# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1943 # CIF-file generated for sm24 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Jan 19 09:47:50 2000' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; ? ; _publ_contact_author_address # address of author for correspondence ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica C' # Publication choise FI FM FO CI CM CO AD _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Regular Structural Paper in Acta Crystallographica C. ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE 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 ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ? ; ? ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Allen, F.H., Kennard, O. & Taylor, R. (1983). Acc. Chem. Res. 16, 146-153. Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garc\'ia-Granda, S., Gould, R.O., Smits, J.M.M. & Smykalla, C. (1992) The DIRDIF96 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Boer, J.L. de & Duisenberg, A.J.M. (1984). Acta Cryst. A40, C-410. Boeyens, J.C.A. (1978). J.Cryst.Mol.Struct. 8, 317-320. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. Flack, H.D. (1983). Acta Cryst. A39, 876-881. LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. Mackay, A.L. (1984). Acta Cryst. A40, 165-166. Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018. North, A.C.T., Phillips, D.C. & Mathews, F.S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. SHELXL93. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1993. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sheldrick, G.M. SHELXS86. Program for Crystal Structure solution. University of G\\"ottingen, Germany, 1986. Sheldrick, G.M. SHELXS97. Program for Crystal Structure solution. University of G\\"ottingen, Germany, 1997. Spek, A.L. (1987). Acta Cryst. C43, 1233-1235. Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1997). HELENA, Program for Datareduction, Utrecht University, The Netherlands. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; View of the title compound with the atom numbering scheme Displacement ellipsoids for non-H atoms are drawn at the 50% probability level ; #=============================================================================== data_sm24 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H28 Fe N8, 2(N O3), 3(H2 O), C2 H3 N' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C42 H37 Fe N11 O9' _chemical_formula_weight 895.676 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.4568(15) _cell_length_b 15.476(2) _cell_length_c 10.9876(13) _cell_angle_alpha 96.259(8) _cell_angle_beta 98.240(5) _cell_angle_gamma 101.269(9) _cell_volume 2035.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.44 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature ? _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10792 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.58 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 6372 # number of observed reflections (> n sig(I)) _reflns_number_gt 5955 _reflns_threshold_expression >2sigma(i) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[^' _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 6372 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2235 _refine_ls_wR_factor_gt 0.2186 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.050 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.093 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Fe1 Fe Uani 0.75967(6) 0.24512(5) 0.49289(6) 1.000 0.0211(2) N1 N Uani 0.8898(3) 0.2614(3) 0.6257(4) 1.000 0.0226(12) N2 N Uani 0.8437(3) 0.1761(3) 0.4117(4) 1.000 0.0226(12) N3 N Uani 0.6568(3) 0.2048(3) 0.3332(4) 1.000 0.0228(12) N4 N Uani 1.1551(5) -0.0690(4) 0.0756(5) 1.000 0.045(2) N5 N Uani 0.6724(3) 0.1524(3) 0.5708(4) 1.000 0.0254(14) N6 N Uani 0.6760(3) 0.3152(3) 0.5741(4) 1.000 0.0235(14) N7 N Uani 0.8178(4) 0.3603(3) 0.4403(4) 1.000 0.0247(14) N8 N Uani 0.3877(5) 0.5705(4) 0.9235(5) 1.000 0.0408(17) C1 C Uani 0.9062(4) 0.3097(4) 0.7380(5) 1.000 0.0261(17) C2 C Uani 1.0025(5) 0.3187(4) 0.8234(5) 1.000 0.0291(16) C3 C Uani 1.0850(5) 0.2758(4) 0.7931(5) 1.000 0.0297(17) C4 C Uani 1.0689(4) 0.2249(4) 0.6778(4) 1.000 0.0247(16) C5 C Uani 0.9716(4) 0.2186(3) 0.5954(4) 1.000 0.0216(16) C6 C Uani 0.9448(4) 0.1685(3) 0.4696(4) 1.000 0.0209(14) C7 C Uani 1.0091(4) 0.1196(4) 0.4110(5) 1.000 0.0241(16) C8 C Uani 0.9685(4) 0.0763(4) 0.2889(5) 1.000 0.0250(17) C9 C Uani 0.8641(4) 0.0839(3) 0.2311(5) 1.000 0.0251(17) C10 C Uani 0.8034(4) 0.1343(3) 0.2945(4) 1.000 0.0224(14) C11 C Uani 0.6939(4) 0.1502(4) 0.2486(5) 1.000 0.0244(17) C12 C Uani 0.6314(5) 0.1155(4) 0.1346(5) 1.000 0.0303(17) C13 C Uani 0.5275(5) 0.1337(4) 0.1031(5) 1.000 0.0332(19) C14 C Uani 0.4886(5) 0.1876(4) 0.1889(5) 1.000 0.0361(19) C15 C Uani 0.5560(4) 0.2222(4) 0.3025(5) 1.000 0.0293(17) C16 C Uani 1.0342(4) 0.0250(4) 0.2192(5) 1.000 0.0263(17) C17 C Uani 0.9838(5) -0.0524(4) 0.1394(5) 1.000 0.0340(17) C18 C Uani 1.0468(6) -0.0967(4) 0.0719(6) 1.000 0.041(2) C19 C Uani 1.2036(5) 0.0071(5) 0.1511(5) 1.000 0.042(2) C20 C Uani 1.1478(5) 0.0537(4) 0.2259(5) 1.000 0.0377(19) C21 C Uani 0.8928(5) 0.3785(4) 0.3657(5) 1.000 0.0313(19) C22 C Uani 0.9273(5) 0.4623(4) 0.3352(5) 1.000 0.0357(19) C23 C Uani 0.8862(5) 0.5321(4) 0.3866(6) 1.000 0.0369(19) C24 C Uani 0.8079(5) 0.5157(4) 0.4628(5) 1.000 0.0311(17) C25 C Uani 0.7747(4) 0.4303(3) 0.4878(5) 1.000 0.0225(16) C26 C Uani 0.6915(4) 0.4036(3) 0.5660(5) 1.000 0.0239(16) C27 C Uani 0.6324(4) 0.4571(4) 0.6268(5) 1.000 0.0262(17) C28 C Uani 0.5563(4) 0.4190(4) 0.6972(5) 1.000 0.0266(17) C29 C Uani 0.5396(4) 0.3272(4) 0.7018(5) 1.000 0.0253(17) C30 C Uani 0.6020(4) 0.2776(3) 0.6413(5) 1.000 0.0226(17) C31 C Uani 0.5991(4) 0.1822(3) 0.6386(5) 1.000 0.0233(16) C32 C Uani 0.5303(4) 0.1261(4) 0.6957(5) 1.000 0.0270(17) C33 C Uani 0.5339(5) 0.0372(4) 0.6838(5) 1.000 0.0310(17) C34 C Uani 0.6076(4) 0.0067(4) 0.6166(5) 1.000 0.0283(17) C35 C Uani 0.6756(4) 0.0655(4) 0.5621(5) 1.000 0.0275(17) C36 C Uani 0.4950(5) 0.4733(4) 0.7696(5) 1.000 0.0280(17) C37 C Uani 0.3859(5) 0.4408(4) 0.7821(6) 1.000 0.0370(19) C38 C Uani 0.3368(5) 0.4927(4) 0.8579(5) 1.000 0.0353(19) C39 C Uani 0.4927(6) 0.6023(4) 0.9116(6) 1.000 0.0387(19) C40 C Uani 0.5476(5) 0.5563(4) 0.8351(5) 1.000 0.0350(17) O1 O Uani 0.3119(4) 0.0948(3) 0.8653(4) 1.000 0.0439(17) O2 O Uani 0.3461(4) 0.2345(3) 0.8497(5) 1.000 0.0624(19) O3 O Uani 0.2632(4) 0.1892(4) 0.9971(4) 1.000 0.0544(18) N9 N Uani 0.3076(4) 0.1734(3) 0.9049(5) 1.000 0.0343(16) O4 O Uani 0.3541(4) 0.2016(3) 0.4634(4) 1.000 0.0462(17) O5 O Uani 0.3792(5) 0.3338(4) 0.4146(6) 1.000 0.072(3) O6 O Uani 0.2433(5) 0.2847(4) 0.5081(6) 1.000 0.076(3) N10 N Uani 0.3230(4) 0.2727(3) 0.4576(5) 1.000 0.0384(17) O8 O Uiso 0.2335(3) 0.0813(3) 0.5976(4) 1.000 0.0357(9) N11 N Uiso 0.2507(4) 0.6387(3) 1.0643(4) 1.000 0.0299(10) C41 C Uiso 0.2262(14) 0.7076(11) 1.0001(15) 1.000 0.136(5) C42 C Uiso 0.1560(12) 0.7489(10) 0.9399(14) 1.000 0.123(5) O9A O Uiso 0.9477(13) 0.6604(10) 0.8446(14) 0.330 0.054(4) O9B O Uiso 0.8627(10) 0.6957(8) 0.8011(11) 0.330 0.036(3) O9C O Uiso 0.8257(13) 0.6756(11) 0.8787(15) 0.330 0.058(4) O7 O Uiso 0.9057(6) 0.5088(5) 0.9200(6) 1.000 0.086(2) H1 H Uiso 0.8511(4) 0.3381(4) 0.7599(5) 1.000 0.0310 H2 H Uiso 1.0119(5) 0.3535(4) 0.9002(5) 1.000 0.0350 H3 H Uiso 1.1498(5) 0.2810(4) 0.8496(5) 1.000 0.0360 H4 H Uiso 1.1232(4) 0.1957(4) 0.6557(4) 1.000 0.0300 H7 H Uiso 1.0778(4) 0.1148(4) 0.4521(5) 1.000 0.0290 H9 H Uiso 0.8358(4) 0.0555(3) 0.1505(5) 1.000 0.0300 H12 H Uiso 0.6584(5) 0.0790(4) 0.0789(5) 1.000 0.0360 H13 H Uiso 0.4845(5) 0.1103(4) 0.0259(5) 1.000 0.0400 H14 H Uiso 0.4190(5) 0.2010(4) 0.1700(5) 1.000 0.0430 H15 H Uiso 0.5297(4) 0.2580(4) 0.3597(5) 1.000 0.0350 H17 H Uiso 0.9077(5) -0.0743(4) 0.1311(5) 1.000 0.0410 H18 H Uiso 1.0116(6) -0.1495(4) 0.0209(6) 1.000 0.0500 H19 H Uiso 1.2789(5) 0.0295(5) 0.1534(5) 1.000 0.0510 H20 H Uiso 1.1864(5) 0.1040(4) 0.2805(5) 1.000 0.0460 H21 H Uiso 0.9222(5) 0.3325(4) 0.3315(5) 1.000 0.0370 H22 H Uiso 0.9788(5) 0.4726(4) 0.2820(5) 1.000 0.0430 H23 H Uiso 0.9101(5) 0.5896(4) 0.3695(6) 1.000 0.0440 H24 H Uiso 0.7781(5) 0.5615(4) 0.4969(5) 1.000 0.0370 H27 H Uiso 0.6441(4) 0.5176(4) 0.6209(5) 1.000 0.0320 H29 H Uiso 0.4872(4) 0.2999(4) 0.7458(5) 1.000 0.0310 H32 H Uiso 0.4821(4) 0.1477(4) 0.7425(5) 1.000 0.0320 H33 H Uiso 0.4863(5) -0.0020(4) 0.7207(5) 1.000 0.0370 H34 H Uiso 0.6109(4) -0.0532(4) 0.6088(5) 1.000 0.0340 H35 H Uiso 0.7256(4) 0.0449(4) 0.5172(5) 1.000 0.0330 H37 H Uiso 0.3469(5) 0.3859(4) 0.7396(6) 1.000 0.0440 H38 H Uiso 0.2628(5) 0.4712(4) 0.8637(5) 1.000 0.0420 H39 H Uiso 0.5301(6) 0.6571(4) 0.9559(6) 1.000 0.0460 H40 H Uiso 0.6202(5) 0.5808(4) 0.8273(5) 1.000 0.0420 H8A H Uiso 0.28210 0.09160 0.67830 1.000 0.0500 H8B H Uiso 0.28220 0.12050 0.56520 1.000 0.0500 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0217(4) 0.0210(4) 0.0232(4) 0.0020(3) 0.0080(3) 0.0083(3) N1 0.026(2) 0.023(2) 0.023(2) 0.003(2) 0.012(2) 0.010(2) N2 0.021(2) 0.024(2) 0.023(2) 0.001(2) 0.003(2) 0.007(2) N3 0.023(2) 0.024(2) 0.024(2) 0.006(2) 0.005(2) 0.009(2) N4 0.063(4) 0.057(4) 0.030(3) 0.008(2) 0.013(2) 0.041(3) N5 0.025(2) 0.028(3) 0.025(2) -0.003(2) 0.007(2) 0.012(2) N6 0.022(2) 0.025(3) 0.024(2) 0.001(2) 0.005(2) 0.007(2) N7 0.027(2) 0.025(3) 0.025(2) 0.002(2) 0.009(2) 0.010(2) N8 0.050(3) 0.043(3) 0.038(3) 0.003(2) 0.017(2) 0.025(3) C1 0.031(3) 0.026(3) 0.025(3) -0.001(2) 0.014(2) 0.011(2) C2 0.040(3) 0.031(3) 0.019(2) 0.001(2) 0.006(2) 0.015(2) C3 0.034(3) 0.031(3) 0.025(3) 0.003(2) 0.005(2) 0.010(2) C4 0.027(3) 0.028(3) 0.020(2) 0.001(2) 0.003(2) 0.010(2) C5 0.025(3) 0.022(3) 0.020(2) 0.001(2) 0.007(2) 0.009(2) C6 0.023(2) 0.017(3) 0.022(2) -0.002(2) 0.007(2) 0.003(2) C7 0.022(2) 0.029(3) 0.023(3) 0.000(2) 0.007(2) 0.009(2) C8 0.028(3) 0.025(3) 0.026(3) 0.003(2) 0.014(2) 0.009(2) C9 0.029(3) 0.022(3) 0.025(3) 0.000(2) 0.010(2) 0.005(2) C10 0.021(2) 0.027(3) 0.021(2) 0.006(2) 0.006(2) 0.006(2) C11 0.026(3) 0.026(3) 0.023(3) 0.007(2) 0.005(2) 0.007(2) C12 0.031(3) 0.032(3) 0.028(3) 0.005(2) 0.003(2) 0.008(2) C13 0.027(3) 0.038(4) 0.033(3) 0.008(2) -0.003(2) 0.007(2) C14 0.031(3) 0.045(4) 0.035(3) 0.008(3) 0.003(2) 0.015(3) C15 0.028(3) 0.032(3) 0.033(3) 0.008(2) 0.006(2) 0.016(2) C16 0.031(3) 0.025(3) 0.028(3) 0.004(2) 0.013(2) 0.012(2) C17 0.042(3) 0.025(3) 0.037(3) 0.000(2) 0.018(3) 0.006(3) C18 0.069(5) 0.023(3) 0.036(3) 0.001(2) 0.018(3) 0.015(3) C19 0.034(3) 0.069(5) 0.029(3) -0.002(3) 0.007(2) 0.027(3) C20 0.031(3) 0.051(4) 0.032(3) -0.006(3) 0.006(2) 0.017(3) C21 0.030(3) 0.040(4) 0.031(3) 0.010(2) 0.016(2) 0.014(2) C22 0.041(3) 0.037(4) 0.034(3) 0.018(2) 0.015(3) 0.007(3) C23 0.037(3) 0.033(4) 0.041(3) 0.013(3) 0.009(3) 0.002(3) C24 0.036(3) 0.023(3) 0.036(3) 0.008(2) 0.008(2) 0.007(2) C25 0.023(2) 0.017(3) 0.028(3) 0.004(2) 0.007(2) 0.003(2) C26 0.023(2) 0.025(3) 0.028(3) 0.004(2) 0.008(2) 0.013(2) C27 0.030(3) 0.019(3) 0.032(3) 0.001(2) 0.010(2) 0.009(2) C28 0.029(3) 0.026(3) 0.028(3) 0.000(2) 0.007(2) 0.014(2) C29 0.026(3) 0.026(3) 0.027(3) 0.001(2) 0.015(2) 0.007(2) C30 0.027(3) 0.018(3) 0.026(3) 0.003(2) 0.009(2) 0.009(2) C31 0.027(3) 0.023(3) 0.023(2) 0.001(2) 0.007(2) 0.012(2) C32 0.025(3) 0.027(3) 0.032(3) 0.006(2) 0.010(2) 0.008(2) C33 0.030(3) 0.030(3) 0.035(3) 0.007(2) 0.012(2) 0.005(2) C34 0.032(3) 0.021(3) 0.033(3) 0.007(2) 0.005(2) 0.007(2) C35 0.028(3) 0.024(3) 0.033(3) 0.000(2) 0.005(2) 0.014(2) C36 0.032(3) 0.029(3) 0.029(3) 0.004(2) 0.012(2) 0.016(2) C37 0.039(3) 0.038(4) 0.039(3) 0.000(3) 0.012(3) 0.019(3) C38 0.031(3) 0.040(4) 0.038(3) -0.003(3) 0.011(2) 0.016(3) C39 0.054(4) 0.024(3) 0.042(3) 0.002(2) 0.019(3) 0.011(3) C40 0.036(3) 0.030(3) 0.042(3) 0.001(2) 0.014(3) 0.011(3) O1 0.048(3) 0.034(3) 0.048(3) 0.004(2) 0.001(2) 0.011(2) O2 0.063(3) 0.042(3) 0.090(4) 0.023(3) 0.037(3) 0.005(3) O3 0.054(3) 0.081(4) 0.031(2) 0.003(2) 0.006(2) 0.025(3) N9 0.026(2) 0.038(3) 0.037(3) 0.005(2) -0.001(2) 0.007(2) O4 0.050(3) 0.031(3) 0.066(3) 0.010(2) 0.024(2) 0.017(2) O5 0.075(4) 0.052(4) 0.115(5) 0.042(3) 0.055(4) 0.032(3) O6 0.077(4) 0.051(4) 0.126(5) 0.027(3) 0.062(4) 0.033(3) N10 0.037(3) 0.024(3) 0.060(3) 0.006(2) 0.021(2) 0.011(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Fe1 N1 1.976(4) . . yes Fe1 N2 1.879(4) . . yes Fe1 N3 1.978(4) . . yes Fe1 N5 1.974(4) . . yes Fe1 N6 1.886(4) . . yes Fe1 N7 1.969(5) . . yes O1 N9 1.260(7) . . yes O2 N9 1.234(7) . . yes O3 N9 1.246(7) . . yes O4 N10 1.241(7) . . yes O5 N10 1.241(8) . . yes O6 N10 1.239(8) . . yes O8 H8A 0.9776 . . no O8 H8B 0.9099 . . no N1 C1 1.338(7) . . yes N1 C5 1.379(6) . . yes N2 C6 1.360(6) . . yes N2 C10 1.355(6) . . yes N3 C11 1.377(7) . . yes N3 C15 1.339(7) . . yes N4 C18 1.327(10) . . yes N4 C19 1.344(9) . . yes N5 C31 1.373(7) . . yes N5 C35 1.347(8) . . yes N6 C26 1.358(7) . . yes N6 C30 1.346(7) . . yes N7 C25 1.385(7) . . yes N7 C21 1.338(8) . . yes N8 C38 1.324(8) . . yes N8 C39 1.335(10) . . yes O9A O9C 1.67(2) . . yes O9A O9B 1.34(2) . . yes O9B O9C 1.07(2) . . yes N11 C41 1.399(17) . . yes C1 C2 1.387(8) . . no C2 C3 1.387(9) . . no C3 C4 1.383(7) . . no C4 C5 1.385(7) . . no C5 C6 1.468(6) . . no C6 C7 1.381(7) . . no C7 C8 1.408(8) . . no C8 C16 1.479(8) . . no C8 C9 1.396(7) . . no C9 C10 1.389(7) . . no C10 C11 1.462(7) . . no C11 C12 1.369(8) . . no C12 C13 1.382(9) . . no C13 C14 1.392(8) . . no C14 C15 1.388(8) . . no C16 C20 1.387(8) . . no C16 C17 1.385(8) . . no C17 C18 1.379(9) . . no C19 C20 1.382(9) . . no C21 C22 1.377(9) . . no C22 C23 1.383(9) . . no C23 C24 1.379(9) . . no C24 C25 1.375(8) . . no C25 C26 1.466(7) . . no C26 C27 1.390(7) . . no C27 C28 1.391(8) . . no C28 C29 1.403(9) . . no C28 C36 1.484(8) . . no C29 C30 1.380(7) . . no C30 C31 1.467(7) . . no C31 C32 1.365(8) . . no C32 C33 1.378(9) . . no C33 C34 1.378(8) . . no C34 C35 1.366(8) . . no C36 C37 1.386(9) . . no C36 C40 1.390(8) . . no C37 C38 1.380(9) . . no C39 C40 1.380(9) . . no C1 H1 0.930(8) . . no C2 H2 0.929(8) . . no C3 H3 0.929(8) . . no C4 H4 0.929(8) . . no C7 H7 0.929(7) . . no C9 H9 0.931(7) . . no C12 H12 0.930(8) . . no C13 H13 0.930(8) . . no C14 H14 0.931(9) . . no C15 H15 0.929(8) . . no C17 H17 0.930(9) . . no C18 H18 0.929(9) . . no C19 H19 0.930(9) . . no C20 H20 0.931(8) . . no C21 H21 0.930(9) . . no C22 H22 0.931(9) . . no C23 H23 0.930(9) . . no C24 H24 0.930(9) . . no C27 H27 0.930(9) . . no C29 H29 0.930(8) . . no C32 H32 0.931(8) . . no C33 H33 0.931(9) . . no C34 H34 0.931(9) . . no C35 H35 0.930(8) . . no C37 H37 0.929(9) . . no C38 H38 0.931(9) . . no C39 H39 0.929(9) . . no C40 H40 0.930(9) . . no C41 C42 1.32(2) . . no 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 N1 Fe1 N2 80.77(18) . . . yes N1 Fe1 N3 161.71(18) . . . yes N1 Fe1 N5 91.96(18) . . . yes N1 Fe1 N6 99.16(18) . . . yes N1 Fe1 N7 91.55(19) . . . yes N2 Fe1 N3 80.94(18) . . . yes N2 Fe1 N5 99.46(19) . . . yes N2 Fe1 N6 179.56(18) . . . yes N2 Fe1 N7 98.7(2) . . . yes N3 Fe1 N5 90.56(18) . . . yes N3 Fe1 N6 99.14(18) . . . yes N3 Fe1 N7 91.68(19) . . . yes N5 Fe1 N6 80.98(19) . . . yes N5 Fe1 N7 161.84(19) . . . yes N6 Fe1 N7 80.9(2) . . . yes H8A O8 H8B 92.64 . . . no Fe1 N1 C1 127.0(3) . . . yes C1 N1 C5 118.3(4) . . . yes Fe1 N1 C5 114.7(3) . . . yes Fe1 N2 C6 120.4(3) . . . yes C6 N2 C10 120.0(4) . . . yes Fe1 N2 C10 119.6(3) . . . yes Fe1 N3 C15 127.1(4) . . . yes C11 N3 C15 118.3(4) . . . yes Fe1 N3 C11 114.5(3) . . . yes C18 N4 C19 116.1(6) . . . yes Fe1 N5 C31 114.2(3) . . . yes Fe1 N5 C35 127.6(3) . . . yes C31 N5 C35 118.2(4) . . . yes Fe1 N6 C30 119.8(4) . . . yes C26 N6 C30 120.2(4) . . . yes Fe1 N6 C26 120.0(3) . . . yes Fe1 N7 C25 114.8(4) . . . yes C21 N7 C25 117.1(5) . . . yes Fe1 N7 C21 128.1(4) . . . yes C38 N8 C39 117.4(6) . . . yes O9B O9A O9C 39.9(9) . . . yes O9A O9B O9C 87.0(14) . . . yes O9A O9C O9B 53.0(11) . . . yes O1 N9 O2 119.1(5) . . . yes O1 N9 O3 120.6(5) . . . yes O2 N9 O3 120.3(5) . . . yes O4 N10 O5 119.7(6) . . . yes O4 N10 O6 118.7(5) . . . yes O5 N10 O6 121.1(6) . . . yes N1 C1 C2 122.3(5) . . . yes C1 C2 C3 119.5(5) . . . no C2 C3 C4 118.9(5) . . . no C3 C4 C5 119.4(5) . . . no N1 C5 C4 121.6(4) . . . yes C4 C5 C6 125.0(5) . . . no N1 C5 C6 113.4(4) . . . yes N2 C6 C7 121.5(4) . . . yes N2 C6 C5 110.8(4) . . . yes C5 C6 C7 127.7(5) . . . no C6 C7 C8 119.1(5) . . . no C7 C8 C16 122.0(5) . . . no C9 C8 C16 119.1(5) . . . no C7 C8 C9 118.8(5) . . . no C8 C9 C10 119.5(5) . . . no C9 C10 C11 127.0(4) . . . no N2 C10 C9 121.1(5) . . . yes N2 C10 C11 111.9(4) . . . yes N3 C11 C10 113.0(4) . . . yes C10 C11 C12 125.4(5) . . . no N3 C11 C12 121.6(5) . . . yes C11 C12 C13 119.9(5) . . . no C12 C13 C14 118.8(5) . . . no C13 C14 C15 118.9(6) . . . no N3 C15 C14 122.4(5) . . . yes C8 C16 C17 121.2(5) . . . no C8 C16 C20 122.0(5) . . . no C17 C16 C20 116.7(5) . . . no C16 C17 C18 119.8(6) . . . no N4 C18 C17 124.1(6) . . . yes N4 C19 C20 123.6(6) . . . yes C16 C20 C19 119.6(6) . . . no N7 C21 C22 123.0(6) . . . yes C21 C22 C23 119.2(6) . . . no C22 C23 C24 119.4(6) . . . no C23 C24 C25 118.8(6) . . . no C24 C25 C26 124.4(5) . . . no N7 C25 C24 122.5(5) . . . yes N7 C25 C26 113.2(4) . . . yes N6 C26 C25 111.2(4) . . . yes N6 C26 C27 121.2(5) . . . yes C25 C26 C27 127.7(5) . . . no C26 C27 C28 119.1(5) . . . no C27 C28 C29 118.8(5) . . . no C29 C28 C36 119.5(5) . . . no C27 C28 C36 121.7(5) . . . no C28 C29 C30 119.6(5) . . . no C29 C30 C31 127.6(5) . . . no N6 C30 C29 121.1(5) . . . yes N6 C30 C31 111.3(4) . . . yes C30 C31 C32 124.7(5) . . . no N5 C31 C30 113.7(4) . . . yes N5 C31 C32 121.7(5) . . . yes C31 C32 C33 119.0(5) . . . no C32 C33 C34 119.8(6) . . . no C33 C34 C35 119.1(6) . . . no N5 C35 C34 122.2(5) . . . yes C28 C36 C40 121.0(6) . . . no C37 C36 C40 117.3(6) . . . no C28 C36 C37 121.5(5) . . . no C36 C37 C38 118.2(6) . . . no N8 C38 C37 124.7(6) . . . yes N8 C39 C40 122.0(6) . . . yes C36 C40 C39 120.4(6) . . . no N1 C1 H1 119.0(6) . . . no C2 C1 H1 118.7(6) . . . no C1 C2 H2 120.2(7) . . . no C3 C2 H2 120.2(7) . . . no C2 C3 H3 120.4(7) . . . no C4 C3 H3 120.7(7) . . . no C5 C4 H4 120.4(5) . . . no C3 C4 H4 120.2(6) . . . no C6 C7 H7 120.3(6) . . . no C8 C7 H7 120.5(6) . . . no C10 C9 H9 120.5(6) . . . no C8 C9 H9 120.0(6) . . . no C13 C12 H12 120.0(7) . . . no C11 C12 H12 120.0(7) . . . no C14 C13 H13 120.7(7) . . . no C12 C13 H13 120.5(7) . . . no C15 C14 H14 120.5(7) . . . no C13 C14 H14 120.6(7) . . . no C14 C15 H15 118.7(6) . . . no N3 C15 H15 118.9(6) . . . no C16 C17 H17 120.1(7) . . . no C18 C17 H17 120.1(7) . . . no N4 C18 H18 117.6(8) . . . no C17 C18 H18 118.3(9) . . . no N4 C19 H19 118.2(8) . . . no C20 C19 H19 118.2(8) . . . no C19 C20 H20 120.1(7) . . . no C16 C20 H20 120.3(7) . . . no N7 C21 H21 118.9(7) . . . no C22 C21 H21 118.2(7) . . . no C23 C22 H22 119.9(7) . . . no C21 C22 H22 120.9(7) . . . no C22 C23 H23 120.8(7) . . . no C24 C23 H23 119.8(7) . . . no C23 C24 H24 120.7(7) . . . no C25 C24 H24 120.5(7) . . . no C26 C27 H27 120.3(6) . . . no C28 C27 H27 120.6(6) . . . no C28 C29 H29 120.3(7) . . . no C30 C29 H29 120.1(7) . . . no C31 C32 H32 120.5(7) . . . no C33 C32 H32 120.5(7) . . . no C32 C33 H33 119.9(7) . . . no C34 C33 H33 120.3(7) . . . no C33 C34 H34 120.2(7) . . . no C35 C34 H34 120.7(6) . . . no C34 C35 H35 119.0(7) . . . no N5 C35 H35 118.8(7) . . . no C36 C37 H37 120.6(7) . . . no C38 C37 H37 121.2(7) . . . no C37 C38 H38 117.6(7) . . . no N8 C38 H38 117.8(7) . . . no C40 C39 H39 118.8(9) . . . no N8 C39 H39 119.2(8) . . . no C36 C40 H40 119.7(7) . . . no C39 C40 H40 120.0(7) . . . no N11 C41 C42 152.5(16) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 179.5(5) . . . . no N2 Fe1 N1 C5 0.6(4) . . . . no N5 Fe1 N1 C1 -81.2(5) . . . . no N5 Fe1 N1 C5 99.9(4) . . . . no N6 Fe1 N1 C1 0.0(5) . . . . no N6 Fe1 N1 C5 -178.9(4) . . . . no N7 Fe1 N1 C1 81.0(5) . . . . no N7 Fe1 N1 C5 -97.9(4) . . . . no N1 Fe1 N2 C6 -0.8(4) . . . . no N1 Fe1 N2 C10 179.7(4) . . . . no N3 Fe1 N2 C6 179.7(4) . . . . no N3 Fe1 N2 C10 0.2(4) . . . . no N5 Fe1 N2 C6 -91.2(4) . . . . no N5 Fe1 N2 C10 89.2(4) . . . . no N7 Fe1 N2 C6 89.4(4) . . . . no N7 Fe1 N2 C10 -90.1(4) . . . . no N2 Fe1 N3 C11 0.4(4) . . . . no N2 Fe1 N3 C15 177.6(5) . . . . no N5 Fe1 N3 C11 -99.1(4) . . . . no N5 Fe1 N3 C15 78.1(5) . . . . no N6 Fe1 N3 C11 179.9(7) . . . . no N6 Fe1 N3 C15 -2.8(5) . . . . no N7 Fe1 N3 C11 98.9(4) . . . . no N7 Fe1 N3 C15 -83.9(5) . . . . no N1 Fe1 N5 C31 99.7(4) . . . . no N1 Fe1 N5 C35 -81.9(4) . . . . no N2 Fe1 N5 C31 -179.4(4) . . . . no N2 Fe1 N5 C35 -1.0(5) . . . . no N3 Fe1 N5 C31 -98.4(4) . . . . no N3 Fe1 N5 C35 80.0(4) . . . . no N6 Fe1 N5 C31 0.7(3) . . . . no N6 Fe1 N5 C35 179.1(5) . . . . no N1 Fe1 N6 C26 88.4(4) . . . . no N1 Fe1 N6 C30 -90.7(4) . . . . no N3 Fe1 N6 C26 -91.9(4) . . . . no N3 Fe1 N6 C30 88.9(4) . . . . no N5 Fe1 N6 C26 179.0(4) . . . . no N5 Fe1 N6 C30 -0.2(4) . . . . no N7 Fe1 N6 C26 -1.7(4) . . . . no N7 Fe1 N6 C30 179.1(4) . . . . no N1 Fe1 N7 C21 82.5(5) . . . . no N1 Fe1 N7 C25 -97.3(4) . . . . no N2 Fe1 N7 C21 1.6(5) . . . . no N2 Fe1 N7 C25 -178.2(4) . . . . no N3 Fe1 N7 C21 -79.5(5) . . . . no N3 Fe1 N7 C25 100.7(4) . . . . no N6 Fe1 N7 C21 -178.5(5) . . . . no N6 Fe1 N7 C25 1.7(4) . . . . no Fe1 N1 C1 C2 -178.1(4) . . . . no C5 N1 C1 C2 0.7(8) . . . . no Fe1 N1 C5 C4 178.8(4) . . . . no Fe1 N1 C5 C6 -0.4(5) . . . . no C1 N1 C5 C4 -0.2(7) . . . . no C1 N1 C5 C6 -179.4(5) . . . . no Fe1 N2 C6 C5 0.7(5) . . . . no Fe1 N2 C6 C7 -178.7(4) . . . . no C10 N2 C6 C5 -179.7(4) . . . . no C10 N2 C6 C7 0.8(7) . . . . no Fe1 N2 C10 C9 179.0(4) . . . . no Fe1 N2 C10 C11 -0.6(6) . . . . no C6 N2 C10 C9 -0.5(7) . . . . no C6 N2 C10 C11 179.8(5) . . . . no Fe1 N3 C11 C10 -0.8(6) . . . . no Fe1 N3 C11 C12 178.9(5) . . . . no C15 N3 C11 C10 -178.3(5) . . . . no C15 N3 C11 C12 1.3(8) . . . . no Fe1 N3 C15 C14 -177.5(4) . . . . no C11 N3 C15 C14 -0.3(8) . . . . no C19 N4 C18 C17 0.2(10) . . . . no C18 N4 C19 C20 2.7(9) . . . . no Fe1 N5 C31 C30 -1.1(6) . . . . no Fe1 N5 C31 C32 178.2(4) . . . . no C35 N5 C31 C30 -179.6(5) . . . . no C35 N5 C31 C32 -0.3(8) . . . . no Fe1 N5 C35 C34 -177.3(4) . . . . no C31 N5 C35 C34 1.0(8) . . . . no Fe1 N6 C26 C25 1.3(6) . . . . no Fe1 N6 C26 C27 -178.8(4) . . . . no C30 N6 C26 C25 -179.5(5) . . . . no C30 N6 C26 C27 0.3(8) . . . . no Fe1 N6 C30 C29 180(2) . . . . no Fe1 N6 C30 C31 -0.3(6) . . . . no C26 N6 C30 C29 0.8(7) . . . . no C26 N6 C30 C31 -179.5(5) . . . . no Fe1 N7 C21 C22 180.0(8) . . . . no C25 N7 C21 C22 -0.2(8) . . . . no Fe1 N7 C25 C24 178.5(4) . . . . no Fe1 N7 C25 C26 -1.5(6) . . . . no C21 N7 C25 C24 -1.3(8) . . . . no C21 N7 C25 C26 178.7(5) . . . . no C39 N8 C38 C37 2.6(9) . . . . no C38 N8 C39 C40 -0.6(9) . . . . no N1 C1 C2 C3 -0.6(9) . . . . no C1 C2 C3 C4 0.0(9) . . . . no C2 C3 C4 C5 0.5(9) . . . . no C3 C4 C5 N1 -0.4(8) . . . . no C3 C4 C5 C6 178.7(5) . . . . no C4 C5 C6 N2 -179.4(5) . . . . no C4 C5 C6 C7 0.0(8) . . . . no N1 C5 C6 C7 179.3(5) . . . . no N1 C5 C6 N2 -0.1(6) . . . . no C5 C6 C7 C8 -179.7(5) . . . . no N2 C6 C7 C8 -0.4(8) . . . . no C6 C7 C8 C16 178.2(5) . . . . no C6 C7 C8 C9 -0.3(8) . . . . no C7 C8 C16 C17 143.5(6) . . . . no C7 C8 C9 C10 0.5(8) . . . . no C16 C8 C9 C10 -178.0(5) . . . . no C9 C8 C16 C20 139.1(6) . . . . no C7 C8 C16 C20 -39.4(9) . . . . no C9 C8 C16 C17 -38.0(8) . . . . no C8 C9 C10 N2 -0.1(7) . . . . no C8 C9 C10 C11 179.4(5) . . . . no C9 C10 C11 N3 -178.7(5) . . . . no C9 C10 C11 C12 1.7(9) . . . . no N2 C10 C11 C12 -178.7(5) . . . . no N2 C10 C11 N3 0.9(6) . . . . no N3 C11 C12 C13 -1.2(9) . . . . no C10 C11 C12 C13 178.3(5) . . . . no C11 C12 C13 C14 0.1(8) . . . . no C12 C13 C14 C15 0.8(9) . . . . no C13 C14 C15 N3 -0.8(9) . . . . no C20 C16 C17 C18 0.1(10) . . . . no C8 C16 C20 C19 -174.7(6) . . . . no C8 C16 C17 C18 177.3(5) . . . . no C17 C16 C20 C19 2.5(8) . . . . no C16 C17 C18 N4 -1.6(10) . . . . no N4 C19 C20 C16 -4.1(10) . . . . no N7 C21 C22 C23 2.3(9) . . . . no C21 C22 C23 C24 -2.9(9) . . . . no C22 C23 C24 C25 1.5(9) . . . . no C23 C24 C25 C26 -179.3(5) . . . . no C23 C24 C25 N7 0.7(9) . . . . no C24 C25 C26 C27 0.3(9) . . . . no N7 C25 C26 N6 0.2(6) . . . . no N7 C25 C26 C27 -179.7(5) . . . . no C24 C25 C26 N6 -179.8(5) . . . . no N6 C26 C27 C28 0.1(8) . . . . no C25 C26 C27 C28 180.0(7) . . . . no C26 C27 C28 C29 -1.7(8) . . . . no C26 C27 C28 C36 176.7(5) . . . . no C29 C28 C36 C37 -37.5(8) . . . . no C27 C28 C29 C30 2.8(8) . . . . no C36 C28 C29 C30 -175.7(5) . . . . no C29 C28 C36 C40 137.7(6) . . . . no C27 C28 C36 C40 -40.7(8) . . . . no C27 C28 C36 C37 144.1(6) . . . . no C28 C29 C30 C31 177.9(5) . . . . no C28 C29 C30 N6 -2.4(8) . . . . no N6 C30 C31 N5 0.9(7) . . . . no N6 C30 C31 C32 -178.4(5) . . . . no C29 C30 C31 N5 -179.4(5) . . . . no C29 C30 C31 C32 1.3(9) . . . . no C30 C31 C32 C33 178.5(5) . . . . no N5 C31 C32 C33 -0.7(8) . . . . no C31 C32 C33 C34 1.0(8) . . . . no C32 C33 C34 C35 -0.4(8) . . . . no C33 C34 C35 N5 -0.6(8) . . . . no C28 C36 C37 C38 175.6(5) . . . . no C37 C36 C40 C39 1.7(9) . . . . no C28 C36 C40 C39 -173.7(6) . . . . no C40 C36 C37 C38 0.2(9) . . . . no C36 C37 C38 N8 -2.5(10) . . . . no N8 C39 C40 C36 -1.6(9) . . . . no 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 O1 C9 3.147(7) . 2_656 no O1 O8 2.935(6) . . no O1 C13 3.379(7) . 1_556 no O2 C3 3.420(8) . 1_455 no O2 C29 3.285(7) . . no O2 C37 3.316(8) . . no O3 C17 3.411(8) . 2_656 no O3 C14 3.266(8) . 1_556 no O3 O9C 2.861(17) . 2_667 no O4 C15 3.261(7) . . no O4 C30 3.330(7) . . no O4 O8 2.835(6) . . no O4 C34 3.391(8) . 2_656 no O4 C29 3.373(7) . . no O5 C15 3.339(8) . . no O5 C27 3.344(9) . 2_666 no O6 C4 3.131(8) . 1_455 no O6 C24 3.266(9) . 2_666 no O7 O9C 2.999(18) . . no O7 N11 2.735(9) . 2_667 no O7 O9A 2.556(17) . . no O7 O7 2.803(10) . 2_767 no O8 O1 2.935(6) . . no O8 O4 2.835(6) . . no O8 C35 3.198(7) . 2_656 no O8 C7 3.412(7) . 1_455 no O9A C21 3.336(17) . 2_766 no O9A C42 2.69(2) . . no O9A C22 3.340(17) . 2_766 no O9A O7 2.556(17) . . no O9C O3 2.861(18) . 2_667 no O9C O7 2.999(18) . . no O1 H8A 2.0283 . . no O1 H17 2.698(8) . 2_656 no O1 H32 2.714(7) . . no O1 H13 2.532(8) . 1_556 no O1 H12 2.904(8) . 2_656 no O1 H9 2.641(7) . 2_656 no O2 H8A 2.6543 . . no O2 H37 2.751(8) . . no O2 H29 2.356(7) . . no O2 H39 2.649(8) . 2_667 no O2 H3 2.680(8) . 1_455 no O2 H32 2.679(7) . . no O3 H3 2.696(8) . 1_455 no O3 H14 2.478(8) . 1_556 no O3 H17 2.606(8) . 2_656 no O4 H15 2.651(7) . . no O4 H20 2.754(7) . 1_455 no O4 H34 2.487(8) . 2_656 no O4 H8B 1.9449 . . no O5 H27 2.439(9) . 2_666 no O5 H15 2.507(8) . . no O6 H24 2.452(9) . 2_666 no O6 H8B 2.7978 . . no O6 H4 2.673(8) . 1_455 no O6 H37 2.826(9) . . no O7 H1 2.912(9) . . no O7 H2 2.673(9) . . no O7 H22 2.823(9) . 2_766 no O8 H7 2.504(7) . 1_455 no O8 H4 2.527(7) . 1_455 no O8 H35 2.388(7) . 2_656 no O9A H22 2.736(17) . 2_766 no O9A H2 2.816(16) . . no O9A H21 2.694(17) . 2_766 no O9C H40 2.638(18) . . no N4 C9 3.323(8) . 2_755 no N4 C42 3.044(16) . 1_644 no N8 C41 3.320(19) . . no N8 N11 2.743(8) . . no N9 C13 3.444(8) . 1_556 no N10 C29 3.425(8) . . no N11 N8 2.743(8) . . no N11 O7 2.735(9) . 2_667 no N11 C1 3.260(7) . 2_667 no N11 C29 3.309(7) . 2_667 no N2 H35 2.732(7) . . no N2 H21 2.716(8) . . no N4 H9 2.532(8) . 2_755 no N6 H15 2.709(7) . . no N6 H1 2.705(7) . . no N9 H17 2.767(8) . 2_656 no N9 H13 2.804(8) . 1_556 no N9 H8A 2.6137 . . no N9 H3 2.857(8) . 1_455 no N10 H8B 2.7415 . . no N11 H1 2.489(7) . 2_667 no C1 N11 3.260(7) . 2_667 no C1 C41 3.525(18) . 2_667 no C3 O2 3.420(8) . 1_655 no C3 C18 3.521(9) . 2_756 no C3 C17 3.581(9) . 2_756 no C4 C17 3.529(8) . 2_756 no C4 O6 3.131(8) . 1_655 no C7 O8 3.412(7) . 1_655 no C9 N4 3.323(8) . 2_755 no C9 O1 3.147(7) . 2_656 no C9 C42 3.386(16) . 2_666 no C10 C42 3.345(16) . 2_666 no C11 C42 3.301(16) . 2_666 no C12 C42 3.303(17) . 2_666 no C12 C41 3.545(18) . 2_666 no C13 N9 3.444(8) . 1_554 no C13 O1 3.379(7) . 1_554 no C14 C39 3.522(9) . 2_666 no C14 O3 3.266(8) . 1_554 no C15 O5 3.339(8) . . no C15 O4 3.261(7) . . no C16 C18 3.573(9) . 2_755 no C17 O3 3.411(8) . 2_656 no C17 C18 3.481(9) . 2_755 no C17 C3 3.581(9) . 2_756 no C17 C4 3.529(8) . 2_756 no C18 C3 3.521(9) . 2_756 no C18 C16 3.573(9) . 2_755 no C18 C17 3.481(9) . 2_755 no C18 C42 3.278(17) . 1_644 no C19 C34 3.269(8) . 2_756 no C21 C23 3.527(9) . 2_766 no C21 O9A 3.336(17) . 2_766 no C22 O9A 3.340(17) . 2_766 no C22 C23 3.546(9) . 2_766 no C23 C21 3.527(9) . 2_766 no C23 C38 3.507(9) . 2_666 no C23 C22 3.546(9) . 2_766 no C24 C37 3.562(9) . 2_666 no C24 O6 3.266(9) . 2_666 no C27 O5 3.344(9) . 2_666 no C29 O2 3.285(7) . . no C29 N10 3.425(8) . . no C29 N11 3.309(7) . 2_667 no C29 O4 3.373(7) . . no C30 O4 3.330(7) . . no C33 C35 3.472(8) . 2_656 no C33 C34 3.441(8) . 2_656 no C34 C19 3.269(8) . 2_756 no C34 C33 3.441(8) . 2_656 no C34 C34 3.390(8) . 2_656 no C34 O4 3.391(8) . 2_656 no C35 C33 3.472(8) . 2_656 no C35 O8 3.198(7) . 2_656 no C37 O2 3.316(8) . . no C37 C24 3.562(9) . 2_666 no C38 C23 3.507(9) . 2_666 no C39 C14 3.522(9) . 2_666 no C41 C1 3.525(18) . 2_667 no C41 C12 3.545(18) . 2_666 no C41 N8 3.320(19) . . no C42 C12 3.303(17) . 2_666 no C42 C10 3.345(16) . 2_666 no C42 N4 3.044(16) . . no C42 C9 3.386(16) . 2_666 no C42 C18 3.278(17) . . no C42 O9A 2.69(2) . . no C42 C11 3.301(16) . 2_666 no C1 H23 2.974(8) . 2_766 no C2 H23 2.899(9) . 2_766 no C3 H23 2.886(9) . 2_766 no C4 H23 2.941(9) . 2_766 no C4 H7 2.880(7) . . no C5 H23 3.002(8) . 2_766 no C7 H20 2.834(8) . . no C7 H4 2.863(7) . . no C9 H12 2.835(8) . . no C9 H17 2.757(8) . . no C10 H21 3.090(8) . . no C11 H33 2.964(8) . 2_656 no C12 H33 2.834(8) . 2_656 no C12 H9 2.865(8) . . no C13 H33 2.958(8) . 2_656 no C14 H39 3.051(9) . 2_666 no C17 H9 2.725(8) . . no C18 H9 3.085(9) . 2_755 no C20 H7 2.874(8) . . no C23 H38 3.079(9) . 2_666 no C24 H27 2.865(8) . . no C26 H1 3.093(8) . . no C27 H24 2.836(8) . . no C27 H40 2.798(8) . . no C29 H32 2.831(9) . . no C29 H37 2.796(8) . . no C30 H15 3.060(8) . . no C32 H8A 3.0073 . . no C32 H29 2.855(8) . . no C34 H19 2.880(8) . 2_756 no C37 H29 2.745(9) . . no C40 H27 2.851(8) . . no C41 H1 3.041(17) . 2_667 no C42 H18 2.786(17) . . no C42 H21 3.049(16) . 2_666 no H1 C41 3.041(17) . 2_667 no H1 N6 2.705(7) . . no H1 C26 3.093(8) . . no H1 N11 2.489(7) . 2_667 no H1 O7 2.912(9) . . no H2 O9A 2.816(16) . 2_767 no H2 O7 2.673(9) . 2_767 no H3 O2 2.680(8) . 1_655 no H3 O3 2.696(8) . 1_655 no H3 N9 2.857(8) . 1_655 no H4 H7 2.375(7) . . no H4 C7 2.863(7) . . no H4 O6 2.673(8) . 1_655 no H4 O8 2.527(7) . 1_655 no H7 O8 2.504(7) . 1_655 no H7 H20 2.483(8) . . no H7 C4 2.880(7) . . no H7 C20 2.874(8) . . no H7 H4 2.375(7) . . no H8A N9 2.6137 . . no H8A C32 3.0073 . . no H8A H32 2.4445 . . no H8A O2 2.6543 . . no H8A O1 2.0283 . . no H8B O4 1.9449 . . no H8B N10 2.7415 . . no H8B O6 2.7978 . . no H8B H35 2.5988 . 2_656 no H9 C17 2.725(8) . . no H9 C12 2.865(8) . . no H9 O1 2.641(7) . 2_656 no H9 H12 2.348(8) . . no H9 H17 2.355(8) . . no H9 N4 2.532(8) . 2_755 no H9 C18 3.085(9) . 2_755 no H12 H9 2.348(8) . . no H12 C9 2.835(8) . . no H12 O1 2.904(8) . 2_656 no H13 N9 2.804(8) . 1_554 no H13 O1 2.532(8) . 1_554 no H14 O3 2.478(8) . 1_554 no H15 N6 2.709(7) . . no H15 C30 3.060(8) . . no H15 O5 2.507(8) . . no H15 O4 2.651(7) . . no H17 C9 2.757(8) . . no H17 O1 2.698(8) . 2_656 no H17 O3 2.606(8) . 2_656 no H17 H9 2.355(8) . . no H17 N9 2.767(8) . 2_656 no H18 C42 2.786(17) . 1_644 no H19 C34 2.880(8) . 2_756 no H20 O4 2.754(7) . 1_655 no H20 C7 2.834(8) . . no H20 H7 2.483(8) . . no H21 N2 2.716(8) . . no H21 O9A 2.694(17) . 2_766 no H21 C42 3.049(16) . 2_666 no H21 C10 3.090(8) . . no H22 O9A 2.736(17) . 2_766 no H22 O7 2.823(9) . 2_766 no H23 C2 2.899(9) . 2_766 no H23 C3 2.886(9) . 2_766 no H23 C1 2.974(8) . 2_766 no H23 C5 3.002(8) . 2_766 no H23 C4 2.941(9) . 2_766 no H24 H27 2.348(8) . . no H24 C27 2.836(8) . . no H24 O6 2.452(9) . 2_666 no H27 O5 2.439(9) . 2_666 no H27 C24 2.865(8) . . no H27 C40 2.851(8) . . no H27 H40 2.452(8) . . no H27 H24 2.348(8) . . no H29 H32 2.340(9) . . no H29 H37 2.393(8) . . no H29 C37 2.745(9) . . no H29 C32 2.855(8) . . no H29 O2 2.356(7) . . no H32 O1 2.714(7) . . no H32 O2 2.679(7) . . no H32 C29 2.831(9) . . no H32 H8A 2.4445 . . no H32 H29 2.340(9) . . no H33 C11 2.964(8) . 2_656 no H33 C12 2.834(8) . 2_656 no H33 C13 2.958(8) . 2_656 no H34 O4 2.487(8) . 2_656 no H35 N2 2.732(7) . . no H35 O8 2.388(7) . 2_656 no H35 H8B 2.5988 . 2_656 no H37 C29 2.796(8) . . no H37 O2 2.751(8) . . no H37 O6 2.826(9) . . no H37 H29 2.393(8) . . no H38 C23 3.079(9) . 2_666 no H39 O2 2.649(8) . 2_667 no H39 C14 3.051(9) . 2_666 no H40 C27 2.798(8) . . no H40 H27 2.452(8) . . no H40 O9C 2.638(18) . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O8 H8A O1 0.9776 2.0283 2.935(6) 153.28 . yes O8 H8B O4 0.9099 1.9449 2.835(6) 165.54 . yes C1 H1 N11 0.930(8) 2.489(7) 3.260(7) 140.3(6) 2_667 yes C4 H4 O8 0.929(8) 2.527(7) 3.434(7) 165.3(6) 1_655 yes C7 H7 O8 0.929(7) 2.504(7) 3.412(7) 165.4(6) 1_655 yes C9 H9 N4 0.931(7) 2.532(8) 3.323(8) 143.0(5) 2_755 yes C13 H13 O1 0.930(8) 2.532(8) 3.379(7) 151.5(7) 1_554 yes C14 H14 O3 0.931(9) 2.478(8) 3.266(8) 142.6(6) 1_554 yes C15 H15 O5 0.929(8) 2.507(8) 3.339(8) 149.2(6) . yes C24 H24 O6 0.930(9) 2.452(9) 3.266(9) 146.1(6) 2_666 yes C27 H27 O5 0.930(9) 2.439(9) 3.344(9) 164.5(6) 2_666 yes C29 H29 O2 0.930(8) 2.356(7) 3.285(7) 176.4(6) . yes C34 H34 O4 0.931(9) 2.487(8) 3.391(8) 163.5(6) 2_656 yes C35 H35 O8 0.930(8) 2.388(7) 3.198(7) 145.6(6) 2_656 yes # End of Crystallographic Information File data_dp9602 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H48 F24 Fe N10 P4' _chemical_formula_weight 1520.79 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.844(9) _cell_length_b 16.940(7) _cell_length_c 13.393(3) _cell_angle_alpha 97.31(3) _cell_angle_beta 106.67(3) _cell_angle_gamma 65.50(3) _cell_volume 3133.4(23) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30 _cell_measurement_theta_max 45 _exptl_crystal_description prism _exptl_crystal_colour 'v dark blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150K _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device AFC7R _diffrn_measurement_method 'omega 2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1% _diffrn_reflns_number 8598 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8165 _reflns_number_observed 4717 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+24.0548P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8163 _refine_ls_number_parameters 837 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_obs 0.0827 _refine_ls_wR_factor_all 0.2177 _refine_ls_wR_factor_obs 0.1736 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.024 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max 0.028 _refine_ls_shift/esd_mean 0.001 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 _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.13052(9) 0.26175(8) 0.21712(10) 0.0263(4) Uani 1 d . . P1 P 0.2502(2) -0.0765(2) 0.7054(2) 0.0398(7) Uani 1 d . . P2 P 0.3396(2) 0.4683(2) 0.1793(2) 0.0296(6) Uani 1 d . . P3 P 0.0000 0.0000 0.0000 0.0351(9) Uani 1 d S . P4 P 0.7019(2) 0.4758(2) 0.2984(2) 0.0418(7) Uani 1 d . . P5 P 0.5000 0.0000 0.5000 0.105(3) Uani 1 d S . F1 F 0.1401(6) -0.0549(5) 0.6419(7) 0.102(3) Uani 1 d . . F2 F 0.2701(6) -0.1033(4) 0.5942(6) 0.095(3) Uani 1 d . . F3 F 0.2281(4) 0.0214(4) 0.6896(5) 0.057(2) Uani 1 d . . F4 F 0.3550(6) -0.0980(6) 0.7591(10) 0.156(5) Uani 1 d . . F5 F 0.2161(8) -0.0517(4) 0.8064(6) 0.131(4) Uani 1 d . . F6 F 0.2698(6) -0.1757(4) 0.7206(5) 0.083(3) Uani 1 d . . F7 F 0.2762(4) 0.4769(3) 0.0603(4) 0.0403(14) Uani 1 d . . F8 F 0.3125(4) 0.5703(3) 0.1825(4) 0.0411(14) Uani 1 d . . F9 F 0.4309(4) 0.4513(4) 0.1399(4) 0.047(2) Uani 1 d . . F10 F 0.4000(4) 0.4621(3) 0.2977(4) 0.0417(14) Uani 1 d . . F11 F 0.3641(4) 0.3667(3) 0.1752(4) 0.0416(14) Uani 1 d . . F12 F 0.2457(4) 0.4868(4) 0.2174(4) 0.0442(15) Uani 1 d . . F13 F -0.0681(6) 0.0076(5) -0.1128(5) 0.092(3) Uani 1 d . . F14 F -0.0867(5) 0.0248(6) 0.0479(7) 0.101(3) Uani 1 d . . F15 F 0.0150(5) -0.0988(4) -0.0013(5) 0.067(2) Uani 1 d . . F16 F 0.7492(5) 0.4691(5) 0.2058(5) 0.067(2) Uani 1 d . . F17 F 0.7184(5) 0.5623(4) 0.3391(5) 0.063(2) Uani 1 d . . F18 F 0.6550(4) 0.4830(4) 0.3929(5) 0.055(2) Uani 1 d . . F19 F 0.8057(4) 0.4207(4) 0.3706(5) 0.057(2) Uani 1 d . . F20 F 0.5990(5) 0.5327(6) 0.2300(6) 0.094(3) Uani 1 d . . F21 F 0.6872(6) 0.3892(5) 0.2601(5) 0.083(2) Uani 1 d . . F22 F 0.4259(6) -0.0052(6) 0.3934(8) 0.140(4) Uani 1 d . . F24 F 0.5571(6) 0.0244(6) 0.4353(8) 0.123(4) Uani 1 d . . N1 N 0.0938(5) 0.3272(4) 0.0883(5) 0.024(2) Uani 1 d . . N2 N 0.0105(5) 0.2561(4) 0.1542(5) 0.023(2) Uani 1 d . . N3 N 0.1295(5) 0.1881(5) 0.3202(5) 0.030(2) Uani 1 d . . N4 N 0.0775(5) 0.3713(5) 0.2941(5) 0.027(2) Uani 1 d . . N5 N 0.2460(5) 0.2727(4) 0.2881(5) 0.024(2) Uani 1 d . . N6 N 0.2210(5) 0.1577(5) 0.1629(6) 0.035(2) Uani 1 d . . N7 N -0.4684(5) 0.3072(5) -0.0259(6) 0.034(2) Uani 1 d . . N8 N 0.6622(5) 0.3404(5) 0.5322(6) 0.034(2) Uani 1 d . . N9 N 0.6327(10) 0.2287(8) 0.7868(9) 0.085(4) Uani 1 d . . N10 N -0.8374(18) 0.2950(11) -0.4429(18) 0.188(11) Uani 1 d . . C1 C 0.1486(7) 0.3581(6) 0.0560(7) 0.031(2) Uani 1 d . . H1 H 0.2094(7) 0.3500(6) 0.0980(7) 0.037 Uiso 1 calc R . C2 C 0.1162(7) 0.4009(6) -0.0372(7) 0.033(2) Uani 1 d . . H2 H 0.1556(7) 0.4199(6) -0.0582(7) 0.040 Uiso 1 calc R . C3 C 0.0249(7) 0.4154(6) -0.0994(7) 0.033(2) Uani 1 d . . H3 H 0.0018(7) 0.4453(6) -0.1617(7) 0.040 Uiso 1 calc R . C4 C -0.0316(6) 0.3849(6) -0.0675(7) 0.029(2) Uani 1 d . . H4 H -0.0931(6) 0.3936(6) -0.1083(7) 0.035 Uiso 1 calc R . C5 C 0.0046(6) 0.3412(5) 0.0257(7) 0.025(2) Uani 1 d . . C6 C -0.0467(6) 0.3035(5) 0.0678(6) 0.022(2) Uani 1 d . . C7 C -0.1410(6) 0.3131(5) 0.0307(6) 0.023(2) Uani 1 d . . H7 H -0.1797(6) 0.3455(5) -0.0288(6) 0.027 Uiso 1 calc R . C8 C -0.1785(6) 0.2743(5) 0.0824(7) 0.024(2) Uani 1 d . . C9 C -0.1178(6) 0.2244(6) 0.1705(7) 0.030(2) Uani 1 d . . H9 H -0.1405(6) 0.1966(6) 0.2055(7) 0.036 Uiso 1 calc R . C10 C -0.0241(6) 0.2170(6) 0.2050(7) 0.025(2) Uani 1 d . . C11 C 0.0492(6) 0.1710(6) 0.2974(7) 0.027(2) Uani 1 d . . C12 C 0.0403(7) 0.1138(6) 0.3553(8) 0.038(3) Uani 1 d . . H12 H -0.0158(7) 0.1041(6) 0.3396(8) 0.046 Uiso 1 calc R . C13 C 0.1180(7) 0.0713(7) 0.4376(8) 0.044(3) Uani 1 d . . H13 H 0.1148(7) 0.0316(7) 0.4768(8) 0.053 Uiso 1 calc R . C14 C 0.1998(7) 0.0879(7) 0.4614(8) 0.044(3) Uani 1 d . . H14 H 0.2516(7) 0.0604(7) 0.5169(8) 0.053 Uiso 1 calc R . C15 C 0.2033(7) 0.1463(6) 0.4007(7) 0.038(3) Uani 1 d . . H15 H 0.2586(7) 0.1571(6) 0.4162(7) 0.045 Uiso 1 calc R . C16 C -0.5907(6) 0.2461(5) -0.1086(6) 0.035(2) Uiso 1 d G . C17 C -0.6141(7) 0.1894(6) -0.0665(6) 0.130(7) Uiso 1 d G . H17A H -0.6209(11) 0.1979(9) 0.0012(7) 0.156 Uiso 1 calc R . C18 C -0.6275(7) 0.1199(6) -0.1258(8) 0.104(5) Uiso 1 d G . H18A H -0.6431(11) 0.0819(8) -0.0977(12) 0.125 Uiso 1 calc R . C19 C -0.6174(7) 0.1071(5) -0.2270(8) 0.083(4) Uiso 1 d G . H19A H -0.6263(10) 0.0606(7) -0.2667(11) 0.100 Uiso 1 calc R . C20 C -0.5940(8) 0.1639(7) -0.2690(6) 0.162(9) Uiso 1 d G . H20A H -0.5872(12) 0.1554(10) -0.3368(7) 0.194 Uiso 1 calc R . C21 C -0.5806(7) 0.2334(6) -0.2098(7) 0.105(5) Uiso 1 d G . H21A H -0.5650(10) 0.2713(8) -0.2379(10) 0.126 Uiso 1 calc R . C22 C -0.5722(7) 0.3208(8) -0.0635(12) 0.079(5) Uani 1 d . . H22A H -0.6009(7) 0.3411(8) -0.0051(12) 0.094 Uiso 1 calc R . H22B H -0.6044(7) 0.3665(8) -0.1149(12) 0.094 Uiso 1 calc R . C23 C -0.4441(6) 0.3727(6) -0.0336(7) 0.029(2) Uani 1 d . . H23 H -0.4910(6) 0.4246(6) -0.0637(7) 0.035 Uiso 1 calc R . F23 F 0.4335(6) 0.0987(6) 0.5070(9) 0.133(4) Uani 1 d . . C24 C -0.3508(6) 0.3635(6) 0.0026(6) 0.025(2) Uani 1 d . . H24 H -0.3351(6) 0.4101(6) -0.0007(6) 0.030 Uiso 1 calc R . C25 C -0.2796(6) 0.2862(5) 0.0442(6) 0.020(2) Uani 1 d . . C26 C -0.3076(7) 0.2197(6) 0.0513(7) 0.033(2) Uani 1 d . . H26 H -0.2619(7) 0.1670(6) 0.0804(7) 0.040 Uiso 1 calc R . C27 C -0.4019(7) 0.2315(6) 0.0160(8) 0.037(3) Uani 1 d . . H27 H -0.4199(7) 0.1868(6) 0.0210(8) 0.044 Uiso 1 calc R . C28 C -0.0149(7) 0.4222(6) 0.2906(7) 0.029(2) Uani 1 d . . H28 H -0.0620(7) 0.4036(6) 0.2506(7) 0.035 Uiso 1 calc R . C29 C -0.0430(7) 0.4991(6) 0.3423(7) 0.033(2) Uani 1 d . . H29 H -0.1078(7) 0.5317(6) 0.3378(7) 0.040 Uiso 1 calc R . C30 C 0.0253(7) 0.5287(6) 0.4017(7) 0.036(2) Uani 1 d . . H30 H 0.0075(7) 0.5821(6) 0.4360(7) 0.043 Uiso 1 calc R . C31 C 0.1208(7) 0.4766(6) 0.4085(7) 0.030(2) Uani 1 d . . H31 H 0.1684(7) 0.4940(6) 0.4497(7) 0.037 Uiso 1 calc R . C32 C 0.1458(6) 0.3992(6) 0.3545(6) 0.026(2) Uani 1 d . . C33 C 0.2434(6) 0.3399(6) 0.3546(6) 0.022(2) Uani 1 d . . C34 C 0.3268(6) 0.3493(6) 0.4106(7) 0.027(2) Uani 1 d . . H34 H 0.3248(6) 0.3953(6) 0.4573(7) 0.033 Uiso 1 calc R . C35 C 0.4136(6) 0.2886(6) 0.3954(7) 0.027(2) Uani 1 d . . C36 C 0.4167(6) 0.2179(6) 0.3305(7) 0.033(2) Uani 1 d . . H36 H 0.4749(6) 0.1759(6) 0.3221(7) 0.039 Uiso 1 calc R . C37 C 0.3301(6) 0.2112(6) 0.2777(7) 0.030(2) Uani 1 d . . C38 C 0.3167(7) 0.1423(6) 0.2030(8) 0.040(3) Uani 1 d . . C39 C 0.3893(8) 0.0688(7) 0.1800(11) 0.083(5) Uani 1 d . . H39 H 0.4532(8) 0.0594(7) 0.2105(11) 0.099 Uiso 1 calc R . C40 C 0.3654(9) 0.0090(9) 0.1106(14) 0.122(8) Uani 1 d . . H40 H 0.4130(9) -0.0410(9) 0.0929(14) 0.147 Uiso 1 calc R . C41 C 0.2691(8) 0.0249(8) 0.0678(13) 0.099(6) Uani 1 d . . H41 H 0.2515(8) -0.0145(8) 0.0209(13) 0.119 Uiso 1 calc R . C42 C 0.2004(8) 0.0987(7) 0.0949(9) 0.054(3) Uani 1 d . . H42 H 0.1363(8) 0.1086(7) 0.0648(9) 0.065 Uiso 1 calc R . C43 C 0.8477(8) 0.2588(7) 0.7307(8) 0.057(3) Uani 1 d . . H43 H 0.8073(8) 0.2982(7) 0.7691(8) 0.069 Uiso 1 calc R . C44 C 0.9213(10) 0.1844(8) 0.7782(9) 0.069(4) Uani 1 d . . H44 H 0.9327(10) 0.1762(8) 0.8490(9) 0.083 Uiso 1 calc R . C45 C 0.9765(9) 0.1236(9) 0.7225(11) 0.074(4) Uani 1 d . . H45 H 1.0266(9) 0.0738(9) 0.7542(11) 0.089 Uiso 1 calc R . C46 C 0.9575(10) 0.1366(11) 0.6190(12) 0.104(6) Uani 1 d . . H46 H 0.9925(10) 0.0934(11) 0.5788(12) 0.125 Uiso 1 calc R . C47 C 0.8877(9) 0.2120(10) 0.5724(11) 0.082(5) Uani 1 d . . H47 H 0.8772(9) 0.2203(10) 0.5019(11) 0.099 Uiso 1 calc R . C48 C 0.8331(7) 0.2757(6) 0.6299(8) 0.036(3) Uani 1 d . . C49 C 0.7523(6) 0.3562(6) 0.5780(8) 0.037(3) Uani 1 d . . H49A H 0.7407(6) 0.4031(6) 0.6288(8) 0.044 Uiso 1 calc R . H49B H 0.7702(6) 0.3733(6) 0.5234(8) 0.044 Uiso 1 calc R . C50 C 0.6498(7) 0.3071(6) 0.4352(8) 0.039(3) Uani 1 d . . H50 H 0.6944(7) 0.2969(6) 0.3976(8) 0.047 Uiso 1 calc R . C51 C 0.5703(6) 0.2884(6) 0.3922(7) 0.035(2) Uani 1 d . . H51 H 0.5617(6) 0.2649(6) 0.3252(7) 0.042 Uiso 1 calc R . C52 C 0.5032(6) 0.3038(5) 0.4462(7) 0.026(2) Uani 1 d . . C53 C 0.5187(7) 0.3375(6) 0.5459(7) 0.036(3) Uani 1 d . . H53 H 0.4749(7) 0.3479(6) 0.5848(7) 0.043 Uiso 1 calc R . C54 C 0.5989(7) 0.3559(6) 0.5879(7) 0.039(3) Uani 1 d . . H54 H 0.6091(7) 0.3790(6) 0.6549(7) 0.047 Uiso 1 calc R . C55 C 0.6741(10) 0.1715(9) 0.7436(10) 0.059(3) Uani 1 d . . C56 C 0.7277(10) 0.0986(9) 0.6852(12) 0.098(5) Uani 1 d . . H56A H 0.6925(32) 0.0626(33) 0.6592(61) 0.117 Uiso 1 calc R . H56B H 0.7891(28) 0.0652(34) 0.7301(21) 0.117 Uiso 1 calc R . H56C H 0.7369(56) 0.1200(9) 0.6278(42) 0.117 Uiso 1 calc R . C57 C -0.8502(13) 0.2690(11) -0.3749(18) 0.100(6) Uani 1 d . . C58 C -0.8633(11) 0.2386(11) -0.2862(14) 0.108(6) Uani 1 d . . H58A H -0.8378(63) 0.1764(11) -0.2873(43) 0.129 Uiso 1 calc R . H58B H -0.9306(12) 0.2611(52) -0.2896(42) 0.129 Uiso 1 calc R . H58C H -0.8303(58) 0.2583(53) -0.2229(14) 0.129 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0264(8) 0.0271(8) 0.0229(8) 0.0052(6) -0.0059(6) -0.0149(6) P1 0.050(2) 0.032(2) 0.040(2) 0.0059(13) 0.0154(14) -0.0150(13) P2 0.0317(14) 0.0309(15) 0.0265(14) 0.0047(11) 0.0011(11) -0.0157(12) P3 0.038(2) 0.037(2) 0.029(2) -0.002(2) 0.001(2) -0.020(2) P4 0.040(2) 0.056(2) 0.029(2) -0.0021(13) 0.0027(13) -0.0226(15) P5 0.054(3) 0.081(4) 0.153(6) 0.068(4) -0.050(4) -0.033(3) F1 0.081(6) 0.081(6) 0.140(8) 0.000(5) 0.002(5) -0.048(5) F2 0.151(8) 0.052(5) 0.067(5) 0.015(4) 0.044(5) -0.011(5) F3 0.064(4) 0.035(4) 0.065(4) 0.015(3) 0.000(3) -0.021(3) F4 0.054(5) 0.079(6) 0.278(14) 0.039(7) -0.057(7) -0.028(5) F5 0.263(12) 0.033(4) 0.083(6) 0.012(4) 0.115(7) 0.002(6) F6 0.173(8) 0.031(4) 0.064(5) -0.004(3) 0.069(5) -0.036(4) F7 0.041(3) 0.050(4) 0.028(3) 0.008(3) -0.001(3) -0.021(3) F8 0.052(4) 0.033(3) 0.036(3) 0.009(3) 0.001(3) -0.020(3) F9 0.034(3) 0.059(4) 0.055(4) 0.004(3) 0.010(3) -0.024(3) F10 0.042(3) 0.041(3) 0.035(3) 0.008(3) -0.008(3) -0.020(3) F11 0.049(4) 0.033(3) 0.038(3) 0.001(3) 0.002(3) -0.018(3) F12 0.040(3) 0.061(4) 0.038(3) 0.008(3) 0.009(3) -0.026(3) F13 0.138(7) 0.104(6) 0.045(4) 0.012(4) -0.032(4) -0.091(6) F14 0.081(5) 0.120(7) 0.136(8) -0.058(6) 0.068(5) -0.063(5) F15 0.085(5) 0.046(4) 0.061(4) 0.005(3) -0.011(4) -0.035(4) F16 0.078(5) 0.102(6) 0.039(4) -0.004(4) 0.016(3) -0.053(4) F17 0.070(5) 0.040(4) 0.080(5) -0.001(3) 0.013(4) -0.027(3) F18 0.051(4) 0.057(4) 0.050(4) -0.002(3) 0.020(3) -0.011(3) F19 0.039(4) 0.060(4) 0.054(4) 0.015(3) 0.003(3) -0.003(3) F20 0.043(4) 0.157(8) 0.069(5) 0.053(5) -0.026(4) -0.038(5) F21 0.126(7) 0.104(6) 0.066(5) -0.038(4) 0.043(5) -0.090(5) F22 0.073(6) 0.143(9) 0.171(10) 0.070(7) -0.072(6) -0.061(6) F24 0.068(6) 0.107(7) 0.179(10) 0.070(7) -0.026(6) -0.039(5) N1 0.033(5) 0.029(4) 0.018(4) -0.004(3) 0.005(4) -0.020(4) N2 0.025(4) 0.018(4) 0.021(4) 0.002(3) -0.005(3) -0.011(3) N3 0.035(5) 0.029(5) 0.020(4) 0.006(3) -0.007(4) -0.015(4) N4 0.033(5) 0.027(4) 0.021(4) 0.002(3) 0.003(4) -0.013(4) N5 0.028(5) 0.024(4) 0.020(4) 0.005(3) -0.005(3) -0.016(4) N6 0.029(5) 0.029(5) 0.039(5) 0.002(4) -0.009(4) -0.013(4) N7 0.021(4) 0.037(5) 0.051(6) -0.005(4) 0.010(4) -0.018(4) N8 0.032(5) 0.032(5) 0.034(5) 0.003(4) -0.003(4) -0.017(4) N9 0.133(11) 0.076(9) 0.071(8) -0.010(7) 0.052(8) -0.051(8) N10 0.297(28) 0.069(12) 0.186(21) 0.001(12) 0.144(21) -0.009(13) C1 0.030(5) 0.036(6) 0.030(6) -0.007(5) 0.006(5) -0.020(5) C2 0.042(6) 0.051(7) 0.022(5) 0.003(5) 0.008(5) -0.032(5) C3 0.046(6) 0.038(6) 0.020(5) 0.011(4) 0.003(5) -0.022(5) C4 0.029(5) 0.036(6) 0.026(5) 0.000(4) 0.002(4) -0.020(5) C5 0.028(5) 0.024(5) 0.022(5) 0.002(4) -0.001(4) -0.014(4) C6 0.020(5) 0.022(5) 0.019(5) 0.004(4) 0.000(4) -0.005(4) C7 0.021(5) 0.022(5) 0.017(5) 0.000(4) -0.004(4) -0.006(4) C8 0.025(5) 0.018(5) 0.030(5) 0.000(4) 0.003(4) -0.013(4) C9 0.034(6) 0.038(6) 0.026(5) 0.004(5) 0.002(5) -0.024(5) C10 0.028(5) 0.030(5) 0.020(5) 0.003(4) -0.005(4) -0.020(4) C11 0.030(5) 0.027(5) 0.019(5) 0.006(4) -0.010(4) -0.016(4) C12 0.038(6) 0.039(6) 0.043(6) 0.015(5) 0.000(5) -0.024(5) C13 0.042(7) 0.044(7) 0.044(7) 0.022(5) -0.003(5) -0.020(5) C14 0.045(7) 0.048(7) 0.035(6) 0.015(5) -0.012(5) -0.026(6) C15 0.034(6) 0.043(6) 0.033(6) 0.010(5) -0.012(5) -0.023(5) C22 0.025(6) 0.057(8) 0.155(14) -0.024(8) 0.017(7) -0.028(6) C23 0.025(5) 0.024(5) 0.036(6) 0.006(4) 0.006(4) -0.007(4) F23 0.079(6) 0.091(7) 0.195(11) 0.070(7) -0.030(6) -0.024(5) C24 0.024(5) 0.034(6) 0.023(5) 0.001(4) 0.006(4) -0.018(4) C25 0.029(5) 0.015(5) 0.018(5) 0.002(4) 0.007(4) -0.009(4) C26 0.033(6) 0.030(6) 0.034(6) 0.008(5) 0.001(5) -0.014(5) C27 0.035(6) 0.036(6) 0.052(7) 0.007(5) 0.007(5) -0.026(5) C28 0.039(6) 0.039(6) 0.021(5) 0.001(5) 0.002(4) -0.029(5) C29 0.033(6) 0.035(6) 0.034(6) -0.004(5) 0.010(5) -0.017(5) C30 0.044(7) 0.034(6) 0.037(6) -0.011(5) 0.028(5) -0.015(5) C31 0.046(6) 0.034(6) 0.025(5) -0.003(4) 0.012(5) -0.028(5) C32 0.037(6) 0.037(6) 0.014(5) 0.007(4) -0.001(4) -0.026(5) C33 0.033(6) 0.026(5) 0.011(5) 0.002(4) 0.002(4) -0.016(4) C34 0.035(6) 0.036(6) 0.018(5) -0.002(4) 0.002(4) -0.025(5) C35 0.034(6) 0.029(6) 0.018(5) 0.006(4) -0.007(4) -0.019(5) C36 0.022(5) 0.025(5) 0.034(6) 0.005(5) -0.013(4) -0.005(4) C37 0.028(6) 0.019(5) 0.032(6) 0.007(4) -0.007(4) -0.007(5) C38 0.029(6) 0.032(6) 0.047(7) -0.006(5) -0.010(5) -0.015(5) C39 0.030(7) 0.035(7) 0.134(13) -0.035(8) -0.015(7) 0.000(6) C40 0.038(8) 0.069(10) 0.195(18) -0.083(11) -0.005(9) -0.006(7) C41 0.039(8) 0.056(9) 0.157(15) -0.058(9) -0.009(8) -0.014(7) C42 0.041(7) 0.041(7) 0.063(8) -0.017(6) -0.013(6) -0.022(6) C43 0.066(8) 0.037(7) 0.032(7) -0.001(5) -0.001(6) 0.005(6) C44 0.088(10) 0.054(8) 0.038(7) 0.001(6) 0.007(7) -0.007(8) C45 0.059(9) 0.068(9) 0.069(10) 0.021(8) 0.002(8) -0.005(7) C46 0.069(10) 0.120(14) 0.073(11) 0.027(10) 0.030(9) 0.026(9) C47 0.054(8) 0.101(12) 0.062(9) 0.028(8) 0.020(7) 0.009(8) C48 0.026(6) 0.040(6) 0.040(7) 0.005(5) -0.002(5) -0.016(5) C49 0.024(5) 0.043(6) 0.039(6) 0.007(5) -0.009(5) -0.019(5) C50 0.030(6) 0.040(6) 0.034(6) -0.010(5) 0.001(5) -0.011(5) C51 0.030(6) 0.039(6) 0.030(6) -0.009(5) 0.003(5) -0.015(5) C52 0.026(5) 0.016(5) 0.026(5) 0.004(4) -0.006(4) -0.006(4) C53 0.035(6) 0.048(7) 0.025(6) 0.009(5) -0.008(5) -0.024(5) C54 0.050(7) 0.049(7) 0.021(5) 0.005(5) -0.002(5) -0.030(6) C55 0.076(9) 0.054(9) 0.047(8) 0.000(7) 0.016(7) -0.026(7) C56 0.089(11) 0.078(11) 0.119(14) -0.037(10) 0.027(10) -0.037(9) C57 0.094(13) 0.050(11) 0.109(16) -0.021(10) 0.019(12) 0.007(9) C58 0.086(12) 0.095(13) 0.106(14) -0.014(11) 0.024(11) -0.005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 1.877(7) . ? Fe1 N2 1.883(7) . ? Fe1 N6 1.965(8) . ? Fe1 N1 1.980(7) . ? Fe1 N4 1.983(7) . ? Fe1 N3 1.983(7) . ? P1 F4 1.513(8) . ? P1 F5 1.544(7) . ? P1 F3 1.576(6) . ? P1 F2 1.582(8) . ? P1 F6 1.606(6) . ? P1 F1 1.611(8) . ? P2 F9 1.584(6) . ? P2 F10 1.591(5) . ? P2 F8 1.596(6) . ? P2 F11 1.597(6) . ? P2 F12 1.606(6) . ? P2 F7 1.608(5) . ? P3 F14 1.560(7) 2 ? P3 F14 1.560(7) . ? P3 F13 1.569(6) . ? P3 F13 1.569(6) 2 ? P3 F15 1.588(6) 2 ? P3 F15 1.588(6) . ? P4 F20 1.578(7) . ? P4 F21 1.579(7) . ? P4 F16 1.595(7) . ? P4 F17 1.595(6) . ? P4 F19 1.598(6) . ? P4 F18 1.610(6) . ? P5 F23 1.572(9) . ? P5 F23 1.572(9) 2_656 ? P5 F22 1.587(8) . ? P5 F22 1.587(8) 2_656 ? P5 F24 1.610(10) . ? P5 F24 1.610(10) 2_656 ? N1 C5 1.359(10) . ? N1 C1 1.365(11) . ? N2 C10 1.355(11) . ? N2 C6 1.355(10) . ? N3 C15 1.347(11) . ? N3 C11 1.363(11) . ? N4 C28 1.346(11) . ? N4 C32 1.369(11) . ? N5 C37 1.342(11) . ? N5 C33 1.347(10) . ? N6 C42 1.343(12) . ? N6 C38 1.378(11) . ? N7 C23 1.339(11) . ? N7 C27 1.340(12) . ? N7 C22 1.501(12) . ? N8 C54 1.339(12) . ? N8 C50 1.342(12) . ? N8 C49 1.503(11) . ? N9 C55 1.119(15) . ? N10 C57 1.16(2) . ? C1 C2 1.379(12) . ? C2 C3 1.383(12) . ? C3 C4 1.381(12) . ? C4 C5 1.381(12) . ? C5 C6 1.473(12) . ? C6 C7 1.379(11) . ? C7 C8 1.392(12) . ? C8 C9 1.400(12) . ? C8 C25 1.470(11) . ? C9 C10 1.377(12) . ? C10 C11 1.469(11) . ? C11 C12 1.389(12) . ? C12 C13 1.392(13) . ? C13 C14 1.379(13) . ? C14 C15 1.384(13) . ? C16 C17 1.39 . ? C16 C21 1.39 . ? C16 C22 1.437(12) . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C23 C24 1.365(12) . ? C24 C25 1.378(11) . ? C25 C26 1.392(12) . ? C26 C27 1.366(12) . ? C28 C29 1.357(12) . ? C29 C30 1.382(13) . ? C30 C31 1.383(13) . ? C31 C32 1.374(12) . ? C32 C33 1.453(12) . ? C33 C34 1.382(11) . ? C34 C35 1.388(12) . ? C35 C36 1.379(12) . ? C35 C52 1.500(12) . ? C36 C37 1.395(12) . ? C37 C38 1.481(13) . ? C38 C39 1.373(14) . ? C39 C40 1.38(2) . ? C40 C41 1.39(2) . ? C41 C42 1.36(2) . ? C43 C48 1.350(14) . ? C43 C44 1.384(15) . ? C44 C45 1.35(2) . ? C45 C46 1.36(2) . ? C46 C47 1.37(2) . ? C47 C48 1.38(2) . ? C48 C49 1.504(13) . ? C50 C51 1.374(13) . ? C51 C52 1.372(13) . ? C52 C53 1.380(12) . ? C53 C54 1.379(13) . ? C55 C56 1.46(2) . ? C57 C58 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Fe1 N2 175.5(3) . . ? N5 Fe1 N6 80.7(3) . . ? N2 Fe1 N6 103.4(3) . . ? N5 Fe1 N1 101.4(3) . . ? N2 Fe1 N1 80.4(3) . . ? N6 Fe1 N1 92.2(3) . . ? N5 Fe1 N4 81.2(3) . . ? N2 Fe1 N4 94.7(3) . . ? N6 Fe1 N4 161.8(3) . . ? N1 Fe1 N4 90.7(3) . . ? N5 Fe1 N3 97.7(3) . . ? N2 Fe1 N3 80.7(3) . . ? N6 Fe1 N3 89.0(3) . . ? N1 Fe1 N3 160.8(3) . . ? N4 Fe1 N3 94.1(3) . . ? F4 P1 F5 95.3(7) . . ? F4 P1 F3 93.1(4) . . ? F5 P1 F3 90.1(4) . . ? F4 P1 F2 93.0(6) . . ? F5 P1 F2 171.3(6) . . ? F3 P1 F2 92.1(4) . . ? F4 P1 F6 88.3(5) . . ? F5 P1 F6 89.5(4) . . ? F3 P1 F6 178.6(4) . . ? F2 P1 F6 88.0(4) . . ? F4 P1 F1 176.7(7) . . ? F5 P1 F1 88.0(6) . . ? F3 P1 F1 86.8(4) . . ? F2 P1 F1 83.7(5) . . ? F6 P1 F1 91.9(4) . . ? F9 P2 F10 91.4(3) . . ? F9 P2 F8 90.4(3) . . ? F10 P2 F8 89.7(3) . . ? F9 P2 F11 90.7(3) . . ? F10 P2 F11 91.1(3) . . ? F8 P2 F11 178.7(3) . . ? F9 P2 F12 178.9(3) . . ? F10 P2 F12 89.5(3) . . ? F8 P2 F12 89.0(3) . . ? F11 P2 F12 89.9(3) . . ? F9 P2 F7 89.7(3) . . ? F10 P2 F7 178.5(3) . . ? F8 P2 F7 89.2(3) . . ? F11 P2 F7 90.0(3) . . ? F12 P2 F7 89.4(3) . . ? F14 P3 F14 180.0 2 . ? F14 P3 F13 89.5(5) 2 . ? F14 P3 F13 90.5(5) . . ? F14 P3 F13 90.5(5) 2 2 ? F14 P3 F13 89.5(5) . 2 ? F13 P3 F13 180.0 . 2 ? F14 P3 F15 89.0(4) 2 2 ? F14 P3 F15 91.0(4) . 2 ? F13 P3 F15 92.1(3) . 2 ? F13 P3 F15 87.9(3) 2 2 ? F14 P3 F15 91.0(4) 2 . ? F14 P3 F15 89.0(4) . . ? F13 P3 F15 87.9(3) . . ? F13 P3 F15 92.1(3) 2 . ? F15 P3 F15 180.0 2 . ? F20 P4 F21 91.7(5) . . ? F20 P4 F16 91.4(4) . . ? F21 P4 F16 90.6(4) . . ? F20 P4 F17 89.3(4) . . ? F21 P4 F17 178.9(4) . . ? F16 P4 F17 89.7(4) . . ? F20 P4 F19 178.1(5) . . ? F21 P4 F19 89.9(4) . . ? F16 P4 F19 89.6(4) . . ? F17 P4 F19 89.0(4) . . ? F20 P4 F18 89.0(4) . . ? F21 P4 F18 89.9(4) . . ? F16 P4 F18 179.3(4) . . ? F17 P4 F18 89.7(4) . . ? F19 P4 F18 90.0(3) . . ? F23 P5 F23 179.999(1) . 2_656 ? F23 P5 F22 88.0(5) . . ? F23 P5 F22 92.0(5) 2_656 . ? F23 P5 F22 92.0(5) . 2_656 ? F23 P5 F22 88.0(5) 2_656 2_656 ? F22 P5 F22 179.998(1) . 2_656 ? F23 P5 F24 90.1(5) . . ? F23 P5 F24 89.9(5) 2_656 . ? F22 P5 F24 88.9(5) . . ? F22 P5 F24 91.1(5) 2_656 . ? F23 P5 F24 89.9(5) . 2_656 ? F23 P5 F24 90.1(5) 2_656 2_656 ? F22 P5 F24 91.1(5) . 2_656 ? F22 P5 F24 88.9(5) 2_656 2_656 ? F24 P5 F24 179.999(2) . 2_656 ? C5 N1 C1 117.6(7) . . ? C5 N1 Fe1 115.5(6) . . ? C1 N1 Fe1 127.0(6) . . ? C10 N2 C6 120.4(7) . . ? C10 N2 Fe1 119.4(5) . . ? C6 N2 Fe1 119.2(6) . . ? C15 N3 C11 118.3(8) . . ? C15 N3 Fe1 126.6(7) . . ? C11 N3 Fe1 114.6(5) . . ? C28 N4 C32 117.3(8) . . ? C28 N4 Fe1 128.9(6) . . ? C32 N4 Fe1 113.7(6) . . ? C37 N5 C33 120.7(7) . . ? C37 N5 Fe1 120.1(6) . . ? C33 N5 Fe1 119.1(6) . . ? C42 N6 C38 116.7(9) . . ? C42 N6 Fe1 127.6(7) . . ? C38 N6 Fe1 115.7(6) . . ? C23 N7 C27 120.9(8) . . ? C23 N7 C22 118.7(8) . . ? C27 N7 C22 120.4(8) . . ? C54 N8 C50 121.6(8) . . ? C54 N8 C49 120.9(8) . . ? C50 N8 C49 117.5(8) . . ? N1 C1 C2 121.9(8) . . ? C1 C2 C3 119.8(8) . . ? C4 C3 C2 119.0(8) . . ? C5 C4 C3 119.1(8) . . ? N1 C5 C4 122.7(8) . . ? N1 C5 C6 112.5(7) . . ? C4 C5 C6 124.8(8) . . ? N2 C6 C7 120.5(8) . . ? N2 C6 C5 111.6(7) . . ? C7 C6 C5 127.9(8) . . ? C6 C7 C8 120.0(8) . . ? C7 C8 C9 118.5(8) . . ? C7 C8 C25 120.0(7) . . ? C9 C8 C25 121.5(8) . . ? C10 C9 C8 119.4(8) . . ? N2 C10 C9 121.1(8) . . ? N2 C10 C11 111.2(7) . . ? C9 C10 C11 127.7(8) . . ? N3 C11 C12 122.4(8) . . ? N3 C11 C10 113.3(8) . . ? C12 C11 C10 124.4(8) . . ? C11 C12 C13 117.9(9) . . ? C14 C13 C12 120.3(9) . . ? C13 C14 C15 118.6(9) . . ? N3 C15 C14 122.5(9) . . ? C17 C16 C21 120.0 . . ? C17 C16 C22 130.5(9) . . ? C21 C16 C22 109.5(9) . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C16 120.0 . . ? C16 C22 N7 115.8(9) . . ? N7 C23 C24 120.3(8) . . ? C23 C24 C25 120.8(8) . . ? C24 C25 C26 117.2(8) . . ? C24 C25 C8 121.9(7) . . ? C26 C25 C8 120.9(7) . . ? C27 C26 C25 120.5(9) . . ? N7 C27 C26 120.2(8) . . ? N4 C28 C29 123.6(8) . . ? C28 C29 C30 119.5(9) . . ? C29 C30 C31 118.0(9) . . ? C32 C31 C30 120.3(9) . . ? N4 C32 C31 121.2(8) . . ? N4 C32 C33 113.6(8) . . ? C31 C32 C33 125.2(8) . . ? N5 C33 C34 121.1(8) . . ? N5 C33 C32 112.2(7) . . ? C34 C33 C32 126.6(8) . . ? C33 C34 C35 118.4(8) . . ? C36 C35 C34 120.5(8) . . ? C36 C35 C52 120.6(8) . . ? C34 C35 C52 118.8(8) . . ? C35 C36 C37 118.3(9) . . ? N5 C37 C36 120.9(8) . . ? N5 C37 C38 111.9(8) . . ? C36 C37 C38 127.2(9) . . ? C39 C38 N6 122.9(9) . . ? C39 C38 C37 125.4(9) . . ? N6 C38 C37 111.6(8) . . ? C38 C39 C40 118.7(10) . . ? C39 C40 C41 118.8(11) . . ? C42 C41 C40 119.6(11) . . ? N6 C42 C41 123.2(10) . . ? C48 C43 C44 121.5(11) . . ? C45 C44 C43 120.4(12) . . ? C44 C45 C46 118.6(12) . . ? C45 C46 C47 121.3(14) . . ? C46 C47 C48 120.3(13) . . ? C43 C48 C47 117.6(10) . . ? C43 C48 C49 121.4(10) . . ? C47 C48 C49 120.6(10) . . ? N8 C49 C48 110.6(7) . . ? N8 C50 C51 119.2(10) . . ? C52 C51 C50 121.2(9) . . ? C51 C52 C53 118.0(8) . . ? C51 C52 C35 120.5(8) . . ? C53 C52 C35 121.5(9) . . ? C54 C53 C52 120.0(10) . . ? N8 C54 C53 120.0(9) . . ? N9 C55 C56 178.4(15) . . ? N10 C57 C58 177.0(24) . . ? _refine_diff_density_max 1.427 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.097 data_CompoundI _audit_creation_date 99-09-07 _audit_creation_method CRYSTALS #========================================================================== _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 11.1385(3) _cell_angle_alpha 90 _cell_length_b 11.4375(5) _cell_angle_beta 90 _cell_length_c 12.1929(5) _cell_angle_gamma 90 _cell_volume 1553.34 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c n ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y,z+1/2' '-x,y,-z+1/2' '-x+1/2,-y+1/2,z+1/2' 'x+1/2,y+1/2,-z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C20 H14 N4 ' _chemical_formula_moiety ' C20 H14 N4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 310.36 _cell_measurement_reflns_used 33912 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _cell_measurement_temperature 293 _cell_formula_units_Z 4 _exptl_crystal_description ' box ' _exptl_crystal_colour ' none ' _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.33 _exptl_crystal_density_meas ? _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.08 _exptl_absorpt_correction_type NONE _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 2588 _reflns_number_total 1361 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_observed 1202 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.44 _refine_diff_density_max 0.41 _refine_ls_number_reflns 1202 _refine_ls_number_parameters 112 _refine_ls_R_factor_obs 0.0532 _refine_ls_wR_factor_obs 0.0447 _refine_ls_goodness_of_fit_obs 0.8204 _refine_ls_shift/esd_max 0.000233 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _diffrn_measurement_method CCD # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 0.18708(9) 0.44821(9) 0.01442(9) 0.0470 1.0000 Uani C1 0.2471(1) 0.3856(1) -0.0605(1) 0.0554 1.0000 Uani C2 0.2390(1) 0.2660(1) -0.0704(1) 0.0554 1.0000 Uani C3 0.1625(1) 0.2079(1) -0.0014(1) 0.0538 1.0000 Uani C4 0.0994(1) 0.2690(1) 0.0776(1) 0.0462 1.0000 Uani C5 0.1154(1) 0.3902(1) 0.08354(9) 0.0377 1.0000 Uani N2 0.0000 0.4003(1) 0.2500 0.0393 1.0000 Uani C6 0.0549(1) 0.4607(1) 0.17005(9) 0.0368 1.0000 Uani C7 0.0574(1) 0.5827(1) 0.1674(1) 0.0380 1.0000 Uani C8 0.0000 0.6453(1) 0.2500 0.0358 1.0000 Uani C9 0.0000 0.7760(1) 0.2500 0.0352 1.0000 Uani C10 0.0902(1) 0.8396(1) 0.1994(1) 0.0434 1.0000 Uani C11 0.0867(1) 0.9605(1) 0.2021(1) 0.0502 1.0000 Uani N3 0.0000 1.0225(1) 0.2500 0.0532 1.0000 Uani H11 0.2989 0.4266 -0.1102 0.0551 1.0000 Uiso H21 0.2855 0.2246 -0.1241 0.0552 1.0000 Uiso H31 0.1527 0.1248 -0.0078 0.0528 1.0000 Uiso H41 0.0460 0.2294 0.1270 0.0457 1.0000 Uiso H71 0.0982 0.6230 0.1092 0.0378 1.0000 Uiso H101 0.1547 0.8000 0.1627 0.0431 1.0000 Uiso H111 0.1508 1.0024 0.1673 0.0493 1.0000 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0479(6) 0.0461(6) 0.0469(6) -0.0063(5) 0.0046(5) -0.0053(5) C1 0.0520(8) 0.0648(9) 0.0496(7) -0.0099(7) 0.0076(6) -0.0072(7) C2 0.0539(8) 0.063(1) 0.0496(7) -0.0184(6) -0.0030(6) 0.0089(7) C3 0.0622(9) 0.0395(7) 0.0599(8) -0.0116(6) -0.0098(7) 0.0098(6) C4 0.0494(7) 0.0373(7) 0.0518(8) -0.0013(5) -0.0005(6) 0.0021(5) C5 0.0346(6) 0.0362(7) 0.0422(6) -0.0026(5) -0.0034(5) 0.0014(5) N2 0.0377(7) 0.0331(7) 0.0470(8) 0.0000 0.0010(6) 0.0000 C6 0.0326(5) 0.0347(6) 0.0432(7) -0.0016(5) -0.0031(5) 0.0002(4) C7 0.0356(6) 0.0341(6) 0.0444(7) 0.0013(5) 0.0009(5) -0.0011(5) C8 0.0319(8) 0.0322(9) 0.0434(9) 0.0000 -0.0043(7) 0.0000 C9 0.0353(8) 0.0316(8) 0.0387(8) 0.0000 -0.0039(7) 0.0000 C10 0.0441(7) 0.0367(7) 0.0495(7) -0.0010(5) 0.0078(6) 0.0016(5) C11 0.0555(8) 0.0374(7) 0.0576(8) 0.0030(6) 0.0144(6) -0.0057(6) N3 0.063(1) 0.0329(9) 0.064(1) 0.0000 0.0124(9) 0.0000 _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.339(2) yes N1 . C5 . 1.337(2) yes C1 . C2 . 1.376(2) yes C1 . H11 . 0.960(1) no C2 . C3 . 1.370(2) yes C2 . H21 . 0.960(1) no C3 . C4 . 1.382(2) yes C3 . H31 . 0.960(1) no C4 . C5 . 1.399(2) yes C4 . H41 . 0.960(1) no C5 . C6 . 1.489(2) yes N2 . C6 . 1.342(1) yes N2 . C6 6_555 1.342(1) yes C6 . C7 . 1.397(2) yes C7 . C8 . 1.392(1) yes C7 . H71 . 0.960(1) no C8 . C9 . 1.494(2) yes C9 . C10 . 1.385(1) yes C9 . C10 6_555 1.385(1) yes C10 . C11 . 1.384(2) yes C10 . H101 . 0.960(1) no C11 . N3 . 1.332(2) yes C11 . H111 . 0.960(1) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C5 . 117.5(1) no N1 . C1 . C2 . 124.0(1) no N1 . C1 . H11 . 118.0(1) no C2 . C1 . H11 . 118.0(1) no C1 . C2 . C3 . 117.9(1) no C1 . C2 . H21 . 121.0(2) no C3 . C2 . H21 . 121.0(1) no C2 . C3 . C4 . 120.0(1) no C2 . C3 . H31 . 120.0(1) no C4 . C3 . H31 . 120.0(1) no C3 . C4 . C5 . 118.2(1) no C3 . C4 . H41 . 120.9(1) no C5 . C4 . H41 . 120.9(1) no N1 . C5 . C4 . 122.4(1) no N1 . C5 . C6 . 116.6(1) no C4 . C5 . C6 . 121.0(1) no C6 . N2 . C6 6_555 118.1(1) no C5 . C6 . N2 . 116.2(1) no C5 . C6 . C7 . 121.0(1) no N2 . C6 . C7 . 122.7(1) no C6 . C7 . C8 . 119.2(1) no C6 . C7 . H71 . 120.4(1) no C8 . C7 . H71 . 120.4(1) no C7 . C8 . C7 6_555 118.1(1) no C7 . C8 . C9 . 120.96(7) no C7 6_555 C8 . C9 . 120.96(7) no C8 . C9 . C10 . 121.67(7) no C8 . C9 . C10 6_555 121.67(7) no C10 . C9 . C10 6_555 116.7(1) no C9 . C10 . C11 . 119.6(1) no C9 . C10 . H101 . 120.2(1) no C11 . C10 . H101 . 120.2(1) no C10 . C11 . N3 . 124.2(1) no C10 . C11 . H111 . 117.9(1) no N3 . C11 . H111 . 117.9(1) no C11 . N3 . C11 6_555 115.7(1) no data_es133 _audit_creation_date 99-10-06 _audit_creation_method CRYSTALS # measured as: es_lig_pf6 #========================================================================== _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 10.1186(3) _cell_length_b 10.4515(2) _cell_length_c 13.5992(5) _cell_angle_alpha 110.415(2) _cell_angle_beta 94.794(2) _cell_angle_gamma 107.592(2) _cell_volume 1255.74 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C27 H21 N4 P1 F6 ' _chemical_formula_moiety ' C27 H21 N4 * PF6 ' _chemical_compound_source ; ? ; _chemical_formula_weight 546.45 _cell_measurement_reflns_used 12145 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _cell_measurement_temperature 293 _cell_formula_units_Z 2 _exptl_crystal_description ' box ' _exptl_crystal_colour ' none ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas ? _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.17 _exptl_absorpt_correction_type NONE _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 12145 _reflns_number_total 4400 _diffrn_reflns_av_R_equivalents 0.00 _reflns_number_observed 3180 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -12 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.46 _refine_diff_density_max 0.37 _refine_ls_number_reflns 3180 _refine_ls_number_parameters 344 _refine_ls_R_factor_obs 0.0623 _refine_ls_wR_factor_obs 0.0812 _refine_ls_goodness_of_fit_obs 0.9290 _refine_ls_shift/esd_max 0.003702 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _diffrn_measurement_method 'CCD' # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 0.0799(3) 0.2924(3) 0.6521(2) 0.0684 1.0000 Uani C1 0.0222(4) 0.3611(4) 0.7296(3) 0.0819 1.0000 Uani C2 -0.0111(4) 0.3171(4) 0.8123(3) 0.0860 1.0000 Uani C3 0.0163(4) 0.1986(4) 0.8164(2) 0.0795 1.0000 Uani C4 0.0767(3) 0.1262(3) 0.7383(2) 0.0655 1.0000 Uani C5 0.1056(3) 0.1754(3) 0.6565(2) 0.0560 1.0000 Uani N2 0.1941(2) -0.0164(2) 0.5735(2) 0.0553 1.0000 Uani C6 0.1688(3) 0.1002(3) 0.5694(2) 0.0508 1.0000 Uani C7 0.1980(3) 0.1491(3) 0.4878(2) 0.0514 1.0000 Uani C8 0.2630(2) 0.0797(3) 0.4111(2) 0.0486 1.0000 Uani C9 0.2933(3) -0.0385(3) 0.4170(2) 0.0518 1.0000 Uani C10 0.2538(3) -0.0857(3) 0.4975(2) 0.0528 1.0000 Uani N3 0.3610(3) -0.2667(3) 0.4402(2) 0.0730 1.0000 Uani C11 0.2751(3) -0.2186(3) 0.5012(2) 0.0579 1.0000 Uani C12 0.2095(4) -0.2866(3) 0.5642(3) 0.0727 1.0000 Uani C13 0.2335(5) -0.4103(4) 0.5636(3) 0.0881 1.0000 Uani C14 0.3215(5) -0.4593(4) 0.5022(3) 0.0894 1.0000 Uani C15 0.3833(5) -0.3855(4) 0.4415(3) 0.0887 1.0000 Uani C16 0.3001(2) 0.1300(3) 0.3240(2) 0.0479 1.0000 Uani C17 0.4216(3) 0.1227(3) 0.2860(2) 0.0583 1.0000 Uani C18 0.4564(3) 0.1705(3) 0.2065(2) 0.0632 1.0000 Uani N4 0.3730(3) 0.2242(2) 0.1637(2) 0.0585 1.0000 Uani C19 0.2531(3) 0.2304(3) 0.1972(2) 0.0624 1.0000 Uani C20 0.2150(3) 0.1849(3) 0.2776(2) 0.0573 1.0000 Uani C21 0.4139(4) 0.2752(4) 0.0762(2) 0.0730 1.0000 Uani C22 0.4146(3) 0.4273(3) 0.1008(2) 0.0550 1.0000 Uani C23 0.3127(3) 0.4504(4) 0.0437(2) 0.0686 1.0000 Uani C24 0.3126(4) 0.5882(5) 0.0622(3) 0.0844 1.0000 Uani C25 0.4150(5) 0.7050(4) 0.1399(3) 0.0888 1.0000 Uani C26 0.5176(5) 0.6871(4) 0.1981(3) 0.0971 1.0000 Uani C27 0.5200(3) 0.5473(4) 0.1784(3) 0.0780 1.0000 Uani P1 0.16879(9) -0.17002(9) -0.10139(6) 0.0672 1.0000 Uani F1 0.2368(2) -0.2916(2) -0.1455(2) 0.0928 1.0000 Uani F2 0.1026(3) -0.0479(3) -0.0608(3) 0.1433 1.0000 Uani F3 0.2812(3) -0.0673(3) -0.1411(3) 0.1299 1.0000 Uani F4 0.2703(5) -0.1059(4) 0.0096(3) 0.1698 1.0000 Uani F5 0.0540(3) -0.2755(3) -0.0670(2) 0.1337 1.0000 Uani F6 0.0651(3) -0.2394(4) -0.2153(2) 0.1241 1.0000 Uani H11 0.0030 0.4449 0.7277 0.0767 1.0000 Uiso H21 -0.0530 0.3691 0.8660 0.0742 1.0000 Uiso H31 -0.0061 0.1663 0.8730 0.0698 1.0000 Uiso H41 0.0984 0.0437 0.7401 0.0614 1.0000 Uiso H71 0.1735 0.2297 0.4847 0.0518 1.0000 Uiso H91 0.3409 -0.0870 0.3664 0.0528 1.0000 Uiso H121 0.1489 -0.2488 0.6073 0.0767 1.0000 Uiso H131 0.1889 -0.4607 0.6058 0.0903 1.0000 Uiso H141 0.3403 -0.5444 0.5011 0.0881 1.0000 Uiso H151 0.4449 -0.4213 0.3984 0.0937 1.0000 Uiso H171 0.4818 0.0838 0.3157 0.0630 1.0000 Uiso H181 0.5412 0.1656 0.1811 0.0708 1.0000 Uiso H191 0.1933 0.2669 0.1646 0.0703 1.0000 Uiso H201 0.1297 0.1911 0.3016 0.0631 1.0000 Uiso H211 0.5070 0.2741 0.0686 0.0820 1.0000 Uiso H212 0.3471 0.2099 0.0101 0.0820 1.0000 Uiso H231 0.2391 0.3679 -0.0109 0.0688 1.0000 Uiso H241 0.2405 0.6016 0.0205 0.0983 1.0000 Uiso H251 0.4147 0.8014 0.1536 0.0974 1.0000 Uiso H261 0.5892 0.7708 0.2534 0.0845 1.0000 Uiso H271 0.5945 0.5349 0.2185 0.0767 1.0000 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.074(2) 0.061(1) 0.066(1) 0.017(1) 0.027(1) 0.025(1) C1 0.082(2) 0.073(2) 0.075(2) 0.009(2) 0.026(2) 0.028(2) C2 0.074(2) 0.091(2) 0.061(2) -0.001(2) 0.027(2) 0.018(2) C3 0.071(2) 0.092(2) 0.052(2) 0.015(2) 0.024(1) 0.011(2) C4 0.063(2) 0.070(2) 0.052(1) 0.020(1) 0.018(1) 0.012(1) C5 0.053(1) 0.057(1) 0.045(1) 0.013(1) 0.014(1) 0.010(1) N2 0.063(1) 0.055(1) 0.045(1) 0.0203(9) 0.015(1) 0.016(1) C6 0.052(1) 0.050(1) 0.045(1) 0.018(1) 0.013(1) 0.012(1) C7 0.052(1) 0.054(1) 0.050(1) 0.022(1) 0.016(1) 0.017(1) C8 0.046(1) 0.055(1) 0.045(1) 0.023(1) 0.012(1) 0.014(1) C9 0.054(1) 0.059(1) 0.046(1) 0.023(1) 0.015(1) 0.021(1) C10 0.059(1) 0.055(1) 0.045(1) 0.021(1) 0.012(1) 0.017(1) N3 0.099(2) 0.066(1) 0.068(1) 0.031(1) 0.031(1) 0.039(1) C11 0.068(2) 0.057(1) 0.048(1) 0.022(1) 0.011(1) 0.019(1) C12 0.090(2) 0.068(2) 0.074(2) 0.040(2) 0.030(2) 0.029(2) C13 0.113(3) 0.072(2) 0.091(2) 0.050(2) 0.030(2) 0.025(2) C14 0.125(3) 0.059(2) 0.092(2) 0.034(2) 0.027(2) 0.038(2) C15 0.125(3) 0.074(2) 0.089(2) 0.037(2) 0.045(2) 0.054(2) C16 0.048(1) 0.053(1) 0.047(1) 0.023(1) 0.014(1) 0.017(1) C17 0.053(1) 0.075(2) 0.063(2) 0.037(1) 0.023(1) 0.030(1) C18 0.064(2) 0.077(2) 0.072(2) 0.041(1) 0.036(1) 0.037(1) N4 0.070(1) 0.066(1) 0.058(1) 0.035(1) 0.033(1) 0.031(1) C19 0.062(2) 0.080(2) 0.070(2) 0.047(1) 0.025(1) 0.036(1) C20 0.053(1) 0.073(2) 0.065(2) 0.040(1) 0.028(1) 0.029(1) C21 0.103(2) 0.081(2) 0.066(2) 0.046(2) 0.048(2) 0.046(2) C22 0.058(1) 0.067(2) 0.051(1) 0.032(1) 0.023(1) 0.023(1) C23 0.061(2) 0.083(2) 0.064(2) 0.040(2) 0.009(1) 0.017(1) C24 0.089(2) 0.115(3) 0.092(2) 0.068(2) 0.037(2) 0.059(2) C25 0.124(3) 0.084(2) 0.089(2) 0.047(2) 0.056(3) 0.054(2) C26 0.104(3) 0.074(2) 0.078(2) 0.012(2) 0.019(2) 0.005(2) C27 0.066(2) 0.098(2) 0.070(2) 0.035(2) 0.010(2) 0.027(2) P1 0.0700(5) 0.0817(6) 0.0665(5) 0.0335(4) 0.0254(4) 0.0417(4) F1 0.079(1) 0.083(1) 0.130(2) 0.042(1) 0.031(1) 0.045(1) F2 0.152(2) 0.137(2) 0.180(3) 0.050(2) 0.084(2) 0.105(2) F3 0.124(2) 0.108(2) 0.212(3) 0.096(2) 0.092(2) 0.061(2) F4 0.209(4) 0.137(2) 0.106(2) 0.005(2) -0.058(2) 0.059(2) F5 0.144(2) 0.138(2) 0.128(2) 0.063(2) 0.083(2) 0.036(2) F6 0.120(2) 0.181(3) 0.087(2) 0.050(2) 0.009(1) 0.082(2) _refine_ls_extinction_coef 316.4(620) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.339(4) yes N1 . C5 . 1.345(4) yes C1 . C2 . 1.386(5) yes C1 . H11 . 0.960(4) no C2 . C3 . 1.367(6) yes C2 . H21 . 0.960(3) no C3 . C4 . 1.379(5) yes C3 . H31 . 0.960(3) no C4 . C5 . 1.396(4) yes C4 . H41 . 0.960(3) no C5 . C6 . 1.487(4) yes N2 . C6 . 1.337(3) yes N2 . C10 . 1.344(3) yes C6 . C7 . 1.393(3) yes C7 . C8 . 1.387(4) yes C7 . H71 . 0.960(3) no C8 . C9 . 1.386(4) yes C8 . C16 . 1.487(3) yes C9 . C10 . 1.389(3) yes C9 . H91 . 0.960(2) no C10 . C11 . 1.486(4) yes N3 . C11 . 1.339(4) yes N3 . C15 . 1.333(4) yes C11 . C12 . 1.383(4) yes C12 . C13 . 1.383(5) yes C12 . H121 . 0.960(3) no C13 . C14 . 1.362(6) yes C13 . H131 . 0.960(3) no C14 . C15 . 1.380(5) yes C14 . H141 . 0.960(3) no C15 . H151 . 0.960(4) no C16 . C17 . 1.385(3) yes C16 . C20 . 1.389(4) yes C17 . C18 . 1.372(4) yes C17 . H171 . 0.960(3) no C18 . N4 . 1.340(4) yes C18 . H181 . 0.960(3) no N4 . C19 . 1.342(4) yes N4 . C21 . 1.504(3) yes C19 . C20 . 1.376(4) yes C19 . H191 . 0.960(3) no C20 . H201 . 0.960(2) no C21 . C22 . 1.503(4) yes C21 . H211 . 0.960(3) no C21 . H212 . 0.960(4) no C22 . C23 . 1.368(4) yes C22 . C27 . 1.380(4) yes C23 . C24 . 1.372(5) yes C23 . H231 . 0.960(3) no C24 . C25 . 1.354(6) yes C24 . H241 . 0.960(3) no C25 . C26 . 1.350(6) yes C25 . H251 . 0.960(4) no C26 . C27 . 1.399(6) yes C26 . H261 . 0.960(4) no C27 . H271 . 0.960(3) no P1 . F1 . 1.586(2) yes P1 . F2 . 1.571(2) yes P1 . F3 . 1.584(2) yes P1 . F4 . 1.550(3) yes P1 . F5 . 1.569(2) yes P1 . F6 . 1.584(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C5 . 117.3(3) no N1 . C1 . C2 . 123.1(3) no N1 . C1 . H11 . 118.4(4) no C2 . C1 . H11 . 118.4(3) no C1 . C2 . C3 . 119.2(3) no C1 . C2 . H21 . 120.4(4) no C3 . C2 . H21 . 120.4(4) no C2 . C3 . C4 . 119.1(3) no C2 . C3 . H31 . 120.4(3) no C4 . C3 . H31 . 120.4(4) no C3 . C4 . C5 . 118.6(3) no C3 . C4 . H41 . 120.7(3) no C5 . C4 . H41 . 120.7(3) no N1 . C5 . C4 . 122.7(3) no N1 . C5 . C6 . 116.4(2) no C4 . C5 . C6 . 120.9(3) no C6 . N2 . C10 . 118.3(2) no C5 . C6 . N2 . 116.5(2) no C5 . C6 . C7 . 121.1(2) no N2 . C6 . C7 . 122.5(2) no C6 . C7 . C8 . 119.0(2) no C6 . C7 . H71 . 120.5(2) no C8 . C7 . H71 . 120.5(2) no C7 . C8 . C9 . 118.6(2) no C7 . C8 . C16 . 121.2(2) no C9 . C8 . C16 . 120.2(2) no C8 . C9 . C10 . 118.9(2) no C8 . C9 . H91 . 120.5(2) no C10 . C9 . H91 . 120.5(2) no N2 . C10 . C9 . 122.6(2) no N2 . C10 . C11 . 117.1(2) no C9 . C10 . C11 . 120.3(2) no C11 . N3 . C15 . 117.4(3) no C10 . C11 . N3 . 115.5(2) no C10 . C11 . C12 . 121.4(3) no N3 . C11 . C12 . 123.0(3) no C11 . C12 . C13 . 118.4(3) no C11 . C12 . H121 . 120.8(3) no C13 . C12 . H121 . 120.8(3) no C12 . C13 . C14 . 118.9(3) no C12 . C13 . H131 . 120.6(4) no C14 . C13 . H131 . 120.6(4) no C13 . C14 . C15 . 119.4(3) no C13 . C14 . H141 . 120.3(4) no C15 . C14 . H141 . 120.3(4) no N3 . C15 . C14 . 122.9(3) no N3 . C15 . H151 . 118.6(3) no C14 . C15 . H151 . 118.6(3) no C8 . C16 . C17 . 120.5(2) no C8 . C16 . C20 . 121.7(2) no C17 . C16 . C20 . 117.8(2) no C16 . C17 . C18 . 120.4(2) no C16 . C17 . H171 . 119.8(2) no C18 . C17 . H171 . 119.8(3) no C17 . C18 . N4 . 120.6(2) no C17 . C18 . H181 . 119.7(3) no N4 . C18 . H181 . 119.7(3) no C18 . N4 . C19 . 120.5(2) no C18 . N4 . C21 . 119.2(2) no C19 . N4 . C21 . 120.2(2) no N4 . C19 . C20 . 120.8(2) no N4 . C19 . H191 . 119.6(3) no C20 . C19 . H191 . 119.6(3) no C16 . C20 . C19 . 119.9(2) no C16 . C20 . H201 . 120.1(2) no C19 . C20 . H201 . 120.1(3) no N4 . C21 . C22 . 111.8(2) no N4 . C21 . H211 . 108.9(3) no C22 . C21 . H211 . 108.9(3) no N4 . C21 . H212 . 108.9(3) no C22 . C21 . H212 . 108.9(3) no H211 . C21 . H212 . 109.5(3) no C21 . C22 . C23 . 120.5(3) no C21 . C22 . C27 . 121.3(3) no C23 . C22 . C27 . 118.2(3) no C22 . C23 . C24 . 121.9(3) no C22 . C23 . H231 . 119.0(3) no C24 . C23 . H231 . 119.0(3) no C23 . C24 . C25 . 119.4(3) no C23 . C24 . H241 . 120.3(4) no C25 . C24 . H241 . 120.3(4) no C24 . C25 . C26 . 120.7(3) no C24 . C25 . H251 . 119.7(5) no C26 . C25 . H251 . 119.7(5) no C25 . C26 . C27 . 120.3(3) no C25 . C26 . H261 . 119.8(5) no C27 . C26 . H261 . 119.8(5) no C22 . C27 . C26 . 119.5(3) no C22 . C27 . H271 . 120.2(4) no C26 . C27 . H271 . 120.2(4) no F1 . P1 . F2 . 178.1(2) no F1 . P1 . F3 . 89.3(1) no F2 . P1 . F3 . 89.1(2) no F1 . P1 . F4 . 90.5(2) no F2 . P1 . F4 . 90.6(2) no F3 . P1 . F4 . 90.6(2) no F1 . P1 . F5 . 90.1(1) no F2 . P1 . F5 . 91.5(2) no F3 . P1 . F5 . 177.6(2) no F4 . P1 . F5 . 91.7(2) no F1 . P1 . F6 . 88.3(1) no F2 . P1 . F6 . 90.7(2) no F3 . P1 . F6 . 90.1(2) no F4 . P1 . F6 . 178.6(2) no F5 . P1 . F6 . 87.6(2) no