# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dongfeng Li' _publ_contact_author_email dfli@mail.ccnu.edu.cn loop_ _publ_author_name 'Guiling Wu' 'Fusheng Mei' 'Fang Han' 'Jianmin Zhang' 'Shemin Lan' ; Xuegang Song ; 'Dongfeng Li' # Attachment '- cifs.cif.txt' # Complex 1 data_Fe(medtb).(ClO4)2.0.5MeOH.0.5MeCN _database_code_depnum_ccdc_archive 'CCDC 804325' #TrackingRef '- cifs.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.5 H43.5 Cl2 Fe N10.5 O8.5' _chemical_formula_weight 928.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3381(7) _cell_length_b 15.3811(7) _cell_length_c 20.1461(9) _cell_angle_alpha 73.2640(10) _cell_angle_beta 69.9250(10) _cell_angle_gamma 83.9370(10) _cell_volume 4274.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4051 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 19.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _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 34832 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1051 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14964 _reflns_number_gt 9096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1098P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14964 _refine_ls_number_parameters 1302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1581 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.2493 _refine_ls_wR_factor_gt 0.2159 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.74867(6) 0.72598(5) 0.83535(4) 0.0403(3) Uani 1 1 d . . . N1 N 0.7735(4) 0.6159(3) 0.7747(3) 0.0477(14) Uani 1 1 d . . . N2 N 0.7201(4) 0.8055(3) 0.7299(3) 0.0459(13) Uani 1 1 d . . . N3 N 0.6878(3) 0.8490(3) 0.8587(3) 0.0398(12) Uani 1 1 d . . . N4 N 0.6020(4) 0.9713(3) 0.8310(3) 0.0542(15) Uani 1 1 d . . . N5 N 0.6149(4) 0.6590(3) 0.8812(3) 0.0448(13) Uani 1 1 d . . . N6 N 0.5274(4) 0.5490(3) 0.8871(3) 0.0500(14) Uani 1 1 d . . . N7 N 0.8066(4) 0.6129(3) 0.8985(3) 0.0496(14) Uani 1 1 d . . . N8 N 0.8984(5) 0.4909(4) 0.8980(4) 0.0713(18) Uani 1 1 d . . . N9 N 0.8808(4) 0.7885(3) 0.7691(3) 0.0448(13) Uani 1 1 d . . . N10 N 0.9651(4) 0.8812(3) 0.6653(3) 0.0479(14) Uani 1 1 d . . . C1 C 0.8604(5) 0.5711(5) 0.7812(4) 0.0597(19) Uani 1 1 d . . . H1A H 0.9130 0.6084 0.7473 0.072 Uiso 1 1 calc R . . H1B H 0.8666 0.5130 0.7701 0.072 Uiso 1 1 calc R . . C2 C 0.7808(5) 0.6645(5) 0.6972(3) 0.060(2) Uani 1 1 d . . . H2A H 0.7738 0.6215 0.6724 0.072 Uiso 1 1 calc R . . H2B H 0.8416 0.6919 0.6715 0.072 Uiso 1 1 calc R . . C3 C 0.7064(5) 0.7374(5) 0.6954(3) 0.0570(19) Uani 1 1 d . . . H3A H 0.7099 0.7666 0.6450 0.068 Uiso 1 1 calc R . . H3B H 0.6456 0.7103 0.7216 0.068 Uiso 1 1 calc R . . C4 C 0.6359(5) 0.8601(4) 0.7538(3) 0.0503(17) Uani 1 1 d . . . H4A H 0.5810 0.8231 0.7709 0.060 Uiso 1 1 calc R . . H4B H 0.6318 0.9107 0.7131 0.060 Uiso 1 1 calc R . . C5 C 0.6422(4) 0.8940(4) 0.8142(4) 0.0468(16) Uani 1 1 d . . . C6 C 0.5459(6) 1.0365(5) 0.7935(5) 0.087(3) Uani 1 1 d . . . H6A H 0.5622 1.0328 0.7439 0.131 Uiso 1 1 calc R . . H6B H 0.5573 1.0968 0.7932 0.131 Uiso 1 1 calc R . . H6C H 0.4813 1.0226 0.8187 0.131 Uiso 1 1 calc R . . C7 C 0.6246(5) 0.9783(4) 0.8908(4) 0.0488(16) Uani 1 1 d . . . C8 C 0.6040(6) 1.0410(5) 0.9299(4) 0.070(2) Uani 1 1 d . . . H8 H 0.5677 1.0919 0.9188 0.084 Uiso 1 1 calc R . . C9 C 0.6395(6) 1.0258(5) 0.9872(5) 0.077(2) Uani 1 1 d . . . H9 H 0.6280 1.0681 1.0143 0.092 Uiso 1 1 calc R . . C10 C 0.6913(6) 0.9494(5) 1.0045(4) 0.065(2) Uani 1 1 d . . . H10 H 0.7126 0.9404 1.0440 0.079 Uiso 1 1 calc R . . C11 C 0.7128(5) 0.8854(4) 0.9646(4) 0.0538(18) Uani 1 1 d . . . H11 H 0.7491 0.8346 0.9760 0.065 Uiso 1 1 calc R . . C12 C 0.6785(4) 0.9002(4) 0.9082(3) 0.0435(15) Uani 1 1 d . . . C13 C 0.5259(5) 0.6679(4) 0.9290(3) 0.0432(16) Uani 1 1 d . . . C14 C 0.4888(5) 0.7284(4) 0.9706(3) 0.0501(17) Uani 1 1 d . . . H14 H 0.5246 0.7747 0.9689 0.060 Uiso 1 1 calc R . . C15 C 0.3973(5) 0.7181(5) 1.0147(4) 0.0600(19) Uani 1 1 d . . . H15 H 0.3705 0.7589 1.0424 0.072 Uiso 1 1 calc R . . C16 C 0.3439(6) 0.6476(5) 1.0186(4) 0.072(2) Uani 1 1 d . . . H16 H 0.2827 0.6419 1.0499 0.086 Uiso 1 1 calc R . . C17 C 0.3786(5) 0.5863(5) 0.9778(4) 0.061(2) Uani 1 1 d . . . H17 H 0.3424 0.5403 0.9795 0.074 Uiso 1 1 calc R . . C18 C 0.4710(5) 0.5972(4) 0.9340(3) 0.0472(17) Uani 1 1 d . . . C19 C 0.4999(6) 0.4694(4) 0.8726(4) 0.069(2) Uani 1 1 d . . . H19A H 0.5538 0.4428 0.8439 0.104 Uiso 1 1 calc R . . H19B H 0.4566 0.4879 0.8461 0.104 Uiso 1 1 calc R . . H19C H 0.4712 0.4256 0.9183 0.104 Uiso 1 1 calc R . . C20 C 0.6116(5) 0.5872(4) 0.8579(3) 0.0471(17) Uani 1 1 d . . . C21 C 0.6957(5) 0.5516(4) 0.8079(4) 0.0572(19) Uani 1 1 d . . . H21A H 0.7154 0.4949 0.8356 0.069 Uiso 1 1 calc R . . H21B H 0.6794 0.5389 0.7692 0.069 Uiso 1 1 calc R . . C22 C 0.8564(5) 0.5579(4) 0.8605(4) 0.0533(18) Uani 1 1 d . . . C23 C 0.9634(7) 0.4203(6) 0.8717(5) 0.108(4) Uani 1 1 d . . . H23A H 0.9493 0.4069 0.8328 0.162 Uiso 1 1 calc R . . H23B H 0.9571 0.3663 0.9114 0.162 Uiso 1 1 calc R . . H23C H 1.0259 0.4420 0.8538 0.162 Uiso 1 1 calc R . . C24 C 0.8718(6) 0.5033(5) 0.9677(4) 0.069(2) Uani 1 1 d . . . C25 C 0.8876(8) 0.4517(6) 1.0324(6) 0.102(3) Uani 1 1 d . . . H25 H 0.9243 0.3995 1.0330 0.123 Uiso 1 1 calc R . . C26 C 0.8478(9) 0.4802(6) 1.0937(5) 0.110(4) Uani 1 1 d . . . H26 H 0.8596 0.4485 1.1366 0.132 Uiso 1 1 calc R . . C27 C 0.8145(5) 0.5792(4) 0.9680(4) 0.0540(18) Uani 1 1 d . . . C28 C 0.7726(6) 0.6069(5) 1.0305(4) 0.066(2) Uani 1 1 d . . . H28 H 0.7343 0.6579 1.0307 0.079 Uiso 1 1 calc R . . C29 C 0.7903(7) 0.5549(6) 1.0938(4) 0.088(3) Uani 1 1 d . . . H29 H 0.7622 0.5713 1.1374 0.106 Uiso 1 1 calc R . . C30 C 0.9705(5) 0.7889(4) 0.7713(3) 0.0438(16) Uani 1 1 d . . . C31 C 1.0108(6) 0.7456(5) 0.8243(4) 0.062(2) Uani 1 1 d . . . H31 H 0.9762 0.7082 0.8691 0.074 Uiso 1 1 calc R . . C32 C 1.1027(6) 0.7596(5) 0.8084(5) 0.071(2) Uani 1 1 d . . . H32 H 1.1307 0.7317 0.8436 0.086 Uiso 1 1 calc R . . C33 C 1.1559(6) 0.8138(6) 0.7421(5) 0.077(2) Uani 1 1 d . . . H33 H 1.2187 0.8204 0.7336 0.093 Uiso 1 1 calc R . . C34 C 1.1189(6) 0.8583(5) 0.6880(5) 0.066(2) Uani 1 1 d . . . H34 H 1.1548 0.8942 0.6429 0.080 Uiso 1 1 calc R . . C35 C 1.0245(5) 0.8462(4) 0.7051(4) 0.0451(16) Uani 1 1 d . . . C36 C 0.9913(6) 0.9457(4) 0.5920(4) 0.066(2) Uani 1 1 d . . . H36A H 0.9430 0.9486 0.5711 0.099 Uiso 1 1 calc R . . H36B H 1.0481 0.9259 0.5610 0.099 Uiso 1 1 calc R . . H36C H 0.9997 1.0048 0.5959 0.099 Uiso 1 1 calc R . . C37 C 0.8829(5) 0.8438(4) 0.7051(3) 0.0443(16) Uani 1 1 d . . . C38 C 0.7991(5) 0.8658(4) 0.6814(3) 0.0564(19) Uani 1 1 d . . . H38A H 0.7805 0.9282 0.6809 0.068 Uiso 1 1 calc R . . H38B H 0.8149 0.8607 0.6317 0.068 Uiso 1 1 calc R . . Fe2 Fe 0.25227(7) 0.19450(6) 0.70452(5) 0.0462(3) Uani 1 1 d . . . N11 N 0.1450(4) 0.1622(3) 0.6598(3) 0.0485(14) Uani 1 1 d . . . N12 N 0.3410(4) 0.1972(4) 0.5854(3) 0.0569(15) Uani 1 1 d . . . N13 N 0.3809(4) 0.2489(4) 0.6900(3) 0.0578(15) Uani 1 1 d . . . N14 N 0.5118(5) 0.3150(5) 0.6151(4) 0.095(2) Uani 1 1 d . . . N15 N 0.1914(4) 0.3246(4) 0.6764(3) 0.0542(14) Uani 1 1 d . . . N16 N 0.0770(4) 0.4071(4) 0.6439(3) 0.0613(16) Uani 1 1 d . . . N17 N 0.1323(4) 0.1526(3) 0.7994(3) 0.0448(13) Uani 1 1 d . . . N18 N 0.0000(4) 0.0747(4) 0.8503(3) 0.0602(16) Uani 1 1 d . . . N19 N 0.3122(4) 0.0592(3) 0.7161(3) 0.0470(13) Uani 1 1 d . . . N20 N 0.4039(4) -0.0420(4) 0.6643(3) 0.0523(14) Uani 1 1 d . . . C39 C 0.0917(5) 0.0864(5) 0.7172(3) 0.0548(18) Uani 1 1 d . . . H39A H 0.1264 0.0302 0.7152 0.066 Uiso 1 1 calc R . . H39B H 0.0334 0.0809 0.7098 0.066 Uiso 1 1 calc R . . C40 C 0.1966(5) 0.1382(5) 0.5903(3) 0.0581(19) Uani 1 1 d . . . H40A H 0.1549 0.1393 0.5631 0.070 Uiso 1 1 calc R . . H40B H 0.2225 0.0774 0.6008 0.070 Uiso 1 1 calc R . . C41 C 0.2735(5) 0.2058(5) 0.5453(3) 0.065(2) Uani 1 1 d . . . H41A H 0.3047 0.1942 0.4978 0.078 Uiso 1 1 calc R . . H41B H 0.2480 0.2669 0.5373 0.078 Uiso 1 1 calc R . . C42 C 0.3995(6) 0.2791(6) 0.5594(4) 0.076(2) Uani 1 1 d . . . H42A H 0.3638 0.3334 0.5465 0.092 Uiso 1 1 calc R . . H42B H 0.4523 0.2758 0.5165 0.092 Uiso 1 1 calc R . . C43 C 0.4316(6) 0.2813(5) 0.6212(4) 0.069(2) Uani 1 1 d . . . C44 C 0.5829(9) 0.3598(9) 0.5445(7) 0.167(6) Uani 1 1 d . . . H44A H 0.6335 0.3183 0.5327 0.250 Uiso 1 1 calc R . . H44B H 0.6055 0.4128 0.5492 0.250 Uiso 1 1 calc R . . H44C H 0.5556 0.3770 0.5062 0.250 Uiso 1 1 calc R . . C45 C 0.5128(7) 0.3047(6) 0.6856(5) 0.079(2) Uani 1 1 d . . . C46 C 0.5790(7) 0.3257(6) 0.7114(7) 0.098(3) Uani 1 1 d . . . H46 H 0.6338 0.3549 0.6794 0.118 Uiso 1 1 calc R . . C47 C 0.5601(8) 0.3018(7) 0.7854(7) 0.098(3) Uani 1 1 d . . . H47 H 0.6039 0.3128 0.8045 0.118 Uiso 1 1 calc R . . C48 C 0.4771(8) 0.2615(6) 0.8326(6) 0.089(3) Uani 1 1 d . . . H48 H 0.4652 0.2482 0.8829 0.107 Uiso 1 1 calc R . . C49 C 0.4101(6) 0.2400(5) 0.8070(4) 0.067(2) Uani 1 1 d . . . H49 H 0.3547 0.2118 0.8388 0.080 Uiso 1 1 calc R . . C50 C 0.4312(6) 0.2630(5) 0.7321(4) 0.0592(19) Uani 1 1 d . . . C51 C 0.1966(6) 0.4141(5) 0.6796(4) 0.063(2) Uani 1 1 d . . . C52 C 0.2597(6) 0.4516(5) 0.6986(5) 0.081(3) Uani 1 1 d . . . H52 H 0.3067 0.4174 0.7134 0.097 Uiso 1 1 calc R . . C53 C 0.2481(8) 0.5446(6) 0.6941(6) 0.100(3) Uani 1 1 d . . . H53 H 0.2897 0.5732 0.7052 0.120 Uiso 1 1 calc R . . C54 C 0.1761(9) 0.5954(7) 0.6735(6) 0.116(4) Uani 1 1 d . . . H54 H 0.1700 0.6566 0.6722 0.139 Uiso 1 1 calc R . . C55 C 0.1143(7) 0.5565(6) 0.6552(5) 0.095(3) Uani 1 1 d . . . H55 H 0.0666 0.5902 0.6409 0.115 Uiso 1 1 calc R . . C56 C 0.1259(6) 0.4646(5) 0.6589(4) 0.067(2) Uani 1 1 d . . . C57 C -0.0040(6) 0.4316(6) 0.6206(5) 0.088(3) Uani 1 1 d . . . H57A H -0.0441 0.4702 0.6483 0.133 Uiso 1 1 calc R . . H57B H -0.0367 0.3776 0.6287 0.133 Uiso 1 1 calc R . . H57C H 0.0153 0.4631 0.5693 0.133 Uiso 1 1 calc R . . C58 C 0.1178(5) 0.3250(5) 0.6558(4) 0.0545(18) Uani 1 1 d . . . C59 C 0.0839(5) 0.2427(5) 0.6476(4) 0.0609(19) Uani 1 1 d . . . H59A H 0.0219 0.2288 0.6824 0.073 Uiso 1 1 calc R . . H59B H 0.0801 0.2554 0.5986 0.073 Uiso 1 1 calc R . . C60 C 0.0933(5) 0.1586(4) 0.8719(3) 0.0475(16) Uani 1 1 d . . . C61 C 0.1209(5) 0.2051(5) 0.9098(4) 0.0601(19) Uani 1 1 d . . . H61 H 0.1756 0.2381 0.8887 0.072 Uiso 1 1 calc R . . C62 C 0.0637(6) 0.2009(6) 0.9810(4) 0.069(2) Uani 1 1 d . . . H62 H 0.0808 0.2316 1.0082 0.083 Uiso 1 1 calc R . . C63 C -0.0166(7) 0.1529(6) 1.0121(4) 0.081(3) Uani 1 1 d . . . H63 H -0.0529 0.1519 1.0600 0.097 Uiso 1 1 calc R . . C64 C -0.0460(6) 0.1059(6) 0.9753(4) 0.079(2) Uani 1 1 d . . . H64 H -0.1005 0.0726 0.9970 0.094 Uiso 1 1 calc R . . C65 C 0.0106(5) 0.1111(5) 0.9040(4) 0.0566(18) Uani 1 1 d . . . C66 C -0.0795(5) 0.0212(5) 0.8592(5) 0.080(3) Uani 1 1 d . . . H66A H -0.1237 0.0608 0.8409 0.121 Uiso 1 1 calc R . . H66B H -0.1084 -0.0084 0.9102 0.121 Uiso 1 1 calc R . . H66C H -0.0583 -0.0235 0.8322 0.121 Uiso 1 1 calc R . . C67 C 0.0734(5) 0.1039(4) 0.7899(3) 0.0495(17) Uani 1 1 d . . . C68 C 0.3087(4) -0.0215(4) 0.7705(3) 0.0467(16) Uani 1 1 d . . . C69 C 0.2620(5) -0.0462(5) 0.8453(4) 0.0563(18) Uani 1 1 d . . . H69 H 0.2233 -0.0048 0.8678 0.068 Uiso 1 1 calc R . . C70 C 0.2735(6) -0.1325(5) 0.8859(4) 0.072(2) Uani 1 1 d . . . H70 H 0.2439 -0.1496 0.9364 0.086 Uiso 1 1 calc R . . C71 C 0.3303(6) -0.1945(6) 0.8507(5) 0.077(2) Uani 1 1 d . . . H71 H 0.3358 -0.2533 0.8786 0.092 Uiso 1 1 calc R . . C72 C 0.3779(6) -0.1727(5) 0.7773(5) 0.073(2) Uani 1 1 d . . . H72 H 0.4160 -0.2147 0.7551 0.088 Uiso 1 1 calc R . . C73 C 0.3669(4) -0.0860(5) 0.7378(4) 0.0489(16) Uani 1 1 d . . . C74 C 0.4660(5) -0.0844(6) 0.6087(4) 0.083(3) Uani 1 1 d . . . H74A H 0.4301 -0.1085 0.5874 0.125 Uiso 1 1 calc R . . H74B H 0.5004 -0.1326 0.6312 0.125 Uiso 1 1 calc R . . H74C H 0.5083 -0.0399 0.5711 0.125 Uiso 1 1 calc R . . C75 C 0.3697(4) 0.0434(5) 0.6544(3) 0.0488(16) Uani 1 1 d . . . C76 C 0.3984(5) 0.1149(5) 0.5829(3) 0.063(2) Uani 1 1 d . . . H76A H 0.4628 0.1302 0.5706 0.076 Uiso 1 1 calc R . . H76B H 0.3935 0.0910 0.5447 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.016(4) 0.269(4) 0.477(3) 0.074(4) Uani 0.72(3) 1 d P A 1 O1 O 0.1091(10) 0.2913(12) 0.4659(6) 0.113(6) Uani 0.72(3) 1 d P A 1 O2 O -0.0023(11) 0.1784(9) 0.5300(7) 0.093(4) Uani 0.72(3) 1 d P A 1 O3 O 0.0091(11) 0.2684(12) 0.4070(9) 0.071(4) Uani 0.72(3) 1 d P A 1 O4 O -0.0447(13) 0.3292(8) 0.5076(7) 0.125(6) Uani 0.72(3) 1 d P A 1 Cl1' Cl 0.004(13) 0.258(11) 0.478(9) 0.09(3) Uani 0.28(3) 1 d P A 2 O1' O 0.092(3) 0.214(3) 0.4694(14) 0.106(15) Uani 0.28(3) 1 d P A 2 O2' O -0.045(3) 0.229(3) 0.538(2) 0.116(15) Uani 0.28(3) 1 d P A 2 O3' O -0.032(4) 0.247(4) 0.432(3) 0.101(13) Uani 0.28(3) 1 d P A 2 O4' O 0.039(3) 0.345(2) 0.4696(16) 0.098(14) Uani 0.28(3) 1 d P A 2 Cl2 Cl 0.174(4) 0.732(4) 0.179(3) 0.102(8) Uani 0.66(3) 1 d P B 1 O5 O 0.216(2) 0.649(3) 0.197(2) 0.124(8) Uani 0.66(3) 1 d P B 1 O6 O 0.1781(14) 0.7630(14) 0.1038(11) 0.133(7) Uani 0.66(3) 1 d P B 1 O7 O 0.0928(15) 0.7521(13) 0.2217(11) 0.143(10) Uani 0.66(3) 1 d P B 1 O8 O 0.2482(13) 0.7873(11) 0.1773(12) 0.138(7) Uani 0.66(3) 1 d P B 1 Cl2' Cl 0.177(9) 0.720(7) 0.197(7) 0.11(2) Uani 0.34(3) 1 d P B 2 O5' O 0.183(4) 0.641(5) 0.182(4) 0.117(16) Uani 0.34(3) 1 d P B 2 O6' O 0.213(3) 0.791(3) 0.132(3) 0.137(17) Uani 0.34(3) 1 d P B 2 O7' O 0.073(3) 0.710(2) 0.205(2) 0.120(12) Uani 0.34(3) 1 d P B 2 O8' O 0.158(2) 0.7551(19) 0.2511(17) 0.129(14) Uani 0.34(3) 1 d P B 2 Cl3 Cl 0.484(7) 0.384(8) 0.338(6) 0.091(7) Uani 0.61(2) 1 d P C 1 O9 O 0.4570(15) 0.2929(11) 0.3800(8) 0.133(7) Uani 0.61(2) 1 d P C 1 O10 O 0.5486(17) 0.3812(14) 0.2693(13) 0.148(8) Uani 0.61(2) 1 d P C 1 O11 O 0.3991(10) 0.4299(10) 0.3216(8) 0.107(5) Uani 0.61(2) 1 d P C 1 O12 O 0.5037(10) 0.4290(11) 0.3778(10) 0.127(6) Uani 0.61(2) 1 d P C 1 Cl3' Cl 0.477(11) 0.380(14) 0.331(9) 0.10(2) Uani 0.39(2) 1 d P C 2 O9' O 0.539(2) 0.3240(18) 0.3699(13) 0.133(10) Uani 0.39(2) 1 d P C 2 O10' O 0.495(2) 0.3523(18) 0.2675(18) 0.110(8) Uani 0.39(2) 1 d P C 2 O11' O 0.3882(19) 0.362(2) 0.3809(15) 0.135(10) Uani 0.39(2) 1 d P C 2 O12' O 0.5309(16) 0.4629(16) 0.3065(16) 0.127(10) Uani 0.39(2) 1 d P C 2 Cl4 Cl 0.304(3) 0.961(3) 0.459(2) 0.106(8) Uani 0.73(3) 1 d P D 1 O13 O 0.3762(17) 0.935(2) 0.4030(16) 0.139(7) Uani 0.73(3) 1 d P D 1 O14 O 0.2143(18) 0.9527(16) 0.4614(12) 0.144(7) Uani 0.73(3) 1 d P D 1 O15 O 0.3060(9) 1.0618(13) 0.4370(9) 0.133(6) Uani 0.73(3) 1 d P D 1 O16 O 0.3200(11) 0.9449(14) 0.5256(8) 0.139(7) Uani 0.73(3) 1 d P D 1 Cl4' Cl 0.306(9) 0.935(9) 0.465(7) 0.12(3) Uani 0.27(3) 1 d P D 2 O13' O 0.366(3) 0.861(3) 0.486(2) 0.15(2) Uani 0.27(3) 1 d P D 2 O14' O 0.215(5) 0.902(4) 0.490(3) 0.136(18) Uani 0.27(3) 1 d P D 2 O15' O 0.337(5) 0.961(5) 0.391(4) 0.127(18) Uani 0.27(3) 1 d P D 2 O16' O 0.322(3) 1.006(4) 0.485(3) 0.135(18) Uani 0.27(3) 1 d P D 2 N1S N 0.8400(12) 0.0487(9) 0.7183(9) 0.180(6) Uani 1 1 d . . . C77 C 0.7788(10) 0.1898(10) 0.6495(8) 0.173(6) Uani 1 1 d . . . H77A H 0.8242 0.2369 0.6309 0.259 Uiso 1 1 calc R . . H77B H 0.7218 0.2096 0.6803 0.259 Uiso 1 1 calc R . . H77C H 0.7679 0.1766 0.6092 0.259 Uiso 1 1 calc R . . C78 C 0.8127(11) 0.1084(10) 0.6919(9) 0.122(5) Uani 1 1 d . . . C1M C 0.2094(12) 0.5139(12) 0.4392(10) 0.178(7) Uani 1 1 d . . . H1M1 H 0.1512 0.4832 0.4565 0.266 Uiso 1 1 calc R . . H1M2 H 0.2362 0.5232 0.3870 0.266 Uiso 1 1 calc R . . H1M3 H 0.1994 0.5715 0.4503 0.266 Uiso 1 1 calc R . . O1M O 0.2658(12) 0.4645(11) 0.4713(8) 0.260(7) Uani 1 1 d . . . H1M H 0.3021 0.4344 0.4434 0.390 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0543(6) 0.0330(5) 0.0340(5) -0.0080(4) -0.0167(4) 0.0021(4) N1 0.061(4) 0.040(3) 0.043(3) -0.013(2) -0.016(3) 0.000(3) N2 0.055(4) 0.044(3) 0.045(3) -0.012(2) -0.025(3) 0.002(3) N3 0.047(3) 0.032(3) 0.040(3) -0.008(2) -0.015(3) 0.001(2) N4 0.060(4) 0.045(3) 0.060(4) -0.015(3) -0.026(3) 0.018(3) N5 0.055(4) 0.040(3) 0.041(3) -0.011(2) -0.015(3) -0.007(3) N6 0.073(4) 0.030(3) 0.047(3) -0.002(2) -0.023(3) -0.010(3) N7 0.064(4) 0.037(3) 0.045(3) -0.003(2) -0.021(3) 0.004(3) N8 0.085(5) 0.047(4) 0.088(5) -0.020(3) -0.040(4) 0.013(3) N9 0.054(4) 0.047(3) 0.034(3) -0.009(2) -0.018(3) 0.005(3) N10 0.060(4) 0.039(3) 0.041(3) -0.005(2) -0.015(3) -0.006(3) C1 0.069(5) 0.052(4) 0.058(4) -0.021(3) -0.018(4) 0.010(4) C2 0.084(6) 0.061(4) 0.037(4) -0.020(3) -0.017(4) -0.005(4) C3 0.078(5) 0.062(4) 0.041(4) -0.015(3) -0.031(4) -0.003(4) C4 0.060(5) 0.054(4) 0.046(4) -0.010(3) -0.032(4) -0.001(3) C5 0.047(4) 0.037(3) 0.055(4) -0.009(3) -0.021(3) 0.006(3) C6 0.103(7) 0.071(5) 0.101(6) -0.028(5) -0.058(6) 0.044(5) C7 0.049(4) 0.041(4) 0.056(4) -0.014(3) -0.017(4) 0.004(3) C8 0.079(6) 0.058(5) 0.080(5) -0.035(4) -0.028(5) 0.028(4) C9 0.109(7) 0.052(5) 0.081(6) -0.034(4) -0.033(5) 0.004(5) C10 0.088(6) 0.063(5) 0.053(4) -0.023(4) -0.023(4) -0.010(4) C11 0.064(5) 0.045(4) 0.057(4) -0.012(3) -0.026(4) -0.002(3) C12 0.048(4) 0.042(3) 0.045(4) -0.011(3) -0.019(3) -0.006(3) C13 0.055(4) 0.035(3) 0.034(3) -0.004(3) -0.013(3) -0.002(3) C14 0.057(5) 0.055(4) 0.036(3) -0.012(3) -0.012(3) -0.003(3) C15 0.064(5) 0.054(4) 0.046(4) -0.002(3) -0.008(4) -0.001(4) C16 0.067(6) 0.070(5) 0.052(4) 0.004(4) -0.002(4) -0.009(4) C17 0.066(5) 0.058(5) 0.054(4) -0.002(4) -0.019(4) -0.019(4) C18 0.067(5) 0.033(3) 0.045(4) -0.006(3) -0.025(4) -0.003(3) C19 0.092(6) 0.043(4) 0.084(5) -0.018(4) -0.037(5) -0.019(4) C20 0.070(5) 0.032(3) 0.038(3) -0.009(3) -0.018(4) 0.001(3) C21 0.084(6) 0.044(4) 0.055(4) -0.027(3) -0.028(4) 0.009(4) C22 0.065(5) 0.036(4) 0.060(4) -0.010(3) -0.025(4) 0.007(3) C23 0.128(9) 0.090(6) 0.136(8) -0.064(6) -0.075(7) 0.072(6) C24 0.094(7) 0.056(5) 0.071(5) -0.010(4) -0.050(5) 0.004(4) C25 0.154(10) 0.075(6) 0.100(7) -0.010(5) -0.088(7) 0.025(6) C26 0.188(12) 0.076(6) 0.085(7) -0.001(5) -0.091(8) 0.012(7) C27 0.067(5) 0.042(4) 0.055(4) -0.007(3) -0.027(4) -0.003(3) C28 0.099(6) 0.045(4) 0.052(4) 0.002(3) -0.031(4) -0.015(4) C29 0.140(9) 0.069(6) 0.062(5) -0.004(4) -0.049(6) -0.006(6) C30 0.055(5) 0.045(4) 0.038(3) -0.013(3) -0.022(3) 0.001(3) C31 0.069(6) 0.065(5) 0.063(5) -0.023(4) -0.032(4) 0.005(4) C32 0.079(7) 0.071(5) 0.080(6) -0.016(5) -0.050(5) 0.003(5) C33 0.066(6) 0.077(6) 0.102(7) -0.032(5) -0.033(6) -0.013(5) C34 0.068(6) 0.051(4) 0.076(5) -0.012(4) -0.020(5) -0.013(4) C35 0.051(5) 0.038(3) 0.052(4) -0.017(3) -0.018(4) -0.001(3) C36 0.084(6) 0.049(4) 0.052(4) 0.005(3) -0.018(4) -0.014(4) C37 0.058(5) 0.043(4) 0.035(3) -0.012(3) -0.017(3) 0.000(3) C38 0.073(5) 0.049(4) 0.042(4) -0.001(3) -0.022(4) 0.002(4) Fe2 0.0489(6) 0.0517(6) 0.0377(5) -0.0132(4) -0.0126(5) -0.0017(4) N11 0.053(4) 0.052(3) 0.044(3) -0.020(3) -0.014(3) 0.000(3) N12 0.062(4) 0.069(4) 0.037(3) -0.010(3) -0.015(3) -0.006(3) N13 0.061(4) 0.059(4) 0.055(4) -0.007(3) -0.025(3) -0.010(3) N14 0.085(6) 0.108(6) 0.074(5) 0.003(4) -0.011(4) -0.052(5) N15 0.060(4) 0.054(3) 0.056(3) -0.018(3) -0.027(3) 0.008(3) N16 0.062(4) 0.070(4) 0.059(4) -0.027(3) -0.027(3) 0.019(3) N17 0.048(3) 0.046(3) 0.037(3) -0.016(2) -0.005(3) -0.002(3) N18 0.057(4) 0.061(4) 0.057(4) -0.018(3) -0.008(3) -0.008(3) N19 0.050(3) 0.057(3) 0.031(3) -0.017(2) -0.008(3) 0.005(3) N20 0.036(3) 0.076(4) 0.050(3) -0.028(3) -0.016(3) 0.013(3) C39 0.053(5) 0.064(4) 0.054(4) -0.027(4) -0.016(4) 0.000(4) C40 0.059(5) 0.080(5) 0.041(4) -0.024(4) -0.017(4) -0.001(4) C41 0.067(5) 0.090(5) 0.034(4) -0.015(4) -0.014(4) -0.003(4) C42 0.077(6) 0.094(6) 0.049(4) -0.006(4) -0.015(4) -0.021(5) C43 0.054(5) 0.086(6) 0.060(5) 0.005(4) -0.019(4) -0.028(4) C44 0.152(12) 0.207(14) 0.126(10) 0.008(9) -0.038(9) -0.109(11) C45 0.082(7) 0.078(6) 0.079(6) -0.016(5) -0.027(5) -0.022(5) C46 0.089(8) 0.093(7) 0.141(10) -0.041(7) -0.060(7) -0.016(6) C47 0.106(9) 0.094(7) 0.150(11) -0.072(7) -0.087(9) 0.027(6) C48 0.116(9) 0.082(6) 0.118(8) -0.065(6) -0.082(7) 0.049(6) C49 0.077(6) 0.057(4) 0.081(6) -0.035(4) -0.036(5) 0.025(4) C50 0.067(6) 0.048(4) 0.076(5) -0.016(4) -0.041(5) 0.004(4) C51 0.083(6) 0.056(4) 0.057(4) -0.017(4) -0.031(4) -0.004(4) C52 0.099(7) 0.069(5) 0.093(6) -0.037(5) -0.044(6) 0.013(5) C53 0.112(8) 0.074(6) 0.133(9) -0.044(6) -0.049(7) -0.001(6) C54 0.136(10) 0.076(7) 0.162(11) -0.054(7) -0.071(9) 0.021(7) C55 0.103(8) 0.074(6) 0.131(8) -0.047(6) -0.055(7) 0.026(5) C56 0.084(6) 0.058(5) 0.068(5) -0.018(4) -0.035(5) 0.006(4) C57 0.076(6) 0.105(7) 0.100(7) -0.047(6) -0.044(6) 0.034(5) C58 0.060(5) 0.060(4) 0.046(4) -0.019(3) -0.019(4) 0.008(4) C59 0.059(5) 0.070(5) 0.063(5) -0.027(4) -0.023(4) 0.002(4) C60 0.051(4) 0.049(4) 0.039(4) -0.016(3) -0.010(3) 0.005(3) C61 0.059(5) 0.070(5) 0.056(4) -0.028(4) -0.018(4) 0.009(4) C62 0.073(6) 0.085(6) 0.060(5) -0.036(4) -0.026(5) 0.022(5) C63 0.087(7) 0.106(7) 0.048(5) -0.036(5) -0.012(5) 0.011(6) C64 0.065(6) 0.093(6) 0.059(5) -0.018(5) 0.002(4) -0.005(5) C65 0.053(5) 0.067(5) 0.045(4) -0.015(4) -0.012(4) 0.003(4) C66 0.058(5) 0.078(5) 0.087(6) -0.016(5) 0.001(5) -0.028(4) C67 0.052(5) 0.045(4) 0.046(4) -0.014(3) -0.005(3) -0.004(3) C68 0.036(4) 0.056(4) 0.046(4) -0.015(3) -0.010(3) -0.002(3) C69 0.059(5) 0.063(4) 0.046(4) -0.017(3) -0.015(4) 0.002(4) C70 0.069(6) 0.079(6) 0.054(5) 0.000(4) -0.017(4) 0.000(4) C71 0.082(6) 0.067(5) 0.078(6) -0.004(4) -0.041(5) 0.014(5) C72 0.064(6) 0.077(6) 0.088(6) -0.031(5) -0.036(5) 0.025(4) C73 0.038(4) 0.061(4) 0.052(4) -0.019(3) -0.021(3) 0.007(3) C74 0.062(5) 0.123(7) 0.070(5) -0.061(5) -0.009(4) 0.036(5) C75 0.040(4) 0.067(5) 0.039(4) -0.017(3) -0.010(3) -0.002(3) C76 0.051(5) 0.091(6) 0.040(4) -0.020(4) -0.002(3) -0.005(4) Cl1 0.098(8) 0.073(9) 0.057(5) -0.025(5) -0.027(5) -0.005(8) O1 0.115(11) 0.135(17) 0.093(7) -0.009(8) -0.044(7) -0.042(10) O2 0.114(11) 0.065(7) 0.088(8) 0.001(6) -0.034(8) -0.011(6) O3 0.075(10) 0.084(9) 0.056(8) -0.028(7) -0.018(6) -0.001(6) O4 0.166(15) 0.105(10) 0.096(9) -0.052(8) -0.022(10) 0.033(9) Cl1' 0.12(6) 0.09(4) 0.068(17) -0.03(2) -0.03(3) 0.00(3) O1' 0.13(3) 0.10(3) 0.086(18) -0.024(17) -0.037(19) 0.02(2) O2' 0.14(3) 0.10(4) 0.08(2) -0.02(2) -0.01(2) -0.02(3) O3' 0.12(4) 0.10(3) 0.09(3) -0.02(2) -0.04(3) -0.01(2) O4' 0.13(4) 0.09(2) 0.077(18) -0.038(15) -0.02(2) -0.01(2) Cl2 0.086(8) 0.088(10) 0.14(2) -0.067(12) -0.021(12) 0.022(6) O5 0.097(18) 0.089(14) 0.18(2) -0.047(12) -0.035(12) 0.020(12) O6 0.120(13) 0.146(14) 0.139(16) -0.066(11) -0.040(10) 0.036(10) O7 0.105(15) 0.127(14) 0.161(17) -0.055(11) 0.005(14) 0.032(14) O8 0.131(14) 0.124(11) 0.166(17) -0.053(11) -0.042(12) -0.022(9) Cl2' 0.09(2) 0.09(3) 0.16(5) -0.08(3) -0.02(2) 0.01(2) O5' 0.11(4) 0.09(2) 0.16(3) -0.068(19) -0.03(3) 0.01(3) O6' 0.12(3) 0.11(3) 0.17(4) -0.05(3) -0.02(3) -0.01(2) O7' 0.10(2) 0.12(3) 0.15(2) -0.073(19) -0.024(17) 0.001(17) O8' 0.11(3) 0.13(2) 0.16(3) -0.091(19) -0.03(2) 0.007(17) Cl3 0.090(14) 0.108(12) 0.089(8) -0.033(7) -0.041(9) 0.000(13) O9 0.148(18) 0.110(12) 0.129(12) -0.007(9) -0.052(11) -0.002(11) O10 0.138(18) 0.157(18) 0.122(14) -0.040(12) -0.009(15) 0.012(13) O11 0.099(11) 0.108(10) 0.119(11) -0.027(8) -0.051(9) 0.013(8) O12 0.134(12) 0.140(13) 0.127(14) -0.042(11) -0.059(10) -0.019(9) Cl3' 0.10(3) 0.109(19) 0.11(5) -0.03(3) -0.04(2) -0.008(14) O9' 0.13(2) 0.13(2) 0.129(17) -0.002(14) -0.059(17) -0.004(17) O10' 0.094(19) 0.127(18) 0.110(17) -0.028(14) -0.035(15) -0.018(14) O11' 0.11(2) 0.14(2) 0.13(2) -0.032(18) -0.024(17) -0.003(17) O12' 0.137(19) 0.115(18) 0.13(2) -0.023(16) -0.056(17) -0.016(15) Cl4 0.089(11) 0.17(2) 0.067(6) -0.015(10) -0.036(5) -0.036(13) O13 0.115(18) 0.20(2) 0.111(15) -0.057(15) -0.033(12) 0.005(12) O14 0.103(12) 0.179(18) 0.133(16) 0.005(11) -0.052(11) -0.025(13) O15 0.133(10) 0.163(15) 0.104(11) -0.026(9) -0.049(8) 0.004(9) O16 0.158(12) 0.187(17) 0.076(9) -0.003(9) -0.061(9) -0.025(11) Cl4' 0.09(3) 0.17(7) 0.09(3) -0.03(4) -0.03(2) -0.01(4) O13' 0.13(3) 0.20(4) 0.13(3) -0.01(3) -0.06(2) 0.02(3) O14' 0.10(3) 0.18(5) 0.11(4) -0.01(3) -0.04(3) -0.03(4) O15' 0.11(5) 0.19(5) 0.08(3) -0.02(3) -0.04(3) 0.00(3) O16' 0.14(3) 0.18(5) 0.09(4) -0.02(4) -0.04(3) -0.03(4) N1S 0.270(17) 0.116(9) 0.208(14) -0.103(10) -0.108(12) 0.028(11) C77 0.149(13) 0.165(14) 0.195(15) -0.063(12) -0.044(12) 0.037(11) C78 0.140(12) 0.100(10) 0.142(12) -0.071(10) -0.035(9) 0.006(9) C1M 0.154(15) 0.186(17) 0.208(18) -0.053(14) -0.083(13) 0.017(12) O1M 0.29(2) 0.248(16) 0.244(15) -0.081(13) -0.078(14) 0.001(13) _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 N3 2.124(5) . ? Fe1 N7 2.146(5) . ? Fe1 N9 2.151(5) . ? Fe1 N5 2.173(5) . ? Fe1 N2 2.287(5) . ? Fe1 N1 2.289(5) . ? N1 C1 1.463(8) . ? N1 C21 1.472(8) . ? N1 C2 1.495(8) . ? N2 C4 1.477(8) . ? N2 C38 1.479(8) . ? N2 C3 1.479(7) . ? N3 C5 1.321(7) . ? N3 C12 1.402(7) . ? N4 C5 1.359(7) . ? N4 C7 1.396(8) . ? N4 C6 1.465(8) . ? N5 C20 1.331(7) . ? N5 C13 1.394(7) . ? N6 C20 1.341(8) . ? N6 C18 1.379(8) . ? N6 C19 1.471(7) . ? N7 C22 1.311(8) . ? N7 C27 1.389(8) . ? N8 C22 1.339(8) . ? N8 C24 1.386(9) . ? N8 C23 1.481(9) . ? N9 C37 1.317(7) . ? N9 C30 1.393(8) . ? N10 C37 1.326(8) . ? N10 C35 1.383(8) . ? N10 C36 1.470(7) . ? C1 C22 1.531(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.515(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.489(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.362(9) . ? C7 C12 1.413(8) . ? C8 C9 1.389(10) . ? C8 H8 0.9300 . ? C9 C10 1.376(10) . ? C9 H9 0.9300 . ? C10 C11 1.389(9) . ? C10 H10 0.9300 . ? C11 C12 1.363(8) . ? C11 H11 0.9300 . ? C13 C14 1.379(8) . ? C13 C18 1.404(8) . ? C14 C15 1.378(9) . ? C14 H14 0.9300 . ? C15 C16 1.395(10) . ? C15 H15 0.9300 . ? C16 C17 1.374(10) . ? C16 H16 0.9300 . ? C17 C18 1.386(9) . ? C17 H17 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.502(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.386(10) . ? C24 C25 1.401(10) . ? C25 C26 1.353(13) . ? C25 H25 0.9300 . ? C26 C29 1.373(12) . ? C26 H26 0.9300 . ? C27 C28 1.370(9) . ? C28 C29 1.394(10) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.386(9) . ? C30 C35 1.401(8) . ? C31 C32 1.361(10) . ? C31 H31 0.9300 . ? C32 C33 1.379(11) . ? C32 H32 0.9300 . ? C33 C34 1.374(11) . ? C33 H33 0.9300 . ? C34 C35 1.387(9) . ? C34 H34 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.493(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? Fe2 N13 2.119(6) . ? Fe2 N15 2.124(5) . ? Fe2 N17 2.141(5) . ? Fe2 N19 2.166(5) . ? Fe2 N11 2.284(5) . ? Fe2 N12 2.308(5) . ? N11 C39 1.462(8) . ? N11 C40 1.483(7) . ? N11 C59 1.486(8) . ? N12 C76 1.467(9) . ? N12 C42 1.484(9) . ? N12 C41 1.492(9) . ? N13 C43 1.310(8) . ? N13 C50 1.397(8) . ? N14 C43 1.338(9) . ? N14 C45 1.389(10) . ? N14 C44 1.488(12) . ? N15 C58 1.330(8) . ? N15 C51 1.408(8) . ? N16 C58 1.344(8) . ? N16 C56 1.372(9) . ? N16 C57 1.452(9) . ? N17 C67 1.325(8) . ? N17 C60 1.401(7) . ? N18 C67 1.342(8) . ? N18 C65 1.414(8) . ? N18 C66 1.474(9) . ? N19 C75 1.326(7) . ? N19 C68 1.392(8) . ? N20 C75 1.346(8) . ? N20 C73 1.379(8) . ? N20 C74 1.464(8) . ? C39 C67 1.493(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.510(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.498(10) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C50 1.369(10) . ? C45 C46 1.390(11) . ? C46 C47 1.362(13) . ? C46 H46 0.9300 . ? C47 C48 1.381(13) . ? C47 H47 0.9300 . ? C48 C49 1.401(11) . ? C48 H48 0.9300 . ? C49 C50 1.375(10) . ? C49 H49 0.9300 . ? C51 C56 1.379(10) . ? C51 C52 1.383(10) . ? C52 C53 1.402(11) . ? C52 H52 0.9300 . ? C53 C54 1.396(13) . ? C53 H53 0.9300 . ? C54 C55 1.372(13) . ? C54 H54 0.9300 . ? C55 C56 1.390(10) . ? C55 H55 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C59 1.490(9) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.369(9) . ? C60 C65 1.386(9) . ? C61 C62 1.388(9) . ? C61 H61 0.9300 . ? C62 C63 1.361(11) . ? C62 H62 0.9300 . ? C63 C64 1.371(11) . ? C63 H63 0.9300 . ? C64 C65 1.385(9) . ? C64 H64 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C68 C69 1.384(8) . ? C68 C73 1.414(8) . ? C69 C70 1.374(9) . ? C69 H69 0.9300 . ? C70 C71 1.401(10) . ? C70 H70 0.9300 . ? C71 C72 1.362(10) . ? C71 H71 0.9300 . ? C72 C73 1.369(9) . ? C72 H72 0.9300 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C76 1.494(9) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? Cl1 O4 1.37(7) . ? Cl1 O1 1.43(6) . ? Cl1 O3 1.45(5) . ? Cl1 O2 1.48(5) . ? Cl1' O2' 1.17(16) . ? Cl1' O3' 1.29(14) . ? Cl1' O1' 1.42(17) . ? Cl1' O4' 1.44(16) . ? Cl2 O7 1.32(7) . ? Cl2 O5 1.37(7) . ? Cl2 O6 1.43(7) . ? Cl2 O8 1.47(6) . ? Cl2' O8' 1.28(11) . ? Cl2' O5' 1.34(13) . ? Cl2' O6' 1.42(14) . ? Cl2' O7' 1.57(14) . ? Cl3 O12 1.31(10) . ? Cl3 O10 1.41(11) . ? Cl3 O9 1.43(13) . ? Cl3 O11 1.52(10) . ? Cl3' O11' 1.39(17) . ? Cl3' O10' 1.39(15) . ? Cl3' O12' 1.5(2) . ? Cl3' O9' 1.49(15) . ? Cl4 O16 1.38(4) . ? Cl4 O14 1.39(5) . ? Cl4 O13 1.41(5) . ? Cl4 O15 1.48(6) . ? Cl4' O16' 1.33(15) . ? Cl4' O15' 1.36(12) . ? Cl4' O14' 1.41(14) . ? Cl4' O13' 1.44(14) . ? N1S C78 1.046(16) . ? C77 C78 1.456(18) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C1M O1M 1.306(16) . ? C1M H1M1 0.9600 . ? C1M H1M2 0.9600 . ? C1M H1M3 0.9600 . ? O1M H1M 0.8500 . ? 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 N3 Fe1 N7 130.83(19) . . ? N3 Fe1 N9 92.89(18) . . ? N7 Fe1 N9 94.4(2) . . ? N3 Fe1 N5 92.12(19) . . ? N7 Fe1 N5 90.4(2) . . ? N9 Fe1 N5 168.21(18) . . ? N3 Fe1 N2 76.52(18) . . ? N7 Fe1 N2 152.37(19) . . ? N9 Fe1 N2 78.21(19) . . ? N5 Fe1 N2 92.60(19) . . ? N3 Fe1 N1 153.0(2) . . ? N7 Fe1 N1 74.80(19) . . ? N9 Fe1 N1 93.08(19) . . ? N5 Fe1 N1 77.77(19) . . ? N2 Fe1 N1 79.01(18) . . ? C1 N1 C21 111.6(5) . . ? C1 N1 C2 112.7(5) . . ? C21 N1 C2 110.5(5) . . ? C1 N1 Fe1 105.3(4) . . ? C21 N1 Fe1 110.6(4) . . ? C2 N1 Fe1 105.9(4) . . ? C4 N2 C38 110.0(5) . . ? C4 N2 C3 113.2(5) . . ? C38 N2 C3 111.7(5) . . ? C4 N2 Fe1 105.3(3) . . ? C38 N2 Fe1 109.8(4) . . ? C3 N2 Fe1 106.6(4) . . ? C5 N3 C12 106.3(5) . . ? C5 N3 Fe1 113.3(4) . . ? C12 N3 Fe1 140.4(4) . . ? C5 N4 C7 107.4(5) . . ? C5 N4 C6 126.8(6) . . ? C7 N4 C6 125.8(6) . . ? C20 N5 C13 105.5(5) . . ? C20 N5 Fe1 114.8(4) . . ? C13 N5 Fe1 139.7(4) . . ? C20 N6 C18 107.7(5) . . ? C20 N6 C19 126.5(6) . . ? C18 N6 C19 125.8(6) . . ? C22 N7 C27 105.5(5) . . ? C22 N7 Fe1 113.7(4) . . ? C27 N7 Fe1 140.7(4) . . ? C22 N8 C24 105.3(6) . . ? C22 N8 C23 128.7(7) . . ? C24 N8 C23 125.9(7) . . ? C37 N9 C30 105.3(5) . . ? C37 N9 Fe1 114.9(5) . . ? C30 N9 Fe1 139.7(4) . . ? C37 N10 C35 107.0(5) . . ? C37 N10 C36 127.8(6) . . ? C35 N10 C36 125.3(6) . . ? N1 C1 C22 106.8(5) . . ? N1 C1 H1A 110.4 . . ? C22 C1 H1A 110.4 . . ? N1 C1 H1B 110.4 . . ? C22 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? N1 C2 C3 110.4(5) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C2 109.5(5) . . ? N2 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C5 108.0(5) . . ? N2 C4 H4A 110.1 . . ? C5 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? C5 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N3 C5 N4 112.4(6) . . ? N3 C5 C4 122.0(5) . . ? N4 C5 C4 125.5(6) . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N4 133.0(6) . . ? C8 C7 C12 121.7(7) . . ? N4 C7 C12 105.4(5) . . ? C7 C8 C9 117.2(7) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? C10 C9 C8 121.2(7) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.9(7) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 117.2(7) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? C11 C12 N3 130.6(6) . . ? C11 C12 C7 120.9(6) . . ? N3 C12 C7 108.5(5) . . ? C14 C13 N5 131.7(6) . . ? C14 C13 C18 119.8(6) . . ? N5 C13 C18 108.5(5) . . ? C15 C14 C13 117.9(6) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? C14 C15 C16 121.2(7) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 122.3(7) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 115.7(7) . . ? C16 C17 H17 122.1 . . ? C18 C17 H17 122.1 . . ? N6 C18 C17 131.3(6) . . ? N6 C18 C13 105.7(6) . . ? C17 C18 C13 122.9(6) . . ? N6 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 N6 112.5(6) . . ? N5 C20 C21 122.3(6) . . ? N6 C20 C21 125.1(6) . . ? N1 C21 C20 112.5(5) . . ? N1 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? N1 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N7 C22 N8 114.1(6) . . ? N7 C22 C1 120.4(6) . . ? N8 C22 C1 125.4(6) . . ? N8 C23 H23A 109.5 . . ? N8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 N8 107.2(6) . . ? C27 C24 C25 120.5(8) . . ? N8 C24 C25 132.1(8) . . ? C26 C25 C24 117.9(9) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 C29 121.3(8) . . ? C25 C26 H26 119.4 . . ? C29 C26 H26 119.4 . . ? C28 C27 C24 121.5(7) . . ? C28 C27 N7 130.5(7) . . ? C24 C27 N7 108.0(6) . . ? C27 C28 C29 116.8(8) . . ? C27 C28 H28 121.6 . . ? C29 C28 H28 121.6 . . ? C26 C29 C28 121.9(9) . . ? C26 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C31 C30 N9 132.5(6) . . ? C31 C30 C35 119.4(7) . . ? N9 C30 C35 108.1(5) . . ? C32 C31 C30 117.8(7) . . ? C32 C31 H31 121.1 . . ? C30 C31 H31 121.1 . . ? C31 C32 C33 122.3(8) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C34 C33 C32 122.0(8) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 115.7(7) . . ? C33 C34 H34 122.2 . . ? C35 C34 H34 122.2 . . ? N10 C35 C34 131.3(7) . . ? N10 C35 C30 105.9(6) . . ? C34 C35 C30 122.8(7) . . ? N10 C36 H36A 109.5 . . ? N10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 N10 113.7(6) . . ? N9 C37 C38 123.0(6) . . ? N10 C37 C38 123.3(6) . . ? N2 C38 C37 112.6(5) . . ? N2 C38 H38A 109.1 . . ? C37 C38 H38A 109.1 . . ? N2 C38 H38B 109.1 . . ? C37 C38 H38B 109.1 . . ? H38A C38 H38B 107.8 . . ? N13 Fe2 N15 93.3(2) . . ? N13 Fe2 N17 132.0(2) . . ? N15 Fe2 N17 90.4(2) . . ? N13 Fe2 N19 90.7(2) . . ? N15 Fe2 N19 170.2(2) . . ? N17 Fe2 N19 93.65(19) . . ? N13 Fe2 N11 151.9(2) . . ? N15 Fe2 N11 79.0(2) . . ? N17 Fe2 N11 75.58(19) . . ? N19 Fe2 N11 93.30(19) . . ? N13 Fe2 N12 75.7(2) . . ? N15 Fe2 N12 95.0(2) . . ? N17 Fe2 N12 151.5(2) . . ? N19 Fe2 N12 77.27(19) . . ? N11 Fe2 N12 78.1(2) . . ? C39 N11 C40 112.9(5) . . ? C39 N11 C59 110.5(5) . . ? C40 N11 C59 111.4(5) . . ? C39 N11 Fe2 105.0(4) . . ? C40 N11 Fe2 107.3(4) . . ? C59 N11 Fe2 109.4(4) . . ? C76 N12 C42 111.1(6) . . ? C76 N12 C41 112.0(6) . . ? C42 N12 C41 112.3(6) . . ? C76 N12 Fe2 111.0(4) . . ? C42 N12 Fe2 104.4(4) . . ? C41 N12 Fe2 105.6(4) . . ? C43 N13 C50 106.3(6) . . ? C43 N13 Fe2 114.2(5) . . ? C50 N13 Fe2 139.5(5) . . ? C43 N14 C45 107.5(7) . . ? C43 N14 C44 125.0(8) . . ? C45 N14 C44 127.5(8) . . ? C58 N15 C51 104.6(6) . . ? C58 N15 Fe2 114.6(4) . . ? C51 N15 Fe2 140.3(5) . . ? C58 N16 C56 107.0(6) . . ? C58 N16 C57 127.2(7) . . ? C56 N16 C57 125.8(7) . . ? C67 N17 C60 105.7(5) . . ? C67 N17 Fe2 113.6(4) . . ? C60 N17 Fe2 140.7(5) . . ? C67 N18 C65 105.7(6) . . ? C67 N18 C66 128.4(6) . . ? C65 N18 C66 125.8(6) . . ? C75 N19 C68 105.7(5) . . ? C75 N19 Fe2 115.1(4) . . ? C68 N19 Fe2 139.2(4) . . ? C75 N20 C73 107.4(5) . . ? C75 N20 C74 128.1(6) . . ? C73 N20 C74 124.5(6) . . ? N11 C39 C67 108.6(5) . . ? N11 C39 H39A 110.0 . . ? C67 C39 H39A 110.0 . . ? N11 C39 H39B 110.0 . . ? C67 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? N11 C40 C41 108.8(5) . . ? N11 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? N11 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N12 C41 C40 108.9(5) . . ? N12 C41 H41A 109.9 . . ? C40 C41 H41A 109.9 . . ? N12 C41 H41B 109.9 . . ? C40 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? N12 C42 C43 106.9(6) . . ? N12 C42 H42A 110.3 . . ? C43 C42 H42A 110.3 . . ? N12 C42 H42B 110.3 . . ? C43 C42 H42B 110.3 . . ? H42A C42 H42B 108.6 . . ? N13 C43 N14 111.8(7) . . ? N13 C43 C42 121.7(7) . . ? N14 C43 C42 126.4(7) . . ? N14 C44 H44A 109.5 . . ? N14 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N14 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 N14 105.9(8) . . ? C50 C45 C46 122.0(9) . . ? N14 C45 C46 132.0(9) . . ? C47 C46 C45 117.2(10) . . ? C47 C46 H46 121.4 . . ? C45 C46 H46 121.4 . . ? C46 C47 C48 121.0(10) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C49 122.1(9) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C50 C49 C48 116.0(9) . . ? C50 C49 H49 122.0 . . ? C48 C49 H49 122.0 . . ? C45 C50 C49 121.6(8) . . ? C45 C50 N13 108.5(7) . . ? C49 C50 N13 129.9(8) . . ? C56 C51 C52 122.0(7) . . ? C56 C51 N15 108.6(7) . . ? C52 C51 N15 129.4(8) . . ? C51 C52 C53 115.8(9) . . ? C51 C52 H52 122.1 . . ? C53 C52 H52 122.1 . . ? C54 C53 C52 122.0(10) . . ? C54 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? C55 C54 C53 121.1(9) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C56 117.2(9) . . ? C54 C55 H55 121.4 . . ? C56 C55 H55 121.4 . . ? N16 C56 C51 106.9(7) . . ? N16 C56 C55 131.2(8) . . ? C51 C56 C55 121.9(8) . . ? N16 C57 H57A 109.5 . . ? N16 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N16 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N15 C58 N16 112.8(6) . . ? N15 C58 C59 123.3(6) . . ? N16 C58 C59 123.9(7) . . ? N11 C59 C58 112.7(6) . . ? N11 C59 H59A 109.1 . . ? C58 C59 H59A 109.1 . . ? N11 C59 H59B 109.1 . . ? C58 C59 H59B 109.1 . . ? H59A C59 H59B 107.8 . . ? C61 C60 C65 120.4(6) . . ? C61 C60 N17 131.2(6) . . ? C65 C60 N17 108.3(6) . . ? C60 C61 C62 117.3(7) . . ? C60 C61 H61 121.4 . . ? C62 C61 H61 121.4 . . ? C63 C62 C61 121.6(8) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C62 C63 C64 122.3(7) . . ? C62 C63 H63 118.9 . . ? C64 C63 H63 118.9 . . ? C63 C64 C65 116.0(8) . . ? C63 C64 H64 122.0 . . ? C65 C64 H64 122.0 . . ? C64 C65 C60 122.4(7) . . ? C64 C65 N18 130.9(7) . . ? C60 C65 N18 106.6(6) . . ? N18 C66 H66A 109.5 . . ? N18 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N18 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N17 C67 N18 113.6(6) . . ? N17 C67 C39 120.3(6) . . ? N18 C67 C39 126.1(6) . . ? C69 C68 N19 132.5(6) . . ? C69 C68 C73 119.1(6) . . ? N19 C68 C73 108.4(5) . . ? C70 C69 C68 119.2(7) . . ? C70 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C69 C70 C71 119.5(7) . . ? C69 C70 H70 120.3 . . ? C71 C70 H70 120.3 . . ? C72 C71 C70 123.1(7) . . ? C72 C71 H71 118.5 . . ? C70 C71 H71 118.5 . . ? C71 C72 C73 116.7(7) . . ? C71 C72 H72 121.6 . . ? C73 C72 H72 121.6 . . ? C72 C73 N20 131.9(7) . . ? C72 C73 C68 122.3(7) . . ? N20 C73 C68 105.7(6) . . ? N20 C74 H74A 109.5 . . ? N20 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N20 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N19 C75 N20 112.8(6) . . ? N19 C75 C76 123.2(6) . . ? N20 C75 C76 123.9(6) . . ? N12 C76 C75 112.1(5) . . ? N12 C76 H76A 109.2 . . ? C75 C76 H76A 109.2 . . ? N12 C76 H76B 109.2 . . ? C75 C76 H76B 109.2 . . ? H76A C76 H76B 107.9 . . ? O4 Cl1 O1 110(4) . . ? O4 Cl1 O3 112(3) . . ? O1 Cl1 O3 109(4) . . ? O4 Cl1 O2 108(4) . . ? O1 Cl1 O2 107(3) . . ? O3 Cl1 O2 112(4) . . ? O2' Cl1' O3' 110(10) . . ? O2' Cl1' O1' 110(10) . . ? O3' Cl1' O1' 111(10) . . ? O2' Cl1' O4' 111(10) . . ? O3' Cl1' O4' 120(10) . . ? O1' Cl1' O4' 94(10) . . ? O7 Cl2 O5 121(5) . . ? O7 Cl2 O6 110(4) . . ? O5 Cl2 O6 114(4) . . ? O7 Cl2 O8 111(4) . . ? O5 Cl2 O8 97(4) . . ? O6 Cl2 O8 100(4) . . ? O8' Cl2' O5' 142(10) . . ? O8' Cl2' O6' 107(7) . . ? O5' Cl2' O6' 111(9) . . ? O8' Cl2' O7' 95(8) . . ? O5' Cl2' O7' 81(7) . . ? O6' Cl2' O7' 105(8) . . ? O12 Cl3 O10 120(9) . . ? O12 Cl3 O9 112(7) . . ? O10 Cl3 O9 108(7) . . ? O12 Cl3 O11 105(6) . . ? O10 Cl3 O11 104(6) . . ? O9 Cl3 O11 106(7) . . ? O11' Cl3' O10' 115(10) . . ? O11' Cl3' O12' 128(10) . . ? O10' Cl3' O12' 105(10) . . ? O11' Cl3' O9' 104(10) . . ? O10' Cl3' O9' 106(10) . . ? O12' Cl3' O9' 95(9) . . ? O16 Cl4 O14 118(3) . . ? O16 Cl4 O13 116(3) . . ? O14 Cl4 O13 117(3) . . ? O16 Cl4 O15 100(3) . . ? O14 Cl4 O15 96(3) . . ? O13 Cl4 O15 105(3) . . ? O16' Cl4' O15' 105(10) . . ? O16' Cl4' O14' 119(10) . . ? O15' Cl4' O14' 109(8) . . ? O16' Cl4' O13' 109(8) . . ? O15' Cl4' O13' 105(10) . . ? O14' Cl4' O13' 109(8) . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N1S C78 C77 175.3(18) . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C1M O1M H1M 109.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.564 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.075 #Complex 5 CCDC 804329 data_Fe(OBu)MeEDTB.(ClO4)3.(MeCN)3.H2O _database_code_depnum_ccdc_archive 'CCDC 804326' #TrackingRef '- newcifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H58 Cl3 Fe N12 O14' _chemical_formula_weight 1165.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8139(13) _cell_length_b 15.555(2) _cell_length_c 16.3662(19) _cell_angle_alpha 86.034(4) _cell_angle_beta 71.979(4) _cell_angle_gamma 89.103(5) _cell_volume 2853.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9740 _cell_measurement_theta_min 1.3114 _cell_measurement_theta_max 27.4834 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1214 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8513 _exptl_absorpt_correction_T_max 0.8628 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21338 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9967 _reflns_number_gt 8826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0738P)^2^+3.4111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9967 _refine_ls_number_parameters 738 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.05047(4) 0.29571(3) 0.28013(3) 0.02071(13) Uani 1 1 d . . . O1 O -0.06053(19) 0.35969(13) 0.25270(13) 0.0281(5) Uani 1 1 d . . . N1 N 0.1866(2) 0.21972(16) 0.33335(16) 0.0242(5) Uani 1 1 d . . . N2 N -0.0505(2) 0.16855(16) 0.33272(16) 0.0240(5) Uani 1 1 d . . . N3 N -0.2651(2) 0.04213(16) 0.41941(17) 0.0283(6) Uani 1 1 d . . . H3 H -0.2335 0.0199 0.3694 0.034 Uiso 1 1 calc R . . N4 N -0.3120(2) 0.13459(17) 0.51803(17) 0.0290(6) Uani 1 1 d . . . N5 N 0.0102(2) 0.33316(16) 0.40559(16) 0.0238(5) Uani 1 1 d . . . N6 N 0.0618(2) 0.34933(17) 0.52278(17) 0.0296(6) Uani 1 1 d . . . N7 N 0.2103(2) 0.36390(16) 0.23229(15) 0.0235(5) Uani 1 1 d . . . N8 N 0.4079(2) 0.36301(17) 0.18072(18) 0.0300(6) Uani 1 1 d . . . N9 N 0.1042(2) 0.21719(16) 0.17323(15) 0.0236(5) Uani 1 1 d . . . N10 N 0.0995(2) 0.09235(16) 0.11545(17) 0.0276(6) Uani 1 1 d . . . C1 C 0.1944(3) 0.2601(2) 0.4112(2) 0.0294(7) Uani 1 1 d . . . H1A H 0.1996 0.2146 0.4552 0.035 Uiso 1 1 calc R . . H1B H 0.2673 0.2961 0.3959 0.035 Uiso 1 1 calc R . . C2 C 0.1426(3) 0.12967(19) 0.3545(2) 0.0279(7) Uani 1 1 d . . . H2A H 0.1800 0.1005 0.3952 0.033 Uiso 1 1 calc R . . H2B H 0.1645 0.0980 0.3014 0.033 Uiso 1 1 calc R . . C3 C 0.0080(3) 0.1289(2) 0.39469(19) 0.0268(7) Uani 1 1 d . . . H3A H -0.0204 0.0688 0.4116 0.032 Uiso 1 1 calc R . . H3B H -0.0137 0.1614 0.4472 0.032 Uiso 1 1 calc R . . C4 C -0.0420(3) 0.1108(2) 0.2621(2) 0.0278(7) Uani 1 1 d . . . H4A H -0.0275 0.0510 0.2810 0.033 Uiso 1 1 calc R . . H4B H -0.1181 0.1116 0.2486 0.033 Uiso 1 1 calc R . . C5 C -0.1762(3) 0.1923(2) 0.3761(2) 0.0265(7) Uani 1 1 d . . . H5A H -0.2143 0.2089 0.3313 0.032 Uiso 1 1 calc R . . H5B H -0.1765 0.2436 0.4087 0.032 Uiso 1 1 calc R . . C6 C -0.2504(3) 0.1231(2) 0.4365(2) 0.0264(7) Uani 1 1 d . . . C7 C -0.3383(3) -0.0013(2) 0.4933(2) 0.0309(7) Uani 1 1 d . . . C8 C -0.3819(3) -0.0855(2) 0.5095(3) 0.0378(8) Uani 1 1 d . . . H8 H -0.3619 -0.1260 0.4665 0.045 Uiso 1 1 calc R . . C9 C -0.4557(3) -0.1067(3) 0.5919(3) 0.0464(10) Uani 1 1 d . . . H9 H -0.4880 -0.1634 0.6056 0.056 Uiso 1 1 calc R . . C10 C -0.4842(3) -0.0485(3) 0.6547(3) 0.0498(11) Uani 1 1 d . . . H10 H -0.5349 -0.0666 0.7105 0.060 Uiso 1 1 calc R . . C11 C -0.4417(3) 0.0354(3) 0.6393(2) 0.0432(9) Uani 1 1 d . . . H11 H -0.4616 0.0755 0.6828 0.052 Uiso 1 1 calc R . . C12 C -0.3680(3) 0.0573(2) 0.5561(2) 0.0317(7) Uani 1 1 d . . . C13 C -0.3256(3) 0.2152(2) 0.5618(2) 0.0421(9) Uani 1 1 d . . . H13A H -0.2512 0.2286 0.5730 0.063 Uiso 1 1 calc R . . H13B H -0.3902 0.2087 0.6164 0.063 Uiso 1 1 calc R . . H13C H -0.3445 0.2622 0.5251 0.063 Uiso 1 1 calc R . . C14 C 0.0883(3) 0.31438(19) 0.44710(19) 0.0263(7) Uani 1 1 d . . . C15 C -0.0768(3) 0.38345(19) 0.45982(19) 0.0255(6) Uani 1 1 d . . . C16 C -0.1813(3) 0.4193(2) 0.4510(2) 0.0306(7) Uani 1 1 d . . . H16 H -0.2036 0.4140 0.4006 0.037 Uiso 1 1 calc R . . C17 C -0.2513(3) 0.4631(2) 0.5195(2) 0.0372(8) Uani 1 1 d . . . H17 H -0.3238 0.4879 0.5161 0.045 Uiso 1 1 calc R . . C18 C -0.2181(3) 0.4717(2) 0.5935(2) 0.0439(9) Uani 1 1 d . . . H18 H -0.2685 0.5025 0.6389 0.053 Uiso 1 1 calc R . . C19 C -0.1149(3) 0.4370(2) 0.6026(2) 0.0403(8) Uani 1 1 d . . . H19 H -0.0923 0.4429 0.6528 0.048 Uiso 1 1 calc R . . C20 C -0.0453(3) 0.3927(2) 0.5342(2) 0.0299(7) Uani 1 1 d . . . C21 C 0.1291(3) 0.3399(2) 0.5844(2) 0.0394(8) Uani 1 1 d . . . H21A H 0.0933 0.2940 0.6286 0.059 Uiso 1 1 calc R . . H21B H 0.1272 0.3942 0.6118 0.059 Uiso 1 1 calc R . . H21C H 0.2117 0.3252 0.5542 0.059 Uiso 1 1 calc R . . C22 C 0.3026(3) 0.2284(2) 0.2643(2) 0.0279(7) Uani 1 1 d . . . H22A H 0.3078 0.1866 0.2204 0.033 Uiso 1 1 calc R . . H22B H 0.3690 0.2176 0.2886 0.033 Uiso 1 1 calc R . . C23 C 0.3090(3) 0.3185(2) 0.22519(19) 0.0259(6) Uani 1 1 d . . . C24 C 0.2477(3) 0.44417(19) 0.18931(19) 0.0246(6) Uani 1 1 d . . . C25 C 0.1829(3) 0.5160(2) 0.1766(2) 0.0283(7) Uani 1 1 d . . . H25 H 0.0984 0.5165 0.1981 0.034 Uiso 1 1 calc R . . C26 C 0.2470(3) 0.5870(2) 0.1312(2) 0.0376(8) Uani 1 1 d . . . H26 H 0.2055 0.6374 0.1210 0.045 Uiso 1 1 calc R . . C27 C 0.3719(3) 0.5866(2) 0.0998(3) 0.0421(9) Uani 1 1 d . . . H27 H 0.4125 0.6369 0.0692 0.051 Uiso 1 1 calc R . . C28 C 0.4371(3) 0.5156(2) 0.1118(2) 0.0404(8) Uani 1 1 d . . . H28 H 0.5216 0.5154 0.0905 0.048 Uiso 1 1 calc R . . C29 C 0.3723(3) 0.4445(2) 0.1569(2) 0.0291(7) Uani 1 1 d . . . C30 C 0.5307(3) 0.3326(3) 0.1593(3) 0.0463(10) Uani 1 1 d . . . H30A H 0.5721 0.3614 0.1933 0.069 Uiso 1 1 calc R . . H30B H 0.5713 0.3458 0.0979 0.069 Uiso 1 1 calc R . . H30C H 0.5308 0.2702 0.1725 0.069 Uiso 1 1 calc R . . C31 C 0.1837(3) 0.2224(2) 0.08936(19) 0.0264(7) Uani 1 1 d . . . C32 C 0.2561(3) 0.2897(2) 0.0407(2) 0.0327(7) Uani 1 1 d . . . H32 H 0.2586 0.3438 0.0638 0.039 Uiso 1 1 calc R . . C33 C 0.3235(3) 0.2747(2) -0.0422(2) 0.0398(8) Uani 1 1 d . . . H33 H 0.3730 0.3196 -0.0768 0.048 Uiso 1 1 calc R . . C34 C 0.3211(3) 0.1956(3) -0.0767(2) 0.0436(9) Uani 1 1 d . . . H34 H 0.3699 0.1877 -0.1338 0.052 Uiso 1 1 calc R . . C35 C 0.2501(3) 0.1288(2) -0.0303(2) 0.0390(8) Uani 1 1 d . . . H35 H 0.2481 0.0748 -0.0537 0.047 Uiso 1 1 calc R . . C36 C 0.1812(3) 0.1445(2) 0.0531(2) 0.0285(7) Uani 1 1 d . . . C37 C 0.0627(3) 0.0054(2) 0.1049(2) 0.0392(8) Uani 1 1 d . . . H37A H 0.0292 -0.0250 0.1617 0.059 Uiso 1 1 calc R . . H37B H 0.1319 -0.0262 0.0711 0.059 Uiso 1 1 calc R . . H37C H 0.0024 0.0091 0.0751 0.059 Uiso 1 1 calc R . . C38 C 0.0561(3) 0.13926(19) 0.18389(19) 0.0253(6) Uani 1 1 d . . . C39 C -0.1339(3) 0.3805(2) 0.2015(2) 0.0314(7) Uani 1 1 d . . . H39A H -0.1795 0.4331 0.2214 0.038 Uiso 1 1 calc R . . H39B H -0.1915 0.3330 0.2083 0.038 Uiso 1 1 calc R . . C40 C -0.0631(3) 0.3956(2) 0.1076(2) 0.0352(8) Uani 1 1 d . . . H40A H -0.0142 0.3440 0.0887 0.042 Uiso 1 1 calc R . . H40B H -0.0082 0.4449 0.1007 0.042 Uiso 1 1 calc R . . C41 C -0.1412(3) 0.4140(2) 0.0498(2) 0.0358(8) Uani 1 1 d . . . H41A H -0.0902 0.4163 -0.0110 0.043 Uiso 1 1 calc R . . H41B H -0.1981 0.3656 0.0586 0.043 Uiso 1 1 calc R . . C42 C -0.2103(3) 0.4972(2) 0.0659(2) 0.0397(8) Uani 1 1 d . . . H42A H -0.2660 0.4936 0.1246 0.060 Uiso 1 1 calc R . . H42B H -0.2547 0.5064 0.0245 0.060 Uiso 1 1 calc R . . H42C H -0.1549 0.5453 0.0591 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.75583(9) 0.14243(6) 0.10982(6) 0.0458(2) Uani 1 1 d . . . O2 O 0.7131(3) 0.17736(19) 0.19150(19) 0.0594(8) Uani 1 1 d . . . O3 O 0.8800(4) 0.1568(3) 0.0761(3) 0.1142(17) Uani 1 1 d . . . O4 O 0.7346(5) 0.0529(2) 0.1224(3) 0.1016(15) Uani 1 1 d . . . O5 O 0.7006(4) 0.1818(3) 0.0526(2) 0.0899(12) Uani 1 1 d . . . Cl2 Cl 0.51180(8) 0.35642(6) 0.40687(7) 0.0449(2) Uani 1 1 d . . . O6 O 0.4417(3) 0.3717(2) 0.3516(2) 0.0655(9) Uani 1 1 d . . . O7 O 0.5491(4) 0.4340(3) 0.4273(4) 0.1096(16) Uani 1 1 d . . . O8 O 0.6090(3) 0.3028(2) 0.3707(2) 0.0696(10) Uani 1 1 d . . . O9 O 0.4359(4) 0.3109(3) 0.4825(2) 0.0998(14) Uani 1 1 d . . . Cl3 Cl 0.0517(16) 0.8818(14) 0.3653(14) 0.042(2) Uani 0.528(11) 1 d P A 1 O10 O -0.069(3) 0.8858(15) 0.422(2) 0.056(4) Uani 0.528(11) 1 d P A 1 O11 O 0.0903(10) 0.7952(7) 0.3601(8) 0.066(3) Uani 0.528(11) 1 d P A 1 O12 O 0.1284(5) 0.9280(4) 0.3997(5) 0.058(2) Uani 0.528(11) 1 d P A 1 O13 O 0.0672(8) 0.9220(6) 0.2822(4) 0.080(3) Uani 0.528(11) 1 d P A 1 Cl3' Cl 0.035(2) 0.8747(18) 0.3583(18) 0.053(4) Uani 0.472(11) 1 d P A 2 O10' O -0.070(4) 0.9098(17) 0.414(3) 0.057(5) Uani 0.472(11) 1 d P A 2 O11' O 0.0766(12) 0.8045(8) 0.4002(6) 0.052(2) Uani 0.472(11) 1 d P A 2 O12' O 0.1182(8) 0.9413(5) 0.3278(7) 0.079(4) Uani 0.472(11) 1 d P A 2 O13' O 0.0052(8) 0.8477(6) 0.2867(4) 0.077(3) Uani 0.472(11) 1 d P A 2 N11 N 0.6768(4) 0.7858(3) 0.3046(3) 0.0773(12) Uani 1 1 d . . . C43 C 0.6060(6) 0.6256(3) 0.3199(4) 0.0868(17) Uani 1 1 d . . . H43A H 0.6727 0.5901 0.2891 0.130 Uiso 1 1 calc R . . H43B H 0.5409 0.6213 0.2951 0.130 Uiso 1 1 calc R . . H43C H 0.5783 0.6053 0.3809 0.130 Uiso 1 1 calc R . . C44 C 0.6450(5) 0.7155(3) 0.3119(3) 0.0620(12) Uani 1 1 d . . . N12 N 0.9188(4) 0.6213(3) 0.2023(3) 0.0776(12) Uani 1 1 d . . . C45 C 0.9711(6) 0.7698(5) 0.1242(5) 0.116(3) Uani 1 1 d . . . H45A H 0.9239 0.8135 0.1602 0.174 Uiso 1 1 calc R . . H45B H 0.9538 0.7718 0.0692 0.174 Uiso 1 1 calc R . . H45C H 1.0560 0.7814 0.1134 0.174 Uiso 1 1 calc R . . C46 C 0.9418(4) 0.6874(3) 0.1670(3) 0.0517(10) Uani 1 1 d . . . O1W O 0.7766(2) 0.95978(17) 0.26985(18) 0.0494(7) Uani 1 1 d . . . H1WA H 0.7483 0.9769 0.2321 0.074 Uiso 1 1 d R . . H1WB H 0.7621 0.9070 0.2759 0.074 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0210(2) 0.0229(2) 0.0178(2) -0.00105(16) -0.00542(17) 0.00115(16) O1 0.0293(12) 0.0311(12) 0.0253(11) -0.0001(9) -0.0113(9) 0.0044(9) N1 0.0223(13) 0.0267(13) 0.0227(13) 0.0002(10) -0.0062(11) 0.0014(10) N2 0.0240(13) 0.0254(13) 0.0217(13) -0.0007(10) -0.0061(11) 0.0000(10) N3 0.0247(13) 0.0272(14) 0.0309(15) 0.0020(11) -0.0063(11) -0.0004(11) N4 0.0243(13) 0.0320(14) 0.0276(14) 0.0026(11) -0.0044(11) 0.0007(11) N5 0.0241(13) 0.0265(13) 0.0218(13) -0.0022(10) -0.0084(11) 0.0026(10) N6 0.0352(15) 0.0337(15) 0.0229(14) -0.0038(11) -0.0131(12) 0.0008(12) N7 0.0229(13) 0.0270(13) 0.0206(13) -0.0013(10) -0.0066(10) -0.0005(10) N8 0.0214(13) 0.0323(15) 0.0334(15) 0.0007(11) -0.0049(11) 0.0009(11) N9 0.0262(13) 0.0241(13) 0.0197(12) -0.0008(10) -0.0061(10) 0.0013(10) N10 0.0314(14) 0.0240(13) 0.0269(14) -0.0059(11) -0.0075(11) 0.0023(11) C1 0.0290(17) 0.0357(18) 0.0260(16) -0.0016(13) -0.0125(14) 0.0031(13) C2 0.0272(16) 0.0241(16) 0.0304(17) 0.0047(13) -0.0078(13) 0.0037(12) C3 0.0302(17) 0.0264(16) 0.0230(16) 0.0051(12) -0.0084(13) 0.0003(12) C4 0.0315(17) 0.0248(16) 0.0265(16) -0.0018(12) -0.0075(14) -0.0034(13) C5 0.0224(15) 0.0267(16) 0.0274(16) 0.0013(12) -0.0042(13) 0.0010(12) C6 0.0210(15) 0.0315(17) 0.0259(16) 0.0014(13) -0.0070(13) 0.0026(12) C7 0.0232(16) 0.0341(18) 0.0360(18) 0.0087(14) -0.0124(14) 0.0000(13) C8 0.0308(18) 0.0310(18) 0.054(2) 0.0129(16) -0.0195(17) -0.0053(14) C9 0.0314(19) 0.044(2) 0.064(3) 0.027(2) -0.0208(19) -0.0111(16) C10 0.034(2) 0.061(3) 0.047(2) 0.028(2) -0.0075(18) -0.0060(18) C11 0.0353(19) 0.056(2) 0.0331(19) 0.0104(17) -0.0062(16) 0.0024(17) C12 0.0225(16) 0.0391(19) 0.0304(17) 0.0084(14) -0.0059(14) 0.0009(13) C13 0.046(2) 0.042(2) 0.0322(19) -0.0062(16) -0.0026(16) 0.0043(16) C14 0.0284(16) 0.0279(16) 0.0233(16) 0.0011(12) -0.0095(13) -0.0025(13) C15 0.0291(16) 0.0250(15) 0.0208(15) -0.0036(12) -0.0047(13) -0.0002(12) C16 0.0302(17) 0.0293(17) 0.0347(18) -0.0063(14) -0.0126(14) 0.0019(13) C17 0.0331(18) 0.0332(18) 0.043(2) -0.0098(15) -0.0071(16) 0.0072(14) C18 0.047(2) 0.045(2) 0.037(2) -0.0197(16) -0.0044(17) 0.0105(17) C19 0.052(2) 0.043(2) 0.0283(18) -0.0131(15) -0.0136(17) 0.0032(17) C20 0.0329(17) 0.0298(17) 0.0264(17) -0.0050(13) -0.0077(14) 0.0014(13) C21 0.048(2) 0.048(2) 0.0291(18) -0.0030(15) -0.0219(17) -0.0028(17) C22 0.0223(15) 0.0322(17) 0.0270(16) -0.0007(13) -0.0049(13) 0.0036(13) C23 0.0242(16) 0.0311(17) 0.0217(15) -0.0046(12) -0.0055(13) 0.0025(12) C24 0.0272(16) 0.0267(16) 0.0216(15) -0.0021(12) -0.0095(13) -0.0029(12) C25 0.0279(16) 0.0318(17) 0.0271(16) -0.0039(13) -0.0107(13) -0.0004(13) C26 0.044(2) 0.0321(18) 0.040(2) 0.0030(15) -0.0185(17) -0.0035(15) C27 0.041(2) 0.0347(19) 0.048(2) 0.0092(16) -0.0113(17) -0.0103(16) C28 0.0282(18) 0.043(2) 0.045(2) 0.0039(16) -0.0057(16) -0.0101(15) C29 0.0274(16) 0.0324(17) 0.0270(16) -0.0008(13) -0.0076(13) -0.0017(13) C30 0.0253(18) 0.051(2) 0.053(2) 0.0071(18) -0.0010(17) 0.0063(16) C31 0.0266(16) 0.0306(16) 0.0207(15) -0.0024(12) -0.0057(13) 0.0038(13) C32 0.0375(19) 0.0316(18) 0.0276(17) -0.0011(13) -0.0080(14) -0.0024(14) C33 0.040(2) 0.046(2) 0.0265(18) 0.0005(15) -0.0001(15) -0.0066(16) C34 0.044(2) 0.054(2) 0.0235(17) -0.0055(16) 0.0043(16) 0.0017(17) C35 0.047(2) 0.039(2) 0.0288(18) -0.0123(15) -0.0064(16) 0.0052(16) C36 0.0309(17) 0.0312(17) 0.0229(16) -0.0009(13) -0.0078(13) 0.0022(13) C37 0.051(2) 0.0307(18) 0.0349(19) -0.0088(15) -0.0108(17) -0.0016(15) C38 0.0271(16) 0.0254(16) 0.0235(16) -0.0019(12) -0.0082(13) 0.0005(12) C39 0.0265(16) 0.0392(19) 0.0302(17) 0.0051(14) -0.0131(14) 0.0021(14) C40 0.0306(18) 0.048(2) 0.0272(17) 0.0011(15) -0.0093(14) 0.0054(15) C41 0.0366(19) 0.045(2) 0.0276(17) 0.0013(15) -0.0134(15) 0.0019(15) C42 0.041(2) 0.044(2) 0.0348(19) 0.0069(16) -0.0148(16) 0.0025(16) Cl1 0.0581(6) 0.0417(5) 0.0382(5) -0.0078(4) -0.0156(4) 0.0168(4) O2 0.075(2) 0.0537(18) 0.0501(17) -0.0187(14) -0.0181(16) 0.0134(15) O3 0.060(2) 0.168(5) 0.093(3) 0.016(3) 0.002(2) 0.026(3) O4 0.189(5) 0.047(2) 0.084(3) -0.0184(18) -0.062(3) 0.003(2) O5 0.119(3) 0.100(3) 0.067(2) -0.012(2) -0.053(2) 0.046(2) Cl2 0.0329(5) 0.0501(5) 0.0597(6) -0.0256(5) -0.0220(4) 0.0125(4) O6 0.0459(17) 0.096(2) 0.066(2) -0.0123(18) -0.0315(16) -0.0016(16) O7 0.094(3) 0.083(3) 0.186(5) -0.068(3) -0.081(3) 0.014(2) O8 0.0366(16) 0.0556(19) 0.105(3) -0.0184(18) -0.0024(17) 0.0174(13) O9 0.075(3) 0.162(4) 0.057(2) -0.004(2) -0.015(2) 0.042(3) Cl3 0.044(3) 0.042(6) 0.036(3) 0.013(4) -0.010(2) 0.011(3) O10 0.043(5) 0.063(13) 0.051(5) 0.014(10) -0.002(4) 0.011(9) O11 0.061(5) 0.041(4) 0.088(8) 0.004(6) -0.014(6) 0.014(3) O12 0.051(4) 0.054(4) 0.075(5) -0.001(3) -0.028(3) -0.006(3) O13 0.097(6) 0.088(7) 0.046(4) 0.015(4) -0.017(4) 0.031(5) Cl3' 0.071(9) 0.039(2) 0.043(4) 0.003(2) -0.012(4) 0.003(5) O10' 0.060(6) 0.045(11) 0.061(10) 0.008(8) -0.012(6) 0.017(8) O11' 0.067(5) 0.044(5) 0.039(5) -0.002(4) -0.011(5) 0.018(3) O12' 0.084(6) 0.049(4) 0.082(9) 0.001(5) 0.003(6) -0.006(4) O13' 0.100(6) 0.092(7) 0.045(4) -0.003(4) -0.029(4) 0.009(5) N11 0.094(3) 0.064(3) 0.075(3) -0.003(2) -0.027(3) -0.003(2) C43 0.106(5) 0.069(4) 0.081(4) -0.016(3) -0.019(3) -0.006(3) C44 0.072(3) 0.060(3) 0.053(3) -0.002(2) -0.019(2) -0.005(2) N12 0.084(3) 0.080(3) 0.068(3) -0.019(2) -0.019(2) 0.013(3) C45 0.089(5) 0.106(5) 0.141(7) 0.045(5) -0.030(5) 0.007(4) C46 0.050(2) 0.055(3) 0.048(2) -0.002(2) -0.013(2) 0.009(2) O1W 0.0543(17) 0.0415(15) 0.0527(17) -0.0096(12) -0.0151(14) -0.0077(12) _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 1.781(2) . ? Fe1 N5 2.082(3) . ? Fe1 N7 2.083(2) . ? Fe1 N9 2.131(2) . ? Fe1 N2 2.298(2) . ? Fe1 N1 2.325(2) . ? O1 C39 1.400(4) . ? N1 C2 1.482(4) . ? N1 C22 1.484(4) . ? N1 C1 1.486(4) . ? N2 C5 1.487(4) . ? N2 C3 1.490(4) . ? N2 C4 1.491(4) . ? N3 C6 1.334(4) . ? N3 C7 1.387(4) . ? N3 H3 0.8800 . ? N4 C6 1.331(4) . ? N4 C12 1.392(4) . ? N4 C13 1.469(4) . ? N5 C14 1.322(4) . ? N5 C15 1.401(4) . ? N6 C14 1.332(4) . ? N6 C20 1.391(4) . ? N6 C21 1.463(4) . ? N7 C23 1.332(4) . ? N7 C24 1.397(4) . ? N8 C23 1.343(4) . ? N8 C29 1.398(4) . ? N8 C30 1.461(4) . ? N9 C38 1.325(4) . ? N9 C31 1.401(4) . ? N10 C38 1.340(4) . ? N10 C36 1.389(4) . ? N10 C37 1.465(4) . ? C1 C14 1.486(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.521(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C38 1.482(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.501(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C12 1.381(5) . ? C7 C8 1.393(5) . ? C8 C9 1.381(5) . ? C8 H8 0.9500 . ? C9 C10 1.376(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(6) . ? C10 H10 0.9500 . ? C11 C12 1.394(5) . ? C11 H11 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.391(4) . ? C15 C20 1.396(4) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.400(5) . ? C17 H17 0.9500 . ? C18 C19 1.371(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.493(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 C25 1.385(4) . ? C24 C29 1.401(4) . ? C25 C26 1.382(5) . ? C25 H25 0.9500 . ? C26 C27 1.404(5) . ? C26 H26 0.9500 . ? C27 C28 1.374(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.391(4) . ? C31 C32 1.398(4) . ? C32 C33 1.377(5) . ? C32 H32 0.9500 . ? C33 C34 1.393(5) . ? C33 H33 0.9500 . ? C34 C35 1.374(5) . ? C34 H34 0.9500 . ? C35 C36 1.391(5) . ? C35 H35 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 C40 1.509(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.523(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.514(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Cl1 O5 1.401(3) . ? Cl1 O4 1.409(4) . ? Cl1 O3 1.414(4) . ? Cl1 O2 1.418(3) . ? Cl2 O7 1.388(4) . ? Cl2 O8 1.409(3) . ? Cl2 O6 1.409(3) . ? Cl2 O9 1.431(4) . ? Cl3 O11 1.42(2) . ? Cl3 O13 1.42(2) . ? Cl3 O12 1.43(2) . ? Cl3 O10 1.44(3) . ? Cl3' O12' 1.40(3) . ? Cl3' O11' 1.41(3) . ? Cl3' O13' 1.41(3) . ? Cl3' O10' 1.42(4) . ? N11 C44 1.148(6) . ? C43 C44 1.464(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N12 C46 1.139(6) . ? C45 C46 1.412(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O1W H1WA 0.8169 . ? O1W H1WB 0.8346 . ? 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 N5 95.91(10) . . ? O1 Fe1 N7 107.14(10) . . ? N5 Fe1 N7 95.88(10) . . ? O1 Fe1 N9 100.46(10) . . ? N5 Fe1 N9 160.21(10) . . ? N7 Fe1 N9 89.87(10) . . ? O1 Fe1 N2 101.71(9) . . ? N5 Fe1 N2 89.34(9) . . ? N7 Fe1 N2 149.93(9) . . ? N9 Fe1 N2 76.57(9) . . ? O1 Fe1 N1 172.53(9) . . ? N5 Fe1 N1 76.62(9) . . ? N7 Fe1 N1 73.94(9) . . ? N9 Fe1 N1 86.89(9) . . ? N2 Fe1 N1 78.57(9) . . ? C39 O1 Fe1 152.2(2) . . ? C2 N1 C22 113.7(2) . . ? C2 N1 C1 111.3(2) . . ? C22 N1 C1 109.7(2) . . ? C2 N1 Fe1 107.11(17) . . ? C22 N1 Fe1 105.92(17) . . ? C1 N1 Fe1 108.91(18) . . ? C5 N2 C3 112.2(2) . . ? C5 N2 C4 111.2(2) . . ? C3 N2 C4 110.8(2) . . ? C5 N2 Fe1 106.27(17) . . ? C3 N2 Fe1 105.08(17) . . ? C4 N2 Fe1 111.10(17) . . ? C6 N3 C7 108.9(3) . . ? C6 N3 H3 125.5 . . ? C7 N3 H3 125.5 . . ? C6 N4 C12 108.7(3) . . ? C6 N4 C13 127.1(3) . . ? C12 N4 C13 124.2(3) . . ? C14 N5 C15 105.7(2) . . ? C14 N5 Fe1 117.4(2) . . ? C15 N5 Fe1 136.5(2) . . ? C14 N6 C20 107.0(3) . . ? C14 N6 C21 126.6(3) . . ? C20 N6 C21 126.4(3) . . ? C23 N7 C24 106.0(2) . . ? C23 N7 Fe1 116.1(2) . . ? C24 N7 Fe1 136.7(2) . . ? C23 N8 C29 107.3(3) . . ? C23 N8 C30 127.1(3) . . ? C29 N8 C30 125.6(3) . . ? C38 N9 C31 105.0(2) . . ? C38 N9 Fe1 117.1(2) . . ? C31 N9 Fe1 137.8(2) . . ? C38 N10 C36 106.7(3) . . ? C38 N10 C37 127.2(3) . . ? C36 N10 C37 126.0(3) . . ? C14 C1 N1 110.6(2) . . ? C14 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C14 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 C3 109.9(2) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 110.6(2) . . ? N2 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C38 C4 N2 110.5(2) . . ? C38 C4 H4A 109.6 . . ? N2 C4 H4A 109.6 . . ? C38 C4 H4B 109.6 . . ? N2 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N2 C5 C6 115.2(2) . . ? N2 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N2 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N4 C6 N3 109.3(3) . . ? N4 C6 C5 123.5(3) . . ? N3 C6 C5 127.2(3) . . ? C12 C7 N3 106.5(3) . . ? C12 C7 C8 121.6(3) . . ? N3 C7 C8 131.9(3) . . ? C9 C8 C7 116.1(4) . . ? C9 C8 H8 122.0 . . ? C7 C8 H8 122.0 . . ? C10 C9 C8 122.2(4) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 122.3(4) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 115.7(4) . . ? C10 C11 H11 122.1 . . ? C12 C11 H11 122.1 . . ? C7 C12 N4 106.6(3) . . ? C7 C12 C11 122.1(3) . . ? N4 C12 C11 131.3(3) . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 N6 113.1(3) . . ? N5 C14 C1 122.4(3) . . ? N6 C14 C1 124.5(3) . . ? C16 C15 C20 120.7(3) . . ? C16 C15 N5 131.3(3) . . ? C20 C15 N5 107.9(3) . . ? C17 C16 C15 116.6(3) . . ? C17 C16 H16 121.7 . . ? C15 C16 H16 121.7 . . ? C16 C17 C18 121.8(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 121.9(3) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 116.2(3) . . ? C18 C19 H19 121.9 . . ? C20 C19 H19 121.9 . . ? C19 C20 N6 131.1(3) . . ? C19 C20 C15 122.7(3) . . ? N6 C20 C15 106.2(3) . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 106.6(2) . . ? N1 C22 H22A 110.4 . . ? C23 C22 H22A 110.4 . . ? N1 C22 H22B 110.4 . . ? C23 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? N7 C23 N8 112.5(3) . . ? N7 C23 C22 120.7(3) . . ? N8 C23 C22 126.8(3) . . ? C25 C24 N7 130.7(3) . . ? C25 C24 C29 120.9(3) . . ? N7 C24 C29 108.5(3) . . ? C26 C25 C24 116.8(3) . . ? C26 C25 H25 121.6 . . ? C24 C25 H25 121.6 . . ? C25 C26 C27 121.7(3) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 122.0(3) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 116.0(3) . . ? C27 C28 H28 122.0 . . ? C29 C28 H28 122.0 . . ? C28 C29 N8 131.6(3) . . ? C28 C29 C24 122.6(3) . . ? N8 C29 C24 105.8(3) . . ? N8 C30 H30A 109.5 . . ? N8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.7(3) . . ? C36 C31 N9 108.7(3) . . ? C32 C31 N9 131.6(3) . . ? C33 C32 C31 117.4(3) . . ? C33 C32 H32 121.3 . . ? C31 C32 H32 121.3 . . ? C32 C33 C34 121.9(3) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C35 C34 C33 121.8(3) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C36 116.2(3) . . ? C34 C35 H35 121.9 . . ? C36 C35 H35 121.9 . . ? N10 C36 C31 106.2(3) . . ? N10 C36 C35 130.8(3) . . ? C31 C36 C35 123.0(3) . . ? N10 C37 H37A 109.5 . . ? N10 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N10 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N9 C38 N10 113.4(3) . . ? N9 C38 C4 122.2(3) . . ? N10 C38 C4 124.4(3) . . ? O1 C39 C40 111.9(3) . . ? O1 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O1 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 113.0(3) . . ? C39 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C42 C41 C40 114.0(3) . . ? C42 C41 H41A 108.8 . . ? C40 C41 H41A 108.8 . . ? C42 C41 H41B 108.8 . . ? C40 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O5 Cl1 O4 112.1(3) . . ? O5 Cl1 O3 108.9(3) . . ? O4 Cl1 O3 108.5(3) . . ? O5 Cl1 O2 110.7(2) . . ? O4 Cl1 O2 107.5(2) . . ? O3 Cl1 O2 109.0(3) . . ? O7 Cl2 O8 111.4(2) . . ? O7 Cl2 O6 110.2(2) . . ? O8 Cl2 O6 111.4(2) . . ? O7 Cl2 O9 110.5(3) . . ? O8 Cl2 O9 107.7(2) . . ? O6 Cl2 O9 105.5(2) . . ? O11 Cl3 O13 110.9(16) . . ? O11 Cl3 O12 107.7(12) . . ? O13 Cl3 O12 105.2(14) . . ? O11 Cl3 O10 110.1(17) . . ? O13 Cl3 O10 113.2(17) . . ? O12 Cl3 O10 109(2) . . ? O12' Cl3' O11' 113.1(17) . . ? O12' Cl3' O13' 107.1(19) . . ? O11' Cl3' O13' 110(2) . . ? O12' Cl3' O10' 108(2) . . ? O11' Cl3' O10' 111(2) . . ? O13' Cl3' O10' 107(2) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N11 C44 C43 179.1(6) . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N12 C46 C45 179.1(6) . . ? H1WA O1W H1WB 103.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.815 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.070 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.500 1.000 0.000 289 50 2(CH3CN) _platon_squeeze_details ; The unit cell contains another 2 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; #Complex 3 data_Fe(OEt)(Hmedtb).(ClO4)3.MeCN _database_code_depnum_ccdc_archive 'CCDC 804327' #TrackingRef '- cifs.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H49 Cl3 Fe N11 O13' _chemical_formula_weight 1078.12 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.386(3) _cell_length_b 14.209(2) _cell_length_c 14.775(3) _cell_angle_alpha 73.413(16) _cell_angle_beta 72.856(14) _cell_angle_gamma 75.288(16) _cell_volume 2339.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7534 _cell_measurement_theta_min 1.7510 _cell_measurement_theta_max 27.4512 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8475 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26006 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8227 _reflns_number_gt 7226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1295P)^2^+3.3660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8227 _refine_ls_number_parameters 714 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.2217 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.05146(6) 0.26040(5) 0.29895(5) 0.0273(2) Uani 1 1 d . A . O1 O 0.1519(3) 0.1703(3) 0.3617(3) 0.0387(9) Uani 1 1 d . . . N1 N -0.0699(3) 0.3894(3) 0.2211(3) 0.0300(9) Uani 1 1 d . . . N2 N 0.1745(3) 0.3106(3) 0.1473(3) 0.0301(9) Uani 1 1 d . . . N3 N 0.3408(4) 0.4753(3) 0.0130(3) 0.0342(9) Uani 1 1 d . A . H3 H 0.2843 0.5226 0.0322 0.041 Uiso 1 1 calc R . . N4 N 0.4517(4) 0.3293(3) 0.0125(3) 0.0351(10) Uani 1 1 d . A . N5 N 0.0725(3) 0.3850(3) 0.3348(3) 0.0276(8) Uani 1 1 d . . . N6 N 0.0283(3) 0.5462(3) 0.3364(3) 0.0316(9) Uani 1 1 d . . . N7 N -0.1096(3) 0.2579(3) 0.3957(3) 0.0303(9) Uani 1 1 d . . . N8 N -0.2949(3) 0.3243(3) 0.4349(3) 0.0316(9) Uani 1 1 d . . . N9 N 0.0380(3) 0.1680(3) 0.2144(3) 0.0317(9) Uani 1 1 d . . . N10 N 0.1206(4) 0.0893(3) 0.0936(3) 0.0334(9) Uani 1 1 d . . . C1 C -0.0755(4) 0.4859(3) 0.2471(4) 0.0298(10) Uani 1 1 d . A . H1A H -0.0597 0.5385 0.1869 0.036 Uiso 1 1 calc R . . H1B H -0.1538 0.5076 0.2855 0.036 Uiso 1 1 calc R . . C2 C -0.0216(4) 0.3940(4) 0.1167(3) 0.0330(11) Uani 1 1 d . A . H2A H -0.0627 0.4539 0.0783 0.040 Uiso 1 1 calc R . . H2B H -0.0314 0.3342 0.1005 0.040 Uiso 1 1 calc R . . C3 C 0.1052(4) 0.3986(4) 0.0913(4) 0.0330(11) Uani 1 1 d . A . H3A H 0.1369 0.4019 0.0209 0.040 Uiso 1 1 calc R . . H3B H 0.1134 0.4607 0.1043 0.040 Uiso 1 1 calc R . . C4 C 0.2779(4) 0.3388(4) 0.1574(4) 0.0327(11) Uani 1 1 d . A . H4A H 0.3219 0.2793 0.1939 0.039 Uiso 1 1 calc R . . H4B H 0.2520 0.3902 0.1964 0.039 Uiso 1 1 calc R . . C5 C 0.4268(4) 0.4888(4) -0.0721(4) 0.0363(12) Uani 1 1 d . . . C6 C 0.4487(5) 0.5716(4) -0.1471(4) 0.0383(12) Uani 1 1 d . . . H6 H 0.4012 0.6356 -0.1464 0.046 Uiso 1 1 calc R . . C7 C 0.5429(5) 0.5561(5) -0.2224(4) 0.0434(13) Uani 1 1 d . . . H7 H 0.5601 0.6105 -0.2759 0.052 Uiso 1 1 calc R . . C8 C 0.6135(5) 0.4628(5) -0.2223(4) 0.0453(14) Uani 1 1 d . . . H8 H 0.6779 0.4558 -0.2757 0.054 Uiso 1 1 calc R . . C9 C 0.5937(4) 0.3803(4) -0.1479(4) 0.0409(13) Uani 1 1 d . . . H9 H 0.6429 0.3170 -0.1481 0.049 Uiso 1 1 calc R . . C10 C 0.4970(4) 0.3954(4) -0.0722(4) 0.0354(12) Uani 1 1 d . . . C11 C 0.5061(5) 0.2231(4) 0.0393(5) 0.0496(14) Uani 1 1 d . . . H11A H 0.4769 0.1965 0.1089 0.074 Uiso 1 1 calc R . . H11B H 0.5896 0.2175 0.0247 0.074 Uiso 1 1 calc R . . H11C H 0.4877 0.1848 0.0019 0.074 Uiso 1 1 calc R . . C12 C 0.3568(4) 0.3784(4) 0.0623(4) 0.0320(11) Uani 1 1 d . . . C13 C 0.0093(4) 0.4733(3) 0.3042(3) 0.0292(10) Uani 1 1 d . A . C14 C 0.1365(4) 0.4011(4) 0.3918(3) 0.0282(10) Uani 1 1 d . A . C15 C 0.2159(4) 0.3361(4) 0.4395(4) 0.0353(11) Uani 1 1 d . . . H15 H 0.2370 0.2675 0.4373 0.042 Uiso 1 1 calc R A . C16 C 0.2638(5) 0.3763(4) 0.4913(4) 0.0408(13) Uani 1 1 d . A . H16 H 0.3185 0.3337 0.5258 0.049 Uiso 1 1 calc R . . C17 C 0.2334(5) 0.4776(5) 0.4937(4) 0.0435(13) Uani 1 1 d . . . H17 H 0.2674 0.5021 0.5301 0.052 Uiso 1 1 calc R A . C18 C 0.1552(5) 0.5422(4) 0.4444(4) 0.0390(12) Uani 1 1 d . A . H18 H 0.1347 0.6110 0.4458 0.047 Uiso 1 1 calc R . . C19 C 0.1078(4) 0.5026(4) 0.3927(3) 0.0307(10) Uani 1 1 d . A . C20 C -0.0205(5) 0.6533(4) 0.3132(4) 0.0406(13) Uani 1 1 d . A . H20A H 0.0400 0.6902 0.2713 0.061 Uiso 1 1 calc R . . H20B H -0.0527 0.6771 0.3735 0.061 Uiso 1 1 calc R . . H20C H -0.0814 0.6642 0.2794 0.061 Uiso 1 1 calc R . . C21 C -0.1488(4) 0.2283(4) 0.4960(3) 0.0302(10) Uani 1 1 d . A . C22 C -0.0903(5) 0.1725(4) 0.5670(4) 0.0354(11) Uani 1 1 d . . . H22 H -0.0106 0.1453 0.5504 0.043 Uiso 1 1 calc R A . C23 C -0.1528(5) 0.1583(4) 0.6628(4) 0.0465(14) Uani 1 1 d . A . H23 H -0.1153 0.1199 0.7128 0.056 Uiso 1 1 calc R . . C24 C -0.2701(6) 0.1992(4) 0.6876(4) 0.0487(15) Uani 1 1 d . . . H24 H -0.3102 0.1879 0.7542 0.058 Uiso 1 1 calc R A . C25 C -0.3296(5) 0.2558(4) 0.6174(4) 0.0443(13) Uani 1 1 d . A . H25 H -0.4091 0.2837 0.6341 0.053 Uiso 1 1 calc R . . C26 C -0.2664(4) 0.2689(4) 0.5224(4) 0.0337(11) Uani 1 1 d . A . C27 C -0.4095(5) 0.3816(4) 0.4279(4) 0.0439(13) Uani 1 1 d . A . H27A H -0.4036 0.4329 0.3670 0.066 Uiso 1 1 calc R . . H27B H -0.4433 0.4136 0.4831 0.066 Uiso 1 1 calc R . . H27C H -0.4584 0.3366 0.4291 0.066 Uiso 1 1 calc R . . C28 C -0.1999(4) 0.3145(4) 0.3629(4) 0.0312(11) Uani 1 1 d . A . C29 C -0.1858(4) 0.3607(4) 0.2565(3) 0.0302(10) Uani 1 1 d . A . H29A H -0.1905 0.3123 0.2217 0.036 Uiso 1 1 calc R . . H29B H -0.2466 0.4204 0.2456 0.036 Uiso 1 1 calc R . . C30 C -0.0231(4) 0.0918(4) 0.2265(4) 0.0336(11) Uani 1 1 d . A . C31 C -0.1160(5) 0.0614(4) 0.2982(4) 0.0390(12) Uani 1 1 d . . . H31 H -0.1513 0.0937 0.3506 0.047 Uiso 1 1 calc R A . C32 C -0.1556(5) -0.0186(4) 0.2906(4) 0.0461(14) Uani 1 1 d . A . H32 H -0.2199 -0.0410 0.3384 0.055 Uiso 1 1 calc R . . C33 C -0.1030(5) -0.0667(4) 0.2141(4) 0.0460(14) Uani 1 1 d . . . H33 H -0.1314 -0.1220 0.2120 0.055 Uiso 1 1 calc R A . C34 C -0.0114(5) -0.0363(4) 0.1416(4) 0.0420(13) Uani 1 1 d . A . H34 H 0.0229 -0.0679 0.0886 0.050 Uiso 1 1 calc R . . C35 C 0.0284(5) 0.0431(4) 0.1500(4) 0.0363(12) Uani 1 1 d . A . C36 C 0.2004(5) 0.0638(5) 0.0058(4) 0.0490(14) Uani 1 1 d . A . H36A H 0.1913 0.1196 -0.0501 0.074 Uiso 1 1 calc R . . H36B H 0.1843 0.0041 -0.0046 0.074 Uiso 1 1 calc R . . H36C H 0.2794 0.0504 0.0131 0.074 Uiso 1 1 calc R . . C37 C 0.1209(4) 0.1614(3) 0.1350(3) 0.0305(10) Uani 1 1 d . A . C38 C 0.2117(4) 0.2249(4) 0.0989(4) 0.0350(11) Uani 1 1 d . A . H38A H 0.2850 0.1844 0.1133 0.042 Uiso 1 1 calc R . . H38B H 0.2244 0.2502 0.0275 0.042 Uiso 1 1 calc R . . C39 C 0.234(2) 0.0817(14) 0.3500(16) 0.055(6) Uani 0.53(4) 1 d P A 1 H39A H 0.3062 0.1007 0.3063 0.066 Uiso 0.53(4) 1 calc PR A 1 H39B H 0.2051 0.0445 0.3171 0.066 Uiso 0.53(4) 1 calc PR A 1 C40 C 0.259(5) 0.014(5) 0.440(4) 0.061(10) Uani 0.53(4) 1 d P A 1 H40A H 0.3027 -0.0503 0.4266 0.091 Uiso 0.53(4) 1 calc PR A 1 H40B H 0.1870 0.0043 0.4886 0.091 Uiso 0.53(4) 1 calc PR A 1 H40C H 0.3047 0.0435 0.4650 0.091 Uiso 0.53(4) 1 calc PR A 1 C39' C 0.175(2) 0.0622(11) 0.3863(17) 0.046(5) Uani 0.47(4) 1 d P A 2 H39C H 0.1935 0.0358 0.3272 0.055 Uiso 0.47(4) 1 calc PR A 2 H39D H 0.1072 0.0364 0.4326 0.055 Uiso 0.47(4) 1 calc PR A 2 C40' C 0.274(6) 0.032(6) 0.431(5) 0.067(14) Uani 0.47(4) 1 d P A 2 H40D H 0.2968 -0.0406 0.4444 0.101 Uiso 0.47(4) 1 calc PR A 2 H40E H 0.2519 0.0546 0.4918 0.101 Uiso 0.47(4) 1 calc PR A 2 H40F H 0.3378 0.0629 0.3861 0.101 Uiso 0.47(4) 1 calc PR A 2 Cl1 Cl 0.54065(18) 0.16748(14) 0.3507(2) 0.0487(8) Uani 0.790(7) 1 d P B 1 O2 O 0.6367(7) 0.2187(9) 0.3104(9) 0.056(3) Uani 0.790(7) 1 d P B 1 O3 O 0.4653(6) 0.2033(5) 0.4327(6) 0.092(3) Uani 0.790(7) 1 d P B 1 O4 O 0.478(3) 0.189(4) 0.279(3) 0.103(9) Uani 0.790(7) 1 d P B 1 O5 O 0.579(3) 0.064(2) 0.3839(14) 0.069(4) Uani 0.790(7) 1 d P B 1 Cl1' Cl 0.5810(11) 0.1632(7) 0.2797(10) 0.072(4) Uani 0.210(7) 1 d P B 2 O2' O 0.633(6) 0.238(4) 0.283(5) 0.13(3) Uani 0.210(7) 1 d P B 2 O3' O 0.640(3) 0.117(2) 0.197(2) 0.094(10) Uani 0.210(7) 1 d P B 2 O4' O 0.468(13) 0.191(14) 0.271(12) 0.11(3) Uani 0.210(7) 1 d P B 2 O5' O 0.581(11) 0.075(7) 0.353(5) 0.066(16) Uani 0.210(7) 1 d P B 2 Cl2 Cl 0.67583(11) 0.67219(10) 0.19993(9) 0.0389(3) Uani 1 1 d . . . O6 O 0.7310(4) 0.6062(3) 0.1352(3) 0.0541(11) Uani 1 1 d . . . O7 O 0.7581(4) 0.7228(3) 0.2062(4) 0.0728(15) Uani 1 1 d . . . O8 O 0.6325(5) 0.6143(4) 0.2945(3) 0.0762(15) Uani 1 1 d . . . O9 O 0.5846(4) 0.7425(3) 0.1648(4) 0.0679(14) Uani 1 1 d . . . Cl3 Cl 0.13873(11) 0.70997(10) 0.04308(10) 0.0431(4) Uani 1 1 d . . . O10 O 0.1538(4) 0.6114(3) 0.1077(3) 0.0585(12) Uani 1 1 d . . . O11 O 0.2061(4) 0.7000(5) -0.0513(3) 0.0793(16) Uani 1 1 d . . . O12 O 0.1781(4) 0.7756(3) 0.0768(4) 0.0737(15) Uani 1 1 d . . . O13 O 0.0221(4) 0.7440(4) 0.0422(4) 0.0704(14) Uani 1 1 d . . . N11 N 0.4087(8) 1.0013(6) 0.1385(7) 0.109(3) Uani 1 1 d . C . C41 C 0.4717(7) 0.9712(6) 0.1867(8) 0.082(3) Uani 1 1 d . . . C42 C 0.572(6) 0.958(5) 0.222(6) 0.078(16) Uani 0.31(9) 1 d P C 1 H42A H 0.5541 0.9338 0.2925 0.117 Uiso 0.31(9) 1 calc PR C 1 H42B H 0.5982 1.0219 0.2042 0.117 Uiso 0.31(9) 1 calc PR C 1 H42C H 0.6336 0.9090 0.1919 0.117 Uiso 0.31(9) 1 calc PR C 1 C42' C 0.543(2) 0.924(3) 0.257(3) 0.083(8) Uani 0.69(9) 1 d P C 2 H42D H 0.6187 0.8928 0.2241 0.124 Uiso 0.69(9) 1 calc PR C 2 H42E H 0.5057 0.8739 0.3087 0.124 Uiso 0.69(9) 1 calc PR C 2 H42F H 0.5521 0.9756 0.2855 0.124 Uiso 0.69(9) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0284(4) 0.0267(4) 0.0298(4) -0.0102(3) -0.0083(3) -0.0048(3) O1 0.043(2) 0.0318(19) 0.048(2) -0.0145(16) -0.0232(17) 0.0026(16) N1 0.034(2) 0.029(2) 0.030(2) -0.0087(17) -0.0091(17) -0.0082(18) N2 0.028(2) 0.027(2) 0.035(2) -0.0092(17) -0.0061(17) -0.0056(17) N3 0.030(2) 0.040(2) 0.035(2) -0.0151(19) -0.0024(17) -0.0101(19) N4 0.031(2) 0.041(2) 0.037(2) -0.016(2) -0.0060(18) -0.0068(19) N5 0.028(2) 0.029(2) 0.028(2) -0.0100(17) -0.0049(16) -0.0064(17) N6 0.032(2) 0.027(2) 0.036(2) -0.0119(17) -0.0035(18) -0.0070(17) N7 0.033(2) 0.028(2) 0.034(2) -0.0090(17) -0.0109(18) -0.0061(18) N8 0.028(2) 0.035(2) 0.035(2) -0.0128(18) -0.0066(17) -0.0067(18) N9 0.035(2) 0.031(2) 0.032(2) -0.0118(18) -0.0097(18) -0.0040(18) N10 0.035(2) 0.035(2) 0.035(2) -0.0141(18) -0.0094(18) -0.0044(19) C1 0.029(2) 0.026(2) 0.034(3) -0.007(2) -0.007(2) -0.006(2) C2 0.035(3) 0.038(3) 0.025(2) -0.003(2) -0.008(2) -0.007(2) C3 0.033(3) 0.033(3) 0.029(3) -0.002(2) -0.005(2) -0.008(2) C4 0.026(2) 0.042(3) 0.035(3) -0.014(2) -0.008(2) -0.008(2) C5 0.027(3) 0.046(3) 0.038(3) -0.014(2) -0.002(2) -0.012(2) C6 0.037(3) 0.045(3) 0.038(3) -0.012(2) -0.009(2) -0.012(2) C7 0.039(3) 0.064(4) 0.031(3) -0.011(3) -0.004(2) -0.023(3) C8 0.033(3) 0.073(4) 0.034(3) -0.020(3) 0.000(2) -0.017(3) C9 0.027(3) 0.057(3) 0.045(3) -0.028(3) -0.002(2) -0.009(2) C10 0.030(3) 0.052(3) 0.032(3) -0.019(2) -0.005(2) -0.013(2) C11 0.041(3) 0.043(3) 0.065(4) -0.017(3) -0.011(3) -0.005(3) C12 0.029(3) 0.035(3) 0.036(3) -0.012(2) -0.008(2) -0.009(2) C13 0.027(2) 0.031(2) 0.031(2) -0.012(2) -0.0009(19) -0.008(2) C14 0.030(2) 0.037(3) 0.020(2) -0.012(2) 0.0011(18) -0.014(2) C15 0.039(3) 0.038(3) 0.031(3) -0.011(2) -0.010(2) -0.006(2) C16 0.035(3) 0.057(3) 0.036(3) -0.015(3) -0.011(2) -0.012(3) C17 0.046(3) 0.061(4) 0.037(3) -0.024(3) -0.007(2) -0.024(3) C18 0.042(3) 0.048(3) 0.032(3) -0.019(2) 0.002(2) -0.020(3) C19 0.033(3) 0.037(3) 0.024(2) -0.013(2) -0.0011(19) -0.008(2) C20 0.045(3) 0.026(3) 0.052(3) -0.015(2) -0.006(3) -0.007(2) C21 0.038(3) 0.032(3) 0.023(2) -0.012(2) -0.003(2) -0.010(2) C22 0.045(3) 0.029(3) 0.032(3) -0.008(2) -0.008(2) -0.009(2) C23 0.059(4) 0.041(3) 0.038(3) -0.008(3) -0.009(3) -0.010(3) C24 0.079(4) 0.042(3) 0.030(3) -0.010(2) -0.007(3) -0.023(3) C25 0.049(3) 0.048(3) 0.039(3) -0.019(3) 0.000(3) -0.014(3) C26 0.040(3) 0.029(2) 0.035(3) -0.013(2) -0.004(2) -0.010(2) C27 0.034(3) 0.049(3) 0.044(3) -0.017(3) -0.003(2) 0.000(3) C28 0.035(3) 0.032(3) 0.032(3) -0.013(2) -0.005(2) -0.011(2) C29 0.025(2) 0.034(3) 0.034(3) -0.008(2) -0.009(2) -0.007(2) C30 0.038(3) 0.029(2) 0.042(3) -0.009(2) -0.020(2) -0.006(2) C31 0.037(3) 0.041(3) 0.044(3) -0.016(2) -0.009(2) -0.009(2) C32 0.043(3) 0.040(3) 0.058(4) -0.011(3) -0.007(3) -0.018(3) C33 0.055(4) 0.034(3) 0.060(4) -0.015(3) -0.024(3) -0.011(3) C34 0.049(3) 0.034(3) 0.053(3) -0.016(3) -0.026(3) 0.001(2) C35 0.046(3) 0.029(3) 0.045(3) -0.014(2) -0.024(2) -0.004(2) C36 0.052(4) 0.056(4) 0.048(3) -0.028(3) -0.010(3) -0.008(3) C37 0.036(3) 0.028(2) 0.031(3) -0.011(2) -0.012(2) -0.003(2) C38 0.035(3) 0.038(3) 0.035(3) -0.016(2) -0.004(2) -0.007(2) C39 0.046(11) 0.049(8) 0.071(11) -0.023(8) -0.026(9) 0.015(8) C40 0.10(2) 0.03(2) 0.075(16) -0.003(12) -0.061(16) -0.007(14) C39' 0.038(11) 0.040(8) 0.063(11) -0.018(7) -0.017(9) 0.000(7) C40' 0.09(2) 0.03(2) 0.09(2) -0.008(15) -0.039(16) -0.007(14) Cl1 0.0426(11) 0.0448(11) 0.0664(19) -0.0204(10) -0.0203(11) -0.0041(8) O2 0.036(4) 0.058(7) 0.087(6) -0.031(6) -0.016(3) -0.014(4) O3 0.067(4) 0.090(5) 0.121(6) -0.068(5) 0.020(4) -0.022(4) O4 0.102(13) 0.109(15) 0.129(16) 0.012(11) -0.091(13) -0.044(11) O5 0.073(6) 0.058(8) 0.067(11) -0.008(8) -0.021(9) -0.001(5) Cl1' 0.082(7) 0.062(6) 0.079(9) -0.005(5) -0.032(7) -0.021(5) O2' 0.16(5) 0.033(17) 0.15(5) 0.02(2) -0.03(3) -0.03(2) O3' 0.15(3) 0.074(18) 0.075(18) -0.018(15) -0.045(18) -0.021(18) O4' 0.11(7) 0.11(6) 0.11(6) -0.02(5) -0.04(6) -0.03(6) O5' 0.09(3) 0.04(2) 0.07(4) 0.00(3) -0.03(4) -0.012(17) Cl2 0.0361(7) 0.0417(7) 0.0419(7) -0.0150(6) -0.0129(5) -0.0022(6) O6 0.056(3) 0.063(3) 0.047(2) -0.030(2) -0.015(2) 0.006(2) O7 0.051(3) 0.060(3) 0.127(5) -0.034(3) -0.042(3) -0.007(2) O8 0.083(4) 0.074(3) 0.050(3) -0.013(2) 0.008(2) -0.005(3) O9 0.064(3) 0.051(3) 0.109(4) -0.033(3) -0.060(3) 0.017(2) Cl3 0.0385(7) 0.0476(8) 0.0474(8) -0.0229(6) -0.0109(6) -0.0008(6) O10 0.054(3) 0.042(2) 0.071(3) -0.017(2) -0.002(2) -0.004(2) O11 0.067(3) 0.120(4) 0.049(3) -0.040(3) 0.003(2) -0.008(3) O12 0.076(3) 0.049(3) 0.120(4) -0.042(3) -0.046(3) -0.002(2) O13 0.038(2) 0.099(4) 0.080(3) -0.043(3) -0.020(2) 0.008(2) N11 0.103(6) 0.069(5) 0.148(8) 0.011(5) -0.047(6) -0.025(5) C41 0.062(5) 0.048(4) 0.138(8) -0.031(5) -0.028(5) 0.002(4) C42 0.06(3) 0.04(2) 0.14(4) -0.05(2) -0.02(3) -0.005(16) C42' 0.062(11) 0.056(13) 0.15(2) -0.051(13) -0.031(11) -0.009(8) _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 1.800(3) . ? Fe1 N5 2.082(4) . ? Fe1 N7 2.085(4) . ? Fe1 N9 2.118(4) . ? Fe1 N1 2.315(4) . ? Fe1 N2 2.340(4) . ? O1 C39 1.418(14) . ? O1 C39' 1.446(16) . ? N1 C2 1.470(6) . ? N1 C29 1.494(6) . ? N1 C1 1.507(6) . ? N2 C38 1.491(6) . ? N2 C4 1.493(6) . ? N2 C3 1.507(6) . ? N3 C12 1.356(7) . ? N3 C5 1.389(6) . ? N3 H3 0.8800 . ? N4 C12 1.332(6) . ? N4 C10 1.394(7) . ? N4 C11 1.480(7) . ? N5 C13 1.333(6) . ? N5 C14 1.409(6) . ? N6 C13 1.351(6) . ? N6 C19 1.387(6) . ? N6 C20 1.469(6) . ? N7 C28 1.332(6) . ? N7 C21 1.391(6) . ? N8 C28 1.341(6) . ? N8 C26 1.402(6) . ? N8 C27 1.463(7) . ? N9 C37 1.319(6) . ? N9 C30 1.414(6) . ? N10 C37 1.337(6) . ? N10 C35 1.391(7) . ? N10 C36 1.456(7) . ? C1 C13 1.479(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.517(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C12 1.505(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.388(8) . ? C5 C10 1.390(7) . ? C6 C7 1.375(7) . ? C6 H6 0.9500 . ? C7 C8 1.390(9) . ? C7 H7 0.9500 . ? C8 C9 1.376(8) . ? C8 H8 0.9500 . ? C9 C10 1.396(7) . ? C9 H9 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 C15 1.376(7) . ? C14 C19 1.398(7) . ? C15 C16 1.397(7) . ? C15 H15 0.9500 . ? C16 C17 1.400(8) . ? C16 H16 0.9500 . ? C17 C18 1.376(8) . ? C17 H17 0.9500 . ? C18 C19 1.387(7) . ? C18 H18 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.391(7) . ? C21 C26 1.404(7) . ? C22 C23 1.383(7) . ? C22 H22 0.9500 . ? C23 C24 1.401(9) . ? C23 H23 0.9500 . ? C24 C25 1.392(8) . ? C24 H24 0.9500 . ? C25 C26 1.376(7) . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.497(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.380(7) . ? C30 C35 1.401(7) . ? C31 C32 1.392(7) . ? C31 H31 0.9500 . ? C32 C33 1.396(8) . ? C32 H32 0.9500 . ? C33 C34 1.375(8) . ? C33 H33 0.9500 . ? C34 C35 1.389(7) . ? C34 H34 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.501(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.47(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C39' C40' 1.47(7) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? Cl1 O5 1.41(3) . ? Cl1 O4 1.41(3) . ? Cl1 O3 1.429(7) . ? Cl1 O2 1.440(10) . ? Cl1' O4' 1.39(13) . ? Cl1' O2' 1.39(7) . ? Cl1' O5' 1.40(8) . ? Cl1' O3' 1.47(3) . ? Cl2 O9 1.422(4) . ? Cl2 O7 1.425(4) . ? Cl2 O8 1.429(5) . ? Cl2 O6 1.437(4) . ? Cl3 O13 1.405(4) . ? Cl3 O12 1.412(4) . ? Cl3 O11 1.424(5) . ? Cl3 O10 1.455(5) . ? N11 C41 1.132(11) . ? C41 C42 1.44(6) . ? C41 C42' 1.47(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N5 96.70(15) . . ? O1 Fe1 N7 105.87(17) . . ? N5 Fe1 N7 92.76(15) . . ? O1 Fe1 N9 96.62(16) . . ? N5 Fe1 N9 160.06(16) . . ? N7 Fe1 N9 97.77(16) . . ? O1 Fe1 N1 173.85(15) . . ? N5 Fe1 N1 77.26(14) . . ? N7 Fe1 N1 75.89(15) . . ? N9 Fe1 N1 88.92(15) . . ? O1 Fe1 N2 100.41(16) . . ? N5 Fe1 N2 87.10(14) . . ? N7 Fe1 N2 153.54(15) . . ? N9 Fe1 N2 75.94(15) . . ? N1 Fe1 N2 78.29(14) . . ? C39 O1 Fe1 139.0(7) . . ? C39' O1 Fe1 132.3(7) . . ? C2 N1 C29 112.6(4) . . ? C2 N1 C1 112.1(4) . . ? C29 N1 C1 109.8(4) . . ? C2 N1 Fe1 105.3(3) . . ? C29 N1 Fe1 106.1(3) . . ? C1 N1 Fe1 110.5(3) . . ? C38 N2 C4 109.3(4) . . ? C38 N2 C3 111.2(4) . . ? C4 N2 C3 110.7(4) . . ? C38 N2 Fe1 107.6(3) . . ? C4 N2 Fe1 111.6(3) . . ? C3 N2 Fe1 106.3(3) . . ? C12 N3 C5 109.9(4) . . ? C12 N3 H3 125.0 . . ? C5 N3 H3 125.0 . . ? C12 N4 C10 109.0(4) . . ? C12 N4 C11 127.9(5) . . ? C10 N4 C11 123.1(4) . . ? C13 N5 C14 106.6(4) . . ? C13 N5 Fe1 118.2(3) . . ? C14 N5 Fe1 135.1(3) . . ? C13 N6 C19 107.6(4) . . ? C13 N6 C20 127.2(4) . . ? C19 N6 C20 125.1(4) . . ? C28 N7 C21 106.1(4) . . ? C28 N7 Fe1 117.0(3) . . ? C21 N7 Fe1 135.2(3) . . ? C28 N8 C26 107.7(4) . . ? C28 N8 C27 128.3(4) . . ? C26 N8 C27 124.0(4) . . ? C37 N9 C30 104.8(4) . . ? C37 N9 Fe1 116.1(3) . . ? C30 N9 Fe1 137.5(3) . . ? C37 N10 C35 106.9(4) . . ? C37 N10 C36 127.0(4) . . ? C35 N10 C36 126.1(4) . . ? C13 C1 N1 110.6(4) . . ? C13 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C13 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 C3 109.5(4) . . ? N1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? N1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 113.5(4) . . ? N2 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N2 C4 C12 114.3(4) . . ? N2 C4 H4A 108.7 . . ? C12 C4 H4A 108.7 . . ? N2 C4 H4B 108.7 . . ? C12 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 N3 132.7(5) . . ? C6 C5 C10 122.0(5) . . ? N3 C5 C10 105.3(5) . . ? C7 C6 C5 116.4(5) . . ? C7 C6 H6 121.8 . . ? C5 C6 H6 121.8 . . ? C6 C7 C8 121.7(5) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 122.6(5) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 115.9(5) . . ? C8 C9 H9 122.0 . . ? C10 C9 H9 122.0 . . ? C5 C10 N4 107.6(4) . . ? C5 C10 C9 121.4(5) . . ? N4 C10 C9 131.0(5) . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 108.2(4) . . ? N4 C12 C4 128.5(5) . . ? N3 C12 C4 123.3(4) . . ? N5 C13 N6 111.6(4) . . ? N5 C13 C1 122.8(4) . . ? N6 C13 C1 125.4(4) . . ? C15 C14 C19 121.7(4) . . ? C15 C14 N5 130.8(4) . . ? C19 C14 N5 107.5(4) . . ? C14 C15 C16 116.5(5) . . ? C14 C15 H15 121.7 . . ? C16 C15 H15 121.7 . . ? C15 C16 C17 121.7(5) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 121.3(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 117.1(5) . . ? C17 C18 H18 121.4 . . ? C19 C18 H18 121.4 . . ? N6 C19 C18 131.7(5) . . ? N6 C19 C14 106.7(4) . . ? C18 C19 C14 121.6(5) . . ? N6 C20 H20A 109.5 . . ? N6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N7 130.7(5) . . ? C22 C21 C26 120.3(4) . . ? N7 C21 C26 108.9(4) . . ? C23 C22 C21 117.4(5) . . ? C23 C22 H22 121.3 . . ? C21 C22 H22 121.3 . . ? C22 C23 C24 121.4(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 121.8(5) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C26 C25 C24 116.1(5) . . ? C26 C25 H25 122.0 . . ? C24 C25 H25 122.0 . . ? C25 C26 N8 131.9(5) . . ? C25 C26 C21 123.0(5) . . ? N8 C26 C21 105.0(4) . . ? N8 C27 H27A 109.5 . . ? N8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N8 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N7 C28 N8 112.2(4) . . ? N7 C28 C29 119.6(4) . . ? N8 C28 C29 128.1(5) . . ? N1 C29 C28 106.2(4) . . ? N1 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? N1 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C31 C30 C35 120.7(5) . . ? C31 C30 N9 131.0(5) . . ? C35 C30 N9 108.2(4) . . ? C30 C31 C32 117.2(5) . . ? C30 C31 H31 121.4 . . ? C32 C31 H31 121.4 . . ? C31 C32 C33 121.4(5) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 121.9(5) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 116.4(5) . . ? C33 C34 H34 121.8 . . ? C35 C34 H34 121.8 . . ? C34 C35 N10 131.7(5) . . ? C34 C35 C30 122.3(5) . . ? N10 C35 C30 106.0(4) . . ? N10 C36 H36A 109.5 . . ? N10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 N10 114.0(4) . . ? N9 C37 C38 122.6(4) . . ? N10 C37 C38 123.3(4) . . ? N2 C38 C37 109.6(4) . . ? N2 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? N2 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? O1 C39 C40 116(3) . . ? O1 C39 H39A 108.4 . . ? C40 C39 H39A 108.4 . . ? O1 C39 H39B 108.4 . . ? C40 C39 H39B 108.4 . . ? H39A C39 H39B 107.4 . . ? O1 C39' C40' 106(3) . . ? O1 C39' H39C 110.5 . . ? C40' C39' H39C 110.5 . . ? O1 C39' H39D 110.5 . . ? C40' C39' H39D 110.5 . . ? H39C C39' H39D 108.7 . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? O5 Cl1 O4 114(2) . . ? O5 Cl1 O3 107.0(11) . . ? O4 Cl1 O3 107.4(19) . . ? O5 Cl1 O2 110.2(14) . . ? O4 Cl1 O2 108(2) . . ? O3 Cl1 O2 110.7(5) . . ? O4' Cl1' O2' 117(8) . . ? O4' Cl1' O5' 104(10) . . ? O2' Cl1' O5' 120(5) . . ? O4' Cl1' O3' 103(7) . . ? O2' Cl1' O3' 113(3) . . ? O5' Cl1' O3' 97(4) . . ? O9 Cl2 O7 110.1(3) . . ? O9 Cl2 O8 110.2(3) . . ? O7 Cl2 O8 108.6(3) . . ? O9 Cl2 O6 109.7(3) . . ? O7 Cl2 O6 109.3(3) . . ? O8 Cl2 O6 108.9(3) . . ? O13 Cl3 O12 110.3(3) . . ? O13 Cl3 O11 110.6(3) . . ? O12 Cl3 O11 110.6(4) . . ? O13 Cl3 O10 109.8(3) . . ? O12 Cl3 O10 108.4(3) . . ? O11 Cl3 O10 106.9(3) . . ? N11 C41 C42 160(4) . . ? N11 C41 C42' 173(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? C41 C42' H42D 109.5 . . ? C41 C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C41 C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.790 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.069 #Complex 2 data_Fe(OMe)(medtb).(ClO4)2.H2O _database_code_depnum_ccdc_archive 'CCDC 804328' #TrackingRef '- cifs.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H45 Cl2 Fe N10 O10' _chemical_formula_weight 940.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.110(2) _cell_length_b 12.182(3) _cell_length_c 17.153(3) _cell_angle_alpha 93.438(4) _cell_angle_beta 92.457(3) _cell_angle_gamma 91.588(4) _cell_volume 2522.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3773 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.36 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _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 14800 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8800 _reflns_number_gt 6305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1927P)^2^+0.0860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8800 _refine_ls_number_parameters 765 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.2883 _refine_ls_wR_factor_gt 0.2601 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.76306(5) 0.12238(5) 0.28078(4) 0.0532(3) Uani 1 1 d . . . O1 O 0.6430(3) 0.0476(3) 0.3127(2) 0.0693(9) Uani 1 1 d . . . N1 N 0.9275(3) 0.2120(3) 0.2533(2) 0.0569(10) Uani 1 1 d . . . N2 N 0.7140(3) 0.3021(3) 0.2916(2) 0.0585(10) Uani 1 1 d . . . N3 N 0.6049(4) 0.5134(4) 0.3447(3) 0.0728(12) Uani 1 1 d . . . N4 N 0.6468(3) 0.4708(4) 0.4678(3) 0.0604(10) Uani 1 1 d . . . N5 N 0.8450(3) 0.1414(3) 0.3902(2) 0.0566(10) Uani 1 1 d . . . N6 N 0.9998(3) 0.1673(3) 0.4621(3) 0.0618(10) Uani 1 1 d . . . N7 N 0.8685(3) 0.0000(3) 0.2421(2) 0.0580(10) Uani 1 1 d . . . N8 N 1.0087(4) -0.0535(4) 0.1722(3) 0.0817(14) Uani 1 1 d . . . N9 N 0.7020(4) 0.1480(4) 0.1679(2) 0.0642(11) Uani 1 1 d . . . N10 N 0.6047(4) 0.2456(5) 0.0871(3) 0.0804(14) Uani 1 1 d . . . C1 C 0.9692(4) 0.1507(4) 0.1848(3) 0.0655(13) Uani 1 1 d . . . H1A H 1.0474 0.1672 0.1800 0.079 Uiso 1 1 calc R . . H1B H 0.9296 0.1697 0.1374 0.079 Uiso 1 1 calc R . . C2 C 0.8991(4) 0.3253(4) 0.2368(3) 0.0670(14) Uani 1 1 d . . . H2A H 0.8649 0.3262 0.1847 0.080 Uiso 1 1 calc R . . H2B H 0.9657 0.3717 0.2391 0.080 Uiso 1 1 calc R . . C3 C 0.8195(4) 0.3698(4) 0.2967(3) 0.0641(13) Uani 1 1 d . . . H3A H 0.8535 0.3683 0.3489 0.077 Uiso 1 1 calc R . . H3B H 0.8036 0.4456 0.2872 0.077 Uiso 1 1 calc R . . C4 C 0.6536(5) 0.3183(4) 0.3649(3) 0.0677(13) Uani 1 1 d . . . H4A H 0.6945 0.2843 0.4064 0.081 Uiso 1 1 calc R . . H4B H 0.5822 0.2801 0.3576 0.081 Uiso 1 1 calc R . . C5 C 0.6353(4) 0.4355(5) 0.3907(3) 0.0652(13) Uani 1 1 d . . . C6 C 0.5977(4) 0.6058(4) 0.3955(4) 0.0699(14) Uani 1 1 d . . . C7 C 0.5695(5) 0.7134(5) 0.3792(5) 0.0875(19) Uani 1 1 d . . . H7 H 0.5524 0.7315 0.3283 0.105 Uiso 1 1 calc R . . C8 C 0.5677(6) 0.7903(6) 0.4398(6) 0.096(2) Uani 1 1 d . . . H8 H 0.5489 0.8619 0.4303 0.115 Uiso 1 1 calc R . . C9 C 0.5941(5) 0.7630(6) 0.5165(6) 0.098(2) Uani 1 1 d . . . H9 H 0.5930 0.8178 0.5566 0.118 Uiso 1 1 calc R . . C10 C 0.6216(5) 0.6578(5) 0.5350(4) 0.0781(16) Uani 1 1 d . . . H10 H 0.6379 0.6398 0.5861 0.094 Uiso 1 1 calc R . . C11 C 0.6231(4) 0.5814(4) 0.4720(3) 0.0632(13) Uani 1 1 d . . . C12 C 0.6793(5) 0.4074(5) 0.5337(4) 0.0794(16) Uani 1 1 d . . . H12A H 0.6478 0.3342 0.5259 0.119 Uiso 1 1 calc R . . H12B H 0.6531 0.4419 0.5809 0.119 Uiso 1 1 calc R . . H12C H 0.7584 0.4042 0.5377 0.119 Uiso 1 1 calc R . . C13 C 0.8228(4) 0.1145(4) 0.4656(3) 0.0582(12) Uani 1 1 d . . . C14 C 0.7264(5) 0.0780(5) 0.4978(3) 0.0702(14) Uani 1 1 d . . . H14 H 0.6612 0.0664 0.4675 0.084 Uiso 1 1 calc R . . C15 C 0.7305(6) 0.0598(5) 0.5754(4) 0.0845(17) Uani 1 1 d . . . H15 H 0.6667 0.0358 0.5985 0.101 Uiso 1 1 calc R . . C16 C 0.8283(7) 0.0764(6) 0.6210(4) 0.096(2) Uani 1 1 d . . . H16 H 0.8286 0.0628 0.6738 0.115 Uiso 1 1 calc R . . C17 C 0.9243(6) 0.1124(5) 0.5896(4) 0.0846(17) Uani 1 1 d . . . H17 H 0.9895 0.1234 0.6201 0.102 Uiso 1 1 calc R . . C18 C 0.9201(5) 0.1313(4) 0.5118(3) 0.0645(13) Uani 1 1 d . . . C19 C 1.1153(4) 0.1967(5) 0.4846(4) 0.0807(17) Uani 1 1 d . . . H19A H 1.1507 0.1343 0.5050 0.121 Uiso 1 1 calc R . . H19B H 1.1182 0.2564 0.5239 0.121 Uiso 1 1 calc R . . H19C H 1.1529 0.2188 0.4396 0.121 Uiso 1 1 calc R . . C20 C 0.9518(4) 0.1735(4) 0.3920(3) 0.0556(11) Uani 1 1 d . . . C21 C 1.0066(4) 0.2096(4) 0.3211(3) 0.0645(13) Uani 1 1 d . . . H21A H 1.0400 0.2825 0.3323 0.077 Uiso 1 1 calc R . . H21B H 1.0651 0.1598 0.3082 0.077 Uiso 1 1 calc R . . C22 C 0.9500(4) 0.0311(4) 0.1986(3) 0.0636(13) Uani 1 1 d . . . C23 C 1.1068(7) -0.0493(7) 0.1225(5) 0.118(3) Uani 1 1 d . . . H23A H 1.1053 0.0161 0.0940 0.177 Uiso 1 1 calc R . . H23B H 1.1048 -0.1128 0.0865 0.177 Uiso 1 1 calc R . . H23C H 1.1732 -0.0485 0.1551 0.177 Uiso 1 1 calc R . . C24 C 0.9639(5) -0.1472(5) 0.2035(4) 0.0811(17) Uani 1 1 d . . . C25 C 0.9927(7) -0.2552(6) 0.1990(6) 0.117(3) Uani 1 1 d . . . H25 H 1.0512 -0.2786 0.1695 0.141 Uiso 1 1 calc R . . C26 C 0.9332(8) -0.3263(7) 0.2389(6) 0.133(3) Uani 1 1 d . . . H26 H 0.9525 -0.3997 0.2377 0.160 Uiso 1 1 calc R . . C27 C 0.8431(7) -0.2927(6) 0.2821(6) 0.117(3) Uani 1 1 d . . . H27 H 0.8031 -0.3444 0.3081 0.141 Uiso 1 1 calc R . . C28 C 0.8133(5) -0.1857(5) 0.2866(4) 0.0820(17) Uani 1 1 d . . . H28 H 0.7543 -0.1627 0.3158 0.098 Uiso 1 1 calc R . . C29 C 0.8751(4) -0.1119(5) 0.2456(3) 0.0683(14) Uani 1 1 d . . . C30 C 0.6873(4) 0.0864(5) 0.0960(3) 0.0696(14) Uani 1 1 d . . . C31 C 0.7191(5) -0.0161(6) 0.0717(4) 0.0860(18) Uani 1 1 d . . . H31 H 0.7584 -0.0596 0.1053 0.103 Uiso 1 1 calc R . . C32 C 0.6905(6) -0.0538(8) -0.0057(5) 0.104(2) Uani 1 1 d . . . H32 H 0.7133 -0.1224 -0.0243 0.125 Uiso 1 1 calc R . . C33 C 0.6301(7) 0.0084(9) -0.0541(5) 0.105(2) Uani 1 1 d . . . H33 H 0.6107 -0.0202 -0.1045 0.126 Uiso 1 1 calc R . . C34 C 0.5971(6) 0.1104(9) -0.0315(4) 0.102(2) Uani 1 1 d . . . H34 H 0.5570 0.1525 -0.0656 0.123 Uiso 1 1 calc R . . C35 C 0.6257(5) 0.1496(6) 0.0449(4) 0.0813(17) Uani 1 1 d . . . C36 C 0.5359(7) 0.3371(8) 0.0596(5) 0.121(3) Uani 1 1 d . . . H36A H 0.4642 0.3082 0.0415 0.182 Uiso 1 1 calc R . . H36B H 0.5713 0.3708 0.0177 0.182 Uiso 1 1 calc R . . H36C H 0.5281 0.3909 0.1020 0.182 Uiso 1 1 calc R . . C37 C 0.6512(4) 0.2411(5) 0.1586(3) 0.0676(14) Uani 1 1 d . . . C38 C 0.6444(4) 0.3283(5) 0.2228(3) 0.0708(14) Uani 1 1 d . . . H38A H 0.6689 0.3985 0.2047 0.085 Uiso 1 1 calc R . . H38B H 0.5683 0.3345 0.2374 0.085 Uiso 1 1 calc R . . C39 C 0.5472(5) 0.0026(7) 0.2755(5) 0.102(2) Uani 1 1 d . . . H39A H 0.5277 0.0442 0.2314 0.153 Uiso 1 1 calc R . . H39B H 0.4883 0.0048 0.3113 0.153 Uiso 1 1 calc R . . H39C H 0.5590 -0.0723 0.2580 0.153 Uiso 1 1 calc R . . Cl1 Cl 0.3010(15) 0.2253(16) 0.2360(11) 0.087(4) Uani 0.51(3) 1 d P A 1 O2 O 0.249(2) 0.306(2) 0.2829(13) 0.152(8) Uani 0.51(3) 1 d P A 1 O3 O 0.2657(19) 0.144(3) 0.2820(17) 0.149(9) Uani 0.51(3) 1 d P A 1 O4 O 0.2457(17) 0.2278(17) 0.1633(10) 0.158(9) Uani 0.51(3) 1 d P A 1 O5 O 0.4082(16) 0.222(2) 0.2165(19) 0.175(11) Uani 0.51(3) 1 d P A 1 Cl1' Cl 0.301(3) 0.224(3) 0.238(2) 0.131(7) Uani 0.49(3) 1 d P A 2 O2' O 0.3901(17) 0.2669(18) 0.2801(14) 0.175(10) Uani 0.49(3) 1 d P A 2 O3' O 0.256(2) 0.118(2) 0.2347(17) 0.145(8) Uani 0.49(3) 1 d P A 2 O4' O 0.2157(19) 0.298(2) 0.2291(19) 0.165(10) Uani 0.49(3) 1 d P A 2 O5' O 0.360(2) 0.221(2) 0.1693(13) 0.167(11) Uani 0.49(3) 1 d P A 2 Cl2 Cl 0.01(2) 0.50(2) 0.485(15) 0.11(3) Uani 0.33(11) 1 d P . 1 O6 O -0.012(8) 0.433(9) 0.547(6) 0.14(3) Uani 0.33(11) 1 d P . 1 O7 O 0.063(15) 0.593(11) 0.517(7) 0.11(3) Uani 0.33(11) 1 d P . 1 O8 O 0.054(7) 0.453(5) 0.421(5) 0.126(15) Uani 0.33(11) 1 d P . 1 O9 O -0.105(5) 0.524(6) 0.462(4) 0.12(2) Uani 0.33(11) 1 d P . 1 Cl2' Cl -0.02(3) 0.50(4) 0.48(2) 0.12(6) Uani 0.17(11) 1 d P . 2 O6' O -0.07(3) 0.41(3) 0.512(16) 0.13(7) Uani 0.17(11) 1 d P . 2 O7' O 0.021(15) 0.59(2) 0.532(12) 0.12(4) Uani 0.17(11) 1 d P . 2 O8' O 0.093(13) 0.450(9) 0.443(10) 0.13(3) Uani 0.17(11) 1 d P . 2 O9' O -0.077(10) 0.563(11) 0.433(9) 0.12(4) Uani 0.17(11) 1 d P . 2 Cl3 Cl 0.87(9) 0.37(6) 0.01(2) 0.18(8) Uani 0.17(3) 1 d P B 1 O10 O 0.929(12) 0.272(11) 0.006(5) 0.16(3) Uani 0.17(3) 1 d P B 1 O11 O 0.921(9) 0.460(6) 0.052(4) 0.19(3) Uani 0.17(3) 1 d P B 1 O12 O 0.818(11) 0.395(7) -0.064(6) 0.19(4) Uani 0.17(3) 1 d P B 1 O13 O 0.80(2) 0.389(14) 0.067(12) 0.18(5) Uani 0.17(3) 1 d P B 1 Cl3' Cl 0.88(5) 0.36(3) 0.007(13) 0.18(6) Uani 0.33(3) 1 d P B 2 O10' O 0.886(6) 0.264(6) 0.027(3) 0.166(18) Uani 0.33(3) 1 d P B 2 O11' O 0.816(13) 0.433(7) 0.062(7) 0.19(2) Uani 0.33(3) 1 d P B 2 O12' O 0.924(4) 0.429(3) -0.0463(19) 0.187(18) Uani 0.33(3) 1 d P B 2 O13' O 0.791(5) 0.335(4) -0.051(3) 0.195(19) Uani 0.33(3) 1 d P B 2 O1W O 0.4935(18) 0.5534(17) 0.1985(12) 0.218(8) Uani 0.50 1 d P C 1 H1WA H 0.5517 0.5881 0.1794 0.261 Uiso 0.50 1 d PR C 1 H1WB H 0.5228 0.5629 0.2444 0.261 Uiso 0.50 1 d PR C 1 O2W O 0.623(4) 0.648(5) 0.143(3) 0.22(2) Uani 0.20 1 d P D 2 H2WA H 0.5778 0.7001 0.1489 0.269 Uiso 0.20 1 d PR D 2 H2WB H 0.6717 0.6680 0.1119 0.269 Uiso 0.20 1 d PR D 2 O3W O 0.328(3) 0.761(3) 0.224(2) 0.243(16) Uani 0.30 1 d P E 2 H3WA H 0.3903 0.7681 0.2037 0.291 Uiso 0.30 1 d PR E 2 H3WB H 0.3073 0.6936 0.2174 0.291 Uiso 0.30 1 d PR E 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 0.0466(4) 0.0597(4) 0.0530(5) 0.0002(3) 0.0106(3) -0.0093(3) O1 0.0529(19) 0.081(2) 0.074(2) 0.0066(18) 0.0123(16) -0.0153(17) N1 0.053(2) 0.059(2) 0.059(2) 0.0033(18) 0.0127(18) -0.0073(18) N2 0.055(2) 0.065(2) 0.056(2) 0.0040(18) 0.0081(18) -0.0038(18) N3 0.089(3) 0.063(3) 0.068(3) 0.007(2) 0.016(2) 0.006(2) N4 0.043(2) 0.072(3) 0.067(3) 0.004(2) 0.0088(18) -0.0053(18) N5 0.051(2) 0.065(2) 0.054(2) 0.0047(18) 0.0070(17) -0.0044(18) N6 0.051(2) 0.060(2) 0.073(3) 0.000(2) -0.004(2) 0.0061(18) N7 0.051(2) 0.059(2) 0.064(2) -0.0004(18) 0.0164(18) -0.0051(17) N8 0.070(3) 0.081(3) 0.093(4) -0.016(3) 0.037(3) -0.009(2) N9 0.061(2) 0.078(3) 0.052(2) 0.000(2) 0.0046(19) -0.016(2) N10 0.072(3) 0.110(4) 0.060(3) 0.017(3) -0.005(2) -0.008(3) C1 0.059(3) 0.072(3) 0.067(3) 0.003(2) 0.021(2) -0.012(2) C2 0.063(3) 0.067(3) 0.073(3) 0.016(3) 0.020(3) -0.013(2) C3 0.062(3) 0.053(3) 0.076(3) 0.001(2) 0.005(2) -0.010(2) C4 0.072(3) 0.065(3) 0.068(3) 0.004(3) 0.019(3) 0.005(3) C5 0.054(3) 0.072(3) 0.070(3) -0.002(3) 0.019(2) -0.003(2) C6 0.054(3) 0.064(3) 0.094(4) 0.008(3) 0.018(3) 0.000(2) C7 0.073(4) 0.075(4) 0.119(6) 0.019(4) 0.023(4) 0.008(3) C8 0.086(4) 0.065(4) 0.139(7) 0.000(4) 0.033(4) 0.001(3) C9 0.071(4) 0.082(5) 0.138(7) -0.040(4) 0.035(4) -0.013(3) C10 0.065(3) 0.079(4) 0.088(4) -0.013(3) 0.017(3) -0.016(3) C11 0.040(2) 0.069(3) 0.081(4) -0.001(3) 0.015(2) -0.005(2) C12 0.068(3) 0.095(4) 0.074(4) 0.005(3) 0.004(3) -0.007(3) C13 0.061(3) 0.052(3) 0.063(3) 0.003(2) 0.013(2) 0.005(2) C14 0.069(3) 0.078(3) 0.065(3) 0.008(3) 0.017(3) 0.003(3) C15 0.091(4) 0.088(4) 0.078(4) 0.013(3) 0.027(3) 0.005(3) C16 0.117(6) 0.106(5) 0.068(4) 0.019(4) 0.015(4) 0.002(4) C17 0.097(5) 0.089(4) 0.068(4) 0.008(3) -0.009(3) 0.006(3) C18 0.069(3) 0.061(3) 0.065(3) 0.006(2) 0.004(3) 0.007(2) C19 0.051(3) 0.093(4) 0.096(4) 0.001(3) -0.010(3) 0.002(3) C20 0.050(3) 0.053(3) 0.063(3) -0.001(2) 0.004(2) -0.001(2) C21 0.050(3) 0.064(3) 0.080(4) 0.000(2) 0.014(2) -0.010(2) C22 0.055(3) 0.071(3) 0.064(3) -0.010(2) 0.018(2) -0.005(2) C23 0.107(5) 0.108(5) 0.142(7) -0.025(5) 0.083(5) -0.014(4) C24 0.075(4) 0.069(4) 0.099(5) -0.013(3) 0.031(3) -0.005(3) C25 0.111(6) 0.088(5) 0.157(8) -0.006(5) 0.064(5) 0.000(4) C26 0.135(7) 0.088(5) 0.181(10) 0.003(6) 0.053(7) 0.012(5) C27 0.114(6) 0.070(4) 0.172(8) 0.014(5) 0.050(6) -0.007(4) C28 0.078(4) 0.064(3) 0.103(5) -0.004(3) 0.027(3) -0.011(3) C29 0.060(3) 0.071(3) 0.073(3) -0.005(3) 0.015(2) -0.009(2) C30 0.058(3) 0.090(4) 0.059(3) -0.006(3) 0.013(2) -0.018(3) C31 0.077(4) 0.109(5) 0.068(4) -0.022(3) 0.011(3) -0.024(3) C32 0.084(4) 0.135(6) 0.086(5) -0.043(5) 0.024(4) -0.031(4) C33 0.087(5) 0.155(8) 0.070(5) -0.013(5) 0.012(4) -0.029(5) C34 0.085(5) 0.157(8) 0.063(4) 0.012(4) -0.006(3) -0.020(5) C35 0.067(3) 0.111(5) 0.063(4) -0.004(3) 0.010(3) -0.024(3) C36 0.119(7) 0.152(8) 0.092(5) 0.025(5) -0.013(5) 0.009(6) C37 0.058(3) 0.078(4) 0.066(3) 0.016(3) 0.002(2) -0.015(3) C38 0.060(3) 0.079(4) 0.072(4) 0.005(3) -0.001(3) -0.003(3) C39 0.072(4) 0.116(5) 0.117(6) 0.024(4) -0.005(4) -0.031(4) Cl1 0.061(8) 0.122(11) 0.075(9) -0.026(8) 0.015(7) -0.016(7) O2 0.160(17) 0.188(16) 0.102(12) -0.048(12) 0.035(12) -0.014(12) O3 0.125(12) 0.18(2) 0.156(19) 0.067(17) 0.046(14) -0.002(12) O4 0.146(18) 0.209(17) 0.113(12) -0.011(11) -0.023(10) -0.020(12) O5 0.101(13) 0.25(2) 0.17(3) 0.01(2) 0.024(13) -0.041(12) Cl1' 0.099(16) 0.17(2) 0.120(17) -0.013(17) 0.021(15) -0.025(15) O2' 0.127(15) 0.25(2) 0.136(15) -0.052(13) -0.021(11) -0.048(13) O3' 0.124(11) 0.165(16) 0.142(18) -0.016(15) 0.022(13) -0.035(10) O4' 0.142(17) 0.186(19) 0.17(3) 0.02(2) 0.007(14) -0.002(14) O5' 0.15(3) 0.23(2) 0.111(13) -0.023(13) 0.031(13) -0.050(17) Cl2 0.07(4) 0.070(18) 0.18(10) -0.02(5) -0.02(6) -0.01(3) O6 0.10(5) 0.13(5) 0.19(6) -0.02(4) 0.01(4) -0.02(3) O7 0.07(4) 0.11(3) 0.15(6) -0.05(5) 0.01(5) -0.02(3) O8 0.08(3) 0.119(18) 0.17(4) -0.05(2) 0.00(2) -0.02(2) O9 0.06(2) 0.12(3) 0.18(4) -0.03(3) -0.007(17) -0.022(15) Cl2' 0.08(11) 0.11(9) 0.17(17) -0.03(5) 0.00(8) -0.02(7) O6' 0.09(11) 0.12(7) 0.18(18) -0.03(12) 0.00(13) -0.02(6) O7' 0.08(6) 0.11(8) 0.16(9) -0.04(6) 0.00(7) -0.02(6) O8' 0.08(6) 0.12(3) 0.17(8) -0.04(4) 0.00(4) -0.01(4) O9' 0.07(5) 0.12(5) 0.17(7) -0.03(5) -0.01(5) -0.02(4) Cl3 0.26(13) 0.17(16) 0.10(12) 0.02(12) 0.03(8) -0.02(11) O10 0.28(11) 0.13(5) 0.07(4) 0.04(3) 0.03(4) 0.00(6) O11 0.27(9) 0.17(6) 0.13(5) 0.03(4) 0.04(5) -0.03(5) O12 0.27(10) 0.16(7) 0.14(6) 0.05(5) 0.03(5) -0.02(7) O13 0.26(12) 0.17(12) 0.12(5) 0.03(7) 0.03(6) -0.02(10) Cl3' 0.27(12) 0.16(5) 0.11(7) 0.03(6) 0.03(4) -0.02(6) O10' 0.27(5) 0.15(3) 0.08(2) 0.04(2) 0.03(2) -0.03(3) O11' 0.26(7) 0.17(6) 0.14(3) 0.03(4) 0.04(3) -0.02(6) O12' 0.28(5) 0.15(2) 0.13(2) 0.042(17) 0.05(2) -0.02(2) O13' 0.26(5) 0.18(4) 0.15(3) 0.03(3) 0.01(3) -0.01(3) O1W 0.24(2) 0.211(18) 0.205(18) 0.013(15) -0.029(15) 0.058(16) O2W 0.23(5) 0.22(5) 0.22(5) 0.01(4) 0.00(4) 0.01(4) O3W 0.24(4) 0.24(4) 0.25(4) 0.02(3) 0.00(3) 0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.816(3) . ? Fe1 N5 2.082(4) . ? Fe1 N7 2.086(4) . ? Fe1 N9 2.088(4) . ? Fe1 N2 2.284(4) . ? Fe1 N1 2.325(4) . ? O1 C39 1.384(7) . ? N1 C1 1.469(7) . ? N1 C2 1.472(7) . ? N1 C21 1.476(7) . ? N2 C38 1.476(7) . ? N2 C4 1.487(7) . ? N2 C3 1.497(6) . ? N3 C5 1.321(7) . ? N3 C6 1.389(7) . ? N4 C5 1.367(7) . ? N4 C11 1.383(7) . ? N4 C12 1.452(7) . ? N5 C20 1.339(6) . ? N5 C13 1.389(6) . ? N6 C20 1.319(6) . ? N6 C18 1.394(7) . ? N6 C19 1.465(6) . ? N7 C22 1.324(6) . ? N7 C29 1.372(7) . ? N8 C22 1.336(7) . ? N8 C24 1.397(8) . ? N8 C23 1.492(7) . ? N9 C37 1.320(7) . ? N9 C30 1.406(7) . ? N10 C37 1.333(7) . ? N10 C35 1.373(8) . ? N10 C36 1.496(10) . ? C1 C22 1.504(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.525(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.494(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 C11 1.385(8) . ? C6 C7 1.405(8) . ? C7 C8 1.358(10) . ? C7 H7 0.9300 . ? C8 C9 1.402(11) . ? C8 H8 0.9300 . ? C9 C10 1.385(10) . ? C9 H9 0.9300 . ? C10 C11 1.386(8) . ? C10 H10 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.387(7) . ? C13 C18 1.395(7) . ? C14 C15 1.362(8) . ? C14 H14 0.9300 . ? C15 C16 1.394(10) . ? C15 H15 0.9300 . ? C16 C17 1.374(10) . ? C16 H16 0.9300 . ? C17 C18 1.367(8) . ? C17 H17 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.495(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.368(9) . ? C24 C29 1.385(8) . ? C25 C26 1.347(11) . ? C25 H25 0.9300 . ? C26 C27 1.402(12) . ? C26 H26 0.9300 . ? C27 C28 1.361(9) . ? C27 H27 0.9300 . ? C28 C29 1.396(8) . ? C28 H28 0.9300 . ? C30 C31 1.364(9) . ? C30 C35 1.405(9) . ? C31 C32 1.406(9) . ? C31 H31 0.9300 . ? C32 C33 1.360(11) . ? C32 H32 0.9300 . ? C33 C34 1.356(12) . ? C33 H33 0.9300 . ? C34 C35 1.395(9) . ? C34 H34 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.491(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? Cl1 O5 1.36(3) . ? Cl1 O3 1.38(3) . ? Cl1 O4 1.39(3) . ? Cl1 O2 1.41(3) . ? Cl1' O2' 1.34(3) . ? Cl1' O3' 1.38(3) . ? Cl1' O4' 1.41(3) . ? Cl1' O5' 1.41(3) . ? Cl2 O8 1.4(2) . ? Cl2 O6 1.4(3) . ? Cl2 O7 1.4(3) . ? Cl2 O9 1.4(3) . ? Cl2' O7' 1.4(6) . ? Cl2' O6' 1.4(5) . ? Cl2' O9' 1.4(4) . ? Cl2' O8' 1.6(4) . ? Cl3 O13 1.4(8) . ? Cl3 O12 1.4(8) . ? Cl3 O11 1.4(5) . ? Cl3 O10 1.4(12) . ? Cl3' O10' 1.3(5) . ? Cl3' O12' 1.4(3) . ? Cl3' O13' 1.4(4) . ? Cl3' O11' 1.5(5) . ? O1W H1WA 0.8963 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8500 . ? 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 N5 96.11(16) . . ? O1 Fe1 N7 104.49(16) . . ? N5 Fe1 N7 92.46(16) . . ? O1 Fe1 N9 97.53(16) . . ? N5 Fe1 N9 163.43(16) . . ? N7 Fe1 N9 93.18(18) . . ? O1 Fe1 N2 103.83(16) . . ? N5 Fe1 N2 89.98(15) . . ? N7 Fe1 N2 151.13(15) . . ? N9 Fe1 N2 77.67(17) . . ? O1 Fe1 N1 173.22(16) . . ? N5 Fe1 N1 77.52(14) . . ? N7 Fe1 N1 73.77(14) . . ? N9 Fe1 N1 89.13(15) . . ? N2 Fe1 N1 78.71(14) . . ? C39 O1 Fe1 134.3(4) . . ? C1 N1 C2 112.4(4) . . ? C1 N1 C21 110.7(4) . . ? C2 N1 C21 111.7(4) . . ? C1 N1 Fe1 105.9(3) . . ? C2 N1 Fe1 106.3(3) . . ? C21 N1 Fe1 109.5(3) . . ? C38 N2 C4 111.2(4) . . ? C38 N2 C3 110.8(4) . . ? C4 N2 C3 110.6(4) . . ? C38 N2 Fe1 110.2(3) . . ? C4 N2 Fe1 107.5(3) . . ? C3 N2 Fe1 106.5(3) . . ? C5 N3 C6 103.9(5) . . ? C5 N4 C11 106.5(4) . . ? C5 N4 C12 127.8(5) . . ? C11 N4 C12 125.6(5) . . ? C20 N5 C13 106.2(4) . . ? C20 N5 Fe1 117.0(3) . . ? C13 N5 Fe1 136.0(3) . . ? C20 N6 C18 108.0(4) . . ? C20 N6 C19 126.2(5) . . ? C18 N6 C19 125.8(5) . . ? C22 N7 C29 106.2(4) . . ? C22 N7 Fe1 116.6(3) . . ? C29 N7 Fe1 137.1(3) . . ? C22 N8 C24 106.5(4) . . ? C22 N8 C23 127.3(5) . . ? C24 N8 C23 126.1(5) . . ? C37 N9 C30 105.9(5) . . ? C37 N9 Fe1 116.4(4) . . ? C30 N9 Fe1 137.2(4) . . ? C37 N10 C35 108.2(5) . . ? C37 N10 C36 125.4(6) . . ? C35 N10 C36 126.2(6) . . ? N1 C1 C22 105.7(4) . . ? N1 C1 H1A 110.6 . . ? C22 C1 H1A 110.6 . . ? N1 C1 H1B 110.6 . . ? C22 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? N1 C2 C3 109.8(4) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 110.5(4) . . ? N2 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N2 C4 C5 115.1(4) . . ? N2 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 N4 113.3(5) . . ? N3 C5 C4 125.7(5) . . ? N4 C5 C4 121.0(5) . . ? C11 C6 N3 111.0(5) . . ? C11 C6 C7 119.6(6) . . ? N3 C6 C7 129.3(6) . . ? C8 C7 C6 118.2(7) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C9 120.8(7) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 122.7(6) . . ? C10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C9 C10 C11 115.1(7) . . ? C9 C10 H10 122.5 . . ? C11 C10 H10 122.5 . . ? N4 C11 C6 105.2(5) . . ? N4 C11 C10 131.3(6) . . ? C6 C11 C10 123.5(5) . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N5 131.5(5) . . ? C14 C13 C18 120.5(5) . . ? N5 C13 C18 108.0(4) . . ? C15 C14 C13 117.7(6) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 121.4(6) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 117.3(6) . . ? C18 C17 H17 121.3 . . ? C16 C17 H17 121.3 . . ? C17 C18 N6 132.5(5) . . ? C17 C18 C13 121.7(5) . . ? N6 C18 C13 105.8(4) . . ? N6 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 N5 112.0(4) . . ? N6 C20 C21 125.9(4) . . ? N5 C20 C21 122.1(4) . . ? N1 C21 C20 111.8(4) . . ? N1 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? N1 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? N7 C22 N8 112.5(5) . . ? N7 C22 C1 120.3(4) . . ? N8 C22 C1 127.2(4) . . ? N8 C23 H23A 109.5 . . ? N8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 121.7(6) . . ? C25 C24 N8 132.5(6) . . ? C29 C24 N8 105.9(5) . . ? C26 C25 C24 117.7(7) . . ? C26 C25 H25 121.2 . . ? C24 C25 H25 121.2 . . ? C25 C26 C27 121.8(8) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 121.0(7) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 117.2(6) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? N7 C29 C24 108.9(5) . . ? N7 C29 C28 130.4(5) . . ? C24 C29 C28 120.6(6) . . ? C31 C30 C35 120.2(6) . . ? C31 C30 N9 132.2(6) . . ? C35 C30 N9 107.5(5) . . ? C30 C31 C32 117.7(8) . . ? C30 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? C33 C32 C31 121.2(8) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 122.4(7) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 117.2(8) . . ? C33 C34 H34 121.4 . . ? C35 C34 H34 121.4 . . ? N10 C35 C34 132.8(7) . . ? N10 C35 C30 105.9(5) . . ? C34 C35 C30 121.3(7) . . ? N10 C36 H36A 109.5 . . ? N10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 N10 112.4(5) . . ? N9 C37 C38 122.8(5) . . ? N10 C37 C38 124.8(6) . . ? N2 C38 C37 110.7(5) . . ? N2 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? O1 C39 H39A 109.5 . . ? O1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O5 Cl1 O3 116(2) . . ? O5 Cl1 O4 102.3(18) . . ? O3 Cl1 O4 115.4(16) . . ? O5 Cl1 O2 128.6(19) . . ? O3 Cl1 O2 91(2) . . ? O4 Cl1 O2 104.0(17) . . ? O2' Cl1' O3' 130(4) . . ? O2' Cl1' O4' 114(3) . . ? O3' Cl1' O4' 109(3) . . ? O2' Cl1' O5' 91(2) . . ? O3' Cl1' O5' 101(2) . . ? O4' Cl1' O5' 107(4) . . ? O8 Cl2 O6 119(10) . . ? O8 Cl2 O7 112(10) . . ? O6 Cl2 O7 106(10) . . ? O8 Cl2 O9 108(10) . . ? O6 Cl2 O9 101(10) . . ? O7 Cl2 O9 110(10) . . ? O7' Cl2' O6' 118(10) . . ? O7' Cl2' O9' 95(10) . . ? O6' Cl2' O9' 121(10) . . ? O7' Cl2' O8' 104(10) . . ? O6' Cl2' O8' 104(10) . . ? O9' Cl2' O8' 115(10) . . ? O13 Cl3 O12 109(10) . . ? O13 Cl3 O11 77(10) . . ? O12 Cl3 O11 116(10) . . ? O13 Cl3 O10 120(10) . . ? O12 Cl3 O10 113(10) . . ? O11 Cl3 O10 117(10) . . ? O10' Cl3' O12' 140(10) . . ? O10' Cl3' O13' 95(10) . . ? O12' Cl3' O13' 88(10) . . ? O10' Cl3' O11' 112(10) . . ? O12' Cl3' O11' 106(10) . . ? O13' Cl3' O11' 97(10) . . ? H1WA O1W H1WB 90.2 . . ? H2WA O2W H2WB 108.6 . . ? H3WA O3W H3WB 107.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.845 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.116 #Complex 4 CCDC 804328 data_Fe(OPr)(Hmedtb).(ClO4)3.2MeCN.n-PrOH _database_code_depnum_ccdc_archive 'CCDC 804329' #TrackingRef '- newcifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H48 Cl3 Fe N10 O13' _chemical_formula_weight 1051.09 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.203(4) _cell_length_b 13.723(5) _cell_length_c 19.511(6) _cell_angle_alpha 95.8751(19) _cell_angle_beta 102.746(3) _cell_angle_gamma 114.876(4) _cell_volume 2820.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8482 _cell_measurement_theta_min 1.6770 _cell_measurement_theta_max 27.4626 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8638 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28719 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9901 _reflns_number_gt 8700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0969P)^2^+2.5266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9901 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36360(4) 0.90760(4) 0.20037(2) 0.03659(16) Uani 1 1 d . . . O1 O 0.4453(2) 0.89195(19) 0.13671(13) 0.0488(6) Uani 1 1 d . . . N1 N 0.2696(3) 0.9494(2) 0.28230(14) 0.0385(6) Uani 1 1 d . . . N2 N 0.4862(3) 0.9012(2) 0.30562(14) 0.0384(6) Uani 1 1 d . . . N3 N 0.7354(3) 0.9314(2) 0.42092(15) 0.0429(6) Uani 1 1 d . . . H3 H 0.6974 0.8590 0.4090 0.052 Uiso 1 1 calc R . . N4 N 0.7885(3) 1.1029(2) 0.41447(16) 0.0445(7) Uani 1 1 d . . . N5 N 0.4592(3) 1.0783(2) 0.23019(15) 0.0390(6) Uani 1 1 d . . . N6 N 0.4564(3) 1.2364(2) 0.26421(17) 0.0500(7) Uani 1 1 d . . . N7 N 0.1981(3) 0.9022(2) 0.13815(14) 0.0402(6) Uani 1 1 d . . . N8 N -0.0006(3) 0.8713(2) 0.12321(15) 0.0447(7) Uani 1 1 d . . . N9 N 0.2700(3) 0.7406(2) 0.20638(15) 0.0417(6) Uani 1 1 d . . . N10 N 0.2752(3) 0.5974(2) 0.24796(17) 0.0473(7) Uani 1 1 d . . . C1 C 0.1313(3) 0.8835(3) 0.24803(18) 0.0429(7) Uani 1 1 d . . . H1A H 0.0850 0.9155 0.2703 0.052 Uiso 1 1 calc R . . H1B H 0.1028 0.8067 0.2540 0.052 Uiso 1 1 calc R . . C2 C 0.3172(3) 0.9180(3) 0.34879(18) 0.0425(7) Uani 1 1 d . . . H2A H 0.2734 0.8370 0.3425 0.051 Uiso 1 1 calc R . . H2B H 0.2996 0.9515 0.3898 0.051 Uiso 1 1 calc R . . C3 C 0.4582(3) 0.9574(3) 0.36455(17) 0.0411(7) Uani 1 1 d . . . H3A H 0.5014 1.0380 0.3689 0.049 Uiso 1 1 calc R . . H3B H 0.4910 0.9415 0.4109 0.049 Uiso 1 1 calc R . . C4 C 0.6209(3) 0.9625(3) 0.30668(18) 0.0416(7) Uani 1 1 d . . . H4A H 0.6320 1.0286 0.2870 0.050 Uiso 1 1 calc R . . H4B H 0.6399 0.9152 0.2743 0.050 Uiso 1 1 calc R . . C5 C 0.7150(3) 0.9981(3) 0.38011(19) 0.0413(7) Uani 1 1 d . . . C6 C 0.8271(3) 0.9960(3) 0.4854(2) 0.0455(8) Uani 1 1 d . . . C7 C 0.8837(4) 0.9680(4) 0.5453(2) 0.0528(9) Uani 1 1 d . . . H7 H 0.8605 0.8935 0.5482 0.063 Uiso 1 1 calc R . . C8 C 0.9742(4) 1.0536(4) 0.5993(2) 0.0576(10) Uani 1 1 d . . . H8 H 1.0159 1.0381 0.6406 0.069 Uiso 1 1 calc R . . C9 C 1.0080(4) 1.1634(4) 0.5964(2) 0.0638(11) Uani 1 1 d . . . H9 H 1.0709 1.2202 0.6358 0.077 Uiso 1 1 calc R . . C10 C 0.9519(4) 1.1906(4) 0.5373(2) 0.0577(10) Uani 1 1 d . . . H10 H 0.9743 1.2651 0.5347 0.069 Uiso 1 1 calc R . . C11 C 0.8608(3) 1.1036(3) 0.48172(19) 0.0463(8) Uani 1 1 d . . . C12 C 0.8007(4) 1.2016(3) 0.3878(2) 0.0591(10) Uani 1 1 d . . . H12A H 0.7916 1.1878 0.3361 0.089 Uiso 1 1 calc R . . H12B H 0.8839 1.2630 0.4133 0.089 Uiso 1 1 calc R . . H12C H 0.7347 1.2201 0.3960 0.089 Uiso 1 1 calc R . . C13 C 0.5525(3) 1.1608(3) 0.20909(19) 0.0428(8) Uani 1 1 d . . . C14 C 0.6388(3) 1.1563(3) 0.1752(2) 0.0498(8) Uani 1 1 d . . . H14 H 0.6401 1.0888 0.1602 0.060 Uiso 1 1 calc R . . C15 C 0.7238(4) 1.2551(3) 0.1640(3) 0.0660(11) Uani 1 1 d . . . H15 H 0.7855 1.2551 0.1417 0.079 Uiso 1 1 calc R . . C16 C 0.7207(5) 1.3537(4) 0.1846(3) 0.0742(13) Uani 1 1 d . . . H16 H 0.7792 1.4190 0.1751 0.089 Uiso 1 1 calc R . . C17 C 0.6340(5) 1.3592(3) 0.2190(3) 0.0697(12) Uani 1 1 d . . . H17 H 0.6321 1.4265 0.2336 0.084 Uiso 1 1 calc R . . C18 C 0.5508(4) 1.2605(3) 0.2306(2) 0.0501(9) Uani 1 1 d . . . C19 C 0.4204(5) 1.3160(3) 0.2969(3) 0.0685(12) Uani 1 1 d . . . H19A H 0.3289 1.2808 0.2893 0.103 Uiso 1 1 calc R . . H19B H 0.4442 1.3796 0.2743 0.103 Uiso 1 1 calc R . . H19C H 0.4641 1.3406 0.3486 0.103 Uiso 1 1 calc R . . C20 C 0.4065(3) 1.1285(3) 0.26307(17) 0.0392(7) Uani 1 1 d . . . C21 C 0.3037(3) 1.0689(3) 0.29518(19) 0.0426(7) Uani 1 1 d . . . H21A H 0.3320 1.1002 0.3476 0.051 Uiso 1 1 calc R . . H21B H 0.2285 1.0785 0.2734 0.051 Uiso 1 1 calc R . . C22 C 0.1077(3) 0.8865(3) 0.16981(18) 0.0413(7) Uani 1 1 d . . . C23 C -0.1183(4) 0.8545(4) 0.1391(2) 0.0610(10) Uani 1 1 d . . . H23A H -0.1071 0.8577 0.1907 0.091 Uiso 1 1 calc R . . H23B H -0.1862 0.7822 0.1116 0.091 Uiso 1 1 calc R . . H23C H -0.1404 0.9122 0.1256 0.091 Uiso 1 1 calc R . . C24 C 0.0191(3) 0.8740(3) 0.05603(18) 0.0449(8) Uani 1 1 d . . . C25 C -0.0608(4) 0.8598(3) -0.0111(2) 0.0559(9) Uani 1 1 d . . . H25 H -0.1460 0.8460 -0.0176 0.067 Uiso 1 1 calc R . . C26 C -0.0099(4) 0.8669(3) -0.0677(2) 0.0609(10) Uani 1 1 d . . . H26 H -0.0619 0.8565 -0.1146 0.073 Uiso 1 1 calc R . . C27 C 0.1153(4) 0.8888(3) -0.0587(2) 0.0562(10) Uani 1 1 d . . . H27 H 0.1462 0.8934 -0.0995 0.067 Uiso 1 1 calc R . . C28 C 0.1961(4) 0.9042(3) 0.00834(19) 0.0480(8) Uani 1 1 d . . . H28 H 0.2818 0.9198 0.0146 0.058 Uiso 1 1 calc R . . C29 C 0.1448(3) 0.8955(3) 0.06605(17) 0.0415(7) Uani 1 1 d . . . C30 C 0.1646(3) 0.6446(3) 0.16332(19) 0.0455(8) Uani 1 1 d . . . C31 C 0.0643(4) 0.6279(3) 0.1047(2) 0.0526(9) Uani 1 1 d . . . H31 H 0.0592 0.6880 0.0866 0.063 Uiso 1 1 calc R . . C32 C -0.0273(4) 0.5205(3) 0.0741(2) 0.0651(11) Uani 1 1 d . . . H32 H -0.0968 0.5070 0.0343 0.078 Uiso 1 1 calc R . . C33 C -0.0202(4) 0.4314(3) 0.1001(3) 0.0692(12) Uani 1 1 d . . . H33 H -0.0846 0.3589 0.0772 0.083 Uiso 1 1 calc R . . C34 C 0.0766(4) 0.4457(3) 0.1575(2) 0.0590(10) Uani 1 1 d . . . H34 H 0.0816 0.3851 0.1750 0.071 Uiso 1 1 calc R . . C35 C 0.1677(4) 0.5538(3) 0.1890(2) 0.0482(8) Uani 1 1 d . . . C36 C 0.3175(4) 0.5338(3) 0.2940(2) 0.0632(11) Uani 1 1 d . . . H36A H 0.3871 0.5264 0.2810 0.095 Uiso 1 1 calc R . . H36B H 0.2471 0.4605 0.2870 0.095 Uiso 1 1 calc R . . H36C H 0.3462 0.5722 0.3446 0.095 Uiso 1 1 calc R . . C37 C 0.3321(3) 0.7079(3) 0.25563(18) 0.0419(7) Uani 1 1 d . . . C38 C 0.4533(3) 0.7847(3) 0.31005(19) 0.0445(8) Uani 1 1 d . . . H38A H 0.5212 0.7675 0.3019 0.053 Uiso 1 1 calc R . . H38B H 0.4467 0.7750 0.3588 0.053 Uiso 1 1 calc R . . C39 C 0.4559(6) 0.8143(4) 0.0905(3) 0.0905(17) Uani 1 1 d . . . H39A H 0.3709 0.7623 0.0582 0.109 Uiso 1 1 calc R . . H39B H 0.4882 0.7716 0.1195 0.109 Uiso 1 1 calc R . . C40 C 0.5408(7) 0.8627(6) 0.0459(4) 0.118(2) Uani 1 1 d . . . H40A H 0.5075 0.9048 0.0169 0.141 Uiso 1 1 calc R . . H40B H 0.6249 0.9159 0.0786 0.141 Uiso 1 1 calc R . . C41 C 0.5576(7) 0.7862(7) -0.0028(4) 0.127(3) Uani 1 1 d . . . H41A H 0.5898 0.7432 0.0248 0.190 Uiso 1 1 calc R . . H41B H 0.6179 0.8274 -0.0276 0.190 Uiso 1 1 calc R . . H41C H 0.4763 0.7365 -0.0383 0.190 Uiso 1 1 calc R . . Cl1 Cl 0.6717(16) 0.6692(11) 0.2327(8) 0.091(4) Uani 0.478(11) 1 d P A 1 O2 O 0.6143(11) 0.6561(11) 0.1586(7) 0.123(5) Uani 0.478(11) 1 d P A 1 O3 O 0.5792(12) 0.5910(9) 0.2561(8) 0.106(5) Uani 0.478(11) 1 d P A 1 O4 O 0.7764(8) 0.6496(6) 0.2355(5) 0.090(3) Uani 0.478(11) 1 d P A 1 O5 O 0.717(4) 0.784(3) 0.252(2) 0.078(7) Uani 0.478(11) 1 d P A 1 Cl1' Cl 0.6527(11) 0.6638(7) 0.2233(5) 0.0597(16) Uani 0.522(11) 1 d P A 2 O2' O 0.6766(10) 0.6196(7) 0.1632(6) 0.101(4) Uani 0.522(11) 1 d P A 2 O3' O 0.5202(8) 0.6385(7) 0.1982(5) 0.103(3) Uani 0.522(11) 1 d P A 2 O4' O 0.6558(13) 0.6067(8) 0.2818(5) 0.094(3) Uani 0.522(11) 1 d P A 2 O5' O 0.721(3) 0.772(2) 0.269(2) 0.079(6) Uani 0.522(11) 1 d P A 2 Cl2 Cl 0.000(3) 0.8451(15) 0.7245(9) 0.0495(17) Uani 0.72(6) 1 d P B 1 O6 O -0.051(2) 0.9080(19) 0.7559(13) 0.077(4) Uani 0.72(6) 1 d P B 1 O7 O -0.037(3) 0.8228(15) 0.6487(4) 0.094(5) Uani 0.72(6) 1 d P B 1 O8 O -0.022(2) 0.7464(12) 0.7459(12) 0.096(4) Uani 0.72(6) 1 d P B 1 O9 O 0.1337(10) 0.9182(13) 0.7476(14) 0.098(4) Uani 0.72(6) 1 d P B 1 Cl2' Cl -0.015(7) 0.839(4) 0.721(3) 0.065(12) Uani 0.28(6) 1 d P B 2 O6' O -0.069(5) 0.878(5) 0.766(3) 0.068(8) Uani 0.28(6) 1 d P B 2 O7' O -0.106(6) 0.801(2) 0.6542(13) 0.088(11) Uani 0.28(6) 1 d P B 2 O8' O 0.029(5) 0.778(4) 0.7622(18) 0.075(9) Uani 0.28(6) 1 d P B 2 O9' O 0.099(5) 0.918(3) 0.714(3) 0.084(11) Uani 0.28(6) 1 d P B 2 Cl3 Cl 0.5805(9) 0.2326(9) 0.4911(6) 0.0529(10) Uani 0.81(5) 1 d P C 1 O10 O 0.6224(17) 0.3323(7) 0.5412(7) 0.106(6) Uani 0.81(5) 1 d P C 1 O11 O 0.580(3) 0.249(2) 0.4199(15) 0.065(3) Uani 0.81(5) 1 d P C 1 O12 O 0.459(3) 0.156(2) 0.4939(15) 0.067(4) Uani 0.81(5) 1 d P C 1 O13 O 0.6621(11) 0.1838(17) 0.5120(7) 0.080(4) Uani 0.81(5) 1 d P C 1 Cl3' Cl 0.561(6) 0.245(5) 0.494(3) 0.074(8) Uani 0.19(5) 1 d P C 2 O10' O 0.553(7) 0.340(3) 0.518(2) 0.093(14) Uani 0.19(5) 1 d P C 2 O11' O 0.557(11) 0.257(10) 0.423(7) 0.071(18) Uani 0.19(5) 1 d P C 2 O12' O 0.444(12) 0.153(9) 0.481(6) 0.062(19) Uani 0.19(5) 1 d P C 2 O13' O 0.673(3) 0.249(6) 0.536(2) 0.09(2) Uani 0.19(5) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0472(3) 0.0327(3) 0.0402(3) 0.01174(19) 0.0199(2) 0.0233(2) O1 0.0630(15) 0.0431(13) 0.0548(14) 0.0139(11) 0.0330(12) 0.0290(12) N1 0.0458(15) 0.0401(14) 0.0387(14) 0.0119(11) 0.0186(12) 0.0241(12) N2 0.0490(15) 0.0349(14) 0.0423(14) 0.0121(11) 0.0181(12) 0.0260(12) N3 0.0466(16) 0.0437(15) 0.0498(16) 0.0162(13) 0.0207(13) 0.0264(13) N4 0.0476(16) 0.0422(15) 0.0514(16) 0.0177(13) 0.0203(13) 0.0231(13) N5 0.0487(15) 0.0342(14) 0.0438(15) 0.0105(11) 0.0186(12) 0.0250(12) N6 0.074(2) 0.0390(15) 0.0576(18) 0.0176(13) 0.0310(16) 0.0374(15) N7 0.0478(15) 0.0427(15) 0.0400(14) 0.0129(12) 0.0179(12) 0.0265(13) N8 0.0443(16) 0.0461(16) 0.0459(16) 0.0108(13) 0.0175(13) 0.0202(13) N9 0.0496(16) 0.0323(14) 0.0472(16) 0.0112(12) 0.0192(13) 0.0196(12) N10 0.0654(19) 0.0334(14) 0.0592(18) 0.0202(13) 0.0336(16) 0.0274(14) C1 0.0464(18) 0.0477(19) 0.0444(18) 0.0127(15) 0.0224(15) 0.0253(16) C2 0.055(2) 0.0452(18) 0.0407(17) 0.0146(14) 0.0239(16) 0.0290(16) C3 0.0521(19) 0.0391(17) 0.0388(17) 0.0092(14) 0.0160(15) 0.0254(15) C4 0.0452(18) 0.0397(17) 0.0487(19) 0.0151(14) 0.0195(15) 0.0235(15) C5 0.0436(18) 0.0447(18) 0.0501(19) 0.0181(15) 0.0229(15) 0.0271(15) C6 0.0439(18) 0.056(2) 0.053(2) 0.0179(16) 0.0243(16) 0.0313(17) C7 0.054(2) 0.073(3) 0.052(2) 0.0233(19) 0.0269(18) 0.042(2) C8 0.053(2) 0.085(3) 0.055(2) 0.021(2) 0.0248(19) 0.044(2) C9 0.051(2) 0.088(3) 0.052(2) 0.009(2) 0.0176(18) 0.031(2) C10 0.052(2) 0.059(2) 0.061(2) 0.0115(19) 0.0187(19) 0.0235(19) C11 0.0404(18) 0.058(2) 0.0458(19) 0.0123(16) 0.0212(15) 0.0226(16) C12 0.071(3) 0.045(2) 0.066(2) 0.0176(18) 0.032(2) 0.0232(19) C13 0.055(2) 0.0346(16) 0.0485(19) 0.0167(14) 0.0209(16) 0.0242(15) C14 0.055(2) 0.0402(18) 0.065(2) 0.0212(16) 0.0287(18) 0.0247(16) C15 0.072(3) 0.053(2) 0.091(3) 0.029(2) 0.044(2) 0.031(2) C16 0.087(3) 0.050(2) 0.098(4) 0.036(2) 0.051(3) 0.027(2) C17 0.100(3) 0.037(2) 0.089(3) 0.027(2) 0.045(3) 0.035(2) C18 0.069(2) 0.0388(18) 0.058(2) 0.0211(16) 0.0280(19) 0.0321(17) C19 0.107(3) 0.048(2) 0.087(3) 0.024(2) 0.052(3) 0.055(2) C20 0.0541(19) 0.0385(17) 0.0393(17) 0.0131(13) 0.0189(15) 0.0305(15) C21 0.054(2) 0.0410(17) 0.0467(18) 0.0120(14) 0.0209(16) 0.0313(16) C22 0.0491(19) 0.0384(17) 0.0433(18) 0.0110(14) 0.0183(15) 0.0234(15) C23 0.045(2) 0.079(3) 0.061(2) 0.018(2) 0.0201(18) 0.027(2) C24 0.055(2) 0.0385(17) 0.0440(18) 0.0122(14) 0.0164(16) 0.0227(16) C25 0.053(2) 0.059(2) 0.050(2) 0.0080(17) 0.0061(17) 0.0255(18) C26 0.076(3) 0.060(2) 0.044(2) 0.0127(17) 0.0092(19) 0.032(2) C27 0.082(3) 0.052(2) 0.045(2) 0.0159(17) 0.025(2) 0.036(2) C28 0.060(2) 0.0433(19) 0.048(2) 0.0145(15) 0.0207(17) 0.0265(17) C29 0.054(2) 0.0369(16) 0.0388(17) 0.0076(13) 0.0146(15) 0.0254(15) C30 0.056(2) 0.0357(17) 0.052(2) 0.0135(15) 0.0292(17) 0.0192(15) C31 0.060(2) 0.0432(19) 0.051(2) 0.0114(16) 0.0185(18) 0.0194(17) C32 0.066(3) 0.052(2) 0.062(2) 0.0137(19) 0.020(2) 0.0121(19) C33 0.072(3) 0.040(2) 0.076(3) 0.0124(19) 0.029(2) 0.0035(19) C34 0.070(3) 0.0374(19) 0.072(3) 0.0217(18) 0.037(2) 0.0174(18) C35 0.057(2) 0.0402(18) 0.051(2) 0.0132(15) 0.0266(18) 0.0194(16) C36 0.085(3) 0.044(2) 0.077(3) 0.0302(19) 0.028(2) 0.038(2) C37 0.057(2) 0.0357(16) 0.0465(18) 0.0148(14) 0.0250(16) 0.0269(15) C38 0.059(2) 0.0377(17) 0.0496(19) 0.0163(15) 0.0210(17) 0.0300(16) C39 0.129(5) 0.075(3) 0.101(4) 0.017(3) 0.070(4) 0.061(3) C40 0.144(6) 0.122(5) 0.136(6) 0.022(4) 0.078(5) 0.089(5) C41 0.128(6) 0.185(8) 0.097(5) 0.000(5) 0.043(4) 0.100(6) Cl1 0.102(5) 0.058(4) 0.108(7) 0.020(3) 0.024(3) 0.034(3) O2 0.107(9) 0.122(9) 0.094(8) 0.023(7) -0.005(7) 0.027(7) O3 0.115(9) 0.073(6) 0.117(11) 0.012(7) 0.073(9) 0.015(7) O4 0.096(6) 0.072(5) 0.120(7) 0.015(4) 0.027(5) 0.059(4) O5 0.087(9) 0.045(7) 0.125(19) 0.028(8) 0.053(12) 0.038(6) Cl1' 0.094(4) 0.042(2) 0.065(2) 0.0153(17) 0.046(3) 0.038(2) O2' 0.117(8) 0.076(5) 0.119(8) 0.001(5) 0.072(7) 0.038(5) O3' 0.082(6) 0.102(6) 0.109(6) 0.001(5) 0.026(5) 0.033(4) O4' 0.141(10) 0.052(5) 0.082(6) 0.013(4) 0.024(6) 0.044(6) O5' 0.082(7) 0.041(9) 0.106(12) 0.013(8) 0.022(7) 0.023(6) Cl2 0.065(3) 0.059(3) 0.046(3) 0.0224(16) 0.0225(19) 0.042(2) O6 0.085(7) 0.088(9) 0.091(9) 0.018(5) 0.032(5) 0.066(8) O7 0.117(12) 0.122(7) 0.050(3) 0.023(3) 0.011(4) 0.068(8) O8 0.126(10) 0.060(5) 0.102(8) 0.037(5) 0.030(8) 0.038(6) O9 0.059(4) 0.117(6) 0.097(9) -0.006(6) 0.021(5) 0.029(3) Cl2' 0.08(2) 0.076(13) 0.059(10) 0.029(8) 0.025(9) 0.049(12) O6' 0.073(13) 0.09(2) 0.070(11) 0.033(12) 0.034(9) 0.051(15) O7' 0.10(2) 0.092(11) 0.055(8) 0.018(7) 0.010(11) 0.038(13) O8' 0.10(2) 0.078(19) 0.074(12) 0.022(12) 0.015(12) 0.067(16) O9' 0.08(2) 0.089(13) 0.09(2) 0.033(14) 0.048(18) 0.036(14) Cl3 0.062(2) 0.0573(16) 0.0459(13) 0.0113(10) 0.0251(13) 0.0290(11) O10 0.120(9) 0.074(4) 0.085(6) -0.021(4) 0.043(6) 0.011(5) O11 0.083(9) 0.075(4) 0.060(4) 0.033(3) 0.039(5) 0.046(5) O12 0.060(6) 0.074(7) 0.070(12) 0.026(7) 0.026(8) 0.029(5) O13 0.080(4) 0.121(10) 0.076(5) 0.053(6) 0.038(4) 0.065(6) Cl3' 0.086(18) 0.070(15) 0.058(9) 0.020(9) 0.023(9) 0.025(9) O10' 0.11(3) 0.067(15) 0.079(18) 0.000(11) 0.03(2) 0.022(16) O11' 0.07(3) 0.07(3) 0.06(3) 0.02(2) 0.02(2) 0.03(2) O12' 0.07(3) 0.07(2) 0.04(2) -0.003(18) 0.02(2) 0.030(17) O13' 0.084(15) 0.09(4) 0.070(18) 0.03(2) 0.011(14) 0.020(16) _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 1.804(2) . ? Fe1 N5 2.076(3) . ? Fe1 N7 2.081(3) . ? Fe1 N9 2.117(3) . ? Fe1 N2 2.293(3) . ? Fe1 N1 2.318(3) . ? O1 C39 1.392(5) . ? N1 C2 1.483(4) . ? N1 C1 1.486(4) . ? N1 C21 1.490(4) . ? N2 C4 1.492(4) . ? N2 C38 1.493(4) . ? N2 C3 1.499(4) . ? N3 C5 1.337(4) . ? N3 C6 1.391(5) . ? N3 H3 0.8800 . ? N4 C5 1.332(4) . ? N4 C11 1.407(5) . ? N4 C12 1.462(5) . ? N5 C20 1.328(4) . ? N5 C13 1.402(4) . ? N6 C20 1.339(4) . ? N6 C18 1.388(5) . ? N6 C19 1.476(4) . ? N7 C22 1.332(4) . ? N7 C29 1.389(4) . ? N8 C22 1.348(4) . ? N8 C24 1.385(4) . ? N8 C23 1.464(5) . ? N9 C37 1.324(4) . ? N9 C30 1.403(4) . ? N10 C37 1.351(4) . ? N10 C35 1.391(5) . ? N10 C36 1.473(5) . ? C1 C22 1.498(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.516(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.506(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 C11 1.371(5) . ? C6 C7 1.397(5) . ? C7 C8 1.360(6) . ? C7 H7 0.9500 . ? C8 C9 1.395(6) . ? C8 H8 0.9500 . ? C9 C10 1.376(6) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.380(5) . ? C13 C18 1.399(5) . ? C14 C15 1.392(5) . ? C14 H14 0.9500 . ? C15 C16 1.390(6) . ? C15 H15 0.9500 . ? C16 C17 1.394(6) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.492(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.389(5) . ? C24 C29 1.398(5) . ? C25 C26 1.374(6) . ? C25 H25 0.9500 . ? C26 C27 1.393(6) . ? C26 H26 0.9500 . ? C27 C28 1.388(5) . ? C27 H27 0.9500 . ? C28 C29 1.397(5) . ? C28 H28 0.9500 . ? C30 C31 1.396(5) . ? C30 C35 1.402(5) . ? C31 C32 1.385(5) . ? C31 H31 0.9500 . ? C32 C33 1.400(6) . ? C32 H32 0.9500 . ? C33 C34 1.366(6) . ? C33 H33 0.9500 . ? C34 C35 1.393(5) . ? C34 H34 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.481(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.487(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.452(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? Cl1 O3 1.394(15) . ? Cl1 O4 1.402(15) . ? Cl1 O5 1.41(3) . ? Cl1 O2 1.417(18) . ? Cl1' O2' 1.407(11) . ? Cl1' O5' 1.43(3) . ? Cl1' O4' 1.452(14) . ? Cl1' O3' 1.455(15) . ? Cl2 O8 1.39(2) . ? Cl2 O7 1.408(19) . ? Cl2 O6 1.42(2) . ? Cl2 O9 1.44(3) . ? Cl2' O8' 1.39(6) . ? Cl2' O6' 1.40(6) . ? Cl2' O7' 1.40(7) . ? Cl2' O9' 1.41(7) . ? Cl3 O10 1.417(13) . ? Cl3 O12 1.43(3) . ? Cl3 O11 1.43(3) . ? Cl3 O13 1.429(10) . ? Cl3' O10' 1.39(6) . ? Cl3' O12' 1.40(13) . ? Cl3' O11' 1.40(13) . ? Cl3' O13' 1.40(5) . ? 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 N5 96.69(11) . . ? O1 Fe1 N7 104.86(11) . . ? N5 Fe1 N7 94.56(11) . . ? O1 Fe1 N9 98.46(11) . . ? N5 Fe1 N9 161.10(11) . . ? N7 Fe1 N9 92.41(11) . . ? O1 Fe1 N2 102.21(11) . . ? N5 Fe1 N2 88.85(10) . . ? N7 Fe1 N2 152.10(10) . . ? N9 Fe1 N2 76.96(10) . . ? O1 Fe1 N1 173.33(10) . . ? N5 Fe1 N1 76.76(10) . . ? N7 Fe1 N1 74.72(10) . . ? N9 Fe1 N1 88.21(10) . . ? N2 Fe1 N1 79.17(10) . . ? C39 O1 Fe1 143.4(3) . . ? C2 N1 C1 113.6(3) . . ? C2 N1 C21 111.9(3) . . ? C1 N1 C21 109.5(3) . . ? C2 N1 Fe1 105.72(18) . . ? C1 N1 Fe1 105.71(19) . . ? C21 N1 Fe1 110.17(19) . . ? C4 N2 C38 110.7(2) . . ? C4 N2 C3 111.4(3) . . ? C38 N2 C3 111.1(3) . . ? C4 N2 Fe1 107.54(19) . . ? C38 N2 Fe1 110.5(2) . . ? C3 N2 Fe1 105.31(18) . . ? C5 N3 C6 108.4(3) . . ? C5 N3 H3 125.8 . . ? C6 N3 H3 125.8 . . ? C5 N4 C11 107.5(3) . . ? C5 N4 C12 127.9(3) . . ? C11 N4 C12 124.5(3) . . ? C20 N5 C13 105.7(3) . . ? C20 N5 Fe1 117.1(2) . . ? C13 N5 Fe1 134.9(2) . . ? C20 N6 C18 107.4(3) . . ? C20 N6 C19 126.5(3) . . ? C18 N6 C19 126.1(3) . . ? C22 N7 C29 106.1(3) . . ? C22 N7 Fe1 116.4(2) . . ? C29 N7 Fe1 136.8(2) . . ? C22 N8 C24 107.2(3) . . ? C22 N8 C23 127.4(3) . . ? C24 N8 C23 125.5(3) . . ? C37 N9 C30 105.9(3) . . ? C37 N9 Fe1 116.4(2) . . ? C30 N9 Fe1 136.6(2) . . ? C37 N10 C35 107.7(3) . . ? C37 N10 C36 126.6(3) . . ? C35 N10 C36 125.7(3) . . ? N1 C1 C22 106.7(3) . . ? N1 C1 H1A 110.4 . . ? C22 C1 H1A 110.4 . . ? N1 C1 H1B 110.4 . . ? C22 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? N1 C2 C3 109.6(3) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 110.6(3) . . ? N2 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N2 C4 C5 114.6(3) . . ? N2 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N2 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N4 C5 N3 110.1(3) . . ? N4 C5 C4 123.8(3) . . ? N3 C5 C4 126.0(3) . . ? C11 C6 N3 106.8(3) . . ? C11 C6 C7 121.6(4) . . ? N3 C6 C7 131.6(4) . . ? C8 C7 C6 116.1(4) . . ? C8 C7 H7 122.0 . . ? C6 C7 H7 122.0 . . ? C7 C8 C9 122.7(4) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 116.4(4) . . ? C9 C10 H10 121.8 . . ? C11 C10 H10 121.8 . . ? C6 C11 C10 122.1(4) . . ? C6 C11 N4 107.1(3) . . ? C10 C11 N4 130.8(4) . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.0(3) . . ? C14 C13 N5 130.8(3) . . ? C18 C13 N5 108.1(3) . . ? C13 C14 C15 116.9(3) . . ? C13 C14 H14 121.5 . . ? C15 C14 H14 121.5 . . ? C16 C15 C14 121.8(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 121.7(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 115.9(4) . . ? C18 C17 H17 122.0 . . ? C16 C17 H17 122.0 . . ? C17 C18 N6 131.3(3) . . ? C17 C18 C13 122.6(4) . . ? N6 C18 C13 106.1(3) . . ? N6 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 N6 112.7(3) . . ? N5 C20 C21 122.5(3) . . ? N6 C20 C21 124.8(3) . . ? N1 C21 C20 110.2(3) . . ? N1 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? N1 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N7 C22 N8 112.2(3) . . ? N7 C22 C1 120.4(3) . . ? N8 C22 C1 127.4(3) . . ? N8 C23 H23A 109.5 . . ? N8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N8 C24 C25 131.6(3) . . ? N8 C24 C29 106.2(3) . . ? C25 C24 C29 122.2(3) . . ? C26 C25 C24 116.3(4) . . ? C26 C25 H25 121.9 . . ? C24 C25 H25 121.9 . . ? C25 C26 C27 122.4(4) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C28 C27 C26 121.7(4) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 116.4(4) . . ? C27 C28 H28 121.8 . . ? C29 C28 H28 121.8 . . ? N7 C29 C28 130.6(3) . . ? N7 C29 C24 108.4(3) . . ? C28 C29 C24 121.0(3) . . ? C31 C30 C35 119.4(3) . . ? C31 C30 N9 131.9(3) . . ? C35 C30 N9 108.6(3) . . ? C32 C31 C30 117.5(4) . . ? C32 C31 H31 121.2 . . ? C30 C31 H31 121.2 . . ? C31 C32 C33 121.7(4) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 121.8(4) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 116.4(4) . . ? C33 C34 H34 121.8 . . ? C35 C34 H34 121.8 . . ? N10 C35 C34 131.5(4) . . ? N10 C35 C30 105.5(3) . . ? C34 C35 C30 123.1(4) . . ? N10 C36 H36A 109.5 . . ? N10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 N10 112.3(3) . . ? N9 C37 C38 122.9(3) . . ? N10 C37 C38 124.8(3) . . ? C37 C38 N2 110.8(3) . . ? C37 C38 H38A 109.5 . . ? N2 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? O1 C39 C40 113.8(5) . . ? O1 C39 H39A 108.8 . . ? C40 C39 H39A 108.8 . . ? O1 C39 H39B 108.8 . . ? C40 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C41 C40 C39 116.7(6) . . ? C41 C40 H40A 108.1 . . ? C39 C40 H40A 108.1 . . ? C41 C40 H40B 108.1 . . ? C39 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 Cl1 O4 113.4(12) . . ? O3 Cl1 O5 125.2(16) . . ? O4 Cl1 O5 107.5(18) . . ? O3 Cl1 O2 105.2(15) . . ? O4 Cl1 O2 105.5(11) . . ? O5 Cl1 O2 97(2) . . ? O2' Cl1' O5' 129.3(16) . . ? O2' Cl1' O4' 114.1(8) . . ? O5' Cl1' O4' 94.8(15) . . ? O2' Cl1' O3' 104.6(10) . . ? O5' Cl1' O3' 108.5(15) . . ? O4' Cl1' O3' 102.6(8) . . ? O8 Cl2 O7 108.2(13) . . ? O8 Cl2 O6 115.6(16) . . ? O7 Cl2 O6 113.5(16) . . ? O8 Cl2 O9 109.8(16) . . ? O7 Cl2 O9 106.2(13) . . ? O6 Cl2 O9 103.0(16) . . ? O8' Cl2' O6' 102(4) . . ? O8' Cl2' O7' 128(5) . . ? O6' Cl2' O7' 103(5) . . ? O8' Cl2' O9' 101(5) . . ? O6' Cl2' O9' 115(4) . . ? O7' Cl2' O9' 108(3) . . ? O10 Cl3 O12 108.8(11) . . ? O10 Cl3 O11 112.4(15) . . ? O12 Cl3 O11 112.2(19) . . ? O10 Cl3 O13 109.9(8) . . ? O12 Cl3 O13 105.9(16) . . ? O11 Cl3 O13 107.5(10) . . ? O10' Cl3' O12' 109(5) . . ? O10' Cl3' O11' 97(5) . . ? O12' Cl3' O11' 100(8) . . ? O10' Cl3' O13' 109(4) . . ? O12' Cl3' O13' 122(7) . . ? O11' Cl3' O13' 117(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.602 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.073 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.003 0.500 0.500 397 172 2(CH3CH2CH2OH) 2 0.500 0.500 1.000 203 89 '4(CH3CN) ' _platon_squeeze_details ; The unit cell contains 2 n-PrOH and 4 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ;