data_03101 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H85 N2 O P Ti' _chemical_formula_weight 845.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 10.866(4) _cell_length_b 11.228(4) _cell_length_c 41.606(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.107(9) _cell_angle_gamma 90.00 _cell_volume 5047(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 894 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.19 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 64.61 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 38799 _diffrn_reflns_av_R_equivalents 0.5623 _diffrn_reflns_av_sigmaI/netI 0.7140 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.15 _reflns_number_total 8996 _reflns_number_gt 1776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8996 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3280 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.644 _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 Ti1 Ti 0.68103(14) 0.61300(13) 0.11389(4) 0.0239(4) Uani 1 1 d . . . P2 P 0.7626(2) 0.5265(2) 0.16932(6) 0.0276(7) Uani 1 1 d . . . C3 C 0.8553(7) 0.5941(7) 0.14172(18) 0.024(2) Uani 1 1 d . . . C4 C 0.8439(8) 0.7275(7) 0.1437(2) 0.028(2) Uani 1 1 d . . . H59 H 0.8589 0.7671 0.1639 0.034 Uiso 1 1 calc R . . C5 C 0.8110(8) 0.7923(8) 0.1154(2) 0.036(3) Uani 1 1 d . . . N6 N 0.7670(6) 0.7316(5) 0.08798(17) 0.0239(19) Uani 1 1 d . . . C7 C 0.7761(9) 0.7817(7) 0.0567(2) 0.027(2) Uani 1 1 d . . . C8 C 0.6674(10) 0.7931(7) 0.0348(2) 0.038(3) Uani 1 1 d . . . C9 C 0.6802(9) 0.8425(7) 0.0043(2) 0.037(3) Uani 1 1 d . . . H60 H 0.6085 0.8500 -0.0107 0.044 Uiso 1 1 calc R . . C10 C 0.7912(9) 0.8804(8) -0.0047(2) 0.046(3) Uani 1 1 d . . . H61 H 0.7968 0.9140 -0.0254 0.055 Uiso 1 1 calc R . . C11 C 0.8944(9) 0.8683(8) 0.0172(2) 0.042(3) Uani 1 1 d . . . H62 H 0.9721 0.8934 0.0111 0.050 Uiso 1 1 calc R . . C12 C 0.8906(8) 0.8218(7) 0.0477(2) 0.030(2) Uani 1 1 d . . . C13 C 1.0116(8) 0.8031(7) 0.0686(2) 0.034(3) Uani 1 1 d . . . H63 H 0.9922 0.7813 0.0908 0.040 Uiso 1 1 calc R . . C14 C 1.0824(8) 0.6974(7) 0.0551(2) 0.048(3) Uani 1 1 d . . . H66 H 1.0267 0.6289 0.0516 0.072 Uiso 1 1 calc R . . H64 H 1.1530 0.6760 0.0706 0.072 Uiso 1 1 calc R . . H65 H 1.1121 0.7207 0.0346 0.072 Uiso 1 1 calc R . . C15 C 1.0933(8) 0.9158(7) 0.0713(2) 0.053(3) Uani 1 1 d . . . H67 H 1.1293 0.9284 0.0510 0.079 Uiso 1 1 calc R . . H69 H 1.1598 0.9057 0.0889 0.079 Uiso 1 1 calc R . . H68 H 1.0428 0.9849 0.0758 0.079 Uiso 1 1 calc R . . C16 C 0.5405(8) 0.7536(8) 0.0420(2) 0.037(3) Uani 1 1 d . . . H70 H 0.5465 0.7267 0.0651 0.044 Uiso 1 1 calc R . . C17 C 0.4432(8) 0.8507(7) 0.0374(2) 0.059(3) Uani 1 1 d . . . H71 H 0.4693 0.9190 0.0511 0.089 Uiso 1 1 calc R . . H73 H 0.3642 0.8202 0.0433 0.089 Uiso 1 1 calc R . . H72 H 0.4331 0.8756 0.0147 0.089 Uiso 1 1 calc R . . C18 C 0.4951(8) 0.6470(7) 0.0201(2) 0.052(3) Uani 1 1 d . . . H74 H 0.4869 0.6722 -0.0025 0.077 Uiso 1 1 calc R . . H75 H 0.4147 0.6198 0.0259 0.077 Uiso 1 1 calc R . . H76 H 0.5552 0.5818 0.0232 0.077 Uiso 1 1 calc R . . C19 C 0.7857(7) 0.3658(6) 0.1650(2) 0.034(3) Uani 1 1 d . . . H77 H 0.7751 0.3474 0.1416 0.041 Uiso 1 1 calc R . . H78 H 0.8731 0.3484 0.1729 0.041 Uiso 1 1 calc R . . C20 C 0.7051(9) 0.2783(8) 0.1816(2) 0.033(2) Uani 1 1 d . . . C21 C 0.5712(8) 0.3116(7) 0.1745(2) 0.051(3) Uani 1 1 d . . . H81 H 0.5193 0.2445 0.1798 0.077 Uiso 1 1 calc R . . H80 H 0.5535 0.3311 0.1515 0.077 Uiso 1 1 calc R . . H79 H 0.5533 0.3809 0.1875 0.077 Uiso 1 1 calc R . . C22 C 0.7258(9) 0.1552(7) 0.1665(2) 0.070(4) Uani 1 1 d . . . H84 H 0.6791 0.0946 0.1770 0.106 Uiso 1 1 calc R . . H83 H 0.8142 0.1355 0.1695 0.106 Uiso 1 1 calc R . . H82 H 0.6974 0.1575 0.1433 0.106 Uiso 1 1 calc R . . C23 C 0.7435(9) 0.2714(8) 0.2172(2) 0.059(3) Uani 1 1 d . . . H86 H 0.8337 0.2636 0.2211 0.089 Uiso 1 1 calc R . . H87 H 0.7044 0.2021 0.2262 0.089 Uiso 1 1 calc R . . H85 H 0.7174 0.3440 0.2277 0.089 Uiso 1 1 calc R . . C24 C 0.8028(9) 0.5583(7) 0.2136(2) 0.030(2) Uani 1 1 d . . . C25 C 0.9215(9) 0.5279(8) 0.2296(2) 0.040(3) Uani 1 1 d . . . C26 C 0.9398(10) 0.5252(8) 0.2632(2) 0.055(3) Uani 1 1 d . . . H88 H 1.0198 0.5061 0.2734 0.066 Uiso 1 1 calc R . . C27 C 0.8488(12) 0.5486(10) 0.2821(3) 0.061(4) Uani 1 1 d . . . C28 C 0.7357(11) 0.5882(9) 0.2673(2) 0.060(4) Uani 1 1 d . . . H89 H 0.6739 0.6120 0.2805 0.072 Uiso 1 1 calc R . . C29 C 0.7084(10) 0.5946(8) 0.2324(2) 0.043(3) Uani 1 1 d . . . C30 C 0.5844(8) 0.6406(7) 0.2182(2) 0.037(3) Uani 1 1 d . . . H90 H 0.5790 0.6330 0.1941 0.044 Uiso 1 1 calc R . . C31 C 0.5726(9) 0.7709(7) 0.2267(2) 0.072(4) Uani 1 1 d . . . H96 H 0.5861 0.7804 0.2503 0.108 Uiso 1 1 calc R . . H94 H 0.4895 0.7992 0.2189 0.108 Uiso 1 1 calc R . . H95 H 0.6344 0.8173 0.2166 0.108 Uiso 1 1 calc R . . C32 C 0.4795(9) 0.5720(8) 0.2301(2) 0.073(4) Uani 1 1 d . . . H93 H 0.4838 0.5788 0.2537 0.110 Uiso 1 1 calc R . . H92 H 0.4858 0.4880 0.2241 0.110 Uiso 1 1 calc R . . H91 H 0.4006 0.6044 0.2203 0.110 Uiso 1 1 calc R . . C33 C 1.0326(8) 0.5053(8) 0.2114(2) 0.045(3) Uani 1 1 d . . . H97 H 1.0016 0.4768 0.1892 0.054 Uiso 1 1 calc R . . C34 C 1.1229(8) 0.4126(9) 0.2267(2) 0.091(4) Uani 1 1 d . . . H100 H 1.1617 0.4423 0.2475 0.137 Uiso 1 1 calc R . . H99 H 1.1868 0.3971 0.2123 0.137 Uiso 1 1 calc R . . H98 H 1.0782 0.3387 0.2301 0.137 Uiso 1 1 calc R . . C35 C 1.0999(8) 0.6269(8) 0.2077(2) 0.066(3) Uani 1 1 d . . . H102 H 1.0416 0.6844 0.1969 0.099 Uiso 1 1 calc R . . H101 H 1.1694 0.6155 0.1949 0.099 Uiso 1 1 calc R . . H103 H 1.1308 0.6572 0.2292 0.099 Uiso 1 1 calc R . . C36 C 0.8615(14) 0.5404(12) 0.3177(2) 0.118(6) Uani 1 1 d . . . H104 H 0.9493 0.5121 0.3202 0.142 Uiso 1 1 calc R . . C37 C 0.8829(11) 0.6458(9) 0.3345(2) 0.101(5) Uani 1 1 d . . . H107 H 0.8090 0.6962 0.3312 0.152 Uiso 1 1 calc R . . H105 H 0.9531 0.6874 0.3266 0.152 Uiso 1 1 calc R . . H106 H 0.9017 0.6285 0.3576 0.152 Uiso 1 1 calc R . . C38 C 0.8106(11) 0.4382(10) 0.3293(2) 0.113(5) Uani 1 1 d . . . H108 H 0.8423 0.4267 0.3520 0.170 Uiso 1 1 calc R . . H110 H 0.8331 0.3695 0.3166 0.170 Uiso 1 1 calc R . . H109 H 0.7203 0.4460 0.3274 0.170 Uiso 1 1 calc R . . C39 C 0.9730(7) 0.5455(7) 0.13061(19) 0.038(3) Uani 1 1 d . . . H111 H 0.9846 0.5787 0.1094 0.057 Uiso 1 1 calc R . . H113 H 0.9676 0.4585 0.1291 0.057 Uiso 1 1 calc R . . H112 H 1.0434 0.5676 0.1462 0.057 Uiso 1 1 calc R . . C40 C 0.8148(7) 0.9263(6) 0.11614(19) 0.029(2) Uani 1 1 d . . . H116 H 0.8855 0.9543 0.1054 0.044 Uiso 1 1 calc R . . H114 H 0.8235 0.9538 0.1386 0.044 Uiso 1 1 calc R . . H115 H 0.7381 0.9580 0.1049 0.044 Uiso 1 1 calc R . . N41 N 0.6386(5) 0.4835(5) 0.09296(14) 0.0156(17) Uani 1 1 d . . . C42 C 0.6331(8) 0.3717(8) 0.07949(19) 0.028(2) Uani 1 1 d . . . C43 C 0.5282(8) 0.2966(7) 0.0805(2) 0.026(2) Uani 1 1 d . . . C44 C 0.5337(8) 0.1813(7) 0.0702(2) 0.036(3) Uani 1 1 d . . . H117 H 0.4656 0.1303 0.0728 0.043 Uiso 1 1 calc R . . C45 C 0.6350(9) 0.1343(8) 0.0562(2) 0.043(3) Uani 1 1 d . . . H118 H 0.6353 0.0546 0.0485 0.052 Uiso 1 1 calc R . . C46 C 0.7344(9) 0.2099(8) 0.0540(2) 0.042(3) Uani 1 1 d . . . H119 H 0.8038 0.1808 0.0444 0.050 Uiso 1 1 calc R . . C47 C 0.7375(9) 0.3249(7) 0.0652(2) 0.032(3) Uani 1 1 d . . . C48 C 0.8431(8) 0.4026(8) 0.0590(2) 0.041(3) Uani 1 1 d . . . H120 H 0.8475 0.4682 0.0753 0.049 Uiso 1 1 calc R . . C49 C 0.9684(8) 0.3391(7) 0.0628(2) 0.074(4) Uani 1 1 d . . . H122 H 0.9759 0.2915 0.0826 0.111 Uiso 1 1 calc R . . H121 H 1.0350 0.3983 0.0639 0.111 Uiso 1 1 calc R . . H123 H 0.9747 0.2869 0.0441 0.111 Uiso 1 1 calc R . . C50 C 0.8233(8) 0.4610(8) 0.0254(2) 0.057(3) Uani 1 1 d . . . H125 H 0.8078 0.3992 0.0088 0.086 Uiso 1 1 calc R . . H126 H 0.8974 0.5062 0.0215 0.086 Uiso 1 1 calc R . . H124 H 0.7520 0.5149 0.0245 0.086 Uiso 1 1 calc R . . C51 C 0.4096(8) 0.3442(7) 0.0922(2) 0.037(3) Uani 1 1 d . . . H127 H 0.4336 0.4068 0.1088 0.045 Uiso 1 1 calc R . . C52 C 0.3348(8) 0.4043(7) 0.0641(2) 0.048(3) Uani 1 1 d . . . H128 H 0.3873 0.4613 0.0540 0.072 Uiso 1 1 calc R . . H130 H 0.2647 0.4465 0.0718 0.072 Uiso 1 1 calc R . . H129 H 0.3039 0.3442 0.0481 0.072 Uiso 1 1 calc R . . C53 C 0.3292(8) 0.2546(7) 0.1073(2) 0.047(3) Uani 1 1 d . . . H131 H 0.2894 0.2022 0.0905 0.070 Uiso 1 1 calc R . . H132 H 0.2657 0.2967 0.1180 0.070 Uiso 1 1 calc R . . H133 H 0.3805 0.2070 0.1233 0.070 Uiso 1 1 calc R . . O54 O 0.5182(5) 0.7068(5) 0.12472(13) 0.0304(16) Uani 1 1 d . . . C55 C 0.3956(8) 0.6640(7) 0.1142(2) 0.040(3) Uani 1 1 d . . . H134 H 0.4004 0.6088 0.0958 0.048 Uiso 1 1 calc R . . H135 H 0.3435 0.7324 0.1062 0.048 Uiso 1 1 calc R . . C56 C 0.3336(9) 0.6007(9) 0.1401(2) 0.084(4) Uani 1 1 d . . . H136 H 0.3919 0.5445 0.1515 0.127 Uiso 1 1 calc R . . H137 H 0.2610 0.5572 0.1302 0.127 Uiso 1 1 calc R . . H138 H 0.3075 0.6592 0.1555 0.127 Uiso 1 1 calc R . . C57 C 0.5166(8) 0.8118(7) 0.1446(2) 0.040(3) Uani 1 1 d . . . H140 H 0.6002 0.8246 0.1560 0.047 Uiso 1 1 calc R . . H139 H 0.4588 0.7989 0.1612 0.047 Uiso 1 1 calc R . . C58 C 0.4782(9) 0.9199(7) 0.1256(2) 0.064(3) Uani 1 1 d . . . H142 H 0.5279 0.9270 0.1074 0.096 Uiso 1 1 calc R . . H141 H 0.4910 0.9904 0.1394 0.096 Uiso 1 1 calc R . . H143 H 0.3905 0.9136 0.1174 0.096 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 Ti1 0.0211(10) 0.0239(9) 0.0274(10) 0.0025(10) 0.0051(8) 0.0032(9) P2 0.0283(16) 0.0270(15) 0.0275(16) 0.0042(13) 0.0037(13) 0.0021(13) C3 0.020(5) 0.034(6) 0.019(5) -0.005(5) 0.003(4) 0.011(5) C4 0.044(7) 0.018(6) 0.026(6) 0.005(5) 0.019(5) -0.008(5) C5 0.033(7) 0.029(6) 0.052(7) -0.017(6) 0.022(6) 0.000(5) N6 0.020(5) 0.019(4) 0.033(5) 0.001(4) 0.002(4) 0.005(4) C7 0.037(7) 0.027(6) 0.015(5) 0.002(5) -0.001(5) -0.008(5) C8 0.053(8) 0.023(6) 0.042(7) -0.003(5) 0.017(6) -0.002(5) C9 0.051(7) 0.026(6) 0.031(6) 0.011(5) -0.007(6) 0.001(5) C10 0.051(8) 0.055(7) 0.034(7) 0.018(6) 0.014(6) -0.018(7) C11 0.032(7) 0.061(8) 0.033(6) 0.001(6) 0.012(5) -0.029(6) C12 0.031(6) 0.029(6) 0.029(6) 0.001(5) -0.003(5) -0.008(5) C13 0.024(6) 0.037(6) 0.041(7) 0.000(5) 0.010(5) -0.011(5) C14 0.031(6) 0.058(7) 0.058(8) -0.011(6) 0.022(6) -0.008(6) C15 0.044(7) 0.066(8) 0.048(7) -0.004(6) 0.001(6) -0.026(6) C16 0.023(6) 0.039(6) 0.048(7) 0.003(6) -0.005(5) 0.001(5) C17 0.050(8) 0.064(8) 0.066(8) 0.008(7) 0.017(6) 0.005(6) C18 0.044(7) 0.047(7) 0.065(8) -0.007(6) 0.009(6) -0.005(6) C19 0.027(6) 0.018(6) 0.058(7) -0.005(5) 0.010(5) 0.002(5) C20 0.033(6) 0.032(6) 0.032(6) -0.002(5) -0.006(5) 0.012(5) C21 0.047(8) 0.042(7) 0.066(8) 0.006(6) 0.012(7) -0.007(6) C22 0.087(10) 0.013(6) 0.116(10) 0.009(6) 0.032(8) 0.001(6) C23 0.074(9) 0.058(7) 0.043(7) 0.029(6) -0.003(7) -0.010(7) C24 0.044(7) 0.025(6) 0.018(6) 0.003(5) -0.010(5) -0.006(5) C25 0.032(7) 0.042(7) 0.045(7) 0.013(6) 0.001(6) -0.003(5) C26 0.053(8) 0.076(9) 0.031(7) 0.018(7) -0.016(6) -0.020(7) C27 0.076(10) 0.072(9) 0.030(7) -0.005(7) -0.008(7) -0.020(8) C28 0.087(10) 0.058(8) 0.041(8) -0.007(7) 0.039(7) -0.031(8) C29 0.055(8) 0.035(7) 0.039(7) -0.012(6) 0.011(6) -0.017(6) C30 0.042(7) 0.031(6) 0.040(7) -0.007(5) 0.018(6) -0.009(5) C31 0.096(10) 0.045(7) 0.076(9) -0.025(7) 0.019(8) 0.029(7) C32 0.082(10) 0.085(9) 0.059(8) -0.010(7) 0.036(7) 0.007(8) C33 0.031(7) 0.055(8) 0.047(7) 0.013(6) -0.007(6) 0.007(6) C34 0.056(9) 0.122(11) 0.088(9) 0.024(9) -0.027(7) 0.053(8) C35 0.066(9) 0.086(9) 0.045(7) -0.026(7) 0.009(6) -0.024(8) C36 0.214(18) 0.135(13) 0.011(7) -0.016(8) 0.033(9) -0.106(13) C37 0.144(14) 0.120(13) 0.040(8) -0.018(8) 0.012(9) 0.018(11) C38 0.149(14) 0.153(14) 0.041(8) -0.004(9) 0.028(9) -0.047(11) C39 0.029(6) 0.040(6) 0.046(7) 0.012(5) 0.003(5) -0.004(5) C40 0.037(6) 0.017(5) 0.036(6) -0.005(5) 0.011(5) 0.000(4) N41 0.026(4) 0.013(4) 0.007(4) -0.002(3) -0.003(3) -0.005(3) C42 0.019(6) 0.041(6) 0.020(5) 0.004(5) -0.016(4) 0.007(5) C43 0.027(6) 0.014(5) 0.036(6) 0.006(5) 0.006(5) 0.009(5) C44 0.029(6) 0.033(6) 0.045(7) 0.010(5) 0.000(5) -0.003(5) C45 0.052(7) 0.027(6) 0.045(7) 0.014(6) -0.018(6) 0.003(6) C46 0.035(7) 0.047(7) 0.043(7) -0.016(6) -0.003(6) 0.019(6) C47 0.043(7) 0.018(6) 0.035(6) -0.012(5) 0.002(6) -0.005(5) C48 0.045(7) 0.034(6) 0.045(7) -0.009(6) 0.012(6) 0.010(6) C49 0.036(7) 0.070(8) 0.114(10) -0.049(8) -0.006(7) 0.025(6) C50 0.059(8) 0.066(7) 0.048(7) -0.007(7) 0.010(6) -0.015(6) C51 0.045(7) 0.030(6) 0.036(6) 0.020(5) -0.002(5) 0.004(5) C52 0.033(6) 0.048(7) 0.062(7) 0.004(6) -0.002(6) -0.001(6) C53 0.030(6) 0.046(7) 0.064(8) 0.000(6) 0.010(6) -0.016(5) O54 0.031(4) 0.026(4) 0.034(4) -0.004(3) 0.003(3) 0.004(3) C55 0.032(7) 0.033(6) 0.054(7) 0.003(5) -0.002(6) 0.002(5) C56 0.061(9) 0.122(10) 0.075(9) 0.013(9) 0.033(7) -0.023(8) C57 0.045(7) 0.037(6) 0.036(7) 0.003(6) 0.001(6) 0.011(5) C58 0.077(9) 0.038(7) 0.077(9) 0.006(6) 0.003(7) 0.000(6) _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 N41 1.732(6) . ? Ti1 N6 2.005(7) . ? Ti1 C3 2.123(8) . ? Ti1 O54 2.147(5) . ? Ti1 C4 2.420(8) . ? Ti1 C5 2.456(9) . ? Ti1 P2 2.572(3) . ? P2 C3 1.776(8) . ? P2 C19 1.833(7) . ? P2 C24 1.882(8) . ? C3 C4 1.506(9) . ? C3 C39 1.508(9) . ? C4 C5 1.397(11) . ? C5 N6 1.372(10) . ? C5 C40 1.505(9) . ? N6 C7 1.433(9) . ? C7 C12 1.409(11) . ? C7 C8 1.418(11) . ? C8 C9 1.404(11) . ? C8 C16 1.509(11) . ? C9 C10 1.367(10) . ? C10 C11 1.375(11) . ? C11 C12 1.376(10) . ? C12 C13 1.511(11) . ? C13 C15 1.543(9) . ? C13 C14 1.551(10) . ? C16 C17 1.517(10) . ? C16 C18 1.552(10) . ? C19 C20 1.529(10) . ? C20 C23 1.499(11) . ? C20 C21 1.501(11) . ? C20 C22 1.545(10) . ? C24 C29 1.415(11) . ? C24 C25 1.428(11) . ? C25 C26 1.394(11) . ? C25 C33 1.513(11) . ? C26 C27 1.354(12) . ? C27 C28 1.388(13) . ? C27 C36 1.473(12) . ? C28 C29 1.452(11) . ? C29 C30 1.504(12) . ? C30 C32 1.503(10) . ? C30 C31 1.515(9) . ? C33 C34 1.522(10) . ? C33 C35 1.563(10) . ? C36 C37 1.382(12) . ? C36 C38 1.383(12) . ? N41 C42 1.373(9) . ? C42 C43 1.423(10) . ? C42 C47 1.435(10) . ? C43 C44 1.367(9) . ? C43 C51 1.522(10) . ? C44 C45 1.403(10) . ? C45 C46 1.384(11) . ? C46 C47 1.371(10) . ? C47 C48 1.486(11) . ? C48 C49 1.530(11) . ? C48 C50 1.537(10) . ? C51 C53 1.512(9) . ? C51 C52 1.512(10) . ? O54 C55 1.440(9) . ? O54 C57 1.443(8) . ? C55 C56 1.510(10) . ? C57 C58 1.485(9) . ? 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 N41 Ti1 N6 113.7(3) . . ? N41 Ti1 C3 111.4(3) . . ? N6 Ti1 C3 85.4(3) . . ? N41 Ti1 O54 109.6(3) . . ? N6 Ti1 O54 103.2(2) . . ? C3 Ti1 O54 129.9(3) . . ? N41 Ti1 C4 147.6(3) . . ? N6 Ti1 C4 64.3(3) . . ? C3 Ti1 C4 38.0(3) . . ? O54 Ti1 C4 101.9(2) . . ? N41 Ti1 C5 145.4(3) . . ? N6 Ti1 C5 33.9(3) . . ? C3 Ti1 C5 65.8(3) . . ? O54 Ti1 C5 94.4(3) . . ? C4 Ti1 C5 33.3(3) . . ? N41 Ti1 P2 100.5(2) . . ? N6 Ti1 P2 126.7(2) . . ? C3 Ti1 P2 43.2(2) . . ? O54 Ti1 P2 102.12(17) . . ? C4 Ti1 P2 65.00(19) . . ? C5 Ti1 P2 98.3(3) . . ? C3 P2 C19 105.3(4) . . ? C3 P2 C24 117.6(4) . . ? C19 P2 C24 105.2(4) . . ? C3 P2 Ti1 54.8(3) . . ? C19 P2 Ti1 108.8(3) . . ? C24 P2 Ti1 145.9(3) . . ? C4 C3 C39 117.0(7) . . ? C4 C3 P2 109.5(5) . . ? C39 C3 P2 127.0(6) . . ? C4 C3 Ti1 81.8(5) . . ? C39 C3 Ti1 127.3(6) . . ? P2 C3 Ti1 82.0(3) . . ? C5 C4 C3 119.1(8) . . ? C5 C4 Ti1 74.7(5) . . ? C3 C4 Ti1 60.2(4) . . ? N6 C5 C4 118.6(8) . . ? N6 C5 C40 121.3(9) . . ? C4 C5 C40 119.9(9) . . ? N6 C5 Ti1 54.7(4) . . ? C4 C5 Ti1 72.0(5) . . ? C40 C5 Ti1 146.6(6) . . ? C5 N6 C7 120.7(7) . . ? C5 N6 Ti1 91.3(5) . . ? C7 N6 Ti1 146.2(6) . . ? C12 C7 C8 120.0(8) . . ? C12 C7 N6 121.0(8) . . ? C8 C7 N6 119.0(8) . . ? C9 C8 C7 117.3(9) . . ? C9 C8 C16 118.5(9) . . ? C7 C8 C16 124.1(9) . . ? C10 C9 C8 123.0(9) . . ? C9 C10 C11 118.0(9) . . ? C10 C11 C12 123.1(8) . . ? C11 C12 C7 118.6(8) . . ? C11 C12 C13 118.2(8) . . ? C7 C12 C13 122.9(8) . . ? C12 C13 C15 112.8(7) . . ? C12 C13 C14 109.5(8) . . ? C15 C13 C14 110.5(7) . . ? C8 C16 C17 113.7(8) . . ? C8 C16 C18 110.4(7) . . ? C17 C16 C18 107.8(7) . . ? C20 C19 P2 119.8(6) . . ? C23 C20 C21 111.7(8) . . ? C23 C20 C19 111.6(8) . . ? C21 C20 C19 109.9(7) . . ? C23 C20 C22 108.7(8) . . ? C21 C20 C22 108.8(8) . . ? C19 C20 C22 106.0(7) . . ? C29 C24 C25 118.9(9) . . ? C29 C24 P2 119.3(7) . . ? C25 C24 P2 120.9(7) . . ? C26 C25 C24 119.8(9) . . ? C26 C25 C33 117.6(9) . . ? C24 C25 C33 122.5(9) . . ? C27 C26 C25 123.1(11) . . ? C26 C27 C28 118.1(11) . . ? C26 C27 C36 125.1(13) . . ? C28 C27 C36 116.8(12) . . ? C27 C28 C29 122.5(11) . . ? C24 C29 C28 117.1(10) . . ? C24 C29 C30 123.5(9) . . ? C28 C29 C30 119.4(10) . . ? C32 C30 C29 111.9(8) . . ? C32 C30 C31 109.3(8) . . ? C29 C30 C31 109.5(8) . . ? C25 C33 C34 114.7(8) . . ? C25 C33 C35 108.0(7) . . ? C34 C33 C35 110.6(8) . . ? C37 C36 C38 125.8(11) . . ? C37 C36 C27 116.6(11) . . ? C38 C36 C27 113.8(11) . . ? C42 N41 Ti1 166.0(6) . . ? N41 C42 C43 122.0(8) . . ? N41 C42 C47 120.1(8) . . ? C43 C42 C47 117.8(8) . . ? C44 C43 C42 119.3(8) . . ? C44 C43 C51 120.0(8) . . ? C42 C43 C51 120.7(8) . . ? C43 C44 C45 123.3(9) . . ? C46 C45 C44 116.6(9) . . ? C47 C46 C45 123.2(9) . . ? C46 C47 C42 119.5(9) . . ? C46 C47 C48 119.0(9) . . ? C42 C47 C48 121.1(8) . . ? C47 C48 C49 113.8(8) . . ? C47 C48 C50 111.9(8) . . ? C49 C48 C50 109.2(8) . . ? C53 C51 C52 109.4(8) . . ? C53 C51 C43 116.4(7) . . ? C52 C51 C43 108.2(7) . . ? C55 O54 C57 112.3(6) . . ? C55 O54 Ti1 121.9(5) . . ? C57 O54 Ti1 125.6(5) . . ? O54 C55 C56 114.1(7) . . ? O54 C57 C58 112.4(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N41 Ti1 P2 C3 110.2(4) . . . . ? N6 Ti1 P2 C3 -20.1(4) . . . . ? O54 Ti1 P2 C3 -136.9(3) . . . . ? C4 Ti1 P2 C3 -39.3(3) . . . . ? C5 Ti1 P2 C3 -40.6(4) . . . . ? N41 Ti1 P2 C19 14.4(3) . . . . ? N6 Ti1 P2 C19 -115.9(3) . . . . ? C3 Ti1 P2 C19 -95.8(4) . . . . ? O54 Ti1 P2 C19 127.2(3) . . . . ? C4 Ti1 P2 C19 -135.2(3) . . . . ? C5 Ti1 P2 C19 -136.4(3) . . . . ? N41 Ti1 P2 C24 -161.6(6) . . . . ? N6 Ti1 P2 C24 68.1(6) . . . . ? C3 Ti1 P2 C24 88.2(6) . . . . ? O54 Ti1 P2 C24 -48.7(6) . . . . ? C4 Ti1 P2 C24 48.9(6) . . . . ? C5 Ti1 P2 C24 47.7(6) . . . . ? C19 P2 C3 C4 -179.3(6) . . . . ? C24 P2 C3 C4 -62.5(7) . . . . ? Ti1 P2 C3 C4 78.3(6) . . . . ? C19 P2 C3 C39 -28.9(8) . . . . ? C24 P2 C3 C39 87.9(8) . . . . ? Ti1 P2 C3 C39 -131.3(8) . . . . ? C19 P2 C3 Ti1 102.4(4) . . . . ? C24 P2 C3 Ti1 -140.8(4) . . . . ? N41 Ti1 C3 C4 166.5(4) . . . . ? N6 Ti1 C3 C4 52.8(4) . . . . ? O54 Ti1 C3 C4 -50.6(6) . . . . ? C5 Ti1 C3 C4 24.0(4) . . . . ? P2 Ti1 C3 C4 -111.2(5) . . . . ? N41 Ti1 C3 C39 48.7(8) . . . . ? N6 Ti1 C3 C39 -65.0(7) . . . . ? O54 Ti1 C3 C39 -168.4(6) . . . . ? C4 Ti1 C3 C39 -117.8(9) . . . . ? C5 Ti1 C3 C39 -93.8(7) . . . . ? P2 Ti1 C3 C39 131.0(8) . . . . ? N41 Ti1 C3 P2 -82.4(3) . . . . ? N6 Ti1 C3 P2 164.0(3) . . . . ? O54 Ti1 C3 P2 60.5(4) . . . . ? C4 Ti1 C3 P2 111.2(5) . . . . ? C5 Ti1 C3 P2 135.1(4) . . . . ? C39 C3 C4 C5 79.5(10) . . . . ? P2 C3 C4 C5 -126.7(7) . . . . ? Ti1 C3 C4 C5 -48.3(8) . . . . ? C39 C3 C4 Ti1 127.8(8) . . . . ? P2 C3 C4 Ti1 -78.5(4) . . . . ? N41 Ti1 C4 C5 113.4(6) . . . . ? N6 Ti1 C4 C5 19.3(5) . . . . ? C3 Ti1 C4 C5 137.5(7) . . . . ? O54 Ti1 C4 C5 -79.8(5) . . . . ? P2 Ti1 C4 C5 -177.8(5) . . . . ? N41 Ti1 C4 C3 -24.0(7) . . . . ? N6 Ti1 C4 C3 -118.2(5) . . . . ? O54 Ti1 C4 C3 142.7(4) . . . . ? C5 Ti1 C4 C3 -137.5(7) . . . . ? P2 Ti1 C4 C3 44.7(4) . . . . ? C3 C4 C5 N6 12.5(12) . . . . ? Ti1 C4 C5 N6 -29.7(7) . . . . ? C3 C4 C5 C40 -172.2(7) . . . . ? Ti1 C4 C5 C40 145.6(8) . . . . ? C3 C4 C5 Ti1 42.2(7) . . . . ? N41 Ti1 C5 N6 27.6(8) . . . . ? C3 Ti1 C5 N6 120.7(5) . . . . ? O54 Ti1 C5 N6 -107.2(5) . . . . ? C4 Ti1 C5 N6 147.8(8) . . . . ? P2 Ti1 C5 N6 149.9(5) . . . . ? N41 Ti1 C5 C4 -120.2(6) . . . . ? N6 Ti1 C5 C4 -147.8(8) . . . . ? C3 Ti1 C5 C4 -27.1(5) . . . . ? O54 Ti1 C5 C4 105.0(5) . . . . ? P2 Ti1 C5 C4 2.0(5) . . . . ? N41 Ti1 C5 C40 122.4(11) . . . . ? N6 Ti1 C5 C40 94.8(14) . . . . ? C3 Ti1 C5 C40 -144.5(13) . . . . ? O54 Ti1 C5 C40 -12.4(13) . . . . ? C4 Ti1 C5 C40 -117.4(15) . . . . ? P2 Ti1 C5 C40 -115.3(12) . . . . ? C4 C5 N6 C7 -156.0(8) . . . . ? C40 C5 N6 C7 28.7(12) . . . . ? Ti1 C5 N6 C7 168.7(8) . . . . ? C4 C5 N6 Ti1 35.2(8) . . . . ? C40 C5 N6 Ti1 -140.0(7) . . . . ? N41 Ti1 N6 C5 -163.3(5) . . . . ? C3 Ti1 N6 C5 -51.9(5) . . . . ? O54 Ti1 N6 C5 78.0(5) . . . . ? C4 Ti1 N6 C5 -18.9(5) . . . . ? P2 Ti1 N6 C5 -38.3(6) . . . . ? N41 Ti1 N6 C7 34.3(11) . . . . ? C3 Ti1 N6 C7 145.6(10) . . . . ? O54 Ti1 N6 C7 -84.4(10) . . . . ? C4 Ti1 N6 C7 178.6(11) . . . . ? C5 Ti1 N6 C7 -162.4(13) . . . . ? P2 Ti1 N6 C7 159.3(9) . . . . ? C5 N6 C7 C12 53.3(12) . . . . ? Ti1 N6 C7 C12 -147.2(8) . . . . ? C5 N6 C7 C8 -125.3(9) . . . . ? Ti1 N6 C7 C8 34.1(15) . . . . ? C12 C7 C8 C9 1.4(13) . . . . ? N6 C7 C8 C9 -180.0(7) . . . . ? C12 C7 C8 C16 -179.7(8) . . . . ? N6 C7 C8 C16 -1.0(13) . . . . ? C7 C8 C9 C10 -0.7(14) . . . . ? C16 C8 C9 C10 -179.7(8) . . . . ? C8 C9 C10 C11 0.4(15) . . . . ? C9 C10 C11 C12 -0.9(16) . . . . ? C10 C11 C12 C7 1.6(15) . . . . ? C10 C11 C12 C13 174.8(9) . . . . ? C8 C7 C12 C11 -1.8(13) . . . . ? N6 C7 C12 C11 179.5(8) . . . . ? C8 C7 C12 C13 -174.6(8) . . . . ? N6 C7 C12 C13 6.7(13) . . . . ? C11 C12 C13 C15 52.0(11) . . . . ? C7 C12 C13 C15 -135.2(8) . . . . ? C11 C12 C13 C14 -71.5(10) . . . . ? C7 C12 C13 C14 101.4(10) . . . . ? C9 C8 C16 C17 -55.3(11) . . . . ? C7 C8 C16 C17 125.7(10) . . . . ? C9 C8 C16 C18 66.0(10) . . . . ? C7 C8 C16 C18 -113.0(10) . . . . ? C3 P2 C19 C20 -171.1(7) . . . . ? C24 P2 C19 C20 64.0(8) . . . . ? Ti1 P2 C19 C20 -113.6(7) . . . . ? P2 C19 C20 C23 -75.5(9) . . . . ? P2 C19 C20 C21 49.0(10) . . . . ? P2 C19 C20 C22 166.4(7) . . . . ? C3 P2 C24 C29 130.5(7) . . . . ? C19 P2 C24 C29 -112.7(7) . . . . ? Ti1 P2 C24 C29 63.4(9) . . . . ? C3 P2 C24 C25 -59.8(8) . . . . ? C19 P2 C24 C25 57.0(8) . . . . ? Ti1 P2 C24 C25 -127.0(7) . . . . ? C29 C24 C25 C26 5.1(14) . . . . ? P2 C24 C25 C26 -164.6(7) . . . . ? C29 C24 C25 C33 -171.0(8) . . . . ? P2 C24 C25 C33 19.3(12) . . . . ? C24 C25 C26 C27 1.1(16) . . . . ? C33 C25 C26 C27 177.3(10) . . . . ? C25 C26 C27 C28 -6.4(17) . . . . ? C25 C26 C27 C36 176.4(10) . . . . ? C26 C27 C28 C29 5.9(17) . . . . ? C36 C27 C28 C29 -176.7(9) . . . . ? C25 C24 C29 C28 -5.4(13) . . . . ? P2 C24 C29 C28 164.4(7) . . . . ? C25 C24 C29 C30 173.5(8) . . . . ? P2 C24 C29 C30 -16.7(12) . . . . ? C27 C28 C29 C24 0.0(15) . . . . ? C27 C28 C29 C30 -178.9(9) . . . . ? C24 C29 C30 C32 125.5(9) . . . . ? C28 C29 C30 C32 -55.6(11) . . . . ? C24 C29 C30 C31 -113.1(10) . . . . ? C28 C29 C30 C31 65.7(11) . . . . ? C26 C25 C33 C34 36.8(13) . . . . ? C24 C25 C33 C34 -147.0(9) . . . . ? C26 C25 C33 C35 -87.0(11) . . . . ? C24 C25 C33 C35 89.2(11) . . . . ? C26 C27 C36 C37 98.6(18) . . . . ? C28 C27 C36 C37 -78.6(17) . . . . ? C26 C27 C36 C38 -101.9(17) . . . . ? C28 C27 C36 C38 80.9(17) . . . . ? N6 Ti1 N41 C42 90(2) . . . . ? C3 Ti1 N41 C42 -4(2) . . . . ? O54 Ti1 N41 C42 -155(2) . . . . ? C4 Ti1 N41 C42 11(3) . . . . ? C5 Ti1 N41 C42 74(2) . . . . ? P2 Ti1 N41 C42 -48(2) . . . . ? Ti1 N41 C42 C43 133(2) . . . . ? Ti1 N41 C42 C47 -44(3) . . . . ? N41 C42 C43 C44 -172.1(8) . . . . ? C47 C42 C43 C44 4.8(13) . . . . ? N41 C42 C43 C51 9.2(13) . . . . ? C47 C42 C43 C51 -174.0(8) . . . . ? C42 C43 C44 C45 -5.3(14) . . . . ? C51 C43 C44 C45 173.5(8) . . . . ? C43 C44 C45 C46 2.4(14) . . . . ? C44 C45 C46 C47 0.8(14) . . . . ? C45 C46 C47 C42 -1.0(15) . . . . ? C45 C46 C47 C48 -174.1(9) . . . . ? N41 C42 C47 C46 175.1(8) . . . . ? C43 C42 C47 C46 -1.8(13) . . . . ? N41 C42 C47 C48 -11.9(13) . . . . ? C43 C42 C47 C48 171.2(8) . . . . ? C46 C47 C48 C49 -40.4(12) . . . . ? C42 C47 C48 C49 146.6(8) . . . . ? C46 C47 C48 C50 84.1(11) . . . . ? C42 C47 C48 C50 -89.0(10) . . . . ? C44 C43 C51 C53 29.3(13) . . . . ? C42 C43 C51 C53 -152.0(8) . . . . ? C44 C43 C51 C52 -94.4(10) . . . . ? C42 C43 C51 C52 84.4(10) . . . . ? N41 Ti1 O54 C55 -2.0(6) . . . . ? N6 Ti1 O54 C55 119.4(6) . . . . ? C3 Ti1 O54 C55 -145.4(6) . . . . ? C4 Ti1 O54 C55 -174.6(6) . . . . ? C5 Ti1 O54 C55 152.6(6) . . . . ? P2 Ti1 O54 C55 -107.9(6) . . . . ? N41 Ti1 O54 C57 173.3(6) . . . . ? N6 Ti1 O54 C57 -65.2(6) . . . . ? C3 Ti1 O54 C57 29.9(7) . . . . ? C4 Ti1 O54 C57 0.8(6) . . . . ? C5 Ti1 O54 C57 -32.0(6) . . . . ? P2 Ti1 O54 C57 67.4(6) . . . . ? C57 O54 C55 C56 -75.2(9) . . . . ? Ti1 O54 C55 C56 100.7(8) . . . . ? C55 O54 C57 C58 -74.2(9) . . . . ? Ti1 O54 C57 C58 110.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.260 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.061