# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Pun, Doris' 'Knobloch, Donald' 'Lobkovsky, Emil' 'Chirik, Paul' _publ_contact_author_name 'Chirik, Paul' _publ_contact_author_email pchirik@princeton.edu _publ_section_title ; Cyclisation of a,o-Dienes Promoted by Bis(Indenyl)zirconium Sandwich and ansa-Titanocene Dinitrogen Complexes. ; # Attachment '- Cifs_combined_01_13_11.txt' data_dp14 _database_code_depnum_ccdc_archive 'CCDC 810043' #TrackingRef '- Cifs_combined_01_13_11.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H57 N Zr, C5 H12' _chemical_formula_sum 'C45 H69 N Zr' _chemical_formula_weight 715.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2599(4) _cell_length_b 17.5475(6) _cell_length_c 17.0737(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.942(2) _cell_angle_gamma 90.00 _cell_volume 3967.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9038 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.21 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8740 _exptl_absorpt_correction_T_max 0.9000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 X8 APEX II diffractometer' _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 54861 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12109 _reflns_number_gt 9212 _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, 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. ; _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^)+(0.0412P)^2^+0.7018P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12109 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.185710(10) 0.471180(7) 0.258705(7) 0.01585(3) Uani 1 1 d . . . N1 N 0.30765(10) 0.61552(7) 0.02467(7) 0.0255(3) Uani 1 1 d . . . C1 C 0.21686(11) 0.33726(8) 0.20847(8) 0.0190(3) Uani 1 1 d . . . C2 C 0.19003(11) 0.33117(8) 0.28686(8) 0.0195(3) Uani 1 1 d . . . H2 H 0.2357(12) 0.3142(9) 0.3270(9) 0.019(4) Uiso 1 1 d . . . C3 C 0.08801(11) 0.35083(8) 0.29538(8) 0.0188(3) Uani 1 1 d . . . C4 C 0.04752(10) 0.36882(8) 0.21849(8) 0.0181(3) Uani 1 1 d . . . C5 C -0.05068(11) 0.38859(8) 0.18746(9) 0.0228(3) Uani 1 1 d . . . H5 H -0.1019(13) 0.3954(9) 0.2190(9) 0.022(4) Uiso 1 1 d . . . C6 C -0.06732(11) 0.39833(9) 0.10885(9) 0.0247(3) Uani 1 1 d . . . H6 H -0.1336(12) 0.4087(9) 0.0894(9) 0.022(4) Uiso 1 1 d . . . C7 C 0.01094(12) 0.38990(9) 0.05690(9) 0.0238(3) Uani 1 1 d . . . H7 H -0.0023(12) 0.3974(9) 0.0056(10) 0.027(4) Uiso 1 1 d . . . C8 C 0.10593(11) 0.37159(8) 0.08369(8) 0.0202(3) Uani 1 1 d . . . H8 H 0.1546(12) 0.3651(8) 0.0505(9) 0.018(4) Uiso 1 1 d . . . C9 C 0.12693(10) 0.36073(8) 0.16505(8) 0.0177(3) Uani 1 1 d . . . C10 C 0.23584(11) 0.49144(8) 0.40217(8) 0.0206(3) Uani 1 1 d . . . C11 C 0.13351(11) 0.51352(8) 0.39058(8) 0.0199(3) Uani 1 1 d . . . H11 H 0.0810(13) 0.4858(9) 0.4118(9) 0.019(4) Uiso 1 1 d . . . C12 C 0.12447(11) 0.58007(8) 0.34459(8) 0.0191(3) Uani 1 1 d . . . C13 C 0.22487(11) 0.60225(8) 0.32953(8) 0.0191(3) Uani 1 1 d . . . C14 C 0.26176(12) 0.66650(8) 0.29009(8) 0.0230(3) Uani 1 1 d . . . H14 H 0.2177(13) 0.7024(9) 0.2669(9) 0.024(4) Uiso 1 1 d . . . C15 C 0.36314(13) 0.67704(9) 0.28826(9) 0.0284(4) Uani 1 1 d . . . H15 H 0.3873(13) 0.7156(9) 0.2647(10) 0.026(4) Uiso 1 1 d . . . C16 C 0.43153(12) 0.62463(10) 0.32411(9) 0.0285(4) Uani 1 1 d . . . H16 H 0.5037(14) 0.6352(10) 0.3244(10) 0.038(5) Uiso 1 1 d . . . C17 C 0.39913(11) 0.56203(9) 0.36157(9) 0.0250(3) Uani 1 1 d . . . H17 H 0.4475(14) 0.5282(9) 0.3847(10) 0.030(5) Uiso 1 1 d . . . C18 C 0.29402(11) 0.54851(8) 0.36537(8) 0.0199(3) Uani 1 1 d . . . C19 C 0.31184(11) 0.30876(8) 0.17405(9) 0.0222(3) Uani 1 1 d . . . H19 H 0.3344(11) 0.3463(8) 0.1354(8) 0.009(3) Uiso 1 1 d . . . C20 C 0.39804(11) 0.29904(10) 0.23488(10) 0.0290(4) Uani 1 1 d . . . H20A H 0.4100 0.3473 0.2628 0.043 Uiso 1 1 calc R . . H20B H 0.4592 0.2841 0.2089 0.043 Uiso 1 1 calc R . . H20C H 0.3807 0.2594 0.2723 0.043 Uiso 1 1 calc R . . C21 C 0.29093(13) 0.23320(9) 0.13162(11) 0.0337(4) Uani 1 1 d . . . H21A H 0.2714 0.1947 0.1695 0.051 Uiso 1 1 calc R . . H21B H 0.3520 0.2164 0.1066 0.051 Uiso 1 1 calc R . . H21C H 0.2361 0.2401 0.0916 0.051 Uiso 1 1 calc R . . C22 C 0.03488(11) 0.33452(8) 0.36976(8) 0.0219(3) Uani 1 1 d . . . H22 H 0.0715(12) 0.3542(9) 0.4119(9) 0.019(4) Uiso 1 1 d . . . C23 C 0.03414(17) 0.24935(10) 0.38534(11) 0.0439(5) Uani 1 1 d . . . H23A H -0.0044 0.2235 0.3426 0.066 Uiso 1 1 calc R . . H23B H 0.0027 0.2394 0.4350 0.066 Uiso 1 1 calc R . . H23C H 0.1036 0.2301 0.3884 0.066 Uiso 1 1 calc R . . C24 C -0.07224(13) 0.36466(12) 0.37231(10) 0.0408(5) Uani 1 1 d . . . H24A H -0.0738 0.4183 0.3564 0.061 Uiso 1 1 calc R . . H24B H -0.0951 0.3601 0.4258 0.061 Uiso 1 1 calc R . . H24C H -0.1169 0.3350 0.3364 0.061 Uiso 1 1 calc R . . C25 C 0.27335(12) 0.43330(9) 0.46194(9) 0.0253(3) Uani 1 1 d . . . H25 H 0.2243(13) 0.3953(10) 0.4664(9) 0.029(5) Uiso 1 1 d . . . C26 C 0.28198(16) 0.47140(11) 0.54249(10) 0.0409(5) Uani 1 1 d . . . H26A H 0.3320 0.5125 0.5420 0.061 Uiso 1 1 calc R . . H26B H 0.3033 0.4336 0.5823 0.061 Uiso 1 1 calc R . . H26C H 0.2162 0.4925 0.5549 0.061 Uiso 1 1 calc R . . C27 C 0.37244(13) 0.39397(10) 0.44602(10) 0.0360(4) Uani 1 1 d . . . H27A H 0.3728 0.3801 0.3904 0.054 Uiso 1 1 calc R . . H27B H 0.3796 0.3479 0.4783 0.054 Uiso 1 1 calc R . . H27C H 0.4288 0.4286 0.4591 0.054 Uiso 1 1 calc R . . C28 C 0.03264(12) 0.62784(9) 0.32726(9) 0.0240(3) Uani 1 1 d . . . H28 H 0.0473(12) 0.6587(9) 0.2836(9) 0.019(4) Uiso 1 1 d . . . C29 C -0.06171(12) 0.58241(11) 0.30718(11) 0.0386(4) Uani 1 1 d . . . H29A H -0.0504 0.5492 0.2623 0.058 Uiso 1 1 calc R . . H29B H -0.1177 0.6172 0.2938 0.058 Uiso 1 1 calc R . . H29C H -0.0783 0.5512 0.3524 0.058 Uiso 1 1 calc R . . C30 C 0.01607(14) 0.68109(10) 0.39581(11) 0.0379(4) Uani 1 1 d . . . H30A H -0.0002 0.6511 0.4419 0.057 Uiso 1 1 calc R . . H30B H -0.0399 0.7158 0.3819 0.057 Uiso 1 1 calc R . . H30C H 0.0776 0.7107 0.4077 0.057 Uiso 1 1 calc R . . C31 C 0.11519(11) 0.54410(8) 0.16013(8) 0.0199(3) Uani 1 1 d . . . H31B H 0.0543(13) 0.5234(9) 0.1437(10) 0.025(4) Uiso 1 1 d . . . H31A H 0.0975(13) 0.5947(10) 0.1779(10) 0.029(5) Uiso 1 1 d . . . C32 C 0.18746(11) 0.54785(8) 0.09233(8) 0.0207(3) Uani 1 1 d . . . H32 H 0.1503(13) 0.5295(8) 0.0431(10) 0.026(4) Uiso 1 1 d . . . C33 C 0.22494(12) 0.62741(9) 0.07627(9) 0.0239(3) Uani 1 1 d . . . H33B H 0.1724(11) 0.6591(8) 0.0521(8) 0.011(4) Uiso 1 1 d . . . H33A H 0.2469(13) 0.6513(9) 0.1293(10) 0.029(4) Uiso 1 1 d . . . C34 C 0.36177(13) 0.54763(10) 0.05406(10) 0.0305(4) Uani 1 1 d . . . H34B H 0.4208(13) 0.5601(9) 0.0848(10) 0.025(4) Uiso 1 1 d . . . H34A H 0.3872(16) 0.5161(11) 0.0092(12) 0.051(6) Uiso 1 1 d . . . C35 C 0.28795(11) 0.50252(9) 0.10342(8) 0.0213(3) Uani 1 1 d . . . H35 H 0.2800(11) 0.4520(8) 0.0805(9) 0.013(4) Uiso 1 1 d . . . C36 C 0.32292(11) 0.49527(9) 0.18957(8) 0.0210(3) Uani 1 1 d . . . H36B H 0.3797(14) 0.4630(9) 0.1973(10) 0.027(5) Uiso 1 1 d . . . H36A H 0.3425(13) 0.5439(9) 0.2067(10) 0.028(5) Uiso 1 1 d . . . C37 C 0.37036(13) 0.68259(10) 0.00887(9) 0.0319(4) Uani 1 1 d . . . C38 C 0.42741(16) 0.71390(11) 0.08159(11) 0.0468(5) Uani 1 1 d . . . H38A H 0.3791 0.7303 0.1197 0.070 Uiso 1 1 calc R . . H38B H 0.4687 0.7575 0.0669 0.070 Uiso 1 1 calc R . . H38C H 0.4712 0.6741 0.1049 0.070 Uiso 1 1 calc R . . C39 C 0.30057(17) 0.74526(11) -0.02455(13) 0.0544(6) Uani 1 1 d . . . H39A H 0.2584 0.7249 -0.0685 0.082 Uiso 1 1 calc R . . H39B H 0.3412 0.7877 -0.0430 0.082 Uiso 1 1 calc R . . H39C H 0.2573 0.7634 0.0164 0.082 Uiso 1 1 calc R . . C40 C 0.44440(16) 0.66076(13) -0.05152(11) 0.0516(6) Uani 1 1 d . . . H40A H 0.4919 0.6229 -0.0291 0.077 Uiso 1 1 calc R . . H40B H 0.4817 0.7061 -0.0670 0.077 Uiso 1 1 calc R . . H40C H 0.4077 0.6392 -0.0976 0.077 Uiso 1 1 calc R . . C1S C 0.7342(2) 0.60543(19) 0.10819(19) 0.1010(11) Uani 1 1 d . . . H1SA H 0.7041 0.6521 0.0859 0.152 Uiso 1 1 calc R . . H1SB H 0.7482 0.5699 0.0658 0.152 Uiso 1 1 calc R . . H1SC H 0.7973 0.6179 0.1378 0.152 Uiso 1 1 calc R . . C2S C 0.6624(2) 0.56927(16) 0.16180(14) 0.0701(8) Uani 1 1 d . . . H2SA H 0.6474 0.6069 0.2028 0.084 Uiso 1 1 calc R . . H2SB H 0.5984 0.5591 0.1311 0.084 Uiso 1 1 calc R . . C3S C 0.69463(16) 0.49777(13) 0.20124(15) 0.0572(6) Uani 1 1 d . . . H3SA H 0.7571 0.5082 0.2337 0.069 Uiso 1 1 calc R . . H3SB H 0.7120 0.4606 0.1605 0.069 Uiso 1 1 calc R . . C4S C 0.62028(17) 0.46141(14) 0.25212(14) 0.0573(6) Uani 1 1 d . . . H4SA H 0.6020 0.4986 0.2926 0.069 Uiso 1 1 calc R . . H4SB H 0.5582 0.4498 0.2196 0.069 Uiso 1 1 calc R . . C5S C 0.6547(2) 0.39218(14) 0.29088(18) 0.0736(8) Uani 1 1 d . . . H5SA H 0.6014 0.3725 0.3232 0.110 Uiso 1 1 calc R . . H5SB H 0.7153 0.4030 0.3243 0.110 Uiso 1 1 calc R . . H5SC H 0.6706 0.3540 0.2514 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01533(6) 0.01499(6) 0.01727(6) 0.00001(5) 0.00117(4) -0.00006(5) N1 0.0261(6) 0.0276(7) 0.0232(6) 0.0061(5) 0.0037(5) -0.0046(5) C1 0.0178(6) 0.0152(6) 0.0242(6) -0.0007(5) 0.0015(5) 0.0001(5) C2 0.0201(7) 0.0158(6) 0.0224(6) 0.0020(5) -0.0006(5) 0.0007(5) C3 0.0175(6) 0.0173(6) 0.0216(6) 0.0011(5) 0.0025(5) -0.0017(5) C4 0.0157(6) 0.0153(6) 0.0234(6) -0.0014(5) 0.0014(5) -0.0023(5) C5 0.0164(7) 0.0241(7) 0.0281(7) -0.0015(6) 0.0033(6) -0.0018(6) C6 0.0176(7) 0.0271(8) 0.0287(7) 0.0005(6) -0.0043(6) -0.0003(6) C7 0.0257(7) 0.0237(7) 0.0216(7) -0.0006(6) -0.0030(6) -0.0032(6) C8 0.0207(7) 0.0191(7) 0.0209(6) -0.0030(5) 0.0039(5) -0.0035(5) C9 0.0175(6) 0.0142(6) 0.0215(6) -0.0010(5) 0.0017(5) -0.0014(5) C10 0.0223(7) 0.0218(7) 0.0177(6) -0.0006(5) -0.0002(5) 0.0008(6) C11 0.0205(7) 0.0201(7) 0.0192(6) -0.0011(5) 0.0043(5) -0.0014(5) C12 0.0200(7) 0.0177(6) 0.0195(6) -0.0033(5) 0.0006(5) 0.0005(5) C13 0.0202(7) 0.0171(6) 0.0200(6) -0.0034(5) 0.0010(5) -0.0004(5) C14 0.0290(8) 0.0177(7) 0.0222(7) -0.0017(6) -0.0006(6) -0.0024(6) C15 0.0330(8) 0.0239(8) 0.0283(7) -0.0009(6) 0.0028(6) -0.0116(6) C16 0.0204(7) 0.0339(8) 0.0311(8) -0.0067(7) -0.0002(6) -0.0082(6) C17 0.0212(7) 0.0272(8) 0.0261(7) -0.0024(6) -0.0030(6) -0.0021(6) C18 0.0200(7) 0.0210(7) 0.0186(6) -0.0027(5) -0.0001(5) -0.0007(5) C19 0.0186(7) 0.0199(7) 0.0283(7) -0.0020(6) 0.0039(6) 0.0023(6) C20 0.0188(7) 0.0325(8) 0.0356(8) -0.0001(7) 0.0011(6) 0.0074(6) C21 0.0290(8) 0.0271(8) 0.0455(9) -0.0115(7) 0.0070(7) 0.0029(7) C22 0.0222(7) 0.0231(7) 0.0209(6) 0.0010(6) 0.0044(5) -0.0046(6) C23 0.0657(13) 0.0269(9) 0.0408(10) 0.0056(8) 0.0212(9) -0.0084(9) C24 0.0260(9) 0.0632(12) 0.0340(8) 0.0123(9) 0.0107(7) 0.0035(8) C25 0.0266(8) 0.0265(8) 0.0228(7) 0.0033(6) -0.0010(6) 0.0009(6) C26 0.0574(12) 0.0439(10) 0.0212(7) 0.0023(7) -0.0009(8) 0.0120(9) C27 0.0356(9) 0.0373(9) 0.0344(8) 0.0057(7) -0.0037(7) 0.0123(8) C28 0.0231(7) 0.0241(7) 0.0252(7) 0.0005(6) 0.0033(6) 0.0066(6) C29 0.0218(8) 0.0399(10) 0.0538(11) -0.0130(9) -0.0023(8) 0.0071(7) C30 0.0395(10) 0.0308(9) 0.0432(10) -0.0110(8) 0.0010(8) 0.0140(7) C31 0.0186(7) 0.0195(7) 0.0216(6) 0.0015(5) 0.0021(5) -0.0003(5) C32 0.0202(7) 0.0230(7) 0.0189(6) 0.0025(5) 0.0001(5) -0.0005(5) C33 0.0231(7) 0.0240(7) 0.0245(7) 0.0046(6) 0.0016(6) -0.0021(6) C34 0.0271(8) 0.0318(9) 0.0336(8) 0.0064(7) 0.0103(7) 0.0003(7) C35 0.0197(7) 0.0209(7) 0.0238(7) 0.0005(6) 0.0057(5) -0.0009(6) C36 0.0181(7) 0.0204(7) 0.0246(7) -0.0014(6) 0.0019(5) -0.0012(6) C37 0.0334(9) 0.0348(9) 0.0276(7) 0.0081(7) 0.0034(7) -0.0117(7) C38 0.0522(12) 0.0471(11) 0.0411(10) 0.0006(9) 0.0042(9) -0.0255(9) C39 0.0583(13) 0.0426(11) 0.0625(13) 0.0285(10) 0.0036(11) -0.0111(10) C40 0.0543(12) 0.0587(13) 0.0441(10) 0.0009(9) 0.0235(9) -0.0239(10) C1S 0.093(2) 0.122(2) 0.088(2) -0.0017(19) 0.0083(18) -0.0618(19) C2S 0.0683(17) 0.0879(19) 0.0541(14) -0.0056(14) 0.0016(12) 0.0104(15) C3S 0.0331(11) 0.0575(13) 0.0813(16) -0.0218(12) 0.0044(11) -0.0093(10) C4S 0.0365(11) 0.0743(16) 0.0609(14) -0.0054(12) 0.0007(10) 0.0055(11) C5S 0.0578(15) 0.0640(16) 0.0971(19) -0.0083(15) -0.0137(14) -0.0072(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C36 2.2589(15) . ? Zr1 C31 2.2765(14) . ? Zr1 C11 2.5021(14) . ? Zr1 C2 2.5034(14) . ? Zr1 C10 2.5300(13) . ? Zr1 C1 2.5426(14) . ? Zr1 C12 2.5657(14) . ? Zr1 C3 2.5717(14) . ? Zr1 C9 2.6063(13) . ? Zr1 C4 2.6318(13) . ? Zr1 C18 2.6367(14) . ? Zr1 C13 2.6376(13) . ? N1 C33 1.457(2) . ? N1 C34 1.466(2) . ? N1 C37 1.474(2) . ? C1 C2 1.406(2) . ? C1 C9 1.4319(19) . ? C1 C19 1.503(2) . ? C2 C3 1.411(2) . ? C3 C4 1.4281(19) . ? C3 C22 1.511(2) . ? C4 C5 1.4233(19) . ? C4 C9 1.435(2) . ? C5 C6 1.360(2) . ? C6 C7 1.407(2) . ? C7 C8 1.356(2) . ? C8 C9 1.4156(19) . ? C10 C11 1.415(2) . ? C10 C18 1.429(2) . ? C10 C25 1.509(2) . ? C11 C12 1.409(2) . ? C12 C13 1.423(2) . ? C12 C28 1.495(2) . ? C13 C14 1.413(2) . ? C13 C18 1.4307(19) . ? C14 C15 1.359(2) . ? C15 C16 1.409(2) . ? C16 C17 1.352(2) . ? C17 C18 1.419(2) . ? C19 C20 1.514(2) . ? C19 C21 1.529(2) . ? C22 C23 1.518(2) . ? C22 C24 1.518(2) . ? C25 C27 1.521(2) . ? C25 C26 1.528(2) . ? C28 C29 1.508(2) . ? C28 C30 1.522(2) . ? C31 C32 1.542(2) . ? C32 C33 1.512(2) . ? C32 C35 1.555(2) . ? C34 C35 1.543(2) . ? C35 C36 1.525(2) . ? C37 C40 1.509(3) . ? C37 C38 1.523(2) . ? C37 C39 1.529(3) . ? C1S C2S 1.495(4) . ? C2S C3S 1.477(4) . ? C3S C4S 1.491(3) . ? C4S C5S 1.446(3) . ? 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 C36 Zr1 C31 79.62(5) . . ? C36 Zr1 C11 133.01(5) . . ? C31 Zr1 C11 112.10(5) . . ? C36 Zr1 C2 105.84(5) . . ? C31 Zr1 C2 134.27(5) . . ? C11 Zr1 C2 97.08(5) . . ? C36 Zr1 C10 107.51(5) . . ? C31 Zr1 C10 135.59(5) . . ? C11 Zr1 C10 32.66(5) . . ? C2 Zr1 C10 87.12(5) . . ? C36 Zr1 C1 81.23(5) . . ? C31 Zr1 C1 109.74(5) . . ? C11 Zr1 C1 129.43(5) . . ? C2 Zr1 C1 32.36(5) . . ? C10 Zr1 C1 114.66(5) . . ? C36 Zr1 C12 116.51(5) . . ? C31 Zr1 C12 82.75(5) . . ? C11 Zr1 C12 32.25(4) . . ? C2 Zr1 C12 128.75(5) . . ? C10 Zr1 C12 54.35(4) . . ? C1 Zr1 C12 160.52(5) . . ? C36 Zr1 C3 135.25(5) . . ? C31 Zr1 C3 116.66(5) . . ? C11 Zr1 C3 81.87(5) . . ? C2 Zr1 C3 32.24(5) . . ? C10 Zr1 C3 89.44(5) . . ? C1 Zr1 C3 54.25(5) . . ? C12 Zr1 C3 107.11(5) . . ? C36 Zr1 C9 92.42(5) . . ? C31 Zr1 C9 82.29(5) . . ? C11 Zr1 C9 133.24(5) . . ? C2 Zr1 C9 52.50(4) . . ? C10 Zr1 C9 138.93(4) . . ? C1 Zr1 C9 32.26(4) . . ? C12 Zr1 C9 144.19(4) . . ? C3 Zr1 C9 53.14(4) . . ? C36 Zr1 C4 124.06(5) . . ? C31 Zr1 C4 86.37(5) . . ? C11 Zr1 C4 102.50(5) . . ? C2 Zr1 C4 52.34(4) . . ? C10 Zr1 C4 119.56(5) . . ? C1 Zr1 C4 53.43(4) . . ? C12 Zr1 C4 114.89(4) . . ? C3 Zr1 C4 31.83(4) . . ? C9 Zr1 C4 31.80(4) . . ? C36 Zr1 C18 80.78(5) . . ? C31 Zr1 C18 114.20(5) . . ? C11 Zr1 C18 52.53(5) . . ? C2 Zr1 C18 111.48(4) . . ? C10 Zr1 C18 32.03(5) . . ? C1 Zr1 C18 128.06(4) . . ? C12 Zr1 C18 53.07(4) . . ? C3 Zr1 C18 121.18(4) . . ? C9 Zr1 C18 160.32(4) . . ? C4 Zr1 C18 151.49(4) . . ? C36 Zr1 C13 86.07(5) . . ? C31 Zr1 C13 84.98(5) . . ? C11 Zr1 C13 52.09(4) . . ? C2 Zr1 C13 139.96(4) . . ? C10 Zr1 C13 52.98(4) . . ? C1 Zr1 C13 158.28(4) . . ? C12 Zr1 C13 31.71(4) . . ? C3 Zr1 C13 133.96(4) . . ? C9 Zr1 C13 167.25(4) . . ? C4 Zr1 C13 146.39(4) . . ? C18 Zr1 C13 31.48(4) . . ? C33 N1 C34 106.26(12) . . ? C33 N1 C37 116.47(13) . . ? C34 N1 C37 116.14(13) . . ? C2 C1 C9 105.66(12) . . ? C2 C1 C19 127.23(13) . . ? C9 C1 C19 125.85(13) . . ? C2 C1 Zr1 72.29(8) . . ? C9 C1 Zr1 76.32(8) . . ? C19 C1 Zr1 126.41(9) . . ? C1 C2 C3 111.73(12) . . ? C1 C2 Zr1 75.35(8) . . ? C3 C2 Zr1 76.54(8) . . ? C2 C3 C4 106.05(12) . . ? C2 C3 C22 122.10(12) . . ? C4 C3 C22 130.17(13) . . ? C2 C3 Zr1 71.22(8) . . ? C4 C3 Zr1 76.41(8) . . ? C22 C3 Zr1 128.51(9) . . ? C5 C4 C3 133.61(14) . . ? C5 C4 C9 118.33(12) . . ? C3 C4 C9 108.00(12) . . ? C5 C4 Zr1 122.83(10) . . ? C3 C4 Zr1 71.76(8) . . ? C9 C4 Zr1 73.12(7) . . ? C6 C5 C4 119.80(14) . . ? C5 C6 C7 121.43(13) . . ? C8 C7 C6 120.95(14) . . ? C7 C8 C9 119.69(14) . . ? C8 C9 C1 131.56(13) . . ? C8 C9 C4 119.78(12) . . ? C1 C9 C4 108.54(12) . . ? C8 C9 Zr1 122.65(9) . . ? C1 C9 Zr1 71.42(8) . . ? C4 C9 Zr1 75.08(8) . . ? C11 C10 C18 106.39(12) . . ? C11 C10 C25 124.05(13) . . ? C18 C10 C25 127.18(13) . . ? C11 C10 Zr1 72.59(8) . . ? C18 C10 Zr1 78.10(8) . . ? C25 C10 Zr1 128.37(10) . . ? C12 C11 C10 110.99(13) . . ? C12 C11 Zr1 76.36(8) . . ? C10 C11 Zr1 74.75(8) . . ? C11 C12 C13 105.89(12) . . ? C11 C12 C28 128.31(13) . . ? C13 C12 C28 124.81(13) . . ? C11 C12 Zr1 71.39(8) . . ? C13 C12 Zr1 76.93(8) . . ? C28 C12 Zr1 125.65(9) . . ? C14 C13 C12 130.85(13) . . ? C14 C13 C18 119.98(13) . . ? C12 C13 C18 109.11(12) . . ? C14 C13 Zr1 122.82(10) . . ? C12 C13 Zr1 71.36(8) . . ? C18 C13 Zr1 74.23(8) . . ? C15 C14 C13 119.10(14) . . ? C14 C15 C16 121.11(15) . . ? C17 C16 C15 121.51(15) . . ? C16 C17 C18 119.62(14) . . ? C17 C18 C10 133.72(14) . . ? C17 C18 C13 118.67(13) . . ? C10 C18 C13 107.54(12) . . ? C17 C18 Zr1 123.78(10) . . ? C10 C18 Zr1 69.87(8) . . ? C13 C18 Zr1 74.30(8) . . ? C1 C19 C20 112.81(12) . . ? C1 C19 C21 109.80(12) . . ? C20 C19 C21 109.84(13) . . ? C3 C22 C23 109.94(13) . . ? C3 C22 C24 115.81(13) . . ? C23 C22 C24 108.87(15) . . ? C10 C25 C27 116.34(13) . . ? C10 C25 C26 108.64(13) . . ? C27 C25 C26 109.51(14) . . ? C12 C28 C29 113.97(13) . . ? C12 C28 C30 109.89(12) . . ? C29 C28 C30 110.40(14) . . ? C32 C31 Zr1 109.36(9) . . ? C33 C32 C31 113.48(12) . . ? C33 C32 C35 101.94(12) . . ? C31 C32 C35 116.65(12) . . ? N1 C33 C32 104.01(12) . . ? N1 C34 C35 106.90(13) . . ? C36 C35 C34 113.57(13) . . ? C36 C35 C32 112.11(12) . . ? C34 C35 C32 103.58(12) . . ? C35 C36 Zr1 107.85(9) . . ? N1 C37 C40 108.38(15) . . ? N1 C37 C38 113.59(13) . . ? C40 C37 C38 109.59(15) . . ? N1 C37 C39 107.83(14) . . ? C40 C37 C39 109.27(16) . . ? C38 C37 C39 108.10(16) . . ? C3S C2S C1S 117.5(2) . . ? C2S C3S C4S 116.4(2) . . ? C5S C4S C3S 115.1(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.797 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.072 #===END data_djk3 _database_code_depnum_ccdc_archive 'CCDC 810044' #TrackingRef '- Cifs_combined_01_13_11.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H49 N Si Ti' _chemical_formula_sum 'C30 H49 N Si Ti' _chemical_formula_weight 499.69 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6335(8) _cell_length_b 9.8554(6) _cell_length_c 17.9416(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.665(3) _cell_angle_gamma 90.00 _cell_volume 2810.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3998 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.87 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 0.9473 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 X8 APEX II diffractometer' _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 26243 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6956 _reflns_number_gt 5011 _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, 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. ; _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^)+(0.0530P)^2^+0.8078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6956 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Ti1 Ti 0.326702(15) 0.21566(3) 0.478325(16) 0.01624(7) Uani 1 1 d . . . Si1 Si 0.47117(3) 0.29336(5) 0.65686(3) 0.01962(10) Uani 1 1 d . . . N1 N 0.12881(8) 0.01336(15) 0.24546(9) 0.0275(4) Uani 1 1 d . . . C1 C 0.42696(9) 0.38111(16) 0.55487(9) 0.0175(3) Uani 1 1 d . . . C2 C 0.34622(9) 0.44607(16) 0.51876(9) 0.0196(3) Uani 1 1 d . . . C3 C 0.31926(9) 0.45589(16) 0.43273(9) 0.0206(4) Uani 1 1 d . . . C4 C 0.38092(9) 0.39466(16) 0.41355(9) 0.0196(3) Uani 1 1 d . . . C5 C 0.44627(9) 0.34692(16) 0.48801(9) 0.0179(3) Uani 1 1 d . . . C6 C 0.39269(9) 0.15367(17) 0.62008(9) 0.0202(4) Uani 1 1 d . . . C7 C 0.30583(9) 0.17121(18) 0.60036(9) 0.0219(4) Uani 1 1 d . . . H7 H 0.2843(10) 0.2395(19) 0.6212(11) 0.025(5) Uiso 1 1 d . . . C8 C 0.25842(9) 0.06516(17) 0.54824(9) 0.0226(4) Uani 1 1 d . . . C9 C 0.31466(10) -0.01303(17) 0.53038(10) 0.0233(4) Uani 1 1 d . . . H9 H 0.3009(9) -0.0876(17) 0.4961(10) 0.016(4) Uiso 1 1 d . . . C10 C 0.39611(10) 0.04120(17) 0.57370(9) 0.0219(4) Uani 1 1 d . . . H10 H 0.4438(10) 0.0101(18) 0.5705(10) 0.019(4) Uiso 1 1 d . . . C11 C 0.30014(11) 0.5126(2) 0.56231(11) 0.0292(4) Uani 1 1 d . . . H11C H 0.3069(13) 0.608(2) 0.5629(13) 0.054(7) Uiso 1 1 d . . . H11B H 0.2406(12) 0.499(2) 0.5331(13) 0.051(6) Uiso 1 1 d . . . H11A H 0.3175(12) 0.487(2) 0.6156(13) 0.046(6) Uiso 1 1 d . . . C12 C 0.24611(11) 0.53872(19) 0.37534(11) 0.0282(4) Uani 1 1 d . . . H12C H 0.2055(14) 0.541(3) 0.3926(14) 0.063(8) Uiso 1 1 d . . . H12B H 0.2259(14) 0.518(3) 0.3214(16) 0.076(8) Uiso 1 1 d . . . H12A H 0.2619(12) 0.630(2) 0.3777(13) 0.051(7) Uiso 1 1 d . . . C13 C 0.38377(10) 0.39478(19) 0.33146(10) 0.0260(4) Uani 1 1 d . . . H13C H 0.3418(11) 0.454(2) 0.2940(12) 0.041(6) Uiso 1 1 d . . . H13B H 0.4379(12) 0.434(2) 0.3368(12) 0.041(6) Uiso 1 1 d . . . H13A H 0.3771(13) 0.307(2) 0.3086(13) 0.052(7) Uiso 1 1 d . . . C14 C 0.52448(10) 0.28002(19) 0.49340(10) 0.0241(4) Uani 1 1 d . . . H14C H 0.5314(11) 0.194(2) 0.5145(11) 0.030(5) Uiso 1 1 d . . . H14B H 0.5245(11) 0.271(2) 0.4430(12) 0.037(6) Uiso 1 1 d . . . H14A H 0.5728(13) 0.326(2) 0.5267(13) 0.050(6) Uiso 1 1 d . . . C15 C 0.58110(11) 0.2312(2) 0.69330(11) 0.0295(4) Uani 1 1 d . . . H15C H 0.5866(11) 0.160(2) 0.6653(12) 0.037(6) Uiso 1 1 d . . . H15B H 0.6211(12) 0.302(2) 0.6934(13) 0.046(6) Uiso 1 1 d . . . H15A H 0.5963(13) 0.204(2) 0.7474(14) 0.053(7) Uiso 1 1 d . . . C16 C 0.46614(11) 0.3919(2) 0.74230(10) 0.0293(4) Uani 1 1 d . . . H16C H 0.4079(12) 0.407(2) 0.7371(12) 0.045(6) Uiso 1 1 d . . . H16B H 0.4939(13) 0.342(2) 0.7917(13) 0.053(7) Uiso 1 1 d . . . H16A H 0.4930(12) 0.472(2) 0.7476(12) 0.047(6) Uiso 1 1 d . . . C17 C 0.16889(10) 0.0276(2) 0.53197(10) 0.0303(4) Uani 1 1 d . . . C18 C 0.17507(13) -0.0342(3) 0.61256(13) 0.0484(6) Uani 1 1 d . . . H18C H 0.2100(11) -0.111(2) 0.6248(11) 0.033(5) Uiso 1 1 d . . . H18B H 0.1172(13) -0.063(2) 0.6074(13) 0.057(7) Uiso 1 1 d . . . H18A H 0.1966(13) 0.040(2) 0.6592(14) 0.057(7) Uiso 1 1 d . . . C19 C 0.11146(11) 0.1510(2) 0.51161(12) 0.0385(5) Uani 1 1 d . . . H19C H 0.1314(13) 0.206(2) 0.5533(14) 0.048(6) Uiso 1 1 d . . . H19B H 0.0992(13) 0.191(2) 0.4539(14) 0.057(7) Uiso 1 1 d . . . H19A H 0.0584(14) 0.120(3) 0.5043(14) 0.064(7) Uiso 1 1 d . . . C20 C 0.13099(12) -0.0775(2) 0.46324(12) 0.0385(5) Uani 1 1 d . . . H20C H 0.1272(10) -0.0418(19) 0.4106(11) 0.028(5) Uiso 1 1 d . . . H20B H 0.1607(12) -0.161(2) 0.4789(13) 0.042(6) Uiso 1 1 d . . . H20A H 0.0736(13) -0.099(2) 0.4548(13) 0.052(6) Uiso 1 1 d . . . C21 C 0.20126(10) 0.22159(18) 0.38065(10) 0.0230(4) Uani 1 1 d . . . H21B H 0.1679(11) 0.2977(19) 0.3804(11) 0.027(5) Uiso 1 1 d . . . H21A H 0.1707(11) 0.148(2) 0.3851(11) 0.035(5) Uiso 1 1 d . . . C22 C 0.20992(10) 0.20768(18) 0.30032(10) 0.0237(4) Uani 1 1 d . . . H22 H 0.2272(10) 0.2940(18) 0.2848(11) 0.023(5) Uiso 1 1 d . . . C23 C 0.27171(10) 0.09280(18) 0.30760(10) 0.0249(4) Uani 1 1 d . . . H23 H 0.2868(11) 0.099(2) 0.2562(12) 0.039(6) Uiso 1 1 d . . . C24 C 0.35026(9) 0.08966(17) 0.38986(9) 0.0208(4) Uani 1 1 d . . . H24B H 0.3633(10) 0.0018(19) 0.4068(11) 0.026(5) Uiso 1 1 d . . . H24A H 0.3997(11) 0.120(2) 0.3830(11) 0.036(5) Uiso 1 1 d . . . C25 C 0.21680(10) -0.0333(2) 0.28981(11) 0.0303(4) Uani 1 1 d . . . H25 H 0.2331(11) -0.094(2) 0.2561(12) 0.037(6) Uiso 1 1 d . . . H25B H 0.2283(11) -0.083(2) 0.3446(12) 0.036(5) Uiso 1 1 d . . . C26 C 0.12980(10) 0.15702(19) 0.22880(10) 0.0286(4) Uani 1 1 d . . . H26 H 0.0777(10) 0.2028(16) 0.2263(10) 0.015(4) Uiso 1 1 d . . . H26B H 0.1320(11) 0.170(2) 0.1763(12) 0.039(6) Uiso 1 1 d . . . C27 C 0.07113(11) -0.0734(2) 0.17767(11) 0.0330(5) Uani 1 1 d . . . C28 C -0.01653(12) -0.0104(3) 0.14532(16) 0.0496(7) Uani 1 1 d . . . H28C H -0.0184(12) 0.073(2) 0.1114(13) 0.046(6) Uiso 1 1 d . . . H28B H -0.0587(12) -0.074(2) 0.1020(13) 0.048(6) Uiso 1 1 d . . . H28A H -0.0305(14) 0.003(3) 0.1915(15) 0.066(8) Uiso 1 1 d . . . C29 C 0.07019(13) -0.2114(2) 0.21396(14) 0.0430(6) Uani 1 1 d . . . H29C H 0.0309(13) -0.268(2) 0.1767(13) 0.049(6) Uiso 1 1 d . . . H29B H 0.0559(12) -0.201(2) 0.2613(13) 0.042(6) Uiso 1 1 d . . . H29A H 0.1262(15) -0.257(3) 0.2328(16) 0.070(8) Uiso 1 1 d . . . C30 C 0.09585(14) -0.0865(2) 0.10604(13) 0.0444(6) Uani 1 1 d . . . H30C H 0.1516(13) -0.125(2) 0.1249(13) 0.052(7) Uiso 1 1 d . . . H30B H 0.0941(14) 0.002(3) 0.0832(15) 0.064(8) Uiso 1 1 d . . . H30A H 0.0602(13) -0.142(2) 0.0648(14) 0.056(7) Uiso 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 Ti1 0.01648(11) 0.01602(14) 0.01547(12) -0.00021(10) 0.00622(9) -0.00130(11) Si1 0.01963(18) 0.0213(2) 0.01621(18) -0.00209(16) 0.00617(15) -0.00328(17) N1 0.0240(6) 0.0273(8) 0.0265(7) -0.0038(6) 0.0064(5) -0.0041(6) C1 0.0173(6) 0.0146(7) 0.0200(7) -0.0028(6) 0.0075(5) -0.0037(6) C2 0.0191(6) 0.0172(8) 0.0233(7) -0.0037(6) 0.0100(6) -0.0016(6) C3 0.0207(7) 0.0154(8) 0.0239(7) -0.0001(6) 0.0082(6) -0.0023(6) C4 0.0218(7) 0.0176(8) 0.0197(7) 0.0005(6) 0.0092(5) -0.0045(6) C5 0.0174(6) 0.0159(8) 0.0204(7) -0.0011(6) 0.0083(5) -0.0036(6) C6 0.0229(7) 0.0201(8) 0.0149(6) 0.0021(6) 0.0056(6) -0.0019(6) C7 0.0250(7) 0.0235(9) 0.0215(7) -0.0002(6) 0.0142(6) -0.0042(7) C8 0.0250(7) 0.0234(9) 0.0181(7) 0.0034(6) 0.0082(6) -0.0051(7) C9 0.0303(8) 0.0162(8) 0.0202(7) 0.0013(6) 0.0080(6) -0.0051(7) C10 0.0216(7) 0.0205(8) 0.0203(7) 0.0046(6) 0.0059(6) 0.0021(7) C11 0.0314(8) 0.0277(10) 0.0326(8) -0.0038(7) 0.0178(7) 0.0033(7) C12 0.0269(8) 0.0214(9) 0.0315(9) 0.0053(7) 0.0082(7) 0.0034(7) C13 0.0313(8) 0.0275(10) 0.0198(7) 0.0011(7) 0.0115(6) -0.0053(7) C14 0.0229(7) 0.0238(9) 0.0277(8) -0.0031(7) 0.0130(6) -0.0007(7) C15 0.0242(8) 0.0315(10) 0.0282(9) 0.0010(8) 0.0070(7) 0.0002(8) C16 0.0328(8) 0.0375(11) 0.0200(7) -0.0072(7) 0.0136(6) -0.0101(8) C17 0.0282(8) 0.0381(11) 0.0264(8) 0.0008(7) 0.0135(6) -0.0110(8) C18 0.0432(10) 0.0678(16) 0.0359(10) 0.0093(10) 0.0186(8) -0.0199(11) C19 0.0283(8) 0.0544(14) 0.0373(10) -0.0056(9) 0.0183(7) -0.0062(9) C20 0.0325(9) 0.0409(12) 0.0384(10) -0.0039(9) 0.0120(8) -0.0184(9) C21 0.0189(7) 0.0219(9) 0.0255(8) 0.0012(6) 0.0071(6) -0.0028(7) C22 0.0224(7) 0.0229(9) 0.0219(7) 0.0002(6) 0.0060(6) -0.0016(7) C23 0.0246(7) 0.0278(9) 0.0207(7) -0.0047(6) 0.0082(6) -0.0018(7) C24 0.0213(7) 0.0199(8) 0.0216(7) -0.0022(6) 0.0097(6) 0.0006(6) C25 0.0243(8) 0.0314(10) 0.0305(9) -0.0052(8) 0.0074(7) -0.0019(7) C26 0.0257(8) 0.0304(10) 0.0225(8) 0.0015(7) 0.0038(7) -0.0007(7) C27 0.0238(8) 0.0340(11) 0.0340(9) -0.0101(8) 0.0057(7) -0.0072(8) C28 0.0240(9) 0.0493(14) 0.0599(14) -0.0125(11) 0.0036(9) -0.0072(9) C29 0.0396(10) 0.0401(12) 0.0447(11) -0.0096(9) 0.0138(9) -0.0133(9) C30 0.0468(11) 0.0472(13) 0.0324(10) -0.0107(9) 0.0108(9) -0.0092(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 Ti1 C21 2.1470(15) . ? Ti1 C24 2.1920(17) . ? Ti1 C1 2.3595(14) . ? Ti1 C10 2.3597(16) . ? Ti1 C2 2.3632(16) . ? Ti1 C6 2.3732(15) . ? Ti1 C7 2.4124(17) . ? Ti1 C5 2.4148(15) . ? Ti1 C9 2.4837(17) . ? Ti1 C3 2.4898(16) . ? Ti1 C4 2.5177(16) . ? Ti1 C8 2.5557(17) . ? Si1 C16 1.8489(19) . ? Si1 C6 1.8587(16) . ? Si1 C1 1.8623(15) . ? Si1 C15 1.8609(18) . ? N1 C26 1.449(2) . ? N1 C27 1.474(2) . ? N1 C25 1.477(2) . ? C1 C5 1.422(2) . ? C1 C2 1.434(2) . ? C2 C3 1.408(2) . ? C2 C11 1.500(2) . ? C3 C4 1.410(2) . ? C3 C12 1.497(2) . ? C4 C5 1.414(2) . ? C4 C13 1.495(2) . ? C5 C14 1.494(2) . ? C6 C10 1.403(2) . ? C6 C7 1.425(2) . ? C7 C8 1.410(2) . ? C8 C9 1.398(2) . ? C8 C17 1.522(2) . ? C9 C10 1.409(2) . ? C17 C19 1.522(3) . ? C17 C20 1.525(3) . ? C17 C18 1.528(3) . ? C21 C22 1.520(3) . ? C22 C26 1.524(2) . ? C22 C23 1.537(2) . ? C23 C25 1.522(3) . ? C23 C24 1.525(2) . ? C27 C29 1.511(3) . ? C27 C30 1.531(3) . ? C27 C28 1.528(3) . ? 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 C21 Ti1 C24 82.86(6) . . ? C21 Ti1 C1 134.72(6) . . ? C24 Ti1 C1 118.93(6) . . ? C21 Ti1 C10 129.73(6) . . ? C24 Ti1 C10 84.89(6) . . ? C1 Ti1 C10 93.38(5) . . ? C21 Ti1 C2 100.72(6) . . ? C24 Ti1 C2 135.93(6) . . ? C1 Ti1 C2 35.36(5) . . ? C10 Ti1 C2 121.11(5) . . ? C21 Ti1 C6 137.34(6) . . ? C24 Ti1 C6 118.13(6) . . ? C1 Ti1 C6 70.01(5) . . ? C10 Ti1 C6 34.48(6) . . ? C2 Ti1 C6 88.84(6) . . ? C21 Ti1 C7 103.74(6) . . ? C24 Ti1 C7 134.88(6) . . ? C1 Ti1 C7 88.14(5) . . ? C10 Ti1 C7 56.26(6) . . ? C2 Ti1 C7 87.42(6) . . ? C6 Ti1 C7 34.65(5) . . ? C21 Ti1 C5 127.08(6) . . ? C24 Ti1 C5 85.54(6) . . ? C1 Ti1 C5 34.63(5) . . ? C10 Ti1 C5 100.12(5) . . ? C2 Ti1 C5 57.09(5) . . ? C6 Ti1 C5 93.05(5) . . ? C7 Ti1 C5 120.24(5) . . ? C21 Ti1 C9 96.08(6) . . ? C24 Ti1 C9 80.34(6) . . ? C1 Ti1 C9 124.94(5) . . ? C10 Ti1 C9 33.71(5) . . ? C2 Ti1 C9 141.38(6) . . ? C6 Ti1 C9 56.32(5) . . ? C7 Ti1 C9 54.72(6) . . ? C5 Ti1 C9 132.32(5) . . ? C21 Ti1 C3 79.45(6) . . ? C24 Ti1 C3 107.48(6) . . ? C1 Ti1 C3 56.89(5) . . ? C10 Ti1 C3 150.24(5) . . ? C2 Ti1 C3 33.60(5) . . ? C6 Ti1 C3 121.91(5) . . ? C7 Ti1 C3 117.63(6) . . ? C5 Ti1 C3 55.55(5) . . ? C9 Ti1 C3 170.24(6) . . ? C21 Ti1 C4 93.85(6) . . ? C24 Ti1 C4 80.43(6) . . ? C1 Ti1 C4 56.35(5) . . ? C10 Ti1 C4 131.60(5) . . ? C2 Ti1 C4 55.56(6) . . ? C6 Ti1 C4 124.55(5) . . ? C7 Ti1 C4 141.62(6) . . ? C5 Ti1 C4 33.24(5) . . ? C9 Ti1 C4 157.04(6) . . ? C3 Ti1 C4 32.71(5) . . ? C21 Ti1 C8 83.03(6) . . ? C24 Ti1 C8 107.70(6) . . ? C1 Ti1 C8 120.59(5) . . ? C10 Ti1 C8 55.10(5) . . ? C2 Ti1 C8 116.35(6) . . ? C6 Ti1 C8 56.02(5) . . ? C7 Ti1 C8 32.82(5) . . ? C5 Ti1 C8 149.08(5) . . ? C9 Ti1 C8 32.18(6) . . ? C3 Ti1 C8 138.09(6) . . ? C4 Ti1 C8 170.75(6) . . ? C16 Si1 C6 112.80(8) . . ? C16 Si1 C1 114.89(8) . . ? C6 Si1 C1 93.71(7) . . ? C16 Si1 C15 107.36(8) . . ? C6 Si1 C15 112.51(8) . . ? C1 Si1 C15 115.29(8) . . ? C26 N1 C27 117.52(13) . . ? C26 N1 C25 108.15(13) . . ? C27 N1 C25 116.90(15) . . ? C5 C1 C2 106.15(13) . . ? C5 C1 Si1 124.58(11) . . ? C2 C1 Si1 124.21(12) . . ? C5 C1 Ti1 74.81(8) . . ? C2 C1 Ti1 72.46(8) . . ? Si1 C1 Ti1 98.06(7) . . ? C3 C2 C1 108.89(14) . . ? C3 C2 C11 122.62(14) . . ? C1 C2 C11 127.98(14) . . ? C3 C2 Ti1 78.14(9) . . ? C1 C2 Ti1 72.18(9) . . ? C11 C2 Ti1 122.70(12) . . ? C2 C3 C4 107.94(13) . . ? C2 C3 C12 124.96(16) . . ? C4 C3 C12 126.25(15) . . ? C2 C3 Ti1 68.26(9) . . ? C4 C3 Ti1 74.74(9) . . ? C12 C3 Ti1 130.68(11) . . ? C3 C4 C5 108.11(14) . . ? C3 C4 C13 126.75(14) . . ? C5 C4 C13 124.71(15) . . ? C3 C4 Ti1 72.56(9) . . ? C5 C4 Ti1 69.38(9) . . ? C13 C4 Ti1 129.54(11) . . ? C4 C5 C1 108.85(13) . . ? C4 C5 C14 124.04(15) . . ? C1 C5 C14 126.99(13) . . ? C4 C5 Ti1 77.38(9) . . ? C1 C5 Ti1 70.56(9) . . ? C14 C5 Ti1 121.41(11) . . ? C10 C6 C7 105.44(13) . . ? C10 C6 Si1 125.39(13) . . ? C7 C6 Si1 123.58(13) . . ? C10 C6 Ti1 72.23(9) . . ? C7 C6 Ti1 74.18(9) . . ? Si1 C6 Ti1 97.69(7) . . ? C8 C7 C6 109.83(15) . . ? C8 C7 Ti1 79.18(10) . . ? C6 C7 Ti1 71.17(9) . . ? C9 C8 C7 106.55(14) . . ? C9 C8 C17 126.99(16) . . ? C7 C8 C17 125.13(16) . . ? C9 C8 Ti1 71.08(10) . . ? C7 C8 Ti1 68.00(9) . . ? C17 C8 Ti1 135.84(11) . . ? C8 C9 C10 108.62(15) . . ? C8 C9 Ti1 76.75(10) . . ? C10 C9 Ti1 68.32(9) . . ? C6 C10 C9 109.35(15) . . ? C6 C10 Ti1 73.28(9) . . ? C9 C10 Ti1 77.98(9) . . ? C19 C17 C8 112.24(16) . . ? C19 C17 C20 109.58(15) . . ? C8 C17 C20 112.05(16) . . ? C19 C17 C18 108.20(17) . . ? C8 C17 C18 105.82(13) . . ? C20 C17 C18 108.76(17) . . ? C22 C21 Ti1 106.29(11) . . ? C21 C22 C26 113.01(15) . . ? C21 C22 C23 110.15(13) . . ? C26 C22 C23 101.23(14) . . ? C25 C23 C24 114.53(14) . . ? C25 C23 C22 102.73(13) . . ? C24 C23 C22 114.23(14) . . ? C23 C24 Ti1 108.15(11) . . ? N1 C25 C23 106.46(15) . . ? N1 C26 C22 103.66(13) . . ? N1 C27 C29 107.38(15) . . ? N1 C27 C30 113.35(16) . . ? C29 C27 C30 110.23(18) . . ? N1 C27 C28 107.53(16) . . ? C29 C27 C28 109.33(18) . . ? C30 C27 C28 108.94(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.529 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.062