# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2146 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-03-08 _audit_update_record ? #======================================================================= # (Publishing Staff 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 ? _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 ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'J.Chem.Soc., Dalton' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_pz3fen # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H20 Fe N14 O6' _chemical_formula_moiety ? _chemical_formula_weight 608.32 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.716(3) _cell_length_b 7.740(2) _cell_length_c 17.280(6) _cell_angle_alpha 90.00000 _cell_angle_beta 101.67(3) _cell_angle_gamma 90.00000 _cell_volume 1272.6(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6 _cell_measurement_theta_min 15.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .66 _exptl_crystal_description ? _exptl_crystal_size_max .25 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .87 _exptl_absorpt_correction_T_max .901 _diffrn_reflns_number 2240 _reflns_number_total 2240 _reflns_Friedel_coverage ? _reflns_number_gt 1786 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 6 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .047 _refine_ls_wR_factor_ref .056 _refine_ls_goodness_of_fit_ref 1.69 _refine_ls_number_reflns 1786 _refine_ls_number_parameters 255 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall #<< use NfA code _refine_ls_shift/su_max .028 _refine_diff_density_min -.45 _refine_diff_density_max .51 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 40 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 40 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 2 .301025 .844971 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe .50000 .00000 .00000 .0331(4) Uani ? ? 1.00000 ? ? N11 .5354(3) -.1495(4) .09454(17) .0395(17) Uani ? ? 1.00000 ? ? N15 .4209(3) -.2013(4) .12319(18) .0420(17) Uani ? ? 1.00000 ? ? N21 .3695(3) .1328(4) .05030(18) .0405(17) Uani ? ? 1.00000 ? ? N25 .2798(3) .0444(4) .08635(18) .0407(17) Uani ? ? 1.00000 ? ? N31 .3430(3) -.1546(4) -.04314(17) .0389(17) Uani ? ? 1.00000 ? ? N35 .2526(3) -.2013(4) .00456(18) .0406(17) Uani ? ? 1.00000 ? ? C1 .2854(4) -.1414(5) .0859(2) .041(2) Uani ? ? 1.00000 ? ? C12 .6427(5) -.2316(6) .1367(2) .049(2) Uani ? ? 1.00000 ? ? C13 .5987(6) -.3384(6) .1923(3) .056(3) Uani ? ? 1.00000 ? ? C14 .4600(5) -.3174(6) .1829(2) .050(2) Uani ? ? 1.00000 ? ? C22 .3417(5) .2993(6) .0606(3) .052(2) Uani ? ? 1.00000 ? ? C23 .2341(5) .3134(7) .1026(3) .063(3) Uani ? ? 1.00000 ? ? C24 .1971(5) .1514(6) .1183(3) .053(3) Uani ? ? 1.00000 ? ? C32 .2920(5) -.2334(6) -.1114(2) .045(2) Uani ? ? 1.00000 ? ? C33 .1730(5) -.3279(6) -.1073(3) .055(3) Uani ? ? 1.00000 ? ? C34 .1516(5) -.3057(6) -.0326(3) .049(2) Uani ? ? 1.00000 ? ? N100 .5253(4) .7854(6) .7007(3) .057(3) Uani ? ? 1.00000 ? ? O101 .461(2) .865(3) .7458(13) .094(10) Uani ? ? .50000 ? ? O102 .5736(18) .8571(18) .6504(8) .139(12) Uani ? ? .50000 ? ? O103 .523(2) .6348(17) .6975(11) .154(12) Uani ? ? .50000 ? ? O104 .4971(13) .658(2) .6606(12) .157(14) Uani ? ? .50000 ? ? O105 .6290(12) .8663(18) .6961(6) .086(6) Uani ? ? .50000 ? ? O106 .4571(17) .829(4) .7448(14) .102(13) Uani ? ? .50000 ? ? H1 .215(4) -.194(5) .112(2) .047(11) Uiso ? ? 1.00000 ? ? H12 .735(5) -.216(5) .127(3) .063(14) Uiso ? ? 1.00000 ? ? H13 .652(4) -.404(6) .224(2) .052(13) Uiso ? ? 1.00000 ? ? H14 .391(4) -.366(5) .207(2) .052(12) Uiso ? ? 1.00000 ? ? H22 .405(4) .394(6) .041(2) .064(13) Uiso ? ? 1.00000 ? ? H23 .197(5) .407(6) .118(3) .062(14) Uiso ? ? 1.00000 ? ? H24 .117(4) .104(5) .141(2) .054(12) Uiso ? ? 1.00000 ? ? H32 .341(4) -.227(5) -.151(2) .052(12) Uiso ? ? 1.00000 ? ? H33 .120(4) -.390(6) -.144(2) .053(13) Uiso ? ? 1.00000 ? ? H34 .075(4) -.349(5) -.011(2) .051(12) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe .0347(4) .0382(4) .0302(4) -.0025(4) .0156(3) .0006(4) N11 .0375(18) .047(2) .0366(17) -.0002(16) .0139(15) .0021(15) N15 .0450(19) .050(2) .0360(17) -.0054(16) .0190(15) .0041(16) N21 .0409(19) .042(2) .0428(19) .0005(15) .0196(16) .0034(16) N25 .0415(18) .046(2) .0403(18) -.0011(15) .0205(15) -.0021(15) N31 .0407(18) .045(2) .0355(17) .0008(15) .0182(15) .0036(15) N35 .0393(18) .048(2) .0390(18) -.0085(16) .0173(15) -.0006(16) C1 .041(2) .049(2) .039(2) -.008(2) .021(2) .001(2) C12 .050(3) .054(3) .042(2) .001(2) .010(2) .002(2) C13 .070(3) .056(3) .040(2) .006(3) .003(2) .010(2) C14 .067(3) .053(3) .033(2) -.005(2) .017(2) .004(2) C22 .057(3) .046(3) .058(3) .002(2) .021(2) -.004(2) C23 .065(3) .057(3) .074(3) .009(3) .031(3) -.017(3) C24 .046(3) .067(3) .052(3) .005(2) .025(2) -.008(2) C32 .050(3) .052(3) .036(2) -.003(2) .010(2) -.004(2) C33 .060(3) .055(3) .048(3) -.015(2) .006(2) -.009(2) C34 .044(2) .048(3) .056(3) -.011(2) .012(2) .005(2) N100 .053(3) .061(3) .063(3) .010(2) .026(2) .014(2) O101 .149(14) .086(8) .058(9) .046(8) .046(9) .003(6) O102 .224(18) .083(9) .163(13) .077(11) .167(13) .073(10) O103 .28(2) .035(6) .167(14) .016(8) .102(13) .034(8) O104 .060(6) .178(18) .24(2) -.028(8) .052(8) -.143(16) O105 .077(6) .097(7) .102(8) -.025(6) .060(6) .014(7) O106 .055(7) .18(2) .092(12) .021(9) .061(8) .011(11) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Fe N11 . . 1.975(3) ? Fe N21 . . 1.966(3) ? Fe N31 . . 1.963(3) ? Fe N11 . '3 655' 1.975(3) ? Fe N21 . '3 655' 1.966(3) ? Fe N31 . '3 655' 1.963(3) ? N11 N15 . . 1.366(5) ? N11 C12 . . 1.309(5) ? N15 C1 . . 1.422(5) ? N15 C14 . . 1.363(5) ? N21 N25 . . 1.355(5) ? N21 C22 . . 1.336(6) ? N25 C1 . . 1.439(5) ? N25 C24 . . 1.347(6) ? N31 N35 . . 1.370(5) ? N31 C32 . . 1.331(5) ? N35 C1 . . 1.452(5) ? N35 C34 . . 1.332(5) ? C1 H1 . . .98(4) ? C12 C13 . . 1.398(7) ? C12 H12 . . .96(5) ? C13 C14 . . 1.335(7) ? C13 H13 . . .84(4) ? C14 H14 . . .93(4) ? C22 C23 . . 1.393(8) ? C22 H22 . . 1.06(4) ? C23 C24 . . 1.347(7) ? C23 H23 . . .87(5) ? C24 H24 . . 1.00(4) ? C32 C33 . . 1.382(7) ? C32 H32 . . .92(4) ? C33 C34 . . 1.359(7) ? C33 H33 . . .87(4) ? C34 H34 . . .96(4) ? N100 O101 . . 1.26(3) ? N100 O102 . . 1.204(17) ? N100 O103 . . 1.167(14) ? N100 O104 . . 1.21(2) ? N100 O105 . . 1.202(13) ? N100 O106 . . 1.16(2) ? O101 O106 . . .28(4) ? O102 O104 . . 1.74(2) ? O102 O105 . . .863(17) ? O103 O104 . . .66(3) ? O103 O106 . . 1.88(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Fe N21 . . . 87.75(13) ? N11 Fe N31 . . . 87.07(12) ? N11 Fe N11 . . '3 655' 180.0000 ? N11 Fe N21 . . '3 655' 92.25(13) ? N11 Fe N31 . . '3 655' 92.93(12) ? N21 Fe N31 . . . 88.02(13) ? N21 Fe N11 . . '3 655' 92.25(13) ? N21 Fe N21 . . '3 655' 180.0000 ? N21 Fe N31 . . '3 655' 91.98(13) ? N31 Fe N11 . . '3 655' 92.93(12) ? N31 Fe N21 . . '3 655' 91.98(13) ? N31 Fe N31 . . '3 655' 180.0000 ? N11 Fe N21 '3 655' . '3 655' 87.75(13) ? N11 Fe N31 '3 655' . '3 655' 87.07(12) ? N21 Fe N31 '3 655' . '3 655' 88.02(13) ? Fe N11 N15 . . . 117.0(2) ? Fe N11 C12 . . . 137.0(3) ? N15 N11 C12 . . . 105.7(3) ? N11 N15 C1 . . . 119.2(3) ? N11 N15 C14 . . . 110.2(3) ? C1 N15 C14 . . . 130.5(4) ? Fe N21 N25 . . . 118.2(2) ? Fe N21 C22 . . . 136.8(3) ? N25 N21 C22 . . . 105.1(3) ? N21 N25 C1 . . . 118.3(3) ? N21 N25 C24 . . . 111.7(3) ? C1 N25 C24 . . . 130.0(4) ? Fe N31 N35 . . . 118.4(2) ? Fe N31 C32 . . . 137.5(3) ? N35 N31 C32 . . . 104.1(3) ? N31 N35 C1 . . . 117.1(3) ? N31 N35 C34 . . . 111.7(3) ? C1 N35 C34 . . . 131.0(4) ? N15 C1 N25 . . . 110.8(3) ? N15 C1 N35 . . . 109.7(3) ? N15 C1 H1 . . . 109(2) ? N25 C1 N35 . . . 108.9(3) ? N25 C1 H1 . . . 112(2) ? N35 C1 H1 . . . 106(2) ? N11 C12 C13 . . . 110.5(4) ? N11 C12 H12 . . . 121(2) ? C13 C12 H12 . . . 129(2) ? C12 C13 C14 . . . 106.6(4) ? C12 C13 H13 . . . 125(3) ? C14 C13 H13 . . . 128(3) ? N15 C14 C13 . . . 107.0(4) ? N15 C14 H14 . . . 119(2) ? C13 C14 H14 . . . 134(2) ? N21 C22 C23 . . . 109.7(4) ? N21 C22 H22 . . . 119(2) ? C23 C22 H22 . . . 131(2) ? C22 C23 C24 . . . 106.9(5) ? C22 C23 H23 . . . 128(3) ? C24 C23 H23 . . . 125(3) ? N25 C24 C23 . . . 106.6(4) ? N25 C24 H24 . . . 120(2) ? C23 C24 H24 . . . 132(2) ? N31 C32 C33 . . . 111.2(4) ? N31 C32 H32 . . . 119(2) ? C33 C32 H32 . . . 130(2) ? C32 C33 C34 . . . 105.8(4) ? C32 C33 H33 . . . 129(3) ? C34 C33 H33 . . . 125(3) ? N35 C34 C33 . . . 107.2(4) ? N35 C34 H34 . . . 125(2) ? C33 C34 H34 . . . 128(2) ? O101 N100 O102 . . . 122.6(14) ? O101 N100 O103 . . . 120.8(16) ? O101 N100 O104 . . . 132.4(13) ? O101 N100 O105 . . . 108.4(13) ? O101 N100 O106 . . . 12.6(18) ? O102 N100 O103 . . . 115.6(13) ? O102 N100 O104 . . . 92.2(12) ? O102 N100 O105 . . . 42.1(9) ? O102 N100 O106 . . . 134.5(16) ? O103 N100 O104 . . . 32.3(13) ? O103 N100 O105 . . . 121.7(13) ? O103 N100 O106 . . . 108.3(17) ? O104 N100 O105 . . . 119.0(11) ? O104 N100 O106 . . . 121.5(15) ? O105 N100 O106 . . . 119.4(14) ? N100 O101 O106 . . . 63(6) ? N100 O102 O104 . . . 44.0(9) ? N100 O102 O105 . . . 68.9(13) ? O104 O102 O105 . . . 100.5(16) ? N100 O103 O104 . . . 77(2) ? N100 O103 O106 . . . 35.6(10) ? O104 O103 O106 . . . 96(2) ? N100 O104 O102 . . . 43.8(8) ? N100 O104 O103 . . . 71(2) ? O102 O104 O103 . . . 104(2) ? N100 O105 O102 . . . 69.0(14) ? N100 O106 O101 . . . 104(7) ? N100 O106 O103 . . . 36.1(10) ? O101 O106 O103 . . . 140(7) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #----------------------------------------------------------------------- # Special items requested by author for inclusion in paper #----------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #----------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Fe N15 2.866(3) . . ? Fe N15 2.866(3) . '3 655' ? Fe N25 2.866(3) . '3 655' ? Fe N25 2.866(3) . . ? Fe N35 2.879(3) . '3 655' ? Fe N35 2.879(3) . . ? Fe C1 3.000(4) . . ? Fe C1 3.000(4) . '3 655' ? Fe C12 3.064(4) . '3 655' ? Fe C12 3.064(4) . . ? Fe C22 3.079(5) . . ? Fe C22 3.079(5) . '3 655' ? Fe C32 3.079(4) . . ? Fe C32 3.079(4) . '3 655' ? N11 N21 2.841(5) . '3 655' ? N11 N21 2.731(4) . . ? N11 N25 2.881(4) . . ? N11 N31 2.712(4) . . ? N11 N31 2.855(5) . '3 655' ? N11 N35 2.899(4) . . ? N11 C1 2.404(5) . . ? N11 C13 2.224(5) . . ? N11 C14 2.238(6) . . ? N11 H12 1.98(4) . . ? N15 N21 2.875(5) . . ? N15 N25 2.356(4) . . ? N15 N31 2.843(4) . . ? N15 N35 2.350(4) . . ? N15 C12 2.133(6) . . ? N15 C13 2.169(6) . . ? N15 H1 1.97(4) . . ? N15 H14 1.99(4) . . ? N21 N31 2.730(4) . . ? N21 N31 2.826(5) . '3 655' ? N21 N35 2.870(4) . . ? N21 C1 2.398(5) . . ? N21 C23 2.233(7) . . ? N21 C24 2.236(6) . . ? N21 H22 2.07(4) . . ? N25 N31 2.883(5) . . ? N25 N35 2.352(4) . . ? N25 C22 2.136(6) . . ? N25 C23 2.159(6) . . ? N25 H1 2.03(4) . . ? N25 H24 2.05(4) . . ? N31 C1 2.408(5) . . ? N31 C33 2.239(5) . . ? N31 C34 2.236(5) . . ? N31 H32 1.95(4) . . ? N35 C32 2.130(6) . . ? N35 C33 2.165(6) . . ? N35 H1 1.97(4) . . ? N35 H34 2.04(4) . . ? C1 C14 2.529(6) . . ? C1 C24 2.526(7) . . ? C1 C34 2.534(6) . . ? C12 C14 2.192(7) . . ? C12 H13 2.00(4) . . ? C13 H12 2.13(5) . . ? C13 H14 2.09(4) . . ? C14 H13 1.97(4) . . ? C22 C24 2.201(7) . . ? C22 H23 2.05(5) . . ? C23 H22 2.24(4) . . ? C23 H24 2.16(4) . . ? C24 H23 1.98(5) . . ? C32 C34 2.187(7) . . ? C32 H33 2.05(4) . . ? C33 H32 2.09(4) . . ? C33 H34 2.09(4) . . ? C34 H33 2.00(4) . . ? O101 O102 2.16(3) . . ? O101 O103 2.11(3) . . ? O101 O104 2.25(3) . . ? O101 O105 1.99(3) . . ? O101 H32 2.42(5) . '1 566' ? O102 O103 2.01(2) . . ? O102 O106 2.18(3) . . ? O102 H1 2.07(4) . 4 ? O102 H23 2.32(5) . '4 565' ? O103 O105 2.07(2) . . ? O103 H24 2.36(4) . 4 ? O104 O105 2.08(2) . . ? O104 O106 2.06(3) . . ? O104 H1 2.44(4) . 4 ? O104 H24 2.40(4) . 4 ? O105 O106 2.04(2) . . ? O105 H1 2.25(4) . 4 ? O105 H23 2.39(5) . '4 565' ? O106 H32 2.34(5) . '1 566' ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 624 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 8 0 0 -8 0 0 0 6 0 0 -6 0 0 0 22 0 0 -22 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 9.119 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .059 _refine_ls_wR_factor_all .058 _refine_ls_goodness_of_fit_all 1.457 _refine_ls_shift/su_mean .0028 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end- data_fepz3 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H20 Fe1 N14 O6' _chemical_formula_moiety ? _chemical_formula_weight 608.32 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 7.739(4) _cell_length_b 9.9690(10) _cell_length_c 16.321(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.21(3) _cell_angle_gamma 90.00000 _cell_volume 1220.6(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 18.29 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .688 _exptl_crystal_description ? _exptl_crystal_size_max .53 _exptl_crystal_size_mid .29 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .813 _exptl_absorpt_correction_T_max .884 _diffrn_reflns_number 3536 _reflns_number_total 3536 _reflns_Friedel_coverage ? _reflns_number_gt 2354 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 6 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .044 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.586 _refine_ls_number_reflns 2354 _refine_ls_number_parameters 228 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .033 _refine_diff_density_min -.38 _refine_diff_density_max .46 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf-Nonius software' _computing_cell_refinement 'Enraf-Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 40 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 40 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 2 .301025 .844971 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 0 .132019 .158997 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe .50000 1.00000 1.00000 .0289(2) Uani ? ? 1.00000 ? ? N11 .6155(3) .8803(2) .93409(14) .0328(11) Uani ? ? 1.00000 ? ? N15 .6946(3) .7670(2) .97185(14) .0338(11) Uani ? ? 1.00000 ? ? N21 .7088(3) .9738(2) 1.09430(14) .0342(11) Uani ? ? 1.00000 ? ? N25 .7724(3) .8467(2) 1.11133(14) .0343(11) Uani ? ? 1.00000 ? ? N31 .3969(3) .8405(2) 1.03929(14) .0336(11) Uani ? ? 1.00000 ? ? N35 .5018(3) .7310(2) 1.06108(14) .0346(11) Uani ? ? 1.00000 ? ? C1 .6848(4) .7397(3) 1.05755(18) .0352(13) Uani ? ? 1.00000 ? ? C12 .6521(4) .8826(3) .85834(18) .0382(14) Uani ? ? 1.00000 ? ? C13 .7561(4) .7721(3) .8491(2) .0456(16) Uani ? ? 1.00000 ? ? C14 .7822(4) .7006(3) .9218(2) .0398(15) Uani ? ? 1.00000 ? ? C22 .8171(4) 1.0494(3) 1.1512(2) .0418(15) Uani ? ? 1.00000 ? ? C23 .9492(4) .9727(3) 1.2031(2) .0471(17) Uani ? ? 1.00000 ? ? C24 .9159(4) .8445(3) 1.17728(18) .0402(15) Uani ? ? 1.00000 ? ? C32 .2400(4) .8047(3) 1.0524(2) .0419(15) Uani ? ? 1.00000 ? ? C33 .2471(5) .6732(3) 1.0829(2) .0489(17) Uani ? ? 1.00000 ? ? C34 .4151(4) .6292(3) 1.08759(19) .0423(15) Uani ? ? 1.00000 ? ? N100 .8624(4) .4213(2) 1.17051(17) .0449(14) Uani ? ? 1.00000 ? ? O101 .9441(4) .5209(2) 1.15297(19) .0787(17) Uani ? ? 1.00000 ? ? O102 .9293(3) .3534(2) 1.23306(15) .0577(13) Uani ? ? 1.00000 ? ? O103 .7139(3) .3927(3) 1.12482(16) .0732(16) Uani ? ? 1.00000 ? ? H1 .745(3) .658(2) 1.0773(15) .024(6) Uiso ? ? 1.00000 ? ? H12 .596(4) .955(3) .8199(18) .046(8) Uiso ? ? 1.00000 ? ? H13 .804(4) .747(3) .807(2) .063(10) Uiso ? ? 1.00000 ? ? H14 .847(3) .619(3) .9433(17) .039(8) Uiso ? ? 1.00000 ? ? H22 .804(3) 1.138(3) 1.1514(17) .033(7) Uiso ? ? 1.00000 ? ? H23 1.030(4) 1.004(3) 1.246(2) .061(10) Uiso ? ? 1.00000 ? ? H24 .967(4) .768(3) 1.1939(19) .055(10) Uiso ? ? 1.00000 ? ? H32 .146(4) .871(3) 1.0399(18) .047(9) Uiso ? ? 1.00000 ? ? H33 .157(4) .624(3) 1.096(2) .069(11) Uiso ? ? 1.00000 ? ? H34 .477(4) .547(3) 1.1030(18) .042(8) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe .0336(3) .0210(2) .0343(3) .0001(2) .0121(2) .0007(2) N11 .0398(13) .0264(11) .0345(12) .0009(10) .0138(10) .0007(9) N15 .0389(13) .0265(11) .0388(12) .0029(10) .0148(11) -.0013(10) N21 .0407(13) .0240(11) .0387(13) -.0002(9) .0112(10) .0007(9) N25 .0378(13) .0271(11) .0379(13) .0014(10) .0088(10) .0012(10) N31 .0376(13) .0255(11) .0399(13) .0006(10) .0138(10) .0002(10) N35 .0419(13) .0245(11) .0388(13) -.0016(10) .0127(11) .0036(10) C1 .0412(16) .0235(13) .0403(16) .0023(12) .0090(13) .0028(12) C12 .0411(16) .0389(16) .0365(15) -.0005(13) .0129(13) -.0015(13) C13 .0478(18) .0464(18) .0484(19) .0010(14) .0228(16) -.0113(15) C14 .0372(16) .0317(15) .0515(19) .0025(13) .0126(14) -.0099(14) C22 .0495(18) .0340(15) .0448(17) -.0092(14) .0170(15) -.0048(14) C23 .0482(19) .052(2) .0374(17) -.0080(15) .0034(14) -.0055(14) C24 .0378(16) .0468(18) .0344(15) .0044(14) .0056(13) .0079(14) C32 .0439(17) .0342(15) .0529(19) -.0025(13) .0219(15) .0031(14) C33 .055(2) .0354(16) .063(2) -.0087(15) .0286(17) .0058(15) C34 .054(2) .0288(15) .0470(17) -.0061(13) .0183(15) .0050(13) N100 .0568(17) .0327(13) .0517(16) .0055(12) .0255(14) -.0038(12) O101 .092(2) .0448(15) .110(2) -.0059(13) .0438(17) .0185(14) O102 .0719(16) .0457(13) .0571(14) .0121(12) .0190(12) .0113(11) O103 .0655(17) .0789(19) .0693(17) .0035(15) .0050(14) -.0130(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Fe N11 . . 1.963(2) ? Fe N21 . . 1.956(2) ? Fe N31 . . 1.957(2) ? Fe N11 . '3 677' 1.963(2) ? Fe N21 . '3 677' 1.956(2) ? Fe N31 . '3 677' 1.957(2) ? N11 N15 . . 1.358(3) ? N11 C12 . . 1.335(4) ? N15 C1 . . 1.445(4) ? N15 C14 . . 1.355(4) ? N21 N25 . . 1.363(3) ? N21 C22 . . 1.324(4) ? N25 C1 . . 1.440(3) ? N25 C24 . . 1.344(3) ? N31 N35 . . 1.355(3) ? N31 C32 . . 1.332(4) ? N35 C1 . . 1.434(4) ? N35 C34 . . 1.345(4) ? C1 H1 . . .96(2) ? C12 C13 . . 1.394(5) ? C12 H12 . . .99(3) ? C13 C14 . . 1.357(5) ? C13 H13 . . .89(4) ? C14 H14 . . .97(3) ? C22 C23 . . 1.386(4) ? C22 H22 . . .89(3) ? C23 C24 . . 1.350(5) ? C23 H23 . . .87(3) ? C24 H24 . . .87(3) ? C32 C33 . . 1.399(4) ? C32 H32 . . .97(3) ? C33 C34 . . 1.357(5) ? C33 H33 . . .92(4) ? C34 H34 . . .96(3) ? N100 O101 . . 1.248(4) ? N100 O102 . . 1.228(3) ? N100 O103 . . 1.240(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Fe N21 . . . 87.16(9) ? N11 Fe N31 . . . 87.87(10) ? N11 Fe N11 . . '3 677' 180.0000 ? N11 Fe N21 . . '3 677' 92.84(9) ? N11 Fe N31 . . '3 677' 92.13(10) ? N21 Fe N31 . . . 87.61(9) ? N21 Fe N11 . . '3 677' 92.84(9) ? N21 Fe N21 . . '3 677' 180.0000 ? N21 Fe N31 . . '3 677' 92.39(9) ? N31 Fe N11 . . '3 677' 92.13(10) ? N31 Fe N21 . . '3 677' 92.39(9) ? N31 Fe N31 . . '3 677' 180.0000 ? N11 Fe N21 '3 677' . '3 677' 87.16(9) ? N11 Fe N31 '3 677' . '3 677' 87.87(10) ? N21 Fe N31 '3 677' . '3 677' 87.61(9) ? Fe N11 N15 . . . 118.16(18) ? Fe N11 C12 . . . 136.54(19) ? N15 N11 C12 . . . 105.1(2) ? N11 N15 C1 . . . 118.1(2) ? N11 N15 C14 . . . 111.6(2) ? C1 N15 C14 . . . 130.1(2) ? Fe N21 N25 . . . 118.14(15) ? Fe N21 C22 . . . 137.3(2) ? N25 N21 C22 . . . 104.6(2) ? N21 N25 C1 . . . 118.1(2) ? N21 N25 C24 . . . 111.3(2) ? C1 N25 C24 . . . 130.5(2) ? Fe N31 N35 . . . 118.31(18) ? Fe N31 C32 . . . 137.01(19) ? N35 N31 C32 . . . 104.7(2) ? N31 N35 C1 . . . 118.4(2) ? N31 N35 C34 . . . 112.2(2) ? C1 N35 C34 . . . 129.4(2) ? N15 C1 N25 . . . 108.8(2) ? N15 C1 N35 . . . 109.7(2) ? N15 C1 H1 . . . 110.5(16) ? N25 C1 N35 . . . 110.0(2) ? N25 C1 H1 . . . 108.0(13) ? N35 C1 H1 . . . 109.9(15) ? N11 C12 C13 . . . 110.2(3) ? N11 C12 H12 . . . 116.3(19) ? C13 C12 H12 . . . 133.3(19) ? C12 C13 C14 . . . 106.6(3) ? C12 C13 H13 . . . 131(2) ? C14 C13 H13 . . . 122(2) ? N15 C14 C13 . . . 106.4(3) ? N15 C14 H14 . . . 118.8(18) ? C13 C14 H14 . . . 134.9(18) ? N21 C22 C23 . . . 111.1(3) ? N21 C22 H22 . . . 120.8(15) ? C23 C22 H22 . . . 128.0(15) ? C22 C23 C24 . . . 106.0(3) ? C22 C23 H23 . . . 125(2) ? C24 C23 H23 . . . 129(2) ? N25 C24 C23 . . . 107.0(3) ? N25 C24 H24 . . . 119.3(19) ? C23 C24 H24 . . . 133.8(19) ? N31 C32 C33 . . . 110.5(3) ? N31 C32 H32 . . . 116.6(18) ? C33 C32 H32 . . . 132.8(18) ? C32 C33 C34 . . . 106.0(3) ? C32 C33 H33 . . . 128(2) ? C34 C33 H33 . . . 126(2) ? N35 C34 C33 . . . 106.6(3) ? N35 C34 H34 . . . 118.4(18) ? C33 C34 H34 . . . 135.0(18) ? O101 N100 O102 . . . 119.7(3) ? O101 N100 O103 . . . 119.5(3) ? O102 N100 O103 . . . 120.8(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Fe N15 2.866(2) . . ? Fe N15 2.866(2) . '3 677' ? Fe N25 2.864(2) . '3 677' ? Fe N25 2.864(2) . . ? Fe N35 2.860(2) . . ? Fe N35 2.860(2) . '3 677' ? Fe C1 3.000(3) . '3 677' ? Fe C1 3.000(3) . . ? Fe C12 3.072(3) . '3 677' ? Fe C12 3.072(3) . . ? Fe C22 3.063(3) . '3 677' ? Fe C22 3.063(3) . . ? Fe C32 3.068(3) . . ? Fe C32 3.068(3) . '3 677' ? N11 N21 2.702(3) . . ? N11 N21 2.839(3) . '3 677' ? N11 N25 2.869(3) . . ? N11 N31 2.823(3) . '3 677' ? N11 N31 2.719(4) . . ? N11 N35 2.860(3) . . ? N11 C1 2.404(4) . . ? N11 C13 2.239(4) . . ? N11 C14 2.245(4) . . ? N11 H12 1.98(3) . . ? N15 N21 2.855(3) . . ? N15 N25 2.346(3) . . ? N15 N31 2.881(4) . . ? N15 N35 2.354(4) . . ? N15 C12 2.138(4) . . ? N15 C13 2.171(4) . . ? N15 H1 1.99(2) . . ? N15 H14 2.01(3) . . ? N21 N31 2.708(3) . . ? N21 N31 2.824(3) . '3 677' ? N21 N35 2.879(3) . . ? N21 C1 2.405(3) . . ? N21 C23 2.234(4) . . ? N21 C24 2.236(4) . . ? N21 H22 1.94(3) . . ? N25 N31 2.856(3) . . ? N25 N35 2.354(3) . . ? N25 C22 2.125(4) . . ? N25 C23 2.165(4) . . ? N25 H1 1.96(2) . . ? N25 H24 1.93(3) . . ? N31 C1 2.395(4) . . ? N31 C33 2.244(4) . . ? N31 C34 2.241(4) . . ? N31 H32 1.97(3) . . ? N35 C32 2.127(4) . . ? N35 C33 2.166(5) . . ? N35 H1 1.98(2) . . ? N35 H34 1.99(3) . . ? C1 C14 2.540(5) . . ? C1 C24 2.529(4) . . ? C1 C34 2.512(5) . . ? C12 C14 2.206(4) . . ? C12 H13 2.10(3) . . ? C13 H12 2.19(3) . . ? C13 H14 2.15(3) . . ? C14 H13 1.98(3) . . ? C22 C24 2.185(5) . . ? C22 H23 2.01(3) . . ? C23 H22 2.06(3) . . ? C23 H24 2.05(3) . . ? C24 H23 2.02(3) . . ? C32 C34 2.201(4) . . ? C32 H33 2.09(3) . . ? C33 H32 2.17(3) . . ? C33 H34 2.14(3) . . ? C34 H33 2.04(4) . . ? O101 O102 2.141(4) . . ? O101 O103 2.149(4) . . ? O101 H1 2.20(2) . . ? O101 H33 2.32(4) . '1 655' ? O102 O103 2.146(3) . . ? O103 H34 2.35(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 624 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 0 -6 -6 0 6 0 -8 0 0 8 0 0 0 -14 0 0 14 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 0 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed 2354 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 0 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .050 _refine_ls_goodness_of_fit_all 1.421 _refine_ls_shift/su_mean .005 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end- #==END data_ertfe1 #----------------------------------------------------------------------- _audit_creation_date 'Wed Jan 21 12:46:48 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution ? _computing_structure_refinement teXsan _computing_publication_material teXsan #----------------------------------------------------------------------- _cell_length_a 8.539(4) _cell_length_b 10.405(4) _cell_length_c 16.500(10) _cell_angle_alpha 90 _cell_angle_beta 102.99(4) _cell_angle_gamma 90 _cell_volume 1428(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 12.4 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas ? _chemical_formula_weight 674.45 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H26 Fe N8 O6 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.710 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Mo_K\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC6R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% -0.05 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 1 2 -2 0 2 0 0 _diffrn_reflns_number 3837 _reflns_number_total 3606 _reflns_number_observed 2592 _reflns_observed_criterion I>3.0sigma(I) _diffrn_reflns_av_R_equivalents .0892 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02531 _diffrn_orient_matrix_UB_12 -0.09118 _diffrn_orient_matrix_UB_13 -0.01718 _diffrn_orient_matrix_UB_21 0.08207 _diffrn_orient_matrix_UB_22 0.00284 _diffrn_orient_matrix_UB_23 -0.03470 _diffrn_orient_matrix_UB_31 0.08407 _diffrn_orient_matrix_UB_32 -0.03024 _diffrn_orient_matrix_UB_33 0.04867 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.003 0.002 'International Tables' H 0 52 0.000 0.000 'International Tables' Fe 0 2 0.346 0.844 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 12 0.011 0.006 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe 0.0000 0.5000 0.0000 0.0234(1) Uij ? ? O1 0.9185(3) 0.3767(2) 0.7189(1) 0.0607(7) Uij ? ? O2 0.7292(3) 0.4182(3) 0.6140(1) 0.0779(8) Uij ? ? O3 0.9436(3) 0.5306(2) 0.6392(2) 0.0871(9) Uij ? ? N1 0.8637(3) 0.4421(2) 0.6571(2) 0.0467(7) Uij ? ? N11 0.1836(2) 0.5186(2) 0.0942(1) 0.0259(5) Uij ? ? N21 0.1062(2) 0.6144(2) -0.0641(1) 0.0264(5) Uij ? ? N31 -0.0984(2) 0.6490(2) 0.0399(1) 0.0268(5) Uij ? ? C1 0.1639(3) 0.7423(2) 0.0596(1) 0.0297(6) Uij ? ? C12 0.2530(3) 0.4196(2) 0.1406(1) 0.0316(6) Uij ? ? C13 0.3800(3) 0.4344(2) 0.2062(1) 0.0385(7) Uij ? ? C14 0.4392(3) 0.5545(3) 0.2266(2) 0.0421(7) Uij ? ? C15 0.3698(3) 0.6568(2) 0.1803(1) 0.0346(6) Uij ? ? C16 0.2434(3) 0.6357(2) 0.1146(1) 0.0273(5) Uij ? ? C22 0.1167(3) 0.5909(2) -0.1428(1) 0.0339(6) Uij ? ? C23 0.2040(3) 0.6664(3) -0.1837(1) 0.0403(7) Uij ? ? C24 0.2847(3) 0.7703(3) -0.1443(2) 0.0440(7) Uij ? ? C25 0.2724(3) 0.7973(2) -0.0650(2) 0.0373(7) Uij ? ? C26 0.1817(3) 0.7190(2) -0.0270(1) 0.0288(6) Uij ? ? C32 -0.2534(3) 0.6543(2) 0.0437(1) 0.0353(6) Uij ? ? C33 -0.3204(3) 0.7600(3) 0.0708(2) 0.0402(7) Uij ? ? C34 -0.2284(3) 0.8665(2) 0.0928(2) 0.0420(7) Uij ? ? C35 -0.0712(3) 0.8644(2) 0.0882(1) 0.0372(7) Uij ? ? C36 -0.0091(3) 0.7536(2) 0.0627(1) 0.0288(5) Uij ? ? H1 0.2176 0.8223 0.0792 0.0356 Uij ? ? H12 0.2108 0.3338 0.1268 0.0379 Uij ? ? H13 0.4280 0.3604 0.2381 0.0462 Uij ? ? H14 0.5295 0.5673 0.2734 0.0505 Uij ? ? H15 0.4097 0.7432 0.1939 0.0415 Uij ? ? H22 0.0611 0.5189 -0.1709 0.0407 Uij ? ? H23 0.2087 0.6465 -0.2405 0.0484 Uij ? ? H24 0.3496 0.8238 -0.1721 0.0528 Uij ? ? H25 0.3273 0.8712 -0.0359 0.0448 Uij ? ? H32 -0.3207 0.5797 0.0264 0.0424 Uij ? ? H33 -0.4323 0.7594 0.0743 0.0482 Uij ? ? H34 -0.2742 0.9432 0.1117 0.0504 Uij ? ? H35 -0.0041 0.9399 0.1026 0.0446 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe 0.0237(2) 0.0209(2) 0.0248(2) -0.0025(2) 0.0039(2) -0.0018(2) O1 0.067(1) 0.056(1) 0.061(1) 0.015(1) 0.020(1) 0.008(1) O2 0.058(1) 0.091(2) 0.078(2) 0.003(1) -0.001(1) -0.021(1) O3 0.077(2) 0.050(1) 0.140(2) -0.004(1) 0.035(2) 0.029(1) N1 0.046(1) 0.038(1) 0.060(1) 0.011(1) 0.018(1) -0.005(1) N11 0.0261(9) 0.0241(10) 0.0269(9) -0.0014(7) 0.0044(7) -0.0005(7) N21 0.0268(9) 0.0256(9) 0.0258(9) -0.0008(8) 0.0038(7) 0.0003(8) N31 0.0271(9) 0.0261(10) 0.0264(9) -0.0003(8) 0.0040(8) -0.0023(7) C1 0.033(1) 0.023(1) 0.031(1) -0.0052(9) 0.0014(10) -0.0023(9) C12 0.032(1) 0.029(1) 0.033(1) 0.0007(10) 0.0049(10) 0.0027(10) C13 0.037(1) 0.041(1) 0.034(1) 0.002(1) 0.000(1) 0.007(1) C14 0.036(1) 0.048(1) 0.034(1) -0.007(1) -0.008(1) 0.004(1) C15 0.035(1) 0.036(1) 0.030(1) -0.009(1) 0.0006(10) -0.002(1) C16 0.026(1) 0.028(1) 0.027(1) -0.0036(9) 0.0040(9) -0.0024(9) C22 0.034(1) 0.037(1) 0.030(1) 0.002(1) 0.0075(10) 0.002(1) C23 0.038(1) 0.051(2) 0.034(1) 0.003(1) 0.013(1) 0.008(1) C24 0.035(1) 0.049(2) 0.050(2) -0.005(1) 0.013(1) 0.017(1) C25 0.031(1) 0.034(1) 0.044(1) -0.006(1) 0.003(1) 0.010(1) C26 0.026(1) 0.026(1) 0.032(1) -0.0017(9) 0.0014(9) 0.0045(9) C32 0.030(1) 0.038(1) 0.039(1) 0.001(1) 0.008(1) 0.000(1) C33 0.037(1) 0.043(1) 0.042(1) 0.010(1) 0.014(1) 0.002(1) C34 0.054(2) 0.034(1) 0.040(1) 0.015(1) 0.015(1) 0.001(1) C35 0.052(2) 0.027(1) 0.031(1) 0.003(1) 0.008(1) -0.0019(10) C36 0.035(1) 0.025(1) 0.024(1) 0.0003(9) 0.0035(9) -0.0016(9) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 5.72963 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2592 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0371 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0438 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.438 _refine_ls_shift/esd_max 0.0014 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.30 _refine_diff_density_max 0.38 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N(11) 1.954(2) ? ? yes Fe N(11)' 1.954(2) ? ? yes Fe N(21) 1.947(2) ? ? yes Fe N(21)' 1.947(2) ? ? yes Fe N(31) 1.947(2) ? ? yes Fe N(31)' 1.947(2) ? ? yes O(1) N(1) 1.228(3) ? ? yes O(2) N(1) 1.232(3) ? ? yes O(3) N(1) 1.221(3) ? ? yes N(11) C(12) 1.339(3) ? ? yes N(11) C(16) 1.335(3) ? ? yes N(21) C(22) 1.343(3) ? ? yes N(21) C(26) 1.340(3) ? ? yes N(31) C(32) 1.340(3) ? ? yes N(31) C(36) 1.334(3) ? ? yes C(1) C(16) 1.496(3) ? ? yes C(1) C(26) 1.490(3) ? ? yes C(1) C(36) 1.495(3) ? ? yes C(12) C(13) 1.358(3) ? ? yes C(13) C(14) 1.362(4) ? ? yes C(14) C(15) 1.365(3) ? ? yes C(15) C(16) 1.364(3) ? ? yes C(22) C(23) 1.362(3) ? ? yes C(23) C(24) 1.365(4) ? ? yes C(24) C(25) 1.365(4) ? ? yes C(25) C(26) 1.370(3) ? ? yes C(32) C(33) 1.361(3) ? ? yes C(33) C(34) 1.360(4) ? ? yes C(34) C(35) 1.362(4) ? ? yes C(35) C(36) 1.373(3) ? ? yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(11) Fe N(11)' 180.0 ? ? ? yes N(11) Fe N(21) 89.07(7) ? ? ? yes N(11) Fe N(21)' 90.93(7) ? ? ? yes N(11) Fe N(31) 88.99(7) ? ? ? yes N(11) Fe N(31)' 91.01(7) ? ? ? yes N(11)' Fe N(21) 90.93(7) ? ? ? yes N(11)' Fe N(21)' 89.07(7) ? ? ? yes N(11)' Fe N(31) 91.01(7) ? ? ? yes N(11)' Fe N(31)' 88.99(7) ? ? ? yes N(21) Fe N(21)' 180.0 ? ? ? yes N(21) Fe N(31) 89.20(8) ? ? ? yes N(21) Fe N(31)' 90.80(8) ? ? ? yes N(21)' Fe N(31) 90.80(8) ? ? ? yes N(21)' Fe N(31)' 89.20(8) ? ? ? yes N(31) Fe N(31)' 180.0 ? ? ? yes O(1) N(1) O(2) 119.9(3) ? ? ? yes O(1) N(1) O(3) 119.3(3) ? ? ? yes O(2) N(1) O(3) 120.7(3) ? ? ? yes Fe N(11) C(12) 123.5(1) ? ? ? yes Fe N(11) C(16) 118.9(1) ? ? ? yes C(12) N(11) C(16) 117.6(2) ? ? ? yes Fe N(21) C(22) 123.6(2) ? ? ? yes Fe N(21) C(26) 118.8(1) ? ? ? yes C(22) N(21) C(26) 117.4(2) ? ? ? yes Fe N(31) C(32) 123.7(2) ? ? ? yes Fe N(31) C(36) 118.8(2) ? ? ? yes C(32) N(31) C(36) 117.5(2) ? ? ? yes C(16) C(1) C(26) 109.3(2) ? ? ? yes C(16) C(1) C(36) 110.8(2) ? ? ? yes C(26) C(1) C(36) 111.1(2) ? ? ? yes N(11) C(12) C(13) 122.7(2) ? ? ? yes C(12) C(13) C(14) 119.1(2) ? ? ? yes C(13) C(14) C(15) 119.1(2) ? ? ? yes C(14) C(15) C(16) 119.1(2) ? ? ? yes N(11) C(16) C(1) 115.4(2) ? ? ? yes N(11) C(16) C(15) 122.4(2) ? ? ? yes C(1) C(16) C(15) 122.2(2) ? ? ? yes N(21) C(22) C(23) 122.4(2) ? ? ? yes C(22) C(23) C(24) 119.7(2) ? ? ? yes C(23) C(24) C(25) 118.6(2) ? ? ? yes C(24) C(25) C(26) 119.3(2) ? ? ? yes N(21) C(26) C(1) 115.4(2) ? ? ? yes N(21) C(26) C(25) 122.4(2) ? ? ? yes C(1) C(26) C(25) 122.1(2) ? ? ? yes N(31) C(32) C(33) 122.8(2) ? ? ? yes C(32) C(33) C(34) 119.1(2) ? ? ? yes C(33) C(34) C(35) 119.3(2) ? ? ? yes C(34) C(35) C(36) 119.0(2) ? ? ? yes N(31) C(36) C(1) 115.7(2) ? ? ? yes N(31) C(36) C(35) 122.4(2) ? ? ? yes C(1) C(36) C(35) 121.9(2) ? ? ? yes #----------------------------------------------------------------------- #===END data_ertfe2 #----------------------------------------------------------------------- _audit_creation_date 'Mon Jun 1 15:26:05 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 11.129(3) _cell_length_b 13.699(3) _cell_length_c 11.239(3) _cell_angle_alpha 90 _cell_angle_beta 92.04(2) _cell_angle_gamma 90 _cell_volume 1712.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30.8 _cell_measurement_theta_max 35.5 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'multifaceted' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_meas ? _chemical_formula_weight 824.47 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H30 Fe N10 O8 P2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.844 _diffrn_special_details none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC6R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% -2.91 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 -2 -1 3 -1 -2 0 -2 _diffrn_reflns_number 4470 _reflns_number_total 4264 _reflns_number_observed 2496 _reflns_observed_criterion I>3.0sigma(I) _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01607 _diffrn_orient_matrix_UB_12 0.05218 _diffrn_orient_matrix_UB_13 -0.05959 _diffrn_orient_matrix_UB_21 -0.00267 _diffrn_orient_matrix_UB_22 -0.04985 _diffrn_orient_matrix_UB_23 -0.06504 _diffrn_orient_matrix_UB_31 -0.08842 _diffrn_orient_matrix_UB_32 0.01099 _diffrn_orient_matrix_UB_33 -0.01209 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' Fe 0 2 0.346 0.844 'International Tables' N 0 20 0.006 0.003 'International Tables' O 0 16 0.011 0.006 'International Tables' P 0 4 0.102 0.094 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe 0.0000 0.5000 0.0000 0.0235(2) Uij ? ? P1 0.2312(1) 0.38487(9) -0.0971(1) 0.0337(3) Uij ? ? O1 0.3319(5) 0.3385(5) -0.1405(6) 0.116(2) Uij ? ? O41 0.9197(5) 0.1875(4) 0.7750(6) 0.113(2) Uij ? ? O42 0.8600(4) 0.0540(4) 0.6992(5) 0.098(2) Uij ? ? O43 0.7968(5) 0.1001(4) 0.8616(5) 0.101(2) Uij ? ? N11 0.0595(3) 0.3740(3) 0.0651(3) 0.0272(9) Uij ? ? N21 0.0125(3) 0.4527(2) -0.1658(3) 0.0270(9) Uij ? ? N31 0.1648(3) 0.5553(2) 0.0007(3) 0.0259(8) Uij ? ? N41 0.8593(5) 0.1140(4) 0.7781(5) 0.061(2) Uij ? ? N51 0.2993(7) 0.1051(5) 0.8388(6) 0.099(3) Uij ? ? C12 0.0041(4) 0.3284(3) 0.1529(4) 0.033(1) Uij ? ? C13 0.0418(4) 0.2418(4) 0.2006(4) 0.040(1) Uij ? ? C14 0.1415(5) 0.1980(4) 0.1596(5) 0.045(1) Uij ? ? C15 0.2016(4) 0.2434(3) 0.0709(4) 0.039(1) Uij ? ? C16 0.1577(4) 0.3295(3) 0.0247(4) 0.028(1) Uij ? ? C22 -0.0756(4) 0.4694(3) -0.2470(4) 0.033(1) Uij ? ? C23 -0.0711(4) 0.4394(4) -0.3620(4) 0.040(1) Uij ? ? C24 0.0244(5) 0.3855(4) -0.3965(4) 0.046(1) Uij ? ? C25 0.1146(4) 0.3656(3) -0.3146(4) 0.041(1) Uij ? ? C26 0.1075(4) 0.4017(3) -0.2014(4) 0.031(1) Uij ? ? C32 0.1887(4) 0.6454(3) 0.0404(4) 0.032(1) Uij ? ? C33 0.2975(4) 0.6893(3) 0.0333(4) 0.039(1) Uij ? ? C34 0.3890(4) 0.6405(4) -0.0192(5) 0.043(1) Uij ? ? C35 0.3681(4) 0.5476(4) -0.0589(4) 0.036(1) Uij ? ? C36 0.2565(3) 0.5074(3) -0.0470(3) 0.0283(10) Uij ? ? C51 0.2148(7) 0.0655(6) 0.8610(6) 0.071(2) Uij ? ? C52 0.1129(7) 0.0137(7) 0.8920(7) 0.095(3) Uij ? ? H12 -0.0654 0.3580 0.1837 0.0382 Uij ? ? H13 -0.0016 0.2121 0.2623 0.0479 Uij ? ? H14 0.1690 0.1374 0.1916 0.0531 Uij ? ? H15 0.2730 0.2156 0.0417 0.0456 Uij ? ? H22 -0.1448 0.5039 -0.2232 0.0386 Uij ? ? H23 -0.1339 0.4558 -0.4178 0.0466 Uij ? ? H24 0.0281 0.3621 -0.4759 0.0548 Uij ? ? H25 0.1816 0.3272 -0.3359 0.0490 Uij ? ? H32 0.1258 0.6809 0.0756 0.0386 Uij ? ? H33 0.3100 0.7531 0.0644 0.0444 Uij ? ? H34 0.4651 0.6706 -0.0278 0.0496 Uij ? ? H35 0.4302 0.5113 -0.0943 0.0426 Uij ? ? H52a 0.0496 0.0581 0.9070 0.1095 Uij ? ? H52b 0.0889 -0.0286 0.8286 0.1095 Uij ? ? H52c 0.1307 -0.0237 0.9616 0.1141 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe 0.0228(4) 0.0240(4) 0.0237(4) 0.0013(4) 0.0005(3) -0.0003(4) P1 0.0321(6) 0.0351(6) 0.0343(6) 0.0021(5) 0.0044(5) 0.0007(5) O1 0.102(4) 0.117(5) 0.131(5) 0.023(4) 0.028(4) -0.009(4) O41 0.103(4) 0.079(4) 0.157(6) -0.021(3) 0.012(4) -0.025(4) O42 0.080(3) 0.111(4) 0.103(4) -0.003(3) 0.004(3) -0.056(4) O43 0.121(5) 0.107(4) 0.076(4) -0.004(4) 0.021(3) -0.009(3) N11 0.027(2) 0.028(2) 0.026(2) 0.001(1) -0.001(1) 0.001(1) N21 0.030(2) 0.026(2) 0.025(2) -0.002(1) 0.001(1) -0.002(1) N31 0.028(2) 0.024(2) 0.026(2) 0.000(1) 0.000(1) 0.000(1) N41 0.055(3) 0.062(3) 0.066(3) 0.005(3) -0.008(3) -0.010(3) N51 0.118(5) 0.095(5) 0.088(5) -0.008(4) 0.051(4) -0.020(4) C12 0.035(2) 0.037(2) 0.027(2) -0.001(2) 0.001(2) 0.001(2) C13 0.045(3) 0.037(3) 0.038(2) -0.003(2) 0.001(2) 0.013(2) C14 0.056(3) 0.033(3) 0.046(3) 0.010(2) -0.002(2) 0.010(2) C15 0.043(3) 0.034(2) 0.039(2) 0.010(2) -0.001(2) 0.001(2) C16 0.027(2) 0.031(2) 0.027(2) 0.002(2) -0.001(2) 0.001(2) C22 0.033(2) 0.033(2) 0.031(2) -0.005(2) -0.003(2) 0.001(2) C23 0.051(3) 0.036(3) 0.032(2) -0.009(2) -0.008(2) -0.001(2) C24 0.064(3) 0.044(3) 0.029(2) -0.005(3) -0.001(2) -0.011(2) C25 0.050(3) 0.034(3) 0.039(2) 0.000(2) 0.009(2) -0.006(2) C26 0.034(2) 0.028(2) 0.030(2) -0.001(2) 0.004(2) -0.003(2) C32 0.035(2) 0.032(2) 0.029(2) 0.001(2) -0.004(2) 0.004(2) C33 0.039(3) 0.037(3) 0.039(2) -0.011(2) -0.007(2) 0.005(2) C34 0.028(2) 0.049(3) 0.052(3) -0.010(2) -0.004(2) 0.008(2) C35 0.027(2) 0.044(3) 0.036(2) -0.001(2) 0.001(2) 0.009(2) C36 0.025(2) 0.033(2) 0.026(2) 0.002(2) -0.002(1) 0.006(2) C51 0.082(5) 0.085(5) 0.047(3) 0.008(4) 0.013(3) -0.004(3) C52 0.070(4) 0.133(8) 0.082(5) -0.008(5) 0.004(4) 0.019(5) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2496 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0540 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_shift/esd_max 0.0360 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.64 _refine_diff_density_max 0.52 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N(11) 1.980(3) ? ? yes Fe N(11)' 1.980(3) ? ? yes Fe N(21) 1.982(3) ? ? yes Fe N(21)' 1.982(3) ? ? yes Fe N(31) 1.984(3) ? ? yes Fe N(31)' 1.984(3) ? ? yes P(1) O(1) 1.391(5) ? ? yes P(1) C(16) 1.788(4) ? ? yes P(1) C(26) 1.791(4) ? ? yes P(1) C(36) 1.790(5) ? ? yes O(41) N(41) 1.213(7) ? ? yes O(42) N(41) 1.209(6) ? ? yes O(43) N(41) 1.202(7) ? ? yes N(11) C(12) 1.336(5) ? ? yes N(11) C(16) 1.346(5) ? ? yes N(21) C(22) 1.335(5) ? ? yes N(21) C(26) 1.342(5) ? ? yes N(31) C(32) 1.337(5) ? ? yes N(31) C(36) 1.341(5) ? ? yes N(51) C(51) 1.121(9) ? ? yes C(12) C(13) 1.362(6) ? ? yes C(13) C(14) 1.357(7) ? ? yes C(14) C(15) 1.370(7) ? ? yes C(15) C(16) 1.371(6) ? ? yes C(22) C(23) 1.359(6) ? ? yes C(23) C(24) 1.362(7) ? ? yes C(24) C(25) 1.365(7) ? ? yes C(25) C(26) 1.369(6) ? ? yes C(32) C(33) 1.356(6) ? ? yes C(33) C(34) 1.369(7) ? ? yes C(34) C(35) 1.366(7) ? ? yes C(35) C(36) 1.370(6) ? ? yes C(51) C(52) 1.393(10) ? ? yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(11) Fe N(11)' 180.0 ? ? ? yes N(11) Fe N(21) 91.7(1) ? ? ? yes N(11) Fe N(21)' 88.3(1) ? ? ? yes N(11) Fe N(31) 92.0(1) ? ? ? yes N(11) Fe N(31)' 88.0(1) ? ? ? yes N(11)' Fe N(21) 88.3(1) ? ? ? yes N(11)' Fe N(21)' 91.7(1) ? ? ? yes N(11)' Fe N(31) 88.0(1) ? ? ? yes N(11)' Fe N(31)' 92.0(1) ? ? ? yes N(21) Fe N(21)' 180.0 ? ? ? yes N(21) Fe N(31) 91.9(1) ? ? ? yes N(21) Fe N(31)' 88.1(1) ? ? ? yes N(21)' Fe N(31) 88.1(1) ? ? ? yes N(21)' Fe N(31)' 91.9(1) ? ? ? yes N(31) Fe N(31)' 180.0 ? ? ? yes O(1) P(1) C(16) 118.1(3) ? ? ? yes O(1) P(1) C(26) 116.0(3) ? ? ? yes O(1) P(1) C(36) 114.8(3) ? ? ? yes C(16) P(1) C(26) 101.2(2) ? ? ? yes C(16) P(1) C(36) 103.2(2) ? ? ? yes C(26) P(1) C(36) 101.2(2) ? ? ? yes Fe N(11) C(12) 121.6(3) ? ? ? yes Fe N(11) C(16) 122.4(3) ? ? ? yes C(12) N(11) C(16) 116.1(4) ? ? ? yes Fe N(21) C(22) 120.8(3) ? ? ? yes Fe N(21) C(26) 122.3(3) ? ? ? yes C(22) N(21) C(26) 116.9(4) ? ? ? yes Fe N(31) C(32) 121.8(3) ? ? ? yes Fe N(31) C(36) 121.9(3) ? ? ? yes C(32) N(31) C(36) 116.1(4) ? ? ? yes O(41) N(41) O(42) 121.7(6) ? ? ? yes O(41) N(41) O(43) 119.4(6) ? ? ? yes O(42) N(41) O(43) 118.9(6) ? ? ? yes N(11) C(12) C(13) 123.7(4) ? ? ? yes C(12) C(13) C(14) 119.7(4) ? ? ? yes C(13) C(14) C(15) 118.2(4) ? ? ? yes C(14) C(15) C(16) 119.3(4) ? ? ? yes P(1) C(16) N(11) 117.8(3) ? ? ? yes P(1) C(16) C(15) 119.2(3) ? ? ? yes N(11) C(16) C(15) 123.0(4) ? ? ? yes N(21) C(22) C(23) 123.1(4) ? ? ? yes C(22) C(23) C(24) 119.4(4) ? ? ? yes C(23) C(24) C(25) 118.6(4) ? ? ? yes C(24) C(25) C(26) 119.3(4) ? ? ? yes P(1) C(26) N(21) 117.9(3) ? ? ? yes P(1) C(26) C(25) 119.6(3) ? ? ? yes N(21) C(26) C(25) 122.5(4) ? ? ? yes N(31) C(32) C(33) 123.8(4) ? ? ? yes C(32) C(33) C(34) 119.3(4) ? ? ? yes C(33) C(34) C(35) 118.4(4) ? ? ? yes C(34) C(35) C(36) 119.1(4) ? ? ? yes P(1) C(36) N(31) 118.1(3) ? ? ? yes P(1) C(36) C(35) 118.6(3) ? ? ? yes N(31) C(36) C(35) 123.3(4) ? ? ? yes N(51) C(51) C(52) 177.5(9) ? ? ? yes #----------------------------------------------------------------------- _publ_requested_journal ' J. Chem. Soc., Dalton Trans ' _publ_contact_author ; Dr ERT TIEKINK, Department of Chemistry, The University of Adelaide, AUSTRALIA 5005 ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 8 8303 5943 ' _publ_contact_author_fax ' 61 8 8303 4358 ' _publ_contact_author_email ' edward.tiekink@adelaide.edu.au ' #==END