#------------------------------------------------------------------------------ #$Date: 2016-04-05 18:07:57 +0300 (Tue, 05 Apr 2016) $ #$Revision: 181581 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/18/1541899.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_1541899 loop_ _publ_author_name 'Arom\'i, G.' 'Beavers, C. M.' 'S\'anchez Costa, J.' 'Craig, G. A.' 'M\'inguez Espallargas, G.' 'Orera, A.' 'Roubeau, O.' _publ_section_title ; Snapshots of a solid-state transformation: coexistence of three phases trapped in one crystal ; _journal_issue 4 _journal_name_full 'Chem. Sci.' _journal_page_first 2907 _journal_paper_doi 10.1039/C5SC04287A _journal_volume 7 _journal_year 2016 _chemical_formula_moiety '(C36 H30 Fe N10 O2),2(Cl O4)' _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 _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 90.221(8) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.679(12) _cell_length_b 20.102(15) _cell_length_c 24.601(18) _cell_measurement_reflns_used 1179 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 24.64 _cell_measurement_theta_min 2.78 _cell_volume 7754(10) _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 'SHELXT (Sheldrick, 2012)' _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.594 _diffrn_measured_fraction_theta_max 0.594 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_orient_matrix_type 'Sparks (1982)' _diffrn_orient_matrix_UB_11 0.00511 _diffrn_orient_matrix_UB_12 -0.01474 _diffrn_orient_matrix_UB_13 0.03870 _diffrn_orient_matrix_UB_21 -0.02480 _diffrn_orient_matrix_UB_22 0.04327 _diffrn_orient_matrix_UB_23 0.01228 _diffrn_orient_matrix_UB_31 -0.05854 _diffrn_orient_matrix_UB_32 -0.01962 _diffrn_orient_matrix_UB_33 -0.00199 _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 0.0857 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_Laue_measured_fraction_full 0.594 _diffrn_reflns_Laue_measured_fraction_max 0.594 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11377 _diffrn_reflns_point_group_measured_fraction_full 0.594 _diffrn_reflns_point_group_measured_fraction_max 0.594 _diffrn_reflns_theta_full 18.835 _diffrn_reflns_theta_max 18.835 _diffrn_reflns_theta_min 2.777 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_T_max 0.7445 _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 1.524 _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 0.290 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1063 _refine_ls_number_reflns 2792 _refine_ls_number_restraints 1482 _refine_ls_restrained_S_all 0.958 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0696 _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^)+(0.0953P)^2^+57.0043P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1604 _refine_ls_wR_factor_ref 0.2093 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1625 _reflns_number_total 2792 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage2_Transient _cod_depositor_comments 'Adding full bibliography for 1541896--1541904.cif.' _cod_database_code 1541899 _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 0.963 _shelx_res_file ; Inter.res created by SHELXL-2014/7 REM Solution 1 R1 0.200 Rweak 0.011, Alpha = 0.1035 in P2(1)/c REM Formula: C87 N18 O8 Cl4 Fe2 TITL samp2 in P2(1)/c Sample folder: srj128c5 CELL 0.77490 15.6793 20.1024 24.6007 90.000 90.221 90.000 ZERR 8.00 0.0118 0.0149 0.0182 0.0000 0.0076 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-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. 20 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 WGHT 0.095300 57.004303 FVAR 0.04063 RESI 1 CLO4 CL1 5 1.017406 0.877972 0.392647 11.00000 0.09261 0.11717 = 0.10316 -0.00012 0.00572 -0.00676 O1 4 1.105782 0.871877 0.385428 11.00000 0.10125 0.13003 = 0.08856 0.01848 0.00687 -0.00148 O2 4 0.973811 0.852154 0.347887 11.00000 0.13752 0.17321 = 0.15914 -0.02833 -0.02209 0.01512 O3 4 0.994543 0.942521 0.405418 11.00000 0.12508 0.12392 = 0.22932 -0.01565 0.00624 -0.00225 O4 4 0.996402 0.836772 0.437652 11.00000 0.16964 0.14237 = 0.14985 0.01253 0.03720 -0.00852 RESI 2 CLO4 CL1 5 0.500126 0.911349 0.239462 11.00000 0.08961 0.13447 = 0.10116 0.02094 -0.00447 -0.01506 O1 4 0.450007 0.855085 0.228314 11.00000 0.07786 0.14342 = 0.12210 0.00491 -0.00439 -0.01134 O2 4 0.532811 0.937782 0.191162 11.00000 0.09305 0.19095 = 0.13211 0.04949 -0.00333 -0.00943 O3 4 0.568283 0.892346 0.273503 11.00000 0.11186 0.12812 = 0.14208 0.03423 -0.03657 -0.03753 O4 4 0.450962 0.959782 0.265584 11.00000 0.13593 0.15065 = 0.14997 0.00731 0.01488 -0.00734 RESI 3 CLO4 CL1 5 0.003058 0.449144 0.371365 11.00000 0.11522 0.09405 = 0.13061 -0.01513 0.00181 -0.01709 O1 4 0.069606 0.493514 0.382436 11.00000 0.14580 0.11175 = 0.15168 0.02091 -0.03345 -0.02579 O2 4 0.032696 0.388649 0.352449 11.00000 0.15032 0.12340 = 0.22488 -0.03179 0.02719 -0.01323 O3 4 -0.051979 0.478549 0.333096 11.00000 0.18559 0.14299 = 0.19385 -0.00790 -0.04711 -0.01706 O4 4 -0.044667 0.439330 0.418757 11.00000 0.19255 0.13766 = 0.19214 0.00691 0.04387 -0.01149 RESI 4 CLO4 CL1 5 0.503634 0.638979 0.490943 11.00000 0.10964 0.14680 = 0.08599 -0.00274 -0.02778 0.01718 O1 4 0.459726 0.616921 0.444854 11.00000 0.13255 0.09429 = 0.10233 0.00516 -0.03483 0.02188 O2 4 0.482347 0.705901 0.501061 11.00000 0.17134 0.17678 = 0.15266 -0.03320 -0.05141 0.03403 O3 4 0.482565 0.602116 0.536960 11.00000 0.22441 0.23393 = 0.12184 0.02229 -0.03080 -0.02426 O4 4 0.592365 0.636403 0.483620 11.00000 0.13500 0.26978 = 0.12255 -0.03826 -0.03173 0.02495 RESI 0 FE01 6 0.224054 0.685107 0.347470 11.00000 0.05851 0.07425 = 0.06037 0.01198 -0.00454 0.00427 FE02 6 0.729968 0.734543 0.354943 11.00000 0.05480 0.07697 = 0.06975 0.00522 -0.00137 -0.00713 O1 4 0.177775 0.867597 0.501396 11.00000 0.14007 0.10668 = 0.09906 -0.00299 0.00400 -0.03698 O2 4 0.330544 0.725243 0.148319 11.00000 0.11211 0.11462 = 0.08896 0.00789 -0.01167 -0.01271 O101 4 0.839530 0.581857 0.185332 11.00000 0.19141 0.10205 = 0.08509 -0.01113 0.01716 0.00195 O102 4 0.631871 0.751241 0.579611 11.00000 0.09221 0.14901 = 0.09406 -0.00243 0.00181 -0.01093 N1 3 0.165276 0.750787 0.452595 11.00000 0.03502 0.07879 = 0.07598 -0.00020 -0.01183 -0.01737 AFIX 43 H1B 2 0.157510 0.790990 0.440455 11.00000 -1.20000 AFIX 0 N2 3 0.188970 0.699246 0.422471 11.00000 0.06965 0.08105 = 0.06707 0.00709 -0.00539 -0.00180 N3 3 0.250755 0.598648 0.378436 11.00000 0.06505 0.07447 = 0.06446 0.01209 -0.00399 0.00030 N4 3 0.272641 0.639326 0.283802 11.00000 0.05484 0.08353 = 0.06679 0.00706 -0.00551 0.00041 N5 3 0.292139 0.654213 0.232313 11.00000 0.07070 0.09086 = 0.06523 0.00345 -0.00898 -0.00345 AFIX 43 H5A 2 0.283630 0.692596 0.216880 11.00000 -1.20000 AFIX 0 N6 3 0.395613 0.732982 0.397523 11.00000 0.06985 0.07534 = 0.07093 0.00749 -0.00902 0.00134 AFIX 43 H6A 2 0.409191 0.698600 0.417215 11.00000 -1.20000 AFIX 0 N7 3 0.326618 0.737422 0.362266 11.00000 0.06020 0.06700 = 0.05371 0.00701 0.00001 0.00298 N8 3 0.195411 0.766593 0.308686 11.00000 0.06769 0.07455 = 0.06403 0.01207 0.00512 0.00714 N9 3 0.108274 0.665241 0.321585 11.00000 0.06269 0.08578 = 0.07357 0.02120 -0.00387 -0.00168 N10 3 0.054920 0.614514 0.324675 11.00000 0.06501 0.08697 = 0.06468 0.01723 0.00220 -0.00040 AFIX 43 H10C 2 0.063870 0.577316 0.341849 11.00000 -1.20000 AFIX 0 N101 3 0.787219 0.689005 0.229751 11.00000 0.05778 0.08553 = 0.07246 -0.00826 -0.00273 -0.00750 AFIX 43 H10D 2 0.775594 0.646840 0.232659 11.00000 -1.20000 AFIX 0 N102 3 0.775220 0.733174 0.270866 11.00000 0.04305 0.07766 = 0.06513 -0.00242 -0.00935 -0.00245 N103 3 0.763029 0.833609 0.334599 11.00000 0.04416 0.07319 = 0.06291 0.00273 -0.00955 0.00797 N104 3 0.697467 0.796188 0.427221 11.00000 0.06430 0.09072 = 0.06746 0.00156 -0.00532 -0.00179 N105 3 0.665383 0.789733 0.477960 11.00000 0.06807 0.10947 = 0.07470 0.00182 -0.00150 -0.00537 AFIX 43 H10E 2 0.644104 0.753454 0.491616 11.00000 -1.20000 AFIX 0 N106 3 0.915808 0.711894 0.414907 11.00000 0.06801 0.08888 = 0.08766 -0.00285 -0.00804 -0.00054 AFIX 43 H10F 2 0.936420 0.751916 0.412027 11.00000 -1.20000 AFIX 0 N107 3 0.842095 0.694704 0.391735 11.00000 0.06378 0.08275 = 0.08005 0.00014 -0.00949 -0.00051 N108 3 0.704462 0.631551 0.368173 11.00000 0.06010 0.07799 = 0.06657 -0.00540 -0.00317 -0.00351 N109 3 0.603726 0.718076 0.322972 11.00000 0.05419 0.08740 = 0.06058 -0.00533 0.00319 -0.00187 N110 3 0.550181 0.750666 0.290695 11.00000 0.06354 0.10031 = 0.08353 0.00283 -0.01284 -0.00837 AFIX 43 H11A 2 0.555309 0.792125 0.281101 11.00000 -1.20000 AFIX 0 C1 1 0.191777 0.938174 0.496161 11.00000 0.21926 0.11030 = 0.12841 0.00385 -0.01510 -0.05507 AFIX 33 H1A 2 0.219563 0.947312 0.461800 11.00000 -1.50000 H1C 2 0.137465 0.961221 0.497359 11.00000 -1.50000 H1D 2 0.227728 0.953481 0.525800 11.00000 -1.50000 AFIX 0 C2 1 0.138188 0.843625 0.548344 11.00000 0.10562 0.09131 = 0.09511 -0.00487 -0.00380 -0.01309 C3 1 0.111435 0.884961 0.592786 11.00000 0.16118 0.09993 = 0.10348 -0.00994 0.01248 -0.01154 AFIX 43 H3A 2 0.115621 0.931596 0.591946 11.00000 -1.20000 AFIX 0 C4 1 0.080344 0.852104 0.635120 11.00000 0.14273 0.09701 = 0.10373 -0.00469 0.01255 0.00120 AFIX 43 H4A 2 0.066677 0.877859 0.665766 11.00000 -1.20000 AFIX 0 C5 1 0.066182 0.786804 0.639333 11.00000 0.17733 0.09877 = 0.09879 -0.00784 0.03824 0.00021 AFIX 43 H5B 2 0.040552 0.768428 0.670379 11.00000 -1.20000 AFIX 0 C6 1 0.090732 0.747483 0.596237 11.00000 0.08225 0.09263 = 0.07914 0.00291 -0.00051 0.00656 AFIX 43 H6B 2 0.083316 0.701177 0.598652 11.00000 -1.20000 AFIX 0 C7 1 0.126603 0.774524 0.548664 11.00000 0.07583 0.09031 = 0.07471 -0.00179 -0.00589 -0.00276 C8 1 0.154596 0.731067 0.506738 11.00000 0.06142 0.08236 = 0.07464 -0.00104 -0.00453 -0.01205 C9 1 0.174388 0.666185 0.507290 11.00000 0.08299 0.08556 = 0.07634 0.00348 0.00000 -0.00463 AFIX 43 H9A 2 0.172010 0.638455 0.538013 11.00000 -1.20000 AFIX 0 C10 1 0.198953 0.646084 0.455601 11.00000 0.08376 0.07736 = 0.06825 0.00957 -0.00124 -0.00247 C11 1 0.233360 0.589062 0.430190 11.00000 0.06726 0.07722 = 0.06552 0.01378 -0.00362 -0.00443 C12 1 0.252496 0.527579 0.453237 11.00000 0.12841 0.08519 = 0.07581 0.02209 0.00886 0.01691 AFIX 43 H12A 2 0.242072 0.519315 0.490228 11.00000 -1.20000 AFIX 0 C13 1 0.286773 0.479639 0.420723 11.00000 0.16091 0.09464 = 0.08440 0.02322 0.01823 0.03009 AFIX 43 H13A 2 0.300798 0.437930 0.435541 11.00000 -1.20000 AFIX 0 C14 1 0.300516 0.491272 0.368418 11.00000 0.13166 0.08731 = 0.08067 0.01424 0.01137 0.01879 AFIX 43 H14A 2 0.320146 0.456716 0.345968 11.00000 -1.20000 AFIX 0 C15 1 0.286348 0.553397 0.346643 11.00000 0.07326 0.08038 = 0.07101 0.00854 0.00158 0.00376 C16 1 0.295708 0.577596 0.291410 11.00000 0.05193 0.08372 = 0.07083 0.00524 -0.00424 -0.00012 C17 1 0.330645 0.550100 0.244104 11.00000 0.07052 0.09119 = 0.07430 0.00044 0.00196 0.00279 AFIX 43 H17A 2 0.351508 0.506704 0.239083 11.00000 -1.20000 AFIX 0 C18 1 0.327611 0.599695 0.207561 11.00000 0.04302 0.08905 = 0.07043 -0.00471 -0.01526 -0.01349 C19 1 0.359303 0.608761 0.149927 11.00000 0.05614 0.11311 = 0.07062 -0.00149 -0.01341 -0.01815 C20 1 0.385729 0.548510 0.125916 11.00000 0.12390 0.12077 = 0.09220 -0.00678 0.00725 -0.00660 AFIX 43 H20A 2 0.381587 0.508321 0.145260 11.00000 -1.20000 AFIX 0 C21 1 0.418452 0.549172 0.072556 11.00000 0.14944 0.14317 = 0.09826 -0.00692 0.01800 -0.00700 AFIX 43 H21A 2 0.442193 0.511275 0.056119 11.00000 -1.20000 AFIX 0 C22 1 0.412841 0.610534 0.046019 11.00000 0.15185 0.14626 = 0.09030 -0.00370 0.00734 -0.01268 AFIX 43 H22A 2 0.429479 0.612122 0.009374 11.00000 -1.20000 AFIX 0 C23 1 0.385349 0.667812 0.068927 11.00000 0.11405 0.13705 = 0.08022 0.00416 -0.00277 -0.01984 AFIX 43 H23A 2 0.385077 0.706802 0.047833 11.00000 -1.20000 AFIX 0 C24 1 0.356771 0.671348 0.123815 11.00000 0.08607 0.11661 = 0.07593 0.00570 -0.01337 -0.02049 C25 1 0.337229 0.785811 0.121757 11.00000 0.14646 0.12486 = 0.10170 0.02266 -0.01237 -0.01510 AFIX 33 H25A 2 0.315332 0.820859 0.144935 11.00000 -1.50000 H25B 2 0.396606 0.794598 0.113479 11.00000 -1.50000 H25C 2 0.304426 0.784366 0.088266 11.00000 -1.50000 AFIX 0 C26 1 0.437786 0.791106 0.395920 11.00000 0.07190 0.07294 = 0.06942 -0.00131 0.00251 -0.00022 AFIX 43 H26A 2 0.487551 0.799983 0.416077 11.00000 -1.20000 AFIX 0 C27 1 0.400099 0.835786 0.361674 11.00000 0.08001 0.07654 = 0.09646 0.01016 -0.00938 -0.00505 AFIX 43 H27A 2 0.417563 0.879005 0.352291 11.00000 -1.20000 AFIX 0 C28 1 0.328121 0.799828 0.344184 11.00000 0.06713 0.06806 = 0.06292 0.00996 0.00402 0.00273 C29 1 0.257958 0.813279 0.307738 11.00000 0.06266 0.07172 = 0.04587 0.00539 0.01332 0.00981 C30 1 0.247473 0.868548 0.274681 11.00000 0.09061 0.08276 = 0.07606 0.02606 0.00383 0.00492 AFIX 43 H30A 2 0.289491 0.901823 0.272899 11.00000 -1.20000 AFIX 0 C31 1 0.173030 0.873163 0.244341 11.00000 0.10082 0.10698 = 0.09970 0.04141 -0.00957 -0.00072 AFIX 43 H31A 2 0.165924 0.908624 0.219832 11.00000 -1.20000 AFIX 0 C32 1 0.109135 0.826302 0.249663 11.00000 0.08655 0.08891 = 0.06520 0.01870 0.00365 0.01316 AFIX 43 H32A 2 0.056393 0.832661 0.232125 11.00000 -1.20000 AFIX 0 C33 1 0.122883 0.770044 0.280822 11.00000 0.06382 0.08076 = 0.05254 0.00919 0.01116 0.01272 C34 1 0.072209 0.713315 0.292067 11.00000 0.06590 0.08874 = 0.06073 0.01739 0.00192 0.00480 C35 1 -0.007788 0.691262 0.274294 11.00000 0.07043 0.09338 = 0.07056 0.01774 -0.00065 0.00410 AFIX 43 H35A 2 -0.047260 0.713532 0.251927 11.00000 -1.20000 AFIX 0 C36 1 -0.014724 0.630541 0.296875 11.00000 0.06706 0.09831 = 0.08293 0.02479 -0.00403 -0.00049 AFIX 43 H36A 2 -0.062857 0.602971 0.293381 11.00000 -1.20000 AFIX 0 C101 1 0.861737 0.511081 0.189568 11.00000 0.52506 0.11840 = 0.12363 -0.00024 0.03919 0.07690 AFIX 33 H10A 2 0.848557 0.495174 0.225801 11.00000 -1.50000 H10B 2 0.829153 0.485919 0.163018 11.00000 -1.50000 H10L 2 0.922173 0.505394 0.182683 11.00000 -1.50000 AFIX 0 C102 1 0.854604 0.611781 0.136044 11.00000 0.10702 0.10381 = 0.07840 -0.01530 -0.00271 0.00181 C103 1 0.881344 0.579989 0.088311 11.00000 0.13875 0.11788 = 0.08726 -0.02431 0.01012 0.00069 AFIX 43 H10G 2 0.890044 0.533728 0.088887 11.00000 -1.20000 AFIX 0 C104 1 0.894811 0.612877 0.042343 11.00000 0.11759 0.12628 = 0.09003 -0.02022 0.00460 -0.00490 AFIX 43 H10H 2 0.913672 0.590242 0.011190 11.00000 -1.20000 AFIX 0 C105 1 0.880792 0.680869 0.040747 11.00000 0.11581 0.12480 = 0.07756 -0.02261 -0.00569 -0.00571 AFIX 43 H10I 2 0.888604 0.704150 0.008005 11.00000 -1.20000 AFIX 0 C106 1 0.854956 0.715525 0.087647 11.00000 0.12112 0.10979 = 0.07123 -0.00860 0.00046 -0.00439 AFIX 43 H10J 2 0.847482 0.761909 0.086770 11.00000 -1.20000 AFIX 0 C107 1 0.840547 0.679676 0.135723 11.00000 0.05956 0.10194 = 0.06589 -0.01415 -0.01447 -0.00531 C108 1 0.818368 0.716138 0.184648 11.00000 0.03626 0.08944 = 0.06653 -0.00892 -0.01270 -0.01265 C109 1 0.826999 0.783464 0.194914 11.00000 0.03692 0.08670 = 0.05584 -0.00289 -0.02149 -0.00894 AFIX 43 H10K 2 0.847184 0.816412 0.171096 11.00000 -1.20000 AFIX 0 C110 1 0.798424 0.792104 0.249869 11.00000 0.04798 0.07722 = 0.05717 0.00088 -0.01587 -0.00344 C111 1 0.796968 0.849821 0.285290 11.00000 0.03580 0.07609 = 0.05782 0.00224 -0.01769 0.00105 C112 1 0.823585 0.911006 0.272271 11.00000 0.06894 0.07861 = 0.07591 0.00503 -0.01168 -0.00442 AFIX 43 H11B 2 0.845815 0.920149 0.237635 11.00000 -1.20000 AFIX 0 C113 1 0.817403 0.961087 0.311704 11.00000 0.06070 0.07646 = 0.08040 0.00219 -0.01159 -0.00687 AFIX 43 H11C 2 0.835892 1.004382 0.303410 11.00000 -1.20000 AFIX 0 C114 1 0.785022 0.947956 0.361830 11.00000 0.06449 0.07618 = 0.08193 0.00228 -0.00775 0.00395 AFIX 43 H11D 2 0.780795 0.981243 0.388520 11.00000 -1.20000 AFIX 0 C115 1 0.758350 0.882797 0.371842 11.00000 0.06450 0.07472 = 0.06970 -0.00268 -0.00282 0.00201 C116 1 0.719730 0.859495 0.421146 11.00000 0.06622 0.08671 = 0.07101 -0.00154 0.00008 0.00049 C117 1 0.705046 0.894807 0.470112 11.00000 0.09409 0.10428 = 0.07836 -0.01001 0.00922 -0.01095 AFIX 43 H11E 2 0.715934 0.939916 0.477428 11.00000 -1.20000 AFIX 0 C118 1 0.671728 0.848543 0.503879 11.00000 0.06153 0.10948 = 0.07534 -0.00274 0.00045 -0.00114 C119 1 0.643383 0.863494 0.563460 11.00000 0.07176 0.14506 = 0.07933 -0.01036 0.00233 -0.00849 C120 1 0.639992 0.931849 0.577583 11.00000 0.16397 0.13914 = 0.08416 -0.01606 0.02357 -0.00758 AFIX 43 H12B 2 0.651044 0.965371 0.551918 11.00000 -1.20000 AFIX 0 C121 1 0.619050 0.947401 0.632492 11.00000 0.19914 0.16704 = 0.09386 -0.01971 0.02911 -0.00069 AFIX 43 H12C 2 0.615739 0.991718 0.644492 11.00000 -1.20000 AFIX 0 C122 1 0.603965 0.895466 0.667043 11.00000 0.14991 0.17030 = 0.10016 -0.01187 0.02341 -0.00002 AFIX 43 H12D 2 0.594390 0.906154 0.703714 11.00000 -1.20000 AFIX 0 C123 1 0.601409 0.828867 0.653376 11.00000 0.07660 0.16848 = 0.08518 -0.00596 0.00571 0.00156 AFIX 43 H12E 2 0.586325 0.795539 0.678358 11.00000 -1.20000 AFIX 0 C124 1 0.623360 0.814642 0.598602 11.00000 0.09023 0.15144 = 0.08608 -0.00276 0.00806 -0.00968 C125 1 0.608819 0.698270 0.616839 11.00000 0.14710 0.16584 = 0.10515 0.00893 -0.00309 -0.03225 AFIX 33 H12H 2 0.617261 0.655584 0.599279 11.00000 -1.50000 H12I 2 0.644381 0.700873 0.649121 11.00000 -1.50000 H12J 2 0.549407 0.702946 0.627001 11.00000 -1.50000 AFIX 0 C126 1 0.955982 0.664823 0.442539 11.00000 0.06695 0.08434 = 0.08995 -0.00470 -0.01869 -0.00407 AFIX 43 H12F 2 1.008574 0.669275 0.460647 11.00000 -1.20000 AFIX 0 C127 1 0.908518 0.610091 0.440062 11.00000 0.07187 0.08433 = 0.09029 0.00130 -0.01925 -0.00519 AFIX 43 H12G 2 0.919808 0.567819 0.454754 11.00000 -1.20000 AFIX 0 C128 1 0.837593 0.631246 0.410104 11.00000 0.06757 0.08250 = 0.06305 -0.00679 -0.00586 0.00071 C129 1 0.761282 0.591941 0.394004 11.00000 0.06031 0.07914 = 0.04163 -0.01119 0.01034 0.00317 C130 1 0.746682 0.524871 0.401952 11.00000 0.09430 0.08347 = 0.09746 0.00249 -0.01283 -0.00376 AFIX 43 H13B 2 0.788219 0.496868 0.417403 11.00000 -1.20000 AFIX 0 C131 1 0.666905 0.500897 0.385802 11.00000 0.09590 0.08930 = 0.12174 0.00450 -0.01941 -0.00480 AFIX 43 H13C 2 0.653146 0.455937 0.391544 11.00000 -1.20000 AFIX 0 C132 1 0.611674 0.539981 0.362992 11.00000 0.08507 0.08747 = 0.10193 0.00289 -0.01376 -0.01167 AFIX 43 H13D 2 0.558233 0.522936 0.352569 11.00000 -1.20000 AFIX 0 C133 1 0.629954 0.606561 0.353659 11.00000 0.05539 0.08349 = 0.06927 -0.00688 0.00364 -0.00500 C134 1 0.575099 0.653914 0.324405 11.00000 0.05380 0.08651 = 0.05451 -0.01118 0.00817 -0.00430 C135 1 0.501346 0.648462 0.295191 11.00000 0.06896 0.09972 = 0.10088 -0.00090 -0.01648 -0.01064 AFIX 43 H13E 2 0.467705 0.610248 0.290081 11.00000 -1.20000 AFIX 0 C136 1 0.487295 0.710155 0.275203 11.00000 0.06186 0.10396 = 0.08382 -0.00331 -0.00984 -0.00740 AFIX 43 H13F 2 0.440307 0.722606 0.253648 11.00000 -1.20000 AFIX 0 HKLF 4 REM samp2 in P2(1)/c Sample folder: srj128c5 REM R1 = 0.0696 for 1625 Fo > 4sig(Fo) and 0.1349 for all 2792 data REM 1063 parameters refined using 1482 restraints END WGHT 0.0952 57.0877 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 O2_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 HTAB_2 C17_0 O3_$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 0.290, deepest hole -0.208, 1-sigma level 0.050 Q1 1 1.0271 0.9298 0.3484 11.00000 0.05 0.29 Q2 1 0.5617 0.5771 0.5003 11.00000 0.05 0.29 Q3 1 0.0639 0.4018 0.4133 11.00000 0.05 0.27 Q4 1 0.4348 0.6583 0.5286 11.00000 0.05 0.25 Q5 1 0.0195 0.4484 0.3074 11.00000 0.05 0.22 Q6 1 1.0324 0.9383 0.4342 11.00000 0.05 0.22 Q7 1 0.6760 0.6995 0.5149 11.00000 0.05 0.21 Q8 1 -0.0861 0.4363 0.3806 11.00000 0.05 0.19 Q9 1 0.5000 0.5000 0.0000 10.50000 0.05 0.19 Q10 1 0.5808 0.7002 0.4625 11.00000 0.05 0.19 Q11 1 0.4663 1.0114 0.2336 11.00000 0.05 0.18 Q12 1 0.6946 0.7430 0.4005 11.00000 0.05 0.18 Q13 1 0.0089 0.5614 0.3770 11.00000 0.05 0.18 Q14 1 0.7273 0.6635 0.3426 11.00000 0.05 0.17 Q15 1 0.9262 0.8418 0.4008 11.00000 0.05 0.17 Q16 1 0.1046 0.4568 0.3333 11.00000 0.05 0.17 Q17 1 0.6860 0.9962 0.6170 11.00000 0.05 0.17 Q18 1 0.1821 0.8621 0.4368 11.00000 0.05 0.17 Q19 1 0.0403 0.4969 0.4032 11.00000 0.05 0.16 Q20 1 0.4582 0.7683 0.2468 11.00000 0.05 0.16 ; _shelx_res_checksum 81971 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 1.0174(5) 0.8780(4) 0.3926(3) 0.104(3) Uani 1 1 d D U O1_1 O 1.1058(7) 0.8719(8) 0.3854(6) 0.107(6) Uani 1 1 d D U O2_1 O 0.9738(11) 0.8522(9) 0.3479(6) 0.157(8) Uani 1 1 d D U O3_1 O 0.9945(11) 0.9425(6) 0.4054(8) 0.159(8) Uani 1 1 d D U O4_1 O 0.9964(11) 0.8368(8) 0.4377(6) 0.154(7) Uani 1 1 d D U Cl1_2 Cl 0.5001(5) 0.9113(4) 0.2395(3) 0.108(3) Uani 1 1 d D U O1_2 O 0.4500(9) 0.8551(6) 0.2283(6) 0.114(6) Uani 1 1 d D U O2_2 O 0.5328(10) 0.9378(8) 0.1912(5) 0.139(7) Uani 1 1 d D U O3_2 O 0.5683(8) 0.8923(8) 0.2735(6) 0.127(7) Uani 1 1 d D U O4_2 O 0.4510(10) 0.9598(7) 0.2656(7) 0.145(7) Uani 1 1 d D U Cl1_3 Cl 0.0031(5) 0.4491(4) 0.3714(4) 0.113(3) Uani 1 1 d D U O1_3 O 0.0696(9) 0.4935(7) 0.3824(7) 0.136(7) Uani 1 1 d D U O2_3 O 0.0327(11) 0.3886(7) 0.3524(8) 0.166(8) Uani 1 1 d D U O3_3 O -0.0520(11) 0.4785(8) 0.3331(7) 0.174(8) Uani 1 1 d D U O4_3 O -0.0447(13) 0.4393(9) 0.4188(6) 0.174(9) Uani 1 1 d D U Cl1_4 Cl 0.5036(5) 0.6390(4) 0.4909(3) 0.114(3) Uani 1 1 d D U O1_4 O 0.4597(10) 0.6169(7) 0.4449(5) 0.110(6) Uani 1 1 d D U O2_4 O 0.4823(12) 0.7059(7) 0.5011(7) 0.167(8) Uani 1 1 d D U O3_4 O 0.4826(13) 0.6021(9) 0.5370(6) 0.193(9) Uani 1 1 d D U O4_4 O 0.5924(7) 0.6364(10) 0.4836(8) 0.176(8) Uani 1 1 d D U Fe01 Fe 0.2241(2) 0.6851(2) 0.34747(13) 0.0644(14) Uani 1 1 d . U Fe02 Fe 0.7300(2) 0.7345(2) 0.35494(15) 0.0672(14) Uani 1 1 d . U O1 O 0.1778(12) 0.8676(10) 0.5014(8) 0.115(7) Uani 1 1 d . U O2 O 0.3305(11) 0.7252(12) 0.1483(8) 0.105(6) Uani 1 1 d . U O101 O 0.8395(13) 0.5819(11) 0.1853(8) 0.126(7) Uani 1 1 d . U O102 O 0.6319(11) 0.7512(12) 0.5796(8) 0.112(6) Uani 1 1 d . U N1 N 0.1653(10) 0.7508(10) 0.4526(8) 0.063(5) Uani 1 1 d . U H1B H 0.1575 0.7910 0.4405 0.076 Uiso 1 1 calc R U N2 N 0.1890(12) 0.6992(11) 0.4225(8) 0.073(5) Uani 1 1 d . U N3 N 0.2508(12) 0.5986(10) 0.3784(9) 0.068(5) Uani 1 1 d . U N4 N 0.2726(12) 0.6393(11) 0.2838(8) 0.068(5) Uani 1 1 d . U N5 N 0.2921(11) 0.6542(10) 0.2323(8) 0.076(5) Uani 1 1 d . U H5A H 0.2836 0.6926 0.2169 0.091 Uiso 1 1 calc R U N6 N 0.3956(12) 0.7330(10) 0.3975(7) 0.072(6) Uani 1 1 d . U H6A H 0.4092 0.6986 0.4172 0.086 Uiso 1 1 calc R U N7 N 0.3266(11) 0.7374(10) 0.3623(7) 0.060(5) Uani 1 1 d . U N8 N 0.1954(13) 0.7666(10) 0.3087(8) 0.069(5) Uani 1 1 d . U N9 N 0.1083(12) 0.6652(11) 0.3216(8) 0.074(5) Uani 1 1 d . U N10 N 0.0549(12) 0.6145(10) 0.3247(7) 0.072(6) Uani 1 1 d . U H10C H 0.0639 0.5773 0.3418 0.087 Uiso 1 1 calc R U N101 N 0.7872(11) 0.6890(10) 0.2298(8) 0.072(5) Uani 1 1 d . U H10D H 0.7756 0.6468 0.2327 0.086 Uiso 1 1 calc R U N102 N 0.7752(10) 0.7332(11) 0.2709(8) 0.062(5) Uani 1 1 d . U N103 N 0.7630(11) 0.8336(10) 0.3346(9) 0.060(5) Uani 1 1 d . U N104 N 0.6975(12) 0.7962(12) 0.4272(8) 0.074(5) Uani 1 1 d . U N105 N 0.6654(12) 0.7897(11) 0.4780(8) 0.084(6) Uani 1 1 d . U H10E H 0.6441 0.7535 0.4916 0.101 Uiso 1 1 calc R U N106 N 0.9158(12) 0.7119(10) 0.4149(8) 0.082(6) Uani 1 1 d . U H10F H 0.9364 0.7519 0.4120 0.098 Uiso 1 1 calc R U N107 N 0.8421(12) 0.6947(11) 0.3917(8) 0.076(6) Uani 1 1 d . U N108 N 0.7045(12) 0.6316(10) 0.3682(8) 0.068(5) Uani 1 1 d . U N109 N 0.6037(12) 0.7181(11) 0.3230(8) 0.067(5) Uani 1 1 d . U N110 N 0.5502(12) 0.7507(11) 0.2907(8) 0.082(7) Uani 1 1 d . U H11A H 0.5553 0.7921 0.2811 0.099 Uiso 1 1 calc R U C1 C 0.192(2) 0.9382(15) 0.4962(12) 0.153(13) Uani 1 1 d . U H1A H 0.2196 0.9473 0.4618 0.229 Uiso 1 1 calc R U H1C H 0.1375 0.9612 0.4974 0.229 Uiso 1 1 calc R U H1D H 0.2277 0.9535 0.5258 0.229 Uiso 1 1 calc R U C2 C 0.1382(17) 0.8436(17) 0.5483(13) 0.097(8) Uani 1 1 d . U C3 C 0.1114(19) 0.8850(16) 0.5928(12) 0.121(10) Uani 1 1 d . U H3A H 0.1156 0.9316 0.5919 0.146 Uiso 1 1 calc R U C4 C 0.0803(18) 0.8521(17) 0.6351(13) 0.114(10) Uani 1 1 d . U H4A H 0.0667 0.8779 0.6658 0.137 Uiso 1 1 calc R U C5 C 0.066(2) 0.7868(17) 0.6393(13) 0.125(12) Uani 1 1 d . U H5B H 0.0406 0.7684 0.6704 0.150 Uiso 1 1 calc R U C6 C 0.0907(15) 0.7475(14) 0.5962(11) 0.085(8) Uani 1 1 d . U H6B H 0.0833 0.7012 0.5987 0.102 Uiso 1 1 calc R U C7 C 0.1266(15) 0.7745(16) 0.5487(11) 0.080(7) Uani 1 1 d . U C8 C 0.1546(14) 0.7311(16) 0.5067(11) 0.073(7) Uani 1 1 d . U C9 C 0.1744(15) 0.6662(14) 0.5073(11) 0.082(8) Uani 1 1 d . U H9A H 0.1720 0.6385 0.5380 0.098 Uiso 1 1 calc R U C10 C 0.1990(16) 0.6461(14) 0.4556(11) 0.076(7) Uani 1 1 d . U C11 C 0.2334(14) 0.5891(14) 0.4302(11) 0.070(6) Uani 1 1 d . U C12 C 0.2525(16) 0.5276(13) 0.4532(11) 0.096(9) Uani 1 1 d . U H12A H 0.2421 0.5193 0.4902 0.116 Uiso 1 1 calc R U C13 C 0.2868(18) 0.4796(14) 0.4207(12) 0.113(10) Uani 1 1 d . U H13A H 0.3008 0.4379 0.4355 0.136 Uiso 1 1 calc R U C14 C 0.3005(16) 0.4913(14) 0.3684(11) 0.100(9) Uani 1 1 d . U H14A H 0.3201 0.4567 0.3460 0.120 Uiso 1 1 calc R U C15 C 0.2863(16) 0.5534(15) 0.3466(11) 0.075(7) Uani 1 1 d . U C16 C 0.2957(15) 0.5776(14) 0.2914(11) 0.069(7) Uani 1 1 d . U C17 C 0.3306(14) 0.5501(13) 0.2441(10) 0.079(7) Uani 1 1 d . U H17A H 0.3515 0.5067 0.2391 0.094 Uiso 1 1 calc R U C18 C 0.3276(13) 0.5997(14) 0.2076(11) 0.068(6) Uani 1 1 d . U C19 C 0.3593(14) 0.6088(16) 0.1499(11) 0.080(7) Uani 1 1 d . U C20 C 0.3857(18) 0.5485(16) 0.1259(12) 0.112(9) Uani 1 1 d . U H20A H 0.3816 0.5083 0.1453 0.135 Uiso 1 1 calc R U C21 C 0.418(2) 0.5492(17) 0.0726(13) 0.130(11) Uani 1 1 d . U H21A H 0.4422 0.5113 0.0561 0.156 Uiso 1 1 calc R U C22 C 0.4128(19) 0.6105(18) 0.0460(14) 0.129(11) Uani 1 1 d . U H22A H 0.4295 0.6121 0.0094 0.155 Uiso 1 1 calc R U C23 C 0.3853(17) 0.6678(16) 0.0689(12) 0.110(9) Uani 1 1 d . U H23A H 0.3851 0.7068 0.0478 0.133 Uiso 1 1 calc R U C24 C 0.3568(17) 0.6713(18) 0.1238(14) 0.093(8) Uani 1 1 d . U C25 C 0.3372(18) 0.7858(15) 0.1218(11) 0.124(11) Uani 1 1 d . U H25A H 0.3153 0.8209 0.1449 0.187 Uiso 1 1 calc R U H25B H 0.3966 0.7946 0.1135 0.187 Uiso 1 1 calc R U H25C H 0.3044 0.7844 0.0883 0.187 Uiso 1 1 calc R U C26 C 0.4378(16) 0.7911(13) 0.3959(10) 0.071(8) Uani 1 1 d . U H26A H 0.4876 0.8000 0.4161 0.086 Uiso 1 1 calc R U C27 C 0.4001(16) 0.8358(14) 0.3617(10) 0.084(8) Uani 1 1 d . U H27A H 0.4176 0.8790 0.3523 0.101 Uiso 1 1 calc R U C28 C 0.3281(16) 0.7998(14) 0.3442(10) 0.066(7) Uani 1 1 d . U C29 C 0.2580(15) 0.8133(13) 0.3077(9) 0.060(6) Uani 1 1 d . U C30 C 0.2475(16) 0.8685(12) 0.2747(10) 0.083(8) Uani 1 1 d . U H30A H 0.2895 0.9018 0.2729 0.100 Uiso 1 1 calc R U C31 C 0.1730(17) 0.8732(14) 0.2443(11) 0.103(9) Uani 1 1 d . U H31A H 0.1659 0.9086 0.2198 0.123 Uiso 1 1 calc R U C32 C 0.1091(17) 0.8263(13) 0.2497(9) 0.080(7) Uani 1 1 d . U H32A H 0.0564 0.8327 0.2321 0.096 Uiso 1 1 calc R U C33 C 0.1229(16) 0.7700(14) 0.2808(10) 0.066(7) Uani 1 1 d . U C34 C 0.0722(17) 0.7133(14) 0.2921(10) 0.072(7) Uani 1 1 d . U C35 C -0.0078(15) 0.6913(13) 0.2743(9) 0.078(7) Uani 1 1 d . U H35A H -0.0473 0.7135 0.2519 0.094 Uiso 1 1 calc R U C36 C -0.0147(16) 0.6305(14) 0.2969(10) 0.083(8) Uani 1 1 d . U H36A H -0.0629 0.6030 0.2934 0.099 Uiso 1 1 calc R U C101 C 0.862(3) 0.5111(19) 0.1896(14) 0.26(3) Uani 1 1 d . U H10A H 0.8486 0.4952 0.2258 0.383 Uiso 1 1 calc R U H10B H 0.8292 0.4859 0.1630 0.383 Uiso 1 1 calc R U H10L H 0.9222 0.5054 0.1827 0.383 Uiso 1 1 calc R U C102 C 0.8546(17) 0.6118(17) 0.1360(13) 0.096(8) Uani 1 1 d . U C103 C 0.8813(18) 0.5800(15) 0.0883(12) 0.115(10) Uani 1 1 d . U H10G H 0.8900 0.5337 0.0889 0.138 Uiso 1 1 calc R U C104 C 0.8948(18) 0.6129(17) 0.0423(13) 0.111(10) Uani 1 1 d . U H10H H 0.9137 0.5902 0.0112 0.134 Uiso 1 1 calc R U C105 C 0.8808(17) 0.6809(17) 0.0407(12) 0.106(9) Uani 1 1 d . U H10I H 0.8886 0.7042 0.0080 0.127 Uiso 1 1 calc R U C106 C 0.8550(16) 0.7155(15) 0.0876(11) 0.101(8) Uani 1 1 d . U H10J H 0.8475 0.7619 0.0868 0.121 Uiso 1 1 calc R U C107 C 0.8405(14) 0.6797(16) 0.1357(11) 0.076(6) Uani 1 1 d . U C108 C 0.8184(13) 0.7161(14) 0.1846(10) 0.064(6) Uani 1 1 d . U C109 C 0.8270(12) 0.7835(13) 0.1949(9) 0.060(6) Uani 1 1 d . U H10K H 0.8472 0.8164 0.1711 0.072 Uiso 1 1 calc R U C110 C 0.7984(13) 0.7921(13) 0.2499(10) 0.061(6) Uani 1 1 d . U C111 C 0.7970(14) 0.8498(14) 0.2853(10) 0.057(6) Uani 1 1 d . U C112 C 0.8236(15) 0.9110(14) 0.2723(11) 0.075(7) Uani 1 1 d . U H11B H 0.8458 0.9201 0.2376 0.089 Uiso 1 1 calc R U C113 C 0.8174(14) 0.9611(13) 0.3117(10) 0.073(7) Uani 1 1 d . U H11C H 0.8359 1.0044 0.3034 0.087 Uiso 1 1 calc R U C114 C 0.7850(15) 0.9480(13) 0.3618(11) 0.074(7) Uani 1 1 d . U H11D H 0.7808 0.9812 0.3885 0.089 Uiso 1 1 calc R U C115 C 0.7584(15) 0.8828(15) 0.3718(11) 0.070(7) Uani 1 1 d . U C116 C 0.7197(15) 0.8595(15) 0.4211(11) 0.075(7) Uani 1 1 d . U C117 C 0.7050(16) 0.8948(14) 0.4701(10) 0.092(8) Uani 1 1 d . U H11E H 0.7159 0.9399 0.4774 0.111 Uiso 1 1 calc R U C118 C 0.6717(16) 0.8485(15) 0.5039(12) 0.082(7) Uani 1 1 d . U C119 C 0.6434(16) 0.8635(18) 0.5635(12) 0.099(7) Uani 1 1 d . U C120 C 0.6400(19) 0.9318(18) 0.5776(12) 0.129(11) Uani 1 1 d . U H12B H 0.6510 0.9654 0.5519 0.155 Uiso 1 1 calc R U C121 C 0.619(2) 0.9474(19) 0.6325(14) 0.153(13) Uani 1 1 d . U H12C H 0.6157 0.9917 0.6445 0.184 Uiso 1 1 calc R U C122 C 0.604(2) 0.8955(19) 0.6670(14) 0.140(12) Uani 1 1 d . U H12D H 0.5944 0.9062 0.7037 0.168 Uiso 1 1 calc R U C123 C 0.6014(16) 0.8289(17) 0.6534(12) 0.110(8) Uani 1 1 d . U H12E H 0.5863 0.7955 0.6784 0.132 Uiso 1 1 calc R U C124 C 0.6234(17) 0.815(2) 0.5986(14) 0.109(9) Uani 1 1 d . U C125 C 0.6088(19) 0.6983(16) 0.6168(12) 0.139(11) Uani 1 1 d . U H12H H 0.6173 0.6556 0.5993 0.209 Uiso 1 1 calc R U H12I H 0.6444 0.7009 0.6491 0.209 Uiso 1 1 calc R U H12J H 0.5494 0.7029 0.6270 0.209 Uiso 1 1 calc R U C126 C 0.9560(16) 0.6648(13) 0.4425(10) 0.080(8) Uani 1 1 d . U H12F H 1.0086 0.6693 0.4606 0.097 Uiso 1 1 calc R U C127 C 0.9085(15) 0.6101(13) 0.4401(9) 0.082(8) Uani 1 1 d . U H12G H 0.9198 0.5678 0.4548 0.099 Uiso 1 1 calc R U C128 C 0.8376(15) 0.6312(14) 0.4101(10) 0.071(7) Uani 1 1 d . U C129 C 0.7613(15) 0.5919(14) 0.3940(8) 0.060(6) Uani 1 1 d . U C130 C 0.7467(17) 0.5249(14) 0.4020(10) 0.092(8) Uani 1 1 d . U H13B H 0.7882 0.4969 0.4174 0.110 Uiso 1 1 calc R U C131 C 0.6669(17) 0.5009(14) 0.3858(11) 0.102(9) Uani 1 1 d . U H13C H 0.6531 0.4559 0.3915 0.123 Uiso 1 1 calc R U C132 C 0.6117(17) 0.5400(15) 0.3630(10) 0.092(8) Uani 1 1 d . U H13D H 0.5582 0.5229 0.3526 0.110 Uiso 1 1 calc R U C133 C 0.6300(16) 0.6066(15) 0.3537(9) 0.069(7) Uani 1 1 d . U C134 C 0.5751(15) 0.6539(14) 0.3244(9) 0.065(6) Uani 1 1 d . U C135 C 0.5013(16) 0.6485(14) 0.2952(10) 0.090(8) Uani 1 1 d . U H13E H 0.4677 0.6102 0.2901 0.108 Uiso 1 1 calc R U C136 C 0.4873(16) 0.7102(14) 0.2752(10) 0.083(8) Uani 1 1 d . U H13F H 0.4403 0.7226 0.2536 0.100 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 0.093(6) 0.117(8) 0.103(7) 0.000(6) 0.006(6) -0.007(6) O1_1 0.101(9) 0.130(15) 0.089(13) 0.018(10) 0.007(9) -0.001(9) O2_1 0.138(15) 0.173(17) 0.159(13) -0.028(11) -0.022(11) 0.015(12) O3_1 0.125(15) 0.124(11) 0.229(19) -0.016(10) 0.006(13) -0.002(10) O4_1 0.170(17) 0.142(15) 0.150(13) 0.013(11) 0.037(11) -0.009(12) Cl1_2 0.090(7) 0.134(9) 0.101(7) 0.021(6) -0.004(5) -0.015(5) O1_2 0.078(12) 0.143(12) 0.122(14) 0.005(9) -0.004(10) -0.011(8) O2_2 0.093(12) 0.191(17) 0.132(11) 0.049(10) -0.003(9) -0.009(11) O3_2 0.112(11) 0.128(15) 0.142(14) 0.034(11) -0.037(10) -0.038(10) O4_2 0.136(14) 0.151(14) 0.150(15) 0.007(10) 0.015(11) -0.007(10) Cl1_3 0.115(8) 0.094(8) 0.131(8) -0.015(6) 0.002(6) -0.017(6) O1_3 0.146(13) 0.112(13) 0.152(16) 0.021(11) -0.033(11) -0.026(10) O2_3 0.150(17) 0.123(12) 0.225(19) -0.032(11) 0.027(13) -0.013(10) O3_3 0.186(16) 0.143(16) 0.194(15) -0.008(12) -0.047(12) -0.017(12) O4_3 0.193(18) 0.138(17) 0.192(14) 0.007(12) 0.044(12) -0.011(13) Cl1_4 0.110(6) 0.147(9) 0.086(7) -0.003(6) -0.028(6) 0.017(7) O1_4 0.133(14) 0.094(13) 0.102(11) 0.005(9) -0.035(10) 0.022(10) O2_4 0.171(17) 0.177(12) 0.153(17) -0.033(11) -0.051(13) 0.034(11) O3_4 0.224(19) 0.234(18) 0.122(13) 0.022(11) -0.031(11) -0.024(14) O4_4 0.135(10) 0.27(2) 0.123(16) -0.038(14) -0.032(10) 0.025(10) Fe01 0.059(3) 0.074(3) 0.060(3) 0.012(2) -0.005(2) 0.004(2) Fe02 0.055(3) 0.077(3) 0.070(3) 0.005(2) -0.001(2) -0.007(2) O1 0.140(16) 0.107(14) 0.099(12) -0.003(11) 0.004(10) -0.037(12) O2 0.112(15) 0.115(15) 0.089(13) 0.008(9) -0.012(10) -0.013(12) O101 0.19(2) 0.102(14) 0.085(12) -0.011(11) 0.017(11) 0.002(12) O102 0.092(15) 0.149(15) 0.094(13) -0.002(10) 0.002(11) -0.011(12) N1 0.035(11) 0.079(10) 0.076(9) 0.000(7) -0.012(8) -0.017(8) N2 0.070(12) 0.081(10) 0.067(7) 0.007(6) -0.005(6) -0.002(8) N3 0.065(12) 0.074(8) 0.064(8) 0.012(6) -0.004(7) 0.000(7) N4 0.055(11) 0.084(9) 0.067(7) 0.007(6) -0.006(7) 0.000(8) N5 0.071(13) 0.091(12) 0.065(9) 0.003(7) -0.009(8) -0.003(9) N6 0.070(10) 0.075(12) 0.071(12) 0.007(10) -0.009(9) 0.001(8) N7 0.060(8) 0.067(9) 0.054(10) 0.007(7) 0.000(6) 0.003(7) N8 0.068(8) 0.075(8) 0.064(11) 0.012(7) 0.005(7) 0.007(6) N9 0.063(7) 0.086(11) 0.074(11) 0.021(8) -0.004(7) -0.002(6) N10 0.065(10) 0.087(11) 0.065(13) 0.017(9) 0.002(9) 0.000(8) N101 0.058(12) 0.086(10) 0.072(9) -0.008(7) -0.003(8) -0.007(8) N102 0.043(10) 0.078(9) 0.065(7) -0.002(6) -0.009(6) -0.002(8) N103 0.044(11) 0.073(8) 0.063(8) 0.003(6) -0.010(7) 0.008(7) N104 0.064(13) 0.091(9) 0.067(8) 0.002(7) -0.005(7) -0.002(8) N105 0.068(14) 0.109(12) 0.075(10) 0.002(8) -0.001(9) -0.005(10) N106 0.068(10) 0.089(12) 0.088(15) -0.003(9) -0.008(9) -0.001(8) N107 0.064(8) 0.083(10) 0.080(12) 0.000(8) -0.009(8) -0.001(7) N108 0.060(9) 0.078(8) 0.067(11) -0.005(7) -0.003(7) -0.004(6) N109 0.054(8) 0.087(10) 0.061(11) -0.005(8) 0.003(7) -0.002(6) N110 0.064(12) 0.100(12) 0.084(15) 0.003(10) -0.013(10) -0.008(8) C1 0.22(3) 0.110(16) 0.13(2) 0.004(15) -0.02(2) -0.055(17) C2 0.106(19) 0.091(12) 0.095(13) -0.005(10) -0.004(12) -0.013(11) C3 0.16(3) 0.100(15) 0.103(15) -0.010(12) 0.012(15) -0.012(13) C4 0.14(3) 0.097(17) 0.104(15) -0.005(13) 0.013(15) 0.001(16) C5 0.18(3) 0.099(17) 0.099(14) -0.008(12) 0.038(16) 0.000(16) C6 0.082(18) 0.093(15) 0.079(12) 0.003(10) -0.001(11) 0.007(12) C7 0.076(16) 0.090(12) 0.075(11) -0.002(9) -0.006(10) -0.003(10) C8 0.061(16) 0.082(12) 0.075(9) -0.001(8) -0.005(9) -0.012(10) C9 0.083(19) 0.086(12) 0.076(9) 0.003(8) 0.000(9) -0.005(11) C10 0.084(18) 0.077(10) 0.068(9) 0.010(7) -0.001(9) -0.002(9) C11 0.067(16) 0.077(10) 0.066(9) 0.014(7) -0.004(9) -0.004(9) C12 0.13(2) 0.085(12) 0.076(12) 0.022(9) 0.009(12) 0.017(12) C13 0.16(3) 0.095(13) 0.084(13) 0.023(10) 0.018(13) 0.030(14) C14 0.13(2) 0.087(11) 0.081(12) 0.014(9) 0.011(12) 0.019(11) C15 0.073(18) 0.080(10) 0.071(9) 0.009(7) 0.002(9) 0.004(10) C16 0.052(16) 0.084(10) 0.071(8) 0.005(7) -0.004(8) 0.000(9) C17 0.071(16) 0.091(12) 0.074(10) 0.000(8) 0.002(10) 0.003(10) C18 0.043(13) 0.089(13) 0.070(9) -0.005(7) -0.015(8) -0.013(10) C19 0.056(15) 0.113(14) 0.071(10) -0.001(8) -0.013(9) -0.018(11) C20 0.12(2) 0.121(15) 0.092(14) -0.007(10) 0.007(14) -0.007(13) C21 0.15(3) 0.143(19) 0.098(16) -0.007(11) 0.018(16) -0.007(16) C22 0.15(3) 0.146(19) 0.090(15) -0.004(12) 0.007(14) -0.013(17) C23 0.11(2) 0.137(18) 0.080(13) 0.004(11) -0.003(12) -0.020(14) C24 0.086(19) 0.117(14) 0.076(12) 0.006(9) -0.013(11) -0.020(11) C25 0.15(3) 0.125(17) 0.10(2) 0.023(12) -0.012(19) -0.015(14) C26 0.072(12) 0.073(14) 0.069(16) -0.001(11) 0.003(11) 0.000(10) C27 0.080(13) 0.077(12) 0.096(18) 0.010(10) -0.009(11) -0.005(10) C28 0.067(10) 0.068(10) 0.063(13) 0.010(9) 0.004(9) 0.003(8) C29 0.063(9) 0.072(10) 0.046(12) 0.005(8) 0.013(8) 0.010(7) C30 0.091(13) 0.083(12) 0.076(16) 0.026(11) 0.004(11) 0.005(10) C31 0.101(14) 0.107(15) 0.100(18) 0.041(14) -0.010(12) -0.001(11) C32 0.087(13) 0.089(13) 0.065(15) 0.019(11) 0.004(11) 0.013(9) C33 0.064(10) 0.081(11) 0.053(14) 0.009(9) 0.011(9) 0.013(8) C34 0.066(10) 0.089(11) 0.061(15) 0.017(9) 0.002(9) 0.005(8) C35 0.070(10) 0.093(14) 0.071(16) 0.018(11) -0.001(10) 0.004(9) C36 0.067(11) 0.098(15) 0.083(19) 0.025(12) -0.004(10) 0.000(10) C101 0.53(7) 0.118(17) 0.12(3) 0.000(17) 0.04(3) 0.08(2) C102 0.11(2) 0.104(12) 0.078(12) -0.015(9) -0.003(11) 0.002(11) C103 0.14(2) 0.118(16) 0.087(13) -0.024(11) 0.010(14) 0.001(13) C104 0.12(2) 0.126(18) 0.090(14) -0.020(12) 0.005(14) -0.005(16) C105 0.12(2) 0.125(18) 0.078(12) -0.023(12) -0.006(12) -0.006(16) C106 0.12(2) 0.110(15) 0.071(11) -0.009(10) 0.000(11) -0.004(13) C107 0.060(15) 0.102(12) 0.066(10) -0.014(9) -0.014(9) -0.005(10) C108 0.036(14) 0.089(11) 0.067(9) -0.009(8) -0.013(8) -0.013(10) C109 0.037(13) 0.087(11) 0.056(9) -0.003(7) -0.021(8) -0.009(9) C110 0.048(14) 0.077(9) 0.057(9) 0.001(7) -0.016(8) -0.003(8) C111 0.036(14) 0.076(9) 0.058(9) 0.002(7) -0.018(8) 0.001(8) C112 0.069(17) 0.079(11) 0.076(12) 0.005(8) -0.012(11) -0.004(10) C113 0.061(16) 0.076(12) 0.080(13) 0.002(9) -0.012(11) -0.007(10) C114 0.064(17) 0.076(11) 0.082(13) 0.002(9) -0.008(11) 0.004(10) C115 0.064(16) 0.075(10) 0.070(9) -0.003(7) -0.003(9) 0.002(9) C116 0.066(16) 0.087(10) 0.071(9) -0.002(7) 0.000(9) 0.000(9) C117 0.094(19) 0.104(12) 0.078(10) -0.010(8) 0.009(10) -0.011(11) C118 0.062(18) 0.109(13) 0.075(9) -0.003(8) 0.000(9) -0.001(11) C119 0.072(17) 0.145(15) 0.079(10) -0.010(9) 0.002(9) -0.008(12) C120 0.16(3) 0.139(15) 0.084(14) -0.016(11) 0.024(15) -0.008(13) C121 0.20(4) 0.167(19) 0.094(16) -0.020(12) 0.029(18) -0.001(16) C122 0.15(3) 0.170(19) 0.100(16) -0.012(13) 0.023(15) 0.000(18) C123 0.077(18) 0.168(19) 0.085(13) -0.006(11) 0.006(11) 0.002(16) C124 0.09(2) 0.151(15) 0.086(12) -0.003(10) 0.008(12) -0.010(12) C125 0.15(3) 0.166(19) 0.11(2) 0.009(14) -0.003(19) -0.032(16) C126 0.067(11) 0.084(15) 0.090(17) -0.005(12) -0.019(11) -0.004(9) C127 0.072(12) 0.084(13) 0.090(17) 0.001(11) -0.019(11) -0.005(9) C128 0.068(10) 0.083(10) 0.063(15) -0.007(9) -0.006(9) 0.001(7) C129 0.060(9) 0.079(10) 0.042(13) -0.011(8) 0.010(8) 0.003(7) C130 0.094(14) 0.083(11) 0.097(19) 0.002(10) -0.013(13) -0.004(9) C131 0.096(14) 0.089(12) 0.12(2) 0.005(11) -0.019(13) -0.005(10) C132 0.085(14) 0.087(11) 0.10(2) 0.003(10) -0.014(13) -0.012(9) C133 0.055(10) 0.083(10) 0.069(15) -0.007(9) 0.004(9) -0.005(7) C134 0.054(10) 0.087(10) 0.055(14) -0.011(9) 0.008(9) -0.004(7) C135 0.069(12) 0.100(14) 0.101(19) -0.001(11) -0.016(12) -0.011(10) C136 0.062(12) 0.104(15) 0.084(17) -0.003(12) -0.010(12) -0.007(10) 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 O3_1 Cl1_1 O2_1 113.7(10) O3_1 Cl1_1 O1_1 111.6(9) O2_1 Cl1_1 O1_1 110.4(9) O3_1 Cl1_1 O4_1 108.0(10) O2_1 Cl1_1 O4_1 106.5(10) O1_1 Cl1_1 O4_1 106.2(9) O4_2 Cl1_2 O2_2 109.2(10) O4_2 Cl1_2 O1_2 110.0(10) O2_2 Cl1_2 O1_2 110.3(9) O4_2 Cl1_2 O3_2 109.5(10) O2_2 Cl1_2 O3_2 109.2(9) O1_2 Cl1_2 O3_2 108.7(9) O2_3 Cl1_3 O1_3 112.0(10) O2_3 Cl1_3 O4_3 109.7(10) O1_3 Cl1_3 O4_3 109.2(10) O2_3 Cl1_3 O3_3 110.5(10) O1_3 Cl1_3 O3_3 108.5(10) O4_3 Cl1_3 O3_3 106.7(10) O3_4 Cl1_4 O1_4 111.9(10) O3_4 Cl1_4 O4_4 108.8(10) O1_4 Cl1_4 O4_4 111.7(9) O3_4 Cl1_4 O2_4 107.9(10) O1_4 Cl1_4 O2_4 109.3(9) O4_4 Cl1_4 O2_4 107.1(10) N3 Fe01 N8 173.6(9) N3 Fe01 N2 79.7(9) N8 Fe01 N2 106.0(9) N3 Fe01 N7 103.4(8) N8 Fe01 N7 80.0(9) N2 Fe01 N7 88.9(8) N3 Fe01 N9 98.2(8) N8 Fe01 N9 78.5(9) N2 Fe01 N9 94.2(8) N7 Fe01 N9 158.3(9) N3 Fe01 N4 79.1(9) N8 Fe01 N4 95.3(9) N2 Fe01 N4 158.7(9) N7 Fe01 N4 94.5(8) N9 Fe01 N4 90.4(8) N103 Fe02 N107 104.6(8) N103 Fe02 N108 173.9(8) N107 Fe02 N108 74.1(8) N103 Fe02 N109 106.5(8) N107 Fe02 N109 148.6(9) N108 Fe02 N109 74.6(8) N103 Fe02 N102 73.0(8) N107 Fe02 N102 97.3(7) N108 Fe02 N102 101.2(8) N109 Fe02 N102 87.4(7) N103 Fe02 N104 73.9(9) N107 Fe02 N104 93.5(8) N108 Fe02 N104 112.0(8) N109 Fe02 N104 99.5(7) N102 Fe02 N104 146.8(8) C2 O1 C1 119(3) C24 O2 C25 119(3) C102 O101 C101 116(3) C124 O102 C125 116(3) N2 N1 C8 110(2) N2 N1 H1B 124.9 C8 N1 H1B 124.9 N1 N2 C10 108(2) N1 N2 Fe01 136.3(18) C10 N2 Fe01 115(2) C11 N3 C15 124(3) C11 N3 Fe01 118(2) C15 N3 Fe01 118(2) C16 N4 N5 107(2) C16 N4 Fe01 115.9(19) N5 N4 Fe01 137.5(18) N4 N5 C18 110(2) N4 N5 H5A 125.2 C18 N5 H5A 125.2 C26 N6 N7 108(2) C26 N6 H6A 126.0 N7 N6 H6A 126.0 C28 N7 N6 105(2) C28 N7 Fe01 117.4(17) N6 N7 Fe01 136.1(16) C33 N8 C29 125(2) C33 N8 Fe01 119.5(19) C29 N8 Fe01 115.1(18) N10 N9 C34 109(2) N10 N9 Fe01 136.3(17) C34 N9 Fe01 114.8(19) N9 N10 C36 108(2) N9 N10 H10C 126.2 C36 N10 H10C 126.2 C108 N101 N102 114(2) C108 N101 H10D 123.1 N102 N101 H10D 123.1 C110 N102 N101 105(2) C110 N102 Fe02 116.2(18) N101 N102 Fe02 139.2(17) C115 N103 C111 117(2) C115 N103 Fe02 121(2) C111 N103 Fe02 122.0(19) C116 N104 N105 107(2) C116 N104 Fe02 112.5(19) N105 N104 Fe02 140.3(19) C118 N105 N104 109(2) C118 N105 H10E 125.5 N104 N105 H10E 125.5 C126 N106 N107 116(2) C126 N106 H10F 121.8 N107 N106 H10F 121.8 N106 N107 C128 98(2) N106 N107 Fe02 142.9(18) C128 N107 Fe02 116.8(17) C133 N108 C129 119(2) C133 N108 Fe02 119.6(19) C129 N108 Fe02 121.3(17) N110 N109 C134 106(2) N110 N109 Fe02 136.2(18) C134 N109 Fe02 115.9(17) N109 N110 C136 110(2) N109 N110 H11A 125.2 C136 N110 H11A 125.2 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 O1 C2 C7 114(3) O1 C2 C3 124(3) C7 C2 C3 122(3) C4 C3 C2 115(3) C4 C3 H3A 122.6 C2 C3 H3A 122.6 C3 C4 C5 128(4) C3 C4 H4A 116.1 C5 C4 H4A 116.1 C4 C5 C6 117(3) C4 C5 H5B 121.4 C6 C5 H5B 121.4 C5 C6 C7 122(3) C5 C6 H6B 119.0 C7 C6 H6B 119.0 C2 C7 C6 116(3) C2 C7 C8 124(3) C6 C7 C8 119(3) C9 C8 N1 105(3) C9 C8 C7 131(3) N1 C8 C7 124(3) C8 C9 C10 110(3) C8 C9 H9A 125.1 C10 C9 H9A 125.1 N2 C10 C9 107(3) N2 C10 C11 115(3) C9 C10 C11 138(3) N3 C11 C12 119(3) N3 C11 C10 113(3) C12 C11 C10 128(3) C13 C12 C11 118(3) C13 C12 H12A 120.9 C11 C12 H12A 120.9 C14 C13 C12 121(3) C14 C13 H13A 119.7 C12 C13 H13A 119.7 C13 C14 C15 121(3) C13 C14 H14A 119.6 C15 C14 H14A 119.6 N3 C15 C14 117(3) N3 C15 C16 112(3) C14 C15 C16 131(3) N4 C16 C17 111(3) N4 C16 C15 115(3) C17 C16 C15 133(3) C18 C17 C16 104(3) C18 C17 H17A 127.8 C16 C17 H17A 127.8 C17 C18 N5 108(3) C17 C18 C19 135(3) N5 C18 C19 117(3) C20 C19 C24 126(3) C20 C19 C18 113(3) C24 C19 C18 122(3) C19 C20 C21 119(3) C19 C20 H20A 120.3 C21 C20 H20A 120.3 C22 C21 C20 115(3) C22 C21 H21A 122.6 C20 C21 H21A 122.6 C23 C22 C21 125(4) C23 C22 H22A 117.4 C21 C22 H22A 117.4 C22 C23 C24 123(3) C22 C23 H23A 118.7 C24 C23 H23A 118.7 O2 C24 C19 122(4) O2 C24 C23 125(3) C19 C24 C23 112(3) 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 112(3) N6 C26 H26A 123.9 C27 C26 H26A 123.9 C26 C27 C28 101(3) C26 C27 H27A 129.4 C28 C27 H27A 129.4 N7 C28 C27 113(2) N7 C28 C29 112(2) C27 C28 C29 135(3) N8 C29 C30 119(2) N8 C29 C28 114(2) C30 C29 C28 127(3) C31 C30 C29 118(3) C31 C30 H30A 121.1 C29 C30 H30A 121.1 C32 C31 C30 121(3) C32 C31 H31A 119.6 C30 C31 H31A 119.6 C31 C32 C33 120(3) C31 C32 H32A 120.0 C33 C32 H32A 120.0 N8 C33 C32 117(3) N8 C33 C34 110(3) C32 C33 C34 133(3) N9 C34 C35 109(3) N9 C34 C33 117(3) C35 C34 C33 134(3) C36 C35 C34 103(2) C36 C35 H35A 128.3 C34 C35 H35A 128.3 N10 C36 C35 111(3) N10 C36 H36A 124.3 C35 C36 H36A 124.3 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 114(3) O101 C102 C103 126(3) C107 C102 C103 120(3) C104 C103 C102 122(3) C104 C103 H10G 118.8 C102 C103 H10G 118.8 C103 C104 C105 119(3) C103 C104 H10H 120.3 C105 C104 H10H 120.3 C104 C105 C106 121(3) C104 C105 H10I 119.6 C106 C105 H10I 119.6 C107 C106 C105 119(3) C107 C106 H10J 120.5 C105 C106 H10J 120.5 C102 C107 C106 119(3) C102 C107 C108 122(3) C106 C107 C108 119(3) N101 C108 C109 107(2) N101 C108 C107 125(3) C109 C108 C107 128(3) C108 C109 C110 105(2) C108 C109 H10K 127.5 C110 C109 H10K 127.5 N102 C110 C109 110(2) N102 C110 C111 118(3) C109 C110 C111 132(3) C112 C111 N103 124(3) C112 C111 C110 126(3) N103 C111 C110 110(3) C111 C112 C113 118(3) C111 C112 H11B 120.9 C113 C112 H11B 120.9 C114 C113 C112 121(3) C114 C113 H11C 119.5 C112 C113 H11C 119.5 C113 C114 C115 117(3) C113 C114 H11D 121.5 C115 C114 H11D 121.5 N103 C115 C114 123(3) N103 C115 C116 111(3) C114 C115 C116 126(3) N104 C116 C117 110(3) N104 C116 C115 121(3) C117 C116 C115 129(3) C118 C117 C116 104(3) C118 C117 H11E 128.0 C116 C117 H11E 128.0 N105 C118 C117 110(3) N105 C118 C119 126(3) C117 C118 C119 124(3) C124 C119 C120 123(3) C124 C119 C118 122(3) C120 C119 C118 115(3) C119 C120 C121 117(3) C119 C120 H12B 121.5 C121 C120 H12B 121.5 C122 C121 C120 118(4) C122 C121 H12C 121.2 C120 C121 H12C 121.2 C121 C122 C123 126(4) C121 C122 H12D 116.8 C123 C122 H12D 116.8 C122 C123 C124 115(4) C122 C123 H12E 122.6 C124 C123 H12E 122.6 C119 C124 O102 116(3) C119 C124 C123 121(4) O102 C124 C123 122(4) 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 N106 C126 C127 108(3) N106 C126 H12F 126.2 C127 C126 H12F 126.2 C126 C127 C128 102(3) C126 C127 H12G 128.8 C128 C127 H12G 128.8 N107 C128 C127 115(2) N107 C128 C129 117(2) C127 C128 C129 128(3) N108 C129 C130 122(2) N108 C129 C128 110(3) C130 C129 C128 128(3) C129 C130 C131 116(3) C129 C130 H13B 121.8 C131 C130 H13B 121.8 C132 C131 C130 121(3) C132 C131 H13C 119.7 C130 C131 H13C 119.7 C131 C132 C133 121(3) C131 C132 H13D 119.4 C133 C132 H13D 119.4 N108 C133 C132 120(3) N108 C133 C134 114(3) C132 C133 C134 126(3) C135 C134 N109 110(3) C135 C134 C133 134(3) N109 C134 C133 116(2) C136 C135 C134 105(3) C136 C135 H13E 127.6 C134 C135 H13E 127.6 N110 C136 C135 110(3) N110 C136 H13F 125.2 C135 C136 H13F 125.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1_1 O3_1 1.383(9) Cl1_1 O2_1 1.394(9) Cl1_1 O1_1 1.403(9) Cl1_1 O4_1 1.422(9) Cl1_2 O4_2 1.400(9) Cl1_2 O2_2 1.401(9) Cl1_2 O1_2 1.404(9) Cl1_2 O3_2 1.408(9) Cl1_3 O2_3 1.383(9) Cl1_3 O1_3 1.399(9) Cl1_3 O4_3 1.402(9) Cl1_3 O3_3 1.405(9) Cl1_4 O3_4 1.394(9) Cl1_4 O1_4 1.396(9) Cl1_4 O4_4 1.405(9) Cl1_4 O2_4 1.408(9) Fe01 N3 1.943(19) Fe01 N8 1.947(19) Fe01 N2 1.95(2) Fe01 N7 1.954(19) Fe01 N9 1.96(2) Fe01 N4 1.97(2) Fe02 N103 2.12(2) Fe02 N107 2.13(2) Fe02 N108 2.13(2) Fe02 N109 2.153(19) Fe02 N102 2.19(2) Fe02 N104 2.23(2) O1 C2 1.40(3) O1 C1 1.44(3) O2 C24 1.31(3) O2 C25 1.39(3) O101 C102 1.37(3) O101 C101 1.47(3) O102 C124 1.36(3) O102 C125 1.45(3) N1 N2 1.33(2) N1 C8 1.40(3) N1 H1B 0.8700 N2 C10 1.35(3) N3 C11 1.32(3) N3 C15 1.32(3) N4 C16 1.31(2) N4 N5 1.34(2) N5 C18 1.37(3) N5 H5A 0.8700 N6 C26 1.34(2) N6 N7 1.39(2) N6 H6A 0.8700 N7 C28 1.33(2) N8 C33 1.33(3) N8 C29 1.36(3) N9 N10 1.32(2) N9 C34 1.33(3) N10 C36 1.33(2) N10 H10C 0.8700 N101 C108 1.33(3) N101 N102 1.36(2) N101 H10D 0.8700 N102 C110 1.34(2) N103 C115 1.35(3) N103 C111 1.37(3) N104 C116 1.33(3) N104 N105 1.35(2) N105 C118 1.35(3) N105 H10E 0.8700 N106 C126 1.32(2) N106 N107 1.33(2) N106 H10F 0.8700 N107 C128 1.36(3) N108 C133 1.32(3) N108 C129 1.35(3) N109 N110 1.33(2) N109 C134 1.37(2) N110 C136 1.33(3) N110 H11A 0.8700 C1 H1A 0.9700 C1 H1C 0.9700 C1 H1D 0.9700 C2 C7 1.40(3) C2 C3 1.44(4) C3 C4 1.33(3) C3 H3A 0.9400 C4 C5 1.34(3) C4 H4A 0.9400 C5 C6 1.38(3) C5 H5B 0.9400 C6 C7 1.41(3) C6 H6B 0.9400 C7 C8 1.42(3) C8 C9 1.34(3) C9 C10 1.39(3) C9 H9A 0.9400 C10 C11 1.41(3) C11 C12 1.39(3) C12 C13 1.36(3) C12 H12A 0.9400 C13 C14 1.33(3) C13 H13A 0.9400 C14 C15 1.38(3) C14 H14A 0.9400 C15 C16 1.45(3) C16 C17 1.40(3) C17 C18 1.34(3) C17 H17A 0.9400 C18 C19 1.52(3) C19 C20 1.41(3) C19 C24 1.41(4) C20 C21 1.41(4) C20 H20A 0.9400 C21 C22 1.40(3) C21 H21A 0.9400 C22 C23 1.35(3) C22 H22A 0.9400 C23 C24 1.43(4) C23 H23A 0.9400 C25 H25A 0.9700 C25 H25B 0.9700 C25 H25C 0.9700 C26 C27 1.36(3) C26 H26A 0.9400 C27 C28 1.41(3) C27 H27A 0.9400 C28 C29 1.44(3) C29 C30 1.39(3) C30 C31 1.39(3) C30 H30A 0.9400 C31 C32 1.38(3) C31 H31A 0.9400 C32 C33 1.38(3) C32 H32A 0.9400 C33 C34 1.42(3) C34 C35 1.40(3) C35 C36 1.35(3) C35 H35A 0.9400 C36 H36A 0.9400 C101 H10A 0.9700 C101 H10B 0.9700 C101 H10L 0.9700 C102 C107 1.38(3) C102 C103 1.40(3) C103 C104 1.33(3) C103 H10G 0.9400 C104 C105 1.38(3) C104 H10H 0.9400 C105 C106 1.41(3) C105 H10I 0.9400 C106 C107 1.40(3) C106 H10J 0.9400 C107 C108 1.45(3) C108 C109 1.38(3) C109 C110 1.44(3) C109 H10K 0.9400 C110 C111 1.45(3) C111 C112 1.34(3) C112 C113 1.40(3) C112 H11B 0.9400 C113 C114 1.36(3) C113 H11C 0.9400 C114 C115 1.40(3) C114 H11D 0.9400 C115 C116 1.44(3) C116 C117 1.42(3) C117 C118 1.35(3) C117 H11E 0.9400 C118 C119 1.56(4) C119 C124 1.35(4) C119 C120 1.42(3) C120 C121 1.43(4) C120 H12B 0.9400 C121 C122 1.37(4) C121 H12C 0.9400 C122 C123 1.38(4) C122 H12D 0.9400 C123 C124 1.42(4) C123 H12E 0.9400 C125 H12H 0.9700 C125 H12I 0.9700 C125 H12J 0.9700 C126 C127 1.33(3) C126 H12F 0.9400 C127 C128 1.40(3) C127 H12G 0.9400 C128 C129 1.49(3) C129 C130 1.38(3) C130 C131 1.40(3) C130 H13B 0.9400 C131 C132 1.30(3) C131 H13C 0.9400 C132 C133 1.39(3) C132 H13D 0.9400 C133 C134 1.47(3) C134 C135 1.36(3) C135 C136 1.35(3) C135 H13E 0.9400 C136 H13F 0.9400