#------------------------------------------------------------------------------ #$Date: 2018-03-28 04:33:33 +0300 (Wed, 28 Mar 2018) $ #$Revision: 207139 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/59/7045930.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_7045930 loop_ _publ_author_name 'Drahos, Bohuslav' 'Travnicek, Zdenek' _publ_section_title ; Spin Crossover Fe(II) Complexes of a Cross-Bridged Cyclam Derivative ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C8DT00414E _journal_year 2018 _chemical_formula_sum 'C48 H78 Cl4 Fe2 N12 O3' _chemical_formula_weight 1124.72 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-03-08 deposited with the CCDC. 2018-03-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.314(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 23.5964(15) _cell_length_b 13.0895(9) _cell_length_c 17.5179(12) _cell_measurement_reflns_used 9850 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 55.08 _cell_measurement_theta_min 4.76 _cell_volume 5040.6(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1303 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 78326 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.325 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.482 _exptl_crystal_description prism _exptl_crystal_F_000 2376 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _exptl_transmission_factor_max 0.837 _exptl_transmission_factor_min 0.769 _refine_diff_density_max 1.341 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 650 _refine_ls_number_reflns 8866 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0451 _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^)+(0.0444P)^2^+3.6107P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0986 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6588 _reflns_number_total 8866 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt00414e2.cif _cod_data_source_block complex2 _cod_database_code 7045930 _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 0.863 _shelx_estimated_absorpt_t_max 0.906 _shelx_res_file ; b.res created by SHELXL-2014/7 TITL bd_2016_18_0ma in P2(1)/c CELL 0.71073 23.5964 13.0895 17.5179 90.000 111.314 90.000 ZERR 4.00 0.0015 0.0009 0.0012 0.000 0.002 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C N CL FE O H UNIT 192 48 16 8 12 312 TEMP -153.150 SIZE 0.120 0.160 0.180 ACTA L.S. 50 OMIT 0 50 FMAP 2 PLAN 20 MERG LIST 1 HTAB BOND $H REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB C1 O1_$1 EQIV $2 -x+1, y-1/2, -z+1/2 HTAB C2 Cl3_$2 EQIV $3 x, -y+1/2, z+1/2 HTAB C3 Cl3_$3 HTAB C5 Cl1 HTAB C6 Cl4 HTAB C9 Cl2 HTAB C9 Cl3_$3 HTAB C11 Cl2_$2 HTAB C11 Cl1 EQIV $4 -x+1, y+1/2, -z+1/2 HTAB C13 O2_$4 HTAB C16 O1_$4 HTAB C19 Cl1 HTAB C21 Cl2_$2 HTAB C23 Cl3 HTAB C24 Cl3 HTAB C25 Cl1_$3 EQIV $5 -x+1, -y+1, -z+1 HTAB C26 Cl2_$5 EQIV $6 -x, y+1/2, -z+1/2 HTAB C29 Cl4_$6 HTAB C30 O3A HTAB C30 O3B HTAB C33 Cl3_$4 EQIV $7 x, y+1, z HTAB C35 Cl4_$7 HTAB C40 Cl1_$7 HTAB C43 Cl4_$6 HTAB C48 Cl2_$4 HTAB O1 Cl3_$3 HTAB O1 Cl2 HTAB O2 Cl2 HTAB O2 Cl3 HTAB O3A Cl4 HTAB O3B Cl4 HTAB O3A Cl1 HTAB O3B Cl1 WGHT 0.044400 3.610700 FVAR 0.08106 0.46105 FE1 4 0.384802 0.169729 0.245935 11.00000 0.00483 0.00545 = 0.00603 0.00027 0.00075 -0.00033 FE1A 4 0.126075 0.633539 0.267218 11.00000 0.00673 0.01123 = 0.00938 0.00071 0.00227 -0.00095 N1 2 0.331495 0.039819 0.238869 11.00000 0.00856 0.01023 = 0.00827 0.00096 0.00437 0.00095 N2 2 0.447722 0.094409 0.340824 11.00000 0.00755 0.00777 = 0.00746 -0.00066 0.00145 -0.00147 N3 2 0.359980 0.241741 0.332286 11.00000 0.00774 0.01078 = 0.01116 -0.00162 0.00298 0.00102 N4 2 0.439250 0.299537 0.255993 11.00000 0.00876 0.00801 = 0.00744 0.00049 0.00064 -0.00012 N5 2 0.404434 0.089975 0.158980 11.00000 0.00829 0.00560 = 0.00687 0.00313 0.00038 0.00047 N6 2 0.327270 0.252535 0.152799 11.00000 0.01000 0.00758 = 0.01106 -0.00065 0.00320 0.00007 N1A 2 0.070869 0.505586 0.263373 11.00000 0.00914 0.01240 = 0.01148 0.00041 0.00199 -0.00126 N3A 2 0.111407 0.700560 0.363025 11.00000 0.01097 0.01456 = 0.01022 -0.00131 0.00254 -0.00172 N2A 2 0.192101 0.549893 0.350085 11.00000 0.00953 0.01562 = 0.01450 0.00067 0.00535 -0.00116 N4A 2 0.182250 0.761423 0.274307 11.00000 0.01004 0.01479 = 0.01349 0.00161 0.00124 -0.00216 N5A 2 0.134374 0.561678 0.170785 11.00000 0.01105 0.01277 = 0.00913 0.00138 0.00250 -0.00087 N6A 2 0.065513 0.723146 0.183069 11.00000 0.00860 0.01202 = 0.01310 -0.00182 0.00330 -0.00110 O1 5 0.647158 0.105549 0.527702 11.00000 0.03267 0.01776 = 0.02168 0.00145 0.01310 0.00601 O2 5 0.619090 0.105448 0.248626 11.00000 0.07180 0.02377 = 0.01803 0.00031 -0.00621 -0.01899 PART 1 O3A 5 0.138749 0.250521 0.191008 21.00000 0.09913 0.02091 = 0.04438 -0.01121 0.04098 -0.00743 PART 2 O3B 5 0.104323 0.236233 0.171895 -21.00000 0.08072 0.02862 = 0.03752 0.00662 0.03829 0.02277 PART 0 C1 1 0.370086 -0.039390 0.296143 11.00000 0.00977 0.00780 = 0.01480 0.00373 0.00203 -0.00035 AFIX 23 H1A 6 0.361744 -0.106933 0.268883 11.00000 -1.20000 H1B 6 0.359002 -0.043114 0.345420 11.00000 -1.20000 AFIX 0 C2 1 0.437080 -0.015941 0.321930 11.00000 0.00995 0.00903 = 0.01277 0.00204 0.00287 -0.00041 AFIX 23 H2A 6 0.460215 -0.056779 0.370937 11.00000 -1.20000 H2B 6 0.451517 -0.034565 0.277308 11.00000 -1.20000 AFIX 0 C3 1 0.437146 0.115274 0.419017 11.00000 0.01204 0.01523 = 0.00553 0.00128 0.00148 -0.00027 AFIX 23 H3A 6 0.476776 0.116444 0.465252 11.00000 -1.20000 H3B 6 0.412570 0.059157 0.428996 11.00000 -1.20000 AFIX 0 C4 1 0.404697 0.215843 0.416420 11.00000 0.01170 0.01665 = 0.00784 -0.00088 0.00418 -0.00151 AFIX 23 H4A 6 0.382845 0.212579 0.455076 11.00000 -1.20000 H4B 6 0.435292 0.271132 0.435021 11.00000 -1.20000 AFIX 0 C5 1 0.274351 0.049203 0.257312 11.00000 0.00644 0.01314 = 0.01507 0.00343 0.00536 -0.00081 AFIX 23 H5A 6 0.259774 -0.020215 0.263168 11.00000 -1.20000 H5B 6 0.242685 0.082256 0.210110 11.00000 -1.20000 AFIX 0 C6 1 0.281646 0.109599 0.333808 11.00000 0.00636 0.01998 = 0.01530 0.00334 0.00633 0.00084 AFIX 23 H6A 6 0.314420 0.078351 0.380794 11.00000 -1.20000 H6B 6 0.243447 0.105107 0.344853 11.00000 -1.20000 AFIX 0 C7 1 0.296652 0.220793 0.327798 11.00000 0.01038 0.02231 = 0.01456 -0.00257 0.00535 0.00427 AFIX 23 H7A 6 0.267948 0.248270 0.275340 11.00000 -1.20000 H7B 6 0.289762 0.258596 0.372603 11.00000 -1.20000 AFIX 0 C8 1 0.512559 0.113762 0.352094 11.00000 0.00565 0.01065 = 0.01249 0.00092 0.00074 0.00002 AFIX 23 H8A 6 0.519659 0.088299 0.303107 11.00000 -1.20000 H8B 6 0.538723 0.073487 0.399692 11.00000 -1.20000 AFIX 0 C9 1 0.532320 0.224535 0.365470 11.00000 0.00591 0.01128 = 0.01185 0.00156 -0.00098 -0.00190 AFIX 23 H9A 6 0.519022 0.253868 0.408305 11.00000 -1.20000 H9B 6 0.577300 0.227597 0.385855 11.00000 -1.20000 AFIX 0 CL1 3 0.146376 0.072778 0.066116 11.00000 0.01162 0.02024 = 0.01444 -0.00320 0.00086 -0.00131 CL2 3 0.707025 0.218330 0.409975 11.00000 0.01595 0.02020 = 0.01878 -0.00498 0.00367 -0.00045 CL3 3 0.558489 0.246428 0.087069 11.00000 0.01550 0.01200 = 0.01521 -0.00296 0.00653 -0.00205 CL4 3 0.127971 0.111834 0.334675 11.00000 0.01258 0.05494 = 0.01676 0.00323 0.00512 0.00230 C10 1 0.506922 0.289147 0.288731 11.00000 0.00669 0.01001 = 0.01168 -0.00149 -0.00007 -0.00424 AFIX 23 H10A 6 0.525148 0.358186 0.300750 11.00000 -1.20000 H10B 6 0.519537 0.258673 0.245667 11.00000 -1.20000 AFIX 0 C11 1 0.313714 0.000621 0.153924 11.00000 0.01109 0.00914 = 0.00890 -0.00066 0.00145 -0.00282 AFIX 23 H11A 6 0.277768 0.038592 0.117507 11.00000 -1.20000 H11B 6 0.302613 -0.072488 0.152434 11.00000 -1.20000 AFIX 0 C12 1 0.420852 0.342439 0.172014 11.00000 0.01333 0.00790 = 0.01288 0.00590 0.00283 -0.00236 AFIX 23 H12A 6 0.443345 0.307160 0.141769 11.00000 -1.20000 H12B 6 0.431492 0.415886 0.175284 11.00000 -1.20000 AFIX 0 C13 1 0.424102 0.375765 0.310111 11.00000 0.02007 0.00652 = 0.01499 -0.00375 0.00255 -0.00195 AFIX 23 H13A 6 0.422597 0.445081 0.286843 11.00000 -1.20000 H13B 6 0.456650 0.375119 0.365104 11.00000 -1.20000 AFIX 0 C14 1 0.363935 0.352623 0.318360 11.00000 0.01728 0.00943 = 0.01598 -0.00414 0.00502 0.00363 AFIX 23 H14A 6 0.360425 0.391499 0.364917 11.00000 -1.20000 H14B 6 0.330151 0.373471 0.267850 11.00000 -1.20000 AFIX 0 C15 1 0.353838 0.329935 0.126698 11.00000 0.00874 0.01357 = 0.00789 -0.00019 0.00243 0.00147 C16 1 0.322660 0.392571 0.061812 11.00000 0.02048 0.01193 = 0.01343 0.00526 0.00873 0.00288 AFIX 43 H16A 6 0.342754 0.447776 0.047084 11.00000 -1.20000 AFIX 0 C17 1 0.261782 0.373955 0.018493 11.00000 0.01544 0.02408 = 0.01168 0.00714 0.00310 0.00809 AFIX 43 H17A 6 0.239520 0.414492 -0.027663 11.00000 -1.20000 AFIX 0 C18 1 0.234232 0.295508 0.043726 11.00000 0.01356 0.01970 = 0.01417 -0.00067 0.00253 0.00248 AFIX 43 H18A 6 0.192522 0.280361 0.014735 11.00000 -1.20000 AFIX 0 C19 1 0.267474 0.239006 0.111303 11.00000 0.01088 0.01444 = 0.01131 0.00058 0.00361 0.00055 AFIX 43 H19A 6 0.247048 0.187550 0.129686 11.00000 -1.20000 AFIX 0 C20 1 0.364901 0.012910 0.124488 11.00000 0.00884 0.00898 = 0.00634 0.00160 0.00109 0.00167 C21 1 0.370590 -0.050005 0.064418 11.00000 0.00779 0.00911 = 0.00883 -0.00150 -0.00387 -0.00167 AFIX 43 H21A 6 0.343031 -0.105092 0.043801 11.00000 -1.20000 AFIX 0 C22 1 0.416451 -0.032851 0.034203 11.00000 0.01648 0.01457 = 0.00923 -0.00184 0.00272 0.00289 AFIX 43 H22A 6 0.420357 -0.074065 -0.008253 11.00000 -1.20000 AFIX 0 C23 1 0.456274 0.046384 0.068096 11.00000 0.01151 0.01308 = 0.01328 -0.00017 0.00719 0.00019 AFIX 43 H23A 6 0.487943 0.061490 0.048468 11.00000 -1.20000 AFIX 0 C24 1 0.449881 0.103090 0.130162 11.00000 0.00921 0.01021 = 0.01092 0.00133 0.00167 -0.00137 AFIX 43 H24A 6 0.479158 0.154786 0.154448 11.00000 -1.20000 AFIX 0 C25 1 0.190961 0.568738 0.434450 11.00000 0.01263 0.02473 = 0.00938 0.00374 0.00341 -0.00021 AFIX 23 H25A 6 0.233306 0.569762 0.474409 11.00000 -1.20000 H25B 6 0.169665 0.511209 0.449160 11.00000 -1.20000 AFIX 0 C26 1 0.159959 0.667842 0.441799 11.00000 0.01631 0.02660 = 0.00958 -0.00246 0.00233 0.00091 AFIX 23 H26A 6 0.141608 0.659457 0.484041 11.00000 -1.20000 H26B 6 0.190991 0.722453 0.460501 11.00000 -1.20000 AFIX 0 C27 1 0.049879 0.684021 0.366521 11.00000 0.01210 0.02273 = 0.01569 -0.00209 0.00563 -0.00017 AFIX 23 H27A 6 0.019198 0.714828 0.317125 11.00000 -1.20000 H27B 6 0.047710 0.720621 0.414841 11.00000 -1.20000 AFIX 0 C28 1 0.033226 0.573136 0.371577 11.00000 0.01161 0.02114 = 0.01708 -0.00134 0.00813 -0.00240 AFIX 23 H28A 6 -0.002446 0.570100 0.388534 11.00000 -1.20000 H28B 6 0.067519 0.538681 0.414426 11.00000 -1.20000 AFIX 0 C29 1 0.018489 0.515323 0.291500 11.00000 0.01282 0.01630 = 0.01583 0.00113 0.00638 -0.00217 AFIX 23 H29A 6 0.004091 0.446039 0.298136 11.00000 -1.20000 H29B 6 -0.015230 0.550714 0.248457 11.00000 -1.20000 AFIX 0 C30 1 0.111131 0.422777 0.314999 11.00000 0.01718 0.01262 = 0.02252 0.00329 0.00812 -0.00123 AFIX 23 H30A 6 0.098314 0.355982 0.287649 11.00000 -1.20000 H30B 6 0.106197 0.420088 0.368720 11.00000 -1.20000 AFIX 0 C31 1 0.177115 0.440736 0.328372 11.00000 0.01284 0.01496 = 0.01655 0.00253 0.00068 0.00387 AFIX 23 H31A 6 0.203142 0.396323 0.373142 11.00000 -1.20000 H31B 6 0.184774 0.423783 0.277891 11.00000 -1.20000 AFIX 0 C32 1 0.255000 0.566224 0.350977 11.00000 0.00659 0.02181 = 0.01759 0.00366 0.00279 0.00235 AFIX 23 H32A 6 0.256046 0.545596 0.297135 11.00000 -1.20000 H32B 6 0.283238 0.520979 0.393003 11.00000 -1.20000 AFIX 0 C33 1 0.277728 0.675209 0.368462 11.00000 0.00705 0.02473 = 0.01514 0.00113 0.00064 -0.00505 AFIX 23 H33A 6 0.322401 0.675634 0.383177 11.00000 -1.20000 H33B 6 0.269138 0.700772 0.416341 11.00000 -1.20000 AFIX 0 C34 1 0.249165 0.747333 0.296951 11.00000 0.00979 0.01762 = 0.01592 0.00063 0.00158 -0.00266 AFIX 23 H34A 6 0.269298 0.814765 0.310903 11.00000 -1.20000 H34B 6 0.256892 0.720754 0.248721 11.00000 -1.20000 AFIX 0 C35 1 0.174499 0.834854 0.336600 11.00000 0.01787 0.01388 = 0.02239 -0.00578 0.00599 -0.00461 AFIX 23 H35A 6 0.210062 0.829437 0.388449 11.00000 -1.20000 H35B 6 0.172841 0.905674 0.316058 11.00000 -1.20000 AFIX 0 C36 1 0.117272 0.812410 0.352865 11.00000 0.01828 0.01258 = 0.01779 -0.00332 0.00575 -0.00094 AFIX 23 H36A 6 0.118539 0.848419 0.403157 11.00000 -1.20000 H36B 6 0.081508 0.837527 0.306589 11.00000 -1.20000 AFIX 0 C37 1 0.045938 0.471808 0.176571 11.00000 0.01765 0.01896 = 0.01472 -0.00313 0.00813 -0.00336 AFIX 23 H37A 6 0.007051 0.507590 0.147647 11.00000 -1.20000 H37B 6 0.037525 0.397549 0.174350 11.00000 -1.20000 AFIX 0 C38 1 0.158256 0.811053 0.192223 11.00000 0.01310 0.01632 = 0.01563 0.00739 0.00108 -0.00159 AFIX 23 H38A 6 0.177919 0.780324 0.156488 11.00000 -1.20000 H38B 6 0.168434 0.884720 0.198066 11.00000 -1.20000 AFIX 0 C39 1 0.090536 0.798444 0.153083 11.00000 0.01127 0.01427 = 0.01094 0.00064 0.00438 0.00164 C40 1 0.057672 0.859942 0.088582 11.00000 0.01505 0.01436 = 0.01441 0.00243 0.00713 0.00104 AFIX 43 H40A 6 0.077440 0.912376 0.070143 11.00000 -1.20000 AFIX 0 C41 1 -0.004070 0.845154 0.050819 11.00000 0.01535 0.01934 = 0.01002 -0.00069 0.00412 0.00479 AFIX 43 H41A 6 -0.027391 0.884463 0.004447 11.00000 -1.20000 AFIX 0 C42 1 -0.030964 0.770996 0.082798 11.00000 0.00785 0.01838 = 0.01255 -0.00415 0.00049 0.00194 AFIX 43 H42A 6 -0.073659 0.760180 0.059626 11.00000 -1.20000 AFIX 0 C43 1 0.004335 0.713230 0.148091 11.00000 0.00953 0.01325 = 0.01651 -0.00515 0.00337 -0.00357 AFIX 43 H43A 6 -0.015118 0.663778 0.169867 11.00000 -1.20000 AFIX 0 C44 1 0.089605 0.493683 0.134175 11.00000 0.01603 0.01342 = 0.01151 0.00047 0.00304 0.00147 C45 1 0.081458 0.447891 0.059814 11.00000 0.02222 0.01827 = 0.01666 -0.00628 0.00477 0.00025 AFIX 43 H45A 6 0.049414 0.400310 0.036379 11.00000 -1.20000 AFIX 0 C46 1 0.120614 0.472375 0.020126 11.00000 0.03311 0.02129 = 0.01371 -0.00120 0.01019 0.00612 AFIX 43 H46A 6 0.115221 0.443689 -0.031867 11.00000 -1.20000 AFIX 0 C47 1 0.167732 0.539345 0.057500 11.00000 0.02193 0.02467 = 0.01762 0.00293 0.01137 0.00429 AFIX 43 H47A 6 0.195660 0.556952 0.031935 11.00000 -1.20000 AFIX 0 C48 1 0.173615 0.580075 0.132097 11.00000 0.01497 0.02172 = 0.01687 0.00211 0.00671 0.00087 AFIX 43 H48A 6 0.207239 0.623815 0.158178 11.00000 -1.20000 AFIX 0 H1V 6 0.629785 0.144355 0.541392 11.00000 -1.20000 H1W 6 0.663772 0.134838 0.499449 11.00000 -1.20000 H3V 6 0.117768 0.199558 0.221873 11.00000 -1.20000 H3W 6 0.129883 0.208586 0.157578 11.00000 -1.20000 H2V 6 0.608625 0.140779 0.213279 11.00000 -1.20000 H2W 6 0.643277 0.136991 0.294000 11.00000 -1.20000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM bd_2016_18_0ma in P2(1)/c REM R1 = 0.0451 for 6588 Fo > 4sig(Fo) and 0.0747 for all 8866 data REM 650 parameters refined using 0 restraints END WGHT 0.0381 4.5274 REM Instructions for potential hydrogen bonds HTAB C1 O1_$1 HTAB C2 Cl3_$2 HTAB C3 Cl3_$3 HTAB C5 Cl1 HTAB C6 Cl4 HTAB C9 Cl3_$3 HTAB C9 Cl2 HTAB C11 Cl1 HTAB C11 Cl2_$2 HTAB C13 O2_$4 HTAB C16 O1_$4 HTAB C19 Cl1 HTAB C21 Cl2_$2 HTAB C23 Cl3 HTAB C24 Cl3 HTAB C25 Cl1_$3 HTAB C26 Cl2_$5 HTAB C29 Cl4_$6 HTAB C30 O3A HTAB C30 O3B HTAB C33 Cl3_$4 HTAB C35 Cl4_$7 HTAB C37 O3B HTAB C40 Cl1_$7 HTAB C43 Cl4_$6 HTAB C48 Cl2_$4 HTAB O1 Cl3_$3 HTAB O1 Cl2 HTAB O3A Cl4 HTAB O3B Cl4 HTAB O3A Cl1 HTAB O3B Cl1 HTAB O2 Cl3 HTAB O2 Cl2 REM Highest difference peak 1.341, deepest hole -0.658, 1-sigma level 0.085 Q1 1 0.1354 0.1865 0.3516 11.00000 0.05 1.34 Q2 1 0.1203 1.0014 0.2204 11.00000 0.05 0.65 Q3 1 0.1122 0.6035 0.2160 11.00000 0.05 0.50 Q4 1 0.1238 0.0709 0.3828 11.00000 0.05 0.48 Q5 1 0.1411 0.0212 0.3307 11.00000 0.05 0.39 Q6 1 0.3590 0.0019 0.0770 11.00000 0.05 0.34 Q7 1 0.5163 0.2448 0.3218 11.00000 0.05 0.34 Q8 1 0.2649 0.2529 0.4564 11.00000 0.05 0.33 Q9 1 0.2207 -0.0304 0.0874 11.00000 0.05 0.32 Q10 1 0.1759 0.6616 0.5571 11.00000 0.05 0.30 Q11 1 0.0784 0.2435 0.0553 11.00000 0.05 0.30 Q12 1 0.0975 0.0613 0.0540 11.00000 0.05 0.30 Q13 1 0.3318 0.4444 0.0744 11.00000 0.05 0.30 Q14 1 -0.0421 0.9576 -0.0010 11.00000 0.05 0.30 Q15 1 0.7081 0.2365 0.4614 11.00000 0.05 0.30 Q16 1 0.1470 0.1797 0.3007 11.00000 0.05 0.30 Q17 1 0.4715 0.2959 0.2804 11.00000 0.05 0.30 Q18 1 0.3355 0.0965 0.2461 11.00000 0.05 0.29 Q19 1 0.3396 0.0180 0.1429 11.00000 0.05 0.29 Q20 1 -0.0096 0.8366 0.1007 11.00000 0.05 0.29 ; _shelx_res_checksum 96335 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.38480(2) 0.16973(3) 0.24593(3) 0.00578(11) Uani 1 1 d . . . . . Fe1A Fe 0.12607(2) 0.63354(3) 0.26722(3) 0.00930(12) Uani 1 1 d . . . . . N1 N 0.33149(11) 0.03982(19) 0.23887(15) 0.0087(6) Uani 1 1 d . . . . . N2 N 0.44772(11) 0.09441(18) 0.34082(15) 0.0079(6) Uani 1 1 d . . . . . N3 N 0.35998(11) 0.24174(19) 0.33229(16) 0.0100(6) Uani 1 1 d . . . . . N4 N 0.43925(11) 0.29954(19) 0.25599(15) 0.0087(6) Uani 1 1 d . . . . . N5 N 0.40443(11) 0.08997(18) 0.15898(15) 0.0076(6) Uani 1 1 d . . . . . N6 N 0.32727(11) 0.25253(19) 0.15280(16) 0.0097(6) Uani 1 1 d . . . . . N1A N 0.07087(11) 0.50559(19) 0.26337(16) 0.0115(6) Uani 1 1 d . . . . . N3A N 0.11141(12) 0.7006(2) 0.36302(16) 0.0123(6) Uani 1 1 d . . . . . N2A N 0.19210(11) 0.5499(2) 0.35009(16) 0.0129(6) Uani 1 1 d . . . . . N4A N 0.18225(12) 0.7614(2) 0.27431(16) 0.0136(6) Uani 1 1 d . . . . . N5A N 0.13437(12) 0.5617(2) 0.17079(16) 0.0113(6) Uani 1 1 d . . . . . N6A N 0.06551(11) 0.72315(19) 0.18307(16) 0.0114(6) Uani 1 1 d . . . . . O1 O 0.64716(13) 0.10555(19) 0.52770(16) 0.0231(6) Uani 1 1 d . . . . . O2 O 0.61909(16) 0.1054(2) 0.24863(18) 0.0442(9) Uani 1 1 d . . . . . O3A O 0.139(3) 0.2505(9) 0.1910(16) 0.051(8) Uani 0.46(7) 1 d . . P A 1 O3B O 0.104(2) 0.2362(19) 0.1719(14) 0.044(7) Uani 0.54(7) 1 d . . P A 2 C1 C 0.37009(13) -0.0394(2) 0.2961(2) 0.0115(7) Uani 1 1 d . . . . . H1A H 0.3617 -0.1069 0.2689 0.014 Uiso 1 1 calc R U . . . H1B H 0.3590 -0.0431 0.3454 0.014 Uiso 1 1 calc R U . . . C2 C 0.43708(14) -0.0159(2) 0.3219(2) 0.0109(7) Uani 1 1 d . . . . . H2A H 0.4602 -0.0568 0.3709 0.013 Uiso 1 1 calc R U . . . H2B H 0.4515 -0.0346 0.2773 0.013 Uiso 1 1 calc R U . . . C3 C 0.43715(14) 0.1153(2) 0.41902(19) 0.0114(7) Uani 1 1 d . . . . . H3A H 0.4768 0.1164 0.4653 0.014 Uiso 1 1 calc R U . . . H3B H 0.4126 0.0592 0.4290 0.014 Uiso 1 1 calc R U . . . C4 C 0.40470(14) 0.2158(2) 0.41642(19) 0.0119(7) Uani 1 1 d . . . . . H4A H 0.3828 0.2126 0.4551 0.014 Uiso 1 1 calc R U . . . H4B H 0.4353 0.2711 0.4350 0.014 Uiso 1 1 calc R U . . . C5 C 0.27435(13) 0.0492(2) 0.25731(19) 0.0111(7) Uani 1 1 d . . . . . H5A H 0.2598 -0.0202 0.2632 0.013 Uiso 1 1 calc R U . . . H5B H 0.2427 0.0823 0.2101 0.013 Uiso 1 1 calc R U . . . C6 C 0.28165(14) 0.1096(2) 0.3338(2) 0.0132(7) Uani 1 1 d . . . . . H6A H 0.3144 0.0784 0.3808 0.016 Uiso 1 1 calc R U . . . H6B H 0.2434 0.1051 0.3449 0.016 Uiso 1 1 calc R U . . . C7 C 0.29665(14) 0.2208(3) 0.3278(2) 0.0155(8) Uani 1 1 d . . . . . H7A H 0.2679 0.2483 0.2753 0.019 Uiso 1 1 calc R U . . . H7B H 0.2898 0.2586 0.3726 0.019 Uiso 1 1 calc R U . . . C8 C 0.51256(13) 0.1138(2) 0.3521(2) 0.0103(7) Uani 1 1 d . . . . . H8A H 0.5197 0.0883 0.3031 0.012 Uiso 1 1 calc R U . . . H8B H 0.5387 0.0735 0.3997 0.012 Uiso 1 1 calc R U . . . C9 C 0.53232(14) 0.2245(2) 0.36547(19) 0.0109(7) Uani 1 1 d . . . . . H9A H 0.5190 0.2539 0.4083 0.013 Uiso 1 1 calc R U . . . H9B H 0.5773 0.2276 0.3859 0.013 Uiso 1 1 calc R U . . . Cl1 Cl 0.14638(4) 0.07278(6) 0.06612(5) 0.01652(19) Uani 1 1 d . . . . . Cl2 Cl 0.70702(4) 0.21833(6) 0.40997(5) 0.0190(2) Uani 1 1 d . . . . . Cl3 Cl 0.55849(4) 0.24643(6) 0.08707(5) 0.01397(18) Uani 1 1 d . . . . . Cl4 Cl 0.12797(4) 0.11183(8) 0.33468(5) 0.0281(2) Uani 1 1 d . . . . . C10 C 0.50692(13) 0.2891(2) 0.28873(19) 0.0104(7) Uani 1 1 d . . . . . H10A H 0.5251 0.3582 0.3008 0.012 Uiso 1 1 calc R U . . . H10B H 0.5195 0.2587 0.2457 0.012 Uiso 1 1 calc R U . . . C11 C 0.31371(14) 0.0006(2) 0.15392(19) 0.0103(7) Uani 1 1 d . . . . . H11A H 0.2778 0.0386 0.1175 0.012 Uiso 1 1 calc R U . . . H11B H 0.3026 -0.0725 0.1524 0.012 Uiso 1 1 calc R U . . . C12 C 0.42085(14) 0.3424(2) 0.17201(19) 0.0119(7) Uani 1 1 d . . . . . H12A H 0.4433 0.3072 0.1418 0.014 Uiso 1 1 calc R U . . . H12B H 0.4315 0.4159 0.1753 0.014 Uiso 1 1 calc R U . . . C13 C 0.42410(15) 0.3758(2) 0.3101(2) 0.0149(7) Uani 1 1 d . . . . . H13A H 0.4226 0.4451 0.2868 0.018 Uiso 1 1 calc R U . . . H13B H 0.4566 0.3751 0.3651 0.018 Uiso 1 1 calc R U . . . C14 C 0.36393(15) 0.3526(2) 0.3184(2) 0.0145(7) Uani 1 1 d . . . . . H14A H 0.3604 0.3915 0.3649 0.017 Uiso 1 1 calc R U . . . H14B H 0.3302 0.3735 0.2679 0.017 Uiso 1 1 calc R U . . . C15 C 0.35384(14) 0.3299(2) 0.12670(19) 0.0102(7) Uani 1 1 d . . . . . C16 C 0.32266(15) 0.3926(2) 0.0618(2) 0.0146(7) Uani 1 1 d . . . . . H16A H 0.3428 0.4478 0.0471 0.017 Uiso 1 1 calc R U . . . C17 C 0.26178(15) 0.3740(3) 0.0185(2) 0.0176(8) Uani 1 1 d . . . . . H17A H 0.2395 0.4145 -0.0277 0.021 Uiso 1 1 calc R U . . . C18 C 0.23423(15) 0.2955(3) 0.0437(2) 0.0165(8) Uani 1 1 d . . . . . H18A H 0.1925 0.2804 0.0147 0.020 Uiso 1 1 calc R U . . . C19 C 0.26747(14) 0.2390(2) 0.11130(19) 0.0123(7) Uani 1 1 d . . . . . H19A H 0.2470 0.1876 0.1297 0.015 Uiso 1 1 calc R U . . . C20 C 0.36490(14) 0.0129(2) 0.12449(19) 0.0085(7) Uani 1 1 d . . . . . C21 C 0.37059(14) -0.0500(2) 0.06442(19) 0.0105(7) Uani 1 1 d . . . . . H21A H 0.3430 -0.1051 0.0438 0.013 Uiso 1 1 calc R U . . . C22 C 0.41645(14) -0.0329(2) 0.0342(2) 0.0140(7) Uani 1 1 d . . . . . H22A H 0.4204 -0.0741 -0.0083 0.017 Uiso 1 1 calc R U . . . C23 C 0.45627(14) 0.0464(2) 0.06810(19) 0.0119(7) Uani 1 1 d . . . . . H23A H 0.4879 0.0615 0.0485 0.014 Uiso 1 1 calc R U . . . C24 C 0.44988(14) 0.1031(2) 0.13016(19) 0.0107(7) Uani 1 1 d . . . . . H24A H 0.4792 0.1548 0.1544 0.013 Uiso 1 1 calc R U . . . C25 C 0.19096(15) 0.5687(3) 0.43445(19) 0.0157(8) Uani 1 1 d . . . . . H25A H 0.2333 0.5698 0.4744 0.019 Uiso 1 1 calc R U . . . H25B H 0.1697 0.5112 0.4492 0.019 Uiso 1 1 calc R U . . . C26 C 0.15996(15) 0.6678(3) 0.4418(2) 0.0182(8) Uani 1 1 d . . . . . H26A H 0.1416 0.6595 0.4840 0.022 Uiso 1 1 calc R U . . . H26B H 0.1910 0.7225 0.4605 0.022 Uiso 1 1 calc R U . . . C27 C 0.04988(15) 0.6840(3) 0.3665(2) 0.0167(8) Uani 1 1 d . . . . . H27A H 0.0192 0.7148 0.3171 0.020 Uiso 1 1 calc R U . . . H27B H 0.0477 0.7206 0.4148 0.020 Uiso 1 1 calc R U . . . C28 C 0.03323(15) 0.5731(3) 0.3716(2) 0.0158(8) Uani 1 1 d . . . . . H28A H -0.0024 0.5701 0.3885 0.019 Uiso 1 1 calc R U . . . H28B H 0.0675 0.5387 0.4144 0.019 Uiso 1 1 calc R U . . . C29 C 0.01849(14) 0.5153(3) 0.2915(2) 0.0147(7) Uani 1 1 d . . . . . H29A H 0.0041 0.4460 0.2981 0.018 Uiso 1 1 calc R U . . . H29B H -0.0152 0.5507 0.2485 0.018 Uiso 1 1 calc R U . . . C30 C 0.11113(15) 0.4228(2) 0.3150(2) 0.0172(8) Uani 1 1 d . . . . . H30A H 0.0983 0.3560 0.2876 0.021 Uiso 1 1 calc R U . . . H30B H 0.1062 0.4201 0.3687 0.021 Uiso 1 1 calc R U . . . C31 C 0.17711(14) 0.4407(2) 0.3284(2) 0.0161(8) Uani 1 1 d . . . . . H31A H 0.2031 0.3963 0.3731 0.019 Uiso 1 1 calc R U . . . H31B H 0.1848 0.4238 0.2779 0.019 Uiso 1 1 calc R U . . . C32 C 0.25500(14) 0.5662(3) 0.3510(2) 0.0158(8) Uani 1 1 d . . . . . H32A H 0.2560 0.5456 0.2971 0.019 Uiso 1 1 calc R U . . . H32B H 0.2832 0.5210 0.3930 0.019 Uiso 1 1 calc R U . . . C33 C 0.27773(14) 0.6752(3) 0.3685(2) 0.0166(8) Uani 1 1 d . . . . . H33A H 0.3224 0.6756 0.3832 0.020 Uiso 1 1 calc R U . . . H33B H 0.2691 0.7008 0.4163 0.020 Uiso 1 1 calc R U . . . C34 C 0.24916(14) 0.7473(3) 0.2970(2) 0.0153(7) Uani 1 1 d . . . . . H34A H 0.2693 0.8148 0.3109 0.018 Uiso 1 1 calc R U . . . H34B H 0.2569 0.7208 0.2487 0.018 Uiso 1 1 calc R U . . . C35 C 0.17450(15) 0.8349(3) 0.3366(2) 0.0184(8) Uani 1 1 d . . . . . H35A H 0.2101 0.8294 0.3884 0.022 Uiso 1 1 calc R U . . . H35B H 0.1728 0.9057 0.3161 0.022 Uiso 1 1 calc R U . . . C36 C 0.11727(15) 0.8124(2) 0.3529(2) 0.0164(8) Uani 1 1 d . . . . . H36A H 0.1185 0.8484 0.4032 0.020 Uiso 1 1 calc R U . . . H36B H 0.0815 0.8375 0.3066 0.020 Uiso 1 1 calc R U . . . C37 C 0.04594(15) 0.4718(3) 0.1766(2) 0.0165(8) Uani 1 1 d . . . . . H37A H 0.0071 0.5076 0.1476 0.020 Uiso 1 1 calc R U . . . H37B H 0.0375 0.3975 0.1743 0.020 Uiso 1 1 calc R U . . . C38 C 0.15826(14) 0.8111(3) 0.1922(2) 0.0162(8) Uani 1 1 d . . . . . H38A H 0.1779 0.7803 0.1565 0.019 Uiso 1 1 calc R U . . . H38B H 0.1684 0.8847 0.1981 0.019 Uiso 1 1 calc R U . . . C39 C 0.09054(14) 0.7984(2) 0.1531(2) 0.0121(7) Uani 1 1 d . . . . . C40 C 0.05767(15) 0.8599(2) 0.0886(2) 0.0141(7) Uani 1 1 d . . . . . H40A H 0.0774 0.9124 0.0701 0.017 Uiso 1 1 calc R U . . . C41 C -0.00407(15) 0.8452(2) 0.0508(2) 0.0150(7) Uani 1 1 d . . . . . H41A H -0.0274 0.8845 0.0044 0.018 Uiso 1 1 calc R U . . . C42 C -0.03096(14) 0.7710(2) 0.0828(2) 0.0138(7) Uani 1 1 d . . . . . H42A H -0.0737 0.7602 0.0596 0.017 Uiso 1 1 calc R U . . . C43 C 0.00433(14) 0.7132(2) 0.1481(2) 0.0135(7) Uani 1 1 d . . . . . H43A H -0.0151 0.6638 0.1699 0.016 Uiso 1 1 calc R U . . . C44 C 0.08961(15) 0.4937(2) 0.1342(2) 0.0142(7) Uani 1 1 d . . . . . C45 C 0.08146(16) 0.4479(3) 0.0598(2) 0.0197(8) Uani 1 1 d . . . . . H45A H 0.0494 0.4003 0.0364 0.024 Uiso 1 1 calc R U . . . C46 C 0.12061(16) 0.4724(3) 0.0201(2) 0.0222(8) Uani 1 1 d . . . . . H46A H 0.1152 0.4437 -0.0319 0.027 Uiso 1 1 calc R U . . . C47 C 0.16773(16) 0.5393(3) 0.0575(2) 0.0202(8) Uani 1 1 d . . . . . H47A H 0.1957 0.5570 0.0319 0.024 Uiso 1 1 calc R U . . . C48 C 0.17361(15) 0.5801(3) 0.1321(2) 0.0176(8) Uani 1 1 d . . . . . H48A H 0.2072 0.6238 0.1582 0.021 Uiso 1 1 calc R U . . . H1V H 0.6298(17) 0.144(3) 0.541(2) 0.021 Uiso 1 1 d . U . . . H1W H 0.6638(16) 0.135(3) 0.499(2) 0.021 Uiso 1 1 d . U . . . H3V H 0.1178(17) 0.200(3) 0.222(2) 0.021 Uiso 1 1 d . U . . . H3W H 0.130(2) 0.209(3) 0.158(3) 0.021 Uiso 1 1 d . U . . . H2V H 0.6086(18) 0.141(3) 0.213(2) 0.021 Uiso 1 1 d . U . . . H2W H 0.6433(16) 0.137(3) 0.294(2) 0.021 Uiso 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 0.0048(2) 0.0054(2) 0.0060(2) 0.00027(18) 0.00075(18) -0.00033(17) Fe1A 0.0067(2) 0.0112(2) 0.0094(2) 0.00071(19) 0.0023(2) -0.00095(18) N1 0.0086(14) 0.0102(14) 0.0083(14) 0.0010(11) 0.0044(12) 0.0010(11) N2 0.0075(13) 0.0078(14) 0.0075(14) -0.0007(11) 0.0015(11) -0.0015(11) N3 0.0077(14) 0.0108(14) 0.0112(15) -0.0016(11) 0.0030(12) 0.0010(11) N4 0.0088(14) 0.0080(14) 0.0074(14) 0.0005(11) 0.0006(12) -0.0001(11) N5 0.0083(14) 0.0056(13) 0.0069(14) 0.0031(11) 0.0004(11) 0.0005(11) N6 0.0100(14) 0.0076(14) 0.0111(14) -0.0007(11) 0.0032(12) 0.0001(11) N1A 0.0091(14) 0.0124(14) 0.0115(15) 0.0004(12) 0.0020(12) -0.0013(11) N3A 0.0110(14) 0.0146(15) 0.0102(15) -0.0013(12) 0.0025(12) -0.0017(11) N2A 0.0095(14) 0.0156(15) 0.0145(15) 0.0007(12) 0.0053(12) -0.0012(12) N4A 0.0100(14) 0.0148(15) 0.0135(15) 0.0016(12) 0.0012(12) -0.0022(12) N5A 0.0111(14) 0.0128(15) 0.0091(15) 0.0014(11) 0.0025(12) -0.0009(11) N6A 0.0086(14) 0.0120(15) 0.0131(15) -0.0018(12) 0.0033(12) -0.0011(11) O1 0.0327(17) 0.0178(15) 0.0217(15) 0.0014(12) 0.0131(13) 0.0060(12) O2 0.072(2) 0.0238(18) 0.0180(18) 0.0003(13) -0.0062(16) -0.0190(16) O3A 0.10(2) 0.021(4) 0.044(7) -0.011(4) 0.041(11) -0.007(6) O3B 0.081(16) 0.029(6) 0.038(6) 0.007(5) 0.038(9) 0.023(8) C1 0.0098(17) 0.0078(17) 0.0148(18) 0.0037(14) 0.0020(14) -0.0003(13) C2 0.0099(17) 0.0090(17) 0.0128(18) 0.0020(14) 0.0029(14) -0.0004(13) C3 0.0120(17) 0.0152(18) 0.0055(16) 0.0013(14) 0.0015(14) -0.0003(14) C4 0.0117(17) 0.0166(18) 0.0078(17) -0.0009(14) 0.0042(14) -0.0015(14) C5 0.0064(16) 0.0131(18) 0.0151(18) 0.0034(14) 0.0054(14) -0.0008(13) C6 0.0064(16) 0.0200(19) 0.0153(18) 0.0033(15) 0.0063(15) 0.0008(14) C7 0.0104(17) 0.0223(19) 0.0146(19) -0.0026(15) 0.0054(15) 0.0043(14) C8 0.0057(16) 0.0107(17) 0.0125(18) 0.0009(14) 0.0007(14) 0.0000(13) C9 0.0059(16) 0.0113(17) 0.0119(17) 0.0016(14) -0.0010(14) -0.0019(13) Cl1 0.0116(4) 0.0202(5) 0.0144(4) -0.0032(4) 0.0009(4) -0.0013(3) Cl2 0.0159(4) 0.0202(5) 0.0188(5) -0.0050(4) 0.0037(4) -0.0005(3) Cl3 0.0155(4) 0.0120(4) 0.0152(4) -0.0030(3) 0.0065(4) -0.0021(3) Cl4 0.0126(4) 0.0549(7) 0.0168(5) 0.0032(4) 0.0051(4) 0.0023(4) C10 0.0067(16) 0.0100(17) 0.0117(18) -0.0015(14) -0.0001(14) -0.0042(13) C11 0.0111(17) 0.0091(17) 0.0089(17) -0.0007(13) 0.0015(14) -0.0028(13) C12 0.0133(17) 0.0079(17) 0.0129(18) 0.0059(14) 0.0028(15) -0.0024(13) C13 0.0201(19) 0.0065(17) 0.0150(19) -0.0037(14) 0.0026(15) -0.0020(14) C14 0.0173(18) 0.0094(18) 0.0160(19) -0.0041(14) 0.0050(15) 0.0036(14) C15 0.0087(16) 0.0136(17) 0.0079(17) -0.0002(14) 0.0024(14) 0.0015(13) C16 0.0205(19) 0.0119(18) 0.0134(18) 0.0053(14) 0.0087(16) 0.0029(14) C17 0.0154(18) 0.024(2) 0.0117(18) 0.0071(15) 0.0031(15) 0.0081(15) C18 0.0136(18) 0.0197(19) 0.0142(19) -0.0007(15) 0.0025(15) 0.0025(15) C19 0.0109(17) 0.0144(18) 0.0113(18) 0.0006(14) 0.0036(14) 0.0005(14) C20 0.0088(16) 0.0090(17) 0.0063(16) 0.0016(13) 0.0011(13) 0.0017(13) C21 0.0078(16) 0.0091(17) 0.0088(17) -0.0015(13) -0.0039(14) -0.0017(13) C22 0.0165(18) 0.0146(18) 0.0092(18) -0.0018(14) 0.0027(15) 0.0029(14) C23 0.0115(17) 0.0131(18) 0.0133(18) -0.0002(14) 0.0072(15) 0.0002(13) C24 0.0092(17) 0.0102(17) 0.0109(17) 0.0013(13) 0.0017(14) -0.0014(13) C25 0.0126(18) 0.025(2) 0.0094(18) 0.0037(15) 0.0034(15) -0.0002(15) C26 0.0163(18) 0.027(2) 0.0096(18) -0.0025(15) 0.0023(15) 0.0009(16) C27 0.0121(18) 0.023(2) 0.0157(19) -0.0021(15) 0.0056(15) -0.0002(15) C28 0.0116(17) 0.0211(19) 0.0171(19) -0.0013(15) 0.0081(15) -0.0024(14) C29 0.0128(17) 0.0163(18) 0.0158(19) 0.0011(14) 0.0064(15) -0.0022(14) C30 0.0172(19) 0.0126(18) 0.023(2) 0.0033(15) 0.0081(16) -0.0012(14) C31 0.0128(18) 0.0150(18) 0.0165(19) 0.0025(15) 0.0007(15) 0.0039(14) C32 0.0066(17) 0.0218(19) 0.0176(19) 0.0037(15) 0.0028(15) 0.0024(14) C33 0.0071(17) 0.025(2) 0.0151(19) 0.0011(16) 0.0006(15) -0.0051(15) C34 0.0098(17) 0.0176(18) 0.0159(19) 0.0006(15) 0.0016(15) -0.0027(14) C35 0.0179(19) 0.0139(18) 0.022(2) -0.0058(15) 0.0060(16) -0.0046(15) C36 0.0183(19) 0.0126(18) 0.0178(19) -0.0033(15) 0.0057(16) -0.0009(14) C37 0.0176(18) 0.0190(19) 0.0147(19) -0.0031(15) 0.0081(16) -0.0034(15) C38 0.0131(18) 0.0163(19) 0.0156(19) 0.0074(15) 0.0011(15) -0.0016(14) C39 0.0113(17) 0.0143(18) 0.0109(18) 0.0006(14) 0.0044(14) 0.0016(14) C40 0.0151(18) 0.0144(18) 0.0144(18) 0.0024(14) 0.0071(15) 0.0010(14) C41 0.0154(18) 0.0193(19) 0.0100(18) -0.0007(14) 0.0041(15) 0.0048(14) C42 0.0079(17) 0.0184(19) 0.0126(18) -0.0041(15) 0.0005(14) 0.0019(14) C43 0.0095(17) 0.0132(17) 0.0165(19) -0.0052(14) 0.0034(15) -0.0036(14) C44 0.0160(18) 0.0134(18) 0.0115(18) 0.0005(14) 0.0030(15) 0.0015(14) C45 0.022(2) 0.018(2) 0.017(2) -0.0063(15) 0.0048(16) 0.0003(15) C46 0.033(2) 0.021(2) 0.014(2) -0.0012(16) 0.0102(17) 0.0061(17) C47 0.022(2) 0.025(2) 0.018(2) 0.0029(16) 0.0114(17) 0.0043(16) C48 0.0150(18) 0.022(2) 0.0169(19) 0.0021(16) 0.0067(16) 0.0009(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N6 Fe1 N5 86.54(10) N6 Fe1 N2 175.66(10) N5 Fe1 N2 93.78(10) N6 Fe1 N3 93.51(10) N5 Fe1 N3 175.61(10) N2 Fe1 N3 86.51(10) N6 Fe1 N1 100.11(10) N5 Fe1 N1 80.46(10) N2 Fe1 N1 84.21(10) N3 Fe1 N1 95.22(10) N6 Fe1 N4 81.05(10) N5 Fe1 N4 100.33(10) N2 Fe1 N4 94.65(10) N3 Fe1 N4 84.01(10) N1 Fe1 N4 178.66(10) N5A Fe1A N6A 85.25(10) N5A Fe1A N2A 93.73(11) N6A Fe1A N2A 175.49(10) N5A Fe1A N3A 175.53(10) N6A Fe1A N3A 93.70(11) N2A Fe1A N3A 87.65(11) N5A Fe1A N4A 99.79(10) N6A Fe1A N4A 81.06(10) N2A Fe1A N4A 94.80(10) N3A Fe1A N4A 84.31(10) N5A Fe1A N1A 81.30(10) N6A Fe1A N1A 99.99(10) N2A Fe1A N1A 84.18(10) N3A Fe1A N1A 94.62(10) N4A Fe1A N1A 178.56(11) C11 N1 C1 108.3(2) C11 N1 C5 107.2(2) C1 N1 C5 106.7(2) C11 N1 Fe1 106.58(17) C1 N1 Fe1 108.47(17) C5 N1 Fe1 119.24(19) C2 N2 C8 106.1(2) C2 N2 C3 108.0(2) C8 N2 C3 110.5(2) C2 N2 Fe1 105.99(18) C8 N2 Fe1 115.75(19) C3 N2 Fe1 110.03(18) C14 N3 C7 107.1(2) C14 N3 C4 108.5(2) C7 N3 C4 110.0(2) C14 N3 Fe1 106.17(19) C7 N3 Fe1 115.32(19) C4 N3 Fe1 109.49(18) C12 N4 C10 107.6(2) C12 N4 C13 108.8(2) C10 N4 C13 106.5(2) C12 N4 Fe1 105.87(18) C10 N4 Fe1 119.66(19) C13 N4 Fe1 108.13(18) C24 N5 C20 116.0(3) C24 N5 Fe1 129.9(2) C20 N5 Fe1 114.08(19) C19 N6 C15 116.1(3) C19 N6 Fe1 129.2(2) C15 N6 Fe1 114.6(2) C37 N1A C29 107.2(2) C37 N1A C30 109.2(3) C29 N1A C30 106.3(2) C37 N1A Fe1A 106.24(18) C29 N1A Fe1A 119.9(2) C30 N1A Fe1A 107.75(18) C36 N3A C27 106.4(2) C36 N3A C26 108.5(3) C27 N3A C26 110.5(2) C36 N3A Fe1A 105.96(19) C27 N3A Fe1A 115.6(2) C26 N3A Fe1A 109.52(19) C31 N2A C32 106.4(2) C31 N2A C25 108.7(2) C32 N2A C25 109.7(2) C31 N2A Fe1A 106.67(19) C32 N2A Fe1A 115.7(2) C25 N2A Fe1A 109.35(19) C38 N4A C34 107.7(2) C38 N4A C35 108.4(3) C34 N4A C35 106.3(2) C38 N4A Fe1A 106.19(19) C34 N4A Fe1A 119.9(2) C35 N4A Fe1A 107.94(18) C44 N5A C48 116.0(3) C44 N5A Fe1A 114.2(2) C48 N5A Fe1A 129.3(2) C39 N6A C43 116.1(3) C39 N6A Fe1A 114.6(2) C43 N6A Fe1A 129.1(2) H1V O1 H1W 108(4) H2V O2 H2W 112(4) H3V O3A H3W 84(4) H3V O3B H3W 91(4) N1 C1 C2 112.0(2) N1 C1 H1A 109.2 C2 C1 H1A 109.2 N1 C1 H1B 109.2 C2 C1 H1B 109.2 H1A C1 H1B 107.9 N2 C2 C1 109.8(2) N2 C2 H2A 109.7 C1 C2 H2A 109.7 N2 C2 H2B 109.7 C1 C2 H2B 109.7 H2A C2 H2B 108.2 N2 C3 C4 112.3(2) N2 C3 H3A 109.1 C4 C3 H3A 109.1 N2 C3 H3B 109.1 C4 C3 H3B 109.1 H3A C3 H3B 107.9 N3 C4 C3 113.0(2) N3 C4 H4A 109.0 C3 C4 H4A 109.0 N3 C4 H4B 109.0 C3 C4 H4B 109.0 H4A C4 H4B 107.8 N1 C5 C6 114.3(2) N1 C5 H5A 108.7 C6 C5 H5A 108.7 N1 C5 H5B 108.7 C6 C5 H5B 108.7 H5A C5 H5B 107.6 C5 C6 C7 113.4(3) C5 C6 H6A 108.9 C7 C6 H6A 108.9 C5 C6 H6B 108.9 C7 C6 H6B 108.9 H6A C6 H6B 107.7 N3 C7 C6 115.4(3) N3 C7 H7A 108.4 C6 C7 H7A 108.4 N3 C7 H7B 108.4 C6 C7 H7B 108.4 H7A C7 H7B 107.5 N2 C8 C9 115.2(2) N2 C8 H8A 108.5 C9 C8 H8A 108.5 N2 C8 H8B 108.5 C9 C8 H8B 108.5 H8A C8 H8B 107.5 C10 C9 C8 113.4(3) C10 C9 H9A 108.9 C8 C9 H9A 108.9 C10 C9 H9B 108.9 C8 C9 H9B 108.9 H9A C9 H9B 107.7 N4 C10 C9 114.5(2) N4 C10 H10A 108.6 C9 C10 H10A 108.6 N4 C10 H10B 108.6 C9 C10 H10B 108.6 H10A C10 H10B 107.6 N1 C11 C20 110.0(2) N1 C11 H11A 109.7 C20 C11 H11A 109.7 N1 C11 H11B 109.7 C20 C11 H11B 109.7 H11A C11 H11B 108.2 N4 C12 C15 110.8(2) N4 C12 H12A 109.5 C15 C12 H12A 109.5 N4 C12 H12B 109.5 C15 C12 H12B 109.5 H12A C12 H12B 108.1 N4 C13 C14 112.0(3) N4 C13 H13A 109.2 C14 C13 H13A 109.2 N4 C13 H13B 109.2 C14 C13 H13B 109.2 H13A C13 H13B 107.9 N3 C14 C13 109.3(3) N3 C14 H14A 109.8 C13 C14 H14A 109.8 N3 C14 H14B 109.8 C13 C14 H14B 109.8 H14A C14 H14B 108.3 N6 C15 C16 123.3(3) N6 C15 C12 115.6(3) C16 C15 C12 121.1(3) C17 C16 C15 119.0(3) C17 C16 H16A 120.5 C15 C16 H16A 120.5 C18 C17 C16 118.4(3) C18 C17 H17A 120.8 C16 C17 H17A 120.8 C19 C18 C17 119.4(3) C19 C18 H18A 120.3 C17 C18 H18A 120.3 N6 C19 C18 123.6(3) N6 C19 H19A 118.2 C18 C19 H19A 118.2 N5 C20 C21 122.7(3) N5 C20 C11 116.1(3) C21 C20 C11 121.1(3) C20 C21 C22 120.0(3) C20 C21 H21A 120.0 C22 C21 H21A 120.0 C23 C22 C21 117.5(3) C23 C22 H22A 121.3 C21 C22 H22A 121.3 C24 C23 C22 119.6(3) C24 C23 H23A 120.2 C22 C23 H23A 120.2 N5 C24 C23 124.0(3) N5 C24 H24A 118.0 C23 C24 H24A 118.0 N2A C25 C26 113.8(3) N2A C25 H25A 108.8 C26 C25 H25A 108.8 N2A C25 H25B 108.8 C26 C25 H25B 108.8 H25A C25 H25B 107.7 N3A C26 C25 113.4(3) N3A C26 H26A 108.9 C25 C26 H26A 108.9 N3A C26 H26B 108.9 C25 C26 H26B 108.9 H26A C26 H26B 107.7 N3A C27 C28 114.8(3) N3A C27 H27A 108.6 C28 C27 H27A 108.6 N3A C27 H27B 108.6 C28 C27 H27B 108.6 H27A C27 H27B 107.6 C27 C28 C29 113.6(3) C27 C28 H28A 108.8 C29 C28 H28A 108.8 C27 C28 H28B 108.8 C29 C28 H28B 108.8 H28A C28 H28B 107.7 N1A C29 C28 114.1(3) N1A C29 H29A 108.7 C28 C29 H29A 108.7 N1A C29 H29B 108.7 C28 C29 H29B 108.7 H29A C29 H29B 107.6 N1A C30 C31 111.8(3) N1A C30 H30A 109.3 C31 C30 H30A 109.3 N1A C30 H30B 109.3 C31 C30 H30B 109.3 H30A C30 H30B 107.9 N2A C31 C30 109.0(3) N2A C31 H31A 109.9 C30 C31 H31A 109.9 N2A C31 H31B 109.9 C30 C31 H31B 109.9 H31A C31 H31B 108.3 N2A C32 C33 114.5(3) N2A C32 H32A 108.6 C33 C32 H32A 108.6 N2A C32 H32B 108.6 C33 C32 H32B 108.6 H32A C32 H32B 107.6 C32 C33 C34 113.6(3) C32 C33 H33A 108.8 C34 C33 H33A 108.8 C32 C33 H33B 108.8 C34 C33 H33B 108.8 H33A C33 H33B 107.7 N4A C34 C33 113.9(3) N4A C34 H34A 108.8 C33 C34 H34A 108.8 N4A C34 H34B 108.8 C33 C34 H34B 108.8 H34A C34 H34B 107.7 C36 C35 N4A 111.3(3) C36 C35 H35A 109.4 N4A C35 H35A 109.4 C36 C35 H35B 109.4 N4A C35 H35B 109.4 H35A C35 H35B 108.0 N3A C36 C35 110.1(3) N3A C36 H36A 109.6 C35 C36 H36A 109.6 N3A C36 H36B 109.6 C35 C36 H36B 109.6 H36A C36 H36B 108.2 N1A C37 C44 111.2(3) N1A C37 H37A 109.4 C44 C37 H37A 109.4 N1A C37 H37B 109.4 C44 C37 H37B 109.4 H37A C37 H37B 108.0 N4A C38 C39 111.2(3) N4A C38 H38A 109.4 C39 C38 H38A 109.4 N4A C38 H38B 109.4 C39 C38 H38B 109.4 H38A C38 H38B 108.0 N6A C39 C40 123.5(3) N6A C39 C38 116.5(3) C40 C39 C38 120.0(3) C39 C40 C41 119.7(3) C39 C40 H40A 120.2 C41 C40 H40A 120.2 C40 C41 C42 117.7(3) C40 C41 H41A 121.2 C42 C41 H41A 121.2 C43 C42 C41 119.7(3) C43 C42 H42A 120.2 C41 C42 H42A 120.2 N6A C43 C42 123.3(3) N6A C43 H43A 118.4 C42 C43 H43A 118.4 N5A C44 C45 123.3(3) N5A C44 C37 116.7(3) C45 C44 C37 119.9(3) C46 C45 C44 119.0(3) C46 C45 H45A 120.5 C44 C45 H45A 120.5 C47 C46 C45 118.7(3) C47 C46 H46A 120.7 C45 C46 H46A 120.7 C48 C47 C46 119.0(3) C48 C47 H47A 120.5 C46 C47 H47A 120.5 N5A C48 C47 123.9(3) N5A C48 H48A 118.1 C47 C48 H48A 118.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N6 2.017(3) Fe1 N5 2.034(2) Fe1 N2 2.036(3) Fe1 N3 2.041(3) Fe1 N1 2.092(3) Fe1 N4 2.099(3) Fe1A N5A 2.004(3) Fe1A N6A 2.015(3) Fe1A N2A 2.022(3) Fe1A N3A 2.032(3) Fe1A N4A 2.111(3) Fe1A N1A 2.108(3) N1 C11 1.483(4) N1 C1 1.499(4) N1 C5 1.501(4) N2 C2 1.483(4) N2 C8 1.491(4) N2 C3 1.504(4) N3 C14 1.480(4) N3 C7 1.493(4) N3 C4 1.507(4) N4 C12 1.485(4) N4 C10 1.494(4) N4 C13 1.506(4) N5 C24 1.352(4) N5 C20 1.358(4) N6 C19 1.343(4) N6 C15 1.355(4) N1A C37 1.484(4) N1A C29 1.493(4) N1A C30 1.507(4) N3A C36 1.487(4) N3A C27 1.491(4) N3A C26 1.500(4) N2A C31 1.488(4) N2A C32 1.494(4) N2A C25 1.508(4) N4A C38 1.489(4) N4A C34 1.493(4) N4A C35 1.514(4) N5A C44 1.352(4) N5A C48 1.353(4) N6A C39 1.350(4) N6A C43 1.354(4) O1 H1V 0.75(4) O1 H1W 0.83(4) O2 H2V 0.74(4) O2 H2W 0.89(4) O3A H3V 1.08(4) O3A H3W 0.77(4) O3B H3V 0.95(4) O3B H3W 0.82(4) C1 C2 1.509(4) C1 H1A 0.9900 C1 H1B 0.9900 C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.515(4) C3 H3A 0.9900 C3 H3B 0.9900 C4 H4A 0.9900 C4 H4B 0.9900 C5 C6 1.511(4) C5 H5A 0.9900 C5 H5B 0.9900 C6 C7 1.511(4) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7A 0.9900 C7 H7B 0.9900 C8 C9 1.515(4) C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.515(4) C9 H9A 0.9900 C9 H9B 0.9900 C10 H10A 0.9900 C10 H10B 0.9900 C11 C20 1.484(4) C11 H11A 0.9900 C11 H11B 0.9900 C12 C15 1.498(4) C12 H12A 0.9900 C12 H12B 0.9900 C13 C14 1.509(4) C13 H13A 0.9900 C13 H13B 0.9900 C14 H14A 0.9900 C14 H14B 0.9900 C15 C16 1.378(4) C16 C17 1.381(5) C16 H16A 0.9500 C17 C18 1.372(5) C17 H17A 0.9500 C18 C19 1.374(4) C18 H18A 0.9500 C19 H19A 0.9500 C20 C21 1.381(4) C21 C22 1.385(4) C21 H21A 0.9500 C22 C23 1.380(4) C22 H22A 0.9500 C23 C24 1.369(4) C23 H23A 0.9500 C24 H24A 0.9500 C25 C26 1.518(5) C25 H25A 0.9900 C25 H25B 0.9900 C26 H26A 0.9900 C26 H26B 0.9900 C27 C28 1.515(5) C27 H27A 0.9900 C27 H27B 0.9900 C28 C29 1.519(4) C28 H28A 0.9900 C28 H28B 0.9900 C29 H29A 0.9900 C29 H29B 0.9900 C30 C31 1.506(4) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31A 0.9900 C31 H31B 0.9900 C32 C33 1.516(5) C32 H32A 0.9900 C32 H32B 0.9900 C33 C34 1.517(4) C33 H33A 0.9900 C33 H33B 0.9900 C34 H34A 0.9900 C34 H34B 0.9900 C35 C36 1.507(4) C35 H35A 0.9900 C35 H35B 0.9900 C36 H36A 0.9900 C36 H36B 0.9900 C37 C44 1.501(4) C37 H37A 0.9900 C37 H37B 0.9900 C38 C39 1.501(4) C38 H38A 0.9900 C38 H38B 0.9900 C39 C40 1.374(4) C40 C41 1.377(5) C40 H40A 0.9500 C41 C42 1.385(5) C41 H41A 0.9500 C42 C43 1.372(4) C42 H42A 0.9500 C43 H43A 0.9500 C44 C45 1.382(5) C45 C46 1.381(5) C45 H45A 0.9500 C46 C47 1.380(5) C46 H46A 0.9500 C47 C48 1.371(5) C47 H47A 0.9500 C48 H48A 0.9500 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 C1 H1B O1 0.99 2.42 3.369(4) 160.0 3_656 C2 H2A Cl3 0.99 2.76 3.479(3) 130.1 2_645 C3 H3A Cl3 0.99 2.92 3.744(3) 141.7 4_566 C5 H5B Cl1 0.99 2.72 3.617(3) 151.5 . C6 H6B Cl4 0.99 2.67 3.632(3) 165.0 . C9 H9B Cl2 0.99 2.94 3.908(3) 167.2 . C9 H9A Cl3 0.99 2.92 3.722(3) 138.2 4_566 C11 H11B Cl2 0.99 2.93 3.840(3) 153.9 2_645 C11 H11A Cl1 0.99 2.93 3.799(3) 146.9 . C13 H13A O2 0.99 2.31 3.221(4) 153.3 2_655 C16 H16A O1 0.95 2.50 3.398(4) 157.2 2_655 C19 H19A Cl1 0.95 2.69 3.447(3) 137.5 . C21 H21A Cl2 0.95 2.84 3.653(3) 143.7 2_645 C23 H23A Cl3 0.95 2.88 3.493(3) 123.7 . C24 H24A Cl3 0.95 2.82 3.473(3) 127.0 . C25 H25B Cl1 0.99 2.55 3.409(3) 144.4 4_566 C26 H26B Cl2 0.99 2.75 3.590(3) 142.8 3_666 C29 H29B Cl4 0.99 2.65 3.588(3) 158.2 2 C30 H30A O3A 0.99 2.62 3.355(17) 131.3 . C30 H30A O3B 0.99 2.61 3.46(2) 144.5 . C33 H33A Cl3 0.99 2.82 3.771(3) 160.8 2_655 C35 H35B Cl4 0.99 2.96 3.785(4) 141.5 1_565 C40 H40A Cl1 0.95 2.67 3.591(3) 162.8 1_565 C43 H43A Cl4 0.95 2.72 3.505(3) 140.3 2 C48 H48A Cl2 0.95 2.97 3.641(3) 129.1 2_655 O1 H1V Cl3 0.75(4) 2.55(4) 3.286(3) 171(4) 4_566 O1 H1W Cl2 0.83(4) 2.42(4) 3.247(3) 177(3) . O2 H2W Cl2 0.89(4) 2.30(4) 3.196(3) 179(3) . O2 H2V Cl3 0.74(4) 2.51(4) 3.243(3) 172(4) . O3A H3V Cl4 1.08(4) 2.22(4) 3.187(13) 147(4) . O3B H3V Cl4 0.95(4) 2.22(4) 3.152(10) 168(4) . O3A H3W Cl1 0.77(4) 2.52(4) 3.243(13) 157(7) . O3B H3W Cl1 0.82(4) 2.52(4) 3.214(12) 144(6) .