# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Leshinksi, Sarah' 'Shalumova, Tamila' 'Tanski, Joseph' 'Waterman, Rory' _publ_contact_author_name 'Waterman, Rory' _publ_contact_author_email rory.waterman@uvm.edu _publ_section_title ; Insertion Reactions Involving a Triamidoamine-Supported Zirconium Complex ; # Attachment '- cmpd-3.cif' data_rw1031zr _database_code_depnum_ccdc_archive 'CCDC 780977' #TrackingRef '- cmpd-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H45 N7 Si3 Zr' _chemical_formula_sum 'C22 H45 N7 Si3 Zr' _chemical_formula_weight 583.14 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.729(3) _cell_length_b 15.794(4) _cell_length_c 17.897(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.125(4) _cell_angle_gamma 90.00 _cell_volume 3030.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9491 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 29.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8844 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36906 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7212 _reflns_number_gt 6024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. EXTI refined to zero and was removed from the refinement. ; _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^)+(0.0267P)^2^+2.8051P] 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 7212 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Zr Zr 0.422982(19) 0.232764(13) 0.218381(12) 0.01880(6) Uani 1 1 d . . . Si1 Si 0.10797(6) 0.23346(4) 0.23994(4) 0.02354(13) Uani 1 1 d . . . Si2 Si 0.51791(6) 0.09855(4) 0.36440(4) 0.02580(14) Uani 1 1 d . . . Si3 Si 0.50301(6) 0.31892(4) 0.04800(4) 0.02349(14) Uani 1 1 d . . . N1 N 0.25486(17) 0.26770(12) 0.26918(11) 0.0239(4) Uani 1 1 d . . . N2 N 0.53878(17) 0.18526(12) 0.30704(11) 0.0239(4) Uani 1 1 d . . . N3 N 0.48975(18) 0.32389(12) 0.14492(11) 0.0237(4) Uani 1 1 d . . . N4 N 0.47968(18) 0.35478(12) 0.29608(11) 0.0254(4) Uani 1 1 d . . . N5 N 0.27400(17) 0.16981(12) 0.14599(11) 0.0237(4) Uani 1 1 d . . . N6 N 0.32654(18) 0.09511(12) 0.14614(10) 0.0230(4) Uani 1 1 d . . . N7 N 0.44754(17) 0.10635(12) 0.15589(10) 0.0222(4) Uani 1 1 d . . . C1 C 0.2660(2) 0.32508(16) 0.33437(14) 0.0306(5) Uani 1 1 d . . . H1A H 0.2928 0.2926 0.3795 0.037 Uiso 1 1 calc R . . H1B H 0.1840 0.3511 0.3435 0.037 Uiso 1 1 calc R . . C2 C 0.6308(2) 0.24813(16) 0.33662(15) 0.0310(5) Uani 1 1 d . . . H2A H 0.6889 0.2641 0.2973 0.037 Uiso 1 1 calc R . . H2B H 0.6799 0.2239 0.3794 0.037 Uiso 1 1 calc R . . C3 C 0.5017(2) 0.41321(15) 0.17079(14) 0.0303(5) Uani 1 1 d . . . H3A H 0.4192 0.4413 0.1676 0.036 Uiso 1 1 calc R . . H3B H 0.5587 0.4445 0.1384 0.036 Uiso 1 1 calc R . . C4 C 0.3608(2) 0.39373(15) 0.31925(14) 0.0307(5) Uani 1 1 d . . . H4A H 0.3277 0.4317 0.2792 0.037 Uiso 1 1 calc R . . H4B H 0.3764 0.4280 0.3650 0.037 Uiso 1 1 calc R . . C5 C 0.5583(2) 0.32561(16) 0.36166(14) 0.0310(5) Uani 1 1 d . . . H5A H 0.5052 0.3107 0.4037 0.037 Uiso 1 1 calc R . . H5B H 0.6166 0.3710 0.3784 0.037 Uiso 1 1 calc R . . C6 C 0.5524(2) 0.41433(15) 0.25067(14) 0.0306(5) Uani 1 1 d . . . H6A H 0.6413 0.3975 0.2524 0.037 Uiso 1 1 calc R . . H6B H 0.5464 0.4723 0.2713 0.037 Uiso 1 1 calc R . . C7 C -0.0032(3) 0.32231(17) 0.2192(2) 0.0471(8) Uani 1 1 d . . . H7A H -0.0186 0.3533 0.2654 0.071 Uiso 1 1 calc R . . H7B H -0.0820 0.2994 0.1985 0.071 Uiso 1 1 calc R . . H7C H 0.0327 0.3608 0.1829 0.071 Uiso 1 1 calc R . . C8 C 0.0295(3) 0.16172(18) 0.30710(15) 0.0361(6) Uani 1 1 d . . . H8A H 0.0181 0.1917 0.3543 0.054 Uiso 1 1 calc R . . H8B H 0.0813 0.1115 0.3164 0.054 Uiso 1 1 calc R . . H8C H -0.0520 0.1445 0.2857 0.054 Uiso 1 1 calc R . . C9 C 0.5082(3) 0.13200(19) 0.46501(14) 0.0404(7) Uani 1 1 d . . . H9A H 0.4358 0.1691 0.4704 0.061 Uiso 1 1 calc R . . H9B H 0.5843 0.1625 0.4805 0.061 Uiso 1 1 calc R . . H9C H 0.4993 0.0818 0.4965 0.061 Uiso 1 1 calc R . . C10 C 0.3667(2) 0.04539(16) 0.33795(15) 0.0322(6) Uani 1 1 d . . . H10A H 0.3697 0.0240 0.2867 0.048 Uiso 1 1 calc R . . H10B H 0.2983 0.0862 0.3412 0.048 Uiso 1 1 calc R . . H10C H 0.3529 -0.0019 0.3722 0.048 Uiso 1 1 calc R . . C11 C 0.6509(2) 0.02204(17) 0.35956(15) 0.0343(6) Uani 1 1 d . . . H11A H 0.6579 0.0024 0.3080 0.051 Uiso 1 1 calc R . . H11B H 0.6358 -0.0265 0.3922 0.051 Uiso 1 1 calc R . . H11C H 0.7285 0.0502 0.3760 0.051 Uiso 1 1 calc R . . C12 C 0.4627(3) 0.21348(16) 0.00668(14) 0.0361(6) Uani 1 1 d . . . H12A H 0.3788 0.1971 0.0211 0.054 Uiso 1 1 calc R . . H12B H 0.5231 0.1712 0.0252 0.054 Uiso 1 1 calc R . . H12C H 0.4649 0.2168 -0.0479 0.054 Uiso 1 1 calc R . . C13 C 0.3940(3) 0.39810(18) 0.00307(15) 0.0368(6) Uani 1 1 d . . . H13A H 0.3077 0.3812 0.0111 0.055 Uiso 1 1 calc R . . H13B H 0.4078 0.4006 -0.0507 0.055 Uiso 1 1 calc R . . H13C H 0.4096 0.4540 0.0253 0.055 Uiso 1 1 calc R . . C14 C 0.6665(2) 0.34353(18) 0.02274(15) 0.0347(6) Uani 1 1 d . . . H14A H 0.7232 0.3011 0.0450 0.052 Uiso 1 1 calc R . . H14B H 0.6897 0.3998 0.0417 0.052 Uiso 1 1 calc R . . H14C H 0.6724 0.3426 -0.0318 0.052 Uiso 1 1 calc R . . C15 C 0.1386(2) 0.17157(16) 0.15094(13) 0.0284(5) Uani 1 1 d . . . H15A H 0.1048 0.1134 0.1541 0.034 Uiso 1 1 calc R . . H15B H 0.0995 0.2001 0.1067 0.034 Uiso 1 1 calc R . . C16 C 0.5194(2) 0.02777(14) 0.15423(14) 0.0280(5) Uani 1 1 d . . . H16A H 0.4704 -0.0163 0.1269 0.034 Uiso 1 1 calc R . . H16B H 0.5367 0.0075 0.2059 0.034 Uiso 1 1 calc R . . C17 C 0.6407(2) 0.04250(14) 0.11619(13) 0.0252(5) Uani 1 1 d . . . C18 C 0.7225(2) 0.10473(17) 0.14272(15) 0.0332(6) Uani 1 1 d . . . H18A H 0.7036 0.1362 0.1861 0.040 Uiso 1 1 calc R . . C19 C 0.8317(2) 0.12110(18) 0.10610(16) 0.0372(6) Uani 1 1 d . . . H19A H 0.8863 0.1645 0.1242 0.045 Uiso 1 1 calc R . . C20 C 0.8620(2) 0.07511(18) 0.04361(15) 0.0348(6) Uani 1 1 d . . . H20A H 0.9373 0.0863 0.0191 0.042 Uiso 1 1 calc R . . C21 C 0.7817(2) 0.01265(17) 0.01711(15) 0.0348(6) Uani 1 1 d . . . H21A H 0.8021 -0.0196 -0.0255 0.042 Uiso 1 1 calc R . . C22 C 0.6712(2) -0.00299(15) 0.05274(14) 0.0293(5) Uani 1 1 d . . . H22A H 0.6158 -0.0453 0.0336 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01918(11) 0.01564(10) 0.02145(11) -0.00104(8) -0.00101(8) -0.00100(8) Si1 0.0209(3) 0.0212(3) 0.0285(3) -0.0023(3) 0.0009(2) 0.0018(3) Si2 0.0246(3) 0.0263(3) 0.0262(3) 0.0039(3) -0.0020(3) 0.0033(3) Si3 0.0251(3) 0.0204(3) 0.0248(3) 0.0026(2) -0.0016(3) -0.0040(2) N1 0.0233(9) 0.0223(9) 0.0261(10) -0.0055(8) 0.0000(8) 0.0009(8) N2 0.0212(9) 0.0231(10) 0.0272(10) -0.0003(8) -0.0028(8) -0.0009(8) N3 0.0281(10) 0.0168(9) 0.0261(10) -0.0004(7) -0.0013(8) -0.0041(8) N4 0.0283(10) 0.0213(10) 0.0265(10) -0.0038(8) -0.0016(8) -0.0029(8) N5 0.0204(9) 0.0253(10) 0.0254(10) -0.0030(8) 0.0008(8) -0.0008(8) N6 0.0246(10) 0.0221(9) 0.0225(9) -0.0014(8) 0.0026(8) -0.0037(8) N7 0.0219(9) 0.0192(9) 0.0255(10) -0.0020(7) -0.0004(8) -0.0014(7) C1 0.0289(13) 0.0327(13) 0.0301(13) -0.0096(10) 0.0022(10) 0.0023(10) C2 0.0267(12) 0.0307(13) 0.0351(14) -0.0012(10) -0.0061(10) -0.0035(10) C3 0.0381(14) 0.0207(12) 0.0320(13) -0.0014(10) 0.0016(11) -0.0059(10) C4 0.0346(14) 0.0247(12) 0.0326(13) -0.0094(10) -0.0015(11) 0.0022(10) C5 0.0337(13) 0.0309(13) 0.0277(12) -0.0066(10) -0.0084(10) -0.0043(11) C6 0.0363(14) 0.0206(12) 0.0345(13) -0.0051(10) -0.0021(11) -0.0082(10) C7 0.0353(15) 0.0265(14) 0.079(2) -0.0067(14) -0.0124(15) 0.0060(12) C8 0.0377(15) 0.0400(15) 0.0312(13) -0.0018(11) 0.0065(11) -0.0081(12) C9 0.0440(16) 0.0495(17) 0.0278(13) 0.0032(12) 0.0018(12) 0.0049(13) C10 0.0258(12) 0.0326(13) 0.0383(14) 0.0082(11) 0.0011(11) 0.0003(10) C11 0.0298(13) 0.0315(14) 0.0408(15) 0.0005(11) -0.0086(11) 0.0074(11) C12 0.0545(17) 0.0289(13) 0.0248(12) 0.0010(10) 0.0008(12) -0.0126(12) C13 0.0342(14) 0.0390(15) 0.0368(14) 0.0083(12) -0.0052(11) 0.0027(12) C14 0.0287(13) 0.0387(15) 0.0367(14) 0.0014(11) 0.0009(11) -0.0021(11) C15 0.0214(11) 0.0358(14) 0.0277(12) -0.0032(10) -0.0011(9) -0.0021(10) C16 0.0323(13) 0.0187(11) 0.0332(13) -0.0013(10) 0.0040(10) 0.0014(10) C17 0.0263(12) 0.0205(11) 0.0286(12) -0.0007(9) -0.0025(9) 0.0061(9) C18 0.0263(12) 0.0368(14) 0.0364(14) -0.0163(11) -0.0025(10) 0.0017(11) C19 0.0210(12) 0.0408(15) 0.0495(16) -0.0133(13) -0.0022(11) -0.0027(11) C20 0.0265(13) 0.0426(15) 0.0355(14) -0.0005(12) 0.0027(11) 0.0021(11) C21 0.0371(15) 0.0380(15) 0.0295(13) -0.0083(11) 0.0035(11) 0.0048(12) C22 0.0333(13) 0.0237(12) 0.0306(13) -0.0058(10) -0.0030(10) -0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N3 2.0936(19) . ? Zr N2 2.1161(19) . ? Zr N1 2.1228(19) . ? Zr N5 2.2514(19) . ? Zr N7 2.3084(19) . ? Zr N4 2.4403(19) . ? Zr N6 2.7147(19) . ? Si1 N1 1.729(2) . ? Si1 C7 1.870(3) . ? Si1 C8 1.874(3) . ? Si1 C15 1.908(2) . ? Si2 N2 1.731(2) . ? Si2 C10 1.872(3) . ? Si2 C11 1.874(3) . ? Si2 C9 1.883(3) . ? Si3 N3 1.747(2) . ? Si3 C12 1.867(3) . ? Si3 C14 1.869(3) . ? Si3 C13 1.873(3) . ? N1 C1 1.479(3) . ? N2 C2 1.484(3) . ? N3 C3 1.489(3) . ? N4 C6 1.483(3) . ? N4 C4 1.488(3) . ? N4 C5 1.493(3) . ? N5 N6 1.307(3) . ? N5 C15 1.459(3) . ? N6 N7 1.316(3) . ? N7 C16 1.462(3) . ? C1 C4 1.518(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.511(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.509(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.390(3) . ? C17 C22 1.393(3) . ? C18 C19 1.388(4) . ? C18 H18A 0.9500 . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.382(4) . ? C20 H20A 0.9500 . ? C21 C22 1.389(4) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zr N2 120.64(8) . . ? N3 Zr N1 113.97(8) . . ? N2 Zr N1 104.81(8) . . ? N3 Zr N5 101.21(7) . . ? N2 Zr N5 131.26(7) . . ? N1 Zr N5 76.40(7) . . ? N3 Zr N7 104.03(7) . . ? N2 Zr N7 88.98(7) . . ? N1 Zr N7 123.12(7) . . ? N5 Zr N7 55.29(7) . . ? N3 Zr N4 74.40(7) . . ? N2 Zr N4 74.08(7) . . ? N1 Zr N4 75.43(7) . . ? N5 Zr N4 146.45(7) . . ? N7 Zr N4 158.22(7) . . ? N3 Zr N6 112.63(7) . . ? N2 Zr N6 106.02(7) . . ? N1 Zr N6 95.58(7) . . ? N5 Zr N6 28.63(6) . . ? N7 Zr N6 28.94(6) . . ? N4 Zr N6 170.54(6) . . ? N1 Si1 C7 113.14(12) . . ? N1 Si1 C8 114.92(11) . . ? C7 Si1 C8 106.39(14) . . ? N1 Si1 C15 103.28(10) . . ? C7 Si1 C15 110.32(13) . . ? C8 Si1 C15 108.73(12) . . ? N2 Si2 C10 109.56(10) . . ? N2 Si2 C11 111.55(11) . . ? C10 Si2 C11 110.69(12) . . ? N2 Si2 C9 110.99(12) . . ? C10 Si2 C9 106.81(13) . . ? C11 Si2 C9 107.12(13) . . ? N3 Si3 C12 114.03(10) . . ? N3 Si3 C14 110.03(11) . . ? C12 Si3 C14 107.20(13) . . ? N3 Si3 C13 108.88(11) . . ? C12 Si3 C13 107.08(13) . . ? C14 Si3 C13 109.51(13) . . ? C1 N1 Si1 118.45(15) . . ? C1 N1 Zr 116.90(14) . . ? Si1 N1 Zr 124.65(10) . . ? C2 N2 Si2 114.63(16) . . ? C2 N2 Zr 113.24(15) . . ? Si2 N2 Zr 129.79(10) . . ? C3 N3 Si3 110.00(15) . . ? C3 N3 Zr 118.93(15) . . ? Si3 N3 Zr 129.40(10) . . ? C6 N4 C4 111.34(19) . . ? C6 N4 C5 109.45(19) . . ? C4 N4 C5 111.95(19) . . ? C6 N4 Zr 108.27(14) . . ? C4 N4 Zr 106.68(14) . . ? C5 N4 Zr 109.03(14) . . ? N6 N5 C15 116.58(19) . . ? N6 N5 Zr 95.76(13) . . ? C15 N5 Zr 130.08(15) . . ? N5 N6 N7 107.57(17) . . ? N5 N6 Zr 55.60(11) . . ? N7 N6 Zr 58.12(10) . . ? N6 N7 C16 113.66(18) . . ? N6 N7 Zr 92.93(12) . . ? C16 N7 Zr 144.48(15) . . ? N1 C1 C4 109.4(2) . . ? N1 C1 H1A 109.8 . . ? C4 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C4 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C5 107.60(19) . . ? N2 C2 H2A 110.2 . . ? C5 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C5 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N3 C3 C6 109.22(19) . . ? N3 C3 H3A 109.8 . . ? C6 C3 H3A 109.8 . . ? N3 C3 H3B 109.8 . . ? C6 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N4 C4 C1 109.97(19) . . ? N4 C4 H4A 109.7 . . ? C1 C4 H4A 109.7 . . ? N4 C4 H4B 109.7 . . ? C1 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N4 C5 C2 107.21(19) . . ? N4 C5 H5A 110.3 . . ? C2 C5 H5A 110.3 . . ? N4 C5 H5B 110.3 . . ? C2 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? N4 C6 C3 109.46(19) . . ? N4 C6 H6A 109.8 . . ? C3 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C3 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 Si1 105.26(15) . . ? N5 C15 H15A 110.7 . . ? Si1 C15 H15A 110.7 . . ? N5 C15 H15B 110.7 . . ? Si1 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? N7 C16 C17 110.03(19) . . ? N7 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? N7 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C22 118.6(2) . . ? C18 C17 C16 120.0(2) . . ? C22 C17 C16 121.4(2) . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C21 C20 C19 119.3(2) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 120.1(2) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C17 120.9(2) . . ? C21 C22 H22A 119.6 . . ? C17 C22 H22A 119.6 . . ? 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 C7 Si1 N1 C1 55.4(2) . . . . ? C8 Si1 N1 C1 -67.0(2) . . . . ? C15 Si1 N1 C1 174.72(18) . . . . ? C7 Si1 N1 Zr -124.89(16) . . . . ? C8 Si1 N1 Zr 112.64(14) . . . . ? C15 Si1 N1 Zr -5.62(15) . . . . ? N3 Zr N1 C1 -80.89(18) . . . . ? N2 Zr N1 C1 53.09(18) . . . . ? N5 Zr N1 C1 -177.28(18) . . . . ? N7 Zr N1 C1 151.75(16) . . . . ? N4 Zr N1 C1 -15.70(16) . . . . ? N6 Zr N1 C1 161.31(17) . . . . ? N3 Zr N1 Si1 99.44(13) . . . . ? N2 Zr N1 Si1 -126.59(12) . . . . ? N5 Zr N1 Si1 3.05(12) . . . . ? N7 Zr N1 Si1 -27.93(16) . . . . ? N4 Zr N1 Si1 164.63(14) . . . . ? N6 Zr N1 Si1 -18.37(13) . . . . ? C10 Si2 N2 C2 160.94(17) . . . . ? C11 Si2 N2 C2 -76.14(19) . . . . ? C9 Si2 N2 C2 43.2(2) . . . . ? C10 Si2 N2 Zr -0.25(18) . . . . ? C11 Si2 N2 Zr 122.66(14) . . . . ? C9 Si2 N2 Zr -117.97(15) . . . . ? N3 Zr N2 C2 31.30(19) . . . . ? N1 Zr N2 C2 -98.86(16) . . . . ? N5 Zr N2 C2 176.40(14) . . . . ? N7 Zr N2 C2 137.04(16) . . . . ? N4 Zr N2 C2 -29.10(15) . . . . ? N6 Zr N2 C2 160.74(15) . . . . ? N3 Zr N2 Si2 -167.30(12) . . . . ? N1 Zr N2 Si2 62.54(15) . . . . ? N5 Zr N2 Si2 -22.20(18) . . . . ? N7 Zr N2 Si2 -61.55(14) . . . . ? N4 Zr N2 Si2 132.30(15) . . . . ? N6 Zr N2 Si2 -37.86(15) . . . . ? C12 Si3 N3 C3 -170.08(17) . . . . ? C14 Si3 N3 C3 69.45(19) . . . . ? C13 Si3 N3 C3 -50.58(19) . . . . ? C12 Si3 N3 Zr -5.23(19) . . . . ? C14 Si3 N3 Zr -125.70(15) . . . . ? C13 Si3 N3 Zr 114.27(15) . . . . ? N2 Zr N3 C3 -75.76(18) . . . . ? N1 Zr N3 C3 50.28(18) . . . . ? N5 Zr N3 C3 130.24(17) . . . . ? N7 Zr N3 C3 -173.05(16) . . . . ? N4 Zr N3 C3 -15.53(16) . . . . ? N6 Zr N3 C3 157.77(16) . . . . ? N2 Zr N3 Si3 120.53(13) . . . . ? N1 Zr N3 Si3 -113.43(13) . . . . ? N5 Zr N3 Si3 -33.46(15) . . . . ? N7 Zr N3 Si3 23.25(15) . . . . ? N4 Zr N3 Si3 -179.23(15) . . . . ? N6 Zr N3 Si3 -5.94(16) . . . . ? N3 Zr N4 C6 -11.96(15) . . . . ? N2 Zr N4 C6 117.08(16) . . . . ? N1 Zr N4 C6 -132.51(16) . . . . ? N5 Zr N4 C6 -98.76(18) . . . . ? N7 Zr N4 C6 76.9(2) . . . . ? N6 Zr N4 C6 -151.0(3) . . . . ? N3 Zr N4 C4 107.97(16) . . . . ? N2 Zr N4 C4 -122.99(16) . . . . ? N1 Zr N4 C4 -12.58(15) . . . . ? N5 Zr N4 C4 21.2(2) . . . . ? N7 Zr N4 C4 -163.19(17) . . . . ? N6 Zr N4 C4 -31.0(5) . . . . ? N3 Zr N4 C5 -130.96(16) . . . . ? N2 Zr N4 C5 -1.92(15) . . . . ? N1 Zr N4 C5 108.49(16) . . . . ? N5 Zr N4 C5 142.24(15) . . . . ? N7 Zr N4 C5 -42.1(3) . . . . ? N6 Zr N4 C5 90.0(4) . . . . ? N3 Zr N5 N6 117.10(13) . . . . ? N2 Zr N5 N6 -32.78(17) . . . . ? N1 Zr N5 N6 -130.69(14) . . . . ? N7 Zr N5 N6 17.69(11) . . . . ? N4 Zr N5 N6 -164.27(12) . . . . ? N3 Zr N5 C15 -110.6(2) . . . . ? N2 Zr N5 C15 99.5(2) . . . . ? N1 Zr N5 C15 1.59(19) . . . . ? N7 Zr N5 C15 150.0(2) . . . . ? N4 Zr N5 C15 -32.0(3) . . . . ? N6 Zr N5 C15 132.3(3) . . . . ? C15 N5 N6 N7 -168.10(18) . . . . ? Zr N5 N6 N7 -27.37(17) . . . . ? C15 N5 N6 Zr -140.7(2) . . . . ? N3 Zr N6 N5 -71.10(14) . . . . ? N2 Zr N6 N5 154.95(13) . . . . ? N1 Zr N6 N5 47.78(14) . . . . ? N7 Zr N6 N5 -148.9(2) . . . . ? N4 Zr N6 N5 65.7(4) . . . . ? N3 Zr N6 N7 77.83(14) . . . . ? N2 Zr N6 N7 -56.12(14) . . . . ? N1 Zr N6 N7 -163.30(13) . . . . ? N5 Zr N6 N7 148.9(2) . . . . ? N4 Zr N6 N7 -145.4(4) . . . . ? N5 N6 N7 C16 -177.65(18) . . . . ? Zr N6 N7 C16 155.8(2) . . . . ? N5 N6 N7 Zr 26.53(16) . . . . ? N3 Zr N7 N6 -111.56(13) . . . . ? N2 Zr N7 N6 127.05(13) . . . . ? N1 Zr N7 N6 19.97(15) . . . . ? N5 Zr N7 N6 -17.51(12) . . . . ? N4 Zr N7 N6 165.42(16) . . . . ? N3 Zr N7 C16 108.7(3) . . . . ? N2 Zr N7 C16 -12.7(3) . . . . ? N1 Zr N7 C16 -119.8(2) . . . . ? N5 Zr N7 C16 -157.3(3) . . . . ? N4 Zr N7 C16 25.7(4) . . . . ? N6 Zr N7 C16 -139.8(3) . . . . ? Si1 N1 C1 C4 -138.48(18) . . . . ? Zr N1 C1 C4 41.8(2) . . . . ? Si2 N2 C2 C5 -107.18(19) . . . . ? Zr N2 C2 C5 57.2(2) . . . . ? Si3 N3 C3 C6 -152.59(17) . . . . ? Zr N3 C3 C6 40.7(3) . . . . ? C6 N4 C4 C1 155.4(2) . . . . ? C5 N4 C4 C1 -81.8(2) . . . . ? Zr N4 C4 C1 37.4(2) . . . . ? N1 C1 C4 N4 -52.3(3) . . . . ? C6 N4 C5 C2 -87.8(2) . . . . ? C4 N4 C5 C2 148.3(2) . . . . ? Zr N4 C5 C2 30.5(2) . . . . ? N2 C2 C5 N4 -55.7(3) . . . . ? C4 N4 C6 C3 -81.2(2) . . . . ? C5 N4 C6 C3 154.5(2) . . . . ? Zr N4 C6 C3 35.8(2) . . . . ? N3 C3 C6 N4 -49.3(3) . . . . ? N6 N5 C15 Si1 119.92(18) . . . . ? Zr N5 C15 Si1 -4.7(2) . . . . ? N1 Si1 C15 N5 5.47(18) . . . . ? C7 Si1 C15 N5 126.67(17) . . . . ? C8 Si1 C15 N5 -117.02(17) . . . . ? N6 N7 C16 C17 143.0(2) . . . . ? Zr N7 C16 C17 -81.8(3) . . . . ? N7 C16 C17 C18 56.3(3) . . . . ? N7 C16 C17 C22 -121.3(2) . . . . ? C22 C17 C18 C19 0.4(4) . . . . ? C16 C17 C18 C19 -177.2(2) . . . . ? C17 C18 C19 C20 -1.1(4) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C17 -1.2(4) . . . . ? C18 C17 C22 C21 0.7(4) . . . . ? C16 C17 C22 C21 178.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.595 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.068 # Attachment '- cmpd-5.cif' data_rw433zr _database_code_depnum_ccdc_archive 'CCDC 780978' #TrackingRef '- cmpd-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 N4 O Si3 Zr' _chemical_formula_weight 632.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0807(3) _cell_length_b 15.3755(5) _cell_length_c 20.9774(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.42 _cell_angle_gamma 90.00 _cell_volume 3251.32(17) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9833 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.32 _exptl_crystal_description Bulk _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9027 _exptl_absorpt_correction_T_max 0.9236 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45315 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.46 _reflns_number_total 9295 _reflns_number_gt 8145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. EXTI refined to 0 ; _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^)+(0.0288P)^2^+1.3874P] 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 9295 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.962373(11) 0.782311(7) 0.143501(5) 0.01362(3) Uani 1 1 d . . . N1 N 1.10089(10) 0.74557(7) 0.07370(5) 0.0198(2) Uani 1 1 d . . . N2 N 0.85610(10) 0.89157(7) 0.10969(5) 0.0184(2) Uani 1 1 d . . . N3 N 1.02830(11) 0.78784(7) 0.23813(5) 0.0214(2) Uani 1 1 d . . . N4 N 1.12522(10) 0.89458(7) 0.14769(5) 0.01754(19) Uani 1 1 d . . . Si1 Si 1.06808(4) 0.69372(2) 0.002224(17) 0.02059(7) Uani 1 1 d . . . Si2 Si 0.70961(3) 0.89253(2) 0.065496(17) 0.01945(7) Uani 1 1 d . . . Si3 Si 0.97800(4) 0.71454(2) 0.296239(16) 0.01894(7) Uani 1 1 d . . . O O 0.84529(8) 0.68434(6) 0.16215(4) 0.01685(16) Uani 1 1 d . . . C1 C 1.23024(13) 0.79115(9) 0.07560(7) 0.0253(3) Uani 1 1 d . . . H1A H 1.2755 0.7845 0.0342 0.030 Uiso 1 1 calc R . . H1B H 1.2875 0.7654 0.1092 0.030 Uiso 1 1 calc R . . C2 C 0.93208(13) 0.97338(8) 0.10365(7) 0.0243(3) Uani 1 1 d . . . H2A H 0.8726 1.0233 0.1118 0.029 Uiso 1 1 calc R . . H2B H 0.9655 0.9787 0.0596 0.029 Uiso 1 1 calc R . . C3 C 1.12189(16) 0.85513(10) 0.26078(7) 0.0303(3) Uani 1 1 d . . . H3A H 1.1781 0.8314 0.2955 0.036 Uiso 1 1 calc R . . H3B H 1.0721 0.9055 0.2777 0.036 Uiso 1 1 calc R . . C4 C 1.20762(12) 0.88712(8) 0.08948(6) 0.0216(2) Uani 1 1 d . . . H4A H 1.2937 0.9168 0.0962 0.026 Uiso 1 1 calc R . . H4B H 1.1617 0.9150 0.0529 0.026 Uiso 1 1 calc R . . C5 C 1.04833(13) 0.97641(8) 0.15014(7) 0.0220(2) Uani 1 1 d . . . H5A H 1.1067 1.0259 0.1394 0.026 Uiso 1 1 calc R . . H5B H 1.0150 0.9855 0.1939 0.026 Uiso 1 1 calc R . . C6 C 1.20853(14) 0.88396(9) 0.20560(7) 0.0265(3) Uani 1 1 d . . . H6A H 1.2524 0.9398 0.2162 0.032 Uiso 1 1 calc R . . H6B H 1.2783 0.8400 0.1978 0.032 Uiso 1 1 calc R . . C7 C 0.89668(15) 0.64756(10) 0.00460(7) 0.0292(3) Uani 1 1 d . . . H7A H 0.8926 0.6020 0.0372 0.044 Uiso 1 1 calc R . . H7B H 0.8741 0.6227 -0.0371 0.044 Uiso 1 1 calc R . . H7C H 0.8335 0.6938 0.0149 0.044 Uiso 1 1 calc R . . C8 C 1.08029(16) 0.77249(10) -0.06603(7) 0.0314(3) Uani 1 1 d . . . H8A H 1.0133 0.8182 -0.0612 0.047 Uiso 1 1 calc R . . H8B H 1.0651 0.7416 -0.1063 0.047 Uiso 1 1 calc R . . H8C H 1.1689 0.7988 -0.0662 0.047 Uiso 1 1 calc R . . C9 C 1.18811(17) 0.60383(10) -0.01382(8) 0.0333(3) Uani 1 1 d . . . H9A H 1.1776 0.5581 0.0183 0.050 Uiso 1 1 calc R . . H9B H 1.2788 0.6266 -0.0119 0.050 Uiso 1 1 calc R . . H9C H 1.1708 0.5796 -0.0563 0.050 Uiso 1 1 calc R . . C10 C 0.74395(15) 0.88606(10) -0.02197(6) 0.0289(3) Uani 1 1 d . . . H10A H 0.7716 0.8268 -0.0329 0.043 Uiso 1 1 calc R . . H10B H 0.8148 0.9270 -0.0328 0.043 Uiso 1 1 calc R . . H10C H 0.6634 0.9010 -0.0460 0.043 Uiso 1 1 calc R . . C11 C 0.61610(16) 0.99594(11) 0.07924(8) 0.0353(3) Uani 1 1 d . . . H11A H 0.6061 1.0054 0.1252 0.053 Uiso 1 1 calc R . . H11B H 0.5283 0.9918 0.0591 0.053 Uiso 1 1 calc R . . H11C H 0.6650 1.0447 0.0606 0.053 Uiso 1 1 calc R . . C12 C 0.60056(14) 0.79936(11) 0.08626(7) 0.0314(3) Uani 1 1 d . . . H12A H 0.5626 0.8088 0.1286 0.047 Uiso 1 1 calc R . . H12B H 0.6527 0.7456 0.0865 0.047 Uiso 1 1 calc R . . H12C H 0.5289 0.7946 0.0547 0.047 Uiso 1 1 calc R . . C13 C 0.95133(16) 0.77124(11) 0.37422(7) 0.0336(3) Uani 1 1 d . . . H13A H 0.8860 0.8178 0.3685 0.050 Uiso 1 1 calc R . . H13B H 1.0354 0.7961 0.3893 0.050 Uiso 1 1 calc R . . H13C H 0.9186 0.7294 0.4057 0.050 Uiso 1 1 calc R . . C14 C 1.10818(13) 0.62924(10) 0.30939(7) 0.0260(3) Uani 1 1 d . . . H14A H 1.1908 0.6569 0.3236 0.039 Uiso 1 1 calc R . . H14B H 1.1237 0.5979 0.2694 0.039 Uiso 1 1 calc R . . H14C H 1.0781 0.5882 0.3420 0.039 Uiso 1 1 calc R . . C15 C 0.81127(12) 0.66707(8) 0.27414(6) 0.0189(2) Uani 1 1 d . . . H15A H 0.7896 0.6223 0.3063 0.023 Uiso 1 1 calc R . . H15B H 0.7445 0.7139 0.2783 0.023 Uiso 1 1 calc R . . C16 C 0.79248(11) 0.62555(8) 0.20774(6) 0.0163(2) Uani 1 1 d . . . C21 C 0.64624(12) 0.61035(8) 0.18908(6) 0.0192(2) Uani 1 1 d . . . C22 C 0.61873(13) 0.56826(9) 0.13141(7) 0.0265(3) Uani 1 1 d . . . H22A H 0.6897 0.5462 0.1066 0.032 Uiso 1 1 calc R . . C23 C 0.48892(15) 0.55823(10) 0.10988(8) 0.0336(3) Uani 1 1 d . . . H23A H 0.4719 0.5297 0.0705 0.040 Uiso 1 1 calc R . . C24 C 0.38459(14) 0.58957(11) 0.14544(8) 0.0353(3) Uani 1 1 d . . . H24A H 0.2960 0.5833 0.1304 0.042 Uiso 1 1 calc R . . C25 C 0.41001(14) 0.63011(11) 0.20297(8) 0.0337(3) Uani 1 1 d . . . H25A H 0.3385 0.6514 0.2277 0.040 Uiso 1 1 calc R . . C26 C 0.54032(13) 0.64000(9) 0.22498(7) 0.0256(3) Uani 1 1 d . . . H26A H 0.5566 0.6673 0.2649 0.031 Uiso 1 1 calc R . . C31 C 0.86673(12) 0.53855(8) 0.20512(6) 0.0177(2) Uani 1 1 d . . . C32 C 0.82035(13) 0.46849(8) 0.24099(6) 0.0228(3) Uani 1 1 d . . . H32A H 0.7420 0.4749 0.2654 0.027 Uiso 1 1 calc R . . C33 C 0.88723(14) 0.38957(9) 0.24143(7) 0.0266(3) Uani 1 1 d . . . H33A H 0.8546 0.3425 0.2661 0.032 Uiso 1 1 calc R . . C34 C 1.00173(14) 0.37932(9) 0.20585(7) 0.0272(3) Uani 1 1 d . . . H34A H 1.0478 0.3254 0.2062 0.033 Uiso 1 1 calc R . . C35 C 1.04851(14) 0.44837(9) 0.16985(7) 0.0259(3) Uani 1 1 d . . . H35A H 1.1268 0.4417 0.1454 0.031 Uiso 1 1 calc R . . C36 C 0.98117(13) 0.52740(9) 0.16936(6) 0.0213(2) Uani 1 1 d . . . H36A H 1.0137 0.5742 0.1444 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01282(5) 0.01379(6) 0.01424(6) 0.00096(4) -0.00091(4) -0.00170(4) N1 0.0161(5) 0.0187(5) 0.0248(5) -0.0029(4) 0.0033(4) -0.0022(4) N2 0.0156(5) 0.0173(5) 0.0222(5) 0.0026(4) -0.0003(4) -0.0007(4) N3 0.0243(5) 0.0216(5) 0.0181(5) 0.0019(4) -0.0041(4) -0.0083(4) N4 0.0173(5) 0.0169(5) 0.0185(5) 0.0012(4) -0.0017(4) -0.0033(4) Si1 0.02340(17) 0.01746(16) 0.02098(17) -0.00075(13) 0.00445(13) -0.00009(13) Si2 0.01652(16) 0.02242(17) 0.01938(16) 0.00169(13) -0.00096(12) 0.00385(13) Si3 0.02007(16) 0.02284(17) 0.01390(15) 0.00143(12) -0.00031(12) -0.00290(13) O 0.0155(4) 0.0177(4) 0.0174(4) 0.0021(3) 0.0005(3) -0.0031(3) C1 0.0165(6) 0.0238(6) 0.0356(7) -0.0035(5) 0.0057(5) -0.0025(5) C2 0.0204(6) 0.0176(6) 0.0350(7) 0.0063(5) -0.0008(5) -0.0001(5) C3 0.0394(8) 0.0308(7) 0.0206(6) 0.0030(5) -0.0089(6) -0.0177(6) C4 0.0174(6) 0.0217(6) 0.0258(6) 0.0000(5) 0.0039(5) -0.0049(5) C5 0.0226(6) 0.0154(6) 0.0282(6) -0.0018(5) 0.0019(5) -0.0036(5) C6 0.0253(7) 0.0280(7) 0.0260(7) 0.0053(5) -0.0102(5) -0.0122(5) C7 0.0315(7) 0.0319(7) 0.0243(7) -0.0031(5) 0.0004(5) -0.0089(6) C8 0.0343(8) 0.0320(8) 0.0282(7) 0.0072(6) 0.0059(6) 0.0003(6) C9 0.0412(8) 0.0237(7) 0.0350(8) -0.0053(6) 0.0057(6) 0.0068(6) C10 0.0352(8) 0.0291(7) 0.0222(6) 0.0034(5) 0.0000(6) 0.0052(6) C11 0.0315(8) 0.0395(8) 0.0349(8) -0.0079(7) -0.0093(6) 0.0178(7) C12 0.0192(6) 0.0432(8) 0.0315(7) 0.0082(6) -0.0052(5) -0.0069(6) C13 0.0370(8) 0.0425(9) 0.0212(7) -0.0072(6) 0.0028(6) -0.0068(7) C14 0.0209(6) 0.0338(7) 0.0234(6) 0.0077(5) -0.0011(5) -0.0007(5) C15 0.0187(5) 0.0197(6) 0.0185(5) 0.0015(4) 0.0021(4) -0.0003(4) C16 0.0147(5) 0.0161(5) 0.0183(5) 0.0022(4) 0.0011(4) -0.0019(4) C21 0.0152(5) 0.0178(6) 0.0247(6) 0.0058(5) 0.0002(4) -0.0028(4) C22 0.0203(6) 0.0280(7) 0.0313(7) -0.0021(5) -0.0026(5) -0.0024(5) C23 0.0272(7) 0.0355(8) 0.0379(8) 0.0005(6) -0.0098(6) -0.0075(6) C24 0.0174(6) 0.0393(8) 0.0490(9) 0.0134(7) -0.0066(6) -0.0075(6) C25 0.0163(6) 0.0413(8) 0.0434(9) 0.0112(7) 0.0055(6) -0.0004(6) C26 0.0193(6) 0.0296(7) 0.0279(7) 0.0060(5) 0.0044(5) -0.0009(5) C31 0.0168(5) 0.0173(5) 0.0189(5) -0.0004(4) -0.0023(4) -0.0011(4) C32 0.0226(6) 0.0202(6) 0.0256(6) 0.0013(5) -0.0006(5) -0.0037(5) C33 0.0312(7) 0.0179(6) 0.0306(7) 0.0026(5) -0.0080(6) -0.0039(5) C34 0.0302(7) 0.0204(6) 0.0308(7) -0.0047(5) -0.0116(6) 0.0051(5) C35 0.0230(6) 0.0285(7) 0.0261(7) -0.0051(5) -0.0031(5) 0.0065(5) C36 0.0199(6) 0.0233(6) 0.0209(6) -0.0004(5) -0.0001(5) 0.0003(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 Zr O 1.9550(8) . ? Zr N3 2.0906(11) . ? Zr N1 2.1078(11) . ? Zr N2 2.1123(10) . ? Zr N4 2.3833(10) . ? N1 C1 1.4806(16) . ? N1 Si1 1.7279(11) . ? N2 C2 1.4786(16) . ? N2 Si2 1.7380(11) . ? N3 C3 1.4764(16) . ? N3 Si3 1.7384(11) . ? N4 C5 1.4789(16) . ? N4 C6 1.4809(16) . ? N4 C4 1.4863(16) . ? Si1 C7 1.8689(15) . ? Si1 C9 1.8691(15) . ? Si1 C8 1.8800(15) . ? Si2 C12 1.8594(15) . ? Si2 C11 1.8717(15) . ? Si2 C10 1.8724(14) . ? Si3 C14 1.8744(14) . ? Si3 C13 1.8748(15) . ? Si3 C15 1.8872(13) . ? O C16 1.4223(14) . ? C1 C4 1.5216(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.5199(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.521(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.5427(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C31 1.5340(17) . ? C16 C21 1.5404(16) . ? C21 C26 1.3881(18) . ? C21 C22 1.3980(19) . ? C22 C23 1.3897(19) . ? C22 H22A 0.9500 . ? C23 C24 1.381(2) . ? C23 H23A 0.9500 . ? C24 C25 1.381(2) . ? C24 H24A 0.9500 . ? C25 C26 1.3975(19) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C36 1.3912(17) . ? C31 C32 1.3967(17) . ? C32 C33 1.3881(19) . ? C32 H32A 0.9500 . ? C33 C34 1.388(2) . ? C33 H33A 0.9500 . ? C34 C35 1.387(2) . ? C34 H34A 0.9500 . ? C35 C36 1.3920(18) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Zr N3 91.70(4) . . ? O Zr N1 109.66(4) . . ? N3 Zr N1 117.58(4) . . ? O Zr N2 111.99(4) . . ? N3 Zr N2 116.32(4) . . ? N1 Zr N2 108.47(4) . . ? O Zr N4 165.33(3) . . ? N3 Zr N4 73.82(4) . . ? N1 Zr N4 76.12(4) . . ? N2 Zr N4 77.52(4) . . ? C1 N1 Si1 113.88(9) . . ? C1 N1 Zr 116.24(8) . . ? Si1 N1 Zr 127.08(6) . . ? C2 N2 Si2 112.69(8) . . ? C2 N2 Zr 116.33(8) . . ? Si2 N2 Zr 127.79(6) . . ? C3 N3 Si3 114.69(8) . . ? C3 N3 Zr 122.14(8) . . ? Si3 N3 Zr 123.17(6) . . ? C5 N4 C6 111.06(10) . . ? C5 N4 C4 112.98(10) . . ? C6 N4 C4 110.40(10) . . ? C5 N4 Zr 104.86(7) . . ? C6 N4 Zr 109.68(7) . . ? C4 N4 Zr 107.63(7) . . ? N1 Si1 C7 108.86(6) . . ? N1 Si1 C9 112.17(7) . . ? C7 Si1 C9 108.89(7) . . ? N1 Si1 C8 110.52(6) . . ? C7 Si1 C8 109.31(7) . . ? C9 Si1 C8 107.05(7) . . ? N2 Si2 C12 111.71(6) . . ? N2 Si2 C11 110.61(6) . . ? C12 Si2 C11 108.61(8) . . ? N2 Si2 C10 111.09(6) . . ? C12 Si2 C10 107.60(7) . . ? C11 Si2 C10 107.04(7) . . ? N3 Si3 C14 110.45(6) . . ? N3 Si3 C13 110.78(7) . . ? C14 Si3 C13 107.56(7) . . ? N3 Si3 C15 110.02(5) . . ? C14 Si3 C15 112.76(6) . . ? C13 Si3 C15 105.13(6) . . ? C16 O Zr 148.62(7) . . ? N1 C1 C4 109.33(10) . . ? N1 C1 H1A 109.8 . . ? C4 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C4 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C5 111.63(10) . . ? N2 C2 H2A 109.3 . . ? C5 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C5 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N3 C3 C6 109.18(11) . . ? N3 C3 H3A 109.8 . . ? C6 C3 H3A 109.8 . . ? N3 C3 H3B 109.8 . . ? C6 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N4 C4 C1 108.50(10) . . ? N4 C4 H4A 110.0 . . ? C1 C4 H4A 110.0 . . ? N4 C4 H4B 110.0 . . ? C1 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N4 C5 C2 110.70(10) . . ? N4 C5 H5A 109.5 . . ? C2 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C3 109.33(11) . . ? N4 C6 H6A 109.8 . . ? C3 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C3 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Si3 119.02(8) . . ? C16 C15 H15A 107.6 . . ? Si3 C15 H15A 107.6 . . ? C16 C15 H15B 107.6 . . ? Si3 C15 H15B 107.6 . . ? H15A C15 H15B 107.0 . . ? O C16 C31 110.18(9) . . ? O C16 C21 106.72(9) . . ? C31 C16 C21 108.96(10) . . ? O C16 C15 107.46(9) . . ? C31 C16 C15 109.67(10) . . ? C21 C16 C15 113.78(10) . . ? C26 C21 C22 118.23(12) . . ? C26 C21 C16 123.42(12) . . ? C22 C21 C16 118.27(11) . . ? C23 C22 C21 120.86(14) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C24 C23 C22 120.33(15) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.51(13) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 120.39(14) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C21 C26 C25 120.66(14) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C36 C31 C32 118.53(12) . . ? C36 C31 C16 122.25(11) . . ? C32 C31 C16 119.20(11) . . ? C33 C32 C31 120.89(13) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 120.10(13) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 119.54(13) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 120.29(13) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C31 C36 C35 120.66(12) . . ? C31 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? 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 O Zr N1 C1 -151.66(9) . . . . ? N3 Zr N1 C1 -48.83(10) . . . . ? N2 Zr N1 C1 85.75(10) . . . . ? N4 Zr N1 C1 14.25(9) . . . . ? O Zr N1 Si1 48.61(8) . . . . ? N3 Zr N1 Si1 151.44(7) . . . . ? N2 Zr N1 Si1 -73.98(8) . . . . ? N4 Zr N1 Si1 -145.48(8) . . . . ? O Zr N2 C2 170.82(9) . . . . ? N3 Zr N2 C2 67.20(10) . . . . ? N1 Zr N2 C2 -68.02(10) . . . . ? N4 Zr N2 C2 2.53(9) . . . . ? O Zr N2 Si2 -31.00(8) . . . . ? N3 Zr N2 Si2 -134.62(7) . . . . ? N1 Zr N2 Si2 90.16(7) . . . . ? N4 Zr N2 Si2 160.71(8) . . . . ? O Zr N3 C3 -176.99(11) . . . . ? N1 Zr N3 C3 69.73(12) . . . . ? N2 Zr N3 C3 -61.36(12) . . . . ? N4 Zr N3 C3 5.41(11) . . . . ? O Zr N3 Si3 2.92(7) . . . . ? N1 Zr N3 Si3 -110.36(7) . . . . ? N2 Zr N3 Si3 118.56(7) . . . . ? N4 Zr N3 Si3 -174.68(8) . . . . ? O Zr N4 C5 -109.86(15) . . . . ? N3 Zr N4 C5 -100.35(8) . . . . ? N1 Zr N4 C5 135.02(8) . . . . ? N2 Zr N4 C5 22.13(8) . . . . ? O Zr N4 C6 9.46(19) . . . . ? N3 Zr N4 C6 18.98(9) . . . . ? N1 Zr N4 C6 -105.65(9) . . . . ? N2 Zr N4 C6 141.46(9) . . . . ? O Zr N4 C4 129.60(14) . . . . ? N3 Zr N4 C4 139.11(8) . . . . ? N1 Zr N4 C4 14.49(8) . . . . ? N2 Zr N4 C4 -98.40(8) . . . . ? C1 N1 Si1 C7 -175.26(9) . . . . ? Zr N1 Si1 C7 -15.13(10) . . . . ? C1 N1 Si1 C9 64.17(11) . . . . ? Zr N1 Si1 C9 -135.70(8) . . . . ? C1 N1 Si1 C8 -55.20(11) . . . . ? Zr N1 Si1 C8 104.93(8) . . . . ? C2 N2 Si2 C12 -168.61(10) . . . . ? Zr N2 Si2 C12 32.55(10) . . . . ? C2 N2 Si2 C11 -47.50(11) . . . . ? Zr N2 Si2 C11 153.66(8) . . . . ? C2 N2 Si2 C10 71.22(10) . . . . ? Zr N2 Si2 C10 -87.61(8) . . . . ? C3 N3 Si3 C14 -79.99(12) . . . . ? Zr N3 Si3 C14 100.10(8) . . . . ? C3 N3 Si3 C13 39.08(12) . . . . ? Zr N3 Si3 C13 -140.83(8) . . . . ? C3 N3 Si3 C15 154.89(10) . . . . ? Zr N3 Si3 C15 -25.02(9) . . . . ? N3 Zr O C16 2.24(15) . . . . ? N1 Zr O C16 122.40(14) . . . . ? N2 Zr O C16 -117.13(14) . . . . ? N4 Zr O C16 11.4(2) . . . . ? Si1 N1 C1 C4 121.54(10) . . . . ? Zr N1 C1 C4 -40.86(14) . . . . ? Si2 N2 C2 C5 171.42(9) . . . . ? Zr N2 C2 C5 -27.15(14) . . . . ? Si3 N3 C3 C6 151.94(10) . . . . ? Zr N3 C3 C6 -28.14(16) . . . . ? C5 N4 C4 C1 -154.37(11) . . . . ? C6 N4 C4 C1 80.58(13) . . . . ? Zr N4 C4 C1 -39.10(11) . . . . ? N1 C1 C4 N4 52.58(14) . . . . ? C6 N4 C5 C2 -161.13(10) . . . . ? C4 N4 C5 C2 74.19(13) . . . . ? Zr N4 C5 C2 -42.73(11) . . . . ? N2 C2 C5 N4 48.25(14) . . . . ? C5 N4 C6 C3 76.77(13) . . . . ? C4 N4 C6 C3 -157.10(11) . . . . ? Zr N4 C6 C3 -38.67(13) . . . . ? N3 C3 C6 N4 42.91(16) . . . . ? N3 Si3 C15 C16 52.84(11) . . . . ? C14 Si3 C15 C16 -70.95(11) . . . . ? C13 Si3 C15 C16 172.15(10) . . . . ? Zr O C16 C31 -98.80(15) . . . . ? Zr O C16 C21 143.05(12) . . . . ? Zr O C16 C15 20.64(19) . . . . ? Si3 C15 C16 O -47.53(12) . . . . ? Si3 C15 C16 C31 72.24(11) . . . . ? Si3 C15 C16 C21 -165.44(8) . . . . ? O C16 C21 C26 -111.34(13) . . . . ? C31 C16 C21 C26 129.71(13) . . . . ? C15 C16 C21 C26 7.01(17) . . . . ? O C16 C21 C22 65.40(14) . . . . ? C31 C16 C21 C22 -53.54(14) . . . . ? C15 C16 C21 C22 -176.25(11) . . . . ? C26 C21 C22 C23 1.5(2) . . . . ? C16 C21 C22 C23 -175.39(13) . . . . ? C21 C22 C23 C24 -0.2(2) . . . . ? C22 C23 C24 C25 -0.8(2) . . . . ? C23 C24 C25 C26 0.5(2) . . . . ? C22 C21 C26 C25 -1.8(2) . . . . ? C16 C21 C26 C25 174.93(12) . . . . ? C24 C25 C26 C21 0.9(2) . . . . ? O C16 C31 C36 8.93(16) . . . . ? C21 C16 C31 C36 125.69(12) . . . . ? C15 C16 C31 C36 -109.16(13) . . . . ? O C16 C31 C32 -172.73(10) . . . . ? C21 C16 C31 C32 -55.96(14) . . . . ? C15 C16 C31 C32 69.18(14) . . . . ? C36 C31 C32 C33 0.45(19) . . . . ? C16 C31 C32 C33 -177.95(12) . . . . ? C31 C32 C33 C34 -0.1(2) . . . . ? C32 C33 C34 C35 -0.1(2) . . . . ? C33 C34 C35 C36 0.0(2) . . . . ? C32 C31 C36 C35 -0.59(19) . . . . ? C16 C31 C36 C35 177.77(11) . . . . ? C34 C35 C36 C31 0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.430 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.054