# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Musa S. Shongwe' _publ_contact_author_address ; Department of Chemistry College of Science Sultan Qaboos University P O Box 36 Al-Khod 123 Muscat Sultanate of Oman ; _publ_contact_author_email musa@squ.edu.om _publ_section_title ; Coordination versatility of tridentate pyridyl aroylhydrazones towards iron: tracking down the elusive aroylhydrazono-based ferric spin-crossover molecular materials ; loop_ _publ_author_name M.S.Shongwe S.H.Al-Rahbi M.A.Al-Azani A.A.Al-Muharbi ; F.Al-Mjeni ; D.Matoga A.Gismelseed Imaddin.Al-Omari A.Yousif H.Adams ; M.J.Morris ; M.Mikuriya # Attachment '- Dalton Trans_SHR38.cif' data_shr38p-1 _database_code_depnum_ccdc_archive 'CCDC 836952' #TrackingRef '- Dalton Trans_SHR38.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Cl Fe N6 O6' _chemical_formula_weight 631.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6635(4) _cell_length_b 14.7148(5) _cell_length_c 17.9725(9) _cell_angle_alpha 71.4020(10) _cell_angle_beta 88.945(2) _cell_angle_gamma 87.4680(10) _cell_volume 2920.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8070 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.90 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7512 _exptl_absorpt_correction_T_max 0.9370 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41361 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 31.09 _reflns_number_total 16294 _reflns_number_gt 9104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The perchlorate molecule Cl1 O5C O6C O7C O8C was found to be disordered and was refined to an occupancy Of 55%-45%. A Platon SQUEEZE function was used to eliminate a void containing disordered solvent molecules. These could not be satisfactorily modelled and were therefore omitted from the refinement. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 357 96 ' ' _platon_squeeze_details ; ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16294 _refine_ls_number_parameters 747 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.3022 _refine_ls_wR_factor_gt 0.2702 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.111 _refine_ls_shift/su_mean 0.003 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 0.76265(5) 0.87069(4) 0.43523(3) 0.02787(17) Uani 1 1 d . . . Fe2 Fe 0.74443(5) 0.58450(4) 0.05720(3) 0.03119(18) Uani 1 1 d . . . O1A O 0.7474(2) 0.5956(2) -0.05075(16) 0.0318(6) Uani 1 1 d . . . O1B O 0.7437(2) 0.8682(2) 0.54134(16) 0.0286(6) Uani 1 1 d . . . O2A O 0.7400(2) 0.4478(2) 0.09359(17) 0.0344(7) Uani 1 1 d . . . O2B O 0.7683(2) 1.00714(19) 0.39277(16) 0.0277(6) Uani 1 1 d . . . N1A N 0.5858(3) 0.6093(3) 0.0353(2) 0.0339(8) Uani 1 1 d . . . N1B N 0.6020(3) 0.8689(3) 0.4418(2) 0.0319(8) Uani 1 1 d . . . N2A N 0.5506(3) 0.6182(3) -0.0385(2) 0.0365(8) Uani 1 1 d . . . N2B N 0.5518(3) 0.8743(3) 0.50969(19) 0.0353(8) Uani 1 1 d . . . N3A N 0.6910(3) 0.5931(3) 0.1596(2) 0.0370(8) Uani 1 1 d . . . N3B N 0.7313(3) 0.8602(3) 0.3320(2) 0.0339(8) Uani 1 1 d . . . N4A N 0.9378(3) 0.4597(2) 0.0995(2) 0.0315(7) Uani 1 1 d . . . N4B N 0.9639(3) 0.9722(2) 0.4068(2) 0.0291(7) Uani 1 1 d . . . N5A N 0.9022(3) 0.5546(3) 0.0758(2) 0.0313(7) Uani 1 1 d . . . N5B N 0.9230(3) 0.8812(2) 0.43096(19) 0.0307(7) Uani 1 1 d . . . N6A N 0.7996(3) 0.7146(3) 0.03059(19) 0.0342(8) Uani 1 1 d . . . N6B N 0.8083(4) 0.7351(3) 0.4723(2) 0.0386(9) Uani 1 1 d . . . C1A C 0.6435(3) 0.6089(3) -0.0806(2) 0.0322(9) Uani 1 1 d . . . C1B C 0.6344(3) 0.8735(3) 0.5590(2) 0.0288(8) Uani 1 1 d . . . C2A C 0.6295(4) 0.6124(3) -0.1620(2) 0.0332(9) Uani 1 1 d . . . C2B C 0.6034(3) 0.8769(3) 0.6377(2) 0.0322(9) Uani 1 1 d . . . C3A C 0.5217(4) 0.6318(3) -0.1979(3) 0.0393(10) Uani 1 1 d . . . H3A H 0.4567 0.6436 -0.1691 0.047 Uiso 1 1 calc R . . C3B C 0.4889(4) 0.8970(3) 0.6549(2) 0.0320(9) Uani 1 1 d . . . H3B H 0.4319 0.9083 0.6156 0.038 Uiso 1 1 calc R . . C4A C 0.5089(4) 0.6341(4) -0.2739(3) 0.0455(11) Uani 1 1 d . . . H4A H 0.4363 0.6510 -0.2987 0.055 Uiso 1 1 calc R . . C4B C 0.4589(4) 0.9004(3) 0.7285(2) 0.0370(10) Uani 1 1 d . . . H4B H 0.3815 0.9147 0.7395 0.044 Uiso 1 1 calc R . . C5A C 0.6040(4) 0.6113(4) -0.3155(3) 0.0413(11) Uani 1 1 d . . . H5A H 0.5949 0.6091 -0.3674 0.050 Uiso 1 1 calc R . . C5B C 0.5419(4) 0.8829(4) 0.7872(3) 0.0403(10) Uani 1 1 d . . . H5B H 0.5210 0.8849 0.8380 0.048 Uiso 1 1 calc R . . C6A C 0.7096(4) 0.5922(3) -0.2802(3) 0.0392(10) Uani 1 1 d . . . H6A H 0.7737 0.5773 -0.3082 0.047 Uiso 1 1 calc R . . C6B C 0.6546(4) 0.8626(4) 0.7706(3) 0.0394(10) Uani 1 1 d . . . H6B H 0.7110 0.8506 0.8104 0.047 Uiso 1 1 calc R . . C7A C 0.7241(4) 0.5943(3) -0.2048(3) 0.0348(9) Uani 1 1 d . . . H7A H 0.7984 0.5835 -0.1821 0.042 Uiso 1 1 calc R . . C7B C 0.6864(4) 0.8594(3) 0.6966(2) 0.0349(9) Uani 1 1 d . . . H7B H 0.7640 0.8454 0.6860 0.042 Uiso 1 1 calc R . . C8A C 0.7549(5) 0.5842(3) 0.2228(3) 0.0448(11) Uani 1 1 d . . . H8A H 0.8356 0.5746 0.2194 0.054 Uiso 1 1 calc R . . C8B C 0.8083(5) 0.8522(3) 0.2776(3) 0.0419(11) Uani 1 1 d . . . H8B H 0.8879 0.8481 0.2893 0.050 Uiso 1 1 calc R . . C9A C 0.7091(6) 0.5885(4) 0.2914(3) 0.0559(14) Uani 1 1 d . . . H9A H 0.7569 0.5817 0.3352 0.067 Uiso 1 1 calc R . . C9B C 0.7740(5) 0.8497(4) 0.2049(3) 0.0495(13) Uani 1 1 d . . . H9B H 0.8295 0.8436 0.1672 0.059 Uiso 1 1 calc R . . C10A C 0.5895(6) 0.6031(4) 0.2968(3) 0.0584(15) Uani 1 1 d . . . H10A H 0.5555 0.6049 0.3448 0.070 Uiso 1 1 calc R . . C10B C 0.6561(5) 0.8564(4) 0.1872(3) 0.0543(14) Uani 1 1 d . . . H10B H 0.6309 0.8568 0.1371 0.065 Uiso 1 1 calc R . . C11A C 0.5223(5) 0.6146(3) 0.2321(3) 0.0515(14) Uani 1 1 d . . . H11A H 0.4418 0.6266 0.2340 0.062 Uiso 1 1 calc R . . C11B C 0.5793(5) 0.8621(3) 0.2436(3) 0.0453(12) Uani 1 1 d . . . H11B H 0.4994 0.8653 0.2332 0.054 Uiso 1 1 calc R . . C12A C 0.5763(4) 0.6083(3) 0.1625(3) 0.0416(11) Uani 1 1 d . . . C12B C 0.6162(4) 0.8635(3) 0.3154(3) 0.0370(10) Uani 1 1 d . . . C13A C 0.5143(4) 0.6172(3) 0.0900(3) 0.0387(10) Uani 1 1 d . . . C13B C 0.5416(4) 0.8690(3) 0.3810(2) 0.0367(10) Uani 1 1 d . . . C14A C 0.3898(4) 0.6330(4) 0.0786(3) 0.0504(13) Uani 1 1 d . . . H14A H 0.3698 0.7018 0.0649 0.076 Uiso 1 1 calc R . . H14B H 0.3500 0.5983 0.1272 0.076 Uiso 1 1 calc R . . H14C H 0.3664 0.6096 0.0361 0.076 Uiso 1 1 calc R . . C14B C 0.4147(4) 0.8742(4) 0.3771(3) 0.0495(13) Uani 1 1 d . . . H14D H 0.3828 0.8836 0.4250 0.074 Uiso 1 1 calc R . . H14E H 0.3877 0.8142 0.3721 0.074 Uiso 1 1 calc R . . H14F H 0.3896 0.9280 0.3314 0.074 Uiso 1 1 calc R . . C15A C 0.8438(4) 0.4097(3) 0.1059(2) 0.0318(9) Uani 1 1 d . . . C15B C 0.8742(3) 1.0330(3) 0.3890(2) 0.0269(8) Uani 1 1 d . . . C16A C 0.8584(4) 0.3041(3) 0.1268(2) 0.0310(9) Uani 1 1 d . . . C16B C 0.8953(3) 1.1360(3) 0.3641(2) 0.0283(8) Uani 1 1 d . . . C17A C 0.7692(5) 0.2491(3) 0.1194(2) 0.0396(10) Uani 1 1 d . . . H17A H 0.6961 0.2788 0.1022 0.048 Uiso 1 1 calc R . . C17B C 0.8073(4) 1.2052(3) 0.3366(2) 0.0298(8) Uani 1 1 d . . . H17B H 0.7314 1.1859 0.3335 0.036 Uiso 1 1 calc R . . C18A C 0.7860(5) 0.1504(4) 0.1371(3) 0.0461(12) Uani 1 1 d . . . H18A H 0.7253 0.1129 0.1304 0.055 Uiso 1 1 calc R . . C18B C 0.8299(4) 1.3028(3) 0.3135(3) 0.0381(10) Uani 1 1 d . . . H18B H 0.7693 1.3493 0.2945 0.046 Uiso 1 1 calc R . . C19A C 0.8907(5) 0.1072(3) 0.1644(3) 0.0494(13) Uani 1 1 d . . . H19A H 0.9013 0.0396 0.1767 0.059 Uiso 1 1 calc R . . C19B C 0.9399(4) 1.3321(3) 0.3181(3) 0.0385(10) Uani 1 1 d . . . H19B H 0.9550 1.3985 0.3027 0.046 Uiso 1 1 calc R . . C20A C 0.9797(5) 0.1596(3) 0.1739(3) 0.0442(11) Uani 1 1 d . . . H20A H 1.0512 0.1284 0.1935 0.053 Uiso 1 1 calc R . . C20B C 1.0279(4) 1.2634(3) 0.3456(2) 0.0358(10) Uani 1 1 d . . . H20B H 1.1036 1.2831 0.3487 0.043 Uiso 1 1 calc R . . C21A C 0.9657(4) 0.2581(3) 0.1550(2) 0.0371(10) Uani 1 1 d . . . H21A H 1.0277 0.2949 0.1610 0.045 Uiso 1 1 calc R . . C21B C 1.0067(3) 1.1671(3) 0.3685(2) 0.0304(8) Uani 1 1 d . . . H21B H 1.0679 1.1211 0.3875 0.037 Uiso 1 1 calc R . . C22A C 0.9756(4) 0.6231(3) 0.0635(2) 0.0297(8) Uani 1 1 d . . . C22B C 0.9911(4) 0.8053(3) 0.4545(2) 0.0351(10) Uani 1 1 d . . . C23A C 1.1009(4) 0.6060(3) 0.0758(3) 0.0352(9) Uani 1 1 d . . . H23A H 1.1199 0.6054 0.1289 0.053 Uiso 1 1 calc R . . H23B H 1.1414 0.6573 0.0372 0.053 Uiso 1 1 calc R . . H23C H 1.1243 0.5441 0.0696 0.053 Uiso 1 1 calc R . . C23B C 1.1177(4) 0.8051(4) 0.4558(3) 0.0470(12) Uani 1 1 d . . . H23D H 1.1428 0.8712 0.4358 0.070 Uiso 1 1 calc R . . H23E H 1.1496 0.7686 0.4225 0.070 Uiso 1 1 calc R . . H23F H 1.1448 0.7752 0.5097 0.070 Uiso 1 1 calc R . . C24A C 0.9142(4) 0.7171(3) 0.0371(2) 0.0326(9) Uani 1 1 d . . . C24B C 0.9224(4) 0.7182(3) 0.4813(2) 0.0389(11) Uani 1 1 d . . . C25A C 0.9671(4) 0.8045(3) 0.0183(3) 0.0396(10) Uani 1 1 d . . . H25A H 1.0477 0.8057 0.0245 0.048 Uiso 1 1 calc R . . C25B C 0.9691(6) 0.6261(3) 0.5158(3) 0.0558(15) Uani 1 1 d . . . H25B H 1.0497 0.6146 0.5219 0.067 Uiso 1 1 calc R . . C26A C 0.9041(5) 0.8880(4) -0.0088(3) 0.0499(13) Uani 1 1 d . . . H26A H 0.9400 0.9478 -0.0219 0.060 Uiso 1 1 calc R . . C26B C 0.8952(8) 0.5520(4) 0.5407(3) 0.078(2) Uani 1 1 d . . . H26B H 0.9251 0.4885 0.5646 0.094 Uiso 1 1 calc R . . C27A C 0.7870(5) 0.8848(3) -0.0170(3) 0.0487(13) Uani 1 1 d . . . H27A H 0.7418 0.9425 -0.0374 0.058 Uiso 1 1 calc R . . C27B C 0.7810(7) 0.5681(4) 0.5317(4) 0.075(2) Uani 1 1 d . . . H27B H 0.7309 0.5163 0.5497 0.090 Uiso 1 1 calc R . . C28A C 0.7362(4) 0.7976(3) 0.0045(3) 0.0407(11) Uani 1 1 d . . . H28A H 0.6552 0.7956 0.0010 0.049 Uiso 1 1 calc R . . C28B C 0.7367(6) 0.6610(3) 0.4960(3) 0.0533(14) Uani 1 1 d . . . H28B H 0.6563 0.6725 0.4882 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.0727(3) 0.65484(18) 0.26785(17) 0.0465(7) Uani 0.717(7) 1 d PD A 1 O5C O 0.1950(5) 0.6518(5) 0.2592(5) 0.090(2) Uiso 0.717(7) 1 d PDU A 1 O6C O 0.0497(6) 0.6881(4) 0.3336(3) 0.0634(15) Uiso 0.717(7) 1 d PDU A 1 O7C O 0.0271(6) 0.7263(4) 0.1990(3) 0.0549(15) Uiso 0.717(7) 1 d PDU A 1 O8C O 0.0308(5) 0.5628(3) 0.2715(3) 0.0515(14) Uiso 0.717(7) 1 d PDU A 1 Cl1' Cl 0.0286(6) 0.6481(5) 0.2860(3) 0.0359(14) Uani 0.283(7) 1 d PD A 2 O6C' O -0.0187(16) 0.6656(12) 0.3364(9) 0.068(4) Uiso 0.283(7) 1 d PU A 2 O5C' O 0.1434(10) 0.6611(12) 0.3079(11) 0.079(3) Uiso 0.283(7) 1 d PDU A 2 O7C' O -0.0154(13) 0.7050(9) 0.2105(6) 0.048(3) Uiso 0.283(7) 1 d PDU A 2 O8C' O 0.0765(17) 0.5604(9) 0.2771(12) 0.081(4) Uiso 0.283(7) 1 d PDU A 2 Cl2 Cl 0.6087(2) 0.38495(19) 0.49791(14) 0.1089(8) Uani 1 1 d . . . O1C O 0.6350(7) 0.3626(5) 0.5824(4) 0.132(2) Uiso 1 1 d . . . O2C O 0.5743(7) 0.3039(6) 0.4810(5) 0.142(3) Uiso 1 1 d . . . O3C O 0.7075(7) 0.4194(6) 0.4533(5) 0.139(3) Uiso 1 1 d . . . O4C O 0.5153(11) 0.4562(9) 0.4810(7) 0.215(5) Uiso 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 0.0260(3) 0.0313(3) 0.0259(3) -0.0081(2) 0.0049(2) -0.0061(2) Fe2 0.0236(3) 0.0361(3) 0.0317(3) -0.0084(2) 0.0039(2) 0.0027(2) O1A 0.0176(14) 0.0417(16) 0.0342(15) -0.0100(12) 0.0050(11) 0.0018(12) O1B 0.0219(14) 0.0352(14) 0.0299(14) -0.0121(12) 0.0050(11) -0.0030(11) O2A 0.0272(16) 0.0364(15) 0.0389(16) -0.0111(13) 0.0046(12) -0.0017(12) O2B 0.0174(13) 0.0321(14) 0.0317(14) -0.0071(11) 0.0026(11) -0.0038(11) N1A 0.0238(18) 0.0395(19) 0.0351(18) -0.0084(15) 0.0078(14) 0.0030(15) N1B 0.0287(19) 0.0387(18) 0.0293(17) -0.0110(14) 0.0054(14) -0.0138(15) N2A 0.0220(18) 0.047(2) 0.0375(19) -0.0101(16) 0.0058(14) 0.0030(15) N2B 0.0250(18) 0.056(2) 0.0253(16) -0.0126(16) 0.0060(14) -0.0170(16) N3A 0.040(2) 0.0320(18) 0.0330(18) -0.0021(15) 0.0057(16) -0.0021(16) N3B 0.037(2) 0.0351(18) 0.0289(17) -0.0092(14) 0.0023(15) -0.0078(15) N4A 0.0263(18) 0.0336(17) 0.0321(17) -0.0075(14) 0.0035(14) 0.0019(14) N4B 0.0205(17) 0.0366(18) 0.0321(17) -0.0137(14) 0.0030(13) -0.0019(14) N5A 0.0276(18) 0.0368(18) 0.0294(17) -0.0107(14) 0.0005(14) 0.0009(15) N5B 0.035(2) 0.0356(18) 0.0233(16) -0.0115(14) 0.0016(14) 0.0003(15) N6A 0.036(2) 0.0383(19) 0.0248(16) -0.0071(14) 0.0050(14) 0.0073(16) N6B 0.054(3) 0.0342(18) 0.0292(18) -0.0124(15) 0.0127(16) -0.0053(17) C1A 0.020(2) 0.039(2) 0.037(2) -0.0118(18) 0.0039(16) 0.0030(17) C1B 0.020(2) 0.035(2) 0.0308(19) -0.0084(16) 0.0058(15) -0.0092(16) C2A 0.026(2) 0.036(2) 0.036(2) -0.0094(17) 0.0030(17) -0.0008(17) C2B 0.021(2) 0.043(2) 0.031(2) -0.0099(17) 0.0074(16) -0.0078(17) C3A 0.023(2) 0.050(3) 0.049(3) -0.022(2) 0.0040(19) -0.0046(19) C3B 0.025(2) 0.039(2) 0.031(2) -0.0088(17) 0.0030(16) -0.0034(17) C4A 0.028(2) 0.066(3) 0.047(3) -0.024(2) -0.002(2) -0.004(2) C4B 0.028(2) 0.044(2) 0.035(2) -0.0079(18) 0.0101(17) -0.0041(18) C5A 0.033(2) 0.055(3) 0.038(2) -0.017(2) 0.0064(19) -0.011(2) C5B 0.035(3) 0.054(3) 0.030(2) -0.0109(19) 0.0103(18) -0.003(2) C6A 0.035(2) 0.046(2) 0.036(2) -0.0113(19) 0.0073(18) -0.004(2) C6B 0.028(2) 0.056(3) 0.032(2) -0.011(2) 0.0014(17) 0.000(2) C7A 0.027(2) 0.035(2) 0.040(2) -0.0090(18) 0.0064(17) -0.0019(17) C7B 0.020(2) 0.050(2) 0.033(2) -0.0112(19) 0.0042(16) -0.0038(18) C8A 0.060(3) 0.040(2) 0.032(2) -0.0088(19) -0.002(2) 0.002(2) C8B 0.050(3) 0.040(2) 0.034(2) -0.0097(19) 0.013(2) -0.011(2) C9A 0.076(4) 0.047(3) 0.039(3) -0.005(2) 0.003(3) -0.002(3) C9B 0.065(4) 0.052(3) 0.035(2) -0.019(2) 0.013(2) -0.009(3) C10A 0.084(5) 0.054(3) 0.033(3) -0.008(2) 0.021(3) -0.006(3) C10B 0.068(4) 0.061(3) 0.035(2) -0.018(2) 0.000(2) -0.005(3) C11A 0.063(4) 0.040(3) 0.042(3) -0.002(2) 0.026(2) 0.003(2) C11B 0.053(3) 0.045(3) 0.038(2) -0.013(2) -0.002(2) -0.014(2) C12A 0.048(3) 0.033(2) 0.037(2) -0.0038(18) 0.014(2) 0.004(2) C12B 0.042(3) 0.035(2) 0.035(2) -0.0109(18) -0.0016(19) -0.0112(19) C13A 0.034(2) 0.037(2) 0.039(2) -0.0058(18) 0.0147(19) 0.0025(19) C13B 0.036(2) 0.044(2) 0.030(2) -0.0100(18) 0.0020(18) -0.0165(19) C14A 0.027(2) 0.060(3) 0.055(3) -0.007(2) 0.016(2) 0.006(2) C14B 0.038(3) 0.069(3) 0.042(3) -0.015(2) -0.002(2) -0.026(2) C15A 0.030(2) 0.039(2) 0.0262(19) -0.0093(16) 0.0035(16) -0.0006(17) C15B 0.0203(19) 0.036(2) 0.0271(18) -0.0139(16) 0.0029(14) -0.0038(16) C16A 0.034(2) 0.034(2) 0.0256(18) -0.0108(16) 0.0065(16) -0.0040(17) C16B 0.0213(19) 0.042(2) 0.0239(18) -0.0137(16) 0.0052(14) -0.0059(16) C17A 0.051(3) 0.040(2) 0.029(2) -0.0117(18) 0.0142(19) -0.011(2) C17B 0.027(2) 0.0310(19) 0.032(2) -0.0098(16) 0.0027(16) -0.0069(16) C18A 0.054(3) 0.044(3) 0.041(3) -0.014(2) 0.020(2) -0.020(2) C18B 0.033(2) 0.040(2) 0.040(2) -0.0105(19) -0.0009(19) 0.0016(19) C19A 0.071(4) 0.034(2) 0.039(2) -0.007(2) 0.019(2) -0.001(2) C19B 0.044(3) 0.036(2) 0.037(2) -0.0119(18) 0.0063(19) -0.015(2) C20A 0.051(3) 0.046(3) 0.033(2) -0.0104(19) 0.010(2) 0.009(2) C20B 0.031(2) 0.045(2) 0.036(2) -0.0172(19) 0.0095(18) -0.0197(19) C21A 0.045(3) 0.035(2) 0.030(2) -0.0088(17) 0.0037(18) 0.0005(19) C21B 0.022(2) 0.041(2) 0.032(2) -0.0158(17) 0.0052(16) -0.0084(17) C22A 0.029(2) 0.033(2) 0.0266(19) -0.0088(16) 0.0018(16) -0.0028(17) C22B 0.038(2) 0.043(2) 0.0254(19) -0.0139(17) -0.0040(17) 0.0126(19) C23A 0.027(2) 0.043(2) 0.036(2) -0.0114(18) 0.0017(17) -0.0051(18) C23B 0.043(3) 0.055(3) 0.046(3) -0.022(2) -0.007(2) 0.016(2) C24A 0.033(2) 0.038(2) 0.0254(19) -0.0089(16) 0.0042(16) -0.0001(18) C24B 0.057(3) 0.035(2) 0.026(2) -0.0132(17) 0.0061(19) 0.008(2) C25A 0.044(3) 0.038(2) 0.036(2) -0.0086(18) 0.001(2) -0.007(2) C25B 0.093(5) 0.039(3) 0.032(2) -0.010(2) 0.008(3) 0.022(3) C26A 0.067(4) 0.040(2) 0.040(3) -0.008(2) 0.011(2) -0.009(2) C26B 0.150(7) 0.034(3) 0.042(3) -0.007(2) 0.040(4) 0.030(4) C27A 0.061(3) 0.036(2) 0.045(3) -0.009(2) 0.003(2) 0.014(2) C27B 0.120(6) 0.039(3) 0.064(4) -0.017(3) 0.060(4) -0.008(3) C28A 0.049(3) 0.037(2) 0.033(2) -0.0075(18) 0.0042(19) 0.008(2) C28B 0.078(4) 0.037(2) 0.050(3) -0.019(2) 0.032(3) -0.019(3) Cl1 0.063(2) 0.0369(10) 0.0412(13) -0.0164(9) -0.0075(11) 0.0096(12) Cl1' 0.038(3) 0.045(3) 0.028(2) -0.017(2) 0.002(2) 0.006(2) Cl2 0.0873(15) 0.1114(17) 0.0999(16) 0.0072(13) -0.0110(12) -0.0084(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1B 1.876(4) . ? Fe1 N5B 1.881(4) . ? Fe1 O1B 1.905(3) . ? Fe1 O2B 1.911(3) . ? Fe1 N6B 1.944(4) . ? Fe1 N3B 1.952(3) . ? Fe2 N5A 1.884(3) . ? Fe2 N1A 1.894(4) . ? Fe2 O1A 1.894(3) . ? Fe2 O2A 1.910(3) . ? Fe2 N6A 1.955(4) . ? Fe2 N3A 1.972(4) . ? O1A C1A 1.315(5) . ? O1B C1B 1.312(5) . ? O2A C15A 1.303(5) . ? O2B C15B 1.303(5) . ? N1A C13A 1.307(5) . ? N1A N2A 1.360(5) . ? N1B C13B 1.310(5) . ? N1B N2B 1.367(5) . ? N2A C1A 1.337(5) . ? N2B C1B 1.318(5) . ? N3A C8A 1.338(6) . ? N3A C12A 1.349(6) . ? N3B C8B 1.345(6) . ? N3B C12B 1.375(6) . ? N4A C15A 1.331(6) . ? N4A N5A 1.371(5) . ? N4B C15B 1.321(5) . ? N4B N5B 1.373(5) . ? N5A C22A 1.313(5) . ? N5B C22B 1.300(5) . ? N6A C28A 1.351(5) . ? N6A C24A 1.346(6) . ? N6B C24B 1.346(6) . ? N6B C28B 1.356(6) . ? C1A C2A 1.460(6) . ? C1B C2B 1.470(6) . ? C2A C3A 1.400(6) . ? C2A C7A 1.398(6) . ? C2B C7B 1.402(6) . ? C2B C3B 1.405(6) . ? C3A C4A 1.367(7) . ? C3A H3A 0.9500 . ? C3B C4B 1.378(6) . ? C3B H3B 0.9500 . ? C4A C5A 1.414(7) . ? C4A H4A 0.9500 . ? C4B C5B 1.399(6) . ? C4B H4B 0.9500 . ? C5A C6A 1.372(6) . ? C5A H5A 0.9500 . ? C5B C6B 1.383(6) . ? C5B H5B 0.9500 . ? C6A C7A 1.379(6) . ? C6A H6A 0.9500 . ? C6B C7B 1.388(6) . ? C6B H6B 0.9500 . ? C7A H7A 0.9500 . ? C7B H7B 0.9500 . ? C8A C9A 1.353(7) . ? C8A H8A 0.9500 . ? C8B C9B 1.386(7) . ? C8B H8B 0.9500 . ? C9A C10A 1.408(9) . ? C9A H9A 0.9500 . ? C9B C10B 1.409(8) . ? C9B H9B 0.9500 . ? C10A C11A 1.375(8) . ? C10A H10A 0.9500 . ? C10B C11B 1.361(7) . ? C10B H10B 0.9500 . ? C11A C12A 1.418(6) . ? C11A H11A 0.9500 . ? C11B C12B 1.375(6) . ? C11B H11B 0.9500 . ? C12A C13A 1.468(7) . ? C12B C13B 1.474(6) . ? C13A C14A 1.469(6) . ? C13B C14B 1.480(7) . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15A C16A 1.481(6) . ? C15B C16B 1.467(6) . ? C16A C17A 1.380(6) . ? C16A C21A 1.418(6) . ? C16B C17B 1.392(6) . ? C16B C21B 1.409(5) . ? C17A C18A 1.390(7) . ? C17A H17A 0.9500 . ? C17B C18B 1.397(6) . ? C17B H17B 0.9500 . ? C18A C19A 1.375(8) . ? C18A H18A 0.9500 . ? C18B C19B 1.384(6) . ? C18B H18B 0.9500 . ? C19A C20A 1.366(7) . ? C19A H19A 0.9500 . ? C19B C20B 1.389(7) . ? C19B H19B 0.9500 . ? C20A C21A 1.383(6) . ? C20A H20A 0.9500 . ? C20B C21B 1.376(6) . ? C20B H20B 0.9500 . ? C21A H21A 0.9500 . ? C21B H21B 0.9500 . ? C22A C24A 1.469(6) . ? C22A C23A 1.480(6) . ? C22B C23B 1.478(7) . ? C22B C24B 1.482(7) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24A C25A 1.391(6) . ? C24B C25B 1.390(6) . ? C25A C26A 1.356(7) . ? C25A H25A 0.9500 . ? C25B C26B 1.374(10) . ? C25B H25B 0.9500 . ? C26A C27A 1.381(8) . ? C26A H26A 0.9500 . ? C26B C27B 1.345(11) . ? C26B H26B 0.9500 . ? C27A C28A 1.375(7) . ? C27A H27A 0.9500 . ? C27B C28B 1.393(8) . ? C27B H27B 0.9500 . ? C28A H28A 0.9500 . ? C28B H28B 0.9500 . ? Cl1 O5C 1.432(4) . ? Cl1 O6C 1.433(4) . ? Cl1 O7C 1.438(4) . ? Cl1 O8C 1.442(4) . ? Cl1' O6C' 1.144(17) . ? Cl1' O8C' 1.437(5) . ? Cl1' O7C' 1.439(4) . ? Cl1' O5C' 1.441(5) . ? Cl2 O2C 1.398(8) . ? Cl2 O3C 1.409(8) . ? Cl2 O4C 1.444(12) . ? Cl2 O1C 1.483(8) . ? O4C O4C 1.66(2) 2_666 ? 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 N1B Fe1 N5B 175.51(15) . . ? N1B Fe1 O1B 80.97(13) . . ? N5B Fe1 O1B 96.57(13) . . ? N1B Fe1 O2B 95.17(14) . . ? N5B Fe1 O2B 81.28(13) . . ? O1B Fe1 O2B 95.17(12) . . ? N1B Fe1 N6B 102.75(17) . . ? N5B Fe1 N6B 80.90(16) . . ? O1B Fe1 N6B 89.37(13) . . ? O2B Fe1 N6B 162.00(15) . . ? N1B Fe1 N3B 81.26(15) . . ? N5B Fe1 N3B 101.49(15) . . ? O1B Fe1 N3B 161.50(14) . . ? O2B Fe1 N3B 91.50(13) . . ? N6B Fe1 N3B 89.57(15) . . ? N5A Fe2 N1A 176.68(16) . . ? N5A Fe2 O1A 96.78(13) . . ? N1A Fe2 O1A 80.93(13) . . ? N5A Fe2 O2A 81.00(14) . . ? N1A Fe2 O2A 96.76(14) . . ? O1A Fe2 O2A 95.08(13) . . ? N5A Fe2 N6A 80.87(15) . . ? N1A Fe2 N6A 101.45(16) . . ? O1A Fe2 N6A 89.43(13) . . ? O2A Fe2 N6A 161.71(14) . . ? N5A Fe2 N3A 101.65(15) . . ? N1A Fe2 N3A 80.82(16) . . ? O1A Fe2 N3A 161.09(14) . . ? O2A Fe2 N3A 91.95(14) . . ? N6A Fe2 N3A 89.36(15) . . ? C1A O1A Fe2 111.5(3) . . ? C1B O1B Fe1 110.7(2) . . ? C15A O2A Fe2 110.2(3) . . ? C15B O2B Fe1 110.1(2) . . ? C13A N1A N2A 122.3(4) . . ? C13A N1A Fe2 120.3(3) . . ? N2A N1A Fe2 117.5(3) . . ? C13B N1B N2B 122.1(4) . . ? C13B N1B Fe1 120.2(3) . . ? N2B N1B Fe1 117.5(3) . . ? C1A N2A N1A 107.7(3) . . ? C1B N2B N1B 107.8(3) . . ? C8A N3A C12A 119.9(4) . . ? C8A N3A Fe2 127.3(3) . . ? C12A N3A Fe2 112.8(3) . . ? C8B N3B C12B 118.9(4) . . ? C8B N3B Fe1 127.4(3) . . ? C12B N3B Fe1 113.7(3) . . ? C15A N4A N5A 106.4(3) . . ? C15B N4B N5B 107.3(3) . . ? C22A N5A N4A 121.4(4) . . ? C22A N5A Fe2 120.6(3) . . ? N4A N5A Fe2 117.9(3) . . ? C22B N5B N4B 121.9(4) . . ? C22B N5B Fe1 120.8(3) . . ? N4B N5B Fe1 117.1(3) . . ? C28A N6A C24A 119.7(4) . . ? C28A N6A Fe2 126.9(3) . . ? C24A N6A Fe2 113.4(3) . . ? C24B N6B C28B 119.9(4) . . ? C24B N6B Fe1 113.7(3) . . ? C28B N6B Fe1 126.1(4) . . ? O1A C1A N2A 122.2(4) . . ? O1A C1A C2A 118.7(4) . . ? N2A C1A C2A 119.2(4) . . ? O1B C1B N2B 122.8(4) . . ? O1B C1B C2B 118.4(3) . . ? N2B C1B C2B 118.8(4) . . ? C3A C2A C7A 119.0(4) . . ? C3A C2A C1A 120.9(4) . . ? C7A C2A C1A 120.1(4) . . ? C7B C2B C3B 119.1(4) . . ? C7B C2B C1B 120.9(4) . . ? C3B C2B C1B 119.9(4) . . ? C4A C3A C2A 120.7(4) . . ? C4A C3A H3A 119.6 . . ? C2A C3A H3A 119.6 . . ? C4B C3B C2B 120.4(4) . . ? C4B C3B H3B 119.8 . . ? C2B C3B H3B 119.8 . . ? C3A C4A C5A 119.8(4) . . ? C3A C4A H4A 120.1 . . ? C5A C4A H4A 120.1 . . ? C3B C4B C5B 120.4(4) . . ? C3B C4B H4B 119.8 . . ? C5B C4B H4B 119.8 . . ? C6A C5A C4A 119.2(4) . . ? C6A C5A H5A 120.4 . . ? C4A C5A H5A 120.4 . . ? C6B C5B C4B 119.4(4) . . ? C6B C5B H5B 120.3 . . ? C4B C5B H5B 120.3 . . ? C7A C6A C5A 121.1(4) . . ? C7A C6A H6A 119.4 . . ? C5A C6A H6A 119.4 . . ? C5B C6B C7B 121.0(4) . . ? C5B C6B H6B 119.5 . . ? C7B C6B H6B 119.5 . . ? C6A C7A C2A 119.9(4) . . ? C6A C7A H7A 120.0 . . ? C2A C7A H7A 120.0 . . ? C6B C7B C2B 119.8(4) . . ? C6B C7B H7B 120.1 . . ? C2B C7B H7B 120.1 . . ? N3A C8A C9A 122.6(5) . . ? N3A C8A H8A 118.7 . . ? C9A C8A H8A 118.7 . . ? N3B C8B C9B 121.3(5) . . ? N3B C8B H8B 119.3 . . ? C9B C8B H8B 119.3 . . ? C8A C9A C10A 119.0(5) . . ? C8A C9A H9A 120.5 . . ? C10A C9A H9A 120.5 . . ? C8B C9B C10B 119.5(5) . . ? C8B C9B H9B 120.2 . . ? C10B C9B H9B 120.2 . . ? C11A C10A C9A 119.5(5) . . ? C11A C10A H10A 120.3 . . ? C9A C10A H10A 120.3 . . ? C11B C10B C9B 118.4(5) . . ? C11B C10B H10B 120.8 . . ? C9B C10B H10B 120.8 . . ? C10A C11A C12A 118.3(5) . . ? C10A C11A H11A 120.9 . . ? C12A C11A H11A 120.9 . . ? C10B C11B C12B 120.7(5) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? N3A C12A C11A 120.7(5) . . ? N3A C12A C13A 115.6(4) . . ? C11A C12A C13A 123.7(5) . . ? C11B C12B N3B 121.2(5) . . ? C11B C12B C13B 125.6(4) . . ? N3B C12B C13B 113.2(4) . . ? N1A C13A C14A 123.6(4) . . ? N1A C13A C12A 110.5(4) . . ? C14A C13A C12A 126.0(4) . . ? N1B C13B C12B 111.3(4) . . ? N1B C13B C14B 125.4(4) . . ? C12B C13B C14B 123.3(4) . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O2A C15A N4A 124.3(4) . . ? O2A C15A C16A 118.0(4) . . ? N4A C15A C16A 117.7(4) . . ? O2B C15B N4B 124.0(4) . . ? O2B C15B C16B 118.1(3) . . ? N4B C15B C16B 117.9(3) . . ? C17A C16A C21A 119.1(4) . . ? C17A C16A C15A 121.1(4) . . ? C21A C16A C15A 119.7(4) . . ? C17B C16B C21B 118.2(4) . . ? C17B C16B C15B 121.8(4) . . ? C21B C16B C15B 119.9(4) . . ? C16A C17A C18A 120.0(5) . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C18B C17B C16B 120.6(4) . . ? C18B C17B H17B 119.7 . . ? C16B C17B H17B 119.7 . . ? C19A C18A C17A 120.0(5) . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C19B C18B C17B 120.5(4) . . ? C19B C18B H18B 119.7 . . ? C17B C18B H18B 119.7 . . ? C20A C19A C18A 121.2(5) . . ? C20A C19A H19A 119.4 . . ? C18A C19A H19A 119.4 . . ? C18B C19B C20B 119.2(4) . . ? C18B C19B H19B 120.4 . . ? C20B C19B H19B 120.4 . . ? C19A C20A C21A 119.9(5) . . ? C19A C20A H20A 120.1 . . ? C21A C20A H20A 120.1 . . ? C21B C20B C19B 120.8(4) . . ? C21B C20B H20B 119.6 . . ? C19B C20B H20B 119.6 . . ? C20A C21A C16A 119.8(5) . . ? C20A C21A H21A 120.1 . . ? C16A C21A H21A 120.1 . . ? C20B C21B C16B 120.7(4) . . ? C20B C21B H21B 119.7 . . ? C16B C21B H21B 119.7 . . ? N5A C22A C24A 109.7(4) . . ? N5A C22A C23A 124.2(4) . . ? C24A C22A C23A 126.1(4) . . ? N5B C22B C23B 125.5(4) . . ? N5B C22B C24B 109.7(4) . . ? C23B C22B C24B 124.8(4) . . ? C22A C23A H23A 109.5 . . ? C22A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C22A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N6A C24A C25A 120.4(4) . . ? N6A C24A C22A 115.4(4) . . ? C25A C24A C22A 124.2(4) . . ? N6B C24B C25B 121.4(5) . . ? N6B C24B C22B 114.6(4) . . ? C25B C24B C22B 123.9(5) . . ? C26A C25A C24A 120.2(5) . . ? C26A C25A H25A 119.9 . . ? C24A C25A H25A 119.9 . . ? C26B C25B C24B 118.0(6) . . ? C26B C25B H25B 121.0 . . ? C24B C25B H25B 121.0 . . ? C25A C26A C27A 119.0(5) . . ? C25A C26A H26A 120.5 . . ? C27A C26A H26A 120.5 . . ? C27B C26B C25B 121.1(5) . . ? C27B C26B H26B 119.4 . . ? C25B C26B H26B 119.4 . . ? C28A C27A C26A 119.6(4) . . ? C28A C27A H27A 120.2 . . ? C26A C27A H27A 120.2 . . ? C26B C27B C28B 119.7(6) . . ? C26B C27B H27B 120.2 . . ? C28B C27B H27B 120.2 . . ? N6A C28A C27A 121.0(5) . . ? N6A C28A H28A 119.5 . . ? C27A C28A H28A 119.5 . . ? N6B C28B C27B 119.9(6) . . ? N6B C28B H28B 120.0 . . ? C27B C28B H28B 120.0 . . ? O5C Cl1 O6C 106.0(4) . . ? O5C Cl1 O7C 107.3(4) . . ? O6C Cl1 O7C 107.8(4) . . ? O5C Cl1 O8C 108.7(4) . . ? O6C Cl1 O8C 117.7(4) . . ? O7C Cl1 O8C 108.8(4) . . ? O6C' Cl1' O8C' 133.0(13) . . ? O6C' Cl1' O7C' 112.2(11) . . ? O8C' Cl1' O7C' 106.8(10) . . ? O6C' Cl1' O5C' 97.6(12) . . ? O8C' Cl1' O5C' 84.6(12) . . ? O7C' Cl1' O5C' 119.8(10) . . ? O2C Cl2 O3C 108.9(5) . . ? O2C Cl2 O4C 109.1(6) . . ? O3C Cl2 O4C 111.9(6) . . ? O2C Cl2 O1C 111.6(5) . . ? O3C Cl2 O1C 109.0(5) . . ? O4C Cl2 O1C 106.3(6) . . ? Cl2 O4C O4C 130.1(13) . 2_666 ? 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 N5A Fe2 O1A C1A 174.6(3) . . . . ? N1A Fe2 O1A C1A -3.0(3) . . . . ? O2A Fe2 O1A C1A 93.1(3) . . . . ? N6A Fe2 O1A C1A -104.7(3) . . . . ? N3A Fe2 O1A C1A -18.3(6) . . . . ? N1B Fe1 O1B C1B -4.4(3) . . . . ? N5B Fe1 O1B C1B 171.8(3) . . . . ? O2B Fe1 O1B C1B 90.0(3) . . . . ? N6B Fe1 O1B C1B -107.4(3) . . . . ? N3B Fe1 O1B C1B -20.7(5) . . . . ? N5A Fe2 O2A C15A -4.1(3) . . . . ? N1A Fe2 O2A C15A 173.5(3) . . . . ? O1A Fe2 O2A C15A 92.0(3) . . . . ? N6A Fe2 O2A C15A -11.7(6) . . . . ? N3A Fe2 O2A C15A -105.5(3) . . . . ? N1B Fe1 O2B C15B 173.1(3) . . . . ? N5B Fe1 O2B C15B -4.2(2) . . . . ? O1B Fe1 O2B C15B 91.7(3) . . . . ? N6B Fe1 O2B C15B -12.4(6) . . . . ? N3B Fe1 O2B C15B -105.6(3) . . . . ? N5A Fe2 N1A C13A 136(3) . . . . ? O1A Fe2 N1A C13A -177.4(4) . . . . ? O2A Fe2 N1A C13A 88.5(3) . . . . ? N6A Fe2 N1A C13A -89.8(3) . . . . ? N3A Fe2 N1A C13A -2.4(3) . . . . ? N5A Fe2 N1A N2A -44(3) . . . . ? O1A Fe2 N1A N2A 2.6(3) . . . . ? O2A Fe2 N1A N2A -91.4(3) . . . . ? N6A Fe2 N1A N2A 90.2(3) . . . . ? N3A Fe2 N1A N2A 177.7(3) . . . . ? N5B Fe1 N1B C13B 123.5(18) . . . . ? O1B Fe1 N1B C13B -179.6(4) . . . . ? O2B Fe1 N1B C13B 86.0(4) . . . . ? N6B Fe1 N1B C13B -92.3(4) . . . . ? N3B Fe1 N1B C13B -4.7(3) . . . . ? N5B Fe1 N1B N2B -52(2) . . . . ? O1B Fe1 N1B N2B 4.8(3) . . . . ? O2B Fe1 N1B N2B -89.6(3) . . . . ? N6B Fe1 N1B N2B 92.1(3) . . . . ? N3B Fe1 N1B N2B 179.7(3) . . . . ? C13A N1A N2A C1A 178.4(4) . . . . ? Fe2 N1A N2A C1A -1.6(4) . . . . ? C13B N1B N2B C1B -179.5(4) . . . . ? Fe1 N1B N2B C1B -4.0(4) . . . . ? N5A Fe2 N3A C8A 3.0(4) . . . . ? N1A Fe2 N3A C8A -179.3(4) . . . . ? O1A Fe2 N3A C8A -163.9(4) . . . . ? O2A Fe2 N3A C8A 84.2(4) . . . . ? N6A Fe2 N3A C8A -77.6(4) . . . . ? N5A Fe2 N3A C12A -176.0(3) . . . . ? N1A Fe2 N3A C12A 1.8(3) . . . . ? O1A Fe2 N3A C12A 17.1(6) . . . . ? O2A Fe2 N3A C12A -94.7(3) . . . . ? N6A Fe2 N3A C12A 103.5(3) . . . . ? N1B Fe1 N3B C8B -177.1(4) . . . . ? N5B Fe1 N3B C8B 6.5(4) . . . . ? O1B Fe1 N3B C8B -160.9(4) . . . . ? O2B Fe1 N3B C8B 87.9(4) . . . . ? N6B Fe1 N3B C8B -74.2(4) . . . . ? N1B Fe1 N3B C12B 4.1(3) . . . . ? N5B Fe1 N3B C12B -172.3(3) . . . . ? O1B Fe1 N3B C12B 20.3(6) . . . . ? O2B Fe1 N3B C12B -90.9(3) . . . . ? N6B Fe1 N3B C12B 107.0(3) . . . . ? C15A N4A N5A C22A -179.5(4) . . . . ? C15A N4A N5A Fe2 -2.0(4) . . . . ? N1A Fe2 N5A C22A 133(3) . . . . ? O1A Fe2 N5A C22A 86.9(3) . . . . ? O2A Fe2 N5A C22A -179.0(3) . . . . ? N6A Fe2 N5A C22A -1.4(3) . . . . ? N3A Fe2 N5A C22A -88.8(3) . . . . ? N1A Fe2 N5A N4A -44(3) . . . . ? O1A Fe2 N5A N4A -90.6(3) . . . . ? O2A Fe2 N5A N4A 3.5(3) . . . . ? N6A Fe2 N5A N4A -178.9(3) . . . . ? N3A Fe2 N5A N4A 93.7(3) . . . . ? C15B N4B N5B C22B -178.2(4) . . . . ? C15B N4B N5B Fe1 -2.3(4) . . . . ? N1B Fe1 N5B C22B 141.9(18) . . . . ? O1B Fe1 N5B C22B 85.4(3) . . . . ? O2B Fe1 N5B C22B 179.7(3) . . . . ? N6B Fe1 N5B C22B -2.9(3) . . . . ? N3B Fe1 N5B C22B -90.6(3) . . . . ? N1B Fe1 N5B N4B -34(2) . . . . ? O1B Fe1 N5B N4B -90.5(3) . . . . ? O2B Fe1 N5B N4B 3.7(3) . . . . ? N6B Fe1 N5B N4B -178.8(3) . . . . ? N3B Fe1 N5B N4B 93.5(3) . . . . ? N5A Fe2 N6A C28A 178.3(4) . . . . ? N1A Fe2 N6A C28A 0.7(4) . . . . ? O1A Fe2 N6A C28A 81.3(4) . . . . ? O2A Fe2 N6A C28A -174.1(4) . . . . ? N3A Fe2 N6A C28A -79.8(4) . . . . ? N5A Fe2 N6A C24A 1.1(3) . . . . ? N1A Fe2 N6A C24A -176.5(3) . . . . ? O1A Fe2 N6A C24A -95.9(3) . . . . ? O2A Fe2 N6A C24A 8.7(6) . . . . ? N3A Fe2 N6A C24A 103.0(3) . . . . ? N1B Fe1 N6B C24B -173.0(3) . . . . ? N5B Fe1 N6B C24B 4.4(3) . . . . ? O1B Fe1 N6B C24B -92.4(3) . . . . ? O2B Fe1 N6B C24B 12.6(6) . . . . ? N3B Fe1 N6B C24B 106.1(3) . . . . ? N1B Fe1 N6B C28B 0.2(4) . . . . ? N5B Fe1 N6B C28B 177.6(4) . . . . ? O1B Fe1 N6B C28B 80.8(4) . . . . ? O2B Fe1 N6B C28B -174.2(4) . . . . ? N3B Fe1 N6B C28B -80.7(4) . . . . ? Fe2 O1A C1A N2A 3.3(5) . . . . ? Fe2 O1A C1A C2A -175.8(3) . . . . ? N1A N2A C1A O1A -1.2(6) . . . . ? N1A N2A C1A C2A 178.0(4) . . . . ? Fe1 O1B C1B N2B 3.8(5) . . . . ? Fe1 O1B C1B C2B -177.3(3) . . . . ? N1B N2B C1B O1B -0.1(6) . . . . ? N1B N2B C1B C2B -179.0(3) . . . . ? O1A C1A C2A C3A -176.4(4) . . . . ? N2A C1A C2A C3A 4.5(6) . . . . ? O1A C1A C2A C7A 4.8(6) . . . . ? N2A C1A C2A C7A -174.3(4) . . . . ? O1B C1B C2B C7B -10.2(6) . . . . ? N2B C1B C2B C7B 168.8(4) . . . . ? O1B C1B C2B C3B 170.4(4) . . . . ? N2B C1B C2B C3B -10.7(6) . . . . ? C7A C2A C3A C4A -0.6(7) . . . . ? C1A C2A C3A C4A -179.4(4) . . . . ? C7B C2B C3B C4B 0.6(6) . . . . ? C1B C2B C3B C4B -180.0(4) . . . . ? C2A C3A C4A C5A 3.6(8) . . . . ? C2B C3B C4B C5B -0.6(7) . . . . ? C3A C4A C5A C6A -3.6(8) . . . . ? C3B C4B C5B C6B 0.3(7) . . . . ? C4A C5A C6A C7A 0.4(7) . . . . ? C4B C5B C6B C7B 0.0(7) . . . . ? C5A C6A C7A C2A 2.6(7) . . . . ? C3A C2A C7A C6A -2.5(6) . . . . ? C1A C2A C7A C6A 176.3(4) . . . . ? C5B C6B C7B C2B -0.1(7) . . . . ? C3B C2B C7B C6B -0.3(7) . . . . ? C1B C2B C7B C6B -179.7(4) . . . . ? C12A N3A C8A C9A 0.9(7) . . . . ? Fe2 N3A C8A C9A -177.9(4) . . . . ? C12B N3B C8B C9B 1.7(6) . . . . ? Fe1 N3B C8B C9B -177.0(3) . . . . ? N3A C8A C9A C10A -0.2(8) . . . . ? N3B C8B C9B C10B 0.4(7) . . . . ? C8A C9A C10A C11A -1.3(8) . . . . ? C8B C9B C10B C11B -1.9(8) . . . . ? C9A C10A C11A C12A 2.0(8) . . . . ? C9B C10B C11B C12B 1.4(8) . . . . ? C8A N3A C12A C11A -0.2(6) . . . . ? Fe2 N3A C12A C11A 178.8(3) . . . . ? C8A N3A C12A C13A 179.8(4) . . . . ? Fe2 N3A C12A C13A -1.1(5) . . . . ? C10A C11A C12A N3A -1.3(7) . . . . ? C10A C11A C12A C13A 178.7(5) . . . . ? C10B C11B C12B N3B 0.8(7) . . . . ? C10B C11B C12B C13B -179.6(5) . . . . ? C8B N3B C12B C11B -2.3(6) . . . . ? Fe1 N3B C12B C11B 176.6(3) . . . . ? C8B N3B C12B C13B 178.0(4) . . . . ? Fe1 N3B C12B C13B -3.1(5) . . . . ? N2A N1A C13A C14A 2.2(7) . . . . ? Fe2 N1A C13A C14A -177.8(4) . . . . ? N2A N1A C13A C12A -177.7(4) . . . . ? Fe2 N1A C13A C12A 2.3(5) . . . . ? N3A C12A C13A N1A -0.6(6) . . . . ? C11A C12A C13A N1A 179.4(4) . . . . ? N3A C12A C13A C14A 179.5(4) . . . . ? C11A C12A C13A C14A -0.5(7) . . . . ? N2B N1B C13B C12B 179.5(4) . . . . ? Fe1 N1B C13B C12B 4.1(5) . . . . ? N2B N1B C13B C14B -0.4(7) . . . . ? Fe1 N1B C13B C14B -175.7(4) . . . . ? C11B C12B C13B N1B 179.9(4) . . . . ? N3B C12B C13B N1B -0.4(5) . . . . ? C11B C12B C13B C14B -0.2(7) . . . . ? N3B C12B C13B C14B 179.4(4) . . . . ? Fe2 O2A C15A N4A 4.6(5) . . . . ? Fe2 O2A C15A C16A -174.0(3) . . . . ? N5A N4A C15A O2A -1.9(5) . . . . ? N5A N4A C15A C16A 176.7(3) . . . . ? Fe1 O2B C15B N4B 4.6(5) . . . . ? Fe1 O2B C15B C16B -175.0(3) . . . . ? N5B N4B C15B O2B -1.7(5) . . . . ? N5B N4B C15B C16B 177.9(3) . . . . ? O2A C15A C16A C17A 11.7(6) . . . . ? N4A C15A C16A C17A -167.0(4) . . . . ? O2A C15A C16A C21A -168.1(4) . . . . ? N4A C15A C16A C21A 13.2(6) . . . . ? O2B C15B C16B C17B -7.1(5) . . . . ? N4B C15B C16B C17B 173.3(4) . . . . ? O2B C15B C16B C21B 172.1(3) . . . . ? N4B C15B C16B C21B -7.5(5) . . . . ? C21A C16A C17A C18A -2.1(6) . . . . ? C15A C16A C17A C18A 178.1(4) . . . . ? C21B C16B C17B C18B 0.5(6) . . . . ? C15B C16B C17B C18B 179.7(4) . . . . ? C16A C17A C18A C19A 2.0(7) . . . . ? C16B C17B C18B C19B -0.5(6) . . . . ? C17A C18A C19A C20A -0.5(7) . . . . ? C17B C18B C19B C20B 0.3(7) . . . . ? C18A C19A C20A C21A -0.9(7) . . . . ? C18B C19B C20B C21B -0.3(7) . . . . ? C19A C20A C21A C16A 0.8(6) . . . . ? C17A C16A C21A C20A 0.7(6) . . . . ? C15A C16A C21A C20A -179.5(4) . . . . ? C19B C20B C21B C16B 0.4(6) . . . . ? C17B C16B C21B C20B -0.5(6) . . . . ? C15B C16B C21B C20B -179.7(4) . . . . ? N4A N5A C22A C24A 178.7(3) . . . . ? Fe2 N5A C22A C24A 1.3(5) . . . . ? N4A N5A C22A C23A -2.0(6) . . . . ? Fe2 N5A C22A C23A -179.4(3) . . . . ? N4B N5B C22B C23B -2.6(6) . . . . ? Fe1 N5B C22B C23B -178.3(3) . . . . ? N4B N5B C22B C24B 176.6(3) . . . . ? Fe1 N5B C22B C24B 0.8(4) . . . . ? C28A N6A C24A C25A 1.0(6) . . . . ? Fe2 N6A C24A C25A 178.4(3) . . . . ? C28A N6A C24A C22A -178.1(4) . . . . ? Fe2 N6A C24A C22A -0.7(4) . . . . ? N5A C22A C24A N6A -0.3(5) . . . . ? C23A C22A C24A N6A -179.6(4) . . . . ? N5A C22A C24A C25A -179.4(4) . . . . ? C23A C22A C24A C25A 1.3(7) . . . . ? C28B N6B C24B C25B -1.2(6) . . . . ? Fe1 N6B C24B C25B 172.5(3) . . . . ? C28B N6B C24B C22B -178.9(4) . . . . ? Fe1 N6B C24B C22B -5.2(5) . . . . ? N5B C22B C24B N6B 3.0(5) . . . . ? C23B C22B C24B N6B -177.9(4) . . . . ? N5B C22B C24B C25B -174.7(4) . . . . ? C23B C22B C24B C25B 4.5(7) . . . . ? N6A C24A C25A C26A -1.8(7) . . . . ? C22A C24A C25A C26A 177.2(4) . . . . ? N6B C24B C25B C26B 0.0(7) . . . . ? C22B C24B C25B C26B 177.5(4) . . . . ? C24A C25A C26A C27A 0.3(7) . . . . ? C24B C25B C26B C27B 0.3(8) . . . . ? C25A C26A C27A C28A 1.9(7) . . . . ? C25B C26B C27B C28B 0.6(9) . . . . ? C24A N6A C28A C27A 1.3(6) . . . . ? Fe2 N6A C28A C27A -175.7(3) . . . . ? C26A C27A C28A N6A -2.7(7) . . . . ? C24B N6B C28B C27B 2.0(7) . . . . ? Fe1 N6B C28B C27B -170.8(4) . . . . ? C26B C27B C28B N6B -1.8(8) . . . . ? O2C Cl2 O4C O4C 153.4(15) . . . 2_666 ? O3C Cl2 O4C O4C -86.0(17) . . . 2_666 ? O1C Cl2 O4C O4C 32.9(18) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.910 _refine_diff_density_min -2.579 _refine_diff_density_rms 0.143 # start Validation Reply Form _vrf_PUBL004_GLOBAL ; PROBLEM: The contact author's name and address are missing, RESPONSE: ... ; _vrf_PUBL005_GLOBAL ; PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and RESPONSE: ... ; _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: ... ; _vrf_PUBL008_GLOBAL ; PROBLEM: _publ_section_title is missing. Title of paper. RESPONSE: ... ; _vrf_PUBL009_GLOBAL ; PROBLEM: _publ_author_name is missing. List of author(s) name(s). RESPONSE: ... ; _vrf_PUBL010_GLOBAL ; PROBLEM: _publ_author_address is missing. Author(s) address(es). RESPONSE: ... ; _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: ... ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 289 A**3 RESPONSE: ... All attemps to model the solvent molecules proved unsuccessfull due possibly to the fact that the crystal was decomposing. hence squeeze was used to complete the refinement. ; # end Validation Reply Form