# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Kehr, Gerald' 'Erker, G' 'Frohlich, Roland' 'Petersen, Jeffrey' 'Bender, Georg' data_erk5953 _database_code_depnum_ccdc_archive 'CCDC 886395' #TrackingRef '- erk5953.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Si2 Zr' _chemical_formula_weight 497.96 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2000(2) _cell_length_b 11.8746(2) _cell_length_c 14.0316(4) _cell_angle_alpha 101.4430(10) _cell_angle_beta 95.9030(10) _cell_angle_gamma 98.217(2) _cell_volume 1313.20(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2666 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7998 _exptl_absorpt_correction_T_max 0.8597 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10381 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4388 _reflns_number_gt 4280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.7926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4388 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.20396(2) 0.398972(15) 0.702405(13) 0.02535(9) Uani 1 1 d . . . Si1 Si 0.47646(7) 0.71993(5) 0.76056(5) 0.03345(15) Uani 1 1 d . . . Si2 Si -0.02907(8) 0.10466(5) 0.71950(5) 0.03385(15) Uani 1 1 d . . . C1 C 0.3912(3) 0.57303(19) 0.77711(16) 0.0328(4) Uani 1 1 d . . . C2 C 0.4070(2) 0.50859(19) 0.83841(16) 0.0317(4) Uani 1 1 d . . . C3 C 0.3908(3) 0.41082(19) 0.87503(16) 0.0328(4) Uani 1 1 d . . . C4 C 0.2568(3) 0.38188(19) 0.93677(16) 0.0341(5) Uani 1 1 d . . . H4A H 0.1901 0.4444 0.9474 0.041 Uiso 1 1 calc R . . H4B H 0.3067 0.3730 1.0008 0.041 Uiso 1 1 calc R . . C5 C 0.1475(3) 0.26768(18) 0.88111(15) 0.0308(4) Uani 1 1 d . . . C6 C 0.1125(2) 0.24522(17) 0.78220(15) 0.0285(4) Uani 1 1 d . . . C7 C 0.5310(3) 0.3421(2) 0.88049(19) 0.0432(5) Uani 1 1 d . . . H7A H 0.6132 0.3669 0.8406 0.065 Uiso 1 1 calc R . . H7B H 0.4878 0.2598 0.8563 0.065 Uiso 1 1 calc R . . H7C H 0.5822 0.3553 0.9481 0.065 Uiso 1 1 calc R . . C8 C 0.0943(3) 0.1912(2) 0.94969(16) 0.0378(5) Uani 1 1 d . . . C9 C -0.0316(4) 0.2299(3) 1.0128(2) 0.0552(7) Uani 1 1 d . . . H9A H -0.0557 0.1752 1.0544 0.083 Uiso 1 1 calc R . . H9B H -0.1328 0.2329 0.9716 0.083 Uiso 1 1 calc R . . H9C H 0.0117 0.3066 1.0533 0.083 Uiso 1 1 calc R . . C10 C 0.1685(4) 0.1008(2) 0.9599(2) 0.0503(6) Uani 1 1 d . . . H10A H 0.1420 0.0591 1.0082 0.060 Uiso 1 1 calc R . . H10B H 0.2474 0.0788 0.9189 0.060 Uiso 1 1 calc R . . C11 C -0.0824(3) 0.4069(2) 0.61861(18) 0.0395(5) Uani 1 1 d . . . H11 H -0.1208 0.3549 0.5580 0.047 Uiso 1 1 calc R . . C12 C -0.1090(3) 0.3871(2) 0.71069(18) 0.0379(5) Uani 1 1 d . . . H12 H -0.1686 0.3191 0.7232 0.045 Uiso 1 1 calc R . . C13 C -0.0313(3) 0.4866(2) 0.78218(18) 0.0375(5) Uani 1 1 d . . . H13 H -0.0284 0.4958 0.8505 0.045 Uiso 1 1 calc R . . C14 C 0.0406(3) 0.5692(2) 0.73341(18) 0.0381(5) Uani 1 1 d . . . H14 H 0.0974 0.6445 0.7631 0.046 Uiso 1 1 calc R . . C15 C 0.0133(3) 0.5200(2) 0.63294(18) 0.0398(5) Uani 1 1 d . . . H15 H 0.0515 0.5556 0.5834 0.048 Uiso 1 1 calc R . . C16 C 0.2085(3) 0.2926(2) 0.52805(17) 0.0469(6) Uani 1 1 d . . . H16 H 0.1069 0.2707 0.4862 0.056 Uiso 1 1 calc R . . C17 C 0.2774(3) 0.2252(2) 0.58690(19) 0.0452(6) Uani 1 1 d . . . H17 H 0.2305 0.1501 0.5921 0.054 Uiso 1 1 calc R . . C18 C 0.4297(3) 0.2896(2) 0.63725(19) 0.0463(6) Uani 1 1 d . . . H18 H 0.5021 0.2654 0.6826 0.056 Uiso 1 1 calc R . . C19 C 0.4542(3) 0.3956(2) 0.6082(2) 0.0482(6) Uani 1 1 d . . . H19 H 0.5473 0.4549 0.6294 0.058 Uiso 1 1 calc R . . C20 C 0.3167(4) 0.3982(2) 0.54206(19) 0.0494(6) Uani 1 1 d . . . H20 H 0.2996 0.4604 0.5121 0.059 Uiso 1 1 calc R . . C21 C 0.3809(4) 0.7460(2) 0.6420(2) 0.0508(6) Uani 1 1 d . . . H21A H 0.3955 0.6842 0.5886 0.076 Uiso 1 1 calc R . . H21B H 0.4342 0.8203 0.6322 0.076 Uiso 1 1 calc R . . H21C H 0.2631 0.7469 0.6438 0.076 Uiso 1 1 calc R . . C22 C 0.7032(3) 0.7238(2) 0.7578(2) 0.0506(6) Uani 1 1 d . . . H22A H 0.7542 0.7114 0.8196 0.076 Uiso 1 1 calc R . . H22B H 0.7530 0.7990 0.7480 0.076 Uiso 1 1 calc R . . H22C H 0.7209 0.6629 0.7045 0.076 Uiso 1 1 calc R . . C23 C 0.4355(3) 0.8331(2) 0.8637(2) 0.0500(6) Uani 1 1 d . . . H23A H 0.3165 0.8302 0.8626 0.075 Uiso 1 1 calc R . . H23B H 0.4862 0.9095 0.8568 0.075 Uiso 1 1 calc R . . H23C H 0.4825 0.8185 0.9256 0.075 Uiso 1 1 calc R . . C24 C -0.1309(3) 0.1010(2) 0.59153(19) 0.0494(6) Uani 1 1 d . . . H24A H -0.0462 0.1218 0.5517 0.074 Uiso 1 1 calc R . . H24B H -0.2077 0.1562 0.5948 0.074 Uiso 1 1 calc R . . H24C H -0.1909 0.0233 0.5625 0.074 Uiso 1 1 calc R . . C25 C -0.2160(3) 0.0690(2) 0.7830(2) 0.0491(6) Uani 1 1 d . . . H25A H -0.2947 0.0061 0.7400 0.074 Uiso 1 1 calc R . . H25B H -0.2685 0.1374 0.7985 0.074 Uiso 1 1 calc R . . H25C H -0.1808 0.0452 0.8430 0.074 Uiso 1 1 calc R . . C26 C 0.0854(4) -0.0230(2) 0.7056(2) 0.0558(7) Uani 1 1 d . . . H26A H 0.1931 -0.0007 0.6857 0.084 Uiso 1 1 calc R . . H26B H 0.0214 -0.0874 0.6562 0.084 Uiso 1 1 calc R . . H26C H 0.1007 -0.0467 0.7678 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02435(13) 0.02884(14) 0.02400(13) 0.00676(9) 0.00422(8) 0.00605(8) Si1 0.0327(3) 0.0301(3) 0.0402(3) 0.0122(3) 0.0075(3) 0.0059(2) Si2 0.0370(3) 0.0279(3) 0.0336(3) 0.0026(2) 0.0033(2) 0.0019(2) C1 0.0287(10) 0.0356(11) 0.0352(11) 0.0093(9) 0.0058(8) 0.0055(8) C2 0.0263(10) 0.0335(11) 0.0307(10) 0.0034(9) -0.0016(8) -0.0009(8) C3 0.0343(11) 0.0316(11) 0.0300(10) 0.0068(8) -0.0010(8) 0.0007(8) C4 0.0397(12) 0.0330(11) 0.0282(10) 0.0079(9) 0.0020(9) 0.0015(9) C5 0.0342(11) 0.0298(10) 0.0293(10) 0.0080(8) 0.0053(8) 0.0051(8) C6 0.0281(10) 0.0267(10) 0.0311(10) 0.0069(8) 0.0047(8) 0.0045(8) C7 0.0377(12) 0.0476(14) 0.0457(14) 0.0160(11) -0.0010(10) 0.0077(10) C8 0.0412(12) 0.0387(12) 0.0300(11) 0.0091(9) 0.0023(9) -0.0059(9) C9 0.0631(17) 0.0564(16) 0.0447(14) 0.0076(12) 0.0217(13) 0.0001(13) C10 0.0561(15) 0.0456(14) 0.0513(15) 0.0246(12) -0.0008(12) 0.0019(11) C11 0.0300(11) 0.0485(13) 0.0397(12) 0.0095(10) -0.0026(9) 0.0107(9) C12 0.0237(10) 0.0445(13) 0.0500(13) 0.0171(11) 0.0069(9) 0.0097(9) C13 0.0355(11) 0.0432(13) 0.0391(12) 0.0102(10) 0.0120(9) 0.0172(9) C14 0.0327(11) 0.0356(12) 0.0484(13) 0.0087(10) 0.0050(10) 0.0147(9) C15 0.0338(11) 0.0494(13) 0.0438(13) 0.0229(11) 0.0036(10) 0.0151(10) C16 0.0447(13) 0.0672(17) 0.0263(11) -0.0010(11) 0.0061(10) 0.0155(12) C17 0.0539(15) 0.0375(12) 0.0449(13) 0.0002(10) 0.0240(11) 0.0105(10) C18 0.0406(13) 0.0652(17) 0.0383(13) 0.0065(12) 0.0116(10) 0.0283(12) C19 0.0375(13) 0.0565(16) 0.0478(14) 0.0005(12) 0.0210(11) 0.0027(11) C20 0.0648(17) 0.0577(16) 0.0370(13) 0.0179(11) 0.0278(12) 0.0220(13) C21 0.0597(16) 0.0466(14) 0.0508(15) 0.0226(12) 0.0045(12) 0.0096(12) C22 0.0381(13) 0.0466(14) 0.0713(18) 0.0178(13) 0.0168(12) 0.0067(10) C23 0.0506(15) 0.0404(13) 0.0578(16) 0.0044(12) 0.0136(12) 0.0078(11) C24 0.0524(15) 0.0474(14) 0.0386(13) 0.0008(11) -0.0040(11) -0.0047(11) C25 0.0420(13) 0.0480(14) 0.0525(15) 0.0088(12) 0.0070(11) -0.0053(10) C26 0.0662(18) 0.0380(14) 0.0603(17) 0.0006(12) 0.0045(14) 0.0163(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C1 2.373(2) . ? Zr1 C6 2.396(2) . ? Zr1 C2 2.419(2) . ? Zr1 C20 2.518(2) . ? Zr1 C15 2.519(2) . ? Zr1 C16 2.528(2) . ? Zr1 C11 2.539(2) . ? Zr1 C17 2.545(2) . ? Zr1 C18 2.552(2) . ? Zr1 C19 2.554(2) . ? Zr1 C12 2.566(2) . ? Zr1 C14 2.571(2) . ? Si1 C1 1.852(2) . ? Si1 C22 1.858(3) . ? Si1 C23 1.863(3) . ? Si1 C21 1.866(3) . ? Si2 C26 1.883(3) . ? Si2 C6 1.887(2) . ? Si2 C25 1.889(3) . ? Si2 C24 1.890(3) . ? C1 C2 1.268(3) . ? C2 C3 1.355(3) . ? C3 C7 1.506(3) . ? C3 C4 1.511(3) . ? C4 C5 1.530(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.352(3) . ? C5 C8 1.503(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C10 1.332(4) . ? C8 C9 1.490(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9400 . ? C10 H10B 0.9400 . ? C11 C12 1.391(3) . ? C11 C15 1.422(3) . ? C11 H11 0.9400 . ? C12 C13 1.411(3) . ? C12 H12 0.9400 . ? C13 C14 1.401(3) . ? C13 H13 0.9400 . ? C14 C15 1.396(4) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.391(4) . ? C16 C20 1.396(4) . ? C16 H16 0.9400 . ? C17 C18 1.405(4) . ? C17 H17 0.9400 . ? C18 C19 1.392(4) . ? C18 H18 0.9400 . ? C19 C20 1.393(4) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zr1 C6 125.53(7) . . ? C1 Zr1 C2 30.68(8) . . ? C6 Zr1 C2 95.51(7) . . ? C1 Zr1 C20 90.47(9) . . ? C6 Zr1 C20 132.15(8) . . ? C2 Zr1 C20 110.65(9) . . ? C1 Zr1 C15 88.85(8) . . ? C6 Zr1 C15 123.88(7) . . ? C2 Zr1 C15 113.83(8) . . ? C20 Zr1 C15 81.72(9) . . ? C1 Zr1 C16 122.30(8) . . ? C6 Zr1 C16 103.21(8) . . ? C2 Zr1 C16 136.52(8) . . ? C20 Zr1 C16 32.12(9) . . ? C15 Zr1 C16 87.45(9) . . ? C1 Zr1 C11 120.63(8) . . ? C6 Zr1 C11 95.63(7) . . ? C2 Zr1 C11 139.76(8) . . ? C20 Zr1 C11 89.41(9) . . ? C15 Zr1 C11 32.65(8) . . ? C16 Zr1 C11 77.30(8) . . ? C1 Zr1 C17 125.18(8) . . ? C6 Zr1 C17 79.48(8) . . ? C2 Zr1 C17 119.57(8) . . ? C20 Zr1 C17 52.90(9) . . ? C15 Zr1 C17 118.41(9) . . ? C16 Zr1 C17 31.84(9) . . ? C11 Zr1 C17 100.46(9) . . ? C1 Zr1 C18 94.49(8) . . ? C6 Zr1 C18 90.21(8) . . ? C2 Zr1 C18 88.77(8) . . ? C20 Zr1 C18 52.77(9) . . ? C15 Zr1 C18 134.33(8) . . ? C16 Zr1 C18 52.82(8) . . ? C11 Zr1 C18 129.68(8) . . ? C17 Zr1 C18 32.00(9) . . ? C1 Zr1 C19 74.48(8) . . ? C6 Zr1 C19 121.77(8) . . ? C2 Zr1 C19 83.96(8) . . ? C20 Zr1 C19 31.87(9) . . ? C15 Zr1 C19 108.55(9) . . ? C16 Zr1 C19 52.79(9) . . ? C11 Zr1 C19 121.28(9) . . ? C17 Zr1 C19 52.67(8) . . ? C18 Zr1 C19 31.65(9) . . ? C1 Zr1 C12 120.38(7) . . ? C6 Zr1 C12 70.98(7) . . ? C2 Zr1 C12 121.22(8) . . ? C20 Zr1 C12 120.56(9) . . ? C15 Zr1 C12 52.96(8) . . ? C16 Zr1 C12 102.02(8) . . ? C11 Zr1 C12 31.62(8) . . ? C17 Zr1 C12 113.68(8) . . ? C18 Zr1 C12 145.12(9) . . ? C19 Zr1 C12 152.22(9) . . ? C1 Zr1 C14 70.80(7) . . ? C6 Zr1 C14 113.28(7) . . ? C2 Zr1 C14 87.15(8) . . ? C20 Zr1 C14 107.55(8) . . ? C15 Zr1 C14 31.81(8) . . ? C16 Zr1 C14 119.18(8) . . ? C11 Zr1 C14 53.03(8) . . ? C17 Zr1 C14 150.10(9) . . ? C18 Zr1 C14 156.43(9) . . ? C19 Zr1 C14 124.78(9) . . ? C12 Zr1 C14 52.52(8) . . ? C1 Si1 C22 106.60(11) . . ? C1 Si1 C23 109.84(11) . . ? C22 Si1 C23 111.25(13) . . ? C1 Si1 C21 110.89(12) . . ? C22 Si1 C21 108.93(13) . . ? C23 Si1 C21 109.30(13) . . ? C26 Si2 C6 111.76(12) . . ? C26 Si2 C25 108.20(14) . . ? C6 Si2 C25 114.10(11) . . ? C26 Si2 C24 105.13(13) . . ? C6 Si2 C24 115.26(11) . . ? C25 Si2 C24 101.50(13) . . ? C2 C1 Si1 139.67(18) . . ? C2 C1 Zr1 76.67(13) . . ? Si1 C1 Zr1 143.66(12) . . ? C1 C2 C3 158.7(2) . . ? C1 C2 Zr1 72.65(13) . . ? C3 C2 Zr1 86.40(13) . . ? C2 C3 C7 121.0(2) . . ? C2 C3 C4 122.7(2) . . ? C7 C3 C4 114.31(19) . . ? C2 C3 Zr1 63.51(12) . . ? C7 C3 Zr1 120.79(15) . . ? C4 C3 Zr1 100.48(13) . . ? C3 C4 C5 107.33(17) . . ? C3 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? C3 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C6 C5 C8 128.12(19) . . ? C6 C5 C4 120.41(18) . . ? C8 C5 C4 111.46(18) . . ? C5 C6 Si2 117.76(15) . . ? C5 C6 Zr1 117.03(14) . . ? Si2 C6 Zr1 124.62(10) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 122.2(2) . . ? C10 C8 C5 121.2(2) . . ? C9 C8 C5 116.4(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 120.0 . . ? C8 C10 H10B 120.0 . . ? H10A C10 H10B 120.0 . . ? C12 C11 C15 107.4(2) . . ? C12 C11 Zr1 75.27(13) . . ? C15 C11 Zr1 72.92(12) . . ? C12 C11 H11 126.3 . . ? C15 C11 H11 126.3 . . ? Zr1 C11 H11 117.6 . . ? C11 C12 C13 108.4(2) . . ? C11 C12 Zr1 73.11(12) . . ? C13 C12 Zr1 74.29(12) . . ? C11 C12 H12 125.8 . . ? C13 C12 H12 125.8 . . ? Zr1 C12 H12 118.7 . . ? C14 C13 C12 107.9(2) . . ? C14 C13 Zr1 74.18(12) . . ? C12 C13 Zr1 73.84(12) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Zr1 C13 H13 117.9 . . ? C15 C14 C13 108.1(2) . . ? C15 C14 Zr1 72.04(12) . . ? C13 C14 Zr1 74.21(12) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Zr1 C14 H14 119.6 . . ? C14 C15 C11 108.1(2) . . ? C14 C15 Zr1 76.15(13) . . ? C11 C15 Zr1 74.43(13) . . ? C14 C15 H15 125.9 . . ? C11 C15 H15 125.9 . . ? Zr1 C15 H15 115.6 . . ? C17 C16 C20 108.0(2) . . ? C17 C16 Zr1 74.75(13) . . ? C20 C16 Zr1 73.55(14) . . ? C17 C16 H16 126.0 . . ? C20 C16 H16 126.0 . . ? Zr1 C16 H16 117.7 . . ? C16 C17 C18 107.8(2) . . ? C16 C17 Zr1 73.41(13) . . ? C18 C17 Zr1 74.28(13) . . ? C16 C17 H17 126.1 . . ? C18 C17 H17 126.1 . . ? Zr1 C17 H17 118.2 . . ? C19 C18 C17 107.9(2) . . ? C19 C18 Zr1 74.25(13) . . ? C17 C18 Zr1 73.72(13) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? Zr1 C18 H18 118.0 . . ? C18 C19 C20 108.0(2) . . ? C18 C19 Zr1 74.10(13) . . ? C20 C19 Zr1 72.63(13) . . ? C18 C19 H19 126.0 . . ? C20 C19 H19 126.0 . . ? Zr1 C19 H19 119.1 . . ? C19 C20 C16 108.2(2) . . ? C19 C20 Zr1 75.49(14) . . ? C16 C20 Zr1 74.34(13) . . ? C19 C20 H20 125.9 . . ? C16 C20 H20 125.9 . . ? Zr1 C20 H20 116.4 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Si1 C1 C2 60.8(3) . . . . ? C23 Si1 C1 C2 -59.8(3) . . . . ? C21 Si1 C1 C2 179.3(3) . . . . ? C22 Si1 C1 Zr1 -117.3(2) . . . . ? C23 Si1 C1 Zr1 122.11(19) . . . . ? C21 Si1 C1 Zr1 1.2(2) . . . . ? C6 Zr1 C1 C2 13.52(17) . . . . ? C20 Zr1 C1 C2 -132.63(15) . . . . ? C15 Zr1 C1 C2 145.66(14) . . . . ? C16 Zr1 C1 C2 -128.08(14) . . . . ? C11 Zr1 C1 C2 137.78(14) . . . . ? C17 Zr1 C1 C2 -89.71(16) . . . . ? C18 Zr1 C1 C2 -79.95(15) . . . . ? C19 Zr1 C1 C2 -104.72(15) . . . . ? C12 Zr1 C1 C2 100.91(15) . . . . ? C14 Zr1 C1 C2 118.92(15) . . . . ? C6 Zr1 C1 Si1 -167.76(16) . . . . ? C2 Zr1 C1 Si1 178.7(3) . . . . ? C20 Zr1 C1 Si1 46.09(19) . . . . ? C15 Zr1 C1 Si1 -35.62(19) . . . . ? C16 Zr1 C1 Si1 50.6(2) . . . . ? C11 Zr1 C1 Si1 -43.5(2) . . . . ? C17 Zr1 C1 Si1 89.0(2) . . . . ? C18 Zr1 C1 Si1 98.77(19) . . . . ? C19 Zr1 C1 Si1 74.00(19) . . . . ? C12 Zr1 C1 Si1 -80.4(2) . . . . ? C14 Zr1 C1 Si1 -62.36(18) . . . . ? Si1 C1 C2 C3 -167.7(5) . . . . ? Zr1 C1 C2 C3 11.1(6) . . . . ? Si1 C1 C2 Zr1 -178.8(3) . . . . ? C6 Zr1 C2 C1 -168.98(14) . . . . ? C20 Zr1 C2 C1 51.83(16) . . . . ? C15 Zr1 C2 C1 -38.06(16) . . . . ? C16 Zr1 C2 C1 75.21(18) . . . . ? C11 Zr1 C2 C1 -63.52(18) . . . . ? C17 Zr1 C2 C1 110.00(15) . . . . ? C18 Zr1 C2 C1 100.93(15) . . . . ? C19 Zr1 C2 C1 69.57(15) . . . . ? C12 Zr1 C2 C1 -97.90(15) . . . . ? C14 Zr1 C2 C1 -55.85(14) . . . . ? C1 Zr1 C2 C3 -176.0(2) . . . . ? C6 Zr1 C2 C3 15.05(14) . . . . ? C20 Zr1 C2 C3 -124.14(14) . . . . ? C15 Zr1 C2 C3 145.97(13) . . . . ? C16 Zr1 C2 C3 -100.76(16) . . . . ? C11 Zr1 C2 C3 120.51(15) . . . . ? C17 Zr1 C2 C3 -65.97(16) . . . . ? C18 Zr1 C2 C3 -75.04(15) . . . . ? C19 Zr1 C2 C3 -106.40(15) . . . . ? C12 Zr1 C2 C3 86.13(15) . . . . ? C14 Zr1 C2 C3 128.18(14) . . . . ? C1 C2 C3 C7 101.0(6) . . . . ? Zr1 C2 C3 C7 111.6(2) . . . . ? C1 C2 C3 C4 -96.1(6) . . . . ? Zr1 C2 C3 C4 -85.5(2) . . . . ? C1 C2 C3 Zr1 -10.6(6) . . . . ? C1 Zr1 C3 C2 2.36(13) . . . . ? C6 Zr1 C3 C2 -163.63(15) . . . . ? C20 Zr1 C3 C2 70.29(16) . . . . ? C15 Zr1 C3 C2 -48.48(18) . . . . ? C16 Zr1 C3 C2 110.49(16) . . . . ? C11 Zr1 C3 C2 -100.09(17) . . . . ? C17 Zr1 C3 C2 124.89(14) . . . . ? C18 Zr1 C3 C2 102.41(15) . . . . ? C19 Zr1 C3 C2 72.78(15) . . . . ? C12 Zr1 C3 C2 -109.96(14) . . . . ? C14 Zr1 C3 C2 -54.55(15) . . . . ? C1 Zr1 C3 C7 -109.52(18) . . . . ? C6 Zr1 C3 C7 84.50(17) . . . . ? C2 Zr1 C3 C7 -111.9(2) . . . . ? C20 Zr1 C3 C7 -41.6(2) . . . . ? C15 Zr1 C3 C7 -160.36(16) . . . . ? C16 Zr1 C3 C7 -1.4(2) . . . . ? C11 Zr1 C3 C7 148.03(17) . . . . ? C17 Zr1 C3 C7 13.01(18) . . . . ? C18 Zr1 C3 C7 -9.47(18) . . . . ? C19 Zr1 C3 C7 -39.10(18) . . . . ? C12 Zr1 C3 C7 138.16(17) . . . . ? C14 Zr1 C3 C7 -166.42(17) . . . . ? C1 Zr1 C3 C4 123.79(15) . . . . ? C6 Zr1 C3 C4 -42.20(13) . . . . ? C2 Zr1 C3 C4 121.4(2) . . . . ? C20 Zr1 C3 C4 -168.28(13) . . . . ? C15 Zr1 C3 C4 72.95(17) . . . . ? C16 Zr1 C3 C4 -128.07(15) . . . . ? C11 Zr1 C3 C4 21.3(2) . . . . ? C17 Zr1 C3 C4 -113.68(14) . . . . ? C18 Zr1 C3 C4 -136.16(15) . . . . ? C19 Zr1 C3 C4 -165.79(14) . . . . ? C12 Zr1 C3 C4 11.47(16) . . . . ? C14 Zr1 C3 C4 66.88(14) . . . . ? C2 C3 C4 C5 117.9(2) . . . . ? C7 C3 C4 C5 -78.2(2) . . . . ? Zr1 C3 C4 C5 52.75(17) . . . . ? C3 C4 C5 C6 -37.2(3) . . . . ? C3 C4 C5 C8 141.67(19) . . . . ? C8 C5 C6 Si2 3.4(3) . . . . ? C4 C5 C6 Si2 -177.97(15) . . . . ? C8 C5 C6 Zr1 174.96(18) . . . . ? C4 C5 C6 Zr1 -6.4(3) . . . . ? C26 Si2 C6 C5 -80.1(2) . . . . ? C25 Si2 C6 C5 43.1(2) . . . . ? C24 Si2 C6 C5 159.96(17) . . . . ? C26 Si2 C6 Zr1 108.99(14) . . . . ? C25 Si2 C6 Zr1 -127.85(13) . . . . ? C24 Si2 C6 Zr1 -10.95(17) . . . . ? C1 Zr1 C6 C5 11.9(2) . . . . ? C2 Zr1 C6 C5 18.78(17) . . . . ? C20 Zr1 C6 C5 143.20(16) . . . . ? C15 Zr1 C6 C5 -104.85(17) . . . . ? C16 Zr1 C6 C5 159.26(16) . . . . ? C11 Zr1 C6 C5 -122.49(16) . . . . ? C17 Zr1 C6 C5 137.88(17) . . . . ? C18 Zr1 C6 C5 107.56(17) . . . . ? C19 Zr1 C6 C5 105.08(17) . . . . ? C12 Zr1 C6 C5 -102.38(17) . . . . ? C14 Zr1 C6 C5 -70.48(17) . . . . ? C1 Zr1 C6 Si2 -177.14(9) . . . . ? C2 Zr1 C6 Si2 -170.25(12) . . . . ? C20 Zr1 C6 Si2 -45.83(17) . . . . ? C15 Zr1 C6 Si2 66.12(14) . . . . ? C16 Zr1 C6 Si2 -29.77(13) . . . . ? C11 Zr1 C6 Si2 48.47(12) . . . . ? C17 Zr1 C6 Si2 -51.16(12) . . . . ? C18 Zr1 C6 Si2 -81.47(12) . . . . ? C19 Zr1 C6 Si2 -83.95(14) . . . . ? C12 Zr1 C6 Si2 68.58(12) . . . . ? C14 Zr1 C6 Si2 100.49(12) . . . . ? C6 C5 C8 C10 77.1(3) . . . . ? C4 C5 C8 C10 -101.6(3) . . . . ? C6 C5 C8 C9 -109.4(3) . . . . ? C4 C5 C8 C9 71.9(3) . . . . ? C1 Zr1 C11 C12 -99.17(15) . . . . ? C6 Zr1 C11 C12 38.32(15) . . . . ? C2 Zr1 C11 C12 -67.10(19) . . . . ? C20 Zr1 C11 C12 170.64(16) . . . . ? C15 Zr1 C11 C12 -113.9(2) . . . . ? C16 Zr1 C11 C12 140.62(16) . . . . ? C17 Zr1 C11 C12 118.62(15) . . . . ? C18 Zr1 C11 C12 133.28(15) . . . . ? C19 Zr1 C11 C12 171.07(14) . . . . ? C14 Zr1 C11 C12 -76.70(16) . . . . ? C1 Zr1 C11 C15 14.72(17) . . . . ? C6 Zr1 C11 C15 152.20(14) . . . . ? C2 Zr1 C11 C15 46.78(19) . . . . ? C20 Zr1 C11 C15 -75.47(15) . . . . ? C16 Zr1 C11 C15 -105.49(15) . . . . ? C17 Zr1 C11 C15 -127.49(14) . . . . ? C18 Zr1 C11 C15 -112.83(16) . . . . ? C19 Zr1 C11 C15 -75.04(16) . . . . ? C12 Zr1 C11 C15 113.9(2) . . . . ? C14 Zr1 C11 C15 37.18(14) . . . . ? C15 C11 C12 C13 0.1(2) . . . . ? Zr1 C11 C12 C13 66.45(15) . . . . ? C15 C11 C12 Zr1 -66.37(15) . . . . ? C1 Zr1 C12 C11 100.04(16) . . . . ? C6 Zr1 C12 C11 -139.26(16) . . . . ? C2 Zr1 C12 C11 135.91(15) . . . . ? C20 Zr1 C12 C11 -10.89(18) . . . . ? C15 Zr1 C12 C11 38.18(14) . . . . ? C16 Zr1 C12 C11 -39.26(16) . . . . ? C17 Zr1 C12 C11 -70.48(16) . . . . ? C18 Zr1 C12 C11 -78.4(2) . . . . ? C19 Zr1 C12 C11 -16.5(3) . . . . ? C14 Zr1 C12 C11 78.46(16) . . . . ? C1 Zr1 C12 C13 -15.34(17) . . . . ? C6 Zr1 C12 C13 105.35(15) . . . . ? C2 Zr1 C12 C13 20.52(16) . . . . ? C20 Zr1 C12 C13 -126.27(15) . . . . ? C15 Zr1 C12 C13 -77.21(15) . . . . ? C16 Zr1 C12 C13 -154.64(14) . . . . ? C11 Zr1 C12 C13 -115.4(2) . . . . ? C17 Zr1 C12 C13 174.13(14) . . . . ? C18 Zr1 C12 C13 166.17(15) . . . . ? C19 Zr1 C12 C13 -131.92(19) . . . . ? C14 Zr1 C12 C13 -36.93(13) . . . . ? C11 C12 C13 C14 1.2(2) . . . . ? Zr1 C12 C13 C14 66.92(15) . . . . ? C11 C12 C13 Zr1 -65.68(15) . . . . ? C1 Zr1 C13 C14 52.29(15) . . . . ? C6 Zr1 C13 C14 178.37(15) . . . . ? C2 Zr1 C13 C14 82.94(15) . . . . ? C20 Zr1 C13 C14 -37.8(2) . . . . ? C15 Zr1 C13 C14 -36.70(14) . . . . ? C16 Zr1 C13 C14 -81.33(17) . . . . ? C11 Zr1 C13 C14 -78.03(15) . . . . ? C17 Zr1 C13 C14 -123.98(17) . . . . ? C18 Zr1 C13 C14 171.1(5) . . . . ? C19 Zr1 C13 C14 5.8(3) . . . . ? C12 Zr1 C13 C14 -114.5(2) . . . . ? C1 Zr1 C13 C12 166.80(14) . . . . ? C6 Zr1 C13 C12 -67.12(14) . . . . ? C2 Zr1 C13 C12 -162.55(14) . . . . ? C20 Zr1 C13 C12 76.70(18) . . . . ? C15 Zr1 C13 C12 77.81(15) . . . . ? C16 Zr1 C13 C12 33.18(18) . . . . ? C11 Zr1 C13 C12 36.48(14) . . . . ? C17 Zr1 C13 C12 -9.5(2) . . . . ? C18 Zr1 C13 C12 -74.4(6) . . . . ? C19 Zr1 C13 C12 120.3(2) . . . . ? C14 Zr1 C13 C12 114.5(2) . . . . ? C12 C13 C14 C15 -2.1(2) . . . . ? Zr1 C13 C14 C15 64.58(15) . . . . ? C12 C13 C14 Zr1 -66.69(15) . . . . ? C1 Zr1 C14 C15 121.42(16) . . . . ? C6 Zr1 C14 C15 -117.24(14) . . . . ? C2 Zr1 C14 C15 147.98(15) . . . . ? C20 Zr1 C14 C15 37.21(16) . . . . ? C16 Zr1 C14 C15 4.44(17) . . . . ? C11 Zr1 C14 C15 -38.21(14) . . . . ? C17 Zr1 C14 C15 -6.8(2) . . . . ? C18 Zr1 C14 C15 67.7(3) . . . . ? C19 Zr1 C14 C15 67.35(17) . . . . ? C12 Zr1 C14 C15 -78.22(15) . . . . ? C1 Zr1 C14 C13 -123.10(16) . . . . ? C6 Zr1 C14 C13 -1.76(16) . . . . ? C2 Zr1 C14 C13 -96.54(15) . . . . ? C20 Zr1 C14 C13 152.69(15) . . . . ? C15 Zr1 C14 C13 115.5(2) . . . . ? C16 Zr1 C14 C13 119.92(15) . . . . ? C11 Zr1 C14 C13 77.27(15) . . . . ? C17 Zr1 C14 C13 108.70(19) . . . . ? C18 Zr1 C14 C13 -176.86(18) . . . . ? C19 Zr1 C14 C13 -177.16(14) . . . . ? C12 Zr1 C14 C13 37.26(14) . . . . ? C13 C14 C15 C11 2.2(2) . . . . ? Zr1 C14 C15 C11 68.18(15) . . . . ? C13 C14 C15 Zr1 -66.02(15) . . . . ? C12 C11 C15 C14 -1.4(2) . . . . ? Zr1 C11 C15 C14 -69.35(15) . . . . ? C12 C11 C15 Zr1 67.95(15) . . . . ? C1 Zr1 C15 C14 -53.72(15) . . . . ? C6 Zr1 C15 C14 79.66(16) . . . . ? C2 Zr1 C15 C14 -35.38(16) . . . . ? C20 Zr1 C15 C14 -144.36(16) . . . . ? C16 Zr1 C15 C14 -176.12(15) . . . . ? C11 Zr1 C15 C14 113.7(2) . . . . ? C17 Zr1 C15 C14 176.16(14) . . . . ? C18 Zr1 C15 C14 -148.87(15) . . . . ? C19 Zr1 C15 C14 -126.92(14) . . . . ? C12 Zr1 C15 C14 76.74(15) . . . . ? C1 Zr1 C15 C11 -167.37(15) . . . . ? C6 Zr1 C15 C11 -33.99(17) . . . . ? C2 Zr1 C15 C11 -149.03(14) . . . . ? C20 Zr1 C15 C11 101.99(15) . . . . ? C16 Zr1 C15 C11 70.23(15) . . . . ? C17 Zr1 C15 C11 62.51(16) . . . . ? C18 Zr1 C15 C11 97.48(17) . . . . ? C19 Zr1 C15 C11 119.43(14) . . . . ? C12 Zr1 C15 C11 -36.91(14) . . . . ? C14 Zr1 C15 C11 -113.7(2) . . . . ? C1 Zr1 C16 C17 105.91(16) . . . . ? C6 Zr1 C16 C17 -42.81(16) . . . . ? C2 Zr1 C16 C17 70.2(2) . . . . ? C20 Zr1 C16 C17 114.5(2) . . . . ? C15 Zr1 C16 C17 -167.06(16) . . . . ? C11 Zr1 C16 C17 -135.70(17) . . . . ? C18 Zr1 C16 C17 37.21(15) . . . . ? C19 Zr1 C16 C17 77.25(17) . . . . ? C12 Zr1 C16 C17 -115.82(16) . . . . ? C14 Zr1 C16 C17 -169.40(14) . . . . ? C1 Zr1 C16 C20 -8.59(19) . . . . ? C6 Zr1 C16 C20 -157.31(16) . . . . ? C2 Zr1 C16 C20 -44.3(2) . . . . ? C15 Zr1 C16 C20 78.44(16) . . . . ? C11 Zr1 C16 C20 109.81(17) . . . . ? C17 Zr1 C16 C20 -114.5(2) . . . . ? C18 Zr1 C16 C20 -77.28(17) . . . . ? C19 Zr1 C16 C20 -37.25(16) . . . . ? C12 Zr1 C16 C20 129.69(16) . . . . ? C14 Zr1 C16 C20 76.10(17) . . . . ? C20 C16 C17 C18 -0.3(3) . . . . ? Zr1 C16 C17 C18 -66.87(16) . . . . ? C20 C16 C17 Zr1 66.59(16) . . . . ? C1 Zr1 C17 C16 -95.97(17) . . . . ? C6 Zr1 C17 C16 137.71(17) . . . . ? C2 Zr1 C17 C16 -131.89(16) . . . . ? C20 Zr1 C17 C16 -37.35(16) . . . . ? C15 Zr1 C17 C16 14.73(18) . . . . ? C11 Zr1 C17 C16 43.86(17) . . . . ? C18 Zr1 C17 C16 -114.6(2) . . . . ? C19 Zr1 C17 C16 -77.68(17) . . . . ? C12 Zr1 C17 C16 74.02(17) . . . . ? C14 Zr1 C17 C16 18.8(2) . . . . ? C1 Zr1 C17 C18 18.6(2) . . . . ? C6 Zr1 C17 C18 -107.72(16) . . . . ? C2 Zr1 C17 C18 -17.32(19) . . . . ? C20 Zr1 C17 C18 77.23(17) . . . . ? C15 Zr1 C17 C18 129.31(16) . . . . ? C16 Zr1 C17 C18 114.6(2) . . . . ? C11 Zr1 C17 C18 158.43(16) . . . . ? C19 Zr1 C17 C18 36.89(16) . . . . ? C12 Zr1 C17 C18 -171.40(15) . . . . ? C14 Zr1 C17 C18 133.37(19) . . . . ? C16 C17 C18 C19 -0.7(3) . . . . ? Zr1 C17 C18 C19 -66.95(16) . . . . ? C16 C17 C18 Zr1 66.29(16) . . . . ? C1 Zr1 C18 C19 -50.29(16) . . . . ? C6 Zr1 C18 C19 -175.97(16) . . . . ? C2 Zr1 C18 C19 -80.46(16) . . . . ? C20 Zr1 C18 C19 36.88(16) . . . . ? C15 Zr1 C18 C19 42.5(2) . . . . ? C16 Zr1 C18 C19 77.53(17) . . . . ? C11 Zr1 C18 C19 86.53(18) . . . . ? C17 Zr1 C18 C19 114.5(2) . . . . ? C12 Zr1 C18 C19 128.40(18) . . . . ? C14 Zr1 C18 C19 -0.5(3) . . . . ? C1 Zr1 C18 C17 -164.84(16) . . . . ? C6 Zr1 C18 C17 69.48(16) . . . . ? C2 Zr1 C18 C17 164.99(16) . . . . ? C20 Zr1 C18 C17 -77.66(17) . . . . ? C15 Zr1 C18 C17 -72.1(2) . . . . ? C16 Zr1 C18 C17 -37.02(15) . . . . ? C11 Zr1 C18 C17 -28.0(2) . . . . ? C19 Zr1 C18 C17 -114.5(2) . . . . ? C12 Zr1 C18 C17 13.9(2) . . . . ? C14 Zr1 C18 C17 -115.0(2) . . . . ? C17 C18 C19 C20 1.3(3) . . . . ? Zr1 C18 C19 C20 -65.24(17) . . . . ? C17 C18 C19 Zr1 66.59(16) . . . . ? C1 Zr1 C19 C18 127.25(17) . . . . ? C6 Zr1 C19 C18 4.74(19) . . . . ? C2 Zr1 C19 C18 97.50(16) . . . . ? C20 Zr1 C19 C18 -115.2(2) . . . . ? C15 Zr1 C19 C18 -149.36(16) . . . . ? C16 Zr1 C19 C18 -77.63(17) . . . . ? C11 Zr1 C19 C18 -116.00(16) . . . . ? C17 Zr1 C19 C18 -37.31(15) . . . . ? C12 Zr1 C19 C18 -106.0(2) . . . . ? C14 Zr1 C19 C18 179.77(14) . . . . ? C1 Zr1 C19 C20 -117.57(18) . . . . ? C6 Zr1 C19 C20 119.92(17) . . . . ? C2 Zr1 C19 C20 -147.32(17) . . . . ? C15 Zr1 C19 C20 -34.18(18) . . . . ? C16 Zr1 C19 C20 37.55(16) . . . . ? C11 Zr1 C19 C20 -0.8(2) . . . . ? C17 Zr1 C19 C20 77.87(18) . . . . ? C18 Zr1 C19 C20 115.2(2) . . . . ? C12 Zr1 C19 C20 9.2(3) . . . . ? C14 Zr1 C19 C20 -65.05(19) . . . . ? C18 C19 C20 C16 -1.5(3) . . . . ? Zr1 C19 C20 C16 -67.74(16) . . . . ? C18 C19 C20 Zr1 66.21(17) . . . . ? C17 C16 C20 C19 1.1(3) . . . . ? Zr1 C16 C20 C19 68.52(17) . . . . ? C17 C16 C20 Zr1 -67.40(16) . . . . ? C1 Zr1 C20 C19 58.67(17) . . . . ? C6 Zr1 C20 C19 -83.65(19) . . . . ? C2 Zr1 C20 C19 35.01(18) . . . . ? C15 Zr1 C20 C19 147.44(17) . . . . ? C16 Zr1 C20 C19 -114.1(2) . . . . ? C11 Zr1 C20 C19 179.30(17) . . . . ? C17 Zr1 C20 C19 -77.08(18) . . . . ? C18 Zr1 C20 C19 -36.61(16) . . . . ? C12 Zr1 C20 C19 -175.02(15) . . . . ? C14 Zr1 C20 C19 128.65(16) . . . . ? C1 Zr1 C20 C16 172.75(16) . . . . ? C6 Zr1 C20 C16 30.4(2) . . . . ? C2 Zr1 C20 C16 149.10(15) . . . . ? C15 Zr1 C20 C16 -98.48(17) . . . . ? C11 Zr1 C20 C16 -66.62(16) . . . . ? C17 Zr1 C20 C16 37.00(15) . . . . ? C18 Zr1 C20 C16 77.47(17) . . . . ? C19 Zr1 C20 C16 114.1(2) . . . . ? C12 Zr1 C20 C16 -60.94(18) . . . . ? C14 Zr1 C20 C16 -117.27(16) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.514 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.054 # Attachment '- erk6177.cif' data_erk6177 _database_code_depnum_ccdc_archive 'CCDC 886396' #TrackingRef '- erk6177.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.50 H39 N Zr' _chemical_formula_weight 462.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.6943(5) _cell_length_b 8.57940(10) _cell_length_c 17.9781(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.7840(10) _cell_angle_gamma 90.00 _cell_volume 5174.14(13) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4525 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8804 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD ApexII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14052 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4477 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C15 atom displayed irregular displacement ellipsoids, which were therefore constrained to be more regular using the program command ISOR. ; _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^)+(0.0413P)^2^+18.2447P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4477 _refine_ls_number_parameters 253 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.162629(9) 0.41013(4) 0.200123(17) 0.03631(13) Uani 1 1 d . . . N1 N 0.17387(10) 0.1554(4) 0.05938(18) 0.0525(8) Uani 1 1 d . . . C1 C 0.23385(14) 0.5129(7) 0.2446(3) 0.0763(14) Uani 1 1 d . . . H1 H 0.2519 0.4602 0.2846 0.092 Uiso 1 1 calc R . . C2 C 0.22779(13) 0.4833(5) 0.1687(3) 0.0663(12) Uani 1 1 d . . . H2 H 0.2408 0.4056 0.1473 0.080 Uiso 1 1 calc R . . C3 C 0.19934(14) 0.5859(5) 0.1272(3) 0.0634(11) Uani 1 1 d . . . H3 H 0.1898 0.5900 0.0734 0.076 Uiso 1 1 calc R . . C4 C 0.18772(14) 0.6809(5) 0.1796(4) 0.0767(15) Uani 1 1 d . . . H4 H 0.1690 0.7623 0.1683 0.092 Uiso 1 1 calc R . . C5 C 0.20934(19) 0.6321(7) 0.2536(3) 0.0888(19) Uani 1 1 d . . . H5 H 0.2072 0.6742 0.3007 0.107 Uiso 1 1 calc R . . C6 C 0.19055(13) 0.2453(5) 0.3193(2) 0.0582(10) Uani 1 1 d . . . H6 H 0.2184 0.2393 0.3385 0.070 Uiso 1 1 calc R . . C7 C 0.16731(13) 0.1458(5) 0.2667(2) 0.0549(10) Uani 1 1 d . . . H7 H 0.1766 0.0603 0.2435 0.066 Uiso 1 1 calc R . . C8 C 0.12749(12) 0.1932(5) 0.2533(2) 0.0577(10) Uani 1 1 d . . . H8 H 0.1053 0.1458 0.2197 0.069 Uiso 1 1 calc R . . C9 C 0.12694(14) 0.3245(5) 0.2993(2) 0.0633(12) Uani 1 1 d . . . H9 H 0.1042 0.3811 0.3025 0.076 Uiso 1 1 calc R . . C10 C 0.16596(15) 0.3560(5) 0.3395(2) 0.0630(11) Uani 1 1 d . . . H10 H 0.1743 0.4384 0.3744 0.076 Uiso 1 1 calc R . . C11 C 0.10585(11) 0.5381(4) 0.1587(2) 0.0465(8) Uani 1 1 d . . . C12 C 0.10735(11) 0.4431(4) 0.1038(2) 0.0478(8) Uani 1 1 d . . . C13 C 0.07671(13) 0.6609(5) 0.1712(3) 0.0621(11) Uani 1 1 d . . . C14 C 0.09143(19) 0.7409(7) 0.2475(3) 0.0978(18) Uani 1 1 d . . . H14A H 0.0941 0.6651 0.2885 0.147 Uiso 1 1 calc R . . H14B H 0.0726 0.8208 0.2528 0.147 Uiso 1 1 calc R . . H14C H 0.1171 0.7883 0.2503 0.147 Uiso 1 1 calc R . . C15 C 0.0715(2) 0.7833(8) 0.1086(4) 0.117(2) Uani 1 1 d U . . H15A H 0.0968 0.8343 0.1119 0.176 Uiso 1 1 calc R . . H15B H 0.0521 0.8599 0.1153 0.176 Uiso 1 1 calc R . . H15C H 0.0622 0.7340 0.0587 0.176 Uiso 1 1 calc R . . C16 C 0.03726(18) 0.5844(8) 0.1693(6) 0.133(3) Uani 1 1 d . . . H16A H 0.0273 0.5322 0.1203 0.199 Uiso 1 1 calc R . . H16B H 0.0183 0.6631 0.1758 0.199 Uiso 1 1 calc R . . H16C H 0.0409 0.5088 0.2106 0.199 Uiso 1 1 calc R . . C17 C 0.08533(14) 0.3936(6) 0.0273(3) 0.0685(12) Uani 1 1 d . . . C18 C 0.09108(19) 0.4630(9) -0.0364(3) 0.102(2) Uani 1 1 d . . . H18A H 0.1096 0.5448 -0.0318 0.123 Uiso 1 1 calc R . . H18B H 0.0766 0.4296 -0.0853 0.123 Uiso 1 1 calc R . . C19 C 0.06039(19) 0.2532(8) 0.0236(4) 0.110(2) Uani 1 1 d . . . H19A H 0.0482 0.2275 -0.0298 0.164 Uiso 1 1 calc R . . H19B H 0.0397 0.2729 0.0500 0.164 Uiso 1 1 calc R . . H19C H 0.0768 0.1668 0.0481 0.164 Uiso 1 1 calc R . . C20 C 0.17011(10) 0.2356(4) 0.1086(2) 0.0458(8) Uani 1 1 d . . . C21 C 0.17776(12) 0.0630(4) -0.0065(2) 0.0508(9) Uani 1 1 d . . . C22 C 0.21614(15) -0.0324(6) 0.0187(3) 0.0757(13) Uani 1 1 d . . . H22A H 0.2387 0.0374 0.0343 0.114 Uiso 1 1 calc R . . H22B H 0.2193 -0.0964 -0.0239 0.114 Uiso 1 1 calc R . . H22C H 0.2147 -0.0988 0.0616 0.114 Uiso 1 1 calc R . . C23 C 0.18120(19) 0.1766(6) -0.0683(3) 0.0869(16) Uani 1 1 d . . . H23A H 0.1568 0.2369 -0.0840 0.130 Uiso 1 1 calc R . . H23B H 0.1855 0.1199 -0.1122 0.130 Uiso 1 1 calc R . . H23C H 0.2035 0.2461 -0.0485 0.130 Uiso 1 1 calc R . . C24 C 0.14207(17) -0.0400(7) -0.0299(3) 0.0945(18) Uani 1 1 d . . . H24A H 0.1407 -0.1073 0.0127 0.142 Uiso 1 1 calc R . . H24B H 0.1441 -0.1033 -0.0735 0.142 Uiso 1 1 calc R . . H24C H 0.1182 0.0235 -0.0442 0.142 Uiso 1 1 calc R . . C25 C 0.0317(4) 0.8553(14) 0.8865(6) 0.207(5) Uiso 1 1 d D . . H25A H 0.0257 0.7452 0.8789 0.310 Uiso 1 1 calc R . . H25B H 0.0207 0.8948 0.9272 0.310 Uiso 1 1 calc R . . H25C H 0.0604 0.8700 0.9006 0.310 Uiso 1 1 calc R . . C26 C 0.0145(5) 0.9387(16) 0.8161(7) 0.281(8) Uiso 1 1 d D . . H26A H 0.0346 1.0093 0.8053 0.338 Uiso 1 1 calc R . . H26B H -0.0077 1.0024 0.8233 0.338 Uiso 1 1 calc R . . C27 C 0.0000 0.837(2) 0.7500 0.225(8) Uiso 1 2 d SD . . H27A H 0.0216 0.7700 0.7422 0.270 Uiso 0.50 1 calc PR . . H27B H -0.0216 0.7700 0.7578 0.270 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0435(2) 0.0356(2) 0.03158(19) -0.00036(13) 0.01270(13) -0.00119(13) N1 0.068(2) 0.0521(18) 0.0420(17) -0.0090(15) 0.0221(15) -0.0053(16) C1 0.059(3) 0.093(4) 0.071(3) 0.013(3) 0.005(2) -0.026(3) C2 0.060(3) 0.061(3) 0.089(3) -0.003(2) 0.039(2) -0.014(2) C3 0.071(3) 0.067(3) 0.053(2) 0.009(2) 0.018(2) -0.025(2) C4 0.068(3) 0.039(2) 0.133(5) 0.000(3) 0.044(3) -0.010(2) C5 0.115(4) 0.097(4) 0.068(3) -0.043(3) 0.048(3) -0.065(4) C6 0.061(2) 0.063(3) 0.050(2) 0.018(2) 0.0121(18) 0.003(2) C7 0.074(3) 0.0414(19) 0.057(2) 0.0093(18) 0.030(2) 0.0040(19) C8 0.062(2) 0.057(2) 0.057(2) 0.013(2) 0.0190(19) -0.014(2) C9 0.073(3) 0.066(3) 0.065(3) 0.030(2) 0.044(2) 0.024(2) C10 0.101(3) 0.055(2) 0.037(2) 0.0040(18) 0.024(2) 0.001(2) C11 0.052(2) 0.048(2) 0.0420(19) 0.0078(16) 0.0153(16) 0.0038(17) C12 0.048(2) 0.053(2) 0.0403(19) 0.0046(17) 0.0070(15) -0.0007(17) C13 0.067(3) 0.057(2) 0.067(3) 0.009(2) 0.025(2) 0.018(2) C14 0.124(5) 0.086(4) 0.087(4) -0.015(3) 0.034(3) 0.037(4) C15 0.154(5) 0.098(4) 0.111(4) 0.041(4) 0.055(4) 0.069(4) C16 0.071(4) 0.113(5) 0.229(9) -0.018(5) 0.065(5) 0.013(4) C17 0.063(3) 0.084(3) 0.049(2) -0.005(2) -0.001(2) 0.005(2) C18 0.120(5) 0.139(5) 0.042(3) -0.004(3) 0.009(3) 0.010(4) C19 0.093(4) 0.123(5) 0.099(4) -0.037(4) -0.003(3) -0.026(4) C20 0.049(2) 0.048(2) 0.0416(19) 0.0020(17) 0.0137(15) -0.0013(16) C21 0.070(2) 0.049(2) 0.0383(19) -0.0091(16) 0.0220(18) -0.0050(18) C22 0.091(3) 0.073(3) 0.066(3) -0.013(2) 0.026(3) 0.011(3) C23 0.138(5) 0.077(3) 0.053(3) 0.007(2) 0.038(3) 0.008(3) C24 0.091(4) 0.110(4) 0.092(4) -0.050(3) 0.040(3) -0.033(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 C11 2.212(4) . ? Zr1 C12 2.250(4) . ? Zr1 C20 2.288(4) . ? Zr1 C10 2.522(4) . ? Zr1 C5 2.526(4) . ? Zr1 C9 2.526(4) . ? Zr1 C4 2.540(4) . ? Zr1 C8 2.541(4) . ? Zr1 C3 2.544(4) . ? Zr1 C6 2.544(4) . ? Zr1 C2 2.545(4) . ? Zr1 C7 2.550(4) . ? N1 C20 1.155(4) . ? N1 C21 1.460(4) . ? C1 C2 1.351(7) . ? C1 C5 1.366(8) . ? C1 H1 0.9400 . ? C2 C3 1.389(6) . ? C2 H2 0.9400 . ? C3 C4 1.382(7) . ? C3 H3 0.9400 . ? C4 C5 1.414(8) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.373(6) . ? C6 C10 1.385(6) . ? C6 H6 0.9400 . ? C7 C8 1.401(6) . ? C7 H7 0.9400 . ? C8 C9 1.402(6) . ? C8 H8 0.9400 . ? C9 C10 1.389(6) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.292(5) . ? C11 C13 1.516(5) . ? C12 C17 1.455(5) . ? C13 C14 1.502(7) . ? C13 C16 1.511(7) . ? C13 C15 1.515(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.349(7) . ? C17 C19 1.475(8) . ? C18 H18A 0.9400 . ? C18 H18B 0.9400 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C21 C24 1.492(6) . ? C21 C23 1.506(6) . ? C21 C22 1.530(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.444(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C27 1.459(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C26 1.459(9) 2_556 ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Zr1 C12 33.65(13) . . ? C11 Zr1 C20 109.73(13) . . ? C12 Zr1 C20 76.08(13) . . ? C11 Zr1 C10 103.72(14) . . ? C12 Zr1 C10 127.02(15) . . ? C20 Zr1 C10 127.52(13) . . ? C11 Zr1 C5 100.6(2) . . ? C12 Zr1 C5 122.4(2) . . ? C20 Zr1 C5 125.99(15) . . ? C10 Zr1 C5 84.16(17) . . ? C11 Zr1 C9 80.06(13) . . ? C12 Zr1 C9 96.03(14) . . ? C20 Zr1 C9 118.91(14) . . ? C10 Zr1 C9 31.93(15) . . ? C5 Zr1 C9 109.44(16) . . ? C11 Zr1 C4 78.80(15) . . ? C12 Zr1 C4 91.70(16) . . ? C20 Zr1 C4 112.84(16) . . ? C10 Zr1 C4 112.47(18) . . ? C5 Zr1 C4 32.40(18) . . ? C9 Zr1 C4 128.04(17) . . ? C11 Zr1 C8 91.08(14) . . ? C12 Zr1 C8 89.14(13) . . ? C20 Zr1 C8 86.80(13) . . ? C10 Zr1 C8 52.87(15) . . ? C5 Zr1 C8 137.03(16) . . ? C9 Zr1 C8 32.11(14) . . ? C4 Zr1 C8 159.95(16) . . ? C11 Zr1 C3 92.98(15) . . ? C12 Zr1 C3 88.23(14) . . ? C20 Zr1 C3 81.59(14) . . ? C10 Zr1 C3 136.01(15) . . ? C5 Zr1 C3 52.58(15) . . ? C9 Zr1 C3 159.50(16) . . ? C4 Zr1 C3 31.54(15) . . ? C8 Zr1 C3 168.39(15) . . ? C11 Zr1 C6 132.42(13) . . ? C12 Zr1 C6 141.71(14) . . ? C20 Zr1 C6 98.82(13) . . ? C10 Zr1 C6 31.73(14) . . ? C5 Zr1 C6 91.66(19) . . ? C9 Zr1 C6 52.65(14) . . ? C4 Zr1 C6 124.04(17) . . ? C8 Zr1 C6 52.57(14) . . ? C3 Zr1 C6 129.12(15) . . ? C11 Zr1 C2 124.61(15) . . ? C12 Zr1 C2 115.40(15) . . ? C20 Zr1 C2 74.42(14) . . ? C10 Zr1 C2 116.62(17) . . ? C5 Zr1 C2 51.59(16) . . ? C9 Zr1 C2 148.41(16) . . ? C4 Zr1 C2 52.09(15) . . ? C8 Zr1 C2 143.39(15) . . ? C3 Zr1 C2 31.69(15) . . ? C6 Zr1 C2 98.95(15) . . ? C11 Zr1 C7 122.97(13) . . ? C12 Zr1 C7 114.37(14) . . ? C20 Zr1 C7 75.52(13) . . ? C10 Zr1 C7 52.31(14) . . ? C5 Zr1 C7 122.28(19) . . ? C9 Zr1 C7 52.70(13) . . ? C4 Zr1 C7 153.93(17) . . ? C8 Zr1 C7 31.93(13) . . ? C3 Zr1 C7 142.09(15) . . ? C6 Zr1 C7 31.28(13) . . ? C2 Zr1 C7 111.71(15) . . ? C20 N1 C21 176.0(4) . . ? C2 C1 C5 108.6(5) . . ? C2 C1 Zr1 74.3(3) . . ? C5 C1 Zr1 73.4(3) . . ? C2 C1 H1 125.7 . . ? C5 C1 H1 125.7 . . ? Zr1 C1 H1 118.5 . . ? C1 C2 C3 109.2(5) . . ? C1 C2 Zr1 74.9(2) . . ? C3 C2 Zr1 74.1(2) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? Zr1 C2 H2 117.5 . . ? C4 C3 C2 107.4(4) . . ? C4 C3 Zr1 74.1(2) . . ? C2 C3 Zr1 74.2(2) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Zr1 C3 H3 117.5 . . ? C3 C4 C5 106.9(4) . . ? C3 C4 Zr1 74.4(2) . . ? C5 C4 Zr1 73.3(3) . . ? C3 C4 H4 126.6 . . ? C5 C4 H4 126.6 . . ? Zr1 C4 H4 117.9 . . ? C1 C5 C4 107.9(4) . . ? C1 C5 Zr1 75.4(3) . . ? C4 C5 Zr1 74.3(3) . . ? C1 C5 H5 126.1 . . ? C4 C5 H5 126.1 . . ? Zr1 C5 H5 116.3 . . ? C7 C6 C10 108.3(4) . . ? C7 C6 Zr1 74.6(2) . . ? C10 C6 Zr1 73.2(2) . . ? C7 C6 H6 125.8 . . ? C10 C6 H6 125.8 . . ? Zr1 C6 H6 118.2 . . ? C6 C7 C8 108.6(4) . . ? C6 C7 Zr1 74.1(2) . . ? C8 C7 Zr1 73.7(2) . . ? C6 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? Zr1 C7 H7 118.3 . . ? C7 C8 C9 107.0(4) . . ? C7 C8 Zr1 74.4(2) . . ? C9 C8 Zr1 73.4(2) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? Zr1 C8 H8 117.9 . . ? C10 C9 C8 107.8(4) . . ? C10 C9 Zr1 73.8(2) . . ? C8 C9 Zr1 74.5(2) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Zr1 C9 H9 117.5 . . ? C6 C10 C9 108.3(4) . . ? C6 C10 Zr1 75.0(2) . . ? C9 C10 Zr1 74.2(2) . . ? C6 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Zr1 C10 H10 116.9 . . ? C12 C11 C13 135.3(4) . . ? C12 C11 Zr1 74.8(2) . . ? C13 C11 Zr1 149.9(3) . . ? C11 C12 C17 142.4(4) . . ? C11 C12 Zr1 71.6(2) . . ? C17 C12 Zr1 146.1(3) . . ? C14 C13 C16 108.3(5) . . ? C14 C13 C15 108.0(5) . . ? C16 C13 C15 110.4(5) . . ? C14 C13 C11 111.6(4) . . ? C16 C13 C11 109.2(4) . . ? C15 C13 C11 109.2(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C12 121.1(5) . . ? C18 C17 C19 122.3(5) . . ? C12 C17 C19 116.2(4) . . ? C17 C18 H18A 120.0 . . ? C17 C18 H18B 120.0 . . ? H18A C18 H18B 120.0 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 Zr1 175.7(3) . . ? N1 C21 C24 108.0(3) . . ? N1 C21 C23 106.8(3) . . ? C24 C21 C23 113.1(4) . . ? N1 C21 C22 107.7(3) . . ? C24 C21 C22 111.3(4) . . ? C23 C21 C22 109.7(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C25 C26 C27 113.3(10) . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C26 C27 C26 106.2(16) 2_556 . ? C26 C27 H27A 110.5 2_556 . ? C26 C27 H27A 110.5 . . ? C26 C27 H27B 110.5 2_556 . ? C26 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? 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 C11 Zr1 C1 C2 -92.4(4) . . . . ? C12 Zr1 C1 C2 -46.1(5) . . . . ? C20 Zr1 C1 C2 34.0(3) . . . . ? C10 Zr1 C1 C2 161.7(3) . . . . ? C5 Zr1 C1 C2 -115.5(5) . . . . ? C9 Zr1 C1 C2 165.4(3) . . . . ? C4 Zr1 C1 C2 -77.2(3) . . . . ? C8 Zr1 C1 C2 128.5(3) . . . . ? C3 Zr1 C1 C2 -37.0(3) . . . . ? C6 Zr1 C1 C2 131.1(3) . . . . ? C7 Zr1 C1 C2 111.3(3) . . . . ? C11 Zr1 C1 C5 23.1(4) . . . . ? C12 Zr1 C1 C5 69.3(4) . . . . ? C20 Zr1 C1 C5 149.5(3) . . . . ? C10 Zr1 C1 C5 -82.8(3) . . . . ? C9 Zr1 C1 C5 -79.1(3) . . . . ? C4 Zr1 C1 C5 38.3(3) . . . . ? C8 Zr1 C1 C5 -116.1(3) . . . . ? C3 Zr1 C1 C5 78.5(3) . . . . ? C6 Zr1 C1 C5 -113.4(3) . . . . ? C2 Zr1 C1 C5 115.5(5) . . . . ? C7 Zr1 C1 C5 -133.2(3) . . . . ? C5 C1 C2 C3 0.9(5) . . . . ? Zr1 C1 C2 C3 66.8(3) . . . . ? C5 C1 C2 Zr1 -65.9(3) . . . . ? C11 Zr1 C2 C1 111.4(3) . . . . ? C12 Zr1 C2 C1 149.0(3) . . . . ? C20 Zr1 C2 C1 -145.1(4) . . . . ? C10 Zr1 C2 C1 -20.5(4) . . . . ? C5 Zr1 C2 C1 36.6(3) . . . . ? C9 Zr1 C2 C1 -24.8(5) . . . . ? C4 Zr1 C2 C1 78.2(4) . . . . ? C8 Zr1 C2 C1 -83.3(4) . . . . ? C3 Zr1 C2 C1 115.6(4) . . . . ? C6 Zr1 C2 C1 -48.4(3) . . . . ? C7 Zr1 C2 C1 -78.1(3) . . . . ? C11 Zr1 C2 C3 -4.1(3) . . . . ? C12 Zr1 C2 C3 33.5(3) . . . . ? C20 Zr1 C2 C3 99.3(3) . . . . ? C10 Zr1 C2 C3 -136.1(3) . . . . ? C5 Zr1 C2 C3 -78.9(3) . . . . ? C9 Zr1 C2 C3 -140.3(3) . . . . ? C4 Zr1 C2 C3 -37.4(3) . . . . ? C8 Zr1 C2 C3 161.2(3) . . . . ? C6 Zr1 C2 C3 -163.9(3) . . . . ? C7 Zr1 C2 C3 166.4(3) . . . . ? C1 C2 C3 C4 0.0(5) . . . . ? Zr1 C2 C3 C4 67.2(3) . . . . ? C1 C2 C3 Zr1 -67.3(3) . . . . ? C11 Zr1 C3 C4 62.8(3) . . . . ? C12 Zr1 C3 C4 96.1(3) . . . . ? C20 Zr1 C3 C4 172.3(3) . . . . ? C10 Zr1 C3 C4 -50.5(4) . . . . ? C5 Zr1 C3 C4 -38.2(3) . . . . ? C9 Zr1 C3 C4 -6.4(6) . . . . ? C8 Zr1 C3 C4 173.2(6) . . . . ? C6 Zr1 C3 C4 -93.1(4) . . . . ? C2 Zr1 C3 C4 -113.8(4) . . . . ? C7 Zr1 C3 C4 -134.6(3) . . . . ? C11 Zr1 C3 C2 176.6(3) . . . . ? C12 Zr1 C3 C2 -150.1(3) . . . . ? C20 Zr1 C3 C2 -73.9(3) . . . . ? C10 Zr1 C3 C2 63.3(4) . . . . ? C5 Zr1 C3 C2 75.5(3) . . . . ? C9 Zr1 C3 C2 107.3(5) . . . . ? C4 Zr1 C3 C2 113.8(4) . . . . ? C8 Zr1 C3 C2 -73.1(8) . . . . ? C6 Zr1 C3 C2 20.7(4) . . . . ? C7 Zr1 C3 C2 -20.9(4) . . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? Zr1 C3 C4 C5 66.6(3) . . . . ? C2 C3 C4 Zr1 -67.3(3) . . . . ? C11 Zr1 C4 C3 -115.1(3) . . . . ? C12 Zr1 C4 C3 -83.8(3) . . . . ? C20 Zr1 C4 C3 -8.2(4) . . . . ? C10 Zr1 C4 C3 144.6(3) . . . . ? C5 Zr1 C4 C3 113.5(4) . . . . ? C9 Zr1 C4 C3 177.1(3) . . . . ? C8 Zr1 C4 C3 -176.0(4) . . . . ? C6 Zr1 C4 C3 110.8(3) . . . . ? C2 Zr1 C4 C3 37.5(3) . . . . ? C7 Zr1 C4 C3 95.9(5) . . . . ? C11 Zr1 C4 C5 131.4(3) . . . . ? C12 Zr1 C4 C5 162.6(3) . . . . ? C20 Zr1 C4 C5 -121.8(3) . . . . ? C10 Zr1 C4 C5 31.0(4) . . . . ? C9 Zr1 C4 C5 63.6(4) . . . . ? C8 Zr1 C4 C5 70.5(6) . . . . ? C3 Zr1 C4 C5 -113.5(4) . . . . ? C6 Zr1 C4 C5 -2.7(4) . . . . ? C2 Zr1 C4 C5 -76.0(3) . . . . ? C7 Zr1 C4 C5 -17.7(5) . . . . ? C2 C1 C5 C4 -1.3(5) . . . . ? Zr1 C1 C5 C4 -67.9(3) . . . . ? C2 C1 C5 Zr1 66.5(3) . . . . ? C3 C4 C5 C1 1.3(5) . . . . ? Zr1 C4 C5 C1 68.6(3) . . . . ? C3 C4 C5 Zr1 -67.3(3) . . . . ? C11 Zr1 C5 C1 -162.2(3) . . . . ? C12 Zr1 C5 C1 -134.4(3) . . . . ? C20 Zr1 C5 C1 -38.1(4) . . . . ? C10 Zr1 C5 C1 94.9(3) . . . . ? C9 Zr1 C5 C1 114.7(3) . . . . ? C4 Zr1 C5 C1 -113.7(4) . . . . ? C8 Zr1 C5 C1 94.6(3) . . . . ? C3 Zr1 C5 C1 -76.6(3) . . . . ? C6 Zr1 C5 C1 64.0(3) . . . . ? C2 Zr1 C5 C1 -36.1(3) . . . . ? C7 Zr1 C5 C1 57.2(3) . . . . ? C11 Zr1 C5 C4 -48.5(3) . . . . ? C12 Zr1 C5 C4 -20.7(4) . . . . ? C20 Zr1 C5 C4 75.6(4) . . . . ? C10 Zr1 C5 C4 -151.4(3) . . . . ? C9 Zr1 C5 C4 -131.6(3) . . . . ? C8 Zr1 C5 C4 -151.7(3) . . . . ? C3 Zr1 C5 C4 37.2(3) . . . . ? C6 Zr1 C5 C4 177.7(3) . . . . ? C2 Zr1 C5 C4 77.6(3) . . . . ? C7 Zr1 C5 C4 170.9(3) . . . . ? C11 Zr1 C6 C7 85.2(3) . . . . ? C12 Zr1 C6 C7 36.6(4) . . . . ? C20 Zr1 C6 C7 -42.0(3) . . . . ? C10 Zr1 C6 C7 115.0(4) . . . . ? C5 Zr1 C6 C7 -168.9(3) . . . . ? C9 Zr1 C6 C7 77.8(3) . . . . ? C4 Zr1 C6 C7 -167.4(2) . . . . ? C8 Zr1 C6 C7 37.0(2) . . . . ? C3 Zr1 C6 C7 -128.3(3) . . . . ? C2 Zr1 C6 C7 -117.5(3) . . . . ? C11 Zr1 C6 C10 -29.9(4) . . . . ? C12 Zr1 C6 C10 -78.4(4) . . . . ? C20 Zr1 C6 C10 -157.1(3) . . . . ? C5 Zr1 C6 C10 76.1(3) . . . . ? C9 Zr1 C6 C10 -37.3(3) . . . . ? C4 Zr1 C6 C10 77.6(3) . . . . ? C8 Zr1 C6 C10 -78.0(3) . . . . ? C3 Zr1 C6 C10 116.6(3) . . . . ? C2 Zr1 C6 C10 127.4(3) . . . . ? C7 Zr1 C6 C10 -115.0(4) . . . . ? C10 C6 C7 C8 -0.2(4) . . . . ? Zr1 C6 C7 C8 -66.2(3) . . . . ? C10 C6 C7 Zr1 66.0(3) . . . . ? C11 Zr1 C7 C6 -118.7(3) . . . . ? C12 Zr1 C7 C6 -156.0(2) . . . . ? C20 Zr1 C7 C6 136.9(3) . . . . ? C10 Zr1 C7 C6 -37.0(3) . . . . ? C5 Zr1 C7 C6 13.2(3) . . . . ? C9 Zr1 C7 C6 -77.6(3) . . . . ? C4 Zr1 C7 C6 24.3(5) . . . . ? C8 Zr1 C7 C6 -115.3(4) . . . . ? C3 Zr1 C7 C6 82.2(3) . . . . ? C2 Zr1 C7 C6 70.6(3) . . . . ? C11 Zr1 C7 C8 -3.4(3) . . . . ? C12 Zr1 C7 C8 -40.7(3) . . . . ? C20 Zr1 C7 C8 -107.8(3) . . . . ? C10 Zr1 C7 C8 78.3(3) . . . . ? C5 Zr1 C7 C8 128.5(3) . . . . ? C9 Zr1 C7 C8 37.7(3) . . . . ? C4 Zr1 C7 C8 139.6(4) . . . . ? C3 Zr1 C7 C8 -162.5(3) . . . . ? C6 Zr1 C7 C8 115.3(4) . . . . ? C2 Zr1 C7 C8 -174.1(3) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? Zr1 C7 C8 C9 -66.6(3) . . . . ? C6 C7 C8 Zr1 66.5(3) . . . . ? C11 Zr1 C8 C7 177.1(3) . . . . ? C12 Zr1 C8 C7 143.5(3) . . . . ? C20 Zr1 C8 C7 67.4(3) . . . . ? C10 Zr1 C8 C7 -76.4(3) . . . . ? C5 Zr1 C8 C7 -76.0(4) . . . . ? C9 Zr1 C8 C7 -113.7(4) . . . . ? C4 Zr1 C8 C7 -123.9(5) . . . . ? C3 Zr1 C8 C7 66.6(8) . . . . ? C6 Zr1 C8 C7 -36.2(2) . . . . ? C2 Zr1 C8 C7 9.2(4) . . . . ? C11 Zr1 C8 C9 -69.2(3) . . . . ? C12 Zr1 C8 C9 -102.8(3) . . . . ? C20 Zr1 C8 C9 -178.9(3) . . . . ? C10 Zr1 C8 C9 37.2(2) . . . . ? C5 Zr1 C8 C9 37.6(4) . . . . ? C4 Zr1 C8 C9 -10.2(6) . . . . ? C6 Zr1 C8 C9 77.4(3) . . . . ? C2 Zr1 C8 C9 122.8(3) . . . . ? C7 Zr1 C8 C9 113.7(4) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? Zr1 C8 C9 C10 -66.9(3) . . . . ? C7 C8 C9 Zr1 67.3(3) . . . . ? C11 Zr1 C9 C10 -137.4(3) . . . . ? C12 Zr1 C9 C10 -167.2(3) . . . . ? C20 Zr1 C9 C10 115.4(3) . . . . ? C5 Zr1 C9 C10 -39.6(3) . . . . ? C4 Zr1 C9 C10 -70.2(3) . . . . ? C8 Zr1 C9 C10 114.2(4) . . . . ? C3 Zr1 C9 C10 -66.0(5) . . . . ? C6 Zr1 C9 C10 37.0(2) . . . . ? C2 Zr1 C9 C10 7.2(4) . . . . ? C7 Zr1 C9 C10 76.7(3) . . . . ? C11 Zr1 C9 C8 108.4(3) . . . . ? C12 Zr1 C9 C8 78.7(3) . . . . ? C20 Zr1 C9 C8 1.2(3) . . . . ? C10 Zr1 C9 C8 -114.2(4) . . . . ? C5 Zr1 C9 C8 -153.8(3) . . . . ? C4 Zr1 C9 C8 175.6(3) . . . . ? C3 Zr1 C9 C8 179.8(4) . . . . ? C6 Zr1 C9 C8 -77.2(3) . . . . ? C2 Zr1 C9 C8 -107.0(4) . . . . ? C7 Zr1 C9 C8 -37.5(2) . . . . ? C7 C6 C10 C9 0.4(4) . . . . ? Zr1 C6 C10 C9 67.3(3) . . . . ? C7 C6 C10 Zr1 -66.9(3) . . . . ? C8 C9 C10 C6 -0.5(4) . . . . ? Zr1 C9 C10 C6 -67.9(3) . . . . ? C8 C9 C10 Zr1 67.4(3) . . . . ? C11 Zr1 C10 C6 157.8(3) . . . . ? C12 Zr1 C10 C6 130.5(3) . . . . ? C20 Zr1 C10 C6 29.0(3) . . . . ? C5 Zr1 C10 C6 -102.8(3) . . . . ? C9 Zr1 C10 C6 114.4(4) . . . . ? C4 Zr1 C10 C6 -118.9(3) . . . . ? C8 Zr1 C10 C6 77.0(3) . . . . ? C3 Zr1 C10 C6 -93.0(3) . . . . ? C2 Zr1 C10 C6 -61.3(3) . . . . ? C7 Zr1 C10 C6 36.5(2) . . . . ? C11 Zr1 C10 C9 43.3(3) . . . . ? C12 Zr1 C10 C9 16.1(3) . . . . ? C20 Zr1 C10 C9 -85.4(3) . . . . ? C5 Zr1 C10 C9 142.8(3) . . . . ? C4 Zr1 C10 C9 126.7(3) . . . . ? C8 Zr1 C10 C9 -37.5(2) . . . . ? C3 Zr1 C10 C9 152.6(3) . . . . ? C6 Zr1 C10 C9 -114.4(4) . . . . ? C2 Zr1 C10 C9 -175.8(3) . . . . ? C7 Zr1 C10 C9 -78.0(3) . . . . ? C20 Zr1 C11 C12 0.2(3) . . . . ? C10 Zr1 C11 C12 -138.7(2) . . . . ? C5 Zr1 C11 C12 134.8(2) . . . . ? C9 Zr1 C11 C12 -117.1(3) . . . . ? C4 Zr1 C11 C12 110.6(3) . . . . ? C8 Zr1 C11 C12 -86.8(2) . . . . ? C3 Zr1 C11 C12 82.3(2) . . . . ? C6 Zr1 C11 C12 -123.1(2) . . . . ? C2 Zr1 C11 C12 84.5(3) . . . . ? C7 Zr1 C11 C12 -85.0(3) . . . . ? C12 Zr1 C11 C13 -179.2(7) . . . . ? C20 Zr1 C11 C13 -179.0(5) . . . . ? C10 Zr1 C11 C13 42.1(6) . . . . ? C5 Zr1 C11 C13 -44.4(6) . . . . ? C9 Zr1 C11 C13 63.7(6) . . . . ? C4 Zr1 C11 C13 -68.6(6) . . . . ? C8 Zr1 C11 C13 94.0(6) . . . . ? C3 Zr1 C11 C13 -96.9(6) . . . . ? C6 Zr1 C11 C13 57.7(6) . . . . ? C2 Zr1 C11 C13 -94.7(6) . . . . ? C7 Zr1 C11 C13 95.8(6) . . . . ? C13 C11 C12 C17 -0.7(9) . . . . ? Zr1 C11 C12 C17 179.9(6) . . . . ? C13 C11 C12 Zr1 179.4(5) . . . . ? C20 Zr1 C12 C11 -179.8(3) . . . . ? C10 Zr1 C12 C11 53.4(3) . . . . ? C5 Zr1 C12 C11 -55.8(3) . . . . ? C9 Zr1 C12 C11 61.8(2) . . . . ? C4 Zr1 C12 C11 -66.7(2) . . . . ? C8 Zr1 C12 C11 93.2(2) . . . . ? C3 Zr1 C12 C11 -98.1(2) . . . . ? C6 Zr1 C12 C11 93.5(3) . . . . ? C2 Zr1 C12 C11 -114.9(2) . . . . ? C7 Zr1 C12 C11 113.4(2) . . . . ? C11 Zr1 C12 C17 -179.9(7) . . . . ? C20 Zr1 C12 C17 0.2(5) . . . . ? C10 Zr1 C12 C17 -126.6(5) . . . . ? C5 Zr1 C12 C17 124.3(5) . . . . ? C9 Zr1 C12 C17 -118.1(6) . . . . ? C4 Zr1 C12 C17 113.4(6) . . . . ? C8 Zr1 C12 C17 -86.7(6) . . . . ? C3 Zr1 C12 C17 82.0(6) . . . . ? C6 Zr1 C12 C17 -86.4(6) . . . . ? C2 Zr1 C12 C17 65.2(6) . . . . ? C7 Zr1 C12 C17 -66.5(6) . . . . ? C12 C11 C13 C14 -178.3(5) . . . . ? Zr1 C11 C13 C14 0.6(8) . . . . ? C12 C11 C13 C16 62.0(7) . . . . ? Zr1 C11 C13 C16 -119.2(6) . . . . ? C12 C11 C13 C15 -58.9(7) . . . . ? Zr1 C11 C13 C15 120.0(6) . . . . ? C11 C12 C17 C18 90.4(8) . . . . ? Zr1 C12 C17 C18 -89.8(7) . . . . ? C11 C12 C17 C19 -96.6(7) . . . . ? Zr1 C12 C17 C19 83.3(7) . . . . ? C21 N1 C20 Zr1 -16(9) . . . . ? C11 Zr1 C20 N1 62(4) . . . . ? C12 Zr1 C20 N1 62(4) . . . . ? C10 Zr1 C20 N1 -172(4) . . . . ? C5 Zr1 C20 N1 -59(4) . . . . ? C9 Zr1 C20 N1 151(4) . . . . ? C4 Zr1 C20 N1 -24(4) . . . . ? C8 Zr1 C20 N1 152(4) . . . . ? C3 Zr1 C20 N1 -29(4) . . . . ? C6 Zr1 C20 N1 -157(4) . . . . ? C2 Zr1 C20 N1 -60(4) . . . . ? C7 Zr1 C20 N1 -178(100) . . . . ? C20 N1 C21 C24 -102(5) . . . . ? C20 N1 C21 C23 20(6) . . . . ? C20 N1 C21 C22 138(5) . . . . ? C25 C26 C27 C26 -177.3(17) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.621 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.065 # Attachment '- erk6214.cif' data_erk6214 _database_code_depnum_ccdc_archive 'CCDC 886397' #TrackingRef '- erk6214.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H27 N Si Zr' _chemical_formula_weight 400.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.9917(3) _cell_length_b 9.8277(4) _cell_length_c 33.0276(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3892.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5038 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 27.88 _exptl_crystal_description column _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7833 _exptl_absorpt_correction_T_max 0.9400 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29274 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4602 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+2.8529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'at N from difmap, others geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4602 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Zr1 Zr 0.457911(16) 0.157215(19) 0.385938(5) 0.02751(8) Uani 1 1 d . . . Si1 Si 0.53088(5) -0.13088(6) 0.306910(17) 0.03303(14) Uani 1 1 d . . . N1 N 0.34926(15) 0.11792(18) 0.43699(5) 0.0345(4) Uani 1 1 d . . . H01 H 0.311(2) 0.184(2) 0.4446(8) 0.041 Uiso 1 1 d . . . C1 C 0.50475(17) -0.0397(2) 0.35513(6) 0.0308(4) Uani 1 1 d . . . C2 C 0.48829(17) -0.0910(2) 0.39040(6) 0.0303(4) Uani 1 1 d . . . C3 C 0.47635(18) -0.1306(2) 0.42904(6) 0.0327(4) Uani 1 1 d . . . C4 C 0.37134(18) -0.1188(2) 0.45084(6) 0.0327(4) Uani 1 1 d . . . H4 H 0.3422 -0.1968 0.4635 0.039 Uiso 1 1 calc R . . C5 C 0.31366(17) -0.0010(2) 0.45379(5) 0.0320(4) Uani 1 1 d . . . C6 C 0.20756(18) 0.0039(2) 0.47834(7) 0.0436(5) Uani 1 1 d . . . H6A H 0.1945 -0.0843 0.4907 0.065 Uiso 1 1 calc R . . H6B H 0.1455 0.0268 0.4608 0.065 Uiso 1 1 calc R . . H6C H 0.2146 0.0723 0.4993 0.065 Uiso 1 1 calc R . . C7 C 0.5750(2) -0.1927(3) 0.45083(7) 0.0506(6) Uani 1 1 d . . . H7A H 0.5635 -0.2900 0.4537 0.076 Uiso 1 1 calc R . . H7B H 0.5822 -0.1519 0.4774 0.076 Uiso 1 1 calc R . . H7C H 0.6424 -0.1762 0.4354 0.076 Uiso 1 1 calc R . . C21 C 0.6495(2) -0.0438(3) 0.28162(8) 0.0584(7) Uani 1 1 d . . . H21A H 0.6309 0.0510 0.2772 0.088 Uiso 1 1 calc R . . H21B H 0.6644 -0.0873 0.2558 0.088 Uiso 1 1 calc R . . H21C H 0.7153 -0.0499 0.2986 0.088 Uiso 1 1 calc R . . C22 C 0.4077(2) -0.1325(2) 0.27268(6) 0.0424(5) Uani 1 1 d . . . H22A H 0.3443 -0.1714 0.2868 0.064 Uiso 1 1 calc R . . H22B H 0.4243 -0.1868 0.2489 0.064 Uiso 1 1 calc R . . H22C H 0.3902 -0.0401 0.2645 0.064 Uiso 1 1 calc R . . C23 C 0.5673(3) -0.3108(3) 0.31884(9) 0.0604(7) Uani 1 1 d . . . H23A H 0.6221 -0.3128 0.3404 0.091 Uiso 1 1 calc R . . H23B H 0.5980 -0.3541 0.2949 0.091 Uiso 1 1 calc R . . H23C H 0.5008 -0.3591 0.3274 0.091 Uiso 1 1 calc R . . C11 C 0.6670(2) 0.1590(3) 0.39838(10) 0.0578(7) Uani 1 1 d . . . H11 H 0.7091 0.0857 0.3884 0.069 Uiso 1 1 calc R . . C12 C 0.6170(2) 0.1667(3) 0.43653(8) 0.0505(6) Uani 1 1 d . . . H12 H 0.6194 0.0993 0.4567 0.061 Uiso 1 1 calc R . . C13 C 0.5631(2) 0.2919(3) 0.43937(8) 0.0509(6) Uani 1 1 d . . . H13 H 0.5224 0.3234 0.4618 0.061 Uiso 1 1 calc R . . C14 C 0.5796(3) 0.3622(3) 0.40348(9) 0.0584(7) Uani 1 1 d . . . H14 H 0.5530 0.4498 0.3974 0.070 Uiso 1 1 calc R . . C15 C 0.6432(2) 0.2791(3) 0.37786(9) 0.0627(8) Uani 1 1 d . . . H15 H 0.6658 0.3008 0.3514 0.075 Uiso 1 1 calc R . . C16 C 0.3981(2) 0.2082(2) 0.31309(6) 0.0391(5) Uani 1 1 d . . . H16 H 0.4424 0.1739 0.2920 0.047 Uiso 1 1 calc R . . C17 C 0.30581(19) 0.1421(2) 0.33083(6) 0.0391(5) Uani 1 1 d . . . H17 H 0.2781 0.0559 0.3237 0.047 Uiso 1 1 calc R . . C18 C 0.2630(2) 0.2267(3) 0.36079(6) 0.0483(6) Uani 1 1 d . . . H18 H 0.2002 0.2087 0.3769 0.058 Uiso 1 1 calc R . . C19 C 0.3297(3) 0.3433(2) 0.36281(7) 0.0548(7) Uani 1 1 d . . . H19 H 0.3212 0.4157 0.3812 0.066 Uiso 1 1 calc R . . C20 C 0.4120(3) 0.3331(2) 0.33235(7) 0.0504(6) Uani 1 1 d . . . H20 H 0.4664 0.3988 0.3262 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.03165(12) 0.02793(12) 0.02293(11) 0.00073(6) 0.00149(6) -0.00185(7) Si1 0.0331(3) 0.0373(3) 0.0287(3) -0.0055(2) 0.0010(2) 0.0030(2) N1 0.0397(10) 0.0330(9) 0.0308(8) 0.0030(7) 0.0096(7) 0.0041(7) C1 0.0308(9) 0.0323(10) 0.0292(9) -0.0011(7) 0.0005(7) 0.0023(8) C2 0.0294(9) 0.0309(10) 0.0306(9) -0.0024(7) -0.0021(7) 0.0044(8) C3 0.0385(11) 0.0305(10) 0.0291(9) 0.0011(8) -0.0038(8) 0.0032(8) C4 0.0400(11) 0.0322(9) 0.0260(8) 0.0028(7) -0.0008(8) -0.0055(9) C5 0.0333(10) 0.0400(10) 0.0227(8) 0.0009(7) -0.0017(7) -0.0048(8) C6 0.0389(11) 0.0497(13) 0.0422(11) 0.0015(10) 0.0101(9) -0.0042(10) C7 0.0511(14) 0.0621(15) 0.0385(12) 0.0083(11) -0.0072(11) 0.0167(13) C21 0.0419(13) 0.083(2) 0.0500(14) -0.0114(13) 0.0150(11) -0.0081(13) C22 0.0431(12) 0.0515(13) 0.0325(10) -0.0077(9) -0.0038(9) 0.0022(10) C23 0.0775(19) 0.0447(14) 0.0589(16) -0.0119(12) -0.0115(14) 0.0179(14) C11 0.0334(12) 0.0645(18) 0.0754(18) -0.0206(14) -0.0006(12) -0.0090(12) C12 0.0461(13) 0.0551(15) 0.0504(13) 0.0009(11) -0.0178(11) -0.0128(11) C13 0.0534(14) 0.0570(15) 0.0424(12) -0.0137(11) -0.0042(11) -0.0151(12) C14 0.0697(18) 0.0425(14) 0.0631(17) 0.0011(12) -0.0114(15) -0.0234(13) C15 0.0556(16) 0.081(2) 0.0516(14) -0.0021(14) 0.0097(12) -0.0357(16) C16 0.0529(13) 0.0381(11) 0.0263(9) 0.0059(8) 0.0001(9) 0.0044(10) C17 0.0400(12) 0.0445(12) 0.0329(10) 0.0065(9) -0.0055(9) 0.0050(9) C18 0.0446(13) 0.0650(16) 0.0354(10) 0.0053(11) -0.0009(9) 0.0223(12) C19 0.085(2) 0.0410(13) 0.0385(12) -0.0010(10) -0.0084(13) 0.0267(13) C20 0.0795(18) 0.0325(12) 0.0392(12) 0.0115(9) -0.0060(12) -0.0034(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.1655(17) . ? Zr1 C1 2.257(2) . ? Zr1 C2 2.471(2) . ? Zr1 C19 2.509(2) . ? Zr1 C20 2.534(2) . ? Zr1 C12 2.538(2) . ? Zr1 C15 2.538(3) . ? Zr1 C11 2.540(3) . ? Zr1 C13 2.541(2) . ? Zr1 C14 2.554(3) . ? Zr1 C16 2.5602(19) . ? Zr1 C18 2.572(2) . ? Si1 C1 1.854(2) . ? Si1 C21 1.858(3) . ? Si1 C22 1.860(2) . ? Si1 C23 1.863(3) . ? N1 C5 1.363(3) . ? N1 H01 0.84(2) . ? C1 C2 1.284(3) . ? C2 C3 1.342(3) . ? C3 C4 1.455(3) . ? C3 C7 1.513(3) . ? C4 C5 1.352(3) . ? C4 H4 0.9400 . ? C5 C6 1.509(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C11 C15 1.391(4) . ? C11 C12 1.397(4) . ? C11 H11 0.9400 . ? C12 C13 1.394(4) . ? C12 H12 0.9400 . ? C13 C14 1.386(4) . ? C13 H13 0.9400 . ? C14 C15 1.402(4) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C20 1.393(3) . ? C16 C17 1.410(3) . ? C16 H16 0.9400 . ? C17 C18 1.391(3) . ? C17 H17 0.9400 . ? C18 C19 1.398(4) . ? C18 H18 0.9400 . ? C19 C20 1.413(4) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C1 110.35(7) . . ? N1 Zr1 C2 82.31(7) . . ? C1 Zr1 C2 31.11(6) . . ? N1 Zr1 C19 89.90(8) . . ? C1 Zr1 C19 129.82(8) . . ? C2 Zr1 C19 145.93(9) . . ? N1 Zr1 C20 122.31(9) . . ? C1 Zr1 C20 108.91(7) . . ? C2 Zr1 C20 138.33(7) . . ? C19 Zr1 C20 32.54(9) . . ? N1 Zr1 C12 86.92(8) . . ? C1 Zr1 C12 98.11(8) . . ? C2 Zr1 C12 83.46(7) . . ? C19 Zr1 C12 129.39(9) . . ? C20 Zr1 C12 126.74(9) . . ? N1 Zr1 C15 133.84(8) . . ? C1 Zr1 C15 98.01(9) . . ? C2 Zr1 C15 110.07(10) . . ? C19 Zr1 C15 99.24(11) . . ? C20 Zr1 C15 78.17(11) . . ? C12 Zr1 C15 52.69(9) . . ? N1 Zr1 C11 117.97(9) . . ? C1 Zr1 C11 80.39(8) . . ? C2 Zr1 C11 81.46(8) . . ? C19 Zr1 C11 130.48(10) . . ? C20 Zr1 C11 108.83(10) . . ? C12 Zr1 C11 31.94(9) . . ? C15 Zr1 C11 31.79(10) . . ? N1 Zr1 C13 81.41(8) . . ? C1 Zr1 C13 129.50(8) . . ? C2 Zr1 C13 113.56(8) . . ? C19 Zr1 C13 97.81(9) . . ? C20 Zr1 C13 103.74(9) . . ? C12 Zr1 C13 31.85(9) . . ? C15 Zr1 C13 52.61(9) . . ? C11 Zr1 C13 52.73(9) . . ? N1 Zr1 C14 107.93(9) . . ? C1 Zr1 C14 129.51(9) . . ? C2 Zr1 C14 132.92(9) . . ? C19 Zr1 C14 81.04(11) . . ? C20 Zr1 C14 75.20(9) . . ? C12 Zr1 C14 52.57(9) . . ? C15 Zr1 C14 31.95(10) . . ? C11 Zr1 C14 52.72(10) . . ? C13 Zr1 C14 31.58(9) . . ? N1 Zr1 C16 126.72(7) . . ? C1 Zr1 C16 79.27(7) . . ? C2 Zr1 C16 106.89(7) . . ? C19 Zr1 C16 53.09(8) . . ? C20 Zr1 C16 31.73(7) . . ? C12 Zr1 C16 145.31(8) . . ? C15 Zr1 C16 93.11(9) . . ? C11 Zr1 C16 115.29(9) . . ? C13 Zr1 C16 133.62(8) . . ? C14 Zr1 C16 102.65(9) . . ? N1 Zr1 C18 75.66(7) . . ? C1 Zr1 C18 107.95(8) . . ? C2 Zr1 C18 114.55(8) . . ? C19 Zr1 C18 31.92(9) . . ? C20 Zr1 C18 52.84(9) . . ? C12 Zr1 C18 152.35(8) . . ? C15 Zr1 C18 129.48(10) . . ? C11 Zr1 C18 161.23(10) . . ? C13 Zr1 C18 122.46(9) . . ? C14 Zr1 C18 112.50(10) . . ? C16 Zr1 C18 52.41(7) . . ? C1 Si1 C21 107.03(11) . . ? C1 Si1 C22 113.07(10) . . ? C21 Si1 C22 109.80(12) . . ? C1 Si1 C23 108.46(11) . . ? C21 Si1 C23 110.63(15) . . ? C22 Si1 C23 107.86(12) . . ? C5 N1 Zr1 131.20(14) . . ? C5 N1 H01 111.7(17) . . ? Zr1 N1 H01 115.4(18) . . ? C2 C1 Si1 127.94(16) . . ? C2 C1 Zr1 83.67(13) . . ? Si1 C1 Zr1 147.53(11) . . ? C1 C2 C3 173.0(2) . . ? C1 C2 Zr1 65.22(12) . . ? C3 C2 Zr1 109.10(14) . . ? C2 C3 C4 122.66(19) . . ? C2 C3 C7 119.1(2) . . ? C4 C3 C7 118.25(19) . . ? C5 C4 C3 123.17(18) . . ? C5 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C4 C5 N1 123.00(18) . . ? C4 C5 C6 119.83(19) . . ? N1 C5 C6 117.10(18) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C15 C11 C12 107.8(3) . . ? C15 C11 Zr1 74.00(16) . . ? C12 C11 Zr1 73.93(15) . . ? C15 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Zr1 C11 H11 117.9 . . ? C13 C12 C11 107.9(2) . . ? C13 C12 Zr1 74.19(14) . . ? C11 C12 Zr1 74.13(15) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Zr1 C12 H12 117.6 . . ? C14 C13 C12 108.4(3) . . ? C14 C13 Zr1 74.74(14) . . ? C12 C13 Zr1 73.95(14) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Zr1 C13 H13 117.5 . . ? C13 C14 C15 107.7(3) . . ? C13 C14 Zr1 73.68(14) . . ? C15 C14 Zr1 73.39(15) . . ? C13 C14 H14 126.2 . . ? C15 C14 H14 126.2 . . ? Zr1 C14 H14 118.7 . . ? C11 C15 C14 108.2(3) . . ? C11 C15 Zr1 74.20(15) . . ? C14 C15 Zr1 74.66(15) . . ? C11 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? Zr1 C15 H15 117.2 . . ? C20 C16 C17 108.1(2) . . ? C20 C16 Zr1 73.11(12) . . ? C17 C16 Zr1 74.90(11) . . ? C20 C16 H16 126.0 . . ? C17 C16 H16 126.0 . . ? Zr1 C16 H16 118.0 . . ? C18 C17 C16 108.0(2) . . ? C18 C17 Zr1 74.00(13) . . ? C16 C17 Zr1 73.27(12) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Zr1 C17 H17 118.7 . . ? C17 C18 C19 108.3(2) . . ? C17 C18 Zr1 74.69(13) . . ? C19 C18 Zr1 71.53(14) . . ? C17 C18 H18 125.9 . . ? C19 C18 H18 125.9 . . ? Zr1 C18 H18 119.7 . . ? C18 C19 C20 107.9(2) . . ? C18 C19 Zr1 76.55(13) . . ? C20 C19 Zr1 74.73(14) . . ? C18 C19 H19 126.1 . . ? C20 C19 H19 126.1 . . ? Zr1 C19 H19 114.9 . . ? C16 C20 C19 107.7(2) . . ? C16 C20 Zr1 75.16(12) . . ? C19 C20 Zr1 72.73(13) . . ? C16 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? Zr1 C20 H20 118.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Zr1 N1 C5 4.9(2) . . . . ? C2 Zr1 N1 C5 -8.79(18) . . . . ? C19 Zr1 N1 C5 137.94(19) . . . . ? C20 Zr1 N1 C5 134.97(18) . . . . ? C12 Zr1 N1 C5 -92.60(19) . . . . ? C15 Zr1 N1 C5 -119.3(2) . . . . ? C11 Zr1 N1 C5 -84.8(2) . . . . ? C13 Zr1 N1 C5 -124.2(2) . . . . ? C14 Zr1 N1 C5 -141.52(19) . . . . ? C16 Zr1 N1 C5 96.57(19) . . . . ? C18 Zr1 N1 C5 109.1(2) . . . . ? C21 Si1 C1 C2 -134.2(2) . . . . ? C22 Si1 C1 C2 104.8(2) . . . . ? C23 Si1 C1 C2 -14.8(2) . . . . ? C21 Si1 C1 Zr1 61.0(2) . . . . ? C22 Si1 C1 Zr1 -60.0(2) . . . . ? C23 Si1 C1 Zr1 -179.6(2) . . . . ? N1 Zr1 C1 C2 -27.03(15) . . . . ? C19 Zr1 C1 C2 -134.89(15) . . . . ? C20 Zr1 C1 C2 -163.89(14) . . . . ? C12 Zr1 C1 C2 62.69(14) . . . . ? C15 Zr1 C1 C2 115.94(14) . . . . ? C11 Zr1 C1 C2 89.37(15) . . . . ? C13 Zr1 C1 C2 68.68(16) . . . . ? C14 Zr1 C1 C2 109.98(15) . . . . ? C16 Zr1 C1 C2 -152.39(14) . . . . ? C18 Zr1 C1 C2 -107.96(14) . . . . ? N1 Zr1 C1 Si1 140.93(19) . . . . ? C2 Zr1 C1 Si1 168.0(3) . . . . ? C19 Zr1 C1 Si1 33.1(3) . . . . ? C20 Zr1 C1 Si1 4.1(2) . . . . ? C12 Zr1 C1 Si1 -129.4(2) . . . . ? C15 Zr1 C1 Si1 -76.1(2) . . . . ? C11 Zr1 C1 Si1 -102.7(2) . . . . ? C13 Zr1 C1 Si1 -123.4(2) . . . . ? C14 Zr1 C1 Si1 -82.1(2) . . . . ? C16 Zr1 C1 Si1 15.6(2) . . . . ? C18 Zr1 C1 Si1 60.0(2) . . . . ? Si1 C1 C2 C3 152.0(17) . . . . ? Zr1 C1 C2 C3 -36.2(18) . . . . ? Si1 C1 C2 Zr1 -171.8(2) . . . . ? N1 Zr1 C2 C1 154.54(14) . . . . ? C19 Zr1 C2 C1 76.24(19) . . . . ? C20 Zr1 C2 C1 23.3(2) . . . . ? C12 Zr1 C2 C1 -117.70(14) . . . . ? C15 Zr1 C2 C1 -71.45(15) . . . . ? C11 Zr1 C2 C1 -85.54(15) . . . . ? C13 Zr1 C2 C1 -128.36(14) . . . . ? C14 Zr1 C2 C1 -98.09(16) . . . . ? C16 Zr1 C2 C1 28.41(15) . . . . ? C18 Zr1 C2 C1 84.20(14) . . . . ? N1 Zr1 C2 C3 -29.80(15) . . . . ? C1 Zr1 C2 C3 175.7(2) . . . . ? C19 Zr1 C2 C3 -108.10(18) . . . . ? C20 Zr1 C2 C3 -161.08(16) . . . . ? C12 Zr1 C2 C3 57.96(16) . . . . ? C15 Zr1 C2 C3 104.22(16) . . . . ? C11 Zr1 C2 C3 90.13(16) . . . . ? C13 Zr1 C2 C3 47.30(17) . . . . ? C14 Zr1 C2 C3 77.58(19) . . . . ? C16 Zr1 C2 C3 -155.92(15) . . . . ? C18 Zr1 C2 C3 -100.14(16) . . . . ? C1 C2 C3 C4 98.1(18) . . . . ? Zr1 C2 C3 C4 63.6(2) . . . . ? C1 C2 C3 C7 -83.1(18) . . . . ? Zr1 C2 C3 C7 -117.6(2) . . . . ? C2 C3 C4 C5 -53.4(3) . . . . ? C7 C3 C4 C5 127.8(2) . . . . ? C3 C4 C5 N1 -0.8(3) . . . . ? C3 C4 C5 C6 -177.64(19) . . . . ? Zr1 N1 C5 C4 25.4(3) . . . . ? Zr1 N1 C5 C6 -157.67(15) . . . . ? N1 Zr1 C11 C15 -129.19(17) . . . . ? C1 Zr1 C11 C15 122.78(18) . . . . ? C2 Zr1 C11 C15 154.28(18) . . . . ? C19 Zr1 C11 C15 -12.4(2) . . . . ? C20 Zr1 C11 C15 15.96(19) . . . . ? C12 Zr1 C11 C15 -114.4(2) . . . . ? C13 Zr1 C11 C15 -77.25(18) . . . . ? C14 Zr1 C11 C15 -37.26(17) . . . . ? C16 Zr1 C11 C15 49.57(19) . . . . ? C18 Zr1 C11 C15 4.5(4) . . . . ? N1 Zr1 C11 C12 -14.79(19) . . . . ? C1 Zr1 C11 C12 -122.82(17) . . . . ? C2 Zr1 C11 C12 -91.32(16) . . . . ? C19 Zr1 C11 C12 102.00(18) . . . . ? C20 Zr1 C11 C12 130.36(16) . . . . ? C15 Zr1 C11 C12 114.4(2) . . . . ? C13 Zr1 C11 C12 37.15(15) . . . . ? C14 Zr1 C11 C12 77.14(17) . . . . ? C16 Zr1 C11 C12 163.97(15) . . . . ? C18 Zr1 C11 C12 118.9(3) . . . . ? C15 C11 C12 C13 -0.2(3) . . . . ? Zr1 C11 C12 C13 -67.07(17) . . . . ? C15 C11 C12 Zr1 66.83(18) . . . . ? N1 Zr1 C12 C13 -78.65(16) . . . . ? C1 Zr1 C12 C13 171.22(16) . . . . ? C2 Zr1 C12 C13 -161.26(16) . . . . ? C19 Zr1 C12 C13 8.7(2) . . . . ? C20 Zr1 C12 C13 50.2(2) . . . . ? C15 Zr1 C12 C13 77.29(18) . . . . ? C11 Zr1 C12 C13 114.4(2) . . . . ? C14 Zr1 C12 C13 36.77(16) . . . . ? C16 Zr1 C12 C13 88.4(2) . . . . ? C18 Zr1 C12 C13 -28.2(3) . . . . ? N1 Zr1 C12 C11 166.95(17) . . . . ? C1 Zr1 C12 C11 56.82(17) . . . . ? C2 Zr1 C12 C11 84.34(16) . . . . ? C19 Zr1 C12 C11 -105.71(18) . . . . ? C20 Zr1 C12 C11 -64.2(2) . . . . ? C15 Zr1 C12 C11 -37.10(17) . . . . ? C13 Zr1 C12 C11 -114.4(2) . . . . ? C14 Zr1 C12 C11 -77.63(18) . . . . ? C16 Zr1 C12 C11 -26.0(2) . . . . ? C18 Zr1 C12 C11 -142.6(2) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? Zr1 C12 C13 C14 -67.39(18) . . . . ? C11 C12 C13 Zr1 67.03(17) . . . . ? N1 Zr1 C13 C14 -147.1(2) . . . . ? C1 Zr1 C13 C14 103.5(2) . . . . ? C2 Zr1 C13 C14 135.17(18) . . . . ? C19 Zr1 C13 C14 -58.4(2) . . . . ? C20 Zr1 C13 C14 -25.8(2) . . . . ? C12 Zr1 C13 C14 114.8(3) . . . . ? C15 Zr1 C13 C14 37.2(2) . . . . ? C11 Zr1 C13 C14 77.5(2) . . . . ? C16 Zr1 C13 C14 -13.4(2) . . . . ? C18 Zr1 C13 C14 -80.3(2) . . . . ? N1 Zr1 C13 C12 98.06(16) . . . . ? C1 Zr1 C13 C12 -11.3(2) . . . . ? C2 Zr1 C13 C12 20.38(18) . . . . ? C19 Zr1 C13 C12 -173.24(16) . . . . ? C20 Zr1 C13 C12 -140.64(17) . . . . ? C15 Zr1 C13 C12 -77.55(18) . . . . ? C11 Zr1 C13 C12 -37.26(16) . . . . ? C14 Zr1 C13 C12 -114.8(3) . . . . ? C16 Zr1 C13 C12 -128.20(16) . . . . ? C18 Zr1 C13 C12 164.91(15) . . . . ? C12 C13 C14 C15 0.8(3) . . . . ? Zr1 C13 C14 C15 -66.05(19) . . . . ? C12 C13 C14 Zr1 66.87(17) . . . . ? N1 Zr1 C14 C13 34.3(2) . . . . ? C1 Zr1 C14 C13 -103.47(19) . . . . ? C2 Zr1 C14 C13 -61.9(2) . . . . ? C19 Zr1 C14 C13 121.3(2) . . . . ? C20 Zr1 C14 C13 154.0(2) . . . . ? C12 Zr1 C14 C13 -37.11(17) . . . . ? C15 Zr1 C14 C13 -114.7(3) . . . . ? C11 Zr1 C14 C13 -77.6(2) . . . . ? C16 Zr1 C14 C13 170.10(18) . . . . ? C18 Zr1 C14 C13 115.81(18) . . . . ? N1 Zr1 C14 C15 148.99(18) . . . . ? C1 Zr1 C14 C15 11.2(2) . . . . ? C2 Zr1 C14 C15 52.7(2) . . . . ? C19 Zr1 C14 C15 -124.05(19) . . . . ? C20 Zr1 C14 C15 -91.3(2) . . . . ? C12 Zr1 C14 C15 77.6(2) . . . . ? C11 Zr1 C14 C15 37.07(18) . . . . ? C13 Zr1 C14 C15 114.7(3) . . . . ? C16 Zr1 C14 C15 -75.23(19) . . . . ? C18 Zr1 C14 C15 -129.52(18) . . . . ? C12 C11 C15 C14 0.7(3) . . . . ? Zr1 C11 C15 C14 67.52(19) . . . . ? C12 C11 C15 Zr1 -66.78(18) . . . . ? C13 C14 C15 C11 -1.0(3) . . . . ? Zr1 C14 C15 C11 -67.22(19) . . . . ? C13 C14 C15 Zr1 66.25(19) . . . . ? N1 Zr1 C15 C11 71.6(2) . . . . ? C1 Zr1 C15 C11 -56.84(18) . . . . ? C2 Zr1 C15 C11 -27.19(19) . . . . ? C19 Zr1 C15 C11 170.47(17) . . . . ? C20 Zr1 C15 C11 -164.58(19) . . . . ? C12 Zr1 C15 C11 37.28(16) . . . . ? C13 Zr1 C15 C11 77.67(18) . . . . ? C14 Zr1 C15 C11 114.5(3) . . . . ? C16 Zr1 C15 C11 -136.43(17) . . . . ? C18 Zr1 C15 C11 -178.11(15) . . . . ? N1 Zr1 C15 C14 -42.8(2) . . . . ? C1 Zr1 C15 C14 -171.30(18) . . . . ? C2 Zr1 C15 C14 -141.65(17) . . . . ? C19 Zr1 C15 C14 56.02(19) . . . . ? C20 Zr1 C15 C14 80.96(19) . . . . ? C12 Zr1 C15 C14 -77.18(19) . . . . ? C11 Zr1 C15 C14 -114.5(3) . . . . ? C13 Zr1 C15 C14 -36.79(17) . . . . ? C16 Zr1 C15 C14 109.11(18) . . . . ? C18 Zr1 C15 C14 67.4(2) . . . . ? N1 Zr1 C16 C20 93.53(18) . . . . ? C1 Zr1 C16 C20 -158.99(18) . . . . ? C2 Zr1 C16 C20 -173.48(17) . . . . ? C19 Zr1 C16 C20 37.80(18) . . . . ? C12 Zr1 C16 C20 -70.2(2) . . . . ? C15 Zr1 C16 C20 -61.42(19) . . . . ? C11 Zr1 C16 C20 -85.10(18) . . . . ? C13 Zr1 C16 C20 -23.4(2) . . . . ? C14 Zr1 C16 C20 -30.59(19) . . . . ? C18 Zr1 C16 C20 78.21(18) . . . . ? N1 Zr1 C16 C17 -21.15(16) . . . . ? C1 Zr1 C16 C17 86.33(14) . . . . ? C2 Zr1 C16 C17 71.84(14) . . . . ? C19 Zr1 C16 C17 -76.88(16) . . . . ? C20 Zr1 C16 C17 -114.7(2) . . . . ? C12 Zr1 C16 C17 175.09(14) . . . . ? C15 Zr1 C16 C17 -176.10(15) . . . . ? C11 Zr1 C16 C17 160.22(13) . . . . ? C13 Zr1 C16 C17 -138.12(14) . . . . ? C14 Zr1 C16 C17 -145.27(14) . . . . ? C18 Zr1 C16 C17 -36.47(14) . . . . ? C20 C16 C17 C18 0.2(2) . . . . ? Zr1 C16 C17 C18 66.39(15) . . . . ? C20 C16 C17 Zr1 -66.14(16) . . . . ? N1 Zr1 C17 C18 48.10(16) . . . . ? C1 Zr1 C17 C18 157.63(16) . . . . ? C2 Zr1 C17 C18 130.92(15) . . . . ? C19 Zr1 C17 C18 -36.78(15) . . . . ? C20 Zr1 C17 C18 -78.03(17) . . . . ? C12 Zr1 C17 C18 -160.4(11) . . . . ? C15 Zr1 C17 C18 -110.24(17) . . . . ? C11 Zr1 C17 C18 -146.58(17) . . . . ? C13 Zr1 C17 C18 -36.0(2) . . . . ? C14 Zr1 C17 C18 -70.49(18) . . . . ? C16 Zr1 C17 C18 -115.0(2) . . . . ? N1 Zr1 C17 C16 163.08(13) . . . . ? C1 Zr1 C17 C16 -87.39(14) . . . . ? C2 Zr1 C17 C16 -114.09(13) . . . . ? C19 Zr1 C17 C16 78.21(15) . . . . ? C20 Zr1 C17 C16 36.95(14) . . . . ? C12 Zr1 C17 C16 -45.4(12) . . . . ? C15 Zr1 C17 C16 4.75(18) . . . . ? C11 Zr1 C17 C16 -31.6(2) . . . . ? C13 Zr1 C17 C16 79.0(2) . . . . ? C14 Zr1 C17 C16 44.50(17) . . . . ? C18 Zr1 C17 C16 115.0(2) . . . . ? C16 C17 C18 C19 -1.8(2) . . . . ? Zr1 C17 C18 C19 64.13(16) . . . . ? C16 C17 C18 Zr1 -65.90(15) . . . . ? N1 Zr1 C18 C17 -130.25(16) . . . . ? C1 Zr1 C18 C17 -23.12(16) . . . . ? C2 Zr1 C18 C17 -55.83(16) . . . . ? C19 Zr1 C18 C17 115.7(2) . . . . ? C20 Zr1 C18 C17 77.36(15) . . . . ? C12 Zr1 C18 C17 177.17(16) . . . . ? C15 Zr1 C18 C17 94.05(17) . . . . ? C11 Zr1 C18 C17 91.0(3) . . . . ? C13 Zr1 C18 C17 159.95(14) . . . . ? C14 Zr1 C18 C17 125.99(15) . . . . ? C16 Zr1 C18 C17 37.12(13) . . . . ? N1 Zr1 C18 C19 114.02(15) . . . . ? C1 Zr1 C18 C19 -138.85(14) . . . . ? C2 Zr1 C18 C19 -171.56(14) . . . . ? C20 Zr1 C18 C19 -38.38(14) . . . . ? C12 Zr1 C18 C19 61.4(2) . . . . ? C15 Zr1 C18 C19 -21.68(19) . . . . ? C11 Zr1 C18 C19 -24.8(3) . . . . ? C13 Zr1 C18 C19 44.22(17) . . . . ? C14 Zr1 C18 C19 10.25(17) . . . . ? C16 Zr1 C18 C19 -78.61(16) . . . . ? C17 C18 C19 C20 2.6(3) . . . . ? Zr1 C18 C19 C20 68.81(17) . . . . ? C17 C18 C19 Zr1 -66.21(16) . . . . ? N1 Zr1 C19 C18 -62.24(14) . . . . ? C1 Zr1 C19 C18 54.58(19) . . . . ? C2 Zr1 C19 C18 13.8(2) . . . . ? C20 Zr1 C19 C18 113.1(2) . . . . ? C12 Zr1 C19 C18 -148.18(14) . . . . ? C15 Zr1 C19 C18 163.21(14) . . . . ? C11 Zr1 C19 C18 169.79(14) . . . . ? C13 Zr1 C19 C18 -143.56(14) . . . . ? C14 Zr1 C19 C18 -170.42(16) . . . . ? C16 Zr1 C19 C18 76.27(15) . . . . ? N1 Zr1 C19 C20 -175.33(16) . . . . ? C1 Zr1 C19 C20 -58.5(2) . . . . ? C2 Zr1 C19 C20 -99.3(2) . . . . ? C12 Zr1 C19 C20 98.74(17) . . . . ? C15 Zr1 C19 C20 50.12(17) . . . . ? C11 Zr1 C19 C20 56.7(2) . . . . ? C13 Zr1 C19 C20 103.35(16) . . . . ? C14 Zr1 C19 C20 76.49(17) . . . . ? C16 Zr1 C19 C20 -36.82(15) . . . . ? C18 Zr1 C19 C20 -113.1(2) . . . . ? C17 C16 C20 C19 1.3(3) . . . . ? Zr1 C16 C20 C19 -65.98(17) . . . . ? C17 C16 C20 Zr1 67.33(15) . . . . ? C18 C19 C20 C16 -2.4(3) . . . . ? Zr1 C19 C20 C16 67.61(17) . . . . ? C18 C19 C20 Zr1 -70.05(16) . . . . ? N1 Zr1 C20 C16 -108.80(16) . . . . ? C1 Zr1 C20 C16 21.86(19) . . . . ? C2 Zr1 C20 C16 9.4(2) . . . . ? C19 Zr1 C20 C16 -114.3(2) . . . . ? C12 Zr1 C20 C16 138.07(16) . . . . ? C15 Zr1 C20 C16 116.38(18) . . . . ? C11 Zr1 C20 C16 107.87(17) . . . . ? C13 Zr1 C20 C16 162.75(16) . . . . ? C14 Zr1 C20 C16 149.10(19) . . . . ? C18 Zr1 C20 C16 -76.72(17) . . . . ? N1 Zr1 C20 C19 5.52(19) . . . . ? C1 Zr1 C20 C19 136.19(16) . . . . ? C2 Zr1 C20 C19 123.73(17) . . . . ? C12 Zr1 C20 C19 -107.60(18) . . . . ? C15 Zr1 C20 C19 -129.29(18) . . . . ? C11 Zr1 C20 C19 -137.80(17) . . . . ? C13 Zr1 C20 C19 -82.92(18) . . . . ? C14 Zr1 C20 C19 -96.57(18) . . . . ? C16 Zr1 C20 C19 114.3(2) . . . . ? C18 Zr1 C20 C19 37.61(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.368 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.060 # Attachment '- erk6382.cif' data_erk6382 _database_code_depnum_ccdc_archive 'CCDC 886398' #TrackingRef '- erk6382.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H38 Si Zr' _chemical_formula_weight 481.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8130(2) _cell_length_b 9.2076(3) _cell_length_c 16.7639(6) _cell_angle_alpha 80.358(2) _cell_angle_beta 77.962(2) _cell_angle_gamma 72.931(2) _cell_volume 1263.57(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2947 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.8867 _exptl_absorpt_process_details 'Denzo (Otwinowski, Bore, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10822 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4312 _reflns_number_gt 4209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+1.2857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4312 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 0.74330(3) 0.61871(2) 0.264305(14) 0.02793(10) Uani 1 1 d . . . Si1 Si 0.80837(9) 0.84319(10) 0.42630(5) 0.04187(19) Uani 1 1 d . . . C1 C 0.7334(3) 0.8139(3) 0.33806(15) 0.0321(5) Uani 1 1 d . . . C2 C 0.6398(3) 0.9247(3) 0.29852(15) 0.0337(5) Uani 1 1 d . . . C3 C 0.5442(4) 1.0296(3) 0.25346(17) 0.0398(6) Uani 1 1 d . . . C4 C 0.6129(4) 1.1080(3) 0.17337(18) 0.0468(7) Uani 1 1 d . . . H4A H 0.5701 1.2188 0.1744 0.056 Uiso 1 1 calc R . . H4B H 0.5743 1.0805 0.1287 0.056 Uiso 1 1 calc R . . C5 C 0.7945(4) 1.0707(3) 0.15389(19) 0.0482(7) Uani 1 1 d . . . H5A H 0.8340 1.0823 0.2023 0.058 Uiso 1 1 calc R . . H5B H 0.8244 1.1463 0.1095 0.058 Uiso 1 1 calc R . . C6 C 0.8807(4) 0.9129(3) 0.12878(16) 0.0387(6) Uani 1 1 d . . . C7 C 0.8024(3) 0.8117(3) 0.12575(14) 0.0311(5) Uani 1 1 d . . . C8 C 0.7320(3) 0.7062(3) 0.12790(14) 0.0276(5) Uani 1 1 d . . . C9 C 0.3644(4) 1.0779(4) 0.2776(2) 0.0565(8) Uani 1 1 d . . . H9A H 0.3331 1.0239 0.3305 0.085 Uiso 1 1 calc R . . H9B H 0.3149 1.0538 0.2367 0.085 Uiso 1 1 calc R . . H9C H 0.3288 1.1871 0.2811 0.085 Uiso 1 1 calc R . . C10 C 1.0607(4) 0.8805(4) 0.1042(2) 0.0557(8) Uani 1 1 d . . . H10A H 1.1047 0.7769 0.0896 0.084 Uiso 1 1 calc R . . H10B H 1.1071 0.8918 0.1497 0.084 Uiso 1 1 calc R . . H10C H 1.0863 0.9520 0.0573 0.084 Uiso 1 1 calc R . . C11 C 0.9933(4) 0.4904(4) 0.3280(2) 0.0531(8) Uani 1 1 d . . . H11 H 0.9937 0.5154 0.3801 0.064 Uiso 1 1 calc R . . C12 C 0.9392(4) 0.3726(4) 0.3124(2) 0.0569(9) Uani 1 1 d . . . H12 H 0.8983 0.3024 0.3521 0.068 Uiso 1 1 calc R . . C13 C 0.9562(4) 0.3766(3) 0.2269(2) 0.0486(7) Uani 1 1 d . . . H13 H 0.9256 0.3117 0.1993 0.058 Uiso 1 1 calc R . . C14 C 1.0263(3) 0.4939(3) 0.19043(18) 0.0427(6) Uani 1 1 d . . . H14 H 1.0544 0.5198 0.1337 0.051 Uiso 1 1 calc R . . C15 C 1.0478(3) 0.5662(3) 0.2521(2) 0.0456(7) Uani 1 1 d . . . H15 H 1.0909 0.6505 0.2444 0.055 Uiso 1 1 calc R . . C16 C 0.4800(4) 0.6499(4) 0.36642(19) 0.0491(7) Uani 1 1 d . . . H16 H 0.4523 0.7238 0.4032 0.059 Uiso 1 1 calc R . . C17 C 0.5705(4) 0.4978(4) 0.38005(19) 0.0493(7) Uani 1 1 d . . . H17 H 0.6169 0.4527 0.4270 0.059 Uiso 1 1 calc R . . C18 C 0.5799(4) 0.4246(3) 0.31177(19) 0.0458(7) Uani 1 1 d . . . H18 H 0.6316 0.3213 0.3053 0.055 Uiso 1 1 calc R . . C19 C 0.4989(3) 0.5324(3) 0.25489(18) 0.0429(6) Uani 1 1 d . . . H19 H 0.4872 0.5141 0.2033 0.051 Uiso 1 1 calc R . . C20 C 0.4380(3) 0.6722(3) 0.2880(2) 0.0446(7) Uani 1 1 d . . . H20 H 0.3796 0.7644 0.2624 0.053 Uiso 1 1 calc R . . C21 C 0.7599(5) 0.7042(4) 0.5142(2) 0.0684(11) Uani 1 1 d . . . H21A H 0.6442 0.7187 0.5268 0.103 Uiso 1 1 calc R . . H21B H 0.7976 0.7199 0.5616 0.103 Uiso 1 1 calc R . . H21C H 0.8123 0.6011 0.5003 0.103 Uiso 1 1 calc R . . C22 C 1.0272(5) 0.8227(7) 0.4035(3) 0.0955(17) Uani 1 1 d . . . H22A H 1.0517 0.8920 0.3553 0.143 Uiso 1 1 calc R . . H22B H 1.0839 0.7183 0.3932 0.143 Uiso 1 1 calc R . . H22C H 1.0611 0.8471 0.4499 0.143 Uiso 1 1 calc R . . C23 C 0.7112(4) 1.0391(4) 0.4548(2) 0.0553(8) Uani 1 1 d . . . H23A H 0.7292 1.1129 0.4078 0.083 Uiso 1 1 calc R . . H23B H 0.7569 1.0551 0.4994 0.083 Uiso 1 1 calc R . . H23C H 0.5964 1.0520 0.4722 0.083 Uiso 1 1 calc R . . C24 C 0.6719(2) 0.6812(2) 0.05000(12) 0.0152(4) Uani 1 1 d . . . C25 C 0.7218(4) 0.5073(3) 0.04103(19) 0.0461(7) Uani 1 1 d . . . H25A H 0.6849 0.4912 -0.0066 0.069 Uiso 1 1 calc R . . H25B H 0.6734 0.4533 0.0898 0.069 Uiso 1 1 calc R . . H25C H 0.8381 0.4689 0.0342 0.069 Uiso 1 1 calc R . . C26 C 0.7532(4) 0.7646(3) -0.02845(17) 0.0443(7) Uani 1 1 d . . . H26A H 0.7178 0.7474 -0.0763 0.066 Uiso 1 1 calc R . . H26B H 0.8693 0.7251 -0.0341 0.066 Uiso 1 1 calc R . . H26C H 0.7230 0.8734 -0.0239 0.066 Uiso 1 1 calc R . . C27 C 0.4882(4) 0.7480(4) 0.0588(2) 0.0493(7) Uani 1 1 d . . . H27A H 0.4525 0.7363 0.0098 0.074 Uiso 1 1 calc R . . H27B H 0.4604 0.8556 0.0658 0.074 Uiso 1 1 calc R . . H27C H 0.4359 0.6940 0.1062 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02899(14) 0.02390(14) 0.02971(15) -0.00036(9) -0.00247(9) -0.00851(9) Si1 0.0377(4) 0.0513(5) 0.0399(4) -0.0123(3) -0.0113(3) -0.0096(3) C1 0.0339(13) 0.0318(13) 0.0304(13) -0.0027(10) -0.0038(10) -0.0103(10) C2 0.0428(14) 0.0317(13) 0.0296(13) -0.0074(10) -0.0037(11) -0.0142(11) C3 0.0520(16) 0.0308(13) 0.0359(14) -0.0043(11) -0.0127(12) -0.0061(12) C4 0.074(2) 0.0253(13) 0.0402(15) -0.0004(11) -0.0157(14) -0.0089(13) C5 0.075(2) 0.0323(14) 0.0453(16) -0.0013(12) -0.0084(15) -0.0301(14) C6 0.0514(16) 0.0364(14) 0.0346(14) -0.0003(11) -0.0059(12) -0.0245(12) C7 0.0375(13) 0.0298(12) 0.0257(12) -0.0024(9) -0.0025(10) -0.0112(10) C8 0.0285(11) 0.0239(11) 0.0305(12) -0.0024(9) -0.0031(9) -0.0086(9) C9 0.0531(19) 0.0504(18) 0.058(2) -0.0078(15) -0.0161(15) 0.0041(15) C10 0.0536(18) 0.063(2) 0.058(2) -0.0025(16) -0.0030(15) -0.0349(16) C11 0.0460(17) 0.0559(19) 0.0498(18) -0.0105(14) -0.0227(14) 0.0107(14) C12 0.0523(18) 0.0371(16) 0.064(2) 0.0121(14) -0.0077(15) 0.0040(14) C13 0.0479(17) 0.0287(14) 0.067(2) -0.0113(13) -0.0152(15) 0.0003(12) C14 0.0345(14) 0.0404(15) 0.0446(16) -0.0087(12) -0.0019(12) 0.0018(12) C15 0.0283(13) 0.0424(15) 0.065(2) -0.0115(14) -0.0116(13) -0.0026(11) C16 0.0424(16) 0.0584(19) 0.0487(17) -0.0162(14) 0.0156(13) -0.0275(14) C17 0.0561(18) 0.0534(18) 0.0392(16) 0.0079(13) 0.0004(13) -0.0287(15) C18 0.0552(17) 0.0352(14) 0.0490(17) 0.0026(12) 0.0009(13) -0.0258(13) C19 0.0432(15) 0.0475(16) 0.0444(16) -0.0025(13) -0.0016(12) -0.0273(13) C20 0.0295(13) 0.0455(16) 0.0577(18) -0.0049(13) 0.0030(12) -0.0162(12) C21 0.092(3) 0.055(2) 0.050(2) -0.0051(16) -0.0283(19) 0.0037(19) C22 0.046(2) 0.149(5) 0.113(4) -0.075(4) -0.004(2) -0.032(2) C23 0.071(2) 0.0509(18) 0.0528(19) -0.0064(15) -0.0173(16) -0.0242(16) C24 0.0200(10) 0.0114(9) 0.0167(9) -0.0001(7) -0.0066(8) -0.0063(7) C25 0.0591(18) 0.0359(15) 0.0476(17) -0.0084(12) -0.0128(14) -0.0148(13) C26 0.0530(17) 0.0448(16) 0.0380(15) -0.0042(12) -0.0096(13) -0.0167(13) C27 0.0479(17) 0.0488(17) 0.0534(18) -0.0011(14) -0.0183(14) -0.0124(14) _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 C8 2.306(2) . ? Zr1 C1 2.318(3) . ? Zr1 C17 2.522(3) . ? Zr1 C13 2.530(3) . ? Zr1 C11 2.534(3) . ? Zr1 C12 2.537(3) . ? Zr1 C18 2.541(3) . ? Zr1 C20 2.546(3) . ? Zr1 C19 2.547(3) . ? Zr1 C16 2.552(3) . ? Zr1 C15 2.553(3) . ? Zr1 C14 2.565(3) . ? Si1 C1 1.829(3) . ? Si1 C22 1.845(4) . ? Si1 C21 1.849(4) . ? Si1 C23 1.852(3) . ? C1 C2 1.292(4) . ? C2 C3 1.325(4) . ? C3 C9 1.501(4) . ? C3 C4 1.511(4) . ? C4 C5 1.511(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.513(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.325(4) . ? C6 C10 1.505(4) . ? C7 C8 1.289(3) . ? C8 C24 1.581(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.387(5) . ? C11 C15 1.408(5) . ? C11 H11 0.9400 . ? C12 C13 1.406(5) . ? C12 H12 0.9400 . ? C13 C14 1.391(4) . ? C13 H13 0.9400 . ? C14 C15 1.390(4) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.401(5) . ? C16 C20 1.406(5) . ? C16 H16 0.9400 . ? C17 C18 1.399(4) . ? C17 H17 0.9400 . ? C18 C19 1.398(4) . ? C18 H18 0.9400 . ? C19 C20 1.401(4) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C27 1.539(4) . ? C24 C25 1.556(3) . ? C24 C26 1.557(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Zr1 C1 111.39(8) . . ? C8 Zr1 C17 135.30(10) . . ? C1 Zr1 C17 93.12(10) . . ? C8 Zr1 C13 91.49(10) . . ? C1 Zr1 C13 133.71(10) . . ? C17 Zr1 C13 97.73(11) . . ? C8 Zr1 C11 127.21(10) . . ? C1 Zr1 C11 81.93(10) . . ? C17 Zr1 C11 91.72(12) . . ? C13 Zr1 C11 53.01(11) . . ? C8 Zr1 C12 123.52(10) . . ? C1 Zr1 C12 110.42(11) . . ? C17 Zr1 C12 76.79(11) . . ? C13 Zr1 C12 32.22(11) . . ? C11 Zr1 C12 31.74(12) . . ? C8 Zr1 C18 109.35(9) . . ? C1 Zr1 C18 124.45(9) . . ? C17 Zr1 C18 32.07(10) . . ? C13 Zr1 C18 79.86(10) . . ? C11 Zr1 C18 101.66(11) . . ? C12 Zr1 C18 74.17(11) . . ? C8 Zr1 C20 87.59(9) . . ? C1 Zr1 C20 92.91(9) . . ? C17 Zr1 C20 53.17(11) . . ? C13 Zr1 C20 129.02(10) . . ? C11 Zr1 C20 144.35(11) . . ? C12 Zr1 C20 125.99(11) . . ? C18 Zr1 C20 53.00(10) . . ? C8 Zr1 C19 82.54(9) . . ? C1 Zr1 C19 124.18(9) . . ? C17 Zr1 C19 52.98(10) . . ? C13 Zr1 C19 97.45(10) . . ? C11 Zr1 C19 133.06(11) . . ? C12 Zr1 C19 103.26(11) . . ? C18 Zr1 C19 31.90(10) . . ? C20 Zr1 C19 31.94(10) . . ? C8 Zr1 C16 118.60(10) . . ? C1 Zr1 C16 74.82(9) . . ? C17 Zr1 C16 32.04(11) . . ? C13 Zr1 C16 129.25(11) . . ? C11 Zr1 C16 114.19(11) . . ? C12 Zr1 C16 107.72(11) . . ? C18 Zr1 C16 52.89(10) . . ? C20 Zr1 C16 32.01(10) . . ? C19 Zr1 C16 52.78(10) . . ? C8 Zr1 C15 96.41(9) . . ? C1 Zr1 C15 84.14(9) . . ? C17 Zr1 C15 123.72(11) . . ? C13 Zr1 C15 52.70(10) . . ? C11 Zr1 C15 32.13(11) . . ? C12 Zr1 C15 52.72(11) . . ? C18 Zr1 C15 126.53(10) . . ? C20 Zr1 C15 175.69(10) . . ? C19 Zr1 C15 150.15(10) . . ? C16 Zr1 C15 143.71(11) . . ? C8 Zr1 C14 76.41(9) . . ? C1 Zr1 C14 113.96(9) . . ? C17 Zr1 C14 127.76(10) . . ? C13 Zr1 C14 31.66(10) . . ? C11 Zr1 C14 52.61(10) . . ? C12 Zr1 C14 52.55(10) . . ? C18 Zr1 C14 111.05(10) . . ? C20 Zr1 C14 152.20(10) . . ? C19 Zr1 C14 121.86(10) . . ? C16 Zr1 C14 159.77(11) . . ? C15 Zr1 C14 31.52(10) . . ? C1 Si1 C22 111.79(17) . . ? C1 Si1 C21 108.83(16) . . ? C22 Si1 C21 110.3(2) . . ? C1 Si1 C23 110.41(14) . . ? C22 Si1 C23 106.6(2) . . ? C21 Si1 C23 108.82(16) . . ? C2 C1 Si1 121.7(2) . . ? C2 C1 Zr1 98.35(17) . . ? Si1 C1 Zr1 139.91(13) . . ? C1 C2 C3 174.9(3) . . ? C1 C2 Zr1 54.63(14) . . ? C3 C2 Zr1 120.30(18) . . ? C2 C3 C9 123.1(3) . . ? C2 C3 C4 120.9(3) . . ? C9 C3 C4 116.0(2) . . ? C3 C4 C5 115.6(2) . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? C5 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 116.1(2) . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5B 108.3 . . ? C6 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C10 122.1(3) . . ? C7 C6 C5 122.2(3) . . ? C10 C6 C5 115.7(2) . . ? C8 C7 C6 175.1(3) . . ? C8 C7 Zr1 57.17(14) . . ? C6 C7 Zr1 118.40(18) . . ? C7 C8 C24 121.8(2) . . ? C7 C8 Zr1 94.80(16) . . ? C24 C8 Zr1 143.39(15) . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 107.9(3) . . ? C12 C11 Zr1 74.25(18) . . ? C15 C11 Zr1 74.66(16) . . ? C12 C11 H11 126.0 . . ? C15 C11 H11 126.0 . . ? Zr1 C11 H11 117.1 . . ? C11 C12 C13 108.1(3) . . ? C11 C12 Zr1 74.01(17) . . ? C13 C12 Zr1 73.62(16) . . ? C11 C12 H12 126.0 . . ? C13 C12 H12 126.0 . . ? Zr1 C12 H12 118.3 . . ? C14 C13 C12 107.7(3) . . ? C14 C13 Zr1 75.55(16) . . ? C12 C13 Zr1 74.16(17) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? Zr1 C13 H13 116.3 . . ? C15 C14 C13 108.5(3) . . ? C15 C14 Zr1 73.75(16) . . ? C13 C14 Zr1 72.79(16) . . ? C15 C14 H14 125.8 . . ? C13 C14 H14 125.8 . . ? Zr1 C14 H14 119.5 . . ? C14 C15 C11 107.8(3) . . ? C14 C15 Zr1 74.73(16) . . ? C11 C15 Zr1 73.22(17) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Zr1 C15 H15 117.9 . . ? C17 C16 C20 107.8(3) . . ? C17 C16 Zr1 72.82(16) . . ? C20 C16 Zr1 73.75(15) . . ? C17 C16 H16 126.1 . . ? C20 C16 H16 126.1 . . ? Zr1 C16 H16 119.2 . . ? C18 C17 C16 108.2(3) . . ? C18 C17 Zr1 74.69(16) . . ? C16 C17 Zr1 75.15(16) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? Zr1 C17 H17 116.4 . . ? C19 C18 C17 107.9(3) . . ? C19 C18 Zr1 74.28(15) . . ? C17 C18 Zr1 73.23(16) . . ? C19 C18 H18 126.1 . . ? C17 C18 H18 126.1 . . ? Zr1 C18 H18 118.4 . . ? C18 C19 C20 108.3(3) . . ? C18 C19 Zr1 73.82(16) . . ? C20 C19 Zr1 73.99(16) . . ? C18 C19 H19 125.8 . . ? C20 C19 H19 125.8 . . ? Zr1 C19 H19 118.3 . . ? C19 C20 C16 107.7(3) . . ? C19 C20 Zr1 74.07(16) . . ? C16 C20 Zr1 74.24(16) . . ? C19 C20 H20 126.2 . . ? C16 C20 H20 126.2 . . ? Zr1 C20 H20 117.6 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 C25 111.3(2) . . ? C27 C24 C26 108.7(2) . . ? C25 C24 C26 108.4(2) . . ? C27 C24 C8 109.74(19) . . ? C25 C24 C8 109.10(18) . . ? C26 C24 C8 109.62(18) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? 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 C22 Si1 C1 C2 -111.4(3) . . . . ? C21 Si1 C1 C2 126.5(2) . . . . ? C23 Si1 C1 C2 7.1(3) . . . . ? C22 Si1 C1 Zr1 71.3(3) . . . . ? C21 Si1 C1 Zr1 -50.9(2) . . . . ? C23 Si1 C1 Zr1 -170.2(2) . . . . ? C8 Zr1 C1 C2 33.82(19) . . . . ? C17 Zr1 C1 C2 -107.99(18) . . . . ? C13 Zr1 C1 C2 148.22(18) . . . . ? C11 Zr1 C1 C2 160.72(19) . . . . ? C12 Zr1 C1 C2 174.96(17) . . . . ? C18 Zr1 C1 C2 -100.64(19) . . . . ? C20 Zr1 C1 C2 -54.74(18) . . . . ? C19 Zr1 C1 C2 -61.8(2) . . . . ? C16 Zr1 C1 C2 -81.42(18) . . . . ? C15 Zr1 C1 C2 128.42(18) . . . . ? C14 Zr1 C1 C2 117.96(17) . . . . ? C8 Zr1 C1 Si1 -148.47(19) . . . . ? C17 Zr1 C1 Si1 69.7(2) . . . . ? C13 Zr1 C1 Si1 -34.1(3) . . . . ? C11 Zr1 C1 Si1 -21.6(2) . . . . ? C12 Zr1 C1 Si1 -7.3(2) . . . . ? C18 Zr1 C1 Si1 77.1(2) . . . . ? C20 Zr1 C1 Si1 123.0(2) . . . . ? C19 Zr1 C1 Si1 115.9(2) . . . . ? C16 Zr1 C1 Si1 96.3(2) . . . . ? C15 Zr1 C1 Si1 -53.9(2) . . . . ? C14 Zr1 C1 Si1 -64.3(2) . . . . ? Si1 C1 C2 C3 177(3) . . . . ? Zr1 C1 C2 C3 -4(3) . . . . ? Si1 C1 C2 Zr1 -178.3(3) . . . . ? C8 Zr1 C2 C1 -148.78(18) . . . . ? C17 Zr1 C2 C1 75.25(19) . . . . ? C13 Zr1 C2 C1 -58.5(3) . . . . ? C11 Zr1 C2 C1 -20.0(2) . . . . ? C12 Zr1 C2 C1 -7.0(2) . . . . ? C18 Zr1 C2 C1 98.52(19) . . . . ? C20 Zr1 C2 C1 123.35(19) . . . . ? C19 Zr1 C2 C1 129.64(18) . . . . ? C16 Zr1 C2 C1 90.56(19) . . . . ? C15 Zr1 C2 C1 -52.54(19) . . . . ? C14 Zr1 C2 C1 -76.27(19) . . . . ? C8 Zr1 C2 C3 30.8(2) . . . . ? C1 Zr1 C2 C3 179.5(3) . . . . ? C17 Zr1 C2 C3 -105.2(2) . . . . ? C13 Zr1 C2 C3 121.1(3) . . . . ? C11 Zr1 C2 C3 159.5(2) . . . . ? C12 Zr1 C2 C3 172.6(2) . . . . ? C18 Zr1 C2 C3 -81.9(2) . . . . ? C20 Zr1 C2 C3 -57.1(2) . . . . ? C19 Zr1 C2 C3 -50.8(2) . . . . ? C16 Zr1 C2 C3 -89.9(2) . . . . ? C15 Zr1 C2 C3 127.0(2) . . . . ? C14 Zr1 C2 C3 103.3(2) . . . . ? C1 C2 C3 C9 100(3) . . . . ? Zr1 C2 C3 C9 95.7(3) . . . . ? C1 C2 C3 C4 -80(3) . . . . ? Zr1 C2 C3 C4 -84.2(3) . . . . ? C2 C3 C4 C5 -6.1(4) . . . . ? C9 C3 C4 C5 173.9(3) . . . . ? C3 C4 C5 C6 72.9(3) . . . . ? C4 C5 C6 C7 -1.5(4) . . . . ? C4 C5 C6 C10 176.1(3) . . . . ? C10 C6 C7 C8 69(3) . . . . ? C5 C6 C7 C8 -113(3) . . . . ? C10 C6 C7 Zr1 93.3(3) . . . . ? C5 C6 C7 Zr1 -89.2(3) . . . . ? C1 Zr1 C7 C8 -151.81(17) . . . . ? C17 Zr1 C7 C8 -61.2(3) . . . . ? C13 Zr1 C7 C8 74.33(18) . . . . ? C11 Zr1 C7 C8 128.25(17) . . . . ? C12 Zr1 C7 C8 95.14(19) . . . . ? C18 Zr1 C7 C8 -11.3(2) . . . . ? C20 Zr1 C7 C8 -59.53(18) . . . . ? C19 Zr1 C7 C8 -26.85(18) . . . . ? C16 Zr1 C7 C8 -83.29(19) . . . . ? C15 Zr1 C7 C8 123.60(18) . . . . ? C14 Zr1 C7 C8 92.04(17) . . . . ? C8 Zr1 C7 C6 -177.6(3) . . . . ? C1 Zr1 C7 C6 30.6(2) . . . . ? C17 Zr1 C7 C6 121.1(3) . . . . ? C13 Zr1 C7 C6 -103.3(2) . . . . ? C11 Zr1 C7 C6 -49.4(2) . . . . ? C12 Zr1 C7 C6 -82.5(2) . . . . ? C18 Zr1 C7 C6 171.0(2) . . . . ? C20 Zr1 C7 C6 122.9(2) . . . . ? C19 Zr1 C7 C6 155.5(2) . . . . ? C16 Zr1 C7 C6 99.1(2) . . . . ? C15 Zr1 C7 C6 -54.0(2) . . . . ? C14 Zr1 C7 C6 -85.6(2) . . . . ? C6 C7 C8 C24 -155(3) . . . . ? Zr1 C7 C8 C24 179.3(3) . . . . ? C6 C7 C8 Zr1 25(3) . . . . ? C1 Zr1 C8 C7 30.43(18) . . . . ? C17 Zr1 C8 C7 149.04(17) . . . . ? C13 Zr1 C8 C7 -108.39(17) . . . . ? C11 Zr1 C8 C7 -65.8(2) . . . . ? C12 Zr1 C8 C7 -104.71(18) . . . . ? C18 Zr1 C8 C7 171.83(16) . . . . ? C20 Zr1 C8 C7 122.62(17) . . . . ? C19 Zr1 C8 C7 154.29(18) . . . . ? C16 Zr1 C8 C7 114.30(17) . . . . ? C15 Zr1 C8 C7 -55.77(17) . . . . ? C14 Zr1 C8 C7 -80.30(17) . . . . ? C1 Zr1 C8 C24 -148.6(2) . . . . ? C17 Zr1 C8 C24 -30.0(3) . . . . ? C13 Zr1 C8 C24 72.6(3) . . . . ? C11 Zr1 C8 C24 115.2(3) . . . . ? C12 Zr1 C8 C24 76.3(3) . . . . ? C18 Zr1 C8 C24 -7.2(3) . . . . ? C20 Zr1 C8 C24 -56.4(3) . . . . ? C19 Zr1 C8 C24 -24.7(3) . . . . ? C16 Zr1 C8 C24 -64.7(3) . . . . ? C15 Zr1 C8 C24 125.2(3) . . . . ? C14 Zr1 C8 C24 100.7(3) . . . . ? C8 Zr1 C11 C12 -95.2(2) . . . . ? C1 Zr1 C11 C12 154.0(2) . . . . ? C17 Zr1 C11 C12 61.1(2) . . . . ? C13 Zr1 C11 C12 -37.3(2) . . . . ? C18 Zr1 C11 C12 30.4(2) . . . . ? C20 Zr1 C11 C12 70.3(3) . . . . ? C19 Zr1 C11 C12 23.9(3) . . . . ? C16 Zr1 C11 C12 84.7(2) . . . . ? C15 Zr1 C11 C12 -114.2(3) . . . . ? C14 Zr1 C11 C12 -77.3(2) . . . . ? C8 Zr1 C11 C15 19.0(2) . . . . ? C1 Zr1 C11 C15 -91.83(19) . . . . ? C17 Zr1 C11 C15 175.26(19) . . . . ? C13 Zr1 C11 C15 76.9(2) . . . . ? C12 Zr1 C11 C15 114.2(3) . . . . ? C18 Zr1 C11 C15 144.51(19) . . . . ? C20 Zr1 C11 C15 -175.54(17) . . . . ? C19 Zr1 C11 C15 138.07(19) . . . . ? C16 Zr1 C11 C15 -161.12(17) . . . . ? C14 Zr1 C11 C15 36.82(17) . . . . ? C15 C11 C12 C13 -1.3(3) . . . . ? Zr1 C11 C12 C13 66.3(2) . . . . ? C15 C11 C12 Zr1 -67.7(2) . . . . ? C8 Zr1 C12 C11 107.9(2) . . . . ? C1 Zr1 C12 C11 -27.6(2) . . . . ? C17 Zr1 C12 C11 -116.0(2) . . . . ? C13 Zr1 C12 C11 114.8(3) . . . . ? C18 Zr1 C12 C11 -149.0(2) . . . . ? C20 Zr1 C12 C11 -137.3(2) . . . . ? C19 Zr1 C12 C11 -162.3(2) . . . . ? C16 Zr1 C12 C11 -107.5(2) . . . . ? C15 Zr1 C12 C11 37.58(19) . . . . ? C14 Zr1 C12 C11 77.5(2) . . . . ? C8 Zr1 C12 C13 -6.9(2) . . . . ? C1 Zr1 C12 C13 -142.42(19) . . . . ? C17 Zr1 C12 C13 129.2(2) . . . . ? C11 Zr1 C12 C13 -114.8(3) . . . . ? C18 Zr1 C12 C13 96.1(2) . . . . ? C20 Zr1 C12 C13 107.9(2) . . . . ? C19 Zr1 C12 C13 82.9(2) . . . . ? C16 Zr1 C12 C13 137.6(2) . . . . ? C15 Zr1 C12 C13 -77.3(2) . . . . ? C14 Zr1 C12 C13 -37.30(19) . . . . ? C11 C12 C13 C14 2.1(3) . . . . ? Zr1 C12 C13 C14 68.7(2) . . . . ? C11 C12 C13 Zr1 -66.6(2) . . . . ? C8 Zr1 C13 C14 60.66(19) . . . . ? C1 Zr1 C13 C14 -61.3(2) . . . . ? C17 Zr1 C13 C14 -163.19(19) . . . . ? C11 Zr1 C13 C14 -76.9(2) . . . . ? C12 Zr1 C13 C14 -113.6(3) . . . . ? C18 Zr1 C13 C14 170.1(2) . . . . ? C20 Zr1 C13 C14 148.77(18) . . . . ? C19 Zr1 C13 C14 143.33(19) . . . . ? C16 Zr1 C13 C14 -169.58(17) . . . . ? C15 Zr1 C13 C14 -36.26(18) . . . . ? C8 Zr1 C13 C12 174.2(2) . . . . ? C1 Zr1 C13 C12 52.3(3) . . . . ? C17 Zr1 C13 C12 -49.6(2) . . . . ? C11 Zr1 C13 C12 36.7(2) . . . . ? C18 Zr1 C13 C12 -76.4(2) . . . . ? C20 Zr1 C13 C12 -97.6(2) . . . . ? C19 Zr1 C13 C12 -103.1(2) . . . . ? C16 Zr1 C13 C12 -56.0(2) . . . . ? C15 Zr1 C13 C12 77.3(2) . . . . ? C14 Zr1 C13 C12 113.6(3) . . . . ? C12 C13 C14 C15 -2.1(3) . . . . ? Zr1 C13 C14 C15 65.65(19) . . . . ? C12 C13 C14 Zr1 -67.8(2) . . . . ? C8 Zr1 C14 C15 127.87(19) . . . . ? C1 Zr1 C14 C15 20.2(2) . . . . ? C17 Zr1 C14 C15 -94.6(2) . . . . ? C13 Zr1 C14 C15 -115.8(3) . . . . ? C11 Zr1 C14 C15 -37.57(19) . . . . ? C12 Zr1 C14 C15 -77.9(2) . . . . ? C18 Zr1 C14 C15 -126.33(19) . . . . ? C20 Zr1 C14 C15 -175.6(2) . . . . ? C19 Zr1 C14 C15 -160.04(18) . . . . ? C16 Zr1 C14 C15 -91.9(3) . . . . ? C8 Zr1 C14 C13 -116.3(2) . . . . ? C1 Zr1 C14 C13 136.06(18) . . . . ? C17 Zr1 C14 C13 21.3(2) . . . . ? C11 Zr1 C14 C13 78.3(2) . . . . ? C12 Zr1 C14 C13 37.98(19) . . . . ? C18 Zr1 C14 C13 -10.5(2) . . . . ? C20 Zr1 C14 C13 -59.7(3) . . . . ? C19 Zr1 C14 C13 -44.2(2) . . . . ? C16 Zr1 C14 C13 23.9(4) . . . . ? C15 Zr1 C14 C13 115.8(3) . . . . ? C13 C14 C15 C11 1.3(3) . . . . ? Zr1 C14 C15 C11 66.31(19) . . . . ? C13 C14 C15 Zr1 -65.0(2) . . . . ? C12 C11 C15 C14 0.0(3) . . . . ? Zr1 C11 C15 C14 -67.33(19) . . . . ? C12 C11 C15 Zr1 67.4(2) . . . . ? C8 Zr1 C15 C14 -50.55(19) . . . . ? C1 Zr1 C15 C14 -161.49(19) . . . . ? C17 Zr1 C15 C14 108.7(2) . . . . ? C13 Zr1 C15 C14 36.44(18) . . . . ? C11 Zr1 C15 C14 114.4(3) . . . . ? C12 Zr1 C15 C14 77.3(2) . . . . ? C18 Zr1 C15 C14 69.3(2) . . . . ? C20 Zr1 C15 C14 151.4(12) . . . . ? C19 Zr1 C15 C14 35.6(3) . . . . ? C16 Zr1 C15 C14 144.27(19) . . . . ? C8 Zr1 C15 C11 -164.91(19) . . . . ? C1 Zr1 C15 C11 84.15(19) . . . . ? C17 Zr1 C15 C11 -5.7(2) . . . . ? C13 Zr1 C15 C11 -77.9(2) . . . . ? C12 Zr1 C15 C11 -37.11(19) . . . . ? C18 Zr1 C15 C11 -45.0(2) . . . . ? C20 Zr1 C15 C11 37.0(13) . . . . ? C19 Zr1 C15 C11 -78.7(3) . . . . ? C16 Zr1 C15 C11 29.9(3) . . . . ? C14 Zr1 C15 C11 -114.4(3) . . . . ? C8 Zr1 C16 C17 130.92(19) . . . . ? C1 Zr1 C16 C17 -122.7(2) . . . . ? C13 Zr1 C16 C17 12.0(2) . . . . ? C11 Zr1 C16 C17 -49.0(2) . . . . ? C12 Zr1 C16 C17 -15.6(2) . . . . ? C18 Zr1 C16 C17 37.43(19) . . . . ? C20 Zr1 C16 C17 115.1(3) . . . . ? C19 Zr1 C16 C17 77.8(2) . . . . ? C15 Zr1 C16 C17 -65.9(3) . . . . ? C14 Zr1 C16 C17 -3.9(4) . . . . ? C8 Zr1 C16 C20 15.8(2) . . . . ? C1 Zr1 C16 C20 122.23(19) . . . . ? C17 Zr1 C16 C20 -115.1(3) . . . . ? C13 Zr1 C16 C20 -103.1(2) . . . . ? C11 Zr1 C16 C20 -164.11(18) . . . . ? C12 Zr1 C16 C20 -130.75(19) . . . . ? C18 Zr1 C16 C20 -77.67(19) . . . . ? C19 Zr1 C16 C20 -37.33(17) . . . . ? C15 Zr1 C16 C20 178.99(17) . . . . ? C14 Zr1 C16 C20 -119.0(3) . . . . ? C20 C16 C17 C18 -2.0(3) . . . . ? Zr1 C16 C17 C18 -68.0(2) . . . . ? C20 C16 C17 Zr1 65.96(19) . . . . ? C8 Zr1 C17 C18 43.5(2) . . . . ? C1 Zr1 C17 C18 168.55(19) . . . . ? C13 Zr1 C17 C18 -56.6(2) . . . . ? C11 Zr1 C17 C18 -109.4(2) . . . . ? C12 Zr1 C17 C18 -81.2(2) . . . . ? C20 Zr1 C17 C18 77.2(2) . . . . ? C19 Zr1 C17 C18 36.97(18) . . . . ? C16 Zr1 C17 C18 114.1(3) . . . . ? C15 Zr1 C17 C18 -106.4(2) . . . . ? C14 Zr1 C17 C18 -67.6(2) . . . . ? C8 Zr1 C17 C16 -70.6(2) . . . . ? C1 Zr1 C17 C16 54.5(2) . . . . ? C13 Zr1 C17 C16 -170.65(19) . . . . ? C11 Zr1 C17 C16 136.5(2) . . . . ? C12 Zr1 C17 C16 164.7(2) . . . . ? C18 Zr1 C17 C16 -114.1(3) . . . . ? C20 Zr1 C17 C16 -36.85(18) . . . . ? C19 Zr1 C17 C16 -77.1(2) . . . . ? C15 Zr1 C17 C16 139.49(18) . . . . ? C14 Zr1 C17 C16 178.28(18) . . . . ? C16 C17 C18 C19 1.5(3) . . . . ? Zr1 C17 C18 C19 -66.8(2) . . . . ? C16 C17 C18 Zr1 68.3(2) . . . . ? C8 Zr1 C18 C19 -34.4(2) . . . . ? C1 Zr1 C18 C19 100.78(19) . . . . ? C17 Zr1 C18 C19 114.7(3) . . . . ? C13 Zr1 C18 C19 -122.44(19) . . . . ? C11 Zr1 C18 C19 -171.07(18) . . . . ? C12 Zr1 C18 C19 -155.0(2) . . . . ? C20 Zr1 C18 C19 36.87(18) . . . . ? C16 Zr1 C18 C19 77.3(2) . . . . ? C15 Zr1 C18 C19 -148.48(18) . . . . ? C14 Zr1 C18 C19 -116.87(18) . . . . ? C8 Zr1 C18 C17 -149.13(18) . . . . ? C1 Zr1 C18 C17 -13.9(2) . . . . ? C13 Zr1 C18 C17 122.9(2) . . . . ? C11 Zr1 C18 C17 74.2(2) . . . . ? C12 Zr1 C18 C17 90.3(2) . . . . ? C20 Zr1 C18 C17 -77.8(2) . . . . ? C19 Zr1 C18 C17 -114.7(3) . . . . ? C16 Zr1 C18 C17 -37.39(19) . . . . ? C15 Zr1 C18 C17 96.8(2) . . . . ? C14 Zr1 C18 C17 128.44(19) . . . . ? C17 C18 C19 C20 -0.4(3) . . . . ? Zr1 C18 C19 C20 -66.51(19) . . . . ? C17 C18 C19 Zr1 66.1(2) . . . . ? C8 Zr1 C19 C18 147.45(19) . . . . ? C1 Zr1 C19 C18 -101.72(19) . . . . ? C17 Zr1 C19 C18 -37.18(18) . . . . ? C13 Zr1 C19 C18 56.91(19) . . . . ? C11 Zr1 C19 C18 12.0(2) . . . . ? C12 Zr1 C19 C18 24.7(2) . . . . ? C20 Zr1 C19 C18 -115.1(3) . . . . ? C16 Zr1 C19 C18 -77.7(2) . . . . ? C15 Zr1 C19 C18 57.6(3) . . . . ? C14 Zr1 C19 C18 78.6(2) . . . . ? C8 Zr1 C19 C20 -97.47(18) . . . . ? C1 Zr1 C19 C20 13.4(2) . . . . ? C17 Zr1 C19 C20 77.9(2) . . . . ? C13 Zr1 C19 C20 172.00(19) . . . . ? C11 Zr1 C19 C20 127.10(19) . . . . ? C12 Zr1 C19 C20 139.75(19) . . . . ? C18 Zr1 C19 C20 115.1(3) . . . . ? C16 Zr1 C19 C20 37.41(18) . . . . ? C15 Zr1 C19 C20 172.7(2) . . . . ? C14 Zr1 C19 C20 -166.34(17) . . . . ? C18 C19 C20 C16 -0.8(3) . . . . ? Zr1 C19 C20 C16 -67.20(19) . . . . ? C18 C19 C20 Zr1 66.4(2) . . . . ? C17 C16 C20 C19 1.7(3) . . . . ? Zr1 C16 C20 C19 67.08(19) . . . . ? C17 C16 C20 Zr1 -65.3(2) . . . . ? C8 Zr1 C20 C19 79.73(18) . . . . ? C1 Zr1 C20 C19 -168.96(18) . . . . ? C17 Zr1 C20 C19 -77.25(19) . . . . ? C13 Zr1 C20 C19 -10.2(2) . . . . ? C11 Zr1 C20 C19 -88.8(2) . . . . ? C12 Zr1 C20 C19 -51.0(2) . . . . ? C18 Zr1 C20 C19 -36.82(17) . . . . ? C16 Zr1 C20 C19 -114.1(3) . . . . ? C15 Zr1 C20 C19 -122.1(12) . . . . ? C14 Zr1 C20 C19 25.5(3) . . . . ? C8 Zr1 C20 C16 -166.14(19) . . . . ? C1 Zr1 C20 C16 -54.83(19) . . . . ? C17 Zr1 C20 C16 36.88(18) . . . . ? C13 Zr1 C20 C16 103.9(2) . . . . ? C11 Zr1 C20 C16 25.4(3) . . . . ? C12 Zr1 C20 C16 63.1(2) . . . . ? C18 Zr1 C20 C16 77.3(2) . . . . ? C19 Zr1 C20 C16 114.1(3) . . . . ? C15 Zr1 C20 C16 -8.0(13) . . . . ? C14 Zr1 C20 C16 139.6(2) . . . . ? C7 C8 C24 C27 -103.1(3) . . . . ? Zr1 C8 C24 C27 75.8(3) . . . . ? C7 C8 C24 C25 134.8(3) . . . . ? Zr1 C8 C24 C25 -46.4(3) . . . . ? C7 C8 C24 C26 16.2(3) . . . . ? Zr1 C8 C24 C26 -165.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.508 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.055