# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 910960' #TrackingRef '15436_web_deposit_cif_file_0_HirokiOguri_1352967251.shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 O2 Si2' _chemical_formula_sum 'C30 H36 O2 Si2' _chemical_formula_weight 484.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2625(5) _cell_length_b 13.3817(6) _cell_length_c 16.1422(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.756(2) _cell_angle_gamma 90.00 _cell_volume 2864.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33007 _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 68.230 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8815 _exptl_absorpt_correction_T_max 0.9622 _exptl_absorpt_process_details Lorentz-polarization _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP 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 33007 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 68.23 _reflns_number_total 5205 _reflns_number_gt 2305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO' _computing_cell_refinement 'Rigaku RAPID AUTO' _computing_data_reduction 'Rigaku RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure and PLATON(Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.1641P)^2^+3.3017P] 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 5205 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2095 _refine_ls_R_factor_gt 0.1148 _refine_ls_wR_factor_ref 0.3826 _refine_ls_wR_factor_gt 0.2893 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Si1 Si 0.67345(15) 0.62451(14) 1.10508(12) 0.0755(7) Uani 1 1 d . . . Si2 Si 0.61093(19) 0.42286(19) 0.63725(13) 0.0980(9) Uani 1 1 d . . . O1 O 1.0464(5) 0.1897(4) 0.7956(3) 0.1023(18) Uani 1 1 d . . . O2 O 1.1453(6) 0.7165(6) 0.9465(4) 0.124(2) Uani 1 1 d . . . C1 C 0.7605(5) 0.4890(4) 0.8209(4) 0.0662(17) Uani 1 1 d . . . H1 H 0.7401 0.5428 0.7812 0.079 Uiso 1 1 calc R . . C2 C 0.6857(5) 0.4033(5) 0.8151(4) 0.0725(19) Uani 1 1 d . . . H2 H 0.6180 0.4264 0.8337 0.087 Uiso 1 1 calc R . . C3 C 0.7181(6) 0.3096(5) 0.8657(4) 0.077(2) Uani 1 1 d . . . H3 H 0.7601 0.3285 0.9144 0.092 Uiso 1 1 calc R . . H4 H 0.6587 0.2717 0.8847 0.092 Uiso 1 1 calc R . . C4 C 0.6772(5) 0.3615(5) 0.7278(4) 0.0710(18) Uani 1 1 d . . . C5 C 0.7008(7) 0.5056(8) 0.5811(6) 0.139(4) Uani 1 1 d . . . H5 H 0.7308 0.5536 0.6200 0.167 Uiso 1 1 calc R . . H6 H 0.6645 0.5417 0.5371 0.167 Uiso 1 1 calc R . . H7 H 0.7541 0.4648 0.5567 0.167 Uiso 1 1 calc R . . C6 C 0.5055(6) 0.4982(7) 0.6752(5) 0.110(3) Uani 1 1 d . . . H8 H 0.4587 0.4552 0.7052 0.132 Uiso 1 1 calc R . . H9 H 0.4702 0.5294 0.6282 0.132 Uiso 1 1 calc R . . H10 H 0.5314 0.5503 0.7125 0.132 Uiso 1 1 calc R . . C7 C 0.5626(10) 0.3230(9) 0.5652(6) 0.173(5) Uani 1 1 d . . . H11 H 0.6189 0.2812 0.5473 0.207 Uiso 1 1 calc R . . H12 H 0.5304 0.3542 0.5167 0.207 Uiso 1 1 calc R . . H13 H 0.5132 0.2816 0.5940 0.207 Uiso 1 1 calc R . . C8 C 0.7281(6) 0.2772(5) 0.7219(5) 0.080(2) Uani 1 1 d . . . H14 H 0.7325 0.2387 0.6726 0.096 Uiso 1 1 calc R . . C9 C 0.7789(6) 0.2491(5) 0.8034(4) 0.075(2) Uani 1 1 d . . . C10 C 0.7854(7) 0.1352(5) 0.8221(5) 0.105(3) Uani 1 1 d . . . H15 H 0.7846 0.1225 0.8825 0.126 Uiso 1 1 calc R . . H16 H 0.7287 0.0988 0.7954 0.126 Uiso 1 1 calc R . . C11 C 0.8875(7) 0.1033(6) 0.7847(6) 0.112(3) Uani 1 1 d . . . H17 H 0.9157 0.0450 0.8147 0.134 Uiso 1 1 calc R . . H18 H 0.8790 0.0857 0.7255 0.134 Uiso 1 1 calc R . . C12 C 0.9539(8) 0.1911(6) 0.7944(5) 0.088(2) Uani 1 1 d . . . C13 C 0.8881(6) 0.2803(5) 0.8015(4) 0.077(2) Uani 1 1 d . . . C14 C 0.9262(6) 0.3728(6) 0.8041(4) 0.078(2) Uani 1 1 d . . . H19 H 0.9972 0.3759 0.7974 0.094 Uiso 1 1 calc R . . C15 C 0.8775(5) 0.4708(5) 0.8157(4) 0.0722(19) Uani 1 1 d . . . H20 H 0.9068 0.5198 0.7759 0.087 Uiso 1 1 calc R . . C16 C 0.8895(5) 0.5133(5) 0.9068(4) 0.0747(19) Uani 1 1 d . . . H21 H 0.9042 0.4558 0.9447 0.090 Uiso 1 1 calc R . . C17 C 0.9708(6) 0.5867(7) 0.9173(4) 0.085(2) Uani 1 1 d . . . H22 H 1.0369 0.5598 0.9139 0.102 Uiso 1 1 calc R . . C18 C 0.9676(7) 0.6836(7) 0.9307(4) 0.090(2) Uani 1 1 d . . . C19 C 1.0595(9) 0.7468(9) 0.9455(5) 0.107(3) Uani 1 1 d . . . C20 C 1.0259(9) 0.8524(9) 0.9568(6) 0.136(4) Uani 1 1 d . . . H23 H 1.0696 0.8985 0.9256 0.163 Uiso 1 1 calc R . . H24 H 1.0288 0.8710 1.0162 0.163 Uiso 1 1 calc R . . C21 C 0.9185(8) 0.8575(6) 0.9243(6) 0.122(3) Uani 1 1 d . . . H25 H 0.9169 0.8756 0.8648 0.147 Uiso 1 1 calc R . . H26 H 0.8790 0.9073 0.9555 0.147 Uiso 1 1 calc R . . C22 C 0.8758(7) 0.7496(6) 0.9377(5) 0.089(2) Uani 1 1 d . A . C23 C 0.8263(7) 0.7300(6) 1.0210(5) 0.100(3) Uani 1 1 d . . . H27 H 0.8495 0.7585 1.0716 0.120 Uiso 1 1 calc R A . C24 C 0.7471(6) 0.6687(5) 1.0155(4) 0.081(2) Uani 1 1 d . A . C25A C 0.7547(11) 0.6358(11) 1.2058(9) 0.099(5) Uiso 0.592(13) 1 d P A 1 C26A C 0.5577(12) 0.6967(12) 1.1099(10) 0.113(6) Uiso 0.592(13) 1 d P A 1 C27A C 0.6396(11) 0.4822(11) 1.0980(9) 0.101(5) Uiso 0.592(13) 1 d P A 1 C25B C 0.7641(16) 0.5651(17) 1.1755(13) 0.101(7) Uiso 0.408(13) 1 d P A 2 C26B C 0.6033(14) 0.7379(14) 1.1596(12) 0.080(6) Uiso 0.408(13) 1 d P A 2 C27B C 0.5637(16) 0.5430(16) 1.0654(13) 0.101(7) Uiso 0.408(13) 1 d P A 2 C28 C 0.7320(5) 0.6374(5) 0.9247(4) 0.0714(19) Uani 1 1 d . . . H28 H 0.6588 0.6395 0.9093 0.086 Uiso 1 1 calc R A . C29 C 0.7891(6) 0.7192(5) 0.8785(5) 0.084(2) Uani 1 1 d . A . H29 H 0.7445 0.7768 0.8666 0.101 Uiso 1 1 calc R . . H30 H 0.8157 0.6933 0.8257 0.101 Uiso 1 1 calc R . . C30 C 0.7741(5) 0.5343(5) 0.9091(4) 0.0695(18) Uani 1 1 d . A . H31 H 0.7434 0.4872 0.9497 0.083 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 Si1 0.0771(14) 0.0698(12) 0.0801(14) -0.0102(10) 0.0148(11) -0.0078(10) Si2 0.1016(19) 0.1177(19) 0.0750(15) -0.0030(13) 0.0113(13) 0.0142(15) O1 0.104(5) 0.110(4) 0.093(4) -0.002(3) 0.009(3) 0.029(4) O2 0.097(5) 0.180(7) 0.096(4) 0.003(4) 0.014(4) -0.055(5) C1 0.076(5) 0.055(4) 0.068(4) 0.006(3) 0.005(3) 0.004(3) C2 0.072(5) 0.074(4) 0.072(5) 0.004(3) 0.013(4) 0.008(4) C3 0.085(5) 0.067(4) 0.081(5) 0.006(4) 0.025(4) -0.001(4) C4 0.068(5) 0.072(5) 0.073(5) 0.007(4) 0.005(3) 0.001(4) C5 0.105(7) 0.194(11) 0.120(7) 0.058(7) 0.038(6) 0.037(7) C6 0.084(6) 0.144(8) 0.102(6) 0.037(5) 0.022(5) 0.030(5) C7 0.225(13) 0.174(10) 0.116(8) -0.063(8) -0.058(8) 0.020(10) C8 0.094(6) 0.067(4) 0.078(5) -0.013(4) 0.019(4) -0.010(4) C9 0.083(5) 0.058(4) 0.083(5) 0.004(3) 0.029(4) -0.003(4) C10 0.136(8) 0.065(5) 0.114(7) 0.013(4) 0.039(6) 0.003(5) C11 0.131(8) 0.078(6) 0.128(7) 0.022(5) 0.053(6) 0.035(6) C12 0.107(7) 0.080(5) 0.077(5) 0.019(4) 0.019(5) 0.011(5) C13 0.092(6) 0.068(5) 0.071(5) 0.022(4) 0.020(4) 0.016(4) C14 0.074(5) 0.083(5) 0.077(5) 0.018(4) 0.021(4) 0.008(4) C15 0.073(5) 0.070(4) 0.074(4) 0.016(4) 0.009(3) -0.002(4) C16 0.083(5) 0.069(4) 0.072(5) 0.012(3) 0.015(4) -0.002(4) C17 0.077(5) 0.097(6) 0.081(5) 0.012(4) 0.010(4) -0.006(5) C18 0.097(6) 0.104(6) 0.067(5) 0.013(4) 0.012(4) -0.023(6) C19 0.113(8) 0.132(9) 0.077(6) -0.006(5) 0.024(6) -0.044(7) C20 0.137(9) 0.141(10) 0.131(9) -0.030(7) 0.040(7) -0.078(8) C21 0.141(9) 0.086(6) 0.142(8) -0.016(5) 0.055(7) -0.039(6) C22 0.103(7) 0.086(5) 0.077(5) -0.014(4) 0.020(5) -0.029(5) C23 0.126(7) 0.096(6) 0.079(5) -0.025(4) 0.024(5) -0.038(5) C24 0.092(6) 0.071(5) 0.081(5) -0.009(4) 0.017(4) -0.015(4) C28 0.077(5) 0.061(4) 0.077(5) 0.000(3) 0.010(4) -0.005(3) C29 0.096(6) 0.072(5) 0.086(5) -0.002(4) 0.011(4) 0.005(4) C30 0.072(5) 0.067(4) 0.070(4) 0.012(3) 0.016(3) -0.002(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 Si1 C26A 1.816(16) . ? Si1 C25B 1.83(2) . ? Si1 C24 1.853(7) . ? Si1 C27B 1.92(2) . ? Si1 C25A 1.945(15) . ? Si1 C27A 1.960(14) . ? Si1 C26B 1.991(18) . ? Si2 C6 1.835(8) . ? Si2 C5 1.870(9) . ? Si2 C7 1.879(10) . ? Si2 C4 1.884(7) . ? O1 C12 1.227(9) . ? O2 C19 1.208(11) . ? C1 C2 1.518(9) . ? C1 C30 1.555(9) . ? C1 C15 1.574(9) . ? C1 H1 1.0000 . ? C2 C4 1.519(9) . ? C2 C3 1.553(9) . ? C2 H2 1.0000 . ? C3 C9 1.530(9) . ? C3 H3 0.9900 . ? C3 H4 0.9900 . ? C4 C8 1.319(9) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C7 H13 0.9800 . ? C8 C9 1.516(10) . ? C8 H14 0.9500 . ? C9 C13 1.508(10) . ? C9 C10 1.555(9) . ? C10 C11 1.549(11) . ? C10 H15 0.9900 . ? C10 H16 0.9900 . ? C11 C12 1.475(11) . ? C11 H17 0.9900 . ? C11 H18 0.9900 . ? C12 C13 1.484(10) . ? C13 C14 1.337(9) . ? C14 C15 1.475(9) . ? C14 H19 0.9500 . ? C15 C16 1.583(9) . ? C15 H20 1.0000 . ? C16 C17 1.467(10) . ? C16 C30 1.558(9) . ? C16 H21 1.0000 . ? C17 C18 1.315(11) . ? C17 H22 0.9500 . ? C18 C19 1.500(12) . ? C18 C22 1.510(11) . ? C19 C20 1.494(14) . ? C20 C21 1.513(14) . ? C20 H23 0.9900 . ? C20 H24 0.9900 . ? C21 C22 1.567(10) . ? C21 H25 0.9900 . ? C21 H26 0.9900 . ? C22 C23 1.527(10) . ? C22 C29 1.539(10) . ? C23 C24 1.334(10) . ? C23 H27 0.9500 . ? C24 C28 1.534(9) . ? C28 C30 1.511(9) . ? C28 C29 1.530(9) . ? C28 H28 1.0000 . ? C29 H29 0.9900 . ? C29 H30 0.9900 . ? C30 H31 1.0000 . ? 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 C26A Si1 C25B 139.0(8) . . ? C26A Si1 C24 108.5(6) . . ? C25B Si1 C24 106.0(7) . . ? C26A Si1 C27B 71.3(8) . . ? C25B Si1 C27B 116.7(9) . . ? C24 Si1 C27B 109.0(7) . . ? C26A Si1 C25A 112.5(7) . . ? C25B Si1 C25A 32.9(7) . . ? C24 Si1 C25A 109.6(5) . . ? C27B Si1 C25A 137.0(8) . . ? C26A Si1 C27A 109.1(7) . . ? C25B Si1 C27A 76.2(8) . . ? C24 Si1 C27A 112.8(5) . . ? C27B Si1 C27A 42.0(7) . . ? C25A Si1 C27A 104.4(6) . . ? C26A Si1 C26B 34.5(6) . . ? C25B Si1 C26B 111.3(9) . . ? C24 Si1 C26B 110.9(6) . . ? C27B Si1 C26B 102.9(8) . . ? C25A Si1 C26B 80.1(7) . . ? C27A Si1 C26B 131.2(7) . . ? C6 Si2 C5 109.3(4) . . ? C6 Si2 C7 110.0(5) . . ? C5 Si2 C7 109.6(5) . . ? C6 Si2 C4 109.3(3) . . ? C5 Si2 C4 109.9(4) . . ? C7 Si2 C4 108.8(4) . . ? C2 C1 C30 114.8(5) . . ? C2 C1 C15 121.6(5) . . ? C30 C1 C15 90.4(5) . . ? C2 C1 H1 109.5 . . ? C30 C1 H1 109.5 . . ? C15 C1 H1 109.5 . . ? C1 C2 C4 112.1(5) . . ? C1 C2 C3 113.6(6) . . ? C4 C2 C3 102.0(5) . . ? C1 C2 H2 109.6 . . ? C4 C2 H2 109.6 . . ? C3 C2 H2 109.6 . . ? C9 C3 C2 103.1(5) . . ? C9 C3 H3 111.1 . . ? C2 C3 H3 111.1 . . ? C9 C3 H4 111.1 . . ? C2 C3 H4 111.1 . . ? H3 C3 H4 109.1 . . ? C8 C4 C2 110.5(6) . . ? C8 C4 Si2 123.4(6) . . ? C2 C4 Si2 126.0(5) . . ? Si2 C5 H5 109.5 . . ? Si2 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? Si2 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? Si2 C6 H8 109.5 . . ? Si2 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? Si2 C6 H10 109.5 . . ? H8 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? Si2 C7 H11 109.5 . . ? Si2 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? Si2 C7 H13 109.5 . . ? H11 C7 H13 109.5 . . ? H12 C7 H13 109.5 . . ? C4 C8 C9 111.8(6) . . ? C4 C8 H14 124.1 . . ? C9 C8 H14 124.1 . . ? C13 C9 C8 109.2(5) . . ? C13 C9 C3 112.4(6) . . ? C8 C9 C3 101.9(6) . . ? C13 C9 C10 103.0(6) . . ? C8 C9 C10 115.7(6) . . ? C3 C9 C10 114.8(6) . . ? C11 C10 C9 104.0(6) . . ? C11 C10 H15 111.0 . . ? C9 C10 H15 111.0 . . ? C11 C10 H16 111.0 . . ? C9 C10 H16 111.0 . . ? H15 C10 H16 109.0 . . ? C12 C11 C10 105.2(7) . . ? C12 C11 H17 110.7 . . ? C10 C11 H17 110.7 . . ? C12 C11 H18 110.7 . . ? C10 C11 H18 110.7 . . ? H17 C11 H18 108.8 . . ? O1 C12 C11 125.8(8) . . ? O1 C12 C13 126.8(8) . . ? C11 C12 C13 107.3(8) . . ? C14 C13 C12 121.7(8) . . ? C14 C13 C9 128.2(6) . . ? C12 C13 C9 110.1(7) . . ? C13 C14 C15 131.4(7) . . ? C13 C14 H19 114.3 . . ? C15 C14 H19 114.3 . . ? C14 C15 C1 125.3(6) . . ? C14 C15 C16 113.4(6) . . ? C1 C15 C16 89.0(5) . . ? C14 C15 H20 109.1 . . ? C1 C15 H20 109.1 . . ? C16 C15 H20 109.1 . . ? C17 C16 C30 126.7(6) . . ? C17 C16 C15 114.4(6) . . ? C30 C16 C15 89.9(5) . . ? C17 C16 H21 107.9 . . ? C30 C16 H21 107.9 . . ? C15 C16 H21 107.9 . . ? C18 C17 C16 130.9(8) . . ? C18 C17 H22 114.6 . . ? C16 C17 H22 114.6 . . ? C17 C18 C19 123.6(9) . . ? C17 C18 C22 128.1(8) . . ? C19 C18 C22 108.2(8) . . ? O2 C19 C20 126.7(10) . . ? O2 C19 C18 125.2(11) . . ? C20 C19 C18 108.0(10) . . ? C19 C20 C21 106.3(8) . . ? C19 C20 H23 110.5 . . ? C21 C20 H23 110.5 . . ? C19 C20 H24 110.5 . . ? C21 C20 H24 110.5 . . ? H23 C20 H24 108.7 . . ? C20 C21 C22 104.5(8) . . ? C20 C21 H25 110.8 . . ? C22 C21 H25 110.8 . . ? C20 C21 H26 110.8 . . ? C22 C21 H26 110.8 . . ? H25 C21 H26 108.9 . . ? C18 C22 C23 108.7(7) . . ? C18 C22 C29 113.3(6) . . ? C23 C22 C29 100.0(6) . . ? C18 C22 C21 103.6(7) . . ? C23 C22 C21 116.1(7) . . ? C29 C22 C21 115.3(8) . . ? C24 C23 C22 113.2(7) . . ? C24 C23 H27 123.4 . . ? C22 C23 H27 123.4 . . ? C23 C24 C28 108.9(6) . . ? C23 C24 Si1 124.5(6) . . ? C28 C24 Si1 126.5(5) . . ? C30 C28 C29 112.7(6) . . ? C30 C28 C24 111.4(6) . . ? C29 C28 C24 102.2(5) . . ? C30 C28 H28 110.1 . . ? C29 C28 H28 110.1 . . ? C24 C28 H28 110.1 . . ? C28 C29 C22 104.9(6) . . ? C28 C29 H29 110.8 . . ? C22 C29 H29 110.8 . . ? C28 C29 H30 110.8 . . ? C22 C29 H30 110.8 . . ? H29 C29 H30 108.8 . . ? C28 C30 C1 118.1(5) . . ? C28 C30 C16 122.3(6) . . ? C1 C30 C16 90.6(5) . . ? C28 C30 H31 108.1 . . ? C1 C30 H31 108.1 . . ? C16 C30 H31 108.1 . . ? 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 C30 C1 C2 C4 -179.1(5) . . . . ? C15 C1 C2 C4 -72.1(8) . . . . ? C30 C1 C2 C3 -64.2(7) . . . . ? C15 C1 C2 C3 42.9(8) . . . . ? C1 C2 C3 C9 -90.1(7) . . . . ? C4 C2 C3 C9 30.8(7) . . . . ? C1 C2 C4 C8 102.2(7) . . . . ? C3 C2 C4 C8 -19.7(7) . . . . ? C1 C2 C4 Si2 -74.1(7) . . . . ? C3 C2 C4 Si2 164.0(5) . . . . ? C6 Si2 C4 C8 153.6(6) . . . . ? C5 Si2 C4 C8 -86.6(7) . . . . ? C7 Si2 C4 C8 33.5(8) . . . . ? C6 Si2 C4 C2 -30.6(7) . . . . ? C5 Si2 C4 C2 89.3(7) . . . . ? C7 Si2 C4 C2 -150.7(7) . . . . ? C2 C4 C8 C9 -0.1(8) . . . . ? Si2 C4 C8 C9 176.3(5) . . . . ? C4 C8 C9 C13 -98.9(7) . . . . ? C4 C8 C9 C3 20.2(8) . . . . ? C4 C8 C9 C10 145.5(7) . . . . ? C2 C3 C9 C13 86.1(7) . . . . ? C2 C3 C9 C8 -30.7(7) . . . . ? C2 C3 C9 C10 -156.6(7) . . . . ? C13 C9 C10 C11 -28.7(8) . . . . ? C8 C9 C10 C11 90.4(9) . . . . ? C3 C9 C10 C11 -151.2(7) . . . . ? C9 C10 C11 C12 32.4(9) . . . . ? C10 C11 C12 O1 157.6(8) . . . . ? C10 C11 C12 C13 -23.1(9) . . . . ? O1 C12 C13 C14 5.0(12) . . . . ? C11 C12 C13 C14 -174.4(7) . . . . ? O1 C12 C13 C9 -176.0(7) . . . . ? C11 C12 C13 C9 4.7(8) . . . . ? C8 C9 C13 C14 70.9(9) . . . . ? C3 C9 C13 C14 -41.4(10) . . . . ? C10 C9 C13 C14 -165.6(7) . . . . ? C8 C9 C13 C12 -108.1(6) . . . . ? C3 C9 C13 C12 139.6(6) . . . . ? C10 C9 C13 C12 15.5(8) . . . . ? C12 C13 C14 C15 -176.0(7) . . . . ? C9 C13 C14 C15 5.1(13) . . . . ? C13 C14 C15 C1 -5.3(12) . . . . ? C13 C14 C15 C16 101.1(9) . . . . ? C2 C1 C15 C14 0.6(10) . . . . ? C30 C1 C15 C14 120.3(7) . . . . ? C2 C1 C15 C16 -117.7(6) . . . . ? C30 C1 C15 C16 2.0(5) . . . . ? C14 C15 C16 C17 98.5(7) . . . . ? C1 C15 C16 C17 -133.0(6) . . . . ? C14 C15 C16 C30 -130.5(6) . . . . ? C1 C15 C16 C30 -2.0(5) . . . . ? C30 C16 C17 C18 0.1(12) . . . . ? C15 C16 C17 C18 109.8(9) . . . . ? C16 C17 C18 C19 175.9(7) . . . . ? C16 C17 C18 C22 -1.4(14) . . . . ? C17 C18 C19 O2 0.2(14) . . . . ? C22 C18 C19 O2 177.9(8) . . . . ? C17 C18 C19 C20 179.2(8) . . . . ? C22 C18 C19 C20 -3.1(9) . . . . ? O2 C19 C20 C21 162.7(9) . . . . ? C18 C19 C20 C21 -16.3(10) . . . . ? C19 C20 C21 C22 28.5(9) . . . . ? C17 C18 C22 C23 73.8(10) . . . . ? C19 C18 C22 C23 -103.8(7) . . . . ? C17 C18 C22 C29 -36.4(11) . . . . ? C19 C18 C22 C29 145.9(6) . . . . ? C17 C18 C22 C21 -162.1(8) . . . . ? C19 C18 C22 C21 20.3(8) . . . . ? C20 C21 C22 C18 -29.8(9) . . . . ? C20 C21 C22 C23 89.3(9) . . . . ? C20 C21 C22 C29 -154.2(7) . . . . ? C18 C22 C23 C24 -99.5(9) . . . . ? C29 C22 C23 C24 19.5(9) . . . . ? C21 C22 C23 C24 144.2(9) . . . . ? C22 C23 C24 C28 0.2(10) . . . . ? C22 C23 C24 Si1 177.0(6) . . . . ? C26A Si1 C24 C23 101.4(9) . . . . ? C25B Si1 C24 C23 -56.1(11) . . . . ? C27B Si1 C24 C23 177.4(10) . . . . ? C25A Si1 C24 C23 -21.8(9) . . . . ? C27A Si1 C24 C23 -137.6(8) . . . . ? C26B Si1 C24 C23 64.8(10) . . . . ? C26A Si1 C24 C28 -82.3(8) . . . . ? C25B Si1 C24 C28 120.2(10) . . . . ? C27B Si1 C24 C28 -6.3(10) . . . . ? C25A Si1 C24 C28 154.5(7) . . . . ? C27A Si1 C24 C28 38.7(8) . . . . ? C26B Si1 C24 C28 -118.9(8) . . . . ? C23 C24 C28 C30 100.6(7) . . . . ? Si1 C24 C28 C30 -76.2(8) . . . . ? C23 C24 C28 C29 -20.0(8) . . . . ? Si1 C24 C28 C29 163.2(6) . . . . ? C30 C28 C29 C22 -88.2(7) . . . . ? C24 C28 C29 C22 31.5(7) . . . . ? C18 C22 C29 C28 84.8(7) . . . . ? C23 C22 C29 C28 -30.7(7) . . . . ? C21 C22 C29 C28 -156.0(6) . . . . ? C29 C28 C30 C1 -68.7(8) . . . . ? C24 C28 C30 C1 177.2(5) . . . . ? C29 C28 C30 C16 41.9(9) . . . . ? C24 C28 C30 C16 -72.3(8) . . . . ? C2 C1 C30 C28 -109.0(7) . . . . ? C15 C1 C30 C28 125.5(6) . . . . ? C2 C1 C30 C16 123.4(6) . . . . ? C15 C1 C30 C16 -2.1(5) . . . . ? C17 C16 C30 C28 -1.2(10) . . . . ? C15 C16 C30 C28 -122.2(6) . . . . ? C17 C16 C30 C1 123.0(7) . . . . ? C15 C16 C30 C1 2.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 68.23 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.514 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.075 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 910961' #TrackingRef '15437_web_deposit_cif_file_1_HirokiOguri_1352967251.shelxl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H38 N2 O5 Si, 0.5(C3 H8 O)' _chemical_formula_sum 'C36.50 H42 N2 O5.50 Si' _chemical_formula_weight 624.81 _chemical_compound_source 'synthesised by authors, see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.06519(18) _cell_length_b 11.1789(2) _cell_length_c 16.4195(3) _cell_angle_alpha 82.6410(10) _cell_angle_beta 81.6980(10) _cell_angle_gamma 64.6870(10) _cell_volume 1648.04(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17152 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 68.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8802 _exptl_absorpt_correction_T_max 0.9238 _exptl_absorpt_process_details Lorentz-polarization _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP 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 19565 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 68.24 _reflns_number_total 5910 _reflns_number_gt 4987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO' _computing_cell_refinement 'Rigaku RAPID AUTO' _computing_data_reduction 'Rigaku RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Crystal Structure and PLATON(Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0825P)^2^+0.6503P] 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 5910 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 Si1 Si 0.48105(5) -0.16317(5) 0.65519(3) 0.03131(16) Uani 1 1 d . . . O1 O -0.48844(16) 0.28903(16) 0.68365(10) 0.0478(4) Uani 1 1 d . . . O2 O -0.40229(16) 0.24626(16) 0.80798(9) 0.0434(4) Uani 1 1 d . . . O3 O -0.26655(17) 0.41371(14) 0.68252(10) 0.0436(4) Uani 1 1 d . . . O4 O 0.21237(16) -0.09068(16) 0.98871(8) 0.0404(4) Uani 1 1 d . . . O5 O -0.04953(18) -0.24342(15) 0.85741(9) 0.0414(4) Uani 1 1 d . . . O6 O 0.3456(5) 0.0930(4) 0.9449(3) 0.0728(11) Uiso 0.50 1 d P . . H39 H 0.3502 0.0363 0.9143 0.087 Uiso 0.50 1 calc PR . . N1 N -0.21868(18) 0.12670(17) 0.60869(10) 0.0318(4) Uani 1 1 d . . . H6 H -0.2737 0.1082 0.5798 0.038 Uiso 1 1 calc R . . N2 N 0.08442(18) -0.19157(16) 0.93955(10) 0.0310(4) Uani 1 1 d . . . C1 C -0.1026(2) 0.14256(18) 0.72300(11) 0.0257(4) Uani 1 1 d . . . H1 H -0.1351 0.2017 0.7695 0.031 Uiso 1 1 calc R . . C2 C -0.2386(2) 0.12943(19) 0.69838(12) 0.0297(4) Uani 1 1 d . . . H2 H -0.2340 0.0410 0.7222 0.036 Uiso 1 1 calc R . . C3 C -0.3894(2) 0.2331(2) 0.72695(13) 0.0358(5) Uani 1 1 d . . . C4 C -0.5442(3) 0.3412(3) 0.84083(17) 0.0602(7) Uani 1 1 d . . . H3 H -0.5419 0.3483 0.8995 0.072 Uiso 1 1 calc R . . H4 H -0.6207 0.3118 0.8346 0.072 Uiso 1 1 calc R . . H5 H -0.5662 0.4281 0.8107 0.072 Uiso 1 1 calc R . . C5 C -0.0940(2) 0.15918(18) 0.57313(11) 0.0272(4) Uani 1 1 d . . . H7 H -0.0085 0.0742 0.5586 0.033 Uiso 1 1 calc R . . C6 C -0.1294(2) 0.24858(19) 0.49396(11) 0.0284(4) Uani 1 1 d . . . C7 C -0.2596(2) 0.3639(2) 0.48963(13) 0.0354(5) Uani 1 1 d . . . H8 H -0.3287 0.3876 0.5372 0.042 Uiso 1 1 calc R . . C8 C -0.2899(2) 0.4447(2) 0.41709(14) 0.0395(5) Uani 1 1 d . . . H9 H -0.3788 0.5233 0.4153 0.047 Uiso 1 1 calc R . . C9 C -0.1907(3) 0.4108(2) 0.34744(13) 0.0405(5) Uani 1 1 d . . . H10 H -0.2112 0.4662 0.2977 0.049 Uiso 1 1 calc R . . C10 C -0.0614(3) 0.2963(2) 0.35012(12) 0.0377(5) Uani 1 1 d . . . H11 H 0.0069 0.2733 0.3022 0.045 Uiso 1 1 calc R . . C11 C -0.0312(2) 0.2146(2) 0.42298(12) 0.0320(4) Uani 1 1 d . . . H12 H 0.0570 0.1352 0.4242 0.038 Uiso 1 1 calc R . . C12 C -0.0528(2) 0.21275(18) 0.64550(11) 0.0262(4) Uani 1 1 d . . . C13 C -0.1428(2) 0.36227(19) 0.64858(12) 0.0314(4) Uani 1 1 d . . . C14 C -0.0519(2) 0.4353(2) 0.60742(14) 0.0400(5) Uani 1 1 d . . . H13 H -0.0395 0.4888 0.6469 0.048 Uiso 1 1 calc R . . H14 H -0.0993 0.4948 0.5600 0.048 Uiso 1 1 calc R . . C15 C 0.0972(2) 0.3260(2) 0.57857(13) 0.0344(5) Uani 1 1 d . . . H15 H 0.1791 0.3502 0.5841 0.041 Uiso 1 1 calc R . . H16 H 0.1004 0.3101 0.5202 0.041 Uiso 1 1 calc R . . C16 C 0.1080(2) 0.20252(19) 0.63591(11) 0.0284(4) Uani 1 1 d . . . C17 C 0.2299(2) 0.07447(19) 0.60638(11) 0.0293(4) Uani 1 1 d . . . H17 H 0.2460 0.0515 0.5509 0.035 Uiso 1 1 calc R . . C18 C 0.3127(2) -0.00316(19) 0.66526(11) 0.0279(4) Uani 1 1 d . . . C19 C 0.5105(3) -0.2162(3) 0.54867(15) 0.0495(6) Uani 1 1 d . . . H18 H 0.4237 -0.2271 0.5370 0.059 Uiso 1 1 calc R . . H19 H 0.5978 -0.3007 0.5439 0.059 Uiso 1 1 calc R . . H20 H 0.5254 -0.1486 0.5090 0.059 Uiso 1 1 calc R . . C20 C 0.6413(3) -0.1349(3) 0.67739(17) 0.0526(6) Uani 1 1 d . . . H21 H 0.6505 -0.0634 0.6391 0.063 Uiso 1 1 calc R . . H22 H 0.7318 -0.2164 0.6705 0.063 Uiso 1 1 calc R . . H23 H 0.6258 -0.1100 0.7342 0.063 Uiso 1 1 calc R . . C21 C 0.4630(3) -0.2943(2) 0.73286(16) 0.0479(6) Uani 1 1 d . . . H24 H 0.5512 -0.3777 0.7258 0.057 Uiso 1 1 calc R . . H25 H 0.3755 -0.3072 0.7249 0.057 Uiso 1 1 calc R . . H26 H 0.4529 -0.2668 0.7886 0.057 Uiso 1 1 calc R . . C22 C 0.2434(2) 0.05804(19) 0.74784(11) 0.0273(4) Uani 1 1 d . . . H27 H 0.3211 0.0466 0.7836 0.033 Uiso 1 1 calc R . . C23 C 0.1559(2) 0.20503(19) 0.72096(12) 0.0297(4) Uani 1 1 d . . . H28 H 0.2187 0.2543 0.7160 0.036 Uiso 1 1 calc R . . H29 H 0.0688 0.2469 0.7609 0.036 Uiso 1 1 calc R . . C24 C 0.1489(2) -0.01370(19) 0.78795(11) 0.0262(4) Uani 1 1 d . . . H30 H 0.2150 -0.1107 0.7901 0.031 Uiso 1 1 calc R . . C25 C 0.0058(2) 0.00313(18) 0.75285(11) 0.0257(4) Uani 1 1 d . . . H31 H 0.0215 -0.0675 0.7161 0.031 Uiso 1 1 calc R . . C26 C -0.0525(2) -0.02285(19) 0.84411(11) 0.0267(4) Uani 1 1 d . . . H32 H -0.1578 0.0378 0.8597 0.032 Uiso 1 1 calc R . . C27 C 0.0603(2) 0.01462(19) 0.87533(11) 0.0277(4) Uani 1 1 d . . . H33 H 0.0217 0.1083 0.8904 0.033 Uiso 1 1 calc R . . C28 C 0.1296(2) -0.0895(2) 0.94177(11) 0.0309(4) Uani 1 1 d . . . C29 C -0.0105(2) -0.1644(2) 0.87759(11) 0.0306(4) Uani 1 1 d . . . C30 C 0.1250(2) -0.3077(2) 0.99595(12) 0.0366(5) Uani 1 1 d . . . C31 C 0.2689(3) -0.3753(3) 1.0140(2) 0.0702(9) Uani 1 1 d . . . H34 H 0.3434 -0.3489 0.9874 0.084 Uiso 1 1 calc R . . C32 C 0.3031(4) -0.4842(4) 1.0726(2) 0.0919(12) Uani 1 1 d . . . H35 H 0.4016 -0.5304 1.0869 0.110 Uiso 1 1 calc R . . C33 C 0.1985(4) -0.5249(3) 1.10927(18) 0.0685(8) Uani 1 1 d . . . H36 H 0.2247 -0.6006 1.1476 0.082 Uiso 1 1 calc R . . C34 C 0.0547(3) -0.4569(2) 1.09128(15) 0.0524(6) Uani 1 1 d . . . H37 H -0.0188 -0.4850 1.1173 0.063 Uiso 1 1 calc R . . C35 C 0.0173(3) -0.3462(2) 1.03448(13) 0.0424(5) Uani 1 1 d . . . H38 H -0.0823 -0.2976 1.0225 0.051 Uiso 1 1 calc R . . C36 C 0.4801(6) 0.0489(6) 0.9792(3) 0.0571(13) Uiso 0.50 1 d P . . C37 C 0.4212(12) 0.0984(11) 1.0493(7) 0.103(3) Uiso 0.50 1 d P . . C38 C 0.5533(10) -0.0452(10) 0.9289(6) 0.090(3) Uiso 0.50 1 d P . . 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 Si1 0.0241(3) 0.0340(3) 0.0347(3) -0.0057(2) 0.0009(2) -0.0114(2) O1 0.0324(8) 0.0503(10) 0.0486(9) 0.0079(7) -0.0105(7) -0.0069(7) O2 0.0326(8) 0.0489(9) 0.0365(8) 0.0001(7) 0.0039(6) -0.0088(7) O3 0.0425(9) 0.0274(8) 0.0491(9) -0.0026(6) 0.0051(7) -0.0063(7) O4 0.0403(8) 0.0590(10) 0.0275(7) 0.0011(6) -0.0065(6) -0.0262(7) O5 0.0612(10) 0.0397(9) 0.0341(8) 0.0058(6) -0.0116(7) -0.0313(8) N1 0.0351(9) 0.0371(9) 0.0298(8) 0.0018(7) -0.0054(7) -0.0218(8) N2 0.0338(9) 0.0307(9) 0.0264(8) 0.0019(7) -0.0040(7) -0.0121(7) C1 0.0258(9) 0.0236(9) 0.0272(9) -0.0002(7) -0.0018(7) -0.0107(8) C2 0.0304(10) 0.0286(10) 0.0314(10) 0.0053(8) -0.0058(8) -0.0147(8) C3 0.0315(10) 0.0360(11) 0.0382(11) 0.0069(9) -0.0034(9) -0.0150(9) C4 0.0413(13) 0.0617(17) 0.0571(16) -0.0079(13) 0.0119(11) -0.0063(12) C5 0.0284(9) 0.0229(9) 0.0289(9) 0.0003(7) -0.0026(7) -0.0099(8) C6 0.0309(10) 0.0269(10) 0.0287(9) 0.0009(8) -0.0060(7) -0.0133(8) C7 0.0326(10) 0.0352(11) 0.0366(11) 0.0025(9) -0.0056(8) -0.0133(9) C8 0.0405(11) 0.0298(11) 0.0470(12) 0.0069(9) -0.0169(10) -0.0124(9) C9 0.0542(13) 0.0410(12) 0.0354(11) 0.0110(9) -0.0176(10) -0.0282(11) C10 0.0502(13) 0.0447(13) 0.0288(10) -0.0012(9) -0.0032(9) -0.0303(11) C11 0.0356(10) 0.0302(10) 0.0330(10) -0.0024(8) -0.0045(8) -0.0161(9) C12 0.0281(9) 0.0234(9) 0.0268(9) 0.0015(7) -0.0031(7) -0.0114(8) C13 0.0375(11) 0.0252(10) 0.0293(10) 0.0000(8) -0.0051(8) -0.0109(8) C14 0.0483(12) 0.0263(11) 0.0476(12) 0.0053(9) -0.0079(10) -0.0189(10) C15 0.0410(11) 0.0317(11) 0.0358(10) 0.0044(8) -0.0035(9) -0.0222(9) C16 0.0304(10) 0.0283(10) 0.0288(9) 0.0012(7) -0.0016(7) -0.0157(8) C17 0.0297(10) 0.0342(11) 0.0272(9) -0.0025(8) 0.0009(7) -0.0174(8) C18 0.0271(9) 0.0297(10) 0.0290(9) -0.0019(7) 0.0008(7) -0.0150(8) C19 0.0441(13) 0.0570(15) 0.0463(13) -0.0178(11) 0.0054(10) -0.0193(12) C20 0.0344(12) 0.0645(17) 0.0638(16) -0.0107(13) -0.0064(11) -0.0232(12) C21 0.0420(12) 0.0305(12) 0.0563(14) -0.0003(10) 0.0054(10) -0.0051(10) C22 0.0250(9) 0.0306(10) 0.0266(9) -0.0021(7) -0.0008(7) -0.0124(8) C23 0.0331(10) 0.0287(10) 0.0316(10) -0.0029(8) -0.0014(8) -0.0173(8) C24 0.0272(9) 0.0261(10) 0.0235(9) -0.0017(7) -0.0018(7) -0.0097(8) C25 0.0275(9) 0.0256(9) 0.0239(9) 0.0003(7) -0.0013(7) -0.0118(8) C26 0.0261(9) 0.0277(10) 0.0244(9) 0.0001(7) -0.0008(7) -0.0103(8) C27 0.0296(9) 0.0286(10) 0.0248(9) -0.0031(7) 0.0004(7) -0.0127(8) C28 0.0298(10) 0.0382(11) 0.0236(9) -0.0053(8) 0.0033(7) -0.0142(9) C29 0.0346(10) 0.0332(11) 0.0236(9) 0.0017(8) -0.0010(8) -0.0153(9) C30 0.0448(12) 0.0316(11) 0.0275(10) 0.0043(8) -0.0062(8) -0.0114(9) C31 0.0475(15) 0.0627(18) 0.079(2) 0.0336(15) -0.0118(14) -0.0118(13) C32 0.065(2) 0.077(2) 0.106(3) 0.049(2) -0.0330(19) -0.0103(18) C33 0.089(2) 0.0494(16) 0.0585(17) 0.0277(13) -0.0236(15) -0.0246(16) C34 0.0777(18) 0.0445(14) 0.0414(13) 0.0104(10) -0.0129(12) -0.0332(13) C35 0.0540(13) 0.0387(12) 0.0381(11) 0.0063(9) -0.0111(10) -0.0232(11) _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 Si1 C19 1.861(2) . ? Si1 C20 1.863(2) . ? Si1 C21 1.868(2) . ? Si1 C18 1.871(2) . ? O1 C3 1.204(2) . ? O2 C3 1.339(3) . ? O2 C4 1.444(3) . ? O3 C13 1.209(2) . ? O4 C28 1.209(2) . ? O5 C29 1.206(2) . ? O6 C36 1.404(7) . ? O6 H39 0.8400 . ? N1 C2 1.460(2) . ? N1 C5 1.473(2) . ? N1 H6 0.8800 . ? N2 C28 1.403(3) . ? N2 C29 1.412(2) . ? N2 C30 1.435(2) . ? C1 C25 1.538(2) . ? C1 C12 1.544(2) . ? C1 C2 1.552(2) . ? C1 H1 1.0000 . ? C2 C3 1.515(3) . ? C2 H2 1.0000 . ? C4 H3 0.9800 . ? C4 H4 0.9800 . ? C4 H5 0.9800 . ? C5 C6 1.521(2) . ? C5 C12 1.575(3) . ? C5 H7 1.0000 . ? C6 C11 1.393(3) . ? C6 C7 1.394(3) . ? C7 C8 1.386(3) . ? C7 H8 0.9500 . ? C8 C9 1.381(3) . ? C8 H9 0.9500 . ? C9 C10 1.382(3) . ? C9 H10 0.9500 . ? C10 C11 1.395(3) . ? C10 H11 0.9500 . ? C11 H12 0.9500 . ? C12 C13 1.527(3) . ? C12 C16 1.559(3) . ? C13 C14 1.510(3) . ? C14 C15 1.531(3) . ? C14 H13 0.9900 . ? C14 H14 0.9900 . ? C15 C16 1.540(3) . ? C15 H15 0.9900 . ? C15 H16 0.9900 . ? C16 C17 1.514(3) . ? C16 C23 1.549(3) . ? C17 C18 1.335(3) . ? C17 H17 0.9500 . ? C18 C22 1.533(3) . ? C19 H18 0.9800 . ? C19 H19 0.9800 . ? C19 H20 0.9800 . ? C20 H21 0.9800 . ? C20 H22 0.9800 . ? C20 H23 0.9800 . ? C21 H24 0.9800 . ? C21 H25 0.9800 . ? C21 H26 0.9800 . ? C22 C24 1.523(3) . ? C22 C23 1.536(3) . ? C22 H27 1.0000 . ? C23 H28 0.9900 . ? C23 H29 0.9900 . ? C24 C25 1.556(2) . ? C24 C27 1.568(2) . ? C24 H30 1.0000 . ? C25 C26 1.567(2) . ? C25 H31 1.0000 . ? C26 C29 1.502(3) . ? C26 C27 1.535(3) . ? C26 H32 1.0000 . ? C27 C28 1.494(3) . ? C27 H33 1.0000 . ? C30 C31 1.373(3) . ? C30 C35 1.376(3) . ? C31 C32 1.401(4) . ? C31 H34 0.9500 . ? C32 C33 1.353(5) . ? C32 H35 0.9500 . ? C33 C34 1.373(4) . ? C33 H36 0.9500 . ? C34 C35 1.396(3) . ? C34 H37 0.9500 . ? C35 H38 0.9500 . ? C36 C36 1.156(11) 2_657 ? C36 C37 1.292(11) . ? C36 C38 1.310(10) . ? C36 C38 1.497(11) 2_657 ? C36 C37 1.607(12) 2_657 ? C37 C38 0.624(13) 2_657 ? C37 C36 1.607(12) 2_657 ? C38 C37 0.624(13) 2_657 ? C38 C36 1.497(11) 2_657 ? 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 C19 Si1 C20 110.35(12) . . ? C19 Si1 C21 110.61(12) . . ? C20 Si1 C21 107.66(12) . . ? C19 Si1 C18 109.69(10) . . ? C20 Si1 C18 107.77(11) . . ? C21 Si1 C18 110.70(9) . . ? C3 O2 C4 115.01(18) . . ? C36 O6 H39 109.5 . . ? C2 N1 C5 110.87(14) . . ? C2 N1 H6 124.6 . . ? C5 N1 H6 124.6 . . ? C28 N2 C29 112.28(16) . . ? C28 N2 C30 123.90(17) . . ? C29 N2 C30 123.78(17) . . ? C25 C1 C12 118.41(15) . . ? C25 C1 C2 107.28(14) . . ? C12 C1 C2 103.84(14) . . ? C25 C1 H1 109.0 . . ? C12 C1 H1 109.0 . . ? C2 C1 H1 109.0 . . ? N1 C2 C3 111.09(16) . . ? N1 C2 C1 106.37(14) . . ? C3 C2 C1 116.84(17) . . ? N1 C2 H2 107.4 . . ? C3 C2 H2 107.4 . . ? C1 C2 H2 107.4 . . ? O1 C3 O2 124.2(2) . . ? O1 C3 C2 124.2(2) . . ? O2 C3 C2 111.34(17) . . ? O2 C4 H3 109.5 . . ? O2 C4 H4 109.5 . . ? H3 C4 H4 109.5 . . ? O2 C4 H5 109.5 . . ? H3 C4 H5 109.5 . . ? H4 C4 H5 109.5 . . ? N1 C5 C6 111.34(15) . . ? N1 C5 C12 105.53(14) . . ? C6 C5 C12 117.20(15) . . ? N1 C5 H7 107.5 . . ? C6 C5 H7 107.5 . . ? C12 C5 H7 107.5 . . ? C11 C6 C7 118.41(18) . . ? C11 C6 C5 119.78(17) . . ? C7 C6 C5 121.81(17) . . ? C8 C7 C6 121.1(2) . . ? C8 C7 H8 119.5 . . ? C6 C7 H8 119.5 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H9 120.0 . . ? C7 C8 H9 120.0 . . ? C8 C9 C10 119.96(19) . . ? C8 C9 H10 120.0 . . ? C10 C9 H10 120.0 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H11 119.9 . . ? C11 C10 H11 119.9 . . ? C6 C11 C10 120.41(19) . . ? C6 C11 H12 119.8 . . ? C10 C11 H12 119.8 . . ? C13 C12 C1 108.56(15) . . ? C13 C12 C16 101.30(15) . . ? C1 C12 C16 118.14(15) . . ? C13 C12 C5 110.84(15) . . ? C1 C12 C5 102.70(14) . . ? C16 C12 C5 115.31(15) . . ? O3 C13 C14 125.23(19) . . ? O3 C13 C12 124.51(18) . . ? C14 C13 C12 110.18(17) . . ? C13 C14 C15 104.74(16) . . ? C13 C14 H13 110.8 . . ? C15 C14 H13 110.8 . . ? C13 C14 H14 110.8 . . ? C15 C14 H14 110.8 . . ? H13 C14 H14 108.9 . . ? C14 C15 C16 104.61(16) . . ? C14 C15 H15 110.8 . . ? C16 C15 H15 110.8 . . ? C14 C15 H16 110.8 . . ? C16 C15 H16 110.8 . . ? H15 C15 H16 108.9 . . ? C17 C16 C15 113.63(15) . . ? C17 C16 C23 101.07(15) . . ? C15 C16 C23 111.87(15) . . ? C17 C16 C12 116.94(15) . . ? C15 C16 C12 103.09(15) . . ? C23 C16 C12 110.55(15) . . ? C18 C17 C16 113.93(17) . . ? C18 C17 H17 123.0 . . ? C16 C17 H17 123.0 . . ? C17 C18 C22 108.20(16) . . ? C17 C18 Si1 128.41(15) . . ? C22 C18 Si1 123.36(13) . . ? Si1 C19 H18 109.5 . . ? Si1 C19 H19 109.5 . . ? H18 C19 H19 109.5 . . ? Si1 C19 H20 109.5 . . ? H18 C19 H20 109.5 . . ? H19 C19 H20 109.5 . . ? Si1 C20 H21 109.5 . . ? Si1 C20 H22 109.5 . . ? H21 C20 H22 109.5 . . ? Si1 C20 H23 109.5 . . ? H21 C20 H23 109.5 . . ? H22 C20 H23 109.5 . . ? Si1 C21 H24 109.5 . . ? Si1 C21 H25 109.5 . . ? H24 C21 H25 109.5 . . ? Si1 C21 H26 109.5 . . ? H24 C21 H26 109.5 . . ? H25 C21 H26 109.5 . . ? C24 C22 C18 105.76(15) . . ? C24 C22 C23 114.67(15) . . ? C18 C22 C23 102.53(15) . . ? C24 C22 H27 111.1 . . ? C18 C22 H27 111.1 . . ? C23 C22 H27 111.1 . . ? C22 C23 C16 104.17(15) . . ? C22 C23 H28 110.9 . . ? C16 C23 H28 110.9 . . ? C22 C23 H29 110.9 . . ? C16 C23 H29 110.9 . . ? H28 C23 H29 108.9 . . ? C22 C24 C25 122.54(15) . . ? C22 C24 C27 123.37(16) . . ? C25 C24 C27 89.15(13) . . ? C22 C24 H30 106.6 . . ? C25 C24 H30 106.6 . . ? C27 C24 H30 106.6 . . ? C1 C25 C24 119.15(15) . . ? C1 C25 C26 106.38(14) . . ? C24 C25 C26 86.55(13) . . ? C1 C25 H31 113.8 . . ? C24 C25 H31 113.8 . . ? C26 C25 H31 113.8 . . ? C29 C26 C27 103.69(15) . . ? C29 C26 C25 117.87(16) . . ? C27 C26 C25 89.94(13) . . ? C29 C26 H32 114.1 . . ? C27 C26 H32 114.1 . . ? C25 C26 H32 114.1 . . ? C28 C27 C26 106.09(15) . . ? C28 C27 C24 113.85(15) . . ? C26 C27 C24 87.21(13) . . ? C28 C27 H33 115.4 . . ? C26 C27 H33 115.4 . . ? C24 C27 H33 115.4 . . ? O4 C28 N2 124.62(19) . . ? O4 C28 C27 127.93(19) . . ? N2 C28 C27 107.43(16) . . ? O5 C29 N2 124.31(18) . . ? O5 C29 C26 127.74(18) . . ? N2 C29 C26 107.94(16) . . ? C31 C30 C35 120.7(2) . . ? C31 C30 N2 120.0(2) . . ? C35 C30 N2 119.23(19) . . ? C30 C31 C32 118.4(3) . . ? C30 C31 H34 120.8 . . ? C32 C31 H34 120.8 . . ? C33 C32 C31 121.3(3) . . ? C33 C32 H35 119.4 . . ? C31 C32 H35 119.4 . . ? C32 C33 C34 120.2(2) . . ? C32 C33 H36 119.9 . . ? C34 C33 H36 119.9 . . ? C33 C34 C35 119.6(2) . . ? C33 C34 H37 120.2 . . ? C35 C34 H37 120.2 . . ? C30 C35 C34 119.8(2) . . ? C30 C35 H38 120.1 . . ? C34 C35 H38 120.1 . . ? C36 C36 C37 81.9(7) 2_657 . ? C36 C36 C38 74.5(7) 2_657 . ? C37 C36 C38 156.3(8) . . ? C36 C36 O6 119.3(7) 2_657 . ? C37 C36 O6 95.2(6) . . ? C38 C36 O6 95.0(6) . . ? C36 C36 C38 57.5(6) 2_657 2_657 ? C37 C36 C38 24.5(6) . 2_657 ? C38 C36 C38 131.9(5) . 2_657 ? O6 C36 C38 107.5(6) . 2_657 ? C36 C36 C37 52.7(6) 2_657 2_657 ? C37 C36 C37 134.6(5) . 2_657 ? C38 C36 C37 21.8(6) . 2_657 ? O6 C36 C37 106.2(6) . 2_657 ? C38 C36 C37 110.2(5) 2_657 2_657 ? C38 C37 C36 96.5(17) 2_657 . ? C38 C37 C36 51.2(14) 2_657 2_657 ? C36 C37 C36 45.4(5) . 2_657 ? C37 C38 C36 107.0(18) 2_657 . ? C37 C38 C36 59.0(15) 2_657 2_657 ? C36 C38 C36 48.1(5) . 2_657 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 C3 118.75(17) . . . . ? C5 N1 C2 C1 -9.4(2) . . . . ? C25 C1 C2 N1 -99.54(17) . . . . ? C12 C1 C2 N1 26.60(19) . . . . ? C25 C1 C2 C3 135.77(16) . . . . ? C12 C1 C2 C3 -98.09(18) . . . . ? C4 O2 C3 O1 -4.0(3) . . . . ? C4 O2 C3 C2 -178.66(19) . . . . ? N1 C2 C3 O1 12.1(3) . . . . ? C1 C2 C3 O1 134.4(2) . . . . ? N1 C2 C3 O2 -173.18(16) . . . . ? C1 C2 C3 O2 -50.9(2) . . . . ? C2 N1 C5 C6 -139.54(16) . . . . ? C2 N1 C5 C12 -11.4(2) . . . . ? N1 C5 C6 C11 -128.90(18) . . . . ? C12 C5 C6 C11 109.5(2) . . . . ? N1 C5 C6 C7 50.1(2) . . . . ? C12 C5 C6 C7 -71.5(2) . . . . ? C11 C6 C7 C8 -1.3(3) . . . . ? C5 C6 C7 C8 179.68(19) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C7 C8 C9 C10 0.1(3) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C7 C6 C11 C10 1.6(3) . . . . ? C5 C6 C11 C10 -179.33(17) . . . . ? C9 C10 C11 C6 -1.1(3) . . . . ? C25 C1 C12 C13 -156.21(16) . . . . ? C2 C1 C12 C13 85.03(17) . . . . ? C25 C1 C12 C16 -41.8(2) . . . . ? C2 C1 C12 C16 -160.51(16) . . . . ? C25 C1 C12 C5 86.37(18) . . . . ? C2 C1 C12 C5 -32.38(17) . . . . ? N1 C5 C12 C13 -88.45(17) . . . . ? C6 C5 C12 C13 36.1(2) . . . . ? N1 C5 C12 C1 27.33(18) . . . . ? C6 C5 C12 C1 151.90(16) . . . . ? N1 C5 C12 C16 157.21(15) . . . . ? C6 C5 C12 C16 -78.2(2) . . . . ? C1 C12 C13 O3 -28.4(3) . . . . ? C16 C12 C13 O3 -153.48(19) . . . . ? C5 C12 C13 O3 83.7(2) . . . . ? C1 C12 C13 C14 148.47(16) . . . . ? C16 C12 C13 C14 23.4(2) . . . . ? C5 C12 C13 C14 -99.45(18) . . . . ? O3 C13 C14 C15 177.0(2) . . . . ? C12 C13 C14 C15 0.1(2) . . . . ? C13 C14 C15 C16 -24.3(2) . . . . ? C14 C15 C16 C17 166.59(16) . . . . ? C14 C15 C16 C23 -79.74(19) . . . . ? C14 C15 C16 C12 39.05(19) . . . . ? C13 C12 C16 C17 -163.00(15) . . . . ? C1 C12 C16 C17 78.6(2) . . . . ? C5 C12 C16 C17 -43.3(2) . . . . ? C13 C12 C16 C15 -37.57(18) . . . . ? C1 C12 C16 C15 -155.93(16) . . . . ? C5 C12 C16 C15 82.16(18) . . . . ? C13 C12 C16 C23 82.13(17) . . . . ? C1 C12 C16 C23 -36.2(2) . . . . ? C5 C12 C16 C23 -158.14(15) . . . . ? C15 C16 C17 C18 133.51(18) . . . . ? C23 C16 C17 C18 13.5(2) . . . . ? C12 C16 C17 C18 -106.52(19) . . . . ? C16 C17 C18 C22 6.5(2) . . . . ? C16 C17 C18 Si1 -175.54(13) . . . . ? C19 Si1 C18 C17 -6.9(2) . . . . ? C20 Si1 C18 C17 113.25(19) . . . . ? C21 Si1 C18 C17 -129.26(19) . . . . ? C19 Si1 C18 C22 170.70(15) . . . . ? C20 Si1 C18 C22 -69.13(18) . . . . ? C21 Si1 C18 C22 48.36(18) . . . . ? C17 C18 C22 C24 96.45(18) . . . . ? Si1 C18 C22 C24 -81.60(17) . . . . ? C17 C18 C22 C23 -24.02(19) . . . . ? Si1 C18 C22 C23 157.94(13) . . . . ? C24 C22 C23 C16 -82.62(18) . . . . ? C18 C22 C23 C16 31.48(17) . . . . ? C17 C16 C23 C22 -27.43(17) . . . . ? C15 C16 C23 C22 -148.67(16) . . . . ? C12 C16 C23 C22 97.06(17) . . . . ? C18 C22 C24 C25 -68.3(2) . . . . ? C23 C22 C24 C25 43.9(2) . . . . ? C18 C22 C24 C27 178.23(16) . . . . ? C23 C22 C24 C27 -69.6(2) . . . . ? C12 C1 C25 C24 67.5(2) . . . . ? C2 C1 C25 C24 -175.55(15) . . . . ? C12 C1 C25 C26 162.79(15) . . . . ? C2 C1 C25 C26 -80.27(17) . . . . ? C22 C24 C25 C1 -42.9(2) . . . . ? C27 C24 C25 C1 87.08(17) . . . . ? C22 C24 C25 C26 -149.79(17) . . . . ? C27 C24 C25 C26 -19.77(13) . . . . ? C1 C25 C26 C29 155.31(16) . . . . ? C24 C25 C26 C29 -85.29(18) . . . . ? C1 C25 C26 C27 -99.19(15) . . . . ? C24 C25 C26 C27 20.21(14) . . . . ? C29 C26 C27 C28 -15.31(19) . . . . ? C25 C26 C27 C28 -134.06(15) . . . . ? C29 C26 C27 C24 98.72(15) . . . . ? C25 C26 C27 C24 -20.03(13) . . . . ? C22 C24 C27 C28 -104.1(2) . . . . ? C25 C24 C27 C28 126.55(16) . . . . ? C22 C24 C27 C26 149.55(17) . . . . ? C25 C24 C27 C26 20.18(14) . . . . ? C29 N2 C28 O4 -179.01(18) . . . . ? C30 N2 C28 O4 3.4(3) . . . . ? C29 N2 C28 C27 -0.5(2) . . . . ? C30 N2 C28 C27 -178.07(17) . . . . ? C26 C27 C28 O4 -171.34(19) . . . . ? C24 C27 C28 O4 94.5(2) . . . . ? C26 C27 C28 N2 10.18(19) . . . . ? C24 C27 C28 N2 -83.96(19) . . . . ? C28 N2 C29 O5 170.89(19) . . . . ? C30 N2 C29 O5 -11.5(3) . . . . ? C28 N2 C29 C26 -9.8(2) . . . . ? C30 N2 C29 C26 167.85(17) . . . . ? C27 C26 C29 O5 -165.4(2) . . . . ? C25 C26 C29 O5 -68.1(3) . . . . ? C27 C26 C29 N2 15.29(19) . . . . ? C25 C26 C29 N2 112.62(18) . . . . ? C28 N2 C30 C31 -45.6(3) . . . . ? C29 N2 C30 C31 137.1(3) . . . . ? C28 N2 C30 C35 131.2(2) . . . . ? C29 N2 C30 C35 -46.1(3) . . . . ? C35 C30 C31 C32 0.0(5) . . . . ? N2 C30 C31 C32 176.7(3) . . . . ? C30 C31 C32 C33 1.8(6) . . . . ? C31 C32 C33 C34 -2.0(6) . . . . ? C32 C33 C34 C35 0.5(5) . . . . ? C31 C30 C35 C34 -1.4(4) . . . . ? N2 C30 C35 C34 -178.2(2) . . . . ? C33 C34 C35 C30 1.2(4) . . . . ? C36 C36 C37 C38 3.2(17) 2_657 . . 2_657 ? C38 C36 C37 C38 7(4) . . . 2_657 ? O6 C36 C37 C38 122.1(16) . . . 2_657 ? C37 C36 C37 C38 3.2(17) 2_657 . . 2_657 ? C38 C36 C37 C36 4(2) . . . 2_657 ? O6 C36 C37 C36 118.9(7) . . . 2_657 ? C38 C36 C37 C36 -3.2(17) 2_657 . . 2_657 ? C37 C36 C37 C36 -0.004(2) 2_657 . . 2_657 ? C36 C36 C38 C37 -3.3(18) 2_657 . . 2_657 ? C37 C36 C38 C37 -7(4) . . . 2_657 ? O6 C36 C38 C37 -122.4(18) . . . 2_657 ? C38 C36 C38 C37 -3.3(18) 2_657 . . 2_657 ? C37 C36 C38 C36 -4(2) . . . 2_657 ? O6 C36 C38 C36 -119.0(7) . . . 2_657 ? C38 C36 C38 C36 0.000(1) 2_657 . . 2_657 ? C37 C36 C38 C36 3.3(18) 2_657 . . 2_657 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.642 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.053