# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Palaniandavar, Mallayan' _publ_contact_author_email palanim51@yahoo.com _publ_author_name M.Palaniandavar data_mpksf8af(2) _database_code_depnum_ccdc_archive 'CCDC 791683' #TrackingRef '[Fe(L2)Cl3] 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H16 Cl3 Fe N2 O' _chemical_formula_weight 354.46 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' 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' H H 0.0000 0.0000 '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 P21/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 7.991(3) _cell_length_b 11.870(4) _cell_length_c 17.249(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.599(12) _cell_angle_gamma 90.00 _cell_volume 1450.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1281 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.48 _exptl_crystal_description PLATES _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6839 _exptl_absorpt_correction_T_max 0.8329 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; As the crystal quality was bad higher angle reflections measured were weak / diffused which was not included in the final refinement cycles. Hence only 2021 refelections were available and used for the refinement cycle ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5212 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.1317 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2021 _reflns_number_gt 1428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0929P)^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 2021 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.2225 _refine_ls_wR_factor_gt 0.2045 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.3325(2) 0.30385(10) 0.38281(9) 0.0294(4) Uani 1 d . . . Cl1 Cl 0.3136(4) 0.4650(2) 0.30616(19) 0.0478(8) Uani 1 d . . . Cl2 Cl 0.3730(4) 0.17375(18) 0.29605(19) 0.0424(7) Uani 1 d . . . Cl3 Cl 0.6408(4) 0.3274(2) 0.48812(18) 0.0430(7) Uani 1 d . . . N1 N 0.2885(11) 0.1776(6) 0.4651(5) 0.0337(19) Uani 1 d . . . N2 N 0.2237(11) 0.3994(6) 0.4605(6) 0.038(2) Uani 1 d . . . H2C H 0.3114 0.4581 0.4751 0.050 Uiso 1 d . . . O1 O 0.0328(9) 0.2805(6) 0.3099(4) 0.0381(16) Uani 1 d . . . C1 C 0.2848(13) 0.0651(8) 0.4532(7) 0.038(2) Uani 1 d . . . H1 H 0.2995 0.0371 0.4064 0.046 Uiso 1 calc R . . C2 C 0.2605(16) -0.0082(9) 0.5073(9) 0.051(3) Uani 1 d . . . H2 H 0.2555 -0.0852 0.4964 0.061 Uiso 1 calc R . . C3 C 0.2429(15) 0.0311(10) 0.5790(8) 0.053(3) Uani 1 d . . . H3 H 0.2314 -0.0187 0.6179 0.064 Uiso 1 calc R . . C4 C 0.2430(15) 0.1469(9) 0.5910(7) 0.043(3) Uani 1 d . . . H4 H 0.2287 0.1771 0.6374 0.052 Uiso 1 calc R . . C5 C 0.2649(14) 0.2149(8) 0.5320(6) 0.036(2) Uani 1 d . . . C6 C 0.2690(16) 0.3421(8) 0.5434(7) 0.040(2) Uani 1 d . . . H6A H 0.1783 0.3638 0.5633 0.048 Uiso 1 calc R . . H6B H 0.3934 0.3652 0.5875 0.048 Uiso 1 calc R . . C7 C 0.0229(15) 0.4229(8) 0.4042(8) 0.046(3) Uani 1 d . . . H7A H 0.0118 0.4859 0.3663 0.055 Uiso 1 calc R . . H7B H -0.0346 0.4450 0.4406 0.055 Uiso 1 calc R . . C8 C -0.0831(16) 0.3248(9) 0.3490(8) 0.049(3) Uani 1 d . . . H8 H -0.1004 0.2669 0.3852 0.059 Uiso 1 calc R . . C9 C -0.2684(14) 0.3531(12) 0.2724(8) 0.060(3) Uani 1 d . . . H9A H -0.3723 0.3259 0.2816 0.072 Uiso 1 calc R . . H9B H -0.2813 0.4340 0.2634 0.072 Uiso 1 calc R . . C10 C -0.267(2) 0.2992(19) 0.2002(10) 0.138(10) Uani 1 d . . . H10A H -0.3249 0.3479 0.1494 0.165 Uiso 1 calc R . . H10B H -0.3404 0.2304 0.1873 0.165 Uiso 1 calc R . . C11 C -0.0771(18) 0.2728(12) 0.2174(8) 0.061(3) Uani 1 d . . . H11A H -0.0706 0.1975 0.1972 0.073 Uiso 1 calc R . . H11B H -0.0328 0.3262 0.1884 0.073 Uiso 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 0.0365(8) 0.0228(7) 0.0314(8) -0.0019(6) 0.0178(6) 0.0034(6) Cl1 0.0693(19) 0.0353(13) 0.0487(17) 0.0070(12) 0.0357(15) 0.0062(12) Cl2 0.0596(18) 0.0313(12) 0.0495(16) -0.0057(11) 0.0364(14) 0.0043(11) Cl3 0.0367(14) 0.0380(14) 0.0457(16) -0.0024(12) 0.0119(12) -0.0027(11) N1 0.035(5) 0.025(4) 0.036(5) 0.000(3) 0.012(4) 0.003(3) N2 0.037(5) 0.033(4) 0.041(5) -0.008(4) 0.016(4) 0.000(4) O1 0.036(4) 0.051(4) 0.025(4) -0.003(3) 0.012(3) 0.013(3) C1 0.032(5) 0.038(5) 0.048(6) 0.000(5) 0.023(5) 0.009(4) C2 0.057(7) 0.039(6) 0.070(8) 0.012(6) 0.042(7) 0.005(5) C3 0.049(7) 0.070(8) 0.046(7) 0.025(6) 0.027(6) 0.009(6) C4 0.055(7) 0.052(6) 0.035(6) -0.001(5) 0.032(6) 0.002(5) C5 0.038(6) 0.036(5) 0.025(5) -0.002(4) 0.006(5) 0.008(4) C6 0.056(7) 0.038(5) 0.027(6) -0.004(5) 0.020(5) 0.006(5) C7 0.049(7) 0.037(5) 0.052(7) -0.013(5) 0.023(6) 0.014(5) C8 0.042(6) 0.064(7) 0.043(7) -0.001(6) 0.022(6) 0.011(5) C9 0.027(6) 0.100(9) 0.061(8) -0.004(8) 0.027(6) 0.009(6) C10 0.080(12) 0.25(3) 0.051(10) -0.008(13) 0.000(9) 0.105(15) C11 0.056(8) 0.083(9) 0.041(7) -0.015(7) 0.020(6) -0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.145(7) . ? Fe1 N1 2.202(8) . ? Fe1 N2 2.218(8) . ? Fe1 Cl2 2.276(3) . ? Fe1 Cl1 2.291(3) . ? Fe1 Cl3 2.303(3) . ? N1 C5 1.328(12) . ? N1 C1 1.350(12) . ? N2 C7 1.466(13) . ? N2 C6 1.469(12) . ? N2 H2C 0.94 . ? O1 C11 1.424(14) . ? O1 C8 1.472(12) . ? C1 C2 1.355(14) . ? C1 H1 0.9300 . ? C2 C3 1.388(16) . ? C2 H2 0.9300 . ? C3 C4 1.390(15) . ? C3 H3 0.9300 . ? C4 C5 1.373(14) . ? C4 H4 0.9300 . ? C5 C6 1.521(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.494(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.497(15) . ? C8 H8 0.9800 . ? C9 C10 1.405(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.44(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N1 79.7(3) . . ? O1 Fe1 N2 77.1(3) . . ? N1 Fe1 N2 74.6(3) . . ? O1 Fe1 Cl2 89.26(19) . . ? N1 Fe1 Cl2 94.4(2) . . ? N2 Fe1 Cl2 163.7(2) . . ? O1 Fe1 Cl1 90.7(2) . . ? N1 Fe1 Cl1 162.4(2) . . ? N2 Fe1 Cl1 89.0(2) . . ? Cl2 Fe1 Cl1 100.28(11) . . ? O1 Fe1 Cl3 166.91(19) . . ? N1 Fe1 Cl3 90.3(2) . . ? N2 Fe1 Cl3 92.1(2) . . ? Cl2 Fe1 Cl3 100.06(11) . . ? Cl1 Fe1 Cl3 96.56(11) . . ? C5 N1 C1 117.4(9) . . ? C5 N1 Fe1 117.6(6) . . ? C1 N1 Fe1 125.0(7) . . ? C7 N2 C6 115.7(8) . . ? C7 N2 Fe1 108.1(6) . . ? C6 N2 Fe1 111.2(6) . . ? C7 N2 H2C 119 . . ? C6 N2 H2C 105 . . ? Fe1 N2 H2C 95 . . ? C11 O1 C8 110.1(8) . . ? C11 O1 Fe1 127.3(7) . . ? C8 O1 Fe1 117.0(6) . . ? N1 C1 C2 122.0(10) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 120.3(10) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 118.2(10) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 117.5(10) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 124.5(9) . . ? N1 C5 C6 116.1(9) . . ? C4 C5 C6 119.4(9) . . ? N2 C6 C5 110.7(8) . . ? N2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 113.4(8) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O1 C8 C7 106.2(8) . . ? O1 C8 C9 104.5(9) . . ? C7 C8 C9 115.1(9) . . ? O1 C8 H8 110.2 . . ? C7 C8 H8 110.2 . . ? C9 C8 H8 110.2 . . ? C10 C9 C8 105.6(9) . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9B 110.6 . . ? C8 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C9 C10 C11 110.9(14) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? O1 C11 C10 105.1(11) . . ? O1 C11 H11A 110.7 . . ? C10 C11 H11A 110.7 . . ? O1 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.750 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.750 _refine_diff_density_max 0.704 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.126 # Attachment '[Fe(L5)(TCC)Cl] 5a.cif' data_mpfa10(5a) _database_code_depnum_ccdc_archive 'CCDC 791684' #TrackingRef '[Fe(L5)(TCC)Cl] 5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H24 Cl5 Fe N3 O3.50' _chemical_formula_weight 631.55 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1080(4) _cell_length_b 16.7012(5) _cell_length_c 14.2209(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.476(2) _cell_angle_gamma 90.00 _cell_volume 2727.50(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4346 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 25.19 _exptl_crystal_description Prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8468 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD diffractometer' _diffrn_measurement_method 'omega-phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24306 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4872 _reflns_number_gt 3351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+10.0242P] 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 4872 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 215.8 44.2 2 0.500 0.500 0.500 215.8 43.5 _platon_squeeze_details ; ? ; 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7241(5) 0.3615(4) 0.0812(4) 0.0587(15) Uani 1 d . . . H1 H 0.6730 0.3335 0.0288 0.070 Uiso 1 calc R . . C2 C 0.7721(6) 0.4317(4) 0.0606(6) 0.0743(19) Uani 1 d . . . H2 H 0.7554 0.4493 -0.0045 0.089 Uiso 1 calc R . . C3 C 0.8426(6) 0.4738(4) 0.1349(6) 0.077(2) Uani 1 d . . . H3 H 0.8741 0.5220 0.1227 0.092 Uiso 1 calc R . . C4 C 0.8685(5) 0.4450(4) 0.2307(6) 0.0737(19) Uani 1 d . . . H4 H 0.9169 0.4739 0.2837 0.088 Uiso 1 calc R . . C5 C 0.8212(4) 0.3726(3) 0.2464(4) 0.0507(14) Uani 1 d . . . C6 C 0.8547(5) 0.3323(4) 0.3436(5) 0.0666(17) Uani 1 d . . . H6A H 0.8828 0.3719 0.3956 0.080 Uiso 1 calc R . . H6B H 0.9176 0.2951 0.3480 0.080 Uiso 1 calc R . . C7 C 0.7949(5) 0.2184(4) 0.4226(4) 0.0586(15) Uani 1 d . . . H7A H 0.7312 0.1973 0.4426 0.070 Uiso 1 calc R . . H7B H 0.8563 0.2347 0.4819 0.070 Uiso 1 calc R . . C8 C 0.8392(4) 0.1552(3) 0.3720(4) 0.0528(14) Uani 1 d . . . C9 C 0.9257(5) 0.1035(4) 0.4216(5) 0.0624(17) Uani 1 d . . . H9 H 0.9607 0.1081 0.4898 0.075 Uiso 1 calc R . . C10 C 0.9598(6) 0.0452(4) 0.3698(6) 0.076(2) Uani 1 d . . . H10 H 1.0179 0.0091 0.4022 0.092 Uiso 1 calc R . . C11 C 0.9072(5) 0.0404(4) 0.2689(6) 0.0710(18) Uani 1 d . . . H11 H 0.9295 0.0014 0.2320 0.085 Uiso 1 calc R . . C12 C 0.8214(5) 0.0941(4) 0.2239(5) 0.0639(16) Uani 1 d . . . H12 H 0.7854 0.0901 0.1558 0.077 Uiso 1 calc R . . C13 C 0.4290(4) 0.2836(3) 0.2095(4) 0.0430(12) Uani 1 d . . . C14 C 0.4480(4) 0.2083(3) 0.2568(4) 0.0449(12) Uani 1 d . . . C15 C 0.3611(5) 0.1731(3) 0.2855(5) 0.0565(15) Uani 1 d . . . C16 C 0.2512(5) 0.2105(4) 0.2648(5) 0.0650(17) Uani 1 d . . . C17 C 0.2334(5) 0.2844(4) 0.2194(5) 0.0693(18) Uani 1 d . . . C18 C 0.3231(5) 0.3208(3) 0.1924(4) 0.0547(14) Uani 1 d . . . C19 C 0.6818(6) 0.3399(4) 0.3980(4) 0.0681(17) Uani 1 d . . . H19A H 0.6173 0.3084 0.4045 0.082 Uiso 1 calc R . . H19B H 0.6492 0.3818 0.3499 0.082 Uiso 1 calc R . . C20 C 0.7427(7) 0.3794(4) 0.4976(5) 0.085(2) Uani 1 d . . . H20A H 0.6868 0.3901 0.5321 0.102 Uiso 1 calc R . . H20B H 0.8020 0.3439 0.5384 0.102 Uiso 1 calc R . . C21 C 0.8687(9) 0.4859(5) 0.5725(7) 0.149(5) Uani 1 d . . . H21A H 0.8219 0.5110 0.6074 0.224 Uiso 1 calc R . . H21B H 0.9187 0.5251 0.5575 0.224 Uiso 1 calc R . . H21C H 0.9152 0.4445 0.6131 0.224 Uiso 1 calc R . . N1 N 0.7472(3) 0.3323(3) 0.1713(3) 0.0465(11) Uani 1 d . . . N2 N 0.7544(4) 0.2882(3) 0.3587(3) 0.0504(11) Uani 1 d . . . N3 N 0.7877(4) 0.1511(3) 0.2723(3) 0.0492(11) Uani 1 d . . . O1 O 0.5171(3) 0.3141(2) 0.1847(3) 0.0487(9) Uani 1 d . . . O2 O 0.5526(3) 0.1760(2) 0.2724(3) 0.0533(10) Uani 1 d . . . O3 O 0.7937(5) 0.4512(3) 0.4812(4) 0.109(2) Uani 1 d . . . Cl1 Cl 0.59859(14) 0.18185(11) 0.05649(12) 0.0724(5) Uani 1 d . . . Cl2 Cl 0.38469(16) 0.08064(11) 0.34052(17) 0.0907(6) Uani 1 d . . . Cl3 Cl 0.14254(16) 0.16497(14) 0.29862(19) 0.1055(8) Uani 1 d . . . Cl4 Cl 0.10239(18) 0.33351(15) 0.1992(2) 0.1250(10) Uani 1 d . . . Cl5 Cl 0.30087(14) 0.41344(10) 0.13569(16) 0.0807(6) Uani 1 d . . . Fe Fe 0.64765(6) 0.23799(4) 0.21069(5) 0.0442(2) Uani 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 C1 0.055(3) 0.068(4) 0.054(4) 0.012(3) 0.019(3) 0.005(3) C2 0.059(4) 0.074(5) 0.091(5) 0.028(4) 0.025(4) -0.001(4) C3 0.056(4) 0.064(4) 0.112(6) 0.031(4) 0.029(4) 0.000(3) C4 0.054(4) 0.066(4) 0.095(5) -0.010(4) 0.014(4) -0.018(3) C5 0.031(3) 0.049(3) 0.064(4) 0.004(3) 0.004(2) 0.001(2) C6 0.049(3) 0.062(4) 0.072(4) -0.004(3) -0.005(3) -0.012(3) C7 0.054(3) 0.063(4) 0.049(3) 0.010(3) 0.003(3) 0.006(3) C8 0.033(3) 0.054(3) 0.067(4) 0.016(3) 0.010(3) 0.002(2) C9 0.052(3) 0.064(4) 0.068(4) 0.029(3) 0.015(3) 0.012(3) C10 0.050(4) 0.061(4) 0.118(6) 0.032(4) 0.026(4) 0.016(3) C11 0.054(4) 0.058(4) 0.105(6) 0.006(4) 0.030(4) 0.010(3) C12 0.054(4) 0.060(4) 0.075(4) -0.005(3) 0.018(3) -0.003(3) C13 0.035(3) 0.048(3) 0.045(3) 0.001(2) 0.011(2) -0.004(2) C14 0.041(3) 0.043(3) 0.050(3) 0.003(2) 0.013(2) -0.001(2) C15 0.049(3) 0.053(3) 0.074(4) 0.011(3) 0.028(3) 0.001(3) C16 0.050(3) 0.068(4) 0.086(5) 0.017(3) 0.034(3) 0.001(3) C17 0.043(3) 0.075(4) 0.094(5) 0.011(4) 0.028(3) 0.010(3) C18 0.044(3) 0.053(3) 0.069(4) 0.010(3) 0.021(3) 0.003(3) C19 0.071(4) 0.069(4) 0.054(4) -0.002(3) 0.004(3) -0.001(3) C20 0.115(6) 0.069(5) 0.062(4) -0.011(4) 0.014(4) -0.001(4) C21 0.165(10) 0.087(6) 0.127(8) -0.028(6) -0.051(7) -0.020(6) N1 0.032(2) 0.051(3) 0.052(3) 0.010(2) 0.008(2) 0.0015(19) N2 0.040(2) 0.055(3) 0.046(3) 0.004(2) 0.000(2) 0.003(2) N3 0.038(2) 0.053(3) 0.050(3) 0.002(2) 0.004(2) 0.001(2) O1 0.0345(18) 0.046(2) 0.061(2) 0.0111(18) 0.0093(17) -0.0024(16) O2 0.040(2) 0.052(2) 0.067(2) 0.0136(19) 0.0152(18) 0.0043(17) O3 0.139(5) 0.070(3) 0.078(3) -0.010(3) -0.022(3) -0.015(3) Cl1 0.0592(9) 0.0843(12) 0.0569(9) -0.0129(8) -0.0056(7) -0.0028(8) Cl2 0.0764(11) 0.0732(12) 0.1374(18) 0.0455(11) 0.0550(12) 0.0089(9) Cl3 0.0626(11) 0.1131(16) 0.158(2) 0.0506(15) 0.0598(13) 0.0021(10) Cl4 0.0665(12) 0.1207(18) 0.213(3) 0.0640(18) 0.0800(15) 0.0377(12) Cl5 0.0627(10) 0.0623(10) 0.1244(16) 0.0310(10) 0.0400(10) 0.0200(8) Fe 0.0285(4) 0.0491(4) 0.0477(4) 0.0052(4) 0.0019(3) -0.0016(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 C1 N1 1.316(7) . ? C1 C2 1.380(8) . ? C1 H1 0.9300 . ? C2 C3 1.330(10) . ? C2 H2 0.9300 . ? C3 C4 1.383(10) . ? C3 H3 0.9300 . ? C4 C5 1.387(8) . ? C4 H4 0.9300 . ? C5 N1 1.338(7) . ? C5 C6 1.473(8) . ? C6 N2 1.493(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.464(7) . ? C7 C8 1.471(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.357(7) . ? C8 C9 1.369(7) . ? C9 C10 1.361(9) . ? C9 H9 0.9300 . ? C10 C11 1.375(10) . ? C10 H10 0.9300 . ? C11 C12 1.368(8) . ? C11 H11 0.9300 . ? C12 N3 1.313(7) . ? C12 H12 0.9300 . ? C13 O1 1.327(6) . ? C13 C18 1.375(7) . ? C13 C14 1.410(7) . ? C14 O2 1.329(6) . ? C14 C15 1.375(7) . ? C15 C16 1.414(8) . ? C15 Cl2 1.714(6) . ? C16 C17 1.379(9) . ? C16 Cl3 1.715(6) . ? C17 C18 1.400(8) . ? C17 Cl4 1.727(6) . ? C18 Cl5 1.726(6) . ? C19 N2 1.465(8) . ? C19 C20 1.524(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O3 1.403(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O3 1.449(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N1 Fe 2.162(4) . ? N2 Fe 2.253(4) . ? N3 Fe 2.193(4) . ? O1 Fe 1.970(3) . ? O2 Fe 1.950(4) . ? Cl1 Fe 2.2837(17) . ? 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 N1 C1 C2 123.2(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.2(7) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.1(6) . . ? N1 C5 C6 115.8(5) . . ? C4 C5 C6 123.0(5) . . ? C5 C6 N2 111.4(4) . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? N2 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 111.7(5) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 122.0(6) . . ? N3 C8 C7 115.4(5) . . ? C9 C8 C7 122.6(6) . . ? C10 C9 C8 119.1(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.1(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 118.8(7) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N3 C12 C11 123.1(6) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? O1 C13 C18 124.3(5) . . ? O1 C13 C14 116.4(4) . . ? C18 C13 C14 119.3(5) . . ? O2 C14 C15 123.7(5) . . ? O2 C14 C13 116.4(4) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 120.6(5) . . ? C14 C15 Cl2 119.2(4) . . ? C16 C15 Cl2 120.1(4) . . ? C17 C16 C15 119.3(5) . . ? C17 C16 Cl3 120.6(5) . . ? C15 C16 Cl3 120.1(5) . . ? C16 C17 C18 119.8(5) . . ? C16 C17 Cl4 120.2(5) . . ? C18 C17 Cl4 120.0(5) . . ? C13 C18 C17 121.1(5) . . ? C13 C18 Cl5 119.1(4) . . ? C17 C18 Cl5 119.8(4) . . ? N2 C19 C20 116.0(5) . . ? N2 C19 H19A 108.3 . . ? C20 C19 H19A 108.3 . . ? N2 C19 H19B 108.3 . . ? C20 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? O3 C20 C19 108.9(6) . . ? O3 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? O3 C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C1 N1 C5 118.2(5) . . ? C1 N1 Fe 124.0(4) . . ? C5 N1 Fe 116.6(4) . . ? C7 N2 C19 110.9(5) . . ? C7 N2 C6 110.8(4) . . ? C19 N2 C6 112.2(5) . . ? C7 N2 Fe 105.3(3) . . ? C19 N2 Fe 109.9(3) . . ? C6 N2 Fe 107.5(3) . . ? C12 N3 C8 117.9(5) . . ? C12 N3 Fe 126.9(4) . . ? C8 N3 Fe 115.2(4) . . ? C13 O1 Fe 111.6(3) . . ? C14 O2 Fe 112.1(3) . . ? C20 O3 C21 112.1(6) . . ? O2 Fe O1 82.79(14) . . ? O2 Fe N1 163.69(17) . . ? O1 Fe N1 87.77(15) . . ? O2 Fe N3 87.72(16) . . ? O1 Fe N3 167.17(17) . . ? N1 Fe N3 99.34(16) . . ? O2 Fe N2 91.32(16) . . ? O1 Fe N2 97.12(16) . . ? N1 Fe N2 76.64(17) . . ? N3 Fe N2 74.40(17) . . ? O2 Fe Cl1 101.70(13) . . ? O1 Fe Cl1 97.79(12) . . ? N1 Fe Cl1 92.71(13) . . ? N3 Fe Cl1 92.57(13) . . ? N2 Fe Cl1 161.29(13) . . ? 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 N1 C1 C2 C3 -2.0(10) . . . . ? C1 C2 C3 C4 1.8(10) . . . . ? C2 C3 C4 C5 0.7(10) . . . . ? C3 C4 C5 N1 -3.1(9) . . . . ? C3 C4 C5 C6 172.3(6) . . . . ? N1 C5 C6 N2 -37.8(7) . . . . ? C4 C5 C6 N2 146.5(6) . . . . ? N2 C7 C8 N3 -31.0(7) . . . . ? N2 C7 C8 C9 149.5(5) . . . . ? N3 C8 C9 C10 -1.2(9) . . . . ? C7 C8 C9 C10 178.3(6) . . . . ? C8 C9 C10 C11 0.6(9) . . . . ? C9 C10 C11 C12 -0.5(10) . . . . ? C10 C11 C12 N3 0.9(10) . . . . ? O1 C13 C14 O2 0.6(7) . . . . ? C18 C13 C14 O2 -179.1(5) . . . . ? O1 C13 C14 C15 179.5(5) . . . . ? C18 C13 C14 C15 -0.2(8) . . . . ? O2 C14 C15 C16 -178.9(6) . . . . ? C13 C14 C15 C16 2.3(9) . . . . ? O2 C14 C15 Cl2 -2.5(8) . . . . ? C13 C14 C15 Cl2 178.7(4) . . . . ? C14 C15 C16 C17 -2.8(10) . . . . ? Cl2 C15 C16 C17 -179.2(5) . . . . ? C14 C15 C16 Cl3 178.6(5) . . . . ? Cl2 C15 C16 Cl3 2.2(8) . . . . ? C15 C16 C17 C18 1.3(10) . . . . ? Cl3 C16 C17 C18 179.9(5) . . . . ? C15 C16 C17 Cl4 -176.7(5) . . . . ? Cl3 C16 C17 Cl4 1.9(9) . . . . ? O1 C13 C18 C17 179.0(5) . . . . ? C14 C13 C18 C17 -1.3(9) . . . . ? O1 C13 C18 Cl5 -0.3(8) . . . . ? C14 C13 C18 Cl5 179.4(4) . . . . ? C16 C17 C18 C13 0.8(10) . . . . ? Cl4 C17 C18 C13 178.7(5) . . . . ? C16 C17 C18 Cl5 -179.9(5) . . . . ? Cl4 C17 C18 Cl5 -1.9(8) . . . . ? N2 C19 C20 O3 86.6(8) . . . . ? C2 C1 N1 C5 -0.4(8) . . . . ? C2 C1 N1 Fe 166.4(5) . . . . ? C4 C5 N1 C1 2.9(8) . . . . ? C6 C5 N1 C1 -172.8(5) . . . . ? C4 C5 N1 Fe -164.8(4) . . . . ? C6 C5 N1 Fe 19.5(6) . . . . ? C8 C7 N2 C19 164.0(5) . . . . ? C8 C7 N2 C6 -70.8(6) . . . . ? C8 C7 N2 Fe 45.2(5) . . . . ? C20 C19 N2 C7 64.8(7) . . . . ? C20 C19 N2 C6 -59.6(7) . . . . ? C20 C19 N2 Fe -179.2(5) . . . . ? C5 C6 N2 C7 150.1(5) . . . . ? C5 C6 N2 C19 -85.4(6) . . . . ? C5 C6 N2 Fe 35.5(6) . . . . ? C11 C12 N3 C8 -1.4(9) . . . . ? C11 C12 N3 Fe -177.6(4) . . . . ? C9 C8 N3 C12 1.6(8) . . . . ? C7 C8 N3 C12 -178.0(5) . . . . ? C9 C8 N3 Fe 178.2(4) . . . . ? C7 C8 N3 Fe -1.4(6) . . . . ? C18 C13 O1 Fe -174.7(4) . . . . ? C14 C13 O1 Fe 5.6(5) . . . . ? C15 C14 O2 Fe 174.6(5) . . . . ? C13 C14 O2 Fe -6.5(6) . . . . ? C19 C20 O3 C21 -170.8(7) . . . . ? C14 O2 Fe O1 7.4(3) . . . . ? C14 O2 Fe N1 62.5(7) . . . . ? C14 O2 Fe N3 178.7(4) . . . . ? C14 O2 Fe N2 104.4(4) . . . . ? C14 O2 Fe Cl1 -89.1(3) . . . . ? C13 O1 Fe O2 -7.0(3) . . . . ? C13 O1 Fe N1 -173.7(3) . . . . ? C13 O1 Fe N3 -49.6(8) . . . . ? C13 O1 Fe N2 -97.5(3) . . . . ? C13 O1 Fe Cl1 93.9(3) . . . . ? C1 N1 Fe O2 -122.6(6) . . . . ? C5 N1 Fe O2 44.4(7) . . . . ? C1 N1 Fe O1 -68.1(4) . . . . ? C5 N1 Fe O1 98.9(4) . . . . ? C1 N1 Fe N3 122.7(4) . . . . ? C5 N1 Fe N3 -70.4(4) . . . . ? C1 N1 Fe N2 -165.9(5) . . . . ? C5 N1 Fe N2 1.0(4) . . . . ? C1 N1 Fe Cl1 29.6(4) . . . . ? C5 N1 Fe Cl1 -163.4(4) . . . . ? C12 N3 Fe O2 104.6(5) . . . . ? C8 N3 Fe O2 -71.7(4) . . . . ? C12 N3 Fe O1 146.8(6) . . . . ? C8 N3 Fe O1 -29.4(9) . . . . ? C12 N3 Fe N1 -90.2(5) . . . . ? C8 N3 Fe N1 93.5(4) . . . . ? C12 N3 Fe N2 -163.4(5) . . . . ? C8 N3 Fe N2 20.3(4) . . . . ? C12 N3 Fe Cl1 3.0(5) . . . . ? C8 N3 Fe Cl1 -173.3(4) . . . . ? C7 N2 Fe O2 53.1(4) . . . . ? C19 N2 Fe O2 -66.3(4) . . . . ? C6 N2 Fe O2 171.3(4) . . . . ? C7 N2 Fe O1 136.0(3) . . . . ? C19 N2 Fe O1 16.6(4) . . . . ? C6 N2 Fe O1 -105.8(4) . . . . ? C7 N2 Fe N1 -138.0(4) . . . . ? C19 N2 Fe N1 102.5(4) . . . . ? C6 N2 Fe N1 -19.8(3) . . . . ? C7 N2 Fe N3 -34.1(3) . . . . ? C19 N2 Fe N3 -153.6(4) . . . . ? C6 N2 Fe N3 84.0(4) . . . . ? C7 N2 Fe Cl1 -81.3(5) . . . . ? C19 N2 Fe Cl1 159.2(4) . . . . ? C6 N2 Fe Cl1 36.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.699 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.077 # Attachment '[Fe(L6)Cl3] 6.cif' data_[Fe(L6)Cl3] _database_code_depnum_ccdc_archive 'CCDC 791685' #TrackingRef '[Fe(L6)Cl3] 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H21 Cl3 Fe N3 O' _chemical_formula_weight 445.57 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 P21/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 8.6152(13) _cell_length_b 14.906(2) _cell_length_c 15.224(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.299(2) _cell_angle_gamma 90.00 _cell_volume 1946.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCKS _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4880 _exptl_absorpt_correction_T_max 0.7154 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11238 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4475 _reflns_number_gt 3843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.6910P] 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 4475 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.32034(3) 0.219862(19) 1.011852(17) 0.03578(10) Uani 1 d . . . Cl3 Cl 0.12128(7) 0.12192(4) 0.98412(4) 0.05842(17) Uani 1 d . . . Cl1 Cl 0.19942(6) 0.33195(4) 1.08457(3) 0.04821(14) Uani 1 d . . . Cl2 Cl 0.44314(7) 0.15199(4) 1.13403(3) 0.05058(15) Uani 1 d . . . O1 O 0.0505(2) 0.45570(12) 0.79594(13) 0.0720(6) Uani 1 d . . . N1 N 0.4669(2) 0.14935(11) 0.92308(11) 0.0411(4) Uani 1 d . . . N2 N 0.25553(18) 0.28906(11) 0.88102(10) 0.0344(3) Uani 1 d . . . N3 N 0.51667(19) 0.31344(12) 1.00022(11) 0.0390(4) Uani 1 d . . . C1 C 0.5910(3) 0.09761(16) 0.94736(16) 0.0527(5) Uani 1 d . . . H1 H 0.6110 0.0823 1.0065 0.063 Uiso 1 calc R . . C2 C 0.6895(3) 0.06638(17) 0.88864(18) 0.0602(6) Uani 1 d . . . H2 H 0.7752 0.0312 0.9078 0.072 Uiso 1 calc R . . C3 C 0.6594(3) 0.08796(18) 0.80078(18) 0.0625(7) Uani 1 d . . . H3 H 0.7239 0.0672 0.7595 0.075 Uiso 1 calc R . . C4 C 0.5328(3) 0.14058(16) 0.77522(15) 0.0545(6) Uani 1 d . . . H4 H 0.5102 0.1557 0.7162 0.065 Uiso 1 calc R . . C5 C 0.4390(2) 0.17095(13) 0.83786(13) 0.0408(4) Uani 1 d . . . C6 C 0.2955(3) 0.22428(14) 0.81235(13) 0.0444(5) Uani 1 d . . . H6A H 0.3097 0.2570 0.7586 0.053 Uiso 1 calc R . . H6B H 0.2087 0.1834 0.7998 0.053 Uiso 1 calc R . . C7 C 0.3450(3) 0.37348(14) 0.87900(15) 0.0456(5) Uani 1 d . . . H7A H 0.2823 0.4219 0.8995 0.055 Uiso 1 calc R . . H7B H 0.3631 0.3864 0.8183 0.055 Uiso 1 calc R . . C8 C 0.4991(2) 0.37248(13) 0.93374(14) 0.0400(4) Uani 1 d . . . C9 C 0.6148(3) 0.43322(17) 0.91830(18) 0.0567(6) Uani 1 d . . . H9 H 0.5999 0.4740 0.8721 0.068 Uiso 1 calc R . . C10 C 0.7527(3) 0.43259(19) 0.9724(2) 0.0651(7) Uani 1 d . . . H10 H 0.8313 0.4733 0.9632 0.078 Uiso 1 calc R . . C11 C 0.7722(3) 0.3718(2) 1.0391(2) 0.0630(7) Uani 1 d . . . H11 H 0.8644 0.3700 1.0760 0.076 Uiso 1 calc R . . C12 C 0.6524(3) 0.31293(18) 1.05104(16) 0.0528(5) Uani 1 d . . . H12 H 0.6664 0.2710 1.0963 0.063 Uiso 1 calc R . . C13 C 0.0860(2) 0.31049(16) 0.86419(14) 0.0428(4) Uani 1 d . . . H13A H 0.0549 0.3455 0.9134 0.051 Uiso 1 calc R . . H13B H 0.0276 0.2548 0.8625 0.051 Uiso 1 calc R . . C14 C 0.0406(3) 0.36227(16) 0.77866(15) 0.0491(5) Uani 1 d . . . H14 H 0.1114 0.3463 0.7343 0.059 Uiso 1 calc R . . C16 C -0.1602(4) 0.4336(2) 0.6898(2) 0.0882(10) Uani 1 d . . . H16A H -0.1315 0.4280 0.6299 0.106 Uiso 1 calc R . . H16B H -0.2698 0.4490 0.6880 0.106 Uiso 1 calc R . . C15 C -0.1255(3) 0.3475(2) 0.7415(2) 0.0733(8) Uani 1 d . . . H15A H -0.1942 0.3405 0.7880 0.088 Uiso 1 calc R . . H15B H -0.1347 0.2953 0.7033 0.088 Uiso 1 calc R . . C17 C -0.0629(3) 0.5012(2) 0.7394(2) 0.0708(8) Uani 1 d . . . H17A H -0.0125 0.5394 0.6990 0.085 Uiso 1 calc R . . H17B H -0.1270 0.5385 0.7738 0.085 Uiso 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 0.03912(16) 0.03937(17) 0.02832(15) 0.00212(10) 0.00021(11) 0.00035(11) Cl3 0.0596(3) 0.0553(3) 0.0579(3) 0.0099(3) -0.0079(3) -0.0183(3) Cl1 0.0518(3) 0.0568(3) 0.0361(3) -0.0039(2) 0.0043(2) 0.0100(2) Cl2 0.0589(3) 0.0578(3) 0.0339(3) 0.0090(2) -0.0020(2) 0.0077(2) O1 0.0719(12) 0.0531(10) 0.0830(13) 0.0138(9) -0.0357(10) -0.0011(9) N1 0.0485(9) 0.0389(9) 0.0356(8) 0.0014(7) 0.0013(7) 0.0059(7) N2 0.0359(8) 0.0372(8) 0.0292(8) -0.0005(6) -0.0010(6) 0.0026(6) N3 0.0354(8) 0.0454(9) 0.0360(8) -0.0016(7) 0.0016(6) 0.0004(7) C1 0.0628(14) 0.0489(12) 0.0457(12) 0.0064(10) 0.0004(10) 0.0149(11) C2 0.0620(15) 0.0522(14) 0.0665(16) 0.0048(11) 0.0063(12) 0.0226(12) C3 0.0689(16) 0.0627(15) 0.0581(15) -0.0036(12) 0.0185(12) 0.0209(13) C4 0.0688(15) 0.0561(14) 0.0397(11) 0.0002(10) 0.0106(10) 0.0159(11) C5 0.0509(11) 0.0351(10) 0.0359(10) -0.0023(8) 0.0007(8) 0.0036(8) C6 0.0534(12) 0.0464(12) 0.0319(10) -0.0044(8) -0.0033(9) 0.0097(9) C7 0.0500(12) 0.0400(11) 0.0450(11) 0.0074(9) -0.0052(9) -0.0011(9) C8 0.0411(10) 0.0380(10) 0.0408(10) -0.0033(8) 0.0043(8) 0.0003(8) C9 0.0513(13) 0.0489(13) 0.0700(16) 0.0107(11) 0.0065(11) -0.0055(10) C10 0.0427(12) 0.0607(16) 0.092(2) -0.0022(14) 0.0091(13) -0.0129(11) C11 0.0357(11) 0.0777(18) 0.0737(17) -0.0036(14) -0.0057(11) -0.0051(11) C12 0.0416(11) 0.0666(15) 0.0486(12) 0.0027(11) -0.0048(9) -0.0008(10) C13 0.0363(10) 0.0523(12) 0.0388(10) 0.0032(9) -0.0011(8) 0.0049(9) C14 0.0455(12) 0.0594(14) 0.0412(11) 0.0040(10) -0.0036(9) 0.0092(10) C16 0.0699(18) 0.098(2) 0.089(2) 0.0299(19) -0.0326(16) 0.0030(17) C15 0.0668(17) 0.0739(18) 0.0725(18) 0.0064(14) -0.0298(14) -0.0073(14) C17 0.0655(16) 0.0690(17) 0.0743(18) 0.0226(14) -0.0117(14) 0.0111(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 Fe1 N1 2.2003(17) . ? Fe1 N3 2.2120(17) . ? Fe1 Cl3 2.2621(7) . ? Fe1 N2 2.2666(16) . ? Fe1 Cl2 2.2890(6) . ? Fe1 Cl1 2.3056(6) . ? O1 C17 1.414(3) . ? O1 C14 1.418(3) . ? N1 C5 1.337(3) . ? N1 C1 1.342(3) . ? N2 C7 1.478(3) . ? N2 C6 1.487(3) . ? N2 C13 1.494(2) . ? N3 C8 1.339(3) . ? N3 C12 1.341(3) . ? C1 C2 1.370(3) . ? C1 H1 0.9300 . ? C2 C3 1.377(4) . ? C2 H2 0.9300 . ? C3 C4 1.370(3) . ? C3 H3 0.9300 . ? C4 C5 1.382(3) . ? C4 H4 0.9300 . ? C5 C6 1.491(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.501(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.382(3) . ? C9 C10 1.381(4) . ? C9 H9 0.9300 . ? C10 C11 1.360(4) . ? C10 H10 0.9300 . ? C11 C12 1.379(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.533(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.505(3) . ? C14 H14 0.9800 . ? C16 C17 1.474(4) . ? C16 C15 1.521(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? 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 N1 Fe1 N3 76.44(7) . . ? N1 Fe1 Cl3 92.59(5) . . ? N3 Fe1 Cl3 164.61(5) . . ? N1 Fe1 N2 77.67(6) . . ? N3 Fe1 N2 76.75(6) . . ? Cl3 Fe1 N2 90.50(4) . . ? N1 Fe1 Cl2 92.27(5) . . ? N3 Fe1 Cl2 92.54(5) . . ? Cl3 Fe1 Cl2 98.74(2) . . ? N2 Fe1 Cl2 166.68(5) . . ? N1 Fe1 Cl1 162.09(5) . . ? N3 Fe1 Cl1 87.95(5) . . ? Cl3 Fe1 Cl1 100.89(3) . . ? N2 Fe1 Cl1 90.38(4) . . ? Cl2 Fe1 Cl1 97.21(2) . . ? C17 O1 C14 109.4(2) . . ? C5 N1 C1 118.22(18) . . ? C5 N1 Fe1 114.78(13) . . ? C1 N1 Fe1 126.38(14) . . ? C7 N2 C6 112.52(17) . . ? C7 N2 C13 108.56(16) . . ? C6 N2 C13 107.74(15) . . ? C7 N2 Fe1 108.61(12) . . ? C6 N2 Fe1 105.54(11) . . ? C13 N2 Fe1 113.93(12) . . ? C8 N3 C12 118.11(19) . . ? C8 N3 Fe1 116.18(13) . . ? C12 N3 Fe1 125.64(16) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.8(2) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.9(2) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 116.84(18) . . ? C4 C5 C6 121.24(19) . . ? N2 C6 C5 113.81(16) . . ? N2 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 114.61(17) . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? N3 C8 C9 121.7(2) . . ? N3 C8 C7 117.29(18) . . ? C9 C8 C7 120.9(2) . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.7(2) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N3 C12 C11 122.9(2) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N2 C13 C14 114.96(17) . . ? N2 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N2 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? O1 C14 C15 104.6(2) . . ? O1 C14 C13 109.30(19) . . ? C15 C14 C13 113.9(2) . . ? O1 C14 H14 109.6 . . ? C15 C14 H14 109.6 . . ? C13 C14 H14 109.6 . . ? C17 C16 C15 103.6(2) . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16B 111.0 . . ? C15 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C14 C15 C16 101.9(2) . . ? C14 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? C14 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.3 . . ? O1 C17 C16 108.2(2) . . ? O1 C17 H17A 110.1 . . ? C16 C17 H17A 110.1 . . ? O1 C17 H17B 110.1 . . ? C16 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 0.413 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.064 # Attachment '- 6a.cif' data_19mpksfm(6a) _database_code_depnum_ccdc_archive 'CCDC 791686' #TrackingRef '- 6a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H21 Br Cl4 Fe N3 O3' _chemical_formula_weight 664.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1129(9) _cell_length_b 15.7217(11) _cell_length_c 14.6905(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.7610(10) _cell_angle_gamma 90.00 _cell_volume 2649.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.512 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.4734 _exptl_absorpt_correction_T_max 0.7525 _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 SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15628 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.22 _reflns_number_total 6121 _reflns_number_gt 4630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+2.1898P] 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 6121 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.59608(4) 0.16993(3) 0.08220(3) 0.03649(15) Uani 1 d . . . Fe1 Fe 0.65303(4) 0.24975(3) 0.23469(4) 0.02151(15) Uani 1 d . . . Cl1 Cl 0.29189(9) 0.42252(6) 0.12450(8) 0.0337(2) Uani 1 d . . . Cl2 Cl 0.09603(10) 0.34465(8) 0.19553(10) 0.0488(3) Uani 1 d . . . Cl3 Cl 0.15235(12) 0.18667(11) 0.33265(14) 0.0771(6) Uani 1 d . . . Cl4 Cl 0.40243(11) 0.10301(10) 0.38973(13) 0.0703(5) Uani 1 d . . . O1 O 0.7504(11) 0.4851(5) 0.4973(5) 0.230(6) Uani 1 d . . . O2 O 0.5182(2) 0.32728(16) 0.19639(19) 0.0242(6) Uani 1 d . . . O3 O 0.5600(2) 0.19067(17) 0.3013(2) 0.0281(6) Uani 1 d . . . N1 N 0.7535(3) 0.34599(19) 0.1937(2) 0.0250(7) Uani 1 d . . . N2 N 0.7517(3) 0.3119(2) 0.3768(2) 0.0300(8) Uani 1 d . . . N3 N 0.7983(3) 0.16529(19) 0.3008(2) 0.0226(7) Uani 1 d . . . C1 C 0.7361(4) 0.3681(3) 0.1018(3) 0.0307(9) Uani 1 d . . . H1 H 0.6893 0.3340 0.0528 0.037 Uiso 1 calc R . . C2 C 0.7859(4) 0.4397(3) 0.0786(4) 0.0409(11) Uani 1 d . . . H2 H 0.7743 0.4530 0.0145 0.049 Uiso 1 calc R . . C3 C 0.8531(4) 0.4920(3) 0.1504(4) 0.0468(13) Uani 1 d . . . H3 H 0.8846 0.5420 0.1355 0.056 Uiso 1 calc R . . C4 C 0.8724(4) 0.4691(3) 0.2441(4) 0.0414(11) Uani 1 d . . . H4 H 0.9179 0.5032 0.2938 0.050 Uiso 1 calc R . . C5 C 0.8234(3) 0.3943(2) 0.2645(3) 0.0327(10) Uani 1 d . . . C6 C 0.8518(4) 0.3601(3) 0.3641(3) 0.0342(10) Uani 1 d . . . H6A H 0.9190 0.3229 0.3776 0.041 Uiso 1 calc R . . H6B H 0.8718 0.4068 0.4096 0.041 Uiso 1 calc R . . C7 C 0.7946(4) 0.2403(3) 0.4440(3) 0.0301(9) Uani 1 d . . . H7A H 0.7307 0.2160 0.4616 0.036 Uiso 1 calc R . . H7B H 0.8530 0.2605 0.5021 0.036 Uiso 1 calc R . . C8 C 0.8468(3) 0.1737(2) 0.3970(3) 0.0246(8) Uani 1 d . . . C9 C 0.9380(3) 0.1226(3) 0.4498(3) 0.0297(9) Uani 1 d . . . H9 H 0.9702 0.1294 0.5160 0.036 Uiso 1 calc R . . C10 C 0.9802(4) 0.0616(3) 0.4024(3) 0.0320(9) Uani 1 d . . . H10 H 1.0414 0.0266 0.4367 0.038 Uiso 1 calc R . . C11 C 0.9321(3) 0.0523(2) 0.3046(3) 0.0305(9) Uani 1 d . . . H11 H 0.9598 0.0113 0.2718 0.037 Uiso 1 calc R . . C12 C 0.8408(3) 0.1058(2) 0.2558(3) 0.0272(8) Uani 1 d . . . H12 H 0.8080 0.1000 0.1895 0.033 Uiso 1 calc R . . C13 C 0.6714(4) 0.3671(4) 0.4090(4) 0.0503(14) Uani 1 d . . . H13A H 0.6014 0.3348 0.4039 0.060 Uiso 1 calc R . . H13B H 0.6487 0.4148 0.3651 0.060 Uiso 1 calc R . . C14 C 0.7220(5) 0.4035(5) 0.5159(6) 0.091(3) Uani 1 d . . . H14 H 0.7872 0.3708 0.5584 0.110 Uiso 1 calc R . . C15 C 0.6296(8) 0.4239(6) 0.5576(7) 0.116(3) Uani 1 d . . . H15A H 0.6144 0.3764 0.5940 0.139 Uiso 1 calc R . . H15B H 0.5578 0.4402 0.5083 0.139 Uiso 1 calc R . . C16 C 0.6827(8) 0.4977(6) 0.6220(6) 0.107(3) Uani 1 d . . . H16A H 0.6241 0.5401 0.6206 0.128 Uiso 1 calc R . . H16B H 0.7187 0.4788 0.6878 0.128 Uiso 1 calc R . . C17 C 0.7649(17) 0.5301(9) 0.5854(13) 0.250(11) Uani 1 d . . . H17A H 0.8428 0.5213 0.6301 0.300 Uiso 1 calc R . . H17B H 0.7529 0.5906 0.5733 0.300 Uiso 1 calc R . . C18 C 0.4308(3) 0.2976(2) 0.2228(3) 0.0232(8) Uani 1 d . . . C19 C 0.3197(3) 0.3335(2) 0.1975(3) 0.0253(8) Uani 1 d . . . C20 C 0.2334(3) 0.2999(3) 0.2300(3) 0.0323(9) Uani 1 d . . . C21 C 0.2589(4) 0.2288(3) 0.2903(4) 0.0416(11) Uani 1 d . . . C22 C 0.3685(4) 0.1920(3) 0.3152(4) 0.0389(11) Uani 1 d . . . C23 C 0.4546(3) 0.2232(3) 0.2817(3) 0.0275(8) Uani 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 Br1 0.0303(2) 0.0428(3) 0.0275(2) -0.00861(17) -0.00305(18) 0.00208(18) Fe1 0.0159(3) 0.0244(3) 0.0212(3) 0.0006(2) 0.0017(2) 0.0009(2) Cl1 0.0248(5) 0.0347(5) 0.0416(6) 0.0116(4) 0.0108(4) 0.0093(4) Cl2 0.0218(5) 0.0555(7) 0.0710(9) 0.0191(6) 0.0176(6) 0.0107(5) Cl3 0.0303(7) 0.0878(11) 0.1239(15) 0.0629(10) 0.0398(8) 0.0131(7) Cl4 0.0354(7) 0.0701(9) 0.1124(13) 0.0625(9) 0.0336(8) 0.0151(6) O1 0.449(17) 0.158(7) 0.118(6) -0.081(5) 0.139(8) -0.190(10) O2 0.0185(13) 0.0277(13) 0.0253(14) 0.0045(10) 0.0058(11) 0.0021(10) O3 0.0174(13) 0.0312(14) 0.0333(16) 0.0083(12) 0.0050(12) 0.0025(11) N1 0.0140(15) 0.0242(16) 0.0337(18) 0.0000(13) 0.0034(13) 0.0039(12) N2 0.0236(17) 0.0344(18) 0.0273(18) -0.0058(14) 0.0016(14) 0.0078(14) N3 0.0173(15) 0.0226(15) 0.0247(16) 0.0021(12) 0.0023(13) 0.0001(12) C1 0.022(2) 0.037(2) 0.034(2) 0.0038(18) 0.0102(18) 0.0046(17) C2 0.035(2) 0.044(3) 0.052(3) 0.020(2) 0.025(2) 0.013(2) C3 0.031(2) 0.028(2) 0.089(4) 0.015(2) 0.031(3) 0.008(2) C4 0.026(2) 0.023(2) 0.073(3) 0.000(2) 0.013(2) 0.0030(17) C5 0.021(2) 0.0207(18) 0.054(3) -0.0015(17) 0.0078(19) 0.0044(16) C6 0.028(2) 0.0253(19) 0.037(2) -0.0064(17) -0.0065(18) 0.0019(17) C7 0.0211(19) 0.045(2) 0.0200(19) 0.0007(17) 0.0008(16) 0.0022(17) C8 0.0175(18) 0.030(2) 0.0241(19) 0.0041(15) 0.0037(15) -0.0027(15) C9 0.0203(19) 0.039(2) 0.027(2) 0.0118(17) 0.0038(16) -0.0014(17) C10 0.0198(19) 0.030(2) 0.045(3) 0.0153(18) 0.0087(18) 0.0033(16) C11 0.023(2) 0.0205(18) 0.047(3) 0.0006(17) 0.0112(19) -0.0009(16) C12 0.0221(19) 0.0231(18) 0.033(2) -0.0006(16) 0.0047(17) -0.0014(15) C13 0.033(3) 0.067(3) 0.040(3) -0.020(2) -0.004(2) 0.020(2) C14 0.032(3) 0.094(5) 0.129(6) -0.088(5) 0.000(3) 0.016(3) C15 0.096(6) 0.130(8) 0.116(7) -0.063(6) 0.026(6) -0.028(6) C16 0.100(6) 0.140(8) 0.078(5) -0.067(5) 0.025(5) 0.008(6) C17 0.34(2) 0.183(13) 0.30(2) -0.191(15) 0.21(2) -0.149(15) C18 0.0213(19) 0.0259(19) 0.0213(18) -0.0011(14) 0.0053(15) 0.0011(15) C19 0.0196(19) 0.0284(19) 0.026(2) 0.0013(15) 0.0039(16) 0.0012(15) C20 0.0172(19) 0.037(2) 0.040(2) -0.0003(18) 0.0054(18) 0.0031(17) C21 0.023(2) 0.052(3) 0.053(3) 0.019(2) 0.016(2) 0.001(2) C22 0.026(2) 0.038(2) 0.055(3) 0.021(2) 0.016(2) 0.0047(19) C23 0.0208(19) 0.0307(19) 0.028(2) 0.0051(16) 0.0036(16) 0.0014(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 Br1 Fe1 2.4648(7) . ? Fe1 O3 1.950(3) . ? Fe1 O2 1.969(3) . ? Fe1 N1 2.146(3) . ? Fe1 N3 2.169(3) . ? Fe1 N2 2.266(3) . ? Cl1 C19 1.729(4) . ? Cl2 C20 1.726(4) . ? Cl3 C21 1.735(4) . ? Cl4 C22 1.742(4) . ? O1 C14 1.378(10) . ? O1 C17 1.435(12) . ? O2 C18 1.324(5) . ? O3 C23 1.318(5) . ? N1 C1 1.344(5) . ? N1 C5 1.345(5) . ? N2 C7 1.478(5) . ? N2 C13 1.489(6) . ? N2 C6 1.492(6) . ? N3 C12 1.339(5) . ? N3 C8 1.352(5) . ? C1 C2 1.371(6) . ? C2 C3 1.379(8) . ? C3 C4 1.368(8) . ? C4 C5 1.393(6) . ? C5 C6 1.492(6) . ? C7 C8 1.500(6) . ? C8 C9 1.384(5) . ? C9 C10 1.376(6) . ? C10 C11 1.374(6) . ? C11 C12 1.390(5) . ? C13 C14 1.597(8) . ? C14 C15 1.475(11) . ? C15 C16 1.504(10) . ? C16 C17 1.374(15) . ? C18 C19 1.396(5) . ? C18 C23 1.428(5) . ? C19 C20 1.385(6) . ? C20 C21 1.397(6) . ? C21 C22 1.386(6) . ? C22 C23 1.378(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 O3 Fe1 O2 82.99(11) . . ? O3 Fe1 N1 161.53(13) . . ? O2 Fe1 N1 88.65(11) . . ? O3 Fe1 N3 90.04(11) . . ? O2 Fe1 N3 170.33(11) . . ? N1 Fe1 N3 96.06(12) . . ? O3 Fe1 N2 87.80(13) . . ? O2 Fe1 N2 98.01(12) . . ? N1 Fe1 N2 77.05(13) . . ? N3 Fe1 N2 74.95(12) . . ? O3 Fe1 Br1 100.12(9) . . ? O2 Fe1 Br1 95.25(8) . . ? N1 Fe1 Br1 97.02(9) . . ? N3 Fe1 Br1 92.56(9) . . ? N2 Fe1 Br1 165.31(9) . . ? C14 O1 C17 104.3(9) . . ? C18 O2 Fe1 111.4(2) . . ? C23 O3 Fe1 112.4(2) . . ? C1 N1 C5 119.1(4) . . ? C1 N1 Fe1 123.0(3) . . ? C5 N1 Fe1 117.0(3) . . ? C7 N2 C13 110.9(4) . . ? C7 N2 C6 110.2(3) . . ? C13 N2 C6 112.6(4) . . ? C7 N2 Fe1 104.8(2) . . ? C13 N2 Fe1 109.9(3) . . ? C6 N2 Fe1 108.2(2) . . ? C12 N3 C8 118.5(3) . . ? C12 N3 Fe1 126.3(3) . . ? C8 N3 Fe1 115.2(2) . . ? N1 C1 C2 121.5(4) . . ? C1 C2 C3 119.9(5) . . ? C4 C3 C2 118.8(4) . . ? C3 C4 C5 119.4(5) . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 116.4(4) . . ? C4 C5 C6 122.4(4) . . ? N2 C6 C5 111.4(3) . . ? N2 C7 C8 109.5(3) . . ? N3 C8 C9 122.0(4) . . ? N3 C8 C7 116.3(3) . . ? C9 C8 C7 121.7(4) . . ? C10 C9 C8 118.7(4) . . ? C11 C10 C9 120.1(4) . . ? C10 C11 C12 118.3(4) . . ? N3 C12 C11 122.4(4) . . ? N2 C13 C14 116.0(4) . . ? O1 C14 C15 98.6(7) . . ? O1 C14 C13 100.4(7) . . ? C15 C14 C13 112.6(5) . . ? C14 C15 C16 101.6(7) . . ? C17 C16 C15 104.9(7) . . ? C16 C17 O1 106.0(10) . . ? O2 C18 C19 124.9(3) . . ? O2 C18 C23 116.3(3) . . ? C19 C18 C23 118.8(3) . . ? C20 C19 C18 121.6(4) . . ? C20 C19 Cl1 120.3(3) . . ? C18 C19 Cl1 118.1(3) . . ? C19 C20 C21 119.1(4) . . ? C19 C20 Cl2 120.4(3) . . ? C21 C20 Cl2 120.5(3) . . ? C22 C21 C20 120.0(4) . . ? C22 C21 Cl3 120.4(3) . . ? C20 C21 Cl3 119.7(3) . . ? C23 C22 C21 121.8(4) . . ? C23 C22 Cl4 117.3(3) . . ? C21 C22 Cl4 120.9(3) . . ? O3 C23 C22 125.0(4) . . ? O3 C23 C18 116.3(3) . . ? C22 C23 C18 118.7(4) . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 1.467 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.121 # Attachment '- 6b.CIF' data_16mpksm(6b) _database_code_depnum_ccdc_archive 'CCDC 791687' #TrackingRef '- 6b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Cl4 Fe2 N6 O11' _chemical_formula_weight 964.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.2392(6) _cell_length_b 10.8799(8) _cell_length_c 22.3047(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.5360(10) _cell_angle_gamma 90.00 _cell_volume 1971.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1856 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.6 _exptl_crystal_description BLOCKS _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.6795 _exptl_absorpt_correction_T_max 0.8642 _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 SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11440 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4570 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+8.2974P] 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 4570 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.11890(6) 0.60933(5) 0.04847(2) 0.01499(16) Uani 1 d . . . Cl1 Cl 0.34575(10) 0.64309(9) 0.00454(4) 0.0232(2) Uani 1 d . . . Cl2 Cl 0.25158(13) 0.95369(11) 0.83131(5) 0.0341(3) Uani 1 d . . . O2 O 0.0000 0.5000 0.0000 0.0178(7) Uani 1 d S . . O3 O 0.2612(6) 1.0891(5) 0.8353(3) 0.0853(19) Uani 1 d . . . O5 O 0.0849(5) 0.9294(5) 0.8139(3) 0.093(2) Uani 1 d . . . O6 O 0.3407(5) 0.9164(3) 0.78517(18) 0.0444(9) Uani 1 d . . . N1 N -0.0405(4) 0.7537(3) 0.01315(14) 0.0177(6) Uani 1 d . . . N2 N -0.0606(4) 0.6115(3) 0.11216(14) 0.0195(6) Uani 1 d . . . N3 N 0.2084(4) 0.4707(3) 0.11246(14) 0.0204(6) Uani 1 d . . . C1 C -0.0109(5) 0.8322(4) -0.03029(17) 0.0222(8) Uani 1 d . . . H1 H 0.0908 0.8300 -0.0432 0.027 Uiso 1 calc R . . C2 C -0.1277(5) 0.9163(4) -0.0563(2) 0.0298(9) Uani 1 d . . . H2 H -0.1059 0.9692 -0.0868 0.036 Uiso 1 calc R . . C3 C -0.2777(6) 0.9200(4) -0.0361(2) 0.0339(10) Uani 1 d . . . H3 H -0.3576 0.9765 -0.0525 0.041 Uiso 1 calc R . . C4 C -0.3079(5) 0.8395(4) 0.0084(2) 0.0293(9) Uani 1 d . . . H4 H -0.4079 0.8416 0.0225 0.035 Uiso 1 calc R . . C5 C -0.1877(4) 0.7553(3) 0.03197(17) 0.0203(7) Uani 1 d . . . C6 C -0.2169(4) 0.6568(4) 0.07667(19) 0.0226(8) Uani 1 d . . . H6A H -0.2855 0.6897 0.1043 0.027 Uiso 1 calc R . . H6B H -0.2753 0.5887 0.0548 0.027 Uiso 1 calc R . . C7 C -0.0722(5) 0.4822(4) 0.13192(17) 0.0231(8) Uani 1 d . . . H7A H -0.1436 0.4365 0.1008 0.028 Uiso 1 calc R . . H7B H -0.1198 0.4796 0.1689 0.028 Uiso 1 calc R . . C8 C 0.0968(5) 0.4235(4) 0.14330(17) 0.0221(8) Uani 1 d . . . C9 C 0.1319(6) 0.3212(4) 0.18070(18) 0.0307(9) Uani 1 d . . . H9 H 0.0537 0.2904 0.2024 0.037 Uiso 1 calc R . . C10 C 0.2840(6) 0.2664(4) 0.1850(2) 0.0354(10) Uani 1 d . . . H10 H 0.3096 0.1979 0.2098 0.042 Uiso 1 calc R . . C11 C 0.3978(6) 0.3133(4) 0.1526(2) 0.0335(10) Uani 1 d . . . H11 H 0.5004 0.2764 0.1546 0.040 Uiso 1 calc R . . C12 C 0.3573(5) 0.4161(4) 0.11700(19) 0.0275(9) Uani 1 d . . . H12 H 0.4348 0.4488 0.0955 0.033 Uiso 1 calc R . . C13 C -0.0014(6) 0.6894(5) 0.1662(2) 0.0415(13) Uani 1 d . . . H13A H -0.0962 0.7185 0.1827 0.050 Uiso 1 calc R . . H13B H 0.0636 0.6387 0.1970 0.050 Uiso 1 calc R . . C14 C 0.0948(7) 0.7927(6) 0.1548(2) 0.0449(12) Uani 1 d . . . H14 H 0.0240 0.8553 0.1321 0.054 Uiso 1 calc R . . C15 C 0.1998(6) 0.8514(5) 0.2115(2) 0.0356(10) Uani 1 d . . . H15A H 0.1469 0.9245 0.2241 0.043 Uiso 1 calc R . . H15B H 0.2177 0.7937 0.2451 0.043 Uiso 1 calc R . . O1 O 0.2189(3) 0.7501(3) 0.11824(12) 0.0253(6) Uani 1 d . . . C16 C 0.3604(5) 0.8834(4) 0.19052(19) 0.0289(9) Uani 1 d . . . H16A H 0.3530 0.9621 0.1698 0.035 Uiso 1 calc R . . H16B H 0.4505 0.8860 0.2245 0.035 Uiso 1 calc R . . C17 C 0.3827(5) 0.7797(4) 0.1475(2) 0.0314(9) Uani 1 d . . . H17A H 0.4497 0.8058 0.1179 0.038 Uiso 1 calc R . . H17B H 0.4345 0.7094 0.1695 0.038 Uiso 1 calc R . . O4 O 0.3346(12) 0.9176(10) 0.8880(3) 0.082(4) Uani 0.682(16) d P A 1 O4A O 0.2455(17) 0.8231(15) 0.8670(7) 0.052(6) Uani 0.318(16) d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0112(2) 0.0165(3) 0.0174(3) -0.00170(18) 0.00291(18) -0.00084(18) Cl1 0.0147(4) 0.0279(5) 0.0286(5) -0.0047(4) 0.0079(3) -0.0044(3) Cl2 0.0264(5) 0.0456(7) 0.0297(5) -0.0025(4) 0.0026(4) 0.0124(4) O2 0.0151(16) 0.0189(18) 0.0199(17) -0.0051(14) 0.0040(13) -0.0032(14) O3 0.056(3) 0.061(3) 0.149(5) -0.059(3) 0.047(3) -0.019(2) O5 0.035(2) 0.073(3) 0.173(6) -0.046(4) 0.026(3) -0.016(2) O6 0.051(2) 0.0329(18) 0.056(2) -0.0067(16) 0.0281(18) 0.0000(16) N1 0.0154(13) 0.0186(15) 0.0185(14) -0.0035(11) 0.0009(11) -0.0009(11) N2 0.0148(14) 0.0222(16) 0.0216(15) -0.0050(12) 0.0033(12) -0.0027(12) N3 0.0205(15) 0.0211(16) 0.0192(15) -0.0001(12) 0.0019(12) 0.0017(12) C1 0.0243(18) 0.0215(19) 0.0209(17) -0.0036(14) 0.0039(14) -0.0020(15) C2 0.036(2) 0.022(2) 0.029(2) 0.0023(16) -0.0021(17) -0.0021(17) C3 0.029(2) 0.024(2) 0.045(3) 0.0007(18) -0.0034(19) 0.0068(17) C4 0.0181(18) 0.024(2) 0.045(2) -0.0004(18) 0.0025(17) 0.0060(15) C5 0.0163(16) 0.0190(17) 0.0250(18) -0.0043(14) 0.0019(14) -0.0005(14) C6 0.0136(16) 0.0207(18) 0.035(2) -0.0024(16) 0.0076(15) 0.0013(14) C7 0.0198(17) 0.032(2) 0.0183(17) 0.0046(15) 0.0047(14) -0.0025(15) C8 0.0264(19) 0.0213(18) 0.0173(17) -0.0028(14) -0.0006(14) -0.0008(15) C9 0.038(2) 0.031(2) 0.0206(18) 0.0053(16) -0.0014(17) -0.0025(18) C10 0.051(3) 0.024(2) 0.027(2) 0.0024(17) -0.0054(19) 0.0047(19) C11 0.034(2) 0.027(2) 0.037(2) -0.0046(18) -0.0039(18) 0.0115(18) C12 0.027(2) 0.029(2) 0.027(2) -0.0027(16) 0.0034(16) 0.0063(16) C13 0.034(2) 0.060(3) 0.035(2) -0.028(2) 0.018(2) -0.019(2) C14 0.041(3) 0.049(3) 0.046(3) -0.009(2) 0.012(2) -0.004(2) C15 0.037(2) 0.042(3) 0.028(2) -0.0140(19) 0.0087(18) -0.018(2) O1 0.0173(12) 0.0327(16) 0.0261(14) -0.0097(12) 0.0046(11) -0.0059(11) C16 0.027(2) 0.031(2) 0.027(2) -0.0027(17) -0.0010(16) -0.0064(17) C17 0.0189(18) 0.034(2) 0.037(2) -0.0090(18) -0.0089(16) 0.0006(16) O4 0.106(7) 0.100(8) 0.036(3) 0.003(4) -0.002(4) 0.049(6) O4A 0.049(8) 0.058(10) 0.057(9) 0.037(8) 0.027(7) 0.028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.7868(5) . ? Fe1 N1 2.115(3) . ? Fe1 N3 2.123(3) . ? Fe1 N2 2.214(3) . ? Fe1 O1 2.241(3) . ? Fe1 Cl1 2.2793(10) . ? Cl2 O5 1.389(5) . ? Cl2 O4 1.391(7) . ? Cl2 O6 1.419(3) . ? Cl2 O3 1.477(5) . ? Cl2 O4A 1.634(12) . ? O2 Fe1 1.7868(5) 3_565 ? N1 C1 1.344(5) . ? N1 C5 1.348(5) . ? N2 C6 1.480(5) . ? N2 C7 1.482(5) . ? N2 C13 1.488(5) . ? N3 C8 1.339(5) . ? N3 C12 1.352(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.384(7) . ? C2 H2 0.9300 . ? C3 C4 1.378(7) . ? C3 H3 0.9300 . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 C6 1.510(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.514(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.392(6) . ? C9 C10 1.377(7) . ? C9 H9 0.9300 . ? C10 C11 1.374(7) . ? C10 H10 0.9300 . ? C11 C12 1.381(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.423(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O1 1.483(6) . ? C14 C15 1.547(7) . ? C14 H14 0.9800 . ? C15 C16 1.515(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O1 C17 1.435(5) . ? C16 C17 1.513(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? 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 O2 Fe1 N1 91.42(8) . . ? O2 Fe1 N3 91.63(9) . . ? N1 Fe1 N3 154.62(12) . . ? O2 Fe1 N2 92.17(8) . . ? N1 Fe1 N2 77.96(12) . . ? N3 Fe1 N2 76.75(12) . . ? O2 Fe1 O1 167.65(7) . . ? N1 Fe1 O1 83.40(11) . . ? N3 Fe1 O1 88.40(12) . . ? N2 Fe1 O1 75.82(11) . . ? O2 Fe1 Cl1 104.69(3) . . ? N1 Fe1 Cl1 102.89(9) . . ? N3 Fe1 Cl1 100.68(9) . . ? N2 Fe1 Cl1 163.06(9) . . ? O1 Fe1 Cl1 87.42(7) . . ? O5 Cl2 O4 121.0(6) . . ? O5 Cl2 O6 110.4(3) . . ? O4 Cl2 O6 110.1(4) . . ? O5 Cl2 O3 104.3(3) . . ? O4 Cl2 O3 102.3(6) . . ? O6 Cl2 O3 107.4(3) . . ? O5 Cl2 O4A 82.1(6) . . ? O4 Cl2 O4A 50.3(6) . . ? O6 Cl2 O4A 99.6(5) . . ? O3 Cl2 O4A 147.5(7) . . ? Fe1 O2 Fe1 180.0 3_565 . ? C1 N1 C5 119.8(3) . . ? C1 N1 Fe1 124.4(3) . . ? C5 N1 Fe1 115.4(2) . . ? C6 N2 C7 112.5(3) . . ? C6 N2 C13 112.5(3) . . ? C7 N2 C13 109.2(3) . . ? C6 N2 Fe1 106.0(2) . . ? C7 N2 Fe1 105.3(2) . . ? C13 N2 Fe1 111.2(2) . . ? C8 N3 C12 119.0(4) . . ? C8 N3 Fe1 115.2(3) . . ? C12 N3 Fe1 124.9(3) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 118.6(4) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.6(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.5(3) . . ? N2 C6 C5 111.7(3) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 110.3(3) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C9 121.5(4) . . ? N3 C8 C7 116.3(3) . . ? C9 C8 C7 122.1(4) . . ? C10 C9 C8 119.0(4) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 118.9(4) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N3 C12 C11 121.9(4) . . ? N3 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C14 C13 N2 115.0(4) . . ? C14 C13 H13A 108.5 . . ? N2 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? N2 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 O1 107.9(4) . . ? C13 C14 C15 115.6(5) . . ? O1 C14 C15 103.6(4) . . ? C13 C14 H14 109.8 . . ? O1 C14 H14 109.8 . . ? C15 C14 H14 109.8 . . ? C16 C15 C14 103.9(4) . . ? C16 C15 H15A 111.0 . . ? C14 C15 H15A 111.0 . . ? C16 C15 H15B 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C17 O1 C14 111.3(3) . . ? C17 O1 Fe1 132.7(2) . . ? C14 O1 Fe1 112.8(3) . . ? C17 C16 C15 103.2(3) . . ? C17 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? C17 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.1 . . ? O1 C17 C16 104.6(3) . . ? O1 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O1 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 2.982 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.122