#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:50:00 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242543 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132597.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_4132597 loop_ _publ_author_name 'Schwamb, C. Benjamin' 'Fitzpatrick, Keegan P.' 'Brueckner, Alexander C.' 'Richardson, H. Camille' 'Cheong, Paul H.-Y.' 'Scheidt, Karl A.' _publ_section_title ; Enantioselective Synthesis of \a-Amidoboronates Catalyzed by Planar-Chiral NHC-Cu(I) Complexes. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10644 _journal_page_last 10648 _journal_paper_doi 10.1021/jacs.8b05045 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C34 H34 Cl Cu Fe N2 O' _chemical_formula_sum 'C34 H34 Cl Cu Fe N2 O' _chemical_formula_weight 641.47 _space_group_crystal_system monoclinic _space_group_IT_number 3 _space_group_name_Hall 'P 2y' _space_group_name_H-M_alt 'P 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-08-29 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 96.359(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.3929(16) _cell_length_b 9.5949(8) _cell_length_c 18.9878(17) _cell_measurement_reflns_used 2846 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 58.331 _cell_measurement_theta_min 2.341 _cell_volume 3330.3(5) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection 'APEX2 V2014.11-0 (Bruker, 2014)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 249.99 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'MX optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_unetI/netI 0.0974 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 22492 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 65.077 _diffrn_reflns_theta_max 65.077 _diffrn_reflns_theta_min 2.341 _diffrn_source microsource _exptl_absorpt_coefficient_mu 5.217 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0831 before and 0.0500 after correction. The Ratio of minimum to maximum transmission is 0.8496. The \l/2 correction factor is Not present.' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.279 _exptl_crystal_description needle _exptl_crystal_F_000 1328 _exptl_crystal_recrystallization_method 'The material was recrystallised from --- by as supplied' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.014 _refine_diff_density_max 0.368 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Flack x determined using 1672 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.003(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 734 _refine_ls_number_reflns 11142 _refine_ls_number_restraints 889 _refine_ls_restrained_S_all 0.978 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0691 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1630 _refine_ls_wR_factor_ref 0.2034 _reflns_Friedel_coverage 0.848 _reflns_Friedel_fraction_full 0.964 _reflns_Friedel_fraction_max 0.964 _reflns_number_gt 5769 _reflns_number_total 11142 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05045_si_002.cif _cod_data_source_block cx1054a _cod_database_code 4132597 _shelx_shelxl_version_number 2017/1 _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_max 0.931 _shelx_estimated_absorpt_t_min 0.508 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3.a Me refined with riding coordinates: C9(H9A,H9B,H9C) 3.b Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C14(H14), C17(H17), C19(H19), C24(H24), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C12A(H12A), C13A(H13A), C14A(H14A), C17A(H17A), C19A(H19A), C24A(H24A), C26A(H26A), C27A(H27A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A) 3.c Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB, H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C21A(H21D,H21E,H21F), C28A(H28D,H28E,H28F) ; _smtbx_masks_special_details ; The solvent masking procedure as implemented in Olex2 was used to remove the electronic contribution of solvent molecules from the refinement. As the exact solvent content is not known, only the atoms used in the refinement model are reported in the formula here. Total solvent accessible volume / cell = 440.2 Ang^3^ [13.2%] Total electron count / cell = 67.4 ; _shelx_res_file ; TITL cx1054a_a.res in P2 cx1054a.res created by SHELXL-2017/1 at 10:22:20 on 29-Aug-2017 REM Old TITL cx1054a in P2 REM SHELXT solution in P2 REM R1 0.188, Rweak 0.033, Alpha 0.055, Orientation as input REM Flack x = 0.192 ( 0.011 ) from Parsons' quotients REM Formula found by SHELXT: C60 N10 O2 Cl2 Fe3 Cu CELL 1.54178 18.3929 9.5949 18.9878 90 96.3594 90 ZERR 4 0.0016 0.0008 0.0017 0 0.0049 0 LATT -1 SYMM -X,+Y,-Z SFAC C H N O Cl Fe Cu UNIT 136 136 8 4 4 4 4 RIGU 0.001 0.001 L.S. 20 PLAN 20 SIZE 0.014 0.025 0.15 TEMP -23.16 BOND $H ABIN fmap 2 acta SHEL 9999 0.85 REM REM REM WGHT 0.090200 FVAR 0.13244 CU1 7 0.012616 0.428984 0.839724 11.00000 0.14026 0.04751 = 0.08347 -0.00622 -0.01245 -0.01129 FE1 6 0.189690 0.252978 1.001850 11.00000 0.06143 0.14719 = 0.06918 -0.02033 0.01109 -0.02390 CL1 5 -0.003831 0.642162 0.839898 11.00000 0.34984 0.04753 = 0.14344 -0.00531 -0.09603 -0.00080 O1 4 -0.132881 0.038632 0.749378 11.00000 0.08049 0.07659 = 0.07110 -0.00227 -0.00110 -0.02037 N1 3 0.053618 0.162848 0.900731 11.00000 0.06362 0.05483 = 0.07086 -0.01055 0.00697 -0.00332 N2 3 0.002036 0.137415 0.794614 11.00000 0.07217 0.05143 = 0.07209 -0.01014 0.00159 -0.00333 C1 1 0.247289 0.259144 0.917028 11.00000 0.06183 0.20396 = 0.09225 -0.01852 0.02223 -0.02578 C2 1 0.256517 0.381530 0.952411 11.00000 0.10234 0.20203 = 0.11312 -0.01923 0.04096 -0.05789 C3 1 0.283948 0.368650 1.021233 11.00000 0.08489 0.27041 = 0.11709 -0.05006 0.02279 -0.08127 C4 1 0.298070 0.224308 1.030109 11.00000 0.06025 0.29883 = 0.10615 -0.00107 0.00942 -0.02690 C5 1 0.273915 0.153489 0.963492 11.00000 0.06124 0.22322 = 0.11951 -0.00668 0.02556 0.00259 C6 1 0.219154 0.237546 0.840058 11.00000 0.11258 0.28827 = 0.08571 -0.02580 0.02571 -0.02948 AFIX 137 H6A 2 0.197338 0.145692 0.833952 11.00000 -1.50000 H6B 2 0.259394 0.245256 0.811304 11.00000 -1.50000 H6C 2 0.182651 0.307815 0.825465 11.00000 -1.50000 AFIX 0 C7 1 0.227441 0.525722 0.919511 11.00000 0.19689 0.19173 = 0.23466 0.02462 0.09283 -0.05338 AFIX 137 H7A 2 0.187995 0.508738 0.882203 11.00000 -1.50000 H7B 2 0.266977 0.574094 0.900012 11.00000 -1.50000 H7C 2 0.209572 0.582507 0.956200 11.00000 -1.50000 AFIX 0 C8 1 0.301228 0.479924 1.079522 11.00000 0.18505 0.39250 = 0.19535 -0.14113 0.06339 -0.19136 AFIX 137 H8A 2 0.264985 0.553630 1.073367 11.00000 -1.50000 H8B 2 0.349415 0.518667 1.076068 11.00000 -1.50000 H8C 2 0.300131 0.437323 1.125721 11.00000 -1.50000 AFIX 0 C9 1 0.328200 0.162694 1.097583 11.00000 0.09843 0.51618 = 0.12581 0.05070 0.00844 0.05898 AFIX 33 H9A 2 0.333469 0.062877 1.091837 11.00000 -1.50000 H9B 2 0.375674 0.203498 1.112459 11.00000 -1.50000 H9C 2 0.295430 0.180860 1.133185 11.00000 -1.50000 AFIX 0 C10 1 0.278700 0.001009 0.947046 11.00000 0.14204 0.22434 = 0.23202 -0.00655 0.08227 0.04431 AFIX 137 H10A 2 0.278048 -0.052506 0.990313 11.00000 -1.50000 H10B 2 0.323802 -0.017417 0.926631 11.00000 -1.50000 H10C 2 0.237345 -0.025615 0.913564 11.00000 -1.50000 AFIX 0 C11 1 0.083609 0.209905 0.966423 11.00000 0.05627 0.07318 = 0.07103 -0.01537 0.00970 -0.00583 C12 1 0.089374 0.346872 0.995303 11.00000 0.08325 0.07958 = 0.07572 -0.02330 0.01727 -0.01725 AFIX 43 H12 2 0.075450 0.430792 0.972066 11.00000 -1.20000 AFIX 0 C13 1 0.121170 0.329740 1.067939 11.00000 0.08566 0.10517 = 0.07329 -0.02492 0.01746 -0.02492 AFIX 43 H13 2 0.132842 0.403072 1.100035 11.00000 -1.20000 AFIX 0 C14 1 0.131599 0.193987 1.082881 11.00000 0.07197 0.11359 = 0.07171 -0.01190 0.01093 -0.01539 AFIX 43 H14 2 0.150809 0.157527 1.127006 11.00000 -1.20000 AFIX 0 C15 1 0.108652 0.113257 1.020513 11.00000 0.05963 0.09100 = 0.07451 -0.00837 0.00708 0.00091 C16 1 0.104465 -0.035086 1.007209 11.00000 0.10958 0.08637 = 0.09142 0.00212 -0.01319 0.01380 C17 1 0.077612 -0.078457 0.941972 11.00000 0.15504 0.06293 = 0.10389 -0.00394 -0.03007 0.01793 AFIX 43 H17 2 0.076252 -0.174476 0.932088 11.00000 -1.20000 AFIX 0 C18 1 0.051215 0.016924 0.887519 11.00000 0.10339 0.05402 = 0.09107 -0.01082 -0.02143 0.00508 C19 1 0.018867 0.006803 0.820755 11.00000 0.10468 0.04910 = 0.09212 -0.01318 -0.02122 -0.00282 AFIX 43 H19 2 0.009246 -0.076974 0.795789 11.00000 -1.20000 AFIX 0 C20 1 0.024428 0.238707 0.844393 11.00000 0.06487 0.05166 = 0.06993 -0.00972 0.00883 -0.00708 C21 1 0.134255 -0.136052 1.065851 11.00000 0.19603 0.11011 = 0.11933 0.02032 -0.04847 0.01487 AFIX 137 H21A 2 0.184778 -0.112919 1.081630 11.00000 -1.50000 H21B 2 0.131560 -0.230620 1.047691 11.00000 -1.50000 H21C 2 0.105303 -0.128593 1.105390 11.00000 -1.50000 AFIX 0 C22 1 -0.031721 0.177059 0.726272 11.00000 0.06841 0.05575 = 0.06882 -0.01044 0.00698 -0.00282 C23 1 -0.102391 0.126958 0.704212 11.00000 0.06737 0.04764 = 0.07244 -0.00907 0.00604 0.00128 C24 1 -0.135336 0.168109 0.637653 11.00000 0.06871 0.05989 = 0.06952 -0.00918 0.00868 0.00936 AFIX 43 H24 2 -0.181987 0.133411 0.621408 11.00000 -1.20000 AFIX 0 C25 1 -0.101383 0.258218 0.595059 11.00000 0.07507 0.06406 = 0.07598 -0.00170 0.01333 0.01348 C26 1 -0.032221 0.301603 0.617350 11.00000 0.08302 0.07826 = 0.07384 -0.00250 0.01563 -0.00116 AFIX 43 H26 2 -0.007472 0.359529 0.587970 11.00000 -1.20000 AFIX 0 C27 1 0.002855 0.260666 0.684106 11.00000 0.08321 0.06794 = 0.07421 -0.00743 0.00822 -0.01607 AFIX 43 H27 2 0.050494 0.292036 0.699021 11.00000 -1.20000 AFIX 0 C28 1 -0.204400 -0.012281 0.727714 11.00000 0.08299 0.10584 = 0.09045 0.00376 -0.00294 -0.03137 AFIX 137 H28A 2 -0.206185 -0.050273 0.680213 11.00000 -1.50000 H28B 2 -0.239327 0.063396 0.728057 11.00000 -1.50000 H28C 2 -0.216519 -0.084726 0.760081 11.00000 -1.50000 AFIX 0 C29 1 -0.136488 0.298058 0.523645 11.00000 0.07935 0.08857 = 0.07533 0.00219 0.01653 0.02416 C30 1 -0.184935 0.207277 0.484040 11.00000 0.09613 0.10587 = 0.08864 -0.00897 -0.00392 0.02710 AFIX 43 H30 2 -0.197586 0.120064 0.501664 11.00000 -1.20000 AFIX 0 C31 1 -0.213369 0.254289 0.416635 11.00000 0.10185 0.15303 = 0.09305 0.00195 -0.00679 0.03976 AFIX 43 H31 2 -0.245476 0.193492 0.389705 11.00000 -1.20000 AFIX 0 C32 1 -0.200374 0.371106 0.387711 11.00000 0.10248 0.15763 = 0.09842 0.01608 0.01198 0.06121 AFIX 43 H32 2 -0.221354 0.392720 0.341601 11.00000 -1.20000 AFIX 0 C33 1 -0.156150 0.461117 0.425053 11.00000 0.11330 0.14898 = 0.09579 0.03597 0.02240 0.03963 AFIX 43 H33 2 -0.147013 0.549264 0.406301 11.00000 -1.20000 AFIX 0 C34 1 -0.122560 0.421834 0.494382 11.00000 0.10649 0.09849 = 0.08805 0.01851 0.02520 0.02844 AFIX 43 H34 2 -0.090103 0.484136 0.519848 11.00000 -1.20000 AFIX 0 CU1A 7 0.352783 0.921805 0.417883 11.00000 0.06514 0.04534 = 0.11661 -0.00272 0.00244 -0.00092 FE1A 6 0.546589 0.742270 0.323250 11.00000 0.06211 0.18042 = 0.06196 0.00377 0.00514 -0.00091 CL1A 5 0.340219 1.136581 0.419004 11.00000 0.10313 0.04353 = 0.33301 -0.01381 -0.02826 -0.00001 O1A 4 0.221972 0.536056 0.302944 11.00000 0.09074 0.09665 = 0.08953 -0.03063 0.00364 0.00288 N1A 3 0.425276 0.653818 0.414492 11.00000 0.06306 0.05280 = 0.06715 -0.00482 0.00405 0.00585 N2A 3 0.310738 0.633151 0.414544 11.00000 0.06264 0.04244 = 0.08255 0.00105 0.00163 0.00071 C1A 1 0.469033 0.736884 0.236688 11.00000 0.09409 0.25808 = 0.06249 0.00609 -0.01212 -0.01223 C2A 1 0.504972 0.877274 0.242254 11.00000 0.09365 0.24019 = 0.07474 0.03977 0.00353 0.00404 C3A 1 0.574293 0.856573 0.239656 11.00000 0.09039 0.27321 = 0.07209 0.03672 0.00740 -0.00887 C4A 1 0.592100 0.705538 0.230761 11.00000 0.11397 0.29752 = 0.06664 0.01673 0.02220 0.03447 C5A 1 0.523195 0.636491 0.231071 11.00000 0.14768 0.25424 = 0.06996 -0.03151 -0.00456 0.00537 C6A 1 0.387547 0.732956 0.238725 11.00000 0.09243 0.33315 = 0.09659 -0.00932 -0.02592 -0.03268 AFIX 137 H6AA 2 0.374997 0.654568 0.267291 11.00000 -1.50000 H6AB 2 0.363369 0.722932 0.190939 11.00000 -1.50000 H6AC 2 0.371720 0.818836 0.259260 11.00000 -1.50000 AFIX 0 C7A 1 0.465023 1.015722 0.252494 11.00000 0.19516 0.25799 = 0.11989 0.05254 0.00041 0.05911 AFIX 137 H7AA 2 0.418626 0.996815 0.270392 11.00000 -1.50000 H7AB 2 0.456365 1.063877 0.207427 11.00000 -1.50000 H7AC 2 0.494927 1.073634 0.286108 11.00000 -1.50000 AFIX 0 C8A 1 0.626436 0.988631 0.243963 11.00000 0.17151 0.34439 = 0.13837 0.07043 0.01632 -0.08950 AFIX 137 H8AA 2 0.620736 1.040634 0.286814 11.00000 -1.50000 H8AB 2 0.613629 1.047647 0.202986 11.00000 -1.50000 H8AC 2 0.676840 0.958391 0.244722 11.00000 -1.50000 AFIX 0 C9A 1 0.666226 0.667325 0.226362 11.00000 0.15341 0.51566 = 0.14784 0.00817 0.07060 0.11941 AFIX 137 H9AA 2 0.694873 0.684959 0.271504 11.00000 -1.50000 H9AB 2 0.685591 0.721919 0.189696 11.00000 -1.50000 H9AC 2 0.668735 0.569054 0.214887 11.00000 -1.50000 AFIX 0 C10A 1 0.501952 0.493301 0.222211 11.00000 0.30696 0.26269 = 0.14714 -0.06858 -0.03370 -0.02235 AFIX 137 H10D 2 0.544500 0.437297 0.215331 11.00000 -1.50000 H10E 2 0.465839 0.484282 0.181184 11.00000 -1.50000 H10F 2 0.481138 0.461411 0.264120 11.00000 -1.50000 AFIX 0 C11A 1 0.496845 0.702537 0.410959 11.00000 0.06122 0.08798 = 0.06276 -0.00569 0.00288 -0.00142 C12A 1 0.527263 0.836825 0.414820 11.00000 0.06399 0.09552 = 0.07206 0.00660 0.00269 -0.01057 AFIX 43 H12A 2 0.502104 0.921042 0.419410 11.00000 -1.20000 AFIX 0 C13A 1 0.605464 0.820469 0.410336 11.00000 0.06230 0.13095 = 0.07378 0.00844 0.00195 -0.00910 AFIX 43 H13A 2 0.639796 0.892974 0.410015 11.00000 -1.20000 AFIX 0 C14A 1 0.620442 0.677000 0.406574 11.00000 0.06228 0.13721 = 0.07175 0.00098 -0.00059 0.00398 AFIX 43 H14A 2 0.667187 0.638897 0.404180 11.00000 -1.20000 AFIX 0 C15A 1 0.553908 0.595921 0.406892 11.00000 0.06327 0.11117 = 0.07206 -0.01806 -0.00001 0.00988 C16A 1 0.537442 0.450582 0.407058 11.00000 0.07620 0.10533 = 0.11818 -0.02543 -0.00664 0.02010 C17A 1 0.470226 0.411297 0.408095 11.00000 0.08079 0.06837 = 0.16229 -0.02322 -0.00399 0.02271 AFIX 43 H17A 2 0.459069 0.315704 0.405455 11.00000 -1.20000 AFIX 0 C18A 1 0.412088 0.510080 0.413184 11.00000 0.07225 0.05051 = 0.10014 -0.00820 0.00047 0.00932 C19A 1 0.339282 0.495442 0.412235 11.00000 0.07245 0.04242 = 0.11184 0.00165 -0.00316 0.00458 AFIX 43 H19A 2 0.312701 0.411602 0.410421 11.00000 -1.20000 AFIX 0 C20A 1 0.362746 0.731004 0.414961 11.00000 0.06165 0.04469 = 0.06315 -0.00375 0.00408 0.00075 C21A 1 0.600358 0.356123 0.401681 11.00000 0.08839 0.14126 = 0.19135 -0.05885 -0.02076 0.04239 AFIX 137 H21D 2 0.622920 0.378121 0.359221 11.00000 -1.50000 H21E 2 0.583423 0.260319 0.399366 11.00000 -1.50000 H21F 2 0.635903 0.368114 0.442939 11.00000 -1.50000 AFIX 0 C22A 1 0.234390 0.665482 0.408237 11.00000 0.06128 0.04570 = 0.07376 0.00035 0.00307 -0.00181 C23A 1 0.188062 0.618202 0.349460 11.00000 0.06501 0.04972 = 0.07506 -0.00186 0.00538 -0.01224 C24A 1 0.117718 0.661737 0.338746 11.00000 0.06458 0.07825 = 0.08514 -0.00334 -0.00187 -0.00845 AFIX 43 H24A 2 0.088237 0.632389 0.297829 11.00000 -1.20000 AFIX 0 C25A 1 0.087786 0.748839 0.386675 11.00000 0.05964 0.06101 = 0.08088 0.01760 0.00704 -0.00486 C26A 1 0.132080 0.791444 0.445523 11.00000 0.06310 0.05971 = 0.08480 0.00023 0.01156 0.00034 AFIX 43 H26A 2 0.113030 0.850378 0.478516 11.00000 -1.20000 AFIX 0 C27A 1 0.205825 0.748399 0.457488 11.00000 0.06136 0.04812 = 0.07518 -0.00117 0.00601 -0.00566 AFIX 43 H27A 2 0.235172 0.776186 0.498787 11.00000 -1.20000 AFIX 0 C28A 1 0.176828 0.478851 0.244582 11.00000 0.11290 0.11755 = 0.09784 -0.04189 0.00482 -0.01598 AFIX 137 H28D 2 0.168179 0.548558 0.207603 11.00000 -1.50000 H28E 2 0.130503 0.450156 0.259874 11.00000 -1.50000 H28F 2 0.200951 0.398748 0.226387 11.00000 -1.50000 AFIX 0 C29A 1 0.010953 0.795964 0.373153 11.00000 0.06223 0.09229 = 0.10705 0.03238 0.01026 0.00344 C30A 1 -0.041312 0.718805 0.333285 11.00000 0.06340 0.11156 = 0.15320 0.03566 -0.01503 -0.00049 AFIX 43 H30A 2 -0.028499 0.631299 0.316130 11.00000 -1.20000 AFIX 0 C31A 1 -0.111570 0.765654 0.317792 11.00000 0.06998 0.16766 = 0.21506 0.06047 -0.02336 0.01630 AFIX 43 H31A 2 -0.145843 0.709350 0.290606 11.00000 -1.20000 AFIX 0 C32A 1 -0.132528 0.889784 0.340485 11.00000 0.05369 0.15653 = 0.22990 0.09243 0.02228 0.01960 AFIX 43 H32A 2 -0.180519 0.921620 0.327755 11.00000 -1.20000 AFIX 0 C33A 1 -0.082899 0.971634 0.383067 11.00000 0.07053 0.14263 = 0.20370 0.06696 0.04609 0.02955 AFIX 43 H33A 2 -0.097802 1.056833 0.401252 11.00000 -1.20000 AFIX 0 C34A 1 -0.009873 0.925385 0.398697 11.00000 0.06508 0.08718 = 0.14771 0.04207 0.03621 0.00921 AFIX 43 H34A 2 0.024514 0.981145 0.426071 11.00000 -1.20000 AFIX 0 HKLF 4 REM cx1054a_a.res in P2 REM R1 = 0.0691 for 5769 Fo > 4sig(Fo) and 0.1340 for all 11142 data REM 734 parameters refined using 889 restraints END WGHT 0.0902 0.0000 REM Highest difference peak 0.368, deepest hole -0.305, 1-sigma level 0.056 Q1 1 0.5759 0.6037 0.2380 11.00000 0.05 0.37 Q2 1 0.5949 0.7640 0.2280 11.00000 0.05 0.35 Q3 1 0.6049 0.4449 0.2214 11.00000 0.05 0.32 Q4 1 0.6304 0.5208 0.2319 11.00000 0.05 0.32 Q5 1 0.6772 0.8151 0.2385 11.00000 0.05 0.29 Q6 1 0.3163 0.0262 1.0969 11.00000 0.05 0.27 Q7 1 0.1895 0.2852 0.9968 11.00000 0.05 0.26 Q8 1 0.0115 0.5324 0.8342 11.00000 0.05 0.26 Q9 1 0.4442 0.4331 0.2344 11.00000 0.05 0.22 Q10 1 0.2871 0.1102 1.0144 11.00000 0.05 0.22 Q11 1 0.2965 0.9262 0.3924 11.00000 0.05 0.21 Q12 1 0.3010 0.2960 1.0119 11.00000 0.05 0.21 Q13 1 0.5419 0.7826 0.3308 11.00000 0.05 0.20 Q14 1 0.6703 0.7472 0.1830 11.00000 0.05 0.20 Q15 1 -0.2269 -0.0016 0.4205 11.00000 0.05 0.20 Q16 1 0.0993 -0.0674 0.9124 11.00000 0.05 0.20 Q17 1 0.2345 0.8744 0.5339 11.00000 0.05 0.20 Q18 1 -0.2388 1.0151 0.3431 11.00000 0.05 0.19 Q19 1 0.5460 0.6818 0.3183 11.00000 0.05 0.19 Q20 1 0.0889 0.1307 0.9813 11.00000 0.05 0.19 ; _shelx_res_checksum 75224 _shelx_hkl_file ; -1 0 0 42.60 0.96 -2 0 0 390.98 6.64 -2 0 0 405.23 7.03 3 0 0 14.05 0.72 -3 0 0 13.29 0.59 -3 0 0 14.10 1.03 -4 0 0 11.35 0.67 -4 0 0 15.11 1.33 -5 0 0 28.37 1.77 -6 0 0 258.81 5.97 -7 0 0 -0.05 1.01 -8 0 0 33.40 2.40 -9 0 0 213.35 6.34 -10 0 0 8.82 2.00 -11 0 0 49.26 3.44 -11 0 0 44.28 2.34 -12 0 0 5.27 1.91 -12 0 0 7.80 1.43 13 0 0 11.52 1.26 -13 0 0 6.24 2.12 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-0.8326 0.1810 20 -1 -3 -0.5246 0.8059 20 -1 -2 -0.0847 0.1920 20 0 2 -0.1830 0.1368 20 0 3 -0.4913 0.1510 20 0 4 0.3103 -0.0148 20 0 5 0.8288 -0.0563 20 0 6 0.5000 -0.0381 20 1 0 0.6268 -1.2321 20 1 2 0.3982 0.5211 20 1 3 0.6819 0.1369 20 1 4 0.5043 0.3726 20 1 5 0.4259 0.4023 20 2 0 1.0993 0.0503 20 2 1 0.6936 -0.0593 20 2 2 -0.0435 0.1946 20 2 3 0.0785 0.5022 20 2 4 -0.0548 0.0481 20 2 5 -0.2974 -0.3430 20 3 0 -0.3819 0.8477 20 3 1 -0.1203 1.0516 20 3 2 0.1229 0.5676 20 3 3 -0.3143 0.5050 20 4 0 -0.3002 -0.9455 21 -2 -5 0.5990 1.4042 21 -2 -4 0.9776 0.5643 21 -2 -3 -0.1208 -0.3412 21 -2 -2 -0.1230 -0.8993 21 -2 -1 0.4194 -0.5390 21 -1 -4 0.2379 0.7430 21 -1 -3 0.3535 -0.5376 21 -1 -2 0.1990 -0.5745 21 -1 -1 -0.5179 -0.3022 21 0 0 0.5388 0.3474 21 0 1 0.0345 0.0048 21 1 0 -1.0524 0.7677 21 1 1 -0.4618 0.4870 21 1 2 -0.0454 -0.3743 21 2 0 -0.3243 -0.2068 21 2 1 -0.7832 -0.2702 0 0 0 0.0 0.0 ; _shelx_fab_checksum 9059 _olex2_date_sample_data_collection 2017-08-28 _olex2_date_sample_submission 2017-08-18 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in Paratone oil' _olex2_submission_original_sample_id cx1054a _olex2_submission_special_instructions 'No special instructions were received' 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 Cu1 Cu 0.01262(13) 0.4290(2) 0.83972(10) 0.0923(7) Uani 1 1 d . U Fe1 Fe 0.18969(11) 0.2530(3) 1.00185(11) 0.0923(8) Uani 1 1 d . U Cl1 Cl -0.0038(5) 0.6422(4) 0.8399(3) 0.189(4) Uani 1 1 d . U O1 O -0.1329(5) 0.0386(10) 0.7494(4) 0.077(2) Uani 1 1 d . U N1 N 0.0536(5) 0.1628(10) 0.9007(5) 0.063(2) Uani 1 1 d . U N2 N 0.0020(6) 0.1374(10) 0.7946(5) 0.066(2) Uani 1 1 d . U C1 C 0.2473(8) 0.259(3) 0.9170(9) 0.118(3) Uani 1 1 d . U C2 C 0.2565(11) 0.382(3) 0.9524(11) 0.137(4) Uani 1 1 d . U C3 C 0.2839(10) 0.369(3) 1.0212(11) 0.157(4) Uani 1 1 d . U C4 C 0.2981(9) 0.224(4) 1.0301(10) 0.155(4) Uani 1 1 d . U C5 C 0.2739(9) 0.153(3) 0.9635(11) 0.133(3) Uani 1 1 d . U C6 C 0.2192(10) 0.238(3) 0.8401(9) 0.161(8) Uani 1 1 d . U H6A H 0.197338 0.145692 0.833952 0.242 Uiso 1 1 calc GR . H6B H 0.259394 0.245256 0.811304 0.242 Uiso 1 1 calc GR . H6C H 0.182651 0.307815 0.825465 0.242 Uiso 1 1 calc GR . C7 C 0.2274(15) 0.526(3) 0.9195(16) 0.203(9) Uani 1 1 d . U H7A H 0.187995 0.508738 0.882203 0.304 Uiso 1 1 calc GR . H7B H 0.266977 0.574094 0.900012 0.304 Uiso 1 1 calc GR . H7C H 0.209572 0.582507 0.956200 0.304 Uiso 1 1 calc GR . C8 C 0.3012(14) 0.480(4) 1.0795(14) 0.254(12) Uani 1 1 d . U H8A H 0.264985 0.553630 1.073367 0.382 Uiso 1 1 calc GR . H8B H 0.349415 0.518667 1.076068 0.382 Uiso 1 1 calc GR . H8C H 0.300131 0.437323 1.125721 0.382 Uiso 1 1 calc GR . C9 C 0.3282(12) 0.163(4) 1.0976(12) 0.247(11) Uani 1 1 d . U H9A H 0.333469 0.062877 1.091837 0.371 Uiso 1 1 calc R . H9B H 0.375674 0.203498 1.112459 0.371 Uiso 1 1 calc R . H9C H 0.295430 0.180860 1.133185 0.371 Uiso 1 1 calc R . C10 C 0.2787(13) 0.001(3) 0.9470(15) 0.195(9) Uani 1 1 d . U H10A H 0.278048 -0.052506 0.990313 0.292 Uiso 1 1 calc GR . H10B H 0.323802 -0.017417 0.926631 0.292 Uiso 1 1 calc GR . H10C H 0.237345 -0.025615 0.913564 0.292 Uiso 1 1 calc GR . C11 C 0.0836(6) 0.2099(14) 0.9664(6) 0.0666(19) Uani 1 1 d . U C12 C 0.0894(7) 0.3469(15) 0.9953(7) 0.079(2) Uani 1 1 d . U H12 H 0.075450 0.430792 0.972066 0.095 Uiso 1 1 calc R . C13 C 0.1212(8) 0.3297(18) 1.0679(7) 0.087(2) Uani 1 1 d . U H13 H 0.132842 0.403072 1.100035 0.105 Uiso 1 1 calc R . C14 C 0.1316(7) 0.1940(17) 1.0829(7) 0.086(2) Uani 1 1 d . U H14 H 0.150809 0.157527 1.127006 0.103 Uiso 1 1 calc R . C15 C 0.1087(7) 0.1133(16) 1.0205(7) 0.075(2) Uani 1 1 d . U C16 C 0.1045(9) -0.0351(16) 1.0072(8) 0.098(4) Uani 1 1 d . U C17 C 0.0776(9) -0.0785(18) 0.9420(8) 0.111(5) Uani 1 1 d . U H17 H 0.076252 -0.174476 0.932088 0.133 Uiso 1 1 calc R . C18 C 0.0512(8) 0.0169(14) 0.8875(7) 0.085(4) Uani 1 1 d . U C19 C 0.0189(8) 0.0068(13) 0.8208(7) 0.084(4) Uani 1 1 d . U H19 H 0.009246 -0.076974 0.795789 0.101 Uiso 1 1 calc R . C20 C 0.0244(6) 0.2387(13) 0.8444(6) 0.062(2) Uani 1 1 d . U C21 C 0.1343(13) -0.136(2) 1.0659(10) 0.147(8) Uani 1 1 d . U H21A H 0.184778 -0.112919 1.081630 0.220 Uiso 1 1 calc GR . H21B H 0.131560 -0.230620 1.047691 0.220 Uiso 1 1 calc GR . H21C H 0.105303 -0.128593 1.105390 0.220 Uiso 1 1 calc GR . C22 C -0.0317(7) 0.1771(12) 0.7263(6) 0.064(2) Uani 1 1 d . U C23 C -0.1024(7) 0.1270(12) 0.7042(6) 0.063(2) Uani 1 1 d . U C24 C -0.1353(7) 0.1681(12) 0.6377(6) 0.066(3) Uani 1 1 d . U H24 H -0.181987 0.133411 0.621408 0.079 Uiso 1 1 calc R . C25 C -0.1014(7) 0.2582(14) 0.5951(6) 0.071(3) Uani 1 1 d . U C26 C -0.0322(7) 0.3016(14) 0.6173(7) 0.078(3) Uani 1 1 d . U H26 H -0.007472 0.359529 0.587970 0.093 Uiso 1 1 calc R . C27 C 0.0029(7) 0.2607(14) 0.6841(6) 0.075(3) Uani 1 1 d . U H27 H 0.050494 0.292036 0.699021 0.090 Uiso 1 1 calc R . C28 C -0.2044(8) -0.0123(16) 0.7277(8) 0.094(5) Uani 1 1 d . U H28A H -0.206185 -0.050273 0.680213 0.141 Uiso 1 1 calc GR . H28B H -0.239327 0.063396 0.728057 0.141 Uiso 1 1 calc GR . H28C H -0.216519 -0.084726 0.760081 0.141 Uiso 1 1 calc GR . C29 C -0.1365(8) 0.2981(15) 0.5236(7) 0.080(3) Uani 1 1 d . U C30 C -0.1849(8) 0.2073(19) 0.4840(8) 0.098(4) Uani 1 1 d . U H30 H -0.197586 0.120064 0.501664 0.118 Uiso 1 1 calc R . C31 C -0.2134(9) 0.254(2) 0.4166(9) 0.117(5) Uani 1 1 d . U H31 H -0.245476 0.193492 0.389705 0.141 Uiso 1 1 calc R . C32 C -0.2004(10) 0.371(2) 0.3877(10) 0.119(5) Uani 1 1 d . U H32 H -0.221354 0.392720 0.341601 0.143 Uiso 1 1 calc R . C33 C -0.1562(10) 0.461(2) 0.4251(9) 0.119(5) Uani 1 1 d . U H33 H -0.147013 0.549264 0.406301 0.142 Uiso 1 1 calc R . C34 C -0.1226(8) 0.422(2) 0.4944(7) 0.097(4) Uani 1 1 d . U H34 H -0.090103 0.484136 0.519848 0.116 Uiso 1 1 calc R . Cu1A Cu 0.35278(10) 0.92181(19) 0.41788(11) 0.0763(5) Uani 1 1 d . U Fe1A Fe 0.54659(11) 0.7423(4) 0.32325(10) 0.1016(9) Uani 1 1 d . U Cl1A Cl 0.3402(3) 1.1366(4) 0.4190(4) 0.164(3) Uani 1 1 d . U O1A O 0.2220(5) 0.5361(12) 0.3029(5) 0.093(3) Uani 1 1 d . U N1A N 0.4253(5) 0.6538(10) 0.4145(5) 0.0612(18) Uani 1 1 d . U N2A N 0.3107(5) 0.6332(10) 0.4145(5) 0.063(2) Uani 1 1 d . U C1A C 0.4690(10) 0.737(3) 0.2367(8) 0.140(4) Uani 1 1 d . U C2A C 0.5050(11) 0.877(3) 0.2423(9) 0.137(4) Uani 1 1 d . U C3A C 0.5743(11) 0.857(3) 0.2397(9) 0.145(4) Uani 1 1 d . U C4A C 0.5921(12) 0.706(4) 0.2308(9) 0.158(4) Uani 1 1 d . U C5A C 0.5232(15) 0.636(3) 0.2311(10) 0.159(4) Uani 1 1 d . U C6A C 0.3875(9) 0.733(3) 0.2387(9) 0.177(8) Uani 1 1 d . U H6AA H 0.374997 0.654568 0.267291 0.265 Uiso 1 1 calc GR . H6AB H 0.363369 0.722932 0.190939 0.265 Uiso 1 1 calc GR . H6AC H 0.371720 0.818836 0.259260 0.265 Uiso 1 1 calc GR . C7A C 0.4650(14) 1.016(3) 0.2525(12) 0.192(8) Uani 1 1 d . U H7AA H 0.418626 0.996815 0.270392 0.288 Uiso 1 1 calc GR . H7AB H 0.456365 1.063877 0.207427 0.288 Uiso 1 1 calc GR . H7AC H 0.494927 1.073634 0.286108 0.288 Uiso 1 1 calc GR . C8A C 0.6264(14) 0.989(3) 0.2440(13) 0.218(9) Uani 1 1 d . U H8AA H 0.620736 1.040634 0.286814 0.327 Uiso 1 1 calc GR . H8AB H 0.613629 1.047647 0.202986 0.327 Uiso 1 1 calc GR . H8AC H 0.676840 0.958391 0.244722 0.327 Uiso 1 1 calc GR . C9A C 0.6662(15) 0.667(4) 0.2264(14) 0.268(12) Uani 1 1 d . U H9AA H 0.694873 0.684959 0.271504 0.402 Uiso 1 1 calc GR . H9AB H 0.685591 0.721919 0.189696 0.402 Uiso 1 1 calc GR . H9AC H 0.668735 0.569054 0.214887 0.402 Uiso 1 1 calc GR . C10A C 0.5020(19) 0.493(3) 0.2222(14) 0.243(11) Uani 1 1 d . U H10D H 0.544500 0.437297 0.215331 0.365 Uiso 1 1 calc GR . H10E H 0.465839 0.484282 0.181184 0.365 Uiso 1 1 calc GR . H10F H 0.481138 0.461411 0.264120 0.365 Uiso 1 1 calc GR . C11A C 0.4968(7) 0.7025(15) 0.4110(6) 0.0710(18) Uani 1 1 d . U C12A C 0.5273(7) 0.8368(16) 0.4148(6) 0.078(2) Uani 1 1 d . U H12A H 0.502104 0.921042 0.419410 0.093 Uiso 1 1 calc R . C13A C 0.6055(8) 0.8205(19) 0.4103(7) 0.089(3) Uani 1 1 d . U H13A H 0.639796 0.892974 0.410015 0.107 Uiso 1 1 calc R . C14A C 0.6204(8) 0.6770(18) 0.4066(7) 0.091(3) Uani 1 1 d . U H14A H 0.667187 0.638897 0.404180 0.109 Uiso 1 1 calc R . C15A C 0.5539(7) 0.5959(18) 0.4069(7) 0.083(2) Uani 1 1 d . U C16A C 0.5374(8) 0.4506(19) 0.4071(9) 0.101(3) Uani 1 1 d . U C17A C 0.4702(8) 0.4113(18) 0.4081(9) 0.105(5) Uani 1 1 d . U H17A H 0.459069 0.315704 0.405455 0.126 Uiso 1 1 calc R . C18A C 0.4121(7) 0.5101(12) 0.4132(7) 0.075(3) Uani 1 1 d . U C19A C 0.3393(7) 0.4954(12) 0.4122(8) 0.077(3) Uani 1 1 d . U H19A H 0.312701 0.411602 0.410421 0.092 Uiso 1 1 calc R . C20A C 0.3627(6) 0.7310(12) 0.4150(5) 0.057(2) Uani 1 1 d . U C21A C 0.6004(10) 0.356(2) 0.4017(12) 0.143(7) Uani 1 1 d . U H21D H 0.622920 0.378121 0.359221 0.215 Uiso 1 1 calc GR . H21E H 0.583423 0.260319 0.399366 0.215 Uiso 1 1 calc GR . H21F H 0.635903 0.368114 0.442939 0.215 Uiso 1 1 calc GR . C22A C 0.2344(6) 0.6655(11) 0.4082(6) 0.061(2) Uani 1 1 d . U C23A C 0.1881(7) 0.6182(12) 0.3495(6) 0.063(2) Uani 1 1 d . U C24A C 0.1177(7) 0.6617(14) 0.3387(7) 0.077(3) Uani 1 1 d . U H24A H 0.088237 0.632389 0.297829 0.092 Uiso 1 1 calc R . C25A C 0.0878(6) 0.7488(13) 0.3867(6) 0.067(2) Uani 1 1 d . U C26A C 0.1321(7) 0.7914(12) 0.4455(7) 0.069(3) Uani 1 1 d . U H26A H 0.113030 0.850378 0.478516 0.083 Uiso 1 1 calc R . C27A C 0.2058(6) 0.7484(12) 0.4575(6) 0.062(2) Uani 1 1 d . U H27A H 0.235172 0.776186 0.498787 0.074 Uiso 1 1 calc R . C28A C 0.1768(10) 0.4789(18) 0.2446(8) 0.110(6) Uani 1 1 d . U H28D H 0.168179 0.548558 0.207603 0.165 Uiso 1 1 calc GR . H28E H 0.130503 0.450156 0.259874 0.165 Uiso 1 1 calc GR . H28F H 0.200951 0.398748 0.226387 0.165 Uiso 1 1 calc GR . C29A C 0.0110(7) 0.7960(16) 0.3732(8) 0.087(3) Uani 1 1 d . U C30A C -0.0413(8) 0.719(2) 0.3333(9) 0.111(5) Uani 1 1 d . U H30A H -0.028499 0.631299 0.316130 0.134 Uiso 1 1 calc R . C31A C -0.1116(9) 0.766(3) 0.3178(13) 0.154(7) Uani 1 1 d . U H31A H -0.145843 0.709350 0.290606 0.185 Uiso 1 1 calc R . C32A C -0.1325(9) 0.890(2) 0.3405(13) 0.146(7) Uani 1 1 d . U H32A H -0.180519 0.921620 0.327755 0.175 Uiso 1 1 calc R . C33A C -0.0829(9) 0.972(2) 0.3831(12) 0.137(6) Uani 1 1 d . U H33A H -0.097802 1.056833 0.401252 0.164 Uiso 1 1 calc R . C34A C -0.0099(7) 0.9254(19) 0.3987(9) 0.098(4) Uani 1 1 d . U H34A H 0.024514 0.981145 0.426071 0.118 Uiso 1 1 calc R . 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 Cu1 0.1403(18) 0.0475(9) 0.0835(12) -0.0062(11) -0.0125(11) -0.0113(13) Fe1 0.0614(12) 0.147(2) 0.0692(12) -0.0203(14) 0.0111(8) -0.0239(14) Cl1 0.350(10) 0.0475(19) 0.143(4) -0.005(3) -0.096(5) -0.001(4) O1 0.080(5) 0.077(5) 0.071(4) -0.002(4) -0.001(3) -0.020(4) N1 0.064(5) 0.055(3) 0.071(3) -0.011(3) 0.007(3) -0.003(3) N2 0.072(6) 0.051(3) 0.072(3) -0.010(3) 0.002(3) -0.003(4) C1 0.062(6) 0.204(9) 0.092(4) -0.019(5) 0.022(3) -0.026(6) C2 0.102(7) 0.202(8) 0.113(6) -0.019(5) 0.041(5) -0.058(6) C3 0.085(6) 0.270(11) 0.117(7) -0.050(7) 0.023(6) -0.081(6) C4 0.060(3) 0.299(12) 0.106(6) -0.001(7) 0.009(5) -0.027(6) C5 0.061(6) 0.223(9) 0.120(6) -0.007(6) 0.026(5) 0.003(6) C6 0.113(13) 0.29(2) 0.086(5) -0.026(9) 0.026(6) -0.029(17) C7 0.20(2) 0.192(10) 0.23(2) 0.025(12) 0.093(17) -0.053(12) C8 0.19(2) 0.39(2) 0.195(16) -0.141(17) 0.063(15) -0.191(18) C9 0.098(13) 0.52(3) 0.126(9) 0.051(15) 0.008(10) 0.06(2) C10 0.14(2) 0.224(9) 0.23(2) -0.007(10) 0.082(17) 0.044(11) C11 0.056(3) 0.073(4) 0.071(3) -0.015(3) 0.010(3) -0.006(4) C12 0.083(4) 0.080(4) 0.076(5) -0.023(4) 0.017(4) -0.017(4) C13 0.086(6) 0.105(5) 0.073(4) -0.025(4) 0.017(3) -0.025(5) C14 0.072(6) 0.114(6) 0.072(4) -0.012(4) 0.011(3) -0.015(5) C15 0.060(5) 0.091(4) 0.075(4) -0.008(3) 0.007(4) 0.001(3) C16 0.110(10) 0.086(4) 0.091(5) 0.002(4) -0.013(6) 0.014(4) C17 0.155(13) 0.063(5) 0.104(5) -0.004(4) -0.030(7) 0.018(7) C18 0.103(10) 0.054(3) 0.091(5) -0.011(3) -0.021(5) 0.005(5) C19 0.105(10) 0.049(3) 0.092(5) -0.013(3) -0.021(6) -0.003(5) C20 0.065(6) 0.052(3) 0.070(4) -0.010(3) 0.009(4) -0.007(4) C21 0.20(2) 0.110(9) 0.119(10) 0.020(9) -0.048(12) 0.015(11) C22 0.068(4) 0.056(6) 0.069(4) -0.010(3) 0.007(3) -0.003(4) C23 0.067(4) 0.048(5) 0.072(4) -0.009(4) 0.006(3) 0.001(4) C24 0.069(5) 0.060(6) 0.070(4) -0.009(4) 0.009(3) 0.009(4) C25 0.075(5) 0.064(6) 0.076(4) -0.002(4) 0.013(3) 0.013(4) C26 0.083(5) 0.078(8) 0.074(5) -0.003(5) 0.016(4) -0.001(5) C27 0.083(6) 0.068(7) 0.074(5) -0.007(5) 0.008(4) -0.016(5) C28 0.083(6) 0.106(12) 0.090(9) 0.004(8) -0.003(6) -0.031(6) C29 0.079(7) 0.089(7) 0.075(4) 0.002(4) 0.017(4) 0.024(5) C30 0.096(9) 0.106(8) 0.089(6) -0.009(6) -0.004(5) 0.027(6) C31 0.102(9) 0.153(12) 0.093(7) 0.002(7) -0.007(6) 0.040(9) C32 0.102(10) 0.158(13) 0.098(9) 0.016(7) 0.012(7) 0.061(8) C33 0.113(11) 0.149(12) 0.096(7) 0.036(7) 0.022(6) 0.040(8) C34 0.106(9) 0.098(7) 0.088(6) 0.019(6) 0.025(5) 0.028(6) Cu1A 0.0651(11) 0.0453(8) 0.1166(14) -0.0027(12) 0.0024(9) -0.0009(10) Fe1A 0.0621(12) 0.180(3) 0.0620(11) 0.0038(16) 0.0051(8) -0.0009(16) Cl1A 0.103(3) 0.0435(18) 0.333(9) -0.014(3) -0.028(4) 0.000(2) O1A 0.091(5) 0.097(6) 0.090(5) -0.031(5) 0.004(4) 0.003(5) N1A 0.063(3) 0.053(3) 0.067(5) -0.005(4) 0.004(3) 0.006(2) N2A 0.063(3) 0.042(3) 0.083(6) 0.001(4) 0.002(3) 0.001(2) C1A 0.094(5) 0.258(11) 0.062(5) 0.006(7) -0.012(4) -0.012(6) C2A 0.094(7) 0.240(10) 0.075(6) 0.040(7) 0.004(6) 0.004(6) C3A 0.090(7) 0.273(10) 0.072(6) 0.037(7) 0.007(5) -0.009(6) C4A 0.114(7) 0.298(11) 0.067(5) 0.017(8) 0.022(5) 0.034(8) C5A 0.148(8) 0.254(10) 0.070(5) -0.032(6) -0.005(6) 0.005(7) C6A 0.092(5) 0.33(2) 0.097(11) -0.009(17) -0.026(7) -0.033(9) C7A 0.195(19) 0.258(12) 0.120(15) 0.053(12) 0.000(14) 0.059(12) C8A 0.172(15) 0.344(15) 0.138(18) 0.070(16) 0.016(16) -0.090(14) C9A 0.153(10) 0.52(3) 0.148(19) 0.01(3) 0.071(13) 0.119(15) C10A 0.31(2) 0.263(12) 0.15(2) -0.069(13) -0.03(2) -0.022(11) C11A 0.061(3) 0.088(4) 0.063(4) -0.006(4) 0.003(3) -0.001(3) C12A 0.064(4) 0.096(4) 0.072(4) 0.007(5) 0.003(4) -0.011(3) C13A 0.062(4) 0.131(6) 0.074(5) 0.008(5) 0.002(4) -0.009(4) C14A 0.062(4) 0.137(6) 0.072(5) 0.001(6) -0.001(4) 0.004(4) C15A 0.063(4) 0.111(4) 0.072(5) -0.018(4) 0.000(4) 0.010(3) C16A 0.076(4) 0.105(4) 0.118(10) -0.025(6) -0.007(6) 0.020(4) C17A 0.081(4) 0.068(5) 0.162(13) -0.023(8) -0.004(6) 0.023(4) C18A 0.072(4) 0.051(3) 0.100(9) -0.008(5) 0.000(5) 0.009(3) C19A 0.072(4) 0.042(3) 0.112(9) 0.002(5) -0.003(5) 0.005(3) C20A 0.062(3) 0.045(2) 0.063(6) -0.004(4) 0.004(4) 0.001(2) C21A 0.088(7) 0.141(9) 0.19(2) -0.059(13) -0.021(10) 0.042(8) C22A 0.061(3) 0.046(5) 0.074(5) 0.000(4) 0.003(3) -0.002(3) C23A 0.065(4) 0.050(6) 0.075(5) -0.002(4) 0.005(3) -0.012(4) C24A 0.065(4) 0.078(7) 0.085(6) -0.003(5) -0.002(4) -0.008(4) C25A 0.060(4) 0.061(6) 0.081(5) 0.018(4) 0.007(3) -0.005(4) C26A 0.063(4) 0.060(7) 0.085(6) 0.000(5) 0.012(3) 0.000(4) C27A 0.061(4) 0.048(5) 0.075(5) -0.001(4) 0.006(3) -0.006(4) C28A 0.113(11) 0.118(14) 0.098(8) -0.042(8) 0.005(7) -0.016(9) C29A 0.062(4) 0.092(6) 0.107(8) 0.032(6) 0.010(4) 0.003(4) C30A 0.063(5) 0.112(8) 0.153(12) 0.036(8) -0.015(6) 0.000(5) C31A 0.070(6) 0.168(13) 0.215(17) 0.060(12) -0.023(8) 0.016(7) C32A 0.054(8) 0.157(13) 0.230(17) 0.092(11) 0.022(8) 0.020(7) C33A 0.071(7) 0.143(12) 0.204(15) 0.067(10) 0.046(7) 0.030(6) C34A 0.065(6) 0.087(6) 0.148(11) 0.042(7) 0.036(6) 0.009(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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 C20 Cu1 Cl1 176.6(5) C1 Fe1 C2 38.9(8) C1 Fe1 C3 67.8(8) C1 Fe1 C4 68.2(7) C1 Fe1 C11 108.1(6) C1 Fe1 C12 119.1(7) C1 Fe1 C14 165.6(9) C1 Fe1 C15 127.4(7) C2 Fe1 C3 38.6(8) C2 Fe1 C12 106.9(9) C2 Fe1 C14 154.6(8) C2 Fe1 C15 162.6(7) C3 Fe1 C15 158.4(8) C4 Fe1 C2 65.1(10) C4 Fe1 C3 40.6(10) C4 Fe1 C11 160.0(10) C4 Fe1 C12 158.6(10) C4 Fe1 C14 110.1(7) C4 Fe1 C15 125.1(10) C5 Fe1 C1 40.4(8) C5 Fe1 C2 66.1(10) C5 Fe1 C3 69.8(10) C5 Fe1 C4 42.3(9) C5 Fe1 C11 122.0(7) C5 Fe1 C12 155.2(7) C5 Fe1 C14 128.6(9) C5 Fe1 C15 110.6(9) C11 Fe1 C2 125.1(7) C11 Fe1 C3 158.0(10) C11 Fe1 C12 40.8(5) C11 Fe1 C14 68.4(5) C11 Fe1 C15 40.6(5) C12 Fe1 C3 120.7(10) C12 Fe1 C14 68.0(6) C12 Fe1 C15 68.5(6) C13 Fe1 C1 154.7(9) C13 Fe1 C2 121.0(9) C13 Fe1 C3 105.3(8) C13 Fe1 C4 123.4(8) C13 Fe1 C5 162.6(8) C13 Fe1 C11 68.7(5) C13 Fe1 C12 41.8(6) C13 Fe1 C14 38.6(6) C13 Fe1 C15 67.5(6) C14 Fe1 C3 120.9(7) C14 Fe1 C15 41.0(5) C23 O1 C28 117.5(10) C11 N1 C18 118.8(10) C20 N1 C11 128.4(10) C20 N1 C18 112.8(9) C19 N2 C20 110.9(10) C19 N2 C22 129.1(10) C20 N2 C22 120.0(10) C2 C1 Fe1 71.2(11) C2 C1 C5 107.5(17) C2 C1 C6 128(2) C5 C1 Fe1 69.8(11) C5 C1 C6 125(2) C6 C1 Fe1 127.8(11) C1 C2 Fe1 69.8(12) C1 C2 C7 123(2) C3 C2 Fe1 71.3(13) C3 C2 C1 114(3) C3 C2 C7 122(3) C7 C2 Fe1 120.9(16) C2 C3 Fe1 70.1(11) C2 C3 C4 104(2) C2 C3 C8 131(3) C4 C3 Fe1 68.5(11) C4 C3 C8 125(3) C8 C3 Fe1 127.1(15) C3 C4 Fe1 70.9(12) C3 C4 C5 109(2) C3 C4 C9 123(3) C5 C4 Fe1 68.8(10) C5 C4 C9 128(3) C9 C4 Fe1 123.6(16) C1 C5 Fe1 69.9(12) C1 C5 C4 105(2) C1 C5 C10 127(2) C4 C5 Fe1 68.9(12) C4 C5 C10 128(3) C10 C5 Fe1 126.9(16) C1 C6 H6A 109.5 C1 C6 H6B 109.5 C1 C6 H6C 109.5 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C2 C7 H7A 109.5 C2 C7 H7B 109.5 C2 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C3 C8 H8A 109.5 C3 C8 H8B 109.5 C3 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C4 C9 H9A 109.5 C4 C9 H9B 109.5 C4 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C5 C10 H10A 109.5 C5 C10 H10B 109.5 C5 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 N1 C11 Fe1 129.6(9) N1 C11 C12 130.9(12) N1 C11 C15 120.2(12) C12 C11 Fe1 70.0(7) C15 C11 Fe1 70.8(7) C15 C11 C12 108.6(11) Fe1 C12 H12 127.1 C11 C12 Fe1 69.2(8) C11 C12 H12 127.2 C11 C12 C13 105.5(13) C13 C12 Fe1 68.0(9) C13 C12 H12 127.2 Fe1 C13 H13 124.3 C12 C13 Fe1 70.3(8) C12 C13 H13 124.9 C14 C13 Fe1 72.1(10) C14 C13 C12 110.2(13) C14 C13 H13 124.9 Fe1 C14 H14 126.6 C13 C14 Fe1 69.3(10) C13 C14 H14 125.5 C13 C14 C15 109.1(14) C15 C14 Fe1 70.1(8) C15 C14 H14 125.5 C11 C15 Fe1 68.6(8) C11 C15 C14 106.6(13) C11 C15 C16 120.6(12) C14 C15 Fe1 68.9(8) C14 C15 C16 132.7(14) C16 C15 Fe1 129.4(12) C15 C16 C21 119.2(14) C17 C16 C15 118.1(14) C17 C16 C21 122.6(15) C16 C17 H17 119.0 C16 C17 C18 122.0(16) C18 C17 H17 119.0 N1 C18 C17 120.2(12) C19 C18 N1 103.9(11) C19 C18 C17 135.9(13) N2 C19 H19 125.2 C18 C19 N2 109.5(11) C18 C19 H19 125.2 N1 C20 Cu1 127.3(8) N1 C20 N2 102.9(10) N2 C20 Cu1 129.7(9) C16 C21 H21A 109.5 C16 C21 H21B 109.5 C16 C21 H21C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C23 C22 N2 118.3(11) C27 C22 N2 121.0(11) C27 C22 C23 120.7(11) O1 C23 C22 117.0(10) O1 C23 C24 125.1(11) C24 C23 C22 117.9(12) C23 C24 H24 119.1 C25 C24 C23 121.9(12) C25 C24 H24 119.1 C24 C25 C29 121.1(12) C26 C25 C24 118.5(12) C26 C25 C29 120.1(13) C25 C26 H26 119.6 C25 C26 C27 120.8(13) C27 C26 H26 119.6 C22 C27 C26 120.1(12) C22 C27 H27 119.9 C26 C27 H27 119.9 O1 C28 H28A 109.5 O1 C28 H28B 109.5 O1 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C30 C29 C25 121.0(14) C34 C29 C25 121.3(14) C34 C29 C30 117.7(14) C29 C30 H30 122.0 C31 C30 C29 116.1(18) C31 C30 H30 122.0 C30 C31 H31 116.4 C32 C31 C30 127(2) C32 C31 H31 116.4 C31 C32 H32 121.0 C31 C32 C33 118.0(18) C33 C32 H32 121.0 C32 C33 H33 120.3 C32 C33 C34 119(2) C34 C33 H33 120.3 C29 C34 C33 121.7(18) C29 C34 H34 119.2 C33 C34 H34 119.2 C20A Cu1A Cl1A 178.7(4) C1A Fe1A C2A 42.4(9) C1A Fe1A C4A 68.0(8) C1A Fe1A C14A 160.9(10) C1A Fe1A C15A 124.4(8) C2A Fe1A C15A 162.3(7) C3A Fe1A C1A 66.6(8) C3A Fe1A C2A 36.6(7) C3A Fe1A C4A 42.9(10) C3A Fe1A C14A 124.0(7) C3A Fe1A C15A 160.3(8) C4A Fe1A C2A 68.2(9) C4A Fe1A C14A 107.9(7) C4A Fe1A C15A 122.0(9) C5A Fe1A C1A 40.1(9) C5A Fe1A C2A 69.5(10) C5A Fe1A C3A 69.2(11) C5A Fe1A C4A 41.0(9) C5A Fe1A C14A 124.6(10) C5A Fe1A C15A 107.8(9) C11A Fe1A C1A 108.5(6) C11A Fe1A C2A 124.1(7) C11A Fe1A C3A 156.4(9) C11A Fe1A C4A 159.1(10) C11A Fe1A C5A 123.0(9) C11A Fe1A C12A 40.5(5) C11A Fe1A C14A 68.4(6) C11A Fe1A C15A 41.7(5) C12A Fe1A C1A 121.7(8) C12A Fe1A C2A 105.6(8) C12A Fe1A C3A 120.6(9) C12A Fe1A C4A 159.3(10) C12A Fe1A C5A 157.5(9) C12A Fe1A C14A 69.0(6) C12A Fe1A C15A 69.8(6) C13A Fe1A C1A 158.0(10) C13A Fe1A C2A 119.5(9) C13A Fe1A C3A 106.3(8) C13A Fe1A C4A 122.1(8) C13A Fe1A C5A 159.5(9) C13A Fe1A C11A 69.3(6) C13A Fe1A C12A 42.3(5) C13A Fe1A C14A 40.3(6) C13A Fe1A C15A 69.4(6) C14A Fe1A C2A 155.2(8) C14A Fe1A C15A 40.6(6) C23A O1A C28A 116.9(11) C18A N1A C11A 119.2(10) C20A N1A C11A 127.8(11) C20A N1A C18A 112.9(10) C19A N2A C22A 124.1(10) C20A N2A C19A 112.6(10) C20A N2A C22A 122.8(9) C2A C1A Fe1A 70.1(9) C2A C1A C6A 117(2) C5A C1A Fe1A 69.0(10) C5A C1A C2A 108(2) C5A C1A C6A 135(3) C6A C1A Fe1A 125.9(12) C1A C2A Fe1A 67.5(11) C1A C2A C7A 125(2) C3A C2A Fe1A 69.6(12) C3A C2A C1A 107(2) C3A C2A C7A 128(3) C7A C2A Fe1A 125.6(14) C2A C3A Fe1A 73.8(13) C2A C3A C4A 112(2) C2A C3A C8A 118(3) C4A C3A Fe1A 69.2(12) C4A C3A C8A 130(2) C8A C3A Fe1A 126.2(14) C3A C4A Fe1A 67.9(12) C5A C4A Fe1A 68.4(11) C5A C4A C3A 104(2) C9A C4A Fe1A 125.2(16) C9A C4A C3A 119(3) C9A C4A C5A 137(3) C1A C5A Fe1A 71.0(12) C1A C5A C4A 109(3) C1A C5A C10A 119(3) C4A C5A Fe1A 70.6(13) C4A C5A C10A 132(3) C10A C5A Fe1A 128(2) C1A C6A H6AA 109.5 C1A C6A H6AB 109.5 C1A C6A H6AC 109.5 H6AA C6A H6AB 109.5 H6AA C6A H6AC 109.5 H6AB C6A H6AC 109.5 C2A C7A H7AA 109.5 C2A C7A H7AB 109.5 C2A C7A H7AC 109.5 H7AA C7A H7AB 109.5 H7AA C7A H7AC 109.5 H7AB C7A H7AC 109.5 C3A C8A H8AA 109.5 C3A C8A H8AB 109.5 C3A C8A H8AC 109.5 H8AA C8A H8AB 109.5 H8AA C8A H8AC 109.5 H8AB C8A H8AC 109.5 C4A C9A H9AA 109.5 C4A C9A H9AB 109.5 C4A C9A H9AC 109.5 H9AA C9A H9AB 109.5 H9AA C9A H9AC 109.5 H9AB C9A H9AC 109.5 C5A C10A H10D 109.5 C5A C10A H10E 109.5 C5A C10A H10F 109.5 H10D C10A H10E 109.5 H10D C10A H10F 109.5 H10E C10A H10F 109.5 N1A C11A Fe1A 127.8(8) N1A C11A C15A 116.6(12) C12A C11A Fe1A 69.9(8) C12A C11A N1A 132.3(12) C12A C11A C15A 111.0(12) C15A C11A Fe1A 72.4(8) Fe1A C12A H12A 126.8 C11A C12A Fe1A 69.6(8) C11A C12A H12A 126.6 C11A C12A C13A 106.7(14) C13A C12A Fe1A 68.5(8) C13A C12A H12A 126.6 Fe1A C13A H13A 124.7 C12A C13A Fe1A 69.2(7) C12A C13A H13A 126.0 C14A C13A Fe1A 71.6(9) C14A C13A C12A 107.9(14) C14A C13A H13A 126.0 Fe1A C14A H14A 127.5 C13A C14A Fe1A 68.1(8) C13A C14A H14A 124.6 C13A C14A C15A 110.8(14) C15A C14A Fe1A 71.5(8) C15A C14A H14A 124.6 C11A C15A Fe1A 65.9(8) C14A C15A Fe1A 67.9(9) C14A C15A C11A 103.5(14) C16A C15A Fe1A 130.9(11) C16A C15A C11A 121.7(14) C16A C15A C14A 134.7(14) C15A C16A C21A 115.5(16) C17A C16A C15A 119.2(15) C17A C16A C21A 125.2(18) C16A C17A H17A 119.1 C16A C17A C18A 121.8(16) C18A C17A H17A 119.1 N1A C18A C17A 121.4(13) C19A C18A N1A 105.9(10) C19A C18A C17A 132.5(13) N2A C19A H19A 127.1 C18A C19A N2A 105.8(10) C18A C19A H19A 127.1 N1A C20A Cu1A 128.7(8) N2A C20A Cu1A 128.6(9) N2A C20A N1A 102.7(10) C16A C21A H21D 109.5 C16A C21A H21E 109.5 C16A C21A H21F 109.5 H21D C21A H21E 109.5 H21D C21A H21F 109.5 H21E C21A H21F 109.5 C23A C22A N2A 120.1(11) C27A C22A N2A 120.9(10) C27A C22A C23A 118.9(11) O1A C23A C22A 114.5(11) C24A C23A O1A 124.8(11) C24A C23A C22A 120.4(12) C23A C24A H24A 119.1 C23A C24A C25A 121.8(11) C25A C24A H24A 119.1 C24A C25A C29A 120.6(12) C26A C25A C24A 118.0(11) C26A C25A C29A 121.4(13) C25A C26A H26A 119.4 C25A C26A C27A 121.2(12) C27A C26A H26A 119.4 C22A C27A C26A 119.5(10) C22A C27A H27A 120.3 C26A C27A H27A 120.3 O1A C28A H28D 109.5 O1A C28A H28E 109.5 O1A C28A H28F 109.5 H28D C28A H28E 109.5 H28D C28A H28F 109.5 H28E C28A H28F 109.5 C30A C29A C25A 121.9(15) C30A C29A C34A 117.8(14) C34A C29A C25A 120.2(13) C29A C30A H30A 119.1 C31A C30A C29A 122(2) C31A C30A H30A 119.1 C30A C31A H31A 119.3 C32A C31A C30A 121(2) C32A C31A H31A 119.3 C31A C32A H32A 120.2 C31A C32A C33A 119.7(17) C33A C32A H32A 120.2 C32A C33A H33A 120.3 C32A C33A C34A 119(2) C34A C33A H33A 120.3 C29A C34A C33A 119.7(18) C29A C34A H34A 120.2 C33A C34A H34A 120.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cu1 Cl1 2.068(5) Cu1 C20 1.840(12) Fe1 C1 2.024(16) Fe1 C2 2.04(2) Fe1 C3 2.057(18) Fe1 C4 2.025(18) Fe1 C5 2.02(2) Fe1 C11 2.035(11) Fe1 C12 2.045(15) Fe1 C13 2.014(15) Fe1 C14 2.048(15) Fe1 C15 2.064(15) O1 C23 1.369(15) O1 C28 1.421(15) N1 C11 1.383(15) N1 C18 1.422(16) N1 C20 1.355(15) N2 C19 1.371(16) N2 C20 1.386(14) N2 C22 1.427(15) C1 C2 1.35(3) C1 C5 1.40(3) C1 C6 1.51(2) C2 C3 1.35(3) C2 C7 1.59(3) C3 C4 1.42(4) C3 C8 1.55(3) C4 C5 1.46(3) C4 C9 1.46(3) C5 C10 1.50(3) C6 H6A 0.9700 C6 H6B 0.9700 C6 H6C 0.9700 C7 H7A 0.9700 C7 H7B 0.9700 C7 H7C 0.9700 C8 H8A 0.9700 C8 H8B 0.9700 C8 H8C 0.9700 C9 H9A 0.9700 C9 H9B 0.9700 C9 H9C 0.9700 C10 H10A 0.9700 C10 H10B 0.9700 C10 H10C 0.9700 C11 C12 1.423(17) C11 C15 1.422(19) C12 H12 0.9400 C12 C13 1.45(2) C13 H13 0.9400 C13 C14 1.34(2) C14 H14 0.9400 C14 C15 1.439(19) C15 C16 1.446(18) C16 C17 1.35(2) C16 C21 1.53(2) C17 H17 0.9400 C17 C18 1.43(2) C18 C19 1.343(17) C19 H19 0.9400 C21 H21A 0.9700 C21 H21B 0.9700 C21 H21C 0.9700 C22 C23 1.406(17) C22 C27 1.342(17) C23 C24 1.397(17) C24 H24 0.9400 C24 C25 1.380(18) C25 C26 1.361(17) C25 C29 1.486(18) C26 H26 0.9400 C26 C27 1.413(18) C27 H27 0.9400 C28 H28A 0.9700 C28 H28B 0.9700 C28 H28C 0.9700 C29 C30 1.40(2) C29 C34 1.35(2) C30 H30 0.9400 C30 C31 1.40(2) C31 H31 0.9400 C31 C32 1.28(3) C32 H32 0.9400 C32 C33 1.34(3) C33 H33 0.9400 C33 C34 1.44(2) C34 H34 0.9400 Cu1A Cl1A 2.074(4) Cu1A C20A 1.841(11) Fe1A C1A 2.054(14) Fe1A C2A 2.090(19) Fe1A C3A 2.04(2) Fe1A C4A 2.058(19) Fe1A C5A 2.03(2) Fe1A C11A 2.023(13) Fe1A C12A 2.027(14) Fe1A C13A 2.018(14) Fe1A C14A 2.065(13) Fe1A C15A 2.113(16) O1A C23A 1.383(15) O1A C28A 1.419(16) N1A C11A 1.405(16) N1A C18A 1.400(15) N1A C20A 1.369(14) N2A C19A 1.424(15) N2A C20A 1.340(14) N2A C22A 1.430(15) C1A C2A 1.50(3) C1A C5A 1.40(3) C1A C6A 1.50(2) C2A C3A 1.30(3) C2A C7A 1.54(3) C3A C4A 1.50(3) C3A C8A 1.59(3) C4A C5A 1.43(3) C4A C9A 1.42(3) C5A C10A 1.43(3) C6A H6AA 0.9700 C6A H6AB 0.9700 C6A H6AC 0.9700 C7A H7AA 0.9700 C7A H7AB 0.9700 C7A H7AC 0.9700 C8A H8AA 0.9700 C8A H8AB 0.9700 C8A H8AC 0.9700 C9A H9AA 0.9700 C9A H9AB 0.9700 C9A H9AC 0.9700 C10A H10D 0.9700 C10A H10E 0.9700 C10A H10F 0.9700 C11A C12A 1.403(19) C11A C15A 1.474(19) C12A H12A 0.9400 C12A C13A 1.459(19) C13A H13A 0.9400 C13A C14A 1.41(2) C14A H14A 0.9400 C14A C15A 1.45(2) C15A C16A 1.43(2) C16A C17A 1.29(2) C16A C21A 1.48(2) C17A H17A 0.9400 C17A C18A 1.440(18) C18A C19A 1.345(18) C19A H19A 0.9400 C21A H21D 0.9700 C21A H21E 0.9700 C21A H21F 0.9700 C22A C23A 1.402(16) C22A C27A 1.376(16) C23A C24A 1.353(18) C24A H24A 0.9400 C24A C25A 1.393(18) C25A C26A 1.370(16) C25A C29A 1.479(18) C26A H26A 0.9400 C26A C27A 1.412(16) C27A H27A 0.9400 C28A H28D 0.9700 C28A H28E 0.9700 C28A H28F 0.9700 C29A C30A 1.37(2) C29A C34A 1.40(2) C30A H30A 0.9400 C30A C31A 1.37(2) C31A H31A 0.9400 C31A C32A 1.34(3) C32A H32A 0.9400 C32A C33A 1.39(3) C33A H33A 0.9400 C33A C34A 1.41(2) C34A H34A 0.9400 loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 0.000 0.650 0.000 12.8 0.0 2 0.123 0.478 0.749 10.3 0.0 3 0.187 0.815 0.825 16.5 0.0 4 0.348 0.310 0.260 28.5 1.5 5 0.500 0.070 0.000 301.9 65.9 6 0.500 0.135 0.500 14.9 0.0 7 0.652 0.310 0.740 28.5 0.0 8 0.813 0.815 0.175 16.5 0.0 9 0.877 0.478 0.251 10.3 0.0