3) ? Cu2 N4 . 2.023(3) ? Cu2 N4 2_667 2.023(3) ? O2 H1O2 . 0.961(10) ? O2 H2O2 . 0.963(10) ? N3 C18 . 1.490(4) ? N3 C17 . 1.492(4) ? N3 H3 . 0.9900 ? N4 C20 . 1.494(4) ? N4 C12 2_667 1.495(4) ? N4 H4 . 0.9900 ? C12 C17 . 1.523(5) ? C12 C13 . 1.526(5) ? C12 H12 . 0.9900 ? C13 C14 . 1.526(5) ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C14 C15 . 1.522(6) ? C14 H14A . 0.9800 ? C14 H14B . 0.9800 ? C15 C16 . 1.521(5) ? C15 H15A . 0.9800 ? C15 H15B . 0.9800 ? C16 C17 . 1.526(5) ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C17 H17 . 0.9900 ? C18 C19 . 1.514(5) ? C18 H18A . 0.9800 ? C18 H18B . 0.9800 ? C19 C20 . 1.516(5) ? C19 H19A . 0.9800 ? C19 H19B . 0.9800 ? C20 C21 . 1.520(6) ? C20 H20 . 0.9900 ? C21 C22 . 1.533(6) ? C21 H21A . 0.9800 ? C21 H21B . 0.9800 ? C22 H22A . 0.9700 ? C22 H22B . 0.9700 ? C22 H22C . 0.9700 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1O1 Br1 2_666 0.958(10) 2.38(2) 3.299(3) 160(5) yes O1 H2O1 Br1 . 0.960(10) 2.39(2) 3.314(3) 161(5) yes O2 H1O2 Br2 2_667 0.961(10) 2.353(12) 3.311(4) 176(6) yes O2 H2O2 Br2 1_655 0.963(10) 2.382(17) 3.335(4) 170(6) yes N1 H1 Br1 . 0.99 2.54 3.517(3) 170.5 yes N2 H2 O1 . 0.99 2.59 3.161(4) 116.3 yes N3 H3 Br2 . 0.99 2.44 3.373(3) 157.0 yes N4 H4 O2 1_455 0.99 1.98 2.957(5) 169.2 yes C10 H10A O1 2_566 0.98 2.47 3.378(5) 154.4 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N2 C1 C2 C3 2_566 . . . -172.3(3) ? C6 C1 C2 C3 . . . . -52.1(4) ? C1 C2 C3 C4 . . . . 55.5(5) ? C2 C3 C4 C5 . . . . -59.7(5) ? C3 C4 C5 C6 . . . . 59.7(5) ? C7 N1 C6 C5 . . . . -61.5(4) ? Cu1 N1 C6 C5 . . . . 169.1(3) ? C7 N1 C6 C1 . . . . 175.5(3) ? Cu1 N1 C6 C1 . . . . 46.0(3) ? C4 C5 C6 N1 . . . . -176.1(3) ? C4 C5 C6 C1 . . . . -55.7(4) ? N2 C1 C6 N1 2_566 . . . -58.0(3) ? C2 C1 C6 N1 . . . . 177.2(3) ? N2 C1 C6 C5 2_566 . . . 177.1(3) ? C2 C1 C6 C5 . . . . 52.3(4) ? C6 N1 C7 C8 . . . . 178.4(3) ? Cu1 N1 C7 C8 . . . . -56.6(3) ? N1 C7 C8 C9 . . . . 76.6(4) ? C1 N2 C9 C10 2_566 . . . 52.8(4) ? Cu1 N2 C9 C10 . . . . -79.2(3) ? C1 N2 C9 C8 2_566 . . . -179.8(3) ? Cu1 N2 C9 C8 . . . . 48.3(3) ? C7 C8 C9 N2 . . . . -69.3(4) ? C7 C8 C9 C10 . . . . 57.0(4) ? N2 C9 C10 C11 . . . . 177.9(3) ? C8 C9 C10 C11 . . . . 53.6(4) ? N4 C12 C13 C14 2_667 . . . 177.4(3) ? C17 C12 C13 C14 . . . . 56.0(4) ? C12 C13 C14 C15 . . . . -55.6(5) ? C13 C14 C15 C16 . . . . 55.8(5) ? C14 C15 C16 C17 . . . . -56.3(5) ? C18 N3 C17 C12 . . . . -178.7(3) ? Cu2 N3 C17 C12 . . . . -43.5(3) ? C18 N3 C17 C16 . . . . 59.5(4) ? Cu2 N3 C17 C16 . . . . -165.4(3) ? N4 C12 C17 N3 2_667 . . . 54.6(3) ? C13 C12 C17 N3 . . . . 179.5(3) ? N4 C12 C17 C16 2_667 . . . 178.3(3) ? C13 C12 C17 C16 . . . . -56.7(4) ? C15 C16 C17 N3 . . . . 176.2(3) ? C15 C16 C17 C12 . . . . 56.9(4) ? C17 N3 C18 C19 . . . . 176.7(3) ? Cu2 N3 C18 C19 . . . . 47.4(4) ? N3 C18 C19 C20 . . . . -68.4(4) ? C12 N4 C20 C19 2_667 . . . 173.1(3) ? Cu2 N4 C20 C19 . . . . -57.8(3) ? C12 N4 C20 C21 2_667 . . . -60.9(4) ? Cu2 N4 C20 C21 . . . . 68.2(4) ? C18 C19 C20 N4 . . . . 74.7(4) ? C18 C19 C20 C21 . . . . -50.3(4) ? N4 C20 C21 C22 . . . . -179.8(4) ? C19 C20 C21 C22 . . . . -55.8(5) ? _cod_database_fobs_code 2243844