#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:25:44 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173540 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541901.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_1541901 loop_ _publ_author_name 'Aromi, Guillem' 'Beavers, Christine' 'Costa, Jos\'e S\'anchez' 'Craig, Gavin A.' 'Minguez Espallargas, Guillermo' 'Orera, Alodia' 'Roubeau, Olivier' _publ_section_title ; Snapshots of a Solid-State Transformation: Coexistence of Three Phases Trapped in One Crystal. ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C5SC04287A _journal_year 2016 _chemical_formula_moiety '(C36 H30 N10 Fe)2, (Cl O4)4' _chemical_formula_sum 'C72 H60 Cl4 Fe2 N20 O20' _chemical_formula_weight 1778.90 _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2015-12-22 deposited with the CCDC. 2016-01-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.45(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.700(3) _cell_length_b 20.035(4) _cell_length_c 24.638(5) _cell_measurement_reflns_used 4552 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 20.6 _cell_measurement_theta_min 2.30 _cell_volume 7750(3) _computing_cell_refinement 'SAINT V8.27B(Bruker, 2012)' _computing_data_collection 'Apex2 v2012.10-0 (Bruker, 2012)' _computing_data_reduction SAINT _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994) ShelXle Rev 699 (Hubschle, 2011) ; _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.694 _diffrn_measured_fraction_theta_max 0.694 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_radiation_monochromator silicon(111) _diffrn_radiation_source 'Advanced Light Source Beamline 11.3.1' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_unetI/netI 0.0475 _diffrn_reflns_laue_measured_fraction_full 0.694 _diffrn_reflns_laue_measured_fraction_max 0.694 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14414 _diffrn_reflns_point_group_measured_fraction_full 0.694 _diffrn_reflns_point_group_measured_fraction_max 0.694 _diffrn_reflns_theta_full 17.908 _diffrn_reflns_theta_max 17.908 _diffrn_reflns_theta_min 2.015 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_correction_T_min 0.5205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Sheldrick, 2012)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.525 _exptl_crystal_description block _exptl_crystal_F_000 3648 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.275 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 679 _refine_ls_number_reflns 2811 _refine_ls_number_restraints 1380 _refine_ls_restrained_S_all 0.859 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0809 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+85.7635P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1908 _refine_ls_wR_factor_ref 0.2456 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1770 _reflns_number_total 2811 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage3_Transient _cod_database_code 1541901 _shelx_shelxl_version_number 2014/7 _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 0.705 _shelx_estimated_absorpt_t_max 0.806 _shelx_res_file ; samp2b.res created by SHELXL-2014/7 TITL samp2b CELL 0.77490 15.7002 20.0353 24.6381 90.000 90.453 90.000 ZERR 4.00 0.0031 0.0040 0.0049 0.000 0.030 0.000 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Cl Fe DISP C -0.00202 0.00197 13.60 DISP H 0.00000 0.00000 0.67 DISP N -0.00306 0.00403 23.92 DISP O -0.00415 0.00737 40.17 DISP Cl 0.14076 0.18956 859.19 DISP Fe 0.20639 0.99298 4412.23 UNIT 288 240 80 80 16 8 TEMP 20 SIZE 0.5 0.4 0.3 !dark red block L.S. 20 fmap 2 PLAN 20 BOND $H CONF LIST 6 acta HTAB HTAB N1 O1 EQIV $1 -x+1, -y+2, -z+1 HTAB_2 N1_0 O2_$1 HTAB_2 N1_0 O3_$1 HTAB_3 N1_0 O2_$1 HTAB N5 O2 EQIV $2 -x, -y+2, -z+1 HTAB_4 N6_0 Cl1_$2 HTAB_4 N6_0 O2_$2 HTAB_4 N6_0 O4_$2 HTAB_5 N6_0 O2_$2 HTAB_1 N10_0 Cl1_$1 HTAB_1 N10_0 O1_$1 HTAB_1 N10_0 O2_$1 EQIV $3 x, -y+3/2, z+1/2 HTAB_6 C16_0 O3_$3 HTAB_7 C16_0 O3_$3 HTAB_7 C30_0 O4_$2 EQIV $4 x, -y+5/2, z+1/2 HTAB_4 C22_0 O3_$4 HTAB_5 C25_0 O4_$4 HTAB_1 C32_0 O4_$4 HTAB N11 O3 HTAB N15 O4 HTAB N15 Cl1_4 HTAB N15 O1_4 HTAB N15 O4_4 HTAB N15 O1_5 HTAB N16 Cl1_6 HTAB N16 O1_6 HTAB N16 Cl1_7 HTAB N16 O1_7 HTAB N20 Cl1_2 HTAB N20 O1_2 HTAB N20 O2_2 HTAB N20 Cl1_3 HTAB N20 O1_3 EQIV $5 x, -y+3/2, z-1/2 HTAB_2 C38_0 O2_$5 EQIV $6 -x+1, y-1/2, -z+1/2 HTAB_1 C47_0 O4_$6 HTAB_3 C60_0 O4_$5 HTAB C61 O3_5 EQIV $7 -x, y+1/2, -z+1/2 HTAB_6 C66_0 O3_$7 RIGU SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4 SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4 EADP Cl1_4 Cl1_5 WGHT 0.094500 85.763474 FVAR 0.03696 0.79200 0.72958 0.64477 FE1 6 0.269573 1.267005 0.645170 11.00000 0.07818 0.08579 = 0.09902 0.00338 -0.00394 -0.00564 O1 4 0.368342 1.250300 0.420779 11.00000 0.13555 0.15350 = 0.11748 0.01895 0.00719 -0.00513 O2 4 0.159757 1.416222 0.816661 11.00000 0.21009 0.09944 = 0.14149 0.00234 0.01010 0.00611 N1 3 0.335180 1.212480 0.521535 11.00000 0.07372 0.10302 = 0.10306 0.01621 -0.00932 0.00912 AFIX 43 H1A 2 0.355162 1.248722 0.507936 11.00000 -1.20000 AFIX 0 N2 3 0.303911 1.204516 0.571946 11.00000 0.08120 0.10021 = 0.09638 0.00567 -0.00680 -0.00079 N3 3 0.235953 1.165860 0.666572 11.00000 0.07026 0.08373 = 0.07544 -0.00711 0.00371 0.01092 N4 3 0.224427 1.268762 0.729028 11.00000 0.06136 0.09633 = 0.09310 -0.00683 -0.00919 -0.01218 N5 3 0.209915 1.310914 0.771646 11.00000 0.07222 0.09347 = 0.09735 -0.00520 -0.01386 -0.00206 AFIX 43 H5B 2 0.219466 1.353125 0.769932 11.00000 -1.20000 AFIX 0 N6 3 0.083532 1.286177 0.586066 11.00000 0.09007 0.07984 = 0.13146 -0.01128 -0.01934 -0.00940 AFIX 43 H6A 2 0.066311 1.245499 0.587919 11.00000 -1.20000 AFIX 0 N7 3 0.155794 1.308599 0.606767 11.00000 0.08551 0.08354 = 0.09548 -0.01159 -0.00930 -0.00674 N8 3 0.295304 1.368727 0.632195 11.00000 0.07410 0.08207 = 0.09970 -0.00462 -0.01680 -0.00183 N9 3 0.395925 1.283084 0.678603 11.00000 0.07475 0.09800 = 0.09024 0.00983 -0.00465 0.00049 N10 3 0.451295 1.249503 0.708398 11.00000 0.07571 0.10238 = 0.11676 0.01747 -0.01653 -0.00628 AFIX 43 H10A 2 0.448142 1.207903 0.716747 11.00000 -1.20000 AFIX 0 C1 1 0.375178 1.183960 0.401942 11.00000 0.16163 C2 1 0.400227 1.174061 0.346491 11.00000 0.13144 AFIX 43 H2A 2 0.416231 1.206995 0.322004 11.00000 -1.20000 AFIX 0 C3 1 0.395976 1.106456 0.336592 11.00000 0.15408 AFIX 43 H3A 2 0.408059 1.095098 0.300873 11.00000 -1.20000 AFIX 0 C4 1 0.377362 1.051923 0.369021 11.00000 0.19323 AFIX 43 H4A 2 0.377808 1.008007 0.356802 11.00000 -1.20000 AFIX 0 C5 1 0.357697 1.070599 0.422579 11.00000 0.11230 AFIX 43 H5A 2 0.345850 1.037647 0.448010 11.00000 -1.20000 AFIX 0 C6 1 0.355551 1.139081 0.438695 11.00000 0.12884 C7 1 0.328931 1.150691 0.495639 11.00000 0.10399 C8 1 0.295377 1.106550 0.529879 11.00000 0.10126 AFIX 43 H8A 2 0.283713 1.061932 0.522531 11.00000 -1.20000 AFIX 0 C9 1 0.281201 1.139240 0.578111 11.00000 0.07539 C10 1 0.245017 1.119578 0.627473 11.00000 0.09530 C11 1 0.216344 1.054273 0.639711 11.00000 0.09582 AFIX 43 H11A 2 0.221259 1.020159 0.614330 11.00000 -1.20000 AFIX 0 C12 1 0.182531 1.042560 0.687700 11.00000 0.10857 AFIX 43 H12A 2 0.162200 0.999757 0.694341 11.00000 -1.20000 AFIX 0 C13 1 0.175205 1.088347 0.728114 11.00000 0.09954 AFIX 43 H13A 2 0.152677 1.078131 0.761908 11.00000 -1.20000 AFIX 0 C14 1 0.204171 1.151593 0.714690 11.00000 0.08942 C15 1 0.201454 1.208689 0.750023 11.00000 0.08462 C16 1 0.174418 1.216266 0.802642 11.00000 0.08236 AFIX 43 H16A 2 0.155575 1.182227 0.825229 11.00000 -1.20000 AFIX 0 C17 1 0.179888 1.281503 0.815919 11.00000 0.08813 C18 1 0.158734 1.318970 0.864812 11.00000 0.08314 C19 1 0.140924 1.284405 0.909718 11.00000 0.13384 AFIX 43 H19A 2 0.144003 1.238056 0.909079 11.00000 -1.20000 AFIX 0 C30 1 0.253410 1.475971 0.598710 11.00000 0.12828 AFIX 43 H30A 2 0.210364 1.503231 0.585038 11.00000 -1.20000 AFIX 0 C20 1 0.117587 1.317041 0.957950 11.00000 0.11845 AFIX 43 H20A 2 0.110627 1.293993 0.990378 11.00000 -1.20000 AFIX 0 C21 1 0.105784 1.384145 0.954495 11.00000 0.11697 AFIX 43 H21A 2 0.087900 1.405837 0.985770 11.00000 -1.20000 AFIX 0 C22 1 0.117444 1.421990 0.910376 11.00000 0.11774 AFIX 43 H22A 2 0.108215 1.467839 0.910015 11.00000 -1.20000 AFIX 0 C23 1 0.145294 1.385674 0.863973 11.00000 0.09910 C24 1 0.393504 1.300570 0.380937 11.00000 0.17266 AFIX 33 H24A 2 0.387302 1.344277 0.396377 11.00000 -1.50000 H24B 2 0.451852 1.293594 0.371050 11.00000 -1.50000 H24C 2 0.357870 1.296826 0.349240 11.00000 -1.50000 AFIX 0 C25 1 0.132136 1.484668 0.814529 11.00000 0.22464 AFIX 33 H25A 2 0.144664 1.502988 0.779485 11.00000 -1.50000 H25B 2 0.071883 1.486781 0.820639 11.00000 -1.50000 H25C 2 0.161435 1.509894 0.842042 11.00000 -1.50000 AFIX 0 C26 1 0.041256 1.335407 0.561982 11.00000 0.11517 AFIX 43 H26A 2 -0.014155 1.332632 0.548549 11.00000 -1.20000 AFIX 0 C27 1 0.091246 1.390186 0.560013 11.00000 0.10650 AFIX 43 H27A 2 0.080443 1.430350 0.542332 11.00000 -1.20000 AFIX 0 C28 1 0.162227 1.372689 0.590395 11.00000 0.08732 C29 1 0.241310 1.406811 0.606948 11.00000 0.09182 C31 1 0.334037 1.501008 0.612350 11.00000 0.12612 AFIX 43 H31A 2 0.349338 1.544844 0.604744 11.00000 -1.20000 AFIX 0 C32 1 0.388526 1.458367 0.637103 11.00000 0.11058 AFIX 43 H32A 2 0.440991 1.474675 0.648823 11.00000 -1.20000 AFIX 0 C33 1 0.370435 1.392148 0.645856 11.00000 0.09099 C34 1 0.423910 1.344318 0.673340 11.00000 0.09124 C35 1 0.498520 1.353052 0.705096 11.00000 0.09792 AFIX 43 H35A 2 0.528885 1.392196 0.711347 11.00000 -1.20000 AFIX 0 C36 1 0.514917 1.292768 0.723736 11.00000 0.10110 AFIX 43 H36A 2 0.562612 1.281185 0.744285 11.00000 -1.20000 AFIX 0 FE2 6 0.225007 0.685540 0.347352 11.00000 0.07662 0.08962 = 0.09434 0.01277 -0.00808 0.00351 O3 4 0.328864 0.723319 0.148264 11.00000 0.15598 0.10853 = 0.12526 0.02459 -0.00465 -0.02662 O4 4 0.176932 0.864978 0.502491 11.00000 0.21043 0.08957 = 0.11415 0.00019 -0.02235 -0.03141 N11 3 0.290888 0.653657 0.232561 11.00000 0.07129 0.12029 = 0.08475 -0.00571 -0.00974 -0.01539 AFIX 43 H11B 2 0.279541 0.691972 0.218529 11.00000 -1.20000 AFIX 0 N12 3 0.273972 0.640088 0.284848 11.00000 0.05171 0.09887 = 0.09140 -0.00016 -0.00433 -0.00801 N13 3 0.250581 0.598961 0.377833 11.00000 0.07357 N14 3 0.187985 0.700029 0.423014 11.00000 0.08059 0.08716 = 0.09579 0.00387 0.00293 -0.00367 N15 3 0.162297 0.749733 0.453238 11.00000 0.07126 0.09352 = 0.09793 -0.00547 -0.00972 -0.00221 AFIX 43 H15A 2 0.151667 0.789318 0.441508 11.00000 -1.20000 AFIX 0 N16 3 0.053651 0.616296 0.322948 11.00000 0.09720 0.09839 = 0.09111 0.01883 -0.00516 -0.02110 AFIX 43 H16B 2 0.060149 0.579394 0.340323 11.00000 -1.20000 AFIX 0 N17 3 0.109945 0.665799 0.321490 11.00000 0.07191 0.07898 = 0.09302 0.00601 0.00703 0.00071 N18 3 0.198878 0.767845 0.310166 11.00000 0.08439 N19 3 0.328231 0.738240 0.363610 11.00000 0.07143 0.08984 = 0.08921 0.00388 0.00469 0.00164 N20 3 0.396301 0.733741 0.396807 11.00000 0.08463 0.11174 = 0.09910 0.00868 -0.00667 0.00594 AFIX 43 H20B 2 0.410718 0.699333 0.415617 11.00000 -1.20000 AFIX 0 C37 1 0.357230 0.668237 0.123180 11.00000 0.10087 C38 1 0.388219 0.668528 0.068604 11.00000 0.12928 AFIX 43 H38A 2 0.390808 0.708198 0.049087 11.00000 -1.20000 AFIX 0 C39 1 0.413530 0.610812 0.045893 11.00000 0.13808 AFIX 43 H39A 2 0.432653 0.612239 0.010283 11.00000 -1.20000 AFIX 0 C40 1 0.413141 0.551589 0.070874 11.00000 0.12886 AFIX 43 H40A 2 0.430888 0.512628 0.053842 11.00000 -1.20000 AFIX 0 C41 1 0.382957 0.552327 0.126678 11.00000 0.11830 AFIX 43 H41A 2 0.381550 0.512851 0.146508 11.00000 -1.20000 AFIX 0 C42 1 0.357581 0.608651 0.149305 11.00000 0.08730 C43 1 0.327301 0.603205 0.202506 11.00000 0.09383 C44 1 0.330455 0.553567 0.242256 11.00000 0.08404 AFIX 43 H44A 2 0.352545 0.511048 0.236783 11.00000 -1.20000 AFIX 0 C45 1 0.296681 0.575449 0.290744 11.00000 0.08562 C46 1 0.283916 0.555062 0.345227 11.00000 0.08673 C47 1 0.302120 0.490759 0.367548 11.00000 0.12215 AFIX 43 H47A 2 0.323010 0.456760 0.345670 11.00000 -1.20000 AFIX 0 C48 1 0.288261 0.479906 0.421939 11.00000 0.14133 AFIX 43 H48A 2 0.303904 0.439623 0.437904 11.00000 -1.20000 AFIX 0 C49 1 0.251972 0.528042 0.451632 11.00000 0.13294 AFIX 43 H49A 2 0.239517 0.519194 0.487763 11.00000 -1.20000 AFIX 0 C50 1 0.232425 0.589809 0.430981 11.00000 0.08791 C51 1 0.198788 0.643983 0.456621 11.00000 0.08346 C52 1 0.180483 0.663983 0.507285 11.00000 0.09665 AFIX 43 H52A 2 0.184704 0.637334 0.538095 11.00000 -1.20000 AFIX 0 C53 1 0.154615 0.729542 0.506957 11.00000 0.08885 C54 1 0.126661 0.776351 0.547701 11.00000 0.09404 C55 1 0.094990 0.747571 0.593892 11.00000 0.10985 AFIX 43 H55A 2 0.090218 0.701336 0.595272 11.00000 -1.20000 AFIX 0 C56 1 0.069208 0.785352 0.639649 11.00000 0.12068 AFIX 43 H56A 2 0.044294 0.766019 0.669947 11.00000 -1.20000 AFIX 0 C57 1 0.083568 0.850840 0.635731 11.00000 0.14505 AFIX 43 H57A 2 0.071492 0.877114 0.665821 11.00000 -1.20000 AFIX 0 C58 1 0.114234 0.881653 0.591444 11.00000 0.13368 AFIX 43 H58A 2 0.116345 0.927999 0.589837 11.00000 -1.20000 AFIX 0 C59 1 0.141620 0.844900 0.549799 11.00000 0.10476 C60 1 0.341341 0.785908 0.123007 11.00000 0.14606 AFIX 33 H60A 2 0.318031 0.820525 0.145365 11.00000 -1.50000 H60B 2 0.401193 0.793506 0.118259 11.00000 -1.50000 H60C 2 0.313269 0.786181 0.088251 11.00000 -1.50000 AFIX 0 C61 1 0.188977 0.933772 0.498348 11.00000 0.15458 AFIX 33 H61A 2 0.214081 0.944048 0.463942 11.00000 -1.50000 H61B 2 0.135044 0.956024 0.501190 11.00000 -1.50000 H61C 2 0.226095 0.948584 0.527060 11.00000 -1.50000 AFIX 0 C62 1 -0.013665 0.632650 0.293587 11.00000 0.12472 AFIX 43 H62A 2 -0.059349 0.604577 0.285858 11.00000 -1.20000 AFIX 0 C63 1 -0.006396 0.695014 0.276791 11.00000 0.09909 AFIX 43 H63A 2 -0.047024 0.720477 0.258536 11.00000 -1.20000 AFIX 0 C64 1 0.075685 0.714315 0.292464 11.00000 0.08416 C65 1 0.123254 0.771644 0.282451 11.00000 0.09587 C66 1 0.111170 0.825838 0.249259 11.00000 0.11287 AFIX 43 H66A 2 0.060892 0.830191 0.229362 11.00000 -1.20000 AFIX 0 C67 1 0.173302 0.873492 0.245498 11.00000 0.11244 AFIX 43 H67A 2 0.165439 0.909595 0.222267 11.00000 -1.20000 AFIX 0 C68 1 0.248729 0.868637 0.276214 11.00000 0.11028 AFIX 43 H68A 2 0.290356 0.901572 0.274447 11.00000 -1.20000 AFIX 0 C69 1 0.259131 0.813626 0.309013 11.00000 0.08462 C70 1 0.331086 0.800564 0.344447 11.00000 0.09182 C71 1 0.399531 0.836944 0.361777 11.00000 0.09974 AFIX 43 H71A 2 0.415409 0.880288 0.352905 11.00000 -1.20000 AFIX 0 C72 1 0.438098 0.792508 0.395526 11.00000 0.09678 AFIX 43 H72A 2 0.487404 0.801511 0.415372 11.00000 -1.20000 AFIX 0 RESI 1 CLO4 CL1 5 0.499590 0.911598 0.240563 11.00000 0.11762 0.13221 = 0.13890 0.02760 -0.00487 -0.01606 O1 4 0.569166 0.890951 0.275381 11.00000 0.15041 O2 4 0.448433 0.853522 0.228302 11.00000 0.15066 O3 4 0.448335 0.960259 0.268114 11.00000 0.17599 O4 4 0.532126 0.939171 0.191072 11.00000 0.15232 PART 1 RESI 2 CLO4 CL1 5 0.511717 0.643146 0.492505 41.00000 0.21643 0.27240 = 0.16575 0.05882 -0.10076 -0.12130 O1 4 0.471836 0.617246 0.443881 41.00000 0.14581 O2 4 0.488926 0.712324 0.499617 41.00000 0.12468 O3 4 0.602693 0.637744 0.487131 41.00000 0.14025 O4 4 0.482978 0.605803 0.538752 41.00000 0.11327 PART 2 RESI 3 CLO4 CL1 5 0.496457 0.633906 0.489934 -41.00000 0.07522 0.02836 = 0.05370 0.00359 0.01632 0.03439 O1 4 0.450305 0.613080 0.441960 -41.00000 0.07631 O2 4 0.560476 0.681959 0.475106 -41.00000 0.24855 O3 4 0.536974 0.576583 0.514309 -41.00000 0.18171 O4 4 0.438283 0.663180 0.528044 -41.00000 0.32165 PART 1 RESI 4 CLO4 CL1 5 0.018765 0.875450 0.395212 21.00000 0.12488 0.12255 = 0.10829 -0.00204 -0.00044 -0.00557 O1 4 0.109613 0.873935 0.387436 21.00000 0.13366 O2 4 -0.024588 0.851477 0.347162 21.00000 0.14050 O3 4 -0.008044 0.943038 0.406122 21.00000 0.13893 O4 4 -0.003693 0.833722 0.440668 21.00000 0.12581 PART 2 RESI 5 CLO4 CL1 5 0.018094 0.888563 0.384479 -21.00000 0.12488 0.12255 = 0.10829 -0.00204 -0.00044 -0.00557 O1 4 0.101246 0.858177 0.382304 -21.00000 0.04938 O2 4 -0.046438 0.837865 0.378261 -21.00000 0.18614 O3 4 0.007743 0.921569 0.436031 -21.00000 0.13212 O4 4 0.009386 0.936884 0.341461 -21.00000 0.19293 PART 1 EADP Cl1_6 Cl1_7 RESI 6 CLO4 CL1 5 0.001691 0.450718 0.369553 31.00000 0.13554 0.09773 = 0.13867 -0.01964 -0.00345 -0.01235 O1 4 0.073468 0.494698 0.377192 31.00000 0.12465 O2 4 -0.059724 0.482289 0.333985 31.00000 0.14217 O3 4 0.030370 0.389227 0.345600 31.00000 0.13313 O4 4 -0.035967 0.436861 0.421482 31.00000 0.15173 PART 2 RESI 7 CLO4 CL1 5 0.005036 0.443431 0.371017 -31.00000 0.13554 0.09773 = 0.13867 -0.01964 -0.00345 -0.01235 O1 4 0.046714 0.496874 0.400045 -31.00000 0.12134 O2 4 0.006841 0.457374 0.313617 -31.00000 0.15306 O3 4 0.048217 0.381360 0.381909 -31.00000 0.14490 O4 4 -0.082174 0.438244 0.388421 -31.00000 0.11658 PART 0 HKLF 4 REM samp2b REM R1 = 0.0809 for 1770 Fo > 4sig(Fo) and 0.1344 for all 2811 data REM 679 parameters refined using 1380 restraints END WGHT 0.0933 84.7176 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB_2 N1_0 O2_$1 HTAB_2 N1_0 O3_$1 HTAB_3 N1_0 O2_$1 HTAB N5 O2 HTAB_4 N6_0 Cl1_$2 HTAB_4 N6_0 O2_$2 HTAB_4 N6_0 O4_$2 HTAB_5 N6_0 O2_$2 HTAB_1 N10_0 Cl1_$1 HTAB_1 N10_0 O1_$1 HTAB_1 N10_0 O2_$1 HTAB_6 C16_0 O3_$3 HTAB_7 C16_0 O3_$3 HTAB_7 C30_0 O4_$2 HTAB_4 C22_0 O3_$4 HTAB_5 C25_0 O4_$4 HTAB_1 C32_0 O4_$4 HTAB N11 O3 HTAB N15 O4 HTAB N15 Cl1_4 HTAB N15 O1_4 HTAB N15 O4_4 HTAB N15 O1_5 HTAB N16 Cl1_6 HTAB N16 O1_6 HTAB N16 Cl1_7 HTAB N16 O1_7 HTAB N20 Cl1_2 HTAB N20 O1_2 HTAB N20 O2_2 HTAB N20 Cl1_3 HTAB N20 O1_3 HTAB_2 C38_0 O2_$5 HTAB_1 C47_0 O4_$6 HTAB_3 C60_0 O4_$5 HTAB C61 O3_5 HTAB_6 C66_0 O3_$7 REM Highest difference peak 0.275, deepest hole -0.235, 1-sigma level 0.065 Q1 1 0.3106 1.2611 0.5739 11.00000 0.05 0.27 Q2 1 0.1591 1.1315 0.7959 11.00000 0.05 0.25 Q3 1 0.4360 1.2614 0.3611 11.00000 0.05 0.25 Q4 1 0.3203 0.8365 0.1428 11.00000 0.05 0.24 Q5 1 0.5567 0.9245 0.3203 11.00000 0.05 0.24 Q6 1 0.3574 0.9899 0.4047 11.00000 0.05 0.23 Q7 1 0.3575 0.7201 0.0975 11.00000 0.05 0.23 Q8 1 0.3575 1.1956 0.4775 11.00000 0.05 0.22 Q9 1 0.0141 0.6993 0.2188 11.00000 0.05 0.22 Q10 1 0.3436 1.2897 0.5005 11.00000 0.05 0.22 Q11 1 0.5986 0.8711 0.2284 11.00000 0.05 0.21 Q12 1 0.2436 1.2365 0.7250 11.00000 0.05 0.21 Q13 1 0.1212 0.4308 0.3407 11.00000 0.05 0.21 Q14 1 0.2103 1.3816 0.7618 11.00000 0.05 0.21 Q15 1 0.2274 0.7768 0.3524 11.00000 0.05 0.21 Q16 1 0.0564 1.2401 0.6230 11.00000 0.05 0.20 Q17 1 0.2513 0.8677 0.3446 11.00000 0.05 0.20 Q18 1 0.1675 0.8200 0.3919 11.00000 0.05 0.20 Q19 1 0.1231 1.2776 0.9755 11.00000 0.05 0.20 Q20 1 0.4425 0.7622 0.3576 11.00000 0.05 0.19 ; _shelx_res_checksum 77775 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_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 Fe1 Fe 0.2696(2) 1.2670(2) 0.64517(13) 0.0877(16) Uani 1 1 d . U . . . O1 O 0.3683(12) 1.2503(11) 0.4208(7) 0.135(7) Uani 1 1 d . . . . . O2 O 0.1598(14) 1.4162(10) 0.8167(8) 0.150(7) Uani 1 1 d . . . . . N1 N 0.3352(13) 1.2125(11) 0.5215(9) 0.093(7) Uani 1 1 d . U . . . H1A H 0.3552 1.2487 0.5079 0.112 Uiso 1 1 calc R U . . . N2 N 0.3039(13) 1.2045(11) 0.5719(9) 0.093(6) Uani 1 1 d . U . . . N3 N 0.2360(12) 1.1659(9) 0.6666(8) 0.076(5) Uani 1 1 d . U . . . N4 N 0.2244(11) 1.2688(10) 0.7290(7) 0.084(5) Uani 1 1 d . U . . . N5 N 0.2099(11) 1.3109(9) 0.7716(8) 0.088(6) Uani 1 1 d . U . . . H5B H 0.2195 1.3531 0.7699 0.105 Uiso 1 1 calc R U . . . N6 N 0.0835(14) 1.2862(10) 0.5861(8) 0.101(7) Uani 1 1 d . U . . . H6A H 0.0663 1.2455 0.5879 0.121 Uiso 1 1 calc R U . . . N7 N 0.1558(14) 1.3086(11) 0.6068(8) 0.088(6) Uani 1 1 d . U . . . N8 N 0.2953(14) 1.3687(9) 0.6322(7) 0.085(5) Uani 1 1 d . U . . . N9 N 0.3959(13) 1.2831(11) 0.6786(8) 0.088(6) Uani 1 1 d . U . . . N10 N 0.4513(13) 1.2495(10) 0.7084(8) 0.098(7) Uani 1 1 d . U . . . H10A H 0.4481 1.2079 0.7167 0.118 Uiso 1 1 calc R U . . . C1 C 0.375(2) 1.184(2) 0.4019(16) 0.162(14) Uiso 1 1 d . . . . . C2 C 0.4002(17) 1.1741(15) 0.3465(12) 0.131(10) Uiso 1 1 d . . . . . H2A H 0.4162 1.2070 0.3220 0.158 Uiso 1 1 calc R U . . . C3 C 0.3960(19) 1.1065(17) 0.3366(13) 0.154(12) Uiso 1 1 d . . . . . H3A H 0.4081 1.0951 0.3009 0.185 Uiso 1 1 calc R U . . . C4 C 0.377(2) 1.052(2) 0.3690(15) 0.193(15) Uiso 1 1 d . . . . . H4A H 0.3778 1.0080 0.3568 0.232 Uiso 1 1 calc R U . . . C5 C 0.3577(16) 1.0706(14) 0.4226(10) 0.112(9) Uiso 1 1 d . . . . . H5A H 0.3458 1.0376 0.4480 0.135 Uiso 1 1 calc R U . . . C6 C 0.3556(18) 1.1391(16) 0.4387(13) 0.129(10) Uiso 1 1 d . . . . . C7 C 0.3289(17) 1.1507(14) 0.4956(12) 0.104(9) Uiso 1 1 d . . . . . C8 C 0.2954(15) 1.1065(13) 0.5299(10) 0.101(9) Uiso 1 1 d . . . . . H8A H 0.2837 1.0619 0.5225 0.122 Uiso 1 1 calc R U . . . C9 C 0.2812(15) 1.1392(13) 0.5781(10) 0.075(8) Uiso 1 1 d . . . . . C10 C 0.2450(16) 1.1196(14) 0.6275(11) 0.095(8) Uiso 1 1 d . . . . . C11 C 0.2163(15) 1.0543(13) 0.6397(10) 0.096(8) Uiso 1 1 d . . . . . H11A H 0.2213 1.0202 0.6143 0.115 Uiso 1 1 calc R U . . . C12 C 0.1825(16) 1.0426(13) 0.6877(11) 0.109(9) Uiso 1 1 d . . . . . H12A H 0.1622 0.9998 0.6943 0.130 Uiso 1 1 calc R U . . . C13 C 0.1752(15) 1.0883(13) 0.7281(10) 0.100(8) Uiso 1 1 d . . . . . H13A H 0.1527 1.0781 0.7619 0.119 Uiso 1 1 calc R U . . . C14 C 0.2042(17) 1.1516(13) 0.7147(11) 0.089(8) Uiso 1 1 d . . . . . C15 C 0.2015(15) 1.2087(13) 0.7500(10) 0.085(8) Uiso 1 1 d . . . . . C16 C 0.1744(15) 1.2163(13) 0.8026(9) 0.082(8) Uiso 1 1 d . . . . . H16A H 0.1556 1.1822 0.8252 0.099 Uiso 1 1 calc R U . . . C17 C 0.1799(15) 1.2815(13) 0.8159(11) 0.088(8) Uiso 1 1 d . . . . . C18 C 0.1587(14) 1.3190(13) 0.8648(9) 0.083(7) Uiso 1 1 d . . . . . C19 C 0.1409(18) 1.2844(16) 0.9097(12) 0.134(11) Uiso 1 1 d . . . . . H19A H 0.1440 1.2381 0.9091 0.161 Uiso 1 1 calc R U . . . C30 C 0.2534(19) 1.4760(15) 0.5987(10) 0.128(10) Uiso 1 1 d . . . . . H30A H 0.2104 1.5032 0.5850 0.154 Uiso 1 1 calc R U . . . C20 C 0.1176(16) 1.3170(14) 0.9580(11) 0.118(9) Uiso 1 1 d . . . . . H20A H 0.1106 1.2940 0.9904 0.142 Uiso 1 1 calc R U . . . C21 C 0.1058(16) 1.3841(14) 0.9545(11) 0.117(9) Uiso 1 1 d . . . . . H21A H 0.0879 1.4058 0.9858 0.140 Uiso 1 1 calc R U . . . C22 C 0.1174(16) 1.4220(14) 0.9104(11) 0.118(9) Uiso 1 1 d . . . . . H22A H 0.1082 1.4678 0.9100 0.141 Uiso 1 1 calc R U . . . C23 C 0.1453(16) 1.3857(15) 0.8640(12) 0.099(9) Uiso 1 1 d . . . . . C24 C 0.394(2) 1.3006(17) 0.3809(13) 0.173(14) Uiso 1 1 d . . . . . H24A H 0.3873 1.3443 0.3964 0.259 Uiso 1 1 calc R U . . . H24B H 0.4519 1.2936 0.3710 0.259 Uiso 1 1 calc R U . . . H24C H 0.3579 1.2968 0.3492 0.259 Uiso 1 1 calc R U . . . C25 C 0.132(3) 1.485(2) 0.8145(15) 0.225(18) Uiso 1 1 d . . . . . H25A H 0.1447 1.5030 0.7795 0.337 Uiso 1 1 calc R U . . . H25B H 0.0719 1.4868 0.8206 0.337 Uiso 1 1 calc R U . . . H25C H 0.1614 1.5099 0.8420 0.337 Uiso 1 1 calc R U . . . C26 C 0.0413(19) 1.3354(14) 0.5620(10) 0.115(10) Uiso 1 1 d . . . . . H26A H -0.0142 1.3326 0.5485 0.138 Uiso 1 1 calc R U . . . C27 C 0.0912(17) 1.3902(14) 0.5600(9) 0.107(9) Uiso 1 1 d . . . . . H27A H 0.0804 1.4303 0.5423 0.128 Uiso 1 1 calc R U . . . C28 C 0.1622(17) 1.3727(14) 0.5904(10) 0.087(8) Uiso 1 1 d . . . . . C29 C 0.2413(18) 1.4068(14) 0.6069(10) 0.092(8) Uiso 1 1 d . . . . . C31 C 0.3340(19) 1.5010(15) 0.6123(10) 0.126(10) Uiso 1 1 d . . . . . H31A H 0.3493 1.5448 0.6047 0.151 Uiso 1 1 calc R U . . . C32 C 0.3885(17) 1.4584(14) 0.6371(9) 0.111(9) Uiso 1 1 d . . . . . H32A H 0.4410 1.4747 0.6488 0.133 Uiso 1 1 calc R U . . . C33 C 0.3704(18) 1.3921(14) 0.6459(9) 0.091(8) Uiso 1 1 d . . . . . C34 C 0.4239(18) 1.3443(14) 0.6733(10) 0.091(8) Uiso 1 1 d . . . . . C35 C 0.4985(16) 1.3531(13) 0.7051(9) 0.098(8) Uiso 1 1 d . . . . . H35A H 0.5289 1.3922 0.7113 0.118 Uiso 1 1 calc R U . . . C36 C 0.5149(18) 1.2928(13) 0.7237(9) 0.101(9) Uiso 1 1 d . . . . . H36A H 0.5626 1.2812 0.7443 0.121 Uiso 1 1 calc R U . . . Fe2 Fe 0.2250(2) 0.6855(2) 0.34735(12) 0.0869(16) Uani 1 1 d . U . . . O3 O 0.3289(13) 0.7233(10) 0.1483(7) 0.130(7) Uani 1 1 d . . . . . O4 O 0.1769(13) 0.8650(9) 0.5025(7) 0.138(7) Uani 1 1 d . . . . . N11 N 0.2909(12) 0.6537(11) 0.2326(8) 0.092(7) Uani 1 1 d . U . . . H11B H 0.2795 0.6920 0.2185 0.111 Uiso 1 1 calc R U . . . N12 N 0.2740(11) 0.6401(10) 0.2848(8) 0.081(6) Uani 1 1 d . U . . . N13 N 0.2506(11) 0.5990(8) 0.3778(7) 0.074(5) Uiso 1 1 d . . . . . N14 N 0.1880(13) 0.7000(11) 0.4230(8) 0.088(6) Uani 1 1 d . U . . . N15 N 0.1623(11) 0.7497(10) 0.4532(8) 0.088(6) Uani 1 1 d . U . . . H15A H 0.1517 0.7893 0.4415 0.105 Uiso 1 1 calc R U . . . N16 N 0.0537(14) 0.6163(10) 0.3229(7) 0.096(6) Uani 1 1 d . U . . . H16B H 0.0601 0.5794 0.3403 0.115 Uiso 1 1 calc R U . . . N17 N 0.1099(12) 0.6658(10) 0.3215(7) 0.081(5) Uani 1 1 d . U . . . N18 N 0.1989(14) 0.7678(10) 0.3102(7) 0.084(6) Uiso 1 1 d . . . . . N19 N 0.3282(12) 0.7382(10) 0.3636(7) 0.083(6) Uani 1 1 d . U . . . N20 N 0.3963(13) 0.7337(11) 0.3968(8) 0.099(7) Uani 1 1 d . U . . . H20B H 0.4107 0.6993 0.4156 0.118 Uiso 1 1 calc R U . . . C37 C 0.3572(16) 0.6682(16) 0.1232(11) 0.101(9) Uiso 1 1 d . . . . . C38 C 0.3882(17) 0.6685(15) 0.0686(11) 0.129(10) Uiso 1 1 d . . . . . H38A H 0.3908 0.7082 0.0491 0.155 Uiso 1 1 calc R U . . . C39 C 0.4135(18) 0.6108(16) 0.0459(12) 0.138(11) Uiso 1 1 d . . . . . H39A H 0.4327 0.6122 0.0103 0.166 Uiso 1 1 calc R U . . . C40 C 0.4131(17) 0.5516(15) 0.0709(11) 0.129(10) Uiso 1 1 d . . . . . H40A H 0.4309 0.5126 0.0538 0.155 Uiso 1 1 calc R U . . . C41 C 0.3830(16) 0.5523(14) 0.1267(11) 0.118(9) Uiso 1 1 d . . . . . H41A H 0.3816 0.5129 0.1465 0.142 Uiso 1 1 calc R U . . . C42 C 0.3576(15) 0.6087(13) 0.1493(10) 0.087(8) Uiso 1 1 d . . . . . C43 C 0.3273(16) 0.6032(13) 0.2025(11) 0.094(8) Uiso 1 1 d . . . . . C44 C 0.3305(13) 0.5536(11) 0.2423(9) 0.084(7) Uiso 1 1 d . . . . . H44A H 0.3525 0.5110 0.2368 0.101 Uiso 1 1 calc R U . . . C45 C 0.2967(15) 0.5754(13) 0.2907(10) 0.086(8) Uiso 1 1 d . . . . . C46 C 0.2839(16) 0.5551(12) 0.3452(10) 0.087(8) Uiso 1 1 d . . . . . C47 C 0.3021(16) 0.4908(14) 0.3675(11) 0.122(9) Uiso 1 1 d . . . . . H47A H 0.3230 0.4568 0.3457 0.147 Uiso 1 1 calc R U . . . C48 C 0.2883(18) 0.4799(16) 0.4219(12) 0.141(11) Uiso 1 1 d . . . . . H48A H 0.3039 0.4396 0.4379 0.170 Uiso 1 1 calc R U . . . C49 C 0.2520(18) 0.5280(15) 0.4516(12) 0.133(10) Uiso 1 1 d . . . . . H49A H 0.2395 0.5192 0.4878 0.160 Uiso 1 1 calc R U . . . C50 C 0.2324(15) 0.5898(13) 0.4310(10) 0.088(8) Uiso 1 1 d . . . . . C51 C 0.1988(16) 0.6440(14) 0.4566(11) 0.083(9) Uiso 1 1 d . . . . . C52 C 0.1805(15) 0.6640(12) 0.5073(11) 0.097(8) Uiso 1 1 d . . . . . H52A H 0.1847 0.6373 0.5381 0.116 Uiso 1 1 calc R U . . . C53 C 0.1546(16) 0.7295(13) 0.5070(11) 0.089(8) Uiso 1 1 d . . . . . C54 C 0.1267(16) 0.7764(14) 0.5477(10) 0.094(9) Uiso 1 1 d . . . . . C55 C 0.0950(15) 0.7476(14) 0.5939(10) 0.110(9) Uiso 1 1 d . . . . . H55A H 0.0902 0.7013 0.5953 0.132 Uiso 1 1 calc R U . . . C56 C 0.0692(17) 0.7854(15) 0.6396(11) 0.121(10) Uiso 1 1 d . . . . . H56A H 0.0443 0.7660 0.6699 0.145 Uiso 1 1 calc R U . . . C57 C 0.0836(19) 0.8508(16) 0.6357(13) 0.145(11) Uiso 1 1 d . . . . . H57A H 0.0715 0.8771 0.6658 0.174 Uiso 1 1 calc R U . . . C58 C 0.1142(18) 0.8817(16) 0.5914(12) 0.134(10) Uiso 1 1 d . . . . . H58A H 0.1163 0.9280 0.5898 0.160 Uiso 1 1 calc R U . . . C59 C 0.1416(17) 0.8449(15) 0.5498(13) 0.105(9) Uiso 1 1 d . . . . . C60 C 0.3413(19) 0.7859(16) 0.1230(12) 0.146(12) Uiso 1 1 d . . . . . H60A H 0.3180 0.8205 0.1454 0.219 Uiso 1 1 calc R U . . . H60B H 0.4012 0.7935 0.1183 0.219 Uiso 1 1 calc R U . . . H60C H 0.3133 0.7862 0.0883 0.219 Uiso 1 1 calc R U . . . C61 C 0.189(2) 0.9338(16) 0.4983(12) 0.155(12) Uiso 1 1 d . . . . . H61A H 0.2141 0.9440 0.4639 0.232 Uiso 1 1 calc R U . . . H61B H 0.1350 0.9560 0.5012 0.232 Uiso 1 1 calc R U . . . H61C H 0.2261 0.9486 0.5271 0.232 Uiso 1 1 calc R U . . . C62 C -0.014(2) 0.6327(15) 0.2936(11) 0.125(10) Uiso 1 1 d . . . . . H62A H -0.0593 0.6046 0.2859 0.150 Uiso 1 1 calc R U . . . C63 C -0.0064(16) 0.6950(13) 0.2768(9) 0.099(8) Uiso 1 1 d . . . . . H63A H -0.0470 0.7205 0.2585 0.119 Uiso 1 1 calc R U . . . C64 C 0.0757(18) 0.7143(14) 0.2925(9) 0.084(8) Uiso 1 1 d . . . . . C65 C 0.1233(17) 0.7716(14) 0.2825(10) 0.096(8) Uiso 1 1 d . . . . . C66 C 0.1112(17) 0.8258(13) 0.2493(10) 0.113(9) Uiso 1 1 d . . . . . H66A H 0.0609 0.8302 0.2294 0.135 Uiso 1 1 calc R U . . . C67 C 0.1733(18) 0.8735(13) 0.2455(10) 0.112(9) Uiso 1 1 d . . . . . H67A H 0.1654 0.9096 0.2223 0.135 Uiso 1 1 calc R U . . . C68 C 0.2487(17) 0.8686(13) 0.2762(10) 0.110(9) Uiso 1 1 d . . . . . H68A H 0.2904 0.9016 0.2744 0.132 Uiso 1 1 calc R U . . . C69 C 0.2591(16) 0.8136(13) 0.3090(9) 0.085(8) Uiso 1 1 d . . . . . C70 C 0.3311(18) 0.8006(15) 0.3444(11) 0.092(9) Uiso 1 1 d . . . . . C71 C 0.3995(17) 0.8369(14) 0.3618(10) 0.100(8) Uiso 1 1 d . . . . . H71A H 0.4154 0.8803 0.3529 0.120 Uiso 1 1 calc R U . . . C72 C 0.4381(18) 0.7925(13) 0.3955(10) 0.097(9) Uiso 1 1 d . . . . . H72A H 0.4874 0.8015 0.4154 0.116 Uiso 1 1 calc R U . . . Cl1_1 Cl 0.4996(5) 0.9116(4) 0.2406(3) 0.130(3) Uani 1 1 d D . . . . O1_1 O 0.5692(8) 0.8910(8) 0.2754(6) 0.150(7) Uiso 1 1 d D . . . . O2_1 O 0.4484(10) 0.8535(7) 0.2283(6) 0.151(7) Uiso 1 1 d D . . . . O3_1 O 0.4483(10) 0.9603(7) 0.2681(7) 0.176(9) Uiso 1 1 d D . . . . O4_1 O 0.5321(10) 0.9392(8) 0.1911(5) 0.152(7) Uiso 1 1 d D . . . . Cl1_2 Cl 0.5117(14) 0.6431(11) 0.4925(7) 0.219(18) Uani 0.64(3) 1 d D . P A 1 O1_2 O 0.472(3) 0.6172(18) 0.4439(10) 0.15(2) Uiso 0.64(3) 1 d D . P A 1 O2_2 O 0.4889(17) 0.7123(11) 0.4996(10) 0.125(16) Uiso 0.64(3) 1 d D . P A 1 O3_2 O 0.6027(16) 0.6377(15) 0.4871(12) 0.140(16) Uiso 0.64(3) 1 d D . P A 1 O4_2 O 0.4830(17) 0.6058(13) 0.5388(9) 0.113(12) Uiso 0.64(3) 1 d D . P A 1 Cl1_3 Cl 0.4965(18) 0.6339(12) 0.4899(8) 0.052(11) Uani 0.36(3) 1 d D . P A 2 O1_3 O 0.450(3) 0.613(2) 0.4420(14) 0.08(3) Uiso 0.36(3) 1 d D . P A 2 O2_3 O 0.560(4) 0.682(3) 0.475(2) 0.25(5) Uiso 0.36(3) 1 d D . P A 2 O3_3 O 0.537(4) 0.5766(18) 0.514(2) 0.18(3) Uiso 0.36(3) 1 d D . P A 2 O4_3 O 0.438(3) 0.663(4) 0.528(2) 0.32(7) Uiso 0.36(3) 1 d D . P A 2 Cl1_4 Cl 0.0188(8) 0.8755(7) 0.3952(5) 0.119(3) Uani 0.79(3) 1 d D . P B 1 O1_4 O 0.1096(10) 0.8739(13) 0.3874(11) 0.134(19) Uiso 0.79(3) 1 d D . P B 1 O2_4 O -0.0246(14) 0.8515(11) 0.3472(7) 0.141(11) Uiso 0.79(3) 1 d D . P B 1 O3_4 O -0.0080(14) 0.9430(8) 0.4061(9) 0.139(11) Uiso 0.79(3) 1 d D . P B 1 O4_4 O -0.0037(13) 0.8337(9) 0.4407(7) 0.126(10) Uiso 0.79(3) 1 d D . P B 1 Cl1_5 Cl 0.018(3) 0.889(2) 0.384(2) 0.119(3) Uani 0.21(3) 1 d D . P B 2 O1_5 O 0.101(4) 0.858(4) 0.382(3) 0.05(4) Uiso 0.21(3) 1 d D . P B 2 O2_5 O -0.046(5) 0.838(4) 0.378(4) 0.19(6) Uiso 0.21(3) 1 d D . P B 2 O3_5 O 0.008(5) 0.922(4) 0.436(2) 0.13(4) Uiso 0.21(3) 1 d D . P B 2 O4_5 O 0.009(5) 0.937(4) 0.341(3) 0.19(5) Uiso 0.21(3) 1 d D . P B 2 Cl1_6 Cl 0.0017(9) 0.4507(7) 0.3696(5) 0.124(3) Uani 0.73(3) 1 d D . P C 1 O1_6 O 0.0735(12) 0.4947(10) 0.3772(10) 0.125(11) Uiso 0.73(3) 1 d D . P C 1 O2_6 O -0.0597(13) 0.4823(10) 0.3340(9) 0.142(12) Uiso 0.73(3) 1 d D . P C 1 O3_6 O 0.0304(14) 0.3892(9) 0.3456(9) 0.133(11) Uiso 0.73(3) 1 d D . P C 1 O4_6 O -0.0360(17) 0.4369(12) 0.4215(7) 0.152(13) Uiso 0.73(3) 1 d D . P C 1 Cl1_7 Cl 0.005(2) 0.4434(18) 0.3710(13) 0.124(3) Uani 0.27(3) 1 d D . P C 2 O1_7 O 0.047(3) 0.497(2) 0.400(2) 0.12(3) Uiso 0.27(3) 1 d D . P C 2 O2_7 O 0.007(4) 0.457(3) 0.3136(14) 0.15(4) Uiso 0.27(3) 1 d D . P C 2 O3_7 O 0.048(3) 0.381(2) 0.382(3) 0.14(3) Uiso 0.27(3) 1 d D . P C 2 O4_7 O -0.082(2) 0.438(3) 0.388(2) 0.12(3) Uiso 0.27(3) 1 d D . P C 2 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 Fe1 0.078(4) 0.086(3) 0.099(3) 0.003(2) -0.004(2) -0.006(2) O1 0.136(18) 0.15(2) 0.117(15) 0.019(15) 0.007(12) -0.005(15) O2 0.21(2) 0.099(16) 0.141(17) 0.002(13) 0.010(15) 0.006(14) N1 0.074(16) 0.103(18) 0.103(11) 0.016(10) -0.009(10) 0.009(12) N2 0.081(14) 0.100(13) 0.096(9) 0.006(8) -0.007(8) -0.001(10) N3 0.070(12) 0.084(9) 0.075(11) -0.007(7) 0.004(9) 0.011(8) N4 0.061(11) 0.096(12) 0.093(9) -0.007(7) -0.009(7) -0.012(9) N5 0.072(14) 0.093(14) 0.097(11) -0.005(10) -0.014(10) -0.002(11) N6 0.090(12) 0.080(16) 0.131(16) -0.011(13) -0.019(10) -0.009(11) N7 0.086(10) 0.084(13) 0.095(12) -0.012(9) -0.009(8) -0.007(8) N8 0.074(12) 0.082(9) 0.100(12) -0.005(8) -0.017(10) -0.002(8) N9 0.075(9) 0.098(13) 0.090(12) 0.010(9) -0.005(7) 0.000(8) N10 0.076(13) 0.102(16) 0.117(15) 0.017(12) -0.017(10) -0.006(11) Fe2 0.077(3) 0.090(3) 0.094(3) 0.0128(19) -0.008(2) 0.004(2) O3 0.16(2) 0.109(17) 0.125(15) 0.025(14) -0.005(12) -0.027(14) O4 0.21(2) 0.090(15) 0.114(15) 0.000(11) -0.022(14) -0.031(14) N11 0.071(15) 0.120(18) 0.085(10) -0.006(11) -0.010(9) -0.015(13) N12 0.052(11) 0.099(14) 0.091(9) 0.000(9) -0.004(8) -0.008(9) N14 0.081(13) 0.087(15) 0.096(9) 0.004(8) 0.003(8) -0.004(10) N15 0.071(16) 0.094(15) 0.098(13) -0.005(10) -0.010(10) -0.002(11) N16 0.097(13) 0.098(15) 0.091(14) 0.019(11) -0.005(11) -0.021(11) N17 0.072(9) 0.079(14) 0.093(11) 0.006(10) 0.007(8) 0.001(8) N19 0.071(10) 0.090(13) 0.089(12) 0.004(10) 0.005(7) 0.002(9) N20 0.085(12) 0.112(18) 0.099(14) 0.009(12) -0.007(9) 0.006(12) Cl1_1 0.118(7) 0.132(7) 0.139(7) 0.028(5) -0.005(5) -0.016(6) Cl1_2 0.22(3) 0.27(4) 0.17(3) 0.06(2) -0.10(2) -0.12(3) Cl1_3 0.08(2) 0.028(18) 0.05(2) 0.004(13) 0.016(14) 0.034(12) Cl1_4 0.125(9) 0.123(9) 0.108(9) -0.002(6) 0.000(5) -0.006(8) Cl1_5 0.125(9) 0.123(9) 0.108(9) -0.002(6) 0.000(5) -0.006(8) Cl1_6 0.136(9) 0.098(7) 0.139(8) -0.020(5) -0.003(5) -0.012(5) Cl1_7 0.136(9) 0.098(7) 0.139(8) -0.020(5) -0.003(5) -0.012(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cl Cl 0.1408 0.1896 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Fe Fe 0.2064 0.9930 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N8 Fe1 N3 173.7(8) N8 Fe1 N9 74.8(8) N3 Fe1 N9 105.8(8) N8 Fe1 N7 73.8(8) N3 Fe1 N7 105.3(8) N9 Fe1 N7 148.5(9) N8 Fe1 N4 101.1(7) N3 Fe1 N4 72.7(8) N9 Fe1 N4 86.6(7) N7 Fe1 N4 97.6(7) N8 Fe1 N2 111.6(8) N3 Fe1 N2 74.7(8) N9 Fe1 N2 99.3(7) N7 Fe1 N2 93.7(7) N4 Fe1 N2 147.3(8) C1 O1 C24 114(3) C23 O2 C25 114(3) N2 N1 C7 107(2) N2 N1 H1A 126.5 C7 N1 H1A 126.5 N1 N2 C9 108(2) N1 N2 Fe1 139.4(18) C9 N2 Fe1 112.2(17) C14 N3 C10 122(2) C14 N3 Fe1 121.1(17) C10 N3 Fe1 116.4(18) C15 N4 N5 102.0(19) C15 N4 Fe1 115.7(17) N5 N4 Fe1 142.3(16) C17 N5 N4 115(2) C17 N5 H5B 122.6 N4 N5 H5B 122.6 N7 N6 C26 110(2) N7 N6 H6A 124.9 C26 N6 H6A 124.9 N6 N7 C28 106(2) N6 N7 Fe1 137.5(19) C28 N7 Fe1 115.5(19) C29 N8 C33 120(2) C29 N8 Fe1 121.2(18) C33 N8 Fe1 118.8(18) C34 N9 N10 108(2) C34 N9 Fe1 114(2) N10 N9 Fe1 137.2(18) N9 N10 C36 108(2) N9 N10 H10A 126.1 C36 N10 H10A 126.1 C6 C1 O1 113(4) C6 C1 C2 129(4) O1 C1 C2 118(3) C3 C2 C1 107(3) C3 C2 H2A 126.6 C1 C2 H2A 126.6 C2 C3 C4 133(3) C2 C3 H3A 113.5 C4 C3 H3A 113.5 C3 C4 C5 112(3) C3 C4 H4A 123.8 C5 C4 H4A 123.8 C4 C5 C6 121(3) C4 C5 H5A 119.3 C6 C5 H5A 119.3 C1 C6 C5 117(3) C1 C6 C7 128(3) C5 C6 C7 115(3) C8 C7 N1 109(3) C8 C7 C6 128(3) N1 C7 C6 123(3) C7 C8 C9 107(3) C7 C8 H8A 126.3 C9 C8 H8A 126.3 N2 C9 C8 108(2) N2 C9 C10 118(2) C8 C9 C10 133(3) N3 C10 C9 118(3) N3 C10 C11 117(3) C9 C10 C11 125(3) C12 C11 C10 119(3) C12 C11 H11A 120.5 C10 C11 H11A 120.5 C11 C12 C13 125(3) C11 C12 H12A 117.5 C13 C12 H12A 117.5 C12 C13 C14 114(3) C12 C13 H13A 122.8 C14 C13 H13A 122.8 N3 C14 C13 123(3) N3 C14 C15 113(3) C13 C14 C15 125(3) N4 C15 C16 110(2) N4 C15 C14 118(2) C16 C15 C14 132(3) C17 C16 C15 108(2) C17 C16 H16A 125.8 C15 C16 H16A 125.8 N5 C17 C16 105(2) N5 C17 C18 122(2) C16 C17 C18 133(3) C19 C18 C23 119(3) C19 C18 C17 118(3) C23 C18 C17 122(2) C18 C19 C20 121(3) C18 C19 H19A 119.5 C20 C19 H19A 119.5 C31 C30 C29 116(3) C31 C30 H30A 122.0 C29 C30 H30A 122.0 C21 C20 C19 116(3) C21 C20 H20A 121.9 C19 C20 H20A 121.9 C22 C21 C20 126(3) C22 C21 H21A 116.9 C20 C21 H21A 116.9 C21 C22 C23 114(3) C21 C22 H22A 123.0 C23 C22 H22A 123.0 O2 C23 C18 116(3) O2 C23 C22 121(3) C18 C23 C22 123(3) O1 C24 H24A 109.5 O1 C24 H24B 109.5 H24A C24 H24B 109.5 O1 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 O2 C25 H25A 109.5 O2 C25 H25B 109.5 H25A C25 H25B 109.5 O2 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 N6 C26 C27 109(3) N6 C26 H26A 125.3 C27 C26 H26A 125.3 C26 C27 C28 104(3) C26 C27 H27A 128.0 C28 C27 H27A 128.0 N7 C28 C27 110(3) N7 C28 C29 115(3) C27 C28 C29 135(3) N8 C29 C30 124(3) N8 C29 C28 114(3) C30 C29 C28 122(3) C32 C31 C30 117(3) C32 C31 H31A 121.6 C30 C31 H31A 121.6 C31 C32 C33 123(3) C31 C32 H32A 118.3 C33 C32 H32A 118.3 N8 C33 C32 119(3) N8 C33 C34 114(3) C32 C33 C34 127(3) N9 C34 C35 110(3) N9 C34 C33 118(3) C35 C34 C33 131(3) C36 C35 C34 104(3) C36 C35 H35A 128.1 C34 C35 H35A 128.1 C35 C36 N10 110(3) C35 C36 H36A 125.0 N10 C36 H36A 125.0 N18 Fe2 N13 174.5(8) N18 Fe2 N17 79.9(9) N13 Fe2 N17 97.7(8) N18 Fe2 N12 96.2(8) N13 Fe2 N12 78.8(8) N17 Fe2 N12 91.0(7) N18 Fe2 N19 79.1(9) N13 Fe2 N19 103.5(8) N17 Fe2 N19 158.7(9) N12 Fe2 N19 94.7(7) N18 Fe2 N14 105.0(8) N13 Fe2 N14 80.0(8) N17 Fe2 N14 93.4(8) N12 Fe2 N14 158.8(8) N19 Fe2 N14 88.7(8) C37 O3 C60 119(2) C59 O4 C61 114(2) N12 N11 C43 117(2) N12 N11 H11B 121.6 C43 N11 H11B 121.6 N11 N12 C45 104(2) N11 N12 Fe2 138.0(17) C45 N12 Fe2 117.9(17) C46 N13 C50 126(2) C46 N13 Fe2 116.7(16) C50 N13 Fe2 116.9(16) N15 N14 C51 108(2) N15 N14 Fe2 137.9(18) C51 N14 Fe2 113.8(19) N14 N15 C53 110(2) N14 N15 H15A 124.8 C53 N15 H15A 124.8 C62 N16 N17 109(2) C62 N16 H16B 125.4 N17 N16 H16B 125.4 C64 N17 N16 107(2) C64 N17 Fe2 113.6(19) N16 N17 Fe2 139.2(17) C69 N18 C65 125(2) C69 N18 Fe2 117.1(19) C65 N18 Fe2 117.7(19) C70 N19 N20 104(2) C70 N19 Fe2 117.3(19) N20 N19 Fe2 137.4(18) N19 N20 C72 108(2) N19 N20 H20B 125.9 C72 N20 H20B 125.9 O3 C37 C42 120(3) O3 C37 C38 123(3) C42 C37 C38 117(3) C39 C38 C37 119(3) C39 C38 H38A 120.3 C37 C38 H38A 120.3 C40 C39 C38 125(3) C40 C39 H39A 117.7 C38 C39 H39A 117.7 C39 C40 C41 115(3) C39 C40 H40A 122.3 C41 C40 H40A 122.3 C42 C41 C40 121(3) C42 C41 H41A 119.7 C40 C41 H41A 119.7 C41 C42 C37 123(3) C41 C42 C43 116(3) C37 C42 C43 121(3) N11 C43 C44 99(2) N11 C43 C42 126(2) C44 C43 C42 134(3) C45 C44 C43 112(2) C45 C44 H44A 124.2 C43 C44 H44A 124.2 N12 C45 C44 108(2) N12 C45 C46 110(2) C44 C45 C46 142(3) N13 C46 C45 117(2) N13 C46 C47 117(2) C45 C46 C47 126(2) C48 C47 C46 119(3) C48 C47 H47A 120.5 C46 C47 H47A 120.5 C49 C48 C47 119(3) C49 C48 H48A 120.4 C47 C48 H48A 120.4 C48 C49 C50 123(3) C48 C49 H49A 118.6 C50 C49 H49A 118.6 N13 C50 C51 115(2) N13 C50 C49 116(2) C51 C50 C49 129(3) C52 C51 C50 139(3) C52 C51 N14 106(3) C50 C51 N14 114(3) C51 C52 C53 110(3) C51 C52 H52A 124.9 C53 C52 H52A 124.9 C52 C53 N15 105(2) C52 C53 C54 135(3) N15 C53 C54 120(2) C55 C54 C59 116(3) C55 C54 C53 115(3) C59 C54 C53 128(3) C54 C55 C56 123(3) C54 C55 H55A 118.6 C56 C55 H55A 118.6 C57 C56 C55 115(3) C57 C56 H56A 122.7 C55 C56 H56A 122.7 C56 C57 C58 125(3) C56 C57 H57A 117.6 C58 C57 H57A 117.6 C59 C58 C57 119(3) C59 C58 H58A 120.4 C57 C58 H58A 120.4 C58 C59 O4 129(3) C58 C59 C54 121(3) O4 C59 C54 109(3) O3 C60 H60A 109.5 O3 C60 H60B 109.5 H60A C60 H60B 109.5 O3 C60 H60C 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 O4 C61 H61A 109.5 O4 C61 H61B 109.5 H61A C61 H61B 109.5 O4 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 N16 C62 C63 110(3) N16 C62 H62A 125.2 C63 C62 H62A 125.2 C62 C63 C64 105(3) C62 C63 H63A 127.6 C64 C63 H63A 127.6 N17 C64 C65 119(3) N17 C64 C63 108(3) C65 C64 C63 132(3) N18 C65 C66 117(3) N18 C65 C64 109(3) C66 C65 C64 133(3) C67 C66 C65 120(3) C67 C66 H66A 120.1 C65 C66 H66A 120.1 C66 C67 C68 121(3) C66 C67 H67A 119.5 C68 C67 H67A 119.5 C69 C68 C67 118(3) C69 C68 H68A 121.0 C67 C68 H68A 121.0 N18 C69 C68 119(3) N18 C69 C70 115(3) C68 C69 C70 126(3) N19 C70 C71 115(3) N19 C70 C69 111(3) C71 C70 C69 135(3) C72 C71 C70 101(3) C72 C71 H71A 129.6 C70 C71 H71A 129.6 N20 C72 C71 112(3) N20 C72 H72A 124.1 C71 C72 H72A 124.1 O4_1 Cl1_1 O3_1 110.1(9) O4_1 Cl1_1 O1_1 110.0(9) O3_1 Cl1_1 O1_1 109.7(9) O4_1 Cl1_1 O2_1 109.5(8) O3_1 Cl1_1 O2_1 109.4(9) O1_1 Cl1_1 O2_1 108.1(8) O4_2 Cl1_2 O3_2 110.6(11) O4_2 Cl1_2 O2_2 108.9(10) O3_2 Cl1_2 O2_2 109.3(10) O4_2 Cl1_2 O1_2 109.5(11) O3_2 Cl1_2 O1_2 108.7(11) O2_2 Cl1_2 O1_2 109.9(11) O4_3 Cl1_3 O2_3 109.9(11) O4_3 Cl1_3 O3_3 109.4(11) O2_3 Cl1_3 O3_3 109.4(11) O4_3 Cl1_3 O1_3 109.6(11) O2_3 Cl1_3 O1_3 109.4(11) O3_3 Cl1_3 O1_3 109.1(11) O1_4 Cl1_4 O2_4 110.2(10) O1_4 Cl1_4 O4_4 109.8(10) O2_4 Cl1_4 O4_4 109.1(10) O1_4 Cl1_4 O3_4 109.6(10) O2_4 Cl1_4 O3_4 109.2(10) O4_4 Cl1_4 O3_4 109.0(10) O4_5 Cl1_5 O1_5 109.7(11) O4_5 Cl1_5 O2_5 109.4(11) O1_5 Cl1_5 O2_5 109.5(11) O4_5 Cl1_5 O3_5 109.2(11) O1_5 Cl1_5 O3_5 109.6(11) O2_5 Cl1_5 O3_5 109.4(11) O3_6 Cl1_6 O4_6 109.3(10) O3_6 Cl1_6 O1_6 109.3(10) O4_6 Cl1_6 O1_6 109.1(10) O3_6 Cl1_6 O2_6 109.6(10) O4_6 Cl1_6 O2_6 110.3(10) O1_6 Cl1_6 O2_6 109.2(9) O3_7 Cl1_7 O4_7 109.2(11) O3_7 Cl1_7 O1_7 109.7(11) O4_7 Cl1_7 O1_7 109.5(11) O3_7 Cl1_7 O2_7 109.7(11) O4_7 Cl1_7 O2_7 109.4(11) O1_7 Cl1_7 O2_7 109.3(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N8 2.103(19) Fe1 N3 2.16(2) Fe1 N9 2.17(2) Fe1 N7 2.18(2) Fe1 N4 2.190(19) Fe1 N2 2.26(2) O1 C1 1.41(4) O1 C24 1.46(3) O2 C23 1.34(3) O2 C25 1.44(4) N1 N2 1.35(2) N1 C7 1.40(3) N1 H1A 0.8600 N2 C9 1.36(3) N3 C14 1.32(3) N3 C10 1.35(3) N4 C15 1.36(2) N4 N5 1.37(2) N5 C17 1.33(2) N5 H5B 0.8600 N6 N7 1.32(2) N6 C26 1.33(3) N6 H6A 0.8600 N7 C28 1.35(3) N8 C29 1.30(3) N8 C33 1.31(3) N9 C34 1.31(3) N9 N10 1.32(2) N10 C36 1.37(3) N10 H10A 0.8600 C1 C6 1.31(4) C1 C2 1.44(4) C2 C3 1.38(3) C2 H2A 0.9300 C3 C4 1.39(4) C3 H3A 0.9300 C4 C5 1.41(3) C4 H4A 0.9300 C5 C6 1.43(3) C5 H5A 0.9300 C6 C7 1.49(3) C7 C8 1.33(3) C8 C9 1.38(3) C8 H8A 0.9300 C9 C10 1.40(3) C10 C11 1.42(3) C11 C12 1.32(3) C11 H11A 0.9300 C12 C13 1.36(3) C12 H12A 0.9300 C13 C14 1.39(3) C13 H13A 0.9300 C14 C15 1.44(3) C15 C16 1.38(3) C16 C17 1.35(3) C16 H16A 0.9300 C17 C18 1.46(3) C18 C19 1.34(3) C18 C23 1.35(3) C19 C20 1.41(3) C19 H19A 0.9300 C30 C31 1.40(3) C30 C29 1.41(3) C30 H30A 0.9300 C20 C21 1.36(3) C20 H20A 0.9300 C21 C22 1.34(3) C21 H21A 0.9300 C22 C23 1.43(3) C22 H22A 0.9300 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 C27 1.35(3) C26 H26A 0.9300 C27 C28 1.38(3) C27 H27A 0.9300 C28 C29 1.47(3) C31 C32 1.35(3) C31 H31A 0.9300 C32 C33 1.37(3) C32 H32A 0.9300 C33 C34 1.44(3) C34 C35 1.41(3) C35 C36 1.32(3) C35 H35A 0.9300 C36 H36A 0.9300 Fe2 N18 1.929(19) Fe2 N13 1.931(17) Fe2 N17 1.95(2) Fe2 N12 1.95(2) Fe2 N19 1.97(2) Fe2 N14 1.98(2) O3 C37 1.34(3) O3 C60 1.41(3) O4 C59 1.36(3) O4 C61 1.40(3) N11 N12 1.35(2) N11 C43 1.38(3) N11 H11B 0.8600 N12 C45 1.35(2) N13 C46 1.30(2) N13 C50 1.35(2) N14 N15 1.31(2) N14 C51 1.40(3) N15 C53 1.39(3) N15 H15A 0.8600 N16 C62 1.32(3) N16 N17 1.33(2) N16 H16B 0.8600 N17 C64 1.32(3) N18 C69 1.32(3) N18 C65 1.37(3) N19 C70 1.34(3) N19 N20 1.34(2) N20 C72 1.35(3) N20 H20B 0.8600 C37 C42 1.36(3) C37 C38 1.43(3) C38 C39 1.35(3) C38 H38A 0.9300 C39 C40 1.34(3) C39 H39A 0.9300 C40 C41 1.46(3) C40 H40A 0.9300 C41 C42 1.32(3) C41 H41A 0.9300 C42 C43 1.40(3) C43 C44 1.40(3) C44 C45 1.38(3) C44 H44A 0.9300 C45 C46 1.42(3) C46 C47 1.43(3) C47 C48 1.38(3) C47 H47A 0.9300 C48 C49 1.34(3) C48 H48A 0.9300 C49 C50 1.37(3) C49 H49A 0.9300 C50 C51 1.36(3) C51 C52 1.34(3) C52 C53 1.37(3) C52 H52A 0.9300 C53 C54 1.44(3) C54 C55 1.37(3) C54 C59 1.39(3) C55 C56 1.42(3) C55 H55A 0.9300 C56 C57 1.33(3) C56 H56A 0.9300 C57 C58 1.35(3) C57 H57A 0.9300 C58 C59 1.34(3) C58 H58A 0.9300 C60 H60A 0.9600 C60 H60B 0.9600 C60 H60C 0.9600 C61 H61A 0.9600 C61 H61B 0.9600 C61 H61C 0.9600 C62 C63 1.32(3) C62 H62A 0.9300 C63 C64 1.40(3) C63 H63A 0.9300 C64 C65 1.39(3) C65 C66 1.37(3) C66 C67 1.37(3) C66 H66A 0.9300 C67 C68 1.40(3) C67 H67A 0.9300 C68 C69 1.38(3) C68 H68A 0.9300 C69 C70 1.45(3) C70 C71 1.36(3) C71 C72 1.36(3) C71 H71A 0.9300 C72 H72A 0.9300 Cl1_1 O4_1 1.436(9) Cl1_1 O3_1 1.438(9) Cl1_1 O1_1 1.444(9) Cl1_1 O2_1 1.444(9) Cl1_2 O4_2 1.439(9) Cl1_2 O3_2 1.440(9) Cl1_2 O2_2 1.442(9) Cl1_2 O1_2 1.444(9) Cl1_3 O4_3 1.440(9) Cl1_3 O2_3 1.441(10) Cl1_3 O3_3 1.442(9) Cl1_3 O1_3 1.443(9) Cl1_4 O1_4 1.441(9) Cl1_4 O2_4 1.443(9) Cl1_4 O4_4 1.444(9) Cl1_4 O3_4 1.444(9) Cl1_5 O4_5 1.441(9) Cl1_5 O1_5 1.442(9) Cl1_5 O2_5 1.442(9) Cl1_5 O3_5 1.442(9) Cl1_6 O3_6 1.440(9) Cl1_6 O4_6 1.441(9) Cl1_6 O1_6 1.442(9) Cl1_6 O2_6 1.444(9) Cl1_7 O3_7 1.441(9) Cl1_7 O4_7 1.442(9) Cl1_7 O1_7 1.442(9) Cl1_7 O2_7 1.442(9) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.86 2.16 2.65(3) 116.0 . N1 H1A O2_2 0.86 2.58 3.19(4) 129.3 3_676 N1 H1A O3_2 0.86 2.37 3.16(4) 153.2 3_676 N1 H1A O2_3 0.86 1.96 2.68(4) 139.7 3_676 N5 H5B O2 0.86 1.95 2.51(3) 121.5 . N6 H6A Cl1_4 0.86 2.80 3.65(2) 168.2 3_576 N6 H6A O2_4 0.86 2.60 3.35(3) 145.1 3_576 N6 H6A O4_4 0.86 1.99 2.79(3) 152.9 3_576 N6 H6A O2_5 0.86 1.89 2.70(7) 155.8 3_576 N10 H10A Cl1_1 0.86 2.74 3.55(2) 157.2 3_676 N10 H10A O1_1 0.86 2.01 2.86(3) 170.7 3_676 N10 H10A O2_1 0.86 2.44 3.02(3) 125.6 3_676 C16 H16A O3_6 0.93 2.49 3.28(3) 143.0 4_576 C16 H16A O3_7 0.93 2.54 3.41(6) 155.8 4_576 C30 H30A O4_7 0.93 2.42 3.21(5) 142.1 3_576 C22 H22A O3_4 0.93 2.55 3.35(3) 143.3 4_586 C25 H25B O4_5 0.96 1.89 2.58(9) 126.3 4_586 C32 H32A O4_1 0.93 2.47 3.32(3) 152.4 4_586 N11 H11B O3 0.86 2.00 2.58(3) 123.2 . N15 H15A O4 0.86 2.17 2.62(3) 112.2 . N15 H15A Cl1_4 0.86 2.93 3.66(2) 144.0 . N15 H15A O1_4 0.86 2.25 3.08(3) 161.5 . N15 H15A O4_4 0.86 2.60 3.12(3) 119.9 . N15 H15A O1_5 0.86 2.15 2.94(6) 152.6 . N16 H16B Cl1_6 0.86 2.83 3.61(2) 150.7 . N16 H16B O1_6 0.86 1.94 2.79(3) 178.0 . N16 H16B Cl1_7 0.86 2.96 3.74(4) 152.3 . N16 H16B O1_7 0.86 2.22 3.06(6) 163.1 . N20 H20B Cl1_2 0.86 2.71 3.47(3) 149.4 . N20 H20B O1_2 0.86 2.02 2.86(4) 163.4 . N20 H20B O2_2 0.86 2.41 2.94(3) 120.4 . N20 H20B Cl1_3 0.86 2.62 3.42(3) 155.6 . N20 H20B O1_3 0.86 1.95 2.79(5) 166.8 . C38 H38A O2_2 0.93 2.53 3.34(4) 144.6 4_575 C47 H47A O4_1 0.93 2.48 3.16(3) 130.1 2_645 C60 H60B O4_3 0.96 2.46 2.98(4) 113.9 4_575 C61 H61B O3_5 0.96 2.65 3.23(8) 119.8 . C66 H66A O3_6 0.93 2.61 3.45(4) 150.9 2 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C7 N1 N2 C9 2(3) C7 N1 N2 Fe1 -172.2(19) C15 N4 N5 C17 0(2) Fe1 N4 N5 C17 -180.0(17) C26 N6 N7 C28 -6(3) C26 N6 N7 Fe1 -172.6(18) C34 N9 N10 C36 2(3) Fe1 N9 N10 C36 -169.5(16) C24 O1 C1 C6 178(3) C24 O1 C1 C2 -4(4) C6 C1 C2 C3 3(5) O1 C1 C2 C3 -175(3) C1 C2 C3 C4 -3(5) C2 C3 C4 C5 1(6) C3 C4 C5 C6 2(4) O1 C1 C6 C5 178(2) C2 C1 C6 C5 -1(6) O1 C1 C6 C7 -1(5) C2 C1 C6 C7 -179(3) C4 C5 C6 C1 -2(5) C4 C5 C6 C7 177(3) N2 N1 C7 C8 -1(3) N2 N1 C7 C6 179(2) C1 C6 C7 C8 168(3) C5 C6 C7 C8 -11(4) C1 C6 C7 N1 -12(5) C5 C6 C7 N1 170(2) N1 C7 C8 C9 -1(3) C6 C7 C8 C9 180(3) N1 N2 C9 C8 -2(3) Fe1 N2 C9 C8 173.3(15) N1 N2 C9 C10 -179(2) Fe1 N2 C9 C10 -3(3) C7 C8 C9 N2 2(3) C7 C8 C9 C10 177(3) C14 N3 C10 C9 -179(2) Fe1 N3 C10 C9 5(3) C14 N3 C10 C11 2(3) Fe1 N3 C10 C11 -174.8(17) N2 C9 C10 N3 -1(4) C8 C9 C10 N3 -176(2) N2 C9 C10 C11 178(2) C8 C9 C10 C11 3(5) N3 C10 C11 C12 0(4) C9 C10 C11 C12 -179(2) C10 C11 C12 C13 -2(4) C11 C12 C13 C14 2(4) C10 N3 C14 C13 -2(4) Fe1 N3 C14 C13 174.4(18) C10 N3 C14 C15 179(2) Fe1 N3 C14 C15 -4(3) C12 C13 C14 N3 0(4) C12 C13 C14 C15 179(2) N5 N4 C15 C16 0(3) Fe1 N4 C15 C16 180.0(15) N5 N4 C15 C14 177(2) Fe1 N4 C15 C14 -4(3) N3 C14 C15 N4 5(3) C13 C14 C15 N4 -174(2) N3 C14 C15 C16 -179(3) C13 C14 C15 C16 2(5) N4 C15 C16 C17 0(3) C14 C15 C16 C17 -176(3) N4 N5 C17 C16 0(3) N4 N5 C17 C18 -178.5(19) C15 C16 C17 N5 0(3) C15 C16 C17 C18 178(2) N5 C17 C18 C19 -170(2) C16 C17 C18 C19 11(4) N5 C17 C18 C23 19(4) C16 C17 C18 C23 -160(3) C23 C18 C19 C20 -7(4) C17 C18 C19 C20 -178(2) C18 C19 C20 C21 7(4) C19 C20 C21 C22 -3(4) C20 C21 C22 C23 0(4) C25 O2 C23 C18 171(3) C25 O2 C23 C22 -9(4) C19 C18 C23 O2 -176(2) C17 C18 C23 O2 -6(4) C19 C18 C23 C22 4(4) C17 C18 C23 C22 174(2) C21 C22 C23 O2 180(2) C21 C22 C23 C18 0(4) N7 N6 C26 C27 8(3) N6 C26 C27 C28 -7(3) N6 N7 C28 C27 1(3) Fe1 N7 C28 C27 171.4(15) N6 N7 C28 C29 -177(2) Fe1 N7 C28 C29 -7(3) C26 C27 C28 N7 3(3) C26 C27 C28 C29 -178(3) C33 N8 C29 C30 -8(4) Fe1 N8 C29 C30 177.6(18) C33 N8 C29 C28 176(2) Fe1 N8 C29 C28 2(3) C31 C30 C29 N8 9(4) C31 C30 C29 C28 -175(2) N7 C28 C29 N8 4(3) C27 C28 C29 N8 -174(3) N7 C28 C29 C30 -172(2) C27 C28 C29 C30 10(4) C29 C30 C31 C32 -7(4) C30 C31 C32 C33 4(4) C29 N8 C33 C32 5(4) Fe1 N8 C33 C32 179.3(16) C29 N8 C33 C34 -180(2) Fe1 N8 C33 C34 -6(3) C31 C32 C33 N8 -3(4) C31 C32 C33 C34 -178(2) N10 N9 C34 C35 -5(3) Fe1 N9 C34 C35 168.8(15) N10 N9 C34 C33 -175(2) Fe1 N9 C34 C33 -1(3) N8 C33 C34 N9 4(3) C32 C33 C34 N9 179(2) N8 C33 C34 C35 -163(2) C32 C33 C34 C35 12(4) N9 C34 C35 C36 6(3) C33 C34 C35 C36 174(3) C34 C35 C36 N10 -4(3) N9 N10 C36 C35 2(3) C43 N11 N12 C45 -3(3) C43 N11 N12 Fe2 -179.7(17) C51 N14 N15 C53 0(3) Fe2 N14 N15 C53 -172.8(18) C62 N16 N17 C64 2(3) C62 N16 N17 Fe2 -175.8(18) C70 N19 N20 C72 -1(2) Fe2 N19 N20 C72 -169.3(16) C60 O3 C37 C42 171(2) C60 O3 C37 C38 -9(4) O3 C37 C38 C39 -178(3) C42 C37 C38 C39 2(4) C37 C38 C39 C40 -1(5) C38 C39 C40 C41 0(4) C39 C40 C41 C42 1(4) C40 C41 C42 C37 0(4) C40 C41 C42 C43 178(2) O3 C37 C42 C41 179(2) C38 C37 C42 C41 -1(4) O3 C37 C42 C43 1(4) C38 C37 C42 C43 -179(2) N12 N11 C43 C44 1(3) N12 N11 C43 C42 -173(2) C41 C42 C43 N11 -174(2) C37 C42 C43 N11 4(4) C41 C42 C43 C44 14(4) C37 C42 C43 C44 -169(3) N11 C43 C44 C45 1(3) C42 C43 C44 C45 175(3) N11 N12 C45 C44 3(2) Fe2 N12 C45 C44 -179.3(14) N11 N12 C45 C46 178.5(18) Fe2 N12 C45 C46 -4(3) C43 C44 C45 N12 -2(3) C43 C44 C45 C46 -176(3) C50 N13 C46 C45 179(2) Fe2 N13 C46 C45 -1(3) C50 N13 C46 C47 1(4) Fe2 N13 C46 C47 -179.4(17) N12 C45 C46 N13 3(3) C44 C45 C46 N13 176(3) N12 C45 C46 C47 -179(2) C44 C45 C46 C47 -5(5) N13 C46 C47 C48 -4(4) C45 C46 C47 C48 178(3) C46 C47 C48 C49 5(4) C47 C48 C49 C50 -4(5) C46 N13 C50 C51 179(2) Fe2 N13 C50 C51 -1(3) C46 N13 C50 C49 0(4) Fe2 N13 C50 C49 -179.4(18) C48 C49 C50 N13 1(4) C48 C49 C50 C51 -177(3) N13 C50 C51 C52 -169(3) C49 C50 C51 C52 9(6) N13 C50 C51 N14 1(3) C49 C50 C51 N14 179(3) N15 N14 C51 C52 -2(3) Fe2 N14 C51 C52 173.0(16) N15 N14 C51 C50 -175(2) Fe2 N14 C51 C50 0(3) C50 C51 C52 C53 173(3) N14 C51 C52 C53 3(3) C51 C52 C53 N15 -3(3) C51 C52 C53 C54 179(3) N14 N15 C53 C52 2(3) N14 N15 C53 C54 -180(2) C52 C53 C54 C55 -23(4) N15 C53 C54 C55 160(2) C52 C53 C54 C59 145(3) N15 C53 C54 C59 -33(4) C59 C54 C55 C56 7(4) C53 C54 C55 C56 176(2) C54 C55 C56 C57 -4(4) C55 C56 C57 C58 5(5) C56 C57 C58 C59 -8(5) C57 C58 C59 O4 -178(3) C57 C58 C59 C54 10(5) C61 O4 C59 C58 3(4) C61 O4 C59 C54 175(2) C55 C54 C59 C58 -10(4) C53 C54 C59 C58 -177(3) C55 C54 C59 O4 177(2) C53 C54 C59 O4 9(4) N17 N16 C62 C63 -6(3) N16 C62 C63 C64 7(3) N16 N17 C64 C65 -177(2) Fe2 N17 C64 C65 1(3) N16 N17 C64 C63 2(3) Fe2 N17 C64 C63 -179.4(14) C62 C63 C64 N17 -5(3) C62 C63 C64 C65 174(3) C69 N18 C65 C66 3(4) Fe2 N18 C65 C66 -169.9(17) C69 N18 C65 C64 179(2) Fe2 N18 C65 C64 6(3) N17 C64 C65 N18 -5(3) C63 C64 C65 N18 176(2) N17 C64 C65 C66 170(3) C63 C64 C65 C66 -9(5) N18 C65 C66 C67 -1(4) C64 C65 C66 C67 -176(3) C65 C66 C67 C68 -2(4) C66 C67 C68 C69 2(4) C65 N18 C69 C68 -3(4) Fe2 N18 C69 C68 170.1(16) C65 N18 C69 C70 176(2) Fe2 N18 C69 C70 -11(3) C67 C68 C69 N18 0(3) C67 C68 C69 C70 -178(2) N20 N19 C70 C71 2(3) Fe2 N19 C70 C71 173.2(17) N20 N19 C70 C69 -178.1(19) Fe2 N19 C70 C69 -7(3) N18 C69 C70 N19 11(3) C68 C69 C70 N19 -170(2) N18 C69 C70 C71 -169(3) C68 C69 C70 C71 10(5) N19 C70 C71 C72 -2(3) C69 C70 C71 C72 178(3) N19 N20 C72 C71 0(3) C70 C71 C72 N20 1(3)