#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:25:44 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173540 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/18/1541897.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_1541897 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_sum 'C36 H30 Cl2 Fe N10 O10' _chemical_formula_weight 889.45 _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 _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 90.353(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.717(3) _cell_length_b 20.127(3) _cell_length_c 24.672(4) _cell_measurement_reflns_used 443 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 9.68 _cell_measurement_theta_min 3.56 _cell_volume 7804(2) _computing_cell_refinement 'SAINT V8.34A(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 SHELXT _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_orient_matrix_type 'Sparks (1982)' _diffrn_orient_matrix_UB_11 -0.00442 _diffrn_orient_matrix_UB_12 -0.01419 _diffrn_orient_matrix_UB_13 -0.03876 _diffrn_orient_matrix_UB_21 0.02481 _diffrn_orient_matrix_UB_22 0.04343 _diffrn_orient_matrix_UB_23 -0.01164 _diffrn_orient_matrix_UB_31 0.05842 _diffrn_orient_matrix_UB_32 -0.01952 _diffrn_orient_matrix_UB_33 0.00228 _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 0.1751 _diffrn_reflns_av_unetI/netI 0.1619 _diffrn_reflns_laue_measured_fraction_full 0.992 _diffrn_reflns_laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15377 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 15.947 _diffrn_reflns_theta_max 15.947 _diffrn_reflns_theta_min 2.768 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Sheldrick, 2012)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.514 _exptl_crystal_description block _exptl_crystal_F_000 3648 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.469 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1063 _refine_ls_number_reflns 2904 _refine_ls_number_restraints 1482 _refine_ls_restrained_S_all 0.890 _refine_ls_R_factor_all 0.1998 _refine_ls_R_factor_gt 0.1521 _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^)+(0.1724P)^2^+203.9031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3468 _refine_ls_wR_factor_ref 0.3892 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1715 _reflns_number_total 2904 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage1_Transient _cod_original_cell_volume 7805(2) _cod_database_code 1541897 _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 0.929 _shelx_estimated_absorpt_t_max 0.964 _shelx_res_file ; tminor.res created by SHELXL-2014/7 TITL tminor in P2(1)/c CELL 0.77490 15.7175 20.1267 24.6722 90.0000 90.3530 90.0000 ZERR 8.00 0.0025 0.0032 0.0037 0.0000 0.0099 0.0000 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 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -23 L.S. 10 SIZE 0.1 0.07 0.05 !dark red block BOND $H 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 FMAP 2 PLAN 20 RIGU HTAB ACTA 31.9 WGHT 0.172400 203.903107 FVAR 0.03912 RESI 1 CLO4 CL1 5 1.018007 0.876663 0.392630 11.00000 0.15069 0.19385 = 0.12105 0.01292 0.01537 0.00549 O1 4 1.105238 0.870652 0.385086 11.00000 0.15842 0.18530 = 0.10792 0.02921 0.01200 0.00449 O2 4 0.974456 0.853340 0.347556 11.00000 0.17014 0.23493 = 0.15356 -0.00411 -0.00283 0.01798 O3 4 0.996653 0.941783 0.403945 11.00000 0.17421 0.20067 = 0.20174 0.00312 0.01241 0.01062 O4 4 0.995721 0.837178 0.437043 11.00000 0.20141 0.21082 = 0.14081 0.01165 0.02707 -0.01160 RESI 2 CLO4 CL1 5 0.500065 0.911385 0.239371 11.00000 0.13892 0.19147 = 0.11480 0.02616 0.00582 -0.01993 O1 4 0.449766 0.855956 0.228651 11.00000 0.14125 0.19612 = 0.10969 0.01875 0.01090 -0.01998 O2 4 0.531023 0.936582 0.190945 11.00000 0.15088 0.21543 = 0.13781 0.04463 0.01719 -0.00080 O3 4 0.567646 0.892544 0.272573 11.00000 0.15751 0.17231 = 0.14443 0.03155 -0.01212 -0.03301 O4 4 0.451499 0.959385 0.264992 11.00000 0.18000 0.19995 = 0.14468 0.02298 0.02173 -0.00886 RESI 3 CLO4 CL1 5 0.002278 0.448628 0.371302 11.00000 0.18700 0.14581 = 0.12945 -0.00350 0.00727 -0.01237 O1 4 0.068450 0.492609 0.381611 11.00000 0.20195 0.14667 = 0.15051 0.01987 -0.01355 -0.01249 O2 4 0.033052 0.388751 0.351961 11.00000 0.20380 0.15805 = 0.20407 -0.01652 0.02277 -0.01683 O3 4 -0.052082 0.477172 0.333130 11.00000 0.22241 0.16785 = 0.17626 0.00113 -0.01744 -0.01525 O4 4 -0.042993 0.437255 0.418670 11.00000 0.25077 0.16956 = 0.17753 0.00604 0.04224 -0.00926 RESI 4 CLO4 CL1 5 0.503631 0.638829 0.491274 11.00000 0.18094 0.22155 = 0.07841 -0.01399 -0.01017 0.02309 O1 4 0.461695 0.616611 0.445215 11.00000 0.16689 0.19986 = 0.08097 -0.00496 0.00637 0.02038 O2 4 0.484271 0.705406 0.500251 11.00000 0.20187 0.23793 = 0.12943 -0.02921 -0.02548 0.02615 O3 4 0.478280 0.602487 0.536229 11.00000 0.24945 0.27146 = 0.10613 -0.00073 -0.00244 0.00491 O4 4 0.591054 0.632583 0.485195 11.00000 0.19348 0.28891 = 0.12101 -0.02996 -0.00995 0.02981 RESI 0 FE01 6 0.223809 0.684818 0.347435 11.00000 0.09757 0.11768 = 0.06673 0.01138 0.00780 0.00239 FE02 6 0.729869 0.734343 0.354858 11.00000 0.09866 0.12296 = 0.07623 0.00330 0.00756 -0.00658 O1 4 0.177115 0.867622 0.502378 11.00000 0.18541 0.15277 = 0.09741 0.00590 0.02220 -0.01446 O2 4 0.330449 0.721945 0.146937 11.00000 0.15603 0.16660 = 0.09261 0.00442 0.00301 -0.02041 O101 4 0.839602 0.582068 0.183229 11.00000 0.26095 0.14240 = 0.09317 -0.01667 0.03450 0.00478 O102 4 0.631522 0.752261 0.580073 11.00000 0.16751 0.17660 = 0.08565 0.01008 0.01017 0.00482 N1 3 0.164145 0.750045 0.452936 11.00000 0.09608 0.12668 = 0.07413 0.01034 0.00610 0.00570 AFIX 43 H1B 2 0.155012 0.789808 0.440354 11.00000 -1.20000 AFIX 0 N2 3 0.188585 0.698049 0.424054 11.00000 0.10295 0.12473 = 0.07163 0.01255 0.00719 0.00579 N3 3 0.248980 0.599777 0.374315 11.00000 0.08211 0.11743 = 0.07696 0.01149 0.00823 -0.00379 N4 3 0.273800 0.640562 0.284576 11.00000 0.09279 0.12731 = 0.07216 0.00811 0.00418 -0.00035 N5 3 0.289467 0.654066 0.232970 11.00000 0.11957 0.14280 = 0.07448 0.01156 0.00745 0.00418 AFIX 43 H5A 2 0.277659 0.692011 0.217802 11.00000 -1.20000 AFIX 0 N6 3 0.395718 0.734767 0.397150 11.00000 0.10531 0.13196 = 0.06078 0.00915 0.01361 -0.00420 AFIX 43 H6A 2 0.409829 0.700103 0.416258 11.00000 -1.20000 AFIX 0 N7 3 0.326248 0.737807 0.361928 11.00000 0.10248 0.12413 = 0.05929 0.00632 0.01432 -0.00080 N8 3 0.201587 0.765706 0.311688 11.00000 0.10611 0.11834 = 0.08099 0.01096 0.00803 0.00256 N9 3 0.108699 0.665977 0.321513 11.00000 0.09777 0.11970 = 0.07659 0.01079 0.00611 0.00295 N10 3 0.055728 0.615243 0.323958 11.00000 0.10163 0.12266 = 0.06838 0.00905 0.00454 0.00056 AFIX 43 H10C 2 0.065748 0.578026 0.340759 11.00000 -1.20000 AFIX 0 N101 3 0.786712 0.689269 0.231159 11.00000 0.10537 0.12688 = 0.07902 -0.00519 0.00581 -0.00601 AFIX 43 H10D 2 0.774764 0.647344 0.235083 11.00000 -1.20000 AFIX 0 N102 3 0.777073 0.733691 0.271069 11.00000 0.08801 0.12135 = 0.07047 -0.00017 0.00253 -0.00273 N103 3 0.765315 0.831103 0.335955 11.00000 0.08752 0.12260 = 0.07248 -0.00020 0.00124 -0.00197 N104 3 0.697430 0.795827 0.426486 11.00000 0.08671 0.13150 = 0.07313 0.00353 -0.00350 0.00532 N105 3 0.665645 0.788630 0.477398 11.00000 0.11859 0.14672 = 0.07867 0.00398 0.00846 0.00127 AFIX 43 H10E 2 0.646235 0.751977 0.491341 11.00000 -1.20000 AFIX 0 N106 3 0.913990 0.711513 0.415260 11.00000 0.10393 0.13294 = 0.10038 0.00411 -0.00269 -0.00131 AFIX 43 H10F 2 0.932755 0.751865 0.411216 11.00000 -1.20000 AFIX 0 N107 3 0.839411 0.691646 0.393112 11.00000 0.09733 0.12854 = 0.07776 0.00135 0.00811 -0.00025 N108 3 0.704544 0.633712 0.367238 11.00000 0.09310 0.12224 = 0.07460 -0.00552 0.01319 0.00140 N109 3 0.606262 0.717584 0.323168 11.00000 0.09282 0.12474 = 0.08077 -0.00284 0.00877 -0.00443 N110 3 0.550160 0.750026 0.292316 11.00000 0.09958 0.12837 = 0.08866 -0.00501 0.00370 -0.00498 AFIX 43 H11A 2 0.553316 0.792146 0.284661 11.00000 -1.20000 AFIX 0 C1 1 0.188557 0.939042 0.494499 11.00000 0.31727 0.15017 = 0.12522 0.00320 0.07317 -0.02351 AFIX 33 H1A 2 0.214585 0.946992 0.459548 11.00000 -1.50000 H1C 2 0.133659 0.960987 0.495752 11.00000 -1.50000 H1D 2 0.225020 0.956538 0.522969 11.00000 -1.50000 AFIX 0 C2 1 0.139942 0.844623 0.551010 11.00000 0.14825 0.14151 = 0.09329 0.00632 0.01287 0.00393 C3 1 0.113511 0.886772 0.592950 11.00000 0.20531 0.14933 = 0.10963 -0.00261 0.03896 -0.00266 AFIX 43 H3A 2 0.118692 0.933256 0.591298 11.00000 -1.20000 AFIX 0 C4 1 0.079590 0.854357 0.636393 11.00000 0.16626 0.14869 = 0.10363 -0.00038 0.02000 -0.00191 AFIX 43 H4A 2 0.063770 0.879988 0.666544 11.00000 -1.20000 AFIX 0 C5 1 0.066881 0.786309 0.639102 11.00000 0.17183 0.14884 = 0.09626 -0.00299 0.03505 -0.00329 AFIX 43 H5B 2 0.041212 0.766571 0.669414 11.00000 -1.20000 AFIX 0 C6 1 0.093354 0.748562 0.595576 11.00000 0.15503 0.14282 = 0.08251 0.00621 0.02169 0.00183 AFIX 43 H6B 2 0.088947 0.702063 0.597761 11.00000 -1.20000 AFIX 0 C7 1 0.126275 0.776649 0.548643 11.00000 0.09979 0.14005 = 0.07650 0.00830 0.00333 0.01017 C8 1 0.155494 0.730571 0.506700 11.00000 0.11407 0.13317 = 0.07437 0.01248 0.00745 0.01068 C9 1 0.178378 0.667291 0.507267 11.00000 0.09210 0.13329 = 0.07580 0.01352 0.00874 0.00664 AFIX 43 H9A 2 0.179481 0.640290 0.538350 11.00000 -1.20000 AFIX 0 C10 1 0.200593 0.646201 0.455509 11.00000 0.11738 0.12817 = 0.07354 0.01701 0.01300 0.01241 C11 1 0.234458 0.589388 0.430756 11.00000 0.09439 0.12522 = 0.07791 0.01476 0.00924 0.00355 C12 1 0.252077 0.528834 0.453761 11.00000 0.16229 0.13379 = 0.08829 0.02378 0.02531 0.02709 AFIX 43 H12A 2 0.241262 0.521523 0.490712 11.00000 -1.20000 AFIX 0 C13 1 0.284850 0.480096 0.423182 11.00000 0.19360 0.14238 = 0.09613 0.02226 0.02936 0.03946 AFIX 43 H13A 2 0.296078 0.438648 0.439264 11.00000 -1.20000 AFIX 0 C14 1 0.303154 0.489028 0.367311 11.00000 0.15687 0.13331 = 0.09257 0.01729 0.01993 0.02399 AFIX 43 H14A 2 0.324483 0.454169 0.345987 11.00000 -1.20000 AFIX 0 C15 1 0.288361 0.550384 0.346144 11.00000 0.11485 0.12833 = 0.08212 0.01052 0.01145 0.01207 C16 1 0.293748 0.578769 0.291444 11.00000 0.07256 0.12678 = 0.07769 0.00567 -0.00139 -0.00670 C17 1 0.333405 0.552470 0.244372 11.00000 0.10062 0.14288 = 0.08092 0.00582 0.00690 0.00462 AFIX 43 H17A 2 0.358940 0.510569 0.240163 11.00000 -1.20000 AFIX 0 C18 1 0.325875 0.602445 0.206291 11.00000 0.08281 0.14238 = 0.07749 0.00283 -0.00572 -0.00962 C19 1 0.357390 0.605397 0.148056 11.00000 0.10636 0.16409 = 0.07661 -0.00018 -0.00160 -0.02158 C20 1 0.386750 0.545376 0.126275 11.00000 0.15108 0.17110 = 0.08797 -0.00117 0.00984 -0.00748 AFIX 43 H20A 2 0.386822 0.504709 0.145010 11.00000 -1.20000 AFIX 0 C21 1 0.417002 0.553709 0.071291 11.00000 0.15460 0.18058 = 0.08921 -0.00470 0.01135 -0.02285 AFIX 43 H21A 2 0.440314 0.516849 0.053301 11.00000 -1.20000 AFIX 0 C22 1 0.413037 0.610863 0.045687 11.00000 0.22326 0.18447 = 0.09774 0.00186 0.02114 -0.01199 AFIX 43 H22A 2 0.429003 0.610802 0.009033 11.00000 -1.20000 AFIX 0 C23 1 0.388258 0.669906 0.066763 11.00000 0.17399 0.17948 = 0.09040 0.00332 0.01202 -0.02223 AFIX 43 H23A 2 0.391637 0.709349 0.046488 11.00000 -1.20000 AFIX 0 C24 1 0.356893 0.669919 0.120822 11.00000 0.13685 0.16709 = 0.08499 0.00488 -0.00342 -0.02320 C25 1 0.336530 0.786076 0.121464 11.00000 0.17186 0.17060 = 0.11352 0.01518 0.01898 -0.01791 AFIX 33 H25A 2 0.314484 0.819795 0.145706 11.00000 -1.50000 H25B 2 0.395612 0.795632 0.113430 11.00000 -1.50000 H25C 2 0.303592 0.786028 0.088087 11.00000 -1.50000 AFIX 0 C26 1 0.437614 0.792412 0.397511 11.00000 0.12441 0.13568 = 0.08484 0.01643 -0.00419 -0.01348 AFIX 43 H26A 2 0.486116 0.802537 0.418406 11.00000 -1.20000 AFIX 0 C27 1 0.397806 0.833458 0.362509 11.00000 0.11363 0.13124 = 0.06402 0.00549 0.01194 -0.00374 AFIX 43 H27A 2 0.414918 0.876768 0.353382 11.00000 -1.20000 AFIX 0 C28 1 0.325319 0.799534 0.341867 11.00000 0.11302 0.12577 = 0.07005 0.00940 0.00955 -0.00311 C29 1 0.256507 0.817129 0.305679 11.00000 0.10434 0.11602 = 0.05346 0.00028 0.02140 0.00477 C30 1 0.245768 0.870061 0.271389 11.00000 0.11072 0.11896 = 0.06711 0.00769 0.01423 0.00211 AFIX 43 H30A 2 0.288302 0.902329 0.266607 11.00000 -1.20000 AFIX 0 C31 1 0.171607 0.873073 0.245281 11.00000 0.11583 0.12807 = 0.08272 0.02010 0.00523 -0.00284 AFIX 43 H31A 2 0.161443 0.909696 0.222501 11.00000 -1.20000 AFIX 0 C32 1 0.109797 0.826429 0.249586 11.00000 0.11326 0.12633 = 0.08727 0.01996 0.00432 -0.00028 AFIX 43 H32A 2 0.058419 0.831514 0.230328 11.00000 -1.20000 AFIX 0 C33 1 0.122731 0.768799 0.283775 11.00000 0.09893 0.11311 = 0.05289 -0.00267 0.02279 0.01087 C34 1 0.071723 0.710207 0.291506 11.00000 0.10027 0.12209 = 0.07937 0.01431 0.00468 0.00271 C35 1 -0.008732 0.690366 0.275679 11.00000 0.10322 0.13022 = 0.08726 0.02128 0.00115 -0.00171 AFIX 43 H35A 2 -0.049245 0.713782 0.255011 11.00000 -1.20000 AFIX 0 C36 1 -0.014664 0.629481 0.297097 11.00000 0.10077 0.12878 = 0.07794 0.01804 0.00238 -0.00202 AFIX 43 H36A 2 -0.061907 0.601145 0.293524 11.00000 -1.20000 AFIX 0 C101 1 0.857826 0.514121 0.187443 11.00000 0.46907 0.15210 = 0.10345 -0.00677 0.07978 0.05142 AFIX 33 H10A 2 0.845810 0.499046 0.223945 11.00000 -1.50000 H10B 2 0.822860 0.489610 0.161816 11.00000 -1.50000 H10L 2 0.917427 0.506662 0.179485 11.00000 -1.50000 AFIX 0 C102 1 0.853133 0.611422 0.134005 11.00000 0.19652 0.14549 = 0.09229 -0.01456 0.02186 0.00382 C103 1 0.883710 0.577290 0.090025 11.00000 0.19437 0.15513 = 0.09015 -0.01857 0.01499 0.00828 AFIX 43 H10G 2 0.897435 0.531882 0.091814 11.00000 -1.20000 AFIX 0 C104 1 0.892696 0.612331 0.044844 11.00000 0.17147 0.15723 = 0.09198 -0.01539 0.01287 0.00963 AFIX 43 H10H 2 0.908810 0.589887 0.013112 11.00000 -1.20000 AFIX 0 C105 1 0.879549 0.680199 0.042095 11.00000 0.15707 0.15774 = 0.08586 -0.01528 0.01309 0.00654 AFIX 43 H10I 2 0.889076 0.702325 0.009133 11.00000 -1.20000 AFIX 0 C106 1 0.852086 0.717383 0.087619 11.00000 0.15053 0.15051 = 0.08514 -0.01116 0.01788 -0.00003 AFIX 43 H10J 2 0.842873 0.763509 0.086471 11.00000 -1.20000 AFIX 0 C107 1 0.839755 0.678671 0.135094 11.00000 0.14041 0.14400 = 0.08439 -0.01484 0.01277 -0.00614 C108 1 0.816777 0.715053 0.183847 11.00000 0.09870 0.13142 = 0.07681 -0.00596 0.00446 -0.00564 C109 1 0.827454 0.782180 0.195543 11.00000 0.08466 0.12986 = 0.06801 -0.00066 -0.00185 -0.00290 AFIX 43 H10K 2 0.849564 0.814852 0.172331 11.00000 -1.20000 AFIX 0 C110 1 0.798431 0.791714 0.249397 11.00000 0.10857 0.12266 = 0.07268 -0.00205 0.00900 -0.00682 C111 1 0.797628 0.848499 0.283595 11.00000 0.09374 0.12026 = 0.07215 0.00072 0.00123 -0.00111 C112 1 0.824775 0.913342 0.272087 11.00000 0.09778 0.12068 = 0.07901 0.00050 0.00423 -0.00304 AFIX 43 H11B 2 0.846577 0.923888 0.237753 11.00000 -1.20000 AFIX 0 C113 1 0.819415 0.958977 0.309664 11.00000 0.12421 0.12367 = 0.08247 -0.00374 0.01140 -0.00644 AFIX 43 H11C 2 0.839464 1.001912 0.301888 11.00000 -1.20000 AFIX 0 C114 1 0.785567 0.946874 0.360325 11.00000 0.09905 0.12499 = 0.07800 -0.00085 0.00142 0.00005 AFIX 43 H11D 2 0.781702 0.980326 0.386783 11.00000 -1.20000 AFIX 0 C115 1 0.757097 0.881312 0.370067 11.00000 0.09526 0.12350 = 0.07333 -0.00115 -0.00123 0.00200 C116 1 0.720135 0.862121 0.421848 11.00000 0.07848 0.13086 = 0.07155 0.00275 -0.00735 0.00663 C117 1 0.702846 0.892687 0.468925 11.00000 0.12960 0.14130 = 0.07782 -0.00295 0.01055 -0.00140 AFIX 43 H11E 2 0.712718 0.937767 0.476688 11.00000 -1.20000 AFIX 0 C118 1 0.669484 0.848524 0.502628 11.00000 0.10738 0.14525 = 0.07784 0.00399 0.00388 0.00585 C119 1 0.645160 0.859845 0.563245 11.00000 0.13686 0.17043 = 0.07973 0.00189 0.01239 0.00272 C120 1 0.641292 0.929525 0.577937 11.00000 0.17597 0.17010 = 0.08793 -0.00262 0.03229 0.00085 AFIX 43 H12B 2 0.651291 0.962397 0.551672 11.00000 -1.20000 AFIX 0 C121 1 0.622995 0.947399 0.630290 11.00000 0.26881 0.18679 = 0.09662 -0.00784 0.05501 -0.01053 AFIX 43 H12C 2 0.625193 0.991226 0.643391 11.00000 -1.20000 AFIX 0 C122 1 0.600537 0.891967 0.661919 11.00000 0.17159 0.19127 = 0.09649 0.00308 0.02903 -0.00137 AFIX 43 H12D 2 0.582832 0.904357 0.696810 11.00000 -1.20000 AFIX 0 C123 1 0.597866 0.821354 0.654317 11.00000 0.14470 0.19110 = 0.08703 0.00456 0.01189 -0.00164 AFIX 43 H12E 2 0.584169 0.787680 0.679180 11.00000 -1.20000 AFIX 0 C124 1 0.621369 0.816157 0.599407 11.00000 0.11221 0.17964 = 0.08535 0.00976 0.00362 0.00188 C125 1 0.611293 0.698705 0.616406 11.00000 0.24084 0.19013 = 0.11216 0.02410 0.01621 -0.01016 AFIX 33 H12H 2 0.620887 0.656573 0.598357 11.00000 -1.50000 H12I 2 0.647273 0.701525 0.648407 11.00000 -1.50000 H12J 2 0.552083 0.701908 0.626949 11.00000 -1.50000 AFIX 0 C126 1 0.958128 0.665647 0.444045 11.00000 0.10877 0.13594 = 0.11175 0.00951 -0.01082 -0.00358 AFIX 43 H12F 2 1.010593 0.669408 0.462282 11.00000 -1.20000 AFIX 0 C127 1 0.907575 0.615068 0.439345 11.00000 0.10369 0.13182 = 0.09032 0.00209 0.00175 0.00068 AFIX 43 H12G 2 0.919547 0.573508 0.455012 11.00000 -1.20000 AFIX 0 C128 1 0.835241 0.627158 0.409661 11.00000 0.09573 0.12671 = 0.06827 -0.00291 0.01541 0.00361 C129 1 0.756231 0.591725 0.392754 11.00000 0.09586 0.12372 = 0.06191 -0.00642 0.01937 0.00395 C130 1 0.745162 0.523460 0.401311 11.00000 0.10876 0.12483 = 0.09563 0.00072 0.00418 0.00033 AFIX 43 H13B 2 0.787408 0.495618 0.416016 11.00000 -1.20000 AFIX 0 C131 1 0.665805 0.501666 0.385859 11.00000 0.11265 0.13139 = 0.11516 0.00632 -0.00293 -0.00413 AFIX 43 H13C 2 0.651702 0.456951 0.392154 11.00000 -1.20000 AFIX 0 C132 1 0.608908 0.539932 0.362849 11.00000 0.11613 0.13161 = 0.15513 0.01738 -0.02030 -0.01204 AFIX 43 H13D 2 0.555522 0.522906 0.352538 11.00000 -1.20000 AFIX 0 C133 1 0.628598 0.605254 0.354072 11.00000 0.09229 0.12511 = 0.07174 -0.00585 0.01824 -0.00052 C134 1 0.574681 0.653977 0.324327 11.00000 0.08489 0.12288 = 0.06001 -0.01098 0.02255 -0.00093 C135 1 0.500112 0.650549 0.292989 11.00000 0.10412 0.12857 = 0.11320 0.00017 -0.00943 -0.00724 AFIX 43 H13E 2 0.465631 0.613173 0.286572 11.00000 -1.20000 AFIX 0 C136 1 0.489332 0.710286 0.274871 11.00000 0.10283 0.13012 = 0.10337 -0.00235 -0.00501 -0.00635 AFIX 43 H13F 2 0.444086 0.723565 0.252255 11.00000 -1.20000 AFIX 0 HKLF 4 REM tminor in P2(1)/c REM R1 = 0.1521 for 1715 Fo > 4sig(Fo) and 0.1998 for all 2904 data REM 1063 parameters refined using 1482 restraints END WGHT 0.1722 204.4107 REM Instructions for potential hydrogen bonds EQIV $1 x-1, y, z HTAB_1 N1_0 O1_$1 HTAB N1 O1 HTAB N5 O2 HTAB N6 Cl1_4 HTAB N6 O1_4 HTAB N6 O2_4 HTAB N10 Cl1_3 HTAB N10 O1_3 HTAB N101 O101 HTAB N105 O4_4 HTAB N105 O102 HTAB N106 Cl1_1 HTAB N106 O4_1 HTAB N110 Cl1_2 HTAB N110 O1_2 HTAB N110 O3_2 EQIV $2 -x+1, y-1/2, -z+1/2 HTAB_2 C14_0 O2_$2 EQIV $3 x, -y+3/2, z-1/2 HTAB_4 C23_0 O2_$3 HTAB C35 N101_$1 EQIV $4 -x+2, y-1/2, -z+1/2 HTAB_1 C103_0 O3_$4 EQIV $5 -x+1, y+1/2, -z+1/2 HTAB_3 C109_0 O2_$5 HTAB_2 C132_0 O2_$2 REM Highest difference peak 0.469, deepest hole -0.451, 1-sigma level 0.095 Q1 1 0.7214 0.6608 0.3475 11.00000 0.05 0.47 Q2 1 0.4914 0.6268 0.4835 11.00000 0.05 0.46 Q3 1 0.2367 0.7685 0.3463 11.00000 0.05 0.45 Q4 1 1.0188 0.8968 0.3796 11.00000 0.05 0.45 Q5 1 0.5535 0.5687 0.5005 11.00000 0.05 0.44 Q6 1 0.0654 0.3810 0.3986 11.00000 0.05 0.43 Q7 1 0.9910 0.9376 0.4370 11.00000 0.05 0.35 Q8 1 0.4989 0.9348 0.2484 11.00000 0.05 0.35 Q9 1 0.0141 0.4367 0.3776 11.00000 0.05 0.33 Q10 1 -0.0984 0.4335 0.3827 11.00000 0.05 0.31 Q11 1 0.4759 0.8340 0.2378 11.00000 0.05 0.30 Q12 1 0.1422 0.7344 0.5166 11.00000 0.05 0.28 Q13 1 0.9267 0.8563 0.3988 11.00000 0.05 0.28 Q14 1 0.2213 0.6111 0.3576 11.00000 0.05 0.28 Q15 1 0.9454 0.8302 0.3836 11.00000 0.05 0.28 Q16 1 0.1630 0.7342 0.4865 11.00000 0.05 0.27 Q17 1 0.4366 0.6677 0.5329 11.00000 0.05 0.27 Q18 1 0.9614 0.8151 0.3678 11.00000 0.05 0.27 Q19 1 0.4118 0.6532 0.5208 11.00000 0.05 0.26 Q20 1 0.1182 0.6663 0.3334 11.00000 0.05 0.26 ; _shelx_res_checksum 22859 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 Cl1_1 Cl 1.0180(9) 0.8767(7) 0.3926(5) 0.155(6) Uani 1 1 d D U O1_1 O 1.1052(11) 0.8707(13) 0.3851(10) 0.150(10) Uani 1 1 d D U O2_1 O 0.9745(16) 0.8533(14) 0.3476(9) 0.186(11) Uani 1 1 d D U O3_1 O 0.9967(17) 0.9418(9) 0.4039(12) 0.192(12) Uani 1 1 d D U O4_1 O 0.9957(17) 0.8372(12) 0.4370(9) 0.184(11) Uani 1 1 d D U Cl1_2 Cl 0.5001(8) 0.9114(7) 0.2394(5) 0.148(6) Uani 1 1 d D U O1_2 O 0.4498(14) 0.8560(10) 0.2287(9) 0.149(10) Uani 1 1 d D U O2_2 O 0.5310(16) 0.9366(13) 0.1909(8) 0.168(11) Uani 1 1 d D U O3_2 O 0.5676(13) 0.8925(12) 0.2726(9) 0.158(10) Uani 1 1 d D U O4_2 O 0.4515(16) 0.9594(11) 0.2650(10) 0.175(11) Uani 1 1 d D U Cl1_3 Cl 0.0023(9) 0.4486(7) 0.3713(5) 0.154(6) Uani 1 1 d D U O1_3 O 0.0684(14) 0.4926(12) 0.3816(11) 0.166(11) Uani 1 1 d D U O2_3 O 0.0331(17) 0.3888(10) 0.3520(11) 0.189(12) Uani 1 1 d D U O3_3 O -0.0521(16) 0.4772(13) 0.3331(10) 0.189(11) Uani 1 1 d D U O4_3 O -0.0430(18) 0.4373(14) 0.4187(9) 0.199(12) Uani 1 1 d D U Cl1_4 Cl 0.5036(9) 0.6388(7) 0.4913(5) 0.160(6) Uani 1 1 d D U O1_4 O 0.4617(15) 0.6166(12) 0.4452(8) 0.149(10) Uani 1 1 d D U O2_4 O 0.4843(19) 0.7054(9) 0.5003(11) 0.190(12) Uani 1 1 d D U O3_4 O 0.4783(19) 0.6025(13) 0.5362(9) 0.209(12) Uani 1 1 d D U O4_4 O 0.5911(12) 0.6326(15) 0.4852(11) 0.201(12) Uani 1 1 d D U Fe01 Fe 0.2238(4) 0.6848(3) 0.3474(2) 0.094(3) Uani 1 1 d . U Fe02 Fe 0.7299(4) 0.7343(3) 0.3549(2) 0.099(3) Uani 1 1 d . U O1 O 0.177(2) 0.8676(18) 0.5024(13) 0.145(11) Uani 1 1 d . U O2 O 0.330(2) 0.722(2) 0.1469(13) 0.138(11) Uani 1 1 d . U O101 O 0.840(2) 0.582(2) 0.1832(14) 0.165(14) Uani 1 1 d . U O102 O 0.632(2) 0.752(2) 0.5801(13) 0.143(11) Uani 1 1 d . U N1 N 0.1641(19) 0.7500(18) 0.4529(13) 0.099(10) Uani 1 1 d . U H1B H 0.1550 0.7898 0.4404 0.119 Uiso 1 1 calc R U N2 N 0.189(2) 0.698(2) 0.4241(14) 0.100(8) Uani 1 1 d . U N3 N 0.249(2) 0.5998(18) 0.3743(14) 0.092(7) Uani 1 1 d . U N4 N 0.274(2) 0.641(2) 0.2846(15) 0.097(7) Uani 1 1 d . U N5 N 0.289(2) 0.6541(19) 0.2330(15) 0.112(11) Uani 1 1 d . U H5A H 0.2777 0.6920 0.2178 0.135 Uiso 1 1 calc R U N6 N 0.396(2) 0.7348(19) 0.3972(12) 0.099(9) Uani 1 1 d . U H6A H 0.4098 0.7001 0.4163 0.119 Uiso 1 1 calc R U N7 N 0.326(2) 0.7378(19) 0.3619(13) 0.095(7) Uani 1 1 d . U N8 N 0.202(2) 0.7657(19) 0.3117(13) 0.102(7) Uani 1 1 d . U N9 N 0.109(2) 0.666(2) 0.3215(13) 0.098(7) Uani 1 1 d . U N10 N 0.056(2) 0.6152(18) 0.3240(12) 0.098(10) Uani 1 1 d . U H10C H 0.0657 0.5780 0.3408 0.117 Uiso 1 1 calc R U N101 N 0.787(2) 0.6893(18) 0.2312(15) 0.104(10) Uani 1 1 d . U H10D H 0.7748 0.6473 0.2351 0.124 Uiso 1 1 calc R U N102 N 0.7771(19) 0.734(2) 0.2711(14) 0.093(8) Uani 1 1 d . U N103 N 0.7653(19) 0.8311(18) 0.3360(15) 0.094(8) Uani 1 1 d . U N104 N 0.697(2) 0.7958(19) 0.4265(14) 0.097(8) Uani 1 1 d . U N105 N 0.666(2) 0.789(2) 0.4774(15) 0.115(11) Uani 1 1 d . U H10E H 0.6462 0.7520 0.4913 0.138 Uiso 1 1 calc R U N106 N 0.914(2) 0.7115(19) 0.4153(14) 0.112(11) Uani 1 1 d . U H10F H 0.9328 0.7519 0.4112 0.135 Uiso 1 1 calc R U N107 N 0.839(2) 0.692(2) 0.3931(13) 0.101(8) Uani 1 1 d . U N108 N 0.705(3) 0.6337(18) 0.3672(13) 0.097(8) Uani 1 1 d . U N109 N 0.606(2) 0.718(2) 0.3232(13) 0.099(8) Uani 1 1 d . U N110 N 0.550(2) 0.7500(19) 0.2923(13) 0.106(10) Uani 1 1 d . U H11A H 0.5533 0.7921 0.2847 0.127 Uiso 1 1 calc R U C1 C 0.189(4) 0.939(3) 0.494(2) 0.20(3) Uani 1 1 d . U H1A H 0.2146 0.9470 0.4595 0.296 Uiso 1 1 calc R U H1C H 0.1337 0.9610 0.4958 0.296 Uiso 1 1 calc R U H1D H 0.2250 0.9565 0.5230 0.296 Uiso 1 1 calc R U C2 C 0.140(3) 0.845(3) 0.551(2) 0.128(16) Uani 1 1 d . U C3 C 0.114(3) 0.887(3) 0.593(2) 0.155(19) Uani 1 1 d . U H3A H 0.1187 0.9333 0.5913 0.186 Uiso 1 1 calc R U C4 C 0.080(3) 0.854(3) 0.636(2) 0.139(18) Uani 1 1 d . U H4A H 0.0638 0.8800 0.6665 0.167 Uiso 1 1 calc R U C5 C 0.067(3) 0.786(3) 0.639(2) 0.139(18) Uani 1 1 d . U H5B H 0.0412 0.7666 0.6694 0.167 Uiso 1 1 calc R U C6 C 0.093(3) 0.749(3) 0.5956(19) 0.127(15) Uani 1 1 d . U H6B H 0.0889 0.7021 0.5978 0.152 Uiso 1 1 calc R U C7 C 0.126(3) 0.777(3) 0.549(2) 0.105(12) Uani 1 1 d . U C8 C 0.155(3) 0.731(3) 0.507(2) 0.107(13) Uani 1 1 d . U C9 C 0.178(2) 0.667(2) 0.5073(19) 0.100(12) Uani 1 1 d . U H9A H 0.1795 0.6403 0.5384 0.120 Uiso 1 1 calc R U C10 C 0.201(3) 0.646(3) 0.456(2) 0.106(14) Uani 1 1 d . U C11 C 0.234(3) 0.589(3) 0.4308(19) 0.099(12) Uani 1 1 d . U C12 C 0.252(3) 0.529(3) 0.454(2) 0.128(17) Uani 1 1 d . U H12A H 0.2413 0.5215 0.4907 0.154 Uiso 1 1 calc R U C13 C 0.285(3) 0.480(3) 0.423(2) 0.144(19) Uani 1 1 d . U H13A H 0.2961 0.4386 0.4393 0.173 Uiso 1 1 calc R U C14 C 0.303(3) 0.489(3) 0.3673(19) 0.128(16) Uani 1 1 d . U H14A H 0.3245 0.4542 0.3460 0.153 Uiso 1 1 calc R U C15 C 0.288(3) 0.550(3) 0.346(2) 0.108(13) Uani 1 1 d . U C16 C 0.294(3) 0.579(3) 0.291(2) 0.092(11) Uani 1 1 d . U C17 C 0.333(3) 0.552(2) 0.2444(17) 0.108(13) Uani 1 1 d . U H17A H 0.3589 0.5106 0.2402 0.130 Uiso 1 1 calc R U C18 C 0.326(3) 0.602(3) 0.206(2) 0.101(12) Uani 1 1 d . U C19 C 0.357(3) 0.605(3) 0.148(2) 0.116(13) Uani 1 1 d . U C20 C 0.387(3) 0.545(3) 0.126(2) 0.137(16) Uani 1 1 d . U H20A H 0.3868 0.5047 0.1450 0.164 Uiso 1 1 calc R U C21 C 0.417(3) 0.554(3) 0.071(2) 0.141(16) Uani 1 1 d . U H21A H 0.4403 0.5168 0.0533 0.170 Uiso 1 1 calc R U C22 C 0.413(4) 0.611(3) 0.046(2) 0.17(2) Uani 1 1 d . U H22A H 0.4290 0.6108 0.0090 0.202 Uiso 1 1 calc R U C23 C 0.388(3) 0.670(3) 0.067(2) 0.148(17) Uani 1 1 d . U H23A H 0.3916 0.7093 0.0465 0.177 Uiso 1 1 calc R U C24 C 0.357(3) 0.670(3) 0.121(3) 0.130(16) Uani 1 1 d . U C25 C 0.337(3) 0.786(3) 0.1215(18) 0.152(18) Uani 1 1 d . U H25A H 0.3145 0.8198 0.1457 0.228 Uiso 1 1 calc R U H25B H 0.3956 0.7956 0.1134 0.228 Uiso 1 1 calc R U H25C H 0.3036 0.7860 0.0881 0.228 Uiso 1 1 calc R U C26 C 0.438(3) 0.792(2) 0.3975(18) 0.115(15) Uani 1 1 d . U H26A H 0.4861 0.8025 0.4184 0.138 Uiso 1 1 calc R U C27 C 0.398(3) 0.833(2) 0.3625(16) 0.103(12) Uani 1 1 d . U H27A H 0.4149 0.8768 0.3534 0.124 Uiso 1 1 calc R U C28 C 0.325(3) 0.800(3) 0.3419(18) 0.103(12) Uani 1 1 d . U C29 C 0.257(3) 0.817(3) 0.3057(17) 0.091(11) Uani 1 1 d . U C30 C 0.246(3) 0.870(2) 0.2714(16) 0.099(12) Uani 1 1 d . U H30A H 0.2883 0.9023 0.2666 0.119 Uiso 1 1 calc R U C31 C 0.172(3) 0.873(2) 0.2453(17) 0.109(14) Uani 1 1 d . U H31A H 0.1614 0.9097 0.2225 0.131 Uiso 1 1 calc R U C32 C 0.110(3) 0.826(2) 0.2496(17) 0.109(13) Uani 1 1 d . U H32A H 0.0584 0.8315 0.2303 0.131 Uiso 1 1 calc R U C33 C 0.123(3) 0.769(3) 0.2838(16) 0.088(10) Uani 1 1 d . U C34 C 0.072(3) 0.710(3) 0.2915(17) 0.101(13) Uani 1 1 d . U C35 C -0.009(3) 0.690(2) 0.2757(17) 0.107(13) Uani 1 1 d . U H35A H -0.0492 0.7138 0.2550 0.128 Uiso 1 1 calc R U C36 C -0.015(3) 0.629(2) 0.2971(16) 0.102(13) Uani 1 1 d . U H36A H -0.0619 0.6011 0.2935 0.123 Uiso 1 1 calc R U C101 C 0.858(5) 0.514(3) 0.187(2) 0.24(4) Uani 1 1 d . U H10A H 0.8458 0.4990 0.2239 0.362 Uiso 1 1 calc R U H10B H 0.8229 0.4896 0.1618 0.362 Uiso 1 1 calc R U H10L H 0.9174 0.5067 0.1795 0.362 Uiso 1 1 calc R U C102 C 0.853(3) 0.611(3) 0.134(3) 0.145(18) Uani 1 1 d . U C103 C 0.884(3) 0.577(3) 0.090(2) 0.146(18) Uani 1 1 d . U H10G H 0.8974 0.5319 0.0918 0.176 Uiso 1 1 calc R U C104 C 0.893(3) 0.612(3) 0.045(2) 0.140(18) Uani 1 1 d . U H10H H 0.9088 0.5899 0.0131 0.168 Uiso 1 1 calc R U C105 C 0.880(3) 0.680(3) 0.042(2) 0.134(17) Uani 1 1 d . U H10I H 0.8891 0.7023 0.0091 0.160 Uiso 1 1 calc R U C106 C 0.852(3) 0.717(3) 0.0876(19) 0.129(15) Uani 1 1 d . U H10J H 0.8429 0.7635 0.0865 0.154 Uiso 1 1 calc R U C107 C 0.840(3) 0.679(3) 0.135(2) 0.123(14) Uani 1 1 d . U C108 C 0.817(3) 0.715(3) 0.184(2) 0.102(12) Uani 1 1 d . U C109 C 0.827(2) 0.782(2) 0.1955(17) 0.094(11) Uani 1 1 d . U H10K H 0.8496 0.8149 0.1723 0.113 Uiso 1 1 calc R U C110 C 0.798(3) 0.792(3) 0.249(2) 0.101(13) Uani 1 1 d . U C111 C 0.798(3) 0.848(3) 0.2836(18) 0.095(12) Uani 1 1 d . U C112 C 0.825(2) 0.913(2) 0.2721(18) 0.099(13) Uani 1 1 d . U H11B H 0.8466 0.9239 0.2378 0.119 Uiso 1 1 calc R U C113 C 0.819(3) 0.959(2) 0.3097(18) 0.110(14) Uani 1 1 d . U H11C H 0.8395 1.0019 0.3019 0.132 Uiso 1 1 calc R U C114 C 0.786(2) 0.947(2) 0.3603(18) 0.101(12) Uani 1 1 d . U H11D H 0.7817 0.9803 0.3868 0.121 Uiso 1 1 calc R U C115 C 0.757(3) 0.881(3) 0.3701(19) 0.097(12) Uani 1 1 d . U C116 C 0.720(3) 0.862(3) 0.422(2) 0.094(11) Uani 1 1 d . U C117 C 0.703(3) 0.893(3) 0.4689(19) 0.116(14) Uani 1 1 d . U H11E H 0.7127 0.9378 0.4767 0.139 Uiso 1 1 calc R U C118 C 0.669(3) 0.849(3) 0.503(2) 0.110(13) Uani 1 1 d . U C119 C 0.645(3) 0.860(3) 0.563(2) 0.129(15) Uani 1 1 d . U C120 C 0.641(3) 0.930(3) 0.578(2) 0.145(17) Uani 1 1 d . U H12B H 0.6513 0.9624 0.5517 0.173 Uiso 1 1 calc R U C121 C 0.623(4) 0.947(3) 0.630(2) 0.18(2) Uani 1 1 d . U H12C H 0.6252 0.9912 0.6434 0.221 Uiso 1 1 calc R U C122 C 0.601(3) 0.892(3) 0.662(2) 0.153(19) Uani 1 1 d . U H12D H 0.5828 0.9044 0.6968 0.184 Uiso 1 1 calc R U C123 C 0.598(3) 0.821(3) 0.654(2) 0.141(16) Uani 1 1 d . U H12E H 0.5842 0.7877 0.6792 0.169 Uiso 1 1 calc R U C124 C 0.621(3) 0.816(3) 0.599(2) 0.126(15) Uani 1 1 d . U C125 C 0.611(4) 0.699(3) 0.616(2) 0.18(2) Uani 1 1 d . U H12H H 0.6209 0.6566 0.5984 0.271 Uiso 1 1 calc R U H12I H 0.6473 0.7015 0.6484 0.271 Uiso 1 1 calc R U H12J H 0.5521 0.7019 0.6269 0.271 Uiso 1 1 calc R U C126 C 0.958(3) 0.666(2) 0.4440(18) 0.119(15) Uani 1 1 d . U H12F H 1.0106 0.6694 0.4623 0.143 Uiso 1 1 calc R U C127 C 0.908(3) 0.615(3) 0.4393(17) 0.109(13) Uani 1 1 d . U H12G H 0.9195 0.5735 0.4550 0.130 Uiso 1 1 calc R U C128 C 0.835(3) 0.627(3) 0.4097(17) 0.097(11) Uani 1 1 d . U C129 C 0.756(3) 0.592(3) 0.3928(16) 0.094(11) Uani 1 1 d . U C130 C 0.745(3) 0.523(2) 0.4013(16) 0.110(13) Uani 1 1 d . U H13B H 0.7874 0.4956 0.4160 0.132 Uiso 1 1 calc R U C131 C 0.666(3) 0.502(3) 0.3859(17) 0.120(15) Uani 1 1 d . U H13C H 0.6517 0.4570 0.3922 0.144 Uiso 1 1 calc R U C132 C 0.609(3) 0.540(3) 0.3628(19) 0.134(17) Uani 1 1 d . U H13D H 0.5555 0.5229 0.3525 0.161 Uiso 1 1 calc R U C133 C 0.629(3) 0.605(3) 0.3541(16) 0.096(11) Uani 1 1 d . U C134 C 0.575(3) 0.654(2) 0.3243(16) 0.089(10) Uani 1 1 d . U C135 C 0.500(3) 0.651(3) 0.2930(18) 0.115(15) Uani 1 1 d . U H13E H 0.4656 0.6132 0.2866 0.138 Uiso 1 1 calc R U C136 C 0.489(3) 0.710(3) 0.2749(18) 0.112(14) Uani 1 1 d . U H13F H 0.4441 0.7236 0.2523 0.135 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 0.151(13) 0.194(15) 0.121(13) 0.013(11) 0.015(12) 0.005(13) O1_1 0.158(14) 0.19(2) 0.11(2) 0.029(16) 0.012(14) 0.004(15) O2_1 0.17(2) 0.23(2) 0.154(18) -0.004(16) -0.003(15) 0.018(18) O3_1 0.17(2) 0.201(17) 0.20(3) 0.003(15) 0.012(19) 0.011(16) O4_1 0.20(2) 0.21(2) 0.141(18) 0.012(15) 0.027(16) -0.012(18) Cl1_2 0.139(16) 0.191(17) 0.115(13) 0.026(11) 0.006(10) -0.020(10) O1_2 0.14(2) 0.20(2) 0.11(2) 0.019(14) 0.011(15) -0.020(13) O2_2 0.15(2) 0.22(2) 0.138(17) 0.045(15) 0.017(14) -0.001(17) O3_2 0.158(19) 0.17(2) 0.14(2) 0.032(16) -0.012(13) -0.033(14) O4_2 0.18(2) 0.20(2) 0.14(2) 0.023(15) 0.022(15) -0.009(14) Cl1_3 0.187(17) 0.146(15) 0.129(14) -0.003(12) 0.007(10) -0.012(11) O1_3 0.20(2) 0.15(2) 0.15(2) 0.020(16) -0.014(15) -0.012(14) O2_3 0.20(2) 0.158(18) 0.20(2) -0.017(15) 0.023(18) -0.017(15) O3_3 0.22(2) 0.17(2) 0.18(2) 0.001(16) -0.017(15) -0.015(16) O4_3 0.25(3) 0.17(2) 0.178(18) 0.006(16) 0.042(15) -0.009(18) Cl1_4 0.181(14) 0.222(16) 0.078(12) -0.014(11) -0.010(11) 0.023(14) O1_4 0.17(2) 0.20(2) 0.081(16) -0.005(15) 0.006(14) 0.020(17) O2_4 0.20(2) 0.238(18) 0.13(2) -0.029(15) -0.025(18) 0.026(16) O3_4 0.25(3) 0.27(2) 0.106(17) -0.001(15) -0.002(16) 0.005(19) O4_4 0.193(16) 0.29(3) 0.12(2) -0.030(19) -0.010(14) 0.030(16) Fe01 0.098(5) 0.118(6) 0.067(5) 0.011(4) 0.008(4) 0.002(4) Fe02 0.099(5) 0.123(6) 0.076(5) 0.003(4) 0.008(4) -0.007(4) O1 0.19(3) 0.15(2) 0.097(18) 0.006(16) 0.022(18) -0.01(2) O2 0.16(3) 0.17(2) 0.09(2) 0.004(15) 0.003(17) -0.020(19) O101 0.26(4) 0.14(2) 0.093(18) -0.017(16) 0.035(19) 0.00(2) O102 0.17(3) 0.18(2) 0.086(19) 0.010(15) 0.010(18) 0.005(19) N1 0.10(2) 0.127(14) 0.074(12) 0.010(10) 0.006(12) 0.006(13) N2 0.103(18) 0.125(13) 0.072(9) 0.013(8) 0.007(8) 0.006(11) N3 0.082(16) 0.117(10) 0.077(10) 0.011(8) 0.008(9) -0.004(9) N4 0.093(16) 0.127(12) 0.072(10) 0.008(8) 0.004(9) 0.000(10) N5 0.12(3) 0.143(16) 0.074(11) 0.012(10) 0.007(12) 0.004(15) N6 0.105(15) 0.132(18) 0.061(18) 0.009(15) 0.014(13) -0.004(12) N7 0.102(11) 0.124(12) 0.059(15) 0.006(10) 0.014(9) -0.001(9) N8 0.106(12) 0.118(11) 0.081(15) 0.011(9) 0.008(10) 0.003(8) N9 0.098(10) 0.120(14) 0.077(15) 0.011(11) 0.006(9) 0.003(9) N10 0.102(15) 0.123(15) 0.07(2) 0.009(13) 0.005(14) 0.001(12) N101 0.11(2) 0.127(14) 0.079(13) -0.005(10) 0.006(13) -0.006(13) N102 0.088(17) 0.121(13) 0.070(10) 0.000(8) 0.003(9) -0.003(11) N103 0.088(18) 0.123(10) 0.072(11) 0.000(8) 0.001(10) -0.002(9) N104 0.087(18) 0.131(12) 0.073(11) 0.004(9) -0.003(10) 0.005(10) N105 0.12(3) 0.147(16) 0.079(13) 0.004(11) 0.008(13) 0.001(15) N106 0.104(15) 0.133(17) 0.10(2) 0.004(14) -0.003(14) -0.001(12) N107 0.097(12) 0.129(13) 0.078(16) 0.001(11) 0.008(10) 0.000(9) N108 0.093(12) 0.122(10) 0.075(17) -0.006(9) 0.013(11) 0.001(8) N109 0.093(11) 0.125(13) 0.081(16) -0.003(11) 0.009(10) -0.004(9) N110 0.100(16) 0.128(16) 0.09(2) -0.005(14) 0.004(15) -0.005(12) C1 0.32(7) 0.15(2) 0.13(4) 0.00(2) 0.07(4) -0.02(2) C2 0.15(4) 0.142(17) 0.093(19) 0.006(13) 0.01(2) 0.004(16) C3 0.21(5) 0.15(2) 0.11(2) -0.003(16) 0.04(3) -0.003(19) C4 0.17(4) 0.15(2) 0.10(2) 0.000(18) 0.02(2) 0.00(2) C5 0.17(4) 0.15(2) 0.096(19) -0.003(18) 0.04(2) 0.00(2) C6 0.16(4) 0.14(2) 0.083(18) 0.006(15) 0.02(2) 0.002(19) C7 0.10(3) 0.140(17) 0.076(15) 0.008(12) 0.003(15) 0.010(15) C8 0.11(3) 0.133(16) 0.074(13) 0.012(10) 0.007(13) 0.011(16) C9 0.09(3) 0.133(16) 0.076(12) 0.014(10) 0.009(12) 0.007(16) C10 0.12(3) 0.128(14) 0.074(11) 0.017(9) 0.013(12) 0.012(15) C11 0.09(3) 0.125(14) 0.078(12) 0.015(9) 0.009(12) 0.004(14) C12 0.16(4) 0.134(16) 0.088(17) 0.024(12) 0.025(18) 0.027(19) C13 0.19(5) 0.142(17) 0.096(18) 0.022(13) 0.03(2) 0.04(2) C14 0.16(4) 0.133(14) 0.093(18) 0.017(12) 0.020(19) 0.024(17) C15 0.11(3) 0.128(13) 0.082(12) 0.011(10) 0.011(13) 0.012(15) C16 0.07(3) 0.127(13) 0.078(11) 0.006(9) -0.001(12) -0.007(13) C17 0.10(3) 0.143(16) 0.081(14) 0.006(11) 0.007(15) 0.005(17) C18 0.08(3) 0.142(18) 0.077(12) 0.003(11) -0.006(13) -0.010(16) C19 0.11(3) 0.16(2) 0.077(14) 0.000(12) -0.002(15) -0.022(17) C20 0.15(4) 0.17(2) 0.09(2) -0.001(15) 0.01(2) -0.007(19) C21 0.15(4) 0.18(3) 0.09(2) -0.005(16) 0.01(2) -0.02(2) C22 0.22(5) 0.18(3) 0.10(2) 0.002(18) 0.02(2) -0.01(3) C23 0.17(4) 0.18(3) 0.090(19) 0.003(16) 0.01(2) -0.02(2) C24 0.14(4) 0.17(2) 0.085(18) 0.005(14) -0.003(18) -0.023(17) C25 0.17(5) 0.17(2) 0.11(4) 0.015(18) 0.02(3) -0.02(2) C26 0.124(19) 0.14(2) 0.08(3) 0.016(17) 0.00(2) -0.013(16) C27 0.114(19) 0.131(17) 0.06(3) 0.005(14) 0.012(16) -0.004(14) C28 0.113(15) 0.126(14) 0.07(2) 0.009(13) 0.010(15) -0.003(11) C29 0.104(14) 0.116(14) 0.05(2) 0.000(13) 0.021(14) 0.005(11) C30 0.11(2) 0.119(16) 0.07(2) 0.008(16) 0.014(16) 0.002(14) C31 0.12(2) 0.128(19) 0.08(3) 0.020(19) 0.005(18) -0.003(14) C32 0.11(2) 0.126(18) 0.09(2) 0.020(18) 0.004(18) 0.000(14) C33 0.099(13) 0.113(14) 0.05(2) -0.003(13) 0.023(12) 0.011(10) C34 0.100(13) 0.122(15) 0.08(3) 0.014(15) 0.005(14) 0.003(11) C35 0.103(14) 0.13(2) 0.09(3) 0.021(19) 0.001(16) -0.002(12) C36 0.101(15) 0.13(2) 0.08(3) 0.018(17) 0.002(15) -0.002(14) C101 0.47(10) 0.15(2) 0.10(3) -0.01(2) 0.08(4) 0.05(3) C102 0.20(5) 0.145(18) 0.092(18) -0.015(14) 0.02(2) 0.004(17) C103 0.19(5) 0.16(2) 0.09(2) -0.019(16) 0.01(2) 0.01(2) C104 0.17(5) 0.16(3) 0.09(2) -0.015(16) 0.01(2) 0.01(3) C105 0.16(4) 0.16(3) 0.086(17) -0.015(17) 0.013(18) 0.01(3) C106 0.15(4) 0.15(2) 0.085(16) -0.011(15) 0.018(18) 0.00(2) C107 0.14(4) 0.144(17) 0.084(14) -0.015(13) 0.013(15) -0.006(16) C108 0.10(3) 0.131(16) 0.077(13) -0.006(11) 0.004(14) -0.006(15) C109 0.08(3) 0.130(15) 0.068(13) -0.001(10) -0.002(14) -0.003(15) C110 0.11(3) 0.123(13) 0.073(12) -0.002(9) 0.009(14) -0.007(12) C111 0.09(3) 0.120(13) 0.072(12) 0.001(9) 0.001(13) -0.001(12) C112 0.10(3) 0.121(14) 0.079(18) 0.001(11) 0.004(17) -0.003(15) C113 0.12(3) 0.124(15) 0.082(19) -0.004(12) 0.011(19) -0.006(16) C114 0.10(3) 0.125(13) 0.078(18) -0.001(12) 0.001(17) 0.000(14) C115 0.10(3) 0.124(12) 0.073(13) -0.001(9) -0.001(14) 0.002(12) C116 0.08(3) 0.131(13) 0.072(12) 0.003(9) -0.007(13) 0.007(13) C117 0.13(4) 0.141(15) 0.078(14) -0.003(11) 0.011(16) -0.001(15) C118 0.11(3) 0.145(17) 0.078(13) 0.004(11) 0.004(14) 0.006(16) C119 0.14(4) 0.17(2) 0.080(14) 0.002(12) 0.012(15) 0.003(17) C120 0.18(5) 0.17(2) 0.09(2) -0.003(14) 0.03(2) 0.001(18) C121 0.27(6) 0.19(2) 0.10(2) -0.008(17) 0.06(3) -0.01(2) C122 0.17(5) 0.19(2) 0.10(2) 0.003(17) 0.03(2) 0.00(3) C123 0.14(4) 0.19(2) 0.087(17) 0.005(16) 0.012(18) 0.00(3) C124 0.11(4) 0.18(2) 0.085(16) 0.010(14) 0.004(17) 0.002(18) C125 0.24(6) 0.19(2) 0.11(3) 0.02(2) 0.02(3) -0.01(2) C126 0.109(17) 0.14(2) 0.11(3) 0.01(2) -0.01(2) -0.004(15) C127 0.104(18) 0.132(18) 0.09(3) 0.002(17) 0.002(18) 0.001(12) C128 0.096(14) 0.127(13) 0.07(2) -0.003(12) 0.015(14) 0.004(10) C129 0.096(14) 0.124(12) 0.06(2) -0.006(12) 0.019(14) 0.004(10) C130 0.11(2) 0.125(14) 0.10(3) 0.001(13) 0.004(19) 0.000(11) C131 0.11(2) 0.131(15) 0.12(3) 0.006(15) -0.003(19) -0.004(13) C132 0.12(2) 0.132(15) 0.16(4) 0.017(16) -0.02(2) -0.012(13) C133 0.092(14) 0.125(13) 0.07(3) -0.006(12) 0.018(14) -0.001(10) C134 0.085(14) 0.123(14) 0.06(2) -0.011(12) 0.023(14) -0.001(10) C135 0.104(18) 0.129(18) 0.11(3) 0.000(16) -0.01(2) -0.007(14) C136 0.103(18) 0.13(2) 0.10(3) -0.002(19) -0.01(2) -0.006(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2064 0.9930 '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 O3_1 Cl1_1 O2_1 111.4(12) O3_1 Cl1_1 O1_1 110.5(12) O2_1 Cl1_1 O1_1 110.3(12) O3_1 Cl1_1 O4_1 108.5(12) O2_1 Cl1_1 O4_1 108.1(12) O1_1 Cl1_1 O4_1 107.9(11) O4_2 Cl1_2 O2_2 109.6(12) O4_2 Cl1_2 O3_2 110.0(12) O2_2 Cl1_2 O3_2 109.6(11) O4_2 Cl1_2 O1_2 109.4(12) O2_2 Cl1_2 O1_2 109.3(11) O3_2 Cl1_2 O1_2 108.9(11) O2_3 Cl1_3 O1_3 110.8(12) O2_3 Cl1_3 O4_3 109.1(12) O1_3 Cl1_3 O4_3 109.7(12) O2_3 Cl1_3 O3_3 109.9(12) O1_3 Cl1_3 O3_3 108.5(12) O4_3 Cl1_3 O3_3 108.7(12) O1_4 Cl1_4 O4_4 110.4(11) O1_4 Cl1_4 O3_4 110.4(12) O4_4 Cl1_4 O3_4 109.1(12) O1_4 Cl1_4 O2_4 109.8(12) O4_4 Cl1_4 O2_4 108.8(12) O3_4 Cl1_4 O2_4 108.4(11) N3 Fe01 N8 172.7(15) N3 Fe01 N9 97.6(15) N8 Fe01 N9 81.1(17) N3 Fe01 N4 77.3(16) N8 Fe01 N4 95.5(15) N9 Fe01 N4 91.6(13) N3 Fe01 N7 105.1(15) N8 Fe01 N7 76.4(17) N9 Fe01 N7 157.4(17) N4 Fe01 N7 93.4(13) N3 Fe01 N2 81.1(16) N8 Fe01 N2 106.1(15) N9 Fe01 N2 94.3(13) N4 Fe01 N2 158.2(16) N7 Fe01 N2 89.3(13) N103 Fe02 N108 173.4(14) N103 Fe02 N109 108.2(14) N108 Fe02 N109 74.0(16) N103 Fe02 N107 105.0(14) N108 Fe02 N107 72.5(16) N109 Fe02 N107 146.5(16) N103 Fe02 N102 72.7(15) N108 Fe02 N102 101.4(13) N109 Fe02 N102 88.1(12) N107 Fe02 N102 97.9(12) N103 Fe02 N104 73.7(14) N108 Fe02 N104 112.3(13) N109 Fe02 N104 99.7(12) N107 Fe02 N104 93.5(12) N102 Fe02 N104 146.3(15) C2 O1 C1 119(4) C24 O2 C25 119(5) C102 O101 C101 117(5) C124 O102 C125 117(5) N2 N1 C8 109(4) N2 N1 H1B 125.6 C8 N1 H1B 125.6 C10 N2 N1 111(4) C10 N2 Fe01 115(4) N1 N2 Fe01 134(3) C15 N3 C11 118(4) C15 N3 Fe01 125(4) C11 N3 Fe01 116(3) C16 N4 N5 106(4) C16 N4 Fe01 116(4) N5 N4 Fe01 138(3) N4 N5 C18 113(4) N4 N5 H5A 123.5 C18 N5 H5A 123.5 C26 N6 N7 111(4) C26 N6 H6A 124.7 N7 N6 H6A 124.7 C28 N7 N6 106(4) C28 N7 Fe01 115(4) N6 N7 Fe01 137(3) C29 N8 C33 118(5) C29 N8 Fe01 126(4) C33 N8 Fe01 115(4) C34 N9 N10 106(5) C34 N9 Fe01 118(4) N10 N9 Fe01 136(3) C36 N10 N9 110(4) C36 N10 H10C 125.2 N9 N10 H10C 125.2 N102 N101 C108 115(4) N102 N101 H10D 122.7 C108 N101 H10D 122.7 C110 N102 N101 105(4) C110 N102 Fe02 117(4) N101 N102 Fe02 137(3) C115 N103 C111 115(5) C115 N103 Fe02 123(4) C111 N103 Fe02 122(3) N105 N104 C116 106(4) N105 N104 Fe02 140(3) C116 N104 Fe02 114(3) C118 N105 N104 108(4) C118 N105 H10E 125.9 N104 N105 H10E 125.9 N107 N106 C126 117(4) N107 N106 H10F 121.6 C126 N106 H10F 121.6 N106 N107 C128 102(4) N106 N107 Fe02 139(3) C128 N107 Fe02 118(4) C129 N108 C133 112(5) C129 N108 Fe02 125(4) C133 N108 Fe02 123(4) N110 N109 C134 103(4) N110 N109 Fe02 137(3) C134 N109 Fe02 118(4) C136 N110 N109 111(4) C136 N110 H11A 124.3 N109 N110 H11A 124.3 O1 C1 H1A 109.5 O1 C1 H1C 109.5 H1A C1 H1C 109.5 O1 C1 H1D 109.5 H1A C1 H1D 109.5 H1C C1 H1D 109.5 C7 C2 C3 126(6) C7 C2 O1 111(6) C3 C2 O1 124(6) C4 C3 C2 114(6) C4 C3 H3A 122.9 C2 C3 H3A 122.9 C3 C4 C5 125(6) C3 C4 H4A 117.7 C5 C4 H4A 117.7 C6 C5 C4 118(5) C6 C5 H5B 121.2 C4 C5 H5B 121.2 C5 C6 C7 123(5) C5 C6 H6B 118.7 C7 C6 H6B 118.7 C2 C7 C6 115(6) C2 C7 C8 127(6) C6 C7 C8 117(6) C9 C8 N1 105(5) C9 C8 C7 133(5) N1 C8 C7 122(5) C8 C9 C10 111(5) C8 C9 H9A 124.7 C10 C9 H9A 124.7 N2 C10 C9 105(5) N2 C10 C11 116(5) C9 C10 C11 138(5) C12 C11 C10 128(5) C12 C11 N3 120(5) C10 C11 N3 112(5) C13 C12 C11 120(5) C13 C12 H12A 120.2 C11 C12 H12A 120.2 C12 C13 C14 122(5) C12 C13 H13A 118.9 C14 C13 H13A 118.9 C15 C14 C13 117(5) C15 C14 H14A 121.6 C13 C14 H14A 121.6 C14 C15 N3 123(5) C14 C15 C16 134(5) N3 C15 C16 102(5) N4 C16 C17 111(5) N4 C16 C15 119(5) C17 C16 C15 129(5) C18 C17 C16 104(5) C18 C17 H17A 127.8 C16 C17 H17A 127.8 N5 C18 C17 105(5) N5 C18 C19 125(5) C17 C18 C19 130(5) C20 C19 C24 126(6) C20 C19 C18 116(5) C24 C19 C18 118(6) C19 C20 C21 112(5) C19 C20 H20A 124.2 C21 C20 H20A 124.2 C22 C21 C20 122(6) C22 C21 H21A 118.8 C20 C21 H21A 118.8 C21 C22 C23 127(6) C21 C22 H22A 116.7 C23 C22 H22A 116.7 C22 C23 C24 117(6) C22 C23 H23A 121.3 C24 C23 H23A 121.3 O2 C24 C23 125(6) O2 C24 C19 119(6) C23 C24 C19 115(6) 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 108(5) N6 C26 H26A 126.2 C27 C26 H26A 126.2 C26 C27 C28 108(5) C26 C27 H27A 126.2 C28 C27 H27A 126.2 N7 C28 C27 108(5) N7 C28 C29 118(5) C27 C28 C29 134(5) N8 C29 C30 126(5) N8 C29 C28 103(5) C30 C29 C28 131(5) C31 C30 C29 116(5) C31 C30 H30A 122.0 C29 C30 H30A 122.0 C30 C31 C32 124(5) C30 C31 H31A 118.1 C32 C31 H31A 118.1 C31 C32 C33 120(5) C31 C32 H32A 119.9 C33 C32 H32A 119.9 N8 C33 C34 113(5) N8 C33 C32 116(5) C34 C33 C32 131(5) N9 C34 C35 112(5) N9 C34 C33 113(6) C35 C34 C33 135(5) C36 C35 C34 103(5) C36 C35 H35A 128.7 C34 C35 H35A 128.7 N10 C36 C35 110(5) N10 C36 H36A 125.1 C35 C36 H36A 125.1 O101 C101 H10A 109.5 O101 C101 H10B 109.5 H10A C101 H10B 109.5 O101 C101 H10L 109.5 H10A C101 H10L 109.5 H10B C101 H10L 109.5 O101 C102 C107 113(6) O101 C102 C103 123(6) C107 C102 C103 124(7) C104 C103 C102 116(6) C104 C103 H10G 122.0 C102 C103 H10G 122.0 C103 C104 C105 123(6) C103 C104 H10H 118.3 C105 C104 H10H 118.3 C104 C105 C106 122(5) C104 C105 H10I 119.1 C106 C105 H10I 119.1 C105 C106 C107 114(5) C105 C106 H10J 123.0 C107 C106 H10J 123.0 C102 C107 C106 120(6) C102 C107 C108 124(6) C106 C107 C108 116(6) N101 C108 C109 104(5) N101 C108 C107 127(5) C109 C108 C107 129(5) C108 C109 C110 107(5) C108 C109 H10K 126.7 C110 C109 H10K 126.7 N102 C110 C109 110(5) N102 C110 C111 118(5) C109 C110 C111 132(5) C112 C111 C110 129(5) C112 C111 N103 121(5) C110 C111 N103 110(5) C113 C112 C111 119(5) C113 C112 H11B 120.4 C111 C112 H11B 120.4 C112 C113 C114 123(5) C112 C113 H11C 118.5 C114 C113 H11C 118.5 C113 C114 C115 116(5) C113 C114 H11D 121.9 C115 C114 H11D 121.9 N103 C115 C114 125(5) N103 C115 C116 113(5) C114 C115 C116 122(5) C117 C116 N104 108(5) C117 C116 C115 136(6) N104 C116 C115 116(5) C118 C117 C116 109(6) C118 C117 H11E 125.7 C116 C117 H11E 125.7 C117 C118 N105 109(5) C117 C118 C119 127(6) N105 C118 C119 124(5) C124 C119 C120 118(6) C124 C119 C118 129(6) C120 C119 C118 113(5) C121 C120 C119 120(5) C121 C120 H12B 120.1 C119 C120 H12B 120.1 C120 C121 C122 112(6) C120 C121 H12C 124.2 C122 C121 H12C 124.2 C121 C122 C123 136(6) C121 C122 H12D 112.0 C123 C122 H12D 112.0 C124 C123 C122 101(5) C124 C123 H12E 129.5 C122 C123 H12E 129.5 C119 C124 O102 111(6) C119 C124 C123 133(7) O102 C124 C123 116(6) O102 C125 H12H 109.5 O102 C125 H12I 109.5 H12H C125 H12I 109.5 O102 C125 H12J 109.5 H12H C125 H12J 109.5 H12I C125 H12J 109.5 C127 C126 N106 100(5) C127 C126 H12F 129.9 N106 C126 H12F 129.9 C126 C127 C128 114(5) C126 C127 H12G 122.8 C128 C127 H12G 122.8 N107 C128 C127 107(5) N107 C128 C129 114(5) C127 C128 C129 139(5) N108 C129 C130 128(5) N108 C129 C128 110(5) C130 C129 C128 122(5) C131 C130 C129 113(5) C131 C130 H13B 123.7 C129 C130 H13B 123.7 C132 C131 C130 123(6) C132 C131 H13C 118.3 C130 C131 H13C 118.3 C131 C132 C133 119(6) C131 C132 H13D 120.7 C133 C132 H13D 120.7 N108 C133 C132 124(5) N108 C133 C134 110(5) C132 C133 C134 126(5) N109 C134 C135 110(5) N109 C134 C133 115(5) C135 C134 C133 135(5) C136 C135 C134 105(5) C136 C135 H13E 127.7 C134 C135 H13E 127.7 C135 C136 N110 111(5) C135 C136 H13F 124.5 N110 C136 H13F 124.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1_1 O3_1 1.382(12) Cl1_1 O2_1 1.384(12) Cl1_1 O1_1 1.390(12) Cl1_1 O4_1 1.400(12) Cl1_2 O4_2 1.386(12) Cl1_2 O2_2 1.389(12) Cl1_2 O3_2 1.390(12) Cl1_2 O1_2 1.392(12) Cl1_3 O2_3 1.384(12) Cl1_3 O1_3 1.388(12) Cl1_3 O4_3 1.391(12) Cl1_3 O3_3 1.392(12) Cl1_4 O1_4 1.384(12) Cl1_4 O4_4 1.389(12) Cl1_4 O3_4 1.389(12) Cl1_4 O2_4 1.392(12) Fe01 N3 1.88(3) Fe01 N8 1.88(4) Fe01 N9 1.95(4) Fe01 N4 1.96(4) Fe01 N7 1.96(4) Fe01 N2 1.99(4) Fe02 N103 2.08(4) Fe02 N108 2.09(4) Fe02 N109 2.12(4) Fe02 N107 2.14(4) Fe02 N102 2.20(4) Fe02 N104 2.22(4) O1 C2 1.42(5) O1 C1 1.46(5) O2 C24 1.30(5) O2 C25 1.44(5) O101 C102 1.37(6) O101 C101 1.40(5) O102 C124 1.38(5) O102 C125 1.44(5) N1 N2 1.32(4) N1 C8 1.39(4) N1 H1B 0.8700 N2 C10 1.31(4) N3 C15 1.36(5) N3 C11 1.43(4) N4 C16 1.29(4) N4 N5 1.33(4) N5 C18 1.36(5) N5 H5A 0.8700 N6 C26 1.33(4) N6 N7 1.39(4) N6 H6A 0.8700 N7 C28 1.34(4) N8 C29 1.36(4) N8 C33 1.42(4) N9 C34 1.29(4) N9 N10 1.32(4) N10 C36 1.32(4) N10 H10C 0.8700 N101 N102 1.34(4) N101 C108 1.36(5) N101 H10D 0.8700 N102 C110 1.33(4) N103 C115 1.32(4) N103 C111 1.43(5) N104 N105 1.36(4) N104 C116 1.39(4) N105 C118 1.36(5) N105 H10E 0.8700 N106 N107 1.35(4) N106 C126 1.35(4) N106 H10F 0.8700 N107 C128 1.36(4) N108 C129 1.33(5) N108 C133 1.36(5) N109 N110 1.33(4) N109 C134 1.37(4) N110 C136 1.32(4) N110 H11A 0.8700 C1 H1A 0.9700 C1 H1C 0.9700 C1 H1D 0.9700 C2 C7 1.39(6) C2 C3 1.40(6) C3 C4 1.37(6) C3 H3A 0.9400 C4 C5 1.39(5) C4 H4A 0.9400 C5 C6 1.38(5) C5 H5B 0.9400 C6 C7 1.39(5) C6 H6B 0.9400 C7 C8 1.47(6) C8 C9 1.32(5) C9 C10 1.39(5) C9 H9A 0.9400 C10 C11 1.40(5) C11 C12 1.37(5) C12 C13 1.34(5) C12 H12A 0.9400 C13 C14 1.42(5) C13 H13A 0.9400 C14 C15 1.36(5) C14 H14A 0.9400 C15 C16 1.47(5) C16 C17 1.42(5) C17 C18 1.38(5) C17 H17A 0.9400 C18 C19 1.52(6) C19 C20 1.40(6) C19 C24 1.46(6) C20 C21 1.45(5) C20 H20A 0.9400 C21 C22 1.31(6) C21 H21A 0.9400 C22 C23 1.36(6) C22 H22A 0.9400 C23 C24 1.42(6) C23 H23A 0.9400 C25 H25A 0.9700 C25 H25B 0.9700 C25 H25C 0.9700 C26 C27 1.35(5) C26 H26A 0.9400 C27 C28 1.42(5) C27 H27A 0.9400 C28 C29 1.44(5) C29 C30 1.37(5) C30 C31 1.33(5) C30 H30A 0.9400 C31 C32 1.36(5) C31 H31A 0.9400 C32 C33 1.45(5) C32 H32A 0.9400 C33 C34 1.44(5) C34 C35 1.38(5) C35 C36 1.34(5) C35 H35A 0.9400 C36 H36A 0.9400 C101 H10A 0.9700 C101 H10B 0.9700 C101 H10L 0.9700 C102 C107 1.37(6) C102 C103 1.37(6) C103 C104 1.33(6) C103 H10G 0.9400 C104 C105 1.38(5) C104 H10H 0.9400 C105 C106 1.42(5) C105 H10I 0.9400 C106 C107 1.42(6) C106 H10J 0.9400 C107 C108 1.46(6) C108 C109 1.39(5) C109 C110 1.42(5) C109 H10K 0.9400 C110 C111 1.42(5) C111 C112 1.40(5) C112 C113 1.31(5) C112 H11B 0.9400 C113 C114 1.38(5) C113 H11C 0.9400 C114 C115 1.41(5) C114 H11D 0.9400 C115 C116 1.46(5) C116 C117 1.34(5) C117 C118 1.33(5) C117 H11E 0.9400 C118 C119 1.56(6) C119 C124 1.31(6) C119 C120 1.45(6) C120 C121 1.37(6) C120 H12B 0.9400 C121 C122 1.41(6) C121 H12C 0.9400 C122 C123 1.43(6) C122 H12D 0.9400 C123 C124 1.41(6) C123 H12E 0.9400 C125 H12H 0.9700 C125 H12I 0.9700 C125 H12J 0.9700 C126 C127 1.30(5) C126 H12F 0.9400 C127 C128 1.37(5) C127 H12G 0.9400 C128 C129 1.49(5) C129 C130 1.40(5) C130 C131 1.37(5) C130 H13B 0.9400 C131 C132 1.31(5) C131 H13C 0.9400 C132 C133 1.37(5) C132 H13D 0.9400 C133 C134 1.49(5) C134 C135 1.40(5) C135 C136 1.29(5) C135 H13E 0.9400 C136 H13F 0.9400