#------------------------------------------------------------------------------ #$Date: 2016-04-05 18:07:57 +0300 (Tue, 05 Apr 2016) $ #$Revision: 181581 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/18/1541898.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_1541898 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),1.25(C3 H6 O)' _chemical_formula_sum 'C39.75 H37.5 Cl2 Fe N10 O11.25' _chemical_formula_weight 962.05 _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 _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 114.290(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.165(5) _cell_length_b 21.596(8) _cell_length_c 15.414(6) _cell_measurement_reflns_used 1221 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 24.6 _cell_measurement_theta_min 2.68 _cell_volume 4298(3) _computing_cell_refinement 'SAINT V8.27B(Bruker, 2012)' _computing_data_collection 'Apex2 v2012.10-0 (Bruker, 2012)' _computing_data_reduction SAINT _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994) ShelXle Rev 699 (Hubschle, 2011) ; _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.250 _diffrn_measured_fraction_theta_max 0.261 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_orient_matrix_type 'Sparks (1982)' _diffrn_orient_matrix_UB_11 -0.04852 _diffrn_orient_matrix_UB_12 0.01369 _diffrn_orient_matrix_UB_13 0.02844 _diffrn_orient_matrix_UB_21 0.01050 _diffrn_orient_matrix_UB_22 -0.04028 _diffrn_orient_matrix_UB_23 0.03475 _diffrn_orient_matrix_UB_31 0.05945 _diffrn_orient_matrix_UB_32 0.01829 _diffrn_orient_matrix_UB_33 0.05523 _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 0.0232 _diffrn_reflns_av_unetI/netI 0.0443 _diffrn_reflns_Laue_measured_fraction_full 0.250 _diffrn_reflns_Laue_measured_fraction_max 0.261 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 4017 _diffrn_reflns_point_group_measured_fraction_full 0.250 _diffrn_reflns_point_group_measured_fraction_max 0.261 _diffrn_reflns_theta_full 27.706 _diffrn_reflns_theta_max 28.046 _diffrn_reflns_theta_min 2.681 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Sheldrick, 2012)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.487 _exptl_crystal_description block _exptl_crystal_F_000 1984 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.309 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 580 _refine_ls_number_reflns 2103 _refine_ls_number_restraints 904 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0771 _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^)+(0.1345P)^2^+5.4453P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2095 _refine_ls_wR_factor_ref 0.2322 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1487 _reflns_number_total 2103 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage2_Initial _cod_depositor_comments 'Adding full bibliography for 1541896--1541904.cif.' _cod_original_formula_sum 'C39.75 H37.50 Cl2 Fe N10 O11.25' _cod_database_code 1541898 _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 ; Initial.res created by SHELXL-2014/7 TITL samp1 in P2(1)/n Sample folder: srj128c5 CELL 0.77490 14.1652 21.5960 15.4141 90.000 114.290 90.000 ZERR 4.00 0.0054 0.0083 0.0059 0.000 0.0041 0.000 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 159 150 40 45 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 RIGU ISOR O4_4 L.S. 200 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 0.134500 5.445300 FVAR 0.12234 0.51287 0.55311 FE1 6 0.424342 0.265126 0.602665 11.00000 0.02901 0.02451 = 0.02349 -0.00044 0.01120 0.00154 O1 4 0.278830 0.343482 0.957088 11.00000 0.18616 0.09221 = 0.09467 -0.01773 0.10462 0.01070 O2 4 0.505510 0.176919 0.320526 11.00000 0.09459 0.05355 = 0.07787 -0.00730 0.05965 -0.00247 O3 4 0.664200 0.122842 0.922451 11.00000 0.08079 0.07178 = 0.08022 -0.01187 0.02913 -0.02612 N1 3 0.363093 0.238267 0.772775 11.00000 0.03705 0.04039 = 0.02588 0.00025 0.01611 -0.00360 AFIX 43 H1 2 0.369927 0.198211 0.777195 11.00000 -1.20000 AFIX 0 N2 3 0.379442 0.273572 0.709102 11.00000 0.03126 0.03542 = 0.02721 -0.00354 0.01232 -0.00024 N3 3 0.400309 0.352928 0.599431 11.00000 0.03278 0.02590 = 0.03236 -0.00483 0.01228 0.00162 N4 3 0.457988 0.289173 0.495986 11.00000 0.03587 0.03470 = 0.02957 -0.00119 0.01513 -0.00101 N5 3 0.486060 0.261087 0.432928 11.00000 0.04556 0.03620 = 0.03442 0.00066 0.02255 -0.00058 AFIX 43 H5 2 0.496538 0.221412 0.432561 11.00000 -1.20000 AFIX 0 N6 3 0.645761 0.307115 0.731056 11.00000 0.03101 0.03852 = 0.03126 0.00235 0.00791 0.00018 AFIX 43 H6 2 0.634624 0.346780 0.730054 11.00000 -1.20000 AFIX 0 N7 3 0.572696 0.264898 0.687015 11.00000 0.03155 0.02907 = 0.03697 -0.00177 0.01431 0.00202 N8 3 0.456419 0.177519 0.608086 11.00000 0.03896 0.02813 = 0.03640 -0.00049 0.02120 0.00519 N9 3 0.285928 0.230241 0.517592 11.00000 0.02690 0.03932 = 0.02696 0.00109 0.00915 -0.00117 N10 3 0.190840 0.253793 0.469675 11.00000 0.02497 0.05661 = 0.03734 -0.00533 0.01288 0.00325 AFIX 43 H10 2 0.174411 0.292860 0.464084 11.00000 -1.20000 AFIX 0 C1 1 0.252754 0.379281 1.022086 11.00000 0.28886 0.10116 = 0.15008 -0.02123 0.17619 0.01972 AFIX 137 H1A 2 0.209218 0.413801 0.988563 11.00000 -1.50000 H1B 2 0.315588 0.394854 1.072559 11.00000 -1.50000 H1C 2 0.215755 0.353487 1.049253 11.00000 -1.50000 AFIX 0 C2 1 0.282290 0.280587 0.969364 11.00000 0.06922 0.09324 = 0.05814 -0.01291 0.04246 -0.00005 C3 1 0.258251 0.257670 1.039424 11.00000 0.09327 0.11064 = 0.06471 -0.00524 0.05257 -0.00215 AFIX 43 H3A 2 0.240110 0.283501 1.079239 11.00000 -1.20000 AFIX 0 C4 1 0.261969 0.194148 1.048893 11.00000 0.07119 0.11275 = 0.06581 -0.00054 0.04187 -0.00484 AFIX 43 H4A 2 0.249984 0.176251 1.099038 11.00000 -1.20000 AFIX 0 C5 1 0.283338 0.154895 0.985270 11.00000 0.08114 0.09114 = 0.06319 0.00855 0.04457 -0.00521 AFIX 43 H5A 2 0.279565 0.111640 0.989859 11.00000 -1.20000 AFIX 0 C6 1 0.309656 0.181006 0.916766 11.00000 0.07341 0.07848 = 0.05172 -0.00382 0.03922 -0.00687 AFIX 43 H6A 2 0.328782 0.155643 0.877096 11.00000 -1.20000 AFIX 0 C7 1 0.307852 0.244941 0.906469 11.00000 0.03971 0.07571 = 0.03837 -0.00344 0.02209 -0.00480 C8 1 0.333595 0.275312 0.830615 11.00000 0.03863 0.04964 = 0.03843 -0.00976 0.02139 -0.00239 C9 1 0.333016 0.335498 0.803939 11.00000 0.05710 0.04824 = 0.04403 -0.01367 0.03048 -0.00491 AFIX 43 H9A 2 0.317805 0.370812 0.831484 11.00000 -1.20000 AFIX 0 C10 1 0.360524 0.332958 0.725227 11.00000 0.03212 0.03666 = 0.03847 -0.00513 0.01539 0.00071 C11 1 0.372541 0.379920 0.662885 11.00000 0.03520 0.03080 = 0.03687 -0.00652 0.01430 0.00071 C12 1 0.356682 0.442638 0.662663 11.00000 0.04452 0.03311 = 0.06201 -0.00327 0.02014 0.00064 AFIX 43 H12A 2 0.337277 0.460621 0.708430 11.00000 -1.20000 AFIX 0 C13 1 0.369760 0.479975 0.593069 11.00000 0.05803 0.02865 = 0.06590 -0.00255 0.02530 0.00078 AFIX 43 H13A 2 0.357783 0.522894 0.590129 11.00000 -1.20000 AFIX 0 C14 1 0.400085 0.451428 0.531234 11.00000 0.04200 0.03231 = 0.05827 0.00259 0.01697 0.00203 AFIX 43 H14A 2 0.409888 0.475095 0.484422 11.00000 -1.20000 AFIX 0 C15 1 0.417182 0.388504 0.534559 11.00000 0.03578 0.02977 = 0.03757 -0.00038 0.01217 -0.00085 C16 1 0.448363 0.349144 0.471707 11.00000 0.03127 0.03429 = 0.02945 0.00184 0.00929 -0.00284 C17 1 0.474222 0.358404 0.393511 11.00000 0.04596 0.04527 = 0.03477 0.00792 0.01476 -0.00124 AFIX 43 H17A 2 0.475700 0.396371 0.364274 11.00000 -1.20000 AFIX 0 C18 1 0.496575 0.301671 0.368747 11.00000 0.03716 0.04687 = 0.03063 0.00255 0.01503 -0.00672 C19 1 0.524887 0.280547 0.292770 11.00000 0.04548 0.05567 = 0.03606 0.00022 0.02124 -0.00458 C20 1 0.547531 0.326898 0.239567 11.00000 0.08300 0.07193 = 0.04009 0.00522 0.03364 -0.00686 AFIX 43 H20A 2 0.542768 0.368771 0.253930 11.00000 -1.20000 AFIX 0 C21 1 0.576985 0.311742 0.165730 11.00000 0.10970 0.08664 = 0.05995 -0.00972 0.05522 -0.02425 AFIX 43 H21A 2 0.596347 0.342410 0.132929 11.00000 -1.20000 AFIX 0 C22 1 0.576304 0.251538 0.143979 11.00000 0.08671 0.08604 = 0.05671 -0.01148 0.04350 -0.02337 AFIX 43 H22A 2 0.591109 0.241093 0.091688 11.00000 -1.20000 AFIX 0 C23 1 0.555008 0.203084 0.193927 11.00000 0.08496 0.07521 = 0.06753 -0.01709 0.05614 -0.01313 AFIX 43 H23A 2 0.558603 0.161564 0.177232 11.00000 -1.20000 AFIX 0 C24 1 0.528366 0.218140 0.268997 11.00000 0.05315 0.06326 = 0.04975 -0.00770 0.02803 -0.00117 C25 1 0.507240 0.114293 0.298986 11.00000 0.23868 0.05823 = 0.17832 -0.01257 0.17626 -0.00402 AFIX 137 H25A 2 0.517790 0.089597 0.354789 11.00000 -1.50000 H25B 2 0.563267 0.106723 0.279605 11.00000 -1.50000 H25C 2 0.441865 0.103019 0.247588 11.00000 -1.50000 AFIX 0 C26 1 0.739747 0.279932 0.777611 11.00000 0.03364 0.04941 = 0.04171 0.00399 0.01622 0.00156 AFIX 43 H26A 2 0.801964 0.300610 0.813923 11.00000 -1.20000 AFIX 0 C27 1 0.728751 0.218372 0.762969 11.00000 0.03312 0.04749 = 0.05257 0.00745 0.01414 0.01103 AFIX 43 H27A 2 0.780231 0.187741 0.786649 11.00000 -1.20000 AFIX 0 C28 1 0.621433 0.210045 0.703447 11.00000 0.03467 0.03578 = 0.03316 0.00864 0.01687 0.00784 C29 1 0.555616 0.158489 0.658558 11.00000 0.03907 0.02859 = 0.04037 0.00488 0.02356 0.00970 C30 1 0.579835 0.097011 0.656311 11.00000 0.06604 0.03615 = 0.05506 0.00697 0.02697 0.01532 AFIX 43 H30A 2 0.648045 0.083510 0.691935 11.00000 -1.20000 AFIX 0 C31 1 0.504842 0.054367 0.602038 11.00000 0.07436 0.03816 = 0.07523 -0.00607 0.02957 0.01307 AFIX 43 H31A 2 0.522231 0.012543 0.600069 11.00000 -1.20000 AFIX 0 C32 1 0.401106 0.075377 0.549476 11.00000 0.07169 0.03618 = 0.05508 0.00001 0.03529 0.00862 AFIX 43 H32A 2 0.348902 0.047771 0.512108 11.00000 -1.20000 AFIX 0 C33 1 0.379305 0.137619 0.554963 11.00000 0.04221 0.03334 = 0.04163 -0.00131 0.02134 -0.00090 C34 1 0.281234 0.168612 0.508337 11.00000 0.03231 0.04285 = 0.03315 -0.00315 0.01492 -0.00291 C35 1 0.178432 0.149583 0.453293 11.00000 0.04307 0.06478 = 0.05054 -0.01309 0.01984 -0.01172 AFIX 43 H35A 2 0.152548 0.109280 0.435742 11.00000 -1.20000 AFIX 0 C36 1 0.124865 0.205804 0.431487 11.00000 0.03664 0.06751 = 0.04546 -0.00798 0.01517 -0.01038 AFIX 43 H36A 2 0.053165 0.209815 0.395415 11.00000 -1.20000 AFIX 0 C37 1 0.619606 0.082287 0.940081 11.00000 0.03839 0.05481 = 0.06895 0.00456 0.00992 0.00011 C38 1 0.616654 0.019445 0.898503 11.00000 0.07477 0.06295 = 0.08892 -0.00206 0.02816 -0.00622 AFIX 137 H38A 2 0.686523 0.006496 0.910563 11.00000 -1.50000 H38B 2 0.575113 0.020847 0.830401 11.00000 -1.50000 H38C 2 0.586409 -0.009808 0.927549 11.00000 -1.50000 AFIX 0 C39 1 0.565363 0.086377 1.005074 11.00000 0.09016 0.09320 = 0.10229 0.01317 0.04963 0.01204 AFIX 137 H39A 2 0.569685 0.128440 1.028478 11.00000 -1.50000 H39B 2 0.597986 0.058396 1.058352 11.00000 -1.50000 H39C 2 0.493223 0.074949 0.970561 11.00000 -1.50000 AFIX 0 PART -1 O4 4 -0.049544 0.062215 0.464538 10.25000 0.10161 C40 1 -0.027850 0.009893 0.464841 10.25000 0.08052 C41 1 0.045147 -0.030089 0.442345 10.25000 0.10554 AFIX 33 H41A 2 0.034407 -0.073086 0.454102 10.25000 -1.50000 H41B 2 0.032566 -0.024872 0.375980 10.25000 -1.50000 H41C 2 0.115884 -0.018281 0.482340 10.25000 -1.50000 AFIX 0 C42 1 -0.020432 -0.003385 0.562589 10.25000 0.10670 AFIX 33 H42A 2 -0.002243 -0.046533 0.578041 10.25000 -1.50000 H42B 2 0.032390 0.022762 0.608258 10.25000 -1.50000 H42C 2 -0.086625 0.004997 0.564915 10.25000 -1.50000 AFIX 0 PART 1 RESI 1 CLO4 CL1 5 0.695710 0.465736 0.745621 21.00000 0.06416 O1 4 0.613401 0.431994 0.754227 21.00000 0.06434 O2 4 0.788305 0.457262 0.828162 21.00000 0.07895 O3 4 0.669245 0.530087 0.737837 21.00000 0.10066 O4 4 0.704997 0.447399 0.661705 21.00000 0.14224 PART 2 RESI 2 CLO4 CL1 5 0.693885 0.474733 0.764996 -21.00000 0.04282 O1 4 0.602147 0.439641 0.740666 -21.00000 0.15799 O2 4 0.723493 0.503416 0.854786 -21.00000 0.14443 O3 4 0.682646 0.519149 0.693515 -21.00000 0.13436 O4 4 0.775903 0.433840 0.770536 -21.00000 0.11561 PART 1 RESI 3 CLO4 CL1 5 0.306545 0.052350 0.736535 31.00000 0.05903 O1 4 0.255214 0.057978 0.798405 31.00000 0.09323 O2 4 0.366739 -0.002648 0.760891 31.00000 0.09964 O3 4 0.232928 0.050354 0.640555 31.00000 0.10592 O4 4 0.371718 0.104909 0.749997 31.00000 0.07091 PART 2 RESI 4 CLO4 CL1 5 0.323675 0.051132 0.755125 -31.00000 0.06354 O1 4 0.330846 0.035342 0.847040 -31.00000 0.09065 O2 4 0.347679 -0.001359 0.712494 -31.00000 0.08915 O3 4 0.220153 0.069564 0.697832 -31.00000 0.10892 O4 4 0.394123 0.100241 0.764710 -31.00000 0.06406 PART 0 HKLF 4 REM samp1 in P2(1)/n Sample folder: srj128c5 REM R1 = 0.0771 for 1487 Fo > 4sig(Fo) and 0.1070 for all 2103 data REM 580 parameters refined using 904 restraints END WGHT 0.1491 11.9866 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 N6 O4_2 HTAB N10 O3_$1 EQIV $2 -x+1, -y+1, -z+2 HTAB_2 C1_0 O2_$2 HTAB C9 O1 EQIV $3 x+1/2, -y+1/2, z+1/2 HTAB C9 O4_$3 EQIV $4 -x+1/2, y+1/2, -z+3/2 HTAB_3 C12_0 O1_$4 EQIV $5 -x+1, -y+1, -z+1 HTAB_2 C14_0 O3_$5 HTAB_1 C17_0 O3_$5 EQIV $6 -x+1, -y, -z+1 HTAB_3 C25_0 O2_$6 HTAB_4 C25_0 O2_$6 HTAB_2 C25_0 O4_$1 EQIV $7 -x+3/2, y-1/2, -z+3/2 HTAB_1 C30_0 O3_$7 HTAB_1 C32_0 O2_$1 HTAB_2 C32_0 O2_$1 HTAB_1 C38_0 O4_$7 EQIV $8 -x+1, -y, -z+2 HTAB_4 C39_0 O1_$8 HTAB C39 O1_4 REM Highest difference peak 0.309, deepest hole -0.327, 1-sigma level 0.057 Q1 1 0.1995 0.0548 0.7453 11.00000 0.05 0.31 Q2 1 0.3764 -0.0044 0.8261 11.00000 0.05 0.31 Q3 1 0.6603 0.4605 0.6615 11.00000 0.05 0.28 Q4 1 0.6431 0.4625 0.8250 11.00000 0.05 0.25 Q5 1 0.2837 -0.0058 0.6658 11.00000 0.05 0.25 Q6 1 0.6284 0.0515 0.7201 11.00000 0.05 0.24 Q7 1 0.4977 0.0493 0.7588 11.00000 0.05 0.23 Q8 1 0.3249 0.1223 0.6987 11.00000 0.05 0.22 Q9 1 0.7521 0.4746 0.8615 11.00000 0.05 0.22 Q10 1 0.2434 0.0869 0.6504 11.00000 0.05 0.21 Q11 1 0.5363 0.0643 0.1964 11.00000 0.05 0.21 Q12 1 0.7502 0.4790 0.7080 11.00000 0.05 0.20 Q13 1 -0.0459 -0.0211 0.5788 11.00000 0.05 0.20 Q14 1 -0.0199 0.0325 0.5102 11.00000 0.05 0.20 Q15 1 0.4769 -0.0381 0.8457 11.00000 0.05 0.19 Q16 1 0.5016 0.3534 0.6367 11.00000 0.05 0.19 Q17 1 0.3603 0.4362 1.0648 11.00000 0.05 0.18 Q18 1 0.4412 0.4907 0.6887 11.00000 0.05 0.18 Q19 1 -0.0684 0.0469 0.4245 11.00000 0.05 0.18 Q20 1 0.3880 0.3579 0.4553 11.00000 0.05 0.18 ; _shelx_res_checksum 93369 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 0.42434(12) 0.26513(9) 0.60267(10) 0.0255(5) Uani 1 1 d . U . . . O1 O 0.2788(14) 0.3435(9) 0.9571(11) 0.109(6) Uani 1 1 d . U . . . O2 O 0.5055(10) 0.1769(7) 0.3205(9) 0.067(4) Uani 1 1 d . U . . . O3 O 0.6642(10) 0.1228(7) 0.9225(9) 0.079(4) Uani 1 1 d D U . . . N1 N 0.3631(7) 0.2383(5) 0.7728(6) 0.033(2) Uani 1 1 d . U . . . H1 H 0.3699 0.1982 0.7772 0.040 Uiso 1 1 calc R U . . . N2 N 0.3794(7) 0.2736(6) 0.7091(7) 0.031(2) Uani 1 1 d . U . . . N3 N 0.4003(8) 0.3529(5) 0.5994(7) 0.031(2) Uani 1 1 d . U . . . N4 N 0.4580(8) 0.2892(6) 0.4960(7) 0.033(2) Uani 1 1 d . U . . . N5 N 0.4861(8) 0.2611(5) 0.4329(7) 0.037(2) Uani 1 1 d . U . . . H5 H 0.4965 0.2214 0.4326 0.044 Uiso 1 1 calc R U . . . N6 N 0.6458(7) 0.3071(5) 0.7311(7) 0.035(2) Uani 1 1 d . U . . . H6 H 0.6346 0.3468 0.7301 0.042 Uiso 1 1 calc R U . . . N7 N 0.5727(8) 0.2649(5) 0.6870(7) 0.032(2) Uani 1 1 d . U . . . N8 N 0.4564(8) 0.1775(5) 0.6081(7) 0.033(2) Uani 1 1 d . U . . . N9 N 0.2859(7) 0.2302(7) 0.5176(7) 0.032(2) Uani 1 1 d . U . . . N10 N 0.1908(7) 0.2538(6) 0.4697(8) 0.040(3) Uani 1 1 d . U . . . H10 H 0.1744 0.2929 0.4641 0.048 Uiso 1 1 calc R U . . . C1 C 0.253(2) 0.3793(11) 1.0221(18) 0.152(13) Uani 1 1 d . U . . . H1A H 0.2092 0.4138 0.9886 0.228 Uiso 1 1 calc R U . . . H1B H 0.3156 0.3949 1.0726 0.228 Uiso 1 1 calc R U . . . H1C H 0.2158 0.3535 1.0493 0.228 Uiso 1 1 calc R U . . . C2 C 0.2823(14) 0.2806(13) 0.9694(13) 0.068(5) Uani 1 1 d . U . . . C3 C 0.2583(16) 0.2577(13) 1.0394(14) 0.083(6) Uani 1 1 d . U . . . H3A H 0.2401 0.2835 1.0792 0.099 Uiso 1 1 calc R U . . . C4 C 0.2620(14) 0.1941(13) 1.0489(14) 0.079(6) Uani 1 1 d . U . . . H4A H 0.2500 0.1763 1.0990 0.094 Uiso 1 1 calc R U . . . C5 C 0.2833(14) 0.1549(10) 0.9853(12) 0.074(5) Uani 1 1 d . U . . . H5A H 0.2796 0.1116 0.9899 0.088 Uiso 1 1 calc R U . . . C6 C 0.3097(13) 0.1810(11) 0.9168(11) 0.063(5) Uani 1 1 d . U . . . H6A H 0.3288 0.1556 0.8771 0.076 Uiso 1 1 calc R U . . . C7 C 0.3079(11) 0.2449(10) 0.9065(10) 0.049(4) Uani 1 1 d . U . . . C8 C 0.3336(10) 0.2753(8) 0.8306(9) 0.040(3) Uani 1 1 d . U . . . C9 C 0.3330(11) 0.3355(8) 0.8039(10) 0.047(3) Uani 1 1 d . U . . . H9A H 0.3178 0.3708 0.8315 0.056 Uiso 1 1 calc R U . . . C10 C 0.3605(9) 0.3330(7) 0.7252(9) 0.035(3) Uani 1 1 d . U . . . C11 C 0.3725(10) 0.3799(8) 0.6629(9) 0.034(3) Uani 1 1 d . U . . . C12 C 0.3567(10) 0.4426(8) 0.6627(11) 0.047(3) Uani 1 1 d . U . . . H12A H 0.3373 0.4606 0.7084 0.057 Uiso 1 1 calc R U . . . C13 C 0.3698(11) 0.4800(7) 0.5931(10) 0.051(3) Uani 1 1 d . U . . . H13A H 0.3578 0.5229 0.5901 0.061 Uiso 1 1 calc R U . . . C14 C 0.4001(10) 0.4514(8) 0.5312(11) 0.045(3) Uani 1 1 d . U . . . H14A H 0.4099 0.4751 0.4844 0.054 Uiso 1 1 calc R U . . . C15 C 0.4172(10) 0.3885(8) 0.5346(9) 0.035(3) Uani 1 1 d . U . . . C16 C 0.4484(9) 0.3491(7) 0.4717(9) 0.033(3) Uani 1 1 d . U . . . C17 C 0.4742(10) 0.3584(7) 0.3935(9) 0.043(3) Uani 1 1 d . U . . . H17A H 0.4757 0.3964 0.3643 0.051 Uiso 1 1 calc R U . . . C18 C 0.4966(9) 0.3017(7) 0.3687(8) 0.038(3) Uani 1 1 d . U . . . C19 C 0.5249(11) 0.2805(8) 0.2928(9) 0.044(3) Uani 1 1 d . U . . . C20 C 0.5475(13) 0.3269(8) 0.2396(11) 0.062(4) Uani 1 1 d . U . . . H20A H 0.5428 0.3688 0.2539 0.075 Uiso 1 1 calc R U . . . C21 C 0.5770(15) 0.3117(11) 0.1657(13) 0.079(6) Uani 1 1 d . U . . . H21A H 0.5963 0.3424 0.1329 0.094 Uiso 1 1 calc R U . . . C22 C 0.5763(13) 0.2515(11) 0.1440(13) 0.072(5) Uani 1 1 d . U . . . H22A H 0.5911 0.2411 0.0917 0.086 Uiso 1 1 calc R U . . . C23 C 0.5550(14) 0.2031(9) 0.1939(12) 0.068(5) Uani 1 1 d . U . . . H23A H 0.5586 0.1616 0.1772 0.081 Uiso 1 1 calc R U . . . C24 C 0.5284(12) 0.2181(10) 0.2690(11) 0.053(4) Uani 1 1 d . U . . . C25 C 0.507(2) 0.1143(12) 0.299(2) 0.129(12) Uani 1 1 d . U . . . H25A H 0.5178 0.0896 0.3548 0.193 Uiso 1 1 calc R U . . . H25B H 0.5633 0.1067 0.2796 0.193 Uiso 1 1 calc R U . . . H25C H 0.4419 0.1030 0.2476 0.193 Uiso 1 1 calc R U . . . C26 C 0.7397(10) 0.2799(8) 0.7776(9) 0.041(3) Uani 1 1 d . U . . . H26A H 0.8020 0.3006 0.8139 0.050 Uiso 1 1 calc R U . . . C27 C 0.7288(10) 0.2184(9) 0.7630(10) 0.046(4) Uani 1 1 d . U . . . H27A H 0.7802 0.1877 0.7866 0.055 Uiso 1 1 calc R U . . . C28 C 0.6214(10) 0.2100(7) 0.7034(9) 0.034(3) Uani 1 1 d . U . . . C29 C 0.5556(10) 0.1585(8) 0.6586(9) 0.034(3) Uani 1 1 d . U . . . C30 C 0.5798(12) 0.0970(8) 0.6563(11) 0.052(4) Uani 1 1 d . U . . . H30A H 0.6480 0.0835 0.6919 0.062 Uiso 1 1 calc R U . . . C31 C 0.5048(12) 0.0544(8) 0.6020(12) 0.063(4) Uani 1 1 d . U . . . H31A H 0.5222 0.0125 0.6001 0.076 Uiso 1 1 calc R U . . . C32 C 0.4011(12) 0.0754(8) 0.5495(11) 0.051(4) Uani 1 1 d . U . . . H32A H 0.3489 0.0478 0.5121 0.062 Uiso 1 1 calc R U . . . C33 C 0.3793(10) 0.1376(8) 0.5550(9) 0.038(3) Uani 1 1 d . U . . . C34 C 0.2812(10) 0.1686(9) 0.5083(9) 0.036(3) Uani 1 1 d . U . . . C35 C 0.1784(11) 0.1496(9) 0.4533(10) 0.053(3) Uani 1 1 d . U . . . H35A H 0.1525 0.1093 0.4357 0.063 Uiso 1 1 calc R U . . . C36 C 0.1249(11) 0.2058(8) 0.4315(10) 0.050(3) Uani 1 1 d . U . . . H36A H 0.0532 0.2098 0.3954 0.061 Uiso 1 1 calc R U . . . C37 C 0.6196(12) 0.0823(10) 0.9401(11) 0.058(4) Uani 1 1 d D U . . . C38 C 0.6167(14) 0.0194(9) 0.8985(13) 0.077(5) Uani 1 1 d D U . . . H38A H 0.6865 0.0065 0.9106 0.116 Uiso 1 1 calc R U . . . H38B H 0.5751 0.0208 0.8304 0.116 Uiso 1 1 calc R U . . . H38C H 0.5864 -0.0098 0.9275 0.116 Uiso 1 1 calc R U . . . C39 C 0.5654(15) 0.0864(10) 1.0051(14) 0.092(6) Uani 1 1 d D U . . . H39A H 0.5697 0.1284 1.0285 0.138 Uiso 1 1 calc R U . . . H39B H 0.5980 0.0584 1.0584 0.138 Uiso 1 1 calc R U . . . H39C H 0.4932 0.0749 0.9706 0.138 Uiso 1 1 calc R U . . . O4 O -0.050(4) 0.062(3) 0.465(5) 0.102(19) Uiso 0.25 1 d D . P A -1 C40 C -0.028(6) 0.010(3) 0.465(5) 0.08(2) Uiso 0.25 1 d D . P A -1 C41 C 0.045(7) -0.030(5) 0.442(7) 0.11(4) Uiso 0.25 1 d D . P A -1 H41A H 0.0344 -0.0731 0.4541 0.158 Uiso 0.25 1 calc R U P A -1 H41B H 0.0326 -0.0249 0.3760 0.158 Uiso 0.25 1 calc R U P A -1 H41C H 0.1159 -0.0183 0.4823 0.158 Uiso 0.25 1 calc R U P A -1 C42 C -0.020(9) -0.003(6) 0.563(5) 0.11(3) Uiso 0.25 1 d D . P A -1 H42A H -0.0022 -0.0465 0.5780 0.160 Uiso 0.25 1 calc R U P A -1 H42B H 0.0324 0.0228 0.6083 0.160 Uiso 0.25 1 calc R U P A -1 H42C H -0.0866 0.0050 0.5649 0.160 Uiso 0.25 1 calc R U P A -1 Cl1_1 Cl 0.6957(8) 0.4657(6) 0.7456(8) 0.064(3) Uiso 0.51(2) 1 d D . P B 1 O1_1 O 0.6134(15) 0.4320(11) 0.7542(16) 0.064(9) Uiso 0.51(2) 1 d D . P B 1 O2_1 O 0.7883(12) 0.4573(11) 0.8282(12) 0.079(9) Uiso 0.51(2) 1 d D . P B 1 O3_1 O 0.6692(19) 0.5301(7) 0.738(2) 0.101(11) Uiso 0.51(2) 1 d D . P B 1 O4_1 O 0.705(2) 0.4474(13) 0.6617(14) 0.142(16) Uiso 0.51(2) 1 d D . P B 1 Cl1_2 Cl 0.6939(6) 0.4747(4) 0.7650(7) 0.043(3) Uiso 0.49(2) 1 d D . P B 2 O1_2 O 0.6021(16) 0.4396(13) 0.741(2) 0.16(3) Uiso 0.49(2) 1 d D . P B 2 O2_2 O 0.723(2) 0.5034(13) 0.8548(13) 0.144(16) Uiso 0.49(2) 1 d D . P B 2 O3_2 O 0.683(2) 0.5191(12) 0.6935(17) 0.134(15) Uiso 0.49(2) 1 d D . P B 2 O4_2 O 0.7759(16) 0.4338(10) 0.771(2) 0.116(12) Uiso 0.49(2) 1 d D . P B 2 Cl1_3 Cl 0.3065(8) 0.0524(5) 0.7365(8) 0.059(3) Uiso 0.55(3) 1 d D . P C 1 O1_3 O 0.2552(17) 0.0580(10) 0.7984(15) 0.093(10) Uiso 0.55(3) 1 d D . P C 1 O2_3 O 0.3667(17) -0.0026(8) 0.7609(18) 0.100(9) Uiso 0.55(3) 1 d D . P C 1 O3_3 O 0.2329(14) 0.0504(11) 0.6406(11) 0.106(10) Uiso 0.55(3) 1 d D . P C 1 O4_3 O 0.3717(17) 0.1049(9) 0.7500(18) 0.071(10) Uiso 0.55(3) 1 d D . P C 1 Cl1_4 Cl 0.3237(11) 0.0511(6) 0.7551(11) 0.064(5) Uiso 0.45(3) 1 d D . P C 2 O1_4 O 0.331(2) 0.0353(12) 0.8470(13) 0.091(11) Uiso 0.45(3) 1 d D . P C 2 O2_4 O 0.348(2) -0.0014(10) 0.7125(18) 0.089(10) Uiso 0.45(3) 1 d D . P C 2 O3_4 O 0.2202(13) 0.0696(12) 0.698(2) 0.109(13) Uiso 0.45(3) 1 d D . P C 2 O4_4 O 0.3941(19) 0.1002(11) 0.765(2) 0.064(11) Uiso 0.45(3) 1 d D . P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0290(10) 0.0245(11) 0.0235(7) -0.0004(7) 0.0112(6) 0.0015(8) O1 0.186(16) 0.092(11) 0.095(11) -0.018(7) 0.105(11) 0.011(9) O2 0.095(9) 0.054(9) 0.078(7) -0.007(6) 0.060(7) -0.002(6) O3 0.081(9) 0.072(9) 0.080(8) -0.012(6) 0.029(6) -0.026(7) N1 0.037(5) 0.040(6) 0.026(4) 0.000(4) 0.016(4) -0.004(4) N2 0.031(5) 0.035(5) 0.027(4) -0.004(3) 0.012(3) 0.000(4) N3 0.033(5) 0.026(5) 0.032(4) -0.005(3) 0.012(3) 0.002(4) N4 0.036(5) 0.035(6) 0.030(4) -0.001(3) 0.015(3) -0.001(4) N5 0.046(6) 0.036(5) 0.034(4) 0.001(4) 0.023(4) -0.001(4) N6 0.031(5) 0.039(6) 0.031(5) 0.002(4) 0.008(3) 0.000(4) N7 0.032(4) 0.029(5) 0.037(4) -0.002(4) 0.014(3) 0.002(3) N8 0.039(4) 0.028(5) 0.036(4) 0.000(3) 0.021(3) 0.005(3) N9 0.027(4) 0.039(6) 0.027(4) 0.001(4) 0.009(3) -0.001(4) N10 0.025(5) 0.057(7) 0.037(5) -0.005(4) 0.013(3) 0.003(4) C1 0.29(4) 0.101(17) 0.15(2) -0.021(14) 0.18(3) 0.020(17) C2 0.069(10) 0.093(11) 0.058(8) -0.013(7) 0.042(8) 0.000(8) C3 0.093(14) 0.111(13) 0.065(10) -0.005(8) 0.053(10) -0.002(10) C4 0.071(11) 0.113(13) 0.066(9) -0.001(8) 0.042(8) -0.005(10) C5 0.081(12) 0.091(11) 0.063(9) 0.009(7) 0.045(9) -0.005(8) C6 0.073(11) 0.078(10) 0.052(8) -0.004(6) 0.039(8) -0.007(8) C7 0.040(7) 0.076(9) 0.038(6) -0.003(5) 0.022(5) -0.005(7) C8 0.039(7) 0.050(7) 0.038(5) -0.010(4) 0.021(5) -0.002(6) C9 0.057(8) 0.048(7) 0.044(6) -0.014(5) 0.030(6) -0.005(6) C10 0.032(6) 0.037(6) 0.038(5) -0.005(4) 0.015(4) 0.001(5) C11 0.035(7) 0.031(6) 0.037(5) -0.007(4) 0.014(4) 0.001(5) C12 0.045(8) 0.033(7) 0.062(7) -0.003(5) 0.020(6) 0.001(6) C13 0.058(9) 0.029(7) 0.066(7) -0.003(5) 0.025(6) 0.001(6) C14 0.042(8) 0.032(7) 0.058(7) 0.003(5) 0.017(5) 0.002(6) C15 0.036(6) 0.030(6) 0.038(5) 0.000(4) 0.012(4) -0.001(5) C16 0.031(6) 0.034(6) 0.029(4) 0.002(4) 0.009(4) -0.003(4) C17 0.046(7) 0.045(7) 0.035(5) 0.008(4) 0.015(5) -0.001(5) C18 0.037(6) 0.047(6) 0.031(5) 0.003(4) 0.015(4) -0.007(5) C19 0.045(7) 0.056(8) 0.036(5) 0.000(4) 0.021(5) -0.005(6) C20 0.083(10) 0.072(9) 0.040(7) 0.005(6) 0.034(7) -0.007(7) C21 0.110(14) 0.087(12) 0.060(9) -0.010(7) 0.055(10) -0.024(9) C22 0.087(12) 0.086(12) 0.057(9) -0.011(7) 0.044(8) -0.023(9) C23 0.085(12) 0.075(11) 0.068(8) -0.017(7) 0.056(9) -0.013(8) C24 0.053(9) 0.063(8) 0.050(7) -0.008(5) 0.028(6) -0.001(6) C25 0.24(3) 0.058(12) 0.18(3) -0.013(9) 0.18(3) -0.004(10) C26 0.034(5) 0.049(8) 0.042(6) 0.004(5) 0.016(4) 0.002(5) C27 0.033(6) 0.047(8) 0.053(7) 0.007(5) 0.014(4) 0.011(5) C28 0.035(5) 0.036(5) 0.033(5) 0.009(4) 0.017(4) 0.008(4) C29 0.039(5) 0.029(6) 0.040(5) 0.005(4) 0.024(4) 0.010(4) C30 0.066(8) 0.036(7) 0.055(7) 0.007(5) 0.027(6) 0.015(5) C31 0.074(8) 0.038(7) 0.075(9) -0.006(6) 0.030(6) 0.013(6) C32 0.072(7) 0.036(7) 0.055(7) 0.000(5) 0.035(6) 0.009(5) C33 0.042(5) 0.033(6) 0.042(6) -0.001(4) 0.021(4) -0.001(4) C34 0.032(5) 0.043(6) 0.033(5) -0.003(4) 0.015(4) -0.003(4) C35 0.043(6) 0.065(8) 0.051(7) -0.013(5) 0.020(5) -0.012(5) C36 0.037(6) 0.068(8) 0.045(7) -0.008(6) 0.015(4) -0.010(5) C37 0.038(8) 0.055(10) 0.069(9) 0.005(7) 0.010(6) 0.000(7) C38 0.075(11) 0.063(11) 0.089(12) -0.002(8) 0.028(9) -0.006(8) C39 0.090(13) 0.093(16) 0.102(12) 0.013(11) 0.050(11) 0.012(11) 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 N8 176.9(4) N3 Fe1 N4 79.6(4) N8 Fe1 N4 99.3(5) N3 Fe1 N7 98.6(4) N8 Fe1 N7 78.5(5) N4 Fe1 N7 89.6(4) N3 Fe1 N2 79.5(4) N8 Fe1 N2 101.6(4) N4 Fe1 N2 159.1(5) N7 Fe1 N2 94.1(4) N3 Fe1 N9 103.8(5) N8 Fe1 N9 79.1(5) N4 Fe1 N9 93.5(4) N7 Fe1 N9 157.6(5) N2 Fe1 N9 90.9(4) C2 O1 C1 116.4(15) C24 O2 C25 118.6(14) N2 N1 C8 109.4(12) N2 N1 H1 125.3 C8 N1 H1 125.3 N1 N2 C10 107.4(11) N1 N2 Fe1 139.6(9) C10 N2 Fe1 113.0(9) C11 N3 C15 119.2(13) C11 N3 Fe1 121.1(10) C15 N3 Fe1 119.6(9) N5 N4 C16 105.2(10) N5 N4 Fe1 137.5(10) C16 N4 Fe1 117.3(8) N4 N5 C18 112.7(12) N4 N5 H5 123.6 C18 N5 H5 123.6 N7 N6 C26 111.1(13) N7 N6 H6 124.5 C26 N6 H6 124.5 N6 N7 C28 106.0(12) N6 N7 Fe1 136.8(9) C28 N7 Fe1 117.0(10) C29 N8 C33 122.3(13) C29 N8 Fe1 119.2(10) C33 N8 Fe1 118.3(10) C34 N9 N10 108.9(10) C34 N9 Fe1 115.9(8) N10 N9 Fe1 135.1(11) N9 N10 C36 107.8(13) N9 N10 H10 126.1 C36 N10 H10 126.1 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 C3 C2 O1 118(2) C3 C2 C7 125(3) O1 C2 C7 117.1(16) C2 C3 C4 116(2) C2 C3 H3A 122.0 C4 C3 H3A 122.0 C3 C4 C5 122.1(18) C3 C4 H4A 119.0 C5 C4 H4A 119.0 C6 C5 C4 119(2) C6 C5 H5A 120.4 C4 C5 H5A 120.4 C5 C6 C7 119.8(17) C5 C6 H6A 120.1 C7 C6 H6A 120.1 C6 C7 C2 117.8(16) C6 C7 C8 121.4(13) C2 C7 C8 120.8(19) C9 C8 N1 108.8(12) C9 C8 C7 132.4(15) N1 C8 C7 118.7(15) C8 C9 C10 104.6(13) C8 C9 H9A 127.7 C10 C9 H9A 127.7 N2 C10 C9 109.8(13) N2 C10 C11 117.0(12) C9 C10 C11 133.3(14) N3 C11 C12 121.9(13) N3 C11 C10 109.3(14) C12 C11 C10 128.8(12) C11 C12 C13 119.5(14) C11 C12 H12A 120.3 C13 C12 H12A 120.3 C14 C13 C12 117.1(16) C14 C13 H13A 121.4 C12 C13 H13A 121.4 C13 C14 C15 121.9(14) C13 C14 H14A 119.1 C15 C14 H14A 119.1 N3 C15 C14 120.3(12) N3 C15 C16 110.2(13) C14 C15 C16 129.4(12) N4 C16 C17 110.1(13) N4 C16 C15 113.2(11) C17 C16 C15 136.7(14) C18 C17 C16 106.5(14) C18 C17 H17A 126.7 C16 C17 H17A 126.7 C17 C18 N5 105.4(12) C17 C18 C19 132.9(15) N5 C18 C19 121.7(14) C24 C19 C20 119.2(15) C24 C19 C18 124.1(15) C20 C19 C18 116.6(16) C21 C20 C19 121.4(18) C21 C20 H20A 119.3 C19 C20 H20A 119.3 C22 C21 C20 117.1(18) C22 C21 H21A 121.5 C20 C21 H21A 121.5 C21 C22 C23 124.5(17) C21 C22 H22A 117.7 C23 C22 H22A 117.7 C24 C23 C22 118.3(19) C24 C23 H23A 120.9 C22 C23 H23A 120.9 O2 C24 C23 124.0(18) O2 C24 C19 116.6(14) C23 C24 C19 119.4(17) 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 108.5(12) C27 C26 H26A 125.7 N6 C26 H26A 125.7 C26 C27 C28 104.6(13) C26 C27 H27A 127.7 C28 C27 H27A 127.7 N7 C28 C27 109.8(14) N7 C28 C29 114.4(13) C27 C28 C29 135.8(15) N8 C29 C30 119.2(14) N8 C29 C28 110.8(13) C30 C29 C28 130.0(13) C29 C30 C31 121.1(15) C29 C30 H30A 119.5 C31 C30 H30A 119.5 C30 C31 C32 118.8(16) C30 C31 H31A 120.6 C32 C31 H31A 120.6 C33 C32 C31 118.4(15) C33 C32 H32A 120.8 C31 C32 H32A 120.8 N8 C33 C32 120.2(13) N8 C33 C34 112.0(15) C32 C33 C34 127.8(14) N9 C34 C35 110.3(13) N9 C34 C33 114.5(12) C35 C34 C33 135.2(17) C36 C35 C34 102.4(16) C36 C35 H35A 128.8 C34 C35 H35A 128.8 N10 C36 C35 110.5(14) N10 C36 H36A 124.7 C35 C36 H36A 124.7 O3 C37 C38 120.0(18) O3 C37 C39 125.7(18) C38 C37 C39 114.2(18) 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 140(7) O4 C40 C42 96(7) C41 C40 C42 111(7) 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_1 112.8(10) O4_1 Cl1_1 O1_1 109.3(10) O2_1 Cl1_1 O1_1 110.0(10) O4_1 Cl1_1 O3_1 108.4(10) O2_1 Cl1_1 O3_1 108.4(10) O1_1 Cl1_1 O3_1 107.9(10) O2_2 Cl1_2 O1_2 111.4(11) O2_2 Cl1_2 O3_2 110.9(11) O1_2 Cl1_2 O3_2 111.0(11) O2_2 Cl1_2 O4_2 107.8(10) O1_2 Cl1_2 O4_2 108.6(11) O3_2 Cl1_2 O4_2 107.0(10) O3_3 Cl1_3 O2_3 110.8(10) O3_3 Cl1_3 O1_3 110.1(10) O2_3 Cl1_3 O1_3 108.1(10) O3_3 Cl1_3 O4_3 109.3(10) O2_3 Cl1_3 O4_3 110.2(10) O1_3 Cl1_3 O4_3 108.3(10) O1_4 Cl1_4 O2_4 109.7(10) O1_4 Cl1_4 O4_4 108.4(10) O2_4 Cl1_4 O4_4 110.6(10) O1_4 Cl1_4 O3_4 108.6(10) O2_4 Cl1_4 O3_4 108.5(10) O4_4 Cl1_4 O3_4 110.9(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3 1.923(12) Fe1 N8 1.940(12) Fe1 N4 1.961(10) Fe1 N7 1.964(10) Fe1 N2 1.997(10) Fe1 N9 2.004(10) O1 C2 1.37(2) O1 C1 1.43(2) O2 C24 1.32(2) O2 C25 1.40(2) O3 C37 1.18(2) N1 N2 1.336(13) N1 C8 1.384(15) N1 H1 0.8700 N2 C10 1.354(15) N3 C11 1.330(16) N3 C15 1.358(17) N4 N5 1.337(14) N4 C16 1.339(15) N5 C18 1.375(15) N5 H5 0.8700 N6 N7 1.336(14) N6 C26 1.359(15) N6 H6 0.8700 N7 C28 1.342(16) N8 C29 1.360(16) N8 C33 1.368(17) N9 C34 1.337(16) N9 N10 1.342(14) N10 C36 1.357(18) N10 H10 0.8700 C1 H1A 0.9700 C1 H1B 0.9700 C1 H1C 0.9700 C2 C3 1.35(3) C2 C7 1.40(2) C3 C4 1.38(2) C3 H3A 0.9400 C4 C5 1.42(3) C4 H4A 0.9400 C5 C6 1.38(2) C5 H5A 0.9400 C6 C7 1.389(19) C6 H6A 0.9400 C7 C8 1.51(2) C8 C9 1.362(17) C9 C10 1.420(17) C9 H9A 0.9400 C10 C11 1.45(2) C11 C12 1.373(16) C12 C13 1.41(2) C12 H12A 0.9400 C13 C14 1.35(2) C13 H13A 0.9400 C14 C15 1.378(16) C14 H14A 0.9400 C15 C16 1.486(19) C16 C17 1.411(17) C17 C18 1.359(18) C17 H17A 0.9400 C18 C19 1.458(18) C19 C24 1.40(2) C19 C20 1.41(2) C20 C21 1.40(2) C20 H20A 0.9400 C21 C22 1.34(2) C21 H21A 0.9400 C22 C23 1.40(2) C22 H22A 0.9400 C23 C24 1.40(2) C23 H23A 0.9400 C25 H25A 0.9700 C25 H25B 0.9700 C25 H25C 0.9700 C26 C27 1.347(17) C26 H26A 0.9400 C27 C28 1.427(17) C27 H27A 0.9400 C28 C29 1.434(19) C29 C30 1.375(17) C30 C31 1.39(2) C30 H30A 0.9400 C31 C32 1.43(2) C31 H31A 0.9400 C32 C33 1.390(17) C32 H32A 0.9400 C33 C34 1.440(19) C34 C35 1.412(18) C35 C36 1.40(2) C35 H35A 0.9400 C36 H36A 0.9400 C37 C38 1.494(16) C37 C39 1.495(16) 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 1.17(2) C40 C41 1.493(18) C40 C42 1.494(18) 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 1.410(10) Cl1_1 O2_1 1.414(9) Cl1_1 O1_1 1.427(9) Cl1_1 O3_1 1.432(10) Cl1_2 O2_2 1.413(10) Cl1_2 O1_2 1.415(10) Cl1_2 O3_2 1.420(10) Cl1_2 O4_2 1.434(10) Cl1_3 O3_3 1.417(9) Cl1_3 O2_3 1.420(9) Cl1_3 O1_3 1.422(9) Cl1_3 O4_3 1.423(9) Cl1_4 O1_4 1.420(10) Cl1_4 O2_4 1.420(9) Cl1_4 O4_4 1.422(9) Cl1_4 O3_4 1.422(10) 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 2.16 3.02(3) 169.0 . N1 H1 O4_3 0.87 2.06 2.91(2) 165.2 . N5 H5 O2 0.87 2.03 2.603(16) 122.9 . N6 H6 O1_2 0.87 2.08 2.94(3) 173.1 . N6 H6 O1_1 0.87 1.93 2.78(3) 168.3 . N6 H6 Cl1_1 0.87 2.69 3.486(17) 152.8 . N6 H6 Cl1_2 0.87 2.87 3.681(15) 155.0 . N10 H10 O3 0.87 1.92 2.75(2) 159.2 4_565