# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelx _audit_creation_date 2013-10-29T12:46:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 2_py_2' _chemical_formula_moiety 'C62 H102 N2 O2 Si4 Ti2, C5 H5 N' _chemical_formula_sum 'C67 H107 N3 O2 Si4 Ti2' _chemical_formula_weight 1194.71 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7134(6) _cell_length_b 16.0497(6) _cell_length_c 18.5403(6) _cell_angle_alpha 85.689(3) _cell_angle_beta 86.517(3) _cell_angle_gamma 66.630(4) _cell_volume 3733.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12809 _cell_measurement_theta_min 3.757 _cell_measurement_theta_max 71.348 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; crysalispro, agilent technologies, version 1.171.36.32 (release 02-08-2013 crysalis171 .net) (compiled aug 2 2013,16:46:58) empirical absorption correction using spherical harmonics, implemented in scale3 abspack scaling algorithm. ; _exptl_absorpt_correction_T_min 0.67895 _exptl_absorpt_correction_T_max 1 _shelx_estimated_absorpt_T_min 0.408 _shelx_estimated_absorpt_T_max 0.612 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source ; Enhance Ultra (Cu) X-ray source ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.1033 _diffrn_measurement_device_type 'xcalibur, eos, gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_number 22701 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.004 _diffrn_reflns_theta_max 71.48 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.958 _reflns_number_total 13931 _reflns_number_gt 12023 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; crysalispro, agilent technologies, version 1.171.36.32 (release 02-08-2013 crysalis171 .net) (compiled aug 2 2013,16:46:58) ; _computing_cell_refinement ; crysalispro, agilent technologies, version 1.171.36.32 (release 02-08-2013 crysalis171 .net) (compiled aug 2 2013,16:46:58) ; _computing_data_reduction ; crysalispro, agilent technologies, version 1.171.36.32 (release 02-08-2013 crysalis171 .net) (compiled aug 2 2013,16:46:58) ; _computing_structure_solution ; DIRDIF-08 (Beurskens et al., 2008) ; _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ortep-3 (farrugia, 1997)' _computing_publication_material ; shelxl-2013 (sheldrick, 2013), platon (spek, 2003), and wingx (farrugia, 2013) ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Atoms of the iPr group C29, C30, C31 and iPr CH3 groups C45, C46 and C51, C52 were positionally disordered over two sites. The disorder was modelled adequately and refinement proceeded normally. Restrain instructions (DELU, SIMU) were applied to iPr group C50>C52 to give the thermal parameters more chemically reasonable values. Each molecule cocrystallized with two disordered pyridine solvate molecules. One of which was included in the model, with the N3 atom assigned to the largest Q-peak, the remaining Q-peaks assigned to C100>C104 and refined anisotropically. The more disordered molecule of pyridine could not be modelled properly; therefore, this disorder was treated by using the SQUEEZE(van der Sluis & Spek, 1990) routine in PLATON (Spek, 2003). 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 'w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+3.1648P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13931 _refine_ls_number_parameters 769 _refine_ls_number_restraints 72 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.611 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0368(2) 0.02381(17) 0.23798(14) 0.0349(5) Uani 1 d . . C2 C 0.1295(2) 0.02244(18) 0.19657(14) 0.0363(5) Uani 1 d . . H2 H 0.1307 0.0374 0.1461 0.044 Uiso 1 calc . . C3 C 0.2180(2) -0.00383(17) 0.24029(15) 0.0360(5) Uani 1 d . . H3 H 0.287 -0.0077 0.2249 0.043 Uiso 1 calc . . C4 C 0.1859(2) -0.02363(16) 0.31203(14) 0.0338(5) Uani 1 d . . C5 C 0.0740(2) -0.00551(16) 0.31111(14) 0.0323(5) Uani 1 d . . C6 C 0.0410(2) -0.02179(17) 0.38287(15) 0.0360(5) Uani 1 d . . H6 H -0.0289 -0.014 0.3994 0.043 Uiso 1 calc . . C7 C 0.1314(2) -0.05156(18) 0.42465(15) 0.0382(5) Uani 1 d . . H7 H 0.1315 -0.0684 0.4749 0.046 Uiso 1 calc . . C8 C 0.2231(2) -0.05376(17) 0.38356(15) 0.0355(5) Uani 1 d . . C9 C -0.06144(19) 0.44946(16) 0.24858(14) 0.0327(5) Uani 1 d . . C10 C 0.0111(2) 0.40518(17) 0.30506(14) 0.0339(5) Uani 1 d . . H10 H -0.0095 0.3904 0.3526 0.041 Uiso 1 calc . . C11 C 0.1172(2) 0.38612(17) 0.28124(14) 0.0336(5) Uani 1 d . . H11 H 0.1787 0.3556 0.309 0.04 Uiso 1 calc . . C12 C 0.11528(19) 0.42119(16) 0.20762(14) 0.0316(5) Uani 1 d . . C13 C 0.00462(19) 0.46040(16) 0.18783(14) 0.0316(5) Uani 1 d . . C14 C 0.0019(2) 0.49408(17) 0.11438(15) 0.0374(5) Uani 1 d . . H14 H -0.0595 0.524 0.0865 0.045 Uiso 1 calc . . C15 C 0.1069(2) 0.47460(19) 0.09148(15) 0.0405(6) Uani 1 d . . H15 H 0.1271 0.4906 0.0443 0.049 Uiso 1 calc . . C16 C 0.1808(2) 0.42805(18) 0.14641(15) 0.0372(5) Uani 1 d . . C17 C -0.2008(3) 0.0632(3) 0.2624(2) 0.0581(8) Uani 1 d . . H17 H -0.1816 0.0229 0.3076 0.07 Uiso 1 calc . . C18 C -0.3005(3) 0.0554(4) 0.2364(3) 0.0888(15) Uani 1 d . . H18A H -0.2826 -0.0065 0.2217 0.133 Uiso 1 calc . . H18B H -0.3282 0.0987 0.1951 0.133 Uiso 1 calc . . H18C H -0.3546 0.069 0.2758 0.133 Uiso 1 calc . . C19 C -0.2267(3) 0.1591(3) 0.2861(3) 0.0813(13) Uani 1 d . . H19A H -0.1622 0.1627 0.3029 0.122 Uiso 1 calc . . H19B H -0.2807 0.1729 0.3255 0.122 Uiso 1 calc . . H19C H -0.2538 0.203 0.245 0.122 Uiso 1 calc . . C20 C -0.0492(3) -0.1091(2) 0.1935(2) 0.0667(10) Uani 1 d . . H20 H -0.1082 -0.1144 0.1676 0.08 Uiso 1 calc . . C21 C 0.0538(4) -0.1551(3) 0.1481(3) 0.0932(16) Uani 1 d . . H21A H 0.0485 -0.122 0.1009 0.14 Uiso 1 calc . . H21B H 0.0644 -0.2181 0.1412 0.14 Uiso 1 calc . . H21C H 0.1143 -0.1545 0.1734 0.14 Uiso 1 calc . . C22 C -0.0419(5) -0.1607(3) 0.2672(3) 0.0956(17) Uani 1 d . . H22A H -0.108 -0.1314 0.2956 0.143 Uiso 1 calc . . H22B H 0.0179 -0.1599 0.293 0.143 Uiso 1 calc . . H22C H -0.0311 -0.2237 0.2601 0.143 Uiso 1 calc . . C23 C -0.0978(3) 0.0697(3) 0.10322(19) 0.0575(8) Uani 1 d . . H23 H -0.025 0.0469 0.0799 0.069 Uiso 1 calc . . C24 C -0.1666(4) 0.0409(3) 0.0563(2) 0.0805(13) Uani 1 d . . H24A H -0.1403 -0.0256 0.0583 0.121 Uiso 1 calc . . H24B H -0.1627 0.0637 0.0061 0.121 Uiso 1 calc . . H24C H -0.2405 0.0662 0.0746 0.121 Uiso 1 calc . . C25 C -0.1376(4) 0.1733(3) 0.0993(2) 0.0828(14) Uani 1 d . . H25A H -0.0938 0.1916 0.1293 0.124 Uiso 1 calc . . H25B H -0.2118 0.1995 0.1171 0.124 Uiso 1 calc . . H25C H -0.1328 0.1954 0.049 0.124 Uiso 1 calc . . C26 C 0.4000(3) -0.2408(2) 0.4033(2) 0.0612(9) Uani 1 d . . H26 H 0.4772 -0.2726 0.4139 0.073 Uiso 1 calc . . C27 C 0.3386(5) -0.2790(3) 0.4584(3) 0.0987(17) Uani 1 d . . H27A H 0.3489 -0.2651 0.5072 0.148 Uiso 1 calc . . H27B H 0.3648 -0.345 0.4552 0.148 Uiso 1 calc . . H27C H 0.2628 -0.2513 0.448 0.148 Uiso 1 calc . . C28 C 0.3863(4) -0.2625(3) 0.3275(3) 0.0854(14) Uani 1 d . . H28A H 0.4272 -0.2388 0.2929 0.128 Uiso 1 calc . . H28B H 0.3109 -0.2342 0.316 0.128 Uiso 1 calc . . H28C H 0.4118 -0.3285 0.3246 0.128 Uiso 1 calc . . C29A C 0.3917(12) -0.0829(12) 0.5015(7) 0.065(3) Uani 0.51(3) d A 1 H29A H 0.4387 -0.054 0.4775 0.078 Uiso 0.51(3) calc A 1 C30A C 0.3305(15) -0.0062(8) 0.5309(8) 0.084(4) Uani 0.51(3) d A 1 H30A H 0.2727 0.0291 0.4985 0.126 Uiso 0.51(3) calc A 1 H30B H 0.3729 0.0291 0.5386 0.126 Uiso 0.51(3) calc A 1 H30C H 0.3006 -0.0198 0.5774 0.126 Uiso 0.51(3) calc A 1 C31A C 0.4847(19) -0.1575(13) 0.5355(12) 0.089(6) Uani 0.51(3) d A 1 H31A H 0.5162 -0.2066 0.5021 0.133 Uiso 0.51(3) calc A 1 H31B H 0.4612 -0.181 0.5805 0.133 Uiso 0.51(3) calc A 1 H31C H 0.5377 -0.1338 0.5461 0.133 Uiso 0.51(3) calc A 1 C29B C 0.3629(12) -0.1081(9) 0.5139(7) 0.054(3) Uani 0.49(3) d A 2 H29B H 0.3262 -0.1501 0.5279 0.065 Uiso 0.49(3) calc A 2 C30B C 0.3004(10) -0.0403(13) 0.5490(6) 0.077(4) Uani 0.49(3) d A 2 H30D H 0.234 -0.0097 0.5233 0.116 Uiso 0.49(3) calc A 2 H30E H 0.3344 0.0024 0.5533 0.116 Uiso 0.49(3) calc A 2 H30F H 0.2848 -0.0619 0.5975 0.116 Uiso 0.49(3) calc A 2 C31B C 0.4727(18) -0.1678(18) 0.5489(14) 0.108(8) Uani 0.49(3) d A 2 H31D H 0.5132 -0.2179 0.518 0.162 Uiso 0.49(3) calc A 2 H31E H 0.4599 -0.1926 0.5968 0.162 Uiso 0.49(3) calc A 2 H31F H 0.5131 -0.1301 0.5537 0.162 Uiso 0.49(3) calc A 2 C32 C 0.4531(3) -0.0817(2) 0.3434(2) 0.0598(9) Uani 1 d . . H32 H 0.4406 -0.0995 0.2953 0.072 Uiso 1 calc . . C33 C 0.5722(3) -0.1356(3) 0.3566(3) 0.0883(15) Uani 1 d . . H33A H 0.5872 -0.2007 0.3618 0.132 Uiso 1 calc . . H33B H 0.591 -0.1165 0.4008 0.132 Uiso 1 calc . . H33C H 0.6143 -0.124 0.3154 0.132 Uiso 1 calc . . C34 C 0.4283(3) 0.0185(3) 0.3341(3) 0.0719(11) Uani 1 d . . H34A H 0.3525 0.0518 0.3252 0.108 Uiso 1 calc . . H34B H 0.4704 0.0301 0.2929 0.108 Uiso 1 calc . . H34C H 0.4459 0.039 0.3781 0.108 Uiso 1 calc . . C35 C -0.2780(2) 0.5011(2) 0.17981(18) 0.0444(6) Uani 1 d . . H35 H -0.2432 0.5219 0.1374 0.053 Uiso 1 calc . . C36 C -0.2649(3) 0.4042(2) 0.1656(2) 0.0603(9) Uani 1 d . . H36A H -0.1893 0.364 0.1657 0.09 Uiso 1 calc . . H36B H -0.2936 0.4042 0.1185 0.09 Uiso 1 calc . . H36C H -0.3035 0.3826 0.2036 0.09 Uiso 1 calc . . C37 C -0.3965(3) 0.5646(2) 0.1791(2) 0.0610(9) Uani 1 d . . H37A H -0.4046 0.6265 0.1879 0.091 Uiso 1 calc . . H37B H -0.4356 0.5435 0.217 0.091 Uiso 1 calc . . H37C H -0.4248 0.5644 0.1318 0.091 Uiso 1 calc . . C38 C -0.2515(2) 0.4645(2) 0.35091(18) 0.0493(7) Uani 1 d . . H38 H -0.2056 0.4704 0.3884 0.059 Uiso 1 calc . . C39 C -0.2338(3) 0.3641(2) 0.3544(2) 0.0699(11) Uani 1 d . . H39A H -0.1604 0.3277 0.339 0.105 Uiso 1 calc . . H39B H -0.2827 0.3554 0.3222 0.105 Uiso 1 calc . . H39C H -0.247 0.3449 0.4041 0.105 Uiso 1 calc . . C40 C -0.3666(3) 0.5209(3) 0.3757(2) 0.0727(11) Uani 1 d . . H40A H -0.3785 0.5854 0.3739 0.109 Uiso 1 calc . . H40B H -0.3791 0.501 0.4255 0.109 Uiso 1 calc . . H40C H -0.4157 0.5122 0.3437 0.109 Uiso 1 calc . . C41 C -0.2356(2) 0.63341(19) 0.27213(18) 0.0459(6) Uani 1 d . . H41 H -0.3138 0.6661 0.2814 0.055 Uiso 1 calc . . C42 C -0.1798(3) 0.6467(3) 0.3366(2) 0.0656(9) Uani 1 d . . H42A H -0.1988 0.6177 0.3805 0.098 Uiso 1 calc . . H42B H -0.2021 0.7118 0.343 0.098 Uiso 1 calc . . H42C H -0.1026 0.6191 0.3277 0.098 Uiso 1 calc . . C43 C -0.2057(3) 0.6787(2) 0.2037(2) 0.0584(8) Uani 1 d . . H43A H -0.2414 0.6704 0.1623 0.088 Uiso 1 calc . . H43B H -0.1285 0.651 0.1948 0.088 Uiso 1 calc . . H43C H -0.2278 0.7438 0.2101 0.088 Uiso 1 calc . . C44A C 0.3477(4) 0.5106(4) 0.1263(3) 0.0836(15) Uani 0.35(5) d B 1 H44A H 0.4243 0.5005 0.1282 0.1 Uiso 0.35(5) calc B 1 C45A C 0.284(4) 0.592(4) 0.071(4) 0.130(17) Uani 0.35(5) d B 1 H45A H 0.3019 0.5728 0.0215 0.195 Uiso 0.35(5) calc B 1 H45B H 0.3041 0.6438 0.0769 0.195 Uiso 0.35(5) calc B 1 H45C H 0.2077 0.6111 0.081 0.195 Uiso 0.35(5) calc B 1 C46A C 0.267(5) 0.5783(19) 0.198(4) 0.139(18) Uani 0.35(5) d B 1 H46A H 0.2916 0.5464 0.2448 0.208 Uiso 0.35(5) calc B 1 H46B H 0.1929 0.5883 0.1926 0.208 Uiso 0.35(5) calc B 1 H46C H 0.2742 0.637 0.1954 0.208 Uiso 0.35(5) calc B 1 C44B C 0.3477(4) 0.5106(4) 0.1263(3) 0.0836(15) Uani 0.65(5) d B 2 H44B H 0.4256 0.4926 0.1321 0.1 Uiso 0.65(5) calc B 2 C45B C 0.3265(19) 0.5493(15) 0.0462(8) 0.090(5) Uani 0.65(5) d B 2 H45D H 0.3735 0.5041 0.0134 0.136 Uiso 0.65(5) calc B 2 H45E H 0.3403 0.6049 0.0393 0.136 Uiso 0.65(5) calc B 2 H45F H 0.2523 0.5634 0.0356 0.136 Uiso 0.65(5) calc B 2 C46B C 0.2969(14) 0.5750(12) 0.1791(12) 0.091(4) Uani 0.65(5) d B 2 H46D H 0.3129 0.5451 0.2276 0.136 Uiso 0.65(5) calc B 2 H46E H 0.2199 0.6004 0.173 0.136 Uiso 0.65(5) calc B 2 H46F H 0.3227 0.624 0.1733 0.136 Uiso 0.65(5) calc B 2 C47 C 0.3811(2) 0.3494(2) 0.2340(2) 0.0535(8) Uani 1 d . . H47 H 0.3275 0.3848 0.271 0.064 Uiso 1 calc . . C48 C 0.3913(3) 0.2508(3) 0.2471(3) 0.0728(12) Uani 1 d . . H48A H 0.3243 0.247 0.236 0.109 Uiso 1 calc . . H48B H 0.4073 0.231 0.2979 0.109 Uiso 1 calc . . H48C H 0.4488 0.2116 0.2158 0.109 Uiso 1 calc . . C49 C 0.4858(3) 0.3557(3) 0.2514(3) 0.0786(13) Uani 1 d . . H49A H 0.4791 0.4188 0.243 0.118 Uiso 1 calc . . H49B H 0.5434 0.3165 0.2201 0.118 Uiso 1 calc . . H49C H 0.5019 0.336 0.3022 0.118 Uiso 1 calc . . C50A C 0.3962(4) 0.3153(4) 0.0709(3) 0.0934(16) Uani 0.20(3) d B 1 H50A H 0.429 0.2537 0.096 0.112 Uiso 0.20(3) calc B 1 C51A C 0.357(4) 0.309(4) 0.021(3) 0.108(13) Uani 0.20(3) d B 1 H51A H 0.2988 0.2896 0.0354 0.162 Uiso 0.20(3) calc B 1 H51B H 0.4089 0.2648 -0.0099 0.162 Uiso 0.20(3) calc B 1 H51C H 0.3277 0.3686 -0.0056 0.162 Uiso 0.20(3) calc B 1 C52A C 0.503(2) 0.356(4) 0.043(2) 0.098(10) Uani 0.20(3) d B 1 H52A H 0.5455 0.3509 0.0852 0.148 Uiso 0.20(3) calc B 1 H52B H 0.4714 0.419 0.0247 0.148 Uiso 0.20(3) calc B 1 H52C H 0.5488 0.3179 0.0055 0.148 Uiso 0.20(3) calc B 1 C50B C 0.3962(4) 0.3153(4) 0.0709(3) 0.0934(16) Uani 0.80(3) d B 2 H50B H 0.3923 0.2576 0.0922 0.112 Uiso 0.80(3) calc B 2 C51B C 0.3395(12) 0.3324(10) -0.0012(6) 0.095(3) Uani 0.80(3) d B 2 H51D H 0.2642 0.3447 0.0085 0.142 Uiso 0.80(3) calc B 2 H51E H 0.3722 0.2786 -0.0298 0.142 Uiso 0.80(3) calc B 2 H51F H 0.3462 0.3849 -0.0283 0.142 Uiso 0.80(3) calc B 2 C52B C 0.5159(6) 0.2927(15) 0.0619(7) 0.121(5) Uani 0.80(3) d B 2 H52D H 0.5468 0.2825 0.1097 0.182 Uiso 0.80(3) calc B 2 H52E H 0.5272 0.3435 0.0355 0.182 Uiso 0.80(3) calc B 2 H52F H 0.5502 0.2377 0.0349 0.182 Uiso 0.80(3) calc B 2 C53 C 0.1619(3) 0.1890(2) 0.41075(17) 0.0465(7) Uani 1 d . . H53 H 0.2186 0.1849 0.3773 0.056 Uiso 1 calc . . C54 C 0.1630(3) 0.2176(3) 0.4787(2) 0.0623(9) Uani 1 d . . H54 H 0.2194 0.2331 0.4917 0.075 Uiso 1 calc . . C55 C 0.0808(4) 0.2235(3) 0.52772(19) 0.0658(10) Uani 1 d . . H55 H 0.0801 0.2428 0.575 0.079 Uiso 1 calc . . C56 C 0.0005(3) 0.2010(2) 0.50715(19) 0.0594(9) Uani 1 d . . H56 H -0.0567 0.2043 0.54 0.071 Uiso 1 calc . . C57 C 0.0041(3) 0.1737(2) 0.43814(17) 0.0460(6) Uani 1 d . . H57 H -0.0525 0.1593 0.4241 0.055 Uiso 1 calc . . C58 C 0.1733(3) 0.2103(2) 0.08031(17) 0.0530(7) Uani 1 d . . H58 H 0.226 0.1791 0.1148 0.064 Uiso 1 calc . . C59 C 0.1930(4) 0.1864(3) 0.0094(2) 0.0725(11) Uani 1 d . . H59 H 0.2584 0.1395 -0.0045 0.087 Uiso 1 calc . . C60 C 0.1179(4) 0.2305(3) -0.04063(19) 0.0713(11) Uani 1 d . . H60 H 0.1307 0.2151 -0.0898 0.086 Uiso 1 calc . . C61 C 0.0242(4) 0.2970(2) -0.01923(19) 0.0623(10) Uani 1 d . . H61 H -0.0294 0.328 -0.0531 0.075 Uiso 1 calc . . C62 C 0.0086(3) 0.3185(2) 0.05246(17) 0.0489(7) Uani 1 d . . H62 H -0.0566 0.365 0.0671 0.059 Uiso 1 calc . . N1 N 0.08311(18) 0.16645(14) 0.38978(12) 0.0348(4) Uani 1 d . . N2 N 0.08199(19) 0.27623(15) 0.10232(12) 0.0377(5) Uani 1 d . . O1 O 0.16888(13) 0.19621(11) 0.24548(10) 0.0331(4) Uani 1 d . . O2 O -0.02658(13) 0.23738(12) 0.24616(10) 0.0339(4) Uani 1 d . . Si1 Si -0.08204(6) 0.01737(5) 0.19921(4) 0.04210(18) Uani 1 d . . Si2 Si 0.36275(6) -0.11466(5) 0.41064(4) 0.04251(18) Uani 1 d . . Si3 Si -0.20869(5) 0.50887(5) 0.26234(4) 0.03652(16) Uani 1 d . . Si4 Si 0.32533(6) 0.40243(6) 0.14277(5) 0.0484(2) Uani 1 d . . Ti1 Ti 0.08484(3) 0.13380(3) 0.27790(2) 0.03005(11) Uani 1 d . . Ti2 Ti 0.05695(3) 0.30184(3) 0.21636(2) 0.02982(11) Uani 1 d . . C104 C 0.1587(7) 0.4467(5) 0.4601(4) 0.115(2) Uani 1 d . . H104 H 0.1083 0.4248 0.4819 0.138 Uiso 1 calc . . C105 C 0.2551(7) 0.3933(5) 0.4609(4) 0.118(2) Uani 1 d . . H105 H 0.2752 0.3325 0.4803 0.142 Uiso 1 calc . . C103 C 0.1220(8) 0.5302(7) 0.4315(6) 0.155(3) Uani 1 d . . H103 H 0.0482 0.5676 0.4328 0.186 Uiso 1 calc . . C101 C 0.3086(9) 0.5010(6) 0.4057(6) 0.151(3) Uani 1 d . . H101 H 0.3667 0.5168 0.3901 0.182 Uiso 1 calc . . C100 C 0.3231(9) 0.4212(6) 0.4361(5) 0.142(3) Uani 1 d . . H100 H 0.3949 0.3793 0.4396 0.17 Uiso 1 calc . . N3 N 0.2012(12) 0.5634(6) 0.3972(6) 0.209(4) Uani 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 C1 0.0346(12) 0.0290(12) 0.0436(13) -0.0044(10) -0.0051(10) -0.0141(10) C2 0.0400(13) 0.0337(13) 0.0382(13) -0.0069(10) -0.0015(10) -0.0169(11) C3 0.0311(12) 0.0314(12) 0.0438(14) -0.0068(10) 0.0017(10) -0.0101(10) C4 0.0310(12) 0.0262(11) 0.0430(13) -0.0008(10) -0.0012(10) -0.0101(10) C5 0.0331(12) 0.0240(11) 0.0433(13) 0.0000(9) -0.0043(10) -0.0149(10) C6 0.0325(12) 0.0317(12) 0.0462(14) -0.0015(10) 0.0011(10) -0.0158(10) C7 0.0405(14) 0.0346(13) 0.0406(13) 0.0031(10) -0.0042(11) -0.0167(11) C8 0.0316(12) 0.0303(12) 0.0445(14) 0.0010(10) -0.0069(10) -0.0119(10) C9 0.0273(11) 0.0253(11) 0.0443(13) -0.0017(9) -0.0028(10) -0.0088(9) C10 0.0355(13) 0.0299(12) 0.0359(12) -0.0033(9) -0.0025(10) -0.0122(10) C11 0.0318(12) 0.0299(12) 0.0396(13) -0.0015(10) -0.0092(10) -0.0115(10) C12 0.0264(11) 0.0278(11) 0.0445(13) 0.0032(9) -0.0085(9) -0.0144(9) C13 0.0264(11) 0.0252(11) 0.0446(13) 0.0038(9) -0.0082(9) -0.0116(9) C14 0.0348(13) 0.0303(12) 0.0459(14) 0.0075(10) -0.0112(10) -0.0119(10) C15 0.0434(14) 0.0384(14) 0.0416(14) 0.0081(11) -0.0058(11) -0.0193(12) C16 0.0301(12) 0.0375(13) 0.0467(14) 0.0060(11) -0.0058(10) -0.0172(11) C17 0.0398(16) 0.067(2) 0.076(2) -0.0022(17) -0.0085(15) -0.0305(16) C18 0.052(2) 0.127(4) 0.109(4) -0.015(3) -0.009(2) -0.056(3) C19 0.049(2) 0.069(3) 0.129(4) -0.028(3) 0.020(2) -0.0260(19) C20 0.080(3) 0.0498(19) 0.085(3) -0.0026(17) -0.031(2) -0.0369(19) C21 0.096(3) 0.052(2) 0.127(4) -0.032(3) -0.023(3) -0.018(2) C22 0.145(5) 0.054(2) 0.110(4) 0.016(2) -0.040(3) -0.061(3) C23 0.065(2) 0.064(2) 0.0544(18) 0.0036(15) -0.0212(15) -0.0352(17) C24 0.111(4) 0.083(3) 0.068(2) 0.001(2) -0.037(2) -0.055(3) C25 0.123(4) 0.070(3) 0.075(3) 0.021(2) -0.047(3) -0.057(3) C26 0.0484(18) 0.0363(16) 0.092(3) 0.0039(16) -0.0148(17) -0.0085(14) C27 0.108(4) 0.066(3) 0.128(5) 0.021(3) -0.010(3) -0.044(3) C28 0.090(3) 0.045(2) 0.113(4) -0.023(2) -0.014(3) -0.014(2) C29A 0.068(6) 0.069(7) 0.056(5) -0.001(5) -0.020(4) -0.023(5) C30A 0.128(10) 0.066(6) 0.065(6) -0.002(5) -0.033(6) -0.042(6) C31A 0.122(15) 0.067(7) 0.073(10) 0.004(6) -0.058(10) -0.026(7) C29B 0.058(6) 0.053(5) 0.050(5) 0.007(4) -0.022(4) -0.018(4) C30B 0.092(7) 0.091(10) 0.051(5) -0.009(5) -0.016(5) -0.036(6) C31B 0.059(7) 0.161(19) 0.060(7) 0.025(8) -0.029(5) 0.001(9) C32 0.0359(15) 0.0484(18) 0.093(3) 0.0003(17) -0.0040(15) -0.0149(14) C33 0.0357(18) 0.072(3) 0.148(5) 0.005(3) -0.003(2) -0.0134(18) C34 0.0498(19) 0.055(2) 0.114(3) 0.006(2) -0.007(2) -0.0254(17) C35 0.0318(13) 0.0423(15) 0.0606(17) 0.0017(12) -0.0101(12) -0.0158(12) C36 0.0514(18) 0.0472(18) 0.085(2) -0.0082(16) -0.0179(17) -0.0196(15) C37 0.0362(16) 0.0531(19) 0.091(3) -0.0017(17) -0.0190(16) -0.0127(14) C38 0.0388(15) 0.0423(16) 0.0597(18) -0.0003(13) 0.0061(13) -0.0099(12) C39 0.069(2) 0.0445(18) 0.085(3) 0.0058(17) 0.028(2) -0.0160(16) C40 0.051(2) 0.063(2) 0.088(3) -0.001(2) 0.0243(19) -0.0085(17) C41 0.0354(14) 0.0319(13) 0.0657(18) -0.0053(12) -0.0026(12) -0.0077(11) C42 0.067(2) 0.053(2) 0.080(2) -0.0120(17) -0.0140(19) -0.0241(17) C43 0.061(2) 0.0310(14) 0.080(2) 0.0032(14) -0.0047(17) -0.0146(14) C44A 0.074(3) 0.088(3) 0.111(4) 0.037(3) -0.026(3) -0.059(3) C45A 0.10(2) 0.13(3) 0.16(3) 0.08(3) -0.03(2) -0.07(2) C46A 0.16(3) 0.043(10) 0.24(4) -0.012(15) -0.04(3) -0.061(15) C44B 0.074(3) 0.088(3) 0.111(4) 0.037(3) -0.026(3) -0.059(3) C45B 0.096(9) 0.094(9) 0.101(7) 0.048(6) -0.017(6) -0.066(7) C46B 0.083(7) 0.065(7) 0.138(10) 0.024(6) -0.022(6) -0.046(5) C47 0.0334(14) 0.0566(19) 0.078(2) 0.0125(16) -0.0187(14) -0.0259(14) C48 0.0445(18) 0.058(2) 0.113(3) 0.024(2) -0.0217(19) -0.0202(16) C49 0.049(2) 0.088(3) 0.109(3) 0.021(3) -0.031(2) -0.039(2) C50A 0.051(2) 0.137(5) 0.083(3) -0.028(3) 0.007(2) -0.025(3) C51A 0.079(18) 0.15(3) 0.09(2) -0.09(2) 0.028(13) -0.039(19) C52A 0.036(10) 0.14(3) 0.094(17) -0.021(18) 0.028(10) -0.015(12) C50B 0.051(2) 0.137(5) 0.083(3) -0.028(3) 0.007(2) -0.025(3) C51B 0.086(5) 0.133(7) 0.064(5) -0.015(5) 0.007(4) -0.041(5) C52B 0.054(3) 0.176(14) 0.121(7) -0.047(9) 0.027(4) -0.027(5) C53 0.0508(16) 0.0488(16) 0.0473(15) 0.0038(12) -0.0127(12) -0.0271(14) C54 0.079(2) 0.068(2) 0.0558(19) -0.0025(16) -0.0173(17) -0.043(2) C55 0.100(3) 0.060(2) 0.0461(17) -0.0104(15) -0.0066(18) -0.039(2) C56 0.077(2) 0.0551(19) 0.0516(18) -0.0136(15) 0.0129(16) -0.0325(18) C57 0.0500(16) 0.0413(15) 0.0509(16) -0.0066(12) 0.0035(13) -0.0222(13) C58 0.0595(19) 0.0487(17) 0.0432(16) -0.0028(13) 0.0025(13) -0.0139(15) C59 0.089(3) 0.066(2) 0.053(2) -0.0145(17) 0.0132(19) -0.021(2) C60 0.128(4) 0.058(2) 0.0403(17) -0.0049(15) -0.0012(19) -0.050(2) C61 0.102(3) 0.0493(18) 0.0489(17) 0.0060(14) -0.0251(18) -0.042(2) C62 0.0624(19) 0.0413(15) 0.0479(16) 0.0032(12) -0.0183(14) -0.0244(14) N1 0.0405(11) 0.0258(10) 0.0388(11) 0.0014(8) -0.0057(9) -0.0137(9) N2 0.0455(12) 0.0325(11) 0.0377(11) 0.0024(9) -0.0037(9) -0.0185(10) O1 0.0259(8) 0.0296(8) 0.0429(9) 0.0047(7) -0.0045(7) -0.0105(7) O2 0.0260(8) 0.0308(9) 0.0449(9) 0.0003(7) -0.0043(7) -0.0114(7) Si1 0.0421(4) 0.0400(4) 0.0522(4) -0.0008(3) -0.0138(3) -0.0233(3) Si2 0.0351(4) 0.0339(4) 0.0537(4) 0.0000(3) -0.0121(3) -0.0073(3) Si3 0.0264(3) 0.0289(3) 0.0516(4) -0.0001(3) -0.0029(3) -0.0083(3) Si4 0.0316(4) 0.0609(5) 0.0575(5) 0.0043(4) -0.0027(3) -0.0244(4) Ti1 0.0288(2) 0.0265(2) 0.0360(2) 0.00040(16) -0.00404(16) -0.01202(17) Ti2 0.0277(2) 0.0270(2) 0.0350(2) 0.00194(16) -0.00441(16) -0.01125(17) C104 0.143(6) 0.108(5) 0.110(5) -0.008(4) -0.010(4) -0.066(5) C105 0.129(6) 0.106(5) 0.116(5) 0.022(4) 0.000(4) -0.048(5) C103 0.142(7) 0.119(7) 0.196(10) -0.027(6) -0.041(7) -0.035(6) C101 0.177(9) 0.107(6) 0.190(9) -0.046(6) 0.030(7) -0.076(6) C100 0.178(9) 0.118(6) 0.133(6) -0.005(5) -0.022(6) -0.060(6) N3 0.295(14) 0.106(6) 0.226(10) -0.021(6) -0.002(10) -0.079(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.438(4) . ? C1 C5 1.455(4) . ? C1 Si1 1.862(3) . ? C1 Ti1 2.297(3) . ? C2 C3 1.404(4) . ? C2 Ti1 2.295(3) . ? C2 H2 0.95 . ? C3 C4 1.428(4) . ? C3 Ti1 2.362(2) . ? C3 H3 0.95 . ? C4 C8 1.429(4) . ? C4 C5 1.446(3) . ? C4 Ti1 2.407(2) . ? C5 C6 1.418(4) . ? C5 Ti1 2.334(2) . ? C6 C7 1.400(4) . ? C6 H6 0.95 . ? C7 C8 1.419(4) . ? C7 H7 0.95 . ? C8 Si2 1.853(3) . ? C9 C10 1.430(4) . ? C9 C13 1.447(4) . ? C9 Si3 1.870(2) . ? C9 Ti2 2.377(2) . ? C10 C11 1.413(4) . ? C10 Ti2 2.304(2) . ? C10 H10 0.95 . ? C11 C12 1.435(4) . ? C11 Ti2 2.283(2) . ? C11 H11 0.95 . ? C12 C16 1.429(4) . ? C12 C13 1.452(3) . ? C12 Ti2 2.343(2) . ? C13 C14 1.424(4) . ? C13 Ti2 2.380(2) . ? C14 C15 1.393(4) . ? C14 H14 0.95 . ? C15 C16 1.426(4) . ? C15 H15 0.95 . ? C16 Si4 1.855(3) . ? C17 C19 1.528(5) . ? C17 C18 1.531(5) . ? C17 Si1 1.875(4) . ? C17 H17 1 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C22 1.530(6) . ? C20 C21 1.540(7) . ? C20 Si1 1.906(4) . ? C20 H20 1 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C25 1.529(5) . ? C23 C24 1.539(5) . ? C23 Si1 1.897(3) . ? C23 H23 1 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 C28 1.512(6) . ? C26 C27 1.529(6) . ? C26 Si2 1.895(3) . ? C26 H26 1 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29A C30A 1.320(17) . ? C29A C31A 1.49(2) . ? C29A Si2 1.904(11) . ? C29A H29A 1 . ? C30A H30A 0.98 . ? C30A H30B 0.98 . ? C30A H30C 0.98 . ? C31A H31A 0.98 . ? C31A H31B 0.98 . ? C31A H31C 0.98 . ? C29B C30B 1.281(17) . ? C29B C31B 1.58(2) . ? C29B Si2 1.926(11) . ? C29B H29B 1 . ? C30B H30D 0.98 . ? C30B H30E 0.98 . ? C30B H30F 0.98 . ? C31B H31D 0.98 . ? C31B H31E 0.98 . ? C31B H31F 0.98 . ? C32 C34 1.505(5) . ? C32 C33 1.541(5) . ? C32 Si2 1.898(4) . ? C32 H32 1 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.533(4) . ? C35 C37 1.538(4) . ? C35 Si3 1.887(3) . ? C35 H35 1 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.528(5) . ? C38 C40 1.538(4) . ? C38 Si3 1.894(3) . ? C38 H38 1 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C42 1.530(5) . ? C41 C43 1.531(5) . ? C41 Si3 1.904(3) . ? C41 H41 1 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44A C46A 1.80(7) . ? C44A C45A 1.59(3) . ? C44A Si4 1.880(4) . ? C44A H44A 1 . ? C45A H45A 0.98 . ? C45A H45B 0.98 . ? C45A H45C 0.98 . ? C46A H46A 0.98 . ? C46A H46B 0.98 . ? C46A H46C 0.98 . ? C45B H45D 0.98 . ? C45B H45E 0.98 . ? C45B H45F 0.98 . ? C46B H46D 0.98 . ? C46B H46E 0.98 . ? C46B H46F 0.98 . ? C47 C49 1.534(4) . ? C47 C48 1.534(5) . ? C47 Si4 1.897(3) . ? C47 H47 1 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50A C51A 1.13(5) . ? C50A C52A 1.85(4) . ? C50A Si4 1.928(5) . ? C50A H50A 1 . ? C51A H51A 0.98 . ? C51A H51B 0.98 . ? C51A H51C 0.98 . ? C52A H52A 0.98 . ? C52A H52B 0.98 . ? C52A H52C 0.98 . ? C51B H51D 0.98 . ? C51B H51E 0.98 . ? C51B H51F 0.98 . ? C52B H52D 0.98 . ? C52B H52E 0.98 . ? C52B H52F 0.98 . ? C53 N1 1.354(4) . ? C53 C54 1.376(5) . ? C53 H53 0.95 . ? C54 C55 1.381(6) . ? C54 H54 0.95 . ? C55 C56 1.369(6) . ? C55 H55 0.95 . ? C56 C57 1.375(5) . ? C56 H56 0.95 . ? C57 N1 1.337(4) . ? C57 H57 0.95 . ? C58 N2 1.344(4) . ? C58 C59 1.377(5) . ? C58 H58 0.95 . ? C59 C60 1.365(6) . ? C59 H59 0.95 . ? C60 C61 1.364(6) . ? C60 H60 0.95 . ? C61 C62 1.381(5) . ? C61 H61 0.95 . ? C62 N2 1.344(4) . ? C62 H62 0.95 . ? N1 Ti1 2.174(2) . ? N2 Ti2 2.165(2) . ? O1 Ti2 1.8495(17) . ? O1 Ti1 1.8531(17) . ? O2 Ti1 1.8416(17) . ? O2 Ti2 1.8615(17) . ? Ti1 Ti2 2.7376(6) . ? C104 C105 1.259(10) . ? C104 C103 1.311(11) . ? C104 H104 0.95 . ? C105 C100 1.238(10) . ? C105 H105 0.95 . ? C103 N3 1.481(13) . ? C103 H103 0.95 . ? C101 C100 1.304(11) . ? C101 N3 1.425(13) . ? C101 H101 0.95 . ? C100 H100 0.95 . ? 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 C2 C1 C5 104.3(2) . . ? C2 C1 Si1 124.8(2) . . ? C5 C1 Si1 126.59(19) . . ? C2 C1 Ti1 71.67(14) . . ? C5 C1 Ti1 73.05(14) . . ? Si1 C1 Ti1 137.60(13) . . ? C3 C2 C1 111.4(2) . . ? C3 C2 Ti1 75.06(15) . . ? C1 C2 Ti1 71.83(14) . . ? C3 C2 H2 124.3 . . ? C1 C2 H2 124.3 . . ? Ti1 C2 H2 120.4 . . ? C2 C3 C4 107.8(2) . . ? C2 C3 Ti1 69.88(14) . . ? C4 C3 Ti1 74.31(14) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Ti1 C3 H3 121.4 . . ? C8 C4 C3 143.4(2) . . ? C8 C4 C5 109.4(2) . . ? C3 C4 C5 107.2(2) . . ? C8 C4 Ti1 122.48(18) . . ? C3 C4 Ti1 70.84(14) . . ? C5 C4 Ti1 69.50(13) . . ? C6 C5 C4 107.3(2) . . ? C6 C5 C1 143.4(2) . . ? C4 C5 C1 109.3(2) . . ? C6 C5 Ti1 119.37(18) . . ? C4 C5 Ti1 75.03(14) . . ? C1 C5 Ti1 70.32(13) . . ? C7 C6 C5 106.6(2) . . ? C7 C6 H6 126.7 . . ? C5 C6 H6 126.7 . . ? C6 C7 C8 112.4(2) . . ? C6 C7 H7 123.8 . . ? C8 C7 H7 123.8 . . ? C7 C8 C4 104.2(2) . . ? C7 C8 Si2 126.1(2) . . ? C4 C8 Si2 127.3(2) . . ? C10 C9 C13 104.7(2) . . ? C10 C9 Si3 124.77(19) . . ? C13 C9 Si3 128.17(18) . . ? C10 C9 Ti2 69.44(14) . . ? C13 C9 Ti2 72.43(13) . . ? Si3 C9 Ti2 135.44(13) . . ? C11 C10 C9 111.4(2) . . ? C11 C10 Ti2 71.26(14) . . ? C9 C10 Ti2 75.02(14) . . ? C11 C10 H10 124.3 . . ? C9 C10 H10 124.3 . . ? Ti2 C10 H10 120.9 . . ? C10 C11 C12 107.6(2) . . ? C10 C11 Ti2 72.86(14) . . ? C12 C11 Ti2 74.22(14) . . ? C10 C11 H11 126.2 . . ? C12 C11 H11 126.2 . . ? Ti2 C11 H11 118.7 . . ? C16 C12 C11 143.8(2) . . ? C16 C12 C13 109.5(2) . . ? C11 C12 C13 106.6(2) . . ? C16 C12 Ti2 118.60(18) . . ? C11 C12 Ti2 69.68(13) . . ? C13 C12 Ti2 73.51(13) . . ? C14 C13 C9 143.3(2) . . ? C14 C13 C12 107.1(2) . . ? C9 C13 C12 109.6(2) . . ? C14 C13 Ti2 120.29(18) . . ? C9 C13 Ti2 72.16(13) . . ? C12 C13 Ti2 70.69(13) . . ? C15 C14 C13 106.6(2) . . ? C15 C14 H14 126.7 . . ? C13 C14 H14 126.7 . . ? C14 C15 C16 112.8(2) . . ? C14 C15 H15 123.6 . . ? C16 C15 H15 123.6 . . ? C15 C16 C12 104.0(2) . . ? C15 C16 Si4 126.8(2) . . ? C12 C16 Si4 128.4(2) . . ? C19 C17 C18 110.5(4) . . ? C19 C17 Si1 115.2(3) . . ? C18 C17 Si1 113.9(3) . . ? C19 C17 H17 105.4 . . ? C18 C17 H17 105.4 . . ? Si1 C17 H17 105.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 109.9(4) . . ? C22 C20 Si1 114.0(3) . . ? C21 C20 Si1 111.1(3) . . ? C22 C20 H20 107.1 . . ? C21 C20 H20 107.1 . . ? Si1 C20 H20 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 109.5(3) . . ? C25 C23 Si1 113.4(3) . . ? C24 C23 Si1 114.5(3) . . ? C25 C23 H23 106.3 . . ? C24 C23 H23 106.3 . . ? Si1 C23 H23 106.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C27 110.3(4) . . ? C28 C26 Si2 111.6(3) . . ? C27 C26 Si2 112.6(3) . . ? C28 C26 H26 107.4 . . ? C27 C26 H26 107.4 . . ? Si2 C26 H26 107.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30A C29A C31A 126.1(12) . . ? C30A C29A Si2 122.2(8) . . ? C31A C29A Si2 111.6(10) . . ? C30A C29A H29A 91.3 . . ? C31A C29A H29A 91.3 . . ? Si2 C29A H29A 91.3 . . ? C29A C30A H30A 109.5 . . ? C29A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C29A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C29A C31A H31A 109.5 . . ? C29A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C29A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C30B C29B C31B 116.6(13) . . ? C30B C29B Si2 124.2(8) . . ? C31B C29B Si2 114.3(12) . . ? C30B C29B H29B 97.4 . . ? C31B C29B H29B 97.4 . . ? Si2 C29B H29B 97.4 . . ? C29B C30B H30D 109.5 . . ? C29B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C29B C31B H31D 109.5 . . ? C29B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C29B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C34 C32 C33 110.5(3) . . ? C34 C32 Si2 115.3(3) . . ? C33 C32 Si2 113.5(3) . . ? C34 C32 H32 105.6 . . ? C33 C32 H32 105.6 . . ? Si2 C32 H32 105.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 109.6(3) . . ? C36 C35 Si3 114.1(2) . . ? C37 C35 Si3 113.7(2) . . ? C36 C35 H35 106.2 . . ? C37 C35 H35 106.2 . . ? Si3 C35 H35 106.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C40 109.0(3) . . ? C39 C38 Si3 115.3(2) . . ? C40 C38 Si3 114.1(2) . . ? C39 C38 H38 105.9 . . ? C40 C38 H38 105.9 . . ? Si3 C38 H38 105.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 109.4(3) . . ? C42 C41 Si3 112.2(2) . . ? C43 C41 Si3 113.1(2) . . ? C42 C41 H41 107.3 . . ? C43 C41 H41 107.3 . . ? Si3 C41 H41 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46A C44A C45A 88(3) . . ? C46A C44A Si4 102.1(15) . . ? C45A C44A Si4 125.2(18) . . ? C46A C44A H44A 112.6 . . ? C45A C44A H44A 112.6 . . ? Si4 C44A H44A 112.6 . . ? C44A C45A H45A 109.5 . . ? C44A C45A H45B 109.5 . . ? H45A C45A H45B 109.5 . . ? C44A C45A H45C 109.5 . . ? H45A C45A H45C 109.5 . . ? H45B C45A H45C 109.5 . . ? C44A C46A H46A 109.5 . . ? C44A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C44A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? H45D C45B H45E 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? H46D C46B H46E 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C49 C47 C48 109.7(3) . . ? C49 C47 Si4 115.6(3) . . ? C48 C47 Si4 113.2(3) . . ? C49 C47 H47 105.9 . . ? C48 C47 H47 105.9 . . ? Si4 C47 H47 105.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51A C50A C52A 109(3) . . ? C51A C50A Si4 123(2) . . ? C52A C50A Si4 97.7(14) . . ? C51A C50A H50A 108.5 . . ? C52A C50A H50A 108.5 . . ? Si4 C50A H50A 108.5 . . ? C50A C51A H51A 109.5 . . ? C50A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C50A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? C50A C52A H52A 109.5 . . ? C50A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C50A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? H51D C51B H51E 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? H52D C52B H52E 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? N1 C53 C54 122.5(3) . . ? N1 C53 H53 118.7 . . ? C54 C53 H53 118.7 . . ? C53 C54 C55 119.0(3) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 119.0(3) . . ? C56 C55 H55 120.5 . . ? C54 C55 H55 120.5 . . ? C55 C56 C57 118.8(3) . . ? C55 C56 H56 120.6 . . ? C57 C56 H56 120.6 . . ? N1 C57 C56 123.5(3) . . ? N1 C57 H57 118.2 . . ? C56 C57 H57 118.2 . . ? N2 C58 C59 122.2(3) . . ? N2 C58 H58 118.9 . . ? C59 C58 H58 118.9 . . ? C60 C59 C58 119.5(4) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C61 C60 C59 119.2(3) . . ? C61 C60 H60 120.4 . . ? C59 C60 H60 120.4 . . ? C60 C61 C62 119.0(3) . . ? C60 C61 H61 120.5 . . ? C62 C61 H61 120.5 . . ? N2 C62 C61 122.6(3) . . ? N2 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? C57 N1 C53 117.1(3) . . ? C57 N1 Ti1 124.28(19) . . ? C53 N1 Ti1 118.39(19) . . ? C62 N2 C58 117.5(3) . . ? C62 N2 Ti2 123.8(2) . . ? C58 N2 Ti2 118.6(2) . . ? Ti2 O1 Ti1 95.35(8) . . ? Ti1 O2 Ti2 95.33(8) . . ? C1 Si1 C17 110.66(14) . . ? C1 Si1 C23 109.24(14) . . ? C17 Si1 C23 116.50(18) . . ? C1 Si1 C20 105.46(14) . . ? C17 Si1 C20 107.08(19) . . ? C23 Si1 C20 107.26(17) . . ? C8 Si2 C26 108.03(14) . . ? C8 Si2 C32 109.16(14) . . ? C26 Si2 C32 106.48(17) . . ? C8 Si2 C29A 114.2(4) . . ? C26 Si2 C29A 114.3(6) . . ? C32 Si2 C29A 104.3(7) . . ? C8 Si2 C29B 106.7(4) . . ? C26 Si2 C29B 100.8(5) . . ? C32 Si2 C29B 124.5(6) . . ? C9 Si3 C35 110.08(13) . . ? C9 Si3 C38 109.25(12) . . ? C35 Si3 C38 115.56(15) . . ? C9 Si3 C41 105.97(12) . . ? C35 Si3 C41 108.18(14) . . ? C38 Si3 C41 107.35(14) . . ? C16 Si4 C44A 109.98(18) . . ? C16 Si4 C47 108.41(13) . . ? C44A Si4 C47 107.61(19) . . ? C16 Si4 C50A 109.89(18) . . ? C44A Si4 C50A 112.9(3) . . ? C47 Si4 C50A 108.0(2) . . ? O2 Ti1 O1 84.85(7) . . ? O2 Ti1 N1 98.65(8) . . ? O1 Ti1 N1 93.42(8) . . ? O2 Ti1 C2 111.13(9) . . ? O1 Ti1 C2 102.40(9) . . ? N1 Ti1 C2 147.20(9) . . ? O2 Ti1 C1 100.60(9) . . ? O1 Ti1 C1 137.84(9) . . ? N1 Ti1 C1 126.23(9) . . ? C2 Ti1 C1 36.50(9) . . ? O2 Ti1 C5 125.09(8) . . ? O1 Ti1 C5 147.98(8) . . ? N1 Ti1 C5 92.77(8) . . ? C2 Ti1 C5 59.16(9) . . ? C1 Ti1 C5 36.62(9) . . ? O2 Ti1 C3 143.57(9) . . ? O1 Ti1 C3 90.53(8) . . ? N1 Ti1 C3 117.71(9) . . ? C2 Ti1 C3 35.06(9) . . ? C1 Ti1 C3 60.51(9) . . ? C5 Ti1 C3 59.02(9) . . ? O2 Ti1 C4 159.90(8) . . ? O1 Ti1 C4 113.27(8) . . ? N1 Ti1 C4 89.21(8) . . ? C2 Ti1 C4 58.19(9) . . ? C1 Ti1 C4 60.34(9) . . ? C5 Ti1 C4 35.47(8) . . ? C3 Ti1 C4 34.84(9) . . ? O2 Ti1 Ti2 42.61(5) . . ? O1 Ti1 Ti2 42.27(5) . . ? N1 Ti1 Ti2 96.95(6) . . ? C2 Ti1 Ti2 114.12(7) . . ? C1 Ti1 Ti2 129.94(7) . . ? C5 Ti1 Ti2 165.43(7) . . ? C3 Ti1 Ti2 124.20(7) . . ? C4 Ti1 Ti2 154.88(6) . . ? O1 Ti2 O2 84.40(7) . . ? O1 Ti2 N2 94.75(8) . . ? O2 Ti2 N2 101.22(8) . . ? O1 Ti2 C11 90.90(8) . . ? O2 Ti2 C11 129.95(9) . . ? N2 Ti2 C11 128.83(9) . . ? O1 Ti2 C10 110.13(9) . . ? O2 Ti2 C10 100.44(9) . . ? N2 Ti2 C10 148.34(9) . . ? C11 Ti2 C10 35.87(9) . . ? O1 Ti2 C12 108.42(8) . . ? O2 Ti2 C12 158.45(9) . . ? N2 Ti2 C12 95.03(9) . . ? C11 Ti2 C12 36.10(9) . . ? C10 Ti2 C12 59.27(9) . . ? O1 Ti2 C9 145.65(9) . . ? O2 Ti2 C9 99.32(8) . . ? N2 Ti2 C9 117.56(9) . . ? C11 Ti2 C9 60.48(9) . . ? C10 Ti2 C9 35.53(9) . . ? C12 Ti2 C9 60.25(8) . . ? O1 Ti2 C13 144.22(8) . . ? O2 Ti2 C13 129.28(8) . . ? N2 Ti2 C13 90.19(9) . . ? C11 Ti2 C13 59.48(9) . . ? C10 Ti2 C13 58.17(9) . . ? C12 Ti2 C13 35.80(8) . . ? C9 Ti2 C13 35.41(8) . . ? O1 Ti2 Ti1 42.37(5) . . ? O2 Ti2 Ti1 42.05(5) . . ? N2 Ti2 Ti1 102.01(6) . . ? C11 Ti2 Ti1 115.41(7) . . ? C10 Ti2 Ti1 109.54(7) . . ? C12 Ti2 Ti1 146.72(6) . . ? C9 Ti2 Ti1 130.78(6) . . ? C13 Ti2 Ti1 166.06(7) . . ? C105 C104 C103 125.4(9) . . ? C105 C104 H104 117.3 . . ? C103 C104 H104 117.3 . . ? C100 C105 C104 118.9(8) . . ? C100 C105 H105 120.6 . . ? C104 C105 H105 120.6 . . ? C104 C103 N3 116.8(9) . . ? C104 C103 H103 121.6 . . ? N3 C103 H103 121.6 . . ? C100 C101 N3 116.6(10) . . ? C100 C101 H101 121.7 . . ? N3 C101 H101 121.7 . . ? C105 C100 C101 128.1(11) . . ? C105 C100 H100 115.9 . . ? C101 C100 H100 115.9 . . ? C101 N3 C103 113.8(9) . . ? 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 C5 C1 C2 C3 -1.2(3) . . . . ? Si1 C1 C2 C3 -159.02(19) . . . . ? Ti1 C1 C2 C3 65.16(19) . . . . ? C5 C1 C2 Ti1 -66.33(16) . . . . ? Si1 C1 C2 Ti1 135.8(2) . . . . ? C1 C2 C3 C4 2.0(3) . . . . ? Ti1 C2 C3 C4 65.16(18) . . . . ? C1 C2 C3 Ti1 -63.18(18) . . . . ? C2 C3 C4 C8 178.7(3) . . . . ? Ti1 C3 C4 C8 -119.1(4) . . . . ? C2 C3 C4 C5 -2.0(3) . . . . ? Ti1 C3 C4 C5 60.31(17) . . . . ? C2 C3 C4 Ti1 -62.26(18) . . . . ? C8 C4 C5 C6 1.8(3) . . . . ? C3 C4 C5 C6 -177.8(2) . . . . ? Ti1 C4 C5 C6 -116.64(19) . . . . ? C8 C4 C5 C1 -179.1(2) . . . . ? C3 C4 C5 C1 1.3(3) . . . . ? Ti1 C4 C5 C1 62.44(16) . . . . ? C8 C4 C5 Ti1 118.43(19) . . . . ? C3 C4 C5 Ti1 -61.17(17) . . . . ? C2 C1 C5 C6 178.4(3) . . . . ? Si1 C1 C5 C6 -24.2(5) . . . . ? Ti1 C1 C5 C6 113.1(4) . . . . ? C2 C1 C5 C4 -0.1(3) . . . . ? Si1 C1 C5 C4 157.23(19) . . . . ? Ti1 C1 C5 C4 -65.44(17) . . . . ? C2 C1 C5 Ti1 65.35(16) . . . . ? Si1 C1 C5 Ti1 -137.3(2) . . . . ? C4 C5 C6 C7 -1.8(3) . . . . ? C1 C5 C6 C7 179.6(3) . . . . ? Ti1 C5 C6 C7 -84.1(2) . . . . ? C5 C6 C7 C8 1.3(3) . . . . ? C6 C7 C8 C4 -0.2(3) . . . . ? C6 C7 C8 Si2 -163.6(2) . . . . ? C3 C4 C8 C7 178.4(3) . . . . ? C5 C4 C8 C7 -1.0(3) . . . . ? Ti1 C4 C8 C7 76.6(2) . . . . ? C3 C4 C8 Si2 -18.4(5) . . . . ? C5 C4 C8 Si2 162.19(19) . . . . ? Ti1 C4 C8 Si2 -120.3(2) . . . . ? C13 C9 C10 C11 -1.9(3) . . . . ? Si3 C9 C10 C11 -165.75(18) . . . . ? Ti2 C9 C10 C11 62.49(18) . . . . ? C13 C9 C10 Ti2 -64.41(16) . . . . ? Si3 C9 C10 Ti2 131.77(19) . . . . ? C9 C10 C11 C12 1.9(3) . . . . ? Ti2 C10 C11 C12 66.65(17) . . . . ? C9 C10 C11 Ti2 -64.79(18) . . . . ? C10 C11 C12 C16 -176.7(3) . . . . ? Ti2 C11 C12 C16 -111.0(4) . . . . ? C10 C11 C12 C13 -1.0(3) . . . . ? Ti2 C11 C12 C13 64.75(17) . . . . ? C10 C11 C12 Ti2 -65.74(17) . . . . ? C10 C9 C13 C14 179.4(3) . . . . ? Si3 C9 C13 C14 -17.5(5) . . . . ? Ti2 C9 C13 C14 117.1(4) . . . . ? C10 C9 C13 C12 1.3(3) . . . . ? Si3 C9 C13 C12 164.33(19) . . . . ? Ti2 C9 C13 C12 -61.09(17) . . . . ? C10 C9 C13 Ti2 62.35(16) . . . . ? Si3 C9 C13 Ti2 -134.6(2) . . . . ? C16 C12 C13 C14 -1.7(3) . . . . ? C11 C12 C13 C14 -179.0(2) . . . . ? Ti2 C12 C13 C14 -116.83(19) . . . . ? C16 C12 C13 C9 177.1(2) . . . . ? C11 C12 C13 C9 -0.2(3) . . . . ? Ti2 C12 C13 C9 62.00(17) . . . . ? C16 C12 C13 Ti2 115.1(2) . . . . ? C11 C12 C13 Ti2 -62.20(16) . . . . ? C9 C13 C14 C15 -177.5(3) . . . . ? C12 C13 C14 C15 0.6(3) . . . . ? Ti2 C13 C14 C15 -76.6(2) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? C14 C15 C16 C12 -1.7(3) . . . . ? C14 C15 C16 Si4 -171.7(2) . . . . ? C11 C12 C16 C15 177.7(3) . . . . ? C13 C12 C16 C15 2.0(3) . . . . ? Ti2 C12 C16 C15 83.4(2) . . . . ? C11 C12 C16 Si4 -12.5(5) . . . . ? C13 C12 C16 Si4 171.8(2) . . . . ? Ti2 C12 C16 Si4 -106.8(2) . . . . ? N1 C53 C54 C55 0.2(5) . . . . ? C53 C54 C55 C56 -0.3(6) . . . . ? C54 C55 C56 C57 -0.3(6) . . . . ? C55 C56 C57 N1 1.1(5) . . . . ? N2 C58 C59 C60 -0.1(6) . . . . ? C58 C59 C60 C61 -0.6(6) . . . . ? C59 C60 C61 C62 0.8(6) . . . . ? C60 C61 C62 N2 -0.3(5) . . . . ? C56 C57 N1 C53 -1.2(4) . . . . ? C56 C57 N1 Ti1 -175.0(3) . . . . ? C54 C53 N1 C57 0.5(4) . . . . ? C54 C53 N1 Ti1 174.7(3) . . . . ? C61 C62 N2 C58 -0.4(4) . . . . ? C61 C62 N2 Ti2 -176.0(2) . . . . ? C59 C58 N2 C62 0.6(5) . . . . ? C59 C58 N2 Ti2 176.4(3) . . . . ? C2 C1 Si1 C17 -159.2(2) . . . . ? C5 C1 Si1 C17 47.9(3) . . . . ? Ti1 C1 Si1 C17 -58.1(2) . . . . ? C2 C1 Si1 C23 -29.6(3) . . . . ? C5 C1 Si1 C23 177.4(2) . . . . ? Ti1 C1 Si1 C23 71.5(2) . . . . ? C2 C1 Si1 C20 85.4(3) . . . . ? C5 C1 Si1 C20 -67.6(3) . . . . ? Ti1 C1 Si1 C20 -173.5(2) . . . . ? C19 C17 Si1 C1 54.0(4) . . . . ? C18 C17 Si1 C1 -176.7(3) . . . . ? C19 C17 Si1 C23 -71.5(4) . . . . ? C18 C17 Si1 C23 57.7(4) . . . . ? C19 C17 Si1 C20 168.5(3) . . . . ? C18 C17 Si1 C20 -62.3(4) . . . . ? C25 C23 Si1 C1 -73.2(3) . . . . ? C24 C23 Si1 C1 160.1(3) . . . . ? C25 C23 Si1 C17 53.1(3) . . . . ? C24 C23 Si1 C17 -73.6(4) . . . . ? C25 C23 Si1 C20 173.0(3) . . . . ? C24 C23 Si1 C20 46.3(4) . . . . ? C7 C8 Si2 C26 72.9(3) . . . . ? C4 C8 Si2 C26 -86.8(3) . . . . ? C7 C8 Si2 C32 -171.7(2) . . . . ? C4 C8 Si2 C32 28.6(3) . . . . ? C7 C8 Si2 C29A -55.4(8) . . . . ? C4 C8 Si2 C29A 144.9(8) . . . . ? C7 C8 Si2 C29B -34.8(6) . . . . ? C4 C8 Si2 C29B 165.5(6) . . . . ? C28 C26 Si2 C8 57.9(3) . . . . ? C27 C26 Si2 C8 -66.8(4) . . . . ? C28 C26 Si2 C32 -59.2(3) . . . . ? C27 C26 Si2 C32 176.1(3) . . . . ? C28 C26 Si2 C29A -173.8(7) . . . . ? C27 C26 Si2 C29A 61.5(7) . . . . ? C28 C26 Si2 C29B 169.7(6) . . . . ? C27 C26 Si2 C29B 45.0(6) . . . . ? C34 C32 Si2 C8 56.8(3) . . . . ? C33 C32 Si2 C8 -174.4(3) . . . . ? C34 C32 Si2 C26 173.2(3) . . . . ? C33 C32 Si2 C26 -58.0(4) . . . . ? C34 C32 Si2 C29A -65.6(5) . . . . ? C33 C32 Si2 C29A 63.2(5) . . . . ? C34 C32 Si2 C29B -70.6(5) . . . . ? C33 C32 Si2 C29B 58.2(5) . . . . ? C10 C9 Si3 C35 -149.5(2) . . . . ? C13 C9 Si3 C35 50.6(3) . . . . ? Ti2 C9 Si3 C35 -54.0(2) . . . . ? C10 C9 Si3 C38 -21.6(3) . . . . ? C13 C9 Si3 C38 178.5(2) . . . . ? Ti2 C9 Si3 C38 73.9(2) . . . . ? C10 C9 Si3 C41 93.8(2) . . . . ? C13 C9 Si3 C41 -66.2(3) . . . . ? Ti2 C9 Si3 C41 -170.70(18) . . . . ? C36 C35 Si3 C9 65.6(3) . . . . ? C37 C35 Si3 C9 -167.6(2) . . . . ? C36 C35 Si3 C38 -58.7(3) . . . . ? C37 C35 Si3 C38 68.1(3) . . . . ? C36 C35 Si3 C41 -179.0(2) . . . . ? C37 C35 Si3 C41 -52.2(3) . . . . ? C39 C38 Si3 C9 -64.2(3) . . . . ? C40 C38 Si3 C9 168.5(3) . . . . ? C39 C38 Si3 C35 60.5(3) . . . . ? C40 C38 Si3 C35 -66.8(3) . . . . ? C39 C38 Si3 C41 -178.7(3) . . . . ? C40 C38 Si3 C41 54.0(3) . . . . ? C15 C16 Si4 C44A 57.3(3) . . . . ? C12 C16 Si4 C44A -110.3(3) . . . . ? C15 C16 Si4 C47 174.7(3) . . . . ? C12 C16 Si4 C47 7.1(3) . . . . ? C15 C16 Si4 C50A -67.5(3) . . . . ? C12 C16 Si4 C50A 124.9(3) . . . . ? C46A C44A Si4 C16 54.0(14) . . . . ? C45A C44A Si4 C16 -42(4) . . . . ? C46A C44A Si4 C47 -63.9(14) . . . . ? C45A C44A Si4 C47 -160(4) . . . . ? C46A C44A Si4 C50A 177.1(14) . . . . ? C45A C44A Si4 C50A 81(4) . . . . ? C49 C47 Si4 C16 -158.3(3) . . . . ? C48 C47 Si4 C16 74.1(3) . . . . ? C49 C47 Si4 C44A -39.4(4) . . . . ? C48 C47 Si4 C44A -167.0(3) . . . . ? C49 C47 Si4 C50A 82.7(4) . . . . ? C48 C47 Si4 C50A -44.9(3) . . . . ? Ti2 O2 Ti1 O1 -1.81(8) . . . . ? Ti2 O2 Ti1 N1 90.88(9) . . . . ? Ti2 O2 Ti1 C2 -103.13(10) . . . . ? Ti2 O2 Ti1 C1 -139.57(9) . . . . ? Ti2 O2 Ti1 C5 -169.53(9) . . . . ? Ti2 O2 Ti1 C3 -85.71(15) . . . . ? Ti2 O2 Ti1 C4 -157.1(2) . . . . ? Ti2 O1 Ti1 O2 1.82(8) . . . . ? Ti2 O1 Ti1 N1 -96.57(9) . . . . ? Ti2 O1 Ti1 C2 112.35(9) . . . . ? Ti2 O1 Ti1 C1 101.95(13) . . . . ? Ti2 O1 Ti1 C5 162.67(13) . . . . ? Ti2 O1 Ti1 C3 145.62(9) . . . . ? Ti2 O1 Ti1 C4 172.82(8) . . . . ? Ti1 O1 Ti2 O2 -1.80(8) . . . . ? Ti1 O1 Ti2 N2 -102.64(9) . . . . ? Ti1 O1 Ti2 C11 128.27(9) . . . . ? Ti1 O1 Ti2 C10 97.29(9) . . . . ? Ti1 O1 Ti2 C12 160.44(8) . . . . ? Ti1 O1 Ti2 C9 96.52(14) . . . . ? Ti1 O1 Ti2 C13 160.40(12) . . . . ? Ti1 O2 Ti2 O1 1.81(8) . . . . ? Ti1 O2 Ti2 N2 95.56(9) . . . . ? Ti1 O2 Ti2 C11 -84.66(12) . . . . ? Ti1 O2 Ti2 C10 -107.67(9) . . . . ? Ti1 O2 Ti2 C12 -126.2(2) . . . . ? Ti1 O2 Ti2 C9 -143.74(9) . . . . ? Ti1 O2 Ti2 C13 -164.84(9) . . . . ? C103 C104 C105 C100 3.5(14) . . . . ? C105 C104 C103 N3 0.5(14) . . . . ? C104 C105 C100 C101 -2.4(16) . . . . ? N3 C101 C100 C105 -2.6(16) . . . . ? C100 C101 N3 C103 6.0(14) . . . . ? C104 C103 N3 C101 -5.1(14) . . . . ? _iucr_refine_instructions_details ; TITL file DDJOB.res = = DIRDIF output for SHELX CELL 1.54184 13.7134 16.0497 18.5403 85.689 86.517 66.630 ZERR 2.00 0.0006 0.0006 0.0006 0.003 0.003 0.004 LATT 1 SFAC C H N O SI TI UNIT 134 214 6 4 8 4 MERG 2 EADP C44A C44B EXYZ C44A C44B EADP C50A C50B EXYZ C50A C50B CONF HTAB ACTA DELU C50A C50B C51A C51B C52A C52B SIMU C50A C50B C51A C51B C52A C52B OMIT 15 10 8 OMIT 15 13 6 OMIT 15 12 8 OMIT 13 7 4 OMIT 13 10 1 OMIT 13 6 4 OMIT 15 11 8 OMIT 15 14 7 OMIT 15 12 9 OMIT 14 9 10 OMIT 13 6 3 OMIT 15 13 7 OMIT 14 9 9 OMIT 13 9 8 OMIT 13 16 6 OMIT 14 12 7 OMIT 14 12 8 OMIT 14 10 11 OMIT 13 8 5 OMIT 14 15 7 OMIT 15 14 6 OMIT 12 10 0 OMIT 14 15 6 OMIT 13 13 12 OMIT 14 14 9 FMAP 2 PLAN 5 SIZE 0.200 0.400 0.400 BOND $H WPDB -1 L.S. 30 TEMP -100.00 WGHT 0.082200 3.164800 FVAR 43.87401 0.51402 0.35039 0.20308 C1 1 0.036764 0.023815 0.237975 11.00000 0.03458 0.02898 = 0.04361 -0.00438 -0.00512 -0.01412 C2 1 0.129482 0.022441 0.196568 11.00000 0.03998 0.03375 = 0.03821 -0.00692 -0.00154 -0.01689 AFIX 43 H2 2 0.130667 0.037405 0.146054 11.00000 -1.20000 AFIX 0 C3 1 0.218037 -0.003828 0.240291 11.00000 0.03114 0.03142 = 0.04377 -0.00680 0.00168 -0.01012 AFIX 43 H3 2 0.286998 -0.007733 0.224905 11.00000 -1.20000 AFIX 0 C4 1 0.185929 -0.023630 0.312031 11.00000 0.03099 0.02619 = 0.04298 -0.00079 -0.00121 -0.01011 C5 1 0.073984 -0.005512 0.311111 11.00000 0.03306 0.02401 = 0.04331 -0.00003 -0.00428 -0.01491 C6 1 0.040961 -0.021793 0.382870 11.00000 0.03250 0.03166 = 0.04622 -0.00149 0.00108 -0.01575 AFIX 43 H6 2 -0.028920 -0.014011 0.399351 11.00000 -1.20000 AFIX 0 C7 1 0.131438 -0.051563 0.424651 11.00000 0.04054 0.03464 = 0.04060 0.00311 -0.00419 -0.01668 AFIX 43 H7 2 0.131492 -0.068410 0.474882 11.00000 -1.20000 AFIX 0 C8 1 0.223110 -0.053760 0.383556 11.00000 0.03155 0.03032 = 0.04450 0.00104 -0.00686 -0.01194 C9 1 -0.061436 0.449460 0.248584 11.00000 0.02727 0.02528 = 0.04428 -0.00168 -0.00279 -0.00884 C10 1 0.011090 0.405178 0.305057 11.00000 0.03550 0.02990 = 0.03591 -0.00326 -0.00249 -0.01218 AFIX 43 H10 2 -0.009479 0.390445 0.352557 11.00000 -1.20000 AFIX 0 C11 1 0.117217 0.386120 0.281243 11.00000 0.03180 0.02990 = 0.03963 -0.00154 -0.00923 -0.01154 AFIX 43 H11 2 0.178722 0.355610 0.308964 11.00000 -1.20000 AFIX 0 C12 1 0.115284 0.421188 0.207615 11.00000 0.02635 0.02776 = 0.04446 0.00323 -0.00854 -0.01441 C13 1 0.004619 0.460403 0.187831 11.00000 0.02642 0.02518 = 0.04457 0.00379 -0.00816 -0.01161 C14 1 0.001923 0.494078 0.114382 11.00000 0.03480 0.03028 = 0.04595 0.00751 -0.01115 -0.01186 AFIX 43 H14 2 -0.059487 0.523982 0.086461 11.00000 -1.20000 AFIX 0 C15 1 0.106914 0.474604 0.091476 11.00000 0.04336 0.03843 = 0.04158 0.00810 -0.00580 -0.01934 AFIX 43 H15 2 0.127142 0.490634 0.044267 11.00000 -1.20000 AFIX 0 C16 1 0.180813 0.428050 0.146413 11.00000 0.03015 0.03751 = 0.04670 0.00599 -0.00578 -0.01715 C17 1 -0.200782 0.063196 0.262446 11.00000 0.03976 0.06747 = 0.07640 -0.00225 -0.00850 -0.03053 AFIX 13 H17 2 -0.181597 0.022876 0.307631 11.00000 -1.20000 AFIX 0 C18 1 -0.300518 0.055397 0.236443 11.00000 0.05216 0.12699 = 0.10906 -0.01457 -0.00903 -0.05623 AFIX 33 H18A 2 -0.282580 -0.006499 0.221737 11.00000 -1.50000 H18B 2 -0.328217 0.098729 0.195128 11.00000 -1.50000 H18C 2 -0.354600 0.068967 0.275819 11.00000 -1.50000 AFIX 0 C19 1 -0.226699 0.159055 0.286089 11.00000 0.04880 0.06920 = 0.12907 -0.02803 0.02015 -0.02600 AFIX 33 H19A 2 -0.162199 0.162726 0.302887 11.00000 -1.50000 H19B 2 -0.280729 0.172931 0.325506 11.00000 -1.50000 H19C 2 -0.253794 0.202997 0.245042 11.00000 -1.50000 AFIX 0 C20 1 -0.049202 -0.109050 0.193526 11.00000 0.08019 0.04982 = 0.08450 -0.00257 -0.03110 -0.03693 AFIX 13 H20 2 -0.108178 -0.114395 0.167649 11.00000 -1.20000 AFIX 0 C21 1 0.053847 -0.155110 0.148108 11.00000 0.09622 0.05250 = 0.12680 -0.03189 -0.02323 -0.01766 AFIX 33 H21A 2 0.048452 -0.122045 0.100889 11.00000 -1.50000 H21B 2 0.064371 -0.218082 0.141173 11.00000 -1.50000 H21C 2 0.114279 -0.154505 0.173367 11.00000 -1.50000 AFIX 0 C22 1 -0.041945 -0.160662 0.267185 11.00000 0.14544 0.05383 = 0.10957 0.01626 -0.03987 -0.06113 AFIX 33 H22A 2 -0.108023 -0.131430 0.295586 11.00000 -1.50000 H22B 2 0.017924 -0.159934 0.293049 11.00000 -1.50000 H22C 2 -0.031088 -0.223673 0.260088 11.00000 -1.50000 AFIX 0 C23 1 -0.097769 0.069691 0.103224 11.00000 0.06486 0.06386 = 0.05442 0.00365 -0.02124 -0.03522 AFIX 13 H23 2 -0.024950 0.046852 0.079868 11.00000 -1.20000 AFIX 0 C24 1 -0.166571 0.040887 0.056279 11.00000 0.11076 0.08304 = 0.06751 0.00107 -0.03718 -0.05516 AFIX 33 H24A 2 -0.140340 -0.025593 0.058260 11.00000 -1.50000 H24B 2 -0.162684 0.063671 0.006100 11.00000 -1.50000 H24C 2 -0.240509 0.066237 0.074580 11.00000 -1.50000 AFIX 0 C25 1 -0.137618 0.173349 0.099319 11.00000 0.12303 0.06965 = 0.07521 0.02091 -0.04691 -0.05689 AFIX 33 H25A 2 -0.093825 0.191637 0.129286 11.00000 -1.50000 H25B 2 -0.211757 0.199450 0.117137 11.00000 -1.50000 H25C 2 -0.132817 0.195409 0.049030 11.00000 -1.50000 AFIX 0 C26 1 0.400027 -0.240827 0.403288 11.00000 0.04843 0.03635 = 0.09161 0.00387 -0.01478 -0.00852 AFIX 13 H26 2 0.477151 -0.272582 0.413947 11.00000 -1.20000 AFIX 0 C27 1 0.338603 -0.278981 0.458385 11.00000 0.10785 0.06614 = 0.12758 0.02090 -0.00994 -0.04385 AFIX 33 H27A 2 0.348864 -0.265107 0.507238 11.00000 -1.50000 H27B 2 0.364800 -0.345010 0.455204 11.00000 -1.50000 H27C 2 0.262781 -0.251275 0.448022 11.00000 -1.50000 AFIX 0 C28 1 0.386296 -0.262506 0.327524 11.00000 0.09041 0.04523 = 0.11285 -0.02279 -0.01420 -0.01398 AFIX 33 H28A 2 0.427232 -0.238830 0.292900 11.00000 -1.50000 H28B 2 0.310914 -0.234207 0.315991 11.00000 -1.50000 H28C 2 0.411843 -0.328529 0.324588 11.00000 -1.50000 AFIX 0 PART 1 C29A 1 0.391694 -0.082950 0.501530 21.00000 0.06781 0.06929 = 0.05624 -0.00103 -0.01971 -0.02263 AFIX 13 H29A 2 0.438670 -0.054027 0.477518 21.00000 -1.20000 AFIX 0 C30A 1 0.330528 -0.006210 0.530903 21.00000 0.12822 0.06636 = 0.06494 -0.00221 -0.03270 -0.04188 AFIX 33 H30A 2 0.272734 0.029065 0.498496 21.00000 -1.50000 H30B 2 0.372858 0.029060 0.538569 21.00000 -1.50000 H30C 2 0.300588 -0.019788 0.577447 21.00000 -1.50000 AFIX 0 C31A 1 0.484692 -0.157486 0.535489 21.00000 0.12189 0.06713 = 0.07280 0.00370 -0.05782 -0.02588 AFIX 33 H31A 2 0.516217 -0.206564 0.502132 21.00000 -1.50000 H31B 2 0.461171 -0.181020 0.580525 21.00000 -1.50000 H31C 2 0.537746 -0.133813 0.546106 21.00000 -1.50000 AFIX 0 PART 2 C29B 1 0.362918 -0.108128 0.513917 -21.00000 0.05760 0.05315 = 0.05013 0.00710 -0.02237 -0.01796 AFIX 13 H29B 2 0.326198 -0.150054 0.527855 -21.00000 -1.20000 AFIX 0 C30B 1 0.300355 -0.040348 0.549044 -21.00000 0.09222 0.09133 = 0.05144 -0.00903 -0.01568 -0.03635 AFIX 33 H30D 2 0.234028 -0.009670 0.523262 -21.00000 -1.50000 H30E 2 0.334397 0.002368 0.553251 -21.00000 -1.50000 H30F 2 0.284792 -0.061903 0.597485 -21.00000 -1.50000 AFIX 0 C31B 1 0.472650 -0.167835 0.548903 -21.00000 0.05854 0.16129 = 0.05978 0.02506 -0.02932 0.00116 AFIX 33 H31D 2 0.513173 -0.217921 0.517958 -21.00000 -1.50000 H31E 2 0.459949 -0.192553 0.596833 -21.00000 -1.50000 H31F 2 0.513051 -0.130150 0.553671 -21.00000 -1.50000 AFIX 0 PART 0 C32 1 0.453056 -0.081695 0.343369 11.00000 0.03594 0.04841 = 0.09308 0.00033 -0.00397 -0.01495 AFIX 13 H32 2 0.440637 -0.099541 0.295324 11.00000 -1.20000 AFIX 0 C33 1 0.572218 -0.135624 0.356550 11.00000 0.03569 0.07234 = 0.14754 0.00529 -0.00325 -0.01336 AFIX 33 H33A 2 0.587200 -0.200730 0.361803 11.00000 -1.50000 H33B 2 0.590969 -0.116490 0.400823 11.00000 -1.50000 H33C 2 0.614279 -0.123954 0.315407 11.00000 -1.50000 AFIX 0 C34 1 0.428286 0.018541 0.334106 11.00000 0.04984 0.05508 = 0.11392 0.00619 -0.00654 -0.02545 AFIX 33 H34A 2 0.352461 0.051777 0.325232 11.00000 -1.50000 H34B 2 0.470351 0.030094 0.292916 11.00000 -1.50000 H34C 2 0.445918 0.039023 0.378140 11.00000 -1.50000 AFIX 0 C35 1 -0.278026 0.501063 0.179806 11.00000 0.03185 0.04231 = 0.06063 0.00171 -0.01005 -0.01584 AFIX 13 H35 2 -0.243191 0.521890 0.137385 11.00000 -1.20000 AFIX 0 C36 1 -0.264927 0.404235 0.165633 11.00000 0.05137 0.04718 = 0.08542 -0.00822 -0.01795 -0.01965 AFIX 33 H36A 2 -0.189349 0.363983 0.165719 11.00000 -1.50000 H36B 2 -0.293550 0.404202 0.118476 11.00000 -1.50000 H36C 2 -0.303509 0.382626 0.203644 11.00000 -1.50000 AFIX 0 C37 1 -0.396514 0.564633 0.179075 11.00000 0.03620 0.05314 = 0.09083 -0.00174 -0.01902 -0.01268 AFIX 33 H37A 2 -0.404642 0.626529 0.187896 11.00000 -1.50000 H37B 2 -0.435615 0.543497 0.217033 11.00000 -1.50000 H37C 2 -0.424763 0.564368 0.131832 11.00000 -1.50000 AFIX 0 C38 1 -0.251508 0.464549 0.350909 11.00000 0.03880 0.04226 = 0.05967 -0.00028 0.00609 -0.00986 AFIX 13 H38 2 -0.205560 0.470403 0.388435 11.00000 -1.20000 AFIX 0 C39 1 -0.233804 0.364139 0.354388 11.00000 0.06903 0.04450 = 0.08451 0.00578 0.02784 -0.01599 AFIX 33 H39A 2 -0.160356 0.327725 0.339021 11.00000 -1.50000 H39B 2 -0.282720 0.355435 0.322232 11.00000 -1.50000 H39C 2 -0.246984 0.344876 0.404143 11.00000 -1.50000 AFIX 0 C40 1 -0.366641 0.520889 0.375746 11.00000 0.05086 0.06253 = 0.08765 -0.00082 0.02425 -0.00848 AFIX 33 H40A 2 -0.378494 0.585367 0.373879 11.00000 -1.50000 H40B 2 -0.379078 0.501002 0.425461 11.00000 -1.50000 H40C 2 -0.415732 0.512206 0.343730 11.00000 -1.50000 AFIX 0 C41 1 -0.235583 0.633406 0.272132 11.00000 0.03539 0.03185 = 0.06571 -0.00534 -0.00264 -0.00765 AFIX 13 H41 2 -0.313796 0.666095 0.281419 11.00000 -1.20000 AFIX 0 C42 1 -0.179779 0.646708 0.336622 11.00000 0.06698 0.05322 = 0.07996 -0.01201 -0.01399 -0.02407 AFIX 33 H42A 2 -0.198808 0.617673 0.380488 11.00000 -1.50000 H42B 2 -0.202136 0.711838 0.342972 11.00000 -1.50000 H42C 2 -0.102643 0.619136 0.327721 11.00000 -1.50000 AFIX 0 C43 1 -0.205653 0.678734 0.203671 11.00000 0.06075 0.03100 = 0.07954 0.00320 -0.00471 -0.01456 AFIX 33 H43A 2 -0.241440 0.670357 0.162315 11.00000 -1.50000 H43B 2 -0.128518 0.651029 0.194799 11.00000 -1.50000 H43C 2 -0.227841 0.743834 0.210075 11.00000 -1.50000 AFIX 0 PART 1 C44A 1 0.347686 0.510614 0.126292 31.00000 0.07399 0.08801 = 0.11065 0.03658 -0.02627 -0.05916 AFIX 13 H44A 2 0.424308 0.500490 0.128217 31.00000 -1.20000 AFIX 0 C45A 1 0.284282 0.592451 0.071099 31.00000 0.10332 0.13192 = 0.16242 0.08087 -0.02737 -0.06580 AFIX 33 H45A 2 0.301910 0.572838 0.021468 31.00000 -1.50000 H45B 2 0.304120 0.643840 0.076853 31.00000 -1.50000 H45C 2 0.207740 0.611114 0.080959 31.00000 -1.50000 AFIX 0 C46A 1 0.267427 0.578274 0.197976 31.00000 0.15801 0.04258 = 0.24146 -0.01160 -0.04147 -0.06130 AFIX 33 H46A 2 0.291599 0.546376 0.244840 31.00000 -1.50000 H46B 2 0.192890 0.588252 0.192620 31.00000 -1.50000 H46C 2 0.274150 0.636986 0.195448 31.00000 -1.50000 AFIX 0 PART 2 C44B 1 0.347686 0.510614 0.126292 -31.00000 0.07399 0.08801 = 0.11065 0.03658 -0.02627 -0.05916 AFIX 13 H44B 2 0.425568 0.492618 0.132052 -31.00000 -1.20000 AFIX 0 C45B 1 0.326465 0.549348 0.046164 -31.00000 0.09650 0.09436 = 0.10058 0.04775 -0.01750 -0.06621 AFIX 33 H45D 2 0.373519 0.504060 0.013399 -31.00000 -1.50000 H45E 2 0.340330 0.604856 0.039305 -31.00000 -1.50000 H45F 2 0.252256 0.563389 0.035604 -31.00000 -1.50000 AFIX 0 C46B 1 0.296863 0.575004 0.179112 -31.00000 0.08275 0.06522 = 0.13792 0.02376 -0.02189 -0.04610 AFIX 33 H46D 2 0.312862 0.545134 0.227555 -31.00000 -1.50000 H46E 2 0.219855 0.600368 0.172988 -31.00000 -1.50000 H46F 2 0.322748 0.624012 0.173299 -31.00000 -1.50000 AFIX 0 PART 0 C47 1 0.381144 0.349402 0.234046 11.00000 0.03344 0.05656 = 0.07778 0.01248 -0.01873 -0.02591 AFIX 13 H47 2 0.327501 0.384844 0.271019 11.00000 -1.20000 AFIX 0 C48 1 0.391305 0.250827 0.247116 11.00000 0.04455 0.05809 = 0.11339 0.02416 -0.02172 -0.02017 AFIX 33 H48A 2 0.324313 0.246975 0.235988 11.00000 -1.50000 H48B 2 0.407313 0.230967 0.297889 11.00000 -1.50000 H48C 2 0.448782 0.211559 0.215823 11.00000 -1.50000 AFIX 0 C49 1 0.485841 0.355746 0.251375 11.00000 0.04913 0.08801 = 0.10942 0.02065 -0.03086 -0.03901 AFIX 33 H49A 2 0.479132 0.418777 0.242952 11.00000 -1.50000 H49B 2 0.543377 0.316529 0.220093 11.00000 -1.50000 H49C 2 0.501917 0.335987 0.302155 11.00000 -1.50000 AFIX 0 PART 1 C50A 1 0.396206 0.315307 0.070929 41.00000 0.05057 0.13736 = 0.08321 -0.02834 0.00747 -0.02490 AFIX 13 H50A 2 0.429018 0.253663 0.095969 41.00000 -1.20000 AFIX 0 C51A 1 0.356593 0.309388 0.021061 41.00000 0.07874 0.15427 = 0.09365 -0.09065 0.02819 -0.03905 AFIX 33 H51A 2 0.298806 0.289629 0.035410 41.00000 -1.50000 H51B 2 0.408873 0.264766 -0.009877 41.00000 -1.50000 H51C 2 0.327705 0.368632 -0.005644 41.00000 -1.50000 AFIX 0 C52A 1 0.503058 0.355517 0.043316 41.00000 0.03597 0.14437 = 0.09360 -0.02072 0.02812 -0.01487 AFIX 33 H52A 2 0.545517 0.350914 0.085224 41.00000 -1.50000 H52B 2 0.471370 0.418997 0.024673 41.00000 -1.50000 H52C 2 0.548785 0.317902 0.005452 41.00000 -1.50000 AFIX 0 PART 2 C50B 1 0.396206 0.315307 0.070929 -41.00000 0.05057 0.13736 = 0.08321 -0.02834 0.00747 -0.02490 AFIX 13 H50B 2 0.392269 0.257563 0.092241 -41.00000 -1.20000 AFIX 0 C51B 1 0.339533 0.332417 -0.001234 -41.00000 0.08633 0.13300 = 0.06407 -0.01543 0.00672 -0.04116 AFIX 33 H51D 2 0.264168 0.344700 0.008457 -41.00000 -1.50000 H51E 2 0.372165 0.278582 -0.029792 -41.00000 -1.50000 H51F 2 0.346197 0.384858 -0.028292 -41.00000 -1.50000 AFIX 0 C52B 1 0.515947 0.292699 0.061946 -41.00000 0.05357 0.17603 = 0.12060 -0.04747 0.02685 -0.02743 AFIX 33 H52D 2 0.546833 0.282502 0.109747 -41.00000 -1.50000 H52E 2 0.527247 0.343485 0.035454 -41.00000 -1.50000 H52F 2 0.550165 0.237685 0.034906 -41.00000 -1.50000 AFIX 0 PART 0 C53 1 0.161897 0.188995 0.410751 11.00000 0.05079 0.04882 = 0.04735 0.00383 -0.01266 -0.02713 AFIX 43 H53 2 0.218649 0.184915 0.377260 11.00000 -1.20000 AFIX 0 C54 1 0.162952 0.217592 0.478701 11.00000 0.07858 0.06786 = 0.05580 -0.00252 -0.01727 -0.04311 AFIX 43 H54 2 0.219353 0.233077 0.491724 11.00000 -1.20000 AFIX 0 C55 1 0.080814 0.223465 0.527718 11.00000 0.09970 0.06025 = 0.04612 -0.01036 -0.00655 -0.03875 AFIX 43 H55 2 0.080055 0.242792 0.575015 11.00000 -1.20000 AFIX 0 C56 1 0.000540 0.201032 0.507151 11.00000 0.07730 0.05507 = 0.05161 -0.01362 0.01288 -0.03253 AFIX 43 H56 2 -0.056651 0.204255 0.539965 11.00000 -1.20000 AFIX 0 C57 1 0.004148 0.173747 0.438140 11.00000 0.04995 0.04126 = 0.05088 -0.00664 0.00355 -0.02223 AFIX 43 H57 2 -0.052525 0.159303 0.424067 11.00000 -1.20000 AFIX 0 C58 1 0.173272 0.210277 0.080312 11.00000 0.05947 0.04869 = 0.04321 -0.00283 0.00254 -0.01389 AFIX 43 H58 2 0.225980 0.179097 0.114787 11.00000 -1.20000 AFIX 0 C59 1 0.192980 0.186367 0.009437 11.00000 0.08909 0.06612 = 0.05281 -0.01451 0.01317 -0.02061 AFIX 43 H59 2 0.258365 0.139497 -0.004490 11.00000 -1.20000 AFIX 0 C60 1 0.117881 0.230507 -0.040631 11.00000 0.12784 0.05832 = 0.04034 -0.00493 -0.00121 -0.04990 AFIX 43 H60 2 0.130696 0.215120 -0.089790 11.00000 -1.20000 AFIX 0 C61 1 0.024219 0.296974 -0.019231 11.00000 0.10191 0.04930 = 0.04890 0.00596 -0.02506 -0.04204 AFIX 43 H61 2 -0.029447 0.327987 -0.053112 11.00000 -1.20000 AFIX 0 C62 1 0.008582 0.318508 0.052457 11.00000 0.06240 0.04126 = 0.04794 0.00323 -0.01830 -0.02438 AFIX 43 H62 2 -0.056644 0.365046 0.067087 11.00000 -1.20000 AFIX 0 N1 3 0.083107 0.166447 0.389779 11.00000 0.04051 0.02584 = 0.03880 0.00142 -0.00569 -0.01369 N2 3 0.081988 0.276227 0.102321 11.00000 0.04552 0.03251 = 0.03765 0.00238 -0.00372 -0.01851 O1 4 0.168880 0.196210 0.245483 11.00000 0.02586 0.02956 = 0.04285 0.00473 -0.00449 -0.01051 O2 4 -0.026581 0.237376 0.246160 11.00000 0.02603 0.03084 = 0.04491 0.00029 -0.00427 -0.01144 SI1 5 -0.082040 0.017370 0.199208 11.00000 0.04207 0.04004 = 0.05222 -0.00075 -0.01375 -0.02330 SI2 5 0.362752 -0.114659 0.410637 11.00000 0.03510 0.03390 = 0.05365 -0.00003 -0.01213 -0.00733 SI3 5 -0.208690 0.508874 0.262343 11.00000 0.02641 0.02894 = 0.05165 -0.00005 -0.00294 -0.00834 SI4 5 0.325328 0.402427 0.142770 11.00000 0.03158 0.06089 = 0.05748 0.00428 -0.00266 -0.02437 TI1 6 0.084841 0.133796 0.277900 11.00000 0.02875 0.02653 = 0.03596 0.00040 -0.00404 -0.01202 TI2 6 0.056946 0.301841 0.216363 11.00000 0.02774 0.02699 = 0.03502 0.00194 -0.00441 -0.01125 C104 1 0.158679 0.446749 0.460051 11.00000 0.14283 0.10810 = 0.11017 -0.00806 -0.01018 -0.06635 AFIX 43 H104 2 0.108312 0.424795 0.481865 11.00000 -1.20000 AFIX 0 C105 1 0.255055 0.393281 0.460929 11.00000 0.12903 0.10603 = 0.11650 0.02229 0.00011 -0.04816 AFIX 43 H105 2 0.275230 0.332505 0.480315 11.00000 -1.20000 AFIX 0 C103 1 0.122036 0.530212 0.431535 11.00000 0.14243 0.11936 = 0.19625 -0.02737 -0.04101 -0.03511 AFIX 43 H103 2 0.048229 0.567605 0.432844 11.00000 -1.20000 AFIX 0 C101 1 0.308618 0.501044 0.405712 11.00000 0.17667 0.10723 = 0.19005 -0.04558 0.03018 -0.07579 AFIX 43 H101 2 0.366666 0.516805 0.390063 11.00000 -1.20000 AFIX 0 C100 1 0.323146 0.421215 0.436103 11.00000 0.17782 0.11844 = 0.13311 -0.00509 -0.02183 -0.06022 AFIX 43 H100 2 0.394947 0.379250 0.439635 11.00000 -1.20000 AFIX 0 N3 3 0.201235 0.563408 0.397180 11.00000 0.29541 0.10569 = 0.22560 -0.02118 -0.00245 -0.07857 HKLF 4 REM file DDJOB.res = = DIRDIF output for SHELX REM R1 = 0.0560 for 12023 Fo > 4sig(Fo) and 0.0652 for all 13931 data REM 769 parameters refined using 72 restraints END ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 1.000 0.000 338 61 ' ' _platon_squeeze_details ; ; # END of CIF _database_code_depnum_ccdc_archive 'CCDC 969254' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelx _audit_creation_date 2013-10-28T17:37:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 3' _chemical_formula_moiety 'C54 H92 O2 Si4 Ti2' _chemical_formula_sum 'C54 H92 O2 Si4 Ti2' _chemical_formula_weight 981.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.894(3) _cell_length_b 22.342(5) _cell_length_c 19.113(4) _cell_angle_alpha 90 _cell_angle_beta 92.18(3) _cell_angle_gamma 90 _cell_volume 5502.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 48981 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; [c.f. R.H. Blessing, Acta Cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9519 _exptl_absorpt_correction_T_max 0.9877 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source ; fine-focus sealed tube ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_number 72543 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.159 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _reflns_number_total 12581 _reflns_number_gt 9225 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112) ; _computing_cell_refinement ; CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112) ; _computing_data_reduction ; CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material ; WINGX publication routines (Farrugia, 2013) ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Atoms of the iPr CH3 group C10 was positionally disordered over two sites. The disorder was modelled adequately and refinement proceeded normally. Restrain instructions (DELU, SIMU) were applied to this iPr group C9>C11 to give the thermal parameters more chemically reasonable values. 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 'w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+10.5184P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12581 _refine_ls_number_parameters 557 _refine_ls_number_restraints 38 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.2107 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.997 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4359(3) 0.15089(16) 0.76095(18) 0.0198(7) Uani 1 d . . C2 C 0.3665(3) 0.15597(17) 0.70063(18) 0.0210(7) Uani 1 d . . H2 H 0.3097 0.1298 0.6911 0.025 Uiso 1 calc . . C3 C 0.3923(3) 0.20378(16) 0.65754(18) 0.0198(7) Uani 1 d . . H3 H 0.3605 0.2132 0.6133 0.024 Uiso 1 calc . . C4 C 0.4758(3) 0.23611(16) 0.69235(18) 0.0202(7) Uani 1 d . . C5 C 0.5035(3) 0.20295(16) 0.75522(18) 0.0200(7) Uani 1 d . . C6 C 0.5848(3) 0.23555(17) 0.79173(19) 0.0230(7) Uani 1 d . . H6 H 0.6221 0.223 0.8329 0.028 Uiso 1 calc . . C7 C 0.5989(3) 0.28958(17) 0.7553(2) 0.0257(8) Uani 1 d . . H7 H 0.644 0.3208 0.7713 0.031 Uiso 1 calc . . C8 C 0.5372(3) 0.29201(16) 0.6909(2) 0.0239(7) Uani 1 d . . C9A C 0.2619(5) 0.1353(3) 0.8596(3) 0.0627(14) Uani 0.63(3) d A 1 H9A H 0.2475 0.1214 0.908 0.075 Uiso 0.63(3) calc A 1 C10A C 0.1735(9) 0.1223(9) 0.8195(6) 0.0627(14) Uani 0.63(3) d A 1 H10A H 0.1671 0.0788 0.8141 0.094 Uiso 0.63(3) calc A 1 H10B H 0.1782 0.1409 0.7733 0.094 Uiso 0.63(3) calc A 1 H10C H 0.1126 0.1378 0.8426 0.094 Uiso 0.63(3) calc A 1 C9B C 0.2619(5) 0.1353(3) 0.8596(3) 0.0627(14) Uani 0.37(3) d A 2 H9B H 0.2557 0.1246 0.9101 0.075 Uiso 0.37(3) calc A 2 C10B C 0.1786(15) 0.0944(15) 0.8243(11) 0.0627(14) Uani 0.37(3) d A 2 H10D H 0.1992 0.0524 0.8305 0.094 Uiso 0.37(3) calc A 2 H10E H 0.1721 0.1037 0.7742 0.094 Uiso 0.37(3) calc A 2 H10F H 0.1118 0.1011 0.8458 0.094 Uiso 0.37(3) calc A 2 C11 C 0.2581(5) 0.2037(3) 0.8625(4) 0.073(2) Uani 1 d . . H11A H 0.3183 0.2186 0.8901 0.11 Uiso 1 calc A 1 H11B H 0.1942 0.2165 0.8844 0.11 Uiso 1 calc A 1 H11C H 0.2595 0.2199 0.8149 0.11 Uiso 1 calc A 1 C12 C 0.4061(4) 0.0262(2) 0.8327(2) 0.0422(11) Uani 1 d . . H12 H 0.4811 0.0159 0.8285 0.051 Uiso 1 calc . . C13 C 0.3689(7) -0.0084(3) 0.8960(3) 0.079(2) Uani 1 d . . H13A H 0.4058 0.0059 0.9386 0.119 Uiso 1 calc . . H13B H 0.3829 -0.0512 0.8899 0.119 Uiso 1 calc . . H13C H 0.2942 -0.0022 0.9003 0.119 Uiso 1 calc . . C14 C 0.3507(6) 0.0035(2) 0.7666(3) 0.0666(19) Uani 1 d . . H14A H 0.3753 0.0256 0.7262 0.1 Uiso 1 calc . . H14B H 0.2758 0.0095 0.77 0.1 Uiso 1 calc . . H14C H 0.3652 -0.0392 0.7609 0.1 Uiso 1 calc . . C15 C 0.4878(4) 0.13623(19) 0.9186(2) 0.0325(9) Uani 1 d . . H15 H 0.4981 0.1801 0.9113 0.039 Uiso 1 calc . . C16 C 0.4419(5) 0.1296(2) 0.9910(2) 0.0465(12) Uani 1 d . . H16A H 0.3727 0.1478 0.9904 0.07 Uiso 1 calc . . H16B H 0.487 0.1498 1.026 0.07 Uiso 1 calc . . H16C H 0.4366 0.0871 1.0027 0.07 Uiso 1 calc . . C17 C 0.5970(4) 0.1080(2) 0.9196(2) 0.0395(10) Uani 1 d . . H17A H 0.6267 0.1126 0.8735 0.059 Uiso 1 calc . . H17B H 0.592 0.0653 0.931 0.059 Uiso 1 calc . . H17C H 0.6416 0.1281 0.955 0.059 Uiso 1 calc . . C18 C 0.3805(5) 0.3922(2) 0.6979(3) 0.0528(13) Uani 1 d . . H18 H 0.3593 0.4321 0.6786 0.063 Uiso 1 calc . . C19 C 0.3999(4) 0.3992(2) 0.7741(3) 0.0463(12) Uani 1 d . . H19A H 0.4574 0.4272 0.7827 0.069 Uiso 1 calc . . H19B H 0.4178 0.3602 0.7948 0.069 Uiso 1 calc . . H19C H 0.3373 0.4147 0.7952 0.069 Uiso 1 calc . . C20 C 0.2902(5) 0.3487(3) 0.6836(4) 0.0644(16) Uani 1 d . . H20A H 0.2779 0.3443 0.633 0.097 Uiso 1 calc . . H20B H 0.2275 0.3645 0.7045 0.097 Uiso 1 calc . . H20C H 0.3074 0.3097 0.7042 0.097 Uiso 1 calc . . C21 C 0.4653(6) 0.3682(2) 0.5557(3) 0.069(2) Uani 1 d . . H21 H 0.4377 0.3277 0.5425 0.083 Uiso 1 calc . . C22 C 0.3944(6) 0.4134(3) 0.5283(3) 0.071(2) Uani 1 d . . H22A H 0.3285 0.4105 0.5519 0.107 Uiso 1 calc . . H22B H 0.3822 0.4073 0.4779 0.107 Uiso 1 calc . . H22C H 0.4246 0.4532 0.5366 0.107 Uiso 1 calc . . C23 C 0.5665(6) 0.3836(3) 0.5071(3) 0.0642(16) Uani 1 d . . H23A H 0.6236 0.3562 0.5194 0.096 Uiso 1 calc . . H23B H 0.589 0.425 0.5158 0.096 Uiso 1 calc . . H23C H 0.5464 0.3788 0.4574 0.096 Uiso 1 calc . . C24 C 0.6107(5) 0.4216(3) 0.6771(3) 0.0550(14) Uani 1 d . . H24 H 0.612 0.4223 0.7294 0.066 Uiso 1 calc . . C25 C 0.5848(6) 0.4863(3) 0.6545(3) 0.0657(17) Uani 1 d . . H25A H 0.5145 0.4963 0.6682 0.099 Uiso 1 calc . . H25B H 0.5889 0.4897 0.6035 0.099 Uiso 1 calc . . H25C H 0.6346 0.5138 0.6773 0.099 Uiso 1 calc . . C26 C 0.7266(5) 0.3992(3) 0.6570(3) 0.073(2) Uani 1 d . . H26A H 0.7372 0.3579 0.6729 0.11 Uiso 1 calc . . H26B H 0.7788 0.4252 0.6799 0.11 Uiso 1 calc . . H26C H 0.7331 0.4011 0.6062 0.11 Uiso 1 calc . . C27 C 0.5184(3) 0.13391(16) 0.54204(18) 0.0218(7) Uani 1 d . . C28 C 0.5576(3) 0.07569(17) 0.56125(19) 0.0230(7) Uani 1 d . . H28 H 0.5209 0.0394 0.5526 0.028 Uiso 1 calc . . C29 C 0.6561(3) 0.07874(17) 0.59414(19) 0.0247(8) Uani 1 d . . H29 H 0.6941 0.0462 0.6143 0.03 Uiso 1 calc . . C53 C 0.6067(4) 0.0742(2) 0.7300(2) 0.0471(13) Uani 1 d . . C30 C 0.6894(3) 0.14003(16) 0.59190(18) 0.0205(7) Uani 1 d . . C31 C 0.6046(3) 0.17429(16) 0.56096(18) 0.0196(7) Uani 1 d . . C32 C 0.6394(3) 0.23500(17) 0.55587(18) 0.0212(7) Uani 1 d . . H32 H 0.5988 0.2682 0.5403 0.025 Uiso 1 calc . . C33 C 0.7445(3) 0.23635(17) 0.57813(19) 0.0232(7) Uani 1 d . . H33 H 0.7873 0.2708 0.5761 0.028 Uiso 1 calc . . C34 C 0.7791(3) 0.17943(17) 0.60434(19) 0.0230(7) Uani 1 d . . C35 C 0.2869(3) 0.10364(18) 0.5060(2) 0.0270(8) Uani 1 d . . H35 H 0.2521 0.1335 0.5363 0.032 Uiso 1 calc . . C36 C 0.2092(3) 0.0879(2) 0.4461(2) 0.0337(9) Uani 1 d . . H36A H 0.1956 0.1234 0.4171 0.05 Uiso 1 calc . . H36B H 0.1442 0.0741 0.4656 0.05 Uiso 1 calc . . H36C H 0.2381 0.0561 0.4174 0.05 Uiso 1 calc . . C37 C 0.3063(3) 0.04742(19) 0.5507(2) 0.0315(9) Uani 1 d . . H37A H 0.3557 0.0568 0.5894 0.047 Uiso 1 calc . . H37B H 0.3349 0.0157 0.5217 0.047 Uiso 1 calc . . H37C H 0.2408 0.0339 0.5696 0.047 Uiso 1 calc . . C38 C 0.3852(3) 0.22324(18) 0.4570(2) 0.0273(8) Uani 1 d . . H38 H 0.3932 0.2436 0.5035 0.033 Uiso 1 calc . . C39 C 0.2762(4) 0.2390(2) 0.4281(3) 0.0411(11) Uani 1 d . . H39A H 0.2244 0.221 0.458 0.062 Uiso 1 calc . . H39B H 0.2668 0.2234 0.3804 0.062 Uiso 1 calc . . H39C H 0.2677 0.2825 0.4276 0.062 Uiso 1 calc . . C40 C 0.4664(4) 0.2519(2) 0.4100(2) 0.0358(10) Uani 1 d . . H40A H 0.5363 0.242 0.4284 0.054 Uiso 1 calc . . H40B H 0.4575 0.2955 0.4097 0.054 Uiso 1 calc . . H40C H 0.457 0.2365 0.3622 0.054 Uiso 1 calc . . C41 C 0.4592(3) 0.0988(2) 0.3950(2) 0.0326(9) Uani 1 d . . H41 H 0.4515 0.0553 0.4061 0.039 Uiso 1 calc . . C54 C 0.7484(4) 0.1672(2) 0.7505(2) 0.0445(11) Uani 1 d . . C42 C 0.3974(4) 0.1089(2) 0.3255(2) 0.0421(11) Uani 1 d . . H42A H 0.3234 0.1023 0.3326 0.063 Uiso 1 calc . . H42B H 0.4213 0.0807 0.2903 0.063 Uiso 1 calc . . H42C H 0.4082 0.15 0.3094 0.063 Uiso 1 calc . . C43 C 0.5754(4) 0.1087(3) 0.3835(2) 0.0470(12) Uani 1 d . . H43A H 0.6149 0.1022 0.4277 0.07 Uiso 1 calc . . H43B H 0.5864 0.1497 0.3673 0.07 Uiso 1 calc . . H43C H 0.5989 0.0804 0.3483 0.07 Uiso 1 calc . . C44 C 0.9634(4) 0.0996(2) 0.6717(3) 0.0488(13) Uani 1 d . . H44 H 0.9707 0.1163 0.7202 0.059 Uiso 1 calc . . C45 C 0.8884(4) 0.0457(3) 0.6725(3) 0.0543(14) Uani 1 d . . H45A H 0.8197 0.0593 0.6859 0.081 Uiso 1 calc . . H45B H 0.9149 0.0159 0.7064 0.081 Uiso 1 calc . . H45C H 0.8832 0.0276 0.6258 0.081 Uiso 1 calc . . C46 C 1.0697(4) 0.0732(3) 0.6515(4) 0.0622(17) Uani 1 d . . H46A H 1.1213 0.1054 0.6505 0.093 Uiso 1 calc . . H46B H 1.0627 0.0546 0.6052 0.093 Uiso 1 calc . . H46C H 1.0922 0.0431 0.6862 0.093 Uiso 1 calc . . C47 C 0.9580(4) 0.1388(2) 0.5178(3) 0.0428(11) Uani 1 d . . H47 H 1.0342 0.1304 0.5194 0.051 Uiso 1 calc . . C48 C 0.9033(4) 0.0822(3) 0.4901(4) 0.0579(15) Uani 1 d . . H48A H 0.9151 0.0494 0.5235 0.087 Uiso 1 calc . . H48B H 0.9311 0.0711 0.4449 0.087 Uiso 1 calc . . H48C H 0.8286 0.0899 0.4842 0.087 Uiso 1 calc . . C49 C 0.9387(6) 0.1890(3) 0.4650(3) 0.0638(17) Uani 1 d . . H49A H 0.9735 0.2255 0.4819 0.096 Uiso 1 calc . . H49B H 0.8639 0.1964 0.4592 0.096 Uiso 1 calc . . H49C H 0.9662 0.1774 0.4198 0.096 Uiso 1 calc . . C50 C 0.9913(3) 0.2343(2) 0.6308(2) 0.0339(9) Uani 1 d . . H50 H 0.9629 0.2648 0.5968 0.041 Uiso 1 calc . . C51 C 0.9709(5) 0.2580(4) 0.7035(4) 0.085(3) Uani 1 d . . H51A H 0.8959 0.2599 0.7098 0.128 Uiso 1 calc . . H51B H 1.0008 0.2981 0.7089 0.128 Uiso 1 calc . . H51C H 1.0028 0.2312 0.7387 0.128 Uiso 1 calc . . C52 C 1.1090(4) 0.2318(3) 0.6211(4) 0.0575(16) Uani 1 d . . H52A H 1.1225 0.2169 0.5741 0.086 Uiso 1 calc . . H52B H 1.1411 0.2048 0.6561 0.086 Uiso 1 calc . . H52C H 1.1386 0.2719 0.627 0.086 Uiso 1 calc . . O1 O 0.6486(3) 0.04083(19) 0.7663(2) 0.0585(10) Uani 1 d . . O2 O 0.8011(3) 0.14290(19) 0.7904(2) 0.0596(10) Uani 1 d . . Si1 Si 0.40021(8) 0.10993(5) 0.84292(5) 0.0252(2) Uani 1 d . . Si2 Si 0.50774(10) 0.36754(5) 0.65145(6) 0.0318(3) Uani 1 d . . Si3 Si 0.41039(8) 0.14103(5) 0.47396(5) 0.0214(2) Uani 1 d . . Si4 Si 0.92187(8) 0.16186(5) 0.60978(6) 0.0264(2) Uani 1 d . . Ti1 Ti 0.53077(5) 0.13360(3) 0.66108(3) 0.01847(16) Uani 1 d . . Ti2 Ti 0.65290(5) 0.21533(3) 0.67804(3) 0.02027(16) Uani 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 C1 0.0191(16) 0.0181(17) 0.0225(16) -0.0001(13) 0.0029(13) 0.0003(13) C2 0.0164(16) 0.0233(18) 0.0234(17) -0.0040(14) 0.0024(13) 0.0004(13) C3 0.0171(16) 0.0216(18) 0.0207(16) -0.0020(13) 0.0012(13) 0.0041(13) C4 0.0190(17) 0.0181(17) 0.0237(17) 0.0008(13) 0.0031(13) 0.0025(13) C5 0.0185(16) 0.0196(17) 0.0221(16) -0.0002(13) 0.0018(13) -0.0001(13) C6 0.0219(18) 0.0247(19) 0.0225(17) 0.0009(14) 0.0017(13) -0.0026(14) C7 0.030(2) 0.0199(18) 0.0273(18) -0.0042(14) 0.0042(15) -0.0036(15) C8 0.0234(18) 0.0186(18) 0.0301(19) 0.0003(14) 0.0052(14) 0.0026(14) C9A 0.046(2) 0.083(4) 0.061(3) 0.010(3) 0.019(2) 0.001(3) C10A 0.046(2) 0.083(4) 0.061(3) 0.010(3) 0.019(2) 0.001(3) C9B 0.046(2) 0.083(4) 0.061(3) 0.010(3) 0.019(2) 0.001(3) C10B 0.046(2) 0.083(4) 0.061(3) 0.010(3) 0.019(2) 0.001(3) C11 0.060(4) 0.091(5) 0.069(4) -0.017(4) 0.016(3) 0.040(4) C12 0.060(3) 0.028(2) 0.038(2) 0.0023(18) 0.000(2) -0.011(2) C13 0.149(7) 0.045(3) 0.042(3) 0.015(2) -0.015(4) -0.048(4) C14 0.135(6) 0.030(3) 0.033(3) -0.003(2) -0.005(3) -0.027(3) C15 0.045(2) 0.027(2) 0.0263(19) 0.0002(16) 0.0037(17) -0.0069(18) C16 0.066(3) 0.051(3) 0.022(2) -0.0032(19) 0.005(2) -0.006(3) C17 0.042(3) 0.044(3) 0.032(2) 0.0030(19) -0.0026(18) -0.006(2) C18 0.065(4) 0.035(3) 0.058(3) 0.007(2) 0.007(3) 0.008(2) C19 0.055(3) 0.044(3) 0.041(3) 0.003(2) 0.012(2) 0.010(2) C20 0.051(3) 0.057(4) 0.087(5) 0.005(3) 0.011(3) 0.006(3) C21 0.097(5) 0.034(3) 0.073(4) -0.019(3) -0.049(4) 0.028(3) C22 0.125(6) 0.046(3) 0.042(3) 0.018(2) -0.021(3) -0.005(4) C23 0.092(5) 0.053(4) 0.049(3) 0.001(3) 0.014(3) -0.004(3) C24 0.069(4) 0.044(3) 0.053(3) 0.004(2) 0.002(3) -0.009(3) C25 0.093(5) 0.039(3) 0.065(4) 0.000(3) -0.001(3) -0.012(3) C26 0.074(4) 0.091(5) 0.056(3) -0.011(3) 0.022(3) -0.055(4) C27 0.0227(18) 0.0213(18) 0.0217(16) -0.0001(13) 0.0031(13) 0.0021(14) C28 0.0256(18) 0.0197(18) 0.0239(17) -0.0018(14) 0.0047(14) 0.0028(14) C29 0.0244(18) 0.0242(19) 0.0258(18) 0.0042(14) 0.0052(14) 0.0077(15) C53 0.057(3) 0.050(3) 0.035(2) 0.015(2) 0.014(2) 0.030(2) C30 0.0168(16) 0.0225(18) 0.0226(16) 0.0012(13) 0.0039(13) 0.0058(13) C31 0.0177(16) 0.0222(18) 0.0191(16) 0.0031(13) 0.0034(12) 0.0031(13) C32 0.0222(17) 0.0212(18) 0.0205(16) 0.0052(13) 0.0035(13) 0.0043(14) C33 0.0196(17) 0.0260(19) 0.0245(17) 0.0029(14) 0.0068(13) 0.0004(14) C34 0.0183(17) 0.028(2) 0.0229(17) 0.0033(14) 0.0034(13) 0.0024(14) C35 0.0226(18) 0.028(2) 0.0306(19) -0.0067(15) 0.0014(15) -0.0009(15) C36 0.027(2) 0.035(2) 0.038(2) -0.0084(18) -0.0014(17) -0.0037(17) C37 0.030(2) 0.029(2) 0.037(2) -0.0056(17) 0.0106(17) -0.0070(17) C38 0.031(2) 0.029(2) 0.0218(17) 0.0040(15) -0.0037(15) 0.0010(16) C39 0.039(2) 0.035(2) 0.049(3) 0.000(2) -0.010(2) 0.008(2) C40 0.039(2) 0.035(2) 0.033(2) 0.0096(17) -0.0026(18) -0.0023(18) C41 0.040(2) 0.033(2) 0.0249(19) -0.0014(16) 0.0044(16) 0.0059(18) C54 0.049(3) 0.052(3) 0.032(2) 0.001(2) -0.003(2) 0.018(2) C42 0.055(3) 0.046(3) 0.025(2) -0.0074(19) 0.0014(19) -0.002(2) C43 0.045(3) 0.066(4) 0.031(2) -0.001(2) 0.012(2) 0.017(2) C44 0.030(2) 0.049(3) 0.066(3) 0.026(3) -0.010(2) -0.001(2) C45 0.046(3) 0.059(4) 0.057(3) 0.012(3) -0.003(2) 0.005(3) C46 0.027(2) 0.044(3) 0.114(5) 0.019(3) -0.014(3) 0.006(2) C47 0.030(2) 0.041(3) 0.059(3) -0.020(2) 0.017(2) -0.0025(19) C48 0.040(3) 0.053(3) 0.082(4) -0.027(3) 0.010(3) -0.003(2) C49 0.087(5) 0.074(4) 0.032(3) -0.005(3) 0.023(3) -0.010(4) C50 0.0208(19) 0.036(2) 0.045(2) -0.0079(19) 0.0023(17) -0.0009(17) C51 0.047(3) 0.134(7) 0.076(4) -0.063(5) 0.010(3) -0.028(4) C52 0.026(2) 0.049(3) 0.098(5) -0.024(3) 0.008(3) -0.005(2) O1 0.064(2) 0.066(3) 0.046(2) 0.0147(18) 0.0053(18) 0.023(2) O2 0.063(3) 0.070(3) 0.045(2) 0.0045(19) -0.0043(18) 0.019(2) Si1 0.0285(5) 0.0262(5) 0.0212(5) 0.0014(4) 0.0046(4) -0.0049(4) Si2 0.0524(7) 0.0162(5) 0.0272(5) 0.0013(4) 0.0035(5) -0.0007(5) Si3 0.0209(5) 0.0224(5) 0.0210(5) -0.0023(4) 0.0001(4) 0.0018(4) Si4 0.0155(5) 0.0273(6) 0.0365(6) 0.0066(4) 0.0029(4) 0.0017(4) Ti1 0.0176(3) 0.0179(3) 0.0201(3) 0.0023(2) 0.0033(2) 0.0026(2) Ti2 0.0168(3) 0.0218(3) 0.0224(3) 0.0016(2) 0.0021(2) 0.0005(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.436(5) . ? C1 C5 1.461(5) . ? C1 Si1 1.886(4) . ? C1 Ti1 2.338(4) . ? C2 C3 1.397(5) . ? C2 Ti1 2.330(3) . ? C2 H2 0.95 . ? C3 C4 1.439(5) . ? C3 Ti1 2.375(3) . ? C3 H3 0.95 . ? C4 C5 1.445(5) . ? C4 C8 1.479(5) . ? C4 Ti2 2.356(4) . ? C4 Ti1 2.477(4) . ? C5 C6 1.435(5) . ? C5 Ti1 2.410(4) . ? C5 Ti2 2.485(4) . ? C6 C7 1.409(5) . ? C6 Ti2 2.417(4) . ? C6 H6 0.95 . ? C7 C8 1.441(5) . ? C7 Ti2 2.344(4) . ? C7 H7 0.95 . ? C8 Si2 1.881(4) . ? C8 Ti2 2.291(4) . ? C9A C10A 1.380(13) . ? C9A C11 1.530(9) . ? C9A Si1 1.910(6) . ? C9A H9A 1 . ? C10A H10A 0.98 . ? C10A H10B 0.98 . ? C10A H10C 0.98 . ? C10B H10D 0.98 . ? C10B H10E 0.98 . ? C10B H10F 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C14 1.515(7) . ? C12 C13 1.528(7) . ? C12 Si1 1.883(5) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.532(6) . ? C15 C17 1.543(7) . ? C15 Si1 1.894(4) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.475(8) . ? C18 C20 1.533(9) . ? C18 Si2 1.974(6) . ? C18 H18 1 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.448(8) . ? C21 C23 1.667(10) . ? C21 Si2 1.890(6) . ? C21 H21 1 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C25 1.542(8) . ? C24 C26 1.634(9) . ? C24 Si2 1.847(6) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.438(5) . ? C27 C31 1.467(5) . ? C27 Si3 1.876(4) . ? C27 Ti1 2.275(4) . ? C28 C29 1.397(5) . ? C28 Ti1 2.342(4) . ? C28 H28 0.95 . ? C29 C30 1.436(5) . ? C29 Ti1 2.431(4) . ? C29 H29 0.95 . ? C53 O1 1.141(6) . ? C53 Ti1 2.087(5) . ? C30 C31 1.443(5) . ? C30 C34 1.465(5) . ? C30 Ti2 2.413(4) . ? C30 Ti1 2.482(4) . ? C31 C32 1.433(5) . ? C31 Ti1 2.352(3) . ? C31 Ti2 2.476(4) . ? C32 C33 1.405(5) . ? C32 Ti2 2.376(3) . ? C32 H32 0.95 . ? C33 C34 1.432(5) . ? C33 Ti2 2.331(4) . ? C33 H33 0.95 . ? C34 Si4 1.881(4) . ? C34 Ti2 2.334(4) . ? C35 C36 1.532(5) . ? C35 C37 1.535(6) . ? C35 Si3 1.919(4) . ? C35 H35 1 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.530(6) . ? C38 C40 1.544(6) . ? C38 Si3 1.891(4) . ? C38 H38 1 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C43 1.538(7) . ? C41 C42 1.539(6) . ? C41 Si3 1.907(4) . ? C41 H41 1 . ? C54 O2 1.140(6) . ? C54 Ti2 2.111(5) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.544(8) . ? C44 C46 1.553(8) . ? C44 Si4 1.891(5) . ? C44 H44 1 . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? C47 C49 1.523(8) . ? C47 C48 1.532(7) . ? C47 Si4 1.907(5) . ? C47 H47 1 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 C51 1.519(7) . ? C50 C52 1.538(6) . ? C50 Si4 1.886(5) . ? C50 H50 1 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? Ti1 Ti2 2.4250(10) . ? 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 C2 C1 C5 103.4(3) . . ? C2 C1 Si1 122.7(3) . . ? C5 C1 Si1 127.9(3) . . ? C2 C1 Ti1 71.75(19) . . ? C5 C1 Ti1 74.8(2) . . ? Si1 C1 Ti1 138.55(19) . . ? C3 C2 C1 112.3(3) . . ? C3 C2 Ti1 74.5(2) . . ? C1 C2 Ti1 72.4(2) . . ? C3 C2 H2 123.9 . . ? C1 C2 H2 123.9 . . ? Ti1 C2 H2 120.7 . . ? C2 C3 C4 107.6(3) . . ? C2 C3 Ti1 71.0(2) . . ? C4 C3 Ti1 76.7(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Ti1 C3 H3 118.1 . . ? C3 C4 C5 106.5(3) . . ? C3 C4 C8 143.8(3) . . ? C5 C4 C8 109.5(3) . . ? C3 C4 Ti2 124.0(2) . . ? C5 C4 Ti2 77.6(2) . . ? C8 C4 Ti2 69.07(19) . . ? C3 C4 Ti1 68.91(19) . . ? C5 C4 Ti1 70.3(2) . . ? C8 C4 Ti1 128.2(2) . . ? Ti2 C4 Ti1 60.17(8) . . ? C6 C5 C4 107.3(3) . . ? C6 C5 C1 142.6(3) . . ? C4 C5 C1 109.9(3) . . ? C6 C5 Ti1 124.4(2) . . ? C4 C5 Ti1 75.4(2) . . ? C1 C5 Ti1 69.41(19) . . ? C6 C5 Ti2 70.4(2) . . ? C4 C5 Ti2 67.79(19) . . ? C1 C5 Ti2 127.7(2) . . ? Ti1 C5 Ti2 59.36(8) . . ? C7 C6 C5 107.5(3) . . ? C7 C6 Ti2 70.0(2) . . ? C5 C6 Ti2 75.6(2) . . ? C7 C6 H6 126.2 . . ? C5 C6 H6 126.2 . . ? Ti2 C6 H6 120 . . ? C6 C7 C8 112.1(3) . . ? C6 C7 Ti2 75.7(2) . . ? C8 C7 Ti2 69.9(2) . . ? C6 C7 H7 123.9 . . ? C8 C7 H7 123.9 . . ? Ti2 C7 H7 122 . . ? C7 C8 C4 103.3(3) . . ? C7 C8 Si2 118.2(3) . . ? C4 C8 Si2 131.7(3) . . ? C7 C8 Ti2 73.9(2) . . ? C4 C8 Ti2 73.8(2) . . ? Si2 C8 Ti2 138.6(2) . . ? C10A C9A C11 101.8(10) . . ? C10A C9A Si1 126.9(7) . . ? C11 C9A Si1 109.5(4) . . ? C10A C9A H9A 105.7 . . ? C11 C9A H9A 105.7 . . ? Si1 C9A H9A 105.7 . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? H10D C10B H10E 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C9A C11 H11A 109.5 . . ? C9A C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9A C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109.8(4) . . ? C14 C12 Si1 113.5(4) . . ? C13 C12 Si1 114.0(4) . . ? C14 C12 H12 106.3 . . ? C13 C12 H12 106.3 . . ? Si1 C12 H12 106.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 109.4(4) . . ? C16 C15 Si1 114.8(3) . . ? C17 C15 Si1 113.6(3) . . ? C16 C15 H15 106.1 . . ? C17 C15 H15 106.1 . . ? Si1 C15 H15 106.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 110.0(5) . . ? C19 C18 Si2 111.2(4) . . ? C20 C18 Si2 112.4(4) . . ? C19 C18 H18 107.7 . . ? C20 C18 H18 107.7 . . ? Si2 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 98.6(6) . . ? C22 C21 Si2 120.7(4) . . ? C23 C21 Si2 109.7(4) . . ? C22 C21 H21 109 . . ? C23 C21 H21 109 . . ? Si2 C21 H21 109 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 114.3(5) . . ? C25 C24 Si2 113.1(4) . . ? C26 C24 Si2 113.1(4) . . ? C25 C24 H24 105.1 . . ? C26 C24 H24 105.1 . . ? Si2 C24 H24 105.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C31 103.7(3) . . ? C28 C27 Si3 119.9(3) . . ? C31 C27 Si3 130.9(3) . . ? C28 C27 Ti1 74.4(2) . . ? C31 C27 Ti1 74.4(2) . . ? Si3 C27 Ti1 135.72(19) . . ? C29 C28 C27 112.1(3) . . ? C29 C28 Ti1 76.5(2) . . ? C27 C28 Ti1 69.3(2) . . ? C29 C28 H28 124 . . ? C27 C28 H28 124 . . ? Ti1 C28 H28 121.7 . . ? C28 C29 C30 107.5(3) . . ? C28 C29 Ti1 69.5(2) . . ? C30 C29 Ti1 75.0(2) . . ? C28 C29 H29 126.2 . . ? C30 C29 H29 126.2 . . ? Ti1 C29 H29 121 . . ? O1 C53 Ti1 178.2(5) . . ? C29 C30 C31 107.2(3) . . ? C29 C30 C34 143.4(3) . . ? C31 C30 C34 109.2(3) . . ? C29 C30 Ti2 125.3(2) . . ? C31 C30 Ti2 75.2(2) . . ? C34 C30 Ti2 69.1(2) . . ? C29 C30 Ti1 71.1(2) . . ? C31 C30 Ti1 67.79(19) . . ? C34 C30 Ti1 127.6(2) . . ? Ti2 C30 Ti1 59.38(8) . . ? C32 C31 C30 107.2(3) . . ? C32 C31 C27 143.3(3) . . ? C30 C31 C27 109.3(3) . . ? C32 C31 Ti1 123.9(2) . . ? C30 C31 Ti1 77.6(2) . . ? C27 C31 Ti1 68.66(19) . . ? C32 C31 Ti2 69.0(2) . . ? C30 C31 Ti2 70.5(2) . . ? C27 C31 Ti2 127.8(2) . . ? Ti1 C31 Ti2 60.23(8) . . ? C33 C32 C31 107.5(3) . . ? C33 C32 Ti2 70.9(2) . . ? C31 C32 Ti2 76.7(2) . . ? C33 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? Ti2 C32 H32 118.1 . . ? C32 C33 C34 111.8(3) . . ? C32 C33 Ti2 74.4(2) . . ? C34 C33 Ti2 72.3(2) . . ? C32 C33 H33 124.1 . . ? C34 C33 H33 124.1 . . ? Ti2 C33 H33 120.8 . . ? C33 C34 C30 104.1(3) . . ? C33 C34 Si4 119.7(3) . . ? C30 C34 Si4 130.4(3) . . ? C33 C34 Ti2 72.0(2) . . ? C30 C34 Ti2 75.0(2) . . ? Si4 C34 Ti2 137.86(19) . . ? C36 C35 C37 108.4(3) . . ? C36 C35 Si3 112.9(3) . . ? C37 C35 Si3 114.4(3) . . ? C36 C35 H35 106.9 . . ? C37 C35 H35 106.9 . . ? Si3 C35 H35 106.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C40 109.2(3) . . ? C39 C38 Si3 115.7(3) . . ? C40 C38 Si3 112.7(3) . . ? C39 C38 H38 106.1 . . ? C40 C38 H38 106.1 . . ? Si3 C38 H38 106.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C42 109.3(4) . . ? C43 C41 Si3 113.2(3) . . ? C42 C41 Si3 115.8(3) . . ? C43 C41 H41 105.9 . . ? C42 C41 H41 105.9 . . ? Si3 C41 H41 105.9 . . ? O2 C54 Ti2 177.9(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C46 105.4(5) . . ? C45 C44 Si4 114.7(3) . . ? C46 C44 Si4 110.8(4) . . ? C45 C44 H44 108.6 . . ? C46 C44 H44 108.6 . . ? Si4 C44 H44 108.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C48 108.5(5) . . ? C49 C47 Si4 111.8(3) . . ? C48 C47 Si4 114.6(4) . . ? C49 C47 H47 107.2 . . ? C48 C47 H47 107.2 . . ? Si4 C47 H47 107.2 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C52 109.2(4) . . ? C51 C50 Si4 113.4(4) . . ? C52 C50 Si4 113.9(3) . . ? C51 C50 H50 106.6 . . ? C52 C50 H50 106.6 . . ? Si4 C50 H50 106.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C12 Si1 C1 112.59(19) . . ? C12 Si1 C15 111.2(2) . . ? C1 Si1 C15 109.05(17) . . ? C12 Si1 C9A 110.7(3) . . ? C1 Si1 C9A 104.7(2) . . ? C15 Si1 C9A 108.3(3) . . ? C24 Si2 C8 110.4(2) . . ? C24 Si2 C21 115.5(3) . . ? C8 Si2 C21 116.2(2) . . ? C24 Si2 C18 107.5(3) . . ? C8 Si2 C18 103.2(2) . . ? C21 Si2 C18 102.6(3) . . ? C27 Si3 C38 108.65(17) . . ? C27 Si3 C41 104.39(18) . . ? C38 Si3 C41 113.88(18) . . ? C27 Si3 C35 110.18(17) . . ? C38 Si3 C35 109.75(18) . . ? C41 Si3 C35 109.84(19) . . ? C34 Si4 C50 106.74(18) . . ? C34 Si4 C44 116.2(2) . . ? C50 Si4 C44 112.2(2) . . ? C34 Si4 C47 106.2(2) . . ? C50 Si4 C47 107.3(2) . . ? C44 Si4 C47 107.7(3) . . ? C53 Ti1 C27 130.30(16) . . ? C53 Ti1 C2 109.98(16) . . ? C27 Ti1 C2 107.09(13) . . ? C53 Ti1 C1 80.62(15) . . ? C27 Ti1 C1 142.85(13) . . ? C2 Ti1 C1 35.84(12) . . ? C53 Ti1 C28 94.75(17) . . ? C27 Ti1 C28 36.26(13) . . ? C2 Ti1 C28 123.18(13) . . ? C1 Ti1 C28 148.71(13) . . ? C53 Ti1 C31 124.38(16) . . ? C27 Ti1 C31 36.91(13) . . ? C2 Ti1 C31 125.60(13) . . ? C1 Ti1 C31 147.22(13) . . ? C28 Ti1 C31 58.25(13) . . ? C53 Ti1 C3 140.49(15) . . ? C27 Ti1 C3 86.87(13) . . ? C2 Ti1 C3 34.52(12) . . ? C1 Ti1 C3 59.87(12) . . ? C28 Ti1 C3 118.41(13) . . ? C31 Ti1 C3 92.80(12) . . ? C53 Ti1 C5 90.88(17) . . ? C27 Ti1 C5 137.57(13) . . ? C2 Ti1 C5 57.31(12) . . ? C1 Ti1 C5 35.79(12) . . ? C28 Ti1 C5 173.50(13) . . ? C31 Ti1 C5 115.71(13) . . ? C3 Ti1 C5 57.74(12) . . ? C53 Ti1 Ti2 96.19(18) . . ? C27 Ti1 Ti2 98.74(10) . . ? C2 Ti1 Ti2 112.88(10) . . ? C1 Ti1 Ti2 97.11(9) . . ? C28 Ti1 Ti2 114.17(10) . . ? C31 Ti1 Ti2 62.41(9) . . ? C3 Ti1 Ti2 89.44(9) . . ? C5 Ti1 Ti2 61.86(9) . . ? C53 Ti1 C29 72.94(15) . . ? C27 Ti1 C29 59.86(13) . . ? C2 Ti1 C29 155.47(13) . . ? C1 Ti1 C29 153.13(13) . . ? C28 Ti1 C29 33.97(13) . . ? C31 Ti1 C29 57.92(12) . . ? C3 Ti1 C29 146.30(12) . . ? C5 Ti1 C29 146.69(13) . . ? Ti2 Ti1 C29 90.50(10) . . ? C53 Ti1 C4 124.53(17) . . ? C27 Ti1 C4 103.22(12) . . ? C2 Ti1 C4 56.75(12) . . ? C1 Ti1 C4 59.14(12) . . ? C28 Ti1 C4 139.45(12) . . ? C31 Ti1 C4 88.12(12) . . ? C3 Ti1 C4 34.41(12) . . ? C5 Ti1 C4 34.36(11) . . ? Ti2 Ti1 C4 57.43(9) . . ? C29 Ti1 C4 142.66(13) . . ? C53 Ti1 C30 89.83(16) . . ? C27 Ti1 C30 59.66(12) . . ? C2 Ti1 C30 159.76(13) . . ? C1 Ti1 C30 153.23(13) . . ? C28 Ti1 C30 56.46(13) . . ? C31 Ti1 C30 34.60(11) . . ? C3 Ti1 C30 125.49(12) . . ? C5 Ti1 C30 120.45(12) . . ? Ti2 Ti1 C30 58.89(9) . . ? C29 Ti1 C30 33.98(12) . . ? C4 Ti1 C30 108.91(12) . . ? C54 Ti2 C8 132.54(17) . . ? C54 Ti2 C33 109.81(17) . . ? C8 Ti2 C33 106.82(14) . . ? C54 Ti2 C34 79.53(16) . . ? C8 Ti2 C34 142.50(13) . . ? C33 Ti2 C34 35.75(13) . . ? C54 Ti2 C7 97.28(17) . . ? C8 Ti2 C7 36.21(14) . . ? C33 Ti2 C7 123.04(14) . . ? C34 Ti2 C7 148.61(14) . . ? C54 Ti2 C4 124.59(17) . . ? C8 Ti2 C4 37.09(13) . . ? C33 Ti2 C4 125.36(13) . . ? C34 Ti2 C4 146.99(13) . . ? C7 Ti2 C4 58.35(13) . . ? C54 Ti2 C32 139.27(16) . . ? C8 Ti2 C32 86.75(13) . . ? C33 Ti2 C32 34.72(12) . . ? C34 Ti2 C32 59.82(12) . . ? C7 Ti2 C32 118.41(13) . . ? C4 Ti2 C32 92.43(13) . . ? C54 Ti2 C30 88.19(16) . . ? C8 Ti2 C30 137.68(13) . . ? C33 Ti2 C30 57.55(13) . . ? C34 Ti2 C30 35.92(13) . . ? C7 Ti2 C30 173.52(13) . . ? C4 Ti2 C30 115.58(13) . . ? C32 Ti2 C30 57.81(12) . . ? C54 Ti2 C6 74.25(16) . . ? C8 Ti2 C6 60.22(13) . . ? C33 Ti2 C6 155.73(14) . . ? C34 Ti2 C6 153.15(13) . . ? C7 Ti2 C6 34.38(13) . . ? C4 Ti2 C6 58.11(12) . . ? C32 Ti2 C6 146.44(13) . . ? C30 Ti2 C6 146.18(13) . . ? C54 Ti2 Ti1 93.66(16) . . ? C8 Ti2 Ti1 98.93(10) . . ? C33 Ti2 Ti1 112.88(10) . . ? C34 Ti2 Ti1 97.16(10) . . ? C7 Ti2 Ti1 114.23(10) . . ? C4 Ti2 Ti1 62.40(9) . . ? C32 Ti2 Ti1 89.13(10) . . ? C30 Ti2 Ti1 61.73(9) . . ? C6 Ti2 Ti1 90.26(9) . . ? C54 Ti2 C31 121.63(16) . . ? C8 Ti2 C31 103.39(13) . . ? C33 Ti2 C31 56.77(13) . . ? C34 Ti2 C31 58.97(12) . . ? C7 Ti2 C31 139.56(13) . . ? C4 Ti2 C31 88.08(12) . . ? C32 Ti2 C31 34.28(12) . . ? C30 Ti2 C31 34.30(11) . . ? C6 Ti2 C31 142.58(12) . . ? Ti1 Ti2 C31 57.36(8) . . ? C54 Ti2 C5 89.99(17) . . ? C8 Ti2 C5 59.81(13) . . ? C33 Ti2 C5 159.52(13) . . ? C34 Ti2 C5 153.32(13) . . ? C7 Ti2 C5 56.61(12) . . ? C4 Ti2 C5 34.60(12) . . ? C32 Ti2 C5 125.06(12) . . ? C30 Ti2 C5 120.21(12) . . ? C6 Ti2 C5 33.99(12) . . ? Ti1 Ti2 C5 58.78(8) . . ? C31 Ti2 C5 108.75(12) . . ? 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 C5 C1 C2 C3 4.4(4) . . . . ? Si1 C1 C2 C3 159.0(3) . . . . ? Ti1 C1 C2 C3 -64.4(3) . . . . ? C5 C1 C2 Ti1 68.7(2) . . . . ? Si1 C1 C2 Ti1 -136.6(3) . . . . ? C1 C2 C3 C4 -5.5(4) . . . . ? Ti1 C2 C3 C4 -68.6(2) . . . . ? C1 C2 C3 Ti1 63.1(3) . . . . ? C2 C3 C4 C5 4.2(4) . . . . ? Ti1 C3 C4 C5 -60.6(2) . . . . ? C2 C3 C4 C8 -168.8(5) . . . . ? Ti1 C3 C4 C8 126.5(5) . . . . ? C2 C3 C4 Ti2 90.2(3) . . . . ? Ti1 C3 C4 Ti2 25.4(2) . . . . ? C2 C3 C4 Ti1 64.7(2) . . . . ? C3 C4 C5 C6 -178.3(3) . . . . ? C8 C4 C5 C6 -2.7(4) . . . . ? Ti2 C4 C5 C6 59.6(3) . . . . ? Ti1 C4 C5 C6 122.0(3) . . . . ? C3 C4 C5 C1 -1.5(4) . . . . ? C8 C4 C5 C1 174.1(3) . . . . ? Ti2 C4 C5 C1 -123.7(3) . . . . ? Ti1 C4 C5 C1 -61.2(2) . . . . ? C3 C4 C5 Ti1 59.7(2) . . . . ? C8 C4 C5 Ti1 -124.7(3) . . . . ? Ti2 C4 C5 Ti1 -62.47(7) . . . . ? C3 C4 C5 Ti2 122.1(3) . . . . ? C8 C4 C5 Ti2 -62.3(2) . . . . ? Ti1 C4 C5 Ti2 62.47(7) . . . . ? C2 C1 C5 C6 173.3(5) . . . . ? Si1 C1 C5 C6 20.4(7) . . . . ? Ti1 C1 C5 C6 -120.2(5) . . . . ? C2 C1 C5 C4 -1.6(4) . . . . ? Si1 C1 C5 C4 -154.5(3) . . . . ? Ti1 C1 C5 C4 64.9(3) . . . . ? C2 C1 C5 Ti1 -66.5(2) . . . . ? Si1 C1 C5 Ti1 140.6(3) . . . . ? C2 C1 C5 Ti2 -78.4(3) . . . . ? Si1 C1 C5 Ti2 128.7(3) . . . . ? Ti1 C1 C5 Ti2 -11.9(2) . . . . ? C4 C5 C6 C7 5.2(4) . . . . ? C1 C5 C6 C7 -169.7(5) . . . . ? Ti1 C5 C6 C7 89.0(4) . . . . ? Ti2 C5 C6 C7 63.1(3) . . . . ? C4 C5 C6 Ti2 -57.9(2) . . . . ? C1 C5 C6 Ti2 127.1(5) . . . . ? Ti1 C5 C6 Ti2 25.9(2) . . . . ? C5 C6 C7 C8 -6.0(4) . . . . ? Ti2 C6 C7 C8 60.9(3) . . . . ? C5 C6 C7 Ti2 -66.9(3) . . . . ? C6 C7 C8 C4 4.2(4) . . . . ? Ti2 C7 C8 C4 68.5(2) . . . . ? C6 C7 C8 Si2 158.7(3) . . . . ? Ti2 C7 C8 Si2 -137.0(3) . . . . ? C6 C7 C8 Ti2 -64.3(3) . . . . ? C3 C4 C8 C7 172.0(5) . . . . ? C5 C4 C8 C7 -0.8(4) . . . . ? Ti2 C4 C8 C7 -68.6(2) . . . . ? Ti1 C4 C8 C7 -80.6(4) . . . . ? C3 C4 C8 Si2 22.6(7) . . . . ? C5 C4 C8 Si2 -150.3(3) . . . . ? Ti2 C4 C8 Si2 142.0(3) . . . . ? Ti1 C4 C8 Si2 129.9(3) . . . . ? C3 C4 C8 Ti2 -119.4(5) . . . . ? C5 C4 C8 Ti2 67.8(3) . . . . ? Ti1 C4 C8 Ti2 -12.0(2) . . . . ? C31 C27 C28 C29 4.2(4) . . . . ? Si3 C27 C28 C29 160.8(3) . . . . ? Ti1 C27 C28 C29 -65.0(3) . . . . ? C31 C27 C28 Ti1 69.2(2) . . . . ? Si3 C27 C28 Ti1 -134.2(3) . . . . ? C27 C28 C29 C30 -5.2(4) . . . . ? Ti1 C28 C29 C30 -65.9(3) . . . . ? C27 C28 C29 Ti1 60.7(3) . . . . ? C28 C29 C30 C31 3.9(4) . . . . ? Ti1 C29 C30 C31 -58.4(2) . . . . ? C28 C29 C30 C34 -169.4(5) . . . . ? Ti1 C29 C30 C34 128.2(5) . . . . ? C28 C29 C30 Ti2 87.7(3) . . . . ? Ti1 C29 C30 Ti2 25.4(2) . . . . ? C28 C29 C30 Ti1 62.3(2) . . . . ? C29 C30 C31 C32 -177.5(3) . . . . ? C34 C30 C31 C32 -1.7(4) . . . . ? Ti2 C30 C31 C32 59.5(2) . . . . ? Ti1 C30 C31 C32 122.0(3) . . . . ? C29 C30 C31 C27 -1.4(4) . . . . ? C34 C30 C31 C27 174.4(3) . . . . ? Ti2 C30 C31 C27 -124.4(3) . . . . ? Ti1 C30 C31 C27 -61.9(2) . . . . ? C29 C30 C31 Ti1 60.5(2) . . . . ? C34 C30 C31 Ti1 -123.7(3) . . . . ? Ti2 C30 C31 Ti1 -62.52(7) . . . . ? C29 C30 C31 Ti2 123.0(3) . . . . ? C34 C30 C31 Ti2 -61.2(2) . . . . ? Ti1 C30 C31 Ti2 62.52(7) . . . . ? C28 C27 C31 C32 172.2(5) . . . . ? Si3 C27 C31 C32 19.3(7) . . . . ? Ti1 C27 C31 C32 -118.6(5) . . . . ? C28 C27 C31 C30 -1.6(4) . . . . ? Si3 C27 C31 C30 -154.5(3) . . . . ? Ti1 C27 C31 C30 67.6(2) . . . . ? C28 C27 C31 Ti1 -69.2(2) . . . . ? Si3 C27 C31 Ti1 137.9(3) . . . . ? C28 C27 C31 Ti2 -81.4(3) . . . . ? Si3 C27 C31 Ti2 125.7(3) . . . . ? Ti1 C27 C31 Ti2 -12.2(2) . . . . ? C30 C31 C32 C33 4.3(4) . . . . ? C27 C31 C32 C33 -169.5(5) . . . . ? Ti1 C31 C32 C33 90.7(3) . . . . ? Ti2 C31 C32 C33 64.7(2) . . . . ? C30 C31 C32 Ti2 -60.4(2) . . . . ? C27 C31 C32 Ti2 125.8(5) . . . . ? Ti1 C31 C32 Ti2 26.0(2) . . . . ? C31 C32 C33 C34 -5.5(4) . . . . ? Ti2 C32 C33 C34 63.1(3) . . . . ? C31 C32 C33 Ti2 -68.6(2) . . . . ? C32 C33 C34 C30 4.3(4) . . . . ? Ti2 C33 C34 C30 68.7(2) . . . . ? C32 C33 C34 Si4 160.2(3) . . . . ? Ti2 C33 C34 Si4 -135.4(3) . . . . ? C32 C33 C34 Ti2 -64.4(3) . . . . ? C29 C30 C34 C33 171.8(5) . . . . ? C31 C30 C34 C33 -1.5(4) . . . . ? Ti2 C30 C34 C33 -66.6(2) . . . . ? Ti1 C30 C34 C33 -77.8(3) . . . . ? C29 C30 C34 Si4 19.6(7) . . . . ? C31 C30 C34 Si4 -153.7(3) . . . . ? Ti2 C30 C34 Si4 141.2(3) . . . . ? Ti1 C30 C34 Si4 130.0(3) . . . . ? C29 C30 C34 Ti2 -121.6(5) . . . . ? C31 C30 C34 Ti2 65.1(2) . . . . ? Ti1 C30 C34 Ti2 -11.2(2) . . . . ? C14 C12 Si1 C1 -48.4(5) . . . . ? C13 C12 Si1 C1 -175.1(4) . . . . ? C14 C12 Si1 C15 -171.2(4) . . . . ? C13 C12 Si1 C15 62.1(5) . . . . ? C14 C12 Si1 C9A 68.4(5) . . . . ? C13 C12 Si1 C9A -58.3(5) . . . . ? C2 C1 Si1 C12 76.1(4) . . . . ? C5 C1 Si1 C12 -135.6(3) . . . . ? Ti1 C1 Si1 C12 -23.4(4) . . . . ? C2 C1 Si1 C15 -159.9(3) . . . . ? C5 C1 Si1 C15 -11.7(4) . . . . ? Ti1 C1 Si1 C15 100.5(3) . . . . ? C2 C1 Si1 C9A -44.2(4) . . . . ? C5 C1 Si1 C9A 104.0(4) . . . . ? Ti1 C1 Si1 C9A -143.8(3) . . . . ? C16 C15 Si1 C12 -80.7(4) . . . . ? C17 C15 Si1 C12 46.3(4) . . . . ? C16 C15 Si1 C1 154.5(3) . . . . ? C17 C15 Si1 C1 -78.5(3) . . . . ? C16 C15 Si1 C9A 41.1(4) . . . . ? C17 C15 Si1 C9A 168.2(3) . . . . ? C25 C24 Si2 C8 -172.6(4) . . . . ? C26 C24 Si2 C8 55.4(5) . . . . ? C25 C24 Si2 C21 53.1(5) . . . . ? C26 C24 Si2 C21 -78.9(5) . . . . ? C25 C24 Si2 C18 -60.8(5) . . . . ? C26 C24 Si2 C18 167.3(4) . . . . ? C7 C8 Si2 C24 27.3(4) . . . . ? C4 C8 Si2 C24 173.1(4) . . . . ? Ti2 C8 Si2 C24 -70.4(4) . . . . ? C7 C8 Si2 C21 161.2(4) . . . . ? C4 C8 Si2 C21 -52.9(5) . . . . ? Ti2 C8 Si2 C21 63.6(4) . . . . ? C7 C8 Si2 C18 -87.3(3) . . . . ? C4 C8 Si2 C18 58.6(4) . . . . ? Ti2 C8 Si2 C18 175.1(3) . . . . ? C22 C21 Si2 C24 -79.4(7) . . . . ? C23 C21 Si2 C24 34.1(4) . . . . ? C22 C21 Si2 C8 149.0(6) . . . . ? C23 C21 Si2 C8 -97.5(4) . . . . ? C22 C21 Si2 C18 37.2(7) . . . . ? C23 C21 Si2 C18 150.7(4) . . . . ? C28 C27 Si3 C38 -175.9(3) . . . . ? C31 C27 Si3 C38 -26.6(4) . . . . ? Ti1 C27 Si3 C38 85.7(3) . . . . ? C28 C27 Si3 C41 -54.1(3) . . . . ? C31 C27 Si3 C41 95.3(4) . . . . ? Ti1 C27 Si3 C41 -152.4(3) . . . . ? C28 C27 Si3 C35 63.8(3) . . . . ? C31 C27 Si3 C35 -146.8(3) . . . . ? Ti1 C27 Si3 C35 -34.5(3) . . . . ? C39 C38 Si3 C27 -155.6(3) . . . . ? C40 C38 Si3 C27 77.6(3) . . . . ? C39 C38 Si3 C41 88.5(4) . . . . ? C40 C38 Si3 C41 -38.3(3) . . . . ? C39 C38 Si3 C35 -35.1(4) . . . . ? C40 C38 Si3 C35 -161.9(3) . . . . ? C33 C34 Si4 C50 33.7(4) . . . . ? C30 C34 Si4 C50 -177.7(3) . . . . ? Ti2 C34 Si4 C50 -62.1(3) . . . . ? C33 C34 Si4 C44 159.7(3) . . . . ? C30 C34 Si4 C44 -51.7(4) . . . . ? Ti2 C34 Si4 C44 63.9(4) . . . . ? C33 C34 Si4 C47 -80.6(3) . . . . ? C30 C34 Si4 C47 68.1(4) . . . . ? Ti2 C34 Si4 C47 -176.3(3) . . . . ? C51 C50 Si4 C34 67.3(5) . . . . ? C52 C50 Si4 C34 -167.0(4) . . . . ? C51 C50 Si4 C44 -61.1(5) . . . . ? C52 C50 Si4 C44 64.7(5) . . . . ? C51 C50 Si4 C47 -179.2(4) . . . . ? C52 C50 Si4 C47 -53.5(5) . . . . ? C45 C44 Si4 C34 39.1(5) . . . . ? C46 C44 Si4 C34 158.3(4) . . . . ? C45 C44 Si4 C50 162.3(4) . . . . ? C46 C44 Si4 C50 -78.5(5) . . . . ? C45 C44 Si4 C47 -79.8(5) . . . . ? C46 C44 Si4 C47 39.4(5) . . . . ? _iucr_refine_instructions_details ; TITL import in P2(1)/n CELL 0.71073 12.8940 22.3423 19.1129 90.000 92.179 90.000 ZERR 4.00 0.0026 0.0045 0.0038 0.000 0.030 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O SI TI UNIT 216 368 8 16 8 MERG 2 OMIT -1 3 4 OMIT -4 5 4 OMIT 2 0 4 OMIT 3 1 6 OMIT -3 1 4 OMIT 0 1 5 OMIT -1 5 3 OMIT -2 3 3 OMIT 4 3 0 OMIT -2 4 5 OMIT 2 4 4 shel 7 0.77 EXYZ C9A C9B EADP C9A C9B C10A C10B DELU C9A C9B C10A C10B SIMU C9A C9B C10A C10B FMAP 2 PLAN 5 SIZE 0.030 0.120 0.120 ACTA HTAB 2.00000 BOND BOND $H CONF L.S. 18 TEMP -173.00 WGHT 0.122600 10.518400 FVAR 0.17787 0.63359 C1 1 0.435882 0.150891 0.760947 11.00000 0.01912 0.01811 = 0.02247 -0.00014 0.00289 0.00031 C2 1 0.366532 0.155968 0.700626 11.00000 0.01638 0.02330 = 0.02338 -0.00405 0.00236 0.00039 AFIX 43 H2 2 0.309652 0.129802 0.691124 11.00000 -1.20000 AFIX 0 C3 1 0.392315 0.203784 0.657545 11.00000 0.01706 0.02156 = 0.02074 -0.00196 0.00124 0.00405 AFIX 43 H3 2 0.360472 0.213245 0.613284 11.00000 -1.20000 AFIX 0 C4 1 0.475841 0.236110 0.692352 11.00000 0.01903 0.01809 = 0.02373 0.00078 0.00315 0.00254 C5 1 0.503547 0.202952 0.755224 11.00000 0.01845 0.01962 = 0.02206 -0.00018 0.00175 -0.00015 C6 1 0.584750 0.235554 0.791726 11.00000 0.02194 0.02474 = 0.02248 0.00092 0.00174 -0.00256 AFIX 43 H6 2 0.622129 0.223003 0.832938 11.00000 -1.20000 AFIX 0 C7 1 0.598950 0.289583 0.755302 11.00000 0.03000 0.01991 = 0.02734 -0.00418 0.00421 -0.00358 AFIX 43 H7 2 0.643958 0.320769 0.771319 11.00000 -1.20000 AFIX 0 C8 1 0.537208 0.292008 0.690897 11.00000 0.02343 0.01863 = 0.03008 0.00030 0.00523 0.00258 PART 1 C9A 1 0.261912 0.135335 0.859624 21.00000 0.04562 0.08265 = 0.06110 0.00956 0.01854 0.00145 AFIX 13 H9A 2 0.247499 0.121422 0.908025 21.00000 -1.20000 AFIX 0 C10A 1 0.173544 0.122258 0.819486 21.00000 0.04562 0.08265 = 0.06110 0.00956 0.01854 0.00145 AFIX 33 H10A 2 0.167108 0.078784 0.814063 21.00000 -1.50000 H10B 2 0.178197 0.140880 0.773288 21.00000 -1.50000 H10C 2 0.112594 0.137825 0.842614 21.00000 -1.50000 AFIX 0 PART 2 C9B 1 0.261912 0.135335 0.859624 -21.00000 0.04562 0.08265 = 0.06110 0.00956 0.01854 0.00145 AFIX 13 H9B 2 0.255685 0.124642 0.910096 -21.00000 -1.20000 AFIX 0 C10B 1 0.178647 0.094388 0.824303 -21.00000 0.04562 0.08265 = 0.06110 0.00956 0.01854 0.00145 AFIX 33 H10D 2 0.199195 0.052434 0.830477 -21.00000 -1.50000 H10E 2 0.172124 0.103695 0.774222 -21.00000 -1.50000 H10F 2 0.111842 0.101082 0.845819 -21.00000 -1.50000 AFIX 0 PART 0 C11 1 0.258149 0.203732 0.862513 11.00000 0.06048 0.09093 = 0.06887 -0.01722 0.01617 0.03994 AFIX 33 H11A 2 0.318326 0.218639 0.890129 11.00000 -1.50000 H11B 2 0.194238 0.216451 0.884363 11.00000 -1.50000 H11C 2 0.259474 0.219917 0.814900 11.00000 -1.50000 AFIX 0 C12 1 0.406102 0.026205 0.832743 11.00000 0.05982 0.02824 = 0.03823 0.00226 -0.00034 -0.01112 AFIX 13 H12 2 0.481054 0.015865 0.828473 11.00000 -1.20000 AFIX 0 C13 1 0.368916 -0.008421 0.896044 11.00000 0.14914 0.04528 = 0.04191 0.01465 -0.01524 -0.04797 AFIX 33 H13A 2 0.405844 0.005944 0.938553 11.00000 -1.50000 H13B 2 0.382887 -0.051173 0.889867 11.00000 -1.50000 H13C 2 0.294176 -0.002233 0.900298 11.00000 -1.50000 AFIX 0 C14 1 0.350728 0.003531 0.766607 11.00000 0.13540 0.03035 = 0.03349 -0.00251 -0.00536 -0.02696 AFIX 33 H14A 2 0.375349 0.025608 0.726159 11.00000 -1.50000 H14B 2 0.275799 0.009529 0.770014 11.00000 -1.50000 H14C 2 0.365220 -0.039211 0.760871 11.00000 -1.50000 AFIX 0 C15 1 0.487790 0.136232 0.918571 11.00000 0.04481 0.02657 = 0.02635 0.00019 0.00374 -0.00686 AFIX 13 H15 2 0.498082 0.180129 0.911338 11.00000 -1.20000 AFIX 0 C16 1 0.441897 0.129620 0.990960 11.00000 0.06641 0.05114 = 0.02212 -0.00324 0.00475 -0.00576 AFIX 33 H16A 2 0.372716 0.147815 0.990435 11.00000 -1.50000 H16B 2 0.487039 0.149753 1.026017 11.00000 -1.50000 H16C 2 0.436590 0.087064 1.002721 11.00000 -1.50000 AFIX 0 C17 1 0.597000 0.107986 0.919624 11.00000 0.04169 0.04399 = 0.03242 0.00297 -0.00259 -0.00626 AFIX 33 H17A 2 0.626723 0.112593 0.873498 11.00000 -1.50000 H17B 2 0.592036 0.065343 0.931031 11.00000 -1.50000 H17C 2 0.641623 0.128076 0.955011 11.00000 -1.50000 AFIX 0 C18 1 0.380499 0.392203 0.697942 11.00000 0.06545 0.03491 = 0.05830 0.00678 0.00673 0.00786 AFIX 13 H18 2 0.359254 0.432147 0.678634 11.00000 -1.20000 AFIX 0 C19 1 0.399878 0.399160 0.774056 11.00000 0.05455 0.04382 = 0.04118 0.00304 0.01203 0.00989 AFIX 33 H19A 2 0.457402 0.427185 0.782750 11.00000 -1.50000 H19B 2 0.417816 0.360213 0.794765 11.00000 -1.50000 H19C 2 0.337293 0.414706 0.795227 11.00000 -1.50000 AFIX 0 C20 1 0.290174 0.348749 0.683613 11.00000 0.05057 0.05657 = 0.08685 0.00505 0.01149 0.00631 AFIX 33 H20A 2 0.277894 0.344337 0.632960 11.00000 -1.50000 H20B 2 0.227477 0.364460 0.704483 11.00000 -1.50000 H20C 2 0.307405 0.309669 0.704234 11.00000 -1.50000 AFIX 0 C21 1 0.465299 0.368161 0.555712 11.00000 0.09675 0.03370 = 0.07280 -0.01917 -0.04857 0.02835 AFIX 13 H21 2 0.437656 0.327731 0.542487 11.00000 -1.20000 AFIX 0 C22 1 0.394430 0.413415 0.528307 11.00000 0.12465 0.04562 = 0.04156 0.01838 -0.02066 -0.00464 AFIX 33 H22A 2 0.328465 0.410456 0.551905 11.00000 -1.50000 H22B 2 0.382230 0.407265 0.477897 11.00000 -1.50000 H22C 2 0.424614 0.453164 0.536566 11.00000 -1.50000 AFIX 0 C23 1 0.566527 0.383632 0.507081 11.00000 0.09167 0.05327 = 0.04863 0.00130 0.01418 -0.00428 AFIX 33 H23A 2 0.623649 0.356205 0.519423 11.00000 -1.50000 H23B 2 0.589011 0.424952 0.515800 11.00000 -1.50000 H23C 2 0.546427 0.378833 0.457433 11.00000 -1.50000 AFIX 0 C24 1 0.610736 0.421570 0.677059 11.00000 0.06873 0.04388 = 0.05253 0.00406 0.00249 -0.00855 AFIX 13 H24 2 0.611957 0.422311 0.729398 11.00000 -1.20000 AFIX 0 C25 1 0.584808 0.486272 0.654459 11.00000 0.09298 0.03887 = 0.06502 -0.00033 -0.00128 -0.01164 AFIX 33 H25A 2 0.514465 0.496347 0.668197 11.00000 -1.50000 H25B 2 0.588905 0.489749 0.603526 11.00000 -1.50000 H25C 2 0.634575 0.513846 0.677289 11.00000 -1.50000 AFIX 0 C26 1 0.726567 0.399198 0.657018 11.00000 0.07360 0.09080 = 0.05643 -0.01111 0.02232 -0.05518 AFIX 33 H26A 2 0.737174 0.357879 0.672941 11.00000 -1.50000 H26B 2 0.778843 0.425164 0.679941 11.00000 -1.50000 H26C 2 0.733144 0.401135 0.606155 11.00000 -1.50000 AFIX 0 C27 1 0.518387 0.133907 0.542038 11.00000 0.02265 0.02127 = 0.02167 -0.00006 0.00308 0.00208 C28 1 0.557625 0.075694 0.561250 11.00000 0.02564 0.01966 = 0.02393 -0.00181 0.00467 0.00284 AFIX 43 H28 2 0.520884 0.039425 0.552593 11.00000 -1.20000 AFIX 0 C29 1 0.656107 0.078742 0.594136 11.00000 0.02443 0.02420 = 0.02578 0.00423 0.00518 0.00772 AFIX 43 H29 2 0.694109 0.046211 0.614300 11.00000 -1.20000 AFIX 0 C53 1 0.606653 0.074220 0.730014 11.00000 0.05749 0.04987 = 0.03483 0.01532 0.01398 0.02966 C30 1 0.689421 0.140032 0.591900 11.00000 0.01680 0.02250 = 0.02256 0.00124 0.00392 0.00583 C31 1 0.604625 0.174292 0.560956 11.00000 0.01767 0.02217 = 0.01914 0.00308 0.00343 0.00311 C32 1 0.639388 0.234997 0.555871 11.00000 0.02217 0.02118 = 0.02046 0.00519 0.00346 0.00433 AFIX 43 H32 2 0.598803 0.268248 0.540295 11.00000 -1.20000 AFIX 0 C33 1 0.744475 0.236352 0.578135 11.00000 0.01961 0.02604 = 0.02451 0.00293 0.00677 0.00037 AFIX 43 H33 2 0.787347 0.270838 0.576052 11.00000 -1.20000 AFIX 0 C34 1 0.779096 0.179435 0.604345 11.00000 0.01833 0.02795 = 0.02287 0.00333 0.00337 0.00240 C35 1 0.286860 0.103640 0.505980 11.00000 0.02260 0.02784 = 0.03057 -0.00669 0.00138 -0.00091 AFIX 13 H35 2 0.252084 0.133471 0.536262 11.00000 -1.20000 AFIX 0 C36 1 0.209173 0.087887 0.446140 11.00000 0.02728 0.03513 = 0.03837 -0.00843 -0.00136 -0.00374 AFIX 33 H36A 2 0.195635 0.123418 0.417146 11.00000 -1.50000 H36B 2 0.144151 0.074069 0.465609 11.00000 -1.50000 H36C 2 0.238051 0.056100 0.417396 11.00000 -1.50000 AFIX 0 C37 1 0.306330 0.047417 0.550741 11.00000 0.02975 0.02871 = 0.03662 -0.00557 0.01064 -0.00703 AFIX 33 H37A 2 0.355736 0.056792 0.589420 11.00000 -1.50000 H37B 2 0.334928 0.015714 0.521743 11.00000 -1.50000 H37C 2 0.240755 0.033851 0.569635 11.00000 -1.50000 AFIX 0 C38 1 0.385155 0.223237 0.456988 11.00000 0.03096 0.02866 = 0.02180 0.00395 -0.00375 0.00096 AFIX 13 H38 2 0.393168 0.243597 0.503473 11.00000 -1.20000 AFIX 0 C39 1 0.276229 0.238955 0.428148 11.00000 0.03897 0.03451 = 0.04880 -0.00007 -0.00997 0.00845 AFIX 33 H39A 2 0.224423 0.221008 0.457952 11.00000 -1.50000 H39B 2 0.266836 0.223387 0.380391 11.00000 -1.50000 H39C 2 0.267657 0.282538 0.427629 11.00000 -1.50000 AFIX 0 C40 1 0.466429 0.251905 0.410040 11.00000 0.03913 0.03501 = 0.03311 0.00958 -0.00261 -0.00227 AFIX 33 H40A 2 0.536326 0.241954 0.428369 11.00000 -1.50000 H40B 2 0.457524 0.295466 0.409742 11.00000 -1.50000 H40C 2 0.457009 0.236486 0.362219 11.00000 -1.50000 AFIX 0 C41 1 0.459167 0.098770 0.394988 11.00000 0.04020 0.03285 = 0.02493 -0.00141 0.00443 0.00594 AFIX 13 H41 2 0.451522 0.055297 0.406125 11.00000 -1.20000 AFIX 0 C54 1 0.748364 0.167237 0.750463 11.00000 0.04945 0.05156 = 0.03211 0.00118 -0.00310 0.01784 C42 1 0.397418 0.108875 0.325523 11.00000 0.05525 0.04587 = 0.02509 -0.00736 0.00143 -0.00188 AFIX 33 H42A 2 0.323404 0.102333 0.332623 11.00000 -1.50000 H42B 2 0.421348 0.080745 0.290253 11.00000 -1.50000 H42C 2 0.408172 0.149982 0.309446 11.00000 -1.50000 AFIX 0 C43 1 0.575372 0.108661 0.383535 11.00000 0.04461 0.06612 = 0.03095 -0.00144 0.01150 0.01670 AFIX 33 H43A 2 0.614875 0.102182 0.427705 11.00000 -1.50000 H43B 2 0.586413 0.149706 0.367339 11.00000 -1.50000 H43C 2 0.598852 0.080396 0.348266 11.00000 -1.50000 AFIX 0 C44 1 0.963412 0.099554 0.671709 11.00000 0.02974 0.04943 = 0.06638 0.02591 -0.01029 -0.00071 AFIX 13 H44 2 0.970686 0.116285 0.720175 11.00000 -1.20000 AFIX 0 C45 1 0.888437 0.045676 0.672509 11.00000 0.04591 0.05921 = 0.05744 0.01191 -0.00311 0.00494 AFIX 33 H45A 2 0.819706 0.059288 0.685881 11.00000 -1.50000 H45B 2 0.914858 0.015919 0.706380 11.00000 -1.50000 H45C 2 0.883169 0.027633 0.625774 11.00000 -1.50000 AFIX 0 C46 1 1.069704 0.073231 0.651533 11.00000 0.02722 0.04417 = 0.11399 0.01886 -0.01438 0.00617 AFIX 33 H46A 2 1.121305 0.105393 0.650526 11.00000 -1.50000 H46B 2 1.062688 0.054586 0.605183 11.00000 -1.50000 H46C 2 1.092174 0.043106 0.686162 11.00000 -1.50000 AFIX 0 C47 1 0.958018 0.138784 0.517768 11.00000 0.03010 0.04062 = 0.05870 -0.01980 0.01683 -0.00247 AFIX 13 H47 2 1.034246 0.130374 0.519449 11.00000 -1.20000 AFIX 0 C48 1 0.903264 0.082202 0.490086 11.00000 0.04009 0.05273 = 0.08152 -0.02745 0.01005 -0.00309 AFIX 33 H48A 2 0.915102 0.049415 0.523503 11.00000 -1.50000 H48B 2 0.931068 0.071145 0.444857 11.00000 -1.50000 H48C 2 0.828605 0.089858 0.484194 11.00000 -1.50000 AFIX 0 C49 1 0.938700 0.189012 0.464974 11.00000 0.08728 0.07357 = 0.03216 -0.00454 0.02273 -0.00977 AFIX 33 H49A 2 0.973517 0.225522 0.481890 11.00000 -1.50000 H49B 2 0.863937 0.196385 0.459236 11.00000 -1.50000 H49C 2 0.966217 0.177444 0.419831 11.00000 -1.50000 AFIX 0 C50 1 0.991294 0.234330 0.630816 11.00000 0.02084 0.03632 = 0.04450 -0.00793 0.00228 -0.00094 AFIX 13 H50 2 0.962893 0.264751 0.596826 11.00000 -1.20000 AFIX 0 C51 1 0.970904 0.257984 0.703505 11.00000 0.04658 0.13418 = 0.07592 -0.06270 0.00950 -0.02813 AFIX 33 H51A 2 0.895899 0.259922 0.709781 11.00000 -1.50000 H51B 2 1.000844 0.298111 0.708896 11.00000 -1.50000 H51C 2 1.002811 0.231182 0.738744 11.00000 -1.50000 AFIX 0 C52 1 1.109048 0.231752 0.621104 11.00000 0.02594 0.04859 = 0.09849 -0.02366 0.00850 -0.00484 AFIX 33 H52A 2 1.122491 0.216923 0.574053 11.00000 -1.50000 H52B 2 1.141093 0.204762 0.656086 11.00000 -1.50000 H52C 2 1.138606 0.271929 0.626986 11.00000 -1.50000 AFIX 0 O1 3 0.648646 0.040825 0.766270 11.00000 0.06364 0.06570 = 0.04640 0.01470 0.00528 0.02319 O2 3 0.801062 0.142896 0.790375 11.00000 0.06319 0.07033 = 0.04485 0.00446 -0.00427 0.01850 SI1 4 0.400213 0.109929 0.842921 11.00000 0.02852 0.02622 = 0.02116 0.00136 0.00459 -0.00489 SI2 4 0.507736 0.367544 0.651450 11.00000 0.05236 0.01616 = 0.02717 0.00135 0.00347 -0.00072 SI3 4 0.410392 0.141032 0.473962 11.00000 0.02089 0.02237 = 0.02097 -0.00228 0.00009 0.00178 SI4 4 0.921874 0.161858 0.609781 11.00000 0.01552 0.02727 = 0.03650 0.00664 0.00293 0.00166 TI1 5 0.530766 0.133599 0.661079 11.00000 0.01764 0.01789 = 0.02006 0.00229 0.00326 0.00257 TI2 5 0.652903 0.215330 0.678039 11.00000 0.01677 0.02178 = 0.02238 0.00157 0.00211 0.00045 HKLF 4 REM import in P2(1)/n REM R1 = 0.0766 for 9225 Fo > 4sig(Fo) and 0.1018 for all 12581 data REM 557 parameters refined using 38 restraints END ; # END of CIF _database_code_depnum_ccdc_archive 'CCDC 969255'