data_[Cp2Zr(C5H4)FeCp][MeB(C6F5)3] _audit_creation_method SHELXL-97 _chemical_formula_sum 'C39 H22 B F15 Fe Zr' _chemical_formula_weight 933.45 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)2(1)2(1) 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' _cell_length_a 13.1770(11) _cell_length_b 15.8640(14) _cell_length_c 16.2706(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3401.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_T_max 0.7475 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 73813 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 38.07 _reflns_number_total 18081 _reflns_number_gt 15672 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.3329P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(7) _refine_ls_number_reflns 18081 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Zr1 Zr 0.176084(8) 0.396666(7) 0.504691(7) 0.01943(2) Uani 1 1 d . . . Fe1 Fe 0.158830(13) 0.219215(11) 0.466720(11) 0.02117(4) Uani 1 1 d . . . C17 C 0.02904(10) 0.22243(10) 0.53757(9) 0.0291(3) Uani 1 1 d . . . H17A H 0.0259 0.2299 0.5973 0.035 Uiso 1 1 calc R . . C11 C 0.28665(10) 0.28709(10) 0.48557(9) 0.0279(3) Uani 1 1 d . . . C15 C 0.29067(10) 0.24770(10) 0.40475(10) 0.0300(3) Uani 1 1 d . . . H15A H 0.2945 0.2779 0.3523 0.036 Uiso 1 1 calc R . . C12 C 0.28277(10) 0.21711(10) 0.54334(10) 0.0319(3) Uani 1 1 d . . . H12A H 0.2805 0.2224 0.6033 0.038 Uiso 1 1 calc R . . C1 C 0.18687(13) 0.42024(10) 0.35060(9) 0.0322(3) Uani 1 1 d . . . H1A H 0.1895 0.3759 0.3087 0.039 Uiso 1 1 calc R . . C16 C 0.03060(10) 0.28812(11) 0.47732(9) 0.0294(3) Uani 1 1 d . . . C18 C 0.03438(11) 0.14504(10) 0.49532(11) 0.0336(3) Uani 1 1 d . . . H18A H 0.0366 0.0890 0.5207 0.040 Uiso 1 1 calc R . . C5 C 0.09908(13) 0.46191(11) 0.37711(11) 0.0366(3) Uani 1 1 d . . . H5A H 0.0302 0.4520 0.3566 0.044 Uiso 1 1 calc R . . C10 C 0.08796(12) 0.41732(12) 0.64019(10) 0.0361(3) Uani 1 1 d . . . H10A H 0.0151 0.4101 0.6500 0.043 Uiso 1 1 calc R . . C19 C 0.03663(12) 0.16228(12) 0.40928(11) 0.0361(3) Uani 1 1 d . . . H19A H 0.0410 0.1199 0.3656 0.043 Uiso 1 1 calc R . . C9 C 0.13652(14) 0.49426(11) 0.62127(11) 0.0386(4) Uani 1 1 d . . . H9A H 0.1035 0.5494 0.6167 0.046 Uiso 1 1 calc R . . C20 C 0.03339(11) 0.25010(11) 0.39733(10) 0.0324(3) Uani 1 1 d . . . H20A H 0.0334 0.2797 0.3444 0.039 Uiso 1 1 calc R . . C2 C 0.27185(12) 0.45976(10) 0.38712(10) 0.0321(3) Uani 1 1 d . . . H2A H 0.3431 0.4487 0.3735 0.039 Uiso 1 1 calc R . . C13 C 0.27741(12) 0.14029(10) 0.49907(14) 0.0400(3) Uani 1 1 d . . . H13A H 0.2708 0.0839 0.5231 0.048 Uiso 1 1 calc R . . C3 C 0.23595(13) 0.52692(10) 0.43610(11) 0.0352(3) Uani 1 1 d . . . H3A H 0.2780 0.5708 0.4614 0.042 Uiso 1 1 calc R . . C7 C 0.25857(12) 0.39396(12) 0.64468(9) 0.0357(3) Uani 1 1 d . . . H7A H 0.3241 0.3681 0.6579 0.043 Uiso 1 1 calc R . . C4 C 0.12904(13) 0.52810(10) 0.43006(12) 0.0376(3) Uani 1 1 d . . . H4A H 0.0846 0.5726 0.4511 0.045 Uiso 1 1 calc R . . C6 C 0.16299(13) 0.35578(11) 0.65434(8) 0.0332(3) Uani 1 1 d . . . H6A H 0.1509 0.2987 0.6752 0.040 Uiso 1 1 calc R . . C8 C 0.24269(15) 0.47946(12) 0.62408(11) 0.0392(4) Uani 1 1 d . . . H8A H 0.2954 0.5229 0.6213 0.047 Uiso 1 1 calc R . . C14 C 0.28290(12) 0.15920(11) 0.41355(12) 0.0379(4) Uani 1 1 d . . . H14A H 0.2803 0.1181 0.3686 0.045 Uiso 1 1 calc R . . F26 F 0.18729(7) 0.70883(5) 0.49761(5) 0.03399(18) Uani 1 1 d . . . F32 F 0.04392(7) 0.74498(5) 0.75992(5) 0.02758(16) Uani 1 1 d . . . C31 C 0.00246(9) 0.72657(8) 0.61861(7) 0.01869(19) Uani 1 1 d . . . F46 F 0.20551(7) 0.68352(5) 0.66633(6) 0.02883(17) Uani 1 1 d . . . C21 C 0.07692(9) 0.82641(7) 0.49393(7) 0.01996(19) Uani 1 1 d . . . F22 F -0.03174(8) 0.94469(6) 0.46965(6) 0.0359(2) Uani 1 1 d . . . C41 C 0.17319(10) 0.82809(7) 0.63337(6) 0.01879(18) Uani 1 1 d . . . F42 F 0.17081(7) 0.97410(5) 0.59915(6) 0.03094(17) Uani 1 1 d . . . F33 F -0.06155(9) 0.61123(7) 0.80788(5) 0.0420(2) Uani 1 1 d . . . F35 F -0.16266(9) 0.56063(6) 0.53488(6) 0.0445(3) Uani 1 1 d . . . F36 F -0.05754(8) 0.69289(6) 0.48415(5) 0.0348(2) Uani 1 1 d . . . C42 C 0.21983(10) 0.90678(8) 0.63124(8) 0.0224(2) Uani 1 1 d . . . C25 C 0.16959(12) 0.77619(9) 0.37162(8) 0.0290(2) Uani 1 1 d . . . C32 C -0.00484(10) 0.70064(8) 0.70032(7) 0.0221(2) Uani 1 1 d . . . C45 C 0.33646(10) 0.77770(9) 0.68694(7) 0.0250(2) Uani 1 1 d . . . C35 C -0.11093(11) 0.60674(9) 0.59017(8) 0.0275(2) Uani 1 1 d . . . C46 C 0.23692(10) 0.76482(8) 0.66229(7) 0.0213(2) Uani 1 1 d . . . C34 C -0.11434(12) 0.58432(9) 0.67202(9) 0.0284(3) Uani 1 1 d . . . C44 C 0.37753(10) 0.85773(11) 0.68479(8) 0.0285(3) Uani 1 1 d . . . C43 C 0.31837(11) 0.92277(9) 0.65686(8) 0.0274(2) Uani 1 1 d . . . C36 C -0.05374(10) 0.67617(8) 0.56551(7) 0.0230(2) Uani 1 1 d . . . F45 F 0.39461(7) 0.71171(7) 0.71003(6) 0.0355(2) Uani 1 1 d . . . F25 F 0.23405(9) 0.72060(8) 0.33793(6) 0.0451(3) Uani 1 1 d . . . C22 C 0.03690(10) 0.88785(9) 0.44209(8) 0.0244(2) Uani 1 1 d . . . F44 F 0.47511(7) 0.87019(8) 0.70684(7) 0.0413(2) Uani 1 1 d . . . F34 F -0.16846(10) 0.51743(6) 0.69698(6) 0.0443(3) Uani 1 1 d . . . B1 B 0.05714(10) 0.81754(8) 0.59464(8) 0.0189(2) Uani 1 1 d . . . F43 F 0.35722(8) 1.00115(6) 0.65104(7) 0.0426(2) Uani 1 1 d . . . C26 C 0.14397(10) 0.77221(8) 0.45434(8) 0.0243(2) Uani 1 1 d . . . C33 C -0.05979(11) 0.63213(9) 0.72777(8) 0.0262(2) Uani 1 1 d . . . C101 C -0.01939(11) 0.88777(9) 0.63407(8) 0.0258(2) Uani 1 1 d . . . C23 C 0.06105(12) 0.89515(10) 0.35898(8) 0.0313(3) Uani 1 1 d . . . F24 F 0.14957(11) 0.84316(8) 0.24323(6) 0.0526(3) Uani 1 1 d . . . F23 F 0.01764(11) 0.95559(8) 0.31286(6) 0.0500(3) Uani 1 1 d . . . C24 C 0.12727(13) 0.83884(10) 0.32385(9) 0.0330(3) Uani 1 1 d . . . H16 H 0.0103(19) 0.3388(15) 0.4886(16) 0.051(6) Uiso 1 1 d . . . H101 H -0.0856(15) 0.8770(12) 0.6192(12) 0.030(5) Uiso 1 1 d . . . H102 H -0.0022(15) 0.9436(13) 0.6223(12) 0.031(5) Uiso 1 1 d . . . H103 H -0.0177(15) 0.8801(12) 0.6955(13) 0.032(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01777(4) 0.01930(4) 0.02123(5) -0.00015(4) 0.00170(4) 0.00049(3) Fe1 0.01884(7) 0.02012(7) 0.02454(8) 0.00008(6) 0.00403(6) -0.00018(6) C17 0.0226(5) 0.0388(7) 0.0259(6) 0.0046(6) 0.0061(4) 0.0000(5) C11 0.0208(5) 0.0339(6) 0.0289(7) 0.0037(5) 0.0001(4) -0.0049(5) C15 0.0207(5) 0.0352(7) 0.0339(7) -0.0023(6) 0.0087(5) -0.0006(5) C12 0.0209(5) 0.0372(7) 0.0377(7) 0.0104(6) -0.0015(5) 0.0029(5) C1 0.0431(8) 0.0303(6) 0.0232(6) 0.0069(5) -0.0001(5) -0.0049(6) C16 0.0229(5) 0.0380(7) 0.0273(6) 0.0050(5) 0.0048(4) 0.0081(5) C18 0.0289(6) 0.0359(7) 0.0359(7) 0.0021(6) 0.0051(6) -0.0118(5) C5 0.0350(8) 0.0365(8) 0.0384(8) 0.0157(6) -0.0073(6) 0.0008(6) C10 0.0307(7) 0.0504(10) 0.0273(7) -0.0097(6) 0.0087(5) 0.0013(6) C19 0.0285(7) 0.0463(9) 0.0335(7) -0.0055(7) 0.0023(5) -0.0144(6) C9 0.0478(9) 0.0336(8) 0.0345(8) -0.0125(6) 0.0064(7) 0.0049(7) C20 0.0227(6) 0.0503(9) 0.0241(6) 0.0038(6) 0.0011(5) -0.0013(6) C2 0.0316(7) 0.0335(7) 0.0312(7) 0.0070(6) 0.0074(5) -0.0053(6) C13 0.0309(7) 0.0301(7) 0.0589(10) 0.0080(8) 0.0039(8) 0.0106(5) C3 0.0404(8) 0.0252(6) 0.0400(8) 0.0050(6) 0.0039(6) -0.0098(6) C7 0.0312(7) 0.0513(9) 0.0247(6) -0.0066(7) -0.0039(5) 0.0000(7) C4 0.0410(8) 0.0246(7) 0.0473(9) 0.0103(6) 0.0050(7) 0.0076(6) C6 0.0401(8) 0.0394(7) 0.0202(5) -0.0008(5) 0.0026(5) -0.0016(6) C8 0.0444(9) 0.0416(9) 0.0316(8) -0.0120(7) 0.0001(6) -0.0123(7) C14 0.0304(7) 0.0317(7) 0.0514(10) -0.0093(7) 0.0106(7) 0.0065(6) F26 0.0496(5) 0.0284(4) 0.0240(3) -0.0024(3) -0.0013(4) 0.0156(3) F32 0.0372(4) 0.0304(4) 0.0151(3) -0.0012(3) -0.0037(3) -0.0111(3) C31 0.0214(5) 0.0191(5) 0.0156(4) -0.0005(4) -0.0018(3) -0.0021(4) F46 0.0301(4) 0.0214(4) 0.0350(4) 0.0050(3) -0.0047(3) 0.0000(3) C21 0.0232(5) 0.0195(4) 0.0172(5) 0.0007(4) -0.0020(4) -0.0016(3) F22 0.0419(5) 0.0339(5) 0.0320(4) 0.0057(4) -0.0007(4) 0.0146(4) C41 0.0218(5) 0.0197(4) 0.0148(4) -0.0015(3) -0.0007(4) -0.0015(4) F42 0.0347(4) 0.0186(3) 0.0395(4) 0.0031(3) -0.0004(4) -0.0016(3) F33 0.0699(7) 0.0372(5) 0.0189(4) 0.0047(3) 0.0015(4) -0.0213(5) F35 0.0641(7) 0.0393(5) 0.0301(4) -0.0032(4) -0.0139(5) -0.0275(5) F36 0.0502(5) 0.0382(5) 0.0160(4) 0.0015(3) -0.0099(3) -0.0165(4) C42 0.0264(5) 0.0219(5) 0.0190(5) -0.0020(4) 0.0009(4) -0.0028(4) C25 0.0352(7) 0.0314(6) 0.0203(5) -0.0047(4) 0.0040(5) -0.0023(6) C32 0.0260(5) 0.0241(6) 0.0162(5) -0.0015(4) -0.0017(4) -0.0044(4) C45 0.0216(5) 0.0359(6) 0.0174(5) 0.0025(4) -0.0001(4) 0.0014(5) C35 0.0350(6) 0.0242(6) 0.0234(5) -0.0035(5) -0.0059(5) -0.0091(5) C46 0.0240(5) 0.0231(5) 0.0168(5) 0.0006(4) -0.0006(4) -0.0008(4) C34 0.0371(7) 0.0227(6) 0.0254(6) -0.0007(4) 0.0007(5) -0.0113(5) C44 0.0229(6) 0.0458(8) 0.0168(5) -0.0016(5) -0.0005(4) -0.0077(5) C43 0.0299(6) 0.0298(6) 0.0226(5) -0.0046(4) 0.0010(5) -0.0107(5) C36 0.0289(6) 0.0239(5) 0.0163(5) -0.0006(4) -0.0042(4) -0.0047(4) F45 0.0267(4) 0.0464(5) 0.0335(5) 0.0086(4) -0.0032(3) 0.0082(4) F25 0.0583(7) 0.0486(6) 0.0286(5) -0.0100(4) 0.0131(4) 0.0106(5) C22 0.0284(6) 0.0238(6) 0.0210(5) 0.0030(4) -0.0025(4) -0.0009(4) F44 0.0233(4) 0.0641(7) 0.0366(5) 0.0038(5) -0.0058(3) -0.0123(4) F34 0.0660(7) 0.0324(5) 0.0345(5) 0.0011(4) 0.0035(5) -0.0281(5) B1 0.0222(5) 0.0190(5) 0.0155(5) -0.0002(4) -0.0015(4) -0.0014(4) F43 0.0413(5) 0.0349(5) 0.0515(6) -0.0035(4) -0.0037(4) -0.0205(4) C26 0.0315(6) 0.0228(5) 0.0185(5) -0.0019(4) -0.0012(4) 0.0007(4) C33 0.0367(7) 0.0244(6) 0.0175(5) 0.0008(4) 0.0010(4) -0.0076(5) C101 0.0275(6) 0.0243(6) 0.0256(6) -0.0002(5) 0.0031(4) 0.0036(5) C23 0.0418(7) 0.0307(6) 0.0215(5) 0.0076(5) -0.0050(5) -0.0038(6) F24 0.0853(9) 0.0554(7) 0.0171(4) 0.0043(4) 0.0112(5) -0.0038(6) F23 0.0757(8) 0.0463(6) 0.0280(5) 0.0174(4) -0.0054(5) 0.0090(6) C24 0.0459(8) 0.0368(7) 0.0163(5) 0.0012(5) 0.0025(5) -0.0090(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C11 2.2894(15) . ? Zr1 C3 2.4773(15) . ? Zr1 C4 2.4912(16) . ? Zr1 C2 2.5008(14) . ? Zr1 C9 2.5034(15) . ? Zr1 C8 2.5037(16) . ? Zr1 C10 2.5132(15) . ? Zr1 C7 2.5242(15) . ? Zr1 C6 2.5257(14) . ? Zr1 C5 2.5317(16) . ? Zr1 C1 2.5389(14) . ? Zr1 C16 2.6151(17) . ? Fe1 C16 2.0199(14) . ? Fe1 C11 2.0224(13) . ? Fe1 C12 2.0548(15) . ? Fe1 C15 2.0589(14) . ? Fe1 C20 2.0608(15) . ? Fe1 C17 2.0631(13) . ? Fe1 C19 2.0693(15) . ? Fe1 C13 2.0703(15) . ? Fe1 C18 2.0713(13) . ? Fe1 C14 2.0802(15) . ? C17 C18 1.409(2) . ? C17 C16 1.431(2) . ? C11 C12 1.455(2) . ? C11 C15 1.457(2) . ? C15 C14 1.415(2) . ? C12 C13 1.417(3) . ? C1 C5 1.400(3) . ? C1 C2 1.414(2) . ? C16 C20 1.435(2) . ? C18 C19 1.427(3) . ? C5 C4 1.414(3) . ? C10 C6 1.408(2) . ? C10 C9 1.412(3) . ? C19 C20 1.407(3) . ? C9 C8 1.419(3) . ? C2 C3 1.412(2) . ? C13 C14 1.425(3) . ? C3 C4 1.412(2) . ? C7 C6 1.406(2) . ? C7 C8 1.413(3) . ? F26 C26 1.3536(15) . ? F32 C32 1.3594(14) . ? C31 C36 1.3908(16) . ? C31 C32 1.3950(17) . ? C31 B1 1.6595(18) . ? F46 C46 1.3562(15) . ? C21 C26 1.3909(18) . ? C21 C22 1.3927(17) . ? C21 B1 1.6650(18) . ? F22 C22 1.3535(16) . ? C41 C46 1.3906(17) . ? C41 C42 1.3919(17) . ? C41 B1 1.6625(18) . ? F42 C42 1.3529(15) . ? F33 C33 1.3452(16) . ? F35 C35 1.3449(15) . ? F36 C36 1.3510(15) . ? C42 C43 1.3872(19) . ? C25 F25 1.3415(18) . ? C25 C24 1.379(2) . ? C25 C26 1.3891(18) . ? C32 C33 1.3803(18) . ? C45 F45 1.3507(16) . ? C45 C44 1.381(2) . ? C45 C46 1.3867(18) . ? C35 C34 1.379(2) . ? C35 C36 1.3935(19) . ? C34 F34 1.3415(16) . ? C34 C33 1.3837(19) . ? C44 F44 1.3494(16) . ? C44 C43 1.371(2) . ? C43 F43 1.3480(17) . ? C22 C23 1.3941(19) . ? B1 C101 1.6340(19) . ? C23 F23 1.3452(18) . ? C23 C24 1.373(2) . ? F24 C24 1.3459(17) . ? 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 Zr1 C3 111.68(5) . . ? C11 Zr1 C4 136.69(6) . . ? C3 Zr1 C4 33.03(6) . . ? C11 Zr1 C2 83.04(5) . . ? C3 Zr1 C2 32.95(6) . . ? C4 Zr1 C2 54.39(6) . . ? C11 Zr1 C9 134.84(6) . . ? C3 Zr1 C9 83.79(6) . . ? C4 Zr1 C9 78.46(7) . . ? C2 Zr1 C9 115.92(6) . . ? C11 Zr1 C8 106.30(6) . . ? C3 Zr1 C8 78.48(6) . . ? C4 Zr1 C8 91.51(7) . . ? C2 Zr1 C8 101.93(6) . . ? C9 Zr1 C8 32.93(6) . . ? C11 Zr1 C10 120.81(6) . . ? C3 Zr1 C10 115.69(6) . . ? C4 Zr1 C10 101.74(6) . . ? C2 Zr1 C10 148.43(6) . . ? C9 Zr1 C10 32.70(6) . . ? C8 Zr1 C10 54.06(6) . . ? C11 Zr1 C7 80.54(5) . . ? C3 Zr1 C7 106.47(6) . . ? C4 Zr1 C7 124.14(6) . . ? C2 Zr1 C7 118.67(6) . . ? C9 Zr1 C7 54.30(6) . . ? C8 Zr1 C7 32.63(6) . . ? C10 Zr1 C7 53.81(5) . . ? C11 Zr1 C6 88.83(5) . . ? C3 Zr1 C6 132.08(6) . . ? C4 Zr1 C6 131.90(6) . . ? C2 Zr1 C6 151.01(6) . . ? C9 Zr1 C6 54.14(6) . . ? C8 Zr1 C6 53.89(6) . . ? C10 Zr1 C6 32.46(6) . . ? C7 Zr1 C6 32.34(6) . . ? C11 Zr1 C5 117.00(6) . . ? C3 Zr1 C5 54.36(6) . . ? C4 Zr1 C5 32.69(6) . . ? C2 Zr1 C5 53.94(6) . . ? C9 Zr1 C5 106.55(6) . . ? C8 Zr1 C5 124.20(7) . . ? C10 Zr1 C5 118.74(6) . . ? C7 Zr1 C5 156.84(6) . . ? C6 Zr1 C5 150.23(6) . . ? C11 Zr1 C1 86.68(5) . . ? C3 Zr1 C1 54.16(6) . . ? C4 Zr1 C1 53.79(6) . . ? C2 Zr1 C1 32.58(5) . . ? C9 Zr1 C1 131.97(6) . . ? C8 Zr1 C1 132.01(6) . . ? C10 Zr1 C1 150.80(6) . . ? C7 Zr1 C1 150.40(5) . . ? C6 Zr1 C1 173.54(5) . . ? C5 Zr1 C1 32.06(6) . . ? C11 Zr1 C16 86.75(5) . . ? C3 Zr1 C16 134.90(5) . . ? C4 Zr1 C16 106.60(5) . . ? C2 Zr1 C16 120.21(5) . . ? C9 Zr1 C16 112.56(5) . . ? C8 Zr1 C16 137.27(5) . . ? C10 Zr1 C16 84.06(5) . . ? C7 Zr1 C16 117.27(5) . . ? C6 Zr1 C16 86.85(5) . . ? C5 Zr1 C16 80.55(5) . . ? C1 Zr1 C16 88.27(5) . . ? C16 Fe1 C11 113.30(6) . . ? C16 Fe1 C12 128.45(7) . . ? C11 Fe1 C12 41.82(6) . . ? C16 Fe1 C15 128.97(6) . . ? C11 Fe1 C15 41.82(6) . . ? C12 Fe1 C15 68.29(6) . . ? C16 Fe1 C20 41.16(6) . . ? C11 Fe1 C20 128.64(6) . . ? C12 Fe1 C20 166.83(7) . . ? C15 Fe1 C20 110.87(6) . . ? C16 Fe1 C17 41.01(6) . . ? C11 Fe1 C17 126.33(6) . . ? C12 Fe1 C17 108.68(6) . . ? C15 Fe1 C17 165.39(6) . . ? C20 Fe1 C17 68.61(6) . . ? C16 Fe1 C19 67.90(7) . . ? C11 Fe1 C19 161.61(6) . . ? C12 Fe1 C19 152.30(7) . . ? C15 Fe1 C19 122.09(7) . . ? C20 Fe1 C19 39.84(7) . . ? C17 Fe1 C19 67.55(6) . . ? C16 Fe1 C13 159.55(7) . . ? C11 Fe1 C13 69.81(6) . . ? C12 Fe1 C13 40.19(8) . . ? C15 Fe1 C13 67.70(7) . . ? C20 Fe1 C13 152.67(8) . . ? C17 Fe1 C13 119.90(7) . . ? C19 Fe1 C13 115.98(8) . . ? C16 Fe1 C18 68.04(7) . . ? C11 Fe1 C18 158.08(7) . . ? C12 Fe1 C18 118.93(7) . . ? C15 Fe1 C18 154.52(7) . . ? C20 Fe1 C18 67.86(7) . . ? C17 Fe1 C18 39.85(7) . . ? C19 Fe1 C18 40.31(7) . . ? C13 Fe1 C18 101.35(7) . . ? C16 Fe1 C14 160.16(7) . . ? C11 Fe1 C14 69.65(7) . . ? C12 Fe1 C14 67.68(7) . . ? C15 Fe1 C14 39.98(7) . . ? C20 Fe1 C14 120.75(7) . . ? C17 Fe1 C14 153.53(7) . . ? C19 Fe1 C14 102.94(7) . . ? C13 Fe1 C14 40.17(8) . . ? C18 Fe1 C14 117.10(7) . . ? C16 Fe1 Zr1 61.35(5) . . ? C11 Fe1 Zr1 51.95(4) . . ? C12 Fe1 Zr1 79.84(5) . . ? C15 Fe1 Zr1 79.90(4) . . ? C20 Fe1 Zr1 87.06(5) . . ? C17 Fe1 Zr1 85.51(5) . . ? C19 Fe1 Zr1 125.64(5) . . ? C13 Fe1 Zr1 118.37(5) . . ? C18 Fe1 Zr1 124.57(5) . . ? C14 Fe1 Zr1 118.21(5) . . ? C18 C17 C16 107.43(14) . . ? C18 C17 Fe1 70.39(8) . . ? C16 C17 Fe1 67.87(7) . . ? C12 C11 C15 104.90(14) . . ? C12 C11 Fe1 70.28(8) . . ? C15 C11 Fe1 70.43(8) . . ? C12 C11 Zr1 117.97(10) . . ? C15 C11 Zr1 118.13(10) . . ? Fe1 C11 Zr1 83.97(5) . . ? C14 C15 C11 109.36(15) . . ? C14 C15 Fe1 70.82(9) . . ? C11 C15 Fe1 67.75(7) . . ? C13 C12 C11 109.23(15) . . ? C13 C12 Fe1 70.49(9) . . ? C11 C12 Fe1 67.90(8) . . ? C5 C1 C2 108.38(14) . . ? C5 C1 Zr1 73.68(9) . . ? C2 C1 Zr1 72.22(8) . . ? C17 C16 C20 108.40(14) . . ? C17 C16 Fe1 71.12(8) . . ? C20 C16 Fe1 70.95(8) . . ? C17 C16 Zr1 111.92(10) . . ? C20 C16 Zr1 114.36(10) . . ? Fe1 C16 Zr1 75.97(5) . . ? C17 C18 C19 108.23(15) . . ? C17 C18 Fe1 69.76(8) . . ? C19 C18 Fe1 69.77(8) . . ? C1 C5 C4 107.91(15) . . ? C1 C5 Zr1 74.25(9) . . ? C4 C5 Zr1 72.08(9) . . ? C6 C10 C9 108.46(15) . . ? C6 C10 Zr1 74.26(8) . . ? C9 C10 Zr1 73.27(9) . . ? C20 C19 C18 108.95(15) . . ? C20 C19 Fe1 69.75(9) . . ? C18 C19 Fe1 69.92(9) . . ? C10 C9 C8 107.25(16) . . ? C10 C9 Zr1 74.03(9) . . ? C8 C9 Zr1 73.55(9) . . ? C19 C20 C16 106.95(14) . . ? C19 C20 Fe1 70.40(9) . . ? C16 C20 Fe1 67.89(8) . . ? C3 C2 C1 107.84(14) . . ? C3 C2 Zr1 72.61(9) . . ? C1 C2 Zr1 75.19(8) . . ? C12 C13 C14 108.21(14) . . ? C12 C13 Fe1 69.31(8) . . ? C14 C13 Fe1 70.29(9) . . ? C2 C3 C4 107.75(16) . . ? C2 C3 Zr1 74.44(8) . . ? C4 C3 Zr1 74.03(9) . . ? C6 C7 C8 107.90(15) . . ? C6 C7 Zr1 73.89(8) . . ? C8 C7 Zr1 72.89(9) . . ? C3 C4 C5 108.12(16) . . ? C3 C4 Zr1 72.94(9) . . ? C5 C4 Zr1 75.23(9) . . ? C7 C6 C10 108.17(15) . . ? C7 C6 Zr1 73.77(9) . . ? C10 C6 Zr1 73.28(9) . . ? C7 C8 C9 108.21(16) . . ? C7 C8 Zr1 74.48(9) . . ? C9 C8 Zr1 73.52(10) . . ? C15 C14 C13 108.15(15) . . ? C15 C14 Fe1 69.20(8) . . ? C13 C14 Fe1 69.54(9) . . ? C36 C31 C32 112.69(11) . . ? C36 C31 B1 125.82(10) . . ? C32 C31 B1 120.69(10) . . ? C26 C21 C22 113.12(11) . . ? C26 C21 B1 120.20(10) . . ? C22 C21 B1 126.57(11) . . ? C46 C41 C42 112.90(11) . . ? C46 C41 B1 127.67(10) . . ? C42 C41 B1 119.14(10) . . ? F42 C42 C43 114.74(12) . . ? F42 C42 C41 120.45(11) . . ? C43 C42 C41 124.74(13) . . ? F25 C25 C24 119.96(13) . . ? F25 C25 C26 121.33(13) . . ? C24 C25 C26 118.71(14) . . ? F32 C32 C33 115.12(11) . . ? F32 C32 C31 119.65(11) . . ? C33 C32 C31 125.23(11) . . ? F45 C45 C44 119.83(12) . . ? F45 C45 C46 120.19(13) . . ? C44 C45 C46 119.93(13) . . ? F35 C35 C34 119.28(12) . . ? F35 C35 C36 120.75(12) . . ? C34 C35 C36 119.97(12) . . ? F46 C46 C45 114.50(11) . . ? F46 C46 C41 121.24(11) . . ? C45 C46 C41 124.24(12) . . ? F34 C34 C35 120.91(12) . . ? F34 C34 C33 120.75(13) . . ? C35 C34 C33 118.34(12) . . ? F44 C44 C43 121.32(14) . . ? F44 C44 C45 120.10(14) . . ? C43 C44 C45 118.53(12) . . ? F43 C43 C44 120.11(13) . . ? F43 C43 C42 120.20(14) . . ? C44 C43 C42 119.63(13) . . ? F36 C36 C31 121.03(11) . . ? F36 C36 C35 114.66(11) . . ? C31 C36 C35 124.30(11) . . ? F22 C22 C21 121.24(12) . . ? F22 C22 C23 114.74(12) . . ? C21 C22 C23 124.00(13) . . ? C101 B1 C31 103.46(10) . . ? C101 B1 C41 110.50(10) . . ? C31 B1 C41 113.44(10) . . ? C101 B1 C21 115.18(10) . . ? C31 B1 C21 111.88(9) . . ? C41 B1 C21 102.74(9) . . ? F26 C26 C25 115.80(12) . . ? F26 C26 C21 119.09(11) . . ? C25 C26 C21 125.10(13) . . ? F33 C33 C32 121.11(12) . . ? F33 C33 C34 119.42(12) . . ? C32 C33 C34 119.47(12) . . ? F23 C23 C24 120.11(13) . . ? F23 C23 C22 120.22(15) . . ? C24 C23 C22 119.65(14) . . ? F24 C24 C23 120.74(15) . . ? F24 C24 C25 119.84(15) . . ? C23 C24 C25 119.41(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 38.07 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.824 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.068 #===end data_[Cp2Zr(C5H3Me)Fe(C5H3Me)][MeB(C6F5)3] _audit_creation_method SHELXL-97 _chemical_formula_sum 'C41 H26 B F15 Fe Zr' _chemical_formula_weight 961.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.4146(16) _cell_length_b 15.9532(17) _cell_length_c 16.5904(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3550.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 0.9760 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 28569 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.63 _reflns_number_total 6676 _reflns_number_gt 5304 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.3709P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(2) _refine_ls_number_reflns 6676 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.50119(3) 0.78265(3) 0.32476(2) 0.02362(10) Uani 1 1 d . . . Fe1 Fe 0.47240(4) 0.78207(4) 0.49694(3) 0.02438(14) Uani 1 1 d . . . F1 F 0.8667(2) 0.94140(17) 1.21764(16) 0.0426(7) Uani 1 1 d . . . F2 F 0.5518(2) 0.49828(15) 0.89604(18) 0.0544(9) Uani 1 1 d . . . F3 F 0.2365(2) 0.96309(17) 0.87694(18) 0.0523(8) Uani 1 1 d . . . F4 F 0.3231(2) 0.98530(18) 1.02412(16) 0.0456(8) Uani 1 1 d . . . F5 F 0.5073(2) 0.93722(15) 1.05046(12) 0.0334(6) Uani 1 1 d . . . F6 F 0.5228(2) 0.75467(14) 1.02938(13) 0.0400(7) Uani 1 1 d . . . F7 F 0.6840(2) 0.56783(17) 0.79050(19) 0.0534(9) Uani 1 1 d . . . F8 F 0.73409(19) 0.72748(16) 0.80209(14) 0.0377(6) Uani 1 1 d . . . F9 F 0.4745(2) 0.59300(15) 1.01642(16) 0.0478(8) Uani 1 1 d . . . F10 F 0.7612(2) 0.73436(14) 1.03820(15) 0.0399(7) Uani 1 1 d . . . F11 F 0.8636(2) 0.77944(19) 1.16673(15) 0.0464(7) Uani 1 1 d . . . F12 F 0.7612(2) 1.05860(14) 1.13424(14) 0.0360(7) Uani 1 1 d . . . F13 F 0.66566(19) 1.01743(14) 1.00001(15) 0.0337(6) Uani 1 1 d . . . F14 F 0.5303(2) 0.84688(16) 0.77876(13) 0.0395(7) Uani 1 1 d . . . F15 F 0.3443(3) 0.89308(18) 0.75500(15) 0.0484(8) Uani 1 1 d . . . C1 C 0.8153(4) 0.9196(3) 1.1519(2) 0.0287(11) Uani 1 1 d . . . C2 C 0.8126(4) 0.8380(3) 1.1263(2) 0.0282(11) Uani 1 1 d . . . C3 C 0.7583(4) 0.8166(3) 1.0586(2) 0.0264(11) Uani 1 1 d . . . C4 C 0.7033(3) 0.8728(3) 1.0123(2) 0.0245(10) Uani 1 1 d . . . C5 C 0.5637(3) 0.7104(3) 0.9671(2) 0.0283(10) Uani 1 1 d . . . C6 C 0.6284(4) 0.7515(2) 0.9157(2) 0.0230(10) Uani 1 1 d . . . C7 C 0.6675(4) 0.6987(3) 0.8569(3) 0.0277(11) Uani 1 1 d . . . C8 C 0.6431(4) 0.6150(3) 0.8493(3) 0.0344(12) Uani 1 1 d . . . C9 C 0.5773(4) 0.5799(3) 0.9019(3) 0.0348(12) Uani 1 1 d . . . C10 C 0.3322(4) 0.9420(3) 0.8887(3) 0.0346(12) Uani 1 1 d . . . C11 C 0.3756(4) 0.9524(3) 0.9626(3) 0.0334(12) Uani 1 1 d . . . C12 C 0.4735(4) 0.9269(3) 0.9737(2) 0.0274(11) Uani 1 1 d . . . C13 C 0.5335(3) 0.8921(2) 0.9152(2) 0.0233(10) Uani 1 1 d . . . C14 C 0.5374(4) 0.6273(3) 0.9627(3) 0.0323(11) Uani 1 1 d . . . C15 C 0.7217(4) 0.8953(3) 0.8577(3) 0.0364(13) Uani 1 1 d . . . H15A H 0.7897 0.8742 0.8654 0.055 Uiso 1 1 calc R . . H15B H 0.7212 0.9563 0.8643 0.055 Uiso 1 1 calc R . . H15C H 0.6986 0.8809 0.8035 0.055 Uiso 1 1 calc R . . C16 C 0.7624(4) 0.9779(3) 1.1088(2) 0.0263(11) Uani 1 1 d . . . C17 C 0.7112(3) 0.9542(3) 1.0414(2) 0.0239(10) Uani 1 1 d . . . C18 C 0.4835(4) 0.8845(2) 0.8418(2) 0.0253(11) Uani 1 1 d . . . C19 C 0.3881(4) 0.9075(3) 0.8277(3) 0.0343(12) Uani 1 1 d . . . C20 C 0.5821(5) 0.6842(3) 0.2269(3) 0.0426(14) Uani 1 1 d . . . H20 H 0.6331 0.7054 0.1927 0.051 Uiso 1 1 calc R . . C21 C 0.4798(5) 0.6836(3) 0.2100(3) 0.0407(14) Uani 1 1 d . . . H21 H 0.4494 0.7045 0.1624 0.049 Uiso 1 1 calc R . . C22 C 0.4307(4) 0.6478(3) 0.2739(3) 0.0329(13) Uani 1 1 d . . . H22 H 0.3607 0.6400 0.2780 0.039 Uiso 1 1 calc R . . C23 C 0.5017(4) 0.6244(3) 0.3325(2) 0.0345(11) Uani 1 1 d . . . H23 H 0.4879 0.5976 0.3824 0.041 Uiso 1 1 calc R . . C24 C 0.5961(4) 0.6475(3) 0.3042(3) 0.0404(14) Uani 1 1 d . . . H24 H 0.6578 0.6402 0.3315 0.048 Uiso 1 1 calc R . . C25 C 0.4556(4) 0.8792(3) 0.2133(3) 0.0392(14) Uani 1 1 d . . . H25 H 0.4190 0.8561 0.1696 0.047 Uiso 1 1 calc R . . C26 C 0.5588(4) 0.8821(3) 0.2204(3) 0.0367(14) Uani 1 1 d . . . H26 H 0.6049 0.8615 0.1818 0.044 Uiso 1 1 calc R . . C27 C 0.5838(4) 0.9199(3) 0.2933(3) 0.0379(14) Uani 1 1 d . . . H27 H 0.6493 0.9296 0.3130 0.046 Uiso 1 1 calc R . . C28 C 0.4942(5) 0.9411(3) 0.3324(3) 0.0373(12) Uani 1 1 d . . . H28 H 0.4886 0.9673 0.3836 0.045 Uiso 1 1 calc R . . C29 C 0.4151(4) 0.9170(3) 0.2831(3) 0.0364(13) Uani 1 1 d . . . H29 H 0.3463 0.9246 0.2943 0.044 Uiso 1 1 calc R . . C30 C 0.6005(3) 0.7133(4) 0.4879(3) 0.0344(11) Uani 1 1 d . . . H30 H 0.6075 0.6572 0.4697 0.041 Uiso 1 1 calc R . . C31 C 0.5884(4) 0.7366(3) 0.5688(3) 0.0341(13) Uani 1 1 d . . . C32 C 0.5869(4) 0.6791(3) 0.6399(3) 0.0474(15) Uani 1 1 d . . . H32A H 0.5446 0.6306 0.6279 0.071 Uiso 1 1 calc R . . H32B H 0.5602 0.7090 0.6868 0.071 Uiso 1 1 calc R . . H32C H 0.6548 0.6601 0.6515 0.071 Uiso 1 1 calc R . . C33 C 0.5860(4) 0.8252(3) 0.5706(3) 0.0363(13) Uani 1 1 d . . . H33 H 0.5792 0.8584 0.6177 0.044 Uiso 1 1 calc R . . C34 C 0.5953(3) 0.8568(3) 0.4904(3) 0.0343(12) Uani 1 1 d . . . H34 H 0.5975 0.9143 0.4755 0.041 Uiso 1 1 calc R . . C35 C 0.6009(3) 0.7861(3) 0.4357(3) 0.0355(11) Uani 1 1 d . . . C36 C 0.3502(4) 0.8545(3) 0.4753(3) 0.0340(12) Uani 1 1 d . . . H36 H 0.3508 0.9113 0.4580 0.041 Uiso 1 1 calc R . . C37 C 0.3516(3) 0.7820(3) 0.4247(3) 0.0322(11) Uani 1 1 d . . . C38 C 0.3473(3) 0.7104(3) 0.4757(2) 0.0326(11) Uani 1 1 d . . . H38 H 0.3451 0.6537 0.4580 0.039 Uiso 1 1 calc R . . C39 C 0.3468(4) 0.7375(3) 0.5571(3) 0.0322(13) Uani 1 1 d . . . C40 C 0.3407(4) 0.6828(3) 0.6299(3) 0.0467(15) Uani 1 1 d . . . H40A H 0.3728 0.7110 0.6755 0.070 Uiso 1 1 calc R . . H40B H 0.3746 0.6296 0.6191 0.070 Uiso 1 1 calc R . . H40C H 0.2706 0.6720 0.6429 0.070 Uiso 1 1 calc R . . C41 C 0.3477(4) 0.8260(3) 0.5554(3) 0.0339(13) Uani 1 1 d . . . H41 H 0.3468 0.8612 0.6016 0.041 Uiso 1 1 calc R . . B1 B 0.6479(4) 0.8528(3) 0.9245(3) 0.0248(12) Uani 1 1 d . . . H37 H 0.336(4) 0.779(3) 0.369(3) 0.055(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0238(2) 0.0262(2) 0.02085(17) 0.00097(18) 0.00167(19) -0.0029(3) Fe1 0.0262(3) 0.0240(3) 0.0229(3) -0.0011(3) -0.0004(3) -0.0036(3) F1 0.046(2) 0.0465(18) 0.0352(15) -0.0058(13) -0.0098(15) -0.0027(15) F2 0.071(2) 0.0184(14) 0.074(2) -0.0019(14) 0.0011(18) -0.0061(15) F3 0.039(2) 0.0507(19) 0.067(2) -0.0043(15) -0.0218(16) 0.0199(16) F4 0.0389(18) 0.0511(19) 0.0469(17) -0.0078(14) 0.0061(14) 0.0147(15) F5 0.0351(16) 0.0442(15) 0.0210(11) -0.0023(10) 0.0036(13) 0.0050(15) F6 0.061(2) 0.0280(13) 0.0313(12) 0.0042(10) 0.0207(14) -0.0024(13) F7 0.070(2) 0.0324(17) 0.0578(18) -0.0142(14) 0.0176(17) 0.0049(15) F8 0.0412(16) 0.0348(15) 0.0372(14) -0.0085(13) 0.0165(12) -0.0012(14) F9 0.061(2) 0.0309(14) 0.0512(16) 0.0114(13) 0.0123(16) -0.0099(15) F10 0.0586(19) 0.0211(15) 0.0401(14) -0.0018(11) -0.0141(14) 0.0132(14) F11 0.0587(19) 0.0418(16) 0.0386(14) 0.0007(15) -0.0165(14) 0.0183(17) F12 0.0474(19) 0.0226(14) 0.0381(14) -0.0053(11) -0.0011(14) -0.0052(13) F13 0.0460(17) 0.0165(13) 0.0386(14) 0.0039(12) -0.0064(14) 0.0004(12) F14 0.056(2) 0.0401(15) 0.0222(12) -0.0043(11) -0.0007(13) 0.0048(15) F15 0.066(2) 0.0431(18) 0.0358(15) -0.0009(13) -0.0261(15) 0.0048(17) C1 0.033(3) 0.034(3) 0.019(2) 0.001(2) 0.001(2) -0.005(2) C2 0.033(3) 0.026(3) 0.025(2) 0.004(2) 0.002(2) 0.008(2) C3 0.029(3) 0.022(2) 0.029(2) 0.0035(18) 0.005(2) 0.003(2) C4 0.030(3) 0.023(2) 0.020(2) 0.0027(18) 0.006(2) 0.003(2) C5 0.040(3) 0.021(2) 0.024(2) 0.006(2) 0.001(2) 0.004(2) C6 0.029(3) 0.020(2) 0.020(2) 0.0033(17) 0.002(2) 0.004(2) C7 0.028(3) 0.025(3) 0.031(2) 0.000(2) -0.001(2) 0.001(2) C8 0.043(3) 0.027(3) 0.034(3) -0.010(2) 0.007(2) 0.010(2) C9 0.043(4) 0.015(2) 0.046(3) -0.001(2) -0.007(3) 0.001(2) C10 0.036(3) 0.022(3) 0.046(3) -0.001(2) -0.010(3) 0.004(2) C11 0.038(3) 0.025(3) 0.038(3) 0.000(2) 0.008(2) 0.006(2) C12 0.037(3) 0.026(2) 0.020(2) 0.0022(17) -0.005(2) 0.004(2) C13 0.032(3) 0.0122(19) 0.026(2) 0.0041(17) 0.002(2) -0.005(2) C14 0.039(3) 0.025(2) 0.033(2) 0.011(2) 0.000(2) -0.004(2) C15 0.049(4) 0.029(3) 0.031(2) 0.005(2) 0.009(2) -0.003(2) C16 0.027(3) 0.020(2) 0.032(2) -0.0020(19) 0.007(2) -0.003(2) C17 0.023(3) 0.021(2) 0.028(2) 0.005(2) -0.001(2) -0.001(2) C18 0.037(3) 0.016(2) 0.023(2) 0.0005(16) -0.002(2) 0.002(2) C19 0.046(3) 0.023(2) 0.033(3) 0.004(2) -0.017(3) -0.001(2) C20 0.050(4) 0.041(3) 0.036(3) -0.007(2) 0.019(3) -0.001(3) C21 0.061(5) 0.038(3) 0.023(2) -0.0048(19) 0.000(3) -0.009(3) C22 0.040(3) 0.033(3) 0.025(3) -0.008(2) 0.002(2) -0.016(3) C23 0.049(3) 0.024(2) 0.030(2) -0.0063(18) -0.003(3) -0.002(3) C24 0.043(4) 0.037(3) 0.042(3) -0.013(3) -0.002(3) 0.014(3) C25 0.047(4) 0.041(3) 0.031(3) 0.016(2) -0.006(3) -0.005(3) C26 0.043(4) 0.034(3) 0.033(3) 0.006(2) 0.013(3) -0.003(3) C27 0.031(3) 0.029(3) 0.053(3) 0.015(3) -0.003(3) -0.014(3) C28 0.056(4) 0.024(2) 0.032(2) 0.0065(18) 0.006(3) -0.001(3) C29 0.031(3) 0.040(3) 0.039(3) 0.013(2) 0.011(3) 0.006(3) C30 0.026(3) 0.041(3) 0.037(3) -0.006(3) -0.002(2) 0.004(3) C31 0.026(3) 0.045(4) 0.031(2) -0.003(2) -0.003(2) -0.003(2) C32 0.044(4) 0.057(4) 0.041(3) 0.007(3) -0.006(3) 0.011(3) C33 0.029(3) 0.041(3) 0.039(3) -0.009(2) -0.005(2) -0.012(3) C34 0.028(3) 0.031(3) 0.043(3) -0.007(2) 0.005(2) -0.012(2) C35 0.031(3) 0.038(3) 0.037(2) 0.000(3) 0.012(2) 0.001(3) C36 0.028(3) 0.034(3) 0.039(3) 0.005(2) 0.003(2) 0.001(3) C37 0.033(3) 0.034(3) 0.030(2) 0.002(3) -0.010(2) -0.007(3) C38 0.029(3) 0.034(3) 0.034(2) 0.001(2) -0.007(2) -0.009(3) C39 0.025(3) 0.039(3) 0.033(3) 0.009(2) 0.001(2) -0.012(2) C40 0.040(3) 0.060(4) 0.039(3) 0.016(2) 0.000(3) -0.017(3) C41 0.028(3) 0.038(3) 0.035(3) -0.003(2) 0.004(2) -0.008(3) B1 0.037(4) 0.019(3) 0.018(2) 0.002(2) 0.006(2) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C35 2.276(5) . ? Zr1 C26 2.472(5) . ? Zr1 C25 2.483(5) . ? Zr1 C21 2.491(4) . ? Zr1 C22 2.497(5) . ? Zr1 C20 2.506(5) . ? Zr1 C27 2.509(5) . ? Zr1 C24 2.527(5) . ? Zr1 C23 2.529(4) . ? Zr1 C29 2.531(5) . ? Zr1 C28 2.533(4) . ? Zr1 C37 2.603(5) . ? Zr1 H37 2.33(5) . ? Fe1 C35 2.003(4) . ? Fe1 C37 2.015(4) . ? Fe1 C36 2.037(5) . ? Fe1 C34 2.038(4) . ? Fe1 C30 2.044(5) . ? Fe1 C41 2.057(5) . ? Fe1 C38 2.061(5) . ? Fe1 C33 2.070(5) . ? Fe1 C39 2.084(5) . ? Fe1 C31 2.090(5) . ? F1 C1 1.336(5) . ? F2 C9 1.350(5) . ? F3 C10 1.342(6) . ? F4 C11 1.346(5) . ? F5 C12 1.362(5) . ? F6 C5 1.366(5) . ? F7 C8 1.350(5) . ? F8 C7 1.354(5) . ? F9 C14 1.344(5) . ? F10 C3 1.355(5) . ? F11 C2 1.338(5) . ? F12 C16 1.354(5) . ? F13 C17 1.365(5) . ? F14 C18 1.359(4) . ? F15 C19 1.361(5) . ? C1 C2 1.370(6) . ? C1 C16 1.371(6) . ? C2 C3 1.382(6) . ? C3 C4 1.393(6) . ? C4 C17 1.390(6) . ? C4 B1 1.666(6) . ? C5 C14 1.374(6) . ? C5 C6 1.383(6) . ? C6 C7 1.392(6) . ? C6 B1 1.642(7) . ? C7 C8 1.381(6) . ? C8 C9 1.361(7) . ? C9 C14 1.369(6) . ? C10 C11 1.367(6) . ? C10 C19 1.374(7) . ? C11 C12 1.387(6) . ? C12 C13 1.377(6) . ? C13 C18 1.396(6) . ? C13 B1 1.666(7) . ? C15 B1 1.633(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.365(6) . ? C18 C19 1.352(6) . ? C20 C21 1.401(8) . ? C20 C24 1.423(7) . ? C20 H20 0.9500 . ? C21 C22 1.372(6) . ? C21 H21 0.9500 . ? C22 C23 1.412(7) . ? C22 H22 0.9500 . ? C23 C24 1.401(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.391(7) . ? C25 C29 1.413(7) . ? C25 H25 0.9500 . ? C26 C27 1.392(7) . ? C26 H26 0.9500 . ? C27 C28 1.407(7) . ? C27 H27 0.9500 . ? C28 C29 1.394(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.402(6) . ? C30 C35 1.448(7) . ? C30 H30 0.9500 . ? C31 C33 1.413(6) . ? C31 C32 1.494(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.428(7) . ? C33 H33 0.9500 . ? C34 C35 1.450(6) . ? C34 H34 0.9500 . ? C36 C41 1.405(6) . ? C36 C37 1.429(7) . ? C36 H36 0.9500 . ? C37 C38 1.423(7) . ? C37 H37 0.95(5) . ? C38 C39 1.418(6) . ? C38 H38 0.9500 . ? C39 C41 1.413(6) . ? C39 C40 1.492(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41 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 C35 Zr1 C26 111.51(18) . . ? C35 Zr1 C25 137.04(19) . . ? C26 Zr1 C25 32.61(16) . . ? C35 Zr1 C21 134.52(18) . . ? C26 Zr1 C21 84.73(17) . . ? C25 Zr1 C21 78.25(16) . . ? C35 Zr1 C22 121.12(18) . . ? C26 Zr1 C22 115.77(16) . . ? C25 Zr1 C22 100.93(17) . . ? C21 Zr1 C22 31.93(15) . . ? C35 Zr1 C20 106.52(19) . . ? C26 Zr1 C20 79.22(16) . . ? C25 Zr1 C20 90.76(18) . . ? C21 Zr1 C20 32.57(18) . . ? C22 Zr1 C20 53.50(18) . . ? C35 Zr1 C27 83.53(18) . . ? C26 Zr1 C27 32.44(16) . . ? C25 Zr1 C27 54.02(18) . . ? C21 Zr1 C27 116.47(17) . . ? C22 Zr1 C27 148.09(17) . . ? C20 Zr1 C27 102.74(18) . . ? C35 Zr1 C24 80.40(17) . . ? C26 Zr1 C24 107.18(18) . . ? C25 Zr1 C24 123.59(17) . . ? C21 Zr1 C24 54.12(17) . . ? C22 Zr1 C24 53.87(18) . . ? C20 Zr1 C24 32.84(16) . . ? C27 Zr1 C24 119.58(17) . . ? C35 Zr1 C23 88.93(17) . . ? C26 Zr1 C23 132.52(16) . . ? C25 Zr1 C23 131.17(16) . . ? C21 Zr1 C23 53.53(14) . . ? C22 Zr1 C23 32.63(15) . . ? C20 Zr1 C23 53.57(16) . . ? C27 Zr1 C23 151.76(18) . . ? C24 Zr1 C23 32.17(17) . . ? C35 Zr1 C29 117.95(19) . . ? C26 Zr1 C29 53.68(17) . . ? C25 Zr1 C29 32.71(16) . . ? C21 Zr1 C29 106.02(17) . . ? C22 Zr1 C29 117.69(16) . . ? C20 Zr1 C29 123.44(17) . . ? C27 Zr1 C29 53.53(16) . . ? C24 Zr1 C29 156.29(17) . . ? C23 Zr1 C29 149.43(18) . . ? C35 Zr1 C28 87.54(18) . . ? C26 Zr1 C28 53.56(16) . . ? C25 Zr1 C28 53.76(16) . . ? C21 Zr1 C28 131.86(15) . . ? C22 Zr1 C28 149.64(17) . . ? C20 Zr1 C28 132.36(16) . . ? C27 Zr1 C28 32.41(16) . . ? C24 Zr1 C28 151.25(19) . . ? C23 Zr1 C28 173.88(13) . . ? C29 Zr1 C28 31.96(16) . . ? C35 Zr1 C37 86.45(15) . . ? C26 Zr1 C37 133.61(17) . . ? C25 Zr1 C37 106.67(17) . . ? C21 Zr1 C37 113.30(17) . . ? C22 Zr1 C37 85.42(16) . . ? C20 Zr1 C37 138.10(17) . . ? C27 Zr1 C37 118.45(17) . . ? C24 Zr1 C37 118.10(17) . . ? C23 Zr1 C37 88.03(17) . . ? C29 Zr1 C37 79.98(16) . . ? C28 Zr1 C37 86.76(17) . . ? C35 Zr1 H37 107.8(12) . . ? C26 Zr1 H37 122.2(13) . . ? C25 Zr1 H37 90.9(13) . . ? C21 Zr1 H37 96.4(13) . . ? C22 Zr1 H37 73.9(13) . . ? C20 Zr1 H37 126.7(13) . . ? C27 Zr1 H37 120.5(13) . . ? C24 Zr1 H37 119.9(13) . . ? C23 Zr1 H37 87.7(13) . . ? C29 Zr1 H37 71.0(13) . . ? C28 Zr1 H37 88.6(13) . . ? C37 Zr1 H37 21.4(12) . . ? C35 Fe1 C37 113.00(18) . . ? C35 Fe1 C36 125.8(2) . . ? C37 Fe1 C36 41.28(19) . . ? C35 Fe1 C34 42.06(19) . . ? C37 Fe1 C34 128.3(2) . . ? C36 Fe1 C34 108.03(19) . . ? C35 Fe1 C30 41.93(19) . . ? C37 Fe1 C30 129.21(19) . . ? C36 Fe1 C30 165.39(18) . . ? C34 Fe1 C30 68.26(18) . . ? C35 Fe1 C41 158.2(2) . . ? C37 Fe1 C41 68.07(19) . . ? C36 Fe1 C41 40.13(18) . . ? C34 Fe1 C41 118.91(19) . . ? C30 Fe1 C41 154.33(18) . . ? C35 Fe1 C38 129.19(19) . . ? C37 Fe1 C38 40.83(18) . . ? C36 Fe1 C38 68.27(18) . . ? C34 Fe1 C38 167.00(18) . . ? C30 Fe1 C38 111.98(19) . . ? C41 Fe1 C38 66.9(2) . . ? C35 Fe1 C33 69.81(19) . . ? C37 Fe1 C33 160.5(2) . . ? C36 Fe1 C33 120.5(2) . . ? C34 Fe1 C33 40.67(19) . . ? C30 Fe1 C33 66.6(2) . . ? C41 Fe1 C33 102.0(2) . . ? C38 Fe1 C33 152.18(19) . . ? C35 Fe1 C39 161.9(2) . . ? C37 Fe1 C39 68.55(18) . . ? C36 Fe1 C39 68.14(19) . . ? C34 Fe1 C39 151.60(18) . . ? C30 Fe1 C39 122.1(2) . . ? C41 Fe1 C39 39.91(17) . . ? C38 Fe1 C39 40.01(17) . . ? C33 Fe1 C39 115.23(19) . . ? C35 Fe1 C31 70.08(18) . . ? C37 Fe1 C31 159.7(2) . . ? C36 Fe1 C31 153.69(18) . . ? C34 Fe1 C31 68.3(2) . . ? C30 Fe1 C31 39.61(17) . . ? C41 Fe1 C31 117.08(19) . . ? C38 Fe1 C31 120.76(19) . . ? C33 Fe1 C31 39.70(17) . . ? C39 Fe1 C31 102.17(19) . . ? C35 Fe1 Zr1 51.80(13) . . ? C37 Fe1 Zr1 61.22(13) . . ? C36 Fe1 Zr1 86.06(13) . . ? C34 Fe1 Zr1 80.62(13) . . ? C30 Fe1 Zr1 79.41(12) . . ? C41 Fe1 Zr1 125.11(14) . . ? C38 Fe1 Zr1 86.63(12) . . ? C33 Fe1 Zr1 119.01(15) . . ? C39 Fe1 Zr1 125.73(12) . . ? C31 Fe1 Zr1 117.80(13) . . ? F1 C1 C2 120.9(4) . . ? F1 C1 C16 121.1(4) . . ? C2 C1 C16 118.0(4) . . ? F11 C2 C1 119.7(4) . . ? F11 C2 C3 120.2(4) . . ? C1 C2 C3 120.1(4) . . ? F10 C3 C2 115.3(4) . . ? F10 C3 C4 120.1(4) . . ? C2 C3 C4 124.6(4) . . ? C17 C4 C3 111.7(4) . . ? C17 C4 B1 121.2(4) . . ? C3 C4 B1 126.5(4) . . ? F6 C5 C14 115.9(4) . . ? F6 C5 C6 118.3(4) . . ? C14 C5 C6 125.8(4) . . ? C5 C6 C7 112.5(4) . . ? C5 C6 B1 120.8(4) . . ? C7 C6 B1 126.6(4) . . ? F8 C7 C8 115.1(4) . . ? F8 C7 C6 121.0(4) . . ? C8 C7 C6 124.0(4) . . ? F7 C8 C9 119.9(4) . . ? F7 C8 C7 120.5(4) . . ? C9 C8 C7 119.6(4) . . ? F2 C9 C8 121.0(4) . . ? F2 C9 C14 119.1(4) . . ? C8 C9 C14 119.9(4) . . ? F3 C10 C11 120.5(5) . . ? F3 C10 C19 121.0(4) . . ? C11 C10 C19 118.5(5) . . ? F4 C11 C10 120.3(5) . . ? F4 C11 C12 120.6(4) . . ? C10 C11 C12 119.1(4) . . ? F5 C12 C13 120.9(4) . . ? F5 C12 C11 113.8(4) . . ? C13 C12 C11 125.3(4) . . ? C12 C13 C18 111.7(4) . . ? C12 C13 B1 128.7(4) . . ? C18 C13 B1 119.4(4) . . ? F9 C14 C9 120.6(4) . . ? F9 C14 C5 121.2(4) . . ? C9 C14 C5 118.2(4) . . ? B1 C15 H15A 109.5 . . ? B1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? B1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? F12 C16 C17 120.8(4) . . ? F12 C16 C1 119.2(4) . . ? C17 C16 C1 120.0(4) . . ? F13 C17 C16 115.7(4) . . ? F13 C17 C4 118.7(4) . . ? C16 C17 C4 125.6(4) . . ? C19 C18 F14 115.2(4) . . ? C19 C18 C13 125.5(4) . . ? F14 C18 C13 119.2(4) . . ? C18 C19 F15 121.0(4) . . ? C18 C19 C10 119.9(4) . . ? F15 C19 C10 119.1(4) . . ? C21 C20 C24 107.8(5) . . ? C21 C20 Zr1 73.1(3) . . ? C24 C20 Zr1 74.4(3) . . ? C21 C20 H20 126.1 . . ? C24 C20 H20 126.1 . . ? Zr1 C20 H20 118.4 . . ? C22 C21 C20 108.6(5) . . ? C22 C21 Zr1 74.3(3) . . ? C20 C21 Zr1 74.3(3) . . ? C22 C21 H21 125.7 . . ? C20 C21 H21 125.7 . . ? Zr1 C21 H21 117.6 . . ? C21 C22 C23 108.6(5) . . ? C21 C22 Zr1 73.8(3) . . ? C23 C22 Zr1 74.9(2) . . ? C21 C22 H22 125.7 . . ? C23 C22 H22 125.7 . . ? Zr1 C22 H22 117.6 . . ? C24 C23 C22 108.0(4) . . ? C24 C23 Zr1 73.8(3) . . ? C22 C23 Zr1 72.5(2) . . ? C24 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? Zr1 C23 H23 119.5 . . ? C23 C24 C20 106.9(5) . . ? C23 C24 Zr1 74.0(3) . . ? C20 C24 Zr1 72.8(3) . . ? C23 C24 H24 126.5 . . ? C20 C24 H24 126.5 . . ? Zr1 C24 H24 118.7 . . ? C26 C25 C29 107.4(5) . . ? C26 C25 Zr1 73.2(3) . . ? C29 C25 Zr1 75.5(3) . . ? C26 C25 H25 126.3 . . ? C29 C25 H25 126.3 . . ? Zr1 C25 H25 117.1 . . ? C25 C26 C27 109.1(5) . . ? C25 C26 Zr1 74.2(3) . . ? C27 C26 Zr1 75.3(3) . . ? C25 C26 H26 125.4 . . ? C27 C26 H26 125.4 . . ? Zr1 C26 H26 117.1 . . ? C26 C27 C28 107.4(5) . . ? C26 C27 Zr1 72.3(3) . . ? C28 C27 Zr1 74.7(3) . . ? C26 C27 H27 126.3 . . ? C28 C27 H27 126.3 . . ? Zr1 C27 H27 118.6 . . ? C29 C28 C27 108.2(4) . . ? C29 C28 Zr1 73.9(3) . . ? C27 C28 Zr1 72.9(3) . . ? C29 C28 H28 125.9 . . ? C27 C28 H28 125.9 . . ? Zr1 C28 H28 119.2 . . ? C28 C29 C25 107.9(5) . . ? C28 C29 Zr1 74.1(3) . . ? C25 C29 Zr1 71.8(3) . . ? C28 C29 H29 126.1 . . ? C25 C29 H29 126.1 . . ? Zr1 C29 H29 119.9 . . ? C31 C30 C35 111.1(5) . . ? C31 C30 Fe1 72.0(3) . . ? C35 C30 Fe1 67.5(3) . . ? C31 C30 H30 124.4 . . ? C35 C30 H30 124.4 . . ? Fe1 C30 H30 127.8 . . ? C30 C31 C33 106.7(5) . . ? C30 C31 C32 126.5(5) . . ? C33 C31 C32 126.6(5) . . ? C30 C31 Fe1 68.4(3) . . ? C33 C31 Fe1 69.4(3) . . ? C32 C31 Fe1 130.7(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 C34 109.4(5) . . ? C31 C33 Fe1 70.9(3) . . ? C34 C33 Fe1 68.5(3) . . ? C31 C33 H33 125.3 . . ? C34 C33 H33 125.3 . . ? Fe1 C33 H33 126.9 . . ? C33 C34 C35 108.2(4) . . ? C33 C34 Fe1 70.9(3) . . ? C35 C34 Fe1 67.7(2) . . ? C33 C34 H34 125.9 . . ? C35 C34 H34 125.9 . . ? Fe1 C34 H34 127.1 . . ? C30 C35 C34 104.4(4) . . ? C30 C35 Fe1 70.6(3) . . ? C34 C35 Fe1 70.3(2) . . ? C30 C35 Zr1 117.5(3) . . ? C34 C35 Zr1 119.6(4) . . ? Fe1 C35 Zr1 84.45(17) . . ? C41 C36 C37 107.1(4) . . ? C41 C36 Fe1 70.7(3) . . ? C37 C36 Fe1 68.5(3) . . ? C41 C36 H36 126.5 . . ? C37 C36 H36 126.5 . . ? Fe1 C36 H36 125.9 . . ? C38 C37 C36 107.5(4) . . ? C38 C37 Fe1 71.3(3) . . ? C36 C37 Fe1 70.2(3) . . ? C38 C37 Zr1 114.4(3) . . ? C36 C37 Zr1 112.4(3) . . ? Fe1 C37 Zr1 76.06(15) . . ? C38 C37 H37 122(3) . . ? C36 C37 H37 128(3) . . ? Fe1 C37 H37 139(3) . . ? Zr1 C37 H37 63(3) . . ? C39 C38 C37 108.7(4) . . ? C39 C38 Fe1 70.8(3) . . ? C37 C38 Fe1 67.8(3) . . ? C39 C38 H38 125.6 . . ? C37 C38 H38 125.6 . . ? Fe1 C38 H38 127.3 . . ? C41 C39 C38 106.6(4) . . ? C41 C39 C40 126.9(5) . . ? C38 C39 C40 126.4(4) . . ? C41 C39 Fe1 69.0(3) . . ? C38 C39 Fe1 69.2(3) . . ? C40 C39 Fe1 129.2(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 C39 110.0(4) . . ? C36 C41 Fe1 69.2(3) . . ? C39 C41 Fe1 71.1(3) . . ? C36 C41 H41 125.0 . . ? C39 C41 H41 125.0 . . ? Fe1 C41 H41 126.3 . . ? C15 B1 C6 116.4(4) . . ? C15 B1 C13 109.9(4) . . ? C6 B1 C13 102.4(4) . . ? C15 B1 C4 104.0(4) . . ? C6 B1 C4 109.7(3) . . ? C13 B1 C4 114.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.486 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.072 #===end data_[Cp2Zr(C5H4)FeCp(PMe3)][MeB(C6F5)3](C6H5Br) _audit_creation_method SHELXL-97 _chemical_formula_sum 'C43.50 H32.25 B Br0.25 F15 Fe P Zr' _chemical_formula_weight 1048.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7013(6) _cell_length_b 15.4895(8) _cell_length_c 22.0666(11) _cell_angle_alpha 110.254(2) _cell_angle_beta 97.413(2) _cell_angle_gamma 91.311(2) _cell_volume 4028.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7515 _exptl_absorpt_correction_T_max 0.9058 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 101607 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 31.72 _reflns_number_total 27023 _reflns_number_gt 20403 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.8288P] 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_number_reflns 27023 _refine_ls_number_parameters 1162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1A Zr 0.227216(13) 0.038903(11) 0.242678(8) 0.01915(4) Uani 1 1 d . . . Zr1B Zr 0.206355(13) 0.398892(11) 0.746630(8) 0.01975(4) Uani 1 1 d . . . Fe1B Fe 0.181661(19) 0.396925(16) 0.581869(11) 0.01922(5) Uani 1 1 d . . . Fe1A Fe -0.01916(2) 0.114829(17) 0.288337(12) 0.02305(6) Uani 1 1 d . . . P1A P 0.31570(4) -0.07213(3) 0.30393(2) 0.02175(9) Uani 1 1 d . . . P1B P 0.28227(4) 0.56765(3) 0.83113(2) 0.02921(11) Uani 1 1 d . . . F32B F 0.39661(9) 0.92715(8) 0.58444(5) 0.0337(3) Uani 1 1 d . . . F32A F 0.14052(9) 0.16643(9) -0.10481(6) 0.0365(3) Uani 1 1 d . . . F33B F 0.27736(11) 1.06935(8) 0.59677(6) 0.0412(3) Uani 1 1 d . . . F33A F 0.25536(11) 0.06713(9) -0.19120(6) 0.0421(3) Uani 1 1 d . . . F34B F 0.10168(10) 1.05582(7) 0.50775(6) 0.0365(3) Uani 1 1 d . . . F34A F 0.47172(10) 0.07597(9) -0.16426(6) 0.0408(3) Uani 1 1 d . . . F35B F 0.04468(8) 0.89174(7) 0.40770(5) 0.0284(2) Uani 1 1 d . . . F35A F 0.57069(9) 0.19205(9) -0.04587(6) 0.0424(3) Uani 1 1 d . . . F36B F 0.15573(8) 0.74864(7) 0.39638(5) 0.0218(2) Uani 1 1 d . . . F36A F 0.45842(9) 0.29260(8) 0.04307(5) 0.0341(3) Uani 1 1 d . . . F42B F 0.43065(10) 0.64762(9) 0.34048(6) 0.0379(3) Uani 1 1 d . . . F42A F 0.37033(9) 0.41586(8) -0.01079(5) 0.0314(2) Uani 1 1 d . . . F43B F 0.34866(11) 0.48618(9) 0.25826(5) 0.0415(3) Uani 1 1 d . . . F43A F 0.43368(10) 0.59183(8) 0.05479(6) 0.0353(3) Uani 1 1 d . . . F44B F 0.18336(12) 0.39559(8) 0.28492(6) 0.0464(3) Uani 1 1 d . . . F44A F 0.35748(10) 0.68668(8) 0.16687(6) 0.0378(3) Uani 1 1 d . . . F45B F 0.11037(10) 0.47053(8) 0.40141(6) 0.0399(3) Uani 1 1 d . . . F45A F 0.21423(10) 0.59952(8) 0.21229(5) 0.0356(3) Uani 1 1 d . . . F46B F 0.19516(8) 0.63332(7) 0.48718(5) 0.0266(2) Uani 1 1 d . . . F46A F 0.15521(9) 0.42202(8) 0.15098(5) 0.0310(2) Uani 1 1 d . . . F52B F 0.53488(9) 0.62360(8) 0.48023(5) 0.0307(2) Uani 1 1 d . . . F52A F 0.12882(9) 0.39196(9) -0.04402(6) 0.0387(3) Uani 1 1 d . . . F53B F 0.61201(9) 0.56900(8) 0.57665(6) 0.0363(3) Uani 1 1 d . . . F53A F -0.07708(11) 0.40383(11) -0.07767(7) 0.0512(4) Uani 1 1 d . . . F54B F 0.53036(9) 0.62514(8) 0.69197(6) 0.0337(3) Uani 1 1 d . . . F54A F -0.22552(9) 0.30202(10) -0.04759(6) 0.0423(3) Uani 1 1 d . . . F55B F 0.36768(10) 0.73838(9) 0.70638(5) 0.0346(3) Uani 1 1 d . . . F55A F -0.16172(11) 0.19179(10) 0.02137(7) 0.0489(3) Uani 1 1 d . . . F56B F 0.28754(9) 0.79440(8) 0.61045(5) 0.0309(2) Uani 1 1 d . . . F56A F 0.04264(11) 0.18186(10) 0.05881(7) 0.0482(3) Uani 1 1 d . . . B1B B 0.37048(15) 0.74751(13) 0.47675(9) 0.0203(4) Uani 1 1 d . . . B1A B 0.22818(16) 0.29381(14) 0.03654(9) 0.0217(4) Uani 1 1 d . . . C1A C 0.40600(15) 0.11879(13) 0.30348(10) 0.0300(4) Uani 1 1 d . . . H1AA H 0.4675 0.0882 0.3184 0.036 Uiso 1 1 calc R . . C1B C 0.3749(2) 0.37044(19) 0.80924(11) 0.0468(6) Uani 1 1 d . . . H1BA H 0.4106 0.4127 0.8529 0.056 Uiso 1 1 calc R . . C2A C 0.32889(15) 0.16341(12) 0.34163(9) 0.0269(4) Uani 1 1 d . . . H2AA H 0.3267 0.1699 0.3881 0.032 Uiso 1 1 calc R . . C2B C 0.40075(17) 0.36733(17) 0.74871(11) 0.0380(5) Uani 1 1 d . . . H2BA H 0.4580 0.4072 0.7421 0.046 Uiso 1 1 calc R . . C3A C 0.26590(16) 0.20869(12) 0.30667(10) 0.0300(4) Uani 1 1 d . . . H3AA H 0.2121 0.2533 0.3242 0.036 Uiso 1 1 calc R . . C3B C 0.34390(19) 0.29127(16) 0.70022(11) 0.0393(5) Uani 1 1 d . . . H3BA H 0.3544 0.2669 0.6533 0.047 Uiso 1 1 calc R . . C4A C 0.30267(18) 0.19057(14) 0.24597(10) 0.0360(5) Uani 1 1 d . . . H4AA H 0.2802 0.2212 0.2137 0.043 Uiso 1 1 calc R . . C4B C 0.2808(2) 0.24722(17) 0.73051(15) 0.0542(7) Uani 1 1 d . . . H4BA H 0.2404 0.1856 0.7090 0.065 Uiso 1 1 calc R . . C5A C 0.39026(17) 0.13585(15) 0.24482(11) 0.0355(5) Uani 1 1 d . . . H5AA H 0.4392 0.1202 0.2111 0.043 Uiso 1 1 calc R . . C5B C 0.3015(2) 0.2966(2) 0.79836(14) 0.0577(8) Uani 1 1 d . . . H5BA H 0.2769 0.2763 0.8329 0.069 Uiso 1 1 calc R . . C6A C 0.24922(16) -0.10805(13) 0.15109(9) 0.0299(4) Uani 1 1 d . . . H6AA H 0.2997 -0.1557 0.1537 0.036 Uiso 1 1 calc R . . C6B C 0.06154(17) 0.44325(18) 0.81813(10) 0.0389(5) Uani 1 1 d . . . H6BA H 0.0717 0.4864 0.8645 0.047 Uiso 1 1 calc R . . C7A C 0.14083(16) -0.11011(13) 0.15948(9) 0.0283(4) Uani 1 1 d . . . H7AA H 0.1019 -0.1594 0.1693 0.034 Uiso 1 1 calc R . . C7B C 0.02839(15) 0.46770(17) 0.76256(10) 0.0358(5) Uani 1 1 d . . . H7BA H 0.0113 0.5307 0.7633 0.043 Uiso 1 1 calc R . . C8A C 0.09413(16) -0.03961(14) 0.14213(9) 0.0298(4) Uani 1 1 d . . . H8AA H 0.0163 -0.0302 0.1375 0.036 Uiso 1 1 calc R . . C8B C 0.00967(16) 0.38613(16) 0.70790(10) 0.0357(5) Uani 1 1 d . . . H8BA H -0.0240 0.3811 0.6632 0.043 Uiso 1 1 calc R . . C9A C 0.17315(17) 0.00830(14) 0.12407(9) 0.0317(4) Uani 1 1 d . . . H9AA H 0.1606 0.0561 0.1035 0.038 Uiso 1 1 calc R . . C9B C 0.03233(18) 0.31133(17) 0.72900(11) 0.0412(5) Uani 1 1 d . . . H9BA H 0.0157 0.2446 0.7019 0.049 Uiso 1 1 calc R . . C10A C 0.26871(17) -0.03551(15) 0.12882(9) 0.0322(4) Uani 1 1 d . . . H10A H 0.3355 -0.0229 0.1128 0.039 Uiso 1 1 calc R . . C10B C 0.06295(18) 0.34742(18) 0.79775(11) 0.0421(5) Uani 1 1 d . . . H10B H 0.0729 0.3104 0.8270 0.050 Uiso 1 1 calc R . . C11A C 0.10033(14) 0.03110(11) 0.30266(8) 0.0220(3) Uani 1 1 d . . . C11B C 0.22897(14) 0.47626(12) 0.67973(8) 0.0218(3) Uani 1 1 d . . . C12B C 0.31430(15) 0.47076(12) 0.64092(8) 0.0238(3) Uani 1 1 d . . . H12A H 0.3842 0.4448 0.6481 0.029 Uiso 1 1 calc R . . C12A C 0.08422(15) 0.10181(12) 0.36351(8) 0.0258(4) Uani 1 1 d . . . H12B H 0.1398 0.1505 0.3924 0.031 Uiso 1 1 calc R . . C13B C 0.28317(16) 0.50639(12) 0.59043(9) 0.0263(4) Uani 1 1 d . . . H13A H 0.3273 0.5105 0.5570 0.032 Uiso 1 1 calc R . . C13A C -0.02158(16) 0.09373(13) 0.37541(9) 0.0295(4) Uani 1 1 d . . . H13B H -0.0526 0.1343 0.4139 0.035 Uiso 1 1 calc R . . C14A C -0.07604(16) 0.01798(13) 0.32286(9) 0.0286(4) Uani 1 1 d . . . H14A H -0.1522 -0.0045 0.3177 0.034 Uiso 1 1 calc R . . C14B C 0.17863(16) 0.53495(12) 0.59589(9) 0.0278(4) Uani 1 1 d . . . H14B H 0.1357 0.5625 0.5669 0.033 Uiso 1 1 calc R . . C15B C 0.14537(15) 0.51678(12) 0.64959(8) 0.0249(4) Uani 1 1 d . . . H15A H 0.0738 0.5287 0.6639 0.030 Uiso 1 1 calc R . . C15A C -0.00276(15) -0.02023(12) 0.27887(9) 0.0244(3) Uani 1 1 d . . . H15B H -0.0201 -0.0739 0.2370 0.029 Uiso 1 1 calc R . . C16B C 0.13037(16) 0.26059(12) 0.56237(10) 0.0298(4) Uani 1 1 d . . . H16A H 0.1253 0.2307 0.5955 0.036 Uiso 1 1 calc R . . C16A C 0.00008(18) 0.18460(16) 0.22439(11) 0.0387(5) Uani 1 1 d . . . H16B H 0.0618 0.1820 0.2000 0.046 Uiso 1 1 calc R . . C17B C 0.22065(16) 0.26601(13) 0.53209(10) 0.0331(4) Uani 1 1 d . . . H17A H 0.2902 0.2396 0.5395 0.040 Uiso 1 1 calc R . . C17A C -0.00810(17) 0.24811(14) 0.28780(12) 0.0361(5) Uani 1 1 d . . . H17B H 0.0464 0.2985 0.3157 0.043 Uiso 1 1 calc R . . C18B C 0.19488(17) 0.31496(14) 0.48901(9) 0.0340(5) Uani 1 1 d . . . H18A H 0.2430 0.3285 0.4604 0.041 Uiso 1 1 calc R . . C18A C -0.10752(17) 0.22793(14) 0.30410(11) 0.0348(4) Uani 1 1 d . . . H18B H -0.1358 0.2620 0.3454 0.042 Uiso 1 1 calc R . . C19B C 0.08853(17) 0.33983(14) 0.49265(9) 0.0315(4) Uani 1 1 d . . . H19A H 0.0485 0.3743 0.4674 0.038 Uiso 1 1 calc R . . C19A C -0.16065(17) 0.15176(14) 0.25146(11) 0.0364(5) Uani 1 1 d . . . H19B H -0.2330 0.1229 0.2491 0.044 Uiso 1 1 calc R . . C20B C 0.04877(15) 0.30637(13) 0.53817(9) 0.0298(4) Uani 1 1 d . . . H20A H -0.0239 0.3142 0.5513 0.036 Uiso 1 1 calc R . . C20A C -0.09402(18) 0.12473(16) 0.20236(11) 0.0396(5) Uani 1 1 d . . . H20B H -0.1107 0.0729 0.1594 0.048 Uiso 1 1 calc R . . C21A C 0.44441(16) -0.11813(14) 0.28826(10) 0.0313(4) Uani 1 1 d . . . H21A H 0.4630 -0.1566 0.3146 0.047 Uiso 1 1 calc R . . H21B H 0.4989 -0.0670 0.2999 0.047 Uiso 1 1 calc R . . H21C H 0.4404 -0.1555 0.2419 0.047 Uiso 1 1 calc R . . C21B C 0.3052(2) 0.58568(17) 0.91790(9) 0.0431(5) Uani 1 1 d . . . H21D H 0.3325 0.6496 0.9425 0.065 Uiso 1 1 calc R . . H21E H 0.3573 0.5437 0.9259 0.065 Uiso 1 1 calc R . . H21F H 0.2381 0.5733 0.9320 0.065 Uiso 1 1 calc R . . C22A C 0.33639(16) -0.01601(13) 0.39229(9) 0.0278(4) Uani 1 1 d . . . H22A H 0.3684 -0.0583 0.4125 0.042 Uiso 1 1 calc R . . H22B H 0.2679 0.0006 0.4074 0.042 Uiso 1 1 calc R . . H22C H 0.3841 0.0398 0.4045 0.042 Uiso 1 1 calc R . . C22B C 0.4092(2) 0.60669(18) 0.81635(11) 0.0494(7) Uani 1 1 d . . . H22D H 0.4319 0.6681 0.8486 0.074 Uiso 1 1 calc R . . H22E H 0.4015 0.6096 0.7724 0.074 Uiso 1 1 calc R . . H22F H 0.4625 0.5634 0.8201 0.074 Uiso 1 1 calc R . . C23A C 0.23094(16) -0.17508(13) 0.29070(10) 0.0301(4) Uani 1 1 d . . . H23A H 0.2669 -0.2124 0.3139 0.045 Uiso 1 1 calc R . . H23B H 0.2165 -0.2112 0.2439 0.045 Uiso 1 1 calc R . . H23C H 0.1637 -0.1572 0.3072 0.045 Uiso 1 1 calc R . . C23B C 0.1986(2) 0.66025(16) 0.82803(12) 0.0546(7) Uani 1 1 d . . . H23D H 0.2312 0.7190 0.8600 0.082 Uiso 1 1 calc R . . H23E H 0.1281 0.6480 0.8382 0.082 Uiso 1 1 calc R . . H23F H 0.1912 0.6637 0.7842 0.082 Uiso 1 1 calc R . . C31B C 0.28366(13) 0.82751(11) 0.49013(8) 0.0194(3) Uani 1 1 d . . . C31A C 0.29253(14) 0.23676(12) -0.02448(8) 0.0216(3) Uani 1 1 d . . . C32B C 0.30763(15) 0.91327(12) 0.53967(8) 0.0242(3) Uani 1 1 d . . . C32A C 0.24773(14) 0.17639(12) -0.08589(8) 0.0234(3) Uani 1 1 d . . . C33B C 0.24777(16) 0.98870(12) 0.54741(9) 0.0278(4) Uani 1 1 d . . . C33A C 0.30561(16) 0.12336(12) -0.13272(9) 0.0273(4) Uani 1 1 d . . . C34B C 0.15789(15) 0.98241(12) 0.50319(9) 0.0259(4) Uani 1 1 d . . . C34A C 0.41440(16) 0.12817(13) -0.11963(9) 0.0282(4) Uani 1 1 d . . . C35B C 0.12929(14) 0.89970(12) 0.45330(8) 0.0219(3) Uani 1 1 d . . . C35A C 0.46402(15) 0.18652(14) -0.05986(9) 0.0282(4) Uani 1 1 d . . . C36B C 0.19122(13) 0.82567(11) 0.44834(8) 0.0183(3) Uani 1 1 d . . . C36A C 0.40317(14) 0.23775(12) -0.01467(8) 0.0245(3) Uani 1 1 d . . . C41B C 0.31863(13) 0.64989(11) 0.41971(8) 0.0202(3) Uani 1 1 d . . . C41A C 0.26603(14) 0.40557(12) 0.06919(8) 0.0218(3) Uani 1 1 d . . . C42B C 0.35171(15) 0.60733(13) 0.35947(9) 0.0249(4) Uani 1 1 d . . . C42A C 0.33356(14) 0.45572(12) 0.04682(8) 0.0235(3) Uani 1 1 d . . . C43B C 0.30857(17) 0.52313(13) 0.31443(9) 0.0291(4) Uani 1 1 d . . . C43A C 0.36626(15) 0.54800(13) 0.07897(9) 0.0261(4) Uani 1 1 d . . . C44B C 0.22671(17) 0.47754(12) 0.32796(9) 0.0312(4) Uani 1 1 d . . . C44A C 0.32794(15) 0.59643(12) 0.13560(9) 0.0273(4) Uani 1 1 d . . . C45B C 0.19002(15) 0.51578(12) 0.38686(9) 0.0270(4) Uani 1 1 d . . . C45A C 0.25645(15) 0.55225(13) 0.15851(8) 0.0259(4) Uani 1 1 d . . . C46B C 0.23630(14) 0.59918(12) 0.43055(8) 0.0212(3) Uani 1 1 d . . . C46A C 0.22769(14) 0.45944(13) 0.12558(8) 0.0234(3) Uani 1 1 d . . . C51B C 0.41026(13) 0.71693(12) 0.54053(8) 0.0206(3) Uani 1 1 d . . . C51A C 0.09876(14) 0.28946(12) 0.01193(8) 0.0234(3) Uani 1 1 d . . . C52B C 0.49130(14) 0.65699(12) 0.53630(8) 0.0225(3) Uani 1 1 d . . . C52A C 0.05967(15) 0.34290(14) -0.02407(9) 0.0267(4) Uani 1 1 d . . . C53B C 0.53223(14) 0.62619(12) 0.58532(9) 0.0248(3) Uani 1 1 d . . . C53A C -0.04647(16) 0.34955(15) -0.04302(9) 0.0319(4) Uani 1 1 d . . . C54B C 0.49157(14) 0.65409(12) 0.64334(9) 0.0240(3) Uani 1 1 d . . . C54A C -0.12173(15) 0.29867(14) -0.02776(9) 0.0314(4) Uani 1 1 d . . . C55B C 0.40966(14) 0.71135(12) 0.65010(8) 0.0233(3) Uani 1 1 d . . . C55A C -0.08867(16) 0.24337(14) 0.00685(10) 0.0325(4) Uani 1 1 d . . . C56B C 0.37032(14) 0.74040(12) 0.59950(8) 0.0222(3) Uani 1 1 d . . . C56A C 0.01901(16) 0.23975(13) 0.02584(9) 0.0287(4) Uani 1 1 d . . . C61B C 0.47313(15) 0.79442(14) 0.45817(10) 0.0292(4) Uani 1 1 d . . . H61A H 0.4994 0.8519 0.4940 0.044 Uiso 1 1 calc R . . H61B H 0.4515 0.8077 0.4182 0.044 Uiso 1 1 calc R . . H61C H 0.5298 0.7516 0.4511 0.044 Uiso 1 1 calc R . . C61A C 0.25691(16) 0.24771(14) 0.09270(9) 0.0291(4) Uani 1 1 d . . . H61D H 0.2350 0.1816 0.0744 0.044 Uiso 1 1 calc R . . H61E H 0.2191 0.2776 0.1297 0.044 Uiso 1 1 calc R . . H61F H 0.3338 0.2564 0.1076 0.044 Uiso 1 1 calc R . . Br1 Br 0.38888(13) 0.90320(6) 0.90121(5) 0.0976(4) Uani 0.50 1 d P . . C101 C 0.4839(6) 0.9793(4) 0.9778(3) 0.0556(15) Uani 0.50 1 d P . . C102 C 0.571(2) 0.9528(15) 0.9701(12) 0.129(8) Uani 0.50 1 d P . . C103 C 0.6572(6) 1.0172(8) 1.0315(6) 0.078(3) Uani 0.50 1 d P . . C105 C 0.5691(12) 0.9586(8) 0.9793(6) 0.047(2) Uani 0.50 1 d P . . C104 C 0.3545(4) 0.9270(5) 0.9311(3) 0.0362(11) Uani 0.50 1 d P . . C106 C 0.4776(7) 0.8983(4) 0.9157(3) 0.0509(14) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1A 0.02066(8) 0.01764(7) 0.01779(7) 0.00564(6) 0.00019(6) -0.00147(6) Zr1B 0.01986(8) 0.02063(8) 0.01766(7) 0.00525(6) 0.00343(6) -0.00033(6) Fe1B 0.01911(12) 0.01739(11) 0.01896(11) 0.00396(9) 0.00238(9) -0.00171(9) Fe1A 0.02281(13) 0.02014(11) 0.02438(12) 0.00530(9) 0.00398(10) 0.00239(9) P1A 0.0233(2) 0.0204(2) 0.0232(2) 0.00936(16) 0.00471(17) 0.00089(16) P1B 0.0377(3) 0.0282(2) 0.0172(2) 0.00412(17) 0.00028(19) -0.0050(2) F32B 0.0328(6) 0.0316(6) 0.0286(6) 0.0060(5) -0.0097(5) -0.0054(5) F32A 0.0214(6) 0.0425(7) 0.0313(6) -0.0026(5) -0.0018(5) -0.0014(5) F33B 0.0536(8) 0.0229(6) 0.0348(6) -0.0039(5) 0.0026(6) -0.0017(5) F33A 0.0441(8) 0.0394(7) 0.0268(6) -0.0071(5) 0.0027(5) -0.0016(6) F34B 0.0416(7) 0.0203(5) 0.0477(7) 0.0094(5) 0.0123(6) 0.0124(5) F34A 0.0409(7) 0.0421(7) 0.0364(6) 0.0048(5) 0.0195(6) 0.0110(6) F35B 0.0232(5) 0.0297(5) 0.0333(6) 0.0130(5) 0.0004(4) 0.0078(4) F35A 0.0202(6) 0.0527(8) 0.0473(7) 0.0075(6) 0.0084(5) 0.0070(5) F36B 0.0207(5) 0.0187(4) 0.0231(5) 0.0055(4) -0.0022(4) 0.0008(4) F36A 0.0224(6) 0.0426(7) 0.0267(5) 0.0012(5) -0.0033(4) 0.0033(5) F42B 0.0372(7) 0.0485(7) 0.0320(6) 0.0146(5) 0.0182(5) 0.0029(6) F42A 0.0371(7) 0.0315(6) 0.0259(5) 0.0076(4) 0.0134(5) 0.0003(5) F43B 0.0592(9) 0.0422(7) 0.0222(5) 0.0084(5) 0.0082(5) 0.0251(6) F43A 0.0336(7) 0.0346(6) 0.0380(6) 0.0133(5) 0.0058(5) -0.0064(5) F44B 0.0697(10) 0.0223(6) 0.0363(7) 0.0040(5) -0.0124(6) -0.0017(6) F44A 0.0457(7) 0.0241(5) 0.0360(6) 0.0032(5) 0.0000(5) 0.0007(5) F45B 0.0352(7) 0.0339(6) 0.0506(7) 0.0197(6) -0.0046(6) -0.0126(5) F45A 0.0434(7) 0.0340(6) 0.0266(6) 0.0041(5) 0.0121(5) 0.0137(5) F46B 0.0216(5) 0.0335(6) 0.0277(5) 0.0132(4) 0.0072(4) 0.0005(4) F46A 0.0316(6) 0.0356(6) 0.0288(5) 0.0115(5) 0.0142(5) 0.0060(5) F52B 0.0274(6) 0.0391(6) 0.0301(6) 0.0154(5) 0.0098(5) 0.0139(5) F52A 0.0275(6) 0.0606(8) 0.0404(7) 0.0352(6) -0.0002(5) 0.0000(6) F53B 0.0285(6) 0.0426(7) 0.0473(7) 0.0264(6) 0.0065(5) 0.0172(5) F53A 0.0337(7) 0.0784(10) 0.0531(8) 0.0404(8) -0.0026(6) 0.0149(7) F54B 0.0319(6) 0.0431(7) 0.0348(6) 0.0269(5) -0.0024(5) 0.0033(5) F54A 0.0195(6) 0.0565(8) 0.0382(7) 0.0017(6) 0.0005(5) 0.0063(5) F55B 0.0386(7) 0.0458(7) 0.0257(5) 0.0182(5) 0.0102(5) 0.0086(5) F55A 0.0320(7) 0.0548(8) 0.0576(9) 0.0162(7) 0.0112(6) -0.0132(6) F56B 0.0299(6) 0.0385(6) 0.0313(6) 0.0179(5) 0.0114(5) 0.0150(5) F56A 0.0383(8) 0.0525(8) 0.0686(9) 0.0407(7) 0.0065(7) -0.0028(6) B1B 0.0174(9) 0.0240(9) 0.0216(8) 0.0108(7) 0.0018(7) 0.0015(7) B1A 0.0204(9) 0.0275(9) 0.0185(8) 0.0094(7) 0.0035(7) 0.0042(7) C1A 0.0217(9) 0.0257(9) 0.0392(10) 0.0110(8) -0.0049(8) -0.0063(7) C1B 0.0439(14) 0.0690(17) 0.0303(11) 0.0204(11) 0.0023(9) 0.0291(12) C2A 0.0286(10) 0.0215(8) 0.0262(8) 0.0065(7) -0.0050(7) -0.0089(7) C2B 0.0264(10) 0.0526(13) 0.0383(11) 0.0186(10) 0.0061(8) 0.0180(9) C3A 0.0306(10) 0.0164(8) 0.0387(10) 0.0078(7) -0.0035(8) -0.0051(7) C3B 0.0441(13) 0.0418(12) 0.0348(11) 0.0132(9) 0.0127(9) 0.0236(10) C4A 0.0457(13) 0.0293(10) 0.0349(10) 0.0196(8) -0.0085(9) -0.0136(9) C4B 0.0637(18) 0.0288(11) 0.0755(19) 0.0204(12) 0.0214(14) 0.0173(11) C5A 0.0313(11) 0.0354(10) 0.0369(11) 0.0097(9) 0.0062(8) -0.0138(8) C5B 0.0739(19) 0.0689(18) 0.0615(16) 0.0510(15) 0.0350(15) 0.0429(16) C6A 0.0333(10) 0.0270(9) 0.0222(8) 0.0001(7) 0.0028(7) 0.0058(8) C6B 0.0250(10) 0.0633(15) 0.0227(9) 0.0062(9) 0.0091(8) -0.0032(9) C7A 0.0323(10) 0.0237(8) 0.0204(8) -0.0021(7) 0.0020(7) -0.0045(7) C7B 0.0191(9) 0.0534(13) 0.0306(10) 0.0077(9) 0.0076(8) 0.0064(9) C8A 0.0261(10) 0.0335(10) 0.0199(8) -0.0009(7) -0.0028(7) 0.0023(8) C8B 0.0194(9) 0.0572(13) 0.0257(9) 0.0095(9) 0.0025(7) -0.0077(9) C9A 0.0382(11) 0.0355(10) 0.0187(8) 0.0079(7) -0.0009(7) 0.0017(8) C9B 0.0339(12) 0.0504(13) 0.0337(10) 0.0089(10) 0.0058(9) -0.0209(10) C10A 0.0320(11) 0.0397(11) 0.0215(8) 0.0055(8) 0.0071(7) 0.0001(8) C10B 0.0338(12) 0.0624(15) 0.0325(10) 0.0198(10) 0.0077(9) -0.0148(10) C11A 0.0233(9) 0.0189(7) 0.0220(8) 0.0057(6) 0.0015(6) 0.0009(6) C11B 0.0243(9) 0.0210(8) 0.0172(7) 0.0036(6) 0.0015(6) 0.0007(6) C12B 0.0249(9) 0.0235(8) 0.0203(8) 0.0057(6) 0.0011(6) -0.0049(7) C12A 0.0282(10) 0.0244(8) 0.0209(8) 0.0040(7) 0.0014(7) -0.0010(7) C13B 0.0321(10) 0.0224(8) 0.0219(8) 0.0063(7) 0.0020(7) -0.0098(7) C13A 0.0333(10) 0.0296(9) 0.0239(8) 0.0059(7) 0.0084(7) 0.0024(8) C14A 0.0266(10) 0.0281(9) 0.0319(9) 0.0104(8) 0.0081(8) -0.0005(7) C14B 0.0395(11) 0.0202(8) 0.0225(8) 0.0079(7) -0.0001(7) 0.0009(7) C15B 0.0299(10) 0.0218(8) 0.0212(8) 0.0053(6) 0.0031(7) 0.0054(7) C15A 0.0249(9) 0.0200(8) 0.0252(8) 0.0045(6) 0.0037(7) -0.0009(6) C16B 0.0346(11) 0.0182(8) 0.0311(9) 0.0034(7) 0.0013(8) -0.0052(7) C16A 0.0382(12) 0.0446(12) 0.0465(12) 0.0292(10) 0.0136(10) 0.0160(10) C17B 0.0279(10) 0.0233(9) 0.0361(10) -0.0042(8) 0.0030(8) 0.0012(7) C17A 0.0321(11) 0.0255(9) 0.0537(13) 0.0173(9) 0.0066(9) 0.0043(8) C18B 0.0358(11) 0.0323(10) 0.0230(9) -0.0044(7) 0.0085(8) -0.0104(8) C18A 0.0317(11) 0.0256(9) 0.0472(12) 0.0113(9) 0.0094(9) 0.0086(8) C19B 0.0330(11) 0.0312(10) 0.0235(9) 0.0040(7) -0.0029(7) -0.0053(8) C19A 0.0258(10) 0.0320(10) 0.0489(12) 0.0125(9) 0.0009(9) 0.0072(8) C20B 0.0217(9) 0.0304(9) 0.0302(9) 0.0032(7) 0.0016(7) -0.0071(7) C20A 0.0403(12) 0.0423(12) 0.0349(11) 0.0135(9) -0.0013(9) 0.0167(10) C21A 0.0279(10) 0.0329(10) 0.0369(10) 0.0158(8) 0.0080(8) 0.0071(8) C21B 0.0547(15) 0.0496(13) 0.0179(9) 0.0050(9) 0.0027(9) -0.0114(11) C22A 0.0335(10) 0.0284(9) 0.0237(8) 0.0127(7) 0.0021(7) 0.0012(8) C22B 0.0590(16) 0.0548(14) 0.0256(10) 0.0074(10) 0.0006(10) -0.0312(12) C23A 0.0340(11) 0.0218(8) 0.0364(10) 0.0112(7) 0.0098(8) -0.0013(7) C23B 0.083(2) 0.0269(11) 0.0420(13) 0.0008(9) -0.0011(13) 0.0101(12) C31B 0.0193(8) 0.0199(7) 0.0203(7) 0.0091(6) 0.0020(6) -0.0005(6) C31A 0.0215(8) 0.0229(8) 0.0209(8) 0.0085(6) 0.0030(6) 0.0020(6) C32B 0.0237(9) 0.0252(8) 0.0226(8) 0.0089(7) -0.0018(7) -0.0030(7) C32A 0.0205(8) 0.0248(8) 0.0234(8) 0.0074(7) 0.0015(6) 0.0001(6) C33B 0.0349(10) 0.0187(8) 0.0255(8) 0.0026(7) 0.0054(7) -0.0032(7) C33A 0.0332(10) 0.0236(8) 0.0209(8) 0.0032(7) 0.0029(7) -0.0010(7) C34B 0.0296(10) 0.0197(8) 0.0317(9) 0.0103(7) 0.0114(7) 0.0067(7) C34A 0.0323(10) 0.0257(9) 0.0285(9) 0.0080(7) 0.0141(8) 0.0069(7) C35B 0.0198(8) 0.0229(8) 0.0254(8) 0.0112(7) 0.0041(6) 0.0025(6) C35A 0.0202(9) 0.0334(9) 0.0324(9) 0.0120(8) 0.0067(7) 0.0045(7) C36B 0.0190(8) 0.0173(7) 0.0189(7) 0.0065(6) 0.0040(6) 0.0002(6) C36A 0.0225(9) 0.0271(8) 0.0219(8) 0.0069(7) 0.0011(7) 0.0023(7) C41B 0.0190(8) 0.0216(7) 0.0225(8) 0.0111(6) 0.0026(6) 0.0049(6) C41A 0.0205(8) 0.0263(8) 0.0192(7) 0.0089(6) 0.0014(6) 0.0059(6) C42B 0.0246(9) 0.0290(9) 0.0245(8) 0.0124(7) 0.0061(7) 0.0088(7) C42A 0.0233(9) 0.0278(8) 0.0190(7) 0.0070(6) 0.0047(6) 0.0055(7) C43B 0.0381(11) 0.0291(9) 0.0198(8) 0.0085(7) 0.0016(7) 0.0159(8) C43A 0.0234(9) 0.0293(9) 0.0270(9) 0.0124(7) 0.0015(7) 0.0016(7) C44B 0.0406(12) 0.0204(8) 0.0281(9) 0.0078(7) -0.0099(8) 0.0044(8) C44A 0.0286(10) 0.0239(8) 0.0253(8) 0.0063(7) -0.0043(7) 0.0042(7) C45B 0.0251(9) 0.0235(8) 0.0338(9) 0.0151(7) -0.0047(7) -0.0001(7) C45A 0.0281(9) 0.0280(9) 0.0194(8) 0.0055(7) 0.0020(7) 0.0095(7) C46B 0.0184(8) 0.0243(8) 0.0229(8) 0.0113(6) 0.0012(6) 0.0047(6) C46A 0.0216(9) 0.0301(9) 0.0206(8) 0.0111(7) 0.0033(6) 0.0062(7) C51B 0.0161(8) 0.0231(8) 0.0235(8) 0.0105(6) -0.0004(6) -0.0004(6) C51A 0.0227(9) 0.0277(8) 0.0189(7) 0.0066(6) 0.0045(6) 0.0029(7) C52B 0.0191(8) 0.0256(8) 0.0240(8) 0.0106(7) 0.0021(6) 0.0017(6) C52A 0.0221(9) 0.0362(10) 0.0213(8) 0.0097(7) 0.0024(7) 0.0035(7) C53B 0.0184(8) 0.0252(8) 0.0334(9) 0.0149(7) -0.0004(7) 0.0027(6) C53A 0.0275(10) 0.0423(11) 0.0237(9) 0.0099(8) -0.0003(7) 0.0090(8) C54B 0.0200(8) 0.0270(8) 0.0276(8) 0.0163(7) -0.0051(7) -0.0039(7) C54A 0.0204(9) 0.0404(11) 0.0228(8) -0.0019(8) 0.0015(7) 0.0054(8) C55B 0.0229(9) 0.0259(8) 0.0220(8) 0.0104(7) 0.0023(6) -0.0022(7) C55A 0.0264(10) 0.0345(10) 0.0295(9) 0.0010(8) 0.0091(8) -0.0043(8) C56B 0.0181(8) 0.0242(8) 0.0256(8) 0.0112(7) 0.0009(6) 0.0018(6) C56A 0.0283(10) 0.0288(9) 0.0292(9) 0.0096(7) 0.0061(7) 0.0017(7) C61B 0.0221(9) 0.0331(10) 0.0365(10) 0.0177(8) 0.0036(8) -0.0014(7) C61A 0.0316(10) 0.0344(10) 0.0269(9) 0.0166(8) 0.0067(8) 0.0093(8) Br1 0.1517(12) 0.0523(5) 0.0867(7) 0.0314(5) -0.0062(7) -0.0123(6) C101 0.078(5) 0.040(3) 0.066(4) 0.037(3) 0.019(4) 0.010(3) C102 0.183(17) 0.115(13) 0.185(17) 0.128(13) 0.141(14) 0.097(12) C103 0.058(4) 0.104(7) 0.122(8) 0.094(6) 0.036(5) 0.034(5) C105 0.070(6) 0.035(4) 0.045(3) 0.021(3) 0.019(4) 0.023(4) C104 0.023(2) 0.045(3) 0.044(3) 0.026(3) -0.009(2) -0.011(2) C106 0.085(5) 0.033(2) 0.039(3) 0.011(2) 0.028(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1A C11A 2.2397(18) . ? Zr1A C4A 2.4907(19) . ? Zr1A C9A 2.4918(18) . ? Zr1A C10A 2.5066(19) . ? Zr1A C5A 2.516(2) . ? Zr1A C8A 2.5158(18) . ? Zr1A C7A 2.5164(17) . ? Zr1A C6A 2.5167(18) . ? Zr1A C3A 2.5184(18) . ? Zr1A C2A 2.5294(17) . ? Zr1A C1A 2.5345(18) . ? Zr1A P1A 2.7118(5) . ? Zr1B C11B 2.2398(18) . ? Zr1B C4B 2.480(2) . ? Zr1B C9B 2.480(2) . ? Zr1B C5B 2.502(2) . ? Zr1B C3B 2.509(2) . ? Zr1B C10B 2.512(2) . ? Zr1B C8B 2.514(2) . ? Zr1B C2B 2.526(2) . ? Zr1B C1B 2.527(2) . ? Zr1B C6B 2.530(2) . ? Zr1B C7B 2.535(2) . ? Zr1B P1B 2.6992(5) . ? Fe1B C18B 2.0337(18) . ? Fe1B C12B 2.0391(18) . ? Fe1B C13B 2.0465(18) . ? Fe1B C15B 2.0465(17) . ? Fe1B C19B 2.0502(19) . ? Fe1B C17B 2.0513(19) . ? Fe1B C14B 2.0535(18) . ? Fe1B C20B 2.0692(19) . ? Fe1B C16B 2.0748(18) . ? Fe1B C11B 2.0804(16) . ? Fe1A C15A 2.0475(18) . ? Fe1A C12A 2.0488(18) . ? Fe1A C19A 2.052(2) . ? Fe1A C18A 2.0539(19) . ? Fe1A C14A 2.0583(19) . ? Fe1A C13A 2.0612(19) . ? Fe1A C20A 2.066(2) . ? Fe1A C17A 2.070(2) . ? Fe1A C11A 2.0822(17) . ? Fe1A C16A 2.086(2) . ? P1A C23A 1.8180(19) . ? P1A C22A 1.8193(18) . ? P1A C21A 1.824(2) . ? P1B C22B 1.816(2) . ? P1B C23B 1.820(3) . ? P1B C21B 1.820(2) . ? F32B C32B 1.361(2) . ? F32A C32A 1.361(2) . ? F33B C33B 1.349(2) . ? F33A C33A 1.347(2) . ? F34B C34B 1.338(2) . ? F34A C34A 1.347(2) . ? F35B C35B 1.346(2) . ? F35A C35A 1.344(2) . ? F36B C36B 1.3553(18) . ? F36A C36A 1.353(2) . ? F42B C42B 1.353(2) . ? F42A C42A 1.3558(19) . ? F43B C43B 1.345(2) . ? F43A C43A 1.349(2) . ? F44B C44B 1.347(2) . ? F44A C44A 1.346(2) . ? F45B C45B 1.351(2) . ? F45A C45A 1.346(2) . ? F46B C46B 1.356(2) . ? F46A C46A 1.353(2) . ? F52B C52B 1.361(2) . ? F52A C52A 1.358(2) . ? F53B C53B 1.350(2) . ? F53A C53A 1.351(2) . ? F54B C54B 1.3424(19) . ? F54A C54A 1.342(2) . ? F55B C55B 1.350(2) . ? F55A C55A 1.350(2) . ? F56B C56B 1.353(2) . ? F56A C56A 1.353(2) . ? B1B C61B 1.642(3) . ? B1B C41B 1.651(3) . ? B1B C31B 1.653(2) . ? B1B C51B 1.658(2) . ? B1A C61A 1.639(3) . ? B1A C51A 1.656(3) . ? B1A C31A 1.660(3) . ? B1A C41A 1.660(3) . ? C1A C5A 1.399(3) . ? C1A C2A 1.409(3) . ? C1B C5B 1.393(4) . ? C1B C2B 1.401(3) . ? C2A C3A 1.403(3) . ? C2B C3B 1.394(3) . ? C3A C4A 1.414(3) . ? C3B C4B 1.409(4) . ? C4A C5A 1.411(3) . ? C4B C5B 1.411(4) . ? C6A C10A 1.402(3) . ? C6A C7A 1.414(3) . ? C6B C10B 1.395(4) . ? C6B C7B 1.421(3) . ? C7A C8A 1.397(3) . ? C7B C8B 1.402(3) . ? C8A C9A 1.411(3) . ? C8B C9B 1.413(3) . ? C9A C10A 1.414(3) . ? C9B C10B 1.420(3) . ? C11A C12A 1.452(2) . ? C11A C15A 1.452(2) . ? C11B C15B 1.450(2) . ? C11B C12B 1.452(3) . ? C12B C13B 1.423(3) . ? C12A C13A 1.413(3) . ? C13B C14B 1.416(3) . ? C13A C14A 1.419(3) . ? C14A C15A 1.421(3) . ? C14B C15B 1.420(3) . ? C16B C17B 1.414(3) . ? C16B C20B 1.420(3) . ? C16A C20A 1.418(3) . ? C16A C17A 1.423(3) . ? C17B C18B 1.420(3) . ? C17A C18A 1.414(3) . ? C18B C19B 1.418(3) . ? C18A C19A 1.417(3) . ? C19B C20B 1.419(3) . ? C19A C20A 1.416(3) . ? C31B C36B 1.389(2) . ? C31B C32B 1.394(2) . ? C31A C32A 1.391(2) . ? C31A C36A 1.393(2) . ? C32B C33B 1.381(3) . ? C32A C33A 1.385(3) . ? C33B C34B 1.381(3) . ? C33A C34A 1.370(3) . ? C34B C35B 1.373(2) . ? C34A C35A 1.374(3) . ? C35B C36B 1.386(2) . ? C35A C36A 1.378(3) . ? C41B C46B 1.387(2) . ? C41B C42B 1.389(2) . ? C41A C42A 1.388(3) . ? C41A C46A 1.392(2) . ? C42B C43B 1.385(3) . ? C42A C43A 1.383(3) . ? C43B C44B 1.364(3) . ? C43A C44A 1.373(3) . ? C44B C45B 1.376(3) . ? C44A C45A 1.370(3) . ? C45B C46B 1.379(3) . ? C45A C46A 1.383(3) . ? C51B C56B 1.391(2) . ? C51B C52B 1.392(2) . ? C51A C56A 1.386(3) . ? C51A C52A 1.391(3) . ? C52B C53B 1.375(2) . ? C52A C53A 1.376(3) . ? C53B C54B 1.375(3) . ? C53A C54A 1.371(3) . ? C54B C55B 1.372(3) . ? C54A C55A 1.371(3) . ? C55B C56B 1.383(2) . ? C55A C56A 1.386(3) . ? Br1 C104 0.822(7) . ? Br1 C106 1.143(8) . ? Br1 C103 1.747(12) 2_677 ? Br1 C101 1.932(6) . ? C101 C101 0.993(12) 2_677 ? C101 C105 1.135(16) . ? C101 C102 1.20(3) . ? C101 C105 1.355(15) 2_677 ? C101 C106 1.495(8) . ? C101 C102 1.52(2) 2_677 ? C101 C103 1.781(10) 2_677 ? C101 C104 1.828(8) . ? C102 C101 1.52(2) 2_677 ? C102 C106 1.56(3) . ? C102 C103 1.63(3) . ? C103 C104 0.996(11) 2_677 ? C103 C105 1.52(2) . ? C103 Br1 1.747(12) 2_677 ? C103 C101 1.781(10) 2_677 ? C105 C101 1.355(15) 2_677 ? C105 C106 1.677(15) . ? C104 C103 0.996(11) 2_677 ? C104 C106 1.681(9) . ? 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 C11A Zr1A C4A 120.90(7) . . ? C11A Zr1A C9A 118.22(7) . . ? C4A Zr1A C9A 84.86(7) . . ? C11A Zr1A C10A 139.46(7) . . ? C4A Zr1A C10A 90.09(7) . . ? C9A Zr1A C10A 32.86(7) . . ? C11A Zr1A C5A 141.75(7) . . ? C4A Zr1A C5A 32.74(7) . . ? C9A Zr1A C5A 91.28(7) . . ? C10A Zr1A C5A 78.37(7) . . ? C11A Zr1A C8A 88.21(6) . . ? C4A Zr1A C8A 112.47(7) . . ? C9A Zr1A C8A 32.73(7) . . ? C10A Zr1A C8A 53.90(7) . . ? C5A Zr1A C8A 124.00(7) . . ? C11A Zr1A C7A 86.79(6) . . ? C4A Zr1A C7A 138.71(7) . . ? C9A Zr1A C7A 54.08(7) . . ? C10A Zr1A C7A 53.83(7) . . ? C5A Zr1A C7A 131.42(7) . . ? C8A Zr1A C7A 32.23(6) . . ? C11A Zr1A C6A 115.69(6) . . ? C4A Zr1A C6A 121.16(7) . . ? C9A Zr1A C6A 54.23(7) . . ? C10A Zr1A C6A 32.42(7) . . ? C5A Zr1A C6A 101.02(7) . . ? C8A Zr1A C6A 53.80(6) . . ? C7A Zr1A C6A 32.62(7) . . ? C11A Zr1A C3A 90.80(6) . . ? C4A Zr1A C3A 32.78(7) . . ? C9A Zr1A C3A 111.77(7) . . ? C10A Zr1A C3A 122.85(7) . . ? C5A Zr1A C3A 53.88(7) . . ? C8A Zr1A C3A 128.95(6) . . ? C7A Zr1A C3A 161.04(6) . . ? C6A Zr1A C3A 153.34(7) . . ? C11A Zr1A C2A 89.07(6) . . ? C4A Zr1A C2A 53.93(6) . . ? C9A Zr1A C2A 138.72(7) . . ? C10A Zr1A C2A 131.47(7) . . ? C5A Zr1A C2A 53.56(7) . . ? C8A Zr1A C2A 160.98(6) . . ? C7A Zr1A C2A 165.97(6) . . ? C6A Zr1A C2A 142.63(6) . . ? C3A Zr1A C2A 32.27(6) . . ? C11A Zr1A C1A 117.27(7) . . ? C4A Zr1A C1A 53.87(7) . . ? C9A Zr1A C1A 122.43(7) . . ? C10A Zr1A C1A 101.80(7) . . ? C5A Zr1A C1A 32.17(7) . . ? C8A Zr1A C1A 154.42(7) . . ? C7A Zr1A C1A 142.70(6) . . ? C6A Zr1A C1A 111.29(7) . . ? C3A Zr1A C1A 53.59(6) . . ? C2A Zr1A C1A 32.32(6) . . ? C11A Zr1A P1A 79.96(4) . . ? C4A Zr1A P1A 127.60(5) . . ? C9A Zr1A P1A 130.03(5) . . ? C10A Zr1A P1A 102.36(5) . . ? C5A Zr1A P1A 100.05(5) . . ? C8A Zr1A P1A 115.88(5) . . ? C7A Zr1A P1A 83.98(5) . . ? C6A Zr1A P1A 75.81(5) . . ? C3A Zr1A P1A 114.12(5) . . ? C2A Zr1A P1A 82.10(4) . . ? C1A Zr1A P1A 73.74(5) . . ? C11B Zr1B C4B 121.34(8) . . ? C11B Zr1B C9B 117.38(7) . . ? C4B Zr1B C9B 84.32(9) . . ? C11B Zr1B C5B 141.02(8) . . ? C4B Zr1B C5B 32.91(9) . . ? C9B Zr1B C5B 92.76(10) . . ? C11B Zr1B C3B 90.79(7) . . ? C4B Zr1B C3B 32.80(8) . . ? C9B Zr1B C3B 110.14(9) . . ? C5B Zr1B C3B 53.96(8) . . ? C11B Zr1B C10B 140.68(8) . . ? C4B Zr1B C10B 87.54(9) . . ? C9B Zr1B C10B 33.04(7) . . ? C5B Zr1B C10B 77.75(9) . . ? C3B Zr1B C10B 120.22(9) . . ? C11B Zr1B C8B 88.10(7) . . ? C4B Zr1B C8B 113.17(9) . . ? C9B Zr1B C8B 32.86(8) . . ? C5B Zr1B C8B 125.53(9) . . ? C3B Zr1B C8B 128.76(8) . . ? C10B Zr1B C8B 54.21(7) . . ? C11B Zr1B C2B 88.07(7) . . ? C4B Zr1B C2B 53.85(9) . . ? C9B Zr1B C2B 138.17(9) . . ? C5B Zr1B C2B 53.47(9) . . ? C3B Zr1B C2B 32.15(8) . . ? C10B Zr1B C2B 131.15(8) . . ? C8B Zr1B C2B 160.42(7) . . ? C11B Zr1B C1B 115.66(8) . . ? C4B Zr1B C1B 53.92(9) . . ? C9B Zr1B C1B 124.34(9) . . ? C5B Zr1B C1B 32.15(10) . . ? C3B Zr1B C1B 53.50(7) . . ? C10B Zr1B C1B 102.75(8) . . ? C8B Zr1B C1B 156.16(9) . . ? C2B Zr1B C1B 32.20(7) . . ? C11B Zr1B C6B 118.46(7) . . ? C4B Zr1B C6B 117.91(9) . . ? C9B Zr1B C6B 54.00(8) . . ? C5B Zr1B C6B 98.88(8) . . ? C3B Zr1B C6B 150.37(8) . . ? C10B Zr1B C6B 32.13(8) . . ? C8B Zr1B C6B 53.77(7) . . ? C2B Zr1B C6B 142.95(7) . . ? C1B Zr1B C6B 111.16(7) . . ? C11B Zr1B C7B 88.80(7) . . ? C4B Zr1B C7B 137.58(9) . . ? C9B Zr1B C7B 54.03(8) . . ? C5B Zr1B C7B 130.05(8) . . ? C3B Zr1B C7B 160.99(8) . . ? C10B Zr1B C7B 53.82(8) . . ? C8B Zr1B C7B 32.24(7) . . ? C2B Zr1B C7B 166.60(8) . . ? C1B Zr1B C7B 142.00(7) . . ? C6B Zr1B C7B 32.60(7) . . ? C11B Zr1B P1B 77.68(4) . . ? C4B Zr1B P1B 129.33(7) . . ? C9B Zr1B P1B 131.46(6) . . ? C5B Zr1B P1B 101.35(8) . . ? C3B Zr1B P1B 115.74(6) . . ? C10B Zr1B P1B 105.56(6) . . ? C8B Zr1B P1B 113.97(5) . . ? C2B Zr1B P1B 83.89(6) . . ? C1B Zr1B P1B 75.42(7) . . ? C6B Zr1B P1B 77.88(6) . . ? C7B Zr1B P1B 82.72(5) . . ? C18B Fe1B C12B 118.73(8) . . ? C18B Fe1B C13B 99.26(8) . . ? C12B Fe1B C13B 40.76(7) . . ? C18B Fe1B C15B 152.67(8) . . ? C12B Fe1B C15B 68.08(7) . . ? C13B Fe1B C15B 68.09(8) . . ? C18B Fe1B C19B 40.62(8) . . ? C12B Fe1B C19B 152.24(8) . . ? C13B Fe1B C19B 114.72(8) . . ? C15B Fe1B C19B 121.05(8) . . ? C18B Fe1B C17B 40.67(9) . . ? C12B Fe1B C17B 108.77(8) . . ? C13B Fe1B C17B 118.74(8) . . ? C15B Fe1B C17B 166.53(8) . . ? C19B Fe1B C17B 68.15(8) . . ? C18B Fe1B C14B 114.45(8) . . ? C12B Fe1B C14B 68.21(8) . . ? C13B Fe1B C14B 40.40(8) . . ? C15B Fe1B C14B 40.53(7) . . ? C19B Fe1B C14B 101.06(8) . . ? C17B Fe1B C14B 151.88(8) . . ? C18B Fe1B C20B 67.87(8) . . ? C12B Fe1B C20B 166.25(8) . . ? C13B Fe1B C20B 152.92(8) . . ? C15B Fe1B C20B 112.15(8) . . ? C19B Fe1B C20B 40.28(8) . . ? C17B Fe1B C20B 67.60(8) . . ? C14B Fe1B C20B 121.56(8) . . ? C18B Fe1B C16B 67.82(8) . . ? C12B Fe1B C16B 128.77(8) . . ? C13B Fe1B C16B 157.97(8) . . ? C15B Fe1B C16B 131.06(8) . . ? C19B Fe1B C16B 67.72(8) . . ? C17B Fe1B C16B 40.09(8) . . ? C14B Fe1B C16B 160.83(8) . . ? C20B Fe1B C16B 40.07(8) . . ? C18B Fe1B C11B 158.56(8) . . ? C12B Fe1B C11B 41.26(7) . . ? C13B Fe1B C11B 69.59(7) . . ? C15B Fe1B C11B 41.11(7) . . ? C19B Fe1B C11B 160.59(8) . . ? C17B Fe1B C11B 127.91(8) . . ? C14B Fe1B C11B 69.44(7) . . ? C20B Fe1B C11B 129.70(8) . . ? C16B Fe1B C11B 115.99(7) . . ? C15A Fe1A C12A 67.72(7) . . ? C15A Fe1A C19A 119.43(8) . . ? C12A Fe1A C19A 152.03(8) . . ? C15A Fe1A C18A 151.47(8) . . ? C12A Fe1A C18A 120.07(8) . . ? C19A Fe1A C18A 40.39(8) . . ? C15A Fe1A C14A 40.50(7) . . ? C12A Fe1A C14A 67.71(8) . . ? C19A Fe1A C14A 99.61(9) . . ? C18A Fe1A C14A 113.72(8) . . ? C15A Fe1A C13A 67.85(7) . . ? C12A Fe1A C13A 40.21(8) . . ? C19A Fe1A C13A 114.27(9) . . ? C18A Fe1A C13A 99.84(8) . . ? C14A Fe1A C13A 40.30(8) . . ? C15A Fe1A C20A 110.86(8) . . ? C12A Fe1A C20A 167.36(9) . . ? C19A Fe1A C20A 40.21(9) . . ? C18A Fe1A C20A 67.59(9) . . ? C14A Fe1A C20A 120.02(9) . . ? C13A Fe1A C20A 152.03(9) . . ? C15A Fe1A C17A 167.95(8) . . ? C12A Fe1A C17A 111.10(8) . . ? C19A Fe1A C17A 67.63(9) . . ? C18A Fe1A C17A 40.09(8) . . ? C14A Fe1A C17A 151.20(8) . . ? C13A Fe1A C17A 119.61(9) . . ? C20A Fe1A C17A 67.46(9) . . ? C15A Fe1A C11A 41.16(7) . . ? C12A Fe1A C11A 41.13(7) . . ? C19A Fe1A C11A 159.23(8) . . ? C18A Fe1A C11A 159.95(8) . . ? C14A Fe1A C11A 69.41(7) . . ? C13A Fe1A C11A 69.28(7) . . ? C20A Fe1A C11A 129.45(8) . . ? C17A Fe1A C11A 129.99(8) . . ? C15A Fe1A C16A 131.10(8) . . ? C12A Fe1A C16A 130.95(9) . . ? C19A Fe1A C16A 67.32(9) . . ? C18A Fe1A C16A 67.25(9) . . ? C14A Fe1A C16A 159.43(9) . . ? C13A Fe1A C16A 158.99(9) . . ? C20A Fe1A C16A 39.94(10) . . ? C17A Fe1A C16A 40.05(9) . . ? C11A Fe1A C16A 117.30(8) . . ? C23A P1A C22A 103.33(9) . . ? C23A P1A C21A 102.72(9) . . ? C22A P1A C21A 102.30(9) . . ? C23A P1A Zr1A 113.16(7) . . ? C22A P1A Zr1A 112.01(6) . . ? C21A P1A Zr1A 121.30(7) . . ? C22B P1B C23B 102.53(14) . . ? C22B P1B C21B 103.22(11) . . ? C23B P1B C21B 102.59(12) . . ? C22B P1B Zr1B 113.76(8) . . ? C23B P1B Zr1B 114.40(9) . . ? C21B P1B Zr1B 118.40(8) . . ? C61B B1B C41B 114.07(15) . . ? C61B B1B C31B 104.58(14) . . ? C41B B1B C31B 111.45(13) . . ? C61B B1B C51B 109.03(14) . . ? C41B B1B C51B 103.64(13) . . ? C31B B1B C51B 114.33(14) . . ? C61A B1A C51A 113.17(15) . . ? C61A B1A C31A 105.78(14) . . ? C51A B1A C31A 111.58(14) . . ? C61A B1A C41A 108.20(14) . . ? C51A B1A C41A 104.83(14) . . ? C31A B1A C41A 113.41(14) . . ? C5A C1A C2A 108.05(18) . . ? C5A C1A Zr1A 73.18(11) . . ? C2A C1A Zr1A 73.64(10) . . ? C5B C1B C2B 108.1(2) . . ? C5B C1B Zr1B 72.93(14) . . ? C2B C1B Zr1B 73.85(12) . . ? C3A C2A C1A 108.18(18) . . ? C3A C2A Zr1A 73.43(10) . . ? C1A C2A Zr1A 74.04(10) . . ? C3B C2B C1B 108.4(2) . . ? C3B C2B Zr1B 73.25(12) . . ? C1B C2B Zr1B 73.95(13) . . ? C2A C3A C4A 107.87(18) . . ? C2A C3A Zr1A 74.29(10) . . ? C4A C3A Zr1A 72.54(11) . . ? C2B C3B C4B 108.0(2) . . ? C2B C3B Zr1B 74.60(12) . . ? C4B C3B Zr1B 72.47(12) . . ? C5A C4A C3A 107.68(18) . . ? C5A C4A Zr1A 74.60(11) . . ? C3A C4A Zr1A 74.69(11) . . ? C3B C4B C5B 107.4(2) . . ? C3B C4B Zr1B 74.73(12) . . ? C5B C4B Zr1B 74.41(13) . . ? C1A C5A C4A 108.19(19) . . ? C1A C5A Zr1A 74.65(11) . . ? C4A C5A Zr1A 72.65(11) . . ? C1B C5B C4B 108.1(2) . . ? C1B C5B Zr1B 74.92(13) . . ? C4B C5B Zr1B 72.68(13) . . ? C10A C6A C7A 107.70(18) . . ? C10A C6A Zr1A 73.39(11) . . ? C7A C6A Zr1A 73.68(10) . . ? C10B C6B C7B 108.38(19) . . ? C10B C6B Zr1B 73.24(12) . . ? C7B C6B Zr1B 73.88(11) . . ? C8A C7A C6A 108.20(18) . . ? C8A C7A Zr1A 73.86(10) . . ? C6A C7A Zr1A 73.70(10) . . ? C8B C7B C6B 107.8(2) . . ? C8B C7B Zr1B 73.07(12) . . ? C6B C7B Zr1B 73.52(12) . . ? C7A C8A C9A 108.35(18) . . ? C7A C8A Zr1A 73.91(10) . . ? C9A C8A Zr1A 72.70(10) . . ? C7B C8B C9B 108.09(19) . . ? C7B C8B Zr1B 74.70(11) . . ? C9B C8B Zr1B 72.27(12) . . ? C8A C9A C10A 107.39(18) . . ? C8A C9A Zr1A 74.57(11) . . ? C10A C9A Zr1A 74.15(11) . . ? C8B C9B C10B 107.9(2) . . ? C8B C9B Zr1B 74.88(12) . . ? C10B C9B Zr1B 74.72(12) . . ? C6A C10A C9A 108.33(18) . . ? C6A C10A Zr1A 74.19(11) . . ? C9A C10A Zr1A 73.00(11) . . ? C6B C10B C9B 107.8(2) . . ? C6B C10B Zr1B 74.63(12) . . ? C9B C10B Zr1B 72.24(12) . . ? C12A C11A C15A 103.64(15) . . ? C12A C11A Fe1A 68.20(10) . . ? C15A C11A Fe1A 68.14(10) . . ? C12A C11A Zr1A 125.39(13) . . ? C15A C11A Zr1A 126.52(12) . . ? Fe1A C11A Zr1A 108.77(7) . . ? C15B C11B C12B 104.03(15) . . ? C15B C11B Fe1B 68.19(9) . . ? C12B C11B Fe1B 67.84(9) . . ? C15B C11B Zr1B 125.23(13) . . ? C12B C11B Zr1B 127.82(13) . . ? Fe1B C11B Zr1B 112.73(8) . . ? C13B C12B C11B 110.01(16) . . ? C13B C12B Fe1B 69.90(10) . . ? C11B C12B Fe1B 70.90(10) . . ? C13A C12A C11A 110.61(16) . . ? C13A C12A Fe1A 70.37(11) . . ? C11A C12A Fe1A 70.66(10) . . ? C14B C13B C12B 107.89(16) . . ? C14B C13B Fe1B 70.07(10) . . ? C12B C13B Fe1B 69.34(10) . . ? C12A C13A C14A 107.79(16) . . ? C12A C13A Fe1A 69.42(11) . . ? C14A C13A Fe1A 69.74(11) . . ? C13A C14A C15A 107.68(17) . . ? C13A C14A Fe1A 69.96(11) . . ? C15A C14A Fe1A 69.34(11) . . ? C13B C14B C15B 107.80(16) . . ? C13B C14B Fe1B 69.53(10) . . ? C15B C14B Fe1B 69.47(10) . . ? C14B C15B C11B 110.26(17) . . ? C14B C15B Fe1B 70.00(10) . . ? C11B C15B Fe1B 70.70(9) . . ? C14A C15A C11A 110.27(15) . . ? C14A C15A Fe1A 70.16(10) . . ? C11A C15A Fe1A 70.70(10) . . ? C17B C16B C20B 107.97(18) . . ? C17B C16B Fe1B 69.06(11) . . ? C20B C16B Fe1B 69.75(11) . . ? C20A C16A C17A 107.9(2) . . ? C20A C16A Fe1A 69.28(13) . . ? C17A C16A Fe1A 69.38(12) . . ? C16B C17B C18B 107.98(18) . . ? C16B C17B Fe1B 70.85(11) . . ? C18B C17B Fe1B 69.00(11) . . ? C18A C17A C16A 107.8(2) . . ? C18A C17A Fe1A 69.33(11) . . ? C16A C17A Fe1A 70.57(12) . . ? C19B C18B C17B 108.17(18) . . ? C19B C18B Fe1B 70.31(11) . . ? C17B C18B Fe1B 70.33(11) . . ? C17A C18A C19A 108.25(19) . . ? C17A C18A Fe1A 70.58(11) . . ? C19A C18A Fe1A 69.74(11) . . ? C18B C19B C20B 107.72(19) . . ? C18B C19B Fe1B 69.06(11) . . ? C20B C19B Fe1B 70.58(11) . . ? C20A C19A C18A 108.0(2) . . ? C20A C19A Fe1A 70.44(12) . . ? C18A C19A Fe1A 69.88(11) . . ? C19B C20B C16B 108.15(18) . . ? C19B C20B Fe1B 69.14(11) . . ? C16B C20B Fe1B 70.18(11) . . ? C19A C20A C16A 108.1(2) . . ? C19A C20A Fe1A 69.35(12) . . ? C16A C20A Fe1A 70.78(12) . . ? C36B C31B C32B 112.17(15) . . ? C36B C31B B1B 125.44(14) . . ? C32B C31B B1B 121.32(15) . . ? C32A C31A C36A 112.40(15) . . ? C32A C31A B1A 126.89(16) . . ? C36A C31A B1A 120.30(15) . . ? F32B C32B C33B 115.38(15) . . ? F32B C32B C31B 119.69(16) . . ? C33B C32B C31B 124.92(16) . . ? F32A C32A C33A 114.50(15) . . ? F32A C32A C31A 121.10(15) . . ? C33A C32A C31A 124.39(17) . . ? F33B C33B C34B 119.38(17) . . ? F33B C33B C32B 120.86(17) . . ? C34B C33B C32B 119.73(16) . . ? F33A C33A C34A 119.79(16) . . ? F33A C33A C32A 120.28(17) . . ? C34A C33A C32A 119.93(17) . . ? F34B C34B C35B 120.73(17) . . ? F34B C34B C33B 120.83(16) . . ? C35B C34B C33B 118.41(16) . . ? F34A C34A C33A 120.65(17) . . ? F34A C34A C35A 120.56(18) . . ? C33A C34A C35A 118.80(16) . . ? F35B C35B C34B 120.24(15) . . ? F35B C35B C36B 120.14(15) . . ? C34B C35B C36B 119.54(16) . . ? F35A C35A C34A 119.80(17) . . ? F35A C35A C36A 120.93(17) . . ? C34A C35A C36A 119.27(17) . . ? F36B C36B C35B 113.80(14) . . ? F36B C36B C31B 120.96(14) . . ? C35B C36B C31B 125.20(15) . . ? F36A C36A C35A 115.34(16) . . ? F36A C36A C31A 119.44(15) . . ? C35A C36A C31A 125.22(17) . . ? C46B C41B C42B 112.81(16) . . ? C46B C41B B1B 120.43(15) . . ? C42B C41B B1B 126.70(16) . . ? C42A C41A C46A 112.91(16) . . ? C42A C41A B1A 127.78(15) . . ? C46A C41A B1A 119.31(16) . . ? F42B C42B C43B 114.75(16) . . ? F42B C42B C41B 120.80(16) . . ? C43B C42B C41B 124.45(18) . . ? F42A C42A C43A 115.04(16) . . ? F42A C42A C41A 120.63(16) . . ? C43A C42A C41A 124.30(16) . . ? F43B C43B C44B 120.47(18) . . ? F43B C43B C42B 119.90(19) . . ? C44B C43B C42B 119.62(17) . . ? F43A C43A C44A 119.34(17) . . ? F43A C43A C42A 120.97(16) . . ? C44A C43A C42A 119.68(18) . . ? F44B C44B C43B 120.73(19) . . ? F44B C44B C45B 120.3(2) . . ? C43B C44B C45B 118.98(17) . . ? F44A C44A C45A 120.58(17) . . ? F44A C44A C43A 120.43(18) . . ? C45A C44A C43A 118.96(17) . . ? F45B C45B C44B 119.61(17) . . ? F45B C45B C46B 121.01(18) . . ? C44B C45B C46B 119.38(18) . . ? F45A C45A C44A 119.90(17) . . ? F45A C45A C46A 120.68(17) . . ? C44A C45A C46A 119.42(16) . . ? F46B C46B C45B 116.16(16) . . ? F46B C46B C41B 119.08(15) . . ? C45B C46B C41B 124.75(17) . . ? F46A C46A C45A 115.33(15) . . ? F46A C46A C41A 120.07(16) . . ? C45A C46A C41A 124.58(17) . . ? C56B C51B C52B 112.77(15) . . ? C56B C51B B1B 128.54(15) . . ? C52B C51B B1B 118.64(15) . . ? C56A C51A C52A 112.95(17) . . ? C56A C51A B1A 126.85(16) . . ? C52A C51A B1A 120.13(16) . . ? F52B C52B C53B 115.19(15) . . ? F52B C52B C51B 119.95(15) . . ? C53B C52B C51B 124.85(17) . . ? F52A C52A C53A 115.48(17) . . ? F52A C52A C51A 119.56(16) . . ? C53A C52A C51A 124.95(19) . . ? F53B C53B C54B 120.09(16) . . ? F53B C53B C52B 120.27(17) . . ? C54B C53B C52B 119.64(16) . . ? F53A C53A C54A 119.81(18) . . ? F53A C53A C52A 120.80(19) . . ? C54A C53A C52A 119.37(19) . . ? F54B C54B C55B 120.80(17) . . ? F54B C54B C53B 120.75(16) . . ? C55B C54B C53B 118.45(16) . . ? F54A C54A C55A 121.0(2) . . ? F54A C54A C53A 120.23(19) . . ? C55A C54A C53A 118.74(18) . . ? F55B C55B C54B 119.29(15) . . ? F55B C55B C56B 120.58(16) . . ? C54B C55B C56B 120.14(16) . . ? F55A C55A C54A 119.43(19) . . ? F55A C55A C56A 120.5(2) . . ? C54A C55A C56A 120.04(19) . . ? F56B C56B C55B 115.39(15) . . ? F56B C56B C51B 120.53(15) . . ? C55B C56B C51B 124.08(16) . . ? F56A C56A C51A 121.03(17) . . ? F56A C56A C55A 115.03(18) . . ? C51A C56A C55A 123.93(19) . . ? C104 Br1 C106 116.6(5) . . ? C104 Br1 C103 17.6(5) . 2_677 ? C106 Br1 C103 107.5(4) . 2_677 ? C104 Br1 C101 70.4(4) . . ? C106 Br1 C101 50.6(3) . . ? C103 Br1 C101 57.6(4) 2_677 . ? C101 C101 C105 78.8(10) 2_677 . ? C101 C101 C102 87.3(16) 2_677 . ? C105 C101 C102 9.1(16) . . ? C101 C101 C105 55.2(8) 2_677 2_677 ? C105 C101 C105 134.0(8) . 2_677 ? C102 C101 C105 142.4(19) . 2_677 ? C101 C101 C106 155.7(11) 2_677 . ? C105 C101 C106 77.9(7) . . ? C102 C101 C106 69.9(13) . . ? C105 C101 C106 147.5(9) 2_677 . ? C101 C101 C102 52.0(13) 2_677 2_677 ? C105 C101 C102 130.6(15) . 2_677 ? C102 C101 C102 139.3(8) . 2_677 ? C105 C101 C102 4.2(14) 2_677 2_677 ? C106 C101 C102 150.1(13) . 2_677 ? C101 C101 C103 110.2(10) 2_677 2_677 ? C105 C101 C103 166.3(8) . 2_677 ? C102 C101 C103 161.0(13) . 2_677 ? C105 C101 C103 55.9(9) 2_677 2_677 ? C106 C101 C103 91.6(6) . 2_677 ? C102 C101 C103 58.7(11) 2_677 2_677 ? C101 C101 C104 140.6(10) 2_677 . ? C105 C101 C104 136.3(8) . . ? C102 C101 C104 129.2(14) . . ? C105 C101 C104 87.8(8) 2_677 . ? C106 C101 C104 59.8(4) . . ? C102 C101 C104 90.4(12) 2_677 . ? C103 C101 C104 32.0(4) 2_677 . ? C101 C101 Br1 165.7(10) 2_677 . ? C105 C101 Br1 114.2(7) . . ? C102 C101 Br1 106.0(14) . . ? C105 C101 Br1 111.6(7) 2_677 . ? C106 C101 Br1 36.2(4) . . ? C102 C101 Br1 114.6(13) 2_677 . ? C103 C101 Br1 56.0(5) 2_677 . ? C104 C101 Br1 25.1(2) . . ? C101 C102 C101 40.7(8) . 2_677 ? C101 C102 C106 64.0(15) . . ? C101 C102 C106 104.4(17) 2_677 . ? C101 C102 C103 109.0(15) . . ? C101 C102 C103 68.7(10) 2_677 . ? C106 C102 C103 173.0(17) . . ? C104 C103 C105 124.2(8) 2_677 . ? C104 C103 C102 128.7(11) 2_677 . ? C105 C103 C102 5.8(13) . . ? C104 C103 Br1 14.5(4) 2_677 2_677 ? C105 C103 Br1 113.8(6) . 2_677 ? C102 C103 Br1 119.0(9) . 2_677 ? C104 C103 C101 76.6(5) 2_677 2_677 ? C105 C103 C101 47.7(6) . 2_677 ? C102 C103 C101 52.7(8) . 2_677 ? Br1 C103 C101 66.4(3) 2_677 2_677 ? C101 C105 C101 46.0(8) . 2_677 ? C101 C105 C103 121.4(10) . . ? C101 C105 C103 76.4(7) 2_677 . ? C101 C105 C106 60.7(6) . . ? C101 C105 C106 106.4(10) 2_677 . ? C103 C105 C106 173.5(11) . . ? Br1 C104 C103 147.9(8) . 2_677 ? Br1 C104 C106 37.5(4) . . ? C103 C104 C106 121.4(7) 2_677 . ? Br1 C104 C101 84.5(4) . . ? C103 C104 C101 71.4(6) 2_677 . ? C106 C104 C101 50.2(3) . . ? Br1 C106 C101 93.2(5) . . ? Br1 C106 C102 139.0(9) . . ? C101 C106 C102 46.1(8) . . ? Br1 C106 C105 134.6(6) . . ? C101 C106 C105 41.4(6) . . ? C102 C106 C105 5.6(13) . . ? Br1 C106 C104 25.9(3) . . ? C101 C106 C104 70.0(4) . . ? C102 C106 C104 115.8(9) . . ? C105 C106 C104 110.7(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 31.72 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.837 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.075 #===end data_[CpTi(NPtBu3)(C5H4)FeCp)][MeB(C6F5)3] _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H44 B F15 Fe N P Ti' _chemical_formula_weight 1041.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7656(3) _cell_length_b 28.7619(7) _cell_length_c 16.3906(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.2340(10) _cell_angle_gamma 90.00 _cell_volume 4420.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8060 _exptl_absorpt_correction_T_max 0.8556 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 39900 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10112 _reflns_number_gt 8522 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.5103P] 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_number_reflns 10112 _refine_ls_number_parameters 609 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40764(3) 0.199386(9) 0.102311(16) 0.01799(7) Uani 1 1 d . . . Ti1 Ti 0.47797(4) 0.161242(11) 0.25984(2) 0.02105(8) Uani 1 1 d . . . P1 P 0.51275(7) 0.044189(18) 0.26440(3) 0.03312(14) Uani 1 1 d . . . N1 N 0.49480(19) 0.09962(5) 0.25184(10) 0.0257(4) Uani 1 1 d . . . C22 C 0.2420(2) 0.22492(7) 0.14198(14) 0.0290(4) Uani 1 1 d . . . H22 H 0.2485 0.2509 0.1835 0.035 Uiso 1 1 calc R . . C23 C 0.6098(2) 0.19009(8) 0.17188(15) 0.0286(5) Uani 1 1 d . . . C21 C 0.2095(2) 0.22993(8) 0.05310(14) 0.0322(5) Uani 1 1 d . . . H21 H 0.1903 0.2599 0.0210 0.039 Uiso 1 1 calc R . . C25 C 0.5458(2) 0.19926(8) 0.02695(14) 0.0333(5) Uani 1 1 d . . . H25 H 0.5195 0.1924 -0.0353 0.040 Uiso 1 1 calc R . . C4 C 0.4833(2) 0.23487(7) 0.33353(13) 0.0282(4) Uani 1 1 d . . . H4 H 0.4631 0.2661 0.3060 0.034 Uiso 1 1 calc R . . C14 C 0.5433(3) 0.01803(7) 0.16541(14) 0.0374(5) Uani 1 1 d . . . C24 C 0.5882(2) 0.16624(7) 0.09274(14) 0.0293(5) Uani 1 1 d . . . H24 H 0.5988 0.1320 0.0853 0.035 Uiso 1 1 calc R . . C18 C 0.2693(2) 0.17658(7) 0.16373(15) 0.0301(5) Uani 1 1 d . . . C5 C 0.6170(2) 0.21463(8) 0.36359(13) 0.0320(5) Uani 1 1 d . . . H5 H 0.7094 0.2291 0.3621 0.038 Uiso 1 1 calc R . . C20 C 0.2115(2) 0.18512(8) 0.01737(15) 0.0344(5) Uani 1 1 d . . . H20 H 0.1938 0.1780 -0.0444 0.041 Uiso 1 1 calc R . . C15 C 0.6954(3) 0.02969(9) 0.16153(17) 0.0480(6) Uani 1 1 d . . . H15A H 0.7059 0.0207 0.1059 0.072 Uiso 1 1 calc R . . H15B H 0.7649 0.0126 0.2062 0.072 Uiso 1 1 calc R . . H15C H 0.7123 0.0632 0.1700 0.072 Uiso 1 1 calc R . . C19 C 0.2443(2) 0.15248(7) 0.08412(15) 0.0321(5) Uani 1 1 d . . . H19 H 0.2530 0.1181 0.0773 0.038 Uiso 1 1 calc R . . C26 C 0.5453(2) 0.24386(7) 0.06415(14) 0.0305(5) Uani 1 1 d . . . H26 H 0.5181 0.2737 0.0325 0.037 Uiso 1 1 calc R . . C1 C 0.6022(3) 0.17288(8) 0.40377(14) 0.0443(7) Uani 1 1 d . . . H1 H 0.6820 0.1532 0.4381 0.053 Uiso 1 1 calc R . . C13 C 0.2219(4) 0.02252(11) 0.1978(2) 0.0705(10) Uani 1 1 d . . . H13A H 0.1315 0.0135 0.2082 0.106 Uiso 1 1 calc R . . H13B H 0.2442 0.0009 0.1570 0.106 Uiso 1 1 calc R . . H13C H 0.2138 0.0541 0.1746 0.106 Uiso 1 1 calc R . . C9 C 0.7962(3) 0.06503(9) 0.35470(18) 0.0581(8) Uani 1 1 d . . . H9A H 0.8710 0.0636 0.4088 0.087 Uiso 1 1 calc R . . H9B H 0.7608 0.0970 0.3444 0.087 Uiso 1 1 calc R . . H9C H 0.8353 0.0552 0.3085 0.087 Uiso 1 1 calc R . . C6 C 0.6724(4) 0.03249(8) 0.35828(15) 0.0542(8) Uani 1 1 d . . . C2 C 0.4577(4) 0.16728(8) 0.39820(15) 0.0495(8) Uani 1 1 d . . . H2 H 0.4170 0.1430 0.4284 0.059 Uiso 1 1 calc R . . C8 C 0.6335(5) 0.04340(10) 0.44139(17) 0.0787(12) Uani 1 1 d . . . H8A H 0.5652 0.0202 0.4500 0.118 Uiso 1 1 calc R . . H8B H 0.5906 0.0744 0.4375 0.118 Uiso 1 1 calc R . . H8C H 0.7198 0.0425 0.4894 0.118 Uiso 1 1 calc R . . C16 C 0.4417(3) 0.04128(8) 0.08746(14) 0.0395(6) Uani 1 1 d . . . H16A H 0.4468 0.0751 0.0946 0.059 Uiso 1 1 calc R . . H16B H 0.3439 0.0308 0.0816 0.059 Uiso 1 1 calc R . . H16C H 0.4694 0.0328 0.0364 0.059 Uiso 1 1 calc R . . C17 C 0.5208(4) -0.03536(8) 0.15836(16) 0.0534(8) Uani 1 1 d . . . H17A H 0.4202 -0.0425 0.1519 0.080 Uiso 1 1 calc R . . H17B H 0.5800 -0.0503 0.2099 0.080 Uiso 1 1 calc R . . H17C H 0.5478 -0.0470 0.1088 0.080 Uiso 1 1 calc R . . C3 C 0.3829(3) 0.20576(9) 0.35410(15) 0.0405(6) Uani 1 1 d . . . H3 H 0.2799 0.2131 0.3463 0.049 Uiso 1 1 calc R . . C10 C 0.3417(4) 0.02090(9) 0.2818(2) 0.0586(8) Uani 1 1 d . . . C12 C 0.3559(5) -0.02937(10) 0.3175(2) 0.0874(14) Uani 1 1 d . . . H12A H 0.2638 -0.0396 0.3241 0.131 Uiso 1 1 calc R . . H12B H 0.4278 -0.0300 0.3729 0.131 Uiso 1 1 calc R . . H12C H 0.3850 -0.0502 0.2781 0.131 Uiso 1 1 calc R . . F5 F 1.22767(12) 0.17512(4) 0.79590(8) 0.0318(3) Uani 1 1 d . . . F3 F 1.42904(14) 0.12592(5) 0.58244(9) 0.0418(3) Uani 1 1 d . . . F10 F 0.74234(12) 0.18315(4) 0.80849(8) 0.0316(3) Uani 1 1 d . . . F11 F 1.00056(14) 0.22739(4) 0.86193(8) 0.0379(3) Uani 1 1 d . . . F4 F 1.45785(13) 0.15729(5) 0.74358(9) 0.0410(3) Uani 1 1 d . . . F6 F 1.12020(13) 0.08219(4) 0.79295(8) 0.0340(3) Uani 1 1 d . . . F2 F 1.16484(16) 0.10960(5) 0.47787(8) 0.0458(4) Uani 1 1 d . . . F15 F 0.89230(14) 0.22795(5) 0.56116(8) 0.0373(3) Uani 1 1 d . . . F9 F 0.70599(14) 0.13299(5) 0.93629(9) 0.0415(3) Uani 1 1 d . . . F14 F 0.90419(15) 0.31990(5) 0.56387(11) 0.0554(4) Uani 1 1 d . . . F8 F 0.88645(18) 0.06165(5) 1.00270(9) 0.0542(4) Uani 1 1 d . . . F1 F 0.93503(14) 0.12445(5) 0.52845(8) 0.0424(3) Uani 1 1 d . . . F7 F 1.09510(17) 0.03842(5) 0.92885(9) 0.0491(4) Uani 1 1 d . . . C34 C 1.2059(2) 0.15837(6) 0.71566(12) 0.0230(4) Uani 1 1 d . . . B1 B 0.9285(2) 0.16381(7) 0.70214(14) 0.0209(4) Uani 1 1 d . . . F12 F 1.00804(18) 0.31889(5) 0.86174(12) 0.0614(5) Uani 1 1 d . . . C29 C 1.0672(2) 0.15068(6) 0.66616(12) 0.0216(4) Uani 1 1 d . . . C35 C 0.93872(19) 0.22145(7) 0.71115(13) 0.0237(4) Uani 1 1 d . . . C31 C 1.1793(2) 0.12657(7) 0.55665(13) 0.0306(5) Uani 1 1 d . . . C46 C 1.0184(2) 0.09884(7) 0.82768(13) 0.0240(4) Uani 1 1 d . . . C41 C 0.9345(2) 0.13657(6) 0.79239(12) 0.0213(4) Uani 1 1 d . . . C36 C 0.9175(2) 0.24858(7) 0.63798(14) 0.0290(4) Uani 1 1 d . . . C33 C 1.3267(2) 0.15033(7) 0.69025(14) 0.0273(4) Uani 1 1 d . . . C43 C 0.8125(2) 0.12217(8) 0.90262(13) 0.0294(4) Uani 1 1 d . . . F13 F 0.96088(17) 0.36736(5) 0.71334(14) 0.0673(5) Uani 1 1 d . . . C28 C 0.7750(2) 0.14837(7) 0.63802(13) 0.0263(4) Uani 1 1 d . . . H28A H 0.7761 0.1149 0.6265 0.039 Uiso 1 1 calc R . . H28B H 0.7580 0.1656 0.5845 0.039 Uiso 1 1 calc R . . H28C H 0.6989 0.1553 0.6645 0.039 Uiso 1 1 calc R . . C37 C 0.9247(2) 0.29669(8) 0.63773(18) 0.0386(6) Uani 1 1 d . . . C30 C 1.0613(2) 0.13433(7) 0.58564(13) 0.0272(4) Uani 1 1 d . . . C44 C 0.9024(3) 0.08581(8) 0.93580(14) 0.0336(5) Uani 1 1 d . . . C32 C 1.3129(2) 0.13466(7) 0.60891(14) 0.0285(4) Uani 1 1 d . . . C38 C 0.9542(2) 0.32051(8) 0.7127(2) 0.0431(6) Uani 1 1 d . . . C42 C 0.8321(2) 0.14671(7) 0.83458(12) 0.0239(4) Uani 1 1 d . . . C40 C 0.9714(2) 0.24797(7) 0.78505(14) 0.0290(4) Uani 1 1 d . . . C45 C 1.0066(2) 0.07436(7) 0.89811(14) 0.0312(5) Uani 1 1 d . . . C39 C 0.9779(2) 0.29610(8) 0.78698(17) 0.0391(6) Uani 1 1 d . . . C11 C 0.2931(4) 0.05292(10) 0.3436(2) 0.0730(11) Uani 1 1 d . . . H11A H 0.2810 0.0846 0.3209 0.109 Uiso 1 1 calc R . . H11B H 0.3651 0.0528 0.3989 0.109 Uiso 1 1 calc R . . H11C H 0.2021 0.0417 0.3503 0.109 Uiso 1 1 calc R . . C7 C 0.7253(4) -0.01867(9) 0.36367(19) 0.0781(12) Uani 1 1 d . . . H7A H 0.7586 -0.0258 0.3139 0.117 Uiso 1 1 calc R . . H7B H 0.6468 -0.0396 0.3650 0.117 Uiso 1 1 calc R . . H7C H 0.8039 -0.0229 0.4155 0.117 Uiso 1 1 calc R . . C27 C 0.5870(2) 0.23871(7) 0.15322(14) 0.0272(4) Uani 1 1 d . . . H27 H 0.5963 0.2643 0.1958 0.033 Uiso 1 1 calc R . . H23 H 0.649(4) 0.1778(14) 0.216(3) 0.105(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01822(13) 0.01810(13) 0.01755(13) 0.00174(10) 0.00484(10) 0.00206(10) Ti1 0.0356(2) 0.01315(15) 0.01506(16) -0.00103(12) 0.00824(14) -0.00083(14) P1 0.0671(4) 0.0131(2) 0.0210(3) -0.0010(2) 0.0152(3) -0.0021(2) N1 0.0446(10) 0.0165(8) 0.0173(8) -0.0016(6) 0.0106(7) -0.0019(7) C22 0.0209(10) 0.0276(11) 0.0407(12) -0.0043(9) 0.0121(9) 0.0052(8) C23 0.0173(9) 0.0269(11) 0.0372(12) 0.0066(9) 0.0006(9) 0.0005(8) C21 0.0220(10) 0.0293(11) 0.0393(12) 0.0020(9) -0.0013(9) 0.0064(8) C25 0.0398(12) 0.0353(12) 0.0324(11) 0.0047(9) 0.0228(10) 0.0011(10) C4 0.0434(12) 0.0176(9) 0.0229(10) -0.0058(8) 0.0081(9) 0.0031(9) C14 0.0669(16) 0.0206(10) 0.0255(11) -0.0047(9) 0.0139(11) 0.0054(10) C24 0.0231(10) 0.0270(10) 0.0426(12) 0.0047(9) 0.0170(9) 0.0048(8) C18 0.0254(10) 0.0285(11) 0.0438(13) -0.0002(9) 0.0220(10) 0.0010(8) C5 0.0344(11) 0.0323(11) 0.0260(11) -0.0139(9) 0.0031(9) -0.0032(9) C20 0.0252(11) 0.0357(12) 0.0339(12) -0.0060(9) -0.0055(9) 0.0055(9) C15 0.0667(18) 0.0378(14) 0.0429(14) -0.0015(11) 0.0210(13) 0.0151(13) C19 0.0192(10) 0.0250(10) 0.0490(14) -0.0052(10) 0.0047(9) -0.0021(8) C26 0.0314(11) 0.0286(11) 0.0359(12) 0.0093(9) 0.0169(9) -0.0015(9) C1 0.0764(19) 0.0304(12) 0.0169(10) -0.0063(9) -0.0021(11) 0.0156(12) C13 0.078(2) 0.0480(17) 0.095(3) -0.0216(17) 0.039(2) -0.0296(16) C9 0.072(2) 0.0368(14) 0.0462(16) -0.0075(12) -0.0154(14) 0.0162(13) C6 0.105(2) 0.0238(12) 0.0238(12) 0.0018(9) 0.0004(13) 0.0134(13) C2 0.106(2) 0.0287(12) 0.0237(11) -0.0104(9) 0.0344(14) -0.0222(14) C8 0.171(4) 0.0354(15) 0.0252(13) 0.0022(11) 0.0201(18) 0.0086(19) C16 0.0640(16) 0.0287(12) 0.0243(11) -0.0063(9) 0.0100(11) 0.0066(11) C17 0.105(2) 0.0183(11) 0.0370(13) -0.0072(10) 0.0197(15) 0.0061(13) C3 0.0415(13) 0.0528(15) 0.0330(12) -0.0249(11) 0.0202(10) -0.0079(11) C10 0.100(2) 0.0280(13) 0.0644(19) -0.0095(12) 0.0508(19) -0.0225(14) C12 0.168(4) 0.0279(14) 0.092(3) -0.0047(16) 0.080(3) -0.030(2) F5 0.0247(6) 0.0355(7) 0.0324(7) -0.0122(5) 0.0032(5) -0.0025(5) F3 0.0366(7) 0.0456(8) 0.0533(8) 0.0068(7) 0.0292(7) 0.0075(6) F10 0.0270(6) 0.0333(7) 0.0341(7) -0.0024(5) 0.0080(5) 0.0097(5) F11 0.0410(7) 0.0314(7) 0.0322(7) -0.0082(5) -0.0049(6) 0.0042(6) F4 0.0200(6) 0.0428(8) 0.0588(9) -0.0126(7) 0.0083(6) -0.0052(5) F6 0.0379(7) 0.0274(6) 0.0433(7) 0.0079(5) 0.0223(6) 0.0129(5) F2 0.0537(9) 0.0611(9) 0.0259(7) -0.0004(6) 0.0167(6) 0.0188(7) F15 0.0351(7) 0.0445(8) 0.0325(7) 0.0124(6) 0.0096(6) 0.0002(6) F9 0.0400(7) 0.0537(8) 0.0389(7) -0.0088(6) 0.0243(6) -0.0019(6) F14 0.0376(8) 0.0468(9) 0.0854(12) 0.0411(8) 0.0229(8) 0.0096(7) F8 0.0789(11) 0.0513(9) 0.0434(8) 0.0177(7) 0.0355(8) 0.0043(8) F1 0.0319(7) 0.0638(9) 0.0272(7) -0.0139(6) 0.0011(5) 0.0054(6) F7 0.0655(10) 0.0360(8) 0.0509(9) 0.0220(7) 0.0248(8) 0.0220(7) C34 0.0251(10) 0.0175(9) 0.0263(10) -0.0008(8) 0.0074(8) -0.0018(7) B1 0.0196(10) 0.0206(10) 0.0211(10) -0.0009(8) 0.0032(8) 0.0005(8) F12 0.0596(10) 0.0342(8) 0.0824(12) -0.0298(8) 0.0067(9) -0.0022(7) C29 0.0241(9) 0.0164(9) 0.0238(9) 0.0021(7) 0.0060(8) 0.0000(7) C35 0.0137(8) 0.0213(9) 0.0337(11) 0.0033(8) 0.0026(8) 0.0022(7) C31 0.0418(12) 0.0279(11) 0.0245(10) 0.0051(8) 0.0136(9) 0.0086(9) C46 0.0251(10) 0.0214(10) 0.0278(10) -0.0015(8) 0.0110(8) 0.0013(8) C41 0.0220(9) 0.0201(9) 0.0211(9) -0.0028(7) 0.0048(7) -0.0020(7) C36 0.0168(9) 0.0312(11) 0.0386(12) 0.0068(9) 0.0072(9) 0.0024(8) C33 0.0219(10) 0.0185(9) 0.0410(12) 0.0015(8) 0.0080(9) -0.0028(8) C43 0.0316(11) 0.0326(11) 0.0279(10) -0.0082(9) 0.0147(9) -0.0033(9) F13 0.0536(10) 0.0174(7) 0.1333(17) 0.0055(8) 0.0302(10) 0.0014(6) C28 0.0226(10) 0.0295(11) 0.0249(10) -0.0015(8) 0.0037(8) -0.0046(8) C37 0.0195(10) 0.0309(12) 0.0668(17) 0.0221(12) 0.0147(10) 0.0056(9) C30 0.0273(10) 0.0274(10) 0.0251(10) 0.0018(8) 0.0042(8) 0.0040(8) C44 0.0459(13) 0.0314(11) 0.0267(11) 0.0026(9) 0.0155(10) -0.0040(10) C32 0.0301(11) 0.0219(10) 0.0391(12) 0.0069(9) 0.0189(9) 0.0050(8) C38 0.0239(11) 0.0178(10) 0.087(2) 0.0041(12) 0.0145(12) 0.0012(9) C42 0.0223(9) 0.0237(10) 0.0246(10) -0.0044(8) 0.0046(8) 0.0013(8) C40 0.0194(9) 0.0245(10) 0.0382(12) -0.0027(9) -0.0002(9) 0.0019(8) C45 0.0408(12) 0.0216(10) 0.0313(11) 0.0050(8) 0.0099(9) 0.0051(9) C39 0.0254(11) 0.0252(11) 0.0629(16) -0.0119(11) 0.0058(11) 0.0008(9) C11 0.116(3) 0.0424(16) 0.090(2) -0.0145(16) 0.077(2) -0.0276(18) C7 0.144(3) 0.0276(14) 0.0422(16) 0.0035(12) -0.0075(19) 0.0268(17) C27 0.0229(10) 0.0235(10) 0.0347(11) 0.0027(9) 0.0071(8) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C23 2.002(2) . ? Fe1 C18 2.008(2) . ? Fe1 C22 2.0414(19) . ? Fe1 C19 2.047(2) . ? Fe1 C24 2.0485(19) . ? Fe1 C27 2.056(2) . ? Fe1 C25 2.069(2) . ? Fe1 C20 2.070(2) . ? Fe1 C21 2.072(2) . ? Fe1 C26 2.075(2) . ? Fe1 Ti1 2.7112(4) . ? Ti1 N1 1.7882(16) . ? Ti1 C18 2.244(2) . ? Ti1 C23 2.337(2) . ? Ti1 C2 2.337(2) . ? Ti1 C1 2.356(2) . ? Ti1 C3 2.385(2) . ? Ti1 C5 2.409(2) . ? Ti1 C4 2.4311(19) . ? P1 N1 1.6108(16) . ? P1 C14 1.886(2) . ? P1 C6 1.890(3) . ? P1 C10 1.894(3) . ? C22 C21 1.409(3) . ? C22 C18 1.442(3) . ? C23 C24 1.430(3) . ? C23 C27 1.435(3) . ? C21 C20 1.418(3) . ? C25 C24 1.409(3) . ? C25 C26 1.421(3) . ? C4 C5 1.388(3) . ? C4 C3 1.400(3) . ? C14 C16 1.535(3) . ? C14 C15 1.542(4) . ? C14 C17 1.551(3) . ? C18 C19 1.437(3) . ? C5 C1 1.396(3) . ? C20 C19 1.409(3) . ? C26 C27 1.409(3) . ? C1 C2 1.398(4) . ? C13 C10 1.538(5) . ? C9 C6 1.542(4) . ? C6 C8 1.546(4) . ? C6 C7 1.554(3) . ? C2 C3 1.409(4) . ? C10 C11 1.539(4) . ? C10 C12 1.552(4) . ? F5 C34 1.361(2) . ? F3 C32 1.347(2) . ? F10 C42 1.357(2) . ? F11 C40 1.349(3) . ? F4 C33 1.348(2) . ? F6 C46 1.363(2) . ? F2 C31 1.350(2) . ? F15 C36 1.351(3) . ? F9 C43 1.344(2) . ? F14 C37 1.348(3) . ? F8 C44 1.343(2) . ? F1 C30 1.354(2) . ? F7 C45 1.351(2) . ? C34 C33 1.376(3) . ? C34 C29 1.389(3) . ? B1 C28 1.633(3) . ? B1 C41 1.661(3) . ? B1 C29 1.664(3) . ? B1 C35 1.665(3) . ? F12 C39 1.348(3) . ? C29 C30 1.387(3) . ? C35 C40 1.391(3) . ? C35 C36 1.397(3) . ? C31 C32 1.365(3) . ? C31 C30 1.382(3) . ? C46 C45 1.384(3) . ? C46 C41 1.385(3) . ? C41 C42 1.396(3) . ? C36 C37 1.385(3) . ? C33 C32 1.378(3) . ? C43 C44 1.376(3) . ? C43 C42 1.378(3) . ? F13 C38 1.349(3) . ? C37 C38 1.365(4) . ? C44 C45 1.370(3) . ? C38 C39 1.368(4) . ? C40 C39 1.386(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Fe1 C18 111.43(9) . . ? C23 Fe1 C22 127.55(9) . . ? C18 Fe1 C22 41.71(8) . . ? C23 Fe1 C19 126.81(9) . . ? C18 Fe1 C19 41.50(9) . . ? C22 Fe1 C19 68.20(8) . . ? C23 Fe1 C24 41.32(9) . . ? C18 Fe1 C24 126.92(9) . . ? C22 Fe1 C24 165.34(9) . . ? C19 Fe1 C24 109.55(9) . . ? C23 Fe1 C27 41.40(8) . . ? C18 Fe1 C27 126.35(9) . . ? C22 Fe1 C27 109.50(9) . . ? C19 Fe1 C27 164.33(9) . . ? C24 Fe1 C27 68.49(9) . . ? C23 Fe1 C25 68.65(9) . . ? C18 Fe1 C25 160.35(9) . . ? C22 Fe1 C25 153.92(9) . . ? C19 Fe1 C25 121.60(9) . . ? C24 Fe1 C25 40.03(9) . . ? C27 Fe1 C25 67.63(9) . . ? C23 Fe1 C20 159.41(9) . . ? C18 Fe1 C20 69.29(10) . . ? C22 Fe1 C20 67.59(9) . . ? C19 Fe1 C20 40.03(9) . . ? C24 Fe1 C20 120.71(9) . . ? C27 Fe1 C20 154.86(9) . . ? C25 Fe1 C20 103.51(10) . . ? C23 Fe1 C21 160.54(9) . . ? C18 Fe1 C21 69.36(9) . . ? C22 Fe1 C21 40.05(9) . . ? C19 Fe1 C21 67.52(9) . . ? C24 Fe1 C21 153.83(9) . . ? C27 Fe1 C21 121.44(9) . . ? C25 Fe1 C21 117.55(9) . . ? C20 Fe1 C21 40.03(9) . . ? C23 Fe1 C26 68.62(9) . . ? C18 Fe1 C26 159.44(9) . . ? C22 Fe1 C26 120.80(9) . . ? C19 Fe1 C26 155.08(9) . . ? C24 Fe1 C26 67.66(8) . . ? C27 Fe1 C26 39.91(8) . . ? C25 Fe1 C26 40.12(9) . . ? C20 Fe1 C26 118.37(9) . . ? C21 Fe1 C26 103.56(9) . . ? C23 Fe1 Ti1 57.10(7) . . ? C18 Fe1 Ti1 54.34(7) . . ? C22 Fe1 Ti1 81.64(6) . . ? C19 Fe1 Ti1 81.46(7) . . ? C24 Fe1 Ti1 83.70(6) . . ? C27 Fe1 Ti1 82.87(6) . . ? C25 Fe1 Ti1 122.28(7) . . ? C20 Fe1 Ti1 120.05(7) . . ? C21 Fe1 Ti1 120.17(7) . . ? C26 Fe1 Ti1 121.58(6) . . ? N1 Ti1 C18 103.14(8) . . ? N1 Ti1 C23 103.23(8) . . ? C18 Ti1 C23 92.63(7) . . ? N1 Ti1 C2 100.33(8) . . ? C18 Ti1 C2 111.10(10) . . ? C23 Ti1 C2 141.52(9) . . ? N1 Ti1 C1 100.50(8) . . ? C18 Ti1 C1 141.96(9) . . ? C23 Ti1 C1 110.43(9) . . ? C2 Ti1 C1 34.65(10) . . ? N1 Ti1 C3 129.79(8) . . ? C18 Ti1 C3 84.70(8) . . ? C23 Ti1 C3 126.17(8) . . ? C2 Ti1 C3 34.70(9) . . ? C1 Ti1 C3 57.30(9) . . ? N1 Ti1 C5 129.67(8) . . ? C18 Ti1 C5 126.33(8) . . ? C23 Ti1 C5 84.85(8) . . ? C2 Ti1 C5 56.74(9) . . ? C1 Ti1 C5 34.06(8) . . ? C3 Ti1 C5 56.30(8) . . ? N1 Ti1 C4 155.53(7) . . ? C18 Ti1 C4 93.82(8) . . ? C23 Ti1 C4 93.34(8) . . ? C2 Ti1 C4 56.57(8) . . ? C1 Ti1 C4 56.30(8) . . ? C3 Ti1 C4 33.78(8) . . ? C5 Ti1 C4 33.33(7) . . ? N1 Ti1 Fe1 109.58(5) . . ? C18 Ti1 Fe1 46.63(5) . . ? C23 Ti1 Fe1 46.00(5) . . ? C2 Ti1 Fe1 145.72(7) . . ? C1 Ti1 Fe1 144.95(7) . . ? C3 Ti1 Fe1 111.03(7) . . ? C5 Ti1 Fe1 110.92(6) . . ? C4 Ti1 Fe1 94.89(5) . . ? N1 P1 C14 108.82(9) . . ? N1 P1 C6 108.41(10) . . ? C14 P1 C6 109.66(12) . . ? N1 P1 C10 107.47(11) . . ? C14 P1 C10 110.28(12) . . ? C6 P1 C10 112.11(15) . . ? P1 N1 Ti1 168.68(11) . . ? C21 C22 C18 109.08(19) . . ? C21 C22 Fe1 71.16(12) . . ? C18 C22 Fe1 67.89(11) . . ? C24 C23 C27 107.42(19) . . ? C24 C23 Fe1 71.07(12) . . ? C27 C23 Fe1 71.28(12) . . ? C24 C23 Ti1 114.98(14) . . ? C27 C23 Ti1 113.44(15) . . ? Fe1 C23 Ti1 76.90(7) . . ? C22 C21 C20 108.01(19) . . ? C22 C21 Fe1 68.79(11) . . ? C20 C21 Fe1 69.90(12) . . ? C24 C25 C26 108.4(2) . . ? C24 C25 Fe1 69.21(11) . . ? C26 C25 Fe1 70.16(11) . . ? C5 C4 C3 108.4(2) . . ? C5 C4 Ti1 72.45(11) . . ? C3 C4 Ti1 71.31(12) . . ? C16 C14 C15 106.1(2) . . ? C16 C14 C17 108.9(2) . . ? C15 C14 C17 109.3(2) . . ? C16 C14 P1 108.75(15) . . ? C15 C14 P1 109.56(16) . . ? C17 C14 P1 113.93(16) . . ? C25 C24 C23 107.95(19) . . ? C25 C24 Fe1 70.76(12) . . ? C23 C24 Fe1 67.61(11) . . ? C19 C18 C22 105.55(19) . . ? C19 C18 Fe1 70.71(12) . . ? C22 C18 Fe1 70.40(11) . . ? C19 C18 Ti1 115.67(14) . . ? C22 C18 Ti1 115.59(15) . . ? Fe1 C18 Ti1 79.03(7) . . ? C4 C5 C1 108.5(2) . . ? C4 C5 Ti1 74.22(12) . . ? C1 C5 Ti1 70.89(12) . . ? C19 C20 C21 108.1(2) . . ? C19 C20 Fe1 69.09(12) . . ? C21 C20 Fe1 70.07(12) . . ? C20 C19 C18 109.13(19) . . ? C20 C19 Fe1 70.88(12) . . ? C18 C19 Fe1 67.79(11) . . ? C27 C26 C25 108.35(19) . . ? C27 C26 Fe1 69.32(11) . . ? C25 C26 Fe1 69.72(12) . . ? C5 C1 C2 107.7(2) . . ? C5 C1 Ti1 75.05(12) . . ? C2 C1 Ti1 71.96(13) . . ? C9 C6 C8 107.4(2) . . ? C9 C6 C7 109.0(3) . . ? C8 C6 C7 107.6(2) . . ? C9 C6 P1 109.75(17) . . ? C8 C6 P1 109.3(2) . . ? C7 C6 P1 113.59(19) . . ? C1 C2 C3 108.2(2) . . ? C1 C2 Ti1 73.39(13) . . ? C3 C2 Ti1 74.51(13) . . ? C4 C3 C2 107.2(2) . . ? C4 C3 Ti1 74.91(12) . . ? C2 C3 Ti1 70.79(13) . . ? C13 C10 C11 105.9(3) . . ? C13 C10 C12 109.4(3) . . ? C11 C10 C12 108.7(2) . . ? C13 C10 P1 109.68(19) . . ? C11 C10 P1 109.56(19) . . ? C12 C10 P1 113.4(3) . . ? F5 C34 C33 115.90(17) . . ? F5 C34 C29 118.96(17) . . ? C33 C34 C29 125.14(19) . . ? C28 B1 C41 104.01(15) . . ? C28 B1 C29 113.67(16) . . ? C41 B1 C29 112.28(15) . . ? C28 B1 C35 110.44(16) . . ? C41 B1 C35 113.86(16) . . ? C29 B1 C35 102.90(15) . . ? C30 C29 C34 112.57(18) . . ? C30 C29 B1 126.36(17) . . ? C34 C29 B1 120.96(17) . . ? C40 C35 C36 112.59(18) . . ? C40 C35 B1 128.08(18) . . ? C36 C35 B1 119.30(18) . . ? F2 C31 C32 119.21(19) . . ? F2 C31 C30 120.8(2) . . ? C32 C31 C30 119.93(19) . . ? F6 C46 C45 114.21(17) . . ? F6 C46 C41 121.07(17) . . ? C45 C46 C41 124.70(18) . . ? C46 C41 C42 112.25(17) . . ? C46 C41 B1 127.67(17) . . ? C42 C41 B1 119.41(17) . . ? F15 C36 C37 115.6(2) . . ? F15 C36 C35 119.96(19) . . ? C37 C36 C35 124.4(2) . . ? F4 C33 C34 121.20(19) . . ? F4 C33 C32 119.64(18) . . ? C34 C33 C32 119.16(19) . . ? F9 C43 C44 119.67(19) . . ? F9 C43 C42 120.85(19) . . ? C44 C43 C42 119.47(19) . . ? F14 C37 C38 120.0(2) . . ? F14 C37 C36 120.2(2) . . ? C38 C37 C36 119.8(2) . . ? F1 C30 C31 114.43(18) . . ? F1 C30 C29 121.15(18) . . ? C31 C30 C29 124.42(19) . . ? F8 C44 C45 120.9(2) . . ? F8 C44 C43 120.6(2) . . ? C45 C44 C43 118.45(19) . . ? F3 C32 C31 120.6(2) . . ? F3 C32 C33 120.60(19) . . ? C31 C32 C33 118.76(18) . . ? F13 C38 C37 120.4(2) . . ? F13 C38 C39 120.6(3) . . ? C37 C38 C39 118.9(2) . . ? F10 C42 C43 115.28(17) . . ? F10 C42 C41 119.64(17) . . ? C43 C42 C41 125.08(19) . . ? F11 C40 C39 114.9(2) . . ? F11 C40 C35 120.68(18) . . ? C39 C40 C35 124.4(2) . . ? F7 C45 C44 119.61(19) . . ? F7 C45 C46 120.42(19) . . ? C44 C45 C46 119.95(19) . . ? F12 C39 C38 120.0(2) . . ? F12 C39 C40 120.2(2) . . ? C38 C39 C40 119.8(2) . . ? C26 C27 C23 107.80(19) . . ? C26 C27 Fe1 70.77(12) . . ? C23 C27 Fe1 67.31(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.350 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.052 #===end