#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:25:44 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173540 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/18/1541896.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_1541896 loop_ _publ_author_name 'Aromi, Guillem' 'Beavers, Christine' 'Costa, Jos\'e S\'anchez' 'Craig, Gavin A.' 'Minguez Espallargas, Guillermo' 'Orera, Alodia' 'Roubeau, Olivier' _publ_section_title ; Snapshots of a Solid-State Transformation: Coexistence of Three Phases Trapped in One Crystal. ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C5SC04287A _journal_year 2016 _chemical_formula_moiety ; C36 H30 Fe N10 O2, 2(Cl O4), 1.35(C3 H6 O) ; _chemical_formula_sum 'C40.05 H38.1 Cl2 Fe N10 O11.35' _chemical_formula_weight 967.85 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 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 114.3394(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.1613(12) _cell_length_b 21.6112(18) _cell_length_c 15.3855(13) _cell_measurement_reflns_used 9477 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 32.8 _cell_measurement_theta_min 2.96 _cell_volume 4290.1(6) _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 SHELXS _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_orient_matrix_type 'Sparks (1982)' _diffrn_orient_matrix_UB_11 -0.04806 _diffrn_orient_matrix_UB_12 0.01315 _diffrn_orient_matrix_UB_13 0.02930 _diffrn_orient_matrix_UB_21 0.01128 _diffrn_orient_matrix_UB_22 -0.04045 _diffrn_orient_matrix_UB_23 0.03438 _diffrn_orient_matrix_UB_31 0.05975 _diffrn_orient_matrix_UB_32 0.01821 _diffrn_orient_matrix_UB_33 0.05521 _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 0.0631 _diffrn_reflns_av_unetI/netI 0.0655 _diffrn_reflns_laue_measured_fraction_full 0.994 _diffrn_reflns_laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 46488 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 27.706 _diffrn_reflns_theta_max 33.613 _diffrn_reflns_theta_min 2.963 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Sheldrick, 2012)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_description block _exptl_crystal_F_000 1997 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.215 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 580 _refine_ls_number_reflns 13023 _refine_ls_number_restraints 403 _refine_ls_restrained_S_all 1.201 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0767 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+3.4646P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2215 _refine_ls_wR_factor_ref 0.2351 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10342 _reflns_number_total 13023 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage1_Initial _cod_original_formula_sum 'C40.05 H38.10 Cl2 Fe N10 O11.35' _cod_database_code 1541896 _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 0.934 _shelx_estimated_absorpt_t_max 0.966 _shelx_res_file ; tmajor.res created by SHELXL-2014/7 TITL tmajor in P2(1)/n CELL 0.77490 14.16130 21.61120 15.38550 90.0000 114.3394 90.0000 ZERR 4.00 0.00120 0.00180 0.00130 0.0000 0.0011 0.0000 LATT 1 SYMM 0.5-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 160.2 152.4 40 45.4 8 4 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! SIZE 0.1 0.07 0.05 !dark red block TEMP -23 SADI 0.01 C40 C41 C40 C42 C37 C38 C37 C39 SADI 0.01 C40 O4 C37 O3 SIMU 0.01 C41 C42 C38 C39 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 REM RIGU ISOR O4_4 L.S. 10 PLAN 20 ACTA Bond $h EQIV $1 x-1/2, -y+1/2, z-1/2 HTAB Htab N1 O4_4 HTAB N1 O4_3 HTAB N5 O2 HTAB N6 O1_2 HTAB N6 O1_1 HTAB N6 Cl1_1 HTAB N6 Cl1_2 HTAB N10 O3_$1 WGHT 0.130700 3.464600 FVAR 0.18770 0.53223 0.50232 FE1 6 0.424615 0.264802 0.603082 11.00000 0.02641 0.02517 = 0.02610 -0.00073 0.01161 0.00150 O1 4 0.276750 0.342039 0.956689 11.00000 0.13287 0.09720 = 0.09650 -0.03127 0.08798 -0.01238 O2 4 0.504055 0.176424 0.322017 11.00000 0.09678 0.04649 = 0.08506 -0.01001 0.06503 -0.00667 O3 4 0.662279 0.123958 0.921531 11.00000 0.07689 0.06333 = 0.09047 -0.00250 0.03395 -0.01958 N1 3 0.362348 0.237931 0.772604 11.00000 0.03963 0.04835 = 0.03304 0.00159 0.01834 -0.00210 AFIX 43 H1 2 0.369276 0.197893 0.776206 11.00000 -1.20000 AFIX 0 N2 3 0.379898 0.273339 0.709390 11.00000 0.03306 0.04027 = 0.03088 -0.00250 0.01619 0.00006 N3 3 0.400408 0.352704 0.599973 11.00000 0.02971 0.02780 = 0.03566 -0.00344 0.01082 0.00194 N4 3 0.457066 0.289441 0.496300 11.00000 0.03324 0.03579 = 0.03085 0.00001 0.01544 -0.00029 N5 3 0.485867 0.260790 0.433418 11.00000 0.03624 0.03879 = 0.03305 -0.00104 0.01709 0.00041 AFIX 43 H5 2 0.496295 0.221134 0.433087 11.00000 -1.20000 AFIX 0 N6 3 0.646394 0.307258 0.731384 11.00000 0.03458 0.05392 = 0.03459 -0.00599 0.01208 -0.00921 AFIX 43 H6 2 0.635469 0.346901 0.730832 11.00000 -1.20000 AFIX 0 N7 3 0.572849 0.264965 0.688337 11.00000 0.02953 0.03886 = 0.02954 0.00075 0.01089 0.00057 N8 3 0.455958 0.177652 0.606978 11.00000 0.03987 0.02804 = 0.03368 0.00159 0.01779 0.00358 N9 3 0.288098 0.231249 0.517864 11.00000 0.03034 0.03746 = 0.02943 -0.00065 0.01200 -0.00190 N10 3 0.191692 0.252472 0.470446 11.00000 0.03074 0.05640 = 0.03537 -0.00150 0.01227 0.00382 AFIX 43 H10 2 0.174093 0.291321 0.465152 11.00000 -1.20000 AFIX 0 C1 1 0.249035 0.380451 1.018809 11.00000 0.19064 0.14381 = 0.13708 -0.06866 0.12429 -0.02127 AFIX 137 H1A 2 0.224593 0.420180 0.988552 11.00000 -1.50000 H1B 2 0.309227 0.386592 1.078417 11.00000 -1.50000 H1C 2 0.194580 0.360503 1.031382 11.00000 -1.50000 AFIX 0 C2 1 0.280981 0.279909 0.969547 11.00000 0.06353 0.10191 = 0.05446 -0.01694 0.03721 -0.00986 C3 1 0.258026 0.250905 1.039241 11.00000 0.08217 0.13843 = 0.05819 -0.01691 0.05044 -0.01816 AFIX 43 H3A 2 0.240947 0.274800 1.081762 11.00000 -1.20000 AFIX 0 C4 1 0.260183 0.188247 1.046113 11.00000 0.07423 0.14924 = 0.05523 0.02107 0.04107 -0.00382 AFIX 43 H4A 2 0.244612 0.169307 1.093633 11.00000 -1.20000 AFIX 0 C5 1 0.284645 0.151994 0.985059 11.00000 0.08356 0.10808 = 0.07056 0.02302 0.04484 0.00170 AFIX 43 H5A 2 0.284657 0.108608 0.989407 11.00000 -1.20000 AFIX 0 C6 1 0.309476 0.181243 0.916416 11.00000 0.07785 0.08025 = 0.05826 0.00681 0.04193 0.00352 AFIX 43 H6A 2 0.328086 0.156713 0.875498 11.00000 -1.20000 AFIX 0 C7 1 0.307854 0.244624 0.906099 11.00000 0.04598 0.07864 = 0.04269 -0.00380 0.02490 -0.00491 C8 1 0.331702 0.273347 0.831574 11.00000 0.03827 0.06419 = 0.03732 -0.00910 0.02035 -0.00249 C9 1 0.331077 0.333721 0.803860 11.00000 0.04558 0.05992 = 0.04485 -0.01555 0.02567 -0.00059 AFIX 43 H9A 2 0.314641 0.368894 0.830818 11.00000 -1.20000 AFIX 0 C10 1 0.360031 0.332149 0.726975 11.00000 0.03387 0.04639 = 0.03802 -0.01140 0.01778 -0.00064 C11 1 0.371807 0.378483 0.664635 11.00000 0.03373 0.03675 = 0.04276 -0.00870 0.01432 0.00138 C12 1 0.355962 0.441849 0.664916 11.00000 0.04860 0.04028 = 0.06225 -0.01448 0.02164 0.00529 AFIX 43 H12A 2 0.335798 0.460091 0.710089 11.00000 -1.20000 AFIX 0 C13 1 0.370893 0.477756 0.595979 11.00000 0.05358 0.02949 = 0.07163 -0.00432 0.01775 0.00366 AFIX 43 H13A 2 0.360687 0.520778 0.594883 11.00000 -1.20000 AFIX 0 C14 1 0.400023 0.451331 0.530336 11.00000 0.04643 0.02970 = 0.05839 0.00508 0.01352 -0.00039 AFIX 43 H14A 2 0.408849 0.475503 0.483433 11.00000 -1.20000 AFIX 0 C15 1 0.416325 0.387837 0.534488 11.00000 0.03353 0.02935 = 0.04097 0.00193 0.01002 -0.00194 C16 1 0.448934 0.349402 0.473573 11.00000 0.03352 0.03680 = 0.03334 0.00305 0.01125 -0.00405 C17 1 0.473624 0.358721 0.395137 11.00000 0.03933 0.04315 = 0.03820 0.00797 0.01355 -0.00772 AFIX 43 H17A 2 0.474316 0.396566 0.365291 11.00000 -1.20000 AFIX 0 C18 1 0.496672 0.301079 0.370720 11.00000 0.03606 0.04529 = 0.03615 0.00226 0.01632 -0.00533 C19 1 0.525006 0.280645 0.293127 11.00000 0.04476 0.05801 = 0.03963 -0.00259 0.02243 -0.01010 C20 1 0.549554 0.326719 0.241105 11.00000 0.08223 0.07772 = 0.05114 0.00314 0.04013 -0.01424 AFIX 43 H20A 2 0.548125 0.368625 0.256891 11.00000 -1.20000 AFIX 0 C21 1 0.575992 0.310448 0.166222 11.00000 0.10896 0.10584 = 0.06748 0.00817 0.06138 -0.01153 AFIX 43 H21A 2 0.592949 0.341166 0.131804 11.00000 -1.20000 AFIX 0 C22 1 0.576998 0.248742 0.143167 11.00000 0.10451 0.11760 = 0.06769 -0.01363 0.06438 -0.01160 AFIX 43 H22A 2 0.593375 0.237547 0.091961 11.00000 -1.20000 AFIX 0 C23 1 0.554098 0.203282 0.194827 11.00000 0.08832 0.08926 = 0.07679 -0.02359 0.05585 -0.00893 AFIX 43 H23A 2 0.556200 0.161326 0.179608 11.00000 -1.20000 AFIX 0 C24 1 0.528226 0.219840 0.268622 11.00000 0.05595 0.06397 = 0.05011 -0.00407 0.03216 -0.00172 C25 1 0.500751 0.113004 0.294052 11.00000 0.19074 0.04963 = 0.15109 -0.01759 0.12870 -0.01039 AFIX 137 H25A 2 0.474879 0.087743 0.331620 11.00000 -1.50000 H25B 2 0.569935 0.099437 0.304630 11.00000 -1.50000 H25C 2 0.455200 0.108858 0.226956 11.00000 -1.50000 AFIX 0 C26 1 0.739777 0.279978 0.775738 11.00000 0.03245 0.08606 = 0.03927 0.00443 0.00970 -0.00729 AFIX 43 H26A 2 0.802717 0.300378 0.810820 11.00000 -1.20000 AFIX 0 C27 1 0.727441 0.218541 0.761181 11.00000 0.03069 0.08201 = 0.04009 0.01362 0.01216 0.01299 AFIX 43 H27A 2 0.779023 0.187895 0.783678 11.00000 -1.20000 AFIX 0 C28 1 0.621136 0.209914 0.705235 11.00000 0.03417 0.05041 = 0.03371 0.00938 0.01570 0.01028 C29 1 0.554108 0.158542 0.658139 11.00000 0.04544 0.03614 = 0.04124 0.00764 0.02065 0.01253 C30 1 0.581218 0.097262 0.657547 11.00000 0.07071 0.04119 = 0.06294 0.01316 0.02880 0.02447 AFIX 43 H30A 2 0.649719 0.084040 0.692895 11.00000 -1.20000 AFIX 0 C31 1 0.504949 0.055566 0.603514 11.00000 0.10158 0.02989 = 0.07343 0.00529 0.03882 0.01807 AFIX 43 H31A 2 0.521902 0.013619 0.602259 11.00000 -1.20000 AFIX 0 C32 1 0.404447 0.075208 0.551630 11.00000 0.08503 0.03038 = 0.05684 -0.00341 0.02955 -0.00215 AFIX 43 H32A 2 0.352795 0.047214 0.514421 11.00000 -1.20000 AFIX 0 C33 1 0.381445 0.137574 0.555774 11.00000 0.05597 0.02877 = 0.03460 -0.00079 0.02015 -0.00165 C34 1 0.282369 0.169153 0.508095 11.00000 0.04448 0.04076 = 0.03105 -0.00477 0.01578 -0.01052 C35 1 0.179697 0.151274 0.454366 11.00000 0.05237 0.05959 = 0.04286 -0.01330 0.01784 -0.02297 AFIX 43 H35A 2 0.153881 0.110914 0.437493 11.00000 -1.20000 AFIX 0 C36 1 0.125590 0.205126 0.431984 11.00000 0.03460 0.07961 = 0.03969 -0.01072 0.01031 -0.01242 AFIX 43 H36A 2 0.053816 0.208795 0.395635 11.00000 -1.20000 AFIX 0 C37 1 0.618968 0.081812 0.939557 11.00000 0.05435 0.05228 = 0.06254 0.00063 0.01879 -0.00453 C38 1 0.616124 0.019963 0.896454 11.00000 0.07530 0.05786 = 0.10466 -0.01019 0.03149 -0.00299 AFIX 137 H38A 2 0.666086 0.018731 0.868330 11.00000 -1.50000 H38B 2 0.547241 0.012345 0.847447 11.00000 -1.50000 H38C 2 0.633188 -0.011580 0.945435 11.00000 -1.50000 AFIX 0 C39 1 0.565261 0.088551 1.003536 11.00000 0.11995 0.09598 = 0.10083 -0.00660 0.07134 -0.00208 AFIX 137 H39A 2 0.574297 0.130428 1.028349 11.00000 -1.50000 H39B 2 0.594273 0.059542 1.056045 11.00000 -1.50000 H39C 2 0.491976 0.080105 0.968191 11.00000 -1.50000 AFIX 0 PART -1 O4 4 -0.035106 0.070877 0.451634 10.35000 0.14761 C40 1 -0.014502 0.019797 0.480446 10.35000 0.08350 C41 1 0.034735 -0.020733 0.434047 10.35000 0.12850 AFIX 33 H41A 2 0.047460 -0.061096 0.464301 10.35000 -1.50000 H41B 2 -0.010795 -0.025110 0.366984 10.35000 -1.50000 H41C 2 0.099936 -0.002661 0.440326 10.35000 -1.50000 AFIX 0 C42 1 -0.010023 -0.000938 0.573406 10.35000 0.12690 AFIX 33 H42A 2 0.008276 -0.044451 0.582287 10.35000 -1.50000 H42B 2 0.041773 0.022960 0.624057 10.35000 -1.50000 H42C 2 -0.077174 0.005040 0.575007 10.35000 -1.50000 AFIX 0 PART 1 RESI 1 CLO4 CL1 5 0.696675 0.466404 0.745310 21.00000 0.05354 O1 4 0.613268 0.434389 0.761793 21.00000 0.05921 O2 4 0.787278 0.460721 0.829375 21.00000 0.09663 O3 4 0.665177 0.531329 0.732993 21.00000 0.09664 O4 4 0.702021 0.445160 0.662326 21.00000 0.13422 PART 2 RESI 2 CLO4 CL1 5 0.691723 0.474730 0.766148 -21.00000 0.04513 O1 4 0.607676 0.432613 0.733324 -21.00000 0.08162 O2 4 0.721310 0.499589 0.857483 -21.00000 0.11797 O3 4 0.683903 0.519637 0.696406 -21.00000 0.10470 O4 4 0.783548 0.436487 0.780996 -21.00000 0.10558 PART 1 RESI 3 CLO4 CL1 5 0.305207 0.050846 0.732748 31.00000 0.05339 O1 4 0.256534 0.058910 0.797866 31.00000 0.10487 O2 4 0.367794 -0.002847 0.762729 31.00000 0.10684 O3 4 0.233212 0.050963 0.637948 31.00000 0.12950 O4 4 0.367448 0.104808 0.744136 31.00000 0.06145 PART 2 RESI 4 CLO4 CL1 5 0.322102 0.052162 0.755274 -31.00000 0.06018 O1 4 0.325074 0.037838 0.846385 -31.00000 0.10661 O2 4 0.350432 0.000120 0.714207 -31.00000 0.10832 O3 4 0.217453 0.067626 0.696150 -31.00000 0.14327 O4 4 0.393752 0.101440 0.766628 -31.00000 0.05791 PART 0 HKLF 4 REM tmajor in P2(1)/n REM R1 = 0.0767 for 10342 Fo > 4sig(Fo) and 0.0902 for all 13023 data REM 580 parameters refined using 403 restraints END WGHT 0.1307 3.4646 REM Instructions for potential hydrogen bonds HTAB N1 O4_3 HTAB N1 O4_4 HTAB N5 O2 HTAB N6 Cl1_1 HTAB N6 O1_1 HTAB N6 Cl1_2 HTAB N6 O1_2 HTAB N10 O3_$1 HTAB C9 O1 EQIV $2 x+1/2, -y+1/2, z+1/2 HTAB C9 O4_$2 EQIV $3 -x+1/2, y+1/2, -z+3/2 HTAB_3 C12_0 O1_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB_2 C14_0 O3_$4 HTAB_1 C17_0 O3_$4 HTAB_2 C25_0 O4_$1 EQIV $5 -x+1, -y, -z+1 HTAB_3 C25_0 O2_$5 HTAB_4 C25_0 O2_$5 EQIV $6 -x+3/2, y-1/2, -z+3/2 HTAB_1 C30_0 O3_$6 HTAB_1 C32_0 O2_$1 HTAB_2 C32_0 O2_$1 HTAB_1 C38_0 O4_$6 HTAB C38 O2_3 EQIV $7 -x+1, -y, -z+2 HTAB_4 C39_0 O1_$7 HTAB C39 O1_4 REM Highest difference peak 1.215, deepest hole -1.414, 1-sigma level 0.091 Q1 1 0.2122 0.0627 0.7481 11.00000 0.05 1.21 Q2 1 0.7619 0.4819 0.8515 11.00000 0.05 0.97 Q3 1 0.2906 0.0111 0.6474 11.00000 0.05 0.86 Q4 1 0.3596 0.0077 0.8199 11.00000 0.05 0.83 Q5 1 0.7504 0.4361 0.7235 11.00000 0.05 0.67 Q6 1 0.6954 0.4578 0.7101 11.00000 0.05 0.66 Q7 1 0.6643 0.5383 0.7821 11.00000 0.05 0.62 Q8 1 0.6180 0.4401 0.6804 11.00000 0.05 0.61 Q9 1 0.6713 0.4799 0.6631 11.00000 0.05 0.52 Q10 1 0.4013 0.2661 0.5505 11.00000 0.05 0.51 Q11 1 0.5331 0.0801 0.6315 11.00000 0.05 0.48 Q12 1 -0.0129 0.0323 0.5144 11.00000 0.05 0.48 Q13 1 0.7996 0.4629 0.7939 11.00000 0.05 0.46 Q14 1 0.3234 0.1096 0.7080 11.00000 0.05 0.44 Q15 1 0.7910 0.4214 0.8165 11.00000 0.05 0.43 Q16 1 0.4084 0.0797 0.7522 11.00000 0.05 0.42 Q17 1 0.4370 0.3709 0.4967 11.00000 0.05 0.39 Q18 1 0.6360 0.1435 1.0109 11.00000 0.05 0.38 Q19 1 -0.0986 0.0513 0.4474 11.00000 0.05 0.38 Q20 1 0.6325 0.5202 0.6931 11.00000 0.05 0.37 ; _shelx_res_checksum 53514 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.42461(2) 0.26480(2) 0.60308(2) 0.02564(11) Uani 1 1 d . . . . . O1 O 0.2767(3) 0.34204(19) 0.9567(3) 0.0954(12) Uani 1 1 d . . . . . O2 O 0.5041(3) 0.17642(12) 0.3220(2) 0.0670(7) Uani 1 1 d . . . . . O3 O 0.6623(3) 0.12396(15) 0.9215(3) 0.0771(9) Uani 1 1 d D . . . . N1 N 0.36235(19) 0.23793(12) 0.77260(17) 0.0392(5) Uani 1 1 d . . . . . H1 H 0.3693 0.1979 0.7762 0.047 Uiso 1 1 calc R U . . . N2 N 0.37990(17) 0.27334(11) 0.70939(15) 0.0337(4) Uani 1 1 d . . . . . N3 N 0.40041(16) 0.35270(10) 0.59997(15) 0.0319(4) Uani 1 1 d . . . . . N4 N 0.45707(16) 0.28944(10) 0.49630(15) 0.0326(4) Uani 1 1 d . . . . . N5 N 0.48587(18) 0.26079(11) 0.43342(16) 0.0351(4) Uani 1 1 d . . . . . H5 H 0.4963 0.2211 0.4331 0.042 Uiso 1 1 calc R U . . . N6 N 0.64639(18) 0.30726(13) 0.73138(17) 0.0417(5) Uani 1 1 d . . . . . H6 H 0.6355 0.3469 0.7308 0.050 Uiso 1 1 calc R U . . . N7 N 0.57285(17) 0.26497(10) 0.68834(15) 0.0331(4) Uani 1 1 d . . . . . N8 N 0.45596(18) 0.17765(10) 0.60698(15) 0.0330(4) Uani 1 1 d . . . . . N9 N 0.28810(17) 0.23125(10) 0.51786(15) 0.0325(4) Uani 1 1 d . . . . . N10 N 0.19169(18) 0.25247(14) 0.47045(17) 0.0413(5) Uani 1 1 d . . . . . H10 H 0.1741 0.2913 0.4652 0.050 Uiso 1 1 calc R U . . . C1 C 0.2490(7) 0.3805(4) 1.0188(6) 0.138(3) Uani 1 1 d . . . . . H1A H 0.2246 0.4202 0.9886 0.208 Uiso 1 1 calc R U . . . H1B H 0.3092 0.3866 1.0784 0.208 Uiso 1 1 calc R U . . . H1C H 0.1946 0.3605 1.0314 0.208 Uiso 1 1 calc R U . . . C2 C 0.2810(3) 0.2799(3) 0.9695(3) 0.0690(11) Uani 1 1 d . . . . . C3 C 0.2580(4) 0.2509(3) 1.0392(3) 0.0858(16) Uani 1 1 d . . . . . H3A H 0.2409 0.2748 1.0818 0.103 Uiso 1 1 calc R U . . . C4 C 0.2602(4) 0.1882(3) 1.0461(3) 0.0881(17) Uani 1 1 d . . . . . H4A H 0.2446 0.1693 1.0936 0.106 Uiso 1 1 calc R U . . . C5 C 0.2846(4) 0.1520(3) 0.9851(4) 0.0831(14) Uani 1 1 d . . . . . H5A H 0.2847 0.1086 0.9894 0.100 Uiso 1 1 calc R U . . . C6 C 0.3095(4) 0.1812(2) 0.9164(3) 0.0675(10) Uani 1 1 d . . . . . H6A H 0.3281 0.1567 0.8755 0.081 Uiso 1 1 calc R U . . . C7 C 0.3079(3) 0.2446(2) 0.9061(2) 0.0536(8) Uani 1 1 d . . . . . C8 C 0.3317(2) 0.27335(16) 0.8316(2) 0.0450(7) Uani 1 1 d . . . . . C9 C 0.3311(2) 0.33372(17) 0.8039(2) 0.0478(7) Uani 1 1 d . . . . . H9A H 0.3146 0.3689 0.8308 0.057 Uiso 1 1 calc R U . . . C10 C 0.3600(2) 0.33215(14) 0.7270(2) 0.0384(5) Uani 1 1 d . . . . . C11 C 0.3718(2) 0.37848(13) 0.6646(2) 0.0382(5) Uani 1 1 d . . . . . C12 C 0.3560(3) 0.44185(15) 0.6649(3) 0.0508(7) Uani 1 1 d . . . . . H12A H 0.3358 0.4601 0.7101 0.061 Uiso 1 1 calc R U . . . C13 C 0.3709(3) 0.47776(14) 0.5960(3) 0.0542(8) Uani 1 1 d . . . . . H13A H 0.3607 0.5208 0.5949 0.065 Uiso 1 1 calc R U . . . C14 C 0.4000(2) 0.45133(13) 0.5303(3) 0.0475(7) Uani 1 1 d . . . . . H14A H 0.4088 0.4755 0.4834 0.057 Uiso 1 1 calc R U . . . C15 C 0.4163(2) 0.38784(12) 0.5345(2) 0.0364(5) Uani 1 1 d . . . . . C16 C 0.4489(2) 0.34940(12) 0.47357(18) 0.0354(5) Uani 1 1 d . . . . . C17 C 0.4736(2) 0.35872(14) 0.3951(2) 0.0410(6) Uani 1 1 d . . . . . H17A H 0.4743 0.3966 0.3653 0.049 Uiso 1 1 calc R U . . . C18 C 0.4967(2) 0.30108(14) 0.37072(19) 0.0387(5) Uani 1 1 d . . . . . C19 C 0.5250(2) 0.28064(17) 0.2931(2) 0.0458(6) Uani 1 1 d . . . . . C20 C 0.5496(4) 0.3267(2) 0.2411(3) 0.0662(10) Uani 1 1 d . . . . . H20A H 0.5481 0.3686 0.2569 0.079 Uiso 1 1 calc R U . . . C21 C 0.5760(5) 0.3104(3) 0.1662(3) 0.0858(15) Uani 1 1 d . . . . . H21A H 0.5929 0.3412 0.1318 0.103 Uiso 1 1 calc R U . . . C22 C 0.5770(5) 0.2487(3) 0.1432(4) 0.0870(15) Uani 1 1 d . . . . . H22A H 0.5934 0.2375 0.0920 0.104 Uiso 1 1 calc R U . . . C23 C 0.5541(4) 0.2033(3) 0.1948(3) 0.0776(13) Uani 1 1 d . . . . . H23A H 0.5562 0.1613 0.1796 0.093 Uiso 1 1 calc R U . . . C24 C 0.5282(3) 0.21984(19) 0.2686(3) 0.0533(8) Uani 1 1 d . . . . . C25 C 0.5008(6) 0.1130(2) 0.2941(5) 0.111(2) Uani 1 1 d . . . . . H25A H 0.4749 0.0877 0.3316 0.167 Uiso 1 1 calc R U . . . H25B H 0.5699 0.0994 0.3046 0.167 Uiso 1 1 calc R U . . . H25C H 0.4552 0.1089 0.2270 0.167 Uiso 1 1 calc R U . . . C26 C 0.7398(2) 0.2800(2) 0.7757(2) 0.0543(8) Uani 1 1 d . . . . . H26A H 0.8027 0.3004 0.8108 0.065 Uiso 1 1 calc R U . . . C27 C 0.7274(2) 0.2185(2) 0.7612(2) 0.0517(8) Uani 1 1 d . . . . . H27A H 0.7790 0.1879 0.7837 0.062 Uiso 1 1 calc R U . . . C28 C 0.6211(2) 0.20991(15) 0.70524(19) 0.0389(6) Uani 1 1 d . . . . . C29 C 0.5541(2) 0.15854(13) 0.6581(2) 0.0400(6) Uani 1 1 d . . . . . C30 C 0.5812(3) 0.09726(16) 0.6575(3) 0.0579(9) Uani 1 1 d . . . . . H30A H 0.6497 0.0840 0.6929 0.069 Uiso 1 1 calc R U . . . C31 C 0.5049(4) 0.05557(15) 0.6035(3) 0.0674(11) Uani 1 1 d . . . . . H31A H 0.5219 0.0136 0.6023 0.081 Uiso 1 1 calc R U . . . C32 C 0.4044(3) 0.07521(15) 0.5516(3) 0.0573(9) Uani 1 1 d . . . . . H32A H 0.3528 0.0472 0.5144 0.069 Uiso 1 1 calc R U . . . C33 C 0.3814(2) 0.13757(12) 0.55577(19) 0.0393(6) Uani 1 1 d . . . . . C34 C 0.2824(2) 0.16915(13) 0.50810(18) 0.0387(5) Uani 1 1 d . . . . . C35 C 0.1797(3) 0.15127(18) 0.4544(2) 0.0522(8) Uani 1 1 d . . . . . H35A H 0.1539 0.1109 0.4375 0.063 Uiso 1 1 calc R U . . . C36 C 0.1256(2) 0.2051(2) 0.4320(2) 0.0530(8) Uani 1 1 d . . . . . H36A H 0.0538 0.2088 0.3956 0.064 Uiso 1 1 calc R U . . . C37 C 0.6190(3) 0.08181(17) 0.9396(3) 0.0581(8) Uani 1 1 d D . . . . C38 C 0.6161(4) 0.0200(2) 0.8965(4) 0.0811(13) Uani 1 1 d D . . . . H38A H 0.6661 0.0187 0.8683 0.122 Uiso 1 1 calc R U . . . H38B H 0.5472 0.0123 0.8474 0.122 Uiso 1 1 calc R U . . . H38C H 0.6332 -0.0116 0.9454 0.122 Uiso 1 1 calc R U . . . C39 C 0.5653(5) 0.0886(3) 1.0035(4) 0.0970(17) Uani 1 1 d D . . . . H39A H 0.5743 0.1304 1.0283 0.146 Uiso 1 1 calc R U . . . H39B H 0.5943 0.0595 1.0560 0.146 Uiso 1 1 calc R U . . . H39C H 0.4920 0.0801 0.9682 0.146 Uiso 1 1 calc R U . . . O4 O -0.0351(14) 0.0709(7) 0.4516(12) 0.148(6) Uiso 0.35 1 d D . P A -1 C40 C -0.0145(13) 0.0198(7) 0.4804(10) 0.084(4) Uiso 0.35 1 d D . P A -1 C41 C 0.035(2) -0.0207(12) 0.4340(18) 0.129(10) Uiso 0.35 1 d D . P A -1 H41A H 0.0475 -0.0611 0.4643 0.193 Uiso 0.35 1 calc R U P A -1 H41B H -0.0108 -0.0251 0.3670 0.193 Uiso 0.35 1 calc R U P A -1 H41C H 0.0999 -0.0027 0.4403 0.193 Uiso 0.35 1 calc R U P A -1 C42 C -0.010(2) -0.0009(15) 0.5734(14) 0.127(8) Uiso 0.35 1 d D . P A -1 H42A H 0.0083 -0.0445 0.5823 0.190 Uiso 0.35 1 calc R U P A -1 H42B H 0.0418 0.0230 0.6241 0.190 Uiso 0.35 1 calc R U P A -1 H42C H -0.0772 0.0050 0.5750 0.190 Uiso 0.35 1 calc R U P A -1 Cl1_1 Cl 0.69667(15) 0.4664(2) 0.7453(2) 0.0535(5) Uiso 0.532(6) 1 d D . P B 1 O1_1 O 0.6133(4) 0.4344(3) 0.7618(5) 0.0592(16) Uiso 0.532(6) 1 d D . P B 1 O2_1 O 0.7873(5) 0.4607(4) 0.8294(5) 0.097(2) Uiso 0.532(6) 1 d D . P B 1 O3_1 O 0.6652(6) 0.5313(3) 0.7330(6) 0.097(2) Uiso 0.532(6) 1 d D . P B 1 O4_1 O 0.7020(8) 0.4452(4) 0.6623(5) 0.134(4) Uiso 0.532(6) 1 d D . P B 1 Cl1_2 Cl 0.69172(15) 0.4747(2) 0.7661(2) 0.0451(5) Uiso 0.468(6) 1 d D . P B 2 O1_2 O 0.6077(5) 0.4326(4) 0.7333(6) 0.082(3) Uiso 0.468(6) 1 d D . P B 2 O2_2 O 0.7213(7) 0.4996(4) 0.8575(5) 0.118(3) Uiso 0.468(6) 1 d D . P B 2 O3_2 O 0.6839(7) 0.5196(4) 0.6964(6) 0.105(3) Uiso 0.468(6) 1 d D . P B 2 O4_2 O 0.7835(6) 0.4365(4) 0.7810(7) 0.106(3) Uiso 0.468(6) 1 d D . P B 2 Cl1_3 Cl 0.3052(2) 0.05085(11) 0.7327(2) 0.0534(6) Uiso 0.502(9) 1 d D . P C 1 O1_3 O 0.2565(7) 0.0589(4) 0.7979(6) 0.105(3) Uiso 0.502(9) 1 d D . P C 1 O2_3 O 0.3678(6) -0.0028(3) 0.7627(7) 0.107(3) Uiso 0.502(9) 1 d D . P C 1 O3_3 O 0.2332(7) 0.0510(5) 0.6379(5) 0.130(4) Uiso 0.502(9) 1 d D . P C 1 O4_3 O 0.3674(5) 0.1048(3) 0.7441(5) 0.0615(18) Uiso 0.502(9) 1 d D . P C 1 Cl1_4 Cl 0.3221(3) 0.05216(12) 0.7553(3) 0.0602(7) Uiso 0.498(9) 1 d D . P C 2 O1_4 O 0.3251(8) 0.0378(4) 0.8464(5) 0.107(3) Uiso 0.498(9) 1 d D . P C 2 O2_4 O 0.3504(7) 0.0001(4) 0.7142(7) 0.108(3) Uiso 0.498(9) 1 d D . P C 2 O3_4 O 0.2175(5) 0.0676(5) 0.6961(8) 0.143(5) Uiso 0.498(9) 1 d D . P C 2 O4_4 O 0.3938(5) 0.1014(3) 0.7666(5) 0.0579(17) Uiso 0.498(9) 1 d D . P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02641(17) 0.02517(17) 0.02610(18) -0.00073(11) 0.01161(13) 0.00150(11) O1 0.133(3) 0.097(3) 0.097(3) -0.031(2) 0.088(3) -0.012(2) O2 0.097(2) 0.0465(13) 0.0851(19) -0.0100(13) 0.0650(18) -0.0067(13) O3 0.0769(19) 0.0633(17) 0.090(2) -0.0025(16) 0.0339(17) -0.0196(15) N1 0.0396(11) 0.0484(13) 0.0330(11) 0.0016(9) 0.0183(9) -0.0021(9) N2 0.0331(10) 0.0403(11) 0.0309(10) -0.0025(8) 0.0162(8) 0.0001(8) N3 0.0297(9) 0.0278(9) 0.0357(10) -0.0034(7) 0.0108(8) 0.0019(7) N4 0.0332(9) 0.0358(10) 0.0309(9) 0.0000(8) 0.0154(8) -0.0003(8) N5 0.0362(10) 0.0388(11) 0.0330(10) -0.0010(8) 0.0171(9) 0.0004(8) N6 0.0346(10) 0.0539(14) 0.0346(11) -0.0060(10) 0.0121(9) -0.0092(10) N7 0.0295(9) 0.0389(11) 0.0295(9) 0.0007(8) 0.0109(8) 0.0006(8) N8 0.0399(10) 0.0280(9) 0.0337(10) 0.0016(8) 0.0178(8) 0.0036(8) N9 0.0303(9) 0.0375(11) 0.0294(9) -0.0006(8) 0.0120(8) -0.0019(8) N10 0.0307(10) 0.0564(14) 0.0354(11) -0.0015(10) 0.0123(9) 0.0038(10) C1 0.191(8) 0.144(6) 0.137(6) -0.069(5) 0.124(6) -0.021(6) C2 0.064(2) 0.102(3) 0.054(2) -0.017(2) 0.0372(18) -0.010(2) C3 0.082(3) 0.138(5) 0.058(2) -0.017(3) 0.050(2) -0.018(3) C4 0.074(3) 0.149(5) 0.055(2) 0.021(3) 0.041(2) -0.004(3) C5 0.084(3) 0.108(4) 0.071(3) 0.023(3) 0.045(2) 0.002(3) C6 0.078(3) 0.080(3) 0.058(2) 0.0068(19) 0.042(2) 0.004(2) C7 0.0460(16) 0.079(2) 0.0427(16) -0.0038(15) 0.0249(14) -0.0049(16) C8 0.0383(13) 0.0642(19) 0.0373(13) -0.0091(12) 0.0203(11) -0.0025(12) C9 0.0456(15) 0.0599(18) 0.0449(15) -0.0156(13) 0.0257(13) -0.0006(13) C10 0.0339(11) 0.0464(14) 0.0380(12) -0.0114(11) 0.0178(10) -0.0006(10) C11 0.0337(11) 0.0368(12) 0.0428(13) -0.0087(10) 0.0143(10) 0.0014(10) C12 0.0486(15) 0.0403(15) 0.0623(19) -0.0145(13) 0.0216(14) 0.0053(12) C13 0.0536(17) 0.0295(13) 0.072(2) -0.0043(13) 0.0178(16) 0.0037(12) C14 0.0464(15) 0.0297(12) 0.0584(18) 0.0051(12) 0.0135(13) -0.0004(11) C15 0.0335(11) 0.0294(11) 0.0410(13) 0.0019(9) 0.0100(10) -0.0019(9) C16 0.0335(11) 0.0368(12) 0.0333(11) 0.0031(9) 0.0113(9) -0.0041(9) C17 0.0393(13) 0.0431(14) 0.0382(13) 0.0080(11) 0.0135(11) -0.0077(11) C18 0.0361(12) 0.0453(14) 0.0362(12) 0.0023(10) 0.0163(10) -0.0053(10) C19 0.0448(14) 0.0580(17) 0.0396(14) -0.0026(12) 0.0224(12) -0.0101(13) C20 0.082(3) 0.078(3) 0.0511(19) 0.0031(18) 0.0401(19) -0.014(2) C21 0.109(4) 0.106(4) 0.067(3) 0.008(3) 0.061(3) -0.012(3) C22 0.105(4) 0.118(4) 0.068(3) -0.014(3) 0.064(3) -0.012(3) C23 0.088(3) 0.089(3) 0.077(3) -0.024(2) 0.056(3) -0.009(3) C24 0.0559(18) 0.064(2) 0.0501(17) -0.0041(15) 0.0322(15) -0.0017(16) C25 0.191(7) 0.050(2) 0.151(6) -0.018(3) 0.129(6) -0.010(3) C26 0.0325(13) 0.086(3) 0.0393(15) 0.0044(15) 0.0097(11) -0.0073(15) C27 0.0307(12) 0.082(2) 0.0401(14) 0.0136(15) 0.0122(11) 0.0130(14) C28 0.0342(11) 0.0504(15) 0.0337(12) 0.0094(11) 0.0157(10) 0.0103(11) C29 0.0454(14) 0.0361(13) 0.0412(13) 0.0076(10) 0.0207(11) 0.0125(11) C30 0.071(2) 0.0412(16) 0.063(2) 0.0132(14) 0.0288(18) 0.0245(15) C31 0.102(3) 0.0299(14) 0.073(2) 0.0053(15) 0.039(2) 0.0181(17) C32 0.085(3) 0.0304(13) 0.0568(19) -0.0034(13) 0.0296(18) -0.0021(14) C33 0.0560(15) 0.0288(11) 0.0346(12) -0.0008(9) 0.0201(12) -0.0016(10) C34 0.0445(13) 0.0408(13) 0.0310(11) -0.0048(10) 0.0158(10) -0.0105(11) C35 0.0524(17) 0.0596(19) 0.0429(15) -0.0133(14) 0.0178(13) -0.0230(15) C36 0.0346(13) 0.080(2) 0.0397(15) -0.0107(15) 0.0103(12) -0.0124(14) C37 0.0543(18) 0.0523(19) 0.063(2) 0.0006(16) 0.0188(16) -0.0045(15) C38 0.075(3) 0.058(2) 0.105(4) -0.010(2) 0.031(3) -0.003(2) C39 0.120(5) 0.096(4) 0.101(4) -0.007(3) 0.071(4) -0.002(3) 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 N3 Fe1 N8 177.09(9) N3 Fe1 N4 79.14(9) N8 Fe1 N4 99.28(9) N3 Fe1 N7 98.34(9) N8 Fe1 N7 79.18(9) N4 Fe1 N7 90.23(9) N3 Fe1 N9 103.31(9) N8 Fe1 N9 79.15(9) N4 Fe1 N9 92.69(9) N7 Fe1 N9 158.32(9) N3 Fe1 N2 79.37(10) N8 Fe1 N2 102.23(9) N4 Fe1 N2 158.49(10) N7 Fe1 N2 93.75(9) N9 Fe1 N2 91.36(9) C2 O1 C1 118.9(5) C24 O2 C25 117.2(3) N2 N1 C8 111.2(3) N2 N1 H1 124.4 C8 N1 H1 124.4 N1 N2 C10 106.0(2) N1 N2 Fe1 139.55(19) C10 N2 Fe1 114.46(19) C11 N3 C15 120.9(2) C11 N3 Fe1 119.76(19) C15 N3 Fe1 119.29(18) C16 N4 N5 106.1(2) C16 N4 Fe1 117.40(18) N5 N4 Fe1 136.49(18) N4 N5 C18 111.9(2) N4 N5 H5 124.1 C18 N5 H5 124.1 N7 N6 C26 110.7(3) N7 N6 H6 124.7 C26 N6 H6 124.7 N6 N7 C28 106.2(2) N6 N7 Fe1 137.01(19) C28 N7 Fe1 116.51(19) C33 N8 C29 121.1(2) C33 N8 Fe1 119.78(19) C29 N8 Fe1 119.03(19) N10 N9 C34 106.2(2) N10 N9 Fe1 137.52(19) C34 N9 Fe1 115.92(18) N9 N10 C36 110.3(3) N9 N10 H10 124.8 C36 N10 H10 124.8 O1 C1 H1A 109.5 O1 C1 H1B 109.5 H1A C1 H1B 109.5 O1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 O1 C2 C3 123.3(4) O1 C2 C7 116.3(4) C3 C2 C7 120.4(5) C4 C3 C2 120.3(5) C4 C3 H3A 119.9 C2 C3 H3A 119.9 C3 C4 C5 121.3(4) C3 C4 H4A 119.3 C5 C4 H4A 119.3 C4 C5 C6 118.2(5) C4 C5 H5A 120.9 C6 C5 H5A 120.9 C7 C6 C5 122.7(4) C7 C6 H6A 118.6 C5 C6 H6A 118.6 C6 C7 C2 117.0(4) C6 C7 C8 121.0(3) C2 C7 C8 122.0(4) C9 C8 N1 106.6(3) C9 C8 C7 132.4(3) N1 C8 C7 121.0(3) C8 C9 C10 105.8(3) C8 C9 H9A 127.1 C10 C9 H9A 127.1 N2 C10 C9 110.4(3) N2 C10 C11 115.4(2) C9 C10 C11 134.2(3) N3 C11 C12 120.7(3) N3 C11 C10 111.0(2) C12 C11 C10 128.3(3) C11 C12 C13 118.0(3) C11 C12 H12A 121.0 C13 C12 H12A 121.0 C14 C13 C12 121.0(3) C14 C13 H13A 119.5 C12 C13 H13A 119.5 C13 C14 C15 118.4(3) C13 C14 H14A 120.8 C15 C14 H14A 120.8 N3 C15 C14 120.9(3) N3 C15 C16 110.6(2) C14 C15 C16 128.5(3) N4 C16 C17 109.9(3) N4 C16 C15 113.5(2) C17 C16 C15 136.6(3) C18 C17 C16 106.0(2) C18 C17 H17A 127.0 C16 C17 H17A 127.0 N5 C18 C17 106.1(2) N5 C18 C19 122.2(3) C17 C18 C19 131.7(3) C24 C19 C20 118.5(3) C24 C19 C18 124.0(3) C20 C19 C18 117.5(3) C21 C20 C19 120.3(4) C21 C20 H20A 119.9 C19 C20 H20A 119.9 C22 C21 C20 119.3(4) C22 C21 H21A 120.3 C20 C21 H21A 120.3 C21 C22 C23 120.5(4) C21 C22 H22A 119.7 C23 C22 H22A 119.7 C24 C23 C22 119.6(5) C24 C23 H23A 120.2 C22 C23 H23A 120.2 C19 C24 C23 121.7(4) C19 C24 O2 116.3(3) C23 C24 O2 122.0(4) 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 C27 C26 N6 108.3(3) C27 C26 H26A 125.8 N6 C26 H26A 125.8 C26 C27 C28 105.4(3) C26 C27 H27A 127.3 C28 C27 H27A 127.3 N7 C28 C27 109.4(3) N7 C28 C29 114.0(2) C27 C28 C29 136.5(3) N8 C29 C30 120.8(3) N8 C29 C28 111.3(2) C30 C29 C28 127.8(3) C29 C30 C31 118.5(3) C29 C30 H30A 120.8 C31 C30 H30A 120.8 C32 C31 C30 120.6(3) C32 C31 H31A 119.7 C30 C31 H31A 119.7 C31 C32 C33 118.4(3) C31 C32 H32A 120.8 C33 C32 H32A 120.8 N8 C33 C32 120.6(3) N8 C33 C34 110.8(2) C32 C33 C34 128.6(3) N9 C34 C35 109.9(3) N9 C34 C33 114.1(2) C35 C34 C33 136.0(3) C36 C35 C34 104.7(3) C36 C35 H35A 127.7 C34 C35 H35A 127.7 N10 C36 C35 108.8(3) N10 C36 H36A 125.6 C35 C36 H36A 125.6 O3 C37 C39 122.3(4) O3 C37 C38 120.3(4) C39 C37 C38 117.3(4) C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C37 C39 H39A 109.5 C37 C39 H39B 109.5 H39A C39 H39B 109.5 C37 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 O4 C40 C41 117.8(17) O4 C40 C42 124(2) C41 C40 C42 116.7(17) C40 C41 H41A 109.5 C40 C41 H41B 109.5 H41A C41 H41B 109.5 C40 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C40 C42 H42A 109.5 C40 C42 H42B 109.5 H42A C42 H42B 109.5 C40 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 O4_1 Cl1_1 O2_1 116.3(5) O4_1 Cl1_1 O3_1 109.1(5) O2_1 Cl1_1 O3_1 108.6(5) O4_1 Cl1_1 O1_1 110.7(5) O2_1 Cl1_1 O1_1 107.0(4) O3_1 Cl1_1 O1_1 104.4(4) O2_2 Cl1_2 O1_2 117.7(6) O2_2 Cl1_2 O3_2 113.3(6) O1_2 Cl1_2 O3_2 112.2(5) O2_2 Cl1_2 O4_2 100.3(5) O1_2 Cl1_2 O4_2 104.6(5) O3_2 Cl1_2 O4_2 106.8(5) O3_3 Cl1_3 O2_3 115.6(6) O3_3 Cl1_3 O4_3 106.0(5) O2_3 Cl1_3 O4_3 110.9(5) O3_3 Cl1_3 O1_3 112.0(5) O2_3 Cl1_3 O1_3 106.7(5) O4_3 Cl1_3 O1_3 105.3(4) O1_4 Cl1_4 O3_4 106.4(6) O1_4 Cl1_4 O2_4 111.5(5) O3_4 Cl1_4 O2_4 108.1(6) O1_4 Cl1_4 O4_4 108.1(5) O3_4 Cl1_4 O4_4 113.7(5) O2_4 Cl1_4 O4_4 109.0(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3 1.927(2) Fe1 N8 1.930(2) Fe1 N4 1.954(2) Fe1 N7 1.964(2) Fe1 N9 1.973(2) Fe1 N2 1.991(2) O1 C2 1.355(6) O1 C1 1.437(6) O2 C24 1.380(4) O2 C25 1.432(5) O3 C37 1.193(5) N1 N2 1.339(3) N1 C8 1.386(4) N1 H1 0.8700 N2 C10 1.353(4) N3 C11 1.340(3) N3 C15 1.353(3) N4 C16 1.335(3) N4 N5 1.346(3) N5 C18 1.354(3) N5 H5 0.8700 N6 N7 1.338(3) N6 C26 1.348(4) N6 H6 0.8700 N7 C28 1.343(4) N8 C33 1.341(4) N8 C29 1.349(3) N9 N10 1.336(3) N9 C34 1.349(4) N10 C36 1.348(4) N10 H10 0.8700 C1 H1A 0.9700 C1 H1B 0.9700 C1 H1C 0.9700 C2 C3 1.391(6) C2 C7 1.409(5) C3 C4 1.358(8) C3 H3A 0.9400 C4 C5 1.373(8) C4 H4A 0.9400 C5 C6 1.395(6) C5 H5A 0.9400 C6 C7 1.378(6) C6 H6A 0.9400 C7 C8 1.461(5) C8 C9 1.372(5) C9 C10 1.403(4) C9 H9A 0.9400 C10 C11 1.443(4) C11 C12 1.388(4) C12 C13 1.399(5) C12 H12A 0.9400 C13 C14 1.364(5) C13 H13A 0.9400 C14 C15 1.389(4) C14 H14A 0.9400 C15 C16 1.462(4) C16 C17 1.402(4) C17 C18 1.379(4) C17 H17A 0.9400 C18 C19 1.475(4) C19 C24 1.373(5) C19 C20 1.408(5) C20 C21 1.395(6) C20 H20A 0.9400 C21 C22 1.382(8) C21 H21A 0.9400 C22 C23 1.384(7) C22 H22A 0.9400 C23 C24 1.376(5) C23 H23A 0.9400 C25 H25A 0.9700 C25 H25B 0.9700 C25 H25C 0.9700 C26 C27 1.346(6) C26 H26A 0.9400 C27 C28 1.405(4) C27 H27A 0.9400 C28 C29 1.446(4) C29 C30 1.380(4) C30 C31 1.389(6) C30 H30A 0.9400 C31 C32 1.381(6) C31 H31A 0.9400 C32 C33 1.394(4) C32 H32A 0.9400 C33 C34 1.457(4) C34 C35 1.399(4) C35 C36 1.357(6) C35 H35A 0.9400 C36 H36A 0.9400 C37 C39 1.478(5) C37 C38 1.485(5) C38 H38A 0.9700 C38 H38B 0.9700 C38 H38C 0.9700 C39 H39A 0.9700 C39 H39B 0.9700 C39 H39C 0.9700 O4 C40 1.181(10) C40 C41 1.474(9) C40 C42 1.475(9) C41 H41A 0.9700 C41 H41B 0.9700 C41 H41C 0.9700 C42 H42A 0.9700 C42 H42B 0.9700 C42 H42C 0.9700 Cl1_1 O4_1 1.388(6) Cl1_1 O2_1 1.402(5) Cl1_1 O3_1 1.461(5) Cl1_1 O1_1 1.478(5) Cl1_2 O2_2 1.398(6) Cl1_2 O1_2 1.416(5) Cl1_2 O3_2 1.417(6) Cl1_2 O4_2 1.477(6) Cl1_3 O3_3 1.393(6) Cl1_3 O2_3 1.417(6) Cl1_3 O4_3 1.428(5) Cl1_3 O1_3 1.442(6) Cl1_4 O1_4 1.419(6) Cl1_4 O3_4 1.423(6) Cl1_4 O2_4 1.426(6) Cl1_4 O4_4 1.431(5) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O4_4 0.87 2.13 2.990(6) 170.8 . N1 H1 O4_3 0.87 2.07 2.915(6) 164.1 . N5 H5 O2 0.87 2.01 2.587(3) 123.3 . N6 H6 O1_2 0.87 1.90 2.767(9) 177.1 . N6 H6 O1_1 0.87 2.01 2.858(7) 166.0 . N6 H6 Cl1_1 0.87 2.70 3.501(4) 152.9 . N6 H6 Cl1_2 0.87 2.86 3.676(4) 156.0 . N10 H10 O3 0.87 1.93 2.759(4) 157.9 4_565