#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:25:44 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173540 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541902.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_1541902 loop_ _publ_author_name 'Aromi, Guillem' 'Beavers, Christine' 'Costa, Jos\'e S\'anchez' 'Craig, Gavin A.' 'Minguez Espallargas, Guillermo' 'Orera, Alodia' 'Roubeau, Olivier' _publ_section_title ; Snapshots of a Solid-State Transformation: Coexistence of Three Phases Trapped in One Crystal. ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C5SC04287A _journal_year 2016 _chemical_formula_moiety 'C36 H30 N10 Fe, C3 H6 O, (Cl O4)2' _chemical_formula_sum 'C39 H36 Cl2 Fe N10 O11' _chemical_formula_weight 947.53 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -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 71.801(5) _cell_angle_beta 69.822(4) _cell_angle_gamma 70.752(4) _cell_formula_units_Z 2 _cell_length_a 13.0297(8) _cell_length_b 13.2995(9) _cell_length_c 14.0177(9) _cell_measurement_reflns_used 4773 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 25.38 _cell_measurement_theta_min 2.26 _cell_volume 2097.8(2) _computing_cell_refinement 'SAINT V8.27B(Bruker, 2012)' _computing_data_collection 'Apex2 v2012.10-0 (Bruker, 2012)' _computing_data_reduction SAINT _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994) ShelXle Rev 699 (Hubschle, 2011) ; _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.927 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_radiation_monochromator silicon(111) _diffrn_radiation_source 'Advanced Light Source Beamline 11.3.1' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_laue_measured_fraction_full 0.927 _diffrn_reflns_laue_measured_fraction_max 0.927 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2709 _diffrn_reflns_point_group_measured_fraction_full 0.927 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 20.425 _diffrn_reflns_theta_max 20.425 _diffrn_reflns_theta_min 2.210 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_T_max 0.745232 _exptl_absorpt_correction_T_min 0.542430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS 2012/1 (Sheldrick, 2012)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.500 _exptl_crystal_description block _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.482 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.116 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 563 _refine_ls_number_reflns 2709 _refine_ls_number_restraints 897 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.1052 _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^)+(0.1912P)^2^+14.0134P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2974 _refine_ls_wR_factor_ref 0.3116 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2265 _reflns_number_total 2709 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage3_Final _cod_original_cell_volume 2097.8(3) _cod_database_code 1541902 _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 0.720 _shelx_estimated_absorpt_t_max 0.817 _shelx_res_file ; Final_twin5.res created by SHELXL-2014/7 TITL twin4 in P-1 CELL 0.77490 13.0297 13.2995 14.0177 71.801 69.822 70.752 ZERR 2.00 0.0008 0.0009 0.0009 0.005 0.004 0.004 LATT 1 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 78 72 20 22 4 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -23.000 L.S. 200 BOND $H ACTA Omit 0 40.85 FMAP 2 PLAN 20 HTAB HTAB N1 O1_2a HTAB N1 O1_4b HTAB N5 O2 HTAB N6 Cl1_1a HTAB N6 O2_1a HTAB N6 O4_1a HTAB N6 Cl1_3b HTAB N6 O1_3b HTAB N6 O2_3b HTAB N10 O3 EQIV $1 -x+1, -y+2, -z HTAB_1a C25_0 O2_$1 HTAB_3b C25_0 O2_$1 HTAB_3b C25_0 O4_$1 HTAB C26 N4_$1 HTAB C26 N5_$1 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 RIGU WGHT 0.191200 14.013400 BASF 0.40254 FVAR 0.58271 0.54333 0.57829 FE1 6 0.498004 0.751973 0.249280 11.00000 0.04957 0.04865 = 0.05644 -0.00971 -0.01008 -0.01121 O1 4 0.131188 0.914607 0.701530 11.00000 0.07850 0.10113 = 0.09724 -0.03677 -0.01568 -0.01279 O2 4 0.834799 0.638486 -0.102556 11.00000 0.06188 0.13239 = 0.07528 -0.04723 -0.01133 -0.03022 N1 3 0.251339 0.812706 0.429288 11.00000 0.05852 0.06223 = 0.07136 -0.01591 -0.00715 -0.02388 AFIX 43 H1D 2 0.208729 0.794823 0.404523 11.00000 -1.20000 AFIX 0 N2 3 0.358405 0.803474 0.381675 11.00000 0.05233 0.04969 = 0.06001 -0.00932 -0.00888 -0.02344 N3 3 0.569953 0.806551 0.328831 11.00000 0.06199 0.03959 = 0.06861 -0.00905 -0.01209 -0.01464 N4 3 0.674438 0.737265 0.158048 11.00000 0.04782 0.03447 = 0.05247 -0.00482 -0.00902 -0.01767 N5 3 0.749687 0.699133 0.075637 11.00000 0.04684 0.06271 = 0.06386 -0.02031 -0.00746 -0.02010 AFIX 43 H5B 2 0.730549 0.676818 0.033600 11.00000 -1.20000 AFIX 0 N6 3 0.391384 0.990999 0.115610 11.00000 0.08200 0.05002 = 0.07289 -0.00017 -0.02914 -0.01556 AFIX 43 H6B 2 0.409212 1.031895 0.142115 11.00000 -1.20000 AFIX 0 N7 3 0.420080 0.882230 0.140894 11.00000 0.04418 0.05103 = 0.05245 -0.00603 -0.00394 -0.01340 N8 3 0.442594 0.671320 0.172044 11.00000 0.04270 0.05668 = 0.06342 -0.01123 -0.00611 -0.01170 N9 3 0.542657 0.579357 0.319123 11.00000 0.04184 0.04727 = 0.06421 -0.00813 -0.00715 -0.01107 N10 3 0.596914 0.513745 0.386313 11.00000 0.04434 0.04906 = 0.06917 -0.00691 -0.00902 -0.00797 AFIX 43 H10A 2 0.621628 0.535962 0.424449 11.00000 -1.20000 AFIX 0 C1 1 0.103311 0.936235 0.808657 11.00000 0.13793 0.15078 = 0.10951 -0.04990 -0.02064 -0.04116 AFIX 137 H1A 2 0.161127 0.888944 0.842829 11.00000 -1.50000 H1B 2 0.030713 0.921635 0.849990 11.00000 -1.50000 H1C 2 0.100239 1.011977 0.801757 11.00000 -1.50000 AFIX 0 C2 1 -0.061158 0.918248 0.725180 11.00000 0.07092 0.11982 = 0.10674 -0.05324 0.00639 -0.02341 AFIX 43 H2A 2 -0.088451 0.942149 0.787849 11.00000 -1.20000 AFIX 0 C3 1 0.049595 0.900052 0.672792 11.00000 0.06709 0.07764 = 0.07953 -0.02390 -0.00144 -0.01546 C4 1 -0.131183 0.900195 0.682560 11.00000 0.06203 0.09699 = 0.10208 -0.04342 0.00730 -0.01714 AFIX 43 H4A 2 -0.208726 0.913357 0.716882 11.00000 -1.20000 AFIX 0 C5 1 -0.095261 0.864755 0.594506 11.00000 0.06508 0.09999 = 0.11231 -0.04885 0.00083 -0.01619 AFIX 43 H5A 2 -0.146447 0.851002 0.569460 11.00000 -1.20000 AFIX 0 C6 1 0.017784 0.848437 0.540445 11.00000 0.05963 0.06805 = 0.08124 -0.02188 -0.00472 -0.01418 AFIX 43 H6A 2 0.043382 0.823347 0.478533 11.00000 -1.20000 AFIX 0 C7 1 0.093072 0.868659 0.576612 11.00000 0.06141 0.05782 = 0.07155 -0.00780 -0.00705 -0.01373 C8 1 0.210136 0.848405 0.512802 11.00000 0.05768 0.04526 = 0.06134 -0.00447 -0.01249 -0.01145 C9 1 0.302339 0.873421 0.524332 11.00000 0.05356 0.06037 = 0.06806 -0.02060 -0.00820 -0.00954 AFIX 43 H9A 2 0.301246 0.906238 0.575249 11.00000 -1.20000 AFIX 0 C10 1 0.394199 0.839438 0.444994 11.00000 0.05666 0.03368 = 0.06083 -0.01077 -0.01115 -0.01014 C11 1 0.507045 0.841766 0.413490 11.00000 0.06131 0.05244 = 0.07077 -0.01430 -0.01155 -0.01731 C12 1 0.557843 0.870050 0.474822 11.00000 0.06429 0.03817 = 0.08381 -0.02252 -0.02204 -0.00110 AFIX 43 H12A 2 0.517121 0.886117 0.540397 11.00000 -1.20000 AFIX 0 C13 1 0.666606 0.872064 0.432742 11.00000 0.06858 0.07565 = 0.08618 -0.03274 -0.02203 -0.01168 AFIX 43 H13A 2 0.699656 0.897106 0.467941 11.00000 -1.20000 AFIX 0 C14 1 0.729738 0.841914 0.346801 11.00000 0.06835 0.04434 = 0.08052 -0.02154 -0.02594 -0.00680 AFIX 43 H14A 2 0.806410 0.842621 0.322551 11.00000 -1.20000 AFIX 0 C15 1 0.680663 0.808255 0.291034 11.00000 0.05945 0.04887 = 0.06090 -0.01232 -0.01380 -0.01586 C16 1 0.739863 0.768693 0.195533 11.00000 0.05282 0.04515 = 0.06012 -0.01213 -0.01499 -0.01363 C17 1 0.849913 0.745372 0.144508 11.00000 0.05461 0.07553 = 0.06878 -0.02766 -0.01006 -0.02338 AFIX 43 H17A 2 0.909878 0.757281 0.158698 11.00000 -1.20000 AFIX 0 C18 1 0.855098 0.698339 0.063745 11.00000 0.04547 0.05123 = 0.06133 -0.01495 -0.00763 -0.01832 C19 1 0.955356 0.658676 -0.021412 11.00000 0.04902 0.08519 = 0.06804 -0.03217 -0.00841 -0.01559 C20 1 1.060930 0.654835 -0.018518 11.00000 0.04959 0.08245 = 0.07475 -0.03220 -0.00902 -0.01742 AFIX 43 H20A 2 1.067873 0.676742 0.036094 11.00000 -1.20000 AFIX 0 C21 1 1.155891 0.620169 -0.092565 11.00000 0.05250 0.11397 = 0.09320 -0.05185 -0.00221 -0.01792 AFIX 43 H21A 2 1.227536 0.618547 -0.089899 11.00000 -1.20000 AFIX 0 C22 1 1.143520 0.586590 -0.173805 11.00000 0.07285 0.13504 = 0.09007 -0.05246 -0.00013 -0.03110 AFIX 43 H22A 2 1.206539 0.559422 -0.225258 11.00000 -1.20000 AFIX 0 C23 1 1.040678 0.595055 -0.174046 11.00000 0.07071 0.10319 = 0.08079 -0.03256 -0.00081 -0.03123 AFIX 43 H23A 2 1.030500 0.579123 -0.230468 11.00000 -1.20000 AFIX 0 C24 1 0.945167 0.626572 -0.094713 11.00000 0.06233 0.07539 = 0.06370 -0.02081 -0.00910 -0.02897 C25 1 0.820758 0.617444 -0.191233 11.00000 0.09072 0.15360 = 0.08429 -0.05360 -0.01863 -0.04611 AFIX 137 H25A 2 0.744662 0.610171 -0.175679 11.00000 -1.50000 H25B 2 0.874583 0.550339 -0.207015 11.00000 -1.50000 H25C 2 0.833550 0.677616 -0.250864 11.00000 -1.50000 AFIX 0 C26 1 0.332355 1.030267 0.045233 11.00000 0.06460 0.06833 = 0.06490 -0.00135 -0.01551 -0.01475 AFIX 43 H26A 2 0.306982 1.104141 0.013951 11.00000 -1.20000 AFIX 0 C27 1 0.315935 0.942332 0.027444 11.00000 0.04784 0.07109 = 0.05950 -0.00770 -0.01003 -0.00942 AFIX 43 H27A 2 0.273442 0.942557 -0.014909 11.00000 -1.20000 AFIX 0 C28 1 0.374985 0.853947 0.084875 11.00000 0.05603 0.06411 = 0.06128 -0.00869 -0.01435 -0.01292 C29 1 0.384836 0.739326 0.100063 11.00000 0.04381 0.06457 = 0.06476 -0.01535 -0.00890 -0.00644 C30 1 0.347947 0.687111 0.047524 11.00000 0.07641 0.07853 = 0.10299 -0.02627 -0.03852 -0.00616 AFIX 43 H30A 2 0.308525 0.728342 -0.002740 11.00000 -1.20000 AFIX 0 C31 1 0.370146 0.582128 0.070871 11.00000 0.07759 0.07886 = 0.11034 -0.02393 -0.03951 -0.00687 AFIX 43 H31A 2 0.345217 0.549723 0.035039 11.00000 -1.20000 AFIX 0 C32 1 0.424435 0.514743 0.140078 11.00000 0.07319 0.06460 = 0.11422 -0.02576 -0.03946 -0.00280 AFIX 43 H32A 2 0.440655 0.438416 0.150528 11.00000 -1.20000 AFIX 0 C33 1 0.456836 0.565036 0.197857 11.00000 0.05514 0.05567 = 0.07863 -0.01061 -0.01655 -0.01081 C34 1 0.515808 0.511735 0.273005 11.00000 0.02722 0.04482 = 0.06508 -0.01383 0.00371 -0.00403 C35 1 0.560941 0.402678 0.317936 11.00000 0.05876 0.04424 = 0.09099 -0.01333 -0.01818 -0.00236 AFIX 43 H35A 2 0.559377 0.338564 0.304023 11.00000 -1.20000 AFIX 0 C36 1 0.610064 0.413287 0.390374 11.00000 0.05113 0.05067 = 0.08261 -0.00732 -0.00972 -0.01053 AFIX 43 H36A 2 0.646848 0.354348 0.434691 11.00000 -1.20000 AFIX 0 PART 1 RESI 1 CLO4 CL1 5 0.473506 1.163772 0.221856 21.00000 0.03809 O1 4 0.566836 1.200961 0.208268 21.00000 0.19025 O2 4 0.431382 1.214141 0.134294 21.00000 0.21594 O3 4 0.388622 1.190456 0.310150 21.00000 0.16541 O4 4 0.504457 1.050971 0.231422 21.00000 0.13014 RESI 2 CLO4 CL1 5 0.089841 0.739386 0.263106 31.00000 0.08947 O1 4 0.182262 0.744835 0.288724 31.00000 0.15242 O2 4 0.083196 0.805869 0.166108 31.00000 0.10328 O3 4 0.099002 0.631220 0.264757 31.00000 0.14360 O4 4 -0.008521 0.774789 0.339463 31.00000 0.11294 PART 2 RESI 4 CLO4 CL1 5 0.088753 0.712186 0.291626 -31.00000 0.05766 O1 4 0.187837 0.679454 0.322950 -31.00000 0.06110 O2 4 0.074180 0.821155 0.236087 -31.00000 0.25294 O3 4 0.096820 0.646866 0.227036 -31.00000 0.19348 O4 4 -0.003511 0.702724 0.379065 -31.00000 0.09407 RESI 3 CLO4 CL1 5 0.469294 1.168054 0.229282 -21.00000 0.28639 O1 4 0.432549 1.075549 0.293798 -21.00000 0.20561 O2 4 0.440672 1.194798 0.135536 -21.00000 0.08045 O3 4 0.586152 1.145726 0.209593 -21.00000 0.19858 O4 4 0.416795 1.255058 0.279251 -21.00000 0.12375 PART 0 RESI 0 C39 1 0.808664 0.597267 0.569605 11.00000 0.09554 0.11632 = 0.10820 -0.04539 -0.03495 -0.02302 AFIX 33 H39A 2 0.890024 0.572217 0.557085 11.00000 -1.50000 H39B 2 0.786236 0.676275 0.558695 11.00000 -1.50000 H39C 2 0.772776 0.565149 0.640816 11.00000 -1.50000 AFIX 0 C37 1 0.864578 0.495814 0.440652 11.00000 0.07329 0.16526 = 0.12942 -0.08613 -0.02966 -0.00977 AFIX 33 H37A 2 0.936578 0.488296 0.451548 11.00000 -1.50000 H37B 2 0.848835 0.424549 0.460911 11.00000 -1.50000 H37C 2 0.867489 0.526851 0.367561 11.00000 -1.50000 AFIX 0 C38 1 0.776560 0.566839 0.503033 11.00000 0.06939 0.10378 = 0.08383 -0.03447 -0.01175 -0.02677 O3 4 0.679479 0.586821 0.500394 11.00000 0.07257 0.12853 = 0.10996 -0.04862 -0.02140 -0.02214 HKLF 5 REM twin4 in P-1 REM R1 = 0.1052 for 2265 Fo > 4sig(Fo) and 0.1228 for all 2709 data REM 563 parameters refined using 897 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 O1_2 HTAB N1 O1_4 HTAB N5 O2 HTAB N6 Cl1_1 HTAB N6 O2_1 HTAB N6 O4_1 HTAB N6 Cl1_3 HTAB N6 O1_3 HTAB N6 O2_3 HTAB N10 O3 EQIV $2 -x+1, -y+2, -z+1 HTAB_1 C12_0 O3_$2 EQIV $3 x+1, y, z HTAB_2 C14_0 O4_$3 HTAB_2 C17_0 O2_$3 EQIV $4 -x+1, -y+1, -z HTAB_4 C25_0 O3_$4 HTAB C26 N4_$1 HTAB C26 N5_$1 EQIV $5 x, y-1, z HTAB_3 C32_0 O4_$5 HTAB_1 C35_0 O1_$5 HTAB_3 C35_0 O4_$5 REM Highest difference peak 0.482, deepest hole -0.489, 1-sigma level 0.116 Q1 1 0.5943 1.0556 0.2176 11.00000 0.05 0.48 Q2 1 0.5193 1.1427 0.2467 11.00000 0.05 0.48 Q3 1 0.3934 0.7856 0.3258 11.00000 0.05 0.43 Q4 1 0.5763 0.7871 0.2626 11.00000 0.05 0.43 Q5 1 0.4993 0.8223 0.3284 11.00000 0.05 0.42 Q6 1 0.9146 0.5784 0.1040 11.00000 0.05 0.42 Q7 1 0.6158 0.7778 0.1614 11.00000 0.05 0.42 Q8 1 0.5027 1.2653 0.1949 11.00000 0.05 0.39 Q9 1 0.2776 1.2021 0.1475 11.00000 0.05 0.39 Q10 1 0.7368 0.4445 0.4827 11.00000 0.05 0.39 Q11 1 0.7284 0.7027 0.1622 11.00000 0.05 0.39 Q12 1 0.0683 0.9165 0.8965 11.00000 0.05 0.39 Q13 1 0.5664 0.6386 0.2718 11.00000 0.05 0.38 Q14 1 0.5935 0.6379 0.2486 11.00000 0.05 0.38 Q15 1 0.0301 0.6450 0.3213 11.00000 0.05 0.37 Q16 1 1.0000 0.5000 0.5000 10.50000 0.05 0.37 Q17 1 0.1836 0.6158 0.2801 11.00000 0.05 0.37 Q18 1 0.4239 1.1324 0.1192 11.00000 0.05 0.35 Q19 1 1.2062 0.4634 -0.1333 11.00000 0.05 0.35 Q20 1 -0.2517 1.0169 0.7043 11.00000 0.05 0.35 ; _shelx_res_checksum 83132 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.4980(2) 0.7520(2) 0.2493(2) 0.0535(11) Uani 1 1 d . U . . . O1 O 0.1312(13) 0.9146(13) 0.7015(13) 0.093(5) Uani 1 1 d . U . . . O2 O 0.8348(11) 0.6385(14) -0.1026(11) 0.084(5) Uani 1 1 d . U . . . N1 N 0.2513(13) 0.8127(13) 0.4293(13) 0.064(4) Uani 1 1 d . U . . . H1D H 0.2087 0.7948 0.4045 0.077 Uiso 1 1 calc R U . . . N2 N 0.3584(12) 0.8035(12) 0.3817(12) 0.054(4) Uani 1 1 d . U . . . N3 N 0.5700(14) 0.8066(12) 0.3288(13) 0.058(4) Uani 1 1 d . U . . . N4 N 0.6744(12) 0.7373(11) 0.1580(11) 0.045(3) Uani 1 1 d . U . . . N5 N 0.7497(12) 0.6991(12) 0.0756(12) 0.057(4) Uani 1 1 d . U . . . H5B H 0.7305 0.6768 0.0336 0.068 Uiso 1 1 calc R U . . . N6 N 0.3914(14) 0.9910(14) 0.1156(13) 0.070(4) Uani 1 1 d . U . . . H6B H 0.4092 1.0319 0.1421 0.084 Uiso 1 1 calc R U . . . N7 N 0.4201(12) 0.8822(13) 0.1409(12) 0.053(4) Uani 1 1 d . U . . . N8 N 0.4426(12) 0.6713(14) 0.1720(13) 0.057(4) Uani 1 1 d . U . . . N9 N 0.5427(12) 0.5794(12) 0.3191(12) 0.054(3) Uani 1 1 d . U . . . N10 N 0.5969(12) 0.5137(13) 0.3863(12) 0.058(4) Uani 1 1 d . U . . . H10A H 0.6216 0.5360 0.4244 0.070 Uiso 1 1 calc R U . . . C1 C 0.103(3) 0.936(3) 0.809(2) 0.130(10) Uani 1 1 d . U . . . H1A H 0.1611 0.8889 0.8428 0.195 Uiso 1 1 calc R U . . . H1B H 0.0307 0.9216 0.8500 0.195 Uiso 1 1 calc R U . . . H1C H 0.1002 1.0120 0.8018 0.195 Uiso 1 1 calc R U . . . C2 C -0.061(2) 0.918(2) 0.725(2) 0.101(8) Uani 1 1 d . U . . . H2A H -0.0885 0.9421 0.7878 0.121 Uiso 1 1 calc R U . . . C3 C 0.050(2) 0.9001(19) 0.6728(18) 0.079(6) Uani 1 1 d . U . . . C4 C -0.131(2) 0.900(2) 0.683(2) 0.091(7) Uani 1 1 d . U . . . H4A H -0.2087 0.9134 0.7169 0.109 Uiso 1 1 calc R U . . . C5 C -0.0953(19) 0.865(2) 0.595(2) 0.094(7) Uani 1 1 d . U . . . H5A H -0.1464 0.8510 0.5695 0.113 Uiso 1 1 calc R U . . . C6 C 0.0178(17) 0.8484(17) 0.5404(18) 0.073(6) Uani 1 1 d . U . . . H6A H 0.0434 0.8233 0.4785 0.087 Uiso 1 1 calc R U . . . C7 C 0.0931(17) 0.8687(17) 0.5766(17) 0.069(5) Uani 1 1 d . U . . . C8 C 0.2101(17) 0.8484(16) 0.5128(17) 0.058(5) Uani 1 1 d . U . . . C9 C 0.3023(16) 0.8734(16) 0.5243(16) 0.063(5) Uani 1 1 d . U . . . H9A H 0.3012 0.9062 0.5752 0.075 Uiso 1 1 calc R U . . . C10 C 0.3942(16) 0.8394(14) 0.4450(15) 0.052(4) Uani 1 1 d . U . . . C11 C 0.5070(17) 0.8418(16) 0.4135(17) 0.062(5) Uani 1 1 d . U . . . C12 C 0.5578(17) 0.8701(15) 0.4748(17) 0.062(5) Uani 1 1 d . U . . . H12A H 0.5171 0.8861 0.5404 0.075 Uiso 1 1 calc R U . . . C13 C 0.6666(18) 0.8721(17) 0.4327(18) 0.075(6) Uani 1 1 d . U . . . H13A H 0.6997 0.8971 0.4679 0.089 Uiso 1 1 calc R U . . . C14 C 0.7297(18) 0.8419(15) 0.3468(17) 0.063(5) Uani 1 1 d . U . . . H14A H 0.8064 0.8426 0.3226 0.075 Uiso 1 1 calc R U . . . C15 C 0.6807(16) 0.8083(16) 0.2910(16) 0.056(5) Uani 1 1 d . U . . . C16 C 0.7399(16) 0.7687(15) 0.1955(16) 0.052(5) Uani 1 1 d . U . . . C17 C 0.8499(16) 0.7454(16) 0.1445(16) 0.063(6) Uani 1 1 d . U . . . H17A H 0.9099 0.7573 0.1587 0.076 Uiso 1 1 calc R U . . . C18 C 0.8551(15) 0.6983(15) 0.0637(15) 0.052(5) Uani 1 1 d . U . . . C19 C 0.9554(17) 0.6587(18) -0.0214(17) 0.066(6) Uani 1 1 d . U . . . C20 C 1.0609(16) 0.6548(17) -0.0185(17) 0.067(6) Uani 1 1 d . U . . . H20A H 1.0679 0.6767 0.0361 0.081 Uiso 1 1 calc R U . . . C21 C 1.1559(18) 0.620(2) -0.0926(19) 0.085(7) Uani 1 1 d . U . . . H21A H 1.2275 0.6185 -0.0899 0.102 Uiso 1 1 calc R U . . . C22 C 1.144(2) 0.587(2) -0.174(2) 0.097(8) Uani 1 1 d . U . . . H22A H 1.2065 0.5594 -0.2253 0.117 Uiso 1 1 calc R U . . . C23 C 1.0407(19) 0.5951(19) -0.1740(18) 0.085(6) Uani 1 1 d . U . . . H23A H 1.0305 0.5791 -0.2305 0.102 Uiso 1 1 calc R U . . . C24 C 0.9452(17) 0.6266(17) -0.0947(17) 0.065(5) Uani 1 1 d . U . . . C25 C 0.821(2) 0.617(2) -0.1912(18) 0.100(9) Uani 1 1 d . U . . . H25A H 0.7447 0.6102 -0.1757 0.150 Uiso 1 1 calc R U . . . H25B H 0.8746 0.5503 -0.2070 0.150 Uiso 1 1 calc R U . . . H25C H 0.8335 0.6776 -0.2509 0.150 Uiso 1 1 calc R U . . . C26 C 0.3324(17) 1.030(2) 0.0452(17) 0.070(5) Uani 1 1 d . U . . . H26A H 0.3070 1.1041 0.0140 0.084 Uiso 1 1 calc R U . . . C27 C 0.3159(16) 0.9423(18) 0.0274(16) 0.064(5) Uani 1 1 d . U . . . H27A H 0.2734 0.9426 -0.0149 0.077 Uiso 1 1 calc R U . . . C28 C 0.3750(16) 0.8539(18) 0.0849(17) 0.063(5) Uani 1 1 d . U . . . C29 C 0.3848(15) 0.7393(17) 0.1001(16) 0.061(4) Uani 1 1 d . U . . . C30 C 0.3479(19) 0.687(2) 0.0475(19) 0.084(6) Uani 1 1 d . U . . . H30A H 0.3085 0.7283 -0.0027 0.101 Uiso 1 1 calc R U . . . C31 C 0.3701(19) 0.582(2) 0.071(2) 0.088(6) Uani 1 1 d . U . . . H31A H 0.3452 0.5497 0.0350 0.105 Uiso 1 1 calc R U . . . C32 C 0.4244(18) 0.5147(19) 0.1401(19) 0.082(6) Uani 1 1 d . U . . . H32A H 0.4407 0.4384 0.1505 0.099 Uiso 1 1 calc R U . . . C33 C 0.4568(17) 0.5650(18) 0.1979(17) 0.065(5) Uani 1 1 d . U . . . C34 C 0.5158(14) 0.5117(15) 0.2730(15) 0.051(4) Uani 1 1 d . U . . . C35 C 0.5609(16) 0.4027(17) 0.3179(17) 0.068(5) Uani 1 1 d . U . . . H35A H 0.5594 0.3386 0.3040 0.082 Uiso 1 1 calc R U . . . C36 C 0.6101(17) 0.4133(18) 0.3904(18) 0.066(5) Uani 1 1 d . U . . . H36A H 0.6468 0.3543 0.4347 0.079 Uiso 1 1 calc R U . . . Cl1_1 Cl 0.4735(7) 1.1638(7) 0.2219(7) 0.038(7) Uiso 0.54(5) 1 d D . P A 1 O1_1 O 0.567(2) 1.201(3) 0.208(3) 0.19(3) Uiso 0.54(5) 1 d D . P A 1 O2_1 O 0.431(4) 1.214(3) 0.134(2) 0.22(5) Uiso 0.54(5) 1 d D . P A 1 O3_1 O 0.389(2) 1.190(4) 0.310(2) 0.17(2) Uiso 0.54(5) 1 d D . P A 1 O4_1 O 0.504(3) 1.0510(12) 0.231(3) 0.130(17) Uiso 0.54(5) 1 d D . P A 1 Cl1_2 Cl 0.0898(11) 0.7394(18) 0.2631(16) 0.089(6) Uiso 0.58(4) 1 d D . P B 1 O1_2 O 0.1823(18) 0.745(3) 0.289(3) 0.152(16) Uiso 0.58(4) 1 d D . P B 1 O2_2 O 0.083(2) 0.806(2) 0.166(2) 0.103(13) Uiso 0.58(4) 1 d D . P B 1 O3_2 O 0.099(3) 0.631(2) 0.265(3) 0.144(19) Uiso 0.58(4) 1 d D . P B 1 O4_2 O -0.0085(16) 0.775(3) 0.339(2) 0.113(12) Uiso 0.58(4) 1 d D . P B 1 Cl1_4 Cl 0.0888(12) 0.7122(15) 0.2916(17) 0.058(7) Uiso 0.42(4) 1 d D . P B 2 O1_4 O 0.1878(16) 0.679(3) 0.323(2) 0.061(13) Uiso 0.42(4) 1 d D . P B 2 O2_4 O 0.074(4) 0.821(2) 0.236(5) 0.25(4) Uiso 0.42(4) 1 d D . P B 2 O3_4 O 0.097(3) 0.647(4) 0.227(3) 0.19(4) Uiso 0.42(4) 1 d D . P B 2 O4_4 O -0.0035(18) 0.703(4) 0.379(2) 0.094(16) Uiso 0.42(4) 1 d D . P B 2 Cl1_3 Cl 0.469(2) 1.168(2) 0.229(2) 0.29(4) Uiso 0.46(5) 1 d D . P A 2 O1_3 O 0.433(5) 1.076(3) 0.294(4) 0.21(3) Uiso 0.46(5) 1 d D . P A 2 O2_3 O 0.441(3) 1.195(3) 0.136(2) 0.080(19) Uiso 0.46(5) 1 d D . P A 2 O3_3 O 0.586(2) 1.146(5) 0.210(4) 0.20(3) Uiso 0.46(5) 1 d D . P A 2 O4_3 O 0.417(3) 1.255(3) 0.279(3) 0.12(2) Uiso 0.46(5) 1 d D . P A 2 C39 C 0.809(2) 0.597(2) 0.570(2) 0.100(8) Uani 1 1 d . U . . . H39A H 0.8900 0.5722 0.5571 0.151 Uiso 1 1 calc R U . . . H39B H 0.7862 0.6763 0.5587 0.151 Uiso 1 1 calc R U . . . H39C H 0.7728 0.5651 0.6408 0.151 Uiso 1 1 calc R U . . . C37 C 0.8646(19) 0.496(2) 0.441(2) 0.114(10) Uani 1 1 d . U . . . H37A H 0.9366 0.4883 0.4515 0.171 Uiso 1 1 calc R U . . . H37B H 0.8488 0.4245 0.4609 0.171 Uiso 1 1 calc R U . . . H37C H 0.8675 0.5269 0.3676 0.171 Uiso 1 1 calc R U . . . C38 C 0.777(2) 0.567(2) 0.5030(19) 0.083(7) Uani 1 1 d . U . . . O3 O 0.6795(13) 0.5868(15) 0.5004(13) 0.100(5) Uani 1 1 d . 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 Fe1 0.0496(19) 0.049(2) 0.056(2) -0.0097(14) -0.0101(13) -0.0112(13) O1 0.078(9) 0.101(12) 0.097(10) -0.037(9) -0.016(7) -0.013(8) O2 0.062(7) 0.132(13) 0.075(9) -0.047(9) -0.011(6) -0.030(7) N1 0.059(6) 0.062(11) 0.071(8) -0.016(8) -0.007(5) -0.024(6) N2 0.052(6) 0.050(9) 0.060(6) -0.009(6) -0.009(5) -0.023(5) N3 0.062(6) 0.040(8) 0.069(7) -0.009(6) -0.012(5) -0.015(5) N4 0.048(5) 0.034(8) 0.052(7) -0.005(6) -0.009(4) -0.018(5) N5 0.047(6) 0.063(10) 0.064(7) -0.020(7) -0.007(5) -0.020(6) N6 0.082(11) 0.050(7) 0.073(10) 0.000(6) -0.029(8) -0.016(6) N7 0.044(7) 0.051(6) 0.052(7) -0.006(5) -0.004(6) -0.013(5) N8 0.043(8) 0.057(6) 0.063(7) -0.011(5) -0.006(6) -0.012(5) N9 0.042(8) 0.047(6) 0.064(7) -0.008(5) -0.007(6) -0.011(5) N10 0.044(8) 0.049(7) 0.069(8) -0.007(7) -0.009(7) -0.008(7) C1 0.14(2) 0.15(3) 0.110(13) -0.050(14) -0.021(13) -0.041(19) C2 0.071(8) 0.12(2) 0.107(12) -0.053(13) 0.006(8) -0.023(9) C3 0.067(8) 0.078(15) 0.080(9) -0.024(9) -0.001(6) -0.015(8) C4 0.062(10) 0.097(18) 0.102(13) -0.043(12) 0.007(8) -0.017(9) C5 0.065(9) 0.100(18) 0.112(14) -0.049(13) 0.001(8) -0.016(9) C6 0.060(8) 0.068(14) 0.081(11) -0.022(10) -0.005(7) -0.014(8) C7 0.061(7) 0.058(13) 0.072(9) -0.008(9) -0.007(6) -0.014(7) C8 0.058(6) 0.045(12) 0.061(9) -0.004(8) -0.012(5) -0.011(6) C9 0.054(7) 0.060(12) 0.068(9) -0.021(9) -0.008(6) -0.010(7) C10 0.057(6) 0.034(11) 0.061(8) -0.011(8) -0.011(5) -0.010(6) C11 0.061(6) 0.052(12) 0.071(8) -0.014(8) -0.012(5) -0.017(6) C12 0.064(8) 0.038(11) 0.084(10) -0.023(9) -0.022(7) -0.001(8) C13 0.069(8) 0.076(15) 0.086(10) -0.033(10) -0.022(7) -0.012(9) C14 0.068(9) 0.044(12) 0.081(10) -0.022(9) -0.026(7) -0.007(8) C15 0.059(6) 0.049(12) 0.061(8) -0.012(8) -0.014(5) -0.016(6) C16 0.053(6) 0.045(11) 0.060(7) -0.012(8) -0.015(5) -0.014(6) C17 0.055(7) 0.076(14) 0.069(9) -0.028(10) -0.010(6) -0.023(7) C18 0.045(6) 0.051(11) 0.061(8) -0.015(8) -0.008(5) -0.018(6) C19 0.049(6) 0.085(15) 0.068(9) -0.032(10) -0.008(5) -0.016(7) C20 0.050(7) 0.082(15) 0.075(11) -0.032(11) -0.009(6) -0.017(8) C21 0.053(8) 0.114(18) 0.093(12) -0.052(12) -0.002(7) -0.018(9) C22 0.073(9) 0.14(2) 0.090(13) -0.052(14) 0.000(8) -0.031(10) C23 0.071(8) 0.103(17) 0.081(10) -0.033(11) -0.001(7) -0.031(9) C24 0.062(7) 0.075(14) 0.064(9) -0.021(9) -0.009(6) -0.029(7) C25 0.091(15) 0.15(2) 0.084(13) -0.054(14) -0.019(11) -0.046(15) C26 0.065(11) 0.068(8) 0.065(11) -0.001(7) -0.016(9) -0.015(7) C27 0.048(10) 0.071(8) 0.059(10) -0.008(7) -0.010(8) -0.009(7) C28 0.056(11) 0.064(7) 0.061(10) -0.009(6) -0.014(8) -0.013(6) C29 0.044(10) 0.065(7) 0.065(9) -0.015(6) -0.009(8) -0.006(6) C30 0.076(14) 0.079(10) 0.103(13) -0.026(9) -0.039(11) -0.006(9) C31 0.078(15) 0.079(10) 0.110(13) -0.024(9) -0.040(12) -0.007(9) C32 0.073(14) 0.065(10) 0.114(13) -0.026(9) -0.039(11) -0.003(9) C33 0.055(10) 0.056(7) 0.079(9) -0.011(6) -0.017(8) -0.011(6) C34 0.027(8) 0.045(7) 0.065(8) -0.014(6) 0.004(7) -0.004(6) C35 0.059(12) 0.044(7) 0.091(12) -0.013(7) -0.018(10) -0.002(6) C36 0.051(11) 0.051(8) 0.083(11) -0.007(7) -0.010(9) -0.011(7) C39 0.096(14) 0.12(2) 0.108(16) -0.045(15) -0.035(12) -0.023(13) C37 0.073(12) 0.17(2) 0.13(2) -0.086(19) -0.030(11) -0.010(12) C38 0.069(10) 0.104(16) 0.084(14) -0.034(12) -0.012(9) -0.027(10) O3 0.073(9) 0.129(14) 0.110(12) -0.049(11) -0.021(9) -0.022(9) 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 N3 Fe1 N7 112.7(6) N3 Fe1 N9 98.1(6) N7 Fe1 N9 149.2(6) N3 Fe1 N8 170.9(6) N7 Fe1 N8 75.6(7) N9 Fe1 N8 73.6(7) N3 Fe1 N4 74.9(6) N7 Fe1 N4 98.7(5) N9 Fe1 N4 88.4(5) N8 Fe1 N4 100.7(6) N3 Fe1 N2 74.9(6) N7 Fe1 N2 90.9(6) N9 Fe1 N2 98.1(5) N8 Fe1 N2 109.6(6) N4 Fe1 N2 149.6(6) C3 O1 C1 118.7(19) C24 O2 C25 120.7(16) C8 N1 N2 118.9(18) C8 N1 H1D 120.5 N2 N1 H1D 120.5 N1 N2 C10 102.3(15) N1 N2 Fe1 145.6(13) C10 N2 Fe1 112.1(11) C11 N3 C15 120.8(17) C11 N3 Fe1 119.5(14) C15 N3 Fe1 119.7(13) C16 N4 N5 102.2(15) C16 N4 Fe1 116.0(12) N5 N4 Fe1 141.6(12) C18 N5 N4 114.5(16) C18 N5 H5B 122.7 N4 N5 H5B 122.7 C26 N6 N7 113(2) C26 N6 H6B 123.7 N7 N6 H6B 123.7 C28 N7 N6 103.8(18) C28 N7 Fe1 116.5(14) N6 N7 Fe1 139.4(14) C33 N8 C29 123.1(18) C33 N8 Fe1 121.2(16) C29 N8 Fe1 115.6(13) N10 N9 C34 106.8(15) N10 N9 Fe1 139.0(13) C34 N9 Fe1 113.9(12) C36 N10 N9 113(2) C36 N10 H10A 123.6 N9 N10 H10A 123.6 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 C4 C2 C3 117(2) C4 C2 H2A 121.7 C3 C2 H2A 121.7 O1 C3 C2 125(2) O1 C3 C7 111(2) C2 C3 C7 123(2) C5 C4 C2 123(2) C5 C4 H4A 118.3 C2 C4 H4A 118.3 C4 C5 C6 120(2) C4 C5 H5A 120.2 C6 C5 H5A 120.2 C7 C6 C5 120(2) C7 C6 H6A 119.8 C5 C6 H6A 119.8 C3 C7 C6 116(2) C3 C7 C8 128(2) C6 C7 C8 115(2) N1 C8 C9 103.8(18) N1 C8 C7 128(2) C9 C8 C7 128(2) C10 C9 C8 105.6(19) C10 C9 H9A 127.2 C8 C9 H9A 127.2 N2 C10 C9 109.1(17) N2 C10 C11 116.7(17) C9 C10 C11 134(2) N3 C11 C10 117(2) N3 C11 C12 120.1(19) C10 C11 C12 122.8(19) C13 C12 C11 116(2) C13 C12 H12A 122.0 C11 C12 H12A 122.0 C14 C13 C12 125(2) C14 C13 H13A 117.6 C12 C13 H13A 117.6 C13 C14 C15 118(2) C13 C14 H14A 120.8 C15 C14 H14A 120.8 N3 C15 C14 119.5(18) N3 C15 C16 115.0(18) C14 C15 C16 125.5(19) N4 C16 C17 113.6(18) N4 C16 C15 114.4(17) C17 C16 C15 131.4(19) C16 C17 C18 104.2(17) C16 C17 H17A 127.9 C18 C17 H17A 127.9 N5 C18 C17 105.3(16) N5 C18 C19 125.1(18) C17 C18 C19 129.5(17) C24 C19 C20 120(2) C24 C19 C18 122.3(19) C20 C19 C18 118(2) C21 C20 C19 122(2) C21 C20 H20A 119.1 C19 C20 H20A 119.1 C20 C21 C22 118(2) C20 C21 H21A 120.9 C22 C21 H21A 120.9 C23 C22 C21 117(2) C23 C22 H22A 121.4 C21 C22 H22A 121.4 C22 C23 C24 123(2) C22 C23 H23A 118.3 C24 C23 H23A 118.3 C19 C24 C23 120(2) C19 C24 O2 119.5(19) C23 C24 O2 120(2) 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 107(2) N6 C26 H26A 126.7 C27 C26 H26A 126.7 C26 C27 C28 105(2) C26 C27 H27A 127.7 C28 C27 H27A 127.7 N7 C28 C27 112(2) N7 C28 C29 118(2) C27 C28 C29 130(2) N8 C29 C30 116.3(19) N8 C29 C28 114.8(19) C30 C29 C28 129(2) C31 C30 C29 118(2) C31 C30 H30A 120.9 C29 C30 H30A 120.9 C30 C31 C32 127(3) C30 C31 H31A 116.5 C32 C31 H31A 116.5 C31 C32 C33 116(2) C31 C32 H32A 122.0 C33 C32 H32A 122.0 N8 C33 C32 119(2) N8 C33 C34 114(2) C32 C33 C34 127(2) C35 C34 C33 136(2) C35 C34 N9 107.1(18) C33 C34 N9 117.0(17) C36 C35 C34 102.8(19) C36 C35 H35A 128.6 C34 C35 H35A 128.6 N10 C36 C35 111(2) N10 C36 H36A 124.7 C35 C36 H36A 124.7 O1_1 Cl1_1 O4_1 110.3(10) O1_1 Cl1_1 O3_1 110.5(10) O4_1 Cl1_1 O3_1 109.9(10) O1_1 Cl1_1 O2_1 108.9(10) O4_1 Cl1_1 O2_1 108.6(10) O3_1 Cl1_1 O2_1 108.6(10) O2_2 Cl1_2 O3_2 110.5(10) O2_2 Cl1_2 O1_2 110.8(10) O3_2 Cl1_2 O1_2 109.6(10) O2_2 Cl1_2 O4_2 109.5(10) O3_2 Cl1_2 O4_2 108.5(10) O1_2 Cl1_2 O4_2 107.9(10) O3_4 Cl1_4 O1_4 109.5(10) O3_4 Cl1_4 O4_4 109.9(10) O1_4 Cl1_4 O4_4 109.8(10) O3_4 Cl1_4 O2_4 109.0(10) O1_4 Cl1_4 O2_4 109.3(10) O4_4 Cl1_4 O2_4 109.3(10) O3_3 Cl1_3 O4_3 109.9(10) O3_3 Cl1_3 O2_3 109.8(10) O4_3 Cl1_3 O2_3 109.6(10) O3_3 Cl1_3 O1_3 109.2(11) O4_3 Cl1_3 O1_3 109.1(10) O2_3 Cl1_3 O1_3 109.3(10) C38 C39 H39A 109.5 C38 C39 H39B 109.5 H39A C39 H39B 109.5 C38 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C38 C37 H37A 109.5 C38 C37 H37B 109.5 H37A C37 H37B 109.5 C38 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 O3 C38 C39 124(2) O3 C38 C37 120(2) C39 C38 C37 115(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3 2.080(16) Fe1 N7 2.145(16) Fe1 N9 2.162(16) Fe1 N8 2.149(16) Fe1 N4 2.189(14) Fe1 N2 2.206(15) O1 C3 1.35(3) O1 C1 1.51(3) O2 C24 1.43(2) O2 C25 1.44(2) N1 C8 1.28(2) N1 N2 1.305(19) N1 H1D 0.8700 N2 C10 1.39(2) N3 C11 1.31(2) N3 C15 1.36(2) N4 C16 1.36(2) N4 N5 1.345(19) N5 C18 1.32(2) N5 H5B 0.8700 N6 C26 1.33(2) N6 N7 1.33(2) N6 H6B 0.8700 N7 C28 1.32(2) N8 C33 1.31(2) N8 C29 1.38(2) N9 N10 1.299(19) N9 C34 1.44(2) N10 C36 1.28(2) N10 H10A 0.8700 C1 H1A 0.9700 C1 H1B 0.9700 C1 H1C 0.9700 C2 C4 1.36(3) C2 C3 1.35(3) C2 H2A 0.9400 C3 C7 1.41(3) C4 C5 1.34(3) C4 H4A 0.9400 C5 C6 1.38(3) C5 H5A 0.9400 C6 C7 1.38(3) C6 H6A 0.9400 C7 C8 1.46(3) C8 C9 1.42(3) C9 C10 1.38(3) C9 H9A 0.9400 C10 C11 1.39(3) C11 C12 1.44(3) C12 C13 1.34(3) C12 H12A 0.9400 C13 C14 1.30(3) C13 H13A 0.9400 C14 C15 1.40(3) C14 H14A 0.9400 C15 C16 1.46(3) C16 C17 1.34(3) C17 C18 1.43(3) C17 H17A 0.9400 C18 C19 1.51(3) C19 C24 1.29(3) C19 C20 1.37(3) C20 C21 1.36(3) C20 H20A 0.9400 C21 C22 1.42(3) C21 H21A 0.9400 C22 C23 1.31(3) C22 H22A 0.9400 C23 C24 1.40(3) 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 1.36(3) C27 H27A 0.9400 C28 C29 1.44(3) C29 C30 1.43(3) C30 C31 1.29(3) C30 H30A 0.9400 C31 C32 1.33(3) C31 H31A 0.9400 C32 C33 1.43(3) C32 H32A 0.9400 C33 C34 1.39(3) C34 C35 1.40(3) C35 C36 1.43(3) C35 H35A 0.9400 C36 H36A 0.9400 Cl1_1 O1_1 1.392(12) Cl1_1 O4_1 1.394(12) Cl1_1 O3_1 1.397(12) Cl1_1 O2_1 1.402(12) Cl1_2 O2_2 1.385(12) Cl1_2 O3_2 1.397(12) Cl1_2 O1_2 1.399(12) Cl1_2 O4_2 1.407(12) Cl1_4 O3_4 1.397(12) Cl1_4 O1_4 1.396(12) Cl1_4 O4_4 1.397(12) Cl1_4 O2_4 1.399(12) Cl1_3 O3_3 1.395(12) Cl1_3 O4_3 1.397(12) Cl1_3 O2_3 1.397(12) Cl1_3 O1_3 1.398(12) C39 C38 1.35(3) C39 H39A 0.9700 C39 H39B 0.9700 C39 H39C 0.9700 C37 C38 1.44(3) C37 H37A 0.9700 C37 H37B 0.9700 C37 H37C 0.9700 C38 O3 1.22(3) 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 H1D O1_2 0.87 2.10 2.89(3) 151.6 . N1 H1D O1_4 0.87 2.31 3.08(3) 148.9 . N5 H5B O2 0.87 2.03 2.62(2) 124.7 . N6 H6B Cl1_1 0.87 2.80 3.67(2) 178.0 . N6 H6B O2_1 0.87 2.50 3.28(5) 149.5 . N6 H6B O4_1 0.87 2.16 2.95(4) 150.6 . N6 H6B Cl1_3 0.87 2.89 3.76(3) 179.7 . N6 H6B O1_3 0.87 2.51 3.30(6) 151.3 . N6 H6B O2_3 0.87 2.30 3.10(4) 151.4 . N10 H10A O3 0.87 1.87 2.74(2) 177.2 . C25 H25A O2_1 0.97 2.73 3.30(5) 118.3 2_675 C25 H25A O2_3 0.97 2.95 3.50(5) 116.6 2_675 C25 H25A O4_3 0.97 2.78 3.44(5) 125.9 2_675 C26 H26A N4 0.94 2.66 3.49(3) 147.4 2_675 C26 H26A N5 0.94 2.51 3.45(3) 176.8 2_675