# ja994393h.cif data_247 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H48 Ti' _chemical_formula_weight 504.62 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.866(3) _cell_length_b 15.594(3) _cell_length_c 18.197(4) _cell_angle_alpha 67.33(3) _cell_angle_beta 76.78(3) _cell_angle_gamma 73.38(3) _cell_volume 3199.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _exptl_crystal_description PRISM _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type NO _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE-IPDS _diffrn_measurement_method 'LASER SCANNED IMAGING PLATE' _diffrn_standards_number 50-200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 360 _diffrn_standards_decay_% ? _diffrn_reflns_number 6470 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 21.05 _reflns_number_total 6470 _reflns_number_observed 3733 _reflns_observed_criterion >2sigma(I) _computing_data_collection STOE-EXPOSE _computing_cell_refinement STOE-CELL _computing_data_reduction STOE-INTEGRATE _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6470 _refine_ls_number_parameters 619 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_obs 0.0525 _refine_ls_wR_factor_all 0.1332 _refine_ls_wR_factor_obs 0.1203 _refine_ls_goodness_of_fit_all 0.879 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 0.877 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C29A C 0.2446(10) -0.0874(9) -0.1588(5) 0.071(4) Uiso 0.50 d PD 1 H29A H 0.1729(10) -0.0504(9) -0.1706(5) 0.107 Uiso 0.50 calc PR 1 H29B H 0.2662(10) -0.1356(9) -0.1833(5) 0.107 Uiso 0.50 calc PR 1 H29C H 0.2958(10) -0.0466(9) -0.1797(5) 0.107 Uiso 0.50 calc PR 1 C67A C 0.2089(11) -0.0512(8) -0.0361(8) 0.069(4) Uiso 0.50 d PD 1 H67A H 0.1374(11) -0.0152(8) -0.0493(8) 0.103 Uiso 0.50 calc PR 1 H67B H 0.2605(11) -0.0109(8) -0.0604(8) 0.103 Uiso 0.50 calc PR 1 H67C H 0.2074(11) -0.0753(8) 0.0212(8) 0.103 Uiso 0.50 calc PR 1 C68A C 0.1604(10) -0.1987(10) -0.0278(8) 0.080(5) Uiso 0.50 d PD 1 H68A H 0.0885(10) -0.1622(10) -0.0399(8) 0.119 Uiso 0.50 calc PR 1 H68B H 0.1606(10) -0.2235(10) 0.0293(8) 0.119 Uiso 0.50 calc PR 1 H68C H 0.1802(10) -0.2506(10) -0.0480(8) 0.119 Uiso 0.50 calc PR 1 C29B C 0.2328(10) -0.1361(11) -0.1495(6) 0.078(4) Uiso 0.50 d PD 2 H29D H 0.1622(10) -0.0995(11) -0.1645(6) 0.117 Uiso 0.50 calc PR 2 H29E H 0.2409(10) -0.2006(11) -0.1460(6) 0.117 Uiso 0.50 calc PR 2 H29F H 0.2889(10) -0.1090(11) -0.1892(6) 0.117 Uiso 0.50 calc PR 2 C67B C 0.2359(15) -0.0345(9) -0.0681(12) 0.125(8) Uiso 0.50 d PD 2 H67D H 0.1652(15) 0.0048(9) -0.0804(12) 0.187 Uiso 0.50 calc PR 2 H67E H 0.2916(15) -0.0072(9) -0.1080(12) 0.187 Uiso 0.50 calc PR 2 H67F H 0.2463(15) -0.0385(9) -0.0162(12) 0.187 Uiso 0.50 calc PR 2 C68B C 0.1503(9) -0.1757(10) -0.0063(7) 0.065(4) Uiso 0.50 d PD 2 H68D H 0.0810(9) -0.1358(10) -0.0216(7) 0.098 Uiso 0.50 calc PR 2 H68E H 0.1569(9) -0.1782(10) 0.0460(7) 0.098 Uiso 0.50 calc PR 2 H68F H 0.1548(9) -0.2388(10) -0.0050(7) 0.098 Uiso 0.50 calc PR 2 C45A C 0.7569(12) -0.5905(8) 0.2340(10) 0.083(5) Uiso 0.50 d PD 1 H45A H 0.7780(12) -0.6330(8) 0.2854(10) 0.125 Uiso 0.50 calc PR 1 H45B H 0.8212(12) -0.5806(8) 0.1957(10) 0.125 Uiso 0.50 calc PR 1 H45C H 0.7134(12) -0.6179(8) 0.2164(10) 0.125 Uiso 0.50 calc PR 1 C65A C 0.5901(9) -0.5273(10) 0.2998(7) 0.090(4) Uiso 0.50 d PD 1 H65A H 0.6122(9) -0.5668(10) 0.3515(7) 0.135 Uiso 0.50 calc PR 1 H65B H 0.5610(9) -0.5629(10) 0.2796(7) 0.135 Uiso 0.50 calc PR 1 H65C H 0.5351(9) -0.4726(10) 0.3047(7) 0.135 Uiso 0.50 calc PR 1 C66A C 0.7547(13) -0.4454(12) 0.2680(10) 0.110(6) Uiso 0.50 d PD 1 H66A H 0.7742(13) -0.4846(12) 0.3206(10) 0.165 Uiso 0.50 calc PR 1 H66B H 0.7106(13) -0.3849(12) 0.2696(10) 0.165 Uiso 0.50 calc PR 1 H66C H 0.8199(13) -0.4361(12) 0.2306(10) 0.165 Uiso 0.50 calc PR 1 C45B C 0.7137(22) -0.5986(10) 0.2521(18) 0.224(16) Uiso 0.50 d PD 2 H45D H 0.7323(22) -0.6362(10) 0.3051(18) 0.336 Uiso 0.50 calc PR 2 H45E H 0.7738(22) -0.6122(10) 0.2129(18) 0.336 Uiso 0.50 calc PR 2 H45F H 0.6502(22) -0.6137(10) 0.2450(18) 0.336 Uiso 0.50 calc PR 2 C65B C 0.5973(9) -0.4727(11) 0.3036(7) 0.095(5) Uiso 0.50 d PD 2 H65D H 0.6159(9) -0.5123(11) 0.3563(7) 0.143 Uiso 0.50 calc PR 2 H65E H 0.5321(9) -0.4849(11) 0.2961(7) 0.143 Uiso 0.50 calc PR 2 H65F H 0.5850(9) -0.4069(11) 0.2980(7) 0.143 Uiso 0.50 calc PR 2 C66B C 0.7928(10) -0.4763(12) 0.2520(10) 0.098(6) Uiso 0.50 d PD 2 H66D H 0.8121(10) -0.5160(12) 0.3045(10) 0.147 Uiso 0.50 calc PR 2 H66E H 0.7813(10) -0.4105(12) 0.2464(10) 0.147 Uiso 0.50 calc PR 2 H66F H 0.8511(10) -0.4905(12) 0.2120(10) 0.147 Uiso 0.50 calc PR 2 C21A C 0.5196(13) -0.0860(9) 0.3857(11) 0.122(6) Uiso 0.50 d PD 1 H21A H 0.5874(13) -0.0869(9) 0.4000(11) 0.182 Uiso 0.50 calc PR 1 H21B H 0.4598(13) -0.0531(9) 0.4142(11) 0.182 Uiso 0.50 calc PR 1 H21C H 0.5191(13) -0.0539(9) 0.3289(11) 0.182 Uiso 0.50 calc PR 1 C62A C 0.6003(13) -0.2540(15) 0.3727(13) 0.165(8) Uiso 0.50 d PD 1 H62A H 0.6686(13) -0.2563(15) 0.3871(13) 0.248 Uiso 0.50 calc PR 1 H62B H 0.6039(13) -0.2301(15) 0.3153(13) 0.248 Uiso 0.50 calc PR 1 H62C H 0.5863(13) -0.3169(15) 0.3936(13) 0.248 Uiso 0.50 calc PR 1 C63A C 0.5010(13) -0.2356(12) 0.4995(7) 0.118(5) Uiso 0.50 d PD 1 H63A H 0.5679(13) -0.2388(12) 0.5163(7) 0.178 Uiso 0.50 calc PR 1 H63B H 0.4897(13) -0.2988(12) 0.5149(7) 0.178 Uiso 0.50 calc PR 1 H63C H 0.4409(13) -0.1988(12) 0.5246(7) 0.178 Uiso 0.50 calc PR 1 C21B C 0.4946(14) -0.1074(11) 0.4409(11) 0.130(6) Uiso 0.50 d PD 2 H21D H 0.5632(14) -0.1102(11) 0.4551(11) 0.196 Uiso 0.50 calc PR 2 H21E H 0.4403(14) -0.1147(11) 0.4875(11) 0.196 Uiso 0.50 calc PR 2 H21F H 0.4721(14) -0.0471(11) 0.4003(11) 0.196 Uiso 0.50 calc PR 2 C62B C 0.5920(10) -0.1699(12) 0.3313(7) 0.109(5) Uiso 0.50 d PD 2 H62D H 0.6608(10) -0.1716(12) 0.3445(7) 0.163 Uiso 0.50 calc PR 2 H62E H 0.5659(10) -0.1086(12) 0.2932(7) 0.163 Uiso 0.50 calc PR 2 H62F H 0.6015(10) -0.2183(12) 0.3085(7) 0.163 Uiso 0.50 calc PR 2 C63B C 0.5564(15) -0.2905(9) 0.4611(11) 0.154(7) Uiso 0.50 d PD 2 H63D H 0.6244(15) -0.2922(9) 0.4755(11) 0.232 Uiso 0.50 calc PR 2 H63E H 0.5690(15) -0.3330(9) 0.4318(11) 0.232 Uiso 0.50 calc PR 2 H63F H 0.5059(15) -0.3100(9) 0.5089(11) 0.232 Uiso 0.50 calc PR 2 C16A C -0.1855(12) -0.0285(11) 0.5088(6) 0.102(5) Uiso 0.50 d PD 1 H16A H -0.2519(12) 0.0088(11) 0.5276(6) 0.153 Uiso 0.50 calc PR 1 H16B H -0.1287(12) -0.0374(11) 0.5390(6) 0.153 Uiso 0.50 calc PR 1 H16C H -0.1972(12) -0.0893(11) 0.5156(6) 0.153 Uiso 0.50 calc PR 1 C58A C -0.1281(12) 0.1169(9) 0.4135(10) 0.113(6) Uiso 0.50 d PD 1 H58A H -0.1946(12) 0.1566(9) 0.4294(10) 0.169 Uiso 0.50 calc PR 1 H58B H -0.1000(12) 0.1490(9) 0.3590(10) 0.169 Uiso 0.50 calc PR 1 H58C H -0.0751(12) 0.1037(9) 0.4481(10) 0.169 Uiso 0.50 calc PR 1 C59A C -0.2410(11) 0.0461(12) 0.3683(9) 0.108(6) Uiso 0.50 d PD 1 H59A H -0.3054(11) 0.0860(12) 0.3865(9) 0.163 Uiso 0.50 calc PR 1 H59B H -0.2578(11) -0.0120(12) 0.3729(9) 0.163 Uiso 0.50 calc PR 1 H59C H -0.2159(11) 0.0787(12) 0.3132(9) 0.163 Uiso 0.50 calc PR 1 C16B C -0.1606(11) 0.0143(10) 0.5082(5) 0.079(4) Uiso 0.50 d PD 2 H16D H -0.2276(11) 0.0549(10) 0.5223(5) 0.119 Uiso 0.50 calc PR 2 H16E H -0.0997(11) 0.0330(10) 0.5154(5) 0.119 Uiso 0.50 calc PR 2 H16F H -0.1601(11) -0.0506(10) 0.5421(5) 0.119 Uiso 0.50 calc PR 2 C58B C -0.1539(11) 0.1290(7) 0.3696(8) 0.091(4) Uiso 0.50 d PD 2 H58D H -0.2208(11) 0.1678(7) 0.3863(8) 0.136 Uiso 0.50 calc PR 2 H58E H -0.1499(11) 0.1385(7) 0.3138(8) 0.136 Uiso 0.50 calc PR 2 H58F H -0.0927(11) 0.1466(7) 0.3775(8) 0.136 Uiso 0.50 calc PR 2 C59B C -0.2491(8) -0.0027(10) 0.4040(8) 0.075(4) Uiso 0.50 d PD 2 H59D H -0.3161(8) 0.0367(10) 0.4197(8) 0.112 Uiso 0.50 calc PR 2 H59E H -0.2492(8) -0.0684(10) 0.4346(8) 0.112 Uiso 0.50 calc PR 2 H59F H -0.2427(8) 0.0075(10) 0.3478(8) 0.112 Uiso 0.50 calc PR 2 C1 C 0.2375(4) -0.2960(4) 0.1950(3) 0.0523(14) Uani 1 d . . C2 C 0.1291(5) -0.3046(4) 0.2018(3) 0.0501(14) Uani 1 d . . C3 C 0.0592(4) -0.2173(4) 0.2051(3) 0.0467(13) Uani 1 d . . C4 C 0.1232(5) -0.1541(4) 0.1949(3) 0.0481(14) Uani 1 d . . C5 C 0.0823(5) -0.0495(4) 0.1816(3) 0.075(2) Uani 1 d . . H5A H 0.1426(5) -0.0220(4) 0.1763(3) 0.112 Uiso 1 calc R . H5B H 0.0299(5) -0.0410(4) 0.2266(3) 0.112 Uiso 1 calc R . H5C H 0.0482(5) -0.0188(4) 0.1335(3) 0.112 Uiso 1 calc R . C6 C 0.0580(5) -0.4080(4) 0.3971(3) 0.058(2) Uani 1 d . . C7 C 0.1714(5) -0.4477(4) 0.3931(3) 0.060(2) Uani 1 d . . C8 C 0.2339(5) -0.5277(4) 0.3628(4) 0.086(2) Uani 1 d . . H8A H 0.3102(5) -0.5395(4) 0.3668(4) 0.129 Uiso 1 calc R . H8B H 0.2246(5) -0.5103(4) 0.3076(4) 0.129 Uiso 1 calc R . H8C H 0.2068(5) -0.5841(4) 0.3945(4) 0.129 Uiso 1 calc R . C9 C 0.0316(5) -0.3470(4) 0.4428(3) 0.057(2) Uani 1 d . . C10 C 0.1271(5) -0.3526(4) 0.4699(3) 0.0564(15) Uani 1 d . . C11 C 0.1352(5) -0.3062(4) 0.5266(3) 0.083(2) Uani 1 d . . H11A H 0.0644(5) -0.2698(4) 0.5401(3) 0.124 Uiso 1 calc R . H11B H 0.1855(5) -0.2648(4) 0.5013(3) 0.124 Uiso 1 calc R . H11C H 0.1609(5) -0.3545(4) 0.5747(3) 0.124 Uiso 1 calc R . C12 C 0.1175(5) -0.1601(4) 0.3546(3) 0.0478(14) Uani 1 d . . C13 C 0.0312(5) -0.0907(4) 0.3767(3) 0.0488(14) Uani 1 d . . C14 C -0.0492(5) -0.0384(4) 0.3953(3) 0.0550(15) Uani 1 d . . C15 C -0.1514(4) 0.0234(4) 0.4198(3) 0.064(2) Uani 1 d D . C17 C 0.2230(5) -0.1951(4) 0.3513(3) 0.0473(14) Uani 1 d . . C18 C 0.3178(5) -0.1848(4) 0.3700(3) 0.0524(14) Uani 1 d . . C19 C 0.4022(5) -0.1851(4) 0.3853(4) 0.074(2) Uani 1 d . . C20 C 0.5080(6) -0.1883(5) 0.4082(4) 0.102(2) Uani 1 d D . C22 C 0.2139(5) -0.4110(4) 0.4376(3) 0.0571(15) Uani 1 d . . C23 C 0.3312(5) -0.4379(4) 0.4526(4) 0.093(2) Uani 1 d . . H23A H 0.3741(5) -0.4786(4) 0.4231(4) 0.140 Uiso 1 calc R . H23B H 0.3351(5) -0.4709(4) 0.5090(4) 0.140 Uiso 1 calc R . H23C H 0.3591(5) -0.3813(4) 0.4353(4) 0.140 Uiso 1 calc R . C24 C 0.6297(4) -0.3300(4) 0.0114(3) 0.0460(13) Uani 1 d . . C25 C 0.5573(4) -0.2763(4) -0.0364(3) 0.0437(13) Uani 1 d . . C26 C 0.4451(5) -0.2351(4) -0.0379(3) 0.0474(14) Uani 1 d . . C27 C 0.3531(5) -0.1922(4) -0.0482(3) 0.0552(15) Uani 1 d . . C28 C 0.2431(4) -0.1347(4) -0.0676(3) 0.063(2) Uani 1 d D . C30 C 0.8303(5) -0.4133(4) -0.1320(4) 0.0550(15) Uani 1 d . . C31 C 0.7296(6) -0.4382(4) -0.0949(3) 0.063(2) Uani 1 d . . C32 C 0.7114(7) -0.5202(4) -0.0172(4) 0.120(3) Uani 1 d . . H32A H 0.7777(7) -0.5476(4) 0.0069(4) 0.180 Uiso 1 calc R . H32B H 0.6910(7) -0.5679(4) -0.0287(4) 0.180 Uiso 1 calc R . H32C H 0.6540(7) -0.4970(4) 0.0191(4) 0.180 Uiso 1 calc R . C33 C 0.7669(5) -0.1319(4) -0.1836(3) 0.0540(15) Uani 1 d . . C34 C 0.8479(4) -0.1895(4) -0.1327(4) 0.0535(14) Uani 1 d . . C35 C 0.7989(5) -0.1992(4) -0.0529(3) 0.0543(15) Uani 1 d . . C36 C 0.6904(5) -0.1457(4) -0.0550(4) 0.059(2) Uani 1 d . . C37 C 0.6696(5) -0.1079(4) -0.1351(4) 0.060(2) Uani 1 d . . C38 C 0.5631(5) -0.0453(4) -0.1646(4) 0.095(2) Uani 1 d . . H38A H 0.5699(5) -0.0289(4) -0.2218(4) 0.142 Uiso 1 calc R . H38B H 0.5464(5) 0.0117(4) -0.1517(4) 0.142 Uiso 1 calc R . H38C H 0.5053(5) -0.0790(4) -0.1392(4) 0.142 Uiso 1 calc R . C39 C 0.7026(5) -0.3229(4) -0.2153(3) 0.058(2) Uani 1 d . . C40 C 0.8148(5) -0.3443(4) -0.2079(3) 0.0554(15) Uani 1 d . . C41 C 0.9047(5) -0.3152(5) -0.2757(4) 0.094(2) Uani 1 d . . H41A H 0.8730(5) -0.2669(5) -0.3214(4) 0.141 Uiso 1 calc R . H41B H 0.9464(5) -0.3696(5) -0.2900(4) 0.141 Uiso 1 calc R . H41C H 0.9519(5) -0.2906(5) -0.2588(4) 0.141 Uiso 1 calc R . C42 C 0.6408(4) -0.3843(4) 0.0938(3) 0.0534(14) Uani 1 d . . C43 C 0.6605(4) -0.4332(4) 0.1607(4) 0.064(2) Uani 1 d . . C44 C 0.6897(4) -0.4947(5) 0.2414(3) 0.080(2) Uani 1 d D . C46 C 0.3410(5) -0.3671(4) 0.1807(3) 0.089(2) Uani 1 d . . H46A H 0.3229(5) -0.4256(4) 0.1877(3) 0.134 Uiso 1 calc R . H46B H 0.3893(5) -0.3790(4) 0.2184(3) 0.134 Uiso 1 calc R . H46C H 0.3765(5) -0.3418(4) 0.1270(3) 0.134 Uiso 1 calc R . C47 C 0.2339(4) -0.2022(4) 0.1895(3) 0.0502(14) Uani 1 d . . C48 C 0.3318(5) -0.1594(5) 0.1717(3) 0.082(2) Uani 1 d . . H48A H 0.3975(5) -0.2078(5) 0.1716(3) 0.123 Uiso 1 calc R . H48B H 0.3289(5) -0.1331(5) 0.2121(3) 0.123 Uiso 1 calc R . H48C H 0.3313(5) -0.1098(5) 0.1200(3) 0.123 Uiso 1 calc R . C49 C 0.9382(5) -0.4598(5) -0.0987(4) 0.103(2) Uani 1 d . . H49A H 0.9260(5) -0.5042(5) -0.0453(4) 0.154 Uiso 1 calc R . H49B H 0.9698(5) -0.4118(5) -0.0971(4) 0.154 Uiso 1 calc R . H49C H 0.9871(5) -0.4928(5) -0.1324(4) 0.154 Uiso 1 calc R . C50 C 0.0955(5) -0.3817(4) 0.1879(3) 0.086(2) Uani 1 d . . H50A H 0.0172(5) -0.3713(4) 0.1965(3) 0.129 Uiso 1 calc R . H50B H 0.1260(5) -0.4427(4) 0.2247(3) 0.129 Uiso 1 calc R . H50C H 0.1222(5) -0.3801(4) 0.1337(3) 0.129 Uiso 1 calc R . C51 C 0.7852(5) -0.0864(4) -0.2740(3) 0.088(2) Uani 1 d . . H51A H 0.7164(5) -0.0515(4) -0.2932(3) 0.131 Uiso 1 calc R . H51B H 0.8175(5) -0.1350(4) -0.2976(3) 0.131 Uiso 1 calc R . H51C H 0.8334(5) -0.0437(4) -0.2886(3) 0.131 Uiso 1 calc R . C52 C 0.6513(4) -0.3816(5) -0.1462(4) 0.065(2) Uani 1 d . . C53 C 0.5335(5) -0.3920(6) -0.1340(5) 0.126(3) Uani 1 d . . H53A H 0.5175(5) -0.4366(6) -0.0813(5) 0.189 Uiso 1 calc R . H53B H 0.5246(5) -0.4148(6) -0.1738(5) 0.189 Uiso 1 calc R . H53C H 0.4844(5) -0.3313(6) -0.1391(5) 0.189 Uiso 1 calc R . C54 C -0.0281(5) -0.4405(5) 0.3750(4) 0.091(2) Uani 1 d . . H54A H -0.0989(5) -0.4010(5) 0.3837(4) 0.136 Uiso 1 calc R . H54B H -0.0284(5) -0.5056(5) 0.4080(4) 0.136 Uiso 1 calc R . H54C H -0.0112(5) -0.4354(5) 0.3195(4) 0.136 Uiso 1 calc R . C55 C 0.9692(4) -0.2152(5) -0.1581(4) 0.086(2) Uani 1 d . . H55A H 1.0051(4) -0.2547(5) -0.1116(4) 0.128 Uiso 1 calc R . H55B H 0.9969(4) -0.1582(5) -0.1841(4) 0.128 Uiso 1 calc R . H55C H 0.9830(4) -0.2493(5) -0.1947(4) 0.128 Uiso 1 calc R . C56 C 0.6118(5) -0.1285(5) 0.0162(4) 0.095(2) Uani 1 d . . H56A H 0.6460(5) -0.1626(5) 0.0641(4) 0.142 Uiso 1 calc R . H56B H 0.5470(5) -0.1503(5) 0.0216(4) 0.142 Uiso 1 calc R . H56C H 0.5927(5) -0.0616(5) 0.0080(4) 0.142 Uiso 1 calc R . C57 C -0.0814(5) -0.2937(5) 0.4645(4) 0.096(2) Uani 1 d . . H57A H -0.1323(5) -0.3013(5) 0.4375(4) 0.144 Uiso 1 calc R . H57B H -0.0818(5) -0.2273(5) 0.4483(4) 0.144 Uiso 1 calc R . H57C H -0.1023(5) -0.3184(5) 0.5215(4) 0.144 Uiso 1 calc R . C60 C 0.6493(6) -0.2564(5) -0.2893(4) 0.120(3) Uani 1 d . . H60A H 0.7018(6) -0.2237(5) -0.3287(4) 0.179 Uiso 1 calc R . H60B H 0.5885(6) -0.2107(5) -0.2748(4) 0.179 Uiso 1 calc R . H60C H 0.6241(6) -0.2925(5) -0.3112(4) 0.179 Uiso 1 calc R . C61 C -0.0643(4) -0.1917(5) 0.2096(4) 0.085(2) Uani 1 d . . H61A H -0.0900(4) -0.2468(5) 0.2168(4) 0.127 Uiso 1 calc R . H61B H -0.0851(4) -0.1421(5) 0.1607(4) 0.127 Uiso 1 calc R . H61C H -0.0961(4) -0.1699(5) 0.2542(4) 0.127 Uiso 1 calc R . C64 C 0.8565(5) -0.2510(5) 0.0210(4) 0.093(2) Uani 1 d . . H64A H 0.9300(5) -0.2817(5) 0.0061(4) 0.140 Uiso 1 calc R . H64B H 0.8180(5) -0.2980(5) 0.0590(4) 0.140 Uiso 1 calc R . H64C H 0.8580(5) -0.2063(5) 0.0449(4) 0.140 Uiso 1 calc R . Ti1 Ti 0.14935(7) -0.28007(6) 0.32175(5) 0.0427(3) Uani 1 d . . Ti2 Ti 0.71127(7) -0.27752(6) -0.10421(5) 0.0422(3) 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 0.062(4) 0.047(4) 0.042(3) -0.018(3) -0.003(3) -0.001(3) C2 0.076(4) 0.036(4) 0.045(3) -0.016(3) -0.007(3) -0.020(3) C3 0.051(4) 0.050(4) 0.041(3) -0.015(3) -0.012(3) -0.009(3) C4 0.068(4) 0.036(4) 0.041(3) -0.013(3) -0.012(3) -0.009(3) C5 0.118(5) 0.045(4) 0.053(4) -0.011(3) -0.024(3) -0.004(3) C6 0.077(5) 0.051(4) 0.049(4) -0.005(3) -0.008(3) -0.035(3) C7 0.083(5) 0.034(4) 0.056(4) -0.004(3) -0.015(3) -0.015(3) C8 0.127(6) 0.035(4) 0.079(5) -0.009(3) -0.012(4) -0.009(4) C9 0.064(4) 0.050(4) 0.046(4) -0.004(3) 0.004(3) -0.022(3) C10 0.085(5) 0.047(4) 0.037(3) -0.006(3) -0.006(3) -0.028(3) C11 0.125(6) 0.081(5) 0.043(4) -0.014(3) -0.010(4) -0.034(4) C12 0.059(4) 0.047(4) 0.042(3) -0.017(3) -0.007(3) -0.016(3) C13 0.061(4) 0.053(4) 0.042(3) -0.022(3) -0.005(3) -0.021(3) C14 0.060(4) 0.066(4) 0.045(3) -0.031(3) -0.001(3) -0.012(3) C15 0.066(4) 0.078(5) 0.054(4) -0.029(3) -0.004(3) -0.019(3) C17 0.056(4) 0.045(4) 0.041(3) -0.010(3) -0.009(3) -0.015(3) C18 0.066(4) 0.042(4) 0.053(4) -0.015(3) -0.016(3) -0.014(3) C19 0.061(4) 0.076(5) 0.097(5) -0.029(4) -0.032(4) -0.017(3) C20 0.090(5) 0.085(6) 0.129(6) -0.027(5) -0.038(5) -0.013(4) C22 0.068(4) 0.045(4) 0.048(4) 0.000(3) -0.015(3) -0.013(3) C23 0.093(5) 0.074(5) 0.096(5) -0.001(4) -0.043(4) -0.010(4) C24 0.053(3) 0.040(4) 0.047(4) -0.016(3) -0.003(3) -0.015(3) C25 0.047(4) 0.039(3) 0.050(3) -0.017(3) -0.013(3) -0.009(3) C26 0.051(4) 0.048(4) 0.042(3) -0.012(3) -0.008(3) -0.013(3) C27 0.054(4) 0.055(4) 0.055(4) -0.016(3) -0.012(3) -0.010(3) C28 0.059(4) 0.068(4) 0.058(4) -0.012(3) -0.023(3) -0.009(3) C30 0.060(4) 0.047(4) 0.066(4) -0.032(3) -0.011(3) -0.005(3) C31 0.093(5) 0.041(4) 0.054(4) -0.023(3) 0.006(4) -0.017(3) C32 0.216(8) 0.040(4) 0.090(5) -0.026(4) 0.037(5) -0.047(5) C33 0.069(4) 0.042(4) 0.057(4) -0.015(3) -0.006(4) -0.027(3) C34 0.049(4) 0.054(4) 0.072(4) -0.031(3) 0.001(3) -0.025(3) C35 0.065(4) 0.057(4) 0.057(4) -0.025(3) -0.009(3) -0.027(3) C36 0.061(4) 0.053(4) 0.073(5) -0.037(3) 0.007(3) -0.020(3) C37 0.059(4) 0.042(4) 0.081(5) -0.019(3) -0.012(4) -0.017(3) C38 0.076(5) 0.045(4) 0.150(7) -0.015(4) -0.033(4) -0.005(3) C39 0.074(5) 0.057(4) 0.052(4) -0.028(3) -0.013(3) -0.015(3) C40 0.060(4) 0.060(4) 0.054(4) -0.030(3) 0.007(3) -0.023(3) C41 0.113(5) 0.106(6) 0.083(5) -0.058(4) 0.035(4) -0.054(4) C42 0.040(3) 0.061(4) 0.056(4) -0.022(3) -0.005(3) -0.006(3) C43 0.060(4) 0.075(5) 0.046(4) -0.009(3) -0.012(3) -0.009(3) C44 0.061(4) 0.112(6) 0.056(4) -0.013(4) -0.013(3) -0.019(4) C46 0.088(5) 0.082(5) 0.067(4) -0.026(4) 0.003(4) 0.018(4) C47 0.059(4) 0.057(4) 0.037(3) -0.014(3) -0.002(3) -0.023(3) C48 0.080(4) 0.106(6) 0.066(4) -0.019(4) 0.003(3) -0.055(4) C49 0.099(5) 0.085(5) 0.143(7) -0.060(5) -0.060(5) 0.016(4) C50 0.135(6) 0.077(5) 0.069(4) -0.034(4) -0.011(4) -0.047(4) C51 0.136(6) 0.064(5) 0.065(4) -0.002(3) -0.014(4) -0.052(4) C52 0.053(4) 0.072(5) 0.095(5) -0.057(4) 0.005(4) -0.024(4) C53 0.066(5) 0.159(8) 0.223(9) -0.145(7) 0.021(5) -0.049(5) C54 0.117(5) 0.081(5) 0.085(5) -0.003(4) -0.020(4) -0.067(4) C55 0.063(4) 0.099(6) 0.120(6) -0.059(4) 0.004(4) -0.040(4) C56 0.104(5) 0.090(6) 0.115(6) -0.073(5) 0.018(4) -0.032(4) C57 0.079(5) 0.092(5) 0.092(5) -0.019(4) 0.026(4) -0.030(4) C60 0.182(8) 0.097(6) 0.101(6) -0.046(5) -0.084(6) 0.007(5) C61 0.070(5) 0.099(5) 0.079(5) -0.019(4) -0.025(3) -0.015(4) C64 0.103(5) 0.120(6) 0.082(5) -0.035(4) -0.031(4) -0.048(4) Ti1 0.0531(6) 0.0360(6) 0.0392(6) -0.0101(4) -0.0074(5) -0.0135(4) Ti2 0.0457(6) 0.0397(6) 0.0444(6) -0.0159(5) -0.0041(5) -0.0136(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C29A C28 1.533(7) . ? C67A C28 1.533(7) . ? C68A C28 1.533(7) . ? C29B C28 1.535(8) . ? C67B C28 1.535(8) . ? C68B C28 1.535(8) . ? C45A C44 1.537(8) . ? C65A C44 1.537(8) . ? C66A C44 1.537(8) . ? C45B C44 1.503(10) . ? C65B C44 1.503(10) . ? C66B C44 1.503(10) . ? C21A C20 1.529(9) . ? C62A C20 1.529(9) . ? C63A C20 1.529(9) . ? C21B C20 1.543(9) . ? C62B C20 1.543(9) . ? C63B C20 1.543(9) . ? C16A C15 1.528(9) . ? C58A C15 1.528(9) . ? C59A C15 1.528(9) . ? C16B C15 1.540(7) . ? C58B C15 1.540(7) . ? C59B C15 1.540(7) . ? C1 C47 1.415(7) . ? C1 C2 1.413(7) . ? C1 C46 1.513(7) . ? C1 Ti1 2.398(5) . ? C2 C3 1.416(7) . ? C2 C50 1.508(7) . ? C2 Ti1 2.438(5) . ? C3 C4 1.392(7) . ? C3 C61 1.514(7) . ? C3 Ti1 2.384(5) . ? C4 C47 1.408(7) . ? C4 C5 1.502(7) . ? C4 Ti1 2.405(5) . ? C6 C7 1.409(7) . ? C6 C9 1.418(7) . ? C6 C54 1.525(7) . ? C6 Ti1 2.396(5) . ? C7 C22 1.421(7) . ? C7 C8 1.503(7) . ? C7 Ti1 2.394(5) . ? C9 C10 1.394(7) . ? C9 C57 1.503(7) . ? C9 Ti1 2.417(5) . ? C10 C22 1.398(7) . ? C10 C11 1.506(7) . ? C10 Ti1 2.472(5) . ? C12 C17 1.306(6) . ? C12 C13 1.417(8) . ? C12 Ti1 2.082(5) . ? C13 C14 1.192(7) . ? C14 C15 1.481(8) . ? C17 C18 1.405(7) . ? C17 Ti1 2.107(5) . ? C18 C19 1.179(7) . ? C19 C20 1.496(8) . ? C22 C23 1.506(7) . ? C22 Ti1 2.411(5) . ? C24 C25 1.298(6) . ? C24 C42 1.428(7) . ? C24 Ti2 2.085(5) . ? C25 C26 1.404(7) . ? C25 Ti2 2.080(5) . ? C26 C27 1.198(6) . ? C27 C28 1.480(7) . ? C30 C40 1.401(7) . ? C30 C31 1.404(7) . ? C30 C49 1.513(7) . ? C30 Ti2 2.387(5) . ? C31 C52 1.398(7) . ? C31 C32 1.521(8) . ? C31 Ti2 2.391(5) . ? C33 C34 1.419(7) . ? C33 C37 1.403(7) . ? C33 C51 1.511(7) . ? C33 Ti2 2.385(5) . ? C34 C35 1.413(7) . ? C34 C55 1.505(7) . ? C34 Ti2 2.379(5) . ? C35 C36 1.407(7) . ? C35 C64 1.512(7) . ? C35 Ti2 2.405(5) . ? C36 C37 1.403(7) . ? C36 C56 1.511(7) . ? C36 Ti2 2.468(5) . ? C37 C38 1.512(7) . ? C37 Ti2 2.405(6) . ? C39 C52 1.390(7) . ? C39 C40 1.411(7) . ? C39 C60 1.516(7) . ? C39 Ti2 2.419(5) . ? C40 C41 1.511(7) . ? C40 Ti2 2.447(5) . ? C42 C43 1.200(7) . ? C43 C44 1.476(8) . ? C47 C48 1.505(7) . ? C47 Ti1 2.398(5) . ? C52 C53 1.527(7) . ? C52 Ti2 2.399(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C47 C1 C2 108.1(4) . . ? C47 C1 C46 124.6(6) . . ? C2 C1 C46 126.4(6) . . ? C47 C1 Ti1 72.8(3) . . ? C2 C1 Ti1 74.6(3) . . ? C46 C1 Ti1 126.8(4) . . ? C1 C2 C3 107.1(5) . . ? C1 C2 C50 126.0(5) . . ? C3 C2 C50 125.4(5) . . ? C1 C2 Ti1 71.5(3) . . ? C3 C2 Ti1 70.9(3) . . ? C50 C2 Ti1 133.7(3) . . ? C4 C3 C2 108.8(4) . . ? C4 C3 C61 124.6(5) . . ? C2 C3 C61 126.3(5) . . ? C4 C3 Ti1 73.9(3) . . ? C2 C3 Ti1 75.0(3) . . ? C61 C3 Ti1 122.4(3) . . ? C3 C4 C47 108.2(5) . . ? C3 C4 C5 125.8(5) . . ? C47 C4 C5 125.6(5) . . ? C3 C4 Ti1 72.3(3) . . ? C47 C4 Ti1 72.7(3) . . ? C5 C4 Ti1 126.5(3) . . ? C7 C6 C9 108.3(5) . . ? C7 C6 C54 127.0(6) . . ? C9 C6 C54 123.1(6) . . ? C7 C6 Ti1 72.8(3) . . ? C9 C6 Ti1 73.7(3) . . ? C54 C6 Ti1 130.4(4) . . ? C6 C7 C22 106.8(5) . . ? C6 C7 C8 127.6(6) . . ? C22 C7 C8 124.6(6) . . ? C6 C7 Ti1 73.0(3) . . ? C22 C7 Ti1 73.5(3) . . ? C8 C7 Ti1 127.8(4) . . ? C10 C9 C6 107.7(5) . . ? C10 C9 C57 126.4(6) . . ? C6 C9 C57 125.6(6) . . ? C10 C9 Ti1 75.6(3) . . ? C6 C9 Ti1 72.0(3) . . ? C57 C9 Ti1 122.6(4) . . ? C22 C10 C9 108.6(5) . . ? C22 C10 C11 125.5(6) . . ? C9 C10 C11 125.9(6) . . ? C22 C10 Ti1 71.0(3) . . ? C9 C10 Ti1 71.3(3) . . ? C11 C10 Ti1 125.1(4) . . ? C17 C12 C13 144.0(5) . . ? C17 C12 Ti1 72.9(3) . . ? C13 C12 Ti1 142.7(4) . . ? C14 C13 C12 172.5(6) . . ? C13 C14 C15 177.7(6) . . ? C14 C15 C59A 112.5(7) . . ? C14 C15 C58A 109.8(7) . . ? C59A C15 C58A 108.7(9) . . ? C14 C15 C16A 106.3(7) . . ? C59A C15 C16A 112.6(9) . . ? C58A C15 C16A 106.9(9) . . ? C14 C15 C16B 111.5(6) . . ? C14 C15 C59B 108.4(6) . . ? C16B C15 C59B 111.9(8) . . ? C14 C15 C58B 110.8(6) . . ? C16B C15 C58B 106.4(8) . . ? C59B C15 C58B 107.9(8) . . ? C12 C17 C18 141.3(5) . . ? C12 C17 Ti1 70.8(3) . . ? C18 C17 Ti1 147.2(4) . . ? C19 C18 C17 173.3(6) . . ? C18 C19 C20 177.6(7) . . ? C19 C20 C62A 109.0(9) . . ? C19 C20 C21A 108.5(8) . . ? C62A C20 C21A 117.1(11) . . ? C19 C20 C63A 107.2(8) . . ? C62A C20 C63A 106.3(10) . . ? C21A C20 C63A 108.4(10) . . ? C19 C20 C63B 109.8(9) . . ? C19 C20 C21B 110.4(8) . . ? C63B C20 C21B 117.3(11) . . ? C19 C20 C62B 108.0(7) . . ? C63B C20 C62B 103.8(10) . . ? C21B C20 C62B 107.0(10) . . ? C10 C22 C7 108.4(5) . . ? C10 C22 C23 126.2(6) . . ? C7 C22 C23 125.2(6) . . ? C10 C22 Ti1 75.8(3) . . ? C7 C22 Ti1 72.1(3) . . ? C23 C22 Ti1 122.1(4) . . ? C25 C24 C42 142.2(5) . . ? C25 C24 Ti2 71.6(3) . . ? C42 C24 Ti2 146.0(4) . . ? C24 C25 C26 143.2(5) . . ? C24 C25 Ti2 72.0(3) . . ? C26 C25 Ti2 144.4(4) . . ? C27 C26 C25 172.0(5) . . ? C26 C27 C28 175.3(5) . . ? C27 C28 C29A 110.3(6) . . ? C27 C28 C68A 108.6(7) . . ? C29A C28 C68A 113.5(8) . . ? C27 C28 C67A 111.1(6) . . ? C29A C28 C67A 104.4(8) . . ? C68A C28 C67A 108.8(9) . . ? C27 C28 C68B 112.9(6) . . ? C27 C28 C29B 106.6(6) . . ? C68B C28 C29B 108.0(8) . . ? C27 C28 C67B 107.2(8) . . ? C68B C28 C67B 108.9(10) . . ? C29B C28 C67B 113.3(9) . . ? C40 C30 C31 107.9(5) . . ? C40 C30 C49 126.3(6) . . ? C31 C30 C49 125.6(6) . . ? C40 C30 Ti2 75.5(3) . . ? C31 C30 Ti2 73.1(3) . . ? C49 C30 Ti2 121.6(4) . . ? C52 C31 C30 108.0(5) . . ? C52 C31 C32 125.6(6) . . ? C30 C31 C32 126.0(6) . . ? C52 C31 Ti2 73.4(3) . . ? C30 C31 Ti2 72.8(3) . . ? C32 C31 Ti2 125.1(4) . . ? C34 C33 C37 108.1(5) . . ? C34 C33 C51 126.7(5) . . ? C37 C33 C51 124.1(6) . . ? C34 C33 Ti2 72.5(3) . . ? C37 C33 Ti2 73.7(3) . . ? C51 C33 Ti2 129.1(4) . . ? C33 C34 C35 107.3(5) . . ? C33 C34 C55 126.7(5) . . ? C35 C34 C55 124.4(5) . . ? C33 C34 Ti2 72.9(3) . . ? C35 C34 Ti2 73.8(3) . . ? C55 C34 Ti2 130.1(4) . . ? C36 C35 C34 108.1(5) . . ? C36 C35 C64 126.0(5) . . ? C34 C35 C64 125.6(5) . . ? C36 C35 Ti2 75.7(3) . . ? C34 C35 Ti2 71.8(3) . . ? C64 C35 Ti2 122.4(4) . . ? C37 C36 C35 108.1(5) . . ? C37 C36 C56 126.0(6) . . ? C35 C36 C56 125.8(6) . . ? C37 C36 Ti2 70.8(3) . . ? C35 C36 Ti2 70.8(3) . . ? C56 C36 Ti2 126.2(4) . . ? C36 C37 C33 108.3(5) . . ? C36 C37 C38 125.8(6) . . ? C33 C37 C38 125.8(6) . . ? C36 C37 Ti2 75.7(3) . . ? C33 C37 Ti2 72.2(3) . . ? C38 C37 Ti2 121.7(4) . . ? C52 C39 C40 108.0(5) . . ? C52 C39 C60 125.4(6) . . ? C40 C39 C60 126.2(6) . . ? C52 C39 Ti2 72.4(3) . . ? C40 C39 Ti2 74.2(3) . . ? C60 C39 Ti2 124.5(4) . . ? C30 C40 C39 107.6(5) . . ? C30 C40 C41 125.5(6) . . ? C39 C40 C41 125.5(6) . . ? C30 C40 Ti2 70.8(3) . . ? C39 C40 Ti2 72.1(3) . . ? C41 C40 Ti2 132.9(4) . . ? C43 C42 C24 173.7(5) . . ? C42 C43 C44 177.5(6) . . ? C43 C44 C66B 109.2(8) . . ? C43 C44 C65B 109.0(7) . . ? C66B C44 C65B 110.4(10) . . ? C43 C44 C45B 111.9(13) . . ? C66B C44 C45B 106.3(13) . . ? C65B C44 C45B 110.0(13) . . ? C43 C44 C65A 111.8(6) . . ? C43 C44 C66A 108.6(8) . . ? C65A C44 C66A 116.9(9) . . ? C43 C44 C45A 106.5(7) . . ? C65A C44 C45A 99.8(9) . . ? C66A C44 C45A 112.6(10) . . ? C4 C47 C1 107.7(4) . . ? C4 C47 C48 126.5(6) . . ? C1 C47 C48 125.4(5) . . ? C4 C47 Ti1 73.2(3) . . ? C1 C47 Ti1 72.8(3) . . ? C48 C47 Ti1 124.8(3) . . ? C39 C52 C31 108.3(5) . . ? C39 C52 C53 125.4(7) . . ? C31 C52 C53 125.7(7) . . ? C39 C52 Ti2 74.0(3) . . ? C31 C52 Ti2 72.7(3) . . ? C53 C52 Ti2 125.7(4) . . ? C12 Ti1 C17 36.3(2) . . ? C12 Ti1 C3 101.2(2) . . ? C17 Ti1 C3 121.2(2) . . ? C12 Ti1 C7 135.0(2) . . ? C17 Ti1 C7 121.8(2) . . ? C3 Ti1 C7 116.5(2) . . ? C12 Ti1 C47 92.9(2) . . ? C17 Ti1 C47 81.8(2) . . ? C3 Ti1 C47 56.6(2) . . ? C7 Ti1 C47 127.6(2) . . ? C12 Ti1 C6 121.3(2) . . ? C17 Ti1 C6 135.0(2) . . ? C3 Ti1 C6 98.1(2) . . ? C7 Ti1 C6 34.2(2) . . ? C47 Ti1 C6 142.3(2) . . ? C12 Ti1 C1 127.2(2) . . ? C17 Ti1 C1 109.9(2) . . ? C3 Ti1 C1 56.8(2) . . ? C7 Ti1 C1 95.0(2) . . ? C47 Ti1 C1 34.3(2) . . ? C6 Ti1 C1 109.8(2) . . ? C12 Ti1 C4 78.7(2) . . ? C17 Ti1 C4 88.5(2) . . ? C3 Ti1 C4 33.8(2) . . ? C7 Ti1 C4 145.8(2) . . ? C47 Ti1 C4 34.1(2) . . ? C6 Ti1 C4 131.6(2) . . ? C1 Ti1 C4 56.7(2) . . ? C12 Ti1 C22 104.4(2) . . ? C17 Ti1 C22 87.9(2) . . ? C3 Ti1 C22 150.9(2) . . ? C7 Ti1 C22 34.4(2) . . ? C47 Ti1 C22 134.4(2) . . ? C6 Ti1 C22 56.4(2) . . ? C1 Ti1 C22 114.6(2) . . ? C4 Ti1 C22 168.4(2) . . ? C12 Ti1 C9 87.4(2) . . ? C17 Ti1 C9 104.7(2) . . ? C3 Ti1 C9 112.2(2) . . ? C7 Ti1 C9 56.9(2) . . ? C47 Ti1 C9 168.7(2) . . ? C6 Ti1 C9 34.3(2) . . ? C1 Ti1 C9 143.9(2) . . ? C4 Ti1 C9 135.6(2) . . ? C22 Ti1 C9 56.0(2) . . ? C12 Ti1 C2 133.6(2) . . ? C17 Ti1 C2 138.2(2) . . ? C3 Ti1 C2 34.1(2) . . ? C7 Ti1 C2 89.5(2) . . ? C47 Ti1 C2 56.5(2) . . ? C6 Ti1 C2 86.7(2) . . ? C1 Ti1 C2 34.0(2) . . ? C4 Ti1 C2 56.2(2) . . ? C22 Ti1 C2 121.9(2) . . ? C9 Ti1 C2 116.1(2) . . ? C12 Ti1 C10 79.0(2) . . ? C17 Ti1 C10 79.4(2) . . ? C3 Ti1 C10 145.1(2) . . ? C7 Ti1 C10 56.0(2) . . ? C47 Ti1 C10 157.7(2) . . ? C6 Ti1 C10 55.6(2) . . ? C1 Ti1 C10 147.7(2) . . ? C4 Ti1 C10 155.5(2) . . ? C22 Ti1 C10 33.2(2) . . ? C9 Ti1 C10 33.1(2) . . ? C2 Ti1 C10 141.7(2) . . ? C25 Ti2 C24 36.3(2) . . ? C25 Ti2 C30 124.9(2) . . ? C24 Ti2 C30 105.9(2) . . ? C25 Ti2 C34 134.8(2) . . ? C24 Ti2 C34 122.1(2) . . ? C30 Ti2 C34 96.5(2) . . ? C25 Ti2 C33 120.5(2) . . ? C24 Ti2 C33 134.9(2) . . ? C30 Ti2 C33 113.5(2) . . ? C34 Ti2 C33 34.7(2) . . ? C25 Ti2 C31 91.0(2) . . ? C24 Ti2 C31 80.3(2) . . ? C30 Ti2 C31 34.2(2) . . ? C34 Ti2 C31 129.9(2) . . ? C33 Ti2 C31 144.4(2) . . ? C25 Ti2 C52 80.5(2) . . ? C24 Ti2 C52 90.7(2) . . ? C30 Ti2 C52 56.5(2) . . ? C34 Ti2 C52 143.7(2) . . ? C33 Ti2 C52 129.0(2) . . ? C31 Ti2 C52 33.9(2) . . ? C25 Ti2 C37 86.9(2) . . ? C24 Ti2 C37 104.5(2) . . ? C30 Ti2 C37 147.6(2) . . ? C34 Ti2 C37 57.0(2) . . ? C33 Ti2 C37 34.1(2) . . ? C31 Ti2 C37 168.0(2) . . ? C52 Ti2 C37 134.2(2) . . ? C25 Ti2 C35 104.6(2) . . ? C24 Ti2 C35 88.1(2) . . ? C30 Ti2 C35 113.4(2) . . ? C34 Ti2 C35 34.4(2) . . ? C33 Ti2 C35 56.9(2) . . ? C31 Ti2 C35 135.3(2) . . ? C52 Ti2 C35 169.1(2) . . ? C37 Ti2 C35 56.4(2) . . ? C25 Ti2 C39 105.6(2) . . ? C24 Ti2 C39 124.0(2) . . ? C30 Ti2 C39 56.4(2) . . ? C34 Ti2 C39 113.0(2) . . ? C33 Ti2 C39 96.5(2) . . ? C31 Ti2 C39 56.1(2) . . ? C52 Ti2 C39 33.5(2) . . ? C37 Ti2 C39 113.3(2) . . ? C35 Ti2 C39 147.3(2) . . ? C25 Ti2 C40 136.1(2) . . ? C24 Ti2 C40 136.0(2) . . ? C30 Ti2 C40 33.7(2) . . ? C34 Ti2 C40 88.2(2) . . ? C33 Ti2 C40 88.6(2) . . ? C31 Ti2 C40 55.9(2) . . ? C52 Ti2 C40 55.8(2) . . ? C37 Ti2 C40 119.3(2) . . ? C35 Ti2 C40 119.2(2) . . ? C39 Ti2 C40 33.7(2) . . ? C25 Ti2 C36 78.6(2) . . ? C24 Ti2 C36 79.1(2) . . ? C30 Ti2 C36 146.9(2) . . ? C34 Ti2 C36 56.2(2) . . ? C33 Ti2 C36 55.9(2) . . ? C31 Ti2 C36 156.8(2) . . ? C52 Ti2 C36 156.2(2) . . ? C37 Ti2 C36 33.4(2) . . ? C35 Ti2 C36 33.5(2) . . ? C39 Ti2 C36 146.7(2) . . ? C40 Ti2 C36 142.5(2) . . ? _refine_diff_density_max 0.331 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.047 #===END data_249 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H48 Zr' _chemical_formula_weight 547.94 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.093(2) _cell_length_b 30.743(6) _cell_length_c 11.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.23(3) _cell_angle_gamma 90.00 _cell_volume 3120.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _exptl_crystal_description PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method ? _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type 'MEAN IMAGING PLATE INTENSITY METHOD' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE-IPDS _diffrn_measurement_method 'LASER SCANNED IMAGING PLATE' _diffrn_standards_number 50-200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 360 _diffrn_standards_decay_% ? _diffrn_reflns_number 6266 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 21.10 _reflns_number_total 3340 _reflns_number_observed 2499 _reflns_observed_criterion >2sigma(I) _computing_data_collection STOE-EXPOSE _computing_cell_refinement STOE-CELL _computing_data_reduction STOE-INTEGRATE _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3340 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_obs 0.0367 _refine_ls_wR_factor_all 0.0859 _refine_ls_wR_factor_obs 0.0821 _refine_ls_goodness_of_fit_all 0.939 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 0.939 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.3228(5) 0.11098(14) 0.5788(4) 0.0476(11) Uani 1 d . . C2 C 0.4318(5) 0.13117(14) 0.6542(4) 0.0435(11) Uani 1 d . . C3 C 0.5030(5) 0.14630(13) 0.7622(4) 0.0414(11) Uani 1 d . . C4 C 0.4973(5) 0.15154(13) 0.8703(4) 0.0405(11) Uani 1 d . . C5 C 0.5837(5) 0.17365(14) 0.9730(4) 0.0431(11) Uani 1 d . . C6 C 0.6478(5) 0.19237(15) 1.0629(4) 0.0468(12) Uani 1 d . . C7 C 0.7281(5) 0.2159(2) 1.1741(4) 0.0561(13) Uani 1 d . . C8 C 0.8981(6) 0.2075(2) 1.2025(5) 0.108(2) Uani 1 d . . H8A H 0.9501(6) 0.2226(2) 1.2747(5) 0.162 Uiso 1 calc R . H8B H 0.9349(6) 0.2178(2) 1.1376(5) 0.162 Uiso 1 calc R . H8C H 0.9173(6) 0.1769(2) 1.2133(5) 0.162 Uiso 1 calc R . C9 C 0.1927(5) 0.03878(14) 0.8365(5) 0.0548(13) Uani 1 d . . C10 C 0.2806(6) 0.03044(13) 0.7565(4) 0.0518(12) Uani 1 d . . C11 C 0.4341(5) 0.04330(14) 0.8117(5) 0.0527(12) Uani 1 d . . C12 C 0.4403(6) 0.05877(14) 0.9261(5) 0.0581(14) Uani 1 d . . C13 C 0.2913(7) 0.05704(14) 0.9413(4) 0.0585(14) Uani 1 d . . C14 C 0.2536(8) 0.0660(2) 1.0583(4) 0.096(2) Uani 1 d . . H14A H 0.3411(8) 0.0786(2) 1.1146(4) 0.144 Uiso 1 calc R . H14B H 0.2270(8) 0.0393(2) 1.0900(4) 0.144 Uiso 1 calc R . H14C H 0.1688(8) 0.0858(2) 1.0441(4) 0.144 Uiso 1 calc R . C15 C 0.0008(5) 0.1407(2) 0.6973(5) 0.0524(13) Uani 1 d . . C16 C 0.0316(5) 0.14171(15) 0.8235(4) 0.0499(12) Uani 1 d . . C17 C 0.1489(5) 0.17262(15) 0.8682(4) 0.0479(12) Uani 1 d . . C18 C 0.1827(5) 0.19285(14) 0.7697(4) 0.0448(11) Uani 1 d . . C19 C 0.0916(5) 0.17310(15) 0.6646(4) 0.0490(12) Uani 1 d . . C20 C 0.0787(6) 0.1894(2) 0.5395(4) 0.077(2) Uani 1 d . . H20A H 0.0103(6) 0.1709(2) 0.4822(4) 0.116 Uiso 1 calc R . H20B H 0.1780(6) 0.1889(2) 0.5256(4) 0.116 Uiso 1 calc R . H20C H 0.0398(6) 0.2186(2) 0.5312(4) 0.116 Uiso 1 calc R . C21 C 0.3029(6) 0.1013(2) 0.4460(4) 0.0619(14) Uani 1 d . . C22 C 0.3310(7) 0.1426(2) 0.3820(4) 0.088(2) Uani 1 d . . H22A H 0.2573(7) 0.1644(2) 0.3871(4) 0.132 Uiso 1 calc R . H22B H 0.3209(7) 0.1362(2) 0.2993(4) 0.132 Uiso 1 calc R . H22C H 0.4324(7) 0.1533(2) 0.4193(4) 0.132 Uiso 1 calc R . C23 C 0.0335(6) 0.0210(2) 0.8203(5) 0.092(2) Uani 1 d . . H23A H -0.0046(6) 0.0307(2) 0.8851(5) 0.139 Uiso 1 calc R . H23B H 0.0367(6) -0.0102(2) 0.8198(5) 0.139 Uiso 1 calc R . H23C H -0.0329(6) 0.0312(2) 0.7457(5) 0.139 Uiso 1 calc R . C24 C 0.2261(7) 0.0042(2) 0.6429(4) 0.079(2) Uani 1 d . . H24A H 0.3056(7) 0.0030(2) 0.6033(4) 0.118 Uiso 1 calc R . H24B H 0.1368(7) 0.0176(2) 0.5909(4) 0.118 Uiso 1 calc R . H24C H 0.2013(7) -0.0248(2) 0.6621(4) 0.118 Uiso 1 calc R . C25 C 0.5703(6) 0.0371(2) 0.7635(5) 0.080(2) Uani 1 d . . H25A H 0.5364(6) 0.0261(2) 0.6831(5) 0.120 Uiso 1 calc R . H25B H 0.6401(6) 0.0168(2) 0.8131(5) 0.120 Uiso 1 calc R . H25C H 0.6210(6) 0.0645(2) 0.7636(5) 0.120 Uiso 1 calc R . C26 C -0.1273(5) 0.1159(2) 0.6111(5) 0.082(2) Uani 1 d . . H26A H -0.1715(5) 0.0957(2) 0.6549(5) 0.123 Uiso 1 calc R . H26B H -0.0872(5) 0.1004(2) 0.5548(5) 0.123 Uiso 1 calc R . H26C H -0.2044(5) 0.1360(2) 0.5687(5) 0.123 Uiso 1 calc R . C27 C 0.2855(5) 0.23146(14) 0.7742(5) 0.0674(14) Uani 1 d . . H27A H 0.3353(5) 0.23865(14) 0.8562(5) 0.101 Uiso 1 calc R . H27B H 0.2255(5) 0.25580(14) 0.7356(5) 0.101 Uiso 1 calc R . H27C H 0.3612(5) 0.22459(14) 0.7337(5) 0.101 Uiso 1 calc R . C28 C -0.0690(6) 0.1225(2) 0.8937(5) 0.088(2) Uani 1 d . . H28A H -0.0234(6) 0.1275(2) 0.9777(5) 0.132 Uiso 1 calc R . H28B H -0.0798(6) 0.0918(2) 0.8787(5) 0.132 Uiso 1 calc R . H28C H -0.1680(6) 0.1361(2) 0.8695(5) 0.132 Uiso 1 calc R . C29 C 0.2063(6) 0.1873(2) 0.9969(4) 0.0708(15) Uani 1 d . . H29A H 0.1673(6) 0.1682(2) 1.0468(4) 0.106 Uiso 1 calc R . H29B H 0.1718(6) 0.2164(2) 1.0040(4) 0.106 Uiso 1 calc R . H29C H 0.3162(6) 0.1865(2) 1.0217(4) 0.106 Uiso 1 calc R . C30 C 0.5847(6) 0.0689(2) 1.0239(5) 0.090(2) Uani 1 d . . H30A H 0.5583(6) 0.0790(2) 1.0937(5) 0.136 Uiso 1 calc R . H30B H 0.6417(6) 0.0910(2) 0.9968(5) 0.136 Uiso 1 calc R . H30C H 0.6460(6) 0.0431(2) 1.0436(5) 0.136 Uiso 1 calc R . C31 C 0.1406(7) 0.0845(2) 0.3831(5) 0.093(2) Uani 1 d . . H31A H 0.0663(7) 0.1058(2) 0.3900(5) 0.140 Uiso 1 calc R . H31B H 0.1227(7) 0.0579(2) 0.4203(5) 0.140 Uiso 1 calc R . H31C H 0.1317(7) 0.0793(2) 0.3000(5) 0.140 Uiso 1 calc R . C32 C 0.4203(8) 0.0677(2) 0.4353(5) 0.102(2) Uani 1 d . . H32A H 0.4048(8) 0.0414(2) 0.4750(5) 0.153 Uiso 1 calc R . H32B H 0.5214(8) 0.0787(2) 0.4719(5) 0.153 Uiso 1 calc R . H32C H 0.4090(8) 0.0617(2) 0.3522(5) 0.153 Uiso 1 calc R . C33 C 0.6669(7) 0.2005(2) 1.2757(5) 0.114(2) Uani 1 d . . H33A H 0.7186(7) 0.2157(2) 1.3479(5) 0.171 Uiso 1 calc R . H33B H 0.6842(7) 0.1698(2) 1.2873(5) 0.171 Uiso 1 calc R . H33C H 0.5590(7) 0.2063(2) 1.2564(5) 0.171 Uiso 1 calc R . C34 C 0.6963(8) 0.2646(2) 1.1532(6) 0.114(2) Uani 1 d . . H34A H 0.7470(8) 0.2804(2) 1.2245(6) 0.171 Uiso 1 calc R . H34B H 0.5880(8) 0.2697(2) 1.1339(6) 0.171 Uiso 1 calc R . H34C H 0.7339(8) 0.2742(2) 1.0882(6) 0.171 Uiso 1 calc R . Zr Zr 0.27619(4) 0.113402(12) 0.77494(3) 0.0342(2) 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 0.056(3) 0.036(3) 0.050(3) -0.002(2) 0.013(3) 0.000(3) C2 0.045(3) 0.041(3) 0.050(3) 0.001(2) 0.021(3) -0.001(2) C3 0.035(3) 0.040(3) 0.053(3) -0.005(2) 0.018(2) -0.005(2) C4 0.042(3) 0.033(3) 0.046(3) 0.000(2) 0.012(2) 0.007(2) C5 0.041(3) 0.042(3) 0.042(3) -0.004(2) 0.004(2) -0.001(2) C6 0.042(3) 0.049(3) 0.048(3) -0.004(3) 0.010(2) -0.001(2) C7 0.050(3) 0.071(4) 0.044(3) -0.012(3) 0.008(2) -0.011(3) C8 0.052(4) 0.187(7) 0.074(4) -0.029(4) 0.000(3) -0.019(4) C9 0.061(3) 0.041(3) 0.063(3) 0.007(3) 0.018(3) -0.014(3) C10 0.064(3) 0.034(3) 0.055(3) 0.001(2) 0.012(3) -0.008(3) C11 0.058(4) 0.028(2) 0.070(4) 0.009(2) 0.015(3) 0.004(2) C12 0.065(4) 0.036(3) 0.062(4) 0.007(2) -0.003(3) -0.005(3) C13 0.087(4) 0.040(3) 0.050(3) 0.012(2) 0.022(3) -0.005(3) C14 0.151(6) 0.087(4) 0.056(4) 0.019(3) 0.040(4) 0.002(4) C15 0.029(3) 0.060(3) 0.064(4) -0.011(3) 0.007(3) -0.001(3) C16 0.040(3) 0.056(3) 0.058(4) 0.000(2) 0.020(3) 0.002(3) C17 0.038(3) 0.055(3) 0.050(3) -0.007(3) 0.011(2) 0.005(2) C18 0.036(3) 0.038(3) 0.059(3) -0.003(2) 0.012(2) 0.006(2) C19 0.042(3) 0.049(3) 0.051(3) 0.001(2) 0.005(3) 0.012(2) C20 0.095(4) 0.069(4) 0.057(3) 0.012(3) 0.005(3) 0.020(3) C21 0.086(4) 0.061(4) 0.041(3) -0.015(2) 0.021(3) -0.012(3) C22 0.143(5) 0.088(4) 0.045(3) -0.004(3) 0.044(3) -0.020(4) C23 0.090(4) 0.067(4) 0.131(5) -0.010(4) 0.049(4) -0.035(3) C24 0.109(5) 0.046(3) 0.078(4) -0.020(3) 0.021(3) -0.022(3) C25 0.070(4) 0.052(3) 0.123(5) 0.002(3) 0.035(4) 0.017(3) C26 0.050(3) 0.091(4) 0.090(4) -0.013(4) -0.006(3) -0.007(3) C27 0.060(3) 0.037(3) 0.102(4) 0.004(3) 0.017(3) 0.004(3) C28 0.063(3) 0.113(5) 0.106(4) -0.008(4) 0.052(3) -0.013(3) C29 0.078(4) 0.076(4) 0.063(3) -0.024(3) 0.028(3) 0.001(3) C30 0.088(4) 0.064(4) 0.087(4) 0.024(3) -0.027(3) -0.007(3) C31 0.111(5) 0.101(5) 0.054(3) -0.020(3) 0.002(3) -0.025(4) C32 0.151(6) 0.093(5) 0.074(4) -0.030(3) 0.051(4) 0.019(5) C33 0.102(5) 0.180(7) 0.063(4) -0.018(4) 0.028(4) -0.035(5) C34 0.149(6) 0.074(4) 0.115(5) -0.045(4) 0.032(5) -0.015(4) Zr 0.0338(2) 0.0320(2) 0.0361(2) -0.0018(2) 0.0086(2) -0.0036(2) _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 1.285(6) . ? C1 C21 1.532(6) . ? C1 Zr 2.434(4) . ? C2 C3 1.325(6) . ? C2 Zr 2.319(4) . ? C3 C4 1.282(6) . ? C3 Zr 2.338(4) . ? C4 C5 1.408(6) . ? C4 Zr 2.324(4) . ? C5 C6 1.192(6) . ? C6 C7 1.483(7) . ? C7 C33 1.515(7) . ? C7 C8 1.510(7) . ? C7 C34 1.532(7) . ? C9 C10 1.408(6) . ? C9 C13 1.412(6) . ? C9 C23 1.509(6) . ? C9 Zr 2.580(4) . ? C10 C11 1.420(6) . ? C10 C24 1.509(6) . ? C10 Zr 2.561(4) . ? C11 C12 1.398(6) . ? C11 C25 1.508(6) . ? C11 Zr 2.558(4) . ? C12 C13 1.416(7) . ? C12 C30 1.510(7) . ? C12 Zr 2.583(4) . ? C13 C14 1.518(6) . ? C13 Zr 2.572(4) . ? C15 C19 1.412(6) . ? C15 C16 1.415(6) . ? C15 C26 1.513(6) . ? C15 Zr 2.554(4) . ? C16 C17 1.414(6) . ? C16 C28 1.506(6) . ? C16 Zr 2.593(4) . ? C17 C18 1.411(6) . ? C17 C29 1.509(6) . ? C17 Zr 2.555(4) . ? C18 C19 1.408(6) . ? C18 C27 1.502(6) . ? C18 Zr 2.581(4) . ? C19 C20 1.511(6) . ? C19 Zr 2.575(4) . ? C21 C32 1.516(7) . ? C21 C22 1.529(6) . ? C21 C31 1.542(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 129.2(4) . . ? C2 C1 Zr 69.5(3) . . ? C21 C1 Zr 161.3(3) . . ? C1 C2 C3 153.5(4) . . ? C1 C2 Zr 79.3(3) . . ? C3 C2 Zr 74.3(3) . . ? C4 C3 C2 146.1(4) . . ? C4 C3 Zr 73.4(3) . . ? C2 C3 Zr 72.7(3) . . ? C3 C4 C5 136.6(4) . . ? C3 C4 Zr 74.7(3) . . ? C5 C4 Zr 148.4(3) . . ? C6 C5 C4 175.4(5) . . ? C5 C6 C7 179.6(4) . . ? C6 C7 C33 109.3(4) . . ? C6 C7 C8 109.4(4) . . ? C33 C7 C8 110.7(5) . . ? C6 C7 C34 108.2(4) . . ? C33 C7 C34 109.5(5) . . ? C8 C7 C34 109.7(5) . . ? C10 C9 C13 107.5(4) . . ? C10 C9 C23 123.6(5) . . ? C13 C9 C23 127.4(5) . . ? C10 C9 Zr 73.4(2) . . ? C13 C9 Zr 73.8(2) . . ? C23 C9 Zr 129.4(3) . . ? C9 C10 C11 108.6(4) . . ? C9 C10 C24 124.6(5) . . ? C11 C10 C24 125.8(5) . . ? C9 C10 Zr 74.8(2) . . ? C11 C10 Zr 73.8(2) . . ? C24 C10 Zr 126.6(3) . . ? C12 C11 C10 107.3(4) . . ? C12 C11 C25 125.3(5) . . ? C10 C11 C25 127.1(5) . . ? C12 C11 Zr 75.2(3) . . ? C10 C11 Zr 74.0(2) . . ? C25 C11 Zr 121.7(3) . . ? C11 C12 C13 108.7(4) . . ? C11 C12 C30 125.6(5) . . ? C13 C12 C30 125.1(5) . . ? C11 C12 Zr 73.3(3) . . ? C13 C12 Zr 73.6(3) . . ? C30 C12 Zr 126.5(3) . . ? C9 C13 C12 107.8(4) . . ? C9 C13 C14 126.7(5) . . ? C12 C13 C14 124.7(5) . . ? C9 C13 Zr 74.4(2) . . ? C12 C13 Zr 74.5(3) . . ? C14 C13 Zr 125.0(3) . . ? C19 C15 C16 107.6(4) . . ? C19 C15 C26 125.2(5) . . ? C16 C15 C26 126.2(5) . . ? C19 C15 Zr 74.8(2) . . ? C16 C15 Zr 75.5(2) . . ? C26 C15 Zr 124.5(3) . . ? C15 C16 C17 107.8(4) . . ? C15 C16 C28 125.4(5) . . ? C17 C16 C28 125.0(5) . . ? C15 C16 Zr 72.5(2) . . ? C17 C16 Zr 72.6(2) . . ? C28 C16 Zr 132.4(3) . . ? C18 C17 C16 108.1(4) . . ? C18 C17 C29 125.4(4) . . ? C16 C17 C29 125.5(4) . . ? C18 C17 Zr 75.1(2) . . ? C16 C17 Zr 75.5(2) . . ? C29 C17 Zr 124.1(3) . . ? C19 C18 C17 107.8(4) . . ? C19 C18 C27 125.5(4) . . ? C17 C18 C27 126.5(4) . . ? C19 C18 Zr 73.9(2) . . ? C17 C18 Zr 73.1(2) . . ? C27 C18 Zr 123.3(3) . . ? C18 C19 C15 108.5(4) . . ? C18 C19 C20 124.1(4) . . ? C15 C19 C20 126.8(4) . . ? C18 C19 Zr 74.4(2) . . ? C15 C19 Zr 73.2(2) . . ? C20 C19 Zr 125.4(3) . . ? C32 C21 C22 108.0(4) . . ? C32 C21 C31 109.5(4) . . ? C22 C21 C31 108.4(4) . . ? C32 C21 C1 109.1(4) . . ? C22 C21 C1 110.0(4) . . ? C31 C21 C1 111.8(4) . . ? C2 Zr C4 65.0(2) . . ? C2 Zr C3 33.0(2) . . ? C4 Zr C3 31.92(14) . . ? C2 Zr C1 31.25(15) . . ? C4 Zr C1 96.2(2) . . ? C3 Zr C1 64.3(2) . . ? C2 Zr C15 114.4(2) . . ? C4 Zr C15 129.41(15) . . ? C3 Zr C15 129.1(2) . . ? C1 Zr C15 95.1(2) . . ? C2 Zr C17 120.9(2) . . ? C4 Zr C17 82.66(14) . . ? C3 Zr C17 103.34(15) . . ? C1 Zr C17 129.60(14) . . ? C15 Zr C17 53.17(14) . . ? C2 Zr C11 83.73(15) . . ? C4 Zr C11 88.57(15) . . ? C3 Zr C11 84.92(14) . . ? C1 Zr C11 83.94(15) . . ? C15 Zr C11 141.7(2) . . ? C17 Zr C11 146.0(2) . . ? C2 Zr C10 99.1(2) . . ? C4 Zr C10 120.72(15) . . ? C3 Zr C10 113.0(2) . . ? C1 Zr C10 83.13(14) . . ? C15 Zr C10 109.5(2) . . ? C17 Zr C10 139.9(2) . . ? C11 Zr C10 32.20(14) . . ? C2 Zr C13 134.4(2) . . ? C4 Zr C13 97.1(2) . . ? C3 Zr C13 118.5(2) . . ? C1 Zr C13 134.20(15) . . ? C15 Zr C13 109.2(2) . . ? C17 Zr C13 95.5(2) . . ? C11 Zr C13 52.9(2) . . ? C10 Zr C13 52.62(14) . . ? C2 Zr C19 87.36(15) . . ? C4 Zr C19 103.57(15) . . ? C3 Zr C19 97.11(15) . . ? C1 Zr C19 79.35(14) . . ? C15 Zr C19 31.96(14) . . ? C17 Zr C19 52.70(14) . . ? C11 Zr C19 160.2(2) . . ? C10 Zr C19 133.8(2) . . ? C13 Zr C19 138.2(2) . . ? C2 Zr C9 130.8(2) . . ? C4 Zr C9 126.79(15) . . ? C3 Zr C9 137.33(15) . . ? C1 Zr C9 112.0(2) . . ? C15 Zr C9 93.1(2) . . ? C17 Zr C9 108.2(2) . . ? C11 Zr C9 53.08(15) . . ? C10 Zr C9 31.79(14) . . ? C13 Zr C9 31.82(14) . . ? C19 Zr C9 124.8(2) . . ? C2 Zr C18 90.88(15) . . ? C4 Zr C18 76.65(14) . . ? C3 Zr C18 83.08(14) . . ? C1 Zr C18 98.58(14) . . ? C15 Zr C18 52.93(14) . . ? C17 Zr C18 31.87(13) . . ? C11 Zr C18 165.17(15) . . ? C10 Zr C18 162.41(15) . . ? C13 Zr C18 127.1(2) . . ? C19 Zr C18 31.70(13) . . ? C9 Zr C18 136.7(2) . . ? _refine_diff_density_max 0.217 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.052 #===END