#------------------------------------------------------------------------------ #$Date: 2021-10-15 02:04:43 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269958 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708560.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_7708560 loop_ _publ_author_name 'Peng, Min' 'Wu, Xiao-Fan' 'Wang, Li-Xin' 'Chen, Si-Huai' 'Xiang, Jing' 'Jin, Xin-Xin' 'Yiu, Shek-Man' 'Wang, Bing-Wu' 'Gao, Song' 'Lau, Tai-Chu' _publ_section_title ; Slow magnetic relaxation in high-coordinate Co(II) and Fe(II) compounds bearing neutral tetradentate ligands. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt02575a _journal_year 2021 _chemical_formula_sum 'C42 H56 Cl2 Fe N20 O10' _chemical_formula_weight 1127.81 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2021-08-29 deposited with the CCDC. 2021-09-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.895(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.9954(9) _cell_length_b 10.5941(5) _cell_length_c 16.1100(9) _cell_measurement_reflns_used 6083 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 25.90 _cell_measurement_theta_min 2.30 _cell_volume 2726.5(3) _computing_cell_refinement 'Bruker Saint' _computing_data_collection 'Bruker Apex3' _computing_data_reduction 'Bruker Saint' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 213(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 Venture Photon II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_unetI/netI 0.0599 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 22503 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.471 _diffrn_reflns_theta_min 2.302 _diffrn_source 'micro focus' _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5716 _exptl_absorpt_correction_type multi-scan _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_crystal_colour orange _exptl_crystal_density_diffrn 1.374 _exptl_crystal_description block _exptl_crystal_F_000 1176 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.550 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 422 _refine_ls_number_reflns 5606 _refine_ls_number_restraints 414 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0570 _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^)+(0.0685P)^2^+2.6930P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1406 _refine_ls_wR_factor_ref 0.1607 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4085 _reflns_number_total 5606 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02575a2.cif _cod_data_source_block 082421b_xj _cod_original_sg_symbol_H-M 'P 2/n' _cod_database_code 7708560 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL 1_a.res in P2/n 082421b_xj.res created by SHELXL-2016/6 at 15:09:16 on 25-Aug-2021 REM Old TITL 1 in P2/n REM SHELXT solution in P2/n REM R1 0.219, Rweak 0.012, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C53 Cl2 Fe N14 CELL 0.71073 15.9954 10.5941 16.1100 90.000 92.895 90.000 ZERR 2.000 0.0009 0.0005 0.0009 0.000 0.002 0.000 LATT 1 SYMM 0.5-X,+Y,0.5-Z SFAC C H Cl Fe N O UNIT 84 112 4 2 40 20 OMIT -1 1 1 OMIT 1 1 0 SADI_CLO4 CL1 O1 CL1 O2 CL1 O3 CL1 O4 SADI_CLO4 O1 O3 O2 O4 O1 O4 O2 O3 O1 O2 O3 O4 SADI_CLO4 CL2 O5 CL2 O6 CL2 O7 CL2 O8 SADI_CLO4 O5 O7 O6 O8 O5 O8 O6 O7 O5 O6 O7 O8 RIGU_CLO4 CL1 > O4 RIGU_CLO4 CL2 > O8 SAME_CLO4 CL1 > O4 SAME_CLO4 CL2 > O8 eadp c13 c13a exyz c13 c13a DELU 0.008 C13 > C16a ISOR 0.04 C13 > C16a SIMU 0.01 C13 > C16a L.S. 20 PLAN 20 TEMP -60(2) CONF BOND $H LIST 4 ACTA fmap 2 MORE -1 WGHT 0.068500 2.693000 FVAR 0.37545 RESI CLO4 1 PART -1 DELU CL1 > O4 ISOR CL1 > O4 SIMU CL1 > O4 spec 0.01 CL1 3 0.249259 0.210946 0.250974 10.50000 0.04578 0.04261 = 0.04633 0.01472 0.00172 0.01406 O1 6 0.205213 0.294201 0.195843 10.50000 0.10703 0.04873 = 0.08906 0.02581 -0.06695 -0.00857 O2 6 0.203287 0.195108 0.320684 10.50000 0.10780 0.19757 = 0.10205 0.05082 0.05517 -0.00533 O3 6 0.323860 0.266910 0.275058 10.50000 0.05623 0.17140 = 0.18815 0.11849 -0.04798 -0.05040 O4 6 0.257064 0.098208 0.214441 10.50000 0.34565 0.06441 = 0.17376 -0.04008 -0.00753 0.08854 RESI CLO4 2 PART -1 DELU CL2 > O8 ISOR CL2 > O8 SIMU CL2 > O8 CL2 3 0.760457 1.294106 0.261941 10.50000 0.03403 0.04708 = 0.05605 -0.00395 0.00822 0.00310 O5 6 0.683675 1.353413 0.271375 10.50000 0.03448 0.09786 = 0.12896 -0.00781 0.00828 0.03085 O6 6 0.747849 1.162837 0.247972 10.50000 0.06953 0.04687 = 0.11586 -0.01453 0.02551 -0.01668 O7 6 0.809254 1.307498 0.338453 10.50000 0.09920 0.11566 = 0.08926 -0.02982 -0.03646 0.02745 O8 6 0.806485 1.346095 0.199943 10.50000 0.10304 0.07716 = 0.11385 0.03002 0.05457 -0.00700 PART 0 RESI 0 FE1 4 0.250000 0.689009 0.250000 10.50000 0.02559 0.02959 = 0.02975 0.00000 -0.00162 0.00000 N1 5 0.342721 0.833785 0.209234 11.00000 0.03217 0.03520 = 0.03630 0.00184 -0.00181 -0.00414 N2 5 0.413533 0.880824 0.241980 11.00000 0.03567 0.04040 = 0.04075 0.00252 -0.00106 -0.00783 N3 5 0.443170 0.952357 0.182990 11.00000 0.03134 0.03948 = 0.03589 -0.00177 0.00095 -0.00893 N4 5 0.395486 0.955881 0.112812 11.00000 0.03569 0.04031 = 0.03366 0.00036 0.00285 -0.00687 N5 5 0.207217 0.769338 0.118492 11.00000 0.02890 0.03078 = 0.02909 -0.00057 -0.00114 0.00090 N6 5 0.121257 0.604889 0.197656 11.00000 0.02835 0.02962 = 0.03180 -0.00147 0.00024 0.00006 N7 5 0.098499 0.429679 0.386927 11.00000 0.04384 0.04679 = 0.03425 0.00142 0.00172 -0.01068 N8 5 0.163949 0.439988 0.440725 11.00000 0.04635 0.03880 = 0.03387 0.00091 -0.00087 -0.00543 N9 5 0.225233 0.510171 0.415452 11.00000 0.04398 0.03882 = 0.03434 0.00207 -0.00092 -0.00361 N10 5 0.199318 0.549113 0.340160 11.00000 0.03238 0.03540 = 0.03264 0.00225 -0.00089 -0.00124 C1 1 0.333074 0.880435 0.131966 11.00000 0.03298 0.03212 = 0.03157 0.00126 0.00271 -0.00051 C2 1 0.259706 0.845341 0.079661 11.00000 0.03241 0.03282 = 0.03282 0.00159 0.00200 0.00061 C3 1 0.245735 0.882406 -0.002137 11.00000 0.04397 0.05346 = 0.03306 0.00629 0.00400 -0.00625 AFIX 43 H3 2 0.283905 0.935232 -0.027885 11.00000 -1.20000 AFIX 0 C4 1 0.174538 0.840031 -0.044944 11.00000 0.04824 0.06368 = 0.03032 0.00853 -0.00335 -0.00289 AFIX 43 H4 2 0.163420 0.863531 -0.100676 11.00000 -1.20000 AFIX 0 C5 1 0.119595 0.762753 -0.005380 11.00000 0.04104 0.05187 = 0.03286 0.00072 -0.00749 -0.00270 AFIX 43 H5 2 0.070361 0.733876 -0.033548 11.00000 -1.20000 AFIX 0 C6 1 0.138167 0.728279 0.076741 11.00000 0.02943 0.03451 = 0.03067 -0.00172 -0.00281 0.00134 C7 1 0.086330 0.640799 0.124224 11.00000 0.02960 0.03269 = 0.03158 -0.00284 -0.00248 0.00116 C8 1 0.006939 0.599027 0.096856 11.00000 0.03659 0.04889 = 0.03920 0.00057 -0.00781 -0.00442 AFIX 43 H8 2 -0.016899 0.625306 0.045192 11.00000 -1.20000 AFIX 0 C9 1 -0.036115 0.518373 0.146923 11.00000 0.03344 0.05122 = 0.05002 -0.00109 -0.00812 -0.01029 AFIX 43 H9 2 -0.089489 0.488744 0.129290 11.00000 -1.20000 AFIX 0 C10 1 -0.000532 0.481565 0.222751 11.00000 0.03378 0.04229 = 0.04778 0.00097 -0.00126 -0.00774 AFIX 43 H10 2 -0.028962 0.427289 0.257875 11.00000 -1.20000 AFIX 0 C11 1 0.078262 0.526986 0.245497 11.00000 0.02880 0.03297 = 0.03625 -0.00318 0.00171 -0.00089 C12 1 0.123201 0.498742 0.324315 11.00000 0.03242 0.03180 = 0.03326 -0.00079 0.00357 -0.00268 part 1 10.5 C13 1 0.523285 1.024813 0.197550 10.50000 0.03374 0.04552 = 0.05133 -0.00746 0.00621 -0.01310 C14 1 0.515569 1.107245 0.273248 10.50000 0.05248 0.07152 = 0.05680 -0.01931 0.00621 -0.02550 AFIX 137 H14A 2 0.565663 1.158221 0.281598 10.50000 -1.50000 H14B 2 0.508859 1.054504 0.321679 10.50000 -1.50000 H14C 2 0.467228 1.161960 0.265094 10.50000 -1.50000 AFIX 0 C15 1 0.534088 1.111418 0.122270 10.50000 0.07091 0.10366 = 0.05938 0.01653 -0.00577 -0.05334 AFIX 137 H15A 2 0.588693 1.151335 0.127115 10.50000 -1.50000 H15B 2 0.490882 1.175747 0.120564 10.50000 -1.50000 H15C 2 0.529507 1.061815 0.071635 10.50000 -1.50000 AFIX 0 C16 1 0.591563 0.934813 0.208695 10.50000 0.04667 0.07770 = 0.12421 -0.01381 0.00460 0.00290 AFIX 137 H16A 2 0.642564 0.979168 0.225980 10.50000 -1.50000 H16B 2 0.599449 0.891468 0.156634 10.50000 -1.50000 H16C 2 0.578223 0.873765 0.250906 10.50000 -1.50000 AFIX 0 part 2 10.5 C13A 1 0.523285 1.024813 0.197550 10.50000 0.03374 0.04552 = 0.05133 -0.00746 0.00621 -0.01310 C14A 1 0.503578 1.139494 0.242410 10.50000 0.04630 0.05522 = 0.08421 -0.02499 0.01347 -0.01410 AFIX 137 H14D 2 0.554860 1.184961 0.257045 10.50000 -1.50000 H14E 2 0.475829 1.117555 0.292594 10.50000 -1.50000 H14F 2 0.466921 1.192354 0.207471 10.50000 -1.50000 AFIX 0 C15A 1 0.558942 1.045924 0.113682 10.50000 0.04861 0.07827 = 0.06497 -0.00829 0.01879 -0.02483 AFIX 137 H15D 2 0.612271 1.089171 0.120840 10.50000 -1.50000 H15E 2 0.520449 1.096974 0.079481 10.50000 -1.50000 H15F 2 0.567019 0.965194 0.086833 10.50000 -1.50000 AFIX 0 C16A 1 0.584784 0.936520 0.249654 10.50000 0.04580 0.06402 = 0.07464 -0.00134 -0.01488 -0.01412 AFIX 137 H16D 2 0.639687 0.975442 0.254886 10.50000 -1.50000 H16E 2 0.588871 0.855748 0.221795 10.50000 -1.50000 H16F 2 0.563798 0.923806 0.304480 10.50000 -1.50000 AFIX 0 part 0 C17 1 0.167945 0.374976 0.523399 11.00000 0.07145 0.06625 = 0.03533 0.00922 -0.00392 -0.02001 C18 1 0.171841 0.232222 0.505729 11.00000 0.15272 0.06777 = 0.08857 0.03100 0.01135 -0.00043 AFIX 137 H18A 2 0.116929 0.202565 0.486239 11.00000 -1.50000 H18B 2 0.189357 0.187829 0.556320 11.00000 -1.50000 H18C 2 0.211688 0.216400 0.463502 11.00000 -1.50000 AFIX 0 C19 1 0.095605 0.411124 0.567774 11.00000 0.15144 0.26006 = 0.07101 0.07842 0.06659 0.12966 AFIX 137 H19A 2 0.096532 0.501561 0.577176 11.00000 -1.50000 H19B 2 0.096495 0.367539 0.620763 11.00000 -1.50000 H19C 2 0.045135 0.388582 0.535227 11.00000 -1.50000 AFIX 0 C20 1 0.252679 0.404707 0.567157 11.00000 0.09456 0.11207 = 0.05683 0.02018 -0.01640 0.00053 AFIX 137 H20A 2 0.297037 0.385813 0.530187 11.00000 -1.50000 H20B 2 0.259919 0.353760 0.617032 11.00000 -1.50000 H20C 2 0.254849 0.493416 0.582021 11.00000 -1.50000 AFIX 0 O9 6 0.084728 0.251771 0.065985 11.00000 0.06404 0.07210 = 0.05749 -0.00320 -0.01693 0.00670 AFIX 147 H9A 2 0.121027 0.271000 0.102429 11.00000 -1.50000 AFIX 0 C21 1 0.099992 0.130586 0.037319 11.00000 0.07104 0.07952 = 0.08135 -0.01377 0.00419 -0.00135 AFIX 137 H21A 2 0.056183 0.106676 -0.003491 11.00000 -1.50000 H21B 2 0.100763 0.071829 0.083529 11.00000 -1.50000 H21C 2 0.153682 0.128694 0.011915 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1_a.res in P2/n REM R1 = 0.0570 for 4085 Fo > 4sig(Fo) and 0.0839 for all 5606 data REM 422 parameters refined using 414 restraints END WGHT 0.0613 3.0036 REM Highest difference peak 0.550, deepest hole -0.564, 1-sigma level 0.063 Q1 1 0.1353 0.5344 0.5775 11.00000 0.05 0.55 Q2 1 0.2245 0.3058 0.5434 11.00000 0.05 0.47 Q3 1 0.2085 0.0965 0.2248 11.00000 0.05 0.46 Q4 1 0.1888 0.4895 0.5856 11.00000 0.05 0.42 Q5 1 0.2429 0.2521 0.3262 11.00000 0.05 0.40 Q6 1 0.0572 0.3205 0.5252 11.00000 0.05 0.34 Q7 1 0.0396 0.3571 0.5378 11.00000 0.05 0.33 Q8 1 0.0734 0.2938 0.5201 11.00000 0.05 0.33 Q9 1 0.5815 0.9576 0.1449 11.00000 0.05 0.32 Q10 1 0.2190 0.1380 0.3106 11.00000 0.05 0.30 Q11 1 0.4819 0.9937 0.1941 11.00000 0.05 0.28 Q12 1 0.5441 0.9860 0.3273 11.00000 0.05 0.25 Q13 1 0.7549 1.3419 0.3356 11.00000 0.05 0.24 Q14 1 0.8205 1.3610 0.2986 11.00000 0.05 0.24 Q15 1 0.1955 0.6308 0.3153 11.00000 0.05 0.24 Q16 1 0.3258 0.1748 0.2470 11.00000 0.05 0.23 Q17 1 0.7785 1.2095 0.3182 11.00000 0.05 0.22 Q18 1 0.1640 0.0982 0.0625 11.00000 0.05 0.22 Q19 1 0.3048 0.7209 0.1981 11.00000 0.05 0.22 Q20 1 0.2988 0.7975 0.2310 11.00000 0.05 0.21 ; _shelx_res_checksum 68335 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' 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 Cl1_1 Cl 0.2493(5) 0.21095(14) 0.2510(5) 0.0449(4) Uani 0.5 1 d D U P A -1 O1_1 O 0.2052(6) 0.2942(8) 0.1958(6) 0.084(3) Uani 0.5 1 d D U P A -1 O2_1 O 0.2033(6) 0.1951(10) 0.3207(5) 0.134(4) Uani 0.5 1 d D U P A -1 O3_1 O 0.3239(6) 0.2669(11) 0.2751(8) 0.140(5) Uani 0.5 1 d D U P A -1 O4_1 O 0.2571(10) 0.0982(7) 0.2144(6) 0.195(6) Uani 0.5 1 d D U P A -1 Cl2_2 Cl 0.7605(3) 1.29411(15) 0.2619(3) 0.0455(8) Uani 0.5 1 d D U P B -1 O5_2 O 0.6837(7) 1.3534(19) 0.2714(8) 0.087(4) Uani 0.5 1 d D U P B -1 O6_2 O 0.7478(16) 1.1628(4) 0.2480(14) 0.0767(16) Uani 0.5 1 d D U P B -1 O7_2 O 0.8093(4) 1.3075(7) 0.3385(4) 0.103(2) Uani 0.5 1 d D U P B -1 O8_2 O 0.8065(9) 1.3461(18) 0.1999(8) 0.096(4) Uani 0.5 1 d D U P B -1 Fe1 Fe 0.250000 0.68901(5) 0.250000 0.02841(18) Uani 1 2 d S T P . . N1 N 0.34272(15) 0.8338(2) 0.20923(16) 0.0347(6) Uani 1 1 d . . . . . N2 N 0.41353(16) 0.8808(3) 0.24198(17) 0.0390(6) Uani 1 1 d . . . . . N3 N 0.44317(15) 0.9524(2) 0.18299(16) 0.0356(6) Uani 1 1 d . . . . . N4 N 0.39549(16) 0.9559(2) 0.11281(16) 0.0365(6) Uani 1 1 d . . . . . N5 N 0.20722(14) 0.7693(2) 0.11849(14) 0.0297(5) Uani 1 1 d . . . . . N6 N 0.12126(14) 0.6049(2) 0.19766(15) 0.0300(5) Uani 1 1 d . . . . . N7 N 0.09850(17) 0.4297(3) 0.38693(16) 0.0416(6) Uani 1 1 d . . . . . N8 N 0.16395(17) 0.4400(2) 0.44072(16) 0.0398(6) Uani 1 1 d . . . . . N9 N 0.22523(16) 0.5102(3) 0.41545(16) 0.0391(6) Uani 1 1 d . . . . . N10 N 0.19932(15) 0.5491(2) 0.34016(15) 0.0336(6) Uani 1 1 d . . . . . C1 C 0.33307(18) 0.8804(3) 0.13197(18) 0.0322(6) Uani 1 1 d . . . . . C2 C 0.25971(18) 0.8453(3) 0.07966(18) 0.0327(6) Uani 1 1 d . . . . . C3 C 0.2457(2) 0.8824(3) -0.0021(2) 0.0434(8) Uani 1 1 d . . . . . H3 H 0.283905 0.935232 -0.027885 0.052 Uiso 1 1 calc R U . . . C4 C 0.1745(2) 0.8400(4) -0.0449(2) 0.0476(8) Uani 1 1 d . . . . . H4 H 0.163420 0.863531 -0.100676 0.057 Uiso 1 1 calc R U . . . C5 C 0.1196(2) 0.7628(3) -0.0054(2) 0.0422(8) Uani 1 1 d . . . . . H5 H 0.070361 0.733876 -0.033548 0.051 Uiso 1 1 calc R U . . . C6 C 0.13817(18) 0.7283(3) 0.07674(18) 0.0317(6) Uani 1 1 d . . . . . C7 C 0.08633(18) 0.6408(3) 0.12422(18) 0.0314(6) Uani 1 1 d . . . . . C8 C 0.00694(19) 0.5990(3) 0.0969(2) 0.0419(8) Uani 1 1 d . . . . . H8 H -0.016899 0.625306 0.045192 0.050 Uiso 1 1 calc R U . . . C9 C -0.0361(2) 0.5184(3) 0.1469(2) 0.0452(8) Uani 1 1 d . . . . . H9 H -0.089489 0.488744 0.129290 0.054 Uiso 1 1 calc R U . . . C10 C -0.00053(19) 0.4816(3) 0.2228(2) 0.0414(8) Uani 1 1 d . . . . . H10 H -0.028962 0.427289 0.257875 0.050 Uiso 1 1 calc R U . . . C11 C 0.07826(18) 0.5270(3) 0.24550(19) 0.0327(7) Uani 1 1 d . . . . . C12 C 0.12320(18) 0.4987(3) 0.32431(18) 0.0324(6) Uani 1 1 d . . . . . C13 C 0.5233(2) 1.0248(3) 0.1976(2) 0.0434(8) Uani 0.5 1 d . U P C 1 C14 C 0.5156(10) 1.1072(13) 0.2732(7) 0.060(3) Uani 0.5 1 d . U P C 1 H14A H 0.565663 1.158221 0.281598 0.090 Uiso 0.5 1 calc R U P C 1 H14B H 0.508859 1.054504 0.321679 0.090 Uiso 0.5 1 calc R U P C 1 H14C H 0.467228 1.161960 0.265094 0.090 Uiso 0.5 1 calc R U P C 1 C15 C 0.5341(7) 1.1114(12) 0.1223(7) 0.078(3) Uani 0.5 1 d . U P C 1 H15A H 0.588693 1.151335 0.127115 0.117 Uiso 0.5 1 calc R U P C 1 H15B H 0.490882 1.175747 0.120564 0.117 Uiso 0.5 1 calc R U P C 1 H15C H 0.529507 1.061815 0.071635 0.117 Uiso 0.5 1 calc R U P C 1 C16 C 0.5916(9) 0.9348(14) 0.2087(8) 0.083(3) Uani 0.5 1 d . U P C 1 H16A H 0.642564 0.979168 0.225980 0.124 Uiso 0.5 1 calc R U P C 1 H16B H 0.599449 0.891468 0.156634 0.124 Uiso 0.5 1 calc R U P C 1 H16C H 0.578223 0.873765 0.250906 0.124 Uiso 0.5 1 calc R U P C 1 C13A C 0.5233(2) 1.0248(3) 0.1976(2) 0.0434(8) Uani 0.5 1 d . U P C 2 C14A C 0.5036(9) 1.1395(13) 0.2424(7) 0.062(3) Uani 0.5 1 d . U P C 2 H14D H 0.554860 1.184961 0.257045 0.092 Uiso 0.5 1 calc R U P C 2 H14E H 0.475829 1.117555 0.292594 0.092 Uiso 0.5 1 calc R U P C 2 H14F H 0.466921 1.192354 0.207471 0.092 Uiso 0.5 1 calc R U P C 2 C15A C 0.5589(7) 1.0459(10) 0.1137(7) 0.063(2) Uani 0.5 1 d . U P C 2 H15D H 0.612271 1.089171 0.120840 0.095 Uiso 0.5 1 calc R U P C 2 H15E H 0.520449 1.096974 0.079481 0.095 Uiso 0.5 1 calc R U P C 2 H15F H 0.567019 0.965194 0.086833 0.095 Uiso 0.5 1 calc R U P C 2 C16A C 0.5848(8) 0.9365(12) 0.2497(6) 0.062(3) Uani 0.5 1 d . U P C 2 H16D H 0.639687 0.975442 0.254886 0.093 Uiso 0.5 1 calc R U P C 2 H16E H 0.588871 0.855748 0.221795 0.093 Uiso 0.5 1 calc R U P C 2 H16F H 0.563798 0.923806 0.304480 0.093 Uiso 0.5 1 calc R U P C 2 C17 C 0.1679(3) 0.3750(4) 0.5234(2) 0.0579(10) Uani 1 1 d . . . . . C18 C 0.1718(4) 0.2322(5) 0.5057(4) 0.1028(19) Uani 1 1 d . . . . . H18A H 0.116929 0.202565 0.486239 0.154 Uiso 1 1 calc R U . . . H18B H 0.189357 0.187829 0.556320 0.154 Uiso 1 1 calc R U . . . H18C H 0.211688 0.216400 0.463502 0.154 Uiso 1 1 calc R U . . . C19 C 0.0956(4) 0.4111(8) 0.5678(4) 0.159(4) Uani 1 1 d . . . . . H19A H 0.096532 0.501561 0.577176 0.238 Uiso 1 1 calc R U . . . H19B H 0.096495 0.367539 0.620763 0.238 Uiso 1 1 calc R U . . . H19C H 0.045135 0.388582 0.535227 0.238 Uiso 1 1 calc R U . . . C20 C 0.2527(3) 0.4047(6) 0.5672(3) 0.0885(16) Uani 1 1 d . . . . . H20A H 0.297037 0.385813 0.530187 0.133 Uiso 1 1 calc R U . . . H20B H 0.259919 0.353760 0.617032 0.133 Uiso 1 1 calc R U . . . H20C H 0.254849 0.493416 0.582021 0.133 Uiso 1 1 calc R U . . . O9 O 0.08473(18) 0.2518(3) 0.06598(18) 0.0652(8) Uani 1 1 d . . . . . H9A H 0.121027 0.271000 0.102429 0.098 Uiso 1 1 calc R U . . . C21 C 0.1000(3) 0.1306(5) 0.0373(3) 0.0773(13) Uani 1 1 d . . . . . H21A H 0.056183 0.106676 -0.003491 0.116 Uiso 1 1 calc R U . . . H21B H 0.100763 0.071829 0.083529 0.116 Uiso 1 1 calc R U . . . H21C H 0.153682 0.128694 0.011915 0.116 Uiso 1 1 calc R U . . . 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 Cl1_1 0.0458(8) 0.0426(8) 0.0463(8) 0.015(3) 0.0017(6) 0.014(3) O1_1 0.107(7) 0.049(3) 0.089(6) 0.026(4) -0.067(5) -0.009(4) O2_1 0.108(6) 0.198(10) 0.102(6) 0.051(7) 0.055(5) -0.005(7) O3_1 0.056(5) 0.171(11) 0.188(13) 0.118(9) -0.048(5) -0.050(7) O4_1 0.346(16) 0.064(5) 0.174(13) -0.040(6) -0.008(13) 0.089(8) Cl2_2 0.034(2) 0.0471(8) 0.056(3) -0.0039(10) 0.0082(14) 0.0031(9) O5_2 0.034(3) 0.098(7) 0.129(9) -0.008(7) 0.008(4) 0.031(4) O6_2 0.070(3) 0.047(2) 0.116(4) -0.015(8) 0.026(3) -0.017(6) O7_2 0.099(5) 0.116(6) 0.089(5) -0.030(4) -0.036(4) 0.027(4) O8_2 0.103(8) 0.077(7) 0.114(7) 0.030(7) 0.055(6) -0.007(6) Fe1 0.0256(3) 0.0296(3) 0.0298(3) 0.000 -0.0016(2) 0.000 N1 0.0322(13) 0.0352(14) 0.0363(14) 0.0018(11) -0.0018(11) -0.0041(10) N2 0.0357(14) 0.0404(16) 0.0407(15) 0.0025(12) -0.0011(11) -0.0078(11) N3 0.0313(13) 0.0395(15) 0.0359(14) -0.0018(12) 0.0010(11) -0.0089(11) N4 0.0357(14) 0.0403(15) 0.0337(14) 0.0004(11) 0.0029(11) -0.0069(11) N5 0.0289(12) 0.0308(13) 0.0291(13) -0.0006(10) -0.0011(10) 0.0009(10) N6 0.0283(12) 0.0296(13) 0.0318(13) -0.0015(10) 0.0002(10) 0.0001(10) N7 0.0438(16) 0.0468(16) 0.0342(15) 0.0014(12) 0.0017(12) -0.0107(12) N8 0.0463(16) 0.0388(15) 0.0339(14) 0.0009(12) -0.0009(12) -0.0054(12) N9 0.0440(15) 0.0388(15) 0.0343(14) 0.0021(12) -0.0009(12) -0.0036(12) N10 0.0324(13) 0.0354(14) 0.0326(14) 0.0022(11) -0.0009(10) -0.0012(10) C1 0.0330(15) 0.0321(16) 0.0316(16) 0.0013(12) 0.0027(12) -0.0005(12) C2 0.0324(15) 0.0328(16) 0.0328(16) 0.0016(13) 0.0020(12) 0.0006(12) C3 0.0440(18) 0.053(2) 0.0331(17) 0.0063(15) 0.0040(14) -0.0063(15) C4 0.048(2) 0.064(2) 0.0303(17) 0.0085(16) -0.0033(14) -0.0029(17) C5 0.0410(18) 0.052(2) 0.0329(17) 0.0007(15) -0.0075(14) -0.0027(15) C6 0.0294(15) 0.0345(16) 0.0307(15) -0.0017(12) -0.0028(12) 0.0013(12) C7 0.0296(15) 0.0327(15) 0.0316(15) -0.0028(12) -0.0025(12) 0.0012(12) C8 0.0366(17) 0.0489(19) 0.0392(18) 0.0006(15) -0.0078(14) -0.0044(14) C9 0.0334(17) 0.051(2) 0.050(2) -0.0011(16) -0.0081(15) -0.0103(14) C10 0.0338(17) 0.0423(19) 0.048(2) 0.0010(15) -0.0013(14) -0.0077(13) C11 0.0288(15) 0.0330(16) 0.0362(16) -0.0032(13) 0.0017(12) -0.0009(11) C12 0.0324(16) 0.0318(15) 0.0333(16) -0.0008(13) 0.0036(12) -0.0027(12) C13 0.0337(16) 0.0455(18) 0.0513(19) -0.0075(15) 0.0062(14) -0.0131(13) C14 0.052(6) 0.072(7) 0.057(5) -0.019(5) 0.006(5) -0.026(5) C15 0.071(7) 0.104(8) 0.059(5) 0.017(5) -0.006(5) -0.053(5) C16 0.047(5) 0.078(6) 0.124(8) -0.014(6) 0.005(7) 0.003(4) C13A 0.0337(16) 0.0455(18) 0.0513(19) -0.0075(15) 0.0062(14) -0.0131(13) C14A 0.046(5) 0.055(6) 0.084(8) -0.025(5) 0.013(6) -0.014(4) C15A 0.049(5) 0.078(6) 0.065(4) -0.008(4) 0.019(4) -0.025(4) C16A 0.046(5) 0.064(5) 0.075(6) -0.001(5) -0.015(5) -0.014(4) C17 0.071(3) 0.066(3) 0.0353(19) 0.0092(18) -0.0039(17) -0.020(2) C18 0.153(6) 0.068(3) 0.089(4) 0.031(3) 0.011(4) 0.000(3) C19 0.151(6) 0.260(9) 0.071(4) 0.078(5) 0.067(4) 0.130(6) C20 0.095(4) 0.112(4) 0.057(3) 0.020(3) -0.016(3) 0.001(3) O9 0.0640(18) 0.0721(19) 0.0575(18) -0.0032(15) -0.0169(14) 0.0067(15) C21 0.071(3) 0.080(3) 0.081(3) -0.014(3) 0.004(2) -0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4_1 Cl1_1 O3_1 114.2(8) . . ? O4_1 Cl1_1 O2_1 108.3(8) . . ? O3_1 Cl1_1 O2_1 108.3(8) . . ? O4_1 Cl1_1 O1_1 109.5(7) . . ? O3_1 Cl1_1 O1_1 107.9(5) . . ? O2_1 Cl1_1 O1_1 108.5(7) . . ? O8_2 Cl2_2 O5_2 113.7(6) . . ? O8_2 Cl2_2 O6_2 110.6(9) . . ? O5_2 Cl2_2 O6_2 109.8(9) . . ? O8_2 Cl2_2 O7_2 107.1(6) . . ? O5_2 Cl2_2 O7_2 107.8(6) . . ? O6_2 Cl2_2 O7_2 107.5(8) . . ? N1 Fe1 N1 94.25(13) 2 . ? N1 Fe1 N10 153.93(9) 2 2 ? N1 Fe1 N10 89.79(9) . 2 ? N1 Fe1 N10 89.79(9) 2 . ? N1 Fe1 N10 153.93(9) . . ? N10 Fe1 N10 97.79(13) 2 . ? N1 Fe1 N5 81.40(9) 2 . ? N1 Fe1 N5 69.96(9) . . ? N10 Fe1 N5 75.84(9) 2 . ? N10 Fe1 N5 136.08(9) . . ? N1 Fe1 N5 69.96(9) 2 2 ? N1 Fe1 N5 81.40(9) . 2 ? N10 Fe1 N5 136.08(9) 2 2 ? N10 Fe1 N5 75.84(9) . 2 ? N5 Fe1 N5 137.59(12) . 2 ? N1 Fe1 N6 77.64(9) 2 . ? N1 Fe1 N6 136.70(9) . . ? N10 Fe1 N6 81.79(8) 2 . ? N10 Fe1 N6 69.29(9) . . ? N5 Fe1 N6 66.79(8) . . ? N5 Fe1 N6 131.85(8) 2 . ? N1 Fe1 N6 136.70(9) 2 2 ? N1 Fe1 N6 77.64(9) . 2 ? N10 Fe1 N6 69.29(9) 2 2 ? N10 Fe1 N6 81.79(8) . 2 ? N5 Fe1 N6 131.85(8) . 2 ? N5 Fe1 N6 66.79(8) 2 2 ? N6 Fe1 N6 135.63(12) . 2 ? N2 N1 C1 106.7(2) . . ? N2 N1 Fe1 134.7(2) . . ? C1 N1 Fe1 118.34(19) . . ? N3 N2 N1 105.1(2) . . ? N2 N3 N4 114.5(2) . . ? N2 N3 C13A 121.0(3) . . ? N4 N3 C13A 124.4(3) . . ? N2 N3 C13 121.0(3) . . ? N4 N3 C13 124.4(3) . . ? C1 N4 N3 101.0(2) . . ? C6 N5 C2 118.8(3) . . ? C6 N5 Fe1 122.06(19) . . ? C2 N5 Fe1 118.48(19) . . ? C7 N6 C11 118.6(2) . . ? C7 N6 Fe1 121.77(19) . . ? C11 N6 Fe1 119.35(19) . . ? C12 N7 N8 101.3(2) . . ? N9 N8 N7 114.9(3) . . ? N9 N8 C17 122.5(3) . . ? N7 N8 C17 122.6(3) . . ? N8 N9 N10 104.8(2) . . ? N9 N10 C12 106.8(2) . . ? N9 N10 Fe1 133.4(2) . . ? C12 N10 Fe1 119.4(2) . . ? N4 C1 N1 112.6(3) . . ? N4 C1 C2 127.7(3) . . ? N1 C1 C2 119.6(3) . . ? N5 C2 C3 122.7(3) . . ? N5 C2 C1 112.8(3) . . ? C3 C2 C1 124.4(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N5 C6 C5 121.7(3) . . ? N5 C6 C7 114.4(3) . . ? C5 C6 C7 123.9(3) . . ? N6 C7 C8 121.5(3) . . ? N6 C7 C6 114.5(2) . . ? C8 C7 C6 124.0(3) . . ? C9 C8 C7 118.9(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 117.9(3) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? N6 C11 C10 123.3(3) . . ? N6 C11 C12 112.4(2) . . ? C10 C11 C12 124.2(3) . . ? N7 C12 N10 112.2(3) . . ? N7 C12 C11 128.6(3) . . ? N10 C12 C11 119.1(3) . . ? C16 C13 N3 108.3(7) . . ? C16 C13 C14 111.8(8) . . ? N3 C13 C14 108.5(6) . . ? C16 C13 C15 112.0(8) . . ? N3 C13 C15 108.1(5) . . ? C14 C13 C15 108.0(7) . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14A C13A N3 107.4(7) . . ? C14A C13A C15A 114.9(7) . . ? N3 C13A C15A 107.1(5) . . ? C14A C13A C16A 112.2(7) . . ? N3 C13A C16A 106.6(5) . . ? C15A C13A C16A 108.2(6) . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C13A C15A H15D 109.5 . . ? C13A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C13A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C13A C16A H16D 109.5 . . ? C13A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C13A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C19 C17 N8 108.6(4) . . ? C19 C17 C20 115.6(5) . . ? N8 C17 C20 108.2(3) . . ? C19 C17 C18 113.2(5) . . ? N8 C17 C18 106.7(3) . . ? C20 C17 C18 104.1(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O9 H9A 109.5 . . ? O9 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O9 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1_1 O4_1 1.340(7) . ? Cl1_1 O3_1 1.371(9) . ? Cl1_1 O2_1 1.383(10) . ? Cl1_1 O1_1 1.414(7) . ? Cl2_2 O8_2 1.385(10) . ? Cl2_2 O5_2 1.395(8) . ? Cl2_2 O6_2 1.422(5) . ? Cl2_2 O7_2 1.432(7) . ? Fe1 N1 2.254(2) 2 ? Fe1 N1 2.254(2) . ? Fe1 N10 2.254(2) 2 ? Fe1 N10 2.254(2) . ? Fe1 N5 2.353(2) . ? Fe1 N5 2.353(2) 2 ? Fe1 N6 2.360(2) . ? Fe1 N6 2.360(2) 2 ? N1 N2 1.323(3) . ? N1 C1 1.341(4) . ? N2 N3 1.322(3) . ? N3 N4 1.332(4) . ? N3 C13A 1.502(4) . ? N3 C13 1.502(4) . ? N4 C1 1.327(4) . ? N5 C6 1.337(4) . ? N5 C2 1.341(4) . ? N6 C7 1.338(4) . ? N6 C11 1.342(4) . ? N7 C12 1.323(4) . ? N7 N8 1.329(4) . ? N8 N9 1.311(4) . ? N8 C17 1.498(4) . ? N9 N10 1.328(4) . ? N10 C12 1.342(4) . ? C1 C2 1.458(4) . ? C2 C3 1.382(4) . ? C3 C4 1.376(5) . ? C3 H3 0.9400 . ? C4 C5 1.380(5) . ? C4 H4 0.9400 . ? C5 C6 1.390(4) . ? C5 H5 0.9400 . ? C6 C7 1.482(4) . ? C7 C8 1.395(4) . ? C8 C9 1.382(5) . ? C8 H8 0.9400 . ? C9 C10 1.378(5) . ? C9 H9 0.9400 . ? C10 C11 1.381(4) . ? C10 H10 0.9400 . ? C11 C12 1.458(4) . ? C13 C16 1.454(14) . ? C13 C14 1.510(13) . ? C13 C15 1.537(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C13A C14A 1.456(13) . ? C13A C15A 1.510(11) . ? C13A C16A 1.570(12) . ? C14A H14D 0.9700 . ? C14A H14E 0.9700 . ? C14A H14F 0.9700 . ? C15A H15D 0.9700 . ? C15A H15E 0.9700 . ? C15A H15F 0.9700 . ? C16A H16D 0.9700 . ? C16A H16E 0.9700 . ? C16A H16F 0.9700 . ? C17 C19 1.442(6) . ? C17 C20 1.529(6) . ? C17 C18 1.541(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? O9 C21 1.390(5) . ? O9 H9A 0.8300 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 _geom_torsion_publ_flag C1 N1 N2 N3 -0.4(3) . . . . ? Fe1 N1 N2 N3 173.0(2) . . . . ? N1 N2 N3 N4 0.3(3) . . . . ? N1 N2 N3 C13A 178.8(3) . . . . ? N1 N2 N3 C13 178.8(3) . . . . ? N2 N3 N4 C1 -0.1(3) . . . . ? C13A N3 N4 C1 -178.5(3) . . . . ? C13 N3 N4 C1 -178.5(3) . . . . ? C12 N7 N8 N9 0.4(3) . . . . ? C12 N7 N8 C17 -178.7(3) . . . . ? N7 N8 N9 N10 -0.1(3) . . . . ? C17 N8 N9 N10 179.1(3) . . . . ? N8 N9 N10 C12 -0.3(3) . . . . ? N8 N9 N10 Fe1 172.0(2) . . . . ? N3 N4 C1 N1 -0.2(3) . . . . ? N3 N4 C1 C2 -179.8(3) . . . . ? N2 N1 C1 N4 0.4(3) . . . . ? Fe1 N1 C1 N4 -174.29(19) . . . . ? N2 N1 C1 C2 -179.9(3) . . . . ? Fe1 N1 C1 C2 5.4(4) . . . . ? C6 N5 C2 C3 -0.5(4) . . . . ? Fe1 N5 C2 C3 170.4(2) . . . . ? C6 N5 C2 C1 -178.7(3) . . . . ? Fe1 N5 C2 C1 -7.9(3) . . . . ? N4 C1 C2 N5 -178.6(3) . . . . ? N1 C1 C2 N5 1.8(4) . . . . ? N4 C1 C2 C3 3.2(5) . . . . ? N1 C1 C2 C3 -176.4(3) . . . . ? N5 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 C4 178.6(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C2 N5 C6 C5 -0.2(4) . . . . ? Fe1 N5 C6 C5 -170.8(2) . . . . ? C2 N5 C6 C7 177.6(3) . . . . ? Fe1 N5 C6 C7 7.1(3) . . . . ? C4 C5 C6 N5 0.9(5) . . . . ? C4 C5 C6 C7 -176.8(3) . . . . ? C11 N6 C7 C8 -0.1(4) . . . . ? Fe1 N6 C7 C8 -174.4(2) . . . . ? C11 N6 C7 C6 179.1(2) . . . . ? Fe1 N6 C7 C6 4.7(3) . . . . ? N5 C6 C7 N6 -7.4(4) . . . . ? C5 C6 C7 N6 170.4(3) . . . . ? N5 C6 C7 C8 171.7(3) . . . . ? C5 C6 C7 C8 -10.5(5) . . . . ? N6 C7 C8 C9 -0.2(5) . . . . ? C6 C7 C8 C9 -179.3(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C7 N6 C11 C10 0.1(4) . . . . ? Fe1 N6 C11 C10 174.6(2) . . . . ? C7 N6 C11 C12 -178.5(3) . . . . ? Fe1 N6 C11 C12 -4.0(3) . . . . ? C9 C10 C11 N6 0.2(5) . . . . ? C9 C10 C11 C12 178.6(3) . . . . ? N8 N7 C12 N10 -0.7(3) . . . . ? N8 N7 C12 C11 -179.0(3) . . . . ? N9 N10 C12 N7 0.7(4) . . . . ? Fe1 N10 C12 N7 -173.0(2) . . . . ? N9 N10 C12 C11 179.1(3) . . . . ? Fe1 N10 C12 C11 5.5(4) . . . . ? N6 C11 C12 N7 177.4(3) . . . . ? C10 C11 C12 N7 -1.2(5) . . . . ? N6 C11 C12 N10 -0.8(4) . . . . ? C10 C11 C12 N10 -179.4(3) . . . . ? N2 N3 C13 C16 65.9(7) . . . . ? N4 N3 C13 C16 -115.7(6) . . . . ? N2 N3 C13 C14 -55.6(6) . . . . ? N4 N3 C13 C14 122.7(6) . . . . ? N2 N3 C13 C15 -172.5(6) . . . . ? N4 N3 C13 C15 5.8(7) . . . . ? N2 N3 C13A C14A -81.1(6) . . . . ? N4 N3 C13A C14A 97.3(6) . . . . ? N2 N3 C13A C15A 155.0(5) . . . . ? N4 N3 C13A C15A -26.7(6) . . . . ? N2 N3 C13A C16A 39.4(6) . . . . ? N4 N3 C13A C16A -142.3(5) . . . . ? N9 N8 C17 C19 125.4(5) . . . . ? N7 N8 C17 C19 -55.5(6) . . . . ? N9 N8 C17 C20 -0.8(5) . . . . ? N7 N8 C17 C20 178.3(3) . . . . ? N9 N8 C17 C18 -112.3(4) . . . . ? N7 N8 C17 C18 66.8(5) . . . . ?