# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1942 data_erk_672 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H33 N Si Zr' _chemical_formula_weight 394.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'Pnma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.338(2) _cell_length_b 12.819(2) _cell_length_c 15.032(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1992.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 8.47 _cell_measurement_theta_max 20.67 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type 'empirical via \y scan data' _exptl_absorpt_correction_T_min 0.8877 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 4218 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.29 _reflns_number_total 2112 _reflns_number_gt 1300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Express (Nonius B.V., 1994)' _computing_cell_refinement 'Express (Nonius B.V., 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Tert.-butyl group disordered (50:50), refined with geometrical and thermal constrains (SADI and EADP). ; _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^)+(0.0506P)^2^+2.3981P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2112 _refine_ls_number_parameters 109 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.018 _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 Zr Zr 0.05756(6) 0.7500 0.43864(4) 0.03119(19) Uani 1 2 d S . . Si Si 0.32754(17) 0.7500 0.51927(12) 0.0359(4) Uani 1 2 d S . . N N 0.1688(5) 0.7500 0.5558(3) 0.0376(12) Uani 1 2 d S . . C2 C -0.1637(5) 0.8027(4) 0.4783(4) 0.0593(15) Uani 1 1 d . . . H2 H -0.2057 0.8361 0.5259 0.071 Uiso 1 1 d R . . C1 C -0.1056(5) 0.8680(5) 0.4125(5) 0.083(2) Uani 1 1 d . . . H1A H -0.0625 0.8380 0.3637 0.100 Uiso 1 1 d R . . H1B H -0.1104 0.9410 0.4179 0.100 Uiso 1 1 d R . . C11 C 0.2829(6) 0.7500 0.3986(4) 0.0285(13) Uani 1 2 d S . . C12 C 0.2302(4) 0.6607(3) 0.3544(3) 0.0325(10) Uani 1 1 d . . . C121 C 0.2576(5) 0.5475(4) 0.3750(3) 0.0461(12) Uani 1 1 d . . . H12A H 0.2330 0.5326 0.4360 0.069 Uiso 1 1 d R . . H12B H 0.3492 0.5338 0.3673 0.069 Uiso 1 1 d R . . H12C H 0.2083 0.5034 0.3350 0.069 Uiso 1 1 d R . . C13 C 0.1472(4) 0.6953(4) 0.2861(3) 0.0362(10) Uani 1 1 d . . . C131 C 0.0790(5) 0.6270(5) 0.2192(3) 0.0552(15) Uani 1 1 d . . . H13A H 0.0562 0.5612 0.2469 0.083 Uiso 1 1 d R . . H13B H 0.1359 0.6141 0.1691 0.083 Uiso 1 1 d R . . H13C H 0.0012 0.6617 0.1987 0.083 Uiso 1 1 d R . . C21 C 0.4295(6) 0.6348(5) 0.5504(3) 0.0674(16) Uani 1 1 d . . . H21A H 0.4629 0.6442 0.6102 0.101 Uiso 1 1 d R . . H21B H 0.5010 0.6285 0.5090 0.101 Uiso 1 1 d R . . H21C H 0.3773 0.5719 0.5482 0.101 Uiso 1 1 d R . . C31 C 0.1313(6) 0.7500 0.6521(5) 0.0515(19) Uani 1 2 d SD . . C32 C 0.0865(10) 0.6464(7) 0.6851(7) 0.076(3) Uani 0.50 1 d PDU . . H32A H 0.1566 0.5964 0.6807 0.114 Uiso 0.50 1 d PR . . H32B H 0.0141 0.6228 0.6493 0.114 Uiso 0.50 1 d PR . . H32C H 0.0595 0.6526 0.7466 0.114 Uiso 0.50 1 d PR . . C33 C 0.2401(10) 0.7896(6) 0.7108(6) 0.076(3) Uani 0.50 1 d PDU . . H33A H 0.2090 0.7971 0.7713 0.114 Uiso 0.50 1 d PR . . H33B H 0.2697 0.8567 0.6890 0.114 Uiso 0.50 1 d PR . . H33C H 0.3111 0.7402 0.7095 0.114 Uiso 0.50 1 d PR . . C34 C 0.0211(9) 0.8282(7) 0.6611(8) 0.076(3) Uani 0.50 1 d PDU . . H34A H 0.0483 0.8952 0.6376 0.114 Uiso 0.50 1 d PR . . H34B H -0.0017 0.8358 0.7234 0.114 Uiso 0.50 1 d PR . . H34C H -0.0534 0.8034 0.6281 0.114 Uiso 0.50 1 d 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 Zr 0.0279(3) 0.0299(3) 0.0357(3) 0.000 0.0031(3) 0.000 Si 0.0338(10) 0.0432(10) 0.0306(9) 0.000 -0.0024(8) 0.000 N 0.039(3) 0.047(3) 0.027(3) 0.000 0.007(3) 0.000 C2 0.038(3) 0.058(3) 0.081(4) 0.007(3) 0.017(3) 0.010(2) C1 0.056(3) 0.071(4) 0.122(6) 0.042(4) 0.047(4) 0.039(3) C11 0.028(3) 0.026(3) 0.031(3) 0.000 0.004(3) 0.000 C12 0.031(2) 0.031(2) 0.036(2) 0.0002(19) 0.0040(19) 0.0007(19) C121 0.047(3) 0.032(3) 0.060(3) -0.005(2) 0.004(2) 0.000(2) C13 0.029(2) 0.048(3) 0.032(2) -0.006(2) 0.0018(17) -0.004(2) C131 0.050(3) 0.073(4) 0.042(3) -0.018(3) -0.003(2) -0.007(3) C21 0.074(4) 0.077(4) 0.051(3) 0.000(3) -0.018(3) 0.032(3) C31 0.044(4) 0.080(6) 0.031(4) 0.000 0.007(3) 0.000 C32 0.124(7) 0.067(5) 0.039(4) -0.005(3) 0.017(4) 0.010(4) C33 0.124(7) 0.067(5) 0.039(4) -0.005(3) 0.017(4) 0.010(4) C34 0.124(7) 0.067(5) 0.039(4) -0.005(3) 0.017(4) 0.010(4) _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 N 2.103(5) . ? Zr C1 2.300(5) 7_575 ? Zr C1 2.300(5) . ? Zr C11 2.406(6) . ? Zr C2 2.459(5) 7_575 ? Zr C2 2.459(5) . ? Zr C12 2.469(4) 7_575 ? Zr C12 2.469(4) . ? Zr C13 2.570(4) . ? Zr C13 2.570(4) 7_575 ? Zr Si 3.0429(19) . ? Si N 1.731(5) . ? Si C11 1.871(7) . ? Si C21 1.874(5) 7_575 ? Si C21 1.874(5) . ? N C31 1.499(8) . ? C2 C2 1.352(11) 7_575 ? C2 C1 1.429(7) . ? C11 C12 1.432(5) . ? C11 C12 1.432(5) 7_575 ? C12 C13 1.409(6) . ? C12 C121 1.511(6) . ? C13 C13 1.401(9) 7_575 ? C13 C131 1.508(6) . ? C31 C32 1.491(7) 7_575 ? C31 C32 1.491(7) . ? C31 C33 1.516(7) . ? C31 C33 1.516(7) 7_575 ? C31 C34 1.524(7) 7_575 ? C31 C34 1.524(7) . ? 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 N Zr C1 123.0(2) . 7_575 ? N Zr C1 123.0(2) . . ? C1 Zr C1 82.3(4) 7_575 . ? N Zr C11 71.3(2) . . ? C1 Zr C11 131.86(16) 7_575 . ? C1 Zr C11 131.86(16) . . ? N Zr C2 107.77(19) . 7_575 ? C1 Zr C2 34.75(18) 7_575 7_575 ? C1 Zr C2 62.6(2) . 7_575 ? C11 Zr C2 164.04(13) . 7_575 ? N Zr C2 107.77(19) . . ? C1 Zr C2 62.6(2) 7_575 . ? C1 Zr C2 34.75(18) . . ? C11 Zr C2 164.04(13) . . ? C2 Zr C2 31.9(3) 7_575 . ? N Zr C12 91.98(15) . 7_575 ? C1 Zr C12 138.3(2) 7_575 7_575 ? C1 Zr C12 97.89(18) . 7_575 ? C11 Zr C12 34.12(12) . 7_575 ? C2 Zr C12 157.54(17) 7_575 7_575 ? C2 Zr C12 132.01(16) . 7_575 ? N Zr C12 91.98(15) . . ? C1 Zr C12 97.89(18) 7_575 . ? C1 Zr C12 138.3(2) . . ? C11 Zr C12 34.12(12) . . ? C2 Zr C12 132.01(16) 7_575 . ? C2 Zr C12 157.54(17) . . ? C12 Zr C12 55.2(2) 7_575 . ? N Zr C13 123.37(16) . . ? C1 Zr C13 86.13(18) 7_575 . ? C1 Zr C13 106.9(2) . . ? C11 Zr C13 55.10(17) . . ? C2 Zr C13 118.48(16) 7_575 . ? C2 Zr C13 128.82(17) . . ? C12 Zr C13 53.72(14) 7_575 . ? C12 Zr C13 32.39(13) . . ? N Zr C13 123.37(16) . 7_575 ? C1 Zr C13 106.9(2) 7_575 7_575 ? C1 Zr C13 86.13(18) . 7_575 ? C11 Zr C13 55.10(17) . 7_575 ? C2 Zr C13 128.82(17) 7_575 7_575 ? C2 Zr C13 118.48(16) . 7_575 ? C12 Zr C13 32.39(13) 7_575 7_575 ? C12 Zr C13 53.72(14) . 7_575 ? C13 Zr C13 31.6(2) . 7_575 ? N Zr Si 33.40(14) . . ? C1 Zr Si 137.80(19) 7_575 . ? C1 Zr Si 137.80(19) . . ? C11 Zr Si 37.95(15) . . ? C2 Zr Si 139.17(15) 7_575 . ? C2 Zr Si 139.17(15) . . ? C12 Zr Si 62.71(10) 7_575 . ? C12 Zr Si 62.71(10) . . ? C13 Zr Si 91.41(10) . . ? C13 Zr Si 91.41(10) 7_575 . ? N Si C11 94.2(3) . . ? N Si C21 117.0(2) . 7_575 ? C11 Si C21 112.39(19) . 7_575 ? N Si C21 117.0(2) . . ? C11 Si C21 112.39(19) . . ? C21 Si C21 104.0(4) 7_575 . ? N Si Zr 41.98(17) . . ? C11 Si Zr 52.26(18) . . ? C21 Si Zr 128.0(2) 7_575 . ? C21 Si Zr 128.0(2) . . ? C31 N Si 123.5(4) . . ? C31 N Zr 131.9(4) . . ? Si N Zr 104.6(2) . . ? C2 C2 C1 125.9(4) 7_575 . ? C2 C2 Zr 74.04(13) 7_575 . ? C1 C2 Zr 66.5(3) . . ? C2 C1 Zr 78.7(3) . . ? C12 C11 C12 106.1(5) . 7_575 ? C12 C11 Si 123.0(3) . . ? C12 C11 Si 123.0(3) 7_575 . ? C12 C11 Zr 75.4(3) . . ? C12 C11 Zr 75.4(3) 7_575 . ? Si C11 Zr 89.8(2) . . ? C13 C12 C11 108.6(4) . . ? C13 C12 C121 124.5(4) . . ? C11 C12 C121 126.9(4) . . ? C13 C12 Zr 77.7(2) . . ? C11 C12 Zr 70.5(3) . . ? C121 C12 Zr 118.4(3) . . ? C13 C13 C12 108.4(3) 7_575 . ? C13 C13 C131 125.5(3) 7_575 . ? C12 C13 C131 125.9(4) . . ? C13 C13 Zr 74.18(10) 7_575 . ? C12 C13 Zr 69.9(2) . . ? C131 C13 Zr 125.8(3) . . ? C32 C31 C32 125.9(10) 7_575 . ? C32 C31 N 113.6(5) 7_575 . ? C32 C31 N 113.6(5) . . ? C32 C31 C33 74.9(6) 7_575 . ? C32 C31 C33 109.6(4) . . ? N C31 C33 111.7(6) . . ? C32 C31 C33 109.6(4) 7_575 7_575 ? C32 C31 C33 74.9(5) . 7_575 ? N C31 C33 111.7(6) . 7_575 ? C33 C31 C33 39.1(6) . 7_575 ? C32 C31 C34 108.9(4) 7_575 7_575 ? C32 C31 C34 32.0(6) . 7_575 ? N C31 C34 106.2(6) . 7_575 ? C33 C31 C34 136.3(7) . 7_575 ? C33 C31 C34 106.4(4) 7_575 7_575 ? C32 C31 C34 32.0(6) 7_575 . ? C32 C31 C34 108.9(4) . . ? N C31 C34 106.2(6) . . ? C33 C31 C34 106.4(4) . . ? C33 C31 C34 136.3(7) 7_575 . ? C34 C31 C34 82.3(8) 7_575 . ? 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 Zr Si N -78.4(2) 7_575 . . . ? C1 Zr Si N 78.4(2) . . . . ? C11 Zr Si N 180.000(1) . . . . ? C2 Zr Si N -24.9(2) 7_575 . . . ? C2 Zr Si N 24.9(2) . . . . ? C12 Zr Si N 148.57(11) 7_575 . . . ? C12 Zr Si N -148.57(11) . . . . ? C13 Zr Si N -164.18(10) . . . . ? C13 Zr Si N 164.18(10) 7_575 . . . ? N Zr Si C11 180.0 . . . . ? C1 Zr Si C11 101.6(2) 7_575 . . . ? C1 Zr Si C11 -101.6(2) . . . . ? C2 Zr Si C11 155.1(2) 7_575 . . . ? C2 Zr Si C11 -155.1(2) . . . . ? C12 Zr Si C11 -31.43(11) 7_575 . . . ? C12 Zr Si C11 31.43(11) . . . . ? C13 Zr Si C11 15.82(10) . . . . ? C13 Zr Si C11 -15.82(10) 7_575 . . . ? N Zr Si C21 -89.6(2) . . . 7_575 ? C1 Zr Si C21 -168.0(3) 7_575 . . 7_575 ? C1 Zr Si C21 -11.2(3) . . . 7_575 ? C11 Zr Si C21 90.4(2) . . . 7_575 ? C2 Zr Si C21 -114.5(3) 7_575 . . 7_575 ? C2 Zr Si C21 -64.7(3) . . . 7_575 ? C12 Zr Si C21 59.0(3) 7_575 . . 7_575 ? C12 Zr Si C21 121.8(3) . . . 7_575 ? C13 Zr Si C21 106.2(3) . . . 7_575 ? C13 Zr Si C21 74.6(2) 7_575 . . 7_575 ? N Zr Si C21 89.6(2) . . . . ? C1 Zr Si C21 11.2(3) 7_575 . . . ? C1 Zr Si C21 168.0(3) . . . . ? C11 Zr Si C21 -90.4(2) . . . . ? C2 Zr Si C21 64.7(3) 7_575 . . . ? C2 Zr Si C21 114.5(3) . . . . ? C12 Zr Si C21 -121.8(3) 7_575 . . . ? C12 Zr Si C21 -59.0(2) . . . . ? C13 Zr Si C21 -74.6(2) . . . . ? C13 Zr Si C21 -106.2(3) 7_575 . . . ? C11 Si N C31 180.000(1) . . . . ? C21 Si N C31 -62.2(2) 7_575 . . . ? C21 Si N C31 62.2(2) . . . . ? Zr Si N C31 180.000(2) . . . . ? C11 Si N Zr 0.0 . . . . ? C21 Si N Zr 117.8(2) 7_575 . . . ? C21 Si N Zr -117.8(2) . . . . ? C1 Zr N C31 -51.65(19) 7_575 . . . ? C1 Zr N C31 51.65(19) . . . . ? C11 Zr N C31 180.000(2) . . . . ? C2 Zr N C31 -16.78(14) 7_575 . . . ? C2 Zr N C31 16.78(14) . . . . ? C12 Zr N C31 152.37(10) 7_575 . . . ? C12 Zr N C31 -152.37(10) . . . . ? C13 Zr N C31 -160.95(13) . . . . ? C13 Zr N C31 160.95(13) 7_575 . . . ? Si Zr N C31 180.000(2) . . . . ? C1 Zr N Si 128.35(19) 7_575 . . . ? C1 Zr N Si -128.35(19) . . . . ? C11 Zr N Si 0.0 . . . . ? C2 Zr N Si 163.22(14) 7_575 . . . ? C2 Zr N Si -163.22(14) . . . . ? C12 Zr N Si -27.63(10) 7_575 . . . ? C12 Zr N Si 27.63(10) . . . . ? C13 Zr N Si 19.05(13) . . . . ? C13 Zr N Si -19.05(13) 7_575 . . . ? N Zr C2 C2 -95.26(7) . . . 7_575 ? C1 Zr C2 C2 23.3(2) 7_575 . . 7_575 ? C1 Zr C2 C2 142.0(4) . . . 7_575 ? C11 Zr C2 C2 -179.5(7) . . . 7_575 ? C12 Zr C2 C2 155.0(2) 7_575 . . 7_575 ? C12 Zr C2 C2 55.3(4) . . . 7_575 ? C13 Zr C2 C2 82.31(17) . . . 7_575 ? C13 Zr C2 C2 118.54(15) 7_575 . . 7_575 ? Si Zr C2 C2 -109.33(17) . . . 7_575 ? N Zr C2 C1 122.7(4) . . . . ? C1 Zr C2 C1 -118.8(6) 7_575 . . . ? C11 Zr C2 C1 38.5(9) . . . . ? C2 Zr C2 C1 -142.0(4) 7_575 . . . ? C12 Zr C2 C1 13.0(5) 7_575 . . . ? C12 Zr C2 C1 -86.8(6) . . . . ? C13 Zr C2 C1 -59.7(5) . . . . ? C13 Zr C2 C1 -23.5(5) 7_575 . . . ? Si Zr C2 C1 108.6(4) . . . . ? C2 C2 C1 Zr -46.9(3) 7_575 . . . ? N Zr C1 C2 -72.8(4) . . . . ? C1 Zr C1 C2 51.7(5) 7_575 . . . ? C11 Zr C1 C2 -166.7(3) . . . . ? C2 Zr C1 C2 21.5(3) 7_575 . . . ? C12 Zr C1 C2 -170.3(4) 7_575 . . . ? C12 Zr C1 C2 145.0(3) . . . . ? C13 Zr C1 C2 135.3(4) . . . . ? C13 Zr C1 C2 159.4(4) 7_575 . . . ? Si Zr C1 C2 -112.7(4) . . . . ? N Si C11 C12 -72.3(4) . . . . ? C21 Si C11 C12 166.2(4) 7_575 . . . ? C21 Si C11 C12 49.2(5) . . . . ? Zr Si C11 C12 -72.3(4) . . . . ? N Si C11 C12 72.3(4) . . . 7_575 ? C21 Si C11 C12 -49.2(5) 7_575 . . 7_575 ? C21 Si C11 C12 -166.2(4) . . . 7_575 ? Zr Si C11 C12 72.3(4) . . . 7_575 ? N Si C11 Zr 0.0 . . . . ? C21 Si C11 Zr -121.5(2) 7_575 . . . ? C21 Si C11 Zr 121.5(2) . . . . ? N Zr C11 C12 124.3(2) . . . . ? C1 Zr C11 C12 6.3(4) 7_575 . . . ? C1 Zr C11 C12 -117.8(3) . . . . ? C2 Zr C11 C12 34.8(9) 7_575 . . . ? C2 Zr C11 C12 -146.2(6) . . . . ? C12 Zr C11 C12 -111.4(5) 7_575 . . . ? C13 Zr C11 C12 -36.3(3) . . . . ? C13 Zr C11 C12 -75.1(3) 7_575 . . . ? Si Zr C11 C12 124.3(2) . . . . ? N Zr C11 C12 -124.3(2) . . . 7_575 ? C1 Zr C11 C12 117.8(3) 7_575 . . 7_575 ? C1 Zr C11 C12 -6.3(4) . . . 7_575 ? C2 Zr C11 C12 146.2(6) 7_575 . . 7_575 ? C2 Zr C11 C12 -34.8(9) . . . 7_575 ? C12 Zr C11 C12 111.4(5) . . . 7_575 ? C13 Zr C11 C12 75.1(3) . . . 7_575 ? C13 Zr C11 C12 36.3(3) 7_575 . . 7_575 ? Si Zr C11 C12 -124.3(2) . . . 7_575 ? N Zr C11 Si 0.0 . . . . ? C1 Zr C11 Si -117.9(3) 7_575 . . . ? C1 Zr C11 Si 117.9(3) . . . . ? C2 Zr C11 Si -89.5(7) 7_575 . . . ? C2 Zr C11 Si 89.5(7) . . . . ? C12 Zr C11 Si 124.3(2) 7_575 . . . ? C12 Zr C11 Si -124.3(2) . . . . ? C13 Zr C11 Si -160.59(13) . . . . ? C13 Zr C11 Si 160.59(13) 7_575 . . . ? C12 C11 C12 C13 -0.5(6) 7_575 . . . ? Si C11 C12 C13 149.1(4) . . . . ? Zr C11 C12 C13 69.1(3) . . . . ? C12 C11 C12 C121 178.9(3) 7_575 . . . ? Si C11 C12 C121 -31.5(7) . . . . ? Zr C11 C12 C121 -111.4(5) . . . . ? C12 C11 C12 Zr -69.7(4) 7_575 . . . ? Si C11 C12 Zr 80.0(4) . . . . ? N Zr C12 C13 -166.6(3) . . . . ? C1 Zr C12 C13 69.8(3) 7_575 . . . ? C1 Zr C12 C13 -17.5(4) . . . . ? C11 Zr C12 C13 -115.0(4) . . . . ? C2 Zr C12 C13 77.2(3) 7_575 . . . ? C2 Zr C12 C13 41.4(5) . . . . ? C12 Zr C12 C13 -75.5(3) 7_575 . . . ? C13 Zr C12 C13 -35.5(3) 7_575 . . . ? Si Zr C12 C13 -149.9(3) . . . . ? N Zr C12 C11 -51.6(3) . . . . ? C1 Zr C12 C11 -175.2(3) 7_575 . . . ? C1 Zr C12 C11 97.5(4) . . . . ? C2 Zr C12 C11 -167.8(3) 7_575 . . . ? C2 Zr C12 C11 156.4(4) . . . . ? C12 Zr C12 C11 39.5(3) 7_575 . . . ? C13 Zr C12 C11 115.0(4) . . . . ? C13 Zr C12 C11 79.5(3) 7_575 . . . ? Si Zr C12 C11 -34.9(2) . . . . ? N Zr C12 C121 70.7(3) . . . . ? C1 Zr C12 C121 -53.0(4) 7_575 . . . ? C1 Zr C12 C121 -140.2(4) . . . . ? C11 Zr C12 C121 122.2(4) . . . . ? C2 Zr C12 C121 -45.6(4) 7_575 . . . ? C2 Zr C12 C121 -81.4(5) . . . . ? C12 Zr C12 C121 161.7(3) 7_575 . . . ? C13 Zr C12 C121 -122.8(5) . . . . ? C13 Zr C12 C121 -158.2(4) 7_575 . . . ? Si Zr C12 C121 87.4(3) . . . . ? C11 C12 C13 C13 0.3(4) . . . 7_575 ? C121 C12 C13 C13 -179.1(3) . . . 7_575 ? Zr C12 C13 C13 64.68(11) . . . 7_575 ? C11 C12 C13 C131 175.4(4) . . . . ? C121 C12 C13 C131 -4.0(7) . . . . ? Zr C12 C13 C131 -120.2(4) . . . . ? C11 C12 C13 Zr -64.4(3) . . . . ? C121 C12 C13 Zr 116.2(4) . . . . ? N Zr C13 C13 -100.75(9) . . . 7_575 ? C1 Zr C13 C13 131.8(2) 7_575 . . 7_575 ? C1 Zr C13 C13 51.05(18) . . . 7_575 ? C11 Zr C13 C13 -78.60(10) . . . 7_575 ? C2 Zr C13 C13 118.61(17) 7_575 . . 7_575 ? C2 Zr C13 C13 82.02(19) . . . 7_575 ? C12 Zr C13 C13 -36.34(15) 7_575 . . 7_575 ? C12 Zr C13 C13 -116.9(2) . . . 7_575 ? Si Zr C13 C13 -90.40(3) . . . 7_575 ? N Zr C13 C12 16.2(3) . . . . ? C1 Zr C13 C12 -111.3(3) 7_575 . . . ? C1 Zr C13 C12 168.0(3) . . . . ? C11 Zr C13 C12 38.3(2) . . . . ? C2 Zr C13 C12 -124.5(3) 7_575 . . . ? C2 Zr C13 C12 -161.1(3) . . . . ? C12 Zr C13 C12 80.6(3) 7_575 . . . ? C13 Zr C13 C12 116.9(2) 7_575 . . . ? Si Zr C13 C12 26.5(2) . . . . ? N Zr C13 C131 136.6(4) . . . . ? C1 Zr C13 C131 9.1(4) 7_575 . . . ? C1 Zr C13 C131 -71.6(4) . . . . ? C11 Zr C13 C131 158.7(5) . . . . ? C2 Zr C13 C131 -4.1(5) 7_575 . . . ? C2 Zr C13 C131 -40.7(5) . . . . ? C12 Zr C13 C131 -159.0(5) 7_575 . . . ? C12 Zr C13 C131 120.4(5) . . . . ? C13 Zr C13 C131 -122.7(4) 7_575 . . . ? Si Zr C13 C131 146.9(4) . . . . ? Si N C31 C32 103.6(4) . . . 7_575 ? Zr N C31 C32 -76.4(4) . . . 7_575 ? Si N C31 C32 -103.6(4) . . . . ? Zr N C31 C32 76.4(4) . . . . ? Si N C31 C33 21.1(3) . . . . ? Zr N C31 C33 -158.9(3) . . . . ? Si N C31 C33 -21.1(3) . . . 7_575 ? Zr N C31 C33 158.9(3) . . . 7_575 ? Si N C31 C34 -136.8(4) . . . 7_575 ? Zr N C31 C34 43.2(4) . . . 7_575 ? Si N C31 C34 136.8(4) . . . . ? Zr N C31 C34 -43.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.711 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.090 data_erk_903 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H33 N Si Ti' _chemical_formula_weight 351.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pnma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.496(4) _cell_length_b 12.629(2) _cell_length_c 15.201(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2015.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17 _cell_measurement_theta_min 18.43 _cell_measurement_theta_max 20.58 _exptl_crystal_description 'block' _exptl_crystal_colour 'red-black' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type 'empirical via \y scan data' _exptl_absorpt_correction_T_min 0.8305 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius MACH3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4.0 _diffrn_reflns_number 2127 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.29 _reflns_number_total 2127 _reflns_number_gt 1310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Express (Nonius B.V., 1994)' _computing_cell_refinement 'Express (Nonius B.V., 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Tert.-butyl group disordered (50:50). ; _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^)+(0.1274P)^2^+0.0083P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2127 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Ti Ti 0.07616(10) 0.2500 0.06523(7) 0.0350(4) Uani 1 2 d S . . Si Si 0.32106(18) 0.2500 -0.01808(11) 0.0426(5) Uani 1 2 d S . . C11 C 0.2825(6) 0.2500 0.1014(4) 0.0338(13) Uani 1 2 d S . . N N 0.1622(6) 0.2500 -0.0509(3) 0.0459(14) Uani 1 2 d S . . C12 C 0.2292(4) 0.3409(3) 0.1457(3) 0.0373(10) Uani 1 1 d . . . C13 C 0.1479(4) 0.3067(3) 0.2128(3) 0.0404(10) Uani 1 1 d . . . C31 C 0.1232(8) 0.2500 -0.1455(4) 0.0519(18) Uani 1 2 d S . . C121 C 0.2578(5) 0.4562(3) 0.1261(3) 0.0535(13) Uani 1 1 d . . . H12A H 0.1955 0.5008 0.1553 0.080 Uiso 1 1 d R . . H12B H 0.2538 0.4681 0.0631 0.080 Uiso 1 1 d R . . H12C H 0.3424 0.4736 0.1474 0.080 Uiso 1 1 d R . . C131 C 0.0821(5) 0.3751(5) 0.2795(3) 0.0678(16) Uani 1 1 d . . . H13A H 0.1404 0.3908 0.3273 0.102 Uiso 1 1 d R . . H13B H 0.0082 0.3381 0.3024 0.102 Uiso 1 1 d R . . H13C H 0.0551 0.4406 0.2519 0.102 Uiso 1 1 d R . . C21 C 0.4207(6) 0.3669(6) -0.0515(4) 0.088(2) Uani 1 1 d . . . H21A H 0.4488 0.3581 -0.1118 0.132 Uiso 1 1 d R . . H21B H 0.4944 0.3720 -0.0131 0.132 Uiso 1 1 d R . . H21C H 0.3705 0.4311 -0.0466 0.132 Uiso 1 1 d R . . C1 C -0.0743(6) 0.3672(6) 0.0483(6) 0.101(3) Uani 1 1 d . . . H1B H -0.0517 0.4403 0.0633 0.121 Uiso 1 1 d R . . H1A H -0.1238 0.3619 -0.0062 0.121 Uiso 1 1 d R . . C2 C -0.1147(6) 0.3055(8) 0.1163(5) 0.136(5) Uani 1 1 d . . . H2 H -0.1449 0.3400 0.1670 0.163 Uiso 1 1 d R . . C32 C -0.0045(12) 0.1837(10) -0.1584(7) 0.072(3) Uani 0.50 1 d P . . H32A H -0.0213 0.1749 -0.2207 0.108 Uiso 0.50 1 d PR . . H32B H -0.0750 0.2212 -0.1312 0.108 Uiso 0.50 1 d PR . . H32C H 0.0049 0.1148 -0.1311 0.108 Uiso 0.50 1 d PR . . C33 C 0.1107(14) 0.3534(9) -0.1763(8) 0.079(4) Uani 0.50 1 d P . . H33A H 0.0682 0.3527 -0.2330 0.118 Uiso 0.50 1 d PR . . H33B H 0.1945 0.3850 -0.1826 0.118 Uiso 0.50 1 d PR . . H33C H 0.0608 0.3945 -0.1348 0.118 Uiso 0.50 1 d PR . . C34 C 0.2262(15) 0.1837(11) -0.2025(7) 0.089(4) Uani 0.50 1 d P . . H34A H 0.2363 0.1137 -0.1773 0.134 Uiso 0.50 1 d PR . . H34B H 0.3074 0.2204 -0.2017 0.134 Uiso 0.50 1 d PR . . H34C H 0.1965 0.1775 -0.2627 0.134 Uiso 0.50 1 d 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 Ti 0.0340(6) 0.0397(6) 0.0314(6) 0.000 -0.0036(5) 0.000 Si 0.0428(11) 0.0504(11) 0.0347(9) 0.000 0.0055(8) 0.000 C11 0.035(3) 0.036(3) 0.031(3) 0.000 -0.002(3) 0.000 N 0.051(3) 0.056(3) 0.031(3) 0.000 -0.006(2) 0.000 C12 0.041(2) 0.034(2) 0.037(2) -0.0026(18) -0.005(2) 0.0030(19) C13 0.037(2) 0.050(2) 0.035(2) -0.0061(19) 0.0024(19) 0.005(2) C31 0.071(5) 0.059(4) 0.026(3) 0.000 0.000(3) 0.000 C121 0.060(3) 0.036(2) 0.064(3) -0.001(2) -0.009(3) 0.000(2) C131 0.061(3) 0.092(4) 0.051(3) -0.021(3) -0.001(3) 0.018(3) C21 0.096(5) 0.108(5) 0.060(4) 0.008(3) 0.018(3) -0.043(4) C1 0.067(4) 0.105(6) 0.132(7) -0.042(5) -0.044(5) 0.046(4) C2 0.055(4) 0.269(16) 0.083(5) -0.076(7) -0.009(4) 0.042(6) C32 0.082(9) 0.089(8) 0.044(6) 0.005(6) -0.028(6) -0.012(7) C33 0.121(12) 0.065(7) 0.050(6) 0.028(6) -0.034(8) -0.012(8) C34 0.107(10) 0.121(11) 0.040(6) -0.020(7) 0.003(7) 0.009(9) _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 Ti N 1.983(5) . ? Ti C1 2.180(6) 7_565 ? Ti C1 2.180(6) . ? Ti C11 2.234(6) . ? Ti C2 2.260(7) 7_565 ? Ti C2 2.260(7) . ? Ti C12 2.323(4) . ? Ti C12 2.323(4) 7_565 ? Ti C13 2.472(4) . ? Ti C13 2.472(4) 7_565 ? Ti Si 2.866(2) . ? Si N 1.740(6) . ? Si C11 1.860(6) . ? Si C21 1.880(6) . ? Si C21 1.880(6) 7_565 ? C11 C12 1.444(5) . ? C11 C12 1.444(5) 7_565 ? N C31 1.496(7) . ? C12 C13 1.398(6) . ? C12 C121 1.517(6) . ? C13 C13 1.431(9) 7_565 ? C13 C131 1.500(6) . ? C31 C33 1.393(11) 7_565 ? C31 C33 1.393(11) . ? C31 C32 1.592(13) . ? C31 C32 1.592(13) 7_565 ? C31 C34 1.618(14) 7_565 ? C31 C34 1.618(14) . ? C1 C2 1.361(11) . ? C2 C2 1.40(2) 7_565 ? 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 N Ti C1 103.0(3) . 7_565 ? N Ti C1 103.0(3) . . ? C1 Ti C1 85.5(4) 7_565 . ? N Ti C11 77.1(2) . . ? C1 Ti C11 137.0(2) 7_565 . ? C1 Ti C11 137.0(2) . . ? N Ti C2 135.2(3) . 7_565 ? C1 Ti C2 35.7(3) 7_565 7_565 ? C1 Ti C2 67.0(4) . 7_565 ? C11 Ti C2 140.8(2) . 7_565 ? N Ti C2 135.2(3) . . ? C1 Ti C2 67.0(4) 7_565 . ? C1 Ti C2 35.7(3) . . ? C11 Ti C2 140.8(2) . . ? C2 Ti C2 36.2(5) 7_565 . ? N Ti C12 98.86(18) . . ? C1 Ti C12 154.0(2) 7_565 . ? C1 Ti C12 103.2(2) . . ? C11 Ti C12 36.89(13) . . ? C2 Ti C12 125.8(3) 7_565 . ? C2 Ti C12 106.2(2) . . ? N Ti C12 98.86(18) . 7_565 ? C1 Ti C12 103.2(2) 7_565 7_565 ? C1 Ti C12 154.0(2) . 7_565 ? C11 Ti C12 36.89(13) . 7_565 ? C2 Ti C12 106.2(2) 7_565 7_565 ? C2 Ti C12 125.8(3) . 7_565 ? C12 Ti C12 59.2(2) . 7_565 ? N Ti C13 132.00(18) . . ? C1 Ti C13 121.6(2) 7_565 . ? C1 Ti C13 97.5(2) . . ? C11 Ti C13 58.78(16) . . ? C2 Ti C13 92.8(2) 7_565 . ? C2 Ti C13 82.5(2) . . ? C12 Ti C13 33.72(14) . . ? C12 Ti C13 56.93(14) 7_565 . ? N Ti C13 132.00(18) . 7_565 ? C1 Ti C13 97.5(2) 7_565 7_565 ? C1 Ti C13 121.6(2) . 7_565 ? C11 Ti C13 58.78(16) . 7_565 ? C2 Ti C13 82.5(2) 7_565 7_565 ? C2 Ti C13 92.8(2) . 7_565 ? C12 Ti C13 56.93(14) . 7_565 ? C12 Ti C13 33.72(14) 7_565 7_565 ? C13 Ti C13 33.7(2) . 7_565 ? N Ti Si 36.67(17) . . ? C1 Ti Si 126.7(2) 7_565 . ? C1 Ti Si 126.7(2) . . ? C11 Ti Si 40.46(15) . . ? C2 Ti Si 161.2(3) 7_565 . ? C2 Ti Si 161.2(3) . . ? C12 Ti Si 67.21(11) . . ? C12 Ti Si 67.21(11) 7_565 . ? C13 Ti Si 97.35(11) . . ? C13 Ti Si 97.35(11) 7_565 . ? N Si C11 94.1(3) . . ? N Si C21 117.1(2) . . ? C11 Si C21 112.6(2) . . ? N Si C21 117.1(2) . 7_565 ? C11 Si C21 112.6(2) . 7_565 ? C21 Si C21 103.6(5) . 7_565 ? N Si Ti 42.88(17) . . ? C11 Si Ti 51.20(19) . . ? C21 Si Ti 128.2(2) . . ? C21 Si Ti 128.2(2) 7_565 . ? C12 C11 C12 105.3(5) . 7_565 ? C12 C11 Si 122.7(3) . . ? C12 C11 Si 122.7(3) 7_565 . ? C12 C11 Ti 74.9(3) . . ? C12 C11 Ti 74.9(3) 7_565 . ? Si C11 Ti 88.3(2) . . ? C31 N Si 122.5(5) . . ? C31 N Ti 137.0(5) . . ? Si N Ti 100.5(2) . . ? C13 C12 C11 109.3(4) . . ? C13 C12 C121 124.1(4) . . ? C11 C12 C121 126.5(4) . . ? C13 C12 Ti 79.0(3) . . ? C11 C12 Ti 68.2(3) . . ? C121 C12 Ti 120.5(3) . . ? C12 C13 C13 108.0(2) . 7_565 ? C12 C13 C131 126.5(4) . . ? C13 C13 C131 125.2(3) 7_565 . ? C12 C13 Ti 67.3(2) . . ? C13 C13 Ti 73.17(10) 7_565 . ? C131 C13 Ti 129.8(3) . . ? C33 C31 C33 139.1(11) 7_565 . ? C33 C31 N 110.4(5) 7_565 . ? C33 C31 N 110.4(5) . . ? C33 C31 C32 52.2(7) 7_565 . ? C33 C31 C32 111.8(10) . . ? N C31 C32 110.4(5) . . ? C33 C31 C32 111.8(10) 7_565 7_565 ? C33 C31 C32 52.2(7) . 7_565 ? N C31 C32 110.4(5) . 7_565 ? C32 C31 C32 63.4(10) . 7_565 ? C33 C31 C34 111.6(10) 7_565 7_565 ? C33 C31 C34 53.0(7) . 7_565 ? N C31 C34 109.4(6) . 7_565 ? C32 C31 C34 140.2(7) . 7_565 ? C32 C31 C34 103.0(8) 7_565 7_565 ? C33 C31 C34 53.0(7) 7_565 . ? C33 C31 C34 111.6(10) . . ? N C31 C34 109.4(7) . . ? C32 C31 C34 103.0(8) . . ? C32 C31 C34 140.2(7) 7_565 . ? C34 C31 C34 62.3(11) 7_565 . ? C2 C1 Ti 75.4(5) . . ? C1 C2 C2 124.9(5) . 7_565 ? C1 C2 Ti 68.9(4) . . ? C2 C2 Ti 71.9(3) 7_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.425 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.085 data_erk1099 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H35 N Si Zr' _chemical_formula_weight 492.87 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 'P212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.567(1) _cell_length_b 16.693(1) _cell_length_c 17.164(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2454.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.45 _cell_measurement_theta_max 21.82 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type 'empirical via \y scan data' _exptl_absorpt_correction_T_min 0.8219 _exptl_absorpt_correction_T_max 0.8830 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius MACH3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5.7 _diffrn_reflns_number 2833 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.31 _reflns_number_total 2833 _reflns_number_gt 2615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Express (Nonius B.V., 1994)' _computing_cell_refinement 'Express (Nonius B.V., 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.1865P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(4) _refine_ls_number_reflns 2833 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Zr Zr 0.70487(3) 0.139700(15) 0.844403(14) 0.02099(8) Uani 1 1 d . . . Si Si 0.68194(9) 0.03738(4) 0.69787(4) 0.02312(16) Uani 1 1 d . . . N N 0.5592(3) 0.07845(14) 0.76736(13) 0.0222(5) Uani 1 1 d . . . C1 C 0.6658(4) 0.1233(3) 0.97609(18) 0.0468(10) Uani 1 1 d . . . H1A H 0.7640 0.1422 0.9601 0.056 Uiso 1 1 calc R . . H1B H 0.6586 0.0774 1.0076 0.056 Uiso 1 1 calc R . . C2 C 0.5259(4) 0.1647(2) 0.95224(18) 0.0397(8) Uani 1 1 d . . . H2 H 0.4297 0.1441 0.9693 0.048 Uiso 1 1 calc R . . C3 C 0.5232(4) 0.2323(2) 0.9063(2) 0.0413(8) Uani 1 1 d . . . H3 H 0.4250 0.2544 0.8946 0.050 Uiso 1 1 calc R . . C4 C 0.6575(5) 0.2716(2) 0.8749(2) 0.0480(9) Uani 1 1 d . . . H4A H 0.7578 0.2514 0.8852 0.058 Uiso 1 1 calc R . . H4B H 0.6454 0.3177 0.8439 0.058 Uiso 1 1 calc R . . C5 C 0.8646(3) 0.07460(18) 0.74616(16) 0.0236(6) Uani 1 1 d . . . C6 C 0.9174(3) 0.04364(17) 0.82003(17) 0.0266(6) Uani 1 1 d . . . C7 C 0.9903(3) 0.10512(19) 0.86207(17) 0.0307(7) Uani 1 1 d . . . C8 C 0.9865(3) 0.17550(18) 0.81566(18) 0.0302(6) Uani 1 1 d . . . C9 C 0.9113(3) 0.15694(17) 0.74491(17) 0.0278(6) Uani 1 1 d . . . C10 C 0.8975(4) -0.04138(18) 0.8492(2) 0.0387(7) Uani 1 1 d . . . H10A H 0.9490 -0.0471 0.8992 0.058 Uiso 1 1 calc R . . H10B H 0.9436 -0.0783 0.8121 0.058 Uiso 1 1 calc R . . H10C H 0.7873 -0.0532 0.8549 0.058 Uiso 1 1 calc R . . C11 C 1.0688(4) 0.0990(2) 0.9402(2) 0.0424(8) Uani 1 1 d . . . H11A H 1.0208 0.0563 0.9702 0.064 Uiso 1 1 calc R . . H11B H 1.0573 0.1493 0.9679 0.064 Uiso 1 1 calc R . . H11C H 1.1788 0.0875 0.9330 0.064 Uiso 1 1 calc R . . C12 C 1.0624(4) 0.2552(2) 0.8351(2) 0.0450(8) Uani 1 1 d . . . H12A H 1.0796 0.2585 0.8909 0.067 Uiso 1 1 calc R . . H12B H 0.9945 0.2985 0.8188 0.067 Uiso 1 1 calc R . . H12C H 1.1616 0.2594 0.8081 0.067 Uiso 1 1 calc R . . C13 C 0.8878(5) 0.2157(2) 0.6792(2) 0.0421(8) Uani 1 1 d . . . H13A H 0.9200 0.1913 0.6305 0.063 Uiso 1 1 calc R . . H13B H 0.9499 0.2633 0.6887 0.063 Uiso 1 1 calc R . . H13C H 0.7784 0.2304 0.6761 0.063 Uiso 1 1 calc R . . C14 C 0.6716(4) -0.07363(18) 0.6867(2) 0.0380(7) Uani 1 1 d . . . H14A H 0.6588 -0.0982 0.7375 0.057 Uiso 1 1 calc R . . H14B H 0.7672 -0.0929 0.6629 0.057 Uiso 1 1 calc R . . H14C H 0.5835 -0.0875 0.6539 0.057 Uiso 1 1 calc R . . C15 C 0.6571(4) 0.0748(2) 0.59606(17) 0.0362(7) Uani 1 1 d . . . H15A H 0.5710 0.0469 0.5714 0.054 Uiso 1 1 calc R . . H15B H 0.7522 0.0652 0.5668 0.054 Uiso 1 1 calc R . . H15C H 0.6354 0.1318 0.5971 0.054 Uiso 1 1 calc R . . C16 C 0.3894(3) 0.06579(18) 0.77519(16) 0.0254(6) Uani 1 1 d . . . H16 H 0.3480 0.1115 0.8055 0.030 Uiso 1 1 calc R . . C17 C 0.3587(4) -0.0094(2) 0.8230(2) 0.0420(8) Uani 1 1 d . . . H17A H 0.3996 -0.0557 0.7955 0.063 Uiso 1 1 calc R . . H17B H 0.2472 -0.0158 0.8306 0.063 Uiso 1 1 calc R . . H17C H 0.4099 -0.0047 0.8732 0.063 Uiso 1 1 calc R . . C18 C 0.3062(4) 0.06660(18) 0.69677(17) 0.0309(6) Uani 1 1 d . . . C19 C 0.2335(4) -0.0006(2) 0.6683(2) 0.0469(9) Uani 1 1 d . . . H19 H 0.2323 -0.0476 0.6984 0.056 Uiso 1 1 calc R . . C20 C 0.1602(5) -0.0001(3) 0.5941(3) 0.0714(16) Uani 1 1 d . . . H20 H 0.1119 -0.0468 0.5752 0.086 Uiso 1 1 calc R . . C21 C 0.1598(5) 0.0669(4) 0.5507(3) 0.0687(15) Uani 1 1 d . . . H21 H 0.1100 0.0665 0.5019 0.082 Uiso 1 1 calc R . . C22 C 0.2318(4) 0.1373(3) 0.57663(19) 0.0527(10) Uani 1 1 d . . . C23 C 0.2359(6) 0.2090(3) 0.5313(2) 0.0717(15) Uani 1 1 d . . . H23 H 0.1882 0.2093 0.4820 0.086 Uiso 1 1 calc R . . C24 C 0.3064(7) 0.2765(3) 0.5571(2) 0.0772(16) Uani 1 1 d . . . H24 H 0.3089 0.3226 0.5256 0.093 Uiso 1 1 calc R . . C25 C 0.3752(6) 0.2774(2) 0.6307(2) 0.0562(11) Uani 1 1 d . . . H25 H 0.4230 0.3245 0.6489 0.067 Uiso 1 1 calc R . . C26 C 0.3739(4) 0.2106(2) 0.67667(19) 0.0388(8) Uani 1 1 d . . . H26 H 0.4202 0.2128 0.7263 0.047 Uiso 1 1 calc R . . C27 C 0.3044(3) 0.1379(2) 0.65148(16) 0.0361(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01899(12) 0.02455(12) 0.01942(12) -0.00258(10) 0.00079(11) 0.00061(11) Si 0.0239(4) 0.0246(3) 0.0209(3) -0.0035(3) 0.0007(3) 0.0001(3) N 0.0172(11) 0.0271(11) 0.0224(11) -0.0015(10) -0.0018(9) 0.0002(10) C1 0.0379(18) 0.080(3) 0.0225(14) 0.0104(16) 0.0066(13) 0.0098(18) C2 0.0301(15) 0.064(2) 0.0247(14) -0.0076(15) 0.0087(13) 0.0015(16) C3 0.0344(17) 0.0452(18) 0.0443(18) -0.0182(16) 0.0051(15) 0.0114(15) C4 0.0417(19) 0.0305(16) 0.072(2) -0.0054(17) 0.0130(18) 0.0063(15) C5 0.0201(13) 0.0279(14) 0.0228(13) -0.0020(11) 0.0059(11) 0.0002(12) C6 0.0196(12) 0.0281(14) 0.0321(14) -0.0005(11) 0.0001(11) 0.0028(11) C7 0.0193(13) 0.0423(16) 0.0304(15) -0.0080(13) -0.0002(11) 0.0001(12) C8 0.0210(13) 0.0353(15) 0.0343(15) -0.0072(14) 0.0042(12) -0.0058(13) C9 0.0213(13) 0.0328(16) 0.0293(14) -0.0010(11) 0.0072(11) -0.0019(12) C10 0.0368(16) 0.0339(15) 0.0455(18) 0.0060(15) -0.0077(17) 0.0033(13) C11 0.0321(17) 0.058(2) 0.0366(17) -0.0077(16) -0.0093(14) 0.0036(17) C12 0.0340(17) 0.0449(18) 0.056(2) -0.0140(18) 0.0019(17) -0.0154(15) C13 0.047(2) 0.0383(17) 0.0406(18) 0.0088(14) 0.0080(16) -0.0052(16) C14 0.0406(19) 0.0317(15) 0.0417(16) -0.0079(13) -0.0005(15) -0.0020(14) C15 0.0404(18) 0.0451(18) 0.0232(13) -0.0027(13) 0.0024(13) 0.0018(15) C16 0.0184(13) 0.0320(14) 0.0258(14) -0.0029(12) 0.0006(11) 0.0017(12) C17 0.0310(16) 0.0454(19) 0.050(2) 0.0083(16) 0.0069(15) -0.0032(15) C18 0.0212(13) 0.0410(15) 0.0304(14) -0.0113(12) -0.0033(14) 0.0057(14) C19 0.0332(17) 0.053(2) 0.055(2) -0.0225(17) -0.0047(16) 0.0006(15) C20 0.051(3) 0.087(4) 0.076(3) -0.050(3) -0.026(2) 0.003(3) C21 0.052(3) 0.110(4) 0.044(2) -0.035(3) -0.0230(19) 0.024(3) C22 0.049(2) 0.082(3) 0.0272(15) -0.0104(18) -0.0098(15) 0.027(2) C23 0.076(3) 0.109(4) 0.0299(18) 0.004(2) -0.016(2) 0.034(3) C24 0.101(4) 0.089(3) 0.042(2) 0.025(2) 0.002(3) 0.039(4) C25 0.071(3) 0.048(2) 0.049(2) 0.0073(17) 0.004(2) 0.017(2) C26 0.0436(19) 0.0424(18) 0.0303(16) 0.0005(13) -0.0007(14) 0.0150(16) C27 0.0301(13) 0.0532(17) 0.0249(13) -0.0096(14) -0.0051(13) 0.0166(16) _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 N 2.086(2) . ? Zr C4 2.300(3) . ? Zr C1 2.301(3) . ? Zr C5 2.428(3) . ? Zr C3 2.437(3) . ? Zr C2 2.440(3) . ? Zr C6 2.462(3) . ? Zr C9 2.475(3) . ? Zr C7 2.530(3) . ? Zr C8 2.534(3) . ? Zr Si 3.0466(8) . ? Si N 1.731(2) . ? Si C14 1.865(3) . ? Si C15 1.868(3) . ? Si C5 1.876(3) . ? N C16 1.477(4) . ? C1 C2 1.443(5) . ? C2 C3 1.376(5) . ? C3 C4 1.431(5) . ? C5 C9 1.432(4) . ? C5 C6 1.442(4) . ? C6 C7 1.401(4) . ? C6 C10 1.515(4) . ? C7 C8 1.420(5) . ? C7 C11 1.504(4) . ? C8 C9 1.409(4) . ? C8 C12 1.517(4) . ? C9 C13 1.509(4) . ? C16 C17 1.522(4) . ? C16 C18 1.523(4) . ? C18 C19 1.372(5) . ? C18 C27 1.422(5) . ? C19 C20 1.421(5) . ? C20 C21 1.343(7) . ? C21 C22 1.400(7) . ? C22 C27 1.427(4) . ? C22 C23 1.428(7) . ? C23 C24 1.352(7) . ? C24 C25 1.394(6) . ? C25 C26 1.366(5) . ? C26 C27 1.418(5) . ? 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 N Zr C4 120.53(13) . . ? N Zr C1 118.51(12) . . ? C4 Zr C1 82.23(15) . . ? N Zr C5 71.18(9) . . ? C4 Zr C5 133.32(12) . . ? C1 Zr C5 135.30(12) . . ? N Zr C3 101.84(11) . . ? C4 Zr C3 35.00(13) . . ? C1 Zr C3 63.52(13) . . ? C5 Zr C3 161.16(11) . . ? N Zr C2 100.89(11) . . ? C4 Zr C2 63.41(13) . . ? C1 Zr C2 35.28(12) . . ? C5 Zr C2 163.26(11) . . ? C3 Zr C2 32.78(12) . . ? N Zr C6 90.88(9) . . ? C4 Zr C6 142.46(12) . . ? C1 Zr C6 101.36(11) . . ? C5 Zr C6 34.29(10) . . ? C3 Zr C6 163.61(11) . . ? C2 Zr C6 134.85(11) . . ? N Zr C9 92.69(9) . . ? C4 Zr C9 99.89(12) . . ? C1 Zr C9 142.70(11) . . ? C5 Zr C9 33.94(10) . . ? C3 Zr C9 133.11(12) . . ? C2 Zr C9 162.29(12) . . ? C6 Zr C9 55.26(10) . . ? N Zr C7 122.83(9) . . ? C4 Zr C7 111.21(12) . . ? C1 Zr C7 89.76(11) . . ? C5 Zr C7 55.72(9) . . ? C3 Zr C7 135.19(11) . . ? C2 Zr C7 123.74(10) . . ? C6 Zr C7 32.57(10) . . ? C9 Zr C7 54.47(10) . . ? N Zr C8 124.17(9) . . ? C4 Zr C8 89.23(12) . . ? C1 Zr C8 110.97(12) . . ? C5 Zr C8 55.52(10) . . ? C3 Zr C8 122.92(11) . . ? C2 Zr C8 134.89(11) . . ? C6 Zr C8 54.29(10) . . ? C9 Zr C8 32.65(10) . . ? C7 Zr C8 32.56(11) . . ? N Zr Si 33.20(6) . . ? C4 Zr Si 135.51(11) . . ? C1 Zr Si 137.28(11) . . ? C5 Zr Si 38.01(7) . . ? C3 Zr Si 132.39(9) . . ? C2 Zr Si 132.98(9) . . ? C6 Zr Si 62.76(7) . . ? C9 Zr Si 62.72(7) . . ? C7 Zr Si 91.91(7) . . ? C8 Zr Si 91.89(7) . . ? N Si C14 115.81(14) . . ? N Si C15 116.28(13) . . ? C14 Si C15 103.35(16) . . ? N Si C5 94.07(12) . . ? C14 Si C5 114.46(15) . . ? C15 Si C5 113.40(15) . . ? N Si Zr 41.28(8) . . ? C14 Si Zr 130.16(11) . . ? C15 Si Zr 126.30(11) . . ? C5 Si Zr 52.84(9) . . ? C16 N Si 127.19(19) . . ? C16 N Zr 127.01(18) . . ? Si N Zr 105.52(11) . . ? C2 C1 Zr 77.60(18) . . ? C3 C2 C1 124.7(3) . . ? C3 C2 Zr 73.52(18) . . ? C1 C2 Zr 67.12(17) . . ? C2 C3 C4 125.4(3) . . ? C2 C3 Zr 73.70(19) . . ? C4 C3 Zr 67.23(18) . . ? C3 C4 Zr 77.8(2) . . ? C9 C5 C6 105.6(3) . . ? C9 C5 Si 123.0(2) . . ? C6 C5 Si 122.1(2) . . ? C9 C5 Zr 74.82(16) . . ? C6 C5 Zr 74.13(16) . . ? Si C5 Zr 89.15(11) . . ? C7 C6 C5 109.3(3) . . ? C7 C6 C10 124.5(3) . . ? C5 C6 C10 126.2(3) . . ? C7 C6 Zr 76.41(17) . . ? C5 C6 Zr 71.58(15) . . ? C10 C6 Zr 118.1(2) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 C11 127.5(3) . . ? C8 C7 C11 124.5(3) . . ? C6 C7 Zr 71.03(16) . . ? C8 C7 Zr 73.87(17) . . ? C11 C7 Zr 123.7(2) . . ? C9 C8 C7 108.2(3) . . ? C9 C8 C12 125.3(3) . . ? C7 C8 C12 126.3(3) . . ? C9 C8 Zr 71.36(16) . . ? C7 C8 Zr 73.57(16) . . ? C12 C8 Zr 124.9(2) . . ? C8 C9 C5 109.0(3) . . ? C8 C9 C13 124.2(3) . . ? C5 C9 C13 126.8(3) . . ? C8 C9 Zr 75.98(17) . . ? C5 C9 Zr 71.24(16) . . ? C13 C9 Zr 119.8(2) . . ? N C16 C17 109.7(3) . . ? N C16 C18 112.3(2) . . ? C17 C16 C18 113.7(3) . . ? C19 C18 C27 119.0(3) . . ? C19 C18 C16 121.3(3) . . ? C27 C18 C16 119.7(3) . . ? C18 C19 C20 121.0(4) . . ? C21 C20 C19 120.2(4) . . ? C20 C21 C22 121.4(4) . . ? C21 C22 C27 119.0(4) . . ? C21 C22 C23 122.8(4) . . ? C27 C22 C23 118.2(4) . . ? C24 C23 C22 122.1(4) . . ? C23 C24 C25 119.6(4) . . ? C26 C25 C24 120.8(5) . . ? C25 C26 C27 121.7(3) . . ? C26 C27 C18 123.0(3) . . ? C26 C27 C22 117.6(3) . . ? C18 C27 C22 119.4(3) . . ? 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 C4 Zr Si N -76.61(18) . . . . ? C1 Zr Si N 68.27(18) . . . . ? C5 Zr Si N 176.69(16) . . . . ? C3 Zr Si N -27.40(18) . . . . ? C2 Zr Si N 17.73(17) . . . . ? C6 Zr Si N 144.92(15) . . . . ? C9 Zr Si N -152.18(15) . . . . ? C7 Zr Si N 159.99(14) . . . . ? C8 Zr Si N -167.43(14) . . . . ? N Zr Si C14 -84.38(19) . . . . ? C4 Zr Si C14 -161.0(2) . . . . ? C1 Zr Si C14 -16.1(2) . . . . ? C5 Zr Si C14 92.30(19) . . . . ? C3 Zr Si C14 -111.8(2) . . . . ? C2 Zr Si C14 -66.65(19) . . . . ? C6 Zr Si C14 60.54(17) . . . . ? C9 Zr Si C14 123.43(17) . . . . ? C7 Zr Si C14 75.61(17) . . . . ? C8 Zr Si C14 108.18(17) . . . . ? N Zr Si C15 89.78(18) . . . . ? C4 Zr Si C15 13.17(19) . . . . ? C1 Zr Si C15 158.05(18) . . . . ? C5 Zr Si C15 -93.54(18) . . . . ? C3 Zr Si C15 62.37(19) . . . . ? C2 Zr Si C15 107.51(18) . . . . ? C6 Zr Si C15 -125.30(16) . . . . ? C9 Zr Si C15 -62.41(16) . . . . ? C7 Zr Si C15 -110.23(16) . . . . ? C8 Zr Si C15 -77.66(16) . . . . ? N Zr Si C5 -176.69(16) . . . . ? C4 Zr Si C5 106.70(18) . . . . ? C1 Zr Si C5 -108.41(17) . . . . ? C3 Zr Si C5 155.91(17) . . . . ? C2 Zr Si C5 -158.95(16) . . . . ? C6 Zr Si C5 -31.76(13) . . . . ? C9 Zr Si C5 31.13(14) . . . . ? C7 Zr Si C5 -16.70(14) . . . . ? C8 Zr Si C5 15.88(13) . . . . ? C14 Si N C16 -51.9(3) . . . . ? C15 Si N C16 69.8(3) . . . . ? C5 Si N C16 -171.6(3) . . . . ? Zr Si N C16 -174.2(3) . . . . ? C14 Si N Zr 122.35(15) . . . . ? C15 Si N Zr -115.99(15) . . . . ? C5 Si N Zr 2.65(13) . . . . ? C4 Zr N C16 -58.1(3) . . . . ? C1 Zr N C16 40.0(3) . . . . ? C5 Zr N C16 172.1(3) . . . . ? C3 Zr N C16 -26.1(3) . . . . ? C2 Zr N C16 7.3(3) . . . . ? C6 Zr N C16 143.5(2) . . . . ? C9 Zr N C16 -161.2(2) . . . . ? C7 Zr N C16 150.2(2) . . . . ? C8 Zr N C16 -170.5(2) . . . . ? Si Zr N C16 174.2(3) . . . . ? C4 Zr N Si 127.67(14) . . . . ? C1 Zr N Si -134.18(14) . . . . ? C5 Zr N Si -2.15(10) . . . . ? C3 Zr N Si 159.68(13) . . . . ? C2 Zr N Si -166.88(13) . . . . ? C6 Zr N Si -30.73(13) . . . . ? C9 Zr N Si 24.53(13) . . . . ? C7 Zr N Si -24.02(17) . . . . ? C8 Zr N Si 15.24(17) . . . . ? N Zr C1 C2 -66.7(3) . . . . ? C4 Zr C1 C2 53.9(2) . . . . ? C5 Zr C1 C2 -158.26(19) . . . . ? C3 Zr C1 C2 22.7(2) . . . . ? C6 Zr C1 C2 -164.0(2) . . . . ? C9 Zr C1 C2 150.0(2) . . . . ? C7 Zr C1 C2 165.4(2) . . . . ? C8 Zr C1 C2 140.1(2) . . . . ? Si Zr C1 C2 -102.1(2) . . . . ? Zr C1 C2 C3 -48.2(3) . . . . ? N Zr C2 C3 -95.0(2) . . . . ? C4 Zr C2 C3 23.8(2) . . . . ? C1 Zr C2 C3 140.3(4) . . . . ? C5 Zr C2 C3 -154.9(3) . . . . ? C6 Zr C2 C3 162.68(19) . . . . ? C9 Zr C2 C3 44.5(4) . . . . ? C7 Zr C2 C3 122.6(2) . . . . ? C8 Zr C2 C3 82.5(2) . . . . ? Si Zr C2 C3 -104.8(2) . . . . ? N Zr C2 C1 124.7(2) . . . . ? C4 Zr C2 C1 -116.5(3) . . . . ? C5 Zr C2 C1 64.8(5) . . . . ? C3 Zr C2 C1 -140.3(4) . . . . ? C6 Zr C2 C1 22.4(3) . . . . ? C9 Zr C2 C1 -95.8(4) . . . . ? C7 Zr C2 C1 -17.7(3) . . . . ? C8 Zr C2 C1 -57.8(3) . . . . ? Si Zr C2 C1 114.9(2) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? Zr C2 C3 C4 -45.4(3) . . . . ? C1 C2 C3 Zr 45.7(3) . . . . ? N Zr C3 C2 91.8(2) . . . . ? C4 Zr C3 C2 -140.9(3) . . . . ? C1 Zr C3 C2 -24.3(2) . . . . ? C5 Zr C3 C2 157.8(3) . . . . ? C6 Zr C3 C2 -48.4(5) . . . . ? C9 Zr C3 C2 -163.03(19) . . . . ? C7 Zr C3 C2 -83.8(3) . . . . ? C8 Zr C3 C2 -123.2(2) . . . . ? Si Zr C3 C2 106.7(2) . . . . ? N Zr C3 C4 -127.3(2) . . . . ? C1 Zr C3 C4 116.6(3) . . . . ? C5 Zr C3 C4 -61.2(4) . . . . ? C2 Zr C3 C4 140.9(3) . . . . ? C6 Zr C3 C4 92.5(4) . . . . ? C9 Zr C3 C4 -22.1(3) . . . . ? C7 Zr C3 C4 57.1(3) . . . . ? C8 Zr C3 C4 17.8(3) . . . . ? Si Zr C3 C4 -112.3(2) . . . . ? C2 C3 C4 Zr 47.9(3) . . . . ? N Zr C4 C3 64.7(3) . . . . ? C1 Zr C4 C3 -53.9(2) . . . . ? C5 Zr C4 C3 157.10(19) . . . . ? C2 Zr C4 C3 -22.4(2) . . . . ? C6 Zr C4 C3 -152.4(2) . . . . ? C9 Zr C4 C3 163.8(2) . . . . ? C7 Zr C4 C3 -140.6(2) . . . . ? C8 Zr C4 C3 -165.2(2) . . . . ? Si Zr C4 C3 102.9(2) . . . . ? N Si C5 C9 -73.4(2) . . . . ? C14 Si C5 C9 165.8(2) . . . . ? C15 Si C5 C9 47.5(3) . . . . ? Zr Si C5 C9 -71.2(2) . . . . ? N Si C5 C6 68.4(2) . . . . ? C14 Si C5 C6 -52.4(3) . . . . ? C15 Si C5 C6 -170.6(2) . . . . ? Zr Si C5 C6 70.6(2) . . . . ? N Si C5 Zr -2.19(11) . . . . ? C14 Si C5 Zr -122.98(14) . . . . ? C15 Si C5 Zr 118.78(13) . . . . ? N Zr C5 C9 126.53(19) . . . . ? C4 Zr C5 C9 11.9(3) . . . . ? C1 Zr C5 C9 -121.6(2) . . . . ? C3 Zr C5 C9 55.7(4) . . . . ? C2 Zr C5 C9 -169.6(3) . . . . ? C6 Zr C5 C9 -111.6(2) . . . . ? C7 Zr C5 C9 -75.72(18) . . . . ? C8 Zr C5 C9 -36.01(17) . . . . ? Si Zr C5 C9 124.6(2) . . . . ? N Zr C5 C6 -121.91(19) . . . . ? C4 Zr C5 C6 123.5(2) . . . . ? C1 Zr C5 C6 -10.0(3) . . . . ? C3 Zr C5 C6 167.2(3) . . . . ? C2 Zr C5 C6 -58.0(4) . . . . ? C9 Zr C5 C6 111.6(2) . . . . ? C7 Zr C5 C6 35.84(17) . . . . ? C8 Zr C5 C6 75.55(18) . . . . ? Si Zr C5 C6 -123.8(2) . . . . ? N Zr C5 Si 1.92(9) . . . . ? C4 Zr C5 Si -112.69(17) . . . . ? C1 Zr C5 Si 113.78(17) . . . . ? C3 Zr C5 Si -69.0(4) . . . . ? C2 Zr C5 Si 65.8(4) . . . . ? C6 Zr C5 Si 123.8(2) . . . . ? C9 Zr C5 Si -124.6(2) . . . . ? C7 Zr C5 Si 159.66(16) . . . . ? C8 Zr C5 Si -160.63(16) . . . . ? C9 C5 C6 C7 1.0(3) . . . . ? Si C5 C6 C7 -146.4(2) . . . . ? Zr C5 C6 C7 -67.7(2) . . . . ? C9 C5 C6 C10 -179.4(3) . . . . ? Si C5 C6 C10 33.1(4) . . . . ? Zr C5 C6 C10 111.8(3) . . . . ? C9 C5 C6 Zr 68.76(19) . . . . ? Si C5 C6 Zr -78.66(19) . . . . ? N Zr C6 C7 169.49(18) . . . . ? C4 Zr C6 C7 20.8(3) . . . . ? C1 Zr C6 C7 -71.2(2) . . . . ? C5 Zr C6 C7 116.0(3) . . . . ? C3 Zr C6 C7 -49.3(5) . . . . ? C2 Zr C6 C7 -84.1(2) . . . . ? C9 Zr C6 C7 76.82(19) . . . . ? C8 Zr C6 C7 36.58(17) . . . . ? Si Zr C6 C7 151.14(19) . . . . ? N Zr C6 C5 53.47(17) . . . . ? C4 Zr C6 C5 -95.2(2) . . . . ? C1 Zr C6 C5 172.81(18) . . . . ? C3 Zr C6 C5 -165.3(4) . . . . ? C2 Zr C6 C5 159.84(18) . . . . ? C9 Zr C6 C5 -39.19(16) . . . . ? C7 Zr C6 C5 -116.0(3) . . . . ? C8 Zr C6 C5 -79.43(18) . . . . ? Si Zr C6 C5 35.13(14) . . . . ? N Zr C6 C10 -68.4(2) . . . . ? C4 Zr C6 C10 142.9(3) . . . . ? C1 Zr C6 C10 50.9(3) . . . . ? C5 Zr C6 C10 -121.9(3) . . . . ? C3 Zr C6 C10 72.8(5) . . . . ? C2 Zr C6 C10 37.9(3) . . . . ? C9 Zr C6 C10 -161.1(3) . . . . ? C7 Zr C6 C10 122.1(3) . . . . ? C8 Zr C6 C10 158.7(3) . . . . ? Si Zr C6 C10 -86.8(2) . . . . ? C5 C6 C7 C8 -0.6(3) . . . . ? C10 C6 C7 C8 179.9(3) . . . . ? Zr C6 C7 C8 -65.2(2) . . . . ? C5 C6 C7 C11 -177.0(3) . . . . ? C10 C6 C7 C11 3.4(5) . . . . ? Zr C6 C7 C11 118.4(3) . . . . ? C5 C6 C7 Zr 64.59(19) . . . . ? C10 C6 C7 Zr -115.0(3) . . . . ? N Zr C7 C6 -12.5(2) . . . . ? C4 Zr C7 C6 -166.56(19) . . . . ? C1 Zr C7 C6 111.9(2) . . . . ? C5 Zr C7 C6 -37.79(17) . . . . ? C3 Zr C7 C6 162.32(19) . . . . ? C2 Zr C7 C6 121.99(19) . . . . ? C9 Zr C7 C6 -79.46(19) . . . . ? C8 Zr C7 C6 -115.9(2) . . . . ? Si Zr C7 C6 -25.43(17) . . . . ? N Zr C7 C8 103.39(19) . . . . ? C4 Zr C7 C8 -50.6(2) . . . . ? C1 Zr C7 C8 -132.2(2) . . . . ? C5 Zr C7 C8 78.14(18) . . . . ? C3 Zr C7 C8 -81.7(2) . . . . ? C2 Zr C7 C8 -122.07(19) . . . . ? C6 Zr C7 C8 115.9(2) . . . . ? C9 Zr C7 C8 36.47(17) . . . . ? Si Zr C7 C8 90.51(16) . . . . ? N Zr C7 C11 -135.5(3) . . . . ? C4 Zr C7 C11 70.4(3) . . . . ? C1 Zr C7 C11 -11.1(3) . . . . ? C5 Zr C7 C11 -160.8(3) . . . . ? C3 Zr C7 C11 39.3(3) . . . . ? C2 Zr C7 C11 -1.0(3) . . . . ? C6 Zr C7 C11 -123.0(4) . . . . ? C9 Zr C7 C11 157.5(3) . . . . ? C8 Zr C7 C11 121.1(4) . . . . ? Si Zr C7 C11 -148.4(3) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C11 C7 C8 C9 176.5(3) . . . . ? Zr C7 C8 C9 -63.4(2) . . . . ? C6 C7 C8 C12 -175.1(3) . . . . ? C11 C7 C8 C12 1.4(5) . . . . ? Zr C7 C8 C12 121.5(3) . . . . ? C6 C7 C8 Zr 63.3(2) . . . . ? C11 C7 C8 Zr -120.1(3) . . . . ? N Zr C8 C9 17.4(2) . . . . ? C4 Zr C8 C9 -109.8(2) . . . . ? C1 Zr C8 C9 168.79(19) . . . . ? C5 Zr C8 C9 37.47(17) . . . . ? C3 Zr C8 C9 -119.91(19) . . . . ? C2 Zr C8 C9 -159.66(19) . . . . ? C6 Zr C8 C9 79.68(19) . . . . ? C7 Zr C8 C9 116.3(3) . . . . ? Si Zr C8 C9 25.68(17) . . . . ? N Zr C8 C7 -98.88(18) . . . . ? C4 Zr C8 C7 133.89(19) . . . . ? C1 Zr C8 C7 52.5(2) . . . . ? C5 Zr C8 C7 -78.80(18) . . . . ? C3 Zr C8 C7 123.82(19) . . . . ? C2 Zr C8 C7 84.1(2) . . . . ? C6 Zr C8 C7 -36.59(17) . . . . ? C9 Zr C8 C7 -116.3(3) . . . . ? Si Zr C8 C7 -90.60(16) . . . . ? N Zr C8 C12 138.0(3) . . . . ? C4 Zr C8 C12 10.7(3) . . . . ? C1 Zr C8 C12 -70.6(3) . . . . ? C5 Zr C8 C12 158.0(3) . . . . ? C3 Zr C8 C12 0.7(3) . . . . ? C2 Zr C8 C12 -39.1(3) . . . . ? C6 Zr C8 C12 -159.7(3) . . . . ? C9 Zr C8 C12 120.6(4) . . . . ? C7 Zr C8 C12 -123.1(3) . . . . ? Si Zr C8 C12 146.3(3) . . . . ? C7 C8 C9 C5 0.8(3) . . . . ? C12 C8 C9 C5 175.9(3) . . . . ? Zr C8 C9 C5 -64.11(19) . . . . ? C7 C8 C9 C13 -178.5(3) . . . . ? C12 C8 C9 C13 -3.4(5) . . . . ? Zr C8 C9 C13 116.7(3) . . . . ? C7 C8 C9 Zr 64.9(2) . . . . ? C12 C8 C9 Zr -120.0(3) . . . . ? C6 C5 C9 C8 -1.1(3) . . . . ? Si C5 C9 C8 146.0(2) . . . . ? Zr C5 C9 C8 67.2(2) . . . . ? C6 C5 C9 C13 178.1(3) . . . . ? Si C5 C9 C13 -34.8(4) . . . . ? Zr C5 C9 C13 -113.6(3) . . . . ? C6 C5 C9 Zr -68.28(19) . . . . ? Si C5 C9 Zr 78.79(19) . . . . ? N Zr C9 C8 -165.66(18) . . . . ? C4 Zr C9 C8 72.7(2) . . . . ? C1 Zr C9 C8 -17.4(3) . . . . ? C5 Zr C9 C8 -116.1(3) . . . . ? C3 Zr C9 C8 85.4(2) . . . . ? C2 Zr C9 C8 54.1(4) . . . . ? C6 Zr C9 C8 -76.46(19) . . . . ? C7 Zr C9 C8 -36.37(18) . . . . ? Si Zr C9 C8 -150.84(19) . . . . ? N Zr C9 C5 -49.59(18) . . . . ? C4 Zr C9 C5 -171.22(19) . . . . ? C1 Zr C9 C5 98.6(2) . . . . ? C3 Zr C9 C5 -158.57(18) . . . . ? C2 Zr C9 C5 170.1(3) . . . . ? C6 Zr C9 C5 39.62(17) . . . . ? C7 Zr C9 C5 79.71(18) . . . . ? C8 Zr C9 C5 116.1(3) . . . . ? Si Zr C9 C5 -34.77(15) . . . . ? N Zr C9 C13 72.7(2) . . . . ? C4 Zr C9 C13 -49.0(3) . . . . ? C1 Zr C9 C13 -139.1(3) . . . . ? C5 Zr C9 C13 122.3(3) . . . . ? C3 Zr C9 C13 -36.3(3) . . . . ? C2 Zr C9 C13 -67.6(4) . . . . ? C6 Zr C9 C13 161.9(3) . . . . ? C7 Zr C9 C13 -158.0(3) . . . . ? C8 Zr C9 C13 -121.7(3) . . . . ? Si Zr C9 C13 87.5(2) . . . . ? Si N C16 C17 85.8(3) . . . . ? Zr N C16 C17 -87.2(3) . . . . ? Si N C16 C18 -41.7(3) . . . . ? Zr N C16 C18 145.3(2) . . . . ? N C16 C18 C19 115.0(3) . . . . ? C17 C16 C18 C19 -10.3(4) . . . . ? N C16 C18 C27 -64.4(3) . . . . ? C17 C16 C18 C27 170.3(3) . . . . ? C27 C18 C19 C20 1.3(5) . . . . ? C16 C18 C19 C20 -178.1(3) . . . . ? C18 C19 C20 C21 -0.6(6) . . . . ? C19 C20 C21 C22 0.6(7) . . . . ? C20 C21 C22 C27 -1.2(6) . . . . ? C20 C21 C22 C23 178.8(4) . . . . ? C21 C22 C23 C24 -179.8(4) . . . . ? C27 C22 C23 C24 0.2(7) . . . . ? C22 C23 C24 C25 -1.1(8) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C24 C25 C26 C27 0.6(6) . . . . ? C25 C26 C27 C18 177.6(3) . . . . ? C25 C26 C27 C22 -1.5(5) . . . . ? C19 C18 C27 C26 178.9(3) . . . . ? C16 C18 C27 C26 -1.7(5) . . . . ? C19 C18 C27 C22 -2.0(4) . . . . ? C16 C18 C27 C22 177.4(3) . . . . ? C21 C22 C27 C26 -178.9(3) . . . . ? C23 C22 C27 C26 1.1(5) . . . . ? C21 C22 C27 C18 1.9(5) . . . . ? C23 C22 C27 C18 -178.1(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.293 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.058