# 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 ? loop_ _publ_author_name _publ_author_address C.J.Schneider ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.Moubaraki ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; J.D.Cashion ; School of Physics, Monash University, PO Box 23, VIC 3800, Australia ; D.R.Turner ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.A.Leita ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; ; S.R.Batten ; ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; K.S.Murray ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_author_address ; School of Chemistry, 171 Monash university, Vic 3800, Australia ; _publ_contact_author_email Keith.murray@monash.edu.au _publ_contact_author_fax +61-3-9905-4597 _publ_contact_author_phone +61-3-9905-4512 #========================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Keith. S. Murray' _publ_contact_letter ; ; _publ_requested_category ? _publ_section_title ; Spin crossover in polynuclear, mixed-ligand tris(pyrazolyl)methane iron(II)complexes. ; data_1.2DME(123K) _database_code_depnum_ccdc_archive 'CCDC 803921' _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(p-C6H4(CH2OCH2C(pz)3]2)](BF4)4(DME)2 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(p-C6H4(CH2OCH2C(pz)3)2))(BF4)4(DME)2 _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 Fe2 N24 O2, 2(C4 H10 O2), 4(B F4)' _chemical_formula_sum 'C70 H94 B4 F16 Fe2 N24 O6' _chemical_formula_weight 1826.63 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5038(3) _cell_length_b 20.7090(6) _cell_length_c 17.4235(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.935(2) _cell_angle_gamma 90.00 _cell_volume 4141.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 4893 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.30 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8055 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _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 26328 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9475 _reflns_number_gt 7271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9475 _refine_ls_number_parameters 584 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.24230(4) 0.70749(3) 0.37727(3) 0.02153(13) Uani 1 1 d . . . F1 F 0.6189(2) 0.91533(13) 0.55047(13) 0.0468(6) Uani 1 1 d . . . F2 F 0.5587(2) 0.89240(15) 0.66940(14) 0.0516(7) Uani 1 1 d . . . F3 F 0.6329(3) 0.99076(15) 0.64330(17) 0.0679(9) Uani 1 1 d . . . F4 F 0.7495(2) 0.90234(15) 0.65273(16) 0.0569(8) Uani 1 1 d . . . F5 F 0.1969(3) 0.45714(14) 0.39496(17) 0.0662(9) Uani 1 1 d . . . F6 F 0.1070(3) 0.40479(15) 0.2982(2) 0.0901(12) Uani 1 1 d . . . F7 F 0.3020(3) 0.39825(17) 0.31708(16) 0.0731(10) Uani 1 1 d . . . F8 F 0.1881(2) 0.34822(12) 0.39801(15) 0.0489(7) Uani 1 1 d . . . O1 O 0.0093(2) 0.55081(13) 0.19368(13) 0.0270(6) Uani 1 1 d . . . O5 O 0.7830(4) 0.4825(2) 0.3530(3) 0.0387(11) Uani 0.80 1 d P A 1 O5' O 0.763(3) 0.5064(14) 0.359(2) 0.073(4) Uani 0.20 1 d PD B 2 O6 O 0.7527(4) 0.6213(2) 0.3521(3) 0.0501(13) Uani 0.80 1 d P A 1 O6' O 0.784(2) 0.6518(15) 0.3647(18) 0.073(4) Uani 0.20 1 d P B 2 N7 N 0.3496(2) 0.76503(15) 0.32353(16) 0.0251(7) Uani 1 1 d . . . N8 N 0.4207(2) 0.80423(15) 0.36914(16) 0.0254(7) Uani 1 1 d . . . N9 N 0.3718(2) 0.68829(15) 0.45387(16) 0.0232(6) Uani 1 1 d . . . N10 N 0.4397(2) 0.73873(15) 0.48065(16) 0.0227(6) Uani 1 1 d . . . N11 N 0.2033(2) 0.78155(15) 0.44303(17) 0.0271(7) Uani 1 1 d . . . N12 N 0.2940(2) 0.82025(15) 0.46912(16) 0.0236(6) Uani 1 1 d . . . N6 N 0.1395(2) 0.65052(15) 0.43094(16) 0.0229(6) Uani 1 1 d . . . N5 N 0.0708(2) 0.60811(14) 0.38971(16) 0.0218(6) Uani 1 1 d . . . N2 N 0.1108(2) 0.72166(15) 0.30193(17) 0.0257(7) Uani 1 1 d . . . N1 N 0.0483(2) 0.66930(15) 0.27490(16) 0.0237(6) Uani 1 1 d . . . N4 N 0.2827(2) 0.63464(15) 0.31410(16) 0.0235(6) Uani 1 1 d . . . N3 N 0.1988(2) 0.59131(14) 0.29079(16) 0.0211(6) Uani 1 1 d . . . C1 C 0.3276(4) 0.7402(2) 0.1828(2) 0.0370(10) Uani 1 1 d . . . H1A H 0.3750 0.7027 0.1708 0.055 Uiso 1 1 calc R . . H1B H 0.3232 0.7700 0.1389 0.055 Uiso 1 1 calc R . . H1C H 0.2490 0.7259 0.1931 0.055 Uiso 1 1 calc R . . C2 C 0.3821(3) 0.7739(2) 0.2521(2) 0.0295(9) Uani 1 1 d . . . C3 C 0.4741(3) 0.8184(2) 0.2534(2) 0.0336(9) Uani 1 1 d . . . H3 H 0.5127 0.8329 0.2101 0.040 Uiso 1 1 calc R . . C4 C 0.4981(3) 0.8371(2) 0.3277(2) 0.0308(9) Uani 1 1 d . . . C5 C 0.5846(4) 0.8838(2) 0.3631(2) 0.0400(10) Uani 1 1 d . . . H5A H 0.6381 0.8972 0.3247 0.060 Uiso 1 1 calc R . . H5B H 0.6288 0.8632 0.4065 0.060 Uiso 1 1 calc R . . H5C H 0.5437 0.9217 0.3815 0.060 Uiso 1 1 calc R . . C6 C 0.3686(3) 0.56943(19) 0.4778(2) 0.0330(9) Uani 1 1 d . . . H6A H 0.3152 0.5599 0.5178 0.049 Uiso 1 1 calc R . . H6B H 0.4325 0.5381 0.4808 0.049 Uiso 1 1 calc R . . H6C H 0.3263 0.5667 0.4271 0.049 Uiso 1 1 calc R . . C7 C 0.4167(3) 0.63582(19) 0.48957(19) 0.0253(8) Uani 1 1 d . . . C8 C 0.5136(3) 0.6536(2) 0.5381(2) 0.0296(9) Uani 1 1 d . . . H8 H 0.5610 0.6253 0.5699 0.035 Uiso 1 1 calc R . . C9 C 0.5275(3) 0.7184(2) 0.5315(2) 0.0274(8) Uani 1 1 d . . . C10 C 0.6158(3) 0.7632(2) 0.5686(2) 0.0406(10) Uani 1 1 d . . . H10A H 0.5783 0.7917 0.6043 0.061 Uiso 1 1 calc R . . H10B H 0.6502 0.7892 0.5290 0.061 Uiso 1 1 calc R . . H10C H 0.6771 0.7381 0.5968 0.061 Uiso 1 1 calc R . . C11 C -0.0106(3) 0.7815(2) 0.4576(3) 0.0425(11) Uani 1 1 d . . . H11A H -0.0098 0.7457 0.4208 0.064 Uiso 1 1 calc R . . H11B H -0.0617 0.8159 0.4362 0.064 Uiso 1 1 calc R . . H11C H -0.0395 0.7661 0.5059 0.064 Uiso 1 1 calc R . . C12 C 0.1100(3) 0.80726(19) 0.4725(2) 0.0306(9) Uani 1 1 d . . . C13 C 0.1425(3) 0.8609(2) 0.5174(2) 0.0313(9) Uani 1 1 d . . . H13 H 0.0921 0.8870 0.5453 0.038 Uiso 1 1 calc R . . C14 C 0.2594(3) 0.86928(18) 0.5139(2) 0.0275(8) Uani 1 1 d . . . C15 C 0.3387(3) 0.9209(2) 0.5451(2) 0.0361(10) Uani 1 1 d . . . H15A H 0.4016 0.9016 0.5782 0.054 Uiso 1 1 calc R . . H15B H 0.2949 0.9513 0.5750 0.054 Uiso 1 1 calc R . . H15C H 0.3719 0.9438 0.5025 0.054 Uiso 1 1 calc R . . C16 C 0.4106(3) 0.80264(18) 0.45143(19) 0.0235(8) Uani 1 1 d . . . H16 H 0.4666 0.8344 0.4764 0.028 Uiso 1 1 calc R . . C23 C 0.1139(3) 0.64282(19) 0.5032(2) 0.0285(8) Uani 1 1 d . . . H23 H 0.1489 0.6664 0.5455 0.034 Uiso 1 1 calc R . . C24 C 0.0295(3) 0.5958(2) 0.5090(2) 0.0306(9) Uani 1 1 d . . . H24 H -0.0031 0.5815 0.5546 0.037 Uiso 1 1 calc R . . C25 C 0.0026(3) 0.57444(18) 0.4362(2) 0.0262(8) Uani 1 1 d . . . H25 H -0.0531 0.5422 0.4208 0.031 Uiso 1 1 calc R . . C17 C 0.0609(3) 0.77221(19) 0.2658(2) 0.0345(9) Uani 1 1 d . . . H17 H 0.0856 0.8157 0.2728 0.041 Uiso 1 1 calc R . . C18 C -0.0323(4) 0.7526(2) 0.2163(2) 0.0411(11) Uani 1 1 d . . . H18 H -0.0816 0.7795 0.1841 0.049 Uiso 1 1 calc R . . C19 C -0.0389(3) 0.68737(19) 0.2232(2) 0.0319(9) Uani 1 1 d . . . H19 H -0.0941 0.6597 0.1968 0.038 Uiso 1 1 calc R . . C20 C 0.3812(3) 0.61055(19) 0.2908(2) 0.0273(8) Uani 1 1 d . . . H20 H 0.4551 0.6310 0.2982 0.033 Uiso 1 1 calc R . . C21 C 0.3621(3) 0.5516(2) 0.2543(2) 0.0320(9) Uani 1 1 d . . . H21 H 0.4186 0.5247 0.2331 0.038 Uiso 1 1 calc R . . C22 C 0.2454(3) 0.54044(19) 0.2551(2) 0.0287(8) Uani 1 1 d . . . H22 H 0.2045 0.5038 0.2345 0.034 Uiso 1 1 calc R . . C26 C 0.0783(3) 0.60585(18) 0.30647(19) 0.0220(7) Uani 1 1 d . . . C27 C -0.0042(3) 0.55411(19) 0.27343(19) 0.0258(8) Uani 1 1 d . . . H27A H 0.0148 0.5119 0.2979 0.031 Uiso 1 1 calc R . . H27B H -0.0856 0.5653 0.2830 0.031 Uiso 1 1 calc R . . C28 C -0.0497(3) 0.4955(2) 0.1601(2) 0.0309(9) Uani 1 1 d . . . H28A H -0.1345 0.4983 0.1662 0.037 Uiso 1 1 calc R . . H28B H -0.0196 0.4553 0.1849 0.037 Uiso 1 1 calc R . . C29 C -0.0258(3) 0.49640(18) 0.0768(2) 0.0269(8) Uani 1 1 d . . . C30 C 0.0754(3) 0.46877(19) 0.0529(2) 0.0278(8) Uani 1 1 d . . . H30 H 0.1274 0.4474 0.0892 0.033 Uiso 1 1 calc R . . C31 C -0.1012(3) 0.52789(19) 0.0231(2) 0.0302(9) Uani 1 1 d . . . H31 H -0.1706 0.5471 0.0389 0.036 Uiso 1 1 calc R . . C32 C 0.6827(6) 0.5777(4) 0.3912(4) 0.0494(18) Uani 0.80 1 d P A 1 H32A H 0.6044 0.5963 0.3965 0.059 Uiso 0.80 1 calc PR A 1 H32B H 0.7189 0.5683 0.4432 0.059 Uiso 0.80 1 calc PR A 1 C32' C 0.721(3) 0.6157(16) 0.4133(18) 0.073(4) Uani 0.20 1 d PD B 2 H32C H 0.6532 0.6401 0.4299 0.088 Uiso 0.20 1 calc PR B 2 H32D H 0.7699 0.6015 0.4592 0.088 Uiso 0.20 1 calc PR B 2 C33 C 0.7430(7) 0.6819(4) 0.3837(5) 0.072(2) Uani 0.80 1 d PD A 1 H33A H 0.6609 0.6948 0.3811 0.109 Uiso 0.80 1 calc PR A 1 H33B H 0.7875 0.7129 0.3550 0.109 Uiso 0.80 1 calc PR A 1 H33C H 0.7738 0.6811 0.4376 0.109 Uiso 0.80 1 calc PR A 1 C33' C 0.710(3) 0.6997(14) 0.3189(19) 0.073(4) Uani 0.20 1 d PD B 2 H33D H 0.6539 0.7191 0.3519 0.110 Uiso 0.20 1 calc PR B 2 H33E H 0.6681 0.6776 0.2756 0.110 Uiso 0.20 1 calc PR B 2 H33F H 0.7597 0.7335 0.2994 0.110 Uiso 0.20 1 calc PR B 2 C34 C 0.6744(4) 0.5187(4) 0.3445(3) 0.0496(17) Uani 0.80 1 d PD A 1 H34A H 0.6097 0.4916 0.3609 0.059 Uiso 0.80 1 calc PR A 1 H34B H 0.6572 0.5302 0.2898 0.059 Uiso 0.80 1 calc PR A 1 C34' C 0.685(3) 0.5619(12) 0.365(2) 0.073(4) Uani 0.20 1 d PD B 2 H34C H 0.6679 0.5788 0.3124 0.088 Uiso 0.20 1 calc PR B 2 H34D H 0.6107 0.5456 0.3830 0.088 Uiso 0.20 1 calc PR B 2 C36 C 0.7797(6) 0.4225(3) 0.3133(4) 0.0509(17) Uani 0.80 1 d PD A 1 H36A H 0.7262 0.3931 0.3373 0.076 Uiso 0.80 1 calc PR A 1 H36B H 0.8580 0.4036 0.3160 0.076 Uiso 0.80 1 calc PR A 1 H36C H 0.7528 0.4295 0.2594 0.076 Uiso 0.80 1 calc PR A 1 C36' C 0.732(3) 0.4386(17) 0.310(2) 0.073(4) Uani 0.20 1 d PD B 2 H36D H 0.6957 0.4073 0.3432 0.110 Uiso 0.20 1 calc PR B 2 H36E H 0.8039 0.4202 0.2922 0.110 Uiso 0.20 1 calc PR B 2 H36F H 0.6781 0.4484 0.2655 0.110 Uiso 0.20 1 calc PR B 2 B1 B 0.6396(4) 0.9258(3) 0.6294(3) 0.0377(11) Uani 1 1 d . . . B2 B 0.1995(4) 0.4015(3) 0.3514(3) 0.0392(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0236(2) 0.0201(3) 0.0207(2) -0.0001(2) 0.00015(19) -0.0016(2) F1 0.0489(14) 0.0578(18) 0.0338(13) -0.0025(13) 0.0022(11) -0.0039(13) F2 0.0359(13) 0.082(2) 0.0377(13) -0.0009(14) 0.0074(11) -0.0031(13) F3 0.094(2) 0.0487(19) 0.0584(18) -0.0110(16) -0.0133(16) 0.0114(17) F4 0.0327(12) 0.073(2) 0.0636(17) 0.0232(16) -0.0040(12) 0.0032(13) F5 0.096(2) 0.0400(17) 0.0675(19) -0.0149(15) 0.0390(17) -0.0196(16) F6 0.092(2) 0.0424(19) 0.125(3) 0.0191(19) -0.070(2) -0.0050(16) F7 0.074(2) 0.092(3) 0.0575(18) 0.0248(18) 0.0301(15) 0.0448(18) F8 0.0546(15) 0.0355(15) 0.0550(16) 0.0014(13) -0.0072(12) 0.0030(12) O1 0.0325(13) 0.0255(15) 0.0227(12) -0.0038(12) 0.0000(10) -0.0061(11) O5 0.032(2) 0.050(3) 0.033(2) -0.001(2) -0.0023(18) -0.006(2) O5' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) O6 0.050(3) 0.051(3) 0.050(3) 0.003(3) 0.013(2) 0.006(2) O6' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) N7 0.0276(14) 0.0263(17) 0.0210(15) 0.0003(14) -0.0013(12) -0.0048(13) N8 0.0281(14) 0.0276(18) 0.0203(14) -0.0012(14) -0.0001(12) -0.0081(13) N9 0.0254(14) 0.0228(17) 0.0214(14) 0.0008(13) 0.0006(12) -0.0025(12) N10 0.0236(13) 0.0236(17) 0.0207(14) -0.0002(14) 0.0002(11) -0.0017(12) N11 0.0248(14) 0.0257(18) 0.0309(16) -0.0035(15) 0.0020(12) -0.0020(13) N12 0.0230(14) 0.0232(16) 0.0246(15) -0.0044(14) 0.0013(12) -0.0008(12) N6 0.0251(14) 0.0213(16) 0.0222(15) -0.0013(14) 0.0012(12) -0.0025(12) N5 0.0227(13) 0.0213(16) 0.0215(14) 0.0015(13) 0.0025(11) -0.0010(12) N2 0.0302(15) 0.0201(17) 0.0267(16) -0.0016(14) 0.0009(13) -0.0029(13) N1 0.0251(14) 0.0209(16) 0.0243(15) 0.0009(14) -0.0033(12) -0.0018(12) N4 0.0245(14) 0.0242(17) 0.0217(14) 0.0010(14) 0.0007(11) -0.0040(12) N3 0.0220(13) 0.0206(16) 0.0207(14) -0.0020(13) 0.0017(11) -0.0016(12) C1 0.048(2) 0.039(3) 0.0237(19) -0.0013(19) 0.0003(17) -0.009(2) C2 0.0334(19) 0.032(2) 0.0221(18) 0.0017(17) -0.0017(15) -0.0015(16) C3 0.040(2) 0.039(3) 0.0221(18) 0.0008(19) 0.0058(16) -0.0100(18) C4 0.0317(18) 0.033(2) 0.0276(19) 0.0053(18) 0.0013(15) -0.0081(17) C5 0.044(2) 0.044(3) 0.031(2) 0.003(2) 0.0037(18) -0.019(2) C6 0.040(2) 0.025(2) 0.033(2) 0.0063(18) 0.0012(17) 0.0008(17) C7 0.0304(17) 0.027(2) 0.0194(17) 0.0034(16) 0.0056(14) 0.0031(15) C8 0.0330(18) 0.033(2) 0.0227(18) 0.0022(18) -0.0017(15) 0.0067(17) C9 0.0260(17) 0.035(2) 0.0214(17) -0.0037(17) 0.0008(14) 0.0057(16) C10 0.039(2) 0.040(3) 0.040(2) -0.004(2) -0.0143(18) 0.0005(19) C11 0.029(2) 0.037(3) 0.061(3) -0.005(2) 0.0038(19) 0.0011(18) C12 0.0293(18) 0.026(2) 0.037(2) 0.0015(19) 0.0042(16) 0.0034(16) C13 0.0313(18) 0.030(2) 0.032(2) -0.0064(19) 0.0030(16) 0.0079(16) C14 0.0306(18) 0.023(2) 0.0279(19) -0.0008(17) -0.0041(15) 0.0050(15) C15 0.0335(19) 0.033(2) 0.040(2) -0.013(2) -0.0087(17) 0.0030(17) C16 0.0240(16) 0.024(2) 0.0221(17) -0.0050(16) -0.0017(13) -0.0048(14) C23 0.0333(18) 0.029(2) 0.0232(18) -0.0020(17) 0.0034(15) -0.0005(16) C24 0.036(2) 0.031(2) 0.0261(19) 0.0017(18) 0.0095(16) -0.0028(17) C25 0.0248(17) 0.024(2) 0.0308(19) 0.0024(17) 0.0061(14) -0.0030(15) C17 0.040(2) 0.019(2) 0.043(2) 0.0053(19) -0.0047(18) 0.0010(17) C18 0.046(2) 0.030(2) 0.045(2) 0.005(2) -0.016(2) 0.0016(19) C19 0.0312(18) 0.026(2) 0.037(2) 0.0023(19) -0.0105(16) -0.0005(16) C20 0.0236(16) 0.034(2) 0.0249(18) 0.0002(18) 0.0021(14) 0.0002(15) C21 0.0301(18) 0.034(2) 0.032(2) -0.0072(19) 0.0027(16) 0.0045(17) C22 0.0336(19) 0.028(2) 0.0247(18) -0.0067(17) 0.0010(15) 0.0008(16) C26 0.0218(15) 0.0220(19) 0.0221(17) -0.0003(16) 0.0018(13) 0.0011(14) C27 0.0294(17) 0.025(2) 0.0231(18) -0.0033(17) 0.0004(14) -0.0033(15) C28 0.0350(19) 0.029(2) 0.0279(19) -0.0038(18) -0.0031(16) -0.0064(17) C29 0.0338(18) 0.021(2) 0.0249(18) -0.0033(17) -0.0016(15) -0.0077(15) C30 0.0316(18) 0.024(2) 0.0268(18) -0.0017(17) -0.0067(15) -0.0003(15) C31 0.0293(18) 0.028(2) 0.032(2) -0.0071(18) -0.0032(15) -0.0022(16) C32 0.039(3) 0.071(5) 0.040(4) 0.003(4) 0.012(3) 0.010(3) C32' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) C33 0.061(5) 0.072(6) 0.086(6) -0.017(5) 0.018(4) 0.003(4) C33' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) C34 0.025(2) 0.091(5) 0.032(3) 0.021(3) -0.003(2) -0.002(3) C34' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) C36 0.062(4) 0.051(4) 0.039(3) 0.001(3) -0.003(3) -0.020(3) C36' 0.063(8) 0.079(11) 0.077(10) 0.017(9) 0.005(7) 0.013(7) B1 0.031(2) 0.045(3) 0.036(3) -0.004(2) -0.0010(19) -0.003(2) B2 0.040(3) 0.036(3) 0.040(3) -0.004(2) -0.003(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.943(3) . ? Fe1 N6 1.954(3) . ? Fe1 N2 1.956(3) . ? Fe1 N9 1.971(3) . ? Fe1 N11 1.984(3) . ? Fe1 N7 1.995(3) . ? F1 B1 1.397(5) . ? F2 B1 1.385(6) . ? F3 B1 1.369(6) . ? F4 B1 1.388(5) . ? F5 B2 1.382(6) . ? F6 B2 1.363(5) . ? F7 B2 1.360(6) . ? F8 B2 1.381(6) . ? O1 C27 1.410(4) . ? O1 C28 1.435(4) . ? O5 C36 1.421(8) . ? O5 C34 1.456(7) . ? O5' C34' 1.464(11) . ? O5' C36' 1.67(4) . ? O6 C33 1.378(9) . ? O6 C32 1.414(9) . ? O6' C32' 1.37(4) . ? O6' C33' 1.50(4) . ? N7 C2 1.336(4) . ? N7 N8 1.368(4) . ? N8 C4 1.366(5) . ? N8 C16 1.447(4) . ? N9 C7 1.338(5) . ? N9 N10 1.367(4) . ? N10 C9 1.365(4) . ? N10 C16 1.449(5) . ? N11 C12 1.332(5) . ? N11 N12 1.368(4) . ? N12 C14 1.357(5) . ? N12 C16 1.444(4) . ? N6 C23 1.322(4) . ? N6 N5 1.355(4) . ? N5 C25 1.358(4) . ? N5 C26 1.460(4) . ? N2 C17 1.331(5) . ? N2 N1 1.366(4) . ? N1 C19 1.354(4) . ? N1 C26 1.457(4) . ? N4 C20 1.327(4) . ? N4 N3 1.360(4) . ? N3 C22 1.352(5) . ? N3 C26 1.463(4) . ? C1 C2 1.495(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.402(5) . ? C3 C4 1.361(5) . ? C3 H3 0.9500 . ? C4 C5 1.491(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.491(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.402(5) . ? C8 C9 1.357(6) . ? C8 H8 0.9500 . ? C9 C10 1.490(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.492(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.396(5) . ? C13 C14 1.361(5) . ? C13 H13 0.9500 . ? C14 C15 1.483(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C23 C24 1.384(5) . ? C23 H23 0.9500 . ? C24 C25 1.360(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C17 C18 1.389(5) . ? C17 H17 0.9500 . ? C18 C19 1.359(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 C22 1.364(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C26 C27 1.518(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.496(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.387(5) . ? C29 C31 1.393(5) . ? C30 C31 1.378(5) 3_565 ? C30 H30 0.9500 . ? C31 C30 1.378(5) 3_565 ? C31 H31 0.9500 . ? C32 C34 1.467(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32' C34' 1.439(11) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N6 88.77(12) . . ? N4 Fe1 N2 86.59(12) . . ? N6 Fe1 N2 86.91(12) . . ? N4 Fe1 N9 91.59(12) . . ? N6 Fe1 N9 90.47(12) . . ? N2 Fe1 N9 176.84(13) . . ? N4 Fe1 N11 179.02(12) . . ? N6 Fe1 N11 91.27(13) . . ? N2 Fe1 N11 94.39(12) . . ? N9 Fe1 N11 87.44(12) . . ? N4 Fe1 N7 91.02(12) . . ? N6 Fe1 N7 179.01(12) . . ? N2 Fe1 N7 94.05(12) . . ? N9 Fe1 N7 88.56(12) . . ? N11 Fe1 N7 88.92(13) . . ? C27 O1 C28 111.1(3) . . ? C36 O5 C34 114.1(5) . . ? C34' O5' C36' 126(3) . . ? C33 O6 C32 108.9(6) . . ? C32' O6' C33' 112(3) . . ? C2 N7 N8 105.4(3) . . ? C2 N7 Fe1 137.8(3) . . ? N8 N7 Fe1 116.5(2) . . ? C4 N8 N7 112.0(3) . . ? C4 N8 C16 129.5(3) . . ? N7 N8 C16 118.5(3) . . ? C7 N9 N10 105.6(3) . . ? C7 N9 Fe1 136.7(3) . . ? N10 N9 Fe1 117.7(2) . . ? C9 N10 N9 111.4(3) . . ? C9 N10 C16 130.8(3) . . ? N9 N10 C16 117.7(3) . . ? C12 N11 N12 104.7(3) . . ? C12 N11 Fe1 138.7(3) . . ? N12 N11 Fe1 116.6(2) . . ? C14 N12 N11 112.5(3) . . ? C14 N12 C16 128.7(3) . . ? N11 N12 C16 118.6(3) . . ? C23 N6 N5 105.5(3) . . ? C23 N6 Fe1 135.3(3) . . ? N5 N6 Fe1 119.2(2) . . ? N6 N5 C25 110.9(3) . . ? N6 N5 C26 118.4(3) . . ? C25 N5 C26 130.7(3) . . ? C17 N2 N1 105.2(3) . . ? C17 N2 Fe1 136.4(3) . . ? N1 N2 Fe1 118.5(2) . . ? C19 N1 N2 111.0(3) . . ? C19 N1 C26 130.2(3) . . ? N2 N1 C26 118.7(3) . . ? C20 N4 N3 105.3(3) . . ? C20 N4 Fe1 135.1(2) . . ? N3 N4 Fe1 119.3(2) . . ? C22 N3 N4 110.8(3) . . ? C22 N3 C26 131.0(3) . . ? N4 N3 C26 118.1(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N7 C2 C3 109.6(3) . . ? N7 C2 C1 124.1(3) . . ? C3 C2 C1 126.4(3) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? C3 C4 N8 105.3(3) . . ? C3 C4 C5 131.7(4) . . ? N8 C4 C5 123.0(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N9 C7 C8 109.5(3) . . ? N9 C7 C6 123.9(3) . . ? C8 C7 C6 126.7(3) . . ? C9 C8 C7 107.5(3) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 N10 105.9(3) . . ? C8 C9 C10 131.3(3) . . ? N10 C9 C10 122.8(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 110.0(3) . . ? N11 C12 C11 123.7(4) . . ? C13 C12 C11 126.3(4) . . ? C14 C13 C12 107.7(3) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? N12 C14 C13 105.1(3) . . ? N12 C14 C15 123.5(3) . . ? C13 C14 C15 131.3(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N12 C16 N8 110.2(3) . . ? N12 C16 N10 110.6(3) . . ? N8 C16 N10 109.7(3) . . ? N12 C16 H16 108.8 . . ? N8 C16 H16 108.8 . . ? N10 C16 H16 108.8 . . ? N6 C23 C24 111.0(3) . . ? N6 C23 H23 124.5 . . ? C24 C23 H23 124.5 . . ? C25 C24 C23 106.1(3) . . ? C25 C24 H24 127.0 . . ? C23 C24 H24 127.0 . . ? N5 C25 C24 106.6(3) . . ? N5 C25 H25 126.7 . . ? C24 C25 H25 126.7 . . ? N2 C17 C18 110.7(4) . . ? N2 C17 H17 124.7 . . ? C18 C17 H17 124.7 . . ? C19 C18 C17 106.3(4) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? N1 C19 C18 106.9(3) . . ? N1 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? N4 C20 C21 111.1(3) . . ? N4 C20 H20 124.5 . . ? C21 C20 H20 124.5 . . ? C22 C21 C20 105.7(3) . . ? C22 C21 H21 127.2 . . ? C20 C21 H21 127.2 . . ? N3 C22 C21 107.1(3) . . ? N3 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? N1 C26 N5 108.5(3) . . ? N1 C26 N3 108.5(3) . . ? N5 C26 N3 108.3(3) . . ? N1 C26 C27 111.6(3) . . ? N5 C26 C27 108.7(3) . . ? N3 C26 C27 111.1(3) . . ? O1 C27 C26 107.4(3) . . ? O1 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O1 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O1 C28 C29 105.8(3) . . ? O1 C28 H28A 110.6 . . ? C29 C28 H28A 110.6 . . ? O1 C28 H28B 110.6 . . ? C29 C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? C30 C29 C31 119.2(3) . . ? C30 C29 C28 120.0(3) . . ? C31 C29 C28 120.7(3) . . ? C31 C30 C29 120.5(3) 3_565 . ? C31 C30 H30 119.7 3_565 . ? C29 C30 H30 119.7 . . ? C30 C31 C29 120.2(4) 3_565 . ? C30 C31 H31 119.9 3_565 . ? C29 C31 H31 119.9 . . ? O6 C32 C34 106.4(5) . . ? O6 C32 H32A 110.5 . . ? C34 C32 H32A 110.5 . . ? O6 C32 H32B 110.5 . . ? C34 C32 H32B 110.5 . . ? H32A C32 H32B 108.6 . . ? O6' C32' C34' 102(3) . . ? O6' C32' H32C 111.4 . . ? C34' C32' H32C 111.4 . . ? O6' C32' H32D 111.4 . . ? C34' C32' H32D 111.4 . . ? H32C C32' H32D 109.3 . . ? O6' C33' H33D 109.5 . . ? O6' C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? O6' C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? O5 C34 C32 110.5(5) . . ? O5 C34 H34A 109.5 . . ? C32 C34 H34A 109.5 . . ? O5 C34 H34B 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C32' C34' O5' 120(3) . . ? C32' C34' H34C 107.4 . . ? O5' C34' H34C 107.4 . . ? C32' C34' H34D 107.4 . . ? O5' C34' H34D 107.4 . . ? H34C C34' H34D 106.9 . . ? O5' C36' H36D 109.5 . . ? O5' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? O5' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? F3 B1 F2 110.7(4) . . ? F3 B1 F4 110.7(4) . . ? F2 B1 F4 107.9(4) . . ? F3 B1 F1 108.6(4) . . ? F2 B1 F1 110.0(3) . . ? F4 B1 F1 108.9(4) . . ? F7 B2 F6 111.3(4) . . ? F7 B2 F8 109.8(4) . . ? F6 B2 F8 109.8(4) . . ? F7 B2 F5 109.5(4) . . ? F6 B2 F5 106.6(4) . . ? F8 B2 F5 109.6(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 Fe1 N7 N8 C16 -1.9(4) . . . . ? Fe1 N9 N10 C16 0.7(4) . . . . ? Fe1 N11 N12 C16 -3.8(4) . . . . ? Fe1 N2 N1 C26 3.4(4) . . . . ? Fe1 N4 N3 C26 7.4(4) . . . . ? Fe1 N6 N5 C26 1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.464 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.070 # Attachment '- 1.2DME(173K).CIF' #========================================================================== data_1.2DME(173K) _database_code_depnum_ccdc_archive 'CCDC 803922' #TrackingRef '- 1.2DME(173K).CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(p-C6H4(CH2OCH2C(pz)3]2)](BF4)4(DME)2 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(p-C6H4(CH2OCH2C(pz)3)2))(BF4)4(DME)2 _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 Fe2 N24 O2, 2(C4 H10 O2), 4(B F4)' _chemical_formula_sum 'C70 H94 B4 F16 Fe2 N24 O6' _chemical_formula_weight 1826.63 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5446(5) _cell_length_b 20.7555(11) _cell_length_c 17.4704(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.932(2) _cell_angle_gamma 90.00 _cell_volume 4176.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 4076 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.47 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8069 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 X8 Apex II CCD' _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 22188 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.16 _reflns_number_total 7065 _reflns_number_gt 5181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7065 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1366 _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 Fe1 Fe 0.24337(4) 0.20708(2) 0.87714(3) 0.02495(16) Uani 1 1 d . . . N2 N 0.1126(2) 0.22129(13) 0.80155(17) 0.0307(7) Uani 1 1 d . . . N10 N 0.4403(2) 0.23848(13) 0.98047(16) 0.0271(6) Uani 1 1 d . . . N8 N 0.4210(2) 0.30400(13) 0.86900(17) 0.0300(7) Uani 1 1 d . . . N11 N 0.2041(2) 0.28133(13) 0.94216(17) 0.0295(7) Uani 1 1 d . . . C16 C 0.4113(3) 0.30225(16) 0.9509(2) 0.0289(8) Uani 1 1 d . . . H16 H 0.4671 0.3341 0.9757 0.035 Uiso 1 1 calc R . . N1 N 0.0502(2) 0.16882(12) 0.77473(16) 0.0274(6) Uani 1 1 d . . . C20 C 0.0634(3) 0.27126(17) 0.7650(2) 0.0398(9) Uani 1 1 d . . . H20 H 0.0884 0.3146 0.7719 0.048 Uiso 1 1 calc R . . N9 N 0.3726(2) 0.18790(13) 0.95408(16) 0.0264(6) Uani 1 1 d . . . N7 N 0.3505(2) 0.26471(13) 0.82345(16) 0.0299(7) Uani 1 1 d . . . C19 C 0.2467(3) 0.04005(17) 0.7553(2) 0.0321(8) Uani 1 1 d . . . H19 H 0.2058 0.0037 0.7344 0.038 Uiso 1 1 calc R . . C13 C 0.5145(3) 0.15346(18) 1.0377(2) 0.0353(9) Uani 1 1 d . . . H13 H 0.5620 0.1254 1.0692 0.042 Uiso 1 1 calc R . . C9 C 0.2597(3) 0.36889(16) 1.0129(2) 0.0315(8) Uani 1 1 d . . . N5 N 0.0715(2) 0.10777(13) 0.88939(16) 0.0261(6) Uani 1 1 d . . . C22 C -0.0366(3) 0.18687(18) 0.7227(2) 0.0387(9) Uani 1 1 d . . . H22 H -0.0916 0.1593 0.6964 0.046 Uiso 1 1 calc R . . C25 C 0.0043(3) 0.07435(16) 0.9363(2) 0.0333(8) Uani 1 1 d . . . H25 H -0.0509 0.0420 0.9212 0.040 Uiso 1 1 calc R . . C18 C 0.3631(3) 0.05094(17) 0.7550(2) 0.0364(9) Uani 1 1 d . . . H18 H 0.4194 0.0239 0.7341 0.044 Uiso 1 1 calc R . . N6 N 0.1413(2) 0.15037(13) 0.93074(16) 0.0265(6) Uani 1 1 d . . . N4 N 0.2840(2) 0.13429(13) 0.81449(16) 0.0278(6) Uani 1 1 d . . . N3 N 0.2004(2) 0.09088(12) 0.79119(16) 0.0253(6) Uani 1 1 d . . . N12 N 0.2946(2) 0.31956(13) 0.96891(16) 0.0278(6) Uani 1 1 d . . . C8 C 0.1435(3) 0.36070(18) 1.0163(2) 0.0371(9) Uani 1 1 d . . . H8 H 0.0933 0.3869 1.0440 0.044 Uiso 1 1 calc R . . C21 C -0.0296(3) 0.25209(19) 0.7153(3) 0.0493(11) Uani 1 1 d . . . H21 H -0.0782 0.2790 0.6829 0.059 Uiso 1 1 calc R . . C24 C 0.0304(3) 0.09549(17) 1.0081(2) 0.0359(9) Uani 1 1 d . . . H24 H -0.0026 0.0812 1.0534 0.043 Uiso 1 1 calc R . . C2 C 0.3825(3) 0.27402(17) 0.7521(2) 0.0339(8) Uani 1 1 d . . . C14 C 0.5278(3) 0.21865(17) 1.0310(2) 0.0319(8) Uani 1 1 d . . . C12 C 0.4182(3) 0.13590(17) 0.9895(2) 0.0299(8) Uani 1 1 d . . . C4 C 0.4979(3) 0.33688(17) 0.8279(2) 0.0362(9) Uani 1 1 d . . . O1 O 0.01079(19) 0.05054(11) 0.69389(14) 0.0319(6) Uani 1 1 d . . . C28 C -0.0481(3) -0.00504(17) 0.6599(2) 0.0360(9) Uani 1 1 d . . . H28A H -0.1326 -0.0026 0.6663 0.043 Uiso 1 1 calc R . . H28B H -0.0175 -0.0452 0.6843 0.043 Uiso 1 1 calc R . . C1 C 0.3279(3) 0.2407(2) 0.6827(2) 0.0456(10) Uani 1 1 d . . . H1A H 0.2510 0.2247 0.6938 0.068 Uiso 1 1 calc R . . H1B H 0.3768 0.2044 0.6692 0.068 Uiso 1 1 calc R . . H1C H 0.3202 0.2711 0.6398 0.068 Uiso 1 1 calc R . . C11 C 0.3704(3) 0.06913(17) 0.9779(2) 0.0413(9) Uani 1 1 d . . . H11A H 0.3382 0.0644 0.9249 0.062 Uiso 1 1 calc R . . H11B H 0.3091 0.0618 1.0131 0.062 Uiso 1 1 calc R . . H11C H 0.4327 0.0376 0.9883 0.062 Uiso 1 1 calc R . . C27 C -0.0026(3) 0.05356(17) 0.7730(2) 0.0304(8) Uani 1 1 d . . . H27A H 0.0163 0.0114 0.7973 0.037 Uiso 1 1 calc R . . H27B H -0.0838 0.0646 0.7825 0.037 Uiso 1 1 calc R . . C17 C 0.3822(3) 0.10981(17) 0.7914(2) 0.0334(8) Uani 1 1 d . . . H17 H 0.4560 0.1300 0.7988 0.040 Uiso 1 1 calc R . . C6 C -0.0093(3) 0.2818(2) 0.9561(3) 0.0498(11) Uani 1 1 d . . . H6A H -0.0092 0.2479 0.9171 0.075 Uiso 1 1 calc R . . H6B H -0.0605 0.3169 0.9375 0.075 Uiso 1 1 calc R . . H6C H -0.0373 0.2640 1.0034 0.075 Uiso 1 1 calc R . . C3 C 0.4741(3) 0.31888(19) 0.7535(2) 0.0406(9) Uani 1 1 d . . . H3 H 0.5123 0.3339 0.7104 0.049 Uiso 1 1 calc R . . C10 C 0.3391(3) 0.42000(18) 1.0448(2) 0.0430(10) Uani 1 1 d . . . H10A H 0.3719 0.4435 1.0027 0.065 Uiso 1 1 calc R . . H10B H 0.4020 0.4003 1.0774 0.065 Uiso 1 1 calc R . . H10C H 0.2958 0.4500 1.0755 0.065 Uiso 1 1 calc R . . C7 C 0.1109(3) 0.30687(16) 0.9718(2) 0.0351(9) Uani 1 1 d . . . C26 C 0.0796(3) 0.10529(15) 0.8065(2) 0.0254(7) Uani 1 1 d . . . C5 C 0.5846(4) 0.3839(2) 0.8633(2) 0.0502(11) Uani 1 1 d . . . H5A H 0.6323 0.3625 0.9044 0.075 Uiso 1 1 calc R . . H5B H 0.5436 0.4204 0.8846 0.075 Uiso 1 1 calc R . . H5C H 0.6346 0.3994 0.8241 0.075 Uiso 1 1 calc R . . C15 C 0.6168(3) 0.2632(2) 1.0678(3) 0.0486(10) Uani 1 1 d . . . H15A H 0.5790 0.2939 1.1006 0.073 Uiso 1 1 calc R . . H15B H 0.6553 0.2866 1.0280 0.073 Uiso 1 1 calc R . . H15C H 0.6746 0.2381 1.0990 0.073 Uiso 1 1 calc R . . F2 F 0.7007(3) 0.39681(17) 0.68338(19) 0.0993(12) Uani 1 1 d . . . C31 C 0.0749(3) -0.03144(17) 0.5520(2) 0.0343(8) Uani 1 1 d . . . H31 H 0.1267 -0.0531 0.5880 0.041 Uiso 1 1 calc R . . C30 C -0.1006(3) 0.02842(17) 0.5235(2) 0.0370(9) Uani 1 1 d . . . H30 H -0.1693 0.0480 0.5395 0.044 Uiso 1 1 calc R . . C29 C -0.0249(3) -0.00360(16) 0.5768(2) 0.0324(8) Uani 1 1 d . . . C23 C 0.1155(3) 0.14251(17) 1.0027(2) 0.0326(8) Uani 1 1 d . . . H23 H 0.1504 0.1658 1.0450 0.039 Uiso 1 1 calc R . . F1 F 0.8030(3) 0.45582(13) 0.60590(19) 0.0872(10) Uani 1 1 d . . . B1 B 0.8010(4) 0.4005(2) 0.6480(3) 0.0461(12) Uani 1 1 d . . . F7 F 0.6209(2) 0.08421(13) 0.55129(14) 0.0591(7) Uani 1 1 d . . . F3 F 0.8131(2) 0.34703(12) 0.60200(16) 0.0636(7) Uani 1 1 d . . . F4 F 0.8947(3) 0.40438(14) 0.6998(2) 0.1151(15) Uani 1 1 d . . . B2 B 0.6402(4) 0.0738(2) 0.6299(3) 0.0445(12) Uani 1 1 d . . . F8 F 0.5590(2) 0.10776(14) 0.66934(15) 0.0663(8) Uani 1 1 d . . . F5 F 0.74875(19) 0.09665(14) 0.65404(17) 0.0718(8) Uani 1 1 d . . . F6 F 0.6323(3) 0.00928(14) 0.64358(19) 0.0904(10) Uani 1 1 d . . . O3 O 0.2415(4) 0.6263(3) 0.6445(3) 0.1099(16) Uani 1 1 d . . . C34 C 0.3096(5) 0.5821(4) 0.6059(4) 0.104(3) Uani 1 1 d . . . H34A H 0.3865 0.6011 0.5978 0.125 Uiso 1 1 calc R . . H34B H 0.2709 0.5712 0.5552 0.125 Uiso 1 1 calc R . . C35 C 0.2619(7) 0.6863(4) 0.6293(8) 0.224(7) Uani 1 1 d . . . H35A H 0.3399 0.6904 0.6109 0.336 Uiso 1 1 calc R . . H35B H 0.2569 0.7122 0.6759 0.336 Uiso 1 1 calc R . . H35C H 0.2044 0.7017 0.5896 0.336 Uiso 1 1 calc R . . O2 O 0.2194(3) 0.48703(19) 0.6457(2) 0.0717(10) Uani 1 1 d . . . C32 C 0.2307(6) 0.4276(3) 0.6860(3) 0.101(2) Uani 1 1 d . . . H32A H 0.2621 0.4356 0.7387 0.152 Uiso 1 1 calc R . . H32B H 0.2835 0.3992 0.6602 0.152 Uiso 1 1 calc R . . H32C H 0.1544 0.4071 0.6869 0.152 Uiso 1 1 calc R . . C33 C 0.3237(5) 0.5226(5) 0.6548(4) 0.111(3) Uani 1 1 d . . . H33A H 0.3893 0.4964 0.6386 0.134 Uiso 1 1 calc R . . H33B H 0.3399 0.5347 0.7093 0.134 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 Fe1 0.0274(2) 0.0220(3) 0.0255(3) -0.0005(2) 0.0025(2) -0.00222(18) N2 0.0344(14) 0.0232(15) 0.0345(18) -0.0008(13) 0.0027(14) -0.0044(11) N10 0.0279(13) 0.0300(15) 0.0238(16) -0.0006(13) 0.0031(12) -0.0003(11) N8 0.0319(14) 0.0298(16) 0.0286(17) -0.0012(13) 0.0037(13) -0.0075(12) N11 0.0301(14) 0.0251(15) 0.0333(18) -0.0032(13) 0.0027(13) -0.0029(11) C16 0.0331(17) 0.0289(18) 0.025(2) -0.0025(15) 0.0039(15) -0.0026(14) N1 0.0292(13) 0.0225(14) 0.0298(17) 0.0011(13) -0.0024(13) -0.0029(11) C20 0.048(2) 0.0233(18) 0.047(3) 0.0065(17) -0.0076(19) 0.0005(16) N9 0.0287(13) 0.0265(15) 0.0243(16) -0.0022(13) 0.0044(12) -0.0021(11) N7 0.0347(14) 0.0287(15) 0.0258(17) -0.0005(13) -0.0001(13) -0.0043(12) C19 0.0359(18) 0.0300(19) 0.031(2) -0.0082(16) 0.0047(16) 0.0011(14) C13 0.0379(18) 0.037(2) 0.031(2) 0.0019(17) -0.0004(17) 0.0093(15) C9 0.0416(19) 0.0240(18) 0.028(2) -0.0006(15) 0.0001(16) 0.0067(14) N5 0.0261(13) 0.0269(15) 0.0256(16) -0.0017(13) 0.0037(12) -0.0034(11) C22 0.0373(19) 0.035(2) 0.042(2) 0.0025(18) -0.0128(18) 0.0009(15) C25 0.0328(17) 0.0291(19) 0.039(2) 0.0026(17) 0.0108(17) -0.0053(14) C18 0.0357(18) 0.036(2) 0.038(2) -0.0084(18) 0.0069(17) 0.0039(15) N6 0.0314(14) 0.0253(15) 0.0232(17) -0.0025(12) 0.0045(13) -0.0012(11) N4 0.0284(14) 0.0288(15) 0.0264(17) 0.0007(13) 0.0030(13) -0.0021(11) N3 0.0264(13) 0.0242(14) 0.0256(16) -0.0023(12) 0.0033(12) -0.0017(11) N12 0.0275(13) 0.0254(14) 0.0306(17) -0.0030(13) 0.0019(13) 0.0001(11) C8 0.0364(18) 0.034(2) 0.041(2) -0.0043(18) 0.0044(18) 0.0112(15) C21 0.055(2) 0.036(2) 0.055(3) 0.009(2) -0.014(2) 0.0057(18) C24 0.043(2) 0.038(2) 0.029(2) 0.0018(17) 0.0123(17) -0.0020(16) C2 0.0416(19) 0.0324(19) 0.028(2) 0.0021(16) 0.0035(17) -0.0040(15) C14 0.0313(17) 0.041(2) 0.023(2) -0.0023(16) 0.0011(15) 0.0047(15) C12 0.0345(17) 0.0344(19) 0.0214(19) 0.0001(16) 0.0057(15) 0.0050(15) C4 0.0406(19) 0.036(2) 0.033(2) 0.0043(17) 0.0060(18) -0.0089(16) O1 0.0383(12) 0.0294(13) 0.0276(14) -0.0039(11) -0.0012(11) -0.0099(10) C28 0.0404(19) 0.0314(19) 0.036(2) -0.0039(17) -0.0010(17) -0.0091(15) C1 0.058(2) 0.052(2) 0.027(2) -0.0032(19) 0.0008(19) -0.015(2) C11 0.051(2) 0.033(2) 0.040(2) 0.0076(18) 0.0043(19) 0.0038(17) C27 0.0319(17) 0.0317(18) 0.028(2) -0.0024(16) 0.0004(16) -0.0041(14) C17 0.0280(16) 0.041(2) 0.031(2) 0.0001(17) 0.0060(16) 0.0005(15) C6 0.0344(19) 0.044(2) 0.072(3) -0.012(2) 0.008(2) 0.0030(17) C3 0.051(2) 0.044(2) 0.028(2) 0.0064(18) 0.0100(18) -0.0110(18) C10 0.045(2) 0.036(2) 0.047(3) -0.0142(19) -0.0038(19) 0.0047(16) C7 0.0328(18) 0.0287(19) 0.044(2) -0.0015(17) 0.0032(17) 0.0031(14) C26 0.0266(15) 0.0240(17) 0.0256(19) -0.0007(14) 0.0014(14) -0.0009(13) C5 0.053(2) 0.056(3) 0.043(3) 0.001(2) 0.005(2) -0.026(2) C15 0.045(2) 0.049(2) 0.050(3) -0.008(2) -0.014(2) 0.0026(18) F2 0.098(2) 0.121(3) 0.085(2) -0.035(2) 0.047(2) -0.061(2) C31 0.0388(18) 0.0293(19) 0.034(2) 0.0006(17) -0.0058(17) -0.0005(15) C30 0.0378(18) 0.034(2) 0.038(2) -0.0078(18) -0.0019(17) -0.0019(15) C29 0.0379(18) 0.0264(18) 0.032(2) -0.0043(16) -0.0019(17) -0.0084(14) C23 0.0362(18) 0.034(2) 0.027(2) -0.0043(16) 0.0028(16) 0.0012(15) F1 0.129(3) 0.0495(16) 0.089(2) 0.0199(16) 0.053(2) 0.0248(17) B1 0.044(2) 0.037(3) 0.056(3) 0.001(2) -0.005(2) -0.0049(19) F7 0.0621(15) 0.0740(17) 0.0415(15) 0.0033(13) 0.0068(12) 0.0044(13) F3 0.0674(15) 0.0433(14) 0.0778(19) -0.0057(14) -0.0109(14) -0.0014(12) F4 0.117(3) 0.0503(17) 0.165(4) -0.029(2) -0.086(3) 0.0055(17) B2 0.031(2) 0.057(3) 0.045(3) 0.007(2) 0.002(2) 0.002(2) F8 0.0428(13) 0.107(2) 0.0506(16) 0.0034(16) 0.0123(12) 0.0043(13) F5 0.0380(12) 0.094(2) 0.082(2) -0.0287(17) -0.0033(13) -0.0011(13) F6 0.126(3) 0.0615(19) 0.080(2) 0.0165(17) -0.0148(19) -0.0187(18) O3 0.096(3) 0.140(4) 0.099(3) -0.038(3) 0.038(3) -0.050(3) C34 0.073(4) 0.168(7) 0.078(5) -0.050(5) 0.046(4) -0.044(4) C35 0.134(7) 0.095(6) 0.46(2) 0.113(9) 0.138(10) 0.035(5) O2 0.0507(18) 0.101(3) 0.062(2) -0.012(2) -0.0026(16) 0.0198(18) C32 0.148(6) 0.098(5) 0.057(4) 0.002(3) 0.004(4) 0.073(4) C33 0.054(3) 0.214(9) 0.067(4) -0.044(5) 0.006(3) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.942(3) . ? Fe1 N6 1.950(3) . ? Fe1 N2 1.959(3) . ? Fe1 N9 1.979(3) . ? Fe1 N11 1.985(3) . ? Fe1 N7 2.000(3) . ? N2 C20 1.325(4) . ? N2 N1 1.371(4) . ? N10 C14 1.360(4) . ? N10 N9 1.370(4) . ? N10 C16 1.451(4) . ? N8 C4 1.362(4) . ? N8 N7 1.368(4) . ? N8 C16 1.443(4) . ? N11 C7 1.336(4) . ? N11 N12 1.369(4) . ? C16 N12 1.450(4) . ? C16 H16 1.0000 . ? N1 C22 1.358(4) . ? N1 C26 1.461(4) . ? C20 C21 1.392(5) . ? C20 H20 0.9500 . ? N9 C12 1.335(4) . ? N7 C2 1.338(5) . ? C19 N3 1.356(4) . ? C19 C18 1.363(5) . ? C19 H19 0.9500 . ? C13 C14 1.367(5) . ? C13 C12 1.396(5) . ? C13 H13 0.9500 . ? C9 C8 1.357(5) . ? C9 N12 1.358(4) . ? C9 C10 1.486(5) . ? N5 C25 1.357(4) . ? N5 N6 1.369(4) . ? N5 C26 1.459(4) . ? C22 C21 1.363(5) . ? C22 H22 0.9500 . ? C25 C24 1.343(5) . ? C25 H25 0.9500 . ? C18 C17 1.388(5) . ? C18 H18 0.9500 . ? N6 C23 1.321(4) . ? N4 C17 1.331(4) . ? N4 N3 1.362(4) . ? N3 C26 1.468(4) . ? C8 C7 1.398(5) . ? C8 H8 0.9500 . ? C21 H21 0.9500 . ? C24 C23 1.393(5) . ? C24 H24 0.9500 . ? C2 C3 1.408(5) . ? C2 C1 1.496(5) . ? C14 C15 1.494(5) . ? C12 C11 1.500(5) . ? C4 C3 1.363(5) . ? C4 C5 1.501(5) . ? O1 C27 1.403(4) . ? O1 C28 1.446(4) . ? C28 C29 1.494(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C27 C26 1.523(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C17 H17 0.9500 . ? C6 C7 1.489(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C3 H3 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? F2 B1 1.352(6) . ? C31 C30 1.374(5) 3_556 ? C31 C29 1.385(5) . ? C31 H31 0.9500 . ? C30 C31 1.374(5) 3_556 ? C30 C29 1.400(5) . ? C30 H30 0.9500 . ? C23 H23 0.9500 . ? F1 B1 1.364(5) . ? B1 F4 1.364(5) . ? B1 F3 1.384(5) . ? F7 B2 1.393(6) . ? B2 F6 1.365(6) . ? B2 F5 1.379(5) . ? B2 F8 1.392(5) . ? O3 C35 1.299(8) . ? O3 C34 1.410(8) . ? C34 C33 1.504(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O2 C33 1.411(7) . ? O2 C32 1.422(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N6 88.76(11) . . ? N4 Fe1 N2 86.68(11) . . ? N6 Fe1 N2 87.21(11) . . ? N4 Fe1 N9 91.51(11) . . ? N6 Fe1 N9 90.27(11) . . ? N2 Fe1 N9 176.92(11) . . ? N4 Fe1 N11 179.13(12) . . ? N6 Fe1 N11 91.40(11) . . ? N2 Fe1 N11 94.18(12) . . ? N9 Fe1 N11 87.64(11) . . ? N4 Fe1 N7 91.14(11) . . ? N6 Fe1 N7 178.95(12) . . ? N2 Fe1 N7 93.83(11) . . ? N9 Fe1 N7 88.69(11) . . ? N11 Fe1 N7 88.69(12) . . ? C20 N2 N1 105.1(3) . . ? C20 N2 Fe1 136.7(2) . . ? N1 N2 Fe1 118.3(2) . . ? C14 N10 N9 111.6(3) . . ? C14 N10 C16 130.5(3) . . ? N9 N10 C16 117.9(3) . . ? C4 N8 N7 112.0(3) . . ? C4 N8 C16 129.2(3) . . ? N7 N8 C16 118.6(3) . . ? C7 N11 N12 104.7(3) . . ? C7 N11 Fe1 138.8(2) . . ? N12 N11 Fe1 116.5(2) . . ? N8 C16 N12 110.2(3) . . ? N8 C16 N10 110.2(3) . . ? N12 C16 N10 110.1(3) . . ? N8 C16 H16 108.8 . . ? N12 C16 H16 108.8 . . ? N10 C16 H16 108.8 . . ? C22 N1 N2 110.8(3) . . ? C22 N1 C26 130.1(3) . . ? N2 N1 C26 118.9(3) . . ? N2 C20 C21 111.3(3) . . ? N2 C20 H20 124.4 . . ? C21 C20 H20 124.4 . . ? C12 N9 N10 105.4(3) . . ? C12 N9 Fe1 137.2(2) . . ? N10 N9 Fe1 117.4(2) . . ? C2 N7 N8 105.4(3) . . ? C2 N7 Fe1 137.9(2) . . ? N8 N7 Fe1 116.5(2) . . ? N3 C19 C18 107.1(3) . . ? N3 C19 H19 126.5 . . ? C18 C19 H19 126.5 . . ? C14 C13 C12 107.2(3) . . ? C14 C13 H13 126.4 . . ? C12 C13 H13 126.4 . . ? C8 C9 N12 105.3(3) . . ? C8 C9 C10 131.2(3) . . ? N12 C9 C10 123.4(3) . . ? C25 N5 N6 110.6(3) . . ? C25 N5 C26 131.3(3) . . ? N6 N5 C26 118.1(2) . . ? N1 C22 C21 106.9(3) . . ? N1 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? C24 C25 N5 107.2(3) . . ? C24 C25 H25 126.4 . . ? N5 C25 H25 126.4 . . ? C19 C18 C17 105.6(3) . . ? C19 C18 H18 127.2 . . ? C17 C18 H18 127.2 . . ? C23 N6 N5 105.0(3) . . ? C23 N6 Fe1 135.6(2) . . ? N5 N6 Fe1 119.3(2) . . ? C17 N4 N3 104.9(3) . . ? C17 N4 Fe1 135.4(2) . . ? N3 N4 Fe1 119.30(19) . . ? C19 N3 N4 111.0(3) . . ? C19 N3 C26 130.7(3) . . ? N4 N3 C26 118.2(2) . . ? C9 N12 N11 112.4(3) . . ? C9 N12 C16 128.8(3) . . ? N11 N12 C16 118.8(3) . . ? C9 C8 C7 107.7(3) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C22 C21 C20 105.9(3) . . ? C22 C21 H21 127.1 . . ? C20 C21 H21 127.1 . . ? C25 C24 C23 106.3(3) . . ? C25 C24 H24 126.9 . . ? C23 C24 H24 126.9 . . ? N7 C2 C3 109.5(3) . . ? N7 C2 C1 124.1(3) . . ? C3 C2 C1 126.4(3) . . ? N10 C14 C13 105.8(3) . . ? N10 C14 C15 123.4(3) . . ? C13 C14 C15 130.8(3) . . ? N9 C12 C13 110.0(3) . . ? N9 C12 C11 123.7(3) . . ? C13 C12 C11 126.4(3) . . ? N8 C4 C3 105.6(3) . . ? N8 C4 C5 123.3(3) . . ? C3 C4 C5 131.0(3) . . ? C27 O1 C28 111.1(3) . . ? O1 C28 C29 105.8(3) . . ? O1 C28 H28A 110.6 . . ? C29 C28 H28A 110.6 . . ? O1 C28 H28B 110.6 . . ? C29 C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C27 C26 107.5(3) . . ? O1 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O1 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? N4 C17 C18 111.3(3) . . ? N4 C17 H17 124.3 . . ? C18 C17 H17 124.3 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C3 C2 107.5(3) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N11 C7 C8 109.8(3) . . ? N11 C7 C6 123.7(3) . . ? C8 C7 C6 126.4(3) . . ? N5 C26 N1 108.4(3) . . ? N5 C26 N3 108.3(2) . . ? N1 C26 N3 108.3(2) . . ? N5 C26 C27 109.0(3) . . ? N1 C26 C27 111.6(3) . . ? N3 C26 C27 111.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C30 C31 C29 121.3(3) 3_556 . ? C30 C31 H31 119.3 3_556 . ? C29 C31 H31 119.3 . . ? C31 C30 C29 119.7(3) 3_556 . ? C31 C30 H30 120.2 3_556 . ? C29 C30 H30 120.2 . . ? C31 C29 C30 119.0(3) . . ? C31 C29 C28 120.3(3) . . ? C30 C29 C28 120.7(3) . . ? N6 C23 C24 110.9(3) . . ? N6 C23 H23 124.6 . . ? C24 C23 H23 124.6 . . ? F2 B1 F4 111.5(5) . . ? F2 B1 F1 109.9(4) . . ? F4 B1 F1 105.5(4) . . ? F2 B1 F3 110.1(4) . . ? F4 B1 F3 109.0(4) . . ? F1 B1 F3 110.8(4) . . ? F6 B2 F5 110.7(4) . . ? F6 B2 F8 110.8(4) . . ? F5 B2 F8 107.7(4) . . ? F6 B2 F7 108.5(4) . . ? F5 B2 F7 109.2(4) . . ? F8 B2 F7 110.0(3) . . ? C35 O3 C34 114.3(6) . . ? O3 C34 C33 107.8(5) . . ? O3 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? O3 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? O3 C35 H35A 109.5 . . ? O3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 O2 C32 110.4(5) . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 107.9(5) . . ? O2 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? O2 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? 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 Fe1 N7 N8 C16 -1.4(4) . . . . ? Fe1 N9 N10 C16 0.8(3) . . . . ? Fe1 N11 N12 C16 -2.3(4) . . . . ? Fe1 N2 N1 C26 3.2(4) . . . . ? Fe1 N4 N3 C26 7.5(4) . . . . ? Fe1 N6 N5 C26 2.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.604 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.073 # Attachment '- 1.2DME(223K).CIF' #========================================================================== data_1.2DME(223K) _database_code_depnum_ccdc_archive 'CCDC 803923' #TrackingRef '- 1.2DME(223K).CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(p-C6H4(CH2OCH2C(pz)3]2)](BF4)4(DME)2 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(p-C6H4(CH2OCH2C(pz)3)2))(BF4)4(DME)2 _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 Fe2 N24 O2, 2(C4 H10 O2), 4(B F4)' _chemical_formula_sum 'C70 H94 B4 F16 Fe2 N24 O6' _chemical_formula_weight 1826.63 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6011(10) _cell_length_b 20.802(2) _cell_length_c 17.4828(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.192(4) _cell_angle_gamma 90.00 _cell_volume 4207.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(1) _cell_measurement_reflns_used 6145 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.19 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(1) _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 X8 Apex II CCD' _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 40611 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9468 _reflns_number_gt 6147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9468 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Fe1 Fe 0.24538(4) 0.70710(2) 0.37660(3) 0.03040(15) Uani 1 1 d . . . N6 N 0.1434(2) 0.65067(13) 0.42986(15) 0.0332(6) Uani 1 1 d . . . O1 O 0.0140(2) 0.55058(11) 0.19346(13) 0.0400(6) Uani 1 1 d . . . N10 N 0.4415(2) 0.73875(13) 0.48004(16) 0.0335(6) Uani 1 1 d . . . N11 N 0.2060(2) 0.78148(13) 0.44095(17) 0.0357(7) Uani 1 1 d . . . N3 N 0.2031(2) 0.59093(12) 0.29098(15) 0.0305(6) Uani 1 1 d . . . N9 N 0.3742(2) 0.68815(13) 0.45347(16) 0.0336(6) Uani 1 1 d . . . N5 N 0.0748(2) 0.60800(12) 0.38865(16) 0.0315(6) Uani 1 1 d . . . N2 N 0.1157(3) 0.72102(13) 0.30085(17) 0.0377(7) Uani 1 1 d . . . N12 N 0.2959(2) 0.81956(13) 0.46769(16) 0.0337(6) Uani 1 1 d . . . N8 N 0.4213(2) 0.80415(14) 0.36850(16) 0.0371(7) Uani 1 1 d . . . N4 N 0.2858(2) 0.63415(13) 0.31460(15) 0.0324(6) Uani 1 1 d . . . N7 N 0.3516(2) 0.76472(13) 0.32300(16) 0.0346(6) Uani 1 1 d . . . N1 N 0.0537(2) 0.66869(12) 0.27423(16) 0.0342(6) Uani 1 1 d . . . C26 C 0.0832(3) 0.60542(15) 0.30633(19) 0.0311(7) Uani 1 1 d . . . C16 C 0.4125(3) 0.80231(16) 0.4502(2) 0.0355(8) Uani 1 1 d . . . H16 H 0.4673 0.8339 0.4748 0.043 Uiso 1 1 calc R . . C14 C 0.2613(3) 0.86875(16) 0.5121(2) 0.0391(8) Uani 1 1 d . . . C27 C 0.0012(3) 0.55377(16) 0.2726(2) 0.0365(8) Uani 1 1 d . . . H27A H 0.0200 0.5121 0.2967 0.044 Uiso 1 1 calc R . . H27B H -0.0788 0.5647 0.2820 0.044 Uiso 1 1 calc R . . C20 C 0.3836(3) 0.61010(17) 0.2923(2) 0.0398(8) Uani 1 1 d . . . H20 H 0.4561 0.6301 0.3002 0.048 Uiso 1 1 calc R . . C23 C 0.1176(3) 0.64286(18) 0.5019(2) 0.0407(8) Uani 1 1 d . . . H23 H 0.1515 0.6661 0.5439 0.049 Uiso 1 1 calc R . . C22 C 0.2492(3) 0.54049(16) 0.2556(2) 0.0404(8) Uani 1 1 d . . . H22 H 0.2091 0.5045 0.2349 0.049 Uiso 1 1 calc R . . C31 C -0.0988(3) 0.52828(17) 0.0242(2) 0.0425(9) Uani 1 1 d . . . H31 H -0.1662 0.5475 0.0405 0.051 Uiso 1 1 calc R . . C7 C 0.4199(3) 0.63644(17) 0.4895(2) 0.0376(8) Uani 1 1 d . . . C2 C 0.3830(3) 0.77417(18) 0.2521(2) 0.0428(9) Uani 1 1 d . . . C13 C 0.1452(3) 0.86053(18) 0.5151(2) 0.0458(9) Uani 1 1 d . . . H13 H 0.0957 0.8861 0.5426 0.055 Uiso 1 1 calc R . . C25 C 0.0075(3) 0.57481(17) 0.4351(2) 0.0388(8) Uani 1 1 d . . . H25 H -0.0472 0.5431 0.4199 0.047 Uiso 1 1 calc R . . C4 C 0.4966(3) 0.83745(18) 0.3277(2) 0.0449(9) Uani 1 1 d . . . C9 C 0.5287(3) 0.71924(18) 0.5302(2) 0.0408(9) Uani 1 1 d . . . C30 C 0.0752(3) 0.46862(17) 0.0515(2) 0.0420(9) Uani 1 1 d . . . H30 H 0.1266 0.4471 0.0867 0.050 Uiso 1 1 calc R . . C29 C -0.0232(3) 0.49677(17) 0.0765(2) 0.0399(8) Uani 1 1 d . . . C8 C 0.5155(3) 0.65450(19) 0.5369(2) 0.0452(9) Uani 1 1 d . . . H8 H 0.5628 0.6269 0.5681 0.054 Uiso 1 1 calc R . . C21 C 0.3646(3) 0.55143(18) 0.2556(2) 0.0440(9) Uani 1 1 d . . . H21 H 0.4201 0.5248 0.2350 0.053 Uiso 1 1 calc R . . C17 C 0.0671(4) 0.77080(18) 0.2639(2) 0.0508(10) Uani 1 1 d . . . H17 H 0.0914 0.8137 0.2707 0.061 Uiso 1 1 calc R . . C28 C -0.0448(3) 0.49547(17) 0.1593(2) 0.0418(9) Uani 1 1 d . . . H28A H -0.1278 0.4979 0.1658 0.050 Uiso 1 1 calc R . . H28B H -0.0144 0.4557 0.1832 0.050 Uiso 1 1 calc R . . C3 C 0.4728(4) 0.81938(19) 0.2538(2) 0.0501(10) Uani 1 1 d . . . H3 H 0.5099 0.8345 0.2112 0.060 Uiso 1 1 calc R . . C12 C 0.1132(3) 0.80720(17) 0.4699(2) 0.0425(9) Uani 1 1 d . . . C1 C 0.3287(4) 0.7407(2) 0.1830(2) 0.0564(11) Uani 1 1 d . . . H1A H 0.3803 0.7073 0.1671 0.085 Uiso 1 1 calc R . . H1B H 0.3144 0.7714 0.1417 0.085 Uiso 1 1 calc R . . H1C H 0.2562 0.7215 0.1954 0.085 Uiso 1 1 calc R . . C19 C -0.0315(3) 0.68653(19) 0.2216(2) 0.0476(9) Uani 1 1 d . . . H19 H -0.0855 0.6593 0.1953 0.057 Uiso 1 1 calc R . . C24 C 0.0339(3) 0.59588(18) 0.5072(2) 0.0452(9) Uani 1 1 d . . . H24 H 0.0019 0.5815 0.5520 0.054 Uiso 1 1 calc R . . C15 C 0.3409(4) 0.91963(19) 0.5448(3) 0.0544(11) Uani 1 1 d . . . H15A H 0.4005 0.9001 0.5791 0.082 Uiso 1 1 calc R . . H15B H 0.2975 0.9503 0.5732 0.082 Uiso 1 1 calc R . . H15C H 0.3763 0.9416 0.5036 0.082 Uiso 1 1 calc R . . C18 C -0.0243(4) 0.7513(2) 0.2141(3) 0.0608(12) Uani 1 1 d . . . H18 H -0.0719 0.7776 0.1816 0.073 Uiso 1 1 calc R . . C6 C 0.3733(4) 0.56988(17) 0.4778(2) 0.0514(10) Uani 1 1 d . . . H6A H 0.3152 0.5618 0.5138 0.077 Uiso 1 1 calc R . . H6B H 0.4358 0.5391 0.4861 0.077 Uiso 1 1 calc R . . H6C H 0.3389 0.5656 0.4258 0.077 Uiso 1 1 calc R . . C5 C 0.5829(4) 0.8843(2) 0.3636(3) 0.0639(13) Uani 1 1 d . . . H5A H 0.5425 0.9205 0.3843 0.096 Uiso 1 1 calc R . . H5B H 0.6326 0.8995 0.3252 0.096 Uiso 1 1 calc R . . H5C H 0.6295 0.8632 0.4046 0.096 Uiso 1 1 calc R . . C11 C -0.0075(3) 0.7820(2) 0.4537(3) 0.0627(13) Uani 1 1 d . . . H11A H -0.0570 0.8161 0.4325 0.094 Uiso 1 1 calc R . . H11B H -0.0367 0.7665 0.5010 0.094 Uiso 1 1 calc R . . H11C H -0.0067 0.7469 0.4172 0.094 Uiso 1 1 calc R . . C10 C 0.6177(4) 0.7638(2) 0.5670(3) 0.0621(12) Uani 1 1 d . . . H10A H 0.6552 0.7870 0.5275 0.093 Uiso 1 1 calc R . . H10B H 0.6750 0.7392 0.5977 0.093 Uiso 1 1 calc R . . H10C H 0.5807 0.7942 0.5995 0.093 Uiso 1 1 calc R . . F1 F 0.3773(2) 0.41700(14) 0.94792(15) 0.0760(8) Uani 1 1 d . . . F3 F 0.4393(2) 0.39259(17) 0.83143(16) 0.0874(9) Uani 1 1 d . . . F4 F 0.2514(2) 0.40402(16) 0.84514(19) 0.0916(10) Uani 1 1 d . . . B1 B 0.3587(4) 0.4270(3) 0.8696(3) 0.0566(13) Uani 1 1 d . . . F2 F 0.3668(4) 0.49039(17) 0.8564(2) 0.1203(13) Uani 1 1 d . . . F6 F 0.1862(2) 0.34666(13) 0.39697(18) 0.0812(8) Uani 1 1 d . . . F5 F 0.1955(4) 0.45444(15) 0.3926(2) 0.1170(14) Uani 1 1 d . . . F8 F 0.2966(4) 0.3963(2) 0.3170(2) 0.1387(17) Uani 1 1 d . . . F7 F 0.1045(4) 0.40406(16) 0.3015(3) 0.157(2) Uani 1 1 d . . . B2 B 0.1969(5) 0.3996(2) 0.3510(3) 0.0603(14) Uani 1 1 d . . . O3 O 0.7654(4) 0.6308(4) 0.3568(3) 0.150(2) Uani 1 1 d . . . C34 C 0.6989(8) 0.5867(6) 0.3981(5) 0.156(4) Uani 1 1 d . . . H34A H 0.6245 0.6058 0.4086 0.188 Uiso 1 1 calc R . . H34B H 0.7405 0.5752 0.4470 0.188 Uiso 1 1 calc R . . C35 C 0.7315(10) 0.6906(5) 0.3582(10) 0.297(11) Uani 1 1 d . . . H35A H 0.6536 0.6926 0.3748 0.445 Uiso 1 1 calc R . . H35B H 0.7324 0.7090 0.3072 0.445 Uiso 1 1 calc R . . H35C H 0.7832 0.7148 0.3935 0.445 Uiso 1 1 calc R . . O2 O 0.7817(3) 0.4901(2) 0.3545(2) 0.0948(13) Uani 1 1 d . . . C32 C 0.7677(8) 0.4305(4) 0.3139(4) 0.130(3) Uani 1 1 d . . . H32A H 0.7065 0.4056 0.3347 0.194 Uiso 1 1 calc R . . H32B H 0.8394 0.4064 0.3194 0.194 Uiso 1 1 calc R . . H32C H 0.7478 0.4390 0.2600 0.194 Uiso 1 1 calc R . . C33 C 0.6806(6) 0.5286(6) 0.3486(5) 0.163(5) Uani 1 1 d . . . H33A H 0.6148 0.5039 0.3648 0.195 Uiso 1 1 calc R . . H33B H 0.6633 0.5418 0.2951 0.195 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 Fe1 0.0328(3) 0.0289(2) 0.0294(3) -0.00047(19) 0.0024(2) -0.00174(19) N6 0.0381(16) 0.0330(15) 0.0284(15) -0.0020(12) 0.0031(13) 0.0010(12) O1 0.0477(15) 0.0413(13) 0.0305(13) -0.0051(10) -0.0009(11) -0.0123(11) N10 0.0346(15) 0.0356(15) 0.0299(16) 0.0003(12) 0.0001(13) -0.0008(12) N11 0.0326(15) 0.0335(15) 0.0411(17) -0.0025(12) 0.0023(13) -0.0038(12) N3 0.0305(14) 0.0292(14) 0.0318(16) -0.0026(11) 0.0029(12) -0.0016(11) N9 0.0364(16) 0.0347(15) 0.0298(15) 0.0003(12) 0.0032(13) -0.0010(12) N5 0.0323(15) 0.0319(14) 0.0306(15) 0.0006(11) 0.0047(12) -0.0034(11) N2 0.0443(17) 0.0280(15) 0.0402(18) -0.0003(12) -0.0010(14) -0.0027(12) N12 0.0336(15) 0.0319(14) 0.0353(16) -0.0032(12) 0.0007(13) 0.0025(12) N8 0.0399(16) 0.0426(17) 0.0287(16) 0.0010(12) 0.0026(13) -0.0110(13) N4 0.0342(15) 0.0346(15) 0.0287(15) 0.0018(12) 0.0030(12) -0.0013(12) N7 0.0398(16) 0.0367(15) 0.0268(15) 0.0016(12) -0.0019(13) -0.0045(12) N1 0.0365(16) 0.0290(14) 0.0361(17) 0.0023(12) -0.0047(13) -0.0010(11) C26 0.0355(18) 0.0283(16) 0.0297(18) 0.0017(13) 0.0036(15) -0.0013(13) C16 0.0372(19) 0.0362(18) 0.0330(19) -0.0031(14) 0.0020(15) -0.0026(14) C14 0.048(2) 0.0351(18) 0.033(2) -0.0029(15) -0.0045(16) 0.0090(15) C27 0.0390(19) 0.0363(18) 0.035(2) -0.0031(15) 0.0045(16) -0.0041(14) C20 0.0364(19) 0.046(2) 0.038(2) -0.0015(16) 0.0070(16) -0.0010(15) C23 0.047(2) 0.046(2) 0.0297(19) -0.0044(16) 0.0064(16) 0.0005(16) C22 0.048(2) 0.0333(18) 0.041(2) -0.0087(15) 0.0064(17) 0.0014(15) C31 0.040(2) 0.043(2) 0.044(2) -0.0062(17) -0.0033(17) -0.0026(16) C7 0.041(2) 0.0407(19) 0.0315(19) 0.0017(15) 0.0048(16) 0.0064(15) C2 0.052(2) 0.044(2) 0.033(2) 0.0021(16) 0.0036(17) -0.0067(17) C13 0.043(2) 0.043(2) 0.051(2) -0.0075(18) 0.0007(18) 0.0121(16) C25 0.0362(19) 0.0407(19) 0.040(2) 0.0029(16) 0.0084(16) -0.0071(15) C4 0.052(2) 0.043(2) 0.040(2) 0.0043(17) 0.0101(18) -0.0121(17) C9 0.037(2) 0.053(2) 0.031(2) -0.0036(16) -0.0033(16) 0.0097(16) C30 0.047(2) 0.040(2) 0.037(2) 0.0010(16) -0.0095(17) 0.0003(16) C29 0.046(2) 0.0358(18) 0.037(2) -0.0065(16) -0.0064(17) -0.0106(16) C8 0.046(2) 0.051(2) 0.037(2) 0.0026(17) -0.0038(18) 0.0128(17) C21 0.041(2) 0.046(2) 0.046(2) -0.0090(17) 0.0091(18) 0.0039(16) C17 0.055(2) 0.0312(19) 0.065(3) 0.0085(18) -0.009(2) 0.0021(17) C28 0.048(2) 0.0376(19) 0.039(2) -0.0037(16) -0.0033(17) -0.0124(16) C3 0.064(3) 0.056(2) 0.032(2) 0.0070(18) 0.0112(19) -0.014(2) C12 0.037(2) 0.038(2) 0.053(2) -0.0028(17) 0.0041(18) 0.0037(15) C1 0.073(3) 0.064(3) 0.032(2) -0.0001(19) 0.000(2) -0.017(2) C19 0.045(2) 0.043(2) 0.052(3) 0.0021(18) -0.0148(19) 0.0006(17) C24 0.051(2) 0.054(2) 0.032(2) 0.0024(17) 0.0161(18) -0.0048(18) C15 0.053(2) 0.049(2) 0.059(3) -0.024(2) -0.008(2) 0.0046(18) C18 0.066(3) 0.045(2) 0.067(3) 0.011(2) -0.022(2) 0.010(2) C6 0.066(3) 0.034(2) 0.055(3) 0.0077(18) 0.007(2) 0.0061(18) C5 0.065(3) 0.071(3) 0.056(3) -0.001(2) 0.006(2) -0.036(2) C11 0.039(2) 0.058(3) 0.091(4) -0.014(2) 0.008(2) 0.0060(19) C10 0.052(3) 0.065(3) 0.066(3) -0.013(2) -0.017(2) 0.005(2) F1 0.0773(18) 0.097(2) 0.0541(17) 0.0065(15) 0.0106(14) 0.0078(15) F3 0.0543(16) 0.143(3) 0.0670(19) 0.0060(18) 0.0171(14) 0.0079(17) F4 0.0436(15) 0.123(3) 0.107(3) -0.034(2) -0.0012(15) 0.0004(15) B1 0.042(3) 0.070(3) 0.058(3) 0.008(3) 0.004(2) 0.000(2) F2 0.167(4) 0.087(2) 0.102(3) 0.027(2) -0.021(3) -0.031(2) F6 0.083(2) 0.0573(16) 0.100(2) 0.0118(15) -0.0162(17) 0.0004(14) F5 0.182(4) 0.0630(19) 0.114(3) -0.0199(18) 0.063(3) -0.031(2) F8 0.136(3) 0.163(4) 0.126(3) 0.052(3) 0.073(3) 0.080(3) F7 0.165(4) 0.070(2) 0.216(5) 0.038(3) -0.129(4) -0.007(2) B2 0.069(4) 0.044(3) 0.065(4) 0.002(2) -0.007(3) 0.004(2) O3 0.110(4) 0.218(7) 0.128(4) 0.047(4) 0.047(3) 0.065(4) C34 0.110(6) 0.262(12) 0.104(6) 0.038(7) 0.060(6) 0.073(7) C35 0.167(10) 0.126(8) 0.62(3) -0.153(14) 0.154(15) -0.024(7) O2 0.064(2) 0.143(4) 0.076(3) 0.019(3) -0.003(2) -0.021(2) C32 0.179(8) 0.129(6) 0.078(5) 0.002(4) -0.010(5) -0.082(6) C33 0.058(4) 0.333(15) 0.098(6) 0.103(8) 0.009(4) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.942(3) . ? Fe1 N6 1.950(3) . ? Fe1 N2 1.952(3) . ? Fe1 N9 1.975(3) . ? Fe1 N11 1.986(3) . ? Fe1 N7 2.001(3) . ? N6 C23 1.326(4) . ? N6 N5 1.363(4) . ? O1 C27 1.405(4) . ? O1 C28 1.441(4) . ? N10 C9 1.351(4) . ? N10 N9 1.371(4) . ? N10 C16 1.452(4) . ? N11 C12 1.334(4) . ? N11 N12 1.365(4) . ? N3 C22 1.348(4) . ? N3 N4 1.357(4) . ? N3 C26 1.467(4) . ? N9 C7 1.336(4) . ? N5 C25 1.355(4) . ? N5 C26 1.451(4) . ? N2 C17 1.325(4) . ? N2 N1 1.368(4) . ? N12 C14 1.362(4) . ? N12 C16 1.453(4) . ? N8 C4 1.357(4) . ? N8 N7 1.366(4) . ? N8 C16 1.441(4) . ? N4 C20 1.324(4) . ? N7 C2 1.332(4) . ? N1 C19 1.352(5) . ? N1 C26 1.462(4) . ? C26 C27 1.525(5) . ? C16 H16 0.9900 . ? C14 C13 1.362(5) . ? C14 C15 1.491(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C20 C21 1.389(5) . ? C20 H20 0.9400 . ? C23 C24 1.385(5) . ? C23 H23 0.9400 . ? C22 C21 1.358(5) . ? C22 H22 0.9400 . ? C31 C30 1.372(5) 3_565 ? C31 C29 1.385(5) . ? C31 H31 0.9400 . ? C7 C8 1.387(5) . ? C7 C6 1.495(5) . ? C2 C3 1.402(5) . ? C2 C1 1.492(5) . ? C13 C12 1.397(5) . ? C13 H13 0.9400 . ? C25 C24 1.349(5) . ? C25 H25 0.9400 . ? C4 C3 1.355(5) . ? C4 C5 1.502(5) . ? C9 C8 1.361(5) . ? C9 C10 1.498(6) . ? C30 C31 1.372(5) 3_565 ? C30 C29 1.382(5) . ? C30 H30 0.9400 . ? C29 C28 1.486(5) . ? C8 H8 0.9400 . ? C21 H21 0.9400 . ? C17 C18 1.382(6) . ? C17 H17 0.9400 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C3 H3 0.9400 . ? C12 C11 1.503(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C19 C18 1.357(6) . ? C19 H19 0.9400 . ? C24 H24 0.9400 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C18 H18 0.9400 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? F1 B1 1.386(6) . ? F3 B1 1.386(6) . ? F4 B1 1.372(6) . ? B1 F2 1.343(6) . ? F6 B2 1.373(6) . ? F5 B2 1.354(6) . ? F8 B2 1.341(6) . ? F7 B2 1.330(6) . ? O3 C35 1.307(10) . ? O3 C34 1.428(11) . ? C34 C33 1.492(13) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? O2 C33 1.418(10) . ? O2 C32 1.433(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N6 88.62(11) . . ? N4 Fe1 N2 86.72(12) . . ? N6 Fe1 N2 87.09(12) . . ? N4 Fe1 N9 91.27(12) . . ? N6 Fe1 N9 90.59(11) . . ? N2 Fe1 N9 176.96(11) . . ? N4 Fe1 N11 179.21(13) . . ? N6 Fe1 N11 91.48(11) . . ? N2 Fe1 N11 94.07(12) . . ? N9 Fe1 N11 87.94(12) . . ? N4 Fe1 N7 91.40(11) . . ? N6 Fe1 N7 179.25(12) . . ? N2 Fe1 N7 93.66(12) . . ? N9 Fe1 N7 88.66(11) . . ? N11 Fe1 N7 88.50(11) . . ? C23 N6 N5 105.0(3) . . ? C23 N6 Fe1 135.6(2) . . ? N5 N6 Fe1 119.4(2) . . ? C27 O1 C28 111.4(2) . . ? C9 N10 N9 111.7(3) . . ? C9 N10 C16 130.5(3) . . ? N9 N10 C16 117.8(3) . . ? C12 N11 N12 104.8(3) . . ? C12 N11 Fe1 138.8(2) . . ? N12 N11 Fe1 116.38(19) . . ? C22 N3 N4 111.1(3) . . ? C22 N3 C26 131.1(3) . . ? N4 N3 C26 117.8(2) . . ? C7 N9 N10 105.2(3) . . ? C7 N9 Fe1 137.3(2) . . ? N10 N9 Fe1 117.5(2) . . ? C25 N5 N6 110.8(3) . . ? C25 N5 C26 131.2(3) . . ? N6 N5 C26 118.0(2) . . ? C17 N2 N1 105.1(3) . . ? C17 N2 Fe1 136.6(3) . . ? N1 N2 Fe1 118.2(2) . . ? C14 N12 N11 112.4(3) . . ? C14 N12 C16 128.5(3) . . ? N11 N12 C16 119.0(3) . . ? C4 N8 N7 112.1(3) . . ? C4 N8 C16 129.0(3) . . ? N7 N8 C16 118.7(3) . . ? C20 N4 N3 105.2(3) . . ? C20 N4 Fe1 135.0(2) . . ? N3 N4 Fe1 119.56(19) . . ? C2 N7 N8 105.3(3) . . ? C2 N7 Fe1 138.1(2) . . ? N8 N7 Fe1 116.5(2) . . ? C19 N1 N2 110.7(3) . . ? C19 N1 C26 130.4(3) . . ? N2 N1 C26 118.9(3) . . ? N5 C26 N1 108.5(2) . . ? N5 C26 N3 108.8(3) . . ? N1 C26 N3 108.3(2) . . ? N5 C26 C27 108.9(2) . . ? N1 C26 C27 111.3(3) . . ? N3 C26 C27 111.0(3) . . ? N8 C16 N10 110.4(3) . . ? N8 C16 N12 109.7(3) . . ? N10 C16 N12 110.2(3) . . ? N8 C16 H16 108.9 . . ? N10 C16 H16 108.9 . . ? N12 C16 H16 108.9 . . ? N12 C14 C13 105.1(3) . . ? N12 C14 C15 123.5(3) . . ? C13 C14 C15 131.3(3) . . ? O1 C27 C26 107.8(3) . . ? O1 C27 H27A 110.1 . . ? C26 C27 H27A 110.1 . . ? O1 C27 H27B 110.1 . . ? C26 C27 H27B 110.1 . . ? H27A C27 H27B 108.5 . . ? N4 C20 C21 111.0(3) . . ? N4 C20 H20 124.5 . . ? C21 C20 H20 124.5 . . ? N6 C23 C24 111.0(3) . . ? N6 C23 H23 124.5 . . ? C24 C23 H23 124.5 . . ? N3 C22 C21 107.1(3) . . ? N3 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? C30 C31 C29 119.8(3) 3_565 . ? C30 C31 H31 120.1 3_565 . ? C29 C31 H31 120.1 . . ? N9 C7 C8 109.6(3) . . ? N9 C7 C6 123.7(3) . . ? C8 C7 C6 126.7(3) . . ? N7 C2 C3 109.4(3) . . ? N7 C2 C1 123.8(3) . . ? C3 C2 C1 126.8(3) . . ? C14 C13 C12 107.5(3) . . ? C14 C13 H13 126.3 . . ? C12 C13 H13 126.3 . . ? C24 C25 N5 107.0(3) . . ? C24 C25 H25 126.5 . . ? N5 C25 H25 126.5 . . ? C3 C4 N8 105.4(3) . . ? C3 C4 C5 131.4(3) . . ? N8 C4 C5 123.1(3) . . ? N10 C9 C8 105.7(3) . . ? N10 C9 C10 123.5(3) . . ? C8 C9 C10 130.8(4) . . ? C31 C30 C29 120.9(4) 3_565 . ? C31 C30 H30 119.5 3_565 . ? C29 C30 H30 119.5 . . ? C30 C29 C31 119.3(3) . . ? C30 C29 C28 120.2(3) . . ? C31 C29 C28 120.5(3) . . ? C9 C8 C7 107.8(3) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C22 C21 C20 105.7(3) . . ? C22 C21 H21 127.2 . . ? C20 C21 H21 127.2 . . ? N2 C17 C18 110.9(3) . . ? N2 C17 H17 124.5 . . ? C18 C17 H17 124.5 . . ? O1 C28 C29 106.3(3) . . ? O1 C28 H28A 110.5 . . ? C29 C28 H28A 110.5 . . ? O1 C28 H28B 110.5 . . ? C29 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? C4 C3 C2 107.8(3) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? N11 C12 C13 110.2(3) . . ? N11 C12 C11 123.7(3) . . ? C13 C12 C11 126.1(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C19 C18 106.9(4) . . ? N1 C19 H19 126.5 . . ? C18 C19 H19 126.5 . . ? C25 C24 C23 106.2(3) . . ? C25 C24 H24 126.9 . . ? C23 C24 H24 126.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C18 C17 106.3(4) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F2 B1 F4 111.2(4) . . ? F2 B1 F1 108.0(4) . . ? F4 B1 F1 109.1(4) . . ? F2 B1 F3 111.5(4) . . ? F4 B1 F3 107.4(4) . . ? F1 B1 F3 109.7(4) . . ? F7 B2 F8 113.3(5) . . ? F7 B2 F5 104.4(5) . . ? F8 B2 F5 109.0(5) . . ? F7 B2 F6 109.5(4) . . ? F8 B2 F6 109.6(4) . . ? F5 B2 F6 110.9(5) . . ? C35 O3 C34 115.4(7) . . ? O3 C34 C33 106.6(7) . . ? O3 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? O3 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? O3 C35 H35A 109.5 . . ? O3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 O2 C32 113.0(7) . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 109.4(7) . . ? O2 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O2 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? 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 Fe1 N7 N8 C16 -0.9(4) . . . . ? Fe1 N9 N10 C16 0.5(3) . . . . ? Fe1 N11 N12 C16 -2.3(4) . . . . ? Fe1 N2 N1 C26 3.1(4) . . . . ? Fe1 N4 N3 C26 6.8(4) . . . . ? Fe1 N6 N5 C26 1.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.670 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.071 # Attachment '- 1.2DME(273K).CIF' #========================================================================== data_1.2DME(273K) _database_code_depnum_ccdc_archive 'CCDC 803924' #TrackingRef '- 1.2DME(273K).CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(p-C6H4(CH2OCH2C(pz)3]2)](BF4)4(DME)2 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(p-C6H4(CH2OCH2C(pz)3)2))(BF4)4(DME)2 _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 Fe2 N24 O2, 2(C4 H10 O2), 4(B F4)' _chemical_formula_sum 'C70 H94 B4 F16 Fe2 N24 O6' _chemical_formula_weight 1826.63 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.632(3) _cell_length_b 20.824(5) _cell_length_c 17.456(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.407(13) _cell_angle_gamma 90.00 _cell_volume 4215.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 273(1) _cell_measurement_reflns_used 3475 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 21.55 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8085 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(1) _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 X8 Apex II CCD' _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 32852 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9660 _reflns_number_gt 5154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9660 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1472 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Fe1 Fe 0.75254(5) 0.70730(3) 0.62371(3) 0.03892(19) Uani 1 1 d . . . N2 N 0.8813(3) 0.72051(17) 0.7001(2) 0.0482(9) Uani 1 1 d . . . C16 C 0.5871(4) 0.8027(2) 0.5502(2) 0.0446(10) Uani 1 1 d . . . H16 H 0.5330 0.8340 0.5259 0.054 Uiso 1 1 calc R . . N9 N 0.6244(3) 0.68902(16) 0.54661(18) 0.0424(8) Uani 1 1 d . . . N8 N 0.5782(3) 0.80458(17) 0.63189(18) 0.0468(9) Uani 1 1 d . . . N10 N 0.5569(3) 0.73967(17) 0.52056(18) 0.0439(8) Uani 1 1 d . . . C13 C 0.4817(4) 0.6566(3) 0.4639(3) 0.0578(12) Uani 1 1 d . . . H13 H 0.4343 0.6297 0.4330 0.069 Uiso 1 1 calc R . . N11 N 0.7914(3) 0.78157(16) 0.55993(19) 0.0449(8) Uani 1 1 d . . . N7 N 0.6478(3) 0.76490(17) 0.67721(18) 0.0435(8) Uani 1 1 d . . . C14 C 0.4695(4) 0.7205(2) 0.4708(2) 0.0533(12) Uani 1 1 d . . . N6 N 0.8540(3) 0.65111(16) 0.57068(18) 0.0413(8) Uani 1 1 d . . . N4 N 0.7120(3) 0.63453(16) 0.68521(18) 0.0409(8) Uani 1 1 d . . . C12 C 0.5770(4) 0.6379(2) 0.5109(2) 0.0494(11) Uani 1 1 d . . . N1 N 0.9433(3) 0.66828(16) 0.72635(19) 0.0452(8) Uani 1 1 d . . . N3 N 0.7946(3) 0.59152(15) 0.70905(18) 0.0392(8) Uani 1 1 d . . . N5 N 0.9216(3) 0.60835(16) 0.61190(18) 0.0401(8) Uani 1 1 d . . . N12 N 0.7024(3) 0.81986(16) 0.53279(19) 0.0435(8) Uani 1 1 d . . . C9 C 0.7368(4) 0.8685(2) 0.4890(2) 0.0492(11) Uani 1 1 d . . . C25 C 0.9883(4) 0.5751(2) 0.5657(2) 0.0499(11) Uani 1 1 d . . . H25 H 1.0417 0.5434 0.5807 0.060 Uiso 1 1 calc R . . C19 C 0.7480(4) 0.5412(2) 0.7442(2) 0.0522(11) Uani 1 1 d . . . H19 H 0.7874 0.5056 0.7648 0.063 Uiso 1 1 calc R . . C29 C 1.0203(4) 0.4972(2) 0.9227(2) 0.0498(11) Uani 1 1 d . . . C30 C 1.0974(4) 0.5290(2) 0.9749(3) 0.0546(11) Uani 1 1 d . . . H30 H 1.1630 0.5484 0.9584 0.065 Uiso 1 1 calc R . . C28 C 1.0418(4) 0.4956(2) 0.8405(2) 0.0562(12) Uani 1 1 d . . . H28A H 1.1238 0.4983 0.8341 0.067 Uiso 1 1 calc R . . H28B H 1.0121 0.4563 0.8168 0.067 Uiso 1 1 calc R . . C23 C 0.8788(4) 0.6434(2) 0.4986(2) 0.0527(11) Uani 1 1 d . . . H23 H 0.8447 0.6661 0.4569 0.063 Uiso 1 1 calc R . . C18 C 0.6335(4) 0.5522(2) 0.7437(3) 0.0594(12) Uani 1 1 d . . . H18 H 0.5786 0.5260 0.7638 0.071 Uiso 1 1 calc R . . O1 O 0.9823(3) 0.55069(14) 0.80657(15) 0.0517(8) Uani 1 1 d . . . F2 F 0.3748(3) 0.9185(2) 0.44712(19) 0.1012(11) Uani 1 1 d . . . C2 C 0.6166(4) 0.7745(2) 0.7482(2) 0.0548(12) Uani 1 1 d . . . C27 C 0.9947(4) 0.5537(2) 0.7274(2) 0.0472(10) Uani 1 1 d . . . H27A H 0.9753 0.5126 0.7035 0.057 Uiso 1 1 calc R . . H27B H 1.0737 0.5641 0.7180 0.057 Uiso 1 1 calc R . . C31 C 0.9246(4) 0.4688(2) 0.9489(2) 0.0506(11) Uani 1 1 d . . . H31 H 0.8732 0.4474 0.9143 0.061 Uiso 1 1 calc R . . C24 C 0.9629(4) 0.5967(2) 0.4939(3) 0.0600(13) Uani 1 1 d . . . H24 H 0.9953 0.5830 0.4496 0.072 Uiso 1 1 calc R . . C3 C 0.5288(5) 0.8198(3) 0.7465(3) 0.0659(14) Uani 1 1 d . . . H3 H 0.4927 0.8349 0.7887 0.079 Uiso 1 1 calc R . . C8 C 0.8521(4) 0.8603(2) 0.4867(3) 0.0577(12) Uani 1 1 d . . . H8 H 0.9011 0.8856 0.4597 0.069 Uiso 1 1 calc R . . C22 C 1.0285(4) 0.6860(3) 0.7797(3) 0.0622(13) Uani 1 1 d . . . H22 H 1.0815 0.6589 0.8059 0.075 Uiso 1 1 calc R . . C7 C 0.8839(4) 0.8075(2) 0.5317(3) 0.0519(11) Uani 1 1 d . . . C26 C 0.9137(3) 0.60546(19) 0.6945(2) 0.0390(9) Uani 1 1 d . . . C17 C 0.6146(4) 0.6106(2) 0.7070(2) 0.0510(11) Uani 1 1 d . . . H17 H 0.5430 0.6303 0.6988 0.061 Uiso 1 1 calc R . . F4 F 0.2513(3) 0.9048(2) 0.3443(2) 0.1190(15) Uani 1 1 d . . . C1 C 0.6700(5) 0.7409(3) 0.8174(3) 0.0735(15) Uani 1 1 d . . . H1A H 0.7454 0.7259 0.8074 0.110 Uiso 1 1 calc R . . H1B H 0.6228 0.7050 0.8295 0.110 Uiso 1 1 calc R . . H1C H 0.6761 0.7701 0.8601 0.110 Uiso 1 1 calc R . . F3 F 0.3637(5) 0.9901(3) 0.3560(3) 0.165(2) Uani 1 1 d . . . C4 C 0.5050(4) 0.8382(2) 0.6725(3) 0.0590(13) Uani 1 1 d . . . F1 F 0.4364(3) 0.8931(2) 0.3320(2) 0.1161(14) Uani 1 1 d . . . C15 C 0.3823(5) 0.7656(3) 0.4345(3) 0.0800(17) Uani 1 1 d . . . H15A H 0.4206 0.7986 0.4076 0.120 Uiso 1 1 calc R . . H15B H 0.3397 0.7848 0.4735 0.120 Uiso 1 1 calc R . . H15C H 0.3305 0.7426 0.3990 0.120 Uiso 1 1 calc R . . C6 C 1.0044(4) 0.7824(3) 0.5479(4) 0.0770(16) Uani 1 1 d . . . H6A H 1.0027 0.7445 0.5792 0.115 Uiso 1 1 calc R . . H6B H 1.0511 0.8145 0.5746 0.115 Uiso 1 1 calc R . . H6C H 1.0364 0.7720 0.5003 0.115 Uiso 1 1 calc R . . C5 C 0.4193(5) 0.8853(3) 0.6373(3) 0.0824(18) Uani 1 1 d . . . H5A H 0.3725 0.8647 0.5968 0.124 Uiso 1 1 calc R . . H5B H 0.4594 0.9209 0.6168 0.124 Uiso 1 1 calc R . . H5C H 0.3712 0.9004 0.6758 0.124 Uiso 1 1 calc R . . C11 C 0.6237(5) 0.5714(2) 0.5216(3) 0.0664(14) Uani 1 1 d . . . H11A H 0.6627 0.5676 0.5719 0.100 Uiso 1 1 calc R . . H11B H 0.6771 0.5629 0.4836 0.100 Uiso 1 1 calc R . . H11C H 0.5615 0.5411 0.5163 0.100 Uiso 1 1 calc R . . C20 C 0.9299(5) 0.7698(2) 0.7372(3) 0.0662(14) Uani 1 1 d . . . H20 H 0.9059 0.8122 0.7307 0.079 Uiso 1 1 calc R . . C10 C 0.6578(4) 0.9191(3) 0.4560(3) 0.0694(15) Uani 1 1 d . . . H10A H 0.6258 0.9424 0.4968 0.104 Uiso 1 1 calc R . . H10B H 0.5966 0.8995 0.4241 0.104 Uiso 1 1 calc R . . H10C H 0.6998 0.9480 0.4258 0.104 Uiso 1 1 calc R . . C21 C 1.0215(5) 0.7503(3) 0.7873(3) 0.0752(16) Uani 1 1 d . . . H21 H 1.0687 0.7763 0.8197 0.090 Uiso 1 1 calc R . . B1 B 0.3567(6) 0.9276(4) 0.3698(4) 0.0754(19) Uani 1 1 d . . . F6 F 0.8067(5) 0.4529(2) 0.6099(3) 0.154(2) Uani 1 1 d . . . F7 F 0.7083(5) 0.3957(3) 0.6834(3) 0.194(3) Uani 1 1 d . . . B2 B 0.8081(8) 0.3987(4) 0.6505(4) 0.083(2) Uani 1 1 d . . . O3 O 0.2305(6) 0.6357(6) 0.6414(5) 0.214(4) Uani 1 1 d . . . C34 C 0.2946(14) 0.5927(11) 0.5997(7) 0.253(11) Uani 1 1 d . . . H34A H 0.3670 0.6121 0.5881 0.303 Uiso 1 1 calc R . . H34B H 0.2519 0.5811 0.5519 0.303 Uiso 1 1 calc R . . C35 C 0.2835(15) 0.6961(7) 0.6596(14) 0.325(13) Uani 1 1 d . . . H35A H 0.3532 0.6998 0.6339 0.487 Uiso 1 1 calc R . . H35B H 0.3014 0.6990 0.7141 0.487 Uiso 1 1 calc R . . H35C H 0.2317 0.7301 0.6432 0.487 Uiso 1 1 calc R . . F5 F 0.8139(3) 0.34615(18) 0.6057(2) 0.1132(13) Uani 1 1 d . . . O2 O 0.2180(4) 0.4932(4) 0.6459(3) 0.131(2) Uani 1 1 d . . . F8 F 0.8945(6) 0.4033(2) 0.6987(4) 0.229(4) Uani 1 1 d . . . C32 C 0.2345(9) 0.4326(5) 0.6872(5) 0.165(5) Uani 1 1 d . . . H32A H 0.2530 0.4411 0.7408 0.247 Uiso 1 1 calc R . . H32B H 0.2963 0.4090 0.6670 0.247 Uiso 1 1 calc R . . H32C H 0.1648 0.4077 0.6811 0.247 Uiso 1 1 calc R . . C33 C 0.3169(9) 0.5328(9) 0.6508(7) 0.218(9) Uani 1 1 d . . . H33A H 0.3822 0.5092 0.6339 0.262 Uiso 1 1 calc R . . H33B H 0.3350 0.5459 0.7036 0.262 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 Fe1 0.0412(3) 0.0374(3) 0.0383(3) -0.0002(2) 0.0038(2) 0.0011(3) N2 0.056(2) 0.039(2) 0.049(2) -0.0011(16) -0.0018(17) 0.0022(17) C16 0.045(2) 0.048(3) 0.042(2) 0.0062(18) 0.0060(18) 0.007(2) N9 0.0441(19) 0.042(2) 0.0411(19) -0.0026(15) 0.0057(15) 0.0013(16) N8 0.052(2) 0.051(2) 0.0384(19) -0.0002(16) 0.0057(16) 0.0103(17) N10 0.0414(19) 0.049(2) 0.0407(19) 0.0010(16) -0.0003(15) -0.0013(17) C13 0.056(3) 0.068(3) 0.049(3) -0.004(2) -0.002(2) -0.022(2) N11 0.0406(19) 0.042(2) 0.052(2) 0.0043(16) 0.0034(16) 0.0021(16) N7 0.048(2) 0.045(2) 0.0371(18) -0.0011(15) 0.0011(15) 0.0046(17) C14 0.048(3) 0.066(3) 0.045(3) 0.004(2) 0.000(2) -0.011(2) N6 0.045(2) 0.0395(19) 0.0391(19) 0.0049(15) 0.0035(15) 0.0006(16) N4 0.0405(19) 0.044(2) 0.0387(18) -0.0011(15) 0.0047(14) 0.0020(16) C12 0.051(3) 0.053(3) 0.044(2) -0.002(2) 0.006(2) -0.010(2) N1 0.047(2) 0.041(2) 0.046(2) -0.0007(16) -0.0076(16) 0.0018(16) N3 0.0397(19) 0.0372(19) 0.0409(18) 0.0047(14) 0.0051(14) -0.0003(15) N5 0.0390(18) 0.042(2) 0.0399(18) -0.0028(15) 0.0070(14) 0.0028(15) N12 0.043(2) 0.0395(19) 0.048(2) 0.0028(16) 0.0027(15) -0.0018(16) C9 0.057(3) 0.040(3) 0.049(2) 0.0050(19) -0.007(2) -0.011(2) C25 0.046(2) 0.052(3) 0.054(3) -0.006(2) 0.014(2) 0.009(2) C19 0.058(3) 0.046(3) 0.053(3) 0.011(2) 0.009(2) -0.002(2) C29 0.057(3) 0.042(2) 0.049(3) 0.006(2) -0.001(2) 0.015(2) C30 0.047(3) 0.053(3) 0.062(3) 0.007(2) 0.000(2) 0.003(2) C28 0.064(3) 0.051(3) 0.053(3) 0.005(2) -0.001(2) 0.014(2) C23 0.058(3) 0.065(3) 0.036(2) 0.006(2) 0.009(2) -0.002(2) C18 0.055(3) 0.062(3) 0.063(3) 0.013(2) 0.014(2) -0.007(2) O1 0.0627(19) 0.0516(18) 0.0402(16) 0.0061(13) 0.0003(13) 0.0153(15) F2 0.106(3) 0.124(3) 0.075(2) 0.010(2) 0.0138(19) 0.012(2) C2 0.065(3) 0.059(3) 0.040(2) -0.004(2) 0.005(2) 0.009(2) C27 0.050(3) 0.050(3) 0.042(2) 0.0039(19) 0.0089(19) 0.006(2) C31 0.051(3) 0.051(3) 0.048(3) 0.003(2) -0.010(2) 0.001(2) C24 0.069(3) 0.067(3) 0.046(3) -0.003(2) 0.018(2) 0.008(3) C3 0.083(4) 0.070(3) 0.046(3) -0.010(2) 0.013(2) 0.022(3) C8 0.053(3) 0.051(3) 0.070(3) 0.007(2) 0.008(2) -0.017(2) C22 0.055(3) 0.061(3) 0.067(3) -0.001(2) -0.021(2) -0.003(2) C7 0.046(3) 0.047(3) 0.063(3) 0.005(2) 0.002(2) -0.006(2) C26 0.040(2) 0.038(2) 0.040(2) -0.0037(17) 0.0052(17) -0.0033(18) C17 0.041(2) 0.063(3) 0.050(3) 0.004(2) 0.0093(19) -0.001(2) F4 0.056(2) 0.169(4) 0.132(3) -0.041(3) 0.001(2) 0.003(2) C1 0.091(4) 0.086(4) 0.042(3) -0.003(3) -0.004(3) 0.018(3) F3 0.221(6) 0.124(4) 0.142(4) 0.043(3) -0.040(4) -0.056(4) C4 0.064(3) 0.062(3) 0.052(3) -0.007(2) 0.012(2) 0.014(2) F1 0.071(2) 0.193(4) 0.087(2) 0.010(3) 0.0228(19) 0.007(3) C15 0.066(3) 0.086(4) 0.084(4) 0.010(3) -0.023(3) -0.004(3) C6 0.049(3) 0.072(4) 0.110(4) 0.018(3) 0.006(3) -0.009(3) C5 0.088(4) 0.086(4) 0.075(4) 0.002(3) 0.014(3) 0.048(3) C11 0.079(4) 0.052(3) 0.070(3) -0.012(2) 0.010(3) -0.012(3) C20 0.075(3) 0.039(3) 0.083(4) -0.014(3) -0.003(3) -0.005(3) C10 0.062(3) 0.062(3) 0.082(4) 0.028(3) -0.006(3) -0.009(3) C21 0.074(4) 0.057(4) 0.089(4) -0.010(3) -0.030(3) -0.009(3) B1 0.051(4) 0.099(6) 0.077(5) 0.016(4) 0.012(3) 0.006(4) F6 0.239(6) 0.084(3) 0.148(4) 0.020(3) 0.076(4) 0.032(3) F7 0.190(5) 0.216(6) 0.192(5) -0.081(4) 0.116(5) -0.104(5) B2 0.107(6) 0.057(4) 0.083(5) -0.008(4) 0.001(4) 0.010(4) O3 0.127(6) 0.349(14) 0.171(7) -0.077(8) 0.044(5) -0.067(7) C34 0.169(13) 0.47(3) 0.132(10) -0.058(14) 0.090(10) -0.139(16) C35 0.228(16) 0.157(14) 0.59(4) 0.083(19) 0.02(2) -0.059(12) F5 0.109(3) 0.079(3) 0.146(3) -0.024(2) -0.030(2) 0.005(2) O2 0.078(3) 0.202(7) 0.112(4) -0.042(4) -0.002(3) 0.030(4) F8 0.258(7) 0.088(3) 0.305(8) -0.041(4) -0.204(7) 0.004(4) C32 0.200(11) 0.173(10) 0.116(7) -0.012(7) -0.020(7) 0.103(9) C33 0.075(6) 0.44(3) 0.146(10) -0.144(13) 0.032(7) -0.021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.936(3) . ? Fe1 N6 1.946(3) . ? Fe1 N2 1.946(4) . ? Fe1 N9 1.968(3) . ? Fe1 N11 1.978(3) . ? Fe1 N7 1.993(3) . ? N2 C20 1.318(6) . ? N2 N1 1.365(5) . ? C16 N8 1.438(5) . ? C16 N12 1.443(5) . ? C16 N10 1.445(5) . ? C16 H16 0.9800 . ? N9 C12 1.331(5) . ? N9 N10 1.371(5) . ? N8 C4 1.345(5) . ? N8 N7 1.366(5) . ? N10 C14 1.346(5) . ? C13 C14 1.344(7) . ? C13 C12 1.383(6) . ? C13 H13 0.9300 . ? N11 C7 1.331(5) . ? N11 N12 1.363(5) . ? N7 C2 1.332(5) . ? C14 C15 1.488(7) . ? N6 C23 1.322(5) . ? N6 N5 1.357(4) . ? N4 C17 1.320(5) . ? N4 N3 1.355(4) . ? C12 C11 1.495(7) . ? N1 C22 1.358(5) . ? N1 C26 1.453(5) . ? N3 C19 1.348(5) . ? N3 C26 1.457(5) . ? N5 C25 1.353(5) . ? N5 C26 1.452(5) . ? N12 C9 1.348(5) . ? C9 C8 1.356(6) . ? C9 C10 1.484(6) . ? C25 C24 1.342(6) . ? C25 H25 0.9300 . ? C19 C18 1.351(6) . ? C19 H19 0.9300 . ? C29 C31 1.371(6) . ? C29 C30 1.395(6) . ? C29 C28 1.476(6) . ? C30 C31 1.373(6) 3_767 ? C30 H30 0.9300 . ? C28 O1 1.442(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C23 C24 1.386(6) . ? C23 H23 0.9300 . ? C18 C17 1.383(6) . ? C18 H18 0.9300 . ? O1 C27 1.402(5) . ? F2 B1 1.363(7) . ? C2 C3 1.390(7) . ? C2 C1 1.490(6) . ? C27 C26 1.516(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C31 C30 1.373(6) 3_767 ? C31 H31 0.9300 . ? C24 H24 0.9300 . ? C3 C4 1.354(6) . ? C3 H3 0.9300 . ? C8 C7 1.386(6) . ? C8 H8 0.9300 . ? C22 C21 1.349(7) . ? C22 H22 0.9300 . ? C7 C6 1.502(7) . ? C17 H17 0.9300 . ? F4 B1 1.357(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? F3 B1 1.328(9) . ? C4 C5 1.496(7) . ? F1 B1 1.380(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C20 C21 1.387(7) . ? C20 H20 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C21 H21 0.9300 . ? F6 B2 1.332(8) . ? F7 B2 1.335(9) . ? B2 F8 1.264(9) . ? B2 F5 1.350(8) . ? O3 C34 1.403(19) . ? O3 C35 1.426(15) . ? C34 C33 1.54(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? O2 C33 1.413(14) . ? O2 C32 1.460(11) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N6 88.60(14) . . ? N4 Fe1 N2 86.46(14) . . ? N6 Fe1 N2 87.02(14) . . ? N4 Fe1 N9 91.36(14) . . ? N6 Fe1 N9 90.78(14) . . ? N2 Fe1 N9 176.94(15) . . ? N4 Fe1 N11 179.05(14) . . ? N6 Fe1 N11 91.67(14) . . ? N2 Fe1 N11 94.46(15) . . ? N9 Fe1 N11 87.73(14) . . ? N4 Fe1 N7 91.58(14) . . ? N6 Fe1 N7 179.51(14) . . ? N2 Fe1 N7 93.45(14) . . ? N9 Fe1 N7 88.76(14) . . ? N11 Fe1 N7 88.15(14) . . ? C20 N2 N1 105.0(4) . . ? C20 N2 Fe1 136.5(3) . . ? N1 N2 Fe1 118.5(3) . . ? N8 C16 N12 110.0(3) . . ? N8 C16 N10 110.2(3) . . ? N12 C16 N10 110.7(3) . . ? N8 C16 H16 108.6 . . ? N12 C16 H16 108.6 . . ? N10 C16 H16 108.6 . . ? C12 N9 N10 104.7(3) . . ? C12 N9 Fe1 137.7(3) . . ? N10 N9 Fe1 117.5(3) . . ? C4 N8 N7 112.3(3) . . ? C4 N8 C16 129.3(4) . . ? N7 N8 C16 118.3(3) . . ? C14 N10 N9 111.7(4) . . ? C14 N10 C16 130.6(4) . . ? N9 N10 C16 117.6(3) . . ? C14 C13 C12 108.1(4) . . ? C14 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? C7 N11 N12 104.4(3) . . ? C7 N11 Fe1 138.7(3) . . ? N12 N11 Fe1 116.9(2) . . ? C2 N7 N8 104.9(3) . . ? C2 N7 Fe1 138.2(3) . . ? N8 N7 Fe1 116.7(2) . . ? C13 C14 N10 105.7(4) . . ? C13 C14 C15 131.3(5) . . ? N10 C14 C15 122.9(5) . . ? C23 N6 N5 105.3(3) . . ? C23 N6 Fe1 135.3(3) . . ? N5 N6 Fe1 119.3(2) . . ? C17 N4 N3 105.4(3) . . ? C17 N4 Fe1 134.9(3) . . ? N3 N4 Fe1 119.4(2) . . ? N9 C12 C13 109.7(4) . . ? N9 C12 C11 123.2(4) . . ? C13 C12 C11 127.1(4) . . ? C22 N1 N2 110.7(4) . . ? C22 N1 C26 130.3(4) . . ? N2 N1 C26 119.0(3) . . ? C19 N3 N4 110.7(3) . . ? C19 N3 C26 130.9(4) . . ? N4 N3 C26 118.4(3) . . ? C25 N5 N6 110.8(3) . . ? C25 N5 C26 130.8(4) . . ? N6 N5 C26 118.4(3) . . ? C9 N12 N11 112.7(3) . . ? C9 N12 C16 128.8(4) . . ? N11 N12 C16 118.4(3) . . ? N12 C9 C8 105.0(4) . . ? N12 C9 C10 123.5(4) . . ? C8 C9 C10 131.5(4) . . ? C24 C25 N5 106.9(4) . . ? C24 C25 H25 126.5 . . ? N5 C25 H25 126.5 . . ? N3 C19 C18 107.2(4) . . ? N3 C19 H19 126.4 . . ? C18 C19 H19 126.4 . . ? C31 C29 C30 118.9(4) . . ? C31 C29 C28 121.2(4) . . ? C30 C29 C28 119.9(4) . . ? C31 C30 C29 119.4(4) 3_767 . ? C31 C30 H30 120.3 3_767 . ? C29 C30 H30 120.3 . . ? O1 C28 C29 105.6(3) . . ? O1 C28 H28A 110.6 . . ? C29 C28 H28A 110.6 . . ? O1 C28 H28B 110.6 . . ? C29 C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? N6 C23 C24 110.4(4) . . ? N6 C23 H23 124.8 . . ? C24 C23 H23 124.8 . . ? C19 C18 C17 105.9(4) . . ? C19 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? C27 O1 C28 110.9(3) . . ? N7 C2 C3 109.5(4) . . ? N7 C2 C1 123.9(4) . . ? C3 C2 C1 126.6(4) . . ? O1 C27 C26 107.3(3) . . ? O1 C27 H27A 110.3 . . ? C26 C27 H27A 110.3 . . ? O1 C27 H27B 110.3 . . ? C26 C27 H27B 110.3 . . ? H27A C27 H27B 108.5 . . ? C29 C31 C30 121.7(4) . 3_767 ? C29 C31 H31 119.2 . . ? C30 C31 H31 119.2 3_767 . ? C25 C24 C23 106.5(4) . . ? C25 C24 H24 126.7 . . ? C23 C24 H24 126.7 . . ? C4 C3 C2 107.9(4) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C9 C8 C7 107.8(4) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C21 C22 N1 107.0(4) . . ? C21 C22 H22 126.5 . . ? N1 C22 H22 126.5 . . ? N11 C7 C8 110.1(4) . . ? N11 C7 C6 123.9(4) . . ? C8 C7 C6 126.0(4) . . ? N5 C26 N1 108.2(3) . . ? N5 C26 N3 108.4(3) . . ? N1 C26 N3 108.2(3) . . ? N5 C26 C27 108.7(3) . . ? N1 C26 C27 111.9(3) . . ? N3 C26 C27 111.3(3) . . ? N4 C17 C18 110.9(4) . . ? N4 C17 H17 124.6 . . ? C18 C17 H17 124.6 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N8 C4 C3 105.4(4) . . ? N8 C4 C5 123.6(4) . . ? C3 C4 C5 131.1(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C20 C21 111.3(5) . . ? N2 C20 H20 124.4 . . ? C21 C20 H20 124.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C22 C21 C20 106.1(4) . . ? C22 C21 H21 127.0 . . ? C20 C21 H21 127.0 . . ? F3 B1 F4 110.5(6) . . ? F3 B1 F2 108.1(7) . . ? F4 B1 F2 110.1(5) . . ? F3 B1 F1 111.7(6) . . ? F4 B1 F1 106.5(6) . . ? F2 B1 F1 110.0(5) . . ? F8 B2 F6 105.5(7) . . ? F8 B2 F7 113.0(8) . . ? F6 B2 F7 107.0(7) . . ? F8 B2 F5 112.0(7) . . ? F6 B2 F5 112.2(6) . . ? F7 B2 F5 107.1(7) . . ? C34 O3 C35 116.1(11) . . ? O3 C34 C33 106.8(9) . . ? O3 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? O3 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? O3 C35 H35A 109.5 . . ? O3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 O2 C32 113.6(9) . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 109.7(11) . . ? O2 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? O2 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? 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 Fe1 N7 N8 C16 -1.1(5) . . . . ? Fe1 N9 N10 C16 1.6(4) . . . . ? Fe1 N11 N12 C16 -1.8(4) . . . . ? Fe1 N2 N1 C26 2.2(5) . . . . ? Fe1 N4 N3 C26 6.5(4) . . . . ? Fe1 N6 N5 C26 1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.708 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.070 data_1.6MeCN(173K) _database_code_depnum_ccdc_archive 'CCDC 803925' #TrackingRef '- 1.6MeCN(173K)revised Mar16 [1].CIF' #========================================================================== _audit_creation_method SHELXL-97 _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(p-C6H4(CH2OCH2C(pz)3]2)](BF4)4(MeCN)6 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(p-C6H4(CH2OCH2C(pz)3)2))(BF4)4(MeCN)6 _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 Fe2 N24 O2, 4(B F4), 6(C2 H3 N)' _chemical_formula_sum 'C74 H92 B4 F16 Fe2 N30 O2' _chemical_formula_weight 1892.72 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' Fe Fe 0.3463 0.8444 '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' B B 0.0013 0.0007 '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' H H 0.0000 0.0000 '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 13.451(3) _cell_length_b 14.795(3) _cell_length_c 15.885(3) _cell_angle_alpha 116.03(3) _cell_angle_beta 104.63(3) _cell_angle_gamma 94.23(3) _cell_volume 2685.8(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11833 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.9659 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _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 26431 _diffrn_reflns_av_R_equivalents 0.1175 _diffrn_reflns_av_sigmaI/netI 0.2263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11833 _reflns_number_gt 4531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. One BF4- anion was disordered over two positions (with one F atom common); these positions were given 50:50 occupancy. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11833 _refine_ls_number_parameters 559 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.3150 _refine_ls_R_factor_gt 0.1583 _refine_ls_wR_factor_ref 0.4585 _refine_ls_wR_factor_gt 0.3848 _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_restrained_S_all 1.285 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28162(9) 0.62365(9) 0.29431(9) 0.0357(5) Uani 1 1 d . . . F1 F 0.6690(6) 0.7908(6) 0.1496(6) 0.108(3) Uani 1 1 d . . . O1 O 0.2105(5) 0.2265(5) 0.1423(5) 0.0543(17) Uiso 1 1 d . . . N1 N 0.2142(6) 0.4263(5) 0.2794(5) 0.0382(18) Uani 1 1 d . . . C1 C 0.5142(9) 0.6440(9) 0.2208(9) 0.073(3) Uani 1 1 d . . . H1A H 0.5597 0.6459 0.2806 0.109 Uiso 1 1 calc R . . H1B H 0.5573 0.6531 0.1826 0.109 Uiso 1 1 calc R . . H1C H 0.4644 0.5775 0.1807 0.109 Uiso 1 1 calc R . . B1 B 0.7045(14) 0.8767(13) 0.1417(11) 0.083(5) Uani 1 1 d . . . F2 F 0.8066(8) 0.8850(10) 0.1546(8) 0.185(5) Uani 1 1 d . . . N2 N 0.1934(6) 0.5242(5) 0.3085(5) 0.0417(19) Uani 1 1 d . . . C2 C 0.4553(7) 0.7282(8) 0.2487(8) 0.053(3) Uani 1 1 d . . . B2 B 0.7501(8) 0.7994(8) 0.5814(7) 0.069(4) Uiso 1 1 d D . . F3 F 0.6568(8) 0.8597(6) 0.0474(5) 0.120(3) Uani 1 1 d . . . N3 N 0.2775(5) 0.4174(5) 0.1519(6) 0.0416(19) Uani 1 1 d . . . C3 C 0.4814(8) 0.8260(8) 0.2526(8) 0.063(3) Uani 1 1 d . . . H3 H 0.5360 0.8485 0.2338 0.075 Uiso 1 1 calc R . . F4 F 0.6767(9) 0.9572(6) 0.2079(6) 0.150(4) Uani 1 1 d . . . N4 N 0.2699(5) 0.5167(5) 0.1658(5) 0.0346(17) Uani 1 1 d . . . C4 C 0.4102(9) 0.8802(8) 0.2896(7) 0.057(3) Uiso 1 1 d . . . F5 F 0.6758(7) 0.7671(6) 0.6105(6) 0.126(3) Uiso 1 1 d D . . N5 N 0.3963(6) 0.4717(6) 0.3094(6) 0.048(2) Uani 1 1 d . . . C5 C 0.3996(10) 0.9883(9) 0.3080(11) 0.094(4) Uani 1 1 d . . . H5A H 0.4042 1.0306 0.3772 0.142 Uiso 1 1 calc R . . H5B H 0.3315 0.9853 0.2649 0.142 Uiso 1 1 calc R . . H5C H 0.4563 1.0187 0.2938 0.142 Uiso 1 1 calc R . . F6A F 0.6866(10) 0.8010(11) 0.4935(9) 0.098(4) Uiso 0.50 1 d PD . . N6 N 0.4012(5) 0.5756(5) 0.3462(5) 0.0384(18) Uani 1 1 d . . . C6 C 0.3328(10) 0.6687(8) 0.5459(8) 0.076(4) Uani 1 1 d . . . H6A H 0.3340 0.6068 0.4877 0.114 Uiso 1 1 calc R . . H6B H 0.2773 0.6529 0.5702 0.114 Uiso 1 1 calc R . . H6C H 0.4010 0.6920 0.5978 0.114 Uiso 1 1 calc R . . N7 N 0.1565(5) 0.6671(5) 0.2394(5) 0.0378(18) Uani 1 1 d . . . C7 C 0.3120(7) 0.7512(7) 0.5188(7) 0.047(2) Uani 1 1 d . . . N8 N 0.1651(5) 0.7715(5) 0.2710(5) 0.0346(17) Uani 1 1 d . . . C8 C 0.3113(8) 0.8558(7) 0.5822(7) 0.056(3) Uani 1 1 d . . . H8 H 0.3247 0.8871 0.6517 0.067 Uiso 1 1 calc R . . F7B F 0.7730(12) 0.7162(10) 0.5136(10) 0.105(6) Uiso 0.50 1 d PD . . N9 N 0.3733(5) 0.7236(5) 0.2791(5) 0.0366(17) Uani 1 1 d . . . C9 C 0.2889(7) 0.9004(7) 0.5265(7) 0.047(2) Uani 1 1 d . . . N10 N 0.3477(6) 0.8187(5) 0.3060(5) 0.0419(19) Uani 1 1 d . . . C10 C 0.2714(11) 1.0070(8) 0.5489(8) 0.087(4) Uani 1 1 d . . . H10A H 0.3025 1.0535 0.6200 0.131 Uiso 1 1 calc R . . H10B H 0.1958 1.0049 0.5287 0.131 Uiso 1 1 calc R . . H10C H 0.3046 1.0319 0.5126 0.131 Uiso 1 1 calc R . . N11 N 0.2935(5) 0.7356(5) 0.4264(5) 0.0354(17) Uani 1 1 d . . . C11 C 0.0164(8) 0.5099(7) 0.1252(8) 0.059(3) Uani 1 1 d . . . H11A H 0.0187 0.4787 0.0572 0.089 Uiso 1 1 calc R . . H11B H -0.0565 0.4978 0.1243 0.089 Uiso 1 1 calc R . . H11C H 0.0584 0.4789 0.1612 0.089 Uiso 1 1 calc R . . N12 N 0.2801(5) 0.8302(5) 0.4331(5) 0.0371(18) Uani 1 1 d . . . C12 C 0.0600(7) 0.6222(7) 0.1749(7) 0.047(2) Uani 1 1 d . . . N13 N 0.2227(11) 0.7414(11) 0.0655(10) 0.129(5) Uani 1 1 d . . . C13 C 0.0090(7) 0.7002(8) 0.1649(7) 0.052(3) Uani 1 1 d . . . H13 H -0.0595 0.6894 0.1222 0.062 Uiso 1 1 calc R . . N14 N 0.212(2) 0.4891(18) 0.8195(18) 0.111(7) Uiso 0.50 1 d P . . C14 C 0.0751(7) 0.7907(7) 0.2267(7) 0.047(2) Uani 1 1 d . . . N15 N 0.4354(18) 0.6542(17) 0.9768(17) 0.098(7) Uiso 0.50 1 d P . . C15 C 0.0624(9) 0.8996(8) 0.2490(8) 0.071(3) Uani 1 1 d . . . H15A H 0.1089 0.9277 0.2238 0.106 Uiso 1 1 calc R . . H15B H 0.0807 0.9431 0.3206 0.106 Uiso 1 1 calc R . . H15C H -0.0107 0.8981 0.2169 0.106 Uiso 1 1 calc R . . N16 N 0.8470(14) 0.7785(13) 0.3416(12) 0.064(5) Uiso 0.50 1 d P . . C16 C 0.2595(6) 0.8398(6) 0.3434(6) 0.037(2) Uani 1 1 d . . . H16 H 0.2528 0.9120 0.3596 0.045 Uiso 1 1 calc R . . N17 N 1.041(2) 0.669(2) 0.5268(19) 0.115(8) Uiso 0.50 1 d P . . C17 C 0.1229(8) 0.5294(8) 0.3516(8) 0.063(3) Uani 1 1 d . . . H17 H 0.0954 0.5890 0.3803 0.076 Uiso 1 1 calc R . . C18 C 0.0916(10) 0.4353(8) 0.3511(9) 0.079(4) Uani 1 1 d . . . H18 H 0.0392 0.4195 0.3758 0.094 Uiso 1 1 calc R . . C19 C 0.1528(8) 0.3722(7) 0.3074(8) 0.055(3) Uani 1 1 d . . . H19 H 0.1532 0.3043 0.2980 0.066 Uiso 1 1 calc R . . C20 C 0.2623(7) 0.5101(7) 0.0779(8) 0.048(2) Uani 1 1 d . . . H20 H 0.2560 0.5661 0.0641 0.058 Uiso 1 1 calc R . . C21 C 0.2645(7) 0.4125(7) 0.0087(7) 0.044(2) Uani 1 1 d . . . H21 H 0.2594 0.3906 -0.0584 0.052 Uiso 1 1 calc R . . C22 C 0.2756(7) 0.3533(7) 0.0567(7) 0.045(2) Uani 1 1 d . . . H22 H 0.2807 0.2831 0.0296 0.054 Uiso 1 1 calc R . . C23 C 0.4950(8) 0.6173(8) 0.4097(8) 0.058(3) Uani 1 1 d . . . H23 H 0.5232 0.6893 0.4456 0.069 Uiso 1 1 calc R . . C24 C 0.5497(8) 0.5436(9) 0.4189(9) 0.064(3) Uani 1 1 d . . . H24 H 0.6181 0.5561 0.4625 0.076 Uiso 1 1 calc R . . C25 C 0.4870(8) 0.4530(8) 0.3548(8) 0.058(3) Uani 1 1 d . . . H25 H 0.5021 0.3875 0.3427 0.070 Uiso 1 1 calc R . . C26 C 0.2977(7) 0.4003(7) 0.2360(7) 0.040(2) Uani 1 1 d . . . C27 C 0.3053(8) 0.2897(7) 0.2093(8) 0.054(3) Uani 1 1 d . . . H27A H 0.3625 0.2718 0.1801 0.065 Uiso 1 1 calc R . . H27B H 0.3211 0.2809 0.2693 0.065 Uiso 1 1 calc R . . C28 C 0.2168(9) 0.1179(7) 0.1085(8) 0.064(3) Uani 1 1 d . . . H28A H 0.2471 0.1060 0.1655 0.077 Uiso 1 1 calc R . . H28B H 0.2609 0.0974 0.0646 0.077 Uiso 1 1 calc R . . C29 C 0.1029(9) 0.0570(7) 0.0522(9) 0.054(3) Uani 1 1 d . . . C30 C 0.0652(10) 0.0157(8) -0.0476(9) 0.062(3) Uani 1 1 d . . . H30 H 0.1102 0.0252 -0.0818 0.074 Uiso 1 1 calc R . . C31 C 0.0376(11) 0.0403(7) 0.1014(8) 0.066(3) Uani 1 1 d . . . H31 H 0.0628 0.0667 0.1710 0.079 Uiso 1 1 calc R . . C32 C 0.0652(13) 0.7615(10) -0.0483(12) 0.126(6) Uani 1 1 d . . . H32A H 0.0810 0.7529 -0.1080 0.189 Uiso 1 1 calc R . . H32B H 0.0498 0.8298 -0.0150 0.189 Uiso 1 1 calc R . . H32C H 0.0041 0.7085 -0.0664 0.189 Uiso 1 1 calc R . . C33 C 0.1547(12) 0.7517(10) 0.0173(10) 0.081(4) Uani 1 1 d . . . C34 C 0.1943(18) 0.4945(17) 0.6524(15) 0.071(6) Uiso 0.50 1 d P . . H34A H 0.1241 0.4553 0.6062 0.106 Uiso 0.50 1 calc PR . . H34B H 0.2477 0.4648 0.6233 0.106 Uiso 0.50 1 calc PR . . H34C H 0.2014 0.5663 0.6656 0.106 Uiso 0.50 1 calc PR . . C35 C 0.2081(18) 0.4904(17) 0.7425(17) 0.068(6) Uiso 0.50 1 d P . . C36 C 0.448(3) 0.663(2) 0.829(2) 0.118(10) Uiso 0.50 1 d P . . H36A H 0.4631 0.7353 0.8439 0.177 Uiso 0.50 1 calc PR . . H36B H 0.3844 0.6259 0.7717 0.177 Uiso 0.50 1 calc PR . . H36C H 0.5076 0.6320 0.8130 0.177 Uiso 0.50 1 calc PR . . C37 C 0.434(2) 0.6569(19) 0.909(2) 0.081(7) Uiso 0.50 1 d P . . C38 C 1.0231(18) 0.7517(18) 0.4109(16) 0.073(6) Uiso 0.50 1 d P . . H38A H 1.0119 0.7056 0.4384 0.109 Uiso 0.50 1 calc PR . . H38B H 1.0755 0.8140 0.4616 0.109 Uiso 0.50 1 calc PR . . H38C H 1.0483 0.7168 0.3544 0.109 Uiso 0.50 1 calc PR . . C39 C 0.935(2) 0.7768(18) 0.3821(17) 0.074(7) Uiso 0.50 1 d P . . C40 C 1.0658(14) 0.8653(13) 0.6566(12) 0.042(4) Uiso 0.50 1 d P . . H40A H 1.0968 0.9035 0.6290 0.063 Uiso 0.50 1 calc PR . . H40B H 1.1070 0.8920 0.7263 0.063 Uiso 0.50 1 calc PR . . H40C H 0.9933 0.8735 0.6515 0.063 Uiso 0.50 1 calc PR . . C41 C 1.0667(17) 0.7540(17) 0.6006(16) 0.065(6) Uiso 0.50 1 d P . . F8A F 0.8031(12) 0.8983(9) 0.6389(11) 0.127(6) Uiso 0.50 1 d PD . . F8B F 0.8332(9) 0.8405(10) 0.6718(9) 0.096(4) Uiso 0.50 1 d PD . . F6B F 0.7244(15) 0.8719(12) 0.5587(14) 0.157(7) Uiso 0.50 1 d PD . . F7A F 0.8109(12) 0.7304(12) 0.5530(13) 0.136(8) Uiso 0.50 1 d PD . . 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 0.0266(7) 0.0341(8) 0.0499(9) 0.0230(7) 0.0120(6) 0.0075(5) F1 0.124(7) 0.102(6) 0.130(6) 0.065(5) 0.069(5) 0.028(5) N1 0.045(5) 0.025(4) 0.051(5) 0.017(4) 0.025(4) 0.018(3) C1 0.054(7) 0.078(8) 0.101(9) 0.047(7) 0.040(7) 0.023(6) B1 0.090(13) 0.086(12) 0.057(10) 0.018(9) 0.034(9) -0.002(10) F2 0.083(7) 0.267(14) 0.181(10) 0.094(10) 0.049(7) -0.032(8) N2 0.037(4) 0.035(4) 0.065(5) 0.026(4) 0.032(4) 0.011(3) C2 0.026(5) 0.064(7) 0.075(7) 0.042(6) 0.011(5) -0.001(5) F3 0.192(9) 0.098(5) 0.070(5) 0.034(4) 0.048(5) 0.058(6) N3 0.033(4) 0.037(4) 0.060(5) 0.027(4) 0.015(4) 0.015(3) C3 0.051(7) 0.070(7) 0.079(8) 0.044(7) 0.026(6) 0.003(6) F4 0.250(12) 0.076(5) 0.089(6) -0.008(5) 0.090(7) 0.026(6) N4 0.030(4) 0.037(4) 0.046(5) 0.027(4) 0.013(4) 0.011(3) N5 0.040(5) 0.060(5) 0.065(5) 0.043(5) 0.023(4) 0.020(4) C5 0.082(10) 0.080(9) 0.145(12) 0.072(9) 0.041(9) 0.002(7) N6 0.027(4) 0.036(4) 0.059(5) 0.028(4) 0.012(4) 0.011(3) C6 0.105(10) 0.077(8) 0.070(7) 0.054(7) 0.025(7) 0.041(7) N7 0.030(4) 0.037(4) 0.043(4) 0.019(4) 0.006(4) 0.008(3) C7 0.029(5) 0.057(6) 0.055(6) 0.033(6) 0.004(5) 0.003(5) N8 0.028(4) 0.027(4) 0.046(4) 0.019(4) 0.001(3) 0.007(3) C8 0.058(7) 0.044(6) 0.041(6) 0.013(5) -0.009(5) 0.002(5) N9 0.024(4) 0.039(4) 0.056(5) 0.030(4) 0.013(4) 0.009(3) C9 0.045(6) 0.039(6) 0.052(6) 0.023(5) 0.006(5) 0.007(5) N10 0.035(4) 0.040(4) 0.051(5) 0.027(4) 0.007(4) -0.005(4) C10 0.124(12) 0.055(7) 0.049(7) 0.011(6) 0.001(7) 0.013(7) N11 0.031(4) 0.045(4) 0.034(4) 0.024(4) 0.005(3) 0.009(3) C11 0.041(6) 0.039(6) 0.076(7) 0.010(5) 0.020(6) -0.006(5) N12 0.040(5) 0.027(4) 0.041(5) 0.017(4) 0.008(4) 0.004(3) C12 0.032(6) 0.046(6) 0.050(6) 0.019(5) 0.000(5) -0.001(5) N13 0.111(11) 0.163(13) 0.130(11) 0.099(11) 0.010(9) 0.032(10) C13 0.023(5) 0.061(7) 0.067(7) 0.034(6) 0.002(5) 0.009(5) C14 0.034(5) 0.055(6) 0.059(6) 0.037(6) 0.006(5) 0.017(5) C15 0.069(8) 0.070(8) 0.067(7) 0.035(7) 0.004(6) 0.027(6) C16 0.026(5) 0.035(5) 0.044(5) 0.021(5) -0.001(4) -0.002(4) C17 0.067(8) 0.046(6) 0.108(9) 0.042(7) 0.062(7) 0.029(6) C18 0.116(10) 0.048(7) 0.106(9) 0.036(7) 0.091(9) 0.017(7) C19 0.069(7) 0.037(6) 0.085(8) 0.039(6) 0.046(6) 0.014(5) C20 0.031(5) 0.043(6) 0.064(7) 0.027(6) 0.005(5) 0.003(4) C21 0.028(5) 0.053(6) 0.031(5) 0.010(5) 0.002(4) -0.002(4) C22 0.039(6) 0.028(5) 0.054(6) 0.007(5) 0.019(5) 0.000(4) C23 0.035(6) 0.057(6) 0.078(8) 0.034(6) 0.009(6) 0.009(5) C24 0.040(6) 0.070(8) 0.089(8) 0.046(7) 0.013(6) 0.027(6) C25 0.049(7) 0.052(7) 0.084(8) 0.039(7) 0.022(6) 0.023(6) C26 0.039(6) 0.044(5) 0.057(6) 0.032(5) 0.025(5) 0.022(5) C27 0.055(7) 0.048(6) 0.081(7) 0.043(6) 0.029(6) 0.031(5) C28 0.103(10) 0.033(5) 0.092(8) 0.043(6) 0.058(7) 0.035(6) C29 0.076(8) 0.026(5) 0.075(8) 0.028(6) 0.040(7) 0.017(5) C30 0.098(10) 0.036(6) 0.067(8) 0.024(6) 0.053(7) 0.017(6) C31 0.119(11) 0.033(6) 0.051(6) 0.016(5) 0.050(7) -0.003(6) C32 0.123(14) 0.067(9) 0.143(13) 0.045(10) -0.018(11) 0.010(9) C33 0.088(11) 0.085(9) 0.080(9) 0.044(8) 0.031(8) 0.020(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.914(7) . ? Fe1 N6 1.945(7) . ? Fe1 N2 1.947(7) . ? Fe1 N7 1.979(6) . ? Fe1 N11 1.979(7) . ? Fe1 N9 1.991(7) . ? F1 B1 1.392(17) . ? O1 C27 1.378(11) . ? O1 C28 1.472(10) . ? N1 C19 1.386(11) . ? N1 N2 1.389(9) . ? N1 C26 1.451(10) . ? C1 C2 1.489(14) . ? B1 F2 1.325(18) . ? B1 F4 1.353(17) . ? B1 F3 1.371(16) . ? N2 C17 1.291(11) . ? C2 N9 1.319(11) . ? C2 C3 1.433(13) . ? B2 F6B 1.316(11) . ? B2 F5 1.342(10) . ? B2 F7A 1.349(11) . ? B2 F8A 1.351(11) . ? B2 F7B 1.353(11) . ? B2 F8B 1.415(11) . ? B2 F6A 1.452(11) . ? N3 C22 1.380(11) . ? N3 N4 1.403(9) . ? N3 C26 1.430(11) . ? C3 C4 1.374(14) . ? N4 C20 1.333(11) . ? C4 N10 1.344(12) . ? C4 C5 1.519(15) . ? N5 C25 1.367(11) . ? N5 N6 1.374(10) . ? N5 C26 1.471(11) . ? F6A F6B 1.065(19) . ? N6 C23 1.299(11) . ? C6 C7 1.485(12) . ? N7 C12 1.335(10) . ? N7 N8 1.384(9) . ? C7 N11 1.333(11) . ? C7 C8 1.432(13) . ? N8 C14 1.355(10) . ? N8 C16 1.418(10) . ? C8 C9 1.309(12) . ? F7B F7A 0.64(2) . ? N9 N10 1.377(9) . ? C9 N12 1.355(11) . ? C9 C10 1.508(13) . ? N10 C16 1.450(11) . ? N11 N12 1.385(8) . ? C11 C12 1.483(12) . ? N12 C16 1.454(10) . ? C12 C13 1.431(12) . ? N13 C33 1.103(15) . ? C13 C14 1.333(12) . ? N14 C35 1.22(3) . ? C14 C15 1.524(13) . ? N15 C37 1.09(3) . ? N16 C39 1.20(3) . ? N17 C41 1.23(3) . ? C17 C18 1.421(13) . ? C18 C19 1.365(14) . ? C20 C21 1.387(12) . ? C21 C22 1.385(12) . ? C23 C24 1.398(13) . ? C24 C25 1.321(14) . ? C26 C27 1.520(12) . ? C28 C29 1.536(15) . ? C29 C30 1.357(14) . ? C29 C31 1.388(14) . ? C30 C31 1.393(15) 2 ? C31 C30 1.393(15) 2 ? C32 C33 1.442(19) . ? C34 C35 1.43(3) . ? C36 C37 1.37(3) . ? C38 C39 1.30(3) . ? C40 C41 1.49(3) . ? F8A F8B 1.226(16) . ? F8A F6B 1.312(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N6 87.4(3) . . ? N4 Fe1 N2 87.9(3) . . ? N6 Fe1 N2 87.1(3) . . ? N4 Fe1 N7 91.4(3) . . ? N6 Fe1 N7 177.8(3) . . ? N2 Fe1 N7 91.0(3) . . ? N4 Fe1 N11 179.2(3) . . ? N6 Fe1 N11 93.1(3) . . ? N2 Fe1 N11 92.7(3) . . ? N7 Fe1 N11 88.1(3) . . ? N4 Fe1 N9 91.4(3) . . ? N6 Fe1 N9 92.2(3) . . ? N2 Fe1 N9 179.0(3) . . ? N7 Fe1 N9 89.8(3) . . ? N11 Fe1 N9 88.0(3) . . ? C27 O1 C28 110.1(7) . . ? C19 N1 N2 109.5(7) . . ? C19 N1 C26 131.1(7) . . ? N2 N1 C26 119.1(6) . . ? F2 B1 F4 115.7(14) . . ? F2 B1 F3 107.0(13) . . ? F4 B1 F3 110.8(14) . . ? F2 B1 F1 107.8(14) . . ? F4 B1 F1 106.5(12) . . ? F3 B1 F1 108.8(12) . . ? C17 N2 N1 106.4(7) . . ? C17 N2 Fe1 134.6(6) . . ? N1 N2 Fe1 118.5(5) . . ? N9 C2 C3 110.6(9) . . ? N9 C2 C1 123.0(8) . . ? C3 C2 C1 126.3(9) . . ? F6B B2 F5 110.3(11) . . ? F6B B2 F7A 133.4(15) . . ? F5 B2 F7A 112.1(10) . . ? F6B B2 F8A 58.9(9) . . ? F5 B2 F8A 116.7(10) . . ? F7A B2 F8A 114.8(11) . . ? F6B B2 F7B 118.5(11) . . ? F5 B2 F7B 108.7(10) . . ? F7A B2 F7B 27.2(10) . . ? F8A B2 F7B 132.1(14) . . ? F6B B2 F8B 111.4(10) . . ? F5 B2 F8B 97.5(8) . . ? F7A B2 F8B 81.4(10) . . ? F8A B2 F8B 52.5(7) . . ? F7B B2 F8B 108.5(10) . . ? F6B B2 F6A 44.9(8) . . ? F5 B2 F6A 101.3(8) . . ? F7A B2 F6A 107.5(10) . . ? F8A B2 F6A 102.5(9) . . ? F7B B2 F6A 82.2(9) . . ? F8B B2 F6A 154.0(11) . . ? C22 N3 N4 111.1(7) . . ? C22 N3 C26 130.1(7) . . ? N4 N3 C26 118.4(7) . . ? C4 C3 C2 105.0(9) . . ? C20 N4 N3 103.9(7) . . ? C20 N4 Fe1 136.2(6) . . ? N3 N4 Fe1 119.7(5) . . ? N10 C4 C3 107.1(9) . . ? N10 C4 C5 124.8(10) . . ? C3 C4 C5 128.1(10) . . ? C25 N5 N6 110.8(8) . . ? C25 N5 C26 130.5(8) . . ? N6 N5 C26 118.5(6) . . ? F6B F6A B2 60.8(7) . . ? C23 N6 N5 104.0(7) . . ? C23 N6 Fe1 136.6(6) . . ? N5 N6 Fe1 119.3(5) . . ? C12 N7 N8 105.7(6) . . ? C12 N7 Fe1 137.4(6) . . ? N8 N7 Fe1 116.9(5) . . ? N11 C7 C8 109.8(8) . . ? N11 C7 C6 122.0(9) . . ? C8 C7 C6 128.2(9) . . ? C14 N8 N7 110.9(7) . . ? C14 N8 C16 130.6(7) . . ? N7 N8 C16 118.4(6) . . ? C9 C8 C7 107.1(9) . . ? F7A F7B B2 76.1(12) . . ? C2 N9 N10 105.3(7) . . ? C2 N9 Fe1 139.2(6) . . ? N10 N9 Fe1 115.4(5) . . ? C8 C9 N12 107.5(8) . . ? C8 C9 C10 132.2(10) . . ? N12 C9 C10 120.3(8) . . ? C4 N10 N9 111.9(8) . . ? C4 N10 C16 128.4(8) . . ? N9 N10 C16 119.7(6) . . ? C7 N11 N12 103.8(7) . . ? C7 N11 Fe1 139.2(6) . . ? N12 N11 Fe1 117.0(5) . . ? C9 N12 N11 111.8(6) . . ? C9 N12 C16 130.4(7) . . ? N11 N12 C16 117.8(7) . . ? N7 C12 C13 108.5(8) . . ? N7 C12 C11 123.7(8) . . ? C13 C12 C11 127.8(8) . . ? C14 C13 C12 107.5(8) . . ? C13 C14 N8 107.3(8) . . ? C13 C14 C15 130.7(8) . . ? N8 C14 C15 122.0(8) . . ? N8 C16 N10 110.4(7) . . ? N8 C16 N12 111.1(6) . . ? N10 C16 N12 108.9(6) . . ? N2 C17 C18 111.8(9) . . ? C19 C18 C17 105.4(9) . . ? C18 C19 N1 106.9(8) . . ? N4 C20 C21 112.7(8) . . ? C22 C21 C20 106.5(8) . . ? N3 C22 C21 105.8(8) . . ? N6 C23 C24 112.0(9) . . ? C25 C24 C23 106.3(9) . . ? C24 C25 N5 106.8(9) . . ? N3 C26 N1 108.9(6) . . ? N3 C26 N5 107.6(7) . . ? N1 C26 N5 107.6(7) . . ? N3 C26 C27 112.1(8) . . ? N1 C26 C27 109.8(7) . . ? N5 C26 C27 110.7(7) . . ? O1 C27 C26 108.2(7) . . ? O1 C28 C29 105.2(8) . . ? C30 C29 C31 118.8(10) . . ? C30 C29 C28 120.2(10) . . ? C31 C29 C28 121.0(11) . . ? C29 C30 C31 121.9(10) . 2 ? C29 C31 C30 119.3(10) . 2 ? N13 C33 C32 178.0(17) . . ? N14 C35 C34 175(3) . . ? N15 C37 C36 172(3) . . ? N16 C39 C38 166(3) . . ? N17 C41 C40 155(2) . . ? F8B F8A F6B 125.6(9) . . ? F8B F8A B2 66.4(7) . . ? F6B F8A B2 59.2(7) . . ? F8A F8B B2 61.0(6) . . ? F6A F6B F8A 133.7(13) . . ? F6A F6B B2 74.3(9) . . ? F8A F6B B2 61.9(7) . . ? F7B F7A B2 76.7(12) . . ? 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 C19 N1 N2 C17 -0.2(10) . . . . ? C26 N1 N2 C17 -174.7(8) . . . . ? C19 N1 N2 Fe1 172.0(6) . . . . ? C26 N1 N2 Fe1 -2.4(9) . . . . ? N4 Fe1 N2 C17 -146.1(10) . . . . ? N6 Fe1 N2 C17 126.3(10) . . . . ? N7 Fe1 N2 C17 -54.8(10) . . . . ? N11 Fe1 N2 C17 33.3(10) . . . . ? N9 Fe1 N2 C17 164(17) . . . . ? N4 Fe1 N2 N1 44.3(6) . . . . ? N6 Fe1 N2 N1 -43.2(6) . . . . ? N7 Fe1 N2 N1 135.7(6) . . . . ? N11 Fe1 N2 N1 -136.2(6) . . . . ? N9 Fe1 N2 N1 -5(18) . . . . ? N9 C2 C3 C4 1.3(11) . . . . ? C1 C2 C3 C4 -175.2(10) . . . . ? C22 N3 N4 C20 0.7(9) . . . . ? C26 N3 N4 C20 173.7(7) . . . . ? C22 N3 N4 Fe1 -175.2(5) . . . . ? C26 N3 N4 Fe1 -2.2(9) . . . . ? N6 Fe1 N4 C20 -129.4(8) . . . . ? N2 Fe1 N4 C20 143.5(8) . . . . ? N7 Fe1 N4 C20 52.6(8) . . . . ? N11 Fe1 N4 C20 4(20) . . . . ? N9 Fe1 N4 C20 -37.3(8) . . . . ? N6 Fe1 N4 N3 44.9(6) . . . . ? N2 Fe1 N4 N3 -42.3(6) . . . . ? N7 Fe1 N4 N3 -133.2(6) . . . . ? N11 Fe1 N4 N3 178(100) . . . . ? N9 Fe1 N4 N3 137.0(6) . . . . ? C2 C3 C4 N10 0.0(11) . . . . ? C2 C3 C4 C5 -178.9(11) . . . . ? F5 B2 F6A F6B 107.4(13) . . . . ? F7A B2 F6A F6B -134.8(17) . . . . ? F8A B2 F6A F6B -13.5(15) . . . . ? F7B B2 F6A F6B -145.0(15) . . . . ? F8B B2 F6A F6B -28(3) . . . . ? C25 N5 N6 C23 2.3(10) . . . . ? C26 N5 N6 C23 178.4(8) . . . . ? C25 N5 N6 Fe1 -179.8(6) . . . . ? C26 N5 N6 Fe1 -3.7(10) . . . . ? N4 Fe1 N6 C23 135.4(10) . . . . ? N2 Fe1 N6 C23 -136.5(10) . . . . ? N7 Fe1 N6 C23 -166(7) . . . . ? N11 Fe1 N6 C23 -44.0(10) . . . . ? N9 Fe1 N6 C23 44.1(10) . . . . ? N4 Fe1 N6 N5 -41.6(6) . . . . ? N2 Fe1 N6 N5 46.5(6) . . . . ? N7 Fe1 N6 N5 17(8) . . . . ? N11 Fe1 N6 N5 139.0(6) . . . . ? N9 Fe1 N6 N5 -132.9(6) . . . . ? N4 Fe1 N7 C12 45.2(9) . . . . ? N6 Fe1 N7 C12 -14(8) . . . . ? N2 Fe1 N7 C12 -42.8(9) . . . . ? N11 Fe1 N7 C12 -135.4(9) . . . . ? N9 Fe1 N7 C12 136.6(9) . . . . ? N4 Fe1 N7 N8 -133.1(6) . . . . ? N6 Fe1 N7 N8 168(7) . . . . ? N2 Fe1 N7 N8 138.9(6) . . . . ? N11 Fe1 N7 N8 46.3(6) . . . . ? N9 Fe1 N7 N8 -41.7(6) . . . . ? C12 N7 N8 C14 0.2(9) . . . . ? Fe1 N7 N8 C14 178.9(6) . . . . ? C12 N7 N8 C16 178.0(7) . . . . ? Fe1 N7 N8 C16 -3.2(9) . . . . ? N11 C7 C8 C9 2.1(11) . . . . ? C6 C7 C8 C9 -179.7(11) . . . . ? F6B B2 F7B F7A 131(2) . . . . ? F5 B2 F7B F7A -102(2) . . . . ? F8A B2 F7B F7A 59(3) . . . . ? F8B B2 F7B F7A 3(2) . . . . ? F6A B2 F7B F7A 158(2) . . . . ? C3 C2 N9 N10 -2.0(10) . . . . ? C1 C2 N9 N10 174.6(9) . . . . ? C3 C2 N9 Fe1 177.2(7) . . . . ? C1 C2 N9 Fe1 -6.2(16) . . . . ? N4 Fe1 N9 C2 -45.4(9) . . . . ? N6 Fe1 N9 C2 42.1(10) . . . . ? N2 Fe1 N9 C2 4(18) . . . . ? N7 Fe1 N9 C2 -136.8(10) . . . . ? N11 Fe1 N9 C2 135.1(10) . . . . ? N4 Fe1 N9 N10 133.7(5) . . . . ? N6 Fe1 N9 N10 -138.8(6) . . . . ? N2 Fe1 N9 N10 -177(100) . . . . ? N7 Fe1 N9 N10 42.3(5) . . . . ? N11 Fe1 N9 N10 -45.8(5) . . . . ? C7 C8 C9 N12 -2.5(11) . . . . ? C7 C8 C9 C10 176.4(11) . . . . ? C3 C4 N10 N9 -1.3(10) . . . . ? C5 C4 N10 N9 177.7(9) . . . . ? C3 C4 N10 C16 -179.1(8) . . . . ? C5 C4 N10 C16 -0.1(15) . . . . ? C2 N9 N10 C4 2.1(9) . . . . ? Fe1 N9 N10 C4 -177.3(6) . . . . ? C2 N9 N10 C16 -180.0(7) . . . . ? Fe1 N9 N10 C16 0.7(9) . . . . ? C8 C7 N11 N12 -0.8(9) . . . . ? C6 C7 N11 N12 -179.1(9) . . . . ? C8 C7 N11 Fe1 179.0(7) . . . . ? C6 C7 N11 Fe1 0.7(15) . . . . ? N4 Fe1 N11 C7 -175(100) . . . . ? N6 Fe1 N11 C7 -41.6(9) . . . . ? N2 Fe1 N11 C7 45.6(9) . . . . ? N7 Fe1 N11 C7 136.5(9) . . . . ? N9 Fe1 N11 C7 -133.7(9) . . . . ? N4 Fe1 N11 N12 5(20) . . . . ? N6 Fe1 N11 N12 138.1(6) . . . . ? N2 Fe1 N11 N12 -134.7(6) . . . . ? N7 Fe1 N11 N12 -43.8(6) . . . . ? N9 Fe1 N11 N12 46.1(6) . . . . ? C8 C9 N12 N11 2.2(10) . . . . ? C10 C9 N12 N11 -176.9(9) . . . . ? C8 C9 N12 C16 -177.8(8) . . . . ? C10 C9 N12 C16 3.1(15) . . . . ? C7 N11 N12 C9 -0.8(9) . . . . ? Fe1 N11 N12 C9 179.4(6) . . . . ? C7 N11 N12 C16 179.2(7) . . . . ? Fe1 N11 N12 C16 -0.6(9) . . . . ? N8 N7 C12 C13 1.2(10) . . . . ? Fe1 N7 C12 C13 -177.2(7) . . . . ? N8 N7 C12 C11 -177.9(9) . . . . ? Fe1 N7 C12 C11 3.7(15) . . . . ? N7 C12 C13 C14 -2.2(11) . . . . ? C11 C12 C13 C14 176.8(10) . . . . ? C12 C13 C14 N8 2.2(11) . . . . ? C12 C13 C14 C15 -178.7(10) . . . . ? N7 N8 C14 C13 -1.6(10) . . . . ? C16 N8 C14 C13 -179.0(9) . . . . ? N7 N8 C14 C15 179.2(8) . . . . ? C16 N8 C14 C15 1.8(14) . . . . ? C14 N8 C16 N10 -120.4(9) . . . . ? N7 N8 C16 N10 62.3(9) . . . . ? C14 N8 C16 N12 118.7(9) . . . . ? N7 N8 C16 N12 -58.6(10) . . . . ? C4 N10 C16 N8 116.5(9) . . . . ? N9 N10 C16 N8 -61.2(9) . . . . ? C4 N10 C16 N12 -121.4(9) . . . . ? N9 N10 C16 N12 61.0(9) . . . . ? C9 N12 C16 N8 -118.9(9) . . . . ? N11 N12 C16 N8 61.1(9) . . . . ? C9 N12 C16 N10 119.3(9) . . . . ? N11 N12 C16 N10 -60.6(9) . . . . ? N1 N2 C17 C18 -1.5(12) . . . . ? Fe1 N2 C17 C18 -172.0(8) . . . . ? N2 C17 C18 C19 2.7(14) . . . . ? C17 C18 C19 N1 -2.6(13) . . . . ? N2 N1 C19 C18 1.9(11) . . . . ? C26 N1 C19 C18 175.4(10) . . . . ? N3 N4 C20 C21 0.0(9) . . . . ? Fe1 N4 C20 C21 174.9(6) . . . . ? N4 C20 C21 C22 -0.7(10) . . . . ? N4 N3 C22 C21 -1.1(9) . . . . ? C26 N3 C22 C21 -173.1(8) . . . . ? C20 C21 C22 N3 1.1(9) . . . . ? N5 N6 C23 C24 -3.0(11) . . . . ? Fe1 N6 C23 C24 179.7(7) . . . . ? N6 C23 C24 C25 2.6(13) . . . . ? C23 C24 C25 N5 -1.0(12) . . . . ? N6 N5 C25 C24 -0.8(12) . . . . ? C26 N5 C25 C24 -176.3(9) . . . . ? C22 N3 C26 N1 -129.3(8) . . . . ? N4 N3 C26 N1 59.2(9) . . . . ? C22 N3 C26 N5 114.3(9) . . . . ? N4 N3 C26 N5 -57.2(9) . . . . ? C22 N3 C26 C27 -7.7(12) . . . . ? N4 N3 C26 C27 -179.1(7) . . . . ? C19 N1 C26 N3 130.5(9) . . . . ? N2 N1 C26 N3 -56.5(10) . . . . ? C19 N1 C26 N5 -113.1(10) . . . . ? N2 N1 C26 N5 59.9(9) . . . . ? C19 N1 C26 C27 7.4(13) . . . . ? N2 N1 C26 C27 -179.5(7) . . . . ? C25 N5 C26 N3 -123.9(9) . . . . ? N6 N5 C26 N3 60.9(9) . . . . ? C25 N5 C26 N1 118.8(10) . . . . ? N6 N5 C26 N1 -56.4(9) . . . . ? C25 N5 C26 C27 -1.2(13) . . . . ? N6 N5 C26 C27 -176.4(8) . . . . ? C28 O1 C27 C26 175.8(8) . . . . ? N3 C26 C27 O1 -61.1(10) . . . . ? N1 C26 C27 O1 60.1(10) . . . . ? N5 C26 C27 O1 178.7(7) . . . . ? C27 O1 C28 C29 168.7(8) . . . . ? O1 C28 C29 C30 95.9(10) . . . . ? O1 C28 C29 C31 -86.1(10) . . . . ? C31 C29 C30 C31 1.8(16) . . . 2 ? C28 C29 C30 C31 179.8(8) . . . 2 ? C30 C29 C31 C30 -1.8(16) . . . 2 ? C28 C29 C31 C30 -179.8(8) . . . 2 ? F6B B2 F8A F8B 177.0(15) . . . . ? F5 B2 F8A F8B 78.4(11) . . . . ? F7A B2 F8A F8B -55.7(14) . . . . ? F7B B2 F8A F8B -81.2(15) . . . . ? F6A B2 F8A F8B -172.0(12) . . . . ? F5 B2 F8A F6B -98.6(12) . . . . ? F7A B2 F8A F6B 127.3(16) . . . . ? F7B B2 F8A F6B 101.8(15) . . . . ? F8B B2 F8A F6B -177.0(15) . . . . ? F6A B2 F8A F6B 11.1(12) . . . . ? F6B F8A F8B B2 3.2(16) . . . . ? F6B B2 F8B F8A -2.8(14) . . . . ? F5 B2 F8B F8A -118.0(11) . . . . ? F7A B2 F8B F8A 130.6(13) . . . . ? F7B B2 F8B F8A 129.3(15) . . . . ? F6A B2 F8B F8A 18(3) . . . . ? B2 F6A F6B F8A 18.9(19) . . . . ? F8B F8A F6B F6A -24(3) . . . . ? B2 F8A F6B F6A -21(2) . . . . ? F8B F8A F6B B2 -3.4(17) . . . . ? F5 B2 F6B F6A -85.7(13) . . . . ? F7A B2 F6B F6A 68.7(19) . . . . ? F8A B2 F6B F6A 164.6(17) . . . . ? F7B B2 F6B F6A 40.3(17) . . . . ? F8B B2 F6B F6A 167.2(13) . . . . ? F5 B2 F6B F8A 109.7(11) . . . . ? F7A B2 F6B F8A -95.9(17) . . . . ? F7B B2 F6B F8A -124.3(16) . . . . ? F8B B2 F6B F8A 2.6(13) . . . . ? F6A B2 F6B F8A -164.6(17) . . . . ? F6B B2 F7A F7B -66(3) . . . . ? F5 B2 F7A F7B 88(2) . . . . ? F8A B2 F7A F7B -136(2) . . . . ? F8B B2 F7A F7B -177(2) . . . . ? F6A B2 F7A F7B -22(2) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.910 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.176 # Attachment '- 2.2.5MeCN.2DME.CIF' #========================================================================== data_2.2.5MeCN.2DME _database_code_depnum_ccdc_archive 'CCDC 803926' #TrackingRef '- 2.2.5MeCN.2DME.CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(C10H(CH2OCH2C(pz)3]2)](BF4)4(MeCN)2.5(DME)2 ; _chemical_name_common ;((Fe((3,5- Me2pz)3CH))2(C10H(CH2OCH2C(pz)3)2))(BF4)4(MeCN)2.5(DME)2 ; _chemical_melting_point ? _chemical_formula_moiety ; C66 H76 Fe2 N24 O2, 2.5(C2 H3 N), 2(C4 H10 O2), 4(B F4) ; _chemical_formula_sum 'C79 H103.50 B4 F16 Fe2 N26.50 O6' _chemical_formula_weight 1979.32 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1238(6) _cell_length_b 16.4661(9) _cell_length_c 23.0010(12) _cell_angle_alpha 69.346(3) _cell_angle_beta 82.768(3) _cell_angle_gamma 70.093(3) _cell_volume 4706.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 16557 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2054 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _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 93505 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16557 _reflns_number_gt 11410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16557 _refine_ls_number_parameters 1235 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 F1 F 0.2578(3) 0.3176(2) 0.68061(16) 0.0638(9) Uani 1 1 d . . . O1 O 0.8821(3) 0.4314(2) 0.34840(14) 0.0412(8) Uani 1 1 d . . . N2 N 0.6045(3) 0.4082(2) 0.33619(16) 0.0308(8) Uani 1 1 d . . . C17 C 0.5314(4) 0.4745(3) 0.3497(2) 0.0354(10) Uani 1 1 d . . . H17 H 0.4638 0.4746 0.3589 0.043 Uiso 1 1 calc R . . B1 B 0.3167(5) 0.2680(5) 0.6462(4) 0.0533(17) Uani 1 1 d . . . F2 F 0.4064(3) 0.2807(3) 0.63176(18) 0.0766(11) Uani 1 1 d . . . O3 O 0.2495(3) 0.6326(3) 0.43476(19) 0.0625(11) Uani 1 1 d . . . N4 N 0.7454(3) 0.2416(2) 0.37298(16) 0.0302(8) Uani 1 1 d . . . C18 C 0.5668(4) 0.5441(3) 0.3485(2) 0.0423(12) Uani 1 1 d . . . H18 H 0.5292 0.5985 0.3572 0.051 Uiso 1 1 calc R . . B2 B 0.0805(5) 0.4258(5) 0.1521(3) 0.0533(16) Uani 1 1 d . . . F3 F 0.3341(6) 0.1798(4) 0.6792(6) 0.233(5) Uani 1 1 d . . . O4 O 0.3387(4) 0.4557(3) 0.4218(3) 0.0807(14) Uani 1 1 d . . . N6 N 0.6879(3) 0.3243(3) 0.25344(16) 0.0317(8) Uani 1 1 d . . . C19 C 0.6655(4) 0.5190(3) 0.3325(2) 0.0401(12) Uani 1 1 d . . . H19 H 0.7104 0.5529 0.3271 0.048 Uiso 1 1 calc R . . B3 B 0.1823(5) 0.0834(4) 0.4409(3) 0.0437(14) Uani 1 1 d . . . F4 F 0.2693(4) 0.2670(7) 0.6028(3) 0.177(4) Uani 1 1 d . . . O2 O 0.7994(2) 0.3318(2) 0.93414(14) 0.0388(8) Uani 1 1 d . . . N1 N 0.6878(3) 0.4356(2) 0.32555(16) 0.0325(8) Uani 1 1 d . . . C20 C 0.7915(3) 0.1642(3) 0.4166(2) 0.0354(10) Uani 1 1 d . . . H20 H 0.7636 0.1165 0.4378 0.042 Uiso 1 1 calc R . . B4 B 0.3334(5) 0.8552(4) 0.8752(3) 0.0438(14) Uani 1 1 d . . . F5 F 0.0645(4) 0.4220(4) 0.21186(18) 0.133(2) Uani 1 1 d . . . O5 O 0.3635(4) 0.3313(4) 0.9163(2) 0.0965(17) Uani 1 1 d . . . N3 N 0.8113(3) 0.2898(2) 0.35549(16) 0.0305(8) Uani 1 1 d . . . C21 C 0.8879(4) 0.1632(3) 0.4269(2) 0.0381(11) Uani 1 1 d . . . H21 H 0.9365 0.1156 0.4555 0.046 Uiso 1 1 calc R . . F6 F 0.0836(4) 0.5097(3) 0.11538(18) 0.0897(13) Uani 1 1 d . . . O6 O 0.2047(3) 0.3832(3) 0.8282(2) 0.0663(11) Uani 1 1 d . . . N5 N 0.7603(3) 0.3641(3) 0.25100(17) 0.0360(9) Uani 1 1 d . . . C22 C 0.8978(3) 0.2427(3) 0.3881(2) 0.0361(11) Uani 1 1 d . . . H22 H 0.9549 0.2624 0.3843 0.043 Uiso 1 1 calc R . . F7 F 0.1727(3) 0.3643(3) 0.14582(19) 0.0926(13) Uani 1 1 d . . . N7 N 0.5487(3) 0.2571(2) 0.41274(16) 0.0285(8) Uani 1 1 d . . . C23 C 0.6865(4) 0.3203(3) 0.1975(2) 0.0401(11) Uani 1 1 d . . . H23 H 0.6432 0.2962 0.1851 0.048 Uiso 1 1 calc R . . F8 F 0.0081(4) 0.4061(4) 0.1342(3) 0.127(2) Uani 1 1 d . . . N9 N 0.6327(3) 0.1679(2) 0.32634(17) 0.0301(8) Uani 1 1 d . . . C24 C 0.7573(5) 0.3563(4) 0.1587(2) 0.0549(15) Uani 1 1 d . . . H24 H 0.7714 0.3603 0.1164 0.066 Uiso 1 1 calc R . . F9 F 0.1241(3) 0.0421(3) 0.4263(2) 0.0769(11) Uani 1 1 d . . . N11 N 0.4846(3) 0.3338(2) 0.29133(17) 0.0319(8) Uani 1 1 d . . . C25 C 0.8017(4) 0.3847(4) 0.1937(2) 0.0499(14) Uani 1 1 d . . . H25 H 0.8524 0.4134 0.1804 0.060 Uiso 1 1 calc R . . F10 F 0.1263(2) 0.1681(2) 0.44196(17) 0.0614(9) Uani 1 1 d . . . N8 N 0.4788(3) 0.2139(2) 0.41772(16) 0.0289(8) Uani 1 1 d . . . C26 C 0.7802(4) 0.3781(3) 0.3067(2) 0.0333(10) Uani 1 1 d . . . F11 F 0.2222(3) 0.0300(3) 0.49923(17) 0.0777(11) Uani 1 1 d . . . N10 N 0.5525(3) 0.1357(2) 0.34638(17) 0.0301(8) Uani 1 1 d . . . C27 C 0.8628(4) 0.4221(4) 0.2933(2) 0.0398(11) Uani 1 1 d . . . H27A H 0.9245 0.3833 0.2786 0.048 Uiso 1 1 calc R . . H27B H 0.8409 0.4829 0.2605 0.048 Uiso 1 1 calc R . . F12 F 0.2641(2) 0.0879(2) 0.40171(15) 0.0593(9) Uani 1 1 d . . . N12 N 0.4253(3) 0.2779(2) 0.31393(16) 0.0308(8) Uani 1 1 d . . . C28 C 0.9589(5) 0.4728(4) 0.3407(2) 0.0539(15) Uani 1 1 d . . . H28A H 0.9351 0.5373 0.3131 0.065 Uiso 1 1 calc R . . H28B H 1.0198 0.4396 0.3219 0.065 Uiso 1 1 calc R . . F13 F 0.2539(3) 0.8240(2) 0.90192(17) 0.0684(9) Uani 1 1 d . . . N18 N 0.8061(3) 0.1306(3) 0.86784(17) 0.0361(9) Uani 1 1 d . . . C29 C 0.9829(4) 0.4685(4) 0.4033(2) 0.0404(12) Uani 1 1 d . . . F14 F 0.3725(3) 0.8747(4) 0.91829(19) 0.0934(14) Uani 1 1 d . . . N16 N 0.8635(3) 0.2616(3) 0.77725(17) 0.0334(9) Uani 1 1 d . . . C30 C 0.9513(4) 0.5443(3) 0.4203(2) 0.0395(11) Uani 1 1 d . . . H30 H 0.9130 0.6007 0.3917 0.047 Uiso 1 1 calc R . . F15 F 0.2985(3) 0.9329(3) 0.82641(17) 0.0830(12) Uani 1 1 d . . . N14 N 1.0018(3) 0.1074(3) 0.84486(17) 0.0331(8) Uani 1 1 d . . . C31 C 0.9732(3) 0.5422(3) 0.4785(2) 0.0339(10) Uani 1 1 d . . . F16 F 0.4074(2) 0.7910(2) 0.85510(17) 0.0645(9) Uani 1 1 d . . . N17 N 0.8179(3) 0.1756(3) 0.90428(17) 0.0354(9) Uani 1 1 d . . . C32 C 1.0367(4) 0.3848(4) 0.4457(3) 0.0471(13) Uani 1 1 d . . . H32 H 1.0587 0.3311 0.4344 0.057 Uiso 1 1 calc R . . N15 N 0.8695(3) 0.2907(2) 0.82446(17) 0.0322(8) Uani 1 1 d . . . C33 C 1.0577(4) 0.3801(4) 0.5031(2) 0.0461(12) Uani 1 1 d . . . H33 H 1.0943 0.3227 0.5315 0.055 Uiso 1 1 calc R . . N13 N 0.9909(3) 0.1571(3) 0.88370(17) 0.0342(9) Uani 1 1 d . . . C2 C 0.5482(3) 0.2662(3) 0.4680(2) 0.0305(10) Uani 1 1 d . . . N23 N 0.9162(3) 0.0003(3) 0.80833(17) 0.0345(9) Uani 1 1 d . . . C3 C 0.4792(3) 0.2299(3) 0.5076(2) 0.0346(10) Uani 1 1 d . . . H3 H 0.4654 0.2278 0.5495 0.042 Uiso 1 1 calc R . . N19 N 0.9753(3) 0.1335(3) 0.71961(16) 0.0315(8) Uani 1 1 d . . . C4 C 0.4348(3) 0.1976(3) 0.4749(2) 0.0329(10) Uani 1 1 d . . . N21 N 0.7726(3) 0.1584(3) 0.74359(17) 0.0343(9) Uani 1 1 d . . . C1 C 0.6137(4) 0.3111(3) 0.4837(2) 0.0384(11) Uani 1 1 d . . . H1A H 0.6752 0.3040 0.4583 0.058 Uiso 1 1 calc R . . H1B H 0.6315 0.2821 0.5278 0.058 Uiso 1 1 calc R . . H1C H 0.5770 0.3764 0.4752 0.058 Uiso 1 1 calc R . . N24 N 0.9084(3) -0.0235(2) 0.75790(17) 0.0321(8) Uani 1 1 d . . . C5 C 0.3562(4) 0.1529(4) 0.4927(2) 0.0425(12) Uani 1 1 d . . . H5A H 0.2989 0.1886 0.4645 0.064 Uiso 1 1 calc R . . H5B H 0.3338 0.1494 0.5354 0.064 Uiso 1 1 calc R . . H5C H 0.3835 0.0910 0.4902 0.064 Uiso 1 1 calc R . . N20 N 0.9588(3) 0.0926(3) 0.68154(16) 0.0317(8) Uani 1 1 d . . . C7 C 0.7021(3) 0.1022(3) 0.3098(2) 0.0336(10) Uani 1 1 d . . . N22 N 0.7862(3) 0.1120(3) 0.70239(17) 0.0337(9) Uani 1 1 d . . . C8 C 0.6661(4) 0.0292(3) 0.3191(2) 0.0382(11) Uani 1 1 d . . . H8 H 0.7017 -0.0259 0.3107 0.046 Uiso 1 1 calc R . . N25 N 0.9107(7) 0.7183(5) 0.0095(3) 0.118(3) Uani 1 1 d . . . C9 C 0.5718(3) 0.0512(3) 0.3421(2) 0.0345(10) Uani 1 1 d . . . C6 C 0.8021(4) 0.1097(4) 0.2826(2) 0.0420(12) Uani 1 1 d . . . H6A H 0.7995 0.1283 0.2373 0.063 Uiso 1 1 calc R . . H6B H 0.8542 0.0502 0.2986 0.063 Uiso 1 1 calc R . . H6C H 0.8179 0.1554 0.2942 0.063 Uiso 1 1 calc R . . C10 C 0.4965(4) 0.0019(3) 0.3597(3) 0.0443(12) Uani 1 1 d . . . H10A H 0.5269 -0.0592 0.3561 0.066 Uiso 1 1 calc R . . H10B H 0.4384 0.0362 0.3320 0.066 Uiso 1 1 calc R . . H10C H 0.4743 -0.0038 0.4027 0.066 Uiso 1 1 calc R . . C12 C 0.4323(4) 0.4028(3) 0.2439(2) 0.0351(10) Uani 1 1 d . . . C13 C 0.3421(4) 0.3902(3) 0.2369(2) 0.0385(11) Uani 1 1 d . . . H13 H 0.2920 0.4302 0.2066 0.046 Uiso 1 1 calc R . . C14 C 0.3389(3) 0.3105(3) 0.2811(2) 0.0373(11) Uani 1 1 d . . . C11 C 0.4689(4) 0.4807(3) 0.2063(2) 0.0434(12) Uani 1 1 d . . . H11A H 0.5252 0.4800 0.2276 0.065 Uiso 1 1 calc R . . H11B H 0.4141 0.5385 0.2010 0.065 Uiso 1 1 calc R . . H11C H 0.4914 0.4749 0.1654 0.065 Uiso 1 1 calc R . . C15 C 0.2611(4) 0.2641(4) 0.2964(3) 0.0516(14) Uani 1 1 d . . . H15A H 0.2900 0.2033 0.2921 0.077 Uiso 1 1 calc R . . H15B H 0.2042 0.3005 0.2679 0.077 Uiso 1 1 calc R . . H15C H 0.2376 0.2579 0.3392 0.077 Uiso 1 1 calc R . . C16 C 0.4619(3) 0.1948(3) 0.3645(2) 0.0294(9) Uani 1 1 d . . . H16 H 0.4098 0.1631 0.3755 0.035 Uiso 1 1 calc R . . C67 C 0.1648(5) 0.7059(4) 0.4362(3) 0.0706(18) Uani 1 1 d . . . H67A H 0.1050 0.6955 0.4268 0.106 Uiso 1 1 calc R . . H67B H 0.1721 0.7623 0.4052 0.106 Uiso 1 1 calc R . . H67C H 0.1574 0.7118 0.4776 0.106 Uiso 1 1 calc R . . C68 C 0.2509(5) 0.5516(4) 0.4845(3) 0.0602(15) Uani 1 1 d . . . H68A H 0.1884 0.5372 0.4843 0.072 Uiso 1 1 calc R . . H68B H 0.2542 0.5604 0.5245 0.072 Uiso 1 1 calc R . . C69 C 0.3394(5) 0.4753(5) 0.4778(4) 0.083(2) Uani 1 1 d . . . H69A H 0.4012 0.4905 0.4783 0.099 Uiso 1 1 calc R . . H69B H 0.3417 0.4196 0.5139 0.099 Uiso 1 1 calc R . . C70 C 0.2663(5) 0.4188(5) 0.4191(4) 0.0730(19) Uani 1 1 d . . . H70A H 0.2693 0.3660 0.4568 0.109 Uiso 1 1 calc R . . H70B H 0.2784 0.3989 0.3826 0.109 Uiso 1 1 calc R . . H70C H 0.1997 0.4649 0.4161 0.109 Uiso 1 1 calc R . . C50 C 0.7386(4) 0.0909(4) 0.8960(2) 0.0451(12) Uani 1 1 d . . . H50 H 0.7144 0.0550 0.8808 0.054 Uiso 1 1 calc R . . C51 C 0.7077(4) 0.1090(4) 0.9512(2) 0.0509(14) Uani 1 1 d . . . H51 H 0.6601 0.0877 0.9803 0.061 Uiso 1 1 calc R . . C52 C 0.7580(4) 0.1621(4) 0.9554(2) 0.0437(12) Uani 1 1 d . . . H52 H 0.7528 0.1861 0.9881 0.052 Uiso 1 1 calc R . . C53 C 0.8445(4) 0.3342(3) 0.7272(2) 0.0429(12) Uani 1 1 d . . . H53 H 0.8345 0.3348 0.6870 0.051 Uiso 1 1 calc R . . C54 C 0.8411(4) 0.4108(4) 0.7418(2) 0.0483(13) Uani 1 1 d . . . H54 H 0.8302 0.4714 0.7137 0.058 Uiso 1 1 calc R . . C55 C 0.8564(4) 0.3817(3) 0.8038(2) 0.0399(11) Uani 1 1 d . . . H55 H 0.8577 0.4177 0.8279 0.048 Uiso 1 1 calc R . . C56 C 1.0963(4) 0.0520(3) 0.8530(2) 0.0402(11) Uani 1 1 d . . . H56 H 1.1263 0.0086 0.8322 0.048 Uiso 1 1 calc R . . C57 C 1.1460(4) 0.0652(4) 0.8958(2) 0.0444(12) Uani 1 1 d . . . H57 H 1.2138 0.0337 0.9091 0.053 Uiso 1 1 calc R . . C58 C 1.0774(4) 0.1325(3) 0.9145(2) 0.0411(11) Uani 1 1 d . . . H58 H 1.0882 0.1575 0.9436 0.049 Uiso 1 1 calc R . . C59 C 0.8925(3) 0.2237(3) 0.8862(2) 0.0333(10) Uani 1 1 d . . . C60 C 0.8954(4) 0.2695(3) 0.9325(2) 0.0400(11) Uani 1 1 d . . . H60A H 0.9136 0.2232 0.9742 0.048 Uiso 1 1 calc R . . H60B H 0.9461 0.3019 0.9195 0.048 Uiso 1 1 calc R . . C61 C 0.7907(4) 0.3682(3) 0.9836(2) 0.0378(11) Uani 1 1 d . . . H61A H 0.8383 0.4031 0.9769 0.045 Uiso 1 1 calc R . . H61B H 0.8059 0.3181 1.0240 0.045 Uiso 1 1 calc R . . C62 C 0.6848(4) 0.4295(3) 0.9829(2) 0.0349(10) Uani 1 1 d . . . C63 C 0.6566(4) 0.5186(3) 0.9396(2) 0.0392(11) Uani 1 1 d . . . H63 H 0.7055 0.5402 0.9121 0.047 Uiso 1 1 calc R . . C64 C 0.5593(4) 0.5742(3) 0.9371(2) 0.0389(11) Uani 1 1 d . . . H64 H 0.5411 0.6340 0.9073 0.047 Uiso 1 1 calc R . . C65 C 0.5147(3) 0.4549(3) 1.0224(2) 0.0328(10) Uani 1 1 d . . . C66 C 0.6151(4) 0.3994(3) 1.0230(2) 0.0355(10) Uani 1 1 d . . . H66 H 0.6351 0.3391 1.0523 0.043 Uiso 1 1 calc R . . C45 C 0.9436(4) -0.0790(3) 0.8548(2) 0.0437(12) Uani 1 1 d . . . C46 C 0.9525(4) -0.1511(3) 0.8341(3) 0.0502(13) Uani 1 1 d . . . H46 H 0.9708 -0.2141 0.8586 0.060 Uiso 1 1 calc R . . C47 C 0.9306(4) -0.1154(3) 0.7725(2) 0.0402(11) Uani 1 1 d . . . C44 C 0.9629(5) -0.0854(4) 0.9187(2) 0.0601(16) Uani 1 1 d . . . H44A H 1.0356 -0.1090 0.9261 0.090 Uiso 1 1 calc R . . H44B H 0.9305 -0.1270 0.9491 0.090 Uiso 1 1 calc R . . H44C H 0.9353 -0.0246 0.9230 0.090 Uiso 1 1 calc R . . C48 C 0.9269(4) -0.1583(4) 0.7262(3) 0.0505(13) Uani 1 1 d . . . H48A H 0.8590 -0.1334 0.7089 0.076 Uiso 1 1 calc R . . H48B H 0.9439 -0.2247 0.7465 0.076 Uiso 1 1 calc R . . H48C H 0.9755 -0.1451 0.6928 0.076 Uiso 1 1 calc R . . C40 C 1.0504(4) 0.1667(3) 0.6932(2) 0.0360(10) Uani 1 1 d . . . C41 C 1.0798(4) 0.1472(3) 0.6384(2) 0.0406(11) Uani 1 1 d . . . H41 H 1.1314 0.1634 0.6109 0.049 Uiso 1 1 calc R . . C42 C 1.0213(4) 0.1006(3) 0.6313(2) 0.0391(11) Uani 1 1 d . . . C39 C 1.0922(4) 0.2169(4) 0.7201(3) 0.0488(13) Uani 1 1 d . . . H39A H 1.0477 0.2329 0.7535 0.073 Uiso 1 1 calc R . . H39B H 1.0974 0.2730 0.6877 0.073 Uiso 1 1 calc R . . H39C H 1.1592 0.1781 0.7370 0.073 Uiso 1 1 calc R . . C43 C 1.0173(5) 0.0634(4) 0.5819(2) 0.0547(15) Uani 1 1 d . . . H43A H 1.0257 -0.0021 0.6004 0.082 Uiso 1 1 calc R . . H43B H 1.0715 0.0722 0.5516 0.082 Uiso 1 1 calc R . . H43C H 0.9521 0.0956 0.5609 0.082 Uiso 1 1 calc R . . C35 C 0.6765(4) 0.2128(3) 0.7363(2) 0.0431(12) Uani 1 1 d . . . C36 C 0.6319(4) 0.2005(3) 0.6907(3) 0.0470(13) Uani 1 1 d . . . H36 H 0.5644 0.2314 0.6767 0.056 Uiso 1 1 calc R . . C37 C 0.7016(3) 0.1365(3) 0.6696(2) 0.0379(11) Uani 1 1 d . . . C34 C 0.6299(4) 0.2765(5) 0.7713(3) 0.0702(19) Uani 1 1 d . . . H34A H 0.5785 0.2559 0.7997 0.105 Uiso 1 1 calc R . . H34B H 0.5985 0.3381 0.7423 0.105 Uiso 1 1 calc R . . H34C H 0.6817 0.2780 0.7952 0.105 Uiso 1 1 calc R . . C38 C 0.6975(4) 0.0970(4) 0.6219(3) 0.0487(13) Uani 1 1 d . . . H38A H 0.7496 0.1072 0.5903 0.073 Uiso 1 1 calc R . . H38B H 0.6311 0.1264 0.6022 0.073 Uiso 1 1 calc R . . H38C H 0.7090 0.0311 0.6414 0.073 Uiso 1 1 calc R . . C49 C 0.8834(3) 0.0474(3) 0.6996(2) 0.0326(10) Uani 1 1 d . . . H49 H 0.8817 0.0195 0.6678 0.039 Uiso 1 1 calc R . . C71 C 0.4428(9) 0.3470(10) 0.9365(5) 0.145(5) Uani 1 1 d . . . H71A H 0.5071 0.3090 0.9247 0.217 Uiso 1 1 calc R . . H71B H 0.4393 0.3314 0.9818 0.217 Uiso 1 1 calc R . . H71C H 0.4377 0.4118 0.9172 0.217 Uiso 1 1 calc R . . C72 C 0.3727(6) 0.3399(7) 0.8537(4) 0.101(3) Uani 1 1 d . . . H72A H 0.4400 0.3001 0.8459 0.121 Uiso 1 1 calc R . . H72B H 0.3673 0.4040 0.8286 0.121 Uiso 1 1 calc R . . C73 C 0.2951(6) 0.3146(6) 0.8341(4) 0.086(2) Uani 1 1 d . . . H73A H 0.3147 0.3040 0.7938 0.103 Uiso 1 1 calc R . . H73B H 0.2887 0.2571 0.8652 0.103 Uiso 1 1 calc R . . C74 C 0.1247(6) 0.3541(5) 0.8207(3) 0.075(2) Uani 1 1 d . . . H74A H 0.1358 0.3379 0.7827 0.113 Uiso 1 1 calc R . . H74B H 0.0608 0.4039 0.8175 0.113 Uiso 1 1 calc R . . H74C H 0.1221 0.3006 0.8565 0.113 Uiso 1 1 calc R . . C75 C 0.8884(6) 0.6561(5) 0.0134(3) 0.0707(19) Uani 1 1 d . . . C76 C 0.8563(5) 0.5802(5) 0.0207(3) 0.0727(19) Uani 1 1 d . . . H76A H 0.8405 0.5820 -0.0201 0.109 Uiso 1 1 calc R . . H76B H 0.7961 0.5830 0.0472 0.109 Uiso 1 1 calc R . . H76C H 0.9101 0.5232 0.0399 0.109 Uiso 1 1 calc R . . N26 N 0.3174(6) 0.0643(6) 0.2302(4) 0.127(3) Uani 1 1 d D . . C80 C 0.3517(12) 0.1891(8) 0.1302(8) 0.264(12) Uani 1 1 d D . . H80A H 0.4205 0.1907 0.1297 0.397 Uiso 1 1 calc R . . H80B H 0.3037 0.2497 0.1269 0.397 Uiso 1 1 calc R . . H80C H 0.3429 0.1720 0.0950 0.397 Uiso 1 1 calc R . . C79 C 0.3338(9) 0.1216(7) 0.1884(5) 0.141(5) Uani 1 1 d D . . Fe1 Fe 0.61715(5) 0.28918(4) 0.33165(3) 0.02769(18) Uani 1 1 d . . . Fe2 Fe 0.88906(5) 0.13176(4) 0.79379(3) 0.02943(18) Uani 1 1 d . . . C82 C 0.4765(14) 0.0810(15) 0.8293(10) 0.098(6) Uani 0.50 1 d P . . N27 N 0.5120(14) 0.0873(14) 0.8628(9) 0.124(6) Uani 0.50 1 d P . . C81 C 0.4329(16) 0.0684(14) 0.7928(9) 0.108(6) Uani 0.50 1 d P . . H81A H 0.4595 0.0039 0.7955 0.162 Uiso 0.50 1 calc PR . . H81B H 0.4430 0.1071 0.7505 0.162 Uiso 0.50 1 calc PR . . H81C H 0.3608 0.0842 0.8027 0.162 Uiso 0.50 1 calc PR . . 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 F1 0.069(2) 0.070(2) 0.082(2) -0.0516(19) 0.0250(18) -0.0398(18) O1 0.049(2) 0.061(2) 0.0332(17) -0.0209(16) 0.0035(15) -0.0369(18) N2 0.039(2) 0.029(2) 0.0287(19) -0.0081(16) -0.0022(16) -0.0180(17) C17 0.042(3) 0.030(2) 0.035(2) -0.011(2) -0.002(2) -0.012(2) B1 0.042(4) 0.056(4) 0.081(5) -0.047(4) 0.002(3) -0.015(3) F2 0.051(2) 0.131(3) 0.081(2) -0.066(2) 0.0092(18) -0.041(2) O3 0.067(3) 0.054(2) 0.066(3) -0.015(2) 0.004(2) -0.025(2) N4 0.033(2) 0.033(2) 0.0307(19) -0.0134(17) 0.0024(16) -0.0150(17) C18 0.060(3) 0.028(2) 0.041(3) -0.013(2) -0.013(2) -0.010(2) B2 0.046(4) 0.061(4) 0.046(4) -0.004(3) -0.002(3) -0.022(3) F3 0.141(6) 0.062(4) 0.460(15) -0.087(6) 0.118(8) -0.030(4) O4 0.064(3) 0.087(3) 0.105(4) -0.050(3) 0.026(3) -0.031(3) N6 0.036(2) 0.037(2) 0.0309(19) -0.0136(16) -0.0029(16) -0.0188(17) C19 0.060(3) 0.031(3) 0.036(3) -0.008(2) -0.010(2) -0.022(2) B3 0.044(3) 0.046(4) 0.049(3) -0.020(3) 0.003(3) -0.021(3) F4 0.061(3) 0.393(12) 0.187(6) -0.235(8) 0.035(3) -0.074(5) O2 0.0369(18) 0.0410(19) 0.0393(18) -0.0244(15) -0.0029(14) -0.0011(15) N1 0.043(2) 0.033(2) 0.0309(19) -0.0109(16) 0.0015(17) -0.0238(18) C20 0.038(3) 0.037(3) 0.035(2) -0.017(2) 0.000(2) -0.011(2) B4 0.050(4) 0.040(3) 0.039(3) -0.014(3) 0.000(3) -0.012(3) F5 0.114(4) 0.144(4) 0.043(2) -0.001(2) 0.019(2) 0.039(3) O5 0.103(4) 0.146(5) 0.076(3) -0.053(3) 0.012(3) -0.070(4) N3 0.032(2) 0.037(2) 0.0303(19) -0.0147(17) 0.0013(16) -0.0186(17) C21 0.038(3) 0.046(3) 0.033(2) -0.018(2) -0.006(2) -0.008(2) F6 0.128(4) 0.086(3) 0.075(3) -0.031(2) 0.030(2) -0.065(3) O6 0.065(3) 0.058(3) 0.079(3) -0.023(2) -0.009(2) -0.020(2) N5 0.044(2) 0.048(2) 0.0274(19) -0.0161(17) 0.0023(17) -0.026(2) C22 0.031(2) 0.052(3) 0.035(2) -0.024(2) -0.001(2) -0.014(2) F7 0.066(2) 0.114(3) 0.074(3) -0.033(2) 0.007(2) -0.001(2) N7 0.0288(19) 0.0284(19) 0.034(2) -0.0112(16) -0.0004(15) -0.0148(16) C23 0.050(3) 0.050(3) 0.033(2) -0.021(2) -0.005(2) -0.023(2) F8 0.071(3) 0.122(4) 0.198(6) -0.040(4) -0.006(3) -0.053(3) N9 0.0265(19) 0.035(2) 0.037(2) -0.0174(17) 0.0004(16) -0.0136(17) C24 0.068(4) 0.084(4) 0.033(3) -0.028(3) 0.010(3) -0.044(3) F9 0.053(2) 0.079(3) 0.128(3) -0.062(2) 0.008(2) -0.0311(19) N11 0.038(2) 0.030(2) 0.035(2) -0.0130(17) 0.0002(17) -0.0165(17) C25 0.057(3) 0.076(4) 0.035(3) -0.022(3) 0.008(2) -0.042(3) F10 0.0500(19) 0.0425(18) 0.094(3) -0.0289(17) 0.0044(17) -0.0124(15) N8 0.031(2) 0.0287(19) 0.0303(19) -0.0103(15) -0.0012(15) -0.0123(16) C26 0.041(3) 0.044(3) 0.027(2) -0.015(2) 0.0003(19) -0.025(2) F11 0.080(3) 0.072(2) 0.066(2) 0.0062(19) -0.0057(19) -0.035(2) N10 0.0279(19) 0.030(2) 0.037(2) -0.0128(16) -0.0028(16) -0.0123(16) C27 0.047(3) 0.056(3) 0.032(2) -0.016(2) 0.002(2) -0.035(3) F12 0.060(2) 0.068(2) 0.071(2) -0.0400(18) 0.0217(17) -0.0356(17) N12 0.031(2) 0.029(2) 0.034(2) -0.0101(16) -0.0051(16) -0.0098(16) C28 0.063(4) 0.083(4) 0.046(3) -0.031(3) 0.011(3) -0.054(3) F13 0.065(2) 0.061(2) 0.080(2) -0.0224(18) 0.0058(18) -0.0238(18) N18 0.037(2) 0.037(2) 0.036(2) -0.0178(18) 0.0037(17) -0.0098(18) C29 0.043(3) 0.056(3) 0.038(3) -0.018(2) 0.003(2) -0.034(3) F14 0.091(3) 0.153(4) 0.077(3) -0.075(3) 0.007(2) -0.054(3) N16 0.038(2) 0.033(2) 0.0293(19) -0.0132(17) -0.0029(16) -0.0073(17) C30 0.040(3) 0.046(3) 0.038(3) -0.009(2) -0.009(2) -0.023(2) F15 0.073(2) 0.064(2) 0.070(2) -0.0043(19) 0.0182(19) 0.0053(19) N14 0.033(2) 0.033(2) 0.033(2) -0.0152(17) -0.0013(16) -0.0052(17) C31 0.034(3) 0.036(2) 0.037(2) -0.0107(19) 0.000(2) -0.020(2) F16 0.056(2) 0.052(2) 0.089(2) -0.0392(18) 0.0008(18) -0.0053(16) N17 0.036(2) 0.037(2) 0.034(2) -0.0185(17) 0.0027(17) -0.0059(18) C32 0.052(3) 0.048(3) 0.055(3) -0.027(3) 0.006(3) -0.025(3) N15 0.036(2) 0.029(2) 0.0313(19) -0.0125(16) -0.0025(16) -0.0055(17) C33 0.052(3) 0.036(3) 0.049(3) -0.010(2) -0.006(2) -0.016(2) N13 0.032(2) 0.037(2) 0.0306(19) -0.0170(17) -0.0051(16) -0.0004(17) C2 0.031(2) 0.028(2) 0.034(2) -0.0115(19) -0.0046(19) -0.0073(19) N23 0.038(2) 0.032(2) 0.032(2) -0.0122(17) -0.0004(17) -0.0082(17) C3 0.034(3) 0.041(3) 0.029(2) -0.013(2) -0.0030(19) -0.011(2) N19 0.032(2) 0.036(2) 0.0296(19) -0.0156(16) 0.0023(16) -0.0109(17) C4 0.030(2) 0.033(2) 0.035(2) -0.010(2) -0.0008(19) -0.010(2) N21 0.030(2) 0.035(2) 0.036(2) -0.0149(17) -0.0039(16) -0.0047(17) C1 0.043(3) 0.043(3) 0.036(3) -0.015(2) -0.005(2) -0.018(2) N24 0.032(2) 0.033(2) 0.035(2) -0.0163(17) 0.0016(16) -0.0098(17) C5 0.040(3) 0.052(3) 0.043(3) -0.016(2) 0.000(2) -0.025(2) N20 0.035(2) 0.037(2) 0.0281(19) -0.0163(16) 0.0002(16) -0.0128(17) C7 0.031(2) 0.038(3) 0.037(2) -0.018(2) -0.003(2) -0.010(2) N22 0.034(2) 0.034(2) 0.034(2) -0.0141(17) -0.0038(17) -0.0086(17) C8 0.042(3) 0.030(2) 0.048(3) -0.019(2) 0.002(2) -0.012(2) N25 0.162(7) 0.098(5) 0.105(5) 0.012(4) -0.064(5) -0.082(5) C9 0.036(3) 0.027(2) 0.046(3) -0.017(2) -0.004(2) -0.009(2) C6 0.037(3) 0.043(3) 0.054(3) -0.026(2) 0.004(2) -0.014(2) C10 0.046(3) 0.034(3) 0.061(3) -0.021(2) 0.003(2) -0.019(2) C12 0.042(3) 0.027(2) 0.034(2) -0.009(2) -0.006(2) -0.007(2) C13 0.033(3) 0.039(3) 0.042(3) -0.010(2) -0.012(2) -0.007(2) C14 0.032(3) 0.040(3) 0.041(3) -0.015(2) -0.007(2) -0.008(2) C11 0.052(3) 0.034(3) 0.043(3) -0.007(2) -0.010(2) -0.016(2) C15 0.038(3) 0.058(3) 0.064(3) -0.014(3) -0.012(3) -0.023(3) C16 0.030(2) 0.028(2) 0.035(2) -0.0122(19) -0.0041(19) -0.0122(19) C67 0.067(4) 0.051(4) 0.089(5) -0.016(3) -0.021(4) -0.013(3) C68 0.069(4) 0.054(4) 0.057(4) -0.013(3) -0.006(3) -0.023(3) C69 0.063(4) 0.067(5) 0.119(6) -0.034(4) -0.023(4) -0.009(4) C70 0.051(4) 0.064(4) 0.102(5) -0.029(4) -0.008(4) -0.013(3) C50 0.043(3) 0.049(3) 0.045(3) -0.020(2) 0.012(2) -0.016(2) C51 0.059(3) 0.056(3) 0.045(3) -0.023(3) 0.020(3) -0.029(3) C52 0.047(3) 0.050(3) 0.036(3) -0.022(2) 0.012(2) -0.014(3) C53 0.057(3) 0.035(3) 0.031(3) -0.011(2) -0.005(2) -0.007(2) C54 0.060(3) 0.035(3) 0.044(3) -0.008(2) -0.004(3) -0.012(3) C55 0.043(3) 0.029(3) 0.043(3) -0.012(2) 0.000(2) -0.007(2) C56 0.037(3) 0.035(3) 0.043(3) -0.017(2) -0.004(2) 0.002(2) C57 0.034(3) 0.050(3) 0.047(3) -0.024(2) -0.009(2) 0.001(2) C58 0.042(3) 0.048(3) 0.035(3) -0.019(2) -0.007(2) -0.008(2) C59 0.030(2) 0.032(2) 0.032(2) -0.014(2) -0.0017(19) 0.000(2) C60 0.037(3) 0.043(3) 0.041(3) -0.025(2) 0.000(2) -0.002(2) C61 0.039(3) 0.045(3) 0.038(3) -0.025(2) 0.005(2) -0.014(2) C62 0.038(3) 0.041(3) 0.032(2) -0.023(2) 0.000(2) -0.008(2) C63 0.039(3) 0.047(3) 0.038(3) -0.021(2) 0.009(2) -0.016(2) C64 0.047(3) 0.034(3) 0.036(3) -0.013(2) 0.002(2) -0.013(2) C65 0.037(3) 0.036(2) 0.031(2) -0.0198(19) 0.0010(19) -0.010(2) C66 0.043(3) 0.034(3) 0.033(2) -0.019(2) 0.000(2) -0.009(2) C45 0.052(3) 0.035(3) 0.038(3) -0.008(2) -0.001(2) -0.011(2) C46 0.059(3) 0.029(3) 0.055(3) -0.012(2) 0.001(3) -0.007(2) C47 0.038(3) 0.032(3) 0.052(3) -0.017(2) 0.003(2) -0.012(2) C44 0.084(4) 0.049(3) 0.037(3) -0.004(3) -0.004(3) -0.018(3) C48 0.056(3) 0.041(3) 0.063(3) -0.027(3) 0.003(3) -0.019(3) C40 0.035(3) 0.038(3) 0.032(2) -0.008(2) -0.001(2) -0.012(2) C41 0.037(3) 0.046(3) 0.038(3) -0.010(2) 0.009(2) -0.020(2) C42 0.041(3) 0.044(3) 0.032(2) -0.014(2) 0.001(2) -0.011(2) C39 0.054(3) 0.051(3) 0.053(3) -0.020(3) 0.004(3) -0.028(3) C43 0.062(4) 0.080(4) 0.039(3) -0.033(3) 0.012(3) -0.033(3) C35 0.031(3) 0.044(3) 0.050(3) -0.020(2) -0.007(2) 0.000(2) C36 0.031(3) 0.041(3) 0.066(3) -0.014(3) -0.013(2) -0.007(2) C37 0.030(2) 0.038(3) 0.045(3) -0.012(2) -0.009(2) -0.010(2) C34 0.040(3) 0.075(4) 0.095(5) -0.053(4) -0.009(3) 0.011(3) C38 0.045(3) 0.047(3) 0.058(3) -0.017(3) -0.021(3) -0.013(2) C49 0.034(2) 0.033(2) 0.034(2) -0.016(2) 0.0023(19) -0.011(2) C71 0.154(10) 0.248(14) 0.107(7) -0.078(8) 0.007(7) -0.139(10) C72 0.073(5) 0.151(8) 0.083(6) -0.047(6) 0.024(4) -0.039(5) C73 0.076(5) 0.102(6) 0.081(5) -0.052(5) -0.019(4) -0.002(4) C74 0.094(5) 0.079(5) 0.070(4) -0.021(4) -0.005(4) -0.050(4) C75 0.085(5) 0.072(4) 0.060(4) -0.004(3) -0.027(3) -0.040(4) C76 0.079(5) 0.078(5) 0.076(4) -0.032(4) 0.011(4) -0.041(4) N26 0.093(6) 0.129(7) 0.138(7) -0.026(6) 0.012(5) -0.034(5) C80 0.207(16) 0.099(9) 0.32(2) 0.021(11) 0.139(16) 0.012(10) C79 0.134(9) 0.113(9) 0.153(10) -0.034(8) 0.063(8) -0.043(7) Fe1 0.0297(3) 0.0285(3) 0.0300(3) -0.0116(3) -0.0013(3) -0.0133(3) Fe2 0.0308(4) 0.0291(4) 0.0269(3) -0.0115(3) -0.0002(3) -0.0056(3) C82 0.069(11) 0.135(16) 0.102(15) -0.035(13) -0.001(10) -0.052(11) N27 0.097(12) 0.161(17) 0.141(16) -0.075(13) -0.006(11) -0.044(12) C81 0.113(15) 0.110(15) 0.098(13) -0.035(11) 0.023(12) -0.041(12) _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 F1 B1 1.347(7) . ? O1 C27 1.400(5) . ? O1 C28 1.429(6) . ? N2 C17 1.321(6) . ? N2 N1 1.364(5) . ? N2 Fe1 1.946(3) . ? C17 C18 1.389(7) . ? C17 H17 0.9500 . ? B1 F4 1.277(8) . ? B1 F3 1.331(10) . ? B1 F2 1.335(7) . ? O3 C67 1.388(7) . ? O3 C68 1.414(7) . ? N4 C20 1.323(6) . ? N4 N3 1.357(5) . ? N4 Fe1 1.933(4) . ? C18 C19 1.355(7) . ? C18 H18 0.9500 . ? B2 F8 1.322(8) . ? B2 F5 1.347(8) . ? B2 F6 1.353(8) . ? B2 F7 1.378(8) . ? O4 C70 1.373(8) . ? O4 C69 1.435(9) . ? N6 C23 1.314(6) . ? N6 N5 1.378(5) . ? N6 Fe1 1.943(4) . ? C19 N1 1.363(6) . ? C19 H19 0.9500 . ? B3 F10 1.357(7) . ? B3 F9 1.364(7) . ? B3 F12 1.379(7) . ? B3 F11 1.382(7) . ? O2 C60 1.399(5) . ? O2 C61 1.437(5) . ? N1 C26 1.447(6) . ? C20 C21 1.404(7) . ? C20 H20 0.9500 . ? B4 F15 1.355(7) . ? B4 F14 1.369(7) . ? B4 F16 1.377(7) . ? B4 F13 1.378(7) . ? O5 C72 1.390(9) . ? O5 C71 1.398(9) . ? N3 C22 1.353(6) . ? N3 C26 1.451(6) . ? C21 C22 1.341(7) . ? C21 H21 0.9500 . ? O6 C73 1.371(8) . ? O6 C74 1.419(7) . ? N5 C25 1.348(6) . ? N5 C26 1.454(5) . ? C22 H22 0.9500 . ? N7 C2 1.331(5) . ? N7 N8 1.373(5) . ? N7 Fe1 1.973(3) . ? C23 C24 1.397(7) . ? C23 H23 0.9500 . ? N9 C7 1.323(6) . ? N9 N10 1.372(5) . ? N9 Fe1 1.979(3) . ? C24 C25 1.362(7) . ? C24 H24 0.9500 . ? N11 C12 1.335(6) . ? N11 N12 1.376(5) . ? N11 Fe1 1.982(4) . ? C25 H25 0.9500 . ? N8 C4 1.359(6) . ? N8 C16 1.431(5) . ? C26 C27 1.520(6) . ? N10 C9 1.360(5) . ? N10 C16 1.435(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N12 C14 1.358(6) . ? N12 C16 1.429(6) . ? C28 C29 1.493(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? N18 C50 1.314(6) . ? N18 N17 1.354(5) . ? N18 Fe2 1.940(4) . ? C29 C30 1.352(7) . ? C29 C32 1.397(8) . ? N16 C53 1.309(6) . ? N16 N15 1.354(5) . ? N16 Fe2 1.944(4) . ? C30 C31 1.399(6) . ? C30 H30 0.9500 . ? N14 C56 1.328(6) . ? N14 N13 1.374(5) . ? N14 Fe2 1.944(4) . ? C31 C33 1.400(7) 2_766 ? C31 C31 1.409(9) 2_766 ? N17 C52 1.357(6) . ? N17 C59 1.462(6) . ? C32 C33 1.359(7) . ? C32 H32 0.9500 . ? N15 C55 1.355(6) . ? N15 C59 1.452(6) . ? C33 C31 1.400(7) 2_766 ? C33 H33 0.9500 . ? N13 C58 1.356(6) . ? N13 C59 1.457(6) . ? C2 C3 1.388(6) . ? C2 C1 1.506(6) . ? N23 C45 1.331(6) . ? N23 N24 1.376(5) . ? N23 Fe2 1.975(4) . ? C3 C4 1.367(6) . ? C3 H3 0.9500 . ? N19 C40 1.338(6) . ? N19 N20 1.360(5) . ? N19 Fe2 1.965(3) . ? C4 C5 1.473(6) . ? N21 C35 1.340(6) . ? N21 N22 1.373(5) . ? N21 Fe2 1.965(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N24 C47 1.359(6) . ? N24 C49 1.421(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N20 C42 1.360(6) . ? N20 C49 1.439(6) . ? C7 C8 1.398(6) . ? C7 C6 1.497(6) . ? N22 C37 1.357(6) . ? N22 C49 1.432(6) . ? C8 C9 1.347(7) . ? C8 H8 0.9500 . ? N25 C75 1.142(8) . ? C9 C10 1.485(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.396(7) . ? C12 C11 1.489(7) . ? C13 C14 1.358(7) . ? C13 H13 0.9500 . ? C14 C15 1.485(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.477(9) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C50 C51 1.390(7) . ? C50 H50 0.9500 . ? C51 C52 1.335(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.400(7) . ? C53 H53 0.9500 . ? C54 C55 1.354(7) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.391(7) . ? C56 H56 0.9500 . ? C57 C58 1.362(7) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.518(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.491(7) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C66 1.359(7) . ? C62 C63 1.405(7) . ? C63 C64 1.362(7) . ? C63 H63 0.9500 . ? C64 C65 1.403(6) 2_667 ? C64 H64 0.9500 . ? C65 C66 1.401(6) . ? C65 C64 1.403(6) 2_667 ? C65 C65 1.430(9) 2_667 ? C66 H66 0.9500 . ? C45 C46 1.391(7) . ? C45 C44 1.490(7) . ? C46 C47 1.359(7) . ? C46 H46 0.9500 . ? C47 C48 1.485(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C40 C41 1.388(7) . ? C40 C39 1.485(7) . ? C41 C42 1.360(7) . ? C41 H41 0.9500 . ? C42 C43 1.483(7) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C35 C36 1.393(7) . ? C35 C34 1.475(7) . ? C36 C37 1.360(7) . ? C36 H36 0.9500 . ? C37 C38 1.475(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C49 H49 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.464(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.420(9) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? N26 C79 1.148(8) . ? C80 C79 1.467(9) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C82 N27 1.02(2) . ? C82 C81 1.21(2) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? 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 C27 O1 C28 112.3(3) . . ? C17 N2 N1 105.7(3) . . ? C17 N2 Fe1 135.6(3) . . ? N1 N2 Fe1 118.7(3) . . ? N2 C17 C18 110.6(4) . . ? N2 C17 H17 124.7 . . ? C18 C17 H17 124.7 . . ? F4 B1 F3 95.3(7) . . ? F4 B1 F2 117.1(6) . . ? F3 B1 F2 106.9(6) . . ? F4 B1 F1 113.3(6) . . ? F3 B1 F1 108.0(7) . . ? F2 B1 F1 113.9(5) . . ? C67 O3 C68 112.3(5) . . ? C20 N4 N3 105.8(4) . . ? C20 N4 Fe1 133.9(3) . . ? N3 N4 Fe1 120.2(3) . . ? C19 C18 C17 106.5(4) . . ? C19 C18 H18 126.7 . . ? C17 C18 H18 126.7 . . ? F8 B2 F5 109.1(6) . . ? F8 B2 F6 110.5(6) . . ? F5 B2 F6 110.7(6) . . ? F8 B2 F7 109.9(6) . . ? F5 B2 F7 110.1(5) . . ? F6 B2 F7 106.5(5) . . ? C70 O4 C69 115.5(6) . . ? C23 N6 N5 105.4(4) . . ? C23 N6 Fe1 136.5(3) . . ? N5 N6 Fe1 118.1(3) . . ? C18 C19 N1 106.6(4) . . ? C18 C19 H19 126.7 . . ? N1 C19 H19 126.7 . . ? F10 B3 F9 110.7(5) . . ? F10 B3 F12 110.4(4) . . ? F9 B3 F12 113.0(5) . . ? F10 B3 F11 109.1(5) . . ? F9 B3 F11 107.9(5) . . ? F12 B3 F11 105.5(5) . . ? C60 O2 C61 111.3(3) . . ? C19 N1 N2 110.5(4) . . ? C19 N1 C26 130.9(4) . . ? N2 N1 C26 118.6(3) . . ? N4 C20 C21 109.9(4) . . ? N4 C20 H20 125.1 . . ? C21 C20 H20 125.1 . . ? F15 B4 F14 109.1(5) . . ? F15 B4 F16 109.6(5) . . ? F14 B4 F16 109.4(5) . . ? F15 B4 F13 108.6(5) . . ? F14 B4 F13 108.6(5) . . ? F16 B4 F13 111.4(5) . . ? C72 O5 C71 112.0(7) . . ? C22 N3 N4 110.8(4) . . ? C22 N3 C26 131.7(4) . . ? N4 N3 C26 117.5(3) . . ? C22 C21 C20 106.3(4) . . ? C22 C21 H21 126.8 . . ? C20 C21 H21 126.8 . . ? C73 O6 C74 111.1(6) . . ? C25 N5 N6 110.7(4) . . ? C25 N5 C26 130.5(4) . . ? N6 N5 C26 118.7(3) . . ? C21 C22 N3 107.3(4) . . ? C21 C22 H22 126.4 . . ? N3 C22 H22 126.4 . . ? C2 N7 N8 105.1(3) . . ? C2 N7 Fe1 138.1(3) . . ? N8 N7 Fe1 116.8(3) . . ? N6 C23 C24 110.9(4) . . ? N6 C23 H23 124.5 . . ? C24 C23 H23 124.5 . . ? C7 N9 N10 104.9(3) . . ? C7 N9 Fe1 138.6(3) . . ? N10 N9 Fe1 116.5(3) . . ? C25 C24 C23 105.9(4) . . ? C25 C24 H24 127.0 . . ? C23 C24 H24 127.0 . . ? C12 N11 N12 104.5(4) . . ? C12 N11 Fe1 139.3(3) . . ? N12 N11 Fe1 116.1(3) . . ? N5 C25 C24 107.0(4) . . ? N5 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? C4 N8 N7 111.5(3) . . ? C4 N8 C16 130.5(4) . . ? N7 N8 C16 118.0(3) . . ? N1 C26 N3 109.1(3) . . ? N1 C26 N5 108.4(4) . . ? N3 C26 N5 108.4(3) . . ? N1 C26 C27 111.1(4) . . ? N3 C26 C27 110.3(4) . . ? N5 C26 C27 109.5(3) . . ? C9 N10 N9 111.8(3) . . ? C9 N10 C16 130.0(4) . . ? N9 N10 C16 118.1(3) . . ? O1 C27 C26 107.7(3) . . ? O1 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O1 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C14 N12 N11 112.2(4) . . ? C14 N12 C16 129.2(4) . . ? N11 N12 C16 118.6(3) . . ? O1 C28 C29 108.0(4) . . ? O1 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? O1 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C50 N18 N17 105.9(4) . . ? C50 N18 Fe2 135.0(3) . . ? N17 N18 Fe2 119.0(3) . . ? C30 C29 C32 119.3(5) . . ? C30 C29 C28 120.8(5) . . ? C32 C29 C28 119.8(5) . . ? C53 N16 N15 106.2(4) . . ? C53 N16 Fe2 134.6(3) . . ? N15 N16 Fe2 119.2(3) . . ? C29 C30 C31 122.0(5) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C56 N14 N13 104.4(4) . . ? C56 N14 Fe2 136.2(3) . . ? N13 N14 Fe2 119.4(3) . . ? C30 C31 C33 123.1(5) . 2_766 ? C30 C31 C31 118.7(5) . 2_766 ? C33 C31 C31 118.2(5) 2_766 2_766 ? N18 N17 C52 110.1(4) . . ? N18 N17 C59 118.8(3) . . ? C52 N17 C59 131.0(4) . . ? C33 C32 C29 120.2(5) . . ? C33 C32 H32 119.9 . . ? C29 C32 H32 119.9 . . ? N16 N15 C55 111.2(4) . . ? N16 N15 C59 118.6(3) . . ? C55 N15 C59 130.2(4) . . ? C32 C33 C31 121.6(5) . 2_766 ? C32 C33 H33 119.2 . . ? C31 C33 H33 119.2 2_766 . ? C58 N13 N14 111.3(4) . . ? C58 N13 C59 131.3(4) . . ? N14 N13 C59 117.4(3) . . ? N7 C2 C3 110.5(4) . . ? N7 C2 C1 123.6(4) . . ? C3 C2 C1 125.9(4) . . ? C45 N23 N24 104.5(4) . . ? C45 N23 Fe2 138.7(3) . . ? N24 N23 Fe2 116.8(3) . . ? C4 C3 C2 107.1(4) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C40 N19 N20 105.8(3) . . ? C40 N19 Fe2 137.0(3) . . ? N20 N19 Fe2 117.2(3) . . ? N8 C4 C3 105.8(4) . . ? N8 C4 C5 122.9(4) . . ? C3 C4 C5 131.3(4) . . ? C35 N21 N22 104.8(4) . . ? C35 N21 Fe2 138.0(3) . . ? N22 N21 Fe2 117.2(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C47 N24 N23 112.2(4) . . ? C47 N24 C49 129.8(4) . . ? N23 N24 C49 118.0(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N19 N20 C42 111.4(4) . . ? N19 N20 C49 118.2(3) . . ? C42 N20 C49 130.4(4) . . ? N9 C7 C8 110.1(4) . . ? N9 C7 C6 123.3(4) . . ? C8 C7 C6 126.5(4) . . ? C37 N22 N21 112.3(4) . . ? C37 N22 C49 129.9(4) . . ? N21 N22 C49 117.8(4) . . ? C9 C8 C7 107.6(4) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 N10 105.6(4) . . ? C8 C9 C10 131.9(4) . . ? N10 C9 C10 122.5(4) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N11 C12 C13 110.3(4) . . ? N11 C12 C11 122.5(4) . . ? C13 C12 C11 127.2(4) . . ? C14 C13 C12 107.6(4) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? C13 C14 N12 105.4(4) . . ? C13 C14 C15 131.4(5) . . ? N12 C14 C15 123.1(4) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N12 C16 N8 110.4(3) . . ? N12 C16 N10 110.1(3) . . ? N8 C16 N10 111.0(3) . . ? N12 C16 H16 108.4 . . ? N8 C16 H16 108.4 . . ? N10 C16 H16 108.4 . . ? O3 C67 H67A 109.5 . . ? O3 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O3 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O3 C68 C69 109.4(6) . . ? O3 C68 H68A 109.8 . . ? C69 C68 H68A 109.8 . . ? O3 C68 H68B 109.8 . . ? C69 C68 H68B 109.8 . . ? H68A C68 H68B 108.2 . . ? O4 C69 C68 113.4(6) . . ? O4 C69 H69A 108.9 . . ? C68 C69 H69A 108.9 . . ? O4 C69 H69B 108.9 . . ? C68 C69 H69B 108.9 . . ? H69A C69 H69B 107.7 . . ? O4 C70 H70A 109.5 . . ? O4 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O4 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N18 C50 C51 110.2(5) . . ? N18 C50 H50 124.9 . . ? C51 C50 H50 124.9 . . ? C52 C51 C50 106.4(5) . . ? C52 C51 H51 126.8 . . ? C50 C51 H51 126.8 . . ? C51 C52 N17 107.2(4) . . ? C51 C52 H52 126.4 . . ? N17 C52 H52 126.4 . . ? N16 C53 C54 110.0(4) . . ? N16 C53 H53 125.0 . . ? C54 C53 H53 125.0 . . ? C55 C54 C53 106.6(4) . . ? C55 C54 H54 126.7 . . ? C53 C54 H54 126.7 . . ? C54 C55 N15 106.1(4) . . ? C54 C55 H55 127.0 . . ? N15 C55 H55 127.0 . . ? N14 C56 C57 111.7(4) . . ? N14 C56 H56 124.2 . . ? C57 C56 H56 124.2 . . ? C58 C57 C56 105.7(4) . . ? C58 C57 H57 127.1 . . ? C56 C57 H57 127.1 . . ? N13 C58 C57 106.9(4) . . ? N13 C58 H58 126.5 . . ? C57 C58 H58 126.5 . . ? N15 C59 N13 108.0(3) . . ? N15 C59 N17 109.3(4) . . ? N13 C59 N17 108.2(4) . . ? N15 C59 C60 110.6(4) . . ? N13 C59 C60 109.3(4) . . ? N17 C59 C60 111.3(4) . . ? O2 C60 C59 107.5(4) . . ? O2 C60 H60A 110.2 . . ? C59 C60 H60A 110.2 . . ? O2 C60 H60B 110.2 . . ? C59 C60 H60B 110.2 . . ? H60A C60 H60B 108.5 . . ? O2 C61 C62 106.6(4) . . ? O2 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? O2 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? C66 C62 C63 119.8(4) . . ? C66 C62 C61 120.6(4) . . ? C63 C62 C61 119.6(4) . . ? C64 C63 C62 120.1(4) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 121.5(5) . 2_667 ? C63 C64 H64 119.3 . . ? C65 C64 H64 119.3 2_667 . ? C66 C65 C64 123.1(4) . 2_667 ? C66 C65 C65 118.6(5) . 2_667 ? C64 C65 C65 118.2(5) 2_667 2_667 ? C62 C66 C65 121.7(4) . . ? C62 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? N23 C45 C46 110.4(4) . . ? N23 C45 C44 122.7(5) . . ? C46 C45 C44 126.9(5) . . ? C47 C46 C45 107.8(5) . . ? C47 C46 H46 126.1 . . ? C45 C46 H46 126.1 . . ? C46 C47 N24 105.2(4) . . ? C46 C47 C48 132.2(5) . . ? N24 C47 C48 122.6(5) . . ? C45 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C45 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N19 C40 C41 109.4(4) . . ? N19 C40 C39 123.3(4) . . ? C41 C40 C39 127.3(4) . . ? C42 C41 C40 107.7(4) . . ? C42 C41 H41 126.1 . . ? C40 C41 H41 126.1 . . ? N20 C42 C41 105.7(4) . . ? N20 C42 C43 122.2(4) . . ? C41 C42 C43 132.1(5) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N21 C35 C36 109.5(4) . . ? N21 C35 C34 123.1(5) . . ? C36 C35 C34 127.3(5) . . ? C37 C36 C35 108.3(4) . . ? C37 C36 H36 125.9 . . ? C35 C36 H36 125.9 . . ? N22 C37 C36 105.1(4) . . ? N22 C37 C38 122.6(4) . . ? C36 C37 C38 132.3(5) . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N24 C49 N22 110.7(3) . . ? N24 C49 N20 110.0(4) . . ? N22 C49 N20 110.4(4) . . ? N24 C49 H49 108.5 . . ? N22 C49 H49 108.5 . . ? N20 C49 H49 108.5 . . ? O5 C71 H71A 109.5 . . ? O5 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O5 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O5 C72 C73 111.9(7) . . ? O5 C72 H72A 109.2 . . ? C73 C72 H72A 109.2 . . ? O5 C72 H72B 109.2 . . ? C73 C72 H72B 109.2 . . ? H72A C72 H72B 107.9 . . ? O6 C73 C72 109.8(7) . . ? O6 C73 H73A 109.7 . . ? C72 C73 H73A 109.7 . . ? O6 C73 H73B 109.7 . . ? C72 C73 H73B 109.7 . . ? H73A C73 H73B 108.2 . . ? O6 C74 H74A 109.5 . . ? O6 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? O6 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N25 C75 C76 176.8(10) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N26 C79 C80 172.8(17) . . ? N4 Fe1 N6 87.91(15) . . ? N4 Fe1 N2 88.08(15) . . ? N6 Fe1 N2 86.54(15) . . ? N4 Fe1 N7 90.23(15) . . ? N6 Fe1 N7 176.97(14) . . ? N2 Fe1 N7 90.99(14) . . ? N4 Fe1 N9 91.21(15) . . ? N6 Fe1 N9 92.58(15) . . ? N2 Fe1 N9 178.89(15) . . ? N7 Fe1 N9 89.86(14) . . ? N4 Fe1 N11 177.84(15) . . ? N6 Fe1 N11 93.65(15) . . ? N2 Fe1 N11 93.50(15) . . ? N7 Fe1 N11 88.27(15) . . ? N9 Fe1 N11 87.24(15) . . ? N18 Fe2 N16 87.72(16) . . ? N18 Fe2 N14 86.77(16) . . ? N16 Fe2 N14 87.88(16) . . ? N18 Fe2 N21 91.84(16) . . ? N16 Fe2 N21 91.15(16) . . ? N14 Fe2 N21 178.34(15) . . ? N18 Fe2 N19 178.73(16) . . ? N16 Fe2 N19 91.76(15) . . ? N14 Fe2 N19 92.05(15) . . ? N21 Fe2 N19 89.32(15) . . ? N18 Fe2 N23 93.70(16) . . ? N16 Fe2 N23 178.52(15) . . ? N14 Fe2 N23 92.64(16) . . ? N21 Fe2 N23 88.36(16) . . ? N19 Fe2 N23 86.83(15) . . ? N27 C82 C81 175(3) . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? 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 Fe1 N7 N8 C16 0.7(5) . . . . ? Fe1 N9 N10 C16 5.0(5) . . . . ? Fe1 N11 N12 C16 1.3(4) . . . . ? Fe1 N2 N1 C26 4.6(5) . . . . ? Fe1 N4 N3 C26 1.9(5) . . . . ? Fe1 N6 N5 C26 -0.1(5) . . . . ? Fe2 N19 N20 C49 -3.0(5) . . . . ? Fe2 N21 N22 C49 0.5(5) . . . . ? Fe2 N23 N24 C49 1.0(5) . . . . ? Fe2 N14 N13 C59 2.5(5) . . . . ? Fe2 N16 N15 C59 -1.5(5) . . . . ? Fe2 N18 N17 C59 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.661 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.107 # Attachment '- 3.2DME(123K).CIF' #========================================================================== data_3.2DME(123K) _database_code_depnum_ccdc_archive 'CCDC 803927' #TrackingRef '- 3.2DME(123K).CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}2(C2H2(CH2OCH2C(pz)3]2)](BF4)4(DME)2 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))2(C2H2(CH2OCH2C(pz)3)2))(BF4)4(DME)2 _chemical_melting_point ? _chemical_formula_moiety 'C58 H72 Fe2 N24 O2, 2(C4 H10 O2), 4(B F4)' _chemical_formula_sum 'C66 H92 B4 F16 Fe2 N24 O6' _chemical_formula_weight 1776.58 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1486(7) _cell_length_b 21.4040(15) _cell_length_c 16.9246(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.734(2) _cell_angle_gamma 90.00 _cell_volume 4034.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 8138 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 30.30 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8369 _exptl_absorpt_correction_T_max 0.9133 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _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 32487 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9141 _reflns_number_gt 7430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9141 _refine_ls_number_parameters 556 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C23 C 0.4023(3) 0.63365(17) 0.0205(2) 0.0214(7) Uani 1 1 d . . . H23 H 0.3715 0.6569 -0.0238 0.026 Uiso 1 1 calc R . . Fe1 Fe 0.26391(4) 0.70027(2) 0.14644(3) 0.01186(12) Uani 1 1 d . . . N4 N 0.2120(2) 0.63123(13) 0.21190(15) 0.0143(6) Uani 1 1 d . A . N7 N 0.1553(2) 0.75879(13) 0.20105(15) 0.0143(6) Uani 1 1 d . . . N6 N 0.3700(3) 0.64234(13) 0.09431(16) 0.0163(6) Uani 1 1 d . . . N2 N 0.3964(3) 0.71194(12) 0.22474(16) 0.0162(6) Uani 1 1 d . . . N9 N 0.1327(3) 0.68362(13) 0.06603(15) 0.0164(6) Uani 1 1 d . . . N11 N 0.3110(3) 0.77131(13) 0.07863(16) 0.0169(6) Uani 1 1 d . . . N8 N 0.0860(3) 0.79855(13) 0.15463(15) 0.0165(6) Uani 1 1 d . . . N3 N 0.2933(3) 0.58723(13) 0.23713(15) 0.0158(6) Uani 1 1 d . A . C16 C 0.0976(3) 0.79496(16) 0.06986(18) 0.0167(7) Uani 1 1 d . . . H16 H 0.0421 0.8263 0.0440 0.020 Uiso 1 1 calc R . . N10 N 0.0632(2) 0.73334(13) 0.04115(15) 0.0149(6) Uani 1 1 d . . . O1 O 0.4745(3) 0.54768(12) 0.34479(14) 0.0284(6) Uani 1 1 d . . . C15 C 0.1803(4) 0.90832(18) -0.0272(2) 0.0291(9) Uani 1 1 d . . . H15A H 0.1146 0.8895 -0.0596 0.044 Uiso 1 1 calc R . . H15B H 0.2268 0.9362 -0.0600 0.044 Uiso 1 1 calc R . . H15C H 0.1471 0.9323 0.0160 0.044 Uiso 1 1 calc R . . N5 N 0.4350(3) 0.59973(13) 0.13855(15) 0.0149(6) Uani 1 1 d . A . N1 N 0.4534(3) 0.66015(13) 0.25561(16) 0.0165(6) Uani 1 1 d . A . C19 C 0.5454(3) 0.67695(18) 0.3072(2) 0.0265(8) Uani 1 1 d . . . H19 H 0.5984 0.6494 0.3356 0.032 Uiso 1 1 calc R . . C2 C 0.1213(3) 0.76963(16) 0.27459(18) 0.0170(7) Uani 1 1 d . . . N12 N 0.2196(3) 0.81017(13) 0.05008(16) 0.0171(6) Uani 1 1 d . . . C17 C 0.4531(3) 0.76037(17) 0.2584(2) 0.0241(8) Uani 1 1 d . . . H17 H 0.4326 0.8028 0.2484 0.029 Uiso 1 1 calc R . . C4 C 0.0098(3) 0.83322(17) 0.1965(2) 0.0219(8) Uani 1 1 d . . . C18 C 0.5472(4) 0.74071(19) 0.3104(2) 0.0314(9) Uani 1 1 d . . . H18 H 0.6009 0.7663 0.3413 0.038 Uiso 1 1 calc R . . C26 C 0.4197(3) 0.59828(15) 0.22377(18) 0.0151(7) Uani 1 1 d . . . C22 C 0.2378(4) 0.53877(16) 0.2718(2) 0.0218(8) Uani 1 1 d . . . H22 H 0.2751 0.5021 0.2929 0.026 Uiso 1 1 calc R A . C25 C 0.5070(3) 0.56510(16) 0.0925(2) 0.0182(7) Uani 1 1 d . . . H25 H 0.5604 0.5328 0.1098 0.022 Uiso 1 1 calc R A . C24 C 0.4875(3) 0.58590(17) 0.0165(2) 0.0236(8) Uani 1 1 d . A . H24 H 0.5241 0.5710 -0.0294 0.028 Uiso 1 1 calc R . . C12 C 0.4106(3) 0.79563(18) 0.0496(2) 0.0243(8) Uani 1 1 d . . . C1 C 0.1744(4) 0.73644(17) 0.34611(19) 0.0230(8) Uani 1 1 d . . . H1A H 0.1189 0.7039 0.3624 0.034 Uiso 1 1 calc R . . H1B H 0.1879 0.7664 0.3894 0.034 Uiso 1 1 calc R . . H1C H 0.2509 0.7173 0.3333 0.034 Uiso 1 1 calc R . . C8 C -0.0195(3) 0.65155(17) -0.0158(2) 0.0219(8) Uani 1 1 d . . . H8 H -0.0711 0.6249 -0.0468 0.026 Uiso 1 1 calc R . . C6 C 0.1326(4) 0.56829(17) 0.0394(2) 0.0257(8) Uani 1 1 d . . . H6A H 0.1862 0.5597 -0.0035 0.038 Uiso 1 1 calc R . . H6B H 0.0664 0.5381 0.0372 0.038 Uiso 1 1 calc R . . H6C H 0.1775 0.5647 0.0904 0.038 Uiso 1 1 calc R . . C3 C 0.0315(3) 0.81547(17) 0.2737(2) 0.0220(8) Uani 1 1 d . . . H3 H -0.0073 0.8313 0.3183 0.026 Uiso 1 1 calc R . . C9 C -0.0311(3) 0.71516(16) -0.00766(19) 0.0191(7) Uani 1 1 d . . . C7 C 0.0829(3) 0.63309(17) 0.03040(19) 0.0191(7) Uani 1 1 d . . . C20 C 0.1065(3) 0.61052(16) 0.23338(19) 0.0190(7) Uani 1 1 d . . . H20 H 0.0327 0.6322 0.2244 0.023 Uiso 1 1 calc R A . C27 C 0.4979(3) 0.54711(16) 0.26301(19) 0.0203(7) Uani 1 1 d . A . H27A H 0.4773 0.5059 0.2396 0.024 Uiso 1 1 calc R . . H27B H 0.5839 0.5556 0.2555 0.024 Uiso 1 1 calc R . . C13 C 0.3811(4) 0.84907(18) 0.0045(2) 0.0264(8) Uani 1 1 d . . . H13 H 0.4357 0.8745 -0.0227 0.032 Uiso 1 1 calc R . . C14 C 0.2604(3) 0.85792(16) 0.00654(19) 0.0198(7) Uani 1 1 d . . . C5 C -0.0741(4) 0.8804(2) 0.1595(2) 0.0345(10) Uani 1 1 d . . . H5A H -0.0277 0.9137 0.1354 0.052 Uiso 1 1 calc R . . H5B H -0.1236 0.8984 0.2001 0.052 Uiso 1 1 calc R . . H5C H -0.1260 0.8602 0.1187 0.052 Uiso 1 1 calc R . . C21 C 0.1182(4) 0.55261(17) 0.2709(2) 0.0241(8) Uani 1 1 d . A . H21 H 0.0560 0.5280 0.2915 0.029 Uiso 1 1 calc R . . F1 F 0.3422(2) 0.46079(11) 0.12869(16) 0.0427(7) Uani 1 1 d . . . F4 F 0.3480(3) 0.39495(14) 0.23237(17) 0.0583(8) Uani 1 1 d . . . O2 O 0.7594(3) 0.59744(14) 0.17679(18) 0.0402(7) Uani 1 1 d . . . C10 C -0.1242(3) 0.75901(19) -0.0418(2) 0.0291(9) Uani 1 1 d . . . H10A H -0.1583 0.7832 0.0008 0.044 Uiso 1 1 calc R . . H10B H -0.1881 0.7351 -0.0697 0.044 Uiso 1 1 calc R . . H10C H -0.0873 0.7875 -0.0790 0.044 Uiso 1 1 calc R . . C11 C 0.5333(4) 0.7693(2) 0.0659(3) 0.0361(10) Uani 1 1 d . . . H11A H 0.5283 0.7329 0.1007 0.054 Uiso 1 1 calc R . . H11B H 0.5848 0.8011 0.0916 0.054 Uiso 1 1 calc R . . H11C H 0.5672 0.7566 0.0160 0.054 Uiso 1 1 calc R . . C33 C 0.7663(5) 0.6585(2) 0.1451(3) 0.0473(12) Uani 1 1 d . . . H33A H 0.8506 0.6714 0.1444 0.071 Uiso 1 1 calc R . . H33B H 0.7224 0.6875 0.1779 0.071 Uiso 1 1 calc R . . H33C H 0.7306 0.6588 0.0911 0.071 Uiso 1 1 calc R . . C32 C 0.8251(4) 0.5530(2) 0.1342(3) 0.0368(10) Uani 1 1 d . . . H32A H 0.9102 0.5659 0.1331 0.044 Uiso 1 1 calc R . . H32B H 0.7920 0.5504 0.0789 0.044 Uiso 1 1 calc R . . C28 C 0.5231(4) 0.4944(2) 0.3870(3) 0.036(3) Uani 0.60(2) 1 d PU A 1 H28A H 0.6114 0.4982 0.3942 0.044 Uiso 0.60(2) 1 calc PR A 1 H28B H 0.5044 0.4556 0.3569 0.044 Uiso 0.60(2) 1 calc PR A 1 B1 B 0.2957(4) 0.4064(2) 0.1571(3) 0.0284(10) Uani 1 1 d . . . F3 F 0.3145(3) 0.35729(11) 0.10519(16) 0.0480(7) Uani 1 1 d . . . F2 F 0.1727(2) 0.41416(14) 0.16300(15) 0.0477(7) Uani 1 1 d . . . O3 O 0.6995(3) 0.46730(14) 0.15893(19) 0.0389(7) Uani 1 1 d . . . F5 F 0.8929(3) 0.58312(16) 0.48034(16) 0.0578(8) Uani 1 1 d . . . C31 C 0.8167(4) 0.4904(2) 0.1732(3) 0.0376(10) Uani 1 1 d . . . H31A H 0.8757 0.4613 0.1515 0.045 Uiso 1 1 calc R . . H31B H 0.8346 0.4945 0.2308 0.045 Uiso 1 1 calc R . . B2 B 0.8476(5) 0.5760(2) 0.4045(3) 0.0331(11) Uani 1 1 d . . . F8 F 0.9108(3) 0.61575(14) 0.35527(17) 0.0553(8) Uani 1 1 d . . . F6 F 0.8616(4) 0.51557(14) 0.37957(17) 0.0661(10) Uani 1 1 d . . . F7 F 0.7302(3) 0.59356(19) 0.4019(2) 0.0808(12) Uani 1 1 d . . . C30 C 0.6791(5) 0.4103(2) 0.1975(4) 0.0572(15) Uani 1 1 d . . . H30A H 0.7322 0.3781 0.1774 0.086 Uiso 1 1 calc R . . H30B H 0.5952 0.3976 0.1875 0.086 Uiso 1 1 calc R . . H30C H 0.6955 0.4154 0.2546 0.086 Uiso 1 1 calc R . . C29 C 0.4664(10) 0.4920(4) 0.4674(5) 0.030(3) Uani 0.60(2) 1 d P . 1 H29 H 0.3853 0.4794 0.4714 0.036 Uiso 0.60(2) 1 calc PR A 1 C29' C 0.5383(17) 0.5132(7) 0.4746(7) 0.034(5) Uani 0.40(2) 1 d P . 2 H29' H 0.5985 0.5419 0.4926 0.040 Uiso 0.40(2) 1 calc PR A 2 C28' C 0.5231(4) 0.4944(2) 0.3870(3) 0.040(3) Uani 0.40(2) 1 d P A 2 H28C H 0.6016 0.4825 0.3664 0.048 Uiso 0.40(2) 1 calc PR A 2 H28D H 0.4678 0.4583 0.3807 0.048 Uiso 0.40(2) 1 calc PR A 2 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 C23 0.026(2) 0.0249(18) 0.0133(16) -0.0008(14) 0.0058(14) 0.0008(15) Fe1 0.0149(2) 0.0128(2) 0.0079(2) -0.00001(17) 0.00079(16) 0.00245(18) N4 0.0161(14) 0.0169(14) 0.0100(12) 0.0000(10) 0.0002(10) 0.0024(11) N7 0.0157(14) 0.0189(14) 0.0082(12) 0.0010(10) -0.0010(10) 0.0032(11) N6 0.0180(15) 0.0189(14) 0.0121(13) 0.0010(11) 0.0024(11) 0.0026(11) N2 0.0200(15) 0.0111(13) 0.0174(13) -0.0003(10) 0.0007(11) 0.0034(11) N9 0.0231(16) 0.0162(13) 0.0099(12) -0.0008(10) 0.0010(11) 0.0025(11) N11 0.0146(14) 0.0196(14) 0.0167(14) 0.0028(11) 0.0020(11) 0.0032(12) N8 0.0218(15) 0.0184(14) 0.0094(12) -0.0009(11) 0.0006(11) 0.0066(12) N3 0.0221(15) 0.0154(13) 0.0100(12) 0.0002(10) 0.0014(11) 0.0042(11) C16 0.0210(18) 0.0206(17) 0.0085(14) 0.0010(12) 0.0020(12) 0.0034(14) N10 0.0163(14) 0.0187(14) 0.0096(12) 0.0010(10) 0.0012(10) 0.0004(11) O1 0.0481(18) 0.0245(13) 0.0122(12) 0.0031(10) -0.0026(11) 0.0140(12) C15 0.041(2) 0.0222(19) 0.0236(19) 0.0076(15) 0.0002(17) -0.0006(17) N5 0.0172(15) 0.0147(13) 0.0128(13) -0.0014(10) 0.0015(11) 0.0035(11) N1 0.0198(15) 0.0155(13) 0.0138(13) -0.0013(11) -0.0033(11) 0.0011(11) C19 0.023(2) 0.029(2) 0.0259(19) -0.0037(16) -0.0090(15) 0.0054(16) C2 0.0230(18) 0.0193(16) 0.0087(14) -0.0007(12) 0.0013(13) 0.0022(14) N12 0.0206(15) 0.0169(14) 0.0139(13) 0.0055(11) 0.0031(11) 0.0006(11) C17 0.029(2) 0.0173(17) 0.0258(19) -0.0049(14) -0.0016(15) -0.0002(15) C4 0.028(2) 0.0235(18) 0.0146(16) 0.0007(14) 0.0038(14) 0.0092(15) C18 0.030(2) 0.027(2) 0.036(2) -0.0092(17) -0.0121(17) -0.0041(17) C26 0.0209(18) 0.0133(15) 0.0111(15) -0.0019(12) 0.0008(12) 0.0028(13) C22 0.036(2) 0.0150(16) 0.0142(16) 0.0003(13) 0.0036(14) -0.0017(15) C25 0.0169(18) 0.0155(16) 0.0227(17) -0.0044(13) 0.0041(13) 0.0027(13) C24 0.026(2) 0.0263(19) 0.0194(17) -0.0014(15) 0.0095(15) 0.0021(15) C12 0.0230(19) 0.0255(19) 0.0245(18) 0.0004(15) 0.0035(15) -0.0026(16) C1 0.034(2) 0.0256(19) 0.0096(15) 0.0009(13) -0.0005(14) 0.0070(16) C8 0.025(2) 0.0269(19) 0.0131(16) 0.0018(14) -0.0025(14) -0.0080(15) C6 0.036(2) 0.0199(18) 0.0214(18) -0.0045(14) 0.0008(16) 0.0017(16) C3 0.029(2) 0.0245(18) 0.0126(15) -0.0004(13) 0.0063(14) 0.0085(15) C9 0.0217(19) 0.0238(18) 0.0117(15) 0.0016(13) -0.0001(13) -0.0046(14) C7 0.0228(19) 0.0242(18) 0.0107(15) -0.0024(13) 0.0031(13) -0.0032(14) C20 0.0206(18) 0.0247(18) 0.0118(15) -0.0052(13) 0.0025(13) -0.0026(14) C27 0.0255(19) 0.0201(17) 0.0150(16) 0.0019(13) -0.0013(14) 0.0077(14) C13 0.028(2) 0.027(2) 0.0244(19) 0.0061(15) 0.0042(15) -0.0047(16) C14 0.027(2) 0.0216(17) 0.0110(15) 0.0022(13) 0.0001(13) -0.0027(15) C5 0.043(3) 0.041(2) 0.0200(18) 0.0023(17) 0.0056(17) 0.027(2) C21 0.031(2) 0.0223(18) 0.0194(17) -0.0039(14) 0.0083(15) -0.0084(16) F1 0.0542(17) 0.0276(13) 0.0485(15) -0.0098(11) 0.0244(13) -0.0126(12) F4 0.069(2) 0.0583(19) 0.0455(16) 0.0033(14) -0.0135(15) 0.0103(16) O2 0.0448(19) 0.0371(17) 0.0395(17) -0.0026(14) 0.0097(14) -0.0022(14) C10 0.022(2) 0.032(2) 0.031(2) 0.0047(17) -0.0103(16) -0.0005(16) C11 0.023(2) 0.035(2) 0.052(3) 0.012(2) 0.0099(19) 0.0014(18) C33 0.039(3) 0.044(3) 0.060(3) 0.005(2) 0.008(2) -0.001(2) C32 0.027(2) 0.045(3) 0.038(2) -0.008(2) 0.0029(18) -0.0045(19) C28 0.037(3) 0.037(3) 0.036(3) 0.0000(10) 0.0017(10) 0.0000(10) B1 0.033(3) 0.027(2) 0.026(2) -0.0040(18) 0.0051(18) -0.0063(19) F3 0.073(2) 0.0247(13) 0.0462(16) -0.0052(11) 0.0067(14) 0.0013(13) F2 0.0336(15) 0.073(2) 0.0376(14) -0.0152(14) 0.0076(11) -0.0192(14) O3 0.0309(17) 0.0307(16) 0.0544(19) 0.0063(14) -0.0034(14) 0.0026(13) F5 0.0580(19) 0.083(2) 0.0312(14) -0.0102(14) -0.0075(13) 0.0083(17) C31 0.032(2) 0.045(3) 0.036(2) -0.003(2) -0.0021(19) 0.002(2) B2 0.030(3) 0.039(3) 0.029(2) 0.002(2) -0.0085(19) 0.001(2) F8 0.074(2) 0.0459(17) 0.0480(17) -0.0042(13) 0.0225(15) -0.0102(15) F6 0.121(3) 0.0358(16) 0.0417(16) 0.0004(13) 0.0044(17) -0.0032(17) F7 0.0320(17) 0.103(3) 0.106(3) 0.039(2) -0.0153(18) 0.0060(17) C30 0.051(3) 0.038(3) 0.083(4) 0.023(3) 0.004(3) 0.005(2) C29 0.032(6) 0.026(4) 0.032(6) 0.005(3) 0.001(4) 0.007(4) C29' 0.045(11) 0.036(7) 0.020(8) 0.010(5) 0.001(5) 0.009(7) C28' 0.040(7) 0.040(4) 0.040(5) 0.000(5) 0.002(5) 0.000(5) _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 C23 N6 1.330(4) . ? C23 C24 1.399(5) . ? C23 H23 0.9500 . ? Fe1 N4 1.951(3) . ? Fe1 N2 1.953(3) . ? Fe1 N6 1.953(3) . ? Fe1 N9 1.982(3) . ? Fe1 N11 1.991(3) . ? Fe1 N7 1.999(3) . ? N4 C20 1.324(4) . ? N4 N3 1.361(4) . ? N7 C2 1.339(4) . ? N7 N8 1.371(4) . ? N6 N5 1.366(4) . ? N2 C17 1.328(4) . ? N2 N1 1.369(4) . ? N9 C7 1.345(4) . ? N9 N10 1.371(4) . ? N11 C12 1.340(5) . ? N11 N12 1.384(4) . ? N8 C4 1.354(4) . ? N8 C16 1.449(4) . ? N3 C22 1.356(4) . ? N3 C26 1.458(4) . ? C16 N10 1.451(4) . ? C16 N12 1.453(4) . ? C16 H16 1.0000 . ? N10 C9 1.362(4) . ? O1 C27 1.421(4) . ? O1 C28 1.438(5) . ? C15 C14 1.496(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N5 C25 1.364(4) . ? N5 C26 1.461(4) . ? N1 C19 1.363(4) . ? N1 C26 1.472(4) . ? C19 C18 1.366(5) . ? C19 H19 0.9500 . ? C2 C3 1.402(5) . ? C2 C1 1.500(4) . ? N12 C14 1.351(4) . ? C17 C18 1.402(5) . ? C17 H17 0.9500 . ? C4 C3 1.371(5) . ? C4 C5 1.494(5) . ? C18 H18 0.9500 . ? C26 C27 1.531(4) . ? C22 C21 1.365(6) . ? C22 H22 0.9500 . ? C25 C24 1.369(5) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? C12 C13 1.406(5) . ? C12 C11 1.492(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C8 C9 1.375(5) . ? C8 C7 1.409(5) . ? C8 H8 0.9500 . ? C6 C7 1.498(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C3 H3 0.9500 . ? C9 C10 1.496(5) . ? C20 C21 1.396(5) . ? C20 H20 0.9500 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C13 C14 1.361(5) . ? C13 H13 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C21 H21 0.9500 . ? F1 B1 1.372(5) . ? F4 B1 1.396(5) . ? O2 C33 1.416(6) . ? O2 C32 1.419(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C32 C31 1.497(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C28 C29 1.528(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? B1 F2 1.390(6) . ? B1 F3 1.393(5) . ? O3 C31 1.407(5) . ? O3 C30 1.408(6) . ? F5 B2 1.366(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? B2 F7 1.360(6) . ? B2 F6 1.371(6) . ? B2 F8 1.405(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29 C29 1.35(2) 3_666 ? C29 H29 0.9500 . ? C29' C29' 1.36(3) 3_666 ? C29' H29' 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 N6 C23 C24 111.2(3) . . ? N6 C23 H23 124.4 . . ? C24 C23 H23 124.4 . . ? N4 Fe1 N2 86.95(11) . . ? N4 Fe1 N6 88.74(12) . . ? N2 Fe1 N6 86.17(12) . . ? N4 Fe1 N9 91.41(11) . . ? N2 Fe1 N9 176.81(12) . . ? N6 Fe1 N9 91.07(12) . . ? N4 Fe1 N11 178.04(12) . . ? N2 Fe1 N11 94.69(12) . . ? N6 Fe1 N11 92.43(12) . . ? N9 Fe1 N11 87.01(12) . . ? N4 Fe1 N7 90.54(11) . . ? N2 Fe1 N7 93.50(11) . . ? N6 Fe1 N7 179.22(11) . . ? N9 Fe1 N7 89.25(11) . . ? N11 Fe1 N7 88.29(11) . . ? C20 N4 N3 105.6(3) . . ? C20 N4 Fe1 134.5(2) . . ? N3 N4 Fe1 119.4(2) . . ? C2 N7 N8 104.4(3) . . ? C2 N7 Fe1 138.0(2) . . ? N8 N7 Fe1 117.45(19) . . ? C23 N6 N5 105.1(3) . . ? C23 N6 Fe1 135.2(2) . . ? N5 N6 Fe1 119.6(2) . . ? C17 N2 N1 105.4(3) . . ? C17 N2 Fe1 136.1(2) . . ? N1 N2 Fe1 118.5(2) . . ? C7 N9 N10 105.7(3) . . ? C7 N9 Fe1 136.7(2) . . ? N10 N9 Fe1 117.4(2) . . ? C12 N11 N12 104.3(3) . . ? C12 N11 Fe1 138.9(2) . . ? N12 N11 Fe1 116.8(2) . . ? C4 N8 N7 113.0(3) . . ? C4 N8 C16 129.4(3) . . ? N7 N8 C16 117.4(3) . . ? C22 N3 N4 110.8(3) . . ? C22 N3 C26 131.0(3) . . ? N4 N3 C26 118.2(3) . . ? N8 C16 N10 110.2(3) . . ? N8 C16 N12 110.2(3) . . ? N10 C16 N12 111.2(3) . . ? N8 C16 H16 108.4 . . ? N10 C16 H16 108.4 . . ? N12 C16 H16 108.4 . . ? C9 N10 N9 111.9(3) . . ? C9 N10 C16 130.3(3) . . ? N9 N10 C16 117.8(3) . . ? C27 O1 C28 113.2(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C25 N5 N6 111.2(3) . . ? C25 N5 C26 130.7(3) . . ? N6 N5 C26 118.1(3) . . ? C19 N1 N2 110.6(3) . . ? C19 N1 C26 130.0(3) . . ? N2 N1 C26 118.9(3) . . ? N1 C19 C18 107.4(3) . . ? N1 C19 H19 126.3 . . ? C18 C19 H19 126.3 . . ? N7 C2 C3 110.2(3) . . ? N7 C2 C1 123.4(3) . . ? C3 C2 C1 126.5(3) . . ? C14 N12 N11 112.6(3) . . ? C14 N12 C16 129.6(3) . . ? N11 N12 C16 117.8(3) . . ? N2 C17 C18 111.2(3) . . ? N2 C17 H17 124.4 . . ? C18 C17 H17 124.4 . . ? N8 C4 C3 105.1(3) . . ? N8 C4 C5 123.2(3) . . ? C3 C4 C5 131.7(3) . . ? C19 C18 C17 105.4(3) . . ? C19 C18 H18 127.3 . . ? C17 C18 H18 127.3 . . ? N3 C26 N5 108.4(3) . . ? N3 C26 N1 108.7(3) . . ? N5 C26 N1 107.6(3) . . ? N3 C26 C27 110.6(3) . . ? N5 C26 C27 110.6(3) . . ? N1 C26 C27 110.8(3) . . ? N3 C22 C21 107.1(3) . . ? N3 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? N5 C25 C24 106.8(3) . . ? N5 C25 H25 126.6 . . ? C24 C25 H25 126.6 . . ? C25 C24 C23 105.7(3) . . ? C25 C24 H24 127.2 . . ? C23 C24 H24 127.2 . . ? N11 C12 C13 109.8(3) . . ? N11 C12 C11 123.6(3) . . ? C13 C12 C11 126.6(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C8 C7 107.4(3) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C3 C2 107.3(3) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? N10 C9 C8 105.7(3) . . ? N10 C9 C10 123.8(3) . . ? C8 C9 C10 130.5(3) . . ? N9 C7 C8 109.2(3) . . ? N9 C7 C6 123.8(3) . . ? C8 C7 C6 127.0(3) . . ? N4 C20 C21 110.9(3) . . ? N4 C20 H20 124.5 . . ? C21 C20 H20 124.5 . . ? O1 C27 C26 106.8(3) . . ? O1 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? O1 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C14 C13 C12 107.7(3) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? N12 C14 C13 105.5(3) . . ? N12 C14 C15 122.9(3) . . ? C13 C14 C15 131.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C22 C21 C20 105.6(3) . . ? C22 C21 H21 127.2 . . ? C20 C21 H21 127.2 . . ? C33 O2 C32 112.9(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C33 H33A 109.5 . . ? O2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C32 C31 109.3(4) . . ? O2 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O2 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? O1 C28 C29 107.9(4) . . ? O1 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? O1 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? F1 B1 F2 108.3(4) . . ? F1 B1 F3 110.4(3) . . ? F2 B1 F3 108.3(4) . . ? F1 B1 F4 108.7(4) . . ? F2 B1 F4 109.1(4) . . ? F3 B1 F4 112.0(4) . . ? C31 O3 C30 113.3(4) . . ? O3 C31 C32 108.4(4) . . ? O3 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O3 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? F7 B2 F5 108.2(4) . . ? F7 B2 F6 112.0(4) . . ? F5 B2 F6 110.6(4) . . ? F7 B2 F8 108.8(4) . . ? F5 B2 F8 108.4(4) . . ? F6 B2 F8 108.7(4) . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C29 C28 118.9(13) 3_666 . ? C29 C29 H29 120.5 3_666 . ? C28 C29 H29 120.5 . . ? C29' C29' H29' 121.4 3_666 . ? 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 Fe1 N7 N8 C16 -0.2(4) . . . . ? Fe1 N9 N10 C16 5.6(3) . . . . ? Fe1 N11 N12 C16 -1.8(4) . . . . ? Fe1 N2 N1 C26 5.2(4) . . . . ? Fe1 N4 N3 C26 8.7(3) . . . . ? Fe1 N6 N5 C26 1.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.661 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.084 # Attachment '- 4-100final.CIF' #========================================================================== data_4.solvent(100K) _database_code_depnum_ccdc_archive 'CCDC 803928' #TrackingRef '- 4-100final.CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}3(C6(CH3)3(CH2OCH2C(pz)3]3)](BF4)6 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))3(C6(CH3)3(CH2OCH2C(pz)3)3))(BF4)6 _chemical_melting_point ? _chemical_formula_moiety '2(C93 H114 Fe3 N36 O3), 12(B F4)' _chemical_formula_sum 'C93 H117 B6 F24 Fe3 N36 O3.75' _chemical_formula_weight 2487.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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 0.0020 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0074 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0211 0.0126 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3552 0.9971 '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 23.066(4) _cell_length_b 23.150(6) _cell_length_c 23.968(4) _cell_angle_alpha 77.782(7) _cell_angle_beta 83.52(2) _cell_angle_gamma 83.41(2) _cell_volume 12374(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 128846 _cell_measurement_theta_min 0.97 _cell_measurement_theta_max 25.62 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5124 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9912 _exptl_absorpt_correction_T_max 0.9991 _exptl_absorpt_process_details 'XDS (Kabsch, 1993)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77489 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 128844 _diffrn_reflns_av_R_equivalents 0.1206 _diffrn_reflns_av_sigmaI/netI 0.1205 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 25.62 _reflns_number_total 33012 _reflns_number_gt 15688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.011 0.005 2125 772 ' ' 2 0.242 0.192 0.742 7 0 ' ' 3 0.758 0.808 0.258 7 0 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 33012 _refine_ls_number_parameters 2882 _refine_ls_number_restraints 237 _refine_ls_R_factor_all 0.2139 _refine_ls_R_factor_gt 0.1460 _refine_ls_wR_factor_ref 0.3616 _refine_ls_wR_factor_gt 0.3421 _refine_ls_goodness_of_fit_ref 1.751 _refine_ls_restrained_S_all 1.748 _refine_ls_shift/su_max 0.004 _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 B1D B -0.0617(4) 0.7358(5) 0.6968(4) 0.130 Uani 1 1 d DU . . F1D F -0.1141(4) 0.7531(4) 0.7188(4) 0.181 Uani 1 1 d D . . F2D F -0.0615(4) 0.6825(4) 0.6796(4) 0.156 Uani 1 1 d D . . F3D F -0.0462(4) 0.7777(4) 0.6488(3) 0.179 Uani 1 1 d D . . F4D F -0.0206(4) 0.7276(5) 0.7336(4) 0.178 Uani 1 1 d D . . B1A B -0.0004(14) 0.5190(12) 0.4717(15) 0.044 Uiso 0.50 1 d PD A -1 F1A F -0.0368(6) 0.5666(7) 0.4543(6) 0.078 Uiso 0.50 1 d PD A -1 F2A F 0.0611(6) 0.5287(7) 0.4431(6) 0.080 Uiso 0.50 1 d PD A -1 F3A F -0.0117(6) 0.4706(7) 0.4355(6) 0.085 Uiso 0.50 1 d PD A -1 F4A F 0.0018(9) 0.4996(8) 0.5285(10) 0.100 Uiso 0.50 1 d PD A -1 B1B B 0.5014(9) 0.9875(11) 0.0398(9) 0.030 Uani 0.50 1 d PDU B -1 F1B F 0.5569(6) 0.9768(7) 0.0612(5) 0.080 Uani 0.50 1 d PD B -1 F2B F 0.4703(6) 1.0296(6) 0.0686(5) 0.071 Uani 0.50 1 d PD B -1 F3B F 0.4701(6) 0.9394(6) 0.0489(6) 0.076 Uani 0.50 1 d PD B -1 F4B F 0.5068(7) 1.0125(8) -0.0173(4) 0.091 Uani 0.50 1 d PD B -1 B1C B -0.2421(4) 0.2813(4) 0.6331(4) 0.081 Uiso 1 1 d D . . F1C F -0.2825(4) 0.2778(5) 0.6769(3) 0.182 Uiso 1 1 d D . . F2C F -0.1961(4) 0.3107(4) 0.6416(4) 0.170 Uiso 1 1 d D . . F3C F -0.2201(4) 0.2245(3) 0.6280(4) 0.139 Uiso 1 1 d D . . F4C F -0.2620(4) 0.3106(4) 0.5836(3) 0.121 Uiso 1 1 d D . . B1E B 0.2895(4) 0.3190(5) 0.6118(4) 0.092 Uani 1 1 d D . . F1E F 0.2965(4) 0.3088(4) 0.5593(2) 0.139 Uani 1 1 d D . . F2E F 0.2956(3) 0.2669(4) 0.6521(3) 0.129 Uani 1 1 d D . . F3E F 0.3325(4) 0.3536(4) 0.6178(4) 0.176 Uani 1 1 d D . . F4E F 0.2367(4) 0.3457(5) 0.6249(3) 0.180 Uani 1 1 d D . . B1F B 0.2283(6) 1.1979(8) -0.1318(5) 0.065 Uani 1 1 d . . . F1F F 0.1731(4) 1.1721(4) -0.1299(3) 0.101 Uani 1 1 d . . . F2F F 0.2738(4) 1.1649(4) -0.1480(3) 0.099 Uani 1 1 d . . . F3F F 0.2212(3) 1.2514(4) -0.1647(3) 0.111 Uani 1 1 d . . . F4F F 0.2266(3) 1.2006(4) -0.0737(3) 0.101 Uani 1 1 d . . . B1G B 0.7685(4) 1.1827(5) -0.1145(4) 0.178 Uani 1 1 d D . . F1G F 0.7187(4) 1.1668(5) -0.1254(4) 0.182 Uani 1 1 d D . . F2G F 0.8148(5) 1.1415(5) -0.1240(5) 0.240 Uani 1 1 d D . . F3G F 0.7647(4) 1.1861(4) -0.0574(3) 0.140 Uani 1 1 d D . . F4G F 0.7825(5) 1.2346(4) -0.1471(4) 0.165 Uani 1 1 d D . . B1H B -0.1999(6) 0.5842(10) -0.0183(6) 0.089 Uani 1 1 d . . . F1H F -0.1587(4) 0.6214(6) -0.0474(3) 0.153 Uani 1 1 d . . . F2H F -0.2437(3) 0.5873(4) -0.0540(3) 0.099 Uani 1 1 d . . . F3H F -0.2207(3) 0.6005(3) 0.0318(2) 0.077 Uani 1 1 d . . . F4H F -0.1727(4) 0.5298(5) -0.0076(4) 0.129 Uani 1 1 d . . . B1I B 0.3230(5) 1.0981(5) 0.4550(4) 0.144 Uani 1 1 d D . . F1I F 0.3128(3) 1.1295(3) 0.4956(3) 0.113 Uani 1 1 d D . . F2I F 0.2818(4) 1.1139(5) 0.4157(3) 0.169 Uani 1 1 d D . . F3I F 0.3770(4) 1.1094(6) 0.4261(4) 0.193 Uani 1 1 d D . . F4I F 0.3219(6) 1.0397(4) 0.4750(4) 0.222 Uani 1 1 d D . . B1J B 0.2903(4) 0.6076(4) -0.0356(4) 0.097 Uiso 1 1 d D . . F1J F 0.3232(3) 0.6442(3) -0.0719(3) 0.083 Uiso 1 1 d D . . F2J F 0.2915(5) 0.6145(6) 0.0200(3) 0.244 Uiso 1 1 d D . . F3J F 0.2330(3) 0.6204(4) -0.0492(4) 0.141 Uiso 1 1 d D . . F4J F 0.3073(5) 0.5504(4) -0.0358(6) 0.253 Uiso 1 1 d D . . B1K B 0.5390(10) 0.7746(12) -0.1980(10) 0.108 Uiso 1 1 d . . . F1K F 0.5153(5) 0.8185(6) -0.1823(5) 0.146 Uiso 1 1 d . . . F2K F 0.5596(5) 0.7758(6) -0.2549(5) 0.163 Uiso 1 1 d . . . F3K F 0.5475(6) 0.7217(7) -0.1639(6) 0.195 Uiso 1 1 d . . . F4K F 0.4844(8) 0.7581(9) -0.2097(8) 0.118 Uiso 0.50 1 d P . . F5K F 0.6027(10) 0.7722(11) -0.1867(10) 0.153 Uiso 0.50 1 d P . . Fe1 Fe 0.24680(7) 0.45549(9) 0.29138(6) 0.059 Uani 1 1 d . . . Fe2 Fe -0.19239(7) 0.43489(9) 0.31080(6) 0.060 Uani 1 1 d . . . Fe3 Fe -0.02841(9) 0.80237(11) 0.36332(7) 0.081 Uani 1 1 d . . . Fe4 Fe 0.51868(7) 0.69713(8) 0.13159(6) 0.055 Uani 1 1 d . . . Fe5 Fe 0.24643(7) 1.05939(8) 0.19594(6) 0.053 Uani 1 1 d . . . Fe6 Fe 0.68670(8) 1.05004(9) 0.21116(8) 0.074 Uani 1 1 d . . . O1 O 0.1479(3) 0.5662(4) 0.1086(3) 0.072 Uani 1 1 d . . . O2 O -0.0986(3) 0.5591(4) 0.1221(3) 0.061 Uani 1 1 d . . . O3 O -0.0066(4) 0.7724(4) 0.1524(3) 0.068 Uani 1 1 d . . . O4 O 0.4858(4) 0.7275(4) 0.3423(3) 0.073 Uani 1 1 d . . . O5 O 0.3292(3) 0.9309(4) 0.3802(3) 0.062 Uani 1 1 d . . . O6 O 0.5761(3) 0.9359(4) 0.3966(3) 0.077 Uani 1 1 d . . . O7 O 0.4710(12) 0.8969(13) 0.2853(12) 0.156 Uiso 0.50 1 d P . . O8 O 0.0471(12) 0.5537(13) 0.2014(11) 0.146 Uiso 0.50 1 d P C 1 O9 O 0.0052(14) 0.6074(15) 0.2201(13) 0.172 Uiso 0.50 1 d P D 2 N1 N 0.1908(4) 0.4619(5) 0.1881(3) 0.064 Uani 1 1 d . . . N2 N 0.1995(4) 0.4273(5) 0.2416(3) 0.067 Uani 1 1 d . . . N3 N 0.2035(4) 0.5537(5) 0.2084(3) 0.070 Uani 1 1 d . . . N4 N 0.2081(4) 0.5334(5) 0.2674(4) 0.061 Uani 1 1 d . . . N5 N 0.2838(4) 0.4995(4) 0.1723(3) 0.054 Uani 1 1 d . . . N6 N 0.3036(4) 0.4733(4) 0.2238(3) 0.057 Uani 1 1 d . . . N7 N 0.1874(4) 0.4349(5) 0.3582(3) 0.072 Uani 1 1 d . . . N8 N 0.2055(4) 0.4060(5) 0.4092(4) 0.067 Uani 1 1 d . . . N9 N 0.2933(4) 0.4842(5) 0.3426(3) 0.055 Uani 1 1 d . . . N10 N 0.2962(4) 0.4484(5) 0.3970(4) 0.059 Uani 1 1 d . . . N11 N 0.2889(4) 0.3742(5) 0.3139(4) 0.064 Uani 1 1 d . . . N12 N 0.2939(4) 0.3556(5) 0.3731(3) 0.063 Uani 1 1 d . . . N13 N -0.2019(4) 0.4471(5) 0.1889(3) 0.075 Uani 1 1 d . . . N14 N -0.2208(5) 0.4185(6) 0.2422(3) 0.081 Uani 1 1 d . . . N15 N -0.1850(4) 0.5358(5) 0.2170(3) 0.063 Uani 1 1 d . . . N16 N -0.2037(4) 0.5191(5) 0.2769(3) 0.067 Uani 1 1 d . . . N17 N -0.1070(4) 0.4610(4) 0.2133(3) 0.058 Uani 1 1 d . . . N18 N -0.1148(4) 0.4339(5) 0.2698(3) 0.060 Uani 1 1 d . . . N19 N -0.2720(4) 0.4355(5) 0.3506(3) 0.066 Uani 1 1 d . . . N20 N -0.2761(4) 0.4027(5) 0.4079(3) 0.065 Uani 1 1 d . . . N21 N -0.1636(4) 0.4533(4) 0.3795(3) 0.051 Uani 1 1 d U . . N22 N -0.1855(4) 0.4247(5) 0.4327(3) 0.066 Uani 1 1 d . . . N23 N -0.1789(4) 0.3481(5) 0.3456(4) 0.076 Uani 1 1 d . . . N24 N -0.1919(5) 0.3327(6) 0.4052(4) 0.084 Uani 1 1 d . . . N25 N -0.0423(5) 0.8760(5) 0.2512(4) 0.076 Uani 1 1 d . . . N26 N -0.0497(5) 0.8755(6) 0.3077(4) 0.079 Uani 1 1 d . . . N27 N 0.0346(5) 0.7979(5) 0.2516(4) 0.083 Uani 1 1 d . . . N28 N 0.0408(5) 0.7917(6) 0.3097(4) 0.092 Uani 1 1 d . . . N29 N -0.0662(5) 0.7749(4) 0.2613(3) 0.064 Uani 1 1 d . . . N30 N -0.0707(4) 0.7596(5) 0.3199(4) 0.067 Uani 1 1 d . . . N31 N 0.0119(5) 0.8467(7) 0.4068(5) 0.105 Uani 1 1 d . . . N32 N -0.0002(6) 0.8332(8) 0.4674(4) 0.141 Uani 1 1 d . . . N33 N -0.0030(5) 0.7278(7) 0.4162(3) 0.091 Uani 1 1 d . . . N34 N -0.0072(5) 0.7298(6) 0.4737(4) 0.089 Uani 1 1 d . . . N35 N -0.0990(5) 0.8112(6) 0.4166(4) 0.087 Uani 1 1 d . . . N36 N -0.0937(4) 0.7957(6) 0.4735(4) 0.088 Uani 1 1 d . . . N37 N 0.4955(4) 0.6240(5) 0.2424(4) 0.066 Uani 1 1 d . . . N38 N 0.5011(4) 0.6233(5) 0.1861(3) 0.059 Uani 1 1 d . . . N39 N 0.5567(4) 0.6997(5) 0.2410(4) 0.065 Uani 1 1 d . . . N40 N 0.5752(4) 0.7063(4) 0.1829(3) 0.057 Uani 1 1 d . . . N41 N 0.4535(4) 0.7229(5) 0.2346(4) 0.067 Uani 1 1 d . . . N42 N 0.4595(5) 0.7382(5) 0.1746(3) 0.068 Uani 1 1 d . . . N43 N 0.4599(4) 0.6899(4) 0.0797(3) 0.051 Uani 1 1 d . . . N44 N 0.4750(4) 0.7058(4) 0.0211(4) 0.053 Uani 1 1 d . . . N45 N 0.5791(4) 0.6522(4) 0.0847(3) 0.051 Uani 1 1 d . . . N46 N 0.5741(4) 0.6666(4) 0.0252(3) 0.053 Uani 1 1 d . . . N47 N 0.5375(4) 0.7728(4) 0.0784(3) 0.050 Uani 1 1 d . . . N48 N 0.5482(4) 0.7695(4) 0.0215(3) 0.048 Uani 1 1 d . . . N49 N 0.2123(4) 1.0387(5) 0.3180(4) 0.065 Uani 1 1 d . . . N50 N 0.1965(4) 1.0688(5) 0.2652(4) 0.065 Uani 1 1 d . . . N51 N 0.2586(3) 0.9550(4) 0.2840(4) 0.051 Uani 1 1 d . . . N52 N 0.2492(4) 0.9743(4) 0.2282(3) 0.053 Uani 1 1 d . . . N53 N 0.3159(4) 1.0324(4) 0.2931(3) 0.053 Uani 1 1 d . . . N54 N 0.3138(4) 1.0611(4) 0.2369(3) 0.057 Uani 1 1 d . . . N55 N 0.2444(4) 1.1464(5) 0.1636(4) 0.059 Uani 1 1 d . . . N56 N 0.2437(4) 1.1634(4) 0.1060(4) 0.053 Uani 1 1 d . . . N57 N 0.1789(4) 1.0590(5) 0.1523(3) 0.063 Uani 1 1 d . . . N58 N 0.1795(4) 1.0946(4) 0.0951(4) 0.058 Uani 1 1 d . . . N59 N 0.2975(4) 1.0450(4) 0.1265(3) 0.052 Uani 1 1 d . . . N60 N 0.2808(4) 1.0752(4) 0.0745(3) 0.050 Uani 1 1 d . . . N61 N 0.7099(4) 1.0056(5) 0.3300(4) 0.075 Uani 1 1 d . . . N62 N 0.7347(5) 1.0322(5) 0.2759(4) 0.084 Uani 1 1 d . . . N63 N 0.6096(5) 1.0412(5) 0.3181(4) 0.076 Uani 1 1 d . . . N64 N 0.6221(5) 1.0789(5) 0.2626(4) 0.077 Uani 1 1 d . . . N65 N 0.6499(4) 0.9472(5) 0.2952(4) 0.068 Uani 1 1 d . . . N66 N 0.6607(4) 0.9712(5) 0.2365(4) 0.069 Uani 1 1 d . . . N67 N 0.7150(5) 1.1324(5) 0.1860(4) 0.086 Uani 1 1 d . . . N68 N 0.7286(5) 1.1489(5) 0.1280(5) 0.093 Uani 1 1 d . . . N69 N 0.6385(4) 1.0683(5) 0.1459(4) 0.070 Uani 1 1 d . . . N70 N 0.6620(5) 1.0971(5) 0.0921(4) 0.076 Uani 1 1 d . . . N71 N 0.7524(4) 1.0224(4) 0.1600(4) 0.057 Uani 1 1 d . . . N72 N 0.7585(5) 1.0539(5) 0.1033(4) 0.071 Uani 1 1 d . . . C1 C 0.0731(5) 0.6326(7) 0.0610(4) 0.071 Uani 1 1 d . . . C2 C 0.0260(5) 0.5974(6) 0.0606(4) 0.056 Uani 1 1 d . . . C3 C -0.0313(6) 0.6235(5) 0.0662(4) 0.056 Uani 1 1 d . . . C4 C -0.0421(5) 0.6803(6) 0.0768(4) 0.061 Uani 1 1 d . . . C5 C 0.0047(6) 0.7122(6) 0.0791(4) 0.072 Uani 1 1 d . . . C6 C 0.0652(6) 0.6915(7) 0.0718(4) 0.073 Uani 1 1 d . . . C7 C 0.1364(5) 0.5989(6) 0.0533(4) 0.076 Uani 1 1 d . . . H7A H 0.1373 0.5720 0.0261 0.091 Uiso 1 1 calc R . . H7B H 0.1660 0.6276 0.0386 0.091 Uiso 1 1 calc R . . C8 C 0.2103(5) 0.5472(6) 0.1082(4) 0.073 Uani 1 1 d . . . H8A H 0.2334 0.5821 0.0966 0.087 Uiso 1 1 calc R . . H8B H 0.2218 0.5206 0.0807 0.087 Uiso 1 1 calc R . . C9 C 0.2221(5) 0.5139(6) 0.1699(4) 0.060 Uani 1 1 d . . . C10 C 0.1598(5) 0.4330(7) 0.1603(5) 0.077 Uani 1 1 d . . . H10 H 0.1494 0.4474 0.1222 0.092 Uiso 1 1 calc R . . C11 C 0.1453(5) 0.3803(7) 0.1937(4) 0.085 Uani 1 1 d . . . H11 H 0.1237 0.3512 0.1852 0.102 Uiso 1 1 calc R . . C12 C 0.1720(5) 0.3806(7) 0.2461(5) 0.075 Uani 1 1 d . . . H12 H 0.1696 0.3501 0.2795 0.090 Uiso 1 1 calc R . . C13 C 0.1842(6) 0.6129(7) 0.2005(5) 0.083 Uani 1 1 d . . . H13 H 0.1787 0.6378 0.1642 0.100 Uiso 1 1 calc R . . C14 C 0.1740(6) 0.6316(8) 0.2515(5) 0.092 Uani 1 1 d . . . H14 H 0.1595 0.6699 0.2583 0.111 Uiso 1 1 calc R . . C15 C 0.1903(5) 0.5810(6) 0.2907(5) 0.073 Uani 1 1 d . . . H15 H 0.1889 0.5800 0.3307 0.088 Uiso 1 1 calc R . . C16 C 0.3292(4) 0.5050(5) 0.1301(4) 0.051 Uani 1 1 d . . . H16 H 0.3259 0.5212 0.0906 0.061 Uiso 1 1 calc R . . C17 C 0.3798(5) 0.4832(6) 0.1547(5) 0.070 Uani 1 1 d . . . H17 H 0.4184 0.4803 0.1363 0.084 Uiso 1 1 calc R . . C18 C 0.3622(5) 0.4660(6) 0.2134(4) 0.064 Uani 1 1 d . . . H18 H 0.3884 0.4510 0.2421 0.077 Uiso 1 1 calc R . . C19 C 0.1282(5) 0.4402(6) 0.3677(4) 0.070 Uani 1 1 d . . . C20 C 0.1116(6) 0.4140(7) 0.4252(4) 0.087 Uani 1 1 d . . . H20 H 0.0727 0.4120 0.4430 0.105 Uiso 1 1 calc R . . C21 C 0.1609(6) 0.3926(7) 0.4495(4) 0.077 Uani 1 1 d . . . C22 C 0.0860(5) 0.4707(8) 0.3226(5) 0.099 Uani 1 1 d . . . H22A H 0.1084 0.4818 0.2853 0.148 Uiso 1 1 calc R . . H22B H 0.0654 0.5064 0.3340 0.148 Uiso 1 1 calc R . . H22C H 0.0576 0.4434 0.3199 0.148 Uiso 1 1 calc R . . C23 C 0.1714(6) 0.3582(6) 0.5104(4) 0.080 Uani 1 1 d . . . H23A H 0.1920 0.3821 0.5296 0.121 Uiso 1 1 calc R . . H23B H 0.1952 0.3207 0.5083 0.121 Uiso 1 1 calc R . . H23C H 0.1337 0.3499 0.5322 0.121 Uiso 1 1 calc R . . C24 C 0.3248(6) 0.5289(6) 0.3422(6) 0.079 Uani 1 1 d . . . C25 C 0.3444(5) 0.5229(7) 0.3972(5) 0.086 Uani 1 1 d . . . H25 H 0.3672 0.5492 0.4088 0.103 Uiso 1 1 calc R . . C26 C 0.3247(6) 0.4723(7) 0.4303(5) 0.083 Uani 1 1 d . . . C27 C 0.3311(5) 0.5782(6) 0.2907(5) 0.080 Uani 1 1 d . . . H27A H 0.3548 0.5630 0.2594 0.120 Uiso 1 1 calc R . . H27B H 0.3505 0.6098 0.3005 0.120 Uiso 1 1 calc R . . H27C H 0.2923 0.5941 0.2786 0.120 Uiso 1 1 calc R . . C28 C 0.3363(7) 0.4444(8) 0.4920(5) 0.108 Uani 1 1 d . . . H28A H 0.3011 0.4513 0.5176 0.162 Uiso 1 1 calc R . . H28B H 0.3688 0.4624 0.5027 0.162 Uiso 1 1 calc R . . H28C H 0.3466 0.4016 0.4955 0.162 Uiso 1 1 calc R . . C29 C 0.3147(5) 0.3310(6) 0.2901(5) 0.059 Uani 1 1 d . . . C30 C 0.3364(6) 0.2848(6) 0.3327(4) 0.078 Uani 1 1 d . . . H30 H 0.3567 0.2482 0.3267 0.094 Uiso 1 1 calc R . . C31 C 0.3238(6) 0.3007(6) 0.3818(5) 0.076 Uani 1 1 d . . . C32 C 0.3184(7) 0.3363(6) 0.2256(4) 0.083 Uani 1 1 d . . . H32A H 0.3024 0.3020 0.2169 0.124 Uiso 1 1 calc R . . H32B H 0.3594 0.3373 0.2098 0.124 Uiso 1 1 calc R . . H32C H 0.2957 0.3729 0.2084 0.124 Uiso 1 1 calc R . . C33 C 0.3348(7) 0.2675(7) 0.4433(5) 0.104 Uani 1 1 d . . . H33A H 0.3568 0.2289 0.4419 0.156 Uiso 1 1 calc R . . H33B H 0.2972 0.2614 0.4661 0.156 Uiso 1 1 calc R . . H33C H 0.3574 0.2910 0.4609 0.156 Uiso 1 1 calc R . . C34 C 0.2674(5) 0.3946(6) 0.4108(4) 0.062 Uani 1 1 d . . . H34 H 0.2751 0.3746 0.4508 0.075 Uiso 1 1 calc R . . C35 C 0.0358(6) 0.5367(7) 0.0520(5) 0.086 Uani 1 1 d . . . H35A H 0.0511 0.5366 0.0121 0.128 Uiso 1 1 calc R . . H35B H -0.0012 0.5183 0.0602 0.128 Uiso 1 1 calc R . . H35C H 0.0643 0.5142 0.0778 0.128 Uiso 1 1 calc R . . C36 C -0.0834(5) 0.5893(6) 0.0640(4) 0.064 Uani 1 1 d . . . H36A H -0.1168 0.6169 0.0492 0.076 Uiso 1 1 calc R . . H36B H -0.0727 0.5603 0.0387 0.076 Uiso 1 1 calc R . . C37 C -0.1421(5) 0.5183(6) 0.1233(4) 0.062 Uani 1 1 d . . . H37A H -0.1260 0.4867 0.1022 0.074 Uiso 1 1 calc R . . H37B H -0.1772 0.5396 0.1053 0.074 Uiso 1 1 calc R . . C38 C -0.1580(4) 0.4917(6) 0.1866(4) 0.050 Uani 1 1 d . . . C39 C -0.2280(6) 0.4345(7) 0.1498(5) 0.081 Uani 1 1 d . . . H39 H -0.2212 0.4495 0.1098 0.098 Uiso 1 1 calc R . . C40 C -0.2684(6) 0.3949(8) 0.1761(6) 0.104 Uani 1 1 d . . . H40 H -0.2943 0.3773 0.1579 0.125 Uiso 1 1 calc R . . C41 C -0.2631(5) 0.3866(7) 0.2328(5) 0.076 Uani 1 1 d . . . H41 H -0.2857 0.3619 0.2619 0.091 Uiso 1 1 calc R . . C42 C -0.2020(5) 0.5941(6) 0.1997(5) 0.066 Uani 1 1 d . . . H42 H -0.1965 0.6162 0.1616 0.079 Uiso 1 1 calc R . . C43 C -0.2287(5) 0.6164(6) 0.2463(5) 0.072 Uani 1 1 d . . . H43 H -0.2428 0.6565 0.2468 0.086 Uiso 1 1 calc R . . C44 C -0.2305(5) 0.5690(6) 0.2915(5) 0.066 Uani 1 1 d . . . H44 H -0.2487 0.5713 0.3287 0.080 Uiso 1 1 calc R . . C45 C -0.0501(5) 0.4529(6) 0.1926(5) 0.072 Uani 1 1 d . . . H45 H -0.0335 0.4697 0.1554 0.086 Uiso 1 1 calc R . . C46 C -0.0216(6) 0.4169(6) 0.2342(4) 0.070 Uani 1 1 d . . . H46 H 0.0182 0.4008 0.2322 0.084 Uiso 1 1 calc R . . C47 C -0.0639(5) 0.4084(6) 0.2817(5) 0.071 Uani 1 1 d . . . H47 H -0.0557 0.3862 0.3185 0.085 Uiso 1 1 calc R . . C48 C -0.3274(5) 0.4551(6) 0.3420(5) 0.071 Uani 1 1 d . . . C49 C -0.3673(7) 0.4360(8) 0.3902(5) 0.109 Uani 1 1 d . . . H49 H -0.4087 0.4437 0.3925 0.130 Uiso 1 1 calc R . . C50 C -0.3352(6) 0.4047(6) 0.4320(4) 0.074 Uani 1 1 d . . . C51 C -0.3418(6) 0.4944(9) 0.2876(5) 0.118 Uani 1 1 d . . . H51A H -0.3621 0.5318 0.2952 0.177 Uiso 1 1 calc R . . H51B H -0.3671 0.4751 0.2684 0.177 Uiso 1 1 calc R . . H51C H -0.3056 0.5024 0.2628 0.177 Uiso 1 1 calc R . . C52 C -0.3507(6) 0.3732(8) 0.4930(5) 0.109 Uani 1 1 d . . . H52A H -0.3828 0.3967 0.5108 0.163 Uiso 1 1 calc R . . H52B H -0.3163 0.3685 0.5148 0.163 Uiso 1 1 calc R . . H52C H -0.3628 0.3340 0.4930 0.163 Uiso 1 1 calc R . . C53 C -0.1322(5) 0.4931(6) 0.3910(4) 0.065 Uani 1 1 d . . . C54 C -0.1375(6) 0.4946(6) 0.4492(4) 0.076 Uani 1 1 d . . . H54 H -0.1212 0.5210 0.4671 0.091 Uiso 1 1 calc R . . C55 C -0.1714(5) 0.4500(6) 0.4750(4) 0.058 Uani 1 1 d . . . C56 C -0.0980(5) 0.5371(6) 0.3438(4) 0.070 Uani 1 1 d . . . H56A H -0.0940 0.5232 0.3075 0.105 Uiso 1 1 calc R . . H56B H -0.0590 0.5392 0.3554 0.105 Uiso 1 1 calc R . . H56C H -0.1195 0.5766 0.3387 0.105 Uiso 1 1 calc R . . C57 C -0.1913(5) 0.4307(6) 0.5381(4) 0.068 Uani 1 1 d . . . H57A H -0.1740 0.4541 0.5603 0.102 Uiso 1 1 calc R . . H57B H -0.1786 0.3885 0.5509 0.102 Uiso 1 1 calc R . . H57C H -0.2341 0.4369 0.5437 0.102 Uiso 1 1 calc R . . C58 C -0.1542(6) 0.2969(6) 0.3314(5) 0.070 Uani 1 1 d . . . C59 C -0.1553(6) 0.2537(7) 0.3791(5) 0.084 Uani 1 1 d . . . H59 H -0.1420 0.2133 0.3789 0.101 Uiso 1 1 calc R . . C60 C -0.1773(7) 0.2737(7) 0.4272(6) 0.095 Uani 1 1 d . . . C61 C -0.1361(7) 0.2911(7) 0.2707(6) 0.101 Uani 1 1 d . . . H61A H -0.0971 0.2696 0.2684 0.151 Uiso 1 1 d R . . H61B H -0.1351 0.3307 0.2462 0.151 Uiso 1 1 d R . . H61C H -0.1643 0.2693 0.2577 0.151 Uiso 1 1 d R . . C62 C -0.1856(9) 0.2467(9) 0.4883(6) 0.152 Uani 1 1 d . . . H62A H -0.1905 0.2044 0.4927 0.228 Uiso 1 1 calc R . . H62B H -0.2207 0.2665 0.5059 0.228 Uiso 1 1 calc R . . H62C H -0.1513 0.2512 0.5072 0.228 Uiso 1 1 calc R . . C63 C -0.2226(5) 0.3792(6) 0.4336(4) 0.065 Uani 1 1 d . . . H63 H -0.2333 0.3607 0.4745 0.078 Uiso 1 1 calc R . . C64 C -0.1025(5) 0.7102(6) 0.0875(5) 0.073 Uani 1 1 d . . . H64A H -0.1269 0.7061 0.0579 0.110 Uiso 1 1 calc R . . H64B H -0.1000 0.7524 0.0864 0.110 Uiso 1 1 calc R . . H64C H -0.1201 0.6917 0.1253 0.110 Uiso 1 1 calc R . . C65 C -0.0030(7) 0.7763(7) 0.0899(5) 0.098 Uani 1 1 d . . . H65A H 0.0308 0.7981 0.0709 0.117 Uiso 1 1 calc R . . H65B H -0.0392 0.7978 0.0743 0.117 Uiso 1 1 calc R . . C66 C -0.0248(6) 0.8294(6) 0.1665(5) 0.079 Uani 1 1 d . . . H66A H -0.0644 0.8440 0.1543 0.095 Uiso 1 1 calc R . . H66B H 0.0029 0.8586 0.1472 0.095 Uiso 1 1 calc R . . C67 C -0.0255(5) 0.8204(6) 0.2326(5) 0.064 Uani 1 1 d . . . C68 C -0.0501(6) 0.9328(6) 0.2193(5) 0.076 Uani 1 1 d . . . H68 H -0.0467 0.9436 0.1786 0.091 Uiso 1 1 calc R . . C69 C -0.0638(5) 0.9708(7) 0.2567(5) 0.076 Uani 1 1 d . . . H69 H -0.0715 1.0128 0.2475 0.092 Uiso 1 1 calc R . . C70 C -0.0640(6) 0.9328(8) 0.3133(5) 0.087 Uani 1 1 d . . . H70 H -0.0727 0.9458 0.3486 0.105 Uiso 1 1 calc R . . C71 C 0.0871(6) 0.7934(7) 0.2222(5) 0.088 Uani 1 1 d . . . H71 H 0.0935 0.7986 0.1817 0.105 Uiso 1 1 calc R . . C72 C 0.1311(6) 0.7801(7) 0.2593(5) 0.086 Uani 1 1 d . . . H72 H 0.1722 0.7728 0.2508 0.103 Uiso 1 1 calc R . . C73 C 0.0977(6) 0.7803(8) 0.3140(5) 0.111 Uani 1 1 d . . . H73 H 0.1148 0.7729 0.3494 0.133 Uiso 1 1 calc R . . C74 C -0.1045(6) 0.7507(6) 0.2386(5) 0.080 Uani 1 1 d . . . H74 H -0.1109 0.7573 0.1992 0.096 Uiso 1 1 calc R . . C75 C -0.1343(6) 0.7131(6) 0.2845(5) 0.086 Uani 1 1 d . . . H75 H -0.1641 0.6883 0.2836 0.103 Uiso 1 1 calc R . . C76 C -0.1082(6) 0.7223(6) 0.3318(5) 0.079 Uani 1 1 d . . . H76 H -0.1181 0.7019 0.3698 0.095 Uiso 1 1 calc R . . C77 C 0.0520(7) 0.8852(9) 0.3998(6) 0.117 Uani 1 1 d . . . C78 C 0.0612(9) 0.9042(11) 0.4485(7) 0.158 Uani 1 1 d . . . H78 H 0.0844 0.9343 0.4522 0.190 Uiso 1 1 calc R . . C79 C 0.0268(8) 0.8671(11) 0.4922(5) 0.156 Uani 1 1 d . . . C80 C 0.0746(8) 0.9154(9) 0.3404(6) 0.139 Uani 1 1 d . . . H80A H 0.1151 0.8994 0.3318 0.208 Uiso 1 1 calc R . . H80B H 0.0734 0.9582 0.3387 0.208 Uiso 1 1 calc R . . H80C H 0.0500 0.9082 0.3123 0.208 Uiso 1 1 calc R . . C81 C 0.0165(9) 0.8653(10) 0.5575(8) 0.158 Uani 1 1 d U . . H81A H -0.0239 0.8810 0.5671 0.237 Uiso 1 1 calc R . . H81B H 0.0438 0.8896 0.5684 0.237 Uiso 1 1 calc R . . H81C H 0.0231 0.8242 0.5784 0.237 Uiso 1 1 calc R . . C82 C 0.0258(6) 0.6726(9) 0.4128(5) 0.099 Uani 1 1 d . . . C83 C 0.0412(7) 0.6436(9) 0.4664(5) 0.112 Uani 1 1 d . . . H83 H 0.0626 0.6057 0.4747 0.134 Uiso 1 1 calc R . . C84 C 0.0213(6) 0.6773(9) 0.5045(7) 0.123 Uani 1 1 d . . . C85 C 0.0362(6) 0.6521(9) 0.3565(5) 0.118 Uani 1 1 d . . . H85A H 0.0478 0.6093 0.3636 0.177 Uiso 1 1 calc R . . H85B H 0.0675 0.6731 0.3323 0.177 Uiso 1 1 calc R . . H85C H 0.0002 0.6606 0.3370 0.177 Uiso 1 1 calc R . . C86 C 0.0263(7) 0.6696(8) 0.5677(4) 0.124 Uani 1 1 d . . . H86A H -0.0118 0.6615 0.5888 0.187 Uiso 1 1 calc R . . H86B H 0.0384 0.7060 0.5757 0.187 Uiso 1 1 calc R . . H86C H 0.0554 0.6363 0.5798 0.187 Uiso 1 1 calc R . . C87 C -0.1580(6) 0.8228(6) 0.4135(5) 0.077 Uani 1 1 d . . . C88 C -0.1875(7) 0.8170(9) 0.4689(7) 0.119 Uani 1 1 d . . . H88 H -0.2283 0.8245 0.4785 0.143 Uiso 1 1 calc R . . C89 C -0.1444(8) 0.7980(9) 0.5067(6) 0.122 Uani 1 1 d . . . C90 C -0.1856(6) 0.8424(6) 0.3575(5) 0.083 Uani 1 1 d . . . H90A H -0.1558 0.8387 0.3256 0.125 Uiso 1 1 calc R . . H90B H -0.2020 0.8839 0.3536 0.125 Uiso 1 1 calc R . . H90C H -0.2170 0.8174 0.3569 0.125 Uiso 1 1 calc R . . C91 C -0.1518(8) 0.7841(9) 0.5729(5) 0.134 Uani 1 1 d . . . H91A H -0.1384 0.7423 0.5870 0.201 Uiso 1 1 calc R . . H91B H -0.1932 0.7916 0.5862 0.201 Uiso 1 1 calc R . . H91C H -0.1284 0.8095 0.5874 0.201 Uiso 1 1 calc R . . C92 C -0.0359(6) 0.7863(8) 0.4920(6) 0.099 Uani 1 1 d . . . H92 H -0.0386 0.7803 0.5347 0.118 Uiso 1 1 calc R . . C93 C 0.1168(7) 0.7213(8) 0.0751(5) 0.121 Uani 1 1 d . . . H93A H 0.1405 0.6971 0.1045 0.181 Uiso 1 1 calc R . . H93B H 0.1044 0.7601 0.0849 0.181 Uiso 1 1 calc R . . H93C H 0.1402 0.7268 0.0379 0.181 Uiso 1 1 calc R . . C94 C 0.4683(8) 0.7822(7) 0.4183(5) 0.087 Uani 1 1 d . . . C95 C 0.4095(6) 0.8143(6) 0.4210(4) 0.066 Uani 1 1 d . . . C96 C 0.4037(6) 0.8691(6) 0.4355(5) 0.068 Uani 1 1 d . . . C97 C 0.4514(5) 0.8979(5) 0.4441(4) 0.055 Uani 1 1 d . . . C98 C 0.5079(6) 0.8659(7) 0.4409(4) 0.073 Uani 1 1 d . . . C99 C 0.5172(7) 0.8102(7) 0.4276(5) 0.088 Uani 1 1 d . . . C100 C 0.4760(7) 0.7184(7) 0.4072(4) 0.100 Uani 1 1 d . . . H10A H 0.5101 0.6952 0.4255 0.120 Uiso 1 1 calc R . . H10B H 0.4405 0.6976 0.4219 0.120 Uiso 1 1 calc R . . C101 C 0.4880(7) 0.6719(6) 0.3262(4) 0.084 Uani 1 1 d . . . H10C H 0.4501 0.6548 0.3381 0.101 Uiso 1 1 calc R . . H10D H 0.5190 0.6441 0.3454 0.101 Uiso 1 1 calc R . . C102 C 0.5009(6) 0.6798(6) 0.2617(4) 0.074 Uani 1 1 d . . . C103 C 0.4927(6) 0.5673(6) 0.2747(6) 0.073 Uani 1 1 d . . . H103 H 0.4906 0.5563 0.3153 0.088 Uiso 1 1 calc R . . C104 C 0.4934(5) 0.5304(6) 0.2377(6) 0.081 Uani 1 1 d . . . H104 H 0.4914 0.4887 0.2466 0.097 Uiso 1 1 calc R . . C105 C 0.4978(5) 0.5685(5) 0.1818(5) 0.056 Uani 1 1 d . . . H105 H 0.4983 0.5555 0.1467 0.068 Uiso 1 1 calc R . . C106 C 0.6023(6) 0.7098(6) 0.2710(5) 0.072 Uani 1 1 d . . . H106 H 0.6009 0.7060 0.3114 0.086 Uiso 1 1 calc R . . C107 C 0.6491(6) 0.7260(6) 0.2324(5) 0.077 Uani 1 1 d . . . H107 H 0.6855 0.7371 0.2397 0.093 Uiso 1 1 calc R . . C108 C 0.6297(5) 0.7222(5) 0.1777(5) 0.061 Uani 1 1 d . . . H108 H 0.6531 0.7302 0.1422 0.073 Uiso 1 1 calc R . . C109 C 0.4043(6) 0.7527(6) 0.2572(5) 0.080 Uani 1 1 d . . . H109 H 0.3914 0.7498 0.2967 0.096 Uiso 1 1 calc R . . C110 C 0.3781(6) 0.7867(6) 0.2128(5) 0.070 Uani 1 1 d . . . H110 H 0.3421 0.8110 0.2138 0.085 Uiso 1 1 calc R . . C111 C 0.4162(6) 0.7781(6) 0.1644(5) 0.068 Uani 1 1 d . . . H111 H 0.4103 0.8001 0.1269 0.082 Uiso 1 1 calc R . . C112 C 0.4032(5) 0.6807(6) 0.0844(5) 0.060 Uani 1 1 d . . . C113 C 0.3826(6) 0.6914(6) 0.0318(5) 0.069 Uani 1 1 d . . . H113 H 0.3440 0.6876 0.0236 0.082 Uiso 1 1 calc R . . C114 C 0.4305(5) 0.7095(6) -0.0084(5) 0.065 Uani 1 1 d . . . C115 C 0.3670(5) 0.6621(6) 0.1400(5) 0.074 Uani 1 1 d . . . H11A H 0.3504 0.6250 0.1400 0.110 Uiso 1 1 calc R . . H11B H 0.3352 0.6931 0.1446 0.110 Uiso 1 1 calc R . . H11C H 0.3918 0.6561 0.1718 0.110 Uiso 1 1 calc R . . C116 C 0.4344(6) 0.7251(8) -0.0736(5) 0.098 Uani 1 1 d . . . H11D H 0.4399 0.7674 -0.0866 0.147 Uiso 1 1 calc R . . H11E H 0.3982 0.7168 -0.0868 0.147 Uiso 1 1 calc R . . H11F H 0.4677 0.7014 -0.0892 0.147 Uiso 1 1 calc R . . C117 C 0.6204(5) 0.6081(5) 0.0909(4) 0.053 Uani 1 1 d . . . C118 C 0.6432(5) 0.5928(5) 0.0392(5) 0.060 Uani 1 1 d . . . H118 H 0.6734 0.5627 0.0332 0.072 Uiso 1 1 calc R . . C119 C 0.6117(5) 0.6315(6) -0.0020(5) 0.058 Uani 1 1 d . . . C120 C 0.6405(5) 0.5774(6) 0.1494(5) 0.075 Uani 1 1 d . . . H12A H 0.6362 0.6060 0.1748 0.112 Uiso 1 1 calc R . . H12B H 0.6816 0.5617 0.1448 0.112 Uiso 1 1 calc R . . H12C H 0.6163 0.5447 0.1662 0.112 Uiso 1 1 calc R . . C121 C 0.6191(5) 0.6381(6) -0.0662(4) 0.067 Uani 1 1 d . . . H12D H 0.5836 0.6278 -0.0794 0.101 Uiso 1 1 calc R . . H12E H 0.6528 0.6114 -0.0770 0.101 Uiso 1 1 calc R . . H12F H 0.6259 0.6792 -0.0841 0.101 Uiso 1 1 calc R . . C122 C 0.5532(5) 0.8240(6) 0.0814(4) 0.061 Uani 1 1 d . . . C123 C 0.5711(5) 0.8577(5) 0.0256(4) 0.058 Uani 1 1 d . . . H123 H 0.5824 0.8970 0.0167 0.069 Uiso 1 1 calc R . . C124 C 0.5685(5) 0.8226(6) -0.0104(5) 0.062 Uani 1 1 d . . . C125 C 0.5445(6) 0.8480(6) 0.1369(4) 0.076 Uani 1 1 d . . . H12G H 0.5134 0.8282 0.1627 0.115 Uiso 1 1 calc R . . H12H H 0.5333 0.8909 0.1280 0.115 Uiso 1 1 calc R . . H12I H 0.5811 0.8403 0.1555 0.115 Uiso 1 1 calc R . . C126 C 0.5829(5) 0.8316(6) -0.0748(4) 0.068 Uani 1 1 d . . . H12J H 0.5487 0.8251 -0.0927 0.102 Uiso 1 1 calc R . . H12K H 0.6160 0.8034 -0.0835 0.102 Uiso 1 1 calc R . . H12L H 0.5934 0.8722 -0.0899 0.102 Uiso 1 1 calc R . . C127 C 0.5348(5) 0.7189(5) 0.0025(5) 0.054 Uani 1 1 d . . . H127 H 0.5402 0.7267 -0.0403 0.065 Uiso 1 1 calc R . . C128 C 0.3576(6) 0.7881(7) 0.4083(5) 0.097 Uani 1 1 d . . . H12M H 0.3274 0.8200 0.3955 0.145 Uiso 1 1 calc R . . H12N H 0.3420 0.7618 0.4430 0.145 Uiso 1 1 calc R . . H12O H 0.3693 0.7654 0.3781 0.145 Uiso 1 1 calc R . . C129 C 0.3424(5) 0.9031(6) 0.4367(4) 0.068 Uani 1 1 d . . . H12P H 0.3128 0.8752 0.4543 0.082 Uiso 1 1 calc R . . H12Q H 0.3410 0.9335 0.4605 0.082 Uiso 1 1 calc R . . C130 C 0.2771(5) 0.9687(6) 0.3825(4) 0.060 Uani 1 1 d . . . H13A H 0.2810 0.9992 0.4049 0.072 Uiso 1 1 calc R . . H13B H 0.2439 0.9458 0.4007 0.072 Uiso 1 1 calc R . . C131 C 0.2665(4) 0.9987(5) 0.3195(5) 0.054 Uani 1 1 d . . . C132 C 0.1730(6) 1.0508(6) 0.3606(5) 0.075 Uani 1 1 d . . . H132 H 0.1733 1.0329 0.4001 0.090 Uiso 1 1 calc R . . C133 C 0.1312(6) 1.0950(6) 0.3355(6) 0.080 Uani 1 1 d . . . H133 H 0.0996 1.1162 0.3538 0.096 Uiso 1 1 calc R . . C134 C 0.1478(6) 1.1001(6) 0.2771(5) 0.070 Uani 1 1 d . . . H134 H 0.1255 1.1243 0.2484 0.084 Uiso 1 1 calc R . . C135 C 0.2559(4) 0.8964(5) 0.3016(5) 0.055 Uani 1 1 d . . . H135 H 0.2605 0.8740 0.3392 0.066 Uiso 1 1 calc R . . C136 C 0.2456(5) 0.8754(6) 0.2556(5) 0.066 Uani 1 1 d . . . H136 H 0.2421 0.8352 0.2540 0.079 Uiso 1 1 calc R . . C137 C 0.2410(5) 0.9269(6) 0.2087(5) 0.062 Uani 1 1 d . . . H137 H 0.2333 0.9265 0.1706 0.075 Uiso 1 1 calc R . . C138 C 0.3638(5) 1.0424(6) 0.3174(4) 0.065 Uani 1 1 d . . . H138 H 0.3751 1.0254 0.3547 0.078 Uiso 1 1 calc R . . C139 C 0.3927(6) 1.0839(6) 0.2741(4) 0.072 Uani 1 1 d . . . H139 H 0.4267 1.1022 0.2769 0.086 Uiso 1 1 calc R . . C140 C 0.3604(5) 1.0922(6) 0.2264(5) 0.071 Uani 1 1 d . . . H140 H 0.3705 1.1172 0.1906 0.085 Uiso 1 1 calc R . . C141 C 0.2501(5) 1.1950(6) 0.1831(5) 0.069 Uani 1 1 d . . . C142 C 0.2522(6) 1.2439(7) 0.1367(6) 0.085 Uani 1 1 d . . . H142 H 0.2555 1.2840 0.1386 0.102 Uiso 1 1 calc R . . C143 C 0.2484(5) 1.2222(6) 0.0878(5) 0.065 Uani 1 1 d . . . C144 C 0.2560(7) 1.1955(7) 0.2449(5) 0.096 Uani 1 1 d . . . H14A H 0.2422 1.1591 0.2693 0.145 Uiso 1 1 calc R . . H14B H 0.2324 1.2301 0.2557 0.145 Uiso 1 1 calc R . . H14C H 0.2972 1.1974 0.2501 0.145 Uiso 1 1 calc R . . C145 C 0.2513(6) 1.2544(6) 0.0273(5) 0.079 Uani 1 1 d . . . H14D H 0.2865 1.2390 0.0062 0.119 Uiso 1 1 calc R . . H14E H 0.2528 1.2968 0.0258 0.119 Uiso 1 1 calc R . . H14F H 0.2165 1.2486 0.0100 0.119 Uiso 1 1 calc R . . C146 C 0.1254(5) 1.0365(7) 0.1576(5) 0.075 Uani 1 1 d . . . C147 C 0.0941(6) 1.0574(7) 0.1097(6) 0.095 Uani 1 1 d . . . H147 H 0.0564 1.0477 0.1046 0.114 Uiso 1 1 calc R . . C148 C 0.1281(5) 1.0940(6) 0.0721(5) 0.067 Uani 1 1 d . . . C149 C 0.1073(5) 0.9928(7) 0.2128(5) 0.092 Uani 1 1 d . . . H14G H 0.1398 0.9624 0.2222 0.138 Uiso 1 1 calc R . . H14H H 0.0731 0.9740 0.2071 0.138 Uiso 1 1 calc R . . H14I H 0.0974 1.0143 0.2442 0.138 Uiso 1 1 calc R . . C150 C 0.1182(5) 1.1302(6) 0.0137(5) 0.078 Uani 1 1 d . . . H15A H 0.0793 1.1249 0.0040 0.118 Uiso 1 1 calc R . . H15B H 0.1481 1.1172 -0.0145 0.118 Uiso 1 1 calc R . . H15C H 0.1206 1.1722 0.0135 0.118 Uiso 1 1 calc R . . C151 C 0.3412(5) 1.0052(5) 0.1145(4) 0.054 Uani 1 1 d . . . C152 C 0.3494(5) 1.0083(5) 0.0538(5) 0.058 Uani 1 1 d . . . H152 H 0.3774 0.9849 0.0337 0.069 Uiso 1 1 calc R . . C153 C 0.3088(5) 1.0520(5) 0.0306(5) 0.052 Uani 1 1 d . . . C154 C 0.3751(5) 0.9634(5) 0.1588(5) 0.070 Uani 1 1 d . . . H15D H 0.3641 0.9740 0.1963 0.105 Uiso 1 1 calc R . . H15E H 0.4171 0.9662 0.1485 0.105 Uiso 1 1 calc R . . H15F H 0.3660 0.9226 0.1605 0.105 Uiso 1 1 calc R . . C155 C 0.2999(5) 1.0733(5) -0.0311(4) 0.062 Uani 1 1 d . . . H15G H 0.2602 1.0668 -0.0376 0.092 Uiso 1 1 calc R . . H15H H 0.3285 1.0514 -0.0542 0.092 Uiso 1 1 calc R . . H15I H 0.3050 1.1158 -0.0421 0.092 Uiso 1 1 calc R . . C156 C 0.2342(5) 1.1211(5) 0.0737(5) 0.052 Uani 1 1 d . . . H156 H 0.2310 1.1420 0.0330 0.063 Uiso 1 1 calc R . . C157 C 0.4450(5) 0.9587(6) 0.4565(6) 0.077 Uani 1 1 d . . . H15J H 0.4577 0.9870 0.4219 0.116 Uiso 1 1 calc R . . H15K H 0.4694 0.9597 0.4872 0.116 Uiso 1 1 calc R . . H15L H 0.4039 0.9695 0.4685 0.116 Uiso 1 1 calc R . . C158 C 0.5620(6) 0.8953(9) 0.4484(5) 0.115 Uani 1 1 d . . . H15M H 0.5536 0.9165 0.4807 0.138 Uiso 1 1 calc R . . H15N H 0.5953 0.8648 0.4569 0.138 Uiso 1 1 calc R . . C159 C 0.6353(6) 0.9551(7) 0.3955(5) 0.083 Uani 1 1 d . . . H15O H 0.6644 0.9204 0.4053 0.100 Uiso 1 1 calc R . . H15P H 0.6357 0.9817 0.4228 0.100 Uiso 1 1 calc R . . C160 C 0.6481(6) 0.9879(6) 0.3338(5) 0.071 Uani 1 1 d . . . C161 C 0.7464(5) 1.0026(7) 0.3713(6) 0.078 Uani 1 1 d . . . H161 H 0.7396 0.9871 0.4112 0.094 Uiso 1 1 calc R . . C162 C 0.7976(6) 1.0282(8) 0.3413(7) 0.108 Uani 1 1 d . . . H162 H 0.8321 1.0326 0.3577 0.130 Uiso 1 1 calc R . . C163 C 0.7878(6) 1.0453(6) 0.2843(6) 0.078 Uani 1 1 d . . . H163 H 0.8148 1.0639 0.2550 0.093 Uiso 1 1 calc R . . C164 C 0.5641(6) 1.0677(7) 0.3465(7) 0.095 Uani 1 1 d . . . H164 H 0.5483 1.0540 0.3848 0.114 Uiso 1 1 calc R . . C165 C 0.5449(7) 1.1186(8) 0.3094(7) 0.107 Uani 1 1 d . . . H165 H 0.5117 1.1452 0.3167 0.128 Uiso 1 1 calc R . . C166 C 0.5836(7) 1.1244(7) 0.2579(7) 0.093 Uani 1 1 d . . . H166 H 0.5813 1.1563 0.2258 0.111 Uiso 1 1 calc R . . C167 C 0.6405(6) 0.8890(7) 0.3026(5) 0.086 Uani 1 1 d . . . H167 H 0.6317 0.8633 0.3383 0.103 Uiso 1 1 calc R . . C168 C 0.6455(6) 0.8741(7) 0.2511(6) 0.091 Uani 1 1 d . . . H168 H 0.6420 0.8359 0.2436 0.109 Uiso 1 1 calc R . . C169 C 0.6569(5) 0.9255(6) 0.2103(5) 0.074 Uani 1 1 d . . . H169 H 0.6614 0.9280 0.1700 0.088 Uiso 1 1 calc R . . C170 C 0.7224(7) 1.1789(7) 0.2080(7) 0.092 Uani 1 1 d . . . C171 C 0.7438(8) 1.2215(7) 0.1642(7) 0.118 Uani 1 1 d . . . H171 H 0.7531 1.2592 0.1685 0.141 Uiso 1 1 calc R . . C172 C 0.7497(6) 1.2029(7) 0.1155(7) 0.088 Uani 1 1 d . . . C173 C 0.7119(8) 1.1772(8) 0.2728(7) 0.120 Uani 1 1 d . . . H17A H 0.6784 1.1545 0.2889 0.180 Uiso 1 1 calc R . . H17B H 0.7037 1.2178 0.2795 0.180 Uiso 1 1 calc R . . H17C H 0.7469 1.1582 0.2914 0.180 Uiso 1 1 calc R . . C174 C 0.7713(8) 1.2352(7) 0.0527(6) 0.110 Uani 1 1 d . . . H17D H 0.7383 1.2436 0.0289 0.165 Uiso 1 1 calc R . . H17E H 0.8023 1.2096 0.0362 0.165 Uiso 1 1 calc R . . H17F H 0.7865 1.2726 0.0543 0.165 Uiso 1 1 calc R . . C175 C 0.5828(6) 1.0634(7) 0.1360(5) 0.084 Uani 1 1 d . . . C176 C 0.5741(6) 1.0871(8) 0.0789(6) 0.097 Uani 1 1 d . . . H176 H 0.5387 1.0880 0.0617 0.117 Uiso 1 1 calc R . . C177 C 0.6232(7) 1.1082(7) 0.0522(6) 0.094 Uani 1 1 d . . . C178 C 0.5383(6) 1.0336(8) 0.1810(5) 0.105 Uani 1 1 d . . . H17G H 0.5567 1.0175 0.2166 0.158 Uiso 1 1 calc R . . H17H H 0.5239 1.0012 0.1674 0.158 Uiso 1 1 calc R . . H17I H 0.5054 1.0627 0.1881 0.158 Uiso 1 1 calc R . . C179 C 0.6393(7) 1.1397(7) -0.0104(5) 0.108 Uani 1 1 d . . . H17J H 0.6490 1.1800 -0.0110 0.162 Uiso 1 1 calc R . . H17K H 0.6059 1.1418 -0.0329 0.162 Uiso 1 1 calc R . . H17L H 0.6731 1.1174 -0.0270 0.162 Uiso 1 1 calc R . . C180 C 0.7892(6) 0.9745(6) 0.1607(5) 0.071 Uani 1 1 d . . . C181 C 0.8203(5) 0.9765(6) 0.1059(6) 0.069 Uani 1 1 d . . . H181 H 0.8493 0.9472 0.0954 0.083 Uiso 1 1 calc R . . C182 C 0.8017(6) 1.0261(6) 0.0721(6) 0.078 Uani 1 1 d . . . C183 C 0.7985(7) 0.9250(6) 0.2132(6) 0.091 Uani 1 1 d . . . H18A H 0.7803 0.9384 0.2478 0.136 Uiso 0.50 1 d PR . . H18B H 0.8406 0.9148 0.2164 0.136 Uiso 0.50 1 d PR . . H18C H 0.7805 0.8899 0.2091 0.136 Uiso 0.50 1 d PR . . H18D H 0.8206 0.8904 0.2011 0.136 Uiso 0.50 1 d PR . . H18E H 0.7604 0.9140 0.2325 0.136 Uiso 0.50 1 d PR . . H18F H 0.8204 0.9389 0.2398 0.136 Uiso 0.50 1 d PR . . C184 C 0.8176(8) 1.0505(7) 0.0090(6) 0.116 Uani 1 1 d . . . H18G H 0.8209 1.0933 0.0031 0.174 Uiso 1 1 calc R . . H18H H 0.7870 1.0436 -0.0135 0.174 Uiso 1 1 calc R . . H18I H 0.8551 1.0305 -0.0035 0.174 Uiso 1 1 calc R . . C185 C 0.7224(6) 1.1085(6) 0.0894(6) 0.076 Uani 1 1 d . . . H185 H 0.7348 1.1283 0.0493 0.091 Uiso 1 1 calc R . . C186 C 0.5778(6) 0.7769(8) 0.4222(6) 0.118 Uani 1 1 d . . . H18J H 0.6078 0.8043 0.4197 0.177 Uiso 1 1 calc R . . H18K H 0.5824 0.7600 0.3875 0.177 Uiso 1 1 calc R . . H18L H 0.5822 0.7448 0.4558 0.177 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 B1D 0.074 0.290 0.005 0.002 0.002 0.005 F1D 0.168 0.174 0.162 0.020 0.076 -0.048 F2D 0.179 0.167 0.116 -0.035 0.050 -0.047 F3D 0.149 0.206 0.151 0.058 -0.007 -0.067 F4D 0.215 0.186 0.124 -0.013 -0.056 0.020 B1B 0.024 0.033 0.034 -0.004 -0.003 -0.009 F1B 0.062 0.089 0.069 0.009 0.005 0.026 F2B 0.068 0.085 0.049 0.023 -0.006 -0.031 F3B 0.060 0.075 0.082 0.007 -0.002 -0.009 F4B 0.078 0.143 0.029 0.026 -0.017 0.011 B1E 0.041 0.132 0.092 -0.014 0.005 0.012 F1E 0.121 0.228 0.053 -0.017 -0.009 0.028 F2E 0.108 0.168 0.075 0.046 -0.009 0.007 F3E 0.231 0.171 0.130 0.021 -0.094 -0.052 F4E 0.163 0.284 0.092 -0.071 -0.043 0.072 B1F 0.059 0.094 0.036 -0.006 0.000 -0.003 F1F 0.098 0.110 0.083 0.012 0.000 -0.028 F2F 0.115 0.095 0.063 0.003 0.027 0.028 F3F 0.082 0.125 0.092 0.038 0.025 -0.015 F4F 0.085 0.133 0.059 0.014 0.002 0.034 B1G 0.082 0.240 0.267 -0.195 0.109 -0.095 F1G 0.122 0.331 0.101 -0.032 0.009 -0.100 F2G 0.226 0.277 0.200 -0.071 0.067 0.009 F3G 0.158 0.192 0.072 -0.018 0.021 -0.078 F4G 0.183 0.150 0.133 0.057 0.001 -0.065 B1H 0.043 0.155 0.050 0.024 -0.022 0.002 F1H 0.113 0.290 0.054 0.007 0.004 -0.103 F2H 0.065 0.180 0.045 -0.006 -0.007 -0.017 F3H 0.081 0.100 0.039 0.005 0.004 -0.008 F4H 0.132 0.159 0.105 -0.058 -0.048 0.052 B1I 0.188 0.174 0.097 -0.059 -0.040 -0.043 F1I 0.113 0.124 0.099 -0.008 -0.023 -0.015 F2I 0.145 0.267 0.089 -0.031 -0.050 0.027 F3I 0.187 0.284 0.124 -0.060 0.000 -0.064 F4I 0.298 0.184 0.224 -0.111 -0.113 0.024 Fe1 0.044 0.090 0.032 0.011 0.005 -0.016 Fe2 0.053 0.089 0.030 0.011 0.001 -0.024 Fe3 0.076 0.131 0.032 0.005 0.001 -0.036 Fe4 0.057 0.064 0.036 0.009 0.001 -0.013 Fe5 0.046 0.061 0.045 0.011 -0.004 -0.014 Fe6 0.069 0.081 0.066 0.010 -0.009 -0.022 O1 0.040 0.125 0.029 0.027 0.001 -0.003 O2 0.064 0.093 0.024 0.015 -0.022 -0.028 O3 0.088 0.073 0.030 0.009 0.009 -0.005 O4 0.108 0.068 0.030 0.013 0.000 -0.012 O5 0.050 0.087 0.037 0.014 0.004 -0.005 O6 0.062 0.108 0.056 0.003 0.002 -0.029 N1 0.035 0.122 0.033 0.004 -0.001 -0.035 N2 0.049 0.133 0.011 0.023 -0.021 -0.031 N3 0.047 0.118 0.024 0.024 0.001 0.001 N4 0.031 0.103 0.040 0.000 0.009 -0.013 N5 0.042 0.080 0.032 0.012 0.002 -0.013 N6 0.043 0.084 0.039 0.003 -0.001 -0.024 N7 0.071 0.108 0.022 0.024 -0.006 -0.014 N8 0.050 0.089 0.048 0.016 0.010 -0.019 N9 0.038 0.096 0.028 0.007 -0.018 -0.020 N10 0.045 0.088 0.042 -0.008 -0.002 -0.009 N11 0.044 0.099 0.042 -0.001 0.001 -0.015 N12 0.059 0.102 0.020 0.021 -0.005 -0.026 N13 0.080 0.119 0.024 0.022 -0.011 -0.057 N14 0.082 0.147 0.018 -0.011 0.002 -0.042 N15 0.052 0.101 0.026 0.015 -0.006 -0.019 N16 0.059 0.103 0.034 0.027 -0.013 -0.050 N17 0.053 0.081 0.029 0.018 0.001 -0.014 N18 0.039 0.101 0.030 0.017 -0.003 -0.019 N19 0.047 0.114 0.026 0.019 -0.003 -0.021 N20 0.042 0.116 0.035 0.007 -0.011 -0.033 N21 0.049 0.081 0.015 0.016 -0.019 -0.005 N22 0.076 0.092 0.018 0.014 0.003 -0.015 N23 0.070 0.114 0.036 0.023 0.004 -0.053 N24 0.068 0.121 0.051 0.012 0.001 -0.024 N25 0.083 0.108 0.039 -0.011 0.007 -0.039 N26 0.084 0.119 0.038 -0.015 0.015 -0.046 N27 0.095 0.116 0.031 0.013 0.000 -0.034 N28 0.076 0.157 0.035 0.009 0.003 -0.039 N29 0.096 0.069 0.021 0.015 -0.008 -0.027 N30 0.065 0.097 0.041 -0.001 -0.003 -0.037 N31 0.084 0.169 0.061 -0.022 0.037 -0.049 N32 0.111 0.302 0.035 -0.044 0.015 -0.122 N33 0.061 0.181 0.018 0.023 -0.001 -0.047 N34 0.062 0.167 0.032 0.008 -0.004 -0.038 N35 0.075 0.150 0.036 0.000 0.008 -0.063 N36 0.060 0.159 0.042 0.000 0.009 -0.052 N37 0.079 0.063 0.051 0.012 -0.005 -0.022 N38 0.057 0.078 0.033 0.003 0.005 -0.010 N39 0.075 0.070 0.043 0.009 -0.005 -0.013 N40 0.085 0.072 0.012 0.001 -0.015 -0.015 N41 0.072 0.077 0.042 0.014 -0.007 -0.014 N42 0.114 0.058 0.025 0.011 -0.001 -0.019 N43 0.052 0.056 0.043 0.001 -0.004 -0.016 N44 0.034 0.064 0.054 0.005 0.002 -0.013 N45 0.043 0.063 0.037 0.013 -0.001 -0.009 N46 0.049 0.067 0.040 -0.008 0.008 -0.009 N47 0.058 0.053 0.037 0.009 -0.009 -0.020 N48 0.045 0.058 0.041 0.000 -0.004 -0.019 N49 0.071 0.068 0.051 0.000 0.018 -0.023 N50 0.053 0.085 0.053 -0.002 0.010 -0.018 N51 0.036 0.067 0.050 -0.003 -0.003 -0.026 N52 0.045 0.072 0.036 0.022 -0.009 -0.031 N53 0.052 0.076 0.032 -0.003 0.005 -0.027 N54 0.051 0.075 0.039 0.012 -0.003 -0.033 N55 0.060 0.063 0.046 0.008 -0.007 -0.006 N56 0.067 0.040 0.046 0.011 -0.010 -0.015 N57 0.067 0.095 0.029 0.011 -0.015 -0.055 N58 0.055 0.077 0.043 -0.001 -0.011 -0.032 N59 0.054 0.063 0.033 0.015 -0.009 -0.020 N60 0.052 0.047 0.042 0.014 -0.002 -0.011 N61 0.067 0.085 0.081 -0.011 -0.025 -0.038 N62 0.071 0.105 0.069 0.020 -0.024 -0.039 N63 0.065 0.077 0.078 0.003 -0.012 -0.008 N64 0.087 0.062 0.075 0.001 -0.006 -0.005 N65 0.056 0.095 0.047 0.005 -0.008 -0.021 N66 0.067 0.087 0.057 -0.004 -0.016 -0.029 N67 0.092 0.085 0.064 0.016 0.005 -0.017 N68 0.098 0.067 0.105 0.006 -0.002 -0.025 N69 0.072 0.076 0.049 0.020 0.000 -0.017 N70 0.068 0.087 0.063 0.014 0.003 -0.025 N71 0.053 0.046 0.065 0.001 0.003 -0.008 N72 0.062 0.087 0.064 -0.005 -0.008 -0.027 C1 0.043 0.129 0.024 0.023 0.007 -0.012 C2 0.058 0.065 0.026 0.005 0.008 0.028 C3 0.091 0.055 0.014 0.007 -0.006 0.004 C4 0.068 0.088 0.013 0.023 0.006 -0.016 C5 0.096 0.083 0.016 0.031 0.005 -0.002 C6 0.094 0.095 0.019 0.015 0.006 -0.017 C7 0.067 0.113 0.034 0.012 0.017 -0.027 C8 0.064 0.114 0.022 0.018 0.012 -0.009 C9 0.050 0.086 0.033 -0.005 0.011 0.008 C10 0.062 0.115 0.046 -0.007 0.016 -0.018 C11 0.066 0.148 0.034 0.007 0.001 -0.034 C12 0.048 0.126 0.046 0.001 0.003 -0.034 C13 0.074 0.111 0.041 0.016 0.000 0.026 C14 0.082 0.126 0.046 0.013 0.006 0.018 C15 0.069 0.086 0.050 0.005 0.008 0.006 C16 0.043 0.065 0.035 0.006 0.011 -0.008 C17 0.049 0.074 0.072 0.002 0.024 -0.004 C18 0.054 0.095 0.036 0.005 -0.005 -0.011 C19 0.053 0.121 0.034 0.009 -0.011 -0.031 C20 0.073 0.167 0.020 0.001 -0.005 -0.045 C21 0.078 0.124 0.023 0.014 0.006 -0.045 C22 0.044 0.187 0.045 0.039 -0.020 -0.028 C23 0.081 0.111 0.034 0.032 -0.010 -0.028 C24 0.061 0.089 0.073 0.010 0.011 -0.014 C25 0.049 0.138 0.069 -0.012 -0.002 -0.023 C26 0.071 0.125 0.048 0.007 0.006 -0.045 C27 0.061 0.088 0.090 -0.007 0.010 -0.041 C28 0.123 0.149 0.051 0.022 -0.039 -0.060 C29 0.060 0.066 0.046 -0.001 0.002 -0.018 C30 0.122 0.082 0.023 0.003 -0.006 -0.008 C31 0.080 0.087 0.044 0.032 -0.015 -0.015 C32 0.127 0.081 0.037 0.001 0.005 -0.034 C33 0.151 0.101 0.043 0.029 -0.014 -0.016 C34 0.082 0.079 0.025 -0.002 0.004 -0.026 C35 0.060 0.140 0.044 -0.005 0.011 0.004 C36 0.065 0.088 0.033 0.006 0.003 -0.032 C37 0.042 0.119 0.023 0.003 -0.012 -0.025 C38 0.041 0.090 0.027 -0.014 -0.005 -0.035 C39 0.089 0.128 0.031 0.002 -0.007 -0.060 C40 0.074 0.201 0.062 -0.044 0.005 -0.091 C41 0.039 0.152 0.041 -0.008 -0.007 -0.047 C42 0.046 0.092 0.045 0.019 -0.011 -0.003 C43 0.056 0.071 0.077 0.015 -0.025 0.005 C44 0.056 0.075 0.071 -0.024 -0.003 -0.001 C45 0.051 0.108 0.041 0.019 0.000 -0.011 C46 0.070 0.089 0.032 0.016 0.004 0.007 C47 0.064 0.084 0.058 0.012 0.008 -0.040 C48 0.031 0.115 0.060 0.004 0.005 -0.021 C49 0.092 0.182 0.044 0.008 0.012 -0.057 C50 0.072 0.109 0.029 0.021 -0.004 -0.020 C51 0.088 0.218 0.039 0.009 -0.014 -0.035 C52 0.079 0.187 0.043 0.014 0.018 -0.028 C53 0.053 0.097 0.033 0.013 0.003 -0.014 C54 0.093 0.099 0.031 0.007 0.004 -0.037 C55 0.066 0.077 0.030 0.003 -0.015 -0.011 C56 0.070 0.091 0.039 0.025 0.002 -0.042 C57 0.051 0.133 0.020 0.009 -0.021 -0.033 C58 0.083 0.059 0.072 -0.014 0.001 -0.031 C59 0.104 0.077 0.063 0.014 -0.012 -0.029 C60 0.122 0.092 0.063 0.007 -0.009 -0.017 C61 0.130 0.102 0.073 -0.030 0.033 -0.037 C62 0.193 0.173 0.062 0.055 -0.030 -0.030 C63 0.054 0.101 0.035 0.012 0.006 -0.040 C64 0.064 0.086 0.055 0.016 -0.004 -0.001 C65 0.135 0.111 0.034 -0.006 -0.011 0.032 C66 0.098 0.083 0.053 -0.008 0.027 -0.035 C67 0.054 0.084 0.046 -0.002 0.014 -0.009 C68 0.083 0.089 0.052 0.007 -0.001 -0.038 C69 0.061 0.087 0.080 -0.004 0.001 -0.034 C70 0.090 0.135 0.057 -0.039 -0.005 -0.055 C71 0.076 0.138 0.049 -0.015 0.021 -0.047 C72 0.087 0.118 0.050 0.019 0.000 -0.068 C73 0.077 0.219 0.036 -0.006 -0.008 -0.047 C74 0.114 0.096 0.024 0.019 -0.017 -0.035 C75 0.125 0.097 0.039 0.014 -0.028 -0.062 C76 0.091 0.080 0.057 0.020 -0.016 -0.025 C77 0.099 0.216 0.047 -0.004 -0.028 -0.081 C78 0.154 0.291 0.065 -0.065 -0.021 -0.105 C79 0.159 0.318 0.022 -0.030 0.000 -0.168 C80 0.137 0.194 0.077 -0.011 0.058 -0.075 C81 0.154 0.190 0.144 -0.035 -0.033 -0.051 C82 0.054 0.177 0.046 0.037 -0.010 -0.030 C83 0.088 0.175 0.043 0.040 0.008 -0.019 C84 0.052 0.189 0.083 0.082 -0.011 -0.030 C85 0.074 0.219 0.048 0.005 -0.003 -0.020 C86 0.117 0.217 0.024 0.044 -0.013 -0.070 C87 0.085 0.091 0.051 0.006 0.003 -0.030 C88 0.071 0.209 0.093 -0.057 0.008 -0.043 C89 0.105 0.195 0.068 -0.020 0.025 -0.068 C90 0.085 0.081 0.069 0.027 -0.009 -0.017 C91 0.123 0.235 0.039 -0.013 0.018 -0.050 C92 0.081 0.169 0.049 -0.014 0.015 -0.055 C93 0.121 0.178 0.062 0.039 -0.013 -0.123 C94 0.133 0.090 0.028 0.011 0.017 -0.034 C95 0.088 0.068 0.029 0.019 0.010 -0.022 C96 0.072 0.077 0.044 0.012 0.009 -0.023 C97 0.064 0.058 0.039 -0.001 -0.011 0.001 C98 0.078 0.097 0.029 0.013 0.004 -0.007 C99 0.111 0.079 0.042 0.036 0.016 0.016 C100 0.139 0.134 0.023 -0.002 0.002 -0.033 C101 0.133 0.077 0.027 0.022 -0.004 -0.003 C102 0.103 0.083 0.028 0.001 0.003 -0.008 C103 0.077 0.064 0.065 0.012 -0.001 -0.003 C104 0.051 0.071 0.102 0.028 0.007 -0.022 C105 0.043 0.046 0.071 0.010 -0.005 -0.008 C106 0.082 0.063 0.062 0.010 -0.016 -0.002 C107 0.079 0.107 0.037 0.012 -0.012 -0.014 C108 0.061 0.042 0.064 0.020 -0.009 0.004 C109 0.102 0.086 0.042 -0.007 0.022 -0.014 C110 0.087 0.075 0.047 -0.014 -0.004 0.007 C111 0.093 0.048 0.060 -0.006 -0.008 -0.002 C112 0.060 0.072 0.045 -0.005 -0.011 -0.001 C113 0.065 0.070 0.072 -0.015 0.000 -0.018 C114 0.038 0.084 0.070 -0.008 -0.007 -0.009 C115 0.062 0.061 0.077 0.021 0.005 0.003 C116 0.076 0.175 0.040 0.013 -0.011 -0.060 C117 0.037 0.071 0.040 0.002 0.007 0.000 C118 0.053 0.055 0.063 0.004 0.004 -0.005 C119 0.044 0.064 0.070 -0.017 -0.003 -0.019 C120 0.064 0.082 0.060 0.032 -0.018 -0.002 C121 0.072 0.086 0.040 -0.008 0.000 -0.003 C122 0.053 0.092 0.033 0.007 -0.001 -0.023 C123 0.080 0.050 0.041 0.003 -0.016 -0.013 C124 0.058 0.066 0.048 0.020 0.005 -0.018 C125 0.094 0.090 0.039 0.013 -0.011 -0.030 C126 0.053 0.092 0.050 0.005 0.003 -0.017 C127 0.042 0.067 0.054 -0.014 -0.002 -0.011 C128 0.115 0.117 0.044 0.037 -0.004 -0.052 C129 0.056 0.106 0.027 0.018 0.000 -0.010 C130 0.061 0.085 0.026 0.009 0.006 -0.015 C131 0.035 0.059 0.059 0.016 -0.005 -0.016 C132 0.077 0.091 0.052 -0.004 0.017 -0.028 C133 0.056 0.070 0.115 -0.030 0.004 0.001 C134 0.069 0.091 0.039 -0.002 0.007 0.000 C135 0.040 0.067 0.053 0.006 0.004 -0.026 C136 0.052 0.053 0.084 0.014 -0.017 -0.008 C137 0.056 0.069 0.054 0.015 -0.010 -0.023 C138 0.061 0.093 0.037 0.012 -0.008 -0.037 C139 0.079 0.081 0.043 0.035 -0.008 -0.042 C140 0.062 0.088 0.047 0.035 -0.008 -0.026 C141 0.064 0.066 0.064 0.018 -0.010 -0.009 C142 0.071 0.108 0.079 -0.008 -0.036 -0.010 C143 0.075 0.069 0.057 -0.013 -0.016 -0.026 C144 0.128 0.096 0.052 0.016 -0.005 -0.013 C145 0.095 0.052 0.084 0.028 -0.037 -0.025 C146 0.046 0.110 0.066 0.003 0.007 -0.040 C147 0.082 0.126 0.070 0.014 -0.019 -0.030 C148 0.054 0.064 0.074 0.014 0.000 -0.023 C149 0.050 0.133 0.074 0.037 0.000 -0.045 C150 0.064 0.092 0.072 0.023 -0.024 -0.032 C151 0.045 0.057 0.050 0.025 -0.016 -0.018 C152 0.052 0.046 0.063 0.018 -0.001 -0.013 C153 0.046 0.029 0.070 0.013 0.009 -0.010 C154 0.065 0.061 0.058 0.032 0.009 0.004 C155 0.061 0.060 0.047 0.020 -0.009 0.008 C156 0.046 0.053 0.048 0.013 -0.002 -0.009 C157 0.056 0.097 0.080 -0.014 -0.003 -0.025 C158 0.065 0.232 0.048 -0.006 -0.005 -0.054 C159 0.076 0.115 0.053 0.010 -0.012 -0.028 C160 0.068 0.092 0.066 -0.020 -0.011 -0.044 C161 0.064 0.116 0.069 -0.030 -0.023 -0.025 C162 0.065 0.171 0.106 -0.052 0.012 -0.058 C163 0.074 0.097 0.069 -0.016 0.000 -0.045 C164 0.060 0.098 0.105 0.034 -0.031 0.002 C165 0.070 0.154 0.098 -0.018 -0.019 -0.022 C166 0.086 0.076 0.118 -0.025 -0.016 0.003 C167 0.111 0.098 0.042 0.016 -0.002 -0.041 C168 0.094 0.094 0.087 0.002 -0.010 -0.054 C169 0.066 0.100 0.060 0.004 -0.034 -0.041 C170 0.104 0.057 0.119 -0.036 0.028 -0.026 C171 0.161 0.057 0.118 -0.019 0.054 0.002 C172 0.082 0.065 0.112 -0.013 0.011 -0.011 C173 0.141 0.113 0.112 -0.040 0.013 -0.035 C174 0.144 0.067 0.103 0.004 0.004 0.001 C175 0.058 0.097 0.071 0.022 0.023 0.003 C176 0.049 0.147 0.075 0.010 0.009 0.009 C177 0.102 0.087 0.077 0.015 -0.019 0.003 C178 0.071 0.150 0.062 0.035 0.024 -0.004 C179 0.105 0.119 0.062 0.044 -0.002 0.029 C180 0.062 0.077 0.073 0.002 -0.014 -0.034 C181 0.044 0.070 0.096 -0.025 0.004 -0.006 C182 0.094 0.055 0.075 0.013 -0.021 -0.007 C183 0.100 0.086 0.086 -0.006 -0.015 -0.030 C184 0.141 0.100 0.092 0.001 0.040 -0.036 C185 0.085 0.063 0.075 0.004 -0.013 -0.017 C186 0.070 0.178 0.073 0.012 -0.014 0.062 _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 B1D F1D 1.317(8) . ? B1D F4D 1.338(8) . ? B1D F2D 1.380(9) . ? B1D F3D 1.380(8) . ? B1A F1A 1.33(3) . ? B1A F4A 1.35(2) . ? B1A F2A 1.52(3) . ? B1A F3A 1.61(3) . ? B1B F3B 1.36(2) . ? B1B F4B 1.37(2) . ? B1B F2B 1.40(2) . ? B1B F1B 1.41(2) . ? B1C F1C 1.317(8) . ? B1C F4C 1.338(8) . ? B1C F2C 1.380(9) . ? B1C F3C 1.380(8) . ? B1E F1E 1.317(8) . ? B1E F4E 1.338(8) . ? B1E F2E 1.380(9) . ? B1E F3E 1.380(8) . ? B1F F2F 1.298(16) . ? B1F F3F 1.324(17) . ? B1F F4F 1.402(14) . ? B1F F1F 1.460(16) . ? B1G F1G 1.317(8) . ? B1G F4G 1.338(8) . ? B1G F2G 1.380(9) . ? B1G F3G 1.380(8) . ? B1H F4H 1.33(2) . ? B1H F3H 1.356(18) . ? B1H F2H 1.382(15) . ? B1H F1H 1.385(18) . ? B1I F1I 1.317(8) . ? B1I F4I 1.338(8) . ? B1I F2I 1.380(9) . ? B1I F3I 1.380(8) . ? B1J F1J 1.317(8) . ? B1J F4J 1.338(8) . ? B1J F2J 1.380(9) . ? B1J F3J 1.380(8) . ? B1K F1K 1.21(2) . ? B1K F3K 1.33(2) . ? B1K F2K 1.39(2) . ? B1K F4K 1.43(3) . ? B1K F5K 1.52(3) . ? Fe1 N4 1.921(11) . ? Fe1 N2 1.957(9) . ? Fe1 N6 1.967(8) . ? Fe1 N9 1.976(8) . ? Fe1 N7 2.001(9) . ? Fe1 N11 2.010(11) . ? Fe2 N18 1.942(9) . ? Fe2 N16 1.947(11) . ? Fe2 N14 1.959(9) . ? Fe2 N19 1.972(9) . ? Fe2 N21 1.985(8) . ? Fe2 N23 2.008(12) . ? Fe3 N28 1.961(11) . ? Fe3 N26 1.971(12) . ? Fe3 N35 1.972(10) . ? Fe3 N31 1.974(13) . ? Fe3 N30 1.975(10) . ? Fe3 N33 1.985(13) . ? Fe4 N42 1.905(11) . ? Fe4 N40 1.948(8) . ? Fe4 N38 1.972(9) . ? Fe4 N43 1.984(8) . ? Fe4 N47 1.996(8) . ? Fe4 N45 2.023(9) . ? Fe5 N54 1.937(8) . ? Fe5 N50 1.946(9) . ? Fe5 N52 1.955(9) . ? Fe5 N57 1.974(8) . ? Fe5 N59 1.994(9) . ? Fe5 N55 1.996(10) . ? Fe6 N66 1.939(11) . ? Fe6 N62 1.952(10) . ? Fe6 N69 1.967(10) . ? Fe6 N64 1.973(12) . ? Fe6 N71 1.974(10) . ? Fe6 N67 2.033(12) . ? O1 C7 1.420(12) . ? O1 C8 1.456(13) . ? O2 C36 1.444(11) . ? O2 C37 1.448(13) . ? O3 C66 1.437(14) . ? O3 C65 1.474(12) . ? O4 C101 1.414(14) . ? O4 C100 1.519(12) . ? O5 C130 1.407(13) . ? O5 C129 1.422(11) . ? O6 C158 1.421(15) . ? O6 C159 1.480(14) . ? N1 C10 1.345(14) . ? N1 N2 1.382(11) . ? N1 C9 1.439(15) . ? N2 C12 1.294(15) . ? N3 C13 1.372(16) . ? N3 N4 1.403(11) . ? N3 C9 1.436(15) . ? N4 C15 1.342(15) . ? N5 N6 1.359(11) . ? N5 C16 1.369(12) . ? N5 C9 1.429(13) . ? N6 C18 1.344(13) . ? N7 N8 1.349(11) . ? N7 C19 1.354(14) . ? N8 C21 1.346(13) . ? N8 C34 1.424(14) . ? N9 C24 1.327(15) . ? N9 N10 1.394(11) . ? N10 C26 1.326(14) . ? N10 C34 1.439(14) . ? N11 C29 1.306(14) . ? N11 N12 1.408(11) . ? N12 C31 1.362(16) . ? N12 C34 1.448(15) . ? N13 C39 1.269(13) . ? N13 N14 1.356(11) . ? N13 C38 1.517(13) . ? N14 C41 1.355(14) . ? N15 C42 1.352(15) . ? N15 C38 1.424(14) . ? N15 N16 1.436(11) . ? N16 C44 1.341(15) . ? N17 C45 1.357(13) . ? N17 N18 1.368(10) . ? N17 C38 1.443(13) . ? N18 C47 1.286(14) . ? N19 C48 1.329(13) . ? N19 N20 1.421(11) . ? N20 C50 1.419(14) . ? N20 C63 1.438(14) . ? N21 C53 1.325(14) . ? N21 N22 1.378(10) . ? N22 C55 1.358(13) . ? N22 C63 1.428(14) . ? N23 C58 1.348(15) . ? N23 N24 1.404(12) . ? N24 C60 1.375(18) . ? N24 C63 1.465(16) . ? N25 N26 1.343(12) . ? N25 C68 1.378(16) . ? N25 C67 1.446(15) . ? N26 C70 1.361(17) . ? N27 C71 1.337(15) . ? N27 N28 1.391(12) . ? N27 C67 1.508(15) . ? N28 C73 1.319(16) . ? N29 C74 1.319(14) . ? N29 N30 1.370(11) . ? N29 C67 1.497(14) . ? N30 C76 1.260(14) . ? N31 C77 1.331(18) . ? N31 N32 1.421(14) . ? N32 C79 1.323(18) . ? N32 C92 1.426(18) . ? N33 N34 1.380(13) . ? N33 C82 1.38(2) . ? N34 C84 1.414(19) . ? N34 C92 1.522(19) . ? N35 N36 1.352(12) . ? N35 C87 1.364(16) . ? N36 C89 1.342(17) . ? N36 C92 1.429(16) . ? N37 N38 1.344(11) . ? N37 C103 1.379(15) . ? N37 C102 1.485(16) . ? N38 C105 1.306(14) . ? N39 N40 1.390(11) . ? N39 C106 1.406(14) . ? N39 C102 1.416(15) . ? N40 C108 1.334(14) . ? N41 C109 1.379(15) . ? N41 N42 1.400(11) . ? N41 C102 1.499(16) . ? N42 C111 1.289(14) . ? N43 C112 1.338(13) . ? N43 N44 1.389(11) . ? N44 C114 1.297(13) . ? N44 C127 1.448(13) . ? N45 C117 1.311(13) . ? N45 N46 1.409(11) . ? N46 C119 1.330(14) . ? N46 C127 1.470(14) . ? N47 C122 1.298(14) . ? N47 N48 1.373(11) . ? N48 C124 1.402(13) . ? N48 C127 1.422(13) . ? N49 C132 1.340(14) . ? N49 N50 1.377(12) . ? N49 C131 1.467(14) . ? N50 C134 1.304(14) . ? N51 C135 1.338(13) . ? N51 N52 1.351(11) . ? N51 C131 1.491(14) . ? N52 C137 1.320(14) . ? N53 C138 1.368(13) . ? N53 N54 1.374(11) . ? N53 C131 1.464(12) . ? N54 C140 1.333(13) . ? N55 C141 1.331(15) . ? N55 N56 1.356(11) . ? N56 C143 1.352(14) . ? N56 C156 1.420(13) . ? N57 C146 1.376(13) . ? N57 N58 1.441(11) . ? N58 C148 1.365(13) . ? N58 C156 1.458(13) . ? N59 C151 1.335(14) . ? N59 N60 1.366(11) . ? N60 C153 1.348(13) . ? N60 C156 1.420(13) . ? N61 C161 1.358(14) . ? N61 N62 1.401(13) . ? N61 C160 1.515(14) . ? N62 C163 1.343(14) . ? N63 C164 1.345(17) . ? N63 C160 1.443(16) . ? N63 N64 1.447(14) . ? N64 C166 1.293(16) . ? N65 C167 1.359(16) . ? N65 N66 1.405(12) . ? N65 C160 1.448(15) . ? N66 C169 1.354(15) . ? N67 C170 1.330(16) . ? N67 N68 1.370(14) . ? N68 C172 1.355(17) . ? N68 C185 1.477(16) . ? N69 C175 1.354(15) . ? N69 N70 1.400(12) . ? N70 C177 1.348(16) . ? N70 C185 1.439(15) . ? N71 C180 1.315(15) . ? N71 N72 1.401(12) . ? N72 C182 1.362(16) . ? N72 C185 1.429(16) . ? C1 C6 1.427(18) . ? C1 C2 1.436(17) . ? C1 C7 1.585(17) . ? C2 C3 1.392(15) . ? C2 C35 1.452(17) . ? C3 C4 1.382(16) . ? C3 C36 1.524(16) . ? C4 C5 1.388(17) . ? C4 C64 1.504(16) . ? C5 C6 1.428(17) . ? C5 C65 1.547(19) . ? C6 C93 1.461(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.554(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.365(18) . ? C10 H10 0.9500 . ? C11 C12 1.461(16) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.369(17) . ? C13 H13 0.9500 . ? C14 C15 1.381(17) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.365(15) . ? C16 H16 0.9500 . ? C17 C18 1.406(15) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.412(14) . ? C19 C22 1.539(15) . ? C20 C21 1.334(17) . ? C20 H20 0.9500 . ? C21 C23 1.538(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.416(17) . ? C24 C27 1.499(17) . ? C25 C26 1.364(18) . ? C25 H25 0.9500 . ? C26 C28 1.524(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.403(16) . ? C29 C32 1.520(14) . ? C30 C31 1.299(16) . ? C30 H30 0.9500 . ? C31 C33 1.546(15) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.533(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 C40 1.386(16) . ? C39 H39 0.9500 . ? C40 C41 1.350(15) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.381(16) . ? C42 H42 0.9500 . ? C43 C44 1.370(16) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.337(15) . ? C45 H45 0.9500 . ? C46 C47 1.410(15) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.419(15) . ? C48 C51 1.471(17) . ? C49 C50 1.346(18) . ? C49 H49 0.9500 . ? C50 C52 1.513(15) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.395(15) . ? C53 C56 1.559(14) . ? C54 C55 1.365(16) . ? C54 H54 0.9500 . ? C55 C57 1.516(13) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.350(16) . ? C58 C61 1.498(17) . ? C59 C60 1.357(18) . ? C59 H59 0.9500 . ? C60 C62 1.466(18) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.551(15) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 C69 1.374(17) . ? C68 H68 0.9500 . ? C69 C70 1.453(18) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.388(17) . ? C71 H71 0.9500 . ? C72 C73 1.446(17) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C74 C75 1.415(16) . ? C74 H74 0.9500 . ? C75 C76 1.406(16) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.377(19) . ? C77 C80 1.509(18) . ? C78 C79 1.43(2) . ? C78 H78 0.9500 . ? C79 C81 1.55(2) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.381(17) . ? C82 C85 1.51(2) . ? C83 C84 1.33(2) . ? C83 H83 0.9500 . ? C84 C86 1.504(18) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.409(18) . ? C87 C90 1.511(16) . ? C88 C89 1.39(2) . ? C88 H88 0.9500 . ? C89 C91 1.544(18) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92 1.0000 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C99 1.42(2) . ? C94 C95 1.472(19) . ? C94 C100 1.544(19) . ? C95 C96 1.375(17) . ? C95 C128 1.489(17) . ? C96 C97 1.406(16) . ? C96 C129 1.536(17) . ? C97 C98 1.427(16) . ? C97 C157 1.487(16) . ? C98 C99 1.380(18) . ? C98 C158 1.533(18) . ? C99 C186 1.523(18) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.515(14) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C103 C104 1.353(17) . ? C103 H103 0.9500 . ? C104 C105 1.439(16) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.373(16) . ? C106 H106 0.9500 . ? C107 C108 1.456(16) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.341(16) . ? C109 H109 0.9500 . ? C110 C111 1.409(16) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 C113 1.361(15) . ? C112 C115 1.500(15) . ? C113 C114 1.420(16) . ? C113 H113 0.9500 . ? C114 C116 1.520(15) . ? C115 H11A 0.9800 . ? C115 H11B 0.9800 . ? C115 H11C 0.9800 . ? C116 H11D 0.9800 . ? C116 H11E 0.9800 . ? C116 H11F 0.9800 . ? C117 C118 1.391(15) . ? C117 C120 1.528(14) . ? C118 C119 1.394(15) . ? C118 H118 0.9500 . ? C119 C121 1.508(15) . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C122 C123 1.440(14) . ? C122 C125 1.531(16) . ? C123 C124 1.314(15) . ? C123 H123 0.9500 . ? C124 C126 1.518(14) . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C126 H12L 0.9800 . ? C127 H127 1.0000 . ? C128 H12M 0.9800 . ? C128 H12N 0.9800 . ? C128 H12O 0.9800 . ? C129 H12P 0.9900 . ? C129 H12Q 0.9900 . ? C130 C131 1.554(14) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C132 C133 1.409(18) . ? C132 H132 0.9500 . ? C133 C134 1.392(16) . ? C133 H133 0.9500 . ? C134 H134 0.9500 . ? C135 C136 1.351(15) . ? C135 H135 0.9500 . ? C136 C137 1.460(15) . ? C136 H136 0.9500 . ? C137 H137 0.9500 . ? C138 C139 1.418(14) . ? C138 H138 0.9500 . ? C139 C140 1.403(15) . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C141 C142 1.411(17) . ? C141 C144 1.506(16) . ? C142 C143 1.383(16) . ? C142 H142 0.9500 . ? C143 C145 1.481(15) . ? C144 H14A 0.9800 . ? C144 H14B 0.9800 . ? C144 H14C 0.9800 . ? C145 H14D 0.9800 . ? C145 H14E 0.9800 . ? C145 H14F 0.9800 . ? C146 C147 1.394(17) . ? C146 C149 1.533(15) . ? C147 C148 1.347(17) . ? C147 H147 0.9500 . ? C148 C150 1.499(15) . ? C149 H14G 0.9800 . ? C149 H14H 0.9800 . ? C149 H14I 0.9800 . ? C150 H15A 0.9800 . ? C150 H15B 0.9800 . ? C150 H15C 0.9800 . ? C151 C152 1.433(15) . ? C151 C154 1.501(14) . ? C152 C153 1.369(14) . ? C152 H152 0.9500 . ? C153 C155 1.485(14) . ? C154 H15D 0.9800 . ? C154 H15E 0.9800 . ? C154 H15F 0.9800 . ? C155 H15G 0.9800 . ? C155 H15H 0.9800 . ? C155 H15I 0.9800 . ? C156 H156 1.0000 . ? C157 H15J 0.9800 . ? C157 H15K 0.9800 . ? C157 H15L 0.9800 . ? C158 H15M 0.9900 . ? C158 H15N 0.9900 . ? C159 C160 1.527(16) . ? C159 H15O 0.9900 . ? C159 H15P 0.9900 . ? C161 C162 1.433(18) . ? C161 H161 0.9500 . ? C162 C163 1.375(18) . ? C162 H162 0.9500 . ? C163 H163 0.9500 . ? C164 C165 1.38(2) . ? C164 H164 0.9500 . ? C165 C166 1.43(2) . ? C165 H165 0.9500 . ? C166 H166 0.9500 . ? C167 C168 1.340(17) . ? C167 H167 0.9500 . ? C168 C169 1.401(17) . ? C168 H168 0.9500 . ? C169 H169 0.9500 . ? C170 C171 1.369(19) . ? C170 C173 1.539(19) . ? C171 C172 1.315(19) . ? C171 H171 0.9500 . ? C172 C174 1.585(19) . ? C173 H17A 0.9800 . ? C173 H17B 0.9800 . ? C173 H17C 0.9800 . ? C174 H17D 0.9800 . ? C174 H17E 0.9800 . ? C174 H17F 0.9800 . ? C175 C176 1.391(17) . ? C175 C178 1.514(16) . ? C176 C177 1.327(19) . ? C176 H176 0.9500 . ? C177 C179 1.548(18) . ? C178 H17G 0.9800 . ? C178 H17H 0.9800 . ? C178 H17I 0.9800 . ? C179 H17J 0.9800 . ? C179 H17K 0.9800 . ? C179 H17L 0.9800 . ? C180 C181 1.418(16) . ? C180 C183 1.530(17) . ? C181 C182 1.314(16) . ? C181 H181 0.9500 . ? C182 C184 1.519(18) . ? C183 H18A 0.9800 . ? C183 H18B 0.9800 . ? C183 H18C 0.9800 . ? C183 H18D 0.9800 . ? C183 H18E 0.9800 . ? C183 H18F 0.9800 . ? C184 H18G 0.9800 . ? C184 H18H 0.9800 . ? C184 H18I 0.9800 . ? C185 H185 1.0000 . ? C186 H18J 0.9800 . ? C186 H18K 0.9800 . ? C186 H18L 0.9800 . ? 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 F1D B1D F4D 113.3(7) . . ? F1D B1D F2D 111.4(7) . . ? F4D B1D F2D 106.2(6) . . ? F1D B1D F3D 108.6(6) . . ? F4D B1D F3D 109.6(7) . . ? F2D B1D F3D 107.6(6) . . ? F1A B1A F4A 118(2) . . ? F1A B1A F2A 110(2) . . ? F4A B1A F2A 109.7(19) . . ? F1A B1A F3A 106(2) . . ? F4A B1A F3A 116.5(19) . . ? F2A B1A F3A 95.0(18) . . ? F3B B1B F4B 109.8(18) . . ? F3B B1B F2B 108.3(17) . . ? F4B B1B F2B 107.7(16) . . ? F3B B1B F1B 115.3(19) . . ? F4B B1B F1B 110.2(14) . . ? F2B B1B F1B 105.2(16) . . ? F1C B1C F4C 113.4(7) . . ? F1C B1C F2C 111.4(7) . . ? F4C B1C F2C 106.2(6) . . ? F1C B1C F3C 108.5(6) . . ? F4C B1C F3C 109.6(7) . . ? F2C B1C F3C 107.6(6) . . ? F1E B1E F4E 113.2(7) . . ? F1E B1E F2E 111.5(7) . . ? F4E B1E F2E 106.3(6) . . ? F1E B1E F3E 108.5(6) . . ? F4E B1E F3E 109.6(7) . . ? F2E B1E F3E 107.5(6) . . ? F2F B1F F3F 114.4(11) . . ? F2F B1F F4F 112.0(11) . . ? F3F B1F F4F 111.8(13) . . ? F2F B1F F1F 113.4(13) . . ? F3F B1F F1F 105.4(11) . . ? F4F B1F F1F 98.6(10) . . ? F1G B1G F4G 113.2(7) . . ? F1G B1G F2G 111.5(7) . . ? F4G B1G F2G 106.2(7) . . ? F1G B1G F3G 108.6(6) . . ? F4G B1G F3G 109.7(7) . . ? F2G B1G F3G 107.5(6) . . ? F4H B1H F3H 109.5(11) . . ? F4H B1H F2H 110.8(16) . . ? F3H B1H F2H 112.1(12) . . ? F4H B1H F1H 106.8(13) . . ? F3H B1H F1H 110.1(16) . . ? F2H B1H F1H 107.4(11) . . ? F1I B1I F4I 113.3(7) . . ? F1I B1I F2I 111.4(7) . . ? F4I B1I F2I 106.3(7) . . ? F1I B1I F3I 108.6(6) . . ? F4I B1I F3I 109.6(7) . . ? F2I B1I F3I 107.6(6) . . ? F1J B1J F4J 113.3(7) . . ? F1J B1J F2J 111.4(7) . . ? F4J B1J F2J 106.3(7) . . ? F1J B1J F3J 108.6(6) . . ? F4J B1J F3J 109.6(7) . . ? F2J B1J F3J 107.5(6) . . ? F1K B1K F3K 124(2) . . ? F1K B1K F2K 122(2) . . ? F3K B1K F2K 114(2) . . ? F1K B1K F4K 91.8(19) . . ? F3K B1K F4K 88.7(18) . . ? F2K B1K F4K 89.0(16) . . ? F1K B1K F5K 105(2) . . ? F3K B1K F5K 77.6(17) . . ? F2K B1K F5K 86.3(17) . . ? F4K B1K F5K 162(2) . . ? N4 Fe1 N2 87.8(4) . . ? N4 Fe1 N6 87.8(4) . . ? N2 Fe1 N6 86.7(3) . . ? N4 Fe1 N9 91.8(4) . . ? N2 Fe1 N9 179.0(4) . . ? N6 Fe1 N9 94.3(4) . . ? N4 Fe1 N7 92.9(4) . . ? N2 Fe1 N7 90.8(4) . . ? N6 Fe1 N7 177.4(4) . . ? N9 Fe1 N7 88.3(4) . . ? N4 Fe1 N11 178.1(4) . . ? N2 Fe1 N11 91.6(4) . . ? N6 Fe1 N11 90.3(4) . . ? N9 Fe1 N11 88.8(4) . . ? N7 Fe1 N11 88.9(4) . . ? N18 Fe2 N16 87.7(4) . . ? N18 Fe2 N14 86.9(4) . . ? N16 Fe2 N14 88.1(4) . . ? N18 Fe2 N19 178.5(4) . . ? N16 Fe2 N19 92.2(4) . . ? N14 Fe2 N19 91.5(4) . . ? N18 Fe2 N21 92.8(4) . . ? N16 Fe2 N21 90.6(4) . . ? N14 Fe2 N21 178.7(4) . . ? N19 Fe2 N21 88.7(4) . . ? N18 Fe2 N23 91.2(4) . . ? N16 Fe2 N23 178.8(4) . . ? N14 Fe2 N23 92.4(5) . . ? N19 Fe2 N23 88.9(4) . . ? N21 Fe2 N23 88.9(4) . . ? N28 Fe3 N26 85.9(5) . . ? N28 Fe3 N35 178.3(5) . . ? N26 Fe3 N35 94.6(5) . . ? N28 Fe3 N31 93.4(5) . . ? N26 Fe3 N31 91.5(5) . . ? N35 Fe3 N31 88.2(4) . . ? N28 Fe3 N30 87.8(4) . . ? N26 Fe3 N30 87.5(4) . . ? N35 Fe3 N30 90.6(4) . . ? N31 Fe3 N30 178.4(5) . . ? N28 Fe3 N33 90.8(5) . . ? N26 Fe3 N33 176.7(5) . . ? N35 Fe3 N33 88.7(5) . . ? N31 Fe3 N33 88.9(5) . . ? N30 Fe3 N33 92.2(5) . . ? N42 Fe4 N40 89.1(4) . . ? N42 Fe4 N38 87.9(4) . . ? N40 Fe4 N38 87.0(4) . . ? N42 Fe4 N43 89.5(4) . . ? N40 Fe4 N43 178.4(4) . . ? N38 Fe4 N43 93.8(4) . . ? N42 Fe4 N47 91.5(4) . . ? N40 Fe4 N47 91.3(4) . . ? N38 Fe4 N47 178.2(4) . . ? N43 Fe4 N47 87.9(3) . . ? N42 Fe4 N45 177.8(4) . . ? N40 Fe4 N45 92.9(4) . . ? N38 Fe4 N45 91.5(4) . . ? N43 Fe4 N45 88.5(4) . . ? N47 Fe4 N45 89.2(4) . . ? N54 Fe5 N50 88.4(4) . . ? N54 Fe5 N52 87.4(4) . . ? N50 Fe5 N52 85.5(4) . . ? N54 Fe5 N57 178.4(3) . . ? N50 Fe5 N57 92.8(4) . . ? N52 Fe5 N57 93.7(4) . . ? N54 Fe5 N59 91.7(4) . . ? N50 Fe5 N59 176.9(4) . . ? N52 Fe5 N59 91.4(4) . . ? N57 Fe5 N59 87.1(4) . . ? N54 Fe5 N55 91.8(4) . . ? N50 Fe5 N55 94.4(4) . . ? N52 Fe5 N55 179.2(4) . . ? N57 Fe5 N55 87.1(4) . . ? N59 Fe5 N55 88.7(4) . . ? N66 Fe6 N62 87.8(4) . . ? N66 Fe6 N69 92.5(4) . . ? N62 Fe6 N69 179.8(5) . . ? N66 Fe6 N64 88.3(5) . . ? N62 Fe6 N64 87.8(5) . . ? N69 Fe6 N64 92.2(4) . . ? N66 Fe6 N71 92.7(4) . . ? N62 Fe6 N71 91.6(5) . . ? N69 Fe6 N71 88.4(4) . . ? N64 Fe6 N71 178.8(4) . . ? N66 Fe6 N67 178.8(4) . . ? N62 Fe6 N67 91.1(5) . . ? N69 Fe6 N67 88.7(4) . . ? N64 Fe6 N67 91.6(5) . . ? N71 Fe6 N67 87.3(4) . . ? C7 O1 C8 108.5(7) . . ? C36 O2 C37 110.5(7) . . ? C66 O3 C65 110.7(9) . . ? C101 O4 C100 109.0(9) . . ? C130 O5 C129 109.8(8) . . ? C158 O6 C159 110.6(9) . . ? C10 N1 N2 108.8(10) . . ? C10 N1 C9 132.7(9) . . ? N2 N1 C9 117.6(9) . . ? C12 N2 N1 106.6(9) . . ? C12 N2 Fe1 134.6(8) . . ? N1 N2 Fe1 118.8(8) . . ? C13 N3 N4 107.0(10) . . ? C13 N3 C9 133.5(9) . . ? N4 N3 C9 119.3(10) . . ? C15 N4 N3 104.8(10) . . ? C15 N4 Fe1 137.0(8) . . ? N3 N4 Fe1 117.3(8) . . ? N6 N5 C16 110.8(8) . . ? N6 N5 C9 118.1(8) . . ? C16 N5 C9 131.1(8) . . ? C18 N6 N5 104.9(8) . . ? C18 N6 Fe1 135.8(7) . . ? N5 N6 Fe1 119.2(6) . . ? N8 N7 C19 104.1(8) . . ? N8 N7 Fe1 119.3(7) . . ? C19 N7 Fe1 136.5(7) . . ? C21 N8 N7 113.0(10) . . ? C21 N8 C34 131.7(10) . . ? N7 N8 C34 115.3(8) . . ? C24 N9 N10 105.3(9) . . ? C24 N9 Fe1 139.8(8) . . ? N10 N9 Fe1 114.9(7) . . ? C26 N10 N9 111.8(10) . . ? C26 N10 C34 129.1(10) . . ? N9 N10 C34 119.1(9) . . ? C29 N11 N12 106.1(10) . . ? C29 N11 Fe1 139.5(8) . . ? N12 N11 Fe1 114.3(8) . . ? C31 N12 N11 107.8(10) . . ? C31 N12 C34 134.0(9) . . ? N11 N12 C34 118.3(10) . . ? C39 N13 N14 113.0(10) . . ? C39 N13 C38 131.2(9) . . ? N14 N13 C38 115.5(9) . . ? C41 N14 N13 103.8(8) . . ? C41 N14 Fe2 134.5(7) . . ? N13 N14 Fe2 121.4(8) . . ? C42 N15 C38 132.2(9) . . ? C42 N15 N16 107.9(10) . . ? C38 N15 N16 119.8(10) . . ? C44 N16 N15 105.0(10) . . ? C44 N16 Fe2 138.3(8) . . ? N15 N16 Fe2 116.2(9) . . ? C45 N17 N18 110.8(8) . . ? C45 N17 C38 131.8(8) . . ? N18 N17 C38 117.4(8) . . ? C47 N18 N17 104.4(9) . . ? C47 N18 Fe2 134.8(7) . . ? N17 N18 Fe2 120.5(7) . . ? C48 N19 N20 103.2(8) . . ? C48 N19 Fe2 141.7(7) . . ? N20 N19 Fe2 115.1(7) . . ? C50 N20 N19 110.5(8) . . ? C50 N20 C63 130.8(8) . . ? N19 N20 C63 118.3(8) . . ? C53 N21 N22 103.8(8) . . ? C53 N21 Fe2 137.3(7) . . ? N22 N21 Fe2 118.2(7) . . ? C55 N22 N21 111.5(10) . . ? C55 N22 C63 131.8(9) . . ? N21 N22 C63 116.3(9) . . ? C58 N23 N24 103.6(11) . . ? C58 N23 Fe2 140.2(8) . . ? N24 N23 Fe2 115.7(10) . . ? C60 N24 N23 113.0(12) . . ? C60 N24 C63 129.9(11) . . ? N23 N24 C63 116.9(11) . . ? N26 N25 C68 111.6(12) . . ? N26 N25 C67 118.7(11) . . ? C68 N25 C67 129.7(10) . . ? N25 N26 C70 106.7(11) . . ? N25 N26 Fe3 120.2(10) . . ? C70 N26 Fe3 132.3(9) . . ? C71 N27 N28 110.2(11) . . ? C71 N27 C67 131.8(10) . . ? N28 N27 C67 116.5(10) . . ? C73 N28 N27 105.0(10) . . ? C73 N28 Fe3 135.2(9) . . ? N27 N28 Fe3 119.8(8) . . ? C74 N29 N30 112.4(9) . . ? C74 N29 C67 129.0(9) . . ? N30 N29 C67 118.1(9) . . ? C76 N30 N29 104.2(10) . . ? C76 N30 Fe3 136.3(9) . . ? N29 N30 Fe3 119.2(7) . . ? C77 N31 N32 102.2(11) . . ? C77 N31 Fe3 141.5(9) . . ? N32 N31 Fe3 116.1(9) . . ? C79 N32 N31 111.3(12) . . ? C79 N32 C92 130.3(11) . . ? N31 N32 C92 118.3(11) . . ? N34 N33 C82 104.8(11) . . ? N34 N33 Fe3 116.4(11) . . ? C82 N33 Fe3 138.2(8) . . ? N33 N34 C84 109.7(15) . . ? N33 N34 C92 118.1(12) . . ? C84 N34 C92 132.0(13) . . ? N36 N35 C87 103.6(9) . . ? N36 N35 Fe3 118.4(8) . . ? C87 N35 Fe3 137.4(8) . . ? C89 N36 N35 114.6(12) . . ? C89 N36 C92 127.0(11) . . ? N35 N36 C92 117.9(9) . . ? N38 N37 C103 110.7(11) . . ? N38 N37 C102 119.9(9) . . ? C103 N37 C102 128.8(10) . . ? C105 N38 N37 106.7(10) . . ? C105 N38 Fe4 135.0(8) . . ? N37 N38 Fe4 118.1(8) . . ? N40 N39 C106 109.8(10) . . ? N40 N39 C102 119.8(9) . . ? C106 N39 C102 130.1(10) . . ? C108 N40 N39 105.4(9) . . ? C108 N40 Fe4 136.8(7) . . ? N39 N40 Fe4 117.6(7) . . ? C109 N41 N42 111.4(10) . . ? C109 N41 C102 132.4(9) . . ? N42 N41 C102 116.1(10) . . ? C111 N42 N41 101.9(10) . . ? C111 N42 Fe4 137.5(8) . . ? N41 N42 Fe4 120.4(8) . . ? C112 N43 N44 104.7(8) . . ? C112 N43 Fe4 137.2(7) . . ? N44 N43 Fe4 117.4(6) . . ? C114 N44 N43 112.2(9) . . ? C114 N44 C127 130.1(10) . . ? N43 N44 C127 117.5(8) . . ? C117 N45 N46 104.1(9) . . ? C117 N45 Fe4 140.8(7) . . ? N46 N45 Fe4 114.7(7) . . ? C119 N46 N45 110.9(9) . . ? C119 N46 C127 130.5(9) . . ? N45 N46 C127 118.3(9) . . ? C122 N47 N48 105.0(8) . . ? C122 N47 Fe4 138.2(7) . . ? N48 N47 Fe4 115.4(7) . . ? N47 N48 C124 110.1(9) . . ? N47 N48 C127 120.2(8) . . ? C124 N48 C127 129.5(9) . . ? C132 N49 N50 112.0(11) . . ? C132 N49 C131 130.5(11) . . ? N50 N49 C131 117.5(9) . . ? C134 N50 N49 103.8(9) . . ? C134 N50 Fe5 135.9(8) . . ? N49 N50 Fe5 120.3(8) . . ? C135 N51 N52 112.9(9) . . ? C135 N51 C131 127.4(9) . . ? N52 N51 C131 119.6(9) . . ? C137 N52 N51 106.3(9) . . ? C137 N52 Fe5 134.7(7) . . ? N51 N52 Fe5 118.9(7) . . ? C138 N53 N54 113.8(8) . . ? C138 N53 C131 129.1(8) . . ? N54 N53 C131 117.1(8) . . ? C140 N54 N53 103.9(8) . . ? C140 N54 Fe5 134.4(7) . . ? N53 N54 Fe5 121.0(6) . . ? C141 N55 N56 106.4(9) . . ? C141 N55 Fe5 136.4(8) . . ? N56 N55 Fe5 116.7(8) . . ? C143 N56 N55 112.1(9) . . ? C143 N56 C156 128.7(9) . . ? N55 N56 C156 119.0(9) . . ? C146 N57 N58 100.9(8) . . ? C146 N57 Fe5 141.5(8) . . ? N58 N57 Fe5 117.5(6) . . ? C148 N58 N57 110.9(8) . . ? C148 N58 C156 134.1(9) . . ? N57 N58 C156 114.9(8) . . ? C151 N59 N60 105.4(8) . . ? C151 N59 Fe5 136.4(7) . . ? N60 N59 Fe5 117.2(7) . . ? C153 N60 N59 112.5(9) . . ? C153 N60 C156 129.0(9) . . ? N59 N60 C156 118.2(9) . . ? C161 N61 N62 111.6(10) . . ? C161 N61 C160 130.9(11) . . ? N62 N61 C160 117.4(9) . . ? C163 N62 N61 105.7(10) . . ? C163 N62 Fe6 134.8(9) . . ? N61 N62 Fe6 119.1(7) . . ? C164 N63 C160 133.1(11) . . ? C164 N63 N64 108.8(11) . . ? C160 N63 N64 117.9(11) . . ? C166 N64 N63 107.7(12) . . ? C166 N64 Fe6 134.8(11) . . ? N63 N64 Fe6 117.4(8) . . ? C167 N65 N66 109.6(10) . . ? C167 N65 C160 134.0(10) . . ? N66 N65 C160 116.3(10) . . ? C169 N66 N65 104.4(10) . . ? C169 N66 Fe6 134.3(8) . . ? N65 N66 Fe6 120.5(8) . . ? C170 N67 N68 106.0(12) . . ? C170 N67 Fe6 139.8(10) . . ? N68 N67 Fe6 114.1(9) . . ? C172 N68 N67 110.0(13) . . ? C172 N68 C185 129.3(13) . . ? N67 N68 C185 120.6(11) . . ? C175 N69 N70 102.2(9) . . ? C175 N69 Fe6 137.9(8) . . ? N70 N69 Fe6 119.8(8) . . ? C177 N70 N69 112.9(11) . . ? C177 N70 C185 132.3(11) . . ? N69 N70 C185 114.8(10) . . ? C180 N71 N72 104.7(10) . . ? C180 N71 Fe6 136.8(8) . . ? N72 N71 Fe6 117.4(8) . . ? C182 N72 N71 110.4(11) . . ? C182 N72 C185 132.4(11) . . ? N71 N72 C185 117.2(11) . . ? C6 C1 C2 124.1(12) . . ? C6 C1 C7 121.5(12) . . ? C2 C1 C7 114.3(13) . . ? C3 C2 C1 118.4(12) . . ? C3 C2 C35 119.1(13) . . ? C1 C2 C35 122.5(11) . . ? C4 C3 C2 120.3(13) . . ? C4 C3 C36 118.4(12) . . ? C2 C3 C36 121.2(12) . . ? C3 C4 C5 119.5(13) . . ? C3 C4 C64 123.8(12) . . ? C5 C4 C64 116.7(13) . . ? C4 C5 C6 125.6(14) . . ? C4 C5 C65 123.3(14) . . ? C6 C5 C65 111.1(14) . . ? C1 C6 C5 111.9(13) . . ? C1 C6 C93 118.9(14) . . ? C5 C6 C93 129.1(16) . . ? O1 C7 C1 105.6(8) . . ? O1 C7 H7A 110.6 . . ? C1 C7 H7A 110.6 . . ? O1 C7 H7B 110.6 . . ? C1 C7 H7B 110.6 . . ? H7A C7 H7B 108.8 . . ? O1 C8 C9 107.4(8) . . ? O1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N5 C9 N3 107.2(10) . . ? N5 C9 N1 111.4(10) . . ? N3 C9 N1 108.6(9) . . ? N5 C9 C8 108.9(8) . . ? N3 C9 C8 108.3(10) . . ? N1 C9 C8 112.3(10) . . ? N1 C10 C11 111.2(11) . . ? N1 C10 H10 124.4 . . ? C11 C10 H10 124.4 . . ? C10 C11 C12 101.3(12) . . ? C10 C11 H11 129.3 . . ? C12 C11 H11 129.3 . . ? N2 C12 C11 112.0(11) . . ? N2 C12 H12 124.0 . . ? C11 C12 H12 124.0 . . ? C14 C13 N3 111.5(11) . . ? C14 C13 H13 124.2 . . ? N3 C13 H13 124.2 . . ? C13 C14 C15 102.6(14) . . ? C13 C14 H14 128.7 . . ? C15 C14 H14 128.7 . . ? N4 C15 C14 114.1(12) . . ? N4 C15 H15 123.0 . . ? C14 C15 H15 123.0 . . ? C17 C16 N5 108.0(9) . . ? C17 C16 H16 126.0 . . ? N5 C16 H16 126.0 . . ? C16 C17 C18 104.6(10) . . ? C16 C17 H17 127.7 . . ? C18 C17 H17 127.7 . . ? N6 C18 C17 111.5(10) . . ? N6 C18 H18 124.3 . . ? C17 C18 H18 124.3 . . ? N7 C19 C20 109.4(10) . . ? N7 C19 C22 124.9(9) . . ? C20 C19 C22 125.6(11) . . ? C21 C20 C19 106.7(11) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? C20 C21 N8 106.8(10) . . ? C20 C21 C23 131.3(11) . . ? N8 C21 C23 121.9(11) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N9 C24 C25 108.9(11) . . ? N9 C24 C27 121.5(12) . . ? C25 C24 C27 129.4(13) . . ? C26 C25 C24 107.3(12) . . ? C26 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? N10 C26 C25 106.6(11) . . ? N10 C26 C28 125.3(12) . . ? C25 C26 C28 127.9(12) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N11 C29 C30 109.3(11) . . ? N11 C29 C32 120.6(11) . . ? C30 C29 C32 130.0(13) . . ? C31 C30 C29 108.0(13) . . ? C31 C30 H30 126.0 . . ? C29 C30 H30 126.0 . . ? C30 C31 N12 108.7(10) . . ? C30 C31 C33 131.2(14) . . ? N12 C31 C33 120.0(12) . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N8 C34 N10 112.0(11) . . ? N8 C34 N12 113.2(10) . . ? N10 C34 N12 108.7(9) . . ? N8 C34 H34 107.6 . . ? N10 C34 H34 107.6 . . ? N12 C34 H34 107.6 . . ? C2 C35 H35A 109.5 . . ? C2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O2 C36 C3 106.3(8) . . ? O2 C36 H36A 110.5 . . ? C3 C36 H36A 110.5 . . ? O2 C36 H36B 110.5 . . ? C3 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? O2 C37 C38 106.3(8) . . ? O2 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? O2 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? N15 C38 N17 110.6(8) . . ? N15 C38 N13 107.8(9) . . ? N17 C38 N13 108.4(10) . . ? N15 C38 C37 111.6(10) . . ? N17 C38 C37 111.0(8) . . ? N13 C38 C37 107.3(8) . . ? N13 C39 C40 107.5(10) . . ? N13 C39 H39 126.2 . . ? C40 C39 H39 126.2 . . ? C41 C40 C39 105.6(10) . . ? C41 C40 H40 127.2 . . ? C39 C40 H40 127.2 . . ? C40 C41 N14 110.1(10) . . ? C40 C41 H41 125.0 . . ? N14 C41 H41 125.0 . . ? N15 C42 C43 109.0(10) . . ? N15 C42 H42 125.5 . . ? C43 C42 H42 125.5 . . ? C44 C43 C42 106.1(13) . . ? C44 C43 H43 127.0 . . ? C42 C43 H43 127.0 . . ? N16 C44 C43 111.8(12) . . ? N16 C44 H44 124.1 . . ? C43 C44 H44 124.1 . . ? C46 C45 N17 107.4(10) . . ? C46 C45 H45 126.3 . . ? N17 C45 H45 126.3 . . ? C45 C46 C47 104.4(11) . . ? C45 C46 H46 127.8 . . ? C47 C46 H46 127.8 . . ? N18 C47 C46 112.8(11) . . ? N18 C47 H47 123.6 . . ? C46 C47 H47 123.6 . . ? N19 C48 C49 113.1(11) . . ? N19 C48 C51 120.2(10) . . ? C49 C48 C51 126.7(12) . . ? C50 C49 C48 106.9(13) . . ? C50 C49 H49 126.5 . . ? C48 C49 H49 126.5 . . ? C49 C50 N20 106.2(10) . . ? C49 C50 C52 133.4(12) . . ? N20 C50 C52 120.3(11) . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N21 C53 C54 112.2(10) . . ? N21 C53 C56 123.4(9) . . ? C54 C53 C56 124.2(12) . . ? C55 C54 C53 105.4(11) . . ? C55 C54 H54 127.3 . . ? C53 C54 H54 127.3 . . ? N22 C55 C54 106.8(9) . . ? N22 C55 C57 124.5(10) . . ? C54 C55 C57 128.7(11) . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N23 C58 C59 108.7(12) . . ? N23 C58 C61 122.7(12) . . ? C59 C58 C61 128.3(14) . . ? C58 C59 C60 113.2(15) . . ? C58 C59 H59 123.4 . . ? C60 C59 H59 123.4 . . ? C59 C60 N24 101.4(12) . . ? C59 C60 C62 135.0(17) . . ? N24 C60 C62 123.6(15) . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.4 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N22 C63 N20 111.9(11) . . ? N22 C63 N24 110.9(9) . . ? N20 C63 N24 110.5(10) . . ? N22 C63 H63 107.8 . . ? N20 C63 H63 107.8 . . ? N24 C63 H63 107.8 . . ? C4 C64 H64A 109.5 . . ? C4 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C4 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O3 C65 C5 107.6(10) . . ? O3 C65 H65A 110.2 . . ? C5 C65 H65A 110.2 . . ? O3 C65 H65B 110.2 . . ? C5 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? O3 C66 C67 106.4(11) . . ? O3 C66 H66A 110.5 . . ? C67 C66 H66A 110.5 . . ? O3 C66 H66B 110.5 . . ? C67 C66 H66B 110.5 . . ? H66A C66 H66B 108.6 . . ? N25 C67 N29 110.7(9) . . ? N25 C67 N27 107.4(11) . . ? N29 C67 N27 107.2(10) . . ? N25 C67 C66 110.7(11) . . ? N29 C67 C66 109.9(10) . . ? N27 C67 C66 110.8(10) . . ? C69 C68 N25 107.8(11) . . ? C69 C68 H68 126.1 . . ? N25 C68 H68 126.1 . . ? C68 C69 C70 104.8(13) . . ? C68 C69 H69 127.6 . . ? C70 C69 H69 127.6 . . ? N26 C70 C69 109.1(12) . . ? N26 C70 H70 125.5 . . ? C69 C70 H70 125.5 . . ? N27 C71 C72 110.4(11) . . ? N27 C71 H71 124.8 . . ? C72 C71 H71 124.8 . . ? C71 C72 C73 101.5(12) . . ? C71 C72 H72 129.3 . . ? C73 C72 H72 129.3 . . ? N28 C73 C72 112.8(12) . . ? N28 C73 H73 123.6 . . ? C72 C73 H73 123.6 . . ? N29 C74 C75 106.6(9) . . ? N29 C74 H74 126.7 . . ? C75 C74 H74 126.7 . . ? C76 C75 C74 101.5(11) . . ? C76 C75 H75 129.2 . . ? C74 C75 H75 129.2 . . ? N30 C76 C75 115.0(11) . . ? N30 C76 H76 122.5 . . ? C75 C76 H76 122.5 . . ? N31 C77 C78 115.2(14) . . ? N31 C77 C80 120.6(13) . . ? C78 C77 C80 122.8(16) . . ? C77 C78 C79 102.4(15) . . ? C77 C78 H78 128.8 . . ? C79 C78 H78 128.8 . . ? N32 C79 C78 108.1(11) . . ? N32 C79 C81 121.7(14) . . ? C78 C79 C81 130.1(15) . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 N33 109.6(15) . . ? C83 C82 C85 129.4(18) . . ? N33 C82 C85 121.0(12) . . ? C84 C83 C82 109.2(17) . . ? C84 C83 H83 125.4 . . ? C82 C83 H83 125.4 . . ? C83 C84 N34 106.6(14) . . ? C83 C84 C86 132.7(16) . . ? N34 C84 C86 120.7(18) . . ? C82 C85 H85A 109.5 . . ? C82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N35 C87 C88 110.4(12) . . ? N35 C87 C90 123.1(11) . . ? C88 C87 C90 126.4(14) . . ? C89 C88 C87 105.9(14) . . ? C89 C88 H88 127.0 . . ? C87 C88 H88 127.0 . . ? N36 C89 C88 105.4(13) . . ? N36 C89 C91 126.2(15) . . ? C88 C89 C91 128.4(15) . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N32 C92 N36 113.9(14) . . ? N32 C92 N34 108.2(12) . . ? N36 C92 N34 106.6(12) . . ? N32 C92 H92 109.3 . . ? N36 C92 H92 109.3 . . ? N34 C92 H92 109.3 . . ? C6 C93 H93A 109.5 . . ? C6 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C6 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C99 C94 C95 119.2(14) . . ? C99 C94 C100 121.0(16) . . ? C95 C94 C100 119.8(15) . . ? C96 C95 C94 118.2(13) . . ? C96 C95 C128 120.8(14) . . ? C94 C95 C128 121.0(14) . . ? C95 C96 C97 123.4(13) . . ? C95 C96 C129 118.0(12) . . ? C97 C96 C129 118.3(13) . . ? C96 C97 C98 117.0(13) . . ? C96 C97 C157 123.1(12) . . ? C98 C97 C157 120.0(12) . . ? C99 C98 C97 123.0(14) . . ? C99 C98 C158 117.3(14) . . ? C97 C98 C158 119.6(14) . . ? C98 C99 C94 119.0(14) . . ? C98 C99 C186 123.0(17) . . ? C94 C99 C186 118.0(16) . . ? O4 C100 C94 103.4(10) . . ? O4 C100 H10A 111.1 . . ? C94 C100 H10A 111.1 . . ? O4 C100 H10B 111.1 . . ? C94 C100 H10B 111.1 . . ? H10A C100 H10B 109.0 . . ? O4 C101 C102 109.5(10) . . ? O4 C101 H10C 109.8 . . ? C102 C101 H10C 109.8 . . ? O4 C101 H10D 109.8 . . ? C102 C101 H10D 109.8 . . ? H10C C101 H10D 108.2 . . ? N39 C102 N37 109.2(10) . . ? N39 C102 N41 110.3(10) . . ? N37 C102 N41 104.4(10) . . ? N39 C102 C101 113.9(11) . . ? N37 C102 C101 110.9(11) . . ? N41 C102 C101 107.7(11) . . ? C104 C103 N37 107.3(11) . . ? C104 C103 H103 126.4 . . ? N37 C103 H103 126.4 . . ? C103 C104 C105 104.6(12) . . ? C103 C104 H104 127.7 . . ? C105 C104 H104 127.7 . . ? N38 C105 C104 110.6(12) . . ? N38 C105 H105 124.7 . . ? C104 C105 H105 124.7 . . ? C107 C106 N39 108.8(11) . . ? C107 C106 H106 125.6 . . ? N39 C106 H106 125.6 . . ? C106 C107 C108 103.5(11) . . ? C106 C107 H107 128.3 . . ? C108 C107 H107 128.3 . . ? N40 C108 C107 112.5(10) . . ? N40 C108 H108 123.8 . . ? C107 C108 H108 123.8 . . ? C110 C109 N41 106.8(10) . . ? C110 C109 H109 126.6 . . ? N41 C109 H109 126.6 . . ? C109 C110 C111 104.3(12) . . ? C109 C110 H110 127.8 . . ? C111 C110 H110 127.8 . . ? N42 C111 C110 115.2(12) . . ? N42 C111 H111 122.4 . . ? C110 C111 H111 122.4 . . ? N43 C112 C113 110.7(10) . . ? N43 C112 C115 124.6(10) . . ? C113 C112 C115 124.7(11) . . ? C112 C113 C114 106.1(11) . . ? C112 C113 H113 127.0 . . ? C114 C113 H113 127.0 . . ? N44 C114 C113 106.1(10) . . ? N44 C114 C116 123.6(10) . . ? C113 C114 C116 130.1(10) . . ? C112 C115 H11A 109.5 . . ? C112 C115 H11B 109.5 . . ? H11A C115 H11B 109.5 . . ? C112 C115 H11C 109.5 . . ? H11A C115 H11C 109.5 . . ? H11B C115 H11C 109.5 . . ? C114 C116 H11D 109.5 . . ? C114 C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? C114 C116 H11F 109.5 . . ? H11D C116 H11F 109.5 . . ? H11E C116 H11F 109.5 . . ? N45 C117 C118 112.8(10) . . ? N45 C117 C120 122.6(10) . . ? C118 C117 C120 124.6(11) . . ? C117 C118 C119 104.7(11) . . ? C117 C118 H118 127.7 . . ? C119 C118 H118 127.7 . . ? N46 C119 C118 107.5(11) . . ? N46 C119 C121 123.6(11) . . ? C118 C119 C121 128.8(12) . . ? C117 C120 H12A 109.5 . . ? C117 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C117 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C119 C121 H12D 109.5 . . ? C119 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C119 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? N47 C122 C123 111.8(10) . . ? N47 C122 C125 122.7(10) . . ? C123 C122 C125 125.0(12) . . ? C124 C123 C122 105.5(11) . . ? C124 C123 H123 127.2 . . ? C122 C123 H123 127.2 . . ? C123 C124 N48 107.4(10) . . ? C123 C124 C126 131.3(11) . . ? N48 C124 C126 121.3(11) . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C124 C126 H12J 109.5 . . ? C124 C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? C124 C126 H12L 109.5 . . ? H12J C126 H12L 109.5 . . ? H12K C126 H12L 109.5 . . ? N48 C127 N44 111.4(9) . . ? N48 C127 N46 110.3(9) . . ? N44 C127 N46 108.4(9) . . ? N48 C127 H127 108.9 . . ? N44 C127 H127 108.9 . . ? N46 C127 H127 108.9 . . ? C95 C128 H12M 109.5 . . ? C95 C128 H12N 109.5 . . ? H12M C128 H12N 109.5 . . ? C95 C128 H12O 109.5 . . ? H12M C128 H12O 109.5 . . ? H12N C128 H12O 109.5 . . ? O5 C129 C96 110.3(9) . . ? O5 C129 H12P 109.6 . . ? C96 C129 H12P 109.6 . . ? O5 C129 H12Q 109.6 . . ? C96 C129 H12Q 109.6 . . ? H12P C129 H12Q 108.1 . . ? O5 C130 C131 106.8(8) . . ? O5 C130 H13A 110.4 . . ? C131 C130 H13A 110.4 . . ? O5 C130 H13B 110.4 . . ? C131 C130 H13B 110.4 . . ? H13A C130 H13B 108.6 . . ? N53 C131 N49 109.4(9) . . ? N53 C131 N51 109.0(9) . . ? N49 C131 N51 105.7(8) . . ? N53 C131 C130 109.7(8) . . ? N49 C131 C130 110.3(9) . . ? N51 C131 C130 112.7(9) . . ? N49 C132 C133 106.8(12) . . ? N49 C132 H132 126.6 . . ? C133 C132 H132 126.6 . . ? C134 C133 C132 102.8(12) . . ? C134 C133 H133 128.6 . . ? C132 C133 H133 128.6 . . ? N50 C134 C133 114.3(12) . . ? N50 C134 H134 122.9 . . ? C133 C134 H134 122.9 . . ? N51 C135 C136 106.7(10) . . ? N51 C135 H135 126.6 . . ? C136 C135 H135 126.6 . . ? C135 C136 C137 105.9(12) . . ? C135 C136 H136 127.1 . . ? C137 C136 H136 127.1 . . ? N52 C137 C136 108.2(11) . . ? N52 C137 H137 125.9 . . ? C136 C137 H137 125.9 . . ? N53 C138 C139 104.2(9) . . ? N53 C138 H138 127.9 . . ? C139 C138 H138 127.9 . . ? C140 C139 C138 105.5(10) . . ? C140 C139 H139 127.2 . . ? C138 C139 H139 127.2 . . ? N54 C140 C139 112.5(9) . . ? N54 C140 H140 123.8 . . ? C139 C140 H140 123.8 . . ? N55 C141 C142 109.2(12) . . ? N55 C141 C144 124.0(11) . . ? C142 C141 C144 126.7(14) . . ? C143 C142 C141 106.6(14) . . ? C143 C142 H142 126.7 . . ? C141 C142 H142 126.7 . . ? N56 C143 C142 105.7(11) . . ? N56 C143 C145 125.5(11) . . ? C142 C143 C145 128.7(13) . . ? C141 C144 H14A 109.5 . . ? C141 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C141 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? C143 C145 H14D 109.5 . . ? C143 C145 H14E 109.5 . . ? H14D C145 H14E 109.5 . . ? C143 C145 H14F 109.5 . . ? H14D C145 H14F 109.5 . . ? H14E C145 H14F 109.5 . . ? N57 C146 C147 113.1(11) . . ? N57 C146 C149 118.8(11) . . ? C147 C146 C149 128.1(11) . . ? C148 C147 C146 106.3(12) . . ? C148 C147 H147 126.9 . . ? C146 C147 H147 126.9 . . ? C147 C148 N58 108.6(11) . . ? C147 C148 C150 131.3(11) . . ? N58 C148 C150 120.1(9) . . ? C146 C149 H14G 109.5 . . ? C146 C149 H14H 109.5 . . ? H14G C149 H14H 109.5 . . ? C146 C149 H14I 109.5 . . ? H14G C149 H14I 109.5 . . ? H14H C149 H14I 109.5 . . ? C148 C150 H15A 109.5 . . ? C148 C150 H15B 109.5 . . ? H15A C150 H15B 109.5 . . ? C148 C150 H15C 109.5 . . ? H15A C150 H15C 109.5 . . ? H15B C150 H15C 109.5 . . ? N59 C151 C152 109.4(9) . . ? N59 C151 C154 124.2(10) . . ? C152 C151 C154 126.3(12) . . ? C153 C152 C151 106.0(11) . . ? C153 C152 H152 127.0 . . ? C151 C152 H152 127.0 . . ? N60 C153 C152 106.4(11) . . ? N60 C153 C155 126.2(10) . . ? C152 C153 C155 127.2(11) . . ? C151 C154 H15D 109.5 . . ? C151 C154 H15E 109.5 . . ? H15D C154 H15E 109.5 . . ? C151 C154 H15F 109.5 . . ? H15D C154 H15F 109.5 . . ? H15E C154 H15F 109.5 . . ? C153 C155 H15G 109.5 . . ? C153 C155 H15H 109.5 . . ? H15G C155 H15H 109.5 . . ? C153 C155 H15I 109.5 . . ? H15G C155 H15I 109.5 . . ? H15H C155 H15I 109.5 . . ? N56 C156 N60 112.5(9) . . ? N56 C156 N58 110.6(9) . . ? N60 C156 N58 109.1(9) . . ? N56 C156 H156 108.2 . . ? N60 C156 H156 108.2 . . ? N58 C156 H156 108.2 . . ? C97 C157 H15J 109.5 . . ? C97 C157 H15K 109.5 . . ? H15J C157 H15K 109.5 . . ? C97 C157 H15L 109.5 . . ? H15J C157 H15L 109.5 . . ? H15K C157 H15L 109.5 . . ? O6 C158 C98 107.9(10) . . ? O6 C158 H15M 110.1 . . ? C98 C158 H15M 110.1 . . ? O6 C158 H15N 110.1 . . ? C98 C158 H15N 110.1 . . ? H15M C158 H15N 108.4 . . ? O6 C159 C160 103.8(9) . . ? O6 C159 H15O 111.0 . . ? C160 C159 H15O 111.0 . . ? O6 C159 H15P 111.0 . . ? C160 C159 H15P 111.0 . . ? H15O C159 H15P 109.0 . . ? N63 C160 N65 113.3(10) . . ? N63 C160 N61 108.0(10) . . ? N65 C160 N61 106.0(10) . . ? N63 C160 C159 113.7(12) . . ? N65 C160 C159 109.7(11) . . ? N61 C160 C159 105.6(10) . . ? N61 C161 C162 104.5(12) . . ? N61 C161 H161 127.7 . . ? C162 C161 H161 127.7 . . ? C163 C162 C161 107.5(12) . . ? C163 C162 H162 126.2 . . ? C161 C162 H162 126.2 . . ? N62 C163 C162 110.7(12) . . ? N62 C163 H163 124.7 . . ? C162 C163 H163 124.7 . . ? N63 C164 C165 106.7(14) . . ? N63 C164 H164 126.7 . . ? C165 C164 H164 126.7 . . ? C164 C165 C166 108.1(16) . . ? C164 C165 H165 125.9 . . ? C166 C165 H165 125.9 . . ? N64 C166 C165 108.5(15) . . ? N64 C166 H166 125.8 . . ? C165 C166 H166 125.8 . . ? C168 C167 N65 108.8(11) . . ? C168 C167 H167 125.6 . . ? N65 C167 H167 125.6 . . ? C167 C168 C169 106.7(14) . . ? C167 C168 H168 126.7 . . ? C169 C168 H168 126.7 . . ? N66 C169 C168 110.4(12) . . ? N66 C169 H169 124.8 . . ? C168 C169 H169 124.8 . . ? N67 C170 C171 107.7(14) . . ? N67 C170 C173 121.6(13) . . ? C171 C170 C173 130.5(15) . . ? C172 C171 C170 110.4(16) . . ? C172 C171 H171 124.8 . . ? C170 C171 H171 124.8 . . ? C171 C172 N68 105.5(15) . . ? C171 C172 C174 130.4(15) . . ? N68 C172 C174 123.9(14) . . ? C170 C173 H17A 109.5 . . ? C170 C173 H17B 109.5 . . ? H17A C173 H17B 109.5 . . ? C170 C173 H17C 109.5 . . ? H17A C173 H17C 109.5 . . ? H17B C173 H17C 109.5 . . ? C172 C174 H17D 109.5 . . ? C172 C174 H17E 109.5 . . ? H17D C174 H17E 109.5 . . ? C172 C174 H17F 109.5 . . ? H17D C174 H17F 109.5 . . ? H17E C174 H17F 109.5 . . ? N69 C175 C176 110.2(11) . . ? N69 C175 C178 123.7(11) . . ? C176 C175 C178 126.0(13) . . ? C177 C176 C175 108.9(13) . . ? C177 C176 H176 125.5 . . ? C175 C176 H176 125.5 . . ? C176 C177 N70 105.8(12) . . ? C176 C177 C179 132.2(14) . . ? N70 C177 C179 122.1(14) . . ? C175 C178 H17G 109.5 . . ? C175 C178 H17H 109.5 . . ? H17G C178 H17H 109.5 . . ? C175 C178 H17I 109.5 . . ? H17G C178 H17I 109.5 . . ? H17H C178 H17I 109.5 . . ? C177 C179 H17J 109.5 . . ? C177 C179 H17K 109.5 . . ? H17J C179 H17K 109.5 . . ? C177 C179 H17L 109.5 . . ? H17J C179 H17L 109.5 . . ? H17K C179 H17L 109.5 . . ? N71 C180 C181 109.9(11) . . ? N71 C180 C183 125.1(12) . . ? C181 C180 C183 125.0(14) . . ? C182 C181 C180 107.9(13) . . ? C182 C181 H181 126.0 . . ? C180 C181 H181 126.0 . . ? C181 C182 N72 107.1(12) . . ? C181 C182 C184 131.2(15) . . ? N72 C182 C184 121.6(13) . . ? C180 C183 H18A 109.5 . . ? C180 C183 H18B 109.4 . . ? H18A C183 H18B 109.5 . . ? C180 C183 H18C 109.4 . . ? H18A C183 H18C 109.5 . . ? H18B C183 H18C 109.5 . . ? C180 C183 H18D 109.4 . . ? H18A C183 H18D 141.1 . . ? H18B C183 H18D 56.3 . . ? H18C C183 H18D 56.3 . . ? C180 C183 H18E 109.5 . . ? H18A C183 H18E 56.2 . . ? H18B C183 H18E 141.1 . . ? H18C C183 H18E 56.3 . . ? H18D C183 H18E 109.5 . . ? C180 C183 H18F 109.5 . . ? H18A C183 H18F 56.3 . . ? H18B C183 H18F 56.3 . . ? H18C C183 H18F 141.1 . . ? H18D C183 H18F 109.5 . . ? H18E C183 H18F 109.5 . . ? C182 C184 H18G 109.5 . . ? C182 C184 H18H 109.5 . . ? H18G C184 H18H 109.5 . . ? C182 C184 H18I 109.5 . . ? H18G C184 H18I 109.5 . . ? H18H C184 H18I 109.5 . . ? N72 C185 N70 110.3(11) . . ? N72 C185 N68 111.6(11) . . ? N70 C185 N68 109.9(12) . . ? N72 C185 H185 108.3 . . ? N70 C185 H185 108.3 . . ? N68 C185 H185 108.3 . . ? C99 C186 H18J 109.5 . . ? C99 C186 H18K 109.5 . . ? H18J C186 H18K 109.5 . . ? C99 C186 H18L 109.5 . . ? H18J C186 H18L 109.5 . . ? H18K C186 H18L 109.5 . . ? 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 Fe1 N7 N8 C34 2.1(15) . . . . ? Fe1 N9 N10 C34 1.5(13) . . . . ? Fe1 N11 N12 C34 1.9(11) . . . . ? Fe1 N2 N1 C9 6.1(13) . . . . ? Fe1 N4 N3 C9 6.2(12) . . . . ? Fe1 N6 N5 C9 1.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 2.074 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.133 # Attachment '- 4-220finalDec6.CIF' #========================================================================== data_4.solvent(220K) _database_code_depnum_ccdc_archive 'CCDC 803929' #TrackingRef '- 4-220finalDec6.CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}3(C6(CH3)3(CH2OCH2C(pz)3]3)](BF4)6 ; _chemical_name_common ((Fe((3,5-Me2pz)3CH))3(C6(CH3)3(CH2OCH2C(pz)3)3))(BF4)6 _chemical_melting_point ? _chemical_formula_moiety '2(C93 H114 Fe3 N36 O3), 12(B F4)' _chemical_formula_sum 'C93 H117 B6 F24 Fe3 N36 O3.75' _chemical_formula_weight 2487.64 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 0.3485 0.8567 '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 23.163(8) _cell_length_b 23.362(8) _cell_length_c 24.048(6) _cell_angle_alpha 77.637(16) _cell_angle_beta 83.25(3) _cell_angle_gamma 83.232(16) _cell_volume 12566(7) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 149112 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 27.18 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5124 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9913 _exptl_absorpt_correction_T_max 0.9991 _exptl_absorpt_process_details 'XDS (Kabsch, 1993)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71253 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 149112 _diffrn_reflns_av_R_equivalents 0.1239 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.18 _reflns_number_total 48008 _reflns_number_gt 20562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.013 0.013 0.007 2164 729 ' ' 2 0.233 0.200 0.742 7 0 ' ' 3 0.267 0.321 0.904 8 3 ' ' 4 0.733 0.679 0.096 8 3 ' ' 5 0.767 0.800 0.258 7 1 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 48008 _refine_ls_number_parameters 2884 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.2052 _refine_ls_R_factor_gt 0.1330 _refine_ls_wR_factor_ref 0.3421 _refine_ls_wR_factor_gt 0.3201 _refine_ls_goodness_of_fit_ref 1.435 _refine_ls_restrained_S_all 1.433 _refine_ls_shift/su_max 0.022 _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 B1D B -0.0608(4) 0.7356(4) 0.6959(3) 0.120 Uani 1 1 d D . . F1D F -0.1092(4) 0.7523(4) 0.7232(4) 0.252 Uani 1 1 d D . . F2D F -0.0644(4) 0.6856(3) 0.6776(4) 0.221 Uani 1 1 d D . . F3D F -0.0469(4) 0.7765(3) 0.6494(3) 0.193 Uani 1 1 d D . . F4D F -0.0179(5) 0.7264(5) 0.7281(4) 0.301 Uani 1 1 d D . . B1A B 0.0027(9) 0.4993(8) 0.4693(10) 0.050 Uiso 0.50 1 d PD A -1 F1A F -0.0376(5) 0.5640(5) 0.4548(5) 0.091 Uiso 0.50 1 d PD A -1 F2A F 0.0578(4) 0.5294(4) 0.4423(4) 0.085 Uiso 0.50 1 d PD A -1 F3A F -0.0109(4) 0.4700(4) 0.4352(4) 0.082 Uiso 0.50 1 d PD A -1 F4A F 0.0043(7) 0.4817(6) 0.5235(7) 0.116 Uiso 0.50 1 d PD A -1 B1B B 0.5012(14) 0.9918(11) 0.0323(15) 0.109 Uani 0.50 1 d PD B -1 F1B F 0.5558(4) 0.9743(4) 0.0593(4) 0.077 Uani 0.50 1 d PD B -1 F2B F 0.4697(3) 1.0312(4) 0.0674(4) 0.068 Uani 0.50 1 d PD B -1 F3B F 0.4690(4) 0.9402(5) 0.0459(5) 0.090 Uani 0.50 1 d PD B -1 F4B F 0.5090(5) 1.0196(7) -0.0230(6) 0.107 Uani 0.50 1 d PD B -1 B1C B -0.2492(3) 0.2880(4) 0.6336(3) 0.112 Uiso 1 1 d D . . F1C F -0.2946(4) 0.2886(5) 0.6705(4) 0.385 Uiso 1 1 d D . . F2C F -0.2068(3) 0.3171(3) 0.6456(3) 0.166 Uiso 1 1 d D . . F3C F -0.2261(4) 0.2327(3) 0.6330(4) 0.182 Uiso 1 1 d D . . F4C F -0.2628(3) 0.3121(3) 0.5822(3) 0.146 Uiso 1 1 d D . . B1E B 0.2893(3) 0.3171(4) 0.6117(3) 0.102 Uani 1 1 d D . . F1E F 0.2954(3) 0.3068(3) 0.5604(2) 0.169 Uani 1 1 d D . . F2E F 0.2964(3) 0.2672(3) 0.6516(3) 0.186 Uani 1 1 d D . . F3E F 0.3292(4) 0.3517(4) 0.6181(3) 0.214 Uani 1 1 d D . . F4E F 0.2378(3) 0.3433(4) 0.6229(3) 0.195 Uani 1 1 d D . . B1F B 0.2264(5) 1.2003(5) -0.1307(4) 0.069 Uani 1 1 d . . . F1F F 0.1739(3) 1.1743(3) -0.1304(3) 0.121 Uani 1 1 d . . . F2F F 0.2745(3) 1.1674(3) -0.1479(2) 0.130 Uani 1 1 d . . . F3F F 0.2217(3) 1.2519(3) -0.1650(3) 0.147 Uani 1 1 d . . . F4F F 0.2256(3) 1.2020(3) -0.0738(3) 0.126 Uani 1 1 d . . . B1G B 0.7692(3) 1.1826(4) -0.1130(3) 0.155 Uani 1 1 d D . . F1G F 0.7217(3) 1.1657(4) -0.1249(3) 0.204 Uani 1 1 d D . . F2G F 0.8157(4) 1.1433(4) -0.1196(4) 0.319 Uani 1 1 d D . . F3G F 0.7648(4) 1.1888(4) -0.0585(2) 0.194 Uani 1 1 d D . . F4G F 0.7805(4) 1.2329(3) -0.1457(3) 0.220 Uani 1 1 d D . . B1H B -0.1985(5) 0.5827(6) -0.0183(4) 0.074 Uani 1 1 d . . . F1H F -0.1556(3) 0.6160(5) -0.0466(3) 0.177 Uani 1 1 d . . . F2H F -0.2425(2) 0.5853(3) -0.0530(2) 0.111 Uani 1 1 d . . . F3H F -0.2179(2) 0.6011(2) 0.0315(2) 0.086 Uani 1 1 d . . . F4H F -0.1722(3) 0.5298(3) -0.0082(3) 0.146 Uani 1 1 d . . . B1I B 0.3246(4) 1.0998(4) 0.4547(3) 0.144 Uani 1 1 d D . . F1I F 0.3144(3) 1.1286(3) 0.4957(2) 0.120 Uani 1 1 d D . . F2I F 0.2845(3) 1.1158(4) 0.4166(3) 0.190 Uani 1 1 d D . . F3I F 0.3767(3) 1.1097(5) 0.4257(3) 0.239 Uani 1 1 d D . . F4I F 0.3247(4) 1.0433(3) 0.4746(4) 0.215 Uani 1 1 d D . . B1J B 0.2886(3) 0.6098(3) -0.0343(3) 0.119 Uiso 1 1 d D . . F1J F 0.3237(2) 0.6414(2) -0.0709(2) 0.104 Uiso 1 1 d D . . F2J F 0.2852(4) 0.6229(4) 0.0180(3) 0.209 Uiso 1 1 d D . . F3J F 0.2343(2) 0.6190(3) -0.0504(3) 0.151 Uiso 1 1 d D . . F4J F 0.3055(4) 0.5540(3) -0.0294(4) 0.279 Uiso 1 1 d D . . B1K B 0.5403(9) 0.7725(9) -0.1999(9) 0.134 Uiso 1 1 d . . . F1K F 0.5172(4) 0.8214(4) -0.1826(4) 0.161 Uiso 1 1 d . . . F2K F 0.5585(4) 0.7748(4) -0.2547(5) 0.190 Uiso 1 1 d . . . F3K F 0.5524(5) 0.7262(5) -0.1608(5) 0.204 Uiso 1 1 d . . . F4K F 0.4804(6) 0.7588(6) -0.2098(6) 0.125 Uiso 0.50 1 d P . . F5K F 0.6033(9) 0.7768(9) -0.1929(8) 0.187 Uiso 0.50 1 d P . . Fe1 Fe 0.24608(4) 0.45475(5) 0.29098(4) 0.050 Uani 1 1 d . . . Fe2 Fe -0.19241(4) 0.43552(5) 0.31117(4) 0.049 Uani 1 1 d . . . Fe3 Fe -0.02869(5) 0.80140(6) 0.36184(4) 0.063 Uani 1 1 d . . . Fe4 Fe 0.51743(4) 0.69781(5) 0.13295(4) 0.046 Uani 1 1 d . . . Fe5 Fe 0.24557(4) 1.05967(5) 0.19609(4) 0.044 Uani 1 1 d . . . Fe6 Fe 0.68520(5) 1.04916(5) 0.21064(5) 0.061 Uani 1 1 d . . . O1 O 0.1487(2) 0.5646(2) 0.10918(19) 0.062 Uani 1 1 d . . . O2 O -0.0993(2) 0.5594(2) 0.12342(18) 0.058 Uani 1 1 d . . . O3 O -0.0051(2) 0.7699(2) 0.15201(19) 0.058 Uani 1 1 d . . . O4 O 0.4837(2) 0.7292(2) 0.34302(19) 0.061 Uani 1 1 d . . . O5 O 0.3279(2) 0.9321(2) 0.38028(19) 0.052 Uani 1 1 d . . . O6 O 0.5757(2) 0.9351(3) 0.3948(2) 0.072 Uani 1 1 d . . . O7 O 0.4683(16) 0.8957(16) 0.2844(16) 0.293 Uiso 0.50 1 d P . . O8 O 0.0509(18) 0.5594(18) 0.2005(17) 0.314 Uiso 0.50 1 d P C 1 O9 O 0.0026(18) 0.6119(18) 0.2243(17) 0.314 Uiso 0.50 1 d P D 2 N1 N 0.1909(2) 0.4607(3) 0.1881(2) 0.051 Uani 1 1 d . . . N2 N 0.1998(3) 0.4271(3) 0.2416(2) 0.059 Uani 1 1 d . . . N3 N 0.2019(3) 0.5531(3) 0.2094(3) 0.058 Uani 1 1 d . . . N4 N 0.2072(2) 0.5318(3) 0.2665(2) 0.056 Uani 1 1 d . . . N5 N 0.2840(2) 0.4991(3) 0.1723(2) 0.045 Uani 1 1 d . . . N6 N 0.3035(2) 0.4734(3) 0.2239(2) 0.048 Uani 1 1 d . . . N7 N 0.1866(3) 0.4349(3) 0.3582(2) 0.059 Uani 1 1 d . . . N8 N 0.2062(3) 0.4061(3) 0.4085(2) 0.054 Uani 1 1 d . . . N9 N 0.2927(2) 0.4835(3) 0.3415(2) 0.050 Uani 1 1 d . . . N10 N 0.2963(3) 0.4489(3) 0.3952(2) 0.051 Uani 1 1 d . . . N11 N 0.2872(3) 0.3744(3) 0.3145(2) 0.056 Uani 1 1 d . . . N12 N 0.2932(3) 0.3562(3) 0.3719(2) 0.056 Uani 1 1 d . . . N13 N -0.2019(3) 0.4491(3) 0.1895(2) 0.059 Uani 1 1 d . . . N14 N -0.2197(3) 0.4183(3) 0.2429(3) 0.062 Uani 1 1 d . . . N15 N -0.1852(2) 0.5362(3) 0.2186(2) 0.049 Uani 1 1 d . . . N16 N -0.2047(3) 0.5188(3) 0.2756(2) 0.053 Uani 1 1 d . . . N17 N -0.1080(2) 0.4611(3) 0.2147(2) 0.048 Uani 1 1 d . . . N18 N -0.1145(3) 0.4349(3) 0.2707(2) 0.055 Uani 1 1 d . . . N19 N -0.2713(3) 0.4362(3) 0.3522(2) 0.058 Uani 1 1 d . . . N20 N -0.2755(2) 0.4033(3) 0.4084(2) 0.055 Uani 1 1 d . . . N21 N -0.1653(3) 0.4546(3) 0.3794(2) 0.053 Uani 1 1 d . . . N22 N -0.1852(3) 0.4259(3) 0.4323(2) 0.057 Uani 1 1 d . . . N23 N -0.1783(3) 0.3498(3) 0.3463(2) 0.059 Uani 1 1 d . . . N24 N -0.1918(3) 0.3347(3) 0.4048(3) 0.062 Uani 1 1 d . . . N25 N -0.0411(3) 0.8728(3) 0.2496(3) 0.061 Uani 1 1 d . . . N26 N -0.0490(3) 0.8742(3) 0.3063(3) 0.066 Uani 1 1 d . . . N27 N 0.0342(3) 0.7979(3) 0.2514(2) 0.063 Uani 1 1 d . . . N28 N 0.0400(3) 0.7904(3) 0.3095(3) 0.072 Uani 1 1 d . . . N29 N -0.0647(3) 0.7744(3) 0.2606(2) 0.052 Uani 1 1 d . . . N30 N -0.0691(3) 0.7602(3) 0.3186(2) 0.060 Uani 1 1 d . . . N31 N 0.0118(3) 0.8461(4) 0.4048(3) 0.081 Uani 1 1 d . . . N32 N -0.0013(3) 0.8336(4) 0.4653(3) 0.100 Uani 1 1 d . . . N33 N -0.0045(3) 0.7279(4) 0.4159(3) 0.071 Uani 1 1 d . . . N34 N -0.0107(3) 0.7317(4) 0.4729(3) 0.086 Uani 1 1 d . . . N35 N -0.1008(3) 0.8110(3) 0.4135(2) 0.070 Uani 1 1 d . . . N36 N -0.0946(3) 0.7965(3) 0.4719(3) 0.072 Uani 1 1 d . . . N37 N 0.4951(3) 0.6270(3) 0.2459(3) 0.056 Uani 1 1 d . . . N38 N 0.5002(3) 0.6265(3) 0.1887(2) 0.057 Uani 1 1 d . . . N39 N 0.5529(2) 0.7010(3) 0.2421(2) 0.047 Uani 1 1 d . . . N40 N 0.5724(3) 0.7079(3) 0.1843(2) 0.054 Uani 1 1 d . . . N41 N 0.4530(3) 0.7245(3) 0.2354(2) 0.055 Uani 1 1 d . . . N42 N 0.4585(3) 0.7407(3) 0.1754(2) 0.056 Uani 1 1 d . . . N43 N 0.4601(3) 0.6887(3) 0.0806(2) 0.055 Uani 1 1 d . . . N44 N 0.4758(2) 0.7042(3) 0.0234(2) 0.050 Uani 1 1 d . . . N45 N 0.5779(3) 0.6544(3) 0.0864(2) 0.050 Uani 1 1 d . . . N46 N 0.5739(2) 0.6668(3) 0.0277(2) 0.050 Uani 1 1 d . . . N47 N 0.5370(3) 0.7728(3) 0.0787(2) 0.055 Uani 1 1 d . . . N48 N 0.5473(3) 0.7693(3) 0.0217(2) 0.050 Uani 1 1 d . . . N49 N 0.2129(2) 1.0398(3) 0.3188(3) 0.054 Uani 1 1 d . . . N50 N 0.1960(3) 1.0702(3) 0.2661(3) 0.057 Uani 1 1 d . . . N51 N 0.2580(2) 0.9551(3) 0.2853(2) 0.047 Uani 1 1 d . . . N52 N 0.2473(2) 0.9751(3) 0.2298(2) 0.048 Uani 1 1 d . . . N53 N 0.3141(2) 1.0333(3) 0.2923(2) 0.048 Uani 1 1 d . . . N54 N 0.3135(2) 1.0601(3) 0.2367(2) 0.051 Uani 1 1 d . . . N55 N 0.2448(3) 1.1455(3) 0.1646(3) 0.052 Uani 1 1 d . . . N56 N 0.2428(3) 1.1627(3) 0.1069(3) 0.054 Uani 1 1 d . . . N57 N 0.1767(3) 1.0604(3) 0.1514(2) 0.054 Uani 1 1 d . . . N58 N 0.1793(2) 1.0944(3) 0.0973(2) 0.048 Uani 1 1 d . . . N59 N 0.2959(2) 1.0446(2) 0.1272(2) 0.044 Uani 1 1 d . . . N60 N 0.2793(2) 1.0752(2) 0.0746(2) 0.045 Uani 1 1 d . . . N61 N 0.7079(3) 1.0038(3) 0.3287(3) 0.061 Uani 1 1 d . . . N62 N 0.7325(3) 1.0307(3) 0.2755(3) 0.069 Uani 1 1 d . . . N63 N 0.6093(3) 1.0394(3) 0.3159(3) 0.060 Uani 1 1 d . . . N64 N 0.6223(3) 1.0761(3) 0.2620(3) 0.074 Uani 1 1 d . . . N65 N 0.6484(3) 0.9475(3) 0.2936(3) 0.066 Uani 1 1 d . . . N66 N 0.6596(3) 0.9705(3) 0.2358(3) 0.060 Uani 1 1 d . . . N67 N 0.7122(3) 1.1318(3) 0.1841(3) 0.079 Uani 1 1 d . . . N68 N 0.7264(3) 1.1465(3) 0.1282(3) 0.081 Uani 1 1 d . . . N69 N 0.6367(3) 1.0681(3) 0.1463(3) 0.064 Uani 1 1 d . . . N70 N 0.6608(3) 1.0966(3) 0.0935(3) 0.070 Uani 1 1 d . . . N71 N 0.7515(3) 1.0205(3) 0.1586(3) 0.058 Uani 1 1 d . . . N72 N 0.7572(3) 1.0528(3) 0.1020(3) 0.064 Uani 1 1 d . . . C1 C 0.0733(3) 0.6281(3) 0.0628(3) 0.049 Uani 1 1 d . . . C2 C 0.0271(3) 0.5964(3) 0.0610(3) 0.050 Uani 1 1 d . . . C3 C -0.0308(3) 0.6237(4) 0.0681(3) 0.049 Uani 1 1 d . . . C4 C -0.0413(3) 0.6806(3) 0.0776(3) 0.048 Uani 1 1 d . . . C5 C 0.0054(3) 0.7121(3) 0.0800(3) 0.048 Uani 1 1 d . . . C6 C 0.0636(3) 0.6863(4) 0.0720(3) 0.052 Uani 1 1 d . . . C7 C 0.1354(3) 0.5998(4) 0.0550(3) 0.058 Uani 1 1 d . . . H7A H 0.1385 0.5752 0.0263 0.070 Uiso 1 1 calc R . . H7B H 0.1626 0.6301 0.0422 0.070 Uiso 1 1 calc R . . C8 C 0.2093(3) 0.5448(4) 0.1086(3) 0.053 Uani 1 1 d . . . H8A H 0.2329 0.5782 0.0957 0.063 Uiso 1 1 calc R . . H8B H 0.2197 0.5174 0.0826 0.063 Uiso 1 1 calc R . . C9 C 0.2207(3) 0.5139(3) 0.1697(3) 0.050 Uani 1 1 d . . . C10 C 0.1578(4) 0.4331(4) 0.1609(3) 0.066 Uani 1 1 d . . . H10 H 0.1457 0.4475 0.1241 0.079 Uiso 1 1 calc R . . C11 C 0.1452(4) 0.3818(4) 0.1954(3) 0.070 Uani 1 1 d . . . H11 H 0.1240 0.3531 0.1874 0.084 Uiso 1 1 calc R . . C12 C 0.1704(3) 0.3803(4) 0.2455(3) 0.063 Uani 1 1 d . . . H12 H 0.1670 0.3500 0.2781 0.076 Uiso 1 1 calc R . . C13 C 0.1823(4) 0.6126(4) 0.2006(4) 0.078 Uani 1 1 d . . . H13 H 0.1769 0.6376 0.1650 0.093 Uiso 1 1 calc R . . C14 C 0.1724(4) 0.6281(4) 0.2512(4) 0.077 Uani 1 1 d . . . H14 H 0.1567 0.6649 0.2587 0.092 Uiso 1 1 calc R . . C15 C 0.1901(4) 0.5789(4) 0.2903(3) 0.068 Uani 1 1 d . . . H15 H 0.1902 0.5783 0.3295 0.081 Uiso 1 1 calc R . . C16 C 0.3288(3) 0.5046(3) 0.1300(3) 0.054 Uani 1 1 d . . . H16 H 0.3257 0.5201 0.0909 0.065 Uiso 1 1 calc R . . C17 C 0.3772(3) 0.4841(4) 0.1539(3) 0.063 Uani 1 1 d . . . H17 H 0.4153 0.4819 0.1356 0.075 Uiso 1 1 calc R . . C18 C 0.3600(3) 0.4657(3) 0.2136(3) 0.053 Uani 1 1 d . . . H18 H 0.3859 0.4502 0.2416 0.063 Uiso 1 1 calc R . . C19 C 0.1297(3) 0.4402(4) 0.3680(3) 0.063 Uani 1 1 d . . . C20 C 0.1113(4) 0.4136(5) 0.4255(3) 0.102 Uani 1 1 d . . . H20 H 0.0729 0.4113 0.4428 0.123 Uiso 1 1 calc R . . C21 C 0.1618(4) 0.3923(4) 0.4498(3) 0.067 Uani 1 1 d . . . C22 C 0.0869(4) 0.4708(5) 0.3251(4) 0.092 Uani 1 1 d . . . H22A H 0.1078 0.4817 0.2876 0.138 Uiso 1 1 calc R . . H22B H 0.0673 0.5058 0.3370 0.138 Uiso 1 1 calc R . . H22C H 0.0582 0.4443 0.3234 0.138 Uiso 1 1 calc R . . C23 C 0.1708(4) 0.3593(4) 0.5093(3) 0.084 Uani 1 1 d . . . H23A H 0.1763 0.3868 0.5329 0.126 Uiso 1 1 calc R . . H23B H 0.2052 0.3312 0.5084 0.126 Uiso 1 1 calc R . . H23C H 0.1369 0.3384 0.5253 0.126 Uiso 1 1 calc R . . C24 C 0.3232(3) 0.5292(4) 0.3415(3) 0.059 Uani 1 1 d . . . C25 C 0.3421(4) 0.5251(4) 0.3942(4) 0.069 Uani 1 1 d . . . H25 H 0.3629 0.5525 0.4050 0.083 Uiso 1 1 calc R . . C26 C 0.3255(4) 0.4739(4) 0.4284(4) 0.071 Uani 1 1 d . . . C27 C 0.3300(4) 0.5779(4) 0.2894(4) 0.074 Uani 1 1 d . . . H27A H 0.3598 0.5649 0.2617 0.112 Uiso 1 1 calc R . . H27B H 0.3413 0.6123 0.3004 0.112 Uiso 1 1 calc R . . H27C H 0.2931 0.5879 0.2725 0.112 Uiso 1 1 calc R . . C28 C 0.3345(5) 0.4461(5) 0.4904(4) 0.102 Uani 1 1 d . . . H28A H 0.2974 0.4477 0.5136 0.154 Uiso 1 1 calc R . . H28B H 0.3615 0.4675 0.5040 0.154 Uiso 1 1 calc R . . H28C H 0.3504 0.4054 0.4930 0.154 Uiso 1 1 calc R . . C29 C 0.3119(4) 0.3302(4) 0.2895(3) 0.060 Uani 1 1 d . . . C30 C 0.3343(4) 0.2863(4) 0.3317(3) 0.071 Uani 1 1 d . . . H30 H 0.3549 0.2507 0.3257 0.085 Uiso 1 1 calc R . . C31 C 0.3226(4) 0.3018(4) 0.3821(4) 0.071 Uani 1 1 d . . . C32 C 0.3173(5) 0.3349(4) 0.2261(3) 0.083 Uani 1 1 d . . . H32A H 0.3059 0.2993 0.2176 0.124 Uiso 1 1 calc R . . H32B H 0.3574 0.3400 0.2108 0.124 Uiso 1 1 calc R . . H32C H 0.2919 0.3685 0.2088 0.124 Uiso 1 1 calc R . . C33 C 0.3337(5) 0.2704(4) 0.4421(4) 0.097 Uani 1 1 d . . . H33A H 0.3475 0.2295 0.4423 0.145 Uiso 1 1 calc R . . H33B H 0.2977 0.2724 0.4670 0.145 Uiso 1 1 calc R . . H33C H 0.3629 0.2891 0.4557 0.145 Uiso 1 1 calc R . . C34 C 0.2684(4) 0.3945(4) 0.4099(3) 0.065 Uani 1 1 d . . . H34 H 0.2765 0.3748 0.4493 0.078 Uiso 1 1 calc R . . C35 C 0.0366(4) 0.5342(4) 0.0541(4) 0.070 Uani 1 1 d . . . H35A H 0.0609 0.5318 0.0188 0.105 Uiso 1 1 calc R . . H35B H -0.0008 0.5198 0.0528 0.105 Uiso 1 1 calc R . . H35C H 0.0558 0.5103 0.0861 0.105 Uiso 1 1 calc R . . C36 C -0.0825(3) 0.5883(4) 0.0658(3) 0.060 Uani 1 1 d . . . H36A H -0.1152 0.6147 0.0498 0.073 Uiso 1 1 calc R . . H36B H -0.0706 0.5592 0.0417 0.073 Uiso 1 1 calc R . . C37 C -0.1420(3) 0.5202(4) 0.1245(3) 0.054 Uani 1 1 d . . . H37A H -0.1261 0.4894 0.1034 0.064 Uiso 1 1 calc R . . H37B H -0.1763 0.5415 0.1066 0.064 Uiso 1 1 calc R . . C38 C -0.1592(3) 0.4927(3) 0.1872(3) 0.046 Uani 1 1 d . . . C39 C -0.2277(4) 0.4350(4) 0.1491(3) 0.076 Uani 1 1 d . . . H39 H -0.2214 0.4500 0.1096 0.092 Uiso 1 1 calc R . . C40 C -0.2660(4) 0.3937(4) 0.1758(4) 0.080 Uani 1 1 d . . . H40 H -0.2908 0.3754 0.1583 0.095 Uiso 1 1 calc R . . C41 C -0.2598(3) 0.3854(4) 0.2338(3) 0.071 Uani 1 1 d . . . H41 H -0.2808 0.3600 0.2627 0.085 Uiso 1 1 calc R . . C42 C -0.2010(3) 0.5949(4) 0.2006(3) 0.062 Uani 1 1 d . . . H42 H -0.1935 0.6173 0.1635 0.075 Uiso 1 1 calc R . . C43 C -0.2304(4) 0.6152(4) 0.2477(4) 0.069 Uani 1 1 d . . . H43 H -0.2464 0.6539 0.2490 0.083 Uiso 1 1 calc R . . C44 C -0.2310(4) 0.5666(4) 0.2925(4) 0.067 Uani 1 1 d . . . H44 H -0.2479 0.5674 0.3298 0.081 Uiso 1 1 calc R . . C45 C -0.0503(3) 0.4540(3) 0.1925(3) 0.052 Uani 1 1 d . . . H45 H -0.0344 0.4700 0.1554 0.063 Uiso 1 1 calc R . . C46 C -0.0215(4) 0.4195(4) 0.2348(3) 0.072 Uani 1 1 d . . . H46 H 0.0182 0.4052 0.2321 0.087 Uiso 1 1 calc R . . C47 C -0.0608(3) 0.4089(4) 0.2827(3) 0.058 Uani 1 1 d . . . H47 H -0.0516 0.3868 0.3186 0.070 Uiso 1 1 calc R . . C48 C -0.3270(3) 0.4557(4) 0.3423(3) 0.069 Uani 1 1 d . . . C49 C -0.3643(4) 0.4359(4) 0.3904(4) 0.084 Uani 1 1 d . . . H49 H -0.4052 0.4434 0.3933 0.101 Uiso 1 1 calc R . . C50 C -0.3329(3) 0.4042(4) 0.4326(3) 0.067 Uani 1 1 d . . . C51 C -0.3433(4) 0.4912(5) 0.2877(4) 0.094 Uani 1 1 d . . . H51A H -0.3640 0.5283 0.2938 0.141 Uiso 1 1 calc R . . H51B H -0.3684 0.4701 0.2712 0.141 Uiso 1 1 calc R . . H51C H -0.3084 0.4988 0.2619 0.141 Uiso 1 1 calc R . . C52 C -0.3509(4) 0.3739(5) 0.4930(4) 0.092 Uani 1 1 d . . . H52A H -0.3730 0.4022 0.5134 0.138 Uiso 1 1 calc R . . H52B H -0.3164 0.3572 0.5122 0.138 Uiso 1 1 calc R . . H52C H -0.3749 0.3427 0.4923 0.138 Uiso 1 1 calc R . . C53 C -0.1325(3) 0.4943(4) 0.3900(3) 0.061 Uani 1 1 d . . . C54 C -0.1369(4) 0.4929(4) 0.4492(3) 0.064 Uani 1 1 d . . . H54 H -0.1195 0.5172 0.4675 0.077 Uiso 1 1 calc R . . C55 C -0.1714(3) 0.4492(4) 0.4747(3) 0.056 Uani 1 1 d . . . C56 C -0.0996(4) 0.5374(4) 0.3450(3) 0.067 Uani 1 1 d . . . H56A H -0.0891 0.5211 0.3109 0.101 Uiso 1 1 calc R . . H56B H -0.0644 0.5447 0.3596 0.101 Uiso 1 1 calc R . . H56C H -0.1241 0.5741 0.3356 0.101 Uiso 1 1 calc R . . C57 C -0.1920(4) 0.4285(5) 0.5375(3) 0.088 Uani 1 1 d . . . H57A H -0.2041 0.4624 0.5549 0.132 Uiso 1 1 calc R . . H57B H -0.1603 0.4046 0.5570 0.132 Uiso 1 1 calc R . . H57C H -0.2247 0.4053 0.5408 0.132 Uiso 1 1 calc R . . C58 C -0.1567(4) 0.3011(4) 0.3306(4) 0.068 Uani 1 1 d . . . C59 C -0.1542(4) 0.2557(4) 0.3790(4) 0.085 Uani 1 1 d . . . H59 H -0.1394 0.2165 0.3789 0.102 Uiso 1 1 calc R . . C60 C -0.1763(5) 0.2769(4) 0.4259(4) 0.087 Uani 1 1 d . . . C61 C -0.1354(5) 0.2948(5) 0.2715(4) 0.098 Uani 1 1 d . . . H61A H -0.0977 0.2719 0.2716 0.147 Uiso 1 1 calc R . . H61B H -0.1317 0.3334 0.2475 0.147 Uiso 1 1 calc R . . H61C H -0.1630 0.2749 0.2568 0.147 Uiso 1 1 calc R . . C62 C -0.1839(6) 0.2493(5) 0.4886(5) 0.137 Uani 1 1 d . . . H62A H -0.1802 0.2067 0.4932 0.205 Uiso 1 1 calc R . . H62B H -0.2222 0.2624 0.5048 0.205 Uiso 1 1 calc R . . H62C H -0.1542 0.2608 0.5080 0.205 Uiso 1 1 calc R . . C63 C -0.2220(3) 0.3802(4) 0.4333(3) 0.060 Uani 1 1 d . . . H63 H -0.2321 0.3617 0.4738 0.073 Uiso 1 1 calc R . . C64 C -0.1036(3) 0.7070(4) 0.0869(4) 0.071 Uani 1 1 d . . . H64A H -0.1239 0.7075 0.0537 0.107 Uiso 1 1 calc R . . H64B H -0.1037 0.7469 0.0925 0.107 Uiso 1 1 calc R . . H64C H -0.1232 0.6835 0.1205 0.107 Uiso 1 1 calc R . . C65 C -0.0049(4) 0.7727(4) 0.0916(3) 0.065 Uani 1 1 d . . . H65A H 0.0259 0.7965 0.0707 0.078 Uiso 1 1 calc R . . H65B H -0.0425 0.7915 0.0787 0.078 Uiso 1 1 calc R . . C66 C -0.0212(4) 0.8261(4) 0.1663(3) 0.062 Uani 1 1 d . . . H66A H -0.0596 0.8420 0.1537 0.074 Uiso 1 1 calc R . . H66B H 0.0073 0.8536 0.1473 0.074 Uiso 1 1 calc R . . C67 C -0.0228(3) 0.8181(4) 0.2321(3) 0.054 Uani 1 1 d . . . C68 C -0.0492(3) 0.9294(4) 0.2180(3) 0.064 Uani 1 1 d . . . H68 H -0.0455 0.9402 0.1779 0.076 Uiso 1 1 calc R . . C69 C -0.0633(3) 0.9670(4) 0.2544(4) 0.068 Uani 1 1 d . . . H69 H -0.0706 1.0082 0.2451 0.082 Uiso 1 1 calc R . . C70 C -0.0644(4) 0.9294(4) 0.3114(4) 0.076 Uani 1 1 d . . . H70 H -0.0745 0.9422 0.3460 0.091 Uiso 1 1 calc R . . C71 C 0.0883(3) 0.7905(4) 0.2226(3) 0.065 Uani 1 1 d . . . H71 H 0.0957 0.7939 0.1828 0.078 Uiso 1 1 calc R . . C72 C 0.1284(4) 0.7780(4) 0.2591(4) 0.073 Uani 1 1 d . . . H72 H 0.1689 0.7713 0.2501 0.088 Uiso 1 1 calc R . . C73 C 0.0991(4) 0.7765(4) 0.3143(4) 0.084 Uani 1 1 d . . . H73 H 0.1169 0.7676 0.3486 0.101 Uiso 1 1 calc R . . C74 C -0.1029(4) 0.7483(4) 0.2388(3) 0.079 Uani 1 1 d . . . H74 H -0.1083 0.7530 0.1999 0.094 Uiso 1 1 calc R . . C75 C -0.1328(4) 0.7132(4) 0.2841(3) 0.077 Uani 1 1 d . . . H75 H -0.1617 0.6885 0.2828 0.093 Uiso 1 1 calc R . . C76 C -0.1103(4) 0.7229(4) 0.3318(3) 0.069 Uani 1 1 d . . . H76 H -0.1228 0.7051 0.3695 0.083 Uiso 1 1 calc R . . C77 C 0.0490(5) 0.8853(6) 0.3974(4) 0.115 Uani 1 1 d . . . C78 C 0.0572(5) 0.9022(6) 0.4481(4) 0.124 Uani 1 1 d . . . H78 H 0.0794 0.9322 0.4516 0.149 Uiso 1 1 calc R . . C79 C 0.0262(5) 0.8661(7) 0.4920(4) 0.134 Uani 1 1 d . . . C80 C 0.0732(5) 0.9147(5) 0.3386(4) 0.115 Uani 1 1 d . . . H80A H 0.1143 0.9016 0.3326 0.173 Uiso 1 1 calc R . . H80B H 0.0684 0.9570 0.3353 0.173 Uiso 1 1 calc R . . H80C H 0.0523 0.9043 0.3100 0.173 Uiso 1 1 calc R . . C81 C 0.0174(7) 0.8606(9) 0.5564(4) 0.209 Uani 1 1 d . . . H81A H -0.0236 0.8698 0.5679 0.313 Uiso 1 1 calc R . . H81B H 0.0403 0.8877 0.5675 0.313 Uiso 1 1 calc R . . H81C H 0.0297 0.8206 0.5749 0.313 Uiso 1 1 calc R . . C82 C 0.0226(4) 0.6748(5) 0.4130(4) 0.082 Uani 1 1 d . . . C83 C 0.0368(4) 0.6432(5) 0.4674(4) 0.089 Uani 1 1 d . . . H83 H 0.0555 0.6049 0.4765 0.107 Uiso 1 1 calc R . . C84 C 0.0180(4) 0.6798(5) 0.5034(4) 0.088 Uani 1 1 d . . . C85 C 0.0352(4) 0.6529(5) 0.3585(4) 0.087 Uani 1 1 d . . . H85A H 0.0574 0.6146 0.3656 0.131 Uiso 1 1 calc R . . H85B H 0.0577 0.6803 0.3307 0.131 Uiso 1 1 calc R . . H85C H -0.0013 0.6496 0.3438 0.131 Uiso 1 1 calc R . . C86 C 0.0233(5) 0.6701(5) 0.5679(4) 0.117 Uani 1 1 d . . . H86A H -0.0151 0.6660 0.5886 0.176 Uiso 1 1 calc R . . H86B H 0.0393 0.7036 0.5761 0.176 Uiso 1 1 calc R . . H86C H 0.0489 0.6347 0.5798 0.176 Uiso 1 1 calc R . . C87 C -0.1587(4) 0.8224(4) 0.4109(4) 0.078 Uani 1 1 d . . . C88 C -0.1872(4) 0.8171(5) 0.4639(4) 0.089 Uani 1 1 d . . . H88 H -0.2279 0.8234 0.4721 0.107 Uiso 1 1 calc R . . C89 C -0.1476(5) 0.8013(5) 0.5034(4) 0.097 Uani 1 1 d . . . C90 C -0.1859(4) 0.8411(4) 0.3570(4) 0.088 Uani 1 1 d . . . H90A H -0.1571 0.8361 0.3253 0.133 Uiso 1 1 calc R . . H90B H -0.2009 0.8822 0.3525 0.133 Uiso 1 1 calc R . . H90C H -0.2177 0.8174 0.3576 0.133 Uiso 1 1 calc R . . C91 C -0.1525(5) 0.7872(7) 0.5704(4) 0.150 Uani 1 1 d . . . H91A H -0.1199 0.7595 0.5835 0.225 Uiso 1 1 calc R . . H91B H -0.1889 0.7702 0.5851 0.225 Uiso 1 1 calc R . . H91C H -0.1517 0.8232 0.5842 0.225 Uiso 1 1 calc R . . C92 C -0.0379(4) 0.7865(4) 0.4899(3) 0.073 Uani 1 1 d . . . H92 H -0.0408 0.7808 0.5321 0.088 Uiso 1 1 calc R . . C93 C 0.1150(4) 0.7222(5) 0.0742(4) 0.094 Uani 1 1 d . . . H93A H 0.1419 0.6988 0.1001 0.141 Uiso 1 1 calc R . . H93B H 0.1001 0.7579 0.0876 0.141 Uiso 1 1 calc R . . H93C H 0.1352 0.7323 0.0363 0.141 Uiso 1 1 calc R . . C94 C 0.4650(4) 0.7851(4) 0.4175(3) 0.062 Uani 1 1 d . . . C95 C 0.4093(3) 0.8172(3) 0.4198(3) 0.051 Uani 1 1 d . . . C96 C 0.4025(3) 0.8725(3) 0.4340(3) 0.052 Uani 1 1 d . . . C97 C 0.4521(3) 0.8981(3) 0.4427(3) 0.052 Uani 1 1 d . . . C98 C 0.5076(3) 0.8671(4) 0.4395(3) 0.060 Uani 1 1 d . . . C99 C 0.5143(3) 0.8113(4) 0.4274(3) 0.059 Uani 1 1 d . . . C100 C 0.4733(5) 0.7230(4) 0.4050(3) 0.081 Uani 1 1 d . . . H10A H 0.5066 0.7001 0.4235 0.098 Uiso 1 1 calc R . . H10B H 0.4382 0.7025 0.4194 0.098 Uiso 1 1 calc R . . C101 C 0.4851(4) 0.6752(3) 0.3265(3) 0.058 Uani 1 1 d . . . H10C H 0.4476 0.6587 0.3393 0.070 Uiso 1 1 calc R . . H10D H 0.5158 0.6476 0.3449 0.070 Uiso 1 1 calc R . . C102 C 0.4963(3) 0.6820(3) 0.2634(3) 0.050 Uani 1 1 d . . . C103 C 0.4907(3) 0.5697(4) 0.2770(3) 0.062 Uani 1 1 d . . . H103 H 0.4864 0.5581 0.3171 0.074 Uiso 1 1 calc R . . C104 C 0.4937(3) 0.5341(4) 0.2399(4) 0.069 Uani 1 1 d . . . H104 H 0.4936 0.4930 0.2492 0.083 Uiso 1 1 calc R . . C105 C 0.4970(3) 0.5689(3) 0.1849(4) 0.057 Uani 1 1 d . . . H105 H 0.4970 0.5553 0.1508 0.069 Uiso 1 1 calc R . . C106 C 0.5976(4) 0.7102(3) 0.2723(4) 0.063 Uani 1 1 d . . . H106 H 0.5956 0.7082 0.3120 0.076 Uiso 1 1 calc R . . C107 C 0.6464(3) 0.7232(4) 0.2325(3) 0.061 Uani 1 1 d . . . H107 H 0.6832 0.7314 0.2396 0.073 Uiso 1 1 calc R . . C108 C 0.6270(3) 0.7209(3) 0.1788(3) 0.053 Uani 1 1 d . . . H108 H 0.6503 0.7279 0.1438 0.063 Uiso 1 1 calc R . . C109 C 0.4014(4) 0.7524(4) 0.2566(3) 0.071 Uani 1 1 d . . . H109 H 0.3868 0.7480 0.2953 0.085 Uiso 1 1 calc R . . C110 C 0.3759(4) 0.7868(4) 0.2120(4) 0.086 Uani 1 1 d . . . H110 H 0.3408 0.8113 0.2136 0.104 Uiso 1 1 calc R . . C111 C 0.4124(4) 0.7789(4) 0.1626(4) 0.066 Uani 1 1 d . . . H111 H 0.4050 0.7981 0.1252 0.079 Uiso 1 1 calc R . . C112 C 0.4043(3) 0.6780(4) 0.0858(3) 0.061 Uani 1 1 d . . . C113 C 0.3839(3) 0.6890(4) 0.0311(4) 0.075 Uani 1 1 d . . . H113 H 0.3459 0.6855 0.0229 0.090 Uiso 1 1 calc R . . C114 C 0.4316(3) 0.7062(4) -0.0090(3) 0.062 Uani 1 1 d . . . C115 C 0.3669(4) 0.6607(4) 0.1405(4) 0.082 Uani 1 1 d . . . H11A H 0.3564 0.6211 0.1439 0.123 Uiso 1 1 calc R . . H11B H 0.3317 0.6878 0.1406 0.123 Uiso 1 1 calc R . . H11C H 0.3882 0.6622 0.1725 0.123 Uiso 1 1 calc R . . C116 C 0.4348(4) 0.7229(6) -0.0719(4) 0.106 Uani 1 1 d . . . H11D H 0.4515 0.7603 -0.0846 0.159 Uiso 1 1 calc R . . H11E H 0.3959 0.7267 -0.0842 0.159 Uiso 1 1 calc R . . H11F H 0.4592 0.6929 -0.0884 0.159 Uiso 1 1 calc R . . C117 C 0.6197(3) 0.6092(3) 0.0943(3) 0.056 Uani 1 1 d . . . C118 C 0.6435(4) 0.5947(4) 0.0422(4) 0.069 Uani 1 1 d . . . H118 H 0.6735 0.5650 0.0370 0.082 Uiso 1 1 calc R . . C119 C 0.6145(4) 0.6323(4) 0.0004(3) 0.067 Uani 1 1 d . . . C120 C 0.6393(4) 0.5814(4) 0.1512(3) 0.079 Uani 1 1 d . . . H12A H 0.6811 0.5824 0.1501 0.119 Uiso 1 1 calc R . . H12B H 0.6299 0.5409 0.1612 0.119 Uiso 1 1 calc R . . H12C H 0.6196 0.6028 0.1796 0.119 Uiso 1 1 calc R . . C121 C 0.6196(4) 0.6379(4) -0.0633(3) 0.072 Uani 1 1 d . . . H12D H 0.5854 0.6244 -0.0742 0.107 Uiso 1 1 calc R . . H12E H 0.6543 0.6142 -0.0750 0.107 Uiso 1 1 calc R . . H12F H 0.6225 0.6788 -0.0818 0.107 Uiso 1 1 calc R . . C122 C 0.5515(4) 0.8241(4) 0.0826(3) 0.060 Uani 1 1 d . . . C123 C 0.5693(3) 0.8550(3) 0.0262(3) 0.056 Uani 1 1 d . . . H123 H 0.5799 0.8938 0.0164 0.067 Uiso 1 1 calc R . . C124 C 0.5683(3) 0.8194(3) -0.0097(3) 0.052 Uani 1 1 d . . . C125 C 0.5455(4) 0.8472(4) 0.1356(3) 0.074 Uani 1 1 d . . . H12G H 0.5068 0.8420 0.1550 0.111 Uiso 1 1 calc R . . H12H H 0.5514 0.8887 0.1264 0.111 Uiso 1 1 calc R . . H12I H 0.5745 0.8260 0.1604 0.111 Uiso 1 1 calc R . . C126 C 0.5835(4) 0.8307(4) -0.0738(3) 0.075 Uani 1 1 d . . . H12J H 0.5493 0.8283 -0.0925 0.112 Uiso 1 1 calc R . . H12K H 0.6143 0.8016 -0.0833 0.112 Uiso 1 1 calc R . . H12L H 0.5967 0.8697 -0.0867 0.112 Uiso 1 1 calc R . . C127 C 0.5359(3) 0.7167(3) 0.0044(3) 0.047 Uani 1 1 d . . . H127 H 0.5415 0.7231 -0.0379 0.057 Uiso 1 1 calc R . . C128 C 0.3569(4) 0.7914(4) 0.4089(4) 0.079 Uani 1 1 d . . . H12M H 0.3220 0.8116 0.4249 0.119 Uiso 1 1 calc R . . H12N H 0.3592 0.7499 0.4266 0.119 Uiso 1 1 calc R . . H12O H 0.3556 0.7959 0.3680 0.119 Uiso 1 1 calc R . . C129 C 0.3435(3) 0.9077(4) 0.4365(3) 0.060 Uani 1 1 d . . . H12P H 0.3140 0.8822 0.4573 0.072 Uiso 1 1 calc R . . H12Q H 0.3448 0.9394 0.4571 0.072 Uiso 1 1 calc R . . C130 C 0.2758(3) 0.9711(4) 0.3816(3) 0.053 Uani 1 1 d . . . H13A H 0.2802 1.0012 0.4033 0.064 Uiso 1 1 calc R . . H13B H 0.2428 0.9493 0.4002 0.064 Uiso 1 1 calc R . . C131 C 0.2651(3) 1.0001(3) 0.3199(3) 0.044 Uani 1 1 d . . . C132 C 0.1726(3) 1.0540(4) 0.3611(3) 0.068 Uani 1 1 d . . . H132 H 0.1736 1.0389 0.4006 0.081 Uiso 1 1 calc R . . C133 C 0.1315(4) 1.0931(4) 0.3368(4) 0.082 Uani 1 1 d . . . H133 H 0.0988 1.1112 0.3556 0.099 Uiso 1 1 calc R . . C134 C 0.1466(4) 1.1017(4) 0.2782(4) 0.068 Uani 1 1 d . . . H134 H 0.1245 1.1268 0.2507 0.082 Uiso 1 1 calc R . . C135 C 0.2542(3) 0.8981(3) 0.3012(3) 0.052 Uani 1 1 d . . . H135 H 0.2589 0.8750 0.3378 0.062 Uiso 1 1 calc R . . C136 C 0.2424(3) 0.8791(4) 0.2559(4) 0.064 Uani 1 1 d . . . H136 H 0.2373 0.8400 0.2549 0.077 Uiso 1 1 calc R . . C137 C 0.2391(3) 0.9270(3) 0.2100(3) 0.054 Uani 1 1 d . . . H137 H 0.2323 0.9261 0.1724 0.065 Uiso 1 1 calc R . . C138 C 0.3605(3) 1.0448(4) 0.3159(3) 0.062 Uani 1 1 d . . . H138 H 0.3699 1.0307 0.3537 0.075 Uiso 1 1 calc R . . C139 C 0.3912(3) 1.0816(4) 0.2730(3) 0.067 Uani 1 1 d . . . H139 H 0.4261 1.0972 0.2757 0.081 Uiso 1 1 calc R . . C140 C 0.3610(3) 1.0908(4) 0.2258(3) 0.066 Uani 1 1 d . . . H140 H 0.3718 1.1152 0.1905 0.079 Uiso 1 1 calc R . . C141 C 0.2492(4) 1.1929(4) 0.1834(4) 0.067 Uani 1 1 d . . . C142 C 0.2502(4) 1.2435(4) 0.1369(4) 0.071 Uani 1 1 d . . . H142 H 0.2530 1.2827 0.1391 0.085 Uiso 1 1 calc R . . C143 C 0.2463(4) 1.2222(3) 0.0890(3) 0.062 Uani 1 1 d . . . C144 C 0.2536(4) 1.1958(4) 0.2450(3) 0.078 Uani 1 1 d . . . H14A H 0.2463 1.1581 0.2694 0.117 Uiso 1 1 calc R . . H14B H 0.2248 1.2261 0.2559 0.117 Uiso 1 1 calc R . . H14C H 0.2924 1.2051 0.2491 0.117 Uiso 1 1 calc R . . C145 C 0.2508(5) 1.2537(4) 0.0268(4) 0.093 Uani 1 1 d . . . H14D H 0.2808 1.2326 0.0052 0.139 Uiso 1 1 calc R . . H14E H 0.2609 1.2934 0.0240 0.139 Uiso 1 1 calc R . . H14F H 0.2136 1.2552 0.0115 0.139 Uiso 1 1 calc R . . C146 C 0.1247(3) 1.0382(4) 0.1601(3) 0.061 Uani 1 1 d . . . C147 C 0.0938(4) 1.0581(4) 0.1109(4) 0.077 Uani 1 1 d . . . H147 H 0.0568 1.0485 0.1057 0.093 Uiso 1 1 calc R . . C148 C 0.1289(3) 1.0942(4) 0.0724(3) 0.059 Uani 1 1 d . . . C149 C 0.1055(4) 0.9976(4) 0.2139(4) 0.088 Uani 1 1 d . . . H14G H 0.0911 0.9637 0.2048 0.133 Uiso 1 1 calc R . . H14H H 0.0745 1.0179 0.2353 0.133 Uiso 1 1 calc R . . H14I H 0.1382 0.9848 0.2367 0.133 Uiso 1 1 calc R . . C150 C 0.1195(4) 1.1296(4) 0.0145(4) 0.083 Uani 1 1 d . . . H15A H 0.0837 1.1203 0.0027 0.124 Uiso 1 1 calc R . . H15B H 0.1521 1.1204 -0.0124 0.124 Uiso 1 1 calc R . . H15C H 0.1166 1.1711 0.0154 0.124 Uiso 1 1 calc R . . C151 C 0.3400(3) 1.0062(3) 0.1149(3) 0.055 Uani 1 1 d . . . C152 C 0.3481(3) 1.0096(3) 0.0544(3) 0.056 Uani 1 1 d . . . H152 H 0.3755 0.9861 0.0349 0.067 Uiso 1 1 calc R . . C153 C 0.3092(3) 1.0527(3) 0.0306(3) 0.051 Uani 1 1 d . . . C154 C 0.3732(4) 0.9650(4) 0.1588(3) 0.074 Uani 1 1 d . . . H15D H 0.3669 0.9790 0.1944 0.111 Uiso 1 1 calc R . . H15E H 0.4145 0.9632 0.1458 0.111 Uiso 1 1 calc R . . H15F H 0.3599 0.9262 0.1648 0.111 Uiso 1 1 calc R . . C155 C 0.2997(4) 1.0769(4) -0.0300(3) 0.069 Uani 1 1 d . . . H15G H 0.2609 1.0700 -0.0368 0.104 Uiso 1 1 calc R . . H15H H 0.3286 1.0577 -0.0544 0.104 Uiso 1 1 calc R . . H15I H 0.3034 1.1189 -0.0386 0.104 Uiso 1 1 calc R . . C156 C 0.2320(3) 1.1209(3) 0.0739(3) 0.045 Uani 1 1 d . . . H156 H 0.2278 1.1416 0.0339 0.054 Uiso 1 1 calc R . . C157 C 0.4468(4) 0.9594(4) 0.4552(4) 0.082 Uani 1 1 d . . . H15J H 0.4302 0.9873 0.4238 0.124 Uiso 1 1 calc R . . H15K H 0.4852 0.9697 0.4595 0.124 Uiso 1 1 calc R . . H15L H 0.4216 0.9605 0.4902 0.124 Uiso 1 1 calc R . . C158 C 0.5616(3) 0.8961(4) 0.4487(3) 0.074 Uani 1 1 d . . . H15M H 0.5523 0.9182 0.4795 0.089 Uiso 1 1 calc R . . H15N H 0.5943 0.8664 0.4584 0.089 Uiso 1 1 calc R . . C159 C 0.6332(4) 0.9542(4) 0.3944(3) 0.073 Uani 1 1 d . . . H15O H 0.6618 0.9204 0.4052 0.088 Uiso 1 1 calc R . . H15P H 0.6325 0.9808 0.4211 0.088 Uiso 1 1 calc R . . C160 C 0.6481(3) 0.9861(4) 0.3331(3) 0.058 Uani 1 1 d . . . C161 C 0.7454(4) 0.9995(4) 0.3702(4) 0.075 Uani 1 1 d . . . H161 H 0.7391 0.9831 0.4095 0.090 Uiso 1 1 calc R . . C162 C 0.7969(4) 1.0259(5) 0.3395(4) 0.087 Uani 1 1 d . . . H162 H 0.8307 1.0315 0.3550 0.105 Uiso 1 1 calc R . . C163 C 0.7860(4) 1.0408(4) 0.2839(4) 0.078 Uani 1 1 d . . . H163 H 0.8134 1.0566 0.2542 0.093 Uiso 1 1 calc R . . C164 C 0.5637(4) 1.0648(4) 0.3448(4) 0.079 Uani 1 1 d . . . H164 H 0.5477 1.0499 0.3821 0.095 Uiso 1 1 calc R . . C165 C 0.5443(4) 1.1179(5) 0.3090(4) 0.095 Uani 1 1 d . . . H165 H 0.5130 1.1456 0.3165 0.114 Uiso 1 1 calc R . . C166 C 0.5827(4) 1.1195(4) 0.2595(4) 0.085 Uani 1 1 d . . . H166 H 0.5797 1.1500 0.2271 0.102 Uiso 1 1 calc R . . C167 C 0.6396(4) 0.8893(4) 0.3008(4) 0.073 Uani 1 1 d . . . H167 H 0.6316 0.8638 0.3362 0.087 Uiso 1 1 calc R . . C168 C 0.6441(4) 0.8745(4) 0.2497(4) 0.080 Uani 1 1 d . . . H168 H 0.6395 0.8374 0.2425 0.096 Uiso 1 1 calc R . . C169 C 0.6570(3) 0.9245(4) 0.2094(4) 0.071 Uani 1 1 d . . . H169 H 0.6631 0.9266 0.1698 0.085 Uiso 1 1 calc R . . C170 C 0.7215(5) 1.1751(5) 0.2062(5) 0.098 Uani 1 1 d . . . C171 C 0.7427(6) 1.2179(5) 0.1638(5) 0.113 Uani 1 1 d . . . H171 H 0.7524 1.2543 0.1690 0.135 Uiso 1 1 calc R . . C172 C 0.7480(5) 1.2010(4) 0.1130(5) 0.100 Uani 1 1 d . . . C173 C 0.7084(6) 1.1751(5) 0.2710(5) 0.120 Uani 1 1 d . . . H17A H 0.6813 1.1461 0.2881 0.180 Uiso 1 1 calc R . . H17B H 0.6913 1.2138 0.2761 0.180 Uiso 1 1 calc R . . H17C H 0.7445 1.1652 0.2893 0.180 Uiso 1 1 calc R . . C174 C 0.7680(6) 1.2318(5) 0.0534(5) 0.125 Uani 1 1 d . . . H17D H 0.7349 1.2421 0.0308 0.188 Uiso 1 1 calc R . . H17E H 0.7969 1.2058 0.0359 0.188 Uiso 1 1 calc R . . H17F H 0.7851 1.2672 0.0552 0.188 Uiso 1 1 calc R . . C175 C 0.5820(4) 1.0605(4) 0.1373(4) 0.083 Uani 1 1 d . . . C176 C 0.5724(4) 1.0872(5) 0.0790(4) 0.094 Uani 1 1 d . . . H176 H 0.5373 1.0895 0.0623 0.113 Uiso 1 1 calc R . . C177 C 0.6232(4) 1.1086(5) 0.0521(4) 0.087 Uani 1 1 d . . . C178 C 0.5346(4) 1.0348(5) 0.1809(4) 0.095 Uani 1 1 d . . . H17G H 0.5493 1.0234 0.2183 0.143 Uiso 1 1 calc R . . H17H H 0.5228 1.0005 0.1702 0.143 Uiso 1 1 calc R . . H17I H 0.5013 1.0640 0.1823 0.143 Uiso 1 1 calc R . . C179 C 0.6396(5) 1.1406(5) -0.0094(4) 0.107 Uani 1 1 d . . . H17J H 0.6670 1.1690 -0.0093 0.161 Uiso 1 1 calc R . . H17K H 0.6048 1.1610 -0.0260 0.161 Uiso 1 1 calc R . . H17L H 0.6575 1.1122 -0.0319 0.161 Uiso 1 1 calc R . . C180 C 0.7876(4) 0.9749(4) 0.1591(4) 0.063 Uani 1 1 d . . . C181 C 0.8206(4) 0.9766(4) 0.1048(4) 0.069 Uani 1 1 d . . . H181 H 0.8506 0.9488 0.0947 0.083 Uiso 1 1 calc R . . C182 C 0.7998(4) 1.0257(4) 0.0717(4) 0.072 Uani 1 1 d . . . C183 C 0.7978(4) 0.9268(4) 0.2108(4) 0.075 Uani 1 1 d . . . H18A H 0.8322 0.9332 0.2274 0.112 Uiso 1 1 calc R . . H18B H 0.8037 0.8890 0.1996 0.112 Uiso 1 1 calc R . . H18C H 0.7642 0.9274 0.2389 0.112 Uiso 1 1 calc R . . C184 C 0.8129(5) 1.0506(5) 0.0099(4) 0.117 Uani 1 1 d . . . H18D H 0.8408 1.0795 0.0052 0.176 Uiso 1 1 calc R . . H18E H 0.7772 1.0692 -0.0061 0.176 Uiso 1 1 calc R . . H18F H 0.8293 1.0192 -0.0096 0.176 Uiso 1 1 calc R . . C185 C 0.7201(4) 1.1083(4) 0.0892(4) 0.069 Uani 1 1 d . . . H185 H 0.7315 1.1287 0.0496 0.082 Uiso 1 1 calc R . . C186 C 0.5766(4) 0.7786(4) 0.4214(4) 0.088 Uani 1 1 d . . . H18G H 0.6056 0.8057 0.4204 0.132 Uiso 1 1 calc R . . H18H H 0.5821 0.7637 0.3863 0.132 Uiso 1 1 calc R . . H18I H 0.5810 0.7461 0.4538 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 B1D 0.112 0.205 0.025 -0.004 0.014 -0.002 F1D 0.247 0.169 0.258 0.039 0.122 0.019 F2D 0.259 0.178 0.217 -0.060 0.107 -0.074 F3D 0.188 0.172 0.178 0.062 -0.004 -0.050 F4D 0.348 0.259 0.302 -0.050 -0.182 0.079 B1B 0.108 0.042 0.183 -0.031 0.033 -0.059 F1B 0.050 0.091 0.075 0.009 -0.002 -0.002 F2B 0.042 0.073 0.074 0.013 0.014 -0.015 F3B 0.051 0.082 0.127 -0.005 0.011 -0.015 F4B 0.069 0.138 0.082 0.014 0.019 0.024 B1E 0.104 0.117 0.066 -0.011 0.041 0.008 F1E 0.182 0.249 0.069 -0.055 -0.027 0.061 F2E 0.146 0.235 0.125 0.068 -0.017 0.004 F3E 0.246 0.245 0.166 0.008 -0.075 -0.123 F4E 0.184 0.267 0.125 -0.069 -0.031 0.083 B1F 0.066 0.083 0.056 -0.008 -0.017 -0.001 F1F 0.109 0.119 0.128 -0.018 0.007 -0.014 F2F 0.143 0.137 0.072 -0.001 0.026 0.068 F3F 0.094 0.144 0.140 0.073 0.039 0.005 F4F 0.107 0.187 0.077 -0.034 -0.029 0.049 B1G 0.075 0.326 0.053 0.024 0.002 -0.094 F1G 0.127 0.353 0.157 -0.074 0.008 -0.100 F2G 0.217 0.329 0.294 0.086 0.097 0.056 F3G 0.263 0.245 0.093 -0.051 0.042 -0.127 F4G 0.295 0.200 0.119 0.054 0.023 -0.043 B1H 0.054 0.120 0.046 -0.019 -0.005 -0.003 F1H 0.116 0.343 0.077 -0.016 0.005 -0.110 F2H 0.062 0.217 0.060 -0.034 -0.009 -0.017 F3H 0.082 0.109 0.060 -0.010 -0.012 0.014 F4H 0.175 0.138 0.140 -0.071 -0.079 0.061 B1I 0.253 0.120 0.085 -0.040 -0.083 -0.027 F1I 0.102 0.133 0.134 -0.046 -0.041 0.021 F2I 0.159 0.299 0.109 -0.051 -0.069 0.064 F3I 0.243 0.325 0.166 -0.090 0.047 -0.088 F4I 0.222 0.181 0.279 -0.110 -0.073 0.001 Fe1 0.038 0.076 0.029 0.006 0.001 -0.012 Fe2 0.041 0.071 0.029 0.006 0.000 -0.010 Fe3 0.054 0.096 0.032 0.005 0.003 -0.023 Fe4 0.043 0.056 0.033 0.002 0.002 -0.005 Fe5 0.037 0.053 0.037 0.004 -0.002 -0.009 Fe6 0.053 0.068 0.056 0.004 -0.002 -0.014 O1 0.038 0.099 0.034 0.018 0.002 -0.007 O2 0.065 0.082 0.023 0.011 -0.008 -0.023 O3 0.069 0.069 0.030 0.002 0.005 -0.011 O4 0.084 0.062 0.025 0.008 0.012 -0.011 O5 0.040 0.071 0.035 0.006 0.004 -0.002 O6 0.053 0.098 0.056 0.013 -0.003 -0.028 N1 0.032 0.080 0.032 0.006 0.004 -0.014 N2 0.036 0.094 0.035 0.015 -0.001 -0.013 N3 0.036 0.085 0.041 0.007 -0.003 -0.002 N4 0.039 0.101 0.023 -0.006 0.003 -0.008 N5 0.033 0.064 0.031 0.006 0.000 -0.008 N6 0.029 0.072 0.039 -0.002 -0.001 -0.006 N7 0.049 0.097 0.025 0.005 -0.008 -0.010 N8 0.041 0.085 0.030 0.005 0.002 -0.012 N9 0.033 0.076 0.037 0.000 -0.005 -0.002 N10 0.055 0.067 0.027 0.003 -0.007 -0.013 N11 0.048 0.090 0.027 0.002 -0.012 -0.008 N12 0.070 0.067 0.025 0.006 -0.003 -0.009 N13 0.047 0.085 0.037 0.013 -0.008 -0.022 N14 0.051 0.088 0.047 -0.013 0.014 -0.026 N15 0.039 0.067 0.033 0.005 -0.006 -0.004 N16 0.042 0.082 0.030 0.003 -0.001 -0.011 N17 0.029 0.070 0.036 0.008 -0.006 -0.001 N18 0.054 0.075 0.025 0.018 -0.010 -0.007 N19 0.053 0.083 0.027 0.017 -0.007 -0.016 N20 0.036 0.081 0.040 0.013 -0.009 -0.012 N21 0.046 0.070 0.031 0.017 0.002 -0.007 N22 0.058 0.079 0.022 0.006 0.005 -0.001 N23 0.043 0.089 0.037 0.005 0.004 -0.017 N24 0.062 0.070 0.046 0.006 0.004 -0.017 N25 0.057 0.083 0.041 -0.001 0.003 -0.026 N26 0.073 0.084 0.043 -0.016 0.012 -0.032 N27 0.056 0.096 0.031 0.006 -0.003 -0.020 N28 0.065 0.101 0.037 0.011 -0.002 -0.010 N29 0.054 0.065 0.033 0.006 -0.007 -0.010 N30 0.062 0.081 0.031 0.012 -0.004 -0.019 N31 0.046 0.141 0.044 0.012 0.006 -0.026 N32 0.085 0.187 0.034 -0.013 0.015 -0.074 N33 0.048 0.120 0.037 0.009 -0.004 -0.021 N34 0.064 0.162 0.026 0.009 -0.005 -0.036 N35 0.070 0.111 0.027 0.008 -0.002 -0.040 N36 0.041 0.128 0.042 -0.002 0.005 -0.027 N37 0.060 0.055 0.043 0.008 0.001 0.001 N38 0.062 0.071 0.034 -0.004 -0.003 -0.001 N39 0.048 0.053 0.037 0.000 -0.002 -0.010 N40 0.059 0.069 0.028 0.002 0.003 -0.014 N41 0.046 0.073 0.039 0.001 -0.011 0.006 N42 0.072 0.060 0.031 0.001 -0.002 -0.009 N43 0.055 0.063 0.043 -0.006 0.011 -0.016 N44 0.041 0.069 0.038 -0.003 -0.001 -0.007 N45 0.044 0.068 0.031 0.008 -0.007 -0.004 N46 0.040 0.070 0.033 -0.006 0.000 0.004 N47 0.066 0.060 0.036 -0.003 -0.001 -0.006 N48 0.053 0.067 0.024 0.004 0.000 -0.014 N49 0.036 0.071 0.051 -0.007 0.001 -0.006 N50 0.042 0.066 0.062 -0.008 -0.010 -0.002 N51 0.026 0.067 0.041 0.005 -0.001 -0.011 N52 0.037 0.062 0.038 0.003 0.003 -0.010 N53 0.034 0.059 0.045 -0.001 0.005 -0.010 N54 0.042 0.061 0.044 0.005 0.000 -0.017 N55 0.062 0.047 0.046 -0.006 -0.008 -0.002 N56 0.052 0.057 0.049 0.002 -0.008 -0.009 N57 0.045 0.067 0.045 0.011 -0.004 -0.021 N58 0.040 0.064 0.040 -0.001 -0.006 -0.018 N59 0.031 0.053 0.036 0.019 -0.011 0.001 N60 0.037 0.049 0.042 0.008 -0.005 -0.005 N61 0.044 0.079 0.058 -0.001 -0.015 -0.013 N62 0.055 0.078 0.075 -0.013 -0.001 -0.026 N63 0.039 0.074 0.059 0.003 -0.003 -0.003 N64 0.073 0.051 0.087 0.006 -0.004 -0.004 N65 0.063 0.088 0.041 0.005 -0.005 -0.021 N66 0.054 0.083 0.039 0.002 -0.009 -0.014 N67 0.084 0.073 0.078 -0.014 0.003 -0.018 N68 0.086 0.072 0.074 0.009 0.019 -0.029 N69 0.047 0.079 0.056 0.014 0.001 -0.024 N70 0.066 0.070 0.062 0.016 0.001 -0.012 N71 0.053 0.049 0.064 0.007 -0.003 -0.008 N72 0.039 0.069 0.069 0.016 0.001 -0.004 C1 0.034 0.075 0.028 0.007 0.000 -0.003 C2 0.047 0.077 0.023 -0.006 -0.010 0.003 C3 0.039 0.077 0.026 0.001 0.003 -0.007 C4 0.046 0.063 0.028 0.001 0.001 0.005 C5 0.049 0.065 0.022 0.013 -0.006 -0.007 C6 0.047 0.075 0.030 0.007 -0.010 -0.011 C7 0.042 0.092 0.029 0.006 0.006 -0.009 C8 0.027 0.086 0.034 0.008 0.002 0.000 C9 0.036 0.079 0.030 -0.002 0.010 -0.019 C10 0.064 0.102 0.034 -0.016 -0.008 -0.007 C11 0.061 0.111 0.038 -0.002 -0.005 -0.028 C12 0.038 0.096 0.045 0.014 -0.002 -0.021 C13 0.080 0.090 0.051 0.002 -0.009 0.016 C14 0.079 0.086 0.054 -0.005 0.003 0.013 C15 0.068 0.084 0.042 -0.007 0.000 0.013 C16 0.041 0.077 0.033 0.007 0.018 -0.008 C17 0.031 0.089 0.060 -0.004 0.015 -0.011 C18 0.035 0.068 0.046 0.005 0.005 -0.007 C19 0.034 0.110 0.035 0.012 -0.003 -0.014 C20 0.085 0.187 0.028 0.022 -0.002 -0.070 C21 0.062 0.108 0.028 0.005 0.006 -0.044 C22 0.060 0.149 0.057 0.010 0.007 -0.044 C23 0.076 0.125 0.037 0.015 0.010 -0.021 C24 0.048 0.067 0.058 -0.008 0.012 -0.013 C25 0.063 0.090 0.058 -0.014 -0.004 -0.027 C26 0.066 0.100 0.051 -0.012 -0.009 -0.024 C27 0.048 0.081 0.088 -0.004 0.010 -0.021 C28 0.129 0.129 0.053 -0.006 -0.040 -0.016 C29 0.066 0.068 0.047 -0.013 0.008 -0.024 C30 0.098 0.066 0.044 -0.007 -0.005 0.001 C31 0.092 0.059 0.051 0.015 -0.018 -0.004 C32 0.114 0.098 0.041 -0.016 -0.006 -0.031 C33 0.141 0.077 0.058 0.013 -0.032 0.018 C34 0.076 0.083 0.032 0.004 0.001 -0.025 C35 0.072 0.072 0.062 -0.014 0.003 0.000 C36 0.063 0.084 0.031 0.002 0.006 -0.029 C37 0.045 0.085 0.026 0.006 -0.007 -0.016 C38 0.042 0.061 0.033 0.004 -0.011 -0.010 C39 0.094 0.117 0.029 -0.018 -0.008 -0.043 C40 0.057 0.116 0.077 -0.024 -0.010 -0.043 C41 0.056 0.107 0.052 -0.005 0.001 -0.046 C42 0.056 0.067 0.051 0.018 -0.009 0.001 C43 0.056 0.070 0.069 0.002 -0.003 0.006 C44 0.062 0.081 0.052 -0.010 0.010 0.004 C45 0.030 0.092 0.025 0.009 0.003 -0.007 C46 0.042 0.109 0.050 0.002 0.012 0.007 C47 0.041 0.081 0.046 0.006 -0.009 -0.006 C48 0.037 0.105 0.049 0.016 0.002 -0.012 C49 0.054 0.118 0.060 0.025 0.014 -0.021 C50 0.041 0.103 0.044 0.016 0.007 -0.021 C51 0.039 0.164 0.058 0.021 -0.003 -0.007 C52 0.078 0.125 0.053 0.020 0.018 -0.021 C53 0.049 0.087 0.038 0.014 -0.002 -0.024 C54 0.071 0.088 0.033 -0.006 -0.012 -0.012 C55 0.038 0.095 0.028 0.003 -0.004 -0.009 C56 0.063 0.086 0.048 0.010 -0.001 -0.034 C57 0.099 0.140 0.022 -0.001 0.005 -0.041 C58 0.062 0.067 0.072 -0.011 0.015 -0.021 C59 0.103 0.073 0.072 -0.001 -0.004 -0.004 C60 0.109 0.067 0.070 0.012 -0.002 -0.003 C61 0.130 0.092 0.060 -0.017 0.008 0.022 C62 0.184 0.119 0.080 0.034 -0.002 -0.017 C63 0.054 0.083 0.035 0.021 -0.003 -0.029 C64 0.045 0.079 0.081 -0.005 0.011 -0.003 C65 0.077 0.075 0.039 -0.002 -0.021 0.003 C66 0.062 0.071 0.043 0.011 0.002 -0.017 C67 0.053 0.070 0.037 -0.003 0.001 -0.020 C68 0.041 0.091 0.051 0.013 -0.012 -0.017 C69 0.054 0.073 0.076 -0.002 -0.007 -0.021 C70 0.066 0.097 0.066 -0.016 0.000 -0.022 C71 0.046 0.110 0.037 -0.007 0.015 -0.032 C72 0.049 0.099 0.071 -0.009 0.006 -0.031 C73 0.061 0.128 0.048 0.015 0.011 -0.026 C74 0.087 0.109 0.038 0.007 -0.008 -0.042 C75 0.090 0.090 0.048 0.009 -0.005 -0.038 C76 0.082 0.079 0.039 0.016 0.004 -0.041 C77 0.103 0.197 0.057 -0.016 0.016 -0.102 C78 0.120 0.209 0.068 -0.044 0.007 -0.106 C79 0.142 0.244 0.044 -0.031 0.013 -0.148 C80 0.131 0.162 0.068 -0.030 0.044 -0.113 C81 0.224 0.404 0.043 -0.057 0.017 -0.221 C82 0.057 0.119 0.053 0.019 0.004 -0.022 C83 0.063 0.127 0.049 0.035 -0.001 0.003 C84 0.044 0.136 0.054 0.060 -0.014 -0.026 C85 0.070 0.116 0.060 0.006 0.005 0.000 C86 0.118 0.170 0.048 0.039 -0.026 -0.048 C87 0.061 0.110 0.058 -0.011 0.003 -0.011 C88 0.045 0.143 0.079 -0.019 0.021 -0.034 C89 0.082 0.150 0.053 -0.018 0.020 -0.022 C90 0.077 0.111 0.056 0.031 -0.009 -0.010 C91 0.123 0.264 0.060 -0.042 0.052 -0.052 C92 0.060 0.127 0.031 0.000 0.011 -0.042 C93 0.080 0.136 0.061 0.013 0.005 -0.065 C94 0.084 0.065 0.029 0.005 0.006 -0.012 C95 0.053 0.056 0.031 0.014 0.003 -0.011 C96 0.046 0.068 0.034 0.004 0.006 0.000 C97 0.043 0.065 0.049 -0.007 -0.010 -0.011 C98 0.049 0.086 0.044 -0.009 -0.008 -0.008 C99 0.047 0.076 0.040 0.014 -0.002 -0.001 C100 0.121 0.086 0.028 0.001 0.003 -0.007 C101 0.069 0.061 0.032 0.013 0.005 -0.002 C102 0.058 0.051 0.036 0.001 -0.005 -0.003 C103 0.060 0.068 0.044 0.010 0.008 -0.006 C104 0.060 0.049 0.087 0.004 0.011 -0.009 C105 0.049 0.052 0.066 -0.005 0.001 -0.003 C106 0.062 0.068 0.055 -0.002 -0.016 0.004 C107 0.038 0.078 0.064 -0.009 -0.011 0.003 C108 0.040 0.064 0.045 0.004 -0.006 0.006 C109 0.066 0.083 0.043 0.004 0.024 0.019 C110 0.085 0.093 0.060 0.003 0.007 0.026 C111 0.064 0.062 0.058 0.004 -0.002 0.013 C112 0.044 0.077 0.060 -0.006 -0.001 -0.014 C113 0.032 0.113 0.074 0.000 -0.013 -0.006 C114 0.053 0.084 0.056 -0.017 -0.010 -0.022 C115 0.060 0.098 0.069 0.018 0.003 -0.007 C116 0.071 0.193 0.054 -0.008 -0.019 -0.028 C117 0.045 0.065 0.048 0.008 -0.005 -0.007 C118 0.068 0.064 0.068 -0.017 0.007 0.013 C119 0.063 0.091 0.045 -0.018 0.009 -0.007 C120 0.071 0.090 0.058 0.027 -0.013 -0.001 C121 0.058 0.103 0.046 -0.010 0.004 0.003 C122 0.071 0.068 0.039 -0.002 0.001 -0.018 C123 0.062 0.053 0.046 0.013 -0.002 -0.023 C124 0.047 0.065 0.038 0.004 0.009 -0.018 C125 0.099 0.071 0.053 -0.005 -0.005 -0.028 C126 0.074 0.086 0.057 -0.002 0.000 -0.006 C127 0.036 0.069 0.033 -0.006 -0.001 -0.002 C128 0.104 0.076 0.053 -0.003 0.011 -0.023 C129 0.053 0.082 0.038 -0.001 -0.007 0.000 C130 0.035 0.080 0.037 -0.001 0.010 -0.011 C131 0.031 0.064 0.034 0.002 0.005 -0.015 C132 0.055 0.098 0.047 -0.023 0.022 -0.005 C133 0.048 0.107 0.091 -0.034 -0.008 0.022 C134 0.052 0.086 0.060 -0.009 -0.005 0.007 C135 0.047 0.051 0.047 0.018 0.003 -0.019 C136 0.063 0.048 0.067 0.012 0.006 -0.005 C137 0.042 0.064 0.057 -0.007 -0.006 -0.007 C138 0.047 0.093 0.048 -0.004 -0.005 -0.032 C139 0.052 0.096 0.046 0.018 -0.006 -0.035 C140 0.046 0.096 0.051 0.006 0.006 -0.038 C141 0.063 0.073 0.066 -0.011 -0.017 -0.006 C142 0.095 0.056 0.063 -0.007 -0.017 -0.013 C143 0.074 0.045 0.059 0.016 -0.012 -0.014 C144 0.104 0.074 0.053 0.000 -0.005 -0.021 C145 0.128 0.064 0.071 0.034 -0.026 -0.021 C146 0.050 0.071 0.063 -0.004 0.007 -0.032 C147 0.039 0.113 0.077 0.003 -0.014 -0.029 C148 0.043 0.074 0.053 0.003 -0.010 -0.007 C149 0.061 0.121 0.068 0.028 0.001 -0.040 C150 0.060 0.107 0.066 0.031 -0.026 -0.014 C151 0.043 0.055 0.055 0.011 0.012 -0.013 C152 0.055 0.056 0.044 0.015 -0.005 -0.003 C153 0.051 0.053 0.045 0.000 0.003 -0.015 C154 0.068 0.070 0.058 0.032 0.012 0.000 C155 0.053 0.096 0.048 0.008 -0.003 -0.003 C156 0.041 0.050 0.039 0.010 -0.005 -0.016 C157 0.054 0.098 0.099 -0.029 0.017 -0.029 C158 0.046 0.129 0.044 0.003 -0.004 -0.028 C159 0.060 0.107 0.049 0.000 -0.013 -0.020 C160 0.049 0.074 0.054 -0.008 -0.007 -0.024 C161 0.062 0.105 0.058 -0.014 -0.013 -0.012 C162 0.046 0.137 0.082 -0.021 -0.001 -0.027 C163 0.060 0.087 0.091 -0.011 -0.014 -0.031 C164 0.062 0.098 0.065 0.011 -0.001 -0.010 C165 0.069 0.124 0.083 -0.005 -0.014 0.004 C166 0.081 0.089 0.082 -0.018 -0.018 0.013 C167 0.089 0.060 0.057 0.023 0.004 -0.035 C168 0.096 0.079 0.071 -0.017 0.002 -0.044 C169 0.058 0.100 0.059 -0.017 -0.001 -0.025 C170 0.126 0.073 0.101 -0.038 0.025 -0.032 C171 0.170 0.073 0.083 0.000 0.010 -0.015 C172 0.112 0.070 0.109 0.002 0.011 -0.023 C173 0.163 0.092 0.112 -0.043 -0.005 -0.005 C174 0.179 0.069 0.102 0.018 0.030 -0.010 C175 0.075 0.094 0.062 0.002 0.023 -0.001 C176 0.056 0.147 0.063 0.000 -0.010 0.023 C177 0.062 0.116 0.062 0.018 0.004 -0.004 C178 0.095 0.128 0.055 0.015 0.005 -0.056 C179 0.133 0.116 0.048 0.021 -0.005 0.018 C180 0.056 0.055 0.080 -0.010 -0.010 -0.020 C181 0.054 0.071 0.080 -0.022 0.006 0.002 C182 0.059 0.080 0.071 -0.008 0.016 -0.021 C183 0.064 0.077 0.076 0.008 -0.017 -0.004 C184 0.135 0.102 0.087 0.013 0.019 0.012 C185 0.066 0.067 0.061 0.005 0.019 -0.016 C186 0.049 0.110 0.081 0.014 -0.015 0.034 _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 B1D F1D 1.294(6) . ? B1D F4D 1.302(6) . ? B1D F3D 1.340(6) . ? B1D F2D 1.348(6) . ? B1A F3A 1.26(2) . ? B1A F4A 1.283(17) . ? B1A F2A 1.54(2) . ? B1A F1A 1.67(2) . ? B1B F4B 1.35(3) . ? B1B F3B 1.45(2) . ? B1B F2B 1.46(3) . ? B1B F1B 1.46(3) . ? B1C F1C 1.294(6) . ? B1C F4C 1.302(6) . ? B1C F3C 1.340(6) . ? B1C F2C 1.348(6) . ? B1E F1E 1.295(6) . ? B1E F4E 1.302(6) . ? B1E F3E 1.340(6) . ? B1E F2E 1.348(6) . ? B1F F3F 1.307(12) . ? B1F F2F 1.352(11) . ? B1F F4F 1.377(11) . ? B1F F1F 1.419(12) . ? B1G F1G 1.294(6) . ? B1G F4G 1.302(6) . ? B1G F3G 1.340(6) . ? B1G F2G 1.348(6) . ? B1H F4H 1.299(12) . ? B1H F1H 1.360(12) . ? B1H F3H 1.368(11) . ? B1H F2H 1.379(11) . ? B1I F1I 1.295(6) . ? B1I F4I 1.302(6) . ? B1I F3I 1.340(6) . ? B1I F2I 1.348(6) . ? B1J F1J 1.295(6) . ? B1J F4J 1.302(6) . ? B1J F3J 1.340(6) . ? B1J F2J 1.348(6) . ? B1K F3K 1.299(19) . ? B1K F2K 1.328(19) . ? B1K F1K 1.331(18) . ? B1K F5K 1.50(2) . ? B1K F4K 1.52(2) . ? F3K F5K 1.76(2) . ? Fe1 N4 1.920(7) . ? Fe1 N2 1.939(6) . ? Fe1 N6 1.973(6) . ? Fe1 N9 1.981(6) . ? Fe1 N11 2.000(7) . ? Fe1 N7 2.008(6) . ? Fe2 N18 1.948(6) . ? Fe2 N16 1.952(7) . ? Fe2 N14 1.960(6) . ? Fe2 N19 1.972(6) . ? Fe2 N21 1.976(6) . ? Fe2 N23 2.004(7) . ? Fe3 N30 1.937(6) . ? Fe3 N28 1.938(7) . ? Fe3 N26 1.972(7) . ? Fe3 N35 1.983(7) . ? Fe3 N33 1.985(7) . ? Fe3 N31 1.990(8) . ? Fe4 N42 1.923(7) . ? Fe4 N40 1.940(6) . ? Fe4 N38 1.951(6) . ? Fe4 N43 1.992(6) . ? Fe4 N45 2.007(6) . ? Fe4 N47 2.012(6) . ? Fe5 N54 1.949(6) . ? Fe5 N52 1.965(6) . ? Fe5 N50 1.967(7) . ? Fe5 N59 1.982(6) . ? Fe5 N55 1.986(6) . ? Fe5 N57 2.021(6) . ? Fe6 N64 1.933(8) . ? Fe6 N66 1.947(7) . ? Fe6 N62 1.955(7) . ? Fe6 N69 1.962(7) . ? Fe6 N71 2.011(7) . ? Fe6 N67 2.046(8) . ? O1 C8 1.426(8) . ? O1 C7 1.429(8) . ? O2 C37 1.420(8) . ? O2 C36 1.436(8) . ? O3 C66 1.425(9) . ? O3 C65 1.438(8) . ? O4 C101 1.397(9) . ? O4 C100 1.459(8) . ? O5 C129 1.421(8) . ? O5 C130 1.424(8) . ? O6 C158 1.442(9) . ? O6 C159 1.452(9) . ? N1 C10 1.358(9) . ? N1 N2 1.382(7) . ? N1 C9 1.456(9) . ? N2 C12 1.338(9) . ? N3 N4 1.371(7) . ? N3 C13 1.390(10) . ? N3 C9 1.456(9) . ? N4 C15 1.346(9) . ? N5 N6 1.362(7) . ? N5 C16 1.363(8) . ? N5 C9 1.471(8) . ? N6 C18 1.300(8) . ? N7 C19 1.305(9) . ? N7 N8 1.354(7) . ? N8 C21 1.360(8) . ? N8 C34 1.437(10) . ? N9 C24 1.347(9) . ? N9 N10 1.374(7) . ? N10 C26 1.362(9) . ? N10 C34 1.451(10) . ? N11 C29 1.343(9) . ? N11 N12 1.372(7) . ? N12 C31 1.358(10) . ? N12 C34 1.440(10) . ? N13 C39 1.316(9) . ? N13 N14 1.375(8) . ? N13 C38 1.490(9) . ? N14 C41 1.338(9) . ? N15 C42 1.367(9) . ? N15 N16 1.381(7) . ? N15 C38 1.429(9) . ? N16 C44 1.326(9) . ? N17 N18 1.352(7) . ? N17 C45 1.386(8) . ? N17 C38 1.469(8) . ? N18 C47 1.352(9) . ? N19 C48 1.348(9) . ? N19 N20 1.404(7) . ? N20 C50 1.388(9) . ? N20 C63 1.437(9) . ? N21 C53 1.347(9) . ? N21 N22 1.360(7) . ? N22 C55 1.337(9) . ? N22 C63 1.439(9) . ? N23 C58 1.302(10) . ? N23 N24 1.383(8) . ? N24 C60 1.359(10) . ? N24 C63 1.453(10) . ? N25 N26 1.361(8) . ? N25 C68 1.380(10) . ? N25 C67 1.433(10) . ? N26 C70 1.323(10) . ? N27 C71 1.370(9) . ? N27 N28 1.391(8) . ? N27 C67 1.444(9) . ? N28 C73 1.380(10) . ? N29 C74 1.342(9) . ? N29 N30 1.358(7) . ? N29 C67 1.492(9) . ? N30 C76 1.335(9) . ? N31 C77 1.300(11) . ? N31 N32 1.424(8) . ? N32 C79 1.347(11) . ? N32 C92 1.451(11) . ? N33 C82 1.334(11) . ? N33 N34 1.382(8) . ? N34 C84 1.413(11) . ? N34 C92 1.476(12) . ? N35 C87 1.342(10) . ? N35 N36 1.393(8) . ? N36 C89 1.372(11) . ? N36 C92 1.408(10) . ? N37 N38 1.370(8) . ? N37 C103 1.395(9) . ? N37 C102 1.439(9) . ? N38 C105 1.379(9) . ? N39 N40 1.393(7) . ? N39 C106 1.394(9) . ? N39 C102 1.436(9) . ? N40 C108 1.320(9) . ? N41 C109 1.388(9) . ? N41 N42 1.408(7) . ? N41 C102 1.444(9) . ? N42 C111 1.327(9) . ? N43 C112 1.332(9) . ? N43 N44 1.361(7) . ? N44 C114 1.348(9) . ? N44 C127 1.457(8) . ? N45 C117 1.344(9) . ? N45 N46 1.390(7) . ? N46 C119 1.366(9) . ? N46 C127 1.428(8) . ? N47 C122 1.307(9) . ? N47 N48 1.382(7) . ? N48 C124 1.358(9) . ? N48 C127 1.441(9) . ? N49 C132 1.367(9) . ? N49 N50 1.390(8) . ? N49 C131 1.432(9) . ? N50 C134 1.324(9) . ? N51 C135 1.315(8) . ? N51 N52 1.359(7) . ? N51 C131 1.508(9) . ? N52 C137 1.352(9) . ? N53 N54 1.350(7) . ? N53 C138 1.353(9) . ? N53 C131 1.462(8) . ? N54 C140 1.355(9) . ? N55 C141 1.302(9) . ? N55 N56 1.364(8) . ? N56 C143 1.375(9) . ? N56 C156 1.442(9) . ? N57 C146 1.345(9) . ? N57 N58 1.370(7) . ? N58 C148 1.373(8) . ? N58 C156 1.435(8) . ? N59 C151 1.328(9) . ? N59 N60 1.386(7) . ? N60 C153 1.361(9) . ? N60 C156 1.436(9) . ? N61 C161 1.378(9) . ? N61 N62 1.389(9) . ? N61 C160 1.477(9) . ? N62 C163 1.335(10) . ? N63 C164 1.344(10) . ? N63 N64 1.415(9) . ? N63 C160 1.460(10) . ? N64 C166 1.281(10) . ? N65 C167 1.370(10) . ? N65 N66 1.384(8) . ? N65 C160 1.443(10) . ? N66 C169 1.370(10) . ? N67 C170 1.291(10) . ? N67 N68 1.326(9) . ? N68 C172 1.384(11) . ? N68 C185 1.454(11) . ? N69 C175 1.347(11) . ? N69 N70 1.387(8) . ? N70 C177 1.362(11) . ? N70 C185 1.420(10) . ? N71 C180 1.273(9) . ? N71 N72 1.407(8) . ? N72 C182 1.336(10) . ? N72 C185 1.464(10) . ? C1 C2 1.380(10) . ? C1 C6 1.412(10) . ? C1 C7 1.518(10) . ? C2 C3 1.424(10) . ? C2 C35 1.488(10) . ? C3 C4 1.385(10) . ? C3 C36 1.547(10) . ? C4 C5 1.390(10) . ? C4 C64 1.512(10) . ? C5 C6 1.419(10) . ? C5 C65 1.488(10) . ? C6 C93 1.546(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.529(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C10 C11 1.345(11) . ? C10 H10 0.9400 . ? C11 C12 1.390(10) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.330(11) . ? C13 H13 0.9400 . ? C14 C15 1.372(11) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.313(10) . ? C16 H16 0.9400 . ? C17 C18 1.431(10) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.428(10) . ? C19 C22 1.522(11) . ? C20 C21 1.363(12) . ? C20 H20 0.9400 . ? C21 C23 1.499(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.371(10) . ? C24 C27 1.508(11) . ? C25 C26 1.367(12) . ? C25 H25 0.9400 . ? C26 C28 1.521(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C30 1.381(11) . ? C29 C32 1.495(10) . ? C30 C31 1.325(11) . ? C30 H30 0.9400 . ? C31 C33 1.510(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34 0.9900 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.532(9) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C39 C40 1.389(12) . ? C39 H39 0.9400 . ? C40 C41 1.389(11) . ? C40 H40 0.9400 . ? C41 H41 0.9400 . ? C42 C43 1.395(11) . ? C42 H42 0.9400 . ? C43 C44 1.388(11) . ? C43 H43 0.9400 . ? C44 H44 0.9400 . ? C45 C46 1.344(10) . ? C45 H45 0.9400 . ? C46 C47 1.380(10) . ? C46 H46 0.9400 . ? C47 H47 0.9400 . ? C48 C49 1.390(10) . ? C48 C51 1.459(11) . ? C49 C50 1.353(11) . ? C49 H49 0.9400 . ? C50 C52 1.507(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 C54 1.409(10) . ? C53 C56 1.513(10) . ? C54 C55 1.366(11) . ? C54 H54 0.9400 . ? C55 C57 1.522(9) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C57 H57C 0.9700 . ? C58 C59 1.398(12) . ? C58 C61 1.480(11) . ? C59 C60 1.350(12) . ? C59 H59 0.9400 . ? C60 C62 1.506(13) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 H63 0.9900 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C66 C67 1.551(10) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C68 C69 1.355(11) . ? C68 H68 0.9400 . ? C69 C70 1.459(12) . ? C69 H69 0.9400 . ? C70 H70 0.9400 . ? C71 C72 1.319(11) . ? C71 H71 0.9400 . ? C72 C73 1.412(11) . ? C72 H72 0.9400 . ? C73 H73 0.9400 . ? C74 C75 1.383(11) . ? C74 H74 0.9400 . ? C75 C76 1.385(11) . ? C75 H75 0.9400 . ? C76 H76 0.9400 . ? C77 C78 1.398(12) . ? C77 C80 1.509(12) . ? C78 C79 1.389(13) . ? C78 H78 0.9400 . ? C79 C81 1.516(13) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C80 H80C 0.9700 . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C81 H81C 0.9700 . ? C82 C83 1.412(11) . ? C82 C85 1.492(12) . ? C83 C84 1.343(13) . ? C83 H83 0.9400 . ? C84 C86 1.538(12) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C85 H85C 0.9700 . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C86 H86C 0.9700 . ? C87 C88 1.353(11) . ? C87 C90 1.466(11) . ? C88 C89 1.363(13) . ? C88 H88 0.9400 . ? C89 C91 1.568(13) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C90 H90C 0.9700 . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C91 H91C 0.9700 . ? C92 H92 0.9900 . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C93 H93C 0.9700 . ? C94 C95 1.415(11) . ? C94 C99 1.423(11) . ? C94 C100 1.531(11) . ? C95 C96 1.393(10) . ? C95 C128 1.490(11) . ? C96 C97 1.411(10) . ? C96 C129 1.513(10) . ? C97 C98 1.403(10) . ? C97 C157 1.513(11) . ? C98 C99 1.382(11) . ? C98 C158 1.550(11) . ? C99 C186 1.557(11) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C101 C102 1.486(9) . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C103 C104 1.333(11) . ? C103 H103 0.9400 . ? C104 C105 1.396(11) . ? C104 H104 0.9400 . ? C105 H105 0.9400 . ? C106 C107 1.409(11) . ? C106 H106 0.9400 . ? C107 C108 1.429(10) . ? C107 H107 0.9400 . ? C108 H108 0.9400 . ? C109 C110 1.347(11) . ? C109 H109 0.9400 . ? C110 C111 1.409(11) . ? C110 H110 0.9400 . ? C111 H111 0.9400 . ? C112 C113 1.413(11) . ? C112 C115 1.493(11) . ? C113 C114 1.414(11) . ? C113 H113 0.9400 . ? C114 C116 1.475(11) . ? C115 H11A 0.9700 . ? C115 H11B 0.9700 . ? C115 H11C 0.9700 . ? C116 H11D 0.9700 . ? C116 H11E 0.9700 . ? C116 H11F 0.9700 . ? C117 C118 1.400(10) . ? C117 C120 1.482(10) . ? C118 C119 1.369(11) . ? C118 H118 0.9400 . ? C119 C121 1.502(10) . ? C120 H12A 0.9700 . ? C120 H12B 0.9700 . ? C120 H12C 0.9700 . ? C121 H12D 0.9700 . ? C121 H12E 0.9700 . ? C121 H12F 0.9700 . ? C122 C123 1.431(9) . ? C122 C125 1.474(10) . ? C123 C124 1.326(10) . ? C123 H123 0.9400 . ? C124 C126 1.513(10) . ? C125 H12G 0.9700 . ? C125 H12H 0.9700 . ? C125 H12I 0.9700 . ? C126 H12J 0.9700 . ? C126 H12K 0.9700 . ? C126 H12L 0.9700 . ? C127 H127 0.9900 . ? C128 H12M 0.9700 . ? C128 H12N 0.9700 . ? C128 H12O 0.9700 . ? C129 H12P 0.9800 . ? C129 H12Q 0.9800 . ? C130 C131 1.531(9) . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C132 C133 1.333(11) . ? C132 H132 0.9400 . ? C133 C134 1.388(11) . ? C133 H133 0.9400 . ? C134 H134 0.9400 . ? C135 C136 1.329(10) . ? C135 H135 0.9400 . ? C136 C137 1.397(10) . ? C136 H136 0.9400 . ? C137 H137 0.9400 . ? C138 C139 1.378(10) . ? C138 H138 0.9400 . ? C139 C140 1.367(10) . ? C139 H139 0.9400 . ? C140 H140 0.9400 . ? C141 C142 1.442(11) . ? C141 C144 1.512(11) . ? C142 C143 1.365(11) . ? C142 H142 0.9400 . ? C143 C145 1.515(11) . ? C144 H14A 0.9700 . ? C144 H14B 0.9700 . ? C144 H14C 0.9700 . ? C145 H14D 0.9700 . ? C145 H14E 0.9700 . ? C145 H14F 0.9700 . ? C146 C147 1.418(11) . ? C146 C149 1.487(10) . ? C147 C148 1.371(11) . ? C147 H147 0.9400 . ? C148 C150 1.485(10) . ? C149 H14G 0.9700 . ? C149 H14H 0.9700 . ? C149 H14I 0.9700 . ? C150 H15A 0.9700 . ? C150 H15B 0.9700 . ? C150 H15C 0.9700 . ? C151 C152 1.429(10) . ? C151 C154 1.487(10) . ? C152 C153 1.346(10) . ? C152 H152 0.9400 . ? C153 C155 1.479(10) . ? C154 H15D 0.9700 . ? C154 H15E 0.9700 . ? C154 H15F 0.9700 . ? C155 H15G 0.9700 . ? C155 H15H 0.9700 . ? C155 H15I 0.9700 . ? C156 H156 0.9900 . ? C157 H15J 0.9700 . ? C157 H15K 0.9700 . ? C157 H15L 0.9700 . ? C158 H15M 0.9800 . ? C158 H15N 0.9800 . ? C159 C160 1.522(11) . ? C159 H15O 0.9800 . ? C159 H15P 0.9800 . ? C161 C162 1.457(12) . ? C161 H161 0.9400 . ? C162 C163 1.352(12) . ? C162 H162 0.9400 . ? C163 H163 0.9400 . ? C164 C165 1.410(13) . ? C164 H164 0.9400 . ? C165 C166 1.394(13) . ? C165 H165 0.9400 . ? C166 H166 0.9400 . ? C167 C168 1.336(11) . ? C167 H167 0.9400 . ? C168 C169 1.387(12) . ? C168 H168 0.9400 . ? C169 H169 0.9400 . ? C170 C171 1.358(14) . ? C170 C173 1.551(14) . ? C171 C172 1.349(14) . ? C171 H171 0.9400 . ? C172 C174 1.506(14) . ? C173 H17A 0.9700 . ? C173 H17B 0.9700 . ? C173 H17C 0.9700 . ? C174 H17D 0.9700 . ? C174 H17E 0.9700 . ? C174 H17F 0.9700 . ? C175 C176 1.439(12) . ? C175 C178 1.510(11) . ? C176 C177 1.370(13) . ? C176 H176 0.9400 . ? C177 C179 1.535(12) . ? C178 H17G 0.9700 . ? C178 H17H 0.9700 . ? C178 H17I 0.9700 . ? C179 H17J 0.9700 . ? C179 H17K 0.9700 . ? C179 H17L 0.9700 . ? C180 C181 1.429(11) . ? C180 C183 1.507(11) . ? C181 C182 1.323(11) . ? C181 H181 0.9400 . ? C182 C184 1.484(12) . ? C183 H18A 0.9700 . ? C183 H18B 0.9700 . ? C183 H18C 0.9700 . ? C184 H18D 0.9700 . ? C184 H18E 0.9700 . ? C184 H18F 0.9700 . ? C185 H185 0.9900 . ? C186 H18G 0.9700 . ? C186 H18H 0.9700 . ? C186 H18I 0.9700 . ? 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 F1D B1D F4D 111.0(5) . . ? F1D B1D F3D 110.9(5) . . ? F4D B1D F3D 108.0(6) . . ? F1D B1D F2D 111.9(6) . . ? F4D B1D F2D 108.0(5) . . ? F3D B1D F2D 106.8(5) . . ? F3A B1A F4A 126.2(17) . . ? F3A B1A F2A 108.2(16) . . ? F4A B1A F2A 110.7(14) . . ? F3A B1A F1A 105.0(16) . . ? F4A B1A F1A 110.6(14) . . ? F2A B1A F1A 90.0(12) . . ? F4B B1B F3B 118(2) . . ? F4B B1B F2B 111.0(19) . . ? F3B B1B F2B 104(2) . . ? F4B B1B F1B 113.5(18) . . ? F3B B1B F1B 106(2) . . ? F2B B1B F1B 102.5(19) . . ? F1C B1C F4C 111.0(6) . . ? F1C B1C F3C 110.9(5) . . ? F4C B1C F3C 107.9(6) . . ? F1C B1C F2C 111.9(6) . . ? F4C B1C F2C 107.9(5) . . ? F3C B1C F2C 107.0(5) . . ? F1E B1E F4E 110.9(5) . . ? F1E B1E F3E 110.9(5) . . ? F4E B1E F3E 108.0(6) . . ? F1E B1E F2E 112.0(6) . . ? F4E B1E F2E 108.1(5) . . ? F3E B1E F2E 106.8(5) . . ? F3F B1F F2F 110.3(9) . . ? F3F B1F F4F 114.7(10) . . ? F2F B1F F4F 110.7(8) . . ? F3F B1F F1F 107.1(8) . . ? F2F B1F F1F 112.9(9) . . ? F4F B1F F1F 100.9(8) . . ? F1G B1G F4G 110.9(5) . . ? F1G B1G F3G 110.9(5) . . ? F4G B1G F3G 108.0(6) . . ? F1G B1G F2G 112.0(6) . . ? F4G B1G F2G 108.0(5) . . ? F3G B1G F2G 106.8(5) . . ? F4H B1H F1H 103.3(9) . . ? F4H B1H F3H 111.1(9) . . ? F1H B1H F3H 109.0(9) . . ? F4H B1H F2H 109.9(10) . . ? F1H B1H F2H 110.3(9) . . ? F3H B1H F2H 112.9(8) . . ? F1I B1I F4I 110.9(5) . . ? F1I B1I F3I 110.9(5) . . ? F4I B1I F3I 107.9(6) . . ? F1I B1I F2I 112.0(6) . . ? F4I B1I F2I 108.1(5) . . ? F3I B1I F2I 106.8(5) . . ? F1J B1J F4J 111.0(5) . . ? F1J B1J F3J 111.0(5) . . ? F4J B1J F3J 107.9(6) . . ? F1J B1J F2J 112.0(6) . . ? F4J B1J F2J 108.0(5) . . ? F3J B1J F2J 106.7(5) . . ? F3K B1K F2K 122.0(18) . . ? F3K B1K F1K 117.6(18) . . ? F2K B1K F1K 119.6(17) . . ? F3K B1K F5K 77.6(14) . . ? F2K B1K F5K 85.2(15) . . ? F1K B1K F5K 98.5(15) . . ? F3K B1K F4K 97.9(15) . . ? F2K B1K F4K 90.6(13) . . ? F1K B1K F4K 90.7(14) . . ? F5K B1K F4K 170.8(18) . . ? B1K F3K F5K 56.4(11) . . ? B1K F5K F3K 46.0(10) . . ? N4 Fe1 N2 87.4(3) . . ? N4 Fe1 N6 87.4(2) . . ? N2 Fe1 N6 87.3(2) . . ? N4 Fe1 N9 92.2(3) . . ? N2 Fe1 N9 179.5(3) . . ? N6 Fe1 N9 92.9(2) . . ? N4 Fe1 N11 178.6(2) . . ? N2 Fe1 N11 91.8(3) . . ? N6 Fe1 N11 91.4(2) . . ? N9 Fe1 N11 88.6(2) . . ? N4 Fe1 N7 92.7(3) . . ? N2 Fe1 N7 91.4(2) . . ? N6 Fe1 N7 178.7(2) . . ? N9 Fe1 N7 88.3(2) . . ? N11 Fe1 N7 88.5(3) . . ? N18 Fe2 N16 87.7(3) . . ? N18 Fe2 N14 87.2(2) . . ? N16 Fe2 N14 87.3(3) . . ? N18 Fe2 N19 179.9(3) . . ? N16 Fe2 N19 92.3(3) . . ? N14 Fe2 N19 92.9(2) . . ? N18 Fe2 N21 92.9(2) . . ? N16 Fe2 N21 91.5(2) . . ? N14 Fe2 N21 178.8(3) . . ? N19 Fe2 N21 87.0(2) . . ? N18 Fe2 N23 91.1(3) . . ? N16 Fe2 N23 178.7(3) . . ? N14 Fe2 N23 92.1(3) . . ? N19 Fe2 N23 88.9(3) . . ? N21 Fe2 N23 89.0(3) . . ? N30 Fe3 N28 87.3(3) . . ? N30 Fe3 N26 87.6(3) . . ? N28 Fe3 N26 86.0(3) . . ? N30 Fe3 N35 90.3(3) . . ? N28 Fe3 N35 177.6(3) . . ? N26 Fe3 N35 93.8(3) . . ? N30 Fe3 N33 92.9(3) . . ? N28 Fe3 N33 91.3(3) . . ? N26 Fe3 N33 177.3(3) . . ? N35 Fe3 N33 88.8(3) . . ? N30 Fe3 N31 178.2(3) . . ? N28 Fe3 N31 92.8(3) . . ? N26 Fe3 N31 90.6(3) . . ? N35 Fe3 N31 89.5(3) . . ? N33 Fe3 N31 88.9(3) . . ? N42 Fe4 N40 87.9(3) . . ? N42 Fe4 N38 88.1(3) . . ? N40 Fe4 N38 86.1(2) . . ? N42 Fe4 N43 91.2(3) . . ? N40 Fe4 N43 179.0(3) . . ? N38 Fe4 N43 94.3(3) . . ? N42 Fe4 N45 178.1(2) . . ? N40 Fe4 N45 93.6(2) . . ? N38 Fe4 N45 93.2(3) . . ? N43 Fe4 N45 87.4(2) . . ? N42 Fe4 N47 90.8(3) . . ? N40 Fe4 N47 91.1(2) . . ? N38 Fe4 N47 177.0(3) . . ? N43 Fe4 N47 88.5(2) . . ? N45 Fe4 N47 88.0(2) . . ? N54 Fe5 N52 86.8(2) . . ? N54 Fe5 N50 88.2(2) . . ? N52 Fe5 N50 85.1(3) . . ? N54 Fe5 N59 91.6(2) . . ? N52 Fe5 N59 91.9(2) . . ? N50 Fe5 N59 177.0(3) . . ? N54 Fe5 N55 91.5(2) . . ? N52 Fe5 N55 178.0(3) . . ? N50 Fe5 N55 93.7(3) . . ? N59 Fe5 N55 89.3(2) . . ? N54 Fe5 N57 178.0(2) . . ? N52 Fe5 N57 94.3(2) . . ? N50 Fe5 N57 93.5(3) . . ? N59 Fe5 N57 86.8(2) . . ? N55 Fe5 N57 87.4(2) . . ? N64 Fe6 N66 88.0(3) . . ? N64 Fe6 N62 86.9(3) . . ? N66 Fe6 N62 87.3(3) . . ? N64 Fe6 N69 92.1(3) . . ? N66 Fe6 N69 92.7(3) . . ? N62 Fe6 N69 179.1(3) . . ? N64 Fe6 N71 178.9(3) . . ? N66 Fe6 N71 91.8(3) . . ? N62 Fe6 N71 92.0(3) . . ? N69 Fe6 N71 88.9(3) . . ? N64 Fe6 N67 92.1(3) . . ? N66 Fe6 N67 179.9(4) . . ? N62 Fe6 N67 92.7(3) . . ? N69 Fe6 N67 87.3(3) . . ? N71 Fe6 N67 88.1(3) . . ? C8 O1 C7 111.0(5) . . ? C37 O2 C36 110.8(5) . . ? C66 O3 C65 111.6(6) . . ? C101 O4 C100 111.7(6) . . ? C129 O5 C130 110.9(5) . . ? C158 O6 C159 109.1(5) . . ? C10 N1 N2 110.0(6) . . ? C10 N1 C9 132.4(6) . . ? N2 N1 C9 117.3(6) . . ? C12 N2 N1 104.1(6) . . ? C12 N2 Fe1 136.0(5) . . ? N1 N2 Fe1 119.8(5) . . ? N4 N3 C13 109.4(7) . . ? N4 N3 C9 118.5(6) . . ? C13 N3 C9 131.9(6) . . ? C15 N4 N3 103.7(6) . . ? C15 N4 Fe1 135.7(5) . . ? N3 N4 Fe1 119.5(5) . . ? N6 N5 C16 111.2(5) . . ? N6 N5 C9 118.1(5) . . ? C16 N5 C9 130.6(6) . . ? C18 N6 N5 104.8(6) . . ? C18 N6 Fe1 136.2(5) . . ? N5 N6 Fe1 118.9(4) . . ? C19 N7 N8 105.2(6) . . ? C19 N7 Fe1 137.1(5) . . ? N8 N7 Fe1 117.6(4) . . ? N7 N8 C21 112.2(6) . . ? N7 N8 C34 116.9(6) . . ? C21 N8 C34 130.8(6) . . ? C24 N9 N10 104.4(6) . . ? C24 N9 Fe1 140.1(5) . . ? N10 N9 Fe1 115.4(4) . . ? C26 N10 N9 111.6(6) . . ? C26 N10 C34 129.1(6) . . ? N9 N10 C34 119.2(6) . . ? C29 N11 N12 106.6(6) . . ? C29 N11 Fe1 137.7(5) . . ? N12 N11 Fe1 115.7(5) . . ? C31 N12 N11 110.0(6) . . ? C31 N12 C34 131.4(6) . . ? N11 N12 C34 118.7(6) . . ? C39 N13 N14 112.1(6) . . ? C39 N13 C38 131.6(6) . . ? N14 N13 C38 116.2(5) . . ? C41 N14 N13 104.6(6) . . ? C41 N14 Fe2 134.6(5) . . ? N13 N14 Fe2 120.3(5) . . ? C42 N15 N16 109.7(6) . . ? C42 N15 C38 130.6(6) . . ? N16 N15 C38 119.3(6) . . ? C44 N16 N15 106.5(6) . . ? C44 N16 Fe2 135.1(5) . . ? N15 N16 Fe2 118.3(5) . . ? N18 N17 C45 110.8(5) . . ? N18 N17 C38 119.3(5) . . ? C45 N17 C38 129.9(6) . . ? N17 N18 C47 105.1(6) . . ? N17 N18 Fe2 118.9(4) . . ? C47 N18 Fe2 135.6(5) . . ? C48 N19 N20 104.3(6) . . ? C48 N19 Fe2 139.7(5) . . ? N20 N19 Fe2 115.8(4) . . ? C50 N20 N19 111.4(6) . . ? C50 N20 C63 130.6(6) . . ? N19 N20 C63 117.6(6) . . ? C53 N21 N22 103.9(6) . . ? C53 N21 Fe2 136.5(5) . . ? N22 N21 Fe2 119.4(5) . . ? C55 N22 N21 113.6(6) . . ? C55 N22 C63 130.7(6) . . ? N21 N22 C63 115.4(6) . . ? C58 N23 N24 105.5(7) . . ? C58 N23 Fe2 138.5(6) . . ? N24 N23 Fe2 115.8(5) . . ? C60 N24 N23 112.2(7) . . ? C60 N24 C63 130.3(7) . . ? N23 N24 C63 117.5(6) . . ? N26 N25 C68 109.3(7) . . ? N26 N25 C67 119.5(7) . . ? C68 N25 C67 131.0(7) . . ? C70 N26 N25 108.2(7) . . ? C70 N26 Fe3 133.0(6) . . ? N25 N26 Fe3 118.5(6) . . ? C71 N27 N28 109.2(6) . . ? C71 N27 C67 132.3(6) . . ? N28 N27 C67 117.9(6) . . ? C73 N28 N27 104.9(7) . . ? C73 N28 Fe3 135.7(6) . . ? N27 N28 Fe3 119.4(5) . . ? C74 N29 N30 111.9(6) . . ? C74 N29 C67 130.9(6) . . ? N30 N29 C67 117.0(6) . . ? C76 N30 N29 103.9(6) . . ? C76 N30 Fe3 134.7(5) . . ? N29 N30 Fe3 120.7(5) . . ? C77 N31 N32 102.4(7) . . ? C77 N31 Fe3 141.9(6) . . ? N32 N31 Fe3 115.7(5) . . ? C79 N32 N31 113.2(7) . . ? C79 N32 C92 128.9(7) . . ? N31 N32 C92 117.8(7) . . ? C82 N33 N34 106.7(8) . . ? C82 N33 Fe3 137.6(6) . . ? N34 N33 Fe3 115.3(7) . . ? N33 N34 C84 107.3(9) . . ? N33 N34 C92 119.8(8) . . ? C84 N34 C92 132.5(8) . . ? C87 N35 N36 104.1(6) . . ? C87 N35 Fe3 139.3(5) . . ? N36 N35 Fe3 116.2(5) . . ? C89 N36 N35 111.1(7) . . ? C89 N36 C92 129.7(7) . . ? N35 N36 C92 118.8(6) . . ? N38 N37 C103 109.1(6) . . ? N38 N37 C102 118.8(6) . . ? C103 N37 C102 132.1(6) . . ? N37 N38 C105 106.0(6) . . ? N37 N38 Fe4 119.7(5) . . ? C105 N38 Fe4 134.0(5) . . ? N40 N39 C106 109.5(6) . . ? N40 N39 C102 121.1(5) . . ? C106 N39 C102 129.2(6) . . ? C108 N40 N39 106.9(6) . . ? C108 N40 Fe4 135.8(5) . . ? N39 N40 Fe4 117.3(4) . . ? C109 N41 N42 109.0(6) . . ? C109 N41 C102 131.8(6) . . ? N42 N41 C102 119.1(6) . . ? C111 N42 N41 105.1(6) . . ? C111 N42 Fe4 135.4(5) . . ? N41 N42 Fe4 118.5(5) . . ? C112 N43 N44 106.1(6) . . ? C112 N43 Fe4 136.2(5) . . ? N44 N43 Fe4 117.0(4) . . ? C114 N44 N43 113.5(6) . . ? C114 N44 C127 127.9(6) . . ? N43 N44 C127 118.5(5) . . ? C117 N45 N46 104.0(6) . . ? C117 N45 Fe4 139.1(5) . . ? N46 N45 Fe4 116.2(4) . . ? C119 N46 N45 111.6(6) . . ? C119 N46 C127 129.7(6) . . ? N45 N46 C127 118.1(6) . . ? C122 N47 N48 106.8(6) . . ? C122 N47 Fe4 136.9(5) . . ? N48 N47 Fe4 115.5(5) . . ? C124 N48 N47 110.3(6) . . ? C124 N48 C127 130.3(6) . . ? N47 N48 C127 119.4(6) . . ? C132 N49 N50 109.2(6) . . ? C132 N49 C131 132.4(7) . . ? N50 N49 C131 118.3(6) . . ? C134 N50 N49 104.9(6) . . ? C134 N50 Fe5 135.9(6) . . ? N49 N50 Fe5 119.2(4) . . ? C135 N51 N52 111.5(6) . . ? C135 N51 C131 130.5(6) . . ? N52 N51 C131 117.5(5) . . ? C137 N52 N51 105.7(6) . . ? C137 N52 Fe5 134.1(5) . . ? N51 N52 Fe5 120.2(5) . . ? N54 N53 C138 112.4(6) . . ? N54 N53 C131 118.8(5) . . ? C138 N53 C131 128.6(6) . . ? N53 N54 C140 104.3(6) . . ? N53 N54 Fe5 120.3(4) . . ? C140 N54 Fe5 134.3(5) . . ? C141 N55 N56 106.4(6) . . ? C141 N55 Fe5 137.4(5) . . ? N56 N55 Fe5 116.0(5) . . ? N55 N56 C143 111.4(6) . . ? N55 N56 C156 120.0(6) . . ? C143 N56 C156 128.3(6) . . ? C146 N57 N58 105.9(6) . . ? C146 N57 Fe5 137.9(5) . . ? N58 N57 Fe5 116.1(4) . . ? N57 N58 C148 110.9(6) . . ? N57 N58 C156 119.1(5) . . ? C148 N58 C156 129.9(6) . . ? C151 N59 N60 104.9(6) . . ? C151 N59 Fe5 137.3(5) . . ? N60 N59 Fe5 117.2(4) . . ? C153 N60 N59 111.9(6) . . ? C153 N60 C156 129.8(6) . . ? N59 N60 C156 118.1(5) . . ? C161 N61 N62 111.1(6) . . ? C161 N61 C160 130.6(7) . . ? N62 N61 C160 118.3(6) . . ? C163 N62 N61 105.5(7) . . ? C163 N62 Fe6 135.2(6) . . ? N61 N62 Fe6 119.2(5) . . ? C164 N63 N64 109.9(7) . . ? C164 N63 C160 131.2(7) . . ? N64 N63 C160 118.6(6) . . ? C166 N64 N63 104.6(8) . . ? C166 N64 Fe6 136.6(7) . . ? N63 N64 Fe6 118.5(5) . . ? C167 N65 N66 109.0(7) . . ? C167 N65 C160 132.9(7) . . ? N66 N65 C160 118.1(7) . . ? C169 N66 N65 104.9(7) . . ? C169 N66 Fe6 134.4(5) . . ? N65 N66 Fe6 120.0(5) . . ? C170 N67 N68 107.6(8) . . ? C170 N67 Fe6 138.5(7) . . ? N68 N67 Fe6 113.9(6) . . ? N67 N68 C172 111.5(9) . . ? N67 N68 C185 122.6(7) . . ? C172 N68 C185 125.8(8) . . ? C175 N69 N70 104.6(6) . . ? C175 N69 Fe6 137.0(6) . . ? N70 N69 Fe6 118.5(5) . . ? C177 N70 N69 113.8(7) . . ? C177 N70 C185 128.8(7) . . ? N69 N70 C185 117.4(6) . . ? C180 N71 N72 105.4(7) . . ? C180 N71 Fe6 137.5(6) . . ? N72 N71 Fe6 116.3(5) . . ? C182 N72 N71 109.2(7) . . ? C182 N72 C185 133.8(7) . . ? N71 N72 C185 116.9(6) . . ? C2 C1 C6 120.8(7) . . ? C2 C1 C7 119.5(7) . . ? C6 C1 C7 119.7(7) . . ? C1 C2 C3 118.8(7) . . ? C1 C2 C35 121.5(7) . . ? C3 C2 C35 119.7(7) . . ? C4 C3 C2 121.2(7) . . ? C4 C3 C36 120.1(7) . . ? C2 C3 C36 118.7(7) . . ? C3 C4 C5 119.8(7) . . ? C3 C4 C64 119.3(7) . . ? C5 C4 C64 120.9(7) . . ? C4 C5 C6 120.1(7) . . ? C4 C5 C65 120.7(7) . . ? C6 C5 C65 119.3(7) . . ? C1 C6 C5 119.3(7) . . ? C1 C6 C93 121.3(8) . . ? C5 C6 C93 119.4(8) . . ? O1 C7 C1 107.1(5) . . ? O1 C7 H7A 110.3 . . ? C1 C7 H7A 110.3 . . ? O1 C7 H7B 110.3 . . ? C1 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? O1 C8 C9 107.3(5) . . ? O1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? O1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? N1 C9 N3 109.1(5) . . ? N1 C9 N5 109.6(6) . . ? N3 C9 N5 106.7(5) . . ? N1 C9 C8 111.6(6) . . ? N3 C9 C8 110.8(6) . . ? N5 C9 C8 108.9(5) . . ? C11 C10 N1 108.6(7) . . ? C11 C10 H10 125.7 . . ? N1 C10 H10 125.7 . . ? C10 C11 C12 105.3(8) . . ? C10 C11 H11 127.4 . . ? C12 C11 H11 127.4 . . ? N2 C12 C11 111.9(7) . . ? N2 C12 H12 124.0 . . ? C11 C12 H12 124.0 . . ? C14 C13 N3 108.3(8) . . ? C14 C13 H13 125.8 . . ? N3 C13 H13 125.8 . . ? C13 C14 C15 105.5(9) . . ? C13 C14 H14 127.2 . . ? C15 C14 H14 127.2 . . ? N4 C15 C14 112.9(8) . . ? N4 C15 H15 123.5 . . ? C14 C15 H15 123.5 . . ? C17 C16 N5 107.3(6) . . ? C17 C16 H16 126.3 . . ? N5 C16 H16 126.3 . . ? C16 C17 C18 105.8(6) . . ? C16 C17 H17 127.1 . . ? C18 C17 H17 127.1 . . ? N6 C18 C17 110.7(6) . . ? N6 C18 H18 124.6 . . ? C17 C18 H18 124.6 . . ? N7 C19 C20 111.4(7) . . ? N7 C19 C22 126.0(7) . . ? C20 C19 C22 122.6(7) . . ? C21 C20 C19 104.7(8) . . ? C21 C20 H20 127.6 . . ? C19 C20 H20 127.6 . . ? N8 C21 C20 106.4(7) . . ? N8 C21 C23 123.7(7) . . ? C20 C21 C23 129.8(7) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N9 C24 C25 110.5(7) . . ? N9 C24 C27 121.1(7) . . ? C25 C24 C27 128.3(8) . . ? C26 C25 C24 107.9(7) . . ? C26 C25 H25 126.1 . . ? C24 C25 H25 126.1 . . ? N10 C26 C25 105.5(7) . . ? N10 C26 C28 123.1(8) . . ? C25 C26 C28 131.5(8) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N11 C29 C30 107.3(7) . . ? N11 C29 C32 122.5(8) . . ? C30 C29 C32 129.9(8) . . ? C31 C30 C29 110.0(8) . . ? C31 C30 H30 125.0 . . ? C29 C30 H30 125.0 . . ? C30 C31 N12 106.1(7) . . ? C30 C31 C33 132.8(8) . . ? N12 C31 C33 121.0(8) . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N8 C34 N12 111.6(6) . . ? N8 C34 N10 110.8(7) . . ? N12 C34 N10 109.6(6) . . ? N8 C34 H34 108.2 . . ? N12 C34 H34 108.2 . . ? N10 C34 H34 108.2 . . ? C2 C35 H35A 109.5 . . ? C2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O2 C36 C3 107.1(5) . . ? O2 C36 H36A 110.3 . . ? C3 C36 H36A 110.3 . . ? O2 C36 H36B 110.3 . . ? C3 C36 H36B 110.3 . . ? H36A C36 H36B 108.6 . . ? O2 C37 C38 107.7(5) . . ? O2 C37 H37A 110.2 . . ? C38 C37 H37A 110.2 . . ? O2 C37 H37B 110.2 . . ? C38 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? N15 C38 N17 109.0(5) . . ? N15 C38 N13 108.8(6) . . ? N17 C38 N13 107.6(6) . . ? N15 C38 C37 111.7(6) . . ? N17 C38 C37 110.7(6) . . ? N13 C38 C37 108.9(5) . . ? N13 C39 C40 107.1(7) . . ? N13 C39 H39 126.4 . . ? C40 C39 H39 126.4 . . ? C41 C40 C39 105.4(7) . . ? C41 C40 H40 127.3 . . ? C39 C40 H40 127.3 . . ? N14 C41 C40 110.7(7) . . ? N14 C41 H41 124.6 . . ? C40 C41 H41 124.6 . . ? N15 C42 C43 106.9(7) . . ? N15 C42 H42 126.5 . . ? C43 C42 H42 126.5 . . ? C44 C43 C42 105.7(8) . . ? C44 C43 H43 127.1 . . ? C42 C43 H43 127.1 . . ? N16 C44 C43 111.2(7) . . ? N16 C44 H44 124.4 . . ? C43 C44 H44 124.4 . . ? C46 C45 N17 106.1(6) . . ? C46 C45 H45 126.9 . . ? N17 C45 H45 126.9 . . ? C45 C46 C47 107.5(7) . . ? C45 C46 H46 126.2 . . ? C47 C46 H46 126.2 . . ? N18 C47 C46 110.3(7) . . ? N18 C47 H47 124.9 . . ? C46 C47 H47 124.9 . . ? N19 C48 C49 109.9(7) . . ? N19 C48 C51 123.0(7) . . ? C49 C48 C51 127.1(8) . . ? C50 C49 C48 109.8(8) . . ? C50 C49 H49 125.1 . . ? C48 C49 H49 125.1 . . ? C49 C50 N20 104.6(7) . . ? C49 C50 C52 131.8(8) . . ? N20 C50 C52 123.6(7) . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N21 C53 C54 109.9(7) . . ? N21 C53 C56 125.3(7) . . ? C54 C53 C56 124.6(7) . . ? C55 C54 C53 106.5(7) . . ? C55 C54 H54 126.7 . . ? C53 C54 H54 126.7 . . ? N22 C55 C54 105.8(6) . . ? N22 C55 C57 124.3(7) . . ? C54 C55 C57 129.9(7) . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N23 C58 C59 109.1(8) . . ? N23 C58 C61 125.8(8) . . ? C59 C58 C61 125.0(9) . . ? C60 C59 C58 109.5(9) . . ? C60 C59 H59 125.2 . . ? C58 C59 H59 125.2 . . ? C59 C60 N24 103.6(8) . . ? C59 C60 C62 133.1(10) . . ? N24 C60 C62 123.3(10) . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N20 C63 N22 111.7(7) . . ? N20 C63 N24 110.2(6) . . ? N22 C63 N24 111.5(6) . . ? N20 C63 H63 107.8 . . ? N22 C63 H63 107.8 . . ? N24 C63 H63 107.8 . . ? C4 C64 H64A 109.5 . . ? C4 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C4 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O3 C65 C5 109.4(6) . . ? O3 C65 H65A 109.8 . . ? C5 C65 H65A 109.8 . . ? O3 C65 H65B 109.8 . . ? C5 C65 H65B 109.8 . . ? H65A C65 H65B 108.3 . . ? O3 C66 C67 107.8(6) . . ? O3 C66 H66A 110.2 . . ? C67 C66 H66A 110.2 . . ? O3 C66 H66B 110.2 . . ? C67 C66 H66B 110.2 . . ? H66A C66 H66B 108.5 . . ? N25 C67 N27 107.4(6) . . ? N25 C67 N29 108.8(6) . . ? N27 C67 N29 109.0(6) . . ? N25 C67 C66 110.6(6) . . ? N27 C67 C66 111.2(6) . . ? N29 C67 C66 109.7(6) . . ? C69 C68 N25 108.7(7) . . ? C69 C68 H68 125.6 . . ? N25 C68 H68 125.6 . . ? C68 C69 C70 104.8(8) . . ? C68 C69 H69 127.6 . . ? C70 C69 H69 127.6 . . ? N26 C70 C69 108.9(8) . . ? N26 C70 H70 125.6 . . ? C69 C70 H70 125.6 . . ? C72 C71 N27 109.7(7) . . ? C72 C71 H71 125.1 . . ? N27 C71 H71 125.1 . . ? C71 C72 C73 107.1(8) . . ? C71 C72 H72 126.5 . . ? C73 C72 H72 126.4 . . ? N28 C73 C72 109.0(8) . . ? N28 C73 H73 125.5 . . ? C72 C73 H73 125.5 . . ? N29 C74 C75 107.5(7) . . ? N29 C74 H74 126.3 . . ? C75 C74 H74 126.3 . . ? C74 C75 C76 103.9(7) . . ? C74 C75 H75 128.1 . . ? C76 C75 H75 128.1 . . ? N30 C76 C75 112.8(7) . . ? N30 C76 H76 123.6 . . ? C75 C76 H76 123.6 . . ? N31 C77 C78 113.2(9) . . ? N31 C77 C80 121.8(8) . . ? C78 C77 C80 124.5(9) . . ? C79 C78 C77 106.6(9) . . ? C79 C78 H78 126.7 . . ? C77 C78 H78 126.7 . . ? N32 C79 C78 104.4(8) . . ? N32 C79 C81 121.6(9) . . ? C78 C79 C81 133.9(9) . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N33 C82 C83 111.4(9) . . ? N33 C82 C85 123.0(8) . . ? C83 C82 C85 125.6(10) . . ? C84 C83 C82 105.2(9) . . ? C84 C83 H83 127.4 . . ? C82 C83 H83 127.4 . . ? C83 C84 N34 109.2(8) . . ? C83 C84 C86 128.9(9) . . ? N34 C84 C86 121.9(10) . . ? C82 C85 H85A 109.5 . . ? C82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N35 C87 C88 110.9(8) . . ? N35 C87 C90 123.5(8) . . ? C88 C87 C90 125.5(9) . . ? C87 C88 C89 109.1(8) . . ? C87 C88 H88 125.4 . . ? C89 C88 H88 125.4 . . ? C88 C89 N36 104.8(8) . . ? C88 C89 C91 134.1(10) . . ? N36 C89 C91 121.1(10) . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N36 C92 N32 114.0(8) . . ? N36 C92 N34 106.8(7) . . ? N32 C92 N34 109.0(7) . . ? N36 C92 H92 109.0 . . ? N32 C92 H92 109.0 . . ? N34 C92 H92 109.0 . . ? C6 C93 H93A 109.5 . . ? C6 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C6 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C95 C94 C99 119.0(8) . . ? C95 C94 C100 121.5(8) . . ? C99 C94 C100 119.5(8) . . ? C96 C95 C94 120.4(7) . . ? C96 C95 C128 119.2(7) . . ? C94 C95 C128 120.3(8) . . ? C95 C96 C97 119.6(7) . . ? C95 C96 C129 121.4(7) . . ? C97 C96 C129 118.9(7) . . ? C98 C97 C96 120.3(7) . . ? C98 C97 C157 118.6(7) . . ? C96 C97 C157 121.1(7) . . ? C99 C98 C97 120.3(7) . . ? C99 C98 C158 120.2(7) . . ? C97 C98 C158 119.5(8) . . ? C98 C99 C94 120.3(7) . . ? C98 C99 C186 119.6(8) . . ? C94 C99 C186 120.0(8) . . ? O4 C100 C94 107.1(6) . . ? O4 C100 H10A 110.3 . . ? C94 C100 H10A 110.3 . . ? O4 C100 H10B 110.3 . . ? C94 C100 H10B 110.3 . . ? H10A C100 H10B 108.5 . . ? O4 C101 C102 111.3(6) . . ? O4 C101 H10C 109.4 . . ? C102 C101 H10C 109.4 . . ? O4 C101 H10D 109.4 . . ? C102 C101 H10D 109.4 . . ? H10C C101 H10D 108.0 . . ? N39 C102 N37 105.6(6) . . ? N39 C102 N41 108.1(6) . . ? N37 C102 N41 108.8(6) . . ? N39 C102 C101 112.4(6) . . ? N37 C102 C101 111.5(6) . . ? N41 C102 C101 110.2(6) . . ? C104 C103 N37 108.1(7) . . ? C104 C103 H103 126.0 . . ? N37 C103 H103 126.0 . . ? C103 C104 C105 107.9(7) . . ? C103 C104 H104 126.1 . . ? C105 C104 H104 126.1 . . ? N38 C105 C104 108.8(7) . . ? N38 C105 H105 125.6 . . ? C104 C105 H105 125.6 . . ? N39 C106 C107 107.4(7) . . ? N39 C106 H106 126.3 . . ? C107 C106 H106 126.3 . . ? C106 C107 C108 104.3(7) . . ? C106 C107 H107 127.8 . . ? C108 C107 H107 127.8 . . ? N40 C108 C107 112.0(7) . . ? N40 C108 H108 124.0 . . ? C107 C108 H108 124.0 . . ? C110 C109 N41 108.0(7) . . ? C110 C109 H109 126.0 . . ? N41 C109 H109 126.0 . . ? C109 C110 C111 106.4(8) . . ? C109 C110 H110 126.8 . . ? C111 C110 H110 126.8 . . ? N42 C111 C110 111.5(7) . . ? N42 C111 H111 124.2 . . ? C110 C111 H111 124.2 . . ? N43 C112 C113 109.4(7) . . ? N43 C112 C115 126.4(7) . . ? C113 C112 C115 124.0(7) . . ? C112 C113 C114 106.7(7) . . ? C112 C113 H113 126.6 . . ? C114 C113 H113 126.6 . . ? N44 C114 C113 104.2(7) . . ? N44 C114 C116 126.0(8) . . ? C113 C114 C116 129.8(8) . . ? C112 C115 H11A 109.5 . . ? C112 C115 H11B 109.5 . . ? H11A C115 H11B 109.5 . . ? C112 C115 H11C 109.5 . . ? H11A C115 H11C 109.5 . . ? H11B C115 H11C 109.5 . . ? C114 C116 H11D 109.5 . . ? C114 C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? C114 C116 H11F 109.5 . . ? H11D C116 H11F 109.5 . . ? H11E C116 H11F 109.5 . . ? N45 C117 C118 111.3(7) . . ? N45 C117 C120 123.0(7) . . ? C118 C117 C120 125.6(8) . . ? C119 C118 C117 106.5(7) . . ? C119 C118 H118 126.7 . . ? C117 C118 H118 126.7 . . ? N46 C119 C118 106.5(7) . . ? N46 C119 C121 121.8(8) . . ? C118 C119 C121 131.7(8) . . ? C117 C120 H12A 109.5 . . ? C117 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C117 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C119 C121 H12D 109.5 . . ? C119 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C119 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? N47 C122 C123 108.1(7) . . ? N47 C122 C125 125.1(7) . . ? C123 C122 C125 126.6(7) . . ? C124 C123 C122 108.0(7) . . ? C124 C123 H123 126.0 . . ? C122 C123 H123 126.0 . . ? C123 C124 N48 106.6(6) . . ? C123 C124 C126 128.9(7) . . ? N48 C124 C126 124.4(7) . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C124 C126 H12J 109.5 . . ? C124 C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? C124 C126 H12L 109.5 . . ? H12J C126 H12L 109.5 . . ? H12K C126 H12L 109.5 . . ? N46 C127 N48 112.0(5) . . ? N46 C127 N44 108.6(6) . . ? N48 C127 N44 109.6(5) . . ? N46 C127 H127 108.9 . . ? N48 C127 H127 108.9 . . ? N44 C127 H127 108.9 . . ? C95 C128 H12M 109.5 . . ? C95 C128 H12N 109.5 . . ? H12M C128 H12N 109.5 . . ? C95 C128 H12O 109.5 . . ? H12M C128 H12O 109.5 . . ? H12N C128 H12O 109.5 . . ? O5 C129 C96 110.1(6) . . ? O5 C129 H12P 109.6 . . ? C96 C129 H12P 109.6 . . ? O5 C129 H12Q 109.6 . . ? C96 C129 H12Q 109.6 . . ? H12P C129 H12Q 108.2 . . ? O5 C130 C131 107.9(5) . . ? O5 C130 H13A 110.1 . . ? C131 C130 H13A 110.1 . . ? O5 C130 H13B 110.1 . . ? C131 C130 H13B 110.1 . . ? H13A C130 H13B 108.4 . . ? N49 C131 N53 108.7(6) . . ? N49 C131 N51 108.0(5) . . ? N53 C131 N51 108.2(5) . . ? N49 C131 C130 110.2(6) . . ? N53 C131 C130 110.2(5) . . ? N51 C131 C130 111.5(6) . . ? C133 C132 N49 108.1(8) . . ? C133 C132 H132 126.0 . . ? N49 C132 H132 126.0 . . ? C132 C133 C134 106.5(8) . . ? C132 C133 H133 126.7 . . ? C134 C133 H133 126.7 . . ? N50 C134 C133 111.2(8) . . ? N50 C134 H134 124.4 . . ? C133 C134 H134 124.4 . . ? N51 C135 C136 107.4(7) . . ? N51 C135 H135 126.3 . . ? C136 C135 H135 126.3 . . ? C135 C136 C137 108.3(7) . . ? C135 C136 H136 125.8 . . ? C137 C136 H136 125.8 . . ? N52 C137 C136 107.0(7) . . ? N52 C137 H137 126.5 . . ? C136 C137 H137 126.5 . . ? N53 C138 C139 105.7(7) . . ? N53 C138 H138 127.2 . . ? C139 C138 H138 127.2 . . ? C140 C139 C138 106.7(7) . . ? C140 C139 H139 126.7 . . ? C138 C139 H139 126.7 . . ? N54 C140 C139 110.9(7) . . ? N54 C140 H140 124.6 . . ? C139 C140 H140 124.6 . . ? N55 C141 C142 110.5(7) . . ? N55 C141 C144 125.8(8) . . ? C142 C141 C144 123.7(8) . . ? C143 C142 C141 105.4(7) . . ? C143 C142 H142 127.3 . . ? C141 C142 H142 127.3 . . ? C142 C143 N56 106.3(7) . . ? C142 C143 C145 129.4(8) . . ? N56 C143 C145 124.0(8) . . ? C141 C144 H14A 109.5 . . ? C141 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C141 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? C143 C145 H14D 109.5 . . ? C143 C145 H14E 109.5 . . ? H14D C145 H14E 109.5 . . ? C143 C145 H14F 109.5 . . ? H14D C145 H14F 109.5 . . ? H14E C145 H14F 109.5 . . ? N57 C146 C147 110.0(7) . . ? N57 C146 C149 122.7(7) . . ? C147 C146 C149 127.3(7) . . ? C148 C147 C146 106.0(7) . . ? C148 C147 H147 127.0 . . ? C146 C147 H147 127.0 . . ? C147 C148 N58 107.1(7) . . ? C147 C148 C150 131.2(7) . . ? N58 C148 C150 121.7(7) . . ? C146 C149 H14G 109.5 . . ? C146 C149 H14H 109.5 . . ? H14G C149 H14H 109.5 . . ? C146 C149 H14I 109.5 . . ? H14G C149 H14I 109.5 . . ? H14H C149 H14I 109.5 . . ? C148 C150 H15A 109.5 . . ? C148 C150 H15B 109.5 . . ? H15A C150 H15B 109.5 . . ? C148 C150 H15C 109.5 . . ? H15A C150 H15C 109.5 . . ? H15B C150 H15C 109.5 . . ? N59 C151 C152 109.5(7) . . ? N59 C151 C154 123.7(7) . . ? C152 C151 C154 126.7(7) . . ? C153 C152 C151 107.4(7) . . ? C153 C152 H152 126.3 . . ? C151 C152 H152 126.3 . . ? C152 C153 N60 106.1(7) . . ? C152 C153 C155 130.8(7) . . ? N60 C153 C155 123.0(7) . . ? C151 C154 H15D 109.5 . . ? C151 C154 H15E 109.5 . . ? H15D C154 H15E 109.5 . . ? C151 C154 H15F 109.5 . . ? H15D C154 H15F 109.5 . . ? H15E C154 H15F 109.5 . . ? C153 C155 H15G 109.5 . . ? C153 C155 H15H 109.5 . . ? H15G C155 H15H 109.5 . . ? C153 C155 H15I 109.5 . . ? H15G C155 H15I 109.5 . . ? H15H C155 H15I 109.5 . . ? N58 C156 N60 108.5(6) . . ? N58 C156 N56 110.0(6) . . ? N60 C156 N56 110.8(5) . . ? N58 C156 H156 109.2 . . ? N60 C156 H156 109.2 . . ? N56 C156 H156 109.2 . . ? C97 C157 H15J 109.5 . . ? C97 C157 H15K 109.5 . . ? H15J C157 H15K 109.5 . . ? C97 C157 H15L 109.5 . . ? H15J C157 H15L 109.5 . . ? H15K C157 H15L 109.5 . . ? O6 C158 C98 104.9(6) . . ? O6 C158 H15M 110.8 . . ? C98 C158 H15M 110.8 . . ? O6 C158 H15N 110.8 . . ? C98 C158 H15N 110.8 . . ? H15M C158 H15N 108.9 . . ? O6 C159 C160 104.9(6) . . ? O6 C159 H15O 110.8 . . ? C160 C159 H15O 110.8 . . ? O6 C159 H15P 110.8 . . ? C160 C159 H15P 110.8 . . ? H15O C159 H15P 108.9 . . ? N65 C160 N63 109.8(6) . . ? N65 C160 N61 107.1(6) . . ? N63 C160 N61 107.5(6) . . ? N65 C160 C159 111.1(7) . . ? N63 C160 C159 113.3(7) . . ? N61 C160 C159 107.8(6) . . ? N61 C161 C162 104.3(8) . . ? N61 C161 H161 127.8 . . ? C162 C161 H161 127.8 . . ? C163 C162 C161 105.8(8) . . ? C163 C162 H162 127.1 . . ? C161 C162 H162 127.1 . . ? N62 C163 C162 113.1(9) . . ? N62 C163 H163 123.4 . . ? C162 C163 H163 123.4 . . ? N63 C164 C165 107.6(8) . . ? N63 C164 H164 126.2 . . ? C165 C164 H164 126.2 . . ? C166 C165 C164 103.2(9) . . ? C166 C165 H165 128.4 . . ? C164 C165 H165 128.4 . . ? N64 C166 C165 114.6(10) . . ? N64 C166 H166 122.7 . . ? C165 C166 H166 122.7 . . ? C168 C167 N65 109.2(7) . . ? C168 C167 H167 125.4 . . ? N65 C167 H167 125.4 . . ? C167 C168 C169 106.6(8) . . ? C167 C168 H168 126.7 . . ? C169 C168 H168 126.7 . . ? N66 C169 C168 110.2(8) . . ? N66 C169 H169 124.9 . . ? C168 C169 H169 124.9 . . ? N67 C170 C171 108.5(10) . . ? N67 C170 C173 122.8(10) . . ? C171 C170 C173 128.7(10) . . ? C172 C171 C170 110.5(11) . . ? C172 C171 H171 124.8 . . ? C170 C171 H171 124.8 . . ? C171 C172 N68 101.8(10) . . ? C171 C172 C174 131.9(10) . . ? N68 C172 C174 126.2(11) . . ? C170 C173 H17A 109.5 . . ? C170 C173 H17B 109.5 . . ? H17A C173 H17B 109.5 . . ? C170 C173 H17C 109.5 . . ? H17A C173 H17C 109.5 . . ? H17B C173 H17C 109.5 . . ? C172 C174 H17D 109.5 . . ? C172 C174 H17E 109.5 . . ? H17D C174 H17E 109.5 . . ? C172 C174 H17F 109.5 . . ? H17D C174 H17F 109.5 . . ? H17E C174 H17F 109.5 . . ? N69 C175 C176 108.8(8) . . ? N69 C175 C178 127.7(8) . . ? C176 C175 C178 123.2(9) . . ? C177 C176 C175 108.2(9) . . ? C177 C176 H176 125.9 . . ? C175 C176 H176 125.9 . . ? N70 C177 C176 104.5(8) . . ? N70 C177 C179 123.3(9) . . ? C176 C177 C179 132.2(10) . . ? C175 C178 H17G 109.5 . . ? C175 C178 H17H 109.5 . . ? H17G C178 H17H 109.5 . . ? C175 C178 H17I 109.5 . . ? H17G C178 H17I 109.5 . . ? H17H C178 H17I 109.5 . . ? C177 C179 H17J 109.5 . . ? C177 C179 H17K 109.5 . . ? H17J C179 H17K 109.5 . . ? C177 C179 H17L 109.5 . . ? H17J C179 H17L 109.5 . . ? H17K C179 H17L 109.5 . . ? N71 C180 C181 111.2(8) . . ? N71 C180 C183 125.2(8) . . ? C181 C180 C183 123.5(8) . . ? C182 C181 C180 105.1(8) . . ? C182 C181 H181 127.5 . . ? C180 C181 H181 127.5 . . ? C181 C182 N72 109.0(8) . . ? C181 C182 C184 131.5(9) . . ? N72 C182 C184 119.3(9) . . ? C180 C183 H18A 109.5 . . ? C180 C183 H18B 109.5 . . ? H18A C183 H18B 109.5 . . ? C180 C183 H18C 109.5 . . ? H18A C183 H18C 109.5 . . ? H18B C183 H18C 109.5 . . ? C182 C184 H18D 109.5 . . ? C182 C184 H18E 109.5 . . ? H18D C184 H18E 109.5 . . ? C182 C184 H18F 109.5 . . ? H18D C184 H18F 109.5 . . ? H18E C184 H18F 109.5 . . ? N70 C185 N68 109.2(7) . . ? N70 C185 N72 109.6(7) . . ? N68 C185 N72 111.4(7) . . ? N70 C185 H185 108.9 . . ? N68 C185 H185 108.9 . . ? N72 C185 H185 108.9 . . ? C99 C186 H18G 109.5 . . ? C99 C186 H18H 109.5 . . ? H18G C186 H18H 109.5 . . ? C99 C186 H18I 109.5 . . ? H18G C186 H18I 109.5 . . ? H18H C186 H18I 109.5 . . ? 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 Fe1 N7 N8 C34 2.6(9) . . . . ? Fe1 N9 N10 C34 2.2(8) . . . . ? Fe1 N11 N12 C34 1.8(8) . . . . ? Fe1 N2 N1 C9 4.4(8) . . . . ? Fe1 N4 N3 C9 6.3(8) . . . . ? Fe1 N6 N5 C9 2.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.959 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.127 # Attachment '- 5.8MeCN.2tBuOMe SRB Dec1.CIF' #========================================================================== data_5.8MeCN.2tBuOMe _database_code_depnum_ccdc_archive 'CCDC 803930' #TrackingRef '- 5.8MeCN.2tBuOMe SRB Dec1.CIF' #========================================================================== _audit_creation_method SHELXL-97 #========================================================================== _publ_section_table_legends ; ; _chemical_name_systematic ; [{Fe((3,5-Me2pz)3CH)}4(C6H2(CH2OCH2C(pz)3]4)](BF4)8(MeCN)4(CH3OC (CH3)3)2 ; _chemical_name_common ;((Fe((3,5- Me2pz)3CH))4(C6H2(CH2OCH2C(pz)3)4))(BF4)8(MeCN)4(CH3OC (CH3)3)2 ; _chemical_melting_point ? _chemical_formula_moiety ; C118 H142 Fe4 N48 O4, 2(C5 H12 O), 8(C2 H3 N), 8(B F4) ; _chemical_formula_sum 'C144 H190 B8 F32 Fe4 N56 O6' _chemical_formula_weight 3719.40 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3526(9) _cell_length_b 17.5492(12) _cell_length_c 32.453(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.077(2) _cell_angle_gamma 90.00 _cell_volume 8634.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 5519 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 22.78 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3852 _exptl_absorpt_coefficient_mu 0.434 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8456 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _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 53029 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.1109 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19201 _reflns_number_gt 9353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19201 _refine_ls_number_parameters 1128 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.1860 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.3275 _refine_ls_wR_factor_gt 0.2669 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.78170(5) 0.39843(5) 0.06840(3) 0.0296(2) Uani 1 1 d . . . F1 F 0.2122(4) 0.5584(3) 0.16757(15) 0.0742(14) Uani 1 1 d D . . O1 O 0.5365(3) 0.1971(3) 0.03079(13) 0.0381(10) Uani 1 1 d . . . N7 N 0.9042(3) 0.3559(3) 0.07559(15) 0.0325(11) Uani 1 1 d . . . C1 C 0.8960(5) 0.2170(4) 0.0616(3) 0.0522(19) Uani 1 1 d . . . H1A H 0.8329 0.2280 0.0543 0.078 Uiso 1 1 calc R . . H1B H 0.9053 0.1808 0.0849 0.078 Uiso 1 1 calc R . . H1C H 0.9179 0.1949 0.0375 0.078 Uiso 1 1 calc R . . B1 B 0.2059(4) 0.6249(4) 0.1446(2) 0.054(2) Uani 1 1 d D . . Fe2 Fe 0.13170(6) -0.04497(5) 0.17239(3) 0.0370(3) Uani 1 1 d . . . F2 F 0.2876(4) 0.6553(3) 0.1447(2) 0.104(2) Uani 1 1 d D . . O2 O 0.3848(3) 0.0315(3) 0.08886(13) 0.0394(11) Uani 1 1 d . . . N8 N 0.9706(3) 0.4069(3) 0.08860(15) 0.0306(11) Uani 1 1 d . . . C2 C 0.9445(4) 0.2888(4) 0.0741(2) 0.0377(15) Uani 1 1 d . . . B2 B 0.5857(4) 0.7163(4) 0.0973(2) 0.103(4) Uiso 1 1 d D . . F3 F 0.1686(6) 0.6059(4) 0.10517(18) 0.135(3) Uani 1 1 d D . . O3 O 0.8496(6) 0.0329(5) 0.0409(3) 0.115(3) Uiso 1 1 d . . . N9 N 0.8154(3) 0.4596(3) 0.12018(16) 0.0342(12) Uani 1 1 d . . . C3 C 1.0351(4) 0.2974(4) 0.0866(2) 0.0375(15) Uani 1 1 d . . . H3 H 1.0782 0.2582 0.0881 0.045 Uiso 1 1 calc R . . B3 B 0.3258(4) 0.2725(3) 0.09359(19) 0.0445(19) Uani 1 1 d D . . F4 F 0.1549(4) 0.6782(3) 0.1609(2) 0.0951(18) Uani 1 1 d D . . N10 N 0.8950(3) 0.4964(3) 0.12407(16) 0.0335(12) Uani 1 1 d . . . C4 C 1.0505(4) 0.3718(4) 0.09622(19) 0.0326(14) Uani 1 1 d . . . F15 F 0.5998(6) 0.0299(4) 0.1818(3) 0.226(6) Uani 1 1 d D C . F5A F 0.5169(7) 0.7080(9) 0.1164(3) 0.161(7) Uiso 0.520(13) 1 d PD A 1 N11 N 0.8242(3) 0.4831(3) 0.03577(16) 0.0347(12) Uani 1 1 d . . . C5 C 1.1331(4) 0.4147(4) 0.1140(2) 0.0454(17) Uani 1 1 d . . . H5A H 1.1843 0.3809 0.1153 0.068 Uiso 1 1 calc R . . H5B H 1.1282 0.4326 0.1422 0.068 Uiso 1 1 calc R . . H5C H 1.1405 0.4585 0.0962 0.068 Uiso 1 1 calc R . . F6A F 0.6582(7) 0.6711(6) 0.1191(3) 0.112(5) Uiso 0.520(13) 1 d PD A 1 N12 N 0.9047(3) 0.5137(3) 0.05233(16) 0.0321(11) Uani 1 1 d . . . C6 C 0.6954(5) 0.4485(5) 0.1636(2) 0.0535(19) Uani 1 1 d . . . H6A H 0.6636 0.4221 0.1392 0.080 Uiso 1 1 calc R . . H6B H 0.6601 0.4917 0.1708 0.080 Uiso 1 1 calc R . . H6C H 0.7060 0.4132 0.1873 0.080 Uiso 1 1 calc R . . F7A F 0.6230(8) 0.7884(5) 0.0993(3) 0.126(6) Uiso 0.520(13) 1 d PD A 1 N6 N 0.6626(3) 0.4424(3) 0.06201(16) 0.0340(12) Uani 1 1 d . . . C7 C 0.7817(4) 0.4770(4) 0.1539(2) 0.0412(16) Uani 1 1 d . . . N5 N 0.5918(3) 0.3955(3) 0.05302(16) 0.0345(12) Uani 1 1 d . . . C8 C 0.8407(5) 0.5240(4) 0.1798(2) 0.0472(17) Uani 1 1 d . . . H8 H 0.8324 0.5440 0.2062 0.057 Uiso 1 1 calc R . . F8 F 0.5773(4) 0.6890(3) 0.05755(16) 0.0899(16) Uiso 1 1 d D A . N2 N 0.7414(3) 0.3382(3) 0.01803(15) 0.0348(12) Uani 1 1 d . . . C9 C 0.9122(5) 0.5359(4) 0.1603(2) 0.0451(17) Uani 1 1 d . . . F9A F 0.4075(5) 0.2727(14) 0.1149(4) 0.131(9) Uani 0.634(18) 1 d PD B 2 N1 N 0.6596(3) 0.3069(3) 0.01381(15) 0.0335(12) Uani 1 1 d . . . C10 C 0.9954(5) 0.5793(5) 0.1731(3) 0.057(2) Uani 1 1 d . . . H10A H 1.0452 0.5438 0.1781 0.085 Uiso 1 1 calc R . . H10B H 0.9915 0.6077 0.1988 0.085 Uiso 1 1 calc R . . H10C H 1.0042 0.6150 0.1509 0.085 Uiso 1 1 calc R . . F11A F 0.3151(11) 0.3400(5) 0.0744(5) 0.108(5) Uani 0.634(18) 1 d PD B 2 N4 N 0.7399(3) 0.3152(3) 0.09957(15) 0.0317(11) Uani 1 1 d . . . C11 C 0.7138(5) 0.5035(5) -0.0280(2) 0.062(2) Uani 1 1 d . . . H11A H 0.7270 0.4760 -0.0526 0.093 Uiso 1 1 calc R . . H11B H 0.6841 0.5516 -0.0368 0.093 Uiso 1 1 calc R . . H11C H 0.6753 0.4722 -0.0135 0.093 Uiso 1 1 calc R . . F12 F 0.2693(3) 0.2581(3) 0.12062(15) 0.0697(13) Uani 1 1 d D B . N3 N 0.6575(3) 0.2851(3) 0.08574(15) 0.0294(11) Uani 1 1 d . . . C12 C 0.7980(4) 0.5197(4) 0.0008(2) 0.0437(17) Uani 1 1 d . . . F10A F 0.3251(7) 0.2173(4) 0.0644(3) 0.074(4) Uani 0.634(18) 1 d PD B 2 N21 N 0.0500(4) -0.1267(3) 0.14570(18) 0.0449(14) Uani 1 1 d . . . C13 C 0.8616(5) 0.5738(4) -0.0056(2) 0.0490(18) Uani 1 1 d . . . H13 H 0.8585 0.6079 -0.0285 0.059 Uiso 1 1 calc R . . N22 N -0.0161(4) -0.1481(4) 0.16721(18) 0.0473(14) Uani 1 1 d . . . C14 C 0.9277(4) 0.5686(4) 0.0266(2) 0.0397(16) Uani 1 1 d . . . N23 N 0.0260(4) 0.0128(3) 0.18359(17) 0.0436(14) Uani 1 1 d . . . C15 C 1.0134(4) 0.6103(4) 0.0351(3) 0.053(2) Uani 1 1 d . . . H15A H 1.0618 0.5748 0.0330 0.079 Uiso 1 1 calc R . . H15B H 1.0209 0.6320 0.0633 0.079 Uiso 1 1 calc R . . H15C H 1.0137 0.6513 0.0147 0.079 Uiso 1 1 calc R . . N24 N -0.0385(4) -0.0288(3) 0.19710(18) 0.0445(14) Uani 1 1 d . . . C16 C 0.9490(4) 0.4857(3) 0.09158(19) 0.0322(13) Uani 1 1 d . . . H16 H 1.0049 0.5150 0.0994 0.039 Uiso 1 1 calc R . . N19 N 0.1332(3) -0.0990(3) 0.22643(16) 0.0386(12) Uani 1 1 d . . . C23 C 0.6313(4) 0.5114(4) 0.0659(2) 0.0430(16) Uani 1 1 d . . . H23 H 0.6664 0.5559 0.0718 0.052 Uiso 1 1 calc R . . N20 N 0.0514(4) -0.1215(3) 0.23526(18) 0.0433(14) Uani 1 1 d . . . C24 C 0.5381(5) 0.5101(4) 0.0602(3) 0.057(2) Uani 1 1 d . . . H24 H 0.4992 0.5518 0.0614 0.069 Uiso 1 1 calc R . . N14 N 0.2103(4) 0.0328(3) 0.19986(17) 0.0417(13) Uani 1 1 d . . . C25 C 0.5168(4) 0.4359(4) 0.0525(2) 0.0485(18) Uani 1 1 d . . . H25 H 0.4587 0.4157 0.0476 0.058 Uiso 1 1 calc R . . N13 N 0.2798(4) 0.0578(3) 0.18155(17) 0.0391(13) Uani 1 1 d . . . C17 C 0.7701(4) 0.3244(4) -0.0176(2) 0.0428(16) Uani 1 1 d . . . H17 H 0.8263 0.3395 -0.0236 0.051 Uiso 1 1 calc R . . N16 N 0.2358(3) -0.0984(3) 0.16039(16) 0.0370(12) Uani 1 1 d . . . C18 C 0.7080(5) 0.2853(5) -0.0452(2) 0.055(2) Uani 1 1 d . . . H18 H 0.7132 0.2689 -0.0726 0.066 Uiso 1 1 calc R . . N15 N 0.3014(3) -0.0571(3) 0.14661(15) 0.0332(12) Uani 1 1 d . . . C19 C 0.6381(5) 0.2751(4) -0.0250(2) 0.0476(18) Uani 1 1 d . . . H19 H 0.5842 0.2505 -0.0358 0.057 Uiso 1 1 calc R . . N18 N 0.1328(4) 0.0089(3) 0.11968(17) 0.0414(13) Uani 1 1 d . . . C20 C 0.7669(4) 0.2827(4) 0.13579(19) 0.0375(15) Uani 1 1 d . . . H20 H 0.8223 0.2920 0.1527 0.045 Uiso 1 1 calc R . . N17 N 0.2105(4) 0.0390(3) 0.11179(16) 0.0386(13) Uani 1 1 d . . . C21 C 0.7027(4) 0.2323(4) 0.1462(2) 0.0440(16) Uani 1 1 d . . . H21 H 0.7066 0.2017 0.1705 0.053 Uiso 1 1 calc R . . N25 N 0.7621(11) 0.3054(9) 0.2502(5) 0.167(6) Uani 1 1 d . . . C22 C 0.6346(4) 0.2363(4) 0.1145(2) 0.0377(15) Uani 1 1 d . . . H22 H 0.5802 0.2096 0.1127 0.045 Uiso 1 1 calc R . . N26 N 0.9750(6) 0.3449(5) 0.1835(3) 0.089(3) Uani 1 1 d . . . C26 C 0.6078(4) 0.3149(3) 0.04735(18) 0.0303(13) Uani 1 1 d . . . N27 N 0.9073(7) 0.7778(5) 0.0062(3) 0.090(3) Uani 1 1 d . . . C27 C 0.5195(4) 0.2744(4) 0.0368(2) 0.0362(14) Uani 1 1 d . . . H27A H 0.4848 0.2805 0.0599 0.043 Uiso 1 1 calc R . . H27B H 0.4852 0.2963 0.0111 0.043 Uiso 1 1 calc R . . N28 N 0.0014(8) 0.0240(7) 0.2901(3) 0.130(4) Uani 1 1 d . . . C28 C 0.4611(4) 0.1588(4) 0.0085(2) 0.0505(19) Uani 1 1 d . . . H28A H 0.4453 0.1814 -0.0196 0.061 Uiso 1 1 calc R . . H28B H 0.4102 0.1649 0.0235 0.061 Uiso 1 1 calc R . . C29 C 0.4821(4) 0.0764(4) 0.0049(2) 0.0362(15) Uani 1 1 d . . . C30 C 0.1015(5) -0.1704(5) 0.0805(2) 0.060(2) Uani 1 1 d . . . H30A H 0.1315 -0.1210 0.0816 0.091 Uiso 1 1 calc R . . H30B H 0.0666 -0.1778 0.0528 0.091 Uiso 1 1 calc R . . H30C H 0.1454 -0.2112 0.0861 0.091 Uiso 1 1 calc R . . C31 C 0.0427(4) -0.1724(5) 0.1124(2) 0.0483(18) Uani 1 1 d . . . C32 C -0.0291(5) -0.2228(5) 0.1141(3) 0.060(2) Uani 1 1 d . . . H32 H -0.0486 -0.2617 0.0945 0.072 Uiso 1 1 calc R . . C33 C -0.0642(5) -0.2063(5) 0.1480(3) 0.055(2) Uani 1 1 d . . . C34 C -0.1405(6) -0.2420(6) 0.1658(3) 0.081(3) Uani 1 1 d . . . H34A H -0.1670 -0.2825 0.1471 0.121 Uiso 1 1 calc R . . H34B H -0.1849 -0.2029 0.1684 0.121 Uiso 1 1 calc R . . H34C H -0.1187 -0.2635 0.1933 0.121 Uiso 1 1 calc R . . C35 C 0.0496(7) 0.1501(5) 0.1689(3) 0.078(3) Uani 1 1 d . . . H35A H 0.0727 0.1786 0.1943 0.117 Uiso 1 1 calc R . . H35B H 0.0122 0.1836 0.1495 0.117 Uiso 1 1 calc R . . H35C H 0.0988 0.1315 0.1558 0.117 Uiso 1 1 calc R . . C36 C -0.0034(6) 0.0841(5) 0.1800(2) 0.059(2) Uani 1 1 d . . . C37 C -0.0886(6) 0.0879(5) 0.1907(3) 0.070(3) Uani 1 1 d . . . H37 H -0.1241 0.1322 0.1906 0.084 Uiso 1 1 calc R . . C38 C -0.1108(5) 0.0153(5) 0.2012(2) 0.058(2) Uani 1 1 d . . . C39 C -0.1899(6) -0.0174(6) 0.2158(3) 0.079(3) Uani 1 1 d . . . H39A H -0.2156 -0.0570 0.1963 0.119 Uiso 1 1 calc R . . H39B H -0.2335 0.0230 0.2171 0.119 Uiso 1 1 calc R . . H39C H -0.1728 -0.0397 0.2436 0.119 Uiso 1 1 calc R . . C40 C 0.2870(5) -0.1053(5) 0.2638(2) 0.062(2) Uani 1 1 d . . . H40A H 0.3031 -0.0946 0.2364 0.092 Uiso 1 1 calc R . . H40B H 0.3196 -0.1501 0.2760 0.092 Uiso 1 1 calc R . . H40C H 0.3019 -0.0612 0.2822 0.092 Uiso 1 1 calc R . . C41 C 0.1904(5) -0.1204(4) 0.2593(2) 0.0445(17) Uani 1 1 d . . . C42 C 0.1472(5) -0.1569(5) 0.2888(2) 0.059(2) Uani 1 1 d . . . H42 H 0.1741 -0.1777 0.3147 0.070 Uiso 1 1 calc R . . C43 C 0.0585(5) -0.1570(5) 0.2733(2) 0.0531(19) Uani 1 1 d . . . C44 C -0.0200(5) -0.1856(6) 0.2906(3) 0.076(3) Uani 1 1 d . . . H44A H -0.0003 -0.2160 0.3156 0.114 Uiso 1 1 calc R . . H44B H -0.0562 -0.2173 0.2696 0.114 Uiso 1 1 calc R . . H44C H -0.0549 -0.1423 0.2978 0.114 Uiso 1 1 calc R . . C45 C -0.0247(5) -0.1081(4) 0.2048(2) 0.0450(17) Uani 1 1 d . . . H45 H -0.0773 -0.1288 0.2158 0.054 Uiso 1 1 calc R . . C52 C 0.2162(5) 0.0720(4) 0.2349(2) 0.0487(18) Uani 1 1 d . . . H52 H 0.1766 0.0668 0.2544 0.058 Uiso 1 1 calc R . . C53 C 0.2877(6) 0.1221(4) 0.2397(2) 0.056(2) Uani 1 1 d . . . H53 H 0.3053 0.1557 0.2624 0.067 Uiso 1 1 calc R . . C54 C 0.3270(5) 0.1128(4) 0.2053(2) 0.0504(18) Uani 1 1 d . . . H54 H 0.3772 0.1393 0.1989 0.060 Uiso 1 1 calc R . . C46 C 0.2639(4) -0.1696(4) 0.1622(2) 0.0391(15) Uani 1 1 d . . . H46 H 0.2318 -0.2116 0.1707 0.047 Uiso 1 1 calc R . . C47 C 0.3478(5) -0.1755(4) 0.1501(2) 0.0466(17) Uani 1 1 d . . . H47 H 0.3815 -0.2205 0.1485 0.056 Uiso 1 1 calc R . . C48 C 0.3697(4) -0.1044(4) 0.14120(19) 0.0388(15) Uani 1 1 d . . . H48 H 0.4235 -0.0892 0.1326 0.047 Uiso 1 1 calc R . . C49 C 0.0729(5) 0.0315(5) 0.0883(2) 0.0533(19) Uani 1 1 d . . . H49 H 0.0121 0.0185 0.0850 0.064 Uiso 1 1 calc R . . C50 C 0.1105(5) 0.0767(5) 0.0610(3) 0.061(2) Uani 1 1 d . . . H50 H 0.0809 0.1000 0.0362 0.073 Uiso 1 1 calc R . . C51 C 0.1965(5) 0.0813(4) 0.0760(2) 0.0491(18) Uani 1 1 d . . . H51 H 0.2397 0.1087 0.0640 0.059 Uiso 1 1 calc R . . C55 C 0.2912(4) 0.0246(3) 0.14155(19) 0.0349(14) Uani 1 1 d . . . C56 C 0.3715(4) 0.0610(4) 0.12811(19) 0.0405(16) Uani 1 1 d . . . H56A H 0.3632 0.1169 0.1261 0.049 Uiso 1 1 calc R . . H56B H 0.4241 0.0505 0.1492 0.049 Uiso 1 1 calc R . . C57 C 0.4684(5) 0.0556(5) 0.0804(2) 0.0486(18) Uani 1 1 d . . . H57A H 0.5153 0.0356 0.1022 0.058 Uiso 1 1 calc R . . H57B H 0.4715 0.1120 0.0811 0.058 Uiso 1 1 calc R . . C58 C 0.4832(4) 0.0277(4) 0.03857(19) 0.0357(15) Uani 1 1 d . . . C59 C 0.5010(4) -0.0472(4) 0.03277(19) 0.0399(16) Uani 1 1 d . . . H59 H 0.5018 -0.0812 0.0556 0.048 Uiso 1 1 calc R . . C61 C 0.7829(6) -0.0032(5) 0.0615(3) 0.067(2) Uiso 1 1 d . . . C62 C 0.7216(9) 0.0517(8) 0.0799(4) 0.119(4) Uiso 1 1 d . . . H62A H 0.7569 0.0866 0.0993 0.179 Uiso 1 1 calc R . . H62B H 0.6818 0.0226 0.0947 0.179 Uiso 1 1 calc R . . H62C H 0.6869 0.0810 0.0573 0.179 Uiso 1 1 calc R . . C63 C 0.7387(8) -0.0649(7) 0.0330(4) 0.109(4) Uiso 1 1 d . . . H63A H 0.6983 -0.0415 0.0101 0.163 Uiso 1 1 calc R . . H63B H 0.7054 -0.0987 0.0489 0.163 Uiso 1 1 calc R . . H63C H 0.7835 -0.0945 0.0216 0.163 Uiso 1 1 calc R . . C64 C 0.8390(9) -0.0410(7) 0.0955(4) 0.111(4) Uiso 1 1 d . . . H64A H 0.8804 -0.0747 0.0842 0.167 Uiso 1 1 calc R . . H64B H 0.8025 -0.0712 0.1116 0.167 Uiso 1 1 calc R . . H64C H 0.8721 -0.0028 0.1136 0.167 Uiso 1 1 calc R . . C65 C 0.8417(11) 0.1780(9) 0.2856(5) 0.147(6) Uani 1 1 d . . . H65A H 0.8543 0.1858 0.3159 0.221 Uiso 1 1 calc R . . H65B H 0.8969 0.1679 0.2750 0.221 Uiso 1 1 calc R . . H65C H 0.8017 0.1346 0.2793 0.221 Uiso 1 1 calc R . . C66 C 0.7994(9) 0.2482(10) 0.2652(4) 0.108(4) Uani 1 1 d . . . C67 C 0.9707(11) 0.3906(10) 0.2588(4) 0.168(8) Uani 1 1 d . . . H67A H 1.0104 0.3590 0.2784 0.252 Uiso 1 1 calc R . . H67B H 0.9104 0.3860 0.2649 0.252 Uiso 1 1 calc R . . H67C H 0.9895 0.4440 0.2618 0.252 Uiso 1 1 calc R . . C68 C 0.9733(6) 0.3644(6) 0.2150(3) 0.072(3) Uani 1 1 d . . . C69 C 0.7665(7) 0.7299(7) 0.0331(4) 0.110(4) Uani 1 1 d . . . H69A H 0.7852 0.6971 0.0573 0.165 Uiso 1 1 calc R . . H69B H 0.7294 0.7007 0.0113 0.165 Uiso 1 1 calc R . . H69C H 0.7328 0.7731 0.0415 0.165 Uiso 1 1 calc R . . C70 C 0.8414(8) 0.7571(7) 0.0176(3) 0.087(3) Uani 1 1 d . . . C71 C 0.1053(8) 0.0045(9) 0.3600(3) 0.116(4) Uani 1 1 d . . . H71A H 0.0976 -0.0472 0.3702 0.174 Uiso 1 1 calc R . . H71B H 0.0912 0.0416 0.3805 0.174 Uiso 1 1 calc R . . H71C H 0.1665 0.0114 0.3557 0.174 Uiso 1 1 calc R . . C72 C 0.0465(7) 0.0158(7) 0.3205(3) 0.082(3) Uani 1 1 d . . . F9B F 0.3988(11) 0.2312(13) 0.1030(8) 0.104(13) Uani 0.366(18) 1 d PD B 1 F11B F 0.3584(15) 0.3430(8) 0.1005(7) 0.085(6) Uani 0.366(18) 1 d PD B 1 F6B F 0.6659(6) 0.7340(9) 0.1161(4) 0.167(8) Uiso 0.480(13) 1 d PD A 2 F7B F 0.5313(8) 0.7845(5) 0.0947(3) 0.099(5) Uiso 0.480(13) 1 d PD A 2 F5B F 0.5410(8) 0.6673(7) 0.1210(3) 0.121(6) Uiso 0.480(13) 1 d PD A 2 C60 C 0.8032(14) 0.0686(12) 0.0041(7) 0.199(8) Uiso 1 1 d . . . H60A H 0.7396 0.0615 0.0031 0.299 Uiso 1 1 calc R . . H60B H 0.8215 0.0455 -0.0207 0.299 Uiso 1 1 calc R . . H60C H 0.8168 0.1232 0.0047 0.299 Uiso 1 1 calc R . . F10B F 0.2875(16) 0.272(2) 0.0537(4) 0.148(11) Uiso 0.366(18) 1 d PD B 1 F16 F 0.5428(3) 0.1435(2) 0.17324(13) 0.0681(13) Uani 1 1 d D C 1 F13 F 0.6555(4) 0.1208(4) 0.22356(18) 0.113(2) Uani 1 1 d D C . B4 B 0.5803(4) 0.0942(4) 0.2020(2) 0.072(3) Uani 1 1 d D . . F14 F 0.5244(4) 0.0746(6) 0.2274(2) 0.231(7) Uani 1 1 d D C . 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 0.0201(5) 0.0399(5) 0.0293(4) 0.0007(4) 0.0057(3) -0.0031(4) F1 0.097(4) 0.061(3) 0.066(3) 0.004(2) 0.020(3) -0.012(3) O1 0.026(2) 0.051(3) 0.037(2) -0.007(2) 0.0039(19) -0.0108(19) N7 0.029(3) 0.031(3) 0.037(3) 0.001(2) 0.003(2) -0.007(2) C1 0.042(4) 0.039(4) 0.076(5) -0.009(4) 0.010(4) -0.005(3) B1 0.049(6) 0.057(6) 0.056(6) 0.012(4) 0.005(4) -0.007(4) Fe2 0.0343(5) 0.0438(5) 0.0345(5) 0.0050(4) 0.0105(4) 0.0021(4) F2 0.078(4) 0.076(4) 0.157(6) 0.007(4) 0.021(4) -0.019(3) O2 0.040(3) 0.051(3) 0.029(2) -0.0071(19) 0.0113(19) -0.011(2) N8 0.025(3) 0.033(3) 0.034(3) 0.001(2) 0.005(2) -0.004(2) C2 0.034(4) 0.038(4) 0.042(4) 0.005(3) 0.010(3) -0.001(3) F3 0.210(8) 0.115(5) 0.063(4) 0.016(4) -0.032(5) -0.040(5) N9 0.026(3) 0.044(3) 0.033(3) -0.005(2) 0.009(2) -0.005(2) C3 0.032(4) 0.035(3) 0.047(4) 0.009(3) 0.012(3) 0.006(3) B3 0.046(5) 0.041(5) 0.046(5) 0.001(4) 0.006(4) -0.001(4) F4 0.079(4) 0.063(3) 0.144(5) 0.020(3) 0.018(4) -0.010(3) N10 0.024(3) 0.037(3) 0.039(3) -0.006(2) 0.004(2) -0.007(2) C4 0.024(3) 0.041(3) 0.033(3) 0.006(3) 0.005(3) 0.004(3) F15 0.204(11) 0.151(8) 0.294(15) -0.062(9) -0.055(10) 0.091(8) N11 0.025(3) 0.045(3) 0.036(3) 0.004(2) 0.007(2) -0.001(2) C5 0.024(3) 0.055(4) 0.054(4) -0.001(3) -0.002(3) -0.001(3) N12 0.021(3) 0.037(3) 0.041(3) 0.005(2) 0.010(2) -0.002(2) C6 0.041(4) 0.078(5) 0.048(4) -0.012(4) 0.024(3) -0.008(4) N6 0.026(3) 0.035(3) 0.042(3) 0.001(2) 0.006(2) -0.006(2) C7 0.036(4) 0.049(4) 0.040(4) -0.009(3) 0.010(3) -0.001(3) N5 0.017(3) 0.044(3) 0.042(3) -0.002(2) 0.003(2) -0.006(2) C8 0.040(4) 0.056(4) 0.046(4) -0.014(3) 0.010(3) -0.004(3) N2 0.026(3) 0.047(3) 0.032(3) -0.002(2) 0.007(2) -0.008(2) C9 0.038(4) 0.049(4) 0.048(4) -0.008(3) 0.006(3) -0.007(3) F9A 0.038(6) 0.29(3) 0.063(6) -0.032(12) 0.002(5) 0.010(9) N1 0.022(3) 0.049(3) 0.031(3) 0.000(2) 0.008(2) -0.004(2) C10 0.048(5) 0.059(5) 0.063(5) -0.024(4) 0.007(4) -0.017(4) F11A 0.189(13) 0.050(6) 0.098(9) 0.034(6) 0.064(9) 0.050(7) N4 0.021(3) 0.045(3) 0.031(3) -0.007(2) 0.007(2) -0.006(2) C11 0.040(4) 0.094(6) 0.052(5) 0.024(4) 0.005(4) 0.002(4) F12 0.070(3) 0.072(3) 0.076(3) -0.013(2) 0.036(3) -0.013(2) N3 0.017(2) 0.042(3) 0.031(3) -0.006(2) 0.009(2) -0.005(2) C12 0.033(4) 0.056(4) 0.043(4) 0.014(3) 0.011(3) 0.007(3) F10A 0.107(8) 0.049(5) 0.083(7) -0.025(4) 0.069(6) -0.028(5) N21 0.032(3) 0.061(4) 0.045(3) 0.005(3) 0.014(3) -0.001(3) C13 0.036(4) 0.058(4) 0.055(4) 0.025(4) 0.014(3) 0.009(3) N22 0.034(3) 0.062(4) 0.047(3) -0.001(3) 0.012(3) -0.007(3) C14 0.029(4) 0.037(4) 0.056(4) 0.006(3) 0.016(3) 0.002(3) N23 0.046(4) 0.047(3) 0.040(3) 0.011(3) 0.014(3) 0.013(3) C15 0.034(4) 0.051(4) 0.077(5) 0.020(4) 0.018(4) 0.000(3) N24 0.037(3) 0.055(4) 0.043(3) 0.010(3) 0.012(3) 0.014(3) C16 0.020(3) 0.036(3) 0.042(3) -0.003(3) 0.009(3) -0.005(2) N19 0.036(3) 0.046(3) 0.036(3) 0.004(2) 0.009(2) 0.003(2) C23 0.027(4) 0.045(4) 0.057(4) 0.005(3) 0.007(3) -0.001(3) N20 0.031(3) 0.055(4) 0.047(3) 0.012(3) 0.017(3) 0.002(3) C24 0.031(4) 0.053(5) 0.090(6) 0.004(4) 0.015(4) 0.004(3) N14 0.045(3) 0.045(3) 0.039(3) 0.001(2) 0.018(3) -0.005(3) C25 0.021(3) 0.046(4) 0.079(5) 0.005(4) 0.008(3) -0.001(3) N13 0.042(3) 0.040(3) 0.038(3) -0.007(2) 0.015(2) -0.008(2) C17 0.032(4) 0.059(4) 0.040(4) -0.010(3) 0.014(3) -0.011(3) N16 0.032(3) 0.043(3) 0.037(3) 0.001(2) 0.010(2) -0.008(2) C18 0.047(4) 0.079(6) 0.041(4) -0.014(4) 0.016(3) -0.021(4) N15 0.029(3) 0.039(3) 0.033(3) -0.003(2) 0.008(2) -0.001(2) C19 0.043(4) 0.069(5) 0.030(3) -0.005(3) 0.004(3) -0.017(4) N18 0.039(3) 0.050(3) 0.039(3) 0.009(3) 0.017(3) -0.003(3) C20 0.032(4) 0.049(4) 0.031(3) 0.000(3) 0.003(3) -0.007(3) N17 0.040(3) 0.044(3) 0.034(3) 0.006(2) 0.011(2) -0.001(2) C21 0.042(4) 0.055(4) 0.037(4) 0.004(3) 0.010(3) -0.009(3) N25 0.215(16) 0.136(12) 0.134(11) 0.011(9) -0.025(10) 0.001(11) C22 0.037(4) 0.041(4) 0.037(4) -0.001(3) 0.012(3) -0.011(3) N26 0.073(6) 0.099(7) 0.097(7) -0.014(6) 0.018(5) 0.002(5) C26 0.021(3) 0.041(3) 0.031(3) -0.007(3) 0.008(2) -0.008(2) N27 0.114(8) 0.079(6) 0.076(6) 0.006(4) 0.009(5) 0.009(5) C27 0.025(3) 0.044(4) 0.041(4) -0.002(3) 0.009(3) -0.006(3) N28 0.142(10) 0.171(11) 0.066(6) -0.019(6) -0.017(6) 0.058(8) C28 0.028(4) 0.062(5) 0.059(5) -0.017(4) -0.004(3) -0.007(3) C29 0.020(3) 0.048(4) 0.039(4) -0.006(3) 0.003(3) -0.011(3) C30 0.059(5) 0.073(6) 0.051(5) -0.016(4) 0.013(4) -0.005(4) C31 0.030(4) 0.070(5) 0.045(4) -0.009(4) 0.003(3) 0.000(3) C32 0.053(5) 0.068(5) 0.060(5) -0.011(4) 0.006(4) -0.009(4) C33 0.032(4) 0.071(5) 0.065(5) -0.001(4) 0.010(4) -0.004(4) C34 0.053(5) 0.096(7) 0.097(7) -0.002(6) 0.024(5) -0.015(5) C35 0.104(7) 0.057(5) 0.081(6) 0.023(5) 0.039(6) 0.029(5) C36 0.073(6) 0.059(5) 0.048(4) 0.016(4) 0.019(4) 0.025(4) C37 0.076(6) 0.075(6) 0.064(5) 0.017(4) 0.026(5) 0.038(5) C38 0.049(5) 0.075(6) 0.052(5) 0.004(4) 0.013(4) 0.024(4) C39 0.051(5) 0.119(8) 0.074(6) 0.015(6) 0.027(5) 0.029(5) C40 0.045(5) 0.092(6) 0.049(5) 0.005(4) 0.008(4) 0.002(4) C41 0.037(4) 0.055(4) 0.043(4) 0.010(3) 0.011(3) 0.011(3) C42 0.064(5) 0.066(5) 0.048(4) 0.024(4) 0.014(4) 0.014(4) C43 0.048(5) 0.064(5) 0.049(4) 0.021(4) 0.013(4) 0.004(4) C44 0.057(5) 0.100(7) 0.077(6) 0.046(5) 0.027(5) 0.006(5) C45 0.034(4) 0.056(4) 0.048(4) 0.004(3) 0.013(3) 0.006(3) C52 0.064(5) 0.048(4) 0.038(4) -0.001(3) 0.020(3) 0.003(4) C53 0.076(6) 0.051(4) 0.045(4) -0.016(3) 0.023(4) -0.011(4) C54 0.059(5) 0.051(4) 0.043(4) -0.008(3) 0.015(4) -0.011(4) C46 0.037(4) 0.036(4) 0.045(4) 0.000(3) 0.009(3) -0.004(3) C47 0.046(4) 0.047(4) 0.047(4) -0.003(3) 0.007(3) 0.004(3) C48 0.034(4) 0.051(4) 0.031(3) -0.006(3) 0.005(3) -0.004(3) C49 0.043(4) 0.076(5) 0.043(4) 0.015(4) 0.013(3) 0.003(4) C50 0.052(5) 0.073(6) 0.055(5) 0.024(4) 0.003(4) 0.012(4) C51 0.054(5) 0.054(4) 0.041(4) 0.014(3) 0.011(3) 0.001(3) C55 0.038(4) 0.038(3) 0.031(3) 0.002(3) 0.011(3) -0.005(3) C56 0.044(4) 0.049(4) 0.030(3) -0.001(3) 0.010(3) -0.009(3) C57 0.038(4) 0.071(5) 0.039(4) -0.011(3) 0.014(3) -0.018(4) C58 0.026(3) 0.049(4) 0.032(3) -0.008(3) 0.007(3) -0.013(3) C59 0.036(4) 0.056(4) 0.028(3) -0.001(3) 0.005(3) -0.016(3) C65 0.178(16) 0.127(12) 0.137(13) 0.007(10) 0.024(11) 0.042(11) C66 0.110(10) 0.147(13) 0.069(8) -0.024(8) 0.015(7) 0.002(9) C67 0.161(14) 0.212(18) 0.111(11) -0.075(12) -0.041(10) 0.058(13) C68 0.066(6) 0.084(7) 0.061(6) -0.011(5) -0.008(5) 0.002(5) C69 0.083(8) 0.115(10) 0.136(11) 0.008(8) 0.029(8) 0.001(7) C70 0.079(8) 0.104(8) 0.079(7) 0.024(6) 0.019(6) 0.005(6) C71 0.102(9) 0.176(13) 0.066(7) 0.014(8) 0.001(6) -0.028(9) C72 0.061(6) 0.118(9) 0.069(6) -0.015(6) 0.017(5) -0.006(6) F9B 0.12(2) 0.091(14) 0.13(2) 0.067(15) 0.094(19) 0.065(13) F11B 0.106(16) 0.084(12) 0.067(12) 0.018(9) 0.024(11) -0.026(11) F16 0.077(3) 0.065(3) 0.056(3) 0.016(2) -0.008(2) -0.018(2) F13 0.100(5) 0.125(5) 0.098(4) 0.044(4) -0.038(4) -0.012(4) B4 0.038(5) 0.095(8) 0.077(7) 0.037(6) -0.002(5) 0.001(5) F14 0.091(5) 0.444(18) 0.164(8) 0.206(11) 0.037(5) 0.024(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 1.942(5) . ? Fe1 N2 1.963(5) . ? Fe1 N6 1.966(5) . ? Fe1 N9 1.993(5) . ? Fe1 N11 1.993(5) . ? Fe1 N7 2.002(5) . ? F1 B1 1.380(6) . ? O1 C27 1.401(8) . ? O1 C28 1.431(7) . ? N7 C2 1.336(8) . ? N7 N8 1.373(6) . ? C1 C2 1.486(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? B1 F3 1.358(6) . ? B1 F2 1.362(6) . ? B1 F4 1.379(6) . ? Fe2 N14 1.943(6) . ? Fe2 N16 1.945(5) . ? Fe2 N18 1.957(5) . ? Fe2 N19 1.991(5) . ? Fe2 N23 1.995(6) . ? Fe2 N21 2.009(6) . ? O2 C57 1.418(8) . ? O2 C56 1.419(7) . ? N8 C4 1.359(7) . ? N8 C16 1.428(8) . ? C2 C3 1.395(9) . ? B2 F5A 1.315(8) . ? B2 F6B 1.322(8) . ? B2 F8 1.364(7) . ? B2 F7A 1.386(8) . ? B2 F5B 1.402(8) . ? B2 F7B 1.454(8) . ? B2 F6A 1.456(8) . ? O3 C60 1.44(2) . ? O3 C61 1.452(12) . ? N9 C7 1.319(8) . ? N9 N10 1.370(7) . ? C3 C4 1.355(9) . ? C3 H3 0.9500 . ? B3 F9B 1.328(8) . ? B3 F9A 1.333(7) . ? B3 F10B 1.336(8) . ? B3 F11A 1.337(7) . ? B3 F11B 1.341(8) . ? B3 F12 1.351(6) . ? B3 F10A 1.354(6) . ? N10 C9 1.355(8) . ? N10 C16 1.452(8) . ? C4 C5 1.511(9) . ? F15 B4 1.361(7) . ? N11 C12 1.312(8) . ? N11 N12 1.376(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N12 C14 1.357(8) . ? N12 C16 1.433(8) . ? C6 C7 1.495(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N6 C23 1.316(8) . ? N6 N5 1.359(7) . ? C7 C8 1.403(9) . ? N5 C25 1.349(8) . ? N5 C26 1.452(8) . ? C8 C9 1.368(10) . ? C8 H8 0.9500 . ? N2 C17 1.324(8) . ? N2 N1 1.358(7) . ? C9 C10 1.488(9) . ? N1 C19 1.370(8) . ? N1 C26 1.453(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N4 C20 1.314(8) . ? N4 N3 1.379(6) . ? C11 C12 1.498(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N3 C22 1.354(8) . ? N3 C26 1.452(8) . ? C12 C13 1.400(10) . ? N21 C31 1.336(9) . ? N21 N22 1.373(8) . ? N21 Fe2 2.009(6) 1 ? C13 C14 1.341(10) . ? C13 H13 0.9500 . ? N22 C33 1.353(9) . ? N22 C45 1.433(9) . ? C14 C15 1.492(9) . ? N23 C36 1.330(9) . ? N23 N24 1.359(8) . ? N23 Fe2 1.995(6) 1 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N24 C38 1.378(9) . ? N24 C45 1.423(9) . ? C16 H16 1.0000 . ? N19 C41 1.325(8) . ? N19 N20 1.389(7) . ? N19 Fe2 1.991(5) 1 ? C23 C24 1.413(10) . ? C23 H23 0.9500 . ? N20 C43 1.370(9) . ? N20 C45 1.426(9) . ? C24 C25 1.356(10) . ? C24 H24 0.9500 . ? N14 C52 1.319(8) . ? N14 N13 1.373(7) . ? N14 Fe2 1.943(6) 1 ? C25 H25 0.9500 . ? N13 C54 1.368(9) . ? N13 C55 1.458(8) . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? N16 C46 1.321(8) . ? N16 N15 1.373(7) . ? N16 Fe2 1.945(5) 1 ? C18 C19 1.353(10) . ? C18 H18 0.9500 . ? N15 C48 1.369(8) . ? N15 C55 1.450(8) . ? C19 H19 0.9500 . ? N18 C49 1.320(9) . ? N18 N17 1.366(7) . ? N18 Fe2 1.957(5) 1 ? C20 C21 1.403(9) . ? C20 H20 0.9500 . ? N17 C51 1.368(8) . ? N17 C55 1.467(8) . ? C21 C22 1.348(9) . ? C21 H21 0.9500 . ? N25 C66 1.219(17) . ? C22 H22 0.9500 . ? N26 C68 1.082(11) . ? C26 C27 1.522(8) . ? N27 C70 1.188(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N28 C72 1.123(12) . ? C28 C29 1.491(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C58 1.384(9) . ? C29 C59 1.388(9) 3_655 ? C30 C31 1.476(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.422(11) . ? C32 C33 1.329(11) . ? C32 H32 0.9500 . ? C33 C34 1.521(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.491(12) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.406(12) . ? C37 C38 1.375(12) . ? C37 H37 0.9500 . ? C38 C39 1.486(12) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.491(10) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.403(10) . ? C42 C43 1.374(11) . ? C42 H42 0.9500 . ? C43 C44 1.495(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45 1.0000 . ? C52 C53 1.395(11) . ? C52 H52 0.9500 . ? C53 C54 1.362(10) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C46 C47 1.408(10) . ? C46 H46 0.9500 . ? C47 C48 1.336(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.384(10) . ? C49 H49 0.9500 . ? C50 C51 1.335(10) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C55 C56 1.512(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.495(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.361(9) . ? C59 C29 1.388(9) 3_655 ? C59 H59 0.9500 . ? C61 C64 1.450(14) . ? C61 C63 1.513(14) . ? C61 C62 1.534(15) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.50(2) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C67 C68 1.502(16) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C69 C70 1.408(15) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C71 C72 1.459(15) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? F16 B4 1.334(6) . ? F13 B4 1.337(6) . ? B4 F14 1.325(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N2 86.7(2) . . ? N4 Fe1 N6 88.4(2) . . ? N2 Fe1 N6 87.6(2) . . ? N4 Fe1 N9 91.7(2) . . ? N2 Fe1 N9 176.7(2) . . ? N6 Fe1 N9 89.5(2) . . ? N4 Fe1 N11 179.3(2) . . ? N2 Fe1 N11 92.6(2) . . ? N6 Fe1 N11 91.6(2) . . ? N9 Fe1 N11 89.0(2) . . ? N4 Fe1 N7 92.3(2) . . ? N2 Fe1 N7 93.6(2) . . ? N6 Fe1 N7 178.6(2) . . ? N9 Fe1 N7 89.3(2) . . ? N11 Fe1 N7 87.7(2) . . ? C27 O1 C28 111.7(5) . . ? C2 N7 N8 105.0(5) . . ? C2 N7 Fe1 139.2(4) . . ? N8 N7 Fe1 115.6(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? F3 B1 F2 110.5(7) . . ? F3 B1 F4 110.3(7) . . ? F2 B1 F4 108.2(6) . . ? F3 B1 F1 106.5(6) . . ? F2 B1 F1 110.1(6) . . ? F4 B1 F1 111.2(5) . . ? Fe2 Fe2 N14 0(10) 1 . ? Fe2 Fe2 N16 0(10) 1 . ? N14 Fe2 N16 87.7(2) . . ? Fe2 Fe2 N18 0(10) 1 . ? N14 Fe2 N18 88.4(2) . . ? N16 Fe2 N18 86.4(2) . . ? Fe2 Fe2 N19 0(10) 1 . ? N14 Fe2 N19 90.6(2) . . ? N16 Fe2 N19 92.9(2) . . ? N18 Fe2 N19 178.8(2) . . ? Fe2 Fe2 N23 0(10) 1 . ? N14 Fe2 N23 91.3(2) . . ? N16 Fe2 N23 178.1(2) . . ? N18 Fe2 N23 91.9(2) . . ? N19 Fe2 N23 88.8(2) . . ? Fe2 Fe2 N21 0(10) 1 . ? N14 Fe2 N21 178.3(2) . . ? N16 Fe2 N21 92.6(2) . . ? N18 Fe2 N21 93.4(2) . . ? N19 Fe2 N21 87.7(2) . . ? N23 Fe2 N21 88.4(2) . . ? C57 O2 C56 109.1(5) . . ? C4 N8 N7 111.4(5) . . ? C4 N8 C16 129.8(5) . . ? N7 N8 C16 118.8(5) . . ? N7 C2 C3 109.9(5) . . ? N7 C2 C1 122.8(6) . . ? C3 C2 C1 127.2(6) . . ? F5A B2 F6B 124.6(9) . . ? F5A B2 F8 116.4(6) . . ? F6B B2 F8 117.4(6) . . ? F5A B2 F7A 115.9(6) . . ? F6B B2 F7A 54.3(7) . . ? F8 B2 F7A 109.9(5) . . ? F6B B2 F5B 113.1(6) . . ? F8 B2 F5B 108.7(5) . . ? F7A B2 F5B 140.3(7) . . ? F5A B2 F7B 67.9(7) . . ? F6B B2 F7B 108.5(6) . . ? F8 B2 F7B 105.5(5) . . ? F7A B2 F7B 58.7(6) . . ? F5B B2 F7B 102.2(5) . . ? F5A B2 F6A 108.6(6) . . ? F6B B2 F6A 47.0(6) . . ? F8 B2 F6A 102.6(5) . . ? F7A B2 F6A 101.3(5) . . ? F5B B2 F6A 78.6(7) . . ? F7B B2 F6A 149.8(7) . . ? C60 O3 C61 106.3(11) . . ? C7 N9 N10 106.0(5) . . ? C7 N9 Fe1 137.8(4) . . ? N10 N9 Fe1 116.2(4) . . ? C4 C3 C2 107.5(6) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? F9B B3 F10B 116.5(16) . . ? F9A B3 F10B 137.5(13) . . ? F9B B3 F11A 128.9(12) . . ? F9A B3 F11A 106.0(12) . . ? F10B B3 F11A 63.2(13) . . ? F9B B3 F11B 100.8(14) . . ? F9A B3 F11B 67.4(11) . . ? F10B B3 F11B 105.1(15) . . ? F9B B3 F12 110.7(9) . . ? F9A B3 F12 108.2(8) . . ? F10B B3 F12 113.5(12) . . ? F11A B3 F12 115.1(7) . . ? F11B B3 F12 109.0(9) . . ? F9B B3 F10A 71.5(12) . . ? F9A B3 F10A 105.5(9) . . ? F10B B3 F10A 50.6(13) . . ? F11A B3 F10A 108.7(8) . . ? F11B B3 F10A 137.6(9) . . ? F12 B3 F10A 112.7(5) . . ? C9 N10 N9 111.7(5) . . ? C9 N10 C16 129.9(5) . . ? N9 N10 C16 118.3(5) . . ? C3 C4 N8 106.1(5) . . ? C3 C4 C5 132.4(6) . . ? N8 C4 C5 121.5(6) . . ? C12 N11 N12 106.3(5) . . ? C12 N11 Fe1 138.0(5) . . ? N12 N11 Fe1 115.6(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 N12 N11 110.0(5) . . ? C14 N12 C16 131.1(5) . . ? N11 N12 C16 118.9(5) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C23 N6 N5 106.7(5) . . ? C23 N6 Fe1 134.3(4) . . ? N5 N6 Fe1 118.9(4) . . ? N9 C7 C8 109.4(6) . . ? N9 C7 C6 125.1(6) . . ? C8 C7 C6 125.4(6) . . ? C25 N5 N6 109.6(5) . . ? C25 N5 C26 132.2(5) . . ? N6 N5 C26 118.2(5) . . ? C9 C8 C7 107.5(6) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C17 N2 N1 105.5(5) . . ? C17 N2 Fe1 136.2(4) . . ? N1 N2 Fe1 117.8(4) . . ? N10 C9 C8 105.3(6) . . ? N10 C9 C10 123.1(6) . . ? C8 C9 C10 131.6(7) . . ? N2 N1 C19 110.0(5) . . ? N2 N1 C26 119.5(5) . . ? C19 N1 C26 130.4(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C20 N4 N3 105.6(5) . . ? C20 N4 Fe1 135.2(4) . . ? N3 N4 Fe1 118.7(4) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C22 N3 N4 110.1(5) . . ? C22 N3 C26 131.4(5) . . ? N4 N3 C26 118.2(5) . . ? N11 C12 C13 109.5(6) . . ? N11 C12 C11 124.4(6) . . ? C13 C12 C11 126.1(6) . . ? C31 N21 N22 105.8(6) . . ? C31 N21 Fe2 138.1(5) . 1 ? N22 N21 Fe2 116.0(4) . 1 ? C31 N21 Fe2 138.1(5) . . ? N22 N21 Fe2 116.0(4) . . ? C14 C13 C12 107.4(6) . . ? C14 C13 H13 126.3 . . ? C12 C13 H13 126.3 . . ? C33 N22 N21 111.4(6) . . ? C33 N22 C45 130.3(6) . . ? N21 N22 C45 118.3(6) . . ? C13 C14 N12 106.8(6) . . ? C13 C14 C15 130.4(6) . . ? N12 C14 C15 122.8(6) . . ? C36 N23 N24 106.2(6) . . ? C36 N23 Fe2 137.5(5) . 1 ? N24 N23 Fe2 116.2(4) . 1 ? C36 N23 Fe2 137.5(5) . . ? N24 N23 Fe2 116.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N23 N24 C38 111.6(6) . . ? N23 N24 C45 119.1(5) . . ? C38 N24 C45 129.2(7) . . ? N8 C16 N12 110.8(5) . . ? N8 C16 N10 109.9(5) . . ? N12 C16 N10 110.9(5) . . ? N8 C16 H16 108.4 . . ? N12 C16 H16 108.4 . . ? N10 C16 H16 108.4 . . ? C41 N19 N20 105.1(5) . . ? C41 N19 Fe2 139.3(5) . 1 ? N20 N19 Fe2 115.6(4) . 1 ? C41 N19 Fe2 139.3(5) . . ? N20 N19 Fe2 115.6(4) . . ? N6 C23 C24 110.4(6) . . ? N6 C23 H23 124.8 . . ? C24 C23 H23 124.8 . . ? C43 N20 N19 111.6(5) . . ? C43 N20 C45 129.7(6) . . ? N19 N20 C45 118.6(5) . . ? C25 C24 C23 104.5(6) . . ? C25 C24 H24 127.7 . . ? C23 C24 H24 127.7 . . ? C52 N14 N13 104.7(5) . . ? C52 N14 Fe2 135.7(5) . 1 ? N13 N14 Fe2 119.6(4) . 1 ? C52 N14 Fe2 135.7(5) . . ? N13 N14 Fe2 119.6(4) . . ? N5 C25 C24 108.7(6) . . ? N5 C25 H25 125.6 . . ? C24 C25 H25 125.6 . . ? C54 N13 N14 111.1(5) . . ? C54 N13 C55 130.9(6) . . ? N14 N13 C55 117.9(5) . . ? N2 C17 C18 111.4(6) . . ? N2 C17 H17 124.3 . . ? C18 C17 H17 124.3 . . ? C46 N16 N15 105.2(5) . . ? C46 N16 Fe2 136.1(4) . 1 ? N15 N16 Fe2 118.6(4) . 1 ? C46 N16 Fe2 136.1(4) . . ? N15 N16 Fe2 118.6(4) . . ? C19 C18 C17 105.8(6) . . ? C19 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? C48 N15 N16 109.7(5) . . ? C48 N15 C55 131.1(5) . . ? N16 N15 C55 119.2(5) . . ? C18 C19 N1 107.3(6) . . ? C18 C19 H19 126.4 . . ? N1 C19 H19 126.4 . . ? C49 N18 N17 105.2(5) . . ? C49 N18 Fe2 135.9(5) . 1 ? N17 N18 Fe2 118.6(4) . 1 ? C49 N18 Fe2 135.9(5) . . ? N17 N18 Fe2 118.6(4) . . ? N4 C20 C21 110.7(6) . . ? N4 C20 H20 124.6 . . ? C21 C20 H20 124.6 . . ? N18 N17 C51 110.1(5) . . ? N18 N17 C55 118.8(5) . . ? C51 N17 C55 131.0(6) . . ? C22 C21 C20 106.0(6) . . ? C22 C21 H21 127.0 . . ? C20 C21 H21 127.0 . . ? C21 C22 N3 107.6(6) . . ? C21 C22 H22 126.2 . . ? N3 C22 H22 126.2 . . ? N3 C26 N5 108.6(5) . . ? N3 C26 N1 109.4(5) . . ? N5 C26 N1 108.3(5) . . ? N3 C26 C27 110.7(5) . . ? N5 C26 C27 108.7(5) . . ? N1 C26 C27 111.1(5) . . ? O1 C27 C26 107.7(5) . . ? O1 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O1 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O1 C28 C29 109.1(5) . . ? O1 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O1 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C58 C29 C59 119.1(6) . 3_655 ? C58 C29 C28 120.9(6) . . ? C59 C29 C28 120.0(6) 3_655 . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N21 C31 C32 108.0(7) . . ? N21 C31 C30 124.7(7) . . ? C32 C31 C30 127.3(7) . . ? C33 C32 C31 108.3(7) . . ? C33 C32 H32 125.8 . . ? C31 C32 H32 125.8 . . ? C32 C33 N22 106.5(7) . . ? C32 C33 C34 131.4(8) . . ? N22 C33 C34 122.1(8) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N23 C36 C37 109.8(7) . . ? N23 C36 C35 124.1(7) . . ? C37 C36 C35 126.0(8) . . ? C38 C37 C36 107.1(7) . . ? C38 C37 H37 126.4 . . ? C36 C37 H37 126.4 . . ? C37 C38 N24 105.2(7) . . ? C37 C38 C39 133.2(8) . . ? N24 C38 C39 121.6(8) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N19 C41 C42 110.7(6) . . ? N19 C41 C40 123.5(6) . . ? C42 C41 C40 125.8(7) . . ? C43 C42 C41 107.4(6) . . ? C43 C42 H42 126.3 . . ? C41 C42 H42 126.3 . . ? N20 C43 C42 105.3(6) . . ? N20 C43 C44 122.4(7) . . ? C42 C43 C44 132.3(7) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N24 C45 N20 111.5(6) . . ? N24 C45 N22 111.1(6) . . ? N20 C45 N22 109.5(6) . . ? N24 C45 H45 108.2 . . ? N20 C45 H45 108.2 . . ? N22 C45 H45 108.2 . . ? N14 C52 C53 111.9(7) . . ? N14 C52 H52 124.1 . . ? C53 C52 H52 124.1 . . ? C54 C53 C52 105.9(6) . . ? C54 C53 H53 127.0 . . ? C52 C53 H53 127.0 . . ? C53 C54 N13 106.4(7) . . ? C53 C54 H54 126.8 . . ? N13 C54 H54 126.8 . . ? N16 C46 C47 111.3(6) . . ? N16 C46 H46 124.3 . . ? C47 C46 H46 124.3 . . ? C48 C47 C46 105.4(6) . . ? C48 C47 H47 127.3 . . ? C46 C47 H47 127.3 . . ? C47 C48 N15 108.3(6) . . ? C47 C48 H48 125.8 . . ? N15 C48 H48 125.8 . . ? N18 C49 C50 110.9(7) . . ? N18 C49 H49 124.6 . . ? C50 C49 H49 124.6 . . ? C51 C50 C49 106.8(7) . . ? C51 C50 H50 126.6 . . ? C49 C50 H50 126.6 . . ? C50 C51 N17 106.9(7) . . ? C50 C51 H51 126.5 . . ? N17 C51 H51 126.5 . . ? N15 C55 N13 108.7(5) . . ? N15 C55 N17 108.1(5) . . ? N13 C55 N17 108.1(5) . . ? N15 C55 C56 111.7(5) . . ? N13 C55 C56 107.8(5) . . ? N17 C55 C56 112.3(5) . . ? O2 C56 C55 110.2(5) . . ? O2 C56 H56A 109.6 . . ? C55 C56 H56A 109.6 . . ? O2 C56 H56B 109.6 . . ? C55 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? O2 C57 C58 110.4(5) . . ? O2 C57 H57A 109.6 . . ? C58 C57 H57A 109.6 . . ? O2 C57 H57B 109.6 . . ? C58 C57 H57B 109.6 . . ? H57A C57 H57B 108.1 . . ? C59 C58 C29 117.7(6) . . ? C59 C58 C57 120.3(6) . . ? C29 C58 C57 122.0(6) . . ? C58 C59 C29 123.2(6) . 3_655 ? C58 C59 H59 118.4 . . ? C29 C59 H59 118.4 3_655 . ? C64 C61 O3 100.0(8) . . ? C64 C61 C63 107.0(9) . . ? O3 C61 C63 108.3(9) . . ? C64 C61 C62 108.6(9) . . ? O3 C61 C62 115.1(9) . . ? C63 C61 C62 116.3(9) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N25 C66 C65 176.6(16) . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N26 C68 C67 179.4(15) . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N27 C70 C69 176.4(12) . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N28 C72 C71 179.5(15) . . ? O3 C60 H60A 109.5 . . ? O3 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O3 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? F14 B4 F16 110.6(5) . . ? F14 B4 F13 110.8(6) . . ? F16 B4 F13 112.4(5) . . ? F14 B4 F15 107.4(6) . . ? F16 B4 F15 107.7(6) . . ? F13 B4 F15 107.7(6) . . ? 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 Fe1 N7 N8 C16 -6.5(6) . . . . ? Fe1 N9 N10 C16 -2.3(7) . . . . ? Fe1 N11 N12 C16 -2.6(7) . . . . ? Fe1 N2 N1 C26 -3.8(7) . . . . ? Fe1 N4 N3 C26 2.9(6) . . . . ? Fe1 N6 N5 C26 -1.8(7) . . . . ? Fe2 N19 N20 C45 3.0(7) . . . . ? Fe2 N21 N22 C45 3.7(8) . . . . ? Fe2 N23 N24 C45 4.0(8) . . . . ? Fe2 N14 N13 C55 0.5(7) . . . . ? Fe2 N16 N15 C55 0.1(7) . . . . ? Fe2 N18 N17 C55 4.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.601 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.116