#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Malcolm A. Halcrow' _publ_contact_author_address ; Department of Chemistry University of Leeds Woodhouse Lane LEEDS LS2 9JT UNITED KINGDOM ; _publ_contact_author_email M.A.HALCROW@LEEDS.AC.UK _publ_section_title ; The Influence of Ligand Conformation on the Thermal Spin Transitions in Iron(III) Saltrien Complexes ; loop_ _publ_author_name 'Malcolm A Halcrow' 'Simon A Barrett' 'Colin A Kilner' 'Ruth Pritchard' data_rpfe7i _database_code_depnum_ccdc_archive 'CCDC 676630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(5-methylsalicylaldiminato)-3,6-diazaoctane]iron(iii) hexafluorophosphate ; _chemical_name_common ; (1,8-Bis(5-methylsalicylaldiminato)-3,6-diazaoctane)iron(iii) hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C22 H28 Fe N4 O2, F6 P' _chemical_formula_sum 'C22 H28 F6 Fe N4 O2 P' _chemical_formula_weight 581.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 10.3752(9) _cell_length_b 13.3931(11) _cell_length_c 19.3373(17) _cell_angle_alpha 107.903(4) _cell_angle_beta 90.780(4) _cell_angle_gamma 101.238(4) _cell_volume 2500.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54204 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 28.08 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 1.196 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54204 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.08 _reflns_number_total 12097 _reflns_number_gt 10576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two cations and two anions, all lying on general crystallographic positions. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0461P)^2^+2.1586P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12097 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.85970(2) 0.530478(18) 0.291005(13) 0.01739(6) Uani 1 1 d . . . N2A N 0.84114(14) 0.37353(12) 0.30015(8) 0.0207(3) Uani 1 1 d . . . C3A C 0.74388(18) 0.34418(15) 0.34987(10) 0.0265(4) Uani 1 1 d . . . H3A H 0.7894 0.3529 0.3973 0.032 Uiso 1 1 calc R . . H3B H 0.6976 0.2683 0.3286 0.032 Uiso 1 1 calc R . . C4A C 0.64470(18) 0.41748(15) 0.36081(11) 0.0284(4) Uani 1 1 d . . . H4A H 0.5827 0.3944 0.3168 0.034 Uiso 1 1 calc R . . H4B H 0.5931 0.4116 0.4026 0.034 Uiso 1 1 calc R . . N5A N 0.71400(15) 0.53147(12) 0.37482(8) 0.0243(3) Uani 1 1 d . . . H5A H 0.6519 0.5687 0.3662 0.029 Uiso 1 1 calc R . . C6A C 0.7755(2) 0.58816(17) 0.45043(10) 0.0326(4) Uani 1 1 d . . . H6A H 0.7316 0.5523 0.4842 0.039 Uiso 1 1 calc R . . H6B H 0.7632 0.6631 0.4660 0.039 Uiso 1 1 calc R . . C7A C 0.9230(2) 0.58781(17) 0.45423(10) 0.0317(4) Uani 1 1 d . . . H7A H 0.9661 0.6383 0.5014 0.038 Uiso 1 1 calc R . . H7B H 0.9356 0.5151 0.4509 0.038 Uiso 1 1 calc R . . N8A N 0.98376(15) 0.62037(12) 0.39303(8) 0.0237(3) Uani 1 1 d . . . H8A H 1.0648 0.6001 0.3881 0.028 Uiso 1 1 calc R . . C9A C 1.00851(18) 0.73868(15) 0.40570(10) 0.0264(4) Uani 1 1 d . . . H9A H 1.0928 0.7744 0.4355 0.032 Uiso 1 1 calc R . . H9B H 0.9368 0.7690 0.4321 0.032 Uiso 1 1 calc R . . C10A C 1.01424(17) 0.75696(14) 0.33149(10) 0.0245(4) Uani 1 1 d . . . H10A H 1.0175 0.8335 0.3372 0.029 Uiso 1 1 calc R . . H10B H 1.0939 0.7368 0.3082 0.029 Uiso 1 1 calc R . . N11A N 0.89406(14) 0.68906(11) 0.28639(8) 0.0195(3) Uani 1 1 d . . . C12A C 0.89528(17) 0.29812(14) 0.25992(9) 0.0217(3) Uani 1 1 d . . . H12A H 0.8649 0.2277 0.2624 0.026 Uiso 1 1 calc R . . C13A C 0.99818(16) 0.31243(13) 0.21161(9) 0.0196(3) Uani 1 1 d . . . C14A C 1.05610(16) 0.41495(13) 0.20529(9) 0.0196(3) Uani 1 1 d . . . C15A C 1.16413(17) 0.42003(14) 0.16159(10) 0.0236(3) Uani 1 1 d . . . H15A H 1.2091 0.4878 0.1593 0.028 Uiso 1 1 calc R . . C16A C 1.20575(18) 0.32759(14) 0.12185(10) 0.0240(3) Uani 1 1 d . . . H16A H 1.2770 0.3338 0.0920 0.029 Uiso 1 1 calc R . . C17A C 1.14515(18) 0.22502(14) 0.12460(10) 0.0233(3) Uani 1 1 d . . . C18A C 1.04393(18) 0.22004(14) 0.17056(10) 0.0226(3) Uani 1 1 d . . . H18A H 1.0037 0.1523 0.1747 0.027 Uiso 1 1 calc R . . O19A O 1.01235(13) 0.50321(10) 0.23792(7) 0.0238(3) Uani 1 1 d . . . C20A C 0.83094(16) 0.72715(13) 0.24556(9) 0.0198(3) Uani 1 1 d . . . H20A H 0.8635 0.7992 0.2471 0.024 Uiso 1 1 calc R . . C21A C 0.71338(16) 0.66711(13) 0.19740(9) 0.0187(3) Uani 1 1 d . . . C22A C 0.65943(17) 0.55672(13) 0.18745(9) 0.0207(3) Uani 1 1 d . . . C23A C 0.54437(19) 0.50806(15) 0.13956(11) 0.0285(4) Uani 1 1 d . . . H23A H 0.5040 0.4355 0.1334 0.034 Uiso 1 1 calc R . . C24A C 0.48901(18) 0.56404(16) 0.10136(11) 0.0285(4) Uani 1 1 d . . . H24A H 0.4124 0.5283 0.0692 0.034 Uiso 1 1 calc R . . C25A C 0.54336(18) 0.67229(15) 0.10895(10) 0.0254(4) Uani 1 1 d . . . C26A C 0.65394(17) 0.72156(14) 0.15748(9) 0.0221(3) Uani 1 1 d . . . H26A H 0.6915 0.7948 0.1643 0.027 Uiso 1 1 calc R . . O27A O 0.71289(13) 0.49830(10) 0.21975(7) 0.0262(3) Uani 1 1 d . . . C28A C 1.1886(2) 0.12442(15) 0.07845(11) 0.0312(4) Uani 1 1 d . . . H28A H 1.1999 0.0796 0.1088 0.047 Uiso 1 1 calc R . . H28B H 1.2725 0.1450 0.0586 0.047 Uiso 1 1 calc R . . H28C H 1.1215 0.0840 0.0383 0.047 Uiso 1 1 calc R . . C29A C 0.4832(2) 0.73141(18) 0.06538(12) 0.0380(5) Uani 1 1 d . . . H29A H 0.4778 0.8029 0.0974 0.057 Uiso 1 1 calc R . . H29B H 0.3945 0.6909 0.0449 0.057 Uiso 1 1 calc R . . H29C H 0.5384 0.7385 0.0258 0.057 Uiso 1 1 calc R . . Fe1B Fe 0.36399(2) 1.015388(19) 0.266340(13) 0.01879(6) Uani 1 1 d . . . N2B N 0.34812(14) 0.84880(12) 0.25187(8) 0.0216(3) Uani 1 1 d . . . C3B C 0.46093(18) 0.82858(15) 0.28941(10) 0.0264(4) Uani 1 1 d . . . H3C H 0.5417 0.8404 0.2639 0.032 Uiso 1 1 calc R . . H3D H 0.4427 0.7537 0.2905 0.032 Uiso 1 1 calc R . . C4B C 0.47837(19) 0.90681(16) 0.36644(10) 0.0289(4) Uani 1 1 d . . . H4C H 0.4016 0.8893 0.3936 0.035 Uiso 1 1 calc R . . H4D H 0.5586 0.9021 0.3925 0.035 Uiso 1 1 calc R . . N5B N 0.49029(15) 1.01728(13) 0.36143(8) 0.0261(3) Uani 1 1 d . . . H5B H 0.5773 1.0408 0.3531 0.031 Uiso 1 1 calc R . . C6B C 0.4627(2) 1.09452(19) 0.43048(11) 0.0364(5) Uani 1 1 d . . . H6C H 0.5057 1.1686 0.4333 0.044 Uiso 1 1 calc R . . H6D H 0.4979 1.0784 0.4728 0.044 Uiso 1 1 calc R . . C7B C 0.3134(2) 1.0843(2) 0.43174(11) 0.0371(5) Uani 1 1 d . . . H7C H 0.2712 1.0128 0.4344 0.045 Uiso 1 1 calc R . . H7D H 0.2925 1.1396 0.4749 0.045 Uiso 1 1 calc R . . N8B N 0.26312(15) 1.09902(13) 0.36355(8) 0.0270(3) Uani 1 1 d . . . H8B H 0.1737 1.0679 0.3554 0.032 Uiso 1 1 calc R . . C9B C 0.2779(2) 1.21515(16) 0.37125(11) 0.0323(4) Uani 1 1 d . . . H9C H 0.3612 1.2567 0.4004 0.039 Uiso 1 1 calc R . . H9D H 0.2038 1.2429 0.3966 0.039 Uiso 1 1 calc R . . C10B C 0.27911(19) 1.22742(16) 0.29580(11) 0.0304(4) Uani 1 1 d . . . H10C H 0.1915 1.1948 0.2689 0.036 Uiso 1 1 calc R . . H10D H 0.3006 1.3043 0.2995 0.036 Uiso 1 1 calc R . . N11B N 0.38072(14) 1.17203(12) 0.25736(8) 0.0223(3) Uani 1 1 d . . . C12B C 0.26297(17) 0.76838(14) 0.21019(9) 0.0222(3) Uani 1 1 d . . . H12B H 0.2743 0.6985 0.2071 0.027 Uiso 1 1 calc R . . C13B C 0.15091(17) 0.77640(13) 0.16761(9) 0.0204(3) Uani 1 1 d . . . C14B C 0.12492(17) 0.87746(13) 0.16785(9) 0.0206(3) Uani 1 1 d . . . C15B C 0.01254(18) 0.87549(14) 0.12398(10) 0.0244(3) Uani 1 1 d . . . H15B H -0.0086 0.9412 0.1236 0.029 Uiso 1 1 calc R . . C16B C -0.06673(18) 0.77901(15) 0.08164(10) 0.0244(3) Uani 1 1 d . . . H16B H -0.1394 0.7805 0.0519 0.029 Uiso 1 1 calc R . . C17B C -0.04237(17) 0.67856(14) 0.08156(9) 0.0232(3) Uani 1 1 d . . . C18B C 0.06562(18) 0.67965(14) 0.12492(10) 0.0236(3) Uani 1 1 d . . . H18B H 0.0833 0.6132 0.1262 0.028 Uiso 1 1 calc R . . O19B O 0.19961(12) 0.97085(10) 0.20649(7) 0.0250(3) Uani 1 1 d . . . C20B C 0.45298(17) 1.21447(14) 0.21556(10) 0.0230(3) Uani 1 1 d . . . H20B H 0.4401 1.2816 0.2131 0.028 Uiso 1 1 calc R . . C21B C 0.55217(17) 1.16799(13) 0.17213(9) 0.0208(3) Uani 1 1 d . . . C22B C 0.57689(17) 1.06569(13) 0.16946(9) 0.0217(3) Uani 1 1 d . . . C23B C 0.67676(19) 1.02821(15) 0.12547(11) 0.0294(4) Uani 1 1 d . . . H23B H 0.6964 0.9609 0.1232 0.035 Uiso 1 1 calc R . . C24B C 0.74633(19) 1.08852(15) 0.08566(11) 0.0293(4) Uani 1 1 d . . . H24B H 0.8113 1.0604 0.0560 0.035 Uiso 1 1 calc R . . C25B C 0.72377(18) 1.18993(15) 0.08784(10) 0.0251(4) Uani 1 1 d . . . C26B C 0.62746(18) 1.22806(14) 0.13153(10) 0.0244(3) Uani 1 1 d . . . H26B H 0.6112 1.2966 0.1345 0.029 Uiso 1 1 calc R . . O27B O 0.51068(13) 1.00533(10) 0.20579(7) 0.0267(3) Uani 1 1 d . . . C28B C -0.1331(2) 0.57443(15) 0.03647(11) 0.0309(4) Uani 1 1 d . . . H28D H -0.1147 0.5590 -0.0149 0.046 Uiso 1 1 calc R . . H28E H -0.2250 0.5814 0.0416 0.046 Uiso 1 1 calc R . . H28F H -0.1181 0.5157 0.0536 0.046 Uiso 1 1 calc R . . C29B C 0.8045(2) 1.25555(18) 0.04555(11) 0.0331(4) Uani 1 1 d . . . H29D H 0.7805 1.3258 0.0570 0.050 Uiso 1 1 calc R . . H29E H 0.7864 1.2177 -0.0068 0.050 Uiso 1 1 calc R . . H29F H 0.8985 1.2654 0.0592 0.050 Uiso 1 1 calc R . . P30 P 0.36005(5) 0.60053(4) 0.40429(3) 0.02823(11) Uani 1 1 d . A 3 F31 F 0.43260(15) 0.53828(17) 0.44590(10) 0.0699(5) Uani 1 1 d . A 3 F32 F 0.49259(15) 0.69008(14) 0.41592(11) 0.0666(5) Uani 1 1 d . A 3 F33 F 0.28616(14) 0.66116(15) 0.36158(10) 0.0632(5) Uani 1 1 d . A 3 F34 F 0.22731(15) 0.50985(14) 0.39117(12) 0.0676(5) Uani 1 1 d . A 3 F35 F 0.41200(18) 0.53578(16) 0.32948(9) 0.0681(5) Uani 1 1 d . A 3 F36 F 0.30792(19) 0.66339(17) 0.47860(10) 0.0764(6) Uani 1 1 d . A 3 P37 P -0.12343(5) 1.06076(4) 0.37801(3) 0.03209(12) Uani 1 1 d . B 3 F38 F -0.01389(15) 1.05319(17) 0.43393(10) 0.0707(5) Uani 1 1 d . B 3 F39 F -0.03195(14) 1.02266(15) 0.31273(8) 0.0646(5) Uani 1 1 d . B 3 F40 F -0.23130(14) 1.07232(17) 0.32179(10) 0.0681(5) Uani 1 1 d . B 3 F41 F -0.21678(14) 1.09506(14) 0.44306(8) 0.0594(4) Uani 1 1 d . B 3 F42 F -0.05212(17) 1.18255(13) 0.39227(12) 0.0758(6) Uani 1 1 d . B 3 F43 F -0.19638(17) 0.93907(12) 0.36362(12) 0.0735(6) Uani 1 1 d . B 3 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 Fe1A 0.01895(12) 0.01723(11) 0.01678(12) 0.00493(9) 0.00070(9) 0.00642(9) N2A 0.0208(7) 0.0231(7) 0.0211(7) 0.0100(6) 0.0041(6) 0.0066(6) C3A 0.0280(9) 0.0275(9) 0.0283(9) 0.0136(7) 0.0101(7) 0.0079(7) C4A 0.0224(8) 0.0290(9) 0.0344(10) 0.0105(8) 0.0084(7) 0.0060(7) N5A 0.0226(7) 0.0269(8) 0.0251(8) 0.0075(6) 0.0059(6) 0.0098(6) C6A 0.0392(11) 0.0347(10) 0.0208(9) 0.0054(8) 0.0099(8) 0.0054(8) C7A 0.0388(11) 0.0365(10) 0.0197(9) 0.0105(8) -0.0034(8) 0.0054(9) N8A 0.0218(7) 0.0287(8) 0.0200(7) 0.0056(6) -0.0009(6) 0.0074(6) C9A 0.0257(9) 0.0271(9) 0.0207(8) 0.0013(7) -0.0030(7) 0.0027(7) C10A 0.0203(8) 0.0246(8) 0.0250(9) 0.0055(7) -0.0033(7) 0.0007(7) N11A 0.0193(7) 0.0179(6) 0.0189(7) 0.0026(5) 0.0001(5) 0.0039(5) C12A 0.0247(8) 0.0189(8) 0.0230(8) 0.0087(7) 0.0021(7) 0.0046(6) C13A 0.0214(8) 0.0187(8) 0.0189(8) 0.0050(6) 0.0014(6) 0.0058(6) C14A 0.0214(8) 0.0188(8) 0.0187(8) 0.0049(6) 0.0011(6) 0.0065(6) C15A 0.0242(8) 0.0188(8) 0.0273(9) 0.0069(7) 0.0060(7) 0.0034(6) C16A 0.0226(8) 0.0247(8) 0.0238(9) 0.0055(7) 0.0055(7) 0.0059(7) C17A 0.0268(9) 0.0207(8) 0.0213(8) 0.0034(7) 0.0013(7) 0.0081(7) C18A 0.0269(9) 0.0176(8) 0.0226(8) 0.0051(6) 0.0015(7) 0.0054(7) O19A 0.0279(6) 0.0182(6) 0.0267(6) 0.0068(5) 0.0087(5) 0.0085(5) C20A 0.0217(8) 0.0165(7) 0.0204(8) 0.0045(6) 0.0031(6) 0.0045(6) C21A 0.0191(7) 0.0198(8) 0.0177(8) 0.0055(6) 0.0012(6) 0.0058(6) C22A 0.0215(8) 0.0201(8) 0.0204(8) 0.0063(6) -0.0013(6) 0.0048(6) C23A 0.0270(9) 0.0219(8) 0.0335(10) 0.0085(7) -0.0075(8) -0.0007(7) C24A 0.0231(9) 0.0314(9) 0.0291(10) 0.0085(8) -0.0073(7) 0.0033(7) C25A 0.0256(9) 0.0295(9) 0.0245(9) 0.0109(7) 0.0002(7) 0.0103(7) C26A 0.0246(8) 0.0208(8) 0.0229(8) 0.0085(7) 0.0023(7) 0.0066(7) O27A 0.0295(7) 0.0186(6) 0.0300(7) 0.0088(5) -0.0096(5) 0.0025(5) C28A 0.0384(11) 0.0237(9) 0.0300(10) 0.0029(8) 0.0089(8) 0.0121(8) C29A 0.0409(12) 0.0403(11) 0.0387(12) 0.0188(10) -0.0084(9) 0.0128(9) Fe1B 0.01755(12) 0.01961(12) 0.01736(12) 0.00461(9) 0.00159(9) 0.00155(9) N2B 0.0207(7) 0.0257(7) 0.0211(7) 0.0112(6) 0.0025(6) 0.0051(6) C3B 0.0235(8) 0.0316(9) 0.0278(9) 0.0143(8) 0.0006(7) 0.0068(7) C4B 0.0248(9) 0.0396(11) 0.0255(9) 0.0159(8) 0.0002(7) 0.0053(8) N5B 0.0209(7) 0.0338(8) 0.0209(7) 0.0074(6) -0.0004(6) 0.0020(6) C6B 0.0369(11) 0.0449(12) 0.0215(9) 0.0031(8) -0.0055(8) 0.0075(9) C7B 0.0397(11) 0.0506(13) 0.0205(9) 0.0076(9) 0.0093(8) 0.0134(10) N8B 0.0222(7) 0.0328(8) 0.0233(8) 0.0059(6) 0.0054(6) 0.0042(6) C9B 0.0291(10) 0.0346(10) 0.0281(10) 0.0009(8) 0.0051(8) 0.0095(8) C10B 0.0281(9) 0.0314(10) 0.0321(10) 0.0061(8) 0.0062(8) 0.0130(8) N11B 0.0218(7) 0.0211(7) 0.0222(7) 0.0030(6) 0.0028(6) 0.0064(6) C12B 0.0258(8) 0.0205(8) 0.0223(8) 0.0094(7) 0.0041(7) 0.0051(7) C13B 0.0225(8) 0.0199(8) 0.0178(8) 0.0059(6) 0.0026(6) 0.0019(6) C14B 0.0212(8) 0.0205(8) 0.0183(8) 0.0055(6) 0.0021(6) 0.0011(6) C15B 0.0249(8) 0.0224(8) 0.0257(9) 0.0083(7) -0.0006(7) 0.0036(7) C16B 0.0225(8) 0.0289(9) 0.0197(8) 0.0074(7) -0.0008(6) 0.0009(7) C17B 0.0241(8) 0.0231(8) 0.0171(8) 0.0029(6) 0.0034(6) -0.0014(7) C18B 0.0277(9) 0.0199(8) 0.0213(8) 0.0052(7) 0.0041(7) 0.0024(7) O19B 0.0241(6) 0.0189(6) 0.0283(7) 0.0045(5) -0.0055(5) 0.0016(5) C20B 0.0242(8) 0.0182(8) 0.0258(9) 0.0051(7) -0.0003(7) 0.0057(6) C21B 0.0208(8) 0.0198(8) 0.0202(8) 0.0050(6) 0.0010(6) 0.0024(6) C22B 0.0224(8) 0.0186(8) 0.0216(8) 0.0043(6) 0.0034(6) 0.0015(6) C23B 0.0321(10) 0.0204(8) 0.0359(10) 0.0079(8) 0.0139(8) 0.0072(7) C24B 0.0297(9) 0.0269(9) 0.0280(9) 0.0047(7) 0.0118(8) 0.0039(7) C25B 0.0241(8) 0.0285(9) 0.0212(8) 0.0096(7) 0.0009(7) -0.0006(7) C26B 0.0261(9) 0.0220(8) 0.0261(9) 0.0100(7) 0.0008(7) 0.0036(7) O27B 0.0295(7) 0.0218(6) 0.0330(7) 0.0125(5) 0.0139(5) 0.0084(5) C28B 0.0312(10) 0.0267(9) 0.0255(9) 0.0001(7) -0.0006(8) -0.0022(8) C29B 0.0289(10) 0.0426(11) 0.0326(10) 0.0217(9) 0.0058(8) 0.0022(8) P30 0.0211(2) 0.0365(3) 0.0338(3) 0.0176(2) 0.00646(19) 0.01080(19) F31 0.0492(9) 0.1197(15) 0.0865(12) 0.0786(12) 0.0288(8) 0.0479(10) F32 0.0338(8) 0.0676(11) 0.1006(14) 0.0391(10) -0.0033(8) -0.0039(7) F33 0.0372(7) 0.0890(12) 0.0968(13) 0.0697(11) 0.0135(8) 0.0246(8) F34 0.0358(8) 0.0582(10) 0.1173(15) 0.0456(10) 0.0041(9) 0.0011(7) F35 0.0680(11) 0.0954(13) 0.0453(9) 0.0132(9) 0.0152(8) 0.0414(10) F36 0.0776(12) 0.1025(15) 0.0539(10) 0.0132(10) 0.0270(9) 0.0472(11) P37 0.0214(2) 0.0347(3) 0.0333(3) 0.0004(2) -0.00090(19) 0.0068(2) F38 0.0401(8) 0.1194(16) 0.0643(11) 0.0379(11) -0.0025(7) 0.0303(9) F39 0.0330(7) 0.0923(13) 0.0449(8) -0.0069(8) 0.0124(6) 0.0039(8) F40 0.0289(7) 0.1182(15) 0.0665(11) 0.0478(11) -0.0047(7) 0.0076(8) F41 0.0358(7) 0.0787(11) 0.0423(8) -0.0118(7) 0.0052(6) 0.0124(7) F42 0.0462(9) 0.0421(9) 0.1249(17) 0.0125(10) 0.0048(10) -0.0007(7) F43 0.0585(10) 0.0364(8) 0.1100(15) 0.0039(9) 0.0284(10) 0.0034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1A O27A 1.9304(13) . ? Fe1A O19A 1.9325(12) . ? Fe1A N11A 2.1138(14) . ? Fe1A N2A 2.1351(14) . ? Fe1A N8A 2.2057(15) . ? Fe1A N5A 2.2301(15) . ? N2A C12A 1.300(2) . ? N2A C3A 1.484(2) . ? C3A C4A 1.529(2) . ? C4A N5A 1.495(2) . ? N5A C6A 1.492(3) . ? C6A C7A 1.532(3) . ? C7A N8A 1.489(2) . ? N8A C9A 1.496(2) . ? C9A C10A 1.528(3) . ? C10A N11A 1.478(2) . ? N11A C20A 1.295(2) . ? C12A C13A 1.451(2) . ? C13A C18A 1.422(2) . ? C13A C14A 1.430(2) . ? C14A O19A 1.3266(19) . ? C14A C15A 1.416(2) . ? C15A C16A 1.394(2) . ? C16A C17A 1.412(3) . ? C17A C18A 1.390(2) . ? C17A C28A 1.524(2) . ? C20A C21A 1.459(2) . ? C21A C26A 1.420(2) . ? C21A C22A 1.427(2) . ? C22A O27A 1.330(2) . ? C22A C23A 1.415(2) . ? C23A C24A 1.391(3) . ? C24A C25A 1.411(3) . ? C25A C26A 1.388(3) . ? C25A C29A 1.522(2) . ? Fe1B O19B 1.9311(13) . ? Fe1B O27B 1.9331(13) . ? Fe1B N11B 2.1318(15) . ? Fe1B N2B 2.1342(15) . ? Fe1B N5B 2.2342(15) . ? Fe1B N8B 2.2582(15) . ? N2B C12B 1.291(2) . ? N2B C3B 1.480(2) . ? C3B C4B 1.519(3) . ? C4B N5B 1.494(3) . ? N5B C6B 1.487(3) . ? C6B C7B 1.529(3) . ? C7B N8B 1.494(3) . ? N8B C9B 1.493(3) . ? C9B C10B 1.517(3) . ? C10B N11B 1.484(2) . ? N11B C20B 1.293(2) . ? C12B C13B 1.455(2) . ? C13B C18B 1.421(2) . ? C13B C14B 1.429(2) . ? C14B O19B 1.325(2) . ? C14B C15B 1.424(2) . ? C15B C16B 1.390(3) . ? C16B C17B 1.416(3) . ? C17B C18B 1.385(3) . ? C17B C28B 1.520(2) . ? C20B C21B 1.450(2) . ? C21B C26B 1.426(2) . ? C21B C22B 1.428(2) . ? C22B O27B 1.328(2) . ? C22B C23B 1.419(2) . ? C23B C24B 1.391(3) . ? C24B C25B 1.411(3) . ? C25B C26B 1.389(3) . ? C25B C29B 1.522(2) . ? P30 F36 1.5878(17) . ? P30 F31 1.5969(14) . ? P30 F32 1.6009(16) . ? P30 F33 1.6021(14) . ? P30 F35 1.6022(16) . ? P30 F34 1.6078(16) . ? P37 F42 1.5911(17) . ? P37 F43 1.5941(17) . ? P37 F38 1.5970(16) . ? P37 F39 1.6062(15) . ? P37 F41 1.6071(15) . ? P37 F40 1.6113(16) . ? 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 O27A Fe1A O19A 107.12(6) . . ? O27A Fe1A N11A 86.94(5) . . ? O19A Fe1A N11A 91.16(5) . . ? O27A Fe1A N2A 97.69(5) . . ? O19A Fe1A N2A 86.30(5) . . ? N11A Fe1A N2A 175.21(6) . . ? O27A Fe1A N8A 156.21(6) . . ? O19A Fe1A N8A 91.74(6) . . ? N11A Fe1A N8A 78.12(6) . . ? N2A Fe1A N8A 97.88(6) . . ? O27A Fe1A N5A 87.79(6) . . ? O19A Fe1A N5A 159.79(6) . . ? N11A Fe1A N5A 103.47(6) . . ? N2A Fe1A N5A 78.06(5) . . ? N8A Fe1A N5A 77.99(6) . . ? C12A N2A C3A 117.37(15) . . ? C12A N2A Fe1A 125.66(12) . . ? C3A N2A Fe1A 116.43(11) . . ? N2A C3A C4A 108.55(14) . . ? N5A C4A C3A 110.64(15) . . ? C6A N5A C4A 115.28(15) . . ? C6A N5A Fe1A 112.42(11) . . ? C4A N5A Fe1A 106.59(10) . . ? N5A C6A C7A 110.72(15) . . ? N8A C7A C6A 109.43(15) . . ? C7A N8A C9A 113.59(14) . . ? C7A N8A Fe1A 109.16(11) . . ? C9A N8A Fe1A 111.34(11) . . ? N8A C9A C10A 108.00(14) . . ? N11A C10A C9A 107.14(14) . . ? C20A N11A C10A 119.57(15) . . ? C20A N11A Fe1A 128.10(12) . . ? C10A N11A Fe1A 112.03(11) . . ? N2A C12A C13A 125.51(16) . . ? C18A C13A C14A 119.55(15) . . ? C18A C13A C12A 117.72(15) . . ? C14A C13A C12A 122.72(15) . . ? O19A C14A C15A 119.83(15) . . ? O19A C14A C13A 122.82(15) . . ? C15A C14A C13A 117.35(15) . . ? C16A C15A C14A 121.28(16) . . ? C15A C16A C17A 121.94(16) . . ? C18A C17A C16A 117.11(15) . . ? C18A C17A C28A 121.77(16) . . ? C16A C17A C28A 121.12(16) . . ? C17A C18A C13A 122.57(16) . . ? C14A O19A Fe1A 133.71(11) . . ? N11A C20A C21A 124.58(15) . . ? C26A C21A C22A 119.50(15) . . ? C26A C21A C20A 117.57(15) . . ? C22A C21A C20A 122.90(15) . . ? O27A C22A C23A 119.34(15) . . ? O27A C22A C21A 123.38(15) . . ? C23A C22A C21A 117.27(15) . . ? C24A C23A C22A 121.51(17) . . ? C23A C24A C25A 121.90(17) . . ? C26A C25A C24A 116.95(16) . . ? C26A C25A C29A 121.94(17) . . ? C24A C25A C29A 121.11(17) . . ? C25A C26A C21A 122.81(16) . . ? C22A O27A Fe1A 133.85(11) . . ? O19B Fe1B O27B 110.28(6) . . ? O19B Fe1B N11B 88.83(5) . . ? O27B Fe1B N11B 85.53(5) . . ? O19B Fe1B N2B 85.53(5) . . ? O27B Fe1B N2B 86.89(5) . . ? N11B Fe1B N2B 168.36(6) . . ? O19B Fe1B N5B 151.95(6) . . ? O27B Fe1B N5B 90.89(6) . . ? N11B Fe1B N5B 111.70(6) . . ? N2B Fe1B N5B 77.20(6) . . ? O19B Fe1B N8B 90.50(6) . . ? O27B Fe1B N8B 152.70(6) . . ? N11B Fe1B N8B 77.13(6) . . ? N2B Fe1B N8B 113.04(6) . . ? N5B Fe1B N8B 76.50(6) . . ? C12B N2B C3B 119.24(15) . . ? C12B N2B Fe1B 128.23(12) . . ? C3B N2B Fe1B 112.11(11) . . ? N2B C3B C4B 106.65(15) . . ? N5B C4B C3B 108.03(15) . . ? C6B N5B C4B 112.34(15) . . ? C6B N5B Fe1B 111.76(12) . . ? C4B N5B Fe1B 110.96(11) . . ? N5B C6B C7B 108.35(16) . . ? N8B C7B C6B 108.12(16) . . ? C9B N8B C7B 111.22(16) . . ? C9B N8B Fe1B 110.73(11) . . ? C7B N8B Fe1B 111.26(12) . . ? N8B C9B C10B 108.65(15) . . ? N11B C10B C9B 107.30(15) . . ? C20B N11B C10B 118.87(15) . . ? C20B N11B Fe1B 127.89(12) . . ? C10B N11B Fe1B 112.41(12) . . ? N2B C12B C13B 125.12(16) . . ? C18B C13B C14B 119.86(16) . . ? C18B C13B C12B 117.99(15) . . ? C14B C13B C12B 122.14(15) . . ? O19B C14B C15B 119.52(15) . . ? O19B C14B C13B 123.27(15) . . ? C15B C14B C13B 117.22(15) . . ? C16B C15B C14B 121.14(16) . . ? C15B C16B C17B 122.00(17) . . ? C18B C17B C16B 117.28(16) . . ? C18B C17B C28B 121.87(17) . . ? C16B C17B C28B 120.85(17) . . ? C17B C18B C13B 122.47(16) . . ? C14B O19B Fe1B 135.20(11) . . ? N11B C20B C21B 125.37(16) . . ? C26B C21B C22B 119.66(15) . . ? C26B C21B C20B 118.06(15) . . ? C22B C21B C20B 122.28(15) . . ? O27B C22B C23B 119.51(15) . . ? O27B C22B C21B 122.97(15) . . ? C23B C22B C21B 117.52(16) . . ? C24B C23B C22B 120.98(17) . . ? C23B C24B C25B 122.32(17) . . ? C26B C25B C24B 117.17(16) . . ? C26B C25B C29B 121.72(17) . . ? C24B C25B C29B 121.09(17) . . ? C25B C26B C21B 122.32(16) . . ? C22B O27B Fe1B 135.28(11) . . ? F36 P30 F31 90.29(10) . . ? F36 P30 F32 92.78(11) . . ? F31 P30 F32 89.84(10) . . ? F36 P30 F33 90.30(10) . . ? F31 P30 F33 179.07(12) . . ? F32 P30 F33 90.85(9) . . ? F36 P30 F35 179.32(12) . . ? F31 P30 F35 89.28(10) . . ? F32 P30 F35 87.74(11) . . ? F33 P30 F35 90.13(10) . . ? F36 P30 F34 88.13(11) . . ? F31 P30 F34 90.46(10) . . ? F32 P30 F34 179.03(12) . . ? F33 P30 F34 88.83(9) . . ? F35 P30 F34 91.34(11) . . ? F42 P37 F43 179.38(11) . . ? F42 P37 F38 88.23(11) . . ? F43 P37 F38 92.28(12) . . ? F42 P37 F39 90.47(10) . . ? F43 P37 F39 89.88(10) . . ? F38 P37 F39 89.26(9) . . ? F42 P37 F41 91.29(10) . . ? F43 P37 F41 88.36(9) . . ? F38 P37 F41 90.59(9) . . ? F39 P37 F41 178.23(10) . . ? F42 P37 F40 89.88(11) . . ? F43 P37 F40 89.61(11) . . ? F38 P37 F40 178.10(11) . . ? F39 P37 F40 90.55(9) . . ? F41 P37 F40 89.66(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5A H5A F32 0.93 2.54 3.367(2) 148.9 . N5A H5A F35 0.93 2.50 3.258(2) 139.4 . N8A H8A F33 0.93 2.40 3.178(2) 141.1 1_655 N8A H8A F34 0.93 2.27 3.163(2) 161.3 1_655 N5B H5B F40 0.93 2.09 3.009(2) 171.6 1_655 N5B H5B F41 0.93 2.58 3.231(2) 127.8 1_655 N8B H8B F38 0.93 2.50 3.228(2) 135.4 . N8B H8B F39 0.93 2.18 3.076(2) 162.3 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.889 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.061 #=END data_rp4n _database_code_depnum_ccdc_archive 'CCDC 676631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(5-tert-butylsalicylaldiminato)-3,6-diazaoctane]iron(III) nitrate 1,2-dichloroethane solvate ; _chemical_name_common ; (1,8-Bis(5-tert-butylsalicylaldiminato)-3,6- diazaoctane)iron(iii) nitrate 1,2-dichloroethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 Fe N4 O2, NO3, C2 H4 Cl2' _chemical_formula_sum 'C30 H44 Cl2 Fe N5 O5' _chemical_formula_weight 681.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1177(7) _cell_length_b 21.6263(10) _cell_length_c 9.8296(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.7226(19) _cell_angle_gamma 90.00 _cell_volume 3426.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39440 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.05 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 1.065 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39440 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.05 _reflns_number_total 8261 _reflns_number_gt 6671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was solved by direct methods in the space group P(-1) then, following an initial refinement, transformed to the correct monoclinic symmetry using the ADDSYMM routine in PLATON (Spek, 2005). The nitrate ion N36-O39 is disordered, and was modelled over two orientations labelled 'A' and 'B' with a refined occupancy ration of 0.70:0.30. The N---O bonds lengths and O...O distances within each partial anion were restrained to 1.24(2) and 2.15(1)\%A, respectively. Slightly high thermal parameters on the dichloroethane solvent molecule imply that there may also be some disorder in this residue, although attempts to model this were unsatisfactory. All non-H atoms except the minor nitrate disorder orientation were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The amino group N8---H8 does not form a hydrogen bond in the crystal, but donates a weak N---H...pi interaction to phenoxy ring C13^i^-C18^i^ (symmetry code i: x, 1.5-y, -0.5+z) with H8...X = 2.72\%A and N8---H8...X = 156.8\% (X = centroid of C13^i^-C18^i^). ; _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^)+(0.0466P)^2^+2.6957P] 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 8261 _refine_ls_number_parameters 411 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.432840(15) 0.652048(11) 0.34413(2) 0.02083(8) Uani 1 1 d . . . N2 N 0.32133(9) 0.61842(7) 0.42866(15) 0.0249(3) Uani 1 1 d . . . C3 C 0.31508(12) 0.55068(8) 0.4465(2) 0.0307(4) Uani 1 1 d . . . H3A H 0.2755 0.5333 0.3788 0.037 Uiso 1 1 calc R . . H3B H 0.2946 0.5410 0.5386 0.037 Uiso 1 1 calc R . . C4 C 0.40083(13) 0.52233(9) 0.42733(19) 0.0297(4) Uani 1 1 d . . . H4A H 0.4344 0.5275 0.5116 0.036 Uiso 1 1 calc R . . H4B H 0.3954 0.4775 0.4085 0.036 Uiso 1 1 calc R . . N5 N 0.44304(10) 0.55330(7) 0.31170(15) 0.0283(3) Uani 1 1 d . . . H5 H 0.4989 0.5424 0.3136 0.034 Uiso 1 1 calc R . . C6 C 0.40748(16) 0.53762(10) 0.17521(19) 0.0397(5) Uani 1 1 d . . . H6A H 0.3462 0.5403 0.1769 0.048 Uiso 1 1 calc R . . H6B H 0.4231 0.4949 0.1497 0.048 Uiso 1 1 calc R . . C7 C 0.44169(16) 0.58332(10) 0.0727(2) 0.0390(5) Uani 1 1 d . . . H7A H 0.5022 0.5773 0.0631 0.047 Uiso 1 1 calc R . . H7B H 0.4148 0.5770 -0.0173 0.047 Uiso 1 1 calc R . . N8 N 0.42414(11) 0.64680(7) 0.12347(15) 0.0303(3) Uani 1 1 d . . . H8 H 0.3705 0.6576 0.0967 0.036 Uiso 1 1 calc R . . C9 C 0.48308(13) 0.69511(10) 0.07139(18) 0.0333(4) Uani 1 1 d . . . H9A H 0.4613 0.7369 0.0915 0.040 Uiso 1 1 calc R . . H9B H 0.4883 0.6911 -0.0285 0.040 Uiso 1 1 calc R . . C10 C 0.56695(13) 0.68685(10) 0.13878(18) 0.0328(4) Uani 1 1 d . . . H10A H 0.5962 0.6513 0.0979 0.039 Uiso 1 1 calc R . . H10B H 0.6011 0.7244 0.1255 0.039 Uiso 1 1 calc R . . N11 N 0.55470(10) 0.67584(7) 0.28595(14) 0.0251(3) Uani 1 1 d . . . C12 C 0.26996(11) 0.65311(9) 0.49297(19) 0.0274(4) Uani 1 1 d . . . H12 H 0.2336 0.6335 0.5548 0.033 Uiso 1 1 calc R . . C13 C 0.26316(11) 0.71955(9) 0.47869(18) 0.0267(4) Uani 1 1 d . . . C14 C 0.31401(11) 0.75427(8) 0.38939(17) 0.0251(4) Uani 1 1 d . . . C15 C 0.29384(12) 0.81754(9) 0.36959(19) 0.0296(4) Uani 1 1 d . . . H15 H 0.3252 0.8417 0.3080 0.035 Uiso 1 1 calc R . . C16 C 0.22876(13) 0.84457(9) 0.4391(2) 0.0336(4) Uani 1 1 d . . . H16 H 0.2167 0.8870 0.4233 0.040 Uiso 1 1 calc R . . C17 C 0.17996(12) 0.81158(10) 0.5324(2) 0.0323(4) Uani 1 1 d . . . C18 C 0.19841(12) 0.74938(10) 0.54940(19) 0.0312(4) Uani 1 1 d . . . H18 H 0.1663 0.7258 0.6110 0.037 Uiso 1 1 calc R . . O19 O 0.37799(8) 0.73024(6) 0.32497(13) 0.0275(3) Uani 1 1 d . . . C20 C 0.62114(12) 0.67348(8) 0.36041(17) 0.0261(4) Uani 1 1 d . . . H20 H 0.6724 0.6809 0.3166 0.031 Uiso 1 1 calc R . . C21 C 0.62430(11) 0.66051(8) 0.50501(17) 0.0234(3) Uani 1 1 d . . . C22 C 0.55171(11) 0.64882(8) 0.58062(16) 0.0217(3) Uani 1 1 d . . . C23 C 0.56216(11) 0.63600(9) 0.72091(17) 0.0262(4) Uani 1 1 d . . . H23 H 0.5148 0.6276 0.7744 0.031 Uiso 1 1 calc R . . C24 C 0.64023(12) 0.63551(9) 0.78174(18) 0.0291(4) Uani 1 1 d . . . H24 H 0.6449 0.6261 0.8759 0.035 Uiso 1 1 calc R . . C25 C 0.71302(12) 0.64843(8) 0.70887(19) 0.0273(4) Uani 1 1 d . . . C26 C 0.70313(11) 0.66003(8) 0.57062(18) 0.0267(4) Uani 1 1 d . . . H26 H 0.7510 0.6680 0.5180 0.032 Uiso 1 1 calc R . . O27 O 0.47599(8) 0.64946(6) 0.52737(12) 0.0244(3) Uani 1 1 d . . . C28 C 0.10789(13) 0.84366(11) 0.6062(2) 0.0397(5) Uani 1 1 d . . . C29 C 0.04120(16) 0.86151(15) 0.5002(3) 0.0595(7) Uani 1 1 d . . . H29A H 0.0205 0.8242 0.4547 0.089 Uiso 1 1 calc R . . H29B H 0.0653 0.8894 0.4328 0.089 Uiso 1 1 calc R . . H29C H -0.0048 0.8824 0.5457 0.089 Uiso 1 1 calc R . . C30 C 0.06937(17) 0.80195(14) 0.7144(3) 0.0608(7) Uani 1 1 d . . . H30A H 0.0273 0.8252 0.7641 0.091 Uiso 1 1 calc R . . H30B H 0.1127 0.7879 0.7781 0.091 Uiso 1 1 calc R . . H30C H 0.0435 0.7660 0.6704 0.091 Uiso 1 1 calc R . . C31 C 0.14044(17) 0.90256(14) 0.6779(3) 0.0607(7) Uani 1 1 d . . . H31A H 0.0955 0.9216 0.7294 0.091 Uiso 1 1 calc R . . H31B H 0.1605 0.9319 0.6097 0.091 Uiso 1 1 calc R . . H31C H 0.1861 0.8916 0.7402 0.091 Uiso 1 1 calc R . . C32 C 0.79859(12) 0.64702(9) 0.7813(2) 0.0324(4) Uani 1 1 d . . . C33 C 0.82090(16) 0.57985(12) 0.8161(3) 0.0525(6) Uani 1 1 d . . . H33A H 0.8234 0.5555 0.7322 0.079 Uiso 1 1 calc R . . H33B H 0.7786 0.5625 0.8758 0.079 Uiso 1 1 calc R . . H33C H 0.8750 0.5787 0.8626 0.079 Uiso 1 1 calc R . . C34 C 0.86724(15) 0.67395(15) 0.6925(3) 0.0573(7) Uani 1 1 d . . . H34A H 0.9201 0.6730 0.7428 0.086 Uiso 1 1 calc R . . H34B H 0.8535 0.7168 0.6686 0.086 Uiso 1 1 calc R . . H34C H 0.8720 0.6493 0.6092 0.086 Uiso 1 1 calc R . . C35 C 0.79532(16) 0.68514(14) 0.9133(3) 0.0593(7) Uani 1 1 d . . . H35A H 0.8499 0.6846 0.9582 0.089 Uiso 1 1 calc R . . H35B H 0.7540 0.6672 0.9741 0.089 Uiso 1 1 calc R . . H35C H 0.7799 0.7279 0.8916 0.089 Uiso 1 1 calc R . . N36A N 0.6650(5) 0.5148(4) 0.1832(8) 0.061(2) Uani 0.70 1 d PD A 1 O37A O 0.62818(16) 0.53557(13) 0.2843(2) 0.0511(6) Uani 0.70 1 d PD A 1 O38A O 0.6582(3) 0.5416(2) 0.0720(3) 0.0548(10) Uani 0.70 1 d PD A 1 O39A O 0.7180(2) 0.47383(19) 0.2023(5) 0.0592(10) Uani 0.70 1 d PD A 1 N36B N 0.6641(5) 0.5156(4) 0.1817(9) 0.0087(18) Uiso 0.30 1 d PD B 2 O37B O 0.5993(5) 0.4967(4) 0.2444(8) 0.074(2) Uiso 0.30 1 d PD B 2 O38B O 0.6506(10) 0.5550(7) 0.0889(14) 0.104(7) Uiso 0.30 1 d PD B 2 O39B O 0.7222(8) 0.4805(8) 0.1687(17) 0.122(8) Uiso 0.30 1 d PD B 2 C40 C 0.9074(3) 0.5026(2) 0.2942(5) 0.1133(16) Uani 1 1 d . . . H40A H 0.9607 0.5192 0.2611 0.136 Uiso 1 1 calc R . . H40B H 0.8724 0.4916 0.2144 0.136 Uiso 1 1 calc R . . C41 C 0.8666(2) 0.5477(2) 0.3746(4) 0.0934(13) Uani 1 1 d . . . H41A H 0.9006 0.5574 0.4564 0.112 Uiso 1 1 calc R . . H41B H 0.8123 0.5317 0.4046 0.112 Uiso 1 1 calc R . . Cl42 Cl 0.92608(6) 0.43464(6) 0.39875(14) 0.1083(4) Uani 1 1 d . . . Cl43 Cl 0.85155(6) 0.61793(5) 0.27050(10) 0.0894(3) Uani 1 1 d . . . 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 0.02174(13) 0.02038(13) 0.02028(12) 0.00220(9) -0.00307(9) 0.00068(9) N2 0.0232(7) 0.0218(7) 0.0295(7) 0.0036(6) -0.0072(6) -0.0022(6) C3 0.0338(10) 0.0223(9) 0.0360(9) 0.0062(7) -0.0038(8) -0.0047(7) C4 0.0398(11) 0.0204(9) 0.0290(8) 0.0057(7) 0.0005(8) 0.0021(8) N5 0.0370(9) 0.0226(8) 0.0253(7) 0.0033(6) -0.0001(6) 0.0023(6) C6 0.0655(15) 0.0257(10) 0.0278(9) -0.0036(8) -0.0020(9) -0.0096(10) C7 0.0606(14) 0.0300(10) 0.0262(9) -0.0022(8) -0.0023(9) -0.0035(10) N8 0.0413(9) 0.0240(8) 0.0254(7) 0.0005(6) -0.0110(7) 0.0012(7) C9 0.0439(11) 0.0322(10) 0.0237(8) 0.0074(7) -0.0032(8) -0.0010(9) C10 0.0447(11) 0.0322(10) 0.0214(8) 0.0060(7) 0.0005(8) -0.0056(9) N11 0.0344(8) 0.0217(7) 0.0192(6) 0.0039(6) 0.0012(6) 0.0006(6) C12 0.0230(8) 0.0293(9) 0.0298(8) 0.0040(7) -0.0047(7) -0.0038(7) C13 0.0234(8) 0.0280(9) 0.0286(8) -0.0007(7) -0.0072(7) 0.0003(7) C14 0.0250(9) 0.0242(9) 0.0258(8) -0.0013(7) -0.0092(7) -0.0006(7) C15 0.0325(10) 0.0250(9) 0.0309(9) 0.0004(7) -0.0088(7) 0.0006(8) C16 0.0356(10) 0.0270(9) 0.0378(10) -0.0041(8) -0.0128(8) 0.0064(8) C17 0.0267(9) 0.0360(11) 0.0339(9) -0.0068(8) -0.0102(8) 0.0047(8) C18 0.0247(9) 0.0355(10) 0.0331(9) -0.0018(8) -0.0051(7) 0.0003(8) O19 0.0295(7) 0.0219(6) 0.0310(6) 0.0032(5) -0.0008(5) 0.0008(5) C20 0.0291(9) 0.0248(8) 0.0244(8) 0.0023(7) 0.0036(7) -0.0029(7) C21 0.0263(8) 0.0210(8) 0.0228(8) 0.0016(6) -0.0004(7) 0.0010(7) C22 0.0264(8) 0.0169(8) 0.0218(7) -0.0011(6) -0.0013(6) 0.0001(6) C23 0.0287(9) 0.0292(9) 0.0207(8) -0.0007(7) 0.0014(7) -0.0023(7) C24 0.0355(10) 0.0315(10) 0.0200(7) 0.0008(7) -0.0041(7) 0.0003(8) C25 0.0281(9) 0.0241(9) 0.0295(8) -0.0023(7) -0.0055(7) 0.0004(7) C26 0.0244(9) 0.0265(9) 0.0292(8) 0.0002(7) 0.0004(7) -0.0007(7) O27 0.0236(6) 0.0288(6) 0.0207(5) 0.0005(5) -0.0016(5) -0.0003(5) C28 0.0316(10) 0.0459(12) 0.0414(11) -0.0088(9) -0.0080(9) 0.0120(9) C29 0.0358(12) 0.090(2) 0.0521(14) -0.0088(14) -0.0121(11) 0.0258(13) C30 0.0514(15) 0.0720(19) 0.0593(15) 0.0003(14) 0.0135(12) 0.0200(14) C31 0.0539(16) 0.0628(17) 0.0652(16) -0.0287(14) -0.0079(13) 0.0153(13) C32 0.0295(10) 0.0344(10) 0.0330(9) -0.0016(8) -0.0089(8) 0.0007(8) C33 0.0434(13) 0.0417(13) 0.0718(17) 0.0034(12) -0.0223(12) 0.0065(10) C34 0.0331(12) 0.0821(19) 0.0563(14) 0.0142(14) -0.0133(11) -0.0144(12) C35 0.0458(14) 0.0735(19) 0.0579(15) -0.0316(14) -0.0241(12) 0.0130(13) N36A 0.063(3) 0.058(3) 0.062(3) -0.0090(17) -0.0128(17) 0.0112(17) O37A 0.0548(15) 0.0620(16) 0.0368(11) 0.0005(11) 0.0114(11) 0.0195(13) O38A 0.083(3) 0.0540(19) 0.0274(12) 0.0109(14) -0.0062(12) -0.0060(17) O39A 0.069(2) 0.0498(18) 0.0586(19) -0.0076(15) -0.0011(15) 0.0373(15) C40 0.076(3) 0.145(4) 0.120(3) -0.030(3) 0.031(2) -0.027(3) C41 0.085(3) 0.125(3) 0.071(2) -0.023(2) 0.0203(19) -0.043(2) Cl42 0.0693(6) 0.1005(8) 0.1552(10) 0.0120(7) 0.0009(6) -0.0250(5) Cl43 0.0682(5) 0.1107(7) 0.0901(6) 0.0126(5) 0.0307(5) -0.0055(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O19 1.9163(13) . ? Fe1 O27 1.9234(12) . ? Fe1 N11 2.1161(16) . ? Fe1 N2 2.1183(15) . ? Fe1 N5 2.1657(15) . ? Fe1 N8 2.1748(15) . ? N2 C12 1.289(2) . ? N2 C3 1.479(2) . ? C3 C4 1.526(3) . ? C4 N5 1.491(2) . ? N5 C6 1.491(2) . ? C6 C7 1.520(3) . ? C7 N8 1.489(3) . ? N8 C9 1.506(3) . ? C9 C10 1.509(3) . ? C10 N11 1.482(2) . ? N11 C20 1.290(2) . ? C12 C13 1.448(3) . ? C13 C18 1.417(3) . ? C13 C14 1.423(3) . ? C14 O19 1.323(2) . ? C14 C15 1.419(3) . ? C15 C16 1.388(3) . ? C16 C17 1.409(3) . ? C17 C18 1.387(3) . ? C17 C28 1.542(3) . ? C20 C21 1.449(2) . ? C21 C22 1.417(2) . ? C21 C26 1.418(3) . ? C22 O27 1.322(2) . ? C22 C23 1.415(2) . ? C23 C24 1.386(3) . ? C24 C25 1.410(3) . ? C25 C26 1.389(3) . ? C25 C32 1.544(3) . ? C28 C30 1.533(4) . ? C28 C29 1.536(3) . ? C28 C31 1.545(3) . ? C32 C34 1.533(3) . ? C32 C33 1.534(3) . ? C32 C35 1.539(3) . ? N36A O38A 1.241(7) . ? N36A O39A 1.244(8) . ? N36A O37A 1.248(8) . ? N36B O39B 1.214(12) . ? N36B O38B 1.265(12) . ? N36B O37B 1.285(10) . ? C40 C41 1.421(6) . ? C40 Cl42 1.816(6) . ? C41 Cl43 1.846(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 O19 Fe1 O27 106.18(5) . . ? O19 Fe1 N11 100.81(6) . . ? O27 Fe1 N11 86.23(5) . . ? O19 Fe1 N2 87.07(6) . . ? O27 Fe1 N2 85.48(5) . . ? N11 Fe1 N2 169.90(6) . . ? O19 Fe1 N5 153.05(6) . . ? O27 Fe1 N5 94.70(6) . . ? N11 Fe1 N5 97.33(6) . . ? N2 Fe1 N5 77.62(6) . . ? O19 Fe1 N8 85.65(6) . . ? O27 Fe1 N8 161.89(6) . . ? N11 Fe1 N8 77.97(6) . . ? N2 Fe1 N8 109.21(6) . . ? N5 Fe1 N8 78.80(6) . . ? C12 N2 C3 118.26(16) . . ? C12 N2 Fe1 123.10(12) . . ? C3 N2 Fe1 116.47(12) . . ? N2 C3 C4 108.68(15) . . ? N5 C4 C3 109.65(15) . . ? C4 N5 C6 114.18(16) . . ? C4 N5 Fe1 107.13(11) . . ? C6 N5 Fe1 109.13(12) . . ? N5 C6 C7 108.05(16) . . ? N8 C7 C6 107.79(16) . . ? C7 N8 C9 113.73(16) . . ? C7 N8 Fe1 111.84(11) . . ? C9 N8 Fe1 105.65(11) . . ? N8 C9 C10 109.53(15) . . ? N11 C10 C9 108.54(16) . . ? C20 N11 C10 116.12(16) . . ? C20 N11 Fe1 127.12(12) . . ? C10 N11 Fe1 116.01(12) . . ? N2 C12 C13 125.34(17) . . ? C18 C13 C14 119.74(17) . . ? C18 C13 C12 117.37(17) . . ? C14 C13 C12 122.70(17) . . ? O19 C14 C15 119.44(16) . . ? O19 C14 C13 123.12(16) . . ? C15 C14 C13 117.44(17) . . ? C16 C15 C14 120.77(18) . . ? C15 C16 C17 122.58(18) . . ? C18 C17 C16 116.67(18) . . ? C18 C17 C28 122.75(19) . . ? C16 C17 C28 120.54(18) . . ? C17 C18 C13 122.71(19) . . ? C14 O19 Fe1 131.37(11) . . ? N11 C20 C21 125.64(16) . . ? C22 C21 C26 120.09(15) . . ? C22 C21 C20 122.01(16) . . ? C26 C21 C20 117.89(16) . . ? O27 C22 C23 119.07(15) . . ? O27 C22 C21 123.70(15) . . ? C23 C22 C21 117.23(16) . . ? C24 C23 C22 121.20(16) . . ? C23 C24 C25 122.40(16) . . ? C26 C25 C24 116.53(17) . . ? C26 C25 C32 123.04(17) . . ? C24 C25 C32 120.39(16) . . ? C25 C26 C21 122.51(17) . . ? C22 O27 Fe1 133.80(11) . . ? C30 C28 C29 109.4(2) . . ? C30 C28 C17 112.09(19) . . ? C29 C28 C17 108.60(18) . . ? C30 C28 C31 107.8(2) . . ? C29 C28 C31 109.4(2) . . ? C17 C28 C31 109.41(19) . . ? C34 C32 C33 108.6(2) . . ? C34 C32 C35 108.0(2) . . ? C33 C32 C35 109.2(2) . . ? C34 C32 C25 112.14(17) . . ? C33 C32 C25 109.10(17) . . ? C35 C32 C25 109.76(17) . . ? O38A N36A O39A 121.3(7) . . ? O38A N36A O37A 119.8(7) . . ? O39A N36A O37A 117.9(7) . . ? O39B N36B O38B 118.1(9) . . ? O39B N36B O37B 119.0(10) . . ? O38B N36B O37B 115.3(9) . . ? C41 C40 Cl42 108.4(3) . . ? C40 C41 Cl43 108.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5 O37A 0.93 2.11 3.024(3) 166.1 . N5 H5 O37B 0.93 2.02 2.886(8) 153.5 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.650 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.057 #=END data_rpfe6im _database_code_depnum_ccdc_archive 'CCDC 676632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(2-hydroxy-1-naphthaldiminato)-3,6-diazaoctane]iron(III) hexafluorophosphate diethylether solvate ; _chemical_name_common ; (1,8-Bis(2-hydroxy-1-naphthaldiminato)-3,6- diazaoctane)iron(iii) hexafluorophosphate diethylether solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 Fe N4 O2, P F6, C4 H10 O' _chemical_formula_sum 'C32 H38 F6 Fe N4 O3 P' _chemical_formula_weight 727.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1874(12) _cell_length_b 15.7976(13) _cell_length_c 29.091(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6520.2(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 128364 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.22 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 1.015 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 128364 _diffrn_reflns_av_R_equivalents 0.1148 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.22 _reflns_number_total 7972 _reflns_number_gt 5133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. No disorder was detected during refinement, and no restraints were applied. All non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0550P)^2^+8.7741P] 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 7972 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91767(3) 0.01365(3) 0.371749(15) 0.01824(12) Uani 1 1 d . . . N2 N 0.98137(17) 0.09772(17) 0.40951(9) 0.0198(6) Uani 1 1 d . . . C3 C 1.0478(2) 0.1523(2) 0.38380(11) 0.0247(7) Uani 1 1 d . . . H3A H 1.1100 0.1244 0.3810 0.030 Uiso 1 1 calc R . . H3B H 1.0563 0.2072 0.3997 0.030 Uiso 1 1 calc R . . C4 C 1.0038(2) 0.1658(2) 0.33624(12) 0.0257(7) Uani 1 1 d . . . H4A H 0.9522 0.2078 0.3384 0.031 Uiso 1 1 calc R . . H4B H 1.0520 0.1879 0.3147 0.031 Uiso 1 1 calc R . . N5 N 0.96560(18) 0.08268(16) 0.31847(9) 0.0217(6) Uani 1 1 d . . . H5 H 0.9141 0.0952 0.2999 0.026 Uiso 1 1 calc R . . C6 C 1.0335(2) 0.0318(2) 0.28995(12) 0.0260(7) Uani 1 1 d . . . H6A H 1.0750 0.0703 0.2722 0.031 Uiso 1 1 calc R . . H6B H 0.9984 -0.0041 0.2679 0.031 Uiso 1 1 calc R . . C7 C 1.0928(2) -0.0237(2) 0.32175(12) 0.0266(7) Uani 1 1 d . . . H7A H 1.1217 -0.0703 0.3039 0.032 Uiso 1 1 calc R . . H7B H 1.1442 0.0104 0.3354 0.032 Uiso 1 1 calc R . . N8 N 1.03223(18) -0.05988(17) 0.35934(9) 0.0220(6) Uani 1 1 d . . . H8 H 1.0681 -0.0619 0.3861 0.026 Uiso 1 1 calc R . . C9 C 0.9959(2) -0.1472(2) 0.34994(12) 0.0243(7) Uani 1 1 d . . . H9A H 0.9764 -0.1745 0.3791 0.029 Uiso 1 1 calc R . . H9B H 1.0460 -0.1821 0.3358 0.029 Uiso 1 1 calc R . . C10 C 0.9116(2) -0.1408(2) 0.31742(11) 0.0220(7) Uani 1 1 d . . . H10A H 0.9330 -0.1290 0.2857 0.026 Uiso 1 1 calc R . . H10B H 0.8753 -0.1943 0.3174 0.026 Uiso 1 1 calc R . . N11 N 0.85250(17) -0.06968(16) 0.33502(9) 0.0196(6) Uani 1 1 d . . . C12 C 0.9597(2) 0.1153(2) 0.45164(11) 0.0212(7) Uani 1 1 d . . . H12 H 0.9880 0.1637 0.4653 0.025 Uiso 1 1 calc R . . C13 C 0.8948(2) 0.0657(2) 0.47942(11) 0.0203(7) Uani 1 1 d . . . C14 C 0.8689(2) -0.0169(2) 0.46542(11) 0.0224(7) Uani 1 1 d . . . C15 C 0.8162(2) -0.0694(2) 0.49701(11) 0.0270(7) Uani 1 1 d . . . H15 H 0.8053 -0.1272 0.4897 0.032 Uiso 1 1 calc R . . C16 C 0.7816(2) -0.0373(2) 0.53726(12) 0.0291(8) Uani 1 1 d . . . H16 H 0.7458 -0.0730 0.5569 0.035 Uiso 1 1 calc R . . C17 C 0.7980(2) 0.0488(2) 0.55055(12) 0.0268(7) Uani 1 1 d . . . C18 C 0.8587(2) 0.1003(2) 0.52265(11) 0.0229(7) Uani 1 1 d . . . O19 O 0.89014(15) -0.05115(14) 0.42538(8) 0.0230(5) Uani 1 1 d . . . C20 C 0.7611(2) -0.07287(19) 0.32707(11) 0.0196(6) Uani 1 1 d . . . H20 H 0.7377 -0.1206 0.3108 0.024 Uiso 1 1 calc R . . C21 C 0.6938(2) -0.0097(2) 0.34112(11) 0.0197(6) Uani 1 1 d . . . C22 C 0.7230(2) 0.0666(2) 0.36249(11) 0.0203(7) Uani 1 1 d . . . C23 C 0.6547(2) 0.1324(2) 0.37059(12) 0.0255(7) Uani 1 1 d . . . H23 H 0.6746 0.1848 0.3834 0.031 Uiso 1 1 calc R . . C24 C 0.5617(2) 0.1207(2) 0.36005(12) 0.0268(8) Uani 1 1 d . . . H24 H 0.5183 0.1655 0.3656 0.032 Uiso 1 1 calc R . . C25 C 0.5277(2) 0.0427(2) 0.34088(11) 0.0224(7) Uani 1 1 d . . . C26 C 0.5934(2) -0.0240(2) 0.33119(11) 0.0200(6) Uani 1 1 d . . . O27 O 0.81035(14) 0.08450(14) 0.37519(8) 0.0217(5) Uani 1 1 d . . . C28 C 0.7541(2) 0.0842(3) 0.59039(12) 0.0320(8) Uani 1 1 d . . . H28 H 0.7133 0.0498 0.6083 0.038 Uiso 1 1 calc R . . C29 C 0.7695(2) 0.1668(3) 0.60338(12) 0.0327(8) Uani 1 1 d . . . H29 H 0.7388 0.1898 0.6296 0.039 Uiso 1 1 calc R . . C30 C 0.8319(2) 0.2169(2) 0.57704(12) 0.0320(8) Uani 1 1 d . . . H30 H 0.8448 0.2732 0.5865 0.038 Uiso 1 1 calc R . . C31 C 0.8748(2) 0.1855(2) 0.53766(12) 0.0262(7) Uani 1 1 d . . . H31 H 0.9155 0.2211 0.5204 0.031 Uiso 1 1 calc R . . C32 C 0.4298(2) 0.0310(2) 0.33130(12) 0.0255(7) Uani 1 1 d . . . H32 H 0.3868 0.0758 0.3372 0.031 Uiso 1 1 calc R . . C33 C 0.3970(2) -0.0440(2) 0.31372(12) 0.0269(8) Uani 1 1 d . . . H33 H 0.3319 -0.0507 0.3070 0.032 Uiso 1 1 calc R . . C34 C 0.4607(2) -0.1117(2) 0.30552(11) 0.0239(7) Uani 1 1 d . . . H34 H 0.4378 -0.1644 0.2945 0.029 Uiso 1 1 calc R . . C35 C 0.5568(2) -0.1009(2) 0.31355(11) 0.0227(7) Uani 1 1 d . . . H35 H 0.5988 -0.1462 0.3070 0.027 Uiso 1 1 calc R . . P36 P 0.77597(6) 0.20397(6) 0.23819(3) 0.0246(2) Uani 1 1 d . . . F37 F 0.88695(15) 0.20933(16) 0.22717(9) 0.0495(6) Uani 1 1 d . . . F38 F 0.79709(14) 0.22785(13) 0.29137(7) 0.0333(5) Uani 1 1 d . . . F39 F 0.78753(16) 0.10517(13) 0.25053(8) 0.0382(5) Uani 1 1 d . . . F40 F 0.66508(14) 0.19968(15) 0.24964(8) 0.0404(5) Uani 1 1 d . . . F41 F 0.75401(17) 0.17969(15) 0.18530(7) 0.0451(6) Uani 1 1 d . . . F42 F 0.76496(18) 0.30374(14) 0.22631(8) 0.0450(6) Uani 1 1 d . . . C43 C 0.8410(3) 0.3133(3) 0.42325(14) 0.0415(10) Uani 1 1 d . . . H43A H 0.8723 0.2835 0.3979 0.062 Uiso 1 1 calc R . . H43B H 0.7871 0.3452 0.4113 0.062 Uiso 1 1 calc R . . H43C H 0.8189 0.2720 0.4460 0.062 Uiso 1 1 calc R . . C44 C 0.9100(3) 0.3738(3) 0.44576(15) 0.0432(10) Uani 1 1 d . . . H44A H 0.9338 0.4146 0.4227 0.052 Uiso 1 1 calc R . . H44B H 0.8779 0.4059 0.4705 0.052 Uiso 1 1 calc R . . O45 O 0.98714(18) 0.32613(16) 0.46468(9) 0.0360(6) Uani 1 1 d . . . C46 C 1.0514(3) 0.3777(3) 0.49038(16) 0.0429(10) Uani 1 1 d . . . H46A H 1.0178 0.4060 0.5160 0.051 Uiso 1 1 calc R . . H46B H 1.0788 0.4219 0.4703 0.051 Uiso 1 1 calc R . . C47 C 1.1288(3) 0.3214(3) 0.50920(15) 0.0450(10) Uani 1 1 d . . . H47A H 1.1011 0.2784 0.5294 0.068 Uiso 1 1 calc R . . H47B H 1.1738 0.3558 0.5266 0.068 Uiso 1 1 calc R . . H47C H 1.1615 0.2935 0.4837 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0119(2) 0.0182(2) 0.0247(2) -0.00069(19) -0.00044(18) 0.00004(17) N2 0.0116(12) 0.0194(14) 0.0285(15) 0.0000(11) -0.0014(11) -0.0009(10) C3 0.0180(16) 0.0246(18) 0.0316(18) -0.0022(14) 0.0061(13) -0.0056(13) C4 0.0256(17) 0.0192(17) 0.0323(19) 0.0016(14) 0.0067(14) -0.0022(13) N5 0.0176(13) 0.0178(14) 0.0297(15) 0.0012(11) 0.0003(11) 0.0022(11) C6 0.0281(18) 0.0224(18) 0.0275(18) -0.0025(14) 0.0070(14) -0.0003(14) C7 0.0145(16) 0.0263(18) 0.039(2) -0.0013(15) 0.0076(14) 0.0000(13) N8 0.0145(13) 0.0215(15) 0.0299(15) -0.0034(11) -0.0004(11) -0.0011(11) C9 0.0181(16) 0.0199(17) 0.0348(19) -0.0008(14) -0.0001(14) 0.0043(13) C10 0.0164(15) 0.0179(16) 0.0318(18) -0.0055(13) 0.0004(14) 0.0020(12) N11 0.0155(13) 0.0162(13) 0.0272(14) -0.0004(11) 0.0013(11) 0.0023(10) C12 0.0129(15) 0.0212(17) 0.0295(18) -0.0018(14) -0.0031(13) -0.0017(12) C13 0.0141(15) 0.0224(17) 0.0245(16) -0.0003(13) -0.0029(12) 0.0008(12) C14 0.0162(15) 0.0272(17) 0.0238(16) 0.0031(14) -0.0020(12) 0.0019(13) C15 0.0258(18) 0.0250(18) 0.0301(18) 0.0071(14) -0.0011(14) -0.0041(14) C16 0.0234(18) 0.036(2) 0.0279(18) 0.0071(15) 0.0011(14) -0.0073(15) C17 0.0170(16) 0.038(2) 0.0259(17) 0.0036(15) -0.0012(13) 0.0004(14) C18 0.0136(15) 0.0300(19) 0.0250(17) -0.0017(14) -0.0026(12) 0.0014(13) O19 0.0189(11) 0.0212(12) 0.0290(12) 0.0006(10) 0.0012(9) -0.0017(9) C20 0.0152(15) 0.0186(15) 0.0250(16) -0.0006(13) -0.0033(12) -0.0025(12) C21 0.0137(14) 0.0191(16) 0.0264(16) 0.0021(13) -0.0007(12) 0.0006(12) C22 0.0137(15) 0.0207(16) 0.0263(17) 0.0036(13) 0.0008(12) -0.0003(12) C23 0.0207(16) 0.0211(17) 0.0346(19) -0.0038(14) 0.0008(15) -0.0003(13) C24 0.0168(16) 0.0234(18) 0.040(2) -0.0004(15) 0.0038(14) 0.0057(13) C25 0.0148(15) 0.0223(16) 0.0302(18) 0.0033(14) 0.0003(13) -0.0003(12) C26 0.0178(15) 0.0189(16) 0.0232(16) 0.0042(13) -0.0005(12) -0.0004(12) O27 0.0122(10) 0.0200(11) 0.0328(13) -0.0015(10) -0.0016(9) -0.0016(8) C28 0.0210(17) 0.049(2) 0.0261(18) 0.0005(17) 0.0015(14) 0.0011(16) C29 0.0215(18) 0.048(2) 0.0283(19) -0.0026(17) -0.0002(14) 0.0081(16) C30 0.0277(19) 0.038(2) 0.0300(19) -0.0079(16) -0.0060(15) 0.0073(16) C31 0.0210(17) 0.0299(19) 0.0276(18) -0.0015(15) -0.0017(14) 0.0042(14) C32 0.0136(16) 0.0283(19) 0.0347(19) 0.0028(14) 0.0014(13) 0.0036(13) C33 0.0155(16) 0.0341(19) 0.0312(19) 0.0064(15) -0.0003(13) -0.0019(13) C34 0.0200(17) 0.0210(17) 0.0305(18) 0.0042(14) -0.0028(13) -0.0046(13) C35 0.0177(15) 0.0202(16) 0.0301(18) 0.0026(14) -0.0018(13) 0.0000(12) P36 0.0188(4) 0.0224(4) 0.0326(5) 0.0016(4) -0.0005(4) 0.0023(3) F37 0.0230(11) 0.0553(16) 0.0703(17) 0.0013(13) 0.0138(11) -0.0016(10) F38 0.0302(11) 0.0335(12) 0.0363(12) -0.0013(9) -0.0081(9) -0.0020(9) F39 0.0434(13) 0.0229(11) 0.0483(13) 0.0011(10) 0.0011(10) 0.0021(9) F40 0.0172(10) 0.0505(14) 0.0534(14) -0.0139(11) -0.0019(9) 0.0015(10) F41 0.0500(14) 0.0521(15) 0.0332(12) -0.0045(11) -0.0049(10) 0.0147(12) F42 0.0592(16) 0.0262(12) 0.0496(14) 0.0079(10) 0.0003(12) 0.0060(11) C43 0.035(2) 0.045(2) 0.044(2) 0.0039(19) -0.0025(18) 0.0141(18) C44 0.039(2) 0.037(2) 0.054(3) 0.0083(19) 0.0029(19) 0.0104(18) O45 0.0286(14) 0.0308(14) 0.0485(16) 0.0029(12) 0.0006(12) 0.0030(11) C46 0.031(2) 0.039(2) 0.059(3) -0.005(2) 0.0079(19) -0.0062(17) C47 0.030(2) 0.057(3) 0.048(3) 0.002(2) 0.0033(18) -0.0072(19) _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 O27 1.892(2) . ? Fe1 O19 1.907(2) . ? Fe1 N11 1.931(3) . ? Fe1 N2 1.946(3) . ? Fe1 N5 2.013(3) . ? Fe1 N8 2.030(3) . ? N2 C12 1.294(4) . ? N2 C3 1.480(4) . ? C3 C4 1.533(5) . ? C4 N5 1.512(4) . ? N5 C6 1.504(4) . ? C6 C7 1.527(5) . ? C7 N8 1.504(4) . ? N8 C9 1.498(4) . ? C9 C10 1.528(4) . ? C10 N11 1.493(4) . ? N11 C20 1.319(4) . ? C12 C13 1.455(4) . ? C13 C14 1.415(5) . ? C13 C18 1.464(4) . ? C14 O19 1.319(4) . ? C14 C15 1.447(4) . ? C15 C16 1.367(5) . ? C16 C17 1.433(5) . ? C17 C28 1.429(5) . ? C17 C18 1.436(5) . ? C18 C31 1.434(5) . ? C20 C21 1.441(4) . ? C21 C22 1.418(4) . ? C21 C26 1.471(4) . ? C22 O27 1.323(4) . ? C22 C23 1.441(4) . ? C23 C24 1.368(5) . ? C24 C25 1.436(5) . ? C25 C32 1.428(4) . ? C25 C26 1.435(4) . ? C26 C35 1.417(4) . ? C28 C29 1.377(5) . ? C29 C30 1.413(5) . ? C30 C31 1.388(5) . ? C32 C33 1.372(5) . ? C33 C34 1.419(5) . ? C34 C35 1.394(4) . ? P36 F37 1.609(2) . ? P36 F40 1.609(2) . ? P36 F39 1.610(2) . ? P36 F41 1.616(2) . ? P36 F38 1.620(2) . ? P36 F42 1.621(2) . ? C43 C44 1.517(6) . ? C44 O45 1.438(4) . ? O45 C46 1.433(5) . ? C46 C47 1.516(6) . ? 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 O27 Fe1 O19 96.28(9) . . ? O27 Fe1 N11 92.71(10) . . ? O19 Fe1 N11 89.35(10) . . ? O27 Fe1 N2 86.57(10) . . ? O19 Fe1 N2 89.98(10) . . ? N11 Fe1 N2 178.96(11) . . ? O27 Fe1 N5 89.55(10) . . ? O19 Fe1 N5 171.88(10) . . ? N11 Fe1 N5 96.03(11) . . ? N2 Fe1 N5 84.72(11) . . ? O27 Fe1 N8 172.75(11) . . ? O19 Fe1 N8 90.14(10) . . ? N11 Fe1 N8 83.96(11) . . ? N2 Fe1 N8 96.84(11) . . ? N5 Fe1 N8 84.41(11) . . ? C12 N2 C3 120.3(3) . . ? C12 N2 Fe1 124.8(2) . . ? C3 N2 Fe1 114.1(2) . . ? N2 C3 C4 106.1(3) . . ? N5 C4 C3 109.5(3) . . ? C6 N5 C4 115.0(2) . . ? C6 N5 Fe1 110.59(19) . . ? C4 N5 Fe1 109.2(2) . . ? N5 C6 C7 109.0(3) . . ? N8 C7 C6 110.1(3) . . ? C9 N8 C7 114.5(3) . . ? C9 N8 Fe1 106.49(18) . . ? C7 N8 Fe1 111.7(2) . . ? N8 C9 C10 108.7(3) . . ? N11 C10 C9 106.1(2) . . ? C20 N11 C10 117.6(3) . . ? C20 N11 Fe1 126.5(2) . . ? C10 N11 Fe1 115.72(19) . . ? N2 C12 C13 124.1(3) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 C18 120.0(3) . . ? C12 C13 C18 119.8(3) . . ? O19 C14 C13 125.0(3) . . ? O19 C14 C15 116.3(3) . . ? C13 C14 C15 118.7(3) . . ? C16 C15 C14 121.1(3) . . ? C15 C16 C17 121.7(3) . . ? C28 C17 C16 121.3(3) . . ? C28 C17 C18 119.9(3) . . ? C16 C17 C18 118.8(3) . . ? C31 C18 C17 117.1(3) . . ? C31 C18 C13 123.8(3) . . ? C17 C18 C13 119.0(3) . . ? C14 O19 Fe1 123.3(2) . . ? N11 C20 C21 125.1(3) . . ? C22 C21 C20 121.3(3) . . ? C22 C21 C26 120.0(3) . . ? C20 C21 C26 118.6(3) . . ? O27 C22 C21 125.3(3) . . ? O27 C22 C23 115.5(3) . . ? C21 C22 C23 119.2(3) . . ? C24 C23 C22 121.0(3) . . ? C23 C24 C25 121.8(3) . . ? C32 C25 C26 119.9(3) . . ? C32 C25 C24 120.9(3) . . ? C26 C25 C24 119.2(3) . . ? C35 C26 C25 117.6(3) . . ? C35 C26 C21 123.9(3) . . ? C25 C26 C21 118.5(3) . . ? C22 O27 Fe1 127.7(2) . . ? C29 C28 C17 121.6(3) . . ? C28 C29 C30 118.8(3) . . ? C31 C30 C29 121.5(4) . . ? C30 C31 C18 121.1(3) . . ? C33 C32 C25 120.9(3) . . ? C32 C33 C34 119.8(3) . . ? C35 C34 C33 120.2(3) . . ? C34 C35 C26 121.6(3) . . ? F37 P36 F40 179.26(15) . . ? F37 P36 F39 89.75(13) . . ? F40 P36 F39 90.72(12) . . ? F37 P36 F41 90.65(13) . . ? F40 P36 F41 89.91(13) . . ? F39 P36 F41 90.10(12) . . ? F37 P36 F38 89.83(13) . . ? F40 P36 F38 89.61(12) . . ? F39 P36 F38 89.66(12) . . ? F41 P36 F38 179.46(14) . . ? F37 P36 F42 90.04(13) . . ? F40 P36 F42 89.48(13) . . ? F39 P36 F42 179.35(14) . . ? F41 P36 F42 90.52(13) . . ? F38 P36 F42 89.72(12) . . ? O45 C44 C43 109.1(3) . . ? C46 O45 C44 112.7(3) . . ? O45 C46 C47 108.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5 F39 0.93 2.30 3.227(3) 171.4 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.824 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.091 #=END data_rp9i _database_code_depnum_ccdc_archive 'CCDC 676633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(salicylaldiminato)-3,6-diazaoctane]iron(III) hexafluorophosphate ; _chemical_name_common ;(1,8-Bis(salicylaldiminato)-3,6-diazaoctane)iron(iii) hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, F6 P' _chemical_formula_sum 'C20 H24 F6 Fe N4 O2 P' _chemical_formula_weight 553.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6187(12) _cell_length_b 27.768(3) _cell_length_c 18.009(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.033(8) _cell_angle_gamma 90.00 _cell_volume 4803.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9553 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.50 _exptl_crystal_description Plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 1.041 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48793 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9553 _reflns_number_gt 4938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two independent complex cations and two anions, all lying on general positions. Both anions are disordered, and were modelled over three equally occupied sites with the refined restraints P---F = 1.61(2) and cis-F...F = 2.28(2)\%A. All wholly occupied non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. The amino group N8A---H8A does not form a hydrogen bond in the crystal, but donates a weak N---H...pi interaction to phenoxy ring C13B-C18B with H8A...X = 2.87\%A and N8A---H8A...X = 155.3\% (X = centroid of C13B-C18B). ; _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^)+(0.0683P)^2^+5.4675P] 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 9553 _refine_ls_number_parameters 656 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.55815(7) 0.99169(2) 0.24633(4) 0.0436(2) Uani 1 1 d . . . N2A N 0.4434(4) 0.92843(13) 0.2170(2) 0.0483(10) Uani 1 1 d . . . C3A C 0.3579(6) 0.9295(2) 0.1456(3) 0.0731(17) Uani 1 1 d . . . H3A1 H 0.2591 0.9261 0.1552 0.088 Uiso 1 1 calc R . . H3A2 H 0.3844 0.9027 0.1138 0.088 Uiso 1 1 calc R . . C4A C 0.3831(7) 0.9777(2) 0.1067(3) 0.0811(18) Uani 1 1 d . . . H4A1 H 0.4676 0.9757 0.0787 0.097 Uiso 1 1 calc R . . H4A2 H 0.3045 0.9850 0.0716 0.097 Uiso 1 1 calc R . . N5A N 0.3986(5) 1.01662(16) 0.1633(3) 0.0659(12) Uani 1 1 d . . . H5A H 0.4313 1.0438 0.1407 0.079 Uiso 1 1 calc R . . C6A C 0.2691(7) 1.0294(3) 0.1997(4) 0.095(2) Uani 1 1 d . . . H6A1 H 0.2157 1.0001 0.2092 0.113 Uiso 1 1 calc R . . H6A2 H 0.2115 1.0505 0.1671 0.113 Uiso 1 1 calc R . . C7A C 0.3069(7) 1.0548(2) 0.2722(4) 0.097(2) Uani 1 1 d . . . H7A1 H 0.3559 1.0849 0.2627 0.117 Uiso 1 1 calc R . . H7A2 H 0.2225 1.0624 0.2980 0.117 Uiso 1 1 calc R . . N8A N 0.3986(5) 1.02188(15) 0.3188(3) 0.0688(13) Uani 1 1 d . . . H8A H 0.3457 0.9971 0.3361 0.083 Uiso 1 1 calc R . . C9A C 0.4768(7) 1.0453(2) 0.3833(3) 0.085(2) Uani 1 1 d . . . H9A1 H 0.5210 1.0206 0.4155 0.102 Uiso 1 1 calc R . . H9A2 H 0.4125 1.0638 0.4126 0.102 Uiso 1 1 calc R . . C10A C 0.5887(8) 1.0790(2) 0.3537(3) 0.089(2) Uani 1 1 d . . . H10A H 0.5482 1.1108 0.3434 0.107 Uiso 1 1 calc R . . H10B H 0.6649 1.0828 0.3916 0.107 Uiso 1 1 calc R . . N11A N 0.6440(5) 1.05879(13) 0.2845(2) 0.0546(11) Uani 1 1 d . . . C12A C 0.4253(5) 0.89263(16) 0.2621(3) 0.0487(12) Uani 1 1 d . . . H12A H 0.3591 0.8693 0.2465 0.058 Uiso 1 1 calc R . . C13A C 0.4971(5) 0.88528(15) 0.3336(3) 0.0419(11) Uani 1 1 d . . . C14A C 0.6062(5) 0.91551(15) 0.3628(3) 0.0431(11) Uani 1 1 d . . . C15A C 0.6745(6) 0.90342(17) 0.4314(3) 0.0581(14) Uani 1 1 d . . . H15A H 0.7506 0.9220 0.4498 0.070 Uiso 1 1 calc R . . C16A C 0.6301(6) 0.86410(19) 0.4725(3) 0.0649(15) Uani 1 1 d . . . H16A H 0.6756 0.8570 0.5187 0.078 Uiso 1 1 calc R . . C17A C 0.5202(6) 0.83533(19) 0.4463(3) 0.0673(16) Uani 1 1 d . . . H17A H 0.4890 0.8097 0.4751 0.081 Uiso 1 1 calc R . . C18A C 0.4573(5) 0.84514(17) 0.3771(3) 0.0592(14) Uani 1 1 d . . . H18A H 0.3861 0.8247 0.3581 0.071 Uiso 1 1 calc R . . O19A O 0.6473(3) 0.95442(10) 0.32570(18) 0.0534(9) Uani 1 1 d . . . C20A C 0.7329(5) 1.08433(16) 0.2501(3) 0.0497(12) Uani 1 1 d . . . H20A H 0.7572 1.1143 0.2712 0.060 Uiso 1 1 calc R . . C21A C 0.7992(5) 1.07136(15) 0.1822(3) 0.0444(11) Uani 1 1 d . . . C22A C 0.7754(4) 1.02629(16) 0.1452(3) 0.0436(11) Uani 1 1 d . . . C23A C 0.8404(5) 1.01804(18) 0.0780(3) 0.0585(14) Uani 1 1 d . . . H23A H 0.8261 0.9885 0.0532 0.070 Uiso 1 1 calc R . . C24A C 0.9255(6) 1.0527(2) 0.0473(3) 0.0715(16) Uani 1 1 d . . . H24A H 0.9660 1.0468 0.0018 0.086 Uiso 1 1 calc R . . C25A C 0.9504(6) 1.09642(19) 0.0844(4) 0.0715(16) Uani 1 1 d . . . H25A H 1.0093 1.1196 0.0645 0.086 Uiso 1 1 calc R . . C26A C 0.8883(5) 1.10540(18) 0.1502(3) 0.0596(14) Uani 1 1 d . . . H26A H 0.9053 1.1349 0.1746 0.072 Uiso 1 1 calc R . . O27A O 0.6965(3) 0.99174(10) 0.17303(18) 0.0518(8) Uani 1 1 d . . . Fe1B Fe 0.04893(7) 0.81295(2) 0.29543(4) 0.0444(2) Uani 1 1 d . . . N2B N -0.0596(4) 0.87372(15) 0.2488(3) 0.0645(12) Uani 1 1 d . . . C3B C -0.1493(9) 0.8618(3) 0.1826(5) 0.126(3) Uani 1 1 d . . . H3B1 H -0.2299 0.8834 0.1804 0.151 Uiso 1 1 calc R . . H3B2 H -0.0973 0.8674 0.1381 0.151 Uiso 1 1 calc R . . C4B C -0.1951(11) 0.8159(3) 0.1819(6) 0.170(5) Uani 1 1 d . . . H4B1 H -0.1956 0.8045 0.1303 0.204 Uiso 1 1 calc R . . H4B2 H -0.2922 0.8164 0.1958 0.204 Uiso 1 1 calc R . . N5B N -0.1223(5) 0.77945(16) 0.2284(3) 0.0716(13) Uani 1 1 d . . . H5B H -0.0833 0.7578 0.1969 0.086 Uiso 1 1 calc R . . C6B C -0.2159(6) 0.7516(2) 0.2766(4) 0.090(2) Uani 1 1 d . . . H6B1 H -0.1786 0.7191 0.2846 0.108 Uiso 1 1 calc R . . H6B2 H -0.3086 0.7488 0.2517 0.108 Uiso 1 1 calc R . . C7B C -0.2271(6) 0.7766(2) 0.3508(4) 0.088(2) Uani 1 1 d . . . H7B1 H -0.2763 0.8073 0.3438 0.105 Uiso 1 1 calc R . . H7B2 H -0.2796 0.7564 0.3841 0.105 Uiso 1 1 calc R . . N8B N -0.0846(4) 0.78513(15) 0.3838(3) 0.0613(12) Uani 1 1 d . . . H8B H -0.0904 0.8088 0.4192 0.074 Uiso 1 1 calc R . . C9B C -0.0220(6) 0.74131(19) 0.4215(3) 0.0724(16) Uani 1 1 d . . . H9B1 H -0.0516 0.7393 0.4726 0.087 Uiso 1 1 calc R . . H9B2 H -0.0538 0.7122 0.3949 0.087 Uiso 1 1 calc R . . C10B C 0.1335(6) 0.74469(19) 0.4218(3) 0.0637(15) Uani 1 1 d . . . H10C H 0.1672 0.7702 0.4559 0.076 Uiso 1 1 calc R . . H10D H 0.1758 0.7141 0.4383 0.076 Uiso 1 1 calc R . . N11B N 0.1717(4) 0.75589(13) 0.3442(2) 0.0476(10) Uani 1 1 d . . . C12B C -0.0536(5) 0.91826(18) 0.2716(3) 0.0625(15) Uani 1 1 d . . . H12B H -0.1078 0.9410 0.2442 0.075 Uiso 1 1 calc R . . C13B C 0.0294(5) 0.93573(16) 0.3353(3) 0.0464(12) Uani 1 1 d . . . C14B C 0.1176(5) 0.90529(15) 0.3792(3) 0.0462(12) Uani 1 1 d . . . C15B C 0.1934(5) 0.92551(17) 0.4410(3) 0.0573(14) Uani 1 1 d . . . H15B H 0.2544 0.9059 0.4702 0.069 Uiso 1 1 calc R . . C16B C 0.1796(6) 0.97375(18) 0.4594(3) 0.0650(15) Uani 1 1 d . . . H16B H 0.2299 0.9862 0.5012 0.078 Uiso 1 1 calc R . . C17B C 0.0922(6) 1.00378(18) 0.4166(3) 0.0676(16) Uani 1 1 d . . . H17B H 0.0832 1.0364 0.4292 0.081 Uiso 1 1 calc R . . C18B C 0.0187(6) 0.98501(17) 0.3554(3) 0.0618(15) Uani 1 1 d . . . H18B H -0.0399 1.0054 0.3262 0.074 Uiso 1 1 calc R . . O19B O 0.1328(3) 0.85852(10) 0.36461(19) 0.0540(9) Uani 1 1 d . . . C20B C 0.2699(5) 0.73202(16) 0.3146(3) 0.0467(12) Uani 1 1 d . . . H20B H 0.3113 0.7069 0.3428 0.056 Uiso 1 1 calc R . . C21B C 0.3221(5) 0.74066(15) 0.2413(3) 0.0444(11) Uani 1 1 d . . . C22B C 0.2703(5) 0.77849(16) 0.1932(3) 0.0460(12) Uani 1 1 d . . . C23B C 0.3315(6) 0.78529(18) 0.1243(3) 0.0594(14) Uani 1 1 d . . . H23B H 0.2997 0.8104 0.0928 0.071 Uiso 1 1 calc R . . C24B C 0.4381(6) 0.7554(2) 0.1025(3) 0.0685(16) Uani 1 1 d . . . H24B H 0.4769 0.7605 0.0564 0.082 Uiso 1 1 calc R . . C25B C 0.4880(5) 0.7182(2) 0.1484(3) 0.0659(16) Uani 1 1 d . . . H25B H 0.5600 0.6981 0.1332 0.079 Uiso 1 1 calc R . . C26B C 0.4312(5) 0.71068(18) 0.2165(3) 0.0574(14) Uani 1 1 d . . . H26B H 0.4651 0.6854 0.2471 0.069 Uiso 1 1 calc R . . O27B O 0.1707(3) 0.80878(11) 0.21359(19) 0.0545(8) Uani 1 1 d . . . P29A P -0.0185(10) 0.6619(3) 0.1206(5) 0.053(4) Uiso 0.34 1 d PD A 1 F30A F -0.1706(8) 0.6564(4) 0.1447(5) 0.056(3) Uiso 0.34 1 d PD A 1 F31A F -0.0453(14) 0.7156(3) 0.0880(5) 0.056(3) Uiso 0.34 1 d PD A 1 F32A F 0.1472(10) 0.6658(5) 0.0881(7) 0.065(4) Uiso 0.34 1 d PD A 1 F33A F 0.0168(12) 0.6078(3) 0.1526(6) 0.059(3) Uiso 0.34 1 d PD A 1 F34A F -0.0613(14) 0.6369(5) 0.0402(6) 0.080(5) Uiso 0.34 1 d PD A 1 F35A F 0.0507(11) 0.6834(3) 0.1931(5) 0.045(3) Uiso 0.34 1 d PD A 1 P29B P -0.0207(12) 0.6612(4) 0.1106(7) 0.079(6) Uiso 0.33 1 d PD B 2 F30B F 0.0598(10) 0.6106(3) 0.1234(6) 0.064(3) Uiso 0.33 1 d PD B 2 F31B F -0.1120(12) 0.7096(4) 0.0936(6) 0.082(4) Uiso 0.33 1 d PD B 2 F32B F -0.1633(11) 0.6359(5) 0.1319(7) 0.103(5) Uiso 0.33 1 d PD B 2 F33B F 0.1198(13) 0.6858(5) 0.0854(9) 0.131(6) Uiso 0.33 1 d PD B 2 F34B F -0.0565(16) 0.6451(6) 0.0247(7) 0.068(6) Uiso 0.33 1 d PD B 2 F35B F 0.010(2) 0.6777(7) 0.1960(8) 0.142(12) Uiso 0.33 1 d PD B 2 P29C P 0.0000(7) 0.6655(2) 0.1093(4) 0.041(2) Uiso 0.33 1 d PD C 3 F30C F -0.1669(9) 0.6748(4) 0.1252(6) 0.078(4) Uiso 0.33 1 d PD C 3 F31C F 0.0127(12) 0.7229(3) 0.0940(6) 0.075(4) Uiso 0.33 1 d PD C 3 F32C F 0.1585(10) 0.6583(4) 0.1088(7) 0.083(5) Uiso 0.33 1 d PD C 3 F33C F -0.0186(13) 0.6104(3) 0.1342(7) 0.078(4) Uiso 0.33 1 d PD C 3 F34C F -0.0333(11) 0.6563(4) 0.0242(5) 0.061(4) Uiso 0.33 1 d PD C 3 F35C F 0.0152(14) 0.6796(4) 0.2028(5) 0.047(4) Uiso 0.33 1 d PD C 3 P36A P 0.3831(7) 1.1394(2) 0.0518(4) 0.053(2) Uiso 0.34 1 d PD D 1 F37A F 0.4672(13) 1.1906(4) 0.0644(7) 0.067(4) Uiso 0.34 1 d PD D 1 F38A F 0.5163(11) 1.1116(4) 0.0925(8) 0.112(4) Uiso 0.34 1 d PD D 1 F39A F 0.3131(13) 1.0887(3) 0.0352(5) 0.058(3) Uiso 0.34 1 d PD D 1 F40A F 0.2589(9) 1.1664(3) 0.0098(5) 0.069(3) Uiso 0.34 1 d PD D 1 F41A F 0.4681(14) 1.1367(4) -0.0259(7) 0.103(5) Uiso 0.34 1 d PD D 1 F42A F 0.3050(12) 1.1442(4) 0.1265(6) 0.082(3) Uiso 0.34 1 d PD D 1 P36B P 0.4215(8) 1.1422(2) 0.0559(4) 0.057(2) Uiso 0.33 1 d PD E 2 F37B F 0.5711(11) 1.1381(4) 0.0220(7) 0.109(4) Uiso 0.33 1 d PD E 2 F38B F 0.3956(15) 1.0847(3) 0.0313(6) 0.102(4) Uiso 0.33 1 d PD E 2 F39B F 0.4887(10) 1.1244(3) 0.1341(5) 0.059(2) Uiso 0.33 1 d PD E 2 F40B F 0.4425(14) 1.1961(4) 0.0798(8) 0.099(6) Uiso 0.33 1 d PD E 2 F41B F 0.3562(15) 1.1582(5) -0.0256(7) 0.135(5) Uiso 0.33 1 d PD E 2 F42B F 0.2689(13) 1.1428(6) 0.0874(9) 0.160(7) Uiso 0.33 1 d PD E 2 P36C P 0.4161(8) 1.1339(2) 0.0367(3) 0.0528(18) Uiso 0.33 1 d PD F 3 F37C F 0.5442(13) 1.1692(5) 0.0475(7) 0.120(4) Uiso 0.33 1 d PD F 3 F38C F 0.5120(10) 1.0882(3) 0.0429(6) 0.081(3) Uiso 0.33 1 d PD F 3 F39C F 0.4032(15) 1.1314(4) 0.1306(5) 0.091(3) Uiso 0.33 1 d PD F 3 F40C F 0.3077(14) 1.1796(5) 0.0352(8) 0.142(6) Uiso 0.33 1 d PD F 3 F41C F 0.2804(13) 1.0992(5) 0.0330(9) 0.135(9) Uiso 0.33 1 d PD F 3 F42C F 0.4175(11) 1.1371(3) -0.0494(5) 0.057(3) Uiso 0.33 1 d PD F 3 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 Fe1A 0.0512(4) 0.0305(3) 0.0490(4) 0.0028(3) 0.0025(3) -0.0020(3) N2A 0.048(2) 0.044(2) 0.052(2) 0.0017(19) -0.008(2) -0.0036(18) C3A 0.075(4) 0.078(4) 0.063(4) 0.003(3) -0.024(3) -0.015(3) C4A 0.091(5) 0.088(4) 0.062(4) 0.018(3) -0.024(3) -0.010(4) N5A 0.069(3) 0.058(3) 0.071(3) 0.021(2) 0.002(3) 0.008(2) C6A 0.069(4) 0.098(5) 0.117(6) 0.037(5) 0.010(4) 0.034(4) C7A 0.094(5) 0.075(4) 0.128(6) 0.031(4) 0.051(5) 0.044(4) N8A 0.083(3) 0.048(3) 0.078(3) 0.010(2) 0.031(3) 0.002(2) C9A 0.129(6) 0.056(3) 0.073(4) -0.014(3) 0.045(4) -0.012(4) C10A 0.146(6) 0.055(3) 0.071(4) -0.020(3) 0.044(4) -0.024(4) N11A 0.081(3) 0.034(2) 0.050(2) -0.0018(18) 0.012(2) -0.007(2) C12A 0.044(3) 0.038(3) 0.063(3) 0.002(2) -0.005(3) -0.009(2) C13A 0.040(3) 0.034(2) 0.052(3) 0.003(2) 0.000(2) 0.003(2) C14A 0.049(3) 0.030(2) 0.050(3) 0.002(2) -0.005(2) 0.004(2) C15A 0.070(4) 0.045(3) 0.058(3) -0.005(2) -0.015(3) 0.001(3) C16A 0.085(4) 0.055(3) 0.055(3) 0.010(3) -0.005(3) 0.014(3) C17A 0.070(4) 0.055(3) 0.077(4) 0.030(3) 0.010(3) 0.004(3) C18A 0.047(3) 0.045(3) 0.086(4) 0.015(3) 0.004(3) -0.002(2) O19A 0.060(2) 0.0380(17) 0.061(2) 0.0063(15) -0.0128(17) -0.0158(15) C20A 0.057(3) 0.034(2) 0.058(3) -0.002(2) -0.007(3) -0.003(2) C21A 0.041(3) 0.040(3) 0.051(3) 0.002(2) -0.006(2) -0.004(2) C22A 0.033(2) 0.043(3) 0.055(3) 0.002(2) -0.001(2) 0.003(2) C23A 0.058(3) 0.052(3) 0.067(4) -0.009(3) 0.014(3) 0.002(3) C24A 0.069(4) 0.070(4) 0.078(4) 0.001(3) 0.028(3) -0.003(3) C25A 0.059(4) 0.054(3) 0.104(5) 0.006(3) 0.028(3) -0.009(3) C26A 0.048(3) 0.046(3) 0.086(4) 0.001(3) 0.008(3) -0.007(2) O27A 0.057(2) 0.0360(16) 0.063(2) -0.0062(15) 0.0126(17) -0.0060(15) Fe1B 0.0374(4) 0.0340(3) 0.0613(5) -0.0071(3) -0.0001(3) 0.0010(3) N2B 0.062(3) 0.052(3) 0.076(3) -0.011(2) -0.023(3) 0.012(2) C3B 0.146(7) 0.082(5) 0.140(7) -0.020(5) -0.087(6) 0.015(5) C4B 0.208(10) 0.094(6) 0.191(10) 0.026(6) -0.151(9) -0.042(6) N5B 0.064(3) 0.058(3) 0.091(4) -0.024(3) -0.009(3) -0.009(2) C6B 0.054(4) 0.091(5) 0.124(6) -0.023(4) -0.009(4) -0.026(3) C7B 0.055(4) 0.084(4) 0.125(6) -0.009(4) 0.023(4) -0.007(3) N8B 0.054(3) 0.050(3) 0.082(3) -0.016(2) 0.020(2) -0.005(2) C9B 0.086(4) 0.057(3) 0.076(4) 0.001(3) 0.021(3) -0.006(3) C10B 0.086(4) 0.053(3) 0.053(3) 0.004(2) 0.012(3) 0.006(3) N11B 0.056(2) 0.040(2) 0.047(2) -0.0041(18) 0.002(2) -0.0014(19) C12B 0.056(3) 0.048(3) 0.083(4) 0.007(3) -0.005(3) 0.018(3) C13B 0.041(3) 0.037(2) 0.061(3) -0.003(2) 0.004(2) 0.006(2) C14B 0.042(3) 0.034(2) 0.063(3) -0.004(2) 0.007(2) -0.003(2) C15B 0.062(3) 0.044(3) 0.066(4) -0.003(2) -0.004(3) 0.002(2) C16B 0.079(4) 0.041(3) 0.075(4) -0.018(3) 0.007(3) -0.004(3) C17B 0.078(4) 0.035(3) 0.091(4) -0.014(3) 0.017(3) 0.001(3) C18B 0.067(4) 0.036(3) 0.083(4) 0.004(3) 0.013(3) 0.012(2) O19B 0.054(2) 0.0337(17) 0.072(2) -0.0087(15) -0.0132(18) 0.0067(15) C20B 0.047(3) 0.034(2) 0.059(3) -0.003(2) -0.005(2) 0.003(2) C21B 0.038(3) 0.040(3) 0.055(3) -0.013(2) -0.001(2) -0.008(2) C22B 0.037(3) 0.043(3) 0.057(3) -0.009(2) 0.001(2) -0.009(2) C23B 0.064(4) 0.051(3) 0.064(4) -0.008(3) 0.013(3) -0.009(3) C24B 0.078(4) 0.061(4) 0.068(4) -0.019(3) 0.023(3) -0.022(3) C25B 0.048(3) 0.060(4) 0.092(5) -0.031(3) 0.017(3) -0.008(3) C26B 0.044(3) 0.049(3) 0.078(4) -0.015(3) 0.000(3) 0.002(2) O27B 0.050(2) 0.0474(19) 0.066(2) 0.0032(16) 0.0064(17) 0.0077(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 Fe1A O27A 1.924(3) . ? Fe1A O19A 1.929(3) . ? Fe1A N2A 2.126(4) . ? Fe1A N11A 2.137(4) . ? Fe1A N5A 2.197(4) . ? Fe1A N8A 2.230(4) . ? N2A C12A 1.300(6) . ? N2A C3A 1.489(6) . ? C3A C4A 1.538(8) . ? C4A N5A 1.487(7) . ? N5A C6A 1.481(7) . ? C6A C7A 1.512(9) . ? C7A N8A 1.496(7) . ? N8A C9A 1.498(7) . ? C9A C10A 1.542(8) . ? C10A N11A 1.490(6) . ? N11A C20A 1.294(6) . ? C12A C13A 1.443(6) . ? C13A C14A 1.423(6) . ? C13A C18A 1.427(6) . ? C14A O19A 1.341(5) . ? C14A C15A 1.409(6) . ? C15A C16A 1.398(7) . ? C16A C17A 1.388(8) . ? C17A C18A 1.383(7) . ? C20A C21A 1.454(7) . ? C21A C26A 1.418(6) . ? C21A C22A 1.431(6) . ? C22A O27A 1.337(5) . ? C22A C23A 1.410(7) . ? C23A C24A 1.397(7) . ? C24A C25A 1.399(8) . ? C25A C26A 1.378(7) . ? Fe1B O19B 1.923(3) . ? Fe1B O27B 1.934(3) . ? Fe1B N2B 2.133(4) . ? Fe1B N11B 2.138(4) . ? Fe1B N5B 2.197(4) . ? Fe1B N8B 2.236(4) . ? N2B C12B 1.303(6) . ? N2B C3B 1.472(7) . ? C3B C4B 1.349(9) . ? C4B N5B 1.466(8) . ? N5B C6B 1.499(8) . ? C6B C7B 1.515(9) . ? C7B N8B 1.484(7) . ? N8B C9B 1.503(7) . ? C9B C10B 1.498(7) . ? C10B N11B 1.496(6) . ? N11B C20B 1.292(6) . ? C12B C13B 1.447(7) . ? C13B C14B 1.410(6) . ? C13B C18B 1.420(6) . ? C14B O19B 1.335(5) . ? C14B C15B 1.414(7) . ? C15B C16B 1.388(7) . ? C16B C17B 1.388(8) . ? C17B C18B 1.380(8) . ? C20B C21B 1.456(7) . ? C21B C26B 1.430(6) . ? C21B C22B 1.435(6) . ? C22B O27B 1.340(5) . ? C22B C23B 1.413(7) . ? C23B C24B 1.391(7) . ? C24B C25B 1.394(8) . ? C25B C26B 1.384(7) . ? P29A F35A 1.554(11) . ? P29A F30A 1.555(11) . ? P29A F31A 1.618(10) . ? P29A F34A 1.637(12) . ? P29A F33A 1.639(11) . ? P29A F32A 1.730(12) . ? P29B F33B 1.602(14) . ? P29B F32B 1.606(13) . ? P29B F30B 1.614(12) . ? P29B F35B 1.616(14) . ? P29B F31B 1.626(12) . ? P29B F34B 1.629(13) . ? P29C F32C 1.538(11) . ? P29C F34C 1.570(10) . ? P29C F33C 1.608(11) . ? P29C F31C 1.623(10) . ? P29C F30C 1.665(10) . ? P29C F35C 1.727(10) . ? P36A F40A 1.570(10) . ? P36A F42A 1.581(10) . ? P36A F39A 1.583(10) . ? P36A F38A 1.635(11) . ? P36A F37A 1.646(10) . ? P36A F41A 1.659(11) . ? P36B F40B 1.566(11) . ? P36B F37B 1.596(12) . ? P36B F39B 1.597(9) . ? P36B F42B 1.601(13) . ? P36B F41B 1.627(11) . ? P36B F38B 1.673(11) . ? P36C F42C 1.553(9) . ? P36C F38C 1.569(9) . ? P36C F37C 1.579(11) . ? P36C F41C 1.622(12) . ? P36C F40C 1.642(12) . ? P36C F39C 1.703(10) . ? 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 O27A Fe1A O19A 102.25(15) . . ? O27A Fe1A N2A 101.50(14) . . ? O19A Fe1A N2A 86.86(13) . . ? O27A Fe1A N11A 87.17(15) . . ? O19A Fe1A N11A 94.61(14) . . ? N2A Fe1A N11A 170.72(16) . . ? O27A Fe1A N5A 90.95(16) . . ? O19A Fe1A N5A 160.15(15) . . ? N2A Fe1A N5A 75.91(16) . . ? N11A Fe1A N5A 100.86(17) . . ? O27A Fe1A N8A 157.51(14) . . ? O19A Fe1A N8A 93.49(16) . . ? N2A Fe1A N8A 95.25(16) . . ? N11A Fe1A N8A 75.52(17) . . ? N5A Fe1A N8A 78.60(18) . . ? C12A N2A C3A 117.9(4) . . ? C12A N2A Fe1A 124.2(3) . . ? C3A N2A Fe1A 117.0(3) . . ? N2A C3A C4A 108.5(4) . . ? N5A C4A C3A 109.4(5) . . ? C6A N5A C4A 114.9(5) . . ? C6A N5A Fe1A 110.3(4) . . ? C4A N5A Fe1A 106.2(3) . . ? N5A C6A C7A 108.9(5) . . ? N8A C7A C6A 107.9(5) . . ? C7A N8A C9A 115.3(5) . . ? C7A N8A Fe1A 107.7(3) . . ? C9A N8A Fe1A 106.5(3) . . ? N8A C9A C10A 109.1(5) . . ? N11A C10A C9A 110.3(4) . . ? C20A N11A C10A 117.9(4) . . ? C20A N11A Fe1A 125.3(3) . . ? C10A N11A Fe1A 116.6(3) . . ? N2A C12A C13A 126.2(4) . . ? C14A C13A C18A 118.1(4) . . ? C14A C13A C12A 123.8(4) . . ? C18A C13A C12A 118.1(4) . . ? O19A C14A C15A 119.5(4) . . ? O19A C14A C13A 121.5(4) . . ? C15A C14A C13A 119.0(4) . . ? C16A C15A C14A 120.6(5) . . ? C17A C16A C15A 121.2(5) . . ? C18A C17A C16A 118.8(5) . . ? C17A C18A C13A 122.1(5) . . ? C14A O19A Fe1A 132.1(3) . . ? N11A C20A C21A 126.7(4) . . ? C26A C21A C22A 118.6(5) . . ? C26A C21A C20A 118.5(4) . . ? C22A C21A C20A 122.8(4) . . ? O27A C22A C23A 119.4(4) . . ? O27A C22A C21A 122.2(4) . . ? C23A C22A C21A 118.3(4) . . ? C24A C23A C22A 121.5(5) . . ? C23A C24A C25A 119.9(5) . . ? C26A C25A C24A 119.8(5) . . ? C25A C26A C21A 121.8(5) . . ? C22A O27A Fe1A 133.2(3) . . ? O19B Fe1B O27B 106.43(15) . . ? O19B Fe1B N2B 85.08(14) . . ? O27B Fe1B N2B 92.94(16) . . ? O19B Fe1B N11B 91.00(13) . . ? O27B Fe1B N11B 85.71(14) . . ? N2B Fe1B N11B 175.32(16) . . ? O19B Fe1B N5B 155.71(16) . . ? O27B Fe1B N5B 91.28(17) . . ? N2B Fe1B N5B 77.39(17) . . ? N11B Fe1B N5B 107.10(16) . . ? O19B Fe1B N8B 90.18(15) . . ? O27B Fe1B N8B 156.35(14) . . ? N2B Fe1B N8B 105.41(17) . . ? N11B Fe1B N8B 77.10(15) . . ? N5B Fe1B N8B 78.63(18) . . ? C12B N2B C3B 118.9(5) . . ? C12B N2B Fe1B 127.9(4) . . ? C3B N2B Fe1B 113.2(4) . . ? C4B C3B N2B 113.5(6) . . ? C3B C4B N5B 120.0(6) . . ? C4B N5B C6B 113.8(6) . . ? C4B N5B Fe1B 110.1(4) . . ? C6B N5B Fe1B 110.8(4) . . ? N5B C6B C7B 110.4(5) . . ? N8B C7B C6B 108.6(5) . . ? C7B N8B C9B 113.0(4) . . ? C7B N8B Fe1B 108.8(4) . . ? C9B N8B Fe1B 111.7(3) . . ? C10B C9B N8B 109.1(4) . . ? N11B C10B C9B 107.7(4) . . ? C20B N11B C10B 120.0(4) . . ? C20B N11B Fe1B 127.6(3) . . ? C10B N11B Fe1B 112.4(3) . . ? N2B C12B C13B 125.5(5) . . ? C14B C13B C18B 119.0(5) . . ? C14B C13B C12B 122.3(4) . . ? C18B C13B C12B 118.7(4) . . ? O19B C14B C13B 122.8(4) . . ? O19B C14B C15B 118.9(4) . . ? C13B C14B C15B 118.2(4) . . ? C16B C15B C14B 121.3(5) . . ? C17B C16B C15B 120.7(5) . . ? C18B C17B C16B 119.1(5) . . ? C17B C18B C13B 121.8(5) . . ? C14B O19B Fe1B 136.1(3) . . ? N11B C20B C21B 125.8(4) . . ? C26B C21B C22B 118.4(5) . . ? C26B C21B C20B 118.8(4) . . ? C22B C21B C20B 122.8(4) . . ? O27B C22B C23B 119.6(4) . . ? O27B C22B C21B 121.7(4) . . ? C23B C22B C21B 118.7(4) . . ? C24B C23B C22B 121.0(5) . . ? C23B C24B C25B 120.7(5) . . ? C26B C25B C24B 119.8(5) . . ? C25B C26B C21B 121.3(5) . . ? C22B O27B Fe1B 135.8(3) . . ? F35A P29A F30A 99.8(7) . . ? F35A P29A F31A 90.2(6) . . ? F30A P29A F31A 93.3(7) . . ? F35A P29A F34A 169.2(8) . . ? F30A P29A F34A 90.5(7) . . ? F31A P29A F34A 92.4(7) . . ? F35A P29A F33A 89.2(6) . . ? F30A P29A F33A 89.5(7) . . ? F31A P29A F33A 177.1(9) . . ? F34A P29A F33A 87.7(7) . . ? F35A P29A F32A 84.2(7) . . ? F30A P29A F32A 176.0(8) . . ? F31A P29A F32A 87.3(7) . . ? F34A P29A F32A 85.4(7) . . ? F33A P29A F32A 89.9(7) . . ? F33B P29B F32B 177.3(10) . . ? F33B P29B F30B 90.3(8) . . ? F32B P29B F30B 89.7(8) . . ? F33B P29B F35B 92.1(9) . . ? F32B P29B F35B 90.6(9) . . ? F30B P29B F35B 92.8(9) . . ? F33B P29B F31B 92.8(8) . . ? F32B P29B F31B 87.0(8) . . ? F30B P29B F31B 175.1(9) . . ? F35B P29B F31B 90.8(9) . . ? F33B P29B F34B 89.2(9) . . ? F32B P29B F34B 88.1(8) . . ? F30B P29B F34B 88.4(8) . . ? F35B P29B F34B 178.2(11) . . ? F31B P29B F34B 87.9(8) . . ? F32C P29C F34C 97.2(7) . . ? F32C P29C F33C 90.1(7) . . ? F34C P29C F33C 95.6(7) . . ? F32C P29C F31C 92.5(7) . . ? F34C P29C F31C 90.5(6) . . ? F33C P29C F31C 173.1(8) . . ? F32C P29C F30C 170.3(8) . . ? F34C P29C F30C 92.6(6) . . ? F33C P29C F30C 88.7(6) . . ? F31C P29C F30C 87.7(6) . . ? F32C P29C F35C 90.1(7) . . ? F34C P29C F35C 172.3(7) . . ? F33C P29C F35C 87.0(6) . . ? F31C P29C F35C 86.6(6) . . ? F30C P29C F35C 80.2(6) . . ? F40A P36A F42A 89.2(6) . . ? F40A P36A F39A 91.6(7) . . ? F42A P36A F39A 91.0(6) . . ? F40A P36A F38A 177.6(7) . . ? F42A P36A F38A 93.1(7) . . ? F39A P36A F38A 88.8(6) . . ? F40A P36A F37A 90.6(6) . . ? F42A P36A F37A 93.6(7) . . ? F39A P36A F37A 174.9(8) . . ? F38A P36A F37A 88.8(6) . . ? F40A P36A F41A 90.7(6) . . ? F42A P36A F41A 177.6(7) . . ? F39A P36A F41A 91.3(6) . . ? F38A P36A F41A 86.9(7) . . ? F37A P36A F41A 84.0(6) . . ? F40B P36B F37B 93.9(7) . . ? F40B P36B F39B 90.8(6) . . ? F37B P36B F39B 89.1(6) . . ? F40B P36B F42B 90.1(8) . . ? F37B P36B F42B 176.0(8) . . ? F39B P36B F42B 91.5(7) . . ? F40B P36B F41B 91.5(7) . . ? F37B P36B F41B 89.3(7) . . ? F39B P36B F41B 177.3(8) . . ? F42B P36B F41B 90.0(8) . . ? F40B P36B F38B 178.7(9) . . ? F37B P36B F38B 87.4(7) . . ? F39B P36B F38B 89.1(6) . . ? F42B P36B F38B 88.7(7) . . ? F41B P36B F38B 88.6(7) . . ? F42C P36C F38C 94.7(6) . . ? F42C P36C F37C 92.3(6) . . ? F38C P36C F37C 92.4(7) . . ? F42C P36C F41C 92.5(7) . . ? F38C P36C F41C 89.5(7) . . ? F37C P36C F41C 174.8(8) . . ? F42C P36C F40C 88.8(6) . . ? F38C P36C F40C 175.3(8) . . ? F37C P36C F40C 90.7(7) . . ? F41C P36C F40C 87.1(7) . . ? F42C P36C F39C 176.2(8) . . ? F38C P36C F39C 88.2(6) . . ? F37C P36C F39C 90.1(6) . . ? F41C P36C F39C 85.1(7) . . ? F40C P36C F39C 88.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1A O19A C14A C13A 19.2(6) . . . . ? Fe1A O19A C14A C15A -162.5(3) . . . . ? Fe1A O27A C22A C21A 18.5(6) . . . . ? Fe1A O27A C22A C23A -162.9(3) . . . . ? Fe1B O19B C14B C13B -5.9(7) . . . . ? Fe1B O19B C14B C15B 174.5(4) . . . . ? Fe1B O27B C22B C21B -8.4(6) . . . . ? Fe1B O27B C22B C23B 175.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5A H5A F38A 0.92 2.25 3.166(12) 176.5 . N5A H5A F39A 0.92 2.50 3.131(12) 126.4 . N5A H5A F38B 0.92 2.29 3.036(12) 138.5 . N5A H5A F39B 0.92 2.31 3.166(9) 154.8 . N5A H5A F38C 0.92 2.32 3.176(10) 155.3 . N5A H5A F39C 0.92 2.45 3.241(11) 143.7 . N5B H5B F31A 0.92 2.33 3.206(10) 159.2 . N5B H5B F35A 0.92 2.44 3.224(10) 143.6 . N5B H5B F31B 0.92 2.30 3.112(11) 147.6 . N5B H5B F35B 0.92 2.40 3.165(18) 140.8 . N5B H5B F31C 0.92 2.32 3.215(11) 162.9 . N5B H5B F35C 0.92 2.37 3.117(12) 138.3 . N8B H8B F34A 0.92 2.65 3.549(13) 165.5 4_576 N8B H8B F34B 0.92 2.30 3.192(16) 163.6 4_576 N8B H8B F34C 0.92 2.17 3.024(11) 154.4 4_576 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.561 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.067 #=END data_rp9i2low _database_code_depnum_ccdc_archive 'CCDC 676634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(salicylaldiminato)-3,6-diazaoctane]iron(III) hexafluorophosphate ; _chemical_name_common ;(1,8-Bis(salicylaldiminato)-3,6-diazaoctane)iron(iii) hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, F6 P' _chemical_formula_sum 'C20 H24 F6 Fe N4 O2 P' _chemical_formula_weight 553.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5581(8) _cell_length_b 27.316(2) _cell_length_c 17.9457(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.340(5) _cell_angle_gamma 90.00 _cell_volume 4681.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 32023 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 24.70 _exptl_crystal_description Plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 1.007 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32023 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.70 _reflns_number_total 7879 _reflns_number_gt 5250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two independent complex cations and two anions, all lying on general positions. Both anions are disordered, and were modelled over three equally occupied sites with the refined restraints P---F = 1.61(2) and cis-F...F = 2.28(2)\%A. All wholly occupied non-H atoms were refined anisotropically, while all H atoms were placed in calculated positions and refined using a riding model. The amino group N8A---H8A does not form a hydrogen bond in the crystal, but donates a weak N---H...pi interaction to phenoxy ring C13B-C18B with H8A...X = 2.85\%A and N8A---H8A...X = 155.0\% (X = centroid of C13B-C18B). ; _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^)+(0.0565P)^2^+7.9306P] 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 7879 _refine_ls_number_parameters 656 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.56325(6) 0.99198(2) 0.24666(3) 0.02537(17) Uani 1 1 d . . . N2A N 0.4416(3) 0.92857(13) 0.22125(19) 0.0282(8) Uani 1 1 d . . . C3A C 0.3507(5) 0.93002(18) 0.1515(3) 0.0418(12) Uani 1 1 d . . . H3A1 H 0.2509 0.9277 0.1639 0.050 Uiso 1 1 calc R . . H3A2 H 0.3729 0.9021 0.1190 0.050 Uiso 1 1 calc R . . C4A C 0.3777(5) 0.97861(18) 0.1110(3) 0.0455(13) Uani 1 1 d . . . H4A1 H 0.4614 0.9754 0.0807 0.055 Uiso 1 1 calc R . . H4A2 H 0.2965 0.9866 0.0772 0.055 Uiso 1 1 calc R . . N5A N 0.3999(4) 1.01848(13) 0.1670(2) 0.0362(9) Uani 1 1 d . . . H5A H 0.4346 1.0457 0.1427 0.043 Uiso 1 1 calc R . . C6A C 0.2715(5) 1.0337(2) 0.2060(3) 0.0525(15) Uani 1 1 d . . . H6A1 H 0.2133 1.0047 0.2163 0.063 Uiso 1 1 calc R . . H6A2 H 0.2152 1.0566 0.1743 0.063 Uiso 1 1 calc R . . C7A C 0.3184(5) 1.05851(19) 0.2787(3) 0.0507(14) Uani 1 1 d . . . H7A1 H 0.3719 1.0886 0.2683 0.061 Uiso 1 1 calc R . . H7A2 H 0.2359 1.0677 0.3073 0.061 Uiso 1 1 calc R . . N8A N 0.4084(4) 1.02322(13) 0.3226(2) 0.0371(9) Uani 1 1 d . . . H8A H 0.3529 0.9981 0.3402 0.045 Uiso 1 1 calc R . . C9A C 0.4905(5) 1.04541(17) 0.3864(3) 0.0440(13) Uani 1 1 d . . . H9A1 H 0.5347 1.0193 0.4175 0.053 Uiso 1 1 calc R . . H9A2 H 0.4274 1.0644 0.4179 0.053 Uiso 1 1 calc R . . C10A C 0.6044(6) 1.07940(17) 0.3563(3) 0.0462(13) Uani 1 1 d . . . H10A H 0.5656 1.1127 0.3481 0.055 Uiso 1 1 calc R . . H10B H 0.6840 1.0817 0.3932 0.055 Uiso 1 1 calc R . . N11A N 0.6540(4) 1.05943(12) 0.28465(19) 0.0311(8) Uani 1 1 d . . . C12A C 0.4203(4) 0.89350(15) 0.2679(2) 0.0287(10) Uani 1 1 d . . . H12A H 0.3483 0.8707 0.2549 0.034 Uiso 1 1 calc R . . C13A C 0.4976(4) 0.88601(14) 0.3387(2) 0.0244(9) Uani 1 1 d . . . C14A C 0.6143(4) 0.91543(14) 0.3630(2) 0.0261(10) Uani 1 1 d . . . C15A C 0.6867(5) 0.90286(15) 0.4309(2) 0.0314(10) Uani 1 1 d . . . H15A H 0.7685 0.9205 0.4464 0.038 Uiso 1 1 calc R . . C16A C 0.6392(5) 0.86496(16) 0.4749(2) 0.0343(11) Uani 1 1 d . . . H16A H 0.6878 0.8576 0.5208 0.041 Uiso 1 1 calc R . . C17A C 0.5213(5) 0.83746(17) 0.4529(3) 0.0379(12) Uani 1 1 d . . . H17A H 0.4880 0.8124 0.4843 0.045 Uiso 1 1 calc R . . C18A C 0.4535(5) 0.84715(16) 0.3849(3) 0.0351(11) Uani 1 1 d . . . H18A H 0.3761 0.8275 0.3687 0.042 Uiso 1 1 calc R . . O19A O 0.6575(3) 0.95353(10) 0.32356(16) 0.0298(7) Uani 1 1 d . . . C20A C 0.7417(4) 1.08569(15) 0.2488(2) 0.0299(10) Uani 1 1 d . . . H20A H 0.7682 1.1163 0.2703 0.036 Uiso 1 1 calc R . . C21A C 0.8033(4) 1.07274(14) 0.1790(2) 0.0258(9) Uani 1 1 d . . . C22A C 0.7765(4) 1.02693(15) 0.1413(2) 0.0252(9) Uani 1 1 d . . . C23A C 0.8375(4) 1.01886(16) 0.0728(2) 0.0335(11) Uani 1 1 d . . . H23A H 0.8201 0.9889 0.0470 0.040 Uiso 1 1 calc R . . C24A C 0.9231(5) 1.05394(17) 0.0416(3) 0.0413(12) Uani 1 1 d . . . H24A H 0.9627 1.0476 -0.0051 0.050 Uiso 1 1 calc R . . C25A C 0.9522(5) 1.09854(17) 0.0782(3) 0.0423(12) Uani 1 1 d . . . H25A H 1.0112 1.1222 0.0567 0.051 Uiso 1 1 calc R . . C26A C 0.8926(4) 1.10734(16) 0.1465(3) 0.0336(11) Uani 1 1 d . . . H26A H 0.9124 1.1372 0.1718 0.040 Uiso 1 1 calc R . . O27A O 0.6973(3) 0.99207(10) 0.17044(15) 0.0295(7) Uani 1 1 d . . . Fe1B Fe 0.04378(6) 0.81430(2) 0.29705(3) 0.02535(17) Uani 1 1 d . . . N2B N -0.0524(4) 0.87760(13) 0.2481(2) 0.0339(9) Uani 1 1 d . . . C3B C -0.1323(5) 0.86665(19) 0.1776(3) 0.0502(14) Uani 1 1 d . . . H3B1 H -0.0675 0.8604 0.1370 0.060 Uiso 1 1 calc R . . H3B2 H -0.1932 0.8947 0.1631 0.060 Uiso 1 1 calc R . . C4B C -0.2186(6) 0.8225(2) 0.1909(3) 0.0546(15) Uani 1 1 d . . . H4B1 H -0.2584 0.8101 0.1428 0.065 Uiso 1 1 calc R . . H4B2 H -0.2972 0.8313 0.2226 0.065 Uiso 1 1 calc R . . N5B N -0.1310(4) 0.78274(13) 0.2291(2) 0.0375(9) Uani 1 1 d . . . H5B H -0.0936 0.7632 0.1924 0.045 Uiso 1 1 calc R . . C6B C -0.2193(5) 0.75123(18) 0.2761(3) 0.0427(12) Uani 1 1 d . . . H6B1 H -0.1751 0.7187 0.2828 0.051 Uiso 1 1 calc R . . H6B2 H -0.3127 0.7466 0.2512 0.051 Uiso 1 1 calc R . . C7B C -0.2347(5) 0.77547(18) 0.3515(3) 0.0426(12) Uani 1 1 d . . . H7B1 H -0.2871 0.8066 0.3454 0.051 Uiso 1 1 calc R . . H7B2 H -0.2870 0.7537 0.3846 0.051 Uiso 1 1 calc R . . N8B N -0.0916(4) 0.78519(13) 0.3848(2) 0.0331(9) Uani 1 1 d . . . H8B H -0.0996 0.8094 0.4208 0.040 Uiso 1 1 calc R . . C9B C -0.0283(5) 0.74088(16) 0.4222(3) 0.0386(11) Uani 1 1 d . . . H9B1 H -0.0576 0.7109 0.3946 0.046 Uiso 1 1 calc R . . H9B2 H -0.0603 0.7383 0.4738 0.046 Uiso 1 1 calc R . . C10B C 0.1311(5) 0.74597(16) 0.4231(2) 0.0334(11) Uani 1 1 d . . . H10C H 0.1622 0.7727 0.4572 0.040 Uiso 1 1 calc R . . H10D H 0.1762 0.7151 0.4403 0.040 Uiso 1 1 calc R . . N11B N 0.1688(4) 0.75711(12) 0.34591(19) 0.0276(8) Uani 1 1 d . . . C12B C -0.0450(4) 0.92287(16) 0.2711(3) 0.0336(11) Uani 1 1 d . . . H12B H -0.0952 0.9468 0.2424 0.040 Uiso 1 1 calc R . . C13B C 0.0341(4) 0.93944(15) 0.3372(2) 0.0270(10) Uani 1 1 d . . . C14B C 0.1159(4) 0.90725(14) 0.3830(2) 0.0263(10) Uani 1 1 d . . . C15B C 0.1899(5) 0.92655(15) 0.4463(2) 0.0321(10) Uani 1 1 d . . . H15B H 0.2467 0.9055 0.4770 0.039 Uiso 1 1 calc R . . C16B C 0.1804(5) 0.97574(16) 0.4641(3) 0.0353(11) Uani 1 1 d . . . H16B H 0.2297 0.9879 0.5073 0.042 Uiso 1 1 calc R . . C17B C 0.0992(5) 1.00778(16) 0.4194(3) 0.0363(11) Uani 1 1 d . . . H17B H 0.0936 1.0415 0.4319 0.044 Uiso 1 1 calc R . . C18B C 0.0275(5) 0.98985(15) 0.3569(3) 0.0347(11) Uani 1 1 d . . . H18B H -0.0275 1.0116 0.3265 0.042 Uiso 1 1 calc R . . O19B O 0.1267(3) 0.85943(10) 0.36819(16) 0.0314(7) Uani 1 1 d . . . C20B C 0.2695(4) 0.73292(15) 0.3162(2) 0.0273(10) Uani 1 1 d . . . H20B H 0.3128 0.7076 0.3452 0.033 Uiso 1 1 calc R . . C21B C 0.3211(4) 0.74136(15) 0.2425(2) 0.0275(10) Uani 1 1 d . . . C22B C 0.2692(4) 0.77948(15) 0.1947(2) 0.0278(10) Uani 1 1 d . . . C23B C 0.3307(5) 0.78650(16) 0.1249(2) 0.0349(11) Uani 1 1 d . . . H23B H 0.2977 0.8120 0.0927 0.042 Uiso 1 1 calc R . . C24B C 0.4387(5) 0.75633(17) 0.1033(3) 0.0388(12) Uani 1 1 d . . . H24B H 0.4792 0.7616 0.0565 0.047 Uiso 1 1 calc R . . C25B C 0.4888(5) 0.71844(17) 0.1494(3) 0.0379(12) Uani 1 1 d . . . H25B H 0.5618 0.6978 0.1336 0.046 Uiso 1 1 calc R . . C26B C 0.4317(4) 0.71117(16) 0.2179(3) 0.0327(10) Uani 1 1 d . . . H26B H 0.4668 0.6856 0.2493 0.039 Uiso 1 1 calc R . . O27B O 0.1670(3) 0.81015(10) 0.21467(16) 0.0326(7) Uani 1 1 d . . . P29A P -0.0113(9) 0.6669(3) 0.1233(4) 0.028(3) Uiso 0.34 1 d PD A 1 F30A F -0.1726(9) 0.6649(5) 0.1389(6) 0.025(3) Uiso 0.34 1 d PD A 1 F31A F -0.0240(15) 0.7238(3) 0.0960(6) 0.023(3) Uiso 0.34 1 d PD A 1 F32A F 0.1561(10) 0.6679(5) 0.1096(7) 0.035(4) Uiso 0.34 1 d PD A 1 F33A F 0.0061(13) 0.6105(3) 0.1529(6) 0.033(3) Uiso 0.34 1 d PD A 1 F34A F -0.0410(16) 0.6474(6) 0.0378(6) 0.041(6) Uiso 0.34 1 d PD A 1 F35A F 0.0180(12) 0.6850(4) 0.2079(5) 0.027(4) Uiso 0.34 1 d PD A 1 P29B P -0.0117(10) 0.6644(3) 0.1127(6) 0.038(4) Uiso 0.33 1 d PD B 2 F30B F 0.0446(9) 0.6098(3) 0.1314(5) 0.029(2) Uiso 0.33 1 d PD B 2 F31B F -0.0681(11) 0.7187(3) 0.0921(6) 0.054(4) Uiso 0.33 1 d PD B 2 F32B F -0.1654(10) 0.6501(4) 0.1394(6) 0.058(4) Uiso 0.33 1 d PD B 2 F33B F 0.1437(9) 0.6783(4) 0.0868(7) 0.047(3) Uiso 0.33 1 d PD B 2 F34B F -0.0596(14) 0.6461(5) 0.0303(7) 0.046(6) Uiso 0.33 1 d PD B 2 F35B F 0.0306(19) 0.6820(6) 0.1975(7) 0.047(10) Uiso 0.33 1 d PD B 2 P29C P 0.0053(7) 0.6698(2) 0.1135(5) 0.022(2) Uiso 0.33 1 d PD C 3 F30C F -0.1617(9) 0.6760(4) 0.1306(6) 0.044(4) Uiso 0.33 1 d PD C 3 F31C F 0.0091(11) 0.7278(3) 0.0941(6) 0.042(4) Uiso 0.33 1 d PD C 3 F32C F 0.1661(10) 0.6649(5) 0.0960(8) 0.038(4) Uiso 0.33 1 d PD C 3 F33C F -0.0076(12) 0.6126(3) 0.1351(7) 0.034(3) Uiso 0.33 1 d PD C 3 F34C F -0.0349(10) 0.6583(3) 0.0273(5) 0.024(3) Uiso 0.33 1 d PD C 3 F35C F 0.0471(14) 0.6841(5) 0.1991(6) 0.028(6) Uiso 0.33 1 d PD C 3 P36A P 0.3829(6) 1.1393(2) 0.0503(4) 0.0276(16) Uiso 0.34 1 d PD D 1 F37A F 0.4707(11) 1.1906(3) 0.0621(6) 0.031(3) Uiso 0.34 1 d PD D 1 F38A F 0.5176(8) 1.1110(3) 0.0938(6) 0.051(2) Uiso 0.34 1 d PD D 1 F39A F 0.3108(13) 1.0877(3) 0.0373(5) 0.024(3) Uiso 0.34 1 d PD D 1 F40A F 0.2615(8) 1.1668(3) 0.0053(5) 0.0274(19) Uiso 0.34 1 d PD D 1 F41A F 0.4732(9) 1.1331(3) -0.0252(5) 0.037(2) Uiso 0.34 1 d PD D 1 F42A F 0.3077(10) 1.1462(3) 0.1271(5) 0.034(2) Uiso 0.34 1 d PD D 1 P36B P 0.4147(8) 1.1416(2) 0.0547(4) 0.037(2) Uiso 0.33 1 d PD E 2 F37B F 0.5475(12) 1.1348(4) 0.0075(7) 0.099(4) Uiso 0.33 1 d PD E 2 F38B F 0.3647(13) 1.0850(4) 0.0340(6) 0.080(5) Uiso 0.33 1 d PD E 2 F39B F 0.4954(8) 1.1220(3) 0.1278(4) 0.0351(19) Uiso 0.33 1 d PD E 2 F40B F 0.4566(12) 1.1965(4) 0.0754(7) 0.059(5) Uiso 0.33 1 d PD E 2 F41B F 0.3204(14) 1.1623(5) -0.0160(7) 0.111(5) Uiso 0.33 1 d PD E 2 F42B F 0.2784(12) 1.1476(5) 0.1059(7) 0.095(6) Uiso 0.33 1 d PD E 2 P36C P 0.4147(6) 1.13315(17) 0.0357(3) 0.0303(14) Uiso 0.33 1 d PD F 3 F37C F 0.5367(11) 1.1733(4) 0.0458(6) 0.084(4) Uiso 0.33 1 d PD F 3 F38C F 0.5186(9) 1.0889(3) 0.0477(5) 0.063(3) Uiso 0.33 1 d PD F 3 F39C F 0.3962(12) 1.1339(3) 0.1274(5) 0.067(3) Uiso 0.33 1 d PD F 3 F40C F 0.2975(11) 1.1771(4) 0.0272(7) 0.080(4) Uiso 0.33 1 d PD F 3 F41C F 0.2843(11) 1.0946(4) 0.0306(7) 0.071(6) Uiso 0.33 1 d PD F 3 F42C F 0.4239(9) 1.1337(3) -0.0502(4) 0.035(2) Uiso 0.33 1 d PD F 3 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 Fe1A 0.0293(3) 0.0181(3) 0.0288(3) 0.0014(3) 0.0022(3) -0.0012(3) N2A 0.0286(19) 0.027(2) 0.029(2) 0.0015(16) -0.0017(16) -0.0034(16) C3A 0.041(3) 0.044(3) 0.039(3) 0.004(2) -0.015(2) -0.011(2) C4A 0.047(3) 0.053(3) 0.036(3) 0.008(2) -0.013(2) -0.005(2) N5A 0.040(2) 0.030(2) 0.039(2) 0.0138(18) 0.0023(18) 0.0028(17) C6A 0.037(3) 0.053(3) 0.067(4) 0.025(3) 0.003(3) 0.016(3) C7A 0.050(3) 0.043(3) 0.060(4) 0.011(3) 0.023(3) 0.018(3) N8A 0.043(2) 0.024(2) 0.045(2) 0.0072(18) 0.0144(19) 0.0027(17) C9A 0.065(3) 0.033(3) 0.035(3) -0.003(2) 0.018(3) -0.001(2) C10A 0.077(4) 0.027(3) 0.035(3) -0.007(2) 0.016(3) -0.012(2) N11A 0.043(2) 0.023(2) 0.028(2) -0.0015(16) 0.0056(17) -0.0006(17) C12A 0.024(2) 0.024(2) 0.038(3) -0.002(2) 0.001(2) -0.0039(18) C13A 0.021(2) 0.019(2) 0.033(2) 0.0005(18) 0.0025(18) 0.0006(17) C14A 0.028(2) 0.019(2) 0.032(2) -0.0018(19) 0.0045(19) 0.0028(18) C15A 0.035(2) 0.024(2) 0.034(3) -0.005(2) -0.004(2) 0.0024(19) C16A 0.041(3) 0.031(3) 0.032(3) 0.005(2) 0.000(2) 0.011(2) C17A 0.042(3) 0.032(3) 0.041(3) 0.016(2) 0.012(2) 0.005(2) C18A 0.029(2) 0.028(3) 0.049(3) 0.006(2) 0.008(2) 0.0000(19) O19A 0.0330(16) 0.0204(16) 0.0356(17) 0.0043(13) -0.0036(14) -0.0071(13) C20A 0.035(2) 0.019(2) 0.035(3) -0.0006(19) -0.005(2) -0.0019(19) C21A 0.023(2) 0.021(2) 0.033(2) 0.0026(19) 0.0005(19) -0.0017(17) C22A 0.020(2) 0.024(2) 0.032(2) 0.0043(19) -0.0028(18) 0.0018(18) C23A 0.034(3) 0.030(3) 0.037(3) -0.006(2) 0.007(2) -0.002(2) C24A 0.042(3) 0.040(3) 0.043(3) -0.001(2) 0.016(2) -0.001(2) C25A 0.037(3) 0.032(3) 0.059(3) 0.006(2) 0.015(2) -0.007(2) C26A 0.029(2) 0.029(3) 0.043(3) -0.001(2) 0.001(2) -0.0036(19) O27A 0.0347(16) 0.0203(15) 0.0339(17) -0.0019(13) 0.0070(14) -0.0058(13) Fe1B 0.0230(3) 0.0189(3) 0.0341(4) -0.0037(3) 0.0010(3) 0.0000(2) N2B 0.033(2) 0.029(2) 0.038(2) -0.0049(18) -0.0112(17) 0.0062(17) C3B 0.054(3) 0.044(3) 0.050(3) -0.005(3) -0.019(3) 0.006(3) C4B 0.048(3) 0.056(4) 0.057(4) -0.001(3) -0.021(3) -0.002(3) N5B 0.034(2) 0.032(2) 0.046(2) -0.0106(18) -0.0035(18) -0.0050(17) C6B 0.026(2) 0.043(3) 0.059(3) -0.009(3) -0.004(2) -0.010(2) C7B 0.031(3) 0.037(3) 0.061(3) -0.006(2) 0.012(2) -0.002(2) N8B 0.032(2) 0.028(2) 0.040(2) -0.0114(17) 0.0094(17) -0.0029(16) C9B 0.046(3) 0.031(3) 0.040(3) -0.006(2) 0.012(2) -0.004(2) C10B 0.047(3) 0.024(2) 0.029(2) 0.001(2) 0.000(2) -0.001(2) N11B 0.031(2) 0.0211(19) 0.030(2) -0.0037(16) 0.0009(16) -0.0027(16) C12B 0.029(2) 0.030(3) 0.042(3) 0.004(2) 0.002(2) 0.007(2) C13B 0.024(2) 0.023(2) 0.035(3) -0.0022(19) 0.0069(19) -0.0011(18) C14B 0.023(2) 0.020(2) 0.037(3) -0.0017(19) 0.0061(19) -0.0005(17) C15B 0.034(2) 0.024(2) 0.038(3) -0.001(2) -0.002(2) 0.0007(19) C16B 0.039(3) 0.025(2) 0.042(3) -0.010(2) 0.002(2) -0.005(2) C17B 0.041(3) 0.021(2) 0.048(3) -0.006(2) 0.008(2) 0.001(2) C18B 0.035(3) 0.021(2) 0.049(3) 0.004(2) 0.006(2) 0.006(2) O19B 0.0335(17) 0.0183(16) 0.0419(18) -0.0047(13) -0.0068(14) 0.0035(13) C20B 0.023(2) 0.022(2) 0.037(3) -0.0033(19) -0.0065(19) -0.0005(18) C21B 0.024(2) 0.023(2) 0.036(3) -0.0082(19) 0.0002(19) -0.0071(18) C22B 0.024(2) 0.025(2) 0.035(3) -0.009(2) 0.0002(19) -0.0042(19) C23B 0.040(3) 0.029(3) 0.036(3) -0.003(2) 0.006(2) -0.010(2) C24B 0.040(3) 0.038(3) 0.039(3) -0.010(2) 0.014(2) -0.013(2) C25B 0.028(2) 0.033(3) 0.053(3) -0.019(2) 0.007(2) -0.005(2) C26B 0.029(2) 0.027(2) 0.042(3) -0.007(2) -0.001(2) -0.0018(19) O27B 0.0322(16) 0.0296(17) 0.0363(17) 0.0023(14) 0.0038(14) 0.0002(14) _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 Fe1A O27A 1.912(3) . ? Fe1A O19A 1.928(3) . ? Fe1A N2A 2.126(3) . ? Fe1A N11A 2.136(4) . ? Fe1A N5A 2.196(4) . ? Fe1A N8A 2.223(4) . ? N2A C12A 1.294(5) . ? N2A C3A 1.494(5) . ? C3A C4A 1.540(7) . ? C4A N5A 1.491(6) . ? N5A C6A 1.496(6) . ? C6A C7A 1.523(7) . ? C7A N8A 1.495(6) . ? N8A C9A 1.490(6) . ? C9A C10A 1.545(6) . ? C10A N11A 1.492(5) . ? N11A C20A 1.294(5) . ? C12A C13A 1.458(6) . ? C13A C18A 1.421(6) . ? C13A C14A 1.429(6) . ? C14A O19A 1.334(5) . ? C14A C15A 1.418(6) . ? C15A C16A 1.390(6) . ? C16A C17A 1.398(6) . ? C17A C18A 1.385(6) . ? C20A C21A 1.450(6) . ? C21A C26A 1.416(6) . ? C21A C22A 1.440(6) . ? C22A O27A 1.336(5) . ? C22A C23A 1.401(6) . ? C23A C24A 1.392(6) . ? C24A C25A 1.406(7) . ? C25A C26A 1.394(6) . ? Fe1B O19B 1.922(3) . ? Fe1B O27B 1.931(3) . ? Fe1B N2B 2.131(4) . ? Fe1B N11B 2.133(3) . ? Fe1B N5B 2.203(4) . ? Fe1B N8B 2.225(3) . ? N2B C12B 1.305(5) . ? N2B C3B 1.481(6) . ? C3B C4B 1.486(7) . ? C4B N5B 1.517(6) . ? N5B C6B 1.491(6) . ? C6B C7B 1.519(6) . ? C7B N8B 1.494(6) . ? N8B C9B 1.499(6) . ? C9B C10B 1.529(6) . ? C10B N11B 1.478(5) . ? N11B C20B 1.300(5) . ? C12B C13B 1.454(6) . ? C13B C14B 1.416(6) . ? C13B C18B 1.424(6) . ? C14B O19B 1.338(5) . ? C14B C15B 1.416(6) . ? C15B C16B 1.385(6) . ? C16B C17B 1.401(6) . ? C17B C18B 1.379(6) . ? C20B C21B 1.449(6) . ? C21B C22B 1.424(6) . ? C21B C26B 1.425(6) . ? C22B O27B 1.346(5) . ? C22B C23B 1.418(6) . ? C23B C24B 1.389(6) . ? C24B C25B 1.397(7) . ? C25B C26B 1.380(6) . ? P29A F30A 1.579(11) . ? P29A F35A 1.610(11) . ? P29A F32A 1.629(11) . ? P29A F31A 1.634(10) . ? P29A F33A 1.634(10) . ? P29A F34A 1.638(12) . ? P29B F34B 1.609(12) . ? P29B F32B 1.612(12) . ? P29B F31B 1.615(11) . ? P29B F30B 1.616(10) . ? P29B F33B 1.620(12) . ? P29B F35B 1.631(12) . ? P29C F32C 1.586(11) . ? P29C F34C 1.609(10) . ? P29C F33C 1.615(10) . ? P29C F35C 1.619(11) . ? P29C F31C 1.623(10) . ? P29C F30C 1.646(10) . ? P36A F40A 1.578(8) . ? P36A F39A 1.582(9) . ? P36A F42A 1.591(9) . ? P36A F37A 1.642(9) . ? P36A F41A 1.645(9) . ? P36A F38A 1.668(9) . ? P36B F37B 1.566(11) . ? P36B F39B 1.587(9) . ? P36B F40B 1.590(11) . ? P36B F41B 1.628(11) . ? P36B F42B 1.632(12) . ? P36B F38B 1.656(10) . ? P36C F42C 1.549(8) . ? P36C F38C 1.574(9) . ? P36C F37C 1.606(10) . ? P36C F41C 1.632(11) . ? P36C F40C 1.645(10) . ? P36C F39C 1.662(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O27A Fe1A O19A 101.87(12) . . ? O27A Fe1A N2A 102.96(12) . . ? O19A Fe1A N2A 86.86(12) . . ? O27A Fe1A N11A 87.26(12) . . ? O19A Fe1A N11A 93.99(13) . . ? N2A Fe1A N11A 169.36(13) . . ? O27A Fe1A N5A 90.74(13) . . ? O19A Fe1A N5A 160.82(13) . . ? N2A Fe1A N5A 76.16(14) . . ? N11A Fe1A N5A 101.07(14) . . ? O27A Fe1A N8A 157.01(13) . . ? O19A Fe1A N8A 94.20(13) . . ? N2A Fe1A N8A 94.14(14) . . ? N11A Fe1A N8A 75.22(14) . . ? N5A Fe1A N8A 78.44(14) . . ? C12A N2A C3A 117.4(4) . . ? C12A N2A Fe1A 124.3(3) . . ? C3A N2A Fe1A 116.9(3) . . ? N2A C3A C4A 108.4(4) . . ? N5A C4A C3A 109.5(4) . . ? C4A N5A C6A 114.9(4) . . ? C4A N5A Fe1A 106.0(3) . . ? C6A N5A Fe1A 111.2(3) . . ? N5A C6A C7A 107.9(4) . . ? N8A C7A C6A 107.9(4) . . ? C9A N8A C7A 114.6(4) . . ? C9A N8A Fe1A 106.6(3) . . ? C7A N8A Fe1A 107.9(3) . . ? N8A C9A C10A 109.4(4) . . ? N11A C10A C9A 109.6(4) . . ? C20A N11A C10A 117.4(4) . . ? C20A N11A Fe1A 125.6(3) . . ? C10A N11A Fe1A 116.8(3) . . ? N2A C12A C13A 125.5(4) . . ? C18A C13A C14A 119.3(4) . . ? C18A C13A C12A 117.4(4) . . ? C14A C13A C12A 123.3(4) . . ? O19A C14A C15A 119.6(4) . . ? O19A C14A C13A 122.1(4) . . ? C15A C14A C13A 118.3(4) . . ? C16A C15A C14A 120.6(4) . . ? C15A C16A C17A 121.2(4) . . ? C18A C17A C16A 119.3(4) . . ? C17A C18A C13A 121.2(4) . . ? C14A O19A Fe1A 131.3(3) . . ? N11A C20A C21A 126.0(4) . . ? C26A C21A C22A 119.0(4) . . ? C26A C21A C20A 117.8(4) . . ? C22A C21A C20A 123.2(4) . . ? O27A C22A C23A 119.6(4) . . ? O27A C22A C21A 121.9(4) . . ? C23A C22A C21A 118.5(4) . . ? C24A C23A C22A 121.1(4) . . ? C23A C24A C25A 121.2(4) . . ? C26A C25A C24A 118.7(4) . . ? C25A C26A C21A 121.5(4) . . ? C22A O27A Fe1A 133.4(3) . . ? O19B Fe1B O27B 107.36(13) . . ? O19B Fe1B N2B 84.99(13) . . ? O27B Fe1B N2B 89.89(13) . . ? O19B Fe1B N11B 89.30(12) . . ? O27B Fe1B N11B 85.57(12) . . ? N2B Fe1B N11B 171.32(14) . . ? O19B Fe1B N5B 154.33(13) . . ? O27B Fe1B N5B 91.46(13) . . ? N2B Fe1B N5B 77.57(14) . . ? N11B Fe1B N5B 109.90(13) . . ? O19B Fe1B N8B 89.71(13) . . ? O27B Fe1B N8B 155.69(13) . . ? N2B Fe1B N8B 109.17(14) . . ? N11B Fe1B N8B 77.28(13) . . ? N5B Fe1B N8B 78.61(14) . . ? C12B N2B C3B 118.7(4) . . ? C12B N2B Fe1B 128.5(3) . . ? C3B N2B Fe1B 112.8(3) . . ? N2B C3B C4B 107.3(4) . . ? C3B C4B N5B 110.7(4) . . ? C6B N5B C4B 110.7(4) . . ? C6B N5B Fe1B 110.3(3) . . ? C4B N5B Fe1B 111.2(3) . . ? N5B C6B C7B 109.3(4) . . ? N8B C7B C6B 108.3(3) . . ? C7B N8B C9B 112.4(3) . . ? C7B N8B Fe1B 109.2(3) . . ? C9B N8B Fe1B 111.7(2) . . ? N8B C9B C10B 108.4(3) . . ? N11B C10B C9B 106.8(3) . . ? C20B N11B C10B 119.6(4) . . ? C20B N11B Fe1B 128.0(3) . . ? C10B N11B Fe1B 112.5(3) . . ? N2B C12B C13B 124.9(4) . . ? C14B C13B C18B 119.0(4) . . ? C14B C13B C12B 122.5(4) . . ? C18B C13B C12B 118.5(4) . . ? O19B C14B C15B 118.9(4) . . ? O19B C14B C13B 122.5(4) . . ? C15B C14B C13B 118.7(4) . . ? C16B C15B C14B 120.7(4) . . ? C15B C16B C17B 120.9(4) . . ? C18B C17B C16B 119.3(4) . . ? C17B C18B C13B 121.3(4) . . ? C14B O19B Fe1B 136.5(3) . . ? N11B C20B C21B 125.4(4) . . ? C22B C21B C26B 118.8(4) . . ? C22B C21B C20B 122.8(4) . . ? C26B C21B C20B 118.3(4) . . ? O27B C22B C23B 118.8(4) . . ? O27B C22B C21B 122.2(4) . . ? C23B C22B C21B 118.9(4) . . ? C24B C23B C22B 120.4(4) . . ? C23B C24B C25B 121.0(4) . . ? C26B C25B C24B 119.7(4) . . ? C25B C26B C21B 121.2(4) . . ? C22B O27B Fe1B 135.4(3) . . ? F30A P29A F35A 88.6(6) . . ? F30A P29A F32A 178.1(8) . . ? F35A P29A F32A 90.2(7) . . ? F30A P29A F31A 91.4(7) . . ? F35A P29A F31A 89.9(6) . . ? F32A P29A F31A 90.0(7) . . ? F30A P29A F33A 89.9(7) . . ? F35A P29A F33A 88.3(6) . . ? F32A P29A F33A 88.7(6) . . ? F31A P29A F33A 177.8(8) . . ? F30A P29A F34A 91.3(7) . . ? F35A P29A F34A 178.9(8) . . ? F32A P29A F34A 89.9(7) . . ? F31A P29A F34A 91.2(7) . . ? F33A P29A F34A 90.5(7) . . ? F34B P29B F32B 88.2(7) . . ? F34B P29B F31B 89.7(7) . . ? F32B P29B F31B 89.5(7) . . ? F34B P29B F30B 89.1(7) . . ? F32B P29B F30B 90.8(7) . . ? F31B P29B F30B 178.8(8) . . ? F34B P29B F33B 92.3(8) . . ? F32B P29B F33B 179.2(9) . . ? F31B P29B F33B 91.1(7) . . ? F30B P29B F33B 88.6(6) . . ? F34B P29B F35B 177.6(10) . . ? F32B P29B F35B 89.4(8) . . ? F31B P29B F35B 90.6(8) . . ? F30B P29B F35B 90.6(8) . . ? F33B P29B F35B 90.1(8) . . ? F32C P29C F34C 89.4(6) . . ? F32C P29C F33C 92.9(6) . . ? F34C P29C F33C 91.4(6) . . ? F32C P29C F35C 90.2(7) . . ? F34C P29C F35C 177.2(7) . . ? F33C P29C F35C 91.4(6) . . ? F32C P29C F31C 90.5(6) . . ? F34C P29C F31C 89.4(6) . . ? F33C P29C F31C 176.5(7) . . ? F35C P29C F31C 87.8(6) . . ? F32C P29C F30C 178.7(8) . . ? F34C P29C F30C 90.2(6) . . ? F33C P29C F30C 88.4(6) . . ? F35C P29C F30C 90.1(7) . . ? F31C P29C F30C 88.3(6) . . ? F40A P36A F39A 92.4(6) . . ? F40A P36A F42A 92.2(6) . . ? F39A P36A F42A 91.4(5) . . ? F40A P36A F37A 91.2(5) . . ? F39A P36A F37A 175.0(7) . . ? F42A P36A F37A 91.9(6) . . ? F40A P36A F41A 91.6(5) . . ? F39A P36A F41A 91.5(6) . . ? F42A P36A F41A 175.2(7) . . ? F37A P36A F41A 85.0(5) . . ? F40A P36A F38A 176.6(6) . . ? F39A P36A F38A 88.8(6) . . ? F42A P36A F38A 91.0(5) . . ? F37A P36A F38A 87.4(5) . . ? F41A P36A F38A 85.2(5) . . ? F37B P36B F39B 91.7(6) . . ? F37B P36B F40B 92.1(7) . . ? F39B P36B F40B 90.9(6) . . ? F37B P36B F41B 93.1(7) . . ? F39B P36B F41B 175.2(8) . . ? F40B P36B F41B 89.0(6) . . ? F37B P36B F42B 178.3(8) . . ? F39B P36B F42B 86.6(6) . . ? F40B P36B F42B 88.5(7) . . ? F41B P36B F42B 88.5(7) . . ? F37B P36B F38B 90.1(7) . . ? F39B P36B F38B 89.8(5) . . ? F40B P36B F38B 177.7(8) . . ? F41B P36B F38B 90.1(6) . . ? F42B P36B F38B 89.4(7) . . ? F42C P36C F38C 94.7(5) . . ? F42C P36C F37C 92.0(5) . . ? F38C P36C F37C 93.3(6) . . ? F42C P36C F41C 91.4(6) . . ? F38C P36C F41C 89.3(6) . . ? F37C P36C F41C 175.5(7) . . ? F42C P36C F40C 88.1(5) . . ? F38C P36C F40C 175.6(6) . . ? F37C P36C F40C 90.0(6) . . ? F41C P36C F40C 87.2(6) . . ? F42C P36C F39C 176.9(7) . . ? F38C P36C F39C 88.1(5) . . ? F37C P36C F39C 89.2(5) . . ? F41C P36C F39C 87.3(6) . . ? F40C P36C F39C 89.1(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5A H5A F38A 0.93 2.15 3.082(9) 176.1 . N5A H5A F39A 0.93 2.47 3.091(12) 124.2 . N5A H5A F38B 0.93 2.30 3.007(12) 132.4 . N5A H5A F39B 0.93 2.18 3.063(8) 157.3 . N5A H5A F38C 0.93 2.25 3.125(10) 157.0 . N5A H5A F39C 0.93 2.45 3.232(10) 141.7 . N5B H5B F31A 0.93 2.16 3.088(11) 172.0 . N5B H5B F35A 0.93 2.40 3.058(12) 127.6 . N5B H5B F31B 0.93 2.19 3.096(11) 163.3 . N5B H5B F35B 0.93 2.51 3.216(17) 132.4 . N5B H5B F31C 0.93 2.27 3.191(11) 170.2 . N5B H5B F35C 0.93 2.55 3.244(14) 132.1 . N8B H8B F34A 0.93 2.45 3.325(14) 156.2 4_576 N8B H8B F34B 0.93 2.33 3.220(15) 160.5 4_576 N8B H8B F34C 0.93 2.17 3.017(10) 150.7 4_576 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.811 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.078 #=END data_rp9blm _database_code_depnum_ccdc_archive 'CCDC 676635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(salicylaldiminato)-3,6-diazaoctane]iron(III) tetraphenylborate hemi-acetone solvate ; _chemical_name_common ; (1,8-Bis(salicylaldiminato)-3,6-diazaoctane)iron(iii) tetraphenylborate hemi-acetone solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C24 H20 B, 0.5[C3 H6 O]' _chemical_formula_sum 'C45.50 H47 B Fe N4 O2.50' _chemical_formula_weight 756.53 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.977(2) _cell_length_b 10.8833(12) _cell_length_c 28.562(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.321(5) _cell_angle_gamma 90.00 _cell_volume 7857.7(14) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 53384 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 31.29 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53384 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 31.29 _reflns_number_total 12790 _reflns_number_gt 9174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. This is isostructural to a putatively unsolvated crystal previously published by Nishida et al (J. Chem. Soc. Dalton Trans., 1987, 1957). Given the poor quality of their refinement, we suggest that their crystal probably did in fact contain half an equivalent of disordered solvent, as here, which they neglected to model. The asymmetric unit contains one cation (Fe1-O27) and anion (B28-C52), and half an acetone molecule (C53-C56) disordered about the C~2~ axis [1/2, y, 3/4]. The latter residue was modelled over two sites, labelled 'A' (occupancy 0.30) and 'B' (0.20), with a common quaternary C atom C53 lying directly on the special position. The restraints C53---C = 1.52(1), C53---O = 1.22(1), 1,3-C...O = 2.37(2) and 1,3-C...C = 2.63(2)\%A were applied to these groups. All crystallographically ordered non-H atoms (including C53) were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. No hydrogen bonds are formed by the N---H groups N5 and N8 in the cation ; _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^)+(0.0528P)^2^+5.5015P] 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 12790 _refine_ls_number_parameters 498 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.602553(8) 0.51038(2) 0.613888(8) 0.02210(6) Uani 1 1 d . . . N2 N 0.61595(5) 0.53233(15) 0.69015(5) 0.0285(3) Uani 1 1 d . . . C3 C 0.63784(8) 0.65268(19) 0.71043(6) 0.0370(4) Uani 1 1 d . . . H3A H 0.6758 0.6436 0.7264 0.044 Uiso 1 1 calc R . . H3B H 0.6188 0.6812 0.7347 0.044 Uiso 1 1 calc R . . C4 C 0.63132(7) 0.74668(18) 0.66942(7) 0.0340(4) Uani 1 1 d . . . H4A H 0.5943 0.7760 0.6605 0.041 Uiso 1 1 calc R . . H4B H 0.6546 0.8183 0.6799 0.041 Uiso 1 1 calc R . . N5 N 0.64562(5) 0.68669(13) 0.62711(5) 0.0268(3) Uani 1 1 d . . . H5 H 0.6342 0.7368 0.6004 0.032 Uiso 1 1 calc R . . C6 C 0.70373(6) 0.66586(17) 0.63384(7) 0.0338(4) Uani 1 1 d . . . H6A H 0.7190 0.6356 0.6668 0.041 Uiso 1 1 calc R . . H6B H 0.7216 0.7437 0.6291 0.041 Uiso 1 1 calc R . . C7 C 0.71176(7) 0.57084(17) 0.59694(8) 0.0355(4) Uani 1 1 d . . . H7A H 0.6987 0.6034 0.5640 0.043 Uiso 1 1 calc R . . H7B H 0.7499 0.5516 0.6016 0.043 Uiso 1 1 calc R . . N8 N 0.68172(5) 0.45716(14) 0.60362(5) 0.0290(3) Uani 1 1 d . . . H8 H 0.7000 0.4158 0.6309 0.035 Uiso 1 1 calc R . . C9 C 0.67160(8) 0.37038(18) 0.56164(7) 0.0360(4) Uani 1 1 d . . . H9A H 0.6571 0.2921 0.5707 0.043 Uiso 1 1 calc R . . H9B H 0.7052 0.3524 0.5522 0.043 Uiso 1 1 calc R . . C10 C 0.63169(8) 0.42959(18) 0.51888(7) 0.0354(4) Uani 1 1 d . . . H10A H 0.6508 0.4803 0.4996 0.043 Uiso 1 1 calc R . . H10B H 0.6121 0.3646 0.4978 0.043 Uiso 1 1 calc R . . N11 N 0.59395(5) 0.50765(13) 0.53773(5) 0.0244(3) Uani 1 1 d . . . C12 C 0.60433(6) 0.45151(19) 0.71974(6) 0.0306(4) Uani 1 1 d . . . H12 H 0.6078 0.4766 0.7522 0.037 Uiso 1 1 calc R . . C13 C 0.58653(6) 0.32687(18) 0.70775(6) 0.0297(4) Uani 1 1 d . . . C14 C 0.58000(6) 0.27524(17) 0.66060(6) 0.0278(3) Uani 1 1 d . . . C15 C 0.56637(7) 0.14930(18) 0.65383(7) 0.0345(4) Uani 1 1 d . . . H15 H 0.5629 0.1129 0.6230 0.041 Uiso 1 1 calc R . . C16 C 0.55794(7) 0.0780(2) 0.69225(8) 0.0435(5) Uani 1 1 d . . . H16 H 0.5485 -0.0060 0.6871 0.052 Uiso 1 1 calc R . . C17 C 0.56318(8) 0.1288(2) 0.73797(8) 0.0485(6) Uani 1 1 d . . . H17 H 0.5571 0.0796 0.7637 0.058 Uiso 1 1 calc R . . C18 C 0.57725(8) 0.2511(2) 0.74575(7) 0.0426(5) Uani 1 1 d . . . H18 H 0.5808 0.2852 0.7769 0.051 Uiso 1 1 calc R . . O19 O 0.58632(5) 0.34195(12) 0.62320(4) 0.0338(3) Uani 1 1 d . . . C20 C 0.56326(6) 0.57959(15) 0.50745(5) 0.0241(3) Uani 1 1 d . . . H20 H 0.5655 0.5749 0.4748 0.029 Uiso 1 1 calc R . . C21 C 0.52572(6) 0.66692(16) 0.51917(6) 0.0249(3) Uani 1 1 d . . . C22 C 0.51448(6) 0.67465(16) 0.56577(6) 0.0259(3) Uani 1 1 d . . . C23 C 0.47863(7) 0.7662(2) 0.57355(7) 0.0409(5) Uani 1 1 d . . . H23 H 0.4702 0.7726 0.6041 0.049 Uiso 1 1 calc R . . C24 C 0.45542(9) 0.8474(2) 0.53673(9) 0.0534(6) Uani 1 1 d . . . H24 H 0.4324 0.9100 0.5430 0.064 Uiso 1 1 calc R . . C25 C 0.46571(9) 0.8378(2) 0.49083(9) 0.0549(6) Uani 1 1 d . . . H25 H 0.4492 0.8923 0.4659 0.066 Uiso 1 1 calc R . . C26 C 0.50009(7) 0.7481(2) 0.48221(7) 0.0383(4) Uani 1 1 d . . . H26 H 0.5067 0.7406 0.4510 0.046 Uiso 1 1 calc R . . O27 O 0.53593(4) 0.59770(12) 0.60157(4) 0.0289(3) Uani 1 1 d . . . B28 B 0.28002(6) 0.51806(15) 0.62231(6) 0.0167(3) Uani 1 1 d . . . C29 C 0.33510(5) 0.43594(14) 0.62439(5) 0.0182(3) Uani 1 1 d . . . C30 C 0.38528(6) 0.48995(16) 0.62646(6) 0.0258(3) Uani 1 1 d . . . H30 H 0.3878 0.5770 0.6262 0.031 Uiso 1 1 calc R . . C31 C 0.43165(6) 0.42057(19) 0.62889(7) 0.0340(4) Uani 1 1 d . . . H31 H 0.4644 0.4612 0.6304 0.041 Uiso 1 1 calc R . . C32 C 0.42970(6) 0.29253(18) 0.62911(6) 0.0307(4) Uani 1 1 d . . . H32 H 0.4609 0.2453 0.6311 0.037 Uiso 1 1 calc R . . C33 C 0.38102(6) 0.23494(16) 0.62640(6) 0.0275(3) Uani 1 1 d . . . H33 H 0.3789 0.1478 0.6263 0.033 Uiso 1 1 calc R . . C34 C 0.33521(6) 0.30564(15) 0.62388(5) 0.0229(3) Uani 1 1 d . . . H34 H 0.3026 0.2640 0.6217 0.028 Uiso 1 1 calc R . . C35 C 0.23042(5) 0.46277(13) 0.57896(5) 0.0171(3) Uani 1 1 d . . . C36 C 0.23973(6) 0.40934(14) 0.53646(5) 0.0203(3) Uani 1 1 d . . . H36 H 0.2751 0.4061 0.5326 0.024 Uiso 1 1 calc R . . C37 C 0.19910(6) 0.36066(14) 0.49953(5) 0.0227(3) Uani 1 1 d . . . H37 H 0.2075 0.3261 0.4717 0.027 Uiso 1 1 calc R . . C38 C 0.14640(6) 0.36312(15) 0.50375(5) 0.0241(3) Uani 1 1 d . . . H38 H 0.1189 0.3294 0.4793 0.029 Uiso 1 1 calc R . . C39 C 0.13530(6) 0.41645(15) 0.54485(6) 0.0251(3) Uani 1 1 d . . . H39 H 0.0998 0.4196 0.5483 0.030 Uiso 1 1 calc R . . C40 C 0.17637(6) 0.46571(14) 0.58134(5) 0.0213(3) Uani 1 1 d . . . H40 H 0.1675 0.5023 0.6086 0.026 Uiso 1 1 calc R . . C41 C 0.26137(5) 0.51043(13) 0.67405(5) 0.0168(3) Uani 1 1 d . . . C42 C 0.27619(6) 0.41502(14) 0.70845(5) 0.0199(3) Uani 1 1 d . . . H42 H 0.3011 0.3554 0.7035 0.024 Uiso 1 1 calc R . . C43 C 0.25539(7) 0.40538(15) 0.74963(6) 0.0255(3) Uani 1 1 d . . . H43 H 0.2664 0.3402 0.7718 0.031 Uiso 1 1 calc R . . C44 C 0.21854(6) 0.49119(15) 0.75811(6) 0.0248(3) Uani 1 1 d . . . H44 H 0.2042 0.4843 0.7857 0.030 Uiso 1 1 calc R . . C45 C 0.20301(6) 0.58767(15) 0.72524(5) 0.0226(3) Uani 1 1 d . . . H45 H 0.1780 0.6467 0.7305 0.027 Uiso 1 1 calc R . . C46 C 0.22456(6) 0.59645(14) 0.68473(5) 0.0200(3) Uani 1 1 d . . . H46 H 0.2140 0.6633 0.6633 0.024 Uiso 1 1 calc R . . C47 C 0.29425(6) 0.66144(14) 0.60985(5) 0.0187(3) Uani 1 1 d . . . C48 C 0.29390(6) 0.69863(14) 0.56216(5) 0.0197(3) Uani 1 1 d . . . H48 H 0.2790 0.6448 0.5364 0.024 Uiso 1 1 calc R . . C49 C 0.31458(6) 0.81150(15) 0.55138(6) 0.0237(3) Uani 1 1 d . . . H49 H 0.3135 0.8326 0.5189 0.028 Uiso 1 1 calc R . . C50 C 0.33678(7) 0.89303(15) 0.58852(6) 0.0260(3) Uani 1 1 d . . . H50 H 0.3514 0.9689 0.5815 0.031 Uiso 1 1 calc R . . C51 C 0.33713(7) 0.86125(16) 0.63611(6) 0.0287(3) Uani 1 1 d . . . H51 H 0.3517 0.9161 0.6616 0.034 Uiso 1 1 calc R . . C52 C 0.31588(7) 0.74821(15) 0.64617(6) 0.0258(3) Uani 1 1 d . . . H52 H 0.3160 0.7290 0.6786 0.031 Uiso 1 1 calc R . . C53 C 0.5000 0.7465(3) 0.7500 0.0598(9) Uani 1 2 d SD . . O54A O 0.5214(3) 0.7318(8) 0.7952(2) 0.086(2) Uiso 0.30 1 d PD A 1 C55A C 0.4925(5) 0.8569(8) 0.7242(3) 0.078(3) Uiso 0.30 1 d PD A 1 H55A H 0.5040 0.9258 0.7462 0.117 Uiso 0.30 1 calc PR A 1 H55B H 0.4549 0.8665 0.7086 0.117 Uiso 0.30 1 calc PR A 1 H55C H 0.5133 0.8557 0.6996 0.117 Uiso 0.30 1 calc PR A 1 C56A C 0.4830(3) 0.6401(7) 0.7134(3) 0.0416(17) Uiso 0.30 1 d PD A 1 H56A H 0.4917 0.5611 0.7298 0.062 Uiso 0.30 1 calc PR A 1 H56B H 0.5018 0.6475 0.6874 0.062 Uiso 0.30 1 calc PR A 1 H56C H 0.4448 0.6446 0.6998 0.062 Uiso 0.30 1 calc PR A 1 O54B O 0.5373(4) 0.8103(11) 0.7373(5) 0.102(4) Uiso 0.20 1 d PD A 2 C55B C 0.4956(6) 0.6171(8) 0.7263(5) 0.058(4) Uiso 0.20 1 d PD A 2 H55D H 0.5119 0.6187 0.6986 0.087 Uiso 0.20 1 calc PR A 2 H55E H 0.4582 0.5944 0.7155 0.087 Uiso 0.20 1 calc PR A 2 H55F H 0.5138 0.5567 0.7498 0.087 Uiso 0.20 1 calc PR A 2 C56B C 0.4509(5) 0.8174(16) 0.7225(7) 0.106(6) Uiso 0.20 1 d PD A 2 H56D H 0.4539 0.8324 0.6894 0.159 Uiso 0.20 1 calc PR A 2 H56E H 0.4485 0.8962 0.7385 0.159 Uiso 0.20 1 calc PR A 2 H56F H 0.4190 0.7688 0.7221 0.159 Uiso 0.20 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02050(10) 0.02708(13) 0.01899(10) 0.00234(9) 0.00511(8) -0.00313(9) N2 0.0236(6) 0.0385(8) 0.0223(6) -0.0001(6) 0.0030(5) -0.0029(6) C3 0.0336(9) 0.0466(12) 0.0287(8) -0.0102(8) 0.0033(7) -0.0059(8) C4 0.0306(8) 0.0330(10) 0.0367(9) -0.0090(8) 0.0040(7) -0.0013(7) N5 0.0214(6) 0.0263(7) 0.0327(7) 0.0022(6) 0.0060(5) 0.0005(5) C6 0.0204(7) 0.0287(9) 0.0521(11) 0.0051(8) 0.0081(7) -0.0027(6) C7 0.0237(8) 0.0327(10) 0.0534(11) 0.0077(8) 0.0157(8) 0.0009(7) N8 0.0259(7) 0.0262(7) 0.0350(8) 0.0063(6) 0.0070(6) 0.0040(5) C9 0.0382(9) 0.0294(9) 0.0432(10) 0.0018(8) 0.0151(8) 0.0111(7) C10 0.0435(10) 0.0355(10) 0.0320(9) 0.0019(8) 0.0184(8) 0.0118(8) N11 0.0264(6) 0.0258(7) 0.0227(6) 0.0002(5) 0.0093(5) 0.0009(5) C12 0.0223(7) 0.0499(11) 0.0196(7) 0.0039(7) 0.0052(6) 0.0060(7) C13 0.0199(7) 0.0429(10) 0.0276(8) 0.0132(7) 0.0084(6) 0.0068(7) C14 0.0170(6) 0.0361(9) 0.0298(8) 0.0113(7) 0.0042(6) 0.0004(6) C15 0.0240(8) 0.0358(10) 0.0428(10) 0.0122(8) 0.0057(7) 0.0000(7) C16 0.0301(9) 0.0389(11) 0.0626(13) 0.0254(10) 0.0129(9) 0.0025(8) C17 0.0390(10) 0.0557(14) 0.0574(13) 0.0330(11) 0.0249(10) 0.0103(10) C18 0.0351(9) 0.0610(14) 0.0371(10) 0.0222(10) 0.0193(8) 0.0120(9) O19 0.0446(7) 0.0331(7) 0.0227(6) 0.0046(5) 0.0060(5) -0.0123(6) C20 0.0256(7) 0.0280(8) 0.0193(7) -0.0007(6) 0.0062(6) -0.0033(6) C21 0.0192(7) 0.0304(9) 0.0237(7) 0.0004(6) 0.0016(5) -0.0007(6) C22 0.0156(6) 0.0350(9) 0.0268(7) -0.0020(7) 0.0044(5) -0.0020(6) C23 0.0299(9) 0.0556(13) 0.0410(10) -0.0033(9) 0.0158(8) 0.0099(8) C24 0.0396(11) 0.0588(15) 0.0641(14) 0.0020(12) 0.0166(10) 0.0250(10) C25 0.0488(12) 0.0646(16) 0.0511(13) 0.0182(11) 0.0112(10) 0.0305(11) C26 0.0348(9) 0.0474(12) 0.0316(9) 0.0076(8) 0.0054(7) 0.0107(8) O27 0.0208(5) 0.0439(7) 0.0234(5) 0.0021(5) 0.0084(4) -0.0010(5) B28 0.0177(6) 0.0163(7) 0.0165(7) -0.0004(6) 0.0049(5) -0.0010(5) C29 0.0172(6) 0.0229(7) 0.0151(6) -0.0007(5) 0.0050(5) -0.0005(5) C30 0.0203(7) 0.0272(8) 0.0299(8) 0.0075(6) 0.0059(6) -0.0023(6) C31 0.0168(7) 0.0488(12) 0.0372(9) 0.0126(8) 0.0077(6) -0.0009(7) C32 0.0224(7) 0.0462(11) 0.0251(8) 0.0031(7) 0.0084(6) 0.0122(7) C33 0.0270(7) 0.0278(8) 0.0267(8) -0.0060(6) 0.0041(6) 0.0071(6) C34 0.0187(6) 0.0239(8) 0.0257(7) -0.0053(6) 0.0041(5) 0.0003(5) C35 0.0194(6) 0.0137(6) 0.0183(6) 0.0014(5) 0.0045(5) 0.0006(5) C36 0.0211(6) 0.0198(7) 0.0204(7) -0.0006(5) 0.0058(5) 0.0002(5) C37 0.0285(7) 0.0203(7) 0.0184(6) -0.0009(5) 0.0040(5) -0.0003(6) C38 0.0241(7) 0.0216(8) 0.0230(7) 0.0016(6) -0.0019(6) -0.0022(6) C39 0.0179(6) 0.0270(8) 0.0290(8) 0.0026(6) 0.0026(6) 0.0030(6) C40 0.0200(6) 0.0229(7) 0.0210(7) 0.0001(6) 0.0049(5) 0.0034(5) C41 0.0169(6) 0.0170(7) 0.0168(6) -0.0018(5) 0.0046(5) -0.0026(5) C42 0.0218(6) 0.0187(7) 0.0191(6) 0.0002(5) 0.0043(5) 0.0006(5) C43 0.0334(8) 0.0226(8) 0.0209(7) 0.0038(6) 0.0072(6) -0.0022(6) C44 0.0295(7) 0.0279(8) 0.0204(7) -0.0013(6) 0.0127(6) -0.0065(6) C45 0.0226(7) 0.0235(8) 0.0240(7) -0.0043(6) 0.0103(6) -0.0007(6) C46 0.0231(7) 0.0187(7) 0.0195(6) 0.0010(5) 0.0072(5) 0.0014(5) C47 0.0207(6) 0.0183(7) 0.0186(6) -0.0005(5) 0.0079(5) 0.0003(5) C48 0.0224(7) 0.0191(7) 0.0186(6) -0.0006(5) 0.0066(5) 0.0016(5) C49 0.0296(7) 0.0232(8) 0.0210(7) 0.0045(6) 0.0115(6) 0.0031(6) C50 0.0342(8) 0.0171(7) 0.0317(8) 0.0001(6) 0.0175(7) -0.0017(6) C51 0.0417(9) 0.0223(8) 0.0265(8) -0.0081(6) 0.0167(7) -0.0087(7) C52 0.0372(8) 0.0244(8) 0.0190(7) -0.0029(6) 0.0127(6) -0.0073(7) C53 0.055(2) 0.045(2) 0.070(2) 0.000 -0.0039(17) 0.000 _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 O19 1.9132(13) . ? Fe1 O27 1.9343(12) . ? Fe1 N11 2.1349(14) . ? Fe1 N2 2.1386(14) . ? Fe1 N5 2.2094(14) . ? Fe1 N8 2.2202(14) . ? N2 C12 1.303(2) . ? N2 C3 1.491(2) . ? C3 C4 1.535(3) . ? C4 N5 1.494(2) . ? N5 C6 1.494(2) . ? C6 C7 1.525(3) . ? C7 N8 1.498(2) . ? N8 C9 1.501(2) . ? C9 C10 1.549(3) . ? C10 N11 1.489(2) . ? N11 C20 1.296(2) . ? C12 C13 1.448(3) . ? C13 C18 1.427(2) . ? C13 C14 1.433(2) . ? C14 O19 1.333(2) . ? C14 C15 1.418(3) . ? C15 C16 1.402(3) . ? C16 C17 1.395(3) . ? C17 C18 1.385(3) . ? C20 C21 1.455(2) . ? C21 C26 1.419(2) . ? C21 C22 1.429(2) . ? C22 O27 1.340(2) . ? C22 C23 1.416(3) . ? C23 C24 1.399(3) . ? C24 C25 1.401(3) . ? C25 C26 1.383(3) . ? B28 C41 1.660(2) . ? B28 C47 1.661(2) . ? B28 C29 1.677(2) . ? B28 C35 1.679(2) . ? C29 C34 1.418(2) . ? C29 C30 1.419(2) . ? C30 C31 1.410(2) . ? C31 C32 1.394(3) . ? C32 C33 1.397(2) . ? C33 C34 1.405(2) . ? C35 C36 1.416(2) . ? C35 C40 1.422(2) . ? C36 C37 1.412(2) . ? C37 C38 1.402(2) . ? C38 C39 1.398(2) . ? C39 C40 1.414(2) . ? C41 C42 1.420(2) . ? C41 C46 1.421(2) . ? C42 C43 1.407(2) . ? C43 C44 1.398(2) . ? C44 C45 1.404(2) . ? C45 C46 1.400(2) . ? C47 C48 1.419(2) . ? C47 C52 1.420(2) . ? C48 C49 1.403(2) . ? C49 C50 1.401(2) . ? C50 C51 1.401(2) . ? C51 C52 1.405(2) . ? C53 O54A 1.292(6) . ? C53 C55A 1.400(7) . ? C53 C56A 1.556(6) . ? C53 O54B 1.310(8) . ? C53 C56B 1.542(9) . ? C53 C55B 1.556(8) . ? 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 O19 Fe1 O27 106.22(6) . . ? O19 Fe1 N11 98.84(5) . . ? O27 Fe1 N11 86.69(5) . . ? O19 Fe1 N2 87.41(6) . . ? O27 Fe1 N2 93.39(5) . . ? N11 Fe1 N2 173.48(6) . . ? O19 Fe1 N5 158.05(5) . . ? O27 Fe1 N5 90.06(5) . . ? N11 Fe1 N5 96.67(5) . . ? N2 Fe1 N5 76.81(6) . . ? O19 Fe1 N8 90.52(6) . . ? O27 Fe1 N8 157.13(5) . . ? N11 Fe1 N8 75.20(5) . . ? N2 Fe1 N8 103.03(5) . . ? N5 Fe1 N8 78.53(5) . . ? C12 N2 C3 117.77(15) . . ? C12 N2 Fe1 125.29(13) . . ? C3 N2 Fe1 116.87(11) . . ? N2 C3 C4 108.89(14) . . ? N5 C4 C3 108.78(15) . . ? C4 N5 C6 113.22(13) . . ? C4 N5 Fe1 107.89(10) . . ? C6 N5 Fe1 110.30(10) . . ? N5 C6 C7 107.99(14) . . ? N8 C7 C6 108.29(14) . . ? C7 N8 C9 114.74(15) . . ? C7 N8 Fe1 109.08(10) . . ? C9 N8 Fe1 105.81(10) . . ? N8 C9 C10 109.29(14) . . ? N11 C10 C9 109.21(14) . . ? C20 N11 C10 117.29(14) . . ? C20 N11 Fe1 125.14(11) . . ? C10 N11 Fe1 116.96(10) . . ? N2 C12 C13 126.03(16) . . ? C18 C13 C14 118.95(18) . . ? C18 C13 C12 117.51(17) . . ? C14 C13 C12 123.49(15) . . ? O19 C14 C15 119.37(16) . . ? O19 C14 C13 122.00(16) . . ? C15 C14 C13 118.64(16) . . ? C16 C15 C14 120.5(2) . . ? C17 C16 C15 121.0(2) . . ? C18 C17 C16 119.72(18) . . ? C17 C18 C13 121.2(2) . . ? C14 O19 Fe1 134.85(12) . . ? N11 C20 C21 125.67(14) . . ? C26 C21 C22 119.65(16) . . ? C26 C21 C20 117.37(15) . . ? C22 C21 C20 122.97(14) . . ? O27 C22 C23 119.54(15) . . ? O27 C22 C21 122.39(15) . . ? C23 C22 C21 118.06(16) . . ? C24 C23 C22 120.76(18) . . ? C23 C24 C25 120.92(19) . . ? C26 C25 C24 119.32(19) . . ? C25 C26 C21 121.23(18) . . ? C22 O27 Fe1 130.03(10) . . ? C41 B28 C47 111.27(11) . . ? C41 B28 C29 111.32(11) . . ? C47 B28 C29 106.14(11) . . ? C41 B28 C35 107.87(11) . . ? C47 B28 C35 110.46(11) . . ? C29 B28 C35 109.80(11) . . ? C34 C29 C30 114.26(14) . . ? C34 C29 B28 122.43(12) . . ? C30 C29 B28 123.31(14) . . ? C31 C30 C29 123.13(16) . . ? C32 C31 C30 120.26(16) . . ? C31 C32 C33 118.77(15) . . ? C32 C33 C34 120.15(16) . . ? C33 C34 C29 123.41(15) . . ? C36 C35 C40 114.58(13) . . ? C36 C35 B28 121.70(12) . . ? C40 C35 B28 123.71(13) . . ? C37 C36 C35 123.26(14) . . ? C38 C37 C36 120.34(14) . . ? C39 C38 C37 118.34(13) . . ? C38 C39 C40 120.65(14) . . ? C39 C40 C35 122.81(14) . . ? C42 C41 C46 114.94(13) . . ? C42 C41 B28 124.36(13) . . ? C46 C41 B28 120.47(12) . . ? C43 C42 C41 122.54(14) . . ? C44 C43 C42 120.34(14) . . ? C43 C44 C45 119.11(14) . . ? C46 C45 C44 119.71(14) . . ? C45 C46 C41 123.34(14) . . ? C48 C47 C52 115.19(14) . . ? C48 C47 B28 121.41(13) . . ? C52 C47 B28 122.59(13) . . ? C49 C48 C47 122.84(14) . . ? C50 C49 C48 120.00(14) . . ? C51 C50 C49 119.19(15) . . ? C50 C51 C52 119.99(15) . . ? C51 C52 C47 122.75(14) . . ? O54A C53 C55A 127.5(6) . . ? O54A C53 C56A 124.7(6) . . ? C55A C53 C56A 107.5(5) . . ? O54B C53 C56B 99.9(8) . . ? O54B C53 C55B 110.1(7) . . ? C56B C53 C55B 105.2(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 31.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.753 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.060 #=END data_rpfe9bd _database_code_depnum_ccdc_archive 'CCDC 676636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(salicylaldiminato)-3,6-diazaoctane]iron(III) tetraphenylborate hemi-(1,2-dichloroethane) solvate ; _chemical_name_common ; (1,8-Bis(salicylaldiminato)-3,6-diazaoctane)iron(iii) tetraphenylborate hemi-(1,2-dichloroethane) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, C24 H20 B, 0.5[C2 H4 Cl2]' _chemical_formula_sum 'C45 H46 B Cl Fe N4 O2' _chemical_formula_weight 776.97 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.180(5) _cell_length_b 10.750(2) _cell_length_c 28.620(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.09(3) _cell_angle_gamma 90.00 _cell_volume 7876(3) _cell_formula_units_Z 8 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 46288 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.87 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 1.105 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46288 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.87 _reflns_number_total 12336 _reflns_number_gt 7881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one cation (Fe1-O27) and anion (B28-C52), and half a 1,2-dichloroethane molecule (C53-Cl54) spanning the C~2~ axis [1/2, y, 3/4]. No disorder was detected during refinement of this structure, and no restraints were applied. All non-H atoms were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. No hydrogen bonds are formed by the N---H groups N5 and N8 in the cation. ; _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^)+(0.0784P)^2^+18.5272P] 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 12336 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.603245(14) 0.51471(4) 0.616607(12) 0.02363(10) Uani 1 1 d . . . N2 N 0.61719(8) 0.5358(2) 0.69287(8) 0.0275(5) Uani 1 1 d . . . C3 C 0.64073(11) 0.6562(3) 0.71253(10) 0.0355(7) Uani 1 1 d . . . H3A H 0.6783 0.6444 0.7268 0.043 Uiso 1 1 calc R . . H3B H 0.6232 0.6862 0.7379 0.043 Uiso 1 1 calc R . . C4 C 0.63431(12) 0.7523(3) 0.67204(11) 0.0360(7) Uani 1 1 d . . . H4A H 0.5980 0.7837 0.6645 0.043 Uiso 1 1 calc R . . H4B H 0.6580 0.8236 0.6819 0.043 Uiso 1 1 calc R . . N5 N 0.64714(9) 0.6907(2) 0.62879(9) 0.0288(5) Uani 1 1 d . . . H5 H 0.6359 0.7422 0.6025 0.035 Uiso 1 1 calc R . . C6 C 0.70432(11) 0.6677(3) 0.63372(11) 0.0347(6) Uani 1 1 d . . . H6A H 0.7196 0.6366 0.6662 0.042 Uiso 1 1 calc R . . H6B H 0.7223 0.7458 0.6285 0.042 Uiso 1 1 calc R . . C7 C 0.71095(11) 0.5709(3) 0.59644(12) 0.0360(7) Uani 1 1 d . . . H7A H 0.6974 0.6038 0.5639 0.043 Uiso 1 1 calc R . . H7B H 0.7484 0.5504 0.5996 0.043 Uiso 1 1 calc R . . N8 N 0.68096(9) 0.4570(2) 0.60473(8) 0.0310(5) Uani 1 1 d . . . H8 H 0.6990 0.4159 0.6318 0.037 Uiso 1 1 calc R . . C9 C 0.67110(13) 0.3687(3) 0.56364(10) 0.0374(7) Uani 1 1 d . . . H9A H 0.6564 0.2901 0.5732 0.045 Uiso 1 1 calc R . . H9B H 0.7044 0.3492 0.5539 0.045 Uiso 1 1 calc R . . C10 C 0.63244(13) 0.4278(3) 0.52139(10) 0.0387(7) Uani 1 1 d . . . H10A H 0.6517 0.4786 0.5019 0.046 Uiso 1 1 calc R . . H10B H 0.6132 0.3618 0.5008 0.046 Uiso 1 1 calc R . . N11 N 0.59483(9) 0.5079(2) 0.54068(7) 0.0266(5) Uani 1 1 d . . . C12 C 0.60665(10) 0.4542(3) 0.72301(9) 0.0314(6) Uani 1 1 d . . . H12 H 0.6120 0.4788 0.7555 0.038 Uiso 1 1 calc R . . C13 C 0.58764(10) 0.3299(3) 0.71165(9) 0.0313(6) Uani 1 1 d . . . C14 C 0.57893(10) 0.2776(3) 0.66425(10) 0.0298(6) Uani 1 1 d . . . C15 C 0.56383(12) 0.1516(3) 0.65773(12) 0.0370(7) Uani 1 1 d . . . H15 H 0.5587 0.1153 0.6268 0.044 Uiso 1 1 calc R . . C16 C 0.55645(12) 0.0796(3) 0.69666(13) 0.0448(8) Uani 1 1 d . . . H16 H 0.5460 -0.0048 0.6918 0.054 Uiso 1 1 calc R . . C17 C 0.56429(13) 0.1308(4) 0.74289(13) 0.0502(9) Uani 1 1 d . . . H17 H 0.5590 0.0813 0.7690 0.060 Uiso 1 1 calc R . . C18 C 0.57967(12) 0.2530(4) 0.75011(11) 0.0425(8) Uani 1 1 d . . . H18 H 0.5851 0.2869 0.7814 0.051 Uiso 1 1 calc R . . O19 O 0.58452(8) 0.34518(19) 0.62639(6) 0.0331(4) Uani 1 1 d . . . C20 C 0.56379(11) 0.5770(3) 0.51033(9) 0.0288(6) Uani 1 1 d . . . H20 H 0.5657 0.5693 0.4777 0.035 Uiso 1 1 calc R . . C21 C 0.52619(10) 0.6653(3) 0.52171(9) 0.0276(5) Uani 1 1 d . . . C22 C 0.51576(10) 0.6790(3) 0.56881(9) 0.0260(5) Uani 1 1 d . . . C23 C 0.47986(12) 0.7720(3) 0.57630(11) 0.0382(7) Uani 1 1 d . . . H23 H 0.4725 0.7828 0.6072 0.046 Uiso 1 1 calc R . . C24 C 0.45530(14) 0.8477(4) 0.53874(12) 0.0505(9) Uani 1 1 d . . . H24 H 0.4321 0.9111 0.5445 0.061 Uiso 1 1 calc R . . C25 C 0.46437(15) 0.8314(4) 0.49198(13) 0.0561(11) Uani 1 1 d . . . H25 H 0.4466 0.8817 0.4664 0.067 Uiso 1 1 calc R . . C26 C 0.49912(13) 0.7420(3) 0.48401(11) 0.0417(8) Uani 1 1 d . . . H26 H 0.5052 0.7312 0.4527 0.050 Uiso 1 1 calc R . . O27 O 0.53848(7) 0.60724(19) 0.60536(6) 0.0291(4) Uani 1 1 d . . . B28 B 0.27836(10) 0.5227(3) 0.62110(9) 0.0184(5) Uani 1 1 d . . . C29 C 0.33364(9) 0.4426(2) 0.62239(8) 0.0202(5) Uani 1 1 d . . . C30 C 0.38270(10) 0.5012(2) 0.62525(9) 0.0239(5) Uani 1 1 d . . . H30 H 0.3843 0.5895 0.6263 0.029 Uiso 1 1 calc R . . C31 C 0.42945(10) 0.4341(3) 0.62660(9) 0.0271(5) Uani 1 1 d . . . H31 H 0.4614 0.4774 0.6284 0.032 Uiso 1 1 calc R . . C32 C 0.42873(10) 0.3045(3) 0.62530(9) 0.0278(5) Uani 1 1 d . . . H32 H 0.4600 0.2588 0.6264 0.033 Uiso 1 1 calc R . . C33 C 0.38098(10) 0.2426(3) 0.62232(9) 0.0259(5) Uani 1 1 d . . . H33 H 0.3798 0.1543 0.6215 0.031 Uiso 1 1 calc R . . C34 C 0.33488(10) 0.3111(2) 0.62059(9) 0.0237(5) Uani 1 1 d . . . H34 H 0.3030 0.2670 0.6181 0.028 Uiso 1 1 calc R . . C35 C 0.22953(10) 0.4656(2) 0.57910(8) 0.0206(5) Uani 1 1 d . . . C36 C 0.23873(10) 0.4086(2) 0.53688(8) 0.0214(5) Uani 1 1 d . . . H36 H 0.2736 0.4043 0.5324 0.026 Uiso 1 1 calc R . . C37 C 0.19860(10) 0.3582(2) 0.50133(9) 0.0245(5) Uani 1 1 d . . . H37 H 0.2069 0.3209 0.4738 0.029 Uiso 1 1 calc R . . C38 C 0.14683(11) 0.3626(2) 0.50636(9) 0.0263(5) Uani 1 1 d . . . H38 H 0.1198 0.3271 0.4828 0.032 Uiso 1 1 calc R . . C39 C 0.13533(10) 0.4206(3) 0.54709(9) 0.0275(5) Uani 1 1 d . . . H39 H 0.1002 0.4260 0.5509 0.033 Uiso 1 1 calc R . . C40 C 0.17623(10) 0.4709(2) 0.58244(9) 0.0244(5) Uani 1 1 d . . . H40 H 0.1676 0.5098 0.6096 0.029 Uiso 1 1 calc R . . C41 C 0.26035(9) 0.5150(2) 0.67345(8) 0.0189(4) Uani 1 1 d . . . C42 C 0.27543(10) 0.4189(2) 0.70736(8) 0.0216(5) Uani 1 1 d . . . H42 H 0.3000 0.3589 0.7016 0.026 Uiso 1 1 calc R . . C43 C 0.25544(11) 0.4084(2) 0.74939(9) 0.0263(5) Uani 1 1 d . . . H43 H 0.2672 0.3433 0.7715 0.032 Uiso 1 1 calc R . . C44 C 0.21846(11) 0.4937(3) 0.75858(9) 0.0280(6) Uani 1 1 d . . . H44 H 0.2046 0.4864 0.7866 0.034 Uiso 1 1 calc R . . C45 C 0.20221(10) 0.5901(2) 0.72586(9) 0.0249(5) Uani 1 1 d . . . H45 H 0.1769 0.6484 0.7315 0.030 Uiso 1 1 calc R . . C46 C 0.22326(10) 0.6007(2) 0.68477(8) 0.0224(5) Uani 1 1 d . . . H46 H 0.2123 0.6681 0.6636 0.027 Uiso 1 1 calc R . . C47 C 0.29113(9) 0.6685(2) 0.60759(8) 0.0198(4) Uani 1 1 d . . . C48 C 0.29268(10) 0.7015(2) 0.55964(8) 0.0220(5) Uani 1 1 d . . . H48 H 0.2794 0.6444 0.5347 0.026 Uiso 1 1 calc R . . C49 C 0.31313(10) 0.8156(2) 0.54778(9) 0.0248(5) Uani 1 1 d . . . H49 H 0.3138 0.8339 0.5154 0.030 Uiso 1 1 calc R . . C50 C 0.33246(10) 0.9022(2) 0.58377(9) 0.0250(5) Uani 1 1 d . . . H50 H 0.3466 0.9791 0.5761 0.030 Uiso 1 1 calc R . . C51 C 0.33068(10) 0.8741(2) 0.63140(9) 0.0245(5) Uani 1 1 d . . . H51 H 0.3434 0.9324 0.6560 0.029 Uiso 1 1 calc R . . C52 C 0.31009(10) 0.7593(2) 0.64261(8) 0.0228(5) Uani 1 1 d . . . H52 H 0.3089 0.7425 0.6750 0.027 Uiso 1 1 calc R . . C53 C 0.48950(13) 0.6530(3) 0.72327(11) 0.0422(7) Uani 1 1 d . . . H53A H 0.4694 0.5757 0.7140 0.051 Uiso 1 1 calc R . . H53B H 0.5191 0.6543 0.7067 0.051 Uiso 1 1 calc R . . Cl54 Cl 0.44821(4) 0.78499(11) 0.70474(3) 0.0599(3) Uani 1 1 d . . . 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 0.03031(19) 0.0275(2) 0.01437(16) 0.00309(14) 0.00767(13) 0.00037(15) N2 0.0283(10) 0.0365(13) 0.0174(10) -0.0001(9) 0.0043(8) 0.0053(9) C3 0.0333(14) 0.0459(18) 0.0266(13) -0.0103(13) 0.0049(11) 0.0022(13) C4 0.0355(14) 0.0346(16) 0.0373(16) -0.0087(13) 0.0059(12) 0.0043(12) N5 0.0314(11) 0.0252(12) 0.0311(12) 0.0033(9) 0.0099(9) 0.0042(9) C6 0.0286(13) 0.0327(16) 0.0444(17) 0.0075(13) 0.0114(12) -0.0017(11) C7 0.0316(14) 0.0382(17) 0.0433(17) 0.0125(14) 0.0192(12) 0.0055(12) N8 0.0391(12) 0.0302(13) 0.0267(11) 0.0073(10) 0.0136(10) 0.0081(10) C9 0.0541(18) 0.0304(16) 0.0305(14) 0.0031(12) 0.0154(13) 0.0149(13) C10 0.0549(18) 0.0395(18) 0.0252(14) 0.0015(12) 0.0165(13) 0.0177(14) N11 0.0379(12) 0.0276(12) 0.0163(9) 0.0015(8) 0.0103(8) 0.0047(9) C12 0.0302(13) 0.0497(18) 0.0155(11) 0.0051(11) 0.0073(10) 0.0121(12) C13 0.0274(12) 0.0471(18) 0.0220(12) 0.0119(12) 0.0110(10) 0.0095(12) C14 0.0283(12) 0.0365(16) 0.0252(13) 0.0116(11) 0.0069(10) 0.0018(11) C15 0.0357(15) 0.0351(17) 0.0394(16) 0.0087(13) 0.0063(12) -0.0005(12) C16 0.0369(16) 0.0398(19) 0.060(2) 0.0224(16) 0.0147(15) 0.0020(13) C17 0.0446(18) 0.062(2) 0.049(2) 0.0307(18) 0.0218(15) 0.0056(16) C18 0.0398(16) 0.063(2) 0.0290(15) 0.0214(15) 0.0175(12) 0.0124(15) O19 0.0492(12) 0.0330(11) 0.0173(8) 0.0052(8) 0.0073(8) -0.0070(9) C20 0.0390(14) 0.0311(15) 0.0176(11) 0.0004(10) 0.0088(10) -0.0007(11) C21 0.0304(13) 0.0335(15) 0.0192(11) 0.0022(10) 0.0060(9) 0.0001(11) C22 0.0271(12) 0.0324(15) 0.0194(11) 0.0015(10) 0.0072(9) -0.0003(10) C23 0.0380(15) 0.053(2) 0.0269(14) 0.0029(13) 0.0140(12) 0.0106(14) C24 0.0516(19) 0.064(2) 0.0402(18) 0.0126(17) 0.0186(15) 0.0289(18) C25 0.062(2) 0.074(3) 0.0346(17) 0.0230(18) 0.0143(16) 0.036(2) C26 0.0466(17) 0.057(2) 0.0229(13) 0.0128(14) 0.0102(12) 0.0141(15) O27 0.0336(10) 0.0391(11) 0.0164(8) 0.0052(8) 0.0097(7) 0.0023(8) B28 0.0270(12) 0.0166(12) 0.0127(10) -0.0003(9) 0.0063(9) -0.0008(10) C29 0.0275(11) 0.0228(12) 0.0114(9) -0.0011(8) 0.0065(8) -0.0007(9) C30 0.0311(12) 0.0225(13) 0.0184(11) 0.0000(9) 0.0062(9) -0.0018(10) C31 0.0268(12) 0.0345(15) 0.0213(12) 0.0013(11) 0.0082(9) -0.0016(11) C32 0.0292(12) 0.0367(15) 0.0185(11) -0.0021(10) 0.0072(9) 0.0065(11) C33 0.0349(13) 0.0226(13) 0.0206(11) -0.0033(10) 0.0071(10) 0.0051(10) C34 0.0295(12) 0.0235(13) 0.0186(11) -0.0005(9) 0.0065(9) -0.0013(10) C35 0.0305(12) 0.0182(12) 0.0137(10) 0.0027(8) 0.0057(9) 0.0012(9) C36 0.0270(11) 0.0214(12) 0.0169(10) 0.0020(9) 0.0071(9) 0.0005(9) C37 0.0366(13) 0.0206(13) 0.0164(11) 0.0001(9) 0.0054(9) 0.0016(10) C38 0.0357(13) 0.0219(13) 0.0189(11) 0.0014(10) 0.0003(10) -0.0017(10) C39 0.0287(12) 0.0303(15) 0.0227(12) 0.0038(10) 0.0038(10) 0.0021(10) C40 0.0313(12) 0.0238(13) 0.0189(11) -0.0002(10) 0.0073(9) 0.0026(10) C41 0.0269(11) 0.0172(11) 0.0134(9) -0.0012(8) 0.0059(8) -0.0020(9) C42 0.0309(12) 0.0206(12) 0.0142(10) -0.0001(9) 0.0072(9) -0.0008(9) C43 0.0429(14) 0.0217(13) 0.0157(10) 0.0023(9) 0.0093(10) -0.0040(11) C44 0.0404(14) 0.0301(15) 0.0170(11) -0.0019(10) 0.0139(10) -0.0065(11) C45 0.0314(12) 0.0246(13) 0.0213(11) -0.0035(10) 0.0118(10) -0.0020(10) C46 0.0313(12) 0.0204(12) 0.0166(10) 0.0005(9) 0.0079(9) 0.0006(10) C47 0.0264(11) 0.0206(12) 0.0138(10) 0.0006(9) 0.0074(8) 0.0020(9) C48 0.0304(12) 0.0223(12) 0.0148(10) 0.0000(9) 0.0081(9) 0.0024(10) C49 0.0362(13) 0.0245(13) 0.0152(10) 0.0045(9) 0.0093(9) 0.0029(10) C50 0.0380(14) 0.0184(12) 0.0215(11) 0.0016(9) 0.0130(10) 0.0000(10) C51 0.0356(13) 0.0221(13) 0.0178(11) -0.0026(9) 0.0105(10) 0.0005(10) C52 0.0344(13) 0.0222(12) 0.0139(10) 0.0007(9) 0.0101(9) 0.0010(10) C53 0.0434(17) 0.052(2) 0.0324(15) -0.0050(14) 0.0102(13) -0.0041(15) Cl54 0.0498(5) 0.0945(8) 0.0360(4) 0.0183(5) 0.0102(4) 0.0198(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O19 1.923(2) . ? Fe1 O27 1.934(2) . ? Fe1 N11 2.139(2) . ? Fe1 N2 2.148(2) . ? Fe1 N5 2.203(2) . ? Fe1 N8 2.220(2) . ? N2 C12 1.300(4) . ? N2 C3 1.492(4) . ? C3 C4 1.535(5) . ? C4 N5 1.502(4) . ? N5 C6 1.495(4) . ? C6 C7 1.526(4) . ? C7 N8 1.500(4) . ? N8 C9 1.491(4) . ? C9 C10 1.542(4) . ? C10 N11 1.498(3) . ? N11 C20 1.293(3) . ? C12 C13 1.439(5) . ? C13 C18 1.427(4) . ? C13 C14 1.442(4) . ? C14 O19 1.338(3) . ? C14 C15 1.413(4) . ? C15 C16 1.403(4) . ? C16 C17 1.408(5) . ? C17 C18 1.377(6) . ? C20 C21 1.453(4) . ? C21 C26 1.423(4) . ? C21 C22 1.438(3) . ? C22 O27 1.335(3) . ? C22 C23 1.419(4) . ? C23 C24 1.393(5) . ? C24 C25 1.418(5) . ? C25 C26 1.375(5) . ? B28 C47 1.664(4) . ? B28 C41 1.664(3) . ? B28 C29 1.677(4) . ? B28 C35 1.677(4) . ? C29 C34 1.415(4) . ? C29 C30 1.417(3) . ? C30 C31 1.414(4) . ? C31 C32 1.394(4) . ? C32 C33 1.403(4) . ? C33 C34 1.406(4) . ? C35 C36 1.419(3) . ? C35 C40 1.420(3) . ? C36 C37 1.409(4) . ? C37 C38 1.394(4) . ? C38 C39 1.409(4) . ? C39 C40 1.417(4) . ? C41 C42 1.416(3) . ? C41 C46 1.424(3) . ? C42 C43 1.413(3) . ? C43 C44 1.398(4) . ? C44 C45 1.402(4) . ? C45 C46 1.404(3) . ? C47 C52 1.413(3) . ? C47 C48 1.427(3) . ? C48 C49 1.408(4) . ? C49 C50 1.402(4) . ? C50 C51 1.406(3) . ? C51 C52 1.410(4) . ? C53 C53 1.513(6) 2_656 ? C53 Cl54 1.795(4) . ? 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 O19 Fe1 O27 105.69(9) . . ? O19 Fe1 N11 98.06(9) . . ? O27 Fe1 N11 87.04(8) . . ? O19 Fe1 N2 86.93(9) . . ? O27 Fe1 N2 94.09(8) . . ? N11 Fe1 N2 174.40(9) . . ? O19 Fe1 N5 158.64(9) . . ? O27 Fe1 N5 89.70(9) . . ? N11 Fe1 N5 97.44(9) . . ? N2 Fe1 N5 77.09(9) . . ? O19 Fe1 N8 91.55(9) . . ? O27 Fe1 N8 156.63(8) . . ? N11 Fe1 N8 74.79(9) . . ? N2 Fe1 N8 102.64(9) . . ? N5 Fe1 N8 78.46(9) . . ? C12 N2 C3 117.6(2) . . ? C12 N2 Fe1 126.0(2) . . ? C3 N2 Fe1 116.33(18) . . ? N2 C3 C4 109.1(2) . . ? N5 C4 C3 108.5(2) . . ? C6 N5 C4 112.8(2) . . ? C6 N5 Fe1 110.57(17) . . ? C4 N5 Fe1 108.03(17) . . ? N5 C6 C7 107.8(2) . . ? N8 C7 C6 107.8(2) . . ? C9 N8 C7 113.9(2) . . ? C9 N8 Fe1 106.61(18) . . ? C7 N8 Fe1 108.82(17) . . ? N8 C9 C10 109.5(2) . . ? N11 C10 C9 108.8(2) . . ? C20 N11 C10 116.9(2) . . ? C20 N11 Fe1 125.42(18) . . ? C10 N11 Fe1 117.28(17) . . ? N2 C12 C13 126.0(3) . . ? C18 C13 C12 117.6(3) . . ? C18 C13 C14 118.7(3) . . ? C12 C13 C14 123.6(2) . . ? O19 C14 C15 119.2(3) . . ? O19 C14 C13 121.9(3) . . ? C15 C14 C13 118.9(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 120.9(3) . . ? C18 C17 C16 119.6(3) . . ? C17 C18 C13 121.5(3) . . ? C14 O19 Fe1 134.98(19) . . ? N11 C20 C21 125.8(2) . . ? C26 C21 C22 119.3(3) . . ? C26 C21 C20 117.5(2) . . ? C22 C21 C20 123.2(2) . . ? O27 C22 C23 119.3(2) . . ? O27 C22 C21 122.3(2) . . ? C23 C22 C21 118.4(2) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 121.0(3) . . ? C26 C25 C24 119.4(3) . . ? C25 C26 C21 121.4(3) . . ? C22 O27 Fe1 131.22(16) . . ? C47 B28 C41 111.37(18) . . ? C47 B28 C29 105.89(19) . . ? C41 B28 C29 111.13(19) . . ? C47 B28 C35 109.77(19) . . ? C41 B28 C35 108.04(18) . . ? C29 B28 C35 110.64(19) . . ? C34 C29 C30 114.7(2) . . ? C34 C29 B28 122.5(2) . . ? C30 C29 B28 122.7(2) . . ? C31 C30 C29 122.9(2) . . ? C32 C31 C30 120.2(2) . . ? C31 C32 C33 118.9(2) . . ? C32 C33 C34 120.1(3) . . ? C33 C34 C29 123.3(2) . . ? C36 C35 C40 114.8(2) . . ? C36 C35 B28 121.9(2) . . ? C40 C35 B28 123.3(2) . . ? C37 C36 C35 123.2(2) . . ? C38 C37 C36 120.4(2) . . ? C37 C38 C39 118.8(2) . . ? C38 C39 C40 119.9(2) . . ? C39 C40 C35 122.9(2) . . ? C42 C41 C46 114.9(2) . . ? C42 C41 B28 124.2(2) . . ? C46 C41 B28 120.5(2) . . ? C43 C42 C41 122.8(2) . . ? C44 C43 C42 120.2(2) . . ? C43 C44 C45 119.0(2) . . ? C44 C45 C46 120.1(2) . . ? C45 C46 C41 123.0(2) . . ? C52 C47 C48 115.7(2) . . ? C52 C47 B28 122.9(2) . . ? C48 C47 B28 120.4(2) . . ? C49 C48 C47 122.5(2) . . ? C50 C49 C48 119.9(2) . . ? C49 C50 C51 119.3(2) . . ? C50 C51 C52 120.0(2) . . ? C51 C52 C47 122.5(2) . . ? C53 C53 Cl54 111.56(18) 2_656 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.87 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.230 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.105 #=END data_rp9palm _database_code_depnum_ccdc_archive 'CCDC 676637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,8-Bis(salicylaldiminato)-3,6-diazaoctane]iron(III) perchlorate ; _chemical_name_common ;(1,8-Bis(salicylaldiminato)-3,6-diazaoctane)iron(iii) perchlorate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Fe N4 O2, Cl O4' _chemical_formula_sum 'C20 H24 Cl Fe N4 O6' _chemical_formula_weight 507.73 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8864(15) _cell_length_b 13.7970(11) _cell_length_c 27.951(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.881(5) _cell_angle_gamma 90.00 _cell_volume 6773.8(10) _cell_formula_units_Z 12 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 88858 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 29.72 _exptl_crystal_description Needle _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3156 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 4 kW. ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88858 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 29.72 _reflns_number_total 18991 _reflns_number_gt 10875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. This is isostructural with the previously reported structure of this compound (Inorg. Chim. Acta 2005, 358, 437). However, this early paper wrongly describes the structure as having Z = 4; in fact, Z = 12. The asymmetric unit contains two wholly occupied complex cation (Fe1A-O27A and Fe1B-O27B); one disordered cation site containing two complete partial molecules, Fe1C-O27C and Fe1D-O27D; and, three disordered perchlorate anions. The disordered cation sites were modelled using the following restraints; C---C = 1.52(2), C---N = C=N = 1.47(2), NC---C(aryl) = 1.45(2), C---O = 1.33(2), 1,3-C...N = 2.46(2), 1,3-C...C = 2.40(2) (not including phenyl groups), 1,3-C(aryl)...O = 2.46(2) 1,3-NC...C(aryl) = 2.47(2)\%A, and with all phenyl rings refined as rigid hexagons. The occupancy ratio of the 'C' and 'D' cations refined to 0.49:0.51, so these were modelled as equally occupied in the final least squares cycles. While the errors on the bond lengths to Fe1C and Fe1D are higher, the Fe---N and Fe---O distances in these molecules imply that cation C has a high-spin structure while cation 'D' is a low-spin structure. Therefore, this cation site seems to exist as a mixture of spin states at the temperature of measurement. Perchlorate anions Cl28-O32 and Cl38-O42 are disordered over two sites, labelled 'A' and 'B'. In both cases, the 'A' and 'B' sites of each anion refined to be equally occupied within experimental error. The third anion, Cl33-O37, is disordered over three equally occupied sites. All Cl---O bonds were restrained to the refined value of 1.45(2)\%A, and O...O distances within each partial anion to 2.37(2)\%A. The following atoms were refined anisotropically: all fully occupied non-H atoms in cations A and B; the half-occupied Fe, N and O atoms in half-cations C and D; the half-occupied Cl atoms Cl28A and Cl28B; and, the complete half-anions Cl38A-O42A and Cl38B-O42B. All non-H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak of +1.0 e.\%A^-3^ is 1.4\%A from Fe1C. ; _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^)+(0.0757P)^2^+22.3027P] 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 18991 _refine_ls_number_parameters 927 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2180 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.62454(4) 0.26550(5) 0.59135(3) 0.03515(19) Uani 1 1 d . . . N2A N 0.5359(3) 0.2266(3) 0.62743(15) 0.0366(10) Uani 1 1 d . . . C3A C 0.5081(4) 0.3029(4) 0.6569(2) 0.0495(15) Uani 1 1 d . . . H3A1 H 0.5312 0.2947 0.6917 0.059 Uiso 1 1 calc R . . H3A2 H 0.4521 0.2988 0.6534 0.059 Uiso 1 1 calc R . . C4A C 0.5308(4) 0.4010(4) 0.6384(2) 0.0543(17) Uani 1 1 d . . . H4A1 H 0.4982 0.4163 0.6066 0.065 Uiso 1 1 calc R . . H4A2 H 0.5241 0.4528 0.6618 0.065 Uiso 1 1 calc R . . N5A N 0.6118(3) 0.3957(3) 0.63325(16) 0.0560(15) Uani 1 1 d . . . H5A H 0.6224 0.4492 0.6154 0.067 Uiso 1 1 calc R . . C6A C 0.6651(6) 0.3971(6) 0.6815(3) 0.084(3) Uani 1 1 d . . . H6A1 H 0.6711 0.4644 0.6940 0.101 Uiso 1 1 calc R . . H6A2 H 0.6437 0.3575 0.7053 0.101 Uiso 1 1 calc R . . C7A C 0.7377(6) 0.3592(7) 0.6765(3) 0.091(3) Uani 1 1 d . . . H7A1 H 0.7713 0.3534 0.7088 0.109 Uiso 1 1 calc R . . H7A2 H 0.7623 0.4030 0.6560 0.109 Uiso 1 1 calc R . . N8A N 0.7245(3) 0.2596(5) 0.6525(2) 0.074(2) Uani 1 1 d . . . H8A H 0.7147 0.2150 0.6756 0.089 Uiso 1 1 calc R . . C9A C 0.7895(4) 0.2229(7) 0.6301(3) 0.084(3) Uani 1 1 d . . . H9A1 H 0.7802 0.1548 0.6195 0.101 Uiso 1 1 calc R . . H9A2 H 0.8377 0.2258 0.6542 0.101 Uiso 1 1 calc R . . C10A C 0.7947(3) 0.2867(5) 0.5865(3) 0.0614(19) Uani 1 1 d . . . H10A H 0.8150 0.3513 0.5977 0.074 Uiso 1 1 calc R . . H10B H 0.8295 0.2571 0.5670 0.074 Uiso 1 1 calc R . . N11A N 0.7170(2) 0.2966(3) 0.55648(17) 0.0380(10) Uani 1 1 d . . . C12A C 0.4991(3) 0.1453(4) 0.62287(19) 0.0387(12) Uani 1 1 d . . . H12A H 0.4576 0.1395 0.6395 0.046 Uiso 1 1 calc R . . C13A C 0.5151(3) 0.0637(4) 0.5953(2) 0.0498(15) Uani 1 1 d . . . C14A C 0.5795(4) 0.0591(5) 0.5729(3) 0.077(3) Uani 1 1 d . . . C15A C 0.5922(7) -0.0256(6) 0.5479(5) 0.164(7) Uani 1 1 d . . . H15A H 0.6354 -0.0297 0.5327 0.197 Uiso 1 1 calc R . . C16A C 0.5422(8) -0.1039(8) 0.5452(7) 0.234(11) Uani 1 1 d . . . H16A H 0.5527 -0.1615 0.5290 0.281 Uiso 1 1 calc R . . C17A C 0.4764(6) -0.0991(6) 0.5659(4) 0.125(5) Uani 1 1 d . . . H17A H 0.4409 -0.1510 0.5623 0.150 Uiso 1 1 calc R . . C18A C 0.4652(4) -0.0171(5) 0.5914(3) 0.074(2) Uani 1 1 d . . . H18A H 0.4226 -0.0143 0.6071 0.089 Uiso 1 1 calc R . . O19A O 0.6290(2) 0.1324(3) 0.5744(2) 0.0688(14) Uani 1 1 d . . . C20A C 0.7111(3) 0.3133(3) 0.5106(2) 0.0336(11) Uani 1 1 d . . . H20A H 0.7572 0.3165 0.4984 0.040 Uiso 1 1 calc R . . C21A C 0.6412(2) 0.3278(3) 0.47574(17) 0.0272(9) Uani 1 1 d . . . C22A C 0.5684(2) 0.3349(3) 0.49025(17) 0.0294(10) Uani 1 1 d . . . C23A C 0.5041(3) 0.3546(4) 0.45329(18) 0.0353(11) Uani 1 1 d . . . H23A H 0.4557 0.3629 0.4620 0.042 Uiso 1 1 calc R . . C24A C 0.5105(3) 0.3618(4) 0.40471(19) 0.0397(12) Uani 1 1 d . . . H24A H 0.4662 0.3732 0.3807 0.048 Uiso 1 1 calc R . . C25A C 0.5818(3) 0.3526(4) 0.39035(18) 0.0391(12) Uani 1 1 d . . . H25A H 0.5858 0.3567 0.3570 0.047 Uiso 1 1 calc R . . C26A C 0.6453(3) 0.3376(4) 0.42581(19) 0.0345(11) Uani 1 1 d . . . H26A H 0.6936 0.3335 0.4165 0.041 Uiso 1 1 calc R . . O27A O 0.55960(19) 0.3227(3) 0.53585(12) 0.0382(8) Uani 1 1 d . . . Fe1B Fe 0.75206(5) 0.66473(5) 0.80034(3) 0.0392(2) Uani 1 1 d . . . N2B N 0.7537(4) 0.8060(3) 0.80023(18) 0.0669(18) Uani 1 1 d . . . C3B C 0.7815(8) 0.8511(5) 0.7583(3) 0.114(4) Uani 1 1 d . . . H3B1 H 0.8370 0.8627 0.7666 0.137 Uiso 1 1 calc R . . H3B2 H 0.7555 0.9137 0.7494 0.137 Uiso 1 1 calc R . . C4B C 0.7628(7) 0.7792(5) 0.7162(2) 0.102(4) Uani 1 1 d . . . H4B1 H 0.7079 0.7826 0.7018 0.123 Uiso 1 1 calc R . . H4B2 H 0.7920 0.7958 0.6906 0.123 Uiso 1 1 calc R . . N5B N 0.7827(4) 0.6788(4) 0.73452(18) 0.0641(17) Uani 1 1 d . . . H5B H 0.7529 0.6361 0.7133 0.077 Uiso 1 1 calc R . . C6B C 0.8638(4) 0.6500(7) 0.7373(3) 0.085(3) Uani 1 1 d . . . H6B1 H 0.8850 0.6843 0.7118 0.102 Uiso 1 1 calc R . . H6B2 H 0.8667 0.5795 0.7315 0.102 Uiso 1 1 calc R . . C7B C 0.9104(5) 0.6750(7) 0.7875(3) 0.089(3) Uani 1 1 d . . . H7B1 H 0.9581 0.6369 0.7935 0.106 Uiso 1 1 calc R . . H7B2 H 0.9239 0.7447 0.7887 0.106 Uiso 1 1 calc R . . N8B N 0.8650(3) 0.6528(4) 0.82641(18) 0.0522(14) Uani 1 1 d . . . H8B H 0.8778 0.6987 0.8509 0.063 Uiso 1 1 calc R . . C9B C 0.8794(3) 0.5554(4) 0.8492(2) 0.0522(17) Uani 1 1 d . . . H9B1 H 0.8653 0.5556 0.8818 0.063 Uiso 1 1 calc R . . H9B2 H 0.9341 0.5393 0.8533 0.063 Uiso 1 1 calc R . . C10B C 0.8321(3) 0.4798(4) 0.8168(2) 0.0480(15) Uani 1 1 d . . . H10C H 0.8542 0.4663 0.7876 0.058 Uiso 1 1 calc R . . H10D H 0.8297 0.4184 0.8349 0.058 Uiso 1 1 calc R . . N11B N 0.7547(2) 0.5236(3) 0.80276(16) 0.0322(9) Uani 1 1 d . . . C12B C 0.7337(5) 0.8620(4) 0.8329(2) 0.071(2) Uani 1 1 d . . . H12B H 0.7370 0.9300 0.8284 0.086 Uiso 1 1 calc R . . C13B C 0.7068(4) 0.8289(4) 0.8755(2) 0.0505(15) Uani 1 1 d . . . C14B C 0.7068(3) 0.7295(4) 0.88859(17) 0.0356(11) Uani 1 1 d . . . C15B C 0.6778(3) 0.7059(5) 0.93114(19) 0.0441(13) Uani 1 1 d . . . H15B H 0.6766 0.6401 0.9410 0.053 Uiso 1 1 calc R . . C16B C 0.6513(3) 0.7778(7) 0.9585(2) 0.067(2) Uani 1 1 d . . . H16B H 0.6314 0.7600 0.9865 0.080 Uiso 1 1 calc R . . C17B C 0.6534(4) 0.8751(7) 0.9461(3) 0.083(3) Uani 1 1 d . . . H17B H 0.6360 0.9237 0.9654 0.100 Uiso 1 1 calc R . . C18B C 0.6809(5) 0.8994(5) 0.9052(3) 0.075(2) Uani 1 1 d . . . H18B H 0.6827 0.9658 0.8965 0.090 Uiso 1 1 calc R . . O19B O 0.7326(2) 0.6580(2) 0.86428(12) 0.0348(8) Uani 1 1 d . . . C20B C 0.6955(2) 0.4690(3) 0.80049(19) 0.0323(10) Uani 1 1 d . . . H20B H 0.7037 0.4028 0.8093 0.039 Uiso 1 1 calc R . . C21B C 0.6177(3) 0.5013(4) 0.78557(18) 0.0331(11) Uani 1 1 d . . . C22B C 0.5986(3) 0.5973(4) 0.76873(17) 0.0383(12) Uani 1 1 d . . . C23B C 0.5202(4) 0.6159(5) 0.7499(2) 0.0572(19) Uani 1 1 d . . . H23B H 0.5055 0.6784 0.7373 0.069 Uiso 1 1 calc R . . C24B C 0.4649(4) 0.5462(7) 0.7493(2) 0.066(2) Uani 1 1 d . . . H24B H 0.4131 0.5621 0.7371 0.080 Uiso 1 1 calc R . . C25B C 0.4836(3) 0.4530(6) 0.7663(2) 0.0594(19) Uani 1 1 d . . . H25B H 0.4452 0.4051 0.7657 0.071 Uiso 1 1 calc R . . C26B C 0.5594(3) 0.4313(5) 0.7841(2) 0.0484(15) Uani 1 1 d . . . H26B H 0.5727 0.3677 0.7957 0.058 Uiso 1 1 calc R . . O27B O 0.6491(2) 0.6680(3) 0.76911(13) 0.0445(9) Uani 1 1 d . . . Fe1C Fe 0.98341(7) 0.79255(10) 0.58917(5) 0.0224(3) Uani 0.50 1 d P A 1 N2C N 0.9590(4) 0.8618(6) 0.5196(3) 0.0235(16) Uani 0.50 1 d PD A 1 C3C C 0.8782(4) 0.8602(7) 0.4939(3) 0.0264(18) Uiso 0.50 1 d PD A 1 H3C1 H 0.8723 0.8160 0.4655 0.032 Uiso 0.50 1 calc PR A 1 H3C2 H 0.8620 0.9259 0.4821 0.032 Uiso 0.50 1 calc PR A 1 C4C C 0.8298(5) 0.8250(6) 0.5298(3) 0.0282(18) Uiso 0.50 1 d PD A 1 H4C1 H 0.8220 0.8785 0.5519 0.034 Uiso 0.50 1 calc PR A 1 H4C2 H 0.7793 0.8040 0.5118 0.034 Uiso 0.50 1 calc PR A 1 N5C N 0.8687(4) 0.7427(5) 0.5585(3) 0.0262(15) Uani 0.50 1 d PD A 1 H5C H 0.8435 0.7299 0.5840 0.031 Uiso 0.50 1 calc PR A 1 C6C C 0.8701(6) 0.6518(7) 0.5297(4) 0.031(2) Uiso 0.50 1 d PD A 1 H6C1 H 0.8805 0.6670 0.4970 0.037 Uiso 0.50 1 calc PR A 1 H6C2 H 0.8204 0.6183 0.5258 0.037 Uiso 0.50 1 calc PR A 1 C7C C 0.9343(5) 0.5866(7) 0.5583(4) 0.031(2) Uiso 0.50 1 d PD A 1 H7C1 H 0.9225 0.5682 0.5903 0.038 Uiso 0.50 1 calc PR A 1 H7C2 H 0.9398 0.5267 0.5397 0.038 Uiso 0.50 1 calc PR A 1 N8C N 1.0065(4) 0.6454(6) 0.5651(3) 0.0289(16) Uani 0.50 1 d PD A 1 H8C H 1.0228 0.6495 0.5355 0.035 Uiso 0.50 1 calc PR A 1 C9C C 1.0683(5) 0.6029(7) 0.6020(3) 0.032(2) Uiso 0.50 1 d PD A 1 H9C1 H 1.1173 0.6343 0.6000 0.038 Uiso 0.50 1 calc PR A 1 H9C2 H 1.0729 0.5328 0.5957 0.038 Uiso 0.50 1 calc PR A 1 C10C C 1.0503(5) 0.6181(6) 0.6529(3) 0.031(2) Uiso 0.50 1 d PD A 1 H10E H 1.0122 0.5699 0.6590 0.037 Uiso 0.50 1 calc PR A 1 H10F H 1.0971 0.6093 0.6779 0.037 Uiso 0.50 1 calc PR A 1 N11C N 1.0204(4) 0.7164(6) 0.6561(3) 0.0229(16) Uani 0.50 1 d PD A 1 C12C C 1.0090(4) 0.9005(7) 0.4970(3) 0.0247(17) Uiso 0.50 1 d PD A 1 H12C H 0.9901 0.9290 0.4661 0.030 Uiso 0.50 1 calc PR A 1 C13C C 1.0912(2) 0.9045(5) 0.5145(2) 0.0294(19) Uiso 0.50 1 d PGD A 1 C14C C 1.1266(3) 0.8696(5) 0.5597(2) 0.0286(19) Uiso 0.50 1 d PGD A 1 C15C C 1.2055(3) 0.8714(5) 0.5729(2) 0.034(2) Uiso 0.50 1 d PGD A 1 H15C H 1.2297 0.8476 0.6039 0.041 Uiso 0.50 1 calc PR A 1 C16C C 1.2491(2) 0.9083(5) 0.5408(3) 0.039(2) Uiso 0.50 1 d PG A 1 H16C H 1.3030 0.9096 0.5498 0.047 Uiso 0.50 1 calc PR A 1 C17C C 1.2137(3) 0.9432(6) 0.4956(2) 0.049(3) Uiso 0.50 1 d PG A 1 H17C H 1.2434 0.9684 0.4736 0.058 Uiso 0.50 1 calc PR A 1 C18C C 1.1348(3) 0.9413(5) 0.4824(2) 0.044(3) Uiso 0.50 1 d PGD A 1 H18C H 1.1106 0.9652 0.4514 0.053 Uiso 0.50 1 calc PR A 1 O19C O 1.0863(8) 0.8353(14) 0.5932(4) 0.038(3) Uani 0.50 1 d PD A 1 C20C C 1.0325(5) 0.7604(6) 0.6981(3) 0.0242(17) Uiso 0.50 1 d PD A 1 H20C H 1.0631 0.7284 0.7249 0.029 Uiso 0.50 1 calc PR A 1 C21C C 1.0018(4) 0.8571(4) 0.7066(2) 0.038(2) Uiso 0.50 1 d PGD A 1 C22C C 0.9525(4) 0.9124(4) 0.67293(17) 0.0291(19) Uiso 0.50 1 d PGD A 1 C23C C 0.9217(4) 0.9974(4) 0.6876(2) 0.039(2) Uiso 0.50 1 d PGD A 1 H23C H 0.8881 1.0352 0.6645 0.047 Uiso 0.50 1 calc PR A 1 C24C C 0.9403(4) 1.0272(4) 0.7359(2) 0.042(2) Uiso 0.50 1 d PG A 1 H24C H 0.9192 1.0853 0.7459 0.050 Uiso 0.50 1 calc PR A 1 C25C C 0.9895(4) 0.9719(5) 0.76954(17) 0.045(3) Uiso 0.50 1 d PG A 1 H25C H 1.0022 0.9922 0.8025 0.054 Uiso 0.50 1 calc PR A 1 C26C C 1.0203(4) 0.8868(5) 0.7549(2) 0.038(2) Uiso 0.50 1 d PGD A 1 H26C H 1.0540 0.8490 0.7779 0.045 Uiso 0.50 1 calc PR A 1 O27C O 0.9403(3) 0.8825(4) 0.6322(3) 0.0187(17) Uani 0.50 1 d PD A 1 Fe1D Fe 0.98861(7) 0.76075(10) 0.56518(5) 0.0209(3) Uani 0.50 1 d P B 2 N2D N 0.9567(4) 0.8225(6) 0.5021(3) 0.0248(17) Uani 0.50 1 d PD B 2 C3D C 0.8743(5) 0.8109(7) 0.4847(4) 0.034(2) Uiso 0.50 1 d PD B 2 H3D1 H 0.8610 0.8250 0.4493 0.041 Uiso 0.50 1 calc PR B 2 H3D2 H 0.8456 0.8558 0.5021 0.041 Uiso 0.50 1 calc PR B 2 C4D C 0.8546(6) 0.7040(7) 0.4948(4) 0.044(3) Uiso 0.50 1 d PD B 2 H4D1 H 0.7988 0.6960 0.4911 0.053 Uiso 0.50 1 calc PR B 2 H4D2 H 0.8730 0.6601 0.4714 0.053 Uiso 0.50 1 calc PR B 2 N5D N 0.8926(5) 0.6804(7) 0.5454(3) 0.037(2) Uani 0.50 1 d PD B 2 H5D H 0.8594 0.6928 0.5666 0.045 Uiso 0.50 1 calc PR B 2 C6D C 0.9136(6) 0.5770(8) 0.5480(5) 0.039(3) Uiso 0.50 1 d PD B 2 H6D1 H 0.8711 0.5378 0.5300 0.047 Uiso 0.50 1 calc PR B 2 H6D2 H 0.9238 0.5555 0.5825 0.047 Uiso 0.50 1 calc PR B 2 C7D C 0.9839(5) 0.5618(7) 0.5262(4) 0.041(2) Uiso 0.50 1 d PD B 2 H7D1 H 1.0084 0.4996 0.5378 0.049 Uiso 0.50 1 calc PR B 2 H7D2 H 0.9694 0.5589 0.4902 0.049 Uiso 0.50 1 calc PR B 2 N8D N 1.0381(5) 0.6426(5) 0.5405(3) 0.0320(18) Uani 0.50 1 d PD B 2 H8D H 1.0572 0.6612 0.5131 0.038 Uiso 0.50 1 calc PR B 2 C9D C 1.1036(5) 0.6133(8) 0.5791(3) 0.036(2) Uiso 0.50 1 d PD B 2 H9D1 H 1.1457 0.6605 0.5810 0.043 Uiso 0.50 1 calc PR B 2 H9D2 H 1.1225 0.5486 0.5717 0.043 Uiso 0.50 1 calc PR B 2 C10D C 1.0748(5) 0.6106(7) 0.6269(3) 0.0292(19) Uiso 0.50 1 d PD B 2 H10G H 1.0433 0.5522 0.6285 0.035 Uiso 0.50 1 calc PR B 2 H10H H 1.1181 0.6096 0.6548 0.035 Uiso 0.50 1 calc PR B 2 N11D N 1.0282(4) 0.7003(5) 0.6282(3) 0.0222(15) Uani 0.50 1 d PD B 2 C12D C 0.9990(4) 0.8674(7) 0.4766(3) 0.0251(18) Uiso 0.50 1 d PD B 2 H12D H 0.9755 0.8933 0.4460 0.030 Uiso 0.50 1 calc PR B 2 C13D C 1.0819(2) 0.8807(4) 0.49239(19) 0.0224(17) Uiso 0.50 1 d PGD B 2 C14D C 1.1198(3) 0.8609(4) 0.53951(17) 0.0225(17) Uiso 0.50 1 d PGD B 2 C15D C 1.1982(3) 0.8734(4) 0.55187(16) 0.0233(17) Uiso 0.50 1 d PGD B 2 H15D H 1.2241 0.8598 0.5841 0.028 Uiso 0.50 1 calc PR B 2 C16D C 1.2387(2) 0.9056(4) 0.5171(2) 0.0225(17) Uiso 0.50 1 d PG B 2 H16D H 1.2923 0.9141 0.5256 0.027 Uiso 0.50 1 calc PR B 2 C17D C 1.2008(3) 0.9254(5) 0.46998(19) 0.035(2) Uiso 0.50 1 d PG B 2 H17D H 1.2285 0.9474 0.4462 0.041 Uiso 0.50 1 calc PR B 2 C18D C 1.1224(3) 0.9130(5) 0.45762(16) 0.031(2) Uiso 0.50 1 d PGD B 2 H18D H 1.0965 0.9265 0.4254 0.037 Uiso 0.50 1 calc PR B 2 O19D O 1.0836(7) 0.8289(13) 0.5757(3) 0.025(2) Uani 0.50 1 d PD B 2 C20D C 1.0317(5) 0.7436(6) 0.6700(4) 0.017(2) Uiso 0.50 1 d PD B 2 H20D H 1.0626 0.7160 0.6980 0.021 Uiso 0.50 1 calc PR B 2 C21D C 0.9897(4) 0.8337(4) 0.6755(2) 0.0230(17) Uiso 0.50 1 d PGD B 2 C22D C 0.9372(4) 0.8798(5) 0.63968(17) 0.110(12) Uiso 0.50 1 d PGD B 2 C23D C 0.8947(4) 0.9571(5) 0.6519(2) 0.040(2) Uiso 0.50 1 d PGD B 2 H23D H 0.8588 0.9886 0.6274 0.048 Uiso 0.50 1 calc PR B 2 C24D C 0.9045(4) 0.9883(4) 0.7000(2) 0.039(2) Uiso 0.50 1 d PG B 2 H24D H 0.8754 1.0411 0.7084 0.047 Uiso 0.50 1 calc PR B 2 C25D C 0.9569(4) 0.9422(5) 0.73582(18) 0.036(2) Uiso 0.50 1 d PG B 2 H25D H 0.9637 0.9635 0.7687 0.043 Uiso 0.50 1 calc PR B 2 C26D C 0.9995(3) 0.8649(4) 0.72357(19) 0.0241(18) Uiso 0.50 1 d PGD B 2 H26D H 1.0354 0.8334 0.7481 0.029 Uiso 0.50 1 calc PR B 2 O27D O 0.9339(3) 0.8547(5) 0.5962(2) 0.0346(16) Uani 0.50 1 d PD B 2 Cl28A Cl 0.7223(5) 0.6165(8) 0.6081(3) 0.0302(14) Uani 0.50 1 d PD C 1 O29A O 0.6807(5) 0.6172(7) 0.6480(3) 0.036(2) Uiso 0.50 1 d PD C 1 O30A O 0.8032(4) 0.6158(6) 0.6285(3) 0.0359(17) Uiso 0.50 1 d PD C 1 O31A O 0.7076(5) 0.7049(6) 0.5797(3) 0.048(2) Uiso 0.50 1 d PD C 1 O32A O 0.6957(6) 0.5378(7) 0.5744(4) 0.053(3) Uiso 0.50 1 d PD C 1 Cl28B Cl 0.7357(5) 0.6031(8) 0.6026(4) 0.0367(17) Uani 0.50 1 d PD D 2 O29B O 0.6823(5) 0.6035(7) 0.6364(3) 0.040(3) Uiso 0.50 1 d PD D 2 O30B O 0.8082(5) 0.5739(7) 0.6284(3) 0.051(2) Uiso 0.50 1 d PD D 2 O31B O 0.7380(8) 0.6954(8) 0.5798(5) 0.089(4) Uiso 0.50 1 d PD D 2 O32B O 0.7126(7) 0.5271(9) 0.5673(4) 0.078(4) Uiso 0.50 1 d PD D 2 Cl33A Cl 0.7418(2) 0.1753(4) 0.78052(16) 0.0206(12) Uiso 0.34 1 d PD E 1 O34A O 0.7904(6) 0.2494(8) 0.8128(5) 0.039(3) Uiso 0.34 1 d PD E 1 O35A O 0.7795(8) 0.1382(11) 0.7474(4) 0.060(4) Uiso 0.34 1 d PD E 1 O36A O 0.6681(6) 0.2253(11) 0.7656(7) 0.022(4) Uiso 0.34 1 d PD E 1 O37A O 0.7278(6) 0.1014(7) 0.8177(4) 0.026(2) Uiso 0.34 1 d PD E 1 Cl33B Cl 0.7377(3) 0.1858(4) 0.7896(3) 0.0171(12) Uiso 0.33 1 d PD F 2 O34B O 0.7651(6) 0.2409(7) 0.8340(4) 0.037(2) Uiso 0.33 1 d PD F 2 O35B O 0.7990(6) 0.1945(10) 0.7605(4) 0.049(3) Uiso 0.33 1 d PD F 2 O36B O 0.6698(8) 0.2191(13) 0.7588(6) 0.045(8) Uiso 0.33 1 d PD F 2 O37B O 0.7326(7) 0.0848(8) 0.8007(5) 0.049(4) Uiso 0.33 1 d PD F 2 Cl33C Cl 0.7430(4) 0.1720(6) 0.7958(3) 0.046(2) Uiso 0.33 1 d PD G 3 O34C O 0.7981(6) 0.2465(8) 0.7936(5) 0.044(3) Uiso 0.33 1 d PD G 3 O35C O 0.7451(10) 0.1119(11) 0.7490(5) 0.083(5) Uiso 0.33 1 d PD G 3 O36C O 0.6657(6) 0.2175(10) 0.7842(5) 0.057(4) Uiso 0.33 1 d PD G 3 O37C O 0.7518(9) 0.1116(10) 0.8345(5) 0.069(5) Uiso 0.33 1 d PD G 3 Cl38A Cl 1.00168(12) 0.69030(17) 0.41098(12) 0.0253(5) Uani 0.50 1 d PD H 1 O39A O 0.9194(5) 0.6819(10) 0.4049(4) 0.053(3) Uani 0.50 1 d PD H 1 O40A O 1.0303(4) 0.6198(5) 0.3798(3) 0.0378(17) Uani 0.50 1 d PD H 1 O41A O 1.0202(5) 0.7870(5) 0.3971(3) 0.035(2) Uani 0.50 1 d PD H 1 O42A O 1.0363(4) 0.6733(6) 0.4617(3) 0.0396(17) Uani 0.50 1 d PD H 1 Cl38B Cl 1.00382(13) 0.67479(19) 0.38548(11) 0.0246(5) Uani 0.50 1 d PD I 2 O39B O 0.9217(5) 0.6650(9) 0.3811(4) 0.046(3) Uani 0.50 1 d PD I 2 O40B O 1.0313(5) 0.6086(5) 0.3525(3) 0.042(2) Uani 0.50 1 d PD I 2 O41B O 1.0209(5) 0.7738(6) 0.3739(3) 0.0307(18) Uani 0.50 1 d PD I 2 O42B O 1.0407(4) 0.6524(5) 0.4351(3) 0.0337(16) Uani 0.50 1 d PD I 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 Fe1A 0.0322(4) 0.0329(4) 0.0376(4) 0.0040(3) -0.0004(3) -0.0158(3) N2A 0.053(3) 0.027(2) 0.029(2) -0.0019(17) 0.0072(18) -0.0116(19) C3A 0.092(5) 0.027(3) 0.032(3) -0.008(2) 0.017(3) -0.015(3) C4A 0.099(5) 0.029(3) 0.036(3) -0.006(2) 0.014(3) -0.018(3) N5A 0.092(4) 0.035(3) 0.032(2) 0.008(2) -0.013(2) -0.035(3) C6A 0.132(8) 0.055(4) 0.049(4) 0.011(3) -0.028(5) -0.056(5) C7A 0.108(7) 0.091(6) 0.058(5) 0.019(4) -0.024(5) -0.068(6) N8A 0.059(3) 0.078(4) 0.073(4) 0.044(3) -0.019(3) -0.024(3) C9A 0.036(3) 0.106(7) 0.098(6) 0.060(5) -0.016(4) -0.002(4) C10A 0.028(3) 0.072(5) 0.074(4) 0.032(4) -0.015(3) -0.012(3) N11A 0.0206(18) 0.037(2) 0.052(3) 0.015(2) -0.0028(17) -0.0108(17) C12A 0.050(3) 0.028(3) 0.042(3) -0.005(2) 0.021(2) -0.015(2) C13A 0.050(3) 0.033(3) 0.076(4) -0.021(3) 0.037(3) -0.017(3) C14A 0.069(4) 0.046(4) 0.136(7) -0.041(4) 0.071(5) -0.031(3) C15A 0.169(10) 0.066(6) 0.321(17) -0.106(8) 0.208(12) -0.070(6) C16A 0.234(14) 0.099(8) 0.46(3) -0.182(12) 0.302(17) -0.119(9) C17A 0.119(7) 0.070(5) 0.224(12) -0.093(7) 0.129(8) -0.067(5) C18A 0.069(4) 0.052(4) 0.120(6) -0.047(4) 0.064(4) -0.035(3) O19A 0.051(3) 0.038(2) 0.130(4) -0.017(3) 0.050(3) -0.022(2) C20A 0.023(2) 0.025(2) 0.053(3) 0.003(2) 0.008(2) -0.0049(18) C21A 0.026(2) 0.021(2) 0.035(2) -0.0023(18) 0.0059(18) -0.0071(17) C22A 0.024(2) 0.030(2) 0.033(2) -0.004(2) 0.0018(18) -0.0039(18) C23A 0.023(2) 0.044(3) 0.037(3) -0.003(2) 0.0022(19) -0.003(2) C24A 0.034(3) 0.046(3) 0.036(3) 0.006(2) -0.001(2) -0.007(2) C25A 0.044(3) 0.044(3) 0.030(2) 0.000(2) 0.007(2) -0.015(2) C26A 0.032(2) 0.030(3) 0.044(3) -0.002(2) 0.015(2) -0.009(2) O27A 0.0287(17) 0.060(2) 0.0256(16) -0.0025(16) 0.0046(13) -0.0070(16) Fe1B 0.0671(5) 0.0210(3) 0.0375(4) -0.0061(3) 0.0307(4) -0.0097(3) N2B 0.149(6) 0.025(2) 0.035(3) -0.002(2) 0.037(3) -0.018(3) C3B 0.260(13) 0.043(4) 0.057(5) -0.009(3) 0.072(6) -0.059(6) C4B 0.230(12) 0.050(4) 0.040(4) -0.008(3) 0.061(5) -0.051(6) N5B 0.107(5) 0.052(3) 0.044(3) -0.021(2) 0.044(3) -0.043(3) C6B 0.092(5) 0.116(7) 0.064(4) -0.053(4) 0.059(4) -0.071(5) C7B 0.094(5) 0.114(7) 0.077(5) -0.062(5) 0.064(4) -0.080(5) N8B 0.060(3) 0.049(3) 0.059(3) -0.033(2) 0.042(3) -0.035(2) C9B 0.026(2) 0.050(4) 0.084(4) -0.038(3) 0.019(3) -0.013(2) C10B 0.020(2) 0.044(3) 0.081(4) -0.029(3) 0.012(2) -0.003(2) N11B 0.0257(19) 0.025(2) 0.051(2) -0.0106(18) 0.0181(17) -0.0028(16) C12B 0.148(8) 0.020(3) 0.044(4) 0.000(3) 0.012(4) 0.005(4) C13B 0.081(4) 0.034(3) 0.034(3) -0.005(2) 0.006(3) 0.025(3) C14B 0.041(3) 0.038(3) 0.030(2) 0.001(2) 0.009(2) 0.020(2) C15B 0.031(3) 0.068(4) 0.035(3) 0.003(3) 0.010(2) 0.016(3) C16B 0.042(3) 0.121(7) 0.039(3) -0.015(4) 0.011(3) 0.038(4) C17B 0.081(5) 0.110(7) 0.051(4) -0.036(4) -0.005(4) 0.069(5) C18B 0.108(6) 0.053(4) 0.054(4) -0.016(3) -0.010(4) 0.049(4) O19B 0.050(2) 0.0252(17) 0.0342(18) 0.0031(14) 0.0209(15) 0.0107(15) C20B 0.024(2) 0.021(2) 0.054(3) 0.006(2) 0.013(2) 0.0010(18) C21B 0.023(2) 0.039(3) 0.039(3) 0.010(2) 0.0112(19) 0.010(2) C22B 0.052(3) 0.041(3) 0.025(2) 0.007(2) 0.016(2) 0.020(3) C23B 0.068(4) 0.072(4) 0.029(3) 0.002(3) 0.003(3) 0.050(4) C24B 0.035(3) 0.118(7) 0.044(3) -0.001(4) 0.003(3) 0.038(4) C25B 0.021(2) 0.105(6) 0.053(4) 0.018(4) 0.009(2) 0.006(3) C26B 0.024(2) 0.062(4) 0.059(4) 0.026(3) 0.008(2) 0.001(2) O27B 0.079(3) 0.0271(19) 0.0308(18) 0.0059(15) 0.0178(18) 0.0143(19) Fe1C 0.0221(6) 0.0207(6) 0.0247(7) 0.0037(6) 0.0051(5) -0.0019(5) N2C 0.028(4) 0.018(4) 0.027(4) -0.002(3) 0.010(3) 0.000(3) N5C 0.025(4) 0.020(4) 0.035(4) 0.003(3) 0.012(3) -0.003(3) N8C 0.028(4) 0.028(4) 0.034(4) 0.007(3) 0.012(3) -0.002(3) N11C 0.026(4) 0.020(4) 0.023(5) 0.001(4) 0.006(4) -0.003(3) O19C 0.023(4) 0.045(7) 0.044(7) 0.024(8) 0.000(5) -0.008(4) O27C 0.016(3) 0.011(3) 0.031(3) -0.012(2) 0.007(2) 0.003(2) Fe1D 0.0173(5) 0.0259(7) 0.0203(6) -0.0004(5) 0.0060(5) -0.0038(5) N2D 0.019(3) 0.030(5) 0.027(4) -0.008(4) 0.007(3) 0.003(3) N5D 0.029(4) 0.056(6) 0.028(5) 0.003(4) 0.007(4) -0.012(5) N8D 0.047(5) 0.020(4) 0.032(4) -0.004(3) 0.013(4) -0.008(3) N11D 0.027(4) 0.022(4) 0.020(4) 0.002(3) 0.010(3) -0.002(3) O19D 0.021(4) 0.027(4) 0.025(5) 0.009(5) 0.003(4) -0.002(3) O27D 0.020(3) 0.038(4) 0.048(4) 0.020(3) 0.012(3) 0.015(3) Cl28A 0.026(2) 0.033(3) 0.029(3) 0.0042(19) 0.0008(19) -0.0107(18) Cl28B 0.043(4) 0.033(3) 0.036(2) -0.0003(17) 0.012(2) -0.014(2) Cl38A 0.0216(10) 0.0233(12) 0.0313(13) 0.0036(11) 0.0056(10) 0.0044(8) O39A 0.018(4) 0.058(7) 0.085(9) 0.014(7) 0.012(5) -0.002(4) O40A 0.050(5) 0.028(4) 0.037(5) -0.016(4) 0.010(4) 0.008(4) O41A 0.041(4) 0.019(4) 0.043(5) 0.007(4) 0.003(5) 0.006(3) O42A 0.054(5) 0.035(4) 0.031(4) 0.008(3) 0.012(4) 0.003(3) Cl38B 0.0257(11) 0.0238(13) 0.0242(12) 0.0031(10) 0.0042(10) 0.0005(9) O39B 0.028(4) 0.041(6) 0.070(7) 0.027(6) 0.010(5) 0.001(4) O40B 0.068(5) 0.035(4) 0.027(4) -0.015(4) 0.015(4) 0.006(4) O41B 0.029(4) 0.026(4) 0.038(5) 0.004(4) 0.009(4) 0.000(3) O42B 0.051(5) 0.030(4) 0.020(3) 0.002(3) 0.006(3) 0.005(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 Fe1A O19A 1.902(4) . ? Fe1A O27A 1.923(3) . ? Fe1A N2A 2.103(4) . ? Fe1A N11A 2.115(4) . ? Fe1A N5A 2.180(5) . ? Fe1A N8A 2.230(5) . ? N2A C12A 1.294(6) . ? N2A C3A 1.479(7) . ? C3A C4A 1.530(8) . ? C4A N5A 1.486(9) . ? N5A C6A 1.498(8) . ? C6A C7A 1.432(13) . ? C7A N8A 1.527(11) . ? N8A C9A 1.510(11) . ? C9A C10A 1.519(9) . ? C10A N11A 1.489(6) . ? N11A C20A 1.288(7) . ? C12A C13A 1.425(7) . ? C13A C14A 1.412(8) . ? C13A C18A 1.419(8) . ? C14A O19A 1.339(7) . ? C14A C15A 1.401(9) . ? C15A C16A 1.396(11) . ? C16A C17A 1.408(10) . ? C17A C18A 1.373(9) . ? C20A C21A 1.447(6) . ? C21A C26A 1.418(7) . ? C21A C22A 1.438(6) . ? C22A O27A 1.324(6) . ? C22A C23A 1.419(6) . ? C23A C24A 1.388(7) . ? C24A C25A 1.414(7) . ? C25A C26A 1.374(7) . ? Fe1B O27B 1.884(4) . ? Fe1B O19B 1.886(3) . ? Fe1B N11B 1.948(4) . ? Fe1B N2B 1.950(5) . ? Fe1B N8B 2.020(5) . ? Fe1B N5B 2.026(5) . ? N2B C12B 1.297(8) . ? N2B C3B 1.492(8) . ? C3B C4B 1.527(10) . ? C4B N5B 1.495(10) . ? N5B C6B 1.491(10) . ? C6B C7B 1.530(10) . ? C7B N8B 1.506(7) . ? N8B C9B 1.488(9) . ? C9B C10B 1.528(7) . ? C10B N11B 1.494(6) . ? N11B C20B 1.292(6) . ? C12B C13B 1.440(9) . ? C13B C18B 1.412(8) . ? C13B C14B 1.420(8) . ? C14B O19B 1.330(6) . ? C14B C15B 1.421(7) . ? C15B C16B 1.390(8) . ? C16B C17B 1.389(12) . ? C17B C18B 1.369(12) . ? C20B C21B 1.446(6) . ? C21B C26B 1.415(7) . ? C21B C22B 1.426(7) . ? C22B O27B 1.327(7) . ? C22B C23B 1.426(8) . ? C23B C24B 1.377(11) . ? C24B C25B 1.390(11) . ? C25B C26B 1.387(7) . ? Fe1C O19C 1.915(13) . ? Fe1C O27C 1.983(6) . ? Fe1C N2C 2.136(8) . ? Fe1C N11C 2.138(8) . ? Fe1C N5C 2.181(7) . ? Fe1C N8C 2.202(8) . ? N2C C12C 1.302(10) . ? N2C C3C 1.488(10) . ? C3C C4C 1.522(10) . ? C4C N5C 1.486(10) . ? N5C C6C 1.493(11) . ? C6C C7C 1.557(12) . ? C7C N8C 1.507(11) . ? N8C C9C 1.483(10) . ? C9C C10C 1.530(11) . ? C10C N11C 1.467(11) . ? N11C C20C 1.303(11) . ? C12C C13C 1.461(8) . ? C13C C14C 1.3900 . ? C13C C18C 1.3900 . ? C14C O19C 1.370(10) . ? C14C C15C 1.3900 . ? C15C C16C 1.3900 . ? C16C C17C 1.3900 . ? C17C C18C 1.3900 . ? C20C C21C 1.478(8) . ? C21C C22C 1.3900 . ? C21C C26C 1.3900 . ? C22C O27C 1.191(8) . ? C22C C23C 1.3900 . ? C23C C24C 1.3900 . ? C24C C25C 1.3900 . ? C25C C26C 1.3900 . ? Fe1D O19D 1.916(13) . ? Fe1D O27D 1.926(7) . ? Fe1D N2D 1.943(8) . ? Fe1D N11D 1.957(8) . ? Fe1D N5D 2.032(9) . ? Fe1D N8D 2.037(8) . ? N2D C12D 1.293(10) . ? N2D C3D 1.471(10) . ? C3D C4D 1.555(12) . ? C4D N5D 1.485(11) . ? N5D C6D 1.474(12) . ? C6D C7D 1.513(12) . ? C7D N8D 1.481(11) . ? N8D C9D 1.490(11) . ? C9D C10D 1.521(11) . ? C10D N11D 1.496(10) . ? N11D C20D 1.302(10) . ? C12D C13D 1.476(8) . ? C13D C14D 1.3900 . ? C13D C18D 1.3900 . ? C14D O19D 1.372(9) . ? C14D C15D 1.3900 . ? C15D C16D 1.3900 . ? C16D C17D 1.3900 . ? C17D C18D 1.3900 . ? C20D C21D 1.477(9) . ? C21D C22D 1.3900 . ? C21D C26D 1.3900 . ? C22D O27D 1.255(8) . ? C22D C23D 1.3900 . ? C23D C24D 1.3900 . ? C24D C25D 1.3900 . ? C25D C26D 1.3900 . ? Cl28A O31A 1.451(12) . ? Cl28A O30A 1.452(10) . ? Cl28A O29A 1.454(11) . ? Cl28A O32A 1.457(12) . ? Cl28B O30B 1.417(12) . ? Cl28B O31B 1.428(13) . ? Cl28B O32B 1.447(13) . ? Cl28B O29B 1.464(10) . ? Cl33A O35A 1.346(11) . ? Cl33A O36A 1.475(10) . ? Cl33A O37A 1.510(10) . ? Cl33A O34A 1.523(10) . ? Cl33B O36B 1.426(12) . ? Cl33B O37B 1.434(11) . ? Cl33B O34B 1.460(11) . ? Cl33B O35B 1.487(11) . ? Cl33C O37C 1.351(12) . ? Cl33C O34C 1.433(11) . ? Cl33C O36C 1.498(12) . ? Cl33C O35C 1.554(13) . ? Cl38A O41A 1.445(8) . ? Cl38A O42A 1.454(7) . ? Cl38A O39A 1.454(9) . ? Cl38A O40A 1.462(7) . ? Cl38B O40B 1.447(7) . ? Cl38B O41B 1.450(8) . ? Cl38B O42B 1.453(7) . ? Cl38B O39B 1.457(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O19A Fe1A O27A 104.1(2) . . ? O19A Fe1A N2A 86.80(17) . . ? O27A Fe1A N2A 95.52(16) . . ? O19A Fe1A N11A 90.46(18) . . ? O27A Fe1A N11A 87.16(15) . . ? N2A Fe1A N11A 176.55(17) . . ? O19A Fe1A N5A 160.6(2) . . ? O27A Fe1A N5A 89.23(17) . . ? N2A Fe1A N5A 77.76(18) . . ? N11A Fe1A N5A 104.49(19) . . ? O19A Fe1A N8A 95.2(2) . . ? O27A Fe1A N8A 155.25(19) . . ? N2A Fe1A N8A 101.0(2) . . ? N11A Fe1A N8A 77.2(2) . . ? N5A Fe1A N8A 76.6(2) . . ? C12A N2A C3A 117.0(5) . . ? C12A N2A Fe1A 126.1(4) . . ? C3A N2A Fe1A 116.7(3) . . ? N2A C3A C4A 107.7(5) . . ? N5A C4A C3A 108.4(5) . . ? C4A N5A C6A 112.2(6) . . ? C4A N5A Fe1A 107.2(3) . . ? C6A N5A Fe1A 112.4(5) . . ? C7A C6A N5A 109.9(7) . . ? C6A C7A N8A 107.7(6) . . ? C9A N8A C7A 114.6(7) . . ? C9A N8A Fe1A 105.2(4) . . ? C7A N8A Fe1A 109.8(5) . . ? N8A C9A C10A 107.9(6) . . ? N11A C10A C9A 108.2(5) . . ? C20A N11A C10A 118.0(5) . . ? C20A N11A Fe1A 124.9(3) . . ? C10A N11A Fe1A 116.7(4) . . ? N2A C12A C13A 126.0(5) . . ? C14A C13A C18A 119.1(5) . . ? C14A C13A C12A 122.7(5) . . ? C18A C13A C12A 118.3(5) . . ? O19A C14A C15A 118.5(6) . . ? O19A C14A C13A 122.8(5) . . ? C15A C14A C13A 118.7(6) . . ? C16A C15A C14A 120.6(7) . . ? C15A C16A C17A 121.2(7) . . ? C18A C17A C16A 117.9(7) . . ? C17A C18A C13A 122.4(6) . . ? C14A O19A Fe1A 132.7(4) . . ? N11A C20A C21A 126.4(4) . . ? C26A C21A C22A 119.2(4) . . ? C26A C21A C20A 118.5(4) . . ? C22A C21A C20A 122.2(4) . . ? O27A C22A C23A 119.9(4) . . ? O27A C22A C21A 122.8(4) . . ? C23A C22A C21A 117.4(4) . . ? C24A C23A C22A 121.4(5) . . ? C23A C24A C25A 121.1(5) . . ? C26A C25A C24A 118.4(5) . . ? C25A C26A C21A 122.4(5) . . ? C22A O27A Fe1A 131.7(3) . . ? O27B Fe1B O19B 95.81(16) . . ? O27B Fe1B N11B 93.15(16) . . ? O19B Fe1B N11B 85.72(16) . . ? O27B Fe1B N2B 89.4(2) . . ? O19B Fe1B N2B 93.24(17) . . ? N11B Fe1B N2B 177.3(2) . . ? O27B Fe1B N8B 172.92(16) . . ? O19B Fe1B N8B 90.28(17) . . ? N11B Fe1B N8B 83.67(18) . . ? N2B Fe1B N8B 93.9(3) . . ? O27B Fe1B N5B 89.2(2) . . ? O19B Fe1B N5B 174.3(2) . . ? N11B Fe1B N5B 96.8(2) . . ? N2B Fe1B N5B 84.0(2) . . ? N8B Fe1B N5B 84.9(2) . . ? C12B N2B C3B 118.8(6) . . ? C12B N2B Fe1B 126.0(4) . . ? C3B N2B Fe1B 115.2(4) . . ? N2B C3B C4B 106.1(5) . . ? N5B C4B C3B 109.6(6) . . ? C6B N5B C4B 115.6(6) . . ? C6B N5B Fe1B 110.7(4) . . ? C4B N5B Fe1B 108.1(4) . . ? N5B C6B C7B 110.1(5) . . ? N8B C7B C6B 109.9(5) . . ? C9B N8B C7B 114.8(6) . . ? C9B N8B Fe1B 108.0(3) . . ? C7B N8B Fe1B 111.2(5) . . ? N8B C9B C10B 109.3(5) . . ? N11B C10B C9B 105.1(4) . . ? C20B N11B C10B 119.1(4) . . ? C20B N11B Fe1B 124.6(3) . . ? C10B N11B Fe1B 115.4(3) . . ? N2B C12B C13B 124.9(5) . . ? C18B C13B C14B 119.8(6) . . ? C18B C13B C12B 117.8(6) . . ? C14B C13B C12B 122.5(5) . . ? O19B C14B C13B 124.6(5) . . ? O19B C14B C15B 118.3(5) . . ? C13B C14B C15B 117.1(5) . . ? C16B C15B C14B 120.9(6) . . ? C17B C16B C15B 121.6(6) . . ? C18B C17B C16B 118.5(6) . . ? C17B C18B C13B 122.2(7) . . ? C14B O19B Fe1B 126.3(3) . . ? N11B C20B C21B 124.8(4) . . ? C26B C21B C22B 119.7(5) . . ? C26B C21B C20B 117.5(4) . . ? C22B C21B C20B 122.6(5) . . ? O27B C22B C23B 119.5(5) . . ? O27B C22B C21B 124.1(5) . . ? C23B C22B C21B 116.5(6) . . ? C24B C23B C22B 122.2(6) . . ? C23B C24B C25B 121.1(5) . . ? C26B C25B C24B 118.6(6) . . ? C25B C26B C21B 121.9(6) . . ? C22B O27B Fe1B 126.2(3) . . ? O19C Fe1C O27C 104.5(6) . . ? O19C Fe1C N2C 86.9(4) . . ? O27C Fe1C N2C 103.7(3) . . ? O19C Fe1C N11C 87.9(4) . . ? O27C Fe1C N11C 82.4(3) . . ? N2C Fe1C N11C 172.8(3) . . ? O19C Fe1C N5C 160.5(4) . . ? O27C Fe1C N5C 89.5(3) . . ? N2C Fe1C N5C 76.6(3) . . ? N11C Fe1C N5C 107.6(3) . . ? O19C Fe1C N8C 93.9(6) . . ? O27C Fe1C N8C 151.5(3) . . ? N2C Fe1C N8C 98.8(3) . . ? N11C Fe1C N8C 76.7(3) . . ? N5C Fe1C N8C 78.8(3) . . ? C12C N2C C3C 117.7(7) . . ? C12C N2C Fe1C 125.8(6) . . ? C3C N2C Fe1C 116.4(5) . . ? N2C C3C C4C 108.0(7) . . ? N5C C4C C3C 109.4(7) . . ? C4C N5C C6C 113.9(7) . . ? C4C N5C Fe1C 106.4(5) . . ? C6C N5C Fe1C 111.5(6) . . ? N5C C6C C7C 107.2(8) . . ? N8C C7C C6C 106.5(8) . . ? C9C N8C C7C 112.5(7) . . ? C9C N8C Fe1C 108.0(6) . . ? C7C N8C Fe1C 109.3(5) . . ? N8C C9C C10C 109.5(7) . . ? N11C C10C C9C 109.0(7) . . ? C20C N11C C10C 119.0(7) . . ? C20C N11C Fe1C 122.0(6) . . ? C10C N11C Fe1C 117.3(6) . . ? N2C C12C C13C 126.4(7) . . ? C14C C13C C18C 120.0 . . ? C14C C13C C12C 123.2(5) . . ? C18C C13C C12C 116.7(5) . . ? O19C C14C C13C 122.3(7) . . ? O19C C14C C15C 117.7(6) . . ? C13C C14C C15C 120.0 . . ? C16C C15C C14C 120.0 . . ? C17C C16C C15C 120.0 . . ? C16C C17C C18C 120.0 . . ? C17C C18C C13C 120.0 . . ? C14C O19C Fe1C 133.6(8) . . ? N11C C20C C21C 124.2(7) . . ? C22C C21C C26C 120.0 . . ? C22C C21C C20C 126.4(5) . . ? C26C C21C C20C 113.3(5) . . ? O27C C22C C23C 124.2(5) . . ? O27C C22C C21C 115.8(5) . . ? C23C C22C C21C 120.0 . . ? C22C C23C C24C 120.0 . . ? C23C C24C C25C 120.0 . . ? C26C C25C C24C 120.0 . . ? C25C C26C C21C 120.0 . . ? C22C O27C Fe1C 140.7(5) . . ? O19D Fe1D O27D 96.5(5) . . ? O19D Fe1D N2D 91.4(4) . . ? O27D Fe1D N2D 91.5(3) . . ? O19D Fe1D N11D 84.9(4) . . ? O27D Fe1D N11D 90.6(3) . . ? N2D Fe1D N11D 175.9(3) . . ? O19D Fe1D N5D 171.7(4) . . ? O27D Fe1D N5D 90.8(3) . . ? N2D Fe1D N5D 84.5(3) . . ? N11D Fe1D N5D 99.0(3) . . ? O19D Fe1D N8D 90.8(5) . . ? O27D Fe1D N8D 169.0(3) . . ? N2D Fe1D N8D 96.6(3) . . ? N11D Fe1D N8D 81.8(3) . . ? N5D Fe1D N8D 82.6(3) . . ? C12D N2D C3D 121.5(8) . . ? C12D N2D Fe1D 127.5(6) . . ? C3D N2D Fe1D 111.0(5) . . ? N2D C3D C4D 106.8(8) . . ? N5D C4D C3D 107.7(8) . . ? C6D N5D C4D 109.1(9) . . ? C6D N5D Fe1D 108.6(7) . . ? C4D N5D Fe1D 110.5(6) . . ? N5D C6D C7D 109.7(8) . . ? N8D C7D C6D 109.8(8) . . ? C7D N8D C9D 112.0(7) . . ? C7D N8D Fe1D 112.9(6) . . ? C9D N8D Fe1D 107.7(6) . . ? N8D C9D C10D 107.1(7) . . ? N11D C10D C9D 106.5(7) . . ? C20D N11D C10D 117.9(7) . . ? C20D N11D Fe1D 124.1(6) . . ? C10D N11D Fe1D 116.0(6) . . ? N2D C12D C13D 123.7(7) . . ? C14D C13D C18D 120.0 . . ? C14D C13D C12D 122.8(4) . . ? C18D C13D C12D 117.2(4) . . ? O19D C14D C15D 116.8(6) . . ? O19D C14D C13D 123.2(6) . . ? C15D C14D C13D 120.0 . . ? C14D C15D C16D 120.0 . . ? C15D C16D C17D 120.0 . . ? C18D C17D C16D 120.0 . . ? C17D C18D C13D 120.0 . . ? C14D O19D Fe1D 125.0(7) . . ? N11D C20D C21D 122.7(8) . . ? C22D C21D C26D 120.0 . . ? C22D C21D C20D 126.7(5) . . ? C26D C21D C20D 112.8(5) . . ? O27D C22D C21D 118.3(5) . . ? O27D C22D C23D 121.5(5) . . ? C21D C22D C23D 120.0 . . ? C22D C23D C24D 120.0 . . ? C25D C24D C23D 120.0 . . ? C24D C25D C26D 120.0 . . ? C25D C26D C21D 120.0 . . ? C22D O27D Fe1D 133.4(5) . . ? O31A Cl28A O30A 106.6(8) . . ? O31A Cl28A O29A 110.3(7) . . ? O30A Cl28A O29A 108.3(7) . . ? O31A Cl28A O32A 105.7(8) . . ? O30A Cl28A O32A 115.4(8) . . ? O29A Cl28A O32A 110.4(8) . . ? O30B Cl28B O31B 112.4(9) . . ? O30B Cl28B O32B 104.9(8) . . ? O31B Cl28B O32B 111.7(10) . . ? O30B Cl28B O29B 108.6(8) . . ? O31B Cl28B O29B 111.2(9) . . ? O32B Cl28B O29B 107.8(9) . . ? O35A Cl33A O36A 121.3(10) . . ? O35A Cl33A O37A 112.6(8) . . ? O36A Cl33A O37A 104.9(8) . . ? O35A Cl33A O34A 111.0(8) . . ? O36A Cl33A O34A 103.6(8) . . ? O37A Cl33A O34A 101.3(7) . . ? O36B Cl33B O37B 111.3(9) . . ? O36B Cl33B O34B 117.1(9) . . ? O37B Cl33B O34B 110.3(8) . . ? O36B Cl33B O35B 106.0(9) . . ? O37B Cl33B O35B 106.3(8) . . ? O34B Cl33B O35B 105.0(7) . . ? O37C Cl33C O34C 120.0(9) . . ? O37C Cl33C O36C 113.3(10) . . ? O34C Cl33C O36C 107.7(8) . . ? O37C Cl33C O35C 109.1(10) . . ? O34C Cl33C O35C 102.8(9) . . ? O36C Cl33C O35C 102.0(9) . . ? O41A Cl38A O42A 109.5(5) . . ? O41A Cl38A O39A 108.7(6) . . ? O42A Cl38A O39A 109.7(6) . . ? O41A Cl38A O40A 109.3(5) . . ? O42A Cl38A O40A 110.0(5) . . ? O39A Cl38A O40A 109.8(6) . . ? O40B Cl38B O41B 109.9(5) . . ? O40B Cl38B O42B 109.0(4) . . ? O41B Cl38B O42B 109.7(5) . . ? O40B Cl38B O39B 110.2(6) . . ? O41B Cl38B O39B 108.7(6) . . ? O42B Cl38B O39B 109.3(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5A H5A O32A 0.93 2.26 3.120(12) 153.9 . N5A H5A O32B 0.93 2.53 3.345(14) 146.9 . N8A H8A O35A 0.93 2.37 3.133(14) 139.1 . N8A H8A O35B 0.93 2.58 3.189(13) 123.8 . N8A H8A O35C 0.93 2.47 3.345(17) 156.1 . N5B H5B O29A 0.93 2.04 2.871(11) 147.2 . N5B H5B O29B 0.93 2.32 3.157(11) 149.3 . N8B H8B O39A 0.93 2.26 3.187(14) 172.8 4_576 N8B H8B O39B 0.93 2.15 3.016(12) 155.1 4_576 N5C H5C O30A 0.93 2.21 3.023(10) 145.5 . N5C H5C O31A 0.93 2.44 3.094(12) 127.8 . N8C H8C O42A 0.93 2.15 3.060(11) 167.3 . N5D H5D O30A 0.93 2.41 3.186(11) 141.2 . N5D H5D O31B 0.93 2.27 3.101(16) 148.4 . N8D H8D O42B 0.93 2.15 2.956(10) 144.8 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.72 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.012 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.102