# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Chen, Yaofeng' _publ_contact_author_name 'Chen, Yaofeng' _publ_contact_author_email yaofchen@mail.sioc.ac.cn _publ_section_title ; Monoalkyl and monoanilide yttrium complexes containing tridentate pyridyl-1-azaallyl dianionic ligands ; # Attachment '- cif.cif' data_cd29353 _database_code_depnum_ccdc_archive 'CCDC 789698' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H51 N2 O Si2 Y' _chemical_formula_weight 612.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2709(11) _cell_length_b 17.719(2) _cell_length_c 21.296(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3498.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3168 _cell_measurement_theta_min 4.598 _cell_measurement_theta_max 41.629 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.428 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.168 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5761 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21215 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.1526 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7892 _reflns_number_gt 3954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0276P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(5) _refine_ls_number_reflns 7892 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y Y 0.03383(4) 0.03096(2) 1.013227(16) 0.04441(11) Uani 1 1 d . . . Si1 Si -0.11447(16) 0.11521(8) 1.14035(6) 0.0621(4) Uani 1 1 d . . . Si2 Si 0.10125(15) -0.15899(7) 1.09246(6) 0.0590(4) Uani 1 1 d . . . O1 O 0.2557(3) 0.08502(16) 0.98158(14) 0.0597(7) Uani 1 1 d . . . N1 N -0.0840(3) 0.00102(17) 0.92235(13) 0.0436(9) Uani 1 1 d . . . N2 N -0.2022(3) 0.00567(18) 1.05247(14) 0.0465(9) Uani 1 1 d . . . C1 C -0.2502(5) -0.0635(3) 0.84925(19) 0.0701(15) Uani 1 1 d . . . H1A H -0.2630 -0.0190 0.8242 0.105 Uiso 1 1 calc R . . H1B H -0.3394 -0.0910 0.8511 0.105 Uiso 1 1 calc R . . H1C H -0.1770 -0.0947 0.8307 0.105 Uiso 1 1 calc R . . C2 C -0.2051(5) -0.0414(2) 0.91453(18) 0.0494(11) Uani 1 1 d . . . C3 C -0.2888(5) -0.0665(2) 0.9630(2) 0.0557(12) Uani 1 1 d . . . H3 H -0.3561 -0.1029 0.9515 0.067 Uiso 1 1 calc R . . C4 C -0.2921(4) -0.0475(2) 1.02760(18) 0.0499(12) Uani 1 1 d . . . C5 C -0.3999(5) -0.0810(3) 1.0657(2) 0.0684(14) Uani 1 1 d . . . H5 H -0.4575 -0.1193 1.0495 0.082 Uiso 1 1 calc R . . C6 C -0.4189(5) -0.0570(3) 1.1258(2) 0.0833(18) Uani 1 1 d . . . H6 H -0.4875 -0.0801 1.1512 0.100 Uiso 1 1 calc R . . C7 C -0.3364(5) 0.0013(3) 1.1489(2) 0.0698(15) Uani 1 1 d . . . H7 H -0.3541 0.0202 1.1889 0.084 Uiso 1 1 calc R . . C8 C -0.2274(4) 0.0319(3) 1.11254(18) 0.0560(11) Uani 1 1 d . . . C11 C -0.0049(4) 0.0247(3) 0.86783(15) 0.0455(10) Uani 1 1 d . . . C12 C -0.0375(5) 0.0927(2) 0.83827(16) 0.0505(10) Uani 1 1 d . . . C13 C 0.0494(6) 0.1180(3) 0.78911(18) 0.0694(14) Uani 1 1 d . . . H13 H 0.0281 0.1632 0.7690 0.083 Uiso 1 1 calc R . . C14 C 0.1661(6) 0.0763(4) 0.7704(2) 0.0809(17) Uani 1 1 d . . . H14 H 0.2243 0.0936 0.7379 0.097 Uiso 1 1 calc R . . C15 C 0.1968(5) 0.0104(3) 0.7988(2) 0.0828(17) Uani 1 1 d . . . H15 H 0.2768 -0.0169 0.7853 0.099 Uiso 1 1 calc R . . C16 C 0.1133(5) -0.0183(3) 0.84756(19) 0.0603(12) Uani 1 1 d . . . C17 C -0.1676(5) 0.1400(3) 0.8570(2) 0.0635(14) Uani 1 1 d . . . H17 H -0.2278 0.1086 0.8843 0.076 Uiso 1 1 calc R . . C18 C -0.1250(6) 0.2087(3) 0.8943(3) 0.104(2) Uani 1 1 d . . . H18A H -0.0768 0.2440 0.8673 0.156 Uiso 1 1 calc R . . H18B H -0.0612 0.1940 0.9276 0.156 Uiso 1 1 calc R . . H18C H -0.2097 0.2317 0.9117 0.156 Uiso 1 1 calc R . . C19 C -0.2603(6) 0.1629(4) 0.8011(2) 0.108(2) Uani 1 1 d . . . H19A H -0.3459 0.1877 0.8158 0.162 Uiso 1 1 calc R . . H19B H -0.2867 0.1187 0.7776 0.162 Uiso 1 1 calc R . . H19C H -0.2068 0.1966 0.7746 0.162 Uiso 1 1 calc R . . C20 C 0.1535(6) -0.0937(3) 0.8762(2) 0.0839(17) Uani 1 1 d . . . H20 H 0.0920 -0.1013 0.9131 0.101 Uiso 1 1 calc R . . C21 C 0.3085(7) -0.0977(3) 0.8979(3) 0.111(2) Uani 1 1 d . . . H21A H 0.3715 -0.0942 0.8622 0.166 Uiso 1 1 calc R . . H21B H 0.3247 -0.1448 0.9191 0.166 Uiso 1 1 calc R . . H21C H 0.3278 -0.0567 0.9261 0.166 Uiso 1 1 calc R . . C22 C 0.1242(7) -0.1590(3) 0.8306(3) 0.132(3) Uani 1 1 d . . . H22A H 0.1758 -0.1505 0.7922 0.198 Uiso 1 1 calc R . . H22B H 0.0227 -0.1618 0.8220 0.198 Uiso 1 1 calc R . . H22C H 0.1558 -0.2055 0.8492 0.198 Uiso 1 1 calc R . . C23 C 0.0063(6) 0.0823(3) 1.20449(19) 0.0940(19) Uani 1 1 d . . . H23A H 0.0799 0.0503 1.1873 0.141 Uiso 1 1 calc R . . H23B H -0.0489 0.0546 1.2349 0.141 Uiso 1 1 calc R . . H23C H 0.0504 0.1251 1.2244 0.141 Uiso 1 1 calc R . . C24 C -0.2441(7) 0.1841(3) 1.1761(2) 0.106(2) Uani 1 1 d . . . H24A H -0.1916 0.2260 1.1933 0.158 Uiso 1 1 calc R . . H24B H -0.2977 0.1597 1.2088 0.158 Uiso 1 1 calc R . . H24C H -0.3093 0.2020 1.1444 0.158 Uiso 1 1 calc R . . C25 C -0.0128(5) 0.1437(2) 1.07252(18) 0.0701(14) Uani 1 1 d . . . H25A H 0.0770 0.1674 1.0851 0.084 Uiso 1 1 calc R . . H25B H -0.0676 0.1795 1.0476 0.084 Uiso 1 1 calc R . . C31 C 0.1573(5) -0.0642(2) 1.07012(19) 0.0585(13) Uani 1 1 d . . . H31A H 0.2468 -0.0715 1.0473 0.070 Uiso 1 1 calc R . . H31B H 0.1841 -0.0402 1.1094 0.070 Uiso 1 1 calc R . . C32 C -0.0335(7) -0.1563(3) 1.1560(2) 0.1043(19) Uani 1 1 d . . . H32A H 0.0010 -0.1248 1.1895 0.156 Uiso 1 1 calc R . . H32B H -0.0492 -0.2065 1.1716 0.156 Uiso 1 1 calc R . . H32C H -0.1226 -0.1363 1.1402 0.156 Uiso 1 1 calc R . . C33 C 0.2549(6) -0.2194(3) 1.1214(2) 0.0897(17) Uani 1 1 d . . . H33A H 0.3197 -0.2297 1.0873 0.135 Uiso 1 1 calc R . . H33B H 0.2175 -0.2661 1.1376 0.135 Uiso 1 1 calc R . . H33C H 0.3057 -0.1932 1.1541 0.135 Uiso 1 1 calc R . . C34 C 0.0222(6) -0.2094(3) 1.0244(2) 0.0995(17) Uani 1 1 d . . . H34A H -0.0560 -0.1803 1.0075 0.149 Uiso 1 1 calc R . . H34B H -0.0132 -0.2577 1.0378 0.149 Uiso 1 1 calc R . . H34C H 0.0947 -0.2163 0.9928 0.149 Uiso 1 1 calc R . . C35 C 0.2824(5) 0.1395(3) 0.9339(2) 0.0822(17) Uani 1 1 d . . . H35A H 0.2515 0.1892 0.9475 0.099 Uiso 1 1 calc R . . H35B H 0.2310 0.1265 0.8957 0.099 Uiso 1 1 calc R . . C36 C 0.4393(6) 0.1385(3) 0.9230(3) 0.0911(17) Uani 1 1 d . . . H36A H 0.4723 0.1859 0.9052 0.109 Uiso 1 1 calc R . . H36B H 0.4664 0.0975 0.8952 0.109 Uiso 1 1 calc R . . C37 C 0.4992(4) 0.1267(3) 0.9878(3) 0.0944(17) Uani 1 1 d . . . H37A H 0.5888 0.0985 0.9863 0.113 Uiso 1 1 calc R . . H37B H 0.5165 0.1746 1.0085 0.113 Uiso 1 1 calc R . . C38 C 0.3848(5) 0.0832(3) 1.0204(3) 0.0965(17) Uani 1 1 d . . . H38A H 0.4158 0.0315 1.0267 0.116 Uiso 1 1 calc R . . H38B H 0.3649 0.1054 1.0611 0.116 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.03433(18) 0.0512(2) 0.04772(19) 0.0012(2) 0.0002(2) 0.0003(2) Si1 0.0649(9) 0.0718(10) 0.0496(8) -0.0048(7) -0.0007(7) 0.0154(8) Si2 0.0564(9) 0.0534(9) 0.0673(8) 0.0087(7) 0.0004(7) 0.0004(7) O1 0.0368(17) 0.069(2) 0.0735(18) 0.0128(19) 0.0040(17) -0.0092(14) N1 0.036(2) 0.054(2) 0.0398(18) 0.0044(15) 0.0005(14) -0.0004(15) N2 0.040(2) 0.056(3) 0.0435(19) 0.0066(17) 0.0018(16) 0.0046(17) C1 0.065(4) 0.085(4) 0.060(3) -0.006(3) -0.003(3) -0.017(3) C2 0.051(3) 0.048(3) 0.049(2) 0.002(2) 0.001(2) -0.002(2) C3 0.041(3) 0.061(3) 0.065(3) 0.005(2) -0.003(2) -0.011(2) C4 0.033(2) 0.062(3) 0.054(3) 0.012(2) 0.003(2) -0.001(2) C5 0.042(3) 0.092(4) 0.071(3) 0.019(3) 0.006(2) -0.012(3) C6 0.052(4) 0.131(5) 0.068(3) 0.021(3) 0.014(3) -0.009(3) C7 0.061(3) 0.099(5) 0.049(3) 0.005(3) 0.012(2) 0.003(3) C8 0.045(3) 0.073(3) 0.049(2) 0.008(3) -0.002(2) 0.008(3) C11 0.042(3) 0.060(3) 0.0338(19) 0.003(2) 0.0026(16) -0.003(2) C12 0.048(3) 0.064(3) 0.040(2) 0.004(2) 0.003(2) -0.002(3) C13 0.068(4) 0.089(4) 0.050(3) 0.019(2) 0.003(3) -0.005(3) C14 0.070(4) 0.123(5) 0.050(3) 0.022(3) 0.025(3) 0.005(3) C15 0.068(4) 0.117(5) 0.064(3) 0.010(3) 0.025(3) 0.022(3) C16 0.055(3) 0.070(4) 0.056(3) 0.006(3) 0.013(2) 0.011(3) C17 0.057(3) 0.076(4) 0.057(3) 0.018(3) 0.009(3) 0.009(3) C18 0.088(5) 0.106(5) 0.117(5) -0.024(4) -0.001(4) 0.024(4) C19 0.080(5) 0.159(6) 0.084(4) 0.020(4) -0.013(3) 0.039(4) C20 0.079(4) 0.085(5) 0.087(4) 0.004(3) 0.031(3) 0.031(3) C21 0.105(5) 0.109(5) 0.119(5) 0.009(4) -0.003(4) 0.045(4) C22 0.119(6) 0.077(5) 0.198(7) -0.018(5) -0.004(5) 0.009(4) C23 0.078(5) 0.132(5) 0.072(3) -0.001(3) -0.019(3) 0.017(4) C24 0.122(6) 0.104(5) 0.090(4) -0.006(3) 0.027(4) 0.041(4) C25 0.081(4) 0.059(3) 0.070(3) -0.003(2) -0.004(3) -0.002(3) C31 0.049(3) 0.065(3) 0.061(3) -0.001(2) -0.008(2) 0.008(2) C32 0.098(4) 0.099(4) 0.116(4) 0.026(3) 0.030(4) -0.001(4) C33 0.098(5) 0.061(4) 0.110(4) -0.003(3) -0.010(4) 0.019(3) C34 0.121(5) 0.082(4) 0.096(4) 0.005(3) -0.020(4) -0.023(3) C35 0.052(3) 0.092(4) 0.102(4) 0.026(3) -0.002(3) -0.017(3) C36 0.056(4) 0.094(4) 0.124(5) 0.011(3) 0.023(4) -0.018(3) C37 0.044(4) 0.090(4) 0.149(5) 0.022(4) -0.005(4) -0.012(2) C38 0.060(3) 0.119(5) 0.111(4) 0.027(4) -0.021(3) -0.019(3) _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 Y N1 2.285(3) . ? Y O1 2.367(3) . ? Y C31 2.371(4) . ? Y N2 2.385(3) . ? Y C25 2.403(4) . ? Si1 C25 1.797(4) . ? Si1 C23 1.860(4) . ? Si1 C24 1.874(5) . ? Si1 C8 1.904(5) . ? Si2 C31 1.821(4) . ? Si2 C32 1.843(5) . ? Si2 C34 1.854(5) . ? Si2 C33 1.886(5) . ? O1 C35 1.423(5) . ? O1 C38 1.455(5) . ? N1 C2 1.362(5) . ? N1 C11 1.436(4) . ? N2 C4 1.364(5) . ? N2 C8 1.381(5) . ? C1 C2 1.504(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.366(5) . ? C3 C4 1.416(6) . ? C3 H3 0.9300 . ? C4 C5 1.417(5) . ? C5 C6 1.360(6) . ? C5 H5 0.9300 . ? C6 C7 1.377(6) . ? C6 H6 0.9300 . ? C7 C8 1.383(6) . ? C7 H7 0.9300 . ? C11 C12 1.393(5) . ? C11 C16 1.403(5) . ? C12 C13 1.395(5) . ? C12 C17 1.522(6) . ? C13 C14 1.368(7) . ? C13 H13 0.9300 . ? C14 C15 1.344(7) . ? C14 H14 0.9300 . ? C15 C16 1.393(6) . ? C15 H15 0.9300 . ? C16 C20 1.514(7) . ? C17 C18 1.506(6) . ? C17 C19 1.523(6) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.512(7) . ? C20 C22 1.534(7) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.473(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.502(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.484(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? 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 N1 Y O1 105.57(10) . . ? N1 Y C31 119.90(12) . . ? O1 Y C31 90.79(13) . . ? N1 Y N2 79.30(11) . . ? O1 Y N2 166.69(10) . . ? C31 Y N2 97.49(13) . . ? N1 Y C25 123.51(13) . . ? O1 Y C25 88.25(14) . . ? C31 Y C25 114.20(14) . . ? N2 Y C25 78.87(14) . . ? C25 Si1 C23 111.3(2) . . ? C25 Si1 C24 118.6(2) . . ? C23 Si1 C24 107.0(2) . . ? C25 Si1 C8 104.86(19) . . ? C23 Si1 C8 108.5(2) . . ? C24 Si1 C8 106.2(2) . . ? C31 Si2 C32 111.2(2) . . ? C31 Si2 C34 110.7(2) . . ? C32 Si2 C34 108.6(3) . . ? C31 Si2 C33 113.2(2) . . ? C32 Si2 C33 106.6(2) . . ? C34 Si2 C33 106.3(2) . . ? C35 O1 C38 106.1(3) . . ? C35 O1 Y 129.0(3) . . ? C38 O1 Y 123.0(3) . . ? C2 N1 C11 118.9(3) . . ? C2 N1 Y 128.8(2) . . ? C11 N1 Y 111.9(2) . . ? C4 N2 C8 119.3(3) . . ? C4 N2 Y 123.6(3) . . ? C8 N2 Y 114.6(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.8(4) . . ? N1 C2 C1 119.1(4) . . ? C3 C2 C1 117.2(4) . . ? C2 C3 C4 132.0(4) . . ? C2 C3 H3 114.0 . . ? C4 C3 H3 114.0 . . ? N2 C4 C3 121.9(4) . . ? N2 C4 C5 119.9(4) . . ? C3 C4 C5 118.1(4) . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 119.9(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.0(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N2 C8 C7 120.6(4) . . ? N2 C8 Si1 117.1(3) . . ? C7 C8 Si1 122.1(4) . . ? C12 C11 C16 120.0(4) . . ? C12 C11 N1 120.5(3) . . ? C16 C11 N1 119.3(4) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 C17 122.0(4) . . ? C13 C12 C17 118.5(4) . . ? C14 C13 C12 120.1(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.4(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 122.3(5) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 117.7(4) . . ? C15 C16 C20 119.1(4) . . ? C11 C16 C20 123.2(4) . . ? C18 C17 C12 112.0(4) . . ? C18 C17 C19 110.2(4) . . ? C12 C17 C19 112.9(4) . . ? C18 C17 H17 107.1 . . ? C12 C17 H17 107.1 . . ? C19 C17 H17 107.1 . . ? 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 . . ? C21 C20 C16 113.5(5) . . ? C21 C20 C22 109.0(4) . . ? C16 C20 C22 111.5(5) . . ? C21 C20 H20 107.5 . . ? C16 C20 H20 107.5 . . ? C22 C20 H20 107.5 . . ? 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 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 Y 106.42(19) . . ? Si1 C25 H25A 110.4 . . ? Y C25 H25A 110.4 . . ? Si1 C25 H25B 110.4 . . ? Y C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? Si2 C31 Y 130.7(2) . . ? Si2 C31 H31A 104.6 . . ? Y C31 H31A 104.6 . . ? Si2 C31 H31B 104.6 . . ? Y C31 H31B 104.6 . . ? H31A C31 H31B 105.7 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O1 C35 C36 106.0(4) . . ? O1 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? O1 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C35 C36 C37 102.8(4) . . ? C35 C36 H36A 111.2 . . ? C37 C36 H36A 111.2 . . ? C35 C36 H36B 111.2 . . ? C37 C36 H36B 111.2 . . ? H36A C36 H36B 109.1 . . ? C38 C37 C36 103.7(4) . . ? C38 C37 H37A 111.0 . . ? C36 C37 H37A 111.0 . . ? C38 C37 H37B 111.0 . . ? C36 C37 H37B 111.0 . . ? H37A C37 H37B 109.0 . . ? O1 C38 C37 108.1(4) . . ? O1 C38 H38A 110.1 . . ? C37 C38 H38A 110.1 . . ? O1 C38 H38B 110.1 . . ? C37 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? 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 N1 Y O1 C35 44.7(4) . . . . ? C31 Y O1 C35 166.1(4) . . . . ? N2 Y O1 C35 -65.2(6) . . . . ? C25 Y O1 C35 -79.7(4) . . . . ? N1 Y O1 C38 -153.5(3) . . . . ? C31 Y O1 C38 -32.1(3) . . . . ? N2 Y O1 C38 96.5(5) . . . . ? C25 Y O1 C38 82.1(3) . . . . ? O1 Y N1 C2 169.0(3) . . . . ? C31 Y N1 C2 68.8(4) . . . . ? N2 Y N1 C2 -23.8(3) . . . . ? C25 Y N1 C2 -92.6(4) . . . . ? O1 Y N1 C11 -3.4(3) . . . . ? C31 Y N1 C11 -103.6(3) . . . . ? N2 Y N1 C11 163.9(3) . . . . ? C25 Y N1 C11 95.0(3) . . . . ? N1 Y N2 C4 34.0(3) . . . . ? O1 Y N2 C4 146.8(4) . . . . ? C31 Y N2 C4 -85.2(3) . . . . ? C25 Y N2 C4 161.6(3) . . . . ? N1 Y N2 C8 -164.1(3) . . . . ? O1 Y N2 C8 -51.3(6) . . . . ? C31 Y N2 C8 76.7(3) . . . . ? C25 Y N2 C8 -36.6(3) . . . . ? C11 N1 C2 C3 -179.6(4) . . . . ? Y N1 C2 C3 8.6(6) . . . . ? C11 N1 C2 C1 1.3(6) . . . . ? Y N1 C2 C1 -170.6(3) . . . . ? N1 C2 C3 C4 12.2(8) . . . . ? C1 C2 C3 C4 -168.6(5) . . . . ? C8 N2 C4 C3 168.2(4) . . . . ? Y N2 C4 C3 -30.7(5) . . . . ? C8 N2 C4 C5 -6.9(6) . . . . ? Y N2 C4 C5 154.2(3) . . . . ? C2 C3 C4 N2 1.0(8) . . . . ? C2 C3 C4 C5 176.2(5) . . . . ? N2 C4 C5 C6 3.8(7) . . . . ? C3 C4 C5 C6 -171.5(4) . . . . ? C4 C5 C6 C7 2.0(7) . . . . ? C5 C6 C7 C8 -4.7(7) . . . . ? C4 N2 C8 C7 4.2(6) . . . . ? Y N2 C8 C7 -158.5(3) . . . . ? C4 N2 C8 Si1 -171.9(3) . . . . ? Y N2 C8 Si1 25.4(4) . . . . ? C6 C7 C8 N2 1.6(7) . . . . ? C6 C7 C8 Si1 177.5(4) . . . . ? C25 Si1 C8 N2 6.0(4) . . . . ? C23 Si1 C8 N2 -112.9(3) . . . . ? C24 Si1 C8 N2 132.4(3) . . . . ? C25 Si1 C8 C7 -170.0(4) . . . . ? C23 Si1 C8 C7 71.0(4) . . . . ? C24 Si1 C8 C7 -43.6(4) . . . . ? C2 N1 C11 C12 89.9(5) . . . . ? Y N1 C11 C12 -96.9(3) . . . . ? C2 N1 C11 C16 -95.2(4) . . . . ? Y N1 C11 C16 78.0(4) . . . . ? C16 C11 C12 C13 -0.9(6) . . . . ? N1 C11 C12 C13 174.0(3) . . . . ? C16 C11 C12 C17 177.7(4) . . . . ? N1 C11 C12 C17 -7.4(6) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? C17 C12 C13 C14 -179.0(5) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 C16 0.1(9) . . . . ? C14 C15 C16 C11 -1.3(8) . . . . ? C14 C15 C16 C20 178.8(5) . . . . ? C12 C11 C16 C15 1.6(6) . . . . ? N1 C11 C16 C15 -173.2(4) . . . . ? C12 C11 C16 C20 -178.5(4) . . . . ? N1 C11 C16 C20 6.7(6) . . . . ? C11 C12 C17 C18 105.1(5) . . . . ? C13 C12 C17 C18 -76.3(5) . . . . ? C11 C12 C17 C19 -129.7(5) . . . . ? C13 C12 C17 C19 48.9(6) . . . . ? C15 C16 C20 C21 53.5(6) . . . . ? C11 C16 C20 C21 -126.4(5) . . . . ? C15 C16 C20 C22 -70.2(6) . . . . ? C11 C16 C20 C22 109.9(5) . . . . ? C23 Si1 C25 Y 84.5(3) . . . . ? C24 Si1 C25 Y -150.8(2) . . . . ? C8 Si1 C25 Y -32.5(2) . . . . ? N1 Y C25 Si1 105.1(2) . . . . ? O1 Y C25 Si1 -147.3(2) . . . . ? C31 Y C25 Si1 -57.2(3) . . . . ? N2 Y C25 Si1 36.0(2) . . . . ? C32 Si2 C31 Y -73.1(3) . . . . ? C34 Si2 C31 Y 47.7(4) . . . . ? C33 Si2 C31 Y 166.9(3) . . . . ? N1 Y C31 Si2 -46.3(3) . . . . ? O1 Y C31 Si2 -154.8(3) . . . . ? N2 Y C31 Si2 35.6(3) . . . . ? C25 Y C31 Si2 116.7(3) . . . . ? C38 O1 C35 C36 30.1(5) . . . . ? Y O1 C35 C36 -165.8(3) . . . . ? O1 C35 C36 C37 -37.2(5) . . . . ? C35 C36 C37 C38 29.3(5) . . . . ? C35 O1 C38 C37 -10.8(6) . . . . ? Y O1 C38 C37 -176.2(3) . . . . ? C36 C37 C38 O1 -12.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.506 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.051 #===END data_cd29458 _database_code_depnum_ccdc_archive 'CCDC 789699' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H47 N2 O Si Y' _chemical_formula_weight 616.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Y Y -2.7962 3.5667 '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 12.1821(11) _cell_length_b 13.4126(12) _cell_length_c 20.8185(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.134(2) _cell_angle_gamma 90.00 _cell_volume 3388.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2873 _cell_measurement_theta_min 4.523 _cell_measurement_theta_max 40.796 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.390 _exptl_crystal_size_min 0.351 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.783 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6429 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19537 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.1463 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7358 _reflns_number_gt 3157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7358 _refine_ls_number_parameters 401 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.853 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C18 C 0.6583(5) 1.2598(7) 0.6699(5) 0.193(5) Uani 0.749(11) 1 d PDU A 1 H18A H 0.6065 1.2065 0.6734 0.290 Uiso 0.749(11) 1 calc PR A 1 H18B H 0.6549 1.2824 0.6260 0.290 Uiso 0.749(11) 1 calc PR A 1 H18C H 0.6405 1.3139 0.6973 0.290 Uiso 0.749(11) 1 calc PR A 1 C19 C 0.8398(7) 1.3185(5) 0.6836(5) 0.137(3) Uani 0.749(11) 1 d PDU A 1 H19A H 0.8138 1.3511 0.6441 0.206 Uiso 0.749(11) 1 calc PR A 1 H19B H 0.9166 1.3029 0.6829 0.206 Uiso 0.749(11) 1 calc PR A 1 H19C H 0.8299 1.3618 0.7193 0.206 Uiso 0.749(11) 1 calc PR A 1 C18' C 0.6642(9) 1.2382(16) 0.7188(9) 0.086(7) Uani 0.251(11) 1 d PDU A 2 H18D H 0.6676 1.2977 0.7445 0.130 Uiso 0.251(11) 1 calc PR A 2 H18E H 0.6489 1.1821 0.7452 0.130 Uiso 0.251(11) 1 calc PR A 2 H18F H 0.6069 1.2447 0.6843 0.130 Uiso 0.251(11) 1 calc PR A 2 C19' C 0.8715(14) 1.2905(16) 0.7124(12) 0.105(9) Uani 0.251(11) 1 d PDU A 2 H19D H 0.8448 1.3488 0.7328 0.158 Uiso 0.251(11) 1 calc PR A 2 H19E H 0.9085 1.3101 0.6756 0.158 Uiso 0.251(11) 1 calc PR A 2 H19F H 0.9222 1.2556 0.7424 0.158 Uiso 0.251(11) 1 calc PR A 2 C32 C 0.6139(8) 0.7775(7) 0.9220(5) 0.140(4) Uani 0.749(11) 1 d PU A 1 H32A H 0.6126 0.8480 0.9297 0.210 Uiso 0.749(11) 1 calc PR A 1 H32B H 0.6101 0.7426 0.9620 0.210 Uiso 0.749(11) 1 calc PR A 1 H32C H 0.5518 0.7593 0.8926 0.210 Uiso 0.749(11) 1 calc PR A 1 C34 C 0.8624(8) 0.7944(7) 0.9368(4) 0.132(4) Uani 0.749(11) 1 d PU A 1 H34A H 0.9104 0.8296 0.9105 0.198 Uiso 0.749(11) 1 calc PR A 1 H34B H 0.9024 0.7412 0.9591 0.198 Uiso 0.749(11) 1 calc PR A 1 H34C H 0.8353 0.8394 0.9675 0.198 Uiso 0.749(11) 1 calc PR A 1 C32' C 0.6700(16) 0.8014(15) 0.9443(9) 0.056(6) Uani 0.251(11) 1 d PU A 2 H32D H 0.5957 0.8123 0.9263 0.085 Uiso 0.251(11) 1 calc PR A 2 H32E H 0.7035 0.8641 0.9566 0.085 Uiso 0.251(11) 1 calc PR A 2 H32F H 0.6697 0.7592 0.9815 0.085 Uiso 0.251(11) 1 calc PR A 2 C34' C 0.9069(14) 0.7608(16) 0.9145(10) 0.058(6) Uani 0.251(11) 1 d PU A 2 H34D H 0.9429 0.6971 0.9163 0.088 Uiso 0.251(11) 1 calc PR A 2 H34E H 0.9144 0.7909 0.9565 0.088 Uiso 0.251(11) 1 calc PR A 2 H34F H 0.9401 0.8031 0.8845 0.088 Uiso 0.251(11) 1 calc PR A 2 Y Y 0.70173(3) 0.95738(3) 0.769283(15) 0.04731(12) Uani 1 1 d . . . Si1 Si 0.74652(9) 0.74283(8) 0.88572(5) 0.0624(3) Uani 1 1 d . . . O1 O 0.58823(18) 0.91547(18) 0.67562(11) 0.0590(7) Uani 1 1 d . . . N1 N 0.8530(2) 1.0324(2) 0.73461(12) 0.0490(7) Uani 1 1 d . . . N2 N 0.7681(2) 1.0456(2) 0.86359(11) 0.0498(7) Uani 1 1 d . . . C1 C 1.0509(3) 1.0719(3) 0.73684(17) 0.0840(13) Uani 1 1 d . . . H1A H 1.0658 1.0176 0.7089 0.126 Uiso 1 1 calc R . . H1B H 1.1125 1.0811 0.7684 0.126 Uiso 1 1 calc R . . H1C H 1.0391 1.1317 0.7118 0.126 Uiso 1 1 calc R . . C2 C 0.9483(3) 1.0487(3) 0.77074(18) 0.0569(9) Uani 1 1 d . . . C3 C 0.9594(3) 1.0503(3) 0.83642(18) 0.0614(10) Uani 1 1 d . . . H3 H 1.0317 1.0473 0.8548 0.074 Uiso 1 1 calc R . . C4 C 0.8782(3) 1.0560(2) 0.88156(17) 0.0540(9) Uani 1 1 d . . . C5 C 0.9133(3) 1.0800(3) 0.94653(19) 0.0721(12) Uani 1 1 d . . . H5 H 0.9880 1.0859 0.9596 0.087 Uiso 1 1 calc R . . C6 C 0.8371(4) 1.0943(3) 0.98957(19) 0.0847(14) Uani 1 1 d . . . H6 H 0.8599 1.1087 1.0324 0.102 Uiso 1 1 calc R . . C7 C 0.7269(4) 1.0877(3) 0.97019(19) 0.0757(12) Uani 1 1 d . . . H7 H 0.6752 1.0989 0.9997 0.091 Uiso 1 1 calc R . . C8 C 0.6924(3) 1.0644(2) 0.90738(18) 0.0564(10) Uani 1 1 d . . . C11 C 0.8460(3) 1.0504(3) 0.66700(16) 0.0511(9) Uani 1 1 d . . . C12 C 0.8751(3) 0.9766(3) 0.62440(18) 0.0537(10) Uani 1 1 d . . . C13 C 0.8610(3) 0.9964(3) 0.5587(2) 0.0774(13) Uani 1 1 d . . . H13 H 0.8811 0.9485 0.5297 0.093 Uiso 1 1 calc R . . C14 C 0.8178(4) 1.0852(4) 0.5358(2) 0.0853(14) Uani 1 1 d . . . H14 H 0.8084 1.0968 0.4916 0.102 Uiso 1 1 calc R . . C15 C 0.7888(3) 1.1566(3) 0.5776(2) 0.0863(13) Uani 1 1 d . . . H15 H 0.7591 1.2164 0.5616 0.104 Uiso 1 1 calc R . . C16 C 0.8028(3) 1.1414(3) 0.6436(2) 0.0687(11) Uani 1 1 d . A . C17 C 0.7746(5) 1.2223(3) 0.6907(2) 0.1132(17) Uani 1 1 d DU . . H17 H 0.7812 1.1982 0.7354 0.136 Uiso 1 1 calc R A 1 C20 C 0.9198(3) 0.8758(3) 0.64624(17) 0.0678(11) Uani 1 1 d . . . H20 H 0.9335 0.8779 0.6933 0.081 Uiso 1 1 calc R . . C21 C 0.8356(3) 0.7929(3) 0.62938(17) 0.0856(13) Uani 1 1 d . . . H21A H 0.7714 0.8040 0.6520 0.128 Uiso 1 1 calc R . . H21B H 0.8676 0.7296 0.6418 0.128 Uiso 1 1 calc R . . H21C H 0.8150 0.7932 0.5838 0.128 Uiso 1 1 calc R . . C22 C 1.0292(3) 0.8496(3) 0.61904(19) 0.0994(14) Uani 1 1 d . . . H22A H 1.0174 0.8424 0.5731 0.149 Uiso 1 1 calc R . . H22B H 1.0570 0.7882 0.6377 0.149 Uiso 1 1 calc R . . H22C H 1.0817 0.9019 0.6293 0.149 Uiso 1 1 calc R . . C23 C 0.5755(3) 1.0586(3) 0.88165(18) 0.0565(10) Uani 1 1 d . . . C24 C 0.5496(3) 1.0305(2) 0.81750(18) 0.0543(9) Uani 1 1 d . . . C25 C 0.4376(3) 1.0320(3) 0.79604(19) 0.0728(11) Uani 1 1 d . . . H25 H 0.4167 1.0150 0.7534 0.087 Uiso 1 1 calc R . . C26 C 0.3566(3) 1.0575(3) 0.8354(3) 0.0903(14) Uani 1 1 d . . . H26 H 0.2831 1.0588 0.8190 0.108 Uiso 1 1 calc R . . C27 C 0.3849(4) 1.0810(3) 0.8985(3) 0.0923(15) Uani 1 1 d . . . H27 H 0.3305 1.0962 0.9256 0.111 Uiso 1 1 calc R . . C28 C 0.4932(4) 1.0819(3) 0.92176(19) 0.0794(13) Uani 1 1 d . . . H28 H 0.5124 1.0983 0.9647 0.095 Uiso 1 1 calc R . . C31 C 0.7376(3) 0.7925(2) 0.80480(15) 0.0738(11) Uani 1 1 d . A . H31A H 0.6821 0.7522 0.7807 0.089 Uiso 1 1 calc R . . H31B H 0.8071 0.7751 0.7884 0.089 Uiso 1 1 calc R . . C33 C 0.7458(3) 0.6045(3) 0.89055(17) 0.0979(14) Uani 1 1 d U A . H33A H 0.6958 0.5782 0.8564 0.147 Uiso 1 1 calc R . . H33B H 0.7224 0.5843 0.9314 0.147 Uiso 1 1 calc R . . H33C H 0.8186 0.5796 0.8863 0.147 Uiso 1 1 calc R . . C35 C 0.5633(3) 0.9681(4) 0.6154(2) 0.1054(16) Uani 1 1 d . . . H35A H 0.6300 0.9798 0.5944 0.126 Uiso 1 1 calc R . . H35B H 0.5290 1.0318 0.6229 0.126 Uiso 1 1 calc R . . C36 C 0.4871(4) 0.9035(4) 0.5754(2) 0.1144(18) Uani 1 1 d . . . H36A H 0.4365 0.9429 0.5472 0.137 Uiso 1 1 calc R . . H36B H 0.5273 0.8587 0.5494 0.137 Uiso 1 1 calc R . . C37 C 0.4275(4) 0.8473(3) 0.6222(3) 0.1120(17) Uani 1 1 d . . . H37A H 0.3997 0.7846 0.6041 0.134 Uiso 1 1 calc R . . H37B H 0.3666 0.8858 0.6362 0.134 Uiso 1 1 calc R . . C38 C 0.5152(3) 0.8304(3) 0.67670(19) 0.0843(13) Uani 1 1 d . . . H38A H 0.4828 0.8267 0.7175 0.101 Uiso 1 1 calc R . . H38B H 0.5548 0.7690 0.6703 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C18 0.210(7) 0.175(8) 0.210(9) -0.058(7) 0.099(6) 0.031(6) C19 0.169(6) 0.102(6) 0.135(7) -0.041(5) -0.016(5) 0.025(6) C18' 0.086(9) 0.098(9) 0.079(9) 0.003(6) 0.028(6) -0.001(6) C19' 0.114(11) 0.098(11) 0.102(11) -0.015(6) -0.002(7) 0.008(7) C32 0.140(7) 0.140(8) 0.148(7) 0.022(6) 0.064(6) 0.022(6) C34 0.159(8) 0.125(7) 0.101(6) 0.026(5) -0.052(5) -0.034(6) C32' 0.070(10) 0.055(9) 0.046(8) 0.006(7) 0.018(7) -0.006(7) C34' 0.052(9) 0.057(9) 0.065(9) 0.005(7) -0.001(7) -0.008(7) Y 0.0589(2) 0.0467(2) 0.0364(2) -0.00119(19) 0.00486(15) -0.0032(2) Si1 0.0831(8) 0.0561(8) 0.0477(7) 0.0067(5) 0.0044(6) -0.0060(6) O1 0.0629(16) 0.0627(18) 0.0505(16) 0.0027(13) -0.0001(13) -0.0090(13) N1 0.0590(18) 0.055(2) 0.0327(17) -0.0032(15) 0.0044(15) -0.0042(16) N2 0.068(2) 0.0456(18) 0.0358(17) -0.0027(15) 0.0027(16) -0.0023(18) C1 0.068(3) 0.103(4) 0.082(3) -0.002(2) 0.011(2) -0.020(2) C2 0.068(3) 0.052(2) 0.052(3) -0.001(2) 0.008(2) -0.004(2) C3 0.055(2) 0.071(3) 0.056(3) -0.006(2) -0.008(2) -0.005(2) C4 0.072(3) 0.046(3) 0.041(2) -0.0032(18) -0.007(2) 0.000(2) C5 0.086(3) 0.074(3) 0.052(3) -0.009(2) -0.018(3) -0.001(2) C6 0.123(4) 0.094(3) 0.033(3) -0.016(2) -0.015(3) 0.006(3) C7 0.100(4) 0.085(3) 0.041(3) -0.012(2) 0.001(3) 0.010(3) C8 0.082(3) 0.048(3) 0.039(2) -0.0042(18) 0.004(2) 0.007(2) C11 0.056(2) 0.051(3) 0.047(2) -0.002(2) 0.0115(19) -0.010(2) C12 0.065(2) 0.051(3) 0.047(3) 0.001(2) 0.015(2) -0.009(2) C13 0.107(3) 0.076(3) 0.051(3) -0.005(2) 0.018(3) -0.005(3) C14 0.120(4) 0.092(4) 0.046(3) 0.015(3) 0.023(3) -0.009(3) C15 0.120(4) 0.069(3) 0.072(3) 0.028(3) 0.020(3) 0.007(3) C16 0.100(3) 0.046(3) 0.063(3) 0.005(2) 0.028(3) -0.003(2) C17 0.188(5) 0.060(4) 0.097(4) 0.025(3) 0.039(4) 0.033(4) C20 0.081(3) 0.069(3) 0.055(3) -0.011(2) 0.018(2) 0.008(3) C21 0.106(3) 0.061(3) 0.094(3) -0.005(2) 0.031(3) 0.001(3) C22 0.092(3) 0.088(4) 0.122(4) -0.011(3) 0.033(3) 0.013(3) C23 0.075(3) 0.047(3) 0.049(3) 0.0042(19) 0.019(2) 0.009(2) C24 0.059(3) 0.046(2) 0.058(3) -0.0019(19) 0.006(2) 0.005(2) C25 0.068(3) 0.074(3) 0.076(3) -0.006(2) 0.006(3) 0.008(3) C26 0.060(3) 0.088(4) 0.124(4) -0.001(3) 0.017(3) 0.010(3) C27 0.095(4) 0.094(4) 0.096(4) 0.002(3) 0.046(3) 0.021(3) C28 0.092(3) 0.084(3) 0.065(3) 0.007(2) 0.023(3) 0.020(3) C31 0.112(3) 0.050(3) 0.059(3) 0.0025(19) 0.008(2) 0.006(2) C33 0.137(3) 0.073(3) 0.083(3) 0.018(2) 0.006(3) -0.006(3) C35 0.089(3) 0.142(5) 0.081(3) 0.045(3) -0.017(3) -0.018(3) C36 0.110(4) 0.168(6) 0.059(3) -0.005(3) -0.023(3) 0.000(4) C37 0.100(4) 0.081(4) 0.145(5) -0.011(3) -0.046(4) -0.009(3) C38 0.087(3) 0.070(3) 0.093(3) 0.001(2) -0.006(3) -0.016(3) _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 C18 C17 1.5296(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C17 1.5287(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C18' C17 1.5286(11) . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' C17 1.5295(11) . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C32 Si1 1.902(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C34 Si1 1.825(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C32' Si1 1.782(18) . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? C34' Si1 2.006(17) . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? Y N1 2.273(3) . ? Y O1 2.355(2) . ? Y C31 2.360(3) . ? Y N2 2.371(3) . ? Y C24 2.396(3) . ? Si1 C31 1.806(3) . ? Si1 C33 1.858(4) . ? O1 C35 1.446(4) . ? O1 C38 1.448(4) . ? N1 C2 1.344(4) . ? N1 C11 1.423(4) . ? N2 C4 1.367(4) . ? N2 C8 1.377(4) . ? C1 C2 1.521(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.362(4) . ? C3 C4 1.426(4) . ? C3 H3 0.9300 . ? C4 C5 1.418(4) . ? C5 C6 1.361(5) . ? C5 H5 0.9300 . ? C6 C7 1.369(5) . ? C6 H6 0.9300 . ? C7 C8 1.373(4) . ? C7 H7 0.9300 . ? C8 C23 1.478(4) . ? C11 C12 1.396(4) . ? C11 C16 1.399(5) . ? C12 C13 1.388(4) . ? C12 C20 1.513(5) . ? C13 C14 1.370(5) . ? C13 H13 0.9300 . ? C14 C15 1.361(5) . ? C14 H14 0.9300 . ? C15 C16 1.385(5) . ? C15 H15 0.9300 . ? C16 C17 1.522(5) . ? C17 H17 0.9800 . ? C20 C21 1.532(4) . ? C20 C22 1.535(4) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.396(4) . ? C23 C28 1.397(4) . ? C24 C25 1.397(4) . ? C25 C26 1.382(5) . ? C25 H25 0.9300 . ? C26 C27 1.364(5) . ? C26 H26 0.9300 . ? C27 C28 1.364(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C35 C36 1.473(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.472(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.504(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? 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 C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17 C19' H19D 109.5 . . ? C17 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? Si1 C32' H32D 109.5 . . ? Si1 C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? Si1 C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? Si1 C34' H34D 109.5 . . ? Si1 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? Si1 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? N1 Y O1 105.97(9) . . ? N1 Y C31 112.41(11) . . ? O1 Y C31 96.57(10) . . ? N1 Y N2 79.41(10) . . ? O1 Y N2 159.38(9) . . ? C31 Y N2 99.67(10) . . ? N1 Y C24 129.16(10) . . ? O1 Y C24 91.48(11) . . ? C31 Y C24 112.40(12) . . ? N2 Y C24 70.62(11) . . ? C32' Si1 C31 119.0(6) . . ? C32' Si1 C34 81.9(6) . . ? C31 Si1 C34 112.5(3) . . ? C32' Si1 C33 113.4(7) . . ? C31 Si1 C33 114.76(16) . . ? C34 Si1 C33 110.7(3) . . ? C32' Si1 C32 26.5(6) . . ? C31 Si1 C32 107.3(3) . . ? C34 Si1 C32 108.5(3) . . ? C33 Si1 C32 102.4(3) . . ? C32' Si1 C34' 107.3(7) . . ? C31 Si1 C34' 102.1(7) . . ? C34 Si1 C34' 25.7(5) . . ? C33 Si1 C34' 96.5(7) . . ? C32 Si1 C34' 133.8(6) . . ? C35 O1 C38 108.4(3) . . ? C35 O1 Y 131.5(3) . . ? C38 O1 Y 119.4(2) . . ? C2 N1 C11 119.9(3) . . ? C2 N1 Y 125.4(2) . . ? C11 N1 Y 114.3(2) . . ? C4 N2 C8 119.9(3) . . ? C4 N2 Y 122.1(2) . . ? C8 N2 Y 116.2(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.6(3) . . ? N1 C2 C1 118.6(3) . . ? C3 C2 C1 116.8(3) . . ? C2 C3 C4 130.6(3) . . ? C2 C3 H3 114.7 . . ? C4 C3 H3 114.7 . . ? N2 C4 C5 119.2(3) . . ? N2 C4 C3 122.4(3) . . ? C5 C4 C3 118.2(4) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.4(4) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 N2 120.5(4) . . ? C7 C8 C23 124.0(4) . . ? N2 C8 C23 115.5(3) . . ? C12 C11 C16 120.5(3) . . ? C12 C11 N1 120.8(3) . . ? C16 C11 N1 118.7(3) . . ? C13 C12 C11 118.3(3) . . ? C13 C12 C20 118.5(3) . . ? C11 C12 C20 123.2(3) . . ? C14 C13 C12 121.3(4) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 121.0(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 118.8(4) . . ? C15 C16 C17 121.3(4) . . ? C11 C16 C17 119.8(4) . . ? C16 C17 C18' 127.0(9) . . ? C16 C17 C19 113.0(5) . . ? C18' C17 C19 113.7(9) . . ? C16 C17 C19' 113.8(10) . . ? C18' C17 C19' 119.1(13) . . ? C19 C17 C19' 29.5(10) . . ? C16 C17 C18 107.9(5) . . ? C18' C17 C18 40.3(6) . . ? C19 C17 C18 99.9(6) . . ? C19' C17 C18 123.9(11) . . ? C16 C17 H17 111.8 . . ? C18' C17 H17 71.5 . . ? C19 C17 H17 111.8 . . ? C19' C17 H17 85.6 . . ? C18 C17 H17 111.8 . . ? C12 C20 C21 111.3(3) . . ? C12 C20 C22 113.3(3) . . ? C21 C20 C22 109.6(3) . . ? C12 C20 H20 107.5 . . ? C21 C20 H20 107.5 . . ? C22 C20 H20 107.5 . . ? 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 . . ? C24 C23 C28 121.3(4) . . ? C24 C23 C8 119.3(3) . . ? C28 C23 C8 119.4(4) . . ? C23 C24 C25 115.7(3) . . ? C23 C24 Y 113.2(3) . . ? C25 C24 Y 129.9(3) . . ? C26 C25 C24 122.9(4) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 119.8(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C23 120.6(4) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? Si1 C31 Y 129.20(17) . . ? Si1 C31 H31A 105.0 . . ? Y C31 H31A 105.0 . . ? Si1 C31 H31B 105.0 . . ? Y C31 H31B 105.0 . . ? H31A C31 H31B 105.8 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O1 C35 C36 106.0(4) . . ? O1 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? O1 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C37 C36 C35 104.5(4) . . ? C37 C36 H36A 110.8 . . ? C35 C36 H36A 110.9 . . ? C37 C36 H36B 110.8 . . ? C35 C36 H36B 110.8 . . ? H36A C36 H36B 108.9 . . ? C36 C37 C38 102.5(4) . . ? C36 C37 H37A 111.3 . . ? C38 C37 H37A 111.3 . . ? C36 C37 H37B 111.3 . . ? C38 C37 H37B 111.3 . . ? H37A C37 H37B 109.2 . . ? O1 C38 C37 105.4(3) . . ? O1 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? O1 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? 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 N1 Y O1 C35 -38.9(3) . . . . ? C31 Y O1 C35 -154.5(3) . . . . ? N2 Y O1 C35 63.7(4) . . . . ? C24 Y O1 C35 92.7(3) . . . . ? N1 Y O1 C38 151.4(2) . . . . ? C31 Y O1 C38 35.8(2) . . . . ? N2 Y O1 C38 -106.0(3) . . . . ? C24 Y O1 C38 -77.0(2) . . . . ? O1 Y N1 C2 -164.9(3) . . . . ? C31 Y N1 C2 -60.6(3) . . . . ? N2 Y N1 C2 35.6(3) . . . . ? C24 Y N1 C2 89.6(3) . . . . ? O1 Y N1 C11 7.0(2) . . . . ? C31 Y N1 C11 111.3(2) . . . . ? N2 Y N1 C11 -152.6(2) . . . . ? C24 Y N1 C11 -98.5(3) . . . . ? N1 Y N2 C4 -37.1(2) . . . . ? O1 Y N2 C4 -144.4(3) . . . . ? C31 Y N2 C4 74.1(3) . . . . ? C24 Y N2 C4 -175.4(3) . . . . ? N1 Y N2 C8 158.3(2) . . . . ? O1 Y N2 C8 51.0(4) . . . . ? C31 Y N2 C8 -90.5(2) . . . . ? C24 Y N2 C8 20.0(2) . . . . ? C11 N1 C2 C3 168.3(3) . . . . ? Y N1 C2 C3 -20.3(5) . . . . ? C11 N1 C2 C1 -8.6(5) . . . . ? Y N1 C2 C1 162.8(2) . . . . ? N1 C2 C3 C4 -13.9(6) . . . . ? C1 C2 C3 C4 163.0(4) . . . . ? C8 N2 C4 C5 4.1(5) . . . . ? Y N2 C4 C5 -159.9(2) . . . . ? C8 N2 C4 C3 -171.6(3) . . . . ? Y N2 C4 C3 24.4(4) . . . . ? C2 C3 C4 N2 10.3(6) . . . . ? C2 C3 C4 C5 -165.4(4) . . . . ? N2 C4 C5 C6 -1.4(5) . . . . ? C3 C4 C5 C6 174.4(4) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? C5 C6 C7 C8 1.3(6) . . . . ? C6 C7 C8 N2 1.4(5) . . . . ? C6 C7 C8 C23 -178.1(4) . . . . ? C4 N2 C8 C7 -4.1(5) . . . . ? Y N2 C8 C7 160.8(3) . . . . ? C4 N2 C8 C23 175.4(3) . . . . ? Y N2 C8 C23 -19.7(4) . . . . ? C2 N1 C11 C12 86.9(4) . . . . ? Y N1 C11 C12 -85.4(3) . . . . ? C2 N1 C11 C16 -97.0(4) . . . . ? Y N1 C11 C16 90.6(3) . . . . ? C16 C11 C12 C13 0.6(5) . . . . ? N1 C11 C12 C13 176.6(3) . . . . ? C16 C11 C12 C20 -178.6(3) . . . . ? N1 C11 C12 C20 -2.6(5) . . . . ? C11 C12 C13 C14 -1.1(6) . . . . ? C20 C12 C13 C14 178.1(4) . . . . ? C12 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C16 0.5(7) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? C14 C15 C16 C17 177.6(4) . . . . ? C12 C11 C16 C15 0.4(5) . . . . ? N1 C11 C16 C15 -175.6(3) . . . . ? C12 C11 C16 C17 -178.2(4) . . . . ? N1 C11 C16 C17 5.8(5) . . . . ? C15 C16 C17 C18' 91.0(11) . . . . ? C11 C16 C17 C18' -90.5(11) . . . . ? C15 C16 C17 C19 -59.1(7) . . . . ? C11 C16 C17 C19 119.5(6) . . . . ? C15 C16 C17 C19' -91.3(12) . . . . ? C11 C16 C17 C19' 87.3(12) . . . . ? C15 C16 C17 C18 50.4(7) . . . . ? C11 C16 C17 C18 -131.1(6) . . . . ? C13 C12 C20 C21 -69.9(4) . . . . ? C11 C12 C20 C21 109.3(4) . . . . ? C13 C12 C20 C22 54.2(5) . . . . ? C11 C12 C20 C22 -126.7(4) . . . . ? C7 C8 C23 C24 -177.6(3) . . . . ? N2 C8 C23 C24 2.9(5) . . . . ? C7 C8 C23 C28 3.0(5) . . . . ? N2 C8 C23 C28 -176.5(3) . . . . ? C28 C23 C24 C25 2.7(5) . . . . ? C8 C23 C24 C25 -176.7(3) . . . . ? C28 C23 C24 Y -165.8(3) . . . . ? C8 C23 C24 Y 14.7(4) . . . . ? N1 Y C24 C23 -75.0(3) . . . . ? O1 Y C24 C23 172.9(2) . . . . ? C31 Y C24 C23 75.2(3) . . . . ? N2 Y C24 C23 -17.5(2) . . . . ? N1 Y C24 C25 118.4(3) . . . . ? O1 Y C24 C25 6.4(3) . . . . ? C31 Y C24 C25 -91.4(3) . . . . ? N2 Y C24 C25 175.9(4) . . . . ? C23 C24 C25 C26 -1.1(6) . . . . ? Y C24 C25 C26 165.1(3) . . . . ? C24 C25 C26 C27 -1.2(6) . . . . ? C25 C26 C27 C28 2.0(7) . . . . ? C26 C27 C28 C23 -0.4(6) . . . . ? C24 C23 C28 C27 -2.1(6) . . . . ? C8 C23 C28 C27 177.4(4) . . . . ? C32' Si1 C31 Y 28.1(8) . . . . ? C34 Si1 C31 Y -65.0(5) . . . . ? C33 Si1 C31 Y 167.2(2) . . . . ? C32 Si1 C31 Y 54.2(4) . . . . ? C34' Si1 C31 Y -89.7(6) . . . . ? N1 Y C31 Si1 109.2(2) . . . . ? O1 Y C31 Si1 -140.5(2) . . . . ? N2 Y C31 Si1 26.8(3) . . . . ? C24 Y C31 Si1 -46.1(3) . . . . ? C38 O1 C35 C36 -9.6(4) . . . . ? Y O1 C35 C36 179.8(2) . . . . ? O1 C35 C36 C37 29.0(5) . . . . ? C35 C36 C37 C38 -36.3(5) . . . . ? C35 O1 C38 C37 -13.1(4) . . . . ? Y O1 C38 C37 158.8(2) . . . . ? C36 C37 C38 O1 30.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.618 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.052 #===END data_cd201356 _database_code_depnum_ccdc_archive 'CCDC 789700' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 N3 O Y' _chemical_formula_weight 705.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6805(11) _cell_length_b 17.3700(19) _cell_length_c 11.7004(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.877(2) _cell_angle_gamma 90.00 _cell_volume 1943.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2128 _cell_measurement_theta_min 4.862 _cell_measurement_theta_max 40.462 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.307 _exptl_crystal_size_mid 0.269 _exptl_crystal_size_min 0.253 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.34768 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10141 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.1294 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6841 _reflns_number_gt 4156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(7) _refine_ls_number_reflns 6841 _refine_ls_number_parameters 448 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C40 C 0.417(3) 0.7989(13) 0.270(2) 0.100(6) Uani 0.70(5) 1 d PU A 1 H40A H 0.3920 0.8503 0.2443 0.149 Uiso 0.70(5) 1 calc PR A 1 H40B H 0.3963 0.7640 0.2059 0.149 Uiso 0.70(5) 1 calc PR A 1 H40C H 0.5147 0.7968 0.2999 0.149 Uiso 0.70(5) 1 calc PR A 1 C40' C 0.478(5) 0.775(2) 0.314(4) 0.076(12) Uani 0.30(5) 1 d PU A 2 H40D H 0.4655 0.7496 0.2403 0.115 Uiso 0.30(5) 1 calc PR A 2 H40E H 0.5464 0.7483 0.3672 0.115 Uiso 0.30(5) 1 calc PR A 2 H40F H 0.5088 0.8271 0.3047 0.115 Uiso 0.30(5) 1 calc PR A 2 Y1 Y 0.03270(4) 0.99918(3) 0.25446(4) 0.04248(15) Uani 1 1 d . . . N1 N 0.0045(4) 0.9342(2) 0.0831(4) 0.0429(11) Uani 1 1 d . . . N2 N 0.1914(4) 1.0675(3) 0.1581(4) 0.0450(11) Uani 1 1 d . . . N3 N 0.1848(5) 0.9234(3) 0.3584(5) 0.0516(13) Uani 1 1 d . . . O1 O -0.1812(3) 0.9817(2) 0.3234(3) 0.0536(12) Uani 1 1 d . . . C1 C 0.0938(7) 0.8514(4) -0.0593(6) 0.078(2) Uani 1 1 d . . . H1A H 0.0779 0.8049 -0.0189 0.117 Uiso 1 1 calc R . . H1B H 0.1774 0.8461 -0.0934 0.117 Uiso 1 1 calc R . . H1C H 0.0158 0.8608 -0.1189 0.117 Uiso 1 1 calc R . . C2 C 0.1102(6) 0.9183(3) 0.0249(5) 0.0554(16) Uani 1 1 d . . . C3 C 0.2335(7) 0.9597(4) 0.0357(6) 0.058(2) Uani 1 1 d . . . H3 H 0.3041 0.9361 0.0029 0.070 Uiso 1 1 calc R . . C4 C 0.2707(6) 1.0308(4) 0.0873(6) 0.0471(17) Uani 1 1 d . . . C5 C 0.3916(6) 1.0675(4) 0.0627(6) 0.071(2) Uani 1 1 d . . . H5 H 0.4491 1.0419 0.0184 0.085 Uiso 1 1 calc R . . C6 C 0.4264(7) 1.1384(4) 0.1012(7) 0.079(2) Uani 1 1 d . . . H6 H 0.5062 1.1620 0.0824 0.095 Uiso 1 1 calc R . . C7 C 0.3432(7) 1.1766(4) 0.1691(7) 0.075(2) Uani 1 1 d . . . H7 H 0.3681 1.2254 0.1979 0.090 Uiso 1 1 calc R . . C8 C 0.2244(6) 1.1421(3) 0.1933(5) 0.0554(16) Uani 1 1 d . . . C11 C -0.1322(5) 0.9031(3) 0.0466(4) 0.0394(13) Uani 1 1 d . . . C12 C -0.2268(6) 0.9458(4) -0.0300(5) 0.0470(17) Uani 1 1 d . . . C13 C -0.3638(6) 0.9203(4) -0.0538(5) 0.0551(17) Uani 1 1 d . . . H13 H -0.4276 0.9485 -0.1050 0.066 Uiso 1 1 calc R . . C14 C -0.4090(6) 0.8550(3) -0.0046(5) 0.0563(16) Uani 1 1 d . . . H14 H -0.5021 0.8397 -0.0210 0.068 Uiso 1 1 calc R . . C15 C -0.3145(6) 0.8127(3) 0.0692(5) 0.0551(16) Uani 1 1 d . . . H15 H -0.3447 0.7684 0.1025 0.066 Uiso 1 1 calc R . . C16 C -0.1747(6) 0.8342(3) 0.0958(5) 0.0487(15) Uani 1 1 d . . . C17 C -0.0737(6) 0.7815(3) 0.1709(5) 0.0592(17) Uani 1 1 d . . . H17 H 0.0201 0.8035 0.1754 0.071 Uiso 1 1 calc R . . C18 C -0.1091(8) 0.7781(4) 0.2946(6) 0.084(2) Uani 1 1 d . . . H18A H -0.0884 0.8268 0.3320 0.126 Uiso 1 1 calc R . . H18B H -0.0544 0.7385 0.3374 0.126 Uiso 1 1 calc R . . H18C H -0.2067 0.7667 0.2915 0.126 Uiso 1 1 calc R . . C19 C -0.0703(7) 0.7010(4) 0.1200(7) 0.091(2) Uani 1 1 d . . . H19A H -0.1588 0.6762 0.1210 0.137 Uiso 1 1 calc R . . H19B H 0.0023 0.6715 0.1652 0.137 Uiso 1 1 calc R . . H19C H -0.0522 0.7045 0.0418 0.137 Uiso 1 1 calc R . . C20 C -0.1832(6) 1.0167(3) -0.0884(5) 0.057(2) Uani 1 1 d . . . H20 H -0.0821 1.0222 -0.0650 0.068 Uiso 1 1 calc R . . C21 C -0.2497(10) 1.0891(4) -0.0524(7) 0.096(3) Uani 1 1 d . . . H21A H -0.3495 1.0851 -0.0714 0.144 Uiso 1 1 calc R . . H21B H -0.2177 1.1323 -0.0924 0.144 Uiso 1 1 calc R . . H21C H -0.2243 1.0963 0.0295 0.144 Uiso 1 1 calc R . . C22 C -0.2093(7) 1.0080(6) -0.2198(5) 0.098(2) Uani 1 1 d . . . H22A H -0.1542 0.9661 -0.2418 0.147 Uiso 1 1 calc R . . H22B H -0.1834 1.0547 -0.2549 0.147 Uiso 1 1 calc R . . H22C H -0.3066 0.9976 -0.2453 0.147 Uiso 1 1 calc R . . C23 C 0.1243(6) 1.1788(3) 0.2607(5) 0.0540(16) Uani 1 1 d . . . C24 C 0.0123(6) 1.1359(3) 0.2897(5) 0.0550(16) Uani 1 1 d . . . C25 C -0.0786(8) 1.1746(4) 0.3514(7) 0.075(2) Uani 1 1 d . . . H25 H -0.1513 1.1474 0.3760 0.090 Uiso 1 1 calc R . . C26 C -0.0642(9) 1.2526(4) 0.3773(6) 0.082(2) Uani 1 1 d . . . H26 H -0.1306 1.2777 0.4134 0.099 Uiso 1 1 calc R . . C27 C 0.0468(9) 1.2920(4) 0.3496(7) 0.086(2) Uani 1 1 d . . . H27 H 0.0587 1.3436 0.3703 0.103 Uiso 1 1 calc R . . C28 C 0.1416(7) 1.2566(4) 0.2916(6) 0.075(2) Uani 1 1 d . . . H28 H 0.2174 1.2841 0.2727 0.090 Uiso 1 1 calc R . . C29 C 0.2712(6) 0.9008(3) 0.4569(5) 0.0424(15) Uani 1 1 d . . . C30 C 0.3477(6) 0.8311(3) 0.4636(5) 0.0473(14) Uani 1 1 d . A . C31 C 0.4366(6) 0.8140(4) 0.5642(6) 0.0685(19) Uani 1 1 d . . . H31 H 0.4911 0.7698 0.5667 0.082 Uiso 1 1 calc R . . C32 C 0.4475(8) 0.8589(5) 0.6588(6) 0.098(3) Uani 1 1 d . . . H32 H 0.5061 0.8449 0.7262 0.118 Uiso 1 1 calc R . . C33 C 0.3689(7) 0.9270(4) 0.6542(6) 0.076(2) Uani 1 1 d . . . H33 H 0.3758 0.9586 0.7190 0.091 Uiso 1 1 calc R . . C34 C 0.2823(7) 0.9474(4) 0.5552(6) 0.0530(18) Uani 1 1 d . . . C35 C 0.2037(7) 1.0241(3) 0.5543(6) 0.063(2) Uani 1 1 d . . . H35 H 0.1266 1.0210 0.4894 0.076 Uiso 1 1 calc R . . C36 C 0.2893(9) 1.0890(4) 0.5294(8) 0.097(3) Uani 1 1 d . . . H36A H 0.3691 1.0932 0.5889 0.145 Uiso 1 1 calc R . . H36B H 0.2353 1.1355 0.5267 0.145 Uiso 1 1 calc R . . H36C H 0.3201 1.0811 0.4561 0.145 Uiso 1 1 calc R . . C37 C 0.1364(8) 1.0370(4) 0.6617(7) 0.111(3) Uani 1 1 d . . . H37A H 0.2075 1.0483 0.7262 0.167 Uiso 1 1 calc R . . H37B H 0.0868 0.9914 0.6779 0.167 Uiso 1 1 calc R . . H37C H 0.0723 1.0795 0.6489 0.167 Uiso 1 1 calc R . . C38 C 0.3347(7) 0.7766(3) 0.3621(6) 0.0625(18) Uani 1 1 d . . . H38 H 0.2376 0.7834 0.3250 0.075 Uiso 1 1 calc R A 1 C39 C 0.3407(10) 0.6917(4) 0.3979(8) 0.126(3) Uani 1 1 d . A . H39A H 0.3071 0.6603 0.3319 0.189 Uiso 1 1 calc R . . H39B H 0.2832 0.6838 0.4567 0.189 Uiso 1 1 calc R . . H39C H 0.4355 0.6779 0.4275 0.189 Uiso 1 1 calc R . . C41 C -0.3163(5) 0.9992(7) 0.2602(5) 0.0799(18) Uani 1 1 d . . . H41A H -0.3481 0.9573 0.2080 0.096 Uiso 1 1 calc R . . H41B H -0.3115 1.0456 0.2148 0.096 Uiso 1 1 calc R . . C42 C -0.4139(6) 1.0105(7) 0.3431(6) 0.105(3) Uani 1 1 d . . . H42A H -0.4308 1.0648 0.3543 0.127 Uiso 1 1 calc R . . H42B H -0.5024 0.9851 0.3169 0.127 Uiso 1 1 calc R . . C43 C -0.3427(8) 0.9754(7) 0.4497(7) 0.127(5) Uani 1 1 d . . . H43A H -0.3560 1.0067 0.5158 0.152 Uiso 1 1 calc R . . H43B H -0.3805 0.9245 0.4595 0.152 Uiso 1 1 calc R . . C44 C -0.1983(7) 0.9702(5) 0.4413(6) 0.097(3) Uani 1 1 d . . . H44A H -0.1627 0.9200 0.4674 0.116 Uiso 1 1 calc R . . H44B H -0.1465 1.0090 0.4899 0.116 Uiso 1 1 calc R . . H3A H 0.183(7) 0.896(4) 0.302(6) 0.09(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C40 0.094(10) 0.119(9) 0.090(10) -0.024(7) 0.024(7) -0.001(7) C40' 0.085(15) 0.071(14) 0.076(14) 0.000(9) 0.023(9) -0.001(9) Y1 0.0408(2) 0.0392(3) 0.0473(3) 0.0019(4) 0.00668(19) 0.0039(5) N1 0.035(3) 0.051(3) 0.042(3) 0.000(2) 0.002(2) -0.003(2) N2 0.040(3) 0.044(3) 0.049(3) 0.003(2) 0.002(2) -0.007(2) N3 0.060(3) 0.050(3) 0.040(3) -0.006(3) -0.007(3) 0.011(2) O1 0.046(2) 0.069(4) 0.048(2) 0.007(2) 0.0129(17) 0.003(2) C1 0.078(5) 0.086(5) 0.075(5) -0.033(4) 0.030(4) -0.011(4) C2 0.045(4) 0.057(4) 0.064(4) -0.003(3) 0.006(3) 0.008(3) C3 0.046(4) 0.064(4) 0.067(5) -0.010(4) 0.019(3) 0.002(3) C4 0.035(3) 0.046(4) 0.062(5) 0.004(3) 0.010(3) 0.005(3) C5 0.049(4) 0.063(5) 0.106(6) 0.003(4) 0.031(4) 0.002(4) C6 0.063(5) 0.062(5) 0.118(7) 0.013(5) 0.033(4) -0.011(4) C7 0.070(5) 0.051(4) 0.103(6) 0.006(4) 0.012(4) -0.022(4) C8 0.050(4) 0.045(4) 0.068(5) 0.013(3) 0.001(3) 0.003(3) C11 0.044(3) 0.040(3) 0.032(3) -0.001(3) 0.001(2) -0.002(3) C12 0.041(4) 0.054(4) 0.043(4) -0.009(3) -0.001(3) -0.002(3) C13 0.050(4) 0.065(5) 0.048(4) -0.003(3) 0.001(3) 0.007(4) C14 0.043(4) 0.053(4) 0.072(5) -0.013(4) 0.007(3) -0.005(3) C15 0.052(4) 0.053(4) 0.061(4) 0.008(3) 0.009(3) -0.009(3) C16 0.046(4) 0.045(4) 0.054(4) -0.003(3) 0.003(3) -0.001(3) C17 0.063(4) 0.057(4) 0.054(5) 0.014(3) -0.004(3) -0.006(3) C18 0.103(6) 0.068(5) 0.075(6) 0.015(4) -0.004(5) 0.004(4) C19 0.100(6) 0.062(5) 0.111(7) 0.011(5) 0.013(5) 0.029(4) C20 0.049(3) 0.063(6) 0.058(4) 0.019(4) 0.008(3) 0.004(3) C21 0.129(8) 0.064(6) 0.110(7) 0.010(5) 0.061(6) -0.003(5) C22 0.138(6) 0.104(6) 0.059(5) 0.009(6) 0.035(4) -0.005(7) C23 0.055(4) 0.042(4) 0.061(4) 0.009(3) -0.002(3) 0.003(3) C24 0.060(4) 0.035(3) 0.072(5) -0.006(3) 0.014(3) 0.011(3) C25 0.084(5) 0.056(5) 0.090(6) 0.000(4) 0.028(4) 0.013(4) C26 0.113(7) 0.054(5) 0.082(6) -0.014(4) 0.020(5) 0.018(5) C27 0.125(7) 0.049(5) 0.080(6) -0.005(4) 0.008(5) 0.013(5) C28 0.085(5) 0.042(4) 0.097(6) 0.002(4) 0.011(4) -0.009(4) C29 0.039(3) 0.048(4) 0.039(4) 0.001(3) 0.004(3) -0.008(3) C30 0.052(4) 0.041(3) 0.045(4) -0.001(3) -0.001(3) 0.006(3) C31 0.077(5) 0.055(4) 0.069(5) -0.004(4) -0.003(4) 0.018(4) C32 0.114(6) 0.110(7) 0.056(5) -0.008(5) -0.032(4) 0.038(5) C33 0.093(5) 0.077(5) 0.050(5) -0.014(4) -0.011(4) 0.026(4) C34 0.054(4) 0.054(5) 0.050(5) -0.003(4) 0.007(3) 0.001(4) C35 0.060(4) 0.075(6) 0.053(4) -0.020(3) 0.002(3) 0.013(4) C36 0.095(7) 0.061(6) 0.135(9) 0.007(6) 0.016(6) -0.005(5) C37 0.135(7) 0.092(6) 0.118(8) -0.021(5) 0.058(6) 0.024(5) C38 0.068(4) 0.051(4) 0.065(5) -0.010(3) 0.000(3) 0.020(3) C39 0.209(10) 0.047(5) 0.121(8) -0.016(5) 0.026(7) 0.010(5) C41 0.051(3) 0.123(5) 0.067(4) -0.026(7) 0.012(3) 0.005(7) C42 0.056(4) 0.184(10) 0.079(5) -0.023(7) 0.018(4) 0.001(7) C43 0.080(5) 0.227(14) 0.083(6) 0.009(7) 0.039(4) -0.034(7) C44 0.093(5) 0.142(9) 0.055(5) 0.024(4) 0.013(4) 0.011(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 C40 C38 1.485(15) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C40' C38 1.57(3) . ? C40' H40D 0.9600 . ? C40' H40E 0.9600 . ? C40' H40F 0.9600 . ? Y1 N3 2.197(5) . ? Y1 N1 2.281(4) . ? Y1 O1 2.355(3) . ? Y1 N2 2.361(4) . ? Y1 C24 2.424(6) . ? Y1 H3A 2.32(7) . ? N1 C2 1.342(6) . ? N1 C11 1.432(6) . ? N2 C4 1.371(7) . ? N2 C8 1.382(7) . ? N3 C29 1.373(7) . ? N3 H3A 0.81(6) . ? O1 C44 1.429(7) . ? O1 C41 1.432(6) . ? C1 C2 1.516(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.383(8) . ? C3 C4 1.397(7) . ? C3 H3 0.9300 . ? C4 C5 1.401(8) . ? C5 C6 1.337(9) . ? C5 H5 0.9300 . ? C6 C7 1.385(9) . ? C6 H6 0.9300 . ? C7 C8 1.366(8) . ? C7 H7 0.9300 . ? C8 C23 1.485(8) . ? C11 C12 1.392(8) . ? C11 C16 1.417(7) . ? C12 C13 1.385(8) . ? C12 C20 1.500(8) . ? C13 C14 1.375(8) . ? C13 H13 0.9300 . ? C14 C15 1.370(7) . ? C14 H14 0.9300 . ? C15 C16 1.392(7) . ? C15 H15 0.9300 . ? C16 C17 1.517(8) . ? C17 C19 1.522(9) . ? C17 C18 1.539(9) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.502(8) . ? C20 C22 1.527(8) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.400(8) . ? C23 C28 1.402(8) . ? C24 C25 1.393(8) . ? C25 C26 1.391(9) . ? C25 H25 0.9300 . ? C26 C27 1.354(9) . ? C26 H26 0.9300 . ? C27 C28 1.369(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.397(8) . ? C29 C30 1.415(7) . ? C30 C31 1.378(8) . ? C30 C38 1.509(8) . ? C31 C32 1.344(9) . ? C31 H31 0.9300 . ? C32 C33 1.404(9) . ? C32 H32 0.9300 . ? C33 C34 1.367(8) . ? C33 H33 0.9300 . ? C34 C35 1.533(8) . ? C35 C36 1.455(8) . ? C35 C37 1.519(8) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.531(8) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C41 C42 1.468(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.461(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.418(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? 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 C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? C38 C40' H40D 109.5 . . ? C38 C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C38 C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? N3 Y1 N1 99.73(18) . . ? N3 Y1 O1 106.46(17) . . ? N1 Y1 O1 104.20(14) . . ? N3 Y1 N2 97.76(17) . . ? N1 Y1 N2 80.05(15) . . ? O1 Y1 N2 154.12(14) . . ? N3 Y1 C24 123.9(2) . . ? N1 Y1 C24 129.26(18) . . ? O1 Y1 C24 88.19(18) . . ? N2 Y1 C24 70.44(18) . . ? N3 Y1 H3A 20.5(16) . . ? N1 Y1 H3A 79.2(17) . . ? O1 Y1 H3A 111.7(17) . . ? N2 Y1 H3A 94.2(17) . . ? C24 Y1 H3A 141.4(17) . . ? C2 N1 C11 120.8(5) . . ? C2 N1 Y1 123.4(4) . . ? C11 N1 Y1 115.4(3) . . ? C4 N2 C8 119.4(5) . . ? C4 N2 Y1 121.5(4) . . ? C8 N2 Y1 117.8(4) . . ? C29 N3 Y1 154.9(4) . . ? C29 N3 H3A 117(5) . . ? Y1 N3 H3A 88(5) . . ? C44 O1 C41 107.2(4) . . ? C44 O1 Y1 126.0(4) . . ? C41 O1 Y1 125.3(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.1(6) . . ? N1 C2 C1 118.4(5) . . ? C3 C2 C1 117.5(6) . . ? C2 C3 C4 131.4(7) . . ? C2 C3 H3 114.3 . . ? C4 C3 H3 114.3 . . ? N2 C4 C3 122.7(6) . . ? N2 C4 C5 118.4(6) . . ? C3 C4 C5 118.8(7) . . ? C6 C5 C4 121.7(6) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.4(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 N2 120.9(6) . . ? C7 C8 C23 124.1(6) . . ? N2 C8 C23 114.9(5) . . ? C12 C11 C16 120.5(5) . . ? C12 C11 N1 118.5(5) . . ? C16 C11 N1 120.7(5) . . ? C13 C12 C11 118.3(6) . . ? C13 C12 C20 119.9(6) . . ? C11 C12 C20 121.8(5) . . ? C14 C13 C12 122.4(6) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C13 118.8(5) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 122.0(5) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 118.0(5) . . ? C15 C16 C17 119.0(5) . . ? C11 C16 C17 122.9(5) . . ? C16 C17 C19 112.3(5) . . ? C16 C17 C18 110.5(5) . . ? C19 C17 C18 110.7(5) . . ? C16 C17 H17 107.7 . . ? C19 C17 H17 107.7 . . ? C18 C17 H17 107.7 . . ? 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 . . ? C12 C20 C21 113.4(5) . . ? C12 C20 C22 111.2(6) . . ? C21 C20 C22 110.7(6) . . ? C12 C20 H20 107.0 . . ? C21 C20 H20 107.0 . . ? C22 C20 H20 107.0 . . ? 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 . . ? C24 C23 C28 121.1(6) . . ? C24 C23 C8 119.6(5) . . ? C28 C23 C8 119.3(6) . . ? C25 C24 C23 116.3(6) . . ? C25 C24 Y1 129.5(5) . . ? C23 C24 Y1 113.2(4) . . ? C26 C25 C24 122.2(7) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C27 C26 C25 119.8(7) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.6(7) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C23 119.9(7) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? N3 C29 C34 119.0(6) . . ? N3 C29 C30 122.5(5) . . ? C34 C29 C30 118.5(5) . . ? C31 C30 C29 118.9(5) . . ? C31 C30 C38 120.2(5) . . ? C29 C30 C38 120.9(5) . . ? C32 C31 C30 122.5(6) . . ? C32 C31 H31 118.7 . . ? C30 C31 H31 118.7 . . ? C31 C32 C33 118.9(6) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 120.6(6) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C29 120.4(6) . . ? C33 C34 C35 118.0(6) . . ? C29 C34 C35 121.5(6) . . ? C36 C35 C37 112.4(6) . . ? C36 C35 C34 112.1(5) . . ? C37 C35 C34 113.5(6) . . ? C36 C35 H35 106.0 . . ? C37 C35 H35 106.0 . . ? C34 C35 H35 106.0 . . ? 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 . . ? C40 C38 C30 114.8(7) . . ? C40 C38 C39 116.6(12) . . ? C30 C38 C39 113.2(6) . . ? C40 C38 C40' 31.3(12) . . ? C30 C38 C40' 108.7(13) . . ? C39 C38 C40' 94.9(17) . . ? C40 C38 H38 103.3 . . ? C30 C38 H38 103.3 . . ? C39 C38 H38 103.3 . . ? C40' C38 H38 132.9 . . ? 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 . . ? O1 C41 C42 108.5(5) . . ? O1 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O1 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? C43 C42 C41 104.0(7) . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42B 111.0 . . ? C41 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C44 C43 C42 107.9(6) . . ? C44 C43 H43A 110.1 . . ? C42 C43 H43A 110.1 . . ? C44 C43 H43B 110.1 . . ? C42 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C43 C44 O1 108.7(6) . . ? C43 C44 H44A 110.0 . . ? O1 C44 H44A 110.0 . . ? C43 C44 H44B 110.0 . . ? O1 C44 H44B 110.0 . . ? H44A C44 H44B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Y1 N1 C2 -58.1(4) . . . . ? O1 Y1 N1 C2 -168.0(4) . . . . ? N2 Y1 N1 C2 38.1(4) . . . . ? C24 Y1 N1 C2 92.5(5) . . . . ? N3 Y1 N1 C11 115.0(4) . . . . ? O1 Y1 N1 C11 5.1(4) . . . . ? N2 Y1 N1 C11 -148.7(4) . . . . ? C24 Y1 N1 C11 -94.3(4) . . . . ? N3 Y1 N2 C4 61.4(4) . . . . ? N1 Y1 N2 C4 -37.2(4) . . . . ? O1 Y1 N2 C4 -139.2(4) . . . . ? C24 Y1 N2 C4 -175.3(5) . . . . ? N3 Y1 N2 C8 -105.2(4) . . . . ? N1 Y1 N2 C8 156.2(4) . . . . ? O1 Y1 N2 C8 54.2(5) . . . . ? C24 Y1 N2 C8 18.1(4) . . . . ? N1 Y1 N3 C29 -179.9(9) . . . . ? O1 Y1 N3 C29 -71.8(10) . . . . ? N2 Y1 N3 C29 99.0(10) . . . . ? C24 Y1 N3 C29 27.4(10) . . . . ? N3 Y1 O1 C44 37.3(5) . . . . ? N1 Y1 O1 C44 142.2(5) . . . . ? N2 Y1 O1 C44 -121.3(5) . . . . ? C24 Y1 O1 C44 -87.6(5) . . . . ? N3 Y1 O1 C41 -158.8(6) . . . . ? N1 Y1 O1 C41 -53.9(6) . . . . ? N2 Y1 O1 C41 42.6(7) . . . . ? C24 Y1 O1 C41 76.3(6) . . . . ? C11 N1 C2 C3 163.3(6) . . . . ? Y1 N1 C2 C3 -23.9(8) . . . . ? C11 N1 C2 C1 -15.9(8) . . . . ? Y1 N1 C2 C1 156.9(4) . . . . ? N1 C2 C3 C4 -12.6(11) . . . . ? C1 C2 C3 C4 166.6(7) . . . . ? C8 N2 C4 C3 -171.3(5) . . . . ? Y1 N2 C4 C3 22.3(7) . . . . ? C8 N2 C4 C5 6.6(8) . . . . ? Y1 N2 C4 C5 -159.8(4) . . . . ? C2 C3 C4 N2 12.4(11) . . . . ? C2 C3 C4 C5 -165.4(7) . . . . ? N2 C4 C5 C6 -3.7(10) . . . . ? C3 C4 C5 C6 174.2(7) . . . . ? C4 C5 C6 C7 1.3(11) . . . . ? C5 C6 C7 C8 -1.7(11) . . . . ? C6 C7 C8 N2 4.7(10) . . . . ? C6 C7 C8 C23 -177.3(6) . . . . ? C4 N2 C8 C7 -7.2(8) . . . . ? Y1 N2 C8 C7 159.7(5) . . . . ? C4 N2 C8 C23 174.6(5) . . . . ? Y1 N2 C8 C23 -18.5(6) . . . . ? C2 N1 C11 C12 -91.2(6) . . . . ? Y1 N1 C11 C12 95.5(5) . . . . ? C2 N1 C11 C16 94.9(6) . . . . ? Y1 N1 C11 C16 -78.5(5) . . . . ? C16 C11 C12 C13 1.9(8) . . . . ? N1 C11 C12 C13 -172.1(5) . . . . ? C16 C11 C12 C20 -176.7(5) . . . . ? N1 C11 C12 C20 9.3(8) . . . . ? C11 C12 C13 C14 0.1(9) . . . . ? C20 C12 C13 C14 178.8(5) . . . . ? C12 C13 C14 C15 -1.2(9) . . . . ? C13 C14 C15 C16 0.2(9) . . . . ? C14 C15 C16 C11 1.8(9) . . . . ? C14 C15 C16 C17 -175.4(6) . . . . ? C12 C11 C16 C15 -2.8(8) . . . . ? N1 C11 C16 C15 171.0(5) . . . . ? C12 C11 C16 C17 174.2(6) . . . . ? N1 C11 C16 C17 -12.0(8) . . . . ? C15 C16 C17 C19 57.2(8) . . . . ? C11 C16 C17 C19 -119.8(6) . . . . ? C15 C16 C17 C18 -67.0(7) . . . . ? C11 C16 C17 C18 116.0(6) . . . . ? C13 C12 C20 C21 66.8(9) . . . . ? C11 C12 C20 C21 -114.5(7) . . . . ? C13 C12 C20 C22 -58.8(8) . . . . ? C11 C12 C20 C22 119.9(6) . . . . ? C7 C8 C23 C24 -174.2(6) . . . . ? N2 C8 C23 C24 3.9(8) . . . . ? C7 C8 C23 C28 7.5(9) . . . . ? N2 C8 C23 C28 -174.4(5) . . . . ? C28 C23 C24 C25 -0.7(9) . . . . ? C8 C23 C24 C25 -178.9(6) . . . . ? C28 C23 C24 Y1 -170.0(5) . . . . ? C8 C23 C24 Y1 11.7(7) . . . . ? N3 Y1 C24 C25 -96.3(6) . . . . ? N1 Y1 C24 C25 119.3(6) . . . . ? O1 Y1 C24 C25 12.4(6) . . . . ? N2 Y1 C24 C25 177.5(6) . . . . ? N3 Y1 C24 C23 71.2(5) . . . . ? N1 Y1 C24 C23 -73.1(5) . . . . ? O1 Y1 C24 C23 179.9(4) . . . . ? N2 Y1 C24 C23 -15.0(4) . . . . ? C23 C24 C25 C26 3.6(11) . . . . ? Y1 C24 C25 C26 170.8(6) . . . . ? C24 C25 C26 C27 -4.8(12) . . . . ? C25 C26 C27 C28 3.0(12) . . . . ? C26 C27 C28 C23 -0.2(11) . . . . ? C24 C23 C28 C27 -0.9(10) . . . . ? C8 C23 C28 C27 177.3(6) . . . . ? Y1 N3 C29 C34 -2.3(13) . . . . ? Y1 N3 C29 C30 176.4(7) . . . . ? N3 C29 C30 C31 177.4(6) . . . . ? C34 C29 C30 C31 -3.9(8) . . . . ? N3 C29 C30 C38 -1.6(8) . . . . ? C34 C29 C30 C38 177.1(6) . . . . ? C29 C30 C31 C32 4.0(10) . . . . ? C38 C30 C31 C32 -177.0(7) . . . . ? C30 C31 C32 C33 -2.1(12) . . . . ? C31 C32 C33 C34 0.2(12) . . . . ? C32 C33 C34 C29 -0.3(11) . . . . ? C32 C33 C34 C35 -177.7(6) . . . . ? N3 C29 C34 C33 -179.1(6) . . . . ? C30 C29 C34 C33 2.1(9) . . . . ? N3 C29 C34 C35 -1.8(9) . . . . ? C30 C29 C34 C35 179.5(5) . . . . ? C33 C34 C35 C36 82.9(8) . . . . ? C29 C34 C35 C36 -94.4(8) . . . . ? C33 C34 C35 C37 -45.8(8) . . . . ? C29 C34 C35 C37 136.8(7) . . . . ? C31 C30 C38 C40 -99.7(16) . . . . ? C29 C30 C38 C40 79.3(17) . . . . ? C31 C30 C38 C39 37.5(9) . . . . ? C29 C30 C38 C39 -143.5(6) . . . . ? C31 C30 C38 C40' -67(2) . . . . ? C29 C30 C38 C40' 112(2) . . . . ? C44 O1 C41 C42 8.8(11) . . . . ? Y1 O1 C41 C42 -157.6(6) . . . . ? O1 C41 C42 C43 -17.4(12) . . . . ? C41 C42 C43 C44 19.7(13) . . . . ? C42 C43 C44 O1 -15.0(12) . . . . ? C41 O1 C44 C43 3.8(10) . . . . ? Y1 O1 C44 C43 170.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.487 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.050