# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kehr, Gerald' 'Erker, G' 'Frohlich, Roland' 'Unverhau, Kerstin' _publ_contact_author_name 'Dr Gerald Kehr' _publ_contact_author_email erker@uni-muenster.de _publ_section_title ; Synthesis of [3]Ferrocenophane-bridged Cp/amido Zirconium Complexes and ansa-Zirconocenes and their Use in Polymerisation Catalysis ; # Attachment '10b.cif' data_erk5236 _database_code_depnum_ccdc_archive 'CCDC 806922' #TrackingRef '10b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H39 Fe N3 Zr' _chemical_formula_weight 600.72 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 9.2847(2) _cell_length_b 10.1003(2) _cell_length_c 15.4314(4) _cell_angle_alpha 93.503(1) _cell_angle_beta 103.467(1) _cell_angle_gamma 100.702(1) _cell_volume 1374.59(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3191 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7364 _exptl_absorpt_correction_T_max 0.9126 _exptl_absorpt_process_details 'Denzo (Otwinwoski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12144 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 28.13 _reflns_number_total 6479 _reflns_number_gt 5930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0379P)^2^+2.4054P] 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 6479 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Zr Zr 0.46832(3) 0.36440(3) 0.211556(17) 0.03037(8) Uani 1 1 d . . . Fe Fe 0.93374(5) 0.73687(4) 0.30705(3) 0.03605(11) Uani 1 1 d . . . N1 N 0.7011(2) 0.4465(2) 0.23597(14) 0.0282(4) Uani 1 1 d . . . C1 C 0.8784(4) 0.8231(3) 0.41243(19) 0.0448(7) Uani 1 1 d . . . C2 C 1.0019(4) 0.9121(4) 0.3913(2) 0.0530(9) Uani 1 1 d . . . H2 H 1.0016 1.0007 0.3758 0.064 Uiso 1 1 calc R . . C3 C 1.1247(4) 0.8446(4) 0.3975(2) 0.0589(10) Uani 1 1 d . . . H3 H 1.2186 0.8799 0.3860 0.071 Uiso 1 1 calc R . . C4 C 1.0805(4) 0.7148(4) 0.4243(2) 0.0543(9) Uani 1 1 d . . . H4 H 1.1402 0.6488 0.4336 0.065 Uiso 1 1 calc R . . C5 C 0.9301(4) 0.7011(4) 0.43452(19) 0.0462(7) Uani 1 1 d . . . H5 H 0.8742 0.6251 0.4527 0.055 Uiso 1 1 calc R . . C6 C 0.7208(4) 0.8453(3) 0.4058(2) 0.0477(8) Uani 1 1 d . . . H6 H 0.7056 0.8443 0.4672 0.057 Uiso 1 1 calc R . . C7 C 0.7008(5) 0.9845(4) 0.3773(3) 0.0615(10) Uani 1 1 d . . . H7A H 0.7722 1.0546 0.4200 0.092 Uiso 1 1 calc R . . H7B H 0.5984 0.9949 0.3755 0.092 Uiso 1 1 calc R . . H7C H 0.7192 0.9921 0.3183 0.092 Uiso 1 1 calc R . . C8 C 0.5976(4) 0.7289(3) 0.3471(2) 0.0433(7) Uani 1 1 d . . . H8A H 0.6165 0.6429 0.3688 0.052 Uiso 1 1 calc R . . H8B H 0.4993 0.7395 0.3563 0.052 Uiso 1 1 calc R . . C9 C 0.5861(3) 0.7182(3) 0.24553(19) 0.0348(6) Uani 1 1 d . . . H9 H 0.5673 0.8058 0.2250 0.042 Uiso 1 1 calc R . . C10 C 0.7277(3) 0.6951(3) 0.22008(17) 0.0306(5) Uani 1 1 d . . . C11 C 0.8304(4) 0.7935(3) 0.18884(19) 0.0389(6) Uani 1 1 d . . . H11 H 0.8177 0.8814 0.1769 0.047 Uiso 1 1 calc R . . C12 C 0.9544(4) 0.7358(3) 0.1790(2) 0.0443(7) Uani 1 1 d . . . H12 H 1.0394 0.7795 0.1609 0.053 Uiso 1 1 calc R . . C13 C 0.9277(3) 0.5999(3) 0.20109(19) 0.0369(6) Uani 1 1 d . . . H13 H 0.9938 0.5397 0.2018 0.044 Uiso 1 1 calc R . . C14 C 0.7828(3) 0.5703(3) 0.22217(16) 0.0290(5) Uani 1 1 d . . . C15 C 0.7810(3) 0.3335(3) 0.25395(18) 0.0315(5) Uani 1 1 d . . . H15 H 0.7054 0.2589 0.2663 0.038 Uiso 1 1 calc R . . C16 C 0.9101(4) 0.3652(3) 0.3396(2) 0.0428(7) Uani 1 1 d . . . H16A H 0.9939 0.4301 0.3294 0.064 Uiso 1 1 calc R . . H16B H 0.9434 0.2825 0.3556 0.064 Uiso 1 1 calc R . . H16C H 0.8744 0.4031 0.3880 0.064 Uiso 1 1 calc R . . C17 C 0.8305(3) 0.2753(3) 0.17409(18) 0.0315(5) Uani 1 1 d . . . C18 C 0.7901(4) 0.3157(3) 0.08905(19) 0.0389(6) Uani 1 1 d . . . H18 H 0.7279 0.3796 0.0789 0.047 Uiso 1 1 calc R . . C19 C 0.8399(4) 0.2633(3) 0.0184(2) 0.0457(7) Uani 1 1 d . . . H19 H 0.8124 0.2930 -0.0385 0.055 Uiso 1 1 calc R . . C20 C 0.9295(4) 0.1681(3) 0.0318(2) 0.0475(8) Uani 1 1 d . . . H20 H 0.9649 0.1339 -0.0155 0.057 Uiso 1 1 calc R . . C21 C 0.9666(4) 0.1235(3) 0.1150(2) 0.0449(7) Uani 1 1 d . . . H21 H 1.0256 0.0570 0.1241 0.054 Uiso 1 1 calc R . . C22 C 0.9176(3) 0.1760(3) 0.1855(2) 0.0369(6) Uani 1 1 d . . . H22 H 0.9434 0.1442 0.2418 0.044 Uiso 1 1 calc R . . C30 C 0.4523(3) 0.6094(3) 0.1945(2) 0.0352(6) Uani 1 1 d . . . C31 C 0.4365(3) 0.5477(3) 0.10646(19) 0.0365(6) Uani 1 1 d . . . H31 H 0.5060 0.5683 0.0711 0.044 Uiso 1 1 calc R . . C32 C 0.2999(3) 0.4508(3) 0.0810(2) 0.0437(7) Uani 1 1 d . . . H32 H 0.2614 0.3963 0.0258 0.052 Uiso 1 1 calc R . . C33 C 0.2316(3) 0.4507(3) 0.1533(3) 0.0495(8) Uani 1 1 d . . . H33 H 0.1402 0.3941 0.1553 0.059 Uiso 1 1 calc R . . C34 C 0.3229(4) 0.5496(3) 0.2219(3) 0.0471(8) Uani 1 1 d . . . H34 H 0.3012 0.5720 0.2769 0.056 Uiso 1 1 calc R . . N41 N 0.4436(3) 0.3056(3) 0.33314(19) 0.0522(7) Uani 1 1 d . . . C42 C 0.2987(6) 0.2309(9) 0.3368(4) 0.139(3) Uani 1 1 d . . . H42A H 0.3118 0.1546 0.3708 0.209 Uiso 1 1 calc R . . H42B H 0.2385 0.1982 0.2764 0.209 Uiso 1 1 calc R . . H42C H 0.2476 0.2894 0.3655 0.209 Uiso 1 1 calc R . . C43 C 0.5419(5) 0.3339(5) 0.4209(2) 0.0618(10) Uani 1 1 d . . . H43A H 0.4986 0.3865 0.4590 0.093 Uiso 1 1 calc R . . H43B H 0.6396 0.3852 0.4180 0.093 Uiso 1 1 calc R . . H43C H 0.5544 0.2495 0.4455 0.093 Uiso 1 1 calc R . . N51 N 0.4266(3) 0.1831(3) 0.1303(2) 0.0479(7) Uani 1 1 d . . . C52 C 0.4325(7) 0.0569(4) 0.1676(4) 0.097(2) Uani 1 1 d . . . H52A H 0.3382 -0.0074 0.1419 0.146 Uiso 1 1 calc R . . H52B H 0.4476 0.0715 0.2321 0.146 Uiso 1 1 calc R . . H52C H 0.5158 0.0212 0.1541 0.146 Uiso 1 1 calc R . . C53 C 0.4000(6) 0.1593(4) 0.0335(3) 0.0695(11) Uani 1 1 d . . . H53A H 0.4813 0.1216 0.0189 0.104 Uiso 1 1 calc R . . H53B H 0.3965 0.2443 0.0078 0.104 Uiso 1 1 calc R . . H53C H 0.3044 0.0961 0.0092 0.104 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 Zr 0.02609(13) 0.03281(14) 0.03132(14) 0.00486(10) 0.00488(10) 0.00625(10) Fe 0.0350(2) 0.0393(2) 0.0263(2) 0.00091(16) -0.00001(16) -0.00056(17) N1 0.0255(10) 0.0310(11) 0.0290(11) 0.0053(8) 0.0049(8) 0.0096(8) C1 0.061(2) 0.0411(16) 0.0228(13) -0.0049(11) -0.0006(12) 0.0040(14) C2 0.062(2) 0.0435(17) 0.0363(16) -0.0060(13) -0.0061(15) -0.0059(15) C3 0.0453(19) 0.065(2) 0.0453(19) -0.0070(17) -0.0097(15) -0.0096(17) C4 0.0493(19) 0.062(2) 0.0372(17) -0.0013(15) -0.0126(14) 0.0075(16) C5 0.060(2) 0.0493(18) 0.0230(13) 0.0030(12) -0.0012(13) 0.0094(15) C6 0.067(2) 0.0447(17) 0.0292(14) -0.0046(12) 0.0082(14) 0.0136(16) C7 0.081(3) 0.0455(19) 0.050(2) -0.0125(16) 0.0008(19) 0.0177(19) C8 0.0470(17) 0.0493(18) 0.0360(15) -0.0020(13) 0.0138(13) 0.0138(14) C9 0.0397(14) 0.0317(13) 0.0326(14) 0.0001(11) 0.0059(11) 0.0116(11) C10 0.0340(13) 0.0320(13) 0.0213(11) 0.0007(9) 0.0004(10) 0.0040(10) C11 0.0451(16) 0.0378(15) 0.0282(13) 0.0049(11) 0.0031(12) 0.0013(12) C12 0.0398(16) 0.0537(18) 0.0346(15) 0.0057(13) 0.0104(12) -0.0043(13) C13 0.0295(13) 0.0473(16) 0.0312(13) -0.0012(12) 0.0068(11) 0.0041(12) C14 0.0289(12) 0.0329(13) 0.0220(11) 0.0002(9) 0.0018(9) 0.0049(10) C15 0.0300(12) 0.0349(13) 0.0308(13) 0.0063(10) 0.0050(10) 0.0118(11) C16 0.0444(16) 0.0518(18) 0.0311(14) 0.0047(13) -0.0011(12) 0.0201(14) C17 0.0291(12) 0.0311(13) 0.0334(13) 0.0022(10) 0.0056(10) 0.0071(10) C18 0.0442(16) 0.0412(15) 0.0322(14) 0.0018(11) 0.0027(12) 0.0199(13) C19 0.061(2) 0.0481(18) 0.0299(14) 0.0024(12) 0.0093(13) 0.0196(15) C20 0.061(2) 0.0417(17) 0.0429(17) -0.0051(13) 0.0158(15) 0.0163(15) C21 0.0499(18) 0.0366(15) 0.0516(18) 0.0010(13) 0.0118(14) 0.0196(14) C22 0.0373(14) 0.0351(14) 0.0393(15) 0.0076(11) 0.0073(12) 0.0115(12) C30 0.0317(13) 0.0333(13) 0.0407(15) 0.0023(11) 0.0041(11) 0.0135(11) C31 0.0388(14) 0.0357(14) 0.0311(13) 0.0048(11) -0.0026(11) 0.0119(12) C32 0.0370(15) 0.0368(15) 0.0490(18) 0.0016(13) -0.0076(13) 0.0106(12) C33 0.0271(14) 0.0449(17) 0.074(2) 0.0000(16) 0.0065(14) 0.0100(12) C34 0.0349(15) 0.0477(18) 0.061(2) -0.0046(15) 0.0159(14) 0.0141(13) N41 0.0398(14) 0.075(2) 0.0390(15) 0.0160(14) 0.0094(11) 0.0012(14) C42 0.050(3) 0.258(9) 0.087(4) 0.085(5) 0.003(3) -0.029(4) C43 0.062(2) 0.079(3) 0.0420(19) 0.0121(18) 0.0120(17) 0.008(2) N51 0.0424(14) 0.0354(13) 0.0587(17) 0.0000(12) -0.0020(12) 0.0102(11) C52 0.138(5) 0.044(2) 0.081(3) 0.002(2) -0.031(3) 0.024(3) C53 0.089(3) 0.051(2) 0.065(3) -0.0051(19) 0.014(2) 0.016(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 Zr N41 2.052(3) . ? Zr N51 2.075(3) . ? Zr N1 2.101(2) . ? Zr C33 2.508(3) . ? Zr C34 2.520(3) . ? Zr C30 2.533(3) . ? Zr C31 2.548(3) . ? Zr C32 2.554(3) . ? Fe C1 2.012(3) . ? Fe C10 2.019(3) . ? Fe C11 2.023(3) . ? Fe C5 2.028(3) . ? Fe C12 2.029(3) . ? Fe C2 2.036(3) . ? Fe C4 2.048(3) . ? Fe C3 2.055(3) . ? Fe C13 2.060(3) . ? Fe C14 2.124(3) . ? N1 C14 1.393(3) . ? N1 C15 1.479(3) . ? C1 C2 1.434(5) . ? C1 C5 1.435(5) . ? C1 C6 1.502(5) . ? C2 C3 1.421(6) . ? C2 H2 0.9400 . ? C3 C4 1.416(6) . ? C3 H3 0.9400 . ? C4 C5 1.424(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.529(5) . ? C6 C8 1.548(5) . ? C6 H6 0.9900 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.542(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.509(4) . ? C9 C30 1.518(4) . ? C9 H9 0.9900 . ? C10 C11 1.432(4) . ? C10 C14 1.446(4) . ? C11 C12 1.417(5) . ? C11 H11 0.9400 . ? C12 C13 1.426(5) . ? C12 H12 0.9400 . ? C13 C14 1.439(4) . ? C13 H13 0.9400 . ? C15 C17 1.533(4) . ? C15 C16 1.534(4) . ? C15 H15 0.9900 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.386(4) . ? C17 C22 1.396(4) . ? C18 C19 1.391(4) . ? C18 H18 0.9400 . ? C19 C20 1.379(5) . ? C19 H19 0.9400 . ? C20 C21 1.375(5) . ? C20 H20 0.9400 . ? C21 C22 1.386(4) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C30 C34 1.409(4) . ? C30 C31 1.423(4) . ? C31 C32 1.408(4) . ? C31 H31 0.9400 . ? C32 C33 1.405(5) . ? C32 H32 0.9400 . ? C33 C34 1.406(5) . ? C33 H33 0.9400 . ? C34 H34 0.9400 . ? N41 C43 1.425(5) . ? N41 C42 1.430(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? N51 C52 1.435(5) . ? N51 C53 1.453(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 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 N41 Zr N51 104.00(13) . . ? N41 Zr N1 103.58(10) . . ? N51 Zr N1 106.82(10) . . ? N41 Zr C33 102.65(13) . . ? N51 Zr C33 101.75(11) . . ? N1 Zr C33 134.69(10) . . ? N41 Zr C34 92.00(13) . . ? N51 Zr C34 134.22(11) . . ? N1 Zr C34 110.60(10) . . ? C33 Zr C34 32.47(11) . . ? N41 Zr C30 113.63(12) . . ? N51 Zr C30 138.30(11) . . ? N1 Zr C30 81.77(9) . . ? C33 Zr C30 53.91(10) . . ? C34 Zr C30 32.39(10) . . ? N41 Zr C31 144.50(12) . . ? N51 Zr C31 106.29(11) . . ? N1 Zr C31 84.96(9) . . ? C33 Zr C31 53.26(11) . . ? C34 Zr C31 53.29(11) . . ? C30 Zr C31 32.53(9) . . ? N41 Zr C32 134.49(12) . . ? N51 Zr C32 87.11(10) . . ? N1 Zr C32 115.28(10) . . ? C33 Zr C32 32.22(12) . . ? C34 Zr C32 53.46(11) . . ? C30 Zr C32 53.80(9) . . ? C31 Zr C32 32.04(9) . . ? C1 Fe C10 98.78(13) . . ? C1 Fe C11 112.84(13) . . ? C10 Fe C11 41.50(11) . . ? C1 Fe C5 41.60(13) . . ? C10 Fe C5 114.03(13) . . ? C11 Fe C5 148.73(14) . . ? C1 Fe C12 150.58(14) . . ? C10 Fe C12 69.58(12) . . ? C11 Fe C12 40.94(13) . . ? C5 Fe C12 167.82(14) . . ? C1 Fe C2 41.50(15) . . ? C10 Fe C2 120.21(14) . . ? C11 Fe C2 104.14(14) . . ? C5 Fe C2 68.90(14) . . ? C12 Fe C2 120.25(15) . . ? C1 Fe C4 69.68(15) . . ? C10 Fe C4 152.10(14) . . ? C11 Fe C4 166.32(15) . . ? C5 Fe C4 40.90(15) . . ? C12 Fe C4 132.00(15) . . ? C2 Fe C4 68.33(15) . . ? C1 Fe C3 69.65(16) . . ? C10 Fe C3 160.02(15) . . ? C11 Fe C3 126.67(15) . . ? C5 Fe C3 68.64(16) . . ? C12 Fe C3 112.28(15) . . ? C2 Fe C3 40.66(16) . . ? C4 Fe C3 40.37(16) . . ? C1 Fe C13 160.53(13) . . ? C10 Fe C13 69.03(11) . . ? C11 Fe C13 68.63(12) . . ? C5 Fe C13 128.21(13) . . ? C12 Fe C13 40.80(13) . . ? C2 Fe C13 157.89(14) . . ? C4 Fe C13 113.83(14) . . ? C3 Fe C13 126.23(15) . . ? C1 Fe C14 120.94(12) . . ? C10 Fe C14 40.75(10) . . ? C11 Fe C14 68.27(11) . . ? C5 Fe C14 106.46(12) . . ? C12 Fe C14 68.14(12) . . ? C2 Fe C14 158.30(14) . . ? C4 Fe C14 122.88(13) . . ? C3 Fe C14 159.23(14) . . ? C13 Fe C14 40.21(10) . . ? C14 N1 C15 118.5(2) . . ? C14 N1 Zr 133.11(16) . . ? C15 N1 Zr 107.09(16) . . ? C2 C1 C5 106.5(3) . . ? C2 C1 C6 127.8(3) . . ? C5 C1 C6 125.5(3) . . ? C2 C1 Fe 70.1(2) . . ? C5 C1 Fe 69.80(18) . . ? C6 C1 Fe 121.2(2) . . ? C3 C2 C1 108.9(3) . . ? C3 C2 Fe 70.4(2) . . ? C1 C2 Fe 68.37(18) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Fe C2 H2 127.3 . . ? C4 C3 C2 107.9(3) . . ? C4 C3 Fe 69.54(19) . . ? C2 C3 Fe 68.95(19) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe C3 H3 127.0 . . ? C3 C4 C5 108.3(3) . . ? C3 C4 Fe 70.08(19) . . ? C5 C4 Fe 68.83(18) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe C4 H4 126.8 . . ? C4 C5 C1 108.4(3) . . ? C4 C5 Fe 70.27(19) . . ? C1 C5 Fe 68.60(17) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe C5 H5 126.9 . . ? C1 C6 C7 112.6(3) . . ? C1 C6 C8 112.7(3) . . ? C7 C6 C8 112.2(3) . . ? C1 C6 H6 106.2 . . ? C7 C6 H6 106.2 . . ? C8 C6 H6 106.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 116.5(3) . . ? C9 C8 H8A 108.2 . . ? C6 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C6 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C30 109.5(2) . . ? C10 C9 C8 114.5(2) . . ? C30 C9 C8 111.4(3) . . ? C10 C9 H9 107.0 . . ? C30 C9 H9 107.0 . . ? C8 C9 H9 107.0 . . ? C11 C10 C14 108.0(2) . . ? C11 C10 C9 125.7(3) . . ? C14 C10 C9 126.3(2) . . ? C11 C10 Fe 69.40(16) . . ? C14 C10 Fe 73.54(15) . . ? C9 C10 Fe 123.06(18) . . ? C12 C11 C10 108.3(3) . . ? C12 C11 Fe 69.78(17) . . ? C10 C11 Fe 69.09(15) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe C11 H11 126.9 . . ? C11 C12 C13 108.1(3) . . ? C11 C12 Fe 69.28(17) . . ? C13 C12 Fe 70.74(17) . . ? C11 C12 H12 125.9 . . ? C13 C12 H12 125.9 . . ? Fe C12 H12 125.6 . . ? C12 C13 C14 108.7(3) . . ? C12 C13 Fe 68.46(17) . . ? C14 C13 Fe 72.30(15) . . ? C12 C13 H13 125.6 . . ? C14 C13 H13 125.6 . . ? Fe C13 H13 125.2 . . ? N1 C14 C13 129.1(2) . . ? N1 C14 C10 124.3(2) . . ? C13 C14 C10 106.5(2) . . ? N1 C14 Fe 134.84(18) . . ? C13 C14 Fe 67.49(15) . . ? C10 C14 Fe 65.71(14) . . ? N1 C15 C17 114.9(2) . . ? N1 C15 C16 112.9(2) . . ? C17 C15 C16 112.2(2) . . ? N1 C15 H15 105.3 . . ? C17 C15 H15 105.3 . . ? C16 C15 H15 105.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 117.6(3) . . ? C18 C17 C15 122.6(2) . . ? C22 C17 C15 119.8(2) . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.4(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 121.1(3) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C34 C30 C31 106.8(3) . . ? C34 C30 C9 128.8(3) . . ? C31 C30 C9 124.4(3) . . ? C34 C30 Zr 73.31(17) . . ? C31 C30 Zr 74.33(16) . . ? C9 C30 Zr 117.72(17) . . ? C32 C31 C30 108.8(3) . . ? C32 C31 Zr 74.21(17) . . ? C30 C31 Zr 73.14(16) . . ? C32 C31 H31 125.6 . . ? C30 C31 H31 125.6 . . ? Zr C31 H31 118.9 . . ? C33 C32 C31 107.3(3) . . ? C33 C32 Zr 72.08(18) . . ? C31 C32 Zr 73.76(16) . . ? C33 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? Zr C32 H32 119.7 . . ? C32 C33 C34 108.6(3) . . ? C32 C33 Zr 75.70(17) . . ? C34 C33 Zr 74.25(18) . . ? C32 C33 H33 125.7 . . ? C34 C33 H33 125.7 . . ? Zr C33 H33 116.4 . . ? C33 C34 C30 108.5(3) . . ? C33 C34 Zr 73.28(18) . . ? C30 C34 Zr 74.30(16) . . ? C33 C34 H34 125.7 . . ? C30 C34 H34 125.7 . . ? Zr C34 H34 118.6 . . ? C43 N41 C42 109.9(3) . . ? C43 N41 Zr 132.2(2) . . ? C42 N41 Zr 117.6(3) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C52 N51 C53 109.0(3) . . ? C52 N51 Zr 121.4(3) . . ? C53 N51 Zr 129.4(2) . . ? N51 C52 H52A 109.5 . . ? N51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N51 C53 H53A 109.5 . . ? N51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 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 N41 Zr N1 C14 -126.8(2) . . . . ? N51 Zr N1 C14 123.8(2) . . . . ? C33 Zr N1 C14 -3.0(3) . . . . ? C34 Zr N1 C14 -29.4(3) . . . . ? C30 Zr N1 C14 -14.3(2) . . . . ? C31 Zr N1 C14 18.3(2) . . . . ? C32 Zr N1 C14 28.9(3) . . . . ? N41 Zr N1 C15 67.00(19) . . . . ? N51 Zr N1 C15 -42.45(18) . . . . ? C33 Zr N1 C15 -169.22(17) . . . . ? C34 Zr N1 C15 164.42(17) . . . . ? C30 Zr N1 C15 179.44(17) . . . . ? C31 Zr N1 C15 -147.96(17) . . . . ? C32 Zr N1 C15 -137.31(16) . . . . ? C10 Fe C1 C2 -126.4(2) . . . . ? C11 Fe C1 C2 -85.6(2) . . . . ? C5 Fe C1 C2 117.1(3) . . . . ? C12 Fe C1 C2 -62.8(3) . . . . ? C4 Fe C1 C2 79.9(2) . . . . ? C3 Fe C1 C2 36.7(2) . . . . ? C13 Fe C1 C2 -175.9(3) . . . . ? C14 Fe C1 C2 -163.18(19) . . . . ? C10 Fe C1 C5 116.5(2) . . . . ? C11 Fe C1 C5 157.3(2) . . . . ? C12 Fe C1 C5 -179.9(2) . . . . ? C2 Fe C1 C5 -117.1(3) . . . . ? C4 Fe C1 C5 -37.2(2) . . . . ? C3 Fe C1 C5 -80.4(2) . . . . ? C13 Fe C1 C5 67.0(4) . . . . ? C14 Fe C1 C5 79.8(2) . . . . ? C10 Fe C1 C6 -3.6(3) . . . . ? C11 Fe C1 C6 37.2(3) . . . . ? C5 Fe C1 C6 -120.1(4) . . . . ? C12 Fe C1 C6 60.0(4) . . . . ? C2 Fe C1 C6 122.8(4) . . . . ? C4 Fe C1 C6 -157.3(3) . . . . ? C3 Fe C1 C6 159.5(3) . . . . ? C13 Fe C1 C6 -53.1(5) . . . . ? C14 Fe C1 C6 -40.3(3) . . . . ? C5 C1 C2 C3 1.8(3) . . . . ? C6 C1 C2 C3 -173.4(3) . . . . ? Fe C1 C2 C3 -58.9(2) . . . . ? C5 C1 C2 Fe 60.7(2) . . . . ? C6 C1 C2 Fe -114.6(3) . . . . ? C1 Fe C2 C3 120.7(3) . . . . ? C10 Fe C2 C3 -172.4(2) . . . . ? C11 Fe C2 C3 -130.7(2) . . . . ? C5 Fe C2 C3 81.4(2) . . . . ? C12 Fe C2 C3 -89.7(3) . . . . ? C4 Fe C2 C3 37.3(2) . . . . ? C13 Fe C2 C3 -62.9(4) . . . . ? C14 Fe C2 C3 162.9(3) . . . . ? C10 Fe C2 C1 67.0(2) . . . . ? C11 Fe C2 C1 108.6(2) . . . . ? C5 Fe C2 C1 -39.3(2) . . . . ? C12 Fe C2 C1 149.6(2) . . . . ? C4 Fe C2 C1 -83.4(2) . . . . ? C3 Fe C2 C1 -120.7(3) . . . . ? C13 Fe C2 C1 176.4(3) . . . . ? C14 Fe C2 C1 42.2(4) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? Fe C2 C3 C4 -58.8(2) . . . . ? C1 C2 C3 Fe 57.6(2) . . . . ? C1 Fe C3 C4 82.2(3) . . . . ? C10 Fe C3 C4 139.3(4) . . . . ? C11 Fe C3 C4 -173.9(2) . . . . ? C5 Fe C3 C4 37.5(2) . . . . ? C12 Fe C3 C4 -129.4(2) . . . . ? C2 Fe C3 C4 119.6(3) . . . . ? C13 Fe C3 C4 -84.9(3) . . . . ? C14 Fe C3 C4 -42.5(5) . . . . ? C1 Fe C3 C2 -37.4(2) . . . . ? C10 Fe C3 C2 19.7(5) . . . . ? C11 Fe C3 C2 66.5(3) . . . . ? C5 Fe C3 C2 -82.1(2) . . . . ? C12 Fe C3 C2 111.0(2) . . . . ? C4 Fe C3 C2 -119.6(3) . . . . ? C13 Fe C3 C2 155.5(2) . . . . ? C14 Fe C3 C2 -162.1(3) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? Fe C3 C4 C5 -58.4(2) . . . . ? C2 C3 C4 Fe 58.5(2) . . . . ? C1 Fe C4 C3 -82.1(3) . . . . ? C10 Fe C4 C3 -151.5(3) . . . . ? C11 Fe C4 C3 21.1(7) . . . . ? C5 Fe C4 C3 -119.9(3) . . . . ? C12 Fe C4 C3 74.3(3) . . . . ? C2 Fe C4 C3 -37.6(2) . . . . ? C13 Fe C4 C3 118.6(2) . . . . ? C14 Fe C4 C3 163.4(2) . . . . ? C1 Fe C4 C5 37.8(2) . . . . ? C10 Fe C4 C5 -31.6(4) . . . . ? C11 Fe C4 C5 141.0(6) . . . . ? C12 Fe C4 C5 -165.8(2) . . . . ? C2 Fe C4 C5 82.4(2) . . . . ? C3 Fe C4 C5 119.9(3) . . . . ? C13 Fe C4 C5 -121.5(2) . . . . ? C14 Fe C4 C5 -76.6(2) . . . . ? C3 C4 C5 C1 1.0(4) . . . . ? Fe C4 C5 C1 -58.1(2) . . . . ? C3 C4 C5 Fe 59.1(2) . . . . ? C2 C1 C5 C4 -1.7(3) . . . . ? C6 C1 C5 C4 173.6(3) . . . . ? Fe C1 C5 C4 59.2(2) . . . . ? C2 C1 C5 Fe -60.9(2) . . . . ? C6 C1 C5 Fe 114.5(3) . . . . ? C1 Fe C5 C4 -120.1(3) . . . . ? C10 Fe C5 C4 164.4(2) . . . . ? C11 Fe C5 C4 -163.3(2) . . . . ? C12 Fe C5 C4 59.7(7) . . . . ? C2 Fe C5 C4 -80.8(2) . . . . ? C3 Fe C5 C4 -37.1(2) . . . . ? C13 Fe C5 C4 82.9(2) . . . . ? C14 Fe C5 C4 121.6(2) . . . . ? C10 Fe C5 C1 -75.5(2) . . . . ? C11 Fe C5 C1 -43.2(3) . . . . ? C12 Fe C5 C1 179.8(6) . . . . ? C2 Fe C5 C1 39.2(2) . . . . ? C4 Fe C5 C1 120.1(3) . . . . ? C3 Fe C5 C1 83.0(2) . . . . ? C13 Fe C5 C1 -157.01(19) . . . . ? C14 Fe C5 C1 -118.3(2) . . . . ? C2 C1 C6 C7 -3.3(4) . . . . ? C5 C1 C6 C7 -177.7(3) . . . . ? Fe C1 C6 C7 -91.4(3) . . . . ? C2 C1 C6 C8 124.8(3) . . . . ? C5 C1 C6 C8 -49.5(4) . . . . ? Fe C1 C6 C8 36.8(4) . . . . ? C1 C6 C8 C9 -70.2(4) . . . . ? C7 C6 C8 C9 58.1(4) . . . . ? C6 C8 C9 C10 60.5(4) . . . . ? C6 C8 C9 C30 -174.5(3) . . . . ? C30 C9 C10 C11 126.9(3) . . . . ? C8 C9 C10 C11 -107.1(3) . . . . ? C30 C9 C10 C14 -52.5(3) . . . . ? C8 C9 C10 C14 73.5(3) . . . . ? C30 C9 C10 Fe -145.9(2) . . . . ? C8 C9 C10 Fe -19.9(3) . . . . ? C1 Fe C10 C11 114.72(19) . . . . ? C5 Fe C10 C11 155.29(18) . . . . ? C12 Fe C10 C11 -37.29(18) . . . . ? C2 Fe C10 C11 76.6(2) . . . . ? C4 Fe C10 C11 177.4(3) . . . . ? C3 Fe C10 C11 61.9(5) . . . . ? C13 Fe C10 C11 -81.04(19) . . . . ? C14 Fe C10 C11 -117.1(2) . . . . ? C1 Fe C10 C14 -128.16(17) . . . . ? C11 Fe C10 C14 117.1(2) . . . . ? C5 Fe C10 C14 -87.59(18) . . . . ? C12 Fe C10 C14 79.84(18) . . . . ? C2 Fe C10 C14 -166.26(17) . . . . ? C4 Fe C10 C14 -65.5(3) . . . . ? C3 Fe C10 C14 179.0(4) . . . . ? C13 Fe C10 C14 36.09(16) . . . . ? C1 Fe C10 C9 -5.2(2) . . . . ? C11 Fe C10 C9 -119.9(3) . . . . ? C5 Fe C10 C9 35.4(3) . . . . ? C12 Fe C10 C9 -157.2(3) . . . . ? C2 Fe C10 C9 -43.3(3) . . . . ? C4 Fe C10 C9 57.4(4) . . . . ? C3 Fe C10 C9 -58.0(5) . . . . ? C13 Fe C10 C9 159.0(3) . . . . ? C14 Fe C10 C9 122.9(3) . . . . ? C14 C10 C11 C12 -4.9(3) . . . . ? C9 C10 C11 C12 175.5(3) . . . . ? Fe C10 C11 C12 58.9(2) . . . . ? C14 C10 C11 Fe -63.85(17) . . . . ? C9 C10 C11 Fe 116.6(3) . . . . ? C1 Fe C11 C12 163.11(19) . . . . ? C10 Fe C11 C12 -120.0(2) . . . . ? C5 Fe C11 C12 -167.3(2) . . . . ? C2 Fe C11 C12 120.2(2) . . . . ? C4 Fe C11 C12 65.2(7) . . . . ? C3 Fe C11 C12 82.1(2) . . . . ? C13 Fe C11 C12 -37.87(18) . . . . ? C14 Fe C11 C12 -81.25(19) . . . . ? C1 Fe C11 C10 -76.93(19) . . . . ? C5 Fe C11 C10 -47.4(3) . . . . ? C12 Fe C11 C10 120.0(2) . . . . ? C2 Fe C11 C10 -119.89(19) . . . . ? C4 Fe C11 C10 -174.8(6) . . . . ? C3 Fe C11 C10 -157.9(2) . . . . ? C13 Fe C11 C10 82.09(17) . . . . ? C14 Fe C11 C10 38.71(16) . . . . ? C10 C11 C12 C13 1.8(3) . . . . ? Fe C11 C12 C13 60.3(2) . . . . ? C10 C11 C12 Fe -58.49(19) . . . . ? C1 Fe C12 C11 -33.0(3) . . . . ? C10 Fe C12 C11 37.78(17) . . . . ? C5 Fe C12 C11 147.3(6) . . . . ? C2 Fe C12 C11 -76.1(2) . . . . ? C4 Fe C12 C11 -163.2(2) . . . . ? C3 Fe C12 C11 -120.8(2) . . . . ? C13 Fe C12 C11 119.0(2) . . . . ? C14 Fe C12 C11 81.59(18) . . . . ? C1 Fe C12 C13 -152.0(3) . . . . ? C10 Fe C12 C13 -81.19(18) . . . . ? C11 Fe C12 C13 -119.0(2) . . . . ? C5 Fe C12 C13 28.3(7) . . . . ? C2 Fe C12 C13 164.95(19) . . . . ? C4 Fe C12 C13 77.8(2) . . . . ? C3 Fe C12 C13 120.2(2) . . . . ? C14 Fe C12 C13 -37.39(16) . . . . ? C11 C12 C13 C14 2.0(3) . . . . ? Fe C12 C13 C14 61.40(19) . . . . ? C11 C12 C13 Fe -59.4(2) . . . . ? C1 Fe C13 C12 136.3(4) . . . . ? C10 Fe C13 C12 82.65(19) . . . . ? C11 Fe C13 C12 37.99(18) . . . . ? C5 Fe C13 C12 -172.7(2) . . . . ? C2 Fe C13 C12 -36.6(4) . . . . ? C4 Fe C13 C12 -127.4(2) . . . . ? C3 Fe C13 C12 -82.6(2) . . . . ? C14 Fe C13 C12 119.2(2) . . . . ? C1 Fe C13 C14 17.1(5) . . . . ? C10 Fe C13 C14 -36.55(15) . . . . ? C11 Fe C13 C14 -81.21(17) . . . . ? C5 Fe C13 C14 68.1(2) . . . . ? C12 Fe C13 C14 -119.2(2) . . . . ? C2 Fe C13 C14 -155.8(3) . . . . ? C4 Fe C13 C14 113.38(19) . . . . ? C3 Fe C13 C14 158.24(19) . . . . ? C15 N1 C14 C13 16.7(4) . . . . ? Zr N1 C14 C13 -148.3(2) . . . . ? C15 N1 C14 C10 -168.3(2) . . . . ? Zr N1 C14 C10 26.7(4) . . . . ? C15 N1 C14 Fe -79.7(3) . . . . ? Zr N1 C14 Fe 115.3(2) . . . . ? C12 C13 C14 N1 170.7(3) . . . . ? Fe C13 C14 N1 -130.3(3) . . . . ? C12 C13 C14 C10 -4.9(3) . . . . ? Fe C13 C14 C10 54.07(17) . . . . ? C12 C13 C14 Fe -59.0(2) . . . . ? C11 C10 C14 N1 -169.9(2) . . . . ? C9 C10 C14 N1 9.7(4) . . . . ? Fe C10 C14 N1 128.9(2) . . . . ? C11 C10 C14 C13 6.0(3) . . . . ? C9 C10 C14 C13 -174.4(2) . . . . ? Fe C10 C14 C13 -55.15(18) . . . . ? C11 C10 C14 Fe 61.19(18) . . . . ? C9 C10 C14 Fe -119.3(3) . . . . ? C1 Fe C14 N1 -50.1(3) . . . . ? C10 Fe C14 N1 -115.1(3) . . . . ? C11 Fe C14 N1 -154.5(3) . . . . ? C5 Fe C14 N1 -7.2(3) . . . . ? C12 Fe C14 N1 161.3(3) . . . . ? C2 Fe C14 N1 -81.3(4) . . . . ? C4 Fe C14 N1 34.5(3) . . . . ? C3 Fe C14 N1 65.9(5) . . . . ? C13 Fe C14 N1 123.4(3) . . . . ? C1 Fe C14 C13 -173.45(18) . . . . ? C10 Fe C14 C13 121.6(2) . . . . ? C11 Fe C14 C13 82.17(19) . . . . ? C5 Fe C14 C13 -130.51(19) . . . . ? C12 Fe C14 C13 37.92(18) . . . . ? C2 Fe C14 C13 155.3(3) . . . . ? C4 Fe C14 C13 -88.9(2) . . . . ? C3 Fe C14 C13 -57.5(4) . . . . ? C1 Fe C14 C10 64.96(19) . . . . ? C11 Fe C14 C10 -39.41(16) . . . . ? C5 Fe C14 C10 107.91(18) . . . . ? C12 Fe C14 C10 -83.66(18) . . . . ? C2 Fe C14 C10 33.7(4) . . . . ? C4 Fe C14 C10 149.53(19) . . . . ? C3 Fe C14 C10 -179.1(4) . . . . ? C13 Fe C14 C10 -121.6(2) . . . . ? C14 N1 C15 C17 -69.0(3) . . . . ? Zr N1 C15 C17 99.6(2) . . . . ? C14 N1 C15 C16 61.4(3) . . . . ? Zr N1 C15 C16 -130.0(2) . . . . ? N1 C15 C17 C18 -6.4(4) . . . . ? C16 C15 C17 C18 -137.1(3) . . . . ? N1 C15 C17 C22 174.8(2) . . . . ? C16 C15 C17 C22 44.1(4) . . . . ? C22 C17 C18 C19 -2.7(5) . . . . ? C15 C17 C18 C19 178.4(3) . . . . ? C17 C18 C19 C20 0.9(5) . . . . ? C18 C19 C20 C21 1.3(5) . . . . ? C19 C20 C21 C22 -1.5(5) . . . . ? C20 C21 C22 C17 -0.3(5) . . . . ? C18 C17 C22 C21 2.4(4) . . . . ? C15 C17 C22 C21 -178.7(3) . . . . ? C10 C9 C30 C34 147.1(3) . . . . ? C8 C9 C30 C34 19.4(4) . . . . ? C10 C9 C30 C31 -32.7(4) . . . . ? C8 C9 C30 C31 -160.5(3) . . . . ? C10 C9 C30 Zr 56.7(3) . . . . ? C8 C9 C30 Zr -71.0(3) . . . . ? N41 Zr C30 C34 -51.8(2) . . . . ? N51 Zr C30 C34 100.8(2) . . . . ? N1 Zr C30 C34 -153.1(2) . . . . ? C33 Zr C30 C34 36.9(2) . . . . ? C31 Zr C30 C34 113.4(3) . . . . ? C32 Zr C30 C34 77.1(2) . . . . ? N41 Zr C30 C31 -165.17(17) . . . . ? N51 Zr C30 C31 -12.5(2) . . . . ? N1 Zr C30 C31 93.55(17) . . . . ? C33 Zr C30 C31 -76.5(2) . . . . ? C34 Zr C30 C31 -113.4(3) . . . . ? C32 Zr C30 C31 -36.29(17) . . . . ? N41 Zr C30 C9 73.8(2) . . . . ? N51 Zr C30 C9 -133.6(2) . . . . ? N1 Zr C30 C9 -27.5(2) . . . . ? C33 Zr C30 C9 162.4(3) . . . . ? C34 Zr C30 C9 125.6(3) . . . . ? C31 Zr C30 C9 -121.1(3) . . . . ? C32 Zr C30 C9 -157.4(3) . . . . ? C34 C30 C31 C32 -0.5(3) . . . . ? C9 C30 C31 C32 179.4(2) . . . . ? Zr C30 C31 C32 66.2(2) . . . . ? C34 C30 C31 Zr -66.7(2) . . . . ? C9 C30 C31 Zr 113.2(3) . . . . ? N41 Zr C31 C32 -92.0(2) . . . . ? N51 Zr C31 C32 55.5(2) . . . . ? N1 Zr C31 C32 161.6(2) . . . . ? C33 Zr C31 C32 -37.13(19) . . . . ? C34 Zr C31 C32 -78.0(2) . . . . ? C30 Zr C31 C32 -115.8(3) . . . . ? N41 Zr C31 C30 23.8(3) . . . . ? N51 Zr C31 C30 171.34(17) . . . . ? N1 Zr C31 C30 -82.58(17) . . . . ? C33 Zr C31 C30 78.66(19) . . . . ? C34 Zr C31 C30 37.83(17) . . . . ? C32 Zr C31 C30 115.8(3) . . . . ? C30 C31 C32 C33 -0.8(3) . . . . ? Zr C31 C32 C33 64.7(2) . . . . ? C30 C31 C32 Zr -65.51(19) . . . . ? N41 Zr C32 C33 10.7(3) . . . . ? N51 Zr C32 C33 117.5(2) . . . . ? N1 Zr C32 C33 -135.19(19) . . . . ? C34 Zr C32 C33 -37.48(19) . . . . ? C30 Zr C32 C33 -78.0(2) . . . . ? C31 Zr C32 C33 -114.9(3) . . . . ? N41 Zr C32 C31 125.6(2) . . . . ? N51 Zr C32 C31 -127.6(2) . . . . ? N1 Zr C32 C31 -20.3(2) . . . . ? C33 Zr C32 C31 114.9(3) . . . . ? C34 Zr C32 C31 77.4(2) . . . . ? C30 Zr C32 C31 36.87(17) . . . . ? C31 C32 C33 C34 1.7(4) . . . . ? Zr C32 C33 C34 67.6(2) . . . . ? C31 C32 C33 Zr -65.9(2) . . . . ? N41 Zr C33 C32 -172.20(19) . . . . ? N51 Zr C33 C32 -64.8(2) . . . . ? N1 Zr C33 C32 63.7(2) . . . . ? C34 Zr C33 C32 114.4(3) . . . . ? C30 Zr C33 C32 77.6(2) . . . . ? C31 Zr C33 C32 36.91(18) . . . . ? N41 Zr C33 C34 73.4(2) . . . . ? N51 Zr C33 C34 -179.2(2) . . . . ? N1 Zr C33 C34 -50.7(3) . . . . ? C30 Zr C33 C34 -36.8(2) . . . . ? C31 Zr C33 C34 -77.5(2) . . . . ? C32 Zr C33 C34 -114.4(3) . . . . ? C32 C33 C34 C30 -2.1(4) . . . . ? Zr C33 C34 C30 66.5(2) . . . . ? C32 C33 C34 Zr -68.6(2) . . . . ? C31 C30 C34 C33 1.5(3) . . . . ? C9 C30 C34 C33 -178.3(3) . . . . ? Zr C30 C34 C33 -65.8(2) . . . . ? C31 C30 C34 Zr 67.38(19) . . . . ? C9 C30 C34 Zr -112.5(3) . . . . ? N41 Zr C34 C33 -110.7(2) . . . . ? N51 Zr C34 C33 1.1(3) . . . . ? N1 Zr C34 C33 144.0(2) . . . . ? C30 Zr C34 C33 115.4(3) . . . . ? C31 Zr C34 C33 77.4(2) . . . . ? C32 Zr C34 C33 37.2(2) . . . . ? N41 Zr C34 C30 133.9(2) . . . . ? N51 Zr C34 C30 -114.3(2) . . . . ? N1 Zr C34 C30 28.6(2) . . . . ? C33 Zr C34 C30 -115.4(3) . . . . ? C31 Zr C34 C30 -38.00(17) . . . . ? C32 Zr C34 C30 -78.2(2) . . . . ? N51 Zr N41 C43 124.5(4) . . . . ? N1 Zr N41 C43 12.9(4) . . . . ? C33 Zr N41 C43 -129.8(4) . . . . ? C34 Zr N41 C43 -98.8(4) . . . . ? C30 Zr N41 C43 -73.9(4) . . . . ? C31 Zr N41 C43 -87.6(4) . . . . ? C32 Zr N41 C43 -135.6(3) . . . . ? N51 Zr N41 C42 -61.6(5) . . . . ? N1 Zr N41 C42 -173.1(5) . . . . ? C33 Zr N41 C42 44.1(5) . . . . ? C34 Zr N41 C42 75.1(5) . . . . ? C30 Zr N41 C42 100.0(5) . . . . ? C31 Zr N41 C42 86.3(5) . . . . ? C32 Zr N41 C42 38.3(5) . . . . ? N41 Zr N51 C52 -17.8(4) . . . . ? N1 Zr N51 C52 91.3(4) . . . . ? C33 Zr N51 C52 -124.2(4) . . . . ? C34 Zr N51 C52 -124.9(4) . . . . ? C30 Zr N51 C52 -172.1(4) . . . . ? C31 Zr N51 C52 -179.1(4) . . . . ? C32 Zr N51 C52 -153.1(4) . . . . ? N41 Zr N51 C53 167.3(3) . . . . ? N1 Zr N51 C53 -83.5(3) . . . . ? C33 Zr N51 C53 60.9(4) . . . . ? C34 Zr N51 C53 60.3(4) . . . . ? C30 Zr N51 C53 13.0(4) . . . . ? C31 Zr N51 C53 6.0(4) . . . . ? C32 Zr N51 C53 32.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.13 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.740 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.074 # Attachment '11b.cif' data_erk5320 _database_code_depnum_ccdc_archive 'CCDC 806923' #TrackingRef '11b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 Cl2 Fe N Zr' _chemical_formula_weight 583.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Zr Zr -2.9673 0.5597 '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 15.5580(3) _cell_length_b 13.6033(2) _cell_length_c 23.1772(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.068(1) _cell_angle_gamma 90.00 _cell_volume 4713.60(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9915 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6243 _exptl_absorpt_correction_T_max 0.9620 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28831 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 27.86 _reflns_number_total 11012 _reflns_number_gt 9273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0386P)^2^+14.0658P] 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 11012 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 -0.08934(4) 0.45288(4) 0.27086(2) 0.03518(13) Uani 1 1 d . . . Zr1 Zr 0.02777(2) 0.45917(3) 0.090638(16) 0.03426(10) Uani 1 1 d . . . Cl1A Cl -0.04950(8) 0.59311(8) 0.01461(4) 0.0463(2) Uani 1 1 d . . . Cl2A Cl 0.03905(9) 0.27870(8) 0.10140(5) 0.0530(3) Uani 1 1 d . . . N1A N -0.0687(2) 0.4722(2) 0.13501(13) 0.0325(6) Uani 1 1 d . . . C1A C -0.0134(3) 0.3408(3) 0.31392(18) 0.0436(9) Uani 1 1 d . . . C2A C -0.0533(3) 0.3906(3) 0.35439(19) 0.0488(10) Uani 1 1 d . . . H2A H -0.0222 0.4210 0.3906 0.059 Uiso 1 1 calc R . . C3A C -0.1473(3) 0.3867(3) 0.3308(2) 0.0506(11) Uani 1 1 d . . . H3A H -0.1894 0.4140 0.3485 0.061 Uiso 1 1 calc R . . C4A C -0.1667(3) 0.3346(3) 0.2764(2) 0.0503(10) Uani 1 1 d . . . H4A H -0.2242 0.3222 0.2510 0.060 Uiso 1 1 calc R . . C5A C -0.0849(3) 0.3039(3) 0.26602(19) 0.0460(10) Uani 1 1 d . . . H5A H -0.0790 0.2661 0.2334 0.055 Uiso 1 1 calc R . . C6A C 0.0848(3) 0.3333(4) 0.31724(19) 0.0478(10) Uani 1 1 d . . . H6A H 0.0994 0.2623 0.3195 0.057 Uiso 1 1 calc R . . C7A C 0.1441(4) 0.3792(5) 0.3736(2) 0.0676(15) Uani 1 1 d . . . H7A1 H 0.1296 0.4483 0.3748 0.101 Uiso 1 1 calc R . . H7A2 H 0.2062 0.3723 0.3738 0.101 Uiso 1 1 calc R . . H7A3 H 0.1347 0.3463 0.4085 0.101 Uiso 1 1 calc R . . C8A C 0.1038(3) 0.3718(3) 0.2594(2) 0.0487(10) Uani 1 1 d . . . H8A1 H 0.0635 0.3376 0.2253 0.058 Uiso 1 1 calc R . . H8A2 H 0.1649 0.3527 0.2604 0.058 Uiso 1 1 calc R . . C9A C 0.0943(3) 0.4837(3) 0.24658(18) 0.0422(9) Uani 1 1 d . . . H9A H 0.1360 0.5174 0.2809 0.051 Uiso 1 1 calc R . . C10A C 0.0019(3) 0.5255(3) 0.24053(17) 0.0359(8) Uani 1 1 d . . . C11A C -0.0262(3) 0.5840(3) 0.28320(18) 0.0415(9) Uani 1 1 d . . . H11A H 0.0112 0.6088 0.3194 0.050 Uiso 1 1 calc R . . C12A C -0.1197(3) 0.5985(3) 0.26188(19) 0.0438(9) Uani 1 1 d . . . H12A H -0.1552 0.6333 0.2818 0.053 Uiso 1 1 calc R . . C13A C -0.1506(3) 0.5512(3) 0.20524(17) 0.0386(8) Uani 1 1 d . . . H13A H -0.2105 0.5476 0.1819 0.046 Uiso 1 1 calc R . . C14A C -0.0751(2) 0.5100(3) 0.18980(16) 0.0327(7) Uani 1 1 d . . . C15A C -0.1466(3) 0.4284(3) 0.09130(17) 0.0382(8) Uani 1 1 d . . . H15A H -0.1237 0.4071 0.0575 0.046 Uiso 1 1 calc R . . C16A C -0.1771(3) 0.3339(3) 0.1149(2) 0.0514(11) Uani 1 1 d . . . H16A H -0.1259 0.2915 0.1307 0.077 Uiso 1 1 calc R . . H16B H -0.2202 0.3006 0.0825 0.077 Uiso 1 1 calc R . . H16C H -0.2046 0.3496 0.1466 0.077 Uiso 1 1 calc R . . C17A C -0.2237(3) 0.4982(3) 0.06291(17) 0.0395(9) Uani 1 1 d . . . C18A C -0.3034(3) 0.4593(4) 0.0275(2) 0.0549(11) Uani 1 1 d . . . H18A H -0.3083 0.3912 0.0207 0.066 Uiso 1 1 calc R . . C19A C -0.3758(3) 0.5197(5) 0.0018(2) 0.0702(15) Uani 1 1 d . . . H19A H -0.4295 0.4919 -0.0216 0.084 Uiso 1 1 calc R . . C20A C -0.3698(3) 0.6188(4) 0.0103(2) 0.0617(13) Uani 1 1 d . . . H20A H -0.4195 0.6593 -0.0063 0.074 Uiso 1 1 calc R . . C21A C -0.2898(3) 0.6596(4) 0.0434(2) 0.0520(11) Uani 1 1 d . . . H21A H -0.2846 0.7282 0.0485 0.062 Uiso 1 1 calc R . . C22A C -0.2172(3) 0.5996(3) 0.06922(17) 0.0424(9) Uani 1 1 d . . . H22A H -0.1630 0.6280 0.0913 0.051 Uiso 1 1 calc R . . C30A C 0.1231(3) 0.5090(3) 0.19119(18) 0.0410(9) Uani 1 1 d . . . C31A C 0.1774(3) 0.4524(4) 0.16343(19) 0.0475(10) Uani 1 1 d . . . H31A H 0.2022 0.3906 0.1764 0.057 Uiso 1 1 calc R . . C32A C 0.1877(3) 0.5045(4) 0.1134(2) 0.0517(11) Uani 1 1 d . . . H32A H 0.2204 0.4834 0.0871 0.062 Uiso 1 1 calc R . . C33A C 0.1414(3) 0.5924(4) 0.1096(2) 0.0506(10) Uani 1 1 d . . . H33A H 0.1381 0.6417 0.0807 0.061 Uiso 1 1 calc R . . C34A C 0.1001(3) 0.5953(3) 0.15651(18) 0.0431(9) Uani 1 1 d . . . H34A H 0.0634 0.6462 0.1636 0.052 Uiso 1 1 calc R . . Fe2 Fe -0.41151(4) 0.64489(4) 0.22933(2) 0.03640(13) Uani 1 1 d . . . Zr2 Zr -0.54716(3) 0.65452(3) 0.394820(17) 0.03612(10) Uani 1 1 d . . . Cl1B Cl -0.51109(8) 0.64059(9) 0.50256(5) 0.0537(3) Uani 1 1 d . . . Cl2B Cl -0.57622(8) 0.82765(8) 0.38215(6) 0.0534(3) Uani 1 1 d . . . N1B N -0.4427(2) 0.6331(2) 0.35967(14) 0.0374(7) Uani 1 1 d . . . C1B C -0.4938(3) 0.7466(3) 0.18016(19) 0.0448(9) Uani 1 1 d . . . C2B C -0.4403(3) 0.7044(3) 0.14512(19) 0.0480(10) Uani 1 1 d . . . H2B H -0.4618 0.6711 0.1084 0.058 Uiso 1 1 calc R . . C3B C -0.3496(3) 0.7218(4) 0.1753(2) 0.0496(10) Uani 1 1 d . . . H3B H -0.3002 0.7013 0.1624 0.060 Uiso 1 1 calc R . . C4B C -0.3457(3) 0.7753(3) 0.2283(2) 0.0507(11) Uani 1 1 d . . . H4B H -0.2933 0.7965 0.2567 0.061 Uiso 1 1 calc R . . C5B C -0.4347(3) 0.7913(3) 0.2311(2) 0.0456(9) Uani 1 1 d . . . H5B H -0.4514 0.8257 0.2614 0.055 Uiso 1 1 calc R . . C6B C -0.5937(3) 0.7403(4) 0.1681(2) 0.0558(12) Uani 1 1 d . . . H6B H -0.6166 0.8084 0.1607 0.067 Uiso 1 1 calc R . . C7B C -0.6364(4) 0.6825(5) 0.1110(2) 0.0782(18) Uani 1 1 d . . . H7B1 H -0.6185 0.7109 0.0777 0.117 Uiso 1 1 calc R . . H7B2 H -0.7010 0.6852 0.1026 0.117 Uiso 1 1 calc R . . H7B3 H -0.6168 0.6146 0.1164 0.117 Uiso 1 1 calc R . . C8B C -0.6218(3) 0.7027(4) 0.2226(2) 0.0522(11) Uani 1 1 d . . . H8B1 H -0.6868 0.7108 0.2137 0.063 Uiso 1 1 calc R . . H8B2 H -0.5946 0.7460 0.2565 0.063 Uiso 1 1 calc R . . C9B C -0.5990(3) 0.5944(3) 0.24395(19) 0.0448(9) Uani 1 1 d . . . H9B H -0.6341 0.5511 0.2116 0.054 Uiso 1 1 calc R . . C10B C -0.5027(3) 0.5647(3) 0.25575(17) 0.0372(8) Uani 1 1 d . . . C11B C -0.4643(3) 0.5080(3) 0.21678(19) 0.0439(9) Uani 1 1 d . . . H11B H -0.4963 0.4796 0.1802 0.053 Uiso 1 1 calc R . . C12B C -0.3710(3) 0.5020(3) 0.2423(2) 0.0468(10) Uani 1 1 d . . . H12B H -0.3303 0.4704 0.2251 0.056 Uiso 1 1 calc R . . C13B C -0.3491(3) 0.5516(3) 0.29798(18) 0.0419(9) Uani 1 1 d . . . H13B H -0.2912 0.5597 0.3239 0.050 Uiso 1 1 calc R . . C14B C -0.4301(2) 0.5875(3) 0.30822(17) 0.0362(8) Uani 1 1 d . . . C15B C -0.3642(3) 0.6741(3) 0.40520(18) 0.0428(9) Uani 1 1 d . . . H15B H -0.3883 0.6976 0.4380 0.051 Uiso 1 1 calc R . . C16B C -0.3254(3) 0.7655(4) 0.3836(2) 0.0534(11) Uani 1 1 d . . . H16D H -0.2973 0.7473 0.3527 0.080 Uiso 1 1 calc R . . H16E H -0.2813 0.7952 0.4171 0.080 Uiso 1 1 calc R . . H16F H -0.3730 0.8123 0.3674 0.080 Uiso 1 1 calc R . . C17B C -0.2951(3) 0.5956(4) 0.43420(18) 0.0472(10) Uani 1 1 d . . . C18B C -0.2036(3) 0.6129(5) 0.4476(2) 0.0615(13) Uani 1 1 d . . . H18B H -0.1826 0.6745 0.4392 0.074 Uiso 1 1 calc R . . C19B C -0.1433(4) 0.5397(6) 0.4733(3) 0.0789(18) Uani 1 1 d . . . H19B H -0.0816 0.5524 0.4817 0.095 Uiso 1 1 calc R . . C20B C -0.1709(4) 0.4504(6) 0.4865(2) 0.0775(18) Uani 1 1 d . . . H20B H -0.1288 0.4021 0.5045 0.093 Uiso 1 1 calc R . . C21B C -0.2616(4) 0.4307(5) 0.4733(2) 0.0677(14) Uani 1 1 d . . . H21B H -0.2815 0.3686 0.4818 0.081 Uiso 1 1 calc R . . C22B C -0.3226(3) 0.5028(4) 0.4475(2) 0.0550(11) Uani 1 1 d . . . H22B H -0.3841 0.4891 0.4388 0.066 Uiso 1 1 calc R . . C30B C -0.6307(3) 0.5739(3) 0.29929(18) 0.0402(9) Uani 1 1 d . . . C31B C -0.6933(3) 0.6298(3) 0.31970(19) 0.0435(9) Uani 1 1 d . . . H31B H -0.7246 0.6852 0.3005 0.052 Uiso 1 1 calc R . . C32B C -0.7006(3) 0.5880(3) 0.3737(2) 0.0477(10) Uani 1 1 d . . . H32B H -0.7378 0.6105 0.3967 0.057 Uiso 1 1 calc R . . C33B C -0.6429(3) 0.5072(3) 0.38740(19) 0.0452(9) Uani 1 1 d . . . H33B H -0.6346 0.4659 0.4210 0.054 Uiso 1 1 calc R . . C34B C -0.5995(3) 0.4989(3) 0.34192(19) 0.0427(9) Uani 1 1 d . . . H34B H -0.5566 0.4511 0.3402 0.051 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) 0.0351(3) 0.0320(3) 0.0027(2) 0.0147(2) 0.0024(2) Zr1 0.03886(19) 0.03612(19) 0.03049(17) 0.00200(14) 0.01408(14) 0.00310(15) Cl1A 0.0636(6) 0.0437(5) 0.0372(5) 0.0061(4) 0.0233(5) 0.0152(5) Cl2A 0.0745(7) 0.0393(5) 0.0532(6) 0.0076(5) 0.0311(6) 0.0111(5) N1A 0.0335(15) 0.0352(16) 0.0291(14) -0.0019(12) 0.0093(12) 0.0002(12) C1A 0.055(2) 0.040(2) 0.038(2) 0.0066(17) 0.0161(18) 0.0036(18) C2A 0.062(3) 0.054(3) 0.035(2) 0.0086(19) 0.0207(19) 0.008(2) C3A 0.060(3) 0.051(3) 0.050(2) 0.014(2) 0.030(2) 0.008(2) C4A 0.056(3) 0.042(2) 0.056(3) 0.010(2) 0.021(2) -0.005(2) C5A 0.063(3) 0.034(2) 0.042(2) 0.0068(17) 0.017(2) 0.0044(19) C6A 0.052(2) 0.055(3) 0.037(2) 0.0109(19) 0.0121(18) 0.015(2) C7A 0.059(3) 0.094(4) 0.047(3) 0.014(3) 0.008(2) 0.006(3) C8A 0.046(2) 0.059(3) 0.044(2) 0.013(2) 0.0172(19) 0.018(2) C9A 0.036(2) 0.056(3) 0.0327(19) -0.0011(18) 0.0077(16) -0.0014(18) C10A 0.0404(19) 0.0347(19) 0.0334(18) 0.0006(15) 0.0117(15) -0.0027(15) C11A 0.054(2) 0.038(2) 0.036(2) -0.0052(16) 0.0174(18) -0.0041(18) C12A 0.058(3) 0.036(2) 0.044(2) 0.0024(17) 0.0238(19) 0.0096(18) C13A 0.044(2) 0.039(2) 0.0357(19) 0.0060(16) 0.0157(16) 0.0053(16) C14A 0.0377(18) 0.0304(18) 0.0316(17) 0.0048(14) 0.0120(15) 0.0022(14) C15A 0.0364(19) 0.042(2) 0.0347(19) -0.0022(16) 0.0068(15) -0.0027(16) C16A 0.050(2) 0.051(3) 0.049(2) 0.004(2) 0.007(2) -0.009(2) C17A 0.038(2) 0.049(2) 0.0318(18) 0.0061(16) 0.0090(15) 0.0038(17) C18A 0.048(2) 0.061(3) 0.050(3) 0.004(2) 0.002(2) -0.001(2) C19A 0.043(3) 0.096(5) 0.062(3) 0.015(3) -0.002(2) -0.001(3) C20A 0.051(3) 0.081(4) 0.053(3) 0.020(3) 0.014(2) 0.019(3) C21A 0.062(3) 0.056(3) 0.040(2) 0.007(2) 0.018(2) 0.009(2) C22A 0.047(2) 0.051(2) 0.0302(18) 0.0042(17) 0.0117(16) 0.0058(18) C30A 0.0320(18) 0.051(2) 0.039(2) -0.0021(18) 0.0077(16) -0.0047(17) C31A 0.034(2) 0.067(3) 0.043(2) 0.004(2) 0.0127(17) 0.0049(19) C32A 0.041(2) 0.071(3) 0.049(2) 0.001(2) 0.0213(19) -0.003(2) C33A 0.047(2) 0.055(3) 0.053(3) 0.006(2) 0.018(2) -0.011(2) C34A 0.043(2) 0.048(2) 0.039(2) -0.0065(18) 0.0126(17) -0.0102(18) Fe2 0.0382(3) 0.0392(3) 0.0341(3) -0.0012(2) 0.0139(2) -0.0007(2) Zr2 0.0389(2) 0.0371(2) 0.03529(19) -0.00169(15) 0.01524(15) -0.00248(15) Cl1B 0.0641(7) 0.0603(7) 0.0388(5) 0.0034(5) 0.0178(5) -0.0071(5) Cl2B 0.0614(7) 0.0411(6) 0.0602(7) 0.0028(5) 0.0208(5) 0.0027(5) N1B 0.0376(16) 0.0420(18) 0.0337(16) -0.0048(14) 0.0116(13) -0.0034(14) C1B 0.051(2) 0.044(2) 0.041(2) 0.0102(18) 0.0150(18) 0.0065(18) C2B 0.057(3) 0.055(3) 0.036(2) 0.0003(19) 0.0193(19) -0.003(2) C3B 0.050(2) 0.059(3) 0.045(2) 0.012(2) 0.022(2) 0.000(2) C4B 0.056(3) 0.051(3) 0.046(2) 0.004(2) 0.017(2) -0.013(2) C5B 0.058(3) 0.037(2) 0.044(2) 0.0024(18) 0.020(2) -0.0012(19) C6B 0.051(3) 0.069(3) 0.049(3) 0.016(2) 0.015(2) 0.011(2) C7B 0.053(3) 0.127(6) 0.049(3) 0.013(3) 0.004(2) -0.019(3) C8B 0.044(2) 0.066(3) 0.051(3) 0.013(2) 0.021(2) 0.011(2) C9B 0.041(2) 0.055(3) 0.040(2) -0.0044(19) 0.0134(17) -0.0053(19) C10B 0.043(2) 0.038(2) 0.0329(18) -0.0041(15) 0.0143(16) -0.0054(16) C11B 0.054(2) 0.038(2) 0.042(2) -0.0069(17) 0.0181(19) -0.0070(18) C12B 0.057(3) 0.042(2) 0.049(2) 0.0034(19) 0.027(2) 0.0087(19) C13B 0.039(2) 0.048(2) 0.041(2) 0.0048(18) 0.0144(17) 0.0032(17) C14B 0.0367(19) 0.0358(19) 0.0378(19) 0.0000(16) 0.0132(16) -0.0017(15) C15B 0.039(2) 0.053(2) 0.037(2) -0.0028(18) 0.0122(16) -0.0099(18) C16B 0.057(3) 0.059(3) 0.045(2) -0.004(2) 0.016(2) -0.020(2) C17B 0.046(2) 0.067(3) 0.0298(19) 0.0022(19) 0.0123(17) 0.001(2) C18B 0.045(2) 0.091(4) 0.046(3) -0.003(3) 0.007(2) -0.008(3) C19B 0.046(3) 0.119(6) 0.067(4) -0.003(4) 0.006(3) 0.010(3) C20B 0.072(4) 0.109(5) 0.047(3) 0.003(3) 0.009(3) 0.033(4) C21B 0.077(4) 0.077(4) 0.049(3) 0.012(3) 0.019(3) 0.013(3) C22B 0.052(3) 0.068(3) 0.046(2) 0.009(2) 0.015(2) 0.003(2) C30B 0.0360(19) 0.044(2) 0.040(2) -0.0042(17) 0.0097(16) -0.0090(16) C31B 0.036(2) 0.050(2) 0.046(2) -0.0002(18) 0.0131(17) -0.0011(17) C32B 0.041(2) 0.057(3) 0.050(2) 0.002(2) 0.0206(19) -0.0048(19) C33B 0.049(2) 0.044(2) 0.042(2) 0.0046(18) 0.0115(18) -0.0113(18) C34B 0.045(2) 0.039(2) 0.046(2) -0.0059(18) 0.0170(18) -0.0088(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C10A 2.009(4) . ? Fe1 C1A 2.017(4) . ? Fe1 C11A 2.018(4) . ? Fe1 C5A 2.031(4) . ? Fe1 C12A 2.033(4) . ? Fe1 C4A 2.035(4) . ? Fe1 C2A 2.044(4) . ? Fe1 C13A 2.052(4) . ? Fe1 C3A 2.062(4) . ? Fe1 C14A 2.101(3) . ? Zr1 N1A 2.049(3) . ? Zr1 C34A 2.465(4) . ? Zr1 Cl2A 2.4690(11) . ? Zr1 C31A 2.470(4) . ? Zr1 C32A 2.475(4) . ? Zr1 C33A 2.484(4) . ? Zr1 C30A 2.486(4) . ? Zr1 Cl1A 2.5879(11) . ? Zr1 Cl1A 2.6509(10) 3_565 ? Zr1 C15A 2.750(4) . ? Cl1A Zr1 2.6509(10) 3_565 ? N1A C14A 1.399(4) . ? N1A C15A 1.473(5) . ? C1A C5A 1.428(6) . ? C1A C2A 1.431(6) . ? C1A C6A 1.511(6) . ? C2A C3A 1.414(7) . ? C2A H2A 0.9400 . ? C3A C4A 1.405(7) . ? C3A H3A 0.9400 . ? C4A C5A 1.421(6) . ? C4A H4A 0.9400 . ? C5A H5A 0.9400 . ? C6A C7A 1.510(7) . ? C6A C8A 1.543(6) . ? C6A H6A 0.9900 . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C7A H7A3 0.9700 . ? C8A C9A 1.549(6) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C9A C30A 1.512(5) . ? C9A C10A 1.515(5) . ? C9A H9A 0.9900 . ? C10A C11A 1.430(5) . ? C10A C14A 1.443(5) . ? C11A C12A 1.414(6) . ? C11A H11A 0.9400 . ? C12A C13A 1.420(6) . ? C12A H12A 0.9400 . ? C13A C14A 1.434(5) . ? C13A H13A 0.9400 . ? C15A C16A 1.523(6) . ? C15A C17A 1.528(5) . ? C15A H15A 0.9900 . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C16A H16C 0.9700 . ? C17A C22A 1.388(6) . ? C17A C18A 1.389(6) . ? C18A C19A 1.388(7) . ? C18A H18A 0.9400 . ? C19A C20A 1.363(8) . ? C19A H19A 0.9400 . ? C20A C21A 1.385(7) . ? C20A H20A 0.9400 . ? C21A C22A 1.387(6) . ? C21A H21A 0.9400 . ? C22A H22A 0.9400 . ? C30A C34A 1.412(6) . ? C30A C31A 1.421(6) . ? C31A C32A 1.405(6) . ? C31A H31A 0.9400 . ? C32A C33A 1.386(7) . ? C32A H32A 0.9400 . ? C33A C34A 1.407(6) . ? C33A H33A 0.9400 . ? C34A H34A 0.9400 . ? Fe2 C1B 2.011(4) . ? Fe2 C10B 2.015(4) . ? Fe2 C11B 2.023(4) . ? Fe2 C5B 2.027(4) . ? Fe2 C12B 2.040(4) . ? Fe2 C2B 2.045(4) . ? Fe2 C4B 2.052(4) . ? Fe2 C13B 2.057(4) . ? Fe2 C3B 2.064(4) . ? Fe2 C14B 2.080(4) . ? Zr2 N1B 2.031(3) . ? Zr2 Cl2B 2.4009(12) . ? Zr2 Cl1B 2.4106(11) . ? Zr2 C34B 2.469(4) . ? Zr2 C32B 2.471(4) . ? Zr2 C33B 2.474(4) . ? Zr2 C31B 2.475(4) . ? Zr2 C30B 2.490(4) . ? Zr2 C15B 2.802(4) . ? N1B C14B 1.405(5) . ? N1B C15B 1.483(5) . ? C1B C5B 1.417(6) . ? C1B C2B 1.434(6) . ? C1B C6B 1.504(6) . ? C2B C3B 1.411(6) . ? C2B H2B 0.9400 . ? C3B C4B 1.414(6) . ? C3B H3B 0.9400 . ? C4B C5B 1.421(6) . ? C4B H4B 0.9400 . ? C5B H5B 0.9400 . ? C6B C7B 1.524(8) . ? C6B C8B 1.535(6) . ? C6B H6B 0.9900 . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C7B H7B3 0.9700 . ? C8B C9B 1.565(6) . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C9B C10B 1.502(6) . ? C9B C30B 1.521(6) . ? C9B H9B 0.9900 . ? C10B C11B 1.437(5) . ? C10B C14B 1.446(5) . ? C11B C12B 1.410(6) . ? C11B H11B 0.9400 . ? C12B C13B 1.412(6) . ? C12B H12B 0.9400 . ? C13B C14B 1.431(5) . ? C13B H13B 0.9400 . ? C15B C16B 1.527(6) . ? C15B C17B 1.532(6) . ? C15B H15B 0.9900 . ? C16B H16D 0.9700 . ? C16B H16E 0.9700 . ? C16B H16F 0.9700 . ? C17B C18B 1.390(6) . ? C17B C22B 1.395(7) . ? C18B C19B 1.385(8) . ? C18B H18B 0.9400 . ? C19B C20B 1.351(9) . ? C19B H19B 0.9400 . ? C20B C21B 1.385(8) . ? C20B H20B 0.9400 . ? C21B C22B 1.381(7) . ? C21B H21B 0.9400 . ? C22B H22B 0.9400 . ? C30B C34B 1.410(6) . ? C30B C31B 1.416(6) . ? C31B C32B 1.408(6) . ? C31B H31B 0.9400 . ? C32B C33B 1.399(6) . ? C32B H32B 0.9400 . ? C33B C34B 1.405(6) . ? C33B H33B 0.9400 . ? C34B H34B 0.9400 . ? 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 C10A Fe1 C1A 99.81(17) . . ? C10A Fe1 C11A 41.58(15) . . ? C1A Fe1 C11A 113.74(18) . . ? C10A Fe1 C5A 115.64(17) . . ? C1A Fe1 C5A 41.31(17) . . ? C11A Fe1 C5A 150.09(18) . . ? C10A Fe1 C12A 69.65(16) . . ? C1A Fe1 C12A 151.05(18) . . ? C11A Fe1 C12A 40.87(17) . . ? C5A Fe1 C12A 167.49(19) . . ? C10A Fe1 C4A 153.93(17) . . ? C1A Fe1 C4A 69.32(19) . . ? C11A Fe1 C4A 164.42(17) . . ? C5A Fe1 C4A 40.92(18) . . ? C12A Fe1 C4A 130.69(19) . . ? C10A Fe1 C2A 119.96(18) . . ? C1A Fe1 C2A 41.27(17) . . ? C11A Fe1 C2A 103.68(19) . . ? C5A Fe1 C2A 68.57(18) . . ? C12A Fe1 C2A 119.71(18) . . ? C4A Fe1 C2A 68.0(2) . . ? C10A Fe1 C13A 69.44(16) . . ? C1A Fe1 C13A 161.54(16) . . ? C11A Fe1 C13A 68.71(17) . . ? C5A Fe1 C13A 128.71(17) . . ? C12A Fe1 C13A 40.70(16) . . ? C4A Fe1 C13A 113.62(18) . . ? C2A Fe1 C13A 157.17(17) . . ? C10A Fe1 C3A 159.03(18) . . ? C1A Fe1 C3A 69.00(18) . . ? C11A Fe1 C3A 125.26(18) . . ? C5A Fe1 C3A 68.23(18) . . ? C12A Fe1 C3A 111.24(17) . . ? C4A Fe1 C3A 40.11(19) . . ? C2A Fe1 C3A 40.28(18) . . ? C13A Fe1 C3A 125.78(17) . . ? C10A Fe1 C14A 41.03(14) . . ? C1A Fe1 C14A 122.00(15) . . ? C11A Fe1 C14A 68.40(15) . . ? C5A Fe1 C14A 107.83(16) . . ? C12A Fe1 C14A 68.10(15) . . ? C4A Fe1 C14A 124.04(17) . . ? C2A Fe1 C14A 158.58(17) . . ? C13A Fe1 C14A 40.38(14) . . ? C3A Fe1 C14A 159.85(18) . . ? N1A Zr1 C34A 84.06(13) . . ? N1A Zr1 Cl2A 94.41(9) . . ? C34A Zr1 Cl2A 132.61(11) . . ? N1A Zr1 C31A 110.09(13) . . ? C34A Zr1 C31A 54.71(15) . . ? Cl2A Zr1 C31A 82.35(12) . . ? N1A Zr1 C32A 134.81(14) . . ? C34A Zr1 C32A 54.61(15) . . ? Cl2A Zr1 C32A 100.78(13) . . ? C31A Zr1 C32A 33.02(14) . . ? N1A Zr1 C33A 115.61(14) . . ? C34A Zr1 C33A 33.03(14) . . ? Cl2A Zr1 C33A 132.86(12) . . ? C31A Zr1 C33A 54.27(16) . . ? C32A Zr1 C33A 32.46(16) . . ? N1A Zr1 C30A 80.57(12) . . ? C34A Zr1 C30A 33.15(14) . . ? Cl2A Zr1 C30A 99.73(11) . . ? C31A Zr1 C30A 33.32(13) . . ? C32A Zr1 C30A 55.11(14) . . ? C33A Zr1 C30A 54.83(14) . . ? N1A Zr1 Cl1A 90.80(9) . . ? C34A Zr1 Cl1A 86.51(11) . . ? Cl2A Zr1 Cl1A 140.85(4) . . ? C31A Zr1 Cl1A 131.57(12) . . ? C32A Zr1 Cl1A 102.70(12) . . ? C33A Zr1 Cl1A 77.34(12) . . ? C30A Zr1 Cl1A 119.39(11) . . ? N1A Zr1 Cl1A 141.53(9) . 3_565 ? C34A Zr1 Cl1A 128.23(10) . 3_565 ? Cl2A Zr1 Cl1A 78.61(4) . 3_565 ? C31A Zr1 Cl1A 106.41(10) . 3_565 ? C32A Zr1 Cl1A 83.47(11) . 3_565 ? C33A Zr1 Cl1A 95.35(11) . 3_565 ? C30A Zr1 Cl1A 137.80(9) . 3_565 ? Cl1A Zr1 Cl1A 73.49(4) . 3_565 ? N1A Zr1 C15A 31.68(11) . . ? C34A Zr1 C15A 113.14(13) . . ? Cl2A Zr1 C15A 83.73(9) . . ? C31A Zr1 C15A 137.35(13) . . ? C32A Zr1 C15A 166.49(14) . . ? C33A Zr1 C15A 139.89(14) . . ? C30A Zr1 C15A 111.73(12) . . ? Cl1A Zr1 C15A 80.66(9) . . ? Cl1A Zr1 C15A 109.98(9) 3_565 . ? Zr1 Cl1A Zr1 106.51(4) . 3_565 ? C14A N1A C15A 121.5(3) . . ? C14A N1A Zr1 137.1(2) . . ? C15A N1A Zr1 101.4(2) . . ? C5A C1A C2A 106.8(4) . . ? C5A C1A C6A 125.2(4) . . ? C2A C1A C6A 127.9(4) . . ? C5A C1A Fe1 69.9(2) . . ? C2A C1A Fe1 70.4(2) . . ? C6A C1A Fe1 121.5(3) . . ? C3A C2A C1A 108.6(4) . . ? C3A C2A Fe1 70.5(2) . . ? C1A C2A Fe1 68.3(2) . . ? C3A C2A H2A 125.7 . . ? C1A C2A H2A 125.7 . . ? Fe1 C2A H2A 127.0 . . ? C4A C3A C2A 108.0(4) . . ? C4A C3A Fe1 68.9(2) . . ? C2A C3A Fe1 69.2(2) . . ? C4A C3A H3A 126.0 . . ? C2A C3A H3A 126.0 . . ? Fe1 C3A H3A 127.5 . . ? C3A C4A C5A 108.6(4) . . ? C3A C4A Fe1 71.0(3) . . ? C5A C4A Fe1 69.4(2) . . ? C3A C4A H4A 125.7 . . ? C5A C4A H4A 125.7 . . ? Fe1 C4A H4A 125.5 . . ? C4A C5A C1A 107.9(4) . . ? C4A C5A Fe1 69.7(2) . . ? C1A C5A Fe1 68.8(2) . . ? C4A C5A H5A 126.0 . . ? C1A C5A H5A 126.0 . . ? Fe1 C5A H5A 127.1 . . ? C7A C6A C1A 112.5(4) . . ? C7A C6A C8A 113.2(4) . . ? C1A C6A C8A 111.5(3) . . ? C7A C6A H6A 106.3 . . ? C1A C6A H6A 106.3 . . ? C8A C6A H6A 106.3 . . ? C6A C7A H7A1 109.5 . . ? C6A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C6A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C6A C8A C9A 118.0(4) . . ? C6A C8A H8A1 107.8 . . ? C9A C8A H8A1 107.8 . . ? C6A C8A H8A2 107.8 . . ? C9A C8A H8A2 107.8 . . ? H8A1 C8A H8A2 107.2 . . ? C30A C9A C10A 109.4(3) . . ? C30A C9A C8A 110.5(3) . . ? C10A C9A C8A 115.1(3) . . ? C30A C9A H9A 107.1 . . ? C10A C9A H9A 107.1 . . ? C8A C9A H9A 107.1 . . ? C11A C10A C14A 107.5(3) . . ? C11A C10A C9A 127.5(4) . . ? C14A C10A C9A 125.0(3) . . ? C11A C10A Fe1 69.5(2) . . ? C14A C10A Fe1 72.9(2) . . ? C9A C10A Fe1 121.8(3) . . ? C12A C11A C10A 108.5(4) . . ? C12A C11A Fe1 70.1(2) . . ? C10A C11A Fe1 68.9(2) . . ? C12A C11A H11A 125.7 . . ? C10A C11A H11A 125.7 . . ? Fe1 C11A H11A 126.8 . . ? C11A C12A C13A 108.2(3) . . ? C11A C12A Fe1 69.0(2) . . ? C13A C12A Fe1 70.3(2) . . ? C11A C12A H12A 125.9 . . ? C13A C12A H12A 125.9 . . ? Fe1 C12A H12A 126.3 . . ? C12A C13A C14A 108.4(4) . . ? C12A C13A Fe1 69.0(2) . . ? C14A C13A Fe1 71.7(2) . . ? C12A C13A H13A 125.8 . . ? C14A C13A H13A 125.8 . . ? Fe1 C13A H13A 125.2 . . ? N1A C14A C13A 129.7(3) . . ? N1A C14A C10A 122.8(3) . . ? C13A C14A C10A 107.0(3) . . ? N1A C14A Fe1 136.6(3) . . ? C13A C14A Fe1 68.0(2) . . ? C10A C14A Fe1 66.1(2) . . ? N1A C15A C16A 111.9(3) . . ? N1A C15A C17A 116.3(3) . . ? C16A C15A C17A 113.2(3) . . ? N1A C15A Zr1 46.92(16) . . ? C16A C15A Zr1 122.4(3) . . ? C17A C15A Zr1 124.1(3) . . ? N1A C15A H15A 104.7 . . ? C16A C15A H15A 104.7 . . ? C17A C15A H15A 104.7 . . ? Zr1 C15A H15A 57.8 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C22A C17A C18A 117.9(4) . . ? C22A C17A C15A 123.2(4) . . ? C18A C17A C15A 118.9(4) . . ? C19A C18A C17A 120.9(5) . . ? C19A C18A H18A 119.5 . . ? C17A C18A H18A 119.5 . . ? C20A C19A C18A 120.6(5) . . ? C20A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C19A C20A C21A 119.5(5) . . ? C19A C20A H20A 120.3 . . ? C21A C20A H20A 120.3 . . ? C20A C21A C22A 120.2(5) . . ? C20A C21A H21A 119.9 . . ? C22A C21A H21A 119.9 . . ? C21A C22A C17A 120.9(4) . . ? C21A C22A H22A 119.6 . . ? C17A C22A H22A 119.6 . . ? C34A C30A C31A 106.3(4) . . ? C34A C30A C9A 125.8(4) . . ? C31A C30A C9A 127.9(4) . . ? C34A C30A Zr1 72.6(2) . . ? C31A C30A Zr1 72.7(2) . . ? C9A C30A Zr1 119.6(3) . . ? C32A C31A C30A 108.6(4) . . ? C32A C31A Zr1 73.7(3) . . ? C30A C31A Zr1 73.9(2) . . ? C32A C31A H31A 125.7 . . ? C30A C31A H31A 125.7 . . ? Zr1 C31A H31A 118.5 . . ? C33A C32A C31A 108.1(4) . . ? C33A C32A Zr1 74.1(3) . . ? C31A C32A Zr1 73.3(2) . . ? C33A C32A H32A 126.0 . . ? C31A C32A H32A 126.0 . . ? Zr1 C32A H32A 118.5 . . ? C32A C33A C34A 108.5(4) . . ? C32A C33A Zr1 73.4(3) . . ? C34A C33A Zr1 72.7(2) . . ? C32A C33A H33A 125.8 . . ? C34A C33A H33A 125.8 . . ? Zr1 C33A H33A 119.9 . . ? C33A C34A C30A 108.5(4) . . ? C33A C34A Zr1 74.2(3) . . ? C30A C34A Zr1 74.2(2) . . ? C33A C34A H34A 125.7 . . ? C30A C34A H34A 125.7 . . ? Zr1 C34A H34A 117.7 . . ? C1B Fe2 C10B 98.82(17) . . ? C1B Fe2 C11B 112.44(19) . . ? C10B Fe2 C11B 41.69(15) . . ? C1B Fe2 C5B 41.09(18) . . ? C10B Fe2 C5B 112.46(17) . . ? C11B Fe2 C5B 147.11(18) . . ? C1B Fe2 C12B 149.45(19) . . ? C10B Fe2 C12B 69.76(17) . . ? C11B Fe2 C12B 40.62(18) . . ? C5B Fe2 C12B 169.45(19) . . ? C1B Fe2 C2B 41.40(17) . . ? C10B Fe2 C2B 121.21(17) . . ? C11B Fe2 C2B 104.73(18) . . ? C5B Fe2 C2B 68.69(18) . . ? C12B Fe2 C2B 119.66(18) . . ? C1B Fe2 C4B 68.91(19) . . ? C10B Fe2 C4B 150.19(17) . . ? C11B Fe2 C4B 167.95(18) . . ? C5B Fe2 C4B 40.78(18) . . ? C12B Fe2 C4B 133.69(19) . . ? C2B Fe2 C4B 67.92(18) . . ? C1B Fe2 C13B 162.39(17) . . ? C10B Fe2 C13B 69.65(16) . . ? C11B Fe2 C13B 68.26(18) . . ? C5B Fe2 C13B 129.76(18) . . ? C12B Fe2 C13B 40.34(17) . . ? C2B Fe2 C13B 156.13(17) . . ? C4B Fe2 C13B 114.35(18) . . ? C1B Fe2 C3B 68.81(18) . . ? C10B Fe2 C3B 160.95(17) . . ? C11B Fe2 C3B 128.19(18) . . ? C5B Fe2 C3B 68.26(18) . . ? C12B Fe2 C3B 113.27(18) . . ? C2B Fe2 C3B 40.15(18) . . ? C4B Fe2 C3B 40.19(18) . . ? C13B Fe2 C3B 125.62(17) . . ? C1B Fe2 C14B 122.32(16) . . ? C10B Fe2 C14B 41.32(15) . . ? C11B Fe2 C14B 68.38(16) . . ? C5B Fe2 C14B 106.41(16) . . ? C12B Fe2 C14B 68.01(16) . . ? C2B Fe2 C14B 160.13(17) . . ? C4B Fe2 C14B 121.74(17) . . ? C13B Fe2 C14B 40.47(15) . . ? C3B Fe2 C14B 157.70(17) . . ? N1B Zr2 Cl2B 103.66(10) . . ? N1B Zr2 Cl1B 114.93(10) . . ? Cl2B Zr2 Cl1B 100.70(4) . . ? N1B Zr2 C34B 82.43(13) . . ? Cl2B Zr2 C34B 139.06(11) . . ? Cl1B Zr2 C34B 113.41(10) . . ? N1B Zr2 C32B 134.79(14) . . ? Cl2B Zr2 C32B 101.31(12) . . ? Cl1B Zr2 C32B 96.39(11) . . ? C34B Zr2 C32B 54.56(15) . . ? N1B Zr2 C33B 112.90(14) . . ? Cl2B Zr2 C33B 134.17(11) . . ? Cl1B Zr2 C33B 88.36(10) . . ? C34B Zr2 C33B 33.03(13) . . ? C32B Zr2 C33B 32.86(15) . . ? N1B Zr2 C31B 112.34(13) . . ? Cl2B Zr2 C31B 86.68(11) . . ? Cl1B Zr2 C31B 128.55(10) . . ? C34B Zr2 C31B 54.66(15) . . ? C32B Zr2 C31B 33.07(14) . . ? C33B Zr2 C31B 54.75(14) . . ? N1B Zr2 C30B 81.90(13) . . ? Cl2B Zr2 C30B 106.78(10) . . ? Cl1B Zr2 C30B 143.23(10) . . ? C34B Zr2 C30B 33.04(14) . . ? C32B Zr2 C30B 54.90(14) . . ? C33B Zr2 C30B 54.94(14) . . ? C31B Zr2 C30B 33.14(13) . . ? N1B Zr2 C15B 30.81(12) . . ? Cl2B Zr2 C15B 94.01(10) . . ? Cl1B Zr2 C15B 88.79(9) . . ? C34B Zr2 C15B 108.15(13) . . ? C32B Zr2 C15B 162.57(14) . . ? C33B Zr2 C15B 131.33(14) . . ? C31B Zr2 C15B 141.92(13) . . ? C30B Zr2 C15B 112.71(12) . . ? C14B N1B C15B 119.3(3) . . ? C14B N1B Zr2 136.0(3) . . ? C15B N1B Zr2 104.7(2) . . ? C5B C1B C2B 107.4(4) . . ? C5B C1B C6B 125.3(4) . . ? C2B C1B C6B 127.2(4) . . ? C5B C1B Fe2 70.1(2) . . ? C2B C1B Fe2 70.6(2) . . ? C6B C1B Fe2 122.0(3) . . ? C3B C2B C1B 108.1(4) . . ? C3B C2B Fe2 70.7(2) . . ? C1B C2B Fe2 68.0(2) . . ? C3B C2B H2B 126.0 . . ? C1B C2B H2B 126.0 . . ? Fe2 C2B H2B 126.9 . . ? C2B C3B C4B 108.2(4) . . ? C2B C3B Fe2 69.2(2) . . ? C4B C3B Fe2 69.4(2) . . ? C2B C3B H3B 125.9 . . ? C4B C3B H3B 125.9 . . ? Fe2 C3B H3B 127.1 . . ? C3B C4B C5B 108.1(4) . . ? C3B C4B Fe2 70.4(3) . . ? C5B C4B Fe2 68.7(2) . . ? C3B C4B H4B 125.9 . . ? C5B C4B H4B 125.9 . . ? Fe2 C4B H4B 126.6 . . ? C1B C5B C4B 108.2(4) . . ? C1B C5B Fe2 68.9(2) . . ? C4B C5B Fe2 70.6(3) . . ? C1B C5B H5B 125.9 . . ? C4B C5B H5B 125.9 . . ? Fe2 C5B H5B 126.2 . . ? C1B C6B C7B 111.7(4) . . ? C1B C6B C8B 112.4(4) . . ? C7B C6B C8B 112.8(4) . . ? C1B C6B H6B 106.5 . . ? C7B C6B H6B 106.5 . . ? C8B C6B H6B 106.5 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C6B C8B C9B 118.9(4) . . ? C6B C8B H8B1 107.6 . . ? C9B C8B H8B1 107.6 . . ? C6B C8B H8B2 107.6 . . ? C9B C8B H8B2 107.6 . . ? H8B1 C8B H8B2 107.0 . . ? C10B C9B C30B 109.7(3) . . ? C10B C9B C8B 116.0(3) . . ? C30B C9B C8B 109.9(3) . . ? C10B C9B H9B 106.9 . . ? C30B C9B H9B 106.9 . . ? C8B C9B H9B 106.9 . . ? C11B C10B C14B 106.3(3) . . ? C11B C10B C9B 126.6(4) . . ? C14B C10B C9B 127.1(3) . . ? C11B C10B Fe2 69.5(2) . . ? C14B C10B Fe2 71.8(2) . . ? C9B C10B Fe2 123.4(3) . . ? C12B C11B C10B 109.0(4) . . ? C12B C11B Fe2 70.3(2) . . ? C10B C11B Fe2 68.8(2) . . ? C12B C11B H11B 125.5 . . ? C10B C11B H11B 125.5 . . ? Fe2 C11B H11B 127.0 . . ? C11B C12B C13B 108.4(4) . . ? C11B C12B Fe2 69.1(2) . . ? C13B C12B Fe2 70.5(2) . . ? C11B C12B H12B 125.8 . . ? C13B C12B H12B 125.8 . . ? Fe2 C12B H12B 126.2 . . ? C12B C13B C14B 108.3(4) . . ? C12B C13B Fe2 69.2(2) . . ? C14B C13B Fe2 70.7(2) . . ? C12B C13B H13B 125.9 . . ? C14B C13B H13B 125.9 . . ? Fe2 C13B H13B 125.9 . . ? N1B C14B C13B 128.8(4) . . ? N1B C14B C10B 123.3(3) . . ? C13B C14B C10B 107.8(3) . . ? N1B C14B Fe2 131.8(3) . . ? C13B C14B Fe2 68.9(2) . . ? C10B C14B Fe2 66.9(2) . . ? N1B C15B C16B 113.3(3) . . ? N1B C15B C17B 113.0(4) . . ? C16B C15B C17B 114.7(4) . . ? N1B C15B Zr2 44.52(17) . . ? C16B C15B Zr2 122.3(3) . . ? C17B C15B Zr2 123.0(3) . . ? N1B C15B H15B 104.9 . . ? C16B C15B H15B 104.9 . . ? C17B C15B H15B 104.9 . . ? Zr2 C15B H15B 60.3 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18B C17B C22B 117.5(5) . . ? C18B C17B C15B 122.1(5) . . ? C22B C17B C15B 120.4(4) . . ? C19B C18B C17B 120.3(6) . . ? C19B C18B H18B 119.8 . . ? C17B C18B H18B 119.8 . . ? C20B C19B C18B 121.5(6) . . ? C20B C19B H19B 119.2 . . ? C18B C19B H19B 119.2 . . ? C19B C20B C21B 119.5(6) . . ? C19B C20B H20B 120.3 . . ? C21B C20B H20B 120.3 . . ? C22B C21B C20B 119.6(6) . . ? C22B C21B H21B 120.2 . . ? C20B C21B H21B 120.2 . . ? C21B C22B C17B 121.5(5) . . ? C21B C22B H22B 119.3 . . ? C17B C22B H22B 119.3 . . ? C34B C30B C31B 106.8(4) . . ? C34B C30B C9B 126.4(4) . . ? C31B C30B C9B 126.7(4) . . ? C34B C30B Zr2 72.6(2) . . ? C31B C30B Zr2 72.8(2) . . ? C9B C30B Zr2 117.3(3) . . ? C32B C31B C30B 108.2(4) . . ? C32B C31B Zr2 73.3(2) . . ? C30B C31B Zr2 74.0(2) . . ? C32B C31B H31B 125.9 . . ? C30B C31B H31B 125.9 . . ? Zr2 C31B H31B 118.6 . . ? C33B C32B C31B 108.3(4) . . ? C33B C32B Zr2 73.7(2) . . ? C31B C32B Zr2 73.6(2) . . ? C33B C32B H32B 125.8 . . ? C31B C32B H32B 125.8 . . ? Zr2 C32B H32B 118.8 . . ? C32B C33B C34B 107.7(4) . . ? C32B C33B Zr2 73.5(2) . . ? C34B C33B Zr2 73.3(2) . . ? C32B C33B H33B 126.1 . . ? C34B C33B H33B 126.1 . . ? Zr2 C33B H33B 119.0 . . ? C33B C34B C30B 108.9(4) . . ? C33B C34B Zr2 73.7(2) . . ? C30B C34B Zr2 74.3(2) . . ? C33B C34B H34B 125.6 . . ? C30B C34B H34B 125.6 . . ? Zr2 C34B H34B 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Zr1 Cl1A Zr1 -144.34(9) . . . 3_565 ? C34A Zr1 Cl1A Zr1 131.66(10) . . . 3_565 ? Cl2A Zr1 Cl1A Zr1 -46.35(7) . . . 3_565 ? C31A Zr1 Cl1A Zr1 97.52(14) . . . 3_565 ? C32A Zr1 Cl1A Zr1 79.14(12) . . . 3_565 ? C33A Zr1 Cl1A Zr1 99.57(12) . . . 3_565 ? C30A Zr1 Cl1A Zr1 136.05(11) . . . 3_565 ? Cl1A Zr1 Cl1A Zr1 0.0 3_565 . . 3_565 ? C15A Zr1 Cl1A Zr1 -114.20(9) . . . 3_565 ? C34A Zr1 N1A C14A -21.8(4) . . . . ? Cl2A Zr1 N1A C14A 110.6(3) . . . . ? C31A Zr1 N1A C14A 27.2(4) . . . . ? C32A Zr1 N1A C14A 0.7(5) . . . . ? C33A Zr1 N1A C14A -31.9(4) . . . . ? C30A Zr1 N1A C14A 11.5(4) . . . . ? Cl1A Zr1 N1A C14A -108.2(4) . . . . ? Cl1A Zr1 N1A C14A -172.2(3) 3_565 . . . ? C15A Zr1 N1A C14A -178.8(5) . . . . ? C34A Zr1 N1A C15A 157.0(2) . . . . ? Cl2A Zr1 N1A C15A -70.5(2) . . . . ? C31A Zr1 N1A C15A -154.0(2) . . . . ? C32A Zr1 N1A C15A 179.5(2) . . . . ? C33A Zr1 N1A C15A 147.0(2) . . . . ? C30A Zr1 N1A C15A -169.7(2) . . . . ? Cl1A Zr1 N1A C15A 70.6(2) . . . . ? Cl1A Zr1 N1A C15A 6.7(3) 3_565 . . . ? C10A Fe1 C1A C5A -117.9(3) . . . . ? C11A Fe1 C1A C5A -159.1(2) . . . . ? C12A Fe1 C1A C5A 176.7(3) . . . . ? C4A Fe1 C1A C5A 37.4(3) . . . . ? C2A Fe1 C1A C5A 117.2(4) . . . . ? C13A Fe1 C1A C5A -65.4(6) . . . . ? C3A Fe1 C1A C5A 80.5(3) . . . . ? C14A Fe1 C1A C5A -80.6(3) . . . . ? C10A Fe1 C1A C2A 124.8(3) . . . . ? C11A Fe1 C1A C2A 83.7(3) . . . . ? C5A Fe1 C1A C2A -117.2(4) . . . . ? C12A Fe1 C1A C2A 59.5(5) . . . . ? C4A Fe1 C1A C2A -79.8(3) . . . . ? C13A Fe1 C1A C2A 177.4(5) . . . . ? C3A Fe1 C1A C2A -36.7(3) . . . . ? C14A Fe1 C1A C2A 162.2(3) . . . . ? C10A Fe1 C1A C6A 1.7(4) . . . . ? C11A Fe1 C1A C6A -39.4(4) . . . . ? C5A Fe1 C1A C6A 119.7(4) . . . . ? C12A Fe1 C1A C6A -63.7(5) . . . . ? C4A Fe1 C1A C6A 157.1(4) . . . . ? C2A Fe1 C1A C6A -123.1(5) . . . . ? C13A Fe1 C1A C6A 54.3(7) . . . . ? C3A Fe1 C1A C6A -159.8(4) . . . . ? C14A Fe1 C1A C6A 39.1(4) . . . . ? C5A C1A C2A C3A -1.5(5) . . . . ? C6A C1A C2A C3A 174.3(4) . . . . ? Fe1 C1A C2A C3A 59.2(3) . . . . ? C5A C1A C2A Fe1 -60.7(3) . . . . ? C6A C1A C2A Fe1 115.1(4) . . . . ? C10A Fe1 C2A C3A 170.7(3) . . . . ? C1A Fe1 C2A C3A -120.3(4) . . . . ? C11A Fe1 C2A C3A 129.2(3) . . . . ? C5A Fe1 C2A C3A -81.2(3) . . . . ? C12A Fe1 C2A C3A 88.4(3) . . . . ? C4A Fe1 C2A C3A -37.0(3) . . . . ? C13A Fe1 C2A C3A 61.8(6) . . . . ? C14A Fe1 C2A C3A -165.5(4) . . . . ? C10A Fe1 C2A C1A -69.0(3) . . . . ? C11A Fe1 C2A C1A -110.5(3) . . . . ? C5A Fe1 C2A C1A 39.1(3) . . . . ? C12A Fe1 C2A C1A -151.3(3) . . . . ? C4A Fe1 C2A C1A 83.3(3) . . . . ? C13A Fe1 C2A C1A -177.9(4) . . . . ? C3A Fe1 C2A C1A 120.3(4) . . . . ? C14A Fe1 C2A C1A -45.2(6) . . . . ? C1A C2A C3A C4A 0.3(5) . . . . ? Fe1 C2A C3A C4A 58.1(3) . . . . ? C1A C2A C3A Fe1 -57.9(3) . . . . ? C10A Fe1 C3A C4A -143.0(5) . . . . ? C1A Fe1 C3A C4A -82.4(3) . . . . ? C11A Fe1 C3A C4A 172.7(3) . . . . ? C5A Fe1 C3A C4A -37.9(3) . . . . ? C12A Fe1 C3A C4A 128.6(3) . . . . ? C2A Fe1 C3A C4A -120.0(4) . . . . ? C13A Fe1 C3A C4A 84.9(3) . . . . ? C14A Fe1 C3A C4A 44.5(6) . . . . ? C10A Fe1 C3A C2A -23.0(6) . . . . ? C1A Fe1 C3A C2A 37.6(3) . . . . ? C11A Fe1 C3A C2A -67.3(3) . . . . ? C5A Fe1 C3A C2A 82.1(3) . . . . ? C12A Fe1 C3A C2A -111.3(3) . . . . ? C4A Fe1 C3A C2A 120.0(4) . . . . ? C13A Fe1 C3A C2A -155.1(3) . . . . ? C14A Fe1 C3A C2A 164.6(4) . . . . ? C2A C3A C4A C5A 1.1(5) . . . . ? Fe1 C3A C4A C5A 59.4(3) . . . . ? C2A C3A C4A Fe1 -58.3(3) . . . . ? C10A Fe1 C4A C3A 150.6(4) . . . . ? C1A Fe1 C4A C3A 81.6(3) . . . . ? C11A Fe1 C4A C3A -22.8(8) . . . . ? C5A Fe1 C4A C3A 119.4(4) . . . . ? C12A Fe1 C4A C3A -73.8(3) . . . . ? C2A Fe1 C4A C3A 37.1(3) . . . . ? C13A Fe1 C4A C3A -118.1(3) . . . . ? C14A Fe1 C4A C3A -163.0(2) . . . . ? C10A Fe1 C4A C5A 31.3(5) . . . . ? C1A Fe1 C4A C5A -37.8(3) . . . . ? C11A Fe1 C4A C5A -142.2(6) . . . . ? C12A Fe1 C4A C5A 166.8(3) . . . . ? C2A Fe1 C4A C5A -82.2(3) . . . . ? C13A Fe1 C4A C5A 122.5(3) . . . . ? C3A Fe1 C4A C5A -119.4(4) . . . . ? C14A Fe1 C4A C5A 77.6(3) . . . . ? C3A C4A C5A C1A -2.1(5) . . . . ? Fe1 C4A C5A C1A 58.3(3) . . . . ? C3A C4A C5A Fe1 -60.4(3) . . . . ? C2A C1A C5A C4A 2.2(5) . . . . ? C6A C1A C5A C4A -173.8(4) . . . . ? Fe1 C1A C5A C4A -58.8(3) . . . . ? C2A C1A C5A Fe1 61.1(3) . . . . ? C6A C1A C5A Fe1 -115.0(4) . . . . ? C10A Fe1 C5A C4A -165.3(3) . . . . ? C1A Fe1 C5A C4A 119.7(4) . . . . ? C11A Fe1 C5A C4A 160.7(3) . . . . ? C12A Fe1 C5A C4A -52.8(9) . . . . ? C2A Fe1 C5A C4A 80.7(3) . . . . ? C13A Fe1 C5A C4A -81.9(3) . . . . ? C3A Fe1 C5A C4A 37.2(3) . . . . ? C14A Fe1 C5A C4A -121.8(3) . . . . ? C10A Fe1 C5A C1A 74.9(3) . . . . ? C11A Fe1 C5A C1A 41.0(4) . . . . ? C12A Fe1 C5A C1A -172.6(7) . . . . ? C4A Fe1 C5A C1A -119.7(4) . . . . ? C2A Fe1 C5A C1A -39.1(2) . . . . ? C13A Fe1 C5A C1A 158.4(2) . . . . ? C3A Fe1 C5A C1A -82.5(3) . . . . ? C14A Fe1 C5A C1A 118.5(2) . . . . ? C5A C1A C6A C7A -179.9(4) . . . . ? C2A C1A C6A C7A 4.9(6) . . . . ? Fe1 C1A C6A C7A 93.6(4) . . . . ? C5A C1A C6A C8A 51.6(6) . . . . ? C2A C1A C6A C8A -123.5(5) . . . . ? Fe1 C1A C6A C8A -34.8(5) . . . . ? C7A C6A C8A C9A -58.7(5) . . . . ? C1A C6A C8A C9A 69.4(5) . . . . ? C6A C8A C9A C30A 175.0(4) . . . . ? C6A C8A C9A C10A -60.3(5) . . . . ? C30A C9A C10A C11A -129.6(4) . . . . ? C8A C9A C10A C11A 105.2(5) . . . . ? C30A C9A C10A C14A 52.1(5) . . . . ? C8A C9A C10A C14A -73.1(5) . . . . ? C30A C9A C10A Fe1 142.8(3) . . . . ? C8A C9A C10A Fe1 17.6(5) . . . . ? C1A Fe1 C10A C11A -114.9(3) . . . . ? C5A Fe1 C10A C11A -155.2(2) . . . . ? C12A Fe1 C10A C11A 37.1(2) . . . . ? C4A Fe1 C10A C11A -177.4(4) . . . . ? C2A Fe1 C10A C11A -76.2(3) . . . . ? C13A Fe1 C10A C11A 80.7(3) . . . . ? C3A Fe1 C10A C11A -59.3(6) . . . . ? C14A Fe1 C10A C11A 116.8(3) . . . . ? C1A Fe1 C10A C14A 128.4(2) . . . . ? C11A Fe1 C10A C14A -116.8(3) . . . . ? C5A Fe1 C10A C14A 88.0(3) . . . . ? C12A Fe1 C10A C14A -79.6(2) . . . . ? C4A Fe1 C10A C14A 65.9(5) . . . . ? C2A Fe1 C10A C14A 167.0(2) . . . . ? C13A Fe1 C10A C14A -36.1(2) . . . . ? C3A Fe1 C10A C14A -176.1(4) . . . . ? C1A Fe1 C10A C9A 7.4(3) . . . . ? C11A Fe1 C10A C9A 122.3(4) . . . . ? C5A Fe1 C10A C9A -32.9(4) . . . . ? C12A Fe1 C10A C9A 159.4(4) . . . . ? C4A Fe1 C10A C9A -55.1(5) . . . . ? C2A Fe1 C10A C9A 46.0(4) . . . . ? C13A Fe1 C10A C9A -157.0(3) . . . . ? C3A Fe1 C10A C9A 63.0(6) . . . . ? C14A Fe1 C10A C9A -121.0(4) . . . . ? C14A C10A C11A C12A 4.4(4) . . . . ? C9A C10A C11A C12A -174.1(4) . . . . ? Fe1 C10A C11A C12A -59.1(3) . . . . ? C14A C10A C11A Fe1 63.5(3) . . . . ? C9A C10A C11A Fe1 -115.0(4) . . . . ? C10A Fe1 C11A C12A 120.1(3) . . . . ? C1A Fe1 C11A C12A -162.3(2) . . . . ? C5A Fe1 C11A C12A 169.5(3) . . . . ? C4A Fe1 C11A C12A -64.2(8) . . . . ? C2A Fe1 C11A C12A -119.9(2) . . . . ? C13A Fe1 C11A C12A 37.5(2) . . . . ? C3A Fe1 C11A C12A -82.0(3) . . . . ? C14A Fe1 C11A C12A 81.0(2) . . . . ? C1A Fe1 C11A C10A 77.6(3) . . . . ? C5A Fe1 C11A C10A 49.3(4) . . . . ? C12A Fe1 C11A C10A -120.1(3) . . . . ? C4A Fe1 C11A C10A 175.7(6) . . . . ? C2A Fe1 C11A C10A 120.0(2) . . . . ? C13A Fe1 C11A C10A -82.6(2) . . . . ? C3A Fe1 C11A C10A 157.9(2) . . . . ? C14A Fe1 C11A C10A -39.1(2) . . . . ? C10A C11A C12A C13A -1.3(5) . . . . ? Fe1 C11A C12A C13A -59.6(3) . . . . ? C10A C11A C12A Fe1 58.3(3) . . . . ? C10A Fe1 C12A C11A -37.7(2) . . . . ? C1A Fe1 C12A C11A 35.1(4) . . . . ? C5A Fe1 C12A C11A -155.1(7) . . . . ? C4A Fe1 C12A C11A 161.4(3) . . . . ? C2A Fe1 C12A C11A 75.9(3) . . . . ? C13A Fe1 C12A C11A -119.5(3) . . . . ? C3A Fe1 C12A C11A 119.8(3) . . . . ? C14A Fe1 C12A C11A -81.9(2) . . . . ? C10A Fe1 C12A C13A 81.8(2) . . . . ? C1A Fe1 C12A C13A 154.6(3) . . . . ? C11A Fe1 C12A C13A 119.5(3) . . . . ? C5A Fe1 C12A C13A -35.6(9) . . . . ? C4A Fe1 C12A C13A -79.1(3) . . . . ? C2A Fe1 C12A C13A -164.6(2) . . . . ? C3A Fe1 C12A C13A -120.7(3) . . . . ? C14A Fe1 C12A C13A 37.7(2) . . . . ? C11A C12A C13A C14A -2.3(4) . . . . ? Fe1 C12A C13A C14A -61.1(3) . . . . ? C11A C12A C13A Fe1 58.8(3) . . . . ? C10A Fe1 C13A C12A -82.3(3) . . . . ? C1A Fe1 C13A C12A -139.0(5) . . . . ? C11A Fe1 C13A C12A -37.7(2) . . . . ? C5A Fe1 C13A C12A 170.7(3) . . . . ? C4A Fe1 C13A C12A 125.7(3) . . . . ? C2A Fe1 C13A C12A 36.6(6) . . . . ? C3A Fe1 C13A C12A 81.2(3) . . . . ? C14A Fe1 C13A C12A -119.0(3) . . . . ? C10A Fe1 C13A C14A 36.6(2) . . . . ? C1A Fe1 C13A C14A -20.1(7) . . . . ? C11A Fe1 C13A C14A 81.3(2) . . . . ? C5A Fe1 C13A C14A -70.3(3) . . . . ? C12A Fe1 C13A C14A 119.0(3) . . . . ? C4A Fe1 C13A C14A -115.4(2) . . . . ? C2A Fe1 C13A C14A 155.5(4) . . . . ? C3A Fe1 C13A C14A -159.9(2) . . . . ? C15A N1A C14A C13A -28.1(6) . . . . ? Zr1 N1A C14A C13A 150.6(3) . . . . ? C15A N1A C14A C10A 160.5(3) . . . . ? Zr1 N1A C14A C10A -20.8(6) . . . . ? C15A N1A C14A Fe1 71.6(5) . . . . ? Zr1 N1A C14A Fe1 -109.7(4) . . . . ? C12A C13A C14A N1A -167.5(4) . . . . ? Fe1 C13A C14A N1A 133.1(4) . . . . ? C12A C13A C14A C10A 5.0(4) . . . . ? Fe1 C13A C14A C10A -54.4(3) . . . . ? C12A C13A C14A Fe1 59.4(3) . . . . ? C11A C10A C14A N1A 167.4(3) . . . . ? C9A C10A C14A N1A -14.1(6) . . . . ? Fe1 C10A C14A N1A -131.3(3) . . . . ? C11A C10A C14A C13A -5.7(4) . . . . ? C9A C10A C14A C13A 172.8(4) . . . . ? Fe1 C10A C14A C13A 55.6(3) . . . . ? C11A C10A C14A Fe1 -61.3(3) . . . . ? C9A C10A C14A Fe1 117.2(4) . . . . ? C10A Fe1 C14A N1A 113.2(5) . . . . ? C1A Fe1 C14A N1A 47.5(4) . . . . ? C11A Fe1 C14A N1A 152.8(4) . . . . ? C5A Fe1 C14A N1A 4.4(4) . . . . ? C12A Fe1 C14A N1A -163.1(4) . . . . ? C4A Fe1 C14A N1A -37.9(4) . . . . ? C2A Fe1 C14A N1A 81.0(6) . . . . ? C13A Fe1 C14A N1A -125.1(5) . . . . ? C3A Fe1 C14A N1A -70.9(6) . . . . ? C10A Fe1 C14A C13A -121.7(3) . . . . ? C1A Fe1 C14A C13A 172.6(2) . . . . ? C11A Fe1 C14A C13A -82.1(3) . . . . ? C5A Fe1 C14A C13A 129.5(3) . . . . ? C12A Fe1 C14A C13A -37.9(2) . . . . ? C4A Fe1 C14A C13A 87.3(3) . . . . ? C2A Fe1 C14A C13A -153.9(5) . . . . ? C3A Fe1 C14A C13A 54.2(6) . . . . ? C1A Fe1 C14A C10A -65.7(3) . . . . ? C11A Fe1 C14A C10A 39.6(2) . . . . ? C5A Fe1 C14A C10A -108.8(2) . . . . ? C12A Fe1 C14A C10A 83.7(2) . . . . ? C4A Fe1 C14A C10A -151.1(2) . . . . ? C2A Fe1 C14A C10A -32.2(6) . . . . ? C13A Fe1 C14A C10A 121.7(3) . . . . ? C3A Fe1 C14A C10A 175.9(5) . . . . ? C14A N1A C15A C16A -66.4(5) . . . . ? Zr1 N1A C15A C16A 114.5(3) . . . . ? C14A N1A C15A C17A 65.9(5) . . . . ? Zr1 N1A C15A C17A -113.2(3) . . . . ? C14A N1A C15A Zr1 179.1(4) . . . . ? C34A Zr1 C15A N1A -25.0(3) . . . . ? Cl2A Zr1 C15A N1A 109.0(2) . . . . ? C31A Zr1 C15A N1A 37.4(3) . . . . ? C32A Zr1 C15A N1A -1.4(7) . . . . ? C33A Zr1 C15A N1A -49.7(3) . . . . ? C30A Zr1 C15A N1A 11.0(3) . . . . ? Cl1A Zr1 C15A N1A -107.1(2) . . . . ? Cl1A Zr1 C15A N1A -175.6(2) 3_565 . . . ? N1A Zr1 C15A C16A -90.6(4) . . . . ? C34A Zr1 C15A C16A -115.6(3) . . . . ? Cl2A Zr1 C15A C16A 18.3(3) . . . . ? C31A Zr1 C15A C16A -53.2(4) . . . . ? C32A Zr1 C15A C16A -92.1(7) . . . . ? C33A Zr1 C15A C16A -140.4(3) . . . . ? C30A Zr1 C15A C16A -79.7(3) . . . . ? Cl1A Zr1 C15A C16A 162.3(3) . . . . ? Cl1A Zr1 C15A C16A 93.8(3) 3_565 . . . ? N1A Zr1 C15A C17A 95.7(4) . . . . ? C34A Zr1 C15A C17A 70.7(3) . . . . ? Cl2A Zr1 C15A C17A -155.3(3) . . . . ? C31A Zr1 C15A C17A 133.1(3) . . . . ? C32A Zr1 C15A C17A 94.3(7) . . . . ? C33A Zr1 C15A C17A 45.9(4) . . . . ? C30A Zr1 C15A C17A 106.6(3) . . . . ? Cl1A Zr1 C15A C17A -11.4(3) . . . . ? Cl1A Zr1 C15A C17A -79.9(3) 3_565 . . . ? N1A C15A C17A C22A 10.3(5) . . . . ? C16A C15A C17A C22A 142.0(4) . . . . ? Zr1 C15A C17A C22A -43.8(5) . . . . ? N1A C15A C17A C18A -171.7(4) . . . . ? C16A C15A C17A C18A -40.1(5) . . . . ? Zr1 C15A C17A C18A 134.1(3) . . . . ? C22A C17A C18A C19A -3.4(7) . . . . ? C15A C17A C18A C19A 178.6(4) . . . . ? C17A C18A C19A C20A 0.9(8) . . . . ? C18A C19A C20A C21A 1.7(8) . . . . ? C19A C20A C21A C22A -1.8(7) . . . . ? C20A C21A C22A C17A -0.7(6) . . . . ? C18A C17A C22A C21A 3.3(6) . . . . ? C15A C17A C22A C21A -178.8(4) . . . . ? C10A C9A C30A C34A 32.7(5) . . . . ? C8A C9A C30A C34A 160.5(4) . . . . ? C10A C9A C30A C31A -147.0(4) . . . . ? C8A C9A C30A C31A -19.2(6) . . . . ? C10A C9A C30A Zr1 -56.5(4) . . . . ? C8A C9A C30A Zr1 71.3(4) . . . . ? N1A Zr1 C30A C34A -93.6(2) . . . . ? Cl2A Zr1 C30A C34A 173.5(2) . . . . ? C31A Zr1 C30A C34A 114.0(4) . . . . ? C32A Zr1 C30A C34A 77.1(3) . . . . ? C33A Zr1 C30A C34A 37.2(2) . . . . ? Cl1A Zr1 C30A C34A -8.0(3) . . . . ? Cl1A Zr1 C30A C34A 89.8(3) 3_565 . . . ? C15A Zr1 C30A C34A -99.4(2) . . . . ? N1A Zr1 C30A C31A 152.5(3) . . . . ? C34A Zr1 C30A C31A -114.0(4) . . . . ? Cl2A Zr1 C30A C31A 59.6(3) . . . . ? C32A Zr1 C30A C31A -36.9(3) . . . . ? C33A Zr1 C30A C31A -76.8(3) . . . . ? Cl1A Zr1 C30A C31A -122.0(2) . . . . ? Cl1A Zr1 C30A C31A -24.2(3) 3_565 . . . ? C15A Zr1 C30A C31A 146.6(2) . . . . ? N1A Zr1 C30A C9A 28.2(3) . . . . ? C34A Zr1 C30A C9A 121.8(4) . . . . ? Cl2A Zr1 C30A C9A -64.7(3) . . . . ? C31A Zr1 C30A C9A -124.3(5) . . . . ? C32A Zr1 C30A C9A -161.1(4) . . . . ? C33A Zr1 C30A C9A 158.9(4) . . . . ? Cl1A Zr1 C30A C9A 113.7(3) . . . . ? Cl1A Zr1 C30A C9A -148.5(3) 3_565 . . . ? C15A Zr1 C30A C9A 22.4(4) . . . . ? C34A C30A C31A C32A 0.7(5) . . . . ? C9A C30A C31A C32A -179.5(4) . . . . ? Zr1 C30A C31A C32A 66.1(3) . . . . ? C34A C30A C31A Zr1 -65.4(3) . . . . ? C9A C30A C31A Zr1 114.4(4) . . . . ? N1A Zr1 C31A C32A -144.5(3) . . . . ? C34A Zr1 C31A C32A -77.7(3) . . . . ? Cl2A Zr1 C31A C32A 123.6(3) . . . . ? C33A Zr1 C31A C32A -36.8(3) . . . . ? C30A Zr1 C31A C32A -115.5(4) . . . . ? Cl1A Zr1 C31A C32A -34.4(3) . . . . ? Cl1A Zr1 C31A C32A 47.9(3) 3_565 . . . ? C15A Zr1 C31A C32A -164.4(3) . . . . ? N1A Zr1 C31A C30A -29.1(3) . . . . ? C34A Zr1 C31A C30A 37.7(2) . . . . ? Cl2A Zr1 C31A C30A -121.0(3) . . . . ? C32A Zr1 C31A C30A 115.5(4) . . . . ? C33A Zr1 C31A C30A 78.6(3) . . . . ? Cl1A Zr1 C31A C30A 81.1(3) . . . . ? Cl1A Zr1 C31A C30A 163.3(2) 3_565 . . . ? C15A Zr1 C31A C30A -48.9(4) . . . . ? C30A C31A C32A C33A 0.3(5) . . . . ? Zr1 C31A C32A C33A 66.5(3) . . . . ? C30A C31A C32A Zr1 -66.3(3) . . . . ? N1A Zr1 C32A C33A -64.7(3) . . . . ? C34A Zr1 C32A C33A -36.9(3) . . . . ? Cl2A Zr1 C32A C33A -172.2(3) . . . . ? C31A Zr1 C32A C33A -115.0(4) . . . . ? C30A Zr1 C32A C33A -77.8(3) . . . . ? Cl1A Zr1 C32A C33A 39.4(3) . . . . ? Cl1A Zr1 C32A C33A 110.8(3) 3_565 . . . ? C15A Zr1 C32A C33A -63.7(7) . . . . ? N1A Zr1 C32A C31A 50.2(4) . . . . ? C34A Zr1 C32A C31A 78.0(3) . . . . ? Cl2A Zr1 C32A C31A -57.2(3) . . . . ? C33A Zr1 C32A C31A 115.0(4) . . . . ? C30A Zr1 C32A C31A 37.2(3) . . . . ? Cl1A Zr1 C32A C31A 154.3(3) . . . . ? Cl1A Zr1 C32A C31A -134.3(3) 3_565 . . . ? C15A Zr1 C32A C31A 51.3(8) . . . . ? C31A C32A C33A C34A -1.2(5) . . . . ? Zr1 C32A C33A C34A 64.8(3) . . . . ? C31A C32A C33A Zr1 -66.0(3) . . . . ? N1A Zr1 C33A C32A 134.6(3) . . . . ? C34A Zr1 C33A C32A 116.0(4) . . . . ? Cl2A Zr1 C33A C32A 10.5(3) . . . . ? C31A Zr1 C33A C32A 37.5(3) . . . . ? C30A Zr1 C33A C32A 78.7(3) . . . . ? Cl1A Zr1 C33A C32A -140.6(3) . . . . ? Cl1A Zr1 C33A C32A -68.9(3) 3_565 . . . ? C15A Zr1 C33A C32A 161.0(2) . . . . ? N1A Zr1 C33A C34A 18.6(3) . . . . ? Cl2A Zr1 C33A C34A -105.5(3) . . . . ? C31A Zr1 C33A C34A -78.5(3) . . . . ? C32A Zr1 C33A C34A -116.0(4) . . . . ? C30A Zr1 C33A C34A -37.3(3) . . . . ? Cl1A Zr1 C33A C34A 103.4(3) . . . . ? Cl1A Zr1 C33A C34A 175.1(3) 3_565 . . . ? C15A Zr1 C33A C34A 45.0(4) . . . . ? C32A C33A C34A C30A 1.7(5) . . . . ? Zr1 C33A C34A C30A 66.9(3) . . . . ? C32A C33A C34A Zr1 -65.2(3) . . . . ? C31A C30A C34A C33A -1.5(5) . . . . ? C9A C30A C34A C33A 178.8(4) . . . . ? Zr1 C30A C34A C33A -66.9(3) . . . . ? C31A C30A C34A Zr1 65.4(3) . . . . ? C9A C30A C34A Zr1 -114.3(4) . . . . ? N1A Zr1 C34A C33A -163.2(3) . . . . ? Cl2A Zr1 C34A C33A 106.3(3) . . . . ? C31A Zr1 C34A C33A 77.1(3) . . . . ? C32A Zr1 C34A C33A 36.3(3) . . . . ? C30A Zr1 C34A C33A 115.0(4) . . . . ? Cl1A Zr1 C34A C33A -72.0(3) . . . . ? Cl1A Zr1 C34A C33A -6.2(3) 3_565 . . . ? C15A Zr1 C34A C33A -150.3(3) . . . . ? N1A Zr1 C34A C30A 81.8(2) . . . . ? Cl2A Zr1 C34A C30A -8.7(3) . . . . ? C31A Zr1 C34A C30A -38.0(2) . . . . ? C32A Zr1 C34A C30A -78.7(3) . . . . ? C33A Zr1 C34A C30A -115.0(4) . . . . ? Cl1A Zr1 C34A C30A 173.0(2) . . . . ? Cl1A Zr1 C34A C30A -121.2(2) 3_565 . . . ? C15A Zr1 C34A C30A 94.7(2) . . . . ? Cl2B Zr2 N1B C14B -109.4(4) . . . . ? Cl1B Zr2 N1B C14B 141.7(4) . . . . ? C34B Zr2 N1B C14B 29.3(4) . . . . ? C32B Zr2 N1B C14B 12.3(5) . . . . ? C33B Zr2 N1B C14B 42.3(4) . . . . ? C31B Zr2 N1B C14B -17.4(4) . . . . ? C30B Zr2 N1B C14B -4.0(4) . . . . ? C15B Zr2 N1B C14B 176.1(5) . . . . ? Cl2B Zr2 N1B C15B 74.5(2) . . . . ? Cl1B Zr2 N1B C15B -34.4(3) . . . . ? C34B Zr2 N1B C15B -146.7(3) . . . . ? C32B Zr2 N1B C15B -163.8(2) . . . . ? C33B Zr2 N1B C15B -133.7(2) . . . . ? C31B Zr2 N1B C15B 166.5(2) . . . . ? C30B Zr2 N1B C15B 179.9(3) . . . . ? C10B Fe2 C1B C5B 114.2(3) . . . . ? C11B Fe2 C1B C5B 155.3(2) . . . . ? C12B Fe2 C1B C5B 179.0(3) . . . . ? C2B Fe2 C1B C5B -117.7(4) . . . . ? C4B Fe2 C1B C5B -37.6(3) . . . . ? C13B Fe2 C1B C5B 66.7(7) . . . . ? C3B Fe2 C1B C5B -80.8(3) . . . . ? C14B Fe2 C1B C5B 77.5(3) . . . . ? C10B Fe2 C1B C2B -128.1(3) . . . . ? C11B Fe2 C1B C2B -87.0(3) . . . . ? C5B Fe2 C1B C2B 117.7(4) . . . . ? C12B Fe2 C1B C2B -63.3(4) . . . . ? C4B Fe2 C1B C2B 80.1(3) . . . . ? C13B Fe2 C1B C2B -175.7(5) . . . . ? C3B Fe2 C1B C2B 36.9(3) . . . . ? C14B Fe2 C1B C2B -164.8(2) . . . . ? C10B Fe2 C1B C6B -5.7(4) . . . . ? C11B Fe2 C1B C6B 35.4(4) . . . . ? C5B Fe2 C1B C6B -119.9(5) . . . . ? C12B Fe2 C1B C6B 59.1(5) . . . . ? C2B Fe2 C1B C6B 122.4(5) . . . . ? C4B Fe2 C1B C6B -157.5(4) . . . . ? C13B Fe2 C1B C6B -53.3(8) . . . . ? C3B Fe2 C1B C6B 159.3(4) . . . . ? C14B Fe2 C1B C6B -42.5(4) . . . . ? C5B C1B C2B C3B 1.2(5) . . . . ? C6B C1B C2B C3B -175.4(4) . . . . ? Fe2 C1B C2B C3B -59.5(3) . . . . ? C5B C1B C2B Fe2 60.7(3) . . . . ? C6B C1B C2B Fe2 -116.0(4) . . . . ? C1B Fe2 C2B C3B 119.8(4) . . . . ? C10B Fe2 C2B C3B -174.8(3) . . . . ? C11B Fe2 C2B C3B -132.8(3) . . . . ? C5B Fe2 C2B C3B 81.1(3) . . . . ? C12B Fe2 C2B C3B -91.7(3) . . . . ? C4B Fe2 C2B C3B 37.1(3) . . . . ? C13B Fe2 C2B C3B -63.5(5) . . . . ? C14B Fe2 C2B C3B 160.3(4) . . . . ? C10B Fe2 C2B C1B 65.4(3) . . . . ? C11B Fe2 C2B C1B 107.4(3) . . . . ? C5B Fe2 C2B C1B -38.7(3) . . . . ? C12B Fe2 C2B C1B 148.5(3) . . . . ? C4B Fe2 C2B C1B -82.7(3) . . . . ? C13B Fe2 C2B C1B 176.8(4) . . . . ? C3B Fe2 C2B C1B -119.8(4) . . . . ? C14B Fe2 C2B C1B 40.5(6) . . . . ? C1B C2B C3B C4B -0.8(5) . . . . ? Fe2 C2B C3B C4B -58.6(3) . . . . ? C1B C2B C3B Fe2 57.8(3) . . . . ? C1B Fe2 C3B C2B -38.0(3) . . . . ? C10B Fe2 C3B C2B 13.7(7) . . . . ? C11B Fe2 C3B C2B 64.5(3) . . . . ? C5B Fe2 C3B C2B -82.3(3) . . . . ? C12B Fe2 C3B C2B 109.0(3) . . . . ? C4B Fe2 C3B C2B -120.0(4) . . . . ? C13B Fe2 C3B C2B 153.6(3) . . . . ? C14B Fe2 C3B C2B -162.5(4) . . . . ? C1B Fe2 C3B C4B 82.0(3) . . . . ? C10B Fe2 C3B C4B 133.7(5) . . . . ? C11B Fe2 C3B C4B -175.5(3) . . . . ? C5B Fe2 C3B C4B 37.7(3) . . . . ? C12B Fe2 C3B C4B -131.0(3) . . . . ? C2B Fe2 C3B C4B 120.0(4) . . . . ? C13B Fe2 C3B C4B -86.4(3) . . . . ? C14B Fe2 C3B C4B -42.5(6) . . . . ? C2B C3B C4B C5B 0.0(5) . . . . ? Fe2 C3B C4B C5B -58.5(3) . . . . ? C2B C3B C4B Fe2 58.5(3) . . . . ? C1B Fe2 C4B C3B -81.7(3) . . . . ? C10B Fe2 C4B C3B -151.7(3) . . . . ? C11B Fe2 C4B C3B 17.1(10) . . . . ? C5B Fe2 C4B C3B -119.6(4) . . . . ? C12B Fe2 C4B C3B 73.5(4) . . . . ? C2B Fe2 C4B C3B -37.1(3) . . . . ? C13B Fe2 C4B C3B 117.1(3) . . . . ? C14B Fe2 C4B C3B 162.5(3) . . . . ? C1B Fe2 C4B C5B 37.8(3) . . . . ? C10B Fe2 C4B C5B -32.1(5) . . . . ? C11B Fe2 C4B C5B 136.7(9) . . . . ? C12B Fe2 C4B C5B -166.9(3) . . . . ? C2B Fe2 C4B C5B 82.5(3) . . . . ? C13B Fe2 C4B C5B -123.4(3) . . . . ? C3B Fe2 C4B C5B 119.6(4) . . . . ? C14B Fe2 C4B C5B -78.0(3) . . . . ? C2B C1B C5B C4B -1.2(5) . . . . ? C6B C1B C5B C4B 175.5(4) . . . . ? Fe2 C1B C5B C4B 59.8(3) . . . . ? C2B C1B C5B Fe2 -61.1(3) . . . . ? C6B C1B C5B Fe2 115.7(4) . . . . ? C3B C4B C5B C1B 0.8(5) . . . . ? Fe2 C4B C5B C1B -58.8(3) . . . . ? C3B C4B C5B Fe2 59.5(3) . . . . ? C10B Fe2 C5B C1B -77.2(3) . . . . ? C11B Fe2 C5B C1B -45.3(4) . . . . ? C12B Fe2 C5B C1B -177.3(9) . . . . ? C2B Fe2 C5B C1B 38.9(3) . . . . ? C4B Fe2 C5B C1B 119.4(4) . . . . ? C13B Fe2 C5B C1B -158.8(2) . . . . ? C3B Fe2 C5B C1B 82.2(3) . . . . ? C14B Fe2 C5B C1B -120.7(3) . . . . ? C1B Fe2 C5B C4B -119.4(4) . . . . ? C10B Fe2 C5B C4B 163.4(3) . . . . ? C11B Fe2 C5B C4B -164.7(3) . . . . ? C12B Fe2 C5B C4B 63.3(10) . . . . ? C2B Fe2 C5B C4B -80.5(3) . . . . ? C13B Fe2 C5B C4B 81.8(3) . . . . ? C3B Fe2 C5B C4B -37.2(3) . . . . ? C14B Fe2 C5B C4B 119.9(3) . . . . ? C5B C1B C6B C7B -176.9(4) . . . . ? C2B C1B C6B C7B -0.8(7) . . . . ? Fe2 C1B C6B C7B -89.8(5) . . . . ? C5B C1B C6B C8B -48.9(6) . . . . ? C2B C1B C6B C8B 127.2(5) . . . . ? Fe2 C1B C6B C8B 38.2(6) . . . . ? C1B C6B C8B C9B -66.5(6) . . . . ? C7B C6B C8B C9B 60.9(6) . . . . ? C6B C8B C9B C10B 53.3(6) . . . . ? C6B C8B C9B C30B 178.5(4) . . . . ? C30B C9B C10B C11B 133.3(4) . . . . ? C8B C9B C10B C11B -101.4(5) . . . . ? C30B C9B C10B C14B -46.9(6) . . . . ? C8B C9B C10B C14B 78.4(5) . . . . ? C30B C9B C10B Fe2 -138.6(3) . . . . ? C8B C9B C10B Fe2 -13.3(5) . . . . ? C1B Fe2 C10B C11B 114.0(3) . . . . ? C5B Fe2 C10B C11B 154.4(3) . . . . ? C12B Fe2 C10B C11B -36.6(3) . . . . ? C2B Fe2 C10B C11B 76.5(3) . . . . ? C4B Fe2 C10B C11B 176.5(3) . . . . ? C13B Fe2 C10B C11B -79.8(3) . . . . ? C3B Fe2 C10B C11B 66.2(6) . . . . ? C14B Fe2 C10B C11B -116.0(3) . . . . ? C1B Fe2 C10B C14B -130.0(2) . . . . ? C11B Fe2 C10B C14B 116.0(3) . . . . ? C5B Fe2 C10B C14B -89.6(3) . . . . ? C12B Fe2 C10B C14B 79.3(3) . . . . ? C2B Fe2 C10B C14B -167.5(2) . . . . ? C4B Fe2 C10B C14B -67.5(4) . . . . ? C13B Fe2 C10B C14B 36.2(2) . . . . ? C3B Fe2 C10B C14B -177.8(5) . . . . ? C1B Fe2 C10B C9B -7.1(4) . . . . ? C11B Fe2 C10B C9B -121.1(4) . . . . ? C5B Fe2 C10B C9B 33.4(4) . . . . ? C12B Fe2 C10B C9B -157.7(4) . . . . ? C2B Fe2 C10B C9B -44.6(4) . . . . ? C4B Fe2 C10B C9B 55.4(5) . . . . ? C13B Fe2 C10B C9B 159.1(4) . . . . ? C3B Fe2 C10B C9B -54.9(7) . . . . ? C14B Fe2 C10B C9B 122.9(4) . . . . ? C14B C10B C11B C12B -3.9(5) . . . . ? C9B C10B C11B C12B 176.0(4) . . . . ? Fe2 C10B C11B C12B 58.9(3) . . . . ? C14B C10B C11B Fe2 -62.8(3) . . . . ? C9B C10B C11B Fe2 117.0(4) . . . . ? C1B Fe2 C11B C12B 161.7(2) . . . . ? C10B Fe2 C11B C12B -120.7(4) . . . . ? C5B Fe2 C11B C12B -167.9(3) . . . . ? C2B Fe2 C11B C12B 118.7(3) . . . . ? C4B Fe2 C11B C12B 67.7(10) . . . . ? C13B Fe2 C11B C12B -37.3(2) . . . . ? C3B Fe2 C11B C12B 81.7(3) . . . . ? C14B Fe2 C11B C12B -81.0(3) . . . . ? C1B Fe2 C11B C10B -77.6(3) . . . . ? C5B Fe2 C11B C10B -47.3(4) . . . . ? C12B Fe2 C11B C10B 120.7(4) . . . . ? C2B Fe2 C11B C10B -120.7(3) . . . . ? C4B Fe2 C11B C10B -171.6(8) . . . . ? C13B Fe2 C11B C10B 83.4(3) . . . . ? C3B Fe2 C11B C10B -157.7(2) . . . . ? C14B Fe2 C11B C10B 39.7(2) . . . . ? C10B C11B C12B C13B 1.7(5) . . . . ? Fe2 C11B C12B C13B 59.7(3) . . . . ? C10B C11B C12B Fe2 -58.0(3) . . . . ? C1B Fe2 C12B C11B -34.8(4) . . . . ? C10B Fe2 C12B C11B 37.6(2) . . . . ? C5B Fe2 C12B C11B 141.7(9) . . . . ? C2B Fe2 C12B C11B -77.6(3) . . . . ? C4B Fe2 C12B C11B -164.5(3) . . . . ? C13B Fe2 C12B C11B 119.6(3) . . . . ? C3B Fe2 C12B C11B -122.2(3) . . . . ? C14B Fe2 C12B C11B 82.0(3) . . . . ? C1B Fe2 C12B C13B -154.4(3) . . . . ? C10B Fe2 C12B C13B -82.0(2) . . . . ? C11B Fe2 C12B C13B -119.6(3) . . . . ? C5B Fe2 C12B C13B 22.1(10) . . . . ? C2B Fe2 C12B C13B 162.8(2) . . . . ? C4B Fe2 C12B C13B 75.9(3) . . . . ? C3B Fe2 C12B C13B 118.2(3) . . . . ? C14B Fe2 C12B C13B -37.6(2) . . . . ? C11B C12B C13B C14B 1.2(5) . . . . ? Fe2 C12B C13B C14B 60.1(3) . . . . ? C11B C12B C13B Fe2 -58.8(3) . . . . ? C1B Fe2 C13B C12B 133.4(6) . . . . ? C10B Fe2 C13B C12B 82.3(3) . . . . ? C11B Fe2 C13B C12B 37.5(2) . . . . ? C5B Fe2 C13B C12B -174.9(3) . . . . ? C2B Fe2 C13B C12B -39.5(5) . . . . ? C4B Fe2 C13B C12B -129.7(3) . . . . ? C3B Fe2 C13B C12B -84.7(3) . . . . ? C14B Fe2 C13B C12B 119.3(3) . . . . ? C1B Fe2 C13B C14B 14.1(7) . . . . ? C10B Fe2 C13B C14B -36.9(2) . . . . ? C11B Fe2 C13B C14B -81.7(2) . . . . ? C5B Fe2 C13B C14B 65.9(3) . . . . ? C12B Fe2 C13B C14B -119.3(3) . . . . ? C2B Fe2 C13B C14B -158.8(4) . . . . ? C4B Fe2 C13B C14B 111.1(3) . . . . ? C3B Fe2 C13B C14B 156.0(2) . . . . ? C15B N1B C14B C13B 17.1(6) . . . . ? Zr2 N1B C14B C13B -158.5(3) . . . . ? C15B N1B C14B C10B -166.1(4) . . . . ? Zr2 N1B C14B C10B 18.2(6) . . . . ? C15B N1B C14B Fe2 -78.6(5) . . . . ? Zr2 N1B C14B Fe2 105.8(4) . . . . ? C12B C13B C14B N1B 173.5(4) . . . . ? Fe2 C13B C14B N1B -127.3(4) . . . . ? C12B C13B C14B C10B -3.6(5) . . . . ? Fe2 C13B C14B C10B 55.5(3) . . . . ? C12B C13B C14B Fe2 -59.2(3) . . . . ? C11B C10B C14B N1B -172.8(4) . . . . ? C9B C10B C14B N1B 7.4(6) . . . . ? Fe2 C10B C14B N1B 125.9(4) . . . . ? C11B C10B C14B C13B 4.6(4) . . . . ? C9B C10B C14B C13B -175.2(4) . . . . ? Fe2 C10B C14B C13B -56.7(3) . . . . ? C11B C10B C14B Fe2 61.3(3) . . . . ? C9B C10B C14B Fe2 -118.5(4) . . . . ? C1B Fe2 C14B N1B -51.2(4) . . . . ? C10B Fe2 C14B N1B -114.7(4) . . . . ? C11B Fe2 C14B N1B -154.8(4) . . . . ? C5B Fe2 C14B N1B -9.2(4) . . . . ? C12B Fe2 C14B N1B 161.3(4) . . . . ? C2B Fe2 C14B N1B -81.7(6) . . . . ? C4B Fe2 C14B N1B 32.6(4) . . . . ? C13B Fe2 C14B N1B 123.8(5) . . . . ? C3B Fe2 C14B N1B 63.4(6) . . . . ? C1B Fe2 C14B C13B -175.0(3) . . . . ? C10B Fe2 C14B C13B 121.4(3) . . . . ? C11B Fe2 C14B C13B 81.4(3) . . . . ? C5B Fe2 C14B C13B -133.0(3) . . . . ? C12B Fe2 C14B C13B 37.5(3) . . . . ? C2B Fe2 C14B C13B 154.4(5) . . . . ? C4B Fe2 C14B C13B -91.3(3) . . . . ? C3B Fe2 C14B C13B -60.4(5) . . . . ? C1B Fe2 C14B C10B 63.6(3) . . . . ? C11B Fe2 C14B C10B -40.0(2) . . . . ? C5B Fe2 C14B C10B 105.6(2) . . . . ? C12B Fe2 C14B C10B -83.9(3) . . . . ? C2B Fe2 C14B C10B 33.0(6) . . . . ? C4B Fe2 C14B C10B 147.3(3) . . . . ? C13B Fe2 C14B C10B -121.4(3) . . . . ? C3B Fe2 C14B C10B 178.1(4) . . . . ? C14B N1B C15B C16B 70.1(5) . . . . ? Zr2 N1B C15B C16B -113.0(3) . . . . ? C14B N1B C15B C17B -62.5(5) . . . . ? Zr2 N1B C15B C17B 114.4(3) . . . . ? C14B N1B C15B Zr2 -176.9(4) . . . . ? Cl2B Zr2 C15B N1B -110.2(2) . . . . ? Cl1B Zr2 C15B N1B 149.2(2) . . . . ? C34B Zr2 C15B N1B 34.9(3) . . . . ? C32B Zr2 C15B N1B 41.4(6) . . . . ? C33B Zr2 C15B N1B 62.4(3) . . . . ? C31B Zr2 C15B N1B -20.5(4) . . . . ? C30B Zr2 C15B N1B -0.1(3) . . . . ? N1B Zr2 C15B C16B 91.4(4) . . . . ? Cl2B Zr2 C15B C16B -18.8(3) . . . . ? Cl1B Zr2 C15B C16B -119.4(3) . . . . ? C34B Zr2 C15B C16B 126.3(3) . . . . ? C32B Zr2 C15B C16B 132.9(5) . . . . ? C33B Zr2 C15B C16B 153.8(3) . . . . ? C31B Zr2 C15B C16B 71.0(4) . . . . ? C30B Zr2 C15B C16B 91.3(3) . . . . ? N1B Zr2 C15B C17B -90.2(4) . . . . ? Cl2B Zr2 C15B C17B 159.7(3) . . . . ? Cl1B Zr2 C15B C17B 59.0(3) . . . . ? C34B Zr2 C15B C17B -55.3(3) . . . . ? C32B Zr2 C15B C17B -48.7(6) . . . . ? C33B Zr2 C15B C17B -27.7(4) . . . . ? C31B Zr2 C15B C17B -110.6(3) . . . . ? C30B Zr2 C15B C17B -90.3(3) . . . . ? N1B C15B C17B C18B 140.9(4) . . . . ? C16B C15B C17B C18B 9.0(6) . . . . ? Zr2 C15B C17B C18B -169.5(3) . . . . ? N1B C15B C17B C22B -38.4(5) . . . . ? C16B C15B C17B C22B -170.3(4) . . . . ? Zr2 C15B C17B C22B 11.2(5) . . . . ? C22B C17B C18B C19B 0.0(7) . . . . ? C15B C17B C18B C19B -179.3(5) . . . . ? C17B C18B C19B C20B -0.6(9) . . . . ? C18B C19B C20B C21B 1.0(9) . . . . ? C19B C20B C21B C22B -0.8(9) . . . . ? C20B C21B C22B C17B 0.2(8) . . . . ? C18B C17B C22B C21B 0.2(7) . . . . ? C15B C17B C22B C21B 179.5(4) . . . . ? C10B C9B C30B C34B -30.2(6) . . . . ? C8B C9B C30B C34B -158.8(4) . . . . ? C10B C9B C30B C31B 146.0(4) . . . . ? C8B C9B C30B C31B 17.3(6) . . . . ? C10B C9B C30B Zr2 57.7(4) . . . . ? C8B C9B C30B Zr2 -71.0(4) . . . . ? N1B Zr2 C30B C34B 88.6(2) . . . . ? Cl2B Zr2 C30B C34B -169.5(2) . . . . ? Cl1B Zr2 C30B C34B -32.8(3) . . . . ? C32B Zr2 C30B C34B -77.3(3) . . . . ? C33B Zr2 C30B C34B -36.9(2) . . . . ? C31B Zr2 C30B C34B -114.5(3) . . . . ? C15B Zr2 C30B C34B 88.6(2) . . . . ? N1B Zr2 C30B C31B -157.0(3) . . . . ? Cl2B Zr2 C30B C31B -55.1(2) . . . . ? Cl1B Zr2 C30B C31B 81.6(3) . . . . ? C34B Zr2 C30B C31B 114.5(3) . . . . ? C32B Zr2 C30B C31B 37.1(2) . . . . ? C33B Zr2 C30B C31B 77.6(3) . . . . ? C15B Zr2 C30B C31B -156.9(2) . . . . ? N1B Zr2 C30B C9B -34.0(3) . . . . ? Cl2B Zr2 C30B C9B 67.9(3) . . . . ? Cl1B Zr2 C30B C9B -155.4(2) . . . . ? C34B Zr2 C30B C9B -122.6(4) . . . . ? C32B Zr2 C30B C9B 160.1(4) . . . . ? C33B Zr2 C30B C9B -159.5(4) . . . . ? C31B Zr2 C30B C9B 122.9(4) . . . . ? C15B Zr2 C30B C9B -34.0(3) . . . . ? C34B C30B C31B C32B -0.7(5) . . . . ? C9B C30B C31B C32B -177.5(4) . . . . ? Zr2 C30B C31B C32B -65.9(3) . . . . ? C34B C30B C31B Zr2 65.2(3) . . . . ? C9B C30B C31B Zr2 -111.6(4) . . . . ? N1B Zr2 C31B C32B 139.9(3) . . . . ? Cl2B Zr2 C31B C32B -116.7(3) . . . . ? Cl1B Zr2 C31B C32B -15.7(3) . . . . ? C34B Zr2 C31B C32B 77.7(3) . . . . ? C33B Zr2 C31B C32B 36.9(3) . . . . ? C30B Zr2 C31B C32B 115.1(4) . . . . ? C15B Zr2 C31B C32B 151.0(3) . . . . ? N1B Zr2 C31B C30B 24.8(3) . . . . ? Cl2B Zr2 C31B C30B 128.2(2) . . . . ? Cl1B Zr2 C31B C30B -130.8(2) . . . . ? C34B Zr2 C31B C30B -37.5(2) . . . . ? C32B Zr2 C31B C30B -115.1(4) . . . . ? C33B Zr2 C31B C30B -78.2(3) . . . . ? C15B Zr2 C31B C30B 35.9(4) . . . . ? C30B C31B C32B C33B 0.4(5) . . . . ? Zr2 C31B C32B C33B -66.0(3) . . . . ? C30B C31B C32B Zr2 66.4(3) . . . . ? N1B Zr2 C32B C33B 58.2(3) . . . . ? Cl2B Zr2 C32B C33B -179.2(2) . . . . ? Cl1B Zr2 C32B C33B -76.9(3) . . . . ? C34B Zr2 C32B C33B 37.4(2) . . . . ? C31B Zr2 C32B C33B 115.4(4) . . . . ? C30B Zr2 C32B C33B 78.1(3) . . . . ? C15B Zr2 C32B C33B 29.7(6) . . . . ? N1B Zr2 C32B C31B -57.1(3) . . . . ? Cl2B Zr2 C32B C31B 65.4(3) . . . . ? Cl1B Zr2 C32B C31B 167.7(2) . . . . ? C34B Zr2 C32B C31B -78.0(3) . . . . ? C33B Zr2 C32B C31B -115.4(4) . . . . ? C30B Zr2 C32B C31B -37.2(2) . . . . ? C15B Zr2 C32B C31B -85.6(5) . . . . ? C31B C32B C33B C34B 0.2(5) . . . . ? Zr2 C32B C33B C34B -65.8(3) . . . . ? C31B C32B C33B Zr2 66.0(3) . . . . ? N1B Zr2 C33B C32B -139.1(3) . . . . ? Cl2B Zr2 C33B C32B 1.1(3) . . . . ? Cl1B Zr2 C33B C32B 104.5(2) . . . . ? C34B Zr2 C33B C32B -114.9(4) . . . . ? C31B Zr2 C33B C32B -37.1(2) . . . . ? C30B Zr2 C33B C32B -78.0(3) . . . . ? C15B Zr2 C33B C32B -168.6(2) . . . . ? N1B Zr2 C33B C34B -24.2(3) . . . . ? Cl2B Zr2 C33B C34B 116.0(2) . . . . ? Cl1B Zr2 C33B C34B -140.7(3) . . . . ? C32B Zr2 C33B C34B 114.9(4) . . . . ? C31B Zr2 C33B C34B 77.7(3) . . . . ? C30B Zr2 C33B C34B 36.9(2) . . . . ? C15B Zr2 C33B C34B -53.7(3) . . . . ? C32B C33B C34B C30B -0.6(5) . . . . ? Zr2 C33B C34B C30B -66.6(3) . . . . ? C32B C33B C34B Zr2 65.9(3) . . . . ? C31B C30B C34B C33B 0.9(5) . . . . ? C9B C30B C34B C33B 177.6(4) . . . . ? Zr2 C30B C34B C33B 66.2(3) . . . . ? C31B C30B C34B Zr2 -65.3(3) . . . . ? C9B C30B C34B Zr2 111.5(4) . . . . ? N1B Zr2 C34B C33B 157.6(3) . . . . ? Cl2B Zr2 C34B C33B -100.2(3) . . . . ? Cl1B Zr2 C34B C33B 43.7(3) . . . . ? C32B Zr2 C34B C33B -37.2(3) . . . . ? C31B Zr2 C34B C33B -78.0(3) . . . . ? C30B Zr2 C34B C33B -115.6(4) . . . . ? C15B Zr2 C34B C33B 140.4(3) . . . . ? N1B Zr2 C34B C30B -86.8(2) . . . . ? Cl2B Zr2 C34B C30B 15.4(3) . . . . ? Cl1B Zr2 C34B C30B 159.3(2) . . . . ? C32B Zr2 C34B C30B 78.5(3) . . . . ? C33B Zr2 C34B C30B 115.6(4) . . . . ? C31B Zr2 C34B C30B 37.6(2) . . . . ? C15B Zr2 C34B C30B -104.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.368 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.081 # Attachment '13.cif' data_erk3815 _database_code_depnum_ccdc_archive 'CCDC 806924' #TrackingRef '13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 Fe N O' _chemical_formula_weight 463.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 10.501(1) _cell_length_b 13.098(1) _cell_length_c 18.067(1) _cell_angle_alpha 90.00 _cell_angle_beta 113.07(1) _cell_angle_gamma 90.00 _cell_volume 2286.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 4639 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8217 _exptl_absorpt_correction_T_max 0.8758 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14863 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.90 _reflns_number_total 5419 _reflns_number_gt 3495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0786P)^2^+0.8252P] 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 5419 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Fe Fe 0.35117(4) -0.03146(3) 0.33492(2) 0.03079(17) Uani 1 1 d . . . O1 O 0.07641(19) 0.19576(15) 0.29433(12) 0.0298(5) Uani 1 1 d . . . H1 H 0.0142 0.1519 0.2734 0.045 Uiso 1 1 calc R . . N1 N -0.0860(2) 0.0302(2) 0.22729(16) 0.0358(6) Uani 1 1 d . . . C1 C 0.3434(4) -0.0347(3) 0.22209(19) 0.0384(8) Uani 1 1 d . . . C2 C 0.4241(4) -0.1182(3) 0.2677(2) 0.0509(10) Uani 1 1 d . . . H2 H 0.4052 -0.1886 0.2559 0.061 Uiso 1 1 calc R . . C3 C 0.5373(4) -0.0774(4) 0.3336(2) 0.0584(12) Uani 1 1 d . . . H3 H 0.6071 -0.1159 0.3739 0.070 Uiso 1 1 calc R . . C4 C 0.5287(4) 0.0305(3) 0.3293(2) 0.0483(10) Uani 1 1 d . . . H4 H 0.5907 0.0773 0.3662 0.058 Uiso 1 1 calc R . . C5 C 0.4103(3) 0.0558(3) 0.2597(2) 0.0387(8) Uani 1 1 d . . . H5 H 0.3808 0.1231 0.2414 0.046 Uiso 1 1 calc R . . C6 C 0.2064(4) -0.0396(3) 0.1510(2) 0.0485(9) Uani 1 1 d . . . H6 H 0.2208 -0.0039 0.1059 0.058 Uiso 1 1 calc R . . C7 C 0.1620(5) -0.1465(4) 0.1220(3) 0.0753(14) Uani 1 1 d . . . H7A H 0.2311 -0.1780 0.1052 0.113 Uiso 1 1 calc R . . H7B H 0.0724 -0.1445 0.0762 0.113 Uiso 1 1 calc R . . H7C H 0.1537 -0.1867 0.1656 0.113 Uiso 1 1 calc R . . C8 C 0.0911(4) 0.0207(3) 0.16528(19) 0.0422(8) Uani 1 1 d . . . H8A H 0.1266 0.0900 0.1844 0.051 Uiso 1 1 calc R . . H8B H 0.0118 0.0286 0.1129 0.051 Uiso 1 1 calc R . . C9 C 0.0372(3) -0.0262(2) 0.22543(18) 0.0339(7) Uani 1 1 d . . . H9 H 0.0071 -0.0976 0.2075 0.041 Uiso 1 1 calc R . . C10 C 0.1462(3) -0.0316(2) 0.31170(17) 0.0262(6) Uani 1 1 d . . . C11 C 0.2086(3) -0.1257(2) 0.34845(19) 0.0343(7) Uani 1 1 d . . . H11 H 0.1828 -0.1915 0.3254 0.041 Uiso 1 1 calc R . . C12 C 0.3146(3) -0.1052(2) 0.42441(19) 0.0339(7) Uani 1 1 d . . . H12 H 0.3733 -0.1543 0.4605 0.041 Uiso 1 1 calc R . . C13 C 0.3176(3) 0.0025(2) 0.43704(17) 0.0280(6) Uani 1 1 d . . . H13 H 0.3792 0.0375 0.4833 0.034 Uiso 1 1 calc R . . C14 C 0.2122(3) 0.0493(2) 0.36837(17) 0.0235(6) Uani 1 1 d . . . C15 C -0.1901(4) 0.0552(3) 0.1471(2) 0.0543(10) Uani 1 1 d . . . H15A H -0.2735 0.0817 0.1522 0.081 Uiso 1 1 calc R . . H15B H -0.2135 -0.0064 0.1137 0.081 Uiso 1 1 calc R . . H15C H -0.1528 0.1070 0.1219 0.081 Uiso 1 1 calc R . . C16 C -0.1518(4) -0.0328(3) 0.2693(2) 0.0468(9) Uani 1 1 d . . . H16A H -0.2276 0.0056 0.2750 0.070 Uiso 1 1 calc R . . H16B H -0.0833 -0.0509 0.3227 0.070 Uiso 1 1 calc R . . H16C H -0.1885 -0.0951 0.2383 0.070 Uiso 1 1 calc R . . C17 C 0.1703(3) 0.1600(2) 0.37015(17) 0.0256(6) Uani 1 1 d . . . C18 C 0.1135(3) 0.1702(2) 0.43689(18) 0.0282(6) Uani 1 1 d . . . C19 C -0.0022(4) 0.1266(3) 0.4421(2) 0.0395(8) Uani 1 1 d . . . H19 H -0.0600 0.0827 0.4007 0.047 Uiso 1 1 calc R . . C20 C -0.0339(4) 0.1475(3) 0.5090(2) 0.0492(10) Uani 1 1 d . . . H20 H -0.1136 0.1177 0.5128 0.059 Uiso 1 1 calc R . . C21 C 0.0499(4) 0.2111(3) 0.5696(2) 0.0473(9) Uani 1 1 d . . . H21 H 0.0276 0.2248 0.6147 0.057 Uiso 1 1 calc R . . C22 C 0.1653(4) 0.2545(3) 0.5646(2) 0.0405(8) Uani 1 1 d . . . H22 H 0.2228 0.2983 0.6062 0.049 Uiso 1 1 calc R . . C23 C 0.1977(3) 0.2340(2) 0.49846(18) 0.0309(7) Uani 1 1 d . . . C24 C 0.3109(3) 0.2726(2) 0.47730(17) 0.0296(7) Uani 1 1 d . . . C25 C 0.4172(3) 0.3400(2) 0.5171(2) 0.0388(8) Uani 1 1 d . . . H25 H 0.4300 0.3654 0.5688 0.047 Uiso 1 1 calc R . . C26 C 0.5044(3) 0.3698(3) 0.4803(2) 0.0454(9) Uani 1 1 d . . . H26 H 0.5797 0.4142 0.5077 0.054 Uiso 1 1 calc R . . C27 C 0.4833(3) 0.3358(3) 0.4043(2) 0.0416(8) Uani 1 1 d . . . H27 H 0.5412 0.3597 0.3786 0.050 Uiso 1 1 calc R . . C28 C 0.3784(3) 0.2670(2) 0.36488(19) 0.0345(7) Uani 1 1 d . . . H28 H 0.3652 0.2429 0.3128 0.041 Uiso 1 1 calc R . . C29 C 0.2929(3) 0.2334(2) 0.40189(17) 0.0267(6) 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 Fe 0.0307(3) 0.0362(3) 0.0294(3) 0.0048(2) 0.01606(19) 0.0105(2) O1 0.0252(10) 0.0255(11) 0.0322(11) 0.0039(9) 0.0042(8) 0.0009(9) N1 0.0249(13) 0.0369(16) 0.0365(15) -0.0016(12) 0.0021(11) -0.0036(11) C1 0.0456(19) 0.049(2) 0.0303(17) 0.0009(16) 0.0250(15) 0.0077(17) C2 0.069(3) 0.050(2) 0.052(2) 0.0025(19) 0.043(2) 0.021(2) C3 0.044(2) 0.092(3) 0.049(2) 0.020(2) 0.0284(19) 0.036(2) C4 0.0308(17) 0.077(3) 0.043(2) 0.002(2) 0.0212(15) 0.0016(18) C5 0.0411(19) 0.045(2) 0.0370(19) 0.0020(15) 0.0229(15) 0.0027(16) C6 0.055(2) 0.058(2) 0.0353(19) -0.0093(18) 0.0203(17) -0.0053(19) C7 0.063(3) 0.086(3) 0.083(3) -0.046(3) 0.036(2) -0.026(2) C8 0.0396(18) 0.057(2) 0.0238(16) -0.0012(16) 0.0050(13) 0.0007(17) C9 0.0309(16) 0.0321(18) 0.0317(16) -0.0066(14) 0.0046(13) -0.0029(14) C10 0.0263(14) 0.0246(15) 0.0275(15) -0.0007(13) 0.0104(12) 0.0004(12) C11 0.0435(18) 0.0252(16) 0.0382(18) 0.0010(14) 0.0202(15) 0.0025(14) C12 0.0376(17) 0.0355(18) 0.0349(17) 0.0125(15) 0.0209(14) 0.0157(15) C13 0.0237(14) 0.0370(17) 0.0249(15) 0.0007(13) 0.0113(12) 0.0029(13) C14 0.0236(14) 0.0252(15) 0.0234(14) 0.0009(12) 0.0112(11) 0.0026(12) C15 0.0349(19) 0.063(3) 0.045(2) 0.0014(19) -0.0058(16) 0.0000(18) C16 0.0342(18) 0.043(2) 0.059(2) -0.0051(18) 0.0142(16) -0.0137(16) C17 0.0239(14) 0.0249(15) 0.0277(15) 0.0010(12) 0.0098(12) 0.0006(12) C18 0.0296(15) 0.0223(15) 0.0373(17) 0.0028(13) 0.0183(13) 0.0062(13) C19 0.0458(19) 0.0302(18) 0.052(2) -0.0040(16) 0.0301(17) -0.0044(15) C20 0.059(2) 0.037(2) 0.075(3) 0.0054(19) 0.051(2) 0.0045(17) C21 0.074(3) 0.036(2) 0.051(2) 0.0063(17) 0.045(2) 0.0136(19) C22 0.056(2) 0.0342(19) 0.0349(18) -0.0018(15) 0.0222(16) 0.0099(16) C23 0.0373(17) 0.0245(16) 0.0309(16) 0.0032(13) 0.0135(13) 0.0066(13) C24 0.0303(15) 0.0238(16) 0.0306(16) 0.0022(13) 0.0076(12) 0.0034(13) C25 0.0389(18) 0.0328(18) 0.0356(18) -0.0040(15) 0.0046(14) -0.0009(15) C26 0.0275(17) 0.0367(19) 0.057(2) 0.0001(17) 0.0005(15) -0.0098(15) C27 0.0306(17) 0.039(2) 0.054(2) 0.0064(17) 0.0154(15) -0.0063(15) C28 0.0336(16) 0.0362(18) 0.0342(17) 0.0020(14) 0.0138(13) -0.0035(14) C29 0.0239(14) 0.0218(15) 0.0320(16) 0.0032(12) 0.0084(12) 0.0005(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 Fe C1 2.008(3) . ? Fe C2 2.020(3) . ? Fe C10 2.025(3) . ? Fe C11 2.028(3) . ? Fe C12 2.045(3) . ? Fe C5 2.049(3) . ? Fe C3 2.053(3) . ? Fe C13 2.058(3) . ? Fe C4 2.072(3) . ? Fe C14 2.075(3) . ? O1 C17 1.417(3) . ? N1 C16 1.464(4) . ? N1 C15 1.470(4) . ? N1 C9 1.501(4) . ? C1 C5 1.409(5) . ? C1 C2 1.431(5) . ? C1 C6 1.509(5) . ? C2 C3 1.417(6) . ? C3 C4 1.416(6) . ? C4 C5 1.418(5) . ? C6 C7 1.504(5) . ? C6 C8 1.550(5) . ? C8 C9 1.536(5) . ? C9 C10 1.532(4) . ? C10 C11 1.430(4) . ? C10 C14 1.447(4) . ? C11 C12 1.413(5) . ? C12 C13 1.427(4) . ? C13 C14 1.437(4) . ? C14 C17 1.520(4) . ? C17 C29 1.526(4) . ? C17 C18 1.547(4) . ? C18 C19 1.379(4) . ? C18 C23 1.396(4) . ? C19 C20 1.400(5) . ? C20 C21 1.382(5) . ? C21 C22 1.373(5) . ? C22 C23 1.391(4) . ? C23 C24 1.474(4) . ? C24 C25 1.383(4) . ? C24 C29 1.398(4) . ? C25 C26 1.383(5) . ? C26 C27 1.376(5) . ? C27 C28 1.385(4) . ? C28 C29 1.385(4) . ? 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 C1 Fe C2 41.62(14) . . ? C1 Fe C10 99.94(13) . . ? C2 Fe C10 119.84(15) . . ? C1 Fe C11 111.81(14) . . ? C2 Fe C11 101.66(15) . . ? C10 Fe C11 41.33(12) . . ? C1 Fe C12 147.91(14) . . ? C2 Fe C12 116.26(14) . . ? C10 Fe C12 69.49(12) . . ? C11 Fe C12 40.61(13) . . ? C1 Fe C5 40.63(14) . . ? C2 Fe C5 68.31(15) . . ? C10 Fe C5 115.91(12) . . ? C11 Fe C5 148.14(14) . . ? C12 Fe C5 170.86(14) . . ? C1 Fe C3 69.08(14) . . ? C2 Fe C3 40.69(16) . . ? C10 Fe C3 159.44(16) . . ? C11 Fe C3 125.04(16) . . ? C12 Fe C3 110.17(14) . . ? C5 Fe C3 67.60(15) . . ? C1 Fe C13 164.01(13) . . ? C2 Fe C13 154.00(14) . . ? C10 Fe C13 69.18(11) . . ? C11 Fe C13 68.26(12) . . ? C12 Fe C13 40.72(12) . . ? C5 Fe C13 132.58(13) . . ? C3 Fe C13 124.84(14) . . ? C1 Fe C4 68.79(14) . . ? C2 Fe C4 68.33(16) . . ? C10 Fe C4 153.38(14) . . ? C11 Fe C4 164.90(14) . . ? C12 Fe C4 132.45(14) . . ? C5 Fe C4 40.25(14) . . ? C3 Fe C4 40.16(17) . . ? C13 Fe C4 115.61(14) . . ? C1 Fe C14 123.56(12) . . ? C2 Fe C14 159.63(14) . . ? C10 Fe C14 41.32(11) . . ? C11 Fe C14 68.77(12) . . ? C12 Fe C14 68.84(11) . . ? C5 Fe C14 109.84(12) . . ? C3 Fe C14 159.02(16) . . ? C13 Fe C14 40.68(11) . . ? C4 Fe C14 124.30(14) . . ? C16 N1 C15 108.5(3) . . ? C16 N1 C9 108.7(3) . . ? C15 N1 C9 113.7(3) . . ? C5 C1 C2 107.1(3) . . ? C5 C1 C6 125.1(3) . . ? C2 C1 C6 127.6(3) . . ? C5 C1 Fe 71.23(18) . . ? C2 C1 Fe 69.64(18) . . ? C6 C1 Fe 120.8(2) . . ? C3 C2 C1 107.9(4) . . ? C3 C2 Fe 70.9(2) . . ? C1 C2 Fe 68.74(18) . . ? C4 C3 C2 108.4(3) . . ? C4 C3 Fe 70.61(19) . . ? C2 C3 Fe 68.40(19) . . ? C3 C4 C5 107.2(3) . . ? C3 C4 Fe 69.2(2) . . ? C5 C4 Fe 69.01(19) . . ? C1 C5 C4 109.3(3) . . ? C1 C5 Fe 68.14(18) . . ? C4 C5 Fe 70.7(2) . . ? C7 C6 C1 113.5(3) . . ? C7 C6 C8 112.1(3) . . ? C1 C6 C8 112.5(3) . . ? C9 C8 C6 116.3(3) . . ? N1 C9 C10 107.9(2) . . ? N1 C9 C8 112.3(3) . . ? C10 C9 C8 113.8(3) . . ? C11 C10 C14 107.3(3) . . ? C11 C10 C9 122.4(3) . . ? C14 C10 C9 130.2(3) . . ? C11 C10 Fe 69.42(17) . . ? C14 C10 Fe 71.16(16) . . ? C9 C10 Fe 121.4(2) . . ? C12 C11 C10 109.3(3) . . ? C12 C11 Fe 70.34(18) . . ? C10 C11 Fe 69.24(17) . . ? C11 C12 C13 107.6(3) . . ? C11 C12 Fe 69.04(17) . . ? C13 C12 Fe 70.14(17) . . ? C12 C13 C14 108.8(3) . . ? C12 C13 Fe 69.14(16) . . ? C14 C13 Fe 70.28(16) . . ? C13 C14 C10 107.0(2) . . ? C13 C14 C17 121.3(3) . . ? C10 C14 C17 130.6(2) . . ? C13 C14 Fe 69.04(15) . . ? C10 C14 Fe 67.51(15) . . ? C17 C14 Fe 137.29(19) . . ? O1 C17 C14 113.1(2) . . ? O1 C17 C29 108.7(2) . . ? C14 C17 C29 113.6(2) . . ? O1 C17 C18 113.0(2) . . ? C14 C17 C18 107.5(2) . . ? C29 C17 C18 100.3(2) . . ? C19 C18 C23 119.6(3) . . ? C19 C18 C17 129.6(3) . . ? C23 C18 C17 110.8(2) . . ? C18 C19 C20 119.4(3) . . ? C21 C20 C19 120.6(3) . . ? C22 C21 C20 120.1(3) . . ? C21 C22 C23 119.7(3) . . ? C22 C23 C18 120.6(3) . . ? C22 C23 C24 130.6(3) . . ? C18 C23 C24 108.8(2) . . ? C25 C24 C29 121.0(3) . . ? C25 C24 C23 130.7(3) . . ? C29 C24 C23 108.2(3) . . ? C26 C25 C24 118.8(3) . . ? C27 C26 C25 120.7(3) . . ? C26 C27 C28 120.5(3) . . ? C27 C28 C29 119.6(3) . . ? C28 C29 C24 119.2(3) . . ? C28 C29 C17 129.0(3) . . ? C24 C29 C17 111.7(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 C2 Fe C1 C5 -117.2(3) . . . . ? C10 Fe C1 C5 118.50(19) . . . . ? C11 Fe C1 C5 159.82(19) . . . . ? C12 Fe C1 C5 -174.5(2) . . . . ? C3 Fe C1 C5 -79.6(2) . . . . ? C13 Fe C1 C5 72.8(5) . . . . ? C4 Fe C1 C5 -36.4(2) . . . . ? C14 Fe C1 C5 81.5(2) . . . . ? C10 Fe C1 C2 -124.3(2) . . . . ? C11 Fe C1 C2 -83.0(2) . . . . ? C12 Fe C1 C2 -57.2(3) . . . . ? C5 Fe C1 C2 117.2(3) . . . . ? C3 Fe C1 C2 37.6(2) . . . . ? C13 Fe C1 C2 -170.0(4) . . . . ? C4 Fe C1 C2 80.8(2) . . . . ? C14 Fe C1 C2 -161.3(2) . . . . ? C2 Fe C1 C6 122.4(4) . . . . ? C10 Fe C1 C6 -1.9(3) . . . . ? C11 Fe C1 C6 39.5(3) . . . . ? C12 Fe C1 C6 65.2(4) . . . . ? C5 Fe C1 C6 -120.4(4) . . . . ? C3 Fe C1 C6 160.1(3) . . . . ? C13 Fe C1 C6 -47.5(6) . . . . ? C4 Fe C1 C6 -156.8(3) . . . . ? C14 Fe C1 C6 -38.8(3) . . . . ? C5 C1 C2 C3 1.4(4) . . . . ? C6 C1 C2 C3 -174.1(3) . . . . ? Fe C1 C2 C3 -60.3(2) . . . . ? C5 C1 C2 Fe 61.8(2) . . . . ? C6 C1 C2 Fe -113.7(3) . . . . ? C1 Fe C2 C3 119.0(3) . . . . ? C10 Fe C2 C3 -171.3(2) . . . . ? C11 Fe C2 C3 -131.2(2) . . . . ? C12 Fe C2 C3 -90.9(3) . . . . ? C5 Fe C2 C3 80.4(3) . . . . ? C13 Fe C2 C3 -67.3(4) . . . . ? C4 Fe C2 C3 36.9(2) . . . . ? C14 Fe C2 C3 169.2(3) . . . . ? C10 Fe C2 C1 69.8(2) . . . . ? C11 Fe C2 C1 109.8(2) . . . . ? C12 Fe C2 C1 150.1(2) . . . . ? C5 Fe C2 C1 -38.5(2) . . . . ? C3 Fe C2 C1 -119.0(3) . . . . ? C13 Fe C2 C1 173.7(3) . . . . ? C4 Fe C2 C1 -82.0(2) . . . . ? C14 Fe C2 C1 50.2(5) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? Fe C2 C3 C4 -59.4(2) . . . . ? C1 C2 C3 Fe 59.0(2) . . . . ? C1 Fe C3 C4 81.5(2) . . . . ? C2 Fe C3 C4 120.0(3) . . . . ? C10 Fe C3 C4 142.0(4) . . . . ? C11 Fe C3 C4 -175.9(2) . . . . ? C12 Fe C3 C4 -132.8(2) . . . . ? C5 Fe C3 C4 37.7(2) . . . . ? C13 Fe C3 C4 -89.5(2) . . . . ? C14 Fe C3 C4 -49.5(5) . . . . ? C1 Fe C3 C2 -38.5(2) . . . . ? C10 Fe C3 C2 22.0(5) . . . . ? C11 Fe C3 C2 64.1(3) . . . . ? C12 Fe C3 C2 107.2(2) . . . . ? C5 Fe C3 C2 -82.3(2) . . . . ? C13 Fe C3 C2 150.5(2) . . . . ? C4 Fe C3 C2 -120.0(3) . . . . ? C14 Fe C3 C2 -169.5(3) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? Fe C3 C4 C5 -58.7(2) . . . . ? C2 C3 C4 Fe 58.1(2) . . . . ? C1 Fe C4 C3 -82.3(2) . . . . ? C2 Fe C4 C3 -37.4(2) . . . . ? C10 Fe C4 C3 -151.1(3) . . . . ? C11 Fe C4 C3 13.0(6) . . . . ? C12 Fe C4 C3 68.9(3) . . . . ? C5 Fe C4 C3 -119.0(3) . . . . ? C13 Fe C4 C3 114.5(2) . . . . ? C14 Fe C4 C3 160.8(2) . . . . ? C1 Fe C4 C5 36.7(2) . . . . ? C2 Fe C4 C5 81.6(2) . . . . ? C10 Fe C4 C5 -32.1(4) . . . . ? C11 Fe C4 C5 132.0(5) . . . . ? C12 Fe C4 C5 -172.04(19) . . . . ? C3 Fe C4 C5 119.0(3) . . . . ? C13 Fe C4 C5 -126.5(2) . . . . ? C14 Fe C4 C5 -80.2(2) . . . . ? C2 C1 C5 C4 -1.8(3) . . . . ? C6 C1 C5 C4 173.8(3) . . . . ? Fe C1 C5 C4 58.9(2) . . . . ? C2 C1 C5 Fe -60.7(2) . . . . ? C6 C1 C5 Fe 114.9(3) . . . . ? C3 C4 C5 C1 1.6(4) . . . . ? Fe C4 C5 C1 -57.3(2) . . . . ? C3 C4 C5 Fe 58.9(2) . . . . ? C2 Fe C5 C1 39.5(2) . . . . ? C10 Fe C5 C1 -74.2(2) . . . . ? C11 Fe C5 C1 -37.4(3) . . . . ? C12 Fe C5 C1 161.2(7) . . . . ? C3 Fe C5 C1 83.5(2) . . . . ? C13 Fe C5 C1 -159.06(18) . . . . ? C4 Fe C5 C1 121.1(3) . . . . ? C14 Fe C5 C1 -118.82(19) . . . . ? C1 Fe C5 C4 -121.1(3) . . . . ? C2 Fe C5 C4 -81.6(2) . . . . ? C10 Fe C5 C4 164.6(2) . . . . ? C11 Fe C5 C4 -158.5(2) . . . . ? C12 Fe C5 C4 40.1(9) . . . . ? C3 Fe C5 C4 -37.6(2) . . . . ? C13 Fe C5 C4 79.8(3) . . . . ? C14 Fe C5 C4 120.1(2) . . . . ? C5 C1 C6 C7 178.4(3) . . . . ? C2 C1 C6 C7 -6.9(5) . . . . ? Fe C1 C6 C7 -93.9(4) . . . . ? C5 C1 C6 C8 -53.0(4) . . . . ? C2 C1 C6 C8 121.7(4) . . . . ? Fe C1 C6 C8 34.8(4) . . . . ? C7 C6 C8 C9 57.8(4) . . . . ? C1 C6 C8 C9 -71.5(4) . . . . ? C16 N1 C9 C10 -68.1(3) . . . . ? C15 N1 C9 C10 171.0(3) . . . . ? C16 N1 C9 C8 165.8(3) . . . . ? C15 N1 C9 C8 44.8(4) . . . . ? C6 C8 C9 N1 -172.7(3) . . . . ? C6 C8 C9 C10 64.5(4) . . . . ? N1 C9 C10 C11 127.6(3) . . . . ? C8 C9 C10 C11 -107.2(3) . . . . ? N1 C9 C10 C14 -57.0(4) . . . . ? C8 C9 C10 C14 68.2(4) . . . . ? N1 C9 C10 Fe -148.2(2) . . . . ? C8 C9 C10 Fe -22.9(4) . . . . ? C1 Fe C10 C11 111.83(19) . . . . ? C2 Fe C10 C11 72.6(2) . . . . ? C12 Fe C10 C11 -36.68(18) . . . . ? C5 Fe C10 C11 151.34(19) . . . . ? C3 Fe C10 C11 56.2(4) . . . . ? C13 Fe C10 C11 -80.34(19) . . . . ? C4 Fe C10 C11 173.8(3) . . . . ? C14 Fe C10 C11 -117.6(2) . . . . ? C1 Fe C10 C14 -130.60(17) . . . . ? C2 Fe C10 C14 -169.84(18) . . . . ? C11 Fe C10 C14 117.6(2) . . . . ? C12 Fe C10 C14 80.89(18) . . . . ? C5 Fe C10 C14 -91.09(19) . . . . ? C3 Fe C10 C14 173.8(4) . . . . ? C13 Fe C10 C14 37.23(16) . . . . ? C4 Fe C10 C14 -68.6(3) . . . . ? C1 Fe C10 C9 -4.4(3) . . . . ? C2 Fe C10 C9 -43.7(3) . . . . ? C11 Fe C10 C9 -116.2(3) . . . . ? C12 Fe C10 C9 -152.9(3) . . . . ? C5 Fe C10 C9 35.1(3) . . . . ? C3 Fe C10 C9 -60.0(5) . . . . ? C13 Fe C10 C9 163.4(3) . . . . ? C4 Fe C10 C9 57.6(4) . . . . ? C14 Fe C10 C9 126.2(3) . . . . ? C14 C10 C11 C12 -2.4(3) . . . . ? C9 C10 C11 C12 173.9(3) . . . . ? Fe C10 C11 C12 59.1(2) . . . . ? C14 C10 C11 Fe -61.46(19) . . . . ? C9 C10 C11 Fe 114.9(3) . . . . ? C1 Fe C11 C12 159.26(18) . . . . ? C2 Fe C11 C12 117.0(2) . . . . ? C10 Fe C11 C12 -120.7(2) . . . . ? C5 Fe C11 C12 -175.6(2) . . . . ? C3 Fe C11 C12 80.2(2) . . . . ? C13 Fe C11 C12 -37.97(17) . . . . ? C4 Fe C11 C12 70.0(6) . . . . ? C14 Fe C11 C12 -81.83(18) . . . . ? C1 Fe C11 C10 -80.01(19) . . . . ? C2 Fe C11 C10 -122.32(19) . . . . ? C12 Fe C11 C10 120.7(2) . . . . ? C5 Fe C11 C10 -54.8(3) . . . . ? C3 Fe C11 C10 -159.10(19) . . . . ? C13 Fe C11 C10 82.76(18) . . . . ? C4 Fe C11 C10 -169.3(5) . . . . ? C14 Fe C11 C10 38.90(17) . . . . ? C10 C11 C12 C13 1.4(3) . . . . ? Fe C11 C12 C13 59.8(2) . . . . ? C10 C11 C12 Fe -58.4(2) . . . . ? C1 Fe C12 C11 -38.2(3) . . . . ? C2 Fe C12 C11 -76.8(2) . . . . ? C10 Fe C12 C11 37.31(18) . . . . ? C5 Fe C12 C11 165.1(7) . . . . ? C3 Fe C12 C11 -120.7(2) . . . . ? C13 Fe C12 C11 118.8(2) . . . . ? C4 Fe C12 C11 -160.6(2) . . . . ? C14 Fe C12 C11 81.67(19) . . . . ? C1 Fe C12 C13 -157.1(2) . . . . ? C2 Fe C12 C13 164.40(19) . . . . ? C10 Fe C12 C13 -81.54(18) . . . . ? C11 Fe C12 C13 -118.8(2) . . . . ? C5 Fe C12 C13 46.2(8) . . . . ? C3 Fe C12 C13 120.4(2) . . . . ? C4 Fe C12 C13 80.5(2) . . . . ? C14 Fe C12 C13 -37.18(17) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? Fe C12 C13 C14 59.27(19) . . . . ? C11 C12 C13 Fe -59.1(2) . . . . ? C1 Fe C13 C12 131.3(5) . . . . ? C2 Fe C13 C12 -33.4(4) . . . . ? C10 Fe C13 C12 82.37(19) . . . . ? C11 Fe C13 C12 37.87(18) . . . . ? C5 Fe C13 C12 -171.04(19) . . . . ? C3 Fe C13 C12 -80.5(3) . . . . ? C4 Fe C13 C12 -126.2(2) . . . . ? C14 Fe C13 C12 120.2(2) . . . . ? C1 Fe C13 C14 11.1(6) . . . . ? C2 Fe C13 C14 -153.6(3) . . . . ? C10 Fe C13 C14 -37.80(17) . . . . ? C11 Fe C13 C14 -82.30(18) . . . . ? C12 Fe C13 C14 -120.2(2) . . . . ? C5 Fe C13 C14 68.8(2) . . . . ? C3 Fe C13 C14 159.3(2) . . . . ? C4 Fe C13 C14 113.6(2) . . . . ? C12 C13 C14 C10 -1.6(3) . . . . ? Fe C13 C14 C10 56.95(18) . . . . ? C12 C13 C14 C17 168.0(2) . . . . ? Fe C13 C14 C17 -133.5(2) . . . . ? C12 C13 C14 Fe -58.57(19) . . . . ? C11 C10 C14 C13 2.4(3) . . . . ? C9 C10 C14 C13 -173.5(3) . . . . ? Fe C10 C14 C13 -57.91(19) . . . . ? C11 C10 C14 C17 -165.8(3) . . . . ? C9 C10 C14 C17 18.3(5) . . . . ? Fe C10 C14 C17 133.9(3) . . . . ? C11 C10 C14 Fe 60.34(19) . . . . ? C9 C10 C14 Fe -115.6(3) . . . . ? C1 Fe C14 C13 -176.34(19) . . . . ? C2 Fe C14 C13 145.9(4) . . . . ? C10 Fe C14 C13 119.8(2) . . . . ? C11 Fe C14 C13 80.92(19) . . . . ? C12 Fe C14 C13 37.21(18) . . . . ? C5 Fe C14 C13 -133.13(18) . . . . ? C3 Fe C14 C13 -54.1(4) . . . . ? C4 Fe C14 C13 -90.5(2) . . . . ? C1 Fe C14 C10 63.8(2) . . . . ? C2 Fe C14 C10 26.1(4) . . . . ? C11 Fe C14 C10 -38.90(17) . . . . ? C12 Fe C14 C10 -82.61(18) . . . . ? C5 Fe C14 C10 107.05(18) . . . . ? C3 Fe C14 C10 -173.9(4) . . . . ? C13 Fe C14 C10 -119.8(2) . . . . ? C4 Fe C14 C10 149.66(18) . . . . ? C1 Fe C14 C17 -62.4(3) . . . . ? C2 Fe C14 C17 -100.2(5) . . . . ? C10 Fe C14 C17 -126.2(4) . . . . ? C11 Fe C14 C17 -165.1(3) . . . . ? C12 Fe C14 C17 151.2(3) . . . . ? C5 Fe C14 C17 -19.2(3) . . . . ? C3 Fe C14 C17 59.8(5) . . . . ? C13 Fe C14 C17 114.0(4) . . . . ? C4 Fe C14 C17 23.4(4) . . . . ? C13 C14 C17 O1 173.3(2) . . . . ? C10 C14 C17 O1 -19.9(4) . . . . ? Fe C14 C17 O1 80.9(3) . . . . ? C13 C14 C17 C29 48.8(3) . . . . ? C10 C14 C17 C29 -144.4(3) . . . . ? Fe C14 C17 C29 -43.6(4) . . . . ? C13 C14 C17 C18 -61.3(3) . . . . ? C10 C14 C17 C18 105.5(3) . . . . ? Fe C14 C17 C18 -153.7(2) . . . . ? O1 C17 C18 C19 61.0(4) . . . . ? C14 C17 C18 C19 -64.5(4) . . . . ? C29 C17 C18 C19 176.5(3) . . . . ? O1 C17 C18 C23 -119.0(3) . . . . ? C14 C17 C18 C23 115.5(3) . . . . ? C29 C17 C18 C23 -3.5(3) . . . . ? C23 C18 C19 C20 0.3(5) . . . . ? C17 C18 C19 C20 -179.6(3) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C19 C20 C21 C22 0.0(5) . . . . ? C20 C21 C22 C23 -0.1(5) . . . . ? C21 C22 C23 C18 0.3(5) . . . . ? C21 C22 C23 C24 177.8(3) . . . . ? C19 C18 C23 C22 -0.4(4) . . . . ? C17 C18 C23 C22 179.6(3) . . . . ? C19 C18 C23 C24 -178.4(3) . . . . ? C17 C18 C23 C24 1.6(3) . . . . ? C22 C23 C24 C25 0.0(6) . . . . ? C18 C23 C24 C25 177.7(3) . . . . ? C22 C23 C24 C29 -176.4(3) . . . . ? C18 C23 C24 C29 1.3(3) . . . . ? C29 C24 C25 C26 1.2(5) . . . . ? C23 C24 C25 C26 -174.9(3) . . . . ? C24 C25 C26 C27 2.2(5) . . . . ? C25 C26 C27 C28 -3.3(5) . . . . ? C26 C27 C28 C29 1.0(5) . . . . ? C27 C28 C29 C24 2.3(4) . . . . ? C27 C28 C29 C17 178.9(3) . . . . ? C25 C24 C29 C28 -3.4(4) . . . . ? C23 C24 C29 C28 173.4(3) . . . . ? C25 C24 C29 C17 179.5(3) . . . . ? C23 C24 C29 C17 -3.7(3) . . . . ? O1 C17 C29 C28 -53.7(4) . . . . ? C14 C17 C29 C28 73.1(4) . . . . ? C18 C17 C29 C28 -172.4(3) . . . . ? O1 C17 C29 C24 123.0(2) . . . . ? C14 C17 C29 C24 -110.1(3) . . . . ? C18 C17 C29 C24 4.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.056 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.088 # Attachment '14.cif' data_erk4629 _database_code_depnum_ccdc_archive 'CCDC 806925' #TrackingRef '14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 Fe N' _chemical_formula_weight 447.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.4004(2) _cell_length_b 15.8211(4) _cell_length_c 29.6255(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4406.04(18) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12315 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7668 _exptl_absorpt_correction_T_max 0.9332 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32361 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5422 _reflns_number_gt 3193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0745P)^2^+0.1034P] 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 5422 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Fe Fe 0.13831(4) 0.224077(19) 0.394069(12) 0.04146(14) Uani 1 1 d . . . N1 N 0.4035(2) 0.05431(14) 0.31542(7) 0.0506(5) Uani 1 1 d . . . C1 C 0.3083(3) 0.22413(15) 0.43690(9) 0.0495(6) Uani 1 1 d . . . C2 C 0.2834(3) 0.30694(16) 0.41956(9) 0.0593(8) Uani 1 1 d . . . H2 H 0.3488 0.3395 0.4031 0.071 Uiso 1 1 calc R . . C3 C 0.1432(3) 0.33185(17) 0.43138(10) 0.0619(8) Uani 1 1 d . . . H3 H 0.0997 0.3834 0.4237 0.074 Uiso 1 1 calc R . . C4 C 0.0803(3) 0.26600(16) 0.45665(9) 0.0568(7) Uani 1 1 d . . . H4 H -0.0119 0.2655 0.4689 0.068 Uiso 1 1 calc R . . C5 C 0.1836(3) 0.20060(17) 0.45998(8) 0.0518(7) Uani 1 1 d . . . H5 H 0.1705 0.1492 0.4753 0.062 Uiso 1 1 calc R . . C6 C 0.4381(3) 0.16855(15) 0.43080(9) 0.0496(6) Uani 1 1 d . . . H6 H 0.4569 0.1425 0.4606 0.060 Uiso 1 1 calc R . . C7 C 0.5704(3) 0.21932(17) 0.41900(10) 0.0612(8) Uani 1 1 d . . . H7A H 0.5616 0.2413 0.3886 0.092 Uiso 1 1 calc R . . H7B H 0.6535 0.1831 0.4209 0.092 Uiso 1 1 calc R . . H7C H 0.5804 0.2659 0.4400 0.092 Uiso 1 1 calc R . . C8 C 0.4146(3) 0.09458(16) 0.39750(8) 0.0464(6) Uani 1 1 d . . . H8A H 0.3405 0.0576 0.4098 0.056 Uiso 1 1 calc R . . H8B H 0.5026 0.0615 0.3958 0.056 Uiso 1 1 calc R . . C9 C 0.3710(2) 0.12071(14) 0.34905(8) 0.0429(6) Uani 1 1 d . . . H9 H 0.4300 0.1703 0.3410 0.052 Uiso 1 1 calc R . . C10 C 0.2177(2) 0.14884(13) 0.34596(8) 0.0397(6) Uani 1 1 d . . . C11 C 0.1798(3) 0.22893(14) 0.32738(8) 0.0474(6) Uani 1 1 d . . . H11 H 0.2425 0.2663 0.3128 0.057 Uiso 1 1 calc R . . C12 C 0.0343(3) 0.24312(16) 0.33432(9) 0.0513(7) Uani 1 1 d . . . H12 H -0.0162 0.2918 0.3258 0.062 Uiso 1 1 calc R . . C13 C -0.0235(3) 0.17170(14) 0.35634(8) 0.0467(6) Uani 1 1 d . . . H13 H -0.1191 0.1648 0.3649 0.056 Uiso 1 1 calc R . . C14 C 0.0877(3) 0.11203(13) 0.36343(8) 0.0383(5) Uani 1 1 d . . . C15 C 0.5549(3) 0.0320(2) 0.31604(12) 0.0912(12) Uani 1 1 d . . . H15A H 0.5776 -0.0012 0.2895 0.137 Uiso 1 1 calc R . . H15B H 0.5756 -0.0008 0.3429 0.137 Uiso 1 1 calc R . . H15C H 0.6117 0.0832 0.3161 0.137 Uiso 1 1 calc R . . C16 C 0.3687(3) 0.0842(2) 0.27005(9) 0.0626(8) Uani 1 1 d . . . H16A H 0.4252 0.1339 0.2632 0.094 Uiso 1 1 calc R . . H16B H 0.2684 0.0986 0.2686 0.094 Uiso 1 1 calc R . . H16C H 0.3893 0.0401 0.2483 0.094 Uiso 1 1 calc R . . C17 C 0.0604(3) 0.02346(14) 0.38168(8) 0.0407(6) Uani 1 1 d . . . H17 H 0.1458 0.0045 0.3984 0.049 Uiso 1 1 calc R . . C18 C -0.0686(3) 0.01357(14) 0.41214(8) 0.0426(6) Uani 1 1 d . . . C19 C -0.1031(3) 0.05376(17) 0.45200(9) 0.0563(7) Uani 1 1 d . . . H19 H -0.0437 0.0964 0.4636 0.068 Uiso 1 1 calc R . . C20 C -0.2262(3) 0.03068(17) 0.47484(9) 0.0593(8) Uani 1 1 d . . . H20 H -0.2509 0.0584 0.5018 0.071 Uiso 1 1 calc R . . C21 C -0.3125(3) -0.03255(17) 0.45830(10) 0.0583(7) Uani 1 1 d . . . H21 H -0.3945 -0.0483 0.4744 0.070 Uiso 1 1 calc R . . C22 C -0.2797(3) -0.07285(17) 0.41854(9) 0.0554(7) Uani 1 1 d . . . H22 H -0.3388 -0.1160 0.4073 0.066 Uiso 1 1 calc R . . C23 C -0.1592(3) -0.04920(16) 0.39531(8) 0.0444(6) Uani 1 1 d . . . C24 C -0.1002(3) -0.08136(14) 0.35278(8) 0.0443(6) Uani 1 1 d . . . C25 C -0.1508(3) -0.14322(16) 0.32341(10) 0.0543(7) Uani 1 1 d . . . H25 H -0.2383 -0.1701 0.3289 0.065 Uiso 1 1 calc R . . C26 C -0.0701(3) -0.16424(16) 0.28620(9) 0.0578(7) Uani 1 1 d . . . H26 H -0.1035 -0.2054 0.2659 0.069 Uiso 1 1 calc R . . C27 C 0.0595(3) -0.12538(16) 0.27839(9) 0.0544(7) Uani 1 1 d . . . H27 H 0.1141 -0.1411 0.2532 0.065 Uiso 1 1 calc R . . C28 C 0.1096(3) -0.06353(16) 0.30743(8) 0.0473(6) Uani 1 1 d . . . H28 H 0.1976 -0.0372 0.3020 0.057 Uiso 1 1 calc R . . C29 C 0.0284(3) -0.04097(13) 0.34441(8) 0.0413(6) 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 Fe 0.0499(3) 0.0350(2) 0.0395(2) -0.00024(14) 0.00234(17) 0.00613(15) N1 0.0496(13) 0.0607(14) 0.0415(13) -0.0096(10) 0.0026(10) 0.0121(10) C1 0.0595(17) 0.0495(15) 0.0394(14) -0.0086(11) -0.0056(13) 0.0030(13) C2 0.072(2) 0.0440(15) 0.0622(19) -0.0072(13) 0.0003(16) -0.0100(14) C3 0.073(2) 0.0404(14) 0.072(2) -0.0122(14) -0.0068(16) 0.0090(13) C4 0.0654(19) 0.0591(17) 0.0460(16) -0.0143(13) 0.0030(14) 0.0106(15) C5 0.0627(18) 0.0549(15) 0.0379(15) -0.0061(12) -0.0035(13) 0.0032(13) C6 0.0540(17) 0.0549(15) 0.0399(14) 0.0016(11) -0.0058(12) 0.0022(13) C7 0.0516(18) 0.0658(18) 0.066(2) -0.0031(15) -0.0057(16) -0.0074(13) C8 0.0449(14) 0.0499(14) 0.0443(15) -0.0018(12) -0.0041(12) 0.0084(12) C9 0.0412(15) 0.0452(13) 0.0425(14) -0.0021(11) 0.0047(11) 0.0034(11) C10 0.0472(15) 0.0400(12) 0.0320(12) 0.0008(10) 0.0008(11) 0.0060(11) C11 0.0546(17) 0.0502(16) 0.0374(14) 0.0057(11) 0.0048(12) 0.0009(12) C12 0.0589(18) 0.0484(14) 0.0465(16) 0.0101(12) -0.0007(14) 0.0148(13) C13 0.0472(15) 0.0519(14) 0.0410(14) 0.0025(11) 0.0001(12) 0.0084(12) C14 0.0452(14) 0.0397(12) 0.0299(12) -0.0008(10) 0.0006(11) 0.0068(11) C15 0.067(2) 0.139(3) 0.068(2) -0.034(2) -0.0034(18) 0.043(2) C16 0.065(2) 0.080(2) 0.0432(17) -0.0047(14) 0.0069(14) 0.0056(14) C17 0.0431(15) 0.0403(13) 0.0388(14) 0.0001(10) -0.0033(11) 0.0021(11) C18 0.0498(16) 0.0423(13) 0.0357(13) 0.0056(10) -0.0008(12) 0.0068(11) C19 0.0703(19) 0.0544(16) 0.0443(16) 0.0023(13) 0.0099(14) -0.0035(14) C20 0.068(2) 0.0664(19) 0.0433(16) 0.0039(13) 0.0114(14) 0.0123(15) C21 0.0574(17) 0.0647(18) 0.0529(18) 0.0191(14) 0.0098(15) 0.0030(15) C22 0.0528(18) 0.0559(16) 0.0573(18) 0.0097(14) -0.0002(14) 0.0018(13) C23 0.0419(15) 0.0485(14) 0.0428(14) 0.0111(11) -0.0006(12) 0.0042(11) C24 0.0465(16) 0.0437(13) 0.0425(15) 0.0035(11) -0.0041(11) 0.0063(11) C25 0.0515(17) 0.0527(15) 0.0585(18) 0.0022(13) -0.0119(14) -0.0038(12) C26 0.072(2) 0.0537(16) 0.0481(16) -0.0099(13) -0.0141(15) 0.0053(15) C27 0.065(2) 0.0559(16) 0.0426(15) -0.0052(12) -0.0039(14) 0.0106(14) C28 0.0517(16) 0.0461(14) 0.0440(15) -0.0009(12) -0.0002(12) 0.0050(11) C29 0.0453(15) 0.0389(12) 0.0396(14) 0.0022(10) -0.0032(11) 0.0082(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 Fe C10 2.001(2) . ? Fe C11 2.015(3) . ? Fe C3 2.033(3) . ? Fe C5 2.033(3) . ? Fe C2 2.037(3) . ? Fe C1 2.040(3) . ? Fe C4 2.043(3) . ? Fe C12 2.045(3) . ? Fe C14 2.047(2) . ? Fe C13 2.062(3) . ? N1 C16 1.462(3) . ? N1 C15 1.467(3) . ? N1 C9 1.480(3) . ? C1 C5 1.407(4) . ? C1 C2 1.427(4) . ? C1 C6 1.515(4) . ? C2 C3 1.419(4) . ? C3 C4 1.412(4) . ? C4 C5 1.422(4) . ? C6 C7 1.521(4) . ? C6 C8 1.547(3) . ? C8 C9 1.549(3) . ? C9 C10 1.511(3) . ? C10 C11 1.427(3) . ? C10 C14 1.449(3) . ? C11 C12 1.401(4) . ? C12 C13 1.413(3) . ? C13 C14 1.424(3) . ? C14 C17 1.524(3) . ? C17 C18 1.520(3) . ? C17 C29 1.533(3) . ? C18 C19 1.380(3) . ? C18 C23 1.400(4) . ? C19 C20 1.390(3) . ? C20 C21 1.378(4) . ? C21 C22 1.374(4) . ? C22 C23 1.378(3) . ? C23 C24 1.467(3) . ? C24 C29 1.390(3) . ? C24 C25 1.393(3) . ? C25 C26 1.379(4) . ? C26 C27 1.385(4) . ? C27 C28 1.385(3) . ? C28 C29 1.382(3) . ? 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 C10 Fe C11 41.62(9) . . ? C10 Fe C3 151.37(11) . . ? C11 Fe C3 119.79(11) . . ? C10 Fe C5 119.81(10) . . ? C11 Fe C5 155.26(12) . . ? C3 Fe C5 68.04(12) . . ? C10 Fe C2 113.39(11) . . ? C11 Fe C2 102.10(12) . . ? C3 Fe C2 40.82(11) . . ? C5 Fe C2 67.74(11) . . ? C10 Fe C1 98.68(10) . . ? C11 Fe C1 117.27(11) . . ? C3 Fe C1 69.12(11) . . ? C5 Fe C1 40.42(11) . . ? C2 Fe C1 40.96(10) . . ? C10 Fe C4 159.85(10) . . ? C11 Fe C4 158.26(10) . . ? C3 Fe C4 40.55(11) . . ? C5 Fe C4 40.84(11) . . ? C2 Fe C4 68.48(12) . . ? C1 Fe C4 69.17(11) . . ? C10 Fe C12 69.48(10) . . ? C11 Fe C12 40.36(11) . . ? C3 Fe C12 110.99(11) . . ? C5 Fe C12 163.49(11) . . ? C2 Fe C12 123.12(11) . . ? C1 Fe C12 155.90(12) . . ? C4 Fe C12 127.61(12) . . ? C10 Fe C14 41.93(9) . . ? C11 Fe C14 69.10(9) . . ? C3 Fe C14 166.57(11) . . ? C5 Fe C14 108.44(10) . . ? C2 Fe C14 151.29(11) . . ? C1 Fe C14 117.25(9) . . ? C4 Fe C14 128.42(11) . . ? C12 Fe C14 68.45(10) . . ? C10 Fe C13 69.52(9) . . ? C11 Fe C13 68.07(11) . . ? C3 Fe C13 130.46(11) . . ? C5 Fe C13 127.01(11) . . ? C2 Fe C13 162.51(10) . . ? C1 Fe C13 156.23(9) . . ? C4 Fe C13 115.19(12) . . ? C12 Fe C13 40.27(10) . . ? C14 Fe C13 40.56(9) . . ? C16 N1 C15 107.9(2) . . ? C16 N1 C9 110.1(2) . . ? C15 N1 C9 111.3(2) . . ? C5 C1 C2 106.3(2) . . ? C5 C1 C6 125.1(2) . . ? C2 C1 C6 128.5(3) . . ? C5 C1 Fe 69.49(16) . . ? C2 C1 Fe 69.38(15) . . ? C6 C1 Fe 123.81(17) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe 69.44(16) . . ? C1 C2 Fe 69.66(15) . . ? C4 C3 C2 108.3(2) . . ? C4 C3 Fe 70.12(15) . . ? C2 C3 Fe 69.75(15) . . ? C3 C4 C5 106.7(3) . . ? C3 C4 Fe 69.33(16) . . ? C5 C4 Fe 69.19(15) . . ? C1 C5 C4 110.0(3) . . ? C1 C5 Fe 70.09(15) . . ? C4 C5 Fe 69.97(15) . . ? C1 C6 C7 112.3(2) . . ? C1 C6 C8 113.6(2) . . ? C7 C6 C8 111.7(2) . . ? C6 C8 C9 115.3(2) . . ? N1 C9 C10 111.41(19) . . ? N1 C9 C8 112.34(19) . . ? C10 C9 C8 112.8(2) . . ? C11 C10 C14 106.5(2) . . ? C11 C10 C9 121.6(2) . . ? C14 C10 C9 131.6(2) . . ? C11 C10 Fe 69.72(13) . . ? C14 C10 Fe 70.74(12) . . ? C9 C10 Fe 119.20(16) . . ? C12 C11 C10 109.3(2) . . ? C12 C11 Fe 70.94(15) . . ? C10 C11 Fe 68.67(13) . . ? C11 C12 C13 108.4(2) . . ? C11 C12 Fe 68.70(15) . . ? C13 C12 Fe 70.52(15) . . ? C12 C13 C14 108.4(2) . . ? C12 C13 Fe 69.22(15) . . ? C14 C13 Fe 69.18(14) . . ? C13 C14 C10 107.47(19) . . ? C13 C14 C17 122.5(2) . . ? C10 C14 C17 129.7(2) . . ? C13 C14 Fe 70.25(13) . . ? C10 C14 Fe 67.33(12) . . ? C17 C14 Fe 132.70(17) . . ? C18 C17 C14 116.09(19) . . ? C18 C17 C29 101.69(19) . . ? C14 C17 C29 112.91(19) . . ? C19 C18 C23 119.3(2) . . ? C19 C18 C17 130.4(2) . . ? C23 C18 C17 110.3(2) . . ? C18 C19 C20 119.4(3) . . ? C21 C20 C19 120.5(3) . . ? C22 C21 C20 120.7(3) . . ? C21 C22 C23 119.1(3) . . ? C22 C23 C18 121.0(2) . . ? C22 C23 C24 130.2(2) . . ? C18 C23 C24 108.8(2) . . ? C29 C24 C25 120.5(2) . . ? C29 C24 C23 108.8(2) . . ? C25 C24 C23 130.6(2) . . ? C26 C25 C24 118.8(3) . . ? C25 C26 C27 120.7(2) . . ? C28 C27 C26 120.6(3) . . ? C29 C28 C27 119.2(3) . . ? C28 C29 C24 120.2(2) . . ? C28 C29 C17 129.4(2) . . ? C24 C29 C17 110.4(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 C10 Fe C1 C5 -126.62(15) . . . . ? C11 Fe C1 C5 -166.07(14) . . . . ? C3 Fe C1 C5 80.25(17) . . . . ? C2 Fe C1 C5 117.5(2) . . . . ? C4 Fe C1 C5 36.71(16) . . . . ? C12 Fe C1 C5 175.2(2) . . . . ? C14 Fe C1 C5 -86.79(16) . . . . ? C13 Fe C1 C5 -68.7(3) . . . . ? C10 Fe C1 C2 115.90(16) . . . . ? C11 Fe C1 C2 76.45(18) . . . . ? C3 Fe C1 C2 -37.23(17) . . . . ? C5 Fe C1 C2 -117.5(2) . . . . ? C4 Fe C1 C2 -80.77(17) . . . . ? C12 Fe C1 C2 57.7(3) . . . . ? C14 Fe C1 C2 155.74(16) . . . . ? C13 Fe C1 C2 173.8(2) . . . . ? C10 Fe C1 C6 -7.3(2) . . . . ? C11 Fe C1 C6 -46.8(2) . . . . ? C3 Fe C1 C6 -160.5(3) . . . . ? C5 Fe C1 C6 119.3(3) . . . . ? C2 Fe C1 C6 -123.3(3) . . . . ? C4 Fe C1 C6 156.0(2) . . . . ? C12 Fe C1 C6 -65.5(3) . . . . ? C14 Fe C1 C6 32.5(3) . . . . ? C13 Fe C1 C6 50.6(4) . . . . ? C5 C1 C2 C3 -1.3(3) . . . . ? C6 C1 C2 C3 176.1(3) . . . . ? Fe C1 C2 C3 58.7(2) . . . . ? C5 C1 C2 Fe -59.98(18) . . . . ? C6 C1 C2 Fe 117.4(3) . . . . ? C10 Fe C2 C3 164.20(17) . . . . ? C11 Fe C2 C3 121.96(18) . . . . ? C5 Fe C2 C3 -81.70(19) . . . . ? C1 Fe C2 C3 -120.1(2) . . . . ? C4 Fe C2 C3 -37.53(17) . . . . ? C12 Fe C2 C3 84.2(2) . . . . ? C14 Fe C2 C3 -169.6(2) . . . . ? C13 Fe C2 C3 68.2(4) . . . . ? C10 Fe C2 C1 -75.67(17) . . . . ? C11 Fe C2 C1 -117.91(16) . . . . ? C3 Fe C2 C1 120.1(2) . . . . ? C5 Fe C2 C1 38.43(15) . . . . ? C4 Fe C2 C1 82.60(17) . . . . ? C12 Fe C2 C1 -155.66(16) . . . . ? C14 Fe C2 C1 -49.5(3) . . . . ? C13 Fe C2 C1 -171.7(3) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? Fe C2 C3 C4 59.7(2) . . . . ? C1 C2 C3 Fe -58.82(19) . . . . ? C10 Fe C3 C4 -150.8(2) . . . . ? C11 Fe C3 C4 167.74(17) . . . . ? C5 Fe C3 C4 -38.43(18) . . . . ? C2 Fe C3 C4 -119.3(3) . . . . ? C1 Fe C3 C4 -81.97(19) . . . . ? C12 Fe C3 C4 123.85(18) . . . . ? C14 Fe C3 C4 38.8(5) . . . . ? C13 Fe C3 C4 82.2(2) . . . . ? C10 Fe C3 C2 -31.4(3) . . . . ? C11 Fe C3 C2 -72.9(2) . . . . ? C5 Fe C3 C2 80.91(19) . . . . ? C1 Fe C3 C2 37.36(17) . . . . ? C4 Fe C3 C2 119.3(3) . . . . ? C12 Fe C3 C2 -116.81(18) . . . . ? C14 Fe C3 C2 158.2(4) . . . . ? C13 Fe C3 C2 -158.49(16) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Fe C3 C4 C5 59.34(18) . . . . ? C2 C3 C4 Fe -59.5(2) . . . . ? C10 Fe C4 C3 137.2(3) . . . . ? C11 Fe C4 C3 -29.8(4) . . . . ? C5 Fe C4 C3 118.2(3) . . . . ? C2 Fe C4 C3 37.77(17) . . . . ? C1 Fe C4 C3 81.84(18) . . . . ? C12 Fe C4 C3 -78.2(2) . . . . ? C14 Fe C4 C3 -169.28(16) . . . . ? C13 Fe C4 C3 -123.58(17) . . . . ? C10 Fe C4 C5 19.0(4) . . . . ? C11 Fe C4 C5 -148.0(3) . . . . ? C3 Fe C4 C5 -118.2(3) . . . . ? C2 Fe C4 C5 -80.42(19) . . . . ? C1 Fe C4 C5 -36.35(17) . . . . ? C12 Fe C4 C5 163.63(17) . . . . ? C14 Fe C4 C5 72.5(2) . . . . ? C13 Fe C4 C5 118.23(18) . . . . ? C2 C1 C5 C4 1.2(3) . . . . ? C6 C1 C5 C4 -176.3(2) . . . . ? Fe C1 C5 C4 -58.69(19) . . . . ? C2 C1 C5 Fe 59.91(18) . . . . ? C6 C1 C5 Fe -117.6(2) . . . . ? C3 C4 C5 C1 -0.7(3) . . . . ? Fe C4 C5 C1 58.76(19) . . . . ? C3 C4 C5 Fe -59.43(19) . . . . ? C10 Fe C5 C1 66.13(17) . . . . ? C11 Fe C5 C1 30.7(3) . . . . ? C3 Fe C5 C1 -83.15(17) . . . . ? C2 Fe C5 C1 -38.94(15) . . . . ? C4 Fe C5 C1 -121.3(2) . . . . ? C12 Fe C5 C1 -173.1(3) . . . . ? C14 Fe C5 C1 110.66(15) . . . . ? C13 Fe C5 C1 151.94(14) . . . . ? C10 Fe C5 C4 -172.56(17) . . . . ? C11 Fe C5 C4 152.1(2) . . . . ? C3 Fe C5 C4 38.16(18) . . . . ? C2 Fe C5 C4 82.38(19) . . . . ? C1 Fe C5 C4 121.3(2) . . . . ? C12 Fe C5 C4 -51.8(4) . . . . ? C14 Fe C5 C4 -128.02(18) . . . . ? C13 Fe C5 C4 -86.7(2) . . . . ? C5 C1 C6 C7 -160.7(2) . . . . ? C2 C1 C6 C7 22.4(4) . . . . ? Fe C1 C6 C7 111.9(2) . . . . ? C5 C1 C6 C8 71.4(3) . . . . ? C2 C1 C6 C8 -105.6(3) . . . . ? Fe C1 C6 C8 -16.1(3) . . . . ? C1 C6 C8 C9 58.9(3) . . . . ? C7 C6 C8 C9 -69.4(3) . . . . ? C16 N1 C9 C10 55.9(3) . . . . ? C15 N1 C9 C10 175.4(2) . . . . ? C16 N1 C9 C8 -176.4(2) . . . . ? C15 N1 C9 C8 -57.0(3) . . . . ? C6 C8 C9 N1 157.9(2) . . . . ? C6 C8 C9 C10 -75.2(3) . . . . ? N1 C9 C10 C11 -106.9(3) . . . . ? C8 C9 C10 C11 125.7(2) . . . . ? N1 C9 C10 C14 80.6(3) . . . . ? C8 C9 C10 C14 -46.8(3) . . . . ? N1 C9 C10 Fe 170.11(16) . . . . ? C8 C9 C10 Fe 42.7(2) . . . . ? C3 Fe C10 C11 -60.0(3) . . . . ? C5 Fe C10 C11 -158.60(16) . . . . ? C2 Fe C10 C11 -81.77(17) . . . . ? C1 Fe C10 C11 -121.75(16) . . . . ? C4 Fe C10 C11 -172.8(3) . . . . ? C12 Fe C10 C11 36.51(16) . . . . ? C14 Fe C10 C11 116.7(2) . . . . ? C13 Fe C10 C11 79.63(16) . . . . ? C11 Fe C10 C14 -116.7(2) . . . . ? C3 Fe C10 C14 -176.7(2) . . . . ? C5 Fe C10 C14 84.69(16) . . . . ? C2 Fe C10 C14 161.53(14) . . . . ? C1 Fe C10 C14 121.54(14) . . . . ? C4 Fe C10 C14 70.5(4) . . . . ? C12 Fe C10 C14 -80.20(14) . . . . ? C13 Fe C10 C14 -37.08(13) . . . . ? C11 Fe C10 C9 115.7(2) . . . . ? C3 Fe C10 C9 55.7(3) . . . . ? C5 Fe C10 C9 -42.9(2) . . . . ? C2 Fe C10 C9 33.9(2) . . . . ? C1 Fe C10 C9 -6.09(19) . . . . ? C4 Fe C10 C9 -57.2(4) . . . . ? C12 Fe C10 C9 152.2(2) . . . . ? C14 Fe C10 C9 -127.6(2) . . . . ? C13 Fe C10 C9 -164.7(2) . . . . ? C14 C10 C11 C12 2.1(3) . . . . ? C9 C10 C11 C12 -172.0(2) . . . . ? Fe C10 C11 C12 -59.48(18) . . . . ? C14 C10 C11 Fe 61.57(16) . . . . ? C9 C10 C11 Fe -112.5(2) . . . . ? C10 Fe C11 C12 120.6(2) . . . . ? C3 Fe C11 C12 -87.92(18) . . . . ? C5 Fe C11 C12 169.8(2) . . . . ? C2 Fe C11 C12 -127.63(16) . . . . ? C1 Fe C11 C12 -168.31(14) . . . . ? C4 Fe C11 C12 -66.0(4) . . . . ? C14 Fe C11 C12 80.92(16) . . . . ? C13 Fe C11 C12 37.22(14) . . . . ? C3 Fe C11 C10 151.44(15) . . . . ? C5 Fe C11 C10 49.2(3) . . . . ? C2 Fe C11 C10 111.73(16) . . . . ? C1 Fe C11 C10 71.05(16) . . . . ? C4 Fe C11 C10 173.3(3) . . . . ? C12 Fe C11 C10 -120.6(2) . . . . ? C14 Fe C11 C10 -39.71(14) . . . . ? C13 Fe C11 C10 -83.42(15) . . . . ? C10 C11 C12 C13 -1.5(3) . . . . ? Fe C11 C12 C13 -59.56(18) . . . . ? C10 C11 C12 Fe 58.10(17) . . . . ? C10 Fe C12 C11 -37.60(14) . . . . ? C3 Fe C12 C11 111.74(16) . . . . ? C5 Fe C12 C11 -164.9(3) . . . . ? C2 Fe C12 C11 67.59(18) . . . . ? C1 Fe C12 C11 26.2(3) . . . . ? C4 Fe C12 C11 154.71(16) . . . . ? C14 Fe C12 C11 -82.67(15) . . . . ? C13 Fe C12 C11 -119.8(2) . . . . ? C10 Fe C12 C13 82.18(15) . . . . ? C11 Fe C12 C13 119.8(2) . . . . ? C3 Fe C12 C13 -128.49(16) . . . . ? C5 Fe C12 C13 -45.1(4) . . . . ? C2 Fe C12 C13 -172.63(15) . . . . ? C1 Fe C12 C13 145.9(2) . . . . ? C4 Fe C12 C13 -85.52(19) . . . . ? C14 Fe C12 C13 37.11(14) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? Fe C12 C13 C14 -58.21(17) . . . . ? C11 C12 C13 Fe 58.43(19) . . . . ? C10 Fe C13 C12 -82.07(16) . . . . ? C11 Fe C13 C12 -37.30(15) . . . . ? C3 Fe C13 C12 73.8(2) . . . . ? C5 Fe C13 C12 165.40(15) . . . . ? C2 Fe C13 C12 20.9(4) . . . . ? C1 Fe C13 C12 -145.4(3) . . . . ? C4 Fe C13 C12 119.22(17) . . . . ? C14 Fe C13 C12 -120.4(2) . . . . ? C10 Fe C13 C14 38.28(13) . . . . ? C11 Fe C13 C14 83.05(15) . . . . ? C3 Fe C13 C14 -165.81(16) . . . . ? C5 Fe C13 C14 -74.24(17) . . . . ? C2 Fe C13 C14 141.3(3) . . . . ? C1 Fe C13 C14 -25.1(3) . . . . ? C4 Fe C13 C14 -120.43(15) . . . . ? C12 Fe C13 C14 120.4(2) . . . . ? C12 C13 C14 C10 1.1(3) . . . . ? Fe C13 C14 C10 -57.17(15) . . . . ? C12 C13 C14 C17 -173.0(2) . . . . ? Fe C13 C14 C17 128.7(2) . . . . ? C12 C13 C14 Fe 58.23(18) . . . . ? C11 C10 C14 C13 -1.9(3) . . . . ? C9 C10 C14 C13 171.4(2) . . . . ? Fe C10 C14 C13 58.98(16) . . . . ? C11 C10 C14 C17 171.6(2) . . . . ? C9 C10 C14 C17 -15.1(4) . . . . ? Fe C10 C14 C17 -127.5(2) . . . . ? C11 C10 C14 Fe -60.90(16) . . . . ? C9 C10 C14 Fe 112.4(3) . . . . ? C10 Fe C14 C13 -119.71(19) . . . . ? C11 Fe C14 C13 -80.28(15) . . . . ? C3 Fe C14 C13 53.4(5) . . . . ? C5 Fe C14 C13 125.89(15) . . . . ? C2 Fe C14 C13 -157.0(2) . . . . ? C1 Fe C14 C13 168.92(15) . . . . ? C4 Fe C14 C13 84.78(18) . . . . ? C12 Fe C14 C13 -36.85(15) . . . . ? C11 Fe C14 C10 39.42(14) . . . . ? C3 Fe C14 C10 173.1(4) . . . . ? C5 Fe C14 C10 -114.40(14) . . . . ? C2 Fe C14 C10 -37.3(3) . . . . ? C1 Fe C14 C10 -71.38(16) . . . . ? C4 Fe C14 C10 -155.52(15) . . . . ? C12 Fe C14 C10 82.86(15) . . . . ? C13 Fe C14 C10 119.71(19) . . . . ? C10 Fe C14 C17 123.8(3) . . . . ? C11 Fe C14 C17 163.2(3) . . . . ? C3 Fe C14 C17 -63.1(6) . . . . ? C5 Fe C14 C17 9.4(3) . . . . ? C2 Fe C14 C17 86.5(3) . . . . ? C1 Fe C14 C17 52.4(3) . . . . ? C4 Fe C14 C17 -31.7(3) . . . . ? C12 Fe C14 C17 -153.4(3) . . . . ? C13 Fe C14 C17 -116.5(3) . . . . ? C13 C14 C17 C18 -28.3(3) . . . . ? C10 C14 C17 C18 159.0(2) . . . . ? Fe C14 C17 C18 64.2(3) . . . . ? C13 C14 C17 C29 88.6(3) . . . . ? C10 C14 C17 C29 -84.1(3) . . . . ? Fe C14 C17 C29 -178.92(17) . . . . ? C14 C17 C18 C19 -57.7(4) . . . . ? C29 C17 C18 C19 179.4(3) . . . . ? C14 C17 C18 C23 124.4(2) . . . . ? C29 C17 C18 C23 1.5(2) . . . . ? C23 C18 C19 C20 0.5(4) . . . . ? C17 C18 C19 C20 -177.2(2) . . . . ? C18 C19 C20 C21 0.9(4) . . . . ? C19 C20 C21 C22 -1.2(4) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C18 1.5(4) . . . . ? C21 C22 C23 C24 179.9(2) . . . . ? C19 C18 C23 C22 -1.7(4) . . . . ? C17 C18 C23 C22 176.4(2) . . . . ? C19 C18 C23 C24 179.5(2) . . . . ? C17 C18 C23 C24 -2.3(3) . . . . ? C22 C23 C24 C29 -176.3(2) . . . . ? C18 C23 C24 C29 2.3(3) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C18 C23 C24 C25 -179.7(2) . . . . ? C29 C24 C25 C26 0.7(4) . . . . ? C23 C24 C25 C26 -177.1(2) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C26 C27 C28 C29 0.0(4) . . . . ? C27 C28 C29 C24 1.4(4) . . . . ? C27 C28 C29 C17 178.7(2) . . . . ? C25 C24 C29 C28 -1.8(3) . . . . ? C23 C24 C29 C28 176.4(2) . . . . ? C25 C24 C29 C17 -179.5(2) . . . . ? C23 C24 C29 C17 -1.3(3) . . . . ? C18 C17 C29 C28 -177.5(2) . . . . ? C14 C17 C29 C28 57.4(3) . . . . ? C18 C17 C29 C24 -0.1(2) . . . . ? C14 C17 C29 C24 -125.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.337 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.056 # Attachment '20.cif' data_erk5367 _database_code_depnum_ccdc_archive 'CCDC 806926' #TrackingRef '20.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Cl2 Fe Zr' _chemical_formula_weight 628.50 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' Cl Cl 0.1484 0.1585 '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' Zr Zr -2.9673 0.5597 '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 11.1780(2) _cell_length_b 15.2159(2) _cell_length_c 15.4479(3) _cell_angle_alpha 76.208(1) _cell_angle_beta 83.575(1) _cell_angle_gamma 78.305(1) _cell_volume 2493.11(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6441 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6378 _exptl_absorpt_correction_T_max 0.9185 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23225 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 27.87 _reflns_number_total 11587 _reflns_number_gt 10563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0323P)^2^+5.1651P] 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 11587 _refine_ls_number_parameters 651 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _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 Zr1A Zr 0.60654(2) 0.519790(18) 0.287476(18) 0.02644(7) Uani 1 1 d . . . Cl1A Cl 0.41246(8) 0.46300(7) 0.30591(7) 0.0515(2) Uani 1 1 d . . . Cl2A Cl 0.52747(9) 0.65485(6) 0.34728(6) 0.0470(2) Uani 1 1 d . . . Fe1A Fe 1.00582(4) 0.64847(3) 0.16166(3) 0.02642(9) Uani 1 1 d . . . C1A C 1.0113(3) 0.7154(2) 0.2591(2) 0.0330(6) Uani 1 1 d . . . C2A C 1.1259(3) 0.7080(2) 0.2082(2) 0.0354(7) Uani 1 1 d . . . H2A H 1.2023 0.6789 0.2305 0.042 Uiso 1 1 calc R . . C3A C 1.1047(3) 0.7523(2) 0.1175(2) 0.0415(7) Uani 1 1 d . . . H3A H 1.1644 0.7566 0.0695 0.050 Uiso 1 1 calc R . . C4A C 0.9777(3) 0.7889(2) 0.1125(3) 0.0415(8) Uani 1 1 d . . . H4A H 0.9383 0.8219 0.0607 0.050 Uiso 1 1 calc R . . C5A C 0.9212(3) 0.7669(2) 0.1993(2) 0.0374(7) Uani 1 1 d . . . H5A H 0.8374 0.7836 0.2151 0.045 Uiso 1 1 calc R . . C6A C 0.9846(3) 0.6712(2) 0.3555(2) 0.0367(7) Uani 1 1 d . . . H6A H 0.9548 0.7220 0.3869 0.044 Uiso 1 1 calc R . . C7A C 1.0989(3) 0.6142(3) 0.4004(2) 0.0446(8) Uani 1 1 d . . . H7AA H 1.1401 0.5706 0.3652 0.067 Uiso 1 1 calc R . . H7AB H 1.0757 0.5812 0.4598 0.067 Uiso 1 1 calc R . . H7AC H 1.1537 0.6547 0.4049 0.067 Uiso 1 1 calc R . . C8A C 0.8806(3) 0.6159(2) 0.3674(2) 0.0352(6) Uani 1 1 d . . . H8AA H 0.8115 0.6552 0.3351 0.042 Uiso 1 1 calc R . . H8AB H 0.8533 0.6023 0.4309 0.042 Uiso 1 1 calc R . . C9A C 0.9107(3) 0.5243(2) 0.33568(19) 0.0294(6) Uani 1 1 d . . . H9A H 0.9797 0.4859 0.3701 0.035 Uiso 1 1 calc R . . C10A C 0.9541(2) 0.53306(18) 0.23774(19) 0.0254(5) Uani 1 1 d . . . C11A C 1.0793(3) 0.51340(19) 0.2050(2) 0.0306(6) Uani 1 1 d . . . H11A H 1.1466 0.4892 0.2403 0.037 Uiso 1 1 calc R . . C12A C 1.0847(3) 0.5367(2) 0.1099(2) 0.0314(6) Uani 1 1 d . . . H12A H 1.1561 0.5319 0.0716 0.038 Uiso 1 1 calc R . . C13A C 0.9631(3) 0.56841(19) 0.08313(19) 0.0283(6) Uani 1 1 d . . . H13A H 0.9403 0.5878 0.0238 0.034 Uiso 1 1 calc R . . C14A C 0.8807(2) 0.56596(18) 0.16137(18) 0.0244(5) Uani 1 1 d . . . C15A C 0.8051(3) 0.4722(2) 0.36069(18) 0.0289(6) Uani 1 1 d . . . C16A C 0.7908(3) 0.3969(2) 0.3261(2) 0.0329(6) Uani 1 1 d . . . H16A H 0.8414 0.3743 0.2804 0.039 Uiso 1 1 calc R . . C17A C 0.6885(3) 0.3616(2) 0.3711(2) 0.0395(7) Uani 1 1 d . . . H17A H 0.6582 0.3123 0.3601 0.047 Uiso 1 1 calc R . . C18A C 0.6391(3) 0.4130(2) 0.4358(2) 0.0404(7) Uani 1 1 d . . . H18A H 0.5704 0.4038 0.4756 0.049 Uiso 1 1 calc R . . C19A C 0.7107(3) 0.4802(2) 0.4303(2) 0.0355(7) Uani 1 1 d . . . H19A H 0.6985 0.5233 0.4665 0.043 Uiso 1 1 calc R . . C20A C 0.7472(2) 0.57044(18) 0.15865(18) 0.0246(5) Uani 1 1 d . . . C21A C 0.6446(2) 0.64649(19) 0.14542(18) 0.0252(5) Uani 1 1 d . . . C22A C 0.6311(3) 0.74037(19) 0.14543(19) 0.0275(5) Uani 1 1 d . . . H22A H 0.6992 0.7650 0.1524 0.033 Uiso 1 1 calc R . . C23A C 0.5183(3) 0.7957(2) 0.1352(2) 0.0309(6) Uani 1 1 d . . . H23A H 0.5100 0.8584 0.1353 0.037 Uiso 1 1 calc R . . C24A C 0.4142(3) 0.7610(2) 0.1246(2) 0.0336(6) Uani 1 1 d . . . H24A H 0.3377 0.8006 0.1192 0.040 Uiso 1 1 calc R . . C25A C 0.4231(3) 0.6712(2) 0.1221(2) 0.0322(6) Uani 1 1 d . . . H25A H 0.3537 0.6484 0.1145 0.039 Uiso 1 1 calc R . . C26A C 0.5392(3) 0.61267(19) 0.13111(19) 0.0261(5) Uani 1 1 d . . . C27A C 0.5789(3) 0.51807(19) 0.12319(19) 0.0279(5) Uani 1 1 d . . . C28A C 0.5168(3) 0.4551(2) 0.1011(2) 0.0348(6) Uani 1 1 d . . . H28A H 0.4316 0.4689 0.0964 0.042 Uiso 1 1 calc R . . C29A C 0.5839(3) 0.3733(2) 0.0868(2) 0.0395(7) Uani 1 1 d . . . H29A H 0.5443 0.3315 0.0701 0.047 Uiso 1 1 calc R . . C30A C 0.7118(3) 0.3505(2) 0.0965(2) 0.0371(7) Uani 1 1 d . . . H30A H 0.7552 0.2939 0.0859 0.045 Uiso 1 1 calc R . . C31A C 0.7733(3) 0.4085(2) 0.1208(2) 0.0325(6) Uani 1 1 d . . . H31A H 0.8578 0.3918 0.1282 0.039 Uiso 1 1 calc R . . C32A C 0.7070(3) 0.49509(19) 0.13498(19) 0.0277(5) Uani 1 1 d . . . Zr1B Zr 0.22561(3) 1.133959(19) 0.218392(19) 0.02791(7) Uani 1 1 d . . . Cl1B Cl 0.00489(8) 1.19024(8) 0.20575(7) 0.0522(2) Uani 1 1 d . . . Cl2B Cl 0.23813(11) 0.99960(7) 0.15822(7) 0.0556(2) Uani 1 1 d . . . Fe1B Fe 0.66061(4) 1.01131(3) 0.33357(3) 0.02568(9) Uani 1 1 d . . . C1B C 0.7324(3) 0.94823(19) 0.2335(2) 0.0293(6) Uani 1 1 d . . . C2B C 0.8276(3) 0.9542(2) 0.2854(2) 0.0338(6) Uani 1 1 d . . . H2B H 0.8942 0.9842 0.2639 0.041 Uiso 1 1 calc R . . C3B C 0.8040(3) 0.9069(2) 0.3756(2) 0.0373(7) Uani 1 1 d . . . H3B H 0.8515 0.9015 0.4238 0.045 Uiso 1 1 calc R . . C4B C 0.6967(3) 0.8697(2) 0.3796(2) 0.0342(6) Uani 1 1 d . . . H4B H 0.6604 0.8351 0.4308 0.041 Uiso 1 1 calc R . . C5B C 0.6536(3) 0.8940(2) 0.2925(2) 0.0315(6) Uani 1 1 d . . . H5B H 0.5844 0.8771 0.2762 0.038 Uiso 1 1 calc R . . C6B C 0.7103(3) 0.9922(2) 0.1375(2) 0.0337(6) Uani 1 1 d . . . H6B H 0.7171 0.9412 0.1067 0.040 Uiso 1 1 calc R . . C7B C 0.8072(3) 1.0484(3) 0.0909(3) 0.0464(8) Uani 1 1 d . . . H7BA H 0.8059 1.0985 0.1200 0.070 Uiso 1 1 calc R . . H7BB H 0.7899 1.0733 0.0288 0.070 Uiso 1 1 calc R . . H7BC H 0.8874 1.0092 0.0943 0.070 Uiso 1 1 calc R . . C8B C 0.5786(3) 1.0471(2) 0.1273(2) 0.0333(6) Uani 1 1 d . . . H8BA H 0.5220 1.0064 0.1582 0.040 Uiso 1 1 calc R . . H8BB H 0.5632 1.0627 0.0637 0.040 Uiso 1 1 calc R . . C9B C 0.5460(3) 1.13696(19) 0.1623(2) 0.0297(6) Uani 1 1 d . . . H9B H 0.6014 1.1778 0.1276 0.036 Uiso 1 1 calc R . . C10B C 0.5663(3) 1.12708(18) 0.2600(2) 0.0268(5) Uani 1 1 d . . . C11B C 0.6724(3) 1.14612(19) 0.2913(2) 0.0315(6) Uani 1 1 d . . . H11B H 0.7366 1.1702 0.2548 0.038 Uiso 1 1 calc R . . C12B C 0.6649(3) 1.1228(2) 0.3861(2) 0.0338(6) Uani 1 1 d . . . H12B H 0.7235 1.1274 0.4232 0.041 Uiso 1 1 calc R . . C13B C 0.5530(3) 1.09115(19) 0.4149(2) 0.0287(6) Uani 1 1 d . . . H13B H 0.5246 1.0715 0.4747 0.034 Uiso 1 1 calc R . . C14B C 0.4900(2) 1.09403(18) 0.33782(19) 0.0255(5) Uani 1 1 d . . . C15B C 0.4170(3) 1.18603(19) 0.14026(19) 0.0299(6) Uani 1 1 d . . . C16B C 0.3467(3) 1.1758(2) 0.0741(2) 0.0357(7) Uani 1 1 d . . . H16B H 0.3692 1.1324 0.0382 0.043 Uiso 1 1 calc R . . C17B C 0.2371(3) 1.2413(2) 0.0704(2) 0.0412(7) Uani 1 1 d . . . H17B H 0.1742 1.2489 0.0322 0.049 Uiso 1 1 calc R . . C18B C 0.2390(3) 1.2932(2) 0.1341(2) 0.0396(7) Uani 1 1 d . . . H18B H 0.1769 1.3413 0.1463 0.048 Uiso 1 1 calc R . . C19B C 0.3497(3) 1.2607(2) 0.1764(2) 0.0321(6) Uani 1 1 d . . . H19B H 0.3750 1.2843 0.2209 0.038 Uiso 1 1 calc R . . C20B C 0.3591(3) 1.08583(18) 0.34437(19) 0.0263(5) Uani 1 1 d . . . C21B C 0.2670(3) 1.15994(19) 0.36895(19) 0.0276(5) Uani 1 1 d . . . C22B C 0.2771(3) 1.2482(2) 0.3807(2) 0.0333(6) Uani 1 1 d . . . H22B H 0.3531 1.2676 0.3715 0.040 Uiso 1 1 calc R . . C23B C 0.1738(3) 1.3039(2) 0.4058(2) 0.0392(7) Uani 1 1 d . . . H23B H 0.1794 1.3619 0.4146 0.047 Uiso 1 1 calc R . . C24B C 0.0585(3) 1.2765(2) 0.4189(2) 0.0417(8) Uani 1 1 d . . . H24B H -0.0108 1.3171 0.4354 0.050 Uiso 1 1 calc R . . C25B C 0.0451(3) 1.1930(2) 0.4083(2) 0.0371(7) Uani 1 1 d . . . H25B H -0.0323 1.1760 0.4165 0.044 Uiso 1 1 calc R . . C26B C 0.1508(3) 1.1320(2) 0.3845(2) 0.0300(6) Uani 1 1 d . . . C27B C 0.1701(3) 1.0373(2) 0.3769(2) 0.0303(6) Uani 1 1 d . . . C28B C 0.0880(3) 0.9753(2) 0.3881(2) 0.0393(7) Uani 1 1 d . . . H28B H 0.0033 0.9954 0.3973 0.047 Uiso 1 1 calc R . . C29B C 0.1338(3) 0.8861(2) 0.3852(3) 0.0461(8) Uani 1 1 d . . . H29B H 0.0799 0.8447 0.3908 0.055 Uiso 1 1 calc R . . C30B C 0.2609(3) 0.8547(2) 0.3739(3) 0.0433(8) Uani 1 1 d . . . H30B H 0.2902 0.7921 0.3749 0.052 Uiso 1 1 calc R . . C31B C 0.3429(3) 0.9132(2) 0.3616(2) 0.0340(6) Uani 1 1 d . . . H31B H 0.4273 0.8909 0.3542 0.041 Uiso 1 1 calc R . . C32B C 0.2992(3) 1.0076(2) 0.36021(19) 0.0278(5) 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 Zr1A 0.02521(13) 0.02370(13) 0.02660(13) -0.00027(10) 0.00125(10) -0.00362(10) Cl1A 0.0366(4) 0.0608(6) 0.0532(5) 0.0059(4) -0.0014(4) -0.0227(4) Cl2A 0.0631(5) 0.0341(4) 0.0339(4) -0.0061(3) 0.0084(4) 0.0057(4) Fe1A 0.02313(19) 0.02115(19) 0.0327(2) -0.00393(15) -0.00062(15) -0.00197(14) C1A 0.0299(14) 0.0279(14) 0.0433(17) -0.0115(12) -0.0061(12) -0.0040(11) C2A 0.0281(14) 0.0342(16) 0.0449(18) -0.0056(13) -0.0071(13) -0.0091(12) C3A 0.0424(18) 0.0362(17) 0.0464(19) -0.0020(14) -0.0033(14) -0.0168(14) C4A 0.0474(19) 0.0218(14) 0.055(2) -0.0021(13) -0.0144(16) -0.0068(13) C5A 0.0338(16) 0.0227(14) 0.058(2) -0.0143(13) -0.0121(14) 0.0011(12) C6A 0.0329(15) 0.0386(17) 0.0430(17) -0.0202(14) -0.0029(13) -0.0034(13) C7A 0.0431(19) 0.049(2) 0.0436(19) -0.0111(16) -0.0098(15) -0.0086(15) C8A 0.0329(15) 0.0381(17) 0.0366(16) -0.0148(13) 0.0041(12) -0.0067(13) C9A 0.0276(14) 0.0301(14) 0.0278(14) -0.0035(11) -0.0020(11) -0.0026(11) C10A 0.0258(13) 0.0190(12) 0.0291(13) -0.0029(10) -0.0011(10) -0.0019(10) C11A 0.0260(13) 0.0232(13) 0.0377(15) -0.0045(11) -0.0001(11) 0.0027(10) C12A 0.0272(14) 0.0243(13) 0.0379(15) -0.0062(11) 0.0062(11) 0.0005(11) C13A 0.0319(14) 0.0233(13) 0.0280(13) -0.0061(10) 0.0015(11) -0.0026(11) C14A 0.0236(12) 0.0186(12) 0.0286(13) -0.0044(10) 0.0013(10) -0.0014(9) C15A 0.0282(13) 0.0291(14) 0.0235(13) 0.0022(10) -0.0028(10) -0.0008(11) C16A 0.0346(15) 0.0240(14) 0.0337(15) 0.0012(11) -0.0053(12) 0.0020(11) C17A 0.0426(18) 0.0248(14) 0.0438(18) 0.0087(13) -0.0048(14) -0.0079(13) C18A 0.0377(17) 0.0456(19) 0.0292(15) 0.0090(13) 0.0015(12) -0.0096(14) C19A 0.0344(15) 0.0425(17) 0.0249(14) -0.0010(12) -0.0004(12) -0.0048(13) C20A 0.0250(13) 0.0207(12) 0.0259(13) -0.0032(10) -0.0026(10) -0.0009(10) C21A 0.0245(13) 0.0258(13) 0.0228(12) -0.0018(10) -0.0007(10) -0.0034(10) C22A 0.0286(13) 0.0224(13) 0.0302(14) -0.0021(10) -0.0037(11) -0.0053(10) C23A 0.0327(15) 0.0205(13) 0.0358(15) -0.0022(11) -0.0041(12) -0.0006(11) C24A 0.0279(14) 0.0274(14) 0.0423(17) -0.0043(12) -0.0057(12) 0.0000(11) C25A 0.0253(13) 0.0298(14) 0.0406(16) -0.0054(12) -0.0037(12) -0.0048(11) C26A 0.0272(13) 0.0223(13) 0.0283(13) -0.0029(10) -0.0047(10) -0.0051(10) C27A 0.0299(14) 0.0232(13) 0.0291(14) -0.0032(10) -0.0029(11) -0.0044(11) C28A 0.0377(16) 0.0298(15) 0.0386(16) -0.0045(12) -0.0067(13) -0.0112(12) C29A 0.055(2) 0.0247(14) 0.0408(17) -0.0047(12) -0.0057(15) -0.0147(14) C30A 0.0510(19) 0.0222(14) 0.0359(16) -0.0061(12) 0.0022(14) -0.0047(13) C31A 0.0374(16) 0.0255(14) 0.0304(14) -0.0036(11) 0.0031(12) -0.0023(12) C32A 0.0294(14) 0.0242(13) 0.0283(13) -0.0043(10) -0.0015(11) -0.0044(11) Zr1B 0.02789(14) 0.02322(13) 0.03060(14) -0.00342(10) -0.00511(10) -0.00131(10) Cl1B 0.0305(4) 0.0670(6) 0.0525(5) -0.0029(4) -0.0119(4) -0.0010(4) Cl2B 0.0848(7) 0.0370(4) 0.0505(5) -0.0160(4) -0.0051(5) -0.0157(4) Fe1B 0.02351(19) 0.01950(18) 0.0322(2) -0.00361(15) -0.00325(15) -0.00152(14) C1B 0.0271(13) 0.0228(13) 0.0348(15) -0.0071(11) 0.0005(11) 0.0024(10) C2B 0.0257(14) 0.0298(15) 0.0429(17) -0.0073(13) -0.0015(12) 0.0007(11) C3B 0.0294(15) 0.0319(16) 0.0445(18) -0.0033(13) -0.0087(13) 0.0056(12) C4B 0.0366(16) 0.0186(13) 0.0408(16) -0.0016(11) 0.0009(13) 0.0028(11) C5B 0.0293(14) 0.0222(13) 0.0424(16) -0.0095(12) -0.0003(12) -0.0013(11) C6B 0.0322(15) 0.0300(15) 0.0364(16) -0.0097(12) 0.0011(12) 0.0010(12) C7B 0.0417(19) 0.0411(19) 0.048(2) -0.0023(15) 0.0094(15) -0.0033(15) C8B 0.0371(16) 0.0260(14) 0.0323(15) -0.0039(11) -0.0033(12) 0.0015(12) C9B 0.0315(14) 0.0221(13) 0.0316(14) -0.0005(11) -0.0006(11) -0.0029(11) C10B 0.0256(13) 0.0175(12) 0.0351(14) -0.0044(10) -0.0007(11) -0.0018(10) C11B 0.0284(14) 0.0207(13) 0.0446(17) -0.0054(12) -0.0001(12) -0.0060(11) C12B 0.0335(15) 0.0253(14) 0.0447(17) -0.0092(12) -0.0070(13) -0.0064(11) C13B 0.0316(14) 0.0211(13) 0.0326(14) -0.0059(11) -0.0029(11) -0.0029(10) C14B 0.0270(13) 0.0155(11) 0.0315(14) -0.0018(10) -0.0027(10) -0.0021(10) C15B 0.0338(15) 0.0220(13) 0.0276(13) 0.0031(10) -0.0011(11) -0.0012(11) C16B 0.0394(17) 0.0327(16) 0.0290(14) -0.0006(12) -0.0029(12) 0.0003(13) C17B 0.0387(17) 0.0403(18) 0.0350(16) 0.0035(13) -0.0081(13) 0.0037(14) C18B 0.0365(16) 0.0247(14) 0.0477(19) 0.0036(13) -0.0041(14) 0.0041(12) C19B 0.0350(15) 0.0221(13) 0.0352(15) -0.0003(11) -0.0018(12) -0.0037(11) C20B 0.0269(13) 0.0202(12) 0.0289(13) -0.0024(10) -0.0017(10) -0.0013(10) C21B 0.0284(13) 0.0224(13) 0.0278(13) -0.0008(10) -0.0041(11) 0.0005(10) C22B 0.0407(16) 0.0215(13) 0.0362(15) -0.0052(11) -0.0039(13) -0.0024(12) C23B 0.052(2) 0.0253(15) 0.0367(16) -0.0091(12) -0.0067(14) 0.0050(13) C24B 0.0424(18) 0.0368(17) 0.0388(17) -0.0101(14) -0.0040(14) 0.0117(14) C25B 0.0288(15) 0.0403(17) 0.0356(16) -0.0056(13) -0.0018(12) 0.0053(13) C26B 0.0277(14) 0.0285(14) 0.0301(14) -0.0036(11) -0.0027(11) 0.0000(11) C27B 0.0264(14) 0.0278(14) 0.0321(14) -0.0011(11) -0.0010(11) -0.0016(11) C28B 0.0265(14) 0.0369(17) 0.052(2) -0.0045(14) -0.0002(13) -0.0085(12) C29B 0.0341(17) 0.0370(18) 0.067(2) -0.0054(16) 0.0017(16) -0.0150(14) C30B 0.0389(17) 0.0218(14) 0.066(2) -0.0055(14) 0.0007(16) -0.0059(12) C31B 0.0272(14) 0.0260(14) 0.0464(17) -0.0049(12) 0.0001(12) -0.0046(11) C32B 0.0246(13) 0.0257(13) 0.0301(14) -0.0014(11) -0.0019(10) -0.0031(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1A Cl2A 2.4174(9) . ? Zr1A Cl1A 2.4573(9) . ? Zr1A C20A 2.467(3) . ? Zr1A C17A 2.488(3) . ? Zr1A C18A 2.489(3) . ? Zr1A C19A 2.499(3) . ? Zr1A C15A 2.500(3) . ? Zr1A C16A 2.504(3) . ? Zr1A C32A 2.571(3) . ? Zr1A C26A 2.598(3) . ? Zr1A C27A 2.598(3) . ? Zr1A C21A 2.612(3) . ? Fe1A C10A 2.019(3) . ? Fe1A C1A 2.021(3) . ? Fe1A C11A 2.032(3) . ? Fe1A C2A 2.039(3) . ? Fe1A C5A 2.042(3) . ? Fe1A C12A 2.048(3) . ? Fe1A C3A 2.052(3) . ? Fe1A C14A 2.061(3) . ? Fe1A C4A 2.062(3) . ? Fe1A C13A 2.063(3) . ? C1A C5A 1.422(4) . ? C1A C2A 1.425(4) . ? C1A C6A 1.505(5) . ? C2A C3A 1.425(5) . ? C2A H2A 0.9400 . ? C3A C4A 1.420(5) . ? C3A H3A 0.9400 . ? C4A C5A 1.411(5) . ? C4A H4A 0.9400 . ? C5A H5A 0.9400 . ? C6A C7A 1.526(5) . ? C6A C8A 1.540(4) . ? C6A H6A 0.9900 . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C7A H7AC 0.9700 . ? C8A C9A 1.547(4) . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C9A C15A 1.517(4) . ? C9A C10A 1.519(4) . ? C9A H9A 0.9900 . ? C10A C11A 1.431(4) . ? C10A C14A 1.443(4) . ? C11A C12A 1.425(4) . ? C11A H11A 0.9400 . ? C12A C13A 1.420(4) . ? C12A H12A 0.9400 . ? C13A C14A 1.433(4) . ? C13A H13A 0.9400 . ? C14A C20A 1.486(4) . ? C15A C16A 1.418(4) . ? C15A C19A 1.429(4) . ? C16A C17A 1.405(4) . ? C16A H16A 0.9400 . ? C17A C18A 1.410(5) . ? C17A H17A 0.9400 . ? C18A C19A 1.403(5) . ? C18A H18A 0.9400 . ? C19A H19A 0.9400 . ? C20A C21A 1.448(4) . ? C20A C32A 1.448(4) . ? C21A C22A 1.406(4) . ? C21A C26A 1.436(4) . ? C22A C23A 1.369(4) . ? C22A H22A 0.9400 . ? C23A C24A 1.412(4) . ? C23A H23A 0.9400 . ? C24A C25A 1.360(4) . ? C24A H24A 0.9400 . ? C25A C26A 1.417(4) . ? C25A H25A 0.9400 . ? C26A C27A 1.448(4) . ? C27A C28A 1.412(4) . ? C27A C32A 1.425(4) . ? C28A C29A 1.370(5) . ? C28A H28A 0.9400 . ? C29A C30A 1.417(5) . ? C29A H29A 0.9400 . ? C30A C31A 1.362(5) . ? C30A H30A 0.9400 . ? C31A C32A 1.428(4) . ? C31A H31A 0.9400 . ? Zr1B Cl2B 2.4133(9) . ? Zr1B Cl1B 2.4557(9) . ? Zr1B C20B 2.465(3) . ? Zr1B C17B 2.480(3) . ? Zr1B C18B 2.487(3) . ? Zr1B C16B 2.491(3) . ? Zr1B C15B 2.513(3) . ? Zr1B C19B 2.521(3) . ? Zr1B C21B 2.556(3) . ? Zr1B C26B 2.604(3) . ? Zr1B C27B 2.618(3) . ? Zr1B C32B 2.632(3) . ? Fe1B C10B 2.017(3) . ? Fe1B C1B 2.018(3) . ? Fe1B C11B 2.026(3) . ? Fe1B C2B 2.032(3) . ? Fe1B C5B 2.050(3) . ? Fe1B C3B 2.055(3) . ? Fe1B C12B 2.058(3) . ? Fe1B C14B 2.065(3) . ? Fe1B C4B 2.072(3) . ? Fe1B C13B 2.073(3) . ? C1B C5B 1.429(4) . ? C1B C2B 1.431(4) . ? C1B C6B 1.500(4) . ? C2B C3B 1.429(5) . ? C2B H2B 0.9400 . ? C3B C4B 1.417(5) . ? C3B H3B 0.9400 . ? C4B C5B 1.419(5) . ? C4B H4B 0.9400 . ? C5B H5B 0.9400 . ? C6B C7B 1.527(5) . ? C6B C8B 1.543(4) . ? C6B H6B 0.9900 . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C7B H7BC 0.9700 . ? C8B C9B 1.549(4) . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C9B C15B 1.519(4) . ? C9B C10B 1.519(4) . ? C9B H9B 0.9900 . ? C10B C11B 1.435(4) . ? C10B C14B 1.443(4) . ? C11B C12B 1.420(5) . ? C11B H11B 0.9400 . ? C12B C13B 1.418(4) . ? C12B H12B 0.9400 . ? C13B C14B 1.437(4) . ? C13B H13B 0.9400 . ? C14B C20B 1.484(4) . ? C15B C16B 1.412(4) . ? C15B C19B 1.425(4) . ? C16B C17B 1.411(4) . ? C16B H16B 0.9400 . ? C17B C18B 1.405(5) . ? C17B H17B 0.9400 . ? C18B C19B 1.409(4) . ? C18B H18B 0.9400 . ? C19B H19B 0.9400 . ? C20B C32B 1.440(4) . ? C20B C21B 1.456(4) . ? C21B C26B 1.425(4) . ? C21B C22B 1.426(4) . ? C22B C23B 1.364(4) . ? C22B H22B 0.9400 . ? C23B C24B 1.412(5) . ? C23B H23B 0.9400 . ? C24B C25B 1.358(5) . ? C24B H24B 0.9400 . ? C25B C26B 1.418(4) . ? C25B H25B 0.9400 . ? C26B C27B 1.444(4) . ? C27B C28B 1.414(4) . ? C27B C32B 1.435(4) . ? C28B C29B 1.360(5) . ? C28B H28B 0.9400 . ? C29B C30B 1.409(5) . ? C29B H29B 0.9400 . ? C30B C31B 1.371(4) . ? C30B H30B 0.9400 . ? C31B C32B 1.416(4) . ? C31B H31B 0.9400 . ? 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 Cl2A Zr1A Cl1A 96.25(4) . . ? Cl2A Zr1A C20A 105.30(7) . . ? Cl1A Zr1A C20A 134.67(7) . . ? Cl2A Zr1A C17A 127.71(9) . . ? Cl1A Zr1A C17A 83.95(8) . . ? C20A Zr1A C17A 111.09(10) . . ? Cl2A Zr1A C18A 95.02(9) . . ? Cl1A Zr1A C18A 82.57(8) . . ? C20A Zr1A C18A 133.00(10) . . ? C17A Zr1A C18A 32.91(12) . . ? Cl2A Zr1A C19A 78.40(8) . . ? Cl1A Zr1A C19A 112.08(8) . . ? C20A Zr1A C19A 111.08(10) . . ? C17A Zr1A C19A 54.26(12) . . ? C18A Zr1A C19A 32.67(11) . . ? Cl2A Zr1A C15A 97.96(7) . . ? Cl1A Zr1A C15A 136.07(7) . . ? C20A Zr1A C15A 80.18(9) . . ? C17A Zr1A C15A 54.82(11) . . ? C18A Zr1A C15A 54.96(10) . . ? C19A Zr1A C15A 33.23(9) . . ? Cl2A Zr1A C16A 129.90(8) . . ? Cl1A Zr1A C16A 114.47(8) . . ? C20A Zr1A C16A 80.88(9) . . ? C17A Zr1A C16A 32.69(10) . . ? C18A Zr1A C16A 54.31(11) . . ? C19A Zr1A C16A 54.18(11) . . ? C15A Zr1A C16A 32.92(10) . . ? Cl2A Zr1A C32A 133.70(7) . . ? Cl1A Zr1A C32A 106.04(7) . . ? C20A Zr1A C32A 33.32(9) . . ? C17A Zr1A C32A 95.14(11) . . ? C18A Zr1A C32A 127.29(11) . . ? C19A Zr1A C32A 126.05(10) . . ? C15A Zr1A C32A 93.33(9) . . ? C16A Zr1A C32A 76.02(10) . . ? Cl2A Zr1A C26A 89.45(7) . . ? Cl1A Zr1A C26A 86.49(7) . . ? C20A Zr1A C26A 55.02(9) . . ? C17A Zr1A C26A 142.37(11) . . ? C18A Zr1A C26A 168.56(10) . . ? C19A Zr1A C26A 158.61(10) . . ? C15A Zr1A C26A 134.83(9) . . ? C16A Zr1A C26A 128.92(10) . . ? C32A Zr1A C26A 53.09(9) . . ? Cl2A Zr1A C27A 121.48(7) . . ? Cl1A Zr1A C27A 79.49(7) . . ? C20A Zr1A C27A 55.21(9) . . ? C17A Zr1A C27A 110.01(11) . . ? C18A Zr1A C27A 140.64(11) . . ? C19A Zr1A C27A 156.87(10) . . ? C15A Zr1A C27A 125.20(9) . . ? C16A Zr1A C27A 103.08(10) . . ? C32A Zr1A C27A 32.00(9) . . ? C26A Zr1A C27A 32.37(8) . . ? Cl2A Zr1A C21A 80.88(6) . . ? Cl1A Zr1A C21A 117.95(6) . . ? C20A Zr1A C21A 32.97(8) . . ? C17A Zr1A C21A 143.85(10) . . ? C18A Zr1A C21A 159.32(10) . . ? C19A Zr1A C21A 127.33(10) . . ? C15A Zr1A C21A 105.27(9) . . ? C16A Zr1A C21A 113.58(9) . . ? C32A Zr1A C21A 52.84(9) . . ? C26A Zr1A C21A 32.00(8) . . ? C27A Zr1A C21A 53.17(9) . . ? C10A Fe1A C1A 98.91(12) . . ? C10A Fe1A C11A 41.38(11) . . ? C1A Fe1A C11A 108.81(13) . . ? C10A Fe1A C2A 119.45(12) . . ? C1A Fe1A C2A 41.10(13) . . ? C11A Fe1A C2A 100.11(13) . . ? C10A Fe1A C5A 114.51(13) . . ? C1A Fe1A C5A 40.99(12) . . ? C11A Fe1A C5A 145.34(14) . . ? C2A Fe1A C5A 68.24(13) . . ? C10A Fe1A C12A 69.49(11) . . ? C1A Fe1A C12A 144.86(13) . . ? C11A Fe1A C12A 40.87(12) . . ? C2A Fe1A C12A 114.72(13) . . ? C5A Fe1A C12A 173.61(13) . . ? C10A Fe1A C3A 159.38(13) . . ? C1A Fe1A C3A 69.03(14) . . ? C11A Fe1A C3A 124.93(14) . . ? C2A Fe1A C3A 40.76(13) . . ? C5A Fe1A C3A 67.88(15) . . ? C12A Fe1A C3A 110.30(14) . . ? C10A Fe1A C14A 41.42(11) . . ? C1A Fe1A C14A 124.57(12) . . ? C11A Fe1A C14A 69.02(11) . . ? C2A Fe1A C14A 159.85(12) . . ? C5A Fe1A C14A 110.59(12) . . ? C12A Fe1A C14A 68.74(11) . . ? C3A Fe1A C14A 159.00(13) . . ? C10A Fe1A C4A 152.08(13) . . ? C1A Fe1A C4A 68.86(14) . . ? C11A Fe1A C4A 165.32(13) . . ? C2A Fe1A C4A 68.29(13) . . ? C5A Fe1A C4A 40.22(15) . . ? C12A Fe1A C4A 134.54(14) . . ? C3A Fe1A C4A 40.39(14) . . ? C14A Fe1A C4A 124.75(12) . . ? C10A Fe1A C13A 69.11(11) . . ? C1A Fe1A C13A 165.24(12) . . ? C11A Fe1A C13A 68.33(12) . . ? C2A Fe1A C13A 152.39(12) . . ? C5A Fe1A C13A 135.12(12) . . ? C12A Fe1A C13A 40.42(12) . . ? C3A Fe1A C13A 124.97(13) . . ? C14A Fe1A C13A 40.67(11) . . ? C4A Fe1A C13A 117.69(13) . . ? C5A C1A C2A 107.0(3) . . ? C5A C1A C6A 124.8(3) . . ? C2A C1A C6A 128.0(3) . . ? C5A C1A Fe1A 70.29(18) . . ? C2A C1A Fe1A 70.15(18) . . ? C6A C1A Fe1A 120.6(2) . . ? C3A C2A C1A 108.2(3) . . ? C3A C2A Fe1A 70.10(18) . . ? C1A C2A Fe1A 68.75(17) . . ? C3A C2A H2A 125.9 . . ? C1A C2A H2A 125.9 . . ? Fe1A C2A H2A 126.8 . . ? C4A C3A C2A 108.0(3) . . ? C4A C3A Fe1A 70.16(19) . . ? C2A C3A Fe1A 69.14(18) . . ? C4A C3A H3A 126.0 . . ? C2A C3A H3A 126.0 . . ? Fe1A C3A H3A 126.3 . . ? C5A C4A C3A 107.7(3) . . ? C5A C4A Fe1A 69.12(18) . . ? C3A C4A Fe1A 69.45(19) . . ? C5A C4A H4A 126.2 . . ? C3A C4A H4A 126.2 . . ? Fe1A C4A H4A 126.8 . . ? C4A C5A C1A 109.1(3) . . ? C4A C5A Fe1A 70.65(19) . . ? C1A C5A Fe1A 68.72(17) . . ? C4A C5A H5A 125.4 . . ? C1A C5A H5A 125.4 . . ? Fe1A C5A H5A 126.8 . . ? C1A C6A C7A 112.6(3) . . ? C1A C6A C8A 112.0(3) . . ? C7A C6A C8A 112.1(3) . . ? C1A C6A H6A 106.5 . . ? C7A C6A H6A 106.5 . . ? C8A C6A H6A 106.5 . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C6A C8A C9A 116.7(3) . . ? C6A C8A H8AA 108.1 . . ? C9A C8A H8AA 108.1 . . ? C6A C8A H8AB 108.1 . . ? C9A C8A H8AB 108.1 . . ? H8AA C8A H8AB 107.3 . . ? C15A C9A C10A 111.7(2) . . ? C15A C9A C8A 111.0(2) . . ? C10A C9A C8A 115.0(2) . . ? C15A C9A H9A 106.2 . . ? C10A C9A H9A 106.2 . . ? C8A C9A H9A 106.2 . . ? C11A C10A C14A 107.6(2) . . ? C11A C10A C9A 124.8(3) . . ? C14A C10A C9A 127.6(2) . . ? C11A C10A Fe1A 69.81(16) . . ? C14A C10A Fe1A 70.85(15) . . ? C9A C10A Fe1A 122.52(19) . . ? C12A C11A C10A 108.5(3) . . ? C12A C11A Fe1A 70.16(16) . . ? C10A C11A Fe1A 68.81(15) . . ? C12A C11A H11A 125.7 . . ? C10A C11A H11A 125.7 . . ? Fe1A C11A H11A 126.9 . . ? C13A C12A C11A 107.9(2) . . ? C13A C12A Fe1A 70.34(16) . . ? C11A C12A Fe1A 68.96(16) . . ? C13A C12A H12A 126.1 . . ? C11A C12A H12A 126.1 . . ? Fe1A C12A H12A 126.2 . . ? C12A C13A C14A 108.8(3) . . ? C12A C13A Fe1A 69.24(17) . . ? C14A C13A Fe1A 69.60(16) . . ? C12A C13A H13A 125.6 . . ? C14A C13A H13A 125.6 . . ? Fe1A C13A H13A 127.1 . . ? C13A C14A C10A 107.2(2) . . ? C13A C14A C20A 122.4(2) . . ? C10A C14A C20A 128.0(2) . . ? C13A C14A Fe1A 69.74(16) . . ? C10A C14A Fe1A 67.73(15) . . ? C20A C14A Fe1A 141.10(19) . . ? C16A C15A C19A 106.3(3) . . ? C16A C15A C9A 125.5(3) . . ? C19A C15A C9A 127.7(3) . . ? C16A C15A Zr1A 73.73(17) . . ? C19A C15A Zr1A 73.37(17) . . ? C9A C15A Zr1A 124.13(18) . . ? C17A C16A C15A 108.8(3) . . ? C17A C16A Zr1A 73.00(17) . . ? C15A C16A Zr1A 73.35(16) . . ? C17A C16A H16A 125.6 . . ? C15A C16A H16A 125.6 . . ? Zr1A C16A H16A 119.8 . . ? C16A C17A C18A 108.1(3) . . ? C16A C17A Zr1A 74.32(17) . . ? C18A C17A Zr1A 73.60(18) . . ? C16A C17A H17A 125.9 . . ? C18A C17A H17A 125.9 . . ? Zr1A C17A H17A 118.1 . . ? C19A C18A C17A 107.9(3) . . ? C19A C18A Zr1A 74.06(18) . . ? C17A C18A Zr1A 73.49(18) . . ? C19A C18A H18A 126.0 . . ? C17A C18A H18A 126.0 . . ? Zr1A C18A H18A 118.4 . . ? C18A C19A C15A 108.8(3) . . ? C18A C19A Zr1A 73.28(18) . . ? C15A C19A Zr1A 73.41(17) . . ? C18A C19A H19A 125.6 . . ? C15A C19A H19A 125.6 . . ? Zr1A C19A H19A 119.5 . . ? C21A C20A C32A 105.6(2) . . ? C21A C20A C14A 132.7(2) . . ? C32A C20A C14A 118.2(2) . . ? C21A C20A Zr1A 79.01(16) . . ? C32A C20A Zr1A 77.29(16) . . ? C14A C20A Zr1A 125.68(18) . . ? C22A C21A C26A 118.2(2) . . ? C22A C21A C20A 133.2(3) . . ? C26A C21A C20A 108.6(2) . . ? C22A C21A Zr1A 123.82(19) . . ? C26A C21A Zr1A 73.46(15) . . ? C20A C21A Zr1A 68.01(15) . . ? C23A C22A C21A 119.6(3) . . ? C23A C22A H22A 120.2 . . ? C21A C22A H22A 120.2 . . ? C22A C23A C24A 121.7(3) . . ? C22A C23A H23A 119.1 . . ? C24A C23A H23A 119.1 . . ? C25A C24A C23A 120.9(3) . . ? C25A C24A H24A 119.6 . . ? C23A C24A H24A 119.6 . . ? C24A C25A C26A 118.6(3) . . ? C24A C25A H25A 120.7 . . ? C26A C25A H25A 120.7 . . ? C25A C26A C21A 120.9(3) . . ? C25A C26A C27A 131.1(3) . . ? C21A C26A C27A 107.9(2) . . ? C25A C26A Zr1A 120.5(2) . . ? C21A C26A Zr1A 74.53(15) . . ? C27A C26A Zr1A 73.82(16) . . ? C28A C27A C32A 120.8(3) . . ? C28A C27A C26A 132.0(3) . . ? C32A C27A C26A 107.0(2) . . ? C28A C27A Zr1A 122.3(2) . . ? C32A C27A Zr1A 72.97(16) . . ? C26A C27A Zr1A 73.81(16) . . ? C29A C28A C27A 118.4(3) . . ? C29A C28A H28A 120.8 . . ? C27A C28A H28A 120.8 . . ? C28A C29A C30A 121.2(3) . . ? C28A C29A H29A 119.4 . . ? C30A C29A H29A 119.4 . . ? C31A C30A C29A 121.7(3) . . ? C31A C30A H30A 119.2 . . ? C29A C30A H30A 119.2 . . ? C30A C31A C32A 118.8(3) . . ? C30A C31A H31A 120.6 . . ? C32A C31A H31A 120.6 . . ? C27A C32A C31A 119.1(3) . . ? C27A C32A C20A 109.8(2) . . ? C31A C32A C20A 131.2(3) . . ? C27A C32A Zr1A 75.03(16) . . ? C31A C32A Zr1A 123.4(2) . . ? C20A C32A Zr1A 69.39(15) . . ? Cl2B Zr1B Cl1B 96.87(4) . . ? Cl2B Zr1B C20B 106.13(7) . . ? Cl1B Zr1B C20B 133.95(7) . . ? Cl2B Zr1B C17B 94.78(9) . . ? Cl1B Zr1B C17B 82.26(8) . . ? C20B Zr1B C17B 133.09(11) . . ? Cl2B Zr1B C18B 127.47(9) . . ? Cl1B Zr1B C18B 82.92(8) . . ? C20B Zr1B C18B 111.13(11) . . ? C17B Zr1B C18B 32.85(12) . . ? Cl2B Zr1B C16B 78.62(8) . . ? Cl1B Zr1B C16B 112.49(8) . . ? C20B Zr1B C16B 110.87(10) . . ? C17B Zr1B C16B 32.96(10) . . ? C18B Zr1B C16B 54.32(11) . . ? Cl2B Zr1B C15B 98.45(7) . . ? Cl1B Zr1B C15B 135.29(7) . . ? C20B Zr1B C15B 80.46(9) . . ? C17B Zr1B C15B 54.82(10) . . ? C18B Zr1B C15B 54.71(10) . . ? C16B Zr1B C15B 32.77(10) . . ? Cl2B Zr1B C19B 130.27(8) . . ? Cl1B Zr1B C19B 113.24(7) . . ? C20B Zr1B C19B 80.98(10) . . ? C17B Zr1B C19B 54.24(11) . . ? C18B Zr1B C19B 32.66(10) . . ? C16B Zr1B C19B 53.97(11) . . ? C15B Zr1B C19B 32.89(9) . . ? Cl2B Zr1B C21B 134.44(7) . . ? Cl1B Zr1B C21B 104.50(7) . . ? C20B Zr1B C21B 33.66(9) . . ? C17B Zr1B C21B 127.33(11) . . ? C18B Zr1B C21B 95.16(11) . . ? C16B Zr1B C21B 126.19(10) . . ? C15B Zr1B C21B 93.91(10) . . ? C19B Zr1B C21B 76.32(10) . . ? Cl2B Zr1B C26B 120.76(7) . . ? Cl1B Zr1B C26B 78.81(7) . . ? C20B Zr1B C26B 55.15(9) . . ? C17B Zr1B C26B 141.23(11) . . ? C18B Zr1B C26B 110.75(11) . . ? C16B Zr1B C26B 157.34(11) . . ? C15B Zr1B C26B 125.90(10) . . ? C19B Zr1B C26B 103.88(10) . . ? C21B Zr1B C26B 32.05(9) . . ? Cl2B Zr1B C27B 89.15(7) . . ? Cl1B Zr1B C27B 87.09(7) . . ? C20B Zr1B C27B 54.72(9) . . ? C17B Zr1B C27B 169.01(10) . . ? C18B Zr1B C27B 142.86(11) . . ? C16B Zr1B C27B 157.83(10) . . ? C15B Zr1B C27B 134.72(9) . . ? C19B Zr1B C27B 129.11(10) . . ? C21B Zr1B C27B 53.08(9) . . ? C26B Zr1B C27B 32.10(9) . . ? Cl2B Zr1B C32B 81.67(7) . . ? Cl1B Zr1B C32B 118.51(7) . . ? C20B Zr1B C32B 32.61(9) . . ? C17B Zr1B C32B 159.16(10) . . ? C18B Zr1B C32B 143.53(11) . . ? C16B Zr1B C32B 126.92(9) . . ? C15B Zr1B C32B 105.17(9) . . ? C19B Zr1B C32B 113.29(9) . . ? C21B Zr1B C32B 52.77(9) . . ? C26B Zr1B C32B 52.70(9) . . ? C27B Zr1B C32B 31.72(8) . . ? C10B Fe1B C1B 98.43(12) . . ? C10B Fe1B C11B 41.59(11) . . ? C1B Fe1B C11B 107.55(13) . . ? C10B Fe1B C2B 119.63(12) . . ? C1B Fe1B C2B 41.39(12) . . ? C11B Fe1B C2B 99.40(13) . . ? C10B Fe1B C5B 114.06(12) . . ? C1B Fe1B C5B 41.13(12) . . ? C11B Fe1B C5B 144.33(13) . . ? C2B Fe1B C5B 68.35(12) . . ? C10B Fe1B C3B 159.87(13) . . ? C1B Fe1B C3B 69.45(13) . . ? C11B Fe1B C3B 125.02(13) . . ? C2B Fe1B C3B 40.93(13) . . ? C5B Fe1B C3B 67.86(13) . . ? C10B Fe1B C12B 69.58(12) . . ? C1B Fe1B C12B 143.17(13) . . ? C11B Fe1B C12B 40.69(13) . . ? C2B Fe1B C12B 113.36(13) . . ? C5B Fe1B C12B 174.95(13) . . ? C3B Fe1B C12B 110.06(13) . . ? C10B Fe1B C14B 41.39(11) . . ? C1B Fe1B C14B 125.29(12) . . ? C11B Fe1B C14B 68.93(11) . . ? C2B Fe1B C14B 160.41(12) . . ? C5B Fe1B C14B 111.51(11) . . ? C3B Fe1B C14B 158.49(13) . . ? C12B Fe1B C14B 68.60(12) . . ? C10B Fe1B C4B 151.64(12) . . ? C1B Fe1B C4B 69.13(12) . . ? C11B Fe1B C4B 165.16(13) . . ? C2B Fe1B C4B 68.27(13) . . ? C5B Fe1B C4B 40.27(13) . . ? C3B Fe1B C4B 40.15(13) . . ? C12B Fe1B C4B 135.28(13) . . ? C14B Fe1B C4B 125.22(12) . . ? C10B Fe1B C13B 69.06(11) . . ? C1B Fe1B C13B 165.80(12) . . ? C11B Fe1B C13B 67.96(12) . . ? C2B Fe1B C13B 150.75(12) . . ? C5B Fe1B C13B 136.82(12) . . ? C3B Fe1B C13B 124.46(13) . . ? C12B Fe1B C13B 40.15(12) . . ? C14B Fe1B C13B 40.64(11) . . ? C4B Fe1B C13B 118.71(12) . . ? C5B C1B C2B 106.6(3) . . ? C5B C1B C6B 124.2(3) . . ? C2B C1B C6B 129.1(3) . . ? C5B C1B Fe1B 70.65(17) . . ? C2B C1B Fe1B 69.85(17) . . ? C6B C1B Fe1B 122.1(2) . . ? C3B C2B C1B 108.4(3) . . ? C3B C2B Fe1B 70.38(17) . . ? C1B C2B Fe1B 68.76(16) . . ? C3B C2B H2B 125.8 . . ? C1B C2B H2B 125.8 . . ? Fe1B C2B H2B 126.6 . . ? C4B C3B C2B 108.0(3) . . ? C4B C3B Fe1B 70.56(17) . . ? C2B C3B Fe1B 68.68(17) . . ? C4B C3B H3B 126.0 . . ? C2B C3B H3B 126.0 . . ? Fe1B C3B H3B 126.3 . . ? C3B C4B C5B 107.8(3) . . ? C3B C4B Fe1B 69.29(17) . . ? C5B C4B Fe1B 69.05(17) . . ? C3B C4B H4B 126.1 . . ? C5B C4B H4B 126.1 . . ? Fe1B C4B H4B 127.1 . . ? C4B C5B C1B 109.1(3) . . ? C4B C5B Fe1B 70.69(17) . . ? C1B C5B Fe1B 68.22(16) . . ? C4B C5B H5B 125.4 . . ? C1B C5B H5B 125.4 . . ? Fe1B C5B H5B 127.2 . . ? C1B C6B C7B 113.2(3) . . ? C1B C6B C8B 111.4(2) . . ? C7B C6B C8B 112.9(3) . . ? C1B C6B H6B 106.3 . . ? C7B C6B H6B 106.3 . . ? C8B C6B H6B 106.3 . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? C6B C8B C9B 117.3(3) . . ? C6B C8B H8BA 108.0 . . ? C9B C8B H8BA 108.0 . . ? C6B C8B H8BB 108.0 . . ? C9B C8B H8BB 108.0 . . ? H8BA C8B H8BB 107.2 . . ? C15B C9B C10B 111.5(2) . . ? C15B C9B C8B 110.4(2) . . ? C10B C9B C8B 115.9(2) . . ? C15B C9B H9B 106.1 . . ? C10B C9B H9B 106.1 . . ? C8B C9B H9B 106.1 . . ? C11B C10B C14B 107.1(3) . . ? C11B C10B C9B 124.4(3) . . ? C14B C10B C9B 128.4(3) . . ? C11B C10B Fe1B 69.53(16) . . ? C14B C10B Fe1B 71.10(15) . . ? C9B C10B Fe1B 122.36(19) . . ? C12B C11B C10B 109.0(3) . . ? C12B C11B Fe1B 70.87(17) . . ? C10B C11B Fe1B 68.88(15) . . ? C12B C11B H11B 125.5 . . ? C10B C11B H11B 125.5 . . ? Fe1B C11B H11B 126.4 . . ? C13B C12B C11B 107.7(3) . . ? C13B C12B Fe1B 70.52(16) . . ? C11B C12B Fe1B 68.44(17) . . ? C13B C12B H12B 126.2 . . ? C11B C12B H12B 126.2 . . ? Fe1B C12B H12B 126.4 . . ? C12B C13B C14B 108.9(3) . . ? C12B C13B Fe1B 69.33(17) . . ? C14B C13B Fe1B 69.37(16) . . ? C12B C13B H13B 125.5 . . ? C14B C13B H13B 125.5 . . ? Fe1B C13B H13B 127.3 . . ? C13B C14B C10B 107.2(2) . . ? C13B C14B C20B 122.1(3) . . ? C10B C14B C20B 129.0(3) . . ? C13B C14B Fe1B 69.99(16) . . ? C10B C14B Fe1B 67.51(15) . . ? C20B C14B Fe1B 138.98(19) . . ? C16B C15B C19B 106.6(3) . . ? C16B C15B C9B 127.9(3) . . ? C19B C15B C9B 125.0(3) . . ? C16B C15B Zr1B 72.78(18) . . ? C19B C15B Zr1B 73.87(17) . . ? C9B C15B Zr1B 124.42(18) . . ? C17B C16B C15B 109.1(3) . . ? C17B C16B Zr1B 73.10(19) . . ? C15B C16B Zr1B 74.45(17) . . ? C17B C16B H16B 125.5 . . ? C15B C16B H16B 125.5 . . ? Zr1B C16B H16B 118.8 . . ? C18B C17B C16B 107.6(3) . . ? C18B C17B Zr1B 73.85(19) . . ? C16B C17B Zr1B 73.93(18) . . ? C18B C17B H17B 126.2 . . ? C16B C17B H17B 126.2 . . ? Zr1B C17B H17B 118.0 . . ? C17B C18B C19B 108.3(3) . . ? C17B C18B Zr1B 73.31(19) . . ? C19B C18B Zr1B 74.96(18) . . ? C17B C18B H18B 125.9 . . ? C19B C18B H18B 125.9 . . ? Zr1B C18B H18B 117.8 . . ? C18B C19B C15B 108.4(3) . . ? C18B C19B Zr1B 72.37(18) . . ? C15B C19B Zr1B 73.25(17) . . ? C18B C19B H19B 125.8 . . ? C15B C19B H19B 125.8 . . ? Zr1B C19B H19B 120.3 . . ? C32B C20B C21B 105.6(2) . . ? C32B C20B C14B 132.4(2) . . ? C21B C20B C14B 118.7(2) . . ? C32B C20B Zr1B 80.07(16) . . ? C21B C20B Zr1B 76.60(16) . . ? C14B C20B Zr1B 124.90(19) . . ? C26B C21B C22B 119.5(3) . . ? C26B C21B C20B 109.2(2) . . ? C22B C21B C20B 131.2(3) . . ? C26B C21B Zr1B 75.82(17) . . ? C22B C21B Zr1B 122.2(2) . . ? C20B C21B Zr1B 69.74(16) . . ? C23B C22B C21B 118.4(3) . . ? C23B C22B H22B 120.8 . . ? C21B C22B H22B 120.8 . . ? C22B C23B C24B 121.6(3) . . ? C22B C23B H23B 119.2 . . ? C24B C23B H23B 119.2 . . ? C25B C24B C23B 121.7(3) . . ? C25B C24B H24B 119.1 . . ? C23B C24B H24B 119.1 . . ? C24B C25B C26B 118.5(3) . . ? C24B C25B H25B 120.8 . . ? C26B C25B H25B 120.8 . . ? C25B C26B C21B 120.2(3) . . ? C25B C26B C27B 132.2(3) . . ? C21B C26B C27B 107.4(2) . . ? C25B C26B Zr1B 121.8(2) . . ? C21B C26B Zr1B 72.13(16) . . ? C27B C26B Zr1B 74.51(17) . . ? C28B C27B C32B 120.8(3) . . ? C28B C27B C26B 131.4(3) . . ? C32B C27B C26B 107.6(3) . . ? C28B C27B Zr1B 120.8(2) . . ? C32B C27B Zr1B 74.64(16) . . ? C26B C27B Zr1B 73.39(16) . . ? C29B C28B C27B 118.8(3) . . ? C29B C28B H28B 120.6 . . ? C27B C28B H28B 120.6 . . ? C28B C29B C30B 121.0(3) . . ? C28B C29B H29B 119.5 . . ? C30B C29B H29B 119.5 . . ? C31B C30B C29B 121.6(3) . . ? C31B C30B H30B 119.2 . . ? C29B C30B H30B 119.2 . . ? C30B C31B C32B 119.4(3) . . ? C30B C31B H31B 120.3 . . ? C32B C31B H31B 120.3 . . ? C31B C32B C27B 118.2(3) . . ? C31B C32B C20B 132.8(3) . . ? C27B C32B C20B 109.0(2) . . ? C31B C32B Zr1B 125.1(2) . . ? C27B C32B Zr1B 73.63(16) . . ? C20B C32B Zr1B 67.33(15) . . ? 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 C10A Fe1A C1A C5A -117.4(2) . . . . ? C11A Fe1A C1A C5A -158.9(2) . . . . ? C2A Fe1A C1A C5A 117.4(3) . . . . ? C12A Fe1A C1A C5A 175.8(2) . . . . ? C3A Fe1A C1A C5A 80.0(2) . . . . ? C14A Fe1A C1A C5A -81.8(2) . . . . ? C4A Fe1A C1A C5A 36.6(2) . . . . ? C13A Fe1A C1A C5A -82.6(5) . . . . ? C10A Fe1A C1A C2A 125.28(19) . . . . ? C11A Fe1A C1A C2A 83.8(2) . . . . ? C5A Fe1A C1A C2A -117.4(3) . . . . ? C12A Fe1A C1A C2A 58.4(3) . . . . ? C3A Fe1A C1A C2A -37.37(19) . . . . ? C14A Fe1A C1A C2A 160.80(17) . . . . ? C4A Fe1A C1A C2A -80.8(2) . . . . ? C13A Fe1A C1A C2A 160.0(4) . . . . ? C10A Fe1A C1A C6A 2.2(3) . . . . ? C11A Fe1A C1A C6A -39.3(3) . . . . ? C2A Fe1A C1A C6A -123.1(3) . . . . ? C5A Fe1A C1A C6A 119.5(3) . . . . ? C12A Fe1A C1A C6A -64.7(3) . . . . ? C3A Fe1A C1A C6A -160.5(3) . . . . ? C14A Fe1A C1A C6A 37.7(3) . . . . ? C4A Fe1A C1A C6A 156.1(3) . . . . ? C13A Fe1A C1A C6A 36.9(6) . . . . ? C5A C1A C2A C3A -1.8(4) . . . . ? C6A C1A C2A C3A 173.1(3) . . . . ? Fe1A C1A C2A C3A 59.2(2) . . . . ? C5A C1A C2A Fe1A -61.0(2) . . . . ? C6A C1A C2A Fe1A 113.9(3) . . . . ? C10A Fe1A C2A C3A 172.4(2) . . . . ? C1A Fe1A C2A C3A -119.8(3) . . . . ? C11A Fe1A C2A C3A 133.2(2) . . . . ? C5A Fe1A C2A C3A -80.9(2) . . . . ? C12A Fe1A C2A C3A 92.9(2) . . . . ? C14A Fe1A C2A C3A -171.6(3) . . . . ? C4A Fe1A C2A C3A -37.5(2) . . . . ? C13A Fe1A C2A C3A 71.1(3) . . . . ? C10A Fe1A C2A C1A -67.9(2) . . . . ? C11A Fe1A C2A C1A -107.09(19) . . . . ? C5A Fe1A C2A C1A 38.85(19) . . . . ? C12A Fe1A C2A C1A -147.32(18) . . . . ? C3A Fe1A C2A C1A 119.8(3) . . . . ? C14A Fe1A C2A C1A -51.8(4) . . . . ? C4A Fe1A C2A C1A 82.3(2) . . . . ? C13A Fe1A C2A C1A -169.2(2) . . . . ? C1A C2A C3A C4A 1.2(4) . . . . ? Fe1A C2A C3A C4A 59.6(2) . . . . ? C1A C2A C3A Fe1A -58.4(2) . . . . ? C10A Fe1A C3A C4A -138.4(3) . . . . ? C1A Fe1A C3A C4A -81.6(2) . . . . ? C11A Fe1A C3A C4A 179.5(2) . . . . ? C2A Fe1A C3A C4A -119.3(3) . . . . ? C5A Fe1A C3A C4A -37.4(2) . . . . ? C12A Fe1A C3A C4A 136.0(2) . . . . ? C14A Fe1A C3A C4A 52.6(5) . . . . ? C13A Fe1A C3A C4A 93.0(2) . . . . ? C10A Fe1A C3A C2A -19.1(5) . . . . ? C1A Fe1A C3A C2A 37.67(19) . . . . ? C11A Fe1A C3A C2A -61.2(2) . . . . ? C5A Fe1A C3A C2A 81.9(2) . . . . ? C12A Fe1A C3A C2A -104.7(2) . . . . ? C14A Fe1A C3A C2A 171.9(3) . . . . ? C4A Fe1A C3A C2A 119.3(3) . . . . ? C13A Fe1A C3A C2A -147.66(19) . . . . ? C2A C3A C4A C5A -0.2(4) . . . . ? Fe1A C3A C4A C5A 58.8(2) . . . . ? C2A C3A C4A Fe1A -59.0(2) . . . . ? C10A Fe1A C4A C5A 30.7(4) . . . . ? C1A Fe1A C4A C5A -37.24(19) . . . . ? C11A Fe1A C4A C5A -120.8(5) . . . . ? C2A Fe1A C4A C5A -81.5(2) . . . . ? C12A Fe1A C4A C5A 174.60(19) . . . . ? C3A Fe1A C4A C5A -119.3(3) . . . . ? C14A Fe1A C4A C5A 80.9(2) . . . . ? C13A Fe1A C4A C5A 128.22(19) . . . . ? C10A Fe1A C4A C3A 150.1(3) . . . . ? C1A Fe1A C4A C3A 82.1(2) . . . . ? C11A Fe1A C4A C3A -1.5(6) . . . . ? C2A Fe1A C4A C3A 37.8(2) . . . . ? C5A Fe1A C4A C3A 119.3(3) . . . . ? C12A Fe1A C4A C3A -66.1(3) . . . . ? C14A Fe1A C4A C3A -159.7(2) . . . . ? C13A Fe1A C4A C3A -112.5(2) . . . . ? C3A C4A C5A C1A -0.9(4) . . . . ? Fe1A C4A C5A C1A 58.1(2) . . . . ? C3A C4A C5A Fe1A -59.0(2) . . . . ? C2A C1A C5A C4A 1.6(3) . . . . ? C6A C1A C5A C4A -173.4(3) . . . . ? Fe1A C1A C5A C4A -59.2(2) . . . . ? C2A C1A C5A Fe1A 60.9(2) . . . . ? C6A C1A C5A Fe1A -114.2(3) . . . . ? C10A Fe1A C5A C4A -164.75(19) . . . . ? C1A Fe1A C5A C4A 120.6(3) . . . . ? C11A Fe1A C5A C4A 157.5(2) . . . . ? C2A Fe1A C5A C4A 81.7(2) . . . . ? C12A Fe1A C5A C4A -37.1(12) . . . . ? C3A Fe1A C5A C4A 37.6(2) . . . . ? C14A Fe1A C5A C4A -119.9(2) . . . . ? C13A Fe1A C5A C4A -80.4(2) . . . . ? C10A Fe1A C5A C1A 74.6(2) . . . . ? C11A Fe1A C5A C1A 36.9(3) . . . . ? C2A Fe1A C5A C1A -38.95(19) . . . . ? C12A Fe1A C5A C1A -157.7(11) . . . . ? C3A Fe1A C5A C1A -83.1(2) . . . . ? C14A Fe1A C5A C1A 119.46(19) . . . . ? C4A Fe1A C5A C1A -120.6(3) . . . . ? C13A Fe1A C5A C1A 159.01(19) . . . . ? C5A C1A C6A C7A 175.4(3) . . . . ? C2A C1A C6A C7A 1.4(5) . . . . ? Fe1A C1A C6A C7A 89.2(3) . . . . ? C5A C1A C6A C8A 48.0(4) . . . . ? C2A C1A C6A C8A -126.0(3) . . . . ? Fe1A C1A C6A C8A -38.3(3) . . . . ? C1A C6A C8A C9A 72.2(4) . . . . ? C7A C6A C8A C9A -55.5(4) . . . . ? C6A C8A C9A C15A 173.7(3) . . . . ? C6A C8A C9A C10A -58.3(4) . . . . ? C15A C9A C10A C11A -132.1(3) . . . . ? C8A C9A C10A C11A 100.3(3) . . . . ? C15A C9A C10A C14A 51.1(4) . . . . ? C8A C9A C10A C14A -76.6(4) . . . . ? C15A C9A C10A Fe1A 141.1(2) . . . . ? C8A C9A C10A Fe1A 13.5(3) . . . . ? C1A Fe1A C10A C11A -108.42(18) . . . . ? C2A Fe1A C10A C11A -70.4(2) . . . . ? C5A Fe1A C10A C11A -148.22(18) . . . . ? C12A Fe1A C10A C11A 37.18(18) . . . . ? C3A Fe1A C10A C11A -56.1(4) . . . . ? C14A Fe1A C10A C11A 117.9(2) . . . . ? C4A Fe1A C10A C11A -169.5(3) . . . . ? C13A Fe1A C10A C11A 80.52(18) . . . . ? C1A Fe1A C10A C14A 133.68(16) . . . . ? C11A Fe1A C10A C14A -117.9(2) . . . . ? C2A Fe1A C10A C14A 171.72(16) . . . . ? C5A Fe1A C10A C14A 93.88(17) . . . . ? C12A Fe1A C10A C14A -80.73(17) . . . . ? C3A Fe1A C10A C14A -174.1(3) . . . . ? C4A Fe1A C10A C14A 72.6(3) . . . . ? C13A Fe1A C10A C14A -37.38(15) . . . . ? C1A Fe1A C10A C9A 10.7(2) . . . . ? C11A Fe1A C10A C9A 119.1(3) . . . . ? C2A Fe1A C10A C9A 48.7(3) . . . . ? C5A Fe1A C10A C9A -29.1(3) . . . . ? C12A Fe1A C10A C9A 156.3(3) . . . . ? C3A Fe1A C10A C9A 62.9(5) . . . . ? C14A Fe1A C10A C9A -123.0(3) . . . . ? C4A Fe1A C10A C9A -50.4(4) . . . . ? C13A Fe1A C10A C9A -160.4(3) . . . . ? C14A C10A C11A C12A 2.0(3) . . . . ? C9A C10A C11A C12A -175.3(3) . . . . ? Fe1A C10A C11A C12A -59.1(2) . . . . ? C14A C10A C11A Fe1A 61.12(19) . . . . ? C9A C10A C11A Fe1A -116.2(3) . . . . ? C10A Fe1A C11A C12A 120.1(2) . . . . ? C1A Fe1A C11A C12A -157.89(18) . . . . ? C2A Fe1A C11A C12A -116.30(19) . . . . ? C5A Fe1A C11A C12A 177.5(2) . . . . ? C3A Fe1A C11A C12A -80.8(2) . . . . ? C14A Fe1A C11A C12A 81.36(18) . . . . ? C4A Fe1A C11A C12A -79.6(6) . . . . ? C13A Fe1A C11A C12A 37.56(17) . . . . ? C1A Fe1A C11A C10A 81.99(19) . . . . ? C2A Fe1A C11A C10A 123.58(18) . . . . ? C5A Fe1A C11A C10A 57.4(3) . . . . ? C12A Fe1A C11A C10A -120.1(2) . . . . ? C3A Fe1A C11A C10A 159.10(18) . . . . ? C14A Fe1A C11A C10A -38.76(16) . . . . ? C4A Fe1A C11A C10A 160.3(5) . . . . ? C13A Fe1A C11A C10A -82.56(18) . . . . ? C10A C11A C12A C13A -1.6(3) . . . . ? Fe1A C11A C12A C13A -59.8(2) . . . . ? C10A C11A C12A Fe1A 58.3(2) . . . . ? C10A Fe1A C12A C13A 81.48(18) . . . . ? C1A Fe1A C12A C13A 157.4(2) . . . . ? C11A Fe1A C12A C13A 119.1(2) . . . . ? C2A Fe1A C12A C13A -164.58(17) . . . . ? C5A Fe1A C12A C13A -48.3(12) . . . . ? C3A Fe1A C12A C13A -120.53(19) . . . . ? C14A Fe1A C12A C13A 37.01(16) . . . . ? C4A Fe1A C12A C13A -81.4(2) . . . . ? C10A Fe1A C12A C11A -37.62(17) . . . . ? C1A Fe1A C12A C11A 38.2(3) . . . . ? C2A Fe1A C12A C11A 76.3(2) . . . . ? C5A Fe1A C12A C11A -167.4(11) . . . . ? C3A Fe1A C12A C11A 120.36(19) . . . . ? C14A Fe1A C12A C11A -82.09(18) . . . . ? C4A Fe1A C12A C11A 159.53(19) . . . . ? C13A Fe1A C12A C11A -119.1(2) . . . . ? C11A C12A C13A C14A 0.5(3) . . . . ? Fe1A C12A C13A C14A -58.48(19) . . . . ? C11A C12A C13A Fe1A 59.0(2) . . . . ? C10A Fe1A C13A C12A -82.53(18) . . . . ? C1A Fe1A C13A C12A -119.6(5) . . . . ? C11A Fe1A C13A C12A -37.97(17) . . . . ? C2A Fe1A C13A C12A 31.4(3) . . . . ? C5A Fe1A C13A C12A 173.2(2) . . . . ? C3A Fe1A C13A C12A 80.3(2) . . . . ? C14A Fe1A C13A C12A -120.6(2) . . . . ? C4A Fe1A C13A C12A 127.27(19) . . . . ? C10A Fe1A C13A C14A 38.05(16) . . . . ? C1A Fe1A C13A C14A 1.0(5) . . . . ? C11A Fe1A C13A C14A 82.61(17) . . . . ? C2A Fe1A C13A C14A 152.0(2) . . . . ? C5A Fe1A C13A C14A -66.2(2) . . . . ? C12A Fe1A C13A C14A 120.6(2) . . . . ? C3A Fe1A C13A C14A -159.10(18) . . . . ? C4A Fe1A C13A C14A -112.15(19) . . . . ? C12A C13A C14A C10A 0.8(3) . . . . ? Fe1A C13A C14A C10A -57.50(18) . . . . ? C12A C13A C14A C20A -163.3(2) . . . . ? Fe1A C13A C14A C20A 138.4(3) . . . . ? C12A C13A C14A Fe1A 58.3(2) . . . . ? C11A C10A C14A C13A -1.7(3) . . . . ? C9A C10A C14A C13A 175.6(3) . . . . ? Fe1A C10A C14A C13A 58.75(19) . . . . ? C11A C10A C14A C20A 161.2(3) . . . . ? C9A C10A C14A C20A -21.6(5) . . . . ? Fe1A C10A C14A C20A -138.4(3) . . . . ? C11A C10A C14A Fe1A -60.46(19) . . . . ? C9A C10A C14A Fe1A 116.8(3) . . . . ? C10A Fe1A C14A C13A -119.5(2) . . . . ? C1A Fe1A C14A C13A -179.69(17) . . . . ? C11A Fe1A C14A C13A -80.76(17) . . . . ? C2A Fe1A C14A C13A -140.8(3) . . . . ? C5A Fe1A C14A C13A 136.40(18) . . . . ? C12A Fe1A C14A C13A -36.79(17) . . . . ? C3A Fe1A C14A C13A 54.7(4) . . . . ? C4A Fe1A C14A C13A 93.5(2) . . . . ? C1A Fe1A C14A C10A -60.20(19) . . . . ? C11A Fe1A C14A C10A 38.73(16) . . . . ? C2A Fe1A C14A C10A -21.3(4) . . . . ? C5A Fe1A C14A C10A -104.11(18) . . . . ? C12A Fe1A C14A C10A 82.69(17) . . . . ? C3A Fe1A C14A C10A 174.2(3) . . . . ? C4A Fe1A C14A C10A -147.05(18) . . . . ? C13A Fe1A C14A C10A 119.5(2) . . . . ? C10A Fe1A C14A C20A 123.6(4) . . . . ? C1A Fe1A C14A C20A 63.4(3) . . . . ? C11A Fe1A C14A C20A 162.3(3) . . . . ? C2A Fe1A C14A C20A 102.2(4) . . . . ? C5A Fe1A C14A C20A 19.5(4) . . . . ? C12A Fe1A C14A C20A -153.7(3) . . . . ? C3A Fe1A C14A C20A -62.3(5) . . . . ? C4A Fe1A C14A C20A -23.5(4) . . . . ? C13A Fe1A C14A C20A -116.9(4) . . . . ? C10A C9A C15A C16A 35.9(4) . . . . ? C8A C9A C15A C16A 165.7(3) . . . . ? C10A C9A C15A C19A -153.0(3) . . . . ? C8A C9A C15A C19A -23.2(4) . . . . ? C10A C9A C15A Zr1A -57.9(3) . . . . ? C8A C9A C15A Zr1A 71.9(3) . . . . ? Cl2A Zr1A C15A C16A 167.38(16) . . . . ? Cl1A Zr1A C15A C16A 59.7(2) . . . . ? C20A Zr1A C15A C16A -88.37(18) . . . . ? C17A Zr1A C15A C16A 36.30(18) . . . . ? C18A Zr1A C15A C16A 76.8(2) . . . . ? C19A Zr1A C15A C16A 113.1(3) . . . . ? C32A Zr1A C15A C16A -57.64(18) . . . . ? C26A Zr1A C15A C16A -95.4(2) . . . . ? C27A Zr1A C15A C16A -54.6(2) . . . . ? C21A Zr1A C15A C16A -109.96(18) . . . . ? Cl2A Zr1A C15A C19A 54.26(19) . . . . ? Cl1A Zr1A C15A C19A -53.4(2) . . . . ? C20A Zr1A C15A C19A 158.5(2) . . . . ? C17A Zr1A C15A C19A -76.8(2) . . . . ? C18A Zr1A C15A C19A -36.30(19) . . . . ? C16A Zr1A C15A C19A -113.1(3) . . . . ? C32A Zr1A C15A C19A -170.76(19) . . . . ? C26A Zr1A C15A C19A 151.46(18) . . . . ? C27A Zr1A C15A C19A -167.67(18) . . . . ? C21A Zr1A C15A C19A 136.92(18) . . . . ? Cl2A Zr1A C15A C9A -70.4(2) . . . . ? Cl1A Zr1A C15A C9A -178.12(18) . . . . ? C20A Zr1A C15A C9A 33.8(2) . . . . ? C17A Zr1A C15A C9A 158.5(3) . . . . ? C18A Zr1A C15A C9A -161.0(3) . . . . ? C19A Zr1A C15A C9A -124.7(3) . . . . ? C16A Zr1A C15A C9A 122.2(3) . . . . ? C32A Zr1A C15A C9A 64.5(2) . . . . ? C26A Zr1A C15A C9A 26.8(3) . . . . ? C27A Zr1A C15A C9A 67.6(3) . . . . ? C21A Zr1A C15A C9A 12.2(2) . . . . ? C19A C15A C16A C17A 1.8(3) . . . . ? C9A C15A C16A C17A 174.5(3) . . . . ? Zr1A C15A C16A C17A -64.9(2) . . . . ? C19A C15A C16A Zr1A 66.7(2) . . . . ? C9A C15A C16A Zr1A -120.6(3) . . . . ? Cl2A Zr1A C16A C17A 100.0(2) . . . . ? Cl1A Zr1A C16A C17A -22.5(2) . . . . ? C20A Zr1A C16A C17A -157.7(2) . . . . ? C18A Zr1A C16A C17A 37.4(2) . . . . ? C19A Zr1A C16A C17A 77.9(2) . . . . ? C15A Zr1A C16A C17A 116.4(3) . . . . ? C32A Zr1A C16A C17A -124.0(2) . . . . ? C26A Zr1A C16A C17A -128.8(2) . . . . ? C27A Zr1A C16A C17A -106.7(2) . . . . ? C21A Zr1A C16A C17A -162.00(19) . . . . ? Cl2A Zr1A C16A C15A -16.4(2) . . . . ? Cl1A Zr1A C16A C15A -138.84(15) . . . . ? C20A Zr1A C16A C15A 85.98(17) . . . . ? C17A Zr1A C16A C15A -116.4(3) . . . . ? C18A Zr1A C16A C15A -78.98(19) . . . . ? C19A Zr1A C16A C15A -38.43(17) . . . . ? C32A Zr1A C16A C15A 119.65(18) . . . . ? C26A Zr1A C16A C15A 114.84(18) . . . . ? C27A Zr1A C16A C15A 136.89(17) . . . . ? C21A Zr1A C16A C15A 81.64(18) . . . . ? C15A C16A C17A C18A -1.3(3) . . . . ? Zr1A C16A C17A C18A -66.4(2) . . . . ? C15A C16A C17A Zr1A 65.1(2) . . . . ? Cl2A Zr1A C17A C16A -107.25(19) . . . . ? Cl1A Zr1A C17A C16A 159.5(2) . . . . ? C20A Zr1A C17A C16A 23.7(2) . . . . ? C18A Zr1A C17A C16A -114.8(3) . . . . ? C19A Zr1A C17A C16A -77.7(2) . . . . ? C15A Zr1A C17A C16A -36.57(18) . . . . ? C32A Zr1A C17A C16A 53.9(2) . . . . ? C26A Zr1A C17A C16A 83.3(2) . . . . ? C27A Zr1A C17A C16A 83.0(2) . . . . ? C21A Zr1A C17A C16A 28.7(3) . . . . ? Cl2A Zr1A C17A C18A 7.6(2) . . . . ? Cl1A Zr1A C17A C18A -85.67(19) . . . . ? C20A Zr1A C17A C18A 138.54(19) . . . . ? C19A Zr1A C17A C18A 37.16(19) . . . . ? C15A Zr1A C17A C18A 78.3(2) . . . . ? C16A Zr1A C17A C18A 114.8(3) . . . . ? C32A Zr1A C17A C18A 168.7(2) . . . . ? C26A Zr1A C17A C18A -161.86(18) . . . . ? C27A Zr1A C17A C18A -162.14(19) . . . . ? C21A Zr1A C17A C18A 143.5(2) . . . . ? C16A C17A C18A C19A 0.2(4) . . . . ? Zr1A C17A C18A C19A -66.6(2) . . . . ? C16A C17A C18A Zr1A 66.9(2) . . . . ? Cl2A Zr1A C18A C19A -59.3(2) . . . . ? Cl1A Zr1A C18A C19A -154.9(2) . . . . ? C20A Zr1A C18A C19A 57.1(3) . . . . ? C17A Zr1A C18A C19A 114.7(3) . . . . ? C15A Zr1A C18A C19A 36.94(18) . . . . ? C16A Zr1A C18A C19A 77.6(2) . . . . ? C32A Zr1A C18A C19A 100.5(2) . . . . ? C26A Zr1A C18A C19A -171.9(5) . . . . ? C27A Zr1A C18A C19A 141.74(19) . . . . ? C21A Zr1A C18A C19A 18.1(4) . . . . ? Cl2A Zr1A C18A C17A -173.99(19) . . . . ? Cl1A Zr1A C18A C17A 90.3(2) . . . . ? C20A Zr1A C18A C17A -57.6(3) . . . . ? C19A Zr1A C18A C17A -114.7(3) . . . . ? C15A Zr1A C18A C17A -77.8(2) . . . . ? C16A Zr1A C18A C17A -37.12(19) . . . . ? C32A Zr1A C18A C17A -14.2(3) . . . . ? C26A Zr1A C18A C17A 73.4(6) . . . . ? C27A Zr1A C18A C17A 27.0(3) . . . . ? C21A Zr1A C18A C17A -96.6(3) . . . . ? C17A C18A C19A C15A 0.9(4) . . . . ? Zr1A C18A C19A C15A -65.4(2) . . . . ? C17A C18A C19A Zr1A 66.2(2) . . . . ? C16A C15A C19A C18A -1.6(3) . . . . ? C9A C15A C19A C18A -174.1(3) . . . . ? Zr1A C15A C19A C18A 65.3(2) . . . . ? C16A C15A C19A Zr1A -66.92(19) . . . . ? C9A C15A C19A Zr1A 120.6(3) . . . . ? Cl2A Zr1A C19A C18A 119.1(2) . . . . ? Cl1A Zr1A C19A C18A 26.9(2) . . . . ? C20A Zr1A C19A C18A -138.9(2) . . . . ? C17A Zr1A C19A C18A -37.4(2) . . . . ? C15A Zr1A C19A C18A -116.1(3) . . . . ? C16A Zr1A C19A C18A -78.0(2) . . . . ? C32A Zr1A C19A C18A -104.7(2) . . . . ? C26A Zr1A C19A C18A 175.6(2) . . . . ? C27A Zr1A C19A C18A -89.7(3) . . . . ? C21A Zr1A C19A C18A -172.05(18) . . . . ? Cl2A Zr1A C19A C15A -124.85(18) . . . . ? Cl1A Zr1A C19A C15A 143.04(16) . . . . ? C20A Zr1A C19A C15A -22.8(2) . . . . ? C17A Zr1A C19A C15A 78.6(2) . . . . ? C18A Zr1A C19A C15A 116.1(3) . . . . ? C16A Zr1A C19A C15A 38.06(18) . . . . ? C32A Zr1A C19A C15A 11.4(2) . . . . ? C26A Zr1A C19A C15A -68.3(3) . . . . ? C27A Zr1A C19A C15A 26.4(4) . . . . ? C21A Zr1A C19A C15A -56.0(2) . . . . ? C13A C14A C20A C21A -90.2(4) . . . . ? C10A C14A C20A C21A 109.2(4) . . . . ? Fe1A C14A C20A C21A 7.5(5) . . . . ? C13A C14A C20A C32A 65.3(4) . . . . ? C10A C14A C20A C32A -95.3(3) . . . . ? Fe1A C14A C20A C32A 163.0(2) . . . . ? C13A C14A C20A Zr1A 159.8(2) . . . . ? C10A C14A C20A Zr1A -0.8(4) . . . . ? Fe1A C14A C20A Zr1A -102.5(3) . . . . ? Cl2A Zr1A C20A C21A -43.66(16) . . . . ? Cl1A Zr1A C20A C21A 71.76(18) . . . . ? C17A Zr1A C20A C21A 174.61(16) . . . . ? C18A Zr1A C20A C21A -155.93(17) . . . . ? C19A Zr1A C20A C21A -126.88(17) . . . . ? C15A Zr1A C20A C21A -139.30(17) . . . . ? C16A Zr1A C20A C21A -172.68(17) . . . . ? C32A Zr1A C20A C21A 108.9(2) . . . . ? C26A Zr1A C20A C21A 34.60(15) . . . . ? C27A Zr1A C20A C21A 74.32(16) . . . . ? Cl2A Zr1A C20A C32A -152.59(14) . . . . ? Cl1A Zr1A C20A C32A -37.18(19) . . . . ? C17A Zr1A C20A C32A 65.67(18) . . . . ? C18A Zr1A C20A C32A 95.1(2) . . . . ? C19A Zr1A C20A C32A 124.18(17) . . . . ? C15A Zr1A C20A C32A 111.76(17) . . . . ? C16A Zr1A C20A C32A 78.38(17) . . . . ? C26A Zr1A C20A C32A -74.34(17) . . . . ? C27A Zr1A C20A C32A -34.62(15) . . . . ? C21A Zr1A C20A C32A -108.9(2) . . . . ? Cl2A Zr1A C20A C14A 91.6(2) . . . . ? Cl1A Zr1A C20A C14A -152.98(18) . . . . ? C17A Zr1A C20A C14A -50.1(2) . . . . ? C18A Zr1A C20A C14A -20.7(3) . . . . ? C19A Zr1A C20A C14A 8.4(2) . . . . ? C15A Zr1A C20A C14A -4.0(2) . . . . ? C16A Zr1A C20A C14A -37.4(2) . . . . ? C32A Zr1A C20A C14A -115.8(3) . . . . ? C26A Zr1A C20A C14A 169.9(3) . . . . ? C27A Zr1A C20A C14A -150.4(3) . . . . ? C21A Zr1A C20A C14A 135.3(3) . . . . ? C32A C20A C21A C22A -170.3(3) . . . . ? C14A C20A C21A C22A -12.6(5) . . . . ? Zr1A C20A C21A C22A 116.4(3) . . . . ? C32A C20A C21A C26A 10.7(3) . . . . ? C14A C20A C21A C26A 168.4(3) . . . . ? Zr1A C20A C21A C26A -62.62(19) . . . . ? C32A C20A C21A Zr1A 73.33(18) . . . . ? C14A C20A C21A Zr1A -129.0(3) . . . . ? Cl2A Zr1A C21A C22A 9.5(2) . . . . ? Cl1A Zr1A C21A C22A 101.7(2) . . . . ? C20A Zr1A C21A C22A -128.1(3) . . . . ? C17A Zr1A C21A C22A -136.7(2) . . . . ? C18A Zr1A C21A C22A -70.5(4) . . . . ? C19A Zr1A C21A C22A -58.3(3) . . . . ? C15A Zr1A C21A C22A -86.4(2) . . . . ? C16A Zr1A C21A C22A -120.2(2) . . . . ? C32A Zr1A C21A C22A -168.8(3) . . . . ? C26A Zr1A C21A C22A 113.3(3) . . . . ? C27A Zr1A C21A C22A 150.8(3) . . . . ? Cl2A Zr1A C21A C26A -103.79(16) . . . . ? Cl1A Zr1A C21A C26A -11.52(18) . . . . ? C20A Zr1A C21A C26A 118.6(2) . . . . ? C17A Zr1A C21A C26A 110.1(2) . . . . ? C18A Zr1A C21A C26A 176.3(3) . . . . ? C19A Zr1A C21A C26A -171.55(16) . . . . ? C15A Zr1A C21A C26A 160.38(16) . . . . ? C16A Zr1A C21A C26A 126.50(16) . . . . ? C32A Zr1A C21A C26A 77.93(17) . . . . ? C27A Zr1A C21A C26A 37.55(15) . . . . ? Cl2A Zr1A C21A C20A 137.59(16) . . . . ? Cl1A Zr1A C21A C20A -130.13(14) . . . . ? C17A Zr1A C21A C20A -8.5(3) . . . . ? C18A Zr1A C21A C20A 57.6(4) . . . . ? C19A Zr1A C21A C20A 69.84(19) . . . . ? C15A Zr1A C21A C20A 41.76(17) . . . . ? C16A Zr1A C21A C20A 7.89(19) . . . . ? C32A Zr1A C21A C20A -40.68(15) . . . . ? C26A Zr1A C21A C20A -118.6(2) . . . . ? C27A Zr1A C21A C20A -81.06(17) . . . . ? C26A C21A C22A C23A 2.4(4) . . . . ? C20A C21A C22A C23A -176.6(3) . . . . ? Zr1A C21A C22A C23A -86.0(3) . . . . ? C21A C22A C23A C24A 0.0(5) . . . . ? C22A C23A C24A C25A -1.5(5) . . . . ? C23A C24A C25A C26A 0.5(5) . . . . ? C24A C25A C26A C21A 1.9(4) . . . . ? C24A C25A C26A C27A -173.7(3) . . . . ? C24A C25A C26A Zr1A 91.4(3) . . . . ? C22A C21A C26A C25A -3.4(4) . . . . ? C20A C21A C26A C25A 175.8(3) . . . . ? Zr1A C21A C26A C25A 116.6(3) . . . . ? C22A C21A C26A C27A 173.2(2) . . . . ? C20A C21A C26A C27A -7.7(3) . . . . ? Zr1A C21A C26A C27A -66.86(19) . . . . ? C22A C21A C26A Zr1A -120.0(2) . . . . ? C20A C21A C26A Zr1A 59.20(19) . . . . ? Cl2A Zr1A C26A C25A -43.6(2) . . . . ? Cl1A Zr1A C26A C25A 52.7(2) . . . . ? C20A Zr1A C26A C25A -152.8(3) . . . . ? C17A Zr1A C26A C25A 128.1(2) . . . . ? C18A Zr1A C26A C25A 69.6(6) . . . . ? C19A Zr1A C26A C25A -98.4(3) . . . . ? C15A Zr1A C26A C25A -144.3(2) . . . . ? C16A Zr1A C26A C25A 171.7(2) . . . . ? C32A Zr1A C26A C25A 165.8(3) . . . . ? C27A Zr1A C26A C25A 128.6(3) . . . . ? C21A Zr1A C26A C25A -117.1(3) . . . . ? Cl2A Zr1A C26A C21A 73.52(15) . . . . ? Cl1A Zr1A C26A C21A 169.82(16) . . . . ? C20A Zr1A C26A C21A -35.67(15) . . . . ? C17A Zr1A C26A C21A -114.8(2) . . . . ? C18A Zr1A C26A C21A -173.3(5) . . . . ? C19A Zr1A C26A C21A 18.7(3) . . . . ? C15A Zr1A C26A C21A -27.2(2) . . . . ? C16A Zr1A C26A C21A -71.24(19) . . . . ? C32A Zr1A C26A C21A -77.08(17) . . . . ? C27A Zr1A C26A C21A -114.3(2) . . . . ? Cl2A Zr1A C26A C27A -172.15(16) . . . . ? Cl1A Zr1A C26A C27A -75.85(16) . . . . ? C20A Zr1A C26A C27A 78.65(17) . . . . ? C17A Zr1A C26A C27A -0.5(2) . . . . ? C18A Zr1A C26A C27A -59.0(6) . . . . ? C19A Zr1A C26A C27A 133.0(3) . . . . ? C15A Zr1A C26A C27A 87.14(19) . . . . ? C16A Zr1A C26A C27A 43.1(2) . . . . ? C32A Zr1A C26A C27A 37.24(16) . . . . ? C21A Zr1A C26A C27A 114.3(2) . . . . ? C25A C26A C27A C28A 2.5(6) . . . . ? C21A C26A C27A C28A -173.5(3) . . . . ? Zr1A C26A C27A C28A 119.1(3) . . . . ? C25A C26A C27A C32A 177.5(3) . . . . ? C21A C26A C27A C32A 1.4(3) . . . . ? Zr1A C26A C27A C32A -65.93(19) . . . . ? C25A C26A C27A Zr1A -116.6(3) . . . . ? C21A C26A C27A Zr1A 67.34(19) . . . . ? Cl2A Zr1A C27A C28A -120.6(2) . . . . ? Cl1A Zr1A C27A C28A -29.7(2) . . . . ? C20A Zr1A C27A C28A 152.2(3) . . . . ? C17A Zr1A C27A C28A 49.9(3) . . . . ? C18A Zr1A C27A C28A 34.6(3) . . . . ? C19A Zr1A C27A C28A 93.0(3) . . . . ? C15A Zr1A C27A C28A 110.3(2) . . . . ? C16A Zr1A C27A C28A 83.2(3) . . . . ? C32A Zr1A C27A C28A 116.1(3) . . . . ? C26A Zr1A C27A C28A -129.8(3) . . . . ? C21A Zr1A C27A C28A -166.9(3) . . . . ? Cl2A Zr1A C27A C32A 123.28(15) . . . . ? Cl1A Zr1A C27A C32A -145.78(16) . . . . ? C20A Zr1A C27A C32A 36.07(16) . . . . ? C17A Zr1A C27A C32A -66.25(18) . . . . ? C18A Zr1A C27A C32A -81.5(2) . . . . ? C19A Zr1A C27A C32A -23.2(3) . . . . ? C15A Zr1A C27A C32A -5.8(2) . . . . ? C16A Zr1A C27A C32A -32.86(18) . . . . ? C26A Zr1A C27A C32A 114.1(2) . . . . ? C21A Zr1A C27A C32A 76.96(17) . . . . ? Cl2A Zr1A C27A C26A 9.21(18) . . . . ? Cl1A Zr1A C27A C26A 100.15(16) . . . . ? C20A Zr1A C27A C26A -78.00(17) . . . . ? C17A Zr1A C27A C26A 179.68(16) . . . . ? C18A Zr1A C27A C26A 164.45(17) . . . . ? C19A Zr1A C27A C26A -137.2(3) . . . . ? C15A Zr1A C27A C26A -119.90(17) . . . . ? C16A Zr1A C27A C26A -146.93(16) . . . . ? C32A Zr1A C27A C26A -114.1(2) . . . . ? C21A Zr1A C27A C26A -37.11(15) . . . . ? C32A C27A C28A C29A -3.4(5) . . . . ? C26A C27A C28A C29A 171.0(3) . . . . ? Zr1A C27A C28A C29A -91.8(3) . . . . ? C27A C28A C29A C30A 2.0(5) . . . . ? C28A C29A C30A C31A 0.3(5) . . . . ? C29A C30A C31A C32A -1.3(5) . . . . ? C28A C27A C32A C31A 2.4(4) . . . . ? C26A C27A C32A C31A -173.2(3) . . . . ? Zr1A C27A C32A C31A 120.3(3) . . . . ? C28A C27A C32A C20A -179.0(3) . . . . ? C26A C27A C32A C20A 5.4(3) . . . . ? Zr1A C27A C32A C20A -61.1(2) . . . . ? C28A C27A C32A Zr1A -117.9(3) . . . . ? C26A C27A C32A Zr1A 66.50(19) . . . . ? C30A C31A C32A C27A 0.0(4) . . . . ? C30A C31A C32A C20A -178.3(3) . . . . ? C30A C31A C32A Zr1A 90.7(3) . . . . ? C21A C20A C32A C27A -9.9(3) . . . . ? C14A C20A C32A C27A -171.5(2) . . . . ? Zr1A C20A C32A C27A 64.6(2) . . . . ? C21A C20A C32A C31A 168.5(3) . . . . ? C14A C20A C32A C31A 6.9(5) . . . . ? Zr1A C20A C32A C31A -116.9(3) . . . . ? C21A C20A C32A Zr1A -74.59(18) . . . . ? C14A C20A C32A Zr1A 123.9(2) . . . . ? Cl2A Zr1A C32A C27A -80.44(18) . . . . ? Cl1A Zr1A C32A C27A 35.12(17) . . . . ? C20A Zr1A C32A C27A -118.3(2) . . . . ? C17A Zr1A C32A C27A 120.28(17) . . . . ? C18A Zr1A C32A C27A 127.97(18) . . . . ? C19A Zr1A C32A C27A 168.99(16) . . . . ? C15A Zr1A C32A C27A 175.23(17) . . . . ? C16A Zr1A C32A C27A 147.00(18) . . . . ? C26A Zr1A C32A C27A -37.68(15) . . . . ? C21A Zr1A C32A C27A -78.09(17) . . . . ? Cl2A Zr1A C32A C31A 164.4(2) . . . . ? Cl1A Zr1A C32A C31A -80.1(2) . . . . ? C20A Zr1A C32A C31A 126.5(3) . . . . ? C17A Zr1A C32A C31A 5.1(3) . . . . ? C18A Zr1A C32A C31A 12.8(3) . . . . ? C19A Zr1A C32A C31A 53.8(3) . . . . ? C15A Zr1A C32A C31A 60.0(3) . . . . ? C16A Zr1A C32A C31A 31.8(2) . . . . ? C26A Zr1A C32A C31A -152.9(3) . . . . ? C27A Zr1A C32A C31A -115.2(3) . . . . ? C21A Zr1A C32A C31A 166.7(3) . . . . ? Cl2A Zr1A C32A C20A 37.88(19) . . . . ? Cl1A Zr1A C32A C20A 153.44(14) . . . . ? C17A Zr1A C32A C20A -121.40(17) . . . . ? C18A Zr1A C32A C20A -113.71(18) . . . . ? C19A Zr1A C32A C20A -72.69(19) . . . . ? C15A Zr1A C32A C20A -66.44(16) . . . . ? C16A Zr1A C32A C20A -94.68(17) . . . . ? C26A Zr1A C32A C20A 80.64(17) . . . . ? C27A Zr1A C32A C20A 118.3(2) . . . . ? C21A Zr1A C32A C20A 40.23(15) . . . . ? C10B Fe1B C1B C5B -117.18(18) . . . . ? C11B Fe1B C1B C5B -158.92(18) . . . . ? C2B Fe1B C1B C5B 116.8(3) . . . . ? C3B Fe1B C1B C5B 79.47(19) . . . . ? C12B Fe1B C1B C5B 175.8(2) . . . . ? C14B Fe1B C1B C5B -82.7(2) . . . . ? C4B Fe1B C1B C5B 36.41(18) . . . . ? C13B Fe1B C1B C5B -89.6(5) . . . . ? C10B Fe1B C1B C2B 126.01(18) . . . . ? C11B Fe1B C1B C2B 84.26(19) . . . . ? C5B Fe1B C1B C2B -116.8(3) . . . . ? C3B Fe1B C1B C2B -37.35(19) . . . . ? C12B Fe1B C1B C2B 59.0(3) . . . . ? C14B Fe1B C1B C2B 160.50(17) . . . . ? C4B Fe1B C1B C2B -80.41(19) . . . . ? C13B Fe1B C1B C2B 153.5(4) . . . . ? C10B Fe1B C1B C6B 1.8(3) . . . . ? C11B Fe1B C1B C6B -40.0(3) . . . . ? C2B Fe1B C1B C6B -124.3(3) . . . . ? C5B Fe1B C1B C6B 118.9(3) . . . . ? C3B Fe1B C1B C6B -161.6(3) . . . . ? C12B Fe1B C1B C6B -65.2(3) . . . . ? C14B Fe1B C1B C6B 36.2(3) . . . . ? C4B Fe1B C1B C6B 155.3(3) . . . . ? C13B Fe1B C1B C6B 29.3(6) . . . . ? C5B C1B C2B C3B -2.1(3) . . . . ? C6B C1B C2B C3B 175.0(3) . . . . ? Fe1B C1B C2B C3B 59.4(2) . . . . ? C5B C1B C2B Fe1B -61.47(19) . . . . ? C6B C1B C2B Fe1B 115.6(3) . . . . ? C10B Fe1B C2B C3B 173.10(18) . . . . ? C1B Fe1B C2B C3B -119.9(3) . . . . ? C11B Fe1B C2B C3B 134.2(2) . . . . ? C5B Fe1B C2B C3B -80.7(2) . . . . ? C12B Fe1B C2B C3B 94.1(2) . . . . ? C14B Fe1B C2B C3B -174.3(3) . . . . ? C4B Fe1B C2B C3B -37.23(19) . . . . ? C13B Fe1B C2B C3B 73.0(3) . . . . ? C10B Fe1B C2B C1B -67.0(2) . . . . ? C11B Fe1B C2B C1B -105.94(19) . . . . ? C5B Fe1B C2B C1B 39.17(18) . . . . ? C3B Fe1B C2B C1B 119.9(3) . . . . ? C12B Fe1B C2B C1B -145.97(18) . . . . ? C14B Fe1B C2B C1B -54.4(4) . . . . ? C4B Fe1B C2B C1B 82.66(19) . . . . ? C13B Fe1B C2B C1B -167.1(2) . . . . ? C1B C2B C3B C4B 1.4(3) . . . . ? Fe1B C2B C3B C4B 59.8(2) . . . . ? C1B C2B C3B Fe1B -58.4(2) . . . . ? C10B Fe1B C3B C4B -137.0(3) . . . . ? C1B Fe1B C3B C4B -81.6(2) . . . . ? C11B Fe1B C3B C4B -179.12(19) . . . . ? C2B Fe1B C3B C4B -119.4(3) . . . . ? C5B Fe1B C3B C4B -37.33(19) . . . . ? C12B Fe1B C3B C4B 137.7(2) . . . . ? C14B Fe1B C3B C4B 55.4(4) . . . . ? C13B Fe1B C3B C4B 95.2(2) . . . . ? C10B Fe1B C3B C2B -17.7(5) . . . . ? C1B Fe1B C3B C2B 37.75(18) . . . . ? C11B Fe1B C3B C2B -59.8(2) . . . . ? C5B Fe1B C3B C2B 82.0(2) . . . . ? C12B Fe1B C3B C2B -102.9(2) . . . . ? C14B Fe1B C3B C2B 174.7(3) . . . . ? C4B Fe1B C3B C2B 119.4(3) . . . . ? C13B Fe1B C3B C2B -145.47(18) . . . . ? C2B C3B C4B C5B -0.2(3) . . . . ? Fe1B C3B C4B C5B 58.5(2) . . . . ? C2B C3B C4B Fe1B -58.6(2) . . . . ? C10B Fe1B C4B C3B 150.4(2) . . . . ? C1B Fe1B C4B C3B 82.5(2) . . . . ? C11B Fe1B C4B C3B 2.8(6) . . . . ? C2B Fe1B C4B C3B 37.9(2) . . . . ? C5B Fe1B C4B C3B 119.7(3) . . . . ? C12B Fe1B C4B C3B -63.8(3) . . . . ? C14B Fe1B C4B C3B -158.32(19) . . . . ? C13B Fe1B C4B C3B -110.6(2) . . . . ? C10B Fe1B C4B C5B 30.7(3) . . . . ? C1B Fe1B C4B C5B -37.16(18) . . . . ? C11B Fe1B C4B C5B -116.9(5) . . . . ? C2B Fe1B C4B C5B -81.73(19) . . . . ? C3B Fe1B C4B C5B -119.7(3) . . . . ? C12B Fe1B C4B C5B 176.49(18) . . . . ? C14B Fe1B C4B C5B 82.0(2) . . . . ? C13B Fe1B C4B C5B 129.77(18) . . . . ? C3B C4B C5B C1B -1.1(3) . . . . ? Fe1B C4B C5B C1B 57.5(2) . . . . ? C3B C4B C5B Fe1B -58.6(2) . . . . ? C2B C1B C5B C4B 2.0(3) . . . . ? C6B C1B C5B C4B -175.3(3) . . . . ? Fe1B C1B C5B C4B -59.0(2) . . . . ? C2B C1B C5B Fe1B 60.96(19) . . . . ? C6B C1B C5B Fe1B -116.3(3) . . . . ? C10B Fe1B C5B C4B -164.58(18) . . . . ? C1B Fe1B C5B C4B 120.9(3) . . . . ? C11B Fe1B C5B C4B 156.9(2) . . . . ? C2B Fe1B C5B C4B 81.5(2) . . . . ? C3B Fe1B C5B C4B 37.23(19) . . . . ? C12B Fe1B C5B C4B -29.3(15) . . . . ? C14B Fe1B C5B C4B -119.59(18) . . . . ? C13B Fe1B C5B C4B -80.1(2) . . . . ? C10B Fe1B C5B C1B 74.51(19) . . . . ? C11B Fe1B C5B C1B 36.0(3) . . . . ? C2B Fe1B C5B C1B -39.41(18) . . . . ? C3B Fe1B C5B C1B -83.68(19) . . . . ? C12B Fe1B C5B C1B -150.2(13) . . . . ? C14B Fe1B C5B C1B 119.51(17) . . . . ? C4B Fe1B C5B C1B -120.9(3) . . . . ? C13B Fe1B C5B C1B 158.99(18) . . . . ? C5B C1B C6B C7B 178.4(3) . . . . ? C2B C1B C6B C7B 1.8(4) . . . . ? Fe1B C1B C6B C7B 91.0(3) . . . . ? C5B C1B C6B C8B 50.0(4) . . . . ? C2B C1B C6B C8B -126.6(3) . . . . ? Fe1B C1B C6B C8B -37.4(3) . . . . ? C1B C6B C8B C9B 70.1(3) . . . . ? C7B C6B C8B C9B -58.5(4) . . . . ? C6B C8B C9B C15B 175.4(3) . . . . ? C6B C8B C9B C10B -56.6(4) . . . . ? C15B C9B C10B C11B -134.6(3) . . . . ? C8B C9B C10B C11B 98.1(3) . . . . ? C15B C9B C10B C14B 48.6(4) . . . . ? C8B C9B C10B C14B -78.8(4) . . . . ? C15B C9B C10B Fe1B 139.3(2) . . . . ? C8B C9B C10B Fe1B 11.9(3) . . . . ? C1B Fe1B C10B C11B -107.00(18) . . . . ? C2B Fe1B C10B C11B -69.0(2) . . . . ? C5B Fe1B C10B C11B -146.86(18) . . . . ? C3B Fe1B C10B C11B -55.8(4) . . . . ? C12B Fe1B C10B C11B 36.93(18) . . . . ? C14B Fe1B C10B C11B 117.4(2) . . . . ? C4B Fe1B C10B C11B -168.1(2) . . . . ? C13B Fe1B C10B C11B 79.97(18) . . . . ? C1B Fe1B C10B C14B 135.65(17) . . . . ? C11B Fe1B C10B C14B -117.4(2) . . . . ? C2B Fe1B C10B C14B 173.62(16) . . . . ? C5B Fe1B C10B C14B 95.79(18) . . . . ? C3B Fe1B C10B C14B -173.2(3) . . . . ? C12B Fe1B C10B C14B -80.42(18) . . . . ? C4B Fe1B C10B C14B 74.6(3) . . . . ? C13B Fe1B C10B C14B -37.38(16) . . . . ? C1B Fe1B C10B C9B 11.5(2) . . . . ? C11B Fe1B C10B C9B 118.5(3) . . . . ? C2B Fe1B C10B C9B 49.5(3) . . . . ? C5B Fe1B C10B C9B -28.3(3) . . . . ? C3B Fe1B C10B C9B 62.7(5) . . . . ? C12B Fe1B C10B C9B 155.5(3) . . . . ? C14B Fe1B C10B C9B -124.1(3) . . . . ? C4B Fe1B C10B C9B -49.5(4) . . . . ? C13B Fe1B C10B C9B -161.5(3) . . . . ? C14B C10B C11B C12B 1.9(3) . . . . ? C9B C10B C11B C12B -175.6(3) . . . . ? Fe1B C10B C11B C12B -59.7(2) . . . . ? C14B C10B C11B Fe1B 61.54(18) . . . . ? C9B C10B C11B Fe1B -115.9(3) . . . . ? C10B Fe1B C11B C12B 120.3(2) . . . . ? C1B Fe1B C11B C12B -156.90(18) . . . . ? C2B Fe1B C11B C12B -115.08(19) . . . . ? C5B Fe1B C11B C12B 179.2(2) . . . . ? C3B Fe1B C11B C12B -80.1(2) . . . . ? C14B Fe1B C11B C12B 81.27(19) . . . . ? C4B Fe1B C11B C12B -82.3(5) . . . . ? C13B Fe1B C11B C12B 37.43(17) . . . . ? C1B Fe1B C11B C10B 82.83(18) . . . . ? C2B Fe1B C11B C10B 124.65(18) . . . . ? C5B Fe1B C11B C10B 58.9(3) . . . . ? C3B Fe1B C11B C10B 159.66(18) . . . . ? C12B Fe1B C11B C10B -120.3(2) . . . . ? C14B Fe1B C11B C10B -39.00(16) . . . . ? C4B Fe1B C11B C10B 157.5(5) . . . . ? C13B Fe1B C11B C10B -82.84(18) . . . . ? C10B C11B C12B C13B -1.4(3) . . . . ? Fe1B C11B C12B C13B -59.8(2) . . . . ? C10B C11B C12B Fe1B 58.45(19) . . . . ? C10B Fe1B C12B C13B 81.38(18) . . . . ? C1B Fe1B C12B C13B 157.71(19) . . . . ? C11B Fe1B C12B C13B 119.1(3) . . . . ? C2B Fe1B C12B C13B -164.17(17) . . . . ? C5B Fe1B C12B C13B -55.3(14) . . . . ? C3B Fe1B C12B C13B -120.09(19) . . . . ? C14B Fe1B C12B C13B 36.93(17) . . . . ? C4B Fe1B C12B C13B -82.1(2) . . . . ? C10B Fe1B C12B C11B -37.72(17) . . . . ? C1B Fe1B C12B C11B 38.6(3) . . . . ? C2B Fe1B C12B C11B 76.7(2) . . . . ? C5B Fe1B C12B C11B -174.4(13) . . . . ? C3B Fe1B C12B C11B 120.81(19) . . . . ? C14B Fe1B C12B C11B -82.17(18) . . . . ? C4B Fe1B C12B C11B 158.85(19) . . . . ? C13B Fe1B C12B C11B -119.1(3) . . . . ? C11B C12B C13B C14B 0.4(3) . . . . ? Fe1B C12B C13B C14B -58.18(19) . . . . ? C11B C12B C13B Fe1B 58.5(2) . . . . ? C10B Fe1B C13B C12B -82.76(19) . . . . ? C1B Fe1B C13B C12B -112.1(5) . . . . ? C11B Fe1B C13B C12B -37.92(18) . . . . ? C2B Fe1B C13B C12B 30.8(3) . . . . ? C5B Fe1B C13B C12B 173.93(19) . . . . ? C3B Fe1B C13B C12B 80.3(2) . . . . ? C14B Fe1B C13B C12B -120.8(2) . . . . ? C4B Fe1B C13B C12B 127.38(19) . . . . ? C10B Fe1B C13B C14B 38.05(16) . . . . ? C1B Fe1B C13B C14B 8.7(6) . . . . ? C11B Fe1B C13B C14B 82.89(17) . . . . ? C2B Fe1B C13B C14B 151.6(2) . . . . ? C5B Fe1B C13B C14B -65.3(2) . . . . ? C3B Fe1B C13B C14B -158.88(17) . . . . ? C12B Fe1B C13B C14B 120.8(2) . . . . ? C4B Fe1B C13B C14B -111.81(18) . . . . ? C12B C13B C14B C10B 0.8(3) . . . . ? Fe1B C13B C14B C10B -57.37(18) . . . . ? C12B C13B C14B C20B -165.8(2) . . . . ? Fe1B C13B C14B C20B 136.0(2) . . . . ? C12B C13B C14B Fe1B 58.2(2) . . . . ? C11B C10B C14B C13B -1.6(3) . . . . ? C9B C10B C14B C13B 175.7(3) . . . . ? Fe1B C10B C14B C13B 58.92(18) . . . . ? C11B C10B C14B C20B 163.8(3) . . . . ? C9B C10B C14B C20B -18.9(5) . . . . ? Fe1B C10B C14B C20B -135.7(3) . . . . ? C11B C10B C14B Fe1B -60.53(18) . . . . ? C9B C10B C14B Fe1B 116.8(3) . . . . ? C10B Fe1B C14B C13B -119.5(2) . . . . ? C1B Fe1B C14B C13B -177.38(17) . . . . ? C11B Fe1B C14B C13B -80.30(18) . . . . ? C2B Fe1B C14B C13B -136.2(3) . . . . ? C5B Fe1B C14B C13B 138.08(17) . . . . ? C3B Fe1B C14B C13B 54.1(4) . . . . ? C12B Fe1B C14B C13B -36.50(17) . . . . ? C4B Fe1B C14B C13B 94.6(2) . . . . ? C1B Fe1B C14B C10B -57.9(2) . . . . ? C11B Fe1B C14B C10B 39.18(17) . . . . ? C2B Fe1B C14B C10B -16.7(4) . . . . ? C5B Fe1B C14B C10B -102.44(18) . . . . ? C3B Fe1B C14B C10B 173.6(3) . . . . ? C12B Fe1B C14B C10B 82.98(18) . . . . ? C4B Fe1B C14B C10B -145.91(18) . . . . ? C13B Fe1B C14B C10B 119.5(2) . . . . ? C10B Fe1B C14B C20B 124.3(4) . . . . ? C1B Fe1B C14B C20B 66.4(3) . . . . ? C11B Fe1B C14B C20B 163.4(3) . . . . ? C2B Fe1B C14B C20B 107.5(4) . . . . ? C5B Fe1B C14B C20B 21.8(3) . . . . ? C3B Fe1B C14B C20B -62.2(5) . . . . ? C12B Fe1B C14B C20B -152.8(3) . . . . ? C4B Fe1B C14B C20B -21.7(4) . . . . ? C13B Fe1B C14B C20B -116.3(4) . . . . ? C10B C9B C15B C16B -151.0(3) . . . . ? C8B C9B C15B C16B -20.7(4) . . . . ? C10B C9B C15B C19B 37.5(4) . . . . ? C8B C9B C15B C19B 167.8(3) . . . . ? C10B C9B C15B Zr1B -56.5(3) . . . . ? C8B C9B C15B Zr1B 73.8(3) . . . . ? Cl2B Zr1B C15B C16B 53.17(17) . . . . ? Cl1B Zr1B C15B C16B -55.6(2) . . . . ? C20B Zr1B C15B C16B 158.23(19) . . . . ? C17B Zr1B C15B C16B -36.74(18) . . . . ? C18B Zr1B C15B C16B -77.2(2) . . . . ? C19B Zr1B C15B C16B -113.6(3) . . . . ? C21B Zr1B C15B C16B -170.80(18) . . . . ? C26B Zr1B C15B C16B -168.60(17) . . . . ? C27B Zr1B C15B C16B 150.42(17) . . . . ? C32B Zr1B C15B C16B 136.77(17) . . . . ? Cl2B Zr1B C15B C19B 166.81(16) . . . . ? Cl1B Zr1B C15B C19B 58.0(2) . . . . ? C20B Zr1B C15B C19B -88.13(18) . . . . ? C17B Zr1B C15B C19B 76.90(19) . . . . ? C18B Zr1B C15B C19B 36.39(18) . . . . ? C16B Zr1B C15B C19B 113.6(3) . . . . ? C21B Zr1B C15B C19B -57.17(18) . . . . ? C26B Zr1B C15B C19B -55.0(2) . . . . ? C27B Zr1B C15B C19B -95.9(2) . . . . ? C32B Zr1B C15B C19B -109.59(18) . . . . ? Cl2B Zr1B C15B C9B -71.4(2) . . . . ? Cl1B Zr1B C15B C9B 179.80(18) . . . . ? C20B Zr1B C15B C9B 33.6(2) . . . . ? C17B Zr1B C15B C9B -161.3(3) . . . . ? C18B Zr1B C15B C9B 158.2(3) . . . . ? C16B Zr1B C15B C9B -124.6(3) . . . . ? C19B Zr1B C15B C9B 121.8(3) . . . . ? C21B Zr1B C15B C9B 64.6(2) . . . . ? C26B Zr1B C15B C9B 66.8(3) . . . . ? C27B Zr1B C15B C9B 25.8(3) . . . . ? C32B Zr1B C15B C9B 12.2(3) . . . . ? C19B C15B C16B C17B -1.2(4) . . . . ? C9B C15B C16B C17B -174.0(3) . . . . ? Zr1B C15B C16B C17B 65.5(2) . . . . ? C19B C15B C16B Zr1B -66.7(2) . . . . ? C9B C15B C16B Zr1B 120.6(3) . . . . ? Cl2B Zr1B C16B C17B 117.8(2) . . . . ? Cl1B Zr1B C16B C17B 25.0(2) . . . . ? C20B Zr1B C16B C17B -139.1(2) . . . . ? C18B Zr1B C16B C17B -37.5(2) . . . . ? C15B Zr1B C16B C17B -116.0(3) . . . . ? C19B Zr1B C16B C17B -78.1(2) . . . . ? C21B Zr1B C16B C17B -104.7(2) . . . . ? C26B Zr1B C16B C17B -91.5(3) . . . . ? C27B Zr1B C16B C17B 175.5(3) . . . . ? C32B Zr1B C16B C17B -171.82(19) . . . . ? Cl2B Zr1B C16B C15B -126.13(17) . . . . ? Cl1B Zr1B C16B C15B 141.07(15) . . . . ? C20B Zr1B C16B C15B -23.0(2) . . . . ? C17B Zr1B C16B C15B 116.0(3) . . . . ? C18B Zr1B C16B C15B 78.6(2) . . . . ? C19B Zr1B C16B C15B 37.96(17) . . . . ? C21B Zr1B C16B C15B 11.4(2) . . . . ? C26B Zr1B C16B C15B 24.6(3) . . . . ? C27B Zr1B C16B C15B -68.4(3) . . . . ? C32B Zr1B C16B C15B -55.8(2) . . . . ? C15B C16B C17B C18B 0.4(4) . . . . ? Zr1B C16B C17B C18B 66.7(2) . . . . ? C15B C16B C17B Zr1B -66.3(2) . . . . ? Cl2B Zr1B C17B C18B -174.78(19) . . . . ? Cl1B Zr1B C17B C18B 88.92(19) . . . . ? C20B Zr1B C17B C18B -57.4(2) . . . . ? C16B Zr1B C17B C18B -114.3(3) . . . . ? C15B Zr1B C17B C18B -77.8(2) . . . . ? C19B Zr1B C17B C18B -37.14(19) . . . . ? C21B Zr1B C17B C18B -13.4(2) . . . . ? C26B Zr1B C17B C18B 27.7(3) . . . . ? C27B Zr1B C17B C18B 74.5(6) . . . . ? C32B Zr1B C17B C18B -95.7(3) . . . . ? Cl2B Zr1B C17B C16B -60.5(2) . . . . ? Cl1B Zr1B C17B C16B -156.8(2) . . . . ? C20B Zr1B C17B C16B 56.9(3) . . . . ? C18B Zr1B C17B C16B 114.3(3) . . . . ? C15B Zr1B C17B C16B 36.51(19) . . . . ? C19B Zr1B C17B C16B 77.2(2) . . . . ? C21B Zr1B C17B C16B 100.9(2) . . . . ? C26B Zr1B C17B C16B 142.1(2) . . . . ? C27B Zr1B C17B C16B -171.1(5) . . . . ? C32B Zr1B C17B C16B 18.6(4) . . . . ? C16B C17B C18B C19B 0.6(4) . . . . ? Zr1B C17B C18B C19B 67.4(2) . . . . ? C16B C17B C18B Zr1B -66.8(2) . . . . ? Cl2B Zr1B C18B C17B 6.6(2) . . . . ? Cl1B Zr1B C18B C17B -86.69(19) . . . . ? C20B Zr1B C18B C17B 138.74(19) . . . . ? C16B Zr1B C18B C17B 37.62(19) . . . . ? C15B Zr1B C18B C17B 78.2(2) . . . . ? C19B Zr1B C18B C17B 114.8(3) . . . . ? C21B Zr1B C18B C17B 169.3(2) . . . . ? C26B Zr1B C18B C17B -161.84(19) . . . . ? C27B Zr1B C18B C17B -162.29(19) . . . . ? C32B Zr1B C18B C17B 143.4(2) . . . . ? Cl2B Zr1B C18B C19B -108.25(19) . . . . ? Cl1B Zr1B C18B C19B 158.5(2) . . . . ? C20B Zr1B C18B C19B 23.9(2) . . . . ? C17B Zr1B C18B C19B -114.8(3) . . . . ? C16B Zr1B C18B C19B -77.2(2) . . . . ? C15B Zr1B C18B C19B -36.65(18) . . . . ? C21B Zr1B C18B C19B 54.5(2) . . . . ? C26B Zr1B C18B C19B 83.3(2) . . . . ? C27B Zr1B C18B C19B 82.9(2) . . . . ? C32B Zr1B C18B C19B 28.6(3) . . . . ? C17B C18B C19B C15B -1.4(4) . . . . ? Zr1B C18B C19B C15B 64.9(2) . . . . ? C17B C18B C19B Zr1B -66.3(2) . . . . ? C16B C15B C19B C18B 1.6(3) . . . . ? C9B C15B C19B C18B 174.6(3) . . . . ? Zr1B C15B C19B C18B -64.3(2) . . . . ? C16B C15B C19B Zr1B 65.9(2) . . . . ? C9B C15B C19B Zr1B -121.1(3) . . . . ? Cl2B Zr1B C19B C18B 99.0(2) . . . . ? Cl1B Zr1B C19B C18B -23.3(2) . . . . ? C20B Zr1B C19B C18B -157.5(2) . . . . ? C17B Zr1B C19B C18B 37.4(2) . . . . ? C16B Zr1B C19B C18B 78.4(2) . . . . ? C15B Zr1B C19B C18B 116.2(3) . . . . ? C21B Zr1B C19B C18B -123.4(2) . . . . ? C26B Zr1B C19B C18B -106.9(2) . . . . ? C27B Zr1B C19B C18B -129.4(2) . . . . ? C32B Zr1B C19B C18B -161.94(19) . . . . ? Cl2B Zr1B C19B C15B -17.2(2) . . . . ? Cl1B Zr1B C19B C15B -139.50(15) . . . . ? C20B Zr1B C19B C15B 86.34(18) . . . . ? C17B Zr1B C19B C15B -78.82(19) . . . . ? C18B Zr1B C19B C15B -116.2(3) . . . . ? C16B Zr1B C19B C15B -37.82(17) . . . . ? C21B Zr1B C19B C15B 120.37(18) . . . . ? C26B Zr1B C19B C15B 136.91(17) . . . . ? C27B Zr1B C19B C15B 114.37(18) . . . . ? C32B Zr1B C19B C15B 81.88(18) . . . . ? C13B C14B C20B C32B -88.3(4) . . . . ? C10B C14B C20B C32B 108.2(4) . . . . ? Fe1B C14B C20B C32B 7.7(5) . . . . ? C13B C14B C20B C21B 67.7(4) . . . . ? C10B C14B C20B C21B -95.8(3) . . . . ? Fe1B C14B C20B C21B 163.7(2) . . . . ? C13B C14B C20B Zr1B 161.1(2) . . . . ? C10B C14B C20B Zr1B -2.4(4) . . . . ? Fe1B C14B C20B Zr1B -102.9(3) . . . . ? Cl2B Zr1B C20B C32B -42.94(17) . . . . ? Cl1B Zr1B C20B C32B 73.92(18) . . . . ? C17B Zr1B C20B C32B -155.85(17) . . . . ? C18B Zr1B C20B C32B 174.82(16) . . . . ? C16B Zr1B C20B C32B -126.65(17) . . . . ? C15B Zr1B C20B C32B -139.05(17) . . . . ? C19B Zr1B C20B C32B -172.38(18) . . . . ? C21B Zr1B C20B C32B 108.8(2) . . . . ? C26B Zr1B C20B C32B 73.64(17) . . . . ? C27B Zr1B C20B C32B 34.15(16) . . . . ? Cl2B Zr1B C20B C21B -151.72(15) . . . . ? Cl1B Zr1B C20B C21B -34.9(2) . . . . ? C17B Zr1B C20B C21B 95.4(2) . . . . ? C18B Zr1B C20B C21B 66.03(18) . . . . ? C16B Zr1B C20B C21B 124.57(17) . . . . ? C15B Zr1B C20B C21B 112.17(17) . . . . ? C19B Zr1B C20B C21B 78.84(17) . . . . ? C26B Zr1B C20B C21B -35.15(16) . . . . ? C27B Zr1B C20B C21B -74.63(17) . . . . ? C32B Zr1B C20B C21B -108.8(2) . . . . ? Cl2B Zr1B C20B C14B 92.5(2) . . . . ? Cl1B Zr1B C20B C14B -150.67(18) . . . . ? C17B Zr1B C20B C14B -20.4(3) . . . . ? C18B Zr1B C20B C14B -49.8(2) . . . . ? C16B Zr1B C20B C14B 8.8(2) . . . . ? C15B Zr1B C20B C14B -3.6(2) . . . . ? C19B Zr1B C20B C14B -37.0(2) . . . . ? C21B Zr1B C20B C14B -115.8(3) . . . . ? C26B Zr1B C20B C14B -151.0(3) . . . . ? C27B Zr1B C20B C14B 169.6(3) . . . . ? C32B Zr1B C20B C14B 135.4(3) . . . . ? C32B C20B C21B C26B -9.4(3) . . . . ? C14B C20B C21B C26B -171.2(2) . . . . ? Zr1B C20B C21B C26B 66.1(2) . . . . ? C32B C20B C21B C22B 168.9(3) . . . . ? C14B C20B C21B C22B 7.1(5) . . . . ? Zr1B C20B C21B C22B -115.6(3) . . . . ? C32B C20B C21B Zr1B -75.49(19) . . . . ? C14B C20B C21B Zr1B 122.7(2) . . . . ? Cl2B Zr1B C21B C26B -77.50(18) . . . . ? Cl1B Zr1B C21B C26B 37.75(16) . . . . ? C20B Zr1B C21B C26B -117.1(2) . . . . ? C17B Zr1B C21B C26B 129.02(17) . . . . ? C18B Zr1B C21B C26B 121.75(17) . . . . ? C16B Zr1B C21B C26B 170.48(16) . . . . ? C15B Zr1B C21B C26B 176.63(16) . . . . ? C19B Zr1B C21B C26B 148.63(18) . . . . ? C27B Zr1B C21B C26B -37.19(16) . . . . ? C32B Zr1B C21B C26B -77.26(17) . . . . ? Cl2B Zr1B C21B C22B 166.3(2) . . . . ? Cl1B Zr1B C21B C22B -78.5(2) . . . . ? C20B Zr1B C21B C22B 126.7(3) . . . . ? C17B Zr1B C21B C22B 12.8(3) . . . . ? C18B Zr1B C21B C22B 5.5(3) . . . . ? C16B Zr1B C21B C22B 54.3(3) . . . . ? C15B Zr1B C21B C22B 60.4(2) . . . . ? C19B Zr1B C21B C22B 32.4(2) . . . . ? C26B Zr1B C21B C22B -116.2(3) . . . . ? C27B Zr1B C21B C22B -153.4(3) . . . . ? C32B Zr1B C21B C22B 166.5(3) . . . . ? Cl2B Zr1B C21B C20B 39.6(2) . . . . ? Cl1B Zr1B C21B C20B 154.85(15) . . . . ? C17B Zr1B C21B C20B -113.87(18) . . . . ? C18B Zr1B C21B C20B -121.15(17) . . . . ? C16B Zr1B C21B C20B -72.41(19) . . . . ? C15B Zr1B C21B C20B -66.26(17) . . . . ? C19B Zr1B C21B C20B -94.27(17) . . . . ? C26B Zr1B C21B C20B 117.1(2) . . . . ? C27B Zr1B C21B C20B 79.91(17) . . . . ? C32B Zr1B C21B C20B 39.85(15) . . . . ? C26B C21B C22B C23B -0.7(4) . . . . ? C20B C21B C22B C23B -178.9(3) . . . . ? Zr1B C21B C22B C23B 90.6(3) . . . . ? C21B C22B C23B C24B -0.8(5) . . . . ? C22B C23B C24B C25B 0.8(5) . . . . ? C23B C24B C25B C26B 0.8(5) . . . . ? C24B C25B C26B C21B -2.4(5) . . . . ? C24B C25B C26B C27B 173.0(3) . . . . ? C24B C25B C26B Zr1B -89.1(3) . . . . ? C22B C21B C26B C25B 2.4(4) . . . . ? C20B C21B C26B C25B -179.1(3) . . . . ? Zr1B C21B C26B C25B -116.9(3) . . . . ? C22B C21B C26B C27B -174.0(3) . . . . ? C20B C21B C26B C27B 4.5(3) . . . . ? Zr1B C21B C26B C27B 66.7(2) . . . . ? C22B C21B C26B Zr1B 119.3(3) . . . . ? C20B C21B C26B Zr1B -62.19(19) . . . . ? Cl2B Zr1B C26B C25B -119.2(2) . . . . ? Cl1B Zr1B C26B C25B -27.9(2) . . . . ? C20B Zr1B C26B C25B 151.9(3) . . . . ? C17B Zr1B C26B C25B 34.4(3) . . . . ? C18B Zr1B C26B C25B 50.1(3) . . . . ? C16B Zr1B C26B C25B 94.7(3) . . . . ? C15B Zr1B C26B C25B 110.8(3) . . . . ? C19B Zr1B C26B C25B 83.6(3) . . . . ? C21B Zr1B C26B C25B 115.0(3) . . . . ? C27B Zr1B C26B C25B -130.4(3) . . . . ? C32B Zr1B C26B C25B -167.5(3) . . . . ? Cl2B Zr1B C26B C21B 125.79(15) . . . . ? Cl1B Zr1B C26B C21B -142.83(16) . . . . ? C20B Zr1B C26B C21B 36.96(15) . . . . ? C17B Zr1B C26B C21B -80.6(2) . . . . ? C18B Zr1B C26B C21B -64.92(18) . . . . ? C16B Zr1B C26B C21B -20.3(3) . . . . ? C15B Zr1B C26B C21B -4.1(2) . . . . ? C19B Zr1B C26B C21B -31.40(18) . . . . ? C27B Zr1B C26B C21B 114.6(2) . . . . ? C32B Zr1B C26B C21B 77.50(17) . . . . ? Cl2B Zr1B C26B C27B 11.21(19) . . . . ? Cl1B Zr1B C26B C27B 102.59(16) . . . . ? C20B Zr1B C26B C27B -77.62(17) . . . . ? C17B Zr1B C26B C27B 164.84(19) . . . . ? C18B Zr1B C26B C27B -179.50(17) . . . . ? C16B Zr1B C26B C27B -134.9(2) . . . . ? C15B Zr1B C26B C27B -118.73(17) . . . . ? C19B Zr1B C26B C27B -145.98(17) . . . . ? C21B Zr1B C26B C27B -114.6(2) . . . . ? C32B Zr1B C26B C27B -37.08(16) . . . . ? C25B C26B C27B C28B 2.4(6) . . . . ? C21B C26B C27B C28B 178.2(3) . . . . ? Zr1B C26B C27B C28B -116.7(4) . . . . ? C25B C26B C27B C32B -173.6(3) . . . . ? C21B C26B C27B C32B 2.2(3) . . . . ? Zr1B C26B C27B C32B 67.4(2) . . . . ? C25B C26B C27B Zr1B 119.1(3) . . . . ? C21B C26B C27B Zr1B -65.1(2) . . . . ? Cl2B Zr1B C27B C28B -41.6(2) . . . . ? Cl1B Zr1B C27B C28B 55.3(2) . . . . ? C20B Zr1B C27B C28B -152.2(3) . . . . ? C17B Zr1B C27B C28B 69.6(7) . . . . ? C18B Zr1B C27B C28B 129.5(3) . . . . ? C16B Zr1B C27B C28B -97.6(3) . . . . ? C15B Zr1B C27B C28B -142.7(2) . . . . ? C19B Zr1B C27B C28B 173.2(2) . . . . ? C21B Zr1B C27B C28B 165.9(3) . . . . ? C26B Zr1B C27B C28B 128.8(3) . . . . ? C32B Zr1B C27B C28B -117.1(3) . . . . ? Cl2B Zr1B C27B C32B 75.42(17) . . . . ? Cl1B Zr1B C27B C32B 172.34(17) . . . . ? C20B Zr1B C27B C32B -35.12(16) . . . . ? C17B Zr1B C27B C32B -173.4(5) . . . . ? C18B Zr1B C27B C32B -113.4(2) . . . . ? C16B Zr1B C27B C32B 19.4(4) . . . . ? C15B Zr1B C27B C32B -25.7(2) . . . . ? C19B Zr1B C27B C32B -69.8(2) . . . . ? C21B Zr1B C27B C32B -77.06(18) . . . . ? C26B Zr1B C27B C32B -114.2(2) . . . . ? Cl2B Zr1B C27B C26B -170.38(16) . . . . ? Cl1B Zr1B C27B C26B -73.46(16) . . . . ? C20B Zr1B C27B C26B 79.08(18) . . . . ? C17B Zr1B C27B C26B -59.2(6) . . . . ? C18B Zr1B C27B C26B 0.8(3) . . . . ? C16B Zr1B C27B C26B 133.6(3) . . . . ? C15B Zr1B C27B C26B 88.5(2) . . . . ? C19B Zr1B C27B C26B 44.4(2) . . . . ? C21B Zr1B C27B C26B 37.13(16) . . . . ? C32B Zr1B C27B C26B 114.2(2) . . . . ? C32B C27B C28B C29B 1.8(5) . . . . ? C26B C27B C28B C29B -173.7(3) . . . . ? Zr1B C27B C28B C29B 91.6(4) . . . . ? C27B C28B C29B C30B 1.9(6) . . . . ? C28B C29B C30B C31B -2.9(6) . . . . ? C29B C30B C31B C32B 0.1(6) . . . . ? C30B C31B C32B C27B 3.5(5) . . . . ? C30B C31B C32B C20B -176.2(3) . . . . ? C30B C31B C32B Zr1B -85.7(4) . . . . ? C28B C27B C32B C31B -4.5(4) . . . . ? C26B C27B C32B C31B 172.0(3) . . . . ? Zr1B C27B C32B C31B -121.5(3) . . . . ? C28B C27B C32B C20B 175.3(3) . . . . ? C26B C27B C32B C20B -8.3(3) . . . . ? Zr1B C27B C32B C20B 58.3(2) . . . . ? C28B C27B C32B Zr1B 117.0(3) . . . . ? C26B C27B C32B Zr1B -66.5(2) . . . . ? C21B C20B C32B C31B -169.5(3) . . . . ? C14B C20B C32B C31B -11.3(6) . . . . ? Zr1B C20B C32B C31B 117.5(3) . . . . ? C21B C20B C32B C27B 10.8(3) . . . . ? C14B C20B C32B C27B 169.0(3) . . . . ? Zr1B C20B C32B C27B -62.2(2) . . . . ? C21B C20B C32B Zr1B 72.96(18) . . . . ? C14B C20B C32B Zr1B -128.8(3) . . . . ? Cl2B Zr1B C32B C31B 11.2(2) . . . . ? Cl1B Zr1B C32B C31B 104.6(2) . . . . ? C20B Zr1B C32B C31B -127.4(3) . . . . ? C17B Zr1B C32B C31B -70.3(4) . . . . ? C18B Zr1B C32B C31B -135.5(2) . . . . ? C16B Zr1B C32B C31B -57.7(3) . . . . ? C15B Zr1B C32B C31B -85.3(2) . . . . ? C19B Zr1B C32B C31B -119.2(2) . . . . ? C21B Zr1B C32B C31B -168.6(3) . . . . ? C26B Zr1B C32B C31B 150.8(3) . . . . ? C27B Zr1B C32B C31B 113.3(3) . . . . ? Cl2B Zr1B C32B C27B -102.03(17) . . . . ? Cl1B Zr1B C32B C27B -8.71(19) . . . . ? C20B Zr1B C32B C27B 119.4(2) . . . . ? C17B Zr1B C32B C27B 176.5(3) . . . . ? C18B Zr1B C32B C27B 111.2(2) . . . . ? C16B Zr1B C32B C27B -170.97(17) . . . . ? C15B Zr1B C32B C27B 161.41(17) . . . . ? C19B Zr1B C32B C27B 127.57(17) . . . . ? C21B Zr1B C32B C27B 78.14(18) . . . . ? C26B Zr1B C32B C27B 37.55(17) . . . . ? Cl2B Zr1B C32B C20B 138.60(16) . . . . ? Cl1B Zr1B C32B C20B -128.08(15) . . . . ? C17B Zr1B C32B C20B 57.1(4) . . . . ? C18B Zr1B C32B C20B -8.2(3) . . . . ? C16B Zr1B C32B C20B 69.7(2) . . . . ? C15B Zr1B C32B C20B 42.04(18) . . . . ? C19B Zr1B C32B C20B 8.20(19) . . . . ? C21B Zr1B C32B C20B -41.23(16) . . . . ? C26B Zr1B C32B C20B -81.82(18) . . . . ? C27B Zr1B C32B C20B -119.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.557 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.082 # Attachment '4.cif' data_erk4330 _database_code_depnum_ccdc_archive 'CCDC 806927' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 Cl Fe N2' _chemical_formula_weight 422.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.4638(3) _cell_length_b 12.4287(4) _cell_length_c 17.3060(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.385(1) _cell_angle_gamma 90.00 _cell_volume 2018.69(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4761 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.8781 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16549 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.84 _reflns_number_total 4786 _reflns_number_gt 3002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0568P)^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 4786 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.96281(4) 0.30483(3) 0.16054(2) 0.03137(14) Uani 1 1 d . . . N1 N 1.3039(2) 0.11784(18) 0.07442(13) 0.0341(6) Uani 1 1 d . . . H1 H 1.3026 0.0828 0.0275 0.041 Uiso 1 1 calc R . . N2 N 1.2708(2) 0.37716(19) 0.17059(13) 0.0330(6) Uani 1 1 d . . . C1 C 0.9024(3) 0.3307(2) 0.04527(16) 0.0345(7) Uani 1 1 d . . . C2 C 0.7865(3) 0.2885(2) 0.08023(17) 0.0395(7) Uani 1 1 d . . . H2 H 0.7377 0.2243 0.0657 0.047 Uiso 1 1 calc R . . C3 C 0.7565(3) 0.3586(3) 0.14044(18) 0.0446(8) Uani 1 1 d . . . H3 H 0.6851 0.3485 0.1728 0.054 Uiso 1 1 calc R . . C4 C 0.8521(3) 0.4465(3) 0.14357(18) 0.0431(8) Uani 1 1 d . . . H4 H 0.8554 0.5050 0.1781 0.052 Uiso 1 1 calc R . . C5 C 0.9422(3) 0.4302(2) 0.08510(17) 0.0391(7) Uani 1 1 d . . . H5 H 1.0156 0.4766 0.0742 0.047 Uiso 1 1 calc R . . C6 C 0.9766(3) 0.2805(2) -0.01809(16) 0.0344(7) Uani 1 1 d . . . H6 H 0.9751 0.3351 -0.0598 0.041 Uiso 1 1 calc R . . C7 C 0.8957(3) 0.1833(2) -0.05468(17) 0.0428(8) Uani 1 1 d . . . H7A H 0.8805 0.1321 -0.0142 0.064 Uiso 1 1 calc R . . H7B H 0.9507 0.1495 -0.0916 0.064 Uiso 1 1 calc R . . H7C H 0.8044 0.2064 -0.0815 0.064 Uiso 1 1 calc R . . C8 C 1.1346(3) 0.2556(2) 0.00889(15) 0.0337(7) Uani 1 1 d . . . H8A H 1.1792 0.2314 -0.0361 0.040 Uiso 1 1 calc R . . H8B H 1.1824 0.3220 0.0283 0.040 Uiso 1 1 calc R . . C9 C 1.1584(3) 0.1694(2) 0.07292(15) 0.0306(6) Uani 1 1 d . . . H9 H 1.0884 0.1118 0.0570 0.037 Uiso 1 1 calc R . . C10 C 1.1275(3) 0.2062(2) 0.15233(15) 0.0294(6) Uani 1 1 d . . . C11 C 1.0275(3) 0.1533(2) 0.19364(16) 0.0335(6) Uani 1 1 d . . . H11 H 0.9808 0.0883 0.1791 0.040 Uiso 1 1 calc R . . C12 C 1.0101(3) 0.2154(2) 0.26070(16) 0.0373(7) Uani 1 1 d . . . H12 H 0.9489 0.1989 0.2977 0.045 Uiso 1 1 calc R . . C13 C 1.1002(3) 0.3063(2) 0.26230(16) 0.0341(7) Uani 1 1 d . . . H13 H 1.1100 0.3601 0.3008 0.041 Uiso 1 1 calc R . . C14 C 1.1740(3) 0.3021(2) 0.19522(15) 0.0302(6) Uani 1 1 d . . . C15 C 1.3291(3) 0.0331(2) 0.13565(18) 0.0454(8) Uani 1 1 d . . . H15A H 1.4158 -0.0057 0.1294 0.068 Uiso 1 1 calc R . . H15B H 1.2493 -0.0165 0.1306 0.068 Uiso 1 1 calc R . . H15C H 1.3385 0.0665 0.1867 0.068 Uiso 1 1 calc R . . C16 C 1.4262(3) 0.1929(2) 0.07987(19) 0.0422(8) Uani 1 1 d . . . H16A H 1.4275 0.2367 0.1263 0.063 Uiso 1 1 calc R . . H16B H 1.4171 0.2390 0.0343 0.063 Uiso 1 1 calc R . . H16C H 1.5141 0.1522 0.0826 0.063 Uiso 1 1 calc R . . C17 C 1.2858(3) 0.4675(2) 0.20491(16) 0.0339(7) Uani 1 1 d . . . H17 H 1.2354 0.4802 0.2474 0.041 Uiso 1 1 calc R . . C18 C 1.3783(3) 0.5531(2) 0.18105(16) 0.0329(6) Uani 1 1 d . . . C19 C 1.4635(3) 0.5379(3) 0.12206(19) 0.0478(8) Uani 1 1 d . . . H19 H 1.4617 0.4718 0.0956 0.057 Uiso 1 1 calc R . . C20 C 1.5502(4) 0.6197(3) 0.1025(2) 0.0588(10) Uani 1 1 d . . . H20 H 1.6096 0.6083 0.0638 0.071 Uiso 1 1 calc R . . C21 C 1.5509(3) 0.7183(3) 0.1392(2) 0.0519(9) Uani 1 1 d . . . H21 H 1.6079 0.7745 0.1243 0.062 Uiso 1 1 calc R . . C22 C 1.4677(3) 0.7336(3) 0.19772(18) 0.0435(8) Uani 1 1 d . . . H22 H 1.4688 0.8003 0.2234 0.052 Uiso 1 1 calc R . . C23 C 1.3829(3) 0.6515(3) 0.21887(17) 0.0419(7) Uani 1 1 d . . . H23 H 1.3273 0.6624 0.2595 0.050 Uiso 1 1 calc R . . Cl1 Cl 1.27816(8) 0.01124(6) -0.08365(4) 0.0412(2) 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 0.0369(2) 0.0287(2) 0.0298(2) 0.00074(18) 0.00890(16) -0.00266(18) N1 0.0423(14) 0.0309(14) 0.0298(13) -0.0058(11) 0.0070(10) 0.0003(11) N2 0.0368(13) 0.0331(14) 0.0303(13) -0.0018(11) 0.0087(10) -0.0073(10) C1 0.0421(16) 0.0339(17) 0.0262(15) 0.0048(13) -0.0004(12) -0.0010(13) C2 0.0350(16) 0.0386(18) 0.0440(19) -0.0005(15) 0.0021(13) -0.0022(13) C3 0.0411(17) 0.045(2) 0.049(2) 0.0020(17) 0.0118(14) 0.0044(15) C4 0.0524(19) 0.0343(18) 0.0432(19) -0.0055(15) 0.0080(14) 0.0093(15) C5 0.0501(18) 0.0272(17) 0.0397(18) 0.0066(14) 0.0046(14) 0.0011(13) C6 0.0451(17) 0.0338(17) 0.0243(15) 0.0043(12) 0.0048(12) -0.0029(13) C7 0.0525(18) 0.0439(19) 0.0317(17) -0.0004(14) 0.0041(14) -0.0086(15) C8 0.0417(17) 0.0338(17) 0.0267(15) -0.0031(13) 0.0082(12) -0.0023(13) C9 0.0362(15) 0.0280(16) 0.0279(15) -0.0044(12) 0.0054(11) -0.0065(12) C10 0.0350(15) 0.0309(15) 0.0224(14) 0.0024(12) 0.0044(11) -0.0020(12) C11 0.0420(16) 0.0269(15) 0.0320(16) 0.0052(13) 0.0067(12) -0.0046(13) C12 0.0451(17) 0.0431(19) 0.0254(15) 0.0030(13) 0.0105(12) -0.0029(14) C13 0.0430(16) 0.0354(17) 0.0240(15) -0.0034(13) 0.0047(12) -0.0049(13) C14 0.0375(15) 0.0277(15) 0.0258(15) -0.0015(12) 0.0051(11) -0.0060(12) C15 0.0515(18) 0.0346(18) 0.049(2) 0.0030(15) 0.0034(14) 0.0073(14) C16 0.0407(17) 0.0394(18) 0.048(2) -0.0056(15) 0.0128(14) -0.0048(14) C17 0.0392(16) 0.0322(17) 0.0313(16) -0.0035(13) 0.0086(12) -0.0037(13) C18 0.0371(15) 0.0276(16) 0.0341(16) -0.0013(13) 0.0048(12) -0.0010(12) C19 0.059(2) 0.0365(19) 0.052(2) -0.0038(16) 0.0242(16) -0.0051(15) C20 0.072(2) 0.048(2) 0.065(2) -0.0001(19) 0.0395(19) -0.0077(18) C21 0.058(2) 0.041(2) 0.058(2) 0.0074(17) 0.0119(17) -0.0166(16) C22 0.0504(19) 0.0340(18) 0.045(2) -0.0042(15) 0.0014(15) -0.0107(14) C23 0.0471(18) 0.0412(18) 0.0385(18) -0.0076(15) 0.0088(13) -0.0061(15) Cl1 0.0579(5) 0.0335(4) 0.0327(4) -0.0030(3) 0.0082(3) 0.0013(3) _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 C10 2.002(3) . ? Fe1 C14 2.012(3) . ? Fe1 C5 2.026(3) . ? Fe1 C1 2.029(3) . ? Fe1 C2 2.040(3) . ? Fe1 C11 2.039(3) . ? Fe1 C4 2.050(3) . ? Fe1 C3 2.051(3) . ? Fe1 C13 2.051(3) . ? Fe1 C12 2.059(3) . ? N1 C16 1.480(3) . ? N1 C15 1.491(4) . ? N1 C9 1.516(3) . ? N2 C17 1.270(3) . ? N2 C14 1.411(3) . ? C1 C2 1.419(4) . ? C1 C5 1.442(4) . ? C1 C6 1.511(4) . ? C2 C3 1.415(4) . ? C3 C4 1.415(4) . ? C4 C5 1.419(4) . ? C6 C7 1.524(4) . ? C6 C8 1.539(4) . ? C8 C9 1.536(4) . ? C9 C10 1.512(4) . ? C10 C11 1.419(4) . ? C10 C14 1.443(4) . ? C11 C12 1.421(4) . ? C12 C13 1.414(4) . ? C13 C14 1.431(4) . ? C17 C18 1.471(4) . ? C18 C23 1.386(4) . ? C18 C19 1.392(4) . ? C19 C20 1.376(4) . ? C20 C21 1.379(5) . ? C21 C22 1.373(5) . ? C22 C23 1.377(4) . ? 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 C10 Fe1 C14 42.12(10) . . ? C10 Fe1 C5 115.87(11) . . ? C14 Fe1 C5 102.39(11) . . ? C10 Fe1 C1 98.68(11) . . ? C14 Fe1 C1 116.07(11) . . ? C5 Fe1 C1 41.67(11) . . ? C10 Fe1 C2 117.81(11) . . ? C14 Fe1 C2 153.60(12) . . ? C5 Fe1 C2 68.60(12) . . ? C1 Fe1 C2 40.83(11) . . ? C10 Fe1 C11 41.10(11) . . ? C14 Fe1 C11 69.51(11) . . ? C5 Fe1 C11 153.09(11) . . ? C1 Fe1 C11 117.32(11) . . ? C2 Fe1 C11 106.80(11) . . ? C10 Fe1 C4 154.61(12) . . ? C14 Fe1 C4 121.78(12) . . ? C5 Fe1 C4 40.73(12) . . ? C1 Fe1 C4 69.44(12) . . ? C2 Fe1 C4 68.29(12) . . ? C11 Fe1 C4 164.26(11) . . ? C10 Fe1 C3 156.98(12) . . ? C14 Fe1 C3 160.70(12) . . ? C5 Fe1 C3 68.25(12) . . ? C1 Fe1 C3 68.88(12) . . ? C2 Fe1 C3 40.48(12) . . ? C11 Fe1 C3 126.40(12) . . ? C4 Fe1 C3 40.38(12) . . ? C10 Fe1 C13 69.67(11) . . ? C14 Fe1 C13 41.22(11) . . ? C5 Fe1 C13 122.99(11) . . ? C1 Fe1 C13 155.58(11) . . ? C2 Fe1 C13 163.56(12) . . ? C11 Fe1 C13 68.44(11) . . ? C4 Fe1 C13 111.80(12) . . ? C3 Fe1 C13 128.89(12) . . ? C10 Fe1 C12 69.06(11) . . ? C14 Fe1 C12 68.90(11) . . ? C5 Fe1 C12 161.80(12) . . ? C1 Fe1 C12 156.41(12) . . ? C2 Fe1 C12 126.15(12) . . ? C11 Fe1 C12 40.56(11) . . ? C4 Fe1 C12 129.47(12) . . ? C3 Fe1 C12 114.69(12) . . ? C13 Fe1 C12 40.24(11) . . ? C16 N1 C15 110.3(2) . . ? C16 N1 C9 115.8(2) . . ? C15 N1 C9 111.9(2) . . ? C17 N2 C14 118.7(2) . . ? C2 C1 C5 106.4(3) . . ? C2 C1 C6 127.8(3) . . ? C5 C1 C6 125.7(3) . . ? C2 C1 Fe1 69.99(16) . . ? C5 C1 Fe1 69.07(15) . . ? C6 C1 Fe1 123.32(19) . . ? C3 C2 C1 109.0(3) . . ? C3 C2 Fe1 70.19(17) . . ? C1 C2 Fe1 69.18(15) . . ? C4 C3 C2 108.4(3) . . ? C4 C3 Fe1 69.79(16) . . ? C2 C3 Fe1 69.33(16) . . ? C3 C4 C5 107.6(3) . . ? C3 C4 Fe1 69.83(17) . . ? C5 C4 Fe1 68.72(16) . . ? C4 C5 C1 108.6(3) . . ? C4 C5 Fe1 70.55(17) . . ? C1 C5 Fe1 69.26(16) . . ? C1 C6 C7 111.9(2) . . ? C1 C6 C8 112.8(2) . . ? C7 C6 C8 112.5(2) . . ? C9 C8 C6 113.9(2) . . ? C10 C9 N1 113.2(2) . . ? C10 C9 C8 114.7(2) . . ? N1 C9 C8 110.8(2) . . ? C11 C10 C14 107.6(2) . . ? C11 C10 C9 122.5(2) . . ? C14 C10 C9 129.5(2) . . ? C11 C10 Fe1 70.85(16) . . ? C14 C10 Fe1 69.31(15) . . ? C9 C10 Fe1 119.52(18) . . ? C10 C11 C12 108.4(2) . . ? C10 C11 Fe1 68.05(15) . . ? C12 C11 Fe1 70.47(16) . . ? C13 C12 C11 108.5(2) . . ? C13 C12 Fe1 69.54(16) . . ? C11 C12 Fe1 68.97(16) . . ? C12 C13 C14 108.2(2) . . ? C12 C13 Fe1 70.21(15) . . ? C14 C13 Fe1 67.96(15) . . ? N2 C14 C13 128.7(2) . . ? N2 C14 C10 123.9(2) . . ? C13 C14 C10 107.4(2) . . ? N2 C14 Fe1 123.88(19) . . ? C13 C14 Fe1 70.82(15) . . ? C10 C14 Fe1 68.57(14) . . ? N2 C17 C18 122.9(3) . . ? C23 C18 C19 118.7(3) . . ? C23 C18 C17 119.3(3) . . ? C19 C18 C17 122.0(3) . . ? C20 C19 C18 120.0(3) . . ? C19 C20 C21 120.7(3) . . ? C22 C21 C20 119.6(3) . . ? C21 C22 C23 120.2(3) . . ? C22 C23 C18 120.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Fe1 C1 C2 123.05(18) . . . . ? C14 Fe1 C1 C2 163.53(17) . . . . ? C5 Fe1 C1 C2 -117.4(2) . . . . ? C11 Fe1 C1 C2 84.24(19) . . . . ? C4 Fe1 C1 C2 -80.20(19) . . . . ? C3 Fe1 C1 C2 -36.86(18) . . . . ? C13 Fe1 C1 C2 -177.9(3) . . . . ? C12 Fe1 C1 C2 66.7(3) . . . . ? C10 Fe1 C1 C5 -119.50(17) . . . . ? C14 Fe1 C1 C5 -79.03(18) . . . . ? C2 Fe1 C1 C5 117.4(2) . . . . ? C11 Fe1 C1 C5 -158.32(16) . . . . ? C4 Fe1 C1 C5 37.25(17) . . . . ? C3 Fe1 C1 C5 80.59(18) . . . . ? C13 Fe1 C1 C5 -60.4(3) . . . . ? C12 Fe1 C1 C5 -175.9(3) . . . . ? C10 Fe1 C1 C6 0.3(2) . . . . ? C14 Fe1 C1 C6 40.7(3) . . . . ? C5 Fe1 C1 C6 119.8(3) . . . . ? C2 Fe1 C1 C6 -122.8(3) . . . . ? C11 Fe1 C1 C6 -38.5(3) . . . . ? C4 Fe1 C1 C6 157.0(3) . . . . ? C3 Fe1 C1 C6 -159.6(3) . . . . ? C13 Fe1 C1 C6 59.4(4) . . . . ? C12 Fe1 C1 C6 -56.1(4) . . . . ? C5 C1 C2 C3 -0.7(3) . . . . ? C6 C1 C2 C3 176.3(3) . . . . ? Fe1 C1 C2 C3 59.0(2) . . . . ? C5 C1 C2 Fe1 -59.77(18) . . . . ? C6 C1 C2 Fe1 117.2(3) . . . . ? C10 Fe1 C2 C3 170.01(17) . . . . ? C14 Fe1 C2 C3 -155.4(2) . . . . ? C5 Fe1 C2 C3 -81.14(19) . . . . ? C1 Fe1 C2 C3 -120.5(3) . . . . ? C11 Fe1 C2 C3 126.95(18) . . . . ? C4 Fe1 C2 C3 -37.20(18) . . . . ? C13 Fe1 C2 C3 56.4(5) . . . . ? C12 Fe1 C2 C3 86.6(2) . . . . ? C10 Fe1 C2 C1 -69.5(2) . . . . ? C14 Fe1 C2 C1 -35.0(3) . . . . ? C5 Fe1 C2 C1 39.32(17) . . . . ? C11 Fe1 C2 C1 -112.58(18) . . . . ? C4 Fe1 C2 C1 83.26(19) . . . . ? C3 Fe1 C2 C1 120.5(3) . . . . ? C13 Fe1 C2 C1 176.9(4) . . . . ? C12 Fe1 C2 C1 -152.92(17) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? Fe1 C2 C3 C4 59.0(2) . . . . ? C1 C2 C3 Fe1 -58.4(2) . . . . ? C10 Fe1 C3 C4 -143.0(3) . . . . ? C14 Fe1 C3 C4 26.1(4) . . . . ? C5 Fe1 C3 C4 -37.79(17) . . . . ? C1 Fe1 C3 C4 -82.71(19) . . . . ? C2 Fe1 C3 C4 -119.9(3) . . . . ? C11 Fe1 C3 C4 168.23(17) . . . . ? C13 Fe1 C3 C4 77.8(2) . . . . ? C12 Fe1 C3 C4 122.65(18) . . . . ? C10 Fe1 C3 C2 -23.1(4) . . . . ? C14 Fe1 C3 C2 146.0(3) . . . . ? C5 Fe1 C3 C2 82.09(19) . . . . ? C1 Fe1 C3 C2 37.17(18) . . . . ? C11 Fe1 C3 C2 -71.9(2) . . . . ? C4 Fe1 C3 C2 119.9(3) . . . . ? C13 Fe1 C3 C2 -162.36(17) . . . . ? C12 Fe1 C3 C2 -117.48(18) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Fe1 C3 C4 C5 58.5(2) . . . . ? C2 C3 C4 Fe1 -58.8(2) . . . . ? C10 Fe1 C4 C3 146.7(2) . . . . ? C14 Fe1 C4 C3 -170.15(17) . . . . ? C5 Fe1 C4 C3 119.3(3) . . . . ? C1 Fe1 C4 C3 81.20(19) . . . . ? C2 Fe1 C4 C3 37.29(18) . . . . ? C11 Fe1 C4 C3 -37.3(5) . . . . ? C13 Fe1 C4 C3 -124.99(18) . . . . ? C12 Fe1 C4 C3 -82.3(2) . . . . ? C10 Fe1 C4 C5 27.4(3) . . . . ? C14 Fe1 C4 C5 70.6(2) . . . . ? C1 Fe1 C4 C5 -38.08(17) . . . . ? C2 Fe1 C4 C5 -81.99(19) . . . . ? C11 Fe1 C4 C5 -156.5(4) . . . . ? C3 Fe1 C4 C5 -119.3(3) . . . . ? C13 Fe1 C4 C5 115.73(18) . . . . ? C12 Fe1 C4 C5 158.37(17) . . . . ? C3 C4 C5 C1 -0.2(3) . . . . ? Fe1 C4 C5 C1 59.00(19) . . . . ? C3 C4 C5 Fe1 -59.2(2) . . . . ? C2 C1 C5 C4 0.6(3) . . . . ? C6 C1 C5 C4 -176.5(3) . . . . ? Fe1 C1 C5 C4 -59.8(2) . . . . ? C2 C1 C5 Fe1 60.36(18) . . . . ? C6 C1 C5 Fe1 -116.7(3) . . . . ? C10 Fe1 C5 C4 -167.32(17) . . . . ? C14 Fe1 C5 C4 -124.84(18) . . . . ? C1 Fe1 C5 C4 119.7(2) . . . . ? C2 Fe1 C5 C4 81.15(19) . . . . ? C11 Fe1 C5 C4 166.2(2) . . . . ? C3 Fe1 C5 C4 37.47(18) . . . . ? C13 Fe1 C5 C4 -85.7(2) . . . . ? C12 Fe1 C5 C4 -65.6(4) . . . . ? C10 Fe1 C5 C1 72.98(18) . . . . ? C14 Fe1 C5 C1 115.47(17) . . . . ? C2 Fe1 C5 C1 -38.55(17) . . . . ? C11 Fe1 C5 C1 46.5(3) . . . . ? C4 Fe1 C5 C1 -119.7(2) . . . . ? C3 Fe1 C5 C1 -82.23(18) . . . . ? C13 Fe1 C5 C1 154.61(16) . . . . ? C12 Fe1 C5 C1 174.7(3) . . . . ? C2 C1 C6 C7 10.9(4) . . . . ? C5 C1 C6 C7 -172.6(2) . . . . ? Fe1 C1 C6 C7 100.5(3) . . . . ? C2 C1 C6 C8 -117.1(3) . . . . ? C5 C1 C6 C8 59.3(4) . . . . ? Fe1 C1 C6 C8 -27.6(3) . . . . ? C1 C6 C8 C9 65.2(3) . . . . ? C7 C6 C8 C9 -62.6(3) . . . . ? C16 N1 C9 C10 -77.5(3) . . . . ? C15 N1 C9 C10 50.1(3) . . . . ? C16 N1 C9 C8 52.9(3) . . . . ? C15 N1 C9 C8 -179.5(2) . . . . ? C6 C8 C9 C10 -72.6(3) . . . . ? C6 C8 C9 N1 157.7(2) . . . . ? N1 C9 C10 C11 -108.6(3) . . . . ? C8 C9 C10 C11 122.9(3) . . . . ? N1 C9 C10 C14 79.8(3) . . . . ? C8 C9 C10 C14 -48.7(4) . . . . ? N1 C9 C10 Fe1 166.36(17) . . . . ? C8 C9 C10 Fe1 37.9(3) . . . . ? C14 Fe1 C10 C11 118.3(2) . . . . ? C5 Fe1 C10 C11 -162.13(16) . . . . ? C1 Fe1 C10 C11 -122.10(17) . . . . ? C2 Fe1 C10 C11 -83.82(18) . . . . ? C4 Fe1 C10 C11 178.4(2) . . . . ? C3 Fe1 C10 C11 -67.1(3) . . . . ? C13 Fe1 C10 C11 80.12(17) . . . . ? C12 Fe1 C10 C11 36.99(16) . . . . ? C5 Fe1 C10 C14 79.59(18) . . . . ? C1 Fe1 C10 C14 119.62(16) . . . . ? C2 Fe1 C10 C14 157.90(16) . . . . ? C11 Fe1 C10 C14 -118.3(2) . . . . ? C4 Fe1 C10 C14 60.1(3) . . . . ? C3 Fe1 C10 C14 174.7(3) . . . . ? C13 Fe1 C10 C14 -38.16(15) . . . . ? C12 Fe1 C10 C14 -81.29(17) . . . . ? C14 Fe1 C10 C9 -124.6(3) . . . . ? C5 Fe1 C10 C9 -45.0(2) . . . . ? C1 Fe1 C10 C9 -4.9(2) . . . . ? C2 Fe1 C10 C9 33.3(2) . . . . ? C11 Fe1 C10 C9 117.2(3) . . . . ? C4 Fe1 C10 C9 -64.5(3) . . . . ? C3 Fe1 C10 C9 50.1(4) . . . . ? C13 Fe1 C10 C9 -162.7(2) . . . . ? C12 Fe1 C10 C9 154.2(2) . . . . ? C14 C10 C11 C12 0.7(3) . . . . ? C9 C10 C11 C12 -172.5(2) . . . . ? Fe1 C10 C11 C12 -59.11(19) . . . . ? C14 C10 C11 Fe1 59.82(18) . . . . ? C9 C10 C11 Fe1 -113.4(2) . . . . ? C14 Fe1 C11 C10 -39.09(16) . . . . ? C5 Fe1 C11 C10 37.6(3) . . . . ? C1 Fe1 C11 C10 70.49(18) . . . . ? C2 Fe1 C11 C10 113.29(17) . . . . ? C4 Fe1 C11 C10 -177.4(4) . . . . ? C3 Fe1 C11 C10 153.42(16) . . . . ? C13 Fe1 C11 C10 -83.38(17) . . . . ? C12 Fe1 C11 C10 -120.2(2) . . . . ? C10 Fe1 C11 C12 120.2(2) . . . . ? C14 Fe1 C11 C12 81.12(17) . . . . ? C5 Fe1 C11 C12 157.8(2) . . . . ? C1 Fe1 C11 C12 -169.31(16) . . . . ? C2 Fe1 C11 C12 -126.50(17) . . . . ? C4 Fe1 C11 C12 -57.2(5) . . . . ? C3 Fe1 C11 C12 -86.4(2) . . . . ? C13 Fe1 C11 C12 36.82(16) . . . . ? C10 C11 C12 C13 -0.8(3) . . . . ? Fe1 C11 C12 C13 -58.5(2) . . . . ? C10 C11 C12 Fe1 57.62(19) . . . . ? C10 Fe1 C12 C13 82.90(18) . . . . ? C14 Fe1 C12 C13 37.62(16) . . . . ? C5 Fe1 C12 C13 -26.5(4) . . . . ? C1 Fe1 C12 C13 144.7(3) . . . . ? C2 Fe1 C12 C13 -167.27(17) . . . . ? C11 Fe1 C12 C13 120.4(2) . . . . ? C4 Fe1 C12 C13 -76.8(2) . . . . ? C3 Fe1 C12 C13 -121.77(18) . . . . ? C10 Fe1 C12 C11 -37.47(16) . . . . ? C14 Fe1 C12 C11 -82.75(17) . . . . ? C5 Fe1 C12 C11 -146.8(3) . . . . ? C1 Fe1 C12 C11 24.3(4) . . . . ? C2 Fe1 C12 C11 72.4(2) . . . . ? C4 Fe1 C12 C11 162.82(16) . . . . ? C3 Fe1 C12 C11 117.86(18) . . . . ? C13 Fe1 C12 C11 -120.4(2) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? Fe1 C12 C13 C14 -57.47(19) . . . . ? C11 C12 C13 Fe1 58.10(19) . . . . ? C10 Fe1 C13 C12 -81.24(18) . . . . ? C14 Fe1 C13 C12 -120.2(2) . . . . ? C5 Fe1 C13 C12 170.44(17) . . . . ? C1 Fe1 C13 C12 -146.0(3) . . . . ? C2 Fe1 C13 C12 38.9(5) . . . . ? C11 Fe1 C13 C12 -37.10(17) . . . . ? C4 Fe1 C13 C12 125.96(18) . . . . ? C3 Fe1 C13 C12 83.0(2) . . . . ? C10 Fe1 C13 C14 38.96(16) . . . . ? C5 Fe1 C13 C14 -69.35(19) . . . . ? C1 Fe1 C13 C14 -25.8(4) . . . . ? C2 Fe1 C13 C14 159.1(4) . . . . ? C11 Fe1 C13 C14 83.10(17) . . . . ? C4 Fe1 C13 C14 -113.84(17) . . . . ? C3 Fe1 C13 C14 -156.83(17) . . . . ? C12 Fe1 C13 C14 120.2(2) . . . . ? C17 N2 C14 C13 -9.4(4) . . . . ? C17 N2 C14 C10 167.8(2) . . . . ? C17 N2 C14 Fe1 82.4(3) . . . . ? C12 C13 C14 N2 177.4(3) . . . . ? Fe1 C13 C14 N2 118.5(3) . . . . ? C12 C13 C14 C10 -0.2(3) . . . . ? Fe1 C13 C14 C10 -59.05(17) . . . . ? C12 C13 C14 Fe1 58.85(19) . . . . ? C11 C10 C14 N2 -178.0(2) . . . . ? C9 C10 C14 N2 -5.5(4) . . . . ? Fe1 C10 C14 N2 -117.2(3) . . . . ? C11 C10 C14 C13 -0.3(3) . . . . ? C9 C10 C14 C13 172.3(3) . . . . ? Fe1 C10 C14 C13 60.48(18) . . . . ? C11 C10 C14 Fe1 -60.80(18) . . . . ? C9 C10 C14 Fe1 111.8(3) . . . . ? C10 Fe1 C14 N2 117.3(3) . . . . ? C5 Fe1 C14 N2 2.2(2) . . . . ? C1 Fe1 C14 N2 44.2(3) . . . . ? C2 Fe1 C14 N2 68.8(4) . . . . ? C11 Fe1 C14 N2 155.4(3) . . . . ? C4 Fe1 C14 N2 -36.8(3) . . . . ? C3 Fe1 C14 N2 -56.4(5) . . . . ? C13 Fe1 C14 N2 -124.3(3) . . . . ? C12 Fe1 C14 N2 -161.1(3) . . . . ? C10 Fe1 C14 C13 -118.5(2) . . . . ? C5 Fe1 C14 C13 126.52(17) . . . . ? C1 Fe1 C14 C13 168.45(16) . . . . ? C2 Fe1 C14 C13 -166.9(2) . . . . ? C11 Fe1 C14 C13 -80.28(17) . . . . ? C4 Fe1 C14 C13 87.47(18) . . . . ? C3 Fe1 C14 C13 67.9(4) . . . . ? C12 Fe1 C14 C13 -36.76(16) . . . . ? C5 Fe1 C14 C10 -115.03(16) . . . . ? C1 Fe1 C14 C10 -73.09(18) . . . . ? C2 Fe1 C14 C10 -48.4(3) . . . . ? C11 Fe1 C14 C10 38.17(15) . . . . ? C4 Fe1 C14 C10 -154.08(16) . . . . ? C3 Fe1 C14 C10 -173.7(3) . . . . ? C13 Fe1 C14 C10 118.5(2) . . . . ? C12 Fe1 C14 C10 81.69(17) . . . . ? C14 N2 C17 C18 -176.8(2) . . . . ? N2 C17 C18 C23 176.5(3) . . . . ? N2 C17 C18 C19 -4.3(4) . . . . ? C23 C18 C19 C20 0.2(5) . . . . ? C17 C18 C19 C20 -178.9(3) . . . . ? C18 C19 C20 C21 -1.9(5) . . . . ? C19 C20 C21 C22 2.3(6) . . . . ? C20 C21 C22 C23 -0.9(5) . . . . ? C21 C22 C23 C18 -0.9(5) . . . . ? C19 C18 C23 C22 1.2(4) . . . . ? C17 C18 C23 C22 -179.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.443 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.075 # Attachment '5.cif' data_erk5254 _database_code_depnum_ccdc_archive 'CCDC 806928' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 Cl Fe N' _chemical_formula_weight 377.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 11.4469(3) _cell_length_b 13.7506(4) _cell_length_c 11.5357(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.176(1) _cell_angle_gamma 90.00 _cell_volume 1734.76(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2895 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7838 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8833 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4017 _reflns_number_gt 3496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0229P)^2^+3.8005P] 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 4017 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Fe Fe 0.24419(4) 0.02195(3) 0.35180(4) 0.03675(13) Uani 1 1 d . . . Cl1 Cl 0.12139(9) 0.33506(6) 0.38069(8) 0.0584(2) Uani 1 1 d . . . C1 C 0.2281(3) 0.0034(2) 0.5197(3) 0.0409(7) Uani 1 1 d . . . C2 C 0.3400(3) -0.0395(2) 0.5125(3) 0.0467(7) Uani 1 1 d . . . H2 H 0.4191 -0.0227 0.5606 0.056 Uiso 1 1 calc R . . C3 C 0.3112(3) -0.1119(2) 0.4203(3) 0.0517(8) Uani 1 1 d . . . H3 H 0.3678 -0.1506 0.3964 0.062 Uiso 1 1 calc R . . C4 C 0.1822(3) -0.1158(2) 0.3707(3) 0.0515(8) Uani 1 1 d . . . H4 H 0.1381 -0.1573 0.3084 0.062 Uiso 1 1 calc R . . C5 C 0.1319(3) -0.0453(2) 0.4326(3) 0.0462(7) Uani 1 1 d . . . H5 H 0.0480 -0.0329 0.4182 0.055 Uiso 1 1 calc R . . C6 C 0.2146(3) 0.0884(2) 0.5980(3) 0.0433(7) Uani 1 1 d . . . H6 H 0.1663 0.0644 0.6506 0.052 Uiso 1 1 calc R . . C7 C 0.3374(3) 0.1211(3) 0.6826(3) 0.0536(8) Uani 1 1 d . . . H7A H 0.3742 0.0682 0.7367 0.080 Uiso 1 1 calc R . . H7B H 0.3252 0.1764 0.7300 0.080 Uiso 1 1 calc R . . H7C H 0.3910 0.1396 0.6351 0.080 Uiso 1 1 calc R . . C8 C 0.1415(3) 0.1735(2) 0.5238(3) 0.0431(7) Uani 1 1 d . . . H8A H 0.0629 0.1487 0.4726 0.052 Uiso 1 1 calc R . . H8B H 0.1243 0.2211 0.5799 0.052 Uiso 1 1 calc R . . C9 C 0.2068(3) 0.2249(2) 0.4434(3) 0.0411(7) Uani 1 1 d . . . H9 H 0.2884 0.2451 0.4955 0.049 Uiso 1 1 calc R . . C10 C 0.2247(3) 0.1664(2) 0.3413(3) 0.0373(6) Uani 1 1 d . . . C11 C 0.3404(3) 0.1397(2) 0.3254(3) 0.0438(7) Uani 1 1 d . . . H11 H 0.4175 0.1606 0.3741 0.053 Uiso 1 1 calc R . . C12 C 0.3191(3) 0.0769(3) 0.2247(3) 0.0475(8) Uani 1 1 d . . . H12 H 0.3796 0.0475 0.1964 0.057 Uiso 1 1 calc R . . C13 C 0.1908(3) 0.0653(2) 0.1730(3) 0.0439(7) Uani 1 1 d . . . H13 H 0.1515 0.0277 0.1045 0.053 Uiso 1 1 calc R . . C14 C 0.1323(3) 0.1215(2) 0.2445(3) 0.0375(6) Uani 1 1 d . . . N1 N 0.0060(2) 0.13105(19) 0.2316(2) 0.0402(6) Uani 1 1 d . . . C15 C -0.0673(3) 0.1271(2) 0.1244(3) 0.0438(7) Uani 1 1 d . . . H15 H -0.0353 0.1201 0.0586 0.053 Uiso 1 1 calc R . . C16 C -0.2003(3) 0.1330(2) 0.1007(3) 0.0475(8) Uani 1 1 d . . . C17 C -0.2741(3) 0.1394(3) -0.0183(4) 0.0660(11) Uani 1 1 d . . . H17 H -0.2385 0.1408 -0.0821 0.079 Uiso 1 1 calc R . . C18 C -0.4002(4) 0.1438(3) -0.0437(5) 0.0821(15) Uani 1 1 d . . . H18 H -0.4498 0.1487 -0.1245 0.099 Uiso 1 1 calc R . . C19 C -0.4522(4) 0.1411(3) 0.0482(6) 0.0828(16) Uani 1 1 d . . . H19 H -0.5379 0.1415 0.0303 0.099 Uiso 1 1 calc R . . C20 C -0.3797(4) 0.1375(3) 0.1680(5) 0.0773(14) Uani 1 1 d . . . H20 H -0.4160 0.1383 0.2312 0.093 Uiso 1 1 calc R . . C21 C -0.2532(3) 0.1329(3) 0.1943(4) 0.0594(10) Uani 1 1 d . . . H21 H -0.2038 0.1298 0.2753 0.071 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 Fe 0.0308(2) 0.0353(2) 0.0438(2) 0.00102(18) 0.01055(17) 0.00057(16) Cl1 0.0773(6) 0.0440(4) 0.0545(5) 0.0032(4) 0.0207(4) 0.0176(4) C1 0.0358(14) 0.0424(16) 0.0431(16) 0.0046(13) 0.0095(12) -0.0012(12) C2 0.0414(16) 0.0437(17) 0.0502(18) 0.0050(14) 0.0063(14) 0.0056(13) C3 0.056(2) 0.0379(17) 0.059(2) 0.0066(15) 0.0136(16) 0.0079(15) C4 0.060(2) 0.0362(16) 0.056(2) 0.0008(15) 0.0136(17) -0.0109(15) C5 0.0443(17) 0.0450(17) 0.0486(17) 0.0044(14) 0.0128(14) -0.0090(14) C6 0.0382(15) 0.0482(17) 0.0420(16) 0.0035(14) 0.0098(13) -0.0006(13) C7 0.0489(19) 0.0508(19) 0.0508(19) -0.0037(16) -0.0013(15) 0.0023(15) C8 0.0406(16) 0.0462(17) 0.0427(16) -0.0047(14) 0.0129(13) 0.0032(13) C9 0.0391(15) 0.0376(15) 0.0433(16) 0.0021(13) 0.0072(13) 0.0028(12) C10 0.0332(14) 0.0350(14) 0.0436(15) 0.0034(12) 0.0111(12) -0.0005(11) C11 0.0315(14) 0.0420(16) 0.0593(19) 0.0056(15) 0.0156(13) -0.0028(12) C12 0.0415(16) 0.0503(19) 0.057(2) 0.0062(16) 0.0251(15) 0.0053(14) C13 0.0444(16) 0.0473(18) 0.0414(16) 0.0005(14) 0.0149(13) 0.0055(14) C14 0.0333(14) 0.0378(15) 0.0416(15) 0.0022(12) 0.0113(12) 0.0047(11) N1 0.0321(12) 0.0418(14) 0.0447(14) -0.0003(11) 0.0083(10) 0.0045(10) C15 0.0363(15) 0.0427(16) 0.0492(17) -0.0025(14) 0.0076(13) 0.0025(13) C16 0.0348(15) 0.0369(16) 0.062(2) -0.0027(15) 0.0013(14) 0.0022(12) C17 0.051(2) 0.067(2) 0.065(2) -0.018(2) -0.0062(18) 0.0121(18) C18 0.048(2) 0.071(3) 0.099(4) -0.020(3) -0.021(2) 0.009(2) C19 0.0341(19) 0.057(2) 0.140(5) 0.016(3) -0.001(2) -0.0018(17) C20 0.045(2) 0.067(3) 0.123(4) 0.032(3) 0.030(2) 0.0083(18) C21 0.0364(17) 0.057(2) 0.081(3) 0.025(2) 0.0126(17) 0.0039(15) _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 Fe C10 1.998(3) . ? Fe C1 2.015(3) . ? Fe C5 2.021(3) . ? Fe C14 2.028(3) . ? Fe C11 2.031(3) . ? Fe C2 2.038(3) . ? Fe C12 2.049(3) . ? Fe C4 2.056(3) . ? Fe C13 2.059(3) . ? Fe C3 2.060(3) . ? Cl1 C9 1.832(3) . ? C1 C5 1.420(4) . ? C1 C2 1.435(4) . ? C1 C6 1.513(5) . ? C2 C3 1.422(5) . ? C2 H2 0.9400 . ? C3 C4 1.418(5) . ? C3 H3 0.9400 . ? C4 C5 1.423(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.523(4) . ? C6 C8 1.543(4) . ? C6 H6 0.9900 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.525(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.490(4) . ? C9 H9 0.9900 . ? C10 C14 1.431(4) . ? C10 C11 1.438(4) . ? C11 C12 1.410(5) . ? C11 H11 0.9400 . ? C12 C13 1.421(4) . ? C12 H12 0.9400 . ? C13 C14 1.433(4) . ? C13 H13 0.9400 . ? C14 N1 1.415(4) . ? N1 C15 1.274(4) . ? C15 C16 1.468(4) . ? C15 H15 0.9400 . ? C16 C21 1.385(5) . ? C16 C17 1.387(5) . ? C17 C18 1.387(6) . ? C17 H17 0.9400 . ? C18 C19 1.362(7) . ? C18 H18 0.9400 . ? C19 C20 1.387(7) . ? C19 H19 0.9400 . ? C20 C21 1.391(5) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? 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 C10 Fe C1 98.28(13) . . ? C10 Fe C5 114.07(13) . . ? C1 Fe C5 41.20(12) . . ? C10 Fe C14 41.64(12) . . ? C1 Fe C14 116.86(12) . . ? C5 Fe C14 102.56(13) . . ? C10 Fe C11 41.80(11) . . ? C1 Fe C11 116.91(13) . . ? C5 Fe C11 151.74(14) . . ? C14 Fe C11 69.09(12) . . ? C10 Fe C2 119.21(13) . . ? C1 Fe C2 41.47(12) . . ? C5 Fe C2 68.62(14) . . ? C14 Fe C2 155.34(13) . . ? C11 Fe C2 107.27(14) . . ? C10 Fe C12 69.70(13) . . ? C1 Fe C12 155.63(14) . . ? C5 Fe C12 163.00(14) . . ? C14 Fe C12 68.67(12) . . ? C11 Fe C12 40.44(14) . . ? C2 Fe C12 125.27(13) . . ? C10 Fe C4 152.37(14) . . ? C1 Fe C4 69.46(14) . . ? C5 Fe C4 40.84(14) . . ? C14 Fe C4 120.75(13) . . ? C11 Fe C4 165.76(14) . . ? C2 Fe C4 68.36(14) . . ? C12 Fe C4 130.22(15) . . ? C10 Fe C13 69.92(13) . . ? C1 Fe C13 156.23(12) . . ? C5 Fe C13 123.61(13) . . ? C14 Fe C13 41.03(12) . . ? C11 Fe C13 68.46(14) . . ? C2 Fe C13 162.20(13) . . ? C12 Fe C13 40.48(13) . . ? C4 Fe C13 111.30(14) . . ? C10 Fe C3 159.02(13) . . ? C1 Fe C3 69.35(14) . . ? C5 Fe C3 68.25(15) . . ? C14 Fe C3 159.09(13) . . ? C11 Fe C3 127.80(14) . . ? C2 Fe C3 40.61(14) . . ? C12 Fe C3 114.66(14) . . ? C4 Fe C3 40.29(14) . . ? C13 Fe C3 127.58(14) . . ? C5 C1 C2 106.5(3) . . ? C5 C1 C6 126.3(3) . . ? C2 C1 C6 127.0(3) . . ? C5 C1 Fe 69.64(18) . . ? C2 C1 Fe 70.13(19) . . ? C6 C1 Fe 122.1(2) . . ? C3 C2 C1 108.5(3) . . ? C3 C2 Fe 70.53(19) . . ? C1 C2 Fe 68.40(18) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe C2 H2 126.9 . . ? C4 C3 C2 108.2(3) . . ? C4 C3 Fe 69.71(19) . . ? C2 C3 Fe 68.86(18) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 127.1 . . ? C3 C4 C5 107.4(3) . . ? C3 C4 Fe 70.00(19) . . ? C5 C4 Fe 68.25(18) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Fe C4 H4 127.0 . . ? C1 C5 C4 109.4(3) . . ? C1 C5 Fe 69.16(18) . . ? C4 C5 Fe 70.91(19) . . ? C1 C5 H5 125.3 . . ? C4 C5 H5 125.3 . . ? Fe C5 H5 126.2 . . ? C1 C6 C7 111.9(3) . . ? C1 C6 C8 112.9(3) . . ? C7 C6 C8 112.2(3) . . ? C1 C6 H6 106.4 . . ? C7 C6 H6 106.4 . . ? C8 C6 H6 106.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 113.9(3) . . ? C9 C8 H8A 108.8 . . ? C6 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C6 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 115.9(3) . . ? C10 C9 Cl1 108.4(2) . . ? C8 C9 Cl1 108.9(2) . . ? C10 C9 H9 107.8 . . ? C8 C9 H9 107.8 . . ? Cl1 C9 H9 107.8 . . ? C14 C10 C11 106.7(3) . . ? C14 C10 C9 127.4(3) . . ? C11 C10 C9 125.9(3) . . ? C14 C10 Fe 70.27(17) . . ? C11 C10 Fe 70.31(17) . . ? C9 C10 Fe 121.8(2) . . ? C12 C11 C10 108.6(3) . . ? C12 C11 Fe 70.47(18) . . ? C10 C11 Fe 67.89(16) . . ? C12 C11 H11 125.7 . . ? C10 C11 H11 125.7 . . ? Fe C11 H11 127.5 . . ? C11 C12 C13 108.7(3) . . ? C11 C12 Fe 69.09(18) . . ? C13 C12 Fe 70.14(18) . . ? C11 C12 H12 125.6 . . ? C13 C12 H12 125.6 . . ? Fe C12 H12 126.7 . . ? C12 C13 C14 107.4(3) . . ? C12 C13 Fe 69.38(18) . . ? C14 C13 Fe 68.30(17) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? Fe C13 H13 127.6 . . ? N1 C14 C10 122.6(3) . . ? N1 C14 C13 128.8(3) . . ? C10 C14 C13 108.6(3) . . ? N1 C14 Fe 124.6(2) . . ? C10 C14 Fe 68.09(16) . . ? C13 C14 Fe 70.67(17) . . ? C15 N1 C14 117.2(3) . . ? N1 C15 C16 121.8(3) . . ? N1 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C21 C16 C17 119.5(3) . . ? C21 C16 C15 121.6(3) . . ? C17 C16 C15 118.9(4) . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.1(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 119.8(5) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 119.8(4) . . ? C16 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? 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 C10 Fe C1 C5 117.4(2) . . . . ? C14 Fe C1 C5 78.0(2) . . . . ? C11 Fe C1 C5 156.92(19) . . . . ? C2 Fe C1 C5 -117.2(3) . . . . ? C12 Fe C1 C5 175.4(3) . . . . ? C4 Fe C1 C5 -37.0(2) . . . . ? C13 Fe C1 C5 59.4(4) . . . . ? C3 Fe C1 C5 -80.2(2) . . . . ? C10 Fe C1 C2 -125.46(19) . . . . ? C5 Fe C1 C2 117.2(3) . . . . ? C14 Fe C1 C2 -164.85(19) . . . . ? C11 Fe C1 C2 -85.9(2) . . . . ? C12 Fe C1 C2 -67.4(4) . . . . ? C4 Fe C1 C2 80.2(2) . . . . ? C13 Fe C1 C2 176.6(3) . . . . ? C3 Fe C1 C2 37.0(2) . . . . ? C10 Fe C1 C6 -3.5(3) . . . . ? C5 Fe C1 C6 -120.8(3) . . . . ? C14 Fe C1 C6 -42.9(3) . . . . ? C11 Fe C1 C6 36.1(3) . . . . ? C2 Fe C1 C6 122.0(3) . . . . ? C12 Fe C1 C6 54.6(4) . . . . ? C4 Fe C1 C6 -157.8(3) . . . . ? C13 Fe C1 C6 -61.4(4) . . . . ? C3 Fe C1 C6 159.0(3) . . . . ? C5 C1 C2 C3 1.1(4) . . . . ? C6 C1 C2 C3 -175.1(3) . . . . ? Fe C1 C2 C3 -59.3(2) . . . . ? C5 C1 C2 Fe 60.4(2) . . . . ? C6 C1 C2 Fe -115.7(3) . . . . ? C10 Fe C2 C3 -172.5(2) . . . . ? C1 Fe C2 C3 120.1(3) . . . . ? C5 Fe C2 C3 81.1(2) . . . . ? C14 Fe C2 C3 154.1(3) . . . . ? C11 Fe C2 C3 -128.6(2) . . . . ? C12 Fe C2 C3 -87.7(2) . . . . ? C4 Fe C2 C3 37.0(2) . . . . ? C13 Fe C2 C3 -55.4(5) . . . . ? C10 Fe C2 C1 67.4(2) . . . . ? C5 Fe C2 C1 -38.99(19) . . . . ? C14 Fe C2 C1 34.0(4) . . . . ? C11 Fe C2 C1 111.3(2) . . . . ? C12 Fe C2 C1 152.20(19) . . . . ? C4 Fe C2 C1 -83.0(2) . . . . ? C13 Fe C2 C1 -175.5(4) . . . . ? C3 Fe C2 C1 -120.1(3) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? Fe C2 C3 C4 -58.8(2) . . . . ? C1 C2 C3 Fe 58.0(2) . . . . ? C10 Fe C3 C4 138.6(4) . . . . ? C1 Fe C3 C4 82.2(2) . . . . ? C5 Fe C3 C4 37.9(2) . . . . ? C14 Fe C3 C4 -29.3(5) . . . . ? C11 Fe C3 C4 -169.1(2) . . . . ? C2 Fe C3 C4 120.0(3) . . . . ? C12 Fe C3 C4 -123.9(2) . . . . ? C13 Fe C3 C4 -78.5(3) . . . . ? C10 Fe C3 C2 18.6(5) . . . . ? C1 Fe C3 C2 -37.8(2) . . . . ? C5 Fe C3 C2 -82.1(2) . . . . ? C14 Fe C3 C2 -149.3(3) . . . . ? C11 Fe C3 C2 70.9(3) . . . . ? C12 Fe C3 C2 116.1(2) . . . . ? C4 Fe C3 C2 -120.0(3) . . . . ? C13 Fe C3 C2 161.5(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? Fe C3 C4 C5 -58.2(2) . . . . ? C2 C3 C4 Fe 58.3(2) . . . . ? C10 Fe C4 C3 -149.3(3) . . . . ? C1 Fe C4 C3 -81.9(2) . . . . ? C5 Fe C4 C3 -119.2(3) . . . . ? C14 Fe C4 C3 168.3(2) . . . . ? C11 Fe C4 C3 37.3(7) . . . . ? C2 Fe C4 C3 -37.3(2) . . . . ? C12 Fe C4 C3 81.2(3) . . . . ? C13 Fe C4 C3 123.5(2) . . . . ? C10 Fe C4 C5 -30.1(4) . . . . ? C1 Fe C4 C5 37.32(19) . . . . ? C14 Fe C4 C5 -72.5(2) . . . . ? C11 Fe C4 C5 156.5(5) . . . . ? C2 Fe C4 C5 81.9(2) . . . . ? C12 Fe C4 C5 -159.5(2) . . . . ? C13 Fe C4 C5 -117.2(2) . . . . ? C3 Fe C4 C5 119.2(3) . . . . ? C2 C1 C5 C4 -1.1(4) . . . . ? C6 C1 C5 C4 175.1(3) . . . . ? Fe C1 C5 C4 59.7(2) . . . . ? C2 C1 C5 Fe -60.8(2) . . . . ? C6 C1 C5 Fe 115.5(3) . . . . ? C3 C4 C5 C1 0.6(4) . . . . ? Fe C4 C5 C1 -58.6(2) . . . . ? C3 C4 C5 Fe 59.2(2) . . . . ? C10 Fe C5 C1 -74.3(2) . . . . ? C14 Fe C5 C1 -116.63(19) . . . . ? C11 Fe C5 C1 -47.6(4) . . . . ? C2 Fe C5 C1 39.24(19) . . . . ? C12 Fe C5 C1 -173.6(4) . . . . ? C4 Fe C5 C1 120.5(3) . . . . ? C13 Fe C5 C1 -155.38(18) . . . . ? C3 Fe C5 C1 83.1(2) . . . . ? C10 Fe C5 C4 165.3(2) . . . . ? C1 Fe C5 C4 -120.5(3) . . . . ? C14 Fe C5 C4 122.9(2) . . . . ? C11 Fe C5 C4 -168.1(3) . . . . ? C2 Fe C5 C4 -81.2(2) . . . . ? C12 Fe C5 C4 66.0(5) . . . . ? C13 Fe C5 C4 84.2(2) . . . . ? C3 Fe C5 C4 -37.4(2) . . . . ? C5 C1 C6 C7 179.1(3) . . . . ? C2 C1 C6 C7 -5.4(5) . . . . ? Fe C1 C6 C7 -93.7(3) . . . . ? C5 C1 C6 C8 -53.1(4) . . . . ? C2 C1 C6 C8 122.3(3) . . . . ? Fe C1 C6 C8 34.0(3) . . . . ? C1 C6 C8 C9 -67.8(3) . . . . ? C7 C6 C8 C9 59.8(4) . . . . ? C6 C8 C9 C10 66.6(4) . . . . ? C6 C8 C9 Cl1 -170.9(2) . . . . ? C8 C9 C10 C14 58.6(4) . . . . ? Cl1 C9 C10 C14 -64.2(4) . . . . ? C8 C9 C10 C11 -117.6(3) . . . . ? Cl1 C9 C10 C11 119.6(3) . . . . ? C8 C9 C10 Fe -30.0(3) . . . . ? Cl1 C9 C10 Fe -152.69(16) . . . . ? C1 Fe C10 C14 -121.57(17) . . . . ? C5 Fe C10 C14 -81.73(19) . . . . ? C11 Fe C10 C14 116.9(3) . . . . ? C2 Fe C10 C14 -159.75(18) . . . . ? C12 Fe C10 C14 80.36(19) . . . . ? C4 Fe C10 C14 -60.7(3) . . . . ? C13 Fe C10 C14 37.10(17) . . . . ? C3 Fe C10 C14 -173.5(3) . . . . ? C1 Fe C10 C11 121.56(19) . . . . ? C5 Fe C10 C11 161.40(19) . . . . ? C14 Fe C10 C11 -116.9(3) . . . . ? C2 Fe C10 C11 83.4(2) . . . . ? C12 Fe C10 C11 -36.51(19) . . . . ? C4 Fe C10 C11 -177.6(3) . . . . ? C13 Fe C10 C11 -79.8(2) . . . . ? C3 Fe C10 C11 69.6(4) . . . . ? C1 Fe C10 C9 0.9(3) . . . . ? C5 Fe C10 C9 40.7(3) . . . . ? C14 Fe C10 C9 122.4(3) . . . . ? C11 Fe C10 C9 -120.7(3) . . . . ? C2 Fe C10 C9 -37.3(3) . . . . ? C12 Fe C10 C9 -157.2(3) . . . . ? C4 Fe C10 C9 61.7(4) . . . . ? C13 Fe C10 C9 159.5(3) . . . . ? C3 Fe C10 C9 -51.1(5) . . . . ? C14 C10 C11 C12 -2.4(3) . . . . ? C9 C10 C11 C12 174.5(3) . . . . ? Fe C10 C11 C12 58.8(2) . . . . ? C14 C10 C11 Fe -61.2(2) . . . . ? C9 C10 C11 Fe 115.6(3) . . . . ? C10 Fe C11 C12 -120.6(3) . . . . ? C1 Fe C11 C12 168.34(18) . . . . ? C5 Fe C11 C12 -158.6(3) . . . . ? C14 Fe C11 C12 -81.3(2) . . . . ? C2 Fe C11 C12 124.6(2) . . . . ? C4 Fe C11 C12 54.8(6) . . . . ? C13 Fe C11 C12 -37.10(18) . . . . ? C3 Fe C11 C12 84.5(2) . . . . ? C1 Fe C11 C10 -71.0(2) . . . . ? C5 Fe C11 C10 -38.0(4) . . . . ? C14 Fe C11 C10 39.39(17) . . . . ? C2 Fe C11 C10 -114.78(19) . . . . ? C12 Fe C11 C10 120.6(3) . . . . ? C4 Fe C11 C10 175.4(5) . . . . ? C13 Fe C11 C10 83.55(19) . . . . ? C3 Fe C11 C10 -154.87(19) . . . . ? C10 C11 C12 C13 1.9(4) . . . . ? Fe C11 C12 C13 59.1(2) . . . . ? C10 C11 C12 Fe -57.3(2) . . . . ? C10 Fe C12 C11 37.69(18) . . . . ? C1 Fe C12 C11 -25.9(4) . . . . ? C5 Fe C12 C11 143.8(4) . . . . ? C14 Fe C12 C11 82.4(2) . . . . ? C2 Fe C12 C11 -74.4(2) . . . . ? C4 Fe C12 C11 -164.75(19) . . . . ? C13 Fe C12 C11 120.2(3) . . . . ? C3 Fe C12 C11 -120.1(2) . . . . ? C10 Fe C12 C13 -82.5(2) . . . . ? C1 Fe C12 C13 -146.1(3) . . . . ? C5 Fe C12 C13 23.6(6) . . . . ? C14 Fe C12 C13 -37.82(19) . . . . ? C11 Fe C12 C13 -120.2(3) . . . . ? C2 Fe C12 C13 165.43(19) . . . . ? C4 Fe C12 C13 75.1(2) . . . . ? C3 Fe C12 C13 119.7(2) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? Fe C12 C13 C14 57.9(2) . . . . ? C11 C12 C13 Fe -58.5(2) . . . . ? C10 Fe C13 C12 81.9(2) . . . . ? C1 Fe C13 C12 145.2(3) . . . . ? C5 Fe C13 C12 -171.9(2) . . . . ? C14 Fe C13 C12 119.5(3) . . . . ? C11 Fe C13 C12 37.06(19) . . . . ? C2 Fe C13 C12 -42.2(5) . . . . ? C4 Fe C13 C12 -127.6(2) . . . . ? C3 Fe C13 C12 -84.8(2) . . . . ? C10 Fe C13 C14 -37.63(17) . . . . ? C1 Fe C13 C14 25.6(4) . . . . ? C5 Fe C13 C14 68.5(2) . . . . ? C11 Fe C13 C14 -82.47(19) . . . . ? C2 Fe C13 C14 -161.8(4) . . . . ? C12 Fe C13 C14 -119.5(3) . . . . ? C4 Fe C13 C14 112.8(2) . . . . ? C3 Fe C13 C14 155.68(19) . . . . ? C11 C10 C14 N1 179.3(3) . . . . ? C9 C10 C14 N1 2.5(5) . . . . ? Fe C10 C14 N1 118.0(3) . . . . ? C11 C10 C14 C13 2.0(3) . . . . ? C9 C10 C14 C13 -174.8(3) . . . . ? Fe C10 C14 C13 -59.2(2) . . . . ? C11 C10 C14 Fe 61.3(2) . . . . ? C9 C10 C14 Fe -115.5(3) . . . . ? C12 C13 C14 N1 -177.9(3) . . . . ? Fe C13 C14 N1 -119.4(3) . . . . ? C12 C13 C14 C10 -0.9(4) . . . . ? Fe C13 C14 C10 57.6(2) . . . . ? C12 C13 C14 Fe -58.6(2) . . . . ? C10 Fe C14 N1 -115.3(3) . . . . ? C1 Fe C14 N1 -44.4(3) . . . . ? C5 Fe C14 N1 -3.1(3) . . . . ? C11 Fe C14 N1 -154.9(3) . . . . ? C2 Fe C14 N1 -68.9(4) . . . . ? C12 Fe C14 N1 161.7(3) . . . . ? C4 Fe C14 N1 36.6(3) . . . . ? C13 Fe C14 N1 124.3(3) . . . . ? C3 Fe C14 N1 58.2(5) . . . . ? C1 Fe C14 C10 70.9(2) . . . . ? C5 Fe C14 C10 112.22(18) . . . . ? C11 Fe C14 C10 -39.53(17) . . . . ? C2 Fe C14 C10 46.4(4) . . . . ? C12 Fe C14 C10 -83.02(19) . . . . ? C4 Fe C14 C10 151.93(19) . . . . ? C13 Fe C14 C10 -120.3(3) . . . . ? C3 Fe C14 C10 173.5(4) . . . . ? C10 Fe C14 C13 120.3(3) . . . . ? C1 Fe C14 C13 -168.73(18) . . . . ? C5 Fe C14 C13 -127.4(2) . . . . ? C11 Fe C14 C13 80.8(2) . . . . ? C2 Fe C14 C13 166.8(3) . . . . ? C12 Fe C14 C13 37.32(19) . . . . ? C4 Fe C14 C13 -87.7(2) . . . . ? C3 Fe C14 C13 -66.1(4) . . . . ? C10 C14 N1 C15 150.6(3) . . . . ? C13 C14 N1 C15 -32.8(5) . . . . ? Fe C14 N1 C15 -125.0(3) . . . . ? C14 N1 C15 C16 178.0(3) . . . . ? N1 C15 C16 C21 -6.9(5) . . . . ? N1 C15 C16 C17 172.7(3) . . . . ? C21 C16 C17 C18 -1.3(6) . . . . ? C15 C16 C17 C18 179.1(4) . . . . ? C16 C17 C18 C19 -0.5(7) . . . . ? C17 C18 C19 C20 2.4(7) . . . . ? C18 C19 C20 C21 -2.5(7) . . . . ? C17 C16 C21 C20 1.1(6) . . . . ? C15 C16 C21 C20 -179.3(3) . . . . ? C19 C20 C21 C16 0.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.350 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.066 # Attachment '8.cif' data_erk4462 _database_code_depnum_ccdc_archive 'CCDC 806929' #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.50 H30 Cl3 Fe N Zr' _chemical_formula_weight 675.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.8528(2) _cell_length_b 12.6309(1) _cell_length_c 19.1447(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.986(1) _cell_angle_gamma 90.00 _cell_volume 5786.38(11) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6148 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6868 _exptl_absorpt_correction_T_max 0.8452 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20203 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7093 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _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 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (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^)+(0.0504P)^2^+10.9239P] 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 7093 _refine_ls_number_parameters 348 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.089 _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 0.014225(14) 0.78603(3) -0.05539(2) 0.02752(10) Uani 1 1 d . . . N1 N 0.10386(9) 0.61770(16) 0.00402(12) 0.0284(4) Uani 1 1 d . . . C1 C 0.02461(11) 0.8335(2) -0.14887(14) 0.0326(5) Uani 1 1 d . . . C2 C -0.01892(12) 0.8942(2) -0.14393(16) 0.0378(6) Uani 1 1 d . . . H2 H -0.0193 0.9681 -0.1385 0.045 Uiso 1 1 calc R . . C3 C -0.06167(12) 0.8227(3) -0.14876(17) 0.0427(7) Uani 1 1 d . . . H3 H -0.0949 0.8414 -0.1467 0.051 Uiso 1 1 calc R . . C4 C -0.04522(12) 0.7185(3) -0.15718(16) 0.0413(7) Uani 1 1 d . . . H4 H -0.0655 0.6560 -0.1615 0.050 Uiso 1 1 calc R . . C5 C 0.00733(12) 0.7256(2) -0.15785(15) 0.0356(6) Uani 1 1 d . . . H5 H 0.0275 0.6682 -0.1634 0.043 Uiso 1 1 calc R . . C6 C 0.07989(11) 0.8742(2) -0.14142(15) 0.0332(5) Uani 1 1 d . . . H6 H 0.0815 0.8531 -0.1901 0.040 Uiso 1 1 calc R . . C7 C 0.08247(14) 0.9956(2) -0.13866(19) 0.0464(7) Uani 1 1 d . . . H7A H 0.0548 1.0240 -0.1882 0.070 Uiso 1 1 calc R . . H7B H 0.1194 1.0187 -0.1293 0.070 Uiso 1 1 calc R . . H7C H 0.0748 1.0208 -0.0967 0.070 Uiso 1 1 calc R . . C8 C 0.13120(11) 0.8241(2) -0.07347(14) 0.0301(5) Uani 1 1 d . . . H8A H 0.1648 0.8463 -0.0776 0.036 Uiso 1 1 calc R . . H8B H 0.1284 0.7470 -0.0794 0.036 Uiso 1 1 calc R . . C9 C 0.13869(10) 0.85293(19) 0.00953(14) 0.0263(5) Uani 1 1 d . . . H9 H 0.1360 0.9310 0.0109 0.032 Uiso 1 1 calc R . . C10 C 0.09338(10) 0.80893(19) 0.02688(13) 0.0255(5) Uani 1 1 d . . . C11 C 0.05608(11) 0.8704(2) 0.04519(14) 0.0309(5) Uani 1 1 d . . . H11 H 0.0569 0.9444 0.0506 0.037 Uiso 1 1 calc R . . C12 C 0.01745(11) 0.8006(2) 0.05384(15) 0.0342(6) Uani 1 1 d . . . H12 H -0.0116 0.8208 0.0657 0.041 Uiso 1 1 calc R . . C13 C 0.03036(11) 0.6950(2) 0.04150(15) 0.0321(5) Uani 1 1 d . . . H13 H 0.0114 0.6335 0.0435 0.038 Uiso 1 1 calc R . . C14 C 0.07761(10) 0.69930(19) 0.02536(14) 0.0270(5) Uani 1 1 d . . . C15 C 0.09591(10) 0.5215(2) 0.01546(15) 0.0294(5) Uani 1 1 d . . . H15 H 0.0739 0.5053 0.0407 0.035 Uiso 1 1 calc R . . C16 C 0.12051(10) 0.4349(2) -0.00997(15) 0.0301(5) Uani 1 1 d . . . C17 C 0.11234(11) 0.3301(2) 0.00526(15) 0.0320(5) Uani 1 1 d . . . H17 H 0.0918 0.3150 0.0329 0.038 Uiso 1 1 calc R . . C18 C 0.13433(12) 0.2481(2) -0.02010(17) 0.0391(6) Uani 1 1 d . . . H18 H 0.1285 0.1776 -0.0100 0.047 Uiso 1 1 calc R . . C19 C 0.16474(15) 0.2695(3) -0.0601(2) 0.0527(8) Uani 1 1 d . . . H19 H 0.1796 0.2136 -0.0771 0.063 Uiso 1 1 calc R . . C20 C 0.17340(19) 0.3729(3) -0.0751(3) 0.0672(12) Uani 1 1 d . . . H20 H 0.1944 0.3874 -0.1022 0.081 Uiso 1 1 calc R . . C21 C 0.15131(16) 0.4551(2) -0.0505(2) 0.0521(8) Uani 1 1 d . . . H21 H 0.1571 0.5254 -0.0613 0.063 Uiso 1 1 calc R . . Zr1 Zr 0.234601(9) 0.901110(18) 0.209746(13) 0.02424(8) Uani 1 1 d . . . Cl1 Cl 0.18649(3) 1.06161(5) 0.14006(4) 0.03627(15) Uani 1 1 d . . . Cl2 Cl 0.32490(3) 0.98599(6) 0.28832(4) 0.04292(17) Uani 1 1 d . . . C30 C 0.19650(10) 0.82357(19) 0.07206(14) 0.0269(5) Uani 1 1 d . . . C31 C 0.24634(11) 0.8791(2) 0.08625(16) 0.0316(5) Uani 1 1 d . . . H31 H 0.2484 0.9398 0.0593 0.038 Uiso 1 1 calc R . . C32 C 0.29203(11) 0.8282(2) 0.14739(17) 0.0362(6) Uani 1 1 d . . . H32 H 0.3298 0.8478 0.1671 0.043 Uiso 1 1 calc R . . C33 C 0.27131(11) 0.7430(2) 0.17381(17) 0.0355(6) Uani 1 1 d . . . H33 H 0.2925 0.6969 0.2153 0.043 Uiso 1 1 calc R . . C34 C 0.21236(11) 0.7395(2) 0.12621(15) 0.0310(5) Uani 1 1 d . . . H34 H 0.1880 0.6892 0.1303 0.037 Uiso 1 1 calc R . . C35 C 0.24510(13) 0.8420(3) 0.34041(17) 0.0469(7) Uani 1 1 d . . . H35 H 0.2812 0.8274 0.3801 0.056 Uiso 1 1 calc R . . C36 C 0.20948(14) 0.7703(2) 0.28592(18) 0.0423(7) Uani 1 1 d . . . H36 H 0.2171 0.6985 0.2821 0.051 Uiso 1 1 calc R . . C37 C 0.16001(13) 0.8239(3) 0.23755(19) 0.0545(9) Uani 1 1 d . . . H37 H 0.1287 0.7947 0.1951 0.065 Uiso 1 1 calc R . . C38 C 0.16549(18) 0.9271(3) 0.2634(2) 0.0644(12) Uani 1 1 d . . . H38 H 0.1381 0.9801 0.2420 0.077 Uiso 1 1 calc R . . C39 C 0.2179(2) 0.9398(3) 0.3260(2) 0.0616(11) Uani 1 1 d . . . H39 H 0.2325 1.0029 0.3538 0.074 Uiso 1 1 calc R . . Cl11 Cl 0.0162(4) 0.2654(6) -0.2519(7) 0.255(4) Uani 0.50 1 d PDU A -1 Cl12 Cl -0.0321(3) 0.4462(4) -0.2243(3) 0.193(2) Uani 0.50 1 d PDU A -1 C101 C 0.0253(10) 0.3946(14) -0.227(3) 0.36(2) Uiso 0.50 1 d PD A -1 H10A H 0.0328 0.4337 -0.2657 0.428 Uiso 0.50 1 calc PR A -1 H10B H 0.0577 0.4027 -0.1759 0.428 Uiso 0.50 1 calc PR A -1 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 0.02478(18) 0.0335(2) 0.02464(18) -0.00274(13) 0.01153(14) -0.00003(14) N1 0.0275(10) 0.0275(11) 0.0308(11) -0.0016(8) 0.0139(9) -0.0019(8) C1 0.0344(13) 0.0420(15) 0.0203(11) -0.0007(10) 0.0114(10) 0.0010(11) C2 0.0385(15) 0.0409(15) 0.0317(13) 0.0035(11) 0.0139(12) 0.0079(12) C3 0.0280(13) 0.0622(19) 0.0322(14) 0.0064(13) 0.0086(11) 0.0082(13) C4 0.0348(14) 0.0528(18) 0.0302(14) -0.0078(12) 0.0094(12) -0.0103(12) C5 0.0378(14) 0.0414(15) 0.0259(12) -0.0084(11) 0.0129(11) -0.0030(11) C6 0.0401(14) 0.0389(14) 0.0253(12) -0.0019(10) 0.0190(11) -0.0024(11) C7 0.0539(18) 0.0420(17) 0.0431(16) 0.0082(13) 0.0219(15) -0.0041(14) C8 0.0333(13) 0.0343(13) 0.0288(12) -0.0036(10) 0.0195(11) -0.0029(10) C9 0.0293(12) 0.0260(12) 0.0269(12) -0.0024(9) 0.0155(10) -0.0019(9) C10 0.0247(11) 0.0305(12) 0.0221(11) -0.0027(9) 0.0113(9) 0.0001(9) C11 0.0308(12) 0.0370(14) 0.0259(12) -0.0066(10) 0.0138(10) -0.0002(10) C12 0.0304(13) 0.0468(16) 0.0316(13) -0.0035(11) 0.0195(11) 0.0016(11) C13 0.0295(12) 0.0405(14) 0.0308(13) -0.0001(11) 0.0177(11) -0.0044(10) C14 0.0257(11) 0.0306(12) 0.0258(11) -0.0004(9) 0.0127(9) -0.0006(9) C15 0.0260(11) 0.0321(13) 0.0300(12) 0.0002(10) 0.0127(10) -0.0030(9) C16 0.0294(12) 0.0290(12) 0.0323(13) -0.0013(10) 0.0143(10) -0.0045(10) C17 0.0296(12) 0.0307(13) 0.0326(13) 0.0015(10) 0.0114(11) -0.0040(10) C18 0.0414(15) 0.0263(13) 0.0426(15) -0.0012(11) 0.0128(13) -0.0031(11) C19 0.064(2) 0.0390(17) 0.069(2) -0.0119(15) 0.0427(19) -0.0008(15) C20 0.095(3) 0.0452(19) 0.103(3) -0.0137(19) 0.081(3) -0.0106(19) C21 0.071(2) 0.0340(16) 0.076(2) -0.0043(15) 0.055(2) -0.0086(14) Zr1 0.02437(12) 0.02321(13) 0.02577(12) 0.00033(8) 0.01193(9) 0.00129(8) Cl1 0.0434(4) 0.0265(3) 0.0350(3) 0.0032(2) 0.0143(3) 0.0076(3) Cl2 0.0323(3) 0.0463(4) 0.0415(4) -0.0093(3) 0.0092(3) -0.0075(3) C30 0.0278(12) 0.0280(12) 0.0292(12) -0.0038(9) 0.0166(10) -0.0027(9) C31 0.0297(12) 0.0371(14) 0.0343(13) -0.0048(10) 0.0201(11) -0.0046(10) C32 0.0248(12) 0.0445(15) 0.0424(15) -0.0101(12) 0.0178(11) -0.0025(11) C33 0.0317(13) 0.0323(13) 0.0393(14) -0.0037(11) 0.0133(11) 0.0088(11) C34 0.0320(13) 0.0248(12) 0.0351(13) -0.0033(10) 0.0142(11) -0.0001(10) C35 0.0401(16) 0.067(2) 0.0315(14) 0.0133(14) 0.0140(13) -0.0015(14) C36 0.0577(18) 0.0347(15) 0.0459(16) 0.0077(12) 0.0335(15) 0.0010(13) C37 0.0334(15) 0.097(3) 0.0369(16) 0.0111(17) 0.0191(13) -0.0084(16) C38 0.071(2) 0.079(3) 0.072(3) 0.040(2) 0.057(2) 0.044(2) C39 0.109(3) 0.0449(19) 0.061(2) -0.0104(16) 0.065(3) -0.011(2) Cl11 0.263(6) 0.255(5) 0.249(5) -0.038(4) 0.116(4) 0.074(4) Cl12 0.227(4) 0.169(4) 0.166(4) -0.035(3) 0.076(3) 0.035(3) _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 C10 2.011(2) . ? Fe1 C1 2.023(3) . ? Fe1 C14 2.025(2) . ? Fe1 C5 2.033(3) . ? Fe1 C11 2.035(2) . ? Fe1 C2 2.041(3) . ? Fe1 C13 2.054(3) . ? Fe1 C12 2.062(3) . ? Fe1 C4 2.062(3) . ? Fe1 C3 2.063(3) . ? N1 C15 1.270(3) . ? N1 C14 1.410(3) . ? C1 C5 1.425(4) . ? C1 C2 1.436(4) . ? C1 C6 1.515(4) . ? C2 C3 1.431(4) . ? C3 C4 1.421(4) . ? C4 C5 1.420(4) . ? C6 C7 1.535(4) . ? C6 C8 1.538(4) . ? C8 C9 1.552(3) . ? C9 C10 1.505(3) . ? C9 C30 1.515(3) . ? C10 C11 1.431(3) . ? C10 C14 1.444(3) . ? C11 C12 1.427(4) . ? C12 C13 1.424(4) . ? C13 C14 1.437(3) . ? C15 C16 1.470(4) . ? C16 C21 1.391(4) . ? C16 C17 1.395(4) . ? C17 C18 1.384(4) . ? C18 C19 1.375(4) . ? C19 C20 1.380(5) . ? C20 C21 1.380(5) . ? Zr1 Cl2 2.4457(7) . ? Zr1 Cl1 2.4484(6) . ? Zr1 C33 2.459(3) . ? Zr1 C36 2.491(3) . ? Zr1 C37 2.493(3) . ? Zr1 C34 2.493(2) . ? Zr1 C35 2.501(3) . ? Zr1 C39 2.510(3) . ? Zr1 C32 2.514(3) . ? Zr1 C38 2.518(3) . ? Zr1 C31 2.538(3) . ? Zr1 C30 2.551(2) . ? C30 C34 1.408(4) . ? C30 C31 1.424(3) . ? C31 C32 1.409(4) . ? C32 C33 1.407(4) . ? C33 C34 1.425(4) . ? C35 C36 1.384(5) . ? C35 C39 1.399(5) . ? C36 C37 1.401(5) . ? C37 C38 1.379(6) . ? C38 C39 1.382(6) . ? Cl11 C101 1.685(10) . ? Cl12 C101 1.697(11) . ? 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 C10 Fe1 C1 97.42(10) . . ? C10 Fe1 C14 41.94(10) . . ? C1 Fe1 C14 115.49(10) . . ? C10 Fe1 C5 114.25(10) . . ? C1 Fe1 C5 41.12(11) . . ? C14 Fe1 C5 102.16(11) . . ? C10 Fe1 C11 41.41(9) . . ? C1 Fe1 C11 116.31(11) . . ? C14 Fe1 C11 69.44(10) . . ? C5 Fe1 C11 151.48(11) . . ? C10 Fe1 C2 117.51(11) . . ? C1 Fe1 C2 41.40(11) . . ? C14 Fe1 C2 153.55(11) . . ? C5 Fe1 C2 68.62(12) . . ? C11 Fe1 C2 106.31(12) . . ? C10 Fe1 C13 70.03(10) . . ? C1 Fe1 C13 155.14(11) . . ? C14 Fe1 C13 41.24(9) . . ? C5 Fe1 C13 123.41(11) . . ? C11 Fe1 C13 68.84(11) . . ? C2 Fe1 C13 163.45(11) . . ? C10 Fe1 C12 69.49(10) . . ? C1 Fe1 C12 155.74(11) . . ? C14 Fe1 C12 68.88(10) . . ? C5 Fe1 C12 162.84(12) . . ? C11 Fe1 C12 40.77(11) . . ? C2 Fe1 C12 125.79(11) . . ? C13 Fe1 C12 40.48(11) . . ? C10 Fe1 C4 152.83(11) . . ? C1 Fe1 C4 69.20(11) . . ? C14 Fe1 C4 121.32(12) . . ? C5 Fe1 C4 40.56(11) . . ? C11 Fe1 C4 165.76(11) . . ? C2 Fe1 C4 68.48(12) . . ? C13 Fe1 C4 112.17(12) . . ? C12 Fe1 C4 130.83(11) . . ? C10 Fe1 C3 157.48(12) . . ? C1 Fe1 C3 69.24(11) . . ? C14 Fe1 C3 160.16(12) . . ? C5 Fe1 C3 68.08(12) . . ? C11 Fe1 C3 127.34(12) . . ? C2 Fe1 C3 40.80(12) . . ? C13 Fe1 C3 128.94(11) . . ? C12 Fe1 C3 115.42(11) . . ? C4 Fe1 C3 40.29(13) . . ? C15 N1 C14 120.3(2) . . ? C5 C1 C2 106.8(2) . . ? C5 C1 C6 126.0(2) . . ? C2 C1 C6 127.2(3) . . ? C5 C1 Fe1 69.82(15) . . ? C2 C1 Fe1 69.95(15) . . ? C6 C1 Fe1 122.66(18) . . ? C3 C2 C1 108.2(3) . . ? C3 C2 Fe1 70.45(16) . . ? C1 C2 Fe1 68.66(15) . . ? C4 C3 C2 108.1(3) . . ? C4 C3 Fe1 69.80(16) . . ? C2 C3 Fe1 68.75(16) . . ? C5 C4 C3 107.7(3) . . ? C5 C4 Fe1 68.64(15) . . ? C3 C4 Fe1 69.91(16) . . ? C4 C5 C1 109.3(2) . . ? C4 C5 Fe1 70.79(16) . . ? C1 C5 Fe1 69.06(14) . . ? C1 C6 C7 111.7(2) . . ? C1 C6 C8 113.8(2) . . ? C7 C6 C8 111.9(2) . . ? C6 C8 C9 114.8(2) . . ? C10 C9 C30 112.1(2) . . ? C10 C9 C8 113.4(2) . . ? C30 C9 C8 111.23(19) . . ? C11 C10 C14 107.1(2) . . ? C11 C10 C9 125.4(2) . . ? C14 C10 C9 127.5(2) . . ? C11 C10 Fe1 70.20(14) . . ? C14 C10 Fe1 69.53(14) . . ? C9 C10 Fe1 123.58(16) . . ? C12 C11 C10 108.6(2) . . ? C12 C11 Fe1 70.61(15) . . ? C10 C11 Fe1 68.39(13) . . ? C13 C12 C11 108.4(2) . . ? C13 C12 Fe1 69.49(15) . . ? C11 C12 Fe1 68.63(14) . . ? C12 C13 C14 107.8(2) . . ? C12 C13 Fe1 70.03(15) . . ? C14 C13 Fe1 68.26(14) . . ? N1 C14 C13 129.9(2) . . ? N1 C14 C10 121.7(2) . . ? C13 C14 C10 108.1(2) . . ? N1 C14 Fe1 122.14(17) . . ? C13 C14 Fe1 70.50(14) . . ? C10 C14 Fe1 68.53(13) . . ? N1 C15 C16 121.3(2) . . ? C21 C16 C17 118.7(3) . . ? C21 C16 C15 121.2(2) . . ? C17 C16 C15 120.0(2) . . ? C18 C17 C16 120.3(3) . . ? C19 C18 C17 120.2(3) . . ? C18 C19 C20 120.1(3) . . ? C21 C20 C19 120.1(3) . . ? C20 C21 C16 120.6(3) . . ? Cl2 Zr1 Cl1 95.91(3) . . ? Cl2 Zr1 C33 96.70(7) . . ? Cl1 Zr1 C33 134.37(7) . . ? Cl2 Zr1 C36 112.76(8) . . ? Cl1 Zr1 C36 130.70(8) . . ? C33 Zr1 C36 82.80(10) . . ? Cl2 Zr1 C37 135.12(8) . . ? Cl1 Zr1 C37 99.44(9) . . ? C33 Zr1 C37 101.82(12) . . ? C36 Zr1 C37 32.66(11) . . ? Cl2 Zr1 C34 129.46(6) . . ? Cl1 Zr1 C34 114.51(6) . . ? C33 Zr1 C34 33.42(9) . . ? C36 Zr1 C34 77.45(10) . . ? C37 Zr1 C34 80.49(11) . . ? Cl2 Zr1 C35 83.42(8) . . ? Cl1 Zr1 C35 125.76(8) . . ? C33 Zr1 C35 99.19(11) . . ? C36 Zr1 C35 32.20(11) . . ? C37 Zr1 C35 53.58(10) . . ? C34 Zr1 C35 106.41(10) . . ? Cl2 Zr1 C39 84.02(11) . . ? Cl1 Zr1 C39 93.39(10) . . ? C33 Zr1 C39 131.45(11) . . ? C36 Zr1 C39 53.50(11) . . ? C37 Zr1 C39 53.31(13) . . ? C34 Zr1 C39 129.87(10) . . ? C35 Zr1 C39 32.41(12) . . ? Cl2 Zr1 C32 78.58(6) . . ? Cl1 Zr1 C32 109.27(7) . . ? C33 Zr1 C32 32.84(9) . . ? C36 Zr1 C32 115.00(10) . . ? C37 Zr1 C32 133.12(12) . . ? C34 Zr1 C32 54.24(9) . . ? C35 Zr1 C32 123.41(11) . . ? C39 Zr1 C32 152.56(13) . . ? Cl2 Zr1 C38 113.61(12) . . ? Cl1 Zr1 C38 79.05(8) . . ? C33 Zr1 C38 133.10(12) . . ? C36 Zr1 C38 53.26(11) . . ? C37 Zr1 C38 31.93(13) . . ? C34 Zr1 C38 111.23(13) . . ? C35 Zr1 C38 53.13(11) . . ? C39 Zr1 C38 31.90(14) . . ? C32 Zr1 C38 165.03(13) . . ? Cl2 Zr1 C31 96.51(6) . . ? Cl1 Zr1 C31 80.85(7) . . ? C33 Zr1 C31 54.24(9) . . ? C36 Zr1 C31 130.83(9) . . ? C37 Zr1 C31 127.41(10) . . ? C34 Zr1 C31 53.68(8) . . ? C35 Zr1 C31 153.34(10) . . ? C39 Zr1 C31 174.24(11) . . ? C32 Zr1 C31 32.38(9) . . ? C38 Zr1 C31 145.14(12) . . ? Cl2 Zr1 C30 128.66(6) . . ? Cl1 Zr1 C30 83.67(6) . . ? C33 Zr1 C30 54.75(9) . . ? C36 Zr1 C30 105.20(9) . . ? C37 Zr1 C30 94.94(10) . . ? C34 Zr1 C30 32.40(8) . . ? C35 Zr1 C30 136.82(10) . . ? C39 Zr1 C30 147.32(12) . . ? C32 Zr1 C30 54.09(8) . . ? C38 Zr1 C30 116.59(13) . . ? C31 Zr1 C30 32.49(8) . . ? C34 C30 C31 106.7(2) . . ? C34 C30 C9 128.7(2) . . ? C31 C30 C9 124.6(2) . . ? C34 C30 Zr1 71.55(14) . . ? C31 C30 Zr1 73.26(14) . . ? C9 C30 Zr1 120.62(15) . . ? C32 C31 C30 108.8(2) . . ? C32 C31 Zr1 72.88(15) . . ? C30 C31 Zr1 74.24(14) . . ? C33 C32 C31 108.1(2) . . ? C33 C32 Zr1 71.43(15) . . ? C31 C32 Zr1 74.75(14) . . ? C32 C33 C34 107.5(2) . . ? C32 C33 Zr1 75.72(15) . . ? C34 C33 Zr1 74.59(14) . . ? C30 C34 C33 108.9(2) . . ? C30 C34 Zr1 76.05(14) . . ? C33 C34 Zr1 71.98(14) . . ? C36 C35 C39 108.0(3) . . ? C36 C35 Zr1 73.49(17) . . ? C39 C35 Zr1 74.15(18) . . ? C35 C36 C37 107.8(3) . . ? C35 C36 Zr1 74.30(17) . . ? C37 C36 Zr1 73.74(17) . . ? C38 C37 C36 107.7(3) . . ? C38 C37 Zr1 75.03(19) . . ? C36 C37 Zr1 73.59(17) . . ? C37 C38 C39 108.8(3) . . ? C37 C38 Zr1 73.03(18) . . ? C39 C38 Zr1 73.74(19) . . ? C38 C39 C35 107.7(3) . . ? C38 C39 Zr1 74.36(19) . . ? C35 C39 Zr1 73.44(18) . . ? Cl11 C101 Cl12 111.3(8) . . ? 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 C10 Fe1 C1 C5 118.72(16) . . . . ? C14 Fe1 C1 C5 78.97(18) . . . . ? C11 Fe1 C1 C5 157.53(16) . . . . ? C2 Fe1 C1 C5 -117.5(2) . . . . ? C13 Fe1 C1 C5 61.3(3) . . . . ? C12 Fe1 C1 C5 173.9(2) . . . . ? C4 Fe1 C1 C5 -36.81(17) . . . . ? C3 Fe1 C1 C5 -80.04(18) . . . . ? C10 Fe1 C1 C2 -123.82(17) . . . . ? C14 Fe1 C1 C2 -163.56(16) . . . . ? C5 Fe1 C1 C2 117.5(2) . . . . ? C11 Fe1 C1 C2 -85.01(18) . . . . ? C13 Fe1 C1 C2 178.7(2) . . . . ? C12 Fe1 C1 C2 -68.6(3) . . . . ? C4 Fe1 C1 C2 80.65(18) . . . . ? C3 Fe1 C1 C2 37.42(17) . . . . ? C10 Fe1 C1 C6 -1.8(2) . . . . ? C14 Fe1 C1 C6 -41.5(3) . . . . ? C5 Fe1 C1 C6 -120.5(3) . . . . ? C11 Fe1 C1 C6 37.0(3) . . . . ? C2 Fe1 C1 C6 122.0(3) . . . . ? C13 Fe1 C1 C6 -59.2(4) . . . . ? C12 Fe1 C1 C6 53.4(4) . . . . ? C4 Fe1 C1 C6 -157.3(3) . . . . ? C3 Fe1 C1 C6 159.4(3) . . . . ? C5 C1 C2 C3 0.9(3) . . . . ? C6 C1 C2 C3 -175.9(2) . . . . ? Fe1 C1 C2 C3 -59.58(19) . . . . ? C5 C1 C2 Fe1 60.43(18) . . . . ? C6 C1 C2 Fe1 -116.4(3) . . . . ? C10 Fe1 C2 C3 -172.14(16) . . . . ? C1 Fe1 C2 C3 119.6(2) . . . . ? C14 Fe1 C2 C3 154.6(2) . . . . ? C5 Fe1 C2 C3 80.79(19) . . . . ? C11 Fe1 C2 C3 -128.91(17) . . . . ? C13 Fe1 C2 C3 -58.5(5) . . . . ? C12 Fe1 C2 C3 -88.5(2) . . . . ? C4 Fe1 C2 C3 37.06(18) . . . . ? C10 Fe1 C2 C1 68.26(18) . . . . ? C14 Fe1 C2 C1 35.0(3) . . . . ? C5 Fe1 C2 C1 -38.80(16) . . . . ? C11 Fe1 C2 C1 111.49(16) . . . . ? C13 Fe1 C2 C1 -178.1(3) . . . . ? C12 Fe1 C2 C1 151.86(16) . . . . ? C4 Fe1 C2 C1 -82.54(17) . . . . ? C3 Fe1 C2 C1 -119.6(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? Fe1 C2 C3 C4 -58.9(2) . . . . ? C1 C2 C3 Fe1 58.47(18) . . . . ? C10 Fe1 C3 C4 138.3(3) . . . . ? C1 Fe1 C3 C4 81.95(18) . . . . ? C14 Fe1 C3 C4 -25.8(4) . . . . ? C5 Fe1 C3 C4 37.66(17) . . . . ? C11 Fe1 C3 C4 -170.18(17) . . . . ? C2 Fe1 C3 C4 119.9(2) . . . . ? C13 Fe1 C3 C4 -78.3(2) . . . . ? C12 Fe1 C3 C4 -123.98(18) . . . . ? C10 Fe1 C3 C2 18.5(4) . . . . ? C1 Fe1 C3 C2 -37.94(17) . . . . ? C14 Fe1 C3 C2 -145.7(3) . . . . ? C5 Fe1 C3 C2 -82.23(18) . . . . ? C11 Fe1 C3 C2 69.9(2) . . . . ? C13 Fe1 C3 C2 161.80(16) . . . . ? C12 Fe1 C3 C2 116.13(18) . . . . ? C4 Fe1 C3 C2 -119.9(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Fe1 C3 C4 C5 -58.43(19) . . . . ? C2 C3 C4 Fe1 58.2(2) . . . . ? C10 Fe1 C4 C5 -26.8(3) . . . . ? C1 Fe1 C4 C5 37.30(17) . . . . ? C14 Fe1 C4 C5 -70.6(2) . . . . ? C11 Fe1 C4 C5 152.8(4) . . . . ? C2 Fe1 C4 C5 81.83(19) . . . . ? C13 Fe1 C4 C5 -115.99(17) . . . . ? C12 Fe1 C4 C5 -158.82(17) . . . . ? C3 Fe1 C4 C5 119.3(3) . . . . ? C10 Fe1 C4 C3 -146.1(2) . . . . ? C1 Fe1 C4 C3 -82.05(19) . . . . ? C14 Fe1 C4 C3 170.03(16) . . . . ? C5 Fe1 C4 C3 -119.3(3) . . . . ? C11 Fe1 C4 C3 33.5(6) . . . . ? C2 Fe1 C4 C3 -37.51(17) . . . . ? C13 Fe1 C4 C3 124.66(18) . . . . ? C12 Fe1 C4 C3 81.8(2) . . . . ? C3 C4 C5 C1 0.8(3) . . . . ? Fe1 C4 C5 C1 -58.47(18) . . . . ? C3 C4 C5 Fe1 59.2(2) . . . . ? C2 C1 C5 C4 -1.0(3) . . . . ? C6 C1 C5 C4 175.9(2) . . . . ? Fe1 C1 C5 C4 59.52(19) . . . . ? C2 C1 C5 Fe1 -60.52(18) . . . . ? C6 C1 C5 Fe1 116.3(3) . . . . ? C10 Fe1 C5 C4 166.96(17) . . . . ? C1 Fe1 C5 C4 -120.5(2) . . . . ? C14 Fe1 C5 C4 124.48(18) . . . . ? C11 Fe1 C5 C4 -166.4(2) . . . . ? C2 Fe1 C5 C4 -81.47(19) . . . . ? C13 Fe1 C5 C4 85.7(2) . . . . ? C12 Fe1 C5 C4 67.9(4) . . . . ? C3 Fe1 C5 C4 -37.42(18) . . . . ? C10 Fe1 C5 C1 -72.51(18) . . . . ? C14 Fe1 C5 C1 -114.99(16) . . . . ? C11 Fe1 C5 C1 -45.9(3) . . . . ? C2 Fe1 C5 C1 39.06(16) . . . . ? C13 Fe1 C5 C1 -153.79(15) . . . . ? C12 Fe1 C5 C1 -171.5(3) . . . . ? C4 Fe1 C5 C1 120.5(2) . . . . ? C3 Fe1 C5 C1 83.11(18) . . . . ? C5 C1 C6 C7 175.8(2) . . . . ? C2 C1 C6 C7 -7.9(4) . . . . ? Fe1 C1 C6 C7 -96.5(3) . . . . ? C5 C1 C6 C8 -56.3(3) . . . . ? C2 C1 C6 C8 119.9(3) . . . . ? Fe1 C1 C6 C8 31.3(3) . . . . ? C1 C6 C8 C9 -66.8(3) . . . . ? C7 C6 C8 C9 61.0(3) . . . . ? C6 C8 C9 C10 66.5(3) . . . . ? C6 C8 C9 C30 -166.0(2) . . . . ? C30 C9 C10 C11 113.5(3) . . . . ? C8 C9 C10 C11 -119.5(3) . . . . ? C30 C9 C10 C14 -69.1(3) . . . . ? C8 C9 C10 C14 57.8(3) . . . . ? C30 C9 C10 Fe1 -158.00(17) . . . . ? C8 C9 C10 Fe1 -31.0(3) . . . . ? C1 Fe1 C10 C11 121.86(16) . . . . ? C14 Fe1 C10 C11 -117.9(2) . . . . ? C5 Fe1 C10 C11 161.10(16) . . . . ? C2 Fe1 C10 C11 83.59(17) . . . . ? C13 Fe1 C10 C11 -80.29(16) . . . . ? C12 Fe1 C10 C11 -37.02(16) . . . . ? C4 Fe1 C10 C11 179.8(2) . . . . ? C3 Fe1 C10 C11 70.1(3) . . . . ? C1 Fe1 C10 C14 -120.28(14) . . . . ? C5 Fe1 C10 C14 -81.04(16) . . . . ? C11 Fe1 C10 C14 117.9(2) . . . . ? C2 Fe1 C10 C14 -158.55(14) . . . . ? C13 Fe1 C10 C14 37.57(14) . . . . ? C12 Fe1 C10 C14 80.84(15) . . . . ? C4 Fe1 C10 C14 -62.3(3) . . . . ? C3 Fe1 C10 C14 -172.0(3) . . . . ? C1 Fe1 C10 C9 1.8(2) . . . . ? C14 Fe1 C10 C9 122.1(2) . . . . ? C5 Fe1 C10 C9 41.1(2) . . . . ? C11 Fe1 C10 C9 -120.0(3) . . . . ? C2 Fe1 C10 C9 -36.4(2) . . . . ? C13 Fe1 C10 C9 159.7(2) . . . . ? C12 Fe1 C10 C9 -157.0(2) . . . . ? C4 Fe1 C10 C9 59.8(3) . . . . ? C3 Fe1 C10 C9 -49.9(4) . . . . ? C14 C10 C11 C12 -0.8(3) . . . . ? C9 C10 C11 C12 177.0(2) . . . . ? Fe1 C10 C11 C12 59.29(18) . . . . ? C14 C10 C11 Fe1 -60.05(16) . . . . ? C9 C10 C11 Fe1 117.7(2) . . . . ? C10 Fe1 C11 C12 -120.3(2) . . . . ? C1 Fe1 C11 C12 169.77(15) . . . . ? C14 Fe1 C11 C12 -81.13(16) . . . . ? C5 Fe1 C11 C12 -158.5(2) . . . . ? C2 Fe1 C11 C12 126.42(17) . . . . ? C13 Fe1 C11 C12 -36.86(16) . . . . ? C4 Fe1 C11 C12 60.0(5) . . . . ? C3 Fe1 C11 C12 86.7(2) . . . . ? C1 Fe1 C11 C10 -69.97(17) . . . . ? C14 Fe1 C11 C10 39.13(14) . . . . ? C5 Fe1 C11 C10 -38.2(3) . . . . ? C2 Fe1 C11 C10 -113.31(16) . . . . ? C13 Fe1 C11 C10 83.41(16) . . . . ? C12 Fe1 C11 C10 120.3(2) . . . . ? C4 Fe1 C11 C10 -179.7(4) . . . . ? C3 Fe1 C11 C10 -153.07(16) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? Fe1 C11 C12 C13 58.25(19) . . . . ? C10 C11 C12 Fe1 -57.93(17) . . . . ? C10 Fe1 C12 C13 -82.90(16) . . . . ? C1 Fe1 C12 C13 -143.3(2) . . . . ? C14 Fe1 C12 C13 -37.88(15) . . . . ? C5 Fe1 C12 C13 23.1(4) . . . . ? C11 Fe1 C12 C13 -120.5(2) . . . . ? C2 Fe1 C12 C13 167.33(16) . . . . ? C4 Fe1 C12 C13 75.9(2) . . . . ? C3 Fe1 C12 C13 121.00(17) . . . . ? C10 Fe1 C12 C11 37.59(15) . . . . ? C1 Fe1 C12 C11 -22.8(3) . . . . ? C14 Fe1 C12 C11 82.61(16) . . . . ? C5 Fe1 C12 C11 143.6(3) . . . . ? C2 Fe1 C12 C11 -72.2(2) . . . . ? C13 Fe1 C12 C11 120.5(2) . . . . ? C4 Fe1 C12 C11 -163.64(17) . . . . ? C3 Fe1 C12 C11 -118.51(17) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? Fe1 C12 C13 C14 57.97(17) . . . . ? C11 C12 C13 Fe1 -57.72(18) . . . . ? C10 Fe1 C13 C12 81.47(16) . . . . ? C1 Fe1 C13 C12 144.3(2) . . . . ? C14 Fe1 C13 C12 119.7(2) . . . . ? C5 Fe1 C13 C12 -172.04(15) . . . . ? C11 Fe1 C13 C12 37.11(15) . . . . ? C2 Fe1 C13 C12 -38.7(5) . . . . ? C4 Fe1 C13 C12 -127.59(16) . . . . ? C3 Fe1 C13 C12 -84.4(2) . . . . ? C10 Fe1 C13 C14 -38.19(14) . . . . ? C1 Fe1 C13 C14 24.6(3) . . . . ? C5 Fe1 C13 C14 68.30(18) . . . . ? C11 Fe1 C13 C14 -82.55(16) . . . . ? C2 Fe1 C13 C14 -158.3(4) . . . . ? C12 Fe1 C13 C14 -119.7(2) . . . . ? C4 Fe1 C13 C14 112.75(16) . . . . ? C3 Fe1 C13 C14 155.89(16) . . . . ? C15 N1 C14 C13 -17.9(4) . . . . ? C15 N1 C14 C10 168.4(2) . . . . ? C15 N1 C14 Fe1 -108.5(2) . . . . ? C12 C13 C14 N1 -175.1(2) . . . . ? Fe1 C13 C14 N1 -116.1(3) . . . . ? C12 C13 C14 C10 -0.7(3) . . . . ? Fe1 C13 C14 C10 58.35(16) . . . . ? C12 C13 C14 Fe1 -59.06(18) . . . . ? C11 C10 C14 N1 175.9(2) . . . . ? C9 C10 C14 N1 -1.8(4) . . . . ? Fe1 C10 C14 N1 115.4(2) . . . . ? C11 C10 C14 C13 0.9(3) . . . . ? C9 C10 C14 C13 -176.8(2) . . . . ? Fe1 C10 C14 C13 -59.58(17) . . . . ? C11 C10 C14 Fe1 60.48(16) . . . . ? C9 C10 C14 Fe1 -117.2(2) . . . . ? C10 Fe1 C14 N1 -114.9(2) . . . . ? C1 Fe1 C14 N1 -43.3(2) . . . . ? C5 Fe1 C14 N1 -2.0(2) . . . . ? C11 Fe1 C14 N1 -153.5(2) . . . . ? C2 Fe1 C14 N1 -68.1(3) . . . . ? C13 Fe1 C14 N1 125.5(3) . . . . ? C12 Fe1 C14 N1 162.7(2) . . . . ? C4 Fe1 C14 N1 36.9(2) . . . . ? C3 Fe1 C14 N1 56.1(4) . . . . ? C10 Fe1 C14 C13 119.6(2) . . . . ? C1 Fe1 C14 C13 -168.82(15) . . . . ? C5 Fe1 C14 C13 -127.50(16) . . . . ? C11 Fe1 C14 C13 80.96(16) . . . . ? C2 Fe1 C14 C13 166.3(2) . . . . ? C12 Fe1 C14 C13 37.21(15) . . . . ? C4 Fe1 C14 C13 -88.63(18) . . . . ? C3 Fe1 C14 C13 -69.4(4) . . . . ? C1 Fe1 C14 C10 71.56(16) . . . . ? C5 Fe1 C14 C10 112.88(14) . . . . ? C11 Fe1 C14 C10 -38.65(13) . . . . ? C2 Fe1 C14 C10 46.7(3) . . . . ? C13 Fe1 C14 C10 -119.6(2) . . . . ? C12 Fe1 C14 C10 -82.41(15) . . . . ? C4 Fe1 C14 C10 151.75(15) . . . . ? C3 Fe1 C14 C10 171.0(3) . . . . ? C14 N1 C15 C16 176.8(2) . . . . ? N1 C15 C16 C21 -2.9(4) . . . . ? N1 C15 C16 C17 178.2(2) . . . . ? C21 C16 C17 C18 -0.4(4) . . . . ? C15 C16 C17 C18 178.5(2) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 -0.4(7) . . . . ? C19 C20 C21 C16 0.4(7) . . . . ? C17 C16 C21 C20 -0.1(5) . . . . ? C15 C16 C21 C20 -179.0(3) . . . . ? C10 C9 C30 C34 21.7(3) . . . . ? C8 C9 C30 C34 -106.4(3) . . . . ? C10 C9 C30 C31 -158.6(2) . . . . ? C8 C9 C30 C31 73.3(3) . . . . ? C10 C9 C30 Zr1 -68.5(2) . . . . ? C8 C9 C30 Zr1 163.37(15) . . . . ? Cl2 Zr1 C30 C34 104.98(14) . . . . ? Cl1 Zr1 C30 C34 -162.51(14) . . . . ? C33 Zr1 C30 C34 37.47(15) . . . . ? C36 Zr1 C30 C34 -31.98(17) . . . . ? C37 Zr1 C30 C34 -63.53(17) . . . . ? C35 Zr1 C30 C34 -24.7(2) . . . . ? C39 Zr1 C30 C34 -76.1(2) . . . . ? C32 Zr1 C30 C34 78.14(16) . . . . ? C38 Zr1 C30 C34 -88.12(17) . . . . ? C31 Zr1 C30 C34 114.6(2) . . . . ? Cl2 Zr1 C30 C31 -9.63(18) . . . . ? Cl1 Zr1 C30 C31 82.88(15) . . . . ? C33 Zr1 C30 C31 -77.15(17) . . . . ? C36 Zr1 C30 C31 -146.59(16) . . . . ? C37 Zr1 C30 C31 -178.14(17) . . . . ? C34 Zr1 C30 C31 -114.6(2) . . . . ? C35 Zr1 C30 C31 -139.29(17) . . . . ? C39 Zr1 C30 C31 169.3(2) . . . . ? C32 Zr1 C30 C31 -36.47(16) . . . . ? C38 Zr1 C30 C31 157.27(16) . . . . ? Cl2 Zr1 C30 C9 -130.36(16) . . . . ? Cl1 Zr1 C30 C9 -37.84(17) . . . . ? C33 Zr1 C30 C9 162.1(2) . . . . ? C36 Zr1 C30 C9 92.68(19) . . . . ? C37 Zr1 C30 C9 61.1(2) . . . . ? C34 Zr1 C30 C9 124.7(2) . . . . ? C35 Zr1 C30 C9 100.0(2) . . . . ? C39 Zr1 C30 C9 48.6(3) . . . . ? C32 Zr1 C30 C9 -157.2(2) . . . . ? C38 Zr1 C30 C9 36.5(2) . . . . ? C31 Zr1 C30 C9 -120.7(3) . . . . ? C34 C30 C31 C32 1.0(3) . . . . ? C9 C30 C31 C32 -178.8(2) . . . . ? Zr1 C30 C31 C32 65.21(18) . . . . ? C34 C30 C31 Zr1 -64.20(17) . . . . ? C9 C30 C31 Zr1 116.0(2) . . . . ? Cl2 Zr1 C31 C32 56.49(16) . . . . ? Cl1 Zr1 C31 C32 151.46(16) . . . . ? C33 Zr1 C31 C32 -37.09(16) . . . . ? C36 Zr1 C31 C32 -71.3(2) . . . . ? C37 Zr1 C31 C32 -113.62(19) . . . . ? C34 Zr1 C31 C32 -78.75(17) . . . . ? C35 Zr1 C31 C32 -31.8(3) . . . . ? C39 Zr1 C31 C32 151.4(11) . . . . ? C38 Zr1 C31 C32 -153.2(2) . . . . ? C30 Zr1 C31 C32 -116.0(2) . . . . ? Cl2 Zr1 C31 C30 172.44(14) . . . . ? Cl1 Zr1 C31 C30 -92.59(15) . . . . ? C33 Zr1 C31 C30 78.86(16) . . . . ? C36 Zr1 C31 C30 44.6(2) . . . . ? C37 Zr1 C31 C30 2.3(2) . . . . ? C34 Zr1 C31 C30 37.20(14) . . . . ? C35 Zr1 C31 C30 84.1(3) . . . . ? C39 Zr1 C31 C30 -92.6(12) . . . . ? C32 Zr1 C31 C30 116.0(2) . . . . ? C38 Zr1 C31 C30 -37.2(3) . . . . ? C30 C31 C32 C33 -2.0(3) . . . . ? Zr1 C31 C32 C33 64.14(19) . . . . ? C30 C31 C32 Zr1 -66.10(17) . . . . ? Cl2 Zr1 C32 C33 122.16(16) . . . . ? Cl1 Zr1 C32 C33 -145.51(15) . . . . ? C36 Zr1 C32 C33 12.20(19) . . . . ? C37 Zr1 C32 C33 -21.1(2) . . . . ? C34 Zr1 C32 C33 -38.66(16) . . . . ? C35 Zr1 C32 C33 48.0(2) . . . . ? C39 Zr1 C32 C33 70.5(3) . . . . ? C38 Zr1 C32 C33 -23.6(5) . . . . ? C31 Zr1 C32 C33 -115.5(2) . . . . ? C30 Zr1 C32 C33 -78.92(17) . . . . ? Cl2 Zr1 C32 C31 -122.31(16) . . . . ? Cl1 Zr1 C32 C31 -29.98(17) . . . . ? C33 Zr1 C32 C31 115.5(2) . . . . ? C36 Zr1 C32 C31 127.73(17) . . . . ? C37 Zr1 C32 C31 94.4(2) . . . . ? C34 Zr1 C32 C31 76.87(16) . . . . ? C35 Zr1 C32 C31 163.55(16) . . . . ? C39 Zr1 C32 C31 -174.0(2) . . . . ? C38 Zr1 C32 C31 91.9(5) . . . . ? C30 Zr1 C32 C31 36.61(15) . . . . ? C31 C32 C33 C34 2.1(3) . . . . ? Zr1 C32 C33 C34 68.45(18) . . . . ? C31 C32 C33 Zr1 -66.32(19) . . . . ? Cl2 Zr1 C33 C32 -56.67(16) . . . . ? Cl1 Zr1 C33 C32 48.39(19) . . . . ? C36 Zr1 C33 C32 -168.87(18) . . . . ? C37 Zr1 C33 C32 164.44(17) . . . . ? C34 Zr1 C33 C32 113.0(2) . . . . ? C35 Zr1 C33 C32 -141.05(17) . . . . ? C39 Zr1 C33 C32 -144.6(2) . . . . ? C38 Zr1 C33 C32 171.87(19) . . . . ? C31 Zr1 C33 C32 36.55(15) . . . . ? C30 Zr1 C33 C32 76.74(17) . . . . ? Cl2 Zr1 C33 C34 -169.69(15) . . . . ? Cl1 Zr1 C33 C34 -64.63(19) . . . . ? C36 Zr1 C33 C34 78.11(18) . . . . ? C37 Zr1 C33 C34 51.41(18) . . . . ? C35 Zr1 C33 C34 105.92(17) . . . . ? C39 Zr1 C33 C34 102.4(2) . . . . ? C32 Zr1 C33 C34 -113.0(2) . . . . ? C38 Zr1 C33 C34 58.8(2) . . . . ? C31 Zr1 C33 C34 -76.48(17) . . . . ? C30 Zr1 C33 C34 -36.28(15) . . . . ? C31 C30 C34 C33 0.3(3) . . . . ? C9 C30 C34 C33 -179.9(2) . . . . ? Zr1 C30 C34 C33 -65.04(18) . . . . ? C31 C30 C34 Zr1 65.36(17) . . . . ? C9 C30 C34 Zr1 -114.9(2) . . . . ? C32 C33 C34 C30 -1.5(3) . . . . ? Zr1 C33 C34 C30 67.70(18) . . . . ? C32 C33 C34 Zr1 -69.22(18) . . . . ? Cl2 Zr1 C34 C30 -102.29(14) . . . . ? Cl1 Zr1 C34 C30 19.17(16) . . . . ? C33 Zr1 C34 C30 -115.6(2) . . . . ? C36 Zr1 C34 C30 148.43(16) . . . . ? C37 Zr1 C34 C30 115.27(16) . . . . ? C35 Zr1 C34 C30 162.67(15) . . . . ? C39 Zr1 C34 C30 136.93(19) . . . . ? C32 Zr1 C34 C30 -77.64(16) . . . . ? C38 Zr1 C34 C30 106.49(16) . . . . ? C31 Zr1 C34 C30 -37.31(14) . . . . ? Cl2 Zr1 C34 C33 13.3(2) . . . . ? Cl1 Zr1 C34 C33 134.77(15) . . . . ? C36 Zr1 C34 C33 -95.97(18) . . . . ? C37 Zr1 C34 C33 -129.13(18) . . . . ? C35 Zr1 C34 C33 -81.73(18) . . . . ? C39 Zr1 C34 C33 -107.5(2) . . . . ? C32 Zr1 C34 C33 37.96(17) . . . . ? C38 Zr1 C34 C33 -137.91(18) . . . . ? C31 Zr1 C34 C33 78.29(18) . . . . ? C30 Zr1 C34 C33 115.6(2) . . . . ? Cl2 Zr1 C35 C36 -156.06(19) . . . . ? Cl1 Zr1 C35 C36 111.38(19) . . . . ? C33 Zr1 C35 C36 -60.3(2) . . . . ? C37 Zr1 C35 C36 37.7(2) . . . . ? C34 Zr1 C35 C36 -26.8(2) . . . . ? C39 Zr1 C35 C36 114.7(3) . . . . ? C32 Zr1 C35 C36 -84.4(2) . . . . ? C38 Zr1 C35 C36 77.7(2) . . . . ? C31 Zr1 C35 C36 -64.7(3) . . . . ? C30 Zr1 C35 C36 -13.3(3) . . . . ? Cl2 Zr1 C35 C39 89.2(2) . . . . ? Cl1 Zr1 C35 C39 -3.4(3) . . . . ? C33 Zr1 C35 C39 -175.1(2) . . . . ? C36 Zr1 C35 C39 -114.7(3) . . . . ? C37 Zr1 C35 C39 -77.1(3) . . . . ? C34 Zr1 C35 C39 -141.5(2) . . . . ? C32 Zr1 C35 C39 160.8(2) . . . . ? C38 Zr1 C35 C39 -37.0(2) . . . . ? C31 Zr1 C35 C39 -179.4(2) . . . . ? C30 Zr1 C35 C39 -128.0(2) . . . . ? C39 C35 C36 C37 0.0(3) . . . . ? Zr1 C35 C36 C37 -66.7(2) . . . . ? C39 C35 C36 Zr1 66.7(2) . . . . ? Cl2 Zr1 C36 C35 25.9(2) . . . . ? Cl1 Zr1 C36 C35 -94.6(2) . . . . ? C33 Zr1 C36 C35 120.2(2) . . . . ? C37 Zr1 C36 C35 -114.4(3) . . . . ? C34 Zr1 C36 C35 153.7(2) . . . . ? C39 Zr1 C36 C35 -37.3(2) . . . . ? C32 Zr1 C36 C35 113.55(19) . . . . ? C38 Zr1 C36 C35 -77.3(2) . . . . ? C31 Zr1 C36 C35 147.59(18) . . . . ? C30 Zr1 C36 C35 170.61(19) . . . . ? Cl2 Zr1 C36 C37 140.3(2) . . . . ? Cl1 Zr1 C36 C37 19.7(2) . . . . ? C33 Zr1 C36 C37 -125.4(2) . . . . ? C34 Zr1 C36 C37 -91.9(2) . . . . ? C35 Zr1 C36 C37 114.4(3) . . . . ? C39 Zr1 C36 C37 77.1(2) . . . . ? C32 Zr1 C36 C37 -132.1(2) . . . . ? C38 Zr1 C36 C37 37.1(2) . . . . ? C31 Zr1 C36 C37 -98.0(2) . . . . ? C30 Zr1 C36 C37 -75.0(2) . . . . ? C35 C36 C37 C38 -0.8(3) . . . . ? Zr1 C36 C37 C38 -67.9(2) . . . . ? C35 C36 C37 Zr1 67.1(2) . . . . ? Cl2 Zr1 C37 C38 57.4(3) . . . . ? Cl1 Zr1 C37 C38 -50.9(2) . . . . ? C33 Zr1 C37 C38 169.7(2) . . . . ? C36 Zr1 C37 C38 114.0(3) . . . . ? C34 Zr1 C37 C38 -164.4(2) . . . . ? C35 Zr1 C37 C38 76.9(2) . . . . ? C39 Zr1 C37 C38 36.3(2) . . . . ? C32 Zr1 C37 C38 -178.8(2) . . . . ? C31 Zr1 C37 C38 -136.6(2) . . . . ? C30 Zr1 C37 C38 -135.3(2) . . . . ? Cl2 Zr1 C37 C36 -56.6(3) . . . . ? Cl1 Zr1 C37 C36 -164.95(19) . . . . ? C33 Zr1 C37 C36 55.7(2) . . . . ? C34 Zr1 C37 C36 81.6(2) . . . . ? C35 Zr1 C37 C36 -37.10(19) . . . . ? C39 Zr1 C37 C36 -77.8(2) . . . . ? C32 Zr1 C37 C36 67.2(2) . . . . ? C38 Zr1 C37 C36 -114.0(3) . . . . ? C31 Zr1 C37 C36 109.4(2) . . . . ? C30 Zr1 C37 C36 110.7(2) . . . . ? C36 C37 C38 C39 1.3(4) . . . . ? Zr1 C37 C38 C39 -65.6(2) . . . . ? C36 C37 C38 Zr1 66.9(2) . . . . ? Cl2 Zr1 C38 C37 -139.5(2) . . . . ? Cl1 Zr1 C38 C37 128.8(2) . . . . ? C33 Zr1 C38 C37 -13.8(3) . . . . ? C36 Zr1 C38 C37 -37.95(19) . . . . ? C34 Zr1 C38 C37 16.5(2) . . . . ? C35 Zr1 C38 C37 -78.5(2) . . . . ? C39 Zr1 C38 C37 -116.1(3) . . . . ? C32 Zr1 C38 C37 3.4(6) . . . . ? C31 Zr1 C38 C37 72.9(3) . . . . ? C30 Zr1 C38 C37 51.6(2) . . . . ? Cl2 Zr1 C38 C39 -23.4(2) . . . . ? Cl1 Zr1 C38 C39 -115.1(2) . . . . ? C33 Zr1 C38 C39 102.3(3) . . . . ? C36 Zr1 C38 C39 78.1(2) . . . . ? C37 Zr1 C38 C39 116.1(3) . . . . ? C34 Zr1 C38 C39 132.6(2) . . . . ? C35 Zr1 C38 C39 37.6(2) . . . . ? C32 Zr1 C38 C39 119.5(5) . . . . ? C31 Zr1 C38 C39 -171.00(19) . . . . ? C30 Zr1 C38 C39 167.7(2) . . . . ? C37 C38 C39 C35 -1.3(4) . . . . ? Zr1 C38 C39 C35 -66.4(2) . . . . ? C37 C38 C39 Zr1 65.1(2) . . . . ? C36 C35 C39 C38 0.8(4) . . . . ? Zr1 C35 C39 C38 67.0(2) . . . . ? C36 C35 C39 Zr1 -66.3(2) . . . . ? Cl2 Zr1 C39 C38 158.5(2) . . . . ? Cl1 Zr1 C39 C38 62.9(2) . . . . ? C33 Zr1 C39 C38 -107.8(3) . . . . ? C36 Zr1 C39 C38 -77.3(2) . . . . ? C37 Zr1 C39 C38 -36.3(2) . . . . ? C34 Zr1 C39 C38 -63.3(3) . . . . ? C35 Zr1 C39 C38 -114.3(3) . . . . ? C32 Zr1 C39 C38 -150.8(3) . . . . ? C31 Zr1 C39 C38 63.0(12) . . . . ? C30 Zr1 C39 C38 -20.7(3) . . . . ? Cl2 Zr1 C39 C35 -87.1(2) . . . . ? Cl1 Zr1 C39 C35 177.3(2) . . . . ? C33 Zr1 C39 C35 6.5(3) . . . . ? C36 Zr1 C39 C35 37.02(19) . . . . ? C37 Zr1 C39 C35 78.0(2) . . . . ? C34 Zr1 C39 C35 51.0(3) . . . . ? C32 Zr1 C39 C35 -36.5(4) . . . . ? C38 Zr1 C39 C35 114.3(3) . . . . ? C31 Zr1 C39 C35 177.3(10) . . . . ? C30 Zr1 C39 C35 93.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.986 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.076