# 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_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Sujoy Baitalik' _publ_contact_author_email sbaitalik@hotmail.com _publ_section_title ; A terpyridyl-imidazole (tpy-HImzPh3) based bifunctional receptor for multichannel detection of Fe2+ and F- ions ; loop_ _publ_author_name S.Baitalik C.Bhaumik S.Das D.Maity # Attachment '- Receptor.cif' data_benzil _database_code_depnum_ccdc_archive 'CCDC 817562' #TrackingRef '- Receptor.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 N5' _chemical_formula_weight 527.61 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 14.6483(15) _cell_length_b 18.3958(19) _cell_length_c 10.1403(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.376(7) _cell_angle_gamma 90.00 _cell_volume 2727.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4094 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 20.68 _exptl_crystal_description prism _exptl_crystal_colour gray _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 36568 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.11 _reflns_number_total 4830 _reflns_number_gt 3106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6026P] 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 4830 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _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 C1 C 0.38614(17) 0.16483(15) 0.7748(2) 0.0547(7) Uani 1 1 d . . . H1 H 0.3698 0.2121 0.7511 0.066 Uiso 1 1 calc R . . C2 C 0.32831(19) 0.12381(17) 0.8471(3) 0.0656(8) Uani 1 1 d . . . H2 H 0.2732 0.1433 0.8717 0.079 Uiso 1 1 calc R . . C3 C 0.3522(2) 0.05426(17) 0.8825(3) 0.0662(8) Uani 1 1 d . . . H3 H 0.3127 0.0263 0.9301 0.079 Uiso 1 1 calc R . . C4 C 0.4333(2) 0.02584(15) 0.8486(3) 0.0671(8) Uani 1 1 d . . . H4 H 0.4495 -0.0212 0.8742 0.081 Uiso 1 1 calc R . . C5 C 0.49209(19) 0.06707(14) 0.7753(3) 0.0596(7) Uani 1 1 d . . . H5 H 0.5475 0.0475 0.7524 0.072 Uiso 1 1 calc R . . C6 C 0.46826(16) 0.13674(12) 0.7369(2) 0.0435(6) Uani 1 1 d . . . C7 C 0.52687(14) 0.18088(12) 0.6537(2) 0.0399(5) Uani 1 1 d . . . C8 C 0.51608(15) 0.19233(12) 0.5200(2) 0.0410(5) Uani 1 1 d . . . C9 C 0.44921(17) 0.16630(13) 0.4166(2) 0.0495(6) Uani 1 1 d . . . C10 C 0.35693(19) 0.16543(18) 0.4359(3) 0.0763(9) Uani 1 1 d . . . H10 H 0.3364 0.1788 0.5174 0.092 Uiso 1 1 calc R . . C11 C 0.2941(2) 0.1447(2) 0.3343(4) 0.0911(12) Uani 1 1 d . . . H11 H 0.2320 0.1436 0.3490 0.109 Uiso 1 1 calc R . . C12 C 0.3230(3) 0.12592(18) 0.2138(3) 0.0846(10) Uani 1 1 d . . . H12 H 0.2808 0.1131 0.1457 0.102 Uiso 1 1 calc R . . C13 C 0.4146(3) 0.12602(18) 0.1934(3) 0.0845(10) Uani 1 1 d . . . H13 H 0.4345 0.1133 0.1112 0.101 Uiso 1 1 calc R . . C14 C 0.4775(2) 0.14503(15) 0.2946(3) 0.0634(8) Uani 1 1 d . . . H14 H 0.5396 0.1435 0.2805 0.076 Uiso 1 1 calc R . . C15 C 0.63643(14) 0.25273(12) 0.6044(2) 0.0383(5) Uani 1 1 d . . . C16 C 0.71141(14) 0.30504(11) 0.6142(2) 0.0392(5) Uani 1 1 d . . . C17 C 0.72823(15) 0.35151(12) 0.5103(2) 0.0426(6) Uani 1 1 d . . . H17 H 0.6941 0.3470 0.4304 0.051 Uiso 1 1 calc R . . C18 C 0.79502(15) 0.40427(12) 0.5243(2) 0.0437(6) Uani 1 1 d . . . H18 H 0.8053 0.4346 0.4533 0.052 Uiso 1 1 calc R . . C19 C 0.84749(14) 0.41310(12) 0.6424(2) 0.0404(5) Uani 1 1 d . . . C20 C 0.83141(16) 0.36551(13) 0.7449(2) 0.0526(7) Uani 1 1 d . . . H20 H 0.8661 0.3696 0.8244 0.063 Uiso 1 1 calc R . . C21 C 0.76527(16) 0.31257(14) 0.7311(2) 0.0530(7) Uani 1 1 d . . . H21 H 0.7564 0.2812 0.8012 0.064 Uiso 1 1 calc R . . C24 C 1.27456(19) 0.56723(17) 0.9515(3) 0.0696(8) Uani 1 1 d . . . H24 H 1.3238 0.5990 0.9482 0.083 Uiso 1 1 calc R . . C23 C 1.2745(2) 0.51461(17) 1.0462(3) 0.0707(8) Uani 1 1 d . . . H23 H 1.3233 0.5097 1.1084 0.085 Uiso 1 1 calc R . . C22 C 1.20041(19) 0.46916(15) 1.0470(3) 0.0666(8) Uani 1 1 d . . . H22 H 1.1999 0.4340 1.1129 0.080 Uiso 1 1 calc R . . N3 N 1.12889(14) 0.47216(11) 0.9590(2) 0.0564(6) Uani 1 1 d . . . C26 C 1.12971(15) 0.52380(13) 0.8665(2) 0.0448(6) Uani 1 1 d . . . C27 C 1.04982(14) 0.52648(12) 0.7684(2) 0.0424(6) Uani 1 1 d . . . C28 C 0.98976(15) 0.46833(13) 0.7521(2) 0.0451(6) Uani 1 1 d . . . H28 H 0.9993 0.4264 0.8022 0.054 Uiso 1 1 calc R . . C29 C 0.91547(14) 0.47295(12) 0.6609(2) 0.0406(5) Uani 1 1 d . . . C30 C 0.90531(15) 0.53725(12) 0.5894(2) 0.0433(6) Uani 1 1 d . . . H30 H 0.8564 0.5428 0.5275 0.052 Uiso 1 1 calc R . . C31 C 0.96787(15) 0.59298(12) 0.6101(2) 0.0421(5) Uani 1 1 d . . . C32 C 0.95732(16) 0.66295(13) 0.5373(2) 0.0464(6) Uani 1 1 d . . . N5 N 0.87865(17) 0.67301(13) 0.4678(3) 0.0798(8) Uani 1 1 d . . . C36 C 0.8672(2) 0.73587(19) 0.4025(4) 0.1005(13) Uani 1 1 d . . . H36 H 0.8116 0.7436 0.3556 0.121 Uiso 1 1 calc R . . C35 C 0.9312(2) 0.78907(17) 0.4002(3) 0.0801(9) Uani 1 1 d . . . H35 H 0.9205 0.8314 0.3516 0.096 Uiso 1 1 calc R . . C34 C 1.0120(2) 0.77820(16) 0.4715(3) 0.0772(9) Uani 1 1 d . . . H34 H 1.0578 0.8132 0.4721 0.093 Uiso 1 1 calc R . . N1 N 0.58668(12) 0.23766(10) 0.49051(17) 0.0403(5) Uani 1 1 d . . . H1A H 0.5974 0.2537 0.4133 0.048 Uiso 1 1 calc R . . N2 N 0.60261(12) 0.21791(10) 0.70592(17) 0.0409(5) Uani 1 1 d . . . C25 C 1.20122(17) 0.57301(15) 0.8610(3) 0.0577(7) Uani 1 1 d . . . H25 H 1.1996 0.6093 0.7971 0.069 Uiso 1 1 calc R . . N4 N 1.03990(12) 0.58785(10) 0.69833(18) 0.0433(5) Uani 1 1 d . . . C33 C 1.0250(2) 0.71473(15) 0.5429(3) 0.0672(8) Uani 1 1 d . . . H33 H 1.0789 0.7071 0.5942 0.081 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 C1 0.0528(16) 0.0608(16) 0.0510(15) 0.0007(13) 0.0071(12) -0.0021(13) C2 0.0521(17) 0.088(2) 0.0580(17) -0.0012(15) 0.0118(13) -0.0121(15) C3 0.071(2) 0.076(2) 0.0514(16) 0.0008(14) 0.0087(14) -0.0303(17) C4 0.084(2) 0.0539(16) 0.0633(18) 0.0091(14) 0.0061(16) -0.0116(16) C5 0.0597(17) 0.0587(17) 0.0608(17) 0.0072(14) 0.0055(13) 0.0008(14) C6 0.0439(14) 0.0489(14) 0.0368(12) -0.0011(10) -0.0040(10) -0.0089(11) C7 0.0360(13) 0.0452(13) 0.0380(12) -0.0003(10) -0.0006(10) -0.0031(10) C8 0.0362(13) 0.0456(13) 0.0407(13) 0.0020(10) -0.0021(10) -0.0063(10) C9 0.0500(15) 0.0547(15) 0.0424(14) 0.0063(11) -0.0087(11) -0.0117(12) C10 0.0568(19) 0.120(3) 0.0511(16) 0.0177(17) -0.0077(14) -0.0294(18) C11 0.0567(19) 0.134(3) 0.080(2) 0.031(2) -0.0234(17) -0.0387(19) C12 0.087(3) 0.092(2) 0.070(2) -0.0003(18) -0.0368(19) -0.0241(19) C13 0.089(3) 0.095(2) 0.066(2) -0.0277(17) -0.0274(18) 0.0055(19) C14 0.0613(17) 0.0665(18) 0.0602(17) -0.0145(14) -0.0150(14) 0.0046(14) C15 0.0359(12) 0.0426(13) 0.0360(12) 0.0008(10) -0.0023(10) -0.0006(10) C16 0.0352(12) 0.0421(13) 0.0400(12) -0.0015(10) 0.0012(10) -0.0027(10) C17 0.0390(13) 0.0532(14) 0.0353(12) -0.0033(10) 0.0009(10) -0.0055(11) C18 0.0444(13) 0.0480(13) 0.0391(13) 0.0030(11) 0.0053(10) -0.0038(11) C19 0.0345(12) 0.0434(13) 0.0434(13) -0.0022(10) 0.0035(10) -0.0003(10) C20 0.0463(14) 0.0620(16) 0.0476(14) 0.0067(12) -0.0119(11) -0.0147(12) C21 0.0507(15) 0.0599(16) 0.0471(14) 0.0124(12) -0.0094(12) -0.0162(13) C24 0.0589(18) 0.078(2) 0.0701(19) -0.0054(16) -0.0124(15) -0.0217(15) C23 0.0633(19) 0.080(2) 0.0658(19) -0.0027(16) -0.0210(15) -0.0020(16) C22 0.0683(19) 0.0670(18) 0.0625(17) 0.0112(14) -0.0125(15) -0.0019(15) N3 0.0532(13) 0.0566(13) 0.0582(13) 0.0053(11) -0.0065(11) -0.0027(10) C26 0.0416(14) 0.0464(13) 0.0463(14) -0.0037(11) 0.0007(11) 0.0005(11) C27 0.0358(13) 0.0460(14) 0.0454(13) -0.0053(11) 0.0044(10) -0.0012(11) C28 0.0394(13) 0.0451(13) 0.0507(14) 0.0013(11) 0.0023(11) -0.0009(11) C29 0.0347(12) 0.0429(13) 0.0447(13) -0.0041(10) 0.0062(10) -0.0012(10) C30 0.0350(12) 0.0488(14) 0.0457(13) -0.0022(11) -0.0004(10) 0.0004(11) C31 0.0371(13) 0.0443(13) 0.0451(13) -0.0030(11) 0.0048(10) 0.0011(11) C32 0.0434(14) 0.0457(14) 0.0503(14) 0.0014(11) 0.0056(11) -0.0009(11) N5 0.0652(16) 0.0651(15) 0.106(2) 0.0331(14) -0.0240(14) -0.0113(12) C36 0.084(2) 0.081(2) 0.132(3) 0.046(2) -0.035(2) -0.0110(19) C35 0.095(3) 0.0576(18) 0.087(2) 0.0228(16) 0.0001(19) -0.0060(18) C34 0.086(2) 0.0551(18) 0.089(2) 0.0100(16) -0.0034(19) -0.0203(17) N1 0.0409(11) 0.0473(11) 0.0323(10) 0.0027(8) -0.0012(8) -0.0058(9) N2 0.0395(11) 0.0482(11) 0.0345(10) 0.0000(8) -0.0015(8) -0.0067(9) C25 0.0539(16) 0.0621(16) 0.0561(16) 0.0029(13) -0.0064(13) -0.0139(13) N4 0.0405(11) 0.0418(11) 0.0476(11) -0.0028(9) 0.0018(9) -0.0036(9) C33 0.0654(19) 0.0534(16) 0.082(2) 0.0095(15) -0.0073(15) -0.0099(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 C1 C2 1.377(4) . ? C1 C6 1.384(3) . ? C2 C3 1.369(4) . ? C3 C4 1.361(4) . ? C4 C5 1.394(4) . ? C5 C6 1.379(3) . ? C6 C7 1.481(3) . ? C7 C8 1.372(3) . ? C7 N2 1.380(3) . ? C8 N1 1.375(3) . ? C8 C9 1.473(3) . ? C9 C10 1.377(4) . ? C9 C14 1.384(4) . ? C10 C11 1.394(4) . ? C11 C12 1.361(5) . ? C12 C13 1.369(5) . ? C13 C14 1.383(4) . ? C15 N2 1.333(3) . ? C15 N1 1.357(3) . ? C15 C16 1.459(3) . ? C16 C17 1.391(3) . ? C16 C21 1.392(3) . ? C17 C18 1.379(3) . ? C18 C19 1.394(3) . ? C19 C20 1.390(3) . ? C19 C29 1.489(3) . ? C20 C21 1.375(3) . ? C24 C23 1.363(4) . ? C24 C25 1.375(4) . ? C23 C22 1.370(4) . ? C22 N3 1.337(3) . ? N3 C26 1.336(3) . ? C26 C25 1.388(3) . ? C26 C27 1.492(3) . ? C27 N4 1.337(3) . ? C27 C28 1.389(3) . ? C28 C29 1.389(3) . ? C29 C30 1.391(3) . ? C30 C31 1.383(3) . ? C31 N4 1.346(3) . ? C31 C32 1.488(3) . ? C32 N5 1.328(3) . ? C32 C33 1.374(3) . ? N5 C36 1.338(4) . ? C36 C35 1.357(4) . ? C35 C34 1.364(4) . ? C34 C33 1.381(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.0(3) . . ? C3 C2 C1 119.8(3) . . ? C4 C3 C2 120.4(3) . . ? C3 C4 C5 120.1(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C1 118.6(2) . . ? C5 C6 C7 121.7(2) . . ? C1 C6 C7 119.7(2) . . ? C8 C7 N2 110.27(19) . . ? C8 C7 C6 127.60(19) . . ? N2 C7 C6 122.13(19) . . ? C7 C8 N1 105.31(18) . . ? C7 C8 C9 133.4(2) . . ? N1 C8 C9 121.27(19) . . ? C10 C9 C14 118.2(2) . . ? C10 C9 C8 121.3(2) . . ? C14 C9 C8 120.5(2) . . ? C9 C10 C11 120.6(3) . . ? C12 C11 C10 120.4(3) . . ? C11 C12 C13 119.7(3) . . ? C12 C13 C14 120.3(3) . . ? C13 C14 C9 120.9(3) . . ? N2 C15 N1 110.71(18) . . ? N2 C15 C16 125.21(19) . . ? N1 C15 C16 123.87(19) . . ? C17 C16 C21 117.9(2) . . ? C17 C16 C15 121.31(19) . . ? C21 C16 C15 120.7(2) . . ? C18 C17 C16 120.7(2) . . ? C17 C18 C19 121.5(2) . . ? C20 C19 C18 117.4(2) . . ? C20 C19 C29 120.9(2) . . ? C18 C19 C29 121.7(2) . . ? C21 C20 C19 121.3(2) . . ? C20 C21 C16 121.2(2) . . ? C23 C24 C25 119.5(3) . . ? C24 C23 C22 118.1(3) . . ? N3 C22 C23 124.1(3) . . ? C26 N3 C22 117.3(2) . . ? N3 C26 C25 122.0(2) . . ? N3 C26 C27 116.9(2) . . ? C25 C26 C27 121.0(2) . . ? N4 C27 C28 122.6(2) . . ? N4 C27 C26 116.02(19) . . ? C28 C27 C26 121.4(2) . . ? C29 C28 C27 119.9(2) . . ? C28 C29 C30 117.1(2) . . ? C28 C29 C19 122.1(2) . . ? C30 C29 C19 120.85(19) . . ? C31 C30 C29 120.1(2) . . ? N4 C31 C30 122.4(2) . . ? N4 C31 C32 116.4(2) . . ? C30 C31 C32 121.1(2) . . ? N5 C32 C33 121.8(2) . . ? N5 C32 C31 116.5(2) . . ? C33 C32 C31 121.7(2) . . ? C32 N5 C36 117.6(2) . . ? N5 C36 C35 124.4(3) . . ? C36 C35 C34 117.6(3) . . ? C35 C34 C33 119.4(3) . . ? C15 N1 C8 108.16(18) . . ? C15 N2 C7 105.54(17) . . ? C24 C25 C26 119.0(3) . . ? C27 N4 C31 117.94(19) . . ? C32 C33 C34 119.1(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.187 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.035 data_q _database_code_depnum_ccdc_archive 'CCDC 817563' #TrackingRef '- FeComplex.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl2 Fe N10 O8' _chemical_formula_weight 1309.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 23.5948(16) _cell_length_b 36.253(3) _cell_length_c 38.053(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32550(4) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 19.85 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10816 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 111775 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.20 _reflns_number_total 7307 _reflns_number_gt 4640 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^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 7307 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2247 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 -0.1250 0.8750 0.013752(16) 0.0540(2) Uani 1 2 d S . . Cl1 Cl 0.74582(5) 0.02728(4) 0.85889(3) 0.0991(4) Uani 1 1 d . . . C1 C 0.5018(3) 1.0143(3) 0.0663(3) 0.189(4) Uani 1 1 d . . . H1 H 0.5372 1.0086 0.0571 0.227 Uiso 1 1 calc R . . C2 C 0.4554(2) 1.01248(19) 0.0453(2) 0.151(2) Uani 1 1 d . . . H2 H 0.4598 1.0048 0.0222 0.181 Uiso 1 1 calc R . . C3 C 0.40345(17) 1.02137(12) 0.05679(18) 0.0985(15) Uani 1 1 d . . . C4 C 0.3983(2) 1.03210(16) 0.0915(2) 0.1272(19) Uani 1 1 d . . . H4 H 0.3626 1.0382 0.1001 0.153 Uiso 1 1 calc R . . C5 C 0.4432(4) 1.0341(2) 0.1133(2) 0.172(3) Uani 1 1 d . . . H5 H 0.4395 1.0416 0.1366 0.206 Uiso 1 1 calc R . . C6 C 0.4979(4) 1.0238(2) 0.0985(3) 0.173(4) Uani 1 1 d . . . H6 H 0.5301 1.0242 0.1126 0.208 Uiso 1 1 calc R . . N1 N 0.30682(13) 0.99981(9) 0.04146(10) 0.0858(10) Uani 1 1 d . . . H1A H 0.3011 0.9882 0.0608 0.103 Uiso 1 1 calc R . . C7 C 0.35399(16) 1.02024(11) 0.03290(13) 0.0863(12) Uani 1 1 d . . . C8 C 0.27099(16) 1.00144(11) 0.01349(12) 0.0807(11) Uani 1 1 d . . . N2 N 0.29272(13) 1.02143(9) -0.01206(9) 0.0866(10) Uani 1 1 d . . . C9 C 0.34449(16) 1.03336(12) 0.00039(13) 0.0887(12) Uani 1 1 d . . . C10 C 0.38044(17) 1.05738(13) -0.02169(16) 0.0934(13) Uani 1 1 d . . . C11 C 0.37744(19) 1.05600(17) -0.05753(17) 0.1173(17) Uani 1 1 d . . . H11 H 0.3525 1.0397 -0.0683 0.141 Uiso 1 1 calc R . . C12 C 0.4115(2) 1.07882(19) -0.07795(18) 0.133(2) Uani 1 1 d . . . H12 H 0.4088 1.0778 -0.1023 0.159 Uiso 1 1 calc R . . C13 C 0.4476(3) 1.1020(2) -0.0632(3) 0.147(3) Uani 1 1 d . . . H13 H 0.4710 1.1164 -0.0773 0.177 Uiso 1 1 calc R . . C14 C 0.4508(3) 1.10489(19) -0.0279(3) 0.157(3) Uani 1 1 d . . . H14 H 0.4756 1.1216 -0.0176 0.188 Uiso 1 1 calc R . . C15 C 0.4169(2) 1.08279(16) -0.00755(18) 0.132(2) Uani 1 1 d . . . H15 H 0.4188 1.0851 0.0168 0.158 Uiso 1 1 calc R . . C16 C 0.21610(15) 0.98263(10) 0.01242(11) 0.0763(10) Uani 1 1 d . . . C17 C 0.19782(16) 0.96029(11) 0.03987(11) 0.0851(12) Uani 1 1 d . . . H17 H 0.2217 0.9562 0.0589 0.102 Uiso 1 1 calc R . . C18 C 0.14542(15) 0.94418(11) 0.03937(10) 0.0764(10) Uani 1 1 d . . . H18 H 0.1345 0.9293 0.0581 0.092 Uiso 1 1 calc R . . C19 C 0.10831(14) 0.94955(9) 0.01169(9) 0.0646(9) Uani 1 1 d . . . C20 C 0.12677(15) 0.97209(12) -0.01580(10) 0.0810(11) Uani 1 1 d . . . H20 H 0.1029 0.9763 -0.0348 0.097 Uiso 1 1 calc R . . C21 C 0.17925(16) 0.98806(12) -0.01521(11) 0.0844(11) Uani 1 1 d . . . H21 H 0.1904 1.0029 -0.0339 0.101 Uiso 1 1 calc R . . C22 C -0.11032(15) 0.81956(10) 0.07073(9) 0.0687(9) Uani 1 1 d . . . H22 H -0.1473 0.8122 0.0660 0.082 Uiso 1 1 calc R . . C23 C -0.08225(18) 0.80334(12) 0.09760(11) 0.0887(12) Uani 1 1 d . . . H23 H -0.0993 0.7848 0.1107 0.106 Uiso 1 1 calc R . . C24 C -0.02728(18) 0.81491(13) 0.10525(12) 0.0982(14) Uani 1 1 d . . . H24 H -0.0074 0.8046 0.1239 0.118 Uiso 1 1 calc R . . C25 C -0.00313(16) 0.84148(11) 0.08498(10) 0.0810(11) Uani 1 1 d . . . H25 H 0.0337 0.8493 0.0896 0.097 Uiso 1 1 calc R . . C26 C -0.03279(13) 0.85677(9) 0.05779(9) 0.0598(8) Uani 1 1 d . . . C27 C -0.01294(13) 0.88644(8) 0.03498(8) 0.0553(8) Uani 1 1 d . . . C28 C 0.04053(14) 0.90193(9) 0.03383(9) 0.0631(8) Uani 1 1 d . . . H28 H 0.0692 0.8925 0.0480 0.076 Uiso 1 1 calc R . . C29 C 0.05180(13) 0.93162(9) 0.01154(8) 0.0583(8) Uani 1 1 d . . . C30 C 0.00751(14) 0.94376(9) -0.01009(9) 0.0623(8) Uani 1 1 d . . . H30 H 0.0133 0.9635 -0.0253 0.075 Uiso 1 1 calc R . . C31 C -0.04418(13) 0.92677(8) -0.00894(8) 0.0535(7) Uani 1 1 d . . . C32 C -0.09471(13) 0.93481(9) -0.03030(8) 0.0580(8) Uani 1 1 d . . . C33 C -0.09731(16) 0.96100(10) -0.05626(10) 0.0718(9) Uani 1 1 d . . . H33 H -0.0660 0.9757 -0.0611 0.086 Uiso 1 1 calc R . . C34 C -0.14658(17) 0.96531(11) -0.07500(10) 0.0789(10) Uani 1 1 d . . . H34 H -0.1490 0.9829 -0.0927 0.095 Uiso 1 1 calc R . . C35 C -0.19181(18) 0.94346(11) -0.06734(11) 0.0849(11) Uani 1 1 d . . . H35 H -0.2255 0.9460 -0.0798 0.102 Uiso 1 1 calc R . . C36 C -0.18740(14) 0.91768(10) -0.04111(10) 0.0695(9) Uani 1 1 d . . . H36 H -0.2188 0.9031 -0.0360 0.083 Uiso 1 1 calc R . . N3 N -0.08689(11) 0.84602(7) 0.05056(7) 0.0589(7) Uani 1 1 d . . . N4 N -0.05407(10) 0.89843(7) 0.01368(6) 0.0528(6) Uani 1 1 d . . . N5 N -0.13991(11) 0.91265(7) -0.02267(7) 0.0571(7) Uani 1 1 d . . . O1 O 0.7175(3) 0.0158(3) 0.88417(14) 0.302(5) Uani 1 1 d . . . O2 O 0.80374(16) 0.02534(14) 0.86215(10) 0.1612(17) Uani 1 1 d . . . O3 O 0.7336(3) 0.0647(3) 0.86507(19) 0.278(4) Uani 1 1 d . . . O4 O 0.72617(14) 0.01917(10) 0.82533(8) 0.1190(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0544(4) 0.0582(4) 0.0495(4) 0.000 0.000 -0.0022(3) Cl1 0.0849(7) 0.1491(11) 0.0632(7) 0.0166(7) 0.0019(5) 0.0440(7) C1 0.083(4) 0.206(9) 0.277(12) 0.051(9) -0.036(7) 0.005(4) C2 0.071(3) 0.188(6) 0.195(7) 0.030(5) -0.005(4) 0.011(3) C3 0.062(3) 0.085(3) 0.148(5) 0.032(3) -0.009(3) -0.011(2) C4 0.100(4) 0.127(4) 0.155(6) 0.016(4) -0.022(4) -0.026(3) C5 0.162(7) 0.153(6) 0.201(8) 0.045(5) -0.072(7) -0.048(5) C6 0.124(6) 0.138(6) 0.257(12) 0.074(7) -0.084(8) -0.051(5) N1 0.0621(18) 0.092(2) 0.103(3) 0.021(2) 0.0012(18) -0.0073(16) C7 0.061(2) 0.087(3) 0.111(3) 0.009(3) 0.006(2) -0.011(2) C8 0.064(2) 0.080(3) 0.098(3) 0.009(2) 0.011(2) -0.0065(19) N2 0.0670(19) 0.093(2) 0.099(3) 0.020(2) 0.0138(18) -0.0101(17) C9 0.066(2) 0.094(3) 0.107(3) 0.027(3) 0.014(2) -0.001(2) C10 0.065(2) 0.088(3) 0.128(4) 0.025(3) 0.022(3) 0.001(2) C11 0.071(3) 0.145(5) 0.135(5) 0.030(4) 0.026(3) -0.003(3) C12 0.101(4) 0.167(5) 0.131(5) 0.049(4) 0.027(4) 0.001(4) C13 0.101(4) 0.141(5) 0.199(8) 0.073(6) 0.037(5) -0.003(4) C14 0.132(5) 0.133(5) 0.205(8) 0.053(6) 0.017(5) -0.055(4) C15 0.113(4) 0.124(4) 0.158(5) 0.029(4) 0.017(4) -0.030(3) C16 0.061(2) 0.083(2) 0.085(3) 0.011(2) 0.009(2) -0.0061(18) C17 0.073(2) 0.092(3) 0.090(3) 0.023(2) -0.016(2) -0.021(2) C18 0.075(2) 0.081(2) 0.072(2) 0.017(2) -0.003(2) -0.0173(19) C19 0.0626(19) 0.069(2) 0.062(2) 0.0041(17) 0.0048(17) -0.0050(16) C20 0.066(2) 0.101(3) 0.075(3) 0.024(2) -0.0010(19) -0.008(2) C21 0.075(2) 0.102(3) 0.077(3) 0.021(2) 0.007(2) -0.011(2) C22 0.068(2) 0.069(2) 0.070(2) 0.0098(19) -0.0006(18) -0.0105(17) C23 0.092(3) 0.093(3) 0.082(3) 0.035(2) -0.005(2) -0.013(2) C24 0.091(3) 0.112(3) 0.092(3) 0.047(3) -0.022(2) -0.009(3) C25 0.072(2) 0.093(3) 0.077(3) 0.034(2) -0.015(2) -0.0133(19) C26 0.0580(18) 0.066(2) 0.0550(19) 0.0066(16) -0.0021(15) -0.0022(16) C27 0.0561(17) 0.0589(18) 0.0509(19) 0.0028(15) -0.0030(15) -0.0035(15) C28 0.0621(19) 0.068(2) 0.059(2) 0.0079(17) -0.0047(16) -0.0010(16) C29 0.0579(18) 0.0619(19) 0.0551(19) 0.0021(16) 0.0042(15) -0.0033(15) C30 0.068(2) 0.0617(19) 0.057(2) 0.0098(16) 0.0025(16) -0.0026(16) C31 0.0601(18) 0.0523(17) 0.0480(18) 0.0021(15) 0.0035(14) 0.0000(14) C32 0.0608(19) 0.0592(19) 0.0539(19) -0.0009(16) 0.0038(15) 0.0036(16) C33 0.074(2) 0.071(2) 0.071(2) 0.0129(19) -0.0016(19) 0.0046(18) C34 0.087(3) 0.085(3) 0.065(2) 0.020(2) -0.001(2) 0.010(2) C35 0.083(3) 0.094(3) 0.077(3) 0.017(2) -0.013(2) 0.016(2) C36 0.061(2) 0.076(2) 0.071(2) 0.0011(19) -0.0044(18) -0.0012(17) N3 0.0562(15) 0.0676(16) 0.0528(16) 0.0038(13) 0.0013(12) -0.0041(13) N4 0.0556(14) 0.0578(15) 0.0450(14) 0.0023(12) 0.0002(12) 0.0007(11) N5 0.0621(16) 0.0596(16) 0.0497(15) -0.0029(12) -0.0008(12) 0.0064(13) O1 0.248(7) 0.540(15) 0.118(4) 0.108(6) -0.028(4) -0.223(8) O2 0.105(3) 0.247(5) 0.132(3) -0.038(3) -0.024(2) 0.046(3) O3 0.277(8) 0.308(8) 0.249(7) -0.129(7) -0.109(6) 0.173(7) O4 0.123(2) 0.158(3) 0.075(2) -0.0115(19) -0.0269(18) 0.048(2) _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 N4 1.877(2) . ? Fe1 N4 1.877(2) 2_465 ? Fe1 N3 1.968(3) 2_465 ? Fe1 N3 1.968(3) . ? Fe1 N5 1.977(3) 2_465 ? Fe1 N5 1.977(3) . ? Cl1 O1 1.243(5) . ? Cl1 O2 1.374(4) . ? Cl1 O4 1.390(3) . ? Cl1 O3 1.405(8) . ? C1 C6 1.276(13) . ? C1 C2 1.358(10) . ? C2 C3 1.340(7) . ? C3 C4 1.383(8) . ? C3 C7 1.480(6) . ? C4 C5 1.347(9) . ? C5 C6 1.456(13) . ? N1 C8 1.360(5) . ? N1 C7 1.376(5) . ? C7 C9 1.344(6) . ? C8 N2 1.317(5) . ? C8 C16 1.464(5) . ? N2 C9 1.380(5) . ? C9 C10 1.478(6) . ? C10 C11 1.367(7) . ? C10 C15 1.371(7) . ? C11 C12 1.390(7) . ? C12 C13 1.323(9) . ? C13 C14 1.349(10) . ? C14 C15 1.372(8) . ? C16 C21 1.379(5) . ? C16 C17 1.390(5) . ? C17 C18 1.368(5) . ? C18 C19 1.383(5) . ? C19 C20 1.397(5) . ? C19 C29 1.483(4) . ? C20 C21 1.367(5) . ? C22 N3 1.347(4) . ? C22 C23 1.353(5) . ? C23 C24 1.394(5) . ? C24 C25 1.359(5) . ? C25 C26 1.366(5) . ? C26 N3 1.363(4) . ? C26 C27 1.460(4) . ? C27 N4 1.337(4) . ? C27 C28 1.382(4) . ? C28 C29 1.396(4) . ? C29 C30 1.401(4) . ? C30 C31 1.367(4) . ? C31 N4 1.360(4) . ? C31 C32 1.472(4) . ? C32 N5 1.367(4) . ? C32 C33 1.372(5) . ? C33 C34 1.373(5) . ? C34 C35 1.361(5) . ? C35 C36 1.371(5) . ? C36 N5 1.335(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N4 179.83(15) . 2_465 ? N4 Fe1 N3 99.60(10) . 2_465 ? N4 Fe1 N3 80.52(10) 2_465 2_465 ? N4 Fe1 N3 80.52(10) . . ? N4 Fe1 N3 99.60(10) 2_465 . ? N3 Fe1 N3 89.26(15) 2_465 . ? N4 Fe1 N5 98.79(10) . 2_465 ? N4 Fe1 N5 81.09(11) 2_465 2_465 ? N3 Fe1 N5 161.59(10) 2_465 2_465 ? N3 Fe1 N5 92.82(10) . 2_465 ? N4 Fe1 N5 81.09(11) . . ? N4 Fe1 N5 98.79(10) 2_465 . ? N3 Fe1 N5 92.81(10) 2_465 . ? N3 Fe1 N5 161.59(11) . . ? N5 Fe1 N5 90.96(14) 2_465 . ? O1 Cl1 O2 116.6(4) . . ? O1 Cl1 O4 117.5(3) . . ? O2 Cl1 O4 113.8(2) . . ? O1 Cl1 O3 94.7(6) . . ? O2 Cl1 O3 103.8(4) . . ? O4 Cl1 O3 106.8(3) . . ? C6 C1 C2 121.3(10) . . ? C3 C2 C1 122.3(9) . . ? C2 C3 C4 117.3(6) . . ? C2 C3 C7 120.9(6) . . ? C4 C3 C7 121.7(5) . . ? C5 C4 C3 122.3(7) . . ? C4 C5 C6 116.4(9) . . ? C1 C6 C5 120.4(9) . . ? C8 N1 C7 107.1(3) . . ? C9 C7 N1 105.9(4) . . ? C9 C7 C3 133.4(4) . . ? N1 C7 C3 120.5(4) . . ? N2 C8 N1 111.1(3) . . ? N2 C8 C16 125.5(4) . . ? N1 C8 C16 123.4(4) . . ? C8 N2 C9 105.3(4) . . ? C7 C9 N2 110.7(3) . . ? C7 C9 C10 129.5(4) . . ? N2 C9 C10 119.8(4) . . ? C11 C10 C15 116.6(5) . . ? C11 C10 C9 121.1(5) . . ? C15 C10 C9 122.2(5) . . ? C10 C11 C12 120.4(6) . . ? C13 C12 C11 120.9(7) . . ? C12 C13 C14 120.5(6) . . ? C13 C14 C15 119.0(7) . . ? C10 C15 C14 122.5(7) . . ? C21 C16 C17 117.4(3) . . ? C21 C16 C8 120.8(4) . . ? C17 C16 C8 121.7(4) . . ? C18 C17 C16 121.2(4) . . ? C17 C18 C19 121.5(3) . . ? C18 C19 C20 117.1(3) . . ? C18 C19 C29 120.7(3) . . ? C20 C19 C29 122.3(3) . . ? C21 C20 C19 121.2(4) . . ? C20 C21 C16 121.6(4) . . ? N3 C22 C23 122.6(3) . . ? C22 C23 C24 118.9(4) . . ? C25 C24 C23 119.0(4) . . ? C24 C25 C26 120.2(4) . . ? N3 C26 C25 121.1(3) . . ? N3 C26 C27 113.0(3) . . ? C25 C26 C27 125.8(3) . . ? N4 C27 C28 120.8(3) . . ? N4 C27 C26 111.6(3) . . ? C28 C27 C26 127.7(3) . . ? C27 C28 C29 120.4(3) . . ? C28 C29 C30 117.2(3) . . ? C28 C29 C19 120.4(3) . . ? C30 C29 C19 122.4(3) . . ? C31 C30 C29 120.3(3) . . ? N4 C31 C30 120.9(3) . . ? N4 C31 C32 111.1(3) . . ? C30 C31 C32 128.0(3) . . ? N5 C32 C33 121.7(3) . . ? N5 C32 C31 113.5(3) . . ? C33 C32 C31 124.8(3) . . ? C32 C33 C34 119.4(3) . . ? C35 C34 C33 119.1(3) . . ? C34 C35 C36 119.5(4) . . ? N5 C36 C35 122.7(3) . . ? C22 N3 C26 118.2(3) . . ? C22 N3 Fe1 126.7(2) . . ? C26 N3 Fe1 114.8(2) . . ? C27 N4 C31 120.3(3) . . ? C27 N4 Fe1 119.9(2) . . ? C31 N4 Fe1 119.7(2) . . ? C36 N5 C32 117.6(3) . . ? C36 N5 Fe1 127.8(2) . . ? C32 N5 Fe1 114.6(2) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.875 0.008 0.375 9 -1 ' ' 2 0.375 0.008 0.875 9 -1 ' ' 3 0.640 0.125 0.125 1304 227 ' ' 4 0.140 0.125 0.625 1304 227 ' ' 5 0.375 0.101 0.375 24 6 ' ' 6 0.875 0.101 0.875 24 6 ' ' 7 0.875 0.149 0.375 24 6 ' ' 8 0.375 0.149 0.875 24 6 ' ' 9 0.375 0.242 0.375 8 -1 ' ' 10 0.875 0.242 0.875 8 -1 ' ' 11 0.625 0.268 0.125 6 0 ' ' 12 0.125 0.268 0.625 6 0 ' ' 13 0.355 0.375 0.375 1301 231 ' ' 14 0.855 0.375 0.875 1301 231 ' ' 15 0.125 0.351 0.125 24 5 ' ' 16 0.625 0.351 0.625 24 5 ' ' 17 0.625 0.399 0.125 24 5 ' ' 18 0.125 0.399 0.625 24 5 ' ' 19 0.125 0.492 0.125 8 -1 ' ' 20 0.625 0.492 0.625 8 -1 ' ' 21 0.375 0.518 0.375 6 0 ' ' 22 0.875 0.518 0.875 6 0 ' ' 23 0.140 0.625 0.125 1300 227 ' ' 24 0.640 0.625 0.625 1300 227 ' ' 25 0.875 0.601 0.375 24 6 ' ' 26 0.375 0.601 0.875 24 6 ' ' 27 0.375 0.649 0.375 24 6 ' ' 28 0.875 0.649 0.875 24 6 ' ' 29 0.875 0.742 0.375 8 -1 ' ' 30 0.375 0.742 0.875 8 -1 ' ' 31 0.125 0.768 0.125 6 0 ' ' 32 0.625 0.768 0.625 6 0 ' ' 33 0.855 0.875 0.375 1298 231 ' ' 34 0.355 0.875 0.875 1298 231 ' ' 35 0.625 0.851 0.125 24 5 ' ' 36 0.125 0.851 0.625 24 5 ' ' 37 0.125 0.899 0.125 24 5 ' ' 38 0.625 0.899 0.625 24 5 ' ' 39 0.625 0.982 0.125 5 0 ' ' 40 0.125 0.982 0.625 5 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.800 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.052