# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Euan Brechin' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Anna Collins' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Ian A. Gass' '' '' 'Kevin Mason' '' '' 'Simon Parsons' '' '' 'Alexandra Slawin' '' '' 'Peter Tasker' '' '' 'Fraser White' '' '' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; Building Fe(III) Clusters with Derivatised Salicylaldoximes ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_address ; School of Chemistry, University of Edinburgh, Joseph Black Building, King's Buildings, West Mains Road, Edinburgh, EH9 3JJ , UK. ; _publ_contact_author_fax '+44 131 000000' _publ_contact_author_phone '+44 131 650 4806' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_requested_journal 'Section E' # Attachment 'Complex 1.cif' data_eb8185 _database_code_depnum_ccdc_archive 'CCDC 755035' #TrackingRef 'Complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Kevin Mason' _exptl_crystal_recrystallization_method 'Slow evaporation of MeOH/pyridine solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cl2 Fe3 N5 O6, 2(C H4 O)' _chemical_formula_sum 'C44 H44 Cl2 Fe3 N5 O8' _chemical_formula_weight 1009.29 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' H H 0.0000 0.0000 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2027(3) _cell_length_b 18.0542(4) _cell_length_c 18.0473(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.0570(10) _cell_angle_gamma 90.00 _cell_volume 4581.98(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7991 _cell_measurement_theta_min 2.5235 _cell_measurement_theta_max 26.3155 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_T_max 0.8498 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42560 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.41 _reflns_number_total 9402 _reflns_number_gt 7742 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 4 These belong to the solvent molecules. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.17 Ratio 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 Noted, no action taken 731_ALERT_1_C Bond Calc 0.85(4), Rep 0.851(10) ...... 4.00 su-Rat O1S -H1S 1.555 1.555 This is due to a restraint. 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 2 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 1 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 13 The data collection strategy used was intended to collect fully complete data to 2TH= 53deg. Please refer to the completeness statistics below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 4789 4787 2 23.01 0.550 1.000 6382 6380 2 25.24 0.600 1.000 8311 8308 3 #----------------------------------------------------------- ACTA Min. Res. ---- 26.41 0.626 0.998 9418 9402 16 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+10.7450P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9402 _refine_ls_number_parameters 544 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.26485(4) 0.18221(3) 0.26599(3) 0.02152(14) Uani 1 1 d . . . Fe2 Fe 0.37882(4) 0.34544(3) 0.28193(3) 0.02489(15) Uani 1 1 d . . . Fe3 Fe 0.16479(4) 0.35264(3) 0.25484(3) 0.02376(15) Uani 1 1 d . . . Cl1 Cl 0.08638(8) 0.35911(6) 0.35449(6) 0.0347(3) Uani 1 1 d . . . Cl2 Cl 0.44777(8) 0.35187(7) 0.17734(6) 0.0369(3) Uani 1 1 d . . . O123 O 0.26857(19) 0.28537(16) 0.26765(16) 0.0274(6) Uani 1 1 d . . . O1F O 0.2755(2) 0.42040(16) 0.27164(18) 0.0332(7) Uani 1 1 d . . . C2F C 0.2864(4) 0.4973(3) 0.2785(3) 0.0499(14) Uani 1 1 d . . . H2F1 H 0.2383 0.5219 0.2426 0.075 Uiso 1 1 calc R . . H2F2 H 0.3500 0.5113 0.2682 0.075 Uiso 1 1 calc R . . H2F3 H 0.2786 0.5124 0.3294 0.075 Uiso 1 1 calc R . . O1A O 0.0962(2) 0.40862(16) 0.17842(16) 0.0292(6) Uani 1 1 d . . . C1A C 0.0116(3) 0.3982(2) 0.1383(2) 0.0300(9) Uani 1 1 d . . . C2A C -0.0299(3) 0.3271(2) 0.1254(2) 0.0281(9) Uani 1 1 d . . . C6A C -0.0375(4) 0.4599(3) 0.1046(3) 0.0444(13) Uani 1 1 d . . . H6A H -0.0099 0.5078 0.1118 0.053 Uiso 1 1 calc R . . C5A C -0.1240(4) 0.4522(3) 0.0621(3) 0.0560(16) Uani 1 1 d . . . H5A H -0.1555 0.4948 0.0399 0.067 Uiso 1 1 calc R . . C4A C -0.1666(4) 0.3841(3) 0.0507(4) 0.0554(15) Uani 1 1 d . . . H4A H -0.2276 0.3797 0.0218 0.067 Uiso 1 1 calc R . . C3A C -0.1198(3) 0.3225(3) 0.0816(3) 0.0400(11) Uani 1 1 d . . . H3A H -0.1489 0.2753 0.0730 0.048 Uiso 1 1 calc R . . C21A C 0.0174(3) 0.2579(2) 0.1524(2) 0.0247(9) Uani 1 1 d . . . N22A N 0.0929(2) 0.25905(18) 0.20237(18) 0.0224(7) Uani 1 1 d . . . C23A C -0.0194(3) 0.1859(2) 0.1204(2) 0.0241(8) Uani 1 1 d . . . C28A C -0.0143(3) 0.1693(2) 0.0457(2) 0.0283(9) Uani 1 1 d . . . H28A H 0.0085 0.2055 0.0143 0.034 Uiso 1 1 calc R . . C24A C -0.0552(3) 0.1326(2) 0.1650(3) 0.0297(9) Uani 1 1 d . . . H24A H -0.0607 0.1435 0.2157 0.036 Uiso 1 1 calc R . . C25A C -0.0827(3) 0.0638(2) 0.1356(3) 0.0361(11) Uani 1 1 d . . . H25A H -0.1059 0.0273 0.1665 0.043 Uiso 1 1 calc R . . C26A C -0.0766(3) 0.0482(3) 0.0620(3) 0.0382(11) Uani 1 1 d . . . H26A H -0.0961 0.0011 0.0421 0.046 Uiso 1 1 calc R . . C27A C -0.0425(3) 0.1002(2) 0.0167(3) 0.0336(10) Uani 1 1 d . . . H27A H -0.0382 0.0889 -0.0341 0.040 Uiso 1 1 calc R . . O2A O 0.13088(19) 0.19097(15) 0.22222(15) 0.0241(6) Uani 1 1 d . . . O1B O 0.4533(2) 0.39694(16) 0.35827(16) 0.0324(7) Uani 1 1 d . . . C1B C 0.5352(3) 0.3813(2) 0.4009(2) 0.0292(9) Uani 1 1 d . . . C2B C 0.5699(3) 0.3086(2) 0.4129(2) 0.0274(9) Uani 1 1 d . . . C6B C 0.5872(4) 0.4407(3) 0.4360(3) 0.0398(11) Uani 1 1 d . . . H6B H 0.5636 0.4897 0.4280 0.048 Uiso 1 1 calc R . . C5B C 0.6711(4) 0.4292(3) 0.4814(3) 0.0488(14) Uani 1 1 d . . . H5B H 0.7047 0.4702 0.5054 0.059 Uiso 1 1 calc R . . C4B C 0.7080(4) 0.3582(3) 0.4929(3) 0.0470(13) Uani 1 1 d . . . H4B H 0.7672 0.3505 0.5236 0.056 Uiso 1 1 calc R . . C3B C 0.6578(3) 0.2993(3) 0.4594(3) 0.0364(11) Uani 1 1 d . . . H3B H 0.6829 0.2508 0.4678 0.044 Uiso 1 1 calc R . . C21B C 0.5175(3) 0.2422(2) 0.3831(2) 0.0252(9) Uani 1 1 d . . . N22B N 0.4433(2) 0.24732(18) 0.33164(18) 0.0240(7) Uani 1 1 d . . . C23B C 0.5498(3) 0.1683(2) 0.4150(2) 0.0277(9) Uani 1 1 d . . . C24B C 0.5875(3) 0.1154(3) 0.3716(3) 0.0372(11) Uani 1 1 d . . . H24B H 0.5928 0.1251 0.3206 0.045 Uiso 1 1 calc R . . C28B C 0.5425(3) 0.1530(3) 0.4894(3) 0.0319(10) Uani 1 1 d . . . H28B H 0.5170 0.1893 0.5191 0.038 Uiso 1 1 calc R . . C27B C 0.5719(3) 0.0856(3) 0.5207(3) 0.0400(11) Uani 1 1 d . . . H27B H 0.5667 0.0754 0.5716 0.048 Uiso 1 1 calc R . . C26B C 0.6089(3) 0.0335(3) 0.4774(3) 0.0421(12) Uani 1 1 d . . . H26B H 0.6288 -0.0132 0.4984 0.050 Uiso 1 1 calc R . . C25B C 0.6175(4) 0.0481(3) 0.4040(3) 0.0464(13) Uani 1 1 d . . . H25B H 0.6443 0.0118 0.3750 0.056 Uiso 1 1 calc R . . O2B O 0.39991(19) 0.18174(15) 0.30958(15) 0.0250(6) Uani 1 1 d . . . N1C N 0.2220(2) 0.16875(18) 0.37786(18) 0.0242(7) Uani 1 1 d . . . C2C C 0.2876(3) 0.1642(3) 0.4383(2) 0.0344(10) Uani 1 1 d . . . H2C H 0.3527 0.1661 0.4315 0.041 Uiso 1 1 calc R . . C6C C 0.1306(3) 0.1648(2) 0.3889(2) 0.0292(9) Uani 1 1 d . . . H6C H 0.0826 0.1680 0.3467 0.035 Uiso 1 1 calc R . . C5C C 0.1034(3) 0.1564(3) 0.4584(3) 0.0347(10) Uani 1 1 d . . . H5C H 0.0379 0.1533 0.4637 0.042 Uiso 1 1 calc R . . C4C C 0.1720(4) 0.1525(3) 0.5206(3) 0.0378(11) Uani 1 1 d . . . H4C H 0.1550 0.1469 0.5693 0.045 Uiso 1 1 calc R . . C3C C 0.2659(4) 0.1570(3) 0.5098(3) 0.0414(12) Uani 1 1 d . . . H3C H 0.3150 0.1552 0.5513 0.050 Uiso 1 1 calc R . . N1D N 0.3076(2) 0.16698(19) 0.15450(19) 0.0276(8) Uani 1 1 d . . . C2D C 0.2410(3) 0.1556(3) 0.0948(3) 0.0388(11) Uani 1 1 d . . . H2D H 0.1760 0.1565 0.1019 0.047 Uiso 1 1 calc R . . C6D C 0.3984(3) 0.1650(3) 0.1425(3) 0.0338(10) Uani 1 1 d . . . H6D H 0.4468 0.1727 0.1838 0.041 Uiso 1 1 calc R . . C5D C 0.4252(4) 0.1523(3) 0.0725(3) 0.0401(12) Uani 1 1 d . . . H5D H 0.4905 0.1511 0.0662 0.048 Uiso 1 1 calc R . . C4D C 0.3555(4) 0.1416(3) 0.0121(3) 0.0430(12) Uani 1 1 d . . . H4D H 0.3717 0.1337 -0.0366 0.052 Uiso 1 1 calc R . . C3D C 0.2624(4) 0.1428(3) 0.0242(3) 0.0451(13) Uani 1 1 d . . . H3D H 0.2129 0.1347 -0.0162 0.054 Uiso 1 1 calc R . . N1E N 0.2529(2) 0.06232(19) 0.25941(18) 0.0266(8) Uani 1 1 d . . . C2E C 0.3304(4) 0.0200(3) 0.2719(3) 0.0409(12) Uani 1 1 d . . . H2E H 0.3899 0.0426 0.2891 0.049 Uiso 1 1 calc R . . C6E C 0.1694(3) 0.0301(3) 0.2362(3) 0.0386(11) Uani 1 1 d . . . H6E H 0.1143 0.0603 0.2268 0.046 Uiso 1 1 calc R . . C5E C 0.1598(4) -0.0454(3) 0.2254(4) 0.0600(17) Uani 1 1 d . . . H5E H 0.0990 -0.0669 0.2105 0.072 Uiso 1 1 calc R . . C4E C 0.2406(5) -0.0891(3) 0.2367(4) 0.077(2) Uani 1 1 d . . . H4E H 0.2368 -0.1410 0.2282 0.092 Uiso 1 1 calc R . . C3E C 0.3269(5) -0.0556(3) 0.2608(4) 0.071(2) Uani 1 1 d . . . H3E H 0.3834 -0.0844 0.2696 0.085 Uiso 1 1 calc R . . O1S O 0.6317(4) 0.2382(3) 0.2336(3) 0.0924(16) Uiso 1 1 d D . . H1S H 0.5742(18) 0.250(5) 0.2184(12) 0.139 Uiso 1 1 d D . . C2S C 0.6783(6) 0.2271(5) 0.1729(4) 0.090(2) Uiso 1 1 d D . . H2S1 H 0.7100 0.2722 0.1569 0.135 Uiso 1 1 d R . . H2S2 H 0.6320 0.2117 0.1258 0.135 Uiso 1 1 d R . . H2S3 H 0.7259 0.1870 0.1797 0.135 Uiso 1 1 d R . . O1T O 0.9005(5) 0.2434(4) 0.3068(4) 0.136(2) Uiso 1 1 d D . . H1T H 0.9524(7) 0.2619(4) 0.3136(4) 0.205 Uiso 1 1 d RD . . C2T C 0.8512(6) 0.2276(5) 0.3622(5) 0.109(3) Uiso 1 1 d D . . H2T1 H 0.8912 0.1979 0.3998 0.163 Uiso 1 1 d R . . H2T2 H 0.7945 0.1991 0.3424 0.163 Uiso 1 1 d R . . H2T3 H 0.8320 0.2732 0.3854 0.163 Uiso 1 1 d 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 Fe1 0.0200(3) 0.0184(3) 0.0252(3) -0.0003(2) -0.0002(2) 0.0003(2) Fe2 0.0235(3) 0.0217(3) 0.0284(3) 0.0017(2) -0.0003(2) -0.0026(2) Fe3 0.0227(3) 0.0189(3) 0.0288(3) -0.0013(2) 0.0003(2) 0.0012(2) Cl1 0.0409(6) 0.0325(6) 0.0309(5) -0.0043(4) 0.0060(5) 0.0058(5) Cl2 0.0363(6) 0.0423(7) 0.0319(6) 0.0052(5) 0.0044(5) -0.0074(5) O123 0.0214(15) 0.0201(15) 0.0389(16) 0.0015(12) -0.0023(12) 0.0006(12) O1F 0.0298(17) 0.0193(15) 0.0487(18) 0.0006(13) -0.0002(14) 0.0004(12) C2F 0.043(3) 0.030(3) 0.078(4) -0.005(3) 0.013(3) -0.002(2) O1A 0.0303(16) 0.0209(15) 0.0343(16) 0.0012(12) -0.0029(13) 0.0011(12) C1A 0.028(2) 0.028(2) 0.033(2) 0.0008(18) 0.0004(18) 0.0043(18) C2A 0.025(2) 0.021(2) 0.038(2) 0.0027(18) 0.0031(18) 0.0027(17) C6A 0.044(3) 0.018(2) 0.068(3) 0.002(2) -0.008(2) 0.003(2) C5A 0.049(3) 0.029(3) 0.082(4) 0.012(3) -0.018(3) 0.012(2) C4A 0.039(3) 0.034(3) 0.085(4) 0.002(3) -0.021(3) 0.006(2) C3A 0.032(3) 0.025(2) 0.059(3) 0.000(2) -0.005(2) 0.002(2) C21A 0.027(2) 0.019(2) 0.029(2) 0.0012(16) 0.0069(17) 0.0010(16) N22A 0.0223(17) 0.0174(17) 0.0274(17) 0.0017(13) 0.0030(13) 0.0037(13) C23A 0.0177(19) 0.018(2) 0.036(2) 0.0000(16) -0.0007(16) 0.0026(15) C28A 0.022(2) 0.026(2) 0.035(2) 0.0020(18) -0.0004(17) 0.0024(17) C24A 0.022(2) 0.030(2) 0.037(2) 0.0026(18) 0.0030(17) 0.0003(18) C25A 0.028(2) 0.023(2) 0.057(3) 0.006(2) 0.006(2) -0.0001(19) C26A 0.029(2) 0.020(2) 0.063(3) -0.007(2) 0.000(2) 0.0024(19) C27A 0.027(2) 0.031(2) 0.042(3) -0.009(2) 0.0000(19) 0.0024(19) O2A 0.0237(15) 0.0169(14) 0.0292(15) 0.0025(11) -0.0054(11) 0.0025(11) O1B 0.0346(17) 0.0252(16) 0.0336(16) -0.0007(13) -0.0077(13) -0.0004(13) C1B 0.031(2) 0.026(2) 0.031(2) -0.0023(18) 0.0030(18) -0.0032(18) C2B 0.024(2) 0.025(2) 0.034(2) 0.0022(17) 0.0027(17) -0.0047(17) C6B 0.042(3) 0.023(2) 0.052(3) -0.001(2) -0.004(2) -0.005(2) C5B 0.040(3) 0.032(3) 0.068(4) -0.001(2) -0.014(3) -0.014(2) C4B 0.029(3) 0.040(3) 0.066(3) -0.001(3) -0.014(2) -0.007(2) C3B 0.027(2) 0.026(2) 0.054(3) 0.000(2) -0.003(2) -0.0034(19) C21B 0.021(2) 0.024(2) 0.031(2) -0.0006(17) 0.0044(16) -0.0004(16) N22B 0.0224(18) 0.0218(18) 0.0272(18) -0.0015(14) 0.0008(14) -0.0021(14) C23B 0.020(2) 0.025(2) 0.037(2) 0.0002(18) -0.0042(17) -0.0056(17) C24B 0.037(3) 0.031(3) 0.042(3) -0.003(2) -0.002(2) 0.002(2) C28B 0.024(2) 0.032(2) 0.039(2) 0.0025(19) 0.0010(18) -0.0010(19) C27B 0.032(3) 0.038(3) 0.049(3) 0.013(2) 0.002(2) -0.004(2) C26B 0.028(3) 0.026(3) 0.068(3) 0.014(2) -0.008(2) -0.003(2) C25B 0.037(3) 0.032(3) 0.067(4) -0.009(2) -0.003(2) 0.008(2) O2B 0.0218(14) 0.0208(15) 0.0307(15) -0.0034(12) -0.0022(11) -0.0015(11) N1C 0.0254(18) 0.0187(17) 0.0273(17) -0.0005(13) -0.0004(14) 0.0012(14) C2C 0.024(2) 0.046(3) 0.033(2) -0.002(2) 0.0018(18) -0.001(2) C6C 0.027(2) 0.025(2) 0.034(2) 0.0014(18) -0.0013(18) 0.0026(18) C5C 0.028(2) 0.036(3) 0.041(3) -0.002(2) 0.0082(19) 0.002(2) C4C 0.045(3) 0.041(3) 0.029(2) 0.000(2) 0.012(2) 0.001(2) C3C 0.039(3) 0.057(3) 0.026(2) 0.003(2) -0.003(2) -0.002(2) N1D 0.0263(19) 0.0252(19) 0.0305(19) 0.0005(14) 0.0011(15) 0.0019(15) C2D 0.032(3) 0.044(3) 0.038(3) -0.001(2) -0.004(2) 0.010(2) C6D 0.033(2) 0.034(3) 0.035(2) -0.0030(19) 0.0043(19) -0.005(2) C5D 0.040(3) 0.043(3) 0.041(3) -0.003(2) 0.018(2) -0.004(2) C4D 0.056(3) 0.044(3) 0.031(2) -0.001(2) 0.013(2) 0.003(3) C3D 0.047(3) 0.056(3) 0.030(2) 0.002(2) 0.000(2) 0.004(3) N1E 0.0307(19) 0.0221(19) 0.0259(17) 0.0012(14) 0.0000(14) 0.0021(15) C2E 0.034(3) 0.035(3) 0.050(3) -0.001(2) -0.008(2) 0.005(2) C6E 0.030(3) 0.025(2) 0.058(3) 0.000(2) -0.003(2) -0.0005(19) C5E 0.053(4) 0.033(3) 0.085(4) -0.003(3) -0.024(3) -0.001(3) C4E 0.079(5) 0.023(3) 0.114(6) -0.016(3) -0.036(4) 0.010(3) C3E 0.056(4) 0.036(3) 0.111(6) -0.010(3) -0.027(4) 0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O123 1.863(3) . ? Fe1 O2A 1.962(3) . ? Fe1 O2B 1.969(3) . ? Fe1 N1E 2.173(3) . ? Fe1 N1D 2.199(4) . ? Fe1 N1C 2.202(3) . ? Fe2 O1B 1.864(3) . ? Fe2 O123 1.892(3) . ? Fe2 O1F 1.986(3) . ? Fe2 N22B 2.133(3) . ? Fe2 Cl2 2.2478(12) . ? Fe3 O1A 1.870(3) . ? Fe3 O123 1.899(3) . ? Fe3 O1F 1.982(3) . ? Fe3 N22A 2.127(3) . ? Fe3 Cl1 2.2470(12) . ? O1F C2F 1.400(6) . ? C2F H2F1 0.9800 . ? C2F H2F2 0.9800 . ? C2F H2F3 0.9800 . ? O1A C1A 1.327(5) . ? C1A C6A 1.407(6) . ? C1A C2A 1.418(6) . ? C2A C3A 1.407(6) . ? C2A C21A 1.468(6) . ? C6A C5A 1.361(7) . ? C6A H6A 0.9500 . ? C5A C4A 1.373(7) . ? C5A H5A 0.9500 . ? C4A C3A 1.374(7) . ? C4A H4A 0.9500 . ? C3A H3A 0.9500 . ? C21A N22A 1.301(5) . ? C21A C23A 1.488(6) . ? N22A O2A 1.370(4) . ? C23A C28A 1.394(6) . ? C23A C24A 1.395(6) . ? C28A C27A 1.389(6) . ? C28A H28A 0.9500 . ? C24A C25A 1.385(6) . ? C24A H24A 0.9500 . ? C25A C26A 1.373(7) . ? C25A H25A 0.9500 . ? C26A C27A 1.377(7) . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? O1B C1B 1.332(5) . ? C1B C6B 1.402(6) . ? C1B C2B 1.408(6) . ? C2B C3B 1.414(6) . ? C2B C21B 1.473(6) . ? C6B C5B 1.365(7) . ? C6B H6B 0.9500 . ? C5B C4B 1.390(7) . ? C5B H5B 0.9500 . ? C4B C3B 1.372(6) . ? C4B H4B 0.9500 . ? C3B H3B 0.9500 . ? C21B N22B 1.307(5) . ? C21B C23B 1.499(6) . ? N22B O2B 1.368(4) . ? C23B C28B 1.390(6) . ? C23B C24B 1.390(6) . ? C24B C25B 1.389(7) . ? C24B H24B 0.9500 . ? C28B C27B 1.382(6) . ? C28B H28B 0.9500 . ? C27B C26B 1.374(7) . ? C27B H27B 0.9500 . ? C26B C25B 1.373(7) . ? C26B H26B 0.9500 . ? C25B H25B 0.9500 . ? N1C C2C 1.334(5) . ? N1C C6C 1.343(5) . ? C2C C3C 1.374(6) . ? C2C H2C 0.9500 . ? C6C C5C 1.371(6) . ? C6C H6C 0.9500 . ? C5C C4C 1.382(7) . ? C5C H5C 0.9500 . ? C4C C3C 1.376(7) . ? C4C H4C 0.9500 . ? C3C H3C 0.9500 . ? N1D C6D 1.337(6) . ? N1D C2D 1.347(6) . ? C2D C3D 1.369(7) . ? C2D H2D 0.9500 . ? C6D C5D 1.390(6) . ? C6D H6D 0.9500 . ? C5D C4D 1.378(7) . ? C5D H5D 0.9500 . ? C4D C3D 1.371(7) . ? C4D H4D 0.9500 . ? C3D H3D 0.9500 . ? N1E C2E 1.334(6) . ? N1E C6E 1.335(6) . ? C2E C3E 1.380(8) . ? C2E H2E 0.9500 . ? C6E C5E 1.381(7) . ? C6E H6E 0.9500 . ? C5E C4E 1.384(8) . ? C5E H5E 0.9500 . ? C4E C3E 1.381(9) . ? C4E H4E 0.9500 . ? C3E H3E 0.9500 . ? O1S C2S 1.372(9) . ? O1S H1S 0.851(10) . ? C2S H2S1 0.9927 . ? C2S H2S2 1.0369 . ? C2S H2S3 0.9862 . ? O1T C2T 1.331(8) . ? O1T H1T 0.8027 . ? C2T H2T1 0.9802 . ? C2T H2T2 0.9798 . ? C2T H2T3 0.9799 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O123 Fe1 O2A 87.11(12) . . ? O123 Fe1 O2B 88.51(12) . . ? O2A Fe1 O2B 175.61(12) . . ? O123 Fe1 N1E 176.64(13) . . ? O2A Fe1 N1E 89.68(12) . . ? O2B Fe1 N1E 94.70(12) . . ? O123 Fe1 N1D 97.40(13) . . ? O2A Fe1 N1D 91.06(12) . . ? O2B Fe1 N1D 89.22(12) . . ? N1E Fe1 N1D 81.66(13) . . ? O123 Fe1 N1C 96.11(13) . . ? O2A Fe1 N1C 90.05(12) . . ? O2B Fe1 N1C 90.70(12) . . ? N1E Fe1 N1C 84.88(12) . . ? N1D Fe1 N1C 166.48(13) . . ? O1B Fe2 O123 139.43(13) . . ? O1B Fe2 O1F 93.69(13) . . ? O123 Fe2 O1F 77.96(12) . . ? O1B Fe2 N22B 86.43(13) . . ? O123 Fe2 N22B 83.09(12) . . ? O1F Fe2 N22B 150.84(13) . . ? O1B Fe2 Cl2 109.03(10) . . ? O123 Fe2 Cl2 111.40(10) . . ? O1F Fe2 Cl2 106.82(10) . . ? N22B Fe2 Cl2 100.62(10) . . ? O1A Fe3 O123 138.65(13) . . ? O1A Fe3 O1F 95.70(13) . . ? O123 Fe3 O1F 77.90(12) . . ? O1A Fe3 N22A 86.16(12) . . ? O123 Fe3 N22A 82.08(12) . . ? O1F Fe3 N22A 151.60(13) . . ? O1A Fe3 Cl1 107.28(10) . . ? O123 Fe3 Cl1 113.53(10) . . ? O1F Fe3 Cl1 108.49(10) . . ? N22A Fe3 Cl1 97.86(9) . . ? Fe1 O123 Fe2 126.58(15) . . ? Fe1 O123 Fe3 128.14(15) . . ? Fe2 O123 Fe3 105.28(14) . . ? C2F O1F Fe3 134.5(3) . . ? C2F O1F Fe2 126.6(3) . . ? Fe3 O1F Fe2 98.84(13) . . ? O1F C2F H2F1 109.5 . . ? O1F C2F H2F2 109.5 . . ? H2F1 C2F H2F2 109.5 . . ? O1F C2F H2F3 109.5 . . ? H2F1 C2F H2F3 109.5 . . ? H2F2 C2F H2F3 109.5 . . ? C1A O1A Fe3 131.6(3) . . ? O1A C1A C6A 118.6(4) . . ? O1A C1A C2A 122.8(4) . . ? C6A C1A C2A 118.5(4) . . ? C3A C2A C1A 118.0(4) . . ? C3A C2A C21A 118.3(4) . . ? C1A C2A C21A 123.7(4) . . ? C5A C6A C1A 121.0(5) . . ? C5A C6A H6A 119.5 . . ? C1A C6A H6A 119.5 . . ? C6A C5A C4A 121.4(5) . . ? C6A C5A H5A 119.3 . . ? C4A C5A H5A 119.3 . . ? C5A C4A C3A 119.0(5) . . ? C5A C4A H4A 120.5 . . ? C3A C4A H4A 120.5 . . ? C4A C3A C2A 122.0(5) . . ? C4A C3A H3A 119.0 . . ? C2A C3A H3A 119.0 . . ? N22A C21A C2A 120.7(4) . . ? N22A C21A C23A 119.5(4) . . ? C2A C21A C23A 119.7(4) . . ? C21A N22A O2A 115.1(3) . . ? C21A N22A Fe3 128.2(3) . . ? O2A N22A Fe3 116.7(2) . . ? C28A C23A C24A 118.9(4) . . ? C28A C23A C21A 120.0(4) . . ? C24A C23A C21A 121.0(4) . . ? C27A C28A C23A 120.4(4) . . ? C27A C28A H28A 119.8 . . ? C23A C28A H28A 119.8 . . ? C25A C24A C23A 120.2(4) . . ? C25A C24A H24A 119.9 . . ? C23A C24A H24A 119.9 . . ? C26A C25A C24A 120.1(4) . . ? C26A C25A H25A 119.9 . . ? C24A C25A H25A 119.9 . . ? C25A C26A C27A 120.7(4) . . ? C25A C26A H26A 119.7 . . ? C27A C26A H26A 119.7 . . ? C26A C27A C28A 119.7(4) . . ? C26A C27A H27A 120.1 . . ? C28A C27A H27A 120.1 . . ? N22A O2A Fe1 120.1(2) . . ? C1B O1B Fe2 132.9(3) . . ? O1B C1B C6B 117.4(4) . . ? O1B C1B C2B 123.0(4) . . ? C6B C1B C2B 119.5(4) . . ? C1B C2B C3B 117.6(4) . . ? C1B C2B C21B 123.7(4) . . ? C3B C2B C21B 118.6(4) . . ? C5B C6B C1B 121.0(5) . . ? C5B C6B H6B 119.5 . . ? C1B C6B H6B 119.5 . . ? C6B C5B C4B 120.6(5) . . ? C6B C5B H5B 119.7 . . ? C4B C5B H5B 119.7 . . ? C3B C4B C5B 119.2(5) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C4B C3B C2B 122.0(4) . . ? C4B C3B H3B 119.0 . . ? C2B C3B H3B 119.0 . . ? N22B C21B C2B 121.1(4) . . ? N22B C21B C23B 120.6(4) . . ? C2B C21B C23B 118.3(4) . . ? C21B N22B O2B 115.5(3) . . ? C21B N22B Fe2 127.9(3) . . ? O2B N22B Fe2 116.6(2) . . ? C28B C23B C24B 119.7(4) . . ? C28B C23B C21B 119.2(4) . . ? C24B C23B C21B 121.1(4) . . ? C25B C24B C23B 118.9(5) . . ? C25B C24B H24B 120.5 . . ? C23B C24B H24B 120.5 . . ? C27B C28B C23B 120.7(4) . . ? C27B C28B H28B 119.7 . . ? C23B C28B H28B 119.7 . . ? C26B C27B C28B 119.3(5) . . ? C26B C27B H27B 120.4 . . ? C28B C27B H27B 120.4 . . ? C25B C26B C27B 120.7(5) . . ? C25B C26B H26B 119.6 . . ? C27B C26B H26B 119.6 . . ? C26B C25B C24B 120.7(5) . . ? C26B C25B H25B 119.6 . . ? C24B C25B H25B 119.6 . . ? N22B O2B Fe1 119.1(2) . . ? C2C N1C C6C 117.0(4) . . ? C2C N1C Fe1 120.3(3) . . ? C6C N1C Fe1 122.6(3) . . ? N1C C2C C3C 123.4(4) . . ? N1C C2C H2C 118.3 . . ? C3C C2C H2C 118.3 . . ? N1C C6C C5C 122.9(4) . . ? N1C C6C H6C 118.5 . . ? C5C C6C H6C 118.5 . . ? C6C C5C C4C 119.4(4) . . ? C6C C5C H5C 120.3 . . ? C4C C5C H5C 120.3 . . ? C3C C4C C5C 118.0(4) . . ? C3C C4C H4C 121.0 . . ? C5C C4C H4C 121.0 . . ? C2C C3C C4C 119.2(4) . . ? C2C C3C H3C 120.4 . . ? C4C C3C H3C 120.4 . . ? C6D N1D C2D 116.9(4) . . ? C6D N1D Fe1 123.2(3) . . ? C2D N1D Fe1 119.9(3) . . ? N1D C2D C3D 123.2(5) . . ? N1D C2D H2D 118.4 . . ? C3D C2D H2D 118.4 . . ? N1D C6D C5D 123.0(4) . . ? N1D C6D H6D 118.5 . . ? C5D C6D H6D 118.5 . . ? C4D C5D C6D 118.9(4) . . ? C4D C5D H5D 120.5 . . ? C6D C5D H5D 120.5 . . ? C3D C4D C5D 118.3(4) . . ? C3D C4D H4D 120.8 . . ? C5D C4D H4D 120.8 . . ? C2D C3D C4D 119.7(5) . . ? C2D C3D H3D 120.1 . . ? C4D C3D H3D 120.1 . . ? C2E N1E C6E 118.6(4) . . ? C2E N1E Fe1 120.4(3) . . ? C6E N1E Fe1 120.7(3) . . ? N1E C2E C3E 122.0(5) . . ? N1E C2E H2E 119.0 . . ? C3E C2E H2E 119.0 . . ? N1E C6E C5E 122.8(5) . . ? N1E C6E H6E 118.6 . . ? C5E C6E H6E 118.6 . . ? C6E C5E C4E 118.5(5) . . ? C6E C5E H5E 120.8 . . ? C4E C5E H5E 120.8 . . ? C3E C4E C5E 118.6(5) . . ? C3E C4E H4E 120.7 . . ? C5E C4E H4E 120.7 . . ? C2E C3E C4E 119.4(5) . . ? C2E C3E H3E 120.3 . . ? C4E C3E H3E 120.3 . . ? C2S O1S H1S 109.0(14) . . ? O1S C2S H2S1 113.6 . . ? O1S C2S H2S2 111.8 . . ? H2S1 C2S H2S2 104.1 . . ? O1S C2S H2S3 114.0 . . ? H2S1 C2S H2S3 107.9 . . ? H2S2 C2S H2S3 104.5 . . ? C2T O1T H1T 122.8 . . ? O1T C2T H2T1 108.8 . . ? O1T C2T H2T2 109.3 . . ? H2T1 C2T H2T2 109.5 . . ? O1T C2T H2T3 110.3 . . ? H2T1 C2T H2T3 109.5 . . ? H2T2 C2T H2T3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.641 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.089 # Attachment 'Complex 2.cif' data_pt9016 _database_code_depnum_ccdc_archive 'CCDC 755036' #TrackingRef 'Complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Kevin Mason' _exptl_crystal_recrystallization_method 'Diffusion of Et2O into MeOH/Py solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Br2 Fe3 N5 O6, C4 H10 O' _chemical_formula_sum 'C46 H46 Br2 Fe3 N5 O7' _chemical_formula_weight 1108.25 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' H H 0.0000 0.0000 '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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6095(5) _cell_length_b 18.2293(6) _cell_length_c 18.2766(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.945(2) _cell_angle_gamma 90.00 _cell_volume 4808.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8117 _cell_measurement_theta_min 2.2375 _cell_measurement_theta_max 26.32 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3098 _exptl_absorpt_correction_T_max 0.4325 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41924 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.42 _reflns_number_total 9844 _reflns_number_gt 7249 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #========================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #========================================================================== Format: alert-number_ALERT_alert-type_alert-level text 360_ALERT_2_B Short C(sp3)-C(sp3) Bond C4S - C5S ... 1.30 Ang. 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C2S 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C4S 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O1S 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O1S' 302_ALERT_4_G Note Anion/Solvent Disorder .................... 29.00 Perc. There is solvent ether in the structure. It is poorly behaved and disordered. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.95 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3E This atom is in a pyridine ring which has ADP's consistent with a 'wagging' motion. 232_ALERT_2_C Hirshfeld Test Diff (M-X) Br1 -- Fe1 .. 7.42 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Br2 -- Fe2 .. 7.12 su This often happens in complexes like this. 063_ALERT_4_B Crystal Size Likely too Large for Beam Size .... 0.66 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 39 The data collection strategy used was to collect fully complete data to 2TH= 53deg. Some higher angle data were collected in the process and these have been included in the refinement. Please refer to the completeness statistics below #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 5038 5038 0 23.01 0.550 1.000 6699 6699 0 25.24 0.600 1.000 8678 8677 1 #----------------------------------------------------------- ACTA Min. Res. --- 26.42 0.626 0.996 9884 9844 40 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 18 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+2.2788P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9844 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12299(3) 0.83994(2) 0.21997(2) 0.02978(12) Uani 1 1 d . . . Fe2 Fe 0.33097(3) 0.84901(2) 0.25288(2) 0.02879(12) Uani 1 1 d . . . Fe3 Fe 0.23737(3) 0.67927(2) 0.23823(2) 0.02574(11) Uani 1 1 d . . . Br1 Br 0.04413(3) 0.85145(2) 0.323431(19) 0.04693(12) Uani 1 1 d . . . Br2 Br 0.41214(3) 0.86005(2) 0.150538(18) 0.04106(11) Uani 1 1 d . . . O123 O 0.23049(14) 0.78103(12) 0.23947(11) 0.0321(5) Uani 1 1 d . . . O1A O 0.05562(15) 0.88770(12) 0.13818(12) 0.0375(5) Uani 1 1 d . . . C1A C -0.0290(2) 0.87316(18) 0.10360(18) 0.0363(8) Uani 1 1 d . . . C2A C -0.0657(2) 0.80136(19) 0.09616(18) 0.0360(8) Uani 1 1 d . . . C3A C -0.1559(2) 0.7925(2) 0.0583(2) 0.0524(10) Uani 1 1 d . . . H3A H -0.1813 0.7445 0.0521 0.063 Uiso 1 1 calc R . . C4A C -0.2093(3) 0.8515(2) 0.0299(3) 0.0691(14) Uani 1 1 d . . . H4A H -0.2712 0.8442 0.0061 0.083 Uiso 1 1 calc R . . C5A C -0.1716(3) 0.9211(2) 0.0364(2) 0.0666(13) Uani 1 1 d . . . H5A H -0.2074 0.9618 0.0159 0.080 Uiso 1 1 calc R . . C6A C -0.0830(3) 0.9320(2) 0.0720(2) 0.0518(10) Uani 1 1 d . . . H6A H -0.0578 0.9802 0.0754 0.062 Uiso 1 1 calc R . . C21A C -0.0126(2) 0.73560(17) 0.12305(16) 0.0300(7) Uani 1 1 d . . . N22A N 0.06083(17) 0.74100(14) 0.17350(13) 0.0297(6) Uani 1 1 d . . . O23A O 0.10536(14) 0.67665(11) 0.19431(11) 0.0288(5) Uani 1 1 d . . . C24A C -0.0444(2) 0.66337(18) 0.09083(18) 0.0327(7) Uani 1 1 d . . . C25A C -0.0469(2) 0.65154(19) 0.01538(19) 0.0398(8) Uani 1 1 d . . . H25A H -0.0274 0.6894 -0.0145 0.048 Uiso 1 1 calc R . . C26A C -0.0773(2) 0.5856(2) -0.0167(2) 0.0498(10) Uani 1 1 d . . . H26A H -0.0769 0.5777 -0.0680 0.060 Uiso 1 1 calc R . . C27A C -0.1081(2) 0.5319(2) 0.0255(2) 0.0528(10) Uani 1 1 d . . . H27A H -0.1310 0.4871 0.0031 0.063 Uiso 1 1 calc R . . C28A C -0.1061(3) 0.5423(2) 0.1004(2) 0.0557(11) Uani 1 1 d . . . H28A H -0.1269 0.5045 0.1296 0.067 Uiso 1 1 calc R . . C29A C -0.0741(2) 0.6074(2) 0.1331(2) 0.0441(9) Uani 1 1 d . . . H29A H -0.0724 0.6141 0.1848 0.053 Uiso 1 1 calc R . . O1B O 0.39425(15) 0.90417(12) 0.33127(11) 0.0360(5) Uani 1 1 d . . . C1B C 0.4791(2) 0.89501(18) 0.36914(17) 0.0343(8) Uani 1 1 d . . . C2B C 0.5222(2) 0.82619(17) 0.38004(16) 0.0315(7) Uani 1 1 d . . . C3B C 0.6119(2) 0.8231(2) 0.4202(2) 0.0441(9) Uani 1 1 d . . . H3B H 0.6421 0.7769 0.4277 0.053 Uiso 1 1 calc R . . C4B C 0.6576(3) 0.8852(2) 0.4490(2) 0.0612(12) Uani 1 1 d . . . H4B H 0.7194 0.8821 0.4744 0.073 Uiso 1 1 calc R . . C5B C 0.6127(3) 0.9520(2) 0.4404(2) 0.0611(12) Uani 1 1 d . . . H5B H 0.6427 0.9947 0.4623 0.073 Uiso 1 1 calc R . . C6B C 0.5255(3) 0.95727(19) 0.4008(2) 0.0466(9) Uani 1 1 d . . . H6B H 0.4960 1.0038 0.3947 0.056 Uiso 1 1 calc R . . C21B C 0.4777(2) 0.75697(17) 0.35373(15) 0.0271(7) Uani 1 1 d . . . N22B N 0.40409(17) 0.75665(13) 0.30324(13) 0.0273(6) Uani 1 1 d . . . O23B O 0.36846(13) 0.68923(11) 0.28263(10) 0.0282(5) Uani 1 1 d . . . C24B C 0.5161(2) 0.68648(17) 0.38557(16) 0.0276(7) Uani 1 1 d . . . C25B C 0.5536(2) 0.63517(19) 0.34275(19) 0.0385(8) Uani 1 1 d . . . H25B H 0.5579 0.6461 0.2926 0.046 Uiso 1 1 calc R . . C26B C 0.5846(2) 0.5689(2) 0.3721(2) 0.0458(9) Uani 1 1 d . . . H26B H 0.6102 0.5343 0.3421 0.055 Uiso 1 1 calc R . . C27B C 0.5789(2) 0.55217(19) 0.4448(2) 0.0420(9) Uani 1 1 d . . . H27B H 0.5998 0.5058 0.4646 0.050 Uiso 1 1 calc R . . C28B C 0.5431(2) 0.60253(19) 0.48881(19) 0.0395(8) Uani 1 1 d . . . H28B H 0.5399 0.5914 0.5391 0.047 Uiso 1 1 calc R . . C29B C 0.5115(2) 0.66976(18) 0.45905(16) 0.0316(7) Uani 1 1 d . . . H29B H 0.4865 0.7046 0.4892 0.038 Uiso 1 1 calc R . . O1C O 0.22227(14) 0.91444(12) 0.23291(12) 0.0396(6) Uani 1 1 d . . . C2C C 0.2154(3) 0.9914(2) 0.2225(2) 0.0542(10) Uani 1 1 d . . . H2C1 H 0.2239 1.0035 0.1718 0.081 Uiso 1 1 calc R . . H2C2 H 0.2634 1.0158 0.2576 0.081 Uiso 1 1 calc R . . H2C3 H 0.1541 1.0080 0.2311 0.081 Uiso 1 1 calc R . . N1D N 0.27564(18) 0.67033(14) 0.12644(13) 0.0294(6) Uani 1 1 d . . . C2D C 0.2100(2) 0.6691(2) 0.06678(18) 0.0448(9) Uani 1 1 d . . . H2D H 0.1470 0.6724 0.0736 0.054 Uiso 1 1 calc R . . C3D C 0.2299(3) 0.6634(2) -0.00460(19) 0.0560(11) Uani 1 1 d . . . H3D H 0.1814 0.6633 -0.0458 0.067 Uiso 1 1 calc R . . C4D C 0.3203(3) 0.6578(2) -0.01501(19) 0.0460(9) Uani 1 1 d . . . H4D H 0.3356 0.6537 -0.0635 0.055 Uiso 1 1 calc R . . C5D C 0.3877(3) 0.6583(2) 0.0452(2) 0.0452(9) Uani 1 1 d . . . H5D H 0.4511 0.6541 0.0396 0.054 Uiso 1 1 calc R . . C6D C 0.3624(2) 0.66502(19) 0.11491(18) 0.0372(8) Uani 1 1 d . . . H6D H 0.4101 0.6658 0.1567 0.045 Uiso 1 1 calc R . . N1E N 0.25428(17) 0.56102(14) 0.24084(13) 0.0290(6) Uani 1 1 d . . . C2E C 0.1818(3) 0.5167(2) 0.2274(2) 0.0482(10) Uani 1 1 d . . . H2E H 0.1220 0.5375 0.2135 0.058 Uiso 1 1 calc R . . C3E C 0.1902(3) 0.4414(2) 0.2327(3) 0.0800(16) Uani 1 1 d . . . H3E H 0.1369 0.4109 0.2231 0.096 Uiso 1 1 calc R . . C4E C 0.2765(3) 0.4112(2) 0.2521(3) 0.0796(16) Uani 1 1 d . . . H4E H 0.2839 0.3595 0.2556 0.096 Uiso 1 1 calc R . . C5E C 0.3506(3) 0.4557(2) 0.2661(2) 0.0602(12) Uani 1 1 d . . . H5E H 0.4110 0.4360 0.2797 0.072 Uiso 1 1 calc R . . C6E C 0.3374(2) 0.53016(19) 0.26024(19) 0.0442(9) Uani 1 1 d . . . H6E H 0.3900 0.5613 0.2705 0.053 Uiso 1 1 calc R . . N1F N 0.19733(19) 0.66061(14) 0.34826(14) 0.0322(6) Uani 1 1 d . . . C2F C 0.2630(3) 0.6454(2) 0.40603(18) 0.0441(9) Uani 1 1 d . . . H2F H 0.3259 0.6443 0.3985 0.053 Uiso 1 1 calc R . . C3F C 0.2429(3) 0.6315(2) 0.47559(19) 0.0555(11) Uani 1 1 d . . . H3F H 0.2914 0.6215 0.5153 0.067 Uiso 1 1 calc R . . C4F C 0.1528(3) 0.6321(2) 0.4875(2) 0.0550(11) Uani 1 1 d . . . H4F H 0.1375 0.6223 0.5352 0.066 Uiso 1 1 calc R . . C5F C 0.0852(3) 0.6472(2) 0.4288(2) 0.0533(10) Uani 1 1 d . . . H5F H 0.0219 0.6480 0.4350 0.064 Uiso 1 1 calc R . . C6F C 0.1103(3) 0.6613(2) 0.36035(18) 0.0418(9) Uani 1 1 d . . . H6F H 0.0629 0.6721 0.3200 0.050 Uiso 1 1 calc R . . O1S O 0.7201(3) 0.7779(3) 0.7468(2) 0.0842(17) Uiso 0.870(9) 1 d P A 1 O1S' O 0.7388(12) 0.8360(11) 0.7440(9) 0.035(7) Uiso 0.130(9) 1 d P A 2 C2S C 0.6920(6) 0.8056(5) 0.6788(5) 0.150(3) Uiso 1 1 d . . . H2S1 H 0.6763 0.8579 0.6843 0.180 Uiso 1 1 calc R A 1 H2S2 H 0.7448 0.8036 0.6509 0.180 Uiso 1 1 calc R A 1 C3S C 0.6242(5) 0.7748(5) 0.6410(4) 0.101(3) Uiso 0.731(9) 1 d P A 1 H3S1 H 0.6102 0.7991 0.5927 0.152 Uiso 0.731(9) 1 calc PR A 1 H3S2 H 0.5703 0.7781 0.6667 0.152 Uiso 0.731(9) 1 calc PR A 1 H3S3 H 0.6390 0.7231 0.6338 0.152 Uiso 0.731(9) 1 calc PR A 1 C3S' C 0.6342(12) 0.8526(10) 0.6356(9) 0.067(6) Uiso 0.269(9) 1 d P A 2 H3S4 H 0.6482 0.8514 0.5848 0.101 Uiso 0.269(9) 1 calc PR A 2 H3S5 H 0.6433 0.9025 0.6553 0.101 Uiso 0.269(9) 1 calc PR A 2 H3S6 H 0.5698 0.8377 0.6355 0.101 Uiso 0.269(9) 1 calc PR A 2 C4S C 0.7984(6) 0.7952(5) 0.7849(4) 0.151(3) Uiso 1 1 d . . . H4S1 H 0.7988 0.8495 0.7878 0.181 Uiso 1 1 calc R A 1 H4S2 H 0.8458 0.7817 0.7541 0.181 Uiso 1 1 calc R A 1 C5S C 0.8300(5) 0.7724(4) 0.8513(4) 0.130(2) Uiso 1 1 d . A . H5S1 H 0.8901 0.7954 0.8685 0.195 Uiso 1 1 calc R . . H5S2 H 0.8375 0.7190 0.8508 0.195 Uiso 1 1 calc R . . H5S3 H 0.7863 0.7855 0.8848 0.195 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 Fe1 0.0298(3) 0.0251(3) 0.0338(2) -0.00022(18) 0.00328(19) 0.0042(2) Fe2 0.0298(3) 0.0232(3) 0.0326(2) 0.00173(18) 0.00254(19) -0.0017(2) Fe3 0.0260(2) 0.0223(2) 0.0281(2) 0.00071(17) 0.00135(17) 0.00051(19) Br1 0.0481(2) 0.0533(3) 0.0404(2) -0.00883(16) 0.01002(16) 0.01042(18) Br2 0.0467(2) 0.0420(2) 0.03478(18) 0.00621(14) 0.00705(15) -0.00856(17) O123 0.0288(12) 0.0227(12) 0.0435(12) 0.0014(9) 0.0016(10) 0.0002(10) O1A 0.0413(14) 0.0281(13) 0.0411(13) 0.0048(10) 0.0000(10) 0.0023(11) C1A 0.036(2) 0.032(2) 0.0390(18) 0.0020(14) 0.0024(15) 0.0065(16) C2A 0.0295(18) 0.034(2) 0.0438(19) 0.0029(15) 0.0037(14) 0.0069(16) C3A 0.034(2) 0.036(2) 0.083(3) -0.001(2) -0.0063(19) 0.0057(18) C4A 0.038(2) 0.048(3) 0.112(4) 0.002(2) -0.018(2) 0.014(2) C5A 0.054(3) 0.040(3) 0.097(3) 0.004(2) -0.018(2) 0.020(2) C6A 0.052(2) 0.031(2) 0.067(3) 0.0013(18) -0.0071(19) 0.0069(18) C21A 0.0258(17) 0.0304(18) 0.0348(16) 0.0027(13) 0.0076(13) 0.0034(14) N22A 0.0285(15) 0.0273(15) 0.0337(14) 0.0021(11) 0.0058(11) 0.0046(12) O23A 0.0271(12) 0.0236(12) 0.0343(11) 0.0030(9) 0.0004(9) 0.0037(9) C24A 0.0191(16) 0.0307(19) 0.0461(19) 0.0028(14) -0.0024(13) 0.0073(14) C25A 0.0297(19) 0.041(2) 0.047(2) 0.0009(16) -0.0007(15) 0.0019(16) C26A 0.038(2) 0.048(3) 0.060(2) -0.0174(19) -0.0006(18) -0.0003(19) C27A 0.033(2) 0.039(2) 0.083(3) -0.013(2) -0.0033(19) 0.0012(18) C28A 0.044(2) 0.035(2) 0.085(3) 0.013(2) 0.002(2) -0.0028(19) C29A 0.044(2) 0.035(2) 0.051(2) 0.0076(17) 0.0013(17) 0.0013(18) O1B 0.0408(14) 0.0275(13) 0.0381(12) -0.0039(10) 0.0017(10) 0.0010(11) C1B 0.038(2) 0.032(2) 0.0329(17) -0.0013(14) 0.0053(14) -0.0061(16) C2B 0.0315(18) 0.0289(18) 0.0334(16) -0.0010(13) 0.0026(13) -0.0067(15) C3B 0.033(2) 0.035(2) 0.060(2) 0.0005(17) -0.0035(16) -0.0072(17) C4B 0.042(2) 0.046(3) 0.087(3) 0.000(2) -0.017(2) -0.014(2) C5B 0.060(3) 0.035(2) 0.081(3) -0.008(2) -0.011(2) -0.016(2) C6B 0.050(2) 0.027(2) 0.060(2) -0.0040(16) -0.0027(18) -0.0035(17) C21B 0.0244(17) 0.0288(18) 0.0292(15) 0.0001(13) 0.0078(13) -0.0037(13) N22B 0.0312(15) 0.0205(14) 0.0304(13) 0.0014(10) 0.0057(11) -0.0047(11) O23B 0.0283(12) 0.0217(12) 0.0332(11) -0.0022(9) -0.0002(9) -0.0012(9) C24B 0.0187(15) 0.0275(18) 0.0357(16) -0.0010(13) 0.0014(12) -0.0053(13) C25B 0.0316(19) 0.043(2) 0.0413(19) -0.0030(16) 0.0075(15) 0.0021(16) C26B 0.034(2) 0.036(2) 0.068(3) -0.0106(18) 0.0099(17) 0.0049(17) C27B 0.0253(19) 0.028(2) 0.071(2) 0.0074(17) 0.0000(17) -0.0001(15) C28B 0.0330(19) 0.037(2) 0.047(2) 0.0099(16) 0.0007(15) -0.0025(16) C29B 0.0264(17) 0.0327(19) 0.0347(17) -0.0043(14) 0.0017(13) -0.0017(14) O1C 0.0350(14) 0.0228(13) 0.0600(15) 0.0026(10) 0.0041(11) 0.0020(10) C2C 0.049(2) 0.029(2) 0.087(3) 0.0080(19) 0.017(2) 0.0033(18) N1D 0.0303(15) 0.0258(15) 0.0316(13) 0.0005(11) 0.0032(11) -0.0004(12) C2D 0.0318(19) 0.069(3) 0.0322(18) -0.0007(17) 0.0013(14) 0.0087(18) C3D 0.052(3) 0.083(3) 0.0319(19) 0.0001(19) 0.0029(17) 0.008(2) C4D 0.059(3) 0.048(2) 0.0340(19) 0.0000(16) 0.0158(17) 0.0005(19) C5D 0.039(2) 0.052(2) 0.048(2) -0.0043(17) 0.0168(17) -0.0013(18) C6D 0.0335(19) 0.041(2) 0.0362(18) -0.0038(15) 0.0035(14) -0.0021(16) N1E 0.0308(15) 0.0248(15) 0.0298(13) 0.0005(10) -0.0003(11) 0.0004(12) C2E 0.038(2) 0.036(2) 0.065(2) 0.0018(18) -0.0072(18) -0.0036(18) C3E 0.066(3) 0.033(3) 0.128(4) 0.005(2) -0.026(3) -0.017(2) C4E 0.081(4) 0.028(2) 0.115(4) 0.005(2) -0.031(3) 0.002(2) C5E 0.051(3) 0.037(2) 0.085(3) 0.003(2) -0.015(2) 0.009(2) C6E 0.037(2) 0.030(2) 0.063(2) -0.0006(17) 0.0004(17) -0.0012(17) N1F 0.0367(16) 0.0276(15) 0.0320(14) -0.0001(11) 0.0042(12) -0.0012(12) C2F 0.043(2) 0.053(2) 0.0341(18) 0.0002(16) -0.0021(15) -0.0071(18) C3F 0.062(3) 0.072(3) 0.0292(19) 0.0035(18) -0.0021(18) -0.008(2) C4F 0.083(3) 0.054(3) 0.032(2) 0.0032(17) 0.021(2) 0.002(2) C5F 0.057(3) 0.058(3) 0.050(2) 0.0081(19) 0.023(2) 0.011(2) C6F 0.044(2) 0.045(2) 0.0371(19) 0.0044(15) 0.0070(16) 0.0108(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1A 1.872(2) . ? Fe1 O123 1.890(2) . ? Fe1 O1C 1.974(2) . ? Fe1 N22A 2.135(3) . ? Fe1 Br1 2.3716(6) . ? Fe2 O1B 1.873(2) . ? Fe2 O123 1.908(2) . ? Fe2 O1C 1.974(2) . ? Fe2 N22B 2.125(2) . ? Fe2 Br2 2.3739(6) . ? Fe3 O123 1.858(2) . ? Fe3 O23B 1.9687(19) . ? Fe3 O23A 1.971(2) . ? Fe3 N1E 2.169(3) . ? Fe3 N1F 2.206(3) . ? Fe3 N1D 2.207(2) . ? O1A C1A 1.325(4) . ? C1A C6A 1.401(5) . ? C1A C2A 1.413(5) . ? C2A C3A 1.400(5) . ? C2A C21A 1.470(4) . ? C3A C4A 1.381(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.381(6) . ? C4A H4A 0.9500 . ? C5A C6A 1.370(5) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C21A N22A 1.306(4) . ? C21A C24A 1.487(4) . ? N22A O23A 1.366(3) . ? C24A C29A 1.389(5) . ? C24A C25A 1.390(5) . ? C25A C26A 1.380(5) . ? C25A H25A 0.9500 . ? C26A C27A 1.365(5) . ? C26A H26A 0.9500 . ? C27A C28A 1.378(5) . ? C27A H27A 0.9500 . ? C28A C29A 1.377(5) . ? C28A H28A 0.9500 . ? C29A H29A 0.9500 . ? O1B C1B 1.333(4) . ? C1B C6B 1.401(5) . ? C1B C2B 1.404(5) . ? C2B C3B 1.401(4) . ? C2B C21B 1.466(4) . ? C3B C4B 1.376(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.381(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.367(5) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C21B N22B 1.303(4) . ? C21B C24B 1.484(4) . ? N22B O23B 1.365(3) . ? C24B C25B 1.386(4) . ? C24B C29B 1.389(4) . ? C25B C26B 1.369(5) . ? C25B H25B 0.9500 . ? C26B C27B 1.380(5) . ? C26B H26B 0.9500 . ? C27B C28B 1.376(5) . ? C27B H27B 0.9500 . ? C28B C29B 1.390(4) . ? C28B H28B 0.9500 . ? C29B H29B 0.9500 . ? O1C C2C 1.417(4) . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? N1D C6D 1.320(4) . ? N1D C2D 1.335(4) . ? C2D C3D 1.384(5) . ? C2D H2D 0.9500 . ? C3D C4D 1.366(5) . ? C3D H3D 0.9500 . ? C4D C5D 1.358(5) . ? C4D H4D 0.9500 . ? C5D C6D 1.387(4) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? N1E C2E 1.324(4) . ? N1E C6E 1.336(4) . ? C2E C3E 1.381(5) . ? C2E H2E 0.9500 . ? C3E C4E 1.370(6) . ? C3E H3E 0.9500 . ? C4E C5E 1.346(6) . ? C4E H4E 0.9500 . ? C5E C6E 1.372(5) . ? C5E H5E 0.9500 . ? C6E H6E 0.9500 . ? N1F C6F 1.324(4) . ? N1F C2F 1.341(4) . ? C2F C3F 1.372(5) . ? C2F H2F 0.9500 . ? C3F C4F 1.368(6) . ? C3F H3F 0.9500 . ? C4F C5F 1.368(5) . ? C4F H4F 0.9500 . ? C5F C6F 1.381(5) . ? C5F H5F 0.9500 . ? C6F H6F 0.9500 . ? O1S C4S 1.283(8) . ? O1S C2S 1.344(8) . ? O1S' C4S 1.291(18) . ? O1S' C2S 1.393(17) . ? C2S C3S 1.249(9) . ? C2S C3S' 1.365(17) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C3S' H3S4 0.9800 . ? C3S' H3S5 0.9800 . ? C3S' H3S6 0.9800 . ? C4S C5S 1.298(8) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Fe1 O123 137.15(9) . . ? O1A Fe1 O1C 93.50(9) . . ? O123 Fe1 O1C 78.16(9) . . ? O1A Fe1 N22A 86.38(10) . . ? O123 Fe1 N22A 83.38(9) . . ? O1C Fe1 N22A 152.60(9) . . ? O1A Fe1 Br1 109.59(7) . . ? O123 Fe1 Br1 113.10(6) . . ? O1C Fe1 Br1 106.42(7) . . ? N22A Fe1 Br1 99.36(7) . . ? O1B Fe2 O123 136.52(9) . . ? O1B Fe2 O1C 95.98(9) . . ? O123 Fe2 O1C 77.76(9) . . ? O1B Fe2 N22B 86.50(9) . . ? O123 Fe2 N22B 82.30(9) . . ? O1C Fe2 N22B 153.42(9) . . ? O1B Fe2 Br2 108.03(7) . . ? O123 Fe2 Br2 115.00(6) . . ? O1C Fe2 Br2 106.80(7) . . ? N22B Fe2 Br2 97.44(7) . . ? O123 Fe3 O23B 87.36(9) . . ? O123 Fe3 O23A 88.73(9) . . ? O23B Fe3 O23A 176.07(9) . . ? O123 Fe3 N1E 176.32(9) . . ? O23B Fe3 N1E 88.99(9) . . ? O23A Fe3 N1E 94.92(9) . . ? O123 Fe3 N1F 96.91(9) . . ? O23B Fe3 N1F 90.99(9) . . ? O23A Fe3 N1F 89.21(9) . . ? N1E Fe3 N1F 82.65(9) . . ? O123 Fe3 N1D 96.15(9) . . ? O23B Fe3 N1D 91.04(9) . . ? O23A Fe3 N1D 89.65(9) . . ? N1E Fe3 N1D 84.41(9) . . ? N1F Fe3 N1D 166.87(10) . . ? Fe3 O123 Fe1 127.58(11) . . ? Fe3 O123 Fe2 127.46(11) . . ? Fe1 O123 Fe2 104.80(10) . . ? C1A O1A Fe1 128.6(2) . . ? O1A C1A C6A 117.8(3) . . ? O1A C1A C2A 122.9(3) . . ? C6A C1A C2A 119.3(3) . . ? C3A C2A C1A 117.9(3) . . ? C3A C2A C21A 118.6(3) . . ? C1A C2A C21A 123.5(3) . . ? C4A C3A C2A 122.0(4) . . ? C4A C3A H3A 119.0 . . ? C2A C3A H3A 119.0 . . ? C3A C4A C5A 119.2(4) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C6A C5A C4A 120.6(4) . . ? C6A C5A H5A 119.7 . . ? C4A C5A H5A 119.7 . . ? C5A C6A C1A 120.9(4) . . ? C5A C6A H6A 119.5 . . ? C1A C6A H6A 119.5 . . ? N22A C21A C2A 120.5(3) . . ? N22A C21A C24A 121.2(3) . . ? C2A C21A C24A 118.3(3) . . ? C21A N22A O23A 115.8(2) . . ? C21A N22A Fe1 126.6(2) . . ? O23A N22A Fe1 117.37(17) . . ? N22A O23A Fe3 119.08(17) . . ? C29A C24A C25A 118.4(3) . . ? C29A C24A C21A 122.4(3) . . ? C25A C24A C21A 119.3(3) . . ? C26A C25A C24A 120.9(3) . . ? C26A C25A H25A 119.6 . . ? C24A C25A H25A 119.6 . . ? C27A C26A C25A 119.8(4) . . ? C27A C26A H26A 120.1 . . ? C25A C26A H26A 120.1 . . ? C26A C27A C28A 120.3(4) . . ? C26A C27A H27A 119.9 . . ? C28A C27A H27A 119.9 . . ? C29A C28A C27A 120.2(4) . . ? C29A C28A H28A 119.9 . . ? C27A C28A H28A 119.9 . . ? C28A C29A C24A 120.4(4) . . ? C28A C29A H29A 119.8 . . ? C24A C29A H29A 119.8 . . ? C1B O1B Fe2 129.7(2) . . ? O1B C1B C6B 117.7(3) . . ? O1B C1B C2B 123.1(3) . . ? C6B C1B C2B 119.2(3) . . ? C3B C2B C1B 118.2(3) . . ? C3B C2B C21B 117.9(3) . . ? C1B C2B C21B 123.8(3) . . ? C4B C3B C2B 121.7(4) . . ? C4B C3B H3B 119.1 . . ? C2B C3B H3B 119.1 . . ? C3B C4B C5B 119.3(4) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C6B C5B C4B 120.6(4) . . ? C6B C5B H5B 119.7 . . ? C4B C5B H5B 119.7 . . ? C5B C6B C1B 120.9(3) . . ? C5B C6B H6B 119.5 . . ? C1B C6B H6B 119.5 . . ? N22B C21B C2B 120.7(3) . . ? N22B C21B C24B 119.6(3) . . ? C2B C21B C24B 119.7(3) . . ? C21B N22B O23B 115.9(2) . . ? C21B N22B Fe2 127.4(2) . . ? O23B N22B Fe2 116.70(17) . . ? N22B O23B Fe3 120.11(16) . . ? C25B C24B C29B 118.7(3) . . ? C25B C24B C21B 121.4(3) . . ? C29B C24B C21B 119.8(3) . . ? C26B C25B C24B 120.7(3) . . ? C26B C25B H25B 119.7 . . ? C24B C25B H25B 119.7 . . ? C25B C26B C27B 120.4(3) . . ? C25B C26B H26B 119.8 . . ? C27B C26B H26B 119.8 . . ? C28B C27B C26B 120.1(3) . . ? C28B C27B H27B 120.0 . . ? C26B C27B H27B 120.0 . . ? C27B C28B C29B 119.5(3) . . ? C27B C28B H28B 120.2 . . ? C29B C28B H28B 120.2 . . ? C24B C29B C28B 120.6(3) . . ? C24B C29B H29B 119.7 . . ? C28B C29B H29B 119.7 . . ? C2C O1C Fe1 129.0(2) . . ? C2C O1C Fe2 131.4(2) . . ? Fe1 O1C Fe2 99.29(10) . . ? O1C C2C H2C1 109.5 . . ? O1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? O1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? C6D N1D C2D 117.0(3) . . ? C6D N1D Fe3 122.7(2) . . ? C2D N1D Fe3 120.3(2) . . ? N1D C2D C3D 122.8(3) . . ? N1D C2D H2D 118.6 . . ? C3D C2D H2D 118.6 . . ? C4D C3D C2D 119.1(3) . . ? C4D C3D H3D 120.5 . . ? C2D C3D H3D 120.5 . . ? C5D C4D C3D 118.8(3) . . ? C5D C4D H4D 120.6 . . ? C3D C4D H4D 120.6 . . ? C4D C5D C6D 118.8(3) . . ? C4D C5D H5D 120.6 . . ? C6D C5D H5D 120.6 . . ? N1D C6D C5D 123.6(3) . . ? N1D C6D H6D 118.2 . . ? C5D C6D H6D 118.2 . . ? C2E N1E C6E 117.4(3) . . ? C2E N1E Fe3 121.1(2) . . ? C6E N1E Fe3 121.3(2) . . ? N1E C2E C3E 122.3(4) . . ? N1E C2E H2E 118.9 . . ? C3E C2E H2E 118.9 . . ? C4E C3E C2E 119.0(4) . . ? C4E C3E H3E 120.5 . . ? C2E C3E H3E 120.5 . . ? C5E C4E C3E 119.3(4) . . ? C5E C4E H4E 120.4 . . ? C3E C4E H4E 120.4 . . ? C4E C5E C6E 118.8(4) . . ? C4E C5E H5E 120.6 . . ? C6E C5E H5E 120.6 . . ? N1E C6E C5E 123.2(3) . . ? N1E C6E H6E 118.4 . . ? C5E C6E H6E 118.4 . . ? C6F N1F C2F 117.3(3) . . ? C6F N1F Fe3 123.2(2) . . ? C2F N1F Fe3 119.4(2) . . ? N1F C2F C3F 122.5(4) . . ? N1F C2F H2F 118.8 . . ? C3F C2F H2F 118.8 . . ? C4F C3F C2F 119.8(4) . . ? C4F C3F H3F 120.1 . . ? C2F C3F H3F 120.1 . . ? C3F C4F C5F 118.1(3) . . ? C3F C4F H4F 120.9 . . ? C5F C4F H4F 120.9 . . ? C4F C5F C6F 119.2(4) . . ? C4F C5F H5F 120.4 . . ? C6F C5F H5F 120.4 . . ? N1F C6F C5F 123.1(3) . . ? N1F C6F H6F 118.4 . . ? C5F C6F H6F 118.4 . . ? C4S O1S C2S 121.8(6) . . ? C4S O1S' C2S 117.6(15) . . ? C3S C2S O1S 116.4(8) . . ? C3S C2S C3S' 66.2(9) . . ? O1S C2S C3S' 147.5(11) . . ? C3S C2S O1S' 153.4(11) . . ? O1S C2S O1S' 47.2(8) . . ? C3S' C2S O1S' 115.0(13) . . ? C3S C2S H2S1 108.2 . . ? O1S C2S H2S1 108.2 . . ? C3S' C2S H2S1 47.2 . . ? O1S' C2S H2S1 67.8 . . ? C3S C2S H2S2 108.2 . . ? O1S C2S H2S2 108.2 . . ? C3S' C2S H2S2 100.7 . . ? O1S' C2S H2S2 97.9 . . ? H2S1 C2S H2S2 107.3 . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C2S C3S' H3S4 109.5 . . ? C2S C3S' H3S5 109.5 . . ? H3S4 C3S' H3S5 109.5 . . ? C2S C3S' H3S6 109.5 . . ? H3S4 C3S' H3S6 109.5 . . ? H3S5 C3S' H3S6 109.5 . . ? O1S C4S O1S' 50.5(9) . . ? O1S C4S C5S 125.9(8) . . ? O1S' C4S C5S 146.8(11) . . ? O1S C4S H4S1 105.9 . . ? O1S' C4S H4S1 56.9 . . ? C5S C4S H4S1 105.9 . . ? O1S C4S H4S2 105.9 . . ? O1S' C4S H4S2 106.4 . . ? C5S C4S H4S2 105.9 . . ? H4S1 C4S H4S2 106.2 . . ? C4S C5S H5S1 109.5 . . ? C4S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? C4S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.721 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.082 # Attachment 'Complex 3.cif' data_eb9020 _database_code_depnum_ccdc_archive 'CCDC 755037' #TrackingRef 'Complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Kevin Mason' _exptl_crystal_recrystallization_method 'Slow evaporation of MeOH/pyridine solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H56 F4 Fe4 N8 O8, 1.5(MeOH)' _chemical_formula_sum 'C73.50 H62 F4 Fe4 N8 O9.50' _chemical_formula_weight 1508.71 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' H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.0878(16) _cell_length_b 20.7755(12) _cell_length_c 27.5991(17) _cell_angle_alpha 90.00 _cell_angle_beta 115.9810(10) _cell_angle_gamma 90.00 _cell_volume 13446.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7456 _cell_measurement_theta_min 2.4285 _cell_measurement_theta_max 26.3075 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6200 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.9392 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 72924 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.26 _reflns_number_total 19311 _reflns_number_gt 14464 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; #========================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #========================================================================== Format: alert-number_ALERT_alert-type_alert-level text 023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.26 Deg. 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 High resolution data had poor merging statistics and were cutoff at 0.9 ang. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.67 Ratio 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.26 Ratio 213_ALERT_2_C Atom C27M has ADP max/min Ratio ............. 3.30 prola 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3F 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3R 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5Q Thermal ellipsoids are consistent with wagging of these groups 230_ALERT_2_B Hirshfeld Test Diff for N1F -- C6F .. 11.22 su 432_ALERT_2_C Short Inter X...Y Contact O1D .. C4F .. 3.01 Ang. 234_ALERT_4_C Large Hirshfeld Difference C2F -- C3F .. 0.22 Ang. 234_ALERT_4_C Large Hirshfeld Difference C3E -- C4E .. 0.16 Ang. 234_ALERT_4_C Large Hirshfeld Difference C4F -- C5F .. 0.19 Ang. Noted. 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 164.00 A**3 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 043_ALERT_1_C Check Reported Molecular Weight ................ 1508.71 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? Squeeze was used to treat the solvent region. One and a half methanol molecules per unit formula were removed from the cell. The formula, F(000) and d calc were calculated with this in mind. 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.03 Residual density is centred around Fe atoms and thus cannot represent missed atoms. Twin laws have been checked for also. 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 6 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.556 6 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 2 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 14081 14072 9 23.01 0.550 0.999 18728 18717 11 23.26 0.556 0.999 19323 19311 12 #----------------------------------------------------------- ACTA Min. Res. --- 083_ALERT_2_G SHELXL Second Parameter in WGHT unusually Large. 56.00 The data are of rather poor quality. 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+56.0031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19311 _refine_ls_number_parameters 1717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.49035(4) 0.27924(5) 0.74983(4) 0.0211(3) Uani 1 1 d . . . Fe2 Fe 0.42721(5) 0.13435(5) 0.75397(4) 0.0234(3) Uani 1 1 d . . . Fe3 Fe 0.30136(5) 0.21243(5) 0.73085(4) 0.0232(3) Uani 1 1 d . . . Fe4 Fe 0.37698(5) 0.35640(5) 0.75671(4) 0.0233(3) Uani 1 1 d . . . F12 F 0.43394(17) 0.21041(18) 0.71432(14) 0.0263(10) Uani 1 1 d . . . F23 F 0.37874(17) 0.18294(19) 0.77990(15) 0.0286(10) Uani 1 1 d . . . F34 F 0.33513(18) 0.28552(18) 0.70805(15) 0.0299(10) Uani 1 1 d . . . F41 F 0.44516(17) 0.30234(18) 0.78878(15) 0.0283(10) Uani 1 1 d . . . O1A O 0.5274(2) 0.2694(2) 0.70445(17) 0.0248(12) Uani 1 1 d . . . C1A C 0.5083(3) 0.2748(3) 0.6517(3) 0.0224(17) Uani 1 1 d . . . C2A C 0.4618(3) 0.3141(3) 0.6204(3) 0.0252(18) Uani 1 1 d . . . C3A C 0.4448(3) 0.3161(4) 0.5643(3) 0.0299(19) Uani 1 1 d . . . H3A H 0.4131 0.3420 0.5423 0.036 Uiso 1 1 calc R . . C4A C 0.4722(3) 0.2821(4) 0.5404(3) 0.037(2) Uani 1 1 d . . . H4A H 0.4598 0.2844 0.5026 0.044 Uiso 1 1 calc R . . C5A C 0.5180(3) 0.2444(4) 0.5718(3) 0.033(2) Uani 1 1 d . . . H5A H 0.5374 0.2203 0.5556 0.039 Uiso 1 1 calc R . . C6A C 0.5360(3) 0.2413(4) 0.6268(3) 0.0286(18) Uani 1 1 d . . . H6A H 0.5681 0.2155 0.6480 0.034 Uiso 1 1 calc R . . C21A C 0.4300(3) 0.3547(3) 0.6415(3) 0.0210(17) Uani 1 1 d . . . N22A N 0.4343(2) 0.3454(3) 0.6898(2) 0.0191(13) Uani 1 1 d . . . O2A O 0.4041(2) 0.3873(2) 0.70558(18) 0.0254(12) Uani 1 1 d . . . C23A C 0.3921(3) 0.4062(3) 0.6063(3) 0.0259(18) Uani 1 1 d . . . C24A C 0.4161(4) 0.4608(4) 0.5945(3) 0.042(2) Uani 1 1 d . . . H24A H 0.4563 0.4656 0.6098 0.050 Uiso 1 1 calc R . . C25A C 0.3817(5) 0.5072(4) 0.5610(4) 0.059(3) Uani 1 1 d . . . H25A H 0.3980 0.5445 0.5535 0.071 Uiso 1 1 calc R . . C26A C 0.3231(5) 0.5001(5) 0.5381(4) 0.068(3) Uani 1 1 d . . . H26A H 0.2992 0.5328 0.5151 0.082 Uiso 1 1 calc R . . C27A C 0.2996(4) 0.4467(5) 0.5482(4) 0.059(3) Uani 1 1 d . . . H27A H 0.2594 0.4414 0.5315 0.070 Uiso 1 1 calc R . . C28A C 0.3344(4) 0.3993(4) 0.5832(3) 0.040(2) Uani 1 1 d . . . H28A H 0.3178 0.3623 0.5907 0.048 Uiso 1 1 calc R . . O1B O 0.4350(2) 0.0662(2) 0.80260(19) 0.0305(13) Uani 1 1 d . . . C1B C 0.4480(3) 0.0700(4) 0.8543(3) 0.0303(19) Uani 1 1 d . . . O2B O 0.5314(2) 0.2190(2) 0.80703(17) 0.0245(12) Uani 1 1 d . . . C2B C 0.4854(3) 0.1181(4) 0.8888(3) 0.0289(19) Uani 1 1 d . . . C3B C 0.4958(3) 0.1172(4) 0.9433(3) 0.032(2) Uani 1 1 d . . . H3B H 0.5207 0.1488 0.9667 0.038 Uiso 1 1 calc R . . C4B C 0.4722(4) 0.0738(4) 0.9642(3) 0.038(2) Uani 1 1 d . . . H4B H 0.4796 0.0758 1.0011 0.046 Uiso 1 1 calc R . . C5B C 0.4371(4) 0.0263(4) 0.9306(3) 0.040(2) Uani 1 1 d . . . H5B H 0.4206 -0.0051 0.9446 0.049 Uiso 1 1 calc R . . C6B C 0.4263(4) 0.0247(4) 0.8773(3) 0.035(2) Uani 1 1 d . . . H6B H 0.4029 -0.0089 0.8553 0.042 Uiso 1 1 calc R . . C21B C 0.5139(3) 0.1669(3) 0.8697(3) 0.0254(18) Uani 1 1 d . . . N22B N 0.4992(2) 0.1764(3) 0.8191(2) 0.0229(14) Uani 1 1 d . . . C23B C 0.5629(3) 0.2051(3) 0.9104(3) 0.0258(18) Uani 1 1 d . . . C24B C 0.6185(3) 0.1899(4) 0.9218(3) 0.035(2) Uani 1 1 d . . . H24B H 0.6256 0.1538 0.9044 0.042 Uiso 1 1 calc R . . C25B C 0.6642(4) 0.2253(4) 0.9574(3) 0.042(2) Uani 1 1 d . . . H25B H 0.7021 0.2142 0.9644 0.051 Uiso 1 1 calc R . . C26B C 0.6536(4) 0.2765(4) 0.9826(3) 0.044(2) Uani 1 1 d . . . H26B H 0.6847 0.3014 1.0072 0.053 Uiso 1 1 calc R . . C27B C 0.5991(4) 0.2930(4) 0.9732(3) 0.043(2) Uani 1 1 d . . . H27B H 0.5928 0.3285 0.9916 0.052 Uiso 1 1 calc R . . C28B C 0.5534(4) 0.2577(4) 0.9368(3) 0.034(2) Uani 1 1 d . . . H28B H 0.5156 0.2693 0.9299 0.041 Uiso 1 1 calc R . . O1C O 0.2264(2) 0.2242(2) 0.67429(18) 0.0310(13) Uani 1 1 d . . . C1C C 0.2170(3) 0.2428(3) 0.6250(3) 0.0255(18) Uani 1 1 d . . . O2C O 0.3580(2) 0.1099(2) 0.69152(18) 0.0247(12) Uani 1 1 d . . . C2C C 0.2496(3) 0.2196(3) 0.5995(3) 0.0278(19) Uani 1 1 d . . . C3C C 0.2388(4) 0.2460(4) 0.5489(3) 0.039(2) Uani 1 1 d . . . H3C H 0.2608 0.2315 0.5312 0.046 Uiso 1 1 calc R . . C4C C 0.1978(4) 0.2917(4) 0.5243(3) 0.035(2) Uani 1 1 d . . . H4C H 0.1929 0.3105 0.4912 0.043 Uiso 1 1 calc R . . C5C C 0.1635(4) 0.3103(4) 0.5487(3) 0.042(2) Uani 1 1 d . . . H5C H 0.1329 0.3395 0.5309 0.050 Uiso 1 1 calc R . . C6C C 0.1735(3) 0.2868(4) 0.5980(3) 0.034(2) Uani 1 1 d . . . H6C H 0.1503 0.3008 0.6145 0.041 Uiso 1 1 calc R . . C21C C 0.2952(3) 0.1700(3) 0.6231(3) 0.0238(17) Uani 1 1 d . . . N22C N 0.3168(3) 0.1578(3) 0.6736(2) 0.0230(14) Uani 1 1 d . . . C23C C 0.3164(3) 0.1372(3) 0.5871(3) 0.0250(17) Uani 1 1 d . . . C24C C 0.3651(4) 0.1601(4) 0.5850(3) 0.036(2) Uani 1 1 d . . . H24C H 0.3847 0.1960 0.6064 0.043 Uiso 1 1 calc R . . C25C C 0.3850(4) 0.1311(4) 0.5520(3) 0.044(2) Uani 1 1 d . . . H25C H 0.4185 0.1471 0.5507 0.053 Uiso 1 1 calc R . . C26C C 0.3574(4) 0.0795(4) 0.5210(3) 0.046(2) Uani 1 1 d . . . H26C H 0.3721 0.0591 0.4990 0.055 Uiso 1 1 calc R . . C27C C 0.3085(4) 0.0571(4) 0.5218(3) 0.037(2) Uani 1 1 d . . . H27C H 0.2886 0.0219 0.4995 0.045 Uiso 1 1 calc R . . C28C C 0.2878(4) 0.0855(4) 0.5549(3) 0.034(2) Uani 1 1 d . . . H28C H 0.2540 0.0696 0.5557 0.041 Uiso 1 1 calc R . . O1D O 0.4103(2) 0.4169(2) 0.81399(19) 0.0316(13) Uani 1 1 d . . . C1D C 0.4321(3) 0.4073(3) 0.8665(3) 0.0262(18) Uani 1 1 d . . . O2D O 0.2974(2) 0.2724(2) 0.78284(18) 0.0271(12) Uani 1 1 d . . . C2D C 0.4116(3) 0.3594(3) 0.8903(3) 0.0246(17) Uani 1 1 d . . . C3D C 0.4370(3) 0.3559(4) 0.9470(3) 0.036(2) Uani 1 1 d . . . H3D H 0.4233 0.3249 0.9638 0.044 Uiso 1 1 calc R . . C4D C 0.4805(3) 0.3956(4) 0.9786(3) 0.035(2) Uani 1 1 d . . . H4D H 0.4967 0.3918 1.0167 0.042 Uiso 1 1 calc R . . C5D C 0.5008(4) 0.4408(4) 0.9556(3) 0.045(2) Uani 1 1 d . . . H5D H 0.5311 0.4685 0.9775 0.053 Uiso 1 1 calc R . . C6D C 0.4767(3) 0.4461(4) 0.8996(3) 0.0303(19) Uani 1 1 d . . . H6D H 0.4914 0.4772 0.8838 0.036 Uiso 1 1 calc R . . C21D C 0.3644(3) 0.3148(4) 0.8596(3) 0.0248(18) Uani 1 1 d . . . N22D N 0.3436(2) 0.3121(3) 0.8074(2) 0.0239(14) Uani 1 1 d . . . C23D C 0.3414(3) 0.2722(4) 0.8880(3) 0.0284(19) Uani 1 1 d . . . C24D C 0.3524(4) 0.2067(4) 0.8914(3) 0.037(2) Uani 1 1 d . . . H24D H 0.3743 0.1890 0.8747 0.044 Uiso 1 1 calc R . . C25D C 0.3318(4) 0.1674(4) 0.9188(3) 0.049(3) Uani 1 1 d . . . H25D H 0.3404 0.1227 0.9218 0.058 Uiso 1 1 calc R . . C26D C 0.2994(4) 0.1915(6) 0.9415(3) 0.058(3) Uani 1 1 d . . . H26D H 0.2859 0.1638 0.9607 0.070 Uiso 1 1 calc R . . C27D C 0.2858(4) 0.2566(6) 0.9370(3) 0.053(3) Uani 1 1 d . . . H27D H 0.2619 0.2730 0.9520 0.063 Uiso 1 1 calc R . . C28D C 0.3072(3) 0.2972(4) 0.9106(3) 0.034(2) Uani 1 1 d . . . H28D H 0.2986 0.3418 0.9079 0.041 Uiso 1 1 calc R . . N1E N 0.5470(3) 0.3582(3) 0.7908(2) 0.0261(15) Uani 1 1 d . . . C2E C 0.5624(4) 0.3700(4) 0.8426(3) 0.037(2) Uani 1 1 d . . . H2E H 0.5493 0.3416 0.8618 0.044 Uiso 1 1 calc R . . C3E C 0.5962(4) 0.4208(4) 0.8700(3) 0.044(2) Uani 1 1 d . . . H3E H 0.6072 0.4268 0.9073 0.052 Uiso 1 1 calc R . . C4E C 0.6133(4) 0.4619(4) 0.8421(4) 0.048(2) Uani 1 1 d . . . H4E H 0.6353 0.4987 0.8595 0.058 Uiso 1 1 calc R . . C5E C 0.5989(4) 0.4506(4) 0.7891(4) 0.047(2) Uani 1 1 d . . . H5E H 0.6117 0.4785 0.7694 0.056 Uiso 1 1 calc R . . C6E C 0.5659(4) 0.3989(4) 0.7649(3) 0.036(2) Uani 1 1 d . . . H6E H 0.5559 0.3912 0.7279 0.043 Uiso 1 1 calc R . . N1F N 0.4874(2) 0.0879(2) 0.7331(2) 0.0336(17) Uani 1 1 d G . . C2F C 0.4928(2) 0.1078(3) 0.68751(19) 0.048(2) Uani 1 1 d G . . H2F H 0.4638 0.1332 0.6610 0.057 Uiso 1 1 calc R . . C3F C 0.5407(3) 0.0905(3) 0.6807(3) 0.077(4) Uani 1 1 d G . . H3F H 0.5444 0.1041 0.6495 0.092 Uiso 1 1 calc R . . C4F C 0.5832(2) 0.0533(3) 0.7195(3) 0.073(3) Uani 1 1 d G . . H4F H 0.6159 0.0415 0.7148 0.087 Uiso 1 1 calc R . . C5F C 0.5778(2) 0.0334(3) 0.7651(3) 0.075(4) Uani 1 1 d G . . H5F H 0.6068 0.0080 0.7916 0.090 Uiso 1 1 calc R . . C6F C 0.5299(3) 0.0507(3) 0.77193(19) 0.068(3) Uani 1 1 d G . . H6F H 0.5262 0.0371 0.8031 0.081 Uiso 1 1 calc R . . N1G N 0.2668(3) 0.1373(3) 0.7613(2) 0.0292(15) Uani 1 1 d . . . C2G C 0.2925(4) 0.0827(4) 0.7802(4) 0.048(2) Uani 1 1 d . . . H2G H 0.3294 0.0756 0.7821 0.058 Uiso 1 1 calc R . . C3G C 0.2673(5) 0.0345(4) 0.7976(4) 0.060(3) Uani 1 1 d . . . H3G H 0.2876 -0.0043 0.8117 0.072 Uiso 1 1 calc R . . C4G C 0.2161(4) 0.0419(5) 0.7947(4) 0.054(3) Uani 1 1 d . . . H4G H 0.1984 0.0084 0.8053 0.065 Uiso 1 1 calc R . . C5G C 0.1891(4) 0.0994(5) 0.7759(4) 0.051(3) Uani 1 1 d . . . H5G H 0.1526 0.1072 0.7745 0.061 Uiso 1 1 calc R . . C6G C 0.2149(4) 0.1449(4) 0.7593(3) 0.045(2) Uani 1 1 d . . . H6G H 0.1953 0.1842 0.7456 0.054 Uiso 1 1 calc R . . N1H N 0.3018(3) 0.4142(3) 0.7193(2) 0.0274(15) Uani 1 1 d . . . C2H C 0.2907(4) 0.4595(4) 0.7469(3) 0.041(2) Uani 1 1 d . . . H2H H 0.3160 0.4648 0.7839 0.049 Uiso 1 1 calc R . . C3H C 0.2434(4) 0.5000(4) 0.7240(4) 0.052(3) Uani 1 1 d . . . H3H H 0.2361 0.5319 0.7449 0.063 Uiso 1 1 calc R . . C4H C 0.2084(4) 0.4923(4) 0.6711(4) 0.049(2) Uani 1 1 d . . . H4H H 0.1764 0.5198 0.6541 0.059 Uiso 1 1 calc R . . C5H C 0.2184(4) 0.4454(4) 0.6419(4) 0.051(3) Uani 1 1 d . . . H5H H 0.1935 0.4392 0.6049 0.062 Uiso 1 1 calc R . . C6H C 0.2660(3) 0.4070(4) 0.6678(3) 0.035(2) Uani 1 1 d . . . H6H H 0.2733 0.3740 0.6478 0.042 Uiso 1 1 calc R . . Fe5 Fe 0.03451(4) 0.78808(5) 0.76384(4) 0.0233(3) Uani 1 1 d . . . Fe6 Fe 0.14321(5) 0.83552(5) 0.73115(4) 0.0245(3) Uani 1 1 d . . . Fe7 Fe 0.15464(4) 0.67724(5) 0.69611(4) 0.0216(3) Uani 1 1 d . . . Fe8 Fe 0.06787(4) 0.62870(5) 0.75548(4) 0.0218(3) Uani 1 1 d . . . F56 F 0.06637(17) 0.80317(18) 0.71110(15) 0.0268(10) Uani 1 1 d . . . F67 F 0.17264(17) 0.74592(17) 0.75030(15) 0.0267(10) Uani 1 1 d . . . F78 F 0.07915(17) 0.66607(18) 0.69537(15) 0.0275(10) Uani 1 1 d . . . F85 F 0.08705(17) 0.71349(18) 0.79129(15) 0.0262(10) Uani 1 1 d . . . O1J O -0.0250(2) 0.8479(2) 0.73105(19) 0.0306(13) Uani 1 1 d . . . C1J C -0.0678(3) 0.8497(3) 0.6813(3) 0.0287(18) Uani 1 1 d . . . O2J O -0.0107(2) 0.6550(2) 0.72406(18) 0.0242(12) Uani 1 1 d . . . C2J C -0.0893(3) 0.7942(3) 0.6485(3) 0.0268(18) Uani 1 1 d . . . C3J C -0.1347(3) 0.8030(4) 0.5968(3) 0.036(2) Uani 1 1 d . . . H3J H -0.1481 0.7670 0.5734 0.043 Uiso 1 1 calc R . . C4J C -0.1602(4) 0.8616(4) 0.5790(3) 0.041(2) Uani 1 1 d . . . H4J H -0.1913 0.8658 0.5443 0.049 Uiso 1 1 calc R . . C5J C -0.1399(3) 0.9148(3) 0.6125(3) 0.032(2) Uani 1 1 d . . . H5J H -0.1573 0.9556 0.6008 0.039 Uiso 1 1 calc R . . C6J C -0.0947(3) 0.9088(4) 0.6626(3) 0.0320(19) Uani 1 1 d . . . H6J H -0.0814 0.9457 0.6850 0.038 Uiso 1 1 calc R . . C21J C -0.0663(3) 0.7298(3) 0.6648(3) 0.0223(17) Uani 1 1 d . . . N22J N -0.0230(3) 0.7193(3) 0.7107(2) 0.0245(14) Uani 1 1 d . . . C23J C -0.0935(3) 0.6735(3) 0.6288(3) 0.0268(18) Uani 1 1 d . . . C24J C -0.0645(3) 0.6446(4) 0.6017(3) 0.0324(19) Uani 1 1 d . . . H24J H -0.0291 0.6616 0.6055 0.039 Uiso 1 1 calc R . . C25J C -0.0879(4) 0.5911(4) 0.5696(3) 0.043(2) Uani 1 1 d . . . H25J H -0.0686 0.5714 0.5512 0.052 Uiso 1 1 calc R . . C26J C -0.1383(4) 0.5667(4) 0.5645(3) 0.049(3) Uani 1 1 d . . . H26J H -0.1543 0.5303 0.5421 0.059 Uiso 1 1 calc R . . C27J C -0.1663(4) 0.5938(4) 0.5912(3) 0.042(2) Uani 1 1 d . . . H27J H -0.2008 0.5752 0.5881 0.051 Uiso 1 1 calc R . . C28J C -0.1448(3) 0.6479(4) 0.6226(3) 0.034(2) Uani 1 1 d . . . H28J H -0.1652 0.6674 0.6400 0.041 Uiso 1 1 calc R . . O1K O 0.2170(2) 0.8728(2) 0.7641(2) 0.0327(13) Uani 1 1 d . . . C1K C 0.2580(3) 0.8626(3) 0.8130(3) 0.0278(18) Uani 1 1 d . . . O2K O 0.0945(2) 0.8436(2) 0.81314(19) 0.0278(12) Uani 1 1 d . . . C2K C 0.2479(3) 0.8489(3) 0.8576(3) 0.031(2) Uani 1 1 d . . . C3K C 0.2961(4) 0.8409(4) 0.9079(4) 0.046(2) Uani 1 1 d . . . H3K H 0.2901 0.8321 0.9388 0.055 Uiso 1 1 calc R . . C4K C 0.3502(4) 0.8455(5) 0.9139(4) 0.055(3) Uani 1 1 d . . . H4K H 0.3812 0.8389 0.9483 0.066 Uiso 1 1 calc R . . C5K C 0.3604(4) 0.8594(4) 0.8705(4) 0.047(2) Uani 1 1 d . . . H5K H 0.3984 0.8637 0.8749 0.056 Uiso 1 1 calc R . . C6K C 0.3154(3) 0.8673(4) 0.8204(3) 0.036(2) Uani 1 1 d . . . H6K H 0.3228 0.8761 0.7903 0.044 Uiso 1 1 calc R . . C21K C 0.1906(3) 0.8437(3) 0.8550(3) 0.0241(18) Uani 1 1 d . . . N22K N 0.1455(3) 0.8448(3) 0.8092(2) 0.0288(16) Uani 1 1 d . . . C23K C 0.1840(3) 0.8342(4) 0.9057(3) 0.0303(19) Uani 1 1 d . . . C24K C 0.1844(3) 0.7715(4) 0.9254(3) 0.036(2) Uani 1 1 d . . . H24K H 0.1899 0.7357 0.9068 0.043 Uiso 1 1 calc R . . C25K C 0.1770(3) 0.7613(4) 0.9714(3) 0.041(2) Uani 1 1 d . . . H25K H 0.1778 0.7190 0.9847 0.049 Uiso 1 1 calc R . . C26K C 0.1685(4) 0.8141(5) 0.9978(3) 0.053(3) Uani 1 1 d . . . H26K H 0.1630 0.8077 1.0293 0.063 Uiso 1 1 calc R . . C27K C 0.1678(5) 0.8754(5) 0.9789(4) 0.063(3) Uani 1 1 d . . . H27K H 0.1615 0.9114 0.9968 0.075 Uiso 1 1 calc R . . C28K C 0.1764(4) 0.8836(4) 0.9331(3) 0.047(2) Uani 1 1 d . . . H28K H 0.1769 0.9261 0.9206 0.056 Uiso 1 1 calc R . . O1L O 0.1316(2) 0.6262(2) 0.63201(18) 0.0257(12) Uani 1 1 d . . . C1L C 0.0871(3) 0.6330(3) 0.5846(3) 0.0225(17) Uani 1 1 d . . . O2L O 0.1399(2) 0.8163(2) 0.66046(19) 0.0294(12) Uani 1 1 d . . . C2L C 0.0584(3) 0.6915(3) 0.5658(3) 0.0228(17) Uani 1 1 d . . . C3L C 0.0112(4) 0.6923(4) 0.5152(3) 0.039(2) Uani 1 1 d . . . H3L H -0.0098 0.7311 0.5028 0.047 Uiso 1 1 calc R . . C4L C -0.0058(4) 0.6380(4) 0.4825(3) 0.044(2) Uani 1 1 d . . . H4L H -0.0377 0.6398 0.4482 0.053 Uiso 1 1 calc R . . C5L C 0.0240(4) 0.5820(4) 0.5005(3) 0.041(2) Uani 1 1 d . . . H5L H 0.0131 0.5449 0.4781 0.049 Uiso 1 1 calc R . . C6L C 0.0693(4) 0.5788(4) 0.5504(3) 0.037(2) Uani 1 1 d . . . H6L H 0.0893 0.5393 0.5622 0.045 Uiso 1 1 calc R . . C21L C 0.0777(3) 0.7533(3) 0.5947(3) 0.0273(18) Uani 1 1 d . . . N22L N 0.1215(3) 0.7548(3) 0.6413(2) 0.0263(15) Uani 1 1 d . . . C23L C 0.0469(3) 0.8130(4) 0.5692(3) 0.0294(19) Uani 1 1 d . . . C24L C 0.0021(4) 0.8318(4) 0.5802(4) 0.053(3) Uani 1 1 d . . . H24L H -0.0060 0.8078 0.6053 0.064 Uiso 1 1 calc R . . C25L C -0.0312(4) 0.8854(4) 0.5549(4) 0.060(3) Uani 1 1 d . . . H25L H -0.0619 0.8980 0.5626 0.072 Uiso 1 1 calc R . . C26L C -0.0186(4) 0.9197(4) 0.5185(4) 0.051(3) Uani 1 1 d . . . H26L H -0.0412 0.9558 0.5003 0.061 Uiso 1 1 calc R . . C27L C 0.0256(4) 0.9021(4) 0.5089(3) 0.048(2) Uani 1 1 d . . . H27L H 0.0340 0.9263 0.4840 0.057 Uiso 1 1 calc R . . C28L C 0.0592(4) 0.8496(3) 0.5343(3) 0.033(2) Uani 1 1 d . . . H28L H 0.0908 0.8388 0.5275 0.040 Uiso 1 1 calc R . . O1M O 0.0732(2) 0.5858(2) 0.81814(19) 0.0266(12) Uani 1 1 d . . . C1M C 0.1147(3) 0.5841(3) 0.8680(3) 0.0221(17) Uani 1 1 d . . . O2M O 0.1824(2) 0.6130(2) 0.75250(18) 0.0221(11) Uani 1 1 d . . . C2M C 0.1723(3) 0.5927(3) 0.8789(3) 0.0187(16) Uani 1 1 d . . . C3M C 0.2127(3) 0.5902(3) 0.9334(3) 0.0283(18) Uani 1 1 d . . . H3M H 0.2519 0.5963 0.9420 0.034 Uiso 1 1 calc R . . C4M C 0.1974(4) 0.5793(4) 0.9748(3) 0.036(2) Uani 1 1 d . . . H4M H 0.2257 0.5782 1.0111 0.044 Uiso 1 1 calc R . . C5M C 0.1421(3) 0.5702(4) 0.9631(3) 0.0320(19) Uani 1 1 d . . . H5M H 0.1313 0.5621 0.9913 0.038 Uiso 1 1 calc R . . C6M C 0.1011(3) 0.5728(4) 0.9106(3) 0.0317(19) Uani 1 1 d . . . H6M H 0.0623 0.5666 0.9031 0.038 Uiso 1 1 calc R . . C21M C 0.1928(3) 0.5996(3) 0.8378(3) 0.0209(17) Uani 1 1 d . . . N22M N 0.1576(2) 0.6109(2) 0.7878(2) 0.0196(14) Uani 1 1 d . . . C23M C 0.2548(3) 0.5945(4) 0.8549(3) 0.0274(18) Uani 1 1 d . . . C24M C 0.2867(4) 0.6478(5) 0.8596(3) 0.046(2) Uani 1 1 d . . . H24M H 0.2690 0.6889 0.8498 0.055 Uiso 1 1 calc R . . C25M C 0.3450(5) 0.6420(7) 0.8786(4) 0.076(4) Uani 1 1 d . . . H25M H 0.3674 0.6794 0.8824 0.091 Uiso 1 1 calc R . . C26M C 0.3709(5) 0.5838(9) 0.8922(4) 0.082(5) Uani 1 1 d . . . H26M H 0.4111 0.5807 0.9054 0.098 Uiso 1 1 calc R . . C27M C 0.3398(5) 0.5305(7) 0.8868(4) 0.067(3) Uani 1 1 d . . . H27M H 0.3580 0.4898 0.8959 0.080 Uiso 1 1 calc R . . C28M C 0.2816(4) 0.5348(4) 0.8682(3) 0.044(2) Uani 1 1 d . . . H28M H 0.2597 0.4969 0.8643 0.053 Uiso 1 1 calc R . . N1N N 0.0012(3) 0.7613(3) 0.8201(2) 0.0265(15) Uani 1 1 d . . . C2N C 0.0343(3) 0.7371(4) 0.8679(3) 0.033(2) Uani 1 1 d . . . H2N H 0.0740 0.7344 0.8778 0.039 Uiso 1 1 calc R . . C3N C 0.0156(4) 0.7158(4) 0.9041(3) 0.048(2) Uani 1 1 d . . . H3N H 0.0415 0.6993 0.9382 0.057 Uiso 1 1 calc R . . C4N C -0.0421(4) 0.7190(4) 0.8897(3) 0.042(2) Uani 1 1 d . . . H4N H -0.0570 0.7045 0.9136 0.051 Uiso 1 1 calc R . . C5N C -0.0775(4) 0.7436(4) 0.8399(3) 0.042(2) Uani 1 1 d . . . H5N H -0.1174 0.7464 0.8289 0.051 Uiso 1 1 calc R . . C6N C -0.0547(4) 0.7640(4) 0.8064(3) 0.036(2) Uani 1 1 d . . . H6N H -0.0795 0.7808 0.7721 0.043 Uiso 1 1 calc R . . N1P N 0.1052(3) 0.9277(3) 0.7013(3) 0.0326(17) Uani 1 1 d . . . C2P C 0.0670(4) 0.9544(4) 0.7134(4) 0.044(2) Uani 1 1 d . . . H2P H 0.0554 0.9323 0.7370 0.053 Uiso 1 1 calc R . . C3P C 0.0431(4) 1.0132(4) 0.6935(4) 0.058(3) Uani 1 1 d . . . H3P H 0.0161 1.0318 0.7038 0.070 Uiso 1 1 calc R . . C4P C 0.0585(4) 1.0442(4) 0.6589(4) 0.058(3) Uani 1 1 d . . . H4P H 0.0425 1.0850 0.6449 0.069 Uiso 1 1 calc R . . C5P C 0.0967(5) 1.0173(4) 0.6443(4) 0.063(3) Uani 1 1 d . . . H5P H 0.1084 1.0388 0.6204 0.076 Uiso 1 1 calc R . . C6P C 0.1182(4) 0.9578(4) 0.6652(4) 0.051(3) Uani 1 1 d . . . H6P H 0.1434 0.9371 0.6535 0.061 Uiso 1 1 calc R . . N1Q N 0.2387(3) 0.6865(3) 0.6998(2) 0.0286(15) Uani 1 1 d . . . C2Q C 0.2790(3) 0.7241(4) 0.7359(3) 0.0317(19) Uani 1 1 d . . . H2Q H 0.2700 0.7478 0.7606 0.038 Uiso 1 1 calc R . . C3Q C 0.3327(4) 0.7303(4) 0.7391(3) 0.039(2) Uani 1 1 d . . . H3Q H 0.3598 0.7579 0.7653 0.047 Uiso 1 1 calc R . . C4Q C 0.3468(4) 0.6974(5) 0.7051(4) 0.052(3) Uani 1 1 d . . . H4Q H 0.3838 0.7016 0.7069 0.063 Uiso 1 1 calc R . . C5Q C 0.3067(5) 0.6570(6) 0.6670(4) 0.072(3) Uani 1 1 d . . . H5Q H 0.3156 0.6329 0.6425 0.087 Uiso 1 1 calc R . . C6Q C 0.2532(4) 0.6533(4) 0.6664(4) 0.050(3) Uani 1 1 d . . . H6Q H 0.2255 0.6257 0.6407 0.060 Uiso 1 1 calc R . . N1R N 0.0443(3) 0.5397(3) 0.7094(2) 0.0261(15) Uani 1 1 d . . . C2R C 0.0815(4) 0.5041(4) 0.7008(4) 0.046(2) Uani 1 1 d . . . H2R H 0.1198 0.5187 0.7144 0.056 Uiso 1 1 calc R . . C3R C 0.0670(5) 0.4461(4) 0.6725(4) 0.067(3) Uani 1 1 d . . . H3R H 0.0950 0.4217 0.6672 0.080 Uiso 1 1 calc R . . C4R C 0.0133(5) 0.4252(4) 0.6529(3) 0.048(3) Uani 1 1 d . . . H4R H 0.0025 0.3862 0.6329 0.057 Uiso 1 1 calc R . . C5R C -0.0261(4) 0.4603(4) 0.6617(4) 0.051(3) Uani 1 1 d . . . H5R H -0.0641 0.4452 0.6491 0.062 Uiso 1 1 calc R . . C6R C -0.0100(3) 0.5181(4) 0.6892(3) 0.036(2) Uani 1 1 d . . . H6R H -0.0379 0.5432 0.6939 0.043 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 Fe1 0.0235(6) 0.0233(6) 0.0174(5) 0.0022(4) 0.0099(5) 0.0027(5) Fe2 0.0257(6) 0.0232(6) 0.0195(5) 0.0019(4) 0.0083(5) 0.0016(5) Fe3 0.0252(6) 0.0271(6) 0.0173(5) -0.0004(4) 0.0092(5) 0.0023(5) Fe4 0.0296(7) 0.0227(6) 0.0188(5) 0.0005(4) 0.0118(5) 0.0044(5) F12 0.032(3) 0.024(2) 0.020(2) 0.0003(17) 0.0083(19) 0.0018(19) F23 0.024(2) 0.036(2) 0.023(2) 0.0031(18) 0.0080(19) 0.0040(19) F34 0.036(3) 0.026(2) 0.026(2) -0.0012(18) 0.012(2) -0.001(2) F41 0.030(3) 0.032(2) 0.024(2) 0.0035(18) 0.014(2) 0.0052(19) O1A 0.022(3) 0.036(3) 0.015(2) -0.001(2) 0.007(2) 0.002(2) C1A 0.019(4) 0.029(4) 0.022(4) 0.003(3) 0.012(3) -0.003(3) C2A 0.031(5) 0.026(4) 0.026(4) -0.005(3) 0.019(4) -0.006(4) C3A 0.028(5) 0.041(5) 0.021(4) -0.001(3) 0.011(4) 0.004(4) C4A 0.037(5) 0.053(5) 0.022(4) 0.001(4) 0.015(4) 0.010(4) C5A 0.033(5) 0.045(5) 0.031(4) -0.011(4) 0.024(4) -0.005(4) C6A 0.024(5) 0.040(5) 0.024(4) 0.004(3) 0.013(4) 0.003(4) C21A 0.021(4) 0.023(4) 0.015(4) 0.003(3) 0.005(3) -0.001(3) N22A 0.022(3) 0.019(3) 0.017(3) -0.002(2) 0.009(3) 0.000(3) O2A 0.032(3) 0.021(3) 0.027(3) 0.005(2) 0.016(2) 0.008(2) C23A 0.029(5) 0.030(4) 0.020(4) -0.002(3) 0.011(4) 0.010(4) C24A 0.044(6) 0.027(5) 0.053(5) 0.014(4) 0.020(5) 0.004(4) C25A 0.085(9) 0.023(5) 0.072(7) 0.022(5) 0.037(7) 0.012(5) C26A 0.082(9) 0.061(7) 0.055(7) 0.032(6) 0.023(6) 0.043(7) C27A 0.035(6) 0.076(8) 0.054(6) 0.012(6) 0.009(5) 0.011(5) C28A 0.045(6) 0.037(5) 0.035(5) 0.007(4) 0.015(4) 0.001(4) O1B 0.039(3) 0.026(3) 0.024(3) 0.001(2) 0.011(3) -0.006(2) C1B 0.025(5) 0.028(4) 0.031(4) 0.007(4) 0.006(4) -0.001(4) O2B 0.022(3) 0.030(3) 0.021(3) 0.007(2) 0.008(2) 0.001(2) C2B 0.027(5) 0.032(4) 0.027(4) 0.010(3) 0.010(4) 0.010(4) C3B 0.032(5) 0.040(5) 0.017(4) 0.006(3) 0.006(4) 0.002(4) C4B 0.041(5) 0.049(5) 0.019(4) 0.010(4) 0.008(4) -0.001(4) C5B 0.048(6) 0.037(5) 0.045(5) 0.018(4) 0.029(5) 0.004(4) C6B 0.042(5) 0.027(4) 0.035(5) 0.011(4) 0.015(4) 0.000(4) C21B 0.025(4) 0.026(4) 0.023(4) 0.006(3) 0.008(4) 0.009(3) N22B 0.015(3) 0.027(3) 0.030(4) 0.004(3) 0.013(3) 0.002(3) C23B 0.035(5) 0.022(4) 0.018(4) 0.004(3) 0.010(4) 0.003(4) C24B 0.034(5) 0.039(5) 0.028(4) -0.004(4) 0.011(4) 0.002(4) C25B 0.025(5) 0.056(6) 0.041(5) -0.004(5) 0.010(4) -0.002(4) C26B 0.041(6) 0.044(6) 0.028(5) 0.002(4) -0.004(4) -0.009(5) C27B 0.071(7) 0.031(5) 0.025(4) -0.001(4) 0.017(5) 0.000(5) C28B 0.033(5) 0.043(5) 0.024(4) 0.010(4) 0.011(4) 0.005(4) O1C 0.025(3) 0.046(3) 0.022(3) 0.003(2) 0.010(2) 0.005(3) C1C 0.027(5) 0.029(4) 0.022(4) 0.002(3) 0.012(4) -0.001(4) O2C 0.028(3) 0.021(3) 0.026(3) -0.004(2) 0.012(2) 0.003(2) C2C 0.040(5) 0.022(4) 0.014(4) 0.002(3) 0.004(4) -0.006(4) C3C 0.053(6) 0.040(5) 0.027(4) -0.001(4) 0.021(4) 0.008(4) C4C 0.050(6) 0.028(4) 0.024(4) 0.011(4) 0.011(4) 0.002(4) C5C 0.044(6) 0.040(5) 0.035(5) 0.005(4) 0.010(4) 0.011(4) C6C 0.037(5) 0.037(5) 0.032(4) 0.001(4) 0.018(4) 0.004(4) C21C 0.024(4) 0.028(4) 0.016(4) 0.002(3) 0.006(3) -0.001(3) N22C 0.030(4) 0.017(3) 0.020(3) 0.001(2) 0.009(3) 0.004(3) C23C 0.025(5) 0.030(4) 0.019(4) 0.003(3) 0.008(3) 0.001(4) C24C 0.036(5) 0.049(5) 0.020(4) -0.006(4) 0.010(4) -0.002(4) C25C 0.037(5) 0.067(6) 0.031(5) -0.006(5) 0.017(4) -0.009(5) C26C 0.059(7) 0.052(6) 0.036(5) 0.004(4) 0.029(5) 0.018(5) C27C 0.056(6) 0.028(5) 0.035(5) -0.010(4) 0.025(5) -0.011(4) C28C 0.039(5) 0.031(5) 0.033(4) 0.003(4) 0.016(4) -0.003(4) O1D 0.039(3) 0.029(3) 0.026(3) -0.005(2) 0.014(3) 0.001(2) C1D 0.028(5) 0.028(4) 0.020(4) -0.008(3) 0.008(4) 0.009(4) O2D 0.025(3) 0.036(3) 0.018(2) -0.008(2) 0.008(2) -0.004(2) C2D 0.028(5) 0.033(4) 0.019(4) -0.006(3) 0.015(3) 0.003(4) C3D 0.038(5) 0.040(5) 0.028(4) 0.005(4) 0.012(4) 0.005(4) C4D 0.033(5) 0.047(5) 0.019(4) -0.011(4) 0.006(4) -0.010(4) C5D 0.050(6) 0.037(5) 0.038(5) -0.011(4) 0.011(5) 0.002(4) C6D 0.033(5) 0.029(4) 0.033(4) -0.002(4) 0.019(4) -0.001(4) C21D 0.021(4) 0.035(4) 0.019(4) -0.008(3) 0.010(3) 0.007(3) N22D 0.019(3) 0.031(4) 0.024(3) 0.002(3) 0.011(3) -0.001(3) C23D 0.025(5) 0.038(5) 0.016(4) -0.005(3) 0.003(3) -0.002(4) C24D 0.039(5) 0.047(5) 0.021(4) -0.001(4) 0.010(4) 0.003(4) C25D 0.053(7) 0.043(5) 0.043(5) 0.014(4) 0.015(5) -0.006(5) C26D 0.047(7) 0.095(9) 0.032(5) 0.010(5) 0.016(5) -0.027(6) C27D 0.040(6) 0.105(9) 0.020(4) 0.007(5) 0.020(4) 0.002(6) C28D 0.031(5) 0.051(5) 0.021(4) -0.006(4) 0.012(4) 0.004(4) N1E 0.029(4) 0.025(3) 0.020(3) 0.004(3) 0.006(3) -0.002(3) C2E 0.050(6) 0.033(5) 0.042(5) 0.000(4) 0.033(4) -0.014(4) C3E 0.056(6) 0.040(5) 0.034(5) -0.008(4) 0.019(5) -0.026(5) C4E 0.048(6) 0.044(6) 0.050(6) -0.017(5) 0.019(5) -0.015(5) C5E 0.047(6) 0.038(5) 0.054(6) 0.012(4) 0.021(5) -0.014(4) C6E 0.047(6) 0.033(5) 0.024(4) 0.007(4) 0.012(4) 0.001(4) N1F 0.037(4) 0.031(4) 0.033(4) 0.009(3) 0.015(3) 0.021(3) C2F 0.055(6) 0.056(6) 0.045(5) 0.010(5) 0.033(5) 0.022(5) C3F 0.117(11) 0.039(6) 0.093(9) 0.011(6) 0.062(8) 0.024(7) C4F 0.091(9) 0.042(6) 0.105(9) -0.006(6) 0.061(8) -0.003(6) C5F 0.063(8) 0.035(6) 0.146(11) 0.003(6) 0.063(8) 0.020(5) C6F 0.066(8) 0.072(7) 0.079(8) -0.036(6) 0.046(7) -0.028(6) N1G 0.027(4) 0.033(4) 0.026(3) -0.004(3) 0.009(3) -0.007(3) C2G 0.042(6) 0.033(5) 0.078(7) 0.005(5) 0.034(5) -0.002(4) C3G 0.072(8) 0.023(5) 0.103(8) 0.013(5) 0.054(7) 0.007(5) C4G 0.061(7) 0.046(6) 0.066(7) 0.001(5) 0.038(6) -0.012(5) C5G 0.047(6) 0.063(7) 0.057(6) -0.008(5) 0.037(5) -0.015(5) C6G 0.048(6) 0.043(5) 0.044(5) 0.004(4) 0.020(5) -0.004(5) N1H 0.030(4) 0.025(3) 0.033(4) 0.001(3) 0.020(3) 0.009(3) C2H 0.034(5) 0.052(6) 0.036(5) -0.011(4) 0.014(4) 0.016(4) C3H 0.049(6) 0.051(6) 0.047(6) -0.011(5) 0.012(5) 0.022(5) C4H 0.039(6) 0.046(6) 0.065(6) 0.009(5) 0.025(5) 0.024(5) C5H 0.052(6) 0.051(6) 0.046(5) 0.007(5) 0.018(5) 0.023(5) C6H 0.036(5) 0.037(5) 0.028(4) -0.003(4) 0.010(4) 0.014(4) Fe5 0.0231(6) 0.0229(6) 0.0228(5) -0.0010(4) 0.0091(5) 0.0020(5) Fe6 0.0273(6) 0.0185(6) 0.0278(6) -0.0007(4) 0.0122(5) -0.0008(5) Fe7 0.0246(6) 0.0179(5) 0.0236(5) 0.0014(4) 0.0117(5) 0.0001(5) Fe8 0.0200(6) 0.0190(6) 0.0259(6) 0.0035(4) 0.0097(5) 0.0007(4) F56 0.025(2) 0.025(2) 0.029(2) -0.0022(18) 0.011(2) -0.0039(18) F67 0.027(2) 0.019(2) 0.032(2) -0.0015(18) 0.011(2) -0.0007(18) F78 0.027(2) 0.028(2) 0.026(2) 0.0007(18) 0.011(2) -0.0003(19) F85 0.027(2) 0.027(2) 0.025(2) 0.0047(18) 0.0114(19) 0.0058(19) O1J 0.033(3) 0.026(3) 0.027(3) -0.002(2) 0.008(3) 0.006(2) C1J 0.027(5) 0.027(4) 0.033(4) 0.003(3) 0.015(4) -0.001(4) O2J 0.024(3) 0.017(3) 0.032(3) 0.003(2) 0.012(2) 0.002(2) C2J 0.027(5) 0.024(4) 0.030(4) -0.008(3) 0.013(4) -0.004(3) C3J 0.040(5) 0.028(5) 0.031(4) 0.001(4) 0.008(4) 0.001(4) C4J 0.040(5) 0.031(5) 0.034(5) 0.013(4) -0.001(4) -0.004(4) C5J 0.028(5) 0.018(4) 0.046(5) 0.007(4) 0.011(4) 0.001(3) C6J 0.031(5) 0.028(4) 0.039(5) 0.004(4) 0.016(4) -0.003(4) C21J 0.017(4) 0.025(4) 0.020(4) 0.002(3) 0.004(3) -0.003(3) N22J 0.024(4) 0.024(3) 0.029(3) 0.003(3) 0.015(3) 0.000(3) C23J 0.028(5) 0.020(4) 0.023(4) 0.009(3) 0.004(4) 0.005(3) C24J 0.028(5) 0.031(5) 0.036(4) 0.005(4) 0.012(4) 0.006(4) C25J 0.064(7) 0.026(5) 0.032(5) -0.005(4) 0.013(5) -0.002(5) C26J 0.064(7) 0.023(5) 0.036(5) -0.001(4) -0.002(5) -0.007(5) C27J 0.030(5) 0.038(5) 0.038(5) 0.009(4) -0.004(4) -0.013(4) C28J 0.035(5) 0.031(5) 0.034(4) 0.004(4) 0.013(4) -0.002(4) O1K 0.037(3) 0.021(3) 0.044(3) -0.006(2) 0.021(3) -0.008(2) C1K 0.021(4) 0.019(4) 0.039(5) -0.001(3) 0.010(4) 0.004(3) O2K 0.024(3) 0.024(3) 0.032(3) 0.002(2) 0.009(2) 0.005(2) C2K 0.028(5) 0.019(4) 0.040(5) -0.006(3) 0.009(4) 0.001(3) C3K 0.042(6) 0.045(5) 0.046(5) 0.001(4) 0.015(5) -0.006(4) C4K 0.033(6) 0.066(7) 0.047(6) 0.020(5) 0.000(5) -0.003(5) C5K 0.027(5) 0.037(5) 0.072(7) 0.005(5) 0.017(5) -0.001(4) C6K 0.029(5) 0.027(4) 0.054(5) -0.003(4) 0.018(4) -0.006(4) C21K 0.024(4) 0.011(4) 0.030(4) -0.008(3) 0.004(4) 0.003(3) N22K 0.029(4) 0.019(3) 0.036(4) -0.007(3) 0.011(3) 0.003(3) C23K 0.019(4) 0.033(5) 0.028(4) -0.008(4) 0.000(4) -0.004(3) C24K 0.032(5) 0.033(5) 0.040(5) 0.002(4) 0.013(4) -0.004(4) C25K 0.033(5) 0.052(6) 0.031(5) 0.002(4) 0.008(4) -0.011(4) C26K 0.052(6) 0.083(8) 0.031(5) 0.004(5) 0.025(5) 0.002(6) C27K 0.103(9) 0.048(6) 0.040(5) -0.006(5) 0.034(6) 0.023(6) C28K 0.065(7) 0.040(5) 0.034(5) 0.002(4) 0.021(5) 0.011(5) O1L 0.031(3) 0.019(3) 0.026(3) 0.001(2) 0.012(3) 0.000(2) C1L 0.027(4) 0.025(4) 0.021(4) 0.002(3) 0.015(4) -0.003(3) O2L 0.037(3) 0.020(3) 0.035(3) -0.002(2) 0.019(3) -0.006(2) C2L 0.020(4) 0.026(4) 0.024(4) 0.003(3) 0.011(3) -0.001(3) C3L 0.044(6) 0.034(5) 0.036(5) 0.000(4) 0.014(4) -0.002(4) C4L 0.048(6) 0.043(5) 0.032(5) 0.000(4) 0.009(4) -0.010(5) C5L 0.057(6) 0.030(5) 0.030(5) -0.007(4) 0.013(4) -0.008(4) C6L 0.049(6) 0.025(4) 0.032(5) 0.000(4) 0.012(4) -0.004(4) C21L 0.034(5) 0.028(4) 0.026(4) 0.006(3) 0.019(4) 0.002(4) N22L 0.034(4) 0.023(3) 0.026(3) 0.003(3) 0.018(3) -0.002(3) C23L 0.037(5) 0.031(4) 0.022(4) 0.000(3) 0.014(4) -0.002(4) C24L 0.061(7) 0.052(6) 0.063(6) 0.031(5) 0.043(6) 0.023(5) C25L 0.065(7) 0.051(6) 0.089(8) 0.035(6) 0.055(6) 0.022(5) C26L 0.067(7) 0.032(5) 0.063(6) 0.014(5) 0.038(6) 0.020(5) C27L 0.068(7) 0.034(5) 0.051(6) 0.020(4) 0.034(5) 0.011(5) C28L 0.048(6) 0.020(4) 0.042(5) 0.004(4) 0.030(4) 0.004(4) O1M 0.019(3) 0.027(3) 0.032(3) 0.009(2) 0.010(2) 0.001(2) C1M 0.027(5) 0.014(4) 0.031(4) 0.000(3) 0.018(4) 0.002(3) O2M 0.030(3) 0.022(3) 0.024(3) 0.002(2) 0.020(2) 0.000(2) C2M 0.022(4) 0.014(4) 0.022(4) -0.003(3) 0.010(3) 0.006(3) C3M 0.029(5) 0.027(4) 0.033(4) -0.001(3) 0.017(4) 0.001(4) C4M 0.036(5) 0.040(5) 0.027(4) -0.004(4) 0.008(4) 0.004(4) C5M 0.030(5) 0.046(5) 0.030(4) 0.001(4) 0.022(4) 0.004(4) C6M 0.029(5) 0.042(5) 0.030(4) 0.003(4) 0.018(4) -0.001(4) C21M 0.022(4) 0.015(4) 0.023(4) 0.003(3) 0.007(3) 0.000(3) N22M 0.024(4) 0.011(3) 0.029(3) 0.004(2) 0.016(3) 0.003(3) C23M 0.025(5) 0.045(5) 0.013(4) -0.001(3) 0.010(3) -0.001(4) C24M 0.035(6) 0.074(7) 0.031(5) 0.006(4) 0.016(4) -0.017(5) C25M 0.045(8) 0.141(12) 0.033(6) -0.002(7) 0.009(5) -0.044(8) C26M 0.023(7) 0.191(16) 0.031(6) -0.008(8) 0.013(5) 0.006(9) C27M 0.033(7) 0.117(10) 0.042(6) -0.008(6) 0.009(5) 0.043(7) C28M 0.043(6) 0.056(6) 0.032(5) -0.001(4) 0.014(4) 0.014(5) N1N 0.025(4) 0.032(4) 0.023(3) -0.001(3) 0.011(3) 0.004(3) C2N 0.028(5) 0.049(5) 0.025(4) -0.001(4) 0.015(4) 0.003(4) C3N 0.052(7) 0.059(6) 0.030(5) 0.000(4) 0.016(5) -0.003(5) C4N 0.049(6) 0.052(6) 0.039(5) -0.003(4) 0.031(5) -0.010(5) C5N 0.033(5) 0.060(6) 0.042(5) -0.023(5) 0.023(5) -0.015(4) C6N 0.032(5) 0.037(5) 0.035(5) -0.001(4) 0.012(4) 0.006(4) N1P 0.038(4) 0.013(3) 0.044(4) 0.007(3) 0.014(4) -0.002(3) C2P 0.049(6) 0.017(4) 0.079(7) 0.015(4) 0.041(5) 0.011(4) C3P 0.033(6) 0.050(6) 0.105(8) 0.028(6) 0.043(6) 0.020(5) C4P 0.063(7) 0.032(5) 0.071(7) 0.016(5) 0.023(6) 0.012(5) C5P 0.102(10) 0.039(6) 0.059(6) 0.007(5) 0.045(7) 0.004(6) C6P 0.072(7) 0.024(5) 0.072(7) 0.008(5) 0.046(6) -0.001(5) N1Q 0.027(4) 0.036(4) 0.032(4) -0.004(3) 0.022(3) -0.002(3) C2Q 0.019(5) 0.051(5) 0.025(4) -0.002(4) 0.009(4) -0.004(4) C3Q 0.027(5) 0.042(5) 0.044(5) 0.000(4) 0.012(4) 0.002(4) C4Q 0.035(6) 0.061(6) 0.071(7) 0.004(5) 0.032(5) -0.015(5) C5Q 0.064(8) 0.098(9) 0.082(8) -0.033(7) 0.057(7) -0.021(7) C6Q 0.038(6) 0.064(6) 0.065(6) -0.019(5) 0.038(5) -0.020(5) N1R 0.029(4) 0.019(3) 0.032(3) 0.002(3) 0.015(3) -0.005(3) C2R 0.046(6) 0.037(5) 0.063(6) -0.019(5) 0.030(5) -0.008(4) C3R 0.075(8) 0.037(6) 0.097(8) -0.025(6) 0.046(7) -0.006(6) C4R 0.068(7) 0.027(5) 0.035(5) -0.002(4) 0.011(5) -0.001(5) C5R 0.050(6) 0.034(5) 0.056(6) 0.008(5) 0.011(5) -0.011(5) C6R 0.024(5) 0.023(4) 0.044(5) 0.009(4) 0.000(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1A 1.898(5) . ? Fe1 O2B 1.930(4) . ? Fe1 F41 1.971(4) . ? Fe1 F12 1.977(4) . ? Fe1 N22A 2.156(5) . ? Fe1 N1E 2.165(6) . ? Fe2 O1B 1.899(5) . ? Fe2 O2C 1.939(5) . ? Fe2 F12 1.973(4) . ? Fe2 F23 1.981(4) . ? Fe2 N1F 2.126(4) . ? Fe2 N22B 2.136(6) . ? Fe3 O1C 1.909(5) . ? Fe3 O2D 1.937(5) . ? Fe3 F23 1.972(4) . ? Fe3 F34 1.991(4) . ? Fe3 N22C 2.121(6) . ? Fe3 N1G 2.150(6) . ? Fe4 O1D 1.906(5) . ? Fe4 O2A 1.943(5) . ? Fe4 F41 1.957(4) . ? Fe4 F34 1.969(4) . ? Fe4 N1H 2.139(6) . ? Fe4 N22D 2.152(6) . ? O1A C1A 1.321(8) . ? C1A C6A 1.383(10) . ? C1A C2A 1.402(10) . ? C2A C3A 1.413(9) . ? C2A C21A 1.471(10) . ? C3A C4A 1.362(10) . ? C3A H3A 0.9500 . ? C4A C5A 1.373(11) . ? C4A H4A 0.9500 . ? C5A C6A 1.379(10) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C21A N22A 1.302(8) . ? C21A C23A 1.490(9) . ? N22A O2A 1.368(7) . ? C23A C28A 1.361(11) . ? C23A C24A 1.402(11) . ? C24A C25A 1.364(11) . ? C24A H24A 0.9500 . ? C25A C26A 1.382(14) . ? C25A H25A 0.9500 . ? C26A C27A 1.355(14) . ? C26A H26A 0.9500 . ? C27A C28A 1.398(12) . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? O1B C1B 1.317(9) . ? C1B C6B 1.387(10) . ? C1B C2B 1.430(10) . ? O2B N22B 1.358(7) . ? C2B C3B 1.406(10) . ? C2B C21B 1.482(11) . ? C3B C4B 1.356(11) . ? C3B H3B 0.9500 . ? C4B C5B 1.388(11) . ? C4B H4B 0.9500 . ? C5B C6B 1.371(11) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C21B N22B 1.292(9) . ? C21B C23B 1.506(10) . ? C23B C24B 1.382(11) . ? C23B C28B 1.393(10) . ? C24B C25B 1.379(11) . ? C24B H24B 0.9500 . ? C25B C26B 1.364(12) . ? C25B H25B 0.9500 . ? C26B C27B 1.372(12) . ? C26B H26B 0.9500 . ? C27B C28B 1.386(11) . ? C27B H27B 0.9500 . ? C28B H28B 0.9500 . ? O1C C1C 1.328(8) . ? C1C C6C 1.391(10) . ? C1C C2C 1.407(11) . ? O2C N22C 1.388(7) . ? C2C C3C 1.411(10) . ? C2C C21C 1.489(10) . ? C3C C4C 1.368(11) . ? C3C H3C 0.9500 . ? C4C C5C 1.392(12) . ? C4C H4C 0.9500 . ? C5C C6C 1.358(11) . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C21C N22C 1.280(8) . ? C21C C23C 1.499(10) . ? C23C C24C 1.380(11) . ? C23C C28C 1.385(10) . ? C24C C25C 1.369(11) . ? C24C H24C 0.9500 . ? C25C C26C 1.365(12) . ? C25C H25C 0.9500 . ? C26C C27C 1.366(12) . ? C26C H26C 0.9500 . ? C27C C28C 1.381(11) . ? C27C H27C 0.9500 . ? C28C H28C 0.9500 . ? O1D C1D 1.320(8) . ? C1D C6D 1.381(10) . ? C1D C2D 1.419(10) . ? O2D N22D 1.369(7) . ? C2D C3D 1.410(10) . ? C2D C21D 1.476(10) . ? C3D C4D 1.365(10) . ? C3D H3D 0.9500 . ? C4D C5D 1.364(12) . ? C4D H4D 0.9500 . ? C5D C6D 1.393(10) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? C21D N22D 1.300(8) . ? C21D C23D 1.473(11) . ? C23D C24D 1.385(11) . ? C23D C28D 1.394(11) . ? C24D C25D 1.373(12) . ? C24D H24D 0.9500 . ? C25D C26D 1.349(13) . ? C25D H25D 0.9500 . ? C26D C27D 1.389(14) . ? C26D H26D 0.9500 . ? C27D C28D 1.382(12) . ? C27D H27D 0.9500 . ? C28D H28D 0.9500 . ? N1E C2E 1.328(9) . ? N1E C6E 1.334(10) . ? C2E C3E 1.370(10) . ? C2E H2E 0.9500 . ? C3E C4E 1.349(12) . ? C3E H3E 0.9500 . ? C4E C5E 1.362(12) . ? C4E H4E 0.9500 . ? C5E C6E 1.356(11) . ? C5E H5E 0.9500 . ? C6E H6E 0.9500 . ? N1F C2F 1.3900 . ? N1F C6F 1.3900 . ? C2F C3F 1.3900 . ? C2F H2F 0.9500 . ? C3F C4F 1.3900 . ? C3F H3F 0.9500 . ? C4F C5F 1.3900 . ? C4F H4F 0.9500 . ? C5F C6F 1.3900 . ? C5F H5F 0.9500 . ? C6F H6F 0.9500 . ? N1G C2G 1.305(10) . ? N1G C6G 1.339(11) . ? C2G C3G 1.392(12) . ? C2G H2G 0.9500 . ? C3G C4G 1.313(13) . ? C3G H3G 0.9500 . ? C4G C5G 1.369(13) . ? C4G H4G 0.9500 . ? C5G C6G 1.352(12) . ? C5G H5G 0.9500 . ? C6G H6G 0.9500 . ? N1H C2H 1.321(9) . ? N1H C6H 1.323(9) . ? C2H C3H 1.394(11) . ? C2H H2H 0.9500 . ? C3H C4H 1.352(12) . ? C3H H3H 0.9500 . ? C4H C5H 1.360(12) . ? C4H H4H 0.9500 . ? C5H C6H 1.383(11) . ? C5H H5H 0.9500 . ? C6H H6H 0.9500 . ? Fe5 O1J 1.882(5) . ? Fe5 O2K 1.940(5) . ? Fe5 F85 1.986(4) . ? Fe5 F56 1.992(4) . ? Fe5 N22J 2.124(6) . ? Fe5 N1N 2.157(6) . ? Fe6 O1K 1.898(5) . ? Fe6 F56 1.950(4) . ? Fe6 O2L 1.956(5) . ? Fe6 F67 1.995(4) . ? Fe6 N22K 2.138(6) . ? Fe6 N1P 2.149(6) . ? Fe7 O1L 1.919(5) . ? Fe7 O2M 1.933(4) . ? Fe7 F67 1.969(4) . ? Fe7 F78 1.974(4) . ? Fe7 N22L 2.118(6) . ? Fe7 N1Q 2.158(6) . ? Fe8 O1M 1.896(5) . ? Fe8 O2J 1.922(5) . ? Fe8 F78 1.967(4) . ? Fe8 F85 1.974(4) . ? Fe8 N22M 2.141(6) . ? Fe8 N1R 2.174(6) . ? O1J C1J 1.337(8) . ? C1J C6J 1.396(10) . ? C1J C2J 1.421(10) . ? O2J N22J 1.385(7) . ? C2J C3J 1.411(10) . ? C2J C21J 1.456(10) . ? C3J C4J 1.371(10) . ? C3J H3J 0.9500 . ? C4J C5J 1.387(10) . ? C4J H4J 0.9500 . ? C5J C6J 1.374(10) . ? C5J H5J 0.9500 . ? C6J H6J 0.9500 . ? C21J N22J 1.294(8) . ? C21J C23J 1.498(10) . ? C23J C28J 1.380(11) . ? C23J C24J 1.409(11) . ? C24J C25J 1.386(10) . ? C24J H24J 0.9500 . ? C25J C26J 1.357(13) . ? C25J H25J 0.9500 . ? C26J C27J 1.365(13) . ? C26J H26J 0.9500 . ? C27J C28J 1.380(11) . ? C27J H27J 0.9500 . ? C28J H28J 0.9500 . ? O1K C1K 1.320(9) . ? C1K C2K 1.396(11) . ? C1K C6K 1.424(11) . ? O2K N22K 1.381(8) . ? C2K C3K 1.417(11) . ? C2K C21K 1.469(11) . ? C3K C4K 1.352(12) . ? C3K H3K 0.9500 . ? C4K C5K 1.367(13) . ? C4K H4K 0.9500 . ? C5K C6K 1.375(11) . ? C5K H5K 0.9500 . ? C6K H6K 0.9500 . ? C21K N22K 1.295(9) . ? C21K C23K 1.496(11) . ? C23K C28K 1.341(11) . ? C23K C24K 1.409(11) . ? C24K C25K 1.383(11) . ? C24K H24K 0.9500 . ? C25K C26K 1.387(12) . ? C25K H25K 0.9500 . ? C26K C27K 1.373(13) . ? C26K H26K 0.9500 . ? C27K C28K 1.389(12) . ? C27K H27K 0.9500 . ? C28K H28K 0.9500 . ? O1L C1L 1.321(8) . ? C1L C2L 1.404(9) . ? C1L C6L 1.412(10) . ? O2L N22L 1.386(7) . ? C2L C3L 1.399(10) . ? C2L C21L 1.479(10) . ? C3L C4L 1.391(11) . ? C3L H3L 0.9500 . ? C4L C5L 1.365(11) . ? C4L H4L 0.9500 . ? C5L C6L 1.369(11) . ? C5L H5L 0.9500 . ? C6L H6L 0.9500 . ? C21L N22L 1.294(9) . ? C21L C23L 1.476(10) . ? C23L C28L 1.373(10) . ? C23L C24L 1.384(11) . ? C24L C25L 1.398(12) . ? C24L H24L 0.9500 . ? C25L C26L 1.387(12) . ? C25L H25L 0.9500 . ? C26L C27L 1.341(12) . ? C26L H26L 0.9500 . ? C27L C28L 1.384(11) . ? C27L H27L 0.9500 . ? C28L H28L 0.9500 . ? O1M C1M 1.328(8) . ? C1M C6M 1.389(10) . ? C1M C2M 1.407(10) . ? O2M N22M 1.385(7) . ? C2M C3M 1.410(9) . ? C2M C21M 1.459(10) . ? C3M C4M 1.382(11) . ? C3M H3M 0.9500 . ? C4M C5M 1.349(11) . ? C4M H4M 0.9500 . ? C5M C6M 1.375(10) . ? C5M H5M 0.9500 . ? C6M H6M 0.9500 . ? C21M N22M 1.300(8) . ? C21M C23M 1.477(10) . ? C23M C24M 1.358(11) . ? C23M C28M 1.393(11) . ? C24M C25M 1.381(14) . ? C24M H24M 0.9500 . ? C25M C26M 1.355(17) . ? C25M H25M 0.9500 . ? C26M C27M 1.342(17) . ? C26M H26M 0.9500 . ? C27M C28M 1.376(13) . ? C27M H27M 0.9500 . ? C28M H28M 0.9500 . ? N1N C2N 1.319(9) . ? N1N C6N 1.338(10) . ? C2N C3N 1.365(11) . ? C2N H2N 0.9500 . ? C3N C4N 1.379(12) . ? C3N H3N 0.9500 . ? C4N C5N 1.373(11) . ? C4N H4N 0.9500 . ? C5N C6N 1.368(11) . ? C5N H5N 0.9500 . ? C6N H6N 0.9500 . ? N1P C2P 1.305(10) . ? N1P C6P 1.339(10) . ? C2P C3P 1.372(11) . ? C2P H2P 0.9500 . ? C3P C4P 1.350(13) . ? C3P H3P 0.9500 . ? C4P C5P 1.348(14) . ? C4P H4P 0.9500 . ? C5P C6P 1.376(12) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? N1Q C6Q 1.334(10) . ? N1Q C2Q 1.339(9) . ? C2Q C3Q 1.370(11) . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.334(12) . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.393(13) . ? C4Q H4Q 0.9500 . ? C5Q C6Q 1.390(12) . ? C5Q H5Q 0.9500 . ? C6Q H6Q 0.9500 . ? N1R C2R 1.321(10) . ? N1R C6R 1.352(9) . ? C2R C3R 1.397(12) . ? C2R H2R 0.9500 . ? C3R C4R 1.333(13) . ? C3R H3R 0.9500 . ? C4R C5R 1.367(13) . ? C4R H4R 0.9500 . ? C5R C6R 1.383(11) . ? C5R H5R 0.9500 . ? C6R H6R 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Fe1 O2B 102.1(2) . . ? O1A Fe1 F41 169.95(19) . . ? O2B Fe1 F41 87.80(18) . . ? O1A Fe1 F12 94.52(19) . . ? O2B Fe1 F12 87.81(18) . . ? F41 Fe1 F12 87.33(17) . . ? O1A Fe1 N22A 86.0(2) . . ? O2B Fe1 N22A 171.3(2) . . ? F41 Fe1 N22A 84.13(19) . . ? F12 Fe1 N22A 88.45(18) . . ? O1A Fe1 N1E 89.9(2) . . ? O2B Fe1 N1E 93.3(2) . . ? F41 Fe1 N1E 88.0(2) . . ? F12 Fe1 N1E 175.1(2) . . ? N22A Fe1 N1E 89.8(2) . . ? O1B Fe2 O2C 101.7(2) . . ? O1B Fe2 F12 168.74(19) . . ? O2C Fe2 F12 89.50(18) . . ? O1B Fe2 F23 90.7(2) . . ? O2C Fe2 F23 87.81(18) . . ? F12 Fe2 F23 91.05(17) . . ? O1B Fe2 N1F 89.4(2) . . ? O2C Fe2 N1F 98.7(2) . . ? F12 Fe2 N1F 87.57(19) . . ? F23 Fe2 N1F 173.35(19) . . ? O1B Fe2 N22B 85.8(2) . . ? O2C Fe2 N22B 171.1(2) . . ? F12 Fe2 N22B 83.14(19) . . ? F23 Fe2 N22B 87.28(19) . . ? N1F Fe2 N22B 86.1(2) . . ? O1C Fe3 O2D 98.9(2) . . ? O1C Fe3 F23 167.1(2) . . ? O2D Fe3 F23 93.56(18) . . ? O1C Fe3 F34 94.6(2) . . ? O2D Fe3 F34 85.28(19) . . ? F23 Fe3 F34 89.56(17) . . ? O1C Fe3 N22C 85.4(2) . . ? O2D Fe3 N22C 169.9(2) . . ? F23 Fe3 N22C 82.75(19) . . ? F34 Fe3 N22C 85.32(19) . . ? O1C Fe3 N1G 87.6(2) . . ? O2D Fe3 N1G 90.5(2) . . ? F23 Fe3 N1G 89.1(2) . . ? F34 Fe3 N1G 175.5(2) . . ? N22C Fe3 N1G 98.7(2) . . ? O1D Fe4 O2A 101.9(2) . . ? O1D Fe4 F41 90.57(19) . . ? O2A Fe4 F41 88.28(18) . . ? O1D Fe4 F34 166.9(2) . . ? O2A Fe4 F34 91.21(19) . . ? F41 Fe4 F34 90.11(17) . . ? O1D Fe4 N1H 91.1(2) . . ? O2A Fe4 N1H 90.7(2) . . ? F41 Fe4 N1H 178.2(2) . . ? F34 Fe4 N1H 88.5(2) . . ? O1D Fe4 N22D 84.8(2) . . ? O2A Fe4 N22D 173.2(2) . . ? F41 Fe4 N22D 90.40(19) . . ? F34 Fe4 N22D 82.1(2) . . ? N1H Fe4 N22D 90.4(2) . . ? Fe2 F12 Fe1 122.15(18) . . ? Fe3 F23 Fe2 122.26(19) . . ? Fe4 F34 Fe3 123.0(2) . . ? Fe4 F41 Fe1 122.36(19) . . ? C1A O1A Fe1 131.5(5) . . ? O1A C1A C6A 118.6(6) . . ? O1A C1A C2A 122.3(7) . . ? C6A C1A C2A 119.1(6) . . ? C1A C2A C3A 117.7(7) . . ? C1A C2A C21A 125.1(6) . . ? C3A C2A C21A 117.2(7) . . ? C4A C3A C2A 122.3(7) . . ? C4A C3A H3A 118.8 . . ? C2A C3A H3A 118.8 . . ? C3A C4A C5A 119.2(7) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C4A C5A C6A 120.2(7) . . ? C4A C5A H5A 119.9 . . ? C6A C5A H5A 119.9 . . ? C5A C6A C1A 121.6(7) . . ? C5A C6A H6A 119.2 . . ? C1A C6A H6A 119.2 . . ? N22A C21A C2A 120.6(6) . . ? N22A C21A C23A 120.6(6) . . ? C2A C21A C23A 118.7(6) . . ? C21A N22A O2A 115.3(5) . . ? C21A N22A Fe1 127.4(5) . . ? O2A N22A Fe1 116.9(4) . . ? N22A O2A Fe4 117.7(4) . . ? C28A C23A C24A 119.3(7) . . ? C28A C23A C21A 120.8(7) . . ? C24A C23A C21A 119.8(7) . . ? C25A C24A C23A 120.1(9) . . ? C25A C24A H24A 119.9 . . ? C23A C24A H24A 119.9 . . ? C24A C25A C26A 120.2(9) . . ? C24A C25A H25A 119.9 . . ? C26A C25A H25A 119.9 . . ? C27A C26A C25A 120.1(9) . . ? C27A C26A H26A 119.9 . . ? C25A C26A H26A 119.9 . . ? C26A C27A C28A 120.3(10) . . ? C26A C27A H27A 119.9 . . ? C28A C27A H27A 119.9 . . ? C23A C28A C27A 120.0(8) . . ? C23A C28A H28A 120.0 . . ? C27A C28A H28A 120.0 . . ? C1B O1B Fe2 128.2(5) . . ? O1B C1B C6B 119.6(7) . . ? O1B C1B C2B 122.6(7) . . ? C6B C1B C2B 117.8(7) . . ? N22B O2B Fe1 116.3(4) . . ? C3B C2B C1B 117.3(7) . . ? C3B C2B C21B 119.8(7) . . ? C1B C2B C21B 123.0(7) . . ? C4B C3B C2B 123.6(8) . . ? C4B C3B H3B 118.2 . . ? C2B C3B H3B 118.2 . . ? C3B C4B C5B 118.6(7) . . ? C3B C4B H4B 120.7 . . ? C5B C4B H4B 120.7 . . ? C6B C5B C4B 120.0(8) . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C1B 122.7(8) . . ? C5B C6B H6B 118.6 . . ? C1B C6B H6B 118.6 . . ? N22B C21B C2B 122.1(7) . . ? N22B C21B C23B 118.6(7) . . ? C2B C21B C23B 119.3(6) . . ? C21B N22B O2B 116.3(6) . . ? C21B N22B Fe2 125.7(5) . . ? O2B N22B Fe2 118.0(4) . . ? C24B C23B C28B 118.1(7) . . ? C24B C23B C21B 120.8(7) . . ? C28B C23B C21B 121.1(7) . . ? C25B C24B C23B 122.1(8) . . ? C25B C24B H24B 118.9 . . ? C23B C24B H24B 118.9 . . ? C26B C25B C24B 118.5(8) . . ? C26B C25B H25B 120.8 . . ? C24B C25B H25B 120.8 . . ? C25B C26B C27B 121.5(8) . . ? C25B C26B H26B 119.3 . . ? C27B C26B H26B 119.3 . . ? C26B C27B C28B 119.7(8) . . ? C26B C27B H27B 120.1 . . ? C28B C27B H27B 120.1 . . ? C27B C28B C23B 120.1(8) . . ? C27B C28B H28B 120.0 . . ? C23B C28B H28B 119.9 . . ? C1C O1C Fe3 122.6(5) . . ? O1C C1C C6C 118.8(7) . . ? O1C C1C C2C 122.1(6) . . ? C6C C1C C2C 119.2(7) . . ? N22C O2C Fe2 113.7(3) . . ? C1C C2C C3C 117.4(7) . . ? C1C C2C C21C 124.1(6) . . ? C3C C2C C21C 118.5(7) . . ? C4C C3C C2C 122.3(8) . . ? C4C C3C H3C 118.8 . . ? C2C C3C H3C 118.8 . . ? C3C C4C C5C 118.9(7) . . ? C3C C4C H4C 120.6 . . ? C5C C4C H4C 120.6 . . ? C6C C5C C4C 120.1(8) . . ? C6C C5C H5C 119.9 . . ? C4C C5C H5C 119.9 . . ? C5C C6C C1C 121.8(8) . . ? C5C C6C H6C 119.1 . . ? C1C C6C H6C 119.1 . . ? N22C C21C C2C 120.0(7) . . ? N22C C21C C23C 121.3(6) . . ? C2C C21C C23C 118.7(6) . . ? C21C N22C O2C 115.6(6) . . ? C21C N22C Fe3 124.6(5) . . ? O2C N22C Fe3 119.3(4) . . ? C24C C23C C28C 119.3(7) . . ? C24C C23C C21C 119.0(7) . . ? C28C C23C C21C 121.7(7) . . ? C25C C24C C23C 119.9(8) . . ? C25C C24C H24C 120.0 . . ? C23C C24C H24C 120.0 . . ? C26C C25C C24C 120.8(9) . . ? C26C C25C H25C 119.6 . . ? C24C C25C H25C 119.6 . . ? C25C C26C C27C 119.9(8) . . ? C25C C26C H26C 120.1 . . ? C27C C26C H26C 120.1 . . ? C26C C27C C28C 120.3(8) . . ? C26C C27C H27C 119.9 . . ? C28C C27C H27C 119.9 . . ? C27C C28C C23C 119.8(8) . . ? C27C C28C H28C 120.1 . . ? C23C C28C H28C 120.1 . . ? C1D O1D Fe4 129.2(5) . . ? O1D C1D C6D 118.2(7) . . ? O1D C1D C2D 123.0(7) . . ? C6D C1D C2D 118.8(6) . . ? N22D O2D Fe3 115.7(4) . . ? C3D C2D C1D 117.4(7) . . ? C3D C2D C21D 118.2(7) . . ? C1D C2D C21D 124.4(6) . . ? C4D C3D C2D 122.2(8) . . ? C4D C3D H3D 118.9 . . ? C2D C3D H3D 118.9 . . ? C5D C4D C3D 120.2(7) . . ? C5D C4D H4D 119.9 . . ? C3D C4D H4D 119.9 . . ? C4D C5D C6D 119.5(8) . . ? C4D C5D H5D 120.3 . . ? C6D C5D H5D 120.3 . . ? C1D C6D C5D 121.8(8) . . ? C1D C6D H6D 119.1 . . ? C5D C6D H6D 119.1 . . ? N22D C21D C23D 119.7(7) . . ? N22D C21D C2D 120.1(7) . . ? C23D C21D C2D 120.3(6) . . ? C21D N22D O2D 115.1(6) . . ? C21D N22D Fe4 127.7(5) . . ? O2D N22D Fe4 117.0(4) . . ? C24D C23D C28D 119.4(8) . . ? C24D C23D C21D 120.3(7) . . ? C28D C23D C21D 120.3(7) . . ? C25D C24D C23D 120.1(9) . . ? C25D C24D H24D 120.0 . . ? C23D C24D H24D 120.0 . . ? C26D C25D C24D 120.8(9) . . ? C26D C25D H25D 119.6 . . ? C24D C25D H25D 119.6 . . ? C25D C26D C27D 120.5(9) . . ? C25D C26D H26D 119.8 . . ? C27D C26D H26D 119.8 . . ? C28D C27D C26D 119.6(9) . . ? C28D C27D H27D 120.2 . . ? C26D C27D H27D 120.2 . . ? C27D C28D C23D 119.6(8) . . ? C27D C28D H28D 120.2 . . ? C23D C28D H28D 120.2 . . ? C2E N1E C6E 116.9(7) . . ? C2E N1E Fe1 121.2(5) . . ? C6E N1E Fe1 121.9(5) . . ? N1E C2E C3E 123.6(7) . . ? N1E C2E H2E 118.2 . . ? C3E C2E H2E 118.2 . . ? C4E C3E C2E 117.9(8) . . ? C4E C3E H3E 121.0 . . ? C2E C3E H3E 121.0 . . ? C3E C4E C5E 119.9(8) . . ? C3E C4E H4E 120.1 . . ? C5E C4E H4E 120.1 . . ? C6E C5E C4E 118.9(8) . . ? C6E C5E H5E 120.6 . . ? C4E C5E H5E 120.6 . . ? N1E C6E C5E 122.8(7) . . ? N1E C6E H6E 118.6 . . ? C5E C6E H6E 118.6 . . ? C2F N1F C6F 120.0 . . ? C2F N1F Fe2 119.4(3) . . ? C6F N1F Fe2 118.5(3) . . ? C3F C2F N1F 120.0 . . ? C3F C2F H2F 120.0 . . ? N1F C2F H2F 120.0 . . ? C4F C3F C2F 120.0 . . ? C4F C3F H3F 120.0 . . ? C2F C3F H3F 120.0 . . ? C3F C4F C5F 120.0 . . ? C3F C4F H4F 120.0 . . ? C5F C4F H4F 120.0 . . ? C6F C5F C4F 120.0 . . ? C6F C5F H5F 120.0 . . ? C4F C5F H5F 120.0 . . ? C5F C6F N1F 120.0 . . ? C5F C6F H6F 120.0 . . ? N1F C6F H6F 120.0 . . ? C2G N1G C6G 117.0(7) . . ? C2G N1G Fe3 123.8(6) . . ? C6G N1G Fe3 119.2(5) . . ? N1G C2G C3G 121.6(9) . . ? N1G C2G H2G 119.2 . . ? C3G C2G H2G 119.2 . . ? C4G C3G C2G 121.2(9) . . ? C4G C3G H3G 119.4 . . ? C2G C3G H3G 119.4 . . ? C3G C4G C5G 117.8(9) . . ? C3G C4G H4G 121.1 . . ? C5G C4G H4G 121.1 . . ? C6G C5G C4G 119.2(10) . . ? C6G C5G H5G 120.4 . . ? C4G C5G H5G 120.4 . . ? N1G C6G C5G 123.2(9) . . ? N1G C6G H6G 118.4 . . ? C5G C6G H6G 118.4 . . ? C2H N1H C6H 117.9(7) . . ? C2H N1H Fe4 120.6(5) . . ? C6H N1H Fe4 121.5(5) . . ? N1H C2H C3H 123.0(8) . . ? N1H C2H H2H 118.5 . . ? C3H C2H H2H 118.5 . . ? C4H C3H C2H 117.5(8) . . ? C4H C3H H3H 121.3 . . ? C2H C3H H3H 121.3 . . ? C3H C4H C5H 120.7(8) . . ? C3H C4H H4H 119.6 . . ? C5H C4H H4H 119.6 . . ? C4H C5H C6H 118.0(8) . . ? C4H C5H H5H 121.0 . . ? C6H C5H H5H 121.0 . . ? N1H C6H C5H 122.8(7) . . ? N1H C6H H6H 118.6 . . ? C5H C6H H6H 118.6 . . ? O1J Fe5 O2K 100.8(2) . . ? O1J Fe5 F85 169.92(19) . . ? O2K Fe5 F85 89.24(18) . . ? O1J Fe5 F56 93.7(2) . . ? O2K Fe5 F56 87.27(19) . . ? F85 Fe5 F56 87.85(16) . . ? O1J Fe5 N22J 85.8(2) . . ? O2K Fe5 N22J 172.9(2) . . ? F85 Fe5 N22J 84.2(2) . . ? F56 Fe5 N22J 89.78(19) . . ? O1J Fe5 N1N 90.5(2) . . ? O2K Fe5 N1N 96.0(2) . . ? F85 Fe5 N1N 87.3(2) . . ? F56 Fe5 N1N 174.1(2) . . ? N22J Fe5 N1N 86.4(2) . . ? O1K Fe6 F56 167.9(2) . . ? O1K Fe6 O2L 98.8(2) . . ? F56 Fe6 O2L 93.20(19) . . ? O1K Fe6 F67 93.56(19) . . ? F56 Fe6 F67 88.97(16) . . ? O2L Fe6 F67 85.25(18) . . ? O1K Fe6 N22K 84.6(2) . . ? F56 Fe6 N22K 83.6(2) . . ? O2L Fe6 N22K 173.3(2) . . ? F67 Fe6 N22K 88.81(19) . . ? O1K Fe6 N1P 91.2(2) . . ? F56 Fe6 N1P 87.4(2) . . ? O2L Fe6 N1P 89.3(2) . . ? F67 Fe6 N1P 173.3(2) . . ? N22K Fe6 N1P 96.4(2) . . ? O1L Fe7 O2M 102.52(19) . . ? O1L Fe7 F67 167.03(18) . . ? O2M Fe7 F67 90.45(17) . . ? O1L Fe7 F78 90.96(19) . . ? O2M Fe7 F78 86.96(18) . . ? F67 Fe7 F78 89.87(17) . . ? O1L Fe7 N22L 84.1(2) . . ? O2M Fe7 N22L 172.5(2) . . ? F67 Fe7 N22L 83.01(19) . . ? F78 Fe7 N22L 89.4(2) . . ? O1L Fe7 N1Q 89.7(2) . . ? O2M Fe7 N1Q 90.5(2) . . ? F67 Fe7 N1Q 90.0(2) . . ? F78 Fe7 N1Q 177.5(2) . . ? N22L Fe7 N1Q 93.1(2) . . ? O1M Fe8 O2J 100.5(2) . . ? O1M Fe8 F78 167.6(2) . . ? O2J Fe8 F78 91.77(18) . . ? O1M Fe8 F85 93.53(18) . . ? O2J Fe8 F85 87.60(18) . . ? F78 Fe8 F85 88.36(16) . . ? O1M Fe8 N22M 84.8(2) . . ? O2J Fe8 N22M 172.9(2) . . ? F78 Fe8 N22M 83.06(19) . . ? F85 Fe8 N22M 87.42(18) . . ? O1M Fe8 N1R 91.3(2) . . ? O2J Fe8 N1R 90.3(2) . . ? F78 Fe8 N1R 87.18(19) . . ? F85 Fe8 N1R 175.01(19) . . ? N22M Fe8 N1R 94.2(2) . . ? Fe6 F56 Fe5 123.57(19) . . ? Fe7 F67 Fe6 122.61(19) . . ? Fe8 F78 Fe7 123.7(2) . . ? Fe8 F85 Fe5 121.61(19) . . ? C1J O1J Fe5 130.9(5) . . ? O1J C1J C6J 117.6(7) . . ? O1J C1J C2J 123.4(6) . . ? C6J C1J C2J 118.9(7) . . ? N22J O2J Fe8 118.1(4) . . ? C3J C2J C1J 117.5(7) . . ? C3J C2J C21J 118.8(6) . . ? C1J C2J C21J 123.6(6) . . ? C4J C3J C2J 122.5(7) . . ? C4J C3J H3J 118.7 . . ? C2J C3J H3J 118.7 . . ? C3J C4J C5J 118.9(7) . . ? C3J C4J H4J 120.5 . . ? C5J C4J H4J 120.5 . . ? C6J C5J C4J 120.5(7) . . ? C6J C5J H5J 119.7 . . ? C4J C5J H5J 119.7 . . ? C5J C6J C1J 121.5(7) . . ? C5J C6J H6J 119.2 . . ? C1J C6J H6J 119.2 . . ? N22J C21J C2J 121.5(6) . . ? N22J C21J C23J 118.4(6) . . ? C2J C21J C23J 120.0(6) . . ? C21J N22J O2J 115.0(6) . . ? C21J N22J Fe5 127.7(5) . . ? O2J N22J Fe5 117.0(4) . . ? C28J C23J C24J 119.2(7) . . ? C28J C23J C21J 122.3(7) . . ? C24J C23J C21J 118.5(7) . . ? C25J C24J C23J 119.5(8) . . ? C25J C24J H24J 120.3 . . ? C23J C24J H24J 120.3 . . ? C26J C25J C24J 120.1(9) . . ? C26J C25J H25J 119.9 . . ? C24J C25J H25J 119.9 . . ? C25J C26J C27J 120.8(8) . . ? C25J C26J H26J 119.6 . . ? C27J C26J H26J 119.6 . . ? C26J C27J C28J 120.6(9) . . ? C26J C27J H27J 119.7 . . ? C28J C27J H27J 119.7 . . ? C27J C28J C23J 119.8(8) . . ? C27J C28J H28J 120.1 . . ? C23J C28J H28J 120.1 . . ? C1K O1K Fe6 128.4(5) . . ? O1K C1K C2K 123.6(7) . . ? O1K C1K C6K 117.8(7) . . ? C2K C1K C6K 118.6(7) . . ? N22K O2K Fe5 117.7(4) . . ? C1K C2K C3K 117.4(8) . . ? C1K C2K C21K 123.6(7) . . ? C3K C2K C21K 119.1(8) . . ? C4K C3K C2K 122.8(9) . . ? C4K C3K H3K 118.6 . . ? C2K C3K H3K 118.6 . . ? C3K C4K C5K 120.1(9) . . ? C3K C4K H4K 119.9 . . ? C5K C4K H4K 119.9 . . ? C4K C5K C6K 119.9(9) . . ? C4K C5K H5K 120.1 . . ? C6K C5K H5K 120.1 . . ? C5K C6K C1K 121.2(8) . . ? C5K C6K H6K 119.4 . . ? C1K C6K H6K 119.4 . . ? N22K C21K C2K 121.2(7) . . ? N22K C21K C23K 119.1(7) . . ? C2K C21K C23K 119.7(6) . . ? C21K N22K O2K 114.8(6) . . ? C21K N22K Fe6 126.3(5) . . ? O2K N22K Fe6 118.3(4) . . ? C28K C23K C24K 117.9(8) . . ? C28K C23K C21K 122.2(7) . . ? C24K C23K C21K 119.9(7) . . ? C25K C24K C23K 121.0(8) . . ? C25K C24K H24K 119.5 . . ? C23K C24K H24K 119.5 . . ? C24K C25K C26K 118.7(8) . . ? C24K C25K H25K 120.6 . . ? C26K C25K H25K 120.6 . . ? C27K C26K C25K 120.8(8) . . ? C27K C26K H26K 119.6 . . ? C25K C26K H26K 119.6 . . ? C26K C27K C28K 118.6(8) . . ? C26K C27K H27K 120.7 . . ? C28K C27K H27K 120.7 . . ? C23K C28K C27K 122.9(8) . . ? C23K C28K H28K 118.6 . . ? C27K C28K H28K 118.6 . . ? C1L O1L Fe7 129.7(4) . . ? O1L C1L C2L 123.6(6) . . ? O1L C1L C6L 117.8(6) . . ? C2L C1L C6L 118.5(6) . . ? N22L O2L Fe6 115.2(4) . . ? C3L C2L C1L 118.2(7) . . ? C3L C2L C21L 118.1(7) . . ? C1L C2L C21L 123.5(6) . . ? C4L C3L C2L 121.9(8) . . ? C4L C3L H3L 119.0 . . ? C2L C3L H3L 119.0 . . ? C5L C4L C3L 119.1(8) . . ? C5L C4L H4L 120.4 . . ? C3L C4L H4L 120.4 . . ? C4L C5L C6L 120.7(8) . . ? C4L C5L H5L 119.7 . . ? C6L C5L H5L 119.7 . . ? C5L C6L C1L 121.4(7) . . ? C5L C6L H6L 119.3 . . ? C1L C6L H6L 119.3 . . ? N22L C21L C23L 120.9(7) . . ? N22L C21L C2L 120.0(6) . . ? C23L C21L C2L 119.1(6) . . ? C21L N22L O2L 114.1(6) . . ? C21L N22L Fe7 126.8(5) . . ? O2L N22L Fe7 117.7(4) . . ? C28L C23L C24L 118.5(7) . . ? C28L C23L C21L 123.6(7) . . ? C24L C23L C21L 117.9(7) . . ? C23L C24L C25L 121.1(8) . . ? C23L C24L H24L 119.5 . . ? C25L C24L H24L 119.5 . . ? C26L C25L C24L 118.5(9) . . ? C26L C25L H25L 120.7 . . ? C24L C25L H25L 120.7 . . ? C27L C26L C25L 120.1(9) . . ? C27L C26L H26L 119.9 . . ? C25L C26L H26L 119.9 . . ? C26L C27L C28L 121.6(8) . . ? C26L C27L H27L 119.2 . . ? C28L C27L H27L 119.2 . . ? C23L C28L C27L 120.1(8) . . ? C23L C28L H28L 120.0 . . ? C27L C28L H28L 120.0 . . ? C1M O1M Fe8 131.1(4) . . ? O1M C1M C6M 119.0(7) . . ? O1M C1M C2M 122.0(6) . . ? C6M C1M C2M 119.0(7) . . ? N22M O2M Fe7 117.6(4) . . ? C1M C2M C3M 117.0(6) . . ? C1M C2M C21M 124.4(6) . . ? C3M C2M C21M 118.4(6) . . ? C4M C3M C2M 122.3(7) . . ? C4M C3M H3M 118.8 . . ? C2M C3M H3M 118.8 . . ? C5M C4M C3M 119.5(7) . . ? C5M C4M H4M 120.2 . . ? C3M C4M H4M 120.2 . . ? C4M C5M C6M 120.2(7) . . ? C4M C5M H5M 119.9 . . ? C6M C5M H5M 119.9 . . ? C5M C6M C1M 122.0(8) . . ? C5M C6M H6M 119.0 . . ? C1M C6M H6M 119.0 . . ? N22M C21M C2M 121.0(7) . . ? N22M C21M C23M 121.1(6) . . ? C2M C21M C23M 117.9(6) . . ? C21M N22M O2M 115.0(6) . . ? C21M N22M Fe8 127.4(5) . . ? O2M N22M Fe8 117.6(4) . . ? C24M C23M C28M 119.0(8) . . ? C24M C23M C21M 120.9(7) . . ? C28M C23M C21M 120.1(7) . . ? C23M C24M C25M 119.5(10) . . ? C23M C24M H24M 120.2 . . ? C25M C24M H24M 120.2 . . ? C26M C25M C24M 121.1(11) . . ? C26M C25M H25M 119.5 . . ? C24M C25M H25M 119.5 . . ? C27M C26M C25M 120.1(11) . . ? C27M C26M H26M 120.0 . . ? C25M C26M H26M 120.0 . . ? C26M C27M C28M 120.3(11) . . ? C26M C27M H27M 119.9 . . ? C28M C27M H27M 119.9 . . ? C27M C28M C23M 120.0(10) . . ? C27M C28M H28M 120.0 . . ? C23M C28M H28M 120.0 . . ? C2N N1N C6N 116.8(7) . . ? C2N N1N Fe5 121.7(5) . . ? C6N N1N Fe5 121.3(5) . . ? N1N C2N C3N 124.8(8) . . ? N1N C2N H2N 117.6 . . ? C3N C2N H2N 117.6 . . ? C2N C3N C4N 117.8(8) . . ? C2N C3N H3N 121.1 . . ? C4N C3N H3N 121.1 . . ? C5N C4N C3N 118.5(8) . . ? C5N C4N H4N 120.8 . . ? C3N C4N H4N 120.8 . . ? C6N C5N C4N 119.4(8) . . ? C6N C5N H5N 120.3 . . ? C4N C5N H5N 120.3 . . ? N1N C6N C5N 122.7(8) . . ? N1N C6N H6N 118.6 . . ? C5N C6N H6N 118.6 . . ? C2P N1P C6P 117.6(7) . . ? C2P N1P Fe6 123.8(5) . . ? C6P N1P Fe6 118.5(6) . . ? N1P C2P C3P 122.7(9) . . ? N1P C2P H2P 118.6 . . ? C3P C2P H2P 118.6 . . ? C4P C3P C2P 118.9(9) . . ? C4P C3P H3P 120.6 . . ? C2P C3P H3P 120.6 . . ? C5P C4P C3P 120.2(9) . . ? C5P C4P H4P 119.9 . . ? C3P C4P H4P 119.9 . . ? C4P C5P C6P 117.7(10) . . ? C4P C5P H5P 121.1 . . ? C6P C5P H5P 121.1 . . ? N1P C6P C5P 122.8(9) . . ? N1P C6P H6P 118.6 . . ? C5P C6P H6P 118.6 . . ? C6Q N1Q C2Q 116.6(7) . . ? C6Q N1Q Fe7 120.7(6) . . ? C2Q N1Q Fe7 122.6(5) . . ? N1Q C2Q C3Q 123.4(8) . . ? N1Q C2Q H2Q 118.3 . . ? C3Q C2Q H2Q 118.3 . . ? C4Q C3Q C2Q 119.7(8) . . ? C4Q C3Q H3Q 120.2 . . ? C2Q C3Q H3Q 120.2 . . ? C3Q C4Q C5Q 119.5(9) . . ? C3Q C4Q H4Q 120.3 . . ? C5Q C4Q H4Q 120.3 . . ? C6Q C5Q C4Q 117.4(9) . . ? C6Q C5Q H5Q 121.3 . . ? C4Q C5Q H5Q 121.3 . . ? N1Q C6Q C5Q 123.4(9) . . ? N1Q C6Q H6Q 118.3 . . ? C5Q C6Q H6Q 118.3 . . ? C2R N1R C6R 117.3(7) . . ? C2R N1R Fe8 122.6(5) . . ? C6R N1R Fe8 120.0(5) . . ? N1R C2R C3R 122.9(9) . . ? N1R C2R H2R 118.5 . . ? C3R C2R H2R 118.5 . . ? C4R C3R C2R 119.1(10) . . ? C4R C3R H3R 120.4 . . ? C2R C3R H3R 120.4 . . ? C3R C4R C5R 119.5(9) . . ? C3R C4R H4R 120.3 . . ? C5R C4R H4R 120.3 . . ? C4R C5R C6R 119.4(9) . . ? C4R C5R H5R 120.3 . . ? C6R C5R H5R 120.3 . . ? N1R C6R C5R 121.7(8) . . ? N1R C6R H6R 119.1 . . ? C5R C6R H6R 119.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.287 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.102 # Attachment 'Complex 4.cif' data_EB7068 _database_code_depnum_ccdc_archive 'CCDC 755038' #TrackingRef 'Complex 4.cif' _audit_creation_date 07-06-27 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb7068 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.8061(8) _cell_length_b 13.5584(9) _cell_length_c 14.0247(9) _cell_angle_alpha 71.209(4) _cell_angle_beta 78.955(4) _cell_angle_gamma 78.812(4) _cell_volume 2239.6(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C80 H96 Fe6 N8 O18 # Dc = 1.33 Fooo = 914.00 Mu = 10.12 M = 896.38 # Found Formula = C78 H70 Fe6 N4 O24 # Dc = 1.32 FOOO = 914.00 Mu = 10.15 M = 891.25 _chemical_formula_sum 'C84 H85 Fe6 N5 O24' _chemical_formula_moiety 'C78 H70 Fe6 N4 O24, C6 H15 N' _chemical_compound_source 'Ian Gass Reaction number N2.17' _chemical_formula_weight 1835.66 _cell_measurement_reflns_used 2757 _cell_measurement_theta_min 2 _cell_measurement_theta_max 21 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 1.015 # Sheldrick geometric approximatio 0.89 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 7881 _reflns_number_total 7881 _diffrn_reflns_av_R_equivalents 0.065 # Number of reflections with Friedels Law is 7881 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8004 _diffrn_reflns_theta_min 1.603 _diffrn_reflns_theta_max 25.129 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.129 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min -14 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.87 _refine_diff_density_max 1.48 _refine_ls_number_reflns 7881 _refine_ls_number_restraints 6 _refine_ls_number_parameters 523 #_refine_ls_R_factor_ref 0.0994 _refine_ls_wR_factor_ref 0.1741 _refine_ls_goodness_of_fit_ref 0.9039 #_reflns_number_all 7881 _refine_ls_R_factor_all 0.0994 _refine_ls_wR_factor_all 0.1741 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4615 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_gt 0.1636 _refine_ls_shift/su_max 0.000363 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 0.02P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. H atoms were added geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. BSV indicates that the bridging oxygen O32 is a hydroxyl oxygen atom. The hydrogen atom was positioned geometrically at a distance of 0.85\%A. In order to charge balance the complex, one ethylsalicylaldoxime ligand must be only singly deprotonated. O33 was selected as having the longer Fe-O distance (2.008\%A compared to 1.922\%A). The hydrogen was added geometrically. Restraints on the adps of atoms C56 and C58 - the terminal carbon atoms of the disordered ethylsalicylaldoxime were applied (restrained to be the same with an e.s.d of 0.01). The structure contains one molecule of N(Et)~3~ per asymmetric unit. This is disordered and the electron density has been treated by the van der Sluis and Spek method, accounting for 106 e/cell. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.66 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.63 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C27 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C55 The output from CRYSTALS #axes indicates that none of the adps have a principal axis of greater than 0.4 (see below). No further action taken. C 5 0.02721 0.02741 0.03596 C 6 0.02989 0.04229 0.05061 C 7 0.02105 0.05554 0.06074 C 8 0.01852 0.06157 0.08033 C 9 0.02784 0.05639 0.07166 C 10 0.02572 0.04265 0.04934 C 11 0.01816 0.02153 0.03576 O 12 0.02013 0.02785 0.03164 O 13 0.02317 0.02848 0.03661 C 14 0.02953 0.03433 0.03981 C 15 0.03240 0.04223 0.06314 C 16 0.02586 0.06203 0.09115 C 17 0.02755 0.06168 0.11546 C 18 0.02596 0.04967 0.10455 C 19 0.03134 0.04707 0.07609 C 20 0.01952 0.03308 0.04092 O 21 0.02337 0.03155 0.03732 C 23 0.02968 0.04147 0.06251 C 24 0.03578 0.04644 0.11368 C 25 0.02934 0.05581 0.18451 C 26 0.03315 0.05605 0.20109 C 27 0.03832 0.10073 0.21285 C 28 0.02005 0.08044 0.1457 C 29 0.02140 0.02788 0.06219 C 34 0.01696 0.02419 0.04723 C 35 0.03249 0.04321 0.05556 C 36 0.01807 0.06238 0.07032 C 37 0.01335 0.06299 0.07372 C 38 0.03207 0.03617 0.06122 C 39 0.01186 0.0315 0 0.05618 C 40 0.01896 0.03081 0.04192 C 43 0.02516 0.03567 0.04724 C 44 0.03947 0.04314 0.05866 C 46 0.01944 0.02665 0.03448 C 47 0.01784 0.03353 0.05367 C 48 0.02108 0.04160 0.06506 C 49 0.02463 0.04536 0.08234 C 50 0.02445 0.04692 0.07612 C 51 0.02305 0.04197 0.04907 C 52 0.01897 0.04052 0.08405 C 55 0.01489 0.04012 0.04856 C 56 0.03835 0.06711 0.08301 C 57 0.01592 0.05986 0.06632 C 58 0.04144 0.05720 0.08814 420_ALERT_2_B D-H Without Acceptor O32 - H321 ... ? 420_ALERT_2_B D-H Without Acceptor O33 - H331 ... ? The squeezed solvent is probably acting as a H acceptor. 911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 129 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 1 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.997 4690 4676 14 23.01 0.550 0.996 6250 6228 22 25.13 0.597 0.984 8011 7881 130 #----------------------------------------------------------- ACTA Min. Res. ---- 301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. No action taken. 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 410_ALERT_2_C Short Intra H...H Contact H501 .. H552 .. 1.99 Ang. 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! See above for use of squeeze to treat the disordered solvent region. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.001 -0.001 456.9 106.4 _platon_squeeze_details ; ? ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.96580(7) 0.38732(7) 0.05152(6) 0.0252 1.0000 Uani . . . . . . Fe2 Fe 0.97841(6) 0.27220(7) 0.29480(6) 0.0246 1.0000 Uani . . . . . . Fe3 Fe 0.95262(7) 0.52758(7) 0.20961(6) 0.0251 1.0000 Uani . . . . . . O4 O 0.9784(3) 0.3939(3) 0.1797(3) 0.0234 1.0000 Uani . . . . . . C5 C 0.7093(5) 0.2005(5) 0.1921(5) 0.0302 1.0000 Uani . . . . . . C6 C 0.6384(5) 0.2373(5) 0.1215(5) 0.0409 1.0000 Uani . . . . . . C7 C 0.5487(5) 0.1863(6) 0.1355(6) 0.0458 1.0000 Uani . . . . . . C8 C 0.5328(6) 0.1017(6) 0.2187(6) 0.0535 1.0000 Uani . . . . . . C9 C 0.6031(6) 0.0659(6) 0.2903(6) 0.0520 1.0000 Uani . . . . . . C10 C 0.6910(5) 0.1151(5) 0.2763(5) 0.0392 1.0000 Uani . . . . . . C11 C 0.8079(4) 0.2519(5) 0.1768(4) 0.0252 1.0000 Uani . . . . . . O12 O 0.8245(3) 0.3261(3) 0.0962(3) 0.0265 1.0000 Uani . . . . . . O13 O 0.8659(3) 0.2155(3) 0.2457(3) 0.0294 1.0000 Uani . . . . . . C14 C 1.1950(5) 0.1082(5) 0.1008(5) 0.0346 1.0000 Uani . . . . . . C15 C 1.2163(6) 0.1055(5) -0.0028(5) 0.0459 1.0000 Uani . . . . . . C16 C 1.2984(6) 0.0375(6) -0.0322(6) 0.0597 1.0000 Uani . . . . . . C17 C 1.3628(7) -0.0310(7) 0.0378(7) 0.0682 1.0000 Uani . . . . . . C18 C 1.3433(6) -0.0330(6) 0.1358(7) 0.0601 1.0000 Uani . . . . . . C19 C 1.2609(6) 0.0374(6) 0.1691(6) 0.0515 1.0000 Uani . . . . . . C20 C 1.1095(5) 0.1826(5) 0.1312(5) 0.0312 1.0000 Uani . . . . . . O21 O 1.0562(3) 0.2449(3) 0.0643(3) 0.0307 1.0000 Uani . . . . . . O22 O 1.0953(3) 0.1835(3) 0.2249(3) 0.0334 1.0000 Uani . . . . . . C23 C 1.2586(6) 0.3861(6) 0.3174(5) 0.0446 1.0000 Uani . . . . . . C24 C 1.3115(6) 0.2916(7) 0.3652(7) 0.0653 1.0000 Uani . . . . . . C25 C 1.4203(8) 0.2775(9) 0.3679(9) 0.0899 1.0000 Uani . . . . . . C26 C 1.4761(8) 0.3578(12) 0.3195(9) 0.0968 1.0000 Uani . . . . . . C27 C 1.4251(9) 0.4530(12) 0.2706(9) 0.1173 1.0000 Uani . . . . . . C28 C 1.3154(7) 0.4689(8) 0.2714(7) 0.0821 1.0000 Uani . . . . . . C29 C 1.1391(5) 0.4007(6) 0.3121(5) 0.0372 1.0000 Uani . . . . . . O30 O 1.0975(3) 0.3159(3) 0.3421(3) 0.0339 1.0000 Uani . . . . . . O31 O 1.0912(3) 0.4906(3) 0.2768(3) 0.0318 1.0000 Uani . . . . . . O32 O 1.0507(3) 0.6020(3) 0.0895(3) 0.0300 1.0000 Uani . . . . . . O33 O 0.8788(3) 0.6641(3) 0.2335(3) 0.0296 1.0000 Uani . . . . . . C34 C 0.7731(5) 0.6831(5) 0.2484(5) 0.0295 1.0000 Uani . . . . . . C35 C 0.7195(5) 0.7227(5) 0.3305(5) 0.0438 1.0000 Uani . . . . . . C36 C 0.6109(6) 0.7468(6) 0.3463(6) 0.0503 1.0000 Uani . . . . . . C37 C 0.5498(6) 0.7360(6) 0.2821(6) 0.0500 1.0000 Uani . . . . . . C38 C 0.5961(5) 0.6988(5) 0.2012(5) 0.0432 1.0000 Uani . . . . . . C39 C 0.7074(5) 0.6712(5) 0.1840(5) 0.0332 1.0000 Uani . . . . . . C40 C 0.7540(5) 0.6312(5) 0.0955(5) 0.0306 1.0000 Uani . . . . . . N41 N 0.8467(4) 0.5739(4) 0.1006(3) 0.0231 1.0000 Uani . . . . . . O42 O 0.8936(3) 0.5420(3) 0.0147(3) 0.0263 1.0000 Uani . . . . . . C43 C 0.6966(5) 0.6536(5) 0.0058(5) 0.0360 1.0000 Uani . . . . . . C44 C 0.6369(6) 0.5640(6) 0.0111(5) 0.0471 1.0000 Uani . . . . . . O45 O 0.9535(3) 0.1639(3) 0.4213(3) 0.0273 1.0000 Uani . . . . . . C46 C 0.8567(5) 0.1415(5) 0.4673(4) 0.0269 1.0000 Uani . . . . . . C47 C 0.8412(5) 0.0353(5) 0.5148(5) 0.0350 1.0000 Uani . . . . . . C48 C 0.7437(6) 0.0086(6) 0.5607(5) 0.0426 1.0000 Uani . . . . . . C49 C 0.6549(6) 0.0834(6) 0.5642(5) 0.0508 1.0000 Uani . . . . . . C50 C 0.6684(6) 0.1877(6) 0.5222(5) 0.0492 1.0000 Uani . . . . . . C51 C 0.7655(5) 0.2205(5) 0.4736(5) 0.0380 1.0000 Uani . . . . . . C52 C 0.7741(5) 0.3329(6) 0.4343(5) 0.0478 1.0000 Uani . . . . . . N53 N 0.8547(4) 0.3629(4) 0.3646(4) 0.0302 1.0000 Uani . . . . . . O54 O 0.8599(3) 0.4689(3) 0.3361(3) 0.0339 1.0000 Uani . . . . . . C55 C 0.6770(14) 0.4172(13) 0.4421(12) 0.0345 0.5093 Uani . . . 1 2 . C56 C 0.6953(15) 0.4463(15) 0.5347(14) 0.0628 0.5093 Uani . U . 1 2 . C57 C 0.7128(13) 0.4052(15) 0.4946(16) 0.0474 0.4907 Uani . . . 1 1 . C58 C 0.6196(15) 0.4683(15) 0.4465(15) 0.0623 0.4907 Uani . U . 1 1 . H61 H 0.6502 0.2943 0.0651 0.0497 1.0000 Uiso R . . . . . H71 H 0.5022 0.2102 0.0879 0.0568 1.0000 Uiso R . . . . . H81 H 0.4738 0.0684 0.2284 0.0710 1.0000 Uiso R . . . . . H91 H 0.5913 0.0079 0.3472 0.0581 1.0000 Uiso R . . . . . H101 H 0.7385 0.0895 0.3233 0.0489 1.0000 Uiso R . . . . . H151 H 1.1731 0.1512 -0.0509 0.0525 1.0000 Uiso R . . . . . H161 H 1.3118 0.0370 -0.1003 0.0715 1.0000 Uiso R . . . . . H171 H 1.4210 -0.0774 0.0168 0.0881 1.0000 Uiso R . . . . . H181 H 1.3856 -0.0818 0.1820 0.0776 1.0000 Uiso R . . . . . H191 H 1.2481 0.0370 0.2372 0.0638 1.0000 Uiso R . . . . . H241 H 1.2735 0.2351 0.3970 0.0838 1.0000 Uiso R . . . . . H251 H 1.4549 0.2126 0.4034 0.1238 1.0000 Uiso R . . . . . H261 H 1.5502 0.3486 0.3198 0.1280 1.0000 Uiso R . . . . . H271 H 1.4648 0.5084 0.2374 0.1381 1.0000 Uiso R . . . . . H281 H 1.2804 0.5356 0.2397 0.1011 1.0000 Uiso R . . . . . H351 H 0.7596 0.7321 0.3744 0.0519 1.0000 Uiso R . . . . . H361 H 0.5797 0.7709 0.4001 0.0594 1.0000 Uiso R . . . . . H371 H 0.4762 0.7543 0.2931 0.0575 1.0000 Uiso R . . . . . H381 H 0.5536 0.6927 0.1576 0.0481 1.0000 Uiso R . . . . . H431 H 0.7463 0.6670 -0.0558 0.0417 1.0000 Uiso R . . . . . H432 H 0.6456 0.7165 0.0036 0.0423 1.0000 Uiso R . . . . . H441 H 0.6039 0.5793 -0.0499 0.0717 1.0000 Uiso R . . . . . H442 H 0.6846 0.4997 0.0185 0.0719 1.0000 Uiso R . . . . . H443 H 0.5802 0.5530 0.0678 0.0719 1.0000 Uiso R . . . . . H471 H 0.8980 -0.0159 0.5159 0.0381 1.0000 Uiso R . . . . . H481 H 0.7377 -0.0626 0.5883 0.0508 1.0000 Uiso R . . . . . H491 H 0.5881 0.0634 0.5946 0.0546 1.0000 Uiso R . . . . . H501 H 0.6084 0.2375 0.5251 0.0549 1.0000 Uiso R . . . . . H581 H 0.5998 0.5307 0.4681 0.0899 0.4908 Uiso R . . 1 1 . H582 H 0.6397 0.4876 0.3739 0.0899 0.4908 Uiso R . . 1 1 . H583 H 0.5616 0.4274 0.4662 0.0899 0.4908 Uiso R . . 1 1 . H561 H 0.6422 0.5044 0.5427 0.0940 0.5092 Uiso R . . 1 2 . H562 H 0.7656 0.4668 0.5234 0.0940 0.5092 Uiso R . . 1 2 . H563 H 0.6890 0.3871 0.5952 0.0939 0.5092 Uiso R . . 1 2 . H571 H 0.7594 0.4524 0.4976 0.0551 0.4908 Uiso R . . 1 1 . H572 H 0.6882 0.3638 0.5635 0.0550 0.4908 Uiso R . . 1 1 . H551 H 0.6790 0.4771 0.3807 0.0428 0.5092 Uiso R . . 1 2 . H552 H 0.6092 0.3906 0.4544 0.0431 0.5092 Uiso R . . 1 2 . H321 H 1.1033 0.6063 0.1090 0.0474 1.0000 Uiso R . . . . . H331 H 0.9148 0.6749 0.2732 0.0387 1.0000 Uiso 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 Fe1 0.0266(5) 0.0263(5) 0.0241(5) -0.0094(4) -0.0007(4) -0.0061(4) Fe2 0.0218(5) 0.0259(5) 0.0256(5) -0.0065(4) -0.0022(4) -0.0052(4) Fe3 0.0259(5) 0.0270(5) 0.0251(5) -0.0116(4) -0.0003(4) -0.0061(4) O4 0.023(2) 0.026(2) 0.025(2) -0.0093(18) -0.0051(17) -0.0072(17) C5 0.027(4) 0.031(4) 0.034(4) -0.013(3) -0.004(3) -0.004(3) C6 0.041(4) 0.039(4) 0.047(4) -0.011(3) -0.010(3) -0.012(3) C7 0.031(4) 0.057(5) 0.057(5) -0.019(4) -0.018(3) -0.008(4) C8 0.041(5) 0.067(6) 0.069(5) -0.031(5) -0.008(4) -0.028(4) C9 0.043(5) 0.054(5) 0.049(5) -0.002(4) 0.006(4) -0.017(4) C10 0.034(4) 0.045(4) 0.043(4) -0.013(3) -0.005(3) -0.015(3) C11 0.018(3) 0.028(4) 0.033(3) -0.015(3) -0.001(3) -0.004(3) O12 0.026(2) 0.027(2) 0.029(2) -0.0073(19) -0.0052(18) -0.0082(18) O13 0.026(2) 0.029(2) 0.033(2) -0.0062(19) -0.0069(19) -0.0062(19) C14 0.030(4) 0.037(4) 0.038(4) -0.013(3) -0.003(3) -0.006(3) C15 0.044(5) 0.040(4) 0.048(4) -0.014(4) 0.006(3) -0.002(4) C16 0.049(5) 0.062(6) 0.070(6) -0.039(5) 0.016(4) -0.004(4) C17 0.048(5) 0.071(6) 0.100(7) -0.057(6) -0.013(5) 0.016(5) C18 0.054(5) 0.057(5) 0.083(6) -0.048(5) -0.023(5) 0.018(4) C19 0.041(5) 0.049(5) 0.071(5) -0.021(4) -0.024(4) 0.000(4) C20 0.022(3) 0.032(4) 0.038(4) -0.007(3) 0.000(3) -0.009(3) O21 0.030(2) 0.030(2) 0.034(2) -0.015(2) -0.004(2) -0.001(2) O22 0.031(2) 0.034(3) 0.029(2) -0.008(2) -0.0007(19) 0.001(2) C23 0.036(4) 0.059(5) 0.047(4) -0.025(4) -0.007(3) -0.011(4) C24 0.041(5) 0.062(6) 0.108(7) -0.047(5) -0.022(5) 0.006(4) C25 0.047(6) 0.098(8) 0.164(11) -0.086(8) -0.047(7) 0.010(6) C26 0.034(6) 0.183(14) 0.105(9) -0.096(9) -0.011(6) 0.006(7) C27 0.067(8) 0.174(14) 0.100(9) 0.000(9) -0.006(6) -0.067(8) C28 0.053(6) 0.096(7) 0.100(7) -0.002(6) -0.027(5) -0.049(5) C29 0.041(4) 0.053(5) 0.022(3) -0.009(3) -0.003(3) -0.022(4) O30 0.027(2) 0.041(3) 0.038(3) -0.014(2) -0.0075(19) -0.008(2) O31 0.036(3) 0.034(3) 0.032(2) -0.011(2) -0.012(2) -0.009(2) O32 0.037(3) 0.030(2) 0.025(2) -0.0070(18) -0.0042(18) -0.011(2) O33 0.028(2) 0.035(3) 0.034(2) -0.022(2) -0.0006(18) -0.0056(19) C34 0.027(4) 0.024(3) 0.034(4) -0.012(3) 0.009(3) -0.004(3) C35 0.039(4) 0.046(4) 0.046(4) -0.017(4) 0.005(3) -0.008(3) C36 0.038(4) 0.060(5) 0.050(5) -0.028(4) 0.016(4) 0.000(4) C37 0.029(4) 0.056(5) 0.057(5) -0.025(4) 0.009(4) 0.013(4) C38 0.036(4) 0.040(4) 0.045(4) 0.000(3) -0.005(3) -0.007(3) C39 0.021(3) 0.031(4) 0.038(4) -0.009(3) 0.012(3) 0.002(3) C40 0.029(4) 0.024(3) 0.035(4) -0.002(3) 0.000(3) -0.008(3) N41 0.022(3) 0.022(3) 0.026(3) -0.012(2) 0.003(2) -0.003(2) O42 0.026(2) 0.029(2) 0.024(2) -0.0087(18) -0.0024(17) -0.0041(18) C43 0.026(4) 0.035(4) 0.042(4) -0.007(3) -0.007(3) -0.001(3) C44 0.045(4) 0.046(5) 0.054(5) -0.018(4) -0.014(4) -0.001(4) O45 0.016(2) 0.035(2) 0.032(2) -0.0086(19) -0.0043(17) -0.0055(18) C46 0.026(3) 0.033(4) 0.020(3) -0.005(3) -0.001(3) -0.006(3) C47 0.023(4) 0.034(4) 0.038(4) -0.003(3) -0.004(3) 0.007(3) C48 0.047(5) 0.042(4) 0.039(4) -0.001(3) -0.005(3) -0.026(4) C49 0.037(4) 0.044(5) 0.055(5) 0.001(4) 0.010(4) -0.011(4) C50 0.037(4) 0.047(5) 0.054(5) -0.014(4) 0.014(3) -0.002(4) C51 0.036(4) 0.043(4) 0.032(4) -0.009(3) 0.006(3) -0.015(3) C52 0.035(4) 0.041(4) 0.053(4) -0.010(4) 0.020(4) -0.004(3) N53 0.020(3) 0.034(3) 0.031(3) -0.004(2) -0.001(2) -0.002(2) O54 0.035(3) 0.027(2) 0.032(2) -0.0030(19) 0.0063(19) -0.008(2) C55 0.026(9) 0.042(10) 0.041(9) -0.011(8) -0.012(8) -0.014(7) C56 0.058(10) 0.063(10) 0.072(11) -0.037(8) 0.003(8) -0.002(8) C57 0.021(10) 0.060(13) 0.057(13) -0.014(10) 0.009(9) -0.014(9) C58 0.048(10) 0.056(10) 0.081(11) -0.027(8) 0.004(8) -0.004(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3110(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O42 2_765 2.116(4) yes Fe1 . O32 2_765 1.985(4) yes Fe1 . Fe1 2_765 3.1465(17) yes Fe1 . Fe3 . 3.3180(12) yes Fe1 . O4 . 1.867(4) yes Fe1 . O12 . 2.042(4) yes Fe1 . O21 . 2.023(4) yes Fe1 . O42 . 2.062(4) yes Fe2 . O4 . 1.901(4) yes Fe2 . O13 . 2.073(4) yes Fe2 . O22 . 2.037(4) yes Fe2 . O30 . 2.027(4) yes Fe2 . O45 . 1.922(4) yes Fe2 . N53 . 2.099(5) yes Fe3 . O4 . 1.942(4) yes Fe3 . O31 . 2.069(4) yes Fe3 . O32 . 2.005(4) yes Fe3 . O33 . 2.008(4) yes Fe3 . N41 . 2.102(5) yes Fe3 . O54 . 1.960(4) yes C5 . C6 . 1.381(8) yes C5 . C10 . 1.382(8) yes C5 . C11 . 1.506(8) yes C6 . C7 . 1.404(9) yes C6 . H61 . 0.922 no C7 . C8 . 1.363(10) yes C7 . H71 . 0.918 no C8 . C9 . 1.383(10) yes C8 . H81 . 0.921 no C9 . C10 . 1.368(9) yes C9 . H91 . 0.934 no C10 . H101 . 0.921 no C11 . O12 . 1.262(7) yes C11 . O13 . 1.246(7) yes C14 . C15 . 1.436(9) yes C14 . C19 . 1.399(9) yes C14 . C20 . 1.438(9) yes C15 . C16 . 1.351(9) yes C15 . H151 . 0.942 no C16 . C17 . 1.390(11) yes C16 . H161 . 0.939 no C17 . C18 . 1.342(11) yes C17 . H171 . 0.944 no C18 . C19 . 1.396(10) yes C18 . H181 . 0.933 no C19 . H191 . 0.935 no C20 . O21 . 1.253(7) yes C20 . O22 . 1.295(7) yes C23 . C24 . 1.354(10) yes C23 . C28 . 1.370(10) yes C23 . C29 . 1.518(9) yes C24 . C25 . 1.375(11) yes C24 . H241 . 0.929 no C25 . C26 . 1.341(15) yes C25 . H251 . 0.932 no C26 . C27 . 1.355(15) yes C26 . H261 . 0.934 no C27 . C28 . 1.378(13) yes C27 . H271 . 0.933 no C28 . H281 . 0.936 no C29 . O30 . 1.273(8) yes C29 . O31 . 1.243(8) yes O32 . H321 . 0.793 no O33 . C34 . 1.316(7) yes O33 . H331 . 0.850 no C34 . C35 . 1.428(9) yes C34 . C39 . 1.411(9) yes C35 . C36 . 1.357(9) yes C35 . H351 . 0.925 no C36 . C37 . 1.358(10) yes C36 . H361 . 0.910 no C37 . C38 . 1.374(10) yes C37 . H371 . 0.923 no C38 . C39 . 1.395(8) yes C38 . H381 . 0.925 no C39 . C40 . 1.489(9) yes C40 . N41 . 1.287(7) yes C40 . C43 . 1.495(8) yes N41 . O42 . 1.399(6) yes C43 . C44 . 1.532(9) yes C43 . H431 . 0.959 no C43 . H432 . 0.964 no C44 . H441 . 0.972 no C44 . H442 . 0.951 no C44 . H443 . 0.962 no O45 . C46 . 1.326(6) yes C46 . C47 . 1.414(8) yes C46 . C51 . 1.434(9) yes C47 . C48 . 1.350(8) yes C47 . H471 . 0.902 no C48 . C49 . 1.374(10) yes C48 . H481 . 0.929 no C49 . C50 . 1.377(9) yes C49 . H491 . 0.928 no C50 . C51 . 1.379(9) yes C50 . H501 . 0.924 no C51 . C52 . 1.462(9) yes C52 . N53 . 1.306(7) yes C52 . C57 . 1.51(2) yes C52 . N53 . 1.306(7) yes C52 . C55 . 1.530(19) yes N53 . O54 . 1.373(6) yes C55 . C56 . 1.54(2) yes C55 . H551 . 0.975 no C55 . H552 . 0.969 no C56 . H561 . 0.957 no C56 . H562 . 0.962 no C56 . H563 . 0.964 no C57 . C58 . 1.47(3) yes C57 . H571 . 0.970 no C57 . H572 . 0.975 no C58 . H581 . 0.962 no C58 . H582 . 0.961 no C58 . H583 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O42 2_765 Fe1 . O32 2_765 85.81(15) yes O42 2_765 Fe1 . Fe1 2_765 40.51(10) yes O32 2_765 Fe1 . Fe1 2_765 83.32(11) yes O42 2_765 Fe1 . Fe3 . 81.79(11) yes O32 2_765 Fe1 . Fe3 . 143.45(12) yes Fe1 2_765 Fe1 . Fe3 . 65.09(3) yes O42 2_765 Fe1 . O4 . 91.61(15) yes O32 2_765 Fe1 . O4 . 173.51(16) yes Fe1 2_765 Fe1 . O4 . 90.85(12) yes Fe3 . Fe1 . O4 . 30.08(11) yes O42 2_765 Fe1 . O12 . 172.31(15) yes O32 2_765 Fe1 . O12 . 86.82(16) yes Fe1 2_765 Fe1 . O12 . 136.15(12) yes Fe3 . Fe1 . O12 . 103.00(11) yes O4 . Fe1 . O12 . 95.50(16) yes O42 2_765 Fe1 . O21 . 88.69(15) yes O32 2_765 Fe1 . O21 . 89.62(16) yes Fe1 2_765 Fe1 . O21 . 128.96(12) yes Fe3 . Fe1 . O21 . 124.12(12) yes O4 . Fe1 . O21 . 96.28(16) yes O42 2_765 Fe1 . O42 . 82.32(16) yes O32 2_765 Fe1 . O42 . 84.12(15) yes Fe1 2_765 Fe1 . O42 . 41.81(11) yes Fe3 . Fe1 . O42 . 60.26(10) yes O4 . Fe1 . O42 . 89.64(16) yes O12 . Fe1 . O21 . 93.44(16) yes O12 . Fe1 . O42 . 94.77(15) yes O21 . Fe1 . O42 . 169.38(15) yes O4 . Fe2 . O13 . 92.04(15) yes O4 . Fe2 . O22 . 94.16(16) yes O13 . Fe2 . O22 . 88.12(17) yes O4 . Fe2 . O30 . 90.44(16) yes O13 . Fe2 . O30 . 174.90(17) yes O22 . Fe2 . O30 . 87.26(17) yes O4 . Fe2 . O45 . 168.91(17) yes O13 . Fe2 . O45 . 86.23(16) yes O22 . Fe2 . O45 . 96.73(16) yes O30 . Fe2 . O45 . 92.18(16) yes O4 . Fe2 . N53 . 85.52(17) yes O13 . Fe2 . N53 . 90.30(18) yes O22 . Fe2 . N53 . 178.37(18) yes O30 . Fe2 . N53 . 94.34(19) yes O45 . Fe2 . N53 . 83.54(17) yes Fe1 . Fe3 . O4 . 28.81(11) yes Fe1 . Fe3 . O31 . 110.90(12) yes O4 . Fe3 . O31 . 91.72(16) yes Fe1 . Fe3 . O32 . 78.55(11) yes O4 . Fe3 . O32 . 96.55(16) yes O31 . Fe3 . O32 . 81.77(16) yes Fe1 . Fe3 . O33 . 140.32(12) yes O4 . Fe3 . O33 . 161.79(16) yes O31 . Fe3 . O33 . 105.51(17) yes O32 . Fe3 . O33 . 91.81(16) yes Fe1 . Fe3 . N41 . 59.86(12) yes O4 . Fe3 . N41 . 84.51(16) yes O31 . Fe3 . N41 . 162.28(17) yes O32 . Fe3 . N41 . 81.47(16) yes O33 . Fe3 . N41 . 80.76(17) yes Fe1 . Fe3 . O54 . 109.44(13) yes O4 . Fe3 . O54 . 90.72(16) yes O31 . Fe3 . O54 . 94.75(17) yes O32 . Fe3 . O54 . 172.01(17) yes O33 . Fe3 . O54 . 82.16(17) yes N41 . Fe3 . O54 . 102.59(17) yes Fe3 . O4 . Fe2 . 115.53(18) yes Fe3 . O4 . Fe1 . 121.11(19) yes Fe2 . O4 . Fe1 . 121.3(2) yes C6 . C5 . C10 . 120.0(6) yes C6 . C5 . C11 . 120.2(6) yes C10 . C5 . C11 . 119.8(6) yes C5 . C6 . C7 . 119.3(6) yes C5 . C6 . H61 . 120.4 no C7 . C6 . H61 . 120.2 no C6 . C7 . C8 . 119.5(6) yes C6 . C7 . H71 . 119.3 no C8 . C7 . H71 . 121.2 no C7 . C8 . C9 . 121.0(7) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 119.3 no C8 . C9 . C10 . 119.5(7) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 120.2 no C5 . C10 . C9 . 120.5(6) yes C5 . C10 . H101 . 120.5 no C9 . C10 . H101 . 119.0 no C5 . C11 . O12 . 117.7(5) yes C5 . C11 . O13 . 115.8(5) yes O12 . C11 . O13 . 126.5(5) yes Fe1 . O12 . C11 . 122.7(4) yes Fe2 . O13 . C11 . 134.8(4) yes C15 . C14 . C19 . 117.6(6) yes C15 . C14 . C20 . 120.4(6) yes C19 . C14 . C20 . 122.0(6) yes C14 . C15 . C16 . 120.5(7) yes C14 . C15 . H151 . 120.2 no C16 . C15 . H151 . 119.3 no C15 . C16 . C17 . 120.2(8) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 120.2 no C16 . C17 . C18 . 121.0(7) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 118.9 no C17 . C18 . C19 . 120.7(8) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 119.8 no C14 . C19 . C18 . 119.9(7) yes C14 . C19 . H191 . 119.3 no C18 . C19 . H191 . 120.8 no C14 . C20 . O21 . 117.7(6) yes C14 . C20 . O22 . 117.9(6) yes O21 . C20 . O22 . 124.4(6) yes Fe1 . O21 . C20 . 133.4(4) yes Fe2 . O22 . C20 . 128.2(4) yes C24 . C23 . C28 . 118.8(7) yes C24 . C23 . C29 . 121.2(7) yes C28 . C23 . C29 . 120.0(7) yes C23 . C24 . C25 . 121.4(9) yes C23 . C24 . H241 . 119.4 no C25 . C24 . H241 . 119.2 no C24 . C25 . C26 . 119.5(10) yes C24 . C25 . H251 . 120.2 no C26 . C25 . H251 . 120.3 no C25 . C26 . C27 . 120.2(10) yes C25 . C26 . H261 . 120.1 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 120.5(11) yes C26 . C27 . H271 . 119.5 no C28 . C27 . H271 . 120.0 no C27 . C28 . C23 . 119.5(10) yes C27 . C28 . H281 . 120.1 no C23 . C28 . H281 . 120.4 no C23 . C29 . O30 . 115.0(6) yes C23 . C29 . O31 . 119.3(6) yes O30 . C29 . O31 . 125.7(6) yes Fe2 . O30 . C29 . 132.0(4) yes Fe3 . O31 . C29 . 126.1(4) yes Fe3 . O32 . Fe1 2_765 121.5(2) yes Fe3 . O32 . H321 . 108.2 no Fe1 2_765 O32 . H321 . 127.1 no Fe3 . O33 . C34 . 120.0(4) yes Fe3 . O33 . H331 . 104.8 no C34 . O33 . H331 . 119.7 no O33 . C34 . C35 . 120.0(6) yes O33 . C34 . C39 . 123.5(5) yes C35 . C34 . C39 . 116.4(6) yes C34 . C35 . C36 . 121.8(7) yes C34 . C35 . H351 . 119.2 no C36 . C35 . H351 . 119.0 no C35 . C36 . C37 . 120.4(7) yes C35 . C36 . H361 . 119.0 no C37 . C36 . H361 . 120.6 no C36 . C37 . C38 . 120.9(7) yes C36 . C37 . H371 . 119.2 no C38 . C37 . H371 . 119.9 no C37 . C38 . C39 . 120.2(7) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 119.8 no C34 . C39 . C38 . 120.2(6) yes C34 . C39 . C40 . 121.4(5) yes C38 . C39 . C40 . 118.3(6) yes C39 . C40 . N41 . 116.4(5) yes C39 . C40 . C43 . 122.6(6) yes N41 . C40 . C43 . 121.0(6) yes Fe3 . N41 . C40 . 132.5(4) yes Fe3 . N41 . O42 . 110.9(3) yes C40 . N41 . O42 . 116.3(5) yes Fe1 2_765 O42 . Fe1 . 97.68(16) yes Fe1 2_765 O42 . N41 . 109.4(3) yes Fe1 . O42 . N41 . 112.5(3) yes C40 . C43 . C44 . 113.2(5) yes C40 . C43 . H431 . 110.3 no C44 . C43 . H431 . 108.7 no C40 . C43 . H432 . 107.5 no C44 . C43 . H432 . 109.0 no H431 . C43 . H432 . 108.1 no C43 . C44 . H441 . 111.1 no C43 . C44 . H442 . 110.8 no H441 . C44 . H442 . 108.4 no C43 . C44 . H443 . 111.9 no H441 . C44 . H443 . 106.9 no H442 . C44 . H443 . 107.5 no Fe2 . O45 . C46 . 123.8(3) yes O45 . C46 . C47 . 119.5(5) yes O45 . C46 . C51 . 123.2(5) yes C47 . C46 . C51 . 117.3(5) yes C46 . C47 . C48 . 121.7(6) yes C46 . C47 . H471 . 119.4 no C48 . C47 . H471 . 119.0 no C47 . C48 . C49 . 121.6(7) yes C47 . C48 . H481 . 117.9 no C49 . C48 . H481 . 120.5 no C48 . C49 . C50 . 118.1(7) yes C48 . C49 . H491 . 120.3 no C50 . C49 . H491 . 121.6 no C49 . C50 . C51 . 123.4(7) yes C49 . C50 . H501 . 117.5 no C51 . C50 . H501 . 119.1 no C46 . C51 . C50 . 117.9(6) yes C46 . C51 . C52 . 122.0(6) yes C50 . C51 . C52 . 120.0(6) yes C51 . C52 . N53 . 118.3(6) yes C51 . C52 . C57 . 119.1(8) yes N53 . C52 . C57 . 120.1(8) yes C51 . C52 . N53 . 118.3(6) yes C51 . C52 . C55 . 122.0(8) yes N53 . C52 . C55 . 116.3(8) yes Fe2 . N53 . C52 . 129.4(5) yes Fe2 . N53 . O54 . 116.2(3) yes C52 . N53 . O54 . 114.4(5) yes N53 . O54 . Fe3 . 117.4(3) yes C52 . C55 . C56 . 100.9(14) yes C52 . C55 . H551 . 110.8 no C56 . C55 . H551 . 111.6 no C52 . C55 . H552 . 112.7 no C56 . C55 . H552 . 111.3 no H551 . C55 . H552 . 109.3 no C55 . C56 . H561 . 108.2 no C55 . C56 . H562 . 110.0 no H561 . C56 . H562 . 109.0 no C55 . C56 . H563 . 110.2 no H561 . C56 . H563 . 109.9 no H562 . C56 . H563 . 109.5 no C52 . C57 . C58 . 110.5(18) yes C52 . C57 . H571 . 109.5 no C58 . C57 . H571 . 108.7 no C52 . C57 . H572 . 109.6 no C58 . C57 . H572 . 109.3 no H571 . C57 . H572 . 109.3 no C57 . C58 . H581 . 108.4 no C57 . C58 . H582 . 108.5 no H581 . C58 . H582 . 109.7 no C57 . C58 . H583 . 109.1 no H581 . C58 . H583 . 110.7 no H582 . C58 . H583 . 110.4 no # Attachment 'Complex 5.cif' data_EB7207 _database_code_depnum_ccdc_archive 'CCDC 755039' #TrackingRef 'Complex 5.cif' _audit_creation_date 08-07-03 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb7207 in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H90 Fe6 N4 O24, 2(C6 H15 N), 2(C2 H3 N)' _chemical_compound_source 'Ian Gass, IAG2436' _exptl_crystal_recrystallization_method ; Slow evaporation of MeCN solution. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Checkcif alerts: 601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 223.00 A**3 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 420_ALERT_2_B D-H Without Acceptor O2 - H21 ... ? The solvent region was treated by the van der Sluis and Spek method, accounting for 89 e/cell. This corresponds to two molecules of MeCN per formular unit and F(000), M, mu, D and the formulae have been calculated on this assumption. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.67 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.64 Ratio The C and H atoms have been restrained (see below) as they appear to exhibit high thermal motion, rather than positional disorder. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.83 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N63 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.85 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 No action taken. 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 3 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 53 A cut-off in (sin(\q/\l)^2^) of 0.01 was applied to eliminate reflections that may be poorly measured in the vicinity of the beamstop. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 5655 5655 0 23.01 0.550 1.000 7521 7520 1 25.24 0.600 1.000 9774 9771 3 #----------------------------------------------------------- ACTA Min. Res. --- 26.48 0.627 0.995 11173 11117 56 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6 The following restraint directive was used in refinement: U(IJ)'S 0.0, 0.010000 = C(68) TO C(69) ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 219.3 45.0 2 0.000 0.500 0.500 219.2 45.5 3 0.500 0.500 0.500 51.1 0.4 4 0.500 0.000 1.000 51.1 0.5 5 0.392 0.378 0.423 5.0 0.1 6 0.392 0.122 0.923 5.8 0.1 7 0.608 0.878 0.077 5.1 0.0 8 0.608 0.622 0.577 6.0 0.1 _platon_squeeze_details ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 14.6892(6) _cell_length_b 19.6643(9) _cell_length_c 19.2762(9) _cell_angle_alpha 90 _cell_angle_beta 104.153(2) _cell_angle_gamma 90 _cell_volume 5399.0(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall 'P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C106 H128 Fe6 N8 O24 # Dc = 1.37 Fooo = 2252.00 Mu = 8.59 M = 1116.65 # Found Formula = C102 H124 Fe6 N6 O24 # Dc = 1.32 FOOO = 2252.00 Mu = 8.55 M = 1076.61 _chemical_formula_sum 'C106 H126 Fe6 N8 O24' _chemical_formula_weight 2231.28 _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 0.858 # Sheldrick geometric approximatio 0.88 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 58382 _reflns_number_total 11117 _diffrn_reflns_av_R_equivalents 0.096 # Number of reflections with Friedels Law is 11117 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11168 _diffrn_reflns_theta_min 1.430 _diffrn_reflns_theta_max 26.479 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.950 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 1.31 _oxford_diffrn_Wilson_scale 51.38 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.08 _refine_diff_density_max 0.96 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 11075 _refine_ls_number_restraints 6 _refine_ls_number_parameters 622 _oxford_refine_ls_R_factor_ref 0.1048 _refine_ls_wR_factor_ref 0.1660 _refine_ls_goodness_of_fit_ref 0.6354 _refine_ls_shift/su_max 0.000453 # The values computed from all data _oxford_reflns_number_all 11075 _refine_ls_R_factor_all 0.1048 _refine_ls_wR_factor_all 0.1660 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6311 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_gt 0.1128 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.02168(5) 0.57128(4) -0.02866(4) 0.0198 1.0000 Uani . . . . . . . O2 O 0.0169(2) 0.51807(17) -0.11765(18) 0.0221 1.0000 Uani . . . . . . . Fe3 Fe -0.07888(5) 0.44312(4) -0.15098(4) 0.0206 1.0000 Uani . . . . . . . O4 O -0.0355(2) 0.39018(17) -0.06185(18) 0.0214 1.0000 Uani . . . . . . . Fe5 Fe -0.04709(5) 0.29446(4) -0.07338(4) 0.0217 1.0000 Uani . . . . . . . O6 O -0.1270(3) 0.28233(18) -0.00115(19) 0.0263 1.0000 Uani . . . . . . . C7 C -0.1683(3) 0.3245(3) 0.0301(3) 0.0225 1.0000 Uani . . . . . . . O8 O -0.1402(2) 0.38457(18) 0.04643(19) 0.0245 1.0000 Uani . . . . . . . C9 C -0.2546(4) 0.3009(3) 0.0511(3) 0.0245 1.0000 Uani . . . . . . . C10 C -0.2829(4) 0.2337(3) 0.0393(3) 0.0280 1.0000 Uani . . . . . . . C11 C -0.3600(4) 0.2103(3) 0.0612(3) 0.0308 1.0000 Uani . . . . . . . C12 C -0.4084(4) 0.2549(3) 0.0946(3) 0.0355 1.0000 Uani . . . . . . . C13 C -0.3818(4) 0.3226(3) 0.1066(3) 0.0314 1.0000 Uani . . . . . . . C14 C -0.3037(4) 0.3451(3) 0.0845(3) 0.0269 1.0000 Uani . . . . . . . C15 C -0.4358(5) 0.3696(4) 0.1436(4) 0.0534 1.0000 Uani . . . . . . . C16 C -0.3921(5) 0.1371(3) 0.0492(4) 0.0504 1.0000 Uani . . . . . . . O17 O -0.0727(3) 0.19931(18) -0.1008(2) 0.0275 1.0000 Uani . . . . . . . C18 C -0.1571(4) 0.1714(3) -0.1065(3) 0.0264 1.0000 Uani . . . . . . . C19 C -0.2413(4) 0.2047(3) -0.1410(3) 0.0305 1.0000 Uani . . . . . . . C20 C -0.2431(4) 0.2733(3) -0.1730(3) 0.0285 1.0000 Uani . . . . . . . N21 N -0.1696(3) 0.3117(2) -0.1537(2) 0.0242 1.0000 Uani . . . . . . . O22 O -0.1759(3) 0.37345(18) -0.1863(2) 0.0286 1.0000 Uani . . . . . . . C23 C -0.3291(4) 0.2997(4) -0.2241(4) 0.0488 1.0000 Uani . . . . . . . C24 C -0.3883(5) 0.3417(4) -0.1862(6) 0.0716 1.0000 Uani . . . . . . . C25 C -0.3263(4) 0.1701(3) -0.1462(3) 0.0386 1.0000 Uani . . . . . . . C26 C -0.3294(5) 0.1058(4) -0.1188(4) 0.0443 1.0000 Uani . . . . . . . C27 C -0.2476(5) 0.0735(3) -0.0859(4) 0.0451 1.0000 Uani . . . . . . . C28 C -0.1623(4) 0.1056(3) -0.0801(3) 0.0353 1.0000 Uani . . . . . . . O29 O 0.0415(3) 0.29644(19) -0.1404(2) 0.0285 1.0000 Uani . . . . . . . C30 C 0.0714(4) 0.3480(3) -0.1664(3) 0.0303 1.0000 Uani . . . . . . . O31 O 0.0222(3) 0.3988(2) -0.1935(2) 0.0298 1.0000 Uani . . . . . . . C32 C 0.1739(4) 0.3514(3) -0.1617(3) 0.0336 1.0000 Uani . . . . . . . C33 C 0.2363(4) 0.3171(4) -0.1068(3) 0.0406 1.0000 Uani . . . . . . . C34 C 0.3325(5) 0.3260(4) -0.0977(4) 0.0532 1.0000 Uani . . . . . . . C35 C 0.3629(5) 0.3691(4) -0.1447(5) 0.0552 1.0000 Uani . . . . . . . C36 C 0.3013(5) 0.4025(4) -0.2009(5) 0.0549 1.0000 Uani . . . . . . . C37 C 0.2074(5) 0.3921(3) -0.2078(4) 0.0425 1.0000 Uani . . . . . . . C38 C 0.3376(7) 0.4488(5) -0.2506(6) 0.0830 1.0000 Uani . . . . . . . C39 C 0.4006(6) 0.2910(6) -0.0366(5) 0.0780 1.0000 Uani . . . . . . . O40 O 0.0674(3) 0.27136(18) 0.0049(2) 0.0285 1.0000 Uani . . . . . . . C41 C 0.1020(4) 0.3033(3) 0.0617(3) 0.0273 1.0000 Uani . . . . . . . O42 O 0.0686(2) 0.35604(18) 0.08263(18) 0.0247 1.0000 Uani . . . . . . . C43 C 0.1917(4) 0.2746(3) 0.1074(3) 0.0287 1.0000 Uani . . . . . . . C44 C 0.2355(4) 0.3048(3) 0.1724(3) 0.0319 1.0000 Uani . . . . . . . C45 C 0.3192(4) 0.2783(3) 0.2126(3) 0.0375 1.0000 Uani . . . . . . . C46 C 0.3592(4) 0.2237(3) 0.1858(4) 0.0458 1.0000 Uani . . . . . . . C47 C 0.3183(5) 0.1930(3) 0.1209(4) 0.0465 1.0000 Uani . . . . . . . C48 C 0.2329(4) 0.2192(3) 0.0823(3) 0.0391 1.0000 Uani . . . . . . . C49 C 0.3628(6) 0.1334(4) 0.0909(4) 0.0594 1.0000 Uani . . . . . . . C50 C 0.3665(5) 0.3088(4) 0.2841(4) 0.0557 1.0000 Uani . . . . . . . O51 O -0.1515(2) 0.49695(18) -0.23012(18) 0.0251 1.0000 Uani . . . . . . . C52 C -0.2426(4) 0.5049(3) -0.2396(3) 0.0278 1.0000 Uani . . . . . . . C53 C -0.2868(4) 0.5184(3) -0.1836(3) 0.0278 1.0000 Uani . . . . . . . C54 C -0.2335(4) 0.5275(3) -0.1082(3) 0.0248 1.0000 Uani . . . . . . . N55 N -0.1506(3) 0.5007(2) -0.0904(2) 0.0222 1.0000 Uani . . . . . . . O56 O -0.0960(2) 0.51417(17) -0.02115(17) 0.0207 1.0000 Uani . . . . . . . C57 C -0.2732(4) 0.5650(3) -0.0546(3) 0.0289 1.0000 Uani . . . . . . . C58 C -0.3137(5) 0.5161(3) -0.0089(4) 0.0411 1.0000 Uani . . . . . . . C59 C -0.3845(4) 0.5263(3) -0.1995(3) 0.0322 1.0000 Uani . . . . . . . C60 C -0.4390(4) 0.5206(3) -0.2687(4) 0.0382 1.0000 Uani . . . . . . . C61 C -0.3965(4) 0.5086(3) -0.3232(3) 0.0407 1.0000 Uani . . . . . . . C62 C -0.3006(4) 0.5011(3) -0.3098(3) 0.0375 1.0000 Uani . . . . . . . N63 N -0.0109(4) 0.8584(3) 0.2023(3) 0.0491 1.0000 Uani . . . . . . . C64 C 0.0359(5) 0.9265(4) 0.2136(4) 0.0550 1.0000 Uani . . . . . . . C65 C 0.1362(5) 0.9243(4) 0.2583(4) 0.0555 1.0000 Uani . . . . . . . C66 C -0.0042(7) 0.8199(5) 0.2707(5) 0.0804 1.0000 Uani . . . . . . . C67 C 0.0769(9) 0.7730(5) 0.2905(5) 0.0907 1.0000 Uani . . . . . . . C68 C -0.1127(6) 0.8638(6) 0.1649(6) 0.0936 1.0000 Uani . U . . . . . C69 C -0.1302(7) 0.8931(7) 0.0932(6) 0.1134 1.0000 Uani . U . . . . . H101 H -0.2514 0.2053 0.0154 0.0345 1.0000 Uiso R . . . . . . H121 H -0.4603 0.2400 0.1094 0.0426 1.0000 Uiso R . . . . . . H141 H -0.2839 0.3896 0.0928 0.0320 1.0000 Uiso R . . . . . . H162 H -0.4045 0.1189 0.0914 0.0779 1.0000 Uiso R . . . . . . H161 H -0.4482 0.1362 0.0117 0.0780 1.0000 Uiso R . . . . . . H163 H -0.3452 0.1112 0.0350 0.0775 1.0000 Uiso R . . . . . . H231 H -0.3108 0.3262 -0.2597 0.0527 1.0000 Uiso R . . . . . . H232 H -0.3656 0.2612 -0.2465 0.0526 1.0000 Uiso R . . . . . . H241 H -0.4407 0.3596 -0.2206 0.1060 1.0000 Uiso R . . . . . . H242 H -0.3513 0.3780 -0.1617 0.1058 1.0000 Uiso R . . . . . . H243 H -0.4104 0.3141 -0.1519 0.1058 1.0000 Uiso R . . . . . . H251 H -0.3820 0.1915 -0.1685 0.0425 1.0000 Uiso R . . . . . . H261 H -0.3871 0.0852 -0.1227 0.0537 1.0000 Uiso R . . . . . . H271 H -0.2486 0.0300 -0.0679 0.0526 1.0000 Uiso R . . . . . . H281 H -0.1078 0.0844 -0.0582 0.0422 1.0000 Uiso R . . . . . . H331 H 0.2139 0.2872 -0.0754 0.0508 1.0000 Uiso R . . . . . . H351 H 0.4294 0.3756 -0.1386 0.0742 1.0000 Uiso R . . . . . . H371 H 0.1634 0.4139 -0.2453 0.0550 1.0000 Uiso R . . . . . . H382 H 0.3029 0.4407 -0.3005 0.1484 1.0000 Uiso R . . . . . . H381 H 0.3316 0.4966 -0.2376 0.1482 1.0000 Uiso R . . . . . . H383 H 0.4038 0.4386 -0.2464 0.1482 1.0000 Uiso R . . . . . . H391 H 0.4605 0.3140 -0.0252 0.1241 1.0000 Uiso R . . . . . . H393 H 0.3758 0.2884 0.0055 0.1241 1.0000 Uiso R . . . . . . H392 H 0.4098 0.2447 -0.0516 0.1242 1.0000 Uiso R . . . . . . H441 H 0.2086 0.3421 0.1895 0.0367 1.0000 Uiso R . . . . . . H461 H 0.4172 0.2068 0.2120 0.0519 1.0000 Uiso R . . . . . . H481 H 0.2030 0.1998 0.0383 0.0459 1.0000 Uiso R . . . . . . H492 H 0.3205 0.0948 0.0842 0.0921 1.0000 Uiso R . . . . . . H491 H 0.3759 0.1469 0.0456 0.0922 1.0000 Uiso R . . . . . . H493 H 0.4206 0.1208 0.1249 0.0920 1.0000 Uiso R . . . . . . H571 H -0.3216 0.5955 -0.0793 0.0365 1.0000 Uiso R . . . . . . H572 H -0.2239 0.5906 -0.0248 0.0367 1.0000 Uiso R . . . . . . H581 H -0.3372 0.5399 0.0274 0.0658 1.0000 Uiso R . . . . . . H583 H -0.3646 0.4912 -0.0385 0.0658 1.0000 Uiso R . . . . . . H582 H -0.2667 0.4846 0.0154 0.0657 1.0000 Uiso R . . . . . . H591 H -0.4137 0.5352 -0.1621 0.0384 1.0000 Uiso R . . . . . . H601 H -0.5034 0.5248 -0.2775 0.0429 1.0000 Uiso R . . . . . . H611 H -0.4325 0.5056 -0.3699 0.0449 1.0000 Uiso R . . . . . . H621 H -0.2735 0.4933 -0.3476 0.0415 1.0000 Uiso R . . . . . . H641 H 0.0004 0.9557 0.2377 0.0691 1.0000 Uiso R . . . . . . H642 H 0.0368 0.9444 0.1664 0.0687 1.0000 Uiso R . . . . . . H651 H 0.1629 0.9686 0.2596 0.0838 1.0000 Uiso R . . . . . . H652 H 0.1364 0.9092 0.3058 0.0839 1.0000 Uiso R . . . . . . H653 H 0.1727 0.8933 0.2366 0.0839 1.0000 Uiso R . . . . . . H661 H -0.0002 0.8528 0.3089 0.1026 1.0000 Uiso R . . . . . . H662 H -0.0616 0.7933 0.2649 0.1030 1.0000 Uiso R . . . . . . H671 H 0.0718 0.7484 0.3330 0.1388 1.0000 Uiso R . . . . . . H673 H 0.1346 0.7989 0.3003 0.1392 1.0000 Uiso R . . . . . . H672 H 0.0749 0.7418 0.2514 0.1389 1.0000 Uiso R . . . . . . H681 H -0.1425 0.8928 0.1936 0.1068 1.0000 Uiso R . . . . . . H682 H -0.1408 0.8190 0.1613 0.1072 1.0000 Uiso R . . . . . . H692 H -0.1963 0.8926 0.0717 0.1818 1.0000 Uiso R . . . . . . H691 H -0.1061 0.9384 0.0973 0.1817 1.0000 Uiso R . . . . . . H693 H -0.0980 0.8663 0.0651 0.1817 1.0000 Uiso R . . . . . . H631 H 0.0180 0.8339 0.1740 0.0759 1.0000 Uiso R . . . . . . H21 H 0.0678 0.5059 -0.1214 0.0341 1.0000 Uiso R . . . . . . H151 H -0.4271 0.4156 0.1322 0.0822 1.0000 Uiso R . . . . . . H153 H -0.5006 0.3597 0.1292 0.0824 1.0000 Uiso R . . . . . . H152 H -0.4162 0.3644 0.1938 0.0826 1.0000 Uiso R . . . . . . H503 H 0.4221 0.2843 0.3058 0.0770 1.0000 Uiso R . . . . . . H502 H 0.3835 0.3548 0.2793 0.0774 1.0000 Uiso R . . . . . . H501 H 0.3263 0.3072 0.3160 0.0775 1.0000 Uiso 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 Fe1 0.0209(4) 0.0175(3) 0.0197(3) -0.0005(3) 0.0028(3) -0.0009(3) O2 0.0212(17) 0.0228(18) 0.0227(18) -0.0034(14) 0.0063(14) -0.0009(14) Fe3 0.0204(4) 0.0207(4) 0.0196(3) -0.0019(3) 0.0025(3) -0.0005(3) O4 0.0203(17) 0.0199(17) 0.0212(17) -0.0010(14) -0.0006(14) -0.0003(14) Fe5 0.0213(4) 0.0198(4) 0.0230(4) -0.0034(3) 0.0034(3) 0.0002(3) O6 0.0273(19) 0.0239(19) 0.0289(19) -0.0018(15) 0.0092(15) -0.0016(15) C7 0.024(3) 0.020(2) 0.022(2) 0.0002(19) 0.002(2) 0.002(2) O8 0.0250(18) 0.0225(18) 0.0269(19) -0.0024(15) 0.0083(15) -0.0029(15) C9 0.023(3) 0.025(3) 0.025(3) 0.003(2) 0.005(2) 0.000(2) C10 0.030(3) 0.027(3) 0.028(3) 0.003(2) 0.008(2) 0.004(2) C11 0.031(3) 0.031(3) 0.030(3) 0.006(2) 0.005(2) -0.007(2) C12 0.021(3) 0.047(4) 0.038(3) 0.006(3) 0.007(2) -0.005(2) C13 0.027(3) 0.035(3) 0.033(3) 0.005(2) 0.009(2) 0.004(2) C14 0.028(3) 0.028(3) 0.024(3) -0.003(2) 0.005(2) -0.003(2) C15 0.048(4) 0.053(4) 0.065(5) -0.009(4) 0.025(4) -0.003(3) C16 0.052(4) 0.038(4) 0.067(5) -0.004(3) 0.027(4) -0.015(3) O17 0.031(2) 0.0202(18) 0.032(2) -0.0059(15) 0.0086(16) -0.0016(15) C18 0.027(3) 0.028(3) 0.025(3) -0.010(2) 0.008(2) -0.009(2) C19 0.024(3) 0.033(3) 0.034(3) -0.009(2) 0.007(2) -0.009(2) C20 0.028(3) 0.028(3) 0.028(3) -0.005(2) 0.002(2) -0.004(2) N21 0.025(2) 0.022(2) 0.023(2) -0.0031(17) 0.0006(17) -0.0008(17) O22 0.029(2) 0.0223(18) 0.029(2) -0.0004(15) -0.0027(16) -0.0004(15) C23 0.034(3) 0.045(4) 0.054(4) 0.007(3) -0.016(3) -0.015(3) C24 0.027(4) 0.043(4) 0.132(8) 0.002(5) -0.003(4) -0.003(3) C25 0.031(3) 0.041(4) 0.041(3) -0.010(3) 0.003(3) -0.011(3) C26 0.041(4) 0.048(4) 0.044(4) -0.010(3) 0.011(3) -0.023(3) C27 0.060(4) 0.034(3) 0.042(4) -0.007(3) 0.014(3) -0.014(3) C28 0.042(3) 0.029(3) 0.034(3) -0.003(2) 0.008(3) -0.004(3) O29 0.028(2) 0.028(2) 0.030(2) -0.0059(16) 0.0101(16) -0.0033(16) C30 0.033(3) 0.027(3) 0.033(3) -0.013(2) 0.011(2) -0.005(2) O31 0.030(2) 0.032(2) 0.028(2) -0.0016(16) 0.0091(16) 0.0005(17) C32 0.037(3) 0.025(3) 0.042(3) -0.006(2) 0.016(3) 0.001(2) C33 0.032(3) 0.052(4) 0.038(3) -0.005(3) 0.008(3) 0.002(3) C34 0.042(4) 0.068(5) 0.046(4) -0.015(4) 0.005(3) 0.013(4) C35 0.028(3) 0.065(5) 0.077(5) -0.019(4) 0.021(4) -0.006(3) C36 0.052(4) 0.039(4) 0.085(6) -0.008(4) 0.037(4) -0.001(3) C37 0.042(4) 0.035(3) 0.055(4) -0.001(3) 0.020(3) 0.002(3) C38 0.077(6) 0.061(5) 0.133(9) 0.013(6) 0.066(6) -0.003(5) C39 0.046(5) 0.117(8) 0.065(5) -0.007(6) 0.002(4) 0.011(5) O40 0.0273(19) 0.0238(19) 0.031(2) -0.0062(16) -0.0003(16) 0.0041(15) C41 0.025(3) 0.024(3) 0.031(3) -0.001(2) 0.004(2) -0.001(2) O42 0.0278(19) 0.0221(18) 0.0216(18) 0.0034(14) 0.0010(15) 0.0013(15) C43 0.027(3) 0.024(3) 0.032(3) 0.001(2) 0.001(2) 0.002(2) C44 0.031(3) 0.025(3) 0.038(3) 0.002(2) 0.004(2) 0.000(2) C45 0.033(3) 0.032(3) 0.041(3) 0.011(3) -0.004(3) -0.001(2) C46 0.027(3) 0.041(4) 0.062(4) 0.009(3) -0.003(3) 0.005(3) C47 0.040(4) 0.038(4) 0.057(4) 0.004(3) 0.003(3) 0.005(3) C48 0.033(3) 0.038(3) 0.042(3) -0.005(3) 0.001(3) 0.005(3) C49 0.055(5) 0.052(5) 0.066(5) 0.002(4) 0.006(4) 0.026(4) C50 0.054(4) 0.043(4) 0.052(4) 0.008(3) -0.022(3) 0.004(3) O51 0.0238(19) 0.0259(19) 0.0228(18) 0.0027(15) 0.0002(15) 0.0000(15) C52 0.031(3) 0.024(3) 0.025(3) 0.001(2) 0.000(2) -0.002(2) C53 0.028(3) 0.024(3) 0.026(3) 0.003(2) -0.003(2) 0.001(2) C54 0.022(3) 0.026(3) 0.027(3) 0.004(2) 0.006(2) -0.002(2) N55 0.025(2) 0.025(2) 0.0146(19) 0.0003(17) 0.0008(17) -0.0035(18) O56 0.0225(17) 0.0233(18) 0.0145(16) -0.0031(13) 0.0011(13) 0.0010(14) C57 0.029(3) 0.028(3) 0.029(3) 0.003(2) 0.007(2) 0.005(2) C58 0.040(4) 0.040(4) 0.047(4) 0.010(3) 0.019(3) 0.008(3) C59 0.029(3) 0.028(3) 0.038(3) 0.002(2) 0.005(2) 0.004(2) C60 0.025(3) 0.032(3) 0.051(4) 0.007(3) -0.003(3) 0.000(2) C61 0.032(3) 0.042(4) 0.036(3) -0.004(3) -0.015(3) 0.001(3) C62 0.038(3) 0.040(3) 0.028(3) 0.003(3) -0.004(2) 0.000(3) N63 0.039(3) 0.062(4) 0.047(3) -0.025(3) 0.013(3) 0.003(3) C64 0.060(5) 0.062(5) 0.048(4) -0.016(4) 0.023(4) 0.017(4) C65 0.056(4) 0.049(4) 0.063(5) -0.024(4) 0.017(4) -0.010(4) C66 0.102(7) 0.102(8) 0.054(5) -0.033(5) 0.051(5) -0.044(6) C67 0.141(10) 0.076(7) 0.041(5) -0.009(4) -0.006(5) -0.030(7) C68 0.040(4) 0.123(8) 0.103(6) -0.070(6) -0.012(4) 0.022(5) C69 0.065(5) 0.145(9) 0.106(7) -0.064(7) -0.026(5) 0.045(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17098(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O56 2_565 2.103(3) yes Fe1 . O42 2_565 2.051(3) yes Fe1 . O8 2_565 2.048(4) yes Fe1 . Fe1 2_565 3.1352(14) yes Fe1 . O4 2_565 1.867(3) yes Fe1 . Fe5 2_565 3.2587(10) yes Fe1 . O2 . 1.996(3) yes Fe1 . O56 . 2.096(4) yes O2 . Fe3 . 2.030(3) yes O2 . H21 . 0.805 no Fe3 . O4 . 1.976(3) yes Fe3 . Fe5 . 3.2648(10) yes Fe3 . O22 . 1.974(4) yes Fe3 . O31 . 2.056(4) yes Fe3 . O51 . 1.947(3) yes Fe3 . N55 . 2.087(4) yes O4 . Fe5 . 1.898(3) yes Fe5 . O6 . 2.043(4) yes Fe5 . O17 . 1.956(4) yes Fe5 . N21 . 2.094(4) yes Fe5 . O29 . 2.045(4) yes Fe5 . O40 . 2.018(4) yes O6 . C7 . 1.265(6) yes C7 . O8 . 1.265(6) yes C7 . C9 . 1.496(7) yes C9 . C10 . 1.387(7) yes C9 . C14 . 1.385(7) yes C10 . C11 . 1.381(7) yes C10 . H101 . 0.917 no C11 . C12 . 1.382(8) yes C11 . C16 . 1.514(8) yes C12 . C13 . 1.392(8) yes C12 . H121 . 0.925 no C13 . C14 . 1.388(7) yes C13 . C15 . 1.507(9) yes C14 . H141 . 0.924 no C15 . H151 . 0.946 no C15 . H153 . 0.944 no C15 . H152 . 0.945 no C16 . H162 . 0.946 no C16 . H161 . 0.954 no C16 . H163 . 0.950 no O17 . C18 . 1.335(6) yes C18 . C19 . 1.415(8) yes C18 . C28 . 1.399(8) yes C19 . C20 . 1.479(8) yes C19 . C25 . 1.405(8) yes C20 . N21 . 1.296(7) yes C20 . C23 . 1.492(8) yes N21 . O22 . 1.361(5) yes C23 . C24 . 1.510(11) yes C23 . H231 . 0.950 no C23 . H232 . 0.968 no C24 . H241 . 0.953 no C24 . H242 . 0.950 no C24 . H243 . 0.970 no C25 . C26 . 1.375(9) yes C25 . H251 . 0.927 no C26 . C27 . 1.370(10) yes C26 . H261 . 0.925 no C27 . C28 . 1.383(9) yes C27 . H271 . 0.925 no C28 . H281 . 0.910 no O29 . C30 . 1.258(7) yes C30 . O31 . 1.267(7) yes C30 . C32 . 1.487(8) yes C32 . C33 . 1.393(9) yes C32 . C37 . 1.375(9) yes C33 . C34 . 1.392(9) yes C33 . H331 . 0.958 no C34 . C35 . 1.392(11) yes C34 . C39 . 1.511(11) yes C35 . C36 . 1.394(11) yes C35 . H351 . 0.962 no C36 . C37 . 1.368(9) yes C36 . C38 . 1.510(11) yes C37 . H371 . 0.947 no C38 . H382 . 0.984 no C38 . H381 . 0.982 no C38 . H383 . 0.977 no C39 . H391 . 0.966 no C39 . H393 . 0.969 no C39 . H392 . 0.974 no O40 . C41 . 1.256(6) yes C41 . O42 . 1.256(6) yes C41 . C43 . 1.504(7) yes C43 . C44 . 1.393(8) yes C43 . C48 . 1.390(8) yes C44 . C45 . 1.384(8) yes C44 . H441 . 0.931 no C45 . C46 . 1.384(9) yes C45 . C50 . 1.508(9) yes C46 . C47 . 1.386(10) yes C46 . H461 . 0.939 no C47 . C48 . 1.391(9) yes C47 . C49 . 1.524(10) yes C48 . H481 . 0.935 no C49 . H492 . 0.969 no C49 . H491 . 0.977 no C49 . H493 . 0.969 no C50 . H503 . 0.954 no C50 . H502 . 0.948 no C50 . H501 . 0.951 no O51 . C52 . 1.315(6) yes C52 . C53 . 1.415(8) yes C52 . C62 . 1.413(7) yes C53 . C54 . 1.484(7) yes C53 . C59 . 1.402(8) yes C54 . N55 . 1.294(7) yes C54 . C57 . 1.498(7) yes N55 . O56 . 1.404(5) yes C57 . C58 . 1.520(8) yes C57 . H571 . 0.964 no C57 . H572 . 0.951 no C58 . H581 . 0.974 no C58 . H583 . 0.957 no C58 . H582 . 0.959 no C59 . C60 . 1.382(8) yes C59 . H591 . 0.942 no C60 . C61 . 1.369(9) yes C60 . H601 . 0.923 no C61 . C62 . 1.377(9) yes C61 . H611 . 0.927 no C62 . H621 . 0.924 no N63 . C64 . 1.498(10) yes N63 . C66 . 1.502(11) yes N63 . C68 . 1.498(9) yes N63 . H631 . 0.908 no C64 . C65 . 1.514(10) yes C64 . H641 . 0.967 no C64 . H642 . 0.978 no C65 . H651 . 0.954 no C65 . H652 . 0.963 no C65 . H653 . 0.973 no C66 . C67 . 1.479(14) yes C66 . H661 . 0.971 no C66 . H662 . 0.975 no C67 . H671 . 0.971 no C67 . H673 . 0.968 no C67 . H672 . 0.968 no C68 . C69 . 1.462(16) yes C68 . H681 . 0.971 no C68 . H682 . 0.968 no C69 . H692 . 0.958 no C69 . H691 . 0.955 no C69 . H693 . 0.959 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O56 2_565 Fe1 . O42 2_565 170.73(14) yes O56 2_565 Fe1 . O8 2_565 92.72(14) yes O42 2_565 Fe1 . O8 2_565 95.19(14) yes O56 2_565 Fe1 . Fe1 2_565 41.60(9) yes O42 2_565 Fe1 . Fe1 2_565 129.78(11) yes O8 2_565 Fe1 . Fe1 2_565 133.81(11) yes O56 2_565 Fe1 . O4 2_565 88.40(14) yes O42 2_565 Fe1 . O4 2_565 95.75(14) yes O8 2_565 Fe1 . O4 2_565 94.69(15) yes Fe1 2_565 Fe1 . O4 2_565 91.07(11) yes O56 2_565 Fe1 . Fe5 2_565 113.68(9) yes O42 2_565 Fe1 . Fe5 2_565 72.91(10) yes O8 2_565 Fe1 . Fe5 2_565 77.35(10) yes Fe1 2_565 Fe1 . Fe5 2_565 120.99(4) yes O4 2_565 Fe1 . Fe5 2_565 30.34(10) yes O56 2_565 Fe1 . O2 . 83.04(13) yes O42 2_565 Fe1 . O2 . 92.68(14) yes O8 2_565 Fe1 . O2 . 86.06(14) yes Fe1 2_565 Fe1 . O2 . 82.33(10) yes O4 2_565 Fe1 . O2 . 171.43(15) yes O56 2_565 Fe1 . O56 . 83.39(14) yes O42 2_565 Fe1 . O56 . 88.09(14) yes O8 2_565 Fe1 . O56 . 171.10(14) yes Fe1 2_565 Fe1 . O56 . 41.79(9) yes O4 2_565 Fe1 . O56 . 93.21(14) yes Fe5 2_565 Fe1 . O2 . 156.68(10) yes Fe5 2_565 Fe1 . O56 . 111.54(9) yes O2 . Fe1 . O56 . 85.53(13) yes Fe1 . O2 . Fe3 . 121.92(17) yes Fe1 . O2 . H21 . 113.2 no Fe3 . O2 . H21 . 110.1 no O2 . Fe3 . O4 . 93.22(14) yes O2 . Fe3 . Fe5 . 119.64(10) yes O4 . Fe3 . Fe5 . 31.85(10) yes O2 . Fe3 . O22 . 177.27(15) yes O4 . Fe3 . O22 . 89.23(15) yes Fe5 . Fe3 . O22 . 63.07(11) yes O2 . Fe3 . O31 . 85.51(15) yes O4 . Fe3 . O31 . 90.69(15) yes Fe5 . Fe3 . O31 . 76.50(11) yes O22 . Fe3 . O31 . 95.69(16) yes O2 . Fe3 . O51 . 93.30(15) yes O4 . Fe3 . O51 . 165.04(15) yes Fe5 . Fe3 . O51 . 146.67(11) yes O22 . Fe3 . O51 . 84.04(15) yes O31 . Fe3 . O51 . 103.24(15) yes O2 . Fe3 . N55 . 80.46(15) yes O4 . Fe3 . N55 . 84.21(15) yes Fe5 . Fe3 . N55 . 105.36(12) yes O22 . Fe3 . N55 . 98.58(16) yes O31 . Fe3 . N55 . 164.76(16) yes O51 . Fe3 . N55 . 83.61(16) yes Fe3 . O4 . Fe1 2_565 122.47(18) yes Fe3 . O4 . Fe5 . 114.83(17) yes Fe1 2_565 O4 . Fe5 . 119.87(18) yes O4 . Fe5 . Fe1 2_565 29.79(10) yes O4 . Fe5 . Fe3 . 33.33(10) yes Fe1 2_565 Fe5 . Fe3 . 62.20(2) yes O4 . Fe5 . O6 . 94.93(15) yes Fe1 2_565 Fe5 . O6 . 71.53(10) yes Fe3 . Fe5 . O6 . 112.03(11) yes O4 . Fe5 . O17 . 170.47(15) yes Fe1 2_565 Fe5 . O17 . 157.59(11) yes Fe3 . Fe5 . O17 . 137.40(11) yes O6 . Fe5 . O17 . 88.18(15) yes O4 . Fe5 . N21 . 87.85(15) yes Fe1 2_565 Fe5 . N21 . 105.43(12) yes Fe3 . Fe5 . N21 . 61.05(12) yes O6 . Fe5 . N21 . 89.40(16) yes O17 . Fe5 . N21 . 83.16(16) yes O4 . Fe5 . O29 . 90.14(15) yes Fe1 2_565 Fe5 . O29 . 111.66(11) yes Fe3 . Fe5 . O29 . 74.65(11) yes O6 . Fe5 . O29 . 173.14(15) yes O17 . Fe5 . O29 . 87.55(15) yes O4 . Fe5 . O40 . 95.81(15) yes Fe1 2_565 Fe5 . O40 . 77.26(10) yes Fe3 . Fe5 . O40 . 122.95(11) yes O6 . Fe5 . O40 . 88.67(15) yes O17 . Fe5 . O40 . 93.27(15) yes N21 . Fe5 . O29 . 95.41(16) yes N21 . Fe5 . O40 . 176.00(16) yes O29 . Fe5 . O40 . 86.22(15) yes Fe5 . O6 . C7 . 132.2(3) yes O6 . C7 . O8 . 124.4(5) yes O6 . C7 . C9 . 117.5(4) yes O8 . C7 . C9 . 118.0(4) yes Fe1 2_565 O8 . C7 . 126.4(3) yes C7 . C9 . C10 . 119.4(5) yes C7 . C9 . C14 . 120.2(5) yes C10 . C9 . C14 . 120.3(5) yes C9 . C10 . C11 . 120.2(5) yes C9 . C10 . H101 . 119.6 no C11 . C10 . H101 . 120.2 no C10 . C11 . C12 . 119.0(5) yes C10 . C11 . C16 . 121.2(6) yes C12 . C11 . C16 . 119.8(5) yes C11 . C12 . C13 . 121.9(5) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 118.1 no C12 . C13 . C14 . 118.2(5) yes C12 . C13 . C15 . 120.4(5) yes C14 . C13 . C15 . 121.4(6) yes C13 . C14 . C9 . 120.4(5) yes C13 . C14 . H141 . 119.8 no C9 . C14 . H141 . 119.8 no C13 . C15 . H151 . 111.0 no C13 . C15 . H153 . 110.2 no H151 . C15 . H153 . 108.3 no C13 . C15 . H152 . 110.6 no H151 . C15 . H152 . 108.5 no H153 . C15 . H152 . 108.2 no C11 . C16 . H162 . 110.3 no C11 . C16 . H161 . 108.2 no H162 . C16 . H161 . 109.4 no C11 . C16 . H163 . 109.5 no H162 . C16 . H163 . 110.6 no H161 . C16 . H163 . 108.9 no Fe5 . O17 . C18 . 121.9(3) yes O17 . C18 . C19 . 122.4(5) yes O17 . C18 . C28 . 118.9(5) yes C19 . C18 . C28 . 118.7(5) yes C18 . C19 . C20 . 122.9(5) yes C18 . C19 . C25 . 118.0(5) yes C20 . C19 . C25 . 119.1(5) yes C19 . C20 . N21 . 118.8(5) yes C19 . C20 . C23 . 121.3(5) yes N21 . C20 . C23 . 119.8(5) yes Fe5 . N21 . C20 . 128.6(4) yes Fe5 . N21 . O22 . 115.8(3) yes C20 . N21 . O22 . 115.4(4) yes N21 . O22 . Fe3 . 119.9(3) yes C20 . C23 . C24 . 111.5(6) yes C20 . C23 . H231 . 108.9 no C24 . C23 . H231 . 110.4 no C20 . C23 . H232 . 108.1 no C24 . C23 . H232 . 108.8 no H231 . C23 . H232 . 109.2 no C23 . C24 . H241 . 109.1 no C23 . C24 . H242 . 108.8 no H241 . C24 . H242 . 109.5 no C23 . C24 . H243 . 110.6 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.2 no C19 . C25 . C26 . 122.1(6) yes C19 . C25 . H251 . 118.7 no C26 . C25 . H251 . 119.2 no C25 . C26 . C27 . 119.7(6) yes C25 . C26 . H261 . 119.1 no C27 . C26 . H261 . 121.2 no C26 . C27 . C28 . 120.1(6) yes C26 . C27 . H271 . 120.7 no C28 . C27 . H271 . 119.3 no C18 . C28 . C27 . 121.5(6) yes C18 . C28 . H281 . 118.2 no C27 . C28 . H281 . 120.3 no Fe5 . O29 . C30 . 127.3(3) yes O29 . C30 . O31 . 125.4(5) yes O29 . C30 . C32 . 117.3(5) yes O31 . C30 . C32 . 117.2(5) yes Fe3 . O31 . C30 . 124.4(4) yes C30 . C32 . C33 . 119.6(6) yes C30 . C32 . C37 . 120.2(6) yes C33 . C32 . C37 . 120.0(6) yes C32 . C33 . C34 . 119.6(7) yes C32 . C33 . H331 . 120.9 no C34 . C33 . H331 . 119.5 no C33 . C34 . C35 . 118.2(7) yes C33 . C34 . C39 . 119.9(8) yes C35 . C34 . C39 . 121.9(7) yes C34 . C35 . C36 . 122.8(6) yes C34 . C35 . H351 . 118.6 no C36 . C35 . H351 . 118.6 no C35 . C36 . C37 . 116.9(7) yes C35 . C36 . C38 . 121.0(7) yes C37 . C36 . C38 . 122.1(8) yes C32 . C37 . C36 . 122.5(7) yes C32 . C37 . H371 . 118.1 no C36 . C37 . H371 . 119.4 no C36 . C38 . H382 . 110.2 no C36 . C38 . H381 . 110.3 no H382 . C38 . H381 . 110.2 no C36 . C38 . H383 . 108.8 no H382 . C38 . H383 . 108.4 no H381 . C38 . H383 . 108.9 no C34 . C39 . H391 . 110.9 no C34 . C39 . H393 . 111.4 no H391 . C39 . H393 . 110.0 no C34 . C39 . H392 . 107.9 no H391 . C39 . H392 . 108.7 no H393 . C39 . H392 . 107.9 no Fe5 . O40 . C41 . 128.7(3) yes O40 . C41 . O42 . 125.9(5) yes O40 . C41 . C43 . 115.7(5) yes O42 . C41 . C43 . 118.4(5) yes Fe1 2_565 O42 . C41 . 131.9(3) yes C41 . C43 . C44 . 120.9(5) yes C41 . C43 . C48 . 118.9(5) yes C44 . C43 . C48 . 120.2(5) yes C43 . C44 . C45 . 119.6(6) yes C43 . C44 . H441 . 120.8 no C45 . C44 . H441 . 119.6 no C44 . C45 . C46 . 118.9(6) yes C44 . C45 . C50 . 120.6(6) yes C46 . C45 . C50 . 120.5(6) yes C45 . C46 . C47 . 123.0(6) yes C45 . C46 . H461 . 119.0 no C47 . C46 . H461 . 118.0 no C46 . C47 . C48 . 117.2(6) yes C46 . C47 . C49 . 123.0(6) yes C48 . C47 . C49 . 119.8(6) yes C47 . C48 . C43 . 121.1(6) yes C47 . C48 . H481 . 119.7 no C43 . C48 . H481 . 119.2 no C47 . C49 . H492 . 109.4 no C47 . C49 . H491 . 109.0 no H492 . C49 . H491 . 110.7 no C47 . C49 . H493 . 109.1 no H492 . C49 . H493 . 108.5 no H491 . C49 . H493 . 110.0 no C45 . C50 . H503 . 110.8 no C45 . C50 . H502 . 111.3 no H503 . C50 . H502 . 107.8 no C45 . C50 . H501 . 110.9 no H503 . C50 . H501 . 107.4 no H502 . C50 . H501 . 108.4 no Fe3 . O51 . C52 . 121.2(3) yes O51 . C52 . C53 . 123.8(5) yes O51 . C52 . C62 . 118.9(5) yes C53 . C52 . C62 . 117.3(5) yes C52 . C53 . C54 . 122.7(5) yes C52 . C53 . C59 . 119.4(5) yes C54 . C53 . C59 . 117.9(5) yes C53 . C54 . N55 . 116.6(5) yes C53 . C54 . C57 . 122.3(5) yes N55 . C54 . C57 . 121.2(5) yes Fe3 . N55 . C54 . 130.1(4) yes Fe3 . N55 . O56 . 112.6(3) yes C54 . N55 . O56 . 117.2(4) yes Fe1 2_565 O56 . Fe1 . 96.61(14) yes Fe1 2_565 O56 . N55 . 113.3(3) yes Fe1 . O56 . N55 . 108.9(3) yes C54 . C57 . C58 . 111.2(5) yes C54 . C57 . H571 . 109.3 no C58 . C57 . H571 . 109.6 no C54 . C57 . H572 . 108.0 no C58 . C57 . H572 . 109.5 no H571 . C57 . H572 . 109.1 no C57 . C58 . H581 . 111.7 no C57 . C58 . H583 . 109.8 no H581 . C58 . H583 . 108.3 no C57 . C58 . H582 . 110.7 no H581 . C58 . H582 . 107.3 no H583 . C58 . H582 . 109.0 no C53 . C59 . C60 . 121.5(6) yes C53 . C59 . H591 . 119.2 no C60 . C59 . H591 . 119.3 no C59 . C60 . C61 . 119.3(6) yes C59 . C60 . H601 . 119.8 no C61 . C60 . H601 . 120.9 no C60 . C61 . C62 . 120.8(6) yes C60 . C61 . H611 . 119.8 no C62 . C61 . H611 . 119.4 no C52 . C62 . C61 . 121.6(6) yes C52 . C62 . H621 . 119.2 no C61 . C62 . H621 . 119.2 no C64 . N63 . C66 . 113.2(6) yes C64 . N63 . C68 . 112.0(7) yes C66 . N63 . C68 . 107.6(7) yes C64 . N63 . H631 . 107.3 no C66 . N63 . H631 . 108.8 no C68 . N63 . H631 . 107.9 no N63 . C64 . C65 . 113.9(6) yes N63 . C64 . H641 . 108.7 no C65 . C64 . H641 . 107.8 no N63 . C64 . H642 . 107.2 no C65 . C64 . H642 . 107.8 no H641 . C64 . H642 . 111.5 no C64 . C65 . H651 . 109.1 no C64 . C65 . H652 . 109.1 no H651 . C65 . H652 . 110.6 no C64 . C65 . H653 . 109.7 no H651 . C65 . H653 . 108.5 no H652 . C65 . H653 . 109.9 no N63 . C66 . C67 . 114.6(7) yes N63 . C66 . H661 . 107.9 no C67 . C66 . H661 . 108.9 no N63 . C66 . H662 . 107.4 no C67 . C66 . H662 . 108.3 no H661 . C66 . H662 . 109.6 no C66 . C67 . H671 . 107.8 no C66 . C67 . H673 . 109.6 no H671 . C67 . H673 . 110.1 no C66 . C67 . H672 . 109.0 no H671 . C67 . H672 . 110.4 no H673 . C67 . H672 . 110.0 no N63 . C68 . C69 . 114.0(9) yes N63 . C68 . H681 . 107.7 no C69 . C68 . H681 . 108.0 no N63 . C68 . H682 . 109.1 no C69 . C68 . H682 . 108.5 no H681 . C68 . H682 . 109.4 no C68 . C69 . H692 . 109.2 no C68 . C69 . H691 . 108.3 no H692 . C69 . H691 . 111.1 no C68 . C69 . H693 . 108.8 no H692 . C69 . H693 . 109.8 no H691 . C69 . H693 . 109.5 no # Attachment 'Complex 6.cif' data_brech7 _database_code_depnum_ccdc_archive 'CCDC 755040' #TrackingRef 'Complex 6.cif' # start Validation Reply Form _vrf_PLAT220_brech7 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.56 Ratio RESPONSE: poor crystal quality. ; _vrf_PLAT241_brech7 ; PROBLEM: Check High Ueq as Compared to Neighbors for C15 RESPONSE: Correct atom assignment. ; _vrf_PLAT242_brech7 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C14 RESPONSE: Correct atom assignment. ; _vrf_PLAT234_brech7 ; PROBLEM: Large Hirshfeld Difference C44 -- C45 .. 0.41 Ang. RESPONSE: Poor crystal quality. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe6,(C11 H12 N2 O4)2,(C7 H5 O2)10,(O)2,(H2 O)2,(C2 H3 N)4' _chemical_formula_sum 'C100 H90 Fe6 N8 O32' _chemical_formula_weight 2250.90 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' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.272(5) _cell_length_b 14.458(4) _cell_length_c 16.754(7) _cell_angle_alpha 69.97(8) _cell_angle_beta 71.74(8) _cell_angle_gamma 69.68(6) _cell_volume 2554.5(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2270 _cell_measurement_theta_min 21.3287 _cell_measurement_theta_max 68.2716 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 7.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1902 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34298 _diffrn_reflns_av_R_equivalents 0.1478 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 68.15 _reflns_number_total 8714 _reflns_number_gt 5164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The OH hydrogen atoms were located from a difference map and refined with riding parameters subject to a distance constraint. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1897P)^2^+0.9713P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8714 _refine_ls_number_parameters 668 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1469 _refine_ls_R_factor_gt 0.1084 _refine_ls_wR_factor_ref 0.3458 _refine_ls_wR_factor_gt 0.2984 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.74700(12) 0.02796(8) 0.78785(8) 0.0927(5) Uani 1 1 d . . . Fe2 Fe 0.55746(13) 0.09804(8) 0.95633(8) 0.0927(5) Uani 1 1 d . . . Fe3 Fe 0.60612(13) 0.27245(8) 0.77425(8) 0.0924(5) Uani 1 1 d . . . O1 O 0.5324(5) -0.0207(4) 0.9276(3) 0.0943(15) Uani 1 1 d . . . N1 N 0.6203(6) -0.0581(4) 0.8634(4) 0.0925(18) Uani 1 1 d . . . C1 C 0.6103(8) -0.1352(5) 0.8487(5) 0.093(2) Uani 1 1 d . . . H1A H 0.5415 -0.1586 0.8801 0.112 Uiso 1 1 calc R . . C2 C 0.6972(9) -0.1898(6) 0.7869(6) 0.094(2) Uani 1 1 d . . . C3 C 0.8108(9) -0.1696(5) 0.7410(6) 0.097(3) Uani 1 1 d . . . O3 O 0.8366(5) -0.0936(4) 0.7490(4) 0.0964(15) Uani 1 1 d . . . C4 C 0.8969(10) -0.2345(6) 0.6907(6) 0.104(3) Uani 1 1 d . . . C5 C 0.8642(10) -0.3095(6) 0.6779(6) 0.106(3) Uani 1 1 d . . . H5A H 0.9188 -0.3512 0.6413 0.127 Uiso 1 1 calc R . . C6 C 0.7505(10) -0.3247(6) 0.7186(6) 0.106(3) Uani 1 1 d . . . C7 C 0.6666(9) -0.2678(6) 0.7744(6) 0.104(3) Uani 1 1 d . . . H7A H 0.5915 -0.2815 0.8029 0.125 Uiso 1 1 calc R . . C8 C 1.0215(10) -0.2155(8) 0.6456(7) 0.117(3) Uani 1 1 d . . . C9 C 1.0990(12) -0.2941(9) 0.5929(9) 0.156(5) Uani 1 1 d . . . H9A H 1.1102 -0.3632 0.6321 0.234 Uiso 1 1 calc R . . H9B H 1.1767 -0.2801 0.5646 0.234 Uiso 1 1 calc R . . H9C H 1.0593 -0.2889 0.5485 0.234 Uiso 1 1 calc R . . C10 C 1.0107(12) -0.1088(8) 0.5791(7) 0.134(4) Uani 1 1 d . . . H10A H 1.0903 -0.0985 0.5516 0.201 Uiso 1 1 calc R . . H10B H 0.9626 -0.0557 0.6093 0.201 Uiso 1 1 calc R . . H10C H 0.9724 -0.1050 0.5343 0.201 Uiso 1 1 calc R . . C11 C 1.0824(10) -0.2294(9) 0.7168(8) 0.133(4) Uani 1 1 d . . . H11A H 1.0883 -0.2984 0.7558 0.200 Uiso 1 1 calc R . . H11B H 1.0357 -0.1789 0.7501 0.200 Uiso 1 1 calc R . . H11C H 1.1625 -0.2198 0.6904 0.200 Uiso 1 1 calc R . . N6 N 0.7186(10) -0.4047(6) 0.7035(6) 0.121(3) Uani 1 1 d . . . O5 O 0.7918(9) -0.4559(6) 0.6563(6) 0.162(3) Uani 1 1 d . . . O6 O 0.6177(8) -0.4186(5) 0.7407(5) 0.122(2) Uani 1 1 d . . . O12 O 0.8351(6) -0.0264(5) 0.8835(5) 0.1132(19) Uani 1 1 d . . . O13 O 0.7017(7) 0.0127(5) 1.0017(4) 0.1107(18) Uani 1 1 d . . . C12 C 0.8051(13) -0.0234(7) 0.9626(8) 0.117(3) Uani 1 1 d . . . C13 C 0.8995(13) -0.0761(10) 1.0115(9) 0.146(4) Uani 1 1 d . . . C14 C 0.9925(16) -0.1508(14) 0.9892(13) 0.203(8) Uani 1 1 d . . . H14A H 1.0019 -0.1695 0.9379 0.244 Uiso 1 1 calc R . . C15 C 1.077(3) -0.202(3) 1.041(2) 0.38(3) Uani 1 1 d . . . H15A H 1.1443 -0.2526 1.0212 0.458 Uiso 1 1 calc R . . C16 C 1.067(2) -0.184(2) 1.1151(14) 0.234(9) Uani 1 1 d . . . H16A H 1.1209 -0.2262 1.1519 0.281 Uiso 1 1 calc R . . C17 C 0.9749(17) -0.1009(16) 1.1380(13) 0.189(6) Uani 1 1 d . . . H17A H 0.9724 -0.0785 1.1857 0.227 Uiso 1 1 calc R . . C18 C 0.8875(13) -0.0520(12) 1.0898(10) 0.150(4) Uani 1 1 d . . . H18A H 0.8192 -0.0019 1.1093 0.180 Uiso 1 1 calc R . . O19 O 0.5930(5) 0.2470(3) 0.6662(4) 0.0979(16) Uani 1 1 d . . . O20 O 0.6646(6) 0.0775(4) 0.6859(4) 0.1029(17) Uani 1 1 d . . . C19 C 0.6183(8) 0.1659(6) 0.6425(6) 0.093(2) Uani 1 1 d . . . C20 C 0.5912(8) 0.1762(6) 0.5594(5) 0.092(2) Uani 1 1 d . . . C21 C 0.5488(9) 0.2704(6) 0.5077(6) 0.102(3) Uani 1 1 d . . . H21A H 0.5344 0.3294 0.5264 0.122 Uiso 1 1 calc R . . C22 C 0.5263(10) 0.2818(7) 0.4280(7) 0.120(3) Uani 1 1 d . . . H22A H 0.4990 0.3480 0.3918 0.143 Uiso 1 1 calc R . . C23 C 0.5440(10) 0.1956(8) 0.4021(7) 0.119(3) Uani 1 1 d . . . H23A H 0.5284 0.2022 0.3481 0.143 Uiso 1 1 calc R . . C24 C 0.5837(12) 0.1018(8) 0.4538(7) 0.134(4) Uani 1 1 d . . . H24A H 0.5951 0.0426 0.4362 0.161 Uiso 1 1 calc R . . C25 C 0.6076(11) 0.0915(7) 0.5320(7) 0.130(4) Uani 1 1 d . . . H25A H 0.6358 0.0251 0.5676 0.156 Uiso 1 1 calc R . . O26 O 0.7798(6) 0.2691(4) 0.7157(4) 0.1012(17) Uani 1 1 d . . . C26 C 0.8708(9) 0.1978(6) 0.6927(6) 0.098(3) Uani 1 1 d . . . O27 O 0.8665(6) 0.1068(4) 0.7121(4) 0.1097(18) Uani 1 1 d . . . C27 C 0.9802(9) 0.2245(7) 0.6400(6) 0.105(3) Uani 1 1 d . . . C28 C 0.9846(12) 0.3260(8) 0.6177(8) 0.132(4) Uani 1 1 d . . . H28A H 0.9171 0.3764 0.6376 0.159 Uiso 1 1 calc R . . C29 C 1.0900(13) 0.3529(10) 0.5655(10) 0.154(5) Uani 1 1 d . . . H29A H 1.0928 0.4220 0.5480 0.185 Uiso 1 1 calc R . . C30 C 1.1883(12) 0.2784(11) 0.5403(9) 0.147(4) Uani 1 1 d . . . H30A H 1.2597 0.2969 0.5071 0.176 Uiso 1 1 calc R . . C31 C 1.1873(13) 0.1773(11) 0.5614(9) 0.151(4) Uani 1 1 d . . . H31A H 1.2555 0.1274 0.5416 0.181 Uiso 1 1 calc R . . C32 C 1.0819(11) 0.1506(9) 0.6131(8) 0.127(3) Uani 1 1 d . . . H32A H 1.0801 0.0813 0.6300 0.152 Uiso 1 1 calc R . . O33 O 0.5798(6) 0.2103(4) 0.9922(4) 0.1067(18) Uani 1 1 d . . . O34 O 0.6150(6) 0.3281(4) 0.8670(4) 0.0993(16) Uani 1 1 d . . . C33 C 0.6090(8) 0.2936(6) 0.9471(7) 0.094(2) Uani 1 1 d . . . C34 C 0.6303(8) 0.3491(6) 0.9974(6) 0.090(2) Uani 1 1 d . . . C35 C 0.6351(10) 0.3108(7) 1.0832(7) 0.116(3) Uani 1 1 d . . . H35A H 0.6244 0.2445 1.1131 0.139 Uiso 1 1 calc R . . C36 C 0.6553(11) 0.3657(9) 1.1279(8) 0.131(4) Uani 1 1 d . . . H36A H 0.6599 0.3363 1.1872 0.157 Uiso 1 1 calc R . . C37 C 0.6684(12) 0.4604(9) 1.0881(8) 0.136(4) Uani 1 1 d . . . H37A H 0.6787 0.4989 1.1198 0.163 Uiso 1 1 calc R . . C38 C 0.6667(10) 0.5009(7) 1.0016(8) 0.118(3) Uani 1 1 d . . . H38A H 0.6804 0.5663 0.9726 0.142 Uiso 1 1 calc R . . C39 C 0.6453(8) 0.4478(6) 0.9555(6) 0.102(3) Uani 1 1 d . . . H39A H 0.6408 0.4778 0.8962 0.122 Uiso 1 1 calc R . . O40 O 0.3945(6) 0.1920(4) 0.9433(4) 0.1071(18) Uani 1 1 d . . . O41 O 0.4249(6) 0.3029(4) 0.8153(5) 0.1056(17) Uani 1 1 d . . . C40 C 0.3576(11) 0.2691(7) 0.8850(7) 0.108(3) Uani 1 1 d . . . C41 C 0.2328(11) 0.3263(8) 0.8967(12) 0.149(5) Uani 1 1 d . . . C42 C 0.1689(16) 0.3106(11) 0.9834(15) 0.209(8) Uani 1 1 d . . . H42A H 0.2052 0.2614 1.0287 0.251 Uiso 1 1 calc R . . C43 C 0.050(3) 0.369(2) 1.002(2) 0.34(2) Uani 1 1 d . . . H43A H 0.0047 0.3693 1.0599 0.403 Uiso 1 1 calc R . . C44 C 0.001(3) 0.431(2) 0.921(4) 0.41(3) Uani 1 1 d . . . H44A H -0.0828 0.4615 0.9286 0.496 Uiso 1 1 calc R . . C45 C 0.065(3) 0.447(2) 0.840(2) 0.295(17) Uani 1 1 d . . . H45A H 0.0328 0.4925 0.7913 0.354 Uiso 1 1 calc R . . C46 C 0.1798(15) 0.3931(12) 0.8309(13) 0.186(7) Uani 1 1 d . . . H46A H 0.2285 0.4024 0.7737 0.224 Uiso 1 1 calc R . . O50 O 0.6345(5) 0.1360(3) 0.8401(3) 0.0895(14) Uani 1 1 d . . . O60 O 0.5708(6) 0.4260(4) 0.7034(4) 0.1036(17) Uani 1 1 d D . . H60A H 0.513(8) 0.453(8) 0.667(6) 0.155 Uiso 1 1 d D . . H60B H 0.576(10) 0.456(8) 0.746(6) 0.155 Uiso 1 1 d D . . N47 N 0.6267(17) 0.5048(12) 0.3839(14) 0.222(7) Uani 1 1 d . . . C47 C 0.6641(14) 0.4962(13) 0.4487(13) 0.165(6) Uani 1 1 d . . . C48 C 0.7000(17) 0.4698(11) 0.5153(9) 0.170(6) Uani 1 1 d . . . H48A H 0.6516 0.4284 0.5621 0.255 Uiso 1 1 calc R . . H48B H 0.6939 0.5305 0.5319 0.255 Uiso 1 1 calc R . . H48C H 0.7833 0.4294 0.5055 0.255 Uiso 1 1 calc R . . N49 N 0.6118(13) 0.0566(10) 0.2558(8) 0.176(5) Uani 1 1 d . . . C49 C 0.6304(12) -0.0170(11) 0.2464(7) 0.134(4) Uani 1 1 d . . . C50 C 0.6524(13) -0.1200(10) 0.2335(10) 0.164(5) Uani 1 1 d . . . H50A H 0.6519 -0.1713 0.2898 0.246 Uiso 1 1 calc R . . H50B H 0.7300 -0.1371 0.1940 0.246 Uiso 1 1 calc R . . H50C H 0.5897 -0.1189 0.2083 0.246 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 Fe1 0.1359(11) 0.0619(7) 0.0928(9) -0.0331(6) -0.0305(7) -0.0242(6) Fe2 0.1391(11) 0.0606(7) 0.0896(9) -0.0319(6) -0.0247(7) -0.0286(7) Fe3 0.1412(12) 0.0596(7) 0.0905(9) -0.0313(6) -0.0329(7) -0.0256(6) O1 0.136(4) 0.067(3) 0.094(4) -0.042(3) -0.016(3) -0.033(3) N1 0.124(5) 0.065(3) 0.094(4) -0.038(3) -0.019(4) -0.019(3) C1 0.133(7) 0.066(4) 0.092(5) -0.043(4) -0.019(5) -0.024(4) C2 0.136(7) 0.063(4) 0.097(6) -0.038(4) -0.039(5) -0.016(4) C3 0.145(8) 0.056(4) 0.096(5) -0.037(4) -0.031(5) -0.015(4) O3 0.127(4) 0.071(3) 0.101(4) -0.038(3) -0.025(3) -0.023(3) C4 0.165(9) 0.063(4) 0.088(5) -0.033(4) -0.028(5) -0.022(5) C5 0.143(8) 0.074(5) 0.091(6) -0.040(4) -0.002(5) -0.023(5) C6 0.180(9) 0.059(4) 0.085(5) -0.036(4) -0.033(6) -0.021(5) C7 0.157(8) 0.064(4) 0.098(6) -0.033(4) -0.029(5) -0.027(4) C8 0.149(9) 0.104(7) 0.101(7) -0.044(5) -0.004(6) -0.043(6) C9 0.193(12) 0.103(7) 0.165(11) -0.070(7) -0.007(9) -0.027(7) C10 0.190(11) 0.098(6) 0.113(8) -0.034(6) -0.006(7) -0.056(7) C11 0.124(8) 0.130(8) 0.149(10) -0.059(7) -0.021(7) -0.025(6) N6 0.181(9) 0.077(4) 0.109(6) -0.051(4) -0.003(6) -0.041(5) O5 0.233(9) 0.115(5) 0.158(7) -0.088(5) 0.026(6) -0.079(6) O6 0.186(7) 0.089(4) 0.110(5) -0.042(3) -0.028(5) -0.049(4) O12 0.140(5) 0.100(4) 0.113(5) -0.051(4) -0.046(4) -0.010(3) O13 0.131(5) 0.093(4) 0.113(5) -0.038(4) -0.027(4) -0.025(4) C12 0.167(11) 0.075(5) 0.125(9) -0.028(5) -0.081(8) -0.005(6) C13 0.179(12) 0.134(9) 0.150(10) -0.067(8) -0.067(9) -0.015(8) C14 0.198(15) 0.197(16) 0.251(19) -0.146(15) -0.111(14) 0.042(12) C15 0.35(3) 0.47(5) 0.37(4) -0.30(4) -0.29(3) 0.20(3) C16 0.24(2) 0.25(2) 0.201(18) -0.060(17) -0.132(17) 0.015(18) C17 0.173(14) 0.206(17) 0.204(17) -0.061(14) -0.099(13) -0.012(12) C18 0.152(11) 0.167(11) 0.150(11) -0.062(9) -0.049(9) -0.030(9) O19 0.151(5) 0.058(3) 0.100(4) -0.028(2) -0.042(3) -0.026(3) O20 0.157(5) 0.065(3) 0.104(4) -0.030(3) -0.055(4) -0.019(3) C19 0.126(7) 0.071(5) 0.093(5) -0.036(4) -0.024(5) -0.026(4) C20 0.121(6) 0.072(4) 0.093(5) -0.042(4) -0.020(5) -0.021(4) C21 0.146(8) 0.080(5) 0.087(6) -0.035(4) -0.027(5) -0.026(5) C22 0.165(9) 0.082(5) 0.110(7) -0.041(5) -0.039(6) -0.008(5) C23 0.164(9) 0.102(7) 0.100(7) -0.043(6) -0.048(6) -0.013(6) C24 0.220(12) 0.092(7) 0.112(8) -0.044(6) -0.059(8) -0.031(7) C25 0.211(11) 0.082(5) 0.120(8) -0.044(5) -0.071(8) -0.017(6) O26 0.140(5) 0.077(3) 0.097(4) -0.030(3) -0.018(3) -0.041(3) C26 0.139(8) 0.071(5) 0.096(6) -0.036(4) -0.029(5) -0.025(5) O27 0.138(5) 0.075(3) 0.124(5) -0.043(3) -0.013(4) -0.035(3) C27 0.130(8) 0.093(6) 0.102(6) -0.032(5) -0.017(6) -0.040(6) C28 0.162(10) 0.090(6) 0.145(9) -0.037(6) -0.025(8) -0.037(6) C29 0.156(11) 0.104(8) 0.185(13) -0.031(8) 0.004(9) -0.057(8) C30 0.126(9) 0.138(10) 0.166(11) -0.039(9) 0.002(8) -0.053(8) C31 0.161(11) 0.132(10) 0.148(10) -0.044(8) -0.004(9) -0.045(8) C32 0.145(9) 0.103(7) 0.137(9) -0.046(6) -0.027(7) -0.028(7) O33 0.172(5) 0.075(3) 0.094(4) -0.035(3) -0.022(4) -0.051(3) O34 0.156(5) 0.064(3) 0.093(4) -0.030(3) -0.038(4) -0.030(3) C33 0.123(6) 0.067(4) 0.104(6) -0.035(4) -0.026(5) -0.028(4) C34 0.120(6) 0.074(4) 0.090(6) -0.036(4) -0.027(4) -0.027(4) C35 0.173(9) 0.093(6) 0.102(7) -0.030(5) -0.037(6) -0.050(6) C36 0.186(10) 0.121(8) 0.126(8) -0.058(7) -0.048(7) -0.051(7) C37 0.207(12) 0.105(7) 0.138(9) -0.062(7) -0.057(8) -0.047(7) C38 0.170(9) 0.076(5) 0.136(9) -0.051(5) -0.048(7) -0.031(5) C39 0.141(7) 0.072(4) 0.110(6) -0.043(4) -0.028(5) -0.030(5) O40 0.138(5) 0.069(3) 0.112(4) -0.039(3) -0.008(4) -0.028(3) O41 0.132(5) 0.078(3) 0.113(5) -0.035(3) -0.045(4) -0.010(3) C40 0.161(10) 0.070(5) 0.106(7) -0.034(5) -0.033(7) -0.033(6) C41 0.115(9) 0.080(6) 0.196(13) -0.018(7) -0.002(9) -0.005(6) C42 0.165(14) 0.110(10) 0.27(2) -0.043(12) 0.007(14) 0.003(9) C43 0.23(3) 0.18(2) 0.41(5) -0.03(3) 0.10(3) -0.036(19) C44 0.21(3) 0.16(2) 0.61(8) 0.08(3) 0.00(4) 0.005(18) C45 0.19(2) 0.20(2) 0.34(4) 0.07(2) -0.05(2) -0.027(18) C46 0.139(12) 0.138(11) 0.243(19) -0.016(12) -0.070(12) 0.001(9) O50 0.132(4) 0.064(3) 0.088(3) -0.034(2) -0.035(3) -0.022(3) O60 0.163(5) 0.061(3) 0.099(4) -0.024(3) -0.044(4) -0.029(3) N47 0.267(19) 0.150(11) 0.241(18) -0.062(12) -0.053(15) -0.040(11) C47 0.142(11) 0.173(14) 0.143(14) -0.023(11) -0.043(10) -0.006(9) C48 0.30(2) 0.123(9) 0.125(10) -0.032(8) -0.071(12) -0.077(11) N49 0.274(15) 0.136(9) 0.140(9) -0.073(7) -0.062(9) -0.029(9) C49 0.172(10) 0.137(10) 0.102(7) -0.053(7) -0.026(7) -0.034(8) C50 0.189(12) 0.134(10) 0.183(13) -0.078(9) -0.018(10) -0.043(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.927(5) . ? Fe1 O50 1.948(5) . ? Fe1 O12 1.997(7) . ? Fe1 O27 2.016(6) . ? Fe1 O20 2.048(6) . ? Fe1 N1 2.145(7) . ? Fe2 O50 1.860(6) . ? Fe2 O13 1.979(8) . ? Fe2 O40 2.019(7) . ? Fe2 O33 2.037(5) . ? Fe2 O1 2.067(6) 2_657 ? Fe2 O1 2.073(4) . ? Fe3 O50 1.872(5) . ? Fe3 O34 2.025(6) . ? Fe3 O19 2.029(5) . ? Fe3 O26 2.039(6) . ? Fe3 O41 2.045(7) . ? Fe3 O60 2.091(6) . ? O1 N1 1.370(8) . ? O1 Fe2 2.067(6) 2_657 ? N1 C1 1.273(9) . ? C1 C2 1.455(11) . ? C1 H1A 0.9500 . ? C2 C7 1.401(11) . ? C2 C3 1.441(13) . ? C3 O3 1.301(9) . ? C3 C4 1.415(11) . ? C4 C5 1.378(12) . ? C4 C8 1.553(14) . ? C5 C6 1.406(14) . ? C5 H5A 0.9500 . ? C6 C7 1.395(12) . ? C6 N6 1.460(11) . ? C7 H7A 0.9500 . ? C8 C11 1.522(16) . ? C8 C9 1.545(13) . ? C8 C10 1.552(14) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N6 O5 1.215(10) . ? N6 O6 1.252(11) . ? O12 C12 1.272(13) . ? O13 C12 1.251(13) . ? C12 C13 1.466(17) . ? C13 C14 1.327(17) . ? C13 C18 1.423(17) . ? C14 C15 1.40(2) . ? C14 H14A 0.9500 . ? C15 C16 1.32(3) . ? C15 H15A 0.9500 . ? C16 C17 1.41(2) . ? C16 H16A 0.9500 . ? C17 C18 1.39(2) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O19 C19 1.271(8) . ? O20 C19 1.267(10) . ? C19 C20 1.478(12) . ? C20 C21 1.363(12) . ? C20 C25 1.380(11) . ? C21 C22 1.392(13) . ? C21 H21A 0.9500 . ? C22 C23 1.383(12) . ? C22 H22A 0.9500 . ? C23 C24 1.351(14) . ? C23 H23A 0.9500 . ? C24 C25 1.379(14) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? O26 C26 1.289(10) . ? C26 O27 1.258(9) . ? C26 C27 1.455(13) . ? C27 C32 1.398(14) . ? C27 C28 1.400(13) . ? C28 C29 1.414(16) . ? C28 H28A 0.9500 . ? C29 C30 1.373(17) . ? C29 H29A 0.9500 . ? C30 C31 1.385(17) . ? C30 H30A 0.9500 . ? C31 C32 1.409(16) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? O33 C33 1.286(10) . ? O34 C33 1.249(10) . ? C33 C34 1.474(11) . ? C34 C35 1.364(12) . ? C34 C39 1.406(11) . ? C35 C36 1.383(13) . ? C35 H35A 0.9500 . ? C36 C37 1.343(15) . ? C36 H36A 0.9500 . ? C37 C38 1.369(15) . ? C37 H37A 0.9500 . ? C38 C39 1.389(11) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? O40 C40 1.258(11) . ? O41 C40 1.253(12) . ? C40 C41 1.453(16) . ? C41 C46 1.36(2) . ? C41 C42 1.40(2) . ? C42 C43 1.41(3) . ? C42 H42A 0.9500 . ? C43 C44 1.53(6) . ? C43 H43A 0.9500 . ? C44 C45 1.33(5) . ? C44 H44A 0.9500 . ? C45 C46 1.34(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? O60 H60A 0.97(2) . ? O60 H60B 0.98(2) . ? N47 C47 1.26(2) . ? C47 C48 1.22(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N49 C49 1.064(14) . ? C49 C50 1.497(18) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O50 169.1(2) . . ? O3 Fe1 O12 88.4(3) . . ? O50 Fe1 O12 91.9(2) . . ? O3 Fe1 O27 93.7(2) . . ? O50 Fe1 O27 97.2(2) . . ? O12 Fe1 O27 90.6(3) . . ? O3 Fe1 O20 88.3(2) . . ? O50 Fe1 O20 91.6(2) . . ? O12 Fe1 O20 176.5(2) . . ? O27 Fe1 O20 88.6(3) . . ? O3 Fe1 N1 84.5(2) . . ? O50 Fe1 N1 84.6(2) . . ? O12 Fe1 N1 91.2(3) . . ? O27 Fe1 N1 177.4(2) . . ? O20 Fe1 N1 89.5(3) . . ? O50 Fe2 O13 96.8(3) . . ? O50 Fe2 O40 96.8(3) . . ? O13 Fe2 O40 164.0(3) . . ? O50 Fe2 O33 95.9(2) . . ? O13 Fe2 O33 84.5(3) . . ? O40 Fe2 O33 86.0(3) . . ? O50 Fe2 O1 162.16(19) . 2_657 ? O13 Fe2 O1 84.5(3) . 2_657 ? O40 Fe2 O1 85.0(3) . 2_657 ? O33 Fe2 O1 101.9(2) . 2_657 ? O50 Fe2 O1 87.3(2) . . ? O13 Fe2 O1 94.2(2) . . ? O40 Fe2 O1 94.6(2) . . ? O33 Fe2 O1 176.6(2) . . ? O1 Fe2 O1 74.9(2) 2_657 . ? O50 Fe3 O34 95.3(2) . . ? O50 Fe3 O19 96.5(2) . . ? O34 Fe3 O19 168.1(2) . . ? O50 Fe3 O26 96.5(3) . . ? O34 Fe3 O26 90.4(3) . . ? O19 Fe3 O26 87.6(2) . . ? O50 Fe3 O41 94.5(3) . . ? O34 Fe3 O41 90.8(3) . . ? O19 Fe3 O41 89.0(3) . . ? O26 Fe3 O41 168.7(3) . . ? O50 Fe3 O60 178.5(3) . . ? O34 Fe3 O60 83.8(2) . . ? O19 Fe3 O60 84.4(2) . . ? O26 Fe3 O60 84.7(3) . . ? O41 Fe3 O60 84.3(3) . . ? N1 O1 Fe2 129.6(4) . 2_657 ? N1 O1 Fe2 114.8(4) . . ? Fe2 O1 Fe2 105.1(2) 2_657 . ? C1 N1 O1 115.7(7) . . ? C1 N1 Fe1 126.2(6) . . ? O1 N1 Fe1 117.6(4) . . ? N1 C1 C2 124.4(8) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C7 C2 C3 119.8(7) . . ? C7 C2 C1 116.2(9) . . ? C3 C2 C1 124.0(7) . . ? O3 C3 C4 119.6(9) . . ? O3 C3 C2 119.7(7) . . ? C4 C3 C2 120.6(7) . . ? C3 O3 Fe1 135.5(6) . . ? C5 C4 C3 118.3(10) . . ? C5 C4 C8 121.2(8) . . ? C3 C4 C8 120.3(8) . . ? C4 C5 C6 120.3(8) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 123.0(8) . . ? C7 C6 N6 118.1(10) . . ? C5 C6 N6 118.9(8) . . ? C6 C7 C2 117.5(9) . . ? C6 C7 H7A 121.3 . . ? C2 C7 H7A 121.3 . . ? C11 C8 C9 108.1(10) . . ? C11 C8 C10 113.2(9) . . ? C9 C8 C10 106.0(9) . . ? C11 C8 C4 107.5(8) . . ? C9 C8 C4 111.0(9) . . ? C10 C8 C4 111.0(9) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 N6 O6 122.7(8) . . ? O5 N6 C6 118.6(10) . . ? O6 N6 C6 118.7(8) . . ? C12 O12 Fe1 133.2(7) . . ? C12 O13 Fe2 130.5(7) . . ? O13 C12 O12 125.2(10) . . ? O13 C12 C13 119.4(11) . . ? O12 C12 C13 115.1(12) . . ? C14 C13 C18 117.9(14) . . ? C14 C13 C12 122.9(13) . . ? C18 C13 C12 119.0(12) . . ? C13 C14 C15 120.5(16) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 124(2) . . ? C16 C15 H15A 118.2 . . ? C14 C15 H15A 118.2 . . ? C15 C16 C17 117.6(19) . . ? C15 C16 H16A 121.2 . . ? C17 C16 H16A 121.2 . . ? C18 C17 C16 119.1(18) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C13 120.5(14) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C19 O19 Fe3 132.6(5) . . ? C19 O20 Fe1 132.4(5) . . ? O20 C19 O19 124.0(8) . . ? O20 C19 C20 118.4(6) . . ? O19 C19 C20 117.7(7) . . ? C21 C20 C25 118.2(8) . . ? C21 C20 C19 120.4(7) . . ? C25 C20 C19 121.4(8) . . ? C20 C21 C22 121.4(8) . . ? C20 C21 H21A 119.3 . . ? C22 C21 H21A 119.3 . . ? C23 C22 C21 119.1(9) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C24 C23 C22 120.0(9) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C20 121.0(9) . . ? C24 C25 H25A 119.5 . . ? C20 C25 H25A 119.5 . . ? C26 O26 Fe3 132.6(5) . . ? O27 C26 O26 122.0(9) . . ? O27 C26 C27 119.3(8) . . ? O26 C26 C27 118.7(7) . . ? C26 O27 Fe1 135.5(6) . . ? C32 C27 C28 119.3(10) . . ? C32 C27 C26 121.4(9) . . ? C28 C27 C26 119.3(9) . . ? C27 C28 C29 119.6(11) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C30 C29 C28 119.5(11) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C29 C30 C31 122.4(12) . . ? C29 C30 H30A 118.8 . . ? C31 C30 H30A 118.8 . . ? C30 C31 C32 118.0(12) . . ? C30 C31 H31A 121.0 . . ? C32 C31 H31A 121.0 . . ? C27 C32 C31 121.1(11) . . ? C27 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C33 O33 Fe2 131.8(6) . . ? C33 O34 Fe3 133.7(5) . . ? O34 C33 O33 123.4(7) . . ? O34 C33 C34 121.4(7) . . ? O33 C33 C34 115.1(8) . . ? C35 C34 C39 117.6(7) . . ? C35 C34 C33 123.7(8) . . ? C39 C34 C33 118.6(8) . . ? C34 C35 C36 121.7(9) . . ? C34 C35 H35A 119.1 . . ? C36 C35 H35A 119.1 . . ? C37 C36 C35 120.6(11) . . ? C37 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? C36 C37 C38 119.5(9) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C37 C38 C39 120.9(9) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C39 C34 119.5(9) . . ? C38 C39 H39A 120.3 . . ? C34 C39 H39A 120.3 . . ? C40 O40 Fe2 133.6(7) . . ? C40 O41 Fe3 132.9(7) . . ? O41 C40 O40 123.0(11) . . ? O41 C40 C41 116.1(10) . . ? O40 C40 C41 120.9(11) . . ? C46 C41 C42 121.0(14) . . ? C46 C41 C40 124.4(15) . . ? C42 C41 C40 114.6(15) . . ? C41 C42 C43 119(2) . . ? C41 C42 H42A 120.5 . . ? C43 C42 H42A 120.5 . . ? C42 C43 C44 113(3) . . ? C42 C43 H43A 123.5 . . ? C44 C43 H43A 123.5 . . ? C45 C44 C43 125(3) . . ? C45 C44 H44A 117.3 . . ? C43 C44 H44A 117.3 . . ? C44 C45 C46 115(3) . . ? C44 C45 H45A 122.5 . . ? C46 C45 H45A 122.5 . . ? C45 C46 C41 126(2) . . ? C45 C46 H46A 117.1 . . ? C41 C46 H46A 117.1 . . ? Fe2 O50 Fe3 122.0(3) . . ? Fe2 O50 Fe1 117.6(3) . . ? Fe3 O50 Fe1 120.4(3) . . ? Fe3 O60 H60A 120(7) . . ? Fe3 O60 H60B 99(7) . . ? H60A O60 H60B 127(10) . . ? C48 C47 N47 168(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N49 C49 C50 178.2(16) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O50 Fe2 O1 N1 31.3(5) . . . . ? O13 Fe2 O1 N1 -65.4(5) . . . . ? O40 Fe2 O1 N1 127.9(5) . . . . ? O1 Fe2 O1 N1 -148.5(6) 2_657 . . . ? O50 Fe2 O1 Fe2 179.8(3) . . . 2_657 ? O13 Fe2 O1 Fe2 83.1(3) . . . 2_657 ? O40 Fe2 O1 Fe2 -83.6(3) . . . 2_657 ? O1 Fe2 O1 Fe2 0.0 2_657 . . 2_657 ? Fe2 O1 N1 C1 36.7(10) 2_657 . . . ? Fe2 O1 N1 C1 175.8(6) . . . . ? Fe2 O1 N1 Fe1 -150.7(4) 2_657 . . . ? Fe2 O1 N1 Fe1 -11.6(7) . . . . ? O3 Fe1 N1 C1 -21.6(7) . . . . ? O50 Fe1 N1 C1 158.4(7) . . . . ? O12 Fe1 N1 C1 -109.8(7) . . . . ? O20 Fe1 N1 C1 66.7(7) . . . . ? O3 Fe1 N1 O1 166.7(6) . . . . ? O50 Fe1 N1 O1 -13.3(5) . . . . ? O12 Fe1 N1 O1 78.4(5) . . . . ? O20 Fe1 N1 O1 -105.0(5) . . . . ? O1 N1 C1 C2 -176.5(7) . . . . ? Fe1 N1 C1 C2 11.7(12) . . . . ? N1 C1 C2 C7 -175.2(8) . . . . ? N1 C1 C2 C3 6.3(14) . . . . ? C7 C2 C3 O3 176.3(8) . . . . ? C1 C2 C3 O3 -5.2(13) . . . . ? C7 C2 C3 C4 -6.8(13) . . . . ? C1 C2 C3 C4 171.7(8) . . . . ? C4 C3 O3 Fe1 165.1(6) . . . . ? C2 C3 O3 Fe1 -18.0(12) . . . . ? O50 Fe1 O3 C3 26.1(17) . . . . ? O12 Fe1 O3 C3 117.6(8) . . . . ? O27 Fe1 O3 C3 -151.9(8) . . . . ? O20 Fe1 O3 C3 -63.5(8) . . . . ? N1 Fe1 O3 C3 26.2(8) . . . . ? O3 C3 C4 C5 -175.1(8) . . . . ? C2 C3 C4 C5 8.0(13) . . . . ? O3 C3 C4 C8 0.2(13) . . . . ? C2 C3 C4 C8 -176.7(8) . . . . ? C3 C4 C5 C6 -4.1(14) . . . . ? C8 C4 C5 C6 -179.3(9) . . . . ? C4 C5 C6 C7 -1.2(14) . . . . ? C4 C5 C6 N6 179.9(8) . . . . ? C5 C6 C7 C2 2.5(14) . . . . ? N6 C6 C7 C2 -178.7(8) . . . . ? C3 C2 C7 C6 1.5(13) . . . . ? C1 C2 C7 C6 -177.1(8) . . . . ? C5 C4 C8 C11 -121.6(10) . . . . ? C3 C4 C8 C11 63.3(11) . . . . ? C5 C4 C8 C9 -3.5(14) . . . . ? C3 C4 C8 C9 -178.7(9) . . . . ? C5 C4 C8 C10 114.1(10) . . . . ? C3 C4 C8 C10 -61.1(12) . . . . ? C7 C6 N6 O5 -178.7(9) . . . . ? C5 C6 N6 O5 0.2(14) . . . . ? C7 C6 N6 O6 0.4(13) . . . . ? C5 C6 N6 O6 179.3(9) . . . . ? O3 Fe1 O12 C12 -143.0(9) . . . . ? O50 Fe1 O12 C12 26.0(9) . . . . ? O27 Fe1 O12 C12 123.3(9) . . . . ? N1 Fe1 O12 C12 -58.6(9) . . . . ? O50 Fe2 O13 C12 -15.1(8) . . . . ? O40 Fe2 O13 C12 -164.0(9) . . . . ? O33 Fe2 O13 C12 -110.5(8) . . . . ? O1 Fe2 O13 C12 147.0(8) 2_657 . . . ? O1 Fe2 O13 C12 72.7(8) . . . . ? Fe2 O13 C12 O12 -12.7(15) . . . . ? Fe2 O13 C12 C13 173.8(7) . . . . ? Fe1 O12 C12 O13 5.1(16) . . . . ? Fe1 O12 C12 C13 178.9(8) . . . . ? O13 C12 C13 C14 150.5(16) . . . . ? O12 C12 C13 C14 -24(2) . . . . ? O13 C12 C13 C18 -24.7(18) . . . . ? O12 C12 C13 C18 161.2(12) . . . . ? C18 C13 C14 C15 -1(3) . . . . ? C12 C13 C14 C15 -177(3) . . . . ? C13 C14 C15 C16 3(5) . . . . ? C14 C15 C16 C17 -8(6) . . . . ? C15 C16 C17 C18 10(4) . . . . ? C16 C17 C18 C13 -9(3) . . . . ? C14 C13 C18 C17 4(2) . . . . ? C12 C13 C18 C17 179.5(14) . . . . ? O50 Fe3 O19 C19 -12.3(8) . . . . ? O34 Fe3 O19 C19 164.3(11) . . . . ? O26 Fe3 O19 C19 84.0(8) . . . . ? O41 Fe3 O19 C19 -106.7(8) . . . . ? O60 Fe3 O19 C19 168.9(8) . . . . ? O3 Fe1 O20 C19 -152.3(8) . . . . ? O50 Fe1 O20 C19 38.6(8) . . . . ? O27 Fe1 O20 C19 -58.6(8) . . . . ? N1 Fe1 O20 C19 123.1(8) . . . . ? Fe1 O20 C19 O19 -14.6(14) . . . . ? Fe1 O20 C19 C20 165.7(6) . . . . ? Fe3 O19 C19 O20 -2.6(14) . . . . ? Fe3 O19 C19 C20 177.1(6) . . . . ? O20 C19 C20 C21 -175.6(8) . . . . ? O19 C19 C20 C21 4.7(13) . . . . ? O20 C19 C20 C25 4.5(14) . . . . ? O19 C19 C20 C25 -175.2(9) . . . . ? C25 C20 C21 C22 -2.1(15) . . . . ? C19 C20 C21 C22 178.0(9) . . . . ? C20 C21 C22 C23 1.9(16) . . . . ? C21 C22 C23 C24 -0.5(18) . . . . ? C22 C23 C24 C25 -0.6(19) . . . . ? C23 C24 C25 C20 0(2) . . . . ? C21 C20 C25 C24 1.0(17) . . . . ? C19 C20 C25 C24 -179.1(10) . . . . ? O50 Fe3 O26 C26 31.2(8) . . . . ? O34 Fe3 O26 C26 126.6(7) . . . . ? O19 Fe3 O26 C26 -65.1(7) . . . . ? O41 Fe3 O26 C26 -137.2(11) . . . . ? O60 Fe3 O26 C26 -149.7(8) . . . . ? Fe3 O26 C26 O27 -6.7(13) . . . . ? Fe3 O26 C26 C27 170.9(6) . . . . ? O26 C26 O27 Fe1 -7.9(14) . . . . ? C27 C26 O27 Fe1 174.5(7) . . . . ? O3 Fe1 O27 C26 172.7(9) . . . . ? O50 Fe1 O27 C26 -6.9(9) . . . . ? O12 Fe1 O27 C26 -98.9(9) . . . . ? O20 Fe1 O27 C26 84.5(9) . . . . ? O27 C26 C27 C32 -2.4(14) . . . . ? O26 C26 C27 C32 179.9(9) . . . . ? O27 C26 C27 C28 179.4(10) . . . . ? O26 C26 C27 C28 1.6(14) . . . . ? C32 C27 C28 C29 2.6(18) . . . . ? C26 C27 C28 C29 -179.1(11) . . . . ? C27 C28 C29 C30 -3(2) . . . . ? C28 C29 C30 C31 2(2) . . . . ? C29 C30 C31 C32 -2(2) . . . . ? C28 C27 C32 C31 -2.3(17) . . . . ? C26 C27 C32 C31 179.4(11) . . . . ? C30 C31 C32 C27 2(2) . . . . ? O50 Fe2 O33 C33 15.5(8) . . . . ? O13 Fe2 O33 C33 111.8(8) . . . . ? O40 Fe2 O33 C33 -81.0(8) . . . . ? O1 Fe2 O33 C33 -165.0(8) 2_657 . . . ? O50 Fe3 O34 C33 -17.2(9) . . . . ? O19 Fe3 O34 C33 166.2(11) . . . . ? O26 Fe3 O34 C33 -113.8(8) . . . . ? O41 Fe3 O34 C33 77.4(9) . . . . ? O60 Fe3 O34 C33 161.7(9) . . . . ? Fe3 O34 C33 O33 -8.7(14) . . . . ? Fe3 O34 C33 C34 174.0(6) . . . . ? Fe2 O33 C33 O34 9.8(14) . . . . ? Fe2 O33 C33 C34 -172.8(6) . . . . ? O34 C33 C34 C35 -174.0(9) . . . . ? O33 C33 C34 C35 8.5(14) . . . . ? O34 C33 C34 C39 6.7(13) . . . . ? O33 C33 C34 C39 -170.8(8) . . . . ? C39 C34 C35 C36 -0.7(16) . . . . ? C33 C34 C35 C36 -179.9(10) . . . . ? C34 C35 C36 C37 1.4(19) . . . . ? C35 C36 C37 C38 -2.7(19) . . . . ? C36 C37 C38 C39 3.5(19) . . . . ? C37 C38 C39 C34 -2.8(16) . . . . ? C35 C34 C39 C38 1.4(14) . . . . ? C33 C34 C39 C38 -179.3(9) . . . . ? O50 Fe2 O40 C40 -16.2(8) . . . . ? O13 Fe2 O40 C40 132.7(10) . . . . ? O33 Fe2 O40 C40 79.3(8) . . . . ? O1 Fe2 O40 C40 -178.4(8) 2_657 . . . ? O1 Fe2 O40 C40 -104.0(8) . . . . ? O50 Fe3 O41 C40 31.1(7) . . . . ? O34 Fe3 O41 C40 -64.3(7) . . . . ? O19 Fe3 O41 C40 127.6(7) . . . . ? O26 Fe3 O41 C40 -160.5(10) . . . . ? O60 Fe3 O41 C40 -147.9(7) . . . . ? Fe3 O41 C40 O40 -11.5(13) . . . . ? Fe3 O41 C40 C41 166.6(8) . . . . ? Fe2 O40 C40 O41 2.2(13) . . . . ? Fe2 O40 C40 C41 -175.8(8) . . . . ? O41 C40 C41 C46 19.1(19) . . . . ? O40 C40 C41 C46 -162.7(13) . . . . ? O41 C40 C41 C42 -158.8(12) . . . . ? O40 C40 C41 C42 19.4(17) . . . . ? C46 C41 C42 C43 -3(3) . . . . ? C40 C41 C42 C43 175(2) . . . . ? C41 C42 C43 C44 9(4) . . . . ? C42 C43 C44 C45 -12(6) . . . . ? C43 C44 C45 C46 8(6) . . . . ? C44 C45 C46 C41 0(5) . . . . ? C42 C41 C46 C45 -2(3) . . . . ? C40 C41 C46 C45 180(2) . . . . ? O13 Fe2 O50 Fe3 -130.1(3) . . . . ? O40 Fe2 O50 Fe3 41.7(3) . . . . ? O33 Fe2 O50 Fe3 -44.9(4) . . . . ? O1 Fe2 O50 Fe3 136.7(7) 2_657 . . . ? O1 Fe2 O50 Fe3 136.0(3) . . . . ? O13 Fe2 O50 Fe1 50.2(3) . . . . ? O40 Fe2 O50 Fe1 -138.1(3) . . . . ? O33 Fe2 O50 Fe1 135.3(3) . . . . ? O1 Fe2 O50 Fe1 -43.0(10) 2_657 . . . ? O1 Fe2 O50 Fe1 -43.7(3) . . . . ? O34 Fe3 O50 Fe2 45.4(4) . . . . ? O19 Fe3 O50 Fe2 -135.2(3) . . . . ? O26 Fe3 O50 Fe2 136.5(3) . . . . ? O41 Fe3 O50 Fe2 -45.8(3) . . . . ? O34 Fe3 O50 Fe1 -134.8(3) . . . . ? O19 Fe3 O50 Fe1 44.5(4) . . . . ? O26 Fe3 O50 Fe1 -43.8(3) . . . . ? O41 Fe3 O50 Fe1 133.9(3) . . . . ? O3 Fe1 O50 Fe2 38.5(14) . . . . ? O12 Fe1 O50 Fe2 -52.6(3) . . . . ? O27 Fe1 O50 Fe2 -143.5(3) . . . . ? O20 Fe1 O50 Fe2 127.8(3) . . . . ? N1 Fe1 O50 Fe2 38.4(3) . . . . ? O3 Fe1 O50 Fe3 -141.2(11) . . . . ? O12 Fe1 O50 Fe3 127.6(3) . . . . ? O27 Fe1 O50 Fe3 36.8(4) . . . . ? O20 Fe1 O50 Fe3 -52.0(3) . . . . ? N1 Fe1 O50 Fe3 -141.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O60 H60A N47 0.97(2) 1.97(4) 2.92(2) 168(10) 2_666 O60 H60B O6 0.98(2) 2.01(8) 2.803(8) 136(9) 1_565 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.628 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.091 # Attachment 'Complex 7.cif' data_eb8177 _database_code_depnum_ccdc_archive 'CCDC 755041' #TrackingRef 'Complex 7.cif' _audit_creation_date 08-12-02 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'eb8177 in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _exptl_crystal_recrystallization_method ; Slow evaporation of MeCN solution ; _publ_section_exptl_refinement ; The hydrogen atoms were placed geometrically and constrained to ride on their host atoms. 910_ALERT_3_A # Missing FCF Reflections Below Th(Min) ........ 47 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 12 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 35 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 37 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.992 5795 5748 47 23.01 0.550 0.994 7719 7672 47 25.24 0.600 0.994 10006 9947 59 #----------------------------------------------------------- ACTA Min. Res. --- 26.40 0.626 0.992 11359 11265 94 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.31 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.67 Ratio 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.68 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O133 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O143 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C26 Some of the groups attached to the ligands have more freedom of motion than others in one direction. See principal axes of thermal ellipsoids below. O133 0.0110 0.0165 0.0789 O143 0.0141 0.0218 0.0640 C26 0.0158 0.0264 0.0889 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The moiety formula given is intended to be more chemically significant. 302_ALERT_4_C Anion/Solvent Disorder ......................... 17.00 Perc. One of the MeCN solvent molecules is partially occupied. 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 18 Noted, no action taken. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 138 VIBRATION 0.0, 0.010000 = C(123) TO C(113) U(IJ)'S 0.0, 0.005000 = C(123) TO C(113) DISTANCE 1.500000 , 0.020000 = C(123) TO C(113) VIBRATION 0.0, 0.010000 = N(113) TO C(113) U(IJ)'S 0.0, 0.005000 = N(113) TO C(113) U(IJ)'S 0.0, 0.010000 = C(35) TO C(85) U(IJ)'S 0.0, 0.010000 = C(85) TO C(75) U(IJ)'S 0.0, 0.005000 = C(65) TO C(75) U(IJ)'S 0.0, 0.005000 = C(65) TO C(55) U(IJ)'S 0.0, 0.010000 = C(55) TO C(45) U(IJ)'S 0.0, 0.010000 = C(35) TO C(45) U(IJ)'S 0.0, 0.010000 = C(33) TO C(43) U(IJ)'S 0.0, 0.010000 = C(43) TO C(53) U(IJ)'S 0.0, 0.005000 = C(63) TO C(53) U(IJ)'S 0.0, 0.010000 = C(63) TO C(73) U(IJ)'S 0.0, 0.005000 = C(73) TO C(83) U(IJ)'S 0.0, 0.010000 = C(33) TO C(83) U(IJ)'S 0.0, 0.010000 = N(112) TO C(112) U(IJ)'S 0.0, 0.010000 = O(133) TO C(13) U(IJ)'S 0.0, 0.010000 = C(610) TO C(612) U(IJ)'S 0.0, 0.010000 = C(16) TO C(26) VIBRATION 0.0, 0.020000 = C(35) TO C(45) VIBRATION 0.0, 0.020000 = C(55) TO C(45) VIBRATION 0.0, 0.020000 = C(65) TO C(55) VIBRATION 0.0, 0.020000 = C(65) TO C(75) VIBRATION 0.0, 0.020000 = C(85) TO C(75) VIBRATION 0.0, 0.020000 = C(35) TO C(85) U(IJ)'S 0.0, 0.010000 = C(26) TO C(36) VIBRATION 0.0, 0.020000 = C(26) TO C(36) U(IJ)'S 0.0, 0.010000 = FE(3) TO O(143) VIBRATION 0.0, 0.020000 = FE(3) TO O(143) U(IJ)'S 0.0, 0.010000 = FE(3) TO O(133) VIBRATION 0.0, 0.020000 = FE(3) TO O(133) ; #end of refcif _cell_length_a 13.8956(6) _cell_length_b 18.6592(8) _cell_length_c 21.4730(9) _cell_angle_alpha 90 _cell_angle_beta 96.520(2) _cell_angle_gamma 90 _cell_volume 5531.5(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C112 H115 Fe6 N7 O28 # Dc = 1.41 Fooo = 2432.00 Mu = 8.44 M = 1171.13 # Found Formula = C112 H115 Fe6 N7 O28 # Dc = 1.41 FOOO = 2432.00 Mu = 8.44 M = 1171.13 _chemical_formula_sum 'C112 H115 Fe6 N7 O28' _chemical_formula_moiety '[Fe6O2(C8H7O2)10(C12H13O2N)2(H2O)2]5(CH3CN)' _chemical_compound_source 'Kevin Mason, KM148' _chemical_formula_weight 2342.26 _cell_measurement_reflns_used 1023 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.844 # Sheldrick geometric approximatio 0.87 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 44591 _reflns_number_total 11310 _diffrn_reflns_av_R_equivalents 0.065 # Number of reflections with Friedels Law is 11310 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11351 _diffrn_reflns_theta_min 1.835 _diffrn_reflns_theta_max 26.404 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.404 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.70 _oxford_diffrn_Wilson_scale 420.07 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.24 _refine_diff_density_max 1.25 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 11265 _refine_ls_number_restraints 138 _refine_ls_number_parameters 703 _oxford_refine_ls_R_factor_ref 0.1178 _refine_ls_wR_factor_ref 0.1936 _refine_ls_goodness_of_fit_ref 1.1351 _refine_ls_shift/su_max 0.000749 # The values computed from all data _oxford_reflns_number_all 11265 _refine_ls_R_factor_all 0.1178 _refine_ls_wR_factor_all 0.1936 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8893 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_gt 0.1856 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +32.70P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.38144(5) 0.50929(4) 0.49172(3) 0.0116 1.0000 Uani . . . . . . . Fe2 Fe 0.34361(6) 0.51281(4) 0.63969(3) 0.0126 1.0000 Uani . . . . . . . Fe3 Fe 0.17670(5) 0.44891(4) 0.52995(4) 0.0123 1.0000 Uani . U . . . . . O1 O 0.2982(3) 0.4896(2) 0.55220(16) 0.0133 1.0000 Uani . . . . . . . O11 O 0.4960(3) 0.4776(2) 0.55364(16) 0.0138 1.0000 Uani . . . . . . . O17 O 0.0413(3) 0.4029(2) 0.50348(19) 0.0210 1.0000 Uani . . . . . . . O71 O 0.4045(3) 0.5185(2) 0.72293(16) 0.0163 1.0000 Uani . . . . . . . O121 O 0.4001(3) 0.6141(2) 0.51541(17) 0.0173 1.0000 Uani . . . . . . . O122 O 0.3809(3) 0.6144(2) 0.61775(17) 0.0180 1.0000 Uani . . . . . . . O132 O 0.2169(3) 0.5554(2) 0.65838(19) 0.0263 1.0000 Uani . . . . . . . O133 O 0.1055(3) 0.5127(3) 0.5862(2) 0.0355 1.0000 Uani . U . . . . . O142 O 0.3024(3) 0.4121(2) 0.66544(19) 0.0279 1.0000 Uani . . . . . . . O143 O 0.1876(3) 0.3718(3) 0.5944(2) 0.0333 1.0000 Uani . U . . . . . O151 O 0.3683(3) 0.4141(2) 0.44717(17) 0.0181 1.0000 Uani . . . . . . . O153 O 0.2204(3) 0.3801(2) 0.4666(2) 0.0263 1.0000 Uani . . . . . . . O161 O 0.2750(3) 0.5486(2) 0.42615(17) 0.0210 1.0000 Uani . . . . . . . O163 O 0.1353(3) 0.5237(2) 0.4639(2) 0.0284 1.0000 Uani . . . . . . . N11 N 0.4810(3) 0.4790(2) 0.6168(2) 0.0137 1.0000 Uani . . . . . . . N111 N 0.0145(6) 0.2662(4) 0.5608(4) 0.0604 1.0000 Uani . . . . . . . N112 N 0.5693(6) 0.8234(4) 0.4577(4) 0.0616 1.0000 Uani . U . . . . . N113 N 0.9190(13) 0.9507(9) 0.4433(7) 0.0640 0.5000 Uani . U . 1 1 . . C11 C 0.5523(4) 0.4569(3) 0.6557(3) 0.0161 1.0000 Uani . . . . . . . C12 C 0.3977(4) 0.6444(3) 0.5674(3) 0.0177 1.0000 Uani . . . . . . . C13 C 0.1336(4) 0.5536(3) 0.6306(3) 0.0186 1.0000 Uani . U . . . . . C14 C 0.2375(4) 0.3686(3) 0.6466(3) 0.0181 1.0000 Uani . . . . . . . C15 C 0.2975(4) 0.3713(3) 0.4423(3) 0.0188 1.0000 Uani . . . . . . . C16 C 0.1855(4) 0.5571(4) 0.4277(3) 0.0242 1.0000 Uani . U . . . . . C21 C 0.5489(4) 0.4515(3) 0.7229(3) 0.0179 1.0000 Uani . . . . . . . C22 C 0.4138(5) 0.7244(3) 0.5696(3) 0.0211 1.0000 Uani . . . . . . . C23 C 0.0591(5) 0.6042(4) 0.6539(3) 0.0263 1.0000 Uani . . . . . . . C24 C 0.2168(5) 0.3087(4) 0.6900(3) 0.0275 1.0000 Uani . . . . . . . C25 C 0.3088(5) 0.3047(4) 0.4034(3) 0.0332 1.0000 Uani . . . . . . . C26 C 0.1296(5) 0.6109(4) 0.3862(4) 0.0437 1.0000 Uani . U . . . . . C31 C 0.6264(4) 0.4152(3) 0.7566(3) 0.0233 1.0000 Uani . . . . . . . C32 C 0.3205(5) 0.7648(3) 0.5530(3) 0.0241 1.0000 Uani . . . . . . . C33 C 0.0011(5) 0.5668(4) 0.6987(3) 0.0352 1.0000 Uani . U . . . . . C34 C 0.3023(5) 0.2604(3) 0.7103(3) 0.0240 1.0000 Uani . . . . . . . C35 C 0.2209(5) 0.2582(4) 0.3916(3) 0.0332 1.0000 Uani . U . . . . . C36 C 0.1823(5) 0.6605(4) 0.3467(3) 0.0300 1.0000 Uani . U . . . . . C41 C 0.6279(5) 0.4041(4) 0.8194(3) 0.0304 1.0000 Uani . . . . . . . C42 C 0.2359(5) 0.7441(4) 0.5754(3) 0.0322 1.0000 Uani . . . . . . . C43 C 0.0433(7) 0.5363(5) 0.7523(4) 0.0470 1.0000 Uani . U . . . . . C44 C 0.3870(5) 0.2865(3) 0.7419(3) 0.0266 1.0000 Uani . . . . . . . C45 C 0.1944(6) 0.2111(5) 0.4346(5) 0.0549 1.0000 Uani . U . . . . . C46 C 0.1454(5) 0.6708(4) 0.2851(3) 0.0312 1.0000 Uani . . . . . . . C51 C 0.5512(5) 0.4296(4) 0.8500(3) 0.0309 1.0000 Uani . . . . . . . C52 C 0.1523(6) 0.7827(4) 0.5619(4) 0.0451 1.0000 Uani . . . . . . . C53 C -0.0127(8) 0.5035(5) 0.7952(5) 0.0652 1.0000 Uani . U . . . . . C54 C 0.4635(5) 0.2416(4) 0.7608(3) 0.0346 1.0000 Uani . . . . . . . C55 C 0.1107(7) 0.1684(5) 0.4207(5) 0.0635 1.0000 Uani . U . . . . . C56 C 0.1872(5) 0.7199(4) 0.2475(3) 0.0312 1.0000 Uani . . . . . . . C61 C 0.4736(4) 0.4677(3) 0.8196(3) 0.0212 1.0000 Uani . . . . . . . C62 C 0.1516(6) 0.8437(4) 0.5258(4) 0.0492 1.0000 Uani . . . . . . . C63 C -0.1103(8) 0.5022(6) 0.7816(5) 0.0675 1.0000 Uani . U . . . . . C64 C 0.4557(6) 0.1691(4) 0.7497(3) 0.0402 1.0000 Uani . . . . . . . C65 C 0.0581(7) 0.1749(5) 0.3642(5) 0.0603 1.0000 Uani . U . . . . . C66 C 0.2664(5) 0.7584(4) 0.2715(4) 0.0397 1.0000 Uani . . . . . . . C71 C 0.4735(4) 0.4800(3) 0.7544(3) 0.0162 1.0000 Uani . . . . . . . C72 C 0.2348(6) 0.8644(4) 0.5018(4) 0.0443 1.0000 Uani . . . . . . . C73 C -0.1532(7) 0.5300(6) 0.7281(5) 0.0688 1.0000 Uani . U . . . . . C74 C 0.3716(6) 0.1426(4) 0.7187(4) 0.0453 1.0000 Uani . . . . . . . C75 C 0.0814(7) 0.2222(5) 0.3211(5) 0.0613 1.0000 Uani . U . . . . . C76 C 0.3037(6) 0.7484(4) 0.3332(4) 0.0477 1.0000 Uani . . . . . . . C82 C 0.3195(5) 0.8257(4) 0.5152(3) 0.0328 1.0000 Uani . . . . . . . C83 C -0.0991(6) 0.5624(5) 0.6859(5) 0.0586 1.0000 Uani . U . . . . . C84 C 0.2957(6) 0.1875(4) 0.6987(3) 0.0363 1.0000 Uani . . . . . . . C85 C 0.1632(6) 0.2629(5) 0.3344(4) 0.0518 1.0000 Uani . U . . . . . C86 C 0.2615(5) 0.6997(4) 0.3712(3) 0.0323 1.0000 Uani . . . . . . . C111 C -0.0111(7) 0.2243(5) 0.5946(5) 0.0558 1.0000 Uani . . . . . . . C112 C 0.5606(6) 0.7668(4) 0.4386(4) 0.0392 1.0000 Uani . U . . . . . C113 C 0.8400(13) 0.9475(10) 0.4388(7) 0.0545 0.5000 Uani D U . . . . . C121 C -0.0419(9) 0.1708(5) 0.6376(5) 0.0767 1.0000 Uani . . . . . . . C122 C 0.5490(6) 0.6951(4) 0.4167(4) 0.0446 1.0000 Uani . . . . . . . C123 C 0.7366(12) 0.9523(9) 0.4299(7) 0.0507 0.5000 Uani D U . . . . . C610 C 0.3890(5) 0.4932(4) 0.8544(3) 0.0301 1.0000 Uani . U . . . . . C611 C 0.2959(5) 0.4542(4) 0.8282(4) 0.0396 1.0000 Uani . . . . . . . C612 C 0.4075(6) 0.4767(5) 0.9247(3) 0.0456 1.0000 Uani . U . . . . . C613 C 0.3743(6) 0.5735(4) 0.8477(3) 0.0384 1.0000 Uani . . . . . . . H111 H 0.6093 0.4441 0.6397 0.0178 1.0000 Uiso R . . . . . . H222 H 0.4402 0.7398 0.6111 0.0228 1.0000 Uiso R . . . . . . H221 H 0.4581 0.7383 0.5397 0.0228 1.0000 Uiso R . . . . . . H231 H 0.0927 0.6453 0.6745 0.0300 1.0000 Uiso R . . . . . . H232 H 0.0161 0.6194 0.6179 0.0299 1.0000 Uiso R . . . . . . H241 H 0.1938 0.3299 0.7269 0.0320 1.0000 Uiso R . . . . . . H242 H 0.1655 0.2790 0.6692 0.0317 1.0000 Uiso R . . . . . . H252 H 0.3599 0.2774 0.4252 0.0379 1.0000 Uiso R . . . . . . H251 H 0.3267 0.3202 0.3637 0.0376 1.0000 Uiso R . . . . . . H261 H 0.0994 0.6417 0.4141 0.0540 1.0000 Uiso R . . . . . . H262 H 0.0810 0.5854 0.3592 0.0542 1.0000 Uiso R . . . . . . H311 H 0.6777 0.3990 0.7354 0.0261 1.0000 Uiso R . . . . . . H411 H 0.6803 0.3813 0.8419 0.0350 1.0000 Uiso R . . . . . . H421 H 0.2351 0.7031 0.6008 0.0369 1.0000 Uiso R . . . . . . H431 H 0.1098 0.5381 0.7616 0.0538 1.0000 Uiso R . . . . . . H441 H 0.3932 0.3352 0.7506 0.0298 1.0000 Uiso R . . . . . . H451 H 0.2302 0.2073 0.4735 0.0648 1.0000 Uiso R . . . . . . H461 H 0.0910 0.6449 0.2690 0.0351 1.0000 Uiso R . . . . . . H511 H 0.5522 0.4208 0.8923 0.0358 1.0000 Uiso R . . . . . . H521 H 0.0956 0.7659 0.5760 0.0552 1.0000 Uiso R . . . . . . H531 H 0.0163 0.4846 0.8327 0.0771 1.0000 Uiso R . . . . . . H541 H 0.5206 0.2614 0.7810 0.0398 1.0000 Uiso R . . . . . . H551 H 0.0928 0.1367 0.4504 0.0761 1.0000 Uiso R . . . . . . H561 H 0.1609 0.7277 0.2060 0.0361 1.0000 Uiso R . . . . . . H621 H 0.0956 0.8718 0.5173 0.0590 1.0000 Uiso R . . . . . . H631 H -0.1482 0.4801 0.8098 0.0821 1.0000 Uiso R . . . . . . H641 H 0.5060 0.1378 0.7630 0.0460 1.0000 Uiso R . . . . . . H651 H 0.0050 0.1458 0.3547 0.0710 1.0000 Uiso R . . . . . . H661 H 0.2946 0.7909 0.2464 0.0479 1.0000 Uiso R . . . . . . H721 H 0.2339 0.9053 0.4766 0.0501 1.0000 Uiso R . . . . . . H731 H -0.2202 0.5287 0.7193 0.0832 1.0000 Uiso R . . . . . . H741 H 0.3659 0.0947 0.7114 0.0530 1.0000 Uiso R . . . . . . H751 H 0.0413 0.2270 0.2830 0.0733 1.0000 Uiso R . . . . . . H761 H 0.3569 0.7745 0.3496 0.0531 1.0000 Uiso R . . . . . . H821 H 0.3758 0.8385 0.4989 0.0377 1.0000 Uiso R . . . . . . H831 H -0.1289 0.5797 0.6483 0.0701 1.0000 Uiso R . . . . . . H841 H 0.2390 0.1690 0.6763 0.0418 1.0000 Uiso R . . . . . . H851 H 0.1820 0.2944 0.3044 0.0611 1.0000 Uiso R . . . . . . H861 H 0.2872 0.6931 0.4126 0.0383 1.0000 Uiso R . . . . . . H6112 H 0.2432 0.4712 0.8488 0.0580 1.0000 Uiso R . . . . . . H6111 H 0.3037 0.4034 0.8355 0.0576 1.0000 Uiso R . . . . . . H6113 H 0.2825 0.4619 0.7841 0.0579 1.0000 Uiso R . . . . . . H6122 H 0.3538 0.4944 0.9448 0.0690 1.0000 Uiso R . . . . . . H6121 H 0.4651 0.5010 0.9428 0.0690 1.0000 Uiso R . . . . . . H6123 H 0.4128 0.4256 0.9322 0.0688 1.0000 Uiso R . . . . . . H6132 H 0.3258 0.5884 0.8726 0.0560 1.0000 Uiso R . . . . . . H6131 H 0.4343 0.5966 0.8628 0.0557 1.0000 Uiso R . . . . . . H6133 H 0.3565 0.5858 0.8049 0.0559 1.0000 Uiso R . . . . . . H172 H 0.0380 0.3624 0.5164 0.0302 1.0000 Uiso R . . . . . . H171 H -0.0042 0.4297 0.5051 0.0301 1.0000 Uiso R . . . . . . H1221 H 0.5733 0.6908 0.3773 0.0549 1.0000 Uiso R . . . . . . H1222 H 0.5834 0.6633 0.4459 0.0549 1.0000 Uiso R . . . . . . H1223 H 0.4822 0.6831 0.4123 0.0549 1.0000 Uiso R . . . . . . H1231 H 0.7095 0.9077 0.4403 0.0627 0.5000 Uiso R . . . . . . H1232 H 0.7158 0.9888 0.4563 0.0627 0.5000 Uiso R . . . . . . H1233 H 0.7157 0.9636 0.3874 0.0627 0.5000 Uiso R . . . . . . H1211 H -0.1112 0.1656 0.6323 0.0939 1.0000 Uiso R . . . . . . H1212 H -0.0240 0.1855 0.6807 0.0939 1.0000 Uiso R . . . . . . H1213 H -0.0133 0.1258 0.6317 0.0939 1.0000 Uiso 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 Fe1 0.0077(4) 0.0156(4) 0.0109(4) 0.0024(3) -0.0007(3) 0.0004(3) Fe2 0.0115(4) 0.0158(4) 0.0103(4) 0.0022(3) -0.0002(3) 0.0006(3) Fe3 0.0071(4) 0.0157(4) 0.0138(4) -0.0004(3) -0.0002(3) 0.0000(3) O1 0.0086(19) 0.019(2) 0.0121(17) 0.0006(15) 0.0002(14) -0.0010(15) O11 0.0108(19) 0.023(2) 0.0072(17) 0.0043(15) -0.0018(14) 0.0010(15) O17 0.011(2) 0.022(2) 0.030(2) -0.0010(18) -0.0002(16) -0.0021(17) O71 0.018(2) 0.019(2) 0.0110(18) 0.0008(15) -0.0006(15) 0.0010(16) O121 0.018(2) 0.017(2) 0.0156(19) -0.0005(16) 0.0000(15) -0.0016(16) O122 0.024(2) 0.015(2) 0.0145(19) 0.0029(15) 0.0012(16) -0.0004(17) O132 0.016(2) 0.043(3) 0.021(2) -0.0057(19) 0.0038(17) 0.010(2) O133 0.015(2) 0.055(3) 0.037(2) -0.032(2) 0.0043(18) 0.001(2) O142 0.032(3) 0.027(2) 0.022(2) 0.0142(18) -0.0084(19) -0.012(2) O143 0.035(3) 0.036(3) 0.026(2) 0.016(2) -0.008(2) -0.015(2) O151 0.014(2) 0.024(2) 0.0162(19) -0.0050(16) 0.0015(15) -0.0041(17) O153 0.020(2) 0.029(2) 0.032(2) -0.0174(19) 0.0127(19) -0.0079(19) O161 0.015(2) 0.033(2) 0.0139(19) 0.0063(17) -0.0057(15) 0.0062(18) O163 0.013(2) 0.038(3) 0.033(2) 0.020(2) -0.0053(18) -0.0012(19) N11 0.011(2) 0.014(2) 0.016(2) 0.0038(18) -0.0009(17) -0.0029(18) N111 0.069(6) 0.039(4) 0.070(5) 0.005(4) -0.002(4) -0.015(4) N112 0.079(5) 0.051(4) 0.055(4) 0.002(4) 0.009(4) -0.015(4) N113 0.088(8) 0.070(7) 0.039(5) 0.013(5) 0.030(7) 0.025(8) C11 0.014(3) 0.010(3) 0.025(3) 0.001(2) 0.006(2) -0.005(2) C12 0.010(3) 0.023(3) 0.018(3) 0.002(2) -0.006(2) -0.001(2) C13 0.010(3) 0.022(3) 0.023(3) -0.002(2) 0.002(2) 0.005(2) C14 0.017(3) 0.019(3) 0.020(3) 0.005(2) 0.007(2) 0.003(2) C15 0.017(3) 0.023(3) 0.016(3) -0.008(2) -0.005(2) 0.001(2) C16 0.010(3) 0.036(4) 0.025(3) 0.010(3) -0.005(2) 0.004(3) C21 0.016(3) 0.020(3) 0.016(3) 0.003(2) -0.001(2) -0.005(2) C22 0.027(3) 0.019(3) 0.016(3) -0.001(2) -0.001(2) -0.007(2) C23 0.024(4) 0.031(4) 0.024(3) -0.004(3) 0.003(3) 0.011(3) C24 0.020(3) 0.031(4) 0.031(3) 0.014(3) 0.001(3) -0.005(3) C25 0.022(4) 0.034(4) 0.045(4) -0.020(3) 0.011(3) -0.002(3) C26 0.026(3) 0.056(4) 0.050(4) 0.035(3) 0.007(3) 0.012(3) C31 0.014(3) 0.029(3) 0.026(3) 0.001(3) -0.001(2) 0.004(3) C32 0.035(4) 0.020(3) 0.018(3) -0.008(2) 0.004(3) -0.005(3) C33 0.025(3) 0.049(4) 0.033(3) -0.014(3) 0.010(3) 0.006(3) C34 0.028(4) 0.021(3) 0.022(3) 0.009(2) 0.001(3) 0.000(3) C35 0.021(3) 0.038(4) 0.043(4) -0.026(3) 0.016(3) -0.005(3) C36 0.021(3) 0.036(4) 0.034(3) 0.014(3) 0.006(3) 0.009(3) C41 0.025(4) 0.043(4) 0.022(3) 0.014(3) -0.002(3) 0.013(3) C42 0.039(4) 0.028(4) 0.031(4) 0.002(3) 0.012(3) 0.004(3) C43 0.048(4) 0.053(4) 0.042(4) -0.004(3) 0.014(3) -0.001(4) C44 0.038(4) 0.022(3) 0.019(3) 0.010(2) 0.002(3) 0.003(3) C45 0.042(4) 0.052(4) 0.070(5) -0.001(4) 0.005(4) -0.009(4) C46 0.024(4) 0.026(4) 0.042(4) 0.016(3) -0.006(3) 0.004(3) C51 0.040(4) 0.041(4) 0.010(3) 0.011(3) -0.002(3) 0.000(3) C52 0.038(5) 0.044(5) 0.056(5) 0.007(4) 0.016(4) 0.009(4) C53 0.077(5) 0.063(4) 0.061(4) -0.001(4) 0.027(4) -0.008(4) C54 0.032(4) 0.048(5) 0.023(3) 0.014(3) 0.000(3) 0.004(3) C55 0.047(4) 0.059(4) 0.086(5) -0.009(4) 0.013(4) -0.014(3) C56 0.035(4) 0.033(4) 0.025(3) 0.010(3) -0.001(3) 0.012(3) C61 0.023(3) 0.025(3) 0.016(3) 0.001(2) 0.002(2) 0.000(2) C62 0.042(5) 0.041(5) 0.065(6) 0.007(4) 0.006(4) 0.018(4) C63 0.072(5) 0.071(5) 0.068(4) -0.011(4) 0.040(4) -0.012(4) C64 0.043(5) 0.043(5) 0.035(4) 0.012(3) 0.005(3) 0.018(4) C65 0.042(4) 0.061(4) 0.079(4) -0.031(3) 0.010(3) -0.014(3) C66 0.034(4) 0.037(4) 0.049(5) 0.022(3) 0.005(3) -0.001(3) C71 0.014(3) 0.015(3) 0.020(3) 0.001(2) 0.001(2) -0.004(2) C72 0.056(5) 0.028(4) 0.050(5) 0.013(3) 0.012(4) 0.010(4) C73 0.044(4) 0.087(5) 0.079(5) -0.022(4) 0.024(4) -0.008(4) C74 0.057(6) 0.022(4) 0.056(5) 0.003(3) 0.003(4) 0.005(4) C75 0.042(4) 0.074(4) 0.068(4) -0.036(4) 0.008(3) -0.015(3) C76 0.048(5) 0.023(4) 0.068(6) 0.008(4) -0.017(4) -0.006(3) C82 0.038(4) 0.028(4) 0.033(4) 0.001(3) 0.004(3) -0.004(3) C83 0.037(4) 0.082(5) 0.060(4) -0.027(4) 0.020(3) -0.002(4) C84 0.040(4) 0.027(4) 0.042(4) 0.002(3) 0.002(3) -0.001(3) C85 0.039(4) 0.073(5) 0.045(4) -0.026(4) 0.013(3) -0.014(4) C86 0.043(4) 0.026(4) 0.026(3) 0.006(3) -0.001(3) 0.009(3) C111 0.061(6) 0.038(5) 0.069(6) 0.000(4) 0.007(5) 0.000(4) C112 0.047(4) 0.036(4) 0.036(4) 0.004(3) 0.011(3) -0.006(3) C113 0.082(8) 0.058(6) 0.029(5) 0.013(5) 0.032(6) 0.024(7) C121 0.098(9) 0.046(6) 0.091(8) 0.012(5) 0.028(7) 0.002(6) C122 0.060(6) 0.044(5) 0.033(4) 0.006(3) 0.021(4) 0.000(4) C123 0.080(8) 0.050(7) 0.029(5) 0.004(5) 0.032(6) 0.016(7) C610 0.038(4) 0.041(4) 0.012(3) 0.005(3) 0.009(2) 0.009(3) C611 0.033(4) 0.048(5) 0.041(4) 0.004(4) 0.022(3) 0.000(3) C612 0.051(5) 0.069(5) 0.018(3) 0.009(3) 0.013(3) 0.023(4) C613 0.051(5) 0.039(4) 0.027(4) -0.004(3) 0.011(3) 0.009(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.069465(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O11 2_666 2.070(4) yes Fe1 . Fe3 . 3.2509(11) yes Fe1 . O1 . 1.871(4) yes Fe1 . O11 . 2.043(4) yes Fe1 . O121 . 2.030(4) yes Fe1 . O151 . 2.016(4) yes Fe1 . O161 . 2.058(4) yes Fe2 . Fe3 . 3.3336(11) yes Fe2 . O1 . 1.961(4) yes Fe2 . O71 . 1.892(4) yes Fe2 . O122 . 2.034(4) yes Fe2 . O132 . 2.013(4) yes Fe2 . O142 . 2.059(4) yes Fe2 . N11 . 2.120(5) yes Fe3 . O1 . 1.863(4) yes Fe3 . O17 . 2.088(4) yes Fe3 . O133 . 2.032(4) yes Fe3 . O143 . 1.990(4) yes Fe3 . O153 . 2.014(4) yes Fe3 . O163 . 2.026(4) yes O11 . N11 . 1.397(5) yes O17 . H172 . 0.806 no O17 . H171 . 0.810 no O71 . C71 . 1.320(7) yes O121 . C12 . 1.256(7) yes O122 . C12 . 1.262(7) yes O132 . C13 . 1.242(7) yes O133 . C13 . 1.248(7) yes O142 . C14 . 1.245(7) yes O143 . C14 . 1.251(7) yes O151 . C15 . 1.262(7) yes O153 . C15 . 1.256(7) yes O161 . C16 . 1.258(7) yes O163 . C16 . 1.265(7) yes N11 . C11 . 1.288(7) yes N111 . C111 . 1.150(11) yes N112 . C112 . 1.134(10) yes N113 . C113 . 1.09(2) yes C11 . C21 . 1.453(8) yes C11 . H111 . 0.930 no C12 . C22 . 1.509(8) yes C13 . C23 . 1.525(8) yes C14 . C24 . 1.504(8) yes C15 . C25 . 1.515(8) yes C16 . C26 . 1.500(8) yes C21 . C31 . 1.402(8) yes C21 . C71 . 1.415(8) yes C22 . C32 . 1.507(9) yes C22 . H222 . 0.969 no C22 . H221 . 0.973 no C23 . C33 . 1.497(9) yes C23 . H231 . 0.978 no C23 . H232 . 0.965 no C24 . C34 . 1.514(9) yes C24 . H241 . 0.972 no C24 . H242 . 0.970 no C25 . C35 . 1.496(9) yes C25 . H252 . 0.953 no C25 . H251 . 0.959 no C26 . C36 . 1.501(9) yes C26 . H261 . 0.962 no C26 . H262 . 0.964 no C31 . C41 . 1.361(8) yes C31 . H311 . 0.939 no C32 . C42 . 1.375(9) yes C32 . C82 . 1.395(9) yes C33 . C43 . 1.356(11) yes C33 . C83 . 1.390(11) yes C34 . C44 . 1.380(9) yes C34 . C84 . 1.383(9) yes C35 . C45 . 1.355(11) yes C35 . C85 . 1.392(11) yes C36 . C46 . 1.377(9) yes C36 . C86 . 1.374(10) yes C41 . C51 . 1.399(9) yes C41 . H411 . 0.929 no C42 . C52 . 1.370(10) yes C42 . H421 . 0.939 no C43 . C53 . 1.411(12) yes C43 . H431 . 0.923 no C44 . C54 . 1.377(9) yes C44 . H441 . 0.930 no C45 . C55 . 1.414(12) yes C45 . H451 . 0.926 no C46 . C56 . 1.391(9) yes C46 . H461 . 0.929 no C51 . C61 . 1.390(9) yes C51 . H511 . 0.920 no C52 . C62 . 1.376(11) yes C52 . H521 . 0.931 no C53 . C63 . 1.355(14) yes C53 . H531 . 0.928 no C54 . C64 . 1.375(11) yes C54 . H541 . 0.937 no C55 . C65 . 1.348(14) yes C55 . H551 . 0.925 no C56 . C66 . 1.365(10) yes C56 . H561 . 0.937 no C61 . C71 . 1.419(8) yes C61 . C610 . 1.538(8) yes C62 . C72 . 1.373(11) yes C62 . H621 . 0.938 no C63 . C73 . 1.337(14) yes C63 . H631 . 0.942 no C64 . C74 . 1.370(11) yes C64 . H641 . 0.931 no C65 . C75 . 1.345(14) yes C65 . H651 . 0.920 no C66 . C76 . 1.379(11) yes C66 . H661 . 0.927 no C72 . C82 . 1.383(10) yes C72 . H721 . 0.935 no C73 . C83 . 1.380(13) yes C73 . H731 . 0.930 no C74 . C84 . 1.378(11) yes C74 . H741 . 0.910 no C75 . C85 . 1.371(12) yes C75 . H751 . 0.939 no C76 . C86 . 1.393(10) yes C76 . H761 . 0.922 no C82 . H821 . 0.925 no C83 . H831 . 0.923 no C84 . H841 . 0.941 no C85 . H851 . 0.931 no C86 . H861 . 0.930 no C111 . C121 . 1.458(13) yes C112 . C122 . 1.422(11) yes C113 . C123 . 1.431(16) yes C121 . H1211 . 0.962 no C121 . H1212 . 0.971 no C121 . H1213 . 0.943 no C122 . H1221 . 0.950 no C122 . H1222 . 0.950 no C122 . H1223 . 0.950 no C123 . H1231 . 0.950 no C123 . H1232 . 0.950 no C123 . H1233 . 0.950 no C610 . C611 . 1.535(10) yes C610 . C612 . 1.533(8) yes C610 . C613 . 1.517(10) yes C611 . H6112 . 0.952 no C611 . H6111 . 0.964 no C611 . H6113 . 0.955 no C612 . H6122 . 0.962 no C612 . H6121 . 0.963 no C612 . H6123 . 0.968 no C613 . H6132 . 0.949 no C613 . H6131 . 0.962 no C613 . H6133 . 0.951 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 2_666 Fe1 . Fe3 . 161.81(11) yes O11 2_666 Fe1 . O1 . 163.01(15) yes Fe3 . Fe1 . O1 . 29.41(11) yes O11 2_666 Fe1 . O11 . 73.64(15) yes Fe3 . Fe1 . O11 . 112.04(10) yes O1 . Fe1 . O11 . 89.39(15) yes O11 2_666 Fe1 . O121 . 85.15(16) yes Fe3 . Fe1 . O121 . 111.19(11) yes O1 . Fe1 . O121 . 94.96(16) yes O11 . Fe1 . O121 . 92.72(16) yes O11 2_666 Fe1 . O151 . 85.18(15) yes Fe3 . Fe1 . O151 . 77.26(11) yes O1 . Fe1 . O151 . 97.28(16) yes O11 . Fe1 . O151 . 94.37(16) yes O121 . Fe1 . O151 . 165.91(16) yes O11 2_666 Fe1 . O161 . 101.64(15) yes Fe3 . Fe1 . O161 . 73.43(12) yes O1 . Fe1 . O161 . 95.25(16) yes O11 . Fe1 . O161 . 174.33(16) yes O121 . Fe1 . O161 . 83.65(16) yes O151 . Fe1 . O161 . 88.29(17) yes Fe3 . Fe2 . O1 . 28.52(11) yes Fe3 . Fe2 . O71 . 152.68(12) yes O1 . Fe2 . O71 . 168.05(16) yes Fe3 . Fe2 . O122 . 110.15(11) yes O1 . Fe2 . O122 . 92.65(15) yes O71 . Fe2 . O122 . 93.94(16) yes Fe3 . Fe2 . O132 . 74.22(12) yes O1 . Fe2 . O132 . 94.83(16) yes O71 . Fe2 . O132 . 95.57(17) yes O122 . Fe2 . O132 . 85.97(18) yes Fe3 . Fe2 . O142 . 70.78(11) yes O1 . Fe2 . O142 . 89.24(16) yes O71 . Fe2 . O142 . 84.56(16) yes O122 . Fe2 . O142 . 177.16(18) yes O132 . Fe2 . O142 . 91.76(19) yes Fe3 . Fe2 . N11 . 107.61(12) yes O1 . Fe2 . N11 . 85.02(16) yes O71 . Fe2 . N11 . 85.26(17) yes O122 . Fe2 . N11 . 87.93(17) yes O132 . Fe2 . N11 . 173.88(18) yes O142 . Fe2 . N11 . 94.35(18) yes Fe1 . Fe3 . Fe2 . 59.73(2) yes Fe1 . Fe3 . O1 . 29.56(11) yes Fe2 . Fe3 . O1 . 30.18(11) yes Fe1 . Fe3 . O17 . 149.48(12) yes Fe2 . Fe3 . O17 . 150.79(12) yes O1 . Fe3 . O17 . 179.01(16) yes Fe1 . Fe3 . O133 . 116.52(14) yes Fe2 . Fe3 . O133 . 73.55(12) yes O1 . Fe3 . O133 . 95.55(17) yes O17 . Fe3 . O133 . 85.30(17) yes Fe1 . Fe3 . O143 . 115.24(14) yes Fe2 . Fe3 . O143 . 76.98(13) yes O1 . Fe3 . O143 . 96.96(17) yes O17 . Fe3 . O143 . 83.52(18) yes O133 . Fe3 . O143 . 90.8(2) yes Fe1 . Fe3 . O153 . 73.21(12) yes Fe2 . Fe3 . O153 . 117.83(13) yes O1 . Fe3 . O153 . 95.73(17) yes O17 . Fe3 . O153 . 83.40(16) yes O133 . Fe3 . O153 . 168.47(18) yes Fe1 . Fe3 . O163 . 76.78(12) yes Fe2 . Fe3 . O163 . 111.59(13) yes O1 . Fe3 . O163 . 94.32(17) yes O17 . Fe3 . O163 . 85.26(17) yes O133 . Fe3 . O163 . 83.9(2) yes O143 . Fe3 . O153 . 90.2(2) yes O143 . Fe3 . O163 . 167.96(19) yes O153 . Fe3 . O163 . 92.8(2) yes Fe2 . O1 . Fe1 . 117.67(18) yes Fe2 . O1 . Fe3 . 121.30(19) yes Fe1 . O1 . Fe3 . 121.03(19) yes Fe1 2_666 O11 . Fe1 . 106.36(15) yes Fe1 2_666 O11 . N11 . 132.6(3) yes Fe1 . O11 . N11 . 115.8(3) yes Fe3 . O17 . H172 . 112.1 no Fe3 . O17 . H171 . 114.6 no H172 . O17 . H171 . 119.3 no Fe2 . O71 . C71 . 132.4(4) yes Fe1 . O121 . C12 . 129.8(4) yes Fe2 . O122 . C12 . 133.5(4) yes Fe2 . O132 . C13 . 133.1(4) yes Fe3 . O133 . C13 . 132.9(4) yes Fe2 . O142 . C14 . 136.1(4) yes Fe3 . O143 . C14 . 130.4(4) yes Fe1 . O151 . C15 . 128.7(4) yes Fe3 . O153 . C15 . 134.6(4) yes Fe1 . O161 . C16 . 131.5(4) yes Fe3 . O163 . C16 . 129.5(4) yes Fe2 . N11 . O11 . 117.9(3) yes Fe2 . N11 . C11 . 126.3(4) yes O11 . N11 . C11 . 115.7(4) yes N11 . C11 . C21 . 123.8(5) yes N11 . C11 . H111 . 117.9 no C21 . C11 . H111 . 118.3 no O122 . C12 . O121 . 126.0(5) yes O122 . C12 . C22 . 117.0(5) yes O121 . C12 . C22 . 116.9(5) yes O133 . C13 . O132 . 125.2(5) yes O133 . C13 . C23 . 117.6(5) yes O132 . C13 . C23 . 117.2(5) yes O143 . C14 . O142 . 124.5(5) yes O143 . C14 . C24 . 117.7(5) yes O142 . C14 . C24 . 117.8(5) yes O151 . C15 . O153 . 125.2(5) yes O151 . C15 . C25 . 115.9(5) yes O153 . C15 . C25 . 118.9(5) yes O163 . C16 . O161 . 124.8(5) yes O163 . C16 . C26 . 114.3(5) yes O161 . C16 . C26 . 120.9(6) yes C11 . C21 . C31 . 116.0(5) yes C11 . C21 . C71 . 123.9(5) yes C31 . C21 . C71 . 120.1(5) yes C12 . C22 . C32 . 111.5(5) yes C12 . C22 . H222 . 111.2 no C32 . C22 . H222 . 107.1 no C12 . C22 . H221 . 110.3 no C32 . C22 . H221 . 107.6 no H222 . C22 . H221 . 109.0 no C13 . C23 . C33 . 111.0(5) yes C13 . C23 . H231 . 109.1 no C33 . C23 . H231 . 109.8 no C13 . C23 . H232 . 107.5 no C33 . C23 . H232 . 108.8 no H231 . C23 . H232 . 110.6 no C14 . C24 . C34 . 115.0(5) yes C14 . C24 . H241 . 107.7 no C34 . C24 . H241 . 109.2 no C14 . C24 . H242 . 108.7 no C34 . C24 . H242 . 107.8 no H241 . C24 . H242 . 108.3 no C15 . C25 . C35 . 115.8(5) yes C15 . C25 . H252 . 106.6 no C35 . C25 . H252 . 108.8 no C15 . C25 . H251 . 107.2 no C35 . C25 . H251 . 108.3 no H252 . C25 . H251 . 110.1 no C16 . C26 . C36 . 119.8(6) yes C16 . C26 . H261 . 105.2 no C36 . C26 . H261 . 105.0 no C16 . C26 . H262 . 107.9 no C36 . C26 . H262 . 108.5 no H261 . C26 . H262 . 110.1 no C21 . C31 . C41 . 120.7(6) yes C21 . C31 . H311 . 119.0 no C41 . C31 . H311 . 120.3 no C22 . C32 . C42 . 121.6(6) yes C22 . C32 . C82 . 119.8(6) yes C42 . C32 . C82 . 118.6(7) yes C23 . C33 . C43 . 121.9(7) yes C23 . C33 . C83 . 120.1(7) yes C43 . C33 . C83 . 118.0(8) yes C24 . C34 . C44 . 122.0(6) yes C24 . C34 . C84 . 119.9(6) yes C44 . C34 . C84 . 118.1(6) yes C25 . C35 . C45 . 122.7(7) yes C25 . C35 . C85 . 119.3(7) yes C45 . C35 . C85 . 117.9(7) yes C26 . C36 . C46 . 118.5(7) yes C26 . C36 . C86 . 122.2(6) yes C46 . C36 . C86 . 119.2(6) yes C31 . C41 . C51 . 119.1(6) yes C31 . C41 . H411 . 120.5 no C51 . C41 . H411 . 120.4 no C32 . C42 . C52 . 121.0(7) yes C32 . C42 . H421 . 119.9 no C52 . C42 . H421 . 119.1 no C33 . C43 . C53 . 121.2(9) yes C33 . C43 . H431 . 119.5 no C53 . C43 . H431 . 119.2 no C34 . C44 . C54 . 121.1(6) yes C34 . C44 . H441 . 119.9 no C54 . C44 . H441 . 119.0 no C35 . C45 . C55 . 120.2(9) yes C35 . C45 . H451 . 120.4 no C55 . C45 . H451 . 119.5 no C36 . C46 . C56 . 120.9(7) yes C36 . C46 . H461 . 118.9 no C56 . C46 . H461 . 120.1 no C41 . C51 . C61 . 123.0(5) yes C41 . C51 . H511 . 118.4 no C61 . C51 . H511 . 118.6 no C42 . C52 . C62 . 120.5(8) yes C42 . C52 . H521 . 118.8 no C62 . C52 . H521 . 120.7 no C43 . C53 . C63 . 118.7(10) yes C43 . C53 . H531 . 120.9 no C63 . C53 . H531 . 120.4 no C44 . C54 . C64 . 120.3(7) yes C44 . C54 . H541 . 118.8 no C64 . C54 . H541 . 120.9 no C45 . C55 . C65 . 119.2(10) yes C45 . C55 . H551 . 119.5 no C65 . C55 . H551 . 121.2 no C46 . C56 . C66 . 120.0(6) yes C46 . C56 . H561 . 120.7 no C66 . C56 . H561 . 119.3 no C51 . C61 . C71 . 117.4(5) yes C51 . C61 . C610 . 121.6(5) yes C71 . C61 . C610 . 120.9(5) yes C52 . C62 . C72 . 119.4(7) yes C52 . C62 . H621 . 121.6 no C72 . C62 . H621 . 119.1 no C53 . C63 . C73 . 121.0(9) yes C53 . C63 . H631 . 119.2 no C73 . C63 . H631 . 119.8 no C54 . C64 . C74 . 119.1(7) yes C54 . C64 . H641 . 121.5 no C74 . C64 . H641 . 119.5 no C55 . C65 . C75 . 122.0(9) yes C55 . C65 . H651 . 119.0 no C75 . C65 . H651 . 119.0 no C56 . C66 . C76 . 119.3(7) yes C56 . C66 . H661 . 120.0 no C76 . C66 . H661 . 120.6 no C61 . C71 . C21 . 119.6(5) yes C61 . C71 . O71 . 120.9(5) yes C21 . C71 . O71 . 119.6(5) yes C62 . C72 . C82 . 120.6(7) yes C62 . C72 . H721 . 119.4 no C82 . C72 . H721 . 120.1 no C63 . C73 . C83 . 120.8(10) yes C63 . C73 . H731 . 120.1 no C83 . C73 . H731 . 119.1 no C64 . C74 . C84 . 120.8(7) yes C64 . C74 . H741 . 119.4 no C84 . C74 . H741 . 119.8 no C65 . C75 . C85 . 118.7(10) yes C65 . C75 . H751 . 119.8 no C85 . C75 . H751 . 121.6 no C66 . C76 . C86 . 120.9(7) yes C66 . C76 . H761 . 119.5 no C86 . C76 . H761 . 119.6 no C32 . C82 . C72 . 119.9(7) yes C32 . C82 . H821 . 118.5 no C72 . C82 . H821 . 121.6 no C33 . C83 . C73 . 120.2(10) yes C33 . C83 . H831 . 119.5 no C73 . C83 . H831 . 120.3 no C34 . C84 . C74 . 120.6(7) yes C34 . C84 . H841 . 119.2 no C74 . C84 . H841 . 120.2 no C35 . C85 . C75 . 122.0(9) yes C35 . C85 . H851 . 118.2 no C75 . C85 . H851 . 119.8 no C76 . C86 . C36 . 119.7(6) yes C76 . C86 . H861 . 120.3 no C36 . C86 . H861 . 120.0 no N111 . C111 . C121 . 179.0(11) yes N112 . C112 . C122 . 178.1(8) yes N113 . C113 . C123 . 173(2) yes C111 . C121 . H1211 . 110.9 no C111 . C121 . H1212 . 110.4 no H1211 . C121 . H1212 . 106.7 no C111 . C121 . H1213 . 111.5 no H1211 . C121 . H1213 . 109.0 no H1212 . C121 . H1213 . 108.2 no C112 . C122 . H1221 . 109.5 no C112 . C122 . H1222 . 109.8 no H1221 . C122 . H1222 . 109.5 no C112 . C122 . H1223 . 109.0 no H1221 . C122 . H1223 . 109.5 no H1222 . C122 . H1223 . 109.5 no C113 . C123 . H1231 . 109.4 no C113 . C123 . H1232 . 109.5 no H1231 . C123 . H1232 . 109.5 no C113 . C123 . H1233 . 109.5 no H1231 . C123 . H1233 . 109.5 no H1232 . C123 . H1233 . 109.5 no C61 . C610 . C611 . 109.5(5) yes C61 . C610 . C612 . 111.3(5) yes C611 . C610 . C612 . 107.8(6) yes C61 . C610 . C613 . 111.2(6) yes C611 . C610 . C613 . 109.6(6) yes C612 . C610 . C613 . 107.3(6) yes C610 . C611 . H6112 . 109.4 no C610 . C611 . H6111 . 109.4 no H6112 . C611 . H6111 . 109.2 no C610 . C611 . H6113 . 110.7 no H6112 . C611 . H6113 . 109.6 no H6111 . C611 . H6113 . 108.4 no C610 . C612 . H6122 . 108.7 no C610 . C612 . H6121 . 109.9 no H6122 . C612 . H6121 . 108.1 no C610 . C612 . H6123 . 111.2 no H6122 . C612 . H6123 . 108.2 no H6121 . C612 . H6123 . 110.6 no C610 . C613 . H6132 . 109.4 no C610 . C613 . H6131 . 108.0 no H6132 . C613 . H6131 . 108.9 no C610 . C613 . H6133 . 110.4 no H6132 . C613 . H6133 . 110.5 no H6131 . C613 . H6133 . 109.8 no # Attachment 'Complex 8.cif' data_eb6113 _database_code_depnum_ccdc_archive 'CCDC 755042' #TrackingRef 'Complex 8.cif' _audit_creation_date 06-10-13 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb6113 in P6(3)/m' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.40610(10) _cell_length_b 12.40610(10) _cell_length_c 28.8478(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3845.16(9) _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m ' _symmetry_space_group_name_Hall '-P 6c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x-y,x,z+1/2 -x+y,-x,-z+1/2 -y,x-y,z y,-x+y,-z -x,-y,z+1/2 x,y,-z+1/2 -x+y,-x,z x-y,x,-z y,-x+y,z+1/2 -y,x-y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C58 H88 Fe6 N6 Na3 O30 # Dc = 1.51 Fooo = 1778.00 Mu = 12.02 M = 292.24 # Found Formula = C57 H84 Fe6 N6 Na3 O29 # Dc = 1.49 FOOO = 1778.00 Mu = 11.99 M = 286.89 _chemical_formula_sum 'C58 H88 Fe6 N6 Na3 O30' _chemical_formula_moiety 'C57 H84 Fe6 N6 Na3 O29. MeOH' _chemical_compound_source ? _chemical_formula_weight 1753.41 _cell_measurement_reflns_used 7947 _cell_measurement_theta_min 5 _cell_measurement_theta_max 56 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1814.000 _exptl_absorpt_coefficient_mu 1.199 # Sheldrick geometric approximatio 0.71 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 46897 _reflns_number_total 3379 _diffrn_reflns_av_R_equivalents 0.066 # Number of reflections with Friedels Law is 3379 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3414 _diffrn_reflns_theta_min 1.412 _diffrn_reflns_theta_max 29.018 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.857 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _reflns_limit_h_min -14 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 39 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.41 _refine_diff_density_max 0.71 _refine_ls_number_reflns 2110 _refine_ls_number_restraints 3 _refine_ls_number_parameters 168 #_refine_ls_R_factor_ref 0.0297 _refine_ls_wR_factor_ref 0.0322 _refine_ls_goodness_of_fit_ref 0.9647 #_reflns_number_all 3379 _refine_ls_R_factor_all 0.0532 _refine_ls_wR_factor_all 0.0375 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2110 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_gt 0.0322 _refine_ls_shift/su_max 0.002562 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.54 0.577 1.27 ; _publ_section_exptl_refinement ; 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 107 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 1388 1388 0 23.01 0.550 1.000 1837 1837 0 25.24 0.600 1.000 2378 2378 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 3016 3016 0 29.02 0.683 0.969 3486 3379 107 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.81 Sadabs corrects for all systematic errors that lead to disparities in the intensities of equivalent data. It is possible that the larger than expected range of transmission is accounted for by crystal decay or absorption by the mounting fibre. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. No action taken. 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.65 Ratio The principle components of the strain tensor for all O atoms appear normal. Principal axes of the thermal ellipsoids, A**2 O 1. 0.0125 0.0151 0.0215 O 2. 0.0127 0.0131 0.0137 O 3. 0.0116 0.0116 0.0134 O 4. 0.0145 0.0203 0.0297 O 6. 0.0123 0.0174 0.0239 O 10. 0.0098 0.0139 0.0182 O 20. 0.0173 0.0289 0.0506 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 91.00 A**3 Structure was squeezed. See SQUEEZE RESULTS in .cif 380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C4 The methyl H-atoms have been positioned geometrically. Constrained refinement of the group also confirms that the position of the methyl group is correct, although the group was (in the end) constrained to a fixed geometry. 731_ALERT_1_C Bond Calc 0.82(4), Rep 0.818(10) ...... 4.00 su-Rat O2 -H2 1.555 1.555 731_ALERT_1_C Bond Calc 0.81(2), Rep 0.815(9) ...... 2.22 su-Rat O4 -H4 1.555 8.556 731_ALERT_1_C Bond Calc 0.81(2), Rep 0.815(9) ...... 2.22 su-Rat O4 -H4 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(3), Rep 0.819(10) ...... 3.00 su-Rat O20 -H20 1.555 1.555 The H atoms above were refined with restraints, with e.s.d's calculated using both variances and covariances which would account for the difference. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 6.6 -0.2 2 0.000 0.000 0.500 6.6 -0.1 3 0.333 0.667 0.534 90.1 16.5 4 0.333 0.667 0.966 90.1 17.3 5 0.333 0.667 0.750 27.0 -0.9 6 0.667 0.333 0.034 90.1 17.2 7 0.667 0.333 0.466 90.0 16.9 8 0.667 0.333 0.250 27.0 -0.9 _platon_squeeze_details ; A disordered MeOH group was squeezed, as the disorder could not be modelled satisfactorilly. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.70995(2) 0.51065(2) 0.695670(8) 0.0121 1.0000 Uani . . . . . . Na1 Na 1.00336(11) 0.79034(11) 0.7500 0.0234 1.0000 Uani S T . . . . C3 C 0.56411(19) 0.4818(2) 0.60585(7) 0.0195 1.0000 Uani . . . . . . C4 C 0.4692(3) 0.4036(2) 0.57004(8) 0.0371 1.0000 Uani . . . . . . C5 C 0.6543(2) 0.6133(2) 0.59584(7) 0.0200 1.0000 Uani . . . . . . C6 C 0.73272(18) 0.69978(19) 0.62982(7) 0.0178 1.0000 Uani . . . . . . C7 C 0.8071(2) 0.82589(19) 0.61705(8) 0.0227 1.0000 Uani . . . . . . C8 C 0.8047(2) 0.8659(2) 0.57242(9) 0.0289 1.0000 Uani . . . . . . C9 C 0.7312(2) 0.7817(2) 0.53885(9) 0.0319 1.0000 Uani . . . . . . C10 C 0.5253(3) 0.5616(3) 0.7500 0.0205 1.0000 Uani S T . . . . C20 C 1.1617(2) 0.7249(2) 0.66126(11) 0.0377 1.0000 Uani . . . . . . C21 C 0.6575(2) 0.6578(2) 0.55076(8) 0.0293 1.0000 Uani . . . . . . N2 N 0.56586(15) 0.43397(15) 0.64563(6) 0.0155 1.0000 Uani . . . . . . O1 O 0.47122(13) 0.31371(13) 0.65271(5) 0.0164 1.0000 Uani . . . . . . O2 O 0.82824(17) 0.57617(18) 0.7500 0.0132 1.0000 Uani DS T . . . . O3 O 0.6667 0.3333 0.70715(8) 0.0122 1.0000 Uani S T . . . . O4 O 1.16955(19) 0.9979(2) 0.7500 0.0215 1.0000 Uani DS T . . . . O6 O 0.73675(13) 0.66961(13) 0.67379(5) 0.0179 1.0000 Uani . . . . . . O10 O 0.59590(17) 0.49985(18) 0.7500 0.0140 1.0000 Uani S T . . . . O20 O 1.06124(16) 0.72620(16) 0.68370(6) 0.0323 1.0000 Uani D . . . . . H2 H 0.870(3) 0.542(3) 0.7500 0.0196 1.0000 Uiso DS . . . . . H4 H 1.212(2) 1.011(3) 0.7730(7) 0.0293 1.0000 Uiso D . . . . . H20 H 0.9965(19) 0.674(3) 0.6714(12) 0.0423 1.0000 Uiso D . . . . . H201 H 1.1621 0.7393 0.6283 0.0556 1.0000 Uiso . . . . . . H202 H 1.1564 0.6459 0.6637 0.0544 1.0000 Uiso . . . . . . H203 H 1.2404 0.7904 0.6729 0.0552 1.0000 Uiso . . . . . . H41 H 0.4173 0.3215 0.5810 0.0495 1.0000 Uiso . . . . . . H42 H 0.4197 0.4415 0.5628 0.0493 1.0000 Uiso . . . . . . H43 H 0.5106 0.3997 0.5430 0.0490 1.0000 Uiso . . . . . . H71 H 0.8561 0.8816 0.6387 0.0271 1.0000 Uiso . . . . . . H81 H 0.8527 0.9493 0.5655 0.0339 1.0000 Uiso . . . . . . H91 H 0.7328 0.8091 0.5087 0.0380 1.0000 Uiso . . . . . . H211 H 0.6062 0.6029 0.5289 0.0339 1.0000 Uiso . . . . . . H102 H 0.5779 0.6497 0.7500 0.0363 1.0000 Uiso . . . . . . H103 H 0.4738 0.5388 0.7764 0.0359 1.0000 Uiso . . . . . . 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 0.01348(13) 0.01230(13) 0.01047(12) 0.00067(10) -0.00033(10) 0.00647(10) Na1 0.0199(6) 0.0183(6) 0.0278(6) 0.0000 0.0000 0.0064(5) C3 0.0226(10) 0.0208(9) 0.0156(9) -0.0003(7) -0.0033(7) 0.0112(8) C4 0.0450(15) 0.0318(12) 0.0189(11) 0.0044(9) -0.0131(10) 0.0074(11) C5 0.0220(9) 0.0222(10) 0.0161(9) 0.0044(7) 0.0018(7) 0.0114(8) C6 0.0179(9) 0.0203(9) 0.0191(9) 0.0030(8) 0.0021(7) 0.0125(8) C7 0.0215(9) 0.0177(9) 0.0268(10) 0.0050(8) 0.0011(8) 0.0082(8) C8 0.0282(12) 0.0254(11) 0.0309(12) 0.0147(9) 0.0065(9) 0.0118(9) C9 0.0367(13) 0.0345(13) 0.0218(11) 0.0128(9) 0.0031(9) 0.0158(11) C10 0.0222(14) 0.0196(13) 0.0267(14) 0.0000 0.0000 0.0157(12) C20 0.0277(12) 0.0308(13) 0.0500(17) 0.0004(11) 0.0071(11) 0.0113(10) C21 0.0334(12) 0.0314(12) 0.0185(11) 0.0050(9) -0.0036(9) 0.0128(10) N2 0.0164(7) 0.0154(8) 0.0142(7) 0.0005(6) -0.0005(6) 0.0076(6) O1 0.0151(6) 0.0145(6) 0.0170(6) 0.0001(5) -0.0033(5) 0.0055(5) O2 0.0136(9) 0.0136(9) 0.0127(8) 0.0000 0.0000 0.0070(7) O3 0.0116(6) 0.0116(6) 0.0134(10) 0.0000 0.0000 0.0058(3) O4 0.0162(10) 0.0210(10) 0.0203(10) 0.0000 0.0000 0.0040(8) O6 0.0236(7) 0.0154(6) 0.0153(6) 0.0023(5) 0.0000(5) 0.0103(6) O10 0.0153(9) 0.0168(9) 0.0139(8) 0.0000 0.0000 0.0111(8) O20 0.0213(8) 0.0273(8) 0.0353(9) -0.0055(7) 0.0044(7) 0.0024(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2484(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 9_665 1.9800(14) yes Fe1 . N2 . 2.1174(16) yes Fe1 . O2 . 2.0194(12) yes Fe1 . O3 . 2.0140(4) yes Fe1 . O6 . 1.9345(14) yes Fe1 . O10 . 2.0704(12) yes Na1 . O20 8_556 2.3192(19) yes Na1 . O4 4_676 2.458(3) yes Na1 . O2 . 2.451(2) yes Na1 . O4 . 2.361(2) yes Na1 . O20 . 2.3192(19) yes C3 . C4 . 1.501(3) yes C3 . C5 . 1.474(3) yes C3 . N2 . 1.297(3) yes C4 . H41 . 0.947 no C4 . H42 . 0.965 no C4 . H43 . 0.948 no C5 . C6 . 1.419(3) yes C5 . C21 . 1.406(3) yes C6 . C7 . 1.411(3) yes C6 . O6 . 1.330(2) yes C7 . C8 . 1.385(3) yes C7 . H71 . 0.904 no C8 . C9 . 1.381(4) yes C8 . H81 . 0.921 no C9 . C21 . 1.383(4) yes C9 . H91 . 0.930 no C10 . H103 8_556 0.942 no C10 . O10 . 1.423(3) yes C10 . H102 . 0.952 no C10 . H103 . 0.942 no C20 . O20 . 1.412(3) yes C20 . H201 . 0.966 no C20 . H202 . 0.950 no C20 . H203 . 0.966 no C21 . H211 . 0.913 no N2 . O1 . 1.376(2) yes O2 . H2 . 0.818(10) no O4 . H4 8_556 0.815(9) no O4 . H4 . 0.815(9) no O20 . H20 . 0.819(10) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 9_665 Fe1 . N2 . 95.22(6) yes O1 9_665 Fe1 . O2 . 92.58(6) yes N2 . Fe1 . O2 . 172.01(6) yes O1 9_665 Fe1 . O3 . 88.83(6) yes N2 . Fe1 . O3 . 85.25(6) yes O2 . Fe1 . O3 . 93.17(7) yes O1 9_665 Fe1 . O6 . 88.30(6) yes N2 . Fe1 . O6 . 84.94(6) yes O2 . Fe1 . O6 . 97.07(7) yes O3 . Fe1 . O6 . 169.48(7) yes O1 9_665 Fe1 . O10 . 169.41(6) yes N2 . Fe1 . O10 . 95.22(6) yes O2 . Fe1 . O10 . 76.94(6) yes O3 . Fe1 . O10 . 90.26(7) yes O6 . Fe1 . O10 . 94.39(7) yes O20 8_556 Na1 . O4 4_676 121.72(6) yes O20 8_556 Na1 . O2 . 83.50(6) yes O4 4_676 Na1 . O2 . 79.95(7) yes O20 8_556 Na1 . O4 . 97.06(6) yes O4 4_676 Na1 . O4 . 99.05(11) yes O2 . Na1 . O4 . 179.00(9) yes O20 8_556 Na1 . O20 . 111.12(11) yes O4 4_676 Na1 . O20 . 121.72(6) yes O2 . Na1 . O20 . 83.50(6) yes O4 . Na1 . O20 . 97.06(6) yes C4 . C3 . C5 . 119.81(18) yes C4 . C3 . N2 . 120.0(2) yes C5 . C3 . N2 . 120.18(18) yes C3 . C4 . H41 . 110.9 no C3 . C4 . H42 . 108.6 no H41 . C4 . H42 . 109.9 no C3 . C4 . H43 . 109.2 no H41 . C4 . H43 . 108.3 no H42 . C4 . H43 . 109.8 no C3 . C5 . C6 . 123.76(18) yes C3 . C5 . C21 . 118.20(19) yes C6 . C5 . C21 . 117.91(19) yes C5 . C6 . C7 . 118.62(19) yes C5 . C6 . O6 . 123.62(18) yes C7 . C6 . O6 . 117.71(19) yes C6 . C7 . C8 . 121.3(2) yes C6 . C7 . H71 . 119.0 no C8 . C7 . H71 . 119.6 no C7 . C8 . C9 . 120.4(2) yes C7 . C8 . H81 . 119.0 no C9 . C8 . H81 . 120.6 no C8 . C9 . C21 . 119.1(2) yes C8 . C9 . H91 . 119.6 no C21 . C9 . H91 . 121.3 no H103 8_556 C10 . O10 . 110.2 no H103 8_556 C10 . H102 . 108.6 no O10 . C10 . H102 . 111.4 no H103 8_556 C10 . H103 . 107.8 no O10 . C10 . H103 . 110.2 no H102 . C10 . H103 . 108.6 no O20 . C20 . H201 . 111.7 no O20 . C20 . H202 . 111.7 no H201 . C20 . H202 . 104.9 no O20 . C20 . H203 . 110.9 no H201 . C20 . H203 . 106.2 no H202 . C20 . H203 . 111.2 no C5 . C21 . C9 . 122.7(2) yes C5 . C21 . H211 . 118.3 no C9 . C21 . H211 . 119.0 no Fe1 . N2 . C3 . 126.94(14) yes Fe1 . N2 . O1 . 117.18(11) yes C3 . N2 . O1 . 115.27(16) yes N2 . O1 . Fe1 5_655 121.93(11) yes Na1 . O2 . Fe1 8_556 120.54(6) yes Na1 . O2 . Fe1 . 120.54(6) yes Fe1 8_556 O2 . Fe1 . 101.82(8) yes Na1 . O2 . H2 . 96(3) no Fe1 8_556 O2 . H2 . 108.3(16) no Fe1 . O2 . H2 . 108.3(16) no Fe1 . O3 . Fe1 5_655 117.35(3) yes Fe1 . O3 . Fe1 9_665 117.35(3) yes Fe1 5_655 O3 . Fe1 9_665 117.35(3) yes Na1 . O4 . Na1 5_765 140.95(11) yes Na1 . O4 . H4 8_556 110(2) no Na1 5_765 O4 . H4 8_556 92(2) no Na1 . O4 . H4 . 110(2) no Na1 5_765 O4 . H4 . 92(2) no H4 8_556 O4 . H4 . 109(4) no C6 . O6 . Fe1 . 125.90(13) yes C10 . O10 . Fe1 . 123.35(8) yes C10 . O10 . Fe1 8_556 123.35(8) yes Fe1 . O10 . Fe1 8_556 98.40(8) yes Na1 . O20 . C20 . 143.96(16) yes Na1 . O20 . H20 . 106(3) no C20 . O20 . H20 . 108(3) no # Attachment 'Complex 9.cif' data_EB8050 _database_code_depnum_ccdc_archive 'CCDC 755043' #TrackingRef 'Complex 9.cif' _audit_creation_date 08-07-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8050 in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H124 Fe12 N12 Na4 O50, 2(N C6 H16)' _chemical_compound_source 'Ian Gass, IAG2892' _exptl_crystal_recrystallization_method ; Slow evaporation of MeOH solution. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Checkcif alerts 020_ALERT_3_B The value of Rint is greater than 0.10 ......... 0.16 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.97 Ratio 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 432_ALERT_2_C Short Inter X...Y Contact C26 .. C38 .. 3.14 Ang. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.86 Ratio 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.57 Ratio 026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 41 Perc. The data are weak and generally low quality. 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 420_ALERT_2_B D-H Without Acceptor O69 - H691 ... ? 420_ALERT_2_B D-H Without Acceptor O78 - H781 ... ? 420_ALERT_2_B D-H Without Acceptor O80 - H801 ... ? The solvent region was treated by the van der Sluis and Spek method, accounting for 244 e/cell. This corresponds to 2 molecules of HN(Et)~3~ ^+^ per formula unit and F(000), M, mu, D and the formulae have been calculated on this assumption. 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 5 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 3 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 41 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 6 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 7791 7785 6 23.01 0.550 0.999 10347 10341 6 25.24 0.600 0.999 13462 13454 8 #----------------------------------------------------------- ACTA Min. Res. --- 26.42 0.626 0.997 15270 15221 49 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 24 The following restraints were applied: U(IJ)'S 0.0, 0.010000 = O(31) TO C(32) U(IJ)'S 0.0, 0.010000 = O(72) TO FE(6) U(IJ)'S 0.0, 0.010000 = C(18) TO C(19) U(IJ)'S 0.0, 0.010000 = C(17) TO C(18) ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.016 0.001 1609.8 244.2 _platon_squeeze_details ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 23.1511(7) _cell_length_b 13.5740(4) _cell_length_c 23.7570(8) _cell_angle_alpha 90 _cell_angle_beta 95.223(2) _cell_angle_gamma 90 _cell_volume 7434.7(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C112 H156 Fe12 N14 Na4 O50 # Dc = 1.46 Fooo = 3132.00 Mu = 12.27 M = 1630.33 # Found Formula = C100 H126 Fe12 N12 Na4 O50 # Dc = 1.37 FOOO = 3132.00 Mu = 12.22 M = 1529.14 _chemical_formula_sum 'C102 H156 Fe12 N14 Na4 O50' _chemical_formula_weight 3260.66 _cell_measurement_reflns_used 3042 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3132 _exptl_absorpt_coefficient_mu 1.222 # Sheldrick geometric approximatio 0.78 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.83 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15221 _reflns_number_total 15221 _diffrn_reflns_av_R_equivalents 0.157 # Number of reflections with Friedels Law is 15221 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 15275 _diffrn_reflns_theta_min 1.862 _diffrn_reflns_theta_max 26.415 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.415 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -28 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 1.19 _oxford_diffrn_Wilson_scale 46.48 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.92 _refine_diff_density_max 1.88 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 15162 _refine_ls_number_restraints 30 _refine_ls_number_parameters 802 _oxford_refine_ls_R_factor_ref 0.1674 _refine_ls_wR_factor_ref 0.1945 _refine_ls_goodness_of_fit_ref 0.6879 _refine_ls_shift/su_max 0.000467 # The values computed from all data _oxford_reflns_number_all 15162 _refine_ls_R_factor_all 0.1674 _refine_ls_wR_factor_all 0.1945 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6186 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_gt 0.1509 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens O1 O 0.7372(3) -0.2573(4) 0.5538(3) 0.0311 1.0000 Uani . . . . . . . C2 C 0.7238(4) -0.3094(6) 0.5974(4) 0.0253 1.0000 Uani . . . . . . . C3 C 0.7290(4) -0.4133(6) 0.5960(4) 0.0344 1.0000 Uani . . . . . . . C4 C 0.7153(4) -0.4694(7) 0.6411(4) 0.0403 1.0000 Uani . . . . . . . C5 C 0.6956(4) -0.4274(7) 0.6887(4) 0.0373 1.0000 Uani . . . . . . . C6 C 0.6886(4) -0.3273(6) 0.6892(4) 0.0339 1.0000 Uani . . . . . . . C7 C 0.7014(4) -0.2674(6) 0.6455(4) 0.0257 1.0000 Uani . . . . . . . C8 C 0.6898(4) -0.1631(6) 0.6512(4) 0.0249 1.0000 Uani . . . . . . . N9 N 0.7007(3) -0.0948(5) 0.6159(3) 0.0266 1.0000 Uani . . . . . . . O10 O 0.6844(3) -0.0019(4) 0.6303(3) 0.0314 1.0000 Uani . . . . . . . O11 O 0.8227(3) -0.1166(4) 0.5826(3) 0.0379 1.0000 Uani . . . . . . . N12 N 0.8587(3) -0.0353(5) 0.5844(3) 0.0287 1.0000 Uani . . . . . . . C13 C 0.9064(4) -0.0420(7) 0.6159(4) 0.0391 1.0000 Uani . . . . . . . C14 C 0.9492(4) 0.0330(7) 0.6255(5) 0.0430 1.0000 Uani . . . . . . . C15 C 0.9953(4) 0.0169(8) 0.6673(6) 0.0585 1.0000 Uani . . . . . . . C16 C 1.0378(4) 0.0882(10) 0.6780(6) 0.0662 1.0000 Uani . . . . . . . C17 C 1.0366(4) 0.1734(8) 0.6477(5) 0.0546 1.0000 Uani . U . . . . . C18 C 0.9929(4) 0.1910(7) 0.6052(5) 0.0472 1.0000 Uani . U . . . . . C19 C 0.9486(4) 0.1218(7) 0.5942(5) 0.0417 1.0000 Uani . U . . . . . O20 O 0.9072(3) 0.1407(5) 0.5514(3) 0.0394 1.0000 Uani . . . . . . . O21 O 0.8108(2) 0.1667(4) 0.6094(2) 0.0315 1.0000 Uani . . . . . . . N22 N 0.7555(3) 0.1807(5) 0.6239(3) 0.0231 1.0000 Uani . . . . . . . C23 C 0.7506(4) 0.2331(6) 0.6682(4) 0.0289 1.0000 Uani . . . . . . . C24 C 0.6978(4) 0.2616(6) 0.6926(4) 0.0220 1.0000 Uani . . . . . . . C25 C 0.7032(4) 0.3188(6) 0.7411(4) 0.0270 1.0000 Uani . . . . . . . C26 C 0.6564(4) 0.3518(7) 0.7655(4) 0.0372 1.0000 Uani . . . . . . . C27 C 0.6017(4) 0.3254(7) 0.7432(4) 0.0350 1.0000 Uani . . . . . . . C28 C 0.5948(4) 0.2676(7) 0.6968(4) 0.0379 1.0000 Uani . . . . . . . C29 C 0.6423(4) 0.2360(6) 0.6686(4) 0.0252 1.0000 Uani . . . . . . . O30 O 0.6338(2) 0.1839(4) 0.6207(2) 0.0258 1.0000 Uani . . . . . . . O31 O 0.5735(2) 0.2142(4) 0.4478(3) 0.0285 1.0000 Uani . U . . . . . C32 C 0.5509(4) 0.2820(6) 0.4115(4) 0.0244 1.0000 Uani . U . . . . . C33 C 0.4933(4) 0.3116(6) 0.4164(4) 0.0290 1.0000 Uani . . . . . . . C34 C 0.4675(4) 0.3811(7) 0.3796(5) 0.0452 1.0000 Uani . . . . . . . C35 C 0.4972(4) 0.4240(7) 0.3389(4) 0.0438 1.0000 Uani . . . . . . . C36 C 0.5524(4) 0.3946(7) 0.3338(4) 0.0383 1.0000 Uani . . . . . . . C37 C 0.5808(4) 0.3242(6) 0.3698(4) 0.0259 1.0000 Uani . . . . . . . C38 C 0.6415(4) 0.3012(6) 0.3623(4) 0.0271 1.0000 Uani . . . . . . . N39 N 0.6732(3) 0.2381(5) 0.3911(3) 0.0222 1.0000 Uani . . . . . . . O40 O 0.7300(2) 0.2313(4) 0.3781(2) 0.0257 1.0000 Uani . . . . . . . O41 O 0.5975(2) 0.0493(4) 0.3929(2) 0.0248 1.0000 Uani . . . . . . . N42 N 0.6194(3) -0.0407(5) 0.3781(3) 0.0216 1.0000 Uani . . . . . . . C43 C 0.5878(4) -0.0897(6) 0.3413(4) 0.0312 1.0000 Uani . . . . . . . C44 C 0.5996(4) -0.1873(6) 0.3217(4) 0.0305 1.0000 Uani . . . . . . . C45 C 0.5621(4) -0.2270(7) 0.2792(4) 0.0385 1.0000 Uani . . . . . . . C46 C 0.5707(5) -0.3204(8) 0.2580(4) 0.0461 1.0000 Uani . . . . . . . C47 C 0.6178(5) -0.3752(7) 0.2783(4) 0.0432 1.0000 Uani . . . . . . . C48 C 0.6547(4) -0.3385(6) 0.3211(4) 0.0312 1.0000 Uani . . . . . . . C49 C 0.6479(4) -0.2461(6) 0.3447(4) 0.0281 1.0000 Uani . . . . . . . O50 O 0.6844(3) -0.2143(4) 0.3875(3) 0.0294 1.0000 Uani . . . . . . . O51 O 0.8448(2) 0.1909(4) 0.3787(3) 0.0298 1.0000 Uani . . . . . . . C52 C 0.8639(4) 0.1832(6) 0.3282(4) 0.0270 1.0000 Uani . . . . . . . C53 C 0.9012(4) 0.2529(7) 0.3095(4) 0.0414 1.0000 Uani . . . . . . . C54 C 0.9230(4) 0.2496(8) 0.2582(4) 0.0441 1.0000 Uani . . . . . . . C55 C 0.9088(4) 0.1743(8) 0.2221(4) 0.0435 1.0000 Uani . . . . . . . C56 C 0.8714(4) 0.1020(8) 0.2392(4) 0.0400 1.0000 Uani . . . . . . . C57 C 0.8492(3) 0.1039(6) 0.2917(3) 0.0232 1.0000 Uani . . . . . . . C58 C 0.8114(4) 0.0243(6) 0.3041(4) 0.0274 1.0000 Uani . . . . . . . N59 N 0.7816(3) 0.0197(5) 0.3482(3) 0.0260 1.0000 Uani . . . . . . . O60 O 0.7489(2) -0.0634(4) 0.3507(2) 0.0260 1.0000 Uani . . . . . . . O61 O 0.8370(2) 0.0311(4) 0.4636(2) 0.0269 1.0000 Uani . . . . . . . C62 C 0.8903(4) -0.0061(7) 0.4480(4) 0.0361 1.0000 Uani . . . . . . . O63 O 0.8100(3) -0.2431(5) 0.3608(3) 0.0542 1.0000 Uani . . . . . . . C64 C 0.8128(5) -0.2825(9) 0.3060(5) 0.0701 1.0000 Uani . . . . . . . O65 O 0.6667(2) -0.1107(4) 0.4913(2) 0.0227 1.0000 Uani . . . . . . . C66 C 0.6205(3) -0.1791(6) 0.4963(4) 0.0262 1.0000 Uani . . . . . . . O67 O 0.6884(2) 0.2142(4) 0.5146(2) 0.0240 1.0000 Uani . . . . . . . C68 C 0.6783(4) 0.3150(6) 0.5240(4) 0.0350 1.0000 Uani . . . . . . . O69 O 0.7982(2) 0.1995(4) 0.4865(2) 0.0287 1.0000 Uani . . . . . . . O70 O 0.7480(2) 0.0322(4) 0.5402(2) 0.0225 1.0000 Uani . . . . . . . O71 O 0.7692(2) -0.1301(4) 0.4658(2) 0.0265 1.0000 Uani . . . . . . . O72 O 0.7132(2) 0.0567(4) 0.4362(2) 0.0183 1.0000 Uani . U . . . . . O73 O 0.6242(2) 0.0612(4) 0.5181(2) 0.0243 1.0000 Uani . . . . . . . O74 O 0.5229(3) 0.2415(6) 0.5729(3) 0.0598 1.0000 Uani . . . . . . . C75 C 0.5066(5) 0.3401(9) 0.5756(5) 0.0750 1.0000 Uani . . . . . . . O76 O 0.5034(3) -0.0180(4) 0.5679(3) 0.0342 1.0000 Uani . . . . . . . C77 C 0.5449(4) -0.0432(8) 0.6150(4) 0.0436 1.0000 Uani . . . . . . . O78 O 0.7193(3) -0.4498(4) 0.4424(3) 0.0432 1.0000 Uani . . . . . . . C79 C 0.6584(4) -0.4568(7) 0.4483(4) 0.0459 1.0000 Uani . . . . . . . O80 O 0.8504(3) -0.3660(5) 0.4917(4) 0.0658 1.0000 Uani . . . . . . . C81 C 0.8976(5) -0.3218(10) 0.4684(6) 0.0848 1.0000 Uani . . . . . . . Fe1 Fe 0.74439(5) -0.11845(9) 0.54312(5) 0.0244 1.0000 Uani . . . . . . . Fe2 Fe 0.82836(5) 0.09577(9) 0.54118(6) 0.0258 1.0000 Uani . . . . . . . Fe3 Fe 0.68468(5) 0.10938(9) 0.57781(5) 0.0215 1.0000 Uani . . . . . . . Fe4 Fe 0.64443(5) 0.13706(9) 0.44855(5) 0.0232 1.0000 Uani . . . . . . . Fe5 Fe 0.78205(6) 0.12619(9) 0.41332(5) 0.0267 1.0000 Uani . . . . . . . Fe6 Fe 0.70235(5) -0.08171(9) 0.41531(5) 0.0226 1.0000 Uani . U . . . . . Na1 Na 0.76449(17) -0.2991(3) 0.44641(17) 0.0405 1.0000 Uani . . . . . . . Na2 Na 0.52783(16) 0.1146(3) 0.51283(16) 0.0414 1.0000 Uani . . . . . . . H481 H 0.6859 -0.3770 0.3351 0.0389 1.0000 Uiso R . . . . . . H471 H 0.6238 -0.4372 0.2634 0.0539 1.0000 Uiso R . . . . . . H461 H 0.5443 -0.3456 0.2301 0.0559 1.0000 Uiso R . . . . . . H451 H 0.5308 -0.1899 0.2643 0.0439 1.0000 Uiso R . . . . . . H431 H 0.5539 -0.0599 0.3254 0.0350 1.0000 Uiso R . . . . . . H581 H 0.8076 -0.0284 0.2788 0.0330 1.0000 Uiso R . . . . . . H561 H 0.8617 0.0498 0.2150 0.0488 1.0000 Uiso R . . . . . . H551 H 0.9230 0.1720 0.1866 0.0489 1.0000 Uiso R . . . . . . H541 H 0.9479 0.2987 0.2484 0.0529 1.0000 Uiso R . . . . . . H531 H 0.9122 0.3045 0.3335 0.0529 1.0000 Uiso R . . . . . . H381 H 0.6584 0.3348 0.3337 0.0330 1.0000 Uiso R . . . . . . H231 H 0.7850 0.2552 0.6868 0.0338 1.0000 Uiso R . . . . . . H281 H 0.5577 0.2480 0.6834 0.0441 1.0000 Uiso R . . . . . . H271 H 0.5695 0.3468 0.7602 0.0419 1.0000 Uiso R . . . . . . H261 H 0.6609 0.3924 0.7971 0.0441 1.0000 Uiso R . . . . . . H251 H 0.7400 0.3352 0.7571 0.0309 1.0000 Uiso R . . . . . . H131 H 0.9134 -0.1018 0.6343 0.0478 1.0000 Uiso R . . . . . . H151 H 0.9978 -0.0416 0.6877 0.0669 1.0000 Uiso R . . . . . . H161 H 1.0675 0.0782 0.7064 0.0798 1.0000 Uiso R . . . . . . H171 H 1.0651 0.2209 0.6559 0.0649 1.0000 Uiso R . . . . . . H181 H 0.9931 0.2480 0.5837 0.0559 1.0000 Uiso R . . . . . . H81 H 0.6727 -0.1441 0.6834 0.0300 1.0000 Uiso R . . . . . . H31 H 0.7414 -0.4435 0.5644 0.0399 1.0000 Uiso R . . . . . . H41 H 0.7188 -0.5370 0.6391 0.0479 1.0000 Uiso R . . . . . . H51 H 0.6878 -0.4657 0.7192 0.0459 1.0000 Uiso R . . . . . . H61 H 0.6745 -0.2984 0.7206 0.0408 1.0000 Uiso R . . . . . . H331 H 0.4723 0.2845 0.4440 0.0339 1.0000 Uiso R . . . . . . H341 H 0.4294 0.3995 0.3830 0.0530 1.0000 Uiso R . . . . . . H351 H 0.4798 0.4721 0.3154 0.0508 1.0000 Uiso R . . . . . . H361 H 0.5720 0.4222 0.3050 0.0429 1.0000 Uiso R . . . . . . H741 H 0.5568 0.2309 0.5839 0.0850 1.0000 Uiso R . . . . . . H753 H 0.4710 0.3509 0.5528 0.1049 1.0000 Uiso R . . . . . . H752 H 0.5016 0.3580 0.6137 0.1050 1.0000 Uiso R . . . . . . H751 H 0.5365 0.3805 0.5622 0.1049 1.0000 Uiso R . . . . . . H631 H 0.7911 -0.1926 0.3530 0.0779 1.0000 Uiso R . . . . . . H801 H 0.8439 -0.4221 0.5022 0.0901 1.0000 Uiso R . . . . . . H811 H 0.9331 -0.3413 0.4893 0.1160 1.0000 Uiso R . . . . . . H813 H 0.8938 -0.2513 0.4696 0.1160 1.0000 Uiso R . . . . . . H812 H 0.8979 -0.3428 0.4299 0.1160 1.0000 Uiso R . . . . . . H781 H 0.7247 -0.4920 0.4187 0.0630 1.0000 Uiso R . . . . . . H792 H 0.6451 -0.5222 0.4395 0.0660 1.0000 Uiso R . . . . . . H793 H 0.6515 -0.4410 0.4864 0.0660 1.0000 Uiso R . . . . . . H791 H 0.6381 -0.4110 0.4233 0.0661 1.0000 Uiso R . . . . . . H771 H 0.5358 -0.1062 0.6301 0.0661 1.0000 Uiso R . . . . . . H772 H 0.5442 0.0058 0.6442 0.0659 1.0000 Uiso R . . . . . . H773 H 0.5829 -0.0453 0.6022 0.0661 1.0000 Uiso R . . . . . . H621 H 0.9172 0.0465 0.4449 0.0551 1.0000 Uiso R . . . . . . H623 H 0.9064 -0.0515 0.4760 0.0549 1.0000 Uiso R . . . . . . H622 H 0.8845 -0.0392 0.4126 0.0550 1.0000 Uiso R . . . . . . H683 H 0.6376 0.3276 0.5200 0.0500 1.0000 Uiso R . . . . . . H682 H 0.6934 0.3336 0.5614 0.0501 1.0000 Uiso R . . . . . . H681 H 0.6962 0.3546 0.4972 0.0500 1.0000 Uiso R . . . . . . H641 H 0.8297 -0.3469 0.3082 0.0979 1.0000 Uiso R . . . . . . H642 H 0.8357 -0.2398 0.2845 0.0980 1.0000 Uiso R . . . . . . H643 H 0.7746 -0.2869 0.2873 0.0980 1.0000 Uiso R . . . . . . H663 H 0.6350 -0.2448 0.4949 0.0349 1.0000 Uiso R . . . . . . H661 H 0.5913 -0.1707 0.4656 0.0350 1.0000 Uiso R . . . . . . H662 H 0.6029 -0.1705 0.5311 0.0350 1.0000 Uiso R . . . . . . H691 H 0.8006 0.2546 0.4999 0.0421 1.0000 Uiso R . . . . . . H711 H 0.7973 -0.0947 0.4607 0.0372 1.0000 Uiso R . . . . . . H731 H 0.6237 0.0010 0.5135 0.0360 1.0000 Uiso R . . . . . . H761 H 0.4714 -0.0278 0.5805 0.0373 1.0000 Uiso R . . . . . . H701 H 0.7364 0.0401 0.5057 0.0292 1.0000 Uiso 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 O1 0.043(4) 0.026(4) 0.025(4) 0.009(3) 0.011(3) 0.005(3) C2 0.037(5) 0.019(5) 0.019(5) 0.008(4) -0.005(4) -0.002(4) C3 0.043(6) 0.020(5) 0.043(6) 0.009(4) 0.015(5) -0.001(4) C4 0.055(7) 0.016(5) 0.049(7) 0.003(5) -0.001(6) 0.003(5) C5 0.049(7) 0.033(6) 0.028(6) 0.014(4) -0.001(5) 0.007(5) C6 0.046(6) 0.026(6) 0.030(6) 0.006(4) 0.006(5) 0.004(5) C7 0.034(5) 0.020(5) 0.025(5) 0.001(4) 0.015(4) -0.008(4) C8 0.034(5) 0.019(5) 0.022(5) 0.004(4) 0.001(4) 0.000(4) N9 0.033(4) 0.014(4) 0.035(5) 0.009(3) 0.011(4) -0.005(3) O10 0.050(4) 0.012(3) 0.034(4) 0.006(3) 0.014(3) 0.004(3) O11 0.034(4) 0.031(4) 0.049(5) 0.015(3) 0.005(3) -0.001(3) N12 0.020(4) 0.022(4) 0.045(5) 0.000(4) 0.006(4) -0.003(3) C13 0.021(5) 0.035(6) 0.060(8) 0.004(5) -0.008(5) -0.004(4) C14 0.013(5) 0.028(6) 0.087(9) 0.002(6) -0.001(5) 0.004(4) C15 0.022(5) 0.043(7) 0.109(11) -0.007(7) -0.004(6) 0.011(5) C16 0.019(5) 0.081(10) 0.096(11) -0.009(8) -0.013(6) 0.018(6) C17 0.028(5) 0.027(5) 0.108(8) -0.012(6) 0.005(5) -0.007(4) C18 0.018(4) 0.037(5) 0.086(7) -0.008(5) 0.004(4) -0.001(4) C19 0.017(4) 0.034(5) 0.075(7) -0.007(5) 0.010(5) 0.001(4) O20 0.032(4) 0.042(4) 0.047(5) 0.002(3) 0.018(3) -0.010(3) O21 0.030(4) 0.040(4) 0.025(4) -0.002(3) 0.007(3) 0.001(3) N22 0.021(4) 0.027(4) 0.022(4) 0.003(3) 0.005(3) -0.009(3) C23 0.023(5) 0.030(6) 0.032(6) 0.010(4) -0.007(4) -0.003(4) C24 0.030(5) 0.014(5) 0.022(5) 0.004(4) 0.003(4) -0.001(4) C25 0.045(6) 0.018(5) 0.018(5) 0.004(4) 0.004(4) -0.002(4) C26 0.062(7) 0.030(6) 0.020(5) 0.008(4) 0.004(5) 0.013(5) C27 0.037(6) 0.044(6) 0.024(6) 0.002(5) 0.006(5) 0.007(5) C28 0.039(6) 0.027(6) 0.048(7) 0.003(5) 0.004(5) 0.003(5) C29 0.041(6) 0.016(5) 0.019(5) -0.001(4) 0.001(4) 0.003(4) O30 0.026(3) 0.022(3) 0.029(4) -0.001(3) 0.002(3) 0.001(3) O31 0.032(3) 0.021(3) 0.034(4) 0.007(3) 0.007(3) 0.004(3) C32 0.027(4) 0.011(4) 0.035(5) -0.007(3) 0.002(4) 0.008(3) C33 0.044(6) 0.024(5) 0.019(5) 0.007(4) 0.006(4) 0.004(4) C34 0.035(6) 0.043(7) 0.056(8) 0.001(6) -0.009(5) -0.001(5) C35 0.048(7) 0.035(6) 0.046(7) 0.008(5) -0.006(5) 0.009(5) C36 0.050(6) 0.033(6) 0.031(6) 0.008(5) 0.002(5) -0.008(5) C37 0.035(5) 0.021(5) 0.020(5) -0.001(4) -0.007(4) -0.008(4) C38 0.045(6) 0.016(5) 0.020(5) -0.002(4) 0.005(4) -0.009(4) N39 0.028(4) 0.014(4) 0.023(4) 0.000(3) 0.001(3) -0.004(3) O40 0.029(3) 0.023(3) 0.027(4) 0.004(3) 0.009(3) -0.003(3) O41 0.026(3) 0.015(3) 0.032(4) 0.001(3) -0.003(3) 0.001(3) N42 0.024(4) 0.020(4) 0.021(4) 0.001(3) 0.001(3) -0.002(3) C43 0.033(5) 0.027(5) 0.034(6) 0.007(4) 0.010(4) -0.008(4) C44 0.049(6) 0.026(5) 0.019(5) 0.000(4) 0.015(4) -0.015(5) C45 0.045(6) 0.047(7) 0.023(6) -0.002(5) -0.001(5) -0.008(5) C46 0.055(7) 0.060(8) 0.026(6) -0.018(5) 0.019(5) -0.025(6) C47 0.069(8) 0.033(6) 0.031(6) -0.005(5) 0.020(6) -0.007(6) C48 0.045(6) 0.020(5) 0.030(6) -0.001(4) 0.011(5) -0.008(4) C49 0.039(6) 0.019(5) 0.027(6) 0.007(4) 0.012(5) -0.006(4) O50 0.039(4) 0.019(3) 0.030(4) 0.005(3) -0.004(3) -0.006(3) O51 0.028(3) 0.032(4) 0.030(4) 0.005(3) 0.008(3) -0.008(3) C52 0.028(5) 0.028(5) 0.025(5) 0.013(4) 0.001(4) 0.005(4) C53 0.050(7) 0.041(6) 0.035(6) 0.000(5) 0.008(5) -0.005(5) C54 0.040(6) 0.057(7) 0.039(7) 0.013(6) 0.026(5) -0.002(5) C55 0.036(6) 0.057(7) 0.042(7) 0.013(6) 0.027(5) 0.010(5) C56 0.039(6) 0.053(7) 0.029(6) 0.006(5) 0.003(5) 0.004(5) C57 0.024(4) 0.029(5) 0.018(5) 0.013(4) 0.003(4) 0.007(4) C58 0.037(5) 0.024(5) 0.021(5) 0.005(4) 0.001(4) 0.015(4) N59 0.028(4) 0.027(4) 0.023(4) 0.002(3) 0.001(3) 0.004(3) O60 0.035(4) 0.016(3) 0.029(4) -0.006(3) 0.013(3) -0.007(3) O61 0.025(3) 0.025(3) 0.031(4) 0.003(3) 0.010(3) 0.002(3) C62 0.025(5) 0.042(6) 0.044(7) 0.000(5) 0.016(5) 0.002(4) O63 0.058(5) 0.046(5) 0.059(6) 0.002(4) 0.009(4) 0.014(4) C64 0.066(9) 0.094(11) 0.052(9) -0.025(7) 0.012(7) 0.015(8) O65 0.031(3) 0.013(3) 0.025(3) 0.003(2) 0.006(3) -0.007(3) C66 0.032(5) 0.020(5) 0.026(5) 0.001(4) 0.000(4) -0.010(4) O67 0.039(4) 0.012(3) 0.021(3) -0.002(2) 0.002(3) 0.000(3) C68 0.048(6) 0.025(5) 0.031(6) 0.002(4) -0.005(5) -0.003(5) O69 0.045(4) 0.013(3) 0.028(4) 0.005(3) 0.005(3) -0.007(3) O70 0.032(3) 0.020(3) 0.017(3) 0.006(2) 0.007(3) 0.003(3) O71 0.025(3) 0.024(3) 0.032(4) 0.005(3) 0.010(3) -0.010(3) O72 0.031(3) 0.013(2) 0.011(2) 0.005(2) 0.000(2) 0.000(2) O73 0.027(3) 0.018(3) 0.028(4) -0.001(3) 0.002(3) -0.008(3) O74 0.052(5) 0.073(6) 0.053(6) -0.030(4) -0.005(4) 0.000(4) C75 0.083(10) 0.085(10) 0.051(9) -0.031(7) -0.029(7) 0.041(8) O76 0.024(3) 0.046(4) 0.033(4) 0.009(3) 0.000(3) 0.003(3) C77 0.032(6) 0.059(7) 0.040(7) 0.005(5) 0.001(5) 0.000(5) O78 0.051(5) 0.030(4) 0.048(5) -0.001(3) 0.005(4) 0.002(3) C79 0.062(8) 0.027(6) 0.049(7) 0.002(5) 0.004(6) 0.004(5) O80 0.053(5) 0.031(5) 0.109(8) 0.011(4) -0.016(5) -0.008(4) C81 0.049(8) 0.098(12) 0.103(13) -0.006(9) -0.014(8) -0.011(8) Fe1 0.0311(7) 0.0171(7) 0.0255(8) 0.0045(5) 0.0049(6) -0.0006(6) Fe2 0.0264(7) 0.0228(7) 0.0289(8) 0.0063(6) 0.0062(6) -0.0014(6) Fe3 0.0266(7) 0.0157(7) 0.0225(7) 0.0002(5) 0.0035(5) -0.0015(5) Fe4 0.0287(7) 0.0165(7) 0.0247(7) 0.0041(5) 0.0042(6) -0.0008(5) Fe5 0.0336(8) 0.0230(7) 0.0246(8) 0.0021(6) 0.0083(6) -0.0052(6) Fe6 0.0280(7) 0.0185(7) 0.0212(7) 0.0004(5) 0.0015(6) -0.0019(5) Na1 0.047(2) 0.022(2) 0.053(3) 0.0020(18) 0.010(2) -0.0006(18) Na2 0.044(2) 0.043(2) 0.039(2) 0.0100(19) 0.0133(19) 0.011(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.18042(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C2 . 1.315(9) yes O1 . Fe1 . 1.910(6) yes O1 . Na1 . 2.742(7) yes C2 . C3 . 1.416(11) yes C2 . C7 . 1.418(11) yes C3 . C4 . 1.374(12) yes C3 . H31 . 0.925 no C4 . C5 . 1.380(13) yes C4 . H41 . 0.923 no C5 . C6 . 1.368(12) yes C5 . H51 . 0.923 no C6 . C7 . 1.372(11) yes C6 . H61 . 0.927 no C7 . C8 . 1.449(11) yes C8 . N9 . 1.292(10) yes C8 . H81 . 0.927 no N9 . O10 . 1.368(8) yes N9 . Fe1 . 2.106(7) yes O10 . Fe3 . 1.959(6) yes O11 . N12 . 1.381(8) yes O11 . Fe1 . 1.964(6) yes N12 . C13 . 1.279(10) yes N12 . Fe2 . 2.140(7) yes C13 . C14 . 1.426(12) yes C13 . H131 . 0.929 no C14 . C15 . 1.407(14) yes C14 . C19 . 1.415(13) yes C15 . C16 . 1.386(14) yes C15 . H151 . 0.930 no C16 . C17 . 1.361(15) yes C16 . H161 . 0.930 no C17 . C18 . 1.384(14) yes C17 . H171 . 0.929 no C18 . C19 . 1.398(12) yes C18 . H181 . 0.928 no C19 . O20 . 1.357(11) yes O20 . Fe2 . 1.919(6) yes O21 . N22 . 1.367(8) yes O21 . Fe2 . 1.960(6) yes N22 . C23 . 1.286(11) yes N22 . Fe3 . 2.121(7) yes C23 . C24 . 1.452(11) yes C23 . H231 . 0.924 no C24 . C25 . 1.386(11) yes C24 . C29 . 1.400(11) yes C25 . C26 . 1.352(12) yes C25 . H251 . 0.927 no C26 . C27 . 1.375(12) yes C26 . H261 . 0.929 no C27 . C28 . 1.351(12) yes C27 . H271 . 0.927 no C28 . C29 . 1.407(12) yes C28 . H281 . 0.926 no C29 . O30 . 1.339(9) yes O30 . Fe3 . 1.915(6) yes O31 . C32 . 1.336(9) yes O31 . Fe4 . 1.946(6) yes O31 . Na2 . 2.373(7) yes C32 . C33 . 1.408(11) yes C32 . C37 . 1.383(11) yes C33 . C34 . 1.384(12) yes C33 . H331 . 0.927 no C34 . C35 . 1.365(13) yes C34 . H341 . 0.928 no C35 . C36 . 1.356(12) yes C35 . H351 . 0.927 no C36 . C37 . 1.405(12) yes C36 . H361 . 0.932 no C37 . C38 . 1.467(12) yes C38 . N39 . 1.284(10) yes C38 . H381 . 0.932 no N39 . O40 . 1.379(8) yes N39 . Fe4 . 2.087(7) yes O40 . Fe5 . 2.001(6) yes O41 . N42 . 1.380(8) yes O41 . Fe4 . 2.022(6) yes N42 . C43 . 1.276(10) yes N42 . Fe6 . 2.114(7) yes C43 . C44 . 1.439(12) yes C43 . H431 . 0.932 no C44 . C45 . 1.379(12) yes C44 . C49 . 1.442(12) yes C45 . C46 . 1.384(13) yes C45 . H451 . 0.926 no C46 . C47 . 1.371(14) yes C46 . H461 . 0.926 no C47 . C48 . 1.361(12) yes C47 . H471 . 0.929 no C48 . C49 . 1.389(11) yes C48 . H481 . 0.929 no C49 . O50 . 1.334(10) yes O50 . Fe6 . 1.949(6) yes O50 . Na1 . 2.499(7) yes O51 . C52 . 1.320(10) yes O51 . Fe5 . 1.943(6) yes C52 . C53 . 1.380(12) yes C52 . C57 . 1.406(12) yes C53 . C54 . 1.361(12) yes C53 . H531 . 0.923 no C54 . C55 . 1.356(13) yes C54 . H541 . 0.925 no C55 . C56 . 1.393(12) yes C55 . H551 . 0.935 no C56 . C57 . 1.392(11) yes C56 . H561 . 0.928 no C57 . C58 . 1.435(11) yes C58 . N59 . 1.308(10) yes C58 . H581 . 0.934 no N59 . O60 . 1.362(8) yes N59 . Fe5 . 2.117(7) yes O60 . Fe6 . 1.970(6) yes O61 . C62 . 1.414(9) yes O61 . Fe2 . 2.067(6) yes O61 . Fe5 . 2.106(6) yes C62 . H621 . 0.955 no C62 . H623 . 0.958 no C62 . H622 . 0.952 no O63 . C64 . 1.414(12) yes O63 . Na1 . 2.492(8) yes O63 . H631 . 0.824 no C64 . H641 . 0.957 no C64 . H642 . 0.963 no C64 . H643 . 0.955 no O65 . C66 . 1.430(8) yes O65 . Fe1 . 2.088(6) yes O65 . Fe6 . 2.090(5) yes C66 . H663 . 0.955 no C66 . H661 . 0.956 no C66 . H662 . 0.960 no O67 . C68 . 1.410(9) yes O67 . Fe3 . 2.076(5) yes O67 . Fe4 . 2.075(6) yes C68 . H683 . 0.953 no C68 . H682 . 0.958 no C68 . H681 . 0.957 no O69 . Fe2 . 1.998(6) yes O69 . Fe5 . 2.008(6) yes O69 . H691 . 0.813 no O70 . Fe1 . 2.048(5) yes O70 . Fe2 . 2.049(5) yes O70 . Fe3 . 2.070(5) yes O70 . H701 . 0.845 no O71 . Fe1 . 1.981(6) yes O71 . Fe6 . 1.981(6) yes O71 . Na1 . 2.340(6) yes O71 . H711 . 0.827 no O72 . Fe4 . 1.973(5) yes O72 . Fe5 . 1.971(5) yes O72 . Fe6 . 1.954(5) yes O73 . Fe3 . 2.010(5) yes O73 . Fe4 . 2.038(5) yes O73 . Na2 . 2.338(6) yes O73 . H731 . 0.825 no O74 . C75 . 1.393(12) yes O74 . Na2 . 2.247(8) yes O74 . H741 . 0.819 no C75 . H753 . 0.955 no C75 . H752 . 0.954 no C75 . H751 . 0.959 no O76 . Na2 2_656 2.380(7) yes O76 . C77 . 1.447(10) yes O76 . Na2 . 2.324(7) yes O76 . H761 . 0.835 no C77 . H771 . 0.959 no C77 . H772 . 0.962 no C77 . H773 . 0.956 no O78 . C79 . 1.431(10) yes O78 . Na1 . 2.297(7) yes O78 . H781 . 0.820 no C79 . H792 . 0.958 no C79 . H793 . 0.958 no C79 . H791 . 0.953 no O80 . C81 . 1.406(12) yes O80 . Na1 . 2.356(8) yes O80 . H801 . 0.819 no C81 . H811 . 0.957 no C81 . H813 . 0.961 no C81 . H812 . 0.958 no Fe1 . Na1 . 3.421(4) yes Fe4 . Fe6 . 3.3812(17) yes Fe4 . Na2 . 3.235(4) yes Fe5 . Fe6 . 3.3745(17) yes Fe6 . Na1 . 3.336(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . O1 . Fe1 . 131.7(6) yes C2 . O1 . Na1 . 135.4(5) yes Fe1 . O1 . Na1 . 92.9(2) yes O1 . C2 . C3 . 119.4(8) yes O1 . C2 . C7 . 123.3(8) yes C3 . C2 . C7 . 117.2(8) yes C2 . C3 . C4 . 120.5(9) yes C2 . C3 . H31 . 119.5 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 121.8(9) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 119.4 no C4 . C5 . C6 . 117.7(9) yes C4 . C5 . H51 . 120.9 no C6 . C5 . H51 . 121.4 no C5 . C6 . C7 . 123.3(9) yes C5 . C6 . H61 . 118.5 no C7 . C6 . H61 . 118.2 no C2 . C7 . C6 . 119.4(8) yes C2 . C7 . C8 . 123.6(8) yes C6 . C7 . C8 . 117.0(8) yes C7 . C8 . N9 . 126.3(8) yes C7 . C8 . H81 . 116.5 no N9 . C8 . H81 . 117.2 no C8 . N9 . O10 . 115.2(7) yes C8 . N9 . Fe1 . 124.1(6) yes O10 . N9 . Fe1 . 120.6(5) yes N9 . O10 . Fe3 . 122.3(5) yes N12 . O11 . Fe1 . 123.6(5) yes O11 . N12 . C13 . 116.5(7) yes O11 . N12 . Fe2 . 118.6(5) yes C13 . N12 . Fe2 . 124.6(6) yes N12 . C13 . C14 . 126.4(9) yes N12 . C13 . H131 . 116.3 no C14 . C13 . H131 . 117.3 no C13 . C14 . C15 . 118.3(10) yes C13 . C14 . C19 . 123.4(9) yes C15 . C14 . C19 . 118.3(9) yes C14 . C15 . C16 . 120.0(11) yes C14 . C15 . H151 . 120.5 no C16 . C15 . H151 . 119.5 no C15 . C16 . C17 . 121.2(11) yes C15 . C16 . H161 . 119.7 no C17 . C16 . H161 . 119.1 no C16 . C17 . C18 . 120.6(10) yes C16 . C17 . H171 . 120.0 no C18 . C17 . H171 . 119.3 no C17 . C18 . C19 . 119.7(11) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.9 no C14 . C19 . C18 . 120.1(10) yes C14 . C19 . O20 . 121.9(9) yes C18 . C19 . O20 . 118.0(10) yes C19 . O20 . Fe2 . 129.3(6) yes N22 . O21 . Fe2 . 123.1(5) yes O21 . N22 . C23 . 116.0(7) yes O21 . N22 . Fe3 . 120.3(5) yes C23 . N22 . Fe3 . 123.6(6) yes N22 . C23 . C24 . 128.0(8) yes N22 . C23 . H231 . 115.7 no C24 . C23 . H231 . 116.3 no C23 . C24 . C25 . 117.6(8) yes C23 . C24 . C29 . 123.1(8) yes C25 . C24 . C29 . 119.3(8) yes C24 . C25 . C26 . 121.8(9) yes C24 . C25 . H251 . 119.1 no C26 . C25 . H251 . 119.1 no C25 . C26 . C27 . 119.7(9) yes C25 . C26 . H261 . 120.6 no C27 . C26 . H261 . 119.8 no C26 . C27 . C28 . 120.2(9) yes C26 . C27 . H271 . 120.0 no C28 . C27 . H271 . 119.8 no C27 . C28 . C29 . 121.7(9) yes C27 . C28 . H281 . 118.9 no C29 . C28 . H281 . 119.3 no C28 . C29 . C24 . 117.3(8) yes C28 . C29 . O30 . 120.3(8) yes C24 . C29 . O30 . 122.4(8) yes C29 . O30 . Fe3 . 132.9(5) yes C32 . O31 . Fe4 . 131.1(5) yes C32 . O31 . Na2 . 129.9(5) yes Fe4 . O31 . Na2 . 96.5(2) yes O31 . C32 . C33 . 117.5(8) yes O31 . C32 . C37 . 123.8(8) yes C33 . C32 . C37 . 118.7(8) yes C32 . C33 . C34 . 120.0(9) yes C32 . C33 . H331 . 120.4 no C34 . C33 . H331 . 119.6 no C33 . C34 . C35 . 121.4(10) yes C33 . C34 . H341 . 119.2 no C35 . C34 . H341 . 119.4 no C34 . C35 . C36 . 118.5(10) yes C34 . C35 . H351 . 120.5 no C36 . C35 . H351 . 121.0 no C35 . C36 . C37 . 122.5(9) yes C35 . C36 . H361 . 118.2 no C37 . C36 . H361 . 119.2 no C36 . C37 . C32 . 118.7(9) yes C36 . C37 . C38 . 118.1(8) yes C32 . C37 . C38 . 123.2(8) yes C37 . C38 . N39 . 125.8(8) yes C37 . C38 . H381 . 117.0 no N39 . C38 . H381 . 117.2 no C38 . N39 . O40 . 115.8(7) yes C38 . N39 . Fe4 . 125.9(6) yes O40 . N39 . Fe4 . 118.0(5) yes N39 . O40 . Fe5 . 120.2(4) yes N42 . O41 . Fe4 . 120.0(4) yes O41 . N42 . C43 . 115.8(7) yes O41 . N42 . Fe6 . 117.8(5) yes C43 . N42 . Fe6 . 126.3(6) yes N42 . C43 . C44 . 126.0(9) yes N42 . C43 . H431 . 117.5 no C44 . C43 . H431 . 116.5 no C43 . C44 . C45 . 118.2(9) yes C43 . C44 . C49 . 123.4(9) yes C45 . C44 . C49 . 118.5(9) yes C44 . C45 . C46 . 121.5(10) yes C44 . C45 . H451 . 119.0 no C46 . C45 . H451 . 119.6 no C45 . C46 . C47 . 120.4(10) yes C45 . C46 . H461 . 119.4 no C47 . C46 . H461 . 120.2 no C46 . C47 . C48 . 119.3(10) yes C46 . C47 . H471 . 119.9 no C48 . C47 . H471 . 120.8 no C47 . C48 . C49 . 123.1(10) yes C47 . C48 . H481 . 118.5 no C49 . C48 . H481 . 118.4 no C44 . C49 . C48 . 117.3(9) yes C44 . C49 . O50 . 121.8(8) yes C48 . C49 . O50 . 120.9(9) yes C49 . O50 . Fe6 . 131.2(5) yes C49 . O50 . Na1 . 131.6(5) yes Fe6 . O50 . Na1 . 96.4(2) yes C52 . O51 . Fe5 . 132.5(6) yes O51 . C52 . C53 . 120.7(9) yes O51 . C52 . C57 . 122.5(8) yes C53 . C52 . C57 . 116.8(8) yes C52 . C53 . C54 . 124.0(10) yes C52 . C53 . H531 . 117.8 no C54 . C53 . H531 . 118.2 no C53 . C54 . C55 . 120.1(10) yes C53 . C54 . H541 . 119.6 no C55 . C54 . H541 . 120.3 no C54 . C55 . C56 . 117.9(9) yes C54 . C55 . H551 . 120.8 no C56 . C55 . H551 . 121.3 no C55 . C56 . C57 . 122.6(10) yes C55 . C56 . H561 . 118.6 no C57 . C56 . H561 . 118.7 no C52 . C57 . C56 . 118.5(8) yes C52 . C57 . C58 . 124.7(8) yes C56 . C57 . C58 . 116.8(8) yes C57 . C58 . N59 . 125.1(8) yes C57 . C58 . H581 . 118.0 no N59 . C58 . H581 . 116.9 no C58 . N59 . O60 . 114.3(7) yes C58 . N59 . Fe5 . 125.8(6) yes O60 . N59 . Fe5 . 119.9(5) yes N59 . O60 . Fe6 . 119.0(4) yes C62 . O61 . Fe2 . 122.9(5) yes C62 . O61 . Fe5 . 124.5(5) yes Fe2 . O61 . Fe5 . 98.2(2) yes O61 . C62 . H621 . 110.1 no O61 . C62 . H623 . 109.9 no H621 . C62 . H623 . 108.7 no O61 . C62 . H622 . 110.1 no H621 . C62 . H622 . 109.0 no H623 . C62 . H622 . 109.0 no C64 . O63 . Na1 . 134.0(7) yes C64 . O63 . H631 . 100.1 no Na1 . O63 . H631 . 100.5 no O63 . C64 . H641 . 110.4 no O63 . C64 . H642 . 109.6 no H641 . C64 . H642 . 109.7 no O63 . C64 . H643 . 109.4 no H641 . C64 . H643 . 108.9 no H642 . C64 . H643 . 108.8 no C66 . O65 . Fe1 . 121.9(5) yes C66 . O65 . Fe6 . 123.5(5) yes Fe1 . O65 . Fe6 . 97.6(2) yes O65 . C66 . H663 . 109.6 no O65 . C66 . H661 . 109.9 no H663 . C66 . H661 . 108.2 no O65 . C66 . H662 . 111.7 no H663 . C66 . H662 . 108.7 no H661 . C66 . H662 . 108.6 no C68 . O67 . Fe3 . 122.1(5) yes C68 . O67 . Fe4 . 122.1(5) yes Fe3 . O67 . Fe4 . 98.7(2) yes O67 . C68 . H683 . 109.7 no O67 . C68 . H682 . 110.6 no H683 . C68 . H682 . 108.6 no O67 . C68 . H681 . 110.6 no H683 . C68 . H681 . 108.4 no H682 . C68 . H681 . 108.9 no Fe2 . O69 . Fe5 . 103.9(3) yes Fe2 . O69 . H691 . 112.8 no Fe5 . O69 . H691 . 142.7 no Fe1 . O70 . Fe2 . 117.4(3) yes Fe1 . O70 . Fe3 . 117.3(2) yes Fe2 . O70 . Fe3 . 117.4(3) yes Fe1 . O70 . H701 . 98.6 no Fe2 . O70 . H701 . 99.6 no Fe3 . O70 . H701 . 100.4 no Fe1 . O71 . Fe6 . 105.0(2) yes Fe1 . O71 . Na1 . 104.4(2) yes Fe6 . O71 . Na1 . 100.7(3) yes Fe1 . O71 . H711 . 112.9 no Fe6 . O71 . H711 . 107.5 no Na1 . O71 . H711 . 124.3 no Fe4 . O72 . Fe5 . 117.4(2) yes Fe4 . O72 . Fe6 . 118.8(3) yes Fe5 . O72 . Fe6 . 118.6(3) yes Fe3 . O73 . Fe4 . 102.2(2) yes Fe3 . O73 . Na2 . 122.5(3) yes Fe4 . O73 . Na2 . 95.1(2) yes Fe3 . O73 . H731 . 114.7 no Fe4 . O73 . H731 . 113.3 no Na2 . O73 . H731 . 107.3 no C75 . O74 . Na2 . 142.8(7) yes C75 . O74 . H741 . 114.1 no Na2 . O74 . H741 . 88.1 no O74 . C75 . H753 . 110.1 no O74 . C75 . H752 . 110.2 no H753 . C75 . H752 . 108.9 no O74 . C75 . H751 . 109.1 no H753 . C75 . H751 . 109.6 no H752 . C75 . H751 . 109.0 no Na2 2_656 O76 . C77 . 128.7(6) yes Na2 2_656 O76 . Na2 . 92.5(3) yes C77 . O76 . Na2 . 116.1(5) yes Na2 2_656 O76 . H761 . 89.3 no C77 . O76 . H761 . 103.4 no Na2 . O76 . H761 . 126.5 no O76 . C77 . H771 . 110.4 no O76 . C77 . H772 . 110.0 no H771 . C77 . H772 . 109.1 no O76 . C77 . H773 . 109.0 no H771 . C77 . H773 . 109.3 no H772 . C77 . H773 . 109.1 no C79 . O78 . Na1 . 120.2(5) yes C79 . O78 . H781 . 103.6 no Na1 . O78 . H781 . 123.6 no O78 . C79 . H792 . 109.9 no O78 . C79 . H793 . 109.2 no H792 . C79 . H793 . 109.6 no O78 . C79 . H791 . 109.2 no H792 . C79 . H791 . 109.8 no H793 . C79 . H791 . 109.1 no C81 . O80 . Na1 . 108.0(7) yes C81 . O80 . H801 . 133.5 no Na1 . O80 . H801 . 109.1 no O80 . C81 . H811 . 109.8 no O80 . C81 . H813 . 109.6 no H811 . C81 . H813 . 109.7 no O80 . C81 . H812 . 108.8 no H811 . C81 . H812 . 109.6 no H813 . C81 . H812 . 109.4 no N9 . Fe1 . O65 . 91.4(2) yes N9 . Fe1 . O70 . 84.2(2) yes O65 . Fe1 . O70 . 88.0(2) yes N9 . Fe1 . O71 . 167.3(3) yes O65 . Fe1 . O71 . 76.3(2) yes O70 . Fe1 . O71 . 91.8(2) yes N9 . Fe1 . O11 . 95.6(3) yes O65 . Fe1 . O11 . 171.6(2) yes O70 . Fe1 . O11 . 88.0(2) yes O71 . Fe1 . O11 . 96.4(3) yes N9 . Fe1 . O1 . 89.3(3) yes O65 . Fe1 . O1 . 92.7(2) yes O70 . Fe1 . O1 . 173.5(2) yes O71 . Fe1 . O1 . 94.6(2) yes O11 . Fe1 . O1 . 92.1(3) yes N9 . Fe1 . Na1 . 140.0(2) yes O65 . Fe1 . Na1 . 78.64(16) yes O70 . Fe1 . Na1 . 133.17(17) yes O71 . Fe1 . Na1 . 41.49(17) yes O11 . Fe1 . Na1 . 98.9(2) yes O1 . Fe1 . Na1 . 53.20(19) yes N12 . Fe2 . O61 . 91.2(3) yes N12 . Fe2 . O70 . 85.0(2) yes O61 . Fe2 . O70 . 88.4(2) yes N12 . Fe2 . O69 . 167.8(3) yes O61 . Fe2 . O69 . 77.0(2) yes O70 . Fe2 . O69 . 91.5(2) yes N12 . Fe2 . O21 . 95.5(3) yes O61 . Fe2 . O21 . 172.0(2) yes O70 . Fe2 . O21 . 87.7(2) yes O69 . Fe2 . O21 . 96.0(2) yes N12 . Fe2 . O20 . 86.4(3) yes O61 . Fe2 . O20 . 94.6(3) yes O70 . Fe2 . O20 . 171.0(3) yes O69 . Fe2 . O20 . 97.5(3) yes O21 . Fe2 . O20 . 90.3(3) yes N22 . Fe3 . O67 . 88.8(2) yes N22 . Fe3 . O70 . 84.8(2) yes O67 . Fe3 . O70 . 87.5(2) yes N22 . Fe3 . O73 . 165.7(2) yes O67 . Fe3 . O73 . 77.6(2) yes O70 . Fe3 . O73 . 90.3(2) yes N22 . Fe3 . O10 . 94.0(3) yes O67 . Fe3 . O10 . 172.5(2) yes O70 . Fe3 . O10 . 85.9(2) yes O73 . Fe3 . O10 . 99.0(2) yes N22 . Fe3 . O30 . 88.2(3) yes O67 . Fe3 . O30 . 95.2(2) yes O70 . Fe3 . O30 . 172.4(2) yes O73 . Fe3 . O30 . 97.1(2) yes O10 . Fe3 . O30 . 91.8(2) yes N39 . Fe4 . O67 . 89.9(2) yes N39 . Fe4 . O73 . 166.8(2) yes O67 . Fe4 . O73 . 77.0(2) yes N39 . Fe4 . O41 . 98.3(2) yes O67 . Fe4 . O41 . 171.7(2) yes O73 . Fe4 . O41 . 94.8(2) yes N39 . Fe4 . O72 . 87.5(2) yes O67 . Fe4 . O72 . 92.5(2) yes O73 . Fe4 . O72 . 95.1(2) yes O41 . Fe4 . O72 . 88.3(2) yes N39 . Fe4 . O31 . 87.7(3) yes O67 . Fe4 . O31 . 95.2(2) yes O73 . Fe4 . O31 . 91.3(2) yes O41 . Fe4 . O31 . 84.8(2) yes O72 . Fe4 . O31 . 170.9(2) yes N39 . Fe4 . Fe6 . 105.51(19) yes O67 . Fe4 . Fe6 . 116.21(16) yes O73 . Fe4 . Fe6 . 82.57(16) yes O41 . Fe4 . Fe6 . 61.98(16) yes O72 . Fe4 . Fe6 . 30.42(15) yes N39 . Fe4 . Na2 . 134.5(2) yes O67 . Fe4 . Na2 . 93.67(17) yes O73 . Fe4 . Na2 . 46.05(16) yes O41 . Fe4 . Na2 . 80.30(18) yes O72 . Fe4 . Na2 . 137.48(16) yes O31 . Fe4 . Fe6 . 145.37(18) yes O31 . Fe4 . Na2 . 46.79(18) yes Fe6 . Fe4 . Na2 . 113.14(8) yes N59 . Fe5 . O61 . 87.6(2) yes N59 . Fe5 . O69 . 163.6(3) yes O61 . Fe5 . O69 . 76.0(2) yes N59 . Fe5 . O40 . 102.6(3) yes O61 . Fe5 . O40 . 169.7(2) yes O69 . Fe5 . O40 . 93.8(2) yes N59 . Fe5 . O72 . 85.7(2) yes O61 . Fe5 . O72 . 90.7(2) yes O69 . Fe5 . O72 . 95.1(2) yes O40 . Fe5 . O72 . 89.1(2) yes N59 . Fe5 . O51 . 87.3(3) yes O61 . Fe5 . O51 . 94.6(2) yes O69 . Fe5 . O51 . 93.2(2) yes O40 . Fe5 . O51 . 86.9(2) yes O72 . Fe5 . O51 . 171.0(2) yes N59 . Fe5 . Fe6 . 58.19(19) yes O61 . Fe5 . Fe6 . 77.45(16) yes O69 . Fe5 . Fe6 . 117.46(16) yes O40 . Fe5 . Fe6 . 107.01(16) yes O72 . Fe5 . Fe6 . 30.57(15) yes O51 . Fe5 . Fe6 . 144.56(19) yes N42 . Fe6 . O65 . 89.7(2) yes N42 . Fe6 . O71 . 165.9(2) yes O65 . Fe6 . O71 . 76.3(2) yes N42 . Fe6 . O60 . 100.5(3) yes O65 . Fe6 . O60 . 169.8(2) yes O71 . Fe6 . O60 . 93.5(2) yes N42 . Fe6 . O72 . 86.8(2) yes O65 . Fe6 . O72 . 90.7(2) yes O71 . Fe6 . O72 . 95.1(2) yes O60 . Fe6 . O72 . 90.6(2) yes N42 . Fe6 . O50 . 86.8(3) yes O65 . Fe6 . O50 . 91.7(2) yes O71 . Fe6 . O50 . 91.7(2) yes O60 . Fe6 . O50 . 88.1(2) yes O72 . Fe6 . O50 . 173.1(2) yes N42 . Fe6 . Fe5 . 104.54(19) yes O65 . Fe6 . Fe5 . 115.40(15) yes O71 . Fe6 . Fe5 . 83.56(16) yes O60 . Fe6 . Fe5 . 62.90(16) yes O72 . Fe6 . Fe5 . 30.85(16) yes N42 . Fe6 . Fe4 . 60.14(19) yes O65 . Fe6 . Fe4 . 76.53(15) yes O71 . Fe6 . Fe4 . 117.02(17) yes O60 . Fe6 . Fe4 . 109.13(16) yes O72 . Fe6 . Fe4 . 30.75(16) yes N42 . Fe6 . Na1 . 133.0(2) yes O65 . Fe6 . Na1 . 80.73(16) yes O71 . Fe6 . Na1 . 43.56(17) yes O60 . Fe6 . Na1 . 91.64(18) yes O72 . Fe6 . Na1 . 138.70(17) yes O50 . Fe6 . Fe5 . 150.16(19) yes O50 . Fe6 . Fe4 . 144.45(18) yes Fe5 . Fe6 . Fe4 . 59.85(4) yes O50 . Fe6 . Na1 . 48.12(18) yes Fe5 . Fe6 . Na1 . 121.16(8) yes Fe4 . Fe6 . Na1 . 153.81(8) yes O78 . Na1 . O71 . 153.4(3) yes O78 . Na1 . O80 . 92.2(3) yes O71 . Na1 . O80 . 105.4(3) yes O78 . Na1 . O63 . 117.5(3) yes O71 . Na1 . O63 . 81.2(2) yes O80 . Na1 . O63 . 95.1(3) yes O78 . Na1 . O50 . 94.3(2) yes O71 . Na1 . O50 . 71.2(2) yes O80 . Na1 . O50 . 170.3(3) yes O63 . Na1 . O50 . 75.5(2) yes O78 . Na1 . Fe6 . 126.4(2) yes O71 . Na1 . Fe6 . 35.70(15) yes O80 . Na1 . Fe6 . 140.5(2) yes O63 . Na1 . Fe6 . 75.85(18) yes O50 . Na1 . Fe6 . 35.49(14) yes O78 . Na1 . O1 . 94.6(2) yes O71 . Na1 . O1 . 68.0(2) yes O80 . Na1 . O1 . 84.9(3) yes O63 . Na1 . O1 . 147.8(3) yes O50 . Na1 . O1 . 101.8(2) yes O78 . Na1 . Fe1 . 125.3(2) yes O71 . Na1 . Fe1 . 34.11(14) yes O80 . Na1 . Fe1 . 97.5(2) yes O63 . Na1 . Fe1 . 115.0(2) yes O50 . Na1 . Fe1 . 84.65(17) yes Fe6 . Na1 . O1 . 83.79(15) yes Fe6 . Na1 . Fe1 . 55.42(6) yes O1 . Na1 . Fe1 . 33.90(13) yes O76 . Na2 . O73 . 90.6(2) yes O76 . Na2 . O31 . 162.4(3) yes O73 . Na2 . O31 . 74.4(2) yes O76 . Na2 . O74 . 102.0(3) yes O73 . Na2 . O74 . 107.9(3) yes O31 . Na2 . O74 . 91.5(3) yes O76 . Na2 . O76 2_656 87.5(3) yes O73 . Na2 . O76 2_656 95.2(2) yes O31 . Na2 . O76 2_656 84.9(2) yes O74 . Na2 . O76 2_656 154.8(3) yes O76 . Na2 . Fe4 . 126.5(2) yes O73 . Na2 . Fe4 . 38.86(14) yes O31 . Na2 . Fe4 . 36.71(14) yes O74 . Na2 . Fe4 . 108.7(2) yes O76 2_656 Na2 . Fe4 . 82.94(18) yes