# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1608 data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. John D. Ranford Department of Chemistry National University of Singapore SINGAPORE 119 260 ; _publ_contact_author_phone '(65) 874 2665' _publ_contact_author_fax '(65) 779 1691' _publ_contact_author_email chmjdr@nus.edu.sg _publ_requested_journal 'J. Chem. Soc. Dalton Commun.' _publ_requested_coeditor_name ' ' _publ_contact_letter ; 'Please consider this CIF submission for publication in ''J. Chem. Soc. Dalton Commun.' ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Clusters in bis-tridentate tethered domains of an iron chelating drug' ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Henderson, William' #<--'Last name, first name' ; Department of Chemistry University of Waikato, Private Bag 3105 Hamilton, New Zealand ; 'Koh, Lip, L.' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Ranford, John. D.' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Robinson, Ward T.' ; Department of Chemistry University of Canterbury, PRivate Bag 4800, Christchurch, New Zealand' ; 'Svensson, Jan O.' ; Department of Chemistry University of Canterbury, PRivate Bag 4800, Christchurch, New Zealand' ; 'Vittal, Jagadese J.' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Yan Xu' ; National Institute of Education Bukit Timah Road Singapore 259 756' ; #============================================================================== # 4. TEXT #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== # 5. CHEMICAL DATA data_Complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Fe N4 O6.5' _chemical_formula_weight 547.5 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M P21/c 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 11.135(2) _cell_length_b 19.350(4) _cell_length_c 12.405(2) _cell_angle_alpha 90 _cell_angle_beta 98.48(3) _cell_angle_gamma 90 _cell_volume 2643.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'polyhedra' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type 'N/A' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4951 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 2639 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4696 _reflns_number_gt 2639 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'SHELEXTL' _computing_cell_refinement 'SHELEXTL' _computing_data_reduction 'SHELEXTL' _computing_structure_solution 'SHELEXTL' _computing_structure_refinement 'SHELEXTL' _computing_molecular_graphics 'SHELEXTL' _computing_publication_material 'SHELEXTL' _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^ > 4sigma(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 F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(F)+(0.0002)F^2^]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef -0.00011(7) _refine_ls_extinction_expression 'Fc^*^=Fc[1+0.002xFc^2^\sin(2\q)]^-1/4^' _refine_ls_number_reflns 4696 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.90 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max 1.439 _refine_ls_shift/su_mean 0.011 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 Fe Fe 0.2654(1) 0.6669(1) 0.0755(1) 0.054(1) Uani 1 1 d . . . O1 O 0.1462(4) 0.7331(2) 0.1031(3) 0.070(2) Uani 1 1 d . . . O8 O 0.3805(3) 0.5853(2) 0.0977(3) 0.068(2) Uani 1 1 d . . . O1' O 0.3920(4) 0.7344(2) 0.0980(3) 0.067(2) Uani 1 1 d . . . O8' O 0.1338(3) 0.6022(2) -0.0086(3) 0.064(2) Uani 1 1 d . . . N1 N 0.2436(4) 0.6253(3) 0.2285(4) 0.053(2) Uani 1 1 d . . . N2 N 0.3151(5) 0.5680(3) 0.2619(4) 0.065(2) Uani 1 1 d . . . N1' N 0.2839(4) 0.6783(2) -0.0914(3) 0.044(2) Uani 1 1 d . . . N2' N 0.2085(5) 0.6349(3) -0.1583(4) 0.055(2) Uani 1 1 d . . . C1 C 0.0667(6) 0.7379(3) 0.1740(5) 0.057(3) Uani 1 1 d . . . C2 C -0.0258(6) 0.7873(4) 0.1572(6) 0.077(3) Uani 1 1 d . . . C3 C -0.1053(7) 0.7942(4) 0.2306(7) 0.086(4) Uani 1 1 d . . . C4 C -0.0959(7) 0.7547(4) 0.3225(7) 0.096(4) Uani 1 1 d . . . C5 C -0.0067(7) 0.7067(4) 0.3393(6) 0.083(3) Uani 1 1 d . . . C6 C 0.0770(6) 0.6960(3) 0.2667(5) 0.055(2) Uani 1 1 d . . . C7 C 0.1641(6) 0.6423(3) 0.2898(5) 0.060(3) Uani 1 1 d . . . C8 C 0.3824(6) 0.5509(3) 0.1865(6) 0.065(3) Uani 1 1 d . . . C9 C 0.4576(6) 0.4867(4) 0.2048(6) 0.087(3) Uani 1 1 d . . . C10 C 0.4204(8) 0.4334(4) 0.1092(8) 0.118(5) Uani 1 1 d . . . C11 C 0.2914(9) 0.4134(5) 0.0928(8) 0.123(5) Uani 1 1 d . . . C12 C 0.2563(8) 0.3639(4) -0.0025(9) 0.117(5) Uani 1 1 d . . . C1' C 0.4614(6) 0.7678(3) 0.0368(5) 0.054(2) Uani 1 1 d . . . C2' C 0.5541(6) 0.8117(3) 0.0857(5) 0.076(3) Uani 1 1 d . . . C3' C 0.6253(6) 0.8473(4) 0.0262(6) 0.083(3) Uani 1 1 d . . . C4' C 0.6101(6) 0.8419(3) -0.0850(6) 0.077(3) Uani 1 1 d . . . C5' C 0.5219(6) 0.7997(3) -0.1351(5) 0.064(3) Uani 1 1 d . . . C6' C 0.4452(5) 0.7617(3) -0.0775(4) 0.046(2) Uani 1 1 d . . . C7' C 0.3577(5) 0.7166(3) -0.1353(4) 0.050(2) Uani 1 1 d . . . C8' C 0.1338(6) 0.5955(3) -0.1097(6) 0.059(3) Uani 1 1 d . . . C9' C 0.0554(6) 0.5445(3) -0.1768(5) 0.073(3) Uani 1 1 d . . . C10' C 0.0918(7) 0.4708(4) -0.1421(6) 0.086(3) Uani 1 1 d . . . C11' C 0.2221(8) 0.4563(4) -0.1505(6) 0.095(4) Uani 1 1 d . . . C12' C 0.2673(8) 0.3839(4) -0.1150(8) 0.113(4) Uani 1 1 d . . . O2W O 0.2427(5) 0.6250(2) -0.3768(4) 0.096(2) Uiso 1 1 d PG . . O4W O 0.0154(43) 0.5323(11) -0.5063(18) 0.248(15) Uiso 0.25 1 d PG . . O3W O -0.1214(22) 0.5279(11) -0.4789(30) 0.325(21) Uiso 0.25 1 d PG . . O1W O 0.3681(7) 0.5338(3) -0.5162(4) 0.155(3) Uiso 1 1 d PG . . H2A H -0.0327 0.8171 0.0947 0.090 Uiso 1 1 calc R . . H3A H -0.1709 0.8267 0.2171 0.095 Uiso 1 1 calc R . . H4A H -0.1502 0.7613 0.3749 0.110 Uiso 1 1 calc R . . H5A H 0.0002 0.6783 0.4033 0.095 Uiso 1 1 calc R . . H7A H 0.1638 0.6167 0.3560 0.070 Uiso 1 1 calc R . . H9A H 0.4439 0.4662 0.2724 0.100 Uiso 1 1 calc R . . H9B H 0.5421 0.4984 0.2102 0.100 Uiso 1 1 calc R . . H10A H 0.4682 0.3921 0.1218 0.130 Uiso 1 1 calc R . . H10B H 0.4376 0.4539 0.0426 0.130 Uiso 1 1 calc R . . H11A H 0.2433 0.4547 0.0812 0.150 Uiso 1 1 calc R . . H11B H 0.2743 0.3920 0.1586 0.150 Uiso 1 1 calc R . . H12C H 0.1721 0.3525 -0.0042 0.130 Uiso 1 1 calc R . . H12D H 0.3012 0.3220 0.0152 0.130 Uiso 1 1 calc R . . H2'A H 0.5663 0.8166 0.1636 0.090 Uiso 1 1 calc R . . H3'A H 0.6883 0.8767 0.0623 0.095 Uiso 1 1 calc R . . H4'A H 0.6593 0.8686 -0.1270 0.085 Uiso 1 1 calc R . . H5'A H 0.5125 0.7943 -0.2128 0.080 Uiso 1 1 calc R . . H7'A H 0.3549 0.7140 -0.2130 0.060 Uiso 1 1 calc R . . H9'A H 0.0650 0.5502 -0.2519 0.085 Uiso 1 1 calc R . . H9'B H -0.0281 0.5529 -0.1699 0.085 Uiso 1 1 calc R . . H10C H 0.0424 0.4379 -0.1864 0.100 Uiso 1 1 calc R . . H10D H 0.0790 0.4648 -0.0679 0.100 Uiso 1 1 calc R . . H11C H 0.2708 0.4890 -0.1051 0.120 Uiso 1 1 calc R . . H11D H 0.2345 0.4643 -0.2245 0.120 Uiso 1 1 calc R . . H12A H 0.2227 0.3517 -0.1643 0.130 Uiso 1 1 calc R . . H12B H 0.3516 0.3793 -0.1221 0.130 Uiso 1 1 calc R . . H1N H 0.2186 0.6288 -0.2294 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.073(1) 0.053(1) 0.040(1) 0.004(1) 0.018(1) 0.003(1) O1 0.092(3) 0.070(3) 0.054(3) 0.024(3) 0.027(3) 0.009(2) O8 0.072(3) 0.071(3) 0.068(3) 0.018(2) 0.031(2) 0.017(2) O1' 0.094(3) 0.073(3) 0.037(2) -0.022(3) 0.015(2) -0.007(2) O8' 0.074(3) 0.068(3) 0.053(3) -0.009(2) 0.022(2) -0.001(2) N1 0.060(3) 0.061(3) 0.041(3) 0.002(3) 0.013(3) 0.006(3) N2 0.073(4) 0.068(4) 0.055(3) 0.014(3) 0.013(3) 0.016(3) N1' 0.056(3) 0.041(3) 0.036(3) -0.005(3) 0.004(2) -0.001(2) N2' 0.068(4) 0.056(3) 0.042(3) -0.007(3) 0.010(3) -0.002(3) C1 0.064(5) 0.061(4) 0.045(4) 0.001(4) 0.005(4) -0.011(3) C2 0.077(5) 0.084(5) 0.068(5) 0.024(5) 0.009(4) -0.006(4) C3 0.067(5) 0.098(6) 0.093(6) 0.024(5) 0.011(5) -0.021(5) C4 0.086(6) 0.111(7) 0.102(7) 0.010(5) 0.047(5) -0.022(6) C5 0.096(6) 0.090(6) 0.072(5) 0.003(5) 0.036(5) -0.007(4) C6 0.056(4) 0.063(4) 0.050(4) -0.002(4) 0.015(3) -0.013(3) C7 0.069(5) 0.077(5) 0.035(4) -0.012(4) 0.011(2) 0.003(3) C8 0.068(5) 0.064(5) 0.065(5) 0.008(4) 0.017(4) 0.013(4) C9 0.079(5) 0.093(6) 0.094(6) 0.037(5) 0.028(4) 0.034(5) C10 0.112(8) 0.055(5) 0.204(11) 0.026(5) 0.084(7) 0.010(6) C11 0.140(9) 0.095(7) 0.149(9) 0.022(7) 0.075(7) 0.027(7) C12 0.160(9) 0.049(5) 0.150(9) 0.010(5) 0.051(7) -0.006(6) C1' 0.067(5) 0.047(4) 0.048(4) -0.003(4) 0.007(4) 0.003(3) C2' 0.094(6) 0.076(5) 0.055(4) -0.024(4) 0.002(4) -0.005(4) C3' 0.081(5) 0.092(6) 0.069(5) -0.033(5) -0.006(4) 0.003(4) C4' 0.081(5) 0.077(5) 0.071(5) -0.029(4) 0.009(4) 0.012(4) C5' 0.076(5) 0.069(4) 0.047(4) -0.007(4) 0.011(4) 0.009(3) C6' 0.050(4) 0.048(4) 0.037(3) -0.001(3) 0.002(3) 0.007(3) C7' 0.067(4) 0.046(4) 0.039(4) 0.004(3) 0.013(3) 0.002(3) C8' 0.058(4) 0.056(4) 0.064(5) 0.000(4) 0.009(4) 0.003(4) C9' 0.069(5) 0.073(5) 0.077(5) -0.019(4) 0.008(4) -0.012(4) C10' 0.082(6) 0.075(5) 0.104(6) -0.025(5) 0.021(5) -0.017(5) C11' 0.125(7) 0.071(6) 0.095(6) -0.003(5) 0.034(5) -0.001(5) C12' 0.150(8) 0.075(6) 0.125(8) -0.001(6) 0.059(6) -0.010(5) O2W 0.146(5) 0.086(3) 0.064(3) -0.022(3) 0.039(3) -0.007(3) O4W 0.433(36) 0.185(24) 0.115(12) 0.005(31) 0.006(18) 0.029(17) O3W 0.274(27) 0.123(18) 0.551(50) 0.004(19) -0.023(27) -0.045(20) O1W 0.251(7) 0.133(5) 0.082(4) 0.037(5) 0.026(4) 0.029(4) _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. ; _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full ? _refine_diff_density_max 0.54 _refine_diff_density_min -0.32 _refine_diff_density_rms ? data_Complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H56 Cl2 Fe2 N12 O14' _chemical_formula_weight 1159.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9265(3) _cell_length_b 13.6996(3) _cell_length_c 18.6798(2) _cell_angle_alpha 72.145(1) _cell_angle_beta 85.219(1) _cell_angle_gamma 87.090(1) _cell_volume 2893.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4849 _cell_measurement_theta_min 0.7385 _cell_measurement_theta_max 0.9044 _exptl_crystal_description 'rectangular thin plates' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type 'semiempirical(Sheldrick, 1996)' _exptl_absorpt_correction_T_min 2.20 _exptl_absorpt_correction_T_max 25.0 _exptl_absorpt_process_details '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 'Siemens SMART CCD System' _diffrn_measurement_method 'frames \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14448 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9630 _reflns_number_gt 6497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (Siemens, 1996)' _computing_molecular_graphics 'SHELXTL (Siemens, 1996)' _computing_publication_material 'SHELXTL (Siemens, 1996)' _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^)+(0.1228P)^2^+8.5245P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9630 _refine_ls_number_parameters 683 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2608 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.26590(9) 0.81472(7) 0.17249(5) 0.0485(3) Uani 1 1 d . . . Fe1A Fe 0.25178(7) 0.22377(6) 0.47626(5) 0.0405(3) Uani 1 1 d . . . O1 O 0.2988(5) 0.9557(3) 0.1188(3) 0.0578(13) Uani 1 1 d . . . C1 C 0.3222(6) 1.0075(5) 0.0482(4) 0.0476(16) Uani 1 1 d . . . C2 C 0.3090(7) 1.1157(5) 0.0280(4) 0.0575(19) Uani 1 1 d . . . N3 N 0.3333(6) 1.1741(5) -0.0419(4) 0.0676(19) Uani 1 1 d . . . C4 C 0.3708(7) 1.1318(6) -0.0951(5) 0.066(2) Uani 1 1 d . . . H4 H 0.3892 1.1750 -0.1434 0.079 Uiso 1 1 calc R . . C5 C 0.3840(6) 1.0282(6) -0.0826(4) 0.0518(18) Uani 1 1 d . . . C6 C 0.3596(6) 0.9626(5) -0.0077(4) 0.0449(16) Uani 1 1 d . . . C7 C 0.3732(6) 0.8533(5) 0.0082(4) 0.0494(17) Uani 1 1 d . . . H7 H 0.4089 0.8276 -0.0287 0.059 Uiso 1 1 calc R . . N1 N 0.3382(5) 0.7894(4) 0.0714(3) 0.0497(14) Uani 1 1 d . . . N2 N 0.3576(6) 0.6855(4) 0.0803(3) 0.0639(18) Uani 1 1 d . . . H2 H 0.3973 0.6636 0.0475 0.077 Uiso 1 1 calc R . . C8 C 0.3103(7) 0.6229(6) 0.1431(4) 0.060(2) Uani 1 1 d . . . O8 O 0.2513(5) 0.6586(4) 0.1890(3) 0.0646(15) Uani 1 1 d . . . C9 C 0.3323(8) 0.5115(5) 0.1558(5) 0.069(2) Uani 1 1 d . . . H9A H 0.4037 0.4928 0.1783 0.082 Uiso 1 1 calc R . . H9B H 0.3396 0.4988 0.1073 0.082 Uiso 1 1 calc R . . C10 C 0.2635(10) 1.1657(7) 0.0853(5) 0.091(3) Uani 1 1 d . . . H10A H 0.2603 1.2387 0.0625 0.137 Uiso 1 1 calc R . . H10B H 0.3117 1.1488 0.1263 0.137 Uiso 1 1 calc R . . H10C H 0.1892 1.1417 0.1039 0.137 Uiso 1 1 calc R . . C11 C 0.4242(8) 0.9867(7) -0.1464(5) 0.072(2) Uani 1 1 d . . . H11A H 0.4373 1.0434 -0.1921 0.086 Uiso 1 1 calc R . . H11B H 0.4951 0.9495 -0.1350 0.086 Uiso 1 1 calc R . . C12 C 0.2432(7) 0.4422(5) 0.2056(5) 0.061(2) Uani 1 1 d . . . H12A H 0.1697 0.4650 0.1871 0.073 Uiso 1 1 calc R . . H12B H 0.2426 0.4464 0.2566 0.073 Uiso 1 1 calc R . . O2 O 0.3460(6) 0.9209(6) -0.1587(4) 0.096(2) Uani 1 1 d . . . H2A H 0.2848 0.9510 -0.1658 0.144 Uiso 1 1 calc R . . O1'A O 0.1828(4) 0.2331(4) 0.5716(3) 0.0545(13) Uani 1 1 d . . . C1'A C 0.0976(5) 0.2874(5) 0.5905(4) 0.0443(16) Uani 1 1 d . . . C2'A C 0.0948(6) 0.3001(6) 0.6630(4) 0.0533(18) Uani 1 1 d . . . N3'A N 0.0126(5) 0.3541(5) 0.6870(4) 0.0630(17) Uani 1 1 d . . . C4'A C -0.0710(6) 0.3955(6) 0.6424(5) 0.060(2) Uani 1 1 d . . . H4'A H -0.1282 0.4323 0.6605 0.072 Uiso 1 1 calc R . . C5'A C -0.0769(6) 0.3868(5) 0.5719(4) 0.0466(16) Uani 1 1 d . . . C6'A C 0.0109(5) 0.3321(4) 0.5440(4) 0.0406(15) Uani 1 1 d . . . C7'A C 0.0120(5) 0.3249(5) 0.4688(4) 0.0442(16) Uani 1 1 d . . . H7'A H -0.0505 0.3509 0.4417 0.053 Uiso 1 1 calc R . . N1'A N 0.0931(4) 0.2849(4) 0.4362(3) 0.0414(12) Uani 1 1 d . . . N2'A N 0.0809(5) 0.2916(4) 0.3615(3) 0.0489(14) Uani 1 1 d . . . H2'A H 0.0232 0.3179 0.3370 0.059 Uiso 1 1 calc R . . C8'A C 0.1710(6) 0.2517(5) 0.3335(4) 0.0474(16) Uani 1 1 d . . . O8'A O 0.2546(4) 0.2117(3) 0.3715(3) 0.0517(12) Uani 1 1 d . . . C9'A C 0.1755(7) 0.2573(6) 0.2526(4) 0.060(2) Uani 1 1 d . . . H9'1 H 0.1029 0.2807 0.2329 0.072 Uiso 1 1 calc R . . H9'2 H 0.1917 0.1895 0.2477 0.072 Uiso 1 1 calc R . . C10B C 0.1869(7) 0.2542(8) 0.7139(5) 0.080(3) Uani 1 1 d . . . H10D H 0.1721 0.2696 0.7607 0.120 Uiso 1 1 calc R . . H10E H 0.2576 0.2823 0.6902 0.120 Uiso 1 1 calc R . . H10F H 0.1901 0.1811 0.7236 0.120 Uiso 1 1 calc R . . C11B C -0.1755(6) 0.4338(6) 0.5274(5) 0.061(2) Uani 1 1 d . . . H11C H -0.2205 0.4746 0.5539 0.073 Uiso 1 1 calc R . . H11D H -0.1481 0.4795 0.4790 0.073 Uiso 1 1 calc R . . C12B C 0.2665(7) 0.3309(5) 0.2064(4) 0.062(2) Uani 1 1 d . . . H12C H 0.3385 0.3079 0.2271 0.075 Uiso 1 1 calc R . . H12D H 0.2718 0.3282 0.1549 0.075 Uiso 1 1 calc R . . O2'A O -0.2451(4) 0.3597(4) 0.5151(3) 0.0552(12) Uani 1 1 d . . . H2'1 H -0.2629 0.3170 0.5555 0.083 Uiso 1 1 calc R . . O1' O 0.1057(4) 0.8356(4) 0.1693(3) 0.0583(13) Uani 1 1 d . . . C1' C 0.0446(6) 0.8981(6) 0.1981(4) 0.0537(18) Uani 1 1 d . . . C2' C -0.0506(7) 0.9476(7) 0.1592(4) 0.070(2) Uani 1 1 d . . . N3' N -0.1193(6) 1.0099(7) 0.1842(5) 0.083(2) Uani 1 1 d . . . C4' C -0.0973(8) 1.0297(8) 0.2467(7) 0.091(3) Uani 1 1 d . . . H4' H -0.1446 1.0767 0.2621 0.109 Uiso 1 1 calc R . . C5' C -0.0083(6) 0.9853(6) 0.2914(5) 0.061(2) Uani 1 1 d . . . C6' C 0.0643(6) 0.9156(5) 0.2661(4) 0.0459(16) Uani 1 1 d . . . C7' C 0.1550(5) 0.8649(5) 0.3104(4) 0.0448(16) Uani 1 1 d . . . H7' H 0.1555 0.8666 0.3597 0.054 Uiso 1 1 calc R . . N1' N 0.2360(4) 0.8169(4) 0.2839(3) 0.0407(12) Uani 1 1 d . . . N2' N 0.3191(5) 0.7698(4) 0.3317(3) 0.0431(13) Uani 1 1 d . . . H2' H 0.3138 0.7553 0.3800 0.052 Uiso 1 1 calc R . . C8' C 0.4072(6) 0.7514(4) 0.2904(4) 0.0441(16) Uani 1 1 d . . . O8' O 0.4124(4) 0.7767(4) 0.2188(3) 0.0591(13) Uani 1 1 d . . . C9' C 0.5104(6) 0.6998(5) 0.3292(4) 0.0498(17) Uani 1 1 d . . . H9'3 H 0.4930 0.6772 0.3833 0.060 Uiso 1 1 calc R . . H9'4 H 0.5702 0.7488 0.3182 0.060 Uiso 1 1 calc R . . C10' C -0.0770(9) 0.9251(10) 0.0876(5) 0.105(4) Uani 1 1 d . . . H10G H -0.1431 0.9638 0.0682 0.158 Uiso 1 1 calc R . . H10H H -0.0899 0.8532 0.0988 0.158 Uiso 1 1 calc R . . H10I H -0.0146 0.9440 0.0507 0.158 Uiso 1 1 calc R . . C11' C 0.0137(8) 1.0164(6) 0.3602(5) 0.078(3) Uani 1 1 d . . . H11E H 0.0920 1.0341 0.3575 0.094 Uiso 1 1 calc R . . H11F H -0.0326 1.0763 0.3612 0.094 Uiso 1 1 calc R . . C12' C 0.5507(6) 0.6079(5) 0.3033(4) 0.0531(18) Uani 1 1 d . . . H12E H 0.6252 0.5863 0.3204 0.064 Uiso 1 1 calc R . . H12F H 0.5567 0.6287 0.2487 0.064 Uiso 1 1 calc R . . O2' O -0.0106(5) 0.9370(5) 0.4251(4) 0.0747(16) Uani 1 1 d . . . H2'2 H -0.0783 0.9266 0.4298 0.112 Uiso 1 1 calc R . . O1A O 0.2588(4) 0.0738(3) 0.5099(3) 0.0536(13) Uani 1 1 d . . . C1A C 0.3226(5) 0.0043(4) 0.5537(4) 0.0391(14) Uani 1 1 d . . . C2A C 0.2932(5) -0.1000(5) 0.5702(4) 0.0436(16) Uani 1 1 d . . . N3A N 0.3538(5) -0.1727(4) 0.6175(3) 0.0483(14) Uani 1 1 d . . . C4A C 0.4422(6) -0.1510(5) 0.6510(4) 0.0522(18) Uani 1 1 d . . . H4A H 0.4785 -0.2040 0.6859 0.063 Uiso 1 1 calc R . . C5A C 0.4787(6) -0.0536(5) 0.6349(4) 0.0425(15) Uani 1 1 d . . . C6A C 0.4200(5) 0.0269(4) 0.5827(3) 0.0373(14) Uani 1 1 d . . . C7A C 0.4681(6) 0.1274(5) 0.5574(4) 0.0417(15) Uani 1 1 d . . . H7A H 0.5364 0.1365 0.5748 0.050 Uiso 1 1 calc R . . N1A N 0.4189(4) 0.2060(4) 0.5110(3) 0.0386(12) Uani 1 1 d . . . N2A N 0.4797(4) 0.2952(4) 0.4875(3) 0.0464(14) Uani 1 1 d . . . H2A1 H 0.5482 0.2997 0.4970 0.056 Uiso 1 1 calc R . . C8A C 0.4176(6) 0.3718(5) 0.4485(4) 0.0445(16) Uani 1 1 d . . . O8A O 0.3159(4) 0.3626(3) 0.4353(3) 0.0490(12) Uani 1 1 d . . . C9A C 0.4696(6) 0.4744(5) 0.4179(4) 0.0438(15) Uani 1 1 d . . . H9A1 H 0.5459 0.4691 0.4332 0.053 Uiso 1 1 calc R . . H9A2 H 0.4276 0.5222 0.4398 0.053 Uiso 1 1 calc R . . C10A C 0.2008(6) -0.1326(5) 0.5349(5) 0.0570(19) Uani 1 1 d . . . H10J H 0.1950 -0.2059 0.5539 0.085 Uiso 1 1 calc R . . H10K H 0.2165 -0.1124 0.4812 0.085 Uiso 1 1 calc R . . H10L H 0.1312 -0.1008 0.5468 0.085 Uiso 1 1 calc R . . C11A C 0.5773(6) -0.0350(5) 0.6737(4) 0.0521(18) Uani 1 1 d . . . H11G H 0.5562 0.0185 0.6968 0.063 Uiso 1 1 calc R . . H11H H 0.5940 -0.0971 0.7138 0.063 Uiso 1 1 calc R . . C12A C 0.4722(6) 0.5168(5) 0.3330(4) 0.0483(17) Uani 1 1 d . . . H12G H 0.3967 0.5387 0.3180 0.058 Uiso 1 1 calc R . . H12H H 0.4977 0.4634 0.3109 0.058 Uiso 1 1 calc R . . O2A O 0.6742(5) -0.0064(4) 0.6266(3) 0.0694(15) Uani 1 1 d . . . H2A2 H 0.6917 -0.0503 0.6058 0.104 Uiso 1 1 calc R . . Cl1 Cl 0.2893(5) 0.6338(4) 0.6342(3) 0.0993(16) Uani 0.50 1 d P . . Cl2 Cl 0.5243(13) 0.6090(11) -0.0118(8) 0.111(4) Uani 0.25 1 d P . . Cl3 Cl -0.0957(11) 0.3914(11) 0.2717(8) 0.103(4) Uani 0.25 1 d P . . Cl4 Cl 0.0437(11) 0.4020(10) 0.8175(8) 0.112(2) Uiso 0.25 1 d P . . Cl5 Cl 0.4318(12) 0.7205(11) -0.1576(8) 0.112(2) Uiso 0.25 1 d P . . Cl6 Cl -0.0867(15) 0.4310(13) 0.2869(10) 0.112(2) Uiso 0.25 1 d P . . Cl7 Cl 0.4704(14) 0.6110(14) -0.0315(10) 0.112(2) Uiso 0.25 1 d P . . O1S O 0.0126(13) 0.3678(12) 0.8363(6) 0.082(3) Uiso 0.20 1 d PG . . O2S O 0.7670(9) 0.6276(11) 0.1036(6) 0.082(3) Uiso 0.20 1 d PG . . O3S O 0.7390(9) 0.6194(11) 0.1161(6) 0.082(3) Uiso 0.20 1 d PG . . O4S O 0.3598(13) 0.5618(16) -0.1940(7) 0.082(3) Uiso 0.20 1 d PG . . O5S O -0.0975(15) 0.3706(14) 0.9544(7) 0.082(3) Uiso 0.20 1 d PG . . O6S O 0.6896(9) 0.6105(9) 0.0631(6) 0.082(3) Uiso 0.20 1 d PG . . O7S O -0.1128(16) 0.5722(15) 0.9737(7) 0.082(3) Uiso 0.20 1 d PG . . O8S O 0.3846(12) 0.7145(14) -0.1685(6) 0.082(3) Uiso 0.20 1 d PG . . O9S O 0.5151(10) 0.6539(9) -0.0312(6) 0.082(3) Uiso 0.20 1 d PG . . O10S O 0.4752(12) 0.7566(12) -0.1617(6) 0.082(3) Uiso 0.20 1 d PG . . 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 0.0559(6) 0.0462(6) 0.0383(6) -0.0090(4) 0.0043(4) 0.0085(5) Fe1A 0.0357(5) 0.0309(5) 0.0493(6) -0.0059(4) 0.0009(4) 0.0054(4) O1 0.084(4) 0.044(3) 0.043(3) -0.013(2) 0.003(3) 0.009(2) C1 0.053(4) 0.046(4) 0.042(4) -0.013(3) 0.000(3) 0.002(3) C2 0.082(6) 0.041(4) 0.051(4) -0.016(3) -0.007(4) 0.002(4) N3 0.092(5) 0.044(4) 0.058(4) -0.003(3) 0.000(4) -0.002(3) C4 0.082(6) 0.050(5) 0.057(5) -0.004(4) 0.005(4) -0.010(4) C5 0.050(4) 0.057(4) 0.044(4) -0.008(3) 0.003(3) -0.005(3) C6 0.045(4) 0.050(4) 0.035(4) -0.007(3) 0.000(3) -0.001(3) C7 0.060(4) 0.049(4) 0.038(4) -0.014(3) 0.001(3) 0.007(3) N1 0.063(4) 0.037(3) 0.044(3) -0.008(3) 0.005(3) 0.005(3) N2 0.092(5) 0.043(3) 0.051(4) -0.013(3) 0.020(3) 0.007(3) C8 0.076(5) 0.045(4) 0.057(5) -0.015(4) 0.000(4) 0.009(4) O8 0.088(4) 0.044(3) 0.055(3) -0.011(2) 0.022(3) 0.003(3) C9 0.097(7) 0.042(4) 0.060(5) -0.013(4) 0.014(5) 0.003(4) C10 0.142(10) 0.053(5) 0.078(6) -0.026(5) 0.005(6) 0.015(5) C11 0.092(7) 0.067(5) 0.051(5) -0.010(4) 0.003(4) -0.022(5) C12 0.077(5) 0.043(4) 0.060(5) -0.014(4) 0.011(4) -0.001(4) O2 0.093(5) 0.118(6) 0.087(5) -0.045(4) -0.027(4) 0.034(4) O1'A 0.046(3) 0.061(3) 0.047(3) -0.006(2) 0.001(2) 0.018(2) C1'A 0.043(4) 0.039(4) 0.046(4) -0.008(3) 0.010(3) -0.006(3) C2'A 0.043(4) 0.059(4) 0.058(5) -0.019(4) 0.002(3) -0.008(3) N3'A 0.052(4) 0.079(5) 0.066(4) -0.036(4) 0.001(3) -0.001(3) C4'A 0.051(5) 0.059(5) 0.076(6) -0.034(4) 0.011(4) -0.003(4) C5'A 0.043(4) 0.035(3) 0.063(5) -0.020(3) 0.008(3) -0.001(3) C6'A 0.040(4) 0.028(3) 0.050(4) -0.008(3) 0.006(3) 0.001(3) C7'A 0.038(4) 0.032(3) 0.059(4) -0.008(3) -0.005(3) 0.004(3) N1'A 0.038(3) 0.040(3) 0.042(3) -0.008(2) 0.004(2) 0.000(2) N2'A 0.051(3) 0.045(3) 0.047(3) -0.007(3) -0.009(3) 0.006(3) C8'A 0.057(4) 0.033(3) 0.051(4) -0.012(3) 0.001(3) -0.002(3) O8'A 0.052(3) 0.045(3) 0.054(3) -0.014(2) -0.002(2) 0.015(2) C9'A 0.083(6) 0.049(4) 0.049(4) -0.017(3) 0.003(4) -0.006(4) C10B 0.062(5) 0.115(8) 0.065(6) -0.030(5) -0.005(4) -0.007(5) C11B 0.043(4) 0.054(4) 0.087(6) -0.029(4) 0.003(4) 0.008(3) C12B 0.091(6) 0.041(4) 0.055(5) -0.017(3) 0.005(4) 0.001(4) O2'A 0.047(3) 0.056(3) 0.062(3) -0.018(3) 0.002(2) -0.004(2) O1' 0.054(3) 0.070(3) 0.053(3) -0.024(3) -0.005(2) 0.012(3) C1' 0.048(4) 0.054(4) 0.053(4) -0.006(3) -0.002(3) 0.001(3) C2' 0.063(5) 0.084(6) 0.051(5) -0.006(4) -0.007(4) 0.017(5) N3' 0.071(5) 0.104(6) 0.074(5) -0.026(5) -0.023(4) 0.033(4) C4' 0.069(6) 0.084(7) 0.121(9) -0.037(6) -0.013(6) 0.040(5) C5' 0.052(5) 0.064(5) 0.068(5) -0.025(4) 0.004(4) 0.010(4) C6' 0.041(4) 0.041(4) 0.053(4) -0.011(3) -0.001(3) 0.003(3) C7' 0.041(4) 0.045(4) 0.046(4) -0.012(3) 0.005(3) 0.001(3) N1' 0.041(3) 0.040(3) 0.037(3) -0.006(2) 0.000(2) 0.002(2) N2' 0.054(3) 0.041(3) 0.032(3) -0.009(2) -0.002(3) 0.008(3) C8' 0.050(4) 0.027(3) 0.051(4) -0.005(3) -0.003(3) 0.003(3) O8' 0.052(3) 0.067(3) 0.046(3) -0.004(2) 0.009(2) 0.016(2) C9' 0.044(4) 0.037(4) 0.062(5) -0.007(3) 0.002(3) -0.003(3) C10' 0.090(7) 0.164(11) 0.050(5) -0.017(6) -0.018(5) 0.032(7) C11' 0.076(6) 0.057(5) 0.092(7) -0.020(5) 0.023(5) 0.018(4) C12' 0.051(4) 0.035(4) 0.062(5) -0.003(3) 0.008(3) 0.010(3) O2' 0.062(4) 0.076(4) 0.086(4) -0.026(3) 0.003(3) -0.001(3) O1A 0.051(3) 0.030(2) 0.074(3) -0.005(2) -0.020(2) 0.006(2) C1A 0.041(4) 0.031(3) 0.044(4) -0.010(3) -0.001(3) 0.008(3) C2A 0.042(4) 0.034(3) 0.051(4) -0.010(3) 0.004(3) 0.003(3) N3A 0.053(3) 0.036(3) 0.052(3) -0.008(3) -0.003(3) 0.007(3) C4A 0.063(5) 0.034(4) 0.050(4) -0.001(3) -0.003(4) 0.012(3) C5A 0.050(4) 0.037(3) 0.038(3) -0.008(3) -0.005(3) 0.008(3) C6A 0.042(4) 0.033(3) 0.035(3) -0.011(3) 0.007(3) 0.004(3) C7A 0.042(4) 0.040(4) 0.043(4) -0.013(3) -0.006(3) 0.012(3) N1A 0.036(3) 0.034(3) 0.044(3) -0.011(2) 0.003(2) -0.001(2) N2A 0.038(3) 0.037(3) 0.056(4) -0.002(3) -0.008(3) -0.003(2) C8A 0.047(4) 0.036(3) 0.050(4) -0.011(3) -0.004(3) 0.002(3) O8A 0.044(3) 0.030(2) 0.066(3) -0.004(2) -0.006(2) 0.0036(19) C9A 0.044(4) 0.035(3) 0.050(4) -0.009(3) 0.000(3) -0.002(3) C10A 0.058(5) 0.039(4) 0.074(5) -0.017(4) -0.008(4) 0.004(3) C11A 0.054(4) 0.046(4) 0.051(4) -0.009(3) -0.004(3) 0.011(3) C12A 0.056(4) 0.038(4) 0.045(4) -0.007(3) 0.000(3) 0.003(3) O2A 0.067(4) 0.059(3) 0.087(4) -0.030(3) -0.009(3) 0.009(3) Cl1 0.103(4) 0.069(3) 0.121(4) -0.021(3) -0.012(3) 0.002(3) Cl2 0.129(12) 0.094(8) 0.103(10) -0.026(7) -0.001(8) 0.021(8) Cl3 0.091(8) 0.127(11) 0.105(9) -0.054(8) -0.026(6) 0.016(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' 1.920(5) . ? Fe1 O1 1.927(5) . ? Fe1 O8' 1.989(5) . ? Fe1 O8 2.079(5) . ? Fe1 N1' 2.092(5) . ? Fe1 N1 2.129(6) . ? Fe1A O1'A 1.937(5) . ? Fe1A O1A 1.955(4) . ? Fe1A O8A 1.987(4) . ? Fe1A O8'A 2.012(5) . ? Fe1A N1A 2.127(5) . ? Fe1A N1'A 2.129(5) . ? O1 C1 1.305(8) . ? C1 C6 1.399(9) . ? C1 C2 1.417(9) . ? C2 N3 1.323(9) . ? C2 C10 1.490(11) . ? N3 C4 1.334(10) . ? C4 C5 1.368(10) . ? C5 C6 1.427(9) . ? C5 C11 1.505(11) . ? C6 C7 1.438(9) . ? C7 N1 1.286(8) . ? N1 N2 1.390(8) . ? N2 C8 1.323(9) . ? C8 O8 1.263(9) . ? C8 C9 1.483(10) . ? C9 C12 1.514(11) . ? C11 O2 1.408(10) . ? C12 C12B 1.532(10) . ? O1'A C1'A 1.317(8) . ? C1'A C6'A 1.400(9) . ? C1'A C2'A 1.415(10) . ? C2'A N3'A 1.328(9) . ? C2'A C10B 1.499(11) . ? N3'A C4'A 1.342(10) . ? C4'A C5'A 1.365(10) . ? C5'A C6'A 1.413(9) . ? C5'A C11B 1.499(10) . ? C6'A C7'A 1.436(9) . ? C7'A N1'A 1.288(8) . ? N1'A N2'A 1.390(7) . ? N2'A C8'A 1.322(9) . ? C8'A O8'A 1.274(8) . ? C8'A C9'A 1.486(10) . ? C9'A C12B 1.536(10) . ? C11B O2'A 1.426(9) . ? O1' C1' 1.307(9) . ? C1' C6' 1.403(10) . ? C1' C2' 1.427(10) . ? C2' N3' 1.316(11) . ? C2' C10' 1.522(13) . ? N3' C4' 1.325(12) . ? C4' C5' 1.400(12) . ? C5' C6' 1.417(10) . ? C5' C11' 1.519(12) . ? C6' C7' 1.435(9) . ? C7' N1' 1.289(8) . ? N1' N2' 1.387(7) . ? N2' C8' 1.311(8) . ? C8' O8' 1.272(8) . ? C8' C9' 1.512(9) . ? C9' C12' 1.523(9) . ? C11' O2' 1.378(10) . ? C12' C12A 1.533(9) . ? O1A C1A 1.306(7) . ? C1A C6A 1.408(9) . ? C1A C2A 1.422(8) . ? C2A N3A 1.337(8) . ? C2A C10A 1.483(10) . ? N3A C4A 1.360(9) . ? C4A C5A 1.361(9) . ? C5A C6A 1.426(8) . ? C5A C11A 1.503(10) . ? C6A C7A 1.444(9) . ? C7A N1A 1.304(8) . ? N1A N2A 1.386(7) . ? N2A C8A 1.312(8) . ? C8A O8A 1.277(8) . ? C8A C9A 1.492(9) . ? C9A C12A 1.510(9) . ? C11A O2A 1.389(9) . ? Cl2 O9S 0.620(17) . ? Cl2 Cl7 0.763(18) . ? Cl3 Cl6 0.701(16) . ? Cl4 O1S 0.612(18) . ? Cl5 O8S 0.632(18) . ? Cl5 O10S 0.716(19) . ? Cl5 Cl7 2.44(2) . ? Cl7 O9S 0.82(2) . ? O2S O6S 1.3133 . ? O3S O6S 1.2337 . ? O8S O10S 1.2829 . ? 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 O1 94.4(2) . . ? O1' Fe1 O8' 157.3(2) . . ? O1 Fe1 O8' 97.1(2) . . ? O1' Fe1 O8 91.1(2) . . ? O1 Fe1 O8 157.5(2) . . ? O8' Fe1 O8 85.7(2) . . ? O1' Fe1 N1' 84.1(2) . . ? O1 Fe1 N1' 102.7(2) . . ? O8' Fe1 N1' 74.3(2) . . ? O8 Fe1 N1' 99.5(2) . . ? O1' Fe1 N1 110.8(2) . . ? O1 Fe1 N1 83.1(2) . . ? O8' Fe1 N1 90.0(2) . . ? O8 Fe1 N1 74.6(2) . . ? N1' Fe1 N1 163.8(2) . . ? O1'A Fe1A O1A 93.8(2) . . ? O1'A Fe1A O8A 99.7(2) . . ? O1A Fe1A O8A 154.8(2) . . ? O1'A Fe1A O8'A 155.9(2) . . ? O1A Fe1A O8'A 85.7(2) . . ? O8A Fe1A O8'A 90.4(2) . . ? O1'A Fe1A N1A 94.9(2) . . ? O1A Fe1A N1A 82.81(19) . . ? O8A Fe1A N1A 74.95(19) . . ? O8'A Fe1A N1A 108.96(19) . . ? O1'A Fe1A N1'A 83.3(2) . . ? O1A Fe1A N1'A 112.91(19) . . ? O8A Fe1A N1'A 89.88(19) . . ? O8'A Fe1A N1'A 74.8(2) . . ? N1A Fe1A N1'A 164.24(19) . . ? C1 O1 Fe1 135.0(4) . . ? O1 C1 C6 123.9(6) . . ? O1 C1 C2 117.3(6) . . ? C6 C1 C2 118.8(6) . . ? N3 C2 C1 121.2(7) . . ? N3 C2 C10 118.6(7) . . ? C1 C2 C10 120.2(7) . . ? C2 N3 C4 120.3(7) . . ? N3 C4 C5 123.6(7) . . ? C4 C5 C6 117.8(7) . . ? C4 C5 C11 120.2(7) . . ? C6 C5 C11 122.0(7) . . ? C1 C6 C5 118.3(6) . . ? C1 C6 C7 121.9(6) . . ? C5 C6 C7 119.8(6) . . ? N1 C7 C6 122.9(6) . . ? C7 N1 N2 117.4(6) . . ? C7 N1 Fe1 130.6(5) . . ? N2 N1 Fe1 111.7(4) . . ? C8 N2 N1 115.0(6) . . ? O8 C8 N2 120.2(7) . . ? O8 C8 C9 123.3(7) . . ? N2 C8 C9 116.6(7) . . ? C8 O8 Fe1 115.6(5) . . ? C8 C9 C12 115.2(7) . . ? O2 C11 C5 112.1(7) . . ? C9 C12 C12B 110.6(6) . . ? C1'A O1'A Fe1A 133.8(4) . . ? O1'A C1'A C6'A 124.4(6) . . ? O1'A C1'A C2'A 117.0(6) . . ? C6'A C1'A C2'A 118.7(6) . . ? N3'A C2'A C1'A 121.4(7) . . ? N3'A C2'A C10B 118.5(7) . . ? C1'A C2'A C10B 120.1(7) . . ? C2'A N3'A C4'A 119.5(7) . . ? N3'A C4'A C5'A 123.7(7) . . ? C4'A C5'A C6'A 118.1(7) . . ? C4'A C5'A C11B 119.5(6) . . ? C6'A C5'A C11B 122.4(7) . . ? C1'A C6'A C5'A 118.6(6) . . ? C1'A C6'A C7'A 120.9(6) . . ? C5'A C6'A C7'A 120.5(6) . . ? N1'A C7'A C6'A 124.9(6) . . ? C7'A N1'A N2'A 115.8(6) . . ? C7'A N1'A Fe1A 129.2(5) . . ? N2'A N1'A Fe1A 114.6(4) . . ? C8'A N2'A N1'A 110.2(6) . . ? O8'A C8'A N2'A 123.5(6) . . ? O8'A C8'A C9'A 118.7(6) . . ? N2'A C8'A C9'A 117.7(7) . . ? C8'A O8'A Fe1A 116.5(4) . . ? C8'A C9'A C12B 111.0(6) . . ? O2'A C11B C5'A 113.2(6) . . ? C12 C12B C9'A 113.3(7) . . ? C1' O1' Fe1 125.6(5) . . ? O1' C1' C6' 124.0(6) . . ? O1' C1' C2' 117.4(7) . . ? C6' C1' C2' 118.5(7) . . ? N3' C2' C1' 122.4(8) . . ? N3' C2' C10' 118.2(8) . . ? C1' C2' C10' 119.3(8) . . ? C2' N3' C4' 118.7(7) . . ? N3' C4' C5' 125.1(8) . . ? C4' C5' C6' 116.6(8) . . ? C4' C5' C11' 121.4(8) . . ? C6' C5' C11' 121.8(7) . . ? C1' C6' C5' 118.6(7) . . ? C1' C6' C7' 121.8(6) . . ? C5' C6' C7' 119.6(7) . . ? N1' C7' C6' 122.1(6) . . ? C7' N1' N2' 117.4(5) . . ? C7' N1' Fe1 127.0(5) . . ? N2' N1' Fe1 115.3(4) . . ? C8' N2' N1' 108.2(5) . . ? O8' C8' N2' 123.8(6) . . ? O8' C8' C9' 117.4(6) . . ? N2' C8' C9' 118.8(6) . . ? C8' O8' Fe1 115.4(4) . . ? C8' C9' C12' 111.4(6) . . ? O2' C11' C5' 110.2(7) . . ? C9' C12' C12A 113.0(6) . . ? C1A O1A Fe1A 134.8(4) . . ? O1A C1A C6A 123.6(6) . . ? O1A C1A C2A 117.4(6) . . ? C6A C1A C2A 118.9(5) . . ? N3A C2A C1A 118.9(6) . . ? N3A C2A C10A 118.1(6) . . ? C1A C2A C10A 122.9(6) . . ? C2A N3A C4A 122.7(6) . . ? N3A C4A C5A 121.6(6) . . ? C4A C5A C6A 118.3(6) . . ? C4A C5A C11A 118.9(6) . . ? C6A C5A C11A 122.8(6) . . ? C1A C6A C5A 119.2(6) . . ? C1A C6A C7A 122.5(6) . . ? C5A C6A C7A 118.1(6) . . ? N1A C7A C6A 122.2(6) . . ? C7A N1A N2A 115.3(5) . . ? C7A N1A Fe1A 129.8(4) . . ? N2A N1A Fe1A 114.4(4) . . ? C8A N2A N1A 110.2(5) . . ? O8A C8A N2A 123.4(6) . . ? O8A C8A C9A 118.7(6) . . ? N2A C8A C9A 117.8(6) . . ? C8A O8A Fe1A 117.0(4) . . ? C8A C9A C12A 113.3(6) . . ? O2A C11A C5A 114.3(6) . . ? C9A C12A C12' 111.1(6) . . ? O9S Cl2 Cl7 71(2) . . ? O8S Cl5 O10S 144(4) . . ? O8S Cl5 Cl7 115(2) . . ? O10S Cl5 Cl7 97.3(16) . . ? Cl2 Cl7 O9S 46.1(17) . . ? Cl2 Cl7 Cl5 126(2) . . ? O9S Cl7 Cl5 86.4(16) . . ? O3S O6S O2S 17.3 . . ? Cl5 O8S O10S 19(2) . . ? Cl2 O9S Cl7 62.4(19) . . ? Cl5 O10S O8S 16.8(17) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.823 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.102 #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./