# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email voloshin@ineos.ac.ru _publ_contact_author_name 'Yan Voloshin' loop_ _publ_author_name 'Yan Voloshin' 'Alexander Belov' 'Oleg Varzatskii' "Sergey Shul'ga" 'Pavel Stuzhin' 'Zoya Starikova' 'Ekaterina Lebed' 'Yurii Bubnov' data_hhh _database_code_depnum_ccdc_archive 'CCDC 816071' #TrackingRef '- CN_clathrochelate_fin.CIF' _vrf_PLAT026_hhh ; PROBLEM:Ratio Observed / Unique Reflections too Low 34 Perc. RESPONSE: The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT220_hhh ; PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) 10.0 Ratio RESPONSE:this is related to impossibility to correctly take into account thermal motion. The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT250_hhh ; PROBLEM:Large U3/U1 Ratio for Average U(i,j) Tensor RESPONSE:this is related to impossibility to correctly take into account thermal motion motion. The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT332_hhh ; PROBLEM:Large Phenyl C-C Range C1S -C6S 0.31 Ang. RESPONSE:this is related to impossibility to correctly take into account thermal motion motion. The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT341_hhh ; PROBLEM:Low Bond Precision on C-C Bonds 0.0159 Ang RESPONSE:this is related to impossibility to correctly take into account thermal motion motion. The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H21 B2 F2 Fe N7 O6, 2.5(C6 H6)' _chemical_formula_sum 'C46 H36 B2 F2 Fe N7 O6' _chemical_formula_weight 898.29 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.500(3) _cell_length_b 16.552(3) _cell_length_c 18.284(3) _cell_angle_alpha 107.773(4) _cell_angle_beta 110.392(3) _cell_angle_gamma 96.086(4) _cell_volume 4329.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 460 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1862 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34537 _diffrn_reflns_av_R_equivalents 0.1690 _diffrn_reflns_av_sigmaI/netI 0.2749 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15131 _reflns_number_gt 5142 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+3.8500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15131 _refine_ls_number_parameters 1151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2381 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1A Fe 0.22052(7) 0.25827(6) 0.25782(7) 0.0296(3) Uani 1 1 d . . . F1A F 0.3907(3) 0.3478(2) 0.5235(3) 0.0446(12) Uani 1 1 d . . . F2A F 0.0510(3) 0.1691(2) -0.0079(3) 0.0419(11) Uani 1 1 d . . . B1A B 0.3352(7) 0.3168(6) 0.4404(6) 0.039(2) Uani 1 1 d . . . B2A B 0.1057(6) 0.1988(5) 0.0755(6) 0.029(2) Uani 1 1 d . . . N1A N 0.2832(4) 0.3747(4) 0.3309(4) 0.0295(15) Uani 1 1 d . . . N2A N 0.1595(4) 0.3256(4) 0.1969(4) 0.0292(15) Uani 1 1 d . . . N3A N 0.1876(4) 0.2465(4) 0.3465(4) 0.0369(17) Uani 1 1 d . . . N4A N 0.1122(4) 0.1688(4) 0.1963(4) 0.0348(16) Uani 1 1 d . . . N5A N 0.3258(4) 0.2283(4) 0.3096(4) 0.0338(16) Uani 1 1 d . . . N6A N 0.2509(4) 0.2112(3) 0.1657(4) 0.0313(16) Uani 1 1 d . . . N7A N 0.5226(7) 0.1647(6) 0.3144(7) 0.021(3) Uiso 0.50 1 d P . . N8A N 0.3781(7) 0.1132(7) 0.0669(8) 0.034(3) Uiso 0.50 1 d P . . O1A O 0.3434(3) 0.3961(3) 0.4140(3) 0.0368(13) Uani 1 1 d . . . O2A O 0.0993(3) 0.2892(3) 0.1146(3) 0.0325(13) Uani 1 1 d . . . O3A O 0.2465(3) 0.2848(3) 0.4295(3) 0.0373(14) Uani 1 1 d . . . O4A O 0.0676(3) 0.1390(3) 0.1097(3) 0.0366(13) Uani 1 1 d . . . O5A O 0.3723(3) 0.2500(3) 0.3948(3) 0.0381(13) Uani 1 1 d . . . O6A O 0.1957(3) 0.1937(3) 0.0840(3) 0.0354(13) Uani 1 1 d . . . C1A C 0.2584(5) 0.4413(4) 0.3122(5) 0.0274(18) Uani 1 1 d . . . C2A C 0.1876(5) 0.4096(4) 0.2281(5) 0.0264(18) Uani 1 1 d . . . C3A C 0.1186(5) 0.1869(4) 0.3265(5) 0.033(2) Uani 1 1 d . . . C4A C 0.0654(5) 0.1470(4) 0.2366(5) 0.033(2) Uani 1 1 d . . . C5A C 0.3712(5) 0.1969(4) 0.2629(6) 0.043(2) Uani 1 1 d . . . H5A H 0.4282 0.1842 0.2853 0.052 Uiso 0.50 1 d PR . . C6A C 0.3246(5) 0.1843(5) 0.1773(5) 0.0331(19) Uani 1 1 d . . . H6A H 0.3396 0.1527 0.1285 0.040 Uiso 0.50 1 d PR . . C7A C 0.2900(5) 0.5334(4) 0.3688(4) 0.0229(17) Uani 1 1 d . . . C8A C 0.2299(5) 0.5807(4) 0.3804(5) 0.034(2) Uani 1 1 d . . . H8AA H 0.1681 0.5550 0.3484 0.041 Uiso 1 1 calc R . . C9A C 0.2571(5) 0.6657(5) 0.4381(5) 0.037(2) Uani 1 1 d . . . H9AA H 0.2143 0.6977 0.4460 0.045 Uiso 1 1 calc R . . C10A C 0.3462(6) 0.7032(5) 0.4837(5) 0.039(2) Uani 1 1 d . . . H10A H 0.3651 0.7609 0.5243 0.047 Uiso 1 1 calc R . . C11A C 0.4086(6) 0.6580(5) 0.4710(5) 0.040(2) Uani 1 1 d . . . H11A H 0.4703 0.6853 0.5012 0.048 Uiso 1 1 calc R . . C12A C 0.3812(5) 0.5716(5) 0.4134(5) 0.0330(19) Uani 1 1 d . . . H12A H 0.4237 0.5397 0.4048 0.040 Uiso 1 1 calc R . . C13A C 0.1601(5) 0.4686(4) 0.1811(5) 0.0316(19) Uani 1 1 d . . . C14A C 0.2214(6) 0.5169(5) 0.1667(5) 0.050(2) Uani 1 1 d . . . H14A H 0.2819 0.5135 0.1873 0.060 Uiso 1 1 calc R . . C15A C 0.1952(8) 0.5715(5) 0.1215(6) 0.066(3) Uani 1 1 d . . . H15A H 0.2376 0.6048 0.1111 0.079 Uiso 1 1 calc R . . C16A C 0.1108(8) 0.5763(5) 0.0933(6) 0.068(3) Uani 1 1 d . . . H16A H 0.0932 0.6123 0.0617 0.082 Uiso 1 1 calc R . . C17A C 0.0467(6) 0.5293(6) 0.1092(6) 0.068(3) Uani 1 1 d . . . H17A H -0.0130 0.5354 0.0911 0.081 Uiso 1 1 calc R . . C18A C 0.0731(6) 0.4736(5) 0.1521(5) 0.050(2) Uani 1 1 d . . . H18A H 0.0305 0.4390 0.1611 0.060 Uiso 1 1 calc R . . C19A C 0.1013(5) 0.1528(5) 0.3876(5) 0.045(2) Uani 1 1 d . . . C20A C 0.1168(6) 0.2091(5) 0.4685(6) 0.066(3) Uani 1 1 d . . . H20A H 0.1351 0.2705 0.4848 0.079 Uiso 1 1 calc R . . C21A C 0.1044(7) 0.1720(7) 0.5249(6) 0.083(3) Uani 1 1 d . . . H21A H 0.1135 0.2090 0.5797 0.099 Uiso 1 1 calc R . . C22A C 0.0797(6) 0.0841(7) 0.5017(7) 0.072(3) Uani 1 1 d . . . H22A H 0.0729 0.0608 0.5413 0.086 Uiso 1 1 calc R . . C23A C 0.0641(7) 0.0274(6) 0.4222(6) 0.074(3) Uani 1 1 d . . . H23A H 0.0469 -0.0341 0.4068 0.089 Uiso 1 1 calc R . . C24A C 0.0745(6) 0.0639(5) 0.3657(6) 0.056(3) Uani 1 1 d . . . H24A H 0.0627 0.0263 0.3103 0.067 Uiso 1 1 calc R . . C25A C -0.0280(5) 0.0990(5) 0.1983(5) 0.0313(19) Uani 1 1 d . . . C26A C -0.0830(6) 0.1323(5) 0.2355(5) 0.041(2) Uani 1 1 d . . . H26A H -0.0595 0.1835 0.2849 0.049 Uiso 1 1 calc R . . C27A C -0.1713(6) 0.0920(5) 0.2015(5) 0.044(2) Uani 1 1 d . . . H27A H -0.2094 0.1160 0.2265 0.052 Uiso 1 1 calc R . . C28A C -0.2056(6) 0.0155(5) 0.1301(5) 0.045(2) Uani 1 1 d . . . H28A H -0.2670 -0.0126 0.1061 0.054 Uiso 1 1 calc R . . C29A C -0.1503(5) -0.0183(5) 0.0950(5) 0.039(2) Uani 1 1 d . . . H29A H -0.1731 -0.0709 0.0471 0.047 Uiso 1 1 calc R . . C30A C -0.0627(5) 0.0227(5) 0.1281(5) 0.040(2) Uani 1 1 d . . . H30A H -0.0249 -0.0012 0.1027 0.048 Uiso 1 1 calc R . . C31A C 0.4589(7) 0.1805(7) 0.2941(7) 0.006(3) Uiso 0.50 1 d P . . C32A C 0.3548(9) 0.1454(9) 0.1169(10) 0.029(4) Uiso 0.50 1 d P . . Fe1B Fe 0.32242(8) 0.50460(7) 0.71210(7) 0.0324(3) Uani 1 1 d . . . F1B F 0.0494(3) 0.3847(3) 0.6532(3) 0.0493(13) Uani 1 1 d . . . F2B F 0.5951(3) 0.6234(2) 0.7680(3) 0.0437(12) Uani 1 1 d . . . B1B B 0.1351(6) 0.4208(6) 0.6719(6) 0.035(2) Uani 1 1 d . . . B2B B 0.5082(6) 0.5865(5) 0.7487(6) 0.032(2) Uani 1 1 d . . . N1B N 0.2809(4) 0.4035(4) 0.7321(4) 0.0336(16) Uani 1 1 d . . . N2B N 0.4188(4) 0.4527(4) 0.7233(4) 0.0329(16) Uani 1 1 d . . . N3B N 0.2430(4) 0.5548(4) 0.7533(4) 0.0286(15) Uani 1 1 d . . . N4B N 0.4015(4) 0.6016(4) 0.8088(4) 0.0298(15) Uani 1 1 d . . . N5B N 0.2255(4) 0.4546(3) 0.6073(4) 0.0341(16) Uani 1 1 d . . . N6B N 0.3644(4) 0.5575(4) 0.6478(4) 0.0344(16) Uani 1 1 d . . . N7B N 0.0997(5) 0.4189(5) 0.3981(5) 0.064(2) Uani 1 1 d . . . O1B O 0.1948(3) 0.3760(3) 0.7184(3) 0.0383(14) Uani 1 1 d . . . O2B O 0.5008(3) 0.4915(3) 0.7311(3) 0.0351(13) Uani 1 1 d . . . O3B O 0.1542(3) 0.5167(3) 0.7246(3) 0.0362(13) Uani 1 1 d . . . O4B O 0.4894(3) 0.6283(3) 0.8245(3) 0.0355(13) Uani 1 1 d . . . O5B O 0.1435(3) 0.4105(3) 0.5906(3) 0.0419(14) Uani 1 1 d . . . O6B O 0.4497(3) 0.6030(3) 0.6763(3) 0.0351(13) Uani 1 1 d . . . C1B C 0.3299(5) 0.3463(5) 0.7355(5) 0.034(2) Uani 1 1 d . . . C2B C 0.4168(5) 0.3771(5) 0.7381(5) 0.033(2) Uani 1 1 d . . . C3B C 0.2738(5) 0.6255(4) 0.8241(5) 0.0288(18) Uani 1 1 d . . . C4B C 0.3695(5) 0.6558(4) 0.8523(4) 0.0257(18) Uani 1 1 d . . . C5B C 0.2320(6) 0.4772(5) 0.5440(5) 0.038(2) Uani 1 1 d . . . C6B C 0.3159(6) 0.5317(5) 0.5688(6) 0.044(2) Uani 1 1 d . . . H6BA H 0.3349 0.5480 0.5308 0.052 Uiso 1 1 calc R . . C7B C 0.2972(5) 0.2573(4) 0.7318(5) 0.034(2) Uani 1 1 d . . . C8B C 0.2596(5) 0.2441(5) 0.7850(5) 0.041(2) Uani 1 1 d . . . H8BA H 0.2526 0.2924 0.8246 0.049 Uiso 1 1 calc R . . C9B C 0.2318(5) 0.1592(5) 0.7805(6) 0.051(3) Uani 1 1 d . . . H9BA H 0.2056 0.1503 0.8170 0.061 Uiso 1 1 calc R . . C10B C 0.2418(6) 0.0897(5) 0.7247(6) 0.057(3) Uani 1 1 d . . . H10B H 0.2209 0.0324 0.7213 0.069 Uiso 1 1 calc R . . C11B C 0.2825(6) 0.1017(5) 0.6722(6) 0.066(3) Uani 1 1 d . . . H11B H 0.2910 0.0531 0.6340 0.079 Uiso 1 1 calc R . . C12B C 0.3105(6) 0.1863(5) 0.6769(5) 0.057(3) Uani 1 1 d . . . H12B H 0.3390 0.1955 0.6421 0.069 Uiso 1 1 calc R . . C13B C 0.4899(5) 0.3327(4) 0.7516(5) 0.037(2) Uani 1 1 d . . . C14B C 0.5382(5) 0.3212(5) 0.7020(5) 0.041(2) Uani 1 1 d . . . H14B H 0.5266 0.3462 0.6601 0.050 Uiso 1 1 calc R . . C15B C 0.6019(5) 0.2747(5) 0.7123(5) 0.046(2) Uani 1 1 d . . . H15B H 0.6340 0.2666 0.6774 0.055 Uiso 1 1 calc R . . C16B C 0.6198(6) 0.2383(5) 0.7761(6) 0.052(3) Uani 1 1 d . . . H16B H 0.6638 0.2054 0.7833 0.063 Uiso 1 1 calc R . . C17B C 0.5748(5) 0.2500(5) 0.8264(5) 0.043(2) Uani 1 1 d . . . H17B H 0.5885 0.2266 0.8695 0.052 Uiso 1 1 calc R . . C18B C 0.5079(5) 0.2965(5) 0.8153(5) 0.043(2) Uani 1 1 d . . . H18B H 0.4753 0.3037 0.8496 0.051 Uiso 1 1 calc R . . C19B C 0.2199(5) 0.6634(4) 0.8679(5) 0.0267(18) Uani 1 1 d . . . C20B C 0.1396(5) 0.6800(5) 0.8259(6) 0.045(2) Uani 1 1 d . . . H20B H 0.1180 0.6652 0.7669 0.054 Uiso 1 1 calc R . . C21B C 0.0909(5) 0.7174(5) 0.8679(5) 0.045(2) Uani 1 1 d . . . H21B H 0.0368 0.7297 0.8381 0.054 Uiso 1 1 calc R . . C22B C 0.1198(6) 0.7375(5) 0.9537(6) 0.050(2) Uani 1 1 d . . . H22B H 0.0851 0.7623 0.9825 0.060 Uiso 1 1 calc R . . C23B C 0.1985(5) 0.7213(5) 0.9963(5) 0.039(2) Uani 1 1 d . . . H23B H 0.2186 0.7351 1.0551 0.047 Uiso 1 1 calc R . . C24B C 0.2498(5) 0.6845(4) 0.9546(5) 0.037(2) Uani 1 1 d . . . H24B H 0.3047 0.6739 0.9849 0.044 Uiso 1 1 calc R . . C25B C 0.4208(5) 0.7405(4) 0.9222(5) 0.034(2) Uani 1 1 d . . . C26B C 0.3886(5) 0.8161(5) 0.9221(5) 0.039(2) Uani 1 1 d . . . H26B H 0.3356 0.8138 0.8778 0.047 Uiso 1 1 calc R . . C27B C 0.4370(6) 0.8946(5) 0.9892(6) 0.053(3) Uani 1 1 d . . . H27B H 0.4162 0.9461 0.9905 0.063 Uiso 1 1 calc R . . C28B C 0.5127(6) 0.8986(6) 1.0524(6) 0.059(3) Uani 1 1 d . . . H28B H 0.5443 0.9530 1.0969 0.071 Uiso 1 1 calc R . . C29B C 0.5454(6) 0.8237(6) 1.0535(6) 0.055(3) Uani 1 1 d . . . H29B H 0.5975 0.8264 1.0989 0.066 Uiso 1 1 calc R . . C30B C 0.5000(5) 0.7468(5) 0.9871(5) 0.044(2) Uani 1 1 d . . . H30B H 0.5231 0.6964 0.9852 0.053 Uiso 1 1 calc R . . C31B C 0.1585(6) 0.4455(6) 0.4610(6) 0.047(2) Uani 1 1 d . . . C1S C 0.8958(11) 0.3020(10) 0.4313(11) 0.120(5) Uani 1 1 d . . . H1SA H 0.9488 0.3457 0.4517 0.144 Uiso 1 1 calc R . . C2S C 0.8080(19) 0.3051(13) 0.3724(11) 0.146(9) Uani 1 1 d . . . H2SA H 0.8065 0.3548 0.3566 0.175 Uiso 1 1 calc R . . C3S C 0.7320(13) 0.2460(15) 0.3397(11) 0.149(9) Uani 1 1 d . . . H3SA H 0.6776 0.2505 0.3020 0.178 Uiso 1 1 calc R . . C4S C 0.7413(11) 0.1743(14) 0.3680(9) 0.135(8) Uani 1 1 d . . . H4SA H 0.6899 0.1285 0.3475 0.162 Uiso 1 1 calc R . . C5S C 0.8084(14) 0.1686(9) 0.4149(10) 0.102(5) Uani 1 1 d . . . H5SA H 0.8067 0.1179 0.4289 0.122 Uiso 1 1 calc R . . C6S C 0.8925(12) 0.2306(13) 0.4530(9) 0.111(5) Uani 1 1 d . . . H6SA H 0.9436 0.2222 0.4918 0.133 Uiso 1 1 calc R . . C7S C 0.5906(10) 0.0327(8) 0.4558(9) 0.106(4) Uani 1 1 d . . . H7SA H 0.5585 0.0668 0.4284 0.127 Uiso 1 1 calc R . . C8S C 0.5527(9) -0.0553(8) 0.4361(8) 0.113(4) Uani 1 1 d . . . H8SA H 0.4937 -0.0802 0.3946 0.136 Uiso 1 1 calc R . . C9S C 0.5956(10) -0.1062(7) 0.4730(7) 0.091(4) Uani 1 1 d . . . H9SA H 0.5667 -0.1646 0.4603 0.110 Uiso 1 1 calc R . . C10S C 0.6826(10) -0.0712(7) 0.5297(8) 0.100(4) Uani 1 1 d . . . H10C H 0.7158 -0.1066 0.5542 0.120 Uiso 1 1 calc R . . C11S C 0.7229(8) 0.0176(7) 0.5516(6) 0.084(3) Uani 1 1 d . . . H11C H 0.7829 0.0418 0.5910 0.101 Uiso 1 1 calc R . . C12S C 0.6757(9) 0.0673(8) 0.5163(8) 0.093(4) Uani 1 1 d . . . H12C H 0.7018 0.1276 0.5335 0.111 Uiso 1 1 calc R . . C13S C 0.3037(10) 0.3681(8) 0.0262(7) 0.085(4) Uani 1 1 d . . . H13A H 0.3300 0.3373 0.0608 0.102 Uiso 1 1 calc R . . C14S C 0.3556(8) 0.4334(7) 0.0259(8) 0.094(4) Uani 1 1 d . . . H14C H 0.4172 0.4515 0.0617 0.113 Uiso 1 1 calc R . . C15S C 0.3178(9) 0.4762(6) -0.0289(8) 0.085(4) Uani 1 1 d . . . H15C H 0.3551 0.5216 -0.0323 0.102 Uiso 1 1 calc R . . C16S C 0.2290(9) 0.4539(7) -0.0769(7) 0.079(4) Uani 1 1 d . . . H16C H 0.2034 0.4839 -0.1126 0.095 Uiso 1 1 calc R . . C17S C 0.1774(7) 0.3866(6) -0.0722(7) 0.075(3) Uani 1 1 d . . . H17C H 0.1152 0.3703 -0.1052 0.091 Uiso 1 1 calc R . . C18S C 0.2139(8) 0.3416(7) -0.0204(7) 0.074(3) Uani 1 1 d . . . H18C H 0.1780 0.2948 -0.0175 0.089 Uiso 1 1 calc R . . C19S C 0.3640(11) -0.0318(9) 0.2110(15) 0.124(7) Uani 1 1 d . . . H19A H 0.4230 -0.0387 0.2324 0.149 Uiso 1 1 calc R . . C20S C 0.3294(10) -0.0009(6) 0.2640(8) 0.086(4) Uani 1 1 d . . . H20C H 0.3637 0.0163 0.3225 0.103 Uiso 1 1 calc R . . C21S C 0.2443(10) 0.0067(6) 0.2361(10) 0.081(4) Uani 1 1 d . . . H21C H 0.2187 0.0274 0.2754 0.097 Uiso 1 1 calc R . . C22S C 0.1930(8) -0.0151(6) 0.1510(11) 0.083(4) Uani 1 1 d . . . H22C H 0.1336 -0.0085 0.1316 0.099 Uiso 1 1 calc R . . C23S C 0.2327(14) -0.0471(7) 0.0952(10) 0.124(6) Uani 1 1 d . . . H23C H 0.2004 -0.0636 0.0365 0.149 Uiso 1 1 calc R . . C24S C 0.3222(15) -0.0544(9) 0.1282(13) 0.128(8) Uani 1 1 d . . . H24C H 0.3515 -0.0750 0.0922 0.153 Uiso 1 1 calc R . . C25S C 0.9378(7) 0.1656(6) 0.8018(6) 0.067(3) Uani 1 1 d . . . H25A H 0.9412 0.1350 0.8386 0.081 Uiso 1 1 calc R . . C26S C 0.8684(7) 0.1979(6) 0.7760(7) 0.077(3) Uani 1 1 d . . . H26C H 0.8221 0.1913 0.7948 0.093 Uiso 1 1 calc R . . C27S C 0.8628(7) 0.2420(7) 0.7211(7) 0.086(4) Uani 1 1 d . . . H27C H 0.8113 0.2632 0.7010 0.104 Uiso 1 1 calc R . . C28S C 0.9284(6) 0.2549(6) 0.6963(6) 0.067(3) Uani 1 1 d . . . H28C H 0.9247 0.2876 0.6612 0.080 Uiso 1 1 calc R . . C29S C 0.9991(7) 0.2222(6) 0.7205(7) 0.073(3) Uani 1 1 d . . . H29C H 1.0449 0.2297 0.7013 0.087 Uiso 1 1 calc R . . C30S C 1.0052(6) 0.1759(6) 0.7755(7) 0.079(3) Uani 1 1 d . . . H30C H 1.0554 0.1525 0.7938 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1A 0.0436(7) 0.0229(6) 0.0210(7) 0.0080(5) 0.0129(6) 0.0030(5) F1A 0.063(3) 0.035(3) 0.027(3) 0.016(2) 0.006(3) 0.007(2) F2A 0.056(3) 0.036(2) 0.025(3) 0.007(2) 0.012(2) 0.003(2) B1A 0.055(7) 0.030(5) 0.025(6) 0.010(5) 0.010(6) 0.007(5) B2A 0.043(6) 0.018(5) 0.016(6) 0.001(4) 0.009(5) 0.000(4) N1A 0.042(4) 0.029(3) 0.014(4) 0.010(3) 0.007(3) 0.002(3) N2A 0.040(4) 0.023(3) 0.018(4) 0.000(3) 0.014(3) -0.003(3) N3A 0.050(4) 0.029(4) 0.035(5) 0.016(4) 0.020(4) 0.000(3) N4A 0.046(4) 0.030(4) 0.016(4) 0.002(3) 0.007(3) -0.004(3) N5A 0.050(4) 0.022(3) 0.023(4) 0.004(3) 0.012(4) 0.003(3) N6A 0.032(4) 0.026(3) 0.037(5) 0.013(3) 0.016(4) 0.006(3) O1A 0.054(4) 0.026(3) 0.030(4) 0.016(3) 0.013(3) 0.005(3) O2A 0.044(3) 0.027(3) 0.019(3) 0.005(3) 0.009(3) -0.002(2) O3A 0.049(4) 0.033(3) 0.023(4) 0.011(3) 0.009(3) -0.003(3) O4A 0.058(4) 0.027(3) 0.017(3) 0.002(3) 0.015(3) -0.005(3) O5A 0.060(4) 0.028(3) 0.020(3) 0.010(3) 0.006(3) 0.010(3) O6A 0.043(3) 0.035(3) 0.026(4) 0.013(3) 0.011(3) 0.005(3) C1A 0.035(5) 0.023(4) 0.028(5) 0.012(4) 0.016(4) 0.003(4) C2A 0.034(5) 0.022(4) 0.019(5) 0.007(4) 0.008(4) 0.005(4) C3A 0.050(5) 0.024(4) 0.021(5) 0.009(4) 0.014(4) -0.003(4) C4A 0.046(5) 0.023(4) 0.029(5) 0.012(4) 0.016(5) -0.006(4) C5A 0.053(6) 0.023(4) 0.052(7) 0.015(5) 0.019(5) 0.012(4) C6A 0.040(5) 0.034(5) 0.033(6) 0.017(4) 0.022(5) 0.005(4) C7A 0.037(5) 0.023(4) 0.015(4) 0.014(4) 0.012(4) 0.004(4) C8A 0.047(5) 0.027(4) 0.026(5) 0.008(4) 0.012(4) 0.008(4) C9A 0.056(6) 0.032(5) 0.021(5) 0.011(4) 0.012(5) 0.009(4) C10A 0.067(6) 0.024(4) 0.022(5) 0.008(4) 0.014(5) 0.010(5) C11A 0.060(6) 0.027(5) 0.025(5) 0.011(4) 0.013(5) -0.009(4) C12A 0.041(5) 0.042(5) 0.021(5) 0.020(4) 0.012(4) 0.005(4) C13A 0.036(5) 0.021(4) 0.025(5) 0.002(4) 0.005(4) -0.001(4) C14A 0.075(7) 0.035(5) 0.030(6) 0.013(4) 0.015(5) -0.003(5) C15A 0.109(9) 0.049(6) 0.038(7) 0.032(5) 0.019(6) 0.002(6) C16A 0.105(9) 0.032(5) 0.034(7) 0.014(5) -0.006(6) -0.001(6) C17A 0.069(7) 0.050(6) 0.056(8) 0.016(6) -0.002(6) 0.007(6) C18A 0.065(7) 0.040(5) 0.034(6) 0.015(5) 0.010(5) 0.002(5) C19A 0.065(6) 0.036(5) 0.028(6) 0.008(4) 0.020(5) -0.009(4) C20A 0.113(8) 0.040(5) 0.031(6) -0.001(5) 0.038(6) -0.024(5) C21A 0.120(9) 0.080(8) 0.051(8) 0.021(7) 0.050(7) -0.010(7) C22A 0.081(8) 0.077(8) 0.058(8) 0.037(7) 0.030(6) -0.018(6) C23A 0.115(9) 0.049(6) 0.039(7) 0.016(6) 0.021(7) -0.019(6) C24A 0.100(7) 0.031(5) 0.043(6) 0.016(5) 0.040(6) -0.004(5) C25A 0.052(5) 0.024(4) 0.023(5) 0.010(4) 0.022(4) 0.003(4) C26A 0.058(6) 0.031(5) 0.045(6) 0.019(4) 0.031(5) 0.005(4) C27A 0.062(6) 0.041(5) 0.048(6) 0.016(5) 0.043(5) 0.020(5) C28A 0.062(6) 0.038(5) 0.028(6) 0.012(5) 0.013(5) -0.001(5) C29A 0.051(6) 0.033(5) 0.029(5) 0.005(4) 0.020(5) -0.006(4) C30A 0.052(6) 0.030(5) 0.048(6) 0.015(5) 0.030(5) 0.008(4) Fe1B 0.0496(7) 0.0264(6) 0.0262(8) 0.0130(6) 0.0194(6) 0.0042(6) F1B 0.047(3) 0.054(3) 0.035(3) 0.016(2) 0.010(2) -0.012(2) F2B 0.054(3) 0.032(2) 0.056(3) 0.019(2) 0.033(3) 0.004(2) B1B 0.039(6) 0.040(6) 0.023(6) 0.002(5) 0.020(5) 0.002(5) B2B 0.037(6) 0.022(5) 0.045(7) 0.004(5) 0.032(5) 0.002(4) N1B 0.035(4) 0.036(4) 0.024(4) 0.011(3) 0.012(3) -0.010(3) N2B 0.029(4) 0.034(4) 0.035(4) 0.007(3) 0.020(3) -0.006(3) N3B 0.041(4) 0.026(3) 0.020(4) 0.016(3) 0.011(3) 0.003(3) N4B 0.039(4) 0.029(4) 0.025(4) 0.016(3) 0.014(3) 0.002(3) N5B 0.047(4) 0.021(3) 0.033(4) 0.009(3) 0.018(4) 0.000(3) N6B 0.048(5) 0.025(4) 0.036(5) 0.013(3) 0.023(4) 0.007(3) N7B 0.067(6) 0.076(6) 0.034(6) 0.025(5) 0.003(5) 0.000(5) O1B 0.049(4) 0.036(3) 0.035(4) 0.017(3) 0.020(3) 0.003(3) O2B 0.050(3) 0.031(3) 0.036(4) 0.017(3) 0.027(3) 0.008(3) O3B 0.044(3) 0.042(3) 0.025(3) 0.016(3) 0.015(3) 0.006(3) O4B 0.036(3) 0.036(3) 0.041(4) 0.017(3) 0.020(3) 0.005(3) O5B 0.052(4) 0.037(3) 0.032(4) 0.009(3) 0.020(3) -0.009(3) O6B 0.046(3) 0.034(3) 0.032(4) 0.020(3) 0.019(3) 0.000(3) C1B 0.050(6) 0.028(4) 0.032(5) 0.014(4) 0.022(5) 0.010(4) C2B 0.058(6) 0.030(4) 0.022(5) 0.017(4) 0.021(4) 0.011(4) C3B 0.041(5) 0.024(4) 0.029(5) 0.013(4) 0.019(4) 0.010(4) C4B 0.044(5) 0.022(4) 0.013(4) 0.011(4) 0.009(4) 0.006(4) C5B 0.057(6) 0.030(5) 0.024(5) 0.008(4) 0.016(5) 0.001(4) C6B 0.064(6) 0.032(5) 0.036(6) 0.015(5) 0.021(5) 0.007(5) C7B 0.048(5) 0.028(4) 0.026(5) 0.015(4) 0.014(4) -0.005(4) C8B 0.058(6) 0.035(5) 0.040(6) 0.022(4) 0.024(5) 0.011(4) C9B 0.056(6) 0.047(6) 0.076(8) 0.044(6) 0.038(6) 0.015(5) C10B 0.081(7) 0.037(5) 0.048(7) 0.017(5) 0.023(6) -0.009(5) C11B 0.109(8) 0.035(5) 0.046(7) 0.012(5) 0.030(6) 0.001(5) C12B 0.116(8) 0.030(5) 0.040(6) 0.017(5) 0.046(6) 0.006(5) C13B 0.059(6) 0.024(4) 0.040(6) 0.021(4) 0.024(5) 0.010(4) C14B 0.057(6) 0.040(5) 0.051(6) 0.030(5) 0.036(5) 0.014(4) C15B 0.056(6) 0.048(5) 0.047(6) 0.023(5) 0.030(5) 0.018(5) C16B 0.067(6) 0.039(5) 0.060(7) 0.028(5) 0.023(6) 0.024(5) C17B 0.060(6) 0.050(5) 0.030(6) 0.025(5) 0.020(5) 0.014(5) C18B 0.055(6) 0.044(5) 0.044(6) 0.030(5) 0.024(5) 0.013(4) C19B 0.034(5) 0.022(4) 0.019(5) 0.004(4) 0.009(4) 0.002(4) C20B 0.051(6) 0.060(6) 0.046(6) 0.029(5) 0.032(5) 0.027(5) C21B 0.051(6) 0.057(6) 0.041(6) 0.034(5) 0.017(5) 0.022(5) C22B 0.065(6) 0.049(5) 0.052(7) 0.022(5) 0.038(6) 0.021(5) C23B 0.047(5) 0.047(5) 0.033(6) 0.018(4) 0.023(5) 0.013(4) C24B 0.048(5) 0.028(4) 0.035(6) 0.010(4) 0.019(5) 0.010(4) C25B 0.051(5) 0.025(4) 0.028(5) 0.007(4) 0.024(5) 0.002(4) C26B 0.055(6) 0.032(5) 0.043(6) 0.015(4) 0.031(5) 0.012(4) C27B 0.064(7) 0.028(5) 0.064(8) 0.005(5) 0.036(6) 0.009(5) C28B 0.065(7) 0.041(6) 0.049(7) -0.009(5) 0.027(6) -0.015(5) C29B 0.058(6) 0.054(6) 0.037(6) 0.003(5) 0.016(5) 0.006(5) C30B 0.055(6) 0.047(6) 0.035(6) 0.019(5) 0.020(5) 0.009(5) C31B 0.054(6) 0.048(6) 0.046(7) 0.029(5) 0.021(6) 0.003(5) C1S 0.158(16) 0.097(11) 0.143(16) 0.025(10) 0.121(14) 0.024(10) C2S 0.29(3) 0.171(18) 0.076(14) 0.084(14) 0.120(16) 0.18(2) C3S 0.139(16) 0.23(3) 0.050(12) 0.001(14) 0.044(12) 0.069(17) C4S 0.131(14) 0.23(2) 0.038(10) 0.028(11) 0.029(9) 0.116(15) C5S 0.169(15) 0.084(10) 0.097(13) 0.038(10) 0.095(13) 0.045(12) C6S 0.165(17) 0.140(13) 0.088(12) 0.053(12) 0.098(12) 0.076(13) C7S 0.142(13) 0.077(9) 0.087(11) 0.037(9) 0.029(10) 0.015(9) C8S 0.131(12) 0.084(10) 0.104(12) 0.030(9) 0.033(9) 0.005(9) C9S 0.176(14) 0.053(7) 0.036(8) 0.018(6) 0.033(8) 0.018(9) C10S 0.200(15) 0.051(8) 0.060(9) 0.029(7) 0.055(10) 0.046(9) C11S 0.138(11) 0.064(7) 0.045(8) 0.014(6) 0.038(7) 0.019(8) C12S 0.148(12) 0.080(9) 0.079(10) 0.054(9) 0.053(9) 0.041(9) C13S 0.151(13) 0.073(8) 0.058(9) 0.041(7) 0.045(9) 0.065(9) C14S 0.121(11) 0.055(7) 0.105(11) 0.037(8) 0.030(9) 0.050(8) C15S 0.119(10) 0.039(6) 0.089(10) 0.014(7) 0.043(9) 0.017(7) C16S 0.160(12) 0.057(7) 0.043(8) 0.023(6) 0.054(9) 0.057(8) C17S 0.098(9) 0.058(7) 0.084(9) 0.019(7) 0.054(8) 0.032(7) C18S 0.122(10) 0.084(8) 0.064(9) 0.057(7) 0.058(8) 0.054(8) C19S 0.165(16) 0.065(9) 0.24(2) 0.082(14) 0.156(19) 0.064(10) C20S 0.107(11) 0.056(7) 0.110(12) 0.043(8) 0.050(10) 0.020(7) C21S 0.094(10) 0.048(7) 0.125(14) 0.037(8) 0.068(10) 0.014(7) C22S 0.089(9) 0.035(6) 0.115(12) 0.031(8) 0.030(10) 0.006(6) C23S 0.25(2) 0.033(7) 0.094(13) 0.022(8) 0.087(17) -0.005(11) C24S 0.23(2) 0.055(8) 0.16(2) 0.030(12) 0.16(2) 0.017(12) C25S 0.081(8) 0.074(7) 0.055(7) 0.047(6) 0.017(6) 0.012(6) C26S 0.107(9) 0.089(8) 0.090(9) 0.065(7) 0.068(8) 0.044(7) C27S 0.080(8) 0.098(8) 0.120(11) 0.073(8) 0.051(8) 0.037(7) C28S 0.050(7) 0.090(8) 0.077(8) 0.060(7) 0.020(6) 0.010(6) C29S 0.071(8) 0.082(8) 0.083(9) 0.040(7) 0.044(7) 0.012(6) C30S 0.054(7) 0.098(8) 0.091(10) 0.057(8) 0.019(7) 0.010(6) _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 Fe1A N5A 1.867(6) . ? Fe1A N6A 1.887(6) . ? Fe1A N1A 1.900(6) . ? Fe1A N4A 1.916(6) . ? Fe1A N2A 1.926(6) . ? Fe1A N3A 1.935(6) . ? F1A B1A 1.366(10) . ? F2A B2A 1.367(9) . ? B1A O3A 1.424(10) . ? B1A O5A 1.494(10) . ? B1A O1A 1.539(9) . ? B2A O6A 1.453(9) . ? B2A O2A 1.481(9) . ? B2A O4A 1.513(9) . ? N1A C1A 1.314(8) . ? N1A O1A 1.402(7) . ? N2A C2A 1.293(7) . ? N2A O2A 1.375(7) . ? N3A C3A 1.286(8) . ? N3A O3A 1.380(7) . ? N4A C4A 1.331(8) . ? N4A O4A 1.388(7) . ? N5A C5A 1.347(9) . ? N5A O5A 1.382(7) . ? N6A C6A 1.310(8) . ? N6A O6A 1.371(7) . ? N7A C31A 1.074(12) . ? N8A C32A 1.122(16) . ? C1A C2A 1.459(9) . ? C1A C7A 1.470(9) . ? C2A C13A 1.494(9) . ? C3A C4A 1.455(10) . ? C3A C19A 1.491(10) . ? C4A C25A 1.464(10) . ? C5A C6A 1.418(10) . ? C5A C31A 1.449(13) . ? C5A H5A 0.9598 . ? C6A C32A 1.378(16) . ? C6A H6A 1.0148 . ? C7A C8A 1.360(9) . ? C7A C12A 1.399(9) . ? C8A C9A 1.388(9) . ? C8A H8AA 0.9500 . ? C9A C10A 1.371(10) . ? C9A H9AA 0.9500 . ? C10A C11A 1.378(9) . ? C10A H10A 0.9500 . ? C11A C12A 1.404(9) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C18A 1.367(10) . ? C13A C14A 1.370(9) . ? C14A C15A 1.407(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.325(11) . ? C15A H15A 0.9500 . ? C16A C17A 1.410(12) . ? C16A H16A 0.9500 . ? C17A C18A 1.395(11) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A C24A 1.378(9) . ? C19A C20A 1.401(10) . ? C20A C21A 1.410(11) . ? C20A H20A 0.9500 . ? C21A C22A 1.357(11) . ? C21A H21A 0.9500 . ? C22A C23A 1.384(12) . ? C22A H22A 0.9500 . ? C23A C24A 1.396(10) . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? C25A C26A 1.378(9) . ? C25A C30A 1.384(10) . ? C26A C27A 1.365(10) . ? C26A H26A 0.9500 . ? C27A C28A 1.398(10) . ? C27A H27A 0.9500 . ? C28A C29A 1.361(10) . ? C28A H28A 0.9500 . ? C29A C30A 1.358(9) . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? Fe1B N2B 1.865(6) . ? Fe1B N3B 1.874(6) . ? Fe1B N5B 1.879(6) . ? Fe1B N4B 1.903(6) . ? Fe1B N6B 1.922(6) . ? Fe1B N1B 1.926(5) . ? F1B B1B 1.353(9) . ? F2B B2B 1.373(9) . ? B1B O1B 1.483(10) . ? B1B O5B 1.500(10) . ? B1B O3B 1.516(9) . ? B2B O6B 1.463(10) . ? B2B O2B 1.489(9) . ? B2B O4B 1.502(9) . ? N1B C1B 1.310(8) . ? N1B O1B 1.354(7) . ? N2B C2B 1.358(8) . ? N2B O2B 1.374(6) . ? N3B C3B 1.340(8) . ? N3B O3B 1.373(7) . ? N4B C4B 1.294(8) . ? N4B O4B 1.370(6) . ? N5B O5B 1.351(7) . ? N5B C5B 1.354(9) . ? N6B C6B 1.287(9) . ? N6B O6B 1.358(7) . ? N7B C31B 1.132(10) . ? C1B C2B 1.450(10) . ? C1B C7B 1.486(9) . ? C2B C13B 1.465(9) . ? C3B C4B 1.455(9) . ? C3B C19B 1.460(9) . ? C4B C25B 1.489(9) . ? C5B C6B 1.408(10) . ? C5B C31B 1.465(11) . ? C6B H6BA 0.9500 . ? C7B C8B 1.380(9) . ? C7B C12B 1.386(10) . ? C8B C9B 1.398(9) . ? C8B H8BA 0.9500 . ? C9B C10B 1.353(10) . ? C9B H9BA 0.9500 . ? C10B C11B 1.397(11) . ? C10B H10B 0.9500 . ? C11B C12B 1.394(10) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.387(9) . ? C13B C18B 1.422(10) . ? C14B C15B 1.362(9) . ? C14B H14B 0.9500 . ? C15B C16B 1.428(11) . ? C15B H15B 0.9500 . ? C16B C17B 1.354(10) . ? C16B H16B 0.9500 . ? C17B C18B 1.403(9) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? C19B C20B 1.385(9) . ? C19B C24B 1.400(10) . ? C20B C21B 1.365(10) . ? C20B H20B 0.9500 . ? C21B C22B 1.388(11) . ? C21B H21B 0.9500 . ? C22B C23B 1.364(10) . ? C22B H22B 0.9500 . ? C23B C24B 1.393(9) . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? C25B C30B 1.392(10) . ? C25B C26B 1.411(9) . ? C26B C27B 1.398(10) . ? C26B H26B 0.9500 . ? C27B C28B 1.352(11) . ? C27B H27B 0.9500 . ? C28B C29B 1.407(11) . ? C28B H28B 0.9500 . ? C29B C30B 1.370(10) . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? C1S C6S 1.359(15) . ? C1S C2S 1.491(19) . ? C1S H1SA 0.9500 . ? C2S C3S 1.32(2) . ? C2S H2SA 0.9500 . ? C3S C4S 1.43(2) . ? C3S H3SA 0.9500 . ? C4S C5S 1.174(16) . ? C4S H4SA 0.9500 . ? C5S C6S 1.432(17) . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S C12S 1.373(14) . ? C7S C8S 1.404(14) . ? C7S H7SA 0.9500 . ? C8S C9S 1.344(14) . ? C8S H8SA 0.9500 . ? C9S C10S 1.375(15) . ? C9S H9SA 0.9500 . ? C10S C11S 1.418(13) . ? C10S H10C 0.9500 . ? C11S C12S 1.346(12) . ? C11S H11C 0.9500 . ? C12S H12C 0.9500 . ? C13S C14S 1.308(13) . ? C13S C18S 1.367(13) . ? C13S H13A 0.9500 . ? C14S C15S 1.410(14) . ? C14S H14C 0.9500 . ? C15S C16S 1.358(13) . ? C15S H15C 0.9500 . ? C16S C17S 1.370(12) . ? C16S H16C 0.9500 . ? C17S C18S 1.394(12) . ? C17S H17C 0.9500 . ? C18S H18C 0.9500 . ? C19S C20S 1.292(15) . ? C19S C24S 1.33(2) . ? C19S H19A 0.9500 . ? C20S C21S 1.352(13) . ? C20S H20C 0.9500 . ? C21S C22S 1.393(15) . ? C21S H21C 0.9500 . ? C22S C23S 1.399(16) . ? C22S H22C 0.9500 . ? C23S C24S 1.42(2) . ? C23S H23C 0.9500 . ? C24S H24C 0.9500 . ? C25S C26S 1.314(11) . ? C25S C30S 1.371(12) . ? C25S H25A 0.9500 . ? C26S C27S 1.396(12) . ? C26S H26C 0.9500 . ? C27S C28S 1.332(11) . ? C27S H27C 0.9500 . ? C28S C29S 1.330(11) . ? C28S H28C 0.9500 . ? C29S C30S 1.423(12) . ? C29S H29C 0.9500 . ? C30S H30C 0.9500 . ? 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 N5A Fe1A N6A 79.2(3) . . ? N5A Fe1A N1A 85.2(2) . . ? N6A Fe1A N1A 115.9(2) . . ? N5A Fe1A N4A 118.9(2) . . ? N6A Fe1A N4A 86.8(3) . . ? N1A Fe1A N4A 150.7(3) . . ? N5A Fe1A N2A 149.5(2) . . ? N6A Fe1A N2A 85.7(3) . . ? N1A Fe1A N2A 77.8(2) . . ? N4A Fe1A N2A 86.2(2) . . ? N5A Fe1A N3A 86.9(3) . . ? N6A Fe1A N3A 151.2(2) . . ? N1A Fe1A N3A 87.6(3) . . ? N4A Fe1A N3A 77.9(3) . . ? N2A Fe1A N3A 117.0(2) . . ? F1A B1A O3A 110.1(8) . . ? F1A B1A O5A 107.5(7) . . ? O3A B1A O5A 114.1(7) . . ? F1A B1A O1A 104.3(6) . . ? O3A B1A O1A 112.0(7) . . ? O5A B1A O1A 108.3(7) . . ? F2A B2A O6A 108.9(7) . . ? F2A B2A O2A 107.9(6) . . ? O6A B2A O2A 112.6(6) . . ? F2A B2A O4A 104.9(6) . . ? O6A B2A O4A 112.1(6) . . ? O2A B2A O4A 110.1(6) . . ? C1A N1A O1A 114.9(6) . . ? C1A N1A Fe1A 120.6(5) . . ? O1A N1A Fe1A 122.9(4) . . ? C2A N2A O2A 116.6(6) . . ? C2A N2A Fe1A 118.8(5) . . ? O2A N2A Fe1A 123.3(4) . . ? C3A N3A O3A 118.8(6) . . ? C3A N3A Fe1A 118.3(6) . . ? O3A N3A Fe1A 121.1(4) . . ? C4A N4A O4A 115.3(6) . . ? C4A N4A Fe1A 119.7(5) . . ? O4A N4A Fe1A 123.3(4) . . ? C5A N5A O5A 114.3(6) . . ? C5A N5A Fe1A 117.9(6) . . ? O5A N5A Fe1A 126.6(5) . . ? C6A N6A O6A 115.9(6) . . ? C6A N6A Fe1A 119.6(5) . . ? O6A N6A Fe1A 124.1(4) . . ? N1A O1A B1A 110.0(5) . . ? N2A O2A B2A 110.3(5) . . ? N3A O3A B1A 113.4(6) . . ? N4A O4A B2A 110.0(5) . . ? N5A O5A B1A 108.4(6) . . ? N6A O6A B2A 111.3(6) . . ? N1A C1A C2A 109.6(6) . . ? N1A C1A C7A 126.1(7) . . ? C2A C1A C7A 124.0(6) . . ? N2A C2A C1A 112.6(6) . . ? N2A C2A C13A 124.7(7) . . ? C1A C2A C13A 122.3(6) . . ? N3A C3A C4A 113.5(7) . . ? N3A C3A C19A 123.5(7) . . ? C4A C3A C19A 122.5(7) . . ? N4A C4A C3A 109.0(6) . . ? N4A C4A C25A 126.0(7) . . ? C3A C4A C25A 124.6(7) . . ? N5A C5A C6A 112.1(7) . . ? N5A C5A C31A 125.8(9) . . ? C6A C5A C31A 122.0(9) . . ? N5A C5A H5A 123.6 . . ? C6A C5A H5A 124.3 . . ? N6A C6A C32A 127.1(9) . . ? N6A C6A C5A 110.9(7) . . ? C32A C6A C5A 122.0(9) . . ? N6A C6A H6A 121.6 . . ? C5A C6A H6A 127.1 . . ? C8A C7A C12A 119.9(7) . . ? C8A C7A C1A 119.6(6) . . ? C12A C7A C1A 120.5(6) . . ? C7A C8A C9A 121.3(7) . . ? C7A C8A H8AA 119.4 . . ? C9A C8A H8AA 119.4 . . ? C10A C9A C8A 119.4(7) . . ? C10A C9A H9AA 120.3 . . ? C8A C9A H9AA 120.3 . . ? C9A C10A C11A 120.5(7) . . ? C9A C10A H10A 119.7 . . ? C11A C10A H10A 119.7 . . ? C10A C11A C12A 120.0(7) . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C7A C12A C11A 118.8(7) . . ? C7A C12A H12A 120.6 . . ? C11A C12A H12A 120.6 . . ? C18A C13A C14A 120.2(7) . . ? C18A C13A C2A 119.6(7) . . ? C14A C13A C2A 120.2(7) . . ? C13A C14A C15A 120.2(8) . . ? C13A C14A H14A 119.9 . . ? C15A C14A H14A 119.9 . . ? C16A C15A C14A 119.6(9) . . ? C16A C15A H15A 120.2 . . ? C14A C15A H15A 120.2 . . ? C15A C16A C17A 121.5(9) . . ? C15A C16A H16A 119.2 . . ? C17A C16A H16A 119.2 . . ? C18A C17A C16A 118.2(9) . . ? C18A C17A H17A 120.9 . . ? C16A C17A H17A 120.9 . . ? C13A C18A C17A 120.2(8) . . ? C13A C18A H18A 119.9 . . ? C17A C18A H18A 119.9 . . ? C24A C19A C20A 119.5(8) . . ? C24A C19A C3A 119.2(7) . . ? C20A C19A C3A 121.1(7) . . ? C19A C20A C21A 118.2(8) . . ? C19A C20A H20A 120.9 . . ? C21A C20A H20A 120.9 . . ? C22A C21A C20A 120.7(9) . . ? C22A C21A H21A 119.6 . . ? C20A C21A H21A 119.6 . . ? C21A C22A C23A 122.0(9) . . ? C21A C22A H22A 119.0 . . ? C23A C22A H22A 119.0 . . ? C22A C23A C24A 117.5(8) . . ? C22A C23A H23A 121.3 . . ? C24A C23A H23A 121.3 . . ? C19A C24A C23A 122.1(8) . . ? C19A C24A H24A 119.0 . . ? C23A C24A H24A 119.0 . . ? C26A C25A C30A 119.2(7) . . ? C26A C25A C4A 117.3(7) . . ? C30A C25A C4A 123.6(7) . . ? C27A C26A C25A 120.1(8) . . ? C27A C26A H26A 119.9 . . ? C25A C26A H26A 119.9 . . ? C26A C27A C28A 120.0(7) . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C29A C28A C27A 119.5(8) . . ? C29A C28A H28A 120.3 . . ? C27A C28A H28A 120.3 . . ? C30A C29A C28A 120.4(8) . . ? C30A C29A H29A 119.8 . . ? C28A C29A H29A 119.8 . . ? C29A C30A C25A 120.7(7) . . ? C29A C30A H30A 119.6 . . ? C25A C30A H30A 119.6 . . ? N2B Fe1B N3B 151.8(3) . . ? N2B Fe1B N5B 115.4(3) . . ? N3B Fe1B N5B 86.6(3) . . ? N2B Fe1B N4B 86.8(3) . . ? N3B Fe1B N4B 78.5(3) . . ? N5B Fe1B N4B 152.6(2) . . ? N2B Fe1B N6B 85.8(3) . . ? N3B Fe1B N6B 116.9(2) . . ? N5B Fe1B N6B 79.6(3) . . ? N4B Fe1B N6B 86.8(3) . . ? N2B Fe1B N1B 78.9(3) . . ? N3B Fe1B N1B 86.0(3) . . ? N5B Fe1B N1B 85.3(3) . . ? N4B Fe1B N1B 116.0(2) . . ? N6B Fe1B N1B 151.4(3) . . ? F1B B1B O1B 109.6(7) . . ? F1B B1B O5B 107.5(7) . . ? O1B B1B O5B 110.9(6) . . ? F1B B1B O3B 107.4(6) . . ? O1B B1B O3B 111.0(7) . . ? O5B B1B O3B 110.3(6) . . ? F2B B2B O6B 109.3(7) . . ? F2B B2B O2B 106.9(6) . . ? O6B B2B O2B 112.0(7) . . ? F2B B2B O4B 107.1(7) . . ? O6B B2B O4B 110.8(6) . . ? O2B B2B O4B 110.4(6) . . ? C1B N1B O1B 116.7(6) . . ? C1B N1B Fe1B 117.8(5) . . ? O1B N1B Fe1B 122.5(5) . . ? C2B N2B O2B 113.7(6) . . ? C2B N2B Fe1B 120.6(5) . . ? O2B N2B Fe1B 124.9(4) . . ? C3B N3B O3B 114.3(6) . . ? C3B N3B Fe1B 120.1(5) . . ? O3B N3B Fe1B 124.7(4) . . ? C4B N4B O4B 116.4(6) . . ? C4B N4B Fe1B 119.5(5) . . ? O4B N4B Fe1B 122.5(5) . . ? O5B N5B C5B 114.6(6) . . ? O5B N5B Fe1B 127.1(5) . . ? C5B N5B Fe1B 117.2(5) . . ? C6B N6B O6B 117.9(7) . . ? C6B N6B Fe1B 117.2(6) . . ? O6B N6B Fe1B 122.9(5) . . ? N1B O1B B1B 112.6(5) . . ? N2B O2B B2B 109.9(5) . . ? N3B O3B B1B 110.0(5) . . ? N4B O4B B2B 111.5(6) . . ? N5B O5B B1B 108.9(6) . . ? N6B O6B B2B 111.2(5) . . ? N1B C1B C2B 112.9(6) . . ? N1B C1B C7B 123.2(7) . . ? C2B C1B C7B 123.8(7) . . ? N2B C2B C1B 108.9(6) . . ? N2B C2B C13B 125.3(7) . . ? C1B C2B C13B 125.8(6) . . ? N3B C3B C4B 109.4(6) . . ? N3B C3B C19B 124.9(7) . . ? C4B C3B C19B 125.7(7) . . ? N4B C4B C3B 111.9(7) . . ? N4B C4B C25B 126.2(7) . . ? C3B C4B C25B 121.9(7) . . ? N5B C5B C6B 111.6(7) . . ? N5B C5B C31B 121.6(7) . . ? C6B C5B C31B 126.8(8) . . ? N6B C6B C5B 113.8(8) . . ? N6B C6B H6BA 123.1 . . ? C5B C6B H6BA 123.1 . . ? C8B C7B C12B 119.2(7) . . ? C8B C7B C1B 121.8(7) . . ? C12B C7B C1B 118.8(7) . . ? C7B C8B C9B 119.8(8) . . ? C7B C8B H8BA 120.1 . . ? C9B C8B H8BA 120.1 . . ? C10B C9B C8B 120.8(8) . . ? C10B C9B H9BA 119.6 . . ? C8B C9B H9BA 119.6 . . ? C9B C10B C11B 120.4(8) . . ? C9B C10B H10B 119.8 . . ? C11B C10B H10B 119.8 . . ? C12B C11B C10B 118.7(9) . . ? C12B C11B H11B 120.6 . . ? C10B C11B H11B 120.6 . . ? C7B C12B C11B 120.9(8) . . ? C7B C12B H12B 119.6 . . ? C11B C12B H12B 119.6 . . ? C14B C13B C18B 119.6(7) . . ? C14B C13B C2B 122.3(7) . . ? C18B C13B C2B 118.0(7) . . ? C15B C14B C13B 121.2(7) . . ? C15B C14B H14B 119.4 . . ? C13B C14B H14B 119.4 . . ? C14B C15B C16B 119.1(8) . . ? C14B C15B H15B 120.4 . . ? C16B C15B H15B 120.4 . . ? C17B C16B C15B 120.9(8) . . ? C17B C16B H16B 119.6 . . ? C15B C16B H16B 119.6 . . ? C16B C17B C18B 120.3(7) . . ? C16B C17B H17B 119.8 . . ? C18B C17B H17B 119.8 . . ? C17B C18B C13B 118.8(7) . . ? C17B C18B H18B 120.6 . . ? C13B C18B H18B 120.6 . . ? C20B C19B C24B 118.5(7) . . ? C20B C19B C3B 121.7(7) . . ? C24B C19B C3B 119.8(7) . . ? C21B C20B C19B 121.1(8) . . ? C21B C20B H20B 119.5 . . ? C19B C20B H20B 119.5 . . ? C20B C21B C22B 120.5(8) . . ? C20B C21B H21B 119.8 . . ? C22B C21B H21B 119.8 . . ? C23B C22B C21B 119.4(8) . . ? C23B C22B H22B 120.3 . . ? C21B C22B H22B 120.3 . . ? C22B C23B C24B 120.8(8) . . ? C22B C23B H23B 119.6 . . ? C24B C23B H23B 119.6 . . ? C23B C24B C19B 119.7(7) . . ? C23B C24B H24B 120.2 . . ? C19B C24B H24B 120.2 . . ? C30B C25B C26B 119.4(7) . . ? C30B C25B C4B 121.6(7) . . ? C26B C25B C4B 119.0(7) . . ? C27B C26B C25B 118.0(8) . . ? C27B C26B H26B 121.0 . . ? C25B C26B H26B 121.0 . . ? C28B C27B C26B 121.5(8) . . ? C28B C27B H27B 119.3 . . ? C26B C27B H27B 119.3 . . ? C27B C28B C29B 121.2(9) . . ? C27B C28B H28B 119.4 . . ? C29B C28B H28B 119.4 . . ? C30B C29B C28B 118.0(9) . . ? C30B C29B H29B 121.0 . . ? C28B C29B H29B 121.0 . . ? C29B C30B C25B 121.9(8) . . ? C29B C30B H30B 119.1 . . ? C25B C30B H30B 119.1 . . ? N7B C31B C5B 177.1(9) . . ? C6S C1S C2S 113.5(15) . . ? C6S C1S H1SA 123.3 . . ? C2S C1S H1SA 123.3 . . ? C3S C2S C1S 126.7(19) . . ? C3S C2S H2SA 116.6 . . ? C1S C2S H2SA 116.6 . . ? C2S C3S C4S 112(2) . . ? C2S C3S H3SA 123.9 . . ? C4S C3S H3SA 123.9 . . ? C5S C4S C3S 124(2) . . ? C5S C4S H4SA 117.9 . . ? C3S C4S H4SA 117.9 . . ? C4S C5S C6S 126.5(18) . . ? C4S C5S H5SA 116.8 . . ? C6S C5S H5SA 116.8 . . ? C1S C6S C5S 117.0(15) . . ? C1S C6S H6SA 121.5 . . ? C5S C6S H6SA 121.5 . . ? C12S C7S C8S 117.3(12) . . ? C12S C7S H7SA 121.3 . . ? C8S C7S H7SA 121.3 . . ? C9S C8S C7S 123.4(13) . . ? C9S C8S H8SA 118.3 . . ? C7S C8S H8SA 118.3 . . ? C8S C9S C10S 117.9(12) . . ? C8S C9S H9SA 121.0 . . ? C10S C9S H9SA 121.0 . . ? C9S C10S C11S 120.2(11) . . ? C9S C10S H10C 119.9 . . ? C11S C10S H10C 119.9 . . ? C12S C11S C10S 119.7(12) . . ? C12S C11S H11C 120.2 . . ? C10S C11S H11C 120.2 . . ? C11S C12S C7S 121.3(12) . . ? C11S C12S H12C 119.4 . . ? C7S C12S H12C 119.4 . . ? C14S C13S C18S 123.9(11) . . ? C14S C13S H13A 118.0 . . ? C18S C13S H13A 118.0 . . ? C13S C14S C15S 118.3(12) . . ? C13S C14S H14C 120.9 . . ? C15S C14S H14C 120.9 . . ? C16S C15S C14S 121.2(11) . . ? C16S C15S H15C 119.4 . . ? C14S C15S H15C 119.4 . . ? C15S C16S C17S 117.9(10) . . ? C15S C16S H16C 121.0 . . ? C17S C16S H16C 121.0 . . ? C16S C17S C18S 121.8(11) . . ? C16S C17S H17C 119.1 . . ? C18S C17S H17C 119.1 . . ? C13S C18S C17S 116.8(10) . . ? C13S C18S H18C 121.6 . . ? C17S C18S H18C 121.6 . . ? C20S C19S C24S 124.4(19) . . ? C20S C19S H19A 117.8 . . ? C24S C19S H19A 117.8 . . ? C19S C20S C21S 119.8(15) . . ? C19S C20S H20C 120.1 . . ? C21S C20S H20C 120.1 . . ? C20S C21S C22S 121.6(13) . . ? C20S C21S H21C 119.2 . . ? C22S C21S H21C 119.2 . . ? C21S C22S C23S 117.3(14) . . ? C21S C22S H22C 121.4 . . ? C23S C22S H22C 121.4 . . ? C22S C23S C24S 118.6(17) . . ? C22S C23S H23C 120.7 . . ? C24S C23S H23C 120.7 . . ? C19S C24S C23S 118.3(19) . . ? C19S C24S H24C 120.9 . . ? C23S C24S H24C 120.9 . . ? C26S C25S C30S 120.1(9) . . ? C26S C25S H25A 119.9 . . ? C30S C25S H25A 119.9 . . ? C25S C26S C27S 120.1(10) . . ? C25S C26S H26C 120.0 . . ? C27S C26S H26C 120.0 . . ? C28S C27S C26S 121.0(10) . . ? C28S C27S H27C 119.5 . . ? C26S C27S H27C 119.5 . . ? C29S C28S C27S 120.5(9) . . ? C29S C28S H28C 119.8 . . ? C27S C28S H28C 119.8 . . ? C28S C29S C30S 119.2(9) . . ? C28S C29S H29C 120.4 . . ? C30S C29S H29C 120.4 . . ? C25S C30S C29S 119.2(9) . . ? C25S C30S H30C 120.4 . . ? C29S C30S H30C 120.4 . . ? 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 N5A Fe1A N1A C1A 157.3(6) . . . . ? N6A Fe1A N1A C1A 81.7(6) . . . . ? N4A Fe1A N1A C1A -55.8(8) . . . . ? N2A Fe1A N1A C1A 2.7(5) . . . . ? N3A Fe1A N1A C1A -115.6(6) . . . . ? N5A Fe1A N1A O1A -37.6(5) . . . . ? N6A Fe1A N1A O1A -113.1(5) . . . . ? N4A Fe1A N1A O1A 109.3(6) . . . . ? N2A Fe1A N1A O1A 167.8(5) . . . . ? N3A Fe1A N1A O1A 49.5(5) . . . . ? N5A Fe1A N2A C2A -55.2(8) . . . . ? N6A Fe1A N2A C2A -115.4(6) . . . . ? N1A Fe1A N2A C2A 2.3(5) . . . . ? N4A Fe1A N2A C2A 157.5(6) . . . . ? N3A Fe1A N2A C2A 83.2(6) . . . . ? N5A Fe1A N2A O2A 111.3(6) . . . . ? N6A Fe1A N2A O2A 51.1(5) . . . . ? N1A Fe1A N2A O2A 168.8(5) . . . . ? N4A Fe1A N2A O2A -36.0(5) . . . . ? N3A Fe1A N2A O2A -110.3(5) . . . . ? N5A Fe1A N3A C3A -116.7(6) . . . . ? N6A Fe1A N3A C3A -55.7(9) . . . . ? N1A Fe1A N3A C3A 158.1(6) . . . . ? N4A Fe1A N3A C3A 3.8(5) . . . . ? N2A Fe1A N3A C3A 83.1(6) . . . . ? N5A Fe1A N3A O3A 47.8(5) . . . . ? N6A Fe1A N3A O3A 108.7(6) . . . . ? N1A Fe1A N3A O3A -37.5(5) . . . . ? N4A Fe1A N3A O3A 168.2(5) . . . . ? N2A Fe1A N3A O3A -112.5(5) . . . . ? N5A Fe1A N4A C4A 84.5(6) . . . . ? N6A Fe1A N4A C4A 160.4(6) . . . . ? N1A Fe1A N4A C4A -57.1(8) . . . . ? N2A Fe1A N4A C4A -113.7(6) . . . . ? N3A Fe1A N4A C4A 5.0(5) . . . . ? N5A Fe1A N4A O4A -111.3(5) . . . . ? N6A Fe1A N4A O4A -35.5(5) . . . . ? N1A Fe1A N4A O4A 107.1(6) . . . . ? N2A Fe1A N4A O4A 50.4(5) . . . . ? N3A Fe1A N4A O4A 169.1(5) . . . . ? N6A Fe1A N5A C5A 4.3(5) . . . . ? N1A Fe1A N5A C5A -113.2(5) . . . . ? N4A Fe1A N5A C5A 84.5(6) . . . . ? N2A Fe1A N5A C5A -57.4(8) . . . . ? N3A Fe1A N5A C5A 158.9(5) . . . . ? N6A Fe1A N5A O5A 170.8(5) . . . . ? N1A Fe1A N5A O5A 53.2(5) . . . . ? N4A Fe1A N5A O5A -109.0(5) . . . . ? N2A Fe1A N5A O5A 109.1(6) . . . . ? N3A Fe1A N5A O5A -34.6(5) . . . . ? N5A Fe1A N6A C6A -2.1(5) . . . . ? N1A Fe1A N6A C6A 77.0(5) . . . . ? N4A Fe1A N6A C6A -122.3(5) . . . . ? N2A Fe1A N6A C6A 151.3(5) . . . . ? N3A Fe1A N6A C6A -64.8(8) . . . . ? N5A Fe1A N6A O6A 170.3(5) . . . . ? N1A Fe1A N6A O6A -110.5(5) . . . . ? N4A Fe1A N6A O6A 50.1(5) . . . . ? N2A Fe1A N6A O6A -36.3(5) . . . . ? N3A Fe1A N6A O6A 107.6(7) . . . . ? C1A N1A O1A B1A 154.2(6) . . . . ? Fe1A N1A O1A B1A -11.7(8) . . . . ? F1A B1A O1A N1A -174.9(6) . . . . ? O3A B1A O1A N1A -55.9(8) . . . . ? O5A B1A O1A N1A 70.8(8) . . . . ? C2A N2A O2A B2A 152.7(6) . . . . ? Fe1A N2A O2A B2A -14.1(7) . . . . ? F2A B2A O2A N2A -174.1(5) . . . . ? O6A B2A O2A N2A -54.0(7) . . . . ? O4A B2A O2A N2A 72.0(7) . . . . ? C3A N3A O3A B1A 152.7(7) . . . . ? Fe1A N3A O3A B1A -11.7(7) . . . . ? F1A B1A O3A N3A -175.5(5) . . . . ? O5A B1A O3A N3A -54.6(8) . . . . ? O1A B1A O3A N3A 68.9(8) . . . . ? C4A N4A O4A B2A 153.2(6) . . . . ? Fe1A N4A O4A B2A -11.6(7) . . . . ? F2A B2A O4A N4A -173.6(5) . . . . ? O6A B2A O4A N4A 68.4(7) . . . . ? O2A B2A O4A N4A -57.7(8) . . . . ? C5A N5A O5A B1A 155.5(6) . . . . ? Fe1A N5A O5A B1A -11.4(7) . . . . ? F1A B1A O5A N5A -170.2(6) . . . . ? O3A B1A O5A N5A 67.4(8) . . . . ? O1A B1A O5A N5A -58.1(8) . . . . ? C6A N6A O6A B2A 160.9(6) . . . . ? Fe1A N6A O6A B2A -11.7(7) . . . . ? F2A B2A O6A N6A -171.6(5) . . . . ? O2A B2A O6A N6A 68.9(7) . . . . ? O4A B2A O6A N6A -56.0(7) . . . . ? O1A N1A C1A C2A -172.6(5) . . . . ? Fe1A N1A C1A C2A -6.3(8) . . . . ? O1A N1A C1A C7A 2.1(10) . . . . ? Fe1A N1A C1A C7A 168.4(5) . . . . ? O2A N2A C2A C1A -173.5(5) . . . . ? Fe1A N2A C2A C1A -6.1(8) . . . . ? O2A N2A C2A C13A -0.7(10) . . . . ? Fe1A N2A C2A C13A 166.7(6) . . . . ? N1A C1A C2A N2A 7.7(9) . . . . ? C7A C1A C2A N2A -167.2(6) . . . . ? N1A C1A C2A C13A -165.4(6) . . . . ? C7A C1A C2A C13A 19.8(11) . . . . ? O3A N3A C3A C4A -175.5(6) . . . . ? Fe1A N3A C3A C4A -10.8(8) . . . . ? O3A N3A C3A C19A -3.9(10) . . . . ? Fe1A N3A C3A C19A 160.9(6) . . . . ? O4A N4A C4A C3A -176.6(5) . . . . ? Fe1A N4A C4A C3A -11.3(8) . . . . ? O4A N4A C4A C25A -3.1(10) . . . . ? Fe1A N4A C4A C25A 162.3(6) . . . . ? N3A C3A C4A N4A 13.7(9) . . . . ? C19A C3A C4A N4A -158.1(7) . . . . ? N3A C3A C4A C25A -160.0(7) . . . . ? C19A C3A C4A C25A 28.2(11) . . . . ? O5A N5A C5A C6A -173.8(5) . . . . ? Fe1A N5A C5A C6A -5.7(8) . . . . ? O5A N5A C5A C31A 3.8(10) . . . . ? Fe1A N5A C5A C31A 171.9(7) . . . . ? O6A N6A C6A C32A 4.2(12) . . . . ? Fe1A N6A C6A C32A 177.2(8) . . . . ? O6A N6A C6A C5A -173.3(6) . . . . ? Fe1A N6A C6A C5A -0.3(8) . . . . ? N5A C5A C6A N6A 3.7(9) . . . . ? C31A C5A C6A N6A -174.0(7) . . . . ? N5A C5A C6A C32A -174.0(9) . . . . ? N1A C1A C7A C8A -126.6(8) . . . . ? C2A C1A C7A C8A 47.4(10) . . . . ? N1A C1A C7A C12A 50.8(10) . . . . ? C2A C1A C7A C12A -135.2(7) . . . . ? C12A C7A C8A C9A -2.3(10) . . . . ? C1A C7A C8A C9A 175.0(6) . . . . ? C7A C8A C9A C10A 0.8(11) . . . . ? C8A C9A C10A C11A 1.7(11) . . . . ? C9A C10A C11A C12A -2.5(11) . . . . ? C8A C7A C12A C11A 1.5(10) . . . . ? C1A C7A C12A C11A -175.8(6) . . . . ? C10A C11A C12A C7A 0.9(10) . . . . ? N2A C2A C13A C18A 63.7(11) . . . . ? C1A C2A C13A C18A -124.1(8) . . . . ? N2A C2A C13A C14A -115.9(8) . . . . ? C1A C2A C13A C14A 56.3(10) . . . . ? C18A C13A C14A C15A -0.4(12) . . . . ? C2A C13A C14A C15A 179.2(7) . . . . ? C13A C14A C15A C16A 0.4(14) . . . . ? C14A C15A C16A C17A 1.4(15) . . . . ? C15A C16A C17A C18A -3.2(14) . . . . ? C14A C13A C18A C17A -1.4(12) . . . . ? C2A C13A C18A C17A 179.0(7) . . . . ? C16A C17A C18A C13A 3.1(13) . . . . ? N3A C3A C19A C24A -134.2(8) . . . . ? C4A C3A C19A C24A 36.8(12) . . . . ? N3A C3A C19A C20A 42.0(12) . . . . ? C4A C3A C19A C20A -147.0(8) . . . . ? C24A C19A C20A C21A 0.2(14) . . . . ? C3A C19A C20A C21A -176.0(8) . . . . ? C19A C20A C21A C22A 1.1(15) . . . . ? C20A C21A C22A C23A -1.2(17) . . . . ? C21A C22A C23A C24A -0.1(16) . . . . ? C20A C19A C24A C23A -1.5(14) . . . . ? C3A C19A C24A C23A 174.7(8) . . . . ? C22A C23A C24A C19A 1.5(15) . . . . ? N4A C4A C25A C26A -132.2(8) . . . . ? C3A C4A C25A C26A 40.4(10) . . . . ? N4A C4A C25A C30A 48.2(11) . . . . ? C3A C4A C25A C30A -139.2(8) . . . . ? C30A C25A C26A C27A -2.2(11) . . . . ? C4A C25A C26A C27A 178.2(7) . . . . ? C25A C26A C27A C28A 1.6(12) . . . . ? C26A C27A C28A C29A 0.2(12) . . . . ? C27A C28A C29A C30A -1.2(12) . . . . ? C28A C29A C30A C25A 0.6(12) . . . . ? C26A C25A C30A C29A 1.2(11) . . . . ? C4A C25A C30A C29A -179.3(7) . . . . ? N2B Fe1B N1B C1B -6.1(6) . . . . ? N3B Fe1B N1B C1B -162.2(6) . . . . ? N5B Fe1B N1B C1B 110.9(6) . . . . ? N4B Fe1B N1B C1B -87.0(6) . . . . ? N6B Fe1B N1B C1B 52.8(9) . . . . ? N2B Fe1B N1B O1B -166.2(6) . . . . ? N3B Fe1B N1B O1B 37.8(5) . . . . ? N5B Fe1B N1B O1B -49.1(5) . . . . ? N4B Fe1B N1B O1B 112.9(5) . . . . ? N6B Fe1B N1B O1B -107.2(7) . . . . ? N3B Fe1B N2B C2B 59.3(8) . . . . ? N5B Fe1B N2B C2B -79.0(6) . . . . ? N4B Fe1B N2B C2B 117.6(6) . . . . ? N6B Fe1B N2B C2B -155.4(6) . . . . ? N1B Fe1B N2B C2B 0.3(6) . . . . ? N3B Fe1B N2B O2B -109.8(6) . . . . ? N5B Fe1B N2B O2B 111.9(5) . . . . ? N4B Fe1B N2B O2B -51.5(5) . . . . ? N6B Fe1B N2B O2B 35.5(5) . . . . ? N1B Fe1B N2B O2B -168.8(6) . . . . ? N2B Fe1B N3B C3B 58.5(8) . . . . ? N5B Fe1B N3B C3B -158.5(5) . . . . ? N4B Fe1B N3B C3B -1.6(5) . . . . ? N6B Fe1B N3B C3B -82.0(6) . . . . ? N1B Fe1B N3B C3B 116.0(5) . . . . ? N2B Fe1B N3B O3B -110.1(6) . . . . ? N5B Fe1B N3B O3B 32.9(5) . . . . ? N4B Fe1B N3B O3B -170.1(5) . . . . ? N6B Fe1B N3B O3B 109.5(5) . . . . ? N1B Fe1B N3B O3B -52.6(5) . . . . ? N2B Fe1B N4B C4B -159.4(5) . . . . ? N3B Fe1B N4B C4B -3.6(5) . . . . ? N5B Fe1B N4B C4B 54.7(8) . . . . ? N6B Fe1B N4B C4B 114.6(5) . . . . ? N1B Fe1B N4B C4B -83.4(5) . . . . ? N2B Fe1B N4B O4B 35.5(5) . . . . ? N3B Fe1B N4B O4B -168.7(5) . . . . ? N5B Fe1B N4B O4B -110.4(7) . . . . ? N6B Fe1B N4B O4B -50.5(5) . . . . ? N1B Fe1B N4B O4B 111.5(5) . . . . ? N2B Fe1B N5B O5B 112.9(5) . . . . ? N3B Fe1B N5B O5B -48.8(5) . . . . ? N4B Fe1B N5B O5B -105.5(7) . . . . ? N6B Fe1B N5B O5B -166.9(5) . . . . ? N1B Fe1B N5B O5B 37.5(5) . . . . ? N2B Fe1B N5B C5B -79.8(5) . . . . ? N3B Fe1B N5B C5B 118.6(5) . . . . ? N4B Fe1B N5B C5B 61.8(8) . . . . ? N6B Fe1B N5B C5B 0.4(5) . . . . ? N1B Fe1B N5B C5B -155.2(5) . . . . ? N2B Fe1B N6B C6B 111.4(6) . . . . ? N3B Fe1B N6B C6B -86.1(6) . . . . ? N5B Fe1B N6B C6B -5.4(6) . . . . ? N4B Fe1B N6B C6B -161.5(6) . . . . ? N1B Fe1B N6B C6B 53.9(9) . . . . ? N2B Fe1B N6B O6B -52.2(5) . . . . ? N3B Fe1B N6B O6B 110.2(5) . . . . ? N5B Fe1B N6B O6B -169.0(5) . . . . ? N4B Fe1B N6B O6B 34.8(5) . . . . ? N1B Fe1B N6B O6B -109.7(7) . . . . ? C1B N1B O1B B1B -149.2(7) . . . . ? Fe1B N1B O1B B1B 11.0(8) . . . . ? F1B B1B O1B N1B 174.2(6) . . . . ? O5B B1B O1B N1B 55.7(8) . . . . ? O3B B1B O1B N1B -67.3(8) . . . . ? C2B N2B O2B B2B -157.0(6) . . . . ? Fe1B N2B O2B B2B 12.7(8) . . . . ? F2B B2B O2B N2B 171.3(6) . . . . ? O6B B2B O2B N2B -68.9(7) . . . . ? O4B B2B O2B N2B 55.1(8) . . . . ? C3B N3B O3B B1B -154.7(6) . . . . ? Fe1B N3B O3B B1B 14.5(7) . . . . ? F1B B1B O3B N3B 173.3(6) . . . . ? O1B B1B O3B N3B 53.4(7) . . . . ? O5B B1B O3B N3B -69.9(8) . . . . ? C4B N4B O4B B2B -152.1(6) . . . . ? Fe1B N4B O4B B2B 13.4(7) . . . . ? F2B B2B O4B N4B 174.3(5) . . . . ? O6B B2B O4B N4B 55.1(7) . . . . ? O2B B2B O4B N4B -69.6(8) . . . . ? C5B N5B O5B B1B -157.5(6) . . . . ? Fe1B N5B O5B B1B 10.2(7) . . . . ? F1B B1B O5B N5B 173.0(6) . . . . ? O1B B1B O5B N5B -67.1(7) . . . . ? O3B B1B O5B N5B 56.3(8) . . . . ? C6B N6B O6B B2B -148.4(7) . . . . ? Fe1B N6B O6B B2B 15.1(7) . . . . ? F2B B2B O6B N6B 171.5(5) . . . . ? O2B B2B O6B N6B 53.1(8) . . . . ? O4B B2B O6B N6B -70.7(7) . . . . ? O1B N1B C1B C2B 171.5(6) . . . . ? Fe1B N1B C1B C2B 10.3(9) . . . . ? O1B N1B C1B C7B -4.9(10) . . . . ? Fe1B N1B C1B C7B -166.1(6) . . . . ? O2B N2B C2B C1B 174.9(6) . . . . ? Fe1B N2B C2B C1B 4.7(8) . . . . ? O2B N2B C2B C13B -6.9(10) . . . . ? Fe1B N2B C2B C13B -177.1(6) . . . . ? N1B C1B C2B N2B -9.2(9) . . . . ? C7B C1B C2B N2B 167.1(7) . . . . ? N1B C1B C2B C13B 172.6(7) . . . . ? C7B C1B C2B C13B -11.0(12) . . . . ? O3B N3B C3B C4B 175.3(5) . . . . ? Fe1B N3B C3B C4B 5.6(7) . . . . ? O3B N3B C3B C19B -2.0(9) . . . . ? Fe1B N3B C3B C19B -171.7(5) . . . . ? O4B N4B C4B C3B 173.5(5) . . . . ? Fe1B N4B C4B C3B 7.5(8) . . . . ? O4B N4B C4B C25B -5.5(10) . . . . ? Fe1B N4B C4B C25B -171.5(5) . . . . ? N3B C3B C4B N4B -8.0(8) . . . . ? C19B C3B C4B N4B 169.3(6) . . . . ? N3B C3B C4B C25B 171.0(6) . . . . ? C19B C3B C4B C25B -11.7(10) . . . . ? O5B N5B C5B C6B 172.9(6) . . . . ? Fe1B N5B C5B C6B 3.9(8) . . . . ? O5B N5B C5B C31B -7.9(10) . . . . ? Fe1B N5B C5B C31B -176.8(6) . . . . ? O6B N6B C6B C5B 173.4(5) . . . . ? Fe1B N6B C6B C5B 9.0(9) . . . . ? N5B C5B C6B N6B -8.2(10) . . . . ? C31B C5B C6B N6B 172.6(8) . . . . ? N1B C1B C7B C8B -52.9(11) . . . . ? C2B C1B C7B C8B 131.1(8) . . . . ? N1B C1B C7B C12B 131.4(9) . . . . ? C2B C1B C7B C12B -44.6(12) . . . . ? C12B C7B C8B C9B -2.8(12) . . . . ? C1B C7B C8B C9B -178.5(7) . . . . ? C7B C8B C9B C10B 0.4(13) . . . . ? C8B C9B C10B C11B 1.8(14) . . . . ? C9B C10B C11B C12B -1.6(14) . . . . ? C8B C7B C12B C11B 3.0(13) . . . . ? C1B C7B C12B C11B 178.8(8) . . . . ? C10B C11B C12B C7B -0.8(14) . . . . ? N2B C2B C13B C14B -44.6(12) . . . . ? C1B C2B C13B C14B 133.3(8) . . . . ? N2B C2B C13B C18B 138.8(8) . . . . ? C1B C2B C13B C18B -43.4(11) . . . . ? C18B C13B C14B C15B 1.0(12) . . . . ? C2B C13B C14B C15B -175.6(7) . . . . ? C13B C14B C15B C16B -0.8(12) . . . . ? C14B C15B C16B C17B -0.5(13) . . . . ? C15B C16B C17B C18B 1.6(13) . . . . ? C16B C17B C18B C13B -1.4(12) . . . . ? C14B C13B C18B C17B 0.2(11) . . . . ? C2B C13B C18B C17B 176.9(7) . . . . ? N3B C3B C19B C20B -48.7(10) . . . . ? C4B C3B C19B C20B 134.3(7) . . . . ? N3B C3B C19B C24B 131.9(7) . . . . ? C4B C3B C19B C24B -45.1(10) . . . . ? C24B C19B C20B C21B 1.0(11) . . . . ? C3B C19B C20B C21B -178.4(7) . . . . ? C19B C20B C21B C22B -1.8(12) . . . . ? C20B C21B C22B C23B 1.4(12) . . . . ? C21B C22B C23B C24B -0.2(12) . . . . ? C22B C23B C24B C19B -0.5(11) . . . . ? C20B C19B C24B C23B 0.1(10) . . . . ? C3B C19B C24B C23B 179.6(6) . . . . ? N4B C4B C25B C30B -48.5(11) . . . . ? C3B C4B C25B C30B 132.7(7) . . . . ? N4B C4B C25B C26B 130.9(7) . . . . ? C3B C4B C25B C26B -48.0(9) . . . . ? C30B C25B C26B C27B -1.8(11) . . . . ? C4B C25B C26B C27B 178.9(7) . . . . ? C25B C26B C27B C28B 0.3(12) . . . . ? C26B C27B C28B C29B -0.5(14) . . . . ? C27B C28B C29B C30B 2.1(13) . . . . ? C28B C29B C30B C25B -3.6(12) . . . . ? C26B C25B C30B C29B 3.5(12) . . . . ? C4B C25B C30B C29B -177.1(7) . . . . ? N5B C5B C31B N7B -4(22) . . . . ? C6B C5B C31B N7B 175(100) . . . . ? C6S C1S C2S C3S -2(2) . . . . ? C1S C2S C3S C4S 0(3) . . . . ? C2S C3S C4S C5S 0(3) . . . . ? C3S C4S C5S C6S 0(3) . . . . ? C2S C1S C6S C5S 2.3(17) . . . . ? C4S C5S C6S C1S -2(2) . . . . ? C12S C7S C8S C9S 0(2) . . . . ? C7S C8S C9S C10S -4(2) . . . . ? C8S C9S C10S C11S 3.8(18) . . . . ? C9S C10S C11S C12S -0.4(17) . . . . ? C10S C11S C12S C7S -3.6(18) . . . . ? C8S C7S C12S C11S 4(2) . . . . ? C18S C13S C14S C15S -3.5(18) . . . . ? C13S C14S C15S C16S 3.6(17) . . . . ? C14S C15S C16S C17S -1.7(16) . . . . ? C15S C16S C17S C18S -0.3(15) . . . . ? C14S C13S C18S C17S 1.6(18) . . . . ? C16S C17S C18S C13S 0.4(15) . . . . ? C24S C19S C20S C21S 3(2) . . . . ? C19S C20S C21S C22S -2.3(16) . . . . ? C20S C21S C22S C23S 1.3(15) . . . . ? C21S C22S C23S C24S -0.7(16) . . . . ? C20S C19S C24S C23S -2(2) . . . . ? C22S C23S C24S C19S 1(2) . . . . ? C30S C25S C26S C27S 0.7(17) . . . . ? C25S C26S C27S C28S -2.5(17) . . . . ? C26S C27S C28S C29S 3.2(17) . . . . ? C27S C28S C29S C30S -2.2(16) . . . . ? C26S C25S C30S C29S 0.2(16) . . . . ? C28S C29S C30S C25S 0.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.681 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.093 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick (2008). Sheldrick G.M.,Acta Cryst.(2008),A64,112-122. ; # Attachment '- Diiodoclt.cif' data_fi _database_code_depnum_ccdc_archive 'CCDC 816072' #TrackingRef '- Diiodoclt.cif' _vrf_THETM01_fi ; PROBLEM:The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5498 RESPONSE:The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT431_fi ; PROBLEM:Short Inter HL..A Contact I1...F1 2.94 Ang. RESPONSE: In crystal complex molecules form centrosymmetrical dimers and this contact correcpond to attractive interaction. ; _vrf_PLAT023_fi ; PROBLEM:Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.00 Deg. RESPONSE:The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _vrf_PLAT029_fi ; PROBLEM:diffrn_measured_fraction_theta_full Low 0.94 RESPONSE:The reason is related to very weak reflection ability of the single crystal samples which were obtained in a form of thin plates. Therefore significant part of the reflections included in the refinement procedure are very weak ones which are measured with lower precision than the strong ones. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 B2 F2 Fe I2 N6 O6, 2(C6 H6)' _chemical_formula_sum 'C42 H32 B2 F2 Fe I2 N6 O6' _chemical_formula_weight 1086.01 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.266(4) _cell_length_b 10.531(3) _cell_length_c 27.206(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.307(5) _cell_angle_gamma 90.00 _cell_volume 4372.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 494 _cell_measurement_theta_min 3 _cell_measurement_theta_max 23 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27556 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5741 _reflns_number_gt 4549 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0091P)^2^+135.0691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5741 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.37276(4) 1.51506(7) 0.03495(2) 0.0252(2) Uani 1 1 d . . . I2 I 0.12429(4) 1.50536(8) 0.03587(3) 0.0296(2) Uani 1 1 d . . . Fe1 Fe 0.24588(10) 1.29906(14) -0.10334(5) 0.0205(4) Uani 1 1 d . . . O1 O 0.4142(4) 1.3535(7) -0.0576(3) 0.0243(17) Uani 1 1 d . . . O2 O 0.0782(4) 1.3744(7) -0.0643(3) 0.0233(17) Uani 1 1 d . . . O3 O 0.3960(4) 1.4266(7) -0.1425(3) 0.0234(17) Uani 1 1 d . . . O4 O 0.0738(4) 1.2925(7) -0.1499(3) 0.0272(18) Uani 1 1 d . . . O5 O 0.4170(4) 1.1999(7) -0.1255(3) 0.0292(19) Uani 1 1 d . . . O6 O 0.0944(4) 1.1467(7) -0.0803(3) 0.0256(18) Uani 1 1 d . . . N1 N 0.3247(5) 1.3584(8) -0.0533(3) 0.020(2) Uani 1 1 d . . . N2 N 0.1674(5) 1.3828(8) -0.0601(3) 0.0184(19) Uani 1 1 d . . . N3 N 0.3083(5) 1.4062(9) -0.1472(3) 0.025(2) Uani 1 1 d . . . N4 N 0.1605(5) 1.3248(9) -0.1548(3) 0.023(2) Uani 1 1 d . . . N5 N 0.3310(5) 1.1721(9) -0.1166(3) 0.024(2) Uani 1 1 d . . . N6 N 0.1827(5) 1.1471(9) -0.0883(3) 0.023(2) Uani 1 1 d . . . F1 F 0.5267(4) 1.3464(6) -0.1113(2) 0.0324(16) Uani 1 1 d . . . F2 F -0.0354(4) 1.2539(7) -0.0962(2) 0.0354(16) Uani 1 1 d . . . B1 B 0.4392(8) 1.3327(13) -0.1084(5) 0.027(3) Uani 1 1 d . . . B2 B 0.0520(8) 1.2663(14) -0.0993(5) 0.028(3) Uani 1 1 d . . . C1 C 0.2948(6) 1.4270(9) -0.0174(4) 0.016(2) Uani 1 1 d . . . C2 C 0.1995(7) 1.4318(10) -0.0199(4) 0.022(2) Uani 1 1 d . . . C3 C 0.2695(7) 1.4346(10) -0.1903(4) 0.023(2) Uani 1 1 d . . . C4 C 0.1797(7) 1.3962(11) -0.1930(4) 0.026(3) Uani 1 1 d . . . C5 C 0.3118(7) 1.0518(11) -0.1084(4) 0.025(3) Uani 1 1 d . . . C6 C 0.2210(7) 1.0387(11) -0.0949(4) 0.024(3) Uani 1 1 d . . . C7 C 0.3158(5) 1.5010(7) -0.2305(2) 0.031(3) Uani 1 1 d G . . C8 C 0.3051(5) 1.4537(6) -0.2780(3) 0.034(3) Uani 1 1 d G . . H8A H 0.2736 1.3770 -0.2835 0.041 Uiso 1 1 calc R . . C9 C 0.3404(5) 1.5187(8) -0.3174(2) 0.042(3) Uani 1 1 d G . . H9A H 0.3331 1.4864 -0.3498 0.051 Uiso 1 1 calc R . . C10 C 0.3864(5) 1.6309(8) -0.3093(3) 0.054(4) Uani 1 1 d G . . H10B H 0.4105 1.6754 -0.3362 0.065 Uiso 1 1 calc R . . C11 C 0.3971(5) 1.6782(7) -0.2618(3) 0.050(4) Uani 1 1 d G . . H11A H 0.4285 1.7549 -0.2563 0.060 Uiso 1 1 calc R . . C12 C 0.3618(5) 1.6132(7) -0.2224(2) 0.040(3) Uani 1 1 d G . . H12B H 0.3691 1.6455 -0.1900 0.048 Uiso 1 1 calc R . . C13 C 0.1184(4) 1.4282(7) -0.2343(2) 0.029(3) Uani 1 1 d G . . C14 C 0.0722(5) 1.3322(6) -0.2585(3) 0.035(3) Uani 1 1 d G . . H14A H 0.0750 1.2476 -0.2465 0.043 Uiso 1 1 calc R . . C15 C 0.0220(5) 1.3601(7) -0.3004(3) 0.048(4) Uani 1 1 d G . . H15A H -0.0096 1.2945 -0.3170 0.057 Uiso 1 1 calc R . . C16 C 0.0179(5) 1.4839(8) -0.3180(2) 0.048(4) Uani 1 1 d G . . H16A H -0.0165 1.5030 -0.3466 0.058 Uiso 1 1 calc R . . C17 C 0.0640(5) 1.5799(6) -0.2937(3) 0.045(4) Uani 1 1 d G . . H17A H 0.0612 1.6645 -0.3057 0.055 Uiso 1 1 calc R . . C18 C 0.1143(5) 1.5520(6) -0.2519(3) 0.040(3) Uani 1 1 d G . . H18A H 0.1458 1.6176 -0.2353 0.048 Uiso 1 1 calc R . . C19 C 0.3771(4) 0.9466(6) -0.1103(3) 0.029(3) Uani 1 1 d G . . C20 C 0.3786(5) 0.8557(7) -0.0732(2) 0.036(3) Uani 1 1 d G . . H20A H 0.3406 0.8635 -0.0462 0.043 Uiso 1 1 calc R . . C21 C 0.4358(5) 0.7533(6) -0.0757(3) 0.043(3) Uani 1 1 d G . . H21A H 0.4369 0.6911 -0.0504 0.051 Uiso 1 1 calc R . . C22 C 0.4914(5) 0.7418(6) -0.1152(3) 0.042(3) Uani 1 1 d G . . H22A H 0.5305 0.6718 -0.1169 0.050 Uiso 1 1 calc R . . C23 C 0.4899(4) 0.8327(7) -0.1522(3) 0.038(3) Uani 1 1 d G . . H23A H 0.5279 0.8249 -0.1792 0.045 Uiso 1 1 calc R . . C24 C 0.4327(5) 0.9351(6) -0.1498(2) 0.027(3) Uani 1 1 d G . . H24A H 0.4316 0.9973 -0.1751 0.033 Uiso 1 1 calc R . . C25 C 0.1746(5) 0.9133(5) -0.0917(3) 0.029(3) Uani 1 1 d G . . C26 C 0.1149(5) 0.8913(6) -0.0548(2) 0.030(3) Uani 1 1 d G . . H26A H 0.1037 0.9555 -0.0313 0.036 Uiso 1 1 calc R . . C27 C 0.0716(5) 0.7754(7) -0.0525(3) 0.045(4) Uani 1 1 d G . . H27A H 0.0308 0.7604 -0.0273 0.054 Uiso 1 1 calc R . . C28 C 0.0881(5) 0.6815(6) -0.0869(3) 0.044(4) Uani 1 1 d G . . H28A H 0.0585 0.6023 -0.0853 0.053 Uiso 1 1 calc R . . C29 C 0.1478(5) 0.7035(6) -0.1238(3) 0.035(3) Uani 1 1 d G . . H29A H 0.1591 0.6393 -0.1474 0.042 Uiso 1 1 calc R . . C30 C 0.1911(4) 0.8194(7) -0.1262(2) 0.034(3) Uani 1 1 d G . . H30A H 0.2319 0.8344 -0.1514 0.041 Uiso 1 1 calc R . . C1S C 0.2212(10) 0.9290(12) -0.3104(4) 0.099(7) Uani 1 1 d G . . H1SA H 0.1950 0.8711 -0.3331 0.119 Uiso 1 1 calc R . . C2S C 0.3057(9) 0.9733(13) -0.3178(4) 0.095(7) Uani 1 1 d G . . H2SA H 0.3371 0.9456 -0.3456 0.114 Uiso 1 1 calc R . . C3S C 0.3441(7) 1.0580(13) -0.2846(5) 0.084(6) Uani 1 1 d G . . H3SA H 0.4018 1.0883 -0.2897 0.101 Uiso 1 1 calc R . . C4S C 0.2980(9) 1.0985(10) -0.2440(4) 0.069(5) Uani 1 1 d G . . H4SA H 0.3243 1.1565 -0.2213 0.083 Uiso 1 1 calc R . . C5S C 0.2136(9) 1.0543(12) -0.2366(3) 0.079(6) Uani 1 1 d G . . H5SA H 0.1821 1.0820 -0.2088 0.094 Uiso 1 1 calc R . . C6S C 0.1752(7) 0.9695(14) -0.2698(5) 0.088(6) Uani 1 1 d G . . H6SA H 0.1174 0.9393 -0.2647 0.106 Uiso 1 1 calc R . . C7S C -0.2213(13) 0.8879(16) -0.0608(5) 0.135(11) Uani 1 1 d G . . H7SA H -0.1848 0.8151 -0.0626 0.162 Uiso 1 1 calc R . . C8S C -0.1865(8) 1.008(2) -0.0685(5) 0.103(7) Uani 1 1 d G . . H8SA H -0.1262 1.0174 -0.0756 0.123 Uiso 1 1 calc R . . C9S C -0.2399(13) 1.1146(14) -0.0657(4) 0.099(8) Uani 1 1 d G . . H9SA H -0.2161 1.1967 -0.0710 0.119 Uiso 1 1 calc R . . C10S C -0.3281(12) 1.1010(13) -0.0553(4) 0.106(8) Uani 1 1 d G . . H10A H -0.3646 1.1738 -0.0534 0.127 Uiso 1 1 calc R . . C11S C -0.3629(8) 0.9809(19) -0.0476(4) 0.090(6) Uani 1 1 d G . . H11B H -0.4232 0.9716 -0.0404 0.108 Uiso 1 1 calc R . . C12S C -0.3095(14) 0.8743(12) -0.0503(5) 0.110(10) Uani 1 1 d G . . H12A H -0.3332 0.7922 -0.0450 0.132 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0256(4) 0.0295(4) 0.0204(4) -0.0055(3) -0.0033(3) -0.0017(3) I2 0.0263(4) 0.0393(5) 0.0232(4) -0.0085(3) 0.0026(3) 0.0011(4) Fe1 0.0225(8) 0.0199(8) 0.0188(8) -0.0032(6) -0.0022(6) 0.0008(7) O1 0.013(4) 0.032(4) 0.028(4) -0.007(3) 0.000(3) 0.003(3) O2 0.018(4) 0.025(4) 0.027(4) -0.011(3) 0.004(3) -0.002(3) O3 0.015(4) 0.030(4) 0.024(4) 0.000(3) 0.000(3) -0.005(3) O4 0.011(4) 0.036(5) 0.035(5) -0.004(4) 0.001(3) -0.004(3) O5 0.013(4) 0.032(5) 0.043(5) -0.013(4) 0.002(3) -0.007(3) O6 0.013(4) 0.025(4) 0.038(5) -0.001(4) 0.006(3) -0.002(3) N1 0.015(5) 0.020(5) 0.024(5) -0.003(4) 0.000(4) 0.004(4) N2 0.021(5) 0.018(5) 0.016(5) -0.009(4) -0.003(4) 0.004(4) N3 0.013(5) 0.035(6) 0.026(5) 0.003(4) 0.004(4) 0.000(4) N4 0.011(5) 0.031(5) 0.027(5) -0.005(4) 0.000(4) 0.003(4) N5 0.017(5) 0.022(5) 0.034(5) -0.008(4) 0.005(4) -0.003(4) N6 0.015(5) 0.027(5) 0.027(5) -0.002(4) -0.001(4) -0.002(4) F1 0.020(3) 0.042(4) 0.035(4) -0.009(3) -0.001(3) 0.007(3) F2 0.021(3) 0.046(4) 0.039(4) -0.013(3) -0.004(3) 0.010(3) B1 0.019(7) 0.024(7) 0.038(8) -0.007(6) 0.011(6) -0.016(6) B2 0.006(6) 0.041(8) 0.038(8) -0.005(7) 0.008(5) -0.003(6) C1 0.021(6) 0.010(5) 0.018(5) 0.009(4) 0.000(4) -0.002(4) C2 0.020(6) 0.017(6) 0.029(6) 0.006(5) 0.004(5) 0.001(5) C3 0.023(6) 0.027(6) 0.018(6) -0.001(5) 0.003(5) -0.005(5) C4 0.027(6) 0.035(7) 0.017(6) 0.001(5) -0.002(5) -0.005(5) C5 0.018(6) 0.030(7) 0.026(6) 0.002(5) -0.001(5) -0.003(5) C6 0.019(6) 0.028(7) 0.024(6) -0.006(5) 0.000(5) -0.007(5) C7 0.023(6) 0.034(7) 0.037(7) -0.006(6) -0.004(5) 0.008(6) C8 0.036(7) 0.043(7) 0.023(6) 0.004(6) -0.001(5) 0.006(6) C9 0.035(7) 0.057(9) 0.034(7) 0.011(7) 0.003(6) 0.005(7) C10 0.036(8) 0.076(11) 0.049(9) 0.018(8) 0.007(7) -0.010(8) C11 0.045(8) 0.055(9) 0.049(9) 0.022(7) -0.006(7) -0.018(7) C12 0.037(7) 0.048(8) 0.035(7) 0.014(6) -0.004(6) 0.000(6) C13 0.022(6) 0.039(7) 0.025(6) -0.006(5) 0.005(5) 0.001(5) C14 0.026(7) 0.047(8) 0.033(7) -0.007(6) -0.006(5) -0.002(6) C15 0.040(8) 0.065(10) 0.038(8) 0.010(7) -0.015(6) -0.011(7) C16 0.027(7) 0.078(11) 0.039(8) 0.001(8) -0.008(6) -0.004(7) C17 0.026(7) 0.059(9) 0.051(9) 0.009(7) 0.000(6) 0.015(7) C18 0.039(8) 0.047(8) 0.034(7) 0.007(6) 0.001(6) 0.007(6) C19 0.024(6) 0.029(7) 0.034(7) -0.010(5) 0.004(5) -0.002(5) C20 0.031(7) 0.027(7) 0.049(8) 0.014(6) -0.002(6) 0.002(6) C21 0.029(7) 0.041(8) 0.059(9) 0.013(7) -0.001(6) 0.005(6) C22 0.027(7) 0.021(7) 0.077(10) -0.005(7) 0.003(7) 0.010(5) C23 0.021(6) 0.050(8) 0.042(8) 0.001(7) 0.010(5) -0.002(6) C24 0.019(6) 0.026(6) 0.037(7) -0.001(5) -0.004(5) 0.004(5) C25 0.020(6) 0.030(7) 0.038(7) -0.006(6) 0.002(5) -0.003(5) C26 0.027(7) 0.019(6) 0.043(7) 0.008(5) 0.000(5) 0.004(5) C27 0.026(7) 0.037(8) 0.074(10) 0.015(7) 0.013(7) 0.002(6) C28 0.017(7) 0.034(8) 0.080(11) 0.013(7) -0.007(7) -0.003(6) C29 0.043(8) 0.024(7) 0.037(7) -0.004(6) -0.015(6) -0.007(6) C30 0.028(7) 0.036(7) 0.037(7) 0.000(6) -0.003(5) 0.006(6) C1S 0.15(2) 0.085(15) 0.060(13) -0.029(11) -0.005(13) -0.019(14) C2S 0.14(2) 0.074(14) 0.076(14) 0.003(11) 0.056(14) 0.018(13) C3S 0.076(13) 0.097(16) 0.080(14) 0.044(12) 0.003(11) -0.006(11) C4S 0.118(16) 0.054(10) 0.035(9) -0.007(8) -0.012(9) 0.023(10) C5S 0.105(15) 0.094(15) 0.036(9) 0.001(9) 0.002(10) 0.042(12) C6S 0.085(13) 0.111(17) 0.069(13) -0.003(12) 0.005(10) 0.006(12) C7S 0.20(3) 0.082(19) 0.12(2) -0.002(15) -0.10(2) 0.021(19) C8S 0.099(16) 0.11(2) 0.094(16) -0.015(15) -0.034(12) 0.002(16) C9S 0.15(2) 0.11(2) 0.037(10) 0.002(11) -0.021(12) -0.079(18) C10S 0.20(3) 0.077(15) 0.038(10) -0.023(10) -0.007(13) -0.016(16) C11S 0.117(16) 0.110(19) 0.043(10) 0.012(11) -0.001(10) -0.035(15) C12S 0.18(2) 0.075(16) 0.072(13) 0.051(12) -0.071(16) -0.069(17) _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 I1 C1 2.057(10) . ? I2 C2 2.074(11) . ? Fe1 N1 1.902(8) . ? Fe1 N5 1.904(9) . ? Fe1 N4 1.910(8) . ? Fe1 N3 1.912(9) . ? Fe1 N2 1.914(8) . ? Fe1 N6 1.917(9) . ? O1 N1 1.375(10) . ? O1 B1 1.459(15) . ? O2 N2 1.367(10) . ? O2 B2 1.531(15) . ? O3 N3 1.359(10) . ? O3 B1 1.499(16) . ? O4 N4 1.375(10) . ? O4 B2 1.451(15) . ? O5 N5 1.373(10) . ? O5 B1 1.509(15) . ? O6 N6 1.370(10) . ? O6 B2 1.502(16) . ? N1 C1 1.306(13) . ? N2 C2 1.294(13) . ? N3 C3 1.337(13) . ? N4 C4 1.323(14) . ? N5 C5 1.320(14) . ? N6 C6 1.298(14) . ? F1 B1 1.348(13) . ? F2 B2 1.346(13) . ? C1 C2 1.456(14) . ? C3 C4 1.429(15) . ? C3 C7 1.490(11) . ? C4 C13 1.483(12) . ? C5 C6 1.448(14) . ? C5 C19 1.491(12) . ? C6 C25 1.502(12) . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 C10 1.3900 . ? C9 H9A 0.9500 . ? C10 C11 1.3900 . ? C10 H10B 0.9500 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 H15A 0.9500 . ? C16 C17 1.3900 . ? C16 H16A 0.9500 . ? C17 C18 1.3900 . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26A 0.9500 . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1SA 0.9500 . ? C2S C3S 1.3900 . ? C2S H2SA 0.9500 . ? C3S C4S 1.3900 . ? C3S H3SA 0.9500 . ? C4S C5S 1.3900 . ? C4S H4SA 0.9500 . ? C5S C6S 1.3900 . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? C7S C8S 1.3900 . ? C7S C12S 1.3900 . ? C7S H7SA 0.9500 . ? C8S C9S 1.3900 . ? C8S H8SA 0.9500 . ? C9S C10S 1.3900 . ? C9S H9SA 0.9500 . ? C10S C11S 1.3900 . ? C10S H10A 0.9500 . ? C11S C12S 1.3900 . ? C11S H11B 0.9500 . ? C12S H12A 0.9500 . ? 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 N1 Fe1 N5 86.7(4) . . ? N1 Fe1 N4 152.6(4) . . ? N5 Fe1 N4 114.7(4) . . ? N1 Fe1 N3 86.3(4) . . ? N5 Fe1 N3 86.8(4) . . ? N4 Fe1 N3 78.5(4) . . ? N1 Fe1 N2 78.7(3) . . ? N5 Fe1 N2 151.6(4) . . ? N4 Fe1 N2 87.6(4) . . ? N3 Fe1 N2 116.1(4) . . ? N1 Fe1 N6 115.8(4) . . ? N5 Fe1 N6 78.7(4) . . ? N4 Fe1 N6 86.3(4) . . ? N3 Fe1 N6 152.3(4) . . ? N2 Fe1 N6 85.9(4) . . ? N1 O1 B1 111.6(8) . . ? N2 O2 B2 110.2(7) . . ? N3 O3 B1 111.9(7) . . ? N4 O4 B2 112.3(8) . . ? N5 O5 B1 110.6(8) . . ? N6 O6 B2 111.1(7) . . ? C1 N1 O1 116.7(8) . . ? C1 N1 Fe1 119.4(7) . . ? O1 N1 Fe1 122.8(6) . . ? C2 N2 O2 117.0(8) . . ? C2 N2 Fe1 118.2(7) . . ? O2 N2 Fe1 123.7(6) . . ? C3 N3 O3 117.6(8) . . ? C3 N3 Fe1 117.6(7) . . ? O3 N3 Fe1 122.6(6) . . ? C4 N4 O4 116.6(8) . . ? C4 N4 Fe1 119.8(7) . . ? O4 N4 Fe1 122.5(6) . . ? C5 N5 O5 116.8(9) . . ? C5 N5 Fe1 119.1(7) . . ? O5 N5 Fe1 122.9(6) . . ? C6 N6 O6 117.9(8) . . ? C6 N6 Fe1 118.3(7) . . ? O6 N6 Fe1 122.6(6) . . ? F1 B1 O1 108.7(10) . . ? F1 B1 O3 108.4(9) . . ? O1 B1 O3 111.5(9) . . ? F1 B1 O5 107.3(9) . . ? O1 B1 O5 111.6(9) . . ? O3 B1 O5 109.2(9) . . ? F2 B2 O4 109.1(10) . . ? F2 B2 O6 108.5(10) . . ? O4 B2 O6 112.3(9) . . ? F2 B2 O2 106.1(9) . . ? O4 B2 O2 112.7(10) . . ? O6 B2 O2 107.8(9) . . ? N1 C1 C2 110.5(9) . . ? N1 C1 I1 124.1(7) . . ? C2 C1 I1 125.4(7) . . ? N2 C2 C1 112.6(9) . . ? N2 C2 I2 124.2(7) . . ? C1 C2 I2 123.2(8) . . ? N3 C3 C4 112.8(9) . . ? N3 C3 C7 122.8(9) . . ? C4 C3 C7 124.5(9) . . ? N4 C4 C3 110.5(9) . . ? N4 C4 C13 125.2(9) . . ? C3 C4 C13 124.2(9) . . ? N5 C5 C6 110.6(9) . . ? N5 C5 C19 123.8(9) . . ? C6 C5 C19 125.5(9) . . ? N6 C6 C5 112.8(9) . . ? N6 C6 C25 123.4(8) . . ? C5 C6 C25 123.7(9) . . ? C8 C7 C12 120.0 . . ? C8 C7 C3 117.8(6) . . ? C12 C7 C3 121.9(6) . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10B 120.0 . . ? C9 C10 H10B 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12B 120.0 . . ? C7 C12 H12B 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 C4 119.9(6) . . ? C18 C13 C4 119.7(6) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 C5 119.2(6) . . ? C24 C19 C5 120.7(6) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24A 120.0 . . ? C19 C24 H24A 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 C6 120.5(6) . . ? C30 C25 C6 119.5(6) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1SA 120.0 . . ? C6S C1S H1SA 120.0 . . ? C1S C2S C3S 120.0 . . ? C1S C2S H2SA 120.0 . . ? C3S C2S H2SA 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3SA 120.0 . . ? C2S C3S H3SA 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4SA 120.0 . . ? C5S C4S H4SA 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5SA 120.0 . . ? C4S C5S H5SA 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6SA 120.0 . . ? C1S C6S H6SA 120.0 . . ? C8S C7S C12S 120.0 . . ? C8S C7S H7SA 120.0 . . ? C12S C7S H7SA 120.0 . . ? C7S C8S C9S 120.0 . . ? C7S C8S H8SA 120.0 . . ? C9S C8S H8SA 120.0 . . ? C10S C9S C8S 120.0 . . ? C10S C9S H9SA 120.0 . . ? C8S C9S H9SA 120.0 . . ? C11S C10S C9S 120.0 . . ? C11S C10S H10A 120.0 . . ? C9S C10S H10A 120.0 . . ? C12S C11S C10S 120.0 . . ? C12S C11S H11B 120.0 . . ? C10S C11S H11B 120.0 . . ? C11S C12S C7S 120.0 . . ? C11S C12S H12A 120.0 . . ? C7S C12S H12A 120.0 . . ? 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 B1 O1 N1 C1 -151.5(9) . . . . ? B1 O1 N1 Fe1 16.1(11) . . . . ? N5 Fe1 N1 C1 -158.6(8) . . . . ? N4 Fe1 N1 C1 58.3(12) . . . . ? N3 Fe1 N1 C1 114.4(8) . . . . ? N2 Fe1 N1 C1 -3.1(8) . . . . ? N6 Fe1 N1 C1 -82.8(8) . . . . ? N5 Fe1 N1 O1 34.1(7) . . . . ? N4 Fe1 N1 O1 -109.0(9) . . . . ? N3 Fe1 N1 O1 -52.9(7) . . . . ? N2 Fe1 N1 O1 -170.4(8) . . . . ? N6 Fe1 N1 O1 109.8(7) . . . . ? B2 O2 N2 C2 -154.2(9) . . . . ? B2 O2 N2 Fe1 13.7(11) . . . . ? N1 Fe1 N2 C2 -2.5(8) . . . . ? N5 Fe1 N2 C2 58.0(12) . . . . ? N4 Fe1 N2 C2 -158.6(8) . . . . ? N3 Fe1 N2 C2 -82.7(8) . . . . ? N6 Fe1 N2 C2 114.9(8) . . . . ? N1 Fe1 N2 O2 -170.2(8) . . . . ? N5 Fe1 N2 O2 -109.7(9) . . . . ? N4 Fe1 N2 O2 33.6(7) . . . . ? N3 Fe1 N2 O2 109.6(7) . . . . ? N6 Fe1 N2 O2 -52.8(7) . . . . ? B1 O3 N3 C3 -148.1(10) . . . . ? B1 O3 N3 Fe1 14.3(11) . . . . ? N1 Fe1 N3 C3 -162.8(8) . . . . ? N5 Fe1 N3 C3 110.3(8) . . . . ? N4 Fe1 N3 C3 -5.7(8) . . . . ? N2 Fe1 N3 C3 -87.3(9) . . . . ? N6 Fe1 N3 C3 52.4(12) . . . . ? N1 Fe1 N3 O3 34.8(8) . . . . ? N5 Fe1 N3 O3 -52.2(8) . . . . ? N4 Fe1 N3 O3 -168.2(8) . . . . ? N2 Fe1 N3 O3 110.3(7) . . . . ? N6 Fe1 N3 O3 -110.1(9) . . . . ? B2 O4 N4 C4 -154.2(10) . . . . ? B2 O4 N4 Fe1 13.5(11) . . . . ? N1 Fe1 N4 C4 57.7(12) . . . . ? N5 Fe1 N4 C4 -81.1(9) . . . . ? N3 Fe1 N4 C4 -0.1(8) . . . . ? N2 Fe1 N4 C4 117.2(9) . . . . ? N6 Fe1 N4 C4 -156.8(9) . . . . ? N1 Fe1 N4 O4 -109.7(9) . . . . ? N5 Fe1 N4 O4 111.6(7) . . . . ? N3 Fe1 N4 O4 -167.4(8) . . . . ? N2 Fe1 N4 O4 -50.2(7) . . . . ? N6 Fe1 N4 O4 35.8(7) . . . . ? B1 O5 N5 C5 -150.5(10) . . . . ? B1 O5 N5 Fe1 17.1(11) . . . . ? N1 Fe1 N5 C5 114.4(9) . . . . ? N4 Fe1 N5 C5 -83.2(9) . . . . ? N3 Fe1 N5 C5 -159.0(9) . . . . ? N2 Fe1 N5 C5 55.7(12) . . . . ? N6 Fe1 N5 C5 -2.7(8) . . . . ? N1 Fe1 N5 O5 -52.8(8) . . . . ? N4 Fe1 N5 O5 109.5(8) . . . . ? N3 Fe1 N5 O5 33.7(8) . . . . ? N2 Fe1 N5 O5 -111.6(9) . . . . ? N6 Fe1 N5 O5 -170.0(8) . . . . ? B2 O6 N6 C6 -150.0(10) . . . . ? B2 O6 N6 Fe1 17.0(11) . . . . ? N1 Fe1 N6 C6 -82.9(9) . . . . ? N5 Fe1 N6 C6 -2.2(8) . . . . ? N4 Fe1 N6 C6 114.0(8) . . . . ? N3 Fe1 N6 C6 57.5(12) . . . . ? N2 Fe1 N6 C6 -158.2(8) . . . . ? N1 Fe1 N6 O6 110.2(7) . . . . ? N5 Fe1 N6 O6 -169.1(8) . . . . ? N4 Fe1 N6 O6 -53.0(7) . . . . ? N3 Fe1 N6 O6 -109.5(9) . . . . ? N2 Fe1 N6 O6 34.9(7) . . . . ? N1 O1 B1 F1 171.6(8) . . . . ? N1 O1 B1 O3 52.1(11) . . . . ? N1 O1 B1 O5 -70.3(11) . . . . ? N3 O3 B1 F1 170.9(8) . . . . ? N3 O3 B1 O1 -69.5(10) . . . . ? N3 O3 B1 O5 54.3(11) . . . . ? N5 O5 B1 F1 170.9(8) . . . . ? N5 O5 B1 O1 51.9(12) . . . . ? N5 O5 B1 O3 -71.8(10) . . . . ? N4 O4 B2 F2 171.0(9) . . . . ? N4 O4 B2 O6 -68.7(11) . . . . ? N4 O4 B2 O2 53.3(12) . . . . ? N6 O6 B2 F2 172.3(8) . . . . ? N6 O6 B2 O4 51.6(11) . . . . ? N6 O6 B2 O2 -73.2(10) . . . . ? N2 O2 B2 F2 171.9(8) . . . . ? N2 O2 B2 O4 -68.7(11) . . . . ? N2 O2 B2 O6 55.9(10) . . . . ? O1 N1 C1 C2 175.3(8) . . . . ? Fe1 N1 C1 C2 7.2(11) . . . . ? O1 N1 C1 I1 -4.7(12) . . . . ? Fe1 N1 C1 I1 -172.7(4) . . . . ? O2 N2 C2 C1 175.4(8) . . . . ? Fe1 N2 C2 C1 6.8(11) . . . . ? O2 N2 C2 I2 -3.1(13) . . . . ? Fe1 N2 C2 I2 -171.7(5) . . . . ? N1 C1 C2 N2 -8.7(12) . . . . ? I1 C1 C2 N2 171.2(7) . . . . ? N1 C1 C2 I2 169.8(7) . . . . ? I1 C1 C2 I2 -10.3(12) . . . . ? O3 N3 C3 C4 173.4(9) . . . . ? Fe1 N3 C3 C4 10.0(12) . . . . ? O3 N3 C3 C7 -7.5(15) . . . . ? Fe1 N3 C3 C7 -170.9(7) . . . . ? O4 N4 C4 C3 173.3(9) . . . . ? Fe1 N4 C4 C3 5.2(13) . . . . ? O4 N4 C4 C13 -9.2(15) . . . . ? Fe1 N4 C4 C13 -177.3(8) . . . . ? N3 C3 C4 N4 -9.4(14) . . . . ? C7 C3 C4 N4 171.5(9) . . . . ? N3 C3 C4 C13 173.0(10) . . . . ? C7 C3 C4 C13 -6.1(17) . . . . ? O5 N5 C5 C6 174.4(8) . . . . ? Fe1 N5 C5 C6 6.3(12) . . . . ? O5 N5 C5 C19 -2.5(15) . . . . ? Fe1 N5 C5 C19 -170.6(7) . . . . ? O6 N6 C6 C5 173.6(8) . . . . ? Fe1 N6 C6 C5 6.0(12) . . . . ? O6 N6 C6 C25 -3.2(14) . . . . ? Fe1 N6 C6 C25 -170.8(7) . . . . ? N5 C5 C6 N6 -7.7(13) . . . . ? C19 C5 C6 N6 169.2(9) . . . . ? N5 C5 C6 C25 169.1(9) . . . . ? C19 C5 C6 C25 -14.0(16) . . . . ? N3 C3 C7 C8 134.8(9) . . . . ? C4 C3 C7 C8 -46.2(13) . . . . ? N3 C3 C7 C12 -51.1(13) . . . . ? C4 C3 C7 C12 127.9(10) . . . . ? C12 C7 C8 C9 0.0 . . . . ? C3 C7 C8 C9 174.2(8) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C7 0.0 . . . . ? C8 C7 C12 C11 0.0 . . . . ? C3 C7 C12 C11 -174.0(8) . . . . ? N4 C4 C13 C14 -50.9(13) . . . . ? C3 C4 C13 C14 126.3(10) . . . . ? N4 C4 C13 C18 135.9(10) . . . . ? C3 C4 C13 C18 -46.8(13) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C4 C13 C14 C15 -173.1(8) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C4 C13 C18 C17 173.1(8) . . . . ? N5 C5 C19 C20 134.9(9) . . . . ? C6 C5 C19 C20 -41.5(12) . . . . ? N5 C5 C19 C24 -48.5(13) . . . . ? C6 C5 C19 C24 135.1(9) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C5 C19 C20 C21 176.6(8) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? C5 C19 C24 C23 -176.6(8) . . . . ? N6 C6 C25 C26 -41.6(12) . . . . ? C5 C6 C25 C26 141.9(9) . . . . ? N6 C6 C25 C30 137.7(9) . . . . ? C5 C6 C25 C30 -38.8(12) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C6 C25 C26 C27 179.3(8) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? C6 C25 C30 C29 -179.3(8) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C2S C1S C6S C5S 0.0 . . . . ? C12S C7S C8S C9S 0.0 . . . . ? C7S C8S C9S C10S 0.0 . . . . ? C8S C9S C10S C11S 0.0 . . . . ? C9S C10S C11S C12S 0.0 . . . . ? C10S C11S C12S C7S 0.0 . . . . ? C8S C7S C12S C11S 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 2.958 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.166 _publ_section_references ; Bruker, Programs APEX II, version 2.0-1; SAINT, version 7.23A; SADABS, version 2004/1; XPREP, version 2005/2; SHELXTL, version 6.1. Bruker AXS Inc., Madison, WI, USA, 2005. G.M. Sheldrick, Programs SHELXS97 (crystal structure solution) and SHELXL97 (crystal structure refinement), University of Gottingen, Germany, 1997. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; There is a high positive residual density of 2.96 e\%A^-3^ near the I1 center (distance 1.09 %A) due to considerable absorption effects which could not be completely corrected. ;