#------------------------------------------------------------------------------ #$Date: 2019-12-12 11:52:55 +0200 (Thu, 12 Dec 2019) $ #$Revision: 245009 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556521.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556521 loop_ _publ_author_name 'Takahashi, K.' 'Sakurai, T.' 'Zhang, W.-M.' 'Okubo, S.' 'Ohta, H.' 'Yamamoto, T.' 'Einaga, Y.' 'Mori, H.' _publ_section_title ; Spin-Singlet Transition in the Magnetic Hybrid Compound from a Spin-Crossover Fe(III) Cation and pi-Radical Anion ; _journal_name_full Inorganics _journal_page_first 54 _journal_paper_doi 10.3390/inorganics5030054 _journal_volume 5 _journal_year 2017 _chemical_formula_moiety 'C32 H22 Fe N4 O2, C8 N4 Ni S4' _chemical_formula_sum 'C40 H22 Fe N8 Ni O2 S4' _chemical_formula_weight 889.45 _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 65.962(11) _cell_angle_beta 85.184(14) _cell_angle_gamma 65.815(9) _cell_formula_units_Z 2 _cell_length_a 11.7638(6) _cell_length_b 13.5893(5) _cell_length_c 14.1000(10) _cell_measurement_reflns_used 7103 _cell_measurement_temperature 293 _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 3.06 _cell_volume 1868.6(3) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.2.4' _computing_publication_material 'CrystalStructure 4.2.4 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL Version 2016/6 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 7.314 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 20124 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.241 _diffrn_reflns_theta_max 27.567 _diffrn_reflns_theta_min 3.049 _diffrn_standards_interval_count . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 904.00 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.90 _refine_diff_density_min -0.66 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 505 _refine_ls_number_reflns 8382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0468 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0757P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1228 _refine_ls_wR_factor_ref 0.1427 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6421 _reflns_number_total 8382 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file 293K.cif _cod_data_source_block Feqsal_Nimnt_293K _cod_original_cell_volume 1868.5(3) _cod_database_code 1556521 _shelx_res_file ; TITL _Ni(mnt)2_20120312 shelxl.res created by SHELXL-2016/6 at 18:29:13 on 12-Jun-2017 CELL 0.71070 11.76380 13.58930 14.10000 65.96170 85.18380 65.81470 ZERR 2 0.00060 0.00000 0.00100 0.01050 0.01400 0.00940 LATT 1 SFAC C H N O FE NI S UNIT 80 44 16 4 2 2 8 L.S. 20 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 20.0 ACTA SIZE 0.200 0.200 0.050 WGHT 0.084500 0.075700 FVAR 1.68837 NI1 6 0.180374 0.934207 -0.028371 11.00000 0.04458 0.04753 = 0.04352 -0.02062 0.00407 -0.02091 FE1 5 0.409370 0.429259 0.327840 11.00000 0.05917 0.04510 = 0.03813 -0.01557 0.00048 -0.02898 S1 7 0.088724 0.930796 -0.151664 11.00000 0.05749 0.06240 = 0.04616 -0.02193 0.00081 -0.02969 S2 7 0.124614 0.807400 0.089515 11.00000 0.05370 0.05410 = 0.04599 -0.02061 0.00472 -0.02709 S3 7 0.231104 1.065099 -0.145319 11.00000 0.06001 0.06815 = 0.04256 -0.01875 0.00452 -0.03750 S4 7 0.269952 0.938854 0.094930 11.00000 0.06287 0.05752 = 0.04328 -0.01936 0.00186 -0.03137 O1 4 0.372178 0.326607 0.455997 11.00000 0.09181 0.05459 = 0.03683 -0.01587 0.00389 -0.04257 O2 4 0.580376 0.322080 0.341772 11.00000 0.06909 0.05800 = 0.06438 -0.02085 -0.00404 -0.01795 N1 3 0.325596 0.369696 0.249808 11.00000 0.05759 0.04802 = 0.03710 -0.01805 0.00327 -0.02987 N2 3 0.409189 0.536043 0.161757 11.00000 0.05104 0.04330 = 0.03906 -0.01713 0.00688 -0.02442 N3 3 0.473930 0.537348 0.362707 11.00000 0.06282 0.05443 = 0.03679 -0.01594 0.00067 -0.03692 N4 3 0.240441 0.566372 0.337267 11.00000 0.05935 0.05342 = 0.04345 -0.01971 0.00440 -0.02984 N5 3 -0.116355 0.803882 -0.193877 11.00000 0.08149 0.11698 = 0.07728 -0.05389 0.01462 -0.06054 N6 3 -0.049982 0.625894 0.124892 11.00000 0.08802 0.08180 = 0.08353 -0.03510 0.01448 -0.05376 N7 3 0.385335 1.261253 -0.183942 11.00000 0.10540 0.10278 = 0.07778 -0.02181 0.01165 -0.07633 N8 3 0.431819 1.100517 0.142041 11.00000 0.07788 0.09855 = 0.07765 -0.04884 0.00616 -0.04838 C1 1 0.358930 0.228374 0.479972 11.00000 0.06886 0.04514 = 0.04215 -0.01601 0.00765 -0.03351 C2 1 0.368599 0.151522 0.584333 11.00000 0.10194 0.06183 = 0.04272 -0.01885 0.01069 -0.04805 AFIX 43 H1 2 0.380902 0.172416 0.636525 11.00000 -1.20000 AFIX 0 C3 1 0.360354 0.046273 0.611320 11.00000 0.12636 0.06399 = 0.04901 -0.01126 0.01181 -0.05700 AFIX 43 H2 2 0.369390 -0.004326 0.681409 11.00000 -1.20000 AFIX 0 C4 1 0.338663 0.013903 0.535468 11.00000 0.14594 0.06229 = 0.06099 -0.01550 0.00958 -0.06913 AFIX 43 H3 2 0.334628 -0.058571 0.554549 11.00000 -1.20000 AFIX 0 C5 1 0.323358 0.088578 0.433237 11.00000 0.12987 0.05898 = 0.05519 -0.02046 0.00497 -0.05805 AFIX 43 H4 2 0.306061 0.067894 0.382601 11.00000 -1.20000 AFIX 0 C6 1 0.333308 0.197085 0.402689 11.00000 0.07775 0.04926 = 0.04483 -0.01781 0.00437 -0.03614 C7 1 0.315806 0.269067 0.293777 11.00000 0.07223 0.05048 = 0.04430 -0.01954 0.00185 -0.03633 AFIX 43 H5 2 0.295461 0.241684 0.249855 11.00000 -1.20000 AFIX 0 C8 1 0.296904 0.435014 0.140188 11.00000 0.05486 0.04555 = 0.03889 -0.01744 0.00447 -0.02247 C9 1 0.226686 0.420799 0.076775 11.00000 0.07348 0.06081 = 0.04730 -0.02220 -0.00053 -0.03732 AFIX 43 H6 2 0.191577 0.366138 0.105669 11.00000 -1.20000 AFIX 0 C10 1 0.208750 0.488724 -0.030613 11.00000 0.07417 0.06901 = 0.04908 -0.02626 -0.00886 -0.03071 AFIX 43 H7 2 0.160728 0.479302 -0.072687 11.00000 -1.20000 AFIX 0 C11 1 0.259910 0.568286 -0.074999 11.00000 0.06811 0.05788 = 0.03557 -0.01702 -0.00101 -0.02013 AFIX 43 H8 2 0.248947 0.610591 -0.147061 11.00000 -1.20000 AFIX 0 C12 1 0.329436 0.587308 -0.012861 11.00000 0.05028 0.04544 = 0.03906 -0.01789 0.00745 -0.01487 C13 1 0.346057 0.521151 0.095698 11.00000 0.04801 0.04301 = 0.03639 -0.01752 0.00620 -0.01846 C14 1 0.386074 0.667135 -0.052930 11.00000 0.05736 0.04627 = 0.04376 -0.01298 0.01107 -0.01768 AFIX 43 H9 2 0.379006 0.711178 -0.124508 11.00000 -1.20000 AFIX 0 C15 1 0.451365 0.679930 0.013222 11.00000 0.05792 0.04593 = 0.05048 -0.01610 0.01581 -0.02446 AFIX 43 H10 2 0.489779 0.732148 -0.012566 11.00000 -1.20000 AFIX 0 C16 1 0.459823 0.613187 0.120834 11.00000 0.05190 0.04645 = 0.04891 -0.01814 0.00513 -0.02498 AFIX 43 H11 2 0.503133 0.623677 0.165589 11.00000 -1.20000 AFIX 0 C17 1 0.687511 0.325238 0.353574 11.00000 0.06757 0.07707 = 0.03947 -0.00617 0.00532 -0.02379 C18 1 0.799006 0.231506 0.351624 11.00000 0.07110 0.09853 = 0.04717 -0.01192 0.00886 -0.00724 AFIX 43 H12 2 0.794752 0.169212 0.342153 11.00000 -1.20000 AFIX 0 C19 1 0.913014 0.231648 0.363539 11.00000 0.08025 0.14346 = 0.06008 -0.01403 0.01705 -0.01907 AFIX 43 H13 2 0.985847 0.168320 0.364270 11.00000 -1.20000 AFIX 0 C20 1 0.920781 0.325327 0.374514 11.00000 0.05653 0.18073 = 0.08884 -0.01960 0.01575 -0.04323 AFIX 43 H14 2 0.998939 0.325685 0.379448 11.00000 -1.20000 AFIX 0 C21 1 0.816965 0.416553 0.378228 11.00000 0.07336 0.13455 = 0.07516 -0.01363 0.00628 -0.05645 AFIX 43 H15 2 0.824048 0.477954 0.387276 11.00000 -1.20000 AFIX 0 C22 1 0.696499 0.417880 0.368159 11.00000 0.05788 0.08250 = 0.04510 -0.00640 0.00267 -0.03371 C23 1 0.591524 0.515476 0.374673 11.00000 0.07640 0.07038 = 0.04503 -0.01160 0.00071 -0.05052 AFIX 43 H16 2 0.608925 0.569192 0.388989 11.00000 -1.20000 AFIX 0 C24 1 0.379275 0.641840 0.365421 11.00000 0.07891 0.04939 = 0.03486 -0.01515 0.00106 -0.03576 C25 1 0.395987 0.729061 0.378801 11.00000 0.11462 0.06465 = 0.05092 -0.02466 0.00170 -0.05441 AFIX 43 H17 2 0.476554 0.723636 0.385537 11.00000 -1.20000 AFIX 0 C26 1 0.293855 0.825919 0.382468 11.00000 0.14370 0.05481 = 0.05772 -0.02337 -0.00523 -0.04499 AFIX 43 H18 2 0.307664 0.884530 0.391177 11.00000 -1.20000 AFIX 0 C27 1 0.174784 0.837631 0.373750 11.00000 0.13210 0.05285 = 0.04921 -0.02458 0.00138 -0.02044 AFIX 43 H19 2 0.108230 0.903300 0.376859 11.00000 -1.20000 AFIX 0 C28 1 0.151931 0.749920 0.359931 11.00000 0.08846 0.05576 = 0.03799 -0.01814 -0.00141 -0.02075 C29 1 0.253704 0.654013 0.353377 11.00000 0.07140 0.04412 = 0.03388 -0.01507 0.00049 -0.02430 C30 1 0.032250 0.752312 0.353127 11.00000 0.07235 0.08054 = 0.05568 -0.02883 0.00287 -0.00883 AFIX 43 H20 2 -0.038256 0.814211 0.357878 11.00000 -1.20000 AFIX 0 C31 1 0.020422 0.663185 0.339515 11.00000 0.06017 0.09665 = 0.06756 -0.03049 0.00526 -0.02734 AFIX 43 H21 2 -0.058250 0.663483 0.335607 11.00000 -1.20000 AFIX 0 C32 1 0.126296 0.571879 0.331498 11.00000 0.06071 0.07272 = 0.06251 -0.02453 0.00279 -0.03395 AFIX 43 H22 2 0.116463 0.512070 0.321651 11.00000 -1.20000 AFIX 0 C33 1 -0.054559 0.816631 -0.146082 11.00000 0.05529 0.07363 = 0.05759 -0.03282 0.00889 -0.03236 C34 1 -0.011938 0.694295 0.077264 11.00000 0.05516 0.06075 = 0.06450 -0.03214 0.00620 -0.02940 C35 1 0.021632 0.833960 -0.085670 11.00000 0.04355 0.05767 = 0.05976 -0.03029 0.00385 -0.02180 C36 1 0.039161 0.778698 0.019398 11.00000 0.04172 0.04739 = 0.06264 -0.02621 0.00530 -0.01808 C37 1 0.308084 1.101069 -0.075225 11.00000 0.04646 0.05684 = 0.05226 -0.02284 0.00661 -0.02656 C38 1 0.325069 1.045935 0.030566 11.00000 0.04448 0.05437 = 0.05410 -0.02515 0.00374 -0.02287 C39 1 0.351898 1.190324 -0.133729 11.00000 0.06397 0.07356 = 0.05777 -0.02363 0.00503 -0.03963 C40 1 0.385030 1.076576 0.091782 11.00000 0.05389 0.06847 = 0.05625 -0.03203 0.00843 -0.02754 HKLF 4 REM _Ni(mnt)2_20120312 REM R1 = 0.0468 for 6421 Fo > 4sig(Fo) and 0.0600 for all 8382 data REM 505 parameters refined using 0 restraints END WGHT 0.0842 0.0783 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z HTAB C7 N5_$1 HTAB C9 N5_$1 HTAB C16 N3 EQIV $2 -x+1, -y+2, -z HTAB C16 N7_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C25 O1_$3 REM Highest difference peak 0.902, deepest hole -0.658, 1-sigma level 0.069 Q1 1 0.7694 0.3025 0.2705 11.00000 0.05 0.67 Q2 1 0.5031 0.4352 0.4529 11.00000 0.05 0.61 Q3 1 0.0540 0.5552 0.3899 11.00000 0.05 0.57 Q4 1 0.3194 0.4199 0.2038 11.00000 0.05 0.56 Q5 1 0.4625 0.5615 0.2106 11.00000 0.05 0.54 Q6 1 0.3591 0.2972 0.4481 11.00000 0.05 0.46 Q7 1 0.3209 1.0625 -0.0189 11.00000 0.05 0.44 Q8 1 0.5346 0.8056 -0.0861 11.00000 0.05 0.37 Q9 1 0.2180 0.8109 0.2127 11.00000 0.05 0.37 Q10 1 0.2417 0.5812 -0.0988 11.00000 0.05 0.36 Q11 1 0.2419 0.9609 0.0234 11.00000 0.05 0.35 Q12 1 0.3471 0.4052 0.2814 11.00000 0.05 0.35 Q13 1 0.3655 0.0747 0.3179 11.00000 0.05 0.35 Q14 1 -0.1408 0.9392 0.2651 11.00000 0.05 0.33 Q15 1 0.0355 0.8068 -0.0362 11.00000 0.05 0.33 Q16 1 0.1217 0.9151 -0.0772 11.00000 0.05 0.32 Q17 1 0.3011 0.5821 -0.0291 11.00000 0.05 0.32 Q18 1 0.3423 1.0640 0.0438 11.00000 0.05 0.32 Q19 1 0.3335 0.5487 0.0370 11.00000 0.05 0.32 Q20 1 0.7203 0.1628 0.3934 11.00000 0.05 0.30 Q21 1 0.0747 0.6716 0.2073 11.00000 0.05 0.30 Q22 1 0.7835 0.4955 0.3960 11.00000 0.05 0.29 Q23 1 0.4728 0.6696 0.0357 11.00000 0.05 0.29 Q24 1 0.4033 0.5117 0.2205 11.00000 0.05 0.29 Q25 1 0.0640 0.7722 0.0371 11.00000 0.05 0.28 ; _shelx_res_checksum 32508 _shelx_hkl_file ; 1 -1 -1 1064.81 18.41 -1 -2 -1 150.14 10.33 -1 -2 -1 165.53 9.37 0 0 -216662.46 150.51 -1 -1 -2 221.63 8.04 -1 -1 -2 252.69 14.29 -1 -2 023707.14 213.12 -1 -2 023018.07 223.29 -1 -2 -2 2040.21 46.22 -1 -2 -2 1964.10 37.48 0 -2 0 6257.49 113.51 0 -2 0 6274.51 115.50 -2 -1 -113633.09 132.70 0 -2 -2 1149.57 28.43 0 -2 -2 1118.94 23.58 -1 1 225208.71 224.76 1 -1 -225933.90 232.42 2 0 019406.02 171.91 -2 0 018599.68 164.56 1 0 2 7457.78 132.41 1 0 2 7382.04 133.76 1 -1 110091.55 103.52 1 -1 110293.86 96.25 -2 -2 -1 297.62 34.11 2 2 1 246.45 15.74 -2 -2 -1 246.87 17.07 2 2 1 259.85 10.42 -2 -1 1 833.40 38.95 2 1 -1 760.63 27.19 -2 -1 1 754.91 21.79 2 1 -1 763.41 21.34 -2 0 127324.67 242.47 2 0 -126946.63 238.34 -2 0 126747.30 237.03 2 0 -127034.14 240.32 -2 -2 0 206.39 47.48 2 2 0 169.36 54.29 -2 -2 0 208.70 45.98 -2 -2 0 187.29 55.75 1 2 -131660.32 301.69 -1 -2 132176.76 289.67 -1 -1 2 2194.10 55.90 1 1 -2 2074.84 51.54 0 1 -210135.84 114.63 0 -1 210249.00 107.63 0 -1 2 9935.88 112.59 0 -1 210213.52 108.57 2 0 1 1761.17 37.27 2 0 1 1834.77 35.51 -2 0 -1 1840.06 39.01 0 1 317172.34 169.76 0 -1 -316920.40 160.70 0 -1 -317268.22 171.65 0 1 316944.71 164.38 -2 -2 -2 2562.08 43.73 2 2 2 2552.54 51.13 -2 -2 -2 2567.25 51.06 1 -2 -131217.62 279.30 -1 2 131193.00 278.96 1 -2 -131525.21 267.59 -2 -1 -2 2093.39 48.80 2 1 2 2151.63 35.94 2 1 2 2043.24 42.91 0 2 -1 8428.75 96.85 0 -2 1 8523.39 95.00 0 -2 1 8769.48 99.98 0 2 -1 8657.77 98.84 -1 -3 -114345.08 147.95 -1 -3 -113748.62 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1937.79 89.85 6 11 11 1896.57 77.25 0 7 -7 28.13 14.85 3 12 0 149.17 50.21 7 10 11 32.88 12.82 0 -7 7 20.44 15.29 0 -7 7 20.05 12.37 7 10 11 46.36 17.81 -7 -10 -11 14.02 8.75 -3 -12 0 110.70 46.04 3 12 0 197.85 34.04 -2 11 6 93.47 31.91 -2 11 6 113.63 24.28 -5 7 -2 368.18 81.60 -2 11 6 106.75 31.28 11 8 0 60.62 22.34 11 4 -3 39.95 16.78 -11 -4 3 14.65 8.51 -1 1 13 399.57 90.82 -7 6 1 164.24 41.97 -11 -8 0 56.72 16.92 1 -1 -13 373.64 98.19 -11 -8 0 74.63 21.09 11 4 -3 13.38 9.89 0 -4 10 231.59 56.42 0 4 -10 221.57 51.46 -8 1 9 621.03 49.93 8 -1 -9 653.77 106.10 6 -5 4 495.01 99.51 -6 5 -4 610.66 122.65 6 -5 4 651.20 15.40 -3 -10 4 1913.91 96.21 3 10 -4 1948.40 166.77 -3 3 13 76.55 28.54 3 -3 -13 113.44 27.42 -5 8 8 126.61 29.32 -5 8 8 139.79 27.17 -5 8 8 92.68 33.28 -6 3 11 1409.83 172.30 8 11 -1 -9.95 20.34 6 -3 -11 1284.59 144.46 7 4 11 236.47 43.29 7 4 11 296.15 75.46 7 2 10 479.31 31.18 7 2 10 483.89 48.78 7 4 11 253.10 40.61 -8 -11 1 9.02 13.28 7 2 10 496.46 36.37 8 -4 -7 624.56 41.85 -3 -3 11 4.86 9.85 0 1 13 13.50 11.91 -8 4 7 686.99 59.38 -8 4 7 670.12 35.39 3 3 -11 2.59 12.90 0 1 13 6.39 16.70 -5 -2 11 617.55 131.27 -3 4 13 685.16 54.39 5 2 -11 673.31 148.05 -3 4 13 644.41 65.50 11 3 -3 109.02 37.90 -11 -3 3 65.08 26.58 11 3 -3 69.16 21.46 -11 -3 3 101.42 21.02 7 13 5 743.79 78.61 6 13 3 1977.44 97.09 7 13 5 825.72 173.69 -7 -13 -5 863.06 44.95 6 13 3 1930.71 215.58 -9 3 0 39.88 16.60 -8 5 3 970.59 58.48 9 -3 0 18.98 9.86 -7 5 -2 597.91 119.23 7 -5 2 682.57 49.50 11 8 5 1013.16 96.75 1 3 -11 60.92 25.46 8 4 10 78.95 29.61 -1 -3 11 69.50 26.98 -6 -12 -10 2004.42 82.30 6 12 10 2014.07 115.63 1 9 13 804.76 55.54 6 12 10 2003.57 85.48 1 9 13 782.81 83.87 4 4 13 291.92 44.77 -4 -4 -13 256.60 43.60 4 4 13 318.05 68.24 -9 3 5 233.33 52.62 9 -3 -5 186.39 54.69 -9 3 5 201.00 35.23 -2 10 10 341.95 34.94 -9 -6 6 2184.15 168.39 -2 10 10 309.38 87.67 -2 10 10 245.63 77.06 9 6 -6 1965.20 111.34 -3 10 8 787.82 120.56 -11 -9 -3 136.05 42.37 11 9 3 168.60 66.42 -3 10 8 648.34 76.37 -11 -9 -3 147.46 43.15 -8 5 4 426.57 108.18 -3 10 8 727.11 38.63 5 -6 4 575.19 23.78 -7 -13 -6 708.63 44.71 5 -6 4 536.82 25.60 7 13 6 690.43 60.65 -5 6 -4 627.92 67.23 7 13 6 744.58 40.63 -2 11 4 38.11 21.09 7 4 -9 -3.27 25.81 8 -2 5 80.79 23.10 2 -11 -4 11.49 8.32 -8 2 -5 109.69 28.22 -7 -4 9 36.41 18.17 -2 11 4 4.30 4.81 8 -2 5 95.36 25.99 8 -2 5 89.36 25.98 -3 10 2 16.77 18.95 -4 9 1 1184.46 81.54 8 6 -7 12.89 20.63 -10 1 4 8.69 5.54 -8 -6 7 42.24 17.05 10 -1 -4 4.52 5.69 -10 1 4 1.32 6.66 4 9 13 36.62 23.16 -10 -4 -7 88.05 31.78 3 13 8 5145.93 203.01 10 4 7 96.31 32.16 4 9 13 48.39 21.99 -4 -9 -13 24.04 17.48 3 13 8 4933.04 242.69 8 12 8 111.99 26.59 10 7 8 1157.84 56.09 -8 -12 -8 86.93 34.58 -5 -4 10 256.26 53.05 8 12 8 128.90 34.40 5 4 -10 285.42 52.94 -5 -7 -13 126.86 40.40 5 7 13 128.14 40.48 11 5 5 121.13 40.44 -10 -2 6 40.51 28.37 10 2 -6 29.96 18.12 5 7 13 169.56 44.75 0 12 8 2.36 6.96 11 5 -3 5.44 11.26 0 12 8 -7.21 18.08 5 -2 -12 560.93 57.51 11 5 -3 3.08 10.15 0 -12 -8 -2.13 12.36 -5 2 12 628.82 66.25 -11 -9 -2 148.33 36.44 11 9 2 139.20 36.40 -11 -9 -2 119.59 44.46 -11 -5 3 6.67 12.23 1 -11 -1 263.42 56.52 -1 11 1 296.26 71.96 -1 11 1 257.21 76.04 6 2 11 195.84 36.66 7 13 4 405.70 99.21 6 2 11 273.16 60.19 6 2 11 243.84 28.34 7 13 4 350.80 35.06 -2 11 7 12.81 6.23 -8 -2 9 13.40 15.92 8 2 -9 13.88 14.24 -2 11 7 13.04 13.72 -2 11 7 9.96 8.04 2 13 6 1998.53 93.79 2 11 -2 879.91 53.29 -2 -11 2 695.57 75.02 2 11 -2 762.73 73.39 2 13 6 1949.00 94.40 -2 1 13 148.17 36.23 2 -1 -13 129.97 28.57 10 8 8 1399.91 65.46 -8 5 2 176.24 38.13 -7 4 -4 1845.22 116.23 6 13 8 159.17 28.61 7 -4 4 1659.85 80.44 7 -4 4 1569.24 48.43 -10 0 -3 137.15 51.65 6 13 8 130.19 35.09 10 0 3 179.91 27.31 10 0 3 185.61 57.15 -6 -13 -8 88.78 37.44 -10 0 -3 206.30 49.02 10 10 0 721.14 193.13 -10 -10 0 781.02 38.05 -10 -10 0 805.43 54.32 -6 -5 9 364.90 87.58 -11 -2 -2 124.86 30.28 -11 -2 -2 83.23 34.52 11 2 2 94.08 24.54 11 9 4 91.93 18.54 6 5 -9 431.82 74.41 11 2 2 110.95 40.66 10 3 -6 69.23 39.98 -10 -3 6 98.26 30.95 5 -3 8 -12.15 11.79 5 -3 8 5.03 5.87 5 -3 8 3.16 6.58 5 -3 8 15.08 9.75 9 11 8 19.73 7.63 -9 -12 -4 103.06 21.13 -9 -11 -8 3.80 5.68 -3 2 13 34.02 23.96 9 12 4 142.91 34.38 -9 -12 -5 974.49 56.84 -9 -12 -4 85.31 31.12 -9 -12 -5 904.33 39.15 3 -2 -13 45.68 32.16 9 12 5 921.16 139.82 6 10 -4 6711.96 367.04 -6 -10 4 7505.39 228.51 0 12 3 1247.68 166.92 0 12 3 961.63 96.93 -7 -8 6 301.94 53.33 7 8 -6 239.78 53.43 0 -12 -3 922.78 57.28 5 6 13 1398.46 68.89 10 8 -3 670.20 117.96 -5 -6 -13 1300.49 55.17 -10 -11 -4 949.11 71.68 5 6 13 1426.19 56.76 -10 -11 -4 955.36 44.23 -5 3 12 550.07 124.28 -2 -13 -5 124.62 53.02 2 13 5 180.76 40.42 2 13 5 196.87 38.01 -3 7 -5 772.30 55.88 -10 -8 3 665.49 48.73 10 11 4 873.90 53.71 3 -7 5 733.61 56.45 5 -3 -12 549.00 52.23 7 11 -2 -0.11 16.74 -7 -11 2 -3.15 16.46 9 10 9 464.80 36.61 8 2 9 2138.93 94.99 10 -1 1 2218.96 119.97 -10 1 -1 2551.76 101.01 8 2 9 1926.99 87.57 10 -1 1 2328.28 92.54 6 -2 8 500.69 31.88 8 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5 6.03 14.40 -8 -11 7 189.11 68.01 -2 -13 4 15.53 7.13 5 8 17 85.45 33.26 -4 13 7 14.60 11.90 2 13 -4 8.34 15.38 0 15 3 112.27 42.78 -13 1 3 119.17 53.60 -4 13 6 70.68 27.98 4 16 2 19.62 12.40 4 16 2 12.40 17.40 3 12 -6 321.09 117.67 8 5 -12 25.69 21.12 -2 10 16 3.71 13.02 5 -3 12 22.01 13.29 -3 -12 6 400.70 112.08 -2 10 16 13.35 17.53 -8 -5 12 18.49 20.27 5 -3 12 24.48 14.22 -7 9 -1 71.27 25.44 -5 4 16 145.03 43.72 -11 -4 10 104.47 19.15 -5 4 16 151.80 60.84 11 4 -10 48.55 47.87 11 9 -7 30.76 17.90 6 12 16 279.03 98.44 -11 -9 7 37.49 14.24 7 -5 8 88.49 40.36 -1 13 14 84.86 27.96 -1 13 14 43.09 18.83 13 11 -2 324.09 101.68 -13 -11 2 357.90 105.76 0 8 -10 4.06 12.63 0 15 11 71.74 29.97 9 15 12 -3.39 19.01 0 -8 10 35.64 18.30 9 16 10 -7.64 21.83 5 9 17 116.34 49.97 0 15 11 100.80 30.21 -8 8 -1 125.00 43.36 -11 5 5 7.79 10.95 -9 8 5 68.47 32.77 -5 3 16 63.05 34.30 -5 3 16 94.52 42.82 -1 14 1 393.27 124.93 13 13 2 195.74 75.77 14 6 6 224.98 116.86 5 14 15 5.14 5.67 11 11 -5 22.48 14.36 13 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-7 10 1 6.44 21.50 -5 12 2 -6.76 14.49 6 11 -8 19.47 14.13 1 7 18 8.69 12.03 1 7 18 16.32 20.13 7 17 4 55.73 24.28 7 17 4 51.12 25.88 -8 9 1 11.30 13.76 -10 7 3 9.94 15.99 14 12 6 27.82 32.82 -6 7 15 39.98 14.67 11 15 1 29.25 24.65 15 8 2 41.44 18.09 -6 7 15 36.65 16.07 -11 -15 -1 3.83 5.55 -7 10 10 -1.75 19.88 12 10 12 10.04 7.81 6 0 14 -7.76 13.27 -1 10 17 519.29 160.54 -1 10 17 411.21 187.82 11 3 11 3.34 5.10 4 16 13 37.50 25.73 2 1 -16 7.41 12.84 -2 12 15 46.79 27.78 1 -11 6 55.01 19.58 8 9 16 371.37 151.68 -11 5 0 70.59 35.05 -4 13 10 122.46 48.07 -7 8 -4 50.74 15.61 -2 12 15 43.11 21.20 -2 -1 16 0.37 8.85 4 16 13 47.82 23.35 -3 12 14 14.78 19.33 11 16 6 60.50 31.07 -11 4 9 96.10 50.76 -3 12 14 17.51 12.74 -10 7 6 27.52 21.91 3 13 -5 38.25 19.36 -3 14 5 19.91 18.42 -3 -13 5 32.14 18.71 3 3 17 5.48 8.29 3 3 17 28.14 13.79 12 9 12 7.81 9.00 11 13 -3 89.40 38.08 6 10 17 8.14 13.32 -11 -13 3 45.22 27.50 1 -6 12 -1.88 15.80 15 6 1 32.43 15.00 -4 13 3 -3.89 8.32 -13 -6 7 6.84 7.01 10 16 10 2.45 19.96 13 6 -7 29.23 17.59 2 7 18 21.29 19.38 9 7 15 21.12 16.89 -8 -13 5 12.85 10.51 2 7 18 28.10 21.34 8 13 -5 -0.51 25.74 2 9 -10 17.26 15.42 2 15 14 675.11 75.00 2 15 14 515.35 165.72 -2 -9 10 1.31 9.26 -2 9 17 1636.30 137.46 -11 3 10 1.02 8.60 14 9 8 -16.78 18.98 0 -4 14 65.80 25.38 5 -1 14 6.81 9.49 -1 -1 16 874.16 135.87 -9 -14 3 65.23 26.57 -1 -1 16 646.24 205.00 5 -1 14 15.32 15.28 9 14 -3 107.40 37.81 0 4 -14 50.17 42.37 8 10 16 14.12 18.05 -2 9 17 1888.74 107.22 15 8 1 15.20 10.87 4 17 5 336.66 149.04 2 8 18 -1.49 21.33 13 11 -3 19.96 31.36 4 17 5 439.38 124.17 2 8 18 0.97 12.40 -13 -11 3 32.77 16.20 -12 3 7 148.10 79.40 -7 9 12 12.50 23.25 11 16 7 18.86 16.91 1 6 18 -1.59 21.34 1 6 18 -21.90 13.48 14 3 -5 72.32 50.60 -12 1 9 217.94 68.29 -6 -15 2 13.06 17.28 12 -1 -9 225.97 94.94 6 15 -2 26.21 24.07 -8 8 -2 57.88 32.87 12 13 11 287.97 110.04 -1 14 0 81.15 43.82 3 12 17 146.78 73.69 3 12 17 169.86 65.39 14 9 -3 65.01 47.59 -14 -9 3 43.65 25.61 15 8 3 19.32 23.51 1 8 18 60.23 23.71 15 7 0 5.15 9.65 12 14 10 -15.73 21.24 1 8 18 21.39 13.83 11 12 13 -1.30 17.27 -12 -5 9 97.91 46.71 12 7 -8 29.68 24.90 12 5 -9 107.64 44.86 -12 -7 8 19.05 21.24 -3 14 9 20.04 19.38 11 7 13 33.77 14.62 15 6 2 12.27 7.83 15 7 3 29.11 19.34 15 6 0 0.23 12.67 11 16 5 119.10 43.06 5 17 4 67.12 29.98 -2 -7 12 36.75 19.00 -8 -4 13 64.47 24.22 8 4 -13 52.35 32.72 -7 9 -2 12.84 14.41 2 7 -12 48.00 32.91 2 0 16 500.18 71.11 2 0 16 327.66 161.65 14 10 -2 23.73 30.02 4 17 10 11.58 6.75 1 -8 10 65.72 30.35 -1 8 -10 22.14 19.41 4 17 10 5.99 14.04 9 17 7 -13.29 12.56 9 17 7 5.98 13.83 4 12 17 39.66 26.51 -10 -7 10 7.07 9.68 -5 10 14 48.71 29.85 10 7 -10 2.89 25.89 4 12 17 56.01 30.08 3 -6 11 39.71 25.72 3 -6 11 21.87 21.94 13 5 9 18.51 18.00 11 -1 -11 39.09 18.38 12 15 8 307.30 146.66 0 7 18 189.02 110.78 0 7 18 262.20 83.01 9 15 13 0.41 14.00 -11 1 11 23.91 14.86 0 6 18 32.27 17.62 1 16 4 26.93 13.57 0 6 18 6.41 18.12 14 10 8 214.63 103.50 2 16 12 -6.28 18.14 -7 7 14 136.95 53.46 10 15 12 191.33 48.31 2 16 12 -0.73 13.17 -3 2 17 116.48 69.43 14 8 8 -2.86 17.12 10 13 -4 121.61 48.88 -10 -13 4 123.02 52.22 13 7 10 -1.84 13.39 8 8 16 159.71 71.36 7 10 -9 -17.22 24.82 12 15 3 14.63 23.52 13 14 3 24.25 13.29 -7 -10 9 -2.43 19.13 3 17 8 46.85 33.50 3 17 8 53.51 25.40 9 17 6 10.14 7.35 9 17 6 2.18 11.15 3 17 7 -18.10 18.02 2 3 -15 196.73 76.25 3 17 7 8.78 14.99 -2 -3 15 140.02 56.54 12 11 12 104.13 35.80 7 15 -2 7.89 24.73 5 5 17 87.81 34.64 -9 4 13 23.89 20.59 9 12 15 26.15 16.95 3 -5 12 9.17 10.92 3 -5 12 7.84 5.84 -3 -1 16 6.92 8.77 -7 -15 2 26.06 18.51 3 1 -16 16.63 15.78 1 13 16 157.58 77.56 14 6 -5 16.18 19.29 -14 -6 5 16.36 16.33 1 13 16 233.05 58.77 -9 6 -4 17.09 17.47 -5 -15 2 59.59 28.33 6 7 17 344.39 144.25 7 1 14 51.98 29.23 5 15 -2 84.97 34.10 7 0 -15 -3.59 27.95 -9 -12 6 551.41 174.93 -7 0 15 -30.37 20.88 13 14 7 -5.83 17.74 9 12 -6 593.86 197.90 -4 11 -3 28.62 19.89 -12 -14 0 27.21 15.93 0 11 17 23.00 17.80 -2 11 16 92.01 37.10 12 14 0 29.63 19.90 0 11 17 -3.63 20.09 -3 -3 15 107.21 45.10 -2 11 16 66.71 26.92 3 3 -15 125.27 48.60 -13 0 7 -1.32 12.20 -6 11 1 9.03 10.12 2 6 18 1.77 7.63 -13 -13 0 -5.29 11.09 10 3 -12 39.51 20.51 2 6 18 0.66 13.27 13 13 0 31.63 21.57 -10 -3 12 46.14 19.79 -3 10 16 35.52 25.59 -3 10 16 35.45 23.05 9 14 14 10.37 7.41 -13 -8 6 101.49 49.72 1 14 15 14.26 19.35 13 8 -6 98.34 36.66 1 14 15 35.90 23.24 9 4 14 12.34 9.88 -9 -8 10 8.69 9.19 12 8 12 4.04 12.49 9 17 8 86.54 45.58 9 17 8 66.93 31.83 -5 7 16 17.33 18.50 -7 -9 10 29.16 20.16 -5 7 16 26.52 17.66 15 9 2 31.65 23.50 7 9 -10 18.38 11.31 9 8 -10 2.13 15.06 13 13 9 66.16 37.68 -12 4 3 7.04 6.70 -13 1 6 3.57 9.37 7 16 13 71.80 27.79 -2 14 12 8.46 19.90 7 16 13 76.30 33.06 10 -3 -12 -0.31 8.20 -14 -8 4 103.26 51.05 -10 3 12 16.94 23.59 7 5 -13 39.75 31.83 -4 4 17 84.36 36.94 -9 8 1 27.52 16.96 -4 4 17 117.45 47.59 14 8 -4 129.29 46.82 8 17 4 148.13 65.50 2 12 17 76.87 47.87 15 9 3 41.13 31.10 3 6 -13 14.60 20.42 8 17 4 114.15 51.24 -3 -6 13 13.48 11.15 2 12 17 99.70 36.60 3 8 18 338.28 50.56 3 -10 6 334.25 167.14 -4 5 17 47.16 22.82 -4 5 17 24.08 25.79 10 4 13 -8.47 13.45 3 11 -8 27.24 16.05 4 6 -13 6.35 15.26 -12 4 4 -2.02 11.44 -4 -6 13 25.95 27.43 6 17 11 213.76 66.93 -3 -11 8 9.83 22.51 6 17 11 178.39 63.90 2 9 18 179.00 91.84 -11 -3 11 1.63 12.65 -9 7 -2 45.79 16.06 2 9 18 141.40 84.26 11 16 8 13.16 14.32 15 8 0 -1.48 21.28 11 3 -11 17.40 16.79 -10 7 2 35.43 18.11 6 14 -4 85.21 39.08 8 17 10 30.82 18.40 -6 9 -4 12.09 10.67 1 -5 13 17.46 14.47 7 5 16 75.56 47.83 8 11 16 4.17 9.79 8 17 10 31.61 21.14 3 -7 10 14.31 15.64 14 12 1 12.55 15.76 -12 -13 2 -6.61 11.73 15 5 1 4.60 10.31 2 2 17 13.29 14.64 2 2 17 1.00 8.10 15 5 0 5.80 11.08 -7 -11 8 -0.89 8.46 3 7 18 9.95 10.17 -6 3 16 47.73 25.60 7 11 -8 8.15 11.95 15 8 4 210.48 139.35 -5 9 15 25.27 23.70 3 17 9 44.54 21.96 3 17 9 36.88 21.90 9 16 1 43.86 25.62 -7 5 15 6.12 22.36 -5 9 15 33.26 14.33 -2 13 14 174.67 67.19 -2 13 14 205.92 34.61 5 17 11 112.32 50.72 5 17 11 176.12 53.89 -9 -16 -1 24.59 14.83 -9 -5 12 37.60 18.73 9 5 -12 50.69 32.89 -2 -10 9 291.55 103.92 2 10 -9 335.83 94.73 0 -1 16 260.96 91.20 0 -1 16 258.92 97.73 -10 7 7 35.91 22.56 15 6 3 17.96 17.41 15 6 -1 -7.15 18.71 -1 15 11 12.50 21.34 4 -8 8 24.73 20.14 1 16 11 -14.01 12.64 0 8 18 19.03 21.54 -10 -16 -2 36.79 18.80 0 8 18 7.74 11.60 10 16 2 29.69 24.63 1 16 11 29.57 18.50 -3 8 17 242.04 89.63 3 17 6 34.46 27.65 -3 8 17 272.33 86.72 0 5 18 15.34 20.87 0 5 18 35.33 18.68 3 17 6 -7.01 16.19 5 12 -7 -4.89 21.99 5 14 -4 72.78 28.87 -5 -14 4 78.50 23.38 11 14 12 15.82 30.30 11 16 4 -1.34 10.91 -12 4 2 85.24 40.58 4 -2 14 321.79 52.95 -13 -3 8 24.06 27.96 -11 -16 -4 15.75 13.55 5 -8 7 4.27 8.08 13 3 -8 7.84 19.01 -8 -6 12 -6.17 19.13 4 -2 14 164.54 87.51 6 7 -12 8.81 18.32 1 5 18 15.29 9.41 13 12 10 57.36 29.62 14 11 -1 52.25 41.65 -4 10 -5 82.90 39.30 15 9 1 24.70 27.71 -5 0 16 17.35 19.27 1 3 -15 25.49 25.41 3 16 13 152.00 64.94 3 16 13 125.55 50.67 9 17 5 147.53 44.68 -1 -3 15 27.58 27.52 -6 -16 0 60.41 36.00 14 12 7 17.81 14.39 -3 14 4 5.16 21.36 -1 1 17 103.55 38.55 6 16 0 51.09 19.99 3 9 18 14.80 8.58 1 9 18 131.84 68.82 15 7 -1 -3.63 19.41 1 9 18 148.39 72.80 -6 10 -2 11.59 11.74 6 12 -7 85.22 34.28 5 12 17 -8.79 22.29 -8 6 -6 70.38 23.48 5 12 17 1.21 9.60 -1 13 15 60.47 23.10 -1 13 15 65.82 40.67 -13 -2 8 200.82 106.42 -8 5 14 35.09 30.00 13 2 -8 158.75 93.04 -13 -12 2 -0.79 10.38 -8 5 14 13.06 16.68 -4 3 17 96.28 43.01 -4 3 17 70.56 32.40 15 9 4 13.05 11.78 15 7 4 80.91 44.20 12 5 11 294.56 132.62 -1 12 16 16.46 20.91 -1 12 16 0.08 19.44 -14 -2 5 94.95 36.48 -7 7 -6 10.54 7.30 3 -4 13 172.22 78.56 -4 -3 15 14.76 19.73 7 16 0 -4.22 20.30 3 -4 13 168.67 75.13 7 17 11 28.94 19.81 -7 -16 0 -1.89 17.63 7 17 11 20.35 17.57 -1 6 18 120.90 47.18 -1 6 18 146.81 41.45 14 11 8 -14.62 20.40 15 5 2 2.79 12.92 0 16 8 41.33 34.15 -13 2 4 41.58 20.64 -3 13 0 124.70 42.35 -7 -14 4 398.00 132.48 6 -2 -16 53.27 36.20 7 14 -4 413.96 130.53 14 7 8 6.12 8.28 -11 5 8 164.84 67.41 -2 -6 13 21.31 13.92 2 6 -13 -2.80 24.38 -12 4 5 9.64 13.07 15 5 -1 4.98 11.33 -1 9 -9 -5.88 16.55 1 -9 9 439.16 178.95 2 -10 7 24.90 18.81 -4 6 17 82.35 34.32 -4 6 17 113.87 38.49 -4 9 16 10.73 9.16 9 17 9 56.05 26.09 9 17 9 55.08 31.72 -4 9 16 19.49 13.45 10 6 14 -3.86 9.31 -8 9 10 4.50 13.15 -2 1 17 491.96 149.10 9 2 13 41.87 21.55 -9 8 9 3.25 11.25 7 8 -11 18.45 13.18 0 1 17 131.75 39.82 -13 -4 8 95.72 32.58 0 1 17 107.93 41.31 13 4 -8 65.32 30.36 5 15 15 18.55 16.58 4 17 4 430.47 157.50 6 17 3 133.60 42.53 6 17 3 132.35 39.93 -1 -12 6 34.37 16.99 5 15 15 25.47 13.48 4 17 4 369.94 147.73 -5 -6 13 -10.41 18.80 -8 -15 2 534.25 157.71 8 2 -14 27.96 30.01 8 15 -2 505.73 180.71 8 4 15 110.30 60.89 5 6 -13 23.99 27.29 4 15 -2 31.69 16.43 8 7 16 40.54 26.92 -9 6 12 1.64 8.05 4 15 15 22.71 13.73 7 17 3 316.71 136.03 -1 7 18 9.06 14.41 4 15 15 -0.39 13.08 7 17 3 343.03 110.78 -1 7 18 -2.41 22.03 -1 -8 11 23.79 15.73 4 14 16 8.94 10.73 4 14 16 16.64 19.46 1 8 -11 15.29 14.04 -11 -10 7 92.22 39.76 -4 12 -1 28.14 16.68 5 16 0 62.36 24.63 5 16 0 55.57 35.53 12 12 12 193.44 103.72 9 3 -13 -6.38 26.73 -1 5 18 13.69 9.06 -6 9 14 -8.04 12.21 5 2 16 10.15 20.60 10 13 14 5.53 14.87 -12 -2 10 164.91 64.95 3 6 18 2.38 9.08 2 -2 15 1103.86 137.45 12 2 -10 122.59 50.22 2 -2 15 1250.49 186.39 -11 -11 6 36.82 14.16 -4 -1 16 2.96 13.18 4 17 11 94.12 44.68 4 17 11 96.09 26.62 14 5 7 52.78 30.41 11 -2 -11 5.35 10.50 -12 -10 6 46.47 26.33 -11 2 11 13.03 17.43 9 6 15 1.70 14.12 1 7 -12 37.76 26.74 12 1 -10 24.74 15.62 -12 -1 10 27.31 16.79 -1 -7 12 19.92 19.06 -10 5 11 30.48 24.54 15 10 3 -12.82 23.76 11 6 -10 34.32 19.74 -11 -6 10 -2.14 16.91 -14 -7 5 71.62 42.84 3 17 10 5.74 10.98 3 17 10 11.60 9.22 14 7 -5 63.62 35.81 -9 7 11 17.64 12.58 8 2 14 49.32 25.47 0 -11 7 189.56 82.27 5 14 16 37.75 21.40 5 14 16 30.58 23.66 -12 4 1 -5.36 11.61 -12 -15 -2 3.06 4.62 6 6 17 43.57 24.40 4 14 -4 0.09 17.16 1 12 17 12.07 15.18 4 1 16 -2.74 17.29 4 1 16 -1.28 10.95 1 12 17 38.07 29.10 12 7 12 9.33 11.49 -6 5 16 23.39 21.90 11 4 12 160.34 90.79 -3 13 13 7.92 17.78 -4 13 2 120.00 48.52 15 8 -1 34.69 16.58 -11 5 -1 -5.75 12.21 -12 -11 5 188.94 65.80 3 17 5 21.33 20.25 3 -8 9 9.80 16.33 15 9 0 146.88 94.15 15 10 2 232.15 123.21 -13 -1 8 20.02 22.61 4 8 18 72.80 31.36 7 12 -7 -27.63 24.17 0 15 13 12.04 11.04 13 1 -8 37.69 22.69 0 15 13 24.21 16.81 -1 -9 10 211.17 91.15 3 14 16 4.84 12.51 2 13 -5 -21.86 14.96 1 9 -10 231.56 71.40 3 14 16 7.10 10.16 -5 12 1 13.43 10.67 2 10 18 28.53 28.02 -8 9 0 4.75 7.56 11 6 13 12.37 10.29 10 2 12 35.30 20.45 5 17 3 137.75 47.62 -13 -7 7 17.68 19.95 5 17 3 123.15 36.47 -7 11 6 -2.64 9.05 6 -4 11 5.05 9.71 -9 -13 5 19.20 17.22 -11 -9 8 13.04 10.56 6 15 15 103.43 53.86 15 6 -2 12.23 11.32 15 10 4 9.71 15.89 15 8 5 304.48 166.37 10 15 -1 78.40 41.35 -10 -15 1 86.54 31.38 15 6 4 75.16 29.61 3 10 18 8.75 12.04 4 9 18 28.61 14.52 13 6 10 1.67 6.94 -8 -16 0 7.44 12.06 0 9 18 112.64 62.10 6 3 16 39.31 30.19 0 4 18 10.85 14.18 1 -4 14 161.93 56.62 1 -4 14 186.57 60.77 6 -5 10 -4.52 11.64 ; _shelx_hkl_checksum 73672 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.18037(3) 0.93421(3) -0.02837(2) 0.04380(12) Uani 1 1 d . . . . . Fe1 Fe 0.40937(3) 0.42926(3) 0.32784(3) 0.04501(13) Uani 1 1 d . . . . . S1 S 0.08872(7) 0.93080(7) -0.15166(5) 0.05339(18) Uani 1 1 d . . . . . S2 S 0.12461(6) 0.80740(6) 0.08951(5) 0.04946(17) Uani 1 1 d . . . . . S3 S 0.23110(7) 1.06510(7) -0.14532(5) 0.05429(19) Uani 1 1 d . . . . . S4 S 0.26995(7) 0.93885(6) 0.09493(5) 0.05243(18) Uani 1 1 d . . . . . O1 O 0.3722(2) 0.32661(17) 0.45600(14) 0.0575(5) Uani 1 1 d . . . . . O2 O 0.5804(2) 0.32208(19) 0.34177(17) 0.0676(6) Uani 1 1 d . . . . . N1 N 0.3256(2) 0.36970(18) 0.24981(16) 0.0443(5) Uani 1 1 d . . . . . N2 N 0.40919(19) 0.53604(18) 0.16176(16) 0.0428(5) Uani 1 1 d . . . . . N3 N 0.4739(2) 0.53735(19) 0.36271(16) 0.0474(5) Uani 1 1 d . . . . . N4 N 0.2404(2) 0.5664(2) 0.33727(17) 0.0497(5) Uani 1 1 d . . . . . N5 N -0.1164(3) 0.8039(3) -0.1939(2) 0.0802(8) Uani 1 1 d . . . . . N6 N -0.0500(3) 0.6259(3) 0.1249(3) 0.0777(8) Uani 1 1 d . . . . . N7 N 0.3853(3) 1.2613(3) -0.1839(2) 0.0889(10) Uani 1 1 d . . . . . N8 N 0.4318(3) 1.1005(3) 0.1420(2) 0.0757(8) Uani 1 1 d . . . . . C1 C 0.3589(3) 0.2284(2) 0.4800(2) 0.0493(6) Uani 1 1 d . . . . . C2 C 0.3686(3) 0.1515(3) 0.5843(2) 0.0648(8) Uani 1 1 d . . . . . H1 H 0.380902 0.172416 0.636525 0.078 Uiso 1 1 calc R U . . . C3 C 0.3604(4) 0.0463(3) 0.6113(3) 0.0779(10) Uani 1 1 d . . . . . H2 H 0.369390 -0.004326 0.681409 0.093 Uiso 1 1 calc R U . . . C4 C 0.3387(4) 0.0139(3) 0.5355(3) 0.0837(11) Uani 1 1 d . . . . . H3 H 0.334628 -0.058571 0.554549 0.100 Uiso 1 1 calc R U . . . C5 C 0.3234(4) 0.0886(3) 0.4332(3) 0.0752(10) Uani 1 1 d . . . . . H4 H 0.306061 0.067894 0.382601 0.090 Uiso 1 1 calc R U . . . C6 C 0.3333(3) 0.1971(2) 0.4027(2) 0.0541(7) Uani 1 1 d . . . . . C7 C 0.3158(3) 0.2691(2) 0.2938(2) 0.0514(6) Uani 1 1 d . . . . . H5 H 0.295461 0.241684 0.249855 0.062 Uiso 1 1 calc R U . . . C8 C 0.2969(2) 0.4350(2) 0.1402(2) 0.0457(6) Uani 1 1 d . . . . . C9 C 0.2267(3) 0.4208(3) 0.0768(2) 0.0566(7) Uani 1 1 d . . . . . H6 H 0.191577 0.366138 0.105669 0.068 Uiso 1 1 calc R U . . . C10 C 0.2088(3) 0.4887(3) -0.0306(2) 0.0619(8) Uani 1 1 d . . . . . H7 H 0.160728 0.479302 -0.072687 0.074 Uiso 1 1 calc R U . . . C11 C 0.2599(3) 0.5683(3) -0.0750(2) 0.0563(7) Uani 1 1 d . . . . . H8 H 0.248947 0.610591 -0.147061 0.068 Uiso 1 1 calc R U . . . C12 C 0.3294(2) 0.5873(2) -0.0129(2) 0.0467(6) Uani 1 1 d . . . . . C13 C 0.3461(2) 0.5212(2) 0.09570(19) 0.0423(5) Uani 1 1 d . . . . . C14 C 0.3861(3) 0.6671(2) -0.0529(2) 0.0529(7) Uani 1 1 d . . . . . H9 H 0.379006 0.711178 -0.124508 0.063 Uiso 1 1 calc R U . . . C15 C 0.4514(3) 0.6799(2) 0.0132(2) 0.0524(6) Uani 1 1 d . . . . . H10 H 0.489779 0.732148 -0.012566 0.063 Uiso 1 1 calc R U . . . C16 C 0.4598(2) 0.6132(2) 0.1208(2) 0.0479(6) Uani 1 1 d . . . . . H11 H 0.503133 0.623677 0.165589 0.057 Uiso 1 1 calc R U . . . C17 C 0.6875(3) 0.3252(3) 0.3536(2) 0.0699(9) Uani 1 1 d . . . . . C18 C 0.7990(3) 0.2315(4) 0.3516(3) 0.0890(13) Uani 1 1 d . . . . . H12 H 0.794752 0.169212 0.342153 0.107 Uiso 1 1 calc R U . . . C19 C 0.9130(4) 0.2316(5) 0.3635(3) 0.1150(19) Uani 1 1 d . . . . . H13 H 0.985847 0.168320 0.364270 0.138 Uiso 1 1 calc R U . . . C20 C 0.9208(4) 0.3253(6) 0.3745(4) 0.124(2) Uani 1 1 d . . . . . H14 H 0.998939 0.325685 0.379448 0.149 Uiso 1 1 calc R U . . . C21 C 0.8170(4) 0.4166(5) 0.3782(3) 0.0999(14) Uani 1 1 d . . . . . H15 H 0.824048 0.477954 0.387276 0.120 Uiso 1 1 calc R U . . . C22 C 0.6965(3) 0.4179(3) 0.3682(2) 0.0670(8) Uani 1 1 d . . . . . C23 C 0.5915(3) 0.5155(3) 0.3747(2) 0.0606(8) Uani 1 1 d . . . . . H16 H 0.608925 0.569192 0.388989 0.073 Uiso 1 1 calc R U . . . C24 C 0.3793(3) 0.6418(2) 0.3654(2) 0.0515(6) Uani 1 1 d . . . . . C25 C 0.3960(4) 0.7291(3) 0.3788(2) 0.0696(9) Uani 1 1 d . . . . . H17 H 0.476554 0.723636 0.385537 0.084 Uiso 1 1 calc R U . . . C26 C 0.2939(5) 0.8259(3) 0.3825(3) 0.0828(11) Uani 1 1 d . . . . . H18 H 0.307664 0.884530 0.391177 0.099 Uiso 1 1 calc R U . . . C27 C 0.1748(5) 0.8376(3) 0.3737(3) 0.0826(12) Uani 1 1 d . . . . . H19 H 0.108230 0.903300 0.376859 0.099 Uiso 1 1 calc R U . . . C28 C 0.1519(3) 0.7499(3) 0.3599(2) 0.0639(8) Uani 1 1 d . . . . . C29 C 0.2537(3) 0.6540(2) 0.35338(19) 0.0496(6) Uani 1 1 d . . . . . C30 C 0.0323(3) 0.7523(3) 0.3531(3) 0.0772(10) Uani 1 1 d . . . . . H20 H -0.038256 0.814211 0.357878 0.093 Uiso 1 1 calc R U . . . C31 C 0.0204(3) 0.6632(4) 0.3395(3) 0.0777(10) Uani 1 1 d . . . . . H21 H -0.058250 0.663483 0.335607 0.093 Uiso 1 1 calc R U . . . C32 C 0.1263(3) 0.5719(3) 0.3315(2) 0.0639(8) Uani 1 1 d . . . . . H22 H 0.116463 0.512070 0.321651 0.077 Uiso 1 1 calc R U . . . C33 C -0.0546(3) 0.8166(3) -0.1461(2) 0.0582(7) Uani 1 1 d . . . . . C34 C -0.0119(3) 0.6943(3) 0.0773(3) 0.0559(7) Uani 1 1 d . . . . . C35 C 0.0216(2) 0.8340(3) -0.0857(2) 0.0510(6) Uani 1 1 d . . . . . C36 C 0.0392(2) 0.7787(2) 0.0194(2) 0.0494(6) Uani 1 1 d . . . . . C37 C 0.3081(2) 1.1011(2) -0.0752(2) 0.0499(6) Uani 1 1 d . . . . . C38 C 0.3251(2) 1.0459(2) 0.0306(2) 0.0490(6) Uani 1 1 d . . . . . C39 C 0.3519(3) 1.1903(3) -0.1337(3) 0.0622(7) Uani 1 1 d . . . . . C40 C 0.3850(3) 1.0766(3) 0.0918(2) 0.0566(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0446(2) 0.0475(2) 0.0435(2) -0.02062(16) 0.00407(14) -0.02091(16) Fe1 0.0592(2) 0.0451(2) 0.0381(2) -0.01557(16) 0.00048(16) -0.02898(19) S1 0.0575(4) 0.0624(4) 0.0462(4) -0.0219(3) 0.0008(3) -0.0297(3) S2 0.0537(4) 0.0541(4) 0.0460(4) -0.0206(3) 0.0047(3) -0.0271(3) S3 0.0600(4) 0.0682(5) 0.0426(4) -0.0188(3) 0.0045(3) -0.0375(4) S4 0.0629(4) 0.0575(4) 0.0433(4) -0.0194(3) 0.0019(3) -0.0314(3) O1 0.0918(14) 0.0546(11) 0.0368(9) -0.0159(8) 0.0039(9) -0.0426(10) O2 0.0691(13) 0.0580(12) 0.0644(14) -0.0209(10) -0.0040(10) -0.0179(10) N1 0.0576(12) 0.0480(12) 0.0371(11) -0.0180(9) 0.0033(9) -0.0299(10) N2 0.0510(11) 0.0433(11) 0.0391(11) -0.0171(9) 0.0069(9) -0.0244(9) N3 0.0628(13) 0.0544(12) 0.0368(11) -0.0159(9) 0.0007(9) -0.0369(11) N4 0.0593(13) 0.0534(13) 0.0435(12) -0.0197(10) 0.0044(9) -0.0298(11) N5 0.0815(19) 0.117(2) 0.077(2) -0.0539(18) 0.0146(15) -0.0605(18) N6 0.088(2) 0.082(2) 0.084(2) -0.0351(17) 0.0145(16) -0.0538(17) N7 0.105(2) 0.103(3) 0.078(2) -0.0218(19) 0.0117(19) -0.076(2) N8 0.0779(18) 0.099(2) 0.078(2) -0.0488(17) 0.0062(15) -0.0484(17) C1 0.0689(17) 0.0451(14) 0.0421(14) -0.0160(11) 0.0077(12) -0.0335(13) C2 0.102(2) 0.0618(18) 0.0427(15) -0.0189(13) 0.0107(15) -0.0481(17) C3 0.126(3) 0.0640(19) 0.0490(18) -0.0113(15) 0.0118(18) -0.057(2) C4 0.146(4) 0.0623(19) 0.061(2) -0.0155(16) 0.010(2) -0.069(2) C5 0.130(3) 0.0590(18) 0.0552(18) -0.0205(15) 0.0050(18) -0.058(2) C6 0.0777(19) 0.0493(15) 0.0448(14) -0.0178(12) 0.0044(13) -0.0361(14) C7 0.0722(17) 0.0505(14) 0.0443(14) -0.0195(12) 0.0019(12) -0.0363(13) C8 0.0549(14) 0.0455(13) 0.0389(13) -0.0174(11) 0.0045(11) -0.0225(12) C9 0.0735(18) 0.0608(17) 0.0473(15) -0.0222(13) -0.0005(13) -0.0373(15) C10 0.0742(19) 0.0690(19) 0.0491(16) -0.0263(14) -0.0089(14) -0.0307(16) C11 0.0681(17) 0.0579(16) 0.0356(13) -0.0170(12) -0.0010(12) -0.0201(14) C12 0.0503(14) 0.0454(13) 0.0391(13) -0.0179(11) 0.0075(10) -0.0149(11) C13 0.0480(13) 0.0430(13) 0.0364(12) -0.0175(10) 0.0062(10) -0.0185(11) C14 0.0574(15) 0.0463(14) 0.0438(14) -0.0130(11) 0.0111(12) -0.0177(12) C15 0.0579(15) 0.0459(14) 0.0505(15) -0.0161(12) 0.0158(12) -0.0245(13) C16 0.0519(14) 0.0464(14) 0.0489(15) -0.0181(11) 0.0051(11) -0.0250(12) C17 0.068(2) 0.077(2) 0.0395(16) -0.0062(15) 0.0053(13) -0.0238(17) C18 0.071(2) 0.099(3) 0.0472(18) -0.0119(18) 0.0089(15) -0.007(2) C19 0.080(3) 0.143(5) 0.060(2) -0.014(3) 0.017(2) -0.019(3) C20 0.057(2) 0.181(6) 0.089(3) -0.020(4) 0.016(2) -0.043(3) C21 0.073(2) 0.135(4) 0.075(3) -0.014(2) 0.0063(19) -0.056(3) C22 0.0579(17) 0.083(2) 0.0451(16) -0.0064(15) 0.0027(13) -0.0337(17) C23 0.076(2) 0.0704(19) 0.0450(15) -0.0116(13) 0.0007(13) -0.0505(17) C24 0.0789(18) 0.0494(14) 0.0349(13) -0.0151(11) 0.0011(12) -0.0358(14) C25 0.115(3) 0.0646(19) 0.0509(17) -0.0247(14) 0.0017(16) -0.0544(19) C26 0.144(4) 0.0548(19) 0.058(2) -0.0234(15) -0.005(2) -0.045(2) C27 0.132(3) 0.0528(18) 0.0492(18) -0.0246(15) 0.001(2) -0.020(2) C28 0.088(2) 0.0558(17) 0.0380(14) -0.0181(12) -0.0014(14) -0.0208(16) C29 0.0714(17) 0.0441(14) 0.0339(12) -0.0151(10) 0.0005(11) -0.0243(13) C30 0.072(2) 0.081(2) 0.0557(19) -0.0288(17) 0.0029(15) -0.0088(18) C31 0.0602(19) 0.097(3) 0.068(2) -0.030(2) 0.0053(16) -0.0273(19) C32 0.0607(17) 0.073(2) 0.0625(19) -0.0245(16) 0.0028(14) -0.0340(16) C33 0.0553(16) 0.0736(19) 0.0576(17) -0.0328(15) 0.0089(13) -0.0324(15) C34 0.0552(15) 0.0608(17) 0.0645(18) -0.0321(15) 0.0062(13) -0.0294(14) C35 0.0436(13) 0.0577(16) 0.0598(17) -0.0303(13) 0.0038(12) -0.0218(12) C36 0.0417(13) 0.0474(14) 0.0626(17) -0.0262(13) 0.0053(11) -0.0181(11) C37 0.0465(13) 0.0568(16) 0.0523(15) -0.0228(12) 0.0066(11) -0.0266(12) C38 0.0445(14) 0.0544(15) 0.0541(16) -0.0252(13) 0.0037(11) -0.0229(12) C39 0.0640(17) 0.074(2) 0.0578(18) -0.0236(15) 0.0050(14) -0.0396(16) C40 0.0539(15) 0.0685(18) 0.0563(17) -0.0320(15) 0.0084(13) -0.0275(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.3463 0.8444 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.3393 1.1124 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 S3 Ni1 S2 178.20(3) . . S3 Ni1 S4 92.30(3) . . S2 Ni1 S4 87.47(3) . . S3 Ni1 S1 87.78(3) . . S2 Ni1 S1 92.43(3) . . S4 Ni1 S1 179.39(3) . . O2 Fe1 O1 94.18(10) . . O2 Fe1 N1 100.26(9) . . O1 Fe1 N1 87.15(8) . . O2 Fe1 N3 87.69(9) . . O1 Fe1 N3 108.32(8) . . N1 Fe1 N3 162.17(8) . . O2 Fe1 N4 163.36(9) . . O1 Fe1 N4 85.80(9) . . N1 Fe1 N4 96.35(8) . . N3 Fe1 N4 76.59(9) . . O2 Fe1 N2 93.71(9) . . O1 Fe1 N2 162.19(8) . . N1 Fe1 N2 75.73(8) . . N3 Fe1 N2 87.93(8) . . N4 Fe1 N2 91.15(8) . . C35 S1 Ni1 103.10(10) . . C36 S2 Ni1 103.35(10) . . C37 S3 Ni1 103.77(10) . . C38 S4 Ni1 103.56(10) . . C1 O1 Fe1 131.08(17) . . C17 O2 Fe1 134.4(2) . . C7 N1 C8 119.3(2) . . C7 N1 Fe1 123.24(18) . . C8 N1 Fe1 116.73(16) . . C16 N2 C13 118.0(2) . . C16 N2 Fe1 127.49(18) . . C13 N2 Fe1 114.44(16) . . C23 N3 C24 120.5(2) . . C23 N3 Fe1 123.9(2) . . C24 N3 Fe1 115.44(16) . . C32 N4 C29 118.0(3) . . C32 N4 Fe1 125.8(2) . . C29 N4 Fe1 116.18(18) . . O1 C1 C2 120.2(2) . . O1 C1 C6 121.9(2) . . C2 C1 C6 117.9(2) . . C3 C2 C1 121.3(3) . . C3 C2 H1 119.3 . . C1 C2 H1 119.3 . . C2 C3 C4 120.8(3) . . C2 C3 H2 119.6 . . C4 C3 H2 119.6 . . C5 C4 C3 119.6(3) . . C5 C4 H3 120.2 . . C3 C4 H3 120.2 . . C4 C5 C6 121.0(3) . . C4 C5 H4 119.5 . . C6 C5 H4 119.5 . . C5 C6 C1 119.3(3) . . C5 C6 C7 116.7(3) . . C1 C6 C7 124.0(2) . . N1 C7 C6 126.1(2) . . N1 C7 H5 117.0 . . C6 C7 H5 117.0 . . C9 C8 C13 119.5(2) . . C9 C8 N1 125.7(2) . . C13 C8 N1 114.8(2) . . C8 C9 C10 119.8(3) . . C8 C9 H6 120.1 . . C10 C9 H6 120.1 . . C11 C10 C9 121.4(3) . . C11 C10 H7 119.3 . . C9 C10 H7 119.3 . . C10 C11 C12 120.5(3) . . C10 C11 H8 119.7 . . C12 C11 H8 119.7 . . C14 C12 C13 117.4(3) . . C14 C12 C11 123.9(3) . . C13 C12 C11 118.6(3) . . N2 C13 C12 122.5(2) . . N2 C13 C8 117.4(2) . . C12 C13 C8 120.1(2) . . C15 C14 C12 119.8(3) . . C15 C14 H9 120.1 . . C12 C14 H9 120.1 . . C14 C15 C16 119.0(3) . . C14 C15 H10 120.5 . . C16 C15 H10 120.5 . . N2 C16 C15 123.2(3) . . N2 C16 H11 118.4 . . C15 C16 H11 118.4 . . O2 C17 C22 122.6(3) . . O2 C17 C18 118.8(4) . . C22 C17 C18 118.6(4) . . C19 C18 C17 120.5(5) . . C19 C18 H12 119.7 . . C17 C18 H12 119.7 . . C18 C19 C20 120.4(5) . . C18 C19 H13 119.8 . . C20 C19 H13 119.8 . . C21 C20 C19 121.4(5) . . C21 C20 H14 119.3 . . C19 C20 H14 119.3 . . C20 C21 C22 119.6(5) . . C20 C21 H15 120.2 . . C22 C21 H15 120.2 . . C17 C22 C23 124.0(3) . . C17 C22 C21 119.4(4) . . C23 C22 C21 116.5(4) . . N3 C23 C22 126.9(3) . . N3 C23 H16 116.6 . . C22 C23 H16 116.6 . . C25 C24 N3 126.8(3) . . C25 C24 C29 118.3(3) . . N3 C24 C29 114.9(2) . . C24 C25 C26 120.6(4) . . C24 C25 H17 119.7 . . C26 C25 H17 119.7 . . C27 C26 C25 122.0(3) . . C27 C26 H18 119.0 . . C25 C26 H18 119.0 . . C26 C27 C28 119.8(3) . . C26 C27 H19 120.1 . . C28 C27 H19 120.1 . . C29 C28 C30 117.4(3) . . C29 C28 C27 118.5(3) . . C30 C28 C27 124.1(3) . . N4 C29 C28 122.7(3) . . N4 C29 C24 116.6(2) . . C28 C29 C24 120.7(3) . . C31 C30 C28 119.4(3) . . C31 C30 H20 120.3 . . C28 C30 H20 120.3 . . C30 C31 C32 119.7(3) . . C30 C31 H21 120.1 . . C32 C31 H21 120.1 . . N4 C32 C31 122.8(3) . . N4 C32 H22 118.6 . . C31 C32 H22 118.6 . . N5 C33 C35 179.2(3) . . N6 C34 C36 178.3(3) . . C36 C35 C33 122.0(3) . . C36 C35 S1 120.5(2) . . C33 C35 S1 117.6(2) . . C35 C36 C34 122.2(3) . . C35 C36 S2 120.6(2) . . C34 C36 S2 117.2(2) . . C38 C37 C39 123.0(3) . . C38 C37 S3 120.3(2) . . C39 C37 S3 116.7(2) . . C37 C38 C40 121.9(3) . . C37 C38 S4 120.0(2) . . C40 C38 S4 118.1(2) . . N7 C39 C37 177.2(4) . . N8 C40 C38 178.9(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 S3 2.1340(8) . Ni1 S2 2.1383(8) . Ni1 S4 2.1421(8) . Ni1 S1 2.1466(8) . Fe1 O2 1.908(2) . Fe1 O1 1.9278(19) . Fe1 N1 2.097(2) . Fe1 N3 2.131(2) . Fe1 N4 2.136(2) . Fe1 N2 2.195(2) . S1 C35 1.718(3) . S2 C36 1.715(3) . S3 C37 1.715(3) . S4 C38 1.720(3) . O1 C1 1.309(3) . O2 C17 1.305(4) . N1 C7 1.302(3) . N1 C8 1.420(3) . N2 C16 1.322(3) . N2 C13 1.361(3) . N3 C23 1.301(4) . N3 C24 1.414(4) . N4 C32 1.321(4) . N4 C29 1.369(3) . N5 C33 1.137(4) . N6 C34 1.139(4) . N7 C39 1.137(4) . N8 C40 1.145(4) . C1 C2 1.396(4) . C1 C6 1.413(4) . C2 C3 1.365(4) . C2 H1 0.9300 . C3 C4 1.387(5) . C3 H2 0.9300 . C4 C5 1.357(5) . C4 H3 0.9300 . C5 C6 1.410(4) . C5 H4 0.9300 . C6 C7 1.422(4) . C7 H5 0.9300 . C8 C9 1.384(4) . C8 C13 1.412(4) . C9 C10 1.395(4) . C9 H6 0.9300 . C10 C11 1.357(4) . C10 H7 0.9300 . C11 C12 1.408(4) . C11 H8 0.9300 . C12 C14 1.403(4) . C12 C13 1.405(4) . C14 C15 1.361(4) . C14 H9 0.9300 . C15 C16 1.402(4) . C15 H10 0.9300 . C16 H11 0.9300 . C17 C22 1.401(5) . C17 C18 1.413(5) . C18 C19 1.366(7) . C18 H12 0.9300 . C19 C20 1.382(8) . C19 H13 0.9300 . C20 C21 1.354(7) . C20 H14 0.9300 . C21 C22 1.428(5) . C21 H15 0.9300 . C22 C23 1.425(5) . C23 H16 0.9300 . C24 C25 1.363(4) . C24 C29 1.434(4) . C25 C26 1.388(5) . C25 H17 0.9300 . C26 C27 1.354(6) . C26 H18 0.9300 . C27 C28 1.411(5) . C27 H19 0.9300 . C28 C29 1.393(4) . C28 C30 1.405(5) . C30 C31 1.362(5) . C30 H20 0.9300 . C31 C32 1.389(5) . C31 H21 0.9300 . C32 H22 0.9300 . C33 C35 1.431(4) . C34 C36 1.436(4) . C35 C36 1.349(4) . C37 C38 1.358(4) . C37 C39 1.429(4) . C38 C40 1.432(4) . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Fe1 O1 C1 C2 161.0(2) . . . . Fe1 O1 C1 C6 -19.7(4) . . . . O1 C1 C2 C3 -177.2(3) . . . . C6 C1 C2 C3 3.5(5) . . . . C1 C2 C3 C4 -1.7(6) . . . . C2 C3 C4 C5 -1.1(7) . . . . C3 C4 C5 C6 2.1(7) . . . . C4 C5 C6 C1 -0.3(6) . . . . C4 C5 C6 C7 180.0(4) . . . . O1 C1 C6 C5 178.3(3) . . . . C2 C1 C6 C5 -2.4(5) . . . . O1 C1 C6 C7 -2.0(5) . . . . C2 C1 C6 C7 177.3(3) . . . . C8 N1 C7 C6 -175.8(3) . . . . Fe1 N1 C7 C6 14.5(4) . . . . C5 C6 C7 N1 -177.4(3) . . . . C1 C6 C7 N1 3.0(5) . . . . C7 N1 C8 C9 19.0(4) . . . . Fe1 N1 C8 C9 -170.6(2) . . . . C7 N1 C8 C13 -161.2(2) . . . . Fe1 N1 C8 C13 9.2(3) . . . . C13 C8 C9 C10 2.1(4) . . . . N1 C8 C9 C10 -178.1(3) . . . . C8 C9 C10 C11 0.7(5) . . . . C9 C10 C11 C12 -2.2(5) . . . . C10 C11 C12 C14 179.4(3) . . . . C10 C11 C12 C13 0.8(4) . . . . C16 N2 C13 C12 -2.3(4) . . . . Fe1 N2 C13 C12 176.04(19) . . . . C16 N2 C13 C8 177.5(2) . . . . Fe1 N2 C13 C8 -4.2(3) . . . . C14 C12 C13 N2 3.0(4) . . . . C11 C12 C13 N2 -178.3(2) . . . . C14 C12 C13 C8 -176.7(2) . . . . C11 C12 C13 C8 2.0(4) . . . . C9 C8 C13 N2 176.8(2) . . . . N1 C8 C13 N2 -3.0(3) . . . . C9 C8 C13 C12 -3.4(4) . . . . N1 C8 C13 C12 176.7(2) . . . . C13 C12 C14 C15 -1.6(4) . . . . C11 C12 C14 C15 179.8(2) . . . . C12 C14 C15 C16 -0.5(4) . . . . C13 N2 C16 C15 0.1(4) . . . . Fe1 N2 C16 C15 -178.03(18) . . . . C14 C15 C16 N2 1.3(4) . . . . Fe1 O2 C17 C22 5.9(5) . . . . Fe1 O2 C17 C18 -174.2(2) . . . . O2 C17 C18 C19 179.9(3) . . . . C22 C17 C18 C19 -0.1(5) . . . . C17 C18 C19 C20 -2.0(6) . . . . C18 C19 C20 C21 2.8(8) . . . . C19 C20 C21 C22 -1.5(7) . . . . O2 C17 C22 C23 1.9(5) . . . . C18 C17 C22 C23 -178.1(3) . . . . O2 C17 C22 C21 -178.6(3) . . . . C18 C17 C22 C21 1.4(5) . . . . C20 C21 C22 C17 -0.6(6) . . . . C20 C21 C22 C23 178.9(4) . . . . C24 N3 C23 C22 -176.3(3) . . . . Fe1 N3 C23 C22 -0.7(4) . . . . C17 C22 C23 N3 -4.1(5) . . . . C21 C22 C23 N3 176.5(3) . . . . C23 N3 C24 C25 0.7(4) . . . . Fe1 N3 C24 C25 -175.2(2) . . . . C23 N3 C24 C29 -178.8(2) . . . . Fe1 N3 C24 C29 5.3(3) . . . . N3 C24 C25 C26 -178.4(3) . . . . C29 C24 C25 C26 1.1(4) . . . . C24 C25 C26 C27 0.4(5) . . . . C25 C26 C27 C28 -0.3(5) . . . . C26 C27 C28 C29 -1.4(5) . . . . C26 C27 C28 C30 178.1(3) . . . . C32 N4 C29 C28 -2.4(4) . . . . Fe1 N4 C29 C28 179.2(2) . . . . C32 N4 C29 C24 176.4(2) . . . . Fe1 N4 C29 C24 -1.9(3) . . . . C30 C28 C29 N4 2.3(4) . . . . C27 C28 C29 N4 -178.2(3) . . . . C30 C28 C29 C24 -176.5(3) . . . . C27 C28 C29 C24 2.9(4) . . . . C25 C24 C29 N4 178.3(2) . . . . N3 C24 C29 N4 -2.2(3) . . . . C25 C24 C29 C28 -2.8(4) . . . . N3 C24 C29 C28 176.7(2) . . . . C29 C28 C30 C31 -0.7(5) . . . . C27 C28 C30 C31 179.9(3) . . . . C28 C30 C31 C32 -0.6(5) . . . . C29 N4 C32 C31 1.0(4) . . . . Fe1 N4 C32 C31 179.2(2) . . . . C30 C31 C32 N4 0.5(5) . . . . Ni1 S1 C35 C36 -2.5(2) . . . . Ni1 S1 C35 C33 176.3(2) . . . . C33 C35 C36 C34 3.3(4) . . . . S1 C35 C36 C34 -178.0(2) . . . . C33 C35 C36 S2 -176.7(2) . . . . S1 C35 C36 S2 2.1(3) . . . . Ni1 S2 C36 C35 -0.5(2) . . . . Ni1 S2 C36 C34 179.56(19) . . . . Ni1 S3 C37 C38 1.2(2) . . . . Ni1 S3 C37 C39 -178.8(2) . . . . C39 C37 C38 C40 2.2(4) . . . . S3 C37 C38 C40 -177.8(2) . . . . C39 C37 C38 S4 -179.7(2) . . . . S3 C37 C38 S4 0.3(3) . . . . Ni1 S4 C38 C37 -1.7(2) . . . . Ni1 S4 C38 C40 176.52(18) . . . .