#Electronic Supplementary Information for Dalton Transactions #This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Polymetallic clusters of iron(III) with derivatised salicylaldoximes ; _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Raod Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_name 'Euan Brechin' loop_ _publ_author_name 'Euan Brechin' 'Laura E. Budd' 'Anna Collins' 'Ian A. Gass' 'Constantinos J. Milios' 'Mark Murrie' ; S.Parsons ; 'Spyros Perlepes' 'Fraser White' # Attachment 'Complex 1.cif' data_eb6154 _database_code_depnum_ccdc_archive 'CCDC 667678' _audit_creation_method SHELXL-97 _audit_creation_date 06-12-23 #_publ_contact_author_name S.Parsons #_publ_contact_author_email S.Parsons@ed.ac.uk _chemical_compound_source 'Ian Gass IAG1183' _exptl_crystal_recrystallization_method ; slow evaporation of MeOH soln ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (NEt3H)[Fe2(MeO)L2LH2].5MeOH _chemical_formula_sum 'C64 H77 Fe2 N5 O14' _chemical_formula_weight 1252.01 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1601(8) _cell_length_b 15.1676(16) _cell_length_c 21.610(3) _cell_angle_alpha 106.158(9) _cell_angle_beta 99.287(7) _cell_angle_gamma 93.760(5) _cell_volume 3135.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2616 _cell_measurement_theta_min 2 _cell_measurement_theta_max 18 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type mutiscan _exptl_absorpt_correction_T_min 0.414 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details 'sadabs scaled by 1.27' _exptl_special_details ; Oxford Crysosystems LT device. ; _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 omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20024 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_sigmaI/netI 0.1214 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 20.87 _reflns_number_total 6596 _reflns_number_gt 3894 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; Weak diffraction, so only Fe was refined anisotropically. Ligands 1 and 3 bind through O1, N8 and O9 and carry -2 charge. Ligands 2 and 4 bind through O1 and N8, but not O9, which is protonated. Similarity restraints were applied to equivalent bonds and angles in 1/3, 2/4, and all the methanol/methoxide bonds. The NEt3NH+ cation was restrained to be three-fold symmetric. The following H-bond restraints were also applied: DFIX 1.82 0.05 H92 O110 DFIX 1.91 0.05 H94 O19 DFIX 2.03 0.05 H17 O13 DFIX 2.25 0.05 H18 O91 DFIX 1.98 0.05 H19 O12 DFIX 1.84 0.05 H110 O14 DFIX 1.88 0.05 H11A O17[-x, -y+1, -z] The displacement parameters in the cation are hight, and the Et groups are likely to be disordered; the data are not good enough to resolve a satisfactory disorder model. Checkcif output: 023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 20.87 Deg. 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 20.87 Deg. 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 66 341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 16 020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 084_ALERT_2_C High R2 Value .................................. 0.26 202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 17 Weak data - see above. 223_ALERT_4_A Large Solvent/Anion H Ueq(max)/Ueq(min) ... 5.26 Ratio 412_ALERT_2_A Short Intra XH3 .. XHn H26C .. H46B .. 1.19 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H21 .. H26B .. 1.91 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H26A .. H122 .. 1.94 Ang. 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C36 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C56 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N16 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.78 Ratio See comments above about cation disorder. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? no action 061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.54 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. 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 0.501 23 no action: #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 6574 6573 1 20.87 0.501 0.997 6619 6596 23 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C122 no action. 731_ALERT_1_C Bond Calc 1.45(3), Rep 1.453(13) ...... 2.31 su-Ra N16 -C16 1.555 1.555 731_ALERT_1_C Bond Calc 1.52(4), Rep 1.530(16) ...... 2.50 su-Ra C16 -C26 1.555 1.555 731_ALERT_1_C Bond Calc 1.409(19), Rep 1.408(9) ...... 2.11 su-Ra O18 -C28 1.555 1.555 The use of restraints in the refinement mean that off diagonal terms in the variance-covariance matrix are significant, and the diagonal approximation used in Platon/Checkcif can be badly in error. 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C6 H16 N 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C H4 O 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C H4 O 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 C H4 O 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N16 No action. ; _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^)+(0.1198P)^2^+12.5464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'riding/rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6596 _refine_ls_number_parameters 316 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.1620 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2567 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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 0.04765(15) 0.16926(10) 0.29074(7) 0.0315(5) Uani 1 1 d . . . Fe2 Fe -0.00708(15) 0.32597(10) 0.21832(7) 0.0303(5) Uani 1 1 d . . . O11 O -0.0547(7) 0.0966(5) 0.3344(3) 0.0402(19) Uiso 1 1 d D . . C11 C -0.0782(11) 0.1306(7) 0.3947(5) 0.046(3) Uiso 1 1 d D . . C21 C -0.0716(12) 0.0744(8) 0.4367(5) 0.058(4) Uiso 1 1 d D . . H21 H -0.0480 0.0135 0.4217 0.070 Uiso 1 1 calc R . . C31 C -0.0986(14) 0.1057(9) 0.4993(6) 0.080(4) Uiso 1 1 d D . . H31 H -0.0973 0.0653 0.5259 0.096 Uiso 1 1 calc R . . C41 C -0.1271(14) 0.1940(9) 0.5232(6) 0.084(5) Uiso 1 1 d D . . H41 H -0.1424 0.2156 0.5669 0.100 Uiso 1 1 calc R . . C51 C -0.1335(12) 0.2519(8) 0.4837(5) 0.060(4) Uiso 1 1 d D . . H51 H -0.1543 0.3132 0.5003 0.071 Uiso 1 1 calc R . . C61 C -0.1098(11) 0.2212(7) 0.4190(5) 0.047(3) Uiso 1 1 d D . . C71 C -0.1341(9) 0.2834(6) 0.3780(4) 0.037(3) Uiso 1 1 d D . . N81 N -0.0796(8) 0.2700(5) 0.3258(4) 0.034(2) Uiso 1 1 d D . . O91 O -0.1118(6) 0.3242(4) 0.2862(3) 0.0328(18) Uiso 1 1 d D . . C101 C -0.2135(6) 0.3614(4) 0.3974(3) 0.035(3) Uiso 1 1 d GD . . C111 C -0.1496(5) 0.4512(4) 0.4235(3) 0.043(3) Uiso 1 1 d GD . . H111 H -0.0553 0.4628 0.4269 0.051 Uiso 1 1 calc R . . C121 C -0.2237(7) 0.5240(3) 0.4446(3) 0.049(3) Uiso 1 1 d GD . . H121 H -0.1800 0.5853 0.4625 0.059 Uiso 1 1 calc R . . C131 C -0.3617(6) 0.5069(4) 0.4397(4) 0.049(3) Uiso 1 1 d GD . . H131 H -0.4123 0.5567 0.4541 0.058 Uiso 1 1 calc R . . C141 C -0.4256(5) 0.4172(5) 0.4135(3) 0.048(3) Uiso 1 1 d GD . . H141 H -0.5199 0.4055 0.4101 0.058 Uiso 1 1 calc R . . C151 C -0.3515(6) 0.3444(3) 0.3924(3) 0.041(3) Uiso 1 1 d GD . . H151 H -0.3952 0.2831 0.3745 0.050 Uiso 1 1 calc R . . O12 O 0.1732(6) 0.0791(4) 0.2711(3) 0.0352(18) Uiso 1 1 d D . . C12 C 0.2286(10) 0.0335(6) 0.3106(4) 0.037(3) Uiso 1 1 d D . . C22 C 0.2523(11) -0.0585(7) 0.2825(5) 0.049(3) Uiso 1 1 d D . . H22 H 0.2274 -0.0855 0.2364 0.059 Uiso 1 1 calc R . . C32 C 0.3106(13) -0.1098(8) 0.3204(6) 0.066(4) Uiso 1 1 d D . . H32 H 0.3287 -0.1708 0.3001 0.080 Uiso 1 1 calc R . . C42 C 0.3430(13) -0.0733(8) 0.3880(6) 0.071(4) Uiso 1 1 d D . . H42 H 0.3789 -0.1101 0.4142 0.085 Uiso 1 1 calc R . . C52 C 0.3229(12) 0.0172(7) 0.4172(5) 0.055(3) Uiso 1 1 d D . . H52 H 0.3466 0.0428 0.4635 0.066 Uiso 1 1 calc R . . C62 C 0.2667(10) 0.0715(6) 0.3781(4) 0.035(3) Uiso 1 1 d D . . C72 C 0.2588(9) 0.1694(6) 0.4127(4) 0.033(3) Uiso 1 1 d D . . N82 N 0.1923(8) 0.2188(5) 0.3832(4) 0.031(2) Uiso 1 1 d D . . O92 O 0.2056(8) 0.3131(5) 0.4231(4) 0.050(2) Uiso 1 1 d D . . H92 H 0.1778 0.3465 0.3998 0.076 Uiso 1 1 calc RD . . C102 C 0.3303(7) 0.2089(5) 0.4823(3) 0.040(3) Uiso 1 1 d GD . . C112 C 0.2563(6) 0.2269(6) 0.5323(4) 0.059(4) Uiso 1 1 d GD . . H112 H 0.1612 0.2144 0.5221 0.071 Uiso 1 1 calc R . . C122 C 0.3215(8) 0.2632(6) 0.5972(3) 0.089(5) Uiso 1 1 d GD . . H122 H 0.2709 0.2755 0.6314 0.107 Uiso 1 1 calc R . . C132 C 0.4607(9) 0.2814(6) 0.6121(3) 0.083(5) Uiso 1 1 d GD . . H132 H 0.5053 0.3062 0.6565 0.099 Uiso 1 1 calc R . . C142 C 0.5347(6) 0.2634(6) 0.5621(4) 0.066(4) Uiso 1 1 d GD . . H142 H 0.6298 0.2759 0.5723 0.080 Uiso 1 1 calc R . . C152 C 0.4695(7) 0.2272(5) 0.4972(3) 0.054(3) Uiso 1 1 d GD . . H152 H 0.5201 0.2149 0.4630 0.065 Uiso 1 1 calc R . . O13 O -0.1528(6) 0.3556(4) 0.1604(3) 0.0299(17) Uiso 1 1 d D . . C13 C -0.1826(10) 0.3143(6) 0.0963(4) 0.033(3) Uiso 1 1 d D . . C23 C -0.2247(11) 0.3669(7) 0.0543(5) 0.044(3) Uiso 1 1 d D . . H23 H -0.2280 0.4313 0.0722 0.052 Uiso 1 1 calc R . . C33 C -0.2615(10) 0.3268(7) -0.0128(5) 0.042(3) Uiso 1 1 d D . . H33 H -0.2904 0.3638 -0.0402 0.050 Uiso 1 1 calc R . . C43 C -0.2568(11) 0.2346(7) -0.0400(5) 0.048(3) Uiso 1 1 d D . . H43 H -0.2792 0.2080 -0.0862 0.057 Uiso 1 1 calc R . . C53 C -0.2192(10) 0.1804(7) 0.0000(5) 0.043(3) Uiso 1 1 d D . . H53 H -0.2178 0.1161 -0.0191 0.052 Uiso 1 1 calc R . . C63 C -0.1826(10) 0.2183(6) 0.0690(4) 0.033(3) Uiso 1 1 d D . . C73 C -0.1540(9) 0.1539(6) 0.1080(4) 0.032(3) Uiso 1 1 d D . . N83 N -0.0842(8) 0.1872(5) 0.1677(3) 0.033(2) Uiso 1 1 d D . . O93 O -0.0669(6) 0.1263(4) 0.2036(3) 0.0342(18) Uiso 1 1 d D . . C103 C -0.2006(6) 0.0538(3) 0.0791(3) 0.034(3) Uiso 1 1 d GD . . C113 C -0.1098(5) -0.0085(4) 0.0601(3) 0.043(3) Uiso 1 1 d GD . . H113 H -0.0167 0.0125 0.0679 0.051 Uiso 1 1 calc R . . C123 C -0.1551(6) -0.1014(4) 0.0297(4) 0.054(3) Uiso 1 1 d GD . . H123 H -0.0931 -0.1440 0.0168 0.065 Uiso 1 1 calc R . . C133 C -0.2913(7) -0.1320(3) 0.0184(3) 0.052(3) Uiso 1 1 d GD . . H133 H -0.3223 -0.1956 -0.0024 0.062 Uiso 1 1 calc R . . C143 C -0.3821(5) -0.0698(4) 0.0373(4) 0.049(3) Uiso 1 1 d GD . . H143 H -0.4751 -0.0907 0.0295 0.059 Uiso 1 1 calc R . . C153 C -0.3367(6) 0.0232(4) 0.0677(3) 0.041(3) Uiso 1 1 d GD . . H153 H -0.3988 0.0657 0.0806 0.049 Uiso 1 1 calc R . . O14 O 0.0720(7) 0.4537(4) 0.2571(3) 0.0387(19) Uiso 1 1 d D . . C14 C 0.0872(11) 0.5155(6) 0.2256(5) 0.041(3) Uiso 1 1 d D . . C24 C 0.0747(12) 0.6084(7) 0.2582(5) 0.059(4) Uiso 1 1 d D . . H24 H 0.0566 0.6235 0.3015 0.071 Uiso 1 1 calc R . . C34 C 0.0879(12) 0.6769(8) 0.2291(5) 0.060(4) Uiso 1 1 d D . . H34 H 0.0796 0.7389 0.2522 0.072 Uiso 1 1 calc R . . C44 C 0.1135(12) 0.6560(8) 0.1659(6) 0.063(4) Uiso 1 1 d D . . H44 H 0.1219 0.7035 0.1455 0.075 Uiso 1 1 calc R . . C54 C 0.1269(11) 0.5657(7) 0.1323(5) 0.047(3) Uiso 1 1 d D . . H54 H 0.1438 0.5515 0.0889 0.057 Uiso 1 1 calc R . . C64 C 0.1153(10) 0.4948(6) 0.1626(4) 0.033(3) Uiso 1 1 d D . . C74 C 0.1466(9) 0.4024(6) 0.1272(4) 0.032(3) Uiso 1 1 d D . . N84 N 0.1181(7) 0.3324(5) 0.1467(4) 0.030(2) Uiso 1 1 d D . . O94 O 0.1628(8) 0.2510(5) 0.1084(3) 0.049(2) Uiso 1 1 d D . . H94 H 0.1674 0.2116 0.1292 0.073 Uiso 1 1 calc RD . . C104 C 0.2122(7) 0.3922(5) 0.0688(3) 0.041(3) Uiso 1 1 d GD . . C114 C 0.3509(7) 0.4115(5) 0.0782(3) 0.055(3) Uiso 1 1 d GD . . H114 H 0.4032 0.4279 0.1212 0.066 Uiso 1 1 calc R . . C124 C 0.4129(5) 0.4068(6) 0.0248(4) 0.064(4) Uiso 1 1 d GD . . H124 H 0.5077 0.4200 0.0312 0.077 Uiso 1 1 calc R . . C134 C 0.3363(8) 0.3828(6) -0.0381(3) 0.063(4) Uiso 1 1 d GD . . H134 H 0.3787 0.3796 -0.0747 0.076 Uiso 1 1 calc R . . C144 C 0.1976(7) 0.3635(6) -0.0476(3) 0.062(4) Uiso 1 1 d GD . . H144 H 0.1452 0.3471 -0.0906 0.075 Uiso 1 1 calc R . . C154 C 0.1356(5) 0.3682(5) 0.0059(3) 0.051(3) Uiso 1 1 d GD . . H154 H 0.0408 0.3551 -0.0006 0.061 Uiso 1 1 calc R . . O15 O 0.1341(6) 0.2698(4) 0.2635(3) 0.0305(17) Uiso 1 1 d . . . C25 C 0.2749(10) 0.2935(8) 0.2719(5) 0.042(3) Uiso 1 1 d . . . H25A H 0.2918 0.3461 0.2550 0.064 Uiso 1 1 calc R . . H25B H 0.3148 0.2405 0.2477 0.064 Uiso 1 1 calc R . . H25C H 0.3150 0.3103 0.3186 0.064 Uiso 1 1 calc R . . N16 N -0.2559(10) -0.0375(7) 0.2562(5) 0.073(3) Uiso 1 1 d D . . H16 H -0.1827 0.0055 0.2796 0.088 Uiso 1 1 calc R . . C16 C -0.287(2) -0.0924(15) 0.2985(11) 0.194(11) Uiso 1 1 d D . . H16A H -0.3623 -0.1412 0.2750 0.233 Uiso 1 1 calc R . . H16B H -0.3143 -0.0526 0.3381 0.233 Uiso 1 1 calc R . . C26 C -0.162(3) -0.136(2) 0.3182(17) 0.31(2) Uiso 1 1 d D . . H26A H -0.1814 -0.1751 0.3456 0.463 Uiso 1 1 calc R . . H26B H -0.0889 -0.0872 0.3429 0.463 Uiso 1 1 calc R . . H26C H -0.1340 -0.1737 0.2787 0.463 Uiso 1 1 calc R . . C36 C -0.2181(18) -0.0902(13) 0.1949(7) 0.148(8) Uiso 1 1 d D . . H36A H -0.2166 -0.0505 0.1656 0.178 Uiso 1 1 calc R . . H36B H -0.2871 -0.1437 0.1727 0.178 Uiso 1 1 calc R . . C46 C -0.0841(19) -0.1245(15) 0.2053(10) 0.163(9) Uiso 1 1 d D . . H46A H -0.0652 -0.1602 0.1631 0.245 Uiso 1 1 calc R . . H46B H -0.0848 -0.1640 0.2343 0.245 Uiso 1 1 calc R . . H46C H -0.0146 -0.0718 0.2255 0.245 Uiso 1 1 calc R . . C56 C -0.3651(17) 0.0143(12) 0.2384(7) 0.118(6) Uiso 1 1 d D . . H56A H -0.4426 -0.0293 0.2104 0.142 Uiso 1 1 calc R . . H56B H -0.3349 0.0544 0.2130 0.142 Uiso 1 1 calc R . . C66 C -0.4082(17) 0.0737(11) 0.2995(8) 0.115(6) Uiso 1 1 d D . . H66A H -0.4821 0.1072 0.2865 0.172 Uiso 1 1 calc R . . H66B H -0.3322 0.1181 0.3267 0.172 Uiso 1 1 calc R . . H66C H -0.4383 0.0341 0.3246 0.172 Uiso 1 1 calc R . . O17 O -0.2957(9) 0.5021(7) 0.2104(5) 0.082(3) Uiso 1 1 d D . . H17 H -0.2288 0.4818 0.1953 0.124 Uiso 1 1 calc RD . . C27 C -0.2822(17) 0.5024(12) 0.2766(6) 0.111(6) Uiso 1 1 d D . . H27A H -0.2097 0.5499 0.3036 0.167 Uiso 1 1 calc R . . H27B H -0.2610 0.4417 0.2803 0.167 Uiso 1 1 calc R . . H27C H -0.3665 0.5157 0.2919 0.167 Uiso 1 1 calc R . . O18 O -0.3895(11) 0.2250(7) 0.2083(5) 0.095(3) Uiso 1 1 d D . . H18 H -0.3263 0.2628 0.2337 0.142 Uiso 1 1 calc RD . . C28 C -0.4632(15) 0.2685(10) 0.1666(7) 0.092(5) Uiso 1 1 d D . . H28A H -0.4502 0.3355 0.1872 0.137 Uiso 1 1 calc R . . H28B H -0.5588 0.2459 0.1589 0.137 Uiso 1 1 calc R . . H28C H -0.4319 0.2543 0.1247 0.137 Uiso 1 1 calc R . . O19 O 0.1934(8) 0.0929(6) 0.1456(4) 0.059(2) Uiso 1 1 d D . . H19 H 0.1716 0.0842 0.1795 0.089 Uiso 1 1 calc RD . . C29 C 0.3124(11) 0.0540(9) 0.1351(6) 0.062(4) Uiso 1 1 d D . . H29A H 0.3884 0.0929 0.1669 0.093 Uiso 1 1 calc R . . H29B H 0.3256 0.0501 0.0905 0.093 Uiso 1 1 calc R . . H29C H 0.3061 -0.0080 0.1405 0.093 Uiso 1 1 calc R . . O110 O 0.1503(7) 0.4599(5) 0.3829(4) 0.048(2) Uiso 1 1 d D . . H110 H 0.1012 0.4605 0.3478 0.072 Uiso 1 1 calc RD . . C210 C 0.2560(10) 0.5323(7) 0.4010(6) 0.054(3) Uiso 1 1 d D . . H21A H 0.2191 0.5907 0.4019 0.081 Uiso 1 1 calc R . . H21B H 0.3159 0.5199 0.3691 0.081 Uiso 1 1 calc R . . H21C H 0.3064 0.5367 0.4447 0.081 Uiso 1 1 calc R . . O111 O 0.3775(11) 0.3300(8) -0.2134(6) 0.102(4) Uiso 1 1 d D . . H11A H 0.3477 0.3794 -0.2163 0.154 Uiso 1 1 calc RD . . C211 C 0.5182(13) 0.3453(13) -0.1951(9) 0.123(7) Uiso 1 1 d D . . H21D H 0.5531 0.3923 -0.2135 0.185 Uiso 1 1 calc R . . H21E H 0.5561 0.2876 -0.2120 0.185 Uiso 1 1 calc R . . H21F H 0.5436 0.3667 -0.1472 0.185 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 0.0369(10) 0.0287(10) 0.0293(9) 0.0059(7) 0.0106(7) 0.0082(8) Fe2 0.0402(10) 0.0234(9) 0.0265(9) 0.0037(7) 0.0101(7) 0.0034(7) _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 O12 1.939(6) . ? Fe1 O93 1.959(6) . ? Fe1 O11 1.983(7) . ? Fe1 O15 1.984(7) . ? Fe1 N81 2.124(7) . ? Fe1 N82 2.188(7) . ? Fe2 O13 1.940(6) . ? Fe2 O14 1.943(7) . ? Fe2 O91 1.952(6) . ? Fe2 O15 1.977(6) . ? Fe2 N83 2.114(7) . ? Fe2 N84 2.174(7) . ? O11 C11 1.328(9) . ? C11 C21 1.405(11) . ? C11 C61 1.406(11) . ? C21 C31 1.382(12) . ? C31 C41 1.362(13) . ? C41 C51 1.383(12) . ? C51 C61 1.411(12) . ? C61 C71 1.471(11) . ? C71 N81 1.308(10) . ? C71 C101 1.478(9) . ? N81 O91 1.359(8) . ? C101 C111 1.3900 . ? C101 C151 1.3900 . ? C111 C121 1.3900 . ? C121 C131 1.3900 . ? C131 C141 1.3900 . ? C141 C151 1.3900 . ? O12 C12 1.320(9) . ? C12 C62 1.391(11) . ? C12 C22 1.412(11) . ? C22 C32 1.374(12) . ? C32 C42 1.386(13) . ? C42 C52 1.385(12) . ? C52 C62 1.419(11) . ? C62 C72 1.479(11) . ? C72 N82 1.272(9) . ? C72 C102 1.496(9) . ? N82 O92 1.435(8) . ? C102 C112 1.3900 . ? C102 C152 1.3900 . ? C112 C122 1.3900 . ? C122 C132 1.3900 . ? C132 C142 1.3900 . ? C142 C152 1.3900 . ? O13 C13 1.327(9) . ? C13 C23 1.402(11) . ? C13 C63 1.411(11) . ? C23 C33 1.384(12) . ? C33 C43 1.365(12) . ? C43 C53 1.379(12) . ? C53 C63 1.417(11) . ? C63 C73 1.472(11) . ? C73 N83 1.310(9) . ? C73 C103 1.483(9) . ? N83 O93 1.365(8) . ? C103 C113 1.3900 . ? C103 C153 1.3900 . ? C113 C123 1.3900 . ? C123 C133 1.3900 . ? C133 C143 1.3900 . ? C143 C153 1.3900 . ? O14 C14 1.318(9) . ? C14 C64 1.391(11) . ? C14 C24 1.414(11) . ? C24 C34 1.367(12) . ? C34 C44 1.386(13) . ? C44 C54 1.386(12) . ? C54 C64 1.414(11) . ? C64 C74 1.480(11) . ? C74 N84 1.279(9) . ? C74 C104 1.496(9) . ? N84 O94 1.429(8) . ? C104 C114 1.3900 . ? C104 C154 1.3900 . ? C114 C124 1.3900 . ? C124 C134 1.3900 . ? C134 C144 1.3900 . ? C144 C154 1.3900 . ? O15 C25 1.421(12) . ? N16 C16 1.453(13) . ? N16 C56 1.464(12) . ? N16 C36 1.469(13) . ? C16 C26 1.530(16) . ? C36 C46 1.494(15) . ? C56 C66 1.525(15) . ? O17 C27 1.415(9) . ? O18 C28 1.408(9) . ? O19 C29 1.403(9) . ? O110 C210 1.408(8) . ? O111 C211 1.407(9) . ? 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 O12 Fe1 O93 95.0(3) . . ? O12 Fe1 O11 93.8(3) . . ? O93 Fe1 O11 97.7(3) . . ? O12 Fe1 O15 99.4(3) . . ? O93 Fe1 O15 88.6(3) . . ? O11 Fe1 O15 164.8(3) . . ? O12 Fe1 N81 172.3(3) . . ? O93 Fe1 N81 92.3(3) . . ? O11 Fe1 N81 82.6(3) . . ? O15 Fe1 N81 83.3(3) . . ? O12 Fe1 N82 81.8(3) . . ? O93 Fe1 N82 174.3(3) . . ? O11 Fe1 N82 87.2(3) . . ? O15 Fe1 N82 87.3(3) . . ? N81 Fe1 N82 91.2(3) . . ? O13 Fe2 O14 94.1(3) . . ? O13 Fe2 O91 94.6(3) . . ? O14 Fe2 O91 95.6(3) . . ? O13 Fe2 O15 167.9(3) . . ? O14 Fe2 O15 96.9(3) . . ? O91 Fe2 O15 89.2(3) . . ? O13 Fe2 N83 84.6(3) . . ? O14 Fe2 N83 174.1(3) . . ? O91 Fe2 N83 90.2(3) . . ? O15 Fe2 N83 83.9(3) . . ? O13 Fe2 N84 87.5(3) . . ? O14 Fe2 N84 82.0(3) . . ? O91 Fe2 N84 177.0(3) . . ? O15 Fe2 N84 89.2(3) . . ? N83 Fe2 N84 92.2(3) . . ? C11 O11 Fe1 123.3(6) . . ? O11 C11 C21 119.2(8) . . ? O11 C11 C61 123.0(8) . . ? C21 C11 C61 117.9(8) . . ? C31 C21 C11 121.4(10) . . ? C41 C31 C21 120.7(11) . . ? C31 C41 C51 119.7(11) . . ? C41 C51 C61 120.9(10) . . ? C11 C61 C51 119.3(8) . . ? C11 C61 C71 123.1(8) . . ? C51 C61 C71 117.2(8) . . ? N81 C71 C61 118.4(8) . . ? N81 C71 C101 121.3(7) . . ? C61 C71 C101 120.3(7) . . ? C71 N81 O91 117.0(7) . . ? C71 N81 Fe1 128.6(6) . . ? O91 N81 Fe1 114.3(5) . . ? N81 O91 Fe2 118.9(5) . . ? C111 C101 C151 120.0 . . ? C111 C101 C71 120.1(5) . . ? C151 C101 C71 119.8(5) . . ? C121 C111 C101 120.0 . . ? C111 C121 C131 120.0 . . ? C121 C131 C141 120.0 . . ? C151 C141 C131 120.0 . . ? C141 C151 C101 120.0 . . ? C12 O12 Fe1 126.3(6) . . ? O12 C12 C62 123.7(8) . . ? O12 C12 C22 118.2(8) . . ? C62 C12 C22 118.1(8) . . ? C32 C22 C12 121.5(9) . . ? C22 C32 C42 120.3(11) . . ? C52 C42 C32 119.8(11) . . ? C42 C52 C62 120.1(9) . . ? C12 C62 C52 120.2(8) . . ? C12 C62 C72 123.3(8) . . ? C52 C62 C72 116.4(8) . . ? N82 C72 C62 120.0(7) . . ? N82 C72 C102 121.0(7) . . ? C62 C72 C102 119.0(7) . . ? C72 N82 O92 111.5(7) . . ? C72 N82 Fe1 126.5(6) . . ? O92 N82 Fe1 121.3(5) . . ? C112 C102 C152 120.0 . . ? C112 C102 C72 119.4(6) . . ? C152 C102 C72 120.6(6) . . ? C102 C112 C122 120.0 . . ? C132 C122 C112 120.0 . . ? C142 C132 C122 120.0 . . ? C132 C142 C152 120.0 . . ? C142 C152 C102 120.0 . . ? C13 O13 Fe2 123.3(6) . . ? O13 C13 C23 118.8(8) . . ? O13 C13 C63 122.5(7) . . ? C23 C13 C63 118.5(8) . . ? C33 C23 C13 121.2(9) . . ? C43 C33 C23 120.7(9) . . ? C33 C43 C53 119.5(10) . . ? C43 C53 C63 121.6(9) . . ? C13 C63 C53 118.3(8) . . ? C13 C63 C73 124.1(8) . . ? C53 C63 C73 117.5(8) . . ? N83 C73 C63 118.2(7) . . ? N83 C73 C103 121.6(7) . . ? C63 C73 C103 120.2(7) . . ? C73 N83 O93 116.3(7) . . ? C73 N83 Fe2 128.1(6) . . ? O93 N83 Fe2 115.4(5) . . ? N83 O93 Fe1 118.4(5) . . ? C113 C103 C153 120.0 . . ? C113 C103 C73 120.3(5) . . ? C153 C103 C73 119.6(5) . . ? C103 C113 C123 120.0 . . ? C133 C123 C113 120.0 . . ? C123 C133 C143 120.0 . . ? C153 C143 C133 120.0 . . ? C143 C153 C103 120.0 . . ? C14 O14 Fe2 126.3(6) . . ? O14 C14 C64 124.0(8) . . ? O14 C14 C24 117.7(8) . . ? C64 C14 C24 118.3(8) . . ? C34 C24 C14 121.7(10) . . ? C24 C34 C44 119.9(11) . . ? C54 C44 C34 120.1(10) . . ? C44 C54 C64 120.2(9) . . ? C14 C64 C54 119.7(8) . . ? C14 C64 C74 122.7(8) . . ? C54 C64 C74 117.3(8) . . ? N84 C74 C64 120.1(8) . . ? N84 C74 C104 120.8(7) . . ? C64 C74 C104 119.2(7) . . ? C74 N84 O94 111.5(7) . . ? C74 N84 Fe2 126.7(6) . . ? O94 N84 Fe2 121.2(5) . . ? C114 C104 C154 120.0 . . ? C114 C104 C74 119.2(5) . . ? C154 C104 C74 120.7(5) . . ? C124 C114 C104 120.0 . . ? C114 C124 C134 120.0 . . ? C124 C134 C144 120.0 . . ? C154 C144 C134 120.0 . . ? C144 C154 C104 120.0 . . ? C25 O15 Fe2 125.8(6) . . ? C25 O15 Fe1 125.3(6) . . ? Fe2 O15 Fe1 108.8(3) . . ? C16 N16 C56 113.3(10) . . ? C16 N16 C36 114.7(10) . . ? C56 N16 C36 107.1(9) . . ? N16 C16 C26 108.1(13) . . ? N16 C36 C46 113.0(12) . . ? N16 C56 C66 110.8(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.87 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.809 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.101 # Attachment 'Complex 2.cif' data_eb6174 _database_code_depnum_ccdc_archive 'CCDC 667679' _audit_creation_method SHELXL-97 _audit_creation_date 06-12-19 #_publ_contact_author_name S.Parsons #_publ_contact_author_email S.Parsons@ed.ac.uk _chemical_compound_source 'M. Sharlow MS94 ' _exptl_crystal_recrystallization_method ; Evaporation of MeOH solution ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe3O(EtSal)(PhCOO)5(MeOH)2].3MeOH' _chemical_formula_sum 'C49 H54 Fe3 N O18' _chemical_formula_weight 1112.48 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 21.0901(12) _cell_length_b 11.5474(7) _cell_length_c 20.5990(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.198(4) _cell_angle_gamma 90.00 _cell_volume 4937.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9523 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.5 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Data collection strategy optimised with COSMO. Oxford Crysosystems LT device. ; _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 omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62527 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.56 _reflns_number_total 14827 _reflns_number_gt 12120 _reflns_threshold_expression >2sigma(I) __computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; ligands: 1 = EtSal 2- 2-6 = PhCOO- 7,8 = ligated MeOH 9-11 = MeOH of solvation. H's placed on methanol using 'circular Fourier' method; those on O17 and O18 were placed to optimise H-bonding. Checkcif output 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action. These were all idealised. 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 327 919_ALERT_3_B # Reflections Likely Effected by the Beamstop .. 1 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 2 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 5 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 5175 5171 4 23.01 0.550 0.999 6879 6875 4 25.24 0.600 0.999 8941 8934 7 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.998 11345 11326 19 29.84 0.700 0.989 14182 14022 160 30.56 0.715 0.978 15161 14827 334 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.78 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 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.52 Ratio No action; MeOH#10 shows quite high librational motion. 232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N81 .. 5.47 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - O17 .. 5.78 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe3 - O18 .. 5.49 su No action. Ton Spek says this often happens with bonds between heavy & light atoms with good data sets. The reason is probably inadequate modelling of bonding density. 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 No action. ; _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^)+(0.0621P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment 'riding/ rotating rigid group' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00123(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14827 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.007 _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 0.284008(11) 0.725143(19) 0.216285(11) 0.02217(6) Uani 1 1 d . . . Fe2 Fe 0.231954(12) 0.464929(19) 0.180293(11) 0.02392(6) Uani 1 1 d . . . Fe3 Fe 0.227439(11) 0.564927(18) 0.327460(11) 0.02078(6) Uani 1 1 d . . . O1 O 0.24485(5) 0.58636(9) 0.24255(5) 0.0229(2) Uani 1 1 d . . . C11 C 0.39844(8) 0.83655(15) 0.18486(8) 0.0261(3) Uani 1 1 d . . . O11 O 0.33424(6) 0.84252(10) 0.17989(6) 0.0279(2) Uani 1 1 d . . . C21 C 0.43416(9) 0.93974(16) 0.19527(9) 0.0312(3) Uani 1 1 d . . . H21 H 0.4121 1.0112 0.1968 0.037 Uiso 1 1 calc R . . C31 C 0.50082(9) 0.93953(18) 0.20335(10) 0.0362(4) Uani 1 1 d . . . H31 H 0.5241 1.0102 0.2104 0.043 Uiso 1 1 calc R . . C41 C 0.53340(9) 0.8358(2) 0.20112(10) 0.0400(4) Uani 1 1 d . . . H41 H 0.5792 0.8348 0.2083 0.048 Uiso 1 1 calc R . . C51 C 0.49919(8) 0.73416(18) 0.18840(9) 0.0344(4) Uani 1 1 d . . . H51 H 0.5221 0.6639 0.1860 0.041 Uiso 1 1 calc R . . C61 C 0.43126(8) 0.73106(15) 0.17890(8) 0.0270(3) Uani 1 1 d . . . C71 C 0.39793(8) 0.62097(14) 0.15998(8) 0.0270(3) Uani 1 1 d . . . N81 N 0.33806(7) 0.60992(12) 0.16734(7) 0.0252(3) Uani 1 1 d . . . O91 O 0.30679(6) 0.51005(10) 0.14363(6) 0.0289(2) Uani 1 1 d . . . C101 C 0.43183(9) 0.52522(16) 0.13013(10) 0.0338(4) Uani 1 1 d . . . H10A H 0.4042 0.4554 0.1254 0.041 Uiso 1 1 calc R . . H10B H 0.4722 0.5059 0.1606 0.041 Uiso 1 1 calc R . . C111 C 0.44776(11) 0.55638(18) 0.06310(10) 0.0394(4) Uani 1 1 d . . . H11A H 0.4698 0.4911 0.0463 0.059 Uiso 1 1 calc R . . H11B H 0.4759 0.6245 0.0675 0.059 Uiso 1 1 calc R . . H11C H 0.4079 0.5736 0.0323 0.059 Uiso 1 1 calc R . . O12 O 0.21337(6) 0.74176(11) 0.13300(6) 0.0290(2) Uani 1 1 d . . . C12 C 0.16946(8) 0.67209(15) 0.10709(8) 0.0270(3) Uani 1 1 d . . . C22 C 0.11277(8) 0.71947(16) 0.06054(9) 0.0305(3) Uani 1 1 d . . . O22 O 0.16917(6) 0.56469(11) 0.11681(6) 0.0312(3) Uani 1 1 d . . . C32 C 0.11273(10) 0.8321(2) 0.03706(12) 0.0455(5) Uani 1 1 d . . . H32 H 0.1495 0.8802 0.0494 0.055 Uiso 1 1 calc R . . C42 C 0.05851(12) 0.8743(2) -0.00474(14) 0.0587(7) Uani 1 1 d . . . H42 H 0.0586 0.9511 -0.0213 0.070 Uiso 1 1 calc R . . C52 C 0.00465(11) 0.8055(2) -0.02234(13) 0.0565(6) Uani 1 1 d . . . H52 H -0.0322 0.8351 -0.0507 0.068 Uiso 1 1 calc R . . C62 C 0.00453(11) 0.6940(2) 0.00130(12) 0.0482(5) Uani 1 1 d . . . H62 H -0.0326 0.6468 -0.0105 0.058 Uiso 1 1 calc R . . C72 C 0.05849(9) 0.65013(18) 0.04232(10) 0.0386(4) Uani 1 1 d . . . H72 H 0.0584 0.5728 0.0580 0.046 Uiso 1 1 calc R . . C13 C 0.28179(7) 0.32742(13) 0.30004(8) 0.0236(3) Uani 1 1 d . . . O13 O 0.27943(6) 0.33926(10) 0.23882(6) 0.0292(2) Uani 1 1 d . . . O23 O 0.26033(6) 0.39894(10) 0.33726(6) 0.0286(2) Uani 1 1 d . . . C23 C 0.31166(7) 0.21889(13) 0.33170(8) 0.0233(3) Uani 1 1 d . . . C33 C 0.33138(8) 0.13083(14) 0.29352(8) 0.0265(3) Uani 1 1 d . . . H33 H 0.3279 0.1409 0.2473 0.032 Uiso 1 1 calc R . . C43 C 0.35612(9) 0.02821(14) 0.32307(9) 0.0303(3) Uani 1 1 d . . . H43 H 0.3688 -0.0324 0.2969 0.036 Uiso 1 1 calc R . . C53 C 0.36217(9) 0.01442(16) 0.39075(10) 0.0335(4) Uani 1 1 d . . . H53 H 0.3798 -0.0551 0.4110 0.040 Uiso 1 1 calc R . . C63 C 0.34252(10) 0.10190(17) 0.42901(9) 0.0372(4) Uani 1 1 d . . . H63 H 0.3464 0.0919 0.4753 0.045 Uiso 1 1 calc R . . C73 C 0.31720(9) 0.20399(15) 0.39961(9) 0.0307(3) Uani 1 1 d . . . H73 H 0.3036 0.2637 0.4258 0.037 Uiso 1 1 calc R . . C14 C 0.11901(8) 0.42926(14) 0.25451(8) 0.0255(3) Uani 1 1 d . . . O14 O 0.14903(6) 0.40100(11) 0.20937(6) 0.0304(3) Uani 1 1 d . . . O24 O 0.13782(6) 0.50317(11) 0.29906(6) 0.0285(2) Uani 1 1 d . . . C24 C 0.05689(8) 0.36860(14) 0.25834(9) 0.0285(3) Uani 1 1 d . . . C34 C 0.03289(10) 0.28454(18) 0.21250(10) 0.0389(4) Uani 1 1 d . . . H34 H 0.0537 0.2701 0.1760 0.047 Uiso 1 1 calc R . . C44 C -0.02153(11) 0.2213(2) 0.21975(12) 0.0465(5) Uani 1 1 d . . . H44 H -0.0377 0.1635 0.1883 0.056 Uiso 1 1 calc R . . C54 C -0.05208(10) 0.24212(19) 0.27241(12) 0.0439(5) Uani 1 1 d . . . H54 H -0.0885 0.1974 0.2780 0.053 Uiso 1 1 calc R . . C64 C -0.02965(10) 0.32794(19) 0.31687(12) 0.0425(5) Uani 1 1 d . . . H64 H -0.0516 0.3442 0.3523 0.051 Uiso 1 1 calc R . . C74 C 0.02498(9) 0.39109(17) 0.31025(10) 0.0360(4) Uani 1 1 d . . . H74 H 0.0404 0.4498 0.3414 0.043 Uiso 1 1 calc R . . O15 O 0.31397(6) 0.61863(12) 0.37336(6) 0.0312(3) Uani 1 1 d . . . C15 C 0.35861(8) 0.67375(14) 0.35371(8) 0.0249(3) Uani 1 1 d . . . O25 O 0.35489(6) 0.72196(10) 0.29826(6) 0.0280(2) Uani 1 1 d . . . C25 C 0.42078(8) 0.68189(14) 0.40145(9) 0.0288(3) Uani 1 1 d . . . C35 C 0.42423(10) 0.63860(18) 0.46483(10) 0.0376(4) Uani 1 1 d . . . H35 H 0.3870 0.6058 0.4775 0.045 Uiso 1 1 calc R . . C45 C 0.48121(11) 0.6427(2) 0.50964(12) 0.0488(5) Uani 1 1 d . . . H45 H 0.4833 0.6135 0.5531 0.059 Uiso 1 1 calc R . . C55 C 0.53531(11) 0.6900(2) 0.49020(14) 0.0550(6) Uani 1 1 d . . . H55 H 0.5750 0.6920 0.5204 0.066 Uiso 1 1 calc R . . C65 C 0.53213(10) 0.73413(19) 0.42768(14) 0.0521(6) Uani 1 1 d . . . H65 H 0.5695 0.7671 0.4153 0.062 Uiso 1 1 calc R . . C75 C 0.47469(9) 0.73101(16) 0.38233(12) 0.0386(4) Uani 1 1 d . . . H75 H 0.4724 0.7619 0.3392 0.046 Uiso 1 1 calc R . . O16 O 0.19235(6) 0.72380(10) 0.33648(6) 0.0283(2) Uani 1 1 d . . . C16 C 0.20005(7) 0.81954(14) 0.30904(8) 0.0245(3) Uani 1 1 d . . . O26 O 0.23225(6) 0.83494(10) 0.26365(6) 0.0294(2) Uani 1 1 d . . . C26 C 0.16765(8) 0.92194(14) 0.33356(9) 0.0265(3) Uani 1 1 d . . . C36 C 0.12180(10) 0.90676(17) 0.37353(10) 0.0373(4) Uani 1 1 d . . . H36 H 0.1123 0.8312 0.3873 0.045 Uiso 1 1 calc R . . C46 C 0.08965(12) 1.0020(2) 0.39340(12) 0.0469(5) Uani 1 1 d . . . H46 H 0.0577 0.9911 0.4200 0.056 Uiso 1 1 calc R . . C56 C 0.10404(10) 1.11247(18) 0.37450(11) 0.0425(5) Uani 1 1 d . . . H56 H 0.0814 1.1774 0.3873 0.051 Uiso 1 1 calc R . . C66 C 0.15103(10) 1.12751(17) 0.33727(13) 0.0450(5) Uani 1 1 d . . . H66 H 0.1624 1.2036 0.3261 0.054 Uiso 1 1 calc R . . C76 C 0.18233(9) 1.03300(16) 0.31556(12) 0.0398(5) Uani 1 1 d . . . H76 H 0.2138 1.0446 0.2884 0.048 Uiso 1 1 calc R . . O17 O 0.21514(7) 0.33909(11) 0.10708(6) 0.0360(3) Uani 1 1 d . . . H17 H 0.1773 0.2946 0.1156 0.043 Uiso 1 1 d R . . C27 C 0.20392(15) 0.3611(2) 0.03814(10) 0.0556(6) Uani 1 1 d . . . H27A H 0.1631 0.4029 0.0257 0.083 Uiso 1 1 calc R . . H27B H 0.2017 0.2875 0.0142 0.083 Uiso 1 1 calc R . . H27C H 0.2392 0.4081 0.0270 0.083 Uiso 1 1 calc R . . O18 O 0.20904(7) 0.54233(10) 0.42350(6) 0.0315(3) Uani 1 1 d . . . H18 H 0.2504 0.5573 0.4534 0.038 Uiso 1 1 d R . . C28 C 0.18355(11) 0.44022(17) 0.44753(10) 0.0402(4) Uani 1 1 d . . . H28A H 0.1449 0.4161 0.4168 0.060 Uiso 1 1 calc R . . H28B H 0.1724 0.4557 0.4909 0.060 Uiso 1 1 calc R . . H28C H 0.2158 0.3784 0.4515 0.060 Uiso 1 1 calc R . . O19 O 0.16911(10) 0.12845(16) 0.11448(12) 0.0682(5) Uani 1 1 d . . . H19 H 0.2079 0.1077 0.1201 0.102 Uiso 1 1 calc R . . C29 C 0.1396(2) 0.0735(4) 0.1569(2) 0.1167(18) Uani 1 1 d . . . H29A H 0.1606 -0.0013 0.1682 0.175 Uiso 1 1 calc R . . H29B H 0.0943 0.0609 0.1371 0.175 Uiso 1 1 calc R . . H29C H 0.1419 0.1203 0.1970 0.175 Uiso 1 1 calc R . . O110 O 0.27739(9) 0.01860(18) 0.10774(11) 0.0677(6) Uani 1 1 d . . . H110 H 0.2961 -0.0352 0.1311 0.102 Uiso 1 1 calc R . . C210 C 0.32279(14) 0.0795(3) 0.07765(19) 0.0807(11) Uani 1 1 d . . . H21A H 0.3322 0.1544 0.0996 0.121 Uiso 1 1 calc R . . H21B H 0.3050 0.0921 0.0309 0.121 Uiso 1 1 calc R . . H21C H 0.3625 0.0341 0.0816 0.121 Uiso 1 1 calc R . . O111 O 0.72787(8) 0.31572(14) 0.48517(7) 0.0466(4) Uani 1 1 d . . . H111 H 0.7370 0.3199 0.4472 0.070 Uiso 1 1 calc R . . C211 C 0.72804(12) 0.19892(19) 0.50484(10) 0.0449(5) Uani 1 1 d . . . H21D H 0.7726 0.1728 0.5189 0.067 Uiso 1 1 calc R . . H21E H 0.7072 0.1514 0.4677 0.067 Uiso 1 1 calc R . . H21F H 0.7045 0.1912 0.5416 0.067 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 0.02549(11) 0.01750(11) 0.02533(11) 0.00186(8) 0.00946(8) -0.00020(8) Fe2 0.03304(12) 0.01766(11) 0.02208(11) 0.00064(8) 0.00768(9) -0.00066(8) Fe3 0.02536(11) 0.01558(10) 0.02279(11) 0.00044(7) 0.00808(8) -0.00024(8) O1 0.0296(5) 0.0175(5) 0.0228(5) 0.0014(4) 0.0082(4) -0.0009(4) C11 0.0274(7) 0.0283(8) 0.0249(7) 0.0029(6) 0.0111(6) 0.0000(6) O11 0.0269(5) 0.0225(5) 0.0373(6) 0.0057(5) 0.0140(5) 0.0012(4) C21 0.0335(8) 0.0305(9) 0.0325(9) -0.0022(7) 0.0140(7) -0.0023(7) C31 0.0328(9) 0.0427(10) 0.0349(9) -0.0078(8) 0.0110(7) -0.0093(8) C41 0.0267(8) 0.0530(12) 0.0409(10) -0.0097(9) 0.0078(7) -0.0006(8) C51 0.0269(8) 0.0418(10) 0.0353(9) -0.0050(8) 0.0077(7) 0.0041(7) C61 0.0288(8) 0.0289(8) 0.0250(7) 0.0006(6) 0.0093(6) 0.0024(6) C71 0.0324(8) 0.0251(8) 0.0258(7) 0.0040(6) 0.0117(6) 0.0052(6) N81 0.0305(7) 0.0220(6) 0.0248(6) 0.0016(5) 0.0092(5) 0.0002(5) O91 0.0390(6) 0.0212(5) 0.0294(6) -0.0031(4) 0.0140(5) -0.0026(5) C101 0.0365(9) 0.0267(8) 0.0424(10) 0.0001(7) 0.0188(8) 0.0046(7) C111 0.0477(11) 0.0398(10) 0.0337(9) -0.0083(8) 0.0155(8) -0.0003(8) O12 0.0304(6) 0.0253(6) 0.0316(6) 0.0057(5) 0.0063(5) -0.0010(5) C12 0.0308(8) 0.0263(8) 0.0253(7) 0.0046(6) 0.0088(6) 0.0014(6) C22 0.0288(8) 0.0327(9) 0.0309(8) 0.0046(7) 0.0080(6) 0.0039(7) O22 0.0380(6) 0.0245(6) 0.0301(6) 0.0025(5) 0.0029(5) -0.0004(5) C32 0.0317(9) 0.0428(11) 0.0613(13) 0.0226(10) 0.0062(9) 0.0020(8) C42 0.0442(12) 0.0532(14) 0.0750(17) 0.0307(13) 0.0004(11) 0.0073(11) C52 0.0398(11) 0.0659(16) 0.0587(14) 0.0107(12) -0.0048(10) 0.0131(11) C62 0.0359(10) 0.0519(13) 0.0535(13) -0.0057(10) -0.0011(9) 0.0000(9) C72 0.0374(9) 0.0347(10) 0.0429(10) -0.0021(8) 0.0048(8) -0.0003(8) C13 0.0255(7) 0.0181(7) 0.0286(7) 0.0010(6) 0.0084(6) 0.0000(6) O13 0.0394(6) 0.0223(6) 0.0279(6) 0.0024(4) 0.0114(5) 0.0054(5) O23 0.0379(6) 0.0205(5) 0.0298(6) 0.0019(4) 0.0125(5) 0.0062(5) C23 0.0243(7) 0.0175(7) 0.0287(8) 0.0004(5) 0.0060(6) 0.0002(5) C33 0.0314(8) 0.0219(7) 0.0279(8) 0.0002(6) 0.0100(6) 0.0013(6) C43 0.0351(8) 0.0208(7) 0.0369(9) -0.0017(6) 0.0118(7) 0.0037(6) C53 0.0379(9) 0.0247(8) 0.0377(9) 0.0056(7) 0.0058(7) 0.0088(7) C63 0.0478(10) 0.0345(9) 0.0277(8) 0.0026(7) 0.0024(7) 0.0120(8) C73 0.0377(9) 0.0255(8) 0.0280(8) -0.0032(6) 0.0034(7) 0.0068(7) C14 0.0264(7) 0.0201(7) 0.0302(8) 0.0040(6) 0.0051(6) -0.0001(6) O14 0.0351(6) 0.0265(6) 0.0308(6) -0.0016(5) 0.0092(5) -0.0055(5) O24 0.0286(6) 0.0239(6) 0.0344(6) -0.0034(5) 0.0098(5) -0.0035(5) C24 0.0268(7) 0.0227(7) 0.0353(9) 0.0033(6) 0.0037(6) -0.0011(6) C34 0.0389(10) 0.0369(10) 0.0406(10) -0.0036(8) 0.0058(8) -0.0087(8) C44 0.0422(11) 0.0402(11) 0.0542(13) -0.0052(9) 0.0006(9) -0.0154(9) C54 0.0295(9) 0.0398(11) 0.0606(13) 0.0091(10) 0.0033(9) -0.0094(8) C64 0.0337(9) 0.0393(11) 0.0578(13) 0.0043(9) 0.0171(9) -0.0041(8) C74 0.0326(9) 0.0299(9) 0.0472(11) -0.0010(8) 0.0118(8) -0.0045(7) O15 0.0299(6) 0.0375(7) 0.0265(6) 0.0035(5) 0.0061(5) -0.0056(5) C15 0.0262(7) 0.0213(7) 0.0279(7) -0.0034(6) 0.0065(6) 0.0022(6) O25 0.0308(6) 0.0255(6) 0.0286(6) 0.0004(4) 0.0080(5) -0.0031(5) C25 0.0274(7) 0.0214(7) 0.0368(9) -0.0045(6) 0.0032(6) 0.0023(6) C35 0.0357(9) 0.0365(10) 0.0379(10) -0.0014(8) -0.0003(7) 0.0010(8) C45 0.0485(12) 0.0435(12) 0.0476(12) -0.0020(9) -0.0100(9) 0.0036(10) C55 0.0393(11) 0.0368(11) 0.0783(17) -0.0049(11) -0.0189(11) 0.0020(9) C65 0.0293(9) 0.0333(10) 0.0898(19) -0.0008(11) -0.0001(10) -0.0058(8) C75 0.0305(9) 0.0260(9) 0.0593(13) 0.0007(8) 0.0081(8) -0.0001(7) O16 0.0361(6) 0.0187(5) 0.0325(6) 0.0002(4) 0.0128(5) 0.0027(5) C16 0.0237(7) 0.0188(7) 0.0310(8) -0.0024(6) 0.0049(6) -0.0002(6) O26 0.0315(6) 0.0195(5) 0.0404(7) 0.0002(5) 0.0154(5) 0.0001(4) C26 0.0254(7) 0.0205(7) 0.0334(8) -0.0037(6) 0.0039(6) 0.0027(6) C36 0.0492(11) 0.0266(8) 0.0397(10) 0.0010(7) 0.0183(8) 0.0057(8) C46 0.0595(13) 0.0382(11) 0.0494(12) -0.0008(9) 0.0269(10) 0.0141(10) C56 0.0453(11) 0.0298(9) 0.0519(12) -0.0069(8) 0.0071(9) 0.0149(8) C66 0.0365(10) 0.0200(8) 0.0783(16) -0.0023(9) 0.0095(10) 0.0043(7) C76 0.0263(8) 0.0223(8) 0.0731(14) 0.0009(8) 0.0150(9) 0.0011(7) O17 0.0549(8) 0.0261(6) 0.0282(6) -0.0024(5) 0.0106(6) -0.0064(6) C27 0.0937(19) 0.0426(12) 0.0292(10) -0.0054(9) 0.0077(11) 0.0002(12) O18 0.0446(7) 0.0242(6) 0.0284(6) 0.0002(5) 0.0143(5) -0.0054(5) C28 0.0589(12) 0.0315(9) 0.0355(10) 0.0019(7) 0.0227(9) -0.0096(9) O19 0.0701(12) 0.0378(9) 0.0994(16) 0.0071(9) 0.0227(11) -0.0019(9) C29 0.144(4) 0.113(3) 0.112(3) 0.067(3) 0.073(3) 0.064(3) O110 0.0545(10) 0.0660(12) 0.0838(14) 0.0372(11) 0.0153(10) 0.0129(9) C210 0.0544(15) 0.083(2) 0.101(3) 0.050(2) 0.0039(16) -0.0059(15) O111 0.0677(10) 0.0414(8) 0.0354(7) -0.0066(6) 0.0221(7) -0.0101(7) C211 0.0632(13) 0.0399(11) 0.0340(10) -0.0069(8) 0.0150(9) -0.0117(10) _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 O1 1.9238(11) . ? Fe1 O11 1.9501(11) . ? Fe1 O26 2.0318(12) . ? Fe1 O25 2.0478(13) . ? Fe1 O12 2.0722(12) . ? Fe1 N81 2.1197(14) . ? Fe2 O1 1.8872(11) . ? Fe2 O91 1.9378(12) . ? Fe2 O13 2.0333(12) . ? Fe2 O22 2.0438(13) . ? Fe2 O17 2.0790(13) . ? Fe2 O14 2.0816(12) . ? Fe3 O1 1.8661(11) . ? Fe3 O16 1.9991(12) . ? Fe3 O15 1.9994(12) . ? Fe3 O24 2.0079(12) . ? Fe3 O23 2.0362(12) . ? Fe3 O18 2.0986(12) . ? C11 O11 1.3413(19) . ? C11 C21 1.406(2) . ? C11 C61 1.417(2) . ? C21 C31 1.386(3) . ? C31 C41 1.386(3) . ? C41 C51 1.379(3) . ? C51 C61 1.412(2) . ? C61 C71 1.471(2) . ? C71 N81 1.304(2) . ? C71 C101 1.506(2) . ? N81 O91 1.3745(18) . ? C101 C111 1.521(3) . ? O12 C12 1.271(2) . ? C12 O22 1.256(2) . ? C12 C22 1.498(2) . ? C22 C32 1.388(3) . ? C22 C72 1.393(3) . ? C32 C42 1.392(3) . ? C42 C52 1.381(4) . ? C52 C62 1.378(4) . ? C62 C72 1.387(3) . ? C13 O13 1.261(2) . ? C13 O23 1.2641(19) . ? C13 C23 1.499(2) . ? C23 C33 1.393(2) . ? C23 C73 1.394(2) . ? C33 C43 1.391(2) . ? C43 C53 1.386(3) . ? C53 C63 1.389(3) . ? C63 C73 1.388(2) . ? C14 O14 1.257(2) . ? C14 O24 1.265(2) . ? C14 C24 1.500(2) . ? C24 C74 1.385(3) . ? C24 C34 1.386(3) . ? C34 C44 1.391(3) . ? C44 C54 1.377(3) . ? C54 C64 1.375(3) . ? C64 C74 1.390(3) . ? O15 C15 1.261(2) . ? C15 O25 1.261(2) . ? C15 C25 1.496(2) . ? C25 C35 1.388(3) . ? C25 C75 1.388(3) . ? C35 C45 1.380(3) . ? C45 C55 1.387(4) . ? C55 C65 1.375(4) . ? C65 C75 1.393(3) . ? O16 C16 1.265(2) . ? C16 O26 1.262(2) . ? C16 C26 1.497(2) . ? C26 C76 1.385(2) . ? C26 C36 1.388(3) . ? C36 C46 1.391(3) . ? C46 C56 1.383(3) . ? C56 C66 1.367(3) . ? C66 C76 1.390(3) . ? O17 C27 1.421(2) . ? O18 C28 1.421(2) . ? O19 C29 1.322(4) . ? O110 C210 1.416(3) . ? O111 C211 1.408(3) . ? 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 O1 Fe1 O11 167.57(5) . . ? O1 Fe1 O26 95.21(5) . . ? O11 Fe1 O26 97.21(5) . . ? O1 Fe1 O25 92.30(5) . . ? O11 Fe1 O25 87.85(5) . . ? O26 Fe1 O25 89.49(5) . . ? O1 Fe1 O12 91.63(5) . . ? O11 Fe1 O12 88.70(5) . . ? O26 Fe1 O12 88.35(5) . . ? O25 Fe1 O12 175.67(5) . . ? O1 Fe1 N81 84.53(5) . . ? O11 Fe1 N81 83.04(5) . . ? O26 Fe1 N81 179.67(5) . . ? O25 Fe1 N81 90.31(5) . . ? O12 Fe1 N81 91.88(5) . . ? O1 Fe2 O91 92.05(5) . . ? O1 Fe2 O13 97.51(5) . . ? O91 Fe2 O13 94.21(5) . . ? O1 Fe2 O22 90.87(5) . . ? O91 Fe2 O22 94.55(5) . . ? O13 Fe2 O22 167.65(5) . . ? O1 Fe2 O17 176.24(5) . . ? O91 Fe2 O17 87.21(5) . . ? O13 Fe2 O17 86.23(5) . . ? O22 Fe2 O17 85.52(5) . . ? O1 Fe2 O14 95.47(5) . . ? O91 Fe2 O14 172.42(5) . . ? O13 Fe2 O14 85.81(5) . . ? O22 Fe2 O14 84.37(5) . . ? O17 Fe2 O14 85.22(5) . . ? O1 Fe3 O16 95.90(5) . . ? O1 Fe3 O15 95.02(5) . . ? O16 Fe3 O15 89.61(5) . . ? O1 Fe3 O24 96.05(5) . . ? O16 Fe3 O24 90.47(5) . . ? O15 Fe3 O24 168.87(5) . . ? O1 Fe3 O23 95.61(5) . . ? O16 Fe3 O23 168.47(5) . . ? O15 Fe3 O23 88.78(5) . . ? O24 Fe3 O23 88.92(5) . . ? O1 Fe3 O18 179.16(5) . . ? O16 Fe3 O18 83.87(5) . . ? O15 Fe3 O18 84.17(5) . . ? O24 Fe3 O18 84.77(5) . . ? O23 Fe3 O18 84.61(5) . . ? Fe3 O1 Fe2 120.65(6) . . ? Fe3 O1 Fe1 122.66(6) . . ? Fe2 O1 Fe1 116.44(6) . . ? O11 C11 C21 118.33(15) . . ? O11 C11 C61 122.65(15) . . ? C21 C11 C61 119.01(15) . . ? C11 O11 Fe1 123.00(10) . . ? C31 C21 C11 121.44(17) . . ? C41 C31 C21 119.73(18) . . ? C51 C41 C31 119.76(17) . . ? C41 C51 C61 122.15(18) . . ? C51 C61 C11 117.75(16) . . ? C51 C61 C71 118.96(16) . . ? C11 C61 C71 123.21(15) . . ? N81 C71 C61 118.73(15) . . ? N81 C71 C101 121.00(16) . . ? C61 C71 C101 120.22(15) . . ? C71 N81 O91 117.01(13) . . ? C71 N81 Fe1 127.38(12) . . ? O91 N81 Fe1 115.53(9) . . ? N81 O91 Fe2 117.37(9) . . ? C71 C101 C111 113.22(15) . . ? C12 O12 Fe1 130.75(11) . . ? O22 C12 O12 125.58(16) . . ? O22 C12 C22 115.90(16) . . ? O12 C12 C22 118.52(15) . . ? C32 C22 C72 119.68(18) . . ? C32 C22 C12 121.12(17) . . ? C72 C22 C12 119.17(16) . . ? C12 O22 Fe2 129.59(12) . . ? C22 C32 C42 119.5(2) . . ? C52 C42 C32 120.6(2) . . ? C62 C52 C42 119.9(2) . . ? C52 C62 C72 120.3(2) . . ? C62 C72 C22 120.0(2) . . ? O13 C13 O23 125.52(15) . . ? O13 C13 C23 117.71(14) . . ? O23 C13 C23 116.77(14) . . ? C13 O13 Fe2 126.78(10) . . ? C13 O23 Fe3 135.00(11) . . ? C33 C23 C73 119.74(15) . . ? C33 C23 C13 120.60(15) . . ? C73 C23 C13 119.60(14) . . ? C43 C33 C23 120.08(16) . . ? C53 C43 C33 119.90(16) . . ? C43 C53 C63 120.23(16) . . ? C73 C63 C53 120.03(17) . . ? C63 C73 C23 120.01(16) . . ? O14 C14 O24 125.28(15) . . ? O14 C14 C24 118.48(15) . . ? O24 C14 C24 116.21(15) . . ? C14 O14 Fe2 132.81(11) . . ? C14 O24 Fe3 127.54(11) . . ? C74 C24 C34 119.25(17) . . ? C74 C24 C14 120.10(16) . . ? C34 C24 C14 120.53(16) . . ? C24 C34 C44 120.2(2) . . ? C54 C44 C34 120.2(2) . . ? C64 C54 C44 119.76(18) . . ? C54 C64 C74 120.4(2) . . ? C24 C74 C64 120.11(19) . . ? C15 O15 Fe3 132.50(11) . . ? O25 C15 O15 125.69(15) . . ? O25 C15 C25 118.32(15) . . ? O15 C15 C25 115.98(15) . . ? C15 O25 Fe1 132.40(11) . . ? C35 C25 C75 120.32(17) . . ? C35 C25 C15 119.30(16) . . ? C75 C25 C15 120.38(17) . . ? C45 C35 C25 120.7(2) . . ? C35 C45 C55 118.9(2) . . ? C65 C55 C45 120.7(2) . . ? C55 C65 C75 120.7(2) . . ? C25 C75 C65 118.6(2) . . ? C16 O16 Fe3 132.97(11) . . ? O26 C16 O16 125.64(15) . . ? O26 C16 C26 118.44(14) . . ? O16 C16 C26 115.92(14) . . ? C16 O26 Fe1 132.32(11) . . ? C76 C26 C36 119.21(16) . . ? C76 C26 C16 120.26(16) . . ? C36 C26 C16 120.52(15) . . ? C26 C36 C46 120.12(19) . . ? C56 C46 C36 120.2(2) . . ? C66 C56 C46 119.47(18) . . ? C56 C66 C76 120.89(19) . . ? C26 C76 C66 119.97(19) . . ? C27 O17 Fe2 125.23(13) . . ? C28 O18 Fe3 125.19(11) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.987 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.089 # Attachment 'complex 3.cif' data_EB7168 _database_code_depnum_ccdc_archive 'CCDC 667680' _audit_creation_date 07-10-22 _audit_creation_method CRYSTALS_ver_12.85 _chemical_formula_moiety 'C64 H60 Fe4 N8 O16, C H4 O' _chemical_compound_source 'Ian Gass, IAG2196' _exptl_crystal_recrystallization_method ; Slow evaporation from MeOH. ; _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ _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: ; 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. The H atoms attached to carbon atoms were positioned geometrically. H atoms in hydroxy groups were positioned on the basis of likely hydrogen bonds at a distance of 0.85\%A. 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. 601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 135.00 A**3 SQUEEZE was applied, accounting for 1 molecule of MeOH solvent per molecule of complex (95 electrons per cell). 912_ALERT_3_B # Missing FCF Reflections Above STh/L= 0.600 876 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 2 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 3 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 2 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 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 1.000 6854 6852 2 23.01 0.550 1.000 9124 9122 2 25.24 0.600 1.000 11834 11829 5 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.998 15067 15041 26 29.84 0.700 0.974 18757 18271 486 30.51 0.714 0.956 19921 19040 881 097_ALERT_2_C Maximum (Positive) Residual Density ............ 2.33 e/A** 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.01 Ratio 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 No action taken. ; _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 13.4558(3) _cell_length_b 18.4743(5) _cell_length_c 26.9983(7) _cell_angle_alpha 90 _cell_angle_beta 102.7650(10) _cell_angle_gamma 90 _cell_volume 6545.5(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-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 4 # Given Formula = C65 H82 Fe4 N8 O17 # Dc = 1.49 Fooo = 2928.00 Mu = 9.45 M = 1470.80 # Found Formula = C64 H60 Fe4 N8 O16 # Dc = 1.44 FOOO = 2928.00 Mu = 9.42 M = 1420.61 _chemical_formula_sum 'C65 H64 Fe4 N8 O17' _chemical_formula_weight 1452.65 _cell_measurement_reflns_used 7180 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.942 # Sheldrick geometric approximatio 0.83 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.84 _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 97083 _reflns_number_total 19572 _diffrn_reflns_av_R_equivalents 0.068 # Number of reflections with Friedels Law is 19040 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 19985 _diffrn_reflns_theta_min 1.573 _diffrn_reflns_theta_max 30.509 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.068 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 36 _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 -1.63 _refine_diff_density_max 2.33 # 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 19040 _refine_ls_number_restraints 0 _refine_ls_number_parameters 829 _oxford_refine_ls_R_factor_ref 0.1546 _refine_ls_wR_factor_ref 0.2116 _refine_ls_goodness_of_fit_ref 0.9134 _refine_ls_shift/su_max 0.000374 # The values computed from all data _oxford_reflns_number_all 19040 _refine_ls_R_factor_all 0.1546 _refine_ls_wR_factor_all 0.2116 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10934 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_gt 0.1911 # 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^ + 0.00P] ,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. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. 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 # 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 0.223 0.181 0.894 133.2 23.0 2 0.097 0.422 0.303 7.8 0.4 3 0.277 0.681 0.606 133.2 23.6 4 0.403 0.922 0.197 7.7 0.3 5 0.723 0.319 0.394 133.2 23.8 6 0.777 0.819 0.106 133.2 23.5 7 0.597 0.078 0.803 7.8 0.3 8 0.903 0.578 0.697 7.7 0.3 _platon_squeeze_details ; 95 electrons per cell of residual electron density were found, which accounts of 4 molecules of MeOH (solvent) in the cell. ; 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 0.84816(6) 0.37917(4) 0.10477(3) 0.0281 1.0000 Uani . . . . . . . O1 O 0.9683(3) 0.41945(18) 0.14874(12) 0.0313 1.0000 Uani . . . . . . . Fe2 Fe 0.94585(6) 0.21416(4) 0.16430(3) 0.0268 1.0000 Uani . . . . . . . C2 C 1.0006(4) 0.4842(3) 0.13539(17) 0.0320 1.0000 Uani . . . . . . . Fe3 Fe 0.76642(6) 0.18506(4) 0.04720(3) 0.0285 1.0000 Uani . . . . . . . C3 C 1.1042(5) 0.4935(3) 0.1366(2) 0.0405 1.0000 Uani . . . . . . . Fe4 Fe 0.65926(6) 0.27075(4) 0.14183(3) 0.0292 1.0000 Uani . . . . . . . C4 C 1.1399(5) 0.5573(4) 0.1216(2) 0.0498 1.0000 Uani . . . . . . . C5 C 1.0738(6) 0.6140(4) 0.1055(2) 0.0533 1.0000 Uani . . . . . . . C6 C 0.9739(5) 0.6075(3) 0.1061(2) 0.0483 1.0000 Uani . . . . . . . C7 C 0.9342(4) 0.5429(3) 0.12067(19) 0.0354 1.0000 Uani . . . . . . . C8 C 0.8263(5) 0.5404(3) 0.1243(2) 0.0402 1.0000 Uani . . . . . . . N9 N 0.7805(4) 0.4788(2) 0.12200(16) 0.0349 1.0000 Uani . . . . . . . O10 O 0.6802(3) 0.4846(2) 0.12675(17) 0.0489 1.0000 Uani . . . . . . . C11 C 0.7705(5) 0.6090(3) 0.1324(3) 0.0652 1.0000 Uani . . . . . . . O12 O 0.8636(3) 0.42009(19) 0.04194(13) 0.0338 1.0000 Uani . . . . . . . C13 C 0.7902(5) 0.4571(3) 0.01124(18) 0.0357 1.0000 Uani . . . . . . . C14 C 0.8164(5) 0.5201(3) -0.0117(2) 0.0437 1.0000 Uani . . . . . . . C15 C 0.7437(6) 0.5616(4) -0.0420(2) 0.0562 1.0000 Uani . . . . . . . C16 C 0.6427(6) 0.5415(4) -0.0519(2) 0.0561 1.0000 Uani . . . . . . . C17 C 0.6137(5) 0.4797(3) -0.0315(2) 0.0471 1.0000 Uani . . . . . . . C18 C 0.6859(4) 0.4352(3) 0.00003(19) 0.0348 1.0000 Uani . . . . . . . C19 C 0.6549(4) 0.3660(3) 0.01899(18) 0.0298 1.0000 Uani . . . . . . . N20 N 0.7154(3) 0.3367(2) 0.05724(15) 0.0301 1.0000 Uani . . . . . . . O21 O 0.6854(3) 0.26710(18) 0.07011(13) 0.0295 1.0000 Uani . . . . . . . C22 C 0.5571(4) 0.3295(3) -0.0060(2) 0.0403 1.0000 Uani . . . . . . . O23 O 0.5866(3) 0.36136(19) 0.13568(15) 0.0360 1.0000 Uani . . . . . . . C24 C 0.5071(5) 0.3696(3) 0.1585(2) 0.0379 1.0000 Uani . . . . . . . C25 C 0.5039(5) 0.4317(3) 0.1869(3) 0.0532 1.0000 Uani . . . . . . . C26 C 0.4238(6) 0.4432(4) 0.2107(3) 0.0701 1.0000 Uani . . . . . . . C27 C 0.3460(6) 0.3924(4) 0.2056(3) 0.0664 1.0000 Uani . . . . . . . C28 C 0.3493(5) 0.3314(4) 0.1776(3) 0.0558 1.0000 Uani . . . . . . . C29 C 0.4289(4) 0.3176(3) 0.1531(2) 0.0412 1.0000 Uani . . . . . . . C30 C 0.4260(5) 0.2508(4) 0.1227(2) 0.0468 1.0000 Uani . . . . . . . N31 N 0.5088(4) 0.2284(3) 0.11043(17) 0.0369 1.0000 Uani . . . . . . . H31 H 1.1492 0.4556 0.1475 0.0478 1.0000 Uiso R . . . . . . O32 O 0.4936(3) 0.1661(3) 0.08092(19) 0.0602 1.0000 Uani . . . . . . . C33 C 0.3272(5) 0.2086(5) 0.1070(4) 0.0881 1.0000 Uani . . . . . . . O34 O 0.6426(3) 0.2461(2) 0.20803(14) 0.0353 1.0000 Uani . . . . . . . C35 C 0.6106(4) 0.1814(3) 0.2205(2) 0.0349 1.0000 Uani . . . . . . . C36 C 0.5409(4) 0.1796(4) 0.2521(2) 0.0421 1.0000 Uani . . . . . . . C37 C 0.5050(5) 0.1147(4) 0.2657(2) 0.0485 1.0000 Uani . . . . . . . C38 C 0.5364(5) 0.0503(4) 0.2488(2) 0.0507 1.0000 Uani . . . . . . . C39 C 0.6047(5) 0.0508(3) 0.2181(2) 0.0421 1.0000 Uani . . . . . . . C40 C 0.6441(4) 0.1156(3) 0.20347(19) 0.0335 1.0000 Uani . . . . . . . C41 C 0.7227(4) 0.1122(3) 0.17305(19) 0.0314 1.0000 Uani . . . . . . . H41 H 1.2089 0.5629 0.1224 0.0608 1.0000 Uiso R . . . . . . N42 N 0.7365(3) 0.1701(2) 0.14829(15) 0.0290 1.0000 Uani . . . . . . . O43 O 0.8179(3) 0.16581(19) 0.12337(13) 0.0294 1.0000 Uani . . . . . . . C44 C 0.7835(5) 0.0461(3) 0.1708(2) 0.0425 1.0000 Uani . . . . . . . O45 O 0.9442(3) 0.16458(19) 0.22671(13) 0.0333 1.0000 Uani . . . . . . . C46 C 0.9702(4) 0.1952(3) 0.2721(2) 0.0346 1.0000 Uani . . . . . . . C47 C 1.0283(5) 0.1554(4) 0.3121(2) 0.0489 1.0000 Uani . . . . . . . C48 C 1.0641(6) 0.1864(4) 0.3592(2) 0.0594 1.0000 Uani . . . . . . . C49 C 1.0421(6) 0.2570(4) 0.3683(2) 0.0584 1.0000 Uani . . . . . . . C50 C 0.9807(5) 0.2960(4) 0.3306(2) 0.0480 1.0000 Uani . . . . . . . C51 C 0.9430(5) 0.2666(3) 0.28203(19) 0.0375 1.0000 Uani . . . . . . . C52 C 0.8731(4) 0.3088(3) 0.24326(19) 0.0325 1.0000 Uani . . . . . . . N53 N 0.8664(3) 0.2939(2) 0.19601(15) 0.0285 1.0000 Uani . . . . . . . O54 O 0.7898(3) 0.33094(18) 0.16132(12) 0.0290 1.0000 Uani . . . . . . . C55 C 0.8071(6) 0.3672(3) 0.2568(2) 0.0571 1.0000 Uani . . . . . . . O56 O 1.0317(3) 0.1496(2) 0.13645(13) 0.0359 1.0000 Uani . . . . . . . C57 C 1.1096(4) 0.1141(3) 0.1665(2) 0.0371 1.0000 Uani . . . . . . . C58 C 1.1343(5) 0.0448(3) 0.1531(2) 0.0449 1.0000 Uani . . . . . . . C59 C 1.2102(5) 0.0061(4) 0.1827(3) 0.0510 1.0000 Uani . . . . . . . C60 C 1.2636(5) 0.0327(3) 0.2285(3) 0.0507 1.0000 Uani . . . . . . . C61 C 1.2433(4) 0.1011(4) 0.2419(2) 0.0467 1.0000 Uani . . . . . . . C62 C 1.1681(4) 0.1455(3) 0.2115(2) 0.0355 1.0000 Uani . . . . . . . C63 C 1.1614(4) 0.2225(3) 0.2258(2) 0.0355 1.0000 Uani . . . . . . . N64 N 1.0896(3) 0.2627(2) 0.19939(16) 0.0332 1.0000 Uani . . . . . . . O65 O 1.0982(3) 0.3357(2) 0.21340(14) 0.0395 1.0000 Uani . . . . . . . C66 C 1.2398(5) 0.2521(4) 0.2702(2) 0.0476 1.0000 Uani . . . . . . . O67 O 0.6458(3) 0.1273(2) 0.03911(14) 0.0380 1.0000 Uani . . . . . . . C68 C 0.6163(5) 0.0864(3) -0.0034(2) 0.0383 1.0000 Uani . . . . . . . C69 C 0.5149(5) 0.0866(3) -0.0285(2) 0.0469 1.0000 Uani . . . . . . . C70 C 0.4821(6) 0.0476(4) -0.0726(3) 0.0571 1.0000 Uani . . . . . . . C71 C 0.5500(6) 0.0078(4) -0.0924(3) 0.0605 1.0000 Uani . . . . . . . C72 C 0.6499(6) 0.0048(3) -0.0671(2) 0.0536 1.0000 Uani . . . . . . . C73 C 0.6866(5) 0.0427(3) -0.0213(2) 0.0407 1.0000 Uani . . . . . . . C74 C 0.7937(5) 0.0330(3) 0.0057(2) 0.0387 1.0000 Uani . . . . . . . N75 N 0.8372(4) 0.0838(3) 0.03603(16) 0.0356 1.0000 Uani . . . . . . . O76 O 0.9368(3) 0.0662(2) 0.05932(16) 0.0488 1.0000 Uani . . . . . . . C77 C 0.8497(6) -0.0368(4) 0.0001(3) 0.0696 1.0000 Uani . . . . . . . O78 O 0.7585(3) 0.2099(2) -0.02216(13) 0.0342 1.0000 Uani . . . . . . . C79 C 0.8364(4) 0.2027(3) -0.0449(2) 0.0339 1.0000 Uani . . . . . . . C80 C 0.8168(5) 0.1761(3) -0.0951(2) 0.0420 1.0000 Uani . . . . . . . C81 C 0.8943(5) 0.1671(3) -0.1206(2) 0.0458 1.0000 Uani . . . . . . . C82 C 0.9937(5) 0.1835(4) -0.0976(2) 0.0468 1.0000 Uani . . . . . . . C83 C 1.0154(5) 0.2120(3) -0.0488(2) 0.0415 1.0000 Uani . . . . . . . C84 C 0.9378(4) 0.2224(3) -0.02230(18) 0.0330 1.0000 Uani . . . . . . . C85 C 0.9625(4) 0.2575(3) 0.02813(19) 0.0298 1.0000 Uani . . . . . . . N86 N 0.9022(3) 0.2467(2) 0.05875(15) 0.0295 1.0000 Uani . . . . . . . O87 O 0.9275(3) 0.28550(18) 0.10459(12) 0.0275 1.0000 Uani . . . . . . . C88 C 1.0543(4) 0.3050(3) 0.0435(2) 0.0406 1.0000 Uani . . . . . . . H51 H 1.0993 0.6564 0.0945 0.0599 1.0000 Uiso R . . . . . . H61 H 0.9304 0.6460 0.0966 0.0549 1.0000 Uiso R . . . . . . H101 H 0.6500 0.4450 0.1296 0.0577 1.0000 Uiso R . . . . . . H111 H 0.8174 0.6478 0.1423 0.0961 1.0000 Uiso R . . . . . . H112 H 0.7340 0.6014 0.1590 0.0961 1.0000 Uiso R . . . . . . H113 H 0.7206 0.6238 0.1008 0.0957 1.0000 Uiso R . . . . . . H141 H 0.8845 0.5333 -0.0059 0.0509 1.0000 Uiso R . . . . . . H151 H 0.7625 0.6037 -0.0564 0.0650 1.0000 Uiso R . . . . . . H161 H 0.5937 0.5698 -0.0724 0.0632 1.0000 Uiso R . . . . . . H171 H 0.5455 0.4669 -0.0387 0.0518 1.0000 Uiso R . . . . . . H221 H 0.5281 0.3530 -0.0376 0.0569 1.0000 Uiso R . . . . . . H222 H 0.5675 0.2799 -0.0121 0.0573 1.0000 Uiso R . . . . . . H223 H 0.5085 0.3331 0.0157 0.0571 1.0000 Uiso R . . . . . . H251 H 0.5565 0.4649 0.1902 0.0657 1.0000 Uiso R . . . . . . H261 H 0.4218 0.4856 0.2295 0.0878 1.0000 Uiso R . . . . . . H271 H 0.2916 0.4009 0.2213 0.0828 1.0000 Uiso R . . . . . . H281 H 0.2978 0.2973 0.1750 0.0691 1.0000 Uiso R . . . . . . H321 H 0.5424 0.1536 0.0675 0.0729 1.0000 Uiso R . . . . . . H331 H 0.3297 0.1653 0.1266 0.1337 1.0000 Uiso R . . . . . . H332 H 0.3172 0.1966 0.0715 0.1340 1.0000 Uiso R . . . . . . H333 H 0.2728 0.2380 0.1116 0.1340 1.0000 Uiso R . . . . . . H361 H 0.5195 0.2230 0.2634 0.0507 1.0000 Uiso R . . . . . . H371 H 0.4597 0.1150 0.2864 0.0581 1.0000 Uiso R . . . . . . H381 H 0.5129 0.0065 0.2582 0.0598 1.0000 Uiso R . . . . . . H391 H 0.6261 0.0078 0.2068 0.0508 1.0000 Uiso R . . . . . . H441 H 0.8246 0.0340 0.2036 0.0672 1.0000 Uiso R . . . . . . H442 H 0.8246 0.0508 0.1470 0.0674 1.0000 Uiso R . . . . . . H443 H 0.7377 0.0063 0.1603 0.0672 1.0000 Uiso R . . . . . . H471 H 1.0449 0.1073 0.3067 0.0589 1.0000 Uiso R . . . . . . H481 H 1.1052 0.1587 0.3848 0.0700 1.0000 Uiso R . . . . . . H491 H 1.0686 0.2778 0.3994 0.0722 1.0000 Uiso R . . . . . . H501 H 0.9637 0.3434 0.3374 0.0589 1.0000 Uiso R . . . . . . H551 H 0.8351 0.3872 0.2895 0.0870 1.0000 Uiso R . . . . . . H552 H 0.7961 0.4056 0.2320 0.0871 1.0000 Uiso R . . . . . . H553 H 0.7408 0.3470 0.2580 0.0873 1.0000 Uiso R . . . . . . H581 H 1.0989 0.0256 0.1230 0.0518 1.0000 Uiso R . . . . . . H591 H 1.2266 -0.0387 0.1722 0.0599 1.0000 Uiso R . . . . . . H601 H 1.3112 0.0045 0.2499 0.0579 1.0000 Uiso R . . . . . . H611 H 1.2795 0.1195 0.2727 0.0529 1.0000 Uiso R . . . . . . H651 H 1.0570 0.3623 0.1928 0.0447 1.0000 Uiso R . . . . . . H661 H 1.3080 0.2448 0.2653 0.0679 1.0000 Uiso R . . . . . . H662 H 1.2260 0.3027 0.2740 0.0683 1.0000 Uiso R . . . . . . H663 H 1.2308 0.2270 0.3008 0.0680 1.0000 Uiso R . . . . . . H691 H 0.4680 0.1125 -0.0152 0.0537 1.0000 Uiso R . . . . . . H701 H 0.4139 0.0486 -0.0889 0.0640 1.0000 Uiso R . . . . . . H711 H 0.5280 -0.0171 -0.1230 0.0668 1.0000 Uiso R . . . . . . H721 H 0.6954 -0.0228 -0.0806 0.0630 1.0000 Uiso R . . . . . . H761 H 0.9667 0.0927 0.0839 0.0541 1.0000 Uiso R . . . . . . H771 H 0.8874 -0.0288 -0.0261 0.0980 1.0000 Uiso R . . . . . . H772 H 0.8949 -0.0478 0.0314 0.0982 1.0000 Uiso R . . . . . . H773 H 0.8010 -0.0750 -0.0090 0.0979 1.0000 Uiso R . . . . . . H801 H 0.7499 0.1648 -0.1112 0.0467 1.0000 Uiso R . . . . . . H811 H 0.8785 0.1492 -0.1535 0.0551 1.0000 Uiso R . . . . . . H821 H 1.0452 0.1752 -0.1154 0.0588 1.0000 Uiso R . . . . . . H831 H 1.0824 0.2237 -0.0336 0.0502 1.0000 Uiso R . . . . . . H881 H 1.0945 0.2884 0.0748 0.0622 1.0000 Uiso R . . . . . . H882 H 1.0929 0.3051 0.0182 0.0620 1.0000 Uiso R . . . . . . H883 H 1.0305 0.3528 0.0481 0.0621 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 0.0370(4) 0.0238(3) 0.0222(3) 0.0003(3) 0.0038(3) -0.0117(3) O1 0.045(2) 0.0255(17) 0.0223(16) -0.0035(14) 0.0050(15) -0.0121(16) Fe2 0.0315(4) 0.0273(3) 0.0211(3) -0.0030(3) 0.0050(3) -0.0080(3) C2 0.047(3) 0.030(2) 0.016(2) -0.0007(19) 0.000(2) -0.015(2) Fe3 0.0349(4) 0.0263(3) 0.0234(3) -0.0021(3) 0.0046(3) -0.0122(3) C3 0.055(4) 0.038(3) 0.027(3) -0.006(2) 0.007(3) -0.017(3) Fe4 0.0327(4) 0.0255(3) 0.0304(4) 0.0035(3) 0.0090(3) -0.0058(3) C4 0.056(4) 0.053(4) 0.043(3) -0.009(3) 0.018(3) -0.029(3) C5 0.074(5) 0.046(4) 0.035(3) 0.004(3) 0.003(3) -0.034(4) C6 0.065(4) 0.035(3) 0.040(3) 0.005(3) -0.001(3) -0.022(3) C7 0.046(3) 0.029(3) 0.026(2) 0.001(2) -0.003(2) -0.018(2) C8 0.053(4) 0.024(2) 0.039(3) 0.006(2) -0.002(3) -0.006(2) N9 0.043(3) 0.031(2) 0.030(2) 0.0010(18) 0.006(2) -0.011(2) O10 0.048(3) 0.031(2) 0.069(3) -0.001(2) 0.017(2) -0.0061(19) C11 0.051(4) 0.025(3) 0.111(7) 0.002(4) -0.001(4) -0.001(3) O12 0.043(2) 0.0325(19) 0.0250(17) 0.0020(15) 0.0060(16) -0.0131(17) C13 0.051(3) 0.035(3) 0.020(2) -0.002(2) 0.006(2) -0.015(3) C14 0.062(4) 0.043(3) 0.024(2) 0.005(2) 0.004(3) -0.028(3) C15 0.083(5) 0.042(3) 0.035(3) 0.016(3) -0.005(3) -0.025(3) C16 0.075(5) 0.044(4) 0.039(3) 0.018(3) -0.009(3) -0.008(3) C17 0.055(4) 0.037(3) 0.043(3) 0.012(3) -0.003(3) -0.010(3) C18 0.045(3) 0.035(3) 0.023(2) 0.000(2) 0.006(2) -0.009(2) C19 0.033(3) 0.034(3) 0.021(2) -0.002(2) 0.002(2) -0.011(2) N20 0.039(2) 0.025(2) 0.027(2) 0.0018(17) 0.0079(18) -0.0091(18) O21 0.035(2) 0.0235(16) 0.0295(17) 0.0030(14) 0.0068(15) -0.0120(15) C22 0.037(3) 0.043(3) 0.035(3) 0.006(2) -0.003(2) -0.017(3) O23 0.037(2) 0.0305(19) 0.042(2) 0.0096(17) 0.0131(18) 0.0011(16) C24 0.041(3) 0.034(3) 0.038(3) 0.017(2) 0.007(2) 0.009(2) C25 0.054(4) 0.036(3) 0.075(5) 0.013(3) 0.025(4) 0.004(3) C26 0.073(5) 0.041(4) 0.107(7) 0.000(4) 0.043(5) 0.012(4) C27 0.054(4) 0.049(4) 0.107(7) 0.001(4) 0.040(5) 0.013(3) C28 0.036(3) 0.059(4) 0.076(5) 0.020(4) 0.022(3) 0.007(3) C29 0.032(3) 0.048(3) 0.045(3) 0.020(3) 0.013(3) 0.007(3) C30 0.038(3) 0.056(4) 0.043(3) 0.007(3) 0.003(3) -0.005(3) N31 0.037(3) 0.035(2) 0.038(2) 0.004(2) 0.007(2) -0.009(2) O32 0.050(3) 0.059(3) 0.076(3) -0.026(3) 0.025(3) -0.027(2) C33 0.033(4) 0.106(7) 0.127(8) -0.046(6) 0.019(5) -0.020(4) O34 0.041(2) 0.0331(19) 0.035(2) 0.0021(16) 0.0150(17) -0.0024(17) C35 0.032(3) 0.042(3) 0.028(2) 0.006(2) 0.001(2) -0.005(2) C36 0.035(3) 0.060(4) 0.031(3) 0.013(3) 0.005(2) 0.005(3) C37 0.036(3) 0.067(4) 0.045(3) 0.030(3) 0.015(3) 0.002(3) C38 0.046(4) 0.053(4) 0.052(4) 0.028(3) 0.009(3) -0.011(3) C39 0.048(4) 0.036(3) 0.044(3) 0.011(3) 0.014(3) -0.009(3) C40 0.033(3) 0.038(3) 0.029(3) 0.006(2) 0.006(2) -0.007(2) C41 0.040(3) 0.026(2) 0.029(2) 0.000(2) 0.008(2) -0.010(2) N42 0.029(2) 0.029(2) 0.027(2) 0.0008(17) 0.0028(17) -0.0095(17) O43 0.0306(19) 0.0300(18) 0.0293(18) -0.0017(15) 0.0099(15) -0.0073(15) C44 0.053(4) 0.028(3) 0.050(4) 0.007(3) 0.019(3) -0.006(3) O45 0.043(2) 0.0307(18) 0.0273(18) 0.0012(15) 0.0098(16) -0.0043(16) C46 0.039(3) 0.040(3) 0.028(2) 0.007(2) 0.014(2) -0.003(2) C47 0.061(4) 0.053(4) 0.035(3) 0.010(3) 0.017(3) 0.010(3) C48 0.073(5) 0.081(5) 0.025(3) 0.008(3) 0.013(3) 0.018(4) C49 0.080(5) 0.077(5) 0.015(2) -0.004(3) 0.005(3) -0.004(4) C50 0.067(4) 0.054(4) 0.023(3) -0.005(3) 0.009(3) -0.008(3) C51 0.050(3) 0.044(3) 0.020(2) 0.002(2) 0.010(2) -0.004(3) C52 0.049(3) 0.024(2) 0.026(2) -0.001(2) 0.013(2) -0.009(2) N53 0.034(2) 0.027(2) 0.025(2) 0.0024(17) 0.0074(17) -0.0073(18) O54 0.035(2) 0.0256(17) 0.0250(17) 0.0016(14) 0.0036(15) -0.0048(15) C55 0.093(6) 0.039(3) 0.041(3) -0.009(3) 0.017(4) 0.010(4) O56 0.038(2) 0.043(2) 0.0237(17) -0.0099(16) 0.0017(16) -0.0033(17) C57 0.033(3) 0.045(3) 0.034(3) 0.001(2) 0.011(2) -0.004(2) C58 0.049(4) 0.043(3) 0.041(3) -0.005(3) 0.006(3) 0.001(3) C59 0.052(4) 0.040(3) 0.061(4) -0.008(3) 0.012(3) 0.001(3) C60 0.044(4) 0.043(3) 0.061(4) 0.002(3) 0.001(3) 0.003(3) C61 0.029(3) 0.065(4) 0.042(3) -0.001(3) -0.002(3) -0.009(3) C62 0.030(3) 0.046(3) 0.028(3) -0.005(2) 0.002(2) -0.010(2) C63 0.034(3) 0.044(3) 0.027(2) -0.003(2) 0.004(2) -0.012(2) N64 0.040(3) 0.038(2) 0.023(2) -0.0021(18) 0.0096(18) -0.010(2) O65 0.046(2) 0.035(2) 0.032(2) -0.0035(16) -0.0035(17) -0.0110(18) C66 0.046(4) 0.049(4) 0.040(3) -0.009(3) -0.007(3) -0.003(3) O67 0.044(2) 0.034(2) 0.036(2) -0.0067(17) 0.0087(17) -0.0189(17) C68 0.053(4) 0.029(3) 0.031(3) 0.005(2) 0.006(3) -0.015(3) C69 0.051(4) 0.041(3) 0.043(3) 0.002(3) -0.001(3) -0.017(3) C70 0.058(4) 0.050(4) 0.051(4) 0.005(3) -0.015(3) -0.021(3) C71 0.090(6) 0.043(4) 0.037(3) -0.006(3) -0.010(4) -0.030(4) C72 0.080(5) 0.040(3) 0.037(3) -0.009(3) 0.003(3) -0.018(3) C73 0.063(4) 0.025(3) 0.030(3) 0.000(2) 0.002(3) -0.015(3) C74 0.049(3) 0.037(3) 0.029(3) -0.004(2) 0.006(2) -0.005(3) N75 0.044(3) 0.037(2) 0.023(2) -0.0049(19) 0.0014(19) -0.010(2) O76 0.051(3) 0.046(2) 0.041(2) -0.018(2) -0.006(2) 0.004(2) C77 0.084(6) 0.054(4) 0.061(5) -0.025(4) -0.006(4) 0.007(4) O78 0.038(2) 0.037(2) 0.0250(17) 0.0013(16) 0.0007(15) -0.0103(17) C79 0.045(3) 0.026(2) 0.030(3) 0.004(2) 0.007(2) -0.005(2) C80 0.055(4) 0.039(3) 0.027(3) -0.004(2) -0.002(3) -0.008(3) C81 0.070(5) 0.040(3) 0.027(3) -0.008(2) 0.011(3) -0.003(3) C82 0.061(4) 0.049(4) 0.035(3) -0.005(3) 0.021(3) 0.003(3) C83 0.051(4) 0.040(3) 0.034(3) -0.004(3) 0.008(3) -0.006(3) C84 0.046(3) 0.031(3) 0.021(2) 0.000(2) 0.005(2) -0.011(2) C85 0.030(3) 0.030(2) 0.029(2) -0.001(2) 0.007(2) -0.013(2) N86 0.039(2) 0.027(2) 0.0206(19) -0.0045(17) 0.0024(17) -0.0073(18) O87 0.0343(19) 0.0278(17) 0.0208(16) -0.0041(14) 0.0070(14) -0.0103(15) C88 0.044(3) 0.045(3) 0.034(3) -0.009(2) 0.010(2) -0.022(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.056418(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 . O1 . 1.931(4) yes Fe1 . N9 . 2.149(5) yes Fe1 . O12 . 1.910(3) yes Fe1 . N20 . 2.107(4) yes Fe1 . O54 . 2.066(3) yes Fe1 . O87 . 2.034(4) yes O1 . C2 . 1.349(6) yes Fe2 . O43 . 2.035(3) yes Fe2 . O45 . 1.922(3) yes Fe2 . N53 . 2.110(4) yes Fe2 . O56 . 1.925(4) yes Fe2 . N64 . 2.153(4) yes Fe2 . O87 . 2.054(3) yes C2 . C3 . 1.397(8) yes C2 . C7 . 1.405(8) yes Fe3 . O21 . 2.041(4) yes Fe3 . O43 . 2.051(3) yes Fe3 . O67 . 1.914(4) yes Fe3 . N75 . 2.151(5) yes Fe3 . O78 . 1.908(3) yes Fe3 . N86 . 2.116(4) yes C3 . C4 . 1.368(8) yes C3 . H31 . 0.932 no Fe4 . O21 . 2.044(3) yes Fe4 . O23 . 1.927(4) yes Fe4 . N31 . 2.161(5) yes Fe4 . O34 . 1.905(4) yes Fe4 . N42 . 2.120(4) yes Fe4 . O54 . 2.047(3) yes C4 . C5 . 1.381(10) yes C4 . H41 . 0.929 no C5 . C6 . 1.354(9) yes C5 . H51 . 0.930 no C6 . C7 . 1.399(7) yes C6 . H61 . 0.921 no C7 . C8 . 1.477(8) yes C8 . N9 . 1.290(6) yes C8 . C11 . 1.513(8) yes N9 . O10 . 1.387(6) yes O10 . H101 . 0.850 no C11 . H111 . 0.954 no C11 . H112 . 0.964 no C11 . H113 . 1.001 no O12 . C13 . 1.329(7) yes C13 . C14 . 1.400(7) yes C13 . C18 . 1.427(8) yes C14 . C15 . 1.364(9) yes C14 . H141 . 0.927 no C15 . C16 . 1.378(10) yes C15 . H151 . 0.929 no C16 . C17 . 1.362(8) yes C16 . H161 . 0.924 no C17 . C18 . 1.407(8) yes C17 . H171 . 0.926 no C18 . C19 . 1.472(7) yes C19 . N20 . 1.284(6) yes C19 . C22 . 1.500(7) yes N20 . O21 . 1.414(5) yes C22 . H221 . 0.959 no C22 . H222 . 0.948 no C22 . H223 . 0.972 no O23 . C24 . 1.355(7) yes C24 . C25 . 1.386(9) yes C24 . C29 . 1.409(8) yes C25 . C26 . 1.389(9) yes C25 . H251 . 0.925 no C26 . C27 . 1.390(10) yes C26 . H261 . 0.937 no C27 . C28 . 1.364(10) yes C27 . H271 . 0.936 no C28 . C29 . 1.401(8) yes C28 . H281 . 0.927 no C29 . C30 . 1.479(9) yes C30 . N31 . 1.299(8) yes C30 . C33 . 1.518(9) yes N31 . O32 . 1.389(6) yes O32 . H321 . 0.850 no C33 . H331 . 0.957 no C33 . H332 . 0.965 no C33 . H333 . 0.941 no O34 . C35 . 1.338(6) yes C35 . C36 . 1.400(8) yes C35 . C40 . 1.409(8) yes C36 . C37 . 1.374(8) yes C36 . H361 . 0.925 no C37 . C38 . 1.373(9) yes C37 . H371 . 0.915 no C38 . C39 . 1.366(8) yes C38 . H381 . 0.923 no C39 . C40 . 1.402(7) yes C39 . H391 . 0.920 no C40 . C41 . 1.477(7) yes C41 . N42 . 1.295(6) yes C41 . C44 . 1.480(7) yes N42 . O43 . 1.408(5) yes C44 . H441 . 0.961 no C44 . H442 . 0.940 no C44 . H443 . 0.961 no O45 . C46 . 1.325(6) yes C46 . C47 . 1.395(8) yes C46 . C51 . 1.409(8) yes C47 . C48 . 1.380(9) yes C47 . H471 . 0.936 no C48 . C49 . 1.372(10) yes C48 . H481 . 0.937 no C49 . C50 . 1.367(9) yes C49 . H491 . 0.921 no C50 . C51 . 1.406(7) yes C50 . H501 . 0.934 no C51 . C52 . 1.468(8) yes C52 . N53 . 1.288(6) yes C52 . C55 . 1.492(8) yes N53 . O54 . 1.407(5) yes C55 . H551 . 0.956 no C55 . H552 . 0.964 no C55 . H553 . 0.974 no O56 . C57 . 1.346(7) yes C57 . C58 . 1.392(8) yes C57 . C62 . 1.418(7) yes C58 . C59 . 1.354(9) yes C58 . H581 . 0.917 no C59 . C60 . 1.376(9) yes C59 . H591 . 0.918 no C60 . C61 . 1.358(9) yes C60 . H601 . 0.924 no C61 . C62 . 1.417(8) yes C61 . H611 . 0.930 no C62 . C63 . 1.481(8) yes C63 . N64 . 1.299(7) yes C63 . C66 . 1.513(7) yes N64 . O65 . 1.400(6) yes O65 . H651 . 0.850 no C66 . H661 . 0.966 no C66 . H662 . 0.963 no C66 . H663 . 0.978 no O67 . C68 . 1.358(6) yes C68 . C69 . 1.383(8) yes C68 . C73 . 1.408(9) yes C69 . C70 . 1.377(9) yes C69 . H691 . 0.926 no C70 . C71 . 1.371(10) yes C70 . H701 . 0.926 no C71 . C72 . 1.367(10) yes C71 . H711 . 0.936 no C72 . C73 . 1.411(8) yes C72 . H721 . 0.930 no C73 . C74 . 1.475(9) yes C74 . N75 . 1.295(7) yes C74 . C77 . 1.519(9) yes N75 . O76 . 1.387(6) yes O76 . H761 . 0.850 no C77 . H771 . 0.967 no C77 . H772 . 0.949 no C77 . H773 . 0.957 no O78 . C79 . 1.334(6) yes C79 . C80 . 1.411(7) yes C79 . C84 . 1.414(8) yes C80 . C81 . 1.380(8) yes C80 . H801 . 0.933 no C81 . C82 . 1.377(9) yes C81 . H811 . 0.928 no C82 . C83 . 1.389(8) yes C82 . H821 . 0.938 no C83 . C84 . 1.404(8) yes C83 . H831 . 0.930 no C84 . C85 . 1.478(7) yes C85 . N86 . 1.296(6) yes C85 . C88 . 1.497(7) yes N86 . O87 . 1.406(5) yes C88 . H881 . 0.950 no C88 . H882 . 0.944 no C88 . H883 . 0.958 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 . Fe1 . N9 . 82.78(16) yes O1 . Fe1 . O12 . 98.79(15) yes N9 . Fe1 . O12 . 89.31(16) yes O1 . Fe1 . N20 . 178.93(17) yes N9 . Fe1 . N20 . 96.17(17) yes O12 . Fe1 . N20 . 81.41(15) yes O1 . Fe1 . O54 . 96.61(14) yes N9 . Fe1 . O54 . 87.76(15) yes O12 . Fe1 . O54 . 163.84(15) yes N20 . Fe1 . O54 . 83.11(14) yes O1 . Fe1 . O87 . 87.75(14) yes N9 . Fe1 . O87 . 167.61(15) yes O12 . Fe1 . O87 . 100.05(15) yes N20 . Fe1 . O87 . 93.26(15) yes O54 . Fe1 . O87 . 85.41(13) yes Fe1 . O1 . C2 . 116.9(3) yes O43 . Fe2 . O45 . 95.43(15) yes O43 . Fe2 . N53 . 94.77(15) yes O45 . Fe2 . N53 . 82.66(15) yes O43 . Fe2 . O56 . 91.39(15) yes O45 . Fe2 . O56 . 99.86(16) yes N53 . Fe2 . O56 . 173.10(16) yes O43 . Fe2 . N64 . 172.67(15) yes O45 . Fe2 . N64 . 89.77(16) yes N53 . Fe2 . N64 . 91.00(17) yes O56 . Fe2 . N64 . 82.61(16) yes O43 . Fe2 . O87 . 85.11(13) yes O45 . Fe2 . O87 . 166.12(15) yes N53 . Fe2 . O87 . 83.47(14) yes O56 . Fe2 . O87 . 93.99(15) yes N64 . Fe2 . O87 . 91.08(15) yes O1 . C2 . C3 . 118.8(5) yes O1 . C2 . C7 . 122.5(5) yes C3 . C2 . C7 . 118.7(5) yes O21 . Fe3 . O43 . 84.82(14) yes O21 . Fe3 . O67 . 87.29(15) yes O43 . Fe3 . O67 . 96.19(15) yes O21 . Fe3 . N75 . 166.20(15) yes O43 . Fe3 . N75 . 85.86(15) yes O67 . Fe3 . N75 . 83.63(17) yes O21 . Fe3 . O78 . 101.59(15) yes O43 . Fe3 . O78 . 163.57(15) yes O67 . Fe3 . O78 . 99.19(16) yes N75 . Fe3 . O78 . 90.13(16) yes O21 . Fe3 . N86 . 93.30(15) yes O43 . Fe3 . N86 . 81.72(14) yes O67 . Fe3 . N86 . 177.77(17) yes N75 . Fe3 . N86 . 95.40(17) yes O78 . Fe3 . N86 . 82.80(15) yes C2 . C3 . C4 . 120.9(6) yes C2 . C3 . H31 . 119.4 no C4 . C3 . H31 . 119.7 no O21 . Fe4 . O23 . 97.89(15) yes O21 . Fe4 . N31 . 87.64(16) yes O23 . Fe4 . N31 . 82.36(17) yes O21 . Fe4 . O34 . 164.00(15) yes O23 . Fe4 . O34 . 97.25(16) yes N31 . Fe4 . O34 . 89.28(17) yes O21 . Fe4 . N42 . 82.23(15) yes O23 . Fe4 . N42 . 178.92(16) yes N31 . Fe4 . N42 . 96.57(17) yes O34 . Fe4 . N42 . 82.53(16) yes O21 . Fe4 . O54 . 86.78(13) yes O23 . Fe4 . O54 . 86.60(15) yes N31 . Fe4 . O54 . 166.83(16) yes O34 . Fe4 . O54 . 99.26(15) yes N42 . Fe4 . O54 . 94.47(15) yes C3 . C4 . C5 . 120.1(6) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 119.7 no C4 . C5 . C6 . 120.1(6) yes C4 . C5 . H51 . 118.8 no C6 . C5 . H51 . 121.1 no C5 . C6 . C7 . 121.4(6) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 118.6 no C2 . C7 . C6 . 118.6(5) yes C2 . C7 . C8 . 122.1(5) yes C6 . C7 . C8 . 119.1(6) yes C7 . C8 . N9 . 119.4(5) yes C7 . C8 . C11 . 120.7(5) yes N9 . C8 . C11 . 119.9(6) yes Fe1 . N9 . C8 . 123.0(4) yes Fe1 . N9 . O10 . 123.6(3) yes C8 . N9 . O10 . 113.0(5) yes N9 . O10 . H101 . 115.9 no C8 . C11 . H111 . 110.5 no C8 . C11 . H112 . 109.8 no H111 . C11 . H112 . 108.4 no C8 . C11 . H113 . 111.4 no H111 . C11 . H113 . 108.0 no H112 . C11 . H113 . 108.6 no Fe1 . O12 . C13 . 123.1(3) yes O12 . C13 . C14 . 118.6(5) yes O12 . C13 . C18 . 123.2(5) yes C14 . C13 . C18 . 118.3(5) yes C13 . C14 . C15 . 121.0(6) yes C13 . C14 . H141 . 118.8 no C15 . C14 . H141 . 120.2 no C14 . C15 . C16 . 120.8(6) yes C14 . C15 . H151 . 119.7 no C16 . C15 . H151 . 119.5 no C15 . C16 . C17 . 120.4(6) yes C15 . C16 . H161 . 120.4 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 120.9(6) yes C16 . C17 . H171 . 119.2 no C18 . C17 . H171 . 119.9 no C13 . C18 . C17 . 118.6(5) yes C13 . C18 . C19 . 120.9(5) yes C17 . C18 . C19 . 120.5(5) yes C18 . C19 . N20 . 117.9(5) yes C18 . C19 . C22 . 121.4(5) yes N20 . C19 . C22 . 120.7(5) yes Fe1 . N20 . C19 . 129.4(3) yes Fe1 . N20 . O21 . 116.0(3) yes C19 . N20 . O21 . 114.6(4) yes N20 . O21 . Fe4 . 108.7(3) yes N20 . O21 . Fe3 . 113.6(3) yes Fe4 . O21 . Fe3 . 121.79(17) yes C19 . C22 . H221 . 110.0 no C19 . C22 . H222 . 111.4 no H221 . C22 . H222 . 109.4 no C19 . C22 . H223 . 109.8 no H221 . C22 . H223 . 108.0 no H222 . C22 . H223 . 108.3 no Fe4 . O23 . C24 . 119.7(3) yes O23 . C24 . C25 . 117.9(5) yes O23 . C24 . C29 . 121.6(5) yes C25 . C24 . C29 . 120.5(6) yes C24 . C25 . C26 . 120.3(7) yes C24 . C25 . H251 . 119.0 no C26 . C25 . H251 . 120.6 no C25 . C26 . C27 . 119.7(7) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 120.5 no C26 . C27 . C28 . 119.8(7) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 120.9 no C27 . C28 . C29 . 122.2(7) yes C27 . C28 . H281 . 119.3 no C29 . C28 . H281 . 118.5 no C24 . C29 . C28 . 117.4(6) yes C24 . C29 . C30 . 123.6(5) yes C28 . C29 . C30 . 119.0(6) yes C29 . C30 . N31 . 119.3(5) yes C29 . C30 . C33 . 119.8(6) yes N31 . C30 . C33 . 120.9(6) yes Fe4 . N31 . C30 . 124.5(4) yes Fe4 . N31 . O32 . 122.1(4) yes C30 . N31 . O32 . 112.6(5) yes N31 . O32 . H321 . 116.2 no C30 . C33 . H331 . 110.7 no C30 . C33 . H332 . 108.5 no H331 . C33 . H332 . 109.7 no C30 . C33 . H333 . 109.1 no H331 . C33 . H333 . 110.1 no H332 . C33 . H333 . 108.7 no Fe4 . O34 . C35 . 124.1(3) yes O34 . C35 . C36 . 118.1(5) yes O34 . C35 . C40 . 123.0(5) yes C36 . C35 . C40 . 118.9(5) yes C35 . C36 . C37 . 120.4(6) yes C35 . C36 . H361 . 118.7 no C37 . C36 . H361 . 120.9 no C36 . C37 . C38 . 121.1(6) yes C36 . C37 . H371 . 118.7 no C38 . C37 . H371 . 120.2 no C37 . C38 . C39 . 119.5(6) yes C37 . C38 . H381 . 121.2 no C39 . C38 . H381 . 119.3 no C38 . C39 . C40 . 121.6(6) yes C38 . C39 . H391 . 119.8 no C40 . C39 . H391 . 118.6 no C35 . C40 . C39 . 118.5(5) yes C35 . C40 . C41 . 122.6(5) yes C39 . C40 . C41 . 118.9(5) yes C40 . C41 . N42 . 117.0(5) yes C40 . C41 . C44 . 121.9(5) yes N42 . C41 . C44 . 121.0(5) yes Fe4 . N42 . C41 . 130.0(4) yes Fe4 . N42 . O43 . 115.4(3) yes C41 . N42 . O43 . 114.6(4) yes N42 . O43 . Fe3 . 110.1(3) yes N42 . O43 . Fe2 . 111.7(3) yes Fe3 . O43 . Fe2 . 121.76(16) yes C41 . C44 . H441 . 111.4 no C41 . C44 . H442 . 111.5 no H441 . C44 . H442 . 110.3 no C41 . C44 . H443 . 108.6 no H441 . C44 . H443 . 107.1 no H442 . C44 . H443 . 107.7 no Fe2 . O45 . C46 . 123.7(3) yes O45 . C46 . C47 . 118.6(5) yes O45 . C46 . C51 . 123.3(5) yes C47 . C46 . C51 . 118.1(5) yes C46 . C47 . C48 . 121.1(6) yes C46 . C47 . H471 . 119.6 no C48 . C47 . H471 . 119.3 no C47 . C48 . C49 . 120.9(6) yes C47 . C48 . H481 . 118.9 no C49 . C48 . H481 . 120.2 no C48 . C49 . C50 . 119.2(6) yes C48 . C49 . H491 . 120.4 no C50 . C49 . H491 . 120.4 no C49 . C50 . C51 . 121.6(6) yes C49 . C50 . H501 . 118.8 no C51 . C50 . H501 . 119.5 no C46 . C51 . C50 . 118.9(5) yes C46 . C51 . C52 . 120.9(5) yes C50 . C51 . C52 . 120.1(5) yes C51 . C52 . N53 . 119.1(5) yes C51 . C52 . C55 . 122.2(5) yes N53 . C52 . C55 . 118.7(5) yes Fe2 . N53 . C52 . 128.3(4) yes Fe2 . N53 . O54 . 115.5(3) yes C52 . N53 . O54 . 115.9(4) yes N53 . O54 . Fe1 . 111.1(3) yes N53 . O54 . Fe4 . 111.6(2) yes Fe1 . O54 . Fe4 . 119.26(16) yes C52 . C55 . H551 . 111.8 no C52 . C55 . H552 . 111.8 no H551 . C55 . H552 . 108.9 no C52 . C55 . H553 . 109.3 no H551 . C55 . H553 . 107.0 no H552 . C55 . H553 . 107.8 no Fe2 . O56 . C57 . 121.4(3) yes O56 . C57 . C58 . 119.4(5) yes O56 . C57 . C62 . 121.9(5) yes C58 . C57 . C62 . 118.7(6) yes C57 . C58 . C59 . 121.6(6) yes C57 . C58 . H581 . 118.5 no C59 . C58 . H581 . 119.8 no C58 . C59 . C60 . 121.2(6) yes C58 . C59 . H591 . 119.6 no C60 . C59 . H591 . 119.1 no C59 . C60 . C61 . 118.5(6) yes C59 . C60 . H601 . 120.8 no C61 . C60 . H601 . 120.8 no C60 . C61 . C62 . 123.0(6) yes C60 . C61 . H611 . 118.9 no C62 . C61 . H611 . 118.2 no C57 . C62 . C61 . 116.7(6) yes C57 . C62 . C63 . 124.2(5) yes C61 . C62 . C63 . 118.8(5) yes C62 . C63 . N64 . 119.1(5) yes C62 . C63 . C66 . 118.8(5) yes N64 . C63 . C66 . 122.1(5) yes Fe2 . N64 . C63 . 119.4(4) yes Fe2 . N64 . O65 . 122.2(3) yes C63 . N64 . O65 . 113.3(4) yes N64 . O65 . H651 . 112.1 no C63 . C66 . H661 . 111.0 no C63 . C66 . H662 . 108.6 no H661 . C66 . H662 . 111.2 no C63 . C66 . H663 . 107.6 no H661 . C66 . H663 . 110.3 no H662 . C66 . H663 . 107.9 no Fe3 . O67 . C68 . 119.2(3) yes O67 . C68 . C69 . 119.0(6) yes O67 . C68 . C73 . 121.1(5) yes C69 . C68 . C73 . 119.9(5) yes C68 . C69 . C70 . 121.0(7) yes C68 . C69 . H691 . 119.6 no C70 . C69 . H691 . 119.4 no C69 . C70 . C71 . 120.3(7) yes C69 . C70 . H701 . 119.6 no C71 . C70 . H701 . 120.1 no C70 . C71 . C72 . 119.6(6) yes C70 . C71 . H711 . 120.0 no C72 . C71 . H711 . 120.4 no C71 . C72 . C73 . 122.2(7) yes C71 . C72 . H721 . 119.1 no C73 . C72 . H721 . 118.7 no C72 . C73 . C68 . 117.0(6) yes C72 . C73 . C74 . 119.3(6) yes C68 . C73 . C74 . 123.7(5) yes C73 . C74 . N75 . 118.8(5) yes C73 . C74 . C77 . 120.3(5) yes N75 . C74 . C77 . 120.9(6) yes Fe3 . N75 . C74 . 124.5(4) yes Fe3 . N75 . O76 . 123.6(3) yes C74 . N75 . O76 . 112.0(5) yes N75 . O76 . H761 . 117.6 no C74 . C77 . H771 . 107.2 no C74 . C77 . H772 . 109.0 no H771 . C77 . H772 . 110.3 no C74 . C77 . H773 . 108.9 no H771 . C77 . H773 . 111.5 no H772 . C77 . H773 . 109.7 no Fe3 . O78 . C79 . 123.3(3) yes O78 . C79 . C80 . 118.6(5) yes O78 . C79 . C84 . 123.9(5) yes C80 . C79 . C84 . 117.5(5) yes C79 . C80 . C81 . 121.3(6) yes C79 . C80 . H801 . 118.7 no C81 . C80 . H801 . 120.0 no C80 . C81 . C82 . 120.9(5) yes C80 . C81 . H811 . 118.8 no C82 . C81 . H811 . 120.3 no C81 . C82 . C83 . 119.4(6) yes C81 . C82 . H821 . 119.2 no C83 . C82 . H821 . 121.5 no C82 . C83 . C84 . 120.8(6) yes C82 . C83 . H831 . 119.1 no C84 . C83 . H831 . 120.1 no C79 . C84 . C83 . 120.0(5) yes C79 . C84 . C85 . 120.7(5) yes C83 . C84 . C85 . 119.2(5) yes C84 . C85 . N86 . 118.3(4) yes C84 . C85 . C88 . 121.1(4) yes N86 . C85 . C88 . 120.6(5) yes Fe3 . N86 . C85 . 129.2(3) yes Fe3 . N86 . O87 . 115.9(3) yes C85 . N86 . O87 . 114.7(4) yes N86 . O87 . Fe2 . 109.1(3) yes N86 . O87 . Fe1 . 114.3(3) yes Fe2 . O87 . Fe1 . 121.08(16) yes C85 . C88 . H881 . 109.3 no C85 . C88 . H882 . 110.7 no H881 . C88 . H882 . 110.5 no C85 . C88 . H883 . 107.3 no H881 . C88 . H883 . 108.7 no H882 . C88 . H883 . 110.3 no # Attachment 'Complex 4 cif.cif' data_EB7004 _database_code_depnum_ccdc_archive 'CCDC 667681' _audit_creation_date 07-01-22 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'EB7004 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.9693(6) _cell_length_b 14.2060(4) _cell_length_c 22.7462(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6452.7(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 '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 4 # Given Formula = C50 H82 Fe6 N6 O24 S2 # Dc = 1.60 Fooo = 3208.00 Mu = 14.58 M = 775.22 # Found Formula = C50 H80 Fe6 N6 O24 S2 # Dc = 1.59 FOOO = 3208.00 Mu = 14.58 M = 774.21 _chemical_formula_sum 'C50 H80 Fe6 N6 O24 S2' _chemical_formula_moiety 'C38 H48 Fe6 N4 O24 S2, 2(C6 H16 N)' _chemical_compound_source ? _chemical_formula_weight 1548.43 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description wedge _exptl_crystal_colour black _exptl_crystal_size_min 0.31 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_max 0.47 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.458 # Sheldrick geometric approximatio 0.63 0.64 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 0.64 _diffrn_measurement_device_type 'Bruker SMART' _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 '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 149468 _reflns_number_total 9291 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 9291 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9390 _diffrn_reflns_theta_min 1.974 _diffrn_reflns_theta_max 29.976 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.377 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 1.54 _oxford_diffrn_Wilson_scale 28.68 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.89 _refine_diff_density_max 1.71 _refine_ls_number_reflns 9264 _refine_ls_number_restraints 0 _refine_ls_number_parameters 397 #_refine_ls_R_factor_ref 0.0485 _refine_ls_wR_factor_ref 0.0732 _refine_ls_goodness_of_fit_ref 1.0215 #_reflns_number_all 9264 _refine_ls_R_factor_all 0.0485 _refine_ls_wR_factor_all 0.0732 # 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 6354 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_gt 0.0579 _refine_ls_shift/su_max 0.002422 # 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, 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: 7.51 9.08 2.21 ; # 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_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: ; 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. The H atoms in the main molecule of the complex were 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 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. Hydrogen atoms attached in the triethylamine solvent were attached geometrically with C--H distances of 0.94\%A. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.88 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. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.73 Ratio Part of a MeOH ligand. 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C43 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N38 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C41 The triethylamine ligand is clearly dynamic within the crystal. The disorder cannot be modelled using partial occupancy of atomic sites, but is too localised to use the special shapes modelling function. This accounts for the differences in Ueq in the solvent. 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.94 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C39 - C40 ... 1.40 Ang. 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C43 - C44 ... 1.37 Ang. 412_ALERT_2_C Short Intra XH3 .. XHn H392 .. H422 .. 1.89 Ang. This results from disorder in the solvent. 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 1 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 92 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data is complete to Acta standards. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 3384 3383 1 23.01 0.550 1.000 4493 4492 1 25.24 0.600 1.000 5832 5831 1 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 7421 7420 1 29.84 0.700 0.995 9274 9223 51 29.98 0.703 0.990 9384 9291 93 ; _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. 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 0.545374(16) 1.04912(2) 0.455953(14) 0.0165 1.0000 Uani . . . . . . Fe2 Fe 0.521895(17) 0.83488(2) 0.427305(14) 0.0189 1.0000 Uani . . . . . . Fe3 Fe 0.602499(17) 0.84291(2) 0.541362(14) 0.0182 1.0000 Uani . . . . . . O4 O 0.66092(9) 0.76609(13) 0.58516(8) 0.0276 1.0000 Uani . . . . . . C5 C 0.66152(13) 0.74034(17) 0.64102(11) 0.0237 1.0000 Uani . . . . . . C6 C 0.72286(14) 0.71109(18) 0.66484(12) 0.0284 1.0000 Uani . . . . . . C7 C 0.72731(15) 0.6802(2) 0.72229(12) 0.0332 1.0000 Uani . . . . . . C8 C 0.67110(16) 0.6782(2) 0.75743(12) 0.0343 1.0000 Uani . . . . . . C9 C 0.61036(15) 0.70727(18) 0.73539(11) 0.0292 1.0000 Uani . . . . . . C10 C 0.60326(13) 0.73860(16) 0.67661(10) 0.0229 1.0000 Uani . . . . . . C11 C 0.53635(13) 0.76570(16) 0.65538(11) 0.0230 1.0000 Uani . . . . . . N12 N 0.52992(11) 0.81515(14) 0.60733(9) 0.0228 1.0000 Uani . . . . . . O13 O 0.46575(8) 0.83916(12) 0.59267(7) 0.0235 1.0000 Uani . . . . . . C14 C 0.47474(15) 0.7374(2) 0.68836(13) 0.0347 1.0000 Uani . . . . . . O15 O 0.50200(9) 0.74994(13) 0.36528(8) 0.0284 1.0000 Uani . . . . . . C16 C 0.46118(13) 0.67678(18) 0.36539(11) 0.0247 1.0000 Uani . . . . . . C17 C 0.47282(15) 0.60496(19) 0.32354(12) 0.0324 1.0000 Uani . . . . . . C18 C 0.43429(17) 0.5247(2) 0.32184(15) 0.0414 1.0000 Uani . . . . . . C19 C 0.38202(17) 0.5138(2) 0.36105(16) 0.0438 1.0000 Uani . . . . . . C20 C 0.36943(16) 0.5827(2) 0.40172(14) 0.0372 1.0000 Uani . . . . . . C21 C 0.40680(13) 0.66585(18) 0.40493(11) 0.0264 1.0000 Uani . . . . . . C22 C 0.38613(13) 0.74025(18) 0.44613(12) 0.0268 1.0000 Uani . . . . . . N23 N 0.42346(10) 0.81459(14) 0.45263(9) 0.0226 1.0000 Uani . . . . . . O24 O 0.39652(9) 0.88675(12) 0.48517(8) 0.0246 1.0000 Uani . . . . . . C25 C 0.32237(16) 0.7315(2) 0.48049(17) 0.0495 1.0000 Uani . . . . . . O26 O 0.50431(8) 0.96157(12) 0.39466(7) 0.0208 1.0000 Uani . . . . . . C27 C 0.50520(15) 0.9779(2) 0.33310(11) 0.0318 1.0000 Uani . . . . . . O28 O 0.63184(9) 0.96550(13) 0.58752(9) 0.0315 1.0000 Uani . . . . . . C29 C 0.69394(19) 0.9847(3) 0.6130(2) 0.0623 1.0000 Uani . . . . . . O30 O 0.56276(9) 0.74601(12) 0.48813(8) 0.0239 1.0000 Uani . . . . . . C31 C 0.53507(15) 0.65997(18) 0.50822(13) 0.0323 1.0000 Uani . . . . . . O32 O 0.53820(8) 0.92352(11) 0.49965(7) 0.0170 1.0000 Uani . . . . . . O33 O 0.64012(8) 1.00862(11) 0.42428(7) 0.0201 1.0000 Uani . . . . . . S34 S 0.66725(3) 0.91104(4) 0.42283(3) 0.0179 1.0000 Uani . . . . . . O35 O 0.73023(8) 0.91053(12) 0.39056(8) 0.0235 1.0000 Uani . . . . . . O36 O 0.61808(8) 0.84797(12) 0.39395(7) 0.0203 1.0000 Uani . . . . . . O37 O 0.67823(8) 0.87706(12) 0.48380(7) 0.0221 1.0000 Uani . . . . . . N38 N 0.77877(15) 1.0920(2) 0.36753(14) 0.0501 1.0000 Uani . . . . . . C39 C 0.8354(3) 1.0784(4) 0.3271(3) 0.1144 1.0000 Uani . . . . . . C40 C 0.8664(3) 0.9901(4) 0.3244(4) 0.1588 1.0000 Uani . . . . . . C41 C 0.7227(2) 1.1484(3) 0.3384(2) 0.0621 1.0000 Uani . . . . . . C42 C 0.6946(3) 1.1044(4) 0.2852(3) 0.1145 1.0000 Uani . . . . . . C43 C 0.7958(4) 1.1379(4) 0.4252(3) 0.1146 1.0000 Uani . . . . . . C44 C 0.8008(3) 1.0832(3) 0.4747(2) 0.0775 1.0000 Uani . . . . . . H61 H 0.7606 0.7134 0.6410 0.0334 1.0000 Uiso R . . . . . H71 H 0.7690 0.6620 0.7372 0.0395 1.0000 Uiso R . . . . . H81 H 0.6742 0.6576 0.7954 0.0410 1.0000 Uiso R . . . . . H91 H 0.5730 0.7069 0.7599 0.0340 1.0000 Uiso R . . . . . H141 H 0.4392 0.7268 0.6621 0.0518 1.0000 Uiso R . . . . . H142 H 0.4613 0.7865 0.7137 0.0527 1.0000 Uiso R . . . . . H143 H 0.4808 0.6822 0.7106 0.0526 1.0000 Uiso R . . . . . H171 H 0.5082 0.6131 0.2966 0.0389 1.0000 Uiso R . . . . . H181 H 0.4434 0.4773 0.2937 0.0500 1.0000 Uiso R . . . . . H191 H 0.3562 0.4601 0.3600 0.0516 1.0000 Uiso R . . . . . H201 H 0.3336 0.5739 0.4287 0.0447 1.0000 Uiso R . . . . . H251 H 0.3166 0.7878 0.5037 0.0751 1.0000 Uiso R . . . . . H252 H 0.3254 0.6771 0.5058 0.0749 1.0000 Uiso R . . . . . H253 H 0.2859 0.7230 0.4545 0.0743 1.0000 Uiso R . . . . . H271 H 0.5494 0.9874 0.3179 0.0486 1.0000 Uiso R . . . . . H272 H 0.4807 1.0339 0.3234 0.0483 1.0000 Uiso R . . . . . H273 H 0.4855 0.9272 0.3123 0.0487 1.0000 Uiso R . . . . . H281 H 0.6103 0.9987 0.6043 0.0500 1.0000 Uiso R . . . . . H291 H 0.7211 1.0181 0.5861 0.0947 1.0000 Uiso R . . . . . H292 H 0.6853 1.0231 0.6465 0.0937 1.0000 Uiso R . . . . . H293 H 0.7144 0.9270 0.6249 0.0940 1.0000 Uiso R . . . . . H311 H 0.5656 0.6303 0.5359 0.0487 1.0000 Uiso R . . . . . H312 H 0.4912 0.6699 0.5269 0.0489 1.0000 Uiso R . . . . . H313 H 0.5271 0.6160 0.4748 0.0491 1.0000 Uiso R . . . . . H381 H 0.7626 1.0354 0.3755 0.0757 1.0000 Uiso R . . . . . H411 H 0.7405 1.2085 0.3285 0.0751 1.0000 Uiso R . . . . . H412 H 0.6865 1.1598 0.3658 0.0752 1.0000 Uiso R . . . . . H421 H 0.6608 1.1432 0.2674 0.1710 1.0000 Uiso R . . . . . H422 H 0.7314 1.0952 0.2584 0.1710 1.0000 Uiso R . . . . . H423 H 0.6762 1.0431 0.2938 0.1707 1.0000 Uiso R . . . . . H441 H 0.8112 1.1195 0.5080 0.0920 1.0000 Uiso R . . . . . H442 H 0.8348 1.0386 0.4685 0.0920 1.0000 Uiso R . . . . . H443 H 0.7598 1.0521 0.4807 0.0920 1.0000 Uiso R . . . . . H391 H 0.8689 1.1226 0.3380 0.1439 1.0000 Uiso R . . . . . H392 H 0.8197 1.0925 0.2887 0.1439 1.0000 Uiso R . . . . . H401 H 0.9019 0.9919 0.2967 0.1870 1.0000 Uiso R . . . . . H402 H 0.8836 0.9742 0.3620 0.1870 1.0000 Uiso R . . . . . H403 H 0.8345 0.9442 0.3127 0.1870 1.0000 Uiso R . . . . . H431 H 0.8380 1.1661 0.4200 0.1399 1.0000 Uiso R . . . . . H432 H 0.7636 1.1848 0.4324 0.1399 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 0.01744(15) 0.01571(14) 0.01648(14) -0.00088(12) 0.00110(12) 0.00102(12) Fe2 0.01934(15) 0.01969(15) 0.01774(15) -0.00293(12) 0.00116(12) -0.00473(13) Fe3 0.01948(15) 0.01882(15) 0.01630(14) 0.00061(12) 0.00022(12) 0.00308(12) O4 0.0298(9) 0.0329(10) 0.0201(8) 0.0060(7) 0.0010(7) 0.0114(8) C5 0.0321(13) 0.0180(11) 0.0209(11) 0.0014(9) -0.0021(10) 0.0039(10) C6 0.0325(13) 0.0263(12) 0.0264(12) 0.0019(10) -0.0050(11) 0.0031(11) C7 0.0379(15) 0.0317(14) 0.0300(13) 0.0045(11) -0.0122(12) 0.0020(12) C8 0.0496(17) 0.0324(14) 0.0208(12) 0.0064(10) -0.0086(12) -0.0014(13) C9 0.0418(15) 0.0247(12) 0.0209(11) 0.0029(9) 0.0010(11) -0.0044(11) C10 0.0326(12) 0.0169(10) 0.0190(10) 0.0009(8) -0.0014(10) -0.0003(9) C11 0.0291(12) 0.0190(11) 0.0210(11) 0.0006(9) 0.0026(9) 0.0012(9) N12 0.0258(10) 0.0204(9) 0.0222(9) 0.0016(8) 0.0030(8) 0.0028(8) O13 0.0211(8) 0.0236(8) 0.0259(8) 0.0051(7) 0.0037(7) 0.0034(7) C14 0.0353(14) 0.0380(15) 0.0309(14) 0.0117(12) 0.0058(12) -0.0019(12) O15 0.0298(9) 0.0272(9) 0.0281(9) -0.0098(8) 0.0043(8) -0.0079(8) C16 0.0261(12) 0.0238(11) 0.0242(11) -0.0039(9) -0.0024(9) -0.0039(10) C17 0.0375(15) 0.0287(13) 0.0309(13) -0.0099(11) -0.0012(12) -0.0007(11) C18 0.0536(19) 0.0279(14) 0.0429(17) -0.0136(13) 0.0005(15) -0.0047(13) C19 0.0500(19) 0.0267(14) 0.055(2) -0.0129(14) 0.0063(16) -0.0160(14) C20 0.0405(16) 0.0271(13) 0.0441(17) -0.0029(12) 0.0052(13) -0.0107(12) C21 0.0280(12) 0.0220(11) 0.0291(12) -0.0033(10) -0.0018(10) -0.0035(10) C22 0.0249(12) 0.0253(12) 0.0302(13) -0.0032(10) 0.0023(10) -0.0036(10) N23 0.0211(9) 0.0223(10) 0.0244(10) -0.0040(8) 0.0003(8) -0.0001(8) O24 0.0262(9) 0.0214(8) 0.0260(9) -0.0066(7) -0.0014(7) 0.0008(7) C25 0.0386(17) 0.0387(17) 0.071(2) -0.0202(17) 0.0262(17) -0.0164(14) O26 0.0212(8) 0.0253(8) 0.0160(7) -0.0031(6) -0.0002(6) -0.0014(7) C27 0.0453(16) 0.0322(14) 0.0178(11) -0.0013(10) -0.0030(11) 0.0044(12) O28 0.0297(10) 0.0300(10) 0.0349(10) -0.0125(8) -0.0110(8) 0.0066(8) C29 0.058(2) 0.0437(19) 0.085(3) 0.003(2) -0.042(2) -0.0110(18) O30 0.0285(9) 0.0153(7) 0.0279(9) -0.0011(7) 0.0045(7) -0.0012(7) C31 0.0371(15) 0.0210(12) 0.0388(15) 0.0041(11) -0.0002(12) -0.0034(11) O32 0.0192(8) 0.0151(7) 0.0169(7) -0.0009(6) 0.0007(6) 0.0009(6) O33 0.0188(8) 0.0176(7) 0.0239(8) -0.0013(6) 0.0034(6) -0.0018(6) S34 0.0160(2) 0.0180(2) 0.0199(2) -0.0012(2) 0.0022(2) -0.0014(2) O35 0.0186(8) 0.0227(8) 0.0292(9) -0.0017(7) 0.0065(7) -0.0013(7) O36 0.0200(8) 0.0197(8) 0.0214(8) -0.0032(6) 0.0028(6) -0.0031(6) O37 0.0182(8) 0.0258(8) 0.0223(8) 0.0019(7) -0.0004(7) 0.0003(7) N38 0.0517(17) 0.0299(13) 0.069(2) 0.0069(14) 0.0115(15) -0.0134(13) C39 0.061(3) 0.086(4) 0.196(7) 0.050(4) 0.073(4) 0.015(3) C40 0.088(4) 0.064(4) 0.325(12) 0.024(5) 0.104(6) -0.006(3) C41 0.068(3) 0.0391(19) 0.079(3) 0.018(2) 0.025(2) -0.0004(19) C42 0.126(5) 0.077(4) 0.140(6) 0.047(4) -0.061(5) -0.020(4) C43 0.189(7) 0.052(3) 0.103(4) -0.002(3) -0.036(5) -0.040(4) C44 0.081(3) 0.064(3) 0.087(4) -0.022(3) -0.021(3) -0.019(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16217(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 . Fe1 2_676 3.0408(6) yes Fe1 . O24 2_676 1.9925(17) yes Fe1 . O32 2_676 1.9890(16) yes Fe1 . O13 2_676 1.9472(17) yes Fe1 . Fe3 2_676 3.3281(5) yes Fe1 . Fe2 2_676 3.4017(5) yes Fe1 . O26 . 2.0403(16) yes Fe1 . O32 . 2.0473(15) yes Fe1 . O33 . 2.1047(16) yes Fe2 . Fe3 . 3.0553(5) yes Fe2 . O15 . 1.8985(18) yes Fe2 . N23 . 2.069(2) yes Fe2 . O26 . 1.9784(17) yes Fe2 . O30 . 2.0431(18) yes Fe2 . O32 . 2.0975(15) yes Fe2 . O36 . 2.0736(16) yes Fe3 . O4 . 1.8827(17) yes Fe3 . N12 . 2.123(2) yes Fe3 . O28 . 2.1162(18) yes Fe3 . O30 . 1.9977(18) yes Fe3 . O32 . 1.9648(16) yes Fe3 . O37 . 2.0583(17) yes O4 . C5 . 1.322(3) yes C5 . C6 . 1.402(3) yes C5 . C10 . 1.418(4) yes C6 . C7 . 1.381(4) yes C6 . H61 . 0.929 no C7 . C8 . 1.378(4) yes C7 . H71 . 0.936 no C8 . C9 . 1.376(4) yes C8 . H81 . 0.914 no C9 . C10 . 1.416(3) yes C9 . H91 . 0.932 no C10 . C11 . 1.472(3) yes C11 . N12 . 1.305(3) yes C11 . C14 . 1.496(4) yes N12 . O13 . 1.367(3) yes C14 . H141 . 0.938 no C14 . H142 . 0.944 no C14 . H143 . 0.942 no O15 . C16 . 1.321(3) yes C16 . C17 . 1.415(3) yes C16 . C21 . 1.419(4) yes C17 . C18 . 1.376(4) yes C17 . H171 . 0.942 no C18 . C19 . 1.382(5) yes C18 . H181 . 0.947 no C19 . C20 . 1.370(4) yes C19 . H191 . 0.921 no C20 . C21 . 1.399(4) yes C20 . H201 . 0.951 no C21 . C22 . 1.472(4) yes C22 . N23 . 1.301(3) yes C22 . C25 . 1.499(4) yes N23 . O24 . 1.374(2) yes C25 . H251 . 0.964 no C25 . H252 . 0.966 no C25 . H253 . 0.947 no O26 . C27 . 1.419(3) yes C27 . H271 . 0.958 no C27 . H272 . 0.961 no C27 . H273 . 0.948 no O28 . C29 . 1.396(4) yes O28 . H281 . 0.744 no C29 . H291 . 0.946 no C29 . H292 . 0.952 no C29 . H293 . 0.955 no O30 . C31 . 1.417(3) yes C31 . H311 . 0.971 no C31 . H312 . 0.984 no C31 . H313 . 0.997 no O33 . S34 . 1.4886(17) yes S34 . O35 . 1.4563(17) yes S34 . O36 . 1.4827(17) yes S34 . O37 . 1.4847(18) yes N38 . C39 . 1.471(5) yes N38 . C41 . 1.528(5) yes N38 . C43 . 1.505(6) yes N38 . H381 . 0.886 no C39 . C40 . 1.400(7) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . H401 . 0.950 no C40 . H402 . 0.950 no C40 . H403 . 0.950 no C41 . C42 . 1.473(7) yes C41 . H411 . 0.951 no C41 . H412 . 0.968 no C42 . H421 . 0.961 no C42 . H422 . 0.963 no C42 . H423 . 0.965 no C43 . C44 . 1.372(7) yes C43 . H431 . 0.940 no C43 . H432 . 0.940 no C44 . H441 . 0.940 no C44 . H442 . 0.940 no C44 . H443 . 0.940 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 Fe1 2_676 Fe1 . O24 2_676 96.55(5) yes Fe1 2_676 Fe1 . O32 2_676 41.85(4) yes O24 2_676 Fe1 . O32 2_676 93.33(7) yes Fe1 2_676 Fe1 . O13 2_676 132.87(5) yes O24 2_676 Fe1 . O13 2_676 94.33(8) yes O32 2_676 Fe1 . O13 2_676 91.92(7) yes Fe1 2_676 Fe1 . Fe3 2_676 70.771(13) yes O24 2_676 Fe1 . Fe3 2_676 107.08(5) yes O32 2_676 Fe1 . Fe3 2_676 32.45(4) yes O13 2_676 Fe1 . Fe3 2_676 62.20(5) yes Fe1 2_676 Fe1 . Fe2 2_676 58.170(12) yes O24 2_676 Fe1 . Fe2 2_676 58.92(5) yes O32 2_676 Fe1 . Fe2 2_676 34.68(4) yes O13 2_676 Fe1 . Fe2 2_676 90.20(5) yes Fe3 2_676 Fe1 . Fe2 2_676 53.986(10) yes Fe1 2_676 Fe1 . O26 . 86.05(5) yes O24 2_676 Fe1 . O26 . 166.42(7) yes O32 2_676 Fe1 . O26 . 97.40(7) yes O13 2_676 Fe1 . O26 . 93.60(7) yes Fe3 2_676 Fe1 . O26 . 86.38(5) yes Fe1 2_676 Fe1 . O32 . 40.40(4) yes O24 2_676 Fe1 . O32 . 96.49(7) yes O32 2_676 Fe1 . O32 . 82.25(7) yes O13 2_676 Fe1 . O32 . 167.98(7) yes Fe3 2_676 Fe1 . O32 . 109.31(5) yes Fe1 2_676 Fe1 . O33 . 129.48(5) yes O24 2_676 Fe1 . O33 . 80.30(7) yes O32 2_676 Fe1 . O33 . 168.96(7) yes O13 2_676 Fe1 . O33 . 97.52(7) yes Fe3 2_676 Fe1 . O33 . 158.41(5) yes Fe2 2_676 Fe1 . O26 . 132.07(5) yes Fe2 2_676 Fe1 . O32 . 90.89(4) yes O26 . Fe1 . O32 . 76.85(6) yes Fe2 2_676 Fe1 . O33 . 138.99(5) yes O26 . Fe1 . O33 . 87.75(7) yes O32 . Fe1 . O33 . 89.48(6) yes Fe1 2_676 Fe2 . Fe3 . 61.777(10) yes Fe1 2_676 Fe2 . O15 . 143.65(6) yes Fe3 . Fe2 . O15 . 139.91(6) yes Fe1 2_676 Fe2 . N23 . 58.32(6) yes Fe3 . Fe2 . N23 . 105.63(6) yes O15 . Fe2 . N23 . 85.39(8) yes Fe1 2_676 Fe2 . O26 . 77.42(5) yes Fe3 . Fe2 . O26 . 112.23(5) yes O15 . Fe2 . O26 . 105.19(8) yes N23 . Fe2 . O26 . 93.59(8) yes Fe1 2_676 Fe2 . O30 . 85.90(5) yes Fe3 . Fe2 . O30 . 40.32(5) yes O15 . Fe2 . O30 . 101.19(8) yes N23 . Fe2 . O30 . 96.02(8) yes O26 . Fe2 . O30 . 152.53(7) yes Fe1 2_676 Fe2 . O32 . 32.65(4) yes Fe3 . Fe2 . O32 . 39.61(4) yes O15 . Fe2 . O32 . 175.61(7) yes N23 . Fe2 . O32 . 90.73(7) yes O26 . Fe2 . O32 . 77.05(6) yes Fe1 2_676 Fe2 . O36 . 127.44(5) yes Fe3 . Fe2 . O36 . 79.59(5) yes O15 . Fe2 . O36 . 88.79(7) yes N23 . Fe2 . O36 . 174.08(7) yes O26 . Fe2 . O36 . 86.87(7) yes O30 . Fe2 . O32 . 77.16(6) yes O30 . Fe2 . O36 . 86.17(7) yes O32 . Fe2 . O36 . 95.13(6) yes Fe2 . Fe3 . Fe1 2_676 64.237(11) yes Fe2 . Fe3 . O4 . 138.95(6) yes Fe1 2_676 Fe3 . O4 . 143.83(6) yes Fe2 . Fe3 . N12 . 103.51(6) yes Fe1 2_676 Fe3 . N12 . 57.79(6) yes O4 . Fe3 . N12 . 86.64(8) yes Fe2 . Fe3 . O28 . 126.71(5) yes Fe1 2_676 Fe3 . O28 . 81.79(5) yes O4 . Fe3 . O28 . 92.46(8) yes N12 . Fe3 . O28 . 89.50(8) yes Fe2 . Fe3 . O30 . 41.44(5) yes Fe1 2_676 Fe3 . O30 . 88.64(5) yes O4 . Fe3 . O30 . 99.64(8) yes N12 . Fe3 . O30 . 91.67(8) yes O28 . Fe3 . O30 . 167.89(7) yes Fe2 . Fe3 . O32 . 42.90(4) yes Fe1 2_676 Fe3 . O32 . 32.90(5) yes O4 . Fe3 . O32 . 176.71(7) yes N12 . Fe3 . O32 . 90.20(7) yes O28 . Fe3 . O32 . 86.61(7) yes Fe2 . Fe3 . O37 . 81.70(5) yes Fe1 2_676 Fe3 . O37 . 123.71(5) yes O4 . Fe3 . O37 . 91.03(7) yes N12 . Fe3 . O37 . 174.21(8) yes O28 . Fe3 . O37 . 85.31(7) yes O30 . Fe3 . O32 . 81.33(7) yes O30 . Fe3 . O37 . 93.94(7) yes O32 . Fe3 . O37 . 92.04(7) yes Fe3 . O4 . C5 . 132.41(17) yes O4 . C5 . C6 . 117.5(2) yes O4 . C5 . C10 . 123.1(2) yes C6 . C5 . C10 . 119.4(2) yes C5 . C6 . C7 . 121.1(3) yes C5 . C6 . H61 . 118.1 no C7 . C6 . H61 . 120.8 no C6 . C7 . C8 . 120.2(3) yes C6 . C7 . H71 . 119.2 no C8 . C7 . H71 . 120.6 no C7 . C8 . C9 . 120.0(2) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 121.8(3) yes C8 . C9 . H91 . 119.1 no C10 . C9 . H91 . 119.1 no C5 . C10 . C9 . 117.5(2) yes C5 . C10 . C11 . 123.6(2) yes C9 . C10 . C11 . 118.9(2) yes C10 . C11 . N12 . 120.3(2) yes C10 . C11 . C14 . 120.8(2) yes N12 . C11 . C14 . 118.9(2) yes Fe3 . N12 . C11 . 128.65(18) yes Fe3 . N12 . O13 . 114.91(14) yes C11 . N12 . O13 . 115.5(2) yes N12 . O13 . Fe1 2_676 116.66(13) yes C11 . C14 . H141 . 110.2 no C11 . C14 . H142 . 110.0 no H141 . C14 . H142 . 107.0 no C11 . C14 . H143 . 112.8 no H141 . C14 . H143 . 107.8 no H142 . C14 . H143 . 108.8 no Fe2 . O15 . C16 . 128.88(16) yes O15 . C16 . C17 . 117.7(2) yes O15 . C16 . C21 . 124.0(2) yes C17 . C16 . C21 . 118.3(2) yes C16 . C17 . C18 . 121.7(3) yes C16 . C17 . H171 . 118.2 no C18 . C17 . H171 . 120.1 no C17 . C18 . C19 . 119.8(3) yes C17 . C18 . H181 . 120.1 no C19 . C18 . H181 . 120.2 no C18 . C19 . C20 . 119.7(3) yes C18 . C19 . H191 . 119.9 no C20 . C19 . H191 . 120.4 no C19 . C20 . C21 . 122.7(3) yes C19 . C20 . H201 . 118.6 no C21 . C20 . H201 . 118.6 no C16 . C21 . C20 . 117.9(2) yes C16 . C21 . C22 . 122.7(2) yes C20 . C21 . C22 . 119.4(2) yes C21 . C22 . N23 . 119.7(2) yes C21 . C22 . C25 . 120.7(2) yes N23 . C22 . C25 . 119.6(2) yes Fe2 . N23 . C22 . 128.75(17) yes Fe2 . N23 . O24 . 114.71(14) yes C22 . N23 . O24 . 116.3(2) yes N23 . O24 . Fe1 2_676 118.37(14) yes C22 . C25 . H251 . 108.6 no C22 . C25 . H252 . 108.9 no H251 . C25 . H252 . 110.2 no C22 . C25 . H253 . 109.8 no H251 . C25 . H253 . 110.9 no H252 . C25 . H253 . 108.5 no Fe1 . O26 . Fe2 . 103.10(7) yes Fe1 . O26 . C27 . 124.74(16) yes Fe2 . O26 . C27 . 121.09(15) yes O26 . C27 . H271 . 113.1 no O26 . C27 . H272 . 110.9 no H271 . C27 . H272 . 105.6 no O26 . C27 . H273 . 111.4 no H271 . C27 . H273 . 108.0 no H272 . C27 . H273 . 107.7 no Fe3 . O28 . C29 . 127.8(2) yes Fe3 . O28 . H281 . 128.0 no C29 . O28 . H281 . 100.2 no O28 . C29 . H291 . 109.7 no O28 . C29 . H292 . 106.5 no H291 . C29 . H292 . 109.5 no O28 . C29 . H293 . 109.3 no H291 . C29 . H293 . 111.7 no H292 . C29 . H293 . 110.1 no Fe2 . O30 . Fe3 . 98.24(7) yes Fe2 . O30 . C31 . 126.54(16) yes Fe3 . O30 . C31 . 123.64(16) yes O30 . C31 . H311 . 109.8 no O30 . C31 . H312 . 111.3 no H311 . C31 . H312 . 109.9 no O30 . C31 . H313 . 110.9 no H311 . C31 . H313 . 108.7 no H312 . C31 . H313 . 106.2 no Fe2 . O32 . Fe1 . 98.81(7) yes Fe2 . O32 . Fe1 2_676 112.67(7) yes Fe1 . O32 . Fe1 2_676 97.75(7) yes Fe2 . O32 . Fe3 . 97.49(7) yes Fe1 . O32 . Fe3 . 134.16(8) yes Fe1 2_676 O32 . Fe3 . 114.65(8) yes Fe1 . O33 . S34 . 126.11(10) yes O33 . S34 . O35 . 109.28(10) yes O33 . S34 . O36 . 109.36(10) yes O35 . S34 . O36 . 110.21(10) yes O33 . S34 . O37 . 109.62(10) yes O35 . S34 . O37 . 109.99(10) yes O36 . S34 . O37 . 108.37(10) yes Fe2 . O36 . S34 . 120.37(9) yes Fe3 . O37 . S34 . 124.22(10) yes C39 . N38 . C41 . 111.2(4) yes C39 . N38 . C43 . 115.4(5) yes C41 . N38 . C43 . 108.5(4) yes C39 . N38 . H381 . 106.9 no C41 . N38 . H381 . 107.3 no C43 . N38 . H381 . 107.3 no N38 . C39 . C40 . 119.0(5) yes N38 . C39 . H391 . 106.9 no C40 . C39 . H391 . 107.0 no N38 . C39 . H392 . 107.1 no C40 . C39 . H392 . 107.1 no H391 . C39 . H392 . 109.5 no C39 . C40 . H401 . 109.6 no C39 . C40 . H402 . 109.5 no H401 . C40 . H402 . 109.5 no C39 . C40 . H403 . 109.3 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no N38 . C41 . C42 . 114.4(4) yes N38 . C41 . H411 . 107.4 no C42 . C41 . H411 . 109.3 no N38 . C41 . H412 . 110.8 no C42 . C41 . H412 . 108.4 no H411 . C41 . H412 . 106.3 no C41 . C42 . H421 . 111.7 no C41 . C42 . H422 . 106.7 no H421 . C42 . H422 . 110.4 no C41 . C42 . H423 . 111.2 no H421 . C42 . H423 . 109.6 no H422 . C42 . H423 . 107.2 no N38 . C43 . C44 . 119.1(4) yes N38 . C43 . H431 . 106.1 no C44 . C43 . H431 . 106.3 no N38 . C43 . H432 . 107.7 no C44 . C43 . H432 . 107.9 no H431 . C43 . H432 . 109.5 no C43 . C44 . H441 . 111.5 no C43 . C44 . H442 . 108.1 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 108.8 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no # Attachment 'Complex 5.cif' data_eb6081 _database_code_depnum_ccdc_archive 'CCDC 667682' _audit_creation_method SHELXL-97 _audit_creation_date 06-07-08 #_publ_contact_author_name S.Parsons #_publ_contact_author_email S.Parsons@ed.ac.uk _chemical_compound_source 'Ian Gass IAG779b ' _exptl_crystal_recrystallization_method ; Diffusion of Et2O into MeOH soln ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe8O3(Me-SaO)3(teaH)3(tea)(OAc)3].3MeOH' _chemical_formula_sum 'C57 H93 Fe8 N7 O30' _chemical_formula_weight 1803.18 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' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3c _symmetry_space_group_name_Hall 'R 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 23.2455(8) _cell_length_b 23.2455(8) _cell_length_c 23.7519(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11114.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7705 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour 'very dark red' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5592 _exptl_absorpt_coefficient_mu 1.606 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.188 _exptl_absorpt_correction_T_max 0.521 _exptl_absorpt_process_details 'Sadabs scaled by 0.77' _exptl_special_details ; Data collection strategy optimised with COSMO. Oxford Crysosystems LT device. ; _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 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68038 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7134 _reflns_number_gt 6260 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; The molecule sits on a 3-fold axis. There is some disorderd solvent: this was modelled as disordered MeOH, where a common carbon site forms two part weight O-sites. Part eight H-atoms were not placed. Checkcif output: 061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.46 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. Rather broad, anisotropic peak shapes may be a problem here. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? No action: these were all idealised. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? Part eight H-atoms were not placed, but are included in the formula, M, Dc etc. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given in more chemically meaningful. 202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2 302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. No action. 309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O25 See above. 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C22 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O42 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N12 No action 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 13 The data collection strategy used aimed to achieve a complete data set to 2\q = 54 deg. Some higher angle data were collected in the process and these have been included in the refinement. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 1297 1297 0 23.01 0.550 1.000 1731 1731 0 25.24 0.600 1.000 2244 2244 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 2855 2855 0 29.84 0.700 0.999 3556 3551 5 30.01 0.704 0.996 3621 3608 13 ; _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^)+(0.0640P)^2^+15.7200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(16) _refine_ls_number_reflns 7134 _refine_ls_number_parameters 305 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.006 _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 0.80591(2) 0.35286(2) -0.084855(19) 0.02315(10) Uani 1 1 d . . . Fe2 Fe 0.6667 0.3333 -0.11343(3) 0.02206(16) Uani 1 3 d S . . Fe3 Fe 0.6667 0.3333 0.00718(3) 0.02186(16) Uani 1 3 d S . . Fe4 Fe 0.78977(2) 0.46436(2) -0.017560(18) 0.02385(10) Uani 1 1 d . . . O1 O 0.74339(11) 0.37672(11) -0.05107(9) 0.0235(4) Uani 1 1 d . . . O11 O 0.87044(12) 0.34698(13) -0.13203(10) 0.0312(5) Uani 1 1 d . . . C11 C 0.89305(17) 0.37465(18) -0.18262(16) 0.0313(7) Uani 1 1 d . . . C21 C 0.9111(2) 0.3406(2) -0.22114(18) 0.0415(9) Uani 1 1 d . . . H21 H 0.9069 0.2993 -0.2106 0.050 Uiso 1 1 calc R . . C31 C 0.9346(2) 0.3658(2) -0.27390(18) 0.0500(11) Uani 1 1 d . . . H31 H 0.9472 0.3423 -0.2990 0.060 Uiso 1 1 calc R . . C41 C 0.9401(3) 0.4256(3) -0.29055(17) 0.0523(11) Uani 1 1 d . . . H41 H 0.9547 0.4421 -0.3275 0.063 Uiso 1 1 calc R . . C51 C 0.9241(2) 0.4613(2) -0.25279(18) 0.0460(9) Uani 1 1 d . . . H51 H 0.9285 0.5024 -0.2643 0.055 Uiso 1 1 calc R . . C61 C 0.90153(18) 0.43788(18) -0.19773(15) 0.0333(7) Uani 1 1 d . . . C71 C 0.89174(18) 0.48043(19) -0.15755(16) 0.0339(7) Uani 1 1 d . . . C81 C 0.9201(2) 0.5539(2) -0.1700(2) 0.0480(10) Uani 1 1 d . . . H81A H 0.9283 0.5784 -0.1346 0.072 Uiso 1 1 calc R . . H81B H 0.8884 0.5599 -0.1929 0.072 Uiso 1 1 calc R . . H81C H 0.9620 0.5708 -0.1907 0.072 Uiso 1 1 calc R . . N91 N 0.85955(14) 0.45556(14) -0.11107(13) 0.0290(6) Uani 1 1 d . . . O101 O 0.85764(13) 0.50067(12) -0.07459(11) 0.0346(5) Uani 1 1 d . . . N12 N 0.6667 0.3333 -0.2341(2) 0.0367(12) Uani 1 3 d S . . C22 C 0.6813(2) 0.4010(2) -0.24449(16) 0.0399(8) Uani 1 1 d . . . H22A H 0.6395 0.4013 -0.2516 0.048 Uiso 1 1 calc R . . H22B H 0.7097 0.4188 -0.2784 0.048 Uiso 1 1 calc R . . C32 C 0.71648(18) 0.44438(18) -0.19449(14) 0.0317(7) Uani 1 1 d . . . H32A H 0.7608 0.4486 -0.1899 0.038 Uiso 1 1 calc R . . H32B H 0.7227 0.4893 -0.2002 0.038 Uiso 1 1 calc R . . O42 O 0.67715(12) 0.41470(11) -0.14552(9) 0.0258(5) Uani 1 1 d . . . N13 N 0.73574(14) 0.18630(15) 0.04156(13) 0.0300(6) Uani 1 1 d . . . C23 C 0.7303(2) 0.2138(2) 0.09640(16) 0.0364(8) Uani 1 1 d . . . H23A H 0.7656 0.2178 0.1221 0.044 Uiso 1 1 calc R . . H23B H 0.6868 0.1833 0.1139 0.044 Uiso 1 1 calc R . . C33 C 0.7369(2) 0.28177(19) 0.08786(15) 0.0357(8) Uani 1 1 d . . . H33A H 0.7260 0.2968 0.1232 0.043 Uiso 1 1 calc R . . H33B H 0.7831 0.3146 0.0772 0.043 Uiso 1 1 calc R . . O43 O 0.69303(12) 0.27655(12) 0.04504(9) 0.0273(5) Uani 1 1 d . . . C53 C 0.80430(17) 0.22071(18) 0.01820(17) 0.0344(7) Uani 1 1 d . . . H53A H 0.8261 0.1943 0.0260 0.041 Uiso 1 1 calc R . . H53B H 0.8308 0.2648 0.0362 0.041 Uiso 1 1 calc R . . C63 C 0.80068(18) 0.22895(18) -0.04497(16) 0.0329(7) Uani 1 1 d . . . H63A H 0.8459 0.2555 -0.0608 0.039 Uiso 1 1 calc R . . H63B H 0.7784 0.1850 -0.0636 0.039 Uiso 1 1 calc R . . O73 O 0.76413(12) 0.26179(12) -0.05391(10) 0.0272(5) Uani 1 1 d . . . C83 C 0.70867(18) 0.11319(19) 0.04376(18) 0.0369(8) Uani 1 1 d . . . H83A H 0.7164 0.0982 0.0069 0.044 Uiso 1 1 calc R . . H83B H 0.6601 0.0909 0.0498 0.044 Uiso 1 1 calc R . . C93 C 0.7396(2) 0.0911(2) 0.0904(2) 0.0453(10) Uani 1 1 d . . . H93A H 0.7880 0.1114 0.0844 0.054 Uiso 1 1 calc R . . H93B H 0.7320 0.1050 0.1277 0.054 Uiso 1 1 calc R . . O103 O 0.70789(15) 0.02027(16) 0.08730(17) 0.0523(8) Uani 1 1 d . . . H103 H 0.7261 0.0095 0.0622 0.078 Uiso 1 1 calc R . . O14 O 0.87139(12) 0.38165(13) -0.01917(11) 0.0312(5) Uani 1 1 d . . . C14 C 0.88418(17) 0.42014(17) 0.02244(15) 0.0311(7) Uani 1 1 d . . . O24 O 0.85643(13) 0.45288(13) 0.03304(11) 0.0332(5) Uani 1 1 d . . . C24 C 0.9371(2) 0.4257(2) 0.06276(19) 0.0485(10) Uani 1 1 d . . . H24A H 0.9772 0.4693 0.0583 0.073 Uiso 1 1 calc R . . H24B H 0.9476 0.3907 0.0546 0.073 Uiso 1 1 calc R . . H24C H 0.9208 0.4209 0.1015 0.073 Uiso 1 1 calc R . . C15 C 0.3645(5) 0.0839(5) 0.1507(4) 0.106(2) Uiso 1 1 d . . . O15 O 0.3909(6) 0.0766(6) 0.1941(6) 0.088(3) Uiso 0.40 1 d P A 1 O25 O 0.3300(6) 0.1121(5) 0.1339(4) 0.107(3) Uiso 0.60 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0212(2) 0.0223(2) 0.0265(2) 0.00070(16) 0.00222(17) 0.01122(17) Fe2 0.0214(2) 0.0214(2) 0.0234(4) 0.000 0.000 0.01069(11) Fe3 0.0216(2) 0.0216(2) 0.0223(4) 0.000 0.000 0.01082(11) Fe4 0.0218(2) 0.0207(2) 0.0285(2) -0.00307(17) -0.00162(17) 0.01023(17) O1 0.0197(10) 0.0248(10) 0.0262(10) -0.0023(8) -0.0009(8) 0.0114(9) O11 0.0297(12) 0.0333(12) 0.0340(12) 0.0033(9) 0.0073(10) 0.0182(10) C11 0.0261(15) 0.0350(17) 0.0346(17) 0.0012(14) 0.0056(13) 0.0167(14) C21 0.039(2) 0.039(2) 0.042(2) -0.0028(16) 0.0090(16) 0.0168(17) C31 0.055(3) 0.056(3) 0.038(2) -0.0062(18) 0.0112(18) 0.027(2) C41 0.060(3) 0.062(3) 0.0294(19) 0.0036(18) 0.0110(18) 0.026(2) C51 0.046(2) 0.048(2) 0.038(2) 0.0124(17) 0.0116(17) 0.0188(19) C61 0.0281(16) 0.0352(18) 0.0343(17) 0.0035(14) 0.0058(13) 0.0140(14) C71 0.0307(17) 0.0330(18) 0.0372(18) 0.0085(14) 0.0042(14) 0.0154(14) C81 0.053(2) 0.034(2) 0.057(3) 0.0149(18) 0.022(2) 0.0210(19) N91 0.0237(13) 0.0241(13) 0.0396(15) -0.0007(11) 0.0029(11) 0.0123(11) O101 0.0343(13) 0.0243(11) 0.0431(14) -0.0002(10) 0.0088(11) 0.0130(10) N12 0.0397(18) 0.0397(18) 0.031(3) 0.000 0.000 0.0198(9) C22 0.047(2) 0.045(2) 0.0260(16) 0.0080(15) 0.0045(15) 0.0215(18) C32 0.0320(17) 0.0349(18) 0.0294(16) 0.0067(13) 0.0069(13) 0.0175(15) O42 0.0283(11) 0.0267(11) 0.0240(11) 0.0054(8) 0.0021(9) 0.0150(9) N13 0.0272(14) 0.0318(15) 0.0333(14) 0.0081(11) 0.0010(11) 0.0165(12) C23 0.040(2) 0.042(2) 0.0326(18) 0.0089(15) -0.0028(14) 0.0246(17) C33 0.044(2) 0.0405(19) 0.0268(16) 0.0001(14) -0.0094(14) 0.0246(17) O43 0.0289(11) 0.0304(12) 0.0248(10) 0.0001(9) -0.0045(9) 0.0165(10) C53 0.0235(16) 0.0349(17) 0.046(2) 0.0127(15) -0.0006(14) 0.0158(14) C63 0.0319(17) 0.0319(17) 0.0408(18) 0.0056(14) 0.0046(14) 0.0204(15) O73 0.0277(11) 0.0269(11) 0.0307(11) 0.0036(9) 0.0006(9) 0.0164(9) C83 0.0287(17) 0.0326(18) 0.053(2) 0.0160(16) 0.0058(15) 0.0181(15) C93 0.045(2) 0.047(2) 0.055(2) 0.0189(19) 0.0071(18) 0.0312(19) O103 0.0350(15) 0.0420(15) 0.084(2) 0.0307(16) 0.0123(15) 0.0222(13) O14 0.0281(12) 0.0328(12) 0.0349(12) -0.0022(10) -0.0026(10) 0.0168(10) C14 0.0256(16) 0.0303(16) 0.0355(17) -0.0030(13) -0.0053(13) 0.0126(13) O24 0.0332(13) 0.0329(13) 0.0367(13) -0.0069(10) -0.0082(10) 0.0190(11) C24 0.045(2) 0.065(3) 0.046(2) -0.016(2) -0.0206(18) 0.036(2) _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 O11 1.931(2) . ? Fe1 O1 1.967(2) . ? Fe1 O73 1.977(2) . ? Fe1 O42 1.995(2) 3_665 ? Fe1 O14 2.045(3) . ? Fe1 N91 2.160(3) . ? Fe2 O42 1.938(2) 3_665 ? Fe2 O42 1.938(2) 2_655 ? Fe2 O42 1.938(2) . ? Fe2 O1 2.143(2) . ? Fe2 O1 2.143(2) 3_665 ? Fe2 O1 2.143(2) 2_655 ? Fe2 Fe3 2.8646(9) . ? Fe3 O43 1.933(2) . ? Fe3 O43 1.933(2) 2_655 ? Fe3 O43 1.933(2) 3_665 ? Fe3 O1 2.077(2) 3_665 ? Fe3 O1 2.077(2) . ? Fe3 O1 2.077(2) 2_655 ? Fe4 O101 1.925(3) . ? Fe4 O1 1.936(2) . ? Fe4 O73 2.005(2) 2_655 ? Fe4 O43 2.027(2) 2_655 ? Fe4 O24 2.081(2) . ? Fe4 N13 2.257(3) 2_655 ? O11 C11 1.340(4) . ? C11 C21 1.403(5) . ? C11 C61 1.428(5) . ? C21 C31 1.376(6) . ? C31 C41 1.388(7) . ? C41 C51 1.392(7) . ? C51 C61 1.413(5) . ? C61 C71 1.472(5) . ? C71 N91 1.296(5) . ? C71 C81 1.521(5) . ? N91 O101 1.378(4) . ? N12 C22 1.455(4) 3_665 ? N12 C22 1.455(4) 2_655 ? N12 C22 1.455(4) . ? C22 C32 1.507(5) . ? C32 O42 1.426(4) . ? O42 Fe1 1.995(2) 2_655 ? N13 C23 1.484(5) . ? N13 C53 1.488(4) . ? N13 C83 1.489(5) . ? N13 Fe4 2.257(3) 3_665 ? C23 C33 1.522(5) . ? C33 O43 1.402(4) . ? O43 Fe4 2.027(2) 3_665 ? C53 C63 1.520(5) . ? C63 O73 1.414(4) . ? O73 Fe4 2.005(2) 3_665 ? C83 C93 1.540(5) . ? C93 O103 1.431(5) . ? O14 C14 1.265(4) . ? C14 O24 1.245(4) . ? C14 C24 1.512(5) . ? C15 O15 1.254(14) . ? C15 O25 1.326(13) . ? 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 O11 Fe1 O1 165.05(10) . . ? O11 Fe1 O73 97.06(10) . . ? O1 Fe1 O73 96.53(9) . . ? O11 Fe1 O42 93.85(10) . 3_665 ? O1 Fe1 O42 79.73(9) . 3_665 ? O73 Fe1 O42 90.87(10) . 3_665 ? O11 Fe1 O14 89.33(11) . . ? O1 Fe1 O14 97.50(10) . . ? O73 Fe1 O14 87.34(10) . . ? O42 Fe1 O14 176.52(10) 3_665 . ? O11 Fe1 N91 82.61(11) . . ? O1 Fe1 N91 84.58(10) . . ? O73 Fe1 N91 173.56(11) . . ? O42 Fe1 N91 95.56(11) 3_665 . ? O14 Fe1 N91 86.23(11) . . ? O42 Fe2 O42 105.54(8) 3_665 2_655 ? O42 Fe2 O42 105.54(8) 3_665 . ? O42 Fe2 O42 105.54(8) 2_655 . ? O42 Fe2 O1 76.78(9) 3_665 . ? O42 Fe2 O1 154.24(9) 2_655 . ? O42 Fe2 O1 98.25(9) . . ? O42 Fe2 O1 98.25(9) 3_665 3_665 ? O42 Fe2 O1 76.78(9) 2_655 3_665 ? O42 Fe2 O1 154.24(9) . 3_665 ? O1 Fe2 O1 77.50(9) . 3_665 ? O42 Fe2 O1 154.24(9) 3_665 2_655 ? O42 Fe2 O1 98.25(9) 2_655 2_655 ? O42 Fe2 O1 76.78(9) . 2_655 ? O1 Fe2 O1 77.50(9) . 2_655 ? O1 Fe2 O1 77.50(9) 3_665 2_655 ? O42 Fe2 Fe3 113.16(7) 3_665 . ? O42 Fe2 Fe3 113.16(7) 2_655 . ? O42 Fe2 Fe3 113.16(7) . . ? O1 Fe2 Fe3 46.28(6) . . ? O1 Fe2 Fe3 46.28(6) 3_665 . ? O1 Fe2 Fe3 46.28(6) 2_655 . ? O43 Fe3 O43 100.09(9) . 2_655 ? O43 Fe3 O43 100.09(9) . 3_665 ? O43 Fe3 O43 100.09(9) 2_655 3_665 ? O43 Fe3 O1 80.39(9) . 3_665 ? O43 Fe3 O1 160.69(10) 2_655 3_665 ? O43 Fe3 O1 98.81(9) 3_665 3_665 ? O43 Fe3 O1 98.81(9) . . ? O43 Fe3 O1 80.39(9) 2_655 . ? O43 Fe3 O1 160.69(10) 3_665 . ? O1 Fe3 O1 80.46(9) 3_665 . ? O43 Fe3 O1 160.69(10) . 2_655 ? O43 Fe3 O1 98.81(9) 2_655 2_655 ? O43 Fe3 O1 80.39(9) 3_665 2_655 ? O1 Fe3 O1 80.46(9) 3_665 2_655 ? O1 Fe3 O1 80.46(9) . 2_655 ? O43 Fe3 Fe2 117.73(7) . . ? O43 Fe3 Fe2 117.73(7) 2_655 . ? O43 Fe3 Fe2 117.73(7) 3_665 . ? O1 Fe3 Fe2 48.23(6) 3_665 . ? O1 Fe3 Fe2 48.23(6) . . ? O1 Fe3 Fe2 48.23(6) 2_655 . ? O101 Fe4 O1 94.31(10) . . ? O101 Fe4 O73 92.48(11) . 2_655 ? O1 Fe4 O73 98.35(9) . 2_655 ? O101 Fe4 O43 171.28(11) . 2_655 ? O1 Fe4 O43 81.57(9) . 2_655 ? O73 Fe4 O43 95.72(10) 2_655 2_655 ? O101 Fe4 O24 87.89(11) . . ? O1 Fe4 O24 99.27(10) . . ? O73 Fe4 O24 162.29(9) 2_655 . ? O43 Fe4 O24 85.22(10) 2_655 . ? O101 Fe4 N13 105.35(11) . 2_655 ? O1 Fe4 N13 160.29(11) . 2_655 ? O73 Fe4 N13 79.73(10) 2_655 2_655 ? O43 Fe4 N13 79.13(10) 2_655 2_655 ? O24 Fe4 N13 83.11(10) . 2_655 ? Fe4 O1 Fe1 111.29(11) . . ? Fe4 O1 Fe3 97.37(10) . . ? Fe1 O1 Fe3 135.31(12) . . ? Fe4 O1 Fe2 132.36(11) . . ? Fe1 O1 Fe2 98.26(9) . . ? Fe3 O1 Fe2 85.49(8) . . ? C11 O11 Fe1 128.2(2) . . ? O11 C11 C21 118.0(3) . . ? O11 C11 C61 122.6(3) . . ? C21 C11 C61 119.3(3) . . ? C31 C21 C11 121.4(4) . . ? C21 C31 C41 120.3(4) . . ? C31 C41 C51 119.6(4) . . ? C41 C51 C61 121.7(4) . . ? C51 C61 C11 117.6(3) . . ? C51 C61 C71 119.6(4) . . ? C11 C61 C71 122.7(3) . . ? N91 C71 C61 120.1(3) . . ? N91 C71 C81 119.8(4) . . ? C61 C71 C81 120.1(3) . . ? C71 N91 O101 115.3(3) . . ? C71 N91 Fe1 128.6(3) . . ? O101 N91 Fe1 116.1(2) . . ? N91 O101 Fe4 116.11(19) . . ? C22 N12 C22 117.18(15) 3_665 2_655 ? C22 N12 C22 117.18(15) 3_665 . ? C22 N12 C22 117.18(15) 2_655 . ? N12 C22 C32 110.2(3) . . ? O42 C32 C22 108.5(3) . . ? C32 O42 Fe2 122.0(2) . . ? C32 O42 Fe1 131.0(2) . 2_655 ? Fe2 O42 Fe1 104.51(10) . 2_655 ? C23 N13 C53 113.3(3) . . ? C23 N13 C83 112.5(3) . . ? C53 N13 C83 110.8(3) . . ? C23 N13 Fe4 103.9(2) . 3_665 ? C53 N13 Fe4 105.8(2) . 3_665 ? C83 N13 Fe4 110.1(2) . 3_665 ? N13 C23 C33 110.1(3) . . ? O43 C33 C23 108.4(3) . . ? C33 O43 Fe3 138.1(2) . . ? C33 O43 Fe4 117.8(2) . 3_665 ? Fe3 O43 Fe4 99.17(10) . 3_665 ? N13 C53 C63 108.9(3) . . ? O73 C63 C53 107.6(3) . . ? C63 O73 Fe1 121.9(2) . . ? C63 O73 Fe4 109.7(2) . 3_665 ? Fe1 O73 Fe4 127.41(12) . 3_665 ? N13 C83 C93 113.8(3) . . ? O103 C93 C83 106.8(4) . . ? C14 O14 Fe1 134.5(2) . . ? O24 C14 O14 125.5(3) . . ? O24 C14 C24 117.8(3) . . ? O14 C14 C24 116.7(3) . . ? C14 O24 Fe4 127.5(2) . . ? O15 C15 O25 140.6(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.805 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.090 # Attachment 'Complex 6.cif' data_eb6102 _database_code_depnum_ccdc_archive 'CCDC 667683' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H87 Fe8 N7 O27, 3(C H4 O)' _chemical_formula_sum 'C60 H99 Fe8 N7 O30' _chemical_formula_weight 1845.26 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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_int_tables_number 161 _symmetry_space_group_name_Hall 'R 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 23.3194(7) _cell_length_b 23.3194(7) _cell_length_c 23.8317(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11223.3(9) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7289 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 21.83 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5736 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.05 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'SADABS version 2006/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50293 _diffrn_reflns_av_R_equivalents 0.1417 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3586 _reflns_number_gt 2785 _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, 1997)' _computing_molecular_graphics Shelxp _computing_publication_material Platon _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 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 23.25 Deg. 023_ALERT_3_B Resolution (too) Low [sin(th)/Lambda < 0.6]..... 23.25 Deg. 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 A data cutoff was applied due to poor agreement in higher angle data. 061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.09 The dataset is quite weak and this is probably a consequence of that. 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 etc. 413_ALERT_2_A Short Inter XH3 .. XHn H23E .. H2S4 .. 1.89 Ang. 420_ALERT_2_B D-H Without Acceptor O45 - H45 ... ? 432_ALERT_2_B Short Inter X...Y Contact O45 .. C2S' .. 2.76 Ang. 413_ALERT_2_C Short Inter XH3 .. XHn H26A .. H2S6 .. 2.14 Ang. There is disorder in this region. This may account for the apparent absence of h-bond acceptors and accounts for short contacts. 020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.14 033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.65 Several different solutions were tried for the unit cell for integration. The solution presented was the most agreeable and provided the lowest R-Factor. The quality of the data is generally low. A data cutoff was applied at a level which gives a sensible R-Factor without throwing out too much data. The dataset is generally weak also and this may have affected the Flack parameter. The esd on the Flack parameter is however 0.033 suggesting both hands are present. 202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2 302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. These are due to disorder in the MeOH molecule present in the asymmetric unit. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 Noted, no action taken 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.00 Deg. H2S3 -C2S -H1S' 1.555 1.555 1.555 This is due to shelxs providing details of bond angles which are between atoms in two different parts. ; _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^)+(0.0710P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.65(3) _refine_ls_number_reflns 3586 _refine_ls_number_parameters 314 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.989 _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 1.0000 1.0000 0.46825(8) 0.0277(5) Uani 1 3 d S . . Fe2 Fe 0.86076(5) 0.88194(5) 0.44067(4) 0.0287(3) Uani 1 1 d . . . Fe3 Fe 1.13158(5) 1.12218(5) 0.37334(4) 0.0293(3) Uani 1 1 d . . . Fe4 Fe 1.0000 1.0000 0.34838(8) 0.0277(5) Uani 1 3 d S . . O11 O 0.7964(2) 0.8122(2) 0.4883(2) 0.0327(12) Uani 1 1 d . . . C11 C 0.7755(4) 0.8179(4) 0.5381(4) 0.0386(19) Uani 1 1 d . . . N12 N 1.0000 1.0000 0.5926(4) 0.040(3) Uani 1 3 d S . . N13 N 1.2159(3) 1.1452(3) 0.3146(2) 0.0335(15) Uani 1 1 d . . . O14 O 1.0323(2) 0.9555(2) 0.40668(19) 0.0290(11) Uani 1 1 d . . . O16 O 1.1203(2) 1.1886(2) 0.32265(19) 0.0344(12) Uani 1 1 d . . . C16 C 0.7822(3) 0.8698(4) 0.3344(3) 0.0346(18) Uani 1 1 d . . . C21 C 0.7659(4) 0.8726(4) 0.5533(3) 0.0345(18) Uani 1 1 d . . . C22 C 0.9459(4) 0.9328(4) 0.6011(3) 0.049(2) Uani 1 1 d . . . H22A H 0.9043 0.9333 0.6080 0.059 Uiso 1 1 calc R . . H22B H 0.9551 0.9132 0.6343 0.059 Uiso 1 1 calc R . . C23 C 1.1838(4) 1.1180(4) 0.2598(3) 0.0377(19) Uani 1 1 d . . . H23A H 1.2152 1.1135 0.2347 0.045 Uiso 1 1 calc R . . H23B H 1.1716 1.1487 0.2419 0.045 Uiso 1 1 calc R . . C24 C 0.8616(4) 0.7512(4) 0.3386(4) 0.043(2) Uani 1 1 d . . . H24A H 0.8391 0.7031 0.3311 0.051 Uiso 1 1 calc R . . H24B H 0.8354 0.7691 0.3208 0.051 Uiso 1 1 calc R . . C25 C 1.2627(4) 1.2182(4) 0.3123(4) 0.041(2) Uani 1 1 d . . . H25A H 1.2858 1.2326 0.3488 0.049 Uiso 1 1 calc R . . H25B H 1.2367 1.2408 0.3072 0.049 Uiso 1 1 calc R . . O26 O 0.7952(2) 0.8461(2) 0.3759(2) 0.0332(12) Uani 1 1 d . . . C26 C 0.7286(4) 0.8245(4) 0.2952(4) 0.051(2) Uani 1 1 d . . . H26A H 0.7453 0.8335 0.2566 0.077 Uiso 1 1 calc R . . H26B H 0.6909 0.8319 0.2985 0.077 Uiso 1 1 calc R . . H26C H 0.7145 0.7785 0.3048 0.077 Uiso 1 1 calc R . . C31 C 0.7460(4) 0.8750(4) 0.6079(3) 0.045(2) Uani 1 1 d . . . H31 H 0.7413 0.9116 0.6187 0.053 Uiso 1 1 calc R . . C32 C 0.9386(4) 0.8919(4) 0.5496(3) 0.0337(18) Uani 1 1 d . . . H32A H 0.9792 0.8890 0.5444 0.040 Uiso 1 1 calc R . . H32B H 0.9008 0.8465 0.5547 0.040 Uiso 1 1 calc R . . C33 C 1.1218(4) 1.0504(4) 0.2679(3) 0.041(2) Uani 1 1 d . . . H33A H 1.0960 1.0361 0.2326 0.050 Uiso 1 1 calc R . . H33B H 1.1344 1.0170 0.2782 0.050 Uiso 1 1 calc R . . C34 C 0.8653(4) 0.7632(4) 0.4013(3) 0.0333(18) Uani 1 1 d . . . H34A H 0.8203 0.7446 0.4172 0.040 Uiso 1 1 calc R . . H34B H 0.8876 0.7416 0.4199 0.040 Uiso 1 1 calc R . . C35 C 1.3138(4) 1.2405(4) 0.2666(4) 0.049(2) Uani 1 1 d . . . H35A H 1.3411 1.2192 0.2713 0.058 Uiso 1 1 calc R . . H35B H 1.2919 1.2278 0.2295 0.058 Uiso 1 1 calc R . . C41 C 0.7330(4) 0.8262(4) 0.6468(3) 0.050(2) Uani 1 1 d . . . H41 H 0.7201 0.8295 0.6839 0.060 Uiso 1 1 calc R . . O42 O 0.9280(2) 0.9203(2) 0.50214(18) 0.0287(12) Uani 1 1 d . . . O43 O 1.0834(2) 1.0559(2) 0.31117(19) 0.0304(13) Uani 1 1 d . . . O44 O 0.9014(2) 0.8316(2) 0.40973(19) 0.0299(12) Uani 1 1 d . . . O45 O 1.3545(3) 1.3107(3) 0.2701(3) 0.0564(16) Uani 1 1 d . . . H45 H 1.3833 1.3240 0.2447 0.085 Uiso 1 1 calc R . . C51 C 0.7391(4) 0.7718(4) 0.6309(4) 0.054(2) Uani 1 1 d . . . H51 H 0.7279 0.7365 0.6564 0.065 Uiso 1 1 calc R . . C61 C 0.7606(4) 0.7698(4) 0.5794(3) 0.045(2) Uani 1 1 d . . . H61 H 0.7663 0.7333 0.5703 0.054 Uiso 1 1 calc R . . O211 O 1.1689(2) 1.1911(3) 0.4297(2) 0.0362(12) Uani 1 1 d . . . N211 N 0.8070(3) 0.9319(3) 0.4672(3) 0.0339(15) Uani 1 1 d . . . C211 C 0.7730(4) 0.9233(4) 0.5119(3) 0.0374(19) Uani 1 1 d . . . C221 C 0.7394(4) 0.9640(4) 0.5237(3) 0.0385(19) Uani 1 1 d . . . H22C H 0.7210 0.9701 0.4882 0.046 Uiso 1 1 calc R . . H22D H 0.7021 0.9392 0.5499 0.046 Uiso 1 1 calc R . . C231 C 0.7860(4) 1.0311(4) 0.5484(4) 0.049(2) Uani 1 1 d . . . H23C H 0.7620 1.0550 0.5550 0.073 Uiso 1 1 calc R . . H23D H 0.8226 1.0564 0.5223 0.073 Uiso 1 1 calc R . . H23E H 0.8036 1.0255 0.5841 0.073 Uiso 1 1 calc R . . O1S O 0.7768(5) 1.1153(5) 0.7197(4) 0.058(4) Uiso 0.556(14) 1 d PD A 1 H1S H 0.7631 1.1226 0.7500 0.087 Uiso 0.556(14) 1 d PR A 1 C2S C 0.7471(6) 1.0472(5) 0.7104(4) 0.109(3) Uiso 0.556(14) 1 d PD A 1 H2S1 H 0.7802 1.0333 0.7140 0.164 Uiso 0.556(14) 1 d PR A 1 H2S2 H 0.7278 1.0365 0.6726 0.164 Uiso 0.556(14) 1 d PR A 1 H2S3 H 0.7121 1.0239 0.7383 0.164 Uiso 0.556(14) 1 d PR A 1 O1S' O 0.7471(6) 1.0472(5) 0.7104(4) 0.109(3) Uiso 0.444(14) 1 d PD A 2 H1S' H 0.7362 1.0338 0.7435 0.164 Uiso 0.444(14) 1 d PR A 2 C2S' C 0.7217(10) 0.9921(9) 0.6751(7) 0.059(7) Uiso 0.444(14) 1 d PD A 2 H2S4 H 0.7456(10) 1.0018(9) 0.6463(7) 0.088 Uiso 0.444(14) 1 d PRD A 2 H2S5 H 0.6828(10) 0.9812(9) 0.6657(7) 0.088 Uiso 0.444(14) 1 d PRD A 2 H2S6 H 0.7217(10) 0.9604(9) 0.6918(7) 0.088 Uiso 0.444(14) 1 d PRD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0222(6) 0.0222(6) 0.0386(12) 0.000 0.000 0.0111(3) Fe2 0.0223(6) 0.0216(6) 0.0414(7) 0.0004(5) 0.0023(5) 0.0103(5) Fe3 0.0227(6) 0.0225(6) 0.0425(7) 0.0023(5) 0.0022(5) 0.0111(5) Fe4 0.0226(7) 0.0226(7) 0.0378(12) 0.000 0.000 0.0113(3) O11 0.029(3) 0.028(3) 0.038(3) 0.003(2) 0.006(2) 0.013(2) C11 0.028(4) 0.028(5) 0.052(5) 0.004(4) -0.003(4) 0.008(4) N12 0.035(4) 0.035(4) 0.051(7) 0.000 0.000 0.017(2) N13 0.027(4) 0.024(4) 0.049(4) 0.006(3) 0.006(3) 0.012(3) O14 0.022(3) 0.029(3) 0.038(3) -0.003(2) -0.001(2) 0.014(2) O16 0.032(3) 0.027(3) 0.050(3) 0.005(2) 0.002(2) 0.019(3) C16 0.020(4) 0.032(5) 0.047(5) -0.012(4) -0.009(4) 0.009(4) C21 0.031(4) 0.033(5) 0.040(5) 0.009(4) 0.005(4) 0.016(4) C22 0.057(6) 0.051(6) 0.045(5) 0.011(4) -0.001(4) 0.030(5) C23 0.027(4) 0.040(5) 0.043(5) 0.007(4) 0.005(4) 0.014(4) C24 0.028(5) 0.019(4) 0.077(6) -0.009(4) 0.006(4) 0.008(4) C25 0.027(5) 0.034(5) 0.067(5) 0.008(4) 0.006(4) 0.019(4) O26 0.026(3) 0.028(3) 0.039(3) 0.002(2) -0.003(2) 0.009(2) C26 0.048(6) 0.029(5) 0.065(6) -0.007(4) -0.017(5) 0.011(4) C31 0.045(5) 0.037(5) 0.049(5) 0.000(4) 0.007(4) 0.020(4) C32 0.028(4) 0.035(4) 0.042(5) 0.006(4) 0.005(3) 0.019(4) C33 0.030(5) 0.033(5) 0.057(5) 0.005(4) 0.008(4) 0.013(4) C34 0.023(4) 0.029(4) 0.047(5) 0.000(4) 0.003(3) 0.012(4) C35 0.035(5) 0.051(6) 0.067(6) 0.014(5) 0.010(4) 0.026(5) C41 0.061(6) 0.051(6) 0.040(5) 0.000(4) 0.006(4) 0.029(5) O42 0.029(3) 0.016(3) 0.034(3) -0.001(2) -0.001(2) 0.006(2) O43 0.029(3) 0.027(3) 0.035(3) 0.000(2) 0.006(2) 0.015(2) O44 0.027(3) 0.020(3) 0.044(3) -0.004(2) -0.001(2) 0.012(2) O45 0.039(3) 0.038(3) 0.096(4) 0.034(3) 0.028(3) 0.022(3) C51 0.057(6) 0.045(6) 0.059(6) 0.017(4) 0.013(5) 0.025(5) C61 0.044(5) 0.038(5) 0.057(6) 0.010(4) 0.007(4) 0.022(4) O211 0.023(3) 0.036(3) 0.049(3) -0.001(2) 0.005(2) 0.013(2) N211 0.023(3) 0.030(4) 0.049(4) 0.003(3) -0.001(3) 0.013(3) C211 0.027(4) 0.033(5) 0.052(5) 0.005(4) 0.007(4) 0.015(4) C221 0.032(5) 0.038(5) 0.048(5) 0.003(4) 0.008(4) 0.020(4) C231 0.047(5) 0.035(5) 0.070(6) -0.002(4) 0.005(4) 0.025(5) _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 O42 1.951(5) 2_765 ? Fe1 O42 1.951(5) 3_675 ? Fe1 O42 1.951(5) . ? Fe1 O14 2.140(5) 3_675 ? Fe1 O14 2.140(5) . ? Fe1 O14 2.140(5) 2_765 ? Fe1 Fe4 2.857(2) . ? Fe2 O11 1.936(5) . ? Fe2 O14 1.966(5) 3_675 ? Fe2 O44 1.984(5) . ? Fe2 O42 2.000(5) . ? Fe2 O26 2.034(5) . ? Fe2 N211 2.188(6) . ? Fe3 O14 1.930(5) 2_765 ? Fe3 O211 1.936(5) . ? Fe3 O44 2.007(5) 2_765 ? Fe3 O43 2.028(5) . ? Fe3 O16 2.083(5) . ? Fe3 N13 2.250(6) . ? Fe4 O43 1.931(5) 3_675 ? Fe4 O43 1.931(5) 2_765 ? Fe4 O43 1.931(5) . ? Fe4 O14 2.087(5) 2_765 ? Fe4 O14 2.087(5) . ? Fe4 O14 2.087(5) 3_675 ? O11 C11 1.313(10) . ? C11 C61 1.400(11) . ? C11 C21 1.449(10) . ? N12 C22 1.453(8) . ? N12 C22 1.453(8) 2_765 ? N12 C22 1.453(8) 3_675 ? N13 C23 1.481(9) . ? N13 C24 1.483(9) 2_765 ? N13 C25 1.494(9) . ? O14 Fe3 1.930(5) 3_675 ? O14 Fe2 1.966(5) 2_765 ? O16 C16 1.281(8) 3_675 ? C16 O26 1.242(9) . ? C16 O16 1.281(8) 2_765 ? C16 C26 1.493(10) . ? C21 C31 1.391(10) . ? C21 C211 1.483(10) . ? C22 C32 1.511(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C33 1.528(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N13 1.483(9) 3_675 ? C24 C34 1.513(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C35 1.501(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C41 1.379(12) . ? C31 H31 0.9500 . ? C32 O42 1.393(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O43 1.414(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O44 1.397(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O45 1.427(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C41 C51 1.399(12) . ? C41 H41 0.9500 . ? O44 Fe3 2.007(5) 3_675 ? O45 H45 0.8400 . ? C51 C61 1.335(11) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? O211 N211 1.378(7) 3_675 ? N211 C211 1.282(9) . ? N211 O211 1.378(7) 2_765 ? C211 C221 1.530(11) . ? C221 C231 1.509(11) . ? C221 H22C 0.9900 . ? C221 H22D 0.9900 . ? C231 H23C 0.9800 . ? C231 H23D 0.9800 . ? C231 H23E 0.9800 . ? O1S C2S 1.398(11) . ? O1S H1S 0.8409 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O1S' H1S' 0.8395 . ? C2S' H2S4 0.8400 . ? C2S' H2S5 0.8400 . ? C2S' H2S6 0.8400 . ? 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 O42 Fe1 O42 104.06(16) 2_765 3_675 ? O42 Fe1 O42 104.06(16) 2_765 . ? O42 Fe1 O42 104.06(16) 3_675 . ? O42 Fe1 O14 155.1(2) 2_765 3_675 ? O42 Fe1 O14 99.56(19) 3_675 3_675 ? O42 Fe1 O14 77.18(18) . 3_675 ? O42 Fe1 O14 77.18(18) 2_765 . ? O42 Fe1 O14 155.1(2) 3_675 . ? O42 Fe1 O14 99.56(19) . . ? O14 Fe1 O14 78.2(2) 3_675 . ? O42 Fe1 O14 99.56(19) 2_765 2_765 ? O42 Fe1 O14 77.18(18) 3_675 2_765 ? O42 Fe1 O14 155.1(2) . 2_765 ? O14 Fe1 O14 78.2(2) 3_675 2_765 ? O14 Fe1 O14 78.2(2) . 2_765 ? O42 Fe1 Fe4 114.46(14) 2_765 . ? O42 Fe1 Fe4 114.46(14) 3_675 . ? O42 Fe1 Fe4 114.46(14) . . ? O14 Fe1 Fe4 46.71(13) 3_675 . ? O14 Fe1 Fe4 46.71(13) . . ? O14 Fe1 Fe4 46.71(13) 2_765 . ? O11 Fe2 O14 164.9(2) . 3_675 ? O11 Fe2 O44 96.9(2) . . ? O14 Fe2 O44 96.82(19) 3_675 . ? O11 Fe2 O42 92.9(2) . . ? O14 Fe2 O42 80.25(19) 3_675 . ? O44 Fe2 O42 92.1(2) . . ? O11 Fe2 O26 89.6(2) . . ? O14 Fe2 O26 97.35(19) 3_675 . ? O44 Fe2 O26 87.60(19) . . ? O42 Fe2 O26 177.5(2) . . ? O11 Fe2 N211 82.4(2) . . ? O14 Fe2 N211 84.7(2) 3_675 . ? O44 Fe2 N211 173.3(2) . . ? O42 Fe2 N211 94.6(2) . . ? O26 Fe2 N211 85.7(2) . . ? O14 Fe3 O211 94.7(2) 2_765 . ? O14 Fe3 O44 98.1(2) 2_765 2_765 ? O211 Fe3 O44 93.1(2) . 2_765 ? O14 Fe3 O43 81.5(2) 2_765 . ? O211 Fe3 O43 171.1(2) . . ? O44 Fe3 O43 95.5(2) 2_765 . ? O14 Fe3 O16 99.0(2) 2_765 . ? O211 Fe3 O16 87.5(2) . . ? O44 Fe3 O16 162.73(19) 2_765 . ? O43 Fe3 O16 85.13(19) . . ? O14 Fe3 N13 160.3(2) 2_765 . ? O211 Fe3 N13 104.9(2) . . ? O44 Fe3 N13 79.9(2) 2_765 . ? O43 Fe3 N13 79.2(2) . . ? O16 Fe3 N13 83.2(2) . . ? O43 Fe4 O43 100.59(19) 3_675 2_765 ? O43 Fe4 O43 100.59(19) 3_675 . ? O43 Fe4 O43 100.59(19) 2_765 . ? O43 Fe4 O14 160.3(2) 3_675 2_765 ? O43 Fe4 O14 98.60(19) 2_765 2_765 ? O43 Fe4 O14 79.97(18) . 2_765 ? O43 Fe4 O14 79.97(18) 3_675 . ? O43 Fe4 O14 160.3(2) 2_765 . ? O43 Fe4 O14 98.60(19) . . ? O14 Fe4 O14 80.51(19) 2_765 . ? O43 Fe4 O14 98.60(19) 3_675 3_675 ? O43 Fe4 O14 79.97(18) 2_765 3_675 ? O43 Fe4 O14 160.3(2) . 3_675 ? O14 Fe4 O14 80.51(19) 2_765 3_675 ? O14 Fe4 O14 80.51(19) . 3_675 ? O43 Fe4 Fe1 117.33(15) 3_675 . ? O43 Fe4 Fe1 117.33(15) 2_765 . ? O43 Fe4 Fe1 117.33(15) . . ? O14 Fe4 Fe1 48.26(13) 2_765 . ? O14 Fe4 Fe1 48.26(13) . . ? O14 Fe4 Fe1 48.26(13) 3_675 . ? C11 O11 Fe2 128.0(5) . . ? O11 C11 C61 120.7(7) . . ? O11 C11 C21 123.0(7) . . ? C61 C11 C21 116.3(8) . . ? C22 N12 C22 118.1(3) . 2_765 ? C22 N12 C22 118.1(3) . 3_675 ? C22 N12 C22 118.1(3) 2_765 3_675 ? C23 N13 C24 113.3(6) . 2_765 ? C23 N13 C25 112.4(6) . . ? C24 N13 C25 110.8(6) 2_765 . ? C23 N13 Fe3 104.6(4) . . ? C24 N13 Fe3 105.0(4) 2_765 . ? C25 N13 Fe3 110.4(4) . . ? Fe3 O14 Fe2 111.6(2) 3_675 2_765 ? Fe3 O14 Fe4 97.6(2) 3_675 . ? Fe2 O14 Fe4 135.0(3) 2_765 . ? Fe3 O14 Fe1 132.7(2) 3_675 . ? Fe2 O14 Fe1 98.02(19) 2_765 . ? Fe4 O14 Fe1 85.03(16) . . ? C16 O16 Fe3 126.7(4) 3_675 . ? O26 C16 O16 124.5(6) . 2_765 ? O26 C16 C26 119.2(7) . . ? O16 C16 C26 116.4(7) 2_765 . ? C31 C21 C11 118.1(7) . . ? C31 C21 C211 119.8(7) . . ? C11 C21 C211 122.0(7) . . ? N12 C22 C32 109.2(7) . . ? N12 C22 H22A 109.8 . . ? C32 C22 H22A 109.8 . . ? N12 C22 H22B 109.8 . . ? C32 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? N13 C23 C33 110.2(6) . . ? N13 C23 H23A 109.6 . . ? C33 C23 H23A 109.6 . . ? N13 C23 H23B 109.6 . . ? C33 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N13 C24 C34 109.7(6) 3_675 . ? N13 C24 H24A 109.7 3_675 . ? C34 C24 H24A 109.7 . . ? N13 C24 H24B 109.7 3_675 . ? C34 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N13 C25 C35 115.0(7) . . ? N13 C25 H25A 108.5 . . ? C35 C25 H25A 108.5 . . ? N13 C25 H25B 108.5 . . ? C35 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C16 O26 Fe2 136.1(5) . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C41 C31 C21 122.5(7) . . ? C41 C31 H31 118.8 . . ? C21 C31 H31 118.8 . . ? O42 C32 C22 110.6(6) . . ? O42 C32 H32A 109.5 . . ? C22 C32 H32A 109.5 . . ? O42 C32 H32B 109.5 . . ? C22 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? O43 C33 C23 108.3(6) . . ? O43 C33 H33A 110.0 . . ? C23 C33 H33A 110.0 . . ? O43 C33 H33B 110.0 . . ? C23 C33 H33B 110.0 . . ? H33A C33 H33B 108.4 . . ? O44 C34 C24 107.4(6) . . ? O44 C34 H34A 110.2 . . ? C24 C34 H34A 110.2 . . ? O44 C34 H34B 110.2 . . ? C24 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? O45 C35 C25 108.3(7) . . ? O45 C35 H35A 110.0 . . ? C25 C35 H35A 110.0 . . ? O45 C35 H35B 110.0 . . ? C25 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? C31 C41 C51 119.0(8) . . ? C31 C41 H41 120.5 . . ? C51 C41 H41 120.5 . . ? C32 O42 Fe1 121.0(4) . . ? C32 O42 Fe2 131.9(4) . . ? Fe1 O42 Fe2 103.4(2) . . ? C33 O43 Fe4 138.0(4) . . ? C33 O43 Fe3 117.8(4) . . ? Fe4 O43 Fe3 99.6(2) . . ? C34 O44 Fe2 122.4(4) . . ? C34 O44 Fe3 109.3(4) . 3_675 ? Fe2 O44 Fe3 127.4(2) . 3_675 ? C35 O45 H45 109.5 . . ? C61 C51 C41 119.5(8) . . ? C61 C51 H51 120.3 . . ? C41 C51 H51 120.3 . . ? C51 C61 C11 124.5(8) . . ? C51 C61 H61 117.8 . . ? C11 C61 H61 117.8 . . ? N211 O211 Fe3 116.4(4) 3_675 . ? C211 N211 O211 115.9(6) . 2_765 ? C211 N211 Fe2 129.1(5) . . ? O211 N211 Fe2 114.9(4) 2_765 . ? N211 C211 C21 119.4(7) . . ? N211 C211 C221 121.6(7) . . ? C21 C211 C221 119.0(7) . . ? C231 C221 C211 112.9(7) . . ? C231 C221 H22C 109.0 . . ? C211 C221 H22C 109.0 . . ? C231 C221 H22D 109.0 . . ? C211 C221 H22D 109.0 . . ? H22C C221 H22D 107.8 . . ? C221 C231 H23C 109.5 . . ? C221 C231 H23D 109.5 . . ? H23C C231 H23D 109.5 . . ? C221 C231 H23E 109.5 . . ? H23C C231 H23E 109.5 . . ? H23D C231 H23E 109.5 . . ? O1S C2S H2S1 109.6 . . ? O1S C2S H2S2 109.8 . . ? H2S1 C2S H2S2 109.5 . . ? O1S C2S H2S3 109.0 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O1S C2S H1S' 99.1 . . ? H2S1 C2S H1S' 86.4 . . ? H2S2 C2S H1S' 138.9 . . ? H2S3 C2S H1S' 31.0 . . ? H2S1 C2S' H2S2 76.0 . . ? H2S4 C2S' H2S5 109.5 . . ? H2S4 C2S' H2S6 109.5 . . ? H2S5 C2S' H2S6 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.702 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.086 _chemical_compound_source 'Ian Gass' _exptl_crystal_recrystallization_method 'Slow evaporation of MeOH solution' # Attachment 'Complex 7 Fe8.cif' data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 667684' _audit_creation_date 06-11-12 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb6103 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.2363(5) _cell_length_b 17.6493(6) _cell_length_c 18.6823(6) _cell_angle_alpha 108.435(2) _cell_angle_beta 98.275(2) _cell_angle_gamma 105.150(2) _cell_volume 4749.9(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' 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' 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 = C73 H103 Fe8 N7 O31 # Dc = 1.41 Fooo = 1948.00 Mu = 12.62 M = 2021.43 # Found Formula = C69 H87 Fe8 N7 O27 # Dc = 1.32 FOOO = 1948.00 Mu = 12.54 M = 1893.26 _chemical_formula_sum 'C73 H103 Fe8 N7 O31' _chemical_formula_moiety '[C69 H87 Fe8 N7 O27] 4[CH3OH]' _chemical_compound_source 'Ian gass' _chemical_formula_weight 2021.43 _cell_measurement_reflns_used 5841 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.19 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.262 # Sheldrick geometric approximatio 0.71 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.79 _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 '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 113796 _reflns_number_total 27792 _diffrn_reflns_av_R_equivalents 0.094 # Number of reflections with Friedels Law is 27792 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 29186 _diffrn_reflns_theta_min 1.390 _diffrn_reflns_theta_max 30.579 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.133 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -23 _reflns_limit_h_max 22 _reflns_limit_k_min -25 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _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 -1.29 _refine_diff_density_max 1.80 _refine_ls_number_reflns 19878 _refine_ls_number_restraints 42 _refine_ls_number_parameters 1000 #_refine_ls_R_factor_ref 0.1049 _refine_ls_wR_factor_ref 0.1600 _refine_ls_goodness_of_fit_ref 0.6171 #_reflns_number_all 19878 _refine_ls_R_factor_all 0.1049 _refine_ls_wR_factor_all 0.1600 # 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 9803 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_gt 0.1088 _refine_ls_shift/su_max 0.000470 # 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 mixed # 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 ; _exptl_crystal_recrystallization_method ; grown from methanol ; _refine_special_details ; The solvent region was treated using the SQUEEZE technique. This accounted for 141 electrons per unit cell. This corresponds to 4 methanol molecules per formula unit and has been included in the formula given. The formula weight, Fooo, density and mu have been updated accordingly. Checkcif output; 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1394 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 8 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 5 919_ALERT_3_B # Reflections Likely Effected by the Beamstop .. 1 026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 35 Perc. The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. The data were weak, therefore a cutoff of d=0.8 Ang was applied during refinement. See completeness statistics below. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.07 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.63 Ratio There was some disorder in this region which could not be modelled any better. 420_ALERT_2_B D-H Without Acceptor O435 - H8654 ... ? 420_ALERT_2_B D-H Without Acceptor O437 - H8655 ... ? There was disordered solvent in this region which could not be modelled, see above. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.77 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 etc. 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.09 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C833 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 68 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C19 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O119 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N16 Noted but no action taken. Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 9950 9945 5 23.01 0.550 1.000 13241 13236 5 25.24 0.600 0.999 17200 17189 11 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.997 21854 21799 55 29.84 0.700 0.973 27308 26576 732 30.58 0.716 0.952 29197 27792 1405 ; # 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. 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. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. 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 0.36907(5) 0.60318(5) 0.31562(5) 0.0296 1.0000 Uani . . . . . . Fe2 Fe 0.29227(5) 0.67023(6) 0.21368(5) 0.0309 1.0000 Uani . . . . . . Fe3 Fe 0.48331(5) 0.78410(5) 0.26942(5) 0.0321 1.0000 Uani . . . . . . Fe4 Fe 0.48414(5) 0.59082(5) 0.19679(5) 0.0301 1.0000 Uani . . . . . . Fe5 Fe 0.25474(5) 0.48888(6) 0.10524(5) 0.0316 1.0000 Uani . . . . . . Fe6 Fe 0.17717(5) 0.47942(6) 0.25367(5) 0.0311 1.0000 Uani . . . . . . Fe7 Fe 0.18716(5) 0.69363(6) 0.33584(5) 0.0327 1.0000 Uani . . . . . . Fe8 Fe 0.39102(5) 0.78269(6) 0.43099(5) 0.0317 1.0000 Uani . . . . . . C18 C 0.2654(4) 0.8825(4) 0.4117(3) 0.0406 1.0000 Uani . . . . . . C28 C 0.2525(5) 0.9668(5) 0.4331(5) 0.0650 1.0000 Uani . . . . . . O118 O 0.2019(3) 0.8192(3) 0.3662(2) 0.0420 1.0000 Uani . . . . . . O128 O 0.3393(3) 0.8797(3) 0.4423(2) 0.0391 1.0000 Uani . . . . . . C19 C 0.0611(4) 0.4324(4) 0.0901(3) 0.0374 1.0000 Uani . . . . . . C29 C -0.0320(4) 0.3969(5) 0.0411(4) 0.0506 1.0000 Uani . . . . . . O119 O 0.0715(3) 0.4384(3) 0.1596(2) 0.0374 1.0000 Uani . . . . . . O129 O 0.1215(3) 0.4540(3) 0.0583(2) 0.0402 1.0000 Uani . . . . . . N17 N 0.2605(3) 0.4667(3) -0.0212(3) 0.0385 1.0000 Uani . . . . . . C217 C 0.3551(4) 0.4772(4) -0.0231(4) 0.0388 1.0000 Uani . . . . . . C227 C 0.3975(4) 0.4568(4) 0.0424(3) 0.0377 1.0000 Uani . . . . . . O237 O 0.3824(3) 0.5064(3) 0.1128(2) 0.0364 1.0000 Uani . . . . . . C317 C 0.2350(4) 0.5368(4) -0.0341(4) 0.0425 1.0000 Uani . . . . . . C327 C 0.2774(4) 0.6198(4) 0.0354(4) 0.0407 1.0000 Uani . . . . . . O337 O 0.2617(3) 0.6039(3) 0.1024(2) 0.0343 1.0000 Uani . . . . . . C417 C 0.2009(4) 0.3861(5) -0.0823(4) 0.0479 1.0000 Uani . . . . . . C427 C 0.2197(6) 0.3084(5) -0.0788(4) 0.0616 1.0000 Uani . . . . . . O437 O 0.1533(5) 0.2381(4) -0.1394(4) 0.0900 1.0000 Uani . . . . . . N16 N 0.0429(3) 0.6815(4) 0.2984(3) 0.0402 1.0000 Uani . . . . . . C216 C -0.0078(4) 0.5897(4) 0.2747(4) 0.0408 1.0000 Uani . . . . . . C226 C 0.0430(4) 0.5491(4) 0.3158(4) 0.0421 1.0000 Uani . . . . . . O236 O 0.1297(3) 0.5699(3) 0.3044(2) 0.0366 1.0000 Uani . . . . . . C316 C 0.0421(4) 0.7062(5) 0.2289(4) 0.0437 1.0000 Uani . . . . . . C326 C 0.0974(4) 0.6689(5) 0.1776(3) 0.0399 1.0000 Uani . . . . . . O336 O 0.1820(2) 0.6889(3) 0.2262(2) 0.0360 1.0000 Uani . . . . . . C416 C 0.0030(4) 0.7367(5) 0.3516(4) 0.0472 1.0000 Uani . . . . . . C426 C -0.0016(4) 0.7267(5) 0.4275(4) 0.0535 1.0000 Uani . . . . . . O436 O 0.0779(3) 0.7726(4) 0.4875(3) 0.0680 1.0000 Uani . . . . . . N15 N 0.5122(3) 0.9222(4) 0.2864(3) 0.0417 1.0000 Uani . . . . . . C215 C 0.4345(5) 0.9207(5) 0.2320(4) 0.0486 1.0000 Uani . . . . . . C225 C 0.3506(4) 0.8604(4) 0.2335(4) 0.0460 1.0000 Uani . . . . . . O235 O 0.3610(3) 0.7801(3) 0.2202(2) 0.0364 1.0000 Uani . . . . . . C315 C 0.5139(5) 0.9681(4) 0.3699(4) 0.0460 1.0000 Uani . . . . . . C325 C 0.5328(4) 0.9178(4) 0.4167(4) 0.0390 1.0000 Uani . . . . . . O335 O 0.4731(3) 0.8334(3) 0.3784(2) 0.0337 1.0000 Uani . . . . . . C415 C 0.5929(5) 0.9646(4) 0.2667(4) 0.0496 1.0000 Uani . . . . . . C425 C 0.6781(5) 0.9684(5) 0.3165(5) 0.0563 1.0000 Uani . . . . . . O435 O 0.7479(4) 1.0009(4) 0.2844(4) 0.0711 1.0000 Uani . . . . . . N14 N 0.4499(3) 0.5379(3) 0.4232(3) 0.0376 1.0000 Uani . . . . . . C214 C 0.5036(4) 0.6178(4) 0.4841(3) 0.0384 1.0000 Uani . . . . . . C224 C 0.5215(4) 0.6861(4) 0.4521(3) 0.0329 1.0000 Uani . . . . . . O234 O 0.4394(2) 0.6879(3) 0.4149(2) 0.0326 1.0000 Uani . . . . . . C314 C 0.4945(4) 0.4915(4) 0.3719(4) 0.0370 1.0000 Uani . . . . . . C324 C 0.4501(4) 0.4689(4) 0.2874(4) 0.0374 1.0000 Uani . . . . . . O334 O 0.4467(3) 0.5430(3) 0.2751(2) 0.0318 1.0000 Uani . . . . . . C414 C 0.3691(4) 0.4907(4) 0.4362(4) 0.0394 1.0000 Uani . . . . . . C424 C 0.2956(4) 0.5251(4) 0.4195(3) 0.0345 1.0000 Uani . . . . . . O434 O 0.2841(2) 0.5242(3) 0.3423(2) 0.0322 1.0000 Uani . . . . . . O13 O 0.1154(3) 0.3966(3) 0.2913(3) 0.0386 1.0000 Uani . . . . . . C23 C 0.1498(4) 0.3452(4) 0.3140(4) 0.0394 1.0000 Uani . . . . . . C33 C 0.1335(4) 0.3305(4) 0.3809(4) 0.0449 1.0000 Uani . . . . . . C43 C 0.1708(5) 0.2817(5) 0.4103(5) 0.0567 1.0000 Uani . . . . . . C53 C 0.2261(6) 0.2444(5) 0.3729(5) 0.0650 1.0000 Uani . . . . . . C63 C 0.2404(5) 0.2556(5) 0.3054(5) 0.0575 1.0000 Uani . . . . . . C73 C 0.2032(4) 0.3043(4) 0.2738(4) 0.0436 1.0000 Uani . . . . . . C83 C 0.2209(4) 0.3121(4) 0.2007(4) 0.0440 1.0000 Uani . U . . . . N93 N 0.2167(3) 0.3762(3) 0.1855(3) 0.0337 1.0000 Uani . . . . . . O103 O 0.2330(3) 0.3798(3) 0.1162(2) 0.0383 1.0000 Uani . . . . . . C813 C 0.2464(6) 0.2435(5) 0.1478(5) 0.0634 1.0000 Uani . U . . . . C823 C 0.1938(9) 0.1608(7) 0.1262(7) 0.1057 1.0000 Uani . U . . . . C833 C 0.2210(11) 0.0947(8) 0.0832(8) 0.1337 1.0000 Uani . U . . . . C843 C 0.3004(10) 0.1149(8) 0.0639(8) 0.1211 1.0000 Uani . U . . . . C853 C 0.3533(8) 0.1933(7) 0.0877(6) 0.0859 1.0000 Uani . U . . . . C863 C 0.3265(6) 0.2581(6) 0.1302(5) 0.0681 1.0000 Uani . U . . . . O12 O 0.5639(3) 0.5275(3) 0.1768(2) 0.0371 1.0000 Uani . . . . . . C22 C 0.6319(4) 0.5274(4) 0.2254(4) 0.0370 1.0000 Uani . . . . . . C32 C 0.6513(4) 0.4519(4) 0.2114(4) 0.0438 1.0000 Uani . . . . . . C42 C 0.7200(5) 0.4472(5) 0.2614(5) 0.0539 1.0000 Uani . . . . . . C52 C 0.7721(5) 0.5175(5) 0.3254(5) 0.0581 1.0000 Uani . . . . . . C62 C 0.7563(4) 0.5933(5) 0.3379(5) 0.0507 1.0000 Uani . . . . . . C72 C 0.6861(4) 0.5996(4) 0.2892(4) 0.0385 1.0000 Uani . . . . . . C82 C 0.6740(4) 0.6829(4) 0.3075(4) 0.0340 1.0000 Uani . . . . . . N92 N 0.5992(3) 0.6899(3) 0.2793(3) 0.0335 1.0000 Uani . . . . . . O102 O 0.5954(3) 0.7696(3) 0.3025(3) 0.0405 1.0000 Uani . . . . . . C812 C 0.7469(4) 0.7619(4) 0.3598(4) 0.0403 1.0000 Uani . . . . . . C822 C 0.7559(4) 0.7934(5) 0.4394(4) 0.0487 1.0000 Uani . . . . . . C832 C 0.8225(5) 0.8665(5) 0.4866(5) 0.0580 1.0000 Uani . . . . . . C842 C 0.8786(5) 0.9096(5) 0.4536(6) 0.0666 1.0000 Uani . . . . . . C852 C 0.8706(5) 0.8795(6) 0.3745(7) 0.0751 1.0000 Uani . . . . . . C862 C 0.8044(5) 0.8045(5) 0.3272(5) 0.0540 1.0000 Uani . . . . . . O11 O 0.4641(3) 0.8412(3) 0.5356(2) 0.0372 1.0000 Uani . . . . . . C21 C 0.4665(4) 0.8156(4) 0.5946(3) 0.0365 1.0000 Uani . . . . . . C31 C 0.5488(4) 0.8436(5) 0.6495(4) 0.0438 1.0000 Uani . . . . . . C41 C 0.5566(5) 0.8179(5) 0.7112(4) 0.0523 1.0000 Uani . . . . . . C51 C 0.4862(5) 0.7628(6) 0.7210(5) 0.0611 1.0000 Uani . . . . . . C61 C 0.4053(5) 0.7367(5) 0.6704(4) 0.0533 1.0000 Uani . . . . . . C71 C 0.3935(4) 0.7626(4) 0.6076(3) 0.0380 1.0000 Uani . . . . . . C81 C 0.3034(4) 0.7361(4) 0.5576(3) 0.0372 1.0000 Uani . . . . . . N91 N 0.2927(3) 0.7367(3) 0.4883(3) 0.0346 1.0000 Uani . . . . . . O101 O 0.2061(3) 0.7101(3) 0.4466(2) 0.0406 1.0000 Uani . . . . . . C811 C 0.2270(4) 0.7092(4) 0.5907(4) 0.0389 1.0000 Uani . . . . . . C821 C 0.2187(5) 0.7667(5) 0.6579(4) 0.0539 1.0000 Uani . . . . . . C831 C 0.1508(5) 0.7434(6) 0.6908(5) 0.0616 1.0000 Uani . . . . . . C841 C 0.0906(5) 0.6626(6) 0.6590(4) 0.0550 1.0000 Uani . . . . . . C851 C 0.0981(4) 0.6048(5) 0.5919(5) 0.0517 1.0000 Uani . . . . . . C861 C 0.1665(4) 0.6290(5) 0.5586(4) 0.0468 1.0000 Uani . . . . . . O3 O 0.2611(2) 0.5486(3) 0.2139(2) 0.0306 1.0000 Uani . . . . . . O7 O 0.3060(2) 0.6979(2) 0.3334(2) 0.0292 1.0000 Uani . . . . . . O29 O 0.5168(3) 0.6459(3) 0.1174(2) 0.0377 1.0000 Uani . . . . . . C30 C 0.5205(4) 0.7160(4) 0.1132(4) 0.0357 1.0000 Uani . . . . . . O31 O 0.5109(3) 0.7770(3) 0.1650(3) 0.0412 1.0000 Uani . . . . . . C865 C 0.5384(5) 0.7317(5) 0.0416(4) 0.0550 1.0000 Uani . . . . . . O2 O 0.4186(2) 0.6660(2) 0.2434(2) 0.0294 1.0000 Uani . . . . . . H281 H 0.3018 1.0077 0.4289 0.0861 1.0000 Uiso R . . . . . H282 H 0.2453 0.9854 0.4851 0.0859 1.0000 Uiso R . . . . . H283 H 0.1994 0.9617 0.3974 0.0858 1.0000 Uiso R . . . . . H291 H -0.0439 0.4335 0.0161 0.0619 1.0000 Uiso R . . . . . H292 H -0.0744 0.3899 0.0716 0.0619 1.0000 Uiso R . . . . . H293 H -0.0419 0.3442 0.0028 0.0619 1.0000 Uiso R . . . . . H2171 H 0.3837 0.5352 -0.0159 0.0410 1.0000 Uiso R . . . . . H2172 H 0.3588 0.4418 -0.0732 0.0410 1.0000 Uiso R . . . . . H2271 H 0.4596 0.4730 0.0461 0.0379 1.0000 Uiso R . . . . . H2272 H 0.3738 0.3970 0.0335 0.0379 1.0000 Uiso R . . . . . H3171 H 0.2482 0.5434 -0.0808 0.0481 1.0000 Uiso R . . . . . H3172 H 0.1710 0.5219 -0.0413 0.0480 1.0000 Uiso R . . . . . H3271 H 0.2519 0.6628 0.0287 0.0457 1.0000 Uiso R . . . . . H3272 H 0.3398 0.6427 0.0417 0.0457 1.0000 Uiso R . . . . . H4171 H 0.2033 0.3898 -0.1330 0.0439 1.0000 Uiso R . . . . . H4172 H 0.1424 0.3833 -0.0741 0.0439 1.0000 Uiso R . . . . . H4271 H 0.2779 0.3097 -0.0901 0.0641 1.0000 Uiso R . . . . . H4272 H 0.2204 0.3022 -0.0283 0.0645 1.0000 Uiso R . . . . . H2161 H -0.0633 0.5861 0.2885 0.0451 1.0000 Uiso R . . . . . H2162 H -0.0185 0.5626 0.2186 0.0449 1.0000 Uiso R . . . . . H2261 H 0.0471 0.5736 0.3723 0.0490 1.0000 Uiso R . . . . . H2262 H 0.0147 0.4891 0.2974 0.0489 1.0000 Uiso R . . . . . H3161 H 0.0636 0.7673 0.2474 0.0448 1.0000 Uiso R . . . . . H3162 H -0.0184 0.6864 0.2000 0.0449 1.0000 Uiso R . . . . . H3261 H 0.1024 0.6918 0.1370 0.0450 1.0000 Uiso R . . . . . H3262 H 0.0716 0.6061 0.1528 0.0446 1.0000 Uiso R . . . . . H4161 H 0.0356 0.7949 0.3616 0.0499 1.0000 Uiso R . . . . . H4162 H -0.0566 0.7251 0.3227 0.0497 1.0000 Uiso R . . . . . H4261 H -0.0496 0.7444 0.4438 0.0578 1.0000 Uiso R . . . . . H4262 H -0.0142 0.6673 0.4186 0.0581 1.0000 Uiso R . . . . . H2151 H 0.4286 0.9766 0.2477 0.0526 1.0000 Uiso R . . . . . H2152 H 0.4423 0.9046 0.1794 0.0528 1.0000 Uiso R . . . . . H2251 H 0.3369 0.8811 0.2821 0.0511 1.0000 Uiso R . . . . . H2252 H 0.3039 0.8547 0.1920 0.0510 1.0000 Uiso R . . . . . H3151 H 0.5601 1.0233 0.3912 0.0509 1.0000 Uiso R . . . . . H3152 H 0.4581 0.9769 0.3740 0.0511 1.0000 Uiso R . . . . . H3251 H 0.5216 0.9423 0.4681 0.0366 1.0000 Uiso R . . . . . H3252 H 0.5916 0.9168 0.4218 0.0371 1.0000 Uiso R . . . . . H4151 H 0.5946 1.0216 0.2727 0.0480 1.0000 Uiso R . . . . . H4152 H 0.5893 0.9309 0.2132 0.0482 1.0000 Uiso R . . . . . H4251 H 0.6877 1.0052 0.3703 0.0578 1.0000 Uiso R . . . . . H4252 H 0.6774 0.9126 0.3145 0.0578 1.0000 Uiso R . . . . . H2141 H 0.5583 0.6132 0.5075 0.0397 1.0000 Uiso R . . . . . H2142 H 0.4730 0.6328 0.5250 0.0401 1.0000 Uiso R . . . . . H2241 H 0.5564 0.7402 0.4940 0.0302 1.0000 Uiso R . . . . . H2242 H 0.5552 0.6718 0.4128 0.0298 1.0000 Uiso R . . . . . H3141 H 0.5545 0.5259 0.3813 0.0429 1.0000 Uiso R . . . . . H3142 H 0.4924 0.4385 0.3789 0.0429 1.0000 Uiso R . . . . . H3241 H 0.4842 0.4429 0.2550 0.0395 1.0000 Uiso R . . . . . H3242 H 0.3908 0.4302 0.2741 0.0398 1.0000 Uiso R . . . . . H4141 H 0.3796 0.4952 0.4905 0.0460 1.0000 Uiso R . . . . . H4142 H 0.3516 0.4303 0.4011 0.0459 1.0000 Uiso R . . . . . H4241 H 0.3103 0.5832 0.4564 0.0380 1.0000 Uiso R . . . . . H4242 H 0.2409 0.4908 0.4248 0.0378 1.0000 Uiso R . . . . . H331 H 0.0950 0.3551 0.4064 0.0526 1.0000 Uiso R . . . . . H431 H 0.1614 0.2764 0.4572 0.0738 1.0000 Uiso R . . . . . H531 H 0.2531 0.2112 0.3919 0.0830 1.0000 Uiso R . . . . . H631 H 0.2783 0.2308 0.2811 0.0719 1.0000 Uiso R . . . . . H8231 H 0.1425 0.1517 0.1439 0.1222 1.0000 Uiso R . . . . . H8331 H 0.1836 0.0392 0.0658 0.1380 1.0000 Uiso R . . . . . H8431 H 0.3165 0.0725 0.0298 0.1322 1.0000 Uiso R . . . . . H8531 H 0.4106 0.2063 0.0817 0.1161 1.0000 Uiso R . . . . . H8631 H 0.3626 0.3137 0.1458 0.0970 1.0000 Uiso R . . . . . H321 H 0.6192 0.4060 0.1680 0.0494 1.0000 Uiso R . . . . . H421 H 0.7281 0.3956 0.2544 0.0648 1.0000 Uiso R . . . . . H521 H 0.8179 0.5154 0.3602 0.0638 1.0000 Uiso R . . . . . H621 H 0.7937 0.6415 0.3783 0.0548 1.0000 Uiso R . . . . . H8221 H 0.7168 0.7629 0.4603 0.0490 1.0000 Uiso R . . . . . H8321 H 0.8273 0.8879 0.5407 0.0622 1.0000 Uiso R . . . . . H8421 H 0.9217 0.9620 0.4846 0.0781 1.0000 Uiso R . . . . . H8521 H 0.9098 0.9078 0.3526 0.0830 1.0000 Uiso R . . . . . H8621 H 0.7972 0.7829 0.2731 0.0587 1.0000 Uiso R . . . . . H311 H 0.5973 0.8805 0.6434 0.0449 1.0000 Uiso R . . . . . H411 H 0.6118 0.8363 0.7445 0.0551 1.0000 Uiso R . . . . . H511 H 0.4949 0.7418 0.7611 0.0808 1.0000 Uiso R . . . . . H611 H 0.3567 0.6998 0.6765 0.0588 1.0000 Uiso R . . . . . H8211 H 0.2610 0.8200 0.6804 0.0549 1.0000 Uiso R . . . . . H8311 H 0.1431 0.7843 0.7345 0.0711 1.0000 Uiso R . . . . . H8411 H 0.0458 0.6468 0.6819 0.0660 1.0000 Uiso R . . . . . H8511 H 0.0585 0.5485 0.5704 0.0600 1.0000 Uiso R . . . . . H8611 H 0.1691 0.5908 0.5117 0.0547 1.0000 Uiso R . . . . . H8651 H 0.5164 0.7761 0.0373 0.0787 1.0000 Uiso R . . . . . H8652 H 0.6008 0.7497 0.0479 0.0792 1.0000 Uiso R . . . . . H8653 H 0.5116 0.6820 -0.0023 0.0789 1.0000 Uiso R . . . . . H1 H 0.1159 0.7515 0.4727 0.0860 1.0000 Uiso R . . . . . H8654 H 0.7971 1.0082 0.3120 0.0941 1.0000 Uiso R . . . . . H8655 H 0.1903 0.2126 -0.1410 0.1053 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 0.0238(4) 0.0366(5) 0.0258(4) 0.0054(3) 0.0065(3) 0.0132(3) Fe2 0.0247(4) 0.0393(5) 0.0255(4) 0.0049(4) 0.0047(3) 0.0147(4) Fe3 0.0260(4) 0.0352(5) 0.0307(4) 0.0046(4) 0.0048(3) 0.0134(4) Fe4 0.0249(4) 0.0375(5) 0.0280(4) 0.0075(4) 0.0081(3) 0.0154(4) Fe5 0.0251(4) 0.0405(5) 0.0241(4) 0.0041(4) 0.0055(3) 0.0125(4) Fe6 0.0226(4) 0.0406(5) 0.0274(4) 0.0077(4) 0.0060(3) 0.0123(4) Fe7 0.0247(4) 0.0445(5) 0.0239(4) 0.0023(4) 0.0043(3) 0.0171(4) Fe8 0.0261(4) 0.0381(5) 0.0256(4) 0.0026(4) 0.0030(3) 0.0151(4) C18 0.041(4) 0.047(4) 0.027(3) 0.001(3) 0.005(3) 0.023(3) C28 0.053(5) 0.061(5) 0.062(5) -0.003(4) -0.014(4) 0.034(4) O118 0.033(2) 0.048(3) 0.037(2) 0.002(2) 0.0026(19) 0.022(2) O128 0.036(2) 0.042(3) 0.034(2) 0.0020(19) 0.0031(18) 0.021(2) C19 0.034(3) 0.041(4) 0.030(3) 0.004(3) 0.003(3) 0.015(3) C29 0.028(3) 0.071(5) 0.040(4) 0.013(4) -0.001(3) 0.010(3) O119 0.025(2) 0.052(3) 0.030(2) 0.0085(19) 0.0068(17) 0.0134(19) O129 0.030(2) 0.055(3) 0.030(2) 0.009(2) 0.0066(18) 0.015(2) N17 0.036(3) 0.048(3) 0.027(3) 0.003(2) 0.008(2) 0.018(2) C217 0.033(3) 0.045(4) 0.035(3) 0.003(3) 0.016(3) 0.018(3) C227 0.032(3) 0.042(4) 0.031(3) 0.000(3) 0.013(2) 0.013(3) O237 0.028(2) 0.046(3) 0.029(2) 0.0020(18) 0.0105(17) 0.0162(19) C317 0.040(3) 0.063(5) 0.030(3) 0.017(3) 0.011(3) 0.023(3) C327 0.042(4) 0.049(4) 0.035(3) 0.014(3) 0.015(3) 0.021(3) O337 0.031(2) 0.045(3) 0.025(2) 0.0079(18) 0.0075(16) 0.0160(19) C417 0.040(4) 0.061(5) 0.028(3) 0.000(3) 0.007(3) 0.014(3) C427 0.065(5) 0.054(5) 0.041(4) -0.001(3) 0.000(4) 0.010(4) O437 0.086(5) 0.073(4) 0.063(4) -0.005(3) -0.012(3) 0.003(4) N16 0.028(3) 0.056(3) 0.033(3) 0.005(2) 0.005(2) 0.023(2) C216 0.021(3) 0.058(4) 0.038(3) 0.007(3) 0.011(2) 0.014(3) C226 0.026(3) 0.052(4) 0.046(4) 0.011(3) 0.015(3) 0.016(3) O236 0.026(2) 0.050(3) 0.033(2) 0.0080(19) 0.0104(17) 0.0168(19) C316 0.030(3) 0.059(4) 0.038(3) 0.010(3) 0.001(3) 0.021(3) C326 0.029(3) 0.063(4) 0.024(3) 0.007(3) 0.002(2) 0.022(3) O336 0.025(2) 0.049(3) 0.027(2) 0.0039(18) 0.0036(16) 0.0158(19) C416 0.033(3) 0.065(5) 0.040(4) 0.006(3) 0.009(3) 0.027(3) C426 0.032(3) 0.079(5) 0.042(4) 0.004(4) 0.011(3) 0.029(4) O436 0.047(3) 0.101(4) 0.041(3) -0.006(3) 0.004(2) 0.042(3) N15 0.033(3) 0.048(3) 0.038(3) 0.008(2) 0.006(2) 0.014(2) C215 0.056(4) 0.046(4) 0.049(4) 0.016(3) 0.010(3) 0.028(4) C225 0.039(4) 0.054(4) 0.047(4) 0.014(3) 0.006(3) 0.026(3) O235 0.030(2) 0.043(3) 0.035(2) 0.0100(19) 0.0046(17) 0.0196(19) C315 0.046(4) 0.034(4) 0.045(4) -0.002(3) 0.008(3) 0.014(3) C325 0.031(3) 0.034(3) 0.039(3) 0.000(3) 0.005(3) 0.009(3) O335 0.029(2) 0.037(2) 0.028(2) 0.0043(17) 0.0013(16) 0.0118(18) C415 0.050(4) 0.037(4) 0.051(4) 0.006(3) 0.008(3) 0.014(3) C425 0.040(4) 0.051(5) 0.059(5) 0.013(4) 0.001(3) 0.002(3) O435 0.048(3) 0.066(4) 0.083(4) 0.017(3) 0.010(3) 0.009(3) N14 0.032(3) 0.040(3) 0.038(3) 0.008(2) 0.011(2) 0.014(2) C214 0.032(3) 0.045(4) 0.030(3) 0.002(3) -0.001(2) 0.019(3) C224 0.023(3) 0.040(3) 0.031(3) 0.006(3) 0.004(2) 0.013(2) O234 0.028(2) 0.043(2) 0.025(2) 0.0036(17) 0.0034(16) 0.0215(18) C314 0.034(3) 0.040(4) 0.040(3) 0.012(3) 0.015(3) 0.018(3) C324 0.036(3) 0.039(4) 0.038(3) 0.009(3) 0.014(3) 0.018(3) O334 0.030(2) 0.040(2) 0.029(2) 0.0103(18) 0.0111(17) 0.0177(18) C414 0.042(4) 0.041(4) 0.035(3) 0.012(3) 0.007(3) 0.019(3) C424 0.031(3) 0.044(4) 0.029(3) 0.008(3) 0.012(2) 0.016(3) O434 0.028(2) 0.042(2) 0.026(2) 0.0095(18) 0.0059(16) 0.0135(18) O13 0.030(2) 0.043(3) 0.043(2) 0.014(2) 0.0119(19) 0.0121(19) C23 0.027(3) 0.038(4) 0.046(4) 0.011(3) 0.005(3) 0.006(3) C33 0.035(3) 0.049(4) 0.052(4) 0.020(3) 0.011(3) 0.014(3) C43 0.052(4) 0.061(5) 0.064(5) 0.031(4) 0.018(4) 0.018(4) C53 0.073(6) 0.066(6) 0.080(6) 0.042(5) 0.029(5) 0.037(5) C63 0.056(5) 0.057(5) 0.074(5) 0.032(4) 0.028(4) 0.028(4) C73 0.039(4) 0.044(4) 0.046(4) 0.013(3) 0.010(3) 0.013(3) C83 0.042(3) 0.048(4) 0.045(4) 0.014(3) 0.014(3) 0.022(3) N93 0.022(2) 0.041(3) 0.030(3) 0.006(2) 0.0063(19) 0.007(2) O103 0.036(2) 0.043(3) 0.033(2) 0.0079(19) 0.0114(18) 0.014(2) C813 0.085(4) 0.052(4) 0.064(4) 0.017(3) 0.032(4) 0.037(3) C823 0.137(7) 0.065(5) 0.104(6) 0.007(5) 0.051(5) 0.035(5) C833 0.174(8) 0.078(6) 0.132(7) 0.006(5) 0.060(6) 0.042(6) C843 0.164(8) 0.095(6) 0.112(6) 0.011(5) 0.072(6) 0.067(6) C853 0.126(6) 0.094(5) 0.074(5) 0.033(4) 0.057(5) 0.073(5) C863 0.096(5) 0.078(5) 0.055(4) 0.026(4) 0.036(4) 0.059(4) O12 0.033(2) 0.046(3) 0.033(2) 0.0075(19) 0.0117(18) 0.021(2) C22 0.028(3) 0.051(4) 0.042(3) 0.020(3) 0.018(3) 0.018(3) C32 0.037(3) 0.047(4) 0.054(4) 0.020(3) 0.017(3) 0.021(3) C42 0.044(4) 0.052(5) 0.075(5) 0.029(4) 0.013(4) 0.026(4) C52 0.034(4) 0.056(5) 0.085(6) 0.031(4) 0.000(4) 0.017(3) C62 0.032(3) 0.056(5) 0.065(5) 0.024(4) 0.008(3) 0.016(3) C72 0.019(3) 0.049(4) 0.053(4) 0.023(3) 0.011(3) 0.013(3) C82 0.025(3) 0.042(4) 0.037(3) 0.017(3) 0.010(2) 0.011(3) N92 0.028(2) 0.037(3) 0.034(3) 0.008(2) 0.007(2) 0.015(2) O102 0.030(2) 0.040(3) 0.043(2) 0.005(2) 0.0033(19) 0.0147(19) C812 0.020(3) 0.043(4) 0.058(4) 0.020(3) 0.004(3) 0.012(3) C822 0.029(3) 0.054(4) 0.053(4) 0.019(4) -0.001(3) 0.006(3) C832 0.036(4) 0.055(5) 0.072(5) 0.018(4) -0.005(4) 0.014(3) C842 0.033(4) 0.039(4) 0.101(7) 0.003(4) 0.003(4) 0.004(3) C852 0.039(4) 0.061(6) 0.122(9) 0.032(6) 0.029(5) 0.009(4) C862 0.043(4) 0.053(5) 0.073(5) 0.028(4) 0.019(4) 0.018(3) O11 0.036(2) 0.043(3) 0.027(2) 0.0047(18) 0.0012(17) 0.019(2) C21 0.035(3) 0.042(4) 0.025(3) -0.002(3) 0.000(2) 0.022(3) C31 0.031(3) 0.055(4) 0.038(3) 0.008(3) 0.004(3) 0.017(3) C41 0.040(4) 0.080(6) 0.037(4) 0.018(4) 0.000(3) 0.029(4) C51 0.043(4) 0.095(7) 0.048(4) 0.031(4) 0.007(3) 0.022(4) C61 0.033(3) 0.084(6) 0.048(4) 0.032(4) 0.011(3) 0.016(4) C71 0.036(3) 0.052(4) 0.027(3) 0.008(3) 0.010(2) 0.022(3) C81 0.029(3) 0.050(4) 0.031(3) 0.009(3) 0.005(2) 0.019(3) N91 0.022(2) 0.042(3) 0.029(3) 0.000(2) 0.0024(19) 0.014(2) O101 0.024(2) 0.064(3) 0.027(2) 0.007(2) 0.0039(17) 0.018(2) C811 0.032(3) 0.048(4) 0.035(3) 0.011(3) 0.010(3) 0.015(3) C821 0.038(4) 0.064(5) 0.046(4) 0.007(4) 0.012(3) 0.011(3) C831 0.054(5) 0.078(6) 0.047(4) 0.010(4) 0.023(4) 0.023(4) C841 0.035(4) 0.086(6) 0.057(5) 0.035(4) 0.022(3) 0.026(4) C851 0.032(3) 0.061(5) 0.062(5) 0.024(4) 0.015(3) 0.012(3) C861 0.040(4) 0.053(4) 0.048(4) 0.013(3) 0.014(3) 0.021(3) O3 0.0230(19) 0.044(2) 0.0209(18) 0.0043(17) 0.0062(15) 0.0131(17) O7 0.0245(19) 0.036(2) 0.0208(18) 0.0004(16) 0.0051(15) 0.0128(17) O29 0.034(2) 0.043(3) 0.037(2) 0.010(2) 0.0125(18) 0.017(2) C30 0.027(3) 0.042(4) 0.039(3) 0.014(3) 0.010(3) 0.014(3) O31 0.041(2) 0.039(3) 0.044(3) 0.012(2) 0.014(2) 0.017(2) C865 0.072(5) 0.051(4) 0.053(4) 0.019(4) 0.031(4) 0.030(4) O2 0.0216(18) 0.035(2) 0.0269(19) 0.0023(17) 0.0043(15) 0.0144(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17871(6) 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 . O234 . 1.930(4) yes Fe1 . O334 . 1.937(4) yes Fe1 . O434 . 1.931(4) yes Fe1 . O3 . 2.148(4) yes Fe1 . O7 . 2.144(4) yes Fe1 . O2 . 2.120(4) yes Fe2 . O337 . 1.950(4) yes Fe2 . O336 . 1.937(4) yes Fe2 . O235 . 1.924(4) yes Fe2 . O3 . 2.075(4) yes Fe2 . O7 . 2.097(4) yes Fe2 . O2 . 2.073(4) yes Fe3 . N15 . 2.265(6) yes Fe3 . O235 . 2.039(4) yes Fe3 . O335 . 1.995(4) yes Fe3 . O102 . 1.944(4) yes Fe3 . O31 . 2.038(4) yes Fe3 . O2 . 1.936(4) yes Fe4 . O237 . 1.975(4) yes Fe4 . O334 . 1.998(4) yes Fe4 . O12 . 1.923(4) yes Fe4 . N92 . 2.164(5) yes Fe4 . O29 . 2.073(4) yes Fe4 . O2 . 1.981(4) yes Fe5 . O129 . 2.060(4) yes Fe5 . N17 . 2.289(5) yes Fe5 . O237 . 1.992(4) yes Fe5 . O337 . 2.022(4) yes Fe5 . O103 . 1.946(5) yes Fe5 . O3 . 1.943(4) yes Fe6 . O119 . 2.058(4) yes Fe6 . O236 . 1.984(4) yes Fe6 . O434 . 2.002(4) yes Fe6 . O13 . 1.930(4) yes Fe6 . N93 . 2.175(5) yes Fe6 . O3 . 1.973(4) yes Fe7 . O118 . 2.044(5) yes Fe7 . N16 . 2.279(5) yes Fe7 . O236 . 1.988(4) yes Fe7 . O336 . 2.011(4) yes Fe7 . O101 . 1.962(4) yes Fe7 . O7 . 1.919(4) yes Fe8 . O128 . 2.062(4) yes Fe8 . O335 . 1.963(4) yes Fe8 . O234 . 1.986(4) yes Fe8 . O11 . 1.926(4) yes Fe8 . N91 . 2.173(5) yes Fe8 . O7 . 1.985(4) yes C18 . C28 . 1.492(9) yes C18 . O118 . 1.257(7) yes C18 . O128 . 1.273(7) yes C28 . H281 . 0.959 no C28 . H282 . 0.957 no C28 . H283 . 0.976 no C19 . C29 . 1.502(8) yes C19 . O119 . 1.252(7) yes C19 . O129 . 1.256(7) yes C29 . H291 . 0.949 no C29 . H292 . 0.963 no C29 . H293 . 0.932 no N17 . C217 . 1.505(7) yes N17 . C317 . 1.479(8) yes N17 . C417 . 1.483(8) yes C217 . C227 . 1.506(9) yes C217 . H2171 . 0.964 no C217 . H2172 . 0.968 no C227 . O237 . 1.425(6) yes C227 . H2271 . 0.960 no C227 . H2272 . 0.974 no C317 . C327 . 1.524(9) yes C317 . H3171 . 0.962 no C317 . H3172 . 0.981 no C327 . O337 . 1.409(7) yes C327 . H3271 . 0.985 no C327 . H3272 . 0.962 no C417 . C427 . 1.499(11) yes C417 . H4171 . 0.974 no C417 . H4172 . 0.975 no C427 . O437 . 1.430(9) yes C427 . H4271 . 0.993 no C427 . H4272 . 0.982 no O437 . H8655 . 0.838 no N16 . C216 . 1.497(8) yes N16 . C316 . 1.493(8) yes N16 . C416 . 1.503(7) yes C216 . C226 . 1.504(9) yes C216 . H2161 . 0.964 no C216 . H2162 . 0.972 no C226 . O236 . 1.425(7) yes C226 . H2261 . 0.990 no C226 . H2262 . 0.959 no C316 . C326 . 1.521(8) yes C316 . H3161 . 0.968 no C316 . H3162 . 0.964 no C326 . O336 . 1.421(6) yes C326 . H3261 . 0.969 no C326 . H3262 . 0.998 no C416 . C426 . 1.495(10) yes C416 . H4161 . 0.967 no C416 . H4162 . 0.972 no C426 . O436 . 1.428(8) yes C426 . H4261 . 0.966 no C426 . H4262 . 0.968 no O436 . H1 . 0.838 no N15 . C215 . 1.491(8) yes N15 . C315 . 1.506(8) yes N15 . C415 . 1.487(9) yes C215 . C225 . 1.503(10) yes C215 . H2151 . 0.973 no C215 . H2152 . 0.970 no C225 . O235 . 1.420(8) yes C225 . H2251 . 0.947 no C225 . H2252 . 0.961 no C315 . C325 . 1.484(9) yes C315 . H3151 . 0.978 no C315 . H3152 . 0.968 no C325 . O335 . 1.429(7) yes C325 . H3251 . 0.986 no C325 . H3252 . 0.951 no C415 . C425 . 1.525(10) yes C415 . H4151 . 0.970 no C415 . H4152 . 0.972 no C425 . O435 . 1.431(9) yes C425 . H4251 . 0.972 no C425 . H4252 . 0.970 no O435 . H8654 . 0.839 no N14 . C214 . 1.448(8) yes N14 . C314 . 1.459(7) yes N14 . C414 . 1.457(8) yes C214 . C224 . 1.490(9) yes C214 . H2141 . 0.967 no C214 . H2142 . 0.975 no C224 . O234 . 1.424(6) yes C224 . H2241 . 0.982 no C224 . H2242 . 0.986 no C314 . C324 . 1.514(8) yes C314 . H3141 . 0.961 no C314 . H3142 . 0.977 no C324 . O334 . 1.411(7) yes C324 . H3241 . 0.968 no C324 . H3242 . 0.968 no C414 . C424 . 1.512(8) yes C414 . H4141 . 0.978 no C414 . H4142 . 0.996 no C424 . O434 . 1.423(7) yes C424 . H4241 . 0.979 no C424 . H4242 . 0.973 no O13 . C23 . 1.326(8) yes C23 . C33 . 1.402(9) yes C23 . C73 . 1.417(9) yes C33 . C43 . 1.373(10) yes C33 . H331 . 0.951 no C43 . C53 . 1.388(11) yes C43 . H431 . 0.940 no C53 . C63 . 1.378(11) yes C53 . H531 . 0.941 no C63 . C73 . 1.394(10) yes C63 . H631 . 0.934 no C73 . C83 . 1.476(10) yes C83 . N93 . 1.267(8) yes C83 . C813 . 1.496(9) yes N93 . O103 . 1.375(6) yes C813 . C823 . 1.378(13) yes C813 . C863 . 1.367(12) yes C823 . C833 . 1.406(15) yes C823 . H8231 . 0.935 no C833 . C843 . 1.377(18) yes C833 . H8331 . 0.930 no C843 . C853 . 1.316(16) yes C843 . H8431 . 0.939 no C853 . C863 . 1.383(11) yes C853 . H8531 . 0.929 no C863 . H8631 . 0.929 no O12 . C22 . 1.325(7) yes C22 . C32 . 1.401(9) yes C22 . C72 . 1.404(9) yes C32 . C42 . 1.386(9) yes C32 . H321 . 0.909 no C42 . C52 . 1.381(11) yes C42 . H421 . 0.925 no C52 . C62 . 1.382(10) yes C52 . H521 . 0.932 no C62 . C72 . 1.405(9) yes C62 . H621 . 0.924 no C72 . C82 . 1.473(9) yes C82 . N92 . 1.304(7) yes C82 . C812 . 1.497(8) yes N92 . O102 . 1.356(6) yes C812 . C822 . 1.383(10) yes C812 . C862 . 1.376(10) yes C822 . C832 . 1.375(10) yes C822 . H8221 . 0.934 no C832 . C842 . 1.372(12) yes C832 . H8321 . 0.943 no C842 . C852 . 1.376(13) yes C842 . H8421 . 0.942 no C852 . C862 . 1.390(11) yes C852 . H8521 . 0.928 no C862 . H8621 . 0.938 no O11 . C21 . 1.316(8) yes C21 . C31 . 1.422(8) yes C21 . C71 . 1.410(9) yes C31 . C41 . 1.368(10) yes C31 . H311 . 0.928 no C41 . C51 . 1.372(11) yes C41 . H411 . 0.926 no C51 . C61 . 1.372(10) yes C51 . H511 . 0.944 no C61 . C71 . 1.393(9) yes C61 . H611 . 0.930 no C71 . C81 . 1.484(8) yes C81 . N91 . 1.285(8) yes C81 . C811 . 1.498(8) yes N91 . O101 . 1.383(6) yes C811 . C821 . 1.391(9) yes C811 . C861 . 1.376(9) yes C821 . C831 . 1.372(10) yes C821 . H8211 . 0.928 no C831 . C841 . 1.382(11) yes C831 . H8311 . 0.953 no C841 . C851 . 1.388(10) yes C841 . H8411 . 0.923 no C851 . C861 . 1.387(9) yes C851 . H8511 . 0.949 no C861 . H8611 . 0.936 no O29 . C30 . 1.251(7) yes C30 . O31 . 1.260(7) yes C30 . C865 . 1.502(9) yes C865 . H8651 . 0.962 no C865 . H8652 . 0.957 no C865 . H8653 . 0.935 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 O234 . Fe1 . O334 . 104.86(16) yes O234 . Fe1 . O434 . 104.17(17) yes O334 . Fe1 . O434 . 104.96(17) yes O234 . Fe1 . O3 . 154.81(15) yes O334 . Fe1 . O3 . 98.75(15) yes O434 . Fe1 . O3 . 77.57(16) yes O234 . Fe1 . O7 . 77.05(15) yes O334 . Fe1 . O7 . 156.58(17) yes O434 . Fe1 . O7 . 96.97(16) yes O3 . Fe1 . O7 . 77.80(14) yes O234 . Fe1 . O2 . 98.12(16) yes O334 . Fe1 . O2 . 77.91(15) yes O434 . Fe1 . O2 . 155.76(15) yes O3 . Fe1 . O2 . 78.21(15) yes O7 . Fe1 . O2 . 78.71(14) yes O337 . Fe2 . O336 . 100.79(16) yes O337 . Fe2 . O235 . 102.63(18) yes O336 . Fe2 . O235 . 100.53(18) yes O337 . Fe2 . O3 . 79.18(16) yes O336 . Fe2 . O3 . 98.35(17) yes O235 . Fe2 . O3 . 160.30(16) yes O337 . Fe2 . O7 . 159.36(17) yes O336 . Fe2 . O7 . 78.69(15) yes O235 . Fe2 . O7 . 97.70(17) yes O3 . Fe2 . O7 . 80.49(15) yes O337 . Fe2 . O2 . 99.33(15) yes O336 . Fe2 . O2 . 159.35(16) yes O235 . Fe2 . O2 . 79.43(16) yes O3 . Fe2 . O2 . 80.92(15) yes O7 . Fe2 . O2 . 80.85(14) yes N15 . Fe3 . O235 . 80.70(18) yes N15 . Fe3 . O335 . 78.51(18) yes O235 . Fe3 . O335 . 94.21(16) yes N15 . Fe3 . O102 . 106.83(19) yes O235 . Fe3 . O102 . 170.40(17) yes O335 . Fe3 . O102 . 93.16(17) yes N15 . Fe3 . O31 . 82.00(19) yes O235 . Fe3 . O31 . 86.18(17) yes O335 . Fe3 . O31 . 160.18(18) yes O102 . Fe3 . O31 . 88.97(18) yes N15 . Fe3 . O2 . 160.56(17) yes O235 . Fe3 . O2 . 80.01(16) yes O335 . Fe3 . O2 . 100.57(17) yes O102 . Fe3 . O2 . 92.61(17) yes O31 . Fe3 . O2 . 99.02(17) yes O237 . Fe4 . O334 . 92.25(17) yes O237 . Fe4 . O12 . 95.93(17) yes O334 . Fe4 . O12 . 92.55(17) yes O237 . Fe4 . N92 . 173.46(19) yes O334 . Fe4 . N92 . 94.27(18) yes O12 . Fe4 . N92 . 84.36(18) yes O237 . Fe4 . O29 . 87.47(18) yes O334 . Fe4 . O29 . 175.65(16) yes O12 . Fe4 . O29 . 91.79(17) yes N92 . Fe4 . O29 . 85.99(18) yes O237 . Fe4 . O2 . 95.78(15) yes O334 . Fe4 . O2 . 79.89(16) yes O12 . Fe4 . O2 . 166.29(17) yes N92 . Fe4 . O2 . 84.82(16) yes O29 . Fe4 . O2 . 95.82(17) yes O129 . Fe5 . N17 . 82.51(17) yes O129 . Fe5 . O237 . 160.66(16) yes N17 . Fe5 . O237 . 78.70(17) yes O129 . Fe5 . O337 . 86.30(17) yes N17 . Fe5 . O337 . 79.36(18) yes O237 . Fe5 . O337 . 94.65(17) yes O129 . Fe5 . O103 . 87.88(18) yes N17 . Fe5 . O103 . 106.80(19) yes O237 . Fe5 . O103 . 93.16(18) yes O337 . Fe5 . O103 . 170.90(17) yes O129 . Fe5 . O3 . 100.19(16) yes N17 . Fe5 . O3 . 159.62(19) yes O237 . Fe5 . O3 . 99.03(16) yes O337 . Fe5 . O3 . 80.66(16) yes O103 . Fe5 . O3 . 93.52(18) yes O119 . Fe6 . O236 . 87.02(17) yes O119 . Fe6 . O434 . 176.42(17) yes O236 . Fe6 . O434 . 92.89(16) yes O119 . Fe6 . O13 . 90.45(18) yes O236 . Fe6 . O13 . 97.08(18) yes O434 . Fe6 . O13 . 93.11(18) yes O119 . Fe6 . N93 . 86.06(17) yes O236 . Fe6 . N93 . 173.04(18) yes O434 . Fe6 . N93 . 93.97(17) yes O13 . Fe6 . N93 . 83.75(19) yes O119 . Fe6 . O3 . 96.25(16) yes O236 . Fe6 . O3 . 95.66(17) yes O434 . Fe6 . O3 . 80.19(16) yes O13 . Fe6 . O3 . 165.89(17) yes N93 . Fe6 . O3 . 84.33(17) yes O118 . Fe7 . N16 . 81.61(19) yes O118 . Fe7 . O236 . 160.08(16) yes N16 . Fe7 . O236 . 79.06(18) yes O118 . Fe7 . O336 . 87.03(18) yes N16 . Fe7 . O336 . 80.74(17) yes O236 . Fe7 . O336 . 94.53(17) yes O118 . Fe7 . O101 . 88.61(19) yes N16 . Fe7 . O101 . 104.28(18) yes O236 . Fe7 . O101 . 91.52(19) yes O336 . Fe7 . O101 . 172.80(18) yes O118 . Fe7 . O7 . 99.61(17) yes N16 . Fe7 . O7 . 161.89(18) yes O236 . Fe7 . O7 . 100.25(16) yes O336 . Fe7 . O7 . 81.27(16) yes O101 . Fe7 . O7 . 93.82(16) yes O128 . Fe8 . O335 . 88.39(18) yes O128 . Fe8 . O234 . 177.43(17) yes O335 . Fe8 . O234 . 90.31(17) yes O128 . Fe8 . O11 . 90.67(17) yes O335 . Fe8 . O11 . 97.48(18) yes O234 . Fe8 . O11 . 91.69(16) yes O128 . Fe8 . N91 . 85.28(18) yes O335 . Fe8 . N91 . 173.58(18) yes O234 . Fe8 . N91 . 95.97(18) yes O11 . Fe8 . N91 . 83.67(18) yes O128 . Fe8 . O7 . 98.27(16) yes O335 . Fe8 . O7 . 94.96(16) yes O234 . Fe8 . O7 . 79.64(15) yes O11 . Fe8 . O7 . 164.87(19) yes N91 . Fe8 . O7 . 84.93(17) yes C28 . C18 . O118 . 117.8(6) yes C28 . C18 . O128 . 117.6(6) yes O118 . C18 . O128 . 124.6(6) yes C18 . C28 . H281 . 110.4 no C18 . C28 . H282 . 110.6 no H281 . C28 . H282 . 109.5 no C18 . C28 . H283 . 108.5 no H281 . C28 . H283 . 109.0 no H282 . C28 . H283 . 108.7 no Fe7 . O118 . C18 . 129.4(4) yes Fe8 . O128 . C18 . 133.1(4) yes C29 . C19 . O119 . 116.8(6) yes C29 . C19 . O129 . 117.6(6) yes O119 . C19 . O129 . 125.6(6) yes C19 . C29 . H291 . 110.8 no C19 . C29 . H292 . 112.1 no H291 . C29 . H292 . 107.0 no C19 . C29 . H293 . 110.9 no H291 . C29 . H293 . 108.3 no H292 . C29 . H293 . 107.6 no Fe6 . O119 . C19 . 135.9(4) yes Fe5 . O129 . C19 . 126.3(4) yes Fe5 . N17 . C217 . 106.2(4) yes Fe5 . N17 . C317 . 102.5(3) yes C217 . N17 . C317 . 110.9(5) yes Fe5 . N17 . C417 . 117.8(4) yes C217 . N17 . C417 . 110.8(5) yes C317 . N17 . C417 . 108.3(5) yes N17 . C217 . C227 . 108.4(5) yes N17 . C217 . H2171 . 107.8 no C227 . C217 . H2171 . 110.2 no N17 . C217 . H2172 . 110.6 no C227 . C217 . H2172 . 111.9 no H2171 . C217 . H2172 . 107.8 no C217 . C227 . O237 . 108.2(5) yes C217 . C227 . H2271 . 107.5 no O237 . C227 . H2271 . 109.0 no C217 . C227 . H2272 . 111.6 no O237 . C227 . H2272 . 110.0 no H2271 . C227 . H2272 . 110.5 no C227 . O237 . Fe5 . 111.9(3) yes C227 . O237 . Fe4 . 119.1(3) yes Fe5 . O237 . Fe4 . 128.39(19) yes N17 . C317 . C327 . 112.3(5) yes N17 . C317 . H3171 . 111.2 no C327 . C317 . H3171 . 110.5 no N17 . C317 . H3172 . 107.3 no C327 . C317 . H3172 . 107.6 no H3171 . C317 . H3172 . 107.6 no C317 . C327 . O337 . 107.5(5) yes C317 . C327 . H3271 . 110.4 no O337 . C327 . H3271 . 110.4 no C317 . C327 . H3272 . 112.5 no O337 . C327 . H3272 . 109.4 no H3271 . C327 . H3272 . 106.6 no C327 . O337 . Fe5 . 118.4(4) yes C327 . O337 . Fe2 . 135.8(4) yes Fe5 . O337 . Fe2 . 99.90(18) yes N17 . C417 . C427 . 115.0(6) yes N17 . C417 . H4171 . 108.3 no C427 . C417 . H4171 . 110.1 no N17 . C417 . H4172 . 104.6 no C427 . C417 . H4172 . 109.1 no H4171 . C417 . H4172 . 109.5 no C417 . C427 . O437 . 106.4(7) yes C417 . C427 . H4271 . 109.2 no O437 . C427 . H4271 . 108.4 no C417 . C427 . H4272 . 114.0 no O437 . C427 . H4272 . 110.5 no H4271 . C427 . H4272 . 108.2 no C427 . O437 . H8655 . 86.8 no Fe7 . N16 . C216 . 105.8(3) yes Fe7 . N16 . C316 . 101.5(4) yes C216 . N16 . C316 . 110.7(5) yes Fe7 . N16 . C416 . 120.2(4) yes C216 . N16 . C416 . 111.6(5) yes C316 . N16 . C416 . 106.4(5) yes N16 . C216 . C226 . 110.1(5) yes N16 . C216 . H2161 . 107.4 no C226 . C216 . H2161 . 110.7 no N16 . C216 . H2162 . 108.7 no C226 . C216 . H2162 . 110.5 no H2161 . C216 . H2162 . 109.4 no C216 . C226 . O236 . 107.7(5) yes C216 . C226 . H2261 . 108.7 no O236 . C226 . H2261 . 108.2 no C216 . C226 . H2262 . 111.5 no O236 . C226 . H2262 . 111.7 no H2261 . C226 . H2262 . 108.9 no C226 . O236 . Fe7 . 112.5(4) yes C226 . O236 . Fe6 . 120.5(4) yes Fe7 . O236 . Fe6 . 126.8(2) yes N16 . C316 . C326 . 112.5(5) yes N16 . C316 . H3161 . 107.8 no C326 . C316 . H3161 . 110.7 no N16 . C316 . H3162 . 106.9 no C326 . C316 . H3162 . 110.2 no H3161 . C316 . H3162 . 108.7 no C316 . C326 . O336 . 107.5(5) yes C316 . C326 . H3261 . 111.0 no O336 . C326 . H3261 . 110.3 no C316 . C326 . H3262 . 111.5 no O336 . C326 . H3262 . 107.8 no H3261 . C326 . H3262 . 108.6 no C326 . O336 . Fe7 . 117.0(3) yes C326 . O336 . Fe2 . 137.1(3) yes Fe7 . O336 . Fe2 . 100.26(18) yes N16 . C416 . C426 . 117.5(6) yes N16 . C416 . H4161 . 107.8 no C426 . C416 . H4161 . 108.9 no N16 . C416 . H4162 . 106.7 no C426 . C416 . H4162 . 108.1 no H4161 . C416 . H4162 . 107.4 no C416 . C426 . O436 . 114.2(6) yes C416 . C426 . H4261 . 107.9 no O436 . C426 . H4261 . 110.0 no C416 . C426 . H4262 . 107.6 no O436 . C426 . H4262 . 107.9 no H4261 . C426 . H4262 . 109.2 no C426 . O436 . H1 . 106.2 no Fe3 . N15 . C215 . 102.6(4) yes Fe3 . N15 . C315 . 106.6(4) yes C215 . N15 . C315 . 111.3(5) yes Fe3 . N15 . C415 . 117.8(4) yes C215 . N15 . C415 . 107.9(5) yes C315 . N15 . C415 . 110.4(5) yes N15 . C215 . C225 . 111.6(6) yes N15 . C215 . H2151 . 109.4 no C225 . C215 . H2151 . 107.4 no N15 . C215 . H2152 . 110.0 no C225 . C215 . H2152 . 109.5 no H2151 . C215 . H2152 . 108.9 no C215 . C225 . O235 . 108.9(5) yes C215 . C225 . H2251 . 110.1 no O235 . C225 . H2251 . 110.5 no C215 . C225 . H2252 . 108.7 no O235 . C225 . H2252 . 108.4 no H2251 . C225 . H2252 . 110.1 no C225 . O235 . Fe3 . 114.6(4) yes C225 . O235 . Fe2 . 137.7(4) yes Fe3 . O235 . Fe2 . 100.09(18) yes N15 . C315 . C325 . 109.3(5) yes N15 . C315 . H3151 . 110.3 no C325 . C315 . H3151 . 108.6 no N15 . C315 . H3152 . 110.8 no C325 . C315 . H3152 . 109.6 no H3151 . C315 . H3152 . 108.2 no C315 . C325 . O335 . 108.1(5) yes C315 . C325 . H3251 . 108.1 no O335 . C325 . H3251 . 108.7 no C315 . C325 . H3252 . 111.6 no O335 . C325 . H3252 . 109.2 no H3251 . C325 . H3252 . 111.1 no C325 . O335 . Fe3 . 110.9(4) yes C325 . O335 . Fe8 . 120.7(4) yes Fe3 . O335 . Fe8 . 128.3(2) yes N15 . C415 . C425 . 113.7(6) yes N15 . C415 . H4151 . 109.0 no C425 . C415 . H4151 . 108.9 no N15 . C415 . H4152 . 106.7 no C425 . C415 . H4152 . 106.9 no H4151 . C415 . H4152 . 111.7 no C415 . C425 . O435 . 106.8(6) yes C415 . C425 . H4251 . 110.6 no O435 . C425 . H4251 . 110.1 no C415 . C425 . H4252 . 111.4 no O435 . C425 . H4252 . 108.3 no H4251 . C425 . H4252 . 109.6 no C425 . O435 . H8654 . 110.8 no C214 . N14 . C314 . 117.4(5) yes C214 . N14 . C414 . 118.1(5) yes C314 . N14 . C414 . 118.6(5) yes N14 . C214 . C224 . 110.3(5) yes N14 . C214 . H2141 . 110.1 no C224 . C214 . H2141 . 110.3 no N14 . C214 . H2142 . 109.9 no C224 . C214 . H2142 . 108.5 no H2141 . C214 . H2142 . 107.7 no C214 . C224 . O234 . 108.4(5) yes C214 . C224 . H2241 . 109.8 no O234 . C224 . H2241 . 112.4 no C214 . C224 . H2242 . 107.9 no O234 . C224 . H2242 . 108.9 no H2241 . C224 . H2242 . 109.4 no C224 . O234 . Fe8 . 130.2(3) yes C224 . O234 . Fe1 . 122.3(3) yes Fe8 . O234 . Fe1 . 105.22(17) yes N14 . C314 . C324 . 110.5(5) yes N14 . C314 . H3141 . 110.0 no C324 . C314 . H3141 . 107.6 no N14 . C314 . H3142 . 111.3 no C324 . C314 . H3142 . 107.0 no H3141 . C314 . H3142 . 110.4 no C314 . C324 . O334 . 109.4(5) yes C314 . C324 . H3241 . 108.7 no O334 . C324 . H3241 . 109.5 no C314 . C324 . H3242 . 110.5 no O334 . C324 . H3242 . 109.0 no H3241 . C324 . H3242 . 109.7 no C324 . O334 . Fe4 . 132.0(3) yes C324 . O334 . Fe1 . 122.3(3) yes Fe4 . O334 . Fe1 . 103.63(18) yes N14 . C414 . C424 . 110.9(5) yes N14 . C414 . H4141 . 109.1 no C424 . C414 . H4141 . 108.8 no N14 . C414 . H4142 . 108.9 no C424 . C414 . H4142 . 109.2 no H4141 . C414 . H4142 . 109.8 no C414 . C424 . O434 . 109.1(5) yes C414 . C424 . H4241 . 109.8 no O434 . C424 . H4241 . 109.5 no C414 . C424 . H4242 . 110.4 no O434 . C424 . H4242 . 109.3 no H4241 . C424 . H4242 . 108.7 no C424 . O434 . Fe6 . 132.0(3) yes C424 . O434 . Fe1 . 121.1(4) yes Fe6 . O434 . Fe1 . 104.14(18) yes Fe6 . O13 . C23 . 124.3(4) yes O13 . C23 . C33 . 119.0(6) yes O13 . C23 . C73 . 123.0(6) yes C33 . C23 . C73 . 118.0(6) yes C23 . C33 . C43 . 122.3(7) yes C23 . C33 . H331 . 118.4 no C43 . C33 . H331 . 119.3 no C33 . C43 . C53 . 119.8(7) yes C33 . C43 . H431 . 119.8 no C53 . C43 . H431 . 120.3 no C43 . C53 . C63 . 118.8(8) yes C43 . C53 . H531 . 121.8 no C63 . C53 . H531 . 119.4 no C53 . C63 . C73 . 122.9(7) yes C53 . C63 . H631 . 118.1 no C73 . C63 . H631 . 119.0 no C23 . C73 . C63 . 118.1(7) yes C23 . C73 . C83 . 122.4(6) yes C63 . C73 . C83 . 119.5(6) yes C73 . C83 . N93 . 120.2(6) yes C73 . C83 . C813 . 117.6(6) yes N93 . C83 . C813 . 122.2(6) yes Fe6 . N93 . C83 . 127.0(4) yes Fe6 . N93 . O103 . 115.1(4) yes C83 . N93 . O103 . 117.8(5) yes N93 . O103 . Fe5 . 116.8(3) yes C83 . C813 . C823 . 118.8(8) yes C83 . C813 . C863 . 122.4(8) yes C823 . C813 . C863 . 118.0(8) yes C813 . C823 . C833 . 119.9(12) yes C813 . C823 . H8231 . 116.9 no C833 . C823 . H8231 . 123.1 no C823 . C833 . C843 . 118.5(13) yes C823 . C833 . H8331 . 119.6 no C843 . C833 . H8331 . 121.7 no C833 . C843 . C853 . 122.1(11) yes C833 . C843 . H8431 . 120.1 no C853 . C843 . H8431 . 117.6 no C843 . C853 . C863 . 119.1(11) yes C843 . C853 . H8531 . 122.1 no C863 . C853 . H8531 . 118.4 no C853 . C863 . C813 . 122.2(10) yes C853 . C863 . H8631 . 119.7 no C813 . C863 . H8631 . 118.1 no Fe4 . O12 . C22 . 129.7(4) yes O12 . C22 . C32 . 118.3(6) yes O12 . C22 . C72 . 123.0(6) yes C32 . C22 . C72 . 118.7(6) yes C22 . C32 . C42 . 121.0(7) yes C22 . C32 . H321 . 119.1 no C42 . C32 . H321 . 119.9 no C32 . C42 . C52 . 120.5(7) yes C32 . C42 . H421 . 119.8 no C52 . C42 . H421 . 119.4 no C42 . C52 . C62 . 119.2(7) yes C42 . C52 . H521 . 121.9 no C62 . C52 . H521 . 118.9 no C52 . C62 . C72 . 121.5(7) yes C52 . C62 . H621 . 119.5 no C72 . C62 . H621 . 118.9 no C62 . C72 . C22 . 119.0(6) yes C62 . C72 . C82 . 117.7(6) yes C22 . C72 . C82 . 123.3(6) yes C72 . C82 . N92 . 121.0(5) yes C72 . C82 . C812 . 120.8(5) yes N92 . C82 . C812 . 118.2(5) yes Fe4 . N92 . C82 . 127.8(4) yes Fe4 . N92 . O102 . 116.9(3) yes C82 . N92 . O102 . 115.3(5) yes N92 . O102 . Fe3 . 117.7(3) yes C82 . C812 . C822 . 121.2(6) yes C82 . C812 . C862 . 118.8(7) yes C822 . C812 . C862 . 119.9(7) yes C812 . C822 . C832 . 120.6(7) yes C812 . C822 . H8221 . 118.5 no C832 . C822 . H8221 . 120.9 no C822 . C832 . C842 . 119.2(8) yes C822 . C832 . H8321 . 119.9 no C842 . C832 . H8321 . 120.9 no C832 . C842 . C852 . 121.1(8) yes C832 . C842 . H8421 . 120.3 no C852 . C842 . H8421 . 118.6 no C842 . C852 . C862 . 119.6(8) yes C842 . C852 . H8521 . 120.8 no C862 . C852 . H8521 . 119.6 no C852 . C862 . C812 . 119.6(8) yes C852 . C862 . H8621 . 121.2 no C812 . C862 . H8621 . 119.1 no Fe8 . O11 . C21 . 128.7(4) yes O11 . C21 . C31 . 117.6(6) yes O11 . C21 . C71 . 124.9(5) yes C31 . C21 . C71 . 117.5(6) yes C21 . C31 . C41 . 120.8(7) yes C21 . C31 . H311 . 119.2 no C41 . C31 . H311 . 120.0 no C31 . C41 . C51 . 121.3(7) yes C31 . C41 . H411 . 117.9 no C51 . C41 . H411 . 120.7 no C41 . C51 . C61 . 119.2(7) yes C41 . C51 . H511 . 119.3 no C61 . C51 . H511 . 121.5 no C51 . C61 . C71 . 121.7(7) yes C51 . C61 . H611 . 120.4 no C71 . C61 . H611 . 117.9 no C21 . C71 . C61 . 119.5(6) yes C21 . C71 . C81 . 121.5(6) yes C61 . C71 . C81 . 119.0(6) yes C71 . C81 . N91 . 120.2(6) yes C71 . C81 . C811 . 117.9(5) yes N91 . C81 . C811 . 122.0(5) yes Fe8 . N91 . C81 . 129.0(4) yes Fe8 . N91 . O101 . 115.5(4) yes C81 . N91 . O101 . 115.4(5) yes N91 . O101 . Fe7 . 116.4(3) yes C81 . C811 . C821 . 118.6(6) yes C81 . C811 . C861 . 122.4(6) yes C821 . C811 . C861 . 118.9(6) yes C811 . C821 . C831 . 120.1(7) yes C811 . C821 . H8211 . 118.6 no C831 . C821 . H8211 . 121.3 no C821 . C831 . C841 . 120.9(7) yes C821 . C831 . H8311 . 119.6 no C841 . C831 . H8311 . 119.4 no C831 . C841 . C851 . 119.5(7) yes C831 . C841 . H8411 . 120.6 no C851 . C841 . H8411 . 119.9 no C841 . C851 . C861 . 119.3(7) yes C841 . C851 . H8511 . 120.4 no C861 . C851 . H8511 . 120.3 no C851 . C861 . C811 . 121.3(7) yes C851 . C861 . H8611 . 118.8 no C811 . C861 . H8611 . 119.8 no Fe1 . O3 . Fe2 . 84.71(14) yes Fe1 . O3 . Fe6 . 97.60(16) yes Fe2 . O3 . Fe6 . 136.09(19) yes Fe1 . O3 . Fe5 . 131.27(18) yes Fe2 . O3 . Fe5 . 98.30(17) yes Fe6 . O3 . Fe5 . 111.63(19) yes Fe1 . O7 . Fe2 . 84.27(13) yes Fe1 . O7 . Fe8 . 97.70(16) yes Fe2 . O7 . Fe8 . 136.3(2) yes Fe1 . O7 . Fe7 . 132.3(2) yes Fe2 . O7 . Fe7 . 97.91(16) yes Fe8 . O7 . Fe7 . 111.43(17) yes Fe4 . O29 . C30 . 133.5(4) yes O29 . C30 . O31 . 125.7(6) yes O29 . C30 . C865 . 119.0(6) yes O31 . C30 . C865 . 115.4(6) yes Fe3 . O31 . C30 . 129.3(4) yes C30 . C865 . H8651 . 108.5 no C30 . C865 . H8652 . 107.9 no H8651 . C865 . H8652 . 109.2 no C30 . C865 . H8653 . 109.9 no H8651 . C865 . H8653 . 111.2 no H8652 . C865 . H8653 . 109.9 no Fe1 . O2 . Fe2 . 85.46(14) yes Fe1 . O2 . Fe4 . 97.85(17) yes Fe2 . O2 . Fe4 . 135.20(19) yes Fe1 . O2 . Fe3 . 129.73(19) yes Fe2 . O2 . Fe3 . 98.49(16) yes Fe4 . O2 . Fe3 . 112.25(18) yes