# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr. Michael Bolte' _publ_contact_author_email bolte@chemie.uni-frankfurt.de loop_ _publ_author_name A.Reichert H.-W.Lerner M.Wagner A.Reichert M.Bolte data_wa1134 _database_code_depnum_ccdc_archive 'CCDC 894219' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 B Cl Fe Zr' _chemical_formula_sum 'C20 H22 B Cl Fe Zr' _chemical_formula_weight 455.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7184(6) _cell_length_b 12.6232(7) _cell_length_c 18.4245(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.130(6) _cell_angle_gamma 90.00 _cell_volume 1794.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11081 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5858 _exptl_absorpt_correction_T_max 0.7288 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 9248 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.63 _reflns_number_total 3338 _reflns_number_gt 2910 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0534P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3338 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Zr1 Zr 0.89322(3) 0.51893(2) 0.722678(13) 0.01727(11) Uani 1 1 d . . . Fe1 Fe 0.64252(5) 0.77584(3) 0.51073(2) 0.01954(13) Uani 1 1 d . . . Cl1 Cl 1.12332(9) 0.59926(6) 0.80377(4) 0.03109(19) Uani 1 1 d . . . B1 B 0.7547(5) 0.6913(3) 0.67320(18) 0.0263(7) Uani 1 1 d . . . H1A H 0.721(5) 0.604(3) 0.658(2) 0.045(11) Uiso 1 1 d . . . H1B H 0.882(4) 0.679(3) 0.7084(19) 0.031(9) Uiso 1 1 d . . . H1C H 0.667(5) 0.715(3) 0.708(2) 0.041(10) Uiso 1 1 d . . . C1 C 0.7902(4) 0.7656(2) 0.60480(15) 0.0233(6) Uani 1 1 d . . . C2 C 0.7155(4) 0.8689(2) 0.59603(17) 0.0271(6) Uani 1 1 d . . . H2 H 0.6393 0.9018 0.6291 0.033 Uiso 1 1 calc R . . C3 C 0.7730(4) 0.9145(3) 0.53043(17) 0.0295(7) Uani 1 1 d . . . H3 H 0.7427 0.9827 0.5124 0.035 Uiso 1 1 calc R . . C4 C 0.8835(4) 0.8407(3) 0.49650(16) 0.0268(6) Uani 1 1 d . . . H4 H 0.9398 0.8503 0.4516 0.032 Uiso 1 1 calc R . . C5 C 0.8949(4) 0.7498(3) 0.54162(16) 0.0267(6) Uani 1 1 d . . . H5 H 0.9610 0.6882 0.5318 0.032 Uiso 1 1 calc R . . C11 C 0.4523(4) 0.6662(3) 0.52168(19) 0.0342(7) Uani 1 1 d . . . H11 H 0.4368 0.6219 0.5627 0.041 Uiso 1 1 calc R . . C12 C 0.3780(4) 0.7679(3) 0.51128(19) 0.0346(7) Uani 1 1 d . . . H12 H 0.3042 0.8037 0.5439 0.041 Uiso 1 1 calc R . . C13 C 0.4339(4) 0.8065(3) 0.44336(17) 0.0311(7) Uani 1 1 d . . . H13 H 0.4036 0.8728 0.4223 0.037 Uiso 1 1 calc R . . C14 C 0.5431(4) 0.7288(3) 0.41232(17) 0.0298(7) Uani 1 1 d . . . H14 H 0.5992 0.7346 0.3671 0.036 Uiso 1 1 calc R . . C15 C 0.5541(4) 0.6416(3) 0.46018(18) 0.0313(7) Uani 1 1 d . . . H15 H 0.6176 0.5782 0.4528 0.038 Uiso 1 1 calc R . . C21 C 0.8249(4) 0.4343(3) 0.84141(17) 0.0358(8) Uani 1 1 d . . . H21 H 0.9168 0.4230 0.8756 0.043 Uiso 1 1 calc R . . C22 C 0.7700(5) 0.3640(3) 0.7877(2) 0.0433(10) Uani 1 1 d . . . H22 H 0.8169 0.2957 0.7793 0.052 Uiso 1 1 calc R . . C23 C 0.6334(4) 0.4110(3) 0.74777(19) 0.0378(8) Uani 1 1 d . . . H23 H 0.5742 0.3813 0.7069 0.045 Uiso 1 1 calc R . . C24 C 0.6003(4) 0.5102(3) 0.77954(17) 0.0290(7) Uani 1 1 d . . . H24 H 0.5118 0.5586 0.7650 0.035 Uiso 1 1 calc R . . C25 C 0.7206(4) 0.5248(3) 0.83608(17) 0.0291(7) Uani 1 1 d . . . H25 H 0.7302 0.5859 0.8660 0.035 Uiso 1 1 calc R . . C31 C 1.1674(4) 0.4567(3) 0.66737(19) 0.0369(8) Uani 1 1 d . . . H31 H 1.2736 0.4656 0.6936 0.044 Uiso 1 1 calc R . . C32 C 1.0581(5) 0.3690(3) 0.67068(19) 0.0381(8) Uani 1 1 d . . . H32 H 1.0763 0.3083 0.7003 0.046 Uiso 1 1 calc R . . C33 C 0.9168(5) 0.3855(3) 0.62282(18) 0.0361(8) Uani 1 1 d . . . H33 H 0.8230 0.3381 0.6142 0.043 Uiso 1 1 calc R . . C34 C 0.9396(4) 0.4840(3) 0.59028(17) 0.0307(7) Uani 1 1 d . . . H34 H 0.8641 0.5151 0.5549 0.037 Uiso 1 1 calc R . . C35 C 1.0927(4) 0.5298(3) 0.61843(17) 0.0296(7) Uani 1 1 d . . . H35 H 1.1375 0.5975 0.6066 0.035 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 Zr1 0.01693(15) 0.01935(17) 0.01560(16) 0.00067(10) 0.00200(10) 0.00057(9) Fe1 0.0199(2) 0.0204(2) 0.0183(2) -0.00123(16) 0.00116(15) 0.00147(15) Cl1 0.0297(4) 0.0293(4) 0.0339(4) 0.0014(3) -0.0106(3) -0.0040(3) B1 0.0310(16) 0.0240(17) 0.0240(16) -0.0017(14) 0.0004(13) 0.0083(14) C1 0.0240(13) 0.0256(15) 0.0200(13) -0.0021(12) -0.0035(11) 0.0018(11) C2 0.0345(15) 0.0225(15) 0.0243(15) -0.0050(12) -0.0014(12) 0.0004(12) C3 0.0386(16) 0.0215(15) 0.0281(16) 0.0002(13) -0.0050(13) -0.0055(13) C4 0.0245(13) 0.0319(17) 0.0241(15) 0.0034(13) -0.0012(11) -0.0064(12) C5 0.0211(13) 0.0327(17) 0.0264(15) 0.0006(13) 0.0009(11) 0.0015(12) C11 0.0268(14) 0.0403(19) 0.0356(17) 0.0018(15) 0.0032(13) -0.0106(14) C12 0.0204(13) 0.047(2) 0.0364(17) -0.0083(16) 0.0040(12) 0.0021(13) C13 0.0263(14) 0.0364(18) 0.0302(16) -0.0036(14) -0.0076(12) 0.0033(13) C14 0.0288(14) 0.0382(18) 0.0224(14) -0.0072(14) -0.0020(12) -0.0032(13) C15 0.0315(15) 0.0270(17) 0.0355(17) -0.0094(14) 0.0003(13) -0.0056(13) C21 0.0298(15) 0.053(2) 0.0249(16) 0.0178(16) 0.0054(13) 0.0032(15) C22 0.054(2) 0.0237(17) 0.053(2) 0.0098(16) 0.0378(19) -0.0004(15) C23 0.0348(16) 0.049(2) 0.0306(17) -0.0085(16) 0.0098(14) -0.0224(15) C24 0.0182(13) 0.0396(18) 0.0296(17) 0.0050(14) 0.0074(12) -0.0023(12) C25 0.0295(15) 0.0378(18) 0.0205(14) -0.0072(13) 0.0098(12) -0.0065(13) C31 0.0203(14) 0.052(2) 0.0386(19) -0.0019(16) 0.0077(13) 0.0124(14) C32 0.0472(19) 0.0303(17) 0.0375(19) 0.0031(15) 0.0205(16) 0.0135(15) C33 0.0439(18) 0.0357(18) 0.0292(17) -0.0120(15) 0.0159(15) -0.0048(15) C34 0.0353(16) 0.0396(19) 0.0174(14) -0.0035(13) 0.0077(12) 0.0076(13) C35 0.0276(15) 0.0333(17) 0.0283(16) 0.0035(13) 0.0149(13) 0.0040(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 Zr1 C23 2.475(3) . ? Zr1 C32 2.483(3) . ? Zr1 C35 2.489(3) . ? Zr1 C22 2.491(3) . ? Zr1 C31 2.493(3) . ? Zr1 C21 2.500(3) . ? Zr1 C25 2.501(3) . ? Zr1 C33 2.504(3) . ? Zr1 C34 2.512(3) . ? Zr1 Cl1 2.5120(8) . ? Zr1 C24 2.513(3) . ? Zr1 B1 2.583(4) . ? Zr1 H1A 2.07(4) . ? Zr1 H1B 2.04(4) . ? Fe1 C11 2.030(3) . ? Fe1 C2 2.033(3) . ? Fe1 C14 2.043(3) . ? Fe1 C15 2.044(3) . ? Fe1 C12 2.044(3) . ? Fe1 C5 2.045(3) . ? Fe1 C3 2.048(3) . ? Fe1 C13 2.050(3) . ? Fe1 C4 2.053(3) . ? Fe1 C1 2.060(3) . ? B1 C1 1.599(4) . ? B1 H1A 1.17(4) . ? B1 H1B 1.18(4) . ? B1 H1C 0.98(4) . ? C1 C2 1.434(4) . ? C1 C5 1.444(4) . ? C2 C3 1.418(4) . ? C2 H2 0.9500 . ? C3 C4 1.417(4) . ? C3 H3 0.9500 . ? C4 C5 1.418(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C12 1.417(5) . ? C11 C15 1.426(5) . ? C11 H11 0.9500 . ? C12 C13 1.418(5) . ? C12 H12 0.9500 . ? C13 C14 1.420(4) . ? C13 H13 0.9500 . ? C14 C15 1.412(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C22 1.389(6) . ? C21 C25 1.400(5) . ? C21 H21 0.9500 . ? C22 C23 1.405(6) . ? C22 H22 0.9500 . ? C23 C24 1.408(5) . ? C23 H23 0.9500 . ? C24 C25 1.394(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.394(5) . ? C31 C35 1.405(5) . ? C31 H31 0.9500 . ? C32 C33 1.405(5) . ? C32 H32 0.9500 . ? C33 C34 1.393(5) . ? C33 H33 0.9500 . ? C34 C35 1.406(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Zr1 C32 94.36(12) . . ? C23 Zr1 C35 133.64(12) . . ? C32 Zr1 C35 54.17(11) . . ? C23 Zr1 C22 32.85(13) . . ? C32 Zr1 C22 77.93(11) . . ? C35 Zr1 C22 131.44(11) . . ? C23 Zr1 C31 126.89(13) . . ? C32 Zr1 C31 32.52(12) . . ? C35 Zr1 C31 32.76(11) . . ? C22 Zr1 C31 106.53(12) . . ? C23 Zr1 C21 54.26(12) . . ? C32 Zr1 C21 97.50(12) . . ? C35 Zr1 C21 147.46(11) . . ? C22 Zr1 C21 32.33(13) . . ? C31 Zr1 C21 114.73(12) . . ? C23 Zr1 C25 54.08(11) . . ? C32 Zr1 C25 129.07(11) . . ? C35 Zr1 C25 172.23(11) . . ? C22 Zr1 C25 53.62(11) . . ? C31 Zr1 C25 145.19(12) . . ? C21 Zr1 C25 32.51(11) . . ? C23 Zr1 C33 80.67(11) . . ? C32 Zr1 C33 32.71(13) . . ? C35 Zr1 C33 54.19(11) . . ? C22 Zr1 C33 81.90(11) . . ? C31 Zr1 C33 54.07(12) . . ? C21 Zr1 C33 112.03(12) . . ? C25 Zr1 C33 132.95(11) . . ? C23 Zr1 C34 102.48(11) . . ? C32 Zr1 C34 53.67(12) . . ? C35 Zr1 C34 32.65(11) . . ? C22 Zr1 C34 113.08(12) . . ? C31 Zr1 C34 53.81(12) . . ? C21 Zr1 C34 144.24(12) . . ? C25 Zr1 C34 154.82(11) . . ? C33 Zr1 C34 32.26(11) . . ? C23 Zr1 Cl1 132.61(9) . . ? C32 Zr1 Cl1 100.10(10) . . ? C35 Zr1 Cl1 89.77(9) . . ? C22 Zr1 Cl1 107.65(11) . . ? C31 Zr1 Cl1 76.97(9) . . ? C21 Zr1 Cl1 79.09(9) . . ? C25 Zr1 Cl1 82.72(8) . . ? C33 Zr1 Cl1 130.38(9) . . ? C34 Zr1 Cl1 122.42(8) . . ? C23 Zr1 C24 32.77(12) . . ? C32 Zr1 C24 126.85(12) . . ? C35 Zr1 C24 154.09(11) . . ? C22 Zr1 C24 53.85(11) . . ? C31 Zr1 C24 159.12(12) . . ? C21 Zr1 C24 53.81(11) . . ? C25 Zr1 C24 32.28(11) . . ? C33 Zr1 C24 110.85(11) . . ? C34 Zr1 C24 122.94(11) . . ? Cl1 Zr1 C24 113.65(8) . . ? C23 Zr1 B1 101.43(13) . . ? C32 Zr1 B1 135.86(11) . . ? C35 Zr1 B1 86.53(10) . . ? C22 Zr1 B1 132.18(12) . . ? C31 Zr1 B1 118.02(11) . . ? C21 Zr1 B1 125.16(11) . . ? C25 Zr1 B1 92.65(11) . . ? C33 Zr1 B1 110.06(12) . . ? C34 Zr1 B1 82.59(11) . . ? Cl1 Zr1 B1 98.79(9) . . ? C24 Zr1 B1 79.30(11) . . ? C23 Zr1 H1A 83.0(11) . . ? C32 Zr1 H1A 120.1(11) . . ? C35 Zr1 H1A 85.9(10) . . ? C22 Zr1 H1A 115.9(11) . . ? C31 Zr1 H1A 118.0(10) . . ? C21 Zr1 H1A 125.5(10) . . ? C25 Zr1 H1A 96.8(10) . . ? C33 Zr1 H1A 88.9(11) . . ? C34 Zr1 H1A 68.5(10) . . ? Cl1 Zr1 H1A 125.0(12) . . ? C24 Zr1 H1A 71.9(10) . . ? B1 Zr1 H1A 26.2(11) . . ? C23 Zr1 H1B 122.5(9) . . ? C32 Zr1 H1B 136.5(9) . . ? C35 Zr1 H1B 82.6(9) . . ? C22 Zr1 H1B 145.5(9) . . ? C31 Zr1 H1B 107.0(9) . . ? C21 Zr1 H1B 121.8(9) . . ? C25 Zr1 H1B 93.3(9) . . ? C33 Zr1 H1B 125.1(10) . . ? C34 Zr1 H1B 93.1(10) . . ? Cl1 Zr1 H1B 72.8(10) . . ? C24 Zr1 H1B 93.6(9) . . ? B1 Zr1 H1B 26.3(10) . . ? H1A Zr1 H1B 52.2(15) . . ? C11 Fe1 C2 120.45(13) . . ? C11 Fe1 C14 68.32(13) . . ? C2 Fe1 C14 161.35(14) . . ? C11 Fe1 C15 40.97(13) . . ? C2 Fe1 C15 156.37(13) . . ? C14 Fe1 C15 40.42(14) . . ? C11 Fe1 C12 40.70(15) . . ? C2 Fe1 C12 106.61(13) . . ? C14 Fe1 C12 68.44(13) . . ? C15 Fe1 C12 68.73(13) . . ? C11 Fe1 C5 123.33(14) . . ? C2 Fe1 C5 68.28(13) . . ? C14 Fe1 C5 122.64(12) . . ? C15 Fe1 C5 107.53(13) . . ? C12 Fe1 C5 159.48(13) . . ? C11 Fe1 C3 156.73(13) . . ? C2 Fe1 C3 40.65(12) . . ? C14 Fe1 C3 125.47(13) . . ? C15 Fe1 C3 161.38(13) . . ? C12 Fe1 C3 121.90(14) . . ? C5 Fe1 C3 68.03(13) . . ? C11 Fe1 C13 68.16(14) . . ? C2 Fe1 C13 124.14(13) . . ? C14 Fe1 C13 40.60(13) . . ? C15 Fe1 C13 68.24(14) . . ? C12 Fe1 C13 40.52(14) . . ? C5 Fe1 C13 158.61(12) . . ? C3 Fe1 C13 108.88(14) . . ? C11 Fe1 C4 160.53(14) . . ? C2 Fe1 C4 68.32(12) . . ? C14 Fe1 C4 109.13(12) . . ? C15 Fe1 C4 124.56(12) . . ? C12 Fe1 C4 158.01(14) . . ? C5 Fe1 C4 40.50(12) . . ? C3 Fe1 C4 40.42(13) . . ? C13 Fe1 C4 123.36(13) . . ? C11 Fe1 C1 105.23(13) . . ? C2 Fe1 C1 41.02(12) . . ? C14 Fe1 C1 157.01(13) . . ? C15 Fe1 C1 120.37(13) . . ? C12 Fe1 C1 121.93(13) . . ? C5 Fe1 C1 41.19(11) . . ? C3 Fe1 C1 69.06(13) . . ? C13 Fe1 C1 159.43(12) . . ? C4 Fe1 C1 69.20(11) . . ? C1 B1 Zr1 134.1(2) . . ? C1 B1 H1A 113.9(19) . . ? Zr1 B1 H1A 52(2) . . ? C1 B1 H1B 111.0(17) . . ? Zr1 B1 H1B 50.0(18) . . ? H1A B1 H1B 101(3) . . ? C1 B1 H1C 118(2) . . ? Zr1 B1 H1C 108(2) . . ? H1A B1 H1C 107(3) . . ? H1B B1 H1C 105(3) . . ? C2 C1 C5 105.4(3) . . ? C2 C1 B1 123.2(2) . . ? C5 C1 B1 131.4(3) . . ? C2 C1 Fe1 68.49(17) . . ? C5 C1 Fe1 68.86(16) . . ? B1 C1 Fe1 126.8(2) . . ? C3 C2 C1 109.5(3) . . ? C3 C2 Fe1 70.26(18) . . ? C1 C2 Fe1 70.49(17) . . ? C3 C2 H2 125.3 . . ? C1 C2 H2 125.3 . . ? Fe1 C2 H2 125.6 . . ? C4 C3 C2 108.1(3) . . ? C4 C3 Fe1 69.97(18) . . ? C2 C3 Fe1 69.09(17) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.5 . . ? C3 C4 C5 107.7(2) . . ? C3 C4 Fe1 69.60(17) . . ? C5 C4 Fe1 69.43(16) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Fe1 C4 H4 126.4 . . ? C4 C5 C1 109.4(3) . . ? C4 C5 Fe1 70.07(17) . . ? C1 C5 Fe1 69.96(16) . . ? C4 C5 H5 125.3 . . ? C1 C5 H5 125.3 . . ? Fe1 C5 H5 126.3 . . ? C12 C11 C15 108.5(3) . . ? C12 C11 Fe1 70.18(19) . . ? C15 C11 Fe1 70.03(18) . . ? C12 C11 H11 125.7 . . ? C15 C11 H11 125.7 . . ? Fe1 C11 H11 125.6 . . ? C11 C12 C13 107.5(3) . . ? C11 C12 Fe1 69.12(17) . . ? C13 C12 Fe1 69.96(17) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? Fe1 C12 H12 126.2 . . ? C12 C13 C14 108.2(3) . . ? C12 C13 Fe1 69.52(18) . . ? C14 C13 Fe1 69.42(18) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Fe1 C13 H13 126.7 . . ? C15 C14 C13 108.4(3) . . ? C15 C14 Fe1 69.83(18) . . ? C13 C14 Fe1 69.98(18) . . ? C15 C14 H14 125.8 . . ? C13 C14 H14 125.8 . . ? Fe1 C14 H14 126.0 . . ? C14 C15 C11 107.4(3) . . ? C14 C15 Fe1 69.74(18) . . ? C11 C15 Fe1 69.00(18) . . ? C14 C15 H15 126.3 . . ? C11 C15 H15 126.3 . . ? Fe1 C15 H15 126.5 . . ? C22 C21 C25 107.7(3) . . ? C22 C21 Zr1 73.49(18) . . ? C25 C21 Zr1 73.80(17) . . ? C22 C21 H21 126.2 . . ? C25 C21 H21 126.2 . . ? Zr1 C21 H21 118.5 . . ? C21 C22 C23 108.6(3) . . ? C21 C22 Zr1 74.18(18) . . ? C23 C22 Zr1 72.96(18) . . ? C21 C22 H22 125.7 . . ? C23 C22 H22 125.7 . . ? Zr1 C22 H22 119.0 . . ? C22 C23 C24 107.4(3) . . ? C22 C23 Zr1 74.19(18) . . ? C24 C23 Zr1 75.08(17) . . ? C22 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? Zr1 C23 H23 116.6 . . ? C25 C24 C23 107.7(3) . . ? C25 C24 Zr1 73.40(16) . . ? C23 C24 Zr1 72.15(16) . . ? C25 C24 H24 126.1 . . ? C23 C24 H24 126.1 . . ? Zr1 C24 H24 120.1 . . ? C24 C25 C21 108.6(3) . . ? C24 C25 Zr1 74.32(16) . . ? C21 C25 Zr1 73.69(16) . . ? C24 C25 H25 125.7 . . ? C21 C25 H25 125.7 . . ? Zr1 C25 H25 118.2 . . ? C32 C31 C35 108.0(3) . . ? C32 C31 Zr1 73.34(17) . . ? C35 C31 Zr1 73.46(16) . . ? C32 C31 H31 126.0 . . ? C35 C31 H31 126.0 . . ? Zr1 C31 H31 119.1 . . ? C31 C32 C33 108.5(3) . . ? C31 C32 Zr1 74.13(18) . . ? C33 C32 Zr1 74.44(18) . . ? C31 C32 H32 125.7 . . ? C33 C32 H32 125.7 . . ? Zr1 C32 H32 117.6 . . ? C34 C33 C32 107.4(3) . . ? C34 C33 Zr1 74.17(18) . . ? C32 C33 Zr1 72.84(19) . . ? C34 C33 H33 126.3 . . ? C32 C33 H33 126.3 . . ? Zr1 C33 H33 118.7 . . ? C33 C34 C35 108.7(3) . . ? C33 C34 Zr1 73.57(18) . . ? C35 C34 Zr1 72.80(17) . . ? C33 C34 H34 125.7 . . ? C35 C34 H34 125.7 . . ? Zr1 C34 H34 119.8 . . ? C31 C35 C34 107.4(3) . . ? C31 C35 Zr1 73.79(16) . . ? C34 C35 Zr1 74.55(16) . . ? C31 C35 H35 126.3 . . ? C34 C35 H35 126.3 . . ? Zr1 C35 H35 117.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 Zr1 B1 C1 -133.5(3) . . . . ? C32 Zr1 B1 C1 -24.8(4) . . . . ? C35 Zr1 B1 C1 0.4(3) . . . . ? C22 Zr1 B1 C1 -146.7(3) . . . . ? C31 Zr1 B1 C1 9.8(4) . . . . ? C21 Zr1 B1 C1 172.4(3) . . . . ? C25 Zr1 B1 C1 172.7(3) . . . . ? C33 Zr1 B1 C1 -49.3(3) . . . . ? C34 Zr1 B1 C1 -32.2(3) . . . . ? Cl1 Zr1 B1 C1 89.6(3) . . . . ? C24 Zr1 B1 C1 -157.8(3) . . . . ? Zr1 B1 C1 C2 -168.0(2) . . . . ? Zr1 B1 C1 C5 11.8(5) . . . . ? Zr1 B1 C1 Fe1 105.2(3) . . . . ? C11 Fe1 C1 C2 -119.16(18) . . . . ? C14 Fe1 C1 C2 170.6(3) . . . . ? C15 Fe1 C1 C2 -160.79(17) . . . . ? C12 Fe1 C1 C2 -78.3(2) . . . . ? C5 Fe1 C1 C2 117.2(2) . . . . ? C3 Fe1 C1 C2 37.08(17) . . . . ? C13 Fe1 C1 C2 -51.0(4) . . . . ? C4 Fe1 C1 C2 80.48(19) . . . . ? C11 Fe1 C1 C5 123.61(19) . . . . ? C2 Fe1 C1 C5 -117.2(2) . . . . ? C14 Fe1 C1 C5 53.4(4) . . . . ? C15 Fe1 C1 C5 82.0(2) . . . . ? C12 Fe1 C1 C5 164.49(19) . . . . ? C3 Fe1 C1 C5 -80.15(19) . . . . ? C13 Fe1 C1 C5 -168.2(4) . . . . ? C4 Fe1 C1 C5 -36.75(18) . . . . ? C11 Fe1 C1 B1 -3.0(3) . . . . ? C2 Fe1 C1 B1 116.1(3) . . . . ? C14 Fe1 C1 B1 -73.3(4) . . . . ? C15 Fe1 C1 B1 -44.7(3) . . . . ? C12 Fe1 C1 B1 37.8(3) . . . . ? C5 Fe1 C1 B1 -126.7(3) . . . . ? C3 Fe1 C1 B1 153.2(3) . . . . ? C13 Fe1 C1 B1 65.1(5) . . . . ? C4 Fe1 C1 B1 -163.4(3) . . . . ? C5 C1 C2 C3 -0.3(3) . . . . ? B1 C1 C2 C3 179.5(3) . . . . ? Fe1 C1 C2 C3 -59.6(2) . . . . ? C5 C1 C2 Fe1 59.3(2) . . . . ? B1 C1 C2 Fe1 -120.8(3) . . . . ? C11 Fe1 C2 C3 -162.0(2) . . . . ? C14 Fe1 C2 C3 -48.3(4) . . . . ? C15 Fe1 C2 C3 165.3(3) . . . . ? C12 Fe1 C2 C3 -119.9(2) . . . . ? C5 Fe1 C2 C3 81.1(2) . . . . ? C13 Fe1 C2 C3 -79.1(2) . . . . ? C4 Fe1 C2 C3 37.39(19) . . . . ? C1 Fe1 C2 C3 120.2(3) . . . . ? C11 Fe1 C2 C1 77.8(2) . . . . ? C14 Fe1 C2 C1 -168.5(3) . . . . ? C15 Fe1 C2 C1 45.1(4) . . . . ? C12 Fe1 C2 C1 119.87(19) . . . . ? C5 Fe1 C2 C1 -39.07(17) . . . . ? C3 Fe1 C2 C1 -120.2(3) . . . . ? C13 Fe1 C2 C1 160.74(17) . . . . ? C4 Fe1 C2 C1 -82.81(18) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? Fe1 C2 C3 C4 -59.3(2) . . . . ? C1 C2 C3 Fe1 59.8(2) . . . . ? C11 Fe1 C3 C4 161.9(3) . . . . ? C2 Fe1 C3 C4 119.5(3) . . . . ? C14 Fe1 C3 C4 -77.5(2) . . . . ? C15 Fe1 C3 C4 -41.9(5) . . . . ? C12 Fe1 C3 C4 -162.49(19) . . . . ? C5 Fe1 C3 C4 37.72(18) . . . . ? C13 Fe1 C3 C4 -119.66(19) . . . . ? C1 Fe1 C3 C4 82.12(19) . . . . ? C11 Fe1 C3 C2 42.4(4) . . . . ? C14 Fe1 C3 C2 162.94(18) . . . . ? C15 Fe1 C3 C2 -161.4(4) . . . . ? C12 Fe1 C3 C2 78.0(2) . . . . ? C5 Fe1 C3 C2 -81.80(19) . . . . ? C13 Fe1 C3 C2 120.82(19) . . . . ? C4 Fe1 C3 C2 -119.5(3) . . . . ? C1 Fe1 C3 C2 -37.40(18) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? Fe1 C3 C4 C5 -59.2(2) . . . . ? C2 C3 C4 Fe1 58.8(2) . . . . ? C11 Fe1 C4 C3 -158.4(4) . . . . ? C2 Fe1 C4 C3 -37.59(19) . . . . ? C14 Fe1 C4 C3 122.68(19) . . . . ? C15 Fe1 C4 C3 164.99(19) . . . . ? C12 Fe1 C4 C3 43.0(4) . . . . ? C5 Fe1 C4 C3 -119.1(3) . . . . ? C13 Fe1 C4 C3 79.9(2) . . . . ? C1 Fe1 C4 C3 -81.74(19) . . . . ? C11 Fe1 C4 C5 -39.3(5) . . . . ? C2 Fe1 C4 C5 81.51(19) . . . . ? C14 Fe1 C4 C5 -118.23(19) . . . . ? C15 Fe1 C4 C5 -75.9(2) . . . . ? C12 Fe1 C4 C5 162.1(3) . . . . ? C3 Fe1 C4 C5 119.1(3) . . . . ? C13 Fe1 C4 C5 -161.02(18) . . . . ? C1 Fe1 C4 C5 37.36(18) . . . . ? C3 C4 C5 C1 0.2(3) . . . . ? Fe1 C4 C5 C1 -59.1(2) . . . . ? C3 C4 C5 Fe1 59.3(2) . . . . ? C2 C1 C5 C4 0.1(3) . . . . ? B1 C1 C5 C4 -179.8(3) . . . . ? Fe1 C1 C5 C4 59.1(2) . . . . ? C2 C1 C5 Fe1 -59.1(2) . . . . ? B1 C1 C5 Fe1 121.1(3) . . . . ? C11 Fe1 C5 C4 165.38(18) . . . . ? C2 Fe1 C5 C4 -81.6(2) . . . . ? C14 Fe1 C5 C4 81.3(2) . . . . ? C15 Fe1 C5 C4 123.11(19) . . . . ? C12 Fe1 C5 C4 -160.9(3) . . . . ? C3 Fe1 C5 C4 -37.66(18) . . . . ? C13 Fe1 C5 C4 48.1(4) . . . . ? C1 Fe1 C5 C4 -120.5(3) . . . . ? C11 Fe1 C5 C1 -74.1(2) . . . . ? C2 Fe1 C5 C1 38.92(18) . . . . ? C14 Fe1 C5 C1 -158.14(18) . . . . ? C15 Fe1 C5 C1 -116.36(19) . . . . ? C12 Fe1 C5 C1 -40.3(4) . . . . ? C3 Fe1 C5 C1 82.87(19) . . . . ? C13 Fe1 C5 C1 168.7(3) . . . . ? C4 Fe1 C5 C1 120.5(3) . . . . ? C2 Fe1 C11 C12 79.9(2) . . . . ? C14 Fe1 C11 C12 -81.7(2) . . . . ? C15 Fe1 C11 C12 -119.4(3) . . . . ? C5 Fe1 C11 C12 162.62(19) . . . . ? C3 Fe1 C11 C12 49.3(4) . . . . ? C13 Fe1 C11 C12 -37.8(2) . . . . ? C4 Fe1 C11 C12 -167.9(3) . . . . ? C1 Fe1 C11 C12 121.6(2) . . . . ? C2 Fe1 C11 C15 -160.7(2) . . . . ? C14 Fe1 C11 C15 37.7(2) . . . . ? C12 Fe1 C11 C15 119.4(3) . . . . ? C5 Fe1 C11 C15 -78.0(2) . . . . ? C3 Fe1 C11 C15 168.7(3) . . . . ? C13 Fe1 C11 C15 81.5(2) . . . . ? C4 Fe1 C11 C15 -48.6(5) . . . . ? C1 Fe1 C11 C15 -119.0(2) . . . . ? C15 C11 C12 C13 -0.1(4) . . . . ? Fe1 C11 C12 C13 59.7(2) . . . . ? C15 C11 C12 Fe1 -59.8(2) . . . . ? C2 Fe1 C12 C11 -117.7(2) . . . . ? C14 Fe1 C12 C11 81.4(2) . . . . ? C15 Fe1 C12 C11 37.8(2) . . . . ? C5 Fe1 C12 C11 -45.4(5) . . . . ? C3 Fe1 C12 C11 -159.33(19) . . . . ? C13 Fe1 C12 C11 118.8(3) . . . . ? C4 Fe1 C12 C11 169.3(3) . . . . ? C1 Fe1 C12 C11 -75.5(2) . . . . ? C11 Fe1 C12 C13 -118.8(3) . . . . ? C2 Fe1 C12 C13 123.5(2) . . . . ? C14 Fe1 C12 C13 -37.4(2) . . . . ? C15 Fe1 C12 C13 -81.0(2) . . . . ? C5 Fe1 C12 C13 -164.2(3) . . . . ? C3 Fe1 C12 C13 81.9(2) . . . . ? C4 Fe1 C12 C13 50.4(4) . . . . ? C1 Fe1 C12 C13 165.65(19) . . . . ? C11 C12 C13 C14 -0.3(4) . . . . ? Fe1 C12 C13 C14 58.8(2) . . . . ? C11 C12 C13 Fe1 -59.1(2) . . . . ? C11 Fe1 C13 C12 38.0(2) . . . . ? C2 Fe1 C13 C12 -74.8(2) . . . . ? C14 Fe1 C13 C12 119.7(3) . . . . ? C15 Fe1 C13 C12 82.3(2) . . . . ? C5 Fe1 C13 C12 164.8(3) . . . . ? C3 Fe1 C13 C12 -117.4(2) . . . . ? C4 Fe1 C13 C12 -159.8(2) . . . . ? C1 Fe1 C13 C12 -36.8(5) . . . . ? C11 Fe1 C13 C14 -81.7(2) . . . . ? C2 Fe1 C13 C14 165.45(18) . . . . ? C15 Fe1 C13 C14 -37.45(19) . . . . ? C12 Fe1 C13 C14 -119.7(3) . . . . ? C5 Fe1 C13 C14 45.1(5) . . . . ? C3 Fe1 C13 C14 122.9(2) . . . . ? C4 Fe1 C13 C14 80.5(2) . . . . ? C1 Fe1 C13 C14 -156.5(3) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? Fe1 C13 C14 C15 59.5(2) . . . . ? C12 C13 C14 Fe1 -58.9(2) . . . . ? C11 Fe1 C14 C15 -38.15(19) . . . . ? C2 Fe1 C14 C15 -160.0(3) . . . . ? C12 Fe1 C14 C15 -82.1(2) . . . . ? C5 Fe1 C14 C15 78.4(2) . . . . ? C3 Fe1 C14 C15 163.33(18) . . . . ? C13 Fe1 C14 C15 -119.4(3) . . . . ? C4 Fe1 C14 C15 121.24(18) . . . . ? C1 Fe1 C14 C15 39.6(4) . . . . ? C11 Fe1 C14 C13 81.3(2) . . . . ? C2 Fe1 C14 C13 -40.6(4) . . . . ? C15 Fe1 C14 C13 119.4(3) . . . . ? C12 Fe1 C14 C13 37.3(2) . . . . ? C5 Fe1 C14 C13 -162.13(19) . . . . ? C3 Fe1 C14 C13 -77.2(2) . . . . ? C4 Fe1 C14 C13 -119.3(2) . . . . ? C1 Fe1 C14 C13 159.0(3) . . . . ? C13 C14 C15 C11 -0.6(4) . . . . ? Fe1 C14 C15 C11 58.9(2) . . . . ? C13 C14 C15 Fe1 -59.6(2) . . . . ? C12 C11 C15 C14 0.5(4) . . . . ? Fe1 C11 C15 C14 -59.4(2) . . . . ? C12 C11 C15 Fe1 59.9(2) . . . . ? C11 Fe1 C15 C14 118.9(3) . . . . ? C2 Fe1 C15 C14 164.1(3) . . . . ? C12 Fe1 C15 C14 81.3(2) . . . . ? C5 Fe1 C15 C14 -120.10(18) . . . . ? C3 Fe1 C15 C14 -47.0(5) . . . . ? C13 Fe1 C15 C14 37.60(18) . . . . ? C4 Fe1 C15 C14 -78.8(2) . . . . ? C1 Fe1 C15 C14 -163.25(17) . . . . ? C2 Fe1 C15 C11 45.3(4) . . . . ? C14 Fe1 C15 C11 -118.9(3) . . . . ? C12 Fe1 C15 C11 -37.6(2) . . . . ? C5 Fe1 C15 C11 121.0(2) . . . . ? C3 Fe1 C15 C11 -165.9(4) . . . . ? C13 Fe1 C15 C11 -81.3(2) . . . . ? C4 Fe1 C15 C11 162.3(2) . . . . ? C1 Fe1 C15 C11 77.9(2) . . . . ? C23 Zr1 C21 C22 37.0(2) . . . . ? C32 Zr1 C21 C22 -53.0(2) . . . . ? C35 Zr1 C21 C22 -79.9(3) . . . . ? C31 Zr1 C21 C22 -81.8(2) . . . . ? C25 Zr1 C21 C22 114.6(3) . . . . ? C33 Zr1 C21 C22 -22.5(2) . . . . ? C34 Zr1 C21 C22 -20.1(3) . . . . ? Cl1 Zr1 C21 C22 -151.9(2) . . . . ? C24 Zr1 C21 C22 77.8(2) . . . . ? B1 Zr1 C21 C22 115.0(2) . . . . ? C23 Zr1 C21 C25 -77.5(2) . . . . ? C32 Zr1 C21 C25 -167.5(2) . . . . ? C35 Zr1 C21 C25 165.5(2) . . . . ? C22 Zr1 C21 C25 -114.6(3) . . . . ? C31 Zr1 C21 C25 163.6(2) . . . . ? C33 Zr1 C21 C25 -137.1(2) . . . . ? C34 Zr1 C21 C25 -134.6(2) . . . . ? Cl1 Zr1 C21 C25 93.6(2) . . . . ? C24 Zr1 C21 C25 -36.75(19) . . . . ? B1 Zr1 C21 C25 0.4(3) . . . . ? C25 C21 C22 C23 1.1(3) . . . . ? Zr1 C21 C22 C23 -65.4(2) . . . . ? C25 C21 C22 Zr1 66.4(2) . . . . ? C23 Zr1 C22 C21 -115.7(3) . . . . ? C32 Zr1 C22 C21 126.0(2) . . . . ? C35 Zr1 C22 C21 135.1(2) . . . . ? C31 Zr1 C22 C21 110.3(2) . . . . ? C25 Zr1 C22 C21 -37.37(19) . . . . ? C33 Zr1 C22 C21 159.0(2) . . . . ? C34 Zr1 C22 C21 167.42(19) . . . . ? Cl1 Zr1 C22 C21 29.1(2) . . . . ? C24 Zr1 C22 C21 -77.7(2) . . . . ? B1 Zr1 C22 C21 -91.2(3) . . . . ? C32 Zr1 C22 C23 -118.3(2) . . . . ? C35 Zr1 C22 C23 -109.3(2) . . . . ? C31 Zr1 C22 C23 -134.0(2) . . . . ? C21 Zr1 C22 C23 115.7(3) . . . . ? C25 Zr1 C22 C23 78.3(2) . . . . ? C33 Zr1 C22 C23 -85.3(2) . . . . ? C34 Zr1 C22 C23 -76.9(2) . . . . ? Cl1 Zr1 C22 C23 144.77(19) . . . . ? C24 Zr1 C22 C23 37.98(19) . . . . ? B1 Zr1 C22 C23 24.5(3) . . . . ? C21 C22 C23 C24 -2.2(3) . . . . ? Zr1 C22 C23 C24 -68.4(2) . . . . ? C21 C22 C23 Zr1 66.2(2) . . . . ? C32 Zr1 C23 C22 59.7(2) . . . . ? C35 Zr1 C23 C22 102.1(2) . . . . ? C31 Zr1 C23 C22 59.6(3) . . . . ? C21 Zr1 C23 C22 -36.4(2) . . . . ? C25 Zr1 C23 C22 -76.8(2) . . . . ? C33 Zr1 C23 C22 89.5(2) . . . . ? C34 Zr1 C23 C22 113.4(2) . . . . ? Cl1 Zr1 C23 C22 -48.3(2) . . . . ? C24 Zr1 C23 C22 -113.4(3) . . . . ? B1 Zr1 C23 C22 -161.8(2) . . . . ? C32 Zr1 C23 C24 173.0(2) . . . . ? C35 Zr1 C23 C24 -144.57(19) . . . . ? C22 Zr1 C23 C24 113.4(3) . . . . ? C31 Zr1 C23 C24 172.93(19) . . . . ? C21 Zr1 C23 C24 76.9(2) . . . . ? C25 Zr1 C23 C24 36.55(19) . . . . ? C33 Zr1 C23 C24 -157.2(2) . . . . ? C34 Zr1 C23 C24 -133.2(2) . . . . ? Cl1 Zr1 C23 C24 65.0(2) . . . . ? B1 Zr1 C23 C24 -48.4(2) . . . . ? C22 C23 C24 C25 2.5(3) . . . . ? Zr1 C23 C24 C25 -65.3(2) . . . . ? C22 C23 C24 Zr1 67.7(2) . . . . ? C23 Zr1 C24 C25 115.5(3) . . . . ? C32 Zr1 C24 C25 106.8(2) . . . . ? C35 Zr1 C24 C25 -170.8(2) . . . . ? C22 Zr1 C24 C25 77.4(2) . . . . ? C31 Zr1 C24 C25 99.4(4) . . . . ? C21 Zr1 C24 C25 37.0(2) . . . . ? C33 Zr1 C24 C25 139.7(2) . . . . ? C34 Zr1 C24 C25 173.40(19) . . . . ? Cl1 Zr1 C24 C25 -17.8(2) . . . . ? B1 Zr1 C24 C25 -112.8(2) . . . . ? C32 Zr1 C24 C23 -8.7(3) . . . . ? C35 Zr1 C24 C23 73.8(3) . . . . ? C22 Zr1 C24 C23 -38.1(2) . . . . ? C31 Zr1 C24 C23 -16.0(4) . . . . ? C21 Zr1 C24 C23 -78.4(2) . . . . ? C25 Zr1 C24 C23 -115.5(3) . . . . ? C33 Zr1 C24 C23 24.2(2) . . . . ? C34 Zr1 C24 C23 58.0(2) . . . . ? Cl1 Zr1 C24 C23 -133.2(2) . . . . ? B1 Zr1 C24 C23 131.8(2) . . . . ? C23 C24 C25 C21 -1.8(3) . . . . ? Zr1 C24 C25 C21 -66.3(2) . . . . ? C23 C24 C25 Zr1 64.5(2) . . . . ? C22 C21 C25 C24 0.5(3) . . . . ? Zr1 C21 C25 C24 66.7(2) . . . . ? C22 C21 C25 Zr1 -66.2(2) . . . . ? C23 Zr1 C25 C24 -37.1(2) . . . . ? C32 Zr1 C25 C24 -99.3(2) . . . . ? C22 Zr1 C25 C24 -78.1(2) . . . . ? C31 Zr1 C25 C24 -142.0(2) . . . . ? C21 Zr1 C25 C24 -115.3(3) . . . . ? C33 Zr1 C25 C24 -55.7(3) . . . . ? C34 Zr1 C25 C24 -13.1(4) . . . . ? Cl1 Zr1 C25 C24 163.6(2) . . . . ? B1 Zr1 C25 C24 65.1(2) . . . . ? C23 Zr1 C25 C21 78.2(2) . . . . ? C32 Zr1 C25 C21 16.0(3) . . . . ? C22 Zr1 C25 C21 37.2(2) . . . . ? C31 Zr1 C25 C21 -26.7(3) . . . . ? C33 Zr1 C25 C21 59.5(3) . . . . ? C34 Zr1 C25 C21 102.2(3) . . . . ? Cl1 Zr1 C25 C21 -81.1(2) . . . . ? C24 Zr1 C25 C21 115.3(3) . . . . ? B1 Zr1 C25 C21 -179.6(2) . . . . ? C23 Zr1 C31 C32 0.2(3) . . . . ? C35 Zr1 C31 C32 -115.2(3) . . . . ? C22 Zr1 C31 C32 29.4(3) . . . . ? C21 Zr1 C31 C32 62.9(3) . . . . ? C25 Zr1 C31 C32 78.3(3) . . . . ? C33 Zr1 C31 C32 -37.2(2) . . . . ? C34 Zr1 C31 C32 -77.4(2) . . . . ? Cl1 Zr1 C31 C32 134.2(2) . . . . ? C24 Zr1 C31 C32 11.0(4) . . . . ? B1 Zr1 C31 C32 -132.6(2) . . . . ? C23 Zr1 C31 C35 115.4(2) . . . . ? C32 Zr1 C31 C35 115.2(3) . . . . ? C22 Zr1 C31 C35 144.6(2) . . . . ? C21 Zr1 C31 C35 178.1(2) . . . . ? C25 Zr1 C31 C35 -166.5(2) . . . . ? C33 Zr1 C31 C35 77.9(2) . . . . ? C34 Zr1 C31 C35 37.7(2) . . . . ? Cl1 Zr1 C31 C35 -110.6(2) . . . . ? C24 Zr1 C31 C35 126.1(3) . . . . ? B1 Zr1 C31 C35 -17.5(3) . . . . ? C35 C31 C32 C33 1.3(3) . . . . ? Zr1 C31 C32 C33 67.1(2) . . . . ? C35 C31 C32 Zr1 -65.8(2) . . . . ? C23 Zr1 C32 C31 -179.8(2) . . . . ? C35 Zr1 C32 C31 37.2(2) . . . . ? C22 Zr1 C32 C31 -151.2(3) . . . . ? C21 Zr1 C32 C31 -125.3(2) . . . . ? C25 Zr1 C32 C31 -133.9(2) . . . . ? C33 Zr1 C32 C31 115.0(3) . . . . ? C34 Zr1 C32 C31 77.9(2) . . . . ? Cl1 Zr1 C32 C31 -45.2(2) . . . . ? C24 Zr1 C32 C31 -175.1(2) . . . . ? B1 Zr1 C32 C31 68.8(3) . . . . ? C23 Zr1 C32 C33 65.2(2) . . . . ? C35 Zr1 C32 C33 -77.8(2) . . . . ? C22 Zr1 C32 C33 93.8(2) . . . . ? C31 Zr1 C32 C33 -115.0(3) . . . . ? C21 Zr1 C32 C33 119.7(2) . . . . ? C25 Zr1 C32 C33 111.1(2) . . . . ? C34 Zr1 C32 C33 -37.11(19) . . . . ? Cl1 Zr1 C32 C33 -160.13(18) . . . . ? C24 Zr1 C32 C33 69.9(2) . . . . ? B1 Zr1 C32 C33 -46.2(3) . . . . ? C31 C32 C33 C34 -0.2(3) . . . . ? Zr1 C32 C33 C34 66.7(2) . . . . ? C31 C32 C33 Zr1 -66.9(2) . . . . ? C23 Zr1 C33 C34 132.1(2) . . . . ? C32 Zr1 C33 C34 -114.4(3) . . . . ? C35 Zr1 C33 C34 -36.67(19) . . . . ? C22 Zr1 C33 C34 165.3(2) . . . . ? C31 Zr1 C33 C34 -77.4(2) . . . . ? C21 Zr1 C33 C34 177.29(19) . . . . ? C25 Zr1 C33 C34 147.3(2) . . . . ? Cl1 Zr1 C33 C34 -88.3(2) . . . . ? C24 Zr1 C33 C34 119.1(2) . . . . ? B1 Zr1 C33 C34 33.3(2) . . . . ? C23 Zr1 C33 C32 -113.5(2) . . . . ? C35 Zr1 C33 C32 77.7(2) . . . . ? C22 Zr1 C33 C32 -80.3(2) . . . . ? C31 Zr1 C33 C32 37.00(19) . . . . ? C21 Zr1 C33 C32 -68.3(2) . . . . ? C25 Zr1 C33 C32 -98.3(2) . . . . ? C34 Zr1 C33 C32 114.4(3) . . . . ? Cl1 Zr1 C33 C32 26.1(2) . . . . ? C24 Zr1 C33 C32 -126.48(19) . . . . ? B1 Zr1 C33 C32 147.68(19) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? Zr1 C33 C34 C35 64.8(2) . . . . ? C32 C33 C34 Zr1 -65.8(2) . . . . ? C23 Zr1 C34 C33 -48.6(2) . . . . ? C32 Zr1 C34 C33 37.7(2) . . . . ? C35 Zr1 C34 C33 116.2(3) . . . . ? C22 Zr1 C34 C33 -15.8(2) . . . . ? C31 Zr1 C34 C33 78.3(2) . . . . ? C21 Zr1 C34 C33 -4.3(3) . . . . ? C25 Zr1 C34 C33 -68.3(3) . . . . ? Cl1 Zr1 C34 C33 115.6(2) . . . . ? C24 Zr1 C34 C33 -76.6(2) . . . . ? B1 Zr1 C34 C33 -148.7(2) . . . . ? C23 Zr1 C34 C35 -164.7(2) . . . . ? C32 Zr1 C34 C35 -78.5(2) . . . . ? C22 Zr1 C34 C35 -132.0(2) . . . . ? C31 Zr1 C34 C35 -37.9(2) . . . . ? C21 Zr1 C34 C35 -120.5(2) . . . . ? C25 Zr1 C34 C35 175.5(2) . . . . ? C33 Zr1 C34 C35 -116.2(3) . . . . ? Cl1 Zr1 C34 C35 -0.6(2) . . . . ? C24 Zr1 C34 C35 167.26(18) . . . . ? B1 Zr1 C34 C35 95.2(2) . . . . ? C32 C31 C35 C34 -1.8(3) . . . . ? Zr1 C31 C35 C34 -67.6(2) . . . . ? C32 C31 C35 Zr1 65.7(2) . . . . ? C33 C34 C35 C31 1.7(3) . . . . ? Zr1 C34 C35 C31 67.1(2) . . . . ? C33 C34 C35 Zr1 -65.3(2) . . . . ? C23 Zr1 C35 C31 -92.9(3) . . . . ? C32 Zr1 C35 C31 -36.9(2) . . . . ? C22 Zr1 C35 C31 -47.9(3) . . . . ? C21 Zr1 C35 C31 -3.2(3) . . . . ? C33 Zr1 C35 C31 -77.5(2) . . . . ? C34 Zr1 C35 C31 -113.7(3) . . . . ? Cl1 Zr1 C35 C31 65.8(2) . . . . ? C24 Zr1 C35 C31 -138.8(3) . . . . ? B1 Zr1 C35 C31 164.6(2) . . . . ? C23 Zr1 C35 C34 20.8(3) . . . . ? C32 Zr1 C35 C34 76.9(2) . . . . ? C22 Zr1 C35 C34 65.9(3) . . . . ? C31 Zr1 C35 C34 113.7(3) . . . . ? C21 Zr1 C35 C34 110.5(3) . . . . ? C33 Zr1 C35 C34 36.2(2) . . . . ? Cl1 Zr1 C35 C34 179.51(19) . . . . ? C24 Zr1 C35 C34 -25.1(4) . . . . ? B1 Zr1 C35 C34 -81.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.587 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.095 data_wa1193 _database_code_depnum_ccdc_archive 'CCDC 894220' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 B Fe Zr' _chemical_formula_sum 'C20 H23 B Fe Zr' _chemical_formula_weight 421.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8828(5) _cell_length_b 12.3274(8) _cell_length_c 17.7040(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.903(6) _cell_angle_gamma 90.00 _cell_volume 1711.25(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7145 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 2.61 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7502 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 14384 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.60 _reflns_number_total 3212 _reflns_number_gt 2215 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3212 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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 0.43182(9) 0.75765(5) 0.50505(4) 0.02152(18) Uani 1 1 d . . . Zr1 Zr 0.09041(6) 0.51438(3) 0.26782(3) 0.01816(13) Uani 1 1 d . . . H1 H 0.002(7) 0.600(4) 0.205(3) 0.023(13) Uiso 1 1 d . . . B1 B 0.2997(7) 0.6554(4) 0.3334(3) 0.0237(12) Uani 1 1 d . . . H1A H 0.179(6) 0.672(3) 0.283(3) 0.015(12) Uiso 1 1 d . . . H1B H 0.284(10) 0.567(6) 0.352(4) 0.07(2) Uiso 1 1 d . . . H1C H 0.430(7) 0.666(4) 0.300(3) 0.025(14) Uiso 1 1 d . . . C1 C 0.2803(6) 0.7340(4) 0.4034(3) 0.0232(11) Uani 1 1 d . . . C2 C 0.3472(7) 0.8423(4) 0.4103(3) 0.0242(11) Uani 1 1 d . . . H2A H 0.4218 0.8767 0.3746 0.029 Uiso 1 1 calc R . . C3 C 0.2920(7) 0.8929(4) 0.4749(3) 0.0254(12) Uani 1 1 d . . . H3A H 0.3199 0.9686 0.4923 0.030 Uiso 1 1 calc R . . C4 C 0.1929(7) 0.8166(4) 0.5120(3) 0.0278(12) Uani 1 1 d . . . H4A H 0.1372 0.8291 0.5595 0.033 Uiso 1 1 calc R . . C5 C 0.1842(6) 0.7191(4) 0.4670(3) 0.0239(11) Uani 1 1 d . . . H5A H 0.1241 0.6509 0.4792 0.029 Uiso 1 1 calc R . . C11 C 0.6236(8) 0.6473(5) 0.5107(4) 0.0398(15) Uani 1 1 d . . . H11A H 0.6423 0.5920 0.4710 0.048 Uiso 1 1 calc R . . C12 C 0.6934(8) 0.7549(5) 0.5152(4) 0.0436(15) Uani 1 1 d . . . H12A H 0.7687 0.7884 0.4794 0.052 Uiso 1 1 calc R . . C13 C 0.6351(8) 0.8047(5) 0.5791(3) 0.0347(14) Uani 1 1 d . . . H13A H 0.6608 0.8808 0.5962 0.042 Uiso 1 1 calc R . . C14 C 0.5306(7) 0.7305(4) 0.6146(3) 0.0334(13) Uani 1 1 d . . . H14A H 0.4724 0.7438 0.6613 0.040 Uiso 1 1 calc R . . C15 C 0.5268(8) 0.6324(4) 0.5713(4) 0.0375(15) Uani 1 1 d . . . H15A H 0.4636 0.5649 0.5824 0.045 Uiso 1 1 calc R . . C21 C 0.2946(6) 0.5047(4) 0.1695(3) 0.0264(11) Uani 1 1 d . . . H21A H 0.3620 0.5668 0.1517 0.032 Uiso 1 1 calc R . . C22 C 0.3514(6) 0.4303(4) 0.2256(3) 0.0242(11) Uani 1 1 d . . . H22A H 0.4668 0.4304 0.2549 0.029 Uiso 1 1 calc R . . C23 C 0.2287(7) 0.3471(4) 0.2269(3) 0.0251(11) Uani 1 1 d . . . H23A H 0.2431 0.2780 0.2564 0.030 Uiso 1 1 calc R . . C24 C 0.0961(7) 0.3707(4) 0.1699(3) 0.0277(12) Uani 1 1 d . . . H24A H -0.0008 0.3211 0.1529 0.033 Uiso 1 1 calc R . . C25 C 0.1349(7) 0.4666(4) 0.1338(3) 0.0285(12) Uani 1 1 d . . . H25A H 0.0709 0.4975 0.0870 0.034 Uiso 1 1 calc R . . C31 C -0.0508(7) 0.3830(4) 0.3463(3) 0.0284(12) Uani 1 1 d . . . H31A H -0.0126 0.3067 0.3574 0.034 Uiso 1 1 calc R . . C32 C -0.1732(7) 0.4150(4) 0.2879(3) 0.0295(13) Uani 1 1 d . . . H32A H -0.2365 0.3653 0.2504 0.035 Uiso 1 1 calc R . . C33 C -0.2109(7) 0.5255(4) 0.2979(3) 0.0309(12) Uani 1 1 d . . . H33A H -0.3046 0.5673 0.2686 0.037 Uiso 1 1 calc R . . C34 C -0.1095(7) 0.5620(4) 0.3637(3) 0.0299(12) Uani 1 1 d . . . H34A H -0.1184 0.6343 0.3885 0.036 Uiso 1 1 calc R . . C35 C -0.0108(7) 0.4736(4) 0.3938(3) 0.0312(12) Uani 1 1 d . . . H35A H 0.0614 0.4725 0.4436 0.037 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 0.0222(4) 0.0218(4) 0.0197(4) 0.0010(3) -0.0021(3) -0.0007(3) Zr1 0.0165(2) 0.0187(2) 0.0191(2) 0.0006(2) 0.00096(16) -0.0012(2) B1 0.023(3) 0.024(3) 0.023(3) 0.002(2) -0.001(2) -0.001(2) C1 0.023(3) 0.026(2) 0.020(3) -0.001(2) -0.001(2) 0.001(2) C2 0.025(3) 0.025(2) 0.021(3) 0.005(2) -0.002(2) -0.001(2) C3 0.032(3) 0.019(2) 0.024(3) 0.001(2) -0.004(2) 0.000(2) C4 0.024(3) 0.035(3) 0.024(3) -0.002(2) 0.000(2) 0.006(2) C5 0.022(3) 0.026(2) 0.022(3) 0.000(2) -0.005(2) -0.0058(19) C11 0.034(3) 0.035(3) 0.049(4) -0.004(3) -0.007(3) 0.010(2) C12 0.026(3) 0.055(4) 0.049(4) 0.003(3) 0.000(3) 0.007(3) C13 0.035(3) 0.035(3) 0.032(3) 0.005(2) -0.009(3) 0.001(2) C14 0.038(3) 0.033(3) 0.026(3) 0.005(2) -0.007(2) 0.005(2) C15 0.045(4) 0.029(3) 0.036(4) 0.011(2) -0.009(3) 0.006(2) C21 0.029(3) 0.031(3) 0.023(3) -0.001(2) 0.018(2) -0.006(2) C22 0.017(3) 0.030(2) 0.026(3) -0.007(2) 0.007(2) 0.0017(19) C23 0.026(3) 0.021(2) 0.029(3) -0.003(2) 0.005(2) 0.0015(19) C24 0.031(3) 0.028(2) 0.024(3) -0.004(2) -0.002(2) -0.006(2) C25 0.033(3) 0.035(3) 0.018(3) -0.002(2) 0.000(2) 0.000(2) C31 0.031(3) 0.023(2) 0.033(3) 0.006(2) 0.014(2) 0.000(2) C32 0.019(3) 0.031(3) 0.040(4) -0.004(2) 0.012(2) -0.014(2) C33 0.019(2) 0.036(3) 0.039(3) -0.002(3) 0.007(2) -0.002(2) C34 0.023(3) 0.026(2) 0.042(4) -0.008(2) 0.013(3) -0.002(2) C35 0.033(3) 0.040(3) 0.023(3) 0.003(2) 0.009(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C11 2.029(6) . ? Fe1 C2 2.029(5) . ? Fe1 C4 2.034(5) . ? Fe1 C15 2.035(5) . ? Fe1 C3 2.039(5) . ? Fe1 C14 2.042(5) . ? Fe1 C13 2.048(6) . ? Fe1 C12 2.052(6) . ? Fe1 C5 2.054(5) . ? Fe1 C1 2.076(5) . ? Zr1 C32 2.469(5) . ? Zr1 C31 2.473(5) . ? Zr1 C23 2.475(5) . ? Zr1 C24 2.482(5) . ? Zr1 C22 2.487(5) . ? Zr1 C33 2.491(5) . ? Zr1 C21 2.493(5) . ? Zr1 C35 2.496(5) . ? Zr1 C34 2.502(6) . ? Zr1 C25 2.505(5) . ? Zr1 B1 2.588(5) . ? Zr1 H1 1.64(5) . ? Zr1 H1A 2.08(4) . ? Zr1 H1B 2.12(7) . ? B1 C1 1.593(8) . ? B1 H1A 1.25(5) . ? B1 H1B 1.14(7) . ? B1 H1C 1.24(6) . ? C1 C5 1.431(7) . ? C1 C2 1.436(7) . ? C2 C3 1.410(8) . ? C2 H2A 1.0000 . ? C3 C4 1.426(8) . ? C3 H3A 1.0000 . ? C4 C5 1.440(7) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C11 C15 1.392(10) . ? C11 C12 1.436(9) . ? C11 H11A 1.0000 . ? C12 C13 1.406(9) . ? C12 H12A 1.0000 . ? C13 C14 1.420(8) . ? C13 H13A 1.0000 . ? C14 C15 1.430(8) . ? C14 H14A 1.0000 . ? C15 H15A 1.0000 . ? C21 C22 1.392(7) . ? C21 C25 1.429(7) . ? C21 H21A 1.0000 . ? C22 C23 1.412(7) . ? C22 H22A 1.0000 . ? C23 C24 1.406(7) . ? C23 H23A 1.0000 . ? C24 C25 1.393(7) . ? C24 H24A 1.0000 . ? C25 H25A 1.0000 . ? C31 C32 1.397(8) . ? C31 C35 1.414(8) . ? C31 H31A 1.0000 . ? C32 C33 1.409(8) . ? C32 H32A 1.0000 . ? C33 C34 1.417(8) . ? C33 H33A 1.0000 . ? C34 C35 1.411(8) . ? C34 H34A 1.0000 . ? C35 H35A 1.0000 . ? 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 C11 Fe1 C2 124.4(3) . . ? C11 Fe1 C4 157.9(2) . . ? C2 Fe1 C4 68.8(2) . . ? C11 Fe1 C15 40.1(3) . . ? C2 Fe1 C15 159.6(2) . . ? C4 Fe1 C15 121.6(3) . . ? C11 Fe1 C3 160.2(3) . . ? C2 Fe1 C3 40.6(2) . . ? C4 Fe1 C3 41.0(2) . . ? C15 Fe1 C3 158.2(3) . . ? C11 Fe1 C14 68.5(3) . . ? C2 Fe1 C14 158.5(2) . . ? C4 Fe1 C14 105.4(2) . . ? C15 Fe1 C14 41.1(2) . . ? C3 Fe1 C14 121.7(2) . . ? C11 Fe1 C13 68.2(2) . . ? C2 Fe1 C13 123.6(2) . . ? C4 Fe1 C13 121.9(2) . . ? C15 Fe1 C13 68.2(2) . . ? C3 Fe1 C13 107.6(2) . . ? C14 Fe1 C13 40.6(2) . . ? C11 Fe1 C12 41.2(3) . . ? C2 Fe1 C12 108.8(2) . . ? C4 Fe1 C12 158.3(2) . . ? C15 Fe1 C12 68.3(3) . . ? C3 Fe1 C12 123.2(2) . . ? C14 Fe1 C12 68.4(3) . . ? C13 Fe1 C12 40.1(3) . . ? C11 Fe1 C5 122.6(2) . . ? C2 Fe1 C5 68.1(2) . . ? C4 Fe1 C5 41.2(2) . . ? C15 Fe1 C5 107.1(2) . . ? C3 Fe1 C5 68.5(2) . . ? C14 Fe1 C5 122.0(2) . . ? C13 Fe1 C5 158.5(2) . . ? C12 Fe1 C5 159.6(2) . . ? C11 Fe1 C1 107.9(2) . . ? C2 Fe1 C1 40.95(19) . . ? C4 Fe1 C1 69.4(2) . . ? C15 Fe1 C1 122.6(2) . . ? C3 Fe1 C1 68.94(19) . . ? C14 Fe1 C1 158.4(2) . . ? C13 Fe1 C1 159.7(2) . . ? C12 Fe1 C1 123.9(2) . . ? C5 Fe1 C1 40.6(2) . . ? C32 Zr1 C31 32.83(18) . . ? C32 Zr1 C23 91.81(18) . . ? C31 Zr1 C23 81.73(18) . . ? C32 Zr1 C24 79.79(19) . . ? C31 Zr1 C24 88.09(18) . . ? C23 Zr1 C24 32.96(17) . . ? C32 Zr1 C22 124.85(17) . . ? C31 Zr1 C22 109.30(17) . . ? C23 Zr1 C22 33.06(16) . . ? C24 Zr1 C22 54.37(17) . . ? C32 Zr1 C33 33.01(18) . . ? C31 Zr1 C33 54.67(18) . . ? C23 Zr1 C33 124.53(17) . . ? C24 Zr1 C33 105.95(18) . . ? C22 Zr1 C33 157.53(16) . . ? C32 Zr1 C21 133.67(18) . . ? C31 Zr1 C21 136.21(17) . . ? C23 Zr1 C21 54.58(17) . . ? C24 Zr1 C21 54.45(17) . . ? C22 Zr1 C21 32.46(17) . . ? C33 Zr1 C21 148.25(18) . . ? C32 Zr1 C35 54.54(19) . . ? C31 Zr1 C35 33.05(18) . . ? C23 Zr1 C35 106.53(18) . . ? C24 Zr1 C35 120.71(18) . . ? C22 Zr1 C35 122.37(18) . . ? C33 Zr1 C35 54.59(19) . . ? C21 Zr1 C35 154.61(17) . . ? C32 Zr1 C34 54.57(18) . . ? C31 Zr1 C34 54.60(17) . . ? C23 Zr1 C34 136.14(18) . . ? C24 Zr1 C34 134.36(18) . . ? C22 Zr1 C34 154.20(18) . . ? C33 Zr1 C34 32.97(18) . . ? C21 Zr1 C34 169.17(17) . . ? C35 Zr1 C34 32.80(18) . . ? C32 Zr1 C25 102.83(19) . . ? C31 Zr1 C25 119.58(17) . . ? C23 Zr1 C25 54.41(17) . . ? C24 Zr1 C25 32.44(17) . . ? C22 Zr1 C25 54.27(17) . . ? C33 Zr1 C25 116.42(18) . . ? C21 Zr1 C25 33.22(17) . . ? C35 Zr1 C25 152.63(17) . . ? C34 Zr1 C25 149.02(19) . . ? C32 Zr1 B1 140.9(2) . . ? C31 Zr1 B1 119.41(19) . . ? C23 Zr1 B1 114.28(18) . . ? C24 Zr1 B1 137.4(2) . . ? C22 Zr1 B1 84.59(18) . . ? C33 Zr1 B1 116.43(19) . . ? C21 Zr1 B1 85.28(18) . . ? C35 Zr1 B1 88.99(19) . . ? C34 Zr1 B1 87.43(19) . . ? C25 Zr1 B1 115.97(19) . . ? C32 Zr1 H1 96.6(19) . . ? C31 Zr1 H1 128.4(19) . . ? C23 Zr1 H1 120.5(19) . . ? C24 Zr1 H1 91.3(18) . . ? C22 Zr1 H1 112(2) . . ? C33 Zr1 H1 76(2) . . ? C21 Zr1 H1 79(2) . . ? C35 Zr1 H1 126(2) . . ? C34 Zr1 H1 93(2) . . ? C25 Zr1 H1 66.3(19) . . ? B1 Zr1 H1 94.4(17) . . ? C32 Zr1 H1A 136.2(14) . . ? C31 Zr1 H1A 134.8(14) . . ? C23 Zr1 H1A 131.9(14) . . ? C24 Zr1 H1A 136.9(14) . . ? C22 Zr1 H1A 98.8(14) . . ? C33 Zr1 H1A 103.6(14) . . ? C21 Zr1 H1A 84.5(14) . . ? C35 Zr1 H1A 101.9(14) . . ? C34 Zr1 H1A 85.3(14) . . ? C25 Zr1 H1A 105.5(14) . . ? B1 Zr1 H1A 28.5(13) . . ? H1 Zr1 H1A 66(2) . . ? C32 Zr1 H1B 127(2) . . ? C31 Zr1 H1B 98(2) . . ? C23 Zr1 H1B 99(2) . . ? C24 Zr1 H1B 130(2) . . ? C22 Zr1 H1B 77(2) . . ? C33 Zr1 H1B 118(2) . . ? C21 Zr1 H1B 92(2) . . ? C35 Zr1 H1B 73(2) . . ? C34 Zr1 H1B 85(2) . . ? C25 Zr1 H1B 125(2) . . ? B1 Zr1 H1B 25.7(19) . . ? H1 Zr1 H1B 120(3) . . ? H1A Zr1 H1B 54(2) . . ? C1 B1 Zr1 130.5(4) . . ? C1 B1 H1A 109(2) . . ? Zr1 B1 H1A 52.4(19) . . ? C1 B1 H1B 110(4) . . ? Zr1 B1 H1B 54(4) . . ? H1A B1 H1B 105(4) . . ? C1 B1 H1C 117(2) . . ? Zr1 B1 H1C 112(2) . . ? H1A B1 H1C 105(3) . . ? H1B B1 H1C 111(5) . . ? C5 C1 C2 105.8(4) . . ? C5 C1 B1 129.4(4) . . ? C2 C1 B1 124.6(5) . . ? C5 C1 Fe1 68.9(3) . . ? C2 C1 Fe1 67.8(3) . . ? B1 C1 Fe1 131.9(3) . . ? C3 C2 C1 109.8(5) . . ? C3 C2 Fe1 70.1(3) . . ? C1 C2 Fe1 71.3(3) . . ? C3 C2 H2A 125.1 . . ? C1 C2 H2A 125.1 . . ? Fe1 C2 H2A 125.1 . . ? C2 C3 C4 108.2(4) . . ? C2 C3 Fe1 69.4(3) . . ? C4 C3 Fe1 69.3(3) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? Fe1 C3 H3A 125.9 . . ? C3 C4 C5 107.0(5) . . ? C3 C4 Fe1 69.7(3) . . ? C5 C4 Fe1 70.1(3) . . ? C3 C4 H4A 126.5 . . ? C5 C4 H4A 126.5 . . ? Fe1 C4 H4A 126.5 . . ? C1 C5 C4 109.3(4) . . ? C1 C5 Fe1 70.5(3) . . ? C4 C5 Fe1 68.6(3) . . ? C1 C5 H5A 125.4 . . ? C4 C5 H5A 125.4 . . ? Fe1 C5 H5A 125.4 . . ? C15 C11 C12 108.4(6) . . ? C15 C11 Fe1 70.2(3) . . ? C12 C11 Fe1 70.2(3) . . ? C15 C11 H11A 125.8 . . ? C12 C11 H11A 125.8 . . ? Fe1 C11 H11A 125.8 . . ? C13 C12 C11 107.0(6) . . ? C13 C12 Fe1 69.8(4) . . ? C11 C12 Fe1 68.6(3) . . ? C13 C12 H12A 126.5 . . ? C11 C12 H12A 126.5 . . ? Fe1 C12 H12A 126.5 . . ? C12 C13 C14 109.1(5) . . ? C12 C13 Fe1 70.1(3) . . ? C14 C13 Fe1 69.5(3) . . ? C12 C13 H13A 125.4 . . ? C14 C13 H13A 125.4 . . ? Fe1 C13 H13A 125.4 . . ? C13 C14 C15 106.8(6) . . ? C13 C14 Fe1 69.9(3) . . ? C15 C14 Fe1 69.2(3) . . ? C13 C14 H14A 126.6 . . ? C15 C14 H14A 126.6 . . ? Fe1 C14 H14A 126.6 . . ? C11 C15 C14 108.6(5) . . ? C11 C15 Fe1 69.8(3) . . ? C14 C15 Fe1 69.8(3) . . ? C11 C15 H15A 125.7 . . ? C14 C15 H15A 125.7 . . ? Fe1 C15 H15A 125.7 . . ? C22 C21 C25 107.7(4) . . ? C22 C21 Zr1 73.5(3) . . ? C25 C21 Zr1 73.9(3) . . ? C22 C21 H21A 125.8 . . ? C25 C21 H21A 125.8 . . ? Zr1 C21 H21A 125.8 . . ? C21 C22 C23 108.6(4) . . ? C21 C22 Zr1 74.0(3) . . ? C23 C22 Zr1 73.0(3) . . ? C21 C22 H22A 125.4 . . ? C23 C22 H22A 125.4 . . ? Zr1 C22 H22A 125.4 . . ? C24 C23 C22 107.3(4) . . ? C24 C23 Zr1 73.8(3) . . ? C22 C23 Zr1 73.9(3) . . ? C24 C23 H23A 125.9 . . ? C22 C23 H23A 125.9 . . ? Zr1 C23 H23A 125.9 . . ? C25 C24 C23 108.8(4) . . ? C25 C24 Zr1 74.7(3) . . ? C23 C24 Zr1 73.3(3) . . ? C25 C24 H24A 125.3 . . ? C23 C24 H24A 125.3 . . ? Zr1 C24 H24A 125.3 . . ? C24 C25 C21 107.5(4) . . ? C24 C25 Zr1 72.9(3) . . ? C21 C25 Zr1 72.9(3) . . ? C24 C25 H25A 126.0 . . ? C21 C25 H25A 126.0 . . ? Zr1 C25 H25A 126.0 . . ? C32 C31 C35 108.1(4) . . ? C32 C31 Zr1 73.4(3) . . ? C35 C31 Zr1 74.4(3) . . ? C32 C31 H31A 125.6 . . ? C35 C31 H31A 125.6 . . ? Zr1 C31 H31A 125.6 . . ? C31 C32 C33 108.7(5) . . ? C31 C32 Zr1 73.7(3) . . ? C33 C32 Zr1 74.3(3) . . ? C31 C32 H32A 125.3 . . ? C33 C32 H32A 125.3 . . ? Zr1 C32 H32A 125.3 . . ? C32 C33 C34 107.5(5) . . ? C32 C33 Zr1 72.6(3) . . ? C34 C33 Zr1 73.9(3) . . ? C32 C33 H33A 126.0 . . ? C34 C33 H33A 126.0 . . ? Zr1 C33 H33A 126.0 . . ? C35 C34 C33 108.0(5) . . ? C35 C34 Zr1 73.4(3) . . ? C33 C34 Zr1 73.1(3) . . ? C35 C34 H34A 125.8 . . ? C33 C34 H34A 125.8 . . ? Zr1 C34 H34A 125.8 . . ? C34 C35 C31 107.8(5) . . ? C34 C35 Zr1 73.8(3) . . ? C31 C35 Zr1 72.6(3) . . ? C34 C35 H35A 125.8 . . ? C31 C35 H35A 125.8 . . ? Zr1 C35 H35A 125.8 . . ? 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 C32 Zr1 B1 C1 -14.6(6) . . . . ? C31 Zr1 B1 C1 -48.0(5) . . . . ? C23 Zr1 B1 C1 -142.2(4) . . . . ? C24 Zr1 B1 C1 -171.8(4) . . . . ? C22 Zr1 B1 C1 -157.1(5) . . . . ? C33 Zr1 B1 C1 14.6(5) . . . . ? C21 Zr1 B1 C1 170.3(5) . . . . ? C35 Zr1 B1 C1 -34.5(4) . . . . ? C34 Zr1 B1 C1 -1.7(4) . . . . ? C25 Zr1 B1 C1 157.2(4) . . . . ? Zr1 B1 C1 C5 29.6(7) . . . . ? Zr1 B1 C1 C2 -143.9(4) . . . . ? Zr1 B1 C1 Fe1 126.0(4) . . . . ? C11 Fe1 C1 C5 119.6(3) . . . . ? C2 Fe1 C1 C5 -118.2(4) . . . . ? C4 Fe1 C1 C5 -37.2(3) . . . . ? C15 Fe1 C1 C5 78.0(4) . . . . ? C3 Fe1 C1 C5 -81.1(3) . . . . ? C14 Fe1 C1 C5 42.8(7) . . . . ? C13 Fe1 C1 C5 -165.0(6) . . . . ? C12 Fe1 C1 C5 162.2(3) . . . . ? C11 Fe1 C1 C2 -122.3(4) . . . . ? C4 Fe1 C1 C2 81.0(3) . . . . ? C15 Fe1 C1 C2 -163.9(4) . . . . ? C3 Fe1 C1 C2 37.0(3) . . . . ? C14 Fe1 C1 C2 160.9(6) . . . . ? C13 Fe1 C1 C2 -46.9(7) . . . . ? C12 Fe1 C1 C2 -79.6(4) . . . . ? C5 Fe1 C1 C2 118.2(4) . . . . ? C11 Fe1 C1 B1 -5.1(5) . . . . ? C2 Fe1 C1 B1 117.2(6) . . . . ? C4 Fe1 C1 B1 -161.8(5) . . . . ? C15 Fe1 C1 B1 -46.7(6) . . . . ? C3 Fe1 C1 B1 154.2(5) . . . . ? C14 Fe1 C1 B1 -81.9(8) . . . . ? C13 Fe1 C1 B1 70.3(8) . . . . ? C12 Fe1 C1 B1 37.6(6) . . . . ? C5 Fe1 C1 B1 -124.7(6) . . . . ? C5 C1 C2 C3 -1.0(5) . . . . ? B1 C1 C2 C3 173.8(4) . . . . ? Fe1 C1 C2 C3 -59.7(3) . . . . ? C5 C1 C2 Fe1 58.7(3) . . . . ? B1 C1 C2 Fe1 -126.5(5) . . . . ? C11 Fe1 C2 C3 -162.5(3) . . . . ? C4 Fe1 C2 C3 37.6(3) . . . . ? C15 Fe1 C2 C3 162.3(7) . . . . ? C14 Fe1 C2 C3 -40.6(8) . . . . ? C13 Fe1 C2 C3 -77.5(4) . . . . ? C12 Fe1 C2 C3 -119.4(3) . . . . ? C5 Fe1 C2 C3 82.1(3) . . . . ? C1 Fe1 C2 C3 120.2(4) . . . . ? C11 Fe1 C2 C1 77.3(4) . . . . ? C4 Fe1 C2 C1 -82.6(3) . . . . ? C15 Fe1 C2 C1 42.1(8) . . . . ? C3 Fe1 C2 C1 -120.2(4) . . . . ? C14 Fe1 C2 C1 -160.8(6) . . . . ? C13 Fe1 C2 C1 162.3(3) . . . . ? C12 Fe1 C2 C1 120.4(3) . . . . ? C5 Fe1 C2 C1 -38.1(3) . . . . ? C1 C2 C3 C4 1.8(6) . . . . ? Fe1 C2 C3 C4 -58.6(3) . . . . ? C1 C2 C3 Fe1 60.4(3) . . . . ? C11 Fe1 C3 C2 47.1(7) . . . . ? C4 Fe1 C3 C2 -119.9(4) . . . . ? C15 Fe1 C3 C2 -163.5(6) . . . . ? C14 Fe1 C3 C2 163.7(3) . . . . ? C13 Fe1 C3 C2 121.4(3) . . . . ? C12 Fe1 C3 C2 80.1(4) . . . . ? C5 Fe1 C3 C2 -81.0(3) . . . . ? C1 Fe1 C3 C2 -37.4(3) . . . . ? C11 Fe1 C3 C4 166.9(6) . . . . ? C2 Fe1 C3 C4 119.9(4) . . . . ? C15 Fe1 C3 C4 -43.6(7) . . . . ? C14 Fe1 C3 C4 -76.4(4) . . . . ? C13 Fe1 C3 C4 -118.7(3) . . . . ? C12 Fe1 C3 C4 -160.0(3) . . . . ? C5 Fe1 C3 C4 38.8(3) . . . . ? C1 Fe1 C3 C4 82.5(3) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? Fe1 C3 C4 C5 -60.5(3) . . . . ? C2 C3 C4 Fe1 58.7(4) . . . . ? C11 Fe1 C4 C3 -168.3(6) . . . . ? C2 Fe1 C4 C3 -37.2(3) . . . . ? C15 Fe1 C4 C3 162.5(3) . . . . ? C14 Fe1 C4 C3 120.9(3) . . . . ? C13 Fe1 C4 C3 80.0(4) . . . . ? C12 Fe1 C4 C3 50.6(8) . . . . ? C5 Fe1 C4 C3 -117.7(4) . . . . ? C1 Fe1 C4 C3 -81.2(3) . . . . ? C11 Fe1 C4 C5 -50.6(7) . . . . ? C2 Fe1 C4 C5 80.5(3) . . . . ? C15 Fe1 C4 C5 -79.8(4) . . . . ? C3 Fe1 C4 C5 117.7(4) . . . . ? C14 Fe1 C4 C5 -121.3(3) . . . . ? C13 Fe1 C4 C5 -162.2(3) . . . . ? C12 Fe1 C4 C5 168.3(6) . . . . ? C1 Fe1 C4 C5 36.6(3) . . . . ? C2 C1 C5 C4 -0.2(5) . . . . ? B1 C1 C5 C4 -174.6(5) . . . . ? Fe1 C1 C5 C4 57.8(3) . . . . ? C2 C1 C5 Fe1 -58.0(3) . . . . ? B1 C1 C5 Fe1 127.6(5) . . . . ? C3 C4 C5 C1 1.3(5) . . . . ? Fe1 C4 C5 C1 -59.0(3) . . . . ? C3 C4 C5 Fe1 60.2(3) . . . . ? C11 Fe1 C5 C1 -79.3(4) . . . . ? C2 Fe1 C5 C1 38.5(3) . . . . ? C4 Fe1 C5 C1 120.9(4) . . . . ? C15 Fe1 C5 C1 -120.4(3) . . . . ? C3 Fe1 C5 C1 82.3(3) . . . . ? C14 Fe1 C5 C1 -162.8(3) . . . . ? C13 Fe1 C5 C1 165.9(5) . . . . ? C12 Fe1 C5 C1 -46.7(8) . . . . ? C11 Fe1 C5 C4 159.8(3) . . . . ? C2 Fe1 C5 C4 -82.4(3) . . . . ? C15 Fe1 C5 C4 118.7(3) . . . . ? C3 Fe1 C5 C4 -38.6(3) . . . . ? C14 Fe1 C5 C4 76.3(4) . . . . ? C13 Fe1 C5 C4 44.9(7) . . . . ? C12 Fe1 C5 C4 -167.6(6) . . . . ? C1 Fe1 C5 C4 -120.9(4) . . . . ? C2 Fe1 C11 C15 -161.8(3) . . . . ? C4 Fe1 C11 C15 -40.3(8) . . . . ? C3 Fe1 C11 C15 162.9(6) . . . . ? C14 Fe1 C11 C15 37.7(4) . . . . ? C13 Fe1 C11 C15 81.6(4) . . . . ? C12 Fe1 C11 C15 119.1(5) . . . . ? C5 Fe1 C11 C15 -77.4(4) . . . . ? C1 Fe1 C11 C15 -119.6(4) . . . . ? C2 Fe1 C11 C12 79.1(4) . . . . ? C4 Fe1 C11 C12 -159.3(6) . . . . ? C15 Fe1 C11 C12 -119.1(5) . . . . ? C3 Fe1 C11 C12 43.8(8) . . . . ? C14 Fe1 C11 C12 -81.4(4) . . . . ? C13 Fe1 C11 C12 -37.5(4) . . . . ? C5 Fe1 C11 C12 163.5(4) . . . . ? C1 Fe1 C11 C12 121.3(4) . . . . ? C15 C11 C12 C13 -0.6(6) . . . . ? Fe1 C11 C12 C13 59.4(4) . . . . ? C15 C11 C12 Fe1 -60.0(4) . . . . ? C11 Fe1 C12 C13 -118.7(5) . . . . ? C2 Fe1 C12 C13 120.2(3) . . . . ? C4 Fe1 C12 C13 40.3(8) . . . . ? C15 Fe1 C12 C13 -81.4(4) . . . . ? C3 Fe1 C12 C13 77.6(4) . . . . ? C14 Fe1 C12 C13 -37.1(3) . . . . ? C5 Fe1 C12 C13 -162.2(6) . . . . ? C1 Fe1 C12 C13 163.1(3) . . . . ? C2 Fe1 C12 C11 -121.2(4) . . . . ? C4 Fe1 C12 C11 159.0(6) . . . . ? C15 Fe1 C12 C11 37.3(4) . . . . ? C3 Fe1 C12 C11 -163.8(4) . . . . ? C14 Fe1 C12 C11 81.6(4) . . . . ? C13 Fe1 C12 C11 118.7(5) . . . . ? C5 Fe1 C12 C11 -43.5(9) . . . . ? C1 Fe1 C12 C11 -78.2(4) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? Fe1 C12 C13 C14 58.6(4) . . . . ? C11 C12 C13 Fe1 -58.7(4) . . . . ? C11 Fe1 C13 C12 38.5(4) . . . . ? C2 Fe1 C13 C12 -79.2(4) . . . . ? C4 Fe1 C13 C12 -163.6(4) . . . . ? C15 Fe1 C13 C12 81.8(4) . . . . ? C3 Fe1 C13 C12 -121.0(4) . . . . ? C14 Fe1 C13 C12 120.5(5) . . . . ? C5 Fe1 C13 C12 163.1(5) . . . . ? C1 Fe1 C13 C12 -44.2(7) . . . . ? C11 Fe1 C13 C14 -82.0(4) . . . . ? C2 Fe1 C13 C14 160.3(3) . . . . ? C4 Fe1 C13 C14 75.8(4) . . . . ? C15 Fe1 C13 C14 -38.7(4) . . . . ? C3 Fe1 C13 C14 118.5(4) . . . . ? C12 Fe1 C13 C14 -120.5(5) . . . . ? C5 Fe1 C13 C14 42.6(7) . . . . ? C1 Fe1 C13 C14 -164.7(5) . . . . ? C12 C13 C14 C15 0.6(6) . . . . ? Fe1 C13 C14 C15 59.6(4) . . . . ? C12 C13 C14 Fe1 -59.0(4) . . . . ? C11 Fe1 C14 C13 81.1(4) . . . . ? C2 Fe1 C14 C13 -50.1(8) . . . . ? C4 Fe1 C14 C13 -121.4(4) . . . . ? C15 Fe1 C14 C13 117.9(5) . . . . ? C3 Fe1 C14 C13 -80.0(4) . . . . ? C12 Fe1 C14 C13 36.6(4) . . . . ? C5 Fe1 C14 C13 -163.0(3) . . . . ? C1 Fe1 C14 C13 165.6(5) . . . . ? C11 Fe1 C14 C15 -36.8(4) . . . . ? C2 Fe1 C14 C15 -168.0(6) . . . . ? C4 Fe1 C14 C15 120.7(4) . . . . ? C3 Fe1 C14 C15 162.1(4) . . . . ? C13 Fe1 C14 C15 -117.9(5) . . . . ? C12 Fe1 C14 C15 -81.3(4) . . . . ? C5 Fe1 C14 C15 79.1(4) . . . . ? C1 Fe1 C14 C15 47.7(8) . . . . ? C12 C11 C15 C14 1.0(6) . . . . ? Fe1 C11 C15 C14 -59.1(4) . . . . ? C12 C11 C15 Fe1 60.1(4) . . . . ? C13 C14 C15 C11 -1.0(6) . . . . ? Fe1 C14 C15 C11 59.1(4) . . . . ? C13 C14 C15 Fe1 -60.1(4) . . . . ? C2 Fe1 C15 C11 47.5(8) . . . . ? C4 Fe1 C15 C11 163.4(3) . . . . ? C3 Fe1 C15 C11 -164.5(5) . . . . ? C14 Fe1 C15 C11 -119.9(5) . . . . ? C13 Fe1 C15 C11 -81.6(4) . . . . ? C12 Fe1 C15 C11 -38.3(4) . . . . ? C5 Fe1 C15 C11 120.7(4) . . . . ? C1 Fe1 C15 C11 78.9(4) . . . . ? C11 Fe1 C15 C14 119.9(5) . . . . ? C2 Fe1 C15 C14 167.4(6) . . . . ? C4 Fe1 C15 C14 -76.7(4) . . . . ? C3 Fe1 C15 C14 -44.6(8) . . . . ? C13 Fe1 C15 C14 38.3(4) . . . . ? C12 Fe1 C15 C14 81.6(4) . . . . ? C5 Fe1 C15 C14 -119.4(4) . . . . ? C1 Fe1 C15 C14 -161.1(3) . . . . ? C32 Zr1 C21 C22 -88.3(3) . . . . ? C31 Zr1 C21 C22 -41.4(4) . . . . ? C23 Zr1 C21 C22 -37.1(3) . . . . ? C24 Zr1 C21 C22 -77.8(3) . . . . ? C33 Zr1 C21 C22 -137.0(3) . . . . ? C35 Zr1 C21 C22 9.8(5) . . . . ? C34 Zr1 C21 C22 135.2(9) . . . . ? C25 Zr1 C21 C22 -114.5(4) . . . . ? B1 Zr1 C21 C22 87.3(3) . . . . ? C32 Zr1 C21 C25 26.2(4) . . . . ? C31 Zr1 C21 C25 73.1(4) . . . . ? C23 Zr1 C21 C25 77.4(3) . . . . ? C24 Zr1 C21 C25 36.7(3) . . . . ? C22 Zr1 C21 C25 114.5(4) . . . . ? C33 Zr1 C21 C25 -22.5(5) . . . . ? C35 Zr1 C21 C25 124.3(4) . . . . ? C34 Zr1 C21 C25 -110.3(10) . . . . ? B1 Zr1 C21 C25 -158.2(3) . . . . ? C25 C21 C22 C23 -1.2(6) . . . . ? Zr1 C21 C22 C23 65.3(4) . . . . ? C25 C21 C22 Zr1 -66.5(3) . . . . ? C32 Zr1 C22 C21 118.2(3) . . . . ? C31 Zr1 C22 C21 151.0(3) . . . . ? C23 Zr1 C22 C21 115.8(4) . . . . ? C24 Zr1 C22 C21 78.1(3) . . . . ? C33 Zr1 C22 C21 110.1(5) . . . . ? C35 Zr1 C22 C21 -175.1(3) . . . . ? C34 Zr1 C22 C21 -162.3(4) . . . . ? C25 Zr1 C22 C21 37.9(3) . . . . ? B1 Zr1 C22 C21 -89.7(3) . . . . ? C32 Zr1 C22 C23 2.4(4) . . . . ? C31 Zr1 C22 C23 35.2(4) . . . . ? C24 Zr1 C22 C23 -37.7(3) . . . . ? C33 Zr1 C22 C23 -5.7(7) . . . . ? C21 Zr1 C22 C23 -115.8(4) . . . . ? C35 Zr1 C22 C23 69.1(4) . . . . ? C34 Zr1 C22 C23 81.9(5) . . . . ? C25 Zr1 C22 C23 -77.9(3) . . . . ? B1 Zr1 C22 C23 154.5(3) . . . . ? C21 C22 C23 C24 0.8(6) . . . . ? Zr1 C22 C23 C24 66.8(4) . . . . ? C21 C22 C23 Zr1 -66.0(4) . . . . ? C32 Zr1 C23 C24 68.0(3) . . . . ? C31 Zr1 C23 C24 99.3(3) . . . . ? C22 Zr1 C23 C24 -114.0(5) . . . . ? C33 Zr1 C23 C24 63.4(4) . . . . ? C21 Zr1 C23 C24 -77.6(3) . . . . ? C35 Zr1 C23 C24 121.4(3) . . . . ? C34 Zr1 C23 C24 104.5(4) . . . . ? C25 Zr1 C23 C24 -36.5(3) . . . . ? B1 Zr1 C23 C24 -142.0(3) . . . . ? C32 Zr1 C23 C22 -178.0(3) . . . . ? C31 Zr1 C23 C22 -146.7(3) . . . . ? C24 Zr1 C23 C22 114.0(5) . . . . ? C33 Zr1 C23 C22 177.4(3) . . . . ? C21 Zr1 C23 C22 36.4(3) . . . . ? C35 Zr1 C23 C22 -124.6(3) . . . . ? C34 Zr1 C23 C22 -141.5(3) . . . . ? C25 Zr1 C23 C22 77.5(3) . . . . ? B1 Zr1 C23 C22 -28.1(4) . . . . ? C22 C23 C24 C25 -0.1(6) . . . . ? Zr1 C23 C24 C25 66.8(4) . . . . ? C22 C23 C24 Zr1 -66.9(4) . . . . ? C32 Zr1 C24 C25 134.7(3) . . . . ? C31 Zr1 C24 C25 166.7(3) . . . . ? C23 Zr1 C24 C25 -115.6(5) . . . . ? C22 Zr1 C24 C25 -77.8(3) . . . . ? C33 Zr1 C24 C25 114.4(3) . . . . ? C21 Zr1 C24 C25 -37.6(3) . . . . ? C35 Zr1 C24 C25 172.3(3) . . . . ? C34 Zr1 C24 C25 134.2(3) . . . . ? B1 Zr1 C24 C25 -59.7(4) . . . . ? C32 Zr1 C24 C23 -109.7(3) . . . . ? C31 Zr1 C24 C23 -77.7(3) . . . . ? C22 Zr1 C24 C23 37.8(3) . . . . ? C33 Zr1 C24 C23 -130.0(3) . . . . ? C21 Zr1 C24 C23 78.0(3) . . . . ? C35 Zr1 C24 C23 -72.1(4) . . . . ? C34 Zr1 C24 C23 -110.2(4) . . . . ? C25 Zr1 C24 C23 115.6(5) . . . . ? B1 Zr1 C24 C23 55.9(4) . . . . ? C23 C24 C25 C21 -0.7(6) . . . . ? Zr1 C24 C25 C21 65.2(4) . . . . ? C23 C24 C25 Zr1 -65.8(4) . . . . ? C22 C21 C25 C24 1.1(6) . . . . ? Zr1 C21 C25 C24 -65.2(4) . . . . ? C22 C21 C25 Zr1 66.3(3) . . . . ? C32 Zr1 C25 C24 -45.8(3) . . . . ? C31 Zr1 C25 C24 -15.3(4) . . . . ? C23 Zr1 C25 C24 37.1(3) . . . . ? C22 Zr1 C25 C24 78.1(3) . . . . ? C33 Zr1 C25 C24 -77.9(3) . . . . ? C21 Zr1 C25 C24 115.1(4) . . . . ? C35 Zr1 C25 C24 -14.5(6) . . . . ? C34 Zr1 C25 C24 -84.9(4) . . . . ? B1 Zr1 C25 C24 139.5(3) . . . . ? C32 Zr1 C25 C21 -160.9(3) . . . . ? C31 Zr1 C25 C21 -130.4(3) . . . . ? C23 Zr1 C25 C21 -78.0(3) . . . . ? C24 Zr1 C25 C21 -115.1(4) . . . . ? C22 Zr1 C25 C21 -37.0(3) . . . . ? C33 Zr1 C25 C21 167.0(3) . . . . ? C35 Zr1 C25 C21 -129.6(4) . . . . ? C34 Zr1 C25 C21 160.0(3) . . . . ? B1 Zr1 C25 C21 24.4(3) . . . . ? C23 Zr1 C31 C32 -106.5(3) . . . . ? C24 Zr1 C31 C32 -74.0(3) . . . . ? C22 Zr1 C31 C32 -125.0(3) . . . . ? C33 Zr1 C31 C32 37.1(3) . . . . ? C21 Zr1 C31 C32 -102.9(4) . . . . ? C35 Zr1 C31 C32 114.8(5) . . . . ? C34 Zr1 C31 C32 77.9(3) . . . . ? C25 Zr1 C31 C32 -65.9(4) . . . . ? B1 Zr1 C31 C32 140.2(3) . . . . ? C32 Zr1 C31 C35 -114.8(5) . . . . ? C23 Zr1 C31 C35 138.6(3) . . . . ? C24 Zr1 C31 C35 171.1(3) . . . . ? C22 Zr1 C31 C35 120.1(3) . . . . ? C33 Zr1 C31 C35 -77.7(3) . . . . ? C21 Zr1 C31 C35 142.2(3) . . . . ? C34 Zr1 C31 C35 -37.0(3) . . . . ? C25 Zr1 C31 C35 179.3(3) . . . . ? B1 Zr1 C31 C35 25.4(4) . . . . ? C35 C31 C32 C33 0.1(6) . . . . ? Zr1 C31 C32 C33 -66.7(4) . . . . ? C35 C31 C32 Zr1 66.9(4) . . . . ? C23 Zr1 C32 C31 71.7(3) . . . . ? C24 Zr1 C32 C31 102.5(3) . . . . ? C22 Zr1 C32 C31 70.4(4) . . . . ? C33 Zr1 C32 C31 -115.3(5) . . . . ? C21 Zr1 C32 C31 111.2(3) . . . . ? C35 Zr1 C32 C31 -37.4(3) . . . . ? C34 Zr1 C32 C31 -78.0(4) . . . . ? C25 Zr1 C32 C31 125.5(3) . . . . ? B1 Zr1 C32 C31 -62.0(4) . . . . ? C31 Zr1 C32 C33 115.3(5) . . . . ? C23 Zr1 C32 C33 -173.0(4) . . . . ? C24 Zr1 C32 C33 -142.2(4) . . . . ? C22 Zr1 C32 C33 -174.3(3) . . . . ? C21 Zr1 C32 C33 -133.5(3) . . . . ? C35 Zr1 C32 C33 77.9(4) . . . . ? C34 Zr1 C32 C33 37.4(3) . . . . ? C25 Zr1 C32 C33 -119.2(3) . . . . ? B1 Zr1 C32 C33 53.3(5) . . . . ? C31 C32 C33 C34 0.1(6) . . . . ? Zr1 C32 C33 C34 -66.3(4) . . . . ? C31 C32 C33 Zr1 66.3(4) . . . . ? C31 Zr1 C33 C32 -36.9(3) . . . . ? C23 Zr1 C33 C32 8.5(4) . . . . ? C24 Zr1 C33 C32 38.9(4) . . . . ? C22 Zr1 C33 C32 12.2(7) . . . . ? C21 Zr1 C33 C32 85.5(5) . . . . ? C35 Zr1 C33 C32 -77.8(4) . . . . ? C34 Zr1 C33 C32 -114.7(5) . . . . ? C25 Zr1 C33 C32 72.0(4) . . . . ? B1 Zr1 C33 C32 -145.6(3) . . . . ? C32 Zr1 C33 C34 114.7(5) . . . . ? C31 Zr1 C33 C34 77.8(3) . . . . ? C23 Zr1 C33 C34 123.2(3) . . . . ? C24 Zr1 C33 C34 153.6(3) . . . . ? C22 Zr1 C33 C34 126.9(5) . . . . ? C21 Zr1 C33 C34 -159.8(3) . . . . ? C35 Zr1 C33 C34 36.9(3) . . . . ? C25 Zr1 C33 C34 -173.4(3) . . . . ? B1 Zr1 C33 C34 -30.9(4) . . . . ? C32 C33 C34 C35 -0.2(6) . . . . ? Zr1 C33 C34 C35 -65.6(4) . . . . ? C32 C33 C34 Zr1 65.4(4) . . . . ? C32 Zr1 C34 C35 77.9(3) . . . . ? C31 Zr1 C34 C35 37.3(3) . . . . ? C23 Zr1 C34 C35 31.1(4) . . . . ? C24 Zr1 C34 C35 78.5(4) . . . . ? C22 Zr1 C34 C35 -20.2(5) . . . . ? C33 Zr1 C34 C35 115.3(5) . . . . ? C21 Zr1 C34 C35 -139.8(9) . . . . ? C25 Zr1 C34 C35 126.9(4) . . . . ? B1 Zr1 C34 C35 -92.1(3) . . . . ? C32 Zr1 C34 C33 -37.4(3) . . . . ? C31 Zr1 C34 C33 -78.0(3) . . . . ? C23 Zr1 C34 C33 -84.2(4) . . . . ? C24 Zr1 C34 C33 -36.7(4) . . . . ? C22 Zr1 C34 C33 -135.4(4) . . . . ? C21 Zr1 C34 C33 104.9(10) . . . . ? C35 Zr1 C34 C33 -115.3(5) . . . . ? C25 Zr1 C34 C33 11.6(5) . . . . ? B1 Zr1 C34 C33 152.6(3) . . . . ? C33 C34 C35 C31 0.3(6) . . . . ? Zr1 C34 C35 C31 -65.1(4) . . . . ? C33 C34 C35 Zr1 65.4(4) . . . . ? C32 C31 C35 C34 -0.3(6) . . . . ? Zr1 C31 C35 C34 66.0(4) . . . . ? C32 C31 C35 Zr1 -66.2(4) . . . . ? C32 Zr1 C35 C34 -77.9(3) . . . . ? C31 Zr1 C35 C34 -115.1(5) . . . . ? C23 Zr1 C35 C34 -158.1(3) . . . . ? C24 Zr1 C35 C34 -125.4(3) . . . . ? C22 Zr1 C35 C34 169.8(3) . . . . ? C33 Zr1 C35 C34 -37.1(3) . . . . ? C21 Zr1 C35 C34 163.6(4) . . . . ? C25 Zr1 C35 C34 -116.4(4) . . . . ? B1 Zr1 C35 C34 86.8(3) . . . . ? C32 Zr1 C35 C31 37.2(3) . . . . ? C23 Zr1 C35 C31 -43.0(3) . . . . ? C24 Zr1 C35 C31 -10.3(4) . . . . ? C22 Zr1 C35 C31 -75.1(4) . . . . ? C33 Zr1 C35 C31 78.0(3) . . . . ? C21 Zr1 C35 C31 -81.3(5) . . . . ? C34 Zr1 C35 C31 115.1(5) . . . . ? C25 Zr1 C35 C31 -1.3(6) . . . . ? B1 Zr1 C35 C31 -158.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.812 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.106 data_wa1196 _database_code_depnum_ccdc_archive 'CCDC 894221' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 B2 Fe2 Zr' _chemical_formula_sum 'C30 H34 B2 Fe2 Zr' _chemical_formula_weight 619.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6961(5) _cell_length_b 11.9241(7) _cell_length_c 14.5443(9) _cell_angle_alpha 79.726(5) _cell_angle_beta 78.431(5) _cell_angle_gamma 88.685(5) _cell_volume 1286.52(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12936 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 26.1 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7298 _exptl_absorpt_correction_T_max 0.7705 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 16842 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.65 _reflns_number_total 4812 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _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^)+(0.0232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4812 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _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 Zr1 Zr 0.37543(3) 0.26258(2) 0.45959(2) 0.01356(8) Uani 1 1 d . . . Fe1 Fe 0.26507(5) 0.07806(4) 0.15797(3) 0.01954(11) Uani 1 1 d . . . Fe2 Fe 0.28228(5) 0.58659(4) 0.15319(3) 0.01873(11) Uani 1 1 d . . . B1 B 0.2710(5) 0.1037(3) 0.3762(3) 0.0244(7) Uani 1 1 d . . . H1A H 0.206(4) 0.184(3) 0.376(3) 0.029(9) Uiso 1 1 d . . . H1C H 0.170(5) 0.036(3) 0.412(3) 0.037(10) Uiso 1 1 d . . . H1B H 0.372(5) 0.102(3) 0.431(3) 0.039(10) Uiso 1 1 d . . . B2 B 0.2737(4) 0.4523(3) 0.3660(3) 0.0222(7) Uani 1 1 d . . . H2A H 0.341(4) 0.438(3) 0.433(3) 0.028(9) Uiso 1 1 d . . . H2B H 0.299(5) 0.360(3) 0.351(3) 0.044(11) Uiso 1 1 d . . . H2C H 0.116(4) 0.470(3) 0.399(3) 0.029(9) Uiso 1 1 d . . . C1 C 0.3767(4) 0.0993(3) 0.2719(2) 0.0223(6) Uani 1 1 d . . . C2 C 0.4216(4) 0.1923(3) 0.1936(2) 0.0257(7) Uani 1 1 d . . . H2 H 0.3945 0.2699 0.1964 0.031 Uiso 1 1 calc R . . C3 C 0.5119(4) 0.1517(3) 0.1115(3) 0.0288(7) Uani 1 1 d . . . H3 H 0.5559 0.1968 0.0508 0.035 Uiso 1 1 calc R . . C4 C 0.5254(4) 0.0318(3) 0.1359(3) 0.0287(7) Uani 1 1 d . . . H4 H 0.5794 -0.0181 0.0947 0.034 Uiso 1 1 calc R . . C5 C 0.4426(4) 0.0000(3) 0.2339(2) 0.0253(7) Uani 1 1 d . . . H5 H 0.4325 -0.0757 0.2688 0.030 Uiso 1 1 calc R . . C11 C -0.0035(4) 0.0685(3) 0.2073(3) 0.0310(8) Uani 1 1 d . . . H11 H -0.0632 0.0758 0.2697 0.037 Uiso 1 1 calc R . . C12 C 0.0395(4) 0.1586(3) 0.1282(3) 0.0317(8) Uani 1 1 d . . . H12 H 0.0129 0.2368 0.1281 0.038 Uiso 1 1 calc R . . C13 C 0.1288(4) 0.1116(3) 0.0495(3) 0.0307(7) Uani 1 1 d . . . H13 H 0.1736 0.1529 -0.0127 0.037 Uiso 1 1 calc R . . C14 C 0.1402(4) -0.0073(3) 0.0792(3) 0.0292(7) Uani 1 1 d . . . H14 H 0.1936 -0.0598 0.0404 0.035 Uiso 1 1 calc R . . C15 C 0.0584(4) -0.0344(3) 0.1766(3) 0.0291(7) Uani 1 1 d . . . H15 H 0.0468 -0.1084 0.2148 0.035 Uiso 1 1 calc R . . C21 C 0.3042(4) 0.2694(3) 0.6345(2) 0.0244(7) Uani 1 1 d . . . H21 H 0.3931 0.2934 0.6639 0.029 Uiso 1 1 calc R . . C22 C 0.1815(4) 0.3395(3) 0.5937(2) 0.0240(6) Uani 1 1 d . . . H22 H 0.1727 0.4196 0.5903 0.029 Uiso 1 1 calc R . . C23 C 0.0730(4) 0.2707(3) 0.5583(2) 0.0263(7) Uani 1 1 d . . . H23 H -0.0203 0.2965 0.5261 0.032 Uiso 1 1 calc R . . C24 C 0.1271(4) 0.1579(3) 0.5789(2) 0.0256(7) Uani 1 1 d . . . H24 H 0.0750 0.0933 0.5647 0.031 Uiso 1 1 calc R . . C25 C 0.2724(4) 0.1569(3) 0.6245(2) 0.0235(6) Uani 1 1 d . . . H25 H 0.3375 0.0917 0.6449 0.028 Uiso 1 1 calc R . . C31 C 0.6746(4) 0.1697(3) 0.4192(3) 0.0306(8) Uani 1 1 d . . . H31 H 0.6803 0.0917 0.4129 0.037 Uiso 1 1 calc R . . C32 C 0.6672(4) 0.2110(3) 0.5035(3) 0.0260(7) Uani 1 1 d . . . H32 H 0.6656 0.1662 0.5647 0.031 Uiso 1 1 calc R . . C33 C 0.6625(3) 0.3313(3) 0.4822(2) 0.0216(6) Uani 1 1 d . . . H33 H 0.6561 0.3815 0.5266 0.026 Uiso 1 1 calc R . . C34 C 0.6687(3) 0.3634(3) 0.3845(2) 0.0242(7) Uani 1 1 d . . . H34 H 0.6704 0.4393 0.3504 0.029 Uiso 1 1 calc R . . C35 C 0.6720(4) 0.2629(3) 0.3449(3) 0.0299(8) Uani 1 1 d . . . H35 H 0.6724 0.2591 0.2802 0.036 Uiso 1 1 calc R . . C41 C 0.3653(4) 0.5480(2) 0.2813(2) 0.0178(6) Uani 1 1 d . . . C42 C 0.3093(4) 0.6641(2) 0.2629(2) 0.0209(6) Uani 1 1 d . . . H42 H 0.2163 0.6974 0.3024 0.025 Uiso 1 1 calc R . . C43 C 0.4151(4) 0.7219(3) 0.1761(2) 0.0250(7) Uani 1 1 d . . . H43 H 0.4046 0.7995 0.1481 0.030 Uiso 1 1 calc R . . C44 C 0.5382(4) 0.6436(3) 0.1390(2) 0.0262(7) Uani 1 1 d . . . H44 H 0.6258 0.6592 0.0820 0.031 Uiso 1 1 calc R . . C45 C 0.5074(4) 0.5368(3) 0.2026(2) 0.0222(6) Uani 1 1 d . . . H45 H 0.5709 0.4688 0.1942 0.027 Uiso 1 1 calc R . . C51 C 0.0758(5) 0.4774(3) 0.1625(3) 0.0379(9) Uani 1 1 d . . . H51 H 0.0299 0.4199 0.2155 0.045 Uiso 1 1 calc R . . C52 C 0.0201(4) 0.5914(4) 0.1481(3) 0.0428(10) Uani 1 1 d . . . H52 H -0.0695 0.6241 0.1900 0.051 Uiso 1 1 calc R . . C53 C 0.1195(5) 0.6488(3) 0.0613(3) 0.0394(9) Uani 1 1 d . . . H53 H 0.1083 0.7265 0.0340 0.047 Uiso 1 1 calc R . . C54 C 0.2396(5) 0.5699(3) 0.0215(3) 0.0355(8) Uani 1 1 d . . . H54 H 0.3237 0.5854 -0.0368 0.043 Uiso 1 1 calc R . . C55 C 0.2113(5) 0.4634(3) 0.0847(3) 0.0339(8) Uani 1 1 d . . . H55 H 0.2730 0.3950 0.0760 0.041 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 Zr1 0.01345(13) 0.01379(14) 0.01400(15) -0.00250(11) -0.00392(10) -0.00090(9) Fe1 0.0230(2) 0.0193(2) 0.0172(2) -0.00325(18) -0.00573(18) -0.00155(16) Fe2 0.0222(2) 0.0191(2) 0.0158(2) -0.00307(18) -0.00577(17) 0.00080(16) B1 0.0308(17) 0.0208(17) 0.025(2) -0.0060(15) -0.0106(15) -0.0049(14) B2 0.0235(15) 0.0220(17) 0.0206(18) 0.0011(15) -0.0074(14) 0.0004(13) C1 0.0253(14) 0.0215(15) 0.0218(17) -0.0026(13) -0.0093(12) -0.0042(12) C2 0.0343(16) 0.0206(15) 0.0247(18) -0.0034(14) -0.0118(13) -0.0053(13) C3 0.0243(15) 0.0362(19) 0.0240(18) -0.0001(15) -0.0038(13) -0.0077(13) C4 0.0223(14) 0.0374(19) 0.0286(19) -0.0108(16) -0.0057(13) 0.0014(13) C5 0.0267(15) 0.0259(16) 0.0241(17) -0.0007(14) -0.0106(13) 0.0010(12) C11 0.0262(15) 0.0361(19) 0.030(2) -0.0066(16) -0.0042(14) 0.0004(14) C12 0.0292(16) 0.0276(17) 0.042(2) -0.0050(16) -0.0176(15) 0.0053(13) C13 0.0332(17) 0.0355(19) 0.0242(18) 0.0027(15) -0.0144(14) -0.0041(14) C14 0.0294(16) 0.0308(18) 0.0307(19) -0.0095(15) -0.0101(14) -0.0047(13) C15 0.0273(15) 0.0282(17) 0.0305(19) -0.0006(15) -0.0056(14) -0.0074(13) C21 0.0199(13) 0.0371(18) 0.0163(16) -0.0066(14) -0.0014(12) -0.0062(12) C22 0.0251(14) 0.0248(16) 0.0193(16) -0.0053(13) 0.0029(12) 0.0044(12) C23 0.0128(13) 0.044(2) 0.0197(17) -0.0040(15) 0.0010(12) 0.0010(12) C24 0.0220(14) 0.0342(18) 0.0182(16) -0.0034(14) 0.0020(12) -0.0140(13) C25 0.0245(14) 0.0252(16) 0.0175(16) 0.0043(13) -0.0034(12) 0.0012(12) C31 0.0180(14) 0.0250(17) 0.049(2) -0.0130(16) -0.0028(14) 0.0037(12) C32 0.0147(13) 0.0269(17) 0.0319(19) 0.0064(15) -0.0048(12) 0.0023(12) C33 0.0134(12) 0.0257(16) 0.0285(18) -0.0067(14) -0.0092(12) -0.0019(11) C34 0.0133(13) 0.0241(16) 0.0335(19) 0.0017(14) -0.0060(12) -0.0056(11) C35 0.0150(13) 0.050(2) 0.0257(18) -0.0128(17) 0.0001(12) -0.0030(13) C41 0.0212(13) 0.0160(14) 0.0182(16) -0.0039(12) -0.0079(12) 0.0013(11) C42 0.0291(14) 0.0173(14) 0.0171(16) -0.0035(12) -0.0066(12) 0.0017(11) C43 0.0379(16) 0.0187(15) 0.0187(16) 0.0010(13) -0.0091(13) -0.0065(13) C44 0.0210(14) 0.0376(18) 0.0190(17) -0.0042(15) -0.0020(12) -0.0048(13) C45 0.0201(14) 0.0278(16) 0.0202(16) -0.0071(14) -0.0052(12) 0.0046(12) C51 0.0397(19) 0.045(2) 0.031(2) -0.0022(17) -0.0138(16) -0.0203(16) C52 0.0262(17) 0.064(3) 0.047(3) -0.024(2) -0.0167(17) 0.0038(17) C53 0.051(2) 0.0329(19) 0.042(2) -0.0047(18) -0.0311(19) 0.0066(16) C54 0.051(2) 0.040(2) 0.0179(18) -0.0046(16) -0.0133(15) -0.0075(16) C55 0.0458(19) 0.0279(18) 0.035(2) -0.0125(16) -0.0179(16) -0.0026(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 Zr1 C33 2.476(3) . ? Zr1 C25 2.485(3) . ? Zr1 C23 2.487(3) . ? Zr1 C32 2.490(3) . ? Zr1 C24 2.496(3) . ? Zr1 C22 2.506(3) . ? Zr1 C21 2.509(3) . ? Zr1 C34 2.530(3) . ? Zr1 C31 2.538(3) . ? Zr1 C35 2.542(3) . ? Zr1 B2 2.614(4) . ? Zr1 B1 2.644(3) . ? Zr1 H1A 2.27(3) . ? Zr1 H1B 2.03(4) . ? Zr1 H2A 2.07(3) . ? Zr1 H2B 1.97(4) . ? Fe1 C5 2.032(3) . ? Fe1 C2 2.038(3) . ? Fe1 C13 2.041(3) . ? Fe1 C14 2.043(3) . ? Fe1 C4 2.043(3) . ? Fe1 C3 2.046(3) . ? Fe1 C11 2.046(3) . ? Fe1 C15 2.049(3) . ? Fe1 C12 2.050(3) . ? Fe1 C1 2.068(3) . ? Fe2 C42 2.028(3) . ? Fe2 C52 2.033(3) . ? Fe2 C43 2.041(3) . ? Fe2 C45 2.042(3) . ? Fe2 C53 2.045(4) . ? Fe2 C51 2.046(3) . ? Fe2 C54 2.051(3) . ? Fe2 C55 2.055(3) . ? Fe2 C44 2.058(3) . ? Fe2 C41 2.062(3) . ? B1 C1 1.580(5) . ? B1 H1A 1.06(4) . ? B1 H1C 1.11(4) . ? B1 H1B 1.22(4) . ? B2 C41 1.582(5) . ? B2 H2A 1.17(4) . ? B2 H2B 1.16(4) . ? B2 H2C 1.24(3) . ? C1 C5 1.434(4) . ? C1 C2 1.435(5) . ? C2 C3 1.414(5) . ? C2 H2 0.9500 . ? C3 C4 1.417(5) . ? C3 H3 0.9500 . ? C4 C5 1.426(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C12 1.418(5) . ? C11 C15 1.420(5) . ? C11 H11 0.9500 . ? C12 C13 1.410(5) . ? C12 H12 0.9500 . ? C13 C14 1.412(5) . ? C13 H13 0.9500 . ? C14 C15 1.413(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C22 1.399(5) . ? C21 C25 1.407(5) . ? C21 H21 0.9500 . ? C22 C23 1.410(4) . ? C22 H22 0.9500 . ? C23 C24 1.398(5) . ? C23 H23 0.9500 . ? C24 C25 1.409(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.391(5) . ? C31 C35 1.408(5) . ? C31 H31 0.9500 . ? C32 C33 1.414(4) . ? C32 H32 0.9500 . ? C33 C34 1.395(5) . ? C33 H33 0.9500 . ? C34 C35 1.416(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C42 1.436(4) . ? C41 C45 1.440(4) . ? C42 C43 1.427(4) . ? C42 H42 0.9500 . ? C43 C44 1.412(5) . ? C43 H43 0.9500 . ? C44 C45 1.428(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C51 C52 1.408(6) . ? C51 C55 1.408(5) . ? C51 H51 0.9500 . ? C52 C53 1.406(6) . ? C52 H52 0.9500 . ? C53 C54 1.419(5) . ? C53 H53 0.9500 . ? C54 C55 1.421(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C33 Zr1 C25 97.36(10) . . ? C33 Zr1 C23 129.68(11) . . ? C25 Zr1 C23 54.36(11) . . ? C33 Zr1 C32 33.09(10) . . ? C25 Zr1 C32 80.27(10) . . ? C23 Zr1 C32 131.82(11) . . ? C33 Zr1 C24 129.74(11) . . ? C25 Zr1 C24 32.86(10) . . ? C23 Zr1 C24 32.58(11) . . ? C32 Zr1 C24 111.21(11) . . ? C33 Zr1 C22 97.26(10) . . ? C25 Zr1 C22 54.04(11) . . ? C23 Zr1 C22 32.80(10) . . ? C32 Zr1 C22 108.94(11) . . ? C24 Zr1 C22 53.97(10) . . ? C33 Zr1 C21 79.31(10) . . ? C25 Zr1 C21 32.72(11) . . ? C23 Zr1 C21 54.20(10) . . ? C32 Zr1 C21 79.28(11) . . ? C24 Zr1 C21 54.13(10) . . ? C22 Zr1 C21 32.39(10) . . ? C33 Zr1 C34 32.35(11) . . ? C25 Zr1 C34 129.43(10) . . ? C23 Zr1 C34 147.65(11) . . ? C32 Zr1 C34 53.87(10) . . ? C24 Zr1 C34 162.09(10) . . ? C22 Zr1 C34 117.66(10) . . ? C21 Zr1 C34 109.61(10) . . ? C33 Zr1 C31 53.78(10) . . ? C25 Zr1 C31 99.34(11) . . ? C23 Zr1 C31 152.51(12) . . ? C32 Zr1 C31 32.09(12) . . ? C24 Zr1 C31 120.75(11) . . ? C22 Zr1 C31 140.60(11) . . ? C21 Zr1 C31 109.24(11) . . ? C34 Zr1 C31 53.36(10) . . ? C33 Zr1 C35 53.89(10) . . ? C25 Zr1 C35 130.95(11) . . ? C23 Zr1 C35 174.48(12) . . ? C32 Zr1 C35 53.66(11) . . ? C24 Zr1 C35 150.48(12) . . ? C22 Zr1 C35 149.48(10) . . ? C21 Zr1 C35 130.77(10) . . ? C34 Zr1 C35 32.42(11) . . ? C31 Zr1 C35 32.18(12) . . ? C33 Zr1 B2 98.40(10) . . ? C25 Zr1 B2 132.66(11) . . ? C23 Zr1 B2 81.76(11) . . ? C32 Zr1 B2 130.19(10) . . ? C24 Zr1 B2 112.66(11) . . ? C22 Zr1 B2 79.81(11) . . ? C21 Zr1 B2 108.92(11) . . ? C34 Zr1 B2 78.16(10) . . ? C31 Zr1 B2 125.73(11) . . ? C35 Zr1 B2 93.67(12) . . ? C33 Zr1 B1 136.10(11) . . ? C25 Zr1 B1 94.87(11) . . ? C23 Zr1 B1 91.10(11) . . ? C32 Zr1 B1 109.82(11) . . ? C24 Zr1 B1 74.44(11) . . ? C22 Zr1 B1 123.57(11) . . ? C21 Zr1 B1 126.35(11) . . ? C34 Zr1 B1 118.10(11) . . ? C31 Zr1 B1 82.70(11) . . ? C35 Zr1 B1 86.95(11) . . ? B2 Zr1 B1 103.65(11) . . ? C33 Zr1 H1A 152.2(9) . . ? C25 Zr1 H1A 102.4(9) . . ? C23 Zr1 H1A 78.1(9) . . ? C32 Zr1 H1A 132.7(9) . . ? C24 Zr1 H1A 73.4(9) . . ? C22 Zr1 H1A 110.2(9) . . ? C21 Zr1 H1A 127.0(9) . . ? C34 Zr1 H1A 123.4(9) . . ? C31 Zr1 H1A 103.3(9) . . ? C35 Zr1 H1A 98.3(9) . . ? B2 Zr1 H1A 82.4(9) . . ? B1 Zr1 H1A 23.5(9) . . ? C33 Zr1 H1B 116.1(10) . . ? C25 Zr1 H1B 80.9(11) . . ? C23 Zr1 H1B 100.7(10) . . ? C32 Zr1 H1B 85.5(11) . . ? C24 Zr1 H1B 73.4(10) . . ? C22 Zr1 H1B 127.3(11) . . ? C21 Zr1 H1B 113.3(11) . . ? C34 Zr1 H1B 111.7(10) . . ? C31 Zr1 H1B 63.5(10) . . ? C35 Zr1 H1B 79.8(10) . . ? B2 Zr1 H1B 129.0(12) . . ? B1 Zr1 H1B 26.3(11) . . ? H1A Zr1 H1B 49.5(14) . . ? C33 Zr1 H2A 79.2(9) . . ? C25 Zr1 H2A 118.7(10) . . ? C23 Zr1 H2A 81.3(9) . . ? C32 Zr1 H2A 112.2(9) . . ? C24 Zr1 H2A 113.5(9) . . ? C22 Zr1 H2A 65.6(10) . . ? C21 Zr1 H2A 88.5(10) . . ? C34 Zr1 H2A 69.7(9) . . ? C31 Zr1 H2A 123.0(9) . . ? C35 Zr1 H2A 96.0(9) . . ? B2 Zr1 H2A 25.8(10) . . ? B1 Zr1 H2A 129.4(10) . . ? H1A Zr1 H2A 107.5(14) . . ? H1B Zr1 H2A 154.7(15) . . ? C33 Zr1 H2B 110.6(11) . . ? C25 Zr1 H2B 144.2(11) . . ? C23 Zr1 H2B 90.0(11) . . ? C32 Zr1 H2B 134.9(11) . . ? C24 Zr1 H2B 113.9(11) . . ? C22 Zr1 H2B 99.2(12) . . ? C21 Zr1 H2B 130.8(12) . . ? C34 Zr1 H2B 82.1(11) . . ? C31 Zr1 H2B 115.0(11) . . ? C35 Zr1 H2B 84.5(11) . . ? B2 Zr1 H2B 24.5(12) . . ? B1 Zr1 H2B 80.5(12) . . ? H1A Zr1 H2B 61.5(15) . . ? H1B Zr1 H2B 104.9(17) . . ? H2A Zr1 H2B 49.8(15) . . ? C5 Fe1 C2 67.93(13) . . ? C5 Fe1 C13 157.57(14) . . ? C2 Fe1 C13 125.10(14) . . ? C5 Fe1 C14 121.65(14) . . ? C2 Fe1 C14 161.33(14) . . ? C13 Fe1 C14 40.47(14) . . ? C5 Fe1 C4 40.96(13) . . ? C2 Fe1 C4 68.24(13) . . ? C13 Fe1 C4 122.12(14) . . ? C14 Fe1 C4 107.54(13) . . ? C5 Fe1 C3 68.26(13) . . ? C2 Fe1 C3 40.51(14) . . ? C13 Fe1 C3 108.61(14) . . ? C14 Fe1 C3 124.58(14) . . ? C4 Fe1 C3 40.55(14) . . ? C5 Fe1 C11 123.39(14) . . ? C2 Fe1 C11 122.14(14) . . ? C13 Fe1 C11 68.06(15) . . ? C14 Fe1 C11 68.08(14) . . ? C4 Fe1 C11 160.05(14) . . ? C3 Fe1 C11 157.86(14) . . ? C5 Fe1 C15 107.04(13) . . ? C2 Fe1 C15 157.16(14) . . ? C13 Fe1 C15 68.05(14) . . ? C14 Fe1 C15 40.40(14) . . ? C4 Fe1 C15 123.54(13) . . ? C3 Fe1 C15 160.44(14) . . ? C11 Fe1 C15 40.58(13) . . ? C5 Fe1 C12 160.18(14) . . ? C2 Fe1 C12 108.66(13) . . ? C13 Fe1 C12 40.34(15) . . ? C14 Fe1 C12 67.94(14) . . ? C4 Fe1 C12 157.79(15) . . ? C3 Fe1 C12 122.75(14) . . ? C11 Fe1 C12 40.50(14) . . ? C15 Fe1 C12 68.07(14) . . ? C5 Fe1 C1 40.94(12) . . ? C2 Fe1 C1 40.89(13) . . ? C13 Fe1 C1 160.69(13) . . ? C14 Fe1 C1 156.53(13) . . ? C4 Fe1 C1 69.45(13) . . ? C3 Fe1 C1 69.14(13) . . ? C11 Fe1 C1 106.40(13) . . ? C15 Fe1 C1 120.61(13) . . ? C12 Fe1 C1 123.59(13) . . ? C42 Fe2 C52 106.49(14) . . ? C42 Fe2 C43 41.06(13) . . ? C52 Fe2 C43 122.61(15) . . ? C42 Fe2 C45 68.41(12) . . ? C52 Fe2 C45 158.19(16) . . ? C43 Fe2 C45 68.37(13) . . ? C42 Fe2 C53 121.99(14) . . ? C52 Fe2 C53 40.35(17) . . ? C43 Fe2 C53 107.52(14) . . ? C45 Fe2 C53 160.34(15) . . ? C42 Fe2 C51 122.16(14) . . ? C52 Fe2 C51 40.40(16) . . ? C43 Fe2 C51 158.60(15) . . ? C45 Fe2 C51 123.00(15) . . ? C53 Fe2 C51 67.90(16) . . ? C42 Fe2 C54 158.65(14) . . ? C52 Fe2 C54 67.98(16) . . ? C43 Fe2 C54 123.16(14) . . ? C45 Fe2 C54 124.37(14) . . ? C53 Fe2 C54 40.54(16) . . ? C51 Fe2 C54 67.89(15) . . ? C42 Fe2 C55 158.51(14) . . ? C52 Fe2 C55 67.81(15) . . ? C43 Fe2 C55 159.52(14) . . ? C45 Fe2 C55 108.72(14) . . ? C53 Fe2 C55 67.99(15) . . ? C51 Fe2 C55 40.17(15) . . ? C54 Fe2 C55 40.49(15) . . ? C42 Fe2 C44 68.41(12) . . ? C52 Fe2 C44 159.03(16) . . ? C43 Fe2 C44 40.31(13) . . ? C45 Fe2 C44 40.77(13) . . ? C53 Fe2 C44 123.77(15) . . ? C51 Fe2 C44 159.55(15) . . ? C54 Fe2 C44 108.94(14) . . ? C55 Fe2 C44 124.27(14) . . ? C42 Fe2 C41 41.11(11) . . ? C52 Fe2 C41 121.15(15) . . ? C43 Fe2 C41 69.45(12) . . ? C45 Fe2 C41 41.07(12) . . ? C53 Fe2 C41 157.39(14) . . ? C51 Fe2 C41 106.31(13) . . ? C54 Fe2 C41 159.60(13) . . ? C55 Fe2 C41 122.60(13) . . ? C44 Fe2 C41 69.26(12) . . ? C1 B1 Zr1 115.9(2) . . ? C1 B1 H1A 109(2) . . ? Zr1 B1 H1A 58.4(19) . . ? C1 B1 H1C 119(2) . . ? Zr1 B1 H1C 124(2) . . ? H1A B1 H1C 107(3) . . ? C1 B1 H1B 110.8(18) . . ? Zr1 B1 H1B 47.7(18) . . ? H1A B1 H1B 105(3) . . ? H1C B1 H1B 105(3) . . ? C41 B2 Zr1 135.5(2) . . ? C41 B2 H2A 114.7(17) . . ? Zr1 B2 H2A 50.5(17) . . ? C41 B2 H2B 114(2) . . ? Zr1 B2 H2B 45(2) . . ? H2A B2 H2B 94(3) . . ? C41 B2 H2C 114.4(17) . . ? Zr1 B2 H2C 110.1(17) . . ? H2A B2 H2C 104(2) . . ? H2B B2 H2C 113(2) . . ? C5 C1 C2 104.8(3) . . ? C5 C1 B1 127.3(3) . . ? C2 C1 B1 127.8(3) . . ? C5 C1 Fe1 68.18(17) . . ? C2 C1 Fe1 68.40(17) . . ? B1 C1 Fe1 125.5(2) . . ? C3 C2 C1 110.1(3) . . ? C3 C2 Fe1 70.08(17) . . ? C1 C2 Fe1 70.71(16) . . ? C3 C2 H2 125.0 . . ? C1 C2 H2 125.0 . . ? Fe1 C2 H2 125.9 . . ? C2 C3 C4 107.9(3) . . ? C2 C3 Fe1 69.41(17) . . ? C4 C3 Fe1 69.61(17) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe1 C3 H3 126.5 . . ? C3 C4 C5 107.2(3) . . ? C3 C4 Fe1 69.83(18) . . ? C5 C4 Fe1 69.11(17) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe1 C4 H4 126.2 . . ? C4 C5 C1 110.0(3) . . ? C4 C5 Fe1 69.94(18) . . ? C1 C5 Fe1 70.88(17) . . ? C4 C5 H5 125.0 . . ? C1 C5 H5 125.0 . . ? Fe1 C5 H5 125.7 . . ? C12 C11 C15 107.9(3) . . ? C12 C11 Fe1 69.87(18) . . ? C15 C11 Fe1 69.82(17) . . ? C12 C11 H11 126.1 . . ? C15 C11 H11 126.1 . . ? Fe1 C11 H11 125.8 . . ? C13 C12 C11 108.0(3) . . ? C13 C12 Fe1 69.51(18) . . ? C11 C12 Fe1 69.63(19) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Fe1 C12 H12 126.4 . . ? C12 C13 C14 108.2(3) . . ? C12 C13 Fe1 70.15(19) . . ? C14 C13 Fe1 69.83(19) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Fe1 C13 H13 125.7 . . ? C13 C14 C15 108.2(3) . . ? C13 C14 Fe1 69.70(18) . . ? C15 C14 Fe1 70.04(18) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Fe1 C14 H14 125.9 . . ? C14 C15 C11 107.8(3) . . ? C14 C15 Fe1 69.56(17) . . ? C11 C15 Fe1 69.60(18) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Fe1 C15 H15 126.3 . . ? C22 C21 C25 107.8(3) . . ? C22 C21 Zr1 73.69(18) . . ? C25 C21 Zr1 72.71(18) . . ? C22 C21 H21 126.1 . . ? C25 C21 H21 126.1 . . ? Zr1 C21 H21 119.4 . . ? C21 C22 C23 108.3(3) . . ? C21 C22 Zr1 73.91(17) . . ? C23 C22 Zr1 72.87(17) . . ? C21 C22 H22 125.9 . . ? C23 C22 H22 125.9 . . ? Zr1 C22 H22 119.2 . . ? C24 C23 C22 107.9(3) . . ? C24 C23 Zr1 74.04(17) . . ? C22 C23 Zr1 74.33(16) . . ? C24 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? Zr1 C23 H23 117.6 . . ? C23 C24 C25 108.1(3) . . ? C23 C24 Zr1 73.38(17) . . ? C25 C24 Zr1 73.16(17) . . ? C23 C24 H24 126.0 . . ? C25 C24 H24 126.0 . . ? Zr1 C24 H24 119.3 . . ? C21 C25 C24 107.9(3) . . ? C21 C25 Zr1 74.56(18) . . ? C24 C25 Zr1 73.98(18) . . ? C21 C25 H25 126.0 . . ? C24 C25 H25 126.0 . . ? Zr1 C25 H25 117.4 . . ? C32 C31 C35 108.5(3) . . ? C32 C31 Zr1 72.03(17) . . ? C35 C31 Zr1 74.05(17) . . ? C32 C31 H31 125.7 . . ? C35 C31 H31 125.7 . . ? Zr1 C31 H31 120.0 . . ? C31 C32 C33 108.0(3) . . ? C31 C32 Zr1 75.88(18) . . ? C33 C32 Zr1 72.90(16) . . ? C31 C32 H32 126.0 . . ? C33 C32 H32 126.0 . . ? Zr1 C32 H32 117.2 . . ? C34 C33 C32 108.1(3) . . ? C34 C33 Zr1 75.95(15) . . ? C32 C33 Zr1 74.01(16) . . ? C34 C33 H33 126.0 . . ? C32 C33 H33 126.0 . . ? Zr1 C33 H33 116.2 . . ? C33 C34 C35 108.0(3) . . ? C33 C34 Zr1 71.69(16) . . ? C35 C34 Zr1 74.27(16) . . ? C33 C34 H34 126.0 . . ? C35 C34 H34 126.0 . . ? Zr1 C34 H34 119.9 . . ? C31 C35 C34 107.4(3) . . ? C31 C35 Zr1 73.78(17) . . ? C34 C35 Zr1 73.31(16) . . ? C31 C35 H35 126.3 . . ? C34 C35 H35 126.3 . . ? Zr1 C35 H35 118.6 . . ? C42 C41 C45 105.4(3) . . ? C42 C41 B2 125.8(3) . . ? C45 C41 B2 128.6(3) . . ? C42 C41 Fe2 68.20(17) . . ? C45 C41 Fe2 68.75(17) . . ? B2 C41 Fe2 122.96(19) . . ? C43 C42 C41 109.4(3) . . ? C43 C42 Fe2 69.94(17) . . ? C41 C42 Fe2 70.70(16) . . ? C43 C42 H42 125.3 . . ? C41 C42 H42 125.3 . . ? Fe2 C42 H42 125.7 . . ? C44 C43 C42 108.0(3) . . ? C44 C43 Fe2 70.49(17) . . ? C42 C43 Fe2 69.00(16) . . ? C44 C43 H43 126.0 . . ? C42 C43 H43 126.0 . . ? Fe2 C43 H43 126.1 . . ? C43 C44 C45 107.7(3) . . ? C43 C44 Fe2 69.20(17) . . ? C45 C44 Fe2 69.04(17) . . ? C43 C44 H44 126.1 . . ? C45 C44 H44 126.1 . . ? Fe2 C44 H44 127.2 . . ? C44 C45 C41 109.4(3) . . ? C44 C45 Fe2 70.19(17) . . ? C41 C45 Fe2 70.18(16) . . ? C44 C45 H45 125.3 . . ? C41 C45 H45 125.3 . . ? Fe2 C45 H45 125.9 . . ? C52 C51 C55 108.1(3) . . ? C52 C51 Fe2 69.31(19) . . ? C55 C51 Fe2 70.28(19) . . ? C52 C51 H51 125.9 . . ? C55 C51 H51 125.9 . . ? Fe2 C51 H51 126.0 . . ? C53 C52 C51 108.5(3) . . ? C53 C52 Fe2 70.3(2) . . ? C51 C52 Fe2 70.28(19) . . ? C53 C52 H52 125.8 . . ? C51 C52 H52 125.8 . . ? Fe2 C52 H52 125.3 . . ? C52 C53 C54 107.8(3) . . ? C52 C53 Fe2 69.4(2) . . ? C54 C53 Fe2 70.0(2) . . ? C52 C53 H53 126.1 . . ? C54 C53 H53 126.1 . . ? Fe2 C53 H53 126.1 . . ? C53 C54 C55 107.7(3) . . ? C53 C54 Fe2 69.5(2) . . ? C55 C54 Fe2 69.91(19) . . ? C53 C54 H54 126.2 . . ? C55 C54 H54 126.2 . . ? Fe2 C54 H54 126.0 . . ? C51 C55 C54 107.9(3) . . ? C51 C55 Fe2 69.55(19) . . ? C54 C55 Fe2 69.60(19) . . ? C51 C55 H55 126.0 . . ? C54 C55 H55 126.0 . . ? Fe2 C55 H55 126.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 Zr1 B1 C1 -47.3(3) . . . . ? C25 Zr1 B1 C1 -153.2(2) . . . . ? C23 Zr1 B1 C1 152.5(2) . . . . ? C32 Zr1 B1 C1 -71.8(3) . . . . ? C24 Zr1 B1 C1 -179.2(3) . . . . ? C22 Zr1 B1 C1 157.4(2) . . . . ? C21 Zr1 B1 C1 -162.9(2) . . . . ? C34 Zr1 B1 C1 -13.0(3) . . . . ? C31 Zr1 B1 C1 -54.4(2) . . . . ? C35 Zr1 B1 C1 -22.4(2) . . . . ? B2 Zr1 B1 C1 70.7(2) . . . . ? C33 Zr1 B2 C41 44.0(3) . . . . ? C25 Zr1 B2 C41 152.2(3) . . . . ? C23 Zr1 B2 C41 173.1(3) . . . . ? C32 Zr1 B2 C41 33.6(4) . . . . ? C24 Zr1 B2 C41 -176.4(3) . . . . ? C22 Zr1 B2 C41 139.9(3) . . . . ? C21 Zr1 B2 C41 125.5(3) . . . . ? C34 Zr1 B2 C41 18.6(3) . . . . ? C31 Zr1 B2 C41 -7.0(4) . . . . ? C35 Zr1 B2 C41 -10.1(3) . . . . ? B1 Zr1 B2 C41 -97.8(3) . . . . ? Zr1 B1 C1 C5 134.8(3) . . . . ? Zr1 B1 C1 C2 -48.0(4) . . . . ? Zr1 B1 C1 Fe1 -136.96(18) . . . . ? C2 Fe1 C1 C5 -117.1(3) . . . . ? C13 Fe1 C1 C5 -167.3(4) . . . . ? C14 Fe1 C1 C5 49.9(4) . . . . ? C4 Fe1 C1 C5 -36.98(18) . . . . ? C3 Fe1 C1 C5 -80.48(19) . . . . ? C11 Fe1 C1 C5 122.43(19) . . . . ? C15 Fe1 C1 C5 80.7(2) . . . . ? C12 Fe1 C1 C5 163.31(19) . . . . ? C5 Fe1 C1 C2 117.1(3) . . . . ? C13 Fe1 C1 C2 -50.3(4) . . . . ? C14 Fe1 C1 C2 166.9(3) . . . . ? C4 Fe1 C1 C2 80.1(2) . . . . ? C3 Fe1 C1 C2 36.61(19) . . . . ? C11 Fe1 C1 C2 -120.5(2) . . . . ? C15 Fe1 C1 C2 -162.27(19) . . . . ? C12 Fe1 C1 C2 -79.6(2) . . . . ? C5 Fe1 C1 B1 -121.0(3) . . . . ? C2 Fe1 C1 B1 121.9(3) . . . . ? C13 Fe1 C1 B1 71.6(5) . . . . ? C14 Fe1 C1 B1 -71.2(4) . . . . ? C4 Fe1 C1 B1 -158.0(3) . . . . ? C3 Fe1 C1 B1 158.5(3) . . . . ? C11 Fe1 C1 B1 1.4(3) . . . . ? C15 Fe1 C1 B1 -40.4(3) . . . . ? C12 Fe1 C1 B1 42.3(3) . . . . ? C5 C1 C2 C3 -0.4(3) . . . . ? B1 C1 C2 C3 -178.1(3) . . . . ? Fe1 C1 C2 C3 -59.2(2) . . . . ? C5 C1 C2 Fe1 58.77(19) . . . . ? B1 C1 C2 Fe1 -118.9(3) . . . . ? C5 Fe1 C2 C3 81.9(2) . . . . ? C13 Fe1 C2 C3 -77.2(2) . . . . ? C14 Fe1 C2 C3 -42.7(5) . . . . ? C4 Fe1 C2 C3 37.6(2) . . . . ? C11 Fe1 C2 C3 -161.6(2) . . . . ? C15 Fe1 C2 C3 163.4(3) . . . . ? C12 Fe1 C2 C3 -118.9(2) . . . . ? C1 Fe1 C2 C3 120.9(3) . . . . ? C5 Fe1 C2 C1 -39.01(18) . . . . ? C13 Fe1 C2 C1 161.89(19) . . . . ? C14 Fe1 C2 C1 -163.7(4) . . . . ? C4 Fe1 C2 C1 -83.3(2) . . . . ? C3 Fe1 C2 C1 -120.9(3) . . . . ? C11 Fe1 C2 C1 77.5(2) . . . . ? C15 Fe1 C2 C1 42.5(4) . . . . ? C12 Fe1 C2 C1 120.1(2) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? Fe1 C2 C3 C4 -59.2(2) . . . . ? C1 C2 C3 Fe1 59.5(2) . . . . ? C5 Fe1 C3 C2 -81.0(2) . . . . ? C13 Fe1 C3 C2 122.7(2) . . . . ? C14 Fe1 C3 C2 164.7(2) . . . . ? C4 Fe1 C3 C2 -119.3(3) . . . . ? C11 Fe1 C3 C2 45.3(5) . . . . ? C15 Fe1 C3 C2 -160.7(4) . . . . ? C12 Fe1 C3 C2 80.4(2) . . . . ? C1 Fe1 C3 C2 -36.94(19) . . . . ? C5 Fe1 C3 C4 38.3(2) . . . . ? C2 Fe1 C3 C4 119.3(3) . . . . ? C13 Fe1 C3 C4 -118.0(2) . . . . ? C14 Fe1 C3 C4 -76.0(2) . . . . ? C11 Fe1 C3 C4 164.6(3) . . . . ? C15 Fe1 C3 C4 -41.3(5) . . . . ? C12 Fe1 C3 C4 -160.3(2) . . . . ? C1 Fe1 C3 C4 82.4(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Fe1 C3 C4 C5 -59.2(2) . . . . ? C2 C3 C4 Fe1 59.1(2) . . . . ? C5 Fe1 C4 C3 -118.5(3) . . . . ? C2 Fe1 C4 C3 -37.6(2) . . . . ? C13 Fe1 C4 C3 81.1(2) . . . . ? C14 Fe1 C4 C3 123.1(2) . . . . ? C11 Fe1 C4 C3 -163.0(4) . . . . ? C15 Fe1 C4 C3 164.6(2) . . . . ? C12 Fe1 C4 C3 48.6(4) . . . . ? C1 Fe1 C4 C3 -81.6(2) . . . . ? C2 Fe1 C4 C5 80.9(2) . . . . ? C13 Fe1 C4 C5 -160.35(19) . . . . ? C14 Fe1 C4 C5 -118.4(2) . . . . ? C3 Fe1 C4 C5 118.5(3) . . . . ? C11 Fe1 C4 C5 -44.5(5) . . . . ? C15 Fe1 C4 C5 -76.9(2) . . . . ? C12 Fe1 C4 C5 167.1(3) . . . . ? C1 Fe1 C4 C5 36.97(18) . . . . ? C3 C4 C5 C1 -0.1(3) . . . . ? Fe1 C4 C5 C1 -59.8(2) . . . . ? C3 C4 C5 Fe1 59.7(2) . . . . ? C2 C1 C5 C4 0.3(3) . . . . ? B1 C1 C5 C4 178.0(3) . . . . ? Fe1 C1 C5 C4 59.2(2) . . . . ? C2 C1 C5 Fe1 -58.92(19) . . . . ? B1 C1 C5 Fe1 118.8(3) . . . . ? C2 Fe1 C5 C4 -81.8(2) . . . . ? C13 Fe1 C5 C4 48.3(4) . . . . ? C14 Fe1 C5 C4 80.2(2) . . . . ? C3 Fe1 C5 C4 -37.95(19) . . . . ? C11 Fe1 C5 C4 163.37(19) . . . . ? C15 Fe1 C5 C4 121.9(2) . . . . ? C12 Fe1 C5 C4 -165.6(4) . . . . ? C1 Fe1 C5 C4 -120.7(3) . . . . ? C2 Fe1 C5 C1 38.97(18) . . . . ? C13 Fe1 C5 C1 169.0(3) . . . . ? C14 Fe1 C5 C1 -159.05(18) . . . . ? C4 Fe1 C5 C1 120.7(3) . . . . ? C3 Fe1 C5 C1 82.79(19) . . . . ? C11 Fe1 C5 C1 -75.9(2) . . . . ? C15 Fe1 C5 C1 -117.35(19) . . . . ? C12 Fe1 C5 C1 -44.9(5) . . . . ? C5 Fe1 C11 C12 164.4(2) . . . . ? C2 Fe1 C11 C12 81.1(2) . . . . ? C13 Fe1 C11 C12 -37.5(2) . . . . ? C14 Fe1 C11 C12 -81.3(2) . . . . ? C4 Fe1 C11 C12 -162.2(4) . . . . ? C3 Fe1 C11 C12 48.1(5) . . . . ? C15 Fe1 C11 C12 -118.9(3) . . . . ? C1 Fe1 C11 C12 122.9(2) . . . . ? C5 Fe1 C11 C15 -76.7(2) . . . . ? C2 Fe1 C11 C15 -160.0(2) . . . . ? C13 Fe1 C11 C15 81.4(2) . . . . ? C14 Fe1 C11 C15 37.6(2) . . . . ? C4 Fe1 C11 C15 -43.4(5) . . . . ? C3 Fe1 C11 C15 167.0(3) . . . . ? C12 Fe1 C11 C15 118.9(3) . . . . ? C1 Fe1 C11 C15 -118.2(2) . . . . ? C15 C11 C12 C13 -0.6(3) . . . . ? Fe1 C11 C12 C13 59.1(2) . . . . ? C15 C11 C12 Fe1 -59.7(2) . . . . ? C5 Fe1 C12 C13 -160.8(4) . . . . ? C2 Fe1 C12 C13 122.7(2) . . . . ? C14 Fe1 C12 C13 -37.7(2) . . . . ? C4 Fe1 C12 C13 44.7(4) . . . . ? C3 Fe1 C12 C13 80.1(2) . . . . ? C11 Fe1 C12 C13 -119.3(3) . . . . ? C15 Fe1 C12 C13 -81.5(2) . . . . ? C1 Fe1 C12 C13 165.49(19) . . . . ? C5 Fe1 C12 C11 -41.5(5) . . . . ? C2 Fe1 C12 C11 -118.0(2) . . . . ? C13 Fe1 C12 C11 119.3(3) . . . . ? C14 Fe1 C12 C11 81.6(2) . . . . ? C4 Fe1 C12 C11 164.0(3) . . . . ? C3 Fe1 C12 C11 -160.5(2) . . . . ? C15 Fe1 C12 C11 37.9(2) . . . . ? C1 Fe1 C12 C11 -75.2(2) . . . . ? C11 C12 C13 C14 0.5(3) . . . . ? Fe1 C12 C13 C14 59.7(2) . . . . ? C11 C12 C13 Fe1 -59.2(2) . . . . ? C5 Fe1 C13 C12 163.0(3) . . . . ? C2 Fe1 C13 C12 -77.1(2) . . . . ? C14 Fe1 C13 C12 119.1(3) . . . . ? C4 Fe1 C13 C12 -161.7(2) . . . . ? C3 Fe1 C13 C12 -119.0(2) . . . . ? C11 Fe1 C13 C12 37.6(2) . . . . ? C15 Fe1 C13 C12 81.5(2) . . . . ? C1 Fe1 C13 C12 -39.1(5) . . . . ? C5 Fe1 C13 C14 43.9(4) . . . . ? C2 Fe1 C13 C14 163.81(19) . . . . ? C4 Fe1 C13 C14 79.2(2) . . . . ? C3 Fe1 C13 C14 121.9(2) . . . . ? C11 Fe1 C13 C14 -81.5(2) . . . . ? C15 Fe1 C13 C14 -37.58(19) . . . . ? C12 Fe1 C13 C14 -119.1(3) . . . . ? C1 Fe1 C13 C14 -158.2(3) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? Fe1 C13 C14 C15 59.7(2) . . . . ? C12 C13 C14 Fe1 -59.9(2) . . . . ? C5 Fe1 C14 C13 -161.9(2) . . . . ? C2 Fe1 C14 C13 -45.5(5) . . . . ? C4 Fe1 C14 C13 -119.3(2) . . . . ? C3 Fe1 C14 C13 -77.8(2) . . . . ? C11 Fe1 C14 C13 81.4(2) . . . . ? C15 Fe1 C14 C13 119.2(3) . . . . ? C12 Fe1 C14 C13 37.6(2) . . . . ? C1 Fe1 C14 C13 162.1(3) . . . . ? C5 Fe1 C14 C15 78.9(2) . . . . ? C2 Fe1 C14 C15 -164.7(4) . . . . ? C13 Fe1 C14 C15 -119.2(3) . . . . ? C4 Fe1 C14 C15 121.5(2) . . . . ? C3 Fe1 C14 C15 162.9(2) . . . . ? C11 Fe1 C14 C15 -37.8(2) . . . . ? C12 Fe1 C14 C15 -81.6(2) . . . . ? C1 Fe1 C14 C15 42.8(4) . . . . ? C13 C14 C15 C11 -0.1(3) . . . . ? Fe1 C14 C15 C11 59.3(2) . . . . ? C13 C14 C15 Fe1 -59.5(2) . . . . ? C12 C11 C15 C14 0.4(3) . . . . ? Fe1 C11 C15 C14 -59.3(2) . . . . ? C12 C11 C15 Fe1 59.7(2) . . . . ? C5 Fe1 C15 C14 -119.1(2) . . . . ? C2 Fe1 C15 C14 167.4(3) . . . . ? C13 Fe1 C15 C14 37.6(2) . . . . ? C4 Fe1 C15 C14 -77.2(2) . . . . ? C3 Fe1 C15 C14 -46.2(5) . . . . ? C11 Fe1 C15 C14 119.1(3) . . . . ? C12 Fe1 C15 C14 81.3(2) . . . . ? C1 Fe1 C15 C14 -161.67(19) . . . . ? C5 Fe1 C15 C11 121.8(2) . . . . ? C2 Fe1 C15 C11 48.3(4) . . . . ? C13 Fe1 C15 C11 -81.4(2) . . . . ? C14 Fe1 C15 C11 -119.1(3) . . . . ? C4 Fe1 C15 C11 163.7(2) . . . . ? C3 Fe1 C15 C11 -165.3(4) . . . . ? C12 Fe1 C15 C11 -37.8(2) . . . . ? C1 Fe1 C15 C11 79.2(2) . . . . ? C33 Zr1 C21 C22 122.51(19) . . . . ? C25 Zr1 C21 C22 -115.2(3) . . . . ? C23 Zr1 C21 C22 -37.08(18) . . . . ? C32 Zr1 C21 C22 156.2(2) . . . . ? C24 Zr1 C21 C22 -77.56(19) . . . . ? C34 Zr1 C21 C22 111.00(18) . . . . ? C31 Zr1 C21 C22 167.86(18) . . . . ? C35 Zr1 C21 C22 139.83(19) . . . . ? B2 Zr1 C21 C22 27.2(2) . . . . ? B1 Zr1 C21 C22 -97.0(2) . . . . ? C33 Zr1 C21 C25 -122.33(19) . . . . ? C23 Zr1 C21 C25 78.08(19) . . . . ? C32 Zr1 C21 C25 -88.64(18) . . . . ? C24 Zr1 C21 C25 37.60(18) . . . . ? C22 Zr1 C21 C25 115.2(3) . . . . ? C34 Zr1 C21 C25 -133.85(18) . . . . ? C31 Zr1 C21 C25 -76.98(19) . . . . ? C35 Zr1 C21 C25 -105.0(2) . . . . ? B2 Zr1 C21 C25 142.36(17) . . . . ? B1 Zr1 C21 C25 18.2(2) . . . . ? C25 C21 C22 C23 0.1(4) . . . . ? Zr1 C21 C22 C23 65.3(2) . . . . ? C25 C21 C22 Zr1 -65.2(2) . . . . ? C33 Zr1 C22 C21 -56.66(19) . . . . ? C25 Zr1 C22 C21 37.20(18) . . . . ? C23 Zr1 C22 C21 115.5(3) . . . . ? C32 Zr1 C22 C21 -24.8(2) . . . . ? C24 Zr1 C22 C21 78.1(2) . . . . ? C34 Zr1 C22 C21 -83.2(2) . . . . ? C31 Zr1 C22 C21 -18.2(3) . . . . ? C35 Zr1 C22 C21 -74.1(3) . . . . ? B2 Zr1 C22 C21 -153.9(2) . . . . ? B1 Zr1 C22 C21 106.4(2) . . . . ? C33 Zr1 C22 C23 -172.1(2) . . . . ? C25 Zr1 C22 C23 -78.3(2) . . . . ? C32 Zr1 C22 C23 -140.26(19) . . . . ? C24 Zr1 C22 C23 -37.36(19) . . . . ? C21 Zr1 C22 C23 -115.5(3) . . . . ? C34 Zr1 C22 C23 161.34(19) . . . . ? C31 Zr1 C22 C23 -133.7(2) . . . . ? C35 Zr1 C22 C23 170.4(2) . . . . ? B2 Zr1 C22 C23 90.6(2) . . . . ? B1 Zr1 C22 C23 -9.1(2) . . . . ? C21 C22 C23 C24 1.0(4) . . . . ? Zr1 C22 C23 C24 67.0(2) . . . . ? C21 C22 C23 Zr1 -66.0(2) . . . . ? C33 Zr1 C23 C24 -104.1(2) . . . . ? C25 Zr1 C23 C24 -37.10(18) . . . . ? C32 Zr1 C23 C24 -60.1(2) . . . . ? C22 Zr1 C23 C24 -114.3(3) . . . . ? C21 Zr1 C23 C24 -77.7(2) . . . . ? C34 Zr1 C23 C24 -146.3(2) . . . . ? C31 Zr1 C23 C24 -18.1(3) . . . . ? B2 Zr1 C23 C24 161.7(2) . . . . ? B1 Zr1 C23 C24 58.1(2) . . . . ? C33 Zr1 C23 C22 10.2(3) . . . . ? C25 Zr1 C23 C22 77.2(2) . . . . ? C32 Zr1 C23 C22 54.2(2) . . . . ? C24 Zr1 C23 C22 114.3(3) . . . . ? C21 Zr1 C23 C22 36.60(19) . . . . ? C34 Zr1 C23 C22 -32.0(3) . . . . ? C31 Zr1 C23 C22 96.2(3) . . . . ? B2 Zr1 C23 C22 -83.9(2) . . . . ? B1 Zr1 C23 C22 172.4(2) . . . . ? C22 C23 C24 C25 -1.7(3) . . . . ? Zr1 C23 C24 C25 65.5(2) . . . . ? C22 C23 C24 Zr1 -67.2(2) . . . . ? C33 Zr1 C24 C23 103.9(2) . . . . ? C25 Zr1 C24 C23 115.4(3) . . . . ? C32 Zr1 C24 C23 136.15(19) . . . . ? C22 Zr1 C24 C23 37.62(18) . . . . ? C21 Zr1 C24 C23 77.9(2) . . . . ? C34 Zr1 C24 C23 105.0(4) . . . . ? C31 Zr1 C24 C23 170.40(18) . . . . ? C35 Zr1 C24 C23 -171.1(2) . . . . ? B2 Zr1 C24 C23 -19.6(2) . . . . ? B1 Zr1 C24 C23 -118.2(2) . . . . ? C33 Zr1 C24 C25 -11.4(2) . . . . ? C23 Zr1 C24 C25 -115.4(3) . . . . ? C32 Zr1 C24 C25 20.8(2) . . . . ? C22 Zr1 C24 C25 -77.7(2) . . . . ? C21 Zr1 C24 C25 -37.44(18) . . . . ? C34 Zr1 C24 C25 -10.3(4) . . . . ? C31 Zr1 C24 C25 55.0(2) . . . . ? C35 Zr1 C24 C25 73.6(3) . . . . ? B2 Zr1 C24 C25 -135.00(19) . . . . ? B1 Zr1 C24 C25 126.4(2) . . . . ? C22 C21 C25 C24 -1.2(3) . . . . ? Zr1 C21 C25 C24 -67.0(2) . . . . ? C22 C21 C25 Zr1 65.9(2) . . . . ? C23 C24 C25 C21 1.8(3) . . . . ? Zr1 C24 C25 C21 67.4(2) . . . . ? C23 C24 C25 Zr1 -65.6(2) . . . . ? C33 Zr1 C25 C21 56.84(18) . . . . ? C23 Zr1 C25 C21 -77.55(19) . . . . ? C32 Zr1 C25 C21 85.29(19) . . . . ? C24 Zr1 C25 C21 -114.3(3) . . . . ? C22 Zr1 C25 C21 -36.80(17) . . . . ? C34 Zr1 C25 C21 61.6(2) . . . . ? C31 Zr1 C25 C21 111.22(18) . . . . ? C35 Zr1 C25 C21 104.4(2) . . . . ? B2 Zr1 C25 C21 -51.8(2) . . . . ? B1 Zr1 C25 C21 -165.40(18) . . . . ? C33 Zr1 C25 C24 171.16(19) . . . . ? C23 Zr1 C25 C24 36.77(18) . . . . ? C32 Zr1 C25 C24 -160.4(2) . . . . ? C22 Zr1 C25 C24 77.5(2) . . . . ? C21 Zr1 C25 C24 114.3(3) . . . . ? C34 Zr1 C25 C24 175.91(18) . . . . ? C31 Zr1 C25 C24 -134.47(19) . . . . ? C35 Zr1 C25 C24 -141.27(19) . . . . ? B2 Zr1 C25 C24 62.5(2) . . . . ? B1 Zr1 C25 C24 -51.1(2) . . . . ? C33 Zr1 C31 C32 38.11(19) . . . . ? C25 Zr1 C31 C32 -54.2(2) . . . . ? C23 Zr1 C31 C32 -69.8(3) . . . . ? C24 Zr1 C31 C32 -81.0(2) . . . . ? C22 Zr1 C31 C32 -11.7(3) . . . . ? C21 Zr1 C31 C32 -21.9(2) . . . . ? C34 Zr1 C31 C32 78.6(2) . . . . ? C35 Zr1 C31 C32 116.1(3) . . . . ? B2 Zr1 C31 C32 110.4(2) . . . . ? B1 Zr1 C31 C32 -148.0(2) . . . . ? C33 Zr1 C31 C35 -78.0(2) . . . . ? C25 Zr1 C31 C35 -170.3(2) . . . . ? C23 Zr1 C31 C35 174.1(2) . . . . ? C32 Zr1 C31 C35 -116.1(3) . . . . ? C24 Zr1 C31 C35 162.89(18) . . . . ? C22 Zr1 C31 C35 -127.8(2) . . . . ? C21 Zr1 C31 C35 -138.06(19) . . . . ? C34 Zr1 C31 C35 -37.49(19) . . . . ? B2 Zr1 C31 C35 -5.7(2) . . . . ? B1 Zr1 C31 C35 95.9(2) . . . . ? C35 C31 C32 C33 -0.8(3) . . . . ? Zr1 C31 C32 C33 -66.40(19) . . . . ? C35 C31 C32 Zr1 65.6(2) . . . . ? C33 Zr1 C32 C31 -114.2(3) . . . . ? C25 Zr1 C32 C31 125.7(2) . . . . ? C23 Zr1 C32 C31 144.5(2) . . . . ? C24 Zr1 C32 C31 114.4(2) . . . . ? C22 Zr1 C32 C31 172.16(19) . . . . ? C21 Zr1 C32 C31 159.0(2) . . . . ? C34 Zr1 C32 C31 -76.9(2) . . . . ? C35 Zr1 C32 C31 -36.41(19) . . . . ? B2 Zr1 C32 C31 -95.3(2) . . . . ? B1 Zr1 C32 C31 34.0(2) . . . . ? C25 Zr1 C32 C33 -120.1(2) . . . . ? C23 Zr1 C32 C33 -101.3(2) . . . . ? C24 Zr1 C32 C33 -131.35(19) . . . . ? C22 Zr1 C32 C33 -73.6(2) . . . . ? C21 Zr1 C32 C33 -86.8(2) . . . . ? C34 Zr1 C32 C33 37.31(18) . . . . ? C31 Zr1 C32 C33 114.2(3) . . . . ? C35 Zr1 C32 C33 77.8(2) . . . . ? B2 Zr1 C32 C33 18.9(3) . . . . ? B1 Zr1 C32 C33 148.21(19) . . . . ? C31 C32 C33 C34 -0.6(3) . . . . ? Zr1 C32 C33 C34 -68.96(19) . . . . ? C31 C32 C33 Zr1 68.4(2) . . . . ? C25 Zr1 C33 C34 173.14(19) . . . . ? C23 Zr1 C33 C34 -137.87(19) . . . . ? C32 Zr1 C33 C34 113.8(3) . . . . ? C24 Zr1 C33 C34 179.37(18) . . . . ? C22 Zr1 C33 C34 -132.34(19) . . . . ? C21 Zr1 C33 C34 -159.4(2) . . . . ? C31 Zr1 C33 C34 76.9(2) . . . . ? C35 Zr1 C33 C34 36.78(19) . . . . ? B2 Zr1 C33 C34 -51.6(2) . . . . ? B1 Zr1 C33 C34 68.2(2) . . . . ? C25 Zr1 C33 C32 59.3(2) . . . . ? C23 Zr1 C33 C32 108.3(2) . . . . ? C24 Zr1 C33 C32 65.5(2) . . . . ? C22 Zr1 C33 C32 113.8(2) . . . . ? C21 Zr1 C33 C32 86.7(2) . . . . ? C34 Zr1 C33 C32 -113.8(3) . . . . ? C31 Zr1 C33 C32 -36.9(2) . . . . ? C35 Zr1 C33 C32 -77.1(2) . . . . ? B2 Zr1 C33 C32 -165.5(2) . . . . ? B1 Zr1 C33 C32 -45.6(3) . . . . ? C32 C33 C34 C35 1.7(3) . . . . ? Zr1 C33 C34 C35 -65.94(19) . . . . ? C32 C33 C34 Zr1 67.65(19) . . . . ? C25 Zr1 C34 C33 -8.8(2) . . . . ? C23 Zr1 C34 C33 74.8(3) . . . . ? C32 Zr1 C34 C33 -38.19(18) . . . . ? C24 Zr1 C34 C33 -1.6(4) . . . . ? C22 Zr1 C34 C33 55.9(2) . . . . ? C21 Zr1 C34 C33 21.5(2) . . . . ? C31 Zr1 C34 C33 -78.3(2) . . . . ? C35 Zr1 C34 C33 -115.5(3) . . . . ? B2 Zr1 C34 C33 127.6(2) . . . . ? B1 Zr1 C34 C33 -133.13(19) . . . . ? C33 Zr1 C34 C35 115.5(3) . . . . ? C25 Zr1 C34 C35 106.7(2) . . . . ? C23 Zr1 C34 C35 -169.7(2) . . . . ? C32 Zr1 C34 C35 77.4(2) . . . . ? C24 Zr1 C34 C35 114.0(4) . . . . ? C22 Zr1 C34 C35 171.43(19) . . . . ? C21 Zr1 C34 C35 137.0(2) . . . . ? C31 Zr1 C34 C35 37.2(2) . . . . ? B2 Zr1 C34 C35 -116.9(2) . . . . ? B1 Zr1 C34 C35 -17.6(2) . . . . ? C32 C31 C35 C34 1.9(3) . . . . ? Zr1 C31 C35 C34 66.13(19) . . . . ? C32 C31 C35 Zr1 -64.3(2) . . . . ? C33 C34 C35 C31 -2.2(3) . . . . ? Zr1 C34 C35 C31 -66.4(2) . . . . ? C33 C34 C35 Zr1 64.24(19) . . . . ? C33 Zr1 C35 C31 77.7(2) . . . . ? C25 Zr1 C35 C31 12.7(3) . . . . ? C32 Zr1 C35 C31 36.31(19) . . . . ? C24 Zr1 C35 C31 -30.9(3) . . . . ? C22 Zr1 C35 C31 99.3(3) . . . . ? C21 Zr1 C35 C31 56.4(2) . . . . ? C34 Zr1 C35 C31 114.4(3) . . . . ? B2 Zr1 C35 C31 175.4(2) . . . . ? B1 Zr1 C35 C31 -81.1(2) . . . . ? C33 Zr1 C35 C34 -36.70(19) . . . . ? C25 Zr1 C35 C34 -101.7(2) . . . . ? C32 Zr1 C35 C34 -78.0(2) . . . . ? C24 Zr1 C35 C34 -145.2(2) . . . . ? C22 Zr1 C35 C34 -15.1(3) . . . . ? C21 Zr1 C35 C34 -57.9(3) . . . . ? C31 Zr1 C35 C34 -114.4(3) . . . . ? B2 Zr1 C35 C34 61.0(2) . . . . ? B1 Zr1 C35 C34 164.5(2) . . . . ? Zr1 B2 C41 C42 -155.2(2) . . . . ? Zr1 B2 C41 C45 31.3(5) . . . . ? Zr1 B2 C41 Fe2 119.3(2) . . . . ? C52 Fe2 C41 C42 -79.2(2) . . . . ? C43 Fe2 C41 C42 37.33(17) . . . . ? C45 Fe2 C41 C42 117.6(2) . . . . ? C53 Fe2 C41 C42 -49.0(4) . . . . ? C51 Fe2 C41 C42 -120.54(19) . . . . ? C54 Fe2 C41 C42 169.2(3) . . . . ? C55 Fe2 C41 C42 -161.27(18) . . . . ? C44 Fe2 C41 C42 80.53(18) . . . . ? C42 Fe2 C41 C45 -117.6(2) . . . . ? C52 Fe2 C41 C45 163.3(2) . . . . ? C43 Fe2 C41 C45 -80.26(19) . . . . ? C53 Fe2 C41 C45 -166.6(3) . . . . ? C51 Fe2 C41 C45 121.9(2) . . . . ? C54 Fe2 C41 C45 51.6(4) . . . . ? C55 Fe2 C41 C45 81.1(2) . . . . ? C44 Fe2 C41 C45 -37.06(18) . . . . ? C42 Fe2 C41 B2 119.4(3) . . . . ? C52 Fe2 C41 B2 40.2(3) . . . . ? C43 Fe2 C41 B2 156.7(3) . . . . ? C45 Fe2 C41 B2 -123.0(3) . . . . ? C53 Fe2 C41 B2 70.4(4) . . . . ? C51 Fe2 C41 B2 -1.1(3) . . . . ? C54 Fe2 C41 B2 -71.4(5) . . . . ? C55 Fe2 C41 B2 -41.9(3) . . . . ? C44 Fe2 C41 B2 -160.1(3) . . . . ? C45 C41 C42 C43 -0.4(3) . . . . ? B2 C41 C42 C43 -175.1(3) . . . . ? Fe2 C41 C42 C43 -59.4(2) . . . . ? C45 C41 C42 Fe2 58.97(19) . . . . ? B2 C41 C42 Fe2 -115.7(3) . . . . ? C52 Fe2 C42 C43 -121.0(2) . . . . ? C45 Fe2 C42 C43 81.4(2) . . . . ? C53 Fe2 C42 C43 -79.8(2) . . . . ? C51 Fe2 C42 C43 -162.3(2) . . . . ? C54 Fe2 C42 C43 -49.5(4) . . . . ? C55 Fe2 C42 C43 167.8(3) . . . . ? C44 Fe2 C42 C43 37.41(19) . . . . ? C41 Fe2 C42 C43 120.2(2) . . . . ? C52 Fe2 C42 C41 118.8(2) . . . . ? C43 Fe2 C42 C41 -120.2(2) . . . . ? C45 Fe2 C42 C41 -38.77(17) . . . . ? C53 Fe2 C42 C41 159.99(19) . . . . ? C51 Fe2 C42 C41 77.5(2) . . . . ? C54 Fe2 C42 C41 -169.7(3) . . . . ? C55 Fe2 C42 C41 47.6(4) . . . . ? C44 Fe2 C42 C41 -82.77(18) . . . . ? C41 C42 C43 C44 -0.1(3) . . . . ? Fe2 C42 C43 C44 -59.9(2) . . . . ? C41 C42 C43 Fe2 59.9(2) . . . . ? C42 Fe2 C43 C44 119.2(3) . . . . ? C52 Fe2 C43 C44 -163.6(2) . . . . ? C45 Fe2 C43 C44 37.64(19) . . . . ? C53 Fe2 C43 C44 -121.9(2) . . . . ? C51 Fe2 C43 C44 164.1(4) . . . . ? C54 Fe2 C43 C44 -80.2(2) . . . . ? C55 Fe2 C43 C44 -48.1(5) . . . . ? C41 Fe2 C43 C44 81.8(2) . . . . ? C52 Fe2 C43 C42 77.2(2) . . . . ? C45 Fe2 C43 C42 -81.52(19) . . . . ? C53 Fe2 C43 C42 118.9(2) . . . . ? C51 Fe2 C43 C42 44.9(5) . . . . ? C54 Fe2 C43 C42 160.69(19) . . . . ? C55 Fe2 C43 C42 -167.2(4) . . . . ? C44 Fe2 C43 C42 -119.2(3) . . . . ? C41 Fe2 C43 C42 -37.37(17) . . . . ? C42 C43 C44 C45 0.6(3) . . . . ? Fe2 C43 C44 C45 -58.5(2) . . . . ? C42 C43 C44 Fe2 59.0(2) . . . . ? C42 Fe2 C44 C43 -38.09(19) . . . . ? C52 Fe2 C44 C43 41.6(5) . . . . ? C45 Fe2 C44 C43 -119.6(3) . . . . ? C53 Fe2 C44 C43 76.8(2) . . . . ? C51 Fe2 C44 C43 -163.3(4) . . . . ? C54 Fe2 C44 C43 119.3(2) . . . . ? C55 Fe2 C44 C43 161.6(2) . . . . ? C41 Fe2 C44 C43 -82.3(2) . . . . ? C42 Fe2 C44 C45 81.54(19) . . . . ? C52 Fe2 C44 C45 161.2(4) . . . . ? C43 Fe2 C44 C45 119.6(3) . . . . ? C53 Fe2 C44 C45 -163.58(19) . . . . ? C51 Fe2 C44 C45 -43.7(5) . . . . ? C54 Fe2 C44 C45 -121.1(2) . . . . ? C55 Fe2 C44 C45 -78.7(2) . . . . ? C41 Fe2 C44 C45 37.31(18) . . . . ? C43 C44 C45 C41 -0.9(3) . . . . ? Fe2 C44 C45 C41 -59.4(2) . . . . ? C43 C44 C45 Fe2 58.6(2) . . . . ? C42 C41 C45 C44 0.8(3) . . . . ? B2 C41 C45 C44 175.3(3) . . . . ? Fe2 C41 C45 C44 59.4(2) . . . . ? C42 C41 C45 Fe2 -58.61(19) . . . . ? B2 C41 C45 Fe2 115.9(3) . . . . ? C42 Fe2 C45 C44 -81.55(19) . . . . ? C52 Fe2 C45 C44 -161.9(4) . . . . ? C43 Fe2 C45 C44 -37.22(19) . . . . ? C53 Fe2 C45 C44 44.3(5) . . . . ? C51 Fe2 C45 C44 163.3(2) . . . . ? C54 Fe2 C45 C44 79.0(2) . . . . ? C55 Fe2 C45 C44 121.2(2) . . . . ? C41 Fe2 C45 C44 -120.4(3) . . . . ? C42 Fe2 C45 C41 38.81(17) . . . . ? C52 Fe2 C45 C41 -41.6(4) . . . . ? C43 Fe2 C45 C41 83.13(18) . . . . ? C53 Fe2 C45 C41 164.7(4) . . . . ? C51 Fe2 C45 C41 -76.4(2) . . . . ? C54 Fe2 C45 C41 -160.66(18) . . . . ? C55 Fe2 C45 C41 -118.49(19) . . . . ? C44 Fe2 C45 C41 120.4(3) . . . . ? C42 Fe2 C51 C52 77.2(3) . . . . ? C43 Fe2 C51 C52 44.0(5) . . . . ? C45 Fe2 C51 C52 160.9(2) . . . . ? C53 Fe2 C51 C52 -37.6(2) . . . . ? C54 Fe2 C51 C52 -81.5(3) . . . . ? C55 Fe2 C51 C52 -119.2(3) . . . . ? C44 Fe2 C51 C52 -166.6(4) . . . . ? C41 Fe2 C51 C52 119.2(2) . . . . ? C42 Fe2 C51 C55 -163.5(2) . . . . ? C52 Fe2 C51 C55 119.2(3) . . . . ? C43 Fe2 C51 C55 163.2(3) . . . . ? C45 Fe2 C51 C55 -79.9(3) . . . . ? C53 Fe2 C51 C55 81.6(2) . . . . ? C54 Fe2 C51 C55 37.7(2) . . . . ? C44 Fe2 C51 C55 -47.3(5) . . . . ? C41 Fe2 C51 C55 -121.6(2) . . . . ? C55 C51 C52 C53 0.3(4) . . . . ? Fe2 C51 C52 C53 60.1(2) . . . . ? C55 C51 C52 Fe2 -59.8(2) . . . . ? C42 Fe2 C52 C53 120.3(2) . . . . ? C43 Fe2 C52 C53 78.4(3) . . . . ? C45 Fe2 C52 C53 -166.7(3) . . . . ? C51 Fe2 C52 C53 -119.1(3) . . . . ? C54 Fe2 C52 C53 -37.8(2) . . . . ? C55 Fe2 C52 C53 -81.7(2) . . . . ? C44 Fe2 C52 C53 47.8(5) . . . . ? C41 Fe2 C52 C53 162.7(2) . . . . ? C42 Fe2 C52 C51 -120.6(2) . . . . ? C43 Fe2 C52 C51 -162.5(2) . . . . ? C45 Fe2 C52 C51 -47.6(5) . . . . ? C53 Fe2 C52 C51 119.1(3) . . . . ? C54 Fe2 C52 C51 81.3(2) . . . . ? C55 Fe2 C52 C51 37.4(2) . . . . ? C44 Fe2 C52 C51 166.9(3) . . . . ? C41 Fe2 C52 C51 -78.2(2) . . . . ? C51 C52 C53 C54 -0.5(4) . . . . ? Fe2 C52 C53 C54 59.6(2) . . . . ? C51 C52 C53 Fe2 -60.1(2) . . . . ? C42 Fe2 C53 C52 -77.4(3) . . . . ? C43 Fe2 C53 C52 -120.1(2) . . . . ? C45 Fe2 C53 C52 165.3(4) . . . . ? C51 Fe2 C53 C52 37.7(2) . . . . ? C54 Fe2 C53 C52 119.0(3) . . . . ? C55 Fe2 C53 C52 81.2(2) . . . . ? C44 Fe2 C53 C52 -161.4(2) . . . . ? C41 Fe2 C53 C52 -41.6(4) . . . . ? C42 Fe2 C53 C54 163.6(2) . . . . ? C52 Fe2 C53 C54 -119.0(3) . . . . ? C43 Fe2 C53 C54 120.9(2) . . . . ? C45 Fe2 C53 C54 46.3(5) . . . . ? C51 Fe2 C53 C54 -81.4(2) . . . . ? C55 Fe2 C53 C54 -37.9(2) . . . . ? C44 Fe2 C53 C54 79.5(2) . . . . ? C41 Fe2 C53 C54 -160.6(3) . . . . ? C52 C53 C54 C55 0.5(4) . . . . ? Fe2 C53 C54 C55 59.7(2) . . . . ? C52 C53 C54 Fe2 -59.3(2) . . . . ? C42 Fe2 C54 C53 -41.2(5) . . . . ? C52 Fe2 C54 C53 37.6(2) . . . . ? C43 Fe2 C54 C53 -77.8(3) . . . . ? C45 Fe2 C54 C53 -162.9(2) . . . . ? C51 Fe2 C54 C53 81.4(2) . . . . ? C55 Fe2 C54 C53 118.8(3) . . . . ? C44 Fe2 C54 C53 -120.2(2) . . . . ? C41 Fe2 C54 C53 158.5(3) . . . . ? C42 Fe2 C54 C55 -160.0(3) . . . . ? C52 Fe2 C54 C55 -81.2(2) . . . . ? C43 Fe2 C54 C55 163.4(2) . . . . ? C45 Fe2 C54 C55 78.3(2) . . . . ? C53 Fe2 C54 C55 -118.8(3) . . . . ? C51 Fe2 C54 C55 -37.4(2) . . . . ? C44 Fe2 C54 C55 121.0(2) . . . . ? C41 Fe2 C54 C55 39.7(5) . . . . ? C52 C51 C55 C54 0.0(4) . . . . ? Fe2 C51 C55 C54 -59.2(2) . . . . ? C52 C51 C55 Fe2 59.2(2) . . . . ? C53 C54 C55 C51 -0.3(4) . . . . ? Fe2 C54 C55 C51 59.2(2) . . . . ? C53 C54 C55 Fe2 -59.5(2) . . . . ? C42 Fe2 C55 C51 40.9(5) . . . . ? C52 Fe2 C55 C51 -37.6(2) . . . . ? C43 Fe2 C55 C51 -162.5(4) . . . . ? C45 Fe2 C55 C51 119.3(2) . . . . ? C53 Fe2 C55 C51 -81.4(3) . . . . ? C54 Fe2 C55 C51 -119.3(3) . . . . ? C44 Fe2 C55 C51 161.9(2) . . . . ? C41 Fe2 C55 C51 76.1(3) . . . . ? C42 Fe2 C55 C54 160.1(3) . . . . ? C52 Fe2 C55 C54 81.6(2) . . . . ? C43 Fe2 C55 C54 -43.2(5) . . . . ? C45 Fe2 C55 C54 -121.4(2) . . . . ? C53 Fe2 C55 C54 37.9(2) . . . . ? C51 Fe2 C55 C54 119.3(3) . . . . ? C44 Fe2 C55 C54 -78.9(3) . . . . ? C41 Fe2 C55 C54 -164.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.305 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.079 data_wa1295 _database_code_depnum_ccdc_archive 'CCDC 894222' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H41 B3 Fe3 Zr' _chemical_formula_sum 'C35 H41 B3 Fe3 Zr' _chemical_formula_weight 752.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5811(3) _cell_length_b 20.6944(11) _cell_length_c 23.8678(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.260(4) _cell_angle_gamma 90.00 _cell_volume 3250.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10402 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.7 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6647 _exptl_absorpt_correction_T_max 0.9370 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 25275 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5738 _reflns_number_gt 3513 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0842P)^2^] 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 5738 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 Zr1 Zr 0.20575(12) 0.70042(4) 0.71556(3) 0.0269(2) Uani 1 1 d . . . Fe1 Fe -0.1143(2) 0.47136(6) 0.64305(5) 0.0368(3) Uani 1 1 d . . . Fe2 Fe 0.5321(2) 0.74769(6) 0.51723(5) 0.0398(3) Uani 1 1 d . . . Fe3 Fe 0.54012(19) 0.53838(5) 0.87852(5) 0.0331(3) Uani 1 1 d . . . B1 B 0.0301(17) 0.6164(5) 0.6675(4) 0.038(2) Uani 1 1 d . . . H1A H 0.1742 0.6064 0.6621 0.058 Uiso 1 1 calc R . . H1B H -0.0042 0.6116 0.7072 0.058 Uiso 1 1 calc R . . H1C H 0.0031 0.6609 0.6555 0.058 Uiso 1 1 calc R . . B2 B 0.4327(16) 0.7391(5) 0.6459(4) 0.038(2) Uani 1 1 d . . . H2A H 0.4555 0.7607 0.6819 0.057 Uiso 1 1 calc R . . H2B H 0.4855 0.6949 0.6477 0.057 Uiso 1 1 calc R . . H2C H 0.2868 0.7380 0.6376 0.057 Uiso 1 1 calc R . . B3 B 0.4194(15) 0.6454(5) 0.7825(4) 0.040(2) Uani 1 1 d . . . H3A H 0.2741 0.6388 0.7892 0.060 Uiso 1 1 calc R . . H3B H 0.4620 0.6195 0.7503 0.060 Uiso 1 1 calc R . . H3C H 0.4447 0.6913 0.7748 0.060 Uiso 1 1 calc R . . C1 C -0.1275(19) 0.7492(6) 0.7352(7) 0.081(4) Uani 1 1 d . . . H1 H -0.2466 0.7286 0.7214 0.097 Uiso 1 1 calc R . . C2 C -0.036(2) 0.7374(5) 0.7865(6) 0.072(4) Uani 1 1 d . . . H2 H -0.0778 0.7067 0.8136 0.086 Uiso 1 1 calc R . . C3 C 0.1360(18) 0.7803(5) 0.7909(4) 0.053(3) Uani 1 1 d . . . H3 H 0.2287 0.7839 0.8214 0.063 Uiso 1 1 calc R . . C4 C 0.1378(15) 0.8153(4) 0.7415(4) 0.044(2) Uani 1 1 d . . . H4 H 0.2327 0.8482 0.7323 0.053 Uiso 1 1 calc R . . C5 C -0.0195(19) 0.7949(5) 0.7080(5) 0.058(3) Uani 1 1 d . . . H5 H -0.0481 0.8105 0.6714 0.070 Uiso 1 1 calc R . . C11 C -0.1023(15) 0.5688(4) 0.6319(4) 0.042(2) Uani 1 1 d . . . C12 C -0.3055(17) 0.5480(5) 0.6436(5) 0.063(3) Uani 1 1 d . . . H12 H -0.3861 0.5620 0.6742 0.075 Uiso 1 1 calc R . . C13 C -0.3655(18) 0.5033(6) 0.6020(6) 0.071(3) Uani 1 1 d . . . H13 H -0.4929 0.4818 0.5999 0.086 Uiso 1 1 calc R . . C14 C -0.206(3) 0.4960(6) 0.5645(5) 0.081(4) Uani 1 1 d . . . H14 H -0.2065 0.4689 0.5323 0.098 Uiso 1 1 calc R . . C15 C -0.0422(18) 0.5362(5) 0.5825(4) 0.052(2) Uani 1 1 d . . . H15 H 0.0855 0.5404 0.5645 0.062 Uiso 1 1 calc R . . C16 C 0.108(2) 0.4492(5) 0.6988(5) 0.069(3) Uani 1 1 d . . . H16 H 0.2076 0.4784 0.7129 0.082 Uiso 1 1 calc R . . C17 C -0.082(3) 0.4384(6) 0.7231(5) 0.081(4) Uani 1 1 d . . . H17 H -0.1357 0.4590 0.7555 0.097 Uiso 1 1 calc R . . C18 C -0.176(2) 0.3928(7) 0.6912(6) 0.084(4) Uani 1 1 d . . . H18 H -0.3053 0.3749 0.6991 0.101 Uiso 1 1 calc R . . C19 C -0.057(2) 0.3755(5) 0.6454(6) 0.074(4) Uani 1 1 d . . . H19 H -0.0914 0.3464 0.6161 0.088 Uiso 1 1 calc R . . C20 C 0.1316(18) 0.4120(5) 0.6525(5) 0.067(3) Uani 1 1 d . . . H20 H 0.2479 0.4100 0.6291 0.080 Uiso 1 1 calc R . . C21 C 0.5440(13) 0.7767(4) 0.5991(3) 0.0343(18) Uani 1 1 d . . . C22 C 0.7453(14) 0.7642(5) 0.5776(3) 0.042(2) Uani 1 1 d . . . H22 H 0.8390 0.7332 0.5918 0.050 Uiso 1 1 calc R . . C23 C 0.7780(16) 0.8062(5) 0.5316(4) 0.051(2) Uani 1 1 d . . . H23 H 0.8983 0.8085 0.5098 0.062 Uiso 1 1 calc R . . C24 C 0.6040(15) 0.8438(5) 0.5238(4) 0.046(2) Uani 1 1 d . . . H24 H 0.5849 0.8755 0.4955 0.055 Uiso 1 1 calc R . . C25 C 0.4617(15) 0.8266(4) 0.5649(3) 0.039(2) Uani 1 1 d . . . H25 H 0.3310 0.8454 0.5692 0.047 Uiso 1 1 calc R . . C26 C 0.389(3) 0.6607(8) 0.5170(5) 0.089(5) Uani 1 1 d . . . H26 H 0.3489 0.6373 0.5493 0.106 Uiso 1 1 calc R . . C27 C 0.574(3) 0.6555(6) 0.4904(5) 0.085(5) Uani 1 1 d . . . H27 H 0.6841 0.6283 0.5012 0.102 Uiso 1 1 calc R . . C28 C 0.571(3) 0.6975(7) 0.4449(4) 0.088(5) Uani 1 1 d . . . H28 H 0.6780 0.7024 0.4187 0.106 Uiso 1 1 calc R . . C29 C 0.395(4) 0.7301(7) 0.4435(6) 0.115(8) Uani 1 1 d . . . H29 H 0.3585 0.7630 0.4176 0.138 Uiso 1 1 calc R . . C30 C 0.272(3) 0.7060(10) 0.4884(8) 0.111(6) Uani 1 1 d . . . H30 H 0.1372 0.7186 0.4970 0.133 Uiso 1 1 calc R . . C31 C 0.5435(12) 0.6242(4) 0.8358(3) 0.0331(18) Uani 1 1 d . . . C32 C 0.7395(14) 0.5945(4) 0.8351(4) 0.041(2) Uani 1 1 d . . . H32 H 0.8129 0.5820 0.8027 0.049 Uiso 1 1 calc R . . C33 C 0.8059(15) 0.5867(4) 0.8919(4) 0.042(2) Uani 1 1 d . . . H33 H 0.9309 0.5678 0.9033 0.050 Uiso 1 1 calc R . . C34 C 0.6586(16) 0.6112(4) 0.9274(4) 0.046(2) Uani 1 1 d . . . H34 H 0.6650 0.6126 0.9672 0.055 Uiso 1 1 calc R . . C35 C 0.4948(13) 0.6342(4) 0.8929(3) 0.0371(19) Uani 1 1 d . . . H35 H 0.3727 0.6531 0.9063 0.045 Uiso 1 1 calc R . . C36 C 0.4671(19) 0.4595(5) 0.8311(5) 0.057(3) Uani 1 1 d . . . H36 H 0.4926 0.4542 0.7922 0.068 Uiso 1 1 calc R . . C37 C 0.5987(19) 0.4423(4) 0.8752(4) 0.055(3) Uani 1 1 d . . . H37 H 0.7297 0.4236 0.8713 0.066 Uiso 1 1 calc R . . C38 C 0.5047(19) 0.4573(5) 0.9257(4) 0.057(3) Uani 1 1 d . . . H38 H 0.5606 0.4503 0.9620 0.069 Uiso 1 1 calc R . . C39 C 0.3140(16) 0.4844(5) 0.9142(4) 0.053(2) Uani 1 1 d . . . H39 H 0.2186 0.4990 0.9411 0.063 Uiso 1 1 calc R . . C40 C 0.2884(18) 0.4864(5) 0.8554(5) 0.060(3) Uani 1 1 d . . . H40 H 0.1735 0.5026 0.8357 0.072 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 Zr1 0.0246(4) 0.0277(4) 0.0283(4) 0.0012(3) -0.0017(3) 0.0019(3) Fe1 0.0337(7) 0.0319(6) 0.0447(7) -0.0021(5) -0.0004(5) -0.0028(5) Fe2 0.0461(8) 0.0441(7) 0.0292(6) 0.0003(5) -0.0019(5) 0.0061(6) Fe3 0.0347(7) 0.0309(6) 0.0335(6) 0.0018(5) -0.0055(5) 0.0011(5) B1 0.045(6) 0.028(5) 0.042(5) 0.003(4) -0.009(4) 0.000(4) B2 0.039(6) 0.045(6) 0.030(5) -0.001(4) -0.005(4) 0.003(4) B3 0.028(5) 0.047(6) 0.044(5) 0.015(4) -0.012(4) -0.002(4) C1 0.037(7) 0.066(8) 0.140(12) -0.053(8) -0.016(7) 0.028(6) C2 0.082(9) 0.035(6) 0.098(9) -0.009(5) 0.071(8) 0.000(5) C3 0.067(7) 0.049(6) 0.042(5) -0.016(4) 0.003(5) 0.007(5) C4 0.044(6) 0.036(5) 0.053(5) -0.015(4) 0.006(4) 0.000(4) C5 0.062(7) 0.042(6) 0.071(7) -0.009(5) -0.014(5) 0.022(6) C11 0.038(5) 0.039(5) 0.048(5) -0.004(4) -0.008(4) -0.002(4) C12 0.043(6) 0.046(6) 0.100(8) -0.010(5) -0.015(6) 0.011(5) C13 0.041(6) 0.061(7) 0.112(10) 0.012(7) -0.030(7) -0.006(5) C14 0.132(13) 0.061(7) 0.050(6) 0.008(5) -0.030(7) -0.046(8) C15 0.065(7) 0.046(5) 0.044(5) -0.001(4) -0.008(4) -0.007(5) C16 0.070(9) 0.048(6) 0.088(8) 0.017(6) -0.029(7) -0.008(6) C17 0.120(13) 0.065(8) 0.059(7) 0.017(6) 0.004(7) -0.007(8) C18 0.063(9) 0.068(8) 0.122(11) 0.038(8) 0.016(8) -0.016(7) C19 0.092(10) 0.033(6) 0.096(9) -0.017(5) -0.015(7) 0.008(6) C20 0.048(7) 0.047(6) 0.105(9) -0.004(6) 0.001(6) 0.012(5) C21 0.031(5) 0.037(4) 0.035(4) -0.003(3) -0.005(3) -0.003(4) C22 0.035(5) 0.056(6) 0.035(4) 0.009(4) 0.003(4) 0.008(4) C23 0.041(6) 0.074(7) 0.039(5) 0.014(5) 0.006(4) -0.001(5) C24 0.046(6) 0.050(6) 0.042(5) 0.015(4) -0.002(4) -0.007(5) C25 0.048(6) 0.035(4) 0.035(4) 0.002(3) 0.001(4) 0.000(4) C26 0.129(15) 0.079(10) 0.058(7) -0.024(7) 0.009(9) -0.052(10) C27 0.139(15) 0.053(7) 0.064(7) -0.023(6) -0.017(8) 0.028(8) C28 0.151(15) 0.073(8) 0.041(6) -0.014(6) 0.023(7) 0.032(9) C29 0.23(2) 0.055(8) 0.060(8) -0.024(6) -0.062(11) 0.047(11) C30 0.083(11) 0.133(15) 0.116(13) -0.084(12) -0.006(10) -0.011(11) C31 0.025(4) 0.036(4) 0.038(4) 0.005(3) -0.005(3) 0.002(4) C32 0.034(5) 0.051(5) 0.039(4) 0.006(4) 0.001(4) -0.002(4) C33 0.037(5) 0.043(5) 0.046(5) 0.007(4) -0.011(4) 0.001(4) C34 0.060(7) 0.042(5) 0.036(4) -0.004(4) -0.007(4) -0.005(5) C35 0.031(5) 0.039(5) 0.041(4) 0.001(4) -0.008(4) 0.003(4) C36 0.072(8) 0.035(5) 0.062(6) -0.006(4) -0.013(5) -0.005(5) C37 0.063(7) 0.031(5) 0.070(7) -0.002(4) -0.012(5) 0.004(5) C38 0.077(8) 0.043(6) 0.052(6) 0.014(4) -0.006(5) -0.011(5) C39 0.044(6) 0.050(6) 0.064(6) 0.010(5) 0.001(5) -0.002(5) C40 0.058(7) 0.042(6) 0.079(7) 0.006(5) -0.015(5) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C2 2.448(9) . ? Zr1 C5 2.460(10) . ? Zr1 C1 2.461(11) . ? Zr1 C3 2.487(8) . ? Zr1 C4 2.498(8) . ? Fe1 C19 2.019(10) . ? Fe1 C12 2.025(10) . ? Fe1 C16 2.028(12) . ? Fe1 C13 2.029(11) . ? Fe1 C15 2.029(10) . ? Fe1 C18 2.032(11) . ? Fe1 C14 2.033(11) . ? Fe1 C11 2.035(9) . ? Fe1 C17 2.039(12) . ? Fe1 C20 2.043(11) . ? Fe2 C29 2.006(13) . ? Fe2 C26 2.030(13) . ? Fe2 C28 2.031(10) . ? Fe2 C30 2.031(16) . ? Fe2 C27 2.031(11) . ? Fe2 C22 2.036(9) . ? Fe2 C25 2.045(9) . ? Fe2 C21 2.046(8) . ? Fe2 C23 2.050(11) . ? Fe2 C24 2.050(10) . ? Fe3 C37 2.027(9) . ? Fe3 C38 2.035(9) . ? Fe3 C35 2.035(9) . ? Fe3 C32 2.038(9) . ? Fe3 C33 2.039(10) . ? Fe3 C36 2.042(10) . ? Fe3 C39 2.048(10) . ? Fe3 C31 2.049(8) . ? Fe3 C40 2.049(11) . ? Fe3 C34 2.058(9) . ? B1 C11 1.564(13) . ? B1 H1A 0.9800 . ? B1 H1B 0.9800 . ? B1 H1C 0.9800 . ? B2 C21 1.547(12) . ? B2 H2A 0.9800 . ? B2 H2B 0.9800 . ? B2 H2C 0.9800 . ? B3 C31 1.571(12) . ? B3 H3A 0.9800 . ? B3 H3B 0.9800 . ? B3 H3C 0.9800 . ? C1 C5 1.351(19) . ? C1 C2 1.385(19) . ? C1 H1 0.9500 . ? C2 C3 1.441(17) . ? C2 H2 0.9500 . ? C3 C4 1.384(14) . ? C3 H3 0.9500 . ? C4 C5 1.372(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C15 1.414(13) . ? C11 C12 1.433(15) . ? C12 C13 1.414(16) . ? C12 H12 0.9500 . ? C13 C14 1.389(19) . ? C13 H13 0.9500 . ? C14 C15 1.429(16) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C20 1.358(17) . ? C16 C17 1.40(2) . ? C16 H16 0.9500 . ? C17 C18 1.359(19) . ? C17 H17 0.9500 . ? C18 C19 1.391(18) . ? C18 H18 0.9500 . ? C19 C20 1.463(18) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C25 1.422(12) . ? C21 C22 1.446(12) . ? C22 C23 1.418(12) . ? C22 H22 0.9500 . ? C23 C24 1.396(14) . ? C23 H23 0.9500 . ? C24 C25 1.406(12) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.38(2) . ? C26 C30 1.39(2) . ? C26 H26 0.9500 . ? C27 C28 1.391(17) . ? C27 H27 0.9500 . ? C28 C29 1.34(2) . ? C28 H28 0.9500 . ? C29 C30 1.43(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C35 1.417(11) . ? C31 C32 1.429(12) . ? C32 C33 1.430(12) . ? C32 H32 0.9500 . ? C33 C34 1.388(14) . ? C33 H33 0.9500 . ? C34 C35 1.435(13) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.407(15) . ? C36 C40 1.427(17) . ? C36 H36 0.9500 . ? C37 C38 1.392(15) . ? C37 H37 0.9500 . ? C38 C39 1.402(16) . ? C38 H38 0.9500 . ? C39 C40 1.413(15) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Zr1 C5 53.8(4) . . ? C2 Zr1 C1 32.8(5) . . ? C5 Zr1 C1 31.9(4) . . ? C2 Zr1 C3 33.9(4) . . ? C5 Zr1 C3 54.0(4) . . ? C1 Zr1 C3 54.7(4) . . ? C2 Zr1 C4 54.1(3) . . ? C5 Zr1 C4 32.1(4) . . ? C1 Zr1 C4 53.3(4) . . ? C3 Zr1 C4 32.2(3) . . ? C19 Fe1 C12 152.2(5) . . ? C19 Fe1 C16 68.0(5) . . ? C12 Fe1 C16 128.3(5) . . ? C19 Fe1 C13 119.0(5) . . ? C12 Fe1 C13 40.8(5) . . ? C16 Fe1 C13 167.4(6) . . ? C19 Fe1 C15 128.7(5) . . ? C12 Fe1 C15 68.5(5) . . ? C16 Fe1 C15 116.5(5) . . ? C13 Fe1 C15 68.5(5) . . ? C19 Fe1 C18 40.2(5) . . ? C12 Fe1 C18 119.9(6) . . ? C16 Fe1 C18 66.0(6) . . ? C13 Fe1 C18 111.7(6) . . ? C15 Fe1 C18 168.2(5) . . ? C19 Fe1 C14 109.1(5) . . ? C12 Fe1 C14 68.1(6) . . ? C16 Fe1 C14 150.9(6) . . ? C13 Fe1 C14 40.0(6) . . ? C15 Fe1 C14 41.2(4) . . ? C18 Fe1 C14 131.5(6) . . ? C19 Fe1 C11 165.7(5) . . ? C12 Fe1 C11 41.3(4) . . ? C16 Fe1 C11 106.4(4) . . ? C13 Fe1 C11 69.3(4) . . ? C15 Fe1 C11 40.7(4) . . ? C18 Fe1 C11 151.0(5) . . ? C14 Fe1 C11 69.0(4) . . ? C19 Fe1 C17 68.1(5) . . ? C12 Fe1 C17 108.5(6) . . ? C16 Fe1 C17 40.4(6) . . ? C13 Fe1 C17 129.9(6) . . ? C15 Fe1 C17 149.8(5) . . ? C18 Fe1 C17 39.0(6) . . ? C14 Fe1 C17 167.8(6) . . ? C11 Fe1 C17 116.7(5) . . ? C19 Fe1 C20 42.2(5) . . ? C12 Fe1 C20 164.2(5) . . ? C16 Fe1 C20 39.0(5) . . ? C13 Fe1 C20 153.1(5) . . ? C15 Fe1 C20 106.8(5) . . ? C18 Fe1 C20 67.4(5) . . ? C14 Fe1 C20 119.0(6) . . ? C11 Fe1 C20 125.4(4) . . ? C17 Fe1 C20 67.6(6) . . ? C29 Fe2 C26 68.3(7) . . ? C29 Fe2 C28 38.8(7) . . ? C26 Fe2 C28 66.7(6) . . ? C29 Fe2 C30 41.6(8) . . ? C26 Fe2 C30 40.1(7) . . ? C28 Fe2 C30 66.7(7) . . ? C29 Fe2 C27 67.4(5) . . ? C26 Fe2 C27 39.7(6) . . ? C28 Fe2 C27 40.1(5) . . ? C30 Fe2 C27 67.1(7) . . ? C29 Fe2 C22 163.1(8) . . ? C26 Fe2 C22 117.9(6) . . ? C28 Fe2 C22 126.7(6) . . ? C30 Fe2 C22 152.5(7) . . ? C27 Fe2 C22 106.5(5) . . ? C29 Fe2 C25 122.1(5) . . ? C26 Fe2 C25 127.1(5) . . ? C28 Fe2 C25 155.6(5) . . ? C30 Fe2 C25 109.6(5) . . ? C27 Fe2 C25 163.1(5) . . ? C22 Fe2 C25 68.2(4) . . ? C29 Fe2 C21 155.0(7) . . ? C26 Fe2 C21 106.2(4) . . ? C28 Fe2 C21 163.2(5) . . ? C30 Fe2 C21 118.4(6) . . ? C27 Fe2 C21 124.9(4) . . ? C22 Fe2 C21 41.5(3) . . ? C25 Fe2 C21 40.7(3) . . ? C29 Fe2 C23 127.3(7) . . ? C26 Fe2 C23 152.8(7) . . ? C28 Fe2 C23 110.0(6) . . ? C30 Fe2 C23 166.0(8) . . ? C27 Fe2 C23 119.9(6) . . ? C22 Fe2 C23 40.6(4) . . ? C25 Fe2 C23 67.4(4) . . ? C21 Fe2 C23 68.8(3) . . ? C29 Fe2 C24 110.2(5) . . ? C26 Fe2 C24 165.2(7) . . ? C28 Fe2 C24 122.0(5) . . ? C30 Fe2 C24 129.1(7) . . ? C27 Fe2 C24 154.5(6) . . ? C22 Fe2 C24 68.0(4) . . ? C25 Fe2 C24 40.2(4) . . ? C21 Fe2 C24 68.6(3) . . ? C23 Fe2 C24 39.8(4) . . ? C37 Fe3 C38 40.1(4) . . ? C37 Fe3 C35 172.1(4) . . ? C38 Fe3 C35 133.9(4) . . ? C37 Fe3 C32 114.6(4) . . ? C38 Fe3 C32 145.7(4) . . ? C35 Fe3 C32 68.0(4) . . ? C37 Fe3 C33 108.9(4) . . ? C38 Fe3 C33 114.7(4) . . ? C35 Fe3 C33 67.8(4) . . ? C32 Fe3 C33 41.1(3) . . ? C37 Fe3 C36 40.4(4) . . ? C38 Fe3 C36 67.7(4) . . ? C35 Fe3 C36 146.9(4) . . ? C32 Fe3 C36 108.9(4) . . ? C33 Fe3 C36 132.7(5) . . ? C37 Fe3 C39 67.7(5) . . ? C38 Fe3 C39 40.2(4) . . ? C35 Fe3 C39 110.7(4) . . ? C32 Fe3 C39 172.7(4) . . ? C33 Fe3 C39 145.8(4) . . ? C36 Fe3 C39 68.0(5) . . ? C37 Fe3 C31 146.0(4) . . ? C38 Fe3 C31 172.8(4) . . ? C35 Fe3 C31 40.6(3) . . ? C32 Fe3 C31 40.9(3) . . ? C33 Fe3 C31 68.9(3) . . ? C36 Fe3 C31 114.8(4) . . ? C39 Fe3 C31 133.5(4) . . ? C37 Fe3 C40 68.2(5) . . ? C38 Fe3 C40 67.8(5) . . ? C35 Fe3 C40 116.0(4) . . ? C32 Fe3 C40 133.1(4) . . ? C33 Fe3 C40 172.6(4) . . ? C36 Fe3 C40 40.8(5) . . ? C39 Fe3 C40 40.3(4) . . ? C31 Fe3 C40 109.4(4) . . ? C37 Fe3 C34 132.0(4) . . ? C38 Fe3 C34 109.5(4) . . ? C35 Fe3 C34 41.0(4) . . ? C32 Fe3 C34 68.1(4) . . ? C33 Fe3 C34 39.6(4) . . ? C36 Fe3 C34 170.9(5) . . ? C39 Fe3 C34 116.0(4) . . ? C31 Fe3 C34 69.0(3) . . ? C40 Fe3 C34 147.3(5) . . ? C11 B1 H1A 109.5 . . ? C11 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? C11 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? C21 B2 H2A 109.5 . . ? C21 B2 H2B 109.5 . . ? H2A B2 H2B 109.5 . . ? C21 B2 H2C 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? C31 B3 H3A 109.5 . . ? C31 B3 H3B 109.5 . . ? H3A B3 H3B 109.5 . . ? C31 B3 H3C 109.5 . . ? H3A B3 H3C 109.5 . . ? H3B B3 H3C 109.5 . . ? C5 C1 C2 108.6(11) . . ? C5 C1 Zr1 74.0(7) . . ? C2 C1 Zr1 73.1(6) . . ? C5 C1 H1 125.7 . . ? C2 C1 H1 125.7 . . ? Zr1 C1 H1 119.0 . . ? C1 C2 C3 107.2(10) . . ? C1 C2 Zr1 74.1(6) . . ? C3 C2 Zr1 74.5(5) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 126.4 . . ? Zr1 C2 H2 117.1 . . ? C4 C3 C2 105.6(10) . . ? C4 C3 Zr1 74.3(5) . . ? C2 C3 Zr1 71.5(5) . . ? C4 C3 H3 127.2 . . ? C2 C3 H3 127.2 . . ? Zr1 C3 H3 119.0 . . ? C5 C4 C3 109.0(10) . . ? C5 C4 Zr1 72.4(5) . . ? C3 C4 Zr1 73.4(5) . . ? C5 C4 H4 125.5 . . ? C3 C4 H4 125.5 . . ? Zr1 C4 H4 120.4 . . ? C1 C5 C4 109.5(10) . . ? C1 C5 Zr1 74.1(6) . . ? C4 C5 Zr1 75.5(6) . . ? C1 C5 H5 125.3 . . ? C4 C5 H5 125.3 . . ? Zr1 C5 H5 117.0 . . ? C15 C11 C12 106.6(9) . . ? C15 C11 B1 126.6(9) . . ? C12 C11 B1 126.8(9) . . ? C15 C11 Fe1 69.4(5) . . ? C12 C11 Fe1 69.0(6) . . ? B1 C11 Fe1 125.0(6) . . ? C13 C12 C11 108.4(10) . . ? C13 C12 Fe1 69.7(6) . . ? C11 C12 Fe1 69.7(6) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Fe1 C12 H12 126.4 . . ? C14 C13 C12 108.4(11) . . ? C14 C13 Fe1 70.2(7) . . ? C12 C13 Fe1 69.5(6) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Fe1 C13 H13 126.1 . . ? C13 C14 C15 108.3(10) . . ? C13 C14 Fe1 69.8(6) . . ? C15 C14 Fe1 69.3(6) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Fe1 C14 H14 126.6 . . ? C11 C15 C14 108.4(11) . . ? C11 C15 Fe1 69.9(5) . . ? C14 C15 Fe1 69.6(6) . . ? C11 C15 H15 125.8 . . ? C14 C15 H15 125.8 . . ? Fe1 C15 H15 126.3 . . ? C20 C16 C17 110.6(12) . . ? C20 C16 Fe1 71.1(7) . . ? C17 C16 Fe1 70.3(8) . . ? C20 C16 H16 124.7 . . ? C17 C16 H16 124.7 . . ? Fe1 C16 H16 125.5 . . ? C18 C17 C16 106.3(12) . . ? C18 C17 Fe1 70.2(7) . . ? C16 C17 Fe1 69.4(7) . . ? C18 C17 H17 126.9 . . ? C16 C17 H17 126.9 . . ? Fe1 C17 H17 125.1 . . ? C17 C18 C19 111.5(12) . . ? C17 C18 Fe1 70.8(7) . . ? C19 C18 Fe1 69.4(7) . . ? C17 C18 H18 124.2 . . ? C19 C18 H18 124.2 . . ? Fe1 C18 H18 127.2 . . ? C18 C19 C20 104.8(11) . . ? C18 C19 Fe1 70.4(7) . . ? C20 C19 Fe1 69.8(6) . . ? C18 C19 H19 127.6 . . ? C20 C19 H19 127.6 . . ? Fe1 C19 H19 123.9 . . ? C16 C20 C19 106.7(11) . . ? C16 C20 Fe1 69.9(7) . . ? C19 C20 Fe1 68.0(6) . . ? C16 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? Fe1 C20 H20 126.9 . . ? C25 C21 C22 105.9(7) . . ? C25 C21 B2 126.8(8) . . ? C22 C21 B2 127.0(8) . . ? C25 C21 Fe2 69.6(4) . . ? C22 C21 Fe2 68.9(5) . . ? B2 C21 Fe2 121.7(6) . . ? C23 C22 C21 107.8(8) . . ? C23 C22 Fe2 70.2(6) . . ? C21 C22 Fe2 69.6(5) . . ? C23 C22 H22 126.1 . . ? C21 C22 H22 126.1 . . ? Fe2 C22 H22 125.7 . . ? C24 C23 C22 108.6(8) . . ? C24 C23 Fe2 70.1(6) . . ? C22 C23 Fe2 69.2(6) . . ? C24 C23 H23 125.7 . . ? C22 C23 H23 125.7 . . ? Fe2 C23 H23 126.6 . . ? C23 C24 C25 108.3(8) . . ? C23 C24 Fe2 70.1(6) . . ? C25 C24 Fe2 69.7(5) . . ? C23 C24 H24 125.9 . . ? C25 C24 H24 125.9 . . ? Fe2 C24 H24 125.9 . . ? C24 C25 C21 109.4(8) . . ? C24 C25 Fe2 70.1(5) . . ? C21 C25 Fe2 69.7(5) . . ? C24 C25 H25 125.3 . . ? C21 C25 H25 125.3 . . ? Fe2 C25 H25 126.5 . . ? C27 C26 C30 108.4(13) . . ? C27 C26 Fe2 70.2(8) . . ? C30 C26 Fe2 70.0(9) . . ? C27 C26 H26 125.8 . . ? C30 C26 H26 125.8 . . ? Fe2 C26 H26 125.6 . . ? C26 C27 C28 107.4(14) . . ? C26 C27 Fe2 70.1(7) . . ? C28 C27 Fe2 69.9(7) . . ? C26 C27 H27 126.3 . . ? C28 C27 H27 126.3 . . ? Fe2 C27 H27 125.2 . . ? C29 C28 C27 110.2(15) . . ? C29 C28 Fe2 69.6(7) . . ? C27 C28 Fe2 70.0(6) . . ? C29 C28 H28 124.9 . . ? C27 C28 H28 124.9 . . ? Fe2 C28 H28 127.1 . . ? C28 C29 C30 107.2(14) . . ? C28 C29 Fe2 71.6(8) . . ? C30 C29 Fe2 70.1(8) . . ? C28 C29 H29 126.4 . . ? C30 C29 H29 126.4 . . ? Fe2 C29 H29 123.5 . . ? C26 C30 C29 106.7(15) . . ? C26 C30 Fe2 69.9(9) . . ? C29 C30 Fe2 68.3(10) . . ? C26 C30 H30 126.6 . . ? C29 C30 H30 126.6 . . ? Fe2 C30 H30 126.7 . . ? C35 C31 C32 106.4(7) . . ? C35 C31 B3 128.2(8) . . ? C32 C31 B3 125.3(7) . . ? C35 C31 Fe3 69.2(5) . . ? C32 C31 Fe3 69.1(5) . . ? B3 C31 Fe3 129.7(6) . . ? C31 C32 C33 108.1(8) . . ? C31 C32 Fe3 69.9(5) . . ? C33 C32 Fe3 69.5(5) . . ? C31 C32 H32 126.0 . . ? C33 C32 H32 126.0 . . ? Fe3 C32 H32 126.2 . . ? C34 C33 C32 109.1(9) . . ? C34 C33 Fe3 71.0(6) . . ? C32 C33 Fe3 69.5(5) . . ? C34 C33 H33 125.5 . . ? C32 C33 H33 125.5 . . ? Fe3 C33 H33 125.7 . . ? C33 C34 C35 107.2(8) . . ? C33 C34 Fe3 69.5(5) . . ? C35 C34 Fe3 68.6(5) . . ? C33 C34 H34 126.4 . . ? C35 C34 H34 126.4 . . ? Fe3 C34 H34 127.1 . . ? C31 C35 C34 109.3(8) . . ? C31 C35 Fe3 70.2(5) . . ? C34 C35 Fe3 70.3(5) . . ? C31 C35 H35 125.3 . . ? C34 C35 H35 125.3 . . ? Fe3 C35 H35 125.7 . . ? C37 C36 C40 107.5(10) . . ? C37 C36 Fe3 69.2(6) . . ? C40 C36 Fe3 69.8(6) . . ? C37 C36 H36 126.3 . . ? C40 C36 H36 126.3 . . ? Fe3 C36 H36 126.3 . . ? C38 C37 C36 108.5(11) . . ? C38 C37 Fe3 70.3(6) . . ? C36 C37 Fe3 70.4(6) . . ? C38 C37 H37 125.7 . . ? C36 C37 H37 125.7 . . ? Fe3 C37 H37 125.2 . . ? C37 C38 C39 108.7(10) . . ? C37 C38 Fe3 69.7(5) . . ? C39 C38 Fe3 70.4(6) . . ? C37 C38 H38 125.7 . . ? C39 C38 H38 125.7 . . ? Fe3 C38 H38 125.8 . . ? C38 C39 C40 108.0(10) . . ? C38 C39 Fe3 69.4(6) . . ? C40 C39 Fe3 69.9(6) . . ? C38 C39 H39 126.0 . . ? C40 C39 H39 126.0 . . ? Fe3 C39 H39 126.3 . . ? C39 C40 C36 107.3(10) . . ? C39 C40 Fe3 69.8(6) . . ? C36 C40 Fe3 69.3(6) . . ? C39 C40 H40 126.3 . . ? C36 C40 H40 126.3 . . ? Fe3 C40 H40 126.1 . . ? 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 C2 Zr1 C1 C5 115.7(10) . . . . ? C3 Zr1 C1 C5 76.9(7) . . . . ? C4 Zr1 C1 C5 36.8(6) . . . . ? C5 Zr1 C1 C2 -115.7(10) . . . . ? C3 Zr1 C1 C2 -38.9(6) . . . . ? C4 Zr1 C1 C2 -79.0(7) . . . . ? C5 C1 C2 C3 1.7(11) . . . . ? Zr1 C1 C2 C3 67.8(7) . . . . ? C5 C1 C2 Zr1 -66.1(8) . . . . ? C5 Zr1 C2 C1 36.1(7) . . . . ? C3 Zr1 C2 C1 113.4(10) . . . . ? C4 Zr1 C2 C1 76.1(8) . . . . ? C5 Zr1 C2 C3 -77.3(7) . . . . ? C1 Zr1 C2 C3 -113.4(10) . . . . ? C4 Zr1 C2 C3 -37.3(6) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? Zr1 C2 C3 C4 67.1(6) . . . . ? C1 C2 C3 Zr1 -67.5(7) . . . . ? C2 Zr1 C3 C4 -112.9(10) . . . . ? C5 Zr1 C3 C4 -35.9(7) . . . . ? C1 Zr1 C3 C4 -75.4(8) . . . . ? C5 Zr1 C3 C2 77.0(8) . . . . ? C1 Zr1 C3 C2 37.5(8) . . . . ? C4 Zr1 C3 C2 112.9(10) . . . . ? C2 C3 C4 C5 -1.0(10) . . . . ? Zr1 C3 C4 C5 64.2(7) . . . . ? C2 C3 C4 Zr1 -65.2(6) . . . . ? C2 Zr1 C4 C5 -77.4(8) . . . . ? C1 Zr1 C4 C5 -36.5(7) . . . . ? C3 Zr1 C4 C5 -116.8(10) . . . . ? C2 Zr1 C4 C3 39.4(8) . . . . ? C5 Zr1 C4 C3 116.8(10) . . . . ? C1 Zr1 C4 C3 80.4(8) . . . . ? C2 C1 C5 C4 -2.4(12) . . . . ? Zr1 C1 C5 C4 -67.8(7) . . . . ? C2 C1 C5 Zr1 65.5(7) . . . . ? C3 C4 C5 C1 2.1(11) . . . . ? Zr1 C4 C5 C1 66.9(7) . . . . ? C3 C4 C5 Zr1 -64.8(7) . . . . ? C2 Zr1 C5 C1 -37.2(7) . . . . ? C3 Zr1 C5 C1 -79.5(8) . . . . ? C4 Zr1 C5 C1 -115.6(10) . . . . ? C2 Zr1 C5 C4 78.4(7) . . . . ? C1 Zr1 C5 C4 115.6(10) . . . . ? C3 Zr1 C5 C4 36.1(6) . . . . ? C19 Fe1 C11 C15 47(2) . . . . ? C12 Fe1 C11 C15 -118.1(9) . . . . ? C16 Fe1 C11 C15 111.8(7) . . . . ? C13 Fe1 C11 C15 -80.7(7) . . . . ? C18 Fe1 C11 C15 -178.4(10) . . . . ? C14 Fe1 C11 C15 -37.8(8) . . . . ? C17 Fe1 C11 C15 154.0(8) . . . . ? C20 Fe1 C11 C15 73.6(8) . . . . ? C19 Fe1 C11 C12 165.2(18) . . . . ? C16 Fe1 C11 C12 -130.1(7) . . . . ? C13 Fe1 C11 C12 37.4(7) . . . . ? C15 Fe1 C11 C12 118.1(9) . . . . ? C18 Fe1 C11 C12 -60.3(12) . . . . ? C14 Fe1 C11 C12 80.3(8) . . . . ? C17 Fe1 C11 C12 -87.9(8) . . . . ? C20 Fe1 C11 C12 -168.3(7) . . . . ? C19 Fe1 C11 B1 -74(2) . . . . ? C12 Fe1 C11 B1 121.0(10) . . . . ? C16 Fe1 C11 B1 -9.1(9) . . . . ? C13 Fe1 C11 B1 158.4(10) . . . . ? C15 Fe1 C11 B1 -120.9(11) . . . . ? C18 Fe1 C11 B1 60.7(14) . . . . ? C14 Fe1 C11 B1 -158.7(10) . . . . ? C17 Fe1 C11 B1 33.0(10) . . . . ? C20 Fe1 C11 B1 -47.4(10) . . . . ? C15 C11 C12 C13 0.3(12) . . . . ? B1 C11 C12 C13 -177.9(9) . . . . ? Fe1 C11 C12 C13 -59.2(7) . . . . ? C15 C11 C12 Fe1 59.5(7) . . . . ? B1 C11 C12 Fe1 -118.7(9) . . . . ? C19 Fe1 C12 C13 -52.5(14) . . . . ? C16 Fe1 C12 C13 -171.0(8) . . . . ? C15 Fe1 C12 C13 81.5(8) . . . . ? C18 Fe1 C12 C13 -89.3(9) . . . . ? C14 Fe1 C12 C13 37.0(7) . . . . ? C11 Fe1 C12 C13 119.7(10) . . . . ? C17 Fe1 C12 C13 -130.5(8) . . . . ? C20 Fe1 C12 C13 156.9(17) . . . . ? C19 Fe1 C12 C11 -172.3(9) . . . . ? C16 Fe1 C12 C11 69.3(8) . . . . ? C13 Fe1 C12 C11 -119.7(10) . . . . ? C15 Fe1 C12 C11 -38.2(6) . . . . ? C18 Fe1 C12 C11 150.9(7) . . . . ? C14 Fe1 C12 C11 -82.7(7) . . . . ? C17 Fe1 C12 C11 109.8(7) . . . . ? C20 Fe1 C12 C11 37(2) . . . . ? C11 C12 C13 C14 -0.4(13) . . . . ? Fe1 C12 C13 C14 -59.6(9) . . . . ? C11 C12 C13 Fe1 59.1(7) . . . . ? C19 Fe1 C13 C14 -85.4(8) . . . . ? C12 Fe1 C13 C14 119.5(11) . . . . ? C16 Fe1 C13 C14 154(2) . . . . ? C15 Fe1 C13 C14 37.9(7) . . . . ? C18 Fe1 C13 C14 -129.4(8) . . . . ? C11 Fe1 C13 C14 81.7(7) . . . . ? C17 Fe1 C13 C14 -170.2(7) . . . . ? C20 Fe1 C13 C14 -46.8(14) . . . . ? C19 Fe1 C13 C12 155.0(8) . . . . ? C16 Fe1 C13 C12 34(3) . . . . ? C15 Fe1 C13 C12 -81.6(8) . . . . ? C18 Fe1 C13 C12 111.0(9) . . . . ? C14 Fe1 C13 C12 -119.5(11) . . . . ? C11 Fe1 C13 C12 -37.8(7) . . . . ? C17 Fe1 C13 C12 70.3(10) . . . . ? C20 Fe1 C13 C12 -166.3(10) . . . . ? C12 C13 C14 C15 0.3(14) . . . . ? Fe1 C13 C14 C15 -58.8(8) . . . . ? C12 C13 C14 Fe1 59.1(8) . . . . ? C19 Fe1 C14 C13 112.7(8) . . . . ? C12 Fe1 C14 C13 -37.8(7) . . . . ? C16 Fe1 C14 C13 -168.5(9) . . . . ? C15 Fe1 C14 C13 -119.7(11) . . . . ? C18 Fe1 C14 C13 73.4(10) . . . . ? C11 Fe1 C14 C13 -82.4(8) . . . . ? C17 Fe1 C14 C13 38(3) . . . . ? C20 Fe1 C14 C13 157.9(7) . . . . ? C19 Fe1 C14 C15 -127.6(8) . . . . ? C12 Fe1 C14 C15 81.9(8) . . . . ? C16 Fe1 C14 C15 -48.8(14) . . . . ? C13 Fe1 C14 C15 119.7(11) . . . . ? C18 Fe1 C14 C15 -166.9(7) . . . . ? C11 Fe1 C14 C15 37.4(7) . . . . ? C17 Fe1 C14 C15 158(2) . . . . ? C20 Fe1 C14 C15 -82.4(8) . . . . ? C12 C11 C15 C14 -0.1(12) . . . . ? B1 C11 C15 C14 178.1(9) . . . . ? Fe1 C11 C15 C14 59.1(8) . . . . ? C12 C11 C15 Fe1 -59.2(7) . . . . ? B1 C11 C15 Fe1 119.0(9) . . . . ? C13 C14 C15 C11 -0.1(13) . . . . ? Fe1 C14 C15 C11 -59.3(7) . . . . ? C13 C14 C15 Fe1 59.1(8) . . . . ? C19 Fe1 C15 C11 -166.6(7) . . . . ? C12 Fe1 C15 C11 38.8(6) . . . . ? C16 Fe1 C15 C11 -84.5(7) . . . . ? C13 Fe1 C15 C11 82.8(7) . . . . ? C18 Fe1 C15 C11 176(2) . . . . ? C14 Fe1 C15 C11 119.7(11) . . . . ? C17 Fe1 C15 C11 -51.2(13) . . . . ? C20 Fe1 C15 C11 -125.2(6) . . . . ? C19 Fe1 C15 C14 73.7(10) . . . . ? C12 Fe1 C15 C14 -80.9(9) . . . . ? C16 Fe1 C15 C14 155.9(9) . . . . ? C13 Fe1 C15 C14 -36.9(8) . . . . ? C18 Fe1 C15 C14 56(3) . . . . ? C11 Fe1 C15 C14 -119.7(11) . . . . ? C17 Fe1 C15 C14 -170.9(12) . . . . ? C20 Fe1 C15 C14 115.1(9) . . . . ? C19 Fe1 C16 C20 39.5(8) . . . . ? C12 Fe1 C16 C20 -166.7(7) . . . . ? C13 Fe1 C16 C20 165(2) . . . . ? C15 Fe1 C16 C20 -84.0(8) . . . . ? C18 Fe1 C16 C20 83.3(8) . . . . ? C14 Fe1 C16 C20 -50.4(12) . . . . ? C11 Fe1 C16 C20 -126.6(7) . . . . ? C17 Fe1 C16 C20 121.2(11) . . . . ? C19 Fe1 C16 C17 -81.7(8) . . . . ? C12 Fe1 C16 C17 72.2(9) . . . . ? C13 Fe1 C16 C17 44(2) . . . . ? C15 Fe1 C16 C17 154.8(7) . . . . ? C18 Fe1 C16 C17 -37.9(8) . . . . ? C14 Fe1 C16 C17 -171.6(9) . . . . ? C11 Fe1 C16 C17 112.2(8) . . . . ? C20 Fe1 C16 C17 -121.2(11) . . . . ? C20 C16 C17 C18 1.0(15) . . . . ? Fe1 C16 C17 C18 60.9(9) . . . . ? C20 C16 C17 Fe1 -59.9(9) . . . . ? C19 Fe1 C17 C18 -35.6(9) . . . . ? C12 Fe1 C17 C18 115.0(9) . . . . ? C16 Fe1 C17 C18 -117.0(12) . . . . ? C13 Fe1 C17 C18 74.5(11) . . . . ? C15 Fe1 C17 C18 -166.2(10) . . . . ? C14 Fe1 C17 C18 43(3) . . . . ? C11 Fe1 C17 C18 159.1(8) . . . . ? C20 Fe1 C17 C18 -81.4(9) . . . . ? C19 Fe1 C17 C16 81.3(8) . . . . ? C12 Fe1 C17 C16 -128.0(8) . . . . ? C13 Fe1 C17 C16 -168.5(7) . . . . ? C15 Fe1 C17 C16 -49.2(14) . . . . ? C18 Fe1 C17 C16 117.0(12) . . . . ? C14 Fe1 C17 C16 160(3) . . . . ? C11 Fe1 C17 C16 -84.0(8) . . . . ? C20 Fe1 C17 C16 35.6(7) . . . . ? C16 C17 C18 C19 -2.8(15) . . . . ? Fe1 C17 C18 C19 57.5(10) . . . . ? C16 C17 C18 Fe1 -60.3(8) . . . . ? C19 Fe1 C18 C17 123.0(13) . . . . ? C12 Fe1 C18 C17 -82.6(10) . . . . ? C16 Fe1 C18 C17 39.2(9) . . . . ? C13 Fe1 C18 C17 -127.3(10) . . . . ? C15 Fe1 C18 C17 144(2) . . . . ? C14 Fe1 C18 C17 -168.8(10) . . . . ? C11 Fe1 C18 C17 -41.1(15) . . . . ? C20 Fe1 C18 C17 81.7(10) . . . . ? C12 Fe1 C18 C19 154.4(8) . . . . ? C16 Fe1 C18 C19 -83.9(9) . . . . ? C13 Fe1 C18 C19 109.6(9) . . . . ? C15 Fe1 C18 C19 21(3) . . . . ? C14 Fe1 C18 C19 68.1(12) . . . . ? C11 Fe1 C18 C19 -164.2(9) . . . . ? C17 Fe1 C18 C19 -123.0(13) . . . . ? C20 Fe1 C18 C19 -41.3(8) . . . . ? C17 C18 C19 C20 3.4(15) . . . . ? Fe1 C18 C19 C20 61.7(8) . . . . ? C17 C18 C19 Fe1 -58.3(10) . . . . ? C12 Fe1 C19 C18 -53.6(14) . . . . ? C16 Fe1 C19 C18 78.3(9) . . . . ? C13 Fe1 C19 C18 -90.0(10) . . . . ? C15 Fe1 C19 C18 -174.6(8) . . . . ? C14 Fe1 C19 C18 -132.7(9) . . . . ? C11 Fe1 C19 C18 147.6(17) . . . . ? C17 Fe1 C19 C18 34.6(9) . . . . ? C20 Fe1 C19 C18 114.9(11) . . . . ? C12 Fe1 C19 C20 -168.5(10) . . . . ? C16 Fe1 C19 C20 -36.6(7) . . . . ? C13 Fe1 C19 C20 155.1(8) . . . . ? C15 Fe1 C19 C20 70.5(9) . . . . ? C18 Fe1 C19 C20 -114.9(11) . . . . ? C14 Fe1 C19 C20 112.5(8) . . . . ? C11 Fe1 C19 C20 33(2) . . . . ? C17 Fe1 C19 C20 -80.2(9) . . . . ? C17 C16 C20 C19 1.0(13) . . . . ? Fe1 C16 C20 C19 -58.3(8) . . . . ? C17 C16 C20 Fe1 59.3(9) . . . . ? C18 C19 C20 C16 -2.6(13) . . . . ? Fe1 C19 C20 C16 59.5(8) . . . . ? C18 C19 C20 Fe1 -62.1(8) . . . . ? C19 Fe1 C20 C16 -118.5(11) . . . . ? C12 Fe1 C20 C16 42(2) . . . . ? C13 Fe1 C20 C16 -173.0(10) . . . . ? C15 Fe1 C20 C16 111.7(7) . . . . ? C18 Fe1 C20 C16 -79.2(9) . . . . ? C14 Fe1 C20 C16 154.6(7) . . . . ? C11 Fe1 C20 C16 70.9(8) . . . . ? C17 Fe1 C20 C16 -36.8(8) . . . . ? C12 Fe1 C20 C19 160.1(17) . . . . ? C16 Fe1 C20 C19 118.5(11) . . . . ? C13 Fe1 C20 C19 -54.5(14) . . . . ? C15 Fe1 C20 C19 -129.8(7) . . . . ? C18 Fe1 C20 C19 39.3(8) . . . . ? C14 Fe1 C20 C19 -86.8(8) . . . . ? C11 Fe1 C20 C19 -170.6(7) . . . . ? C17 Fe1 C20 C19 81.7(8) . . . . ? C29 Fe2 C21 C25 -55.5(14) . . . . ? C26 Fe2 C21 C25 -128.8(8) . . . . ? C28 Fe2 C21 C25 168.7(18) . . . . ? C30 Fe2 C21 C25 -87.4(9) . . . . ? C27 Fe2 C21 C25 -168.1(8) . . . . ? C22 Fe2 C21 C25 117.2(7) . . . . ? C23 Fe2 C21 C25 79.5(6) . . . . ? C24 Fe2 C21 C25 36.6(6) . . . . ? C29 Fe2 C21 C22 -172.7(12) . . . . ? C26 Fe2 C21 C22 114.0(8) . . . . ? C28 Fe2 C21 C22 52(2) . . . . ? C30 Fe2 C21 C22 155.5(9) . . . . ? C27 Fe2 C21 C22 74.7(8) . . . . ? C25 Fe2 C21 C22 -117.2(7) . . . . ? C23 Fe2 C21 C22 -37.7(6) . . . . ? C24 Fe2 C21 C22 -80.6(6) . . . . ? C29 Fe2 C21 B2 65.9(15) . . . . ? C26 Fe2 C21 B2 -7.4(10) . . . . ? C28 Fe2 C21 B2 -70(2) . . . . ? C30 Fe2 C21 B2 34.1(11) . . . . ? C27 Fe2 C21 B2 -46.7(10) . . . . ? C22 Fe2 C21 B2 -121.4(9) . . . . ? C25 Fe2 C21 B2 121.4(10) . . . . ? C23 Fe2 C21 B2 -159.1(8) . . . . ? C24 Fe2 C21 B2 158.0(8) . . . . ? C25 C21 C22 C23 -0.1(10) . . . . ? B2 C21 C22 C23 174.5(8) . . . . ? Fe2 C21 C22 C23 60.1(7) . . . . ? C25 C21 C22 Fe2 -60.1(6) . . . . ? B2 C21 C22 Fe2 114.4(9) . . . . ? C29 Fe2 C22 C23 50.6(18) . . . . ? C26 Fe2 C22 C23 158.2(8) . . . . ? C28 Fe2 C22 C23 77.6(8) . . . . ? C30 Fe2 C22 C23 -171.0(12) . . . . ? C27 Fe2 C22 C23 116.9(7) . . . . ? C25 Fe2 C22 C23 -80.1(6) . . . . ? C21 Fe2 C22 C23 -118.8(8) . . . . ? C24 Fe2 C22 C23 -36.7(6) . . . . ? C29 Fe2 C22 C21 169.3(16) . . . . ? C26 Fe2 C22 C21 -83.0(8) . . . . ? C28 Fe2 C22 C21 -163.6(6) . . . . ? C30 Fe2 C22 C21 -52.2(14) . . . . ? C27 Fe2 C22 C21 -124.4(7) . . . . ? C25 Fe2 C22 C21 38.6(5) . . . . ? C23 Fe2 C22 C21 118.8(8) . . . . ? C24 Fe2 C22 C21 82.0(5) . . . . ? C21 C22 C23 C24 -0.5(11) . . . . ? Fe2 C22 C23 C24 59.2(7) . . . . ? C21 C22 C23 Fe2 -59.7(6) . . . . ? C29 Fe2 C23 C24 76.4(8) . . . . ? C26 Fe2 C23 C24 -165.8(9) . . . . ? C28 Fe2 C23 C24 116.4(6) . . . . ? C30 Fe2 C23 C24 43(2) . . . . ? C27 Fe2 C23 C24 159.5(6) . . . . ? C22 Fe2 C23 C24 -120.0(8) . . . . ? C25 Fe2 C23 C24 -37.5(5) . . . . ? C21 Fe2 C23 C24 -81.5(6) . . . . ? C29 Fe2 C23 C22 -163.6(7) . . . . ? C26 Fe2 C23 C22 -45.8(12) . . . . ? C28 Fe2 C23 C22 -123.5(7) . . . . ? C30 Fe2 C23 C22 163(2) . . . . ? C27 Fe2 C23 C22 -80.5(7) . . . . ? C25 Fe2 C23 C22 82.5(6) . . . . ? C21 Fe2 C23 C22 38.5(5) . . . . ? C24 Fe2 C23 C22 120.0(8) . . . . ? C22 C23 C24 C25 0.9(12) . . . . ? Fe2 C23 C24 C25 59.5(7) . . . . ? C22 C23 C24 Fe2 -58.6(7) . . . . ? C29 Fe2 C24 C23 -124.5(9) . . . . ? C26 Fe2 C24 C23 153.9(19) . . . . ? C28 Fe2 C24 C23 -83.1(8) . . . . ? C30 Fe2 C24 C23 -167.8(8) . . . . ? C27 Fe2 C24 C23 -44.9(12) . . . . ? C22 Fe2 C24 C23 37.4(5) . . . . ? C25 Fe2 C24 C23 119.3(8) . . . . ? C21 Fe2 C24 C23 82.3(6) . . . . ? C29 Fe2 C24 C25 116.2(9) . . . . ? C26 Fe2 C24 C25 35(2) . . . . ? C28 Fe2 C24 C25 157.6(7) . . . . ? C30 Fe2 C24 C25 72.9(9) . . . . ? C27 Fe2 C24 C25 -164.2(10) . . . . ? C22 Fe2 C24 C25 -81.9(6) . . . . ? C21 Fe2 C24 C25 -37.0(5) . . . . ? C23 Fe2 C24 C25 -119.3(8) . . . . ? C23 C24 C25 C21 -0.9(11) . . . . ? Fe2 C24 C25 C21 58.8(6) . . . . ? C23 C24 C25 Fe2 -59.7(7) . . . . ? C22 C21 C25 C24 0.6(10) . . . . ? B2 C21 C25 C24 -174.0(8) . . . . ? Fe2 C21 C25 C24 -59.0(6) . . . . ? C22 C21 C25 Fe2 59.6(6) . . . . ? B2 C21 C25 Fe2 -114.9(8) . . . . ? C29 Fe2 C25 C24 -83.7(10) . . . . ? C26 Fe2 C25 C24 -169.5(8) . . . . ? C28 Fe2 C25 C24 -51.5(16) . . . . ? C30 Fe2 C25 C24 -128.1(9) . . . . ? C27 Fe2 C25 C24 156.2(18) . . . . ? C22 Fe2 C25 C24 81.3(6) . . . . ? C21 Fe2 C25 C24 120.7(8) . . . . ? C23 Fe2 C25 C24 37.2(6) . . . . ? C29 Fe2 C25 C21 155.7(9) . . . . ? C26 Fe2 C25 C21 69.8(9) . . . . ? C28 Fe2 C25 C21 -172.1(13) . . . . ? C30 Fe2 C25 C21 111.2(9) . . . . ? C27 Fe2 C25 C21 36(2) . . . . ? C22 Fe2 C25 C21 -39.4(5) . . . . ? C23 Fe2 C25 C21 -83.4(6) . . . . ? C24 Fe2 C25 C21 -120.7(8) . . . . ? C29 Fe2 C26 C27 80.3(10) . . . . ? C28 Fe2 C26 C27 38.2(9) . . . . ? C30 Fe2 C26 C27 119.2(12) . . . . ? C22 Fe2 C26 C27 -82.4(9) . . . . ? C25 Fe2 C26 C27 -165.2(7) . . . . ? C21 Fe2 C26 C27 -125.6(8) . . . . ? C23 Fe2 C26 C27 -50.5(13) . . . . ? C24 Fe2 C26 C27 167.5(15) . . . . ? C29 Fe2 C26 C30 -38.9(10) . . . . ? C28 Fe2 C26 C30 -81.0(10) . . . . ? C27 Fe2 C26 C30 -119.2(12) . . . . ? C22 Fe2 C26 C30 158.4(8) . . . . ? C25 Fe2 C26 C30 75.6(10) . . . . ? C21 Fe2 C26 C30 115.2(9) . . . . ? C23 Fe2 C26 C30 -169.7(10) . . . . ? C24 Fe2 C26 C30 48(2) . . . . ? C30 C26 C27 C28 -0.5(15) . . . . ? Fe2 C26 C27 C28 -60.3(9) . . . . ? C30 C26 C27 Fe2 59.8(9) . . . . ? C29 Fe2 C27 C26 -82.9(12) . . . . ? C28 Fe2 C27 C26 -118.1(14) . . . . ? C30 Fe2 C27 C26 -37.6(9) . . . . ? C22 Fe2 C27 C26 113.9(9) . . . . ? C25 Fe2 C27 C26 45(2) . . . . ? C21 Fe2 C27 C26 72.1(11) . . . . ? C23 Fe2 C27 C26 156.0(9) . . . . ? C24 Fe2 C27 C26 -172.6(10) . . . . ? C29 Fe2 C27 C28 35.2(12) . . . . ? C26 Fe2 C27 C28 118.1(14) . . . . ? C30 Fe2 C27 C28 80.5(12) . . . . ? C22 Fe2 C27 C28 -128.0(10) . . . . ? C25 Fe2 C27 C28 162.7(16) . . . . ? C21 Fe2 C27 C28 -169.8(9) . . . . ? C23 Fe2 C27 C28 -85.9(11) . . . . ? C24 Fe2 C27 C28 -54.5(16) . . . . ? C26 C27 C28 C29 2.3(16) . . . . ? Fe2 C27 C28 C29 -58.1(11) . . . . ? C26 C27 C28 Fe2 60.4(9) . . . . ? C26 Fe2 C28 C29 83.9(13) . . . . ? C30 Fe2 C28 C29 40.1(12) . . . . ? C27 Fe2 C28 C29 121.8(16) . . . . ? C22 Fe2 C28 C29 -167.8(11) . . . . ? C25 Fe2 C28 C29 -46(2) . . . . ? C21 Fe2 C28 C29 151.9(17) . . . . ? C23 Fe2 C28 C29 -125.2(11) . . . . ? C24 Fe2 C28 C29 -82.6(13) . . . . ? C29 Fe2 C28 C27 -121.8(16) . . . . ? C26 Fe2 C28 C27 -37.9(11) . . . . ? C30 Fe2 C28 C27 -81.6(12) . . . . ? C22 Fe2 C28 C27 70.4(12) . . . . ? C25 Fe2 C28 C27 -167.9(12) . . . . ? C21 Fe2 C28 C27 30(2) . . . . ? C23 Fe2 C28 C27 113.0(10) . . . . ? C24 Fe2 C28 C27 155.6(9) . . . . ? C27 C28 C29 C30 -3.1(17) . . . . ? Fe2 C28 C29 C30 -61.5(9) . . . . ? C27 C28 C29 Fe2 58.3(10) . . . . ? C26 Fe2 C29 C28 -79.4(11) . . . . ? C30 Fe2 C29 C28 -116.9(14) . . . . ? C27 Fe2 C29 C28 -36.3(10) . . . . ? C22 Fe2 C29 C28 36(2) . . . . ? C25 Fe2 C29 C28 159.5(8) . . . . ? C21 Fe2 C29 C28 -161.2(10) . . . . ? C23 Fe2 C29 C28 74.8(11) . . . . ? C24 Fe2 C29 C28 116.4(10) . . . . ? C26 Fe2 C29 C30 37.5(10) . . . . ? C28 Fe2 C29 C30 116.9(14) . . . . ? C27 Fe2 C29 C30 80.5(11) . . . . ? C22 Fe2 C29 C30 152.5(18) . . . . ? C25 Fe2 C29 C30 -83.7(11) . . . . ? C21 Fe2 C29 C30 -44.3(16) . . . . ? C23 Fe2 C29 C30 -168.3(10) . . . . ? C24 Fe2 C29 C30 -126.7(10) . . . . ? C27 C26 C30 C29 -1.4(15) . . . . ? Fe2 C26 C30 C29 58.6(10) . . . . ? C27 C26 C30 Fe2 -59.9(9) . . . . ? C28 C29 C30 C26 2.8(16) . . . . ? Fe2 C29 C30 C26 -59.6(9) . . . . ? C28 C29 C30 Fe2 62.4(11) . . . . ? C29 Fe2 C30 C26 118.4(13) . . . . ? C28 Fe2 C30 C26 80.9(9) . . . . ? C27 Fe2 C30 C26 37.3(8) . . . . ? C22 Fe2 C30 C26 -44.7(15) . . . . ? C25 Fe2 C30 C26 -125.0(8) . . . . ? C21 Fe2 C30 C26 -81.3(9) . . . . ? C23 Fe2 C30 C26 160.3(18) . . . . ? C24 Fe2 C30 C26 -165.8(7) . . . . ? C26 Fe2 C30 C29 -118.4(13) . . . . ? C28 Fe2 C30 C29 -37.5(8) . . . . ? C27 Fe2 C30 C29 -81.2(9) . . . . ? C22 Fe2 C30 C29 -163.1(10) . . . . ? C25 Fe2 C30 C29 116.6(9) . . . . ? C21 Fe2 C30 C29 160.3(8) . . . . ? C23 Fe2 C30 C29 42(3) . . . . ? C24 Fe2 C30 C29 75.8(10) . . . . ? C37 Fe3 C31 C35 -172.9(7) . . . . ? C38 Fe3 C31 C35 42(3) . . . . ? C32 Fe3 C31 C35 -117.9(7) . . . . ? C33 Fe3 C31 C35 -80.0(5) . . . . ? C36 Fe3 C31 C35 151.5(6) . . . . ? C39 Fe3 C31 C35 69.0(7) . . . . ? C40 Fe3 C31 C35 107.7(6) . . . . ? C34 Fe3 C31 C35 -37.5(5) . . . . ? C37 Fe3 C31 C32 -55.0(9) . . . . ? C38 Fe3 C31 C32 160(3) . . . . ? C35 Fe3 C31 C32 117.9(7) . . . . ? C33 Fe3 C31 C32 37.9(5) . . . . ? C36 Fe3 C31 C32 -90.6(6) . . . . ? C39 Fe3 C31 C32 -173.2(6) . . . . ? C40 Fe3 C31 C32 -134.5(6) . . . . ? C34 Fe3 C31 C32 80.4(6) . . . . ? C37 Fe3 C31 B3 64.1(11) . . . . ? C38 Fe3 C31 B3 -81(3) . . . . ? C35 Fe3 C31 B3 -123.0(10) . . . . ? C32 Fe3 C31 B3 119.1(10) . . . . ? C33 Fe3 C31 B3 157.0(9) . . . . ? C36 Fe3 C31 B3 28.5(9) . . . . ? C39 Fe3 C31 B3 -54.0(10) . . . . ? C40 Fe3 C31 B3 -15.3(9) . . . . ? C34 Fe3 C31 B3 -160.5(9) . . . . ? C35 C31 C32 C33 0.2(10) . . . . ? B3 C31 C32 C33 176.2(8) . . . . ? Fe3 C31 C32 C33 -59.2(6) . . . . ? C35 C31 C32 Fe3 59.4(6) . . . . ? B3 C31 C32 Fe3 -124.5(9) . . . . ? C37 Fe3 C32 C31 149.7(5) . . . . ? C38 Fe3 C32 C31 -175.7(7) . . . . ? C35 Fe3 C32 C31 -38.3(5) . . . . ? C33 Fe3 C32 C31 -119.3(7) . . . . ? C36 Fe3 C32 C31 106.4(6) . . . . ? C39 Fe3 C32 C31 43(3) . . . . ? C40 Fe3 C32 C31 67.3(7) . . . . ? C34 Fe3 C32 C31 -82.8(6) . . . . ? C37 Fe3 C32 C33 -91.0(6) . . . . ? C38 Fe3 C32 C33 -56.4(9) . . . . ? C35 Fe3 C32 C33 80.9(6) . . . . ? C36 Fe3 C32 C33 -134.3(6) . . . . ? C39 Fe3 C32 C33 162(3) . . . . ? C31 Fe3 C32 C33 119.3(7) . . . . ? C40 Fe3 C32 C33 -173.4(6) . . . . ? C34 Fe3 C32 C33 36.5(6) . . . . ? C31 C32 C33 C34 -0.6(11) . . . . ? Fe3 C32 C33 C34 -60.1(7) . . . . ? C31 C32 C33 Fe3 59.5(6) . . . . ? C37 Fe3 C33 C34 -134.0(6) . . . . ? C38 Fe3 C33 C34 -91.2(6) . . . . ? C35 Fe3 C33 C34 38.3(5) . . . . ? C32 Fe3 C33 C34 119.9(8) . . . . ? C36 Fe3 C33 C34 -172.9(6) . . . . ? C39 Fe3 C33 C34 -56.2(9) . . . . ? C31 Fe3 C33 C34 82.2(6) . . . . ? C40 Fe3 C33 C34 160(3) . . . . ? C37 Fe3 C33 C32 106.0(6) . . . . ? C38 Fe3 C33 C32 148.9(6) . . . . ? C35 Fe3 C33 C32 -81.6(6) . . . . ? C36 Fe3 C33 C32 67.2(7) . . . . ? C39 Fe3 C33 C32 -176.1(7) . . . . ? C31 Fe3 C33 C32 -37.8(5) . . . . ? C40 Fe3 C33 C32 40(3) . . . . ? C34 Fe3 C33 C32 -119.9(8) . . . . ? C32 C33 C34 C35 0.7(11) . . . . ? Fe3 C33 C34 C35 -58.4(6) . . . . ? C32 C33 C34 Fe3 59.2(6) . . . . ? C37 Fe3 C34 C33 66.2(7) . . . . ? C38 Fe3 C34 C33 105.5(6) . . . . ? C35 Fe3 C34 C33 -119.0(7) . . . . ? C32 Fe3 C34 C33 -37.8(5) . . . . ? C36 Fe3 C34 C33 35(3) . . . . ? C39 Fe3 C34 C33 148.7(5) . . . . ? C31 Fe3 C34 C33 -81.9(5) . . . . ? C40 Fe3 C34 C33 -175.4(7) . . . . ? C37 Fe3 C34 C35 -174.8(6) . . . . ? C38 Fe3 C34 C35 -135.4(6) . . . . ? C32 Fe3 C34 C35 81.2(6) . . . . ? C33 Fe3 C34 C35 119.0(7) . . . . ? C36 Fe3 C34 C35 154(2) . . . . ? C39 Fe3 C34 C35 -92.3(6) . . . . ? C31 Fe3 C34 C35 37.1(5) . . . . ? C40 Fe3 C34 C35 -56.4(9) . . . . ? C32 C31 C35 C34 0.3(10) . . . . ? B3 C31 C35 C34 -175.6(9) . . . . ? Fe3 C31 C35 C34 59.7(6) . . . . ? C32 C31 C35 Fe3 -59.4(6) . . . . ? B3 C31 C35 Fe3 124.7(9) . . . . ? C33 C34 C35 C31 -0.6(10) . . . . ? Fe3 C34 C35 C31 -59.6(6) . . . . ? C33 C34 C35 Fe3 59.0(6) . . . . ? C37 Fe3 C35 C31 150(3) . . . . ? C38 Fe3 C35 C31 -173.3(6) . . . . ? C32 Fe3 C35 C31 38.7(5) . . . . ? C33 Fe3 C35 C31 83.1(5) . . . . ? C36 Fe3 C35 C31 -52.5(10) . . . . ? C39 Fe3 C35 C31 -133.7(5) . . . . ? C40 Fe3 C35 C31 -89.9(6) . . . . ? C34 Fe3 C35 C31 120.1(8) . . . . ? C37 Fe3 C35 C34 30(3) . . . . ? C38 Fe3 C35 C34 66.5(8) . . . . ? C32 Fe3 C35 C34 -81.5(6) . . . . ? C33 Fe3 C35 C34 -37.0(5) . . . . ? C36 Fe3 C35 C34 -172.7(8) . . . . ? C39 Fe3 C35 C34 106.2(6) . . . . ? C31 Fe3 C35 C34 -120.1(8) . . . . ? C40 Fe3 C35 C34 149.9(6) . . . . ? C38 Fe3 C36 C37 -37.5(7) . . . . ? C35 Fe3 C36 C37 -175.4(7) . . . . ? C32 Fe3 C36 C37 106.0(7) . . . . ? C33 Fe3 C36 C37 66.3(8) . . . . ? C39 Fe3 C36 C37 -81.0(7) . . . . ? C31 Fe3 C36 C37 149.9(6) . . . . ? C40 Fe3 C36 C37 -118.8(9) . . . . ? C34 Fe3 C36 C37 37(3) . . . . ? C37 Fe3 C36 C40 118.8(9) . . . . ? C38 Fe3 C36 C40 81.4(7) . . . . ? C35 Fe3 C36 C40 -56.6(10) . . . . ? C32 Fe3 C36 C40 -135.2(6) . . . . ? C33 Fe3 C36 C40 -174.9(6) . . . . ? C39 Fe3 C36 C40 37.8(6) . . . . ? C31 Fe3 C36 C40 -91.3(7) . . . . ? C34 Fe3 C36 C40 155(2) . . . . ? C40 C36 C37 C38 0.6(11) . . . . ? Fe3 C36 C37 C38 60.2(7) . . . . ? C40 C36 C37 Fe3 -59.6(7) . . . . ? C35 Fe3 C37 C38 42(3) . . . . ? C32 Fe3 C37 C38 150.2(7) . . . . ? C33 Fe3 C37 C38 106.3(7) . . . . ? C36 Fe3 C37 C38 -119.1(11) . . . . ? C39 Fe3 C37 C38 -37.3(7) . . . . ? C31 Fe3 C37 C38 -173.6(7) . . . . ? C40 Fe3 C37 C38 -81.0(8) . . . . ? C34 Fe3 C37 C38 68.2(9) . . . . ? C38 Fe3 C37 C36 119.1(11) . . . . ? C35 Fe3 C37 C36 161(3) . . . . ? C32 Fe3 C37 C36 -90.7(8) . . . . ? C33 Fe3 C37 C36 -134.7(7) . . . . ? C39 Fe3 C37 C36 81.8(8) . . . . ? C31 Fe3 C37 C36 -54.5(11) . . . . ? C40 Fe3 C37 C36 38.1(7) . . . . ? C34 Fe3 C37 C36 -172.7(7) . . . . ? C36 C37 C38 C39 -0.4(12) . . . . ? Fe3 C37 C38 C39 59.9(7) . . . . ? C36 C37 C38 Fe3 -60.2(7) . . . . ? C35 Fe3 C38 C37 -172.6(6) . . . . ? C32 Fe3 C38 C37 -53.4(10) . . . . ? C33 Fe3 C38 C37 -90.4(7) . . . . ? C36 Fe3 C38 C37 37.8(7) . . . . ? C39 Fe3 C38 C37 119.6(10) . . . . ? C31 Fe3 C38 C37 150(3) . . . . ? C40 Fe3 C38 C37 82.1(7) . . . . ? C34 Fe3 C38 C37 -132.9(7) . . . . ? C37 Fe3 C38 C39 -119.6(10) . . . . ? C35 Fe3 C38 C39 67.7(8) . . . . ? C32 Fe3 C38 C39 -173.0(7) . . . . ? C33 Fe3 C38 C39 150.0(6) . . . . ? C36 Fe3 C38 C39 -81.8(7) . . . . ? C31 Fe3 C38 C39 30(3) . . . . ? C40 Fe3 C38 C39 -37.6(7) . . . . ? C34 Fe3 C38 C39 107.5(7) . . . . ? C37 C38 C39 C40 0.0(12) . . . . ? Fe3 C38 C39 C40 59.4(7) . . . . ? C37 C38 C39 Fe3 -59.4(7) . . . . ? C37 Fe3 C39 C38 37.2(6) . . . . ? C35 Fe3 C39 C38 -134.5(6) . . . . ? C32 Fe3 C39 C38 147(3) . . . . ? C33 Fe3 C39 C38 -53.9(10) . . . . ? C36 Fe3 C39 C38 81.1(7) . . . . ? C31 Fe3 C39 C38 -175.0(6) . . . . ? C40 Fe3 C39 C38 119.3(9) . . . . ? C34 Fe3 C39 C38 -90.0(7) . . . . ? C37 Fe3 C39 C40 -82.1(7) . . . . ? C38 Fe3 C39 C40 -119.3(9) . . . . ? C35 Fe3 C39 C40 106.2(6) . . . . ? C32 Fe3 C39 C40 28(3) . . . . ? C33 Fe3 C39 C40 -173.2(7) . . . . ? C36 Fe3 C39 C40 -38.3(7) . . . . ? C31 Fe3 C39 C40 65.7(8) . . . . ? C34 Fe3 C39 C40 150.7(6) . . . . ? C38 C39 C40 C36 0.3(11) . . . . ? Fe3 C39 C40 C36 59.4(7) . . . . ? C38 C39 C40 Fe3 -59.1(7) . . . . ? C37 C36 C40 C39 -0.6(11) . . . . ? Fe3 C36 C40 C39 -59.7(7) . . . . ? C37 C36 C40 Fe3 59.2(7) . . . . ? C37 Fe3 C40 C39 80.8(7) . . . . ? C38 Fe3 C40 C39 37.4(6) . . . . ? C35 Fe3 C40 C39 -91.9(7) . . . . ? C32 Fe3 C40 C39 -175.4(6) . . . . ? C33 Fe3 C40 C39 149(3) . . . . ? C36 Fe3 C40 C39 118.5(9) . . . . ? C31 Fe3 C40 C39 -135.6(6) . . . . ? C34 Fe3 C40 C39 -54.5(10) . . . . ? C37 Fe3 C40 C36 -37.8(6) . . . . ? C38 Fe3 C40 C36 -81.1(7) . . . . ? C35 Fe3 C40 C36 149.5(6) . . . . ? C32 Fe3 C40 C36 66.1(8) . . . . ? C33 Fe3 C40 C36 30(3) . . . . ? C39 Fe3 C40 C36 -118.5(9) . . . . ? C31 Fe3 C40 C36 105.9(6) . . . . ? C34 Fe3 C40 C36 -173.0(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.606 _refine_diff_density_min -1.577 _refine_diff_density_rms 0.187 data_wa1117 _database_code_depnum_ccdc_archive 'CCDC 894223' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H51 B3 Fe3 Zr' _chemical_formula_sum 'C40 H51 B3 Fe3 Zr' _chemical_formula_weight 823.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7895(7) _cell_length_b 23.3720(19) _cell_length_c 20.470(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.081(8) _cell_angle_gamma 90.00 _cell_volume 3726.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8181 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 16.0 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6965 _exptl_absorpt_correction_T_max 0.8458 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21865 _diffrn_reflns_av_R_equivalents 0.1558 _diffrn_reflns_av_sigmaI/netI 0.1692 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.69 _reflns_number_total 6621 _reflns_number_gt 3569 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0345P)^2^] 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 6621 _refine_ls_number_parameters 432 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _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 Zr1 Zr 0.75404(10) 0.62756(3) 0.75360(4) 0.02110(16) Uani 1 1 d . . . Fe1 Fe 1.03914(15) 0.71185(4) 0.53696(6) 0.0279(3) Uani 1 1 d . . . Fe2 Fe 0.40326(15) 0.46301(4) 0.62802(6) 0.0288(3) Uani 1 1 d . . . Fe3 Fe 0.92861(16) 0.43394(4) 0.88715(6) 0.0343(3) Uani 1 1 d . . . B1 B 0.9501(12) 0.6729(3) 0.6811(4) 0.0259(17) Uani 1 1 d U . . H1A H 0.9819 0.6789 0.7269 0.039 Uiso 1 1 calc R . . H1B H 0.9568 0.6320 0.6708 0.039 Uiso 1 1 calc R . . H1C H 0.8326 0.6865 0.6738 0.039 Uiso 1 1 calc R . . B2 B 0.5608(11) 0.5800(3) 0.6830(4) 0.0239(18) Uani 1 1 d . . . H2A H 0.6731 0.5689 0.6657 0.036 Uiso 1 1 calc R . . H2B H 0.5524 0.5682 0.7289 0.036 Uiso 1 1 calc R . . H2C H 0.5475 0.6216 0.6799 0.036 Uiso 1 1 calc R . . B3 B 0.9167(10) 0.5510(3) 0.7994(4) 0.0195(16) Uani 1 1 d . . . H3A H 0.7957 0.5488 0.8123 0.029 Uiso 1 1 calc R . . H3B H 0.9271 0.5427 0.7527 0.029 Uiso 1 1 calc R . . H3C H 0.9605 0.5896 0.8082 0.029 Uiso 1 1 calc R . . C1 C 0.5703(12) 0.7108(3) 0.7834(4) 0.042(2) Uani 1 1 d . . . C2 C 0.7289(12) 0.7219(3) 0.8109(4) 0.0351(19) Uani 1 1 d . . . C3 C 0.7619(11) 0.6806(3) 0.8598(4) 0.036(2) Uani 1 1 d . . . C4 C 0.6150(11) 0.6440(3) 0.8629(4) 0.0322(18) Uani 1 1 d . . . C5 C 0.4971(10) 0.6627(3) 0.8155(4) 0.035(2) Uani 1 1 d . . . C6 C 0.4833(18) 0.7490(4) 0.7342(5) 0.078(4) Uani 1 1 d . . . H6A H 0.3628 0.7543 0.7465 0.117 Uiso 1 1 calc R . . H6B H 0.4894 0.7312 0.6908 0.117 Uiso 1 1 calc R . . H6C H 0.5411 0.7862 0.7331 0.117 Uiso 1 1 calc R . . C7 C 0.8481(17) 0.7719(4) 0.7983(6) 0.076(4) Uani 1 1 d . . . H7A H 0.8487 0.7808 0.7515 0.114 Uiso 1 1 calc R . . H7B H 0.9646 0.7619 0.8124 0.114 Uiso 1 1 calc R . . H7C H 0.8081 0.8054 0.8228 0.114 Uiso 1 1 calc R . . C8 C 0.9056(15) 0.6790(6) 0.9081(6) 0.087(5) Uani 1 1 d . . . H8A H 0.8711 0.6991 0.9480 0.131 Uiso 1 1 calc R . . H8B H 1.0069 0.6976 0.8894 0.131 Uiso 1 1 calc R . . H8C H 0.9331 0.6391 0.9186 0.131 Uiso 1 1 calc R . . C9 C 0.5819(18) 0.5977(4) 0.9135(5) 0.072(3) Uani 1 1 d . . . H9A H 0.6676 0.5673 0.9088 0.107 Uiso 1 1 calc R . . H9B H 0.4669 0.5817 0.9068 0.107 Uiso 1 1 calc R . . H9C H 0.5897 0.6142 0.9574 0.107 Uiso 1 1 calc R . . C10 C 0.3181(12) 0.6409(5) 0.8046(6) 0.066(3) Uani 1 1 d . . . H10A H 0.2356 0.6717 0.8129 0.099 Uiso 1 1 calc R . . H10B H 0.2955 0.6090 0.8345 0.099 Uiso 1 1 calc R . . H10C H 0.3062 0.6277 0.7594 0.099 Uiso 1 1 calc R . . C11 C 1.0769(9) 0.7070(3) 0.6358(4) 0.0248(16) Uani 1 1 d . . . C12 C 1.2184(11) 0.6828(3) 0.6011(4) 0.0342(19) Uani 1 1 d . . . H12 H 1.2568 0.6444 0.6051 0.041 Uiso 1 1 calc R . . C13 C 1.2927(11) 0.7246(3) 0.5598(4) 0.039(2) Uani 1 1 d . . . H13 H 1.3873 0.7191 0.5312 0.047 Uiso 1 1 calc R . . C14 C 1.2002(11) 0.7757(3) 0.5691(4) 0.037(2) Uani 1 1 d . . . H14 H 1.2224 0.8111 0.5479 0.044 Uiso 1 1 calc R . . C15 C 1.0666(11) 0.7654(3) 0.6159(4) 0.0325(18) Uani 1 1 d . . . H15 H 0.9855 0.7927 0.6310 0.039 Uiso 1 1 calc R . . C16 C 0.8211(14) 0.6666(4) 0.5209(4) 0.049(3) Uani 1 1 d . . . H16 H 0.7536 0.6484 0.5534 0.059 Uiso 1 1 calc R . . C17 C 0.9577(15) 0.6422(4) 0.4860(5) 0.057(3) Uani 1 1 d . . . H17 H 0.9989 0.6042 0.4908 0.069 Uiso 1 1 calc R . . C18 C 1.0221(16) 0.6828(4) 0.4434(5) 0.060(3) Uani 1 1 d . . . H18 H 1.1159 0.6771 0.4145 0.072 Uiso 1 1 calc R . . C19 C 0.9302(14) 0.7326(4) 0.4493(5) 0.053(3) Uani 1 1 d . . . H19 H 0.9477 0.7669 0.4252 0.063 Uiso 1 1 calc R . . C20 C 0.8032(13) 0.7233(4) 0.4985(5) 0.048(2) Uani 1 1 d . . . H20 H 0.7214 0.7505 0.5134 0.058 Uiso 1 1 calc R . . C21 C 0.4142(10) 0.5497(3) 0.6420(4) 0.0265(17) Uani 1 1 d . . . C22 C 0.4145(10) 0.5361(3) 0.5731(4) 0.0294(17) Uani 1 1 d . . . H22 H 0.5020 0.5458 0.5428 0.035 Uiso 1 1 calc R . . C23 C 0.2610(12) 0.5056(3) 0.5588(4) 0.037(2) Uani 1 1 d . . . H23 H 0.2285 0.4920 0.5168 0.044 Uiso 1 1 calc R . . C24 C 0.1636(11) 0.4987(3) 0.6171(4) 0.039(2) Uani 1 1 d . . . H24 H 0.0569 0.4792 0.6211 0.047 Uiso 1 1 calc R . . C25 C 0.2566(10) 0.5265(3) 0.6687(4) 0.0303(18) Uani 1 1 d . . . H25 H 0.2208 0.5292 0.7129 0.036 Uiso 1 1 calc R . . C26 C 0.6074(12) 0.4309(3) 0.6788(5) 0.040(2) Uani 1 1 d . . . H26 H 0.6850 0.4522 0.7051 0.048 Uiso 1 1 calc R . . C27 C 0.6260(14) 0.4197(3) 0.6121(5) 0.050(3) Uani 1 1 d . . . H27 H 0.7182 0.4322 0.5854 0.060 Uiso 1 1 calc R . . C28 C 0.4826(14) 0.3862(3) 0.5910(5) 0.052(3) Uani 1 1 d . . . H28 H 0.4639 0.3723 0.5480 0.062 Uiso 1 1 calc R . . C29 C 0.3743(13) 0.3777(3) 0.6449(6) 0.057(3) Uani 1 1 d . . . H29 H 0.2685 0.3574 0.6446 0.068 Uiso 1 1 calc R . . C30 C 0.4515(13) 0.4048(3) 0.7006(5) 0.044(2) Uani 1 1 d . . . H30 H 0.4074 0.4053 0.7438 0.053 Uiso 1 1 calc R . . C31 C 1.0239(10) 0.5059(3) 0.8397(4) 0.0312(18) Uani 1 1 d . . . C32 C 1.0942(13) 0.4533(4) 0.8130(5) 0.049(2) Uani 1 1 d . . . H32 H 1.0832 0.4405 0.7692 0.059 Uiso 1 1 calc R . . C33 C 1.1831(14) 0.4240(4) 0.8645(5) 0.056(3) Uani 1 1 d . . . H33 H 1.2438 0.3890 0.8603 0.067 Uiso 1 1 calc R . . C34 C 1.1653(13) 0.4558(4) 0.9219(5) 0.050(3) Uani 1 1 d . . . H34 H 1.2114 0.4458 0.9634 0.060 Uiso 1 1 calc R . . C35 C 1.0660(12) 0.5059(3) 0.9078(5) 0.048(3) Uani 1 1 d . . . H35 H 1.0335 0.5343 0.9385 0.057 Uiso 1 1 calc R . . C36 C 0.6691(13) 0.4329(3) 0.8724(5) 0.049(3) Uani 1 1 d . . . H36 H 0.6034 0.4601 0.8487 0.059 Uiso 1 1 calc R . . C37 C 0.7475(13) 0.3837(3) 0.8461(5) 0.048(3) Uani 1 1 d . . . H37 H 0.7445 0.3726 0.8014 0.058 Uiso 1 1 calc R . . C38 C 0.8321(14) 0.3532(3) 0.8973(5) 0.053(3) Uani 1 1 d . . . H38 H 0.8948 0.3186 0.8932 0.064 Uiso 1 1 calc R . . C39 C 0.8037(12) 0.3852(3) 0.9559(5) 0.046(2) Uani 1 1 d . . . H39 H 0.8439 0.3751 0.9982 0.055 Uiso 1 1 calc R . . C40 C 0.7045(11) 0.4349(4) 0.9399(5) 0.044(2) Uani 1 1 d . . . H40 H 0.6691 0.4639 0.9695 0.053 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 Zr1 0.0211(3) 0.0214(3) 0.0208(3) 0.0014(3) 0.0021(3) -0.0012(3) Fe1 0.0304(6) 0.0260(5) 0.0274(6) 0.0037(4) 0.0050(5) -0.0031(4) Fe2 0.0323(7) 0.0236(5) 0.0304(6) -0.0034(4) -0.0056(5) 0.0034(4) Fe3 0.0395(7) 0.0312(5) 0.0321(7) 0.0072(5) 0.0016(6) -0.0015(5) B1 0.026(2) 0.0261(19) 0.0257(19) 0.0006(10) 0.0006(10) -0.0008(10) B2 0.024(5) 0.021(4) 0.027(4) 0.000(3) 0.002(4) -0.001(3) B3 0.012(4) 0.022(3) 0.025(4) 0.005(3) 0.007(3) 0.005(3) C1 0.059(6) 0.023(4) 0.045(5) -0.009(3) -0.015(5) 0.022(4) C2 0.049(5) 0.023(3) 0.033(4) -0.007(3) 0.026(4) -0.009(3) C3 0.022(4) 0.061(5) 0.026(4) -0.018(4) 0.001(4) 0.001(4) C4 0.037(5) 0.028(3) 0.032(4) -0.001(3) 0.023(4) 0.010(3) C5 0.017(4) 0.042(4) 0.047(5) -0.021(4) 0.012(4) -0.002(3) C6 0.123(12) 0.057(6) 0.053(7) -0.008(5) -0.011(8) 0.052(7) C7 0.109(10) 0.040(5) 0.079(8) -0.019(5) 0.068(7) -0.027(6) C8 0.048(7) 0.159(12) 0.056(7) -0.049(8) -0.014(7) 0.026(7) C9 0.110(11) 0.051(5) 0.053(7) 0.010(5) 0.030(7) 0.011(6) C10 0.035(5) 0.084(7) 0.079(8) -0.040(6) 0.017(6) 0.000(5) C11 0.018(4) 0.025(3) 0.032(4) 0.004(3) 0.003(3) -0.006(3) C12 0.033(5) 0.036(4) 0.034(5) 0.004(3) 0.003(4) 0.003(3) C13 0.033(5) 0.041(4) 0.044(5) 0.000(4) 0.013(4) 0.002(4) C14 0.043(5) 0.034(4) 0.033(5) 0.003(3) 0.009(4) -0.011(4) C15 0.035(5) 0.033(4) 0.030(4) 0.005(3) 0.006(4) -0.003(3) C16 0.063(7) 0.056(5) 0.029(5) 0.010(4) -0.001(5) -0.030(5) C17 0.073(8) 0.050(5) 0.050(6) -0.018(5) -0.005(6) -0.002(5) C18 0.068(8) 0.075(7) 0.036(6) -0.017(5) 0.002(6) -0.005(6) C19 0.064(7) 0.056(5) 0.038(6) 0.020(4) -0.014(5) -0.022(5) C20 0.040(6) 0.055(5) 0.049(6) -0.007(4) -0.006(5) 0.006(4) C21 0.031(4) 0.024(3) 0.024(4) -0.006(3) 0.005(4) 0.001(3) C22 0.030(4) 0.028(4) 0.030(4) -0.001(3) 0.003(4) 0.007(3) C23 0.049(6) 0.027(4) 0.034(5) -0.005(3) -0.021(5) 0.004(4) C24 0.034(5) 0.032(4) 0.050(6) -0.001(4) -0.011(5) -0.004(4) C25 0.024(4) 0.026(3) 0.041(5) -0.001(3) 0.000(4) 0.006(3) C26 0.042(5) 0.027(4) 0.050(6) -0.003(4) -0.023(5) 0.005(4) C27 0.062(7) 0.035(4) 0.052(6) -0.001(4) -0.004(6) 0.027(4) C28 0.073(7) 0.024(4) 0.059(7) -0.017(4) -0.021(6) 0.018(4) C29 0.050(6) 0.027(4) 0.092(9) 0.002(5) -0.027(6) -0.006(4) C30 0.054(6) 0.037(4) 0.040(5) 0.012(4) 0.007(5) 0.019(4) C31 0.024(4) 0.030(4) 0.040(5) 0.006(3) 0.011(4) -0.001(3) C32 0.060(7) 0.051(5) 0.036(5) 0.019(4) 0.008(5) 0.015(4) C33 0.060(7) 0.050(5) 0.057(7) 0.024(5) 0.009(6) 0.014(5) C34 0.047(6) 0.048(5) 0.055(6) 0.026(4) -0.011(5) -0.003(4) C35 0.048(6) 0.042(4) 0.052(6) 0.014(4) -0.023(5) -0.012(4) C36 0.047(6) 0.041(4) 0.061(6) 0.011(4) -0.016(5) -0.006(4) C37 0.065(7) 0.039(5) 0.041(5) 0.002(4) -0.013(5) -0.012(4) C38 0.083(8) 0.027(4) 0.050(6) 0.001(4) -0.006(6) -0.005(4) C39 0.054(6) 0.039(5) 0.043(5) 0.014(4) 0.004(5) -0.005(4) C40 0.034(5) 0.048(5) 0.051(6) 0.002(4) 0.018(5) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C1 2.492(8) . ? Zr1 C3 2.503(7) . ? Zr1 C2 2.505(7) . ? Zr1 C5 2.509(9) . ? Zr1 C4 2.517(8) . ? Fe1 C20 2.016(9) . ? Fe1 C16 2.027(9) . ? Fe1 C12 2.032(7) . ? Fe1 C17 2.034(8) . ? Fe1 C18 2.035(9) . ? Fe1 C19 2.042(8) . ? Fe1 C11 2.047(7) . ? Fe1 C13 2.051(9) . ? Fe1 C15 2.055(8) . ? Fe1 C14 2.058(7) . ? Fe2 C27 2.035(10) . ? Fe2 C29 2.037(9) . ? Fe2 C26 2.041(7) . ? Fe2 C28 2.044(8) . ? Fe2 C22 2.046(7) . ? Fe2 C21 2.047(6) . ? Fe2 C30 2.049(8) . ? Fe2 C25 2.050(8) . ? Fe2 C23 2.055(7) . ? Fe2 C24 2.057(8) . ? Fe3 C37 2.018(8) . ? Fe3 C35 2.037(8) . ? Fe3 C34 2.040(9) . ? Fe3 C38 2.041(8) . ? Fe3 C32 2.043(11) . ? Fe3 C36 2.043(10) . ? Fe3 C33 2.049(12) . ? Fe3 C39 2.057(9) . ? Fe3 C40 2.054(10) . ? Fe3 C31 2.080(8) . ? B1 C11 1.573(12) . ? B1 H1A 0.9800 . ? B1 H1B 0.9800 . ? B1 H1C 0.9800 . ? B2 C21 1.583(10) . ? B2 H2A 0.9800 . ? B2 H2B 0.9800 . ? B2 H2C 0.9800 . ? B3 C31 1.577(9) . ? B3 H3A 0.9800 . ? B3 H3B 0.9800 . ? B3 H3C 0.9800 . ? C1 C2 1.381(12) . ? C1 C5 1.423(13) . ? C1 C6 1.506(11) . ? C2 C3 1.413(11) . ? C2 C7 1.516(12) . ? C3 C4 1.429(11) . ? C3 C8 1.493(11) . ? C4 C5 1.405(10) . ? C4 C9 1.521(12) . ? C5 C10 1.502(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.429(12) . ? C11 C15 1.426(9) . ? C12 C13 1.415(12) . ? C12 H12 0.9500 . ? C13 C14 1.409(11) . ? C13 H13 0.9500 . ? C14 C15 1.436(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.403(15) . ? C16 C20 1.409(12) . ? C16 H16 0.9500 . ? C17 C18 1.383(15) . ? C17 H17 0.9500 . ? C18 C19 1.371(14) . ? C18 H18 0.9500 . ? C19 C20 1.429(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.445(10) . ? C21 C25 1.450(12) . ? C22 C23 1.422(11) . ? C22 H22 0.9500 . ? C23 C24 1.425(14) . ? C23 H23 0.9500 . ? C24 C25 1.435(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.397(14) . ? C26 C30 1.431(14) . ? C26 H26 0.9500 . ? C27 C28 1.430(13) . ? C27 H27 0.9500 . ? C28 C29 1.405(16) . ? C28 H28 0.9500 . ? C29 C30 1.436(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C35 1.430(12) . ? C31 C32 1.453(12) . ? C32 C33 1.434(11) . ? C32 H32 0.9500 . ? C33 C34 1.397(15) . ? C33 H33 0.9500 . ? C34 C35 1.433(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C40 1.410(13) . ? C36 C37 1.409(13) . ? C36 H36 0.9500 . ? C37 C38 1.428(11) . ? C37 H37 0.9500 . ? C38 C39 1.431(14) . ? C38 H38 0.9500 . ? C39 C40 1.434(12) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zr1 C3 54.1(2) . . ? C1 Zr1 C2 32.1(3) . . ? C3 Zr1 C2 32.8(3) . . ? C1 Zr1 C5 33.1(3) . . ? C3 Zr1 C5 54.4(2) . . ? C2 Zr1 C5 54.0(3) . . ? C1 Zr1 C4 54.2(3) . . ? C3 Zr1 C4 33.1(3) . . ? C2 Zr1 C4 54.2(2) . . ? C5 Zr1 C4 32.5(2) . . ? C20 Fe1 C16 40.8(4) . . ? C20 Fe1 C12 157.2(4) . . ? C16 Fe1 C12 120.4(3) . . ? C20 Fe1 C17 67.8(4) . . ? C16 Fe1 C17 40.4(4) . . ? C12 Fe1 C17 106.1(4) . . ? C20 Fe1 C18 67.6(4) . . ? C16 Fe1 C18 67.7(5) . . ? C12 Fe1 C18 122.7(4) . . ? C17 Fe1 C18 39.7(4) . . ? C20 Fe1 C19 41.2(4) . . ? C16 Fe1 C19 68.5(4) . . ? C12 Fe1 C19 158.6(5) . . ? C17 Fe1 C19 67.1(4) . . ? C18 Fe1 C19 39.3(4) . . ? C20 Fe1 C11 121.5(4) . . ? C16 Fe1 C11 104.5(3) . . ? C12 Fe1 C11 41.0(3) . . ? C17 Fe1 C11 120.5(4) . . ? C18 Fe1 C11 157.0(4) . . ? C19 Fe1 C11 160.1(4) . . ? C20 Fe1 C13 161.2(4) . . ? C16 Fe1 C13 156.8(4) . . ? C12 Fe1 C13 40.6(3) . . ? C17 Fe1 C13 122.2(4) . . ? C18 Fe1 C13 108.9(5) . . ? C19 Fe1 C13 124.4(4) . . ? C11 Fe1 C13 69.2(3) . . ? C20 Fe1 C15 108.7(4) . . ? C16 Fe1 C15 122.1(4) . . ? C12 Fe1 C15 67.9(3) . . ? C17 Fe1 C15 157.3(4) . . ? C18 Fe1 C15 161.7(4) . . ? C19 Fe1 C15 126.1(4) . . ? C11 Fe1 C15 40.7(3) . . ? C13 Fe1 C15 68.5(4) . . ? C20 Fe1 C14 125.7(3) . . ? C16 Fe1 C14 160.2(4) . . ? C12 Fe1 C14 67.5(3) . . ? C17 Fe1 C14 159.1(5) . . ? C18 Fe1 C14 125.5(4) . . ? C19 Fe1 C14 111.1(3) . . ? C11 Fe1 C14 68.8(3) . . ? C13 Fe1 C14 40.1(3) . . ? C15 Fe1 C14 40.9(3) . . ? C27 Fe2 C29 68.6(4) . . ? C27 Fe2 C26 40.1(4) . . ? C29 Fe2 C26 68.9(3) . . ? C27 Fe2 C28 41.0(4) . . ? C29 Fe2 C28 40.3(4) . . ? C26 Fe2 C28 68.3(3) . . ? C27 Fe2 C22 106.9(4) . . ? C29 Fe2 C22 156.3(4) . . ? C26 Fe2 C22 123.5(3) . . ? C28 Fe2 C22 121.1(4) . . ? C27 Fe2 C21 118.6(4) . . ? C29 Fe2 C21 161.7(4) . . ? C26 Fe2 C21 105.1(3) . . ? C28 Fe2 C21 155.2(4) . . ? C22 Fe2 C21 41.3(3) . . ? C27 Fe2 C30 68.3(4) . . ? C29 Fe2 C30 41.1(4) . . ? C26 Fe2 C30 41.0(4) . . ? C28 Fe2 C30 68.3(4) . . ? C22 Fe2 C30 160.8(3) . . ? C21 Fe2 C30 123.2(3) . . ? C27 Fe2 C25 154.3(3) . . ? C29 Fe2 C25 125.3(4) . . ? C26 Fe2 C25 119.6(3) . . ? C28 Fe2 C25 162.7(4) . . ? C22 Fe2 C25 69.1(3) . . ? C21 Fe2 C25 41.5(3) . . ? C30 Fe2 C25 106.7(4) . . ? C27 Fe2 C23 126.1(4) . . ? C29 Fe2 C23 122.1(3) . . ? C26 Fe2 C23 161.4(4) . . ? C28 Fe2 C23 109.4(3) . . ? C22 Fe2 C23 40.6(3) . . ? C21 Fe2 C23 68.9(3) . . ? C30 Fe2 C23 156.9(4) . . ? C25 Fe2 C23 68.2(3) . . ? C27 Fe2 C24 163.4(3) . . ? C29 Fe2 C24 108.3(4) . . ? C26 Fe2 C24 155.6(4) . . ? C28 Fe2 C24 126.2(3) . . ? C22 Fe2 C24 69.0(3) . . ? C21 Fe2 C24 69.6(3) . . ? C30 Fe2 C24 120.9(4) . . ? C25 Fe2 C24 40.9(3) . . ? C23 Fe2 C24 40.6(4) . . ? C37 Fe3 C35 159.0(3) . . ? C37 Fe3 C34 157.2(4) . . ? C35 Fe3 C34 41.1(3) . . ? C37 Fe3 C38 41.2(3) . . ? C35 Fe3 C38 159.3(3) . . ? C34 Fe3 C38 121.9(3) . . ? C37 Fe3 C32 105.2(4) . . ? C35 Fe3 C32 68.8(4) . . ? C34 Fe3 C32 68.4(4) . . ? C38 Fe3 C32 120.9(4) . . ? C37 Fe3 C36 40.6(4) . . ? C35 Fe3 C36 124.1(4) . . ? C34 Fe3 C36 161.4(4) . . ? C38 Fe3 C36 68.9(4) . . ? C32 Fe3 C36 121.2(4) . . ? C37 Fe3 C33 121.1(4) . . ? C35 Fe3 C33 68.4(4) . . ? C34 Fe3 C33 39.9(4) . . ? C38 Fe3 C33 106.0(4) . . ? C32 Fe3 C33 41.0(3) . . ? C36 Fe3 C33 157.2(4) . . ? C37 Fe3 C39 68.4(4) . . ? C35 Fe3 C39 124.4(4) . . ? C34 Fe3 C39 109.1(4) . . ? C38 Fe3 C39 40.9(4) . . ? C32 Fe3 C39 158.5(4) . . ? C36 Fe3 C39 68.0(4) . . ? C33 Fe3 C39 123.4(3) . . ? C37 Fe3 C40 68.4(4) . . ? C35 Fe3 C40 109.2(4) . . ? C34 Fe3 C40 125.6(4) . . ? C38 Fe3 C40 69.1(4) . . ? C32 Fe3 C40 157.8(3) . . ? C36 Fe3 C40 40.2(4) . . ? C33 Fe3 C40 160.6(4) . . ? C39 Fe3 C40 40.8(3) . . ? C37 Fe3 C31 121.7(3) . . ? C35 Fe3 C31 40.6(3) . . ? C34 Fe3 C31 68.7(3) . . ? C38 Fe3 C31 157.9(4) . . ? C32 Fe3 C31 41.3(3) . . ? C36 Fe3 C31 107.1(3) . . ? C33 Fe3 C31 68.9(3) . . ? C39 Fe3 C31 159.6(3) . . ? C40 Fe3 C31 122.7(3) . . ? C11 B1 H1A 109.5 . . ? C11 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? C11 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? C21 B2 H2A 109.5 . . ? C21 B2 H2B 109.5 . . ? H2A B2 H2B 109.5 . . ? C21 B2 H2C 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? C31 B3 H3A 109.5 . . ? C31 B3 H3B 109.5 . . ? H3A B3 H3B 109.5 . . ? C31 B3 H3C 109.5 . . ? H3A B3 H3C 109.5 . . ? H3B B3 H3C 109.5 . . ? C2 C1 C5 108.5(6) . . ? C2 C1 C6 124.3(9) . . ? C5 C1 C6 126.7(9) . . ? C2 C1 Zr1 74.5(5) . . ? C5 C1 Zr1 74.1(4) . . ? C6 C1 Zr1 123.8(6) . . ? C1 C2 C3 108.8(7) . . ? C1 C2 C7 128.5(8) . . ? C3 C2 C7 122.4(8) . . ? C1 C2 Zr1 73.4(4) . . ? C3 C2 Zr1 73.5(4) . . ? C7 C2 Zr1 123.4(6) . . ? C2 C3 C4 107.2(6) . . ? C2 C3 C8 128.4(9) . . ? C4 C3 C8 123.6(9) . . ? C2 C3 Zr1 73.7(4) . . ? C4 C3 Zr1 74.0(4) . . ? C8 C3 Zr1 125.5(6) . . ? C5 C4 C3 107.8(7) . . ? C5 C4 C9 125.4(9) . . ? C3 C4 C9 126.4(8) . . ? C5 C4 Zr1 73.4(5) . . ? C3 C4 Zr1 72.9(5) . . ? C9 C4 Zr1 124.7(6) . . ? C4 C5 C1 107.7(6) . . ? C4 C5 C10 127.1(9) . . ? C1 C5 C10 124.9(8) . . ? C4 C5 Zr1 74.1(5) . . ? C1 C5 Zr1 72.8(5) . . ? C10 C5 Zr1 123.7(6) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 106.2(7) . . ? C12 C11 B1 125.3(6) . . ? C15 C11 B1 128.2(7) . . ? C12 C11 Fe1 68.9(4) . . ? C15 C11 Fe1 69.9(4) . . ? B1 C11 Fe1 121.4(5) . . ? C13 C12 C11 109.9(7) . . ? C13 C12 Fe1 70.4(4) . . ? C11 C12 Fe1 70.1(4) . . ? C13 C12 H12 125.1 . . ? C11 C12 H12 125.1 . . ? Fe1 C12 H12 126.0 . . ? C14 C13 C12 107.2(8) . . ? C14 C13 Fe1 70.2(5) . . ? C12 C13 Fe1 69.0(5) . . ? C14 C13 H13 126.4 . . ? C12 C13 H13 126.4 . . ? Fe1 C13 H13 126.0 . . ? C13 C14 C15 108.5(7) . . ? C13 C14 Fe1 69.7(4) . . ? C15 C14 Fe1 69.5(4) . . ? C13 C14 H14 125.7 . . ? C15 C14 H14 125.7 . . ? Fe1 C14 H14 126.7 . . ? C11 C15 C14 108.2(7) . . ? C11 C15 Fe1 69.4(4) . . ? C14 C15 Fe1 69.7(5) . . ? C11 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? Fe1 C15 H15 126.6 . . ? C17 C16 C20 107.0(9) . . ? C17 C16 Fe1 70.1(6) . . ? C20 C16 Fe1 69.2(5) . . ? C17 C16 H16 126.5 . . ? C20 C16 H16 126.5 . . ? Fe1 C16 H16 125.8 . . ? C18 C17 C16 108.5(9) . . ? C18 C17 Fe1 70.2(5) . . ? C16 C17 Fe1 69.5(5) . . ? C18 C17 H17 125.7 . . ? C16 C17 H17 125.7 . . ? Fe1 C17 H17 126.2 . . ? C19 C18 C17 109.7(11) . . ? C19 C18 Fe1 70.6(6) . . ? C17 C18 Fe1 70.1(6) . . ? C19 C18 H18 125.2 . . ? C17 C18 H18 125.2 . . ? Fe1 C18 H18 125.7 . . ? C18 C19 C20 107.2(9) . . ? C18 C19 Fe1 70.1(5) . . ? C20 C19 Fe1 68.4(5) . . ? C18 C19 H19 126.4 . . ? C20 C19 H19 126.4 . . ? Fe1 C19 H19 126.6 . . ? C16 C20 C19 107.7(9) . . ? C16 C20 Fe1 70.0(5) . . ? C19 C20 Fe1 70.3(5) . . ? C16 C20 H20 126.2 . . ? C19 C20 H20 126.2 . . ? Fe1 C20 H20 125.1 . . ? C22 C21 C25 106.7(6) . . ? C22 C21 B2 127.8(8) . . ? C25 C21 B2 125.3(7) . . ? C22 C21 Fe2 69.3(4) . . ? C25 C21 Fe2 69.4(4) . . ? B2 C21 Fe2 123.1(5) . . ? C23 C22 C21 108.0(8) . . ? C23 C22 Fe2 70.1(4) . . ? C21 C22 Fe2 69.4(4) . . ? C23 C22 H22 126.0 . . ? C21 C22 H22 126.0 . . ? Fe2 C22 H22 126.1 . . ? C22 C23 C24 109.4(7) . . ? C22 C23 Fe2 69.4(4) . . ? C24 C23 Fe2 69.8(4) . . ? C22 C23 H23 125.3 . . ? C24 C23 H23 125.3 . . ? Fe2 C23 H23 127.2 . . ? C23 C24 C25 107.2(7) . . ? C23 C24 Fe2 69.7(5) . . ? C25 C24 Fe2 69.3(4) . . ? C23 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? Fe2 C24 H24 126.2 . . ? C24 C25 C21 108.6(8) . . ? C24 C25 Fe2 69.8(5) . . ? C21 C25 Fe2 69.2(4) . . ? C24 C25 H25 125.7 . . ? C21 C25 H25 125.7 . . ? Fe2 C25 H25 126.9 . . ? C27 C26 C30 108.3(8) . . ? C27 C26 Fe2 69.7(5) . . ? C30 C26 Fe2 69.8(4) . . ? C27 C26 H26 125.8 . . ? C30 C26 H26 125.8 . . ? Fe2 C26 H26 126.2 . . ? C26 C27 C28 108.4(10) . . ? C26 C27 Fe2 70.2(6) . . ? C28 C27 Fe2 69.8(5) . . ? C26 C27 H27 125.8 . . ? C28 C27 H27 125.8 . . ? Fe2 C27 H27 125.8 . . ? C29 C28 C27 108.1(8) . . ? C29 C28 Fe2 69.6(5) . . ? C27 C28 Fe2 69.1(5) . . ? C29 C28 H28 126.0 . . ? C27 C28 H28 126.0 . . ? Fe2 C28 H28 126.8 . . ? C28 C29 C30 108.0(8) . . ? C28 C29 Fe2 70.1(5) . . ? C30 C29 Fe2 69.9(4) . . ? C28 C29 H29 126.0 . . ? C30 C29 H29 126.0 . . ? Fe2 C29 H29 125.6 . . ? C26 C30 C29 107.1(9) . . ? C26 C30 Fe2 69.2(4) . . ? C29 C30 Fe2 69.0(5) . . ? C26 C30 H30 126.4 . . ? C29 C30 H30 126.4 . . ? Fe2 C30 H30 126.9 . . ? C35 C31 C32 106.2(7) . . ? C35 C31 B3 129.1(7) . . ? C32 C31 B3 124.6(7) . . ? C35 C31 Fe3 68.1(4) . . ? C32 C31 Fe3 68.0(5) . . ? B3 C31 Fe3 126.5(5) . . ? C33 C32 C31 108.0(8) . . ? C33 C32 Fe3 69.7(6) . . ? C31 C32 Fe3 70.7(6) . . ? C33 C32 H32 126.0 . . ? C31 C32 H32 126.0 . . ? Fe3 C32 H32 125.2 . . ? C34 C33 C32 108.4(8) . . ? C34 C33 Fe3 69.7(7) . . ? C32 C33 Fe3 69.3(6) . . ? C34 C33 H33 125.8 . . ? C32 C33 H33 125.8 . . ? Fe3 C33 H33 126.8 . . ? C33 C34 C35 108.6(8) . . ? C33 C34 Fe3 70.4(6) . . ? C35 C34 Fe3 69.3(5) . . ? C33 C34 H34 125.7 . . ? C35 C34 H34 125.7 . . ? Fe3 C34 H34 126.2 . . ? C31 C35 C34 108.7(9) . . ? C31 C35 Fe3 71.3(4) . . ? C34 C35 Fe3 69.6(5) . . ? C31 C35 H35 125.6 . . ? C34 C35 H35 125.6 . . ? Fe3 C35 H35 125.1 . . ? C40 C36 C37 108.6(7) . . ? C40 C36 Fe3 70.3(5) . . ? C37 C36 Fe3 68.7(5) . . ? C40 C36 H36 125.7 . . ? C37 C36 H36 125.7 . . ? Fe3 C36 H36 126.8 . . ? C36 C37 C38 109.0(8) . . ? C36 C37 Fe3 70.7(5) . . ? C38 C37 Fe3 70.3(5) . . ? C36 C37 H37 125.5 . . ? C38 C37 H37 125.5 . . ? Fe3 C37 H37 125.1 . . ? C37 C38 C39 106.5(8) . . ? C37 C38 Fe3 68.5(4) . . ? C39 C38 Fe3 70.1(5) . . ? C37 C38 H38 126.8 . . ? C39 C38 H38 126.8 . . ? Fe3 C38 H38 126.1 . . ? C38 C39 C40 108.4(7) . . ? C38 C39 Fe3 69.0(6) . . ? C40 C39 Fe3 69.5(5) . . ? C38 C39 H39 125.8 . . ? C40 C39 H39 125.8 . . ? Fe3 C39 H39 127.3 . . ? C36 C40 C39 107.5(8) . . ? C36 C40 Fe3 69.5(6) . . ? C39 C40 Fe3 69.7(5) . . ? C36 C40 H40 126.2 . . ? C39 C40 H40 126.2 . . ? Fe3 C40 H40 126.2 . . ? 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 C3 Zr1 C1 C2 36.9(5) . . . . ? C5 Zr1 C1 C2 115.0(7) . . . . ? C4 Zr1 C1 C2 78.0(5) . . . . ? C3 Zr1 C1 C5 -78.1(5) . . . . ? C2 Zr1 C1 C5 -115.0(7) . . . . ? C4 Zr1 C1 C5 -36.9(4) . . . . ? C3 Zr1 C1 C6 158.1(10) . . . . ? C2 Zr1 C1 C6 121.2(12) . . . . ? C5 Zr1 C1 C6 -123.8(10) . . . . ? C4 Zr1 C1 C6 -160.8(10) . . . . ? C5 C1 C2 C3 1.3(10) . . . . ? C6 C1 C2 C3 173.8(9) . . . . ? Zr1 C1 C2 C3 -65.5(6) . . . . ? C5 C1 C2 C7 -173.3(9) . . . . ? C6 C1 C2 C7 -0.8(15) . . . . ? Zr1 C1 C2 C7 119.9(9) . . . . ? C5 C1 C2 Zr1 66.9(6) . . . . ? C6 C1 C2 Zr1 -120.6(9) . . . . ? C3 Zr1 C2 C1 -116.0(8) . . . . ? C5 Zr1 C2 C1 -37.7(5) . . . . ? C4 Zr1 C2 C1 -78.0(6) . . . . ? C1 Zr1 C2 C3 116.0(8) . . . . ? C5 Zr1 C2 C3 78.4(6) . . . . ? C4 Zr1 C2 C3 38.0(5) . . . . ? C1 Zr1 C2 C7 -125.6(10) . . . . ? C3 Zr1 C2 C7 118.4(10) . . . . ? C5 Zr1 C2 C7 -163.3(9) . . . . ? C4 Zr1 C2 C7 156.3(9) . . . . ? C1 C2 C3 C4 -1.5(9) . . . . ? C7 C2 C3 C4 173.5(8) . . . . ? Zr1 C2 C3 C4 -67.0(5) . . . . ? C1 C2 C3 C8 -171.9(9) . . . . ? C7 C2 C3 C8 3.1(15) . . . . ? Zr1 C2 C3 C8 122.6(10) . . . . ? C1 C2 C3 Zr1 65.5(6) . . . . ? C7 C2 C3 Zr1 -119.5(9) . . . . ? C1 Zr1 C3 C2 -36.1(5) . . . . ? C5 Zr1 C3 C2 -77.1(5) . . . . ? C4 Zr1 C3 C2 -113.8(7) . . . . ? C1 Zr1 C3 C4 77.7(5) . . . . ? C2 Zr1 C3 C4 113.8(7) . . . . ? C5 Zr1 C3 C4 36.7(4) . . . . ? C1 Zr1 C3 C8 -162.0(11) . . . . ? C2 Zr1 C3 C8 -125.9(12) . . . . ? C5 Zr1 C3 C8 156.9(10) . . . . ? C4 Zr1 C3 C8 120.2(11) . . . . ? C2 C3 C4 C5 1.1(9) . . . . ? C8 C3 C4 C5 172.0(8) . . . . ? Zr1 C3 C4 C5 -65.7(5) . . . . ? C2 C3 C4 C9 -172.3(8) . . . . ? C8 C3 C4 C9 -1.4(14) . . . . ? Zr1 C3 C4 C9 120.9(9) . . . . ? C2 C3 C4 Zr1 66.8(6) . . . . ? C8 C3 C4 Zr1 -122.3(9) . . . . ? C1 Zr1 C4 C5 37.7(4) . . . . ? C3 Zr1 C4 C5 115.1(6) . . . . ? C2 Zr1 C4 C5 77.5(5) . . . . ? C1 Zr1 C4 C3 -77.5(5) . . . . ? C2 Zr1 C4 C3 -37.6(4) . . . . ? C5 Zr1 C4 C3 -115.1(6) . . . . ? C1 Zr1 C4 C9 159.7(9) . . . . ? C3 Zr1 C4 C9 -122.8(10) . . . . ? C2 Zr1 C4 C9 -160.5(9) . . . . ? C5 Zr1 C4 C9 122.0(10) . . . . ? C3 C4 C5 C1 -0.3(9) . . . . ? C9 C4 C5 C1 173.2(8) . . . . ? Zr1 C4 C5 C1 -65.6(6) . . . . ? C3 C4 C5 C10 -174.1(8) . . . . ? C9 C4 C5 C10 -0.7(13) . . . . ? Zr1 C4 C5 C10 120.5(8) . . . . ? C3 C4 C5 Zr1 65.3(6) . . . . ? C9 C4 C5 Zr1 -121.2(8) . . . . ? C2 C1 C5 C4 -0.6(9) . . . . ? C6 C1 C5 C4 -172.9(8) . . . . ? Zr1 C1 C5 C4 66.5(5) . . . . ? C2 C1 C5 C10 173.4(8) . . . . ? C6 C1 C5 C10 1.1(14) . . . . ? Zr1 C1 C5 C10 -119.5(8) . . . . ? C2 C1 C5 Zr1 -67.1(6) . . . . ? C6 C1 C5 Zr1 120.6(9) . . . . ? C1 Zr1 C5 C4 -114.7(6) . . . . ? C3 Zr1 C5 C4 -37.4(4) . . . . ? C2 Zr1 C5 C4 -78.2(5) . . . . ? C3 Zr1 C5 C1 77.3(5) . . . . ? C2 Zr1 C5 C1 36.5(4) . . . . ? C4 Zr1 C5 C1 114.7(6) . . . . ? C1 Zr1 C5 C10 121.0(10) . . . . ? C3 Zr1 C5 C10 -161.8(9) . . . . ? C2 Zr1 C5 C10 157.5(9) . . . . ? C4 Zr1 C5 C10 -124.3(10) . . . . ? C20 Fe1 C11 C12 160.5(5) . . . . ? C16 Fe1 C11 C12 119.9(5) . . . . ? C17 Fe1 C11 C12 79.3(6) . . . . ? C18 Fe1 C11 C12 53.0(12) . . . . ? C19 Fe1 C11 C12 -173.4(9) . . . . ? C13 Fe1 C11 C12 -36.7(4) . . . . ? C15 Fe1 C11 C12 -117.4(6) . . . . ? C14 Fe1 C11 C12 -79.8(5) . . . . ? C20 Fe1 C11 C15 -82.1(6) . . . . ? C16 Fe1 C11 C15 -122.8(5) . . . . ? C12 Fe1 C11 C15 117.4(6) . . . . ? C17 Fe1 C11 C15 -163.3(6) . . . . ? C18 Fe1 C11 C15 170.4(10) . . . . ? C19 Fe1 C11 C15 -56.0(11) . . . . ? C13 Fe1 C11 C15 80.7(5) . . . . ? C14 Fe1 C11 C15 37.6(5) . . . . ? C20 Fe1 C11 B1 41.1(7) . . . . ? C16 Fe1 C11 B1 0.5(7) . . . . ? C12 Fe1 C11 B1 -119.4(7) . . . . ? C17 Fe1 C11 B1 -40.1(8) . . . . ? C18 Fe1 C11 B1 -66.3(13) . . . . ? C19 Fe1 C11 B1 67.3(11) . . . . ? C13 Fe1 C11 B1 -156.0(7) . . . . ? C15 Fe1 C11 B1 123.2(8) . . . . ? C14 Fe1 C11 B1 160.8(7) . . . . ? C15 C11 C12 C13 -1.0(8) . . . . ? B1 C11 C12 C13 173.6(7) . . . . ? Fe1 C11 C12 C13 59.4(5) . . . . ? C15 C11 C12 Fe1 -60.3(5) . . . . ? B1 C11 C12 Fe1 114.3(7) . . . . ? C20 Fe1 C12 C13 -168.0(8) . . . . ? C16 Fe1 C12 C13 162.5(6) . . . . ? C17 Fe1 C12 C13 121.0(6) . . . . ? C18 Fe1 C12 C13 81.0(6) . . . . ? C19 Fe1 C12 C13 52.9(10) . . . . ? C11 Fe1 C12 C13 -120.8(6) . . . . ? C15 Fe1 C12 C13 -82.2(5) . . . . ? C14 Fe1 C12 C13 -37.9(5) . . . . ? C20 Fe1 C12 C11 -47.2(10) . . . . ? C16 Fe1 C12 C11 -76.7(6) . . . . ? C17 Fe1 C12 C11 -118.2(5) . . . . ? C18 Fe1 C12 C11 -158.2(5) . . . . ? C19 Fe1 C12 C11 173.8(8) . . . . ? C13 Fe1 C12 C11 120.8(6) . . . . ? C15 Fe1 C12 C11 38.6(4) . . . . ? C14 Fe1 C12 C11 83.0(5) . . . . ? C11 C12 C13 C14 0.9(9) . . . . ? Fe1 C12 C13 C14 60.1(5) . . . . ? C11 C12 C13 Fe1 -59.1(5) . . . . ? C20 Fe1 C13 C14 47.2(14) . . . . ? C16 Fe1 C13 C14 -159.6(9) . . . . ? C12 Fe1 C13 C14 -118.3(8) . . . . ? C17 Fe1 C13 C14 165.0(6) . . . . ? C18 Fe1 C13 C14 123.1(6) . . . . ? C19 Fe1 C13 C14 82.3(7) . . . . ? C11 Fe1 C13 C14 -81.3(5) . . . . ? C15 Fe1 C13 C14 -37.5(5) . . . . ? C20 Fe1 C13 C12 165.5(11) . . . . ? C16 Fe1 C13 C12 -41.2(12) . . . . ? C17 Fe1 C13 C12 -76.7(7) . . . . ? C18 Fe1 C13 C12 -118.5(6) . . . . ? C19 Fe1 C13 C12 -159.4(5) . . . . ? C11 Fe1 C13 C12 37.0(5) . . . . ? C15 Fe1 C13 C12 80.8(5) . . . . ? C14 Fe1 C13 C12 118.3(8) . . . . ? C12 C13 C14 C15 -0.6(9) . . . . ? Fe1 C13 C14 C15 58.8(5) . . . . ? C12 C13 C14 Fe1 -59.3(5) . . . . ? C20 Fe1 C14 C13 -163.1(6) . . . . ? C16 Fe1 C14 C13 156.1(9) . . . . ? C12 Fe1 C14 C13 38.3(5) . . . . ? C17 Fe1 C14 C13 -37.9(12) . . . . ? C18 Fe1 C14 C13 -76.8(6) . . . . ? C19 Fe1 C14 C13 -118.8(6) . . . . ? C11 Fe1 C14 C13 82.6(5) . . . . ? C15 Fe1 C14 C13 120.0(7) . . . . ? C20 Fe1 C14 C15 76.9(6) . . . . ? C16 Fe1 C14 C15 36.1(11) . . . . ? C12 Fe1 C14 C15 -81.8(5) . . . . ? C17 Fe1 C14 C15 -157.9(9) . . . . ? C18 Fe1 C14 C15 163.2(5) . . . . ? C19 Fe1 C14 C15 121.2(5) . . . . ? C11 Fe1 C14 C15 -37.4(4) . . . . ? C13 Fe1 C14 C15 -120.0(7) . . . . ? C12 C11 C15 C14 0.6(8) . . . . ? B1 C11 C15 C14 -173.8(7) . . . . ? Fe1 C11 C15 C14 -59.1(5) . . . . ? C12 C11 C15 Fe1 59.6(5) . . . . ? B1 C11 C15 Fe1 -114.7(7) . . . . ? C13 C14 C15 C11 0.0(8) . . . . ? Fe1 C14 C15 C11 58.9(5) . . . . ? C13 C14 C15 Fe1 -58.9(5) . . . . ? C20 Fe1 C15 C11 117.0(5) . . . . ? C16 Fe1 C15 C11 74.0(6) . . . . ? C12 Fe1 C15 C11 -38.9(5) . . . . ? C17 Fe1 C15 C11 40.0(12) . . . . ? C18 Fe1 C15 C11 -168.1(13) . . . . ? C19 Fe1 C15 C11 159.6(5) . . . . ? C13 Fe1 C15 C11 -82.8(5) . . . . ? C14 Fe1 C15 C11 -119.6(7) . . . . ? C20 Fe1 C15 C14 -123.4(5) . . . . ? C16 Fe1 C15 C14 -166.4(5) . . . . ? C12 Fe1 C15 C14 80.7(5) . . . . ? C17 Fe1 C15 C14 159.6(9) . . . . ? C18 Fe1 C15 C14 -48.4(15) . . . . ? C19 Fe1 C15 C14 -80.8(6) . . . . ? C11 Fe1 C15 C14 119.6(7) . . . . ? C13 Fe1 C15 C14 36.9(4) . . . . ? C20 Fe1 C16 C17 118.0(8) . . . . ? C12 Fe1 C16 C17 -79.0(7) . . . . ? C18 Fe1 C16 C17 36.9(6) . . . . ? C19 Fe1 C16 C17 79.4(7) . . . . ? C11 Fe1 C16 C17 -120.2(6) . . . . ? C13 Fe1 C16 C17 -49.2(12) . . . . ? C15 Fe1 C16 C17 -160.6(5) . . . . ? C14 Fe1 C16 C17 172.4(9) . . . . ? C12 Fe1 C16 C20 163.0(6) . . . . ? C17 Fe1 C16 C20 -118.0(8) . . . . ? C18 Fe1 C16 C20 -81.1(6) . . . . ? C19 Fe1 C16 C20 -38.6(6) . . . . ? C11 Fe1 C16 C20 121.7(6) . . . . ? C13 Fe1 C16 C20 -167.2(9) . . . . ? C15 Fe1 C16 C20 81.4(6) . . . . ? C14 Fe1 C16 C20 54.3(12) . . . . ? C20 C16 C17 C18 0.1(10) . . . . ? Fe1 C16 C17 C18 -59.5(6) . . . . ? C20 C16 C17 Fe1 59.6(5) . . . . ? C20 Fe1 C17 C18 81.2(7) . . . . ? C16 Fe1 C17 C18 119.7(9) . . . . ? C12 Fe1 C17 C18 -122.1(7) . . . . ? C19 Fe1 C17 C18 36.4(7) . . . . ? C11 Fe1 C17 C18 -164.3(6) . . . . ? C13 Fe1 C17 C18 -80.9(7) . . . . ? C15 Fe1 C17 C18 166.6(9) . . . . ? C14 Fe1 C17 C18 -53.0(13) . . . . ? C20 Fe1 C17 C16 -38.5(5) . . . . ? C12 Fe1 C17 C16 118.2(6) . . . . ? C18 Fe1 C17 C16 -119.7(9) . . . . ? C19 Fe1 C17 C16 -83.3(6) . . . . ? C11 Fe1 C17 C16 76.0(6) . . . . ? C13 Fe1 C17 C16 159.4(5) . . . . ? C15 Fe1 C17 C16 47.0(12) . . . . ? C14 Fe1 C17 C16 -172.7(8) . . . . ? C16 C17 C18 C19 -0.6(10) . . . . ? Fe1 C17 C18 C19 -59.7(6) . . . . ? C16 C17 C18 Fe1 59.1(6) . . . . ? C20 Fe1 C18 C19 38.7(6) . . . . ? C16 Fe1 C18 C19 83.0(7) . . . . ? C12 Fe1 C18 C19 -164.3(6) . . . . ? C17 Fe1 C18 C19 120.5(10) . . . . ? C11 Fe1 C18 C19 157.1(9) . . . . ? C13 Fe1 C18 C19 -121.6(6) . . . . ? C15 Fe1 C18 C19 -43.1(17) . . . . ? C14 Fe1 C18 C19 -80.0(8) . . . . ? C20 Fe1 C18 C17 -81.8(7) . . . . ? C16 Fe1 C18 C17 -37.5(6) . . . . ? C12 Fe1 C18 C17 75.2(8) . . . . ? C19 Fe1 C18 C17 -120.5(10) . . . . ? C11 Fe1 C18 C17 36.6(14) . . . . ? C13 Fe1 C18 C17 117.9(7) . . . . ? C15 Fe1 C18 C17 -163.5(11) . . . . ? C14 Fe1 C18 C17 159.5(6) . . . . ? C17 C18 C19 C20 0.8(10) . . . . ? Fe1 C18 C19 C20 -58.6(6) . . . . ? C17 C18 C19 Fe1 59.4(6) . . . . ? C20 Fe1 C19 C18 -118.7(8) . . . . ? C16 Fe1 C19 C18 -80.5(7) . . . . ? C12 Fe1 C19 C18 38.6(12) . . . . ? C17 Fe1 C19 C18 -36.7(7) . . . . ? C11 Fe1 C19 C18 -153.5(9) . . . . ? C13 Fe1 C19 C18 77.6(7) . . . . ? C15 Fe1 C19 C18 164.6(6) . . . . ? C14 Fe1 C19 C18 120.8(7) . . . . ? C16 Fe1 C19 C20 38.2(5) . . . . ? C12 Fe1 C19 C20 157.3(8) . . . . ? C17 Fe1 C19 C20 82.0(6) . . . . ? C18 Fe1 C19 C20 118.7(8) . . . . ? C11 Fe1 C19 C20 -34.7(11) . . . . ? C13 Fe1 C19 C20 -163.7(5) . . . . ? C15 Fe1 C19 C20 -76.7(6) . . . . ? C14 Fe1 C19 C20 -120.5(5) . . . . ? C17 C16 C20 C19 0.4(9) . . . . ? Fe1 C16 C20 C19 60.6(6) . . . . ? C17 C16 C20 Fe1 -60.2(6) . . . . ? C18 C19 C20 C16 -0.7(9) . . . . ? Fe1 C19 C20 C16 -60.4(5) . . . . ? C18 C19 C20 Fe1 59.6(6) . . . . ? C12 Fe1 C20 C16 -40.6(12) . . . . ? C17 Fe1 C20 C16 38.2(6) . . . . ? C18 Fe1 C20 C16 81.3(6) . . . . ? C19 Fe1 C20 C16 118.2(8) . . . . ? C11 Fe1 C20 C16 -74.9(6) . . . . ? C13 Fe1 C20 C16 164.3(11) . . . . ? C15 Fe1 C20 C16 -117.9(6) . . . . ? C14 Fe1 C20 C16 -160.2(6) . . . . ? C16 Fe1 C20 C19 -118.2(8) . . . . ? C12 Fe1 C20 C19 -158.8(8) . . . . ? C17 Fe1 C20 C19 -80.0(6) . . . . ? C18 Fe1 C20 C19 -36.9(5) . . . . ? C11 Fe1 C20 C19 166.9(5) . . . . ? C13 Fe1 C20 C19 46.1(14) . . . . ? C15 Fe1 C20 C19 123.9(5) . . . . ? C14 Fe1 C20 C19 81.6(7) . . . . ? C27 Fe2 C21 C22 83.1(5) . . . . ? C29 Fe2 C21 C22 -167.9(10) . . . . ? C26 Fe2 C21 C22 124.0(5) . . . . ? C28 Fe2 C21 C22 53.2(9) . . . . ? C30 Fe2 C21 C22 164.7(5) . . . . ? C25 Fe2 C21 C22 -118.1(6) . . . . ? C23 Fe2 C21 C22 -37.5(5) . . . . ? C24 Fe2 C21 C22 -81.0(5) . . . . ? C27 Fe2 C21 C25 -158.8(5) . . . . ? C29 Fe2 C21 C25 -49.7(12) . . . . ? C26 Fe2 C21 C25 -117.9(5) . . . . ? C28 Fe2 C21 C25 171.4(7) . . . . ? C22 Fe2 C21 C25 118.1(6) . . . . ? C30 Fe2 C21 C25 -77.2(5) . . . . ? C23 Fe2 C21 C25 80.6(5) . . . . ? C24 Fe2 C21 C25 37.1(5) . . . . ? C27 Fe2 C21 B2 -39.4(8) . . . . ? C29 Fe2 C21 B2 69.7(14) . . . . ? C26 Fe2 C21 B2 1.6(8) . . . . ? C28 Fe2 C21 B2 -69.2(10) . . . . ? C22 Fe2 C21 B2 -122.4(9) . . . . ? C30 Fe2 C21 B2 42.3(9) . . . . ? C25 Fe2 C21 B2 119.4(8) . . . . ? C23 Fe2 C21 B2 -159.9(8) . . . . ? C24 Fe2 C21 B2 156.6(8) . . . . ? C25 C21 C22 C23 0.1(7) . . . . ? B2 C21 C22 C23 176.1(6) . . . . ? Fe2 C21 C22 C23 59.6(5) . . . . ? C25 C21 C22 Fe2 -59.5(4) . . . . ? B2 C21 C22 Fe2 116.5(7) . . . . ? C27 Fe2 C22 C23 126.4(5) . . . . ? C29 Fe2 C22 C23 51.4(11) . . . . ? C26 Fe2 C22 C23 167.1(5) . . . . ? C28 Fe2 C22 C23 83.9(6) . . . . ? C21 Fe2 C22 C23 -119.2(7) . . . . ? C30 Fe2 C22 C23 -161.3(11) . . . . ? C25 Fe2 C22 C23 -80.5(5) . . . . ? C24 Fe2 C22 C23 -36.6(5) . . . . ? C27 Fe2 C22 C21 -114.4(5) . . . . ? C29 Fe2 C22 C21 170.6(9) . . . . ? C26 Fe2 C22 C21 -73.7(6) . . . . ? C28 Fe2 C22 C21 -156.9(5) . . . . ? C30 Fe2 C22 C21 -42.1(13) . . . . ? C25 Fe2 C22 C21 38.7(4) . . . . ? C23 Fe2 C22 C21 119.2(7) . . . . ? C24 Fe2 C22 C21 82.6(5) . . . . ? C21 C22 C23 C24 -0.9(8) . . . . ? Fe2 C22 C23 C24 58.4(5) . . . . ? C21 C22 C23 Fe2 -59.2(5) . . . . ? C27 Fe2 C23 C22 -72.5(6) . . . . ? C29 Fe2 C23 C22 -158.2(6) . . . . ? C26 Fe2 C23 C22 -35.9(12) . . . . ? C28 Fe2 C23 C22 -115.4(6) . . . . ? C21 Fe2 C23 C22 38.2(5) . . . . ? C30 Fe2 C23 C22 164.4(8) . . . . ? C25 Fe2 C23 C22 82.9(5) . . . . ? C24 Fe2 C23 C22 121.2(6) . . . . ? C27 Fe2 C23 C24 166.3(5) . . . . ? C29 Fe2 C23 C24 80.6(6) . . . . ? C26 Fe2 C23 C24 -157.1(9) . . . . ? C28 Fe2 C23 C24 123.4(5) . . . . ? C22 Fe2 C23 C24 -121.2(6) . . . . ? C21 Fe2 C23 C24 -83.0(5) . . . . ? C30 Fe2 C23 C24 43.3(10) . . . . ? C25 Fe2 C23 C24 -38.3(4) . . . . ? C22 C23 C24 C25 1.2(8) . . . . ? Fe2 C23 C24 C25 59.4(5) . . . . ? C22 C23 C24 Fe2 -58.1(5) . . . . ? C27 Fe2 C24 C23 -41.9(14) . . . . ? C29 Fe2 C24 C23 -118.3(5) . . . . ? C26 Fe2 C24 C23 162.5(6) . . . . ? C28 Fe2 C24 C23 -77.2(6) . . . . ? C22 Fe2 C24 C23 36.6(4) . . . . ? C21 Fe2 C24 C23 80.9(5) . . . . ? C30 Fe2 C24 C23 -161.8(4) . . . . ? C25 Fe2 C24 C23 118.5(7) . . . . ? C27 Fe2 C24 C25 -160.4(12) . . . . ? C29 Fe2 C24 C25 123.1(6) . . . . ? C26 Fe2 C24 C25 44.0(9) . . . . ? C28 Fe2 C24 C25 164.3(6) . . . . ? C22 Fe2 C24 C25 -81.9(5) . . . . ? C21 Fe2 C24 C25 -37.6(5) . . . . ? C30 Fe2 C24 C25 79.7(6) . . . . ? C23 Fe2 C24 C25 -118.5(7) . . . . ? C23 C24 C25 C21 -1.1(8) . . . . ? Fe2 C24 C25 C21 58.5(5) . . . . ? C23 C24 C25 Fe2 -59.6(5) . . . . ? C22 C21 C25 C24 0.6(7) . . . . ? B2 C21 C25 C24 -175.5(6) . . . . ? Fe2 C21 C25 C24 -58.8(5) . . . . ? C22 C21 C25 Fe2 59.5(4) . . . . ? B2 C21 C25 Fe2 -116.6(6) . . . . ? C27 Fe2 C25 C24 167.3(8) . . . . ? C29 Fe2 C25 C24 -76.8(6) . . . . ? C26 Fe2 C25 C24 -160.7(5) . . . . ? C28 Fe2 C25 C24 -47.5(13) . . . . ? C22 Fe2 C25 C24 81.7(5) . . . . ? C21 Fe2 C25 C24 120.2(7) . . . . ? C30 Fe2 C25 C24 -118.1(5) . . . . ? C23 Fe2 C25 C24 38.0(5) . . . . ? C27 Fe2 C25 C21 47.0(10) . . . . ? C29 Fe2 C25 C21 163.0(4) . . . . ? C26 Fe2 C25 C21 79.0(5) . . . . ? C28 Fe2 C25 C21 -167.8(11) . . . . ? C22 Fe2 C25 C21 -38.6(4) . . . . ? C30 Fe2 C25 C21 121.6(5) . . . . ? C23 Fe2 C25 C21 -82.3(5) . . . . ? C24 Fe2 C25 C21 -120.2(7) . . . . ? C29 Fe2 C26 C27 81.4(7) . . . . ? C28 Fe2 C26 C27 38.0(6) . . . . ? C22 Fe2 C26 C27 -75.7(6) . . . . ? C21 Fe2 C26 C27 -116.7(6) . . . . ? C30 Fe2 C26 C27 119.6(7) . . . . ? C25 Fe2 C26 C27 -159.1(5) . . . . ? C23 Fe2 C26 C27 -48.4(11) . . . . ? C24 Fe2 C26 C27 169.4(7) . . . . ? C27 Fe2 C26 C30 -119.6(7) . . . . ? C29 Fe2 C26 C30 -38.1(6) . . . . ? C28 Fe2 C26 C30 -81.5(6) . . . . ? C22 Fe2 C26 C30 164.8(5) . . . . ? C21 Fe2 C26 C30 123.7(5) . . . . ? C25 Fe2 C26 C30 81.4(6) . . . . ? C23 Fe2 C26 C30 -168.0(8) . . . . ? C24 Fe2 C26 C30 49.8(9) . . . . ? C30 C26 C27 C28 -0.2(8) . . . . ? Fe2 C26 C27 C28 -59.6(5) . . . . ? C30 C26 C27 Fe2 59.3(5) . . . . ? C29 Fe2 C27 C26 -82.2(6) . . . . ? C28 Fe2 C27 C26 -119.3(9) . . . . ? C22 Fe2 C27 C26 122.4(5) . . . . ? C21 Fe2 C27 C26 79.2(6) . . . . ? C30 Fe2 C27 C26 -37.9(5) . . . . ? C25 Fe2 C27 C26 45.7(11) . . . . ? C23 Fe2 C27 C26 162.8(5) . . . . ? C24 Fe2 C27 C26 -164.6(11) . . . . ? C29 Fe2 C27 C28 37.1(6) . . . . ? C26 Fe2 C27 C28 119.3(9) . . . . ? C22 Fe2 C27 C28 -118.2(6) . . . . ? C21 Fe2 C27 C28 -161.5(6) . . . . ? C30 Fe2 C27 C28 81.5(6) . . . . ? C25 Fe2 C27 C28 165.0(8) . . . . ? C23 Fe2 C27 C28 -77.8(7) . . . . ? C24 Fe2 C27 C28 -45.3(16) . . . . ? C26 C27 C28 C29 0.9(9) . . . . ? Fe2 C27 C28 C29 -58.9(6) . . . . ? C26 C27 C28 Fe2 59.8(5) . . . . ? C27 Fe2 C28 C29 119.7(8) . . . . ? C26 Fe2 C28 C29 82.5(6) . . . . ? C22 Fe2 C28 C29 -160.5(5) . . . . ? C21 Fe2 C28 C29 161.4(6) . . . . ? C30 Fe2 C28 C29 38.3(5) . . . . ? C25 Fe2 C28 C29 -38.1(13) . . . . ? C23 Fe2 C28 C29 -117.2(5) . . . . ? C24 Fe2 C28 C29 -74.9(6) . . . . ? C29 Fe2 C28 C27 -119.7(8) . . . . ? C26 Fe2 C28 C27 -37.2(6) . . . . ? C22 Fe2 C28 C27 79.9(6) . . . . ? C21 Fe2 C28 C27 41.7(10) . . . . ? C30 Fe2 C28 C27 -81.4(6) . . . . ? C25 Fe2 C28 C27 -157.8(10) . . . . ? C23 Fe2 C28 C27 123.1(6) . . . . ? C24 Fe2 C28 C27 165.4(6) . . . . ? C27 C28 C29 C30 -1.2(9) . . . . ? Fe2 C28 C29 C30 -59.8(5) . . . . ? C27 C28 C29 Fe2 58.6(5) . . . . ? C27 Fe2 C29 C28 -37.8(5) . . . . ? C26 Fe2 C29 C28 -80.9(6) . . . . ? C22 Fe2 C29 C28 45.4(11) . . . . ? C21 Fe2 C29 C28 -154.7(10) . . . . ? C30 Fe2 C29 C28 -118.9(8) . . . . ? C25 Fe2 C29 C28 167.0(5) . . . . ? C23 Fe2 C29 C28 82.3(6) . . . . ? C24 Fe2 C29 C28 124.8(5) . . . . ? C27 Fe2 C29 C30 81.1(6) . . . . ? C26 Fe2 C29 C30 38.0(6) . . . . ? C28 Fe2 C29 C30 118.9(8) . . . . ? C22 Fe2 C29 C30 164.3(8) . . . . ? C21 Fe2 C29 C30 -35.9(14) . . . . ? C25 Fe2 C29 C30 -74.1(7) . . . . ? C23 Fe2 C29 C30 -158.8(6) . . . . ? C24 Fe2 C29 C30 -116.3(6) . . . . ? C27 C26 C30 C29 -0.5(8) . . . . ? Fe2 C26 C30 C29 58.8(5) . . . . ? C27 C26 C30 Fe2 -59.3(5) . . . . ? C28 C29 C30 C26 1.1(9) . . . . ? Fe2 C29 C30 C26 -58.9(5) . . . . ? C28 C29 C30 Fe2 60.0(6) . . . . ? C27 Fe2 C30 C26 37.1(5) . . . . ? C29 Fe2 C30 C26 118.9(9) . . . . ? C28 Fe2 C30 C26 81.4(6) . . . . ? C22 Fe2 C30 C26 -41.8(14) . . . . ? C21 Fe2 C30 C26 -73.8(6) . . . . ? C25 Fe2 C30 C26 -116.1(5) . . . . ? C23 Fe2 C30 C26 170.3(8) . . . . ? C24 Fe2 C30 C26 -158.4(5) . . . . ? C27 Fe2 C30 C29 -81.8(7) . . . . ? C26 Fe2 C30 C29 -118.9(9) . . . . ? C28 Fe2 C30 C29 -37.5(6) . . . . ? C22 Fe2 C30 C29 -160.7(11) . . . . ? C21 Fe2 C30 C29 167.3(6) . . . . ? C25 Fe2 C30 C29 124.9(6) . . . . ? C23 Fe2 C30 C29 51.4(12) . . . . ? C24 Fe2 C30 C29 82.6(7) . . . . ? C37 Fe3 C31 C35 164.7(6) . . . . ? C34 Fe3 C31 C35 -38.1(6) . . . . ? C38 Fe3 C31 C35 -161.4(10) . . . . ? C32 Fe3 C31 C35 -119.2(7) . . . . ? C36 Fe3 C31 C35 122.7(6) . . . . ? C33 Fe3 C31 C35 -81.0(6) . . . . ? C39 Fe3 C31 C35 49.8(11) . . . . ? C40 Fe3 C31 C35 81.4(6) . . . . ? C37 Fe3 C31 C32 -76.2(6) . . . . ? C35 Fe3 C31 C32 119.2(7) . . . . ? C34 Fe3 C31 C32 81.1(6) . . . . ? C38 Fe3 C31 C32 -42.2(12) . . . . ? C36 Fe3 C31 C32 -118.1(5) . . . . ? C33 Fe3 C31 C32 38.1(5) . . . . ? C39 Fe3 C31 C32 169.0(8) . . . . ? C40 Fe3 C31 C32 -159.4(5) . . . . ? C37 Fe3 C31 B3 41.5(8) . . . . ? C35 Fe3 C31 B3 -123.2(9) . . . . ? C34 Fe3 C31 B3 -161.3(8) . . . . ? C38 Fe3 C31 B3 75.4(12) . . . . ? C32 Fe3 C31 B3 117.6(8) . . . . ? C36 Fe3 C31 B3 -0.5(8) . . . . ? C33 Fe3 C31 B3 155.8(8) . . . . ? C39 Fe3 C31 B3 -73.4(11) . . . . ? C40 Fe3 C31 B3 -41.8(8) . . . . ? C35 C31 C32 C33 -2.5(11) . . . . ? B3 C31 C32 C33 179.9(8) . . . . ? Fe3 C31 C32 C33 -60.0(7) . . . . ? C35 C31 C32 Fe3 57.5(6) . . . . ? B3 C31 C32 Fe3 -120.1(7) . . . . ? C37 Fe3 C32 C33 -120.2(6) . . . . ? C35 Fe3 C32 C33 81.0(6) . . . . ? C34 Fe3 C32 C33 36.7(5) . . . . ? C38 Fe3 C32 C33 -78.5(7) . . . . ? C36 Fe3 C32 C33 -161.1(6) . . . . ? C39 Fe3 C32 C33 -51.0(12) . . . . ? C40 Fe3 C32 C33 170.1(9) . . . . ? C31 Fe3 C32 C33 118.6(8) . . . . ? C37 Fe3 C32 C31 121.2(5) . . . . ? C35 Fe3 C32 C31 -37.6(4) . . . . ? C34 Fe3 C32 C31 -81.9(5) . . . . ? C38 Fe3 C32 C31 162.9(5) . . . . ? C36 Fe3 C32 C31 80.3(6) . . . . ? C33 Fe3 C32 C31 -118.6(8) . . . . ? C39 Fe3 C32 C31 -169.5(8) . . . . ? C40 Fe3 C32 C31 51.5(11) . . . . ? C31 C32 C33 C34 1.8(12) . . . . ? Fe3 C32 C33 C34 -58.8(8) . . . . ? C31 C32 C33 Fe3 60.6(7) . . . . ? C37 Fe3 C33 C34 -163.1(5) . . . . ? C35 Fe3 C33 C34 37.9(5) . . . . ? C38 Fe3 C33 C34 -121.0(5) . . . . ? C32 Fe3 C33 C34 120.1(8) . . . . ? C36 Fe3 C33 C34 165.8(8) . . . . ? C39 Fe3 C33 C34 -79.9(6) . . . . ? C40 Fe3 C33 C34 -48.7(13) . . . . ? C31 Fe3 C33 C34 81.7(5) . . . . ? C37 Fe3 C33 C32 76.8(6) . . . . ? C35 Fe3 C33 C32 -82.1(6) . . . . ? C34 Fe3 C33 C32 -120.1(8) . . . . ? C38 Fe3 C33 C32 119.0(6) . . . . ? C36 Fe3 C33 C32 45.7(11) . . . . ? C39 Fe3 C33 C32 160.1(5) . . . . ? C40 Fe3 C33 C32 -168.7(10) . . . . ? C31 Fe3 C33 C32 -38.4(5) . . . . ? C32 C33 C34 C35 -0.4(12) . . . . ? Fe3 C33 C34 C35 -59.0(7) . . . . ? C32 C33 C34 Fe3 58.6(7) . . . . ? C37 Fe3 C34 C33 40.0(12) . . . . ? C35 Fe3 C34 C33 -119.7(8) . . . . ? C38 Fe3 C34 C33 76.2(7) . . . . ? C32 Fe3 C34 C33 -37.6(5) . . . . ? C36 Fe3 C34 C33 -162.6(10) . . . . ? C39 Fe3 C34 C33 119.6(5) . . . . ? C40 Fe3 C34 C33 162.1(5) . . . . ? C31 Fe3 C34 C33 -82.1(6) . . . . ? C37 Fe3 C34 C35 159.7(9) . . . . ? C38 Fe3 C34 C35 -164.1(6) . . . . ? C32 Fe3 C34 C35 82.1(6) . . . . ? C36 Fe3 C34 C35 -42.9(14) . . . . ? C33 Fe3 C34 C35 119.7(8) . . . . ? C39 Fe3 C34 C35 -120.7(6) . . . . ? C40 Fe3 C34 C35 -78.2(7) . . . . ? C31 Fe3 C34 C35 37.6(6) . . . . ? C32 C31 C35 C34 2.3(10) . . . . ? B3 C31 C35 C34 179.7(8) . . . . ? Fe3 C31 C35 C34 59.7(6) . . . . ? C32 C31 C35 Fe3 -57.5(6) . . . . ? B3 C31 C35 Fe3 120.0(8) . . . . ? C33 C34 C35 C31 -1.2(11) . . . . ? Fe3 C34 C35 C31 -60.8(6) . . . . ? C33 C34 C35 Fe3 59.6(7) . . . . ? C37 Fe3 C35 C31 -38.8(15) . . . . ? C34 Fe3 C35 C31 119.2(9) . . . . ? C38 Fe3 C35 C31 160.2(12) . . . . ? C32 Fe3 C35 C31 38.1(5) . . . . ? C36 Fe3 C35 C31 -76.0(7) . . . . ? C33 Fe3 C35 C31 82.3(6) . . . . ? C39 Fe3 C35 C31 -161.1(5) . . . . ? C40 Fe3 C35 C31 -118.3(5) . . . . ? C37 Fe3 C35 C34 -158.0(12) . . . . ? C38 Fe3 C35 C34 41.1(16) . . . . ? C32 Fe3 C35 C34 -81.0(7) . . . . ? C36 Fe3 C35 C34 164.8(6) . . . . ? C33 Fe3 C35 C34 -36.8(6) . . . . ? C39 Fe3 C35 C34 79.7(7) . . . . ? C40 Fe3 C35 C34 122.6(6) . . . . ? C31 Fe3 C35 C34 -119.2(9) . . . . ? C37 Fe3 C36 C40 120.1(7) . . . . ? C35 Fe3 C36 C40 -79.4(6) . . . . ? C34 Fe3 C36 C40 -46.6(13) . . . . ? C38 Fe3 C36 C40 82.2(6) . . . . ? C32 Fe3 C36 C40 -163.6(5) . . . . ? C33 Fe3 C36 C40 163.1(8) . . . . ? C39 Fe3 C36 C40 38.2(5) . . . . ? C31 Fe3 C36 C40 -120.8(5) . . . . ? C35 Fe3 C36 C37 160.5(5) . . . . ? C34 Fe3 C36 C37 -166.8(10) . . . . ? C38 Fe3 C36 C37 -37.9(6) . . . . ? C32 Fe3 C36 C37 76.2(6) . . . . ? C33 Fe3 C36 C37 42.9(11) . . . . ? C39 Fe3 C36 C37 -82.0(6) . . . . ? C40 Fe3 C36 C37 -120.1(7) . . . . ? C31 Fe3 C36 C37 119.1(5) . . . . ? C40 C36 C37 C38 0.9(11) . . . . ? Fe3 C36 C37 C38 60.1(7) . . . . ? C40 C36 C37 Fe3 -59.2(7) . . . . ? C35 Fe3 C37 C36 -50.4(15) . . . . ? C34 Fe3 C37 C36 169.1(10) . . . . ? C38 Fe3 C37 C36 119.5(9) . . . . ? C32 Fe3 C37 C36 -120.6(6) . . . . ? C33 Fe3 C37 C36 -162.1(6) . . . . ? C39 Fe3 C37 C36 81.0(6) . . . . ? C40 Fe3 C37 C36 36.9(6) . . . . ? C31 Fe3 C37 C36 -79.1(7) . . . . ? C35 Fe3 C37 C38 -169.9(12) . . . . ? C34 Fe3 C37 C38 49.6(13) . . . . ? C32 Fe3 C37 C38 119.9(6) . . . . ? C36 Fe3 C37 C38 -119.5(9) . . . . ? C33 Fe3 C37 C38 78.4(7) . . . . ? C39 Fe3 C37 C38 -38.5(6) . . . . ? C40 Fe3 C37 C38 -82.6(7) . . . . ? C31 Fe3 C37 C38 161.4(6) . . . . ? C36 C37 C38 C39 -0.1(11) . . . . ? Fe3 C37 C38 C39 60.2(7) . . . . ? C36 C37 C38 Fe3 -60.3(7) . . . . ? C35 Fe3 C38 C37 169.8(12) . . . . ? C34 Fe3 C38 C37 -159.6(7) . . . . ? C32 Fe3 C38 C37 -77.2(7) . . . . ? C36 Fe3 C38 C37 37.4(6) . . . . ? C33 Fe3 C38 C37 -119.2(7) . . . . ? C39 Fe3 C38 C37 117.8(9) . . . . ? C40 Fe3 C38 C37 80.6(7) . . . . ? C31 Fe3 C38 C37 -46.1(13) . . . . ? C37 Fe3 C38 C39 -117.8(9) . . . . ? C35 Fe3 C38 C39 52.0(16) . . . . ? C34 Fe3 C38 C39 82.6(7) . . . . ? C32 Fe3 C38 C39 165.0(5) . . . . ? C36 Fe3 C38 C39 -80.4(6) . . . . ? C33 Fe3 C38 C39 123.0(6) . . . . ? C40 Fe3 C38 C39 -37.2(5) . . . . ? C31 Fe3 C38 C39 -163.9(8) . . . . ? C37 C38 C39 C40 -0.7(11) . . . . ? Fe3 C38 C39 C40 58.5(6) . . . . ? C37 C38 C39 Fe3 -59.2(7) . . . . ? C37 Fe3 C39 C38 38.8(6) . . . . ? C35 Fe3 C39 C38 -160.2(6) . . . . ? C34 Fe3 C39 C38 -117.0(6) . . . . ? C32 Fe3 C39 C38 -37.4(12) . . . . ? C36 Fe3 C39 C38 82.7(6) . . . . ? C33 Fe3 C39 C38 -75.0(7) . . . . ? C40 Fe3 C39 C38 120.3(7) . . . . ? C31 Fe3 C39 C38 162.7(8) . . . . ? C37 Fe3 C39 C40 -81.5(5) . . . . ? C35 Fe3 C39 C40 79.5(6) . . . . ? C34 Fe3 C39 C40 122.7(5) . . . . ? C38 Fe3 C39 C40 -120.3(7) . . . . ? C32 Fe3 C39 C40 -157.7(9) . . . . ? C36 Fe3 C39 C40 -37.6(5) . . . . ? C33 Fe3 C39 C40 164.7(5) . . . . ? C31 Fe3 C39 C40 42.4(11) . . . . ? C37 C36 C40 C39 -1.3(11) . . . . ? Fe3 C36 C40 C39 -59.5(6) . . . . ? C37 C36 C40 Fe3 58.2(7) . . . . ? C38 C39 C40 C36 1.2(11) . . . . ? Fe3 C39 C40 C36 59.4(7) . . . . ? C38 C39 C40 Fe3 -58.2(7) . . . . ? C37 Fe3 C40 C36 -37.2(5) . . . . ? C35 Fe3 C40 C36 120.5(5) . . . . ? C34 Fe3 C40 C36 163.4(5) . . . . ? C38 Fe3 C40 C36 -81.6(5) . . . . ? C32 Fe3 C40 C36 39.6(11) . . . . ? C33 Fe3 C40 C36 -160.2(10) . . . . ? C39 Fe3 C40 C36 -118.8(7) . . . . ? C31 Fe3 C40 C36 77.5(6) . . . . ? C37 Fe3 C40 C39 81.5(5) . . . . ? C35 Fe3 C40 C39 -120.8(5) . . . . ? C34 Fe3 C40 C39 -77.8(6) . . . . ? C38 Fe3 C40 C39 37.2(5) . . . . ? C32 Fe3 C40 C39 158.4(9) . . . . ? C36 Fe3 C40 C39 118.8(7) . . . . ? C33 Fe3 C40 C39 -41.4(13) . . . . ? C31 Fe3 C40 C39 -163.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.752 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.108 data_wa1302 _database_code_depnum_ccdc_archive 'CCDC 894224' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 B2 Cl2 Fe Zr2' _chemical_formula_sum 'C30 H34 B2 Cl2 Fe Zr2' _chemical_formula_weight 725.38 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' B B 0.0013 0.0007 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-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 12.0793(4) _cell_length_b 13.6685(5) _cell_length_c 35.3514(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5836.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24095 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.3 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7585 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 33532 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5158 _reflns_number_gt 4115 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5158 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Fe1 Fe 0.82857(4) 0.68625(4) 0.951778(12) 0.02974(13) Uani 1 1 d . . . B1 B 0.5778(4) 0.6045(3) 0.94212(12) 0.0374(9) Uani 1 1 d . . . H1A H 0.597(4) 0.544(4) 0.9595(12) 0.057(13) Uiso 1 1 d . . . H1B H 0.480(4) 0.633(4) 0.9478(12) 0.060(13) Uiso 1 1 d . . . H1C H 0.574(4) 0.578(3) 0.9095(12) 0.054(13) Uiso 1 1 d . . . B2 B 0.9648(4) 0.6711(4) 0.87467(11) 0.0364(9) Uani 1 1 d . . . H2A H 0.997(4) 0.749(3) 0.8734(11) 0.049(11) Uiso 1 1 d . . . H2B H 1.018(4) 0.620(3) 0.8562(11) 0.046(11) Uiso 1 1 d . . . H2C H 0.882(3) 0.674(3) 0.8556(10) 0.038(10) Uiso 1 1 d . . . Zr1 Zr 0.41030(3) 0.60265(2) 0.896320(9) 0.02852(10) Uani 1 1 d . . . Cl1 Cl 0.50295(9) 0.56036(8) 0.83485(2) 0.0453(2) Uani 1 1 d . . . Zr2 Zr 0.93846(3) 0.61705(3) 0.806601(9) 0.03126(10) Uani 1 1 d . . . Cl2 Cl 1.13457(9) 0.56808(11) 0.79278(3) 0.0619(3) Uani 1 1 d . . . C1 C 0.6577(3) 0.6940(3) 0.94785(9) 0.0337(8) Uani 1 1 d . . . C2 C 0.6967(3) 0.7311(3) 0.98350(10) 0.0420(9) Uani 1 1 d . . . H2 H 0.6765 0.7064 1.0077 0.050 Uiso 1 1 calc R . . C3 C 0.7697(3) 0.8099(3) 0.97705(12) 0.0482(10) Uani 1 1 d . . . H3 H 0.8067 0.8466 0.9960 0.058 Uiso 1 1 calc R . . C4 C 0.7787(3) 0.8249(3) 0.93764(13) 0.0484(10) Uani 1 1 d . . . H4 H 0.8220 0.8736 0.9254 0.058 Uiso 1 1 calc R . . C5 C 0.7106(3) 0.7534(3) 0.91963(10) 0.0404(9) Uani 1 1 d . . . H5 H 0.7016 0.7462 0.8931 0.048 Uiso 1 1 calc R . . C6 C 0.9485(3) 0.6320(3) 0.91606(9) 0.0317(7) Uani 1 1 d . . . C7 C 0.8803(3) 0.5543(3) 0.93048(10) 0.0356(8) Uani 1 1 d . . . H7 H 0.8378 0.5104 0.9156 0.043 Uiso 1 1 calc R . . C8 C 0.8864(3) 0.5537(3) 0.97060(10) 0.0387(9) Uani 1 1 d . . . H8 H 0.8482 0.5101 0.9869 0.046 Uiso 1 1 calc R . . C9 C 0.9591(3) 0.6288(3) 0.98202(10) 0.0416(9) Uani 1 1 d . . . H9 H 0.9794 0.6440 1.0073 0.050 Uiso 1 1 calc R . . C10 C 0.9967(3) 0.6778(3) 0.94887(9) 0.0344(8) Uani 1 1 d . . . H10 H 1.0458 0.7321 0.9485 0.041 Uiso 1 1 calc R . . C11 C 0.2599(3) 0.7269(3) 0.89499(13) 0.0491(10) Uani 1 1 d . . . H11 H 0.1866 0.7069 0.9008 0.059 Uiso 1 1 calc R . . C12 C 0.3083(4) 0.7265(3) 0.85943(11) 0.0487(11) Uani 1 1 d . . . H12 H 0.2752 0.7040 0.8367 0.058 Uiso 1 1 calc R . . C13 C 0.4147(4) 0.7654(3) 0.86322(12) 0.0525(11) Uani 1 1 d . . . H13 H 0.4657 0.7756 0.8432 0.063 Uiso 1 1 calc R . . C14 C 0.4338(3) 0.7866(3) 0.90092(12) 0.0441(9) Uani 1 1 d . . . H14 H 0.4997 0.8131 0.9114 0.053 Uiso 1 1 calc R . . C15 C 0.3378(4) 0.7617(3) 0.92059(10) 0.0434(9) Uani 1 1 d . . . H15 H 0.3274 0.7675 0.9471 0.052 Uiso 1 1 calc R . . C16 C 0.4025(4) 0.4278(3) 0.91548(13) 0.0477(10) Uani 1 1 d . . . H16 H 0.4708 0.3940 0.9179 0.057 Uiso 1 1 calc R . . C17 C 0.3383(4) 0.4351(3) 0.88260(12) 0.0520(11) Uani 1 1 d . . . H17 H 0.3542 0.4051 0.8590 0.062 Uiso 1 1 calc R . . C18 C 0.2468(4) 0.4941(3) 0.89060(12) 0.0479(10) Uani 1 1 d . . . H18 H 0.1908 0.5135 0.8733 0.058 Uiso 1 1 calc R . . C19 C 0.2529(3) 0.5196(3) 0.92915(11) 0.0434(9) Uani 1 1 d . . . H19 H 0.2006 0.5581 0.9426 0.052 Uiso 1 1 calc R . . C20 C 0.3481(4) 0.4791(3) 0.94399(11) 0.0460(10) Uani 1 1 d . . . H20 H 0.3725 0.4851 0.9694 0.055 Uiso 1 1 calc R . . C21 C 0.8194(5) 0.7497(4) 0.78133(18) 0.0794(17) Uani 1 1 d . . . H21 H 0.7438 0.7481 0.7886 0.095 Uiso 1 1 calc R . . C22 C 0.8653(6) 0.7030(4) 0.74973(14) 0.0723(17) Uani 1 1 d . . . H22 H 0.8261 0.6661 0.7313 0.087 Uiso 1 1 calc R . . C23 C 0.9774(6) 0.7205(4) 0.75020(13) 0.0741(16) Uani 1 1 d . . . H23 H 1.0298 0.6970 0.7323 0.089 Uiso 1 1 calc R . . C24 C 1.0010(6) 0.7796(4) 0.78197(16) 0.0805(19) Uani 1 1 d . . . H24 H 1.0720 0.8024 0.7895 0.097 Uiso 1 1 calc R . . C25 C 0.9029(7) 0.7982(4) 0.80001(15) 0.0765(18) Uani 1 1 d . . . H25 H 0.8939 0.8380 0.8218 0.092 Uiso 1 1 calc R . . C26 C 0.8557(4) 0.4762(3) 0.77348(11) 0.0495(11) Uani 1 1 d . . . H26 H 0.8622 0.4758 0.7467 0.059 Uiso 1 1 calc R . . C27 C 0.7695(3) 0.5185(3) 0.79435(10) 0.0447(10) Uani 1 1 d . . . H27 H 0.7065 0.5508 0.7842 0.054 Uiso 1 1 calc R . . C28 C 0.7921(3) 0.5051(3) 0.83266(10) 0.0407(9) Uani 1 1 d . . . H28 H 0.7471 0.5264 0.8531 0.049 Uiso 1 1 calc R . . C29 C 0.8932(4) 0.4545(3) 0.83577(10) 0.0431(9) Uani 1 1 d . . . H29 H 0.9296 0.4370 0.8586 0.052 Uiso 1 1 calc R . . C30 C 0.9306(4) 0.4346(3) 0.79898(11) 0.0520(11) Uani 1 1 d . . . H30 H 0.9954 0.3991 0.7925 0.062 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 0.0256(3) 0.0315(3) 0.0322(2) -0.00026(19) 0.00113(18) 0.0017(2) B1 0.026(2) 0.041(2) 0.046(2) 0.0047(19) -0.0039(16) 0.0044(19) B2 0.032(2) 0.046(3) 0.0317(19) -0.0050(17) -0.0013(16) -0.0027(19) Zr1 0.02532(17) 0.02624(18) 0.03399(17) 0.00121(13) 0.00109(12) 0.00042(13) Cl1 0.0487(6) 0.0476(6) 0.0395(4) -0.0031(4) 0.0130(4) 0.0085(5) Zr2 0.03334(19) 0.03250(19) 0.02794(16) -0.00056(13) -0.00138(12) -0.00113(14) Cl2 0.0373(6) 0.1049(10) 0.0435(5) -0.0143(5) 0.0097(4) -0.0002(6) C1 0.0226(17) 0.037(2) 0.0414(18) 0.0018(15) 0.0022(13) 0.0051(16) C2 0.034(2) 0.049(2) 0.0427(19) -0.0095(17) 0.0046(15) 0.0038(18) C3 0.039(2) 0.043(2) 0.063(2) -0.0144(19) -0.0006(18) 0.0002(19) C4 0.029(2) 0.032(2) 0.084(3) 0.011(2) 0.0041(19) 0.0031(17) C5 0.0316(19) 0.044(2) 0.0454(19) 0.0107(17) 0.0010(15) 0.0084(18) C6 0.0272(18) 0.0328(19) 0.0350(16) -0.0041(14) -0.0010(13) -0.0001(15) C7 0.033(2) 0.032(2) 0.0412(18) -0.0029(15) 0.0004(15) 0.0037(16) C8 0.037(2) 0.038(2) 0.0408(19) 0.0099(16) 0.0061(15) 0.0059(17) C9 0.038(2) 0.054(3) 0.0331(18) 0.0031(16) -0.0050(15) 0.0088(19) C10 0.0261(18) 0.041(2) 0.0365(17) -0.0029(15) -0.0003(14) 0.0010(16) C11 0.027(2) 0.032(2) 0.088(3) 0.007(2) 0.0024(19) 0.0068(16) C12 0.066(3) 0.032(2) 0.048(2) 0.0005(17) -0.022(2) 0.010(2) C13 0.071(3) 0.028(2) 0.058(2) 0.0120(18) 0.029(2) 0.005(2) C14 0.036(2) 0.0237(18) 0.073(3) -0.0018(17) -0.0090(18) 0.0018(16) C15 0.056(3) 0.035(2) 0.0395(19) -0.0008(16) 0.0018(17) 0.0148(19) C16 0.037(2) 0.027(2) 0.079(3) 0.0121(19) 0.001(2) 0.0004(17) C17 0.064(3) 0.036(2) 0.056(2) -0.0082(18) 0.011(2) -0.019(2) C18 0.042(2) 0.041(2) 0.061(2) 0.0125(19) -0.0150(19) -0.0174(19) C19 0.037(2) 0.036(2) 0.057(2) 0.0072(17) 0.0132(18) -0.0075(18) C20 0.054(3) 0.040(2) 0.044(2) 0.0155(17) -0.0020(18) -0.012(2) C21 0.072(4) 0.067(4) 0.099(4) 0.036(3) -0.010(3) 0.029(3) C22 0.117(5) 0.046(3) 0.054(3) 0.014(2) -0.039(3) -0.012(3) C23 0.119(5) 0.061(3) 0.042(2) 0.019(2) 0.006(3) -0.018(3) C24 0.121(6) 0.051(3) 0.070(3) 0.023(3) -0.025(3) -0.042(4) C25 0.138(6) 0.036(3) 0.056(3) 0.001(2) -0.020(3) 0.018(3) C26 0.071(3) 0.038(2) 0.0388(19) -0.0099(17) -0.0056(19) -0.012(2) C27 0.040(2) 0.046(2) 0.047(2) 0.0053(17) -0.0103(17) -0.0157(19) C28 0.043(2) 0.038(2) 0.0420(19) 0.0035(16) -0.0028(16) -0.0085(18) C29 0.061(3) 0.029(2) 0.0394(19) 0.0038(15) -0.0063(17) 0.0008(19) C30 0.072(3) 0.033(2) 0.051(2) -0.0065(17) 0.000(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C10 2.036(3) . ? Fe1 C3 2.039(4) . ? Fe1 C5 2.041(4) . ? Fe1 C2 2.042(4) . ? Fe1 C4 2.051(4) . ? Fe1 C7 2.052(4) . ? Fe1 C8 2.053(4) . ? Fe1 C6 2.060(3) . ? Fe1 C9 2.060(4) . ? Fe1 C1 2.072(3) . ? B1 C1 1.571(6) . ? B1 Zr1 2.591(4) . ? B1 H1A 1.06(5) . ? B1 H1B 1.26(5) . ? B1 H1C 1.21(4) . ? B2 C6 1.570(5) . ? B2 Zr2 2.537(4) . ? B2 H2A 1.13(5) . ? B2 H2B 1.15(4) . ? B2 H2C 1.20(4) . ? Zr1 C12 2.467(4) . ? Zr1 C18 2.479(4) . ? Zr1 C16 2.485(4) . ? Zr1 C11 2.487(4) . ? Zr1 C15 2.495(4) . ? Zr1 C17 2.498(4) . ? Zr1 C19 2.500(4) . ? Zr1 C20 2.502(4) . ? Zr1 Cl1 2.5116(9) . ? Zr1 C13 2.514(4) . ? Zr1 C14 2.535(4) . ? Zr1 H1B 2.05(4) . ? Zr1 H1C 2.06(5) . ? Zr2 C26 2.465(4) . ? Zr2 C21 2.480(5) . ? Zr2 C27 2.484(4) . ? Zr2 C23 2.489(4) . ? Zr2 C22 2.491(4) . ? Zr2 C24 2.504(5) . ? Zr2 Cl2 2.5097(12) . ? Zr2 C30 2.510(4) . ? Zr2 C29 2.510(4) . ? Zr2 C28 2.513(4) . ? Zr2 C25 2.523(5) . ? Zr2 H2B 2.00(4) . ? Zr2 H2C 2.02(4) . ? C1 C5 1.436(5) . ? C1 C2 1.439(5) . ? C2 C3 1.410(6) . ? C2 H2 0.9500 . ? C3 C4 1.413(6) . ? C3 H3 0.9500 . ? C4 C5 1.428(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.438(5) . ? C6 C10 1.440(5) . ? C7 C8 1.420(5) . ? C7 H7 0.9500 . ? C8 C9 1.410(6) . ? C8 H8 0.9500 . ? C9 C10 1.424(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 C15 1.389(6) . ? C11 H11 0.9500 . ? C12 C13 1.397(7) . ? C12 H12 0.9500 . ? C13 C14 1.383(6) . ? C13 H13 0.9500 . ? C14 C15 1.394(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C20 1.391(6) . ? C16 C17 1.401(7) . ? C16 H16 0.9500 . ? C17 C18 1.398(7) . ? C17 H17 0.9500 . ? C18 C19 1.408(6) . ? C18 H18 0.9500 . ? C19 C20 1.381(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C25 1.375(9) . ? C21 C22 1.401(8) . ? C21 H21 0.9500 . ? C22 C23 1.376(9) . ? C22 H22 0.9500 . ? C23 C24 1.413(8) . ? C23 H23 0.9500 . ? C24 C25 1.370(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.397(6) . ? C26 C27 1.402(6) . ? C26 H26 0.9500 . ? C27 C28 1.394(5) . ? C27 H27 0.9500 . ? C28 C29 1.408(6) . ? C28 H28 0.9500 . ? C29 C30 1.403(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Fe1 C3 114.63(16) . . ? C10 Fe1 C5 133.94(15) . . ? C3 Fe1 C5 68.17(17) . . ? C10 Fe1 C2 145.33(15) . . ? C3 Fe1 C2 40.43(17) . . ? C5 Fe1 C2 68.05(16) . . ? C10 Fe1 C4 109.46(16) . . ? C3 Fe1 C4 40.41(18) . . ? C5 Fe1 C4 40.86(17) . . ? C2 Fe1 C4 68.12(17) . . ? C10 Fe1 C7 68.16(15) . . ? C3 Fe1 C7 174.39(16) . . ? C5 Fe1 C7 113.79(16) . . ? C2 Fe1 C7 134.65(17) . . ? C4 Fe1 C7 144.34(16) . . ? C10 Fe1 C8 68.07(16) . . ? C3 Fe1 C8 135.07(16) . . ? C5 Fe1 C8 144.60(17) . . ? C2 Fe1 C8 110.65(16) . . ? C4 Fe1 C8 174.15(17) . . ? C7 Fe1 C8 40.48(14) . . ? C10 Fe1 C6 41.17(13) . . ? C3 Fe1 C6 144.28(17) . . ? C5 Fe1 C6 108.16(14) . . ? C2 Fe1 C6 173.35(15) . . ? C4 Fe1 C6 112.94(16) . . ? C7 Fe1 C6 40.95(15) . . ? C8 Fe1 C6 69.00(14) . . ? C10 Fe1 C9 40.66(15) . . ? C3 Fe1 C9 110.80(17) . . ? C5 Fe1 C9 174.10(17) . . ? C2 Fe1 C9 115.23(15) . . ? C4 Fe1 C9 134.70(18) . . ? C7 Fe1 C9 67.82(16) . . ? C8 Fe1 C9 40.09(17) . . ? C6 Fe1 C9 69.06(14) . . ? C10 Fe1 C1 173.26(13) . . ? C3 Fe1 C1 68.89(16) . . ? C5 Fe1 C1 40.87(15) . . ? C2 Fe1 C1 40.92(14) . . ? C4 Fe1 C1 69.14(16) . . ? C7 Fe1 C1 108.87(15) . . ? C8 Fe1 C1 113.95(16) . . ? C6 Fe1 C1 132.70(14) . . ? C9 Fe1 C1 144.76(15) . . ? C1 B1 Zr1 124.6(3) . . ? C1 B1 H1A 114(3) . . ? Zr1 B1 H1A 122(3) . . ? C1 B1 H1B 108(2) . . ? Zr1 B1 H1B 51(2) . . ? H1A B1 H1B 111(3) . . ? C1 B1 H1C 112(2) . . ? Zr1 B1 H1C 51(2) . . ? H1A B1 H1C 109(3) . . ? H1B B1 H1C 102(3) . . ? C6 B2 Zr2 140.3(3) . . ? C6 B2 H2A 113(2) . . ? Zr2 B2 H2A 106(2) . . ? C6 B2 H2B 113(2) . . ? Zr2 B2 H2B 50(2) . . ? H2A B2 H2B 111(3) . . ? C6 B2 H2C 115.4(18) . . ? Zr2 B2 H2C 51.4(18) . . ? H2A B2 H2C 103(3) . . ? H2B B2 H2C 100(3) . . ? C12 Zr1 C18 88.26(15) . . ? C12 Zr1 C16 141.72(15) . . ? C18 Zr1 C16 54.31(14) . . ? C12 Zr1 C11 32.50(14) . . ? C18 Zr1 C11 79.92(15) . . ? C16 Zr1 C11 129.33(14) . . ? C12 Zr1 C15 53.76(13) . . ? C18 Zr1 C15 105.64(16) . . ? C16 Zr1 C15 136.91(14) . . ? C11 Zr1 C15 32.39(14) . . ? C12 Zr1 C17 110.67(16) . . ? C18 Zr1 C17 32.63(16) . . ? C16 Zr1 C17 32.65(15) . . ? C11 Zr1 C17 111.61(16) . . ? C15 Zr1 C17 138.03(16) . . ? C12 Zr1 C19 100.21(16) . . ? C18 Zr1 C19 32.86(13) . . ? C16 Zr1 C19 53.70(14) . . ? C11 Zr1 C19 76.31(14) . . ? C15 Zr1 C19 88.22(14) . . ? C17 Zr1 C19 53.77(14) . . ? C12 Zr1 C20 132.05(16) . . ? C18 Zr1 C20 53.95(13) . . ? C16 Zr1 C20 32.40(14) . . ? C11 Zr1 C20 104.75(15) . . ? C15 Zr1 C20 104.55(14) . . ? C17 Zr1 C20 53.63(14) . . ? C19 Zr1 C20 32.05(14) . . ? C12 Zr1 Cl1 85.59(11) . . ? C18 Zr1 Cl1 98.45(11) . . ? C16 Zr1 Cl1 91.81(11) . . ? C11 Zr1 Cl1 117.79(11) . . ? C15 Zr1 Cl1 130.86(9) . . ? C17 Zr1 Cl1 77.06(10) . . ? C19 Zr1 Cl1 129.50(10) . . ? C20 Zr1 Cl1 124.14(11) . . ? C12 Zr1 C13 32.56(16) . . ? C18 Zr1 C13 120.56(16) . . ? C16 Zr1 C13 168.05(15) . . ? C11 Zr1 C13 53.31(15) . . ? C15 Zr1 C13 52.90(13) . . ? C17 Zr1 C13 136.76(16) . . ? C19 Zr1 C13 129.33(15) . . ? C20 Zr1 C13 156.55(14) . . ? Cl1 Zr1 C13 77.97(10) . . ? C12 Zr1 C14 53.78(14) . . ? C18 Zr1 C14 133.45(14) . . ? C16 Zr1 C14 160.07(15) . . ? C11 Zr1 C14 53.54(14) . . ? C15 Zr1 C14 32.16(14) . . ? C17 Zr1 C14 163.91(15) . . ? C19 Zr1 C14 120.36(14) . . ? C20 Zr1 C14 131.30(14) . . ? Cl1 Zr1 C14 103.52(10) . . ? C13 Zr1 C14 31.79(14) . . ? C12 Zr1 B1 135.53(15) . . ? C18 Zr1 B1 132.76(14) . . ? C16 Zr1 B1 82.45(15) . . ? C11 Zr1 B1 125.13(15) . . ? C15 Zr1 B1 92.90(14) . . ? C17 Zr1 B1 113.70(16) . . ? C19 Zr1 B1 107.94(14) . . ? C20 Zr1 B1 79.62(14) . . ? Cl1 Zr1 B1 101.24(10) . . ? C13 Zr1 B1 105.42(16) . . ? C14 Zr1 B1 82.14(14) . . ? C12 Zr1 H1B 122.3(14) . . ? C18 Zr1 H1B 121.6(14) . . ? C16 Zr1 H1B 88.4(14) . . ? C11 Zr1 H1B 100.2(14) . . ? C15 Zr1 H1B 70.1(14) . . ? C17 Zr1 H1B 120.3(14) . . ? C19 Zr1 H1B 89.7(14) . . ? C20 Zr1 H1B 70.4(14) . . ? Cl1 Zr1 H1B 129.2(14) . . ? C13 Zr1 H1B 102.9(14) . . ? C14 Zr1 H1B 72.1(14) . . ? B1 Zr1 H1B 28.6(14) . . ? C12 Zr1 H1C 135.4(13) . . ? C18 Zr1 H1C 133.3(13) . . ? C16 Zr1 H1C 79.4(13) . . ? C11 Zr1 H1C 144.9(13) . . ? C15 Zr1 H1C 113.7(13) . . ? C17 Zr1 H1C 103.1(13) . . ? C19 Zr1 H1C 123.4(13) . . ? C20 Zr1 H1C 91.4(13) . . ? Cl1 Zr1 H1C 74.3(12) . . ? C13 Zr1 H1C 103.3(13) . . ? C14 Zr1 H1C 92.4(14) . . ? B1 Zr1 H1C 27.2(12) . . ? H1B Zr1 H1C 55.7(18) . . ? C26 Zr2 C21 99.5(2) . . ? C26 Zr2 C27 32.91(15) . . ? C21 Zr2 C27 81.8(2) . . ? C26 Zr2 C23 98.05(17) . . ? C21 Zr2 C23 53.6(2) . . ? C27 Zr2 C23 108.90(17) . . ? C26 Zr2 C22 80.87(16) . . ? C21 Zr2 C22 32.7(2) . . ? C27 Zr2 C22 79.84(17) . . ? C23 Zr2 C22 32.1(2) . . ? C26 Zr2 C24 130.58(16) . . ? C21 Zr2 C24 53.2(2) . . ? C27 Zr2 C24 131.97(18) . . ? C23 Zr2 C24 32.87(18) . . ? C22 Zr2 C24 53.67(18) . . ? C26 Zr2 Cl2 94.70(12) . . ? C21 Zr2 Cl2 132.22(16) . . ? C27 Zr2 Cl2 126.67(11) . . ? C23 Zr2 Cl2 79.46(17) . . ? C22 Zr2 Cl2 107.67(17) . . ? C24 Zr2 Cl2 83.3(2) . . ? C26 Zr2 C30 32.61(15) . . ? C21 Zr2 C30 131.7(2) . . ? C27 Zr2 C30 53.93(16) . . ? C23 Zr2 C30 119.05(17) . . ? C22 Zr2 C30 111.63(16) . . ? C24 Zr2 C30 148.9(2) . . ? Cl2 Zr2 C30 75.52(12) . . ? C26 Zr2 C29 54.22(13) . . ? C21 Zr2 C29 131.99(19) . . ? C27 Zr2 C29 54.03(14) . . ? C23 Zr2 C29 150.83(16) . . ? C22 Zr2 C29 132.23(16) . . ? C24 Zr2 C29 173.97(17) . . ? Cl2 Zr2 C29 92.82(11) . . ? C30 Zr2 C29 32.46(13) . . ? C26 Zr2 C28 54.07(14) . . ? C21 Zr2 C28 99.75(18) . . ? C27 Zr2 C28 32.38(12) . . ? C23 Zr2 C28 140.58(18) . . ? C22 Zr2 C28 109.48(18) . . ? C24 Zr2 C28 151.7(2) . . ? Cl2 Zr2 C28 124.96(11) . . ? C30 Zr2 C28 53.67(15) . . ? C29 Zr2 C28 32.57(14) . . ? C26 Zr2 C25 130.80(18) . . ? C21 Zr2 C25 31.9(2) . . ? C27 Zr2 C25 112.1(2) . . ? C23 Zr2 C25 53.2(2) . . ? C22 Zr2 C25 53.29(17) . . ? C24 Zr2 C25 31.6(2) . . ? Cl2 Zr2 C25 113.9(2) . . ? C30 Zr2 C25 163.40(18) . . ? C29 Zr2 C25 150.4(2) . . ? C28 Zr2 C25 120.8(2) . . ? C26 Zr2 B2 136.78(15) . . ? C21 Zr2 B2 101.6(2) . . ? C27 Zr2 B2 115.24(13) . . ? C23 Zr2 B2 124.78(18) . . ? C22 Zr2 B2 132.27(17) . . ? C24 Zr2 B2 91.92(17) . . ? Cl2 Zr2 B2 98.28(10) . . ? C30 Zr2 B2 113.32(14) . . ? C29 Zr2 B2 84.00(14) . . ? C28 Zr2 B2 85.29(13) . . ? C25 Zr2 B2 79.82(16) . . ? C26 Zr2 H2B 128.7(13) . . ? C21 Zr2 H2B 125.5(13) . . ? C27 Zr2 H2B 123.9(13) . . ? C23 Zr2 H2B 126.9(13) . . ? C22 Zr2 H2B 150.4(13) . . ? C24 Zr2 H2B 98.3(13) . . ? Cl2 Zr2 H2B 73.9(13) . . ? C30 Zr2 H2B 97.5(13) . . ? C29 Zr2 H2B 76.1(13) . . ? C28 Zr2 H2B 91.6(12) . . ? C25 Zr2 H2B 98.3(13) . . ? B2 Zr2 H2B 26.2(13) . . ? C26 Zr2 H2C 125.0(12) . . ? C21 Zr2 H2C 80.3(11) . . ? C27 Zr2 H2C 94.7(12) . . ? C23 Zr2 H2C 122.1(12) . . ? C22 Zr2 H2C 113.0(11) . . ? C24 Zr2 H2C 93.2(12) . . ? Cl2 Zr2 H2C 126.0(11) . . ? C30 Zr2 H2C 117.6(12) . . ? C29 Zr2 H2C 85.2(12) . . ? C28 Zr2 H2C 71.6(12) . . ? C25 Zr2 H2C 69.0(12) . . ? B2 Zr2 H2C 27.8(11) . . ? H2B Zr2 H2C 53.3(17) . . ? C5 C1 C2 105.3(3) . . ? C5 C1 B1 128.6(3) . . ? C2 C1 B1 126.1(3) . . ? C5 C1 Fe1 68.4(2) . . ? C2 C1 Fe1 68.4(2) . . ? B1 C1 Fe1 125.5(3) . . ? C3 C2 C1 109.4(3) . . ? C3 C2 Fe1 69.7(2) . . ? C1 C2 Fe1 70.6(2) . . ? C3 C2 H2 125.3 . . ? C1 C2 H2 125.3 . . ? Fe1 C2 H2 126.0 . . ? C2 C3 C4 108.6(4) . . ? C2 C3 Fe1 69.9(2) . . ? C4 C3 Fe1 70.2(2) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe1 C3 H3 125.7 . . ? C3 C4 C5 107.2(4) . . ? C3 C4 Fe1 69.4(2) . . ? C5 C4 Fe1 69.2(2) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe1 C4 H4 126.6 . . ? C4 C5 C1 109.5(3) . . ? C4 C5 Fe1 69.9(2) . . ? C1 C5 Fe1 70.7(2) . . ? C4 C5 H5 125.2 . . ? C1 C5 H5 125.2 . . ? Fe1 C5 H5 125.7 . . ? C7 C6 C10 105.5(3) . . ? C7 C6 B2 130.8(3) . . ? C10 C6 B2 123.5(3) . . ? C7 C6 Fe1 69.2(2) . . ? C10 C6 Fe1 68.55(19) . . ? B2 C6 Fe1 122.5(3) . . ? C8 C7 C6 109.2(3) . . ? C8 C7 Fe1 69.8(2) . . ? C6 C7 Fe1 69.8(2) . . ? C8 C7 H7 125.4 . . ? C6 C7 H7 125.4 . . ? Fe1 C7 H7 126.5 . . ? C9 C8 C7 108.3(3) . . ? C9 C8 Fe1 70.2(2) . . ? C7 C8 Fe1 69.7(2) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe1 C8 H8 125.8 . . ? C8 C9 C10 107.8(3) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 Fe1 68.8(2) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 127.0 . . ? C9 C10 C6 109.3(3) . . ? C9 C10 Fe1 70.6(2) . . ? C6 C10 Fe1 70.3(2) . . ? C9 C10 H10 125.4 . . ? C6 C10 H10 125.4 . . ? Fe1 C10 H10 125.4 . . ? C12 C11 C15 107.8(4) . . ? C12 C11 Zr1 73.0(2) . . ? C15 C11 Zr1 74.1(2) . . ? C12 C11 H11 126.1 . . ? C15 C11 H11 126.1 . . ? Zr1 C11 H11 118.7 . . ? C11 C12 C13 107.4(4) . . ? C11 C12 Zr1 74.5(2) . . ? C13 C12 Zr1 75.6(2) . . ? C11 C12 H12 126.3 . . ? C13 C12 H12 126.3 . . ? Zr1 C12 H12 115.8 . . ? C14 C13 C12 109.0(4) . . ? C14 C13 Zr1 75.0(2) . . ? C12 C13 Zr1 71.9(2) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Zr1 C13 H13 119.4 . . ? C13 C14 C15 106.9(4) . . ? C13 C14 Zr1 73.3(2) . . ? C15 C14 Zr1 72.3(2) . . ? C13 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? Zr1 C14 H14 119.8 . . ? C11 C15 C14 108.8(3) . . ? C11 C15 Zr1 73.5(2) . . ? C14 C15 Zr1 75.5(2) . . ? C11 C15 H15 125.6 . . ? C14 C15 H15 125.6 . . ? Zr1 C15 H15 117.3 . . ? C20 C16 C17 107.7(4) . . ? C20 C16 Zr1 74.4(2) . . ? C17 C16 Zr1 74.2(2) . . ? C20 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Zr1 C16 H16 117.3 . . ? C18 C17 C16 108.1(4) . . ? C18 C17 Zr1 72.9(2) . . ? C16 C17 Zr1 73.2(2) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Zr1 C17 H17 119.7 . . ? C17 C18 C19 107.3(4) . . ? C17 C18 Zr1 74.4(2) . . ? C19 C18 Zr1 74.4(2) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? Zr1 C18 H18 116.9 . . ? C20 C19 C18 108.2(4) . . ? C20 C19 Zr1 74.0(2) . . ? C18 C19 Zr1 72.7(2) . . ? C20 C19 H19 125.9 . . ? C18 C19 H19 125.9 . . ? Zr1 C19 H19 119.2 . . ? C19 C20 C16 108.6(4) . . ? C19 C20 Zr1 73.9(2) . . ? C16 C20 Zr1 73.2(2) . . ? C19 C20 H20 125.7 . . ? C16 C20 H20 125.7 . . ? Zr1 C20 H20 119.1 . . ? C25 C21 C22 108.2(6) . . ? C25 C21 Zr2 75.8(3) . . ? C22 C21 Zr2 74.1(3) . . ? C25 C21 H21 125.9 . . ? C22 C21 H21 125.9 . . ? Zr2 C21 H21 116.3 . . ? C23 C22 C21 107.5(5) . . ? C23 C22 Zr2 73.9(3) . . ? C21 C22 Zr2 73.2(3) . . ? C23 C22 H22 126.3 . . ? C21 C22 H22 126.3 . . ? Zr2 C22 H22 118.6 . . ? C22 C23 C24 107.9(6) . . ? C22 C23 Zr2 74.0(3) . . ? C24 C23 Zr2 74.1(3) . . ? C22 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? Zr2 C23 H23 117.8 . . ? C25 C24 C23 107.6(6) . . ? C25 C24 Zr2 75.0(3) . . ? C23 C24 Zr2 73.0(3) . . ? C25 C24 H24 126.2 . . ? C23 C24 H24 126.2 . . ? Zr2 C24 H24 117.8 . . ? C24 C25 C21 108.8(5) . . ? C24 C25 Zr2 73.4(3) . . ? C21 C25 Zr2 72.3(3) . . ? C24 C25 H25 125.6 . . ? C21 C25 H25 125.6 . . ? Zr2 C25 H25 120.4 . . ? C30 C26 C27 108.0(3) . . ? C30 C26 Zr2 75.5(2) . . ? C27 C26 Zr2 74.3(2) . . ? C30 C26 H26 126.0 . . ? C27 C26 H26 126.0 . . ? Zr2 C26 H26 116.4 . . ? C28 C27 C26 108.1(4) . . ? C28 C27 Zr2 75.0(2) . . ? C26 C27 Zr2 72.8(2) . . ? C28 C27 H27 125.9 . . ? C26 C27 H27 125.9 . . ? Zr2 C27 H27 118.2 . . ? C27 C28 C29 108.1(4) . . ? C27 C28 Zr2 72.6(2) . . ? C29 C28 Zr2 73.6(2) . . ? C27 C28 H28 125.9 . . ? C29 C28 H28 125.9 . . ? Zr2 C28 H28 119.7 . . ? C30 C29 C28 107.5(4) . . ? C30 C29 Zr2 73.8(2) . . ? C28 C29 Zr2 73.8(2) . . ? C30 C29 H29 126.2 . . ? C28 C29 H29 126.2 . . ? Zr2 C29 H29 118.1 . . ? C26 C30 C29 108.2(4) . . ? C26 C30 Zr2 71.9(2) . . ? C29 C30 Zr2 73.8(2) . . ? C26 C30 H30 125.9 . . ? C29 C30 H30 125.9 . . ? Zr2 C30 H30 120.2 . . ? 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 C1 B1 Zr1 C12 -11.9(4) . . . . ? C1 B1 Zr1 C18 -163.8(3) . . . . ? C1 B1 Zr1 C16 173.7(3) . . . . ? C1 B1 Zr1 C11 -52.8(4) . . . . ? C1 B1 Zr1 C15 -49.3(3) . . . . ? C1 B1 Zr1 C17 164.0(3) . . . . ? C1 B1 Zr1 C19 -138.4(3) . . . . ? C1 B1 Zr1 C20 -153.6(3) . . . . ? C1 B1 Zr1 Cl1 83.3(3) . . . . ? C1 B1 Zr1 C13 2.9(3) . . . . ? C1 B1 Zr1 C14 -19.0(3) . . . . ? C6 B2 Zr2 C26 7.1(5) . . . . ? C6 B2 Zr2 C21 124.8(4) . . . . ? C6 B2 Zr2 C27 38.4(5) . . . . ? C6 B2 Zr2 C23 178.2(4) . . . . ? C6 B2 Zr2 C22 137.9(4) . . . . ? C6 B2 Zr2 C24 177.5(5) . . . . ? C6 B2 Zr2 Cl2 -98.9(4) . . . . ? C6 B2 Zr2 C30 -21.2(5) . . . . ? C6 B2 Zr2 C29 -6.9(4) . . . . ? C6 B2 Zr2 C28 25.7(4) . . . . ? C6 B2 Zr2 C25 148.2(5) . . . . ? Zr1 B1 C1 C5 -47.4(5) . . . . ? Zr1 B1 C1 C2 135.3(3) . . . . ? Zr1 B1 C1 Fe1 -136.9(2) . . . . ? C10 Fe1 C1 C5 -42.1(14) . . . . ? C3 Fe1 C1 C5 80.6(3) . . . . ? C2 Fe1 C1 C5 117.4(3) . . . . ? C4 Fe1 C1 C5 37.2(2) . . . . ? C7 Fe1 C1 C5 -104.9(2) . . . . ? C8 Fe1 C1 C5 -148.2(2) . . . . ? C6 Fe1 C1 C5 -65.3(3) . . . . ? C9 Fe1 C1 C5 177.1(3) . . . . ? C10 Fe1 C1 C2 -159.5(13) . . . . ? C3 Fe1 C1 C2 -36.8(3) . . . . ? C5 Fe1 C1 C2 -117.4(3) . . . . ? C4 Fe1 C1 C2 -80.2(3) . . . . ? C7 Fe1 C1 C2 137.7(2) . . . . ? C8 Fe1 C1 C2 94.4(3) . . . . ? C6 Fe1 C1 C2 177.3(2) . . . . ? C9 Fe1 C1 C2 59.7(4) . . . . ? C10 Fe1 C1 B1 80.8(14) . . . . ? C3 Fe1 C1 B1 -156.6(3) . . . . ? C5 Fe1 C1 B1 122.8(4) . . . . ? C2 Fe1 C1 B1 -119.7(4) . . . . ? C4 Fe1 C1 B1 160.0(3) . . . . ? C7 Fe1 C1 B1 18.0(3) . . . . ? C8 Fe1 C1 B1 -25.3(3) . . . . ? C6 Fe1 C1 B1 57.5(4) . . . . ? C9 Fe1 C1 B1 -60.1(4) . . . . ? C5 C1 C2 C3 0.2(4) . . . . ? B1 C1 C2 C3 178.1(4) . . . . ? Fe1 C1 C2 C3 59.0(3) . . . . ? C5 C1 C2 Fe1 -58.8(2) . . . . ? B1 C1 C2 Fe1 119.0(4) . . . . ? C10 Fe1 C2 C3 55.4(4) . . . . ? C5 Fe1 C2 C3 -81.7(3) . . . . ? C4 Fe1 C2 C3 -37.4(3) . . . . ? C7 Fe1 C2 C3 176.0(2) . . . . ? C8 Fe1 C2 C3 136.4(3) . . . . ? C6 Fe1 C2 C3 -137.9(13) . . . . ? C9 Fe1 C2 C3 93.0(3) . . . . ? C1 Fe1 C2 C3 -120.4(3) . . . . ? C10 Fe1 C2 C1 175.9(3) . . . . ? C3 Fe1 C2 C1 120.4(3) . . . . ? C5 Fe1 C2 C1 38.8(2) . . . . ? C4 Fe1 C2 C1 83.0(2) . . . . ? C7 Fe1 C2 C1 -63.5(3) . . . . ? C8 Fe1 C2 C1 -103.2(2) . . . . ? C6 Fe1 C2 C1 -17.5(15) . . . . ? C9 Fe1 C2 C1 -146.6(2) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? Fe1 C2 C3 C4 59.8(3) . . . . ? C1 C2 C3 Fe1 -59.6(3) . . . . ? C10 Fe1 C3 C2 -149.0(2) . . . . ? C5 Fe1 C3 C2 81.3(3) . . . . ? C4 Fe1 C3 C2 119.5(3) . . . . ? C7 Fe1 C3 C2 -30.2(17) . . . . ? C8 Fe1 C3 C2 -66.0(3) . . . . ? C6 Fe1 C3 C2 172.4(2) . . . . ? C9 Fe1 C3 C2 -104.9(3) . . . . ? C1 Fe1 C3 C2 37.3(2) . . . . ? C10 Fe1 C3 C4 91.5(3) . . . . ? C5 Fe1 C3 C4 -38.2(2) . . . . ? C2 Fe1 C3 C4 -119.5(3) . . . . ? C7 Fe1 C3 C4 -149.7(16) . . . . ? C8 Fe1 C3 C4 174.5(2) . . . . ? C6 Fe1 C3 C4 52.9(4) . . . . ? C9 Fe1 C3 C4 135.6(2) . . . . ? C1 Fe1 C3 C4 -82.2(2) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? Fe1 C3 C4 C5 59.1(3) . . . . ? C2 C3 C4 Fe1 -59.6(3) . . . . ? C10 Fe1 C4 C3 -105.5(2) . . . . ? C5 Fe1 C4 C3 118.8(3) . . . . ? C2 Fe1 C4 C3 37.5(2) . . . . ? C7 Fe1 C4 C3 175.1(3) . . . . ? C8 Fe1 C4 C3 -41.4(16) . . . . ? C6 Fe1 C4 C3 -149.6(2) . . . . ? C9 Fe1 C4 C3 -66.9(3) . . . . ? C1 Fe1 C4 C3 81.6(2) . . . . ? C10 Fe1 C4 C5 135.8(2) . . . . ? C3 Fe1 C4 C5 -118.8(3) . . . . ? C2 Fe1 C4 C5 -81.3(2) . . . . ? C7 Fe1 C4 C5 56.4(4) . . . . ? C8 Fe1 C4 C5 -160.2(15) . . . . ? C6 Fe1 C4 C5 91.6(2) . . . . ? C9 Fe1 C4 C5 174.3(2) . . . . ? C1 Fe1 C4 C5 -37.2(2) . . . . ? C3 C4 C5 C1 0.7(5) . . . . ? Fe1 C4 C5 C1 59.9(3) . . . . ? C3 C4 C5 Fe1 -59.2(3) . . . . ? C2 C1 C5 C4 -0.6(4) . . . . ? B1 C1 C5 C4 -178.3(4) . . . . ? Fe1 C1 C5 C4 -59.4(3) . . . . ? C2 C1 C5 Fe1 58.8(2) . . . . ? B1 C1 C5 Fe1 -118.9(4) . . . . ? C10 Fe1 C5 C4 -66.0(3) . . . . ? C3 Fe1 C5 C4 37.7(2) . . . . ? C2 Fe1 C5 C4 81.5(3) . . . . ? C7 Fe1 C5 C4 -148.0(2) . . . . ? C8 Fe1 C5 C4 176.6(3) . . . . ? C6 Fe1 C5 C4 -104.3(2) . . . . ? C9 Fe1 C5 C4 -43.3(16) . . . . ? C1 Fe1 C5 C4 120.3(3) . . . . ? C10 Fe1 C5 C1 173.7(2) . . . . ? C3 Fe1 C5 C1 -82.5(2) . . . . ? C2 Fe1 C5 C1 -38.8(2) . . . . ? C4 Fe1 C5 C1 -120.3(3) . . . . ? C7 Fe1 C5 C1 91.8(2) . . . . ? C8 Fe1 C5 C1 56.3(3) . . . . ? C6 Fe1 C5 C1 135.4(2) . . . . ? C9 Fe1 C5 C1 -163.6(15) . . . . ? Zr2 B2 C6 C7 -20.4(7) . . . . ? Zr2 B2 C6 C10 165.6(3) . . . . ? Zr2 B2 C6 Fe1 -110.1(4) . . . . ? C10 Fe1 C6 C7 117.1(3) . . . . ? C3 Fe1 C6 C7 176.7(3) . . . . ? C5 Fe1 C6 C7 -105.7(2) . . . . ? C2 Fe1 C6 C7 -51.4(15) . . . . ? C4 Fe1 C6 C7 -149.1(2) . . . . ? C8 Fe1 C6 C7 36.8(2) . . . . ? C9 Fe1 C6 C7 79.9(2) . . . . ? C1 Fe1 C6 C7 -66.9(3) . . . . ? C3 Fe1 C6 C10 59.6(3) . . . . ? C5 Fe1 C6 C10 137.2(2) . . . . ? C2 Fe1 C6 C10 -168.5(13) . . . . ? C4 Fe1 C6 C10 93.8(2) . . . . ? C7 Fe1 C6 C10 -117.1(3) . . . . ? C8 Fe1 C6 C10 -80.3(2) . . . . ? C9 Fe1 C6 C10 -37.2(2) . . . . ? C1 Fe1 C6 C10 176.0(2) . . . . ? C10 Fe1 C6 B2 -117.0(4) . . . . ? C3 Fe1 C6 B2 -57.3(4) . . . . ? C5 Fe1 C6 B2 20.3(3) . . . . ? C2 Fe1 C6 B2 74.5(15) . . . . ? C4 Fe1 C6 B2 -23.2(3) . . . . ? C7 Fe1 C6 B2 125.9(4) . . . . ? C8 Fe1 C6 B2 162.8(3) . . . . ? C9 Fe1 C6 B2 -154.2(3) . . . . ? C1 Fe1 C6 B2 59.0(4) . . . . ? C10 C6 C7 C8 0.4(4) . . . . ? B2 C6 C7 C8 -174.4(4) . . . . ? Fe1 C6 C7 C8 -58.9(3) . . . . ? C10 C6 C7 Fe1 59.3(2) . . . . ? B2 C6 C7 Fe1 -115.5(4) . . . . ? C10 Fe1 C7 C8 81.4(2) . . . . ? C3 Fe1 C7 C8 -39.5(17) . . . . ? C5 Fe1 C7 C8 -148.8(2) . . . . ? C2 Fe1 C7 C8 -66.8(3) . . . . ? C4 Fe1 C7 C8 174.6(3) . . . . ? C6 Fe1 C7 C8 120.5(3) . . . . ? C9 Fe1 C7 C8 37.3(2) . . . . ? C1 Fe1 C7 C8 -105.1(2) . . . . ? C10 Fe1 C7 C6 -39.1(2) . . . . ? C3 Fe1 C7 C6 -160.0(16) . . . . ? C5 Fe1 C7 C6 90.7(2) . . . . ? C2 Fe1 C7 C6 172.7(2) . . . . ? C4 Fe1 C7 C6 54.1(3) . . . . ? C8 Fe1 C7 C6 -120.5(3) . . . . ? C9 Fe1 C7 C6 -83.2(2) . . . . ? C1 Fe1 C7 C6 134.4(2) . . . . ? C6 C7 C8 C9 -1.0(4) . . . . ? Fe1 C7 C8 C9 -59.9(3) . . . . ? C6 C7 C8 Fe1 58.9(3) . . . . ? C10 Fe1 C8 C9 37.7(2) . . . . ? C3 Fe1 C8 C9 -65.8(3) . . . . ? C5 Fe1 C8 C9 174.1(2) . . . . ? C2 Fe1 C8 C9 -105.1(2) . . . . ? C4 Fe1 C8 C9 -28.4(16) . . . . ? C7 Fe1 C8 C9 119.3(3) . . . . ? C6 Fe1 C8 C9 82.1(2) . . . . ? C1 Fe1 C8 C9 -149.3(2) . . . . ? C10 Fe1 C8 C7 -81.6(2) . . . . ? C3 Fe1 C8 C7 174.9(2) . . . . ? C5 Fe1 C8 C7 54.8(3) . . . . ? C2 Fe1 C8 C7 135.7(2) . . . . ? C4 Fe1 C8 C7 -147.6(15) . . . . ? C6 Fe1 C8 C7 -37.2(2) . . . . ? C9 Fe1 C8 C7 -119.3(3) . . . . ? C1 Fe1 C8 C7 91.4(2) . . . . ? C7 C8 C9 C10 1.2(4) . . . . ? Fe1 C8 C9 C10 -58.4(3) . . . . ? C7 C8 C9 Fe1 59.5(3) . . . . ? C10 Fe1 C9 C8 -119.6(3) . . . . ? C3 Fe1 C9 C8 136.5(2) . . . . ? C5 Fe1 C9 C8 -144.7(15) . . . . ? C2 Fe1 C9 C8 92.6(2) . . . . ? C4 Fe1 C9 C8 176.1(2) . . . . ? C7 Fe1 C9 C8 -37.7(2) . . . . ? C6 Fe1 C9 C8 -81.9(2) . . . . ? C1 Fe1 C9 C8 53.9(3) . . . . ? C3 Fe1 C9 C10 -104.0(2) . . . . ? C5 Fe1 C9 C10 -25.2(17) . . . . ? C2 Fe1 C9 C10 -147.8(2) . . . . ? C4 Fe1 C9 C10 -64.4(3) . . . . ? C7 Fe1 C9 C10 81.8(2) . . . . ? C8 Fe1 C9 C10 119.6(3) . . . . ? C6 Fe1 C9 C10 37.7(2) . . . . ? C1 Fe1 C9 C10 173.5(2) . . . . ? C8 C9 C10 C6 -0.9(4) . . . . ? Fe1 C9 C10 C6 -59.8(3) . . . . ? C8 C9 C10 Fe1 58.9(3) . . . . ? C7 C6 C10 C9 0.3(4) . . . . ? B2 C6 C10 C9 175.6(3) . . . . ? Fe1 C6 C10 C9 60.0(3) . . . . ? C7 C6 C10 Fe1 -59.7(2) . . . . ? B2 C6 C10 Fe1 115.6(3) . . . . ? C3 Fe1 C10 C9 93.8(3) . . . . ? C5 Fe1 C10 C9 176.5(3) . . . . ? C2 Fe1 C10 C9 57.8(4) . . . . ? C4 Fe1 C10 C9 137.2(3) . . . . ? C7 Fe1 C10 C9 -80.9(2) . . . . ? C8 Fe1 C10 C9 -37.1(2) . . . . ? C6 Fe1 C10 C9 -119.9(3) . . . . ? C1 Fe1 C10 C9 -146.0(13) . . . . ? C3 Fe1 C10 C6 -146.3(2) . . . . ? C5 Fe1 C10 C6 -63.6(3) . . . . ? C2 Fe1 C10 C6 177.7(3) . . . . ? C4 Fe1 C10 C6 -102.9(2) . . . . ? C7 Fe1 C10 C6 38.9(2) . . . . ? C8 Fe1 C10 C6 82.7(2) . . . . ? C9 Fe1 C10 C6 119.9(3) . . . . ? C1 Fe1 C10 C6 -26.1(14) . . . . ? C18 Zr1 C11 C12 -102.8(3) . . . . ? C16 Zr1 C11 C12 -127.1(3) . . . . ? C15 Zr1 C11 C12 114.9(4) . . . . ? C17 Zr1 C11 C12 -94.9(3) . . . . ? C19 Zr1 C11 C12 -136.2(3) . . . . ? C20 Zr1 C11 C12 -151.1(3) . . . . ? Cl1 Zr1 C11 C12 -8.5(3) . . . . ? C13 Zr1 C11 C12 38.1(3) . . . . ? C14 Zr1 C11 C12 78.0(3) . . . . ? B1 Zr1 C11 C12 121.3(3) . . . . ? C12 Zr1 C11 C15 -114.9(4) . . . . ? C18 Zr1 C11 C15 142.3(3) . . . . ? C16 Zr1 C11 C15 118.1(3) . . . . ? C17 Zr1 C11 C15 150.3(2) . . . . ? C19 Zr1 C11 C15 108.9(3) . . . . ? C20 Zr1 C11 C15 94.0(3) . . . . ? Cl1 Zr1 C11 C15 -123.4(2) . . . . ? C13 Zr1 C11 C15 -76.7(3) . . . . ? C14 Zr1 C11 C15 -36.8(2) . . . . ? B1 Zr1 C11 C15 6.5(3) . . . . ? C15 C11 C12 C13 -2.6(5) . . . . ? Zr1 C11 C12 C13 -69.1(3) . . . . ? C15 C11 C12 Zr1 66.5(3) . . . . ? C18 Zr1 C12 C11 73.8(3) . . . . ? C16 Zr1 C12 C11 85.1(3) . . . . ? C15 Zr1 C12 C11 -37.1(3) . . . . ? C17 Zr1 C12 C11 98.1(3) . . . . ? C19 Zr1 C12 C11 43.1(3) . . . . ? C20 Zr1 C12 C11 39.0(3) . . . . ? Cl1 Zr1 C12 C11 172.5(3) . . . . ? C13 Zr1 C12 C11 -113.1(4) . . . . ? C14 Zr1 C12 C11 -77.2(3) . . . . ? B1 Zr1 C12 C11 -86.0(3) . . . . ? C18 Zr1 C12 C13 -173.1(3) . . . . ? C16 Zr1 C12 C13 -161.8(3) . . . . ? C11 Zr1 C12 C13 113.1(4) . . . . ? C15 Zr1 C12 C13 76.0(3) . . . . ? C17 Zr1 C12 C13 -148.9(2) . . . . ? C19 Zr1 C12 C13 156.2(2) . . . . ? C20 Zr1 C12 C13 152.0(2) . . . . ? Cl1 Zr1 C12 C13 -74.5(2) . . . . ? C14 Zr1 C12 C13 35.8(2) . . . . ? B1 Zr1 C12 C13 27.1(3) . . . . ? C11 C12 C13 C14 2.0(5) . . . . ? Zr1 C12 C13 C14 -66.3(3) . . . . ? C11 C12 C13 Zr1 68.3(3) . . . . ? C12 Zr1 C13 C14 116.3(4) . . . . ? C18 Zr1 C13 C14 124.3(3) . . . . ? C16 Zr1 C13 C14 -174.6(6) . . . . ? C11 Zr1 C13 C14 78.2(3) . . . . ? C15 Zr1 C13 C14 37.4(2) . . . . ? C17 Zr1 C13 C14 161.2(3) . . . . ? C19 Zr1 C13 C14 85.3(3) . . . . ? C20 Zr1 C13 C14 55.2(5) . . . . ? Cl1 Zr1 C13 C14 -142.9(3) . . . . ? B1 Zr1 C13 C14 -44.4(3) . . . . ? C18 Zr1 C13 C12 8.0(3) . . . . ? C16 Zr1 C13 C12 69.2(8) . . . . ? C11 Zr1 C13 C12 -38.1(2) . . . . ? C15 Zr1 C13 C12 -78.9(3) . . . . ? C17 Zr1 C13 C12 44.9(3) . . . . ? C19 Zr1 C13 C12 -31.0(3) . . . . ? C20 Zr1 C13 C12 -61.1(5) . . . . ? Cl1 Zr1 C13 C12 100.8(2) . . . . ? C14 Zr1 C13 C12 -116.3(4) . . . . ? B1 Zr1 C13 C12 -160.7(2) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? Zr1 C13 C14 C15 -65.0(3) . . . . ? C12 C13 C14 Zr1 64.3(3) . . . . ? C12 Zr1 C14 C13 -36.7(3) . . . . ? C18 Zr1 C14 C13 -78.5(3) . . . . ? C16 Zr1 C14 C13 176.7(4) . . . . ? C11 Zr1 C14 C13 -77.4(3) . . . . ? C15 Zr1 C14 C13 -114.5(4) . . . . ? C17 Zr1 C14 C13 -52.8(6) . . . . ? C19 Zr1 C14 C13 -116.7(3) . . . . ? C20 Zr1 C14 C13 -154.2(3) . . . . ? Cl1 Zr1 C14 C13 37.3(3) . . . . ? B1 Zr1 C14 C13 137.1(3) . . . . ? C12 Zr1 C14 C15 77.8(3) . . . . ? C18 Zr1 C14 C15 36.0(3) . . . . ? C16 Zr1 C14 C15 -68.8(5) . . . . ? C11 Zr1 C14 C15 37.1(2) . . . . ? C17 Zr1 C14 C15 61.7(6) . . . . ? C19 Zr1 C14 C15 -2.2(3) . . . . ? C20 Zr1 C14 C15 -39.7(3) . . . . ? Cl1 Zr1 C14 C15 151.9(2) . . . . ? C13 Zr1 C14 C15 114.5(4) . . . . ? B1 Zr1 C14 C15 -108.4(3) . . . . ? C12 C11 C15 C14 2.2(5) . . . . ? Zr1 C11 C15 C14 67.9(3) . . . . ? C12 C11 C15 Zr1 -65.7(3) . . . . ? C13 C14 C15 C11 -0.9(4) . . . . ? Zr1 C14 C15 C11 -66.5(3) . . . . ? C13 C14 C15 Zr1 65.6(3) . . . . ? C12 Zr1 C15 C11 37.2(3) . . . . ? C18 Zr1 C15 C11 -38.7(3) . . . . ? C16 Zr1 C15 C11 -92.7(3) . . . . ? C17 Zr1 C15 C11 -43.6(3) . . . . ? C19 Zr1 C15 C11 -66.8(3) . . . . ? C20 Zr1 C15 C11 -94.7(3) . . . . ? Cl1 Zr1 C15 C11 77.7(3) . . . . ? C13 Zr1 C15 C11 78.1(3) . . . . ? C14 Zr1 C15 C11 115.0(3) . . . . ? B1 Zr1 C15 C11 -174.7(3) . . . . ? C12 Zr1 C15 C14 -77.8(3) . . . . ? C18 Zr1 C15 C14 -153.7(2) . . . . ? C16 Zr1 C15 C14 152.3(2) . . . . ? C11 Zr1 C15 C14 -115.0(3) . . . . ? C17 Zr1 C15 C14 -158.6(3) . . . . ? C19 Zr1 C15 C14 178.1(3) . . . . ? C20 Zr1 C15 C14 150.3(2) . . . . ? Cl1 Zr1 C15 C14 -37.3(3) . . . . ? C13 Zr1 C15 C14 -36.9(2) . . . . ? B1 Zr1 C15 C14 70.2(2) . . . . ? C12 Zr1 C16 C20 -91.2(3) . . . . ? C18 Zr1 C16 C20 -77.3(3) . . . . ? C11 Zr1 C16 C20 -47.4(3) . . . . ? C15 Zr1 C16 C20 -3.6(4) . . . . ? C17 Zr1 C16 C20 -114.1(4) . . . . ? C19 Zr1 C16 C20 -36.4(2) . . . . ? Cl1 Zr1 C16 C20 -176.4(2) . . . . ? C13 Zr1 C16 C20 -145.5(7) . . . . ? C14 Zr1 C16 C20 42.9(5) . . . . ? B1 Zr1 C16 C20 82.5(3) . . . . ? C12 Zr1 C16 C17 22.9(4) . . . . ? C18 Zr1 C16 C17 36.8(3) . . . . ? C11 Zr1 C16 C17 66.7(3) . . . . ? C15 Zr1 C16 C17 110.4(3) . . . . ? C19 Zr1 C16 C17 77.7(3) . . . . ? C20 Zr1 C16 C17 114.1(4) . . . . ? Cl1 Zr1 C16 C17 -62.3(3) . . . . ? C13 Zr1 C16 C17 -31.4(9) . . . . ? C14 Zr1 C16 C17 157.0(4) . . . . ? B1 Zr1 C16 C17 -163.4(3) . . . . ? C20 C16 C17 C18 2.4(5) . . . . ? Zr1 C16 C17 C18 -65.1(3) . . . . ? C20 C16 C17 Zr1 67.5(3) . . . . ? C12 Zr1 C17 C18 -49.5(3) . . . . ? C16 Zr1 C17 C18 115.6(4) . . . . ? C11 Zr1 C17 C18 -14.6(3) . . . . ? C15 Zr1 C17 C18 8.8(4) . . . . ? C19 Zr1 C17 C18 38.1(2) . . . . ? C20 Zr1 C17 C18 78.2(3) . . . . ? Cl1 Zr1 C17 C18 -129.7(3) . . . . ? C13 Zr1 C17 C18 -73.5(3) . . . . ? C14 Zr1 C17 C18 -35.7(6) . . . . ? B1 Zr1 C17 C18 133.6(2) . . . . ? C12 Zr1 C17 C16 -165.1(3) . . . . ? C18 Zr1 C17 C16 -115.6(4) . . . . ? C11 Zr1 C17 C16 -130.2(3) . . . . ? C15 Zr1 C17 C16 -106.8(3) . . . . ? C19 Zr1 C17 C16 -77.5(3) . . . . ? C20 Zr1 C17 C16 -37.4(3) . . . . ? Cl1 Zr1 C17 C16 114.7(3) . . . . ? C13 Zr1 C17 C16 170.9(3) . . . . ? C14 Zr1 C17 C16 -151.3(5) . . . . ? B1 Zr1 C17 C16 18.0(3) . . . . ? C16 C17 C18 C19 -2.5(5) . . . . ? Zr1 C17 C18 C19 -67.7(3) . . . . ? C16 C17 C18 Zr1 65.3(3) . . . . ? C12 Zr1 C18 C17 134.6(3) . . . . ? C16 Zr1 C18 C17 -36.8(3) . . . . ? C11 Zr1 C18 C17 166.2(3) . . . . ? C15 Zr1 C18 C17 -173.9(2) . . . . ? C19 Zr1 C18 C17 -113.4(4) . . . . ? C20 Zr1 C18 C17 -77.1(3) . . . . ? Cl1 Zr1 C18 C17 49.3(2) . . . . ? C13 Zr1 C18 C17 130.3(3) . . . . ? C14 Zr1 C18 C17 167.1(2) . . . . ? B1 Zr1 C18 C17 -64.6(3) . . . . ? C12 Zr1 C18 C19 -112.0(3) . . . . ? C16 Zr1 C18 C19 76.6(3) . . . . ? C11 Zr1 C18 C19 -80.3(3) . . . . ? C15 Zr1 C18 C19 -60.5(3) . . . . ? C17 Zr1 C18 C19 113.4(4) . . . . ? C20 Zr1 C18 C19 36.4(2) . . . . ? Cl1 Zr1 C18 C19 162.8(2) . . . . ? C13 Zr1 C18 C19 -116.3(3) . . . . ? C14 Zr1 C18 C19 -79.4(3) . . . . ? B1 Zr1 C18 C19 48.8(3) . . . . ? C17 C18 C19 C20 1.7(5) . . . . ? Zr1 C18 C19 C20 -66.1(3) . . . . ? C17 C18 C19 Zr1 67.8(3) . . . . ? C12 Zr1 C19 C20 -174.2(3) . . . . ? C18 Zr1 C19 C20 115.4(4) . . . . ? C16 Zr1 C19 C20 36.8(3) . . . . ? C11 Zr1 C19 C20 -152.0(3) . . . . ? C15 Zr1 C19 C20 -121.6(3) . . . . ? C17 Zr1 C19 C20 77.6(3) . . . . ? Cl1 Zr1 C19 C20 93.1(3) . . . . ? C13 Zr1 C19 C20 -157.9(3) . . . . ? C14 Zr1 C19 C20 -120.4(3) . . . . ? B1 Zr1 C19 C20 -29.1(3) . . . . ? C12 Zr1 C19 C18 70.4(3) . . . . ? C16 Zr1 C19 C18 -78.6(3) . . . . ? C11 Zr1 C19 C18 92.6(3) . . . . ? C15 Zr1 C19 C18 123.0(3) . . . . ? C17 Zr1 C19 C18 -37.8(3) . . . . ? C20 Zr1 C19 C18 -115.4(4) . . . . ? Cl1 Zr1 C19 C18 -22.3(3) . . . . ? C13 Zr1 C19 C18 86.7(3) . . . . ? C14 Zr1 C19 C18 124.2(3) . . . . ? B1 Zr1 C19 C18 -144.5(3) . . . . ? C18 C19 C20 C16 -0.2(5) . . . . ? Zr1 C19 C20 C16 -65.4(3) . . . . ? C18 C19 C20 Zr1 65.2(3) . . . . ? C17 C16 C20 C19 -1.3(5) . . . . ? Zr1 C16 C20 C19 65.9(3) . . . . ? C17 C16 C20 Zr1 -67.3(3) . . . . ? C12 Zr1 C20 C19 7.7(3) . . . . ? C18 Zr1 C20 C19 -37.3(3) . . . . ? C16 Zr1 C20 C19 -115.8(4) . . . . ? C11 Zr1 C20 C19 28.1(3) . . . . ? C15 Zr1 C20 C19 61.6(3) . . . . ? C17 Zr1 C20 C19 -78.1(3) . . . . ? Cl1 Zr1 C20 C19 -111.4(2) . . . . ? C13 Zr1 C20 C19 47.1(5) . . . . ? C14 Zr1 C20 C19 82.2(3) . . . . ? B1 Zr1 C20 C19 152.0(3) . . . . ? C12 Zr1 C20 C16 123.5(3) . . . . ? C18 Zr1 C20 C16 78.5(3) . . . . ? C11 Zr1 C20 C16 143.9(3) . . . . ? C15 Zr1 C20 C16 177.4(3) . . . . ? C17 Zr1 C20 C16 37.7(3) . . . . ? C19 Zr1 C20 C16 115.8(4) . . . . ? Cl1 Zr1 C20 C16 4.4(3) . . . . ? C13 Zr1 C20 C16 162.9(4) . . . . ? C14 Zr1 C20 C16 -162.0(2) . . . . ? B1 Zr1 C20 C16 -92.2(3) . . . . ? C26 Zr2 C21 C25 -170.2(4) . . . . ? C27 Zr2 C21 C25 162.0(4) . . . . ? C23 Zr2 C21 C25 -77.1(4) . . . . ? C22 Zr2 C21 C25 -114.1(6) . . . . ? C24 Zr2 C21 C25 -35.9(3) . . . . ? Cl2 Zr2 C21 C25 -64.9(5) . . . . ? C30 Zr2 C21 C25 -175.8(4) . . . . ? C29 Zr2 C21 C25 140.1(4) . . . . ? C28 Zr2 C21 C25 134.9(4) . . . . ? B2 Zr2 C21 C25 47.8(4) . . . . ? C26 Zr2 C21 C22 -56.1(4) . . . . ? C27 Zr2 C21 C22 -84.0(4) . . . . ? C23 Zr2 C21 C22 36.9(3) . . . . ? C24 Zr2 C21 C22 78.2(4) . . . . ? Cl2 Zr2 C21 C22 49.2(5) . . . . ? C30 Zr2 C21 C22 -61.7(4) . . . . ? C29 Zr2 C21 C22 -105.8(4) . . . . ? C28 Zr2 C21 C22 -111.0(4) . . . . ? C25 Zr2 C21 C22 114.1(6) . . . . ? B2 Zr2 C21 C22 161.8(4) . . . . ? C25 C21 C22 C23 2.2(6) . . . . ? Zr2 C21 C22 C23 -66.5(4) . . . . ? C25 C21 C22 Zr2 68.7(3) . . . . ? C26 Zr2 C22 C23 -121.6(4) . . . . ? C21 Zr2 C22 C23 114.5(5) . . . . ? C27 Zr2 C22 C23 -154.9(4) . . . . ? C24 Zr2 C22 C23 37.8(4) . . . . ? Cl2 Zr2 C22 C23 -29.5(4) . . . . ? C30 Zr2 C22 C23 -110.5(3) . . . . ? C29 Zr2 C22 C23 -140.6(3) . . . . ? C28 Zr2 C22 C23 -168.2(3) . . . . ? C25 Zr2 C22 C23 77.5(4) . . . . ? B2 Zr2 C22 C23 90.1(4) . . . . ? C26 Zr2 C22 C21 124.0(4) . . . . ? C27 Zr2 C22 C21 90.6(4) . . . . ? C23 Zr2 C22 C21 -114.5(5) . . . . ? C24 Zr2 C22 C21 -76.6(4) . . . . ? Cl2 Zr2 C22 C21 -144.0(4) . . . . ? C30 Zr2 C22 C21 135.0(4) . . . . ? C29 Zr2 C22 C21 105.0(4) . . . . ? C28 Zr2 C22 C21 77.4(4) . . . . ? C25 Zr2 C22 C21 -37.0(4) . . . . ? B2 Zr2 C22 C21 -24.4(5) . . . . ? C21 C22 C23 C24 -0.9(6) . . . . ? Zr2 C22 C23 C24 -67.0(3) . . . . ? C21 C22 C23 Zr2 66.0(3) . . . . ? C26 Zr2 C23 C22 58.2(4) . . . . ? C21 Zr2 C23 C22 -37.7(4) . . . . ? C27 Zr2 C23 C22 26.1(4) . . . . ? C24 Zr2 C23 C22 -114.5(6) . . . . ? Cl2 Zr2 C23 C22 151.5(4) . . . . ? C30 Zr2 C23 C22 84.7(4) . . . . ? C29 Zr2 C23 C22 74.8(5) . . . . ? C28 Zr2 C23 C22 17.7(5) . . . . ? C25 Zr2 C23 C22 -77.8(4) . . . . ? B2 Zr2 C23 C22 -115.7(3) . . . . ? C26 Zr2 C23 C24 172.6(4) . . . . ? C21 Zr2 C23 C24 76.7(5) . . . . ? C27 Zr2 C23 C24 140.6(4) . . . . ? C22 Zr2 C23 C24 114.5(6) . . . . ? Cl2 Zr2 C23 C24 -94.1(4) . . . . ? C30 Zr2 C23 C24 -160.8(4) . . . . ? C29 Zr2 C23 C24 -170.7(4) . . . . ? C28 Zr2 C23 C24 132.2(4) . . . . ? C25 Zr2 C23 C24 36.7(4) . . . . ? B2 Zr2 C23 C24 -1.3(5) . . . . ? C22 C23 C24 C25 -0.7(6) . . . . ? Zr2 C23 C24 C25 -67.6(4) . . . . ? C22 C23 C24 Zr2 66.9(3) . . . . ? C26 Zr2 C24 C25 104.5(4) . . . . ? C21 Zr2 C24 C25 36.2(3) . . . . ? C27 Zr2 C24 C25 60.2(4) . . . . ? C23 Zr2 C24 C25 114.1(6) . . . . ? C22 Zr2 C24 C25 77.2(4) . . . . ? Cl2 Zr2 C24 C25 -165.0(3) . . . . ? C30 Zr2 C24 C25 147.8(4) . . . . ? C29 Zr2 C24 C25 -114.3(19) . . . . ? C28 Zr2 C24 C25 16.7(5) . . . . ? B2 Zr2 C24 C25 -66.9(3) . . . . ? C26 Zr2 C24 C23 -9.6(6) . . . . ? C21 Zr2 C24 C23 -77.9(4) . . . . ? C27 Zr2 C24 C23 -53.9(5) . . . . ? C22 Zr2 C24 C23 -36.9(4) . . . . ? Cl2 Zr2 C24 C23 80.9(4) . . . . ? C30 Zr2 C24 C23 33.7(6) . . . . ? C29 Zr2 C24 C23 131.6(17) . . . . ? C28 Zr2 C24 C23 -97.4(5) . . . . ? C25 Zr2 C24 C23 -114.1(6) . . . . ? B2 Zr2 C24 C23 179.0(4) . . . . ? C23 C24 C25 C21 2.1(6) . . . . ? Zr2 C24 C25 C21 -64.2(4) . . . . ? C23 C24 C25 Zr2 66.3(4) . . . . ? C22 C21 C25 C24 -2.7(6) . . . . ? Zr2 C21 C25 C24 64.9(4) . . . . ? C22 C21 C25 Zr2 -67.6(3) . . . . ? C26 Zr2 C25 C24 -103.7(4) . . . . ? C21 Zr2 C25 C24 -116.6(5) . . . . ? C27 Zr2 C25 C24 -135.9(3) . . . . ? C23 Zr2 C25 C24 -38.2(3) . . . . ? C22 Zr2 C25 C24 -78.6(4) . . . . ? Cl2 Zr2 C25 C24 16.3(4) . . . . ? C30 Zr2 C25 C24 -105.5(8) . . . . ? C29 Zr2 C25 C24 168.8(3) . . . . ? C28 Zr2 C25 C24 -170.9(3) . . . . ? B2 Zr2 C25 C24 110.9(4) . . . . ? C26 Zr2 C25 C21 12.8(5) . . . . ? C27 Zr2 C25 C21 -19.3(4) . . . . ? C23 Zr2 C25 C21 78.3(4) . . . . ? C22 Zr2 C25 C21 38.0(4) . . . . ? C24 Zr2 C25 C21 116.6(5) . . . . ? Cl2 Zr2 C25 C21 132.8(4) . . . . ? C30 Zr2 C25 C21 11.1(10) . . . . ? C29 Zr2 C25 C21 -74.6(5) . . . . ? C28 Zr2 C25 C21 -54.3(4) . . . . ? B2 Zr2 C25 C21 -132.5(4) . . . . ? C21 Zr2 C26 C30 -172.2(3) . . . . ? C27 Zr2 C26 C30 -113.9(4) . . . . ? C23 Zr2 C26 C30 133.6(3) . . . . ? C22 Zr2 C26 C30 160.7(3) . . . . ? C24 Zr2 C26 C30 138.8(3) . . . . ? Cl2 Zr2 C26 C30 53.6(3) . . . . ? C29 Zr2 C26 C30 -36.5(3) . . . . ? C28 Zr2 C26 C30 -77.0(3) . . . . ? C25 Zr2 C26 C30 -179.1(3) . . . . ? B2 Zr2 C26 C30 -53.8(4) . . . . ? C21 Zr2 C26 C27 -58.3(3) . . . . ? C23 Zr2 C26 C27 -112.6(3) . . . . ? C22 Zr2 C26 C27 -85.4(3) . . . . ? C24 Zr2 C26 C27 -107.3(3) . . . . ? Cl2 Zr2 C26 C27 167.5(2) . . . . ? C30 Zr2 C26 C27 113.9(4) . . . . ? C29 Zr2 C26 C27 77.4(3) . . . . ? C28 Zr2 C26 C27 36.9(2) . . . . ? C25 Zr2 C26 C27 -65.2(3) . . . . ? B2 Zr2 C26 C27 60.1(3) . . . . ? C30 C26 C27 C28 1.3(5) . . . . ? Zr2 C26 C27 C28 -67.3(3) . . . . ? C30 C26 C27 Zr2 68.5(3) . . . . ? C26 Zr2 C27 C28 114.9(4) . . . . ? C21 Zr2 C27 C28 -123.2(3) . . . . ? C23 Zr2 C27 C28 -170.0(3) . . . . ? C22 Zr2 C27 C28 -156.3(3) . . . . ? C24 Zr2 C27 C28 -142.4(3) . . . . ? Cl2 Zr2 C27 C28 99.2(3) . . . . ? C30 Zr2 C27 C28 77.3(3) . . . . ? C29 Zr2 C27 C28 36.9(2) . . . . ? C25 Zr2 C27 C28 -113.0(3) . . . . ? B2 Zr2 C27 C28 -24.1(3) . . . . ? C21 Zr2 C27 C26 122.0(3) . . . . ? C23 Zr2 C27 C26 75.1(3) . . . . ? C22 Zr2 C27 C26 88.9(3) . . . . ? C24 Zr2 C27 C26 102.7(3) . . . . ? Cl2 Zr2 C27 C26 -15.7(3) . . . . ? C30 Zr2 C27 C26 -37.6(2) . . . . ? C29 Zr2 C27 C26 -78.0(3) . . . . ? C28 Zr2 C27 C26 -114.9(4) . . . . ? C25 Zr2 C27 C26 132.1(3) . . . . ? B2 Zr2 C27 C26 -139.0(2) . . . . ? C26 C27 C28 C29 0.3(5) . . . . ? Zr2 C27 C28 C29 -65.6(3) . . . . ? C26 C27 C28 Zr2 65.8(3) . . . . ? C26 Zr2 C28 C27 -37.5(3) . . . . ? C21 Zr2 C28 C27 57.2(3) . . . . ? C23 Zr2 C28 C27 15.0(4) . . . . ? C22 Zr2 C28 C27 24.8(3) . . . . ? C24 Zr2 C28 C27 72.9(4) . . . . ? Cl2 Zr2 C28 C27 -105.0(3) . . . . ? C30 Zr2 C28 C27 -78.2(3) . . . . ? C29 Zr2 C28 C27 -115.6(4) . . . . ? C25 Zr2 C28 C27 83.0(3) . . . . ? B2 Zr2 C28 C27 158.2(3) . . . . ? C26 Zr2 C28 C29 78.1(3) . . . . ? C21 Zr2 C28 C29 172.8(3) . . . . ? C27 Zr2 C28 C29 115.6(4) . . . . ? C23 Zr2 C28 C29 130.5(3) . . . . ? C22 Zr2 C28 C29 140.4(2) . . . . ? C24 Zr2 C28 C29 -171.5(3) . . . . ? Cl2 Zr2 C28 C29 10.6(2) . . . . ? C30 Zr2 C28 C29 37.4(2) . . . . ? C25 Zr2 C28 C29 -161.4(2) . . . . ? B2 Zr2 C28 C29 -86.2(2) . . . . ? C27 C28 C29 C30 -1.7(5) . . . . ? Zr2 C28 C29 C30 -66.6(3) . . . . ? C27 C28 C29 Zr2 64.9(3) . . . . ? C26 Zr2 C29 C30 36.7(3) . . . . ? C21 Zr2 C29 C30 104.7(4) . . . . ? C27 Zr2 C29 C30 77.6(3) . . . . ? C23 Zr2 C29 C30 16.2(5) . . . . ? C22 Zr2 C29 C30 60.0(4) . . . . ? C24 Zr2 C29 C30 -107.4(19) . . . . ? Cl2 Zr2 C29 C30 -57.1(3) . . . . ? C28 Zr2 C29 C30 114.3(4) . . . . ? C25 Zr2 C29 C30 147.9(4) . . . . ? B2 Zr2 C29 C30 -155.1(3) . . . . ? C26 Zr2 C29 C28 -77.6(3) . . . . ? C21 Zr2 C29 C28 -9.6(3) . . . . ? C27 Zr2 C29 C28 -36.6(2) . . . . ? C23 Zr2 C29 C28 -98.0(4) . . . . ? C22 Zr2 C29 C28 -54.2(3) . . . . ? C24 Zr2 C29 C28 138.3(19) . . . . ? Cl2 Zr2 C29 C28 -171.3(2) . . . . ? C30 Zr2 C29 C28 -114.3(4) . . . . ? C25 Zr2 C29 C28 33.7(4) . . . . ? B2 Zr2 C29 C28 90.6(2) . . . . ? C27 C26 C30 C29 -2.3(5) . . . . ? Zr2 C26 C30 C29 65.4(3) . . . . ? C27 C26 C30 Zr2 -67.7(3) . . . . ? C28 C29 C30 C26 2.5(5) . . . . ? Zr2 C29 C30 C26 -64.2(3) . . . . ? C28 C29 C30 Zr2 66.7(3) . . . . ? C21 Zr2 C30 C26 10.3(4) . . . . ? C27 Zr2 C30 C26 37.9(3) . . . . ? C23 Zr2 C30 C26 -55.2(3) . . . . ? C22 Zr2 C30 C26 -20.5(3) . . . . ? C24 Zr2 C30 C26 -75.3(5) . . . . ? Cl2 Zr2 C30 C26 -124.1(3) . . . . ? C29 Zr2 C30 C26 115.9(4) . . . . ? C28 Zr2 C30 C26 78.3(3) . . . . ? C25 Zr2 C30 C26 2.5(8) . . . . ? B2 Zr2 C30 C26 143.0(3) . . . . ? C26 Zr2 C30 C29 -115.9(4) . . . . ? C21 Zr2 C30 C29 -105.6(3) . . . . ? C27 Zr2 C30 C29 -77.9(3) . . . . ? C23 Zr2 C30 C29 -171.0(3) . . . . ? C22 Zr2 C30 C29 -136.4(3) . . . . ? C24 Zr2 C30 C29 168.8(3) . . . . ? Cl2 Zr2 C30 C29 120.0(3) . . . . ? C28 Zr2 C30 C29 -37.5(2) . . . . ? C25 Zr2 C30 C29 -113.4(7) . . . . ? B2 Zr2 C30 C29 27.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.484 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.090