#------------------------------------------------------------------------------ #$Date: 2019-10-25 07:02:28 +0300 (Fri, 25 Oct 2019) $ #$Revision: 219510 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021796.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_2021796 loop_ _publ_author_name 'Clendening, Reese A.' 'Zeller, Matthias' 'Ren, Tong' _publ_section_title ; Crystal structures of two (5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III) complexes ; _journal_coeditor_code CU3157 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619013925 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '[Fe Cl2 (C16 H36 N4)] [Fe Cl4]' _chemical_formula_moiety 'C16 H36 Cl2 Fe N4 +, Cl4 Fe -' _chemical_formula_sum 'C16 H36 Cl6 Fe2 N4' _chemical_formula_weight 608.89 _chemical_name_systematic ; Dichlorido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III) tetrachloridoferrate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 95.3558(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.5569(2) _cell_length_b 19.1663(5) _cell_length_c 20.2946(5) _cell_measurement_reflns_used 9909 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 80.2194 _cell_measurement_theta_min 3.1759 _cell_volume 2539.32(12) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) and SHELXLE (H\"ubschle et al., 2011) ; _computing_structure_solution ; SHELXM (Sheldrick, 2008) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 7.4074 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Bruker AXS D8 Quest CMOS' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'laterally graded multilayer (Goebel) mirror' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_unetI/netI 0.0365 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 26483 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 81.308 _diffrn_reflns_theta_min 3.178 _diffrn_source 'I-mu-S microsource X-ray tube' _exptl_absorpt_coefficient_mu 15.058 _exptl_absorpt_correction_T_max 0.7543 _exptl_absorpt_correction_T_min 0.4258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (Krause et al., 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.593 _exptl_crystal_description Plate _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.760 _refine_diff_density_min -0.569 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 5481 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0318 _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^)+(0.0331P)^2^+2.0722P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0858 _reflns_number_gt 4930 _reflns_number_total 5481 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cu3157sup1.cif _cod_data_source_block 2 _cod_database_code 2021796 _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 0.172 _shelx_estimated_absorpt_t_max 0.520 _shelx_hkl_file ; -1 0 0 530.147 28.9067 2 -4 0 0 473.288 24.0523 10 -4 0 0 426.329 24.8921 11 -4 0 0 427.748 24.6743 12 -4 0 0 419.595 23.9225 8 -4 0 0 433.966 23.6795 7 -4 0 0 470.864 25.9825 9 -4 0 0 383.901 24.8783 4 -4 0 0 405.030 23.9897 5 -4 0 0 418.147 26.0262 2 -5 0 0 31.3028 7.14823 2 -5 0 0 39.9456 6.71867 13 -6 0 0 587.887 35.7126 9 -6 0 0 559.971 32.5312 10 -6 0 0 571.918 34.2744 11 -6 0 0 578.221 32.8087 8 -6 0 0 573.055 33.7436 12 -6 0 0 578.634 32.7586 5 -6 0 0 589.736 34.4976 4 -6 0 0 564.053 32.0670 7 -7 0 0 81.8406 10.5547 9 -7 0 0 98.1268 10.7651 12 -7 0 0 80.6020 7.73251 8 -7 0 0 83.0859 9.61564 11 -7 0 0 69.1461 10.6981 4 -7 0 0 72.1177 8.81473 5 -7 0 0 86.0323 7.08315 7 -7 0 0 77.8272 8.16123 10 0 -1 0 0.23041 0.21684 2 0 1 0 0.00468 0.31476 1 1 -1 0 1639.27 84.9937 1 1 -1 0 1590.92 84.9439 1 -1 -1 0 1775.15 85.2106 1 -1 -1 0 1525.59 84.9338 2 -1 -1 0 1515.14 84.7716 1 -1 1 0 1414.19 84.7457 2 -2 -1 0 647.731 35.8438 2 -2 1 0 645.016 35.6437 2 -3 -1 0 52.0976 5.69068 2 -3 1 0 53.3000 5.34744 2 -4 -1 0 56.2225 5.65466 12 -4 -1 0 45.9706 5.93223 4 -4 -1 0 59.4081 4.82343 10 -4 -1 0 55.1216 7.12949 2 -4 -1 0 59.4038 4.63183 8 -4 -1 0 46.1261 4.70140 5 -4 -1 0 52.0935 4.25652 7 -4 -1 0 57.5925 5.26744 11 -4 -1 0 56.5033 7.01479 9 -4 1 0 48.3629 5.93318 4 -4 1 0 51.4240 5.97309 11 -4 1 0 50.2400 7.10234 9 -4 1 0 54.7359 4.83841 10 -4 1 0 47.5589 4.65442 5 -4 1 0 45.6671 4.65781 8 -4 1 0 46.0708 4.19499 7 -4 1 0 51.5891 6.80571 2 -4 1 0 52.9616 5.88407 12 -5 -1 0 25.7007 7.77525 9 -5 -1 0 9.28904 6.07195 2 -5 -1 0 18.6639 5.75162 13 -5 1 0 9.70566 5.53422 2 -5 1 0 27.1197 10.9208 9 -5 1 0 22.3114 4.37937 10 -5 1 0 29.3042 6.25923 13 -5 1 0 16.2744 4.70167 7 -6 -1 0 929.662 50.7104 8 -6 -1 0 911.690 51.5460 12 -6 -1 0 922.036 50.6317 5 -6 -1 0 913.881 50.0079 7 -6 -1 0 888.671 50.4163 10 -6 -1 0 921.973 52.2435 4 -6 -1 0 906.473 51.8932 11 -6 -1 0 962.742 53.2938 9 -6 -1 0 844.281 53.9582 2 -6 -1 0 811.613 51.8189 13 -6 1 0 915.853 50.4585 10 -6 1 0 912.374 52.0695 11 -6 1 0 948.842 52.2234 4 -6 1 0 950.964 50.8491 8 -6 1 0 922.854 50.0689 7 -6 1 0 914.566 51.4882 12 -6 1 0 915.125 50.6742 5 -6 1 0 958.404 53.2985 9 -7 -1 0 34.1549 5.63892 5 -7 -1 0 45.5153 6.04387 8 -7 -1 0 36.4466 5.36512 10 -7 -1 0 42.6587 7.51373 12 -7 -1 0 21.2288 7.11538 9 -7 -1 0 38.6369 7.14210 4 -7 -1 0 42.9675 4.56159 7 -7 -1 0 43.9918 7.94603 11 -7 1 0 36.8123 4.70826 7 -7 1 0 32.9064 5.50517 10 -7 1 0 40.4752 7.95139 11 -7 1 0 44.8605 7.14933 12 -7 1 0 42.0871 5.79485 5 -7 1 0 33.7694 7.16025 9 -7 1 0 40.2919 6.01925 8 0 -2 0 1631.39 88.3948 1 -1 -2 0 595.545 33.3754 2 -1 -2 0 609.446 33.6600 1 1 -2 0 628.516 33.9126 1 -1 -2 0 639.220 33.7778 1 1 -2 0 625.389 33.8742 1 -1 2 0 560.421 33.0958 2 2 -2 0 860.000 43.4910 1 2 -2 0 794.716 43.2894 1 -2 -2 0 784.394 43.5697 2 -2 -2 0 798.140 43.0936 1 -2 -2 0 736.106 42.8727 1 -2 2 0 758.994 43.2021 2 -3 -2 0 539.702 30.0940 2 -3 2 0 499.549 29.5817 2 -4 -2 0 1333.40 68.5879 5 -4 -2 0 1244.26 68.2462 8 -4 -2 0 1317.98 68.2360 10 -4 -2 0 1232.37 69.2512 12 -4 -2 0 1190.12 69.2848 4 -4 -2 0 1249.92 70.3930 9 -4 -2 0 1238.02 67.9604 7 -4 -2 0 1202.40 68.8843 11 -4 -2 0 1300.41 70.5565 2 -4 2 0 1219.32 68.2606 8 -4 2 0 1335.72 70.3316 2 -4 2 0 1215.65 69.0639 11 -4 2 0 1342.89 68.2167 7 -4 2 0 1283.54 69.9132 9 -4 2 0 1295.44 68.3136 10 -4 2 0 1184.39 69.1401 4 -4 2 0 1221.67 68.2687 5 -4 2 0 1258.97 68.8960 12 -5 -2 0 2.92714 3.78136 8 -5 -2 0 5.25676 5.48033 4 -5 -2 0 9.06346 5.15225 12 -5 -2 0 0.72901 5.45105 11 -5 -2 0 3.56770 5.19308 13 -5 -2 0 3.83584 3.52094 5 -5 -2 0 4.67449 5.82166 2 -5 -2 0 4.95941 6.26340 9 -5 2 0 8.81830 5.51783 4 -5 2 0 5.24615 3.23180 7 -5 2 0 2.15698 5.51772 11 -5 2 0 8.28000 3.83639 10 -5 2 0 5.81442 9.76817 9 -5 2 0 11.9314 5.76155 13 -6 -2 0 46.0414 7.89368 12 -6 -2 0 55.1493 8.34175 4 -6 -2 0 51.6700 8.55060 2 -6 -2 0 56.0225 6.52485 5 -6 -2 0 52.1539 5.18284 7 -6 -2 0 62.8283 9.69605 13 -6 -2 0 64.6943 10.2028 9 -6 -2 0 58.2101 6.11171 10 -6 -2 0 42.6192 6.43302 8 -6 -2 0 54.5039 8.56496 11 -6 2 0 52.5848 8.61541 11 -6 2 0 49.1166 6.62420 8 -6 2 0 53.2127 5.41131 7 -6 2 0 48.6708 6.34497 10 -6 2 0 59.2385 9.44811 9 -6 2 0 53.8833 6.62431 5 -6 2 0 65.9866 8.68754 4 -6 2 0 51.4613 7.46237 12 -7 -2 0 58.4949 8.21816 4 -7 -2 0 58.3260 8.84683 9 -7 -2 0 49.3962 6.36025 8 -7 -2 0 57.5295 6.37034 5 -7 -2 0 46.1218 5.62989 10 -7 -2 0 50.6912 4.91148 7 -7 -2 0 57.4765 8.46638 11 -7 2 0 56.2227 8.48975 11 -7 2 0 45.0657 7.12909 12 -7 2 0 41.8450 5.20709 7 -7 2 0 52.2981 9.82137 9 -7 2 0 44.4899 6.56157 5 -7 2 0 49.6569 6.00387 10 0 -3 0 0.36241 0.94343 1 0 -3 0 -0.3880 1.05685 1 0 -3 0 -0.0536 0.65666 2 1 -3 0 1898.25 97.9826 1 -1 -3 0 1825.73 97.7167 1 -1 -3 0 1664.18 97.4796 1 -1 -3 0 1753.48 96.8270 2 1 -3 0 1829.97 97.8581 1 -2 -3 0 1027.33 55.2905 1 -2 -3 0 1005.19 55.2507 2 2 -3 0 992.652 55.6165 1 -2 -3 0 1043.38 55.4304 1 2 -3 0 1024.98 55.7448 1 -2 3 0 934.377 54.7635 2 -3 -3 0 1599.07 86.6382 2 -3 3 0 1554.70 86.1081 2 -4 -3 0 44.2526 5.93263 12 -4 -3 0 39.1781 4.25165 10 -4 -3 0 42.4684 6.04886 4 -4 -3 0 44.0110 6.81868 2 -4 -3 0 42.4068 6.85187 9 -4 -3 0 38.4170 4.22783 5 -4 -3 0 33.7022 3.48660 7 -4 3 0 40.7784 4.60813 10 -4 3 0 33.0436 5.54551 13 -4 3 0 33.3576 3.88481 8 -4 3 0 42.7985 5.99588 2 -4 3 0 40.1606 5.19490 12 -4 3 0 33.0027 4.05852 5 -4 3 0 36.5098 6.48047 9 -4 3 0 41.1773 3.44931 7 -5 -3 0 782.478 45.5548 4 -5 -3 0 797.190 44.1806 10 -5 -3 0 812.268 46.0265 13 -5 -3 0 808.837 45.0453 12 -5 -3 0 847.269 46.8009 9 -5 -3 0 788.392 43.7557 7 -5 -3 0 757.969 45.0257 11 -5 -3 0 778.024 44.0496 8 -5 -3 0 840.496 47.6123 2 -5 -3 0 807.732 44.1051 5 -5 3 0 788.867 43.9998 10 -5 3 0 815.881 45.5281 4 -5 3 0 734.241 44.8726 12 -5 3 0 815.213 43.6624 7 -5 3 0 806.095 44.4139 8 -5 3 0 778.982 45.3056 11 -6 -3 0 15.8852 7.15772 11 -6 -3 0 19.3268 6.83631 12 -6 -3 0 13.6650 6.91673 2 -6 -3 0 20.2690 7.07179 4 -6 -3 0 16.0171 3.81938 7 -6 -3 0 2.69273 6.29057 13 -6 -3 0 17.3136 8.12743 9 -6 -3 0 14.2147 4.53547 10 -6 -3 0 19.5777 5.24948 5 -6 -3 0 14.6695 5.21954 8 -6 3 0 19.6531 5.57795 5 -6 3 0 22.1117 6.02653 12 -6 3 0 14.6417 5.15424 10 -6 3 0 11.7976 7.30265 9 -6 3 0 13.5239 7.08256 11 -6 3 0 12.5808 5.42636 8 -6 3 0 17.4598 6.74156 4 -6 3 0 20.3874 4.41675 7 -7 -3 0 43.3172 5.29190 7 -7 -3 0 47.3637 7.33580 4 -7 -3 0 44.7503 7.96349 12 -7 -3 0 60.9428 6.58014 8 -7 -3 0 57.3425 7.63560 5 -7 -3 0 54.1010 10.1282 9 -7 3 0 41.4220 5.91493 10 -7 3 0 61.3776 9.49726 9 -7 3 0 51.7212 6.98419 12 -7 3 0 51.2966 8.40215 11 0 -4 0 3399.56 184.174 1 1 -4 0 5646.33 288.273 1 -1 -4 0 5163.88 287.703 1 -1 -4 0 5097.41 287.791 1 1 -4 0 5447.21 288.106 1 2 -4 0 279.127 17.7342 1 -2 -4 0 279.531 17.3513 1 2 -4 0 280.024 17.7164 1 -2 -4 0 289.492 16.9719 2 -2 -4 0 282.916 17.3008 1 3 -4 0 3205.95 177.084 1 3 -4 0 3167.94 177.303 1 -3 -4 0 3459.83 177.739 2 -4 -4 0 144.330 10.8396 11 -4 -4 0 149.740 9.19029 7 -4 -4 0 148.750 11.6091 4 -4 -4 0 154.393 9.54800 10 -4 -4 0 146.715 9.74363 8 -4 -4 0 148.672 12.6650 2 -4 -4 0 157.351 9.89699 5 -4 -4 0 171.820 12.5159 9 -4 -4 0 161.682 10.9010 12 -4 4 0 135.380 9.53506 5 -4 4 0 158.220 9.86188 10 -4 4 0 164.894 9.43697 7 -4 4 0 163.928 11.5608 11 -4 4 0 157.098 11.0964 4 -4 4 0 143.388 11.5607 13 -4 4 0 164.965 11.5100 9 -5 -4 0 277.218 16.3974 7 -5 -4 0 276.028 18.6094 11 -5 -4 0 271.955 20.5034 2 -5 -4 0 278.620 16.7958 10 -5 -4 0 286.518 17.1416 8 -5 -4 0 285.891 19.0824 4 -5 -4 0 271.908 17.1826 5 -5 -4 0 302.024 18.6105 12 -5 -4 0 305.134 20.3691 9 -5 -4 0 287.061 19.5674 13 -5 4 0 291.501 17.3981 8 -5 4 0 283.542 17.1044 10 -5 4 0 283.022 19.0440 11 -5 4 0 270.727 18.8490 4 -5 4 0 288.973 18.0262 12 -5 4 0 263.200 20.5224 9 -5 4 0 299.267 16.6604 7 -6 -4 0 759.902 51.4311 9 -6 -4 0 829.988 48.1760 2 -7 -4 0 3.38028 4.68269 7 -7 -4 0 7.99995 4.95799 8 -7 -4 0 4.04737 6.12656 9 -7 -4 0 6.47760 4.55455 5 -7 4 0 6.08941 6.89295 11 -7 4 0 5.54170 5.51395 9 -7 4 0 6.68071 4.76638 10 -8 4 0 9.94944 3.91016 11 0 -5 0 1.59234 1.13749 2 0 -5 0 -0.5881 1.44676 1 0 -5 0 0.91530 1.52231 1 1 -5 0 226.470 14.6587 1 -1 -5 0 215.103 12.6386 2 1 -5 0 207.304 14.2988 1 -1 -5 0 201.316 14.2521 1 -1 -5 0 202.217 13.9820 1 2 -5 0 267.929 18.0113 1 -2 -5 0 270.144 17.4422 1 -2 -5 0 271.511 17.5129 1 2 -5 0 281.840 18.1549 1 3 -5 0 336.917 21.7543 1 -3 -5 0 374.157 21.8467 2 -3 -5 0 345.457 21.4006 1 -4 -5 0 63.3982 8.75697 2 -4 -5 0 73.1823 5.72225 10 -4 -5 0 75.4825 7.48246 11 -4 -5 0 72.4186 6.17355 8 -4 -5 0 84.9153 5.42164 7 -4 -5 0 78.3761 8.86779 9 -4 -5 0 72.5959 7.65016 12 -4 -5 0 77.5214 6.07944 5 -4 -5 0 72.6949 8.72903 13 -4 -5 0 68.1171 7.84137 4 -4 5 0 83.2189 6.33643 10 -4 5 0 68.5718 5.83406 5 -4 5 0 72.4030 6.95447 12 -4 5 0 76.0664 7.77166 9 -4 5 0 75.4278 8.07469 11 -4 5 0 69.9281 5.58875 7 -4 5 0 71.8870 6.31952 8 -4 5 0 77.9610 7.82018 4 -5 -5 0 836.111 47.2927 9 -5 -5 0 789.637 43.9421 7 -5 -5 0 830.669 44.5712 8 -5 -5 0 772.940 45.6433 11 -5 -5 0 823.690 44.6307 5 -5 -5 0 819.894 45.6425 12 -5 -5 0 836.768 46.4828 4 -5 -5 0 775.277 44.2189 10 -5 -5 0 806.807 47.9873 2 -5 5 0 812.081 45.9775 4 -5 5 0 809.134 44.5758 5 -5 5 0 749.835 46.0318 11 -5 5 0 832.325 44.1116 7 -5 5 0 746.394 45.1235 12 -5 5 0 838.202 46.5236 9 -5 5 0 800.007 44.4606 10 -5 5 0 798.008 44.6669 8 -6 -5 0 122.036 12.9983 11 -6 -5 0 118.398 9.89258 5 -6 -5 0 126.630 14.6845 9 -6 -5 0 120.420 12.5185 12 -6 -5 0 125.650 10.3015 8 -6 -5 0 100.590 9.10304 10 -6 -5 0 135.862 13.4319 2 -6 -5 0 97.9947 11.3649 13 -6 -5 0 118.543 12.2273 4 -6 -5 0 118.719 8.23070 7 -6 5 0 106.695 10.8060 12 -6 5 0 117.384 12.3294 9 -6 5 0 120.028 9.11028 7 -6 5 0 105.508 13.4272 11 -6 5 0 107.848 10.1427 10 -6 5 0 119.043 9.63280 5 -7 -5 0 0.86985 2.56260 7 -7 -5 0 -1.2914 9.34061 9 -7 -5 0 5.91780 10.0147 4 -8 5 0 25.7660 4.31698 11 0 -6 0 49.5685 3.82693 2 0 -6 0 47.9420 5.63820 1 0 -6 0 45.9872 5.67485 1 -1 -6 0 543.625 31.9129 1 -1 -6 0 537.138 29.4811 2 -1 -6 0 474.500 31.2701 1 1 -6 0 539.972 32.1541 1 -2 -6 0 1185.98 70.7039 1 -2 -6 0 1278.15 69.2457 2 -2 -6 0 1246.75 70.9734 1 2 -6 0 1324.60 71.8932 1 2 -6 0 1243.45 71.5109 1 -3 -6 0 1491.39 76.0154 2 3 -6 0 1289.43 76.8765 1 -3 -6 0 1312.39 76.4940 1 -4 -6 0 863.321 47.8066 12 -4 -6 0 843.772 49.7246 13 -4 -6 0 836.783 46.6205 10 -4 -6 0 844.843 46.8338 8 -4 -6 0 902.983 46.7207 7 -4 -6 0 821.961 48.3708 4 -4 -6 0 853.579 46.9458 5 -4 -6 0 926.706 50.0271 2 -4 -6 0 855.819 47.7998 11 -4 -6 0 903.500 48.9396 9 -4 6 0 860.929 46.5700 7 -4 6 0 826.187 47.9125 4 -4 6 0 818.232 46.8637 5 -4 6 0 890.934 46.8681 10 -4 6 0 803.639 48.0727 11 -4 6 0 845.079 47.4784 12 -4 6 0 876.084 48.3762 9 -4 6 0 837.751 46.9936 8 -5 -6 0 90.0186 11.3539 2 -5 -6 0 96.6394 8.26000 8 -5 -6 0 85.0751 10.6045 13 -5 -6 0 102.588 12.2332 9 -5 -6 0 103.822 10.5830 12 -5 -6 0 97.1694 11.0199 11 -5 -6 0 100.922 7.71435 10 -5 -6 0 87.9752 8.16354 5 -5 -6 0 96.9343 7.01853 7 -5 -6 0 77.6043 10.9184 4 -5 6 0 96.6135 9.20914 12 -5 6 0 101.662 8.31094 10 -5 6 0 84.8801 10.2977 11 -5 6 0 84.7037 7.95546 5 -5 6 0 90.7412 7.49134 7 -5 6 0 105.113 10.9172 9 -6 -6 0 74.0971 8.44893 5 -6 -6 0 66.9927 10.2609 2 -6 -6 0 94.2077 8.74533 8 -6 -6 0 71.1252 7.78273 10 -6 -6 0 83.3228 11.6845 4 -6 -6 0 85.3734 12.3551 9 -6 -6 0 85.8282 6.68595 7 -6 -6 0 71.7488 9.50035 13 -6 -6 0 77.3894 9.69251 12 -6 6 0 77.0733 10.3062 9 -6 6 0 97.0909 7.89306 7 -6 6 0 89.1421 8.82799 10 -6 6 0 74.5973 10.6443 11 -6 6 0 78.7106 9.52868 12 -7 -6 0 110.441 9.49743 8 -7 -6 0 78.4415 6.03678 7 -7 -6 0 77.2873 12.0560 9 -7 -6 0 88.0653 10.0378 4 -7 -6 0 93.0324 8.70981 5 -7 6 0 72.4043 10.0846 11 -7 6 0 82.6889 8.14862 12 -8 6 0 66.1969 6.50329 11 0 -7 0 -0.0174 1.53088 2 0 -7 0 0.44817 2.01052 1 0 -7 0 1.83328 2.05054 1 -1 -7 0 336.099 21.9911 1 -1 -7 0 319.891 21.5545 1 1 -7 0 317.539 18.1621 2 1 -7 0 308.834 21.8226 1 -1 -7 0 328.123 19.1019 2 1 -7 0 348.447 22.9931 1 2 -7 0 217.749 16.1061 1 -2 -7 0 213.284 13.5983 2 2 -7 0 203.523 15.8258 1 -2 -7 0 182.941 14.7790 1 3 -7 0 1235.29 76.1812 1 -3 -7 0 1391.38 73.0930 2 -3 -7 0 1284.94 74.4566 1 -4 -7 0 16.5803 5.37990 4 -4 -7 0 21.4764 3.02451 10 -4 -7 0 14.7566 3.63423 5 -4 -7 0 22.8167 5.43576 12 -4 -7 0 19.3881 6.12932 13 -4 -7 0 22.9840 3.77971 8 -4 -7 0 24.0647 5.92979 9 -4 -7 0 12.1323 6.19467 2 -4 -7 0 22.9662 2.69478 7 -4 7 0 25.9722 4.58720 12 -4 7 0 21.6384 4.74978 9 -4 7 0 15.5712 6.32475 11 -4 7 0 22.9555 3.37170 5 -4 7 0 29.9460 3.74982 10 -4 7 0 18.9679 3.05847 7 -5 -7 0 23.8027 7.93139 2 -5 -7 0 17.7171 4.61352 8 -5 -7 0 15.8436 6.80657 12 -5 -7 0 19.1077 6.61622 4 -5 -7 0 9.40907 7.34133 9 -5 -7 0 15.9343 3.12038 7 -5 -7 0 19.0214 4.64416 5 -5 -7 0 6.09786 6.33135 13 -5 -7 0 18.0045 3.62628 10 -5 7 0 11.1517 6.82654 11 -5 7 0 14.8009 3.85540 7 -5 7 0 16.4262 6.21238 9 -5 7 0 19.2655 4.56972 10 -5 7 0 19.6221 5.22368 12 -6 -7 0 145.757 22.8698 2 -6 -7 0 172.901 16.5637 9 -6 -7 0 186.012 12.4349 8 -6 -7 0 193.828 15.3793 4 -6 -7 0 160.695 10.6586 7 -6 -7 0 187.522 12.4685 5 -6 7 0 153.951 15.7693 11 -6 7 0 168.341 13.4757 9 -6 7 0 167.279 12.9140 12 -6 7 0 177.358 12.3497 10 -7 -7 0 123.620 9.44439 5 -7 -7 0 123.811 10.4879 4 -7 -7 0 123.624 10.1462 8 -7 7 0 125.689 9.66648 12 -7 7 0 111.733 12.5433 11 0 -8 0 4760.44 266.182 1 0 -8 0 5072.02 266.459 1 0 -8 0 4792.54 261.876 2 1 -8 0 194.532 15.3657 1 -1 -8 0 164.633 14.4727 1 -1 -8 0 184.817 14.5688 1 1 -8 0 180.689 14.7290 1 1 -8 0 173.400 10.5304 2 -1 -8 0 187.594 11.7456 2 2 -8 0 326.069 23.6882 1 2 -8 0 310.257 18.2446 2 -2 -8 0 367.256 25.6817 1 -2 -8 0 340.349 20.5293 2 -3 -8 0 2556.20 152.987 4 -3 -8 0 2857.38 151.568 8 -3 -8 0 3153.75 154.385 2 -3 -8 0 2940.34 152.489 12 -3 8 0 2597.41 153.192 11 -4 -8 0 47.9886 4.42405 7 -4 -8 0 53.4235 5.82454 8 -4 -8 0 62.2850 7.73381 4 -4 -8 0 55.0694 5.69399 5 -4 -8 0 47.7988 7.01732 12 -4 -8 0 52.2559 8.33887 13 -4 -8 0 48.0513 3.32096 6 -4 -8 0 52.4226 8.74434 2 -4 -8 0 50.1553 9.01060 9 -4 8 0 48.4861 4.93607 7 -4 8 0 45.2796 7.62748 11 -4 8 0 54.1990 5.72659 10 -4 8 0 59.3334 6.24523 12 -5 -8 0 626.843 34.4306 5 -5 -8 0 583.918 36.5020 13 -5 -8 0 623.128 36.8667 4 -5 -8 0 511.295 40.9474 2 -5 -8 0 650.870 37.2816 9 -5 -8 0 629.700 34.4038 8 -5 -8 0 602.719 33.7629 10 -5 -8 0 604.799 33.5640 7 -5 8 0 655.990 34.3127 10 -5 8 0 581.950 36.6196 11 -5 8 0 578.966 34.9608 12 -5 8 0 636.446 35.5838 9 -6 -8 0 405.071 29.0914 2 -6 -8 0 449.395 25.5163 5 -6 -8 0 470.493 25.8392 8 -6 -8 0 410.175 24.3698 7 -6 -8 0 453.035 28.8609 9 -6 -8 0 466.027 27.6653 4 -6 8 0 396.567 28.0785 11 -6 8 0 452.592 25.6356 10 -6 8 0 444.664 26.0582 12 -7 -8 0 129.844 9.14534 5 -7 -8 0 132.039 10.2264 4 -7 -8 0 127.480 9.30833 8 -7 8 0 99.5835 8.60551 12 -7 8 0 107.917 11.6821 11 0 -9 0 4.40021 2.95028 1 0 -9 0 3.90314 2.07978 2 0 -9 0 -1.0623 2.65115 1 -1 -9 0 15.5292 5.15278 1 -1 -9 0 12.6635 3.44383 2 1 -9 0 11.3497 4.07348 1 1 -9 0 22.0056 5.54048 1 -1 -9 0 12.5862 3.81799 1 1 -9 0 12.2900 2.03789 2 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118.508 16.6986 9 -6 1 10 116.165 9.82418 5 -6 1 10 110.527 10.8942 11 -6 1 10 103.671 16.0762 9 -6 1 10 102.676 12.5241 12 5 -1 -10 223.064 17.9517 3 -5 -1 10 207.673 14.9707 5 -5 -1 10 245.140 16.7855 12 -5 -1 10 223.334 19.8682 9 -5 -1 10 233.601 15.6574 11 -5 1 10 227.119 15.2469 11 -5 1 10 221.400 16.6484 12 5 1 -10 220.437 17.2426 3 -5 1 10 205.881 14.5638 5 -5 1 10 235.248 20.8810 9 -4 -1 10 1387.94 74.4130 11 -4 -1 10 1352.06 74.5377 5 -4 -1 10 1324.18 74.8045 12 4 -1 -10 1440.40 77.0062 3 -4 -1 10 1376.79 78.0070 9 -4 -1 10 1339.30 76.9333 2 -4 1 10 1308.02 74.9797 12 -4 1 10 1347.10 74.3191 5 -4 1 10 1213.61 75.4830 2 4 1 -10 1389.60 76.6426 3 -4 1 10 1417.33 78.6969 9 -4 1 10 1434.21 74.4291 11 3 -1 -10 313.465 19.5982 3 -3 -1 10 281.094 19.5607 2 -3 1 10 281.010 17.4022 12 3 1 -10 281.129 18.9741 3 -3 1 10 270.126 18.2523 2 -2 -1 10 429.686 29.2482 2 2 -1 -10 445.026 28.6415 3 -2 -1 10 503.520 34.9776 1 2 -1 -10 534.403 36.6620 1 2 1 -10 471.548 28.7555 3 -2 1 10 535.038 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16.5480 13 -4 3 -10 174.531 13.2233 4 -4 3 -10 175.050 13.9850 10 -4 3 -10 187.240 11.7635 7 -5 -3 -10 18.8549 6.55547 4 -5 -3 -10 9.31989 8.92508 13 -5 -3 -10 20.5221 5.98085 10 -5 -3 -10 18.1926 4.60572 8 -5 -3 -10 19.2589 5.56251 7 -5 3 -10 13.7950 9.23685 13 -5 3 -10 13.2689 4.72114 7 -5 3 -10 22.3460 6.22303 4 -5 3 -10 21.7474 6.62049 10 -6 -3 -10 6.56426 4.62652 7 -6 -3 -10 18.0135 8.08033 13 -6 -3 -10 6.69263 6.89224 10 -6 3 -10 9.61126 5.73162 10 -7 -3 -10 29.1443 3.51574 7 -7 -3 -10 24.1548 3.47948 10 -7 3 -10 19.2084 4.19086 10 -7 -4 10 24.5317 6.58967 9 -7 -4 10 32.6533 5.25047 5 -7 -4 10 30.4980 5.58610 12 -7 4 10 13.8993 5.98034 9 -7 4 10 37.1544 5.06159 11 -7 4 10 27.9932 6.55419 12 -6 -4 10 117.817 11.5641 5 6 -4 -10 105.704 12.5688 3 -6 -4 10 132.115 9.47068 8 -6 -4 10 127.124 15.3323 9 -6 -4 10 139.695 12.4567 12 -6 4 10 136.241 14.2092 12 -6 4 10 125.956 16.1688 9 -6 4 10 135.081 11.1001 11 -5 -4 10 420.135 25.1967 12 -5 -4 10 394.694 28.2654 9 -5 -4 10 358.577 27.9454 2 -5 -4 10 424.187 23.4464 8 -5 -4 10 405.600 25.0178 5 5 -4 -10 457.995 28.9997 3 -5 4 10 423.126 24.6233 11 -5 4 10 411.656 29.0433 9 -5 4 10 404.568 23.5244 5 -5 4 10 405.889 26.3880 12 -4 -4 10 130.917 10.4118 5 -4 -4 10 108.857 9.87693 12 -4 -4 10 116.295 13.7622 2 -4 -4 10 117.071 8.47272 8 4 -4 -10 128.235 15.8384 3 -4 -4 10 121.528 14.0135 9 -4 4 10 111.656 11.8828 12 -4 4 10 114.633 9.74426 11 -4 4 10 120.530 8.37057 5 -4 4 10 133.300 16.9269 9 4 4 -10 135.714 11.4131 3 -3 -4 10 366.029 31.3849 2 -3 -4 10 341.383 23.5022 9 3 -4 -10 357.362 23.0087 3 -3 4 10 335.547 21.4707 12 3 4 -10 365.710 22.3716 3 2 -4 -10 3542.47 186.572 3 -2 -4 10 3252.35 187.722 2 2 4 -10 3625.93 186.376 3 -2 4 10 3303.02 184.985 2 -1 -4 10 568.432 41.2211 1 1 -4 -10 592.367 35.3600 3 1 4 -10 644.226 43.1919 1 1 4 -10 630.356 35.6760 3 0 -4 10 153.719 15.3773 1 0 -4 -10 146.607 15.5720 1 0 -4 -10 132.057 10.5857 3 0 4 -10 146.094 15.7073 1 0 4 10 144.253 15.0878 1 -1 -4 -10 1379.37 76.8865 3 -1 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46.8514 3 3 5 -10 786.210 45.9282 3 -3 5 10 803.593 45.5861 12 2 -5 -10 123.663 10.8807 3 -2 -5 10 103.742 11.8917 2 2 5 -10 121.090 10.0520 3 -1 -5 10 3043.92 178.024 1 1 -5 -10 2727.05 159.116 3 1 -5 -10 2521.81 166.771 1 -1 5 10 2915.02 167.596 1 1 5 -10 3453.20 178.153 1 1 5 -10 3014.70 159.375 3 0 -5 -10 1688.51 93.3768 3 0 -5 10 1652.85 101.045 1 0 5 -10 1828.60 94.0243 3 0 5 10 1634.36 107.678 1 0 5 -10 1676.02 101.338 1 -1 -5 -10 48.6034 3.90331 6 -1 -5 -10 46.5687 6.26516 3 -1 5 -10 38.8556 7.15145 3 -1 5 -10 42.0637 3.69460 6 -2 -5 -10 1231.98 77.7857 3 -2 -5 -10 1422.60 75.7867 6 -2 -5 -10 1501.23 78.2088 13 -2 -5 -10 1316.92 76.8222 4 -2 5 -10 1352.37 75.7701 6 -2 5 -10 1611.52 78.8553 13 -3 -5 -10 225.795 13.0237 6 -3 -5 -10 230.575 14.2952 10 -3 -5 -10 215.129 13.2463 8 -3 -5 -10 211.988 14.4820 7 -3 -5 -10 238.234 17.3575 13 -3 -5 -10 238.692 15.3751 4 -3 5 -10 239.486 17.0491 13 -3 5 -10 223.021 13.3853 7 -3 5 -10 223.711 14.8661 10 -3 5 -10 226.760 14.5715 4 -3 5 -10 238.283 13.1235 6 -4 -5 -10 38.8824 3.41653 6 -4 -5 -10 39.0739 5.88743 7 -4 -5 -10 44.2368 6.90131 4 -4 -5 -10 45.7031 4.69505 8 -4 -5 -10 43.6257 9.79510 13 -4 -5 -10 40.9943 5.92684 10 -4 5 -10 52.8012 9.70383 13 -4 5 -10 40.5433 7.05354 10 -4 5 -10 37.4335 4.65441 7 -4 5 -10 27.5195 5.67178 11 -4 5 -10 34.1029 5.84282 4 -5 -5 -10 -1.0471 4.79493 7 -5 -5 -10 2.24476 3.93036 8 -5 -5 -10 -0.7715 8.45909 13 -5 -5 -10 -1.0897 4.89662 10 -5 -5 -10 1.62892 5.91014 4 -5 5 -10 -0.1535 6.21610 10 -5 5 -10 -1.1959 3.88860 7 -6 -5 -10 -0.2567 3.67252 10 -6 -5 -10 2.32998 4.46273 7 -6 -5 -10 -9.2366 9.02716 13 -6 5 -10 0.39680 5.49172 10 -6 5 -10 2.18734 3.32516 7 -7 -5 -10 7.91215 2.09413 7 -7 -5 -10 3.92061 2.11027 4 -7 5 -10 5.48875 2.41249 10 -7 -6 10 6.17799 4.27769 5 -7 -6 10 2.79688 4.64074 9 -7 6 10 2.62278 5.73400 9 -7 6 10 6.62641 5.17639 11 -7 6 10 10.0547 5.85776 12 -6 -6 10 797.005 43.4612 5 -6 -6 10 755.933 45.7275 9 -6 -6 10 771.523 43.0381 12 6 -6 -10 684.347 47.4477 3 -6 6 10 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31.9308 1 0 6 10 376.137 30.3911 1 0 6 -10 415.426 24.5436 3 -1 -6 -10 235.110 13.3473 6 -1 -6 -10 241.872 15.7087 3 -1 6 -10 226.492 13.3619 6 -1 6 -10 238.901 17.0182 3 -2 -6 -10 2125.79 119.393 4 -2 -6 -10 2025.08 120.108 3 -2 -6 -10 2151.31 118.745 10 -2 -6 -10 2217.08 118.284 6 -2 6 -10 2447.56 120.651 13 -2 6 -10 2232.18 118.295 6 -3 -6 -10 118.550 14.4070 4 -3 -6 -10 134.638 8.70047 8 -3 -6 -10 132.862 9.59381 10 -3 -6 -10 136.918 8.45895 6 -3 -6 -10 164.925 13.9297 13 -3 -6 -10 121.963 10.3069 7 -3 6 -10 159.590 11.5129 10 -3 6 -10 134.678 8.80052 7 -4 -6 -10 129.969 7.81132 6 -4 -6 -10 122.401 10.7997 7 -4 -6 -10 124.047 10.4773 10 -4 -6 -10 131.828 11.8736 4 -4 -6 -10 148.578 15.3239 13 -4 -6 -10 129.894 9.20551 8 -4 6 -10 142.789 9.61226 11 -4 6 -10 129.070 9.31350 7 -4 6 -10 137.153 12.0580 10 -5 -6 -10 69.7501 7.01367 10 -5 -6 -10 83.9308 9.99490 4 -5 -6 -10 69.2434 11.3446 13 -5 -6 -10 61.8982 7.25248 7 -5 -6 -10 75.9563 7.24347 8 -5 6 -10 75.5940 7.02173 11 -5 6 -10 62.8131 8.28345 10 -5 6 -10 75.0117 7.17950 7 -6 -6 -10 -1.1094 4.59532 4 -6 -6 -10 -0.1166 7.91411 13 -6 -6 -10 4.37815 4.21950 7 -6 -6 -10 -0.9206 2.95333 10 -6 6 -10 -0.0271 2.96221 7 -6 6 -10 3.74776 5.29783 10 -7 -6 -10 10.2168 1.89879 7 -7 -6 -10 6.70886 2.08069 4 -7 6 -10 7.42224 1.95349 10 -7 -7 10 124.013 9.50786 5 -7 -7 10 123.650 10.6977 9 -7 7 10 122.471 8.32268 11 -7 7 10 139.022 10.9046 12 -6 -7 10 2.65861 7.15998 9 6 -7 -10 5.07890 5.95799 3 -6 -7 10 4.90132 5.71636 5 -6 -7 10 4.39800 4.52134 8 -6 7 10 6.26429 7.46611 12 -6 7 10 1.96434 7.36949 9 -5 -7 10 205.818 19.5476 2 5 -7 -10 227.531 19.7407 3 -5 -7 10 202.498 14.9149 12 -5 -7 10 229.059 13.8408 8 -5 -7 10 214.503 18.8889 9 -5 7 10 215.303 15.0925 11 -5 7 10 215.163 23.3932 9 -4 -7 10 53.5968 7.03843 5 -4 -7 10 29.2250 5.40380 12 4 -7 -10 65.2198 10.5447 3 -4 -7 10 42.1952 10.5289 2 -4 -7 10 53.7901 5.50441 8 -4 -7 10 41.3016 8.37050 9 -4 7 10 40.1034 5.88279 11 -4 7 10 23.7392 8.13687 12 -4 7 10 51.5837 10.9905 9 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10 -4 5 23 0.46857 2.31494 9 -3 -5 23 29.5341 3.71222 5 -3 5 23 33.7929 5.77863 9 2 -5 -23 13.4959 2.16204 6 -2 -5 23 20.5352 3.41868 5 2 5 -23 14.4189 2.12953 6 1 -5 -23 660.175 35.8818 6 0 -5 -23 10.0560 3.11204 10 0 -5 -23 13.1487 2.37075 7 0 -5 -23 13.7766 2.45133 6 0 5 -23 9.46279 2.49260 6 -1 -5 -23 61.9139 4.61953 7 -1 -5 -23 71.4570 5.01051 6 -1 -5 -23 66.1306 5.28620 10 -1 5 -23 69.7394 4.97824 6 -1 5 -23 80.0020 6.06825 10 -2 -5 -23 25.5467 2.00730 6 -2 5 -23 21.9471 2.83645 10 -3 -6 23 4.33477 2.33440 5 -3 -6 23 3.72014 1.65330 6 -3 6 23 3.37709 4.06277 9 2 -6 -23 137.050 8.30258 6 -2 -6 23 144.586 8.99044 5 1 -6 -23 56.9838 4.38517 7 1 6 -23 60.1614 4.59345 6 0 -6 -23 82.0940 6.07028 10 0 -6 -23 83.6660 5.85947 6 0 -6 -23 81.9583 6.05729 7 0 6 -23 97.7591 6.09940 6 0 6 -23 93.8318 6.96850 10 -1 -6 -23 73.6236 4.78561 6 -1 -6 -23 68.2667 4.76697 7 -1 6 -23 72.8570 6.08985 10 -2 -6 -23 5.86636 1.26606 6 -2 6 -23 3.08902 1.83439 10 -3 -7 23 55.7076 3.69958 6 -3 7 23 57.6752 5.74660 9 -2 -7 23 32.6001 4.06258 5 2 -7 -23 17.6280 2.88128 6 2 -7 -23 26.0442 2.46171 7 -2 -7 23 32.6770 3.17030 6 -2 7 23 32.8644 6.11145 9 1 -7 -23 63.6045 4.99303 6 1 -7 -23 71.7732 4.62748 7 1 -7 -23 63.7325 5.58821 10 0 -7 23 81.8548 5.44925 6 0 -7 -23 84.3201 5.55713 6 0 -7 -23 76.0687 5.28327 7 0 7 -23 83.2530 5.41047 6 0 7 -23 81.6226 6.43909 10 -1 -7 -23 124.645 7.81335 7 -1 -7 -23 146.419 7.94494 6 -2 7 -23 67.0802 4.48067 10 -3 -8 23 0.87259 1.87016 5 -3 -8 23 0.62595 0.99063 6 -3 8 23 -1.0727 2.66022 9 -2 -8 23 4.00941 2.56704 6 2 -8 -23 1.89596 1.52005 7 -2 -8 23 0.84797 3.73347 5 -2 8 23 2.19479 3.69654 9 1 -8 -23 52.1665 4.20265 6 -1 -8 23 62.6307 4.60544 6 1 -8 -23 51.3502 3.97466 7 0 -8 23 0.07834 1.66515 6 0 -8 -23 -1.6918 1.72809 6 0 -8 -23 -0.3282 1.62677 7 0 8 -23 -0.1084 2.15845 10 -1 -8 -23 7.79656 1.61060 6 -1 -8 -23 8.92218 1.56107 7 -1 8 -23 7.43014 2.17858 10 -2 -9 23 3.94201 1.42608 6 -2 -9 23 6.57978 2.14138 5 2 -9 -23 5.10912 1.12807 7 -2 9 23 1.06127 3.01979 9 1 -9 -23 150.533 8.67391 6 0 -9 -23 43.2853 3.41940 6 0 -9 -23 42.9121 3.37327 7 -1 -9 -23 145.936 8.33595 7 -1 -9 -23 147.168 8.14951 6 -2 10 23 72.4778 5.06668 9 1 -10 -23 -0.5324 1.33824 7 -1 -10 23 0.05610 1.19904 6 -1 -10 23 0.34952 1.78768 5 1 -10 -23 -0.5167 1.76678 6 -1 10 23 0.85125 2.73660 9 0 -10 -23 15.8335 2.14671 7 0 -11 23 15.8177 1.95597 5 0 -11 -23 16.0282 1.68736 6 -3 0 24 43.8291 4.71664 9 -2 0 24 293.070 20.4343 9 2 0 -24 348.028 17.7395 6 -1 0 24 28.9681 5.12202 9 0 0 -24 33.7609 3.62758 6 -1 0 -24 38.4892 3.28048 6 -1 0 -24 31.7561 3.59374 10 -3 -1 24 18.2499 3.16296 9 -3 1 24 30.6605 4.59031 9 2 -1 -24 7.10618 1.72473 6 -2 -1 24 3.79259 3.49821 9 -2 1 24 0.80168 4.18704 9 2 1 -24 2.98359 1.56535 6 1 -1 -24 36.0960 3.65577 6 -1 -1 24 27.7329 4.96994 9 1 1 -24 31.8377 3.00275 6 0 -1 -24 21.1369 2.70210 6 0 1 -24 31.7380 2.85965 6 -1 -1 -24 13.1546 1.94193 6 -1 -1 -24 13.0353 3.31985 10 -1 1 -24 13.4444 2.97915 10 -1 1 -24 15.0306 2.04787 6 -2 -1 -24 29.3072 3.07350 10 -2 1 -24 21.1645 2.43556 10 -3 2 24 156.277 10.4860 9 -2 -2 24 95.9711 6.71309 9 -2 2 24 58.0068 7.52636 9 2 2 -24 74.1280 5.18074 6 -1 -2 24 2.20746 3.57149 9 1 -2 -24 0.23911 1.94383 6 1 2 -24 0.99665 1.96289 6 0 -2 -24 50.1725 4.09628 6 0 -2 -24 49.9520 5.37649 10 0 2 -24 48.5411 4.27630 6 -1 -2 -24 145.774 9.37161 10 -1 -2 -24 138.718 8.08165 6 -1 2 -24 129.007 8.98184 10 -1 2 -24 147.172 8.18472 6 -2 -2 -24 2.14860 1.93277 10 -2 2 -24 3.04826 1.65856 10 -3 3 24 41.7568 5.03508 9 -2 -3 24 46.4196 3.79800 5 2 3 -24 49.2845 3.65054 6 -2 3 24 39.1861 7.50179 9 1 -3 -24 32.1375 3.54735 6 1 3 -24 32.3795 3.70399 6 0 -3 -24 15.6154 2.36894 6 0 -3 -24 16.9527 3.10877 10 0 3 -24 13.9190 2.30323 6 0 3 -24 18.4583 3.61338 10 -1 -3 -24 17.6171 2.50743 10 -1 -3 -24 22.9520 2.34397 6 -1 3 -24 17.7061 2.28509 6 -1 3 -24 17.0490 2.95024 10 -2 3 -24 23.8195 2.75190 10 -3 4 24 6.12049 2.72659 9 2 -4 -24 56.5090 4.37319 6 -2 -4 24 63.4360 4.69624 5 -2 4 24 64.9484 7.42912 9 1 -4 -24 1.40596 2.33012 6 1 4 -24 1.94241 2.08628 6 0 -4 -24 164.789 9.67681 10 0 -4 -24 153.362 9.37027 6 0 4 -24 177.297 10.2460 10 0 4 -24 155.940 9.30710 6 -1 -4 -24 3.96746 1.79692 10 -1 -4 -24 4.53044 2.01821 6 -1 4 -24 5.35880 1.84009 6 -1 4 -24 1.98551 2.99221 10 -3 -5 24 31.4149 2.17807 6 -3 5 24 26.3589 3.81572 9 -2 -5 24 8.77517 2.07536 5 1 -5 -24 156.585 9.25884 6 1 5 -24 166.714 9.32489 6 0 -5 -24 14.1743 2.42754 10 0 -5 24 14.4480 2.10745 6 0 -5 -24 18.7657 2.31190 6 0 5 -24 18.5101 3.27753 10 0 5 -24 11.3284 2.37369 6 -1 -5 -24 0.91484 1.34853 6 -1 5 -24 0.53903 2.19453 10 -3 -6 24 19.9788 1.75747 6 -1 -6 24 1.01149 1.51792 6 1 -6 -24 1.57635 1.58212 6 1 6 -24 -0.1700 2.35967 10 -1 -6 -24 8.57995 1.19744 6 -1 6 -24 3.99182 1.73075 10 -2 -7 24 105.573 6.04085 6 -2 7 24 99.3316 7.41271 9 -1 -7 24 51.9962 3.65338 6 1 7 -24 53.1464 4.55568 10 0 -7 -24 2.65618 1.29678 6 0 7 -24 1.60119 2.13191 10 -1 -7 -24 82.9814 4.87268 6 -1 -8 24 3.68310 1.42006 6 -1 -8 24 2.48213 1.63914 5 1 -8 -24 4.93626 1.38596 6 -1 8 24 0.86136 2.66687 9 0 -8 -24 34.0080 2.44691 6 -1 -9 24 21.4804 2.61490 5 -1 9 24 12.4741 2.47484 9 0 -9 -24 0.42181 0.85931 6 1 0 -25 0.76528 1.28591 6 -1 0 25 0.49730 3.17043 9 0 0 -25 0.81844 2.40008 10 0 0 -25 -0.4748 1.36084 6 -1 0 -25 0.73550 0.91342 6 -1 0 -25 -1.4189 1.45511 10 -2 1 25 65.8415 4.91255 9 1 -1 -25 105.834 5.88879 6 1 1 -25 98.2096 5.86318 6 -1 1 25 90.9257 7.05215 9 0 -1 -25 102.173 6.24542 6 0 -1 -25 107.337 6.66800 10 0 1 -25 106.013 6.24914 6 0 1 -25 108.930 7.01118 10 -1 -1 -25 15.1234 2.25287 10 -1 -1 -25 25.7062 1.80228 6 -1 1 -25 20.5422 2.18152 10 -1 1 -25 23.3698 1.77370 6 -2 2 25 4.16952 2.66202 9 1 2 -25 86.2784 4.97022 6 -1 2 25 74.3472 6.53090 9 0 -2 -25 35.7620 3.34896 10 0 2 -25 37.7032 3.02950 6 0 2 -25 37.6574 3.80297 10 -1 -2 -25 17.8706 1.81488 6 -1 2 -25 9.98445 1.78997 10 -2 3 25 3.23430 2.80937 9 1 -3 -25 150.577 7.99868 10 -1 3 25 120.889 9.19979 9 0 -3 -25 21.1697 2.31323 10 0 3 -25 21.2468 2.62317 10 0 3 -25 22.0930 2.16032 6 -2 4 25 13.8177 2.85807 9 -1 4 25 29.4863 4.33628 9 0 -4 -25 61.9202 3.92393 6 -1 4 -25 4.79067 1.97383 10 -2 -5 25 22.6408 1.89044 6 -2 5 25 24.1903 3.45618 9 -1 5 25 18.3188 3.42946 9 -1 6 25 46.2384 4.75210 9 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7543 _exptl_absorpt_correction_T_min 0.4258 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54171 6.577 19.182 20.319 89.967 95.343 90.050 ) ; _shelx_hkl_checksum 51176 _shelx_res_file ; TITL RAC5_I132_0m in P2(1)/c RAC5I132_0m.res created by SHELXL-2018/3 at 11:31:20 on 05-Oct-2019 CELL 1.54178 6.55690 19.16630 20.29460 90.0000 95.3558 90.0000 ZERR 4.00 0.00020 0.00050 0.00050 0.0000 0.0015 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL FE UNIT 64 144 16 24 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.130 SIZE 0.05 0.09 0.18 L.S. 4 BOND $H ACTA CONF HTAB EQIV $1 -x, -y+2, -z HTAB N1 Cl6_$1 EQIV $4 x-1, y, z HTAB N2 Cl1_$4 EQIV $7 -x, -y+1, -z HTAB N3 Cl2_$7 HTAB N4 Cl4 SADI N1 H1 N2 H2 N3 H3 N4 H4 FMAP 2 PLAN 20 WGHT 0.033100 2.072200 FVAR 0.38212 C1 1 -0.049230 1.118126 0.106839 11.00000 0.03442 0.02036 = 0.01464 -0.00051 0.00179 0.00223 C2 1 -0.163344 1.187871 0.108975 11.00000 0.05302 0.02281 = 0.02832 -0.00427 0.00556 0.00802 AFIX 137 H2A 2 -0.084339 1.224426 0.089129 11.00000 -1.50000 H2B 2 -0.180296 1.200042 0.155047 11.00000 -1.50000 H2C 2 -0.298274 1.183688 0.084114 11.00000 -1.50000 AFIX 0 C3 1 0.155544 1.123265 0.148898 11.00000 0.04095 0.02867 = 0.01805 -0.00431 -0.00468 -0.00602 AFIX 137 H3A 2 0.231959 1.079690 0.145364 11.00000 -1.50000 H3B 2 0.131237 1.131251 0.195216 11.00000 -1.50000 H3C 2 0.234986 1.162156 0.133134 11.00000 -1.50000 AFIX 0 C4 1 -0.189679 1.063141 0.134133 11.00000 0.02957 0.02661 = 0.01744 -0.00151 0.00633 0.00336 AFIX 23 H4A 2 -0.215710 1.077966 0.179321 11.00000 -1.20000 H4AB 2 -0.322629 1.065052 0.106727 11.00000 -1.20000 AFIX 0 C5 1 -0.123115 0.986776 0.138203 11.00000 0.02393 0.02772 = 0.01076 0.00107 0.00467 -0.00082 AFIX 13 H5 2 0.027068 0.984812 0.152253 11.00000 -1.20000 AFIX 0 C6 1 -0.236952 0.947890 0.189018 11.00000 0.03132 0.03563 = 0.01842 0.00560 0.00892 -0.00141 AFIX 137 H6A 2 -0.384013 0.947843 0.174889 11.00000 -1.50000 H6B 2 -0.212902 0.971097 0.232071 11.00000 -1.50000 H6C 2 -0.187189 0.899710 0.192790 11.00000 -1.50000 AFIX 0 C7 1 -0.129420 0.878578 0.067706 11.00000 0.03132 0.02025 = 0.02123 0.00412 0.00666 -0.00233 AFIX 23 H7A 2 -0.238405 0.853989 0.089144 11.00000 -1.20000 H7AB 2 0.004589 0.865893 0.091186 11.00000 -1.20000 AFIX 0 C8 1 -0.135755 0.857813 -0.004325 11.00000 0.03809 0.01981 = 0.02383 0.00030 0.00620 -0.00557 AFIX 23 H8A 2 -0.107160 0.807318 -0.008034 11.00000 -1.20000 H8AB 2 -0.273230 0.867329 -0.026998 11.00000 -1.20000 AFIX 0 C9 1 0.358975 0.386003 0.098715 11.00000 0.02128 0.02220 = 0.01838 0.00271 0.00245 0.00052 C10 1 0.155802 0.356709 0.118530 11.00000 0.02587 0.03667 = 0.02866 0.00777 0.00465 -0.00459 AFIX 137 H10A 2 0.060053 0.395164 0.123661 11.00000 -1.50000 H10B 2 0.180228 0.331459 0.160515 11.00000 -1.50000 H10C 2 0.097286 0.324785 0.084078 11.00000 -1.50000 AFIX 0 C11 1 0.512151 0.326167 0.097348 11.00000 0.02883 0.02434 = 0.02536 0.00448 -0.00208 0.00613 AFIX 137 H11A 2 0.453000 0.288955 0.068458 11.00000 -1.50000 H11B 2 0.543601 0.307893 0.142246 11.00000 -1.50000 H11C 2 0.638195 0.343238 0.080461 11.00000 -1.50000 AFIX 0 C12 1 0.430913 0.440941 0.150584 11.00000 0.02277 0.02615 = 0.01533 0.00191 0.00434 0.00443 AFIX 23 H12A 2 0.320651 0.476148 0.151269 11.00000 -1.20000 H12B 2 0.442905 0.417652 0.194316 11.00000 -1.20000 AFIX 0 C13 1 0.630491 0.480064 0.144317 11.00000 0.02098 0.02511 = 0.01381 0.00058 -0.00072 0.00306 AFIX 13 H13 2 0.734764 0.446424 0.130329 11.00000 -1.20000 AFIX 0 C14 1 0.709557 0.511522 0.211113 11.00000 0.03450 0.03566 = 0.01495 -0.00207 -0.00379 -0.00009 AFIX 137 H14A 2 0.841309 0.534543 0.207154 11.00000 -1.50000 H14B 2 0.727466 0.474415 0.244372 11.00000 -1.50000 H14C 2 0.610562 0.545765 0.224616 11.00000 -1.50000 AFIX 0 C15 1 0.768010 0.583445 0.087051 11.00000 0.02017 0.02506 = 0.01790 -0.00602 -0.00031 -0.00422 AFIX 23 H15A 2 0.896328 0.556868 0.084148 11.00000 -1.20000 H15B 2 0.785607 0.613909 0.126568 11.00000 -1.20000 AFIX 0 C16 1 0.720978 0.627011 0.025421 11.00000 0.02376 0.02136 = 0.02134 -0.00338 0.00020 -0.00307 AFIX 23 H16A 2 0.600184 0.656944 0.030186 11.00000 -1.20000 H16B 2 0.838984 0.657466 0.018423 11.00000 -1.20000 AFIX 0 N1 3 -0.021089 1.101166 0.035396 11.00000 0.02423 0.01959 = 0.01518 -0.00139 0.00146 -0.00202 REM AFIX 13 H1 2 -0.139378 1.111412 0.013395 11.00000 -1.20000 REM AFIX 0 N2 3 -0.160940 0.955189 0.070704 11.00000 0.02168 0.02084 = 0.01419 0.00101 0.00092 0.00130 REM AFIX 13 H2 2 -0.288378 0.962736 0.056239 11.00000 -1.20000 REM AFIX 0 N3 3 0.320887 0.420670 0.031554 11.00000 0.01707 0.01895 = 0.01574 -0.00066 0.00099 0.00231 REM AFIX 13 H3 2 0.209386 0.444281 0.033546 11.00000 -1.20000 REM AFIX 0 N4 3 0.593954 0.534746 0.092366 11.00000 0.01549 0.02334 = 0.01426 -0.00179 0.00192 0.00095 REM AFIX 13 H4 2 0.489938 0.557572 0.104994 11.00000 -1.20000 REM AFIX 0 CL1 4 0.309358 0.977746 0.061269 11.00000 0.01947 0.02932 = 0.02119 0.00171 0.00196 -0.00010 CL2 4 0.219516 0.569509 0.002826 11.00000 0.01677 0.02306 = 0.02071 -0.00202 0.00231 0.00348 CL3 4 0.695854 0.741210 0.200823 11.00000 0.03219 0.04077 = 0.06582 0.00690 -0.00295 -0.00081 CL4 4 0.242037 0.637932 0.186175 11.00000 0.03897 0.02922 = 0.03742 -0.00163 0.00272 -0.00479 CL5 4 0.218253 0.822241 0.225649 11.00000 0.04633 0.03764 = 0.03100 -0.01294 -0.00298 0.00974 CL6 4 0.327596 0.767730 0.062908 11.00000 0.07668 0.04649 = 0.02434 0.00557 0.00804 0.03074 FE1 5 0.000000 1.000000 0.000000 10.50000 0.01756 0.01564 = 0.01196 0.00091 0.00293 -0.00026 FE2 5 0.500000 0.500000 0.000000 10.50000 0.01279 0.01689 = 0.01139 -0.00157 0.00103 0.00094 FE3 5 0.367703 0.742858 0.169402 11.00000 0.03218 0.02371 = 0.02228 0.00045 0.00095 0.00353 HKLF 4 REM RAC5_I132_0m in P2(1)/c REM wR2 = 0.0858, GooF = S = 1.111, Restrained GooF = 1.111 for all data REM R1 = 0.0318 for 4930 Fo > 4sig(Fo) and 0.0357 for all 5481 data REM 274 parameters refined using 6 restraints END WGHT 0.0331 2.0722 REM Instructions for potential hydrogen bonds HTAB C3 Cl1 EQIV $3 -x, y+1/2, -z+1/2 HTAB C4 Cl4_$3 HTAB C5 Cl1 HTAB C6 Cl1_$4 HTAB C7 Cl6 EQIV $5 -x+1, y-1/2, -z+1/2 HTAB C11 Cl5_$5 EQIV $2 -x+1, -y+1, -z HTAB C11 Cl2_$2 HTAB C13 Cl2_$2 EQIV $6 x+1, y, z HTAB C15 Cl2_$6 HTAB C15 Cl3 HTAB C16 Cl6 HTAB N1 Cl1_$1 HTAB N1 Cl6_$1 HTAB N2 Cl1_$4 HTAB N2 Cl1_$1 HTAB N3 Cl2 HTAB N3 Cl2_$7 HTAB N4 Cl4 REM Highest difference peak 0.760, deepest hole -0.569, 1-sigma level 0.072 Q1 1 0.2296 0.7398 0.1585 11.00000 0.05 0.76 Q2 1 0.2125 0.7489 0.0625 11.00000 0.05 0.71 Q3 1 0.5252 0.7509 0.1993 11.00000 0.05 0.35 Q4 1 0.3346 0.6803 0.1779 11.00000 0.05 0.35 Q5 1 0.8290 0.7366 0.1954 11.00000 0.05 0.34 Q6 1 -0.1065 0.9877 0.0524 11.00000 0.05 0.34 Q7 1 0.0280 1.0634 0.0181 11.00000 0.05 0.33 Q8 1 -0.1314 1.0951 0.1201 11.00000 0.05 0.31 Q9 1 0.3495 0.6405 0.1991 11.00000 0.05 0.31 Q10 1 -0.1102 0.9753 0.1016 11.00000 0.05 0.31 Q11 1 0.4134 0.7378 0.1115 11.00000 0.05 0.31 Q12 1 0.3222 0.8389 0.2179 11.00000 0.05 0.31 Q13 1 0.6688 0.7441 0.1597 11.00000 0.05 0.31 Q14 1 0.4353 0.3590 0.0973 11.00000 0.05 0.30 Q15 1 0.3822 0.7541 0.0704 11.00000 0.05 0.27 Q16 1 -0.1662 0.9735 0.1695 11.00000 0.05 0.27 Q17 1 0.1411 1.0050 0.0502 11.00000 0.05 0.27 Q18 1 0.6084 0.5148 0.0540 11.00000 0.05 0.27 Q19 1 0.7410 0.8024 0.1819 11.00000 0.05 0.27 Q20 1 -0.1638 1.0262 0.1315 11.00000 0.05 0.26 ; _shelx_res_checksum 61502 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 C C1 -0.0492(4) 1.11813(12) 0.10684(11) 0.0232(5) Uani d 1 C C2 -0.1633(5) 1.18787(14) 0.10898(14) 0.0346(6) Uani d 1 H H2A -0.084339 1.224426 0.089129 0.052 Uiso calc 1 H H2B -0.180296 1.200042 0.155047 0.052 Uiso calc 1 H H2C -0.298274 1.183688 0.084114 0.052 Uiso calc 1 C C3 0.1555(4) 1.12327(14) 0.14890(12) 0.0297(5) Uani d 1 H H3A 0.231959 1.079690 0.145364 0.045 Uiso calc 1 H H3B 0.131237 1.131251 0.195216 0.045 Uiso calc 1 H H3C 0.234986 1.162156 0.133134 0.045 Uiso calc 1 C C4 -0.1897(4) 1.06314(13) 0.13413(11) 0.0243(5) Uani d 1 H H4A -0.215710 1.077966 0.179321 0.029 Uiso calc 1 H H4AB -0.322629 1.065052 0.106727 0.029 Uiso calc 1 C C5 -0.1231(4) 0.98678(13) 0.13820(11) 0.0206(4) Uani d 1 H H5 0.027068 0.984812 0.152253 0.025 Uiso calc 1 C C6 -0.2370(4) 0.94789(14) 0.18902(12) 0.0280(5) Uani d 1 H H6A -0.384013 0.947843 0.174889 0.042 Uiso calc 1 H H6B -0.212902 0.971097 0.232071 0.042 Uiso calc 1 H H6C -0.187189 0.899710 0.192790 0.042 Uiso calc 1 C C7 -0.1294(4) 0.87858(12) 0.06771(12) 0.0240(5) Uani d 1 H H7A -0.238405 0.853989 0.089144 0.029 Uiso calc 1 H H7AB 0.004589 0.865893 0.091186 0.029 Uiso calc 1 C C8 -0.1358(4) 0.85781(13) -0.00432(12) 0.0270(5) Uani d 1 H H8A -0.107160 0.807318 -0.008034 0.032 Uiso calc 1 H H8AB -0.273230 0.867329 -0.026998 0.032 Uiso calc 1 C C9 0.3590(3) 0.38600(12) 0.09872(11) 0.0206(4) Uani d 1 C C10 0.1558(4) 0.35671(15) 0.11853(13) 0.0303(5) Uani d 1 H H10A 0.060053 0.395164 0.123661 0.045 Uiso calc 1 H H10B 0.180228 0.331459 0.160515 0.045 Uiso calc 1 H H10C 0.097286 0.324785 0.084078 0.045 Uiso calc 1 C C11 0.5122(4) 0.32617(13) 0.09735(12) 0.0265(5) Uani d 1 H H11A 0.453000 0.288955 0.068458 0.040 Uiso calc 1 H H11B 0.543601 0.307893 0.142246 0.040 Uiso calc 1 H H11C 0.638195 0.343238 0.080461 0.040 Uiso calc 1 C C12 0.4309(3) 0.44094(12) 0.15058(11) 0.0213(4) Uani d 1 H H12A 0.320651 0.476148 0.151269 0.026 Uiso calc 1 H H12B 0.442905 0.417652 0.194316 0.026 Uiso calc 1 C C13 0.6305(3) 0.48006(12) 0.14432(11) 0.0201(4) Uani d 1 H H13 0.734764 0.446424 0.130329 0.024 Uiso calc 1 C C14 0.7096(4) 0.51152(14) 0.21111(12) 0.0288(5) Uani d 1 H H14A 0.841309 0.534543 0.207154 0.043 Uiso calc 1 H H14B 0.727466 0.474415 0.244372 0.043 Uiso calc 1 H H14C 0.610562 0.545765 0.224616 0.043 Uiso calc 1 C C15 0.7680(3) 0.58345(12) 0.08705(11) 0.0212(4) Uani d 1 H H15A 0.896328 0.556868 0.084148 0.025 Uiso calc 1 H H15B 0.785607 0.613909 0.126568 0.025 Uiso calc 1 C C16 0.7210(4) 0.62701(12) 0.02542(11) 0.0223(5) Uani d 1 H H16A 0.600184 0.656944 0.030186 0.027 Uiso calc 1 H H16B 0.838984 0.657466 0.018423 0.027 Uiso calc 1 N N1 -0.0211(3) 1.10117(10) 0.03540(9) 0.0197(4) Uani d 1 H H1 -0.139(3) 1.1114(15) 0.0134(13) 0.024 Uiso d 1 N N2 -0.1609(3) 0.95519(10) 0.07070(9) 0.0190(4) Uani d 1 H H2 -0.288(3) 0.9627(15) 0.0562(14) 0.023 Uiso d 1 N N3 0.3209(3) 0.42067(10) 0.03155(9) 0.0173(4) Uani d 1 H H3 0.209(3) 0.4443(13) 0.0335(14) 0.021 Uiso d 1 N N4 0.5940(3) 0.53475(10) 0.09237(9) 0.0177(4) Uani d 1 H H4 0.490(3) 0.5576(14) 0.1050(13) 0.021 Uiso d 1 Cl Cl1 0.30936(8) 0.97775(3) 0.06127(3) 0.02332(12) Uani d 1 Cl Cl2 0.21952(7) 0.56951(3) 0.00283(3) 0.02014(11) Uani d 1 Cl Cl3 0.69585(11) 0.74121(4) 0.20082(4) 0.04673(19) Uani d 1 Cl Cl4 0.24204(10) 0.63793(3) 0.18618(3) 0.03526(15) Uani d 1 Cl Cl5 0.21825(11) 0.82224(4) 0.22565(3) 0.03874(16) Uani d 1 Cl Cl6 0.32760(14) 0.76773(4) 0.06291(3) 0.0490(2) Uani d 1 Fe Fe1 0.000000 1.000000 0.000000 0.01496(11) Uani d 1 Fe Fe2 0.500000 0.500000 0.000000 0.01370(11) Uani d 1 Fe Fe3 0.36770(6) 0.74286(2) 0.16940(2) 0.02616(10) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0344(12) 0.0204(11) 0.0146(10) 0.0022(9) 0.0018(9) -0.0005(8) C2 0.0530(16) 0.0228(12) 0.0283(13) 0.0080(12) 0.0056(12) -0.0043(10) C3 0.0409(14) 0.0287(13) 0.0180(11) -0.0060(11) -0.0047(10) -0.0043(9) C4 0.0296(12) 0.0266(12) 0.0174(10) 0.0034(10) 0.0063(9) -0.0015(9) C5 0.0239(11) 0.0277(12) 0.0108(10) -0.0008(9) 0.0047(8) 0.0011(8) C6 0.0313(13) 0.0356(14) 0.0184(11) -0.0014(10) 0.0089(9) 0.0056(10) C7 0.0313(12) 0.0203(11) 0.0212(11) -0.0023(9) 0.0067(9) 0.0041(9) C8 0.0381(13) 0.0198(11) 0.0238(12) -0.0056(10) 0.0062(10) 0.0003(9) C9 0.0213(10) 0.0222(11) 0.0184(10) 0.0005(9) 0.0025(8) 0.0027(9) C10 0.0259(12) 0.0367(14) 0.0287(13) -0.0046(10) 0.0046(10) 0.0078(11) C11 0.0288(12) 0.0243(12) 0.0254(12) 0.0061(10) -0.0021(9) 0.0045(10) C12 0.0228(11) 0.0261(12) 0.0153(10) 0.0044(9) 0.0043(8) 0.0019(9) C13 0.0210(10) 0.0251(11) 0.0138(10) 0.0031(9) -0.0007(8) 0.0006(8) C14 0.0345(13) 0.0357(14) 0.0149(11) -0.0001(11) -0.0038(9) -0.0021(10) C15 0.0202(10) 0.0251(11) 0.0179(10) -0.0042(9) -0.0003(8) -0.0060(9) C16 0.0238(11) 0.0214(11) 0.0213(11) -0.0031(9) 0.0002(9) -0.0034(9) N1 0.0242(9) 0.0196(9) 0.0152(9) -0.0020(7) 0.0015(7) -0.0014(7) N2 0.0217(9) 0.0208(9) 0.0142(8) 0.0013(7) 0.0009(7) 0.0010(7) N3 0.0171(8) 0.0190(9) 0.0157(8) 0.0023(7) 0.0010(7) -0.0007(7) N4 0.0155(8) 0.0233(9) 0.0143(8) 0.0010(7) 0.0019(7) -0.0018(7) Cl1 0.0195(2) 0.0293(3) 0.0212(3) -0.0001(2) 0.00196(19) 0.0017(2) Cl2 0.0168(2) 0.0231(3) 0.0207(2) 0.00348(19) 0.00231(18) -0.00202(19) Cl3 0.0322(3) 0.0408(4) 0.0658(5) -0.0008(3) -0.0029(3) 0.0069(3) Cl4 0.0390(3) 0.0292(3) 0.0374(3) -0.0048(3) 0.0027(3) -0.0016(3) Cl5 0.0463(4) 0.0376(4) 0.0310(3) 0.0097(3) -0.0030(3) -0.0129(3) Cl6 0.0767(5) 0.0465(4) 0.0243(3) 0.0307(4) 0.0080(3) 0.0056(3) Fe1 0.0176(2) 0.0156(2) 0.0120(2) -0.00026(17) 0.00293(17) 0.00091(17) Fe2 0.0128(2) 0.0169(2) 0.0114(2) 0.00094(17) 0.00103(16) -0.00157(16) Fe3 0.0322(2) 0.0237(2) 0.0223(2) 0.00353(15) 0.00095(15) 0.00045(14) 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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 C1 C3 . . 111.7(2) ? N1 C1 C2 . . 108.51(19) ? C3 C1 C2 . . 109.5(2) ? N1 C1 C4 . . 109.19(18) ? C3 C1 C4 . . 111.62(19) ? C2 C1 C4 . . 106.1(2) ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 C3 H3A . . 109.5 ? C1 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C1 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C5 C4 C1 . . 119.9(2) ? C5 C4 H4A . . 107.3 ? C1 C4 H4A . . 107.3 ? C5 C4 H4AB . . 107.3 ? C1 C4 H4AB . . 107.3 ? H4A C4 H4AB . . 106.9 ? N2 C5 C6 . . 111.8(2) ? N2 C5 C4 . . 108.42(18) ? C6 C5 C4 . . 110.5(2) ? N2 C5 H5 . . 108.7 ? C6 C5 H5 . . 108.7 ? C4 C5 H5 . . 108.7 ? C5 C6 H6A . . 109.5 ? C5 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C5 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? N2 C7 C8 . . 107.97(18) ? N2 C7 H7A . . 110.1 ? C8 C7 H7A . . 110.1 ? N2 C7 H7AB . . 110.1 ? C8 C7 H7AB . . 110.1 ? H7A C7 H7AB . . 108.4 ? N1 C8 C7 3_575 . 108.32(19) ? N1 C8 H8A 3_575 . 110.0 ? C7 C8 H8A . . 110.0 ? N1 C8 H8AB 3_575 . 110.0 ? C7 C8 H8AB . . 110.0 ? H8A C8 H8AB . . 108.4 ? N3 C9 C11 . . 111.50(19) ? N3 C9 C12 . . 109.32(18) ? C11 C9 C12 . . 111.59(19) ? N3 C9 C10 . . 108.78(18) ? C11 C9 C10 . . 108.6(2) ? C12 C9 C10 . . 106.90(19) ? C9 C10 H10A . . 109.5 ? C9 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C9 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C9 C11 H11A . . 109.5 ? C9 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C9 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C13 C12 C9 . . 119.51(19) ? C13 C12 H12A . . 107.4 ? C9 C12 H12A . . 107.4 ? C13 C12 H12B . . 107.4 ? C9 C12 H12B . . 107.4 ? H12A C12 H12B . . 107.0 ? N4 C13 C12 . . 108.82(17) ? N4 C13 C14 . . 111.64(19) ? C12 C13 C14 . . 110.04(19) ? N4 C13 H13 . . 108.8 ? C12 C13 H13 . . 108.8 ? C14 C13 H13 . . 108.8 ? C13 C14 H14A . . 109.5 ? C13 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C13 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? N4 C15 C16 . . 107.96(17) ? N4 C15 H15A . . 110.1 ? C16 C15 H15A . . 110.1 ? N4 C15 H15B . . 110.1 ? C16 C15 H15B . . 110.1 ? H15A C15 H15B . . 108.4 ? N3 C16 C15 3_665 . 108.31(18) ? N3 C16 H16A 3_665 . 110.0 ? C15 C16 H16A . . 110.0 ? N3 C16 H16B 3_665 . 110.0 ? C15 C16 H16B . . 110.0 ? H16A C16 H16B . . 108.4 ? C8 N1 C1 3_575 . 116.44(18) ? C8 N1 Fe1 3_575 . 106.08(14) ? C1 N1 Fe1 . . 123.35(14) ? C8 N1 H1 3_575 . 106.2(19) ? C1 N1 H1 . . 104.9(19) ? Fe1 N1 H1 . . 96.7(19) ? C7 N2 C5 . . 115.19(18) ? C7 N2 Fe1 . . 107.65(14) ? C5 N2 Fe1 . . 114.80(14) ? C7 N2 H2 . . 106.4(19) ? C5 N2 H2 . . 108.2(19) ? Fe1 N2 H2 . . 103.6(19) ? C16 N3 C9 3_665 . 115.78(18) ? C16 N3 Fe2 3_665 . 106.42(14) ? C9 N3 Fe2 . . 123.52(13) ? C16 N3 H3 3_665 . 105.3(18) ? C9 N3 H3 . . 104.9(19) ? Fe2 N3 H3 . . 97.9(18) ? C15 N4 C13 . . 114.79(17) ? C15 N4 Fe2 . . 107.94(13) ? C13 N4 Fe2 . . 115.95(14) ? C15 N4 H4 . . 109.5(18) ? C13 N4 H4 . . 103.0(19) ? Fe2 N4 H4 . . 105.0(18) ? N2 Fe1 N2 3_575 . 180.0 ? N2 Fe1 N1 3_575 3_575 95.39(8) ? N2 Fe1 N1 . 3_575 84.61(8) y N2 Fe1 N1 3_575 . 84.61(8) ? N2 Fe1 N1 . . 95.39(8) y N1 Fe1 N1 3_575 . 180.0 ? N2 Fe1 Cl1 3_575 . 88.32(5) ? N2 Fe1 Cl1 . . 91.68(5) y N1 Fe1 Cl1 3_575 . 86.02(5) ? N1 Fe1 Cl1 . . 93.98(5) y N2 Fe1 Cl1 3_575 3_575 91.68(5) ? N2 Fe1 Cl1 . 3_575 88.32(5) y N1 Fe1 Cl1 3_575 3_575 93.98(5) ? N1 Fe1 Cl1 . 3_575 86.02(5) y Cl1 Fe1 Cl1 . 3_575 180.0 ? N4 Fe2 N4 . 3_665 180.0 ? N4 Fe2 N3 . . 95.04(7) y N4 Fe2 N3 3_665 . 84.97(7) ? N4 Fe2 N3 . 3_665 84.96(7) y N4 Fe2 N3 3_665 3_665 95.03(7) ? N3 Fe2 N3 . 3_665 180.0 ? N4 Fe2 Cl2 . . 87.76(5) y N4 Fe2 Cl2 3_665 . 92.23(5) ? N3 Fe2 Cl2 . . 86.49(5) y N3 Fe2 Cl2 3_665 . 93.51(5) ? N4 Fe2 Cl2 . 3_665 92.23(5) y N4 Fe2 Cl2 3_665 3_665 87.77(5) ? N3 Fe2 Cl2 . 3_665 93.51(5) y N3 Fe2 Cl2 3_665 3_665 86.49(5) ? Cl2 Fe2 Cl2 . 3_665 180.0 ? Cl3 Fe3 Cl5 . . 109.53(3) y Cl3 Fe3 Cl6 . . 108.24(4) y Cl5 Fe3 Cl6 . . 110.05(3) y Cl3 Fe3 Cl4 . . 108.22(3) y Cl5 Fe3 Cl4 . . 111.14(3) y Cl6 Fe3 Cl4 . . 109.60(3) y 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 C1 N1 . 1.514(3) ? C1 C3 . 1.525(3) ? C1 C2 . 1.535(3) ? C1 C4 . 1.536(3) ? C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C2 H2C . 0.9800 ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? C4 C5 . 1.527(3) ? C4 H4A . 0.9900 ? C4 H4AB . 0.9900 ? C5 N2 . 1.497(3) ? C5 C6 . 1.523(3) ? C5 H5 . 1.0000 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C7 N2 . 1.485(3) ? C7 C8 . 1.512(3) ? C7 H7A . 0.9900 ? C7 H7AB . 0.9900 ? C8 N1 3_575 1.481(3) ? C8 H8A . 0.9900 ? C8 H8AB . 0.9900 ? C9 N3 . 1.516(3) ? C9 C11 . 1.526(3) ? C9 C12 . 1.532(3) ? C9 C10 . 1.534(3) ? C10 H10A . 0.9800 ? C10 H10B . 0.9800 ? C10 H10C . 0.9800 ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 C13 . 1.524(3) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 N4 . 1.490(3) ? C13 C14 . 1.529(3) ? C13 H13 . 1.0000 ? C14 H14A . 0.9800 ? C14 H14B . 0.9800 ? C14 H14C . 0.9800 ? C15 N4 . 1.486(3) ? C15 C16 . 1.512(3) ? C15 H15A . 0.9900 ? C15 H15B . 0.9900 ? C16 N3 3_665 1.479(3) ? C16 H16A . 0.9900 ? C16 H16B . 0.9900 ? Fe1 N1 . 2.0768(19) y N1 H1 . 0.880(19) ? Fe1 N2 . 2.0477(19) y N2 H2 . 0.872(19) ? Fe2 N3 . 2.0595(19) y N3 H3 . 0.864(19) ? Fe2 N4 . 2.0301(18) y N4 H4 . 0.869(19) ? Fe1 Cl1 . 2.3177(5) y Fe2 Cl2 . 2.2760(5) y Fe3 Cl3 . 2.1866(8) y Fe3 Cl4 . 2.2117(8) y Fe3 Cl5 . 2.1879(7) y Fe3 Cl6 . 2.2048(8) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 Cl6 3_575 0.880(19) 2.99(2) 3.686(2) 138(2) yes N2 H2 Cl1 1_455 0.872(19) 2.66(2) 3.487(2) 158(2) yes N3 H3 Cl2 3_565 0.864(19) 2.85(2) 3.5519(19) 139(2) yes N4 H4 Cl4 . 0.869(19) 2.87(2) 3.699(2) 160(2) 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_4 _geom_torsion N1 C1 C4 C5 . 62.5(3) C3 C1 C4 C5 . -61.5(3) C2 C1 C4 C5 . 179.3(2) C1 C4 C5 N2 . -79.0(2) C1 C4 C5 C6 . 158.1(2) N2 C7 C8 N1 3_575 56.4(3) N3 C9 C12 C13 . -62.2(3) C11 C9 C12 C13 . 61.6(3) C10 C9 C12 C13 . -179.8(2) C9 C12 C13 N4 . 77.3(2) C9 C12 C13 C14 . -160.0(2) N4 C15 C16 N3 3_665 -55.2(2) C3 C1 N1 C8 3_575 -46.7(3) C2 C1 N1 C8 3_575 74.1(3) C4 C1 N1 C8 3_575 -170.6(2) C3 C1 N1 Fe1 . 87.5(2) C2 C1 N1 Fe1 . -151.62(17) C4 C1 N1 Fe1 . -36.4(2) C8 C7 N2 C5 . -169.80(19) C8 C7 N2 Fe1 . -40.3(2) C6 C5 N2 C7 . -50.4(3) C4 C5 N2 C7 . -172.44(19) C6 C5 N2 Fe1 . -176.30(15) C4 C5 N2 Fe1 . 61.7(2) C11 C9 N3 C16 3_665 47.7(3) C12 C9 N3 C16 3_665 171.61(18) C10 C9 N3 C16 3_665 -72.0(2) C11 C9 N3 Fe2 . -86.4(2) C12 C9 N3 Fe2 . 37.5(2) C10 C9 N3 Fe2 . 153.86(16) C16 C15 N4 C13 . 170.47(18) C16 C15 N4 Fe2 . 39.5(2) C12 C13 N4 C15 . 172.13(18) C14 C13 N4 C15 . 50.5(3) C12 C13 N4 Fe2 . -60.9(2) C14 C13 N4 Fe2 . 177.49(15) _cod_database_fobs_code 2021796