Supplementary material (ESI) for Dalton Trans. This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Tomas Cuenca' _publ_contact_author_email TOMAS.CUENCA@UAH.ES _publ_section_title ; Olefin Isomerisation versus Hydrozirconation: A case of stable b-Hydrogen containing Zr-Alkyl Derivative ; loop_ _publ_author_name 'Tomas Cuenca' 'Obis Castano' 'Luis M Frutos' 'Marta E G Mosquera' 'Cristina E Petrisor' ; E.Royo ; # Attachment 'cif.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 676069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H32 Cl N Si2 Zr' _chemical_formula_weight 457.31 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' Cl Cl 0.1484 0.1585 '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 7.3620(13) _cell_length_b 9.2080(10) _cell_length_c 17.5130(14) _cell_angle_alpha 86.139(10) _cell_angle_beta 85.044(9) _cell_angle_gamma 76.824(12) _cell_volume 1150.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_max 21.651 _cell_measurement_theta_min 5.23 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 0.724 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22003 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5209 _reflns_number_gt 3051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5209 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.2559 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.75469(8) 0.46730(7) 0.25836(4) 0.0283(3) Uani 1 1 d . . . N1 N 0.8789(7) 0.2748(6) 0.3265(3) 0.0322(13) Uani 1 1 d . . . Si1 Si 0.7565(3) 0.2978(2) 0.41743(12) 0.0380(5) Uani 1 1 d . . . Si2 Si 0.5710(3) 0.7415(2) 0.07821(12) 0.0407(5) Uani 1 1 d . . . Cl1 Cl 1.0205(2) 0.5936(2) 0.23448(13) 0.0471(5) Uani 1 1 d . . . C1 C 0.6101(10) 0.4855(8) 0.3916(4) 0.0421(18) Uani 1 1 d . . . C2 C 0.4585(9) 0.5161(9) 0.3407(4) 0.0373(16) Uani 1 1 d . . . H2 H 0.3767 0.4521 0.3347 0.045 Uiso 1 1 calc R . . C3 C 0.4525(10) 0.6550(8) 0.3019(4) 0.0388(17) Uani 1 1 d . . . H3 H 0.3659 0.7017 0.2656 0.047 Uiso 1 1 calc R . . C4 C 0.5980(10) 0.7132(8) 0.3263(5) 0.0422(18) Uani 1 1 d . . . H4 H 0.6256 0.8067 0.3096 0.051 Uiso 1 1 calc R . . C5 C 0.6939(10) 0.6109(9) 0.3787(5) 0.0442(19) Uani 1 1 d . . . H5 H 0.8002 0.6227 0.4027 0.053 Uiso 1 1 calc R . . C6 C 0.5215(10) 0.4553(8) 0.1614(4) 0.0358(16) Uani 1 1 d . . . H6 H 0.3924 0.4885 0.1764 0.043 Uiso 1 1 calc R . . C7 C 0.6301(11) 0.3073(8) 0.1723(4) 0.0400(17) Uani 1 1 d . . . H7 H 0.5866 0.2250 0.1967 0.048 Uiso 1 1 calc R . . C8 C 0.8116(11) 0.3043(9) 0.1408(5) 0.049(2) Uani 1 1 d . . . H8 H 0.9121 0.2187 0.1396 0.059 Uiso 1 1 calc R . . C9 C 0.8218(10) 0.4478(8) 0.1113(4) 0.0405(17) Uani 1 1 d . . . H9 H 0.9306 0.4752 0.0871 0.049 Uiso 1 1 calc R . . C10 C 0.6418(9) 0.5466(8) 0.1234(4) 0.0348(15) Uani 1 1 d . . . C11 C 0.8953(13) 0.3218(10) 0.4983(5) 0.057(2) Uani 1 1 d . . . H11A H 0.9737 0.2250 0.5138 0.085 Uiso 1 1 calc R . . H11B H 0.8100 0.3613 0.5420 0.085 Uiso 1 1 calc R . . H11C H 0.9749 0.3917 0.4817 0.085 Uiso 1 1 calc R . . C12 C 0.6082(12) 0.1587(11) 0.4454(6) 0.059(2) Uani 1 1 d . . . H12A H 0.5382 0.1473 0.4019 0.088 Uiso 1 1 calc R . . H12B H 0.5205 0.1942 0.4890 0.088 Uiso 1 1 calc R . . H12C H 0.6887 0.0622 0.4598 0.088 Uiso 1 1 calc R . . C13 C 1.0294(10) 0.1357(8) 0.3094(5) 0.0416(18) Uani 1 1 d . . . C14 C 1.1219(12) 0.0664(9) 0.3853(5) 0.054(2) Uani 1 1 d . . . H14A H 1.1761 0.1404 0.4075 0.082 Uiso 1 1 calc R . . H14B H 1.2205 -0.0220 0.3735 0.082 Uiso 1 1 calc R . . H14C H 1.0266 0.0378 0.4221 0.082 Uiso 1 1 calc R . . C15 C 0.9474(12) 0.0172(9) 0.2778(6) 0.054(2) Uani 1 1 d . . . H15A H 0.8888 0.0565 0.2303 0.081 Uiso 1 1 calc R . . H15B H 0.8532 -0.0103 0.3156 0.081 Uiso 1 1 calc R . . H15C H 1.0471 -0.0712 0.2672 0.081 Uiso 1 1 calc R . . C16 C 1.1860(10) 0.1779(9) 0.2551(6) 0.052(2) Uani 1 1 d . . . H16A H 1.2348 0.2543 0.2778 0.078 Uiso 1 1 calc R . . H16B H 1.1364 0.2171 0.2058 0.078 Uiso 1 1 calc R . . H16C H 1.2870 0.0892 0.2469 0.078 Uiso 1 1 calc R . . C21 C 0.6293(15) 0.8892(10) 0.1342(6) 0.065(3) Uani 1 1 d . . . H21A H 0.7641 0.8661 0.1404 0.097 Uiso 1 1 calc R . . H21B H 0.5609 0.8924 0.1848 0.097 Uiso 1 1 calc R . . H21C H 0.5935 0.9865 0.1067 0.097 Uiso 1 1 calc R . . C22 C 0.3120(13) 0.7816(12) 0.0666(6) 0.071(3) Uani 1 1 d . . . H22A H 0.2713 0.8825 0.0435 0.106 Uiso 1 1 calc R . . H22B H 0.2447 0.7742 0.1170 0.106 Uiso 1 1 calc R . . H22C H 0.2852 0.7088 0.0334 0.106 Uiso 1 1 calc R . . C23 C 0.7035(14) 0.7379(11) -0.0165(5) 0.065(3) Uani 1 1 d . . . H23A H 0.8377 0.7179 -0.0093 0.097 Uiso 1 1 calc R . . H23B H 0.6655 0.8347 -0.0442 0.097 Uiso 1 1 calc R . . H23C H 0.6777 0.6592 -0.0461 0.097 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 0.0198(3) 0.0241(4) 0.0421(4) -0.0072(3) -0.0039(2) -0.0050(2) N1 0.025(3) 0.020(3) 0.053(4) -0.001(2) -0.008(2) -0.005(2) Si1 0.0335(10) 0.0355(11) 0.0468(12) -0.0040(9) -0.0052(9) -0.0103(8) Si2 0.0395(11) 0.0351(11) 0.0438(12) -0.0030(9) -0.0057(9) 0.0008(8) Cl1 0.0268(9) 0.0370(10) 0.0802(14) -0.0012(9) -0.0036(8) -0.0130(7) C1 0.038(4) 0.040(4) 0.047(4) -0.015(3) -0.002(3) -0.003(3) C2 0.026(3) 0.048(4) 0.036(4) -0.009(3) 0.002(3) -0.005(3) C3 0.029(3) 0.042(4) 0.040(4) -0.012(3) 0.003(3) 0.005(3) C4 0.035(4) 0.033(4) 0.058(5) -0.024(3) -0.001(3) -0.001(3) C5 0.033(4) 0.042(4) 0.058(5) -0.025(4) -0.012(3) -0.001(3) C6 0.031(4) 0.039(4) 0.041(4) -0.011(3) -0.004(3) -0.012(3) C7 0.051(4) 0.036(4) 0.037(4) -0.008(3) -0.006(3) -0.015(3) C8 0.040(4) 0.035(4) 0.071(6) -0.024(4) -0.009(4) 0.003(3) C9 0.037(4) 0.041(4) 0.040(4) -0.011(3) -0.002(3) 0.001(3) C10 0.031(3) 0.028(3) 0.043(4) -0.012(3) -0.005(3) 0.001(3) C11 0.053(5) 0.047(5) 0.068(6) -0.009(4) -0.016(4) -0.001(4) C12 0.048(5) 0.063(6) 0.067(6) 0.002(5) 0.005(4) -0.022(4) C13 0.031(4) 0.022(3) 0.071(5) -0.010(3) -0.009(3) 0.000(3) C14 0.049(5) 0.039(4) 0.070(6) 0.006(4) -0.022(4) 0.005(4) C15 0.057(5) 0.028(4) 0.077(6) -0.012(4) -0.005(4) -0.008(4) C16 0.026(4) 0.046(5) 0.082(6) -0.017(4) 0.007(4) 0.000(3) C21 0.089(7) 0.039(5) 0.066(6) -0.002(4) -0.018(5) -0.009(5) C22 0.058(6) 0.070(7) 0.075(7) 0.022(5) -0.019(5) 0.000(5) C23 0.071(6) 0.052(5) 0.063(6) 0.003(4) 0.010(5) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.137(5) . ? Zr1 C1 2.480(8) . ? Zr1 C2 2.476(7) . ? Zr1 Cl1 2.4877(18) . ? Zr1 C5 2.517(7) . ? Zr1 C7 2.537(7) . ? Zr1 C6 2.541(7) . ? Zr1 C10 2.577(7) . ? Zr1 C3 2.579(6) . ? Zr1 C8 2.578(8) . ? Zr1 C9 2.591(7) . ? Zr1 C4 2.609(7) . ? N1 C13 1.518(8) . ? N1 Si1 1.761(6) . ? Si1 C1 1.866(8) . ? Si1 C12 1.879(9) . ? Si1 C11 1.870(9) . ? Si2 C21 1.875(9) . ? Si2 C23 1.848(9) . ? Si2 C22 1.884(10) . ? Si2 C10 1.890(7) . ? C1 C5 1.425(11) . ? C1 C2 1.454(10) . ? C2 C3 1.401(10) . ? C2 H2 0.9500 . ? C3 C4 1.411(11) . ? C3 H3 0.9500 . ? C4 C5 1.387(11) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.424(10) . ? C6 C10 1.447(10) . ? C6 H6 0.9500 . ? C7 C8 1.395(11) . ? C7 H7 0.9500 . ? C8 C9 1.402(11) . ? C8 H8 0.9500 . ? C9 C10 1.435(9) . ? C9 H9 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.533(11) . ? C13 C15 1.517(10) . ? C13 C14 1.576(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 N1 Zr1 C1 70.3(2) . . ? N1 Zr1 C2 93.7(2) . . ? C1 Zr1 C2 34.1(2) . . ? N1 Zr1 Cl1 100.91(15) . . ? C1 Zr1 Cl1 113.51(19) . . ? C2 Zr1 Cl1 134.31(19) . . ? N1 Zr1 C5 87.9(2) . . ? C1 Zr1 C5 33.1(3) . . ? C2 Zr1 C5 54.2(2) . . ? Cl1 Zr1 C5 83.10(19) . . ? N1 Zr1 C7 91.2(2) . . ? C1 Zr1 C7 116.0(2) . . ? C2 Zr1 C7 92.0(3) . . ? Cl1 Zr1 C7 130.23(18) . . ? C5 Zr1 C7 146.0(2) . . ? N1 Zr1 C6 121.6(2) . . ? C1 Zr1 C6 112.6(2) . . ? C2 Zr1 C6 79.3(2) . . ? Cl1 Zr1 C6 125.12(17) . . ? C5 Zr1 C6 127.3(2) . . ? C7 Zr1 C6 32.6(2) . . ? N1 Zr1 C10 141.7(2) . . ? C1 Zr1 C10 135.8(2) . . ? C2 Zr1 C10 102.4(2) . . ? Cl1 Zr1 C10 92.31(17) . . ? C5 Zr1 C10 129.6(2) . . ? C7 Zr1 C10 54.1(2) . . ? C6 Zr1 C10 32.8(2) . . ? N1 Zr1 C3 123.6(2) . . ? C1 Zr1 C3 54.7(2) . . ? C2 Zr1 C3 32.1(2) . . ? Cl1 Zr1 C3 110.64(18) . . ? C5 Zr1 C3 52.9(2) . . ? C7 Zr1 C3 101.4(2) . . ? C6 Zr1 C3 74.7(2) . . ? C10 Zr1 C3 83.3(2) . . ? N1 Zr1 C8 88.9(2) . . ? C1 Zr1 C8 143.0(3) . . ? C2 Zr1 C8 123.6(3) . . ? Cl1 Zr1 C8 99.9(2) . . ? C5 Zr1 C8 176.0(3) . . ? C7 Zr1 C8 31.6(2) . . ? C6 Zr1 C8 52.9(2) . . ? C10 Zr1 C8 53.3(2) . . ? C3 Zr1 C8 127.7(2) . . ? N1 Zr1 C9 115.7(2) . . ? C1 Zr1 C9 165.7(3) . . ? C2 Zr1 C9 131.9(2) . . ? Cl1 Zr1 C9 78.94(19) . . ? C5 Zr1 C9 152.5(3) . . ? C7 Zr1 C9 52.8(2) . . ? C6 Zr1 C9 53.1(2) . . ? C10 Zr1 C9 32.2(2) . . ? C3 Zr1 C9 115.4(2) . . ? C8 Zr1 C9 31.5(3) . . ? N1 Zr1 C4 118.9(2) . . ? C1 Zr1 C4 53.9(3) . . ? C2 Zr1 C4 53.0(3) . . ? Cl1 Zr1 C4 82.43(18) . . ? C5 Zr1 C4 31.3(3) . . ? C7 Zr1 C4 132.2(2) . . ? C6 Zr1 C4 102.4(2) . . ? C10 Zr1 C4 98.3(2) . . ? C3 Zr1 C4 31.5(2) . . ? C8 Zr1 C4 151.4(3) . . ? C9 Zr1 C4 124.6(3) . . ? C13 N1 Si1 121.5(5) . . ? C13 N1 Zr1 133.5(5) . . ? Si1 N1 Zr1 104.9(3) . . ? N1 Si1 C1 94.8(3) . . ? N1 Si1 C12 114.7(4) . . ? C1 Si1 C12 111.4(4) . . ? N1 Si1 C11 116.3(4) . . ? C1 Si1 C11 107.1(4) . . ? C12 Si1 C11 111.1(5) . . ? N1 Si1 Zr1 41.78(17) . . ? C1 Si1 Zr1 53.1(2) . . ? C12 Si1 Zr1 123.1(3) . . ? C11 Si1 Zr1 125.8(3) . . ? C21 Si2 C23 108.3(5) . . ? C21 Si2 C22 110.4(5) . . ? C23 Si2 C22 110.6(5) . . ? C21 Si2 C10 113.7(4) . . ? C23 Si2 C10 105.9(4) . . ? C22 Si2 C10 107.8(4) . . ? C5 C1 C2 104.4(7) . . ? C5 C1 Si1 120.0(6) . . ? C2 C1 Si1 126.1(6) . . ? C5 C1 Zr1 74.9(5) . . ? C2 C1 Zr1 72.8(4) . . ? Si1 C1 Zr1 89.9(3) . . ? C3 C2 C1 109.1(7) . . ? C3 C2 Zr1 78.0(4) . . ? C1 C2 Zr1 73.1(4) . . ? C3 C2 H2 125.4 . . ? C1 C2 H2 125.4 . . ? Zr1 C2 H2 115.5 . . ? C2 C3 C4 107.7(7) . . ? C2 C3 Zr1 69.9(4) . . ? C4 C3 Zr1 75.4(4) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Zr1 C3 H3 120.3 . . ? C5 C4 C3 108.4(7) . . ? C5 C4 Zr1 70.7(4) . . ? C3 C4 Zr1 73.0(4) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Zr1 C4 H4 122.2 . . ? C4 C5 C1 110.3(7) . . ? C4 C5 Zr1 78.0(4) . . ? C1 C5 Zr1 72.0(4) . . ? C4 C5 H5 124.9 . . ? C1 C5 H5 124.9 . . ? Zr1 C5 H5 116.9 . . ? C7 C6 C10 108.3(6) . . ? C7 C6 Zr1 73.6(4) . . ? C10 C6 Zr1 74.9(4) . . ? C7 C6 H6 125.9 . . ? C10 C6 H6 125.9 . . ? Zr1 C6 H6 117.6 . . ? C8 C7 C6 108.0(7) . . ? C8 C7 Zr1 75.8(4) . . ? C6 C7 Zr1 73.9(4) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Zr1 C7 H7 116.5 . . ? C9 C8 C7 109.1(7) . . ? C9 C8 Zr1 74.8(4) . . ? C7 C8 Zr1 72.6(4) . . ? C9 C8 H8 125.5 . . ? C7 C8 H8 125.5 . . ? Zr1 C8 H8 119.0 . . ? C8 C9 C10 109.1(7) . . ? C8 C9 Zr1 73.8(5) . . ? C10 C9 Zr1 73.3(4) . . ? C8 C9 H9 125.5 . . ? C10 C9 H9 125.5 . . ? Zr1 C9 H9 119.2 . . ? C6 C10 C9 105.5(6) . . ? C6 C10 Si2 127.9(5) . . ? C9 C10 Si2 125.2(6) . . ? C6 C10 Zr1 72.2(4) . . ? C9 C10 Zr1 74.4(4) . . ? Si2 C10 Zr1 128.4(3) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 N1 109.6(6) . . ? C16 C13 C15 112.3(7) . . ? N1 C13 C15 111.1(6) . . ? C16 C13 C14 106.4(6) . . ? N1 C13 C14 110.1(6) . . ? C15 C13 C14 107.2(6) . . ? 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 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.288 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.202