# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'G. Erker' 'Roland Frohlich' 'Stefan Grimme' 'Gerald Kehr' 'Juri Ugolotti' _publ_contact_author_name 'Gerhard Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Nitrile Insertion into a Boryl-substituted Five-membered Zirconacycloallenoid: Unexpected formation of a Zwitterionic Boratirane Product ; # Attachment '5a.cif' data_erk5058 _database_code_depnum_ccdc_archive 'CCDC 743302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 B F10 N Si2 Zr' _chemical_formula_weight 908.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9479(2) _cell_length_b 10.8207(2) _cell_length_c 35.2290(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.172(1) _cell_angle_gamma 90.00 _cell_volume 4172.49(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9128 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8113 _exptl_absorpt_correction_T_max 0.8902 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34244 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9312 _reflns_number_gt 6812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.2314P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9312 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Zr Zr -0.73968(2) 0.89613(2) 0.621357(7) 0.03212(9) Uani 1 1 d . . . N1 N -0.6464(2) 0.8353(2) 0.57671(7) 0.0440(6) Uani 1 1 d . . . C1 C -0.5813(2) 0.7796(2) 0.55291(7) 0.0333(6) Uani 1 1 d . . . C2 C -0.4974(2) 0.6817(3) 0.56422(7) 0.0351(6) Uani 1 1 d . . . H2 H -0.4960 0.6106 0.5465 0.042 Uiso 1 1 calc R . . C3 C -0.4942(2) 0.6456(2) 0.60665(7) 0.0312(5) Uani 1 1 d . . . C4 C -0.5648(2) 0.7188(2) 0.63213(9) 0.0402(6) Uani 1 1 d . . . C5 C -0.6191(2) 0.7593(2) 0.66056(8) 0.0371(6) Uani 1 1 d . . . C6 C -0.5886(3) 0.8133(3) 0.51132(8) 0.0561(8) Uani 1 1 d . . . H6A H -0.6328 0.7495 0.4974 0.084 Uiso 1 1 calc R . . H6B H -0.5068 0.8205 0.5015 0.084 Uiso 1 1 calc R . . H6C H -0.6310 0.8915 0.5083 0.084 Uiso 1 1 calc R . . B1 B -0.3710(3) 0.7051(3) 0.58700(8) 0.0326(6) Uani 1 1 d . . . Si31 Si -0.51532(7) 0.47583(7) 0.61717(2) 0.04196(19) Uani 1 1 d . . . C32 C -0.4338(4) 0.4310(4) 0.66217(10) 0.0724(11) Uani 1 1 d . . . H32A H -0.4464 0.4942 0.6812 0.109 Uiso 1 1 calc R . . H32B H -0.3472 0.4229 0.6576 0.109 Uiso 1 1 calc R . . H32C H -0.4656 0.3528 0.6711 0.109 Uiso 1 1 calc R . . C33 C -0.6822(3) 0.4448(3) 0.62093(12) 0.0709(11) Uani 1 1 d . . . H33A H -0.7216 0.4552 0.5962 0.106 Uiso 1 1 calc R . . H33B H -0.7174 0.5023 0.6388 0.106 Uiso 1 1 calc R . . H33C H -0.6945 0.3609 0.6297 0.106 Uiso 1 1 calc R . . C34 C -0.4561(3) 0.3764(3) 0.57826(10) 0.0581(9) Uani 1 1 d . . . H34A H -0.4742 0.2904 0.5836 0.087 Uiso 1 1 calc R . . H34B H -0.3684 0.3871 0.5766 0.087 Uiso 1 1 calc R . . H34C H -0.4949 0.3999 0.5543 0.087 Uiso 1 1 calc R . . Si51 Si -0.62824(8) 0.73919(9) 0.71287(3) 0.0541(2) Uani 1 1 d . . . C52 C -0.7291(5) 0.8518(4) 0.73510(10) 0.0885(14) Uani 1 1 d . . . H52A H -0.6925 0.9333 0.7338 0.133 Uiso 1 1 calc R . . H52B H -0.7405 0.8293 0.7614 0.133 Uiso 1 1 calc R . . H52C H -0.8075 0.8524 0.7218 0.133 Uiso 1 1 calc R . . C53 C -0.4757(4) 0.7450(6) 0.73559(11) 0.1051(18) Uani 1 1 d . . . H53A H -0.4234 0.6838 0.7241 0.158 Uiso 1 1 calc R . . H53B H -0.4823 0.7277 0.7625 0.158 Uiso 1 1 calc R . . H53C H -0.4409 0.8266 0.7322 0.158 Uiso 1 1 calc R . . C54 C -0.6960(5) 0.5825(4) 0.72134(13) 0.0931(15) Uani 1 1 d . . . H54A H -0.7729 0.5753 0.7073 0.140 Uiso 1 1 calc R . . H54B H -0.7102 0.5720 0.7482 0.140 Uiso 1 1 calc R . . H54C H -0.6401 0.5193 0.7128 0.140 Uiso 1 1 calc R . . C11 C -0.6965(3) 1.1128(2) 0.59962(8) 0.0419(6) Uani 1 1 d . . . C12 C -0.7777(3) 1.1234(3) 0.62985(9) 0.0450(7) Uani 1 1 d . . . H12 H -0.8586 1.1520 0.6279 0.054 Uiso 1 1 calc R . . C13 C -0.7186(3) 1.0845(3) 0.66326(8) 0.0460(7) Uani 1 1 d . . . H13 H -0.7528 1.0821 0.6875 0.055 Uiso 1 1 calc R . . C14 C -0.6002(3) 1.0499(3) 0.65440(8) 0.0442(7) Uani 1 1 d . . . H14 H -0.5402 1.0203 0.6716 0.053 Uiso 1 1 calc R . . C15 C -0.5863(2) 1.0671(2) 0.61531(9) 0.0425(7) Uani 1 1 d . . . H15 H -0.5149 1.0507 0.6018 0.051 Uiso 1 1 calc R . . C111 C -0.7224(3) 1.1486(3) 0.55914(9) 0.0639(9) Uani 1 1 d . . . H11A H -0.8062 1.1275 0.5524 0.096 Uiso 1 1 calc R . . H11B H -0.6674 1.1045 0.5427 0.096 Uiso 1 1 calc R . . H11C H -0.7105 1.2369 0.5562 0.096 Uiso 1 1 calc R . . C16 C -0.9282(3) 0.8293(3) 0.58247(10) 0.0562(8) Uani 1 1 d . . . C17 C -0.9646(3) 0.9150(4) 0.60943(13) 0.0711(11) Uani 1 1 d . . . H17 H -0.9947 0.9947 0.6042 0.085 Uiso 1 1 calc R . . C18 C -0.9490(3) 0.8627(5) 0.64583(12) 0.0839(14) Uani 1 1 d . . . H18 H -0.9665 0.9000 0.6692 0.101 Uiso 1 1 calc R . . C19 C -0.9024(3) 0.7451(5) 0.64029(13) 0.0787(12) Uani 1 1 d . . . H19 H -0.8839 0.6875 0.6595 0.094 Uiso 1 1 calc R . . C20 C -0.8878(3) 0.7266(3) 0.60217(12) 0.0639(10) Uani 1 1 d . . . H20 H -0.8553 0.6549 0.5912 0.077 Uiso 1 1 calc R . . C161 C -0.9369(4) 0.8431(5) 0.54030(12) 0.0952(14) Uani 1 1 d . . . H16A H -0.8737 0.7941 0.5287 0.143 Uiso 1 1 calc R . . H16B H -0.9264 0.9293 0.5336 0.143 Uiso 1 1 calc R . . H16C H -1.0165 0.8149 0.5313 0.143 Uiso 1 1 calc R . . C21 C -0.2601(2) 0.6137(2) 0.57720(8) 0.0364(6) Uani 1 1 d . . . C22 C -0.1809(2) 0.5694(3) 0.60514(9) 0.0438(7) Uani 1 1 d . . . F22 F -0.19308(17) 0.60905(17) 0.64115(5) 0.0590(5) Uani 1 1 d . . . C23 C -0.0900(3) 0.4840(3) 0.59880(11) 0.0589(9) Uani 1 1 d . . . F23 F -0.01868(19) 0.4423(2) 0.62763(7) 0.0881(7) Uani 1 1 d . . . C24 C -0.0730(3) 0.4413(3) 0.56260(13) 0.0664(10) Uani 1 1 d . . . F24 F 0.0132(2) 0.3569(2) 0.55617(9) 0.1064(9) Uani 1 1 d . . . C25 C -0.1460(3) 0.4851(3) 0.53373(11) 0.0641(10) Uani 1 1 d . . . F25 F -0.1308(2) 0.4431(2) 0.49809(7) 0.0982(8) Uani 1 1 d . . . C26 C -0.2360(3) 0.5698(3) 0.54114(9) 0.0488(7) Uani 1 1 d . . . F26 F -0.30427(19) 0.60717(19) 0.51103(5) 0.0684(6) Uani 1 1 d . . . C41 C -0.3277(2) 0.8427(2) 0.59761(7) 0.0307(5) Uani 1 1 d . . . C42 C -0.3151(2) 0.8902(3) 0.63387(7) 0.0364(6) Uani 1 1 d . . . F42 F -0.34231(15) 0.81999(17) 0.66411(4) 0.0518(4) Uani 1 1 d . . . C43 C -0.2749(2) 1.0085(3) 0.64194(8) 0.0463(7) Uani 1 1 d . . . F43 F -0.26893(19) 1.0490(2) 0.67808(5) 0.0743(6) Uani 1 1 d . . . C44 C -0.2399(3) 1.0838(3) 0.61336(10) 0.0490(8) Uani 1 1 d . . . F44 F -0.1972(2) 1.19810(18) 0.62072(6) 0.0766(6) Uani 1 1 d . . . C45 C -0.2457(2) 1.0416(3) 0.57683(9) 0.0456(7) Uani 1 1 d . . . F45 F -0.2044(2) 1.11302(19) 0.54858(6) 0.0742(6) Uani 1 1 d . . . C46 C -0.2894(2) 0.9238(3) 0.56976(7) 0.0377(6) Uani 1 1 d . . . F46 F -0.29198(17) 0.88678(17) 0.53314(4) 0.0579(5) Uani 1 1 d . . . C61 C 0.0014(3) 0.7076(5) 0.79682(11) 0.0752(12) Uani 1 1 d . . . H61 H 0.0500 0.7120 0.8191 0.090 Uiso 1 1 calc R . . C62 C -0.0793(4) 0.7982(4) 0.78840(11) 0.0718(10) Uani 1 1 d . . . H62 H -0.0877 0.8653 0.8051 0.086 Uiso 1 1 calc R . . C63 C -0.1491(4) 0.7931(4) 0.75576(12) 0.0737(10) Uani 1 1 d . . . H63 H -0.2063 0.8557 0.7502 0.088 Uiso 1 1 calc R . . C64 C -0.1352(4) 0.6971(4) 0.73152(11) 0.0742(11) Uani 1 1 d . . . H64 H -0.1804 0.6955 0.7086 0.089 Uiso 1 1 calc R . . C65 C -0.0573(4) 0.6037(4) 0.73987(14) 0.0793(12) Uani 1 1 d . . . H65 H -0.0509 0.5359 0.7234 0.095 Uiso 1 1 calc R . . C66 C 0.0122(4) 0.6087(5) 0.77258(14) 0.0850(14) Uani 1 1 d . . . H66 H 0.0672 0.5446 0.7785 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.02442(13) 0.03336(15) 0.03879(15) -0.00465(11) 0.00597(10) -0.00054(10) N1 0.0371(12) 0.0476(14) 0.0476(13) -0.0140(12) 0.0094(10) -0.0059(11) C1 0.0319(12) 0.0410(14) 0.0271(12) -0.0071(11) 0.0032(10) -0.0018(11) C2 0.0347(13) 0.0395(14) 0.0309(13) -0.0049(11) 0.0008(10) -0.0002(11) C3 0.0312(12) 0.0310(13) 0.0314(13) -0.0017(10) 0.0053(10) 0.0021(10) C4 0.0306(13) 0.0302(13) 0.0602(18) -0.0053(13) 0.0079(12) -0.0048(11) C5 0.0359(13) 0.0308(13) 0.0450(15) -0.0025(12) 0.0131(12) -0.0044(11) C6 0.0556(18) 0.076(2) 0.0369(16) 0.0023(16) -0.0034(13) 0.0176(17) B1 0.0297(13) 0.0383(16) 0.0300(14) 0.0024(13) 0.0028(11) 0.0029(12) Si31 0.0454(4) 0.0291(4) 0.0519(5) -0.0017(3) 0.0138(4) 0.0010(3) C32 0.095(3) 0.060(2) 0.062(2) 0.0186(18) 0.011(2) 0.010(2) C33 0.055(2) 0.0412(18) 0.118(3) -0.017(2) 0.026(2) -0.0090(16) C34 0.065(2) 0.0335(16) 0.076(2) -0.0110(15) 0.0198(18) 0.0011(14) Si51 0.0538(5) 0.0601(6) 0.0489(5) 0.0120(4) 0.0120(4) -0.0006(4) C52 0.129(4) 0.090(3) 0.047(2) 0.004(2) 0.028(2) 0.023(3) C53 0.079(3) 0.183(5) 0.053(2) 0.034(3) -0.005(2) -0.014(3) C54 0.120(4) 0.071(3) 0.090(3) 0.023(2) 0.049(3) -0.007(3) C11 0.0512(17) 0.0312(14) 0.0436(16) 0.0006(12) 0.0070(13) -0.0003(12) C12 0.0395(15) 0.0367(15) 0.0592(19) -0.0035(13) 0.0108(13) 0.0085(12) C13 0.0614(19) 0.0377(16) 0.0391(16) -0.0078(12) 0.0109(14) 0.0021(14) C14 0.0479(16) 0.0308(14) 0.0537(18) -0.0062(13) -0.0063(13) -0.0040(13) C15 0.0343(14) 0.0322(14) 0.0612(19) -0.0062(13) 0.0097(13) -0.0070(11) C111 0.080(2) 0.055(2) 0.057(2) 0.0081(17) 0.0055(18) -0.0026(18) C16 0.0288(14) 0.069(2) 0.071(2) -0.0167(19) -0.0060(14) -0.0051(15) C17 0.0270(15) 0.072(2) 0.114(3) -0.029(2) -0.0055(18) 0.0090(15) C18 0.0330(17) 0.145(4) 0.074(3) -0.036(3) 0.0224(18) -0.021(2) C19 0.0437(19) 0.102(3) 0.091(3) 0.024(3) 0.005(2) -0.036(2) C20 0.0384(16) 0.057(2) 0.096(3) -0.013(2) 0.0024(18) -0.0159(15) C161 0.068(3) 0.139(4) 0.077(3) -0.012(3) -0.027(2) -0.015(3) C21 0.0297(13) 0.0379(14) 0.0418(15) 0.0026(12) 0.0091(11) 0.0010(11) C22 0.0322(14) 0.0419(15) 0.0575(19) 0.0076(14) 0.0050(13) -0.0005(12) F22 0.0539(11) 0.0729(13) 0.0497(10) 0.0050(9) -0.0115(8) 0.0065(9) C23 0.0338(15) 0.0489(19) 0.094(3) 0.0180(19) -0.0015(16) 0.0021(14) F23 0.0564(12) 0.0780(14) 0.129(2) 0.0270(14) -0.0200(13) 0.0197(11) C24 0.0423(18) 0.0466(19) 0.111(3) -0.002(2) 0.025(2) 0.0101(15) F24 0.0649(14) 0.0741(15) 0.182(3) -0.0119(16) 0.0363(16) 0.0348(12) C25 0.056(2) 0.058(2) 0.080(2) -0.0141(19) 0.0350(19) 0.0028(17) F25 0.0960(17) 0.1016(17) 0.0989(17) -0.0386(15) 0.0516(14) 0.0165(14) C26 0.0444(16) 0.0505(18) 0.0520(18) -0.0019(15) 0.0170(14) 0.0052(14) F26 0.0779(14) 0.0917(15) 0.0362(9) -0.0073(10) 0.0136(9) 0.0187(11) C41 0.0226(11) 0.0379(14) 0.0317(13) 0.0031(11) 0.0017(9) 0.0027(10) C42 0.0253(12) 0.0481(16) 0.0358(14) 0.0031(13) 0.0013(10) -0.0019(11) F42 0.0524(10) 0.0721(12) 0.0311(8) 0.0024(8) 0.0033(7) -0.0205(9) C43 0.0318(14) 0.0597(19) 0.0472(17) -0.0134(15) -0.0029(12) -0.0071(13) F43 0.0768(14) 0.0897(15) 0.0564(12) -0.0307(11) 0.0005(10) -0.0290(12) C44 0.0345(15) 0.0438(17) 0.068(2) -0.0019(15) -0.0132(14) -0.0039(12) F44 0.0749(13) 0.0500(11) 0.1038(17) -0.0030(11) -0.0234(11) -0.0233(10) C45 0.0331(14) 0.0458(17) 0.0574(19) 0.0216(15) -0.0109(13) -0.0075(12) F45 0.0764(14) 0.0760(14) 0.0694(13) 0.0385(11) -0.0171(10) -0.0319(11) C46 0.0322(13) 0.0465(16) 0.0342(14) 0.0068(12) -0.0018(11) -0.0008(12) F46 0.0684(12) 0.0734(13) 0.0319(9) 0.0088(8) 0.0025(8) -0.0139(9) C61 0.0466(19) 0.120(4) 0.059(2) 0.023(2) 0.0004(17) -0.010(2) C62 0.072(2) 0.069(2) 0.076(3) -0.003(2) 0.006(2) -0.022(2) C63 0.075(2) 0.063(2) 0.083(3) 0.010(2) -0.013(2) 0.008(2) C64 0.069(2) 0.092(3) 0.061(2) -0.010(2) -0.0050(18) 0.004(2) C65 0.069(3) 0.079(3) 0.091(3) -0.015(2) 0.023(2) 0.009(2) C66 0.054(2) 0.108(4) 0.094(3) 0.031(3) 0.020(2) 0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.004(2) . ? Zr C5 2.402(3) . ? Zr C18 2.491(3) . ? Zr C17 2.498(3) . ? Zr C15 2.511(3) . ? Zr C12 2.513(3) . ? Zr C11 2.514(3) . ? Zr C19 2.518(3) . ? Zr C13 2.525(3) . ? Zr C14 2.527(3) . ? Zr C20 2.532(3) . ? Zr C16 2.558(3) . ? N1 C1 1.265(3) . ? C1 C2 1.453(4) . ? C1 C6 1.511(4) . ? C2 C3 1.545(3) . ? C2 B1 1.606(4) . ? C3 C4 1.435(4) . ? C3 B1 1.659(4) . ? C3 Si31 1.889(3) . ? C4 C5 1.254(4) . ? C5 Si51 1.860(3) . ? B1 C41 1.604(4) . ? B1 C21 1.608(4) . ? Si31 C33 1.865(3) . ? Si31 C32 1.867(4) . ? Si31 C34 1.870(3) . ? Si51 C52 1.830(4) . ? Si51 C53 1.838(4) . ? Si51 C54 1.877(4) . ? C11 C12 1.406(4) . ? C11 C15 1.407(4) . ? C11 C111 1.499(4) . ? C12 C13 1.396(4) . ? C13 C14 1.391(4) . ? C14 C15 1.401(4) . ? C16 C20 1.379(5) . ? C16 C17 1.392(5) . ? C16 C161 1.494(5) . ? C17 C18 1.409(6) . ? C18 C19 1.386(6) . ? C19 C20 1.371(5) . ? C21 C22 1.384(4) . ? C21 C26 1.387(4) . ? C22 F22 1.349(3) . ? C22 C23 1.380(4) . ? C23 F23 1.346(4) . ? C23 C24 1.372(5) . ? C24 F24 1.336(4) . ? C24 C25 1.366(5) . ? C25 F25 1.349(4) . ? C25 C26 1.374(4) . ? C26 F26 1.348(4) . ? C41 C42 1.381(4) . ? C41 C46 1.388(4) . ? C42 F42 1.347(3) . ? C42 C43 1.381(4) . ? C43 F43 1.347(3) . ? C43 C44 1.356(4) . ? C44 F44 1.346(3) . ? C44 C45 1.365(4) . ? C45 F45 1.345(3) . ? C45 C46 1.383(4) . ? C46 F46 1.351(3) . ? C61 C62 1.349(6) . ? C61 C66 1.376(6) . ? C62 C63 1.369(5) . ? C63 C64 1.355(5) . ? C64 C65 1.351(6) . ? C65 C66 1.369(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr C5 88.05(10) . . ? N1 Zr C18 135.32(12) . . ? C5 Zr C18 102.13(15) . . ? N1 Zr C17 114.28(12) . . ? C5 Zr C17 132.50(12) . . ? C18 Zr C17 32.81(14) . . ? N1 Zr C15 79.80(9) . . ? C5 Zr C15 98.17(9) . . ? C18 Zr C15 139.30(14) . . ? C17 Zr C15 125.76(12) . . ? N1 Zr C12 120.21(10) . . ? C5 Zr C12 128.69(10) . . ? C18 Zr C12 86.86(15) . . ? C17 Zr C12 76.99(11) . . ? C15 Zr C12 53.25(9) . . ? N1 Zr C11 88.01(10) . . ? C5 Zr C11 130.19(9) . . ? C18 Zr C11 114.90(15) . . ? C17 Zr C11 93.63(12) . . ? C15 Zr C11 32.52(9) . . ? C12 Zr C11 32.48(9) . . ? N1 Zr C19 111.68(14) . . ? C5 Zr C19 80.28(12) . . ? C18 Zr C19 32.12(14) . . ? C17 Zr C19 52.93(14) . . ? C15 Zr C19 168.25(13) . . ? C12 Zr C19 118.94(14) . . ? C11 Zr C19 145.54(13) . . ? N1 Zr C13 133.02(10) . . ? C5 Zr C13 96.83(10) . . ? C18 Zr C13 89.35(13) . . ? C17 Zr C13 96.34(11) . . ? C15 Zr C13 53.22(9) . . ? C12 Zr C13 32.18(10) . . ? C11 Zr C13 53.82(9) . . ? C19 Zr C13 115.22(14) . . ? N1 Zr C14 105.37(9) . . ? C5 Zr C14 79.69(10) . . ? C18 Zr C14 119.20(12) . . ? C17 Zr C14 127.45(11) . . ? C15 Zr C14 32.29(9) . . ? C12 Zr C14 53.17(10) . . ? C11 Zr C14 53.88(10) . . ? C19 Zr C14 136.87(13) . . ? C13 Zr C14 31.97(10) . . ? N1 Zr C20 83.46(11) . . ? C5 Zr C20 92.77(11) . . ? C18 Zr C20 53.02(13) . . ? C17 Zr C20 52.45(12) . . ? C15 Zr C20 159.62(12) . . ? C12 Zr C20 129.38(11) . . ? C11 Zr C20 135.89(12) . . ? C19 Zr C20 31.50(13) . . ? C13 Zr C20 142.36(11) . . ? C14 Zr C20 168.03(12) . . ? N1 Zr C16 84.56(10) . . ? C5 Zr C16 124.18(11) . . ? C18 Zr C16 53.60(12) . . ? C17 Zr C16 31.93(11) . . ? C15 Zr C16 134.16(11) . . ? C12 Zr C16 101.93(11) . . ? C11 Zr C16 104.78(11) . . ? C19 Zr C16 52.47(13) . . ? C13 Zr C16 127.20(11) . . ? C14 Zr C16 155.01(11) . . ? C20 Zr C16 31.43(12) . . ? C1 N1 Zr 168.6(2) . . ? N1 C1 C2 121.8(2) . . ? N1 C1 C6 120.6(3) . . ? C2 C1 C6 117.6(2) . . ? C1 C2 C3 116.9(2) . . ? C1 C2 B1 123.8(2) . . ? C3 C2 B1 63.49(17) . . ? C4 C3 C2 117.6(2) . . ? C4 C3 B1 120.0(2) . . ? C2 C3 B1 60.07(16) . . ? C4 C3 Si31 110.13(17) . . ? C2 C3 Si31 115.78(17) . . ? B1 C3 Si31 124.27(17) . . ? C5 C4 C3 164.3(3) . . ? C5 C4 Zr 61.52(17) . . ? C3 C4 Zr 133.3(2) . . ? C4 C5 Si51 141.8(2) . . ? C4 C5 Zr 91.2(2) . . ? Si51 C5 Zr 126.98(13) . . ? C41 B1 C2 120.7(2) . . ? C41 B1 C21 113.6(2) . . ? C2 B1 C21 116.3(2) . . ? C41 B1 C3 120.1(2) . . ? C2 B1 C3 56.44(15) . . ? C21 B1 C3 118.3(2) . . ? C33 Si31 C32 110.18(19) . . ? C33 Si31 C34 107.67(16) . . ? C32 Si31 C34 107.83(17) . . ? C33 Si31 C3 108.24(14) . . ? C32 Si31 C3 111.14(15) . . ? C34 Si31 C3 111.72(13) . . ? C52 Si51 C53 110.0(2) . . ? C52 Si51 C5 113.02(16) . . ? C53 Si51 C5 111.12(15) . . ? C52 Si51 C54 106.8(2) . . ? C53 Si51 C54 108.7(2) . . ? C5 Si51 C54 107.01(17) . . ? C12 C11 C15 106.4(3) . . ? C12 C11 C111 126.1(3) . . ? C15 C11 C111 127.5(3) . . ? C12 C11 Zr 73.72(16) . . ? C15 C11 Zr 73.61(15) . . ? C111 C11 Zr 119.8(2) . . ? C13 C12 C11 108.9(3) . . ? C13 C12 Zr 74.36(16) . . ? C11 C12 Zr 73.80(15) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 Zr 74.11(16) . . ? C12 C13 Zr 73.46(16) . . ? C13 C14 C15 107.8(3) . . ? C13 C14 Zr 73.93(17) . . ? C15 C14 Zr 73.22(16) . . ? C14 C15 C11 108.9(2) . . ? C14 C15 Zr 74.49(16) . . ? C11 C15 Zr 73.87(15) . . ? C20 C16 C17 106.7(4) . . ? C20 C16 C161 126.5(4) . . ? C17 C16 C161 126.8(4) . . ? C20 C16 Zr 73.23(18) . . ? C17 C16 Zr 71.65(18) . . ? C161 C16 Zr 122.6(2) . . ? C16 C17 C18 108.8(4) . . ? C16 C17 Zr 76.42(17) . . ? C18 C17 Zr 73.32(19) . . ? C19 C18 C17 106.2(4) . . ? C19 C18 Zr 75.00(18) . . ? C17 C18 Zr 73.87(18) . . ? C20 C19 C18 108.9(4) . . ? C20 C19 Zr 74.82(19) . . ? C18 C19 Zr 72.9(2) . . ? C19 C20 C16 109.4(4) . . ? C19 C20 Zr 73.7(2) . . ? C16 C20 Zr 75.34(19) . . ? C22 C21 C26 113.8(3) . . ? C22 C21 B1 121.7(2) . . ? C26 C21 B1 124.5(3) . . ? F22 C22 C23 116.8(3) . . ? F22 C22 C21 119.1(2) . . ? C23 C22 C21 124.1(3) . . ? F23 C23 C24 120.0(3) . . ? F23 C23 C22 120.8(3) . . ? C24 C23 C22 119.2(3) . . ? F24 C24 C25 121.0(4) . . ? F24 C24 C23 119.8(4) . . ? C25 C24 C23 119.1(3) . . ? F25 C25 C24 119.7(3) . . ? F25 C25 C26 120.2(4) . . ? C24 C25 C26 120.1(3) . . ? F26 C26 C25 116.0(3) . . ? F26 C26 C21 120.3(3) . . ? C25 C26 C21 123.6(3) . . ? C42 C41 C46 113.1(2) . . ? C42 C41 B1 125.8(2) . . ? C46 C41 B1 120.9(2) . . ? F42 C42 C41 120.1(2) . . ? F42 C42 C43 115.8(2) . . ? C41 C42 C43 124.1(2) . . ? F43 C43 C44 119.8(3) . . ? F43 C43 C42 120.3(3) . . ? C44 C43 C42 119.8(3) . . ? F44 C44 C43 120.7(3) . . ? F44 C44 C45 119.8(3) . . ? C43 C44 C45 119.4(3) . . ? F45 C45 C44 119.7(3) . . ? F45 C45 C46 121.1(3) . . ? C44 C45 C46 119.1(3) . . ? F46 C46 C45 116.5(2) . . ? F46 C46 C41 119.2(2) . . ? C45 C46 C41 124.4(3) . . ? C62 C61 C66 119.5(4) . . ? C61 C62 C63 120.5(4) . . ? C64 C63 C62 119.5(4) . . ? C65 C64 C63 121.0(4) . . ? C64 C65 C66 119.4(4) . . ? C65 C66 C61 120.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Zr N1 C1 16.1(10) . . . . ? C18 Zr N1 C1 -89.3(10) . . . . ? C17 Zr N1 C1 -120.5(10) . . . . ? C15 Zr N1 C1 114.7(10) . . . . ? C12 Zr N1 C1 150.8(10) . . . . ? C11 Zr N1 C1 146.4(10) . . . . ? C19 Zr N1 C1 -62.7(10) . . . . ? C13 Zr N1 C1 113.6(10) . . . . ? C14 Zr N1 C1 94.8(10) . . . . ? C20 Zr N1 C1 -76.9(10) . . . . ? C16 Zr N1 C1 -108.5(10) . . . . ? Zr N1 C1 C2 -13.2(12) . . . . ? Zr N1 C1 C6 166.7(9) . . . . ? N1 C1 C2 C3 1.9(4) . . . . ? C6 C1 C2 C3 -178.1(2) . . . . ? N1 C1 C2 B1 -72.9(3) . . . . ? C6 C1 C2 B1 107.2(3) . . . . ? C1 C2 C3 C4 -5.8(3) . . . . ? B1 C2 C3 C4 110.5(3) . . . . ? C1 C2 C3 B1 -116.3(3) . . . . ? C1 C2 C3 Si31 127.3(2) . . . . ? B1 C2 C3 Si31 -116.3(2) . . . . ? C2 C3 C4 C5 169.9(9) . . . . ? B1 C3 C4 C5 -120.5(9) . . . . ? Si31 C3 C4 C5 34.3(10) . . . . ? C2 C3 C4 Zr 11.2(3) . . . . ? B1 C3 C4 Zr 80.9(3) . . . . ? Si31 C3 C4 Zr -124.38(18) . . . . ? N1 Zr C4 C5 177.3(2) . . . . ? C18 Zr C4 C5 -54.5(2) . . . . ? C17 Zr C4 C5 -88.9(2) . . . . ? C15 Zr C4 C5 101.05(18) . . . . ? C12 Zr C4 C5 74.6(2) . . . . ? C11 Zr C4 C5 112.67(18) . . . . ? C19 Zr C4 C5 -67.8(2) . . . . ? C13 Zr C4 C5 50.50(19) . . . . ? C14 Zr C4 C5 69.05(18) . . . . ? C20 Zr C4 C5 -99.27(19) . . . . ? C16 Zr C4 C5 -115.54(19) . . . . ? N1 Zr C4 C3 -9.1(2) . . . . ? C5 Zr C4 C3 173.6(3) . . . . ? C18 Zr C4 C3 119.1(2) . . . . ? C17 Zr C4 C3 84.6(3) . . . . ? C15 Zr C4 C3 -85.4(2) . . . . ? C12 Zr C4 C3 -111.8(2) . . . . ? C11 Zr C4 C3 -73.8(3) . . . . ? C19 Zr C4 C3 105.7(3) . . . . ? C13 Zr C4 C3 -135.9(2) . . . . ? C14 Zr C4 C3 -117.4(2) . . . . ? C20 Zr C4 C3 74.3(2) . . . . ? C16 Zr C4 C3 58.0(3) . . . . ? C3 C4 C5 Si51 15.5(12) . . . . ? Zr C4 C5 Si51 178.0(4) . . . . ? C3 C4 C5 Zr -162.5(9) . . . . ? N1 Zr C5 C4 -2.35(17) . . . . ? C18 Zr C5 C4 133.73(19) . . . . ? C17 Zr C5 C4 119.44(19) . . . . ? C15 Zr C5 C4 -81.76(18) . . . . ? C12 Zr C5 C4 -130.50(17) . . . . ? C11 Zr C5 C4 -88.09(19) . . . . ? C19 Zr C5 C4 110.0(2) . . . . ? C13 Zr C5 C4 -135.46(17) . . . . ? C14 Zr C5 C4 -108.36(18) . . . . ? C20 Zr C5 C4 81.00(18) . . . . ? C16 Zr C5 C4 79.73(19) . . . . ? N1 Zr C5 Si51 179.20(16) . . . . ? C18 Zr C5 Si51 -44.72(19) . . . . ? C17 Zr C5 Si51 -59.0(2) . . . . ? C15 Zr C5 Si51 99.79(16) . . . . ? C12 Zr C5 Si51 51.0(2) . . . . ? C11 Zr C5 Si51 93.46(17) . . . . ? C19 Zr C5 Si51 -68.42(19) . . . . ? C13 Zr C5 Si51 46.09(17) . . . . ? C14 Zr C5 Si51 73.19(16) . . . . ? C20 Zr C5 Si51 -97.45(17) . . . . ? C16 Zr C5 Si51 -98.72(17) . . . . ? C1 C2 B1 C41 -1.9(4) . . . . ? C3 C2 B1 C41 -107.8(2) . . . . ? C1 C2 B1 C21 -146.2(2) . . . . ? C3 C2 B1 C21 107.9(2) . . . . ? C1 C2 B1 C3 105.9(3) . . . . ? C4 C3 B1 C41 2.3(4) . . . . ? C2 C3 B1 C41 108.8(3) . . . . ? Si31 C3 B1 C41 -148.75(19) . . . . ? C4 C3 B1 C2 -106.6(3) . . . . ? Si31 C3 B1 C2 102.4(2) . . . . ? C4 C3 B1 C21 149.2(3) . . . . ? C2 C3 B1 C21 -104.2(3) . . . . ? Si31 C3 B1 C21 -1.8(3) . . . . ? C4 C3 Si31 C33 48.2(2) . . . . ? C2 C3 Si31 C33 -88.3(2) . . . . ? B1 C3 Si31 C33 -158.3(2) . . . . ? C4 C3 Si31 C32 -72.9(2) . . . . ? C2 C3 Si31 C32 150.6(2) . . . . ? B1 C3 Si31 C32 80.6(2) . . . . ? C4 C3 Si31 C34 166.6(2) . . . . ? C2 C3 Si31 C34 30.1(2) . . . . ? B1 C3 Si31 C34 -39.9(3) . . . . ? C4 C5 Si51 C52 174.9(4) . . . . ? Zr C5 Si51 C52 -7.6(3) . . . . ? C4 C5 Si51 C53 50.7(4) . . . . ? Zr C5 Si51 C53 -131.8(2) . . . . ? C4 C5 Si51 C54 -67.8(4) . . . . ? Zr C5 Si51 C54 109.7(2) . . . . ? N1 Zr C11 C12 172.90(19) . . . . ? C5 Zr C11 C12 -101.3(2) . . . . ? C18 Zr C11 C12 32.7(2) . . . . ? C17 Zr C11 C12 58.7(2) . . . . ? C15 Zr C11 C12 -113.1(3) . . . . ? C19 Zr C11 C12 45.8(3) . . . . ? C13 Zr C11 C12 -36.51(18) . . . . ? C14 Zr C11 C12 -76.39(19) . . . . ? C20 Zr C11 C12 94.4(2) . . . . ? C16 Zr C11 C12 89.05(19) . . . . ? N1 Zr C11 C15 -74.04(17) . . . . ? C5 Zr C11 C15 11.7(2) . . . . ? C18 Zr C11 C15 145.77(18) . . . . ? C17 Zr C11 C15 171.75(18) . . . . ? C12 Zr C11 C15 113.1(3) . . . . ? C19 Zr C11 C15 158.9(2) . . . . ? C13 Zr C11 C15 76.55(18) . . . . ? C14 Zr C11 C15 36.67(16) . . . . ? C20 Zr C11 C15 -152.53(18) . . . . ? C16 Zr C11 C15 -157.88(17) . . . . ? N1 Zr C11 C111 50.2(2) . . . . ? C5 Zr C11 C111 136.0(2) . . . . ? C18 Zr C11 C111 -90.0(3) . . . . ? C17 Zr C11 C111 -64.0(3) . . . . ? C15 Zr C11 C111 124.3(3) . . . . ? C12 Zr C11 C111 -122.7(3) . . . . ? C19 Zr C11 C111 -76.8(3) . . . . ? C13 Zr C11 C111 -159.2(3) . . . . ? C14 Zr C11 C111 160.9(3) . . . . ? C20 Zr C11 C111 -28.3(3) . . . . ? C16 Zr C11 C111 -33.6(3) . . . . ? C15 C11 C12 C13 -0.3(3) . . . . ? C111 C11 C12 C13 -178.0(3) . . . . ? Zr C11 C12 C13 66.6(2) . . . . ? C15 C11 C12 Zr -66.91(19) . . . . ? C111 C11 C12 Zr 115.4(3) . . . . ? N1 Zr C12 C13 -123.84(18) . . . . ? C5 Zr C12 C13 -9.3(2) . . . . ? C18 Zr C12 C13 93.8(2) . . . . ? C17 Zr C12 C13 125.4(2) . . . . ? C15 Zr C12 C13 -77.50(19) . . . . ? C11 Zr C12 C13 -115.6(3) . . . . ? C19 Zr C12 C13 92.0(2) . . . . ? C14 Zr C12 C13 -36.87(17) . . . . ? C20 Zr C12 C13 128.3(2) . . . . ? C16 Zr C12 C13 145.53(18) . . . . ? N1 Zr C12 C11 -8.2(2) . . . . ? C5 Zr C12 C11 106.35(19) . . . . ? C18 Zr C12 C11 -150.6(2) . . . . ? C17 Zr C12 C11 -118.9(2) . . . . ? C15 Zr C12 C11 38.12(18) . . . . ? C19 Zr C12 C11 -152.36(19) . . . . ? C13 Zr C12 C11 115.6(3) . . . . ? C14 Zr C12 C11 78.8(2) . . . . ? C20 Zr C12 C11 -116.1(2) . . . . ? C16 Zr C12 C11 -98.85(19) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? Zr C12 C13 C14 66.6(2) . . . . ? C11 C12 C13 Zr -66.3(2) . . . . ? N1 Zr C13 C14 -35.9(2) . . . . ? C5 Zr C13 C14 57.84(18) . . . . ? C18 Zr C13 C14 160.0(2) . . . . ? C17 Zr C13 C14 -167.9(2) . . . . ? C15 Zr C13 C14 -37.27(17) . . . . ? C12 Zr C13 C14 -114.9(3) . . . . ? C11 Zr C13 C14 -78.02(19) . . . . ? C19 Zr C13 C14 140.28(19) . . . . ? C20 Zr C13 C14 161.4(2) . . . . ? C16 Zr C13 C14 -158.92(18) . . . . ? N1 Zr C13 C12 79.0(2) . . . . ? C5 Zr C13 C12 172.73(17) . . . . ? C18 Zr C13 C12 -85.1(2) . . . . ? C17 Zr C13 C12 -53.0(2) . . . . ? C15 Zr C13 C12 77.61(18) . . . . ? C11 Zr C13 C12 36.86(17) . . . . ? C19 Zr C13 C12 -104.8(2) . . . . ? C14 Zr C13 C12 114.9(3) . . . . ? C20 Zr C13 C12 -83.7(2) . . . . ? C16 Zr C13 C12 -44.0(2) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? Zr C13 C14 C15 65.92(19) . . . . ? C12 C13 C14 Zr -66.2(2) . . . . ? N1 Zr C14 C13 153.62(18) . . . . ? C5 Zr C14 C13 -121.31(18) . . . . ? C18 Zr C14 C13 -23.1(2) . . . . ? C17 Zr C14 C13 15.2(3) . . . . ? C15 Zr C14 C13 114.8(3) . . . . ? C12 Zr C14 C13 37.13(17) . . . . ? C11 Zr C14 C13 77.82(19) . . . . ? C19 Zr C14 C13 -57.7(3) . . . . ? C20 Zr C14 C13 -69.7(6) . . . . ? C16 Zr C14 C13 42.7(3) . . . . ? N1 Zr C14 C15 38.86(19) . . . . ? C5 Zr C14 C15 123.93(18) . . . . ? C18 Zr C14 C15 -137.8(2) . . . . ? C17 Zr C14 C15 -99.5(2) . . . . ? C12 Zr C14 C15 -77.64(18) . . . . ? C11 Zr C14 C15 -36.95(16) . . . . ? C19 Zr C14 C15 -172.5(2) . . . . ? C13 Zr C14 C15 -114.8(3) . . . . ? C20 Zr C14 C15 175.5(5) . . . . ? C16 Zr C14 C15 -72.1(3) . . . . ? C13 C14 C15 C11 0.1(3) . . . . ? Zr C14 C15 C11 66.46(19) . . . . ? C13 C14 C15 Zr -66.4(2) . . . . ? C12 C11 C15 C14 0.1(3) . . . . ? C111 C11 C15 C14 177.8(3) . . . . ? Zr C11 C15 C14 -66.87(19) . . . . ? C12 C11 C15 Zr 66.99(19) . . . . ? C111 C11 C15 Zr -115.3(3) . . . . ? N1 Zr C15 C14 -142.07(18) . . . . ? C5 Zr C15 C14 -55.56(18) . . . . ? C18 Zr C15 C14 63.9(3) . . . . ? C17 Zr C15 C14 105.3(2) . . . . ? C12 Zr C15 C14 77.36(18) . . . . ? C11 Zr C15 C14 115.4(2) . . . . ? C19 Zr C15 C14 26.0(7) . . . . ? C13 Zr C15 C14 36.88(17) . . . . ? C20 Zr C15 C14 -177.3(3) . . . . ? C16 Zr C15 C14 145.92(18) . . . . ? N1 Zr C15 C11 102.50(18) . . . . ? C5 Zr C15 C11 -170.99(16) . . . . ? C18 Zr C15 C11 -51.5(3) . . . . ? C17 Zr C15 C11 -10.2(2) . . . . ? C12 Zr C15 C11 -38.06(16) . . . . ? C19 Zr C15 C11 -89.5(6) . . . . ? C13 Zr C15 C11 -78.54(18) . . . . ? C14 Zr C15 C11 -115.4(2) . . . . ? C20 Zr C15 C11 67.2(4) . . . . ? C16 Zr C15 C11 30.5(2) . . . . ? N1 Zr C16 C20 86.4(2) . . . . ? C5 Zr C16 C20 2.4(3) . . . . ? C18 Zr C16 C20 -76.9(3) . . . . ? C17 Zr C16 C20 -114.6(3) . . . . ? C15 Zr C16 C20 156.5(2) . . . . ? C12 Zr C16 C20 -153.9(2) . . . . ? C11 Zr C16 C20 172.8(2) . . . . ? C19 Zr C16 C20 -36.4(2) . . . . ? C13 Zr C16 C20 -131.6(2) . . . . ? C14 Zr C16 C20 -158.4(2) . . . . ? N1 Zr C16 C17 -159.1(3) . . . . ? C5 Zr C16 C17 117.0(2) . . . . ? C18 Zr C16 C17 37.7(3) . . . . ? C15 Zr C16 C17 -89.0(3) . . . . ? C12 Zr C16 C17 -39.3(3) . . . . ? C11 Zr C16 C17 -72.6(3) . . . . ? C19 Zr C16 C17 78.2(3) . . . . ? C13 Zr C16 C17 -17.1(3) . . . . ? C14 Zr C16 C17 -43.8(4) . . . . ? C20 Zr C16 C17 114.6(3) . . . . ? N1 Zr C16 C161 -36.6(3) . . . . ? C5 Zr C16 C161 -120.5(3) . . . . ? C18 Zr C16 C161 160.2(4) . . . . ? C17 Zr C16 C161 122.5(5) . . . . ? C15 Zr C16 C161 33.5(4) . . . . ? C12 Zr C16 C161 83.2(3) . . . . ? C11 Zr C16 C161 49.9(3) . . . . ? C19 Zr C16 C161 -159.4(4) . . . . ? C13 Zr C16 C161 105.4(3) . . . . ? C14 Zr C16 C161 78.6(4) . . . . ? C20 Zr C16 C161 -123.0(4) . . . . ? C20 C16 C17 C18 -1.4(4) . . . . ? C161 C16 C17 C18 175.8(3) . . . . ? Zr C16 C17 C18 -66.8(2) . . . . ? C20 C16 C17 Zr 65.4(2) . . . . ? C161 C16 C17 Zr -117.4(3) . . . . ? N1 Zr C17 C16 23.0(3) . . . . ? C5 Zr C17 C16 -88.3(3) . . . . ? C18 Zr C17 C16 -114.7(4) . . . . ? C15 Zr C17 C16 117.9(2) . . . . ? C12 Zr C17 C16 140.5(3) . . . . ? C11 Zr C17 C16 112.4(2) . . . . ? C19 Zr C17 C16 -76.6(3) . . . . ? C13 Zr C17 C16 166.4(2) . . . . ? C14 Zr C17 C16 158.4(2) . . . . ? C20 Zr C17 C16 -36.7(2) . . . . ? N1 Zr C17 C18 137.7(3) . . . . ? C5 Zr C17 C18 26.4(3) . . . . ? C15 Zr C17 C18 -127.4(3) . . . . ? C12 Zr C17 C18 -104.8(3) . . . . ? C11 Zr C17 C18 -132.8(3) . . . . ? C19 Zr C17 C18 38.1(2) . . . . ? C13 Zr C17 C18 -78.9(3) . . . . ? C14 Zr C17 C18 -86.9(3) . . . . ? C20 Zr C17 C18 78.0(3) . . . . ? C16 Zr C17 C18 114.7(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? Zr C17 C18 C19 -68.6(2) . . . . ? C16 C17 C18 Zr 68.8(2) . . . . ? N1 Zr C18 C19 51.5(4) . . . . ? C5 Zr C18 C19 -48.2(3) . . . . ? C17 Zr C18 C19 112.2(4) . . . . ? C15 Zr C18 C19 -166.4(2) . . . . ? C12 Zr C18 C19 -177.1(3) . . . . ? C11 Zr C18 C19 166.0(2) . . . . ? C13 Zr C18 C19 -145.0(3) . . . . ? C14 Zr C18 C19 -133.0(2) . . . . ? C20 Zr C18 C19 36.1(2) . . . . ? C16 Zr C18 C19 75.6(3) . . . . ? N1 Zr C18 C17 -60.7(4) . . . . ? C5 Zr C18 C17 -160.4(2) . . . . ? C15 Zr C18 C17 81.4(3) . . . . ? C12 Zr C18 C17 70.7(3) . . . . ? C11 Zr C18 C17 53.8(3) . . . . ? C19 Zr C18 C17 -112.2(4) . . . . ? C13 Zr C18 C17 102.8(3) . . . . ? C14 Zr C18 C17 114.8(2) . . . . ? C20 Zr C18 C17 -76.1(2) . . . . ? C16 Zr C18 C17 -36.6(2) . . . . ? C17 C18 C19 C20 1.1(4) . . . . ? Zr C18 C19 C20 -66.7(2) . . . . ? C17 C18 C19 Zr 67.8(2) . . . . ? N1 Zr C19 C20 -28.0(3) . . . . ? C5 Zr C19 C20 -111.9(3) . . . . ? C18 Zr C19 C20 115.7(4) . . . . ? C17 Zr C19 C20 76.8(3) . . . . ? C15 Zr C19 C20 164.7(5) . . . . ? C12 Zr C19 C20 119.0(3) . . . . ? C11 Zr C19 C20 92.9(3) . . . . ? C13 Zr C19 C20 155.1(2) . . . . ? C14 Zr C19 C20 -175.3(2) . . . . ? C16 Zr C19 C20 36.3(2) . . . . ? N1 Zr C19 C18 -143.7(3) . . . . ? C5 Zr C19 C18 132.4(3) . . . . ? C17 Zr C19 C18 -39.0(2) . . . . ? C15 Zr C19 C18 49.0(7) . . . . ? C12 Zr C19 C18 3.3(3) . . . . ? C11 Zr C19 C18 -22.8(4) . . . . ? C13 Zr C19 C18 39.3(3) . . . . ? C14 Zr C19 C18 69.0(3) . . . . ? C20 Zr C19 C18 -115.7(4) . . . . ? C16 Zr C19 C18 -79.4(3) . . . . ? C18 C19 C20 C16 -2.0(4) . . . . ? Zr C19 C20 C16 -67.5(2) . . . . ? C18 C19 C20 Zr 65.5(2) . . . . ? C17 C16 C20 C19 2.1(4) . . . . ? C161 C16 C20 C19 -175.1(3) . . . . ? Zr C16 C20 C19 66.4(2) . . . . ? C17 C16 C20 Zr -64.3(2) . . . . ? C161 C16 C20 Zr 118.5(3) . . . . ? N1 Zr C20 C19 154.0(3) . . . . ? C5 Zr C20 C19 66.3(3) . . . . ? C18 Zr C20 C19 -36.8(3) . . . . ? C17 Zr C20 C19 -78.4(3) . . . . ? C15 Zr C20 C19 -171.1(3) . . . . ? C12 Zr C20 C19 -81.9(3) . . . . ? C11 Zr C20 C19 -125.7(3) . . . . ? C13 Zr C20 C19 -38.7(4) . . . . ? C14 Zr C20 C19 15.7(7) . . . . ? C16 Zr C20 C19 -115.8(3) . . . . ? N1 Zr C20 C16 -90.3(2) . . . . ? C5 Zr C20 C16 -178.0(2) . . . . ? C18 Zr C20 C16 78.9(3) . . . . ? C17 Zr C20 C16 37.3(2) . . . . ? C15 Zr C20 C16 -55.4(4) . . . . ? C12 Zr C20 C16 33.9(3) . . . . ? C11 Zr C20 C16 -10.0(3) . . . . ? C19 Zr C20 C16 115.8(3) . . . . ? C13 Zr C20 C16 77.1(3) . . . . ? C14 Zr C20 C16 131.5(5) . . . . ? C41 B1 C21 C22 72.7(3) . . . . ? C2 B1 C21 C22 -140.6(3) . . . . ? C3 B1 C21 C22 -76.3(3) . . . . ? C41 B1 C21 C26 -108.9(3) . . . . ? C2 B1 C21 C26 37.9(4) . . . . ? C3 B1 C21 C26 102.1(3) . . . . ? C26 C21 C22 F22 177.8(2) . . . . ? B1 C21 C22 F22 -3.6(4) . . . . ? C26 C21 C22 C23 -3.5(4) . . . . ? B1 C21 C22 C23 175.1(3) . . . . ? F22 C22 C23 F23 0.7(4) . . . . ? C21 C22 C23 F23 -178.0(3) . . . . ? F22 C22 C23 C24 -179.5(3) . . . . ? C21 C22 C23 C24 1.8(5) . . . . ? F23 C23 C24 F24 1.0(5) . . . . ? C22 C23 C24 F24 -178.8(3) . . . . ? F23 C23 C24 C25 -179.7(3) . . . . ? C22 C23 C24 C25 0.4(5) . . . . ? F24 C24 C25 F25 -0.2(5) . . . . ? C23 C24 C25 F25 -179.5(3) . . . . ? F24 C24 C25 C26 178.5(3) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? F25 C25 C26 F26 -0.7(5) . . . . ? C24 C25 C26 F26 -179.5(3) . . . . ? F25 C25 C26 C21 177.5(3) . . . . ? C24 C25 C26 C21 -1.2(5) . . . . ? C22 C21 C26 F26 -178.6(3) . . . . ? B1 C21 C26 F26 2.8(4) . . . . ? C22 C21 C26 C25 3.2(4) . . . . ? B1 C21 C26 C25 -175.3(3) . . . . ? C2 B1 C41 C42 114.7(3) . . . . ? C21 B1 C41 C42 -100.2(3) . . . . ? C3 B1 C41 C42 48.2(4) . . . . ? C2 B1 C41 C46 -70.5(3) . . . . ? C21 B1 C41 C46 74.6(3) . . . . ? C3 B1 C41 C46 -137.0(2) . . . . ? C46 C41 C42 F42 -176.5(2) . . . . ? B1 C41 C42 F42 -1.3(4) . . . . ? C46 C41 C42 C43 3.3(4) . . . . ? B1 C41 C42 C43 178.4(2) . . . . ? F42 C42 C43 F43 -2.4(4) . . . . ? C41 C42 C43 F43 177.9(2) . . . . ? F42 C42 C43 C44 176.9(2) . . . . ? C41 C42 C43 C44 -2.9(4) . . . . ? F43 C43 C44 F44 1.2(4) . . . . ? C42 C43 C44 F44 -178.1(3) . . . . ? F43 C43 C44 C45 179.6(3) . . . . ? C42 C43 C44 C45 0.3(4) . . . . ? F44 C44 C45 F45 2.4(4) . . . . ? C43 C44 C45 F45 -176.1(3) . . . . ? F44 C44 C45 C46 179.8(2) . . . . ? C43 C44 C45 C46 1.3(4) . . . . ? F45 C45 C46 F46 -2.1(4) . . . . ? C44 C45 C46 F46 -179.4(2) . . . . ? F45 C45 C46 C41 176.7(2) . . . . ? C44 C45 C46 C41 -0.7(4) . . . . ? C42 C41 C46 F46 177.2(2) . . . . ? B1 C41 C46 F46 1.8(4) . . . . ? C42 C41 C46 C45 -1.5(4) . . . . ? B1 C41 C46 C45 -176.9(2) . . . . ? C66 C61 C62 C63 -0.9(6) . . . . ? C61 C62 C63 C64 -1.1(6) . . . . ? C62 C63 C64 C65 2.9(6) . . . . ? C63 C64 C65 C66 -2.7(6) . . . . ? C64 C65 C66 C61 0.7(6) . . . . ? C62 C61 C66 C65 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.704 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.094