Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 #============================================================================== # 1. SUBMISSION DETAILS loop_ _publ_author_name 'Hazell, Alan' 'McKenzie, C. J.' 'Nielsen, Lars Preuss' 'Schindler, Siegfried' 'Weitzer, Markus' _publ_contact_author # Name and address of author for correspondence ; Christine J. McKenzie Department of Chemistry University of Southern Denmark, Main Campus: Odense University, Campusvej 55 DK-5230 Odense M, Denmark. ; _publ_contact_author_phone '+45 6550 2518' _publ_contact_author_fax '+45 6615 8780' _publ_contact_author_email chk@chem.sdu.dk _publ_requested_journal 'Dalton Transactions' #============================================================================== # 3. TITLE _publ_section_title ; Mononuclear non-heme iron(III) peroxide complexes: syntheses, characterisation, mass spectrometric and kinetic studies. ; data_Febztpenbr #================================== _database_code_CSD 163870 # 5. CHEMICAL DATA _chemical_name_systematic ; [Fe(bztpen)Br]PF6 ; _chemical_name_common [Fe(bztpen)Br]PF6 _chemical_formula_sum 'C27 H29 Br1 Cl1 Fe1 N5 O4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C27 H29 Br Fe N5, Cl O4' _chemical_formula_weight 658.79 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,-y,1/2+z' '-x,1/2+y,1/2-z' '1/2+x,1/2-y,-z' '-x,-y,-z' '1/2+x,+y,1/2-z' '+x,1/2-y,1/2+z' '1/2-x,1/2+y,+z' _cell_length_a 16.6209(7) _cell_length_b 17.8973(8) _cell_length_c 18.1065(8) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 5386.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120 _cell_measurement_reflns_used 6820 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 29.84 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 2.191 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP,1995' _exptl_absorpt_correction_T_min 0.391 _exptl_absorpt_correction_T_max 0.646 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 67452 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 29.84 _diffrn_reflns_reduction_process 67452 _reflns_number_total 7728 _reflns_number_gt 6422 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix the extinction coefficient was > 3sigma and was set to zero ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^-|F|}^2^ A = 0.03, B = 0.1 ; _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6422 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.033 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_shift/su_max 0.0012 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.64(7) _refine_diff_density_min -0.43(7) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe 0.36766(1) 0.22766(1) 0.71791(1) 0.0154(1) Uij Br 0.238340(10) 0.277503(10) 0.765255(10) 0.02274(9) Uij N1 0.49098(8) 0.18722(8) 0.69211(8) 0.0165(6) Uij N4 0.41297(8) 0.32274(8) 0.64656(8) 0.0172(7) Uij N11 0.36036(9) 0.10715(8) 0.72652(8) 0.0183(7) Uij N21 0.43771(9) 0.25925(8) 0.81660(8) 0.0179(7) Uij N31 0.31202(9) 0.21029(8) 0.60463(8) 0.0189(7) Uij C2 0.53588(10) 0.24470(10) 0.64951(10) 0.0192(8) Uij C3 0.47915(10) 0.29022(9) 0.60186(9) 0.0183(8) Uij C12 0.29891(11) 0.06795(10) 0.75584(9) 0.0214(8) Uij C13 0.28816(12) -0.00771(11) 0.74193(10) 0.0253(9) Uij C14 0.34235(12) -0.04381(10) 0.69610(11) 0.0276(10) Uij C15 0.40632(11) -0.00450(10) 0.66709(10) 0.0240(9) Uij C16 0.41373(10) 0.07115(9) 0.68352(9) 0.0188(8) Uij C17 0.48026(11) 0.11727(10) 0.65025(10) 0.0207(8) Uij C22 0.41704(11) 0.31148(10) 0.86663(9) 0.0208(8) Uij C23 0.46973(12) 0.33841(10) 0.91949(10) 0.0234(9) Uij C24 0.54745(12) 0.31050(10) 0.92121(10) 0.0246(9) Uij C25 0.56958(11) 0.25649(10) 0.86998(10) 0.0216(8) Uij C26 0.51346(10) 0.23203(9) 0.81876(9) 0.0177(8) Uij C27 0.53201(10) 0.17160(9) 0.76312(9) 0.0193(8) Uij C32 0.27758(11) 0.14856(10) 0.57601(10) 0.0224(9) Uij C33 0.23759(11) 0.14809(11) 0.50899(10) 0.0249(9) Uij C34 0.23208(11) 0.21393(11) 0.46939(10) 0.0267(9) Uij C35 0.26742(11) 0.27757(10) 0.49771(10) 0.0240(9) Uij C36 0.30643(10) 0.27414(9) 0.56546(9) 0.0186(8) Uij C37 0.34387(10) 0.34262(9) 0.59883(9) 0.0196(8) Uij C41 0.43960(11) 0.38885(9) 0.69089(9) 0.0201(8) Uij C42 0.47144(11) 0.45432(9) 0.64669(9) 0.0199(8) Uij C43 0.55375(11) 0.46189(10) 0.63502(10) 0.0233(9) Uij C44 0.58469(12) 0.52247(11) 0.59597(10) 0.0273(9) Uij C45 0.53277(13) 0.57600(10) 0.56833(10) 0.0271(9) Uij C46 0.45066(12) 0.56872(10) 0.57827(10) 0.0260(9) Uij C47 0.41988(11) 0.50845(10) 0.61795(10) 0.0232(9) Uij Cl1 0.66638(3) 0.03120(2) 0.55187(3) 0.0231(2) Uij O1 0.68366(11) -0.02753(9) 0.60294(9) 0.0446(10) Uij O2 0.66548(10) 0.10095(8) 0.59208(10) 0.0437(9) Uij O3 0.72840(9) 0.03440(8) 0.49602(9) 0.0359(8) Uij O4 0.59005(10) 0.01859(10) 0.51868(9) 0.0481(10) Uij H2a 0.57428 0.22065 0.61876 0.0230 Uiso H2b 0.56280 0.27708 0.68294 0.0230 Uiso H3a 0.50846 0.32953 0.57908 0.0220 Uiso H3b 0.45678 0.25879 0.56489 0.0220 Uiso H12 0.26170 0.09293 0.78708 0.0256 Uiso H13 0.24450 -0.03416 0.76344 0.0304 Uiso H14 0.33551 -0.09524 0.68474 0.0331 Uiso H15 0.44469 -0.02866 0.63641 0.0288 Uiso H17a 0.52895 0.08950 0.65147 0.0248 Uiso H17b 0.46705 0.12889 0.60051 0.0248 Uiso H22 0.36379 0.33074 0.86561 0.0249 Uiso H23 0.45294 0.37532 0.95391 0.0281 Uiso H24 0.58497 0.32799 0.95682 0.0296 Uiso H25 0.62255 0.23655 0.87004 0.0259 Uiso H27a 0.58847 0.16968 0.75513 0.0231 Uiso H27b 0.51402 0.12488 0.78175 0.0231 Uiso H32 0.28092 0.10323 0.60313 0.0269 Uiso H33 0.21434 0.10334 0.49052 0.0299 Uiso H34 0.20445 0.21536 0.42348 0.0320 Uiso H35 0.26509 0.32327 0.47112 0.0288 Uiso H37a 0.36201 0.37451 0.56033 0.0235 Uiso H37b 0.30467 0.36799 0.62762 0.0235 Uiso H41a 0.48102 0.37283 0.72339 0.0242 Uiso H41b 0.39486 0.40585 0.71889 0.0242 Uiso H43 0.58945 0.42515 0.65400 0.0279 Uiso H44 0.64104 0.52698 0.58837 0.0328 Uiso H45 0.55359 0.61791 0.54243 0.0325 Uiso H46 0.41514 0.60490 0.55799 0.0311 Uiso H47 0.36349 0.50422 0.62546 0.0278 Uiso 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 0.0137(1) 0.0177(1) 0.0149(1) 0.0011(1) 0.0013(1) 0.0006(1) Br 0.01491(8) 0.03180(10) 0.02149(9) 0.00341(7) 0.00134(6) -0.00115(7) N1 0.0159(7) 0.0180(7) 0.0157(6) -0.0001(5) 0.0013(5) 0.0022(5) N4 0.0156(7) 0.0181(6) 0.0178(7) 0.0011(5) 0.0005(5) 0.0001(5) N11 0.0179(7) 0.0200(7) 0.0171(7) 0.0008(5) 0.0001(5) 0.0024(5) N21 0.0164(7) 0.0208(7) 0.0164(7) 0.0005(5) 0.0007(5) 0.0019(5) N31 0.0183(7) 0.0205(7) 0.0179(7) 0.0004(5) -0.0004(5) 0.0005(5) C2 0.0151(8) 0.0212(8) 0.0213(8) -0.0007(6) 0.0034(6) 0.0027(6) C3 0.0172(8) 0.0209(8) 0.0169(8) 0.0000(6) 0.0035(6) 0.0013(6) C12 0.0191(8) 0.0265(9) 0.0185(8) -0.0005(7) 0.0001(7) 0.0035(7) C13 0.0242(9) 0.0264(9) 0.0254(9) -0.0068(7) -0.0033(7) 0.0048(7) C14 0.0318(10) 0.0215(9) 0.0295(10) -0.0031(7) -0.0059(8) -0.0005(7) C15 0.0271(10) 0.0222(8) 0.0226(9) 0.0018(7) -0.0004(7) -0.0021(7) C16 0.0189(8) 0.0214(8) 0.0160(7) 0.0013(6) -0.0016(6) 0.0009(6) C17 0.0201(8) 0.0215(8) 0.0204(8) 0.0019(7) 0.0035(7) -0.0016(6) C22 0.0196(8) 0.0240(8) 0.0187(8) 0.0015(7) 0.0026(6) 0.0013(6) C23 0.0289(10) 0.0228(8) 0.0186(8) -0.0005(7) 0.0008(7) -0.0005(7) C24 0.0269(10) 0.0262(9) 0.0208(8) -0.0059(7) -0.0053(7) 0.0021(7) C25 0.0185(8) 0.0226(8) 0.0238(9) -0.0003(7) -0.0026(7) 0.0055(7) C26 0.0170(8) 0.0186(8) 0.0175(7) -0.0012(6) 0.0007(6) 0.0048(6) C27 0.0169(8) 0.0217(8) 0.0191(8) 0.0027(6) -0.0009(6) 0.0029(6) C32 0.0217(9) 0.0223(8) 0.0232(9) 0.0011(7) -0.0014(7) -0.0008(7) C33 0.0195(9) 0.0293(9) 0.0259(9) 0.0027(7) -0.0025(7) -0.0092(7) C34 0.0207(9) 0.0404(11) 0.0189(8) 0.0060(8) -0.0040(7) -0.0033(7) C35 0.0220(9) 0.0299(9) 0.0202(8) 0.0060(7) -0.0013(7) 0.0038(7) C36 0.0155(8) 0.0223(8) 0.0180(8) 0.0032(6) 0.0018(6) 0.0005(6) C37 0.0187(8) 0.0198(8) 0.0202(8) 0.0024(6) 0.0000(6) 0.0038(6) C41 0.0208(9) 0.0199(8) 0.0196(8) -0.0012(6) 0.0010(7) -0.0006(6) C42 0.0227(9) 0.0193(8) 0.0177(8) -0.0027(6) -0.0002(7) -0.0012(6) C43 0.0230(9) 0.0249(9) 0.0219(9) -0.0014(7) -0.0028(7) -0.0007(7) C44 0.0252(10) 0.0337(10) 0.0230(9) -0.0080(8) 0.0037(7) -0.0040(8) C45 0.0405(11) 0.0230(9) 0.0177(8) -0.0088(8) 0.0017(8) -0.0005(7) C46 0.0352(11) 0.0180(8) 0.0247(9) 0.0002(7) -0.0054(8) -0.0018(7) C47 0.0234(9) 0.0207(8) 0.0254(9) -0.0007(7) -0.0006(7) -0.0034(7) Cl1 0.0188(2) 0.0219(2) 0.0286(2) -0.0014(2) 0.0018(2) 0.0012(2) O1 0.0608(11) 0.0399(9) 0.0332(8) 0.0019(8) -0.0058(8) 0.0100(7) O2 0.0413(9) 0.0293(8) 0.0605(11) -0.0067(7) 0.0227(8) -0.0131(7) O3 0.0336(8) 0.0339(8) 0.0402(8) -0.0006(6) 0.0155(7) -0.0030(6) O4 0.0286(8) 0.0695(11) 0.0462(10) -0.0124(8) -0.0106(7) 0.0055(9) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe N1 2.223(1) yes Fe N4 2.265(1) yes Fe N11 2.166(1) yes Fe N21 2.206(1) yes Fe N31 2.271(1) yes Fe Br 2.4801(3) yes N1 C17 1.474(2) no N1 C27 1.482(2) no N1 C2 1.487(2) no N4 C37 1.481(2) no N4 C3 1.485(2) no N4 C41 1.497(2) no N11 C16 1.345(2) no N11 C12 1.348(2) no N21 C22 1.346(2) no N21 C26 1.351(2) no N31 C32 1.348(2) no N31 C36 1.348(2) no C2 C3 1.516(2) no C12 C13 1.389(2) no C13 C14 1.385(3) no C14 C15 1.379(3) no C15 C16 1.392(2) no C16 C17 1.506(2) no C22 C23 1.384(2) no C23 C24 1.385(3) no C24 C25 1.389(3) no C25 C26 1.386(2) no C26 C27 1.510(2) no C32 C33 1.384(2) no C33 C34 1.382(3) no C34 C35 1.380(3) no C35 C36 1.389(2) no C36 C37 1.502(2) no C41 C42 1.514(2) no C42 C43 1.391(2) no C42 C47 1.394(2) no C43 C44 1.393(2) no C44 C45 1.383(3) no C45 C46 1.383(3) no C46 C47 1.393(2) no Cl1 O1 1.429(2) no Cl1 O2 1.445(2) no Cl1 O3 1.445(1) no Cl1 O4 1.422(2) no C2 H2a 0.950 no C2 H2b 0.950 no C3 H3a 0.950 no C3 H3b 0.950 no C12 H12 0.950 no C13 H13 0.950 no C14 H14 0.950 no C15 H15 0.950 no C17 H17a 0.950 no C17 H17b 0.950 no C22 H22 0.950 no C23 H23 0.950 no C24 H24 0.950 no C25 H25 0.950 no C27 H27a 0.950 no C27 H27b 0.950 no C32 H32 0.950 no C33 H33 0.950 no C34 H34 0.950 no C35 H35 0.950 no C37 H37a 0.950 no C37 H37b 0.950 no C41 H41a 0.950 no C41 H41b 0.950 no C43 H43 0.950 no C44 H44 0.950 no C45 H45 0.950 no C46 H46 0.950 no C47 H47 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Br Fe N1 171.38(4) yes Br Fe N4 102.42(4) yes Br Fe N11 106.54(4) yes Br Fe N21 94.89(4) yes Br Fe N31 90.48(4) yes N1 Fe N4 79.53(5) yes N1 Fe N11 75.09(5) yes N1 Fe N21 76.53(5) yes N1 Fe N31 98.11(5) yes N4 Fe N11 143.87(5) yes N4 Fe N21 95.39(5) yes N4 Fe N31 73.92(5) yes N11 Fe N21 103.09(5) yes N11 Fe N31 84.60(5) yes N21 Fe N31 168.89(5) yes Fe N1 C2 110.3(1) yes Fe N1 C17 105.8(1) yes Fe N1 C27 107.7(1) yes Fe N4 C3 105.2(1) yes Fe N4 C37 104.8(1) yes Fe N4 C41 112.7(1) yes Fe N11 C12 126.1(1) yes Fe N11 C16 113.5(1) yes Fe N21 C22 126.0(1) yes Fe N21 C26 115.0(1) yes Fe N31 C32 129.2(1) yes Fe N31 C36 112.8(1) yes C17 N1 C27 110.0(1) no C2 N1 C17 112.4(1) no C2 N1 C27 110.5(1) no C3 N4 C37 110.5(1) no C37 N4 C41 110.6(1) no C3 N4 C41 112.5(1) no C12 N11 C16 118.6(1) no C22 N21 C26 118.0(1) no C32 N31 C36 117.6(1) no N1 C2 C3 110.8(1) no N4 C3 C2 111.2(1) no N11 C12 C13 122.2(2) no C12 C13 C14 118.7(2) no C13 C14 C15 119.5(2) no C14 C15 C16 118.9(2) no N11 C16 C15 122.1(2) no N11 C16 C17 117.0(1) no C15 C16 C17 120.9(2) no N1 C17 C16 110.4(1) no N21 C22 C23 123.1(2) no C22 C23 C24 118.7(2) no C23 C24 C25 118.9(2) no C24 C25 C26 119.2(2) no N21 C26 C25 122.2(2) no N21 C26 C27 115.4(1) no C25 C26 C27 122.4(2) no N1 C27 C26 110.5(1) no N31 C32 C33 123.1(2) no C32 C33 C34 118.8(2) no C33 C34 C35 118.8(2) no C34 C35 C36 119.4(2) no N31 C36 C35 122.3(2) no N31 C36 C37 116.9(1) no C35 C36 C37 120.8(2) no N4 C37 C36 111.1(1) no N4 C41 C42 115.6(1) no C43 C42 C47 118.7(2) no C41 C42 C43 120.0(2) no C41 C42 C47 121.3(2) no C42 C43 C44 121.1(2) no C43 C44 C45 119.5(2) no C44 C45 C46 120.2(2) no C45 C46 C47 120.2(2) no C42 C47 C46 120.3(2) no O1 Cl1 O2 108.1(1) no O1 Cl1 O3 109.8(1) no O1 Cl1 O4 109.6(1) no O2 Cl1 O3 109.0(1) no O2 Cl1 O4 109.9(1) no O3 Cl1 O4 110.3(1) no H2a C2 H2b 109.5 no N1 C2 H2a 109.1 no C3 C2 H2a 109.1 no N1 C2 H2b 109.1 no C3 C2 H2b 109.1 no H3a C3 H3b 109.5 no N4 C3 H3a 109.0 no C2 C3 H3a 109.0 no N4 C3 H3b 109.0 no C2 C3 H3b 109.0 no N11 C12 H12 118.9 no C13 C12 H12 118.9 no C14 C13 H13 120.7 no C12 C13 H13 120.7 no C15 C14 H14 120.3 no C13 C14 H14 120.3 no C14 C15 H15 120.6 no C16 C15 H15 120.6 no H17a C17 H17b 109.5 no N1 C17 H17a 109.2 no C16 C17 H17a 109.2 no N1 C17 H17b 109.2 no C16 C17 H17b 109.2 no N21 C22 H22 118.5 no C23 C22 H22 118.5 no C22 C23 H23 120.7 no C24 C23 H23 120.7 no C23 C24 H24 120.6 no C25 C24 H24 120.6 no C26 C25 H25 120.4 no C24 C25 H25 120.4 no H27a C27 H27b 109.5 no N1 C27 H27a 109.2 no C26 C27 H27a 109.2 no N1 C27 H27b 109.2 no C26 C27 H27b 109.2 no N31 C32 H32 118.5 no C33 C32 H32 118.5 no C34 C33 H33 120.6 no C32 C33 H33 120.6 no C35 C34 H34 120.6 no C33 C34 H34 120.6 no C34 C35 H35 120.3 no C36 C35 H35 120.3 no H37a C37 H37b 109.5 no N4 C37 H37a 109.1 no C36 C37 H37a 109.1 no N4 C37 H37b 109.1 no C36 C37 H37b 109.1 no H41a C41 H41b 109.5 no N4 C41 H41a 107.9 no C42 C41 H41a 107.9 no N4 C41 H41b 107.9 no C42 C41 H41b 107.9 no C42 C43 H43 119.5 no C44 C43 H43 119.5 no C45 C44 H44 120.2 no C43 C44 H44 120.2 no C46 C45 H45 119.9 no C44 C45 H45 119.9 no C45 C46 H46 119.9 no C47 C46 H46 119.9 no C46 C47 H47 119.8 no C42 C47 H47 119.8 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag Fe N1 C2 C3 -31.0(2) no N1 C2 C3 N4 54.0(2) no C2 C3 N4 Fe -46.7(1) no C3 N4 Fe N1 22.3(1) no C3 C2 N1 C17 86.9(2) no C3 C2 N1 C27 -149.9(1) no C2 C3 N4 C37 -159.4(1) no C2 C3 N4 C41 76.4(2) no data_Fetpenbz _database_code_CSD 163871 #============================================================================== #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [FetpenbzCl](PF6).0.192CH2Cl2 ; _chemical_name_common '[FetpenbzCl](PF6).0.192CH2Cl2' _chemical_formula_sum 'C27.192 H29.384 Cl1.384 F6 Fe1 N5 P 1' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_weight 676.16 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R-3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-y,+x-y,+z' '-x+y,-x,+z' '-x,-y,-z' '+y,-x+y,-z' '+x-y,+x,-z' '2/3+x,1/3+y,1/3+z' '2/3-y,1/3+x-y,1/3+z' '2/3-x+y,1/3-x,1/3+z' '2/3-x,1/3-y,1/3-z' '2/3+y,1/3-x+y,1/3-z' '2/3+x-y,1/3+x,1/3-z' '1/3+x,2/3+y,2/3+z' '1/3-y,2/3+x-y,2/3+z' '1/3-x+y,2/3-x,2/3+z' '1/3-x,2/3-y,2/3-z' '1/3+y,2/3-x+y,2/3-z' '1/3+x-y,2/3+x,2/3-z' _cell_length_a 29.1500(9) _cell_length_b 29.1500(9) _cell_length_c 17.661(1) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 12996(1) _cell_formula_units_Z 18 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 29.84 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6189.984 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP (Siemens, 1955)' _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.886 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 42461 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.4 _diffrn_reflns_theta_max 29.84 _diffrn_reflns_reduction_process 42461 _reflns_number_total 7899 _reflns_number_gt 6585 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix The extinction parameter was less than one sigma and has been set to zero Hydrogen atoms of ligand constrained to have C-H = 0.95\%A and Uiso 20% larger than Ueq of the atom to which it is attached. Hydrogen atoms of solvent molecules were neither located nor included in the calculations. The site occupation factors for the atoms of the solvent molecule were constrained to be identical, the central C atom was only refined isotropically becaususe of its closeness to the 3-fold axis. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1 /{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^-|F|}^2^ A = 0.03, B = 7.0 ; _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6787 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_number_constraints 6 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.037 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_shift/su_max 0.0012 _refine_ls_shift/su_mean 0.0005 _refine_diff_density_max 1.1(1) _refine_diff_density_min -1.1(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_occupancy Fe 0.44834(1) 0.04930(1) 0.71495(2) 0.0159(2) Uij 1.0 Cl 0.40297(2) 0.05459(2) 0.61010(3) 0.0228(4) Uij 1.0 N1 0.47818(7) 0.04428(7) 0.8303(1) 0.018(1) Uij 1.0 C2 0.45705(9) -0.01228(9) 0.8504(1) 0.021(1) Uij 1.0 C3 0.45129(9) -0.04543(9) 0.7809(1) 0.020(1) Uij 1.0 N4 0.41925(7) -0.03816(7) 0.7213(1) 0.017(1) Uij 1.0 N11 0.51630(7) 0.12723(7) 0.7373(1) 0.019(1) Uij 1.0 C12 0.52880(9) 0.17200(9) 0.6994(1) 0.023(2) Uij 1.0 C13 0.57765(10) 0.21772(9) 0.7065(1) 0.028(2) Uij 1.0 C14 0.61486(10) 0.21715(10) 0.7544(1) 0.030(2) Uij 1.0 C15 0.60223(9) 0.17150(10) 0.7944(1) 0.026(2) Uij 1.0 C16 0.55269(9) 0.12700(9) 0.7845(1) 0.020(1) Uij 1.0 C17 0.53642(9) 0.07495(9) 0.8240(1) 0.021(1) Uij 1.0 N21 0.39231(7) 0.05454(7) 0.7954(1) 0.020(1) Uij 1.0 C22 0.34507(9) 0.04985(9) 0.7775(1) 0.023(1) Uij 1.0 C23 0.31246(9) 0.05441(9) 0.8300(1) 0.024(1) Uij 1.0 C24 0.32905(9) 0.06425(9) 0.9050(1) 0.024(1) Uij 1.0 C25 0.37705(9) 0.06881(9) 0.9243(1) 0.021(1) Uij 1.0 C26 0.40748(9) 0.06335(8) 0.8683(1) 0.019(1) Uij 1.0 C27 0.46080(9) 0.07000(9) 0.8868(1) 0.021(1) Uij 1.0 N31 0.50567(7) 0.03695(7) 0.6421(1) 0.019(1) Uij 1.0 C32 0.55313(9) 0.07298(9) 0.6144(1) 0.021(1) Uij 1.0 C33 0.58270(9) 0.06021(10) 0.5664(1) 0.024(2) Uij 1.0 C34 0.56306(9) 0.00776(10) 0.5467(1) 0.023(2) Uij 1.0 C35 0.51372(9) -0.02996(9) 0.5739(1) 0.021(1) Uij 1.0 C36 0.48611(8) -0.01393(9) 0.6207(1) 0.019(1) Uij 1.0 C37 0.43088(9) -0.05301(9) 0.6467(1) 0.019(1) Uij 1.0 C41 0.36102(8) -0.06951(9) 0.7368(1) 0.020(1) Uij 1.0 C42 0.33573(8) -0.12942(9) 0.7337(1) 0.021(1) Uij 1.0 C43 0.31671(9) -0.15718(9) 0.6658(1) 0.024(2) Uij 1.0 C44 0.29149(9) -0.21219(10) 0.6640(2) 0.030(2) Uij 1.0 C45 0.28489(11) -0.24009(10) 0.7306(2) 0.039(2) Uij 1.0 C46 0.30372(11) -0.21310(10) 0.7981(2) 0.039(2) Uij 1.0 C47 0.32904(10) -0.15798(10) 0.7998(1) 0.028(2) Uij 1.0 Cl2 0.0000 0.0000 0.0702(5) 0.171(5) Uij 0.192(2) Cl3 0.0035(3) -0.0206(2) 0.2267(7) 0.179(9) Uij 0.192 C1 -0.0078(13) 0.0204(11) 0.1723(14) 0.086(7) Uiso 0.192 P1 0.45771(2) -0.15796(3) 0.93817(4) 0.0243(4) Uij 1.0 F1 0.46121(16) -0.10326(11) 0.94813(13) 0.129(4) Uij 1.0 F2 0.43763(7) -0.17071(7) 1.02336(9) 0.054(1) Uij 1.0 F3 0.45732(15) -0.21097(9) 0.92855(13) 0.115(3) Uij 1.0 F4 0.47884(8) -0.14373(8) 0.85338(10) 0.061(2) Uij 1.0 F5 0.51582(8) -0.13243(13) 0.96860(13) 0.114(3) Uij 1.0 F6 0.40050(8) -0.18286(15) 0.90853(13) 0.126(3) Uij 1.0 H2a 0.42331 -0.02556 0.8735 0.025 Uiso 1.0 H2b 0.48062 -0.01481 0.8850 0.025 Uiso 1.0 H3a 0.43425 -0.08173 0.7949 0.024 Uiso 1.0 H3b 0.48547 -0.03497 0.7612 0.024 Uiso 1.0 H12 0.50317 0.17230 0.6665 0.027 Uiso 1.0 H13 0.58540 0.24878 0.6790 0.033 Uiso 1.0 H14 0.64878 0.24782 0.7599 0.036 Uiso 1.0 H15 0.62715 0.17063 0.8282 0.031 Uiso 1.0 H17a 0.54841 0.05534 0.7954 0.025 Uiso 1.0 H17b 0.55167 0.08167 0.8731 0.025 Uiso 1.0 H22 0.33371 0.04306 0.7263 0.028 Uiso 1.0 H23 0.27953 0.05092 0.8152 0.029 Uiso 1.0 H24 0.30764 0.06779 0.9424 0.028 Uiso 1.0 H25 0.38913 0.07561 0.9752 0.026 Uiso 1.0 H27a 0.48609 0.10675 0.8884 0.025 Uiso 1.0 H27b 0.45893 0.05472 0.9351 0.025 Uiso 1.0 H32 0.56714 0.10902 0.6284 0.026 Uiso 1.0 H33 0.61587 0.08702 0.5474 0.029 Uiso 1.0 H34 0.58296 -0.00228 0.5152 0.028 Uiso 1.0 H35 0.49908 -0.06621 0.5607 0.025 Uiso 1.0 H37a 0.40620 -0.05400 0.6107 0.023 Uiso 1.0 H37b 0.42749 -0.08708 0.6504 0.023 Uiso 1.0 H41a 0.34368 -0.05942 0.7005 0.024 Uiso 1.0 H41b 0.35517 -0.06035 0.7860 0.024 Uiso 1.0 H43 0.32106 -0.13818 0.6201 0.028 Uiso 1.0 H44 0.27884 -0.23059 0.6174 0.036 Uiso 1.0 H45 0.26746 -0.27769 0.7298 0.047 Uiso 1.0 H46 0.29938 -0.23224 0.8436 0.047 Uiso 1.0 H47 0.34182 -0.13978 0.8465 0.033 Uiso 1.0 H1a -0.04252 0.01479 0.1802 0.103 Uiso 0.192 H1b 0.01742 0.05645 0.1821 0.103 Uiso 0.192 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 0.0171(2) 0.0204(2) 0.0126(1) 0.0110(1) -0.0022(1) -0.0014(1) Cl 0.0245(3) 0.0330(3) 0.0147(2) 0.0173(2) -0.0034(2) 0.0012(2) N1 0.018(1) 0.022(1) 0.016(1) 0.012(1) -0.001(1) 0.000(1) C2 0.022(1) 0.027(1) 0.017(1) 0.014(1) -0.002(1) 0.003(1) C3 0.020(1) 0.023(1) 0.020(1) 0.013(1) -0.001(1) 0.003(1) N4 0.017(1) 0.020(1) 0.014(1) 0.010(1) 0.000(1) 0.000(1) N11 0.022(1) 0.024(1) 0.016(1) 0.014(1) -0.002(1) -0.003(1) C12 0.029(1) 0.026(1) 0.018(1) 0.017(1) -0.001(1) -0.003(1) C13 0.031(1) 0.024(1) 0.026(1) 0.012(1) 0.005(1) 0.002(1) C14 0.022(1) 0.029(1) 0.033(1) 0.008(1) 0.002(1) -0.004(1) C15 0.020(1) 0.032(1) 0.025(1) 0.013(1) -0.003(1) -0.005(1) C16 0.021(1) 0.026(1) 0.016(1) 0.015(1) 0.001(1) -0.003(1) C17 0.019(1) 0.028(1) 0.019(1) 0.014(1) -0.004(1) -0.002(1) N21 0.021(1) 0.023(1) 0.019(1) 0.012(1) -0.002(1) -0.003(1) C22 0.022(1) 0.024(1) 0.025(1) 0.013(1) -0.005(1) -0.005(1) C23 0.020(1) 0.020(1) 0.035(1) 0.011(1) 0.001(1) 0.000(1) C24 0.027(1) 0.017(1) 0.029(1) 0.013(1) 0.010(1) 0.004(1) C25 0.029(1) 0.018(1) 0.019(1) 0.013(1) 0.005(1) 0.002(1) C26 0.021(1) 0.017(1) 0.018(1) 0.010(1) 0.001(1) 0.001(1) C27 0.026(1) 0.027(1) 0.014(1) 0.016(1) -0.001(1) -0.003(1) N31 0.019(1) 0.023(1) 0.016(1) 0.011(1) -0.001(1) -0.001(1) C32 0.019(1) 0.024(1) 0.018(1) 0.009(1) -0.001(1) -0.003(1) C33 0.018(1) 0.034(1) 0.017(1) 0.011(1) 0.000(1) -0.001(1) C34 0.023(1) 0.039(1) 0.015(1) 0.021(1) -0.001(1) -0.002(1) C35 0.026(1) 0.027(1) 0.015(1) 0.017(1) -0.002(1) -0.001(1) C36 0.020(1) 0.023(1) 0.014(1) 0.012(1) -0.002(1) 0.001(1) C37 0.021(1) 0.021(1) 0.017(1) 0.011(1) 0.000(1) -0.002(1) C41 0.019(1) 0.025(1) 0.017(1) 0.012(1) 0.001(1) 0.000(1) C42 0.016(1) 0.024(1) 0.023(1) 0.010(1) -0.001(1) -0.001(1) C43 0.020(1) 0.028(1) 0.023(1) 0.012(1) -0.001(1) -0.001(1) C44 0.023(1) 0.029(1) 0.038(1) 0.012(1) -0.007(1) -0.009(1) C45 0.032(1) 0.022(1) 0.055(2) 0.008(1) -0.010(1) 0.000(1) C46 0.039(2) 0.027(1) 0.041(2) 0.009(1) -0.009(1) 0.009(1) C47 0.026(1) 0.028(1) 0.025(1) 0.010(1) -0.004(1) 0.002(1) Cl2 0.134(3) 0.134 0.245(8) 0.067 0.000 0.000 Cl3 0.039(3) 0.072(5) 0.393(14) 0.003(3) -0.051(7) 0.127(6) P1 0.0214(3) 0.0292(3) 0.0220(3) 0.0123(3) 0.0005(2) 0.0053(2) F1 0.302(4) 0.094(2) 0.0526(14) 0.146(3) 0.025(2) 0.0213(13) F2 0.043(1) 0.067(1) 0.0253(8) 0.0082(9) 0.0049(7) 0.0108(8) F3 0.261(4) 0.072(2) 0.0484(13) 0.110(2) -0.033(2) -0.0134(11) F4 0.063(1) 0.065(1) 0.0269(9) 0.0098(10) 0.0160(8) 0.0006(8) F5 0.033(1) 0.228(3) 0.0639(14) 0.053(2) -0.0178(10) -0.0898(18) F6 0.037(1) 0.279(4) 0.0454(13) 0.065(2) -0.0151(10) -0.0211(18) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe Cl 2.325(1) yes Fe N1 2.248(2) yes Fe N4 2.251(2) yes Fe N11 2.177(2) yes Fe N21 2.227(2) yes Fe N31 2.276(2) yes N1 C17 1.475(3) no N1 C27 1.482(3) no N1 C2 1.486(3) no C2 C3 1.519(3) no C3 N4 1.491(3) no N4 C37 1.478(3) no N4 C41 1.497(3) no N11 C12 1.345(3) no N11 C16 1.352(3) no C12 C13 1.386(3) no C13 C14 1.383(4) no C14 C15 1.384(4) no C15 C16 1.387(3) no C16 C17 1.514(3) no N21 C26 1.345(3) no N21 C22 1.351(3) no C22 C23 1.380(3) no C23 C24 1.390(3) no C24 C25 1.380(3) no C25 C26 1.389(3) no C26 C27 1.503(3) no N31 C32 1.343(3) no N31 C36 1.350(3) no C32 C33 1.386(3) no C33 C34 1.383(3) no C34 C35 1.388(3) no C35 C36 1.387(3) no C36 C37 1.506(3) no C41 C42 1.519(3) no C42 C47 1.390(3) no C42 C43 1.397(3) no C43 C44 1.391(3) no C44 C45 1.387(4) no C45 C46 1.383(4) no C46 C47 1.393(4) no P1 F1 1.556(2) no P1 F2 1.590(2) no P1 F3 1.549(2) no P1 F4 1.593(2) no P1 F5 1.566(2) no P1 F6 1.540(2) no Cl3 C1 1.69(2 no Cl2 C1 1.95(2) no C2 H2a 0.950 no C2 H2b 0.950 no C3 H3a 0.950 no C3 H3b 0.950 no C12 H12 0.950 no C13 H13 0.950 no C14 H14 0.950 no C15 H15 0.950 no C17 H17a 0.950 no C17 H17b 0.950 no C22 H22 0.950 no C23 H23 0.950 no C24 H24 0.950 no C25 H25 0.950 no C27 H27a 0.950 no C27 H27b 0.950 no C32 H32 0.950 no C33 H33 0.950 no C34 H34 0.950 no C35 H35 0.950 no C37 H37a 0.950 no C37 H37b 0.950 no C41 H41a 0.950 no C41 H41b 0.950 no C43 H43 0.950 no C44 H44 0.950 no C45 H45 0.950 no C46 H46 0.950 no C47 H47 0.950 no C1 H1a 0.950 no C1 H1b 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl Fe N1 167.77(5) no Cl Fe N4 102.13(5) no Cl Fe N11 109.04(5) no Cl Fe N21 92.42(5) no Cl Fe N31 92.72(5) no N1 Fe N4 79.63(6) no N1 Fe N11 73.97(7) no N1 Fe N21 75.38(6) no N1 Fe N31 99.40(6) no N4 Fe N11 143.46(6) no N4 Fe N21 99.90(7) no N4 Fe N31 74.91(6) no N11 Fe N21 97.39(7) no N11 Fe N31 84.87(6) no N21 Fe N31 173.37(7) no Fe N1 C2 109.2(1) no Fe N1 C17 104.9(1) no Fe N1 C27 109.6(1) no Fe N4 C3 106.7(1) no Fe N4 C37 106.0(1) no Fe N4 C41 111.8(1) no Fe N11 C12 125.9(1) no Fe N11 C16 114.4(1) no Fe N21 C22 126.2(1) no Fe N21 C26 116.2(1) no Fe N31 C32 129.3(1) no Fe N31 C36 113.1(1) no C17 N1 C27 109.0(2) no C2 N1 C17 113.8(2) no C2 N1 C27 110.1(2) no N1 C2 C3 111.4(2) no C2 C3 N4 111.0(2) no C3 N4 C37 109.6(2) no C37 N4 C41 109.9(2) no C3 N4 C41 112.6(2) no C12 N11 C16 118.6(2) no N11 C12 C13 122.5(2) no C12 C13 C14 118.6(2) no C13 C14 C15 119.4(2) no C14 C15 C16 119.1(2) no N11 C16 C15 121.7(2) no N11 C16 C17 115.8(2) no C15 C16 C17 122.5(2) no N1 C17 C16 109.3(2) no C22 N21 C26 117.6(2) no N21 C22 C23 123.4(2) no C22 C23 C24 118.3(2) no C23 C24 C25 119.1(2) no C24 C25 C26 119.2(2) no N21 C26 C25 122.4(2) no N21 C26 C27 116.9(2) no C25 C26 C27 120.6(2) no N1 C27 C26 112.4(2) no C32 N31 C36 117.4(2) no N31 C32 C33 123.3(2) no C32 C33 C34 118.8(2) no C33 C34 C35 118.8(2) no C34 C35 C36 119.0(2) no N31 C36 C35 122.7(2) no N31 C36 C37 116.7(2) no C35 C36 C37 120.5(2) no N4 C37 C36 111.5(2) no N4 C41 C42 116.5(2) no C43 C42 C47 118.6(2) no C41 C42 C47 120.0(2) no C41 C42 C43 121.4(2) no C42 C43 C44 121.0(2) no C43 C44 C45 119.7(2) no C44 C45 C46 119.9(2) no C45 C46 C47 120.4(2) no C42 C47 C46 120.5(2) no F1 P1 F2 87.7(1) no F1 P1 F3 177.1(2) no F1 P1 F4 91.2(1) no F1 P1 F5 88.5(2) no F1 P1 F6 91.3(2) no F2 P1 F3 93.0(1) no F2 P1 F4 178.6(1) no F2 P1 F5 88.3(1) no F2 P1 F6 91.5(1) no F3 P1 F4 88.0(1) no F3 P1 F5 88.8(2) no F3 P1 F6 91.5(2) no F5 P1 F6 179.7(3) no F4 P1 F5 90.8(1) no F4 P1 F6 89.4(1) no Cl2 C1 Cl3 103(1) no H2a C2 H2b 109.5 no N1 C2 H2a 109.0 no C3 C2 H2a 109.0 no N1 C2 H2b 109.0 no C3 C2 H2b 109.0 no H3a C3 H3b 109.5 no N4 C3 H3a 109.1 no C2 C3 H3a 109.1 no N4 C3 H3b 109.1 no C2 C3 H3b 109.1 no N11 C12 H12 118.7 no C13 C12 H12 118.7 no C14 C13 H13 120.7 no C12 C13 H13 120.7 no C13 C14 H14 120.3 no C15 C14 H14 120.3 no C14 C15 H15 120.4 no C16 C15 H15 120.4 no H17a C17 H17b 109.5 no N1 C17 H17a 109.5 no C16 C17 H17a 109.5 no N1 C17 H17b 109.5 no C16 C17 H17b 109.5 no N21 C22 H22 118.3 no C23 C22 H22 118.3 no C22 C23 H23 120.9 no C24 C23 H23 120.9 no C25 C24 H24 120.4 no C23 C24 H24 120.4 no C24 C25 H25 120.4 no C26 C25 H25 120.4 no H27a C27 H27b 109.5 no N1 C27 H27a 108.7 no C26 C27 H27a 108.7 no N1 C27 H27b 108.7 no C26 C27 H27b 108.7 no N31 C32 H32 118.4 no C33 C32 H32 118.4 no C34 C33 H33 120.6 no C32 C33 H33 120.6 no C33 C34 H34 120.6 no C35 C34 H34 120.6 no C36 C35 H35 120.5 no C34 C35 H35 120.5 no H37a C37 H37b 109.5 no N4 C37 H37a 109.0 no C36 C37 H37a 109.0 no N4 C37 H37b 109.0 no C36 C37 H37b 109.0 no H41a C41 H41b 109.5 no N4 C41 H41a 107.7 no C42 C41 H41a 107.7 no N4 C41 H41b 107.7 no C42 C41 H41b 107.7 no C44 C43 H43 119.5 no C42 C43 H43 119.5 no C45 C44 H44 120.2 no C43 C44 H44 120.2 no C46 C45 H45 120.0 no C44 C45 H45 120.0 no C45 C46 H46 119.8 no C47 C46 H46 119.8 no C42 C47 H47 119.7 no C46 C47 H47 119.8 no H1a C1 H1b 109.5 no 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 Fe N1 C2 C3 33.3(2) N1 C2 C3 N4 -53.6(2) C2 C3 N4 Fe 44.1(2) C3 N4 Fe N1 -19.6(1) C3 C2 N1 C17 -83.6(2) C3 C2 N1 C27 153.8(2) C2 C3 N4 C37 158.5(2) C2 C3 N4 C41 -78.9(2) data_Fetpenol _database_code_CSD 163872 #============================================================================== #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [Fetpenol](PF6) ; _chemical_name_common '[Fetpenol](PF6)' _chemical_formula_sum 'C22 H27 Cl1 F6 Fe N5 O P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C22 H27 Cl Fe N5 O, F6 P' _chemical_formula_weight 613.78 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Fdd2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,+z' '1/4+x,1/4-y,1/4+z' '1/4-x,1/4+y,1/4+z' '+x,1/2+y,1/2+z' '-x,1/2-y,1/2+z' '1/4+x,3/4-y,3/4+z' '1/4-x,3/4+y,3/4+z' '1/2+x,+y,1/2+z' '1/2-x,-y,1/2+z' '3/4+x,1/4-y,3/4+z' '3/4-x,1/4+y,3/4+z' '1/2+x,1/2+y,+z' '1/2-x,1/2-y,+z' '3/4+x,3/4-y,1/4+z' '3/4-x,3/4+y,1/4+z' _cell_length_a 21.345(1) _cell_length_b 53.473(3) _cell_length_c 9.0756(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 10359(1) _cell_formula_units_Z 16 _cell_measurement_temperature 120 _cell_measurement_reflns_used 6648 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.6 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5024 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP, Siemens 1995' _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.911 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 16435 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 28.6 _diffrn_reflns_reduction_process 16435 _reflns_number_total 5618 _reflns_number_gt 5399 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix hydrogen atoms fixed with C-H = 0.95\%A except for the hydroxyl hydrogen which was refined isotropically ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^-|F|}^2^ A = 0.03, B = 0.2 ; _refine_ls_hydrogen_treatment mixed _refine_ls_abs_structure_details ; refine Rogers factor ; _refine_ls_abs_structure_Rogers 0.88(2) _refine_ls_number_reflns 5399 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.027 _refine_ls_wR_factor_reF 0.037 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_shift/su_max 0.0028 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_max 0.60(8) _refine_diff_density_min -0.48(8) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type Fe Fe 0.61819(1) 0.538743(5) 0.11950 0.0133(1) Uij Cl Cl 0.60643(3) 0.508663(10) 0.30827(6) 0.0190(2) Uij N1 N 0.61183(8) 0.56129(3) -0.0902(2) 0.016(1) Uij C2 C 0.67570(10) 0.56644(4) -0.1475(2) 0.018(1) Uij C3 C 0.72178(10) 0.56894(4) -0.0211(2) 0.017(1) Uij N4 N 0.72114(8) 0.54673(3) 0.0775(2) 0.014(1) Uij N11 N 0.52544(8) 0.55554(3) 0.1198(2) 0.018(1) Uij C12 C 0.47644(10) 0.54817(4) 0.2018(3) 0.021(1) Uij C13 C 0.42174(11) 0.56177(5) 0.2127(3) 0.026(1) Uij C14 C 0.41725(11) 0.58407(5) 0.1345(3) 0.029(1) Uij C15 C 0.46726(11) 0.59171(4) 0.0468(3) 0.025(1) Uij C16 C 0.52055(10) 0.57702(4) 0.0427(3) 0.019(1) Uij C17 C 0.57715(10) 0.58423(4) -0.0479(3) 0.019(1) Uij N21 N 0.60509(8) 0.51066(3) -0.0567(2) 0.016(1) Uij C22 C 0.61172(10) 0.48570(4) -0.0420(3) 0.018(1) Uij C23 C 0.60074(10) 0.46902(4) -0.1555(3) 0.021(1) Uij C24 C 0.58329(10) 0.47822(4) -0.2923(3) 0.021(1) Uij C25 C 0.57704(10) 0.50410(4) -0.3095(2) 0.018(1) Uij C26 C 0.58758(9) 0.51942(4) -0.1894(2) 0.015(1) Uij C27 C 0.57505(10) 0.54711(4) -0.2000(2) 0.018(1) Uij N31 N 0.64491(8) 0.56836(3) 0.2829(2) 0.017(1) Uij C32 C 0.60549(9) 0.58192(4) 0.3670(3) 0.021(1) Uij C33 C 0.62574(11) 0.59851(4) 0.4736(3) 0.022(1) Uij C34 C 0.68945(11) 0.60172(4) 0.4935(3) 0.023(1) Uij C35 C 0.73060(10) 0.58782(4) 0.4088(2) 0.020(1) Uij C36 C 0.70697(10) 0.57108(4) 0.3065(2) 0.016(1) Uij C37 C 0.74947(10) 0.55399(4) 0.2199(2) 0.018(1) Uij C41 C 0.75755(10) 0.52599(4) 0.0092(2) 0.018(1) Uij C42 C 0.75953(9) 0.50247(4) 0.1032(3) 0.018(1) Uij O1 O 0.77474(8) 0.48100(3) 0.0180(2) 0.025(1) Uij P1 P 0.66902(2) 0.650559(9) -0.13990(7) 0.0168(3) Uij F1 F 0.70362(7) 0.62684(3) -0.0702(2) 0.040(1) Uij F2 F 0.62408(7) 0.63254(3) -0.2315(2) 0.039(1) Uij F3 F 0.62029(7) 0.65036(3) -0.0055(2) 0.039(1) Uij F4 F 0.63386(7) 0.67437(3) -0.2082(2) 0.030(1) Uij F5 F 0.71413(7) 0.66876(3) -0.0495(2) 0.036(1) Uij F6 F 0.71757(7) 0.65081(3) -0.2742(2) 0.033(1) Uij HO H 0.807(1) 0.4819(5) -0.023(4) 0.030(8) Uiso H2a H 0.67513 0.58156 -0.2024 0.022 Uiso H2b H 0.68840 0.55306 -0.2095 0.022 Uiso H3a H 0.71114 0.58333 0.0350 0.021 Uiso H3b H 0.76273 0.57088 -0.0605 0.021 Uiso H12 H 0.47959 0.53289 0.2547 0.026 Uiso H13 H 0.38800 0.55607 0.2721 0.031 Uiso H14 H 0.38042 0.59398 0.1408 0.035 Uiso H15 H 0.46482 0.60672 -0.0089 0.030 Uiso H17a H 0.56396 0.59282 -0.1341 0.023 Uiso H17b H 0.60366 0.59481 0.0086 0.023 Uiso H22 H 0.62457 0.47928 0.0508 0.022 Uiso H23 H 0.60508 0.45153 -0.1399 0.025 Uiso H24 H 0.57575 0.46720 -0.3725 0.026 Uiso H25 H 0.56575 0.51103 -0.4022 0.022 Uiso H27a H 0.58601 0.55272 -0.2959 0.022 Uiso H27b H 0.53173 0.55004 -0.1833 0.022 Uiso H32 H 0.56169 0.57998 0.3523 0.025 Uiso H33 H 0.59649 0.60752 0.5320 0.027 Uiso H34 H 0.70474 0.61330 0.5643 0.028 Uiso H35 H 0.77455 0.58974 0.4207 0.024 Uiso H37a H 0.78791 0.56239 0.2016 0.022 Uiso H37b H 0.75723 0.53934 0.2762 0.022 Uiso H41a H 0.79928 0.53157 -0.0063 0.022 Uiso H41b H 0.73893 0.52195 -0.0829 0.022 Uiso H42a H 0.71963 0.50005 0.1474 0.022 Uiso H42b H 0.79025 0.50452 0.1780 0.022 Uiso 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 0.0156(1) 0.0123(1) 0.0121(1) -0.0015(1) -0.0002(1) 0.0004(1) Cl 0.0243(2) 0.0191(3) 0.0135(2) -0.0028(2) -0.0007(2) 0.0036(2) N1 0.018(1) 0.012(1) 0.017(1) 0.000(1) -0.001(1) 0.000(1) C2 0.022(1) 0.018(1) 0.015(1) -0.002(1) 0.001(1) 0.003(1) C3 0.018(1) 0.016(1) 0.018(1) -0.003(1) 0.003(1) 0.003(1) N4 0.018(1) 0.012(1) 0.013(1) 0.000(1) 0.001(1) 0.000(1) N11 0.019(1) 0.016(1) 0.018(1) -0.003(1) -0.003(1) -0.003(1) C12 0.021(1) 0.022(1) 0.021(1) -0.005(1) -0.002(1) -0.002(1) C13 0.022(1) 0.033(1) 0.024(1) -0.004(1) 0.002(1) -0.011(1) C14 0.024(1) 0.029(1) 0.034(1) 0.008(1) -0.001(1) -0.013(1) C15 0.028(1) 0.019(1) 0.028(1) 0.004(1) -0.004(1) -0.007(1) C16 0.022(1) 0.016(1) 0.019(1) -0.001(1) -0.002(1) -0.005(1) C17 0.023(1) 0.013(1) 0.022(1) -0.001(1) -0.004(1) 0.000(1) N21 0.018(1) 0.015(1) 0.014(1) -0.002(1) -0.001(1) 0.001(1) C22 0.018(1) 0.016(1) 0.021(1) 0.000(1) 0.002(1) 0.003(1) C23 0.018(1) 0.016(1) 0.028(1) -0.001(1) 0.003(1) -0.002(1) C24 0.018(1) 0.022(1) 0.024(1) -0.002(1) 0.003(1) -0.008(1) C25 0.016(1) 0.025(1) 0.014(1) 0.000(1) 0.002(1) -0.001(1) C26 0.014(1) 0.017(1) 0.014(1) -0.001(1) 0.001(1) 0.000(1) C27 0.021(1) 0.018(1) 0.015(1) 0.000(1) -0.003(1) 0.001(1) N31 0.018(1) 0.016(1) 0.017(1) -0.001(1) -0.001(1) -0.003(1) C32 0.021(1) 0.021(1) 0.022(1) 0.001(1) 0.001(1) -0.003(1) C33 0.028(1) 0.019(1) 0.020(1) 0.002(1) 0.002(1) -0.004(1) C34 0.031(1) 0.018(1) 0.020(1) -0.006(1) -0.002(1) -0.003(1) C35 0.022(1) 0.019(1) 0.018(1) -0.004(1) -0.001(1) -0.002(1) C36 0.019(1) 0.013(1) 0.016(1) 0.000(1) 0.001(1) 0.000(1) C37 0.018(1) 0.020(1) 0.017(1) -0.001(1) -0.001(1) -0.002(1) C41 0.018(1) 0.021(1) 0.015(1) 0.001(1) 0.002(1) -0.004(1) C42 0.019(1) 0.017(1) 0.020(1) 0.001(1) 0.003(1) -0.003(1) O1 0.028(1) 0.018(1) 0.030(1) 0.002(1) 0.008(1) -0.005(1) P1 0.0190(2) 0.0130(2) 0.0182(3) -0.0024(2) 0.0007(2) -0.0029(2) F1 0.047(1) 0.020(1) 0.052(1) 0.009(1) 0.000(1) 0.009(1) F2 0.042(1) 0.038(1) 0.038(1) -0.022(1) -0.003(1) -0.013(1) F3 0.040(1) 0.048(1) 0.028(1) 0.005(1) 0.015(1) 0.005(1) F4 0.031(1) 0.028(1) 0.031(1) 0.008(1) -0.002(1) 0.004(1) F5 0.041(1) 0.027(1) 0.040(1) -0.007(1) -0.017(1) -0.009(1) F6 0.030(1) 0.035(1) 0.034(1) -0.002(1) 0.013(1) -0.003(1) #================================= # 10. MOLECULAR GEOMETRY #10_664 1.500000 -1 0 0 1.000000 0 -1 0 -0.500000 0 0 1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe Cl 2.363(1) yes Fe N1 2.257(2) yes Fe N4 2.271(2) yes Fe N11 2.174(2) yes Fe N21 2.212(2) yes Fe N31 2.243(2) yes N1 C27 1.478(3) no N1 C17 1.484(3) no N1 C2 1.485(3) no C2 C3 1.517(3) no C3 N4 1.487(2) no N4 C37 1.479(3) no N4 C41 1.489(3) no N11 C12 1.342(3) no N11 C16 1.350(3) no C12 C13 1.379(3) no C13 C14 1.391(4) no C14 C15 1.393(4) no C15 C16 1.383(3) no C16 C17 1.511(3) no N21 C26 1.345(3) no N21 C22 1.349(3) no C22 C23 1.382(3) no C23 C24 1.387(3) no C24 C25 1.399(3) no C25 C26 1.382(3) no C26 C27 1.508(3) no N31 C32 1.347(3) no N31 C36 1.350(3) no C32 C33 1.382(3) no C33 C34 1.383(3) no C34 C35 1.384(3) no C35 C36 1.385(3) no C36 C37 1.508(3) no C41 C42 1.521(3) no C42 O1 1.422(2) no P1 F1 1.598(1) no P1 F2 1.594(2) no P1 F4 1.603(2) no P1 F3 1.603(2) no P1 F5 1.596(2) no P1 F6 1.600(2) no C2 H2a 0.950 no C2 H2b 0.950 no C3 H3a 0.950 no C3 H3b 0.950 no C12 H12 0.950 no C13 H13 0.950 no C14 H14 0.950 no C15 H15 0.950 no C17 H17a 0.950 no C17 H17b 0.950 no C22 H22 0.950 no C23 H23 0.950 no C24 H24 0.950 no C25 H25 0.950 no C27 H27a 0.950 no C27 H27b 0.950 no C32 H32 0.950 no C33 H33 0.950 no C34 H34 0.950 no C35 H35 0.950 no C37 H37a 0.950 no C37 H37b 0.950 no C41 H41a 0.950 no C41 H41b 0.950 no C42 H42a 0.950 no C42 H42b 0.950 no O1 HO 0.79(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl Fe N1 165.57(5) yes Cl Fe N4 110.64(5) yes Cl Fe N11 100.56(5) yes Cl Fe N21 92.78(5) yes Cl Fe N31 91.62(5) yes N1 Fe N4 79.40(6) yes N1 Fe N11 74.09(7) yes N1 Fe N21 75.25(6) yes N1 Fe N31 101.28(7) yes N4 Fe N11 143.50(6) yes N4 Fe N21 97.39(6) yes N4 Fe N31 74.47(6) yes N11 Fe N21 99.58(7) yes N11 Fe N31 86.50(6) yes N21 Fe N31 171.71(7) yes Fe N1 C2 109.8(1) no Fe N1 C17 104.7(1) no Fe N1 C27 109.0(1) no Fe N4 C3 105.1(1) no Fe N4 C37 107.3(1) no Fe N11 C12 126.1(1) no Fe N11 C16 114.9(1) no Fe N21 C22 126.0(2) no Fe N21 C26 116.5(1) no Fe N31 C32 126.5(1) no Fe N31 C36 115.5(1) no C17 N1 C27 109.5(2) no C2 N1 C27 110.3(2) no C2 N1 C17 113.3(2) no N1 C2 C3 110.3(2) no C2 C3 N4 112.2(2) no C3 N4 C37 108.2(2) no C37 N4 C41 110.2(2) no C3 N4 C41 109.9(2) no C12 N11 C16 118.5(2) no N11 C12 C13 123.0(2) no C12 C13 C14 118.3(2) no C13 C14 C15 119.4(2) no C14 C15 C16 118.6(2) no N11 C16 C15 122.2(2) no N11 C16 C17 116.0(2) no C15 C16 C17 121.8(2) no N1 C17 C16 109.2(2) no C22 N21 C26 117.5(2) no N21 C22 C23 123.2(2) no C22 C23 C24 118.9(2) no C23 C24 C25 118.4(2) no C24 C25 C26 118.9(2) no N21 C26 C25 123.0(2) no N21 C26 C27 116.6(2) no C25 C26 C27 120.2(2) no N1 C27 C26 111.5(2) no C32 N31 C36 117.7(2) no N31 C32 C33 123.1(2) no C32 C33 C34 118.6(2) no C33 C34 C35 119.0(2) no C34 C35 C36 119.2(2) no N31 C36 C35 122.2(2) no N31 C36 C37 116.3(2) no C35 C36 C37 121.5(2) no N4 C37 C36 111.6(2) no N4 C41 C42 113.4(2) no C41 C42 O1 111.6(2) no F1 P1 F2 90.28(9) no F1 P1 F3 89.61(9) no F1 P1 F4 179.4(1) no F1 P1 F5 90.09(9) no F1 P1 F6 90.52(9) no F2 P1 F3 90.14(9) no F2 P1 F4 89.82(9) no F2 P1 F5 179.5(2) no F2 P1 F6 89.86(9) no F3 P1 F4 89.75(8) no F3 P1 F5 90.24(9) no F3 P1 F6 179.9(6) no F4 P1 F5 89.82(9) no F4 P1 F6 90.12(9) no F5 P1 F6 89.75(9) no H2a C2 H2b 109.5 no N1 C2 H2a 109.3 no C3 C2 H2a 109.3 no N1 C2 H2b 109.3 no C3 C2 H2b 109.3 no H3a C3 H3b 109.5 no N4 C3 H3a 108.8 no C2 C3 H3a 108.8 no N4 C3 H3b 108.8 no C2 C3 H3b 108.8 no N11 C12 H12 118.5 no C13 C12 H12 118.5 no C12 C13 H13 120.9 no C14 C13 H13 120.9 no C13 C14 H14 120.3 no C15 C14 H14 120.3 no C16 C15 H15 120.7 no C14 C15 H15 120.7 no H17a C17 H17b 109.5 no N1 C17 H17a 109.5 no C16 C17 H17a 109.5 no N1 C17 H17b 109.5 no C16 C17 H17b 109.5 no N21 C22 H22 118.4 no C23 C22 H22 118.4 no C22 C23 H23 120.5 no C24 C23 H23 120.5 no C23 C24 H24 120.8 no C25 C24 H24 120.8 no C26 C25 H25 120.6 no C24 C25 H25 120.6 no H27a C27 H27b 109.5 no N1 C27 H27a 109.0 no C26 C27 H27a 109.0 no N1 C27 H27b 109.0 no C26 C27 H27b 109.0 no N31 C32 H32 118.4 no C33 C32 H32 118.4 no C32 C33 H33 120.7 no C34 C33 H33 120.7 no C33 C34 H34 120.5 no C35 C34 H34 120.5 no C34 C35 H35 120.4 no C36 C35 H35 120.4 no H37a C37 H37b 109.5 no N4 C37 H37a 108.9 no C36 C37 H37a 108.9 no N4 C37 H37b 108.9 no C36 C37 H37b 108.9 no H41a C41 H41b 109.5 no N4 C41 H41a 108.5 no C42 C41 H41a 108.5 no N4 C41 H41b 108.5 no C42 C41 H41b 108.5 no H42a C42 H42b 109.5 no O1 C42 H42a 108.9 no C41 C42 H42a 108.9 no O1 C42 H42b 108.9 no C41 C42 H42b 108.9 no C42 O1 HO 114(2) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag Fe N1 C2 C3 -32.1(2) yes N1 C2 C3 N4 55.0(2) yes C2 C3 N4 Fe -46.5(2) yes C3 N4 Fe N1 21.1(1) yes C3 C2 N1 C17 84.5(2) yes C3 C2 N1 C27 -152.4(2) yes C2 C3 N4 C37 -160.9(2) yes C2 C3 N4 C41 78.7(2) yes loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O1 HO Cl 0.79(3) 2.45(3) 3.219(2) 166(3) 10_664 data_Fetpenpr #============================================================================== _database_code_CSD 163873 #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [Fetpenol](PF6).0.5CH3CH2OCH2CH3 ; _chemical_name_common '[Fetpenol](PF6).0.5CH3CH2OCH2CH3' _chemical_formula_sum 'C25 H34 Cl F6 Fe N5 O0.5 P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_weight 648.870 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,-z' _cell_length_a 8.7288(4) _cell_length_b 12.3068(6) _cell_length_c 13.5844(6) _cell_angle_alpha 100.215(1) _cell_angle_beta 96.395(1) _cell_angle_gamma 94.920(1) _cell_volume 1418.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 8127 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29.7 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP,1995' _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.916 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 10123 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.7 _diffrn_reflns_reduction_process 10123 _reflns_number_total 6520 _reflns_number_gt 5945 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix Hydrogen atoms were fixed in calculated positions with C-H = 0.95A and Uiso 20% larger than Ueq for the atom to which it is attached. The solvent molecule O45,C46,C47,C48 is on a symmetry centre and is disorderd. > ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^-|F|}^2^ A = 0.03, B = 0.20 ; _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5945 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_ref 0.038 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_shift/su_max 0.0006 _refine_ls_shift/su_mean 0.00004 _refine_diff_density_max 0.47(6) _refine_diff_density_min -0.39(6) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_occupancy Fe 0.64960(2) 0.25508(2) 0.29988(2) 0.0131(1) Uij 1.0 Cl 0.41725(4) 0.27849(3) 0.37284(3) 0.0183(2) Uij 1.0 N1 0.8329(1) 0.2704(1) 0.1928(1) 0.0164(6) Uij 1.0 C2 0.9886(2) 0.2670(1) 0.2475(1) 0.0193(7) Uij 1.0 C3 1.0013(2) 0.3275(1) 0.3561(1) 0.0179(7) Uij 1.0 N4 0.8792(1) 0.2797(1) 0.4094(1) 0.0153(6) Uij 1.0 N11 0.5302(1) 0.1822(1) 0.1476(1) 0.0189(6) Uij 1.0 C12 0.3750(2) 0.1643(1) 0.1223(1) 0.0244(8) Uij 1.0 C13 0.3056(2) 0.1324(2) 0.0237(1) 0.0281(9) Uij 1.0 C14 0.3987(2) 0.1199(2) -0.0528(1) 0.0302(9) Uij 1.0 C15 0.5584(2) 0.1355(1) -0.0277(1) 0.0265(8) Uij 1.0 C16 0.6201(2) 0.1646(1) 0.0730(1) 0.0195(7) Uij 1.0 C17 0.7926(2) 0.1767(1) 0.1066(1) 0.0207(7) Uij 1.0 N21 0.6833(1) 0.4340(1) 0.2985(1) 0.0174(6) Uij 1.0 C22 0.6317(2) 0.5127(1) 0.3646(1) 0.0213(8) Uij 1.0 C23 0.6637(2) 0.6252(1) 0.3666(1) 0.0257(8) Uij 1.0 C24 0.7528(2) 0.6585(1) 0.2969(1) 0.0279(9) Uij 1.0 C25 0.8085(2) 0.5783(1) 0.2287(1) 0.0234(8) Uij 1.0 C26 0.7715(2) 0.4669(1) 0.2317(1) 0.0180(7) Uij 1.0 C27 0.8206(2) 0.3759(1) 0.1560(1) 0.0207(7) Uij 1.0 N31 0.6665(1) 0.0926(1) 0.3397(1) 0.0160(6) Uij 1.0 C32 0.5454(2) 0.0129(1) 0.3174(1) 0.0189(7) Uij 1.0 C33 0.5305(2) -0.0746(1) 0.3684(1) 0.0234(8) Uij 1.0 C34 0.6430(2) -0.0788(1) 0.4477(1) 0.0236(8) Uij 1.0 C35 0.7691(2) 0.0019(1) 0.4705(1) 0.0199(7) Uij 1.0 C36 0.7782(2) 0.0851(1) 0.4138(1) 0.0162(7) Uij 1.0 C37 0.9181(2) 0.1698(1) 0.4304(1) 0.0181(7) Uij 1.0 C41 0.8740(2) 0.3572(1) 0.5064(1) 0.0185(7) Uij 1.0 C42 0.7555(2) 0.3181(1) 0.5702(1) 0.0222(8) Uij 1.0 C43 0.7565(2) 0.4022(2) 0.6672(1) 0.0291(9) Uij 1.0 P 1.05638(4) -0.10082(3) 0.21160(3) 0.0174(2) Uij 1.0 F1 1.15516(12) 0.00869(9) 0.27803(8) 0.0332(6) Uij 1.0 F2 0.90213(12) -0.03993(10) 0.21987(9) 0.0357(6) Uij 1.0 F3 1.03128(13) -0.14628(10) 0.31258(8) 0.0358(6) Uij 1.0 F4 0.95647(14) -0.20927(9) 0.14580(8) 0.0363(6) Uij 1.0 F5 1.21130(13) -0.16019(10) 0.20484(10) 0.0411(7) Uij 1.0 F6 1.08017(14) -0.05461(10) 0.11112(8) 0.0366(6) Uij 1.0 O44 0.5493(4) 0.4899(3) 0.0204(3) 0.059(2) Uij 0.50 C45 0.7553(10) 0.5386(7) -0.0648(5) 0.081(5) Uij 0.50 C46 0.5892(7) 0.4753(6) -0.0788(5) 0.066(4) Uij 0.50 C47 0.3952(8) 0.4264(8) 0.0152(6) 0.090(6) Uij 0.50 C48 0.3353(10) 0.4384(6) 0.1012(5) 0.076(5) Uij 0.50 H2a 1.0647 0.3013 0.2147 0.023 Uiso 1.0 H2b 1.0063 0.1917 0.2467 0.023 Uiso 1.0 H3a 0.9894 0.4037 0.3569 0.022 Uiso 1.0 H3b 1.1004 0.3211 0.3899 0.022 Uiso 1.0 H12 0.3108 0.1739 0.1746 0.029 Uiso 1.0 H13 0.1959 0.1193 0.0086 0.034 Uiso 1.0 H14 0.3538 0.1010 -0.1214 0.036 Uiso 1.0 H15 0.6247 0.1264 -0.0788 0.032 Uiso 1.0 H17a 0.8210 0.1102 0.1265 0.025 Uiso 1.0 H17b 0.8467 0.1907 0.0524 0.025 Uiso 1.0 H22 0.5703 0.4900 0.4124 0.026 Uiso 1.0 H23 0.6255 0.6785 0.4148 0.031 Uiso 1.0 H24 0.7755 0.7351 0.2957 0.034 Uiso 1.0 H25 0.8710 0.5992 0.1808 0.028 Uiso 1.0 H27a 0.7466 0.3622 0.0972 0.025 Uiso 1.0 H27b 0.9190 0.4005 0.1394 0.025 Uiso 1.0 H32 0.4667 0.0169 0.2642 0.023 Uiso 1.0 H33 0.4451 -0.1305 0.3495 0.028 Uiso 1.0 H34 0.6339 -0.1362 0.4858 0.028 Uiso 1.0 H35 0.8482 0.0003 0.5241 0.024 Uiso 1.0 H37a 0.9637 0.1794 0.4987 0.022 Uiso 1.0 H37b 0.9903 0.1430 0.3871 0.022 Uiso 1.0 H41a 0.8496 0.4267 0.4914 0.022 Uiso 1.0 H41b 0.9737 0.3663 0.5448 0.022 Uiso 1.0 H42a 0.7797 0.2492 0.5867 0.027 Uiso 1.0 H42b 0.6552 0.3087 0.5326 0.027 Uiso 1.0 H43a 0.6825 0.3778 0.7071 0.035 Uiso 1.0 H43b 0.7323 0.4712 0.6507 0.035 Uiso 1.0 H43c 0.8568 0.4116 0.7048 0.035 Uiso 1.0 H45a 0.7822 0.5288 -0.1314 0.097 Uiso 0.50 H45b 0.8255 0.5070 -0.0222 0.097 Uiso 0.50 H45c 0.7543 0.6150 -0.0373 0.097 Uiso 0.50 H46a 0.5190 0.5068 -0.1214 0.080 Uiso 0.50 H46b 0.5902 0.3988 -0.1062 0.080 Uiso 0.50 H47a 0.4055 0.3498 -0.0060 0.108 Uiso 0.50 H47b 0.3254 0.4502 -0.0334 0.108 Uiso 0.50 H48a 0.2367 0.3977 0.0978 0.091 Uiso 0.50 H48b 0.3250 0.5149 0.1224 0.091 Uiso 0.50 H48c 0.4051 0.4145 0.1498 0.091 Uiso 0.50 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 0.0115(1) 0.0146(1) 0.0143(1) 0.0020(1) 0.0025(1) 0.0046(1) Cl 0.0140(2) 0.0229(2) 0.0200(2) 0.0036(1) 0.0060(1) 0.0063(1) N1 0.0155(6) 0.0175(6) 0.0169(6) 0.0031(5) 0.0040(5) 0.0036(5) C2 0.0135(6) 0.0234(7) 0.0219(7) 0.0036(6) 0.0042(6) 0.0048(6) C3 0.0125(6) 0.0200(7) 0.0215(7) 0.0007(5) 0.0023(5) 0.0046(6) N4 0.0138(5) 0.0152(6) 0.0171(6) 0.0009(4) 0.0020(5) 0.0036(5) N11 0.0165(6) 0.0243(6) 0.0165(6) 0.0030(5) 0.0013(5) 0.0054(5) C12 0.0180(7) 0.0346(9) 0.0205(7) 0.0024(6) 0.0012(6) 0.0061(6) C13 0.0199(8) 0.0384(9) 0.0246(8) 0.0016(7) -0.0031(6) 0.0065(7) C14 0.0315(9) 0.0380(10) 0.0180(7) 0.0009(7) -0.0036(7) 0.0031(7) C15 0.0284(8) 0.0316(9) 0.0183(7) 0.0022(7) 0.0043(6) 0.0014(6) C16 0.0201(7) 0.0204(7) 0.0178(7) 0.0029(6) 0.0027(6) 0.0029(6) C17 0.0200(7) 0.0226(7) 0.0185(7) 0.0029(6) 0.0048(6) -0.0001(6) N21 0.0159(6) 0.0169(6) 0.0209(6) 0.0032(5) 0.0036(5) 0.0065(5) C22 0.0196(7) 0.0202(7) 0.0252(8) 0.0039(6) 0.0058(6) 0.0046(6) C23 0.0228(8) 0.0184(7) 0.0348(9) 0.0041(6) 0.0053(7) 0.0002(6) C24 0.0251(8) 0.0161(7) 0.0428(10) 0.0006(6) 0.0052(7) 0.0066(7) C25 0.0202(7) 0.0211(7) 0.0319(8) 0.0010(6) 0.0063(6) 0.0118(6) C26 0.0149(6) 0.0191(7) 0.0211(7) 0.0025(5) 0.0015(5) 0.0071(6) C27 0.0236(7) 0.0216(7) 0.0197(7) 0.0023(6) 0.0072(6) 0.0088(6) N31 0.0167(6) 0.0157(6) 0.0160(6) 0.0024(5) 0.0027(5) 0.0036(5) C32 0.0203(7) 0.0169(7) 0.0186(7) 0.0011(6) 0.0022(6) 0.0017(5) C33 0.0274(8) 0.0156(7) 0.0267(8) -0.0020(6) 0.0083(7) 0.0021(6) C34 0.0373(9) 0.0149(7) 0.0216(7) 0.0056(6) 0.0107(7) 0.0059(6) C35 0.0276(8) 0.0168(7) 0.0172(7) 0.0082(6) 0.0038(6) 0.0050(5) C36 0.0178(7) 0.0150(6) 0.0159(6) 0.0043(5) 0.0037(5) 0.0016(5) C37 0.0153(6) 0.0194(7) 0.0202(7) 0.0050(5) 0.0002(5) 0.0052(6) C41 0.0179(7) 0.0185(7) 0.0175(7) 0.0011(5) -0.0001(6) 0.0013(5) C42 0.0196(7) 0.0270(8) 0.0194(7) 0.0005(6) 0.0027(6) 0.0033(6) C43 0.0237(8) 0.0385(10) 0.0224(8) 0.0017(7) 0.0039(6) -0.0012(7) P 0.0169(2) 0.0199(2) 0.0156(2) 0.0006(1) 0.0019(1) 0.0043(1) F1 0.0314(5) 0.0297(5) 0.0326(6) -0.0075(4) -0.0031(4) 0.0000(4) F2 0.0240(5) 0.0458(7) 0.0358(6) 0.0136(5) 0.0001(4) 0.0014(5) F3 0.0356(6) 0.0492(7) 0.0237(5) -0.0072(5) -0.0004(4) 0.0183(5) F4 0.0474(7) 0.0246(5) 0.0309(6) -0.0085(5) -0.0070(5) 0.0020(4) F5 0.0305(6) 0.0480(7) 0.0479(7) 0.0191(5) 0.0095(5) 0.0076(6) F6 0.0490(7) 0.0398(6) 0.0234(5) -0.0030(5) 0.0081(5) 0.0142(4) O44 0.058(2) 0.071(2) 0.044(2) -0.005(2) 0.003(2) 0.010(2) C45 0.085(5) 0.110(6) 0.050(3) 0.000(4) 0.005(3) 0.029(4) C46 0.061(3) 0.081(4) 0.057(3) 0.018(3) 0.003(3) 0.011(3) C47 0.075(4) 0.131(7) 0.097(5) 0.050(4) 0.029(4) 0.080(5) C48 0.096(5) 0.074(4) 0.059(4) 0.010(4) 0.016(4) 0.012(3) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe N1 2.297(1) yes Fe N4 2.323(1) yes Fe Cl 2.3717(4) yes Fe N11 2.207(1) yes Fe N21 2.201(1) yes Fe N31 2.175(1) yes N1 C17 1.478(2) no N1 C27 1.480(2) no N1 C2 1.482(2) no C2 C3 1.518(2) no C3 N4 1.491(2) no N4 C37 1.489(2) no N4 C41 1.491(2) no N11 C16 1.347(2) no N11 C12 1.349(2) no C12 C13 1.382(2) no C13 C14 1.384(2) no C14 C15 1.387(2) no C15 C16 1.385(2) no C16 C17 1.510(2) no N21 C22 1.343(2) no N21 C26 1.346(2) no C22 C23 1.384(2) no C23 C24 1.385(2) no C24 C25 1.388(2) no C25 C26 1.390(2) no C26 C27 1.505(2) no N31 C36 1.342(2) no N31 C32 1.348(2) no C32 C33 1.384(2) no C33 C34 1.385(2) no C34 C35 1.386(2) no C35 C36 1.388(2) no C36 C37 1.506(2) no C41 C42 1.521(2) no C42 C43 1.524(2) no P F4 1.595(1) no P F5 1.595(1) no P F6 1.596(1) no P F3 1.600(1) no P F2 1.601(1) no P F1 1.603(1) no O44 C46 1.414(7) no O44 C47 1.484(9) no C45 C46 1.561(10) no C47 C48 1.322(10) no C2 H2a 0.950 no C2 H2b 0.950 no C3 H3a 0.950 no C3 H3b 0.950 no C12 H12 0.950 no C13 H13 0.950 no C14 H14 0.950 no C15 H15 0.950 no C17 H17a 0.950 no C17 H17b 0.950 no C22 H22 0.950 no C23 H23 0.950 no C24 H24 0.950 no C25 H25 0.950 no C27 H27a 0.950 no C27 H27b 0.950 no C32 H32 0.950 no C33 H33 0.950 no C34 H34 0.950 no C35 H35 0.950 no C37 H37a 0.950 no C37 H37b 0.950 no C41 H41a 0.950 no C41 H41b 0.950 no C42 H42a 0.950 no C42 H42b 0.950 no C43 H43a 0.950 no C43 H43b 0.950 no C43 H43c 0.950 no C45 H45a 0.950 no C45 H45b 0.950 no C45 H45c 0.950 no C46 H46a 0.950 no C46 H46b 0.950 no C47 H47a 0.950 no C47 H47b 0.950 no C48 H48a 0.950 no C48 H48b 0.950 no C48 H48c 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl Fe N1 159.52(3) yes Cl Fe N4 117.15(3) yes Cl Fe N11 94.55(4) yes Cl Fe N21 90.31(3) yes Cl Fe N31 92.89(3) yes N1 Fe N4 77.95(4) yes N1 Fe N11 74.55(5) yes N1 Fe N21 75.95(5) yes N1 Fe N31 104.65(5) yes N4 Fe N11 146.49(5) yes N4 Fe N21 87.58(4) yes N4 Fe N31 76.38(4) yes N11 Fe N21 103.72(5) yes N11 Fe N31 92.37(5) yes N21 Fe N31 163.30(5) yes Fe N1 C2 109.27(9) yes Fe N1 C17 106.77(9) yes Fe N1 C27 107.96(9) yes Fe N4 C3 106.34(8) yes Fe N4 C37 109.26(8) yes Fe N4 C41 113.59(9) yes Fe N11 C12 125.0(1) yes Fe N11 C16 116.7(1) yes Fe N21 C22 124.3(1) yes Fe N21 C26 117.5(1) yes Fe N31 C32 121.4(1) yes Fe N31 C36 117.15(9) yes C17 N1 C27 109.0(1) no C2 N1 C17 111.9(1) no C2 N1 C27 111.8(1) no N1 C2 C3 111.0(1) no C2 C3 N4 111.0(1) no C37 N4 C41 109.6(1) no C3 N4 C37 109.6(1) no C3 N4 C41 108.4(1) no C12 N11 C16 118.0(1) no N11 C12 C13 122.8(2) no C12 C13 C14 118.8(2) no C13 C14 C15 119.0(2) no C14 C15 C16 119.0(2) no N11 C16 C15 122.3(1) no N11 C16 C17 115.6(1) no C15 C16 C17 122.1(1) no N1 C17 C16 109.5(1) no C22 N21 C26 118.1(1) no N21 C22 C23 123.2(1) no C22 C23 C24 118.5(2) no C23 C24 C25 119.0(1) no C24 C25 C26 119.0(1) no N21 C26 C25 122.2(1) no N21 C26 C27 116.2(1) no C25 C26 C27 121.5(1) no N1 C27 C26 113.6(1) no C32 N31 C36 118.0(1) no N31 C32 C33 122.9(1) no C32 C33 C34 118.6(1) no C33 C34 C35 119.0(1) no C34 C35 C36 119.0(1) no N31 C36 C35 122.4(1) no N31 C36 C37 116.4(1) no C35 C36 C37 121.1(1) no N4 C37 C36 112.7(1) no N4 C41 C42 114.3(1) no C41 C42 C43 111.0(1) no F4 P F5 90.76(7) no F4 P F6 89.97(6) no F3 P F4 90.17(6) no F2 P F4 90.05(6) no F1 P F4 179.4(2) no F5 P F6 90.50(7) no F3 P F5 90.05(7) no F2 P F5 179.1(1) no F1 P F5 89.82(7) no F3 P F6 179.4(2) no F2 P F6 89.82(6) no F1 P F6 90.16(6) no F2 P F3 89.63(6) no F1 P F3 89.70(6) no F1 P F2 89.37(6) no C46 O44 C47 107.1(5) no O44 C46 C45 103.4(5) no O44 C47 C48 114.7(8) no N1 C2 H2a 109.1 no C3 C2 H2a 109.1 no N1 C2 H2b 109.1 no C3 C2 H2b 109.1 no H3a C3 H3b 109.5 no N4 C3 H3a 109.1 no C2 C3 H3a 109.1 no N4 C3 H3b 109.1 no C2 C3 H3b 109.1 no N11 C12 H12 118.6 no C13 C12 H12 118.6 no C12 C13 H13 120.6 no C14 C13 H13 120.6 no C13 C14 H14 120.5 no C15 C14 H14 120.5 no C16 C15 H15 120.5 no C14 C15 H15 120.5 no H17a C17 H17b 109.5 no N1 C17 H17a 109.5 no C16 C17 H17a 109.5 no N1 C17 H17b 109.5 no C16 C17 H17b 109.5 no N21 C22 H22 118.4 no C23 C22 H22 118.4 no C22 C23 H23 120.7 no C24 C23 H23 120.7 no C23 C24 H24 120.5 no C25 C24 H24 120.5 no C24 C25 H25 120.5 no C26 C25 H25 120.5 no H27a C27 H27b 109.5 no N1 C27 H27a 108.4 no C26 C27 H27a 108.4 no N1 C27 H27b 108.4 no C26 C27 H27b 108.4 no N31 C32 H32 118.6 no C33 C32 H32 118.6 no C32 C33 H33 120.7 no C34 C33 H33 120.7 no C33 C34 H34 120.5 no C35 C34 H34 120.5 no C34 C35 H35 120.5 no C36 C35 H35 120.5 no H37a C37 H37b 109.5 no N4 C37 H37a 108.6 no C36 C37 H37a 108.6 no N4 C37 H37b 108.6 no C36 C37 H37b 108.6 no H41a C41 H41b 109.5 no N4 C41 H41a 108.2 no C42 C41 H41a 108.2 no N4 C41 H41b 108.2 no C42 C41 H41b 108.2 no H42a C42 H42b 109.5 no C41 C42 H42a 109.1 no C43 C42 H42a 109.1 no C41 C42 H42b 109.1 no C43 C42 H42b 109.1 no H43a C43 H43b 109.1 no H43a C43 H43c 109.1 no C42 C43 H43a 111.0 no H43b C43 H43c 109.5 no C42 C43 H43b 109.1 no C42 C43 H43c 109.1 no H45a C45 H45b 111.0 no H45a C45 H45c 111.0 no C46 C45 H45a 103.4 no H45b C45 H45c 109.5 no C46 C45 H45b 111.0 no C46 C45 H45c 111.0 no H46a C46 H46b 109.5 no O44 C46 H46a 111.0 no C45 C46 H46a 111.0 no O44 C46 H46b 111.0 no C45 C46 H46b 111.0 no H47a C47 H47b 109.5 no C48 C47 H47a 108.1 no O44 C47 H47a 108.1 no C48 C47 H47b 108.1 no O44 C47 H47b 108.1 no H48a C48 H48b 108.1 no H48a C48 H48c 108.1 no C47 C48 H48a 114.7 no H48b C48 H48c 109.5 no C47 C48 H48b 108.1 no C47 C48 H48c 108.1 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag Fe N1 C2 C3 -37.2(1) no N1 C2 C3 N4 57.2(2) no C2 C3 N4 Fe -44.8(1) no C3 N4 Fe N1 18.4(1) no C3 C2 N1 C17 -155.2(1) no C3 C2 N1 C27 82.3(1) no C2 C3 N4 C37 73.2(1) no C2 C3 N4 C41 -167.2(1) no