# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_str715m _database_code_depnum_ccdc_archive 'CCDC 285438' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration syn _chemical_formula_moiety ? _chemical_formula_sum 'C43 H66 O6 Si3' _chemical_formula_weight 763.23 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.7933(14) _cell_length_b 16.163(2) _cell_length_c 13.5195(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.480(4) _cell_angle_gamma 90.00 _cell_volume 2351.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1728 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 17.40 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.335 _exptl_crystal_size_mid 0.204 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _Ratio_of_minimum_to_maximum_apparent_transmission 0.873207 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 12310 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.1947 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7080 _reflns_number_gt 2977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1813P)^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 0.3(4) _refine_ls_number_reflns 7080 _refine_ls_number_parameters 398 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2282 _refine_ls_R_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.3501 _refine_ls_wR_factor_gt 0.2684 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 1.0420(9) 0.9440(7) 0.8676(7) 0.060(3) Uani 1 1 d . . . C2 C 1.0071(11) 0.9601(9) 0.7676(9) 0.086(4) Uani 1 1 d . . . H2 H 0.9663 0.9182 0.7309 0.103 Uiso 1 1 calc R . . C3 C 1.0278(15) 1.0308(12) 0.7207(11) 0.108(5) Uani 1 1 d . . . H3 H 1.0020 1.0378 0.6540 0.129 Uiso 1 1 calc R . . C4 C 1.0871(15) 1.0916(9) 0.7732(16) 0.103(5) Uani 1 1 d . . . H4 H 1.1024 1.1412 0.7416 0.124 Uiso 1 1 calc R . . C5 C 1.1259(15) 1.0829(10) 0.8714(14) 0.110(5) Uani 1 1 d . . . H5 H 1.1658 1.1258 0.9068 0.132 Uiso 1 1 calc R . . C6 C 1.1042(11) 1.0101(7) 0.9149(9) 0.071(3) Uani 1 1 d . . . H6 H 1.1328 1.0035 0.9811 0.085 Uiso 1 1 calc R . . C7 C 0.9773(10) 0.8682(7) 1.0587(7) 0.058(3) Uani 1 1 d . . . C8 C 0.9215(13) 0.9445(10) 1.0811(10) 0.096(4) Uani 1 1 d . . . H8 H 0.9031 0.9810 1.0288 0.115 Uiso 1 1 calc R . . C9 C 0.8925(16) 0.9687(10) 1.1726(11) 0.119(6) Uani 1 1 d . . . H9 H 0.8549 1.0193 1.1834 0.143 Uiso 1 1 calc R . . C10 C 0.9237(18) 0.9113(14) 1.2516(12) 0.126(7) Uani 1 1 d . . . H10 H 0.9137 0.9277 1.3165 0.151 Uiso 1 1 calc R . . C11 C 0.9636(19) 0.8405(14) 1.2369(9) 0.133(7) Uani 1 1 d . . . H11 H 0.9732 0.8029 1.2890 0.160 Uiso 1 1 calc R . . C12 C 0.9959(14) 0.8161(8) 1.1359(9) 0.093(4) Uani 1 1 d . . . H12 H 1.0294 0.7641 1.1261 0.112 Uiso 1 1 calc R . . C13 C 1.1419(11) 0.7731(7) 0.9167(8) 0.070(3) Uani 1 1 d . . . C14 C 1.1074(15) 0.6808(9) 0.9493(12) 0.114(5) Uani 1 1 d . . . H14A H 1.0888 0.6809 1.0176 0.170 Uiso 1 1 calc R . . H14B H 1.1766 0.6448 0.9412 0.170 Uiso 1 1 calc R . . H14C H 1.0363 0.6617 0.9086 0.170 Uiso 1 1 calc R . . C15 C 1.1676(13) 0.7620(10) 0.8062(10) 0.106(5) Uani 1 1 d . . . H15A H 1.0934 0.7430 0.7692 0.159 Uiso 1 1 calc R . . H15B H 1.2326 0.7221 0.8011 0.159 Uiso 1 1 calc R . . H15C H 1.1926 0.8140 0.7798 0.159 Uiso 1 1 calc R . . C16 C 1.2594(11) 0.7999(9) 0.9762(11) 0.107(5) Uani 1 1 d . . . H16A H 1.2433 0.8055 1.0447 0.161 Uiso 1 1 calc R . . H16B H 1.2864 0.8521 0.9517 0.161 Uiso 1 1 calc R . . H16C H 1.3231 0.7592 0.9701 0.161 Uiso 1 1 calc R . . C17 C 0.7699(10) 0.8286(7) 0.8495(7) 0.066(3) Uani 1 1 d . . . H17 H 0.7717 0.8884 0.8621 0.079 Uiso 1 1 calc R . . C18 C 0.6817(13) 0.7892(10) 0.9190(9) 0.102(4) Uani 1 1 d . . . H18A H 0.7097 0.8016 0.9865 0.154 Uiso 1 1 calc R . . H18B H 0.6805 0.7304 0.9095 0.154 Uiso 1 1 calc R . . H18C H 0.5995 0.8110 0.9047 0.154 Uiso 1 1 calc R . . C19 C 0.7387(10) 0.8156(6) 0.7398(8) 0.064(3) Uani 1 1 d . . . C20 C 0.6136(9) 0.8521(8) 0.6974(7) 0.066(3) Uani 1 1 d . . . H20 H 0.5477 0.8297 0.7356 0.079 Uiso 1 1 calc R . . C21 C 0.3615(13) 0.9738(12) 0.6893(19) 0.182(10) Uani 1 1 d . . . H21A H 0.3612 0.9169 0.6688 0.273 Uiso 1 1 calc R . . H21B H 0.3353 1.0081 0.6337 0.273 Uiso 1 1 calc R . . H21C H 0.3055 0.9808 0.7405 0.273 Uiso 1 1 calc R . . C22 C 0.535(4) 1.025(4) 0.8687(15) 0.60(6) Uani 1 1 d D . . H22A H 0.5169 0.9759 0.9053 0.896 Uiso 1 1 calc R . . H22B H 0.4795 1.0683 0.8843 0.896 Uiso 1 1 calc R . . H22C H 0.6193 1.0416 0.8862 0.896 Uiso 1 1 calc R . . C27 C 0.5790(10) 0.8353(8) 0.5881(8) 0.074(3) Uani 1 1 d . . . C28 C 0.6776(10) 0.8629(7) 0.5210(7) 0.066(3) Uani 1 1 d . . . H28 H 0.7100 0.9170 0.5431 0.079 Uiso 1 1 calc R . . C29 C 0.7783(8) 0.8034(5) 0.5255(5) 0.0274(18) Uani 1 1 d . . . H29A H 0.7760 0.7736 0.5876 0.033 Uiso 1 1 calc R . . H29B H 0.7595 0.7636 0.4727 0.033 Uiso 1 1 calc R . . C30 C 0.8937(15) 0.8280(8) 0.5191(7) 0.079(4) Uani 1 1 d . . . C31 C 0.9856(11) 0.7603(8) 0.5280(7) 0.065(3) Uani 1 1 d . . . C32 C 1.1116(14) 0.7818(10) 0.5295(8) 0.093(4) Uani 1 1 d . . . H32 H 1.1354 0.8366 0.5225 0.112 Uiso 1 1 calc R . . C33 C 1.2020(17) 0.7184(17) 0.5418(13) 0.132(7) Uani 1 1 d . . . H33 H 1.2865 0.7303 0.5454 0.159 Uiso 1 1 calc R . . C34 C 1.1589(19) 0.6380(15) 0.5484(11) 0.118(6) Uani 1 1 d . . . H34 H 1.2182 0.5963 0.5566 0.142 Uiso 1 1 calc R . . C35 C 1.0355(18) 0.6144(12) 0.5439(11) 0.122(6) Uani 1 1 d . . . H35 H 1.0108 0.5593 0.5452 0.146 Uiso 1 1 calc R . . C36 C 0.9511(13) 0.6798(9) 0.5371(9) 0.084(4) Uani 1 1 d . . . H36 H 0.8670 0.6679 0.5389 0.100 Uiso 1 1 calc R . . C37 C 0.6252(14) 0.8691(9) 0.4124(9) 0.103(5) Uani 1 1 d . A . H37A H 0.6929 0.8751 0.3698 0.123 Uiso 1 1 calc R . . H37B H 0.5801 0.8190 0.3935 0.123 Uiso 1 1 calc R . . Si1 Si 1.0112(3) 0.84451(19) 0.92860(19) 0.0574(8) Uani 1 1 d . . . Si2 Si 0.5156(5) 1.0027(3) 0.7361(7) 0.179(3) Uani 1 1 d D . . O1 O 0.8934(6) 0.7976(4) 0.8692(4) 0.0598(19) Uani 1 1 d . . . O2 O 0.7319(8) 0.7254(5) 0.7226(6) 0.086(2) Uani 1 1 d . . . H2A H 0.7149 0.7165 0.6634 0.130 Uiso 1 1 calc R . . O3 O 0.6221(6) 0.9360(5) 0.7152(5) 0.066(2) Uani 1 1 d . . . O4 O 0.5466(7) 0.7515(5) 0.5696(6) 0.086(2) Uani 1 1 d . . . H4A H 0.5523 0.7257 0.6220 0.129 Uiso 1 1 calc R . . O5 O 0.9187(8) 0.8998(6) 0.5088(6) 0.092(3) Uani 1 1 d . . . O6 O 0.5455(4) 0.9374(2) 0.4003(3) 0.151(5) Uani 1 1 d . . . Si3 Si 0.4050(4) 0.9496(2) 0.3334(3) 0.086(2) Uani 0.50 1 d PR A 1 C38 C 0.3227(4) 1.0324(2) 0.3952(3) 0.129(11) Uiso 0.50 1 d PR A 1 H38A H 0.3714 1.0821 0.3964 0.193 Uiso 0.50 1 calc PR A 1 H38B H 0.3102 1.0159 0.4620 0.193 Uiso 0.50 1 calc PR A 1 H38C H 0.2437 1.0422 0.3596 0.193 Uiso 0.50 1 calc PR A 1 C39 C 0.3226(4) 0.8499(2) 0.3255(3) 0.22(2) Uiso 0.50 1 d PR A 1 H39A H 0.3711 0.8102 0.2925 0.332 Uiso 0.50 1 calc PR A 1 H39B H 0.2435 0.8569 0.2887 0.332 Uiso 0.50 1 calc PR A 1 H39C H 0.3101 0.8306 0.3911 0.332 Uiso 0.50 1 calc PR A 1 C40 C 0.4474(4) 0.9916(2) 0.2002(3) 0.131(11) Uiso 0.50 1 d PR A 1 C41 C 0.5383(4) 1.0704(2) 0.2539(3) 0.087(8) Uiso 0.50 1 d PR A 1 H41A H 0.6146 1.0477 0.2836 0.130 Uiso 0.50 1 calc PR A 1 H41B H 0.4943 1.0973 0.3039 0.130 Uiso 0.50 1 calc PR A 1 H41C H 0.5563 1.1099 0.2039 0.130 Uiso 0.50 1 calc PR A 1 C42 C 0.3308(4) 1.0193(2) 0.1536(3) 0.076(7) Uiso 0.50 1 d PR A 1 H42A H 0.2944 1.0588 0.1957 0.114 Uiso 0.50 1 calc PR A 1 H42B H 0.2758 0.9730 0.1427 0.114 Uiso 0.50 1 calc PR A 1 H42C H 0.3442 1.0448 0.0912 0.114 Uiso 0.50 1 calc PR A 1 C43 C 0.5529(4) 0.9287(2) 0.1730(3) 0.063(6) Uiso 0.50 1 d PR A 1 H43A H 0.6179 0.9277 0.2257 0.095 Uiso 0.50 1 calc PR A 1 H43B H 0.5864 0.9461 0.1127 0.095 Uiso 0.50 1 calc PR A 1 H43C H 0.5181 0.8743 0.1642 0.095 Uiso 0.50 1 calc PR A 1 Si3A Si 0.5075(4) 0.9697(2) 0.2810(3) 0.082(2) Uani 0.50 1 d PR A 2 C38A C 0.5361(4) 1.0751(2) 0.2192(3) 0.42(6) Uiso 0.50 1 d PR A 2 H38D H 0.5245 1.1189 0.2656 0.631 Uiso 0.50 1 calc PR A 2 H38E H 0.4786 1.0819 0.1620 0.631 Uiso 0.50 1 calc PR A 2 H38F H 0.6196 1.0770 0.1994 0.631 Uiso 0.50 1 calc PR A 2 C39A C 0.5345(4) 0.8869(2) 0.1783(3) 0.116(10) Uiso 0.50 1 d PR A 2 H39D H 0.5217 0.8325 0.2041 0.174 Uiso 0.50 1 calc PR A 2 H39E H 0.6180 0.8915 0.1590 0.174 Uiso 0.50 1 calc PR A 2 H39F H 0.4770 0.8964 0.1216 0.174 Uiso 0.50 1 calc PR A 2 C40A C 0.3187(4) 0.9439(2) 0.2755(3) 0.142(13) Uiso 0.50 1 d PR A 2 C42A C 0.2699(4) 1.0102(2) 0.3719(3) 0.089(7) Uiso 0.50 1 d PR A 2 H42D H 0.2831 1.0669 0.3544 0.134 Uiso 0.50 1 calc PR A 2 H42E H 0.3174 0.9977 0.4331 0.134 Uiso 0.50 1 calc PR A 2 H42F H 0.1833 1.0013 0.3797 0.134 Uiso 0.50 1 calc PR A 2 C41A C 0.2986(4) 0.8581(2) 0.3026(3) 0.085(8) Uiso 0.50 1 d PR A 2 H41D H 0.3547 0.8436 0.3584 0.128 Uiso 0.50 1 calc PR A 2 H41E H 0.3132 0.8229 0.2475 0.128 Uiso 0.50 1 calc PR A 2 H41F H 0.2145 0.8512 0.3196 0.128 Uiso 0.50 1 calc PR A 2 C43A C 0.2441(4) 0.9975(2) 0.1835(3) 0.137(12) Uiso 0.50 1 d PR A 2 H43D H 0.2766 1.0528 0.1829 0.206 Uiso 0.50 1 calc PR A 2 H43E H 0.1570 0.9994 0.1934 0.206 Uiso 0.50 1 calc PR A 2 H43F H 0.2558 0.9711 0.1213 0.206 Uiso 0.50 1 calc PR A 2 C600 C 0.5575(4) 1.0936(2) 0.7396(3) 0.261(15) Uiso 1 1 d R . . C602 C 0.5511(4) 1.1026(2) 0.6188(3) 0.214(10) Uiso 1 1 d R . . H60A H 0.4680 1.0916 0.5915 0.321 Uiso 1 1 calc R . . H60B H 0.6072 1.0638 0.5925 0.321 Uiso 1 1 calc R . . H60C H 0.5744 1.1578 0.6016 0.321 Uiso 1 1 calc R . . C601 C 0.4741(4) 1.1639(2) 0.7742(3) 0.204(10) Uiso 1 1 d R . . H60D H 0.3899 1.1547 0.7482 0.306 Uiso 1 1 calc R . . H60E H 0.5027 1.2159 0.7505 0.306 Uiso 1 1 calc R . . H60F H 0.4779 1.1646 0.8454 0.306 Uiso 1 1 calc R . . C603 C 0.6907(4) 1.1113(2) 0.7830(3) 0.260(14) Uiso 1 1 d R . . H60G H 0.7452 1.0686 0.7628 0.390 Uiso 1 1 calc R . . H60H H 0.6926 1.1125 0.8541 0.390 Uiso 1 1 calc R . . H60I H 0.7174 1.1638 0.7592 0.390 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 C1 0.062(7) 0.073(8) 0.045(6) 0.020(6) 0.003(5) 0.001(6) C2 0.085(9) 0.100(11) 0.071(9) 0.007(8) 0.005(7) -0.019(7) C3 0.124(12) 0.124(14) 0.076(10) 0.048(10) 0.010(9) -0.016(11) C4 0.104(12) 0.064(10) 0.148(16) 0.041(10) 0.059(11) 0.026(9) C5 0.123(13) 0.097(13) 0.115(13) -0.002(10) 0.035(11) -0.013(9) C6 0.082(8) 0.054(8) 0.081(8) 0.001(7) 0.026(7) -0.003(6) C7 0.069(7) 0.062(8) 0.043(6) 0.015(5) 0.001(5) -0.002(6) C8 0.098(10) 0.119(13) 0.071(9) -0.009(8) 0.018(7) -0.017(9) C9 0.161(15) 0.123(13) 0.080(10) 0.032(10) 0.053(10) 0.024(11) C10 0.174(17) 0.123(15) 0.086(12) -0.028(12) 0.045(11) -0.074(14) C11 0.23(2) 0.131(16) 0.037(7) 0.001(9) -0.008(9) -0.057(15) C12 0.137(12) 0.068(9) 0.078(9) -0.017(7) 0.028(8) -0.027(8) C13 0.084(8) 0.056(8) 0.067(7) -0.011(6) -0.003(6) 0.004(6) C14 0.143(13) 0.077(10) 0.125(12) 0.022(9) 0.030(10) 0.032(9) C15 0.115(11) 0.117(12) 0.088(9) -0.013(9) 0.021(8) 0.026(9) C16 0.054(8) 0.126(12) 0.139(12) -0.011(10) -0.011(8) 0.024(8) C17 0.060(7) 0.075(8) 0.060(6) -0.016(6) -0.012(5) -0.008(6) C18 0.112(10) 0.122(12) 0.075(8) 0.013(8) 0.019(8) -0.011(9) C19 0.078(8) 0.044(7) 0.067(7) -0.004(5) -0.018(6) 0.009(5) C20 0.054(7) 0.074(9) 0.070(6) -0.009(7) -0.002(5) 0.000(6) C21 0.053(10) 0.143(16) 0.35(3) 0.006(17) 0.052(13) -0.002(9) C22 0.48(7) 0.98(14) 0.31(5) -0.36(7) -0.07(5) 0.50(9) C27 0.075(8) 0.083(9) 0.060(6) -0.005(7) -0.013(6) -0.007(7) C28 0.082(8) 0.067(8) 0.046(6) 0.001(5) -0.016(6) -0.005(6) C29 0.030(5) 0.026(5) 0.024(4) -0.001(3) -0.009(3) 0.002(4) C30 0.136(14) 0.055(9) 0.045(6) 0.012(6) 0.001(6) -0.006(9) C31 0.071(9) 0.080(10) 0.044(6) 0.007(6) 0.008(5) 0.008(7) C32 0.090(11) 0.125(12) 0.066(8) -0.006(8) 0.014(7) 0.014(10) C33 0.091(12) 0.20(2) 0.111(13) -0.013(14) 0.024(9) 0.055(16) C34 0.113(17) 0.154(19) 0.090(10) -0.006(11) 0.035(10) 0.040(13) C35 0.105(14) 0.148(16) 0.116(12) -0.017(11) 0.033(10) 0.040(13) C36 0.072(9) 0.083(10) 0.094(10) 0.010(8) -0.002(7) 0.022(8) C37 0.116(11) 0.113(12) 0.072(8) -0.014(8) -0.043(7) 0.012(9) Si1 0.0668(19) 0.063(2) 0.0408(14) 0.0072(15) -0.0041(12) -0.0027(16) Si2 0.084(3) 0.121(4) 0.329(9) -0.127(5) -0.016(4) 0.023(3) O1 0.069(5) 0.066(5) 0.041(3) 0.005(3) -0.011(3) -0.014(4) O2 0.101(6) 0.067(6) 0.088(6) -0.009(4) -0.018(5) -0.007(4) O3 0.064(5) 0.063(5) 0.070(5) -0.018(4) -0.003(4) 0.019(4) O4 0.082(5) 0.087(7) 0.087(5) -0.017(5) -0.009(4) -0.017(5) O5 0.100(7) 0.085(7) 0.090(6) 0.008(5) 0.003(5) 0.002(5) O6 0.201(11) 0.111(8) 0.124(8) -0.011(6) -0.097(8) 0.072(8) Si3 0.089(5) 0.092(6) 0.078(5) 0.021(4) 0.007(4) 0.017(4) Si3A 0.086(5) 0.096(6) 0.064(4) 0.002(4) -0.006(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.390(15) . ? C1 C2 1.400(15) . ? C1 Si1 1.848(11) . ? C2 C3 1.333(19) . ? C3 C4 1.34(2) . ? C4 C5 1.37(2) . ? C5 C6 1.344(18) . ? C7 C12 1.344(15) . ? C7 C8 1.415(17) . ? C7 Si1 1.864(10) . ? C8 C9 1.358(18) . ? C9 C10 1.43(2) . ? C10 C11 1.24(2) . ? C11 C12 1.49(2) . ? C13 C16 1.512(16) . ? C13 C15 1.551(16) . ? C13 C14 1.606(18) . ? C13 Si1 1.840(12) . ? C17 O1 1.430(12) . ? C17 C19 1.509(13) . ? C17 C18 1.528(16) . ? C19 O2 1.477(12) . ? C19 C20 1.543(14) . ? C20 O3 1.378(13) . ? C20 C27 1.520(14) . ? C21 Si2 1.794(17) . ? C22 Si2 1.823(10) . ? C27 O4 1.417(14) . ? C27 C28 1.519(15) . ? C28 C29 1.449(13) . ? C28 C37 1.534(14) . ? C29 C30 1.317(16) . ? C30 O5 1.201(13) . ? C30 C31 1.476(17) . ? C31 C36 1.360(16) . ? C31 C32 1.403(17) . ? C32 C33 1.41(2) . ? C33 C34 1.39(2) . ? C34 C35 1.38(2) . ? C35 C36 1.394(19) . ? C37 O6 1.401(14) . ? Si1 O1 1.635(7) . ? Si2 C600 1.537(7) . ? Si2 O3 1.618(8) . ? O6 Si3A 1.7148 . ? O6 Si3 1.7152 . ? Si3 C39 1.8405 . ? Si3 C38 1.8422 . ? Si3 C40 2.0096 . ? C40 C42 1.4345 . ? C40 C43 1.5906 . ? C40 C41 1.7327 . ? Si3A C38A 1.9330 . ? Si3A C39A 1.9669 . ? Si3A C40A 2.0756 . ? C40A C41A 1.4551 . ? C40A C43A 1.6701 . ? C40A C42A 1.7964 . ? C600 C603 1.5359 . ? C600 C601 1.5443 . ? C600 C602 1.6350 . ? 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 C6 C1 C2 112.6(11) . . ? C6 C1 Si1 124.1(8) . . ? C2 C1 Si1 123.3(10) . . ? C3 C2 C1 125.2(14) . . ? C2 C3 C4 117.8(14) . . ? C3 C4 C5 122.3(14) . . ? C6 C5 C4 117.7(15) . . ? C5 C6 C1 124.5(13) . . ? C12 C7 C8 114.8(11) . . ? C12 C7 Si1 125.1(10) . . ? C8 C7 Si1 120.0(8) . . ? C9 C8 C7 125.3(14) . . ? C8 C9 C10 115.8(16) . . ? C11 C10 C9 122.7(16) . . ? C10 C11 C12 119.9(16) . . ? C7 C12 C11 121.0(14) . . ? C16 C13 C15 109.9(10) . . ? C16 C13 C14 108.8(11) . . ? C15 C13 C14 102.7(10) . . ? C16 C13 Si1 113.0(8) . . ? C15 C13 Si1 110.7(8) . . ? C14 C13 Si1 111.3(8) . . ? O1 C17 C19 105.5(8) . . ? O1 C17 C18 110.9(9) . . ? C19 C17 C18 116.4(9) . . ? O2 C19 C17 107.3(8) . . ? O2 C19 C20 106.7(9) . . ? C17 C19 C20 115.7(9) . . ? O3 C20 C27 110.7(9) . . ? O3 C20 C19 105.4(8) . . ? C27 C20 C19 115.8(9) . . ? O4 C27 C28 110.5(10) . . ? O4 C27 C20 112.4(9) . . ? C28 C27 C20 113.5(8) . . ? C29 C28 C27 109.8(9) . . ? C29 C28 C37 107.7(9) . . ? C27 C28 C37 111.6(10) . . ? C30 C29 C28 120.5(9) . . ? O5 C30 C29 121.4(13) . . ? O5 C30 C31 124.8(14) . . ? C29 C30 C31 113.8(11) . . ? C36 C31 C32 120.5(12) . . ? C36 C31 C30 122.0(12) . . ? C32 C31 C30 117.5(13) . . ? C31 C32 C33 118.8(16) . . ? C34 C33 C32 117.1(18) . . ? C35 C34 C33 125.7(18) . . ? C34 C35 C36 114.6(17) . . ? C31 C36 C35 123.3(14) . . ? O6 C37 C28 109.9(10) . . ? O1 Si1 C13 103.8(4) . . ? O1 Si1 C1 110.1(4) . . ? C13 Si1 C1 109.9(5) . . ? O1 Si1 C7 110.9(4) . . ? C13 Si1 C7 114.8(5) . . ? C1 Si1 C7 107.3(5) . . ? C600 Si2 O3 115.5(5) . . ? C600 Si2 C21 121.5(7) . . ? O3 Si2 C21 114.6(7) . . ? C600 Si2 C22 77(2) . . ? O3 Si2 C22 105.8(11) . . ? C21 Si2 C22 115(2) . . ? C17 O1 Si1 127.3(6) . . ? C20 O3 Si2 130.4(7) . . ? C37 O6 Si3A 116.7(5) . . ? C37 O6 Si3 131.5(5) . . ? Si3A O6 Si3 48.1 . . ? O6 Si3 C39 109.4 . . ? O6 Si3 C38 106.4 . . ? C39 Si3 C38 114.5 . . ? O6 Si3 C40 105.0 . . ? C39 Si3 C40 112.7 . . ? C38 Si3 C40 108.3 . . ? C42 C40 C43 135.9 . . ? C42 C40 C41 113.7 . . ? C43 C40 C41 100.0 . . ? C42 C40 Si3 104.2 . . ? C43 C40 Si3 102.0 . . ? C41 C40 Si3 91.9 . . ? O6 Si3A C38A 129.8 . . ? O6 Si3A C39A 114.8 . . ? C38A Si3A C39A 104.9 . . ? O6 Si3A C40A 97.7 . . ? C38A Si3A C40A 110.6 . . ? C39A Si3A C40A 92.1 . . ? C41A C40A C43A 127.5 . . ? C41A C40A C42A 109.1 . . ? C43A C40A C42A 94.6 . . ? C41A C40A Si3A 110.4 . . ? C43A C40A Si3A 109.7 . . ? C42A C40A Si3A 101.4 . . ? C603 C600 Si2 117.0(3) . . ? C603 C600 C601 107.3 . . ? Si2 C600 C601 122.3(3) . . ? C603 C600 C602 109.3 . . ? Si2 C600 C602 93.7(4) . . ? C601 C600 C602 104.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.399 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.069 data_str848m _database_code_depnum_ccdc_archive 'CCDC 762867' #TrackingRef '282_web_deposit_cif_file_0_JoseA.Martinez_1264091012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rmad _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 O8 Si2' _chemical_formula_sum 'C34 H52 O8 Si2' _chemical_formula_weight 644.94 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' 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' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 19 _symmetry_space_group_name_H-M P212121 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 14.316(3) _cell_length_b 15.960(4) _cell_length_c 16.397(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3746.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0015 _exptl_absorpt_correction_T_max 0.710216 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21072 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6585 _reflns_number_gt 3659 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_number_reflns 6585 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.2038 _refine_ls_goodness_of_fit_ref 1.300 _refine_ls_restrained_S_all 1.300 _refine_ls_shift/su_max 0.158 _refine_ls_shift/su_mean 0.006 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 0.62460(14) 0.28647(12) 0.96071(12) 0.0842(6) Uani 1 1 d . . . O1 O 0.6781(4) 0.3587(3) 0.9061(2) 0.0918(14) Uani 1 1 d . . . C1 C 0.7135(4) 0.4358(4) 0.9283(4) 0.0722(17) Uani 1 1 d . . . H1A H 0.7812 0.4341 0.9259 0.087 Uiso 1 1 calc R . . H1B H 0.6956 0.4480 0.9842 0.087 Uiso 1 1 calc R . . Si2 Si 0.94674(13) 0.49462(13) 0.7811(2) 0.1447(13) Uani 1 1 d . . . O2 O 0.5835(3) 0.5242(2) 0.8971(3) 0.0741(12) Uani 1 1 d . . . C2 C 0.6787(3) 0.5031(3) 0.8743(4) 0.0611(15) Uani 1 1 d . . . H2 H 0.7184 0.5527 0.8805 0.073 Uiso 1 1 calc R . . C3 C 0.6742(3) 0.4791(3) 0.7851(3) 0.0540(14) Uani 1 1 d . . . H3 H 0.6274 0.4348 0.7790 0.065 Uiso 1 1 calc R . . O3 O 0.6324(3) 0.6205(3) 0.9842(3) 0.0943(15) Uani 1 1 d . . . O4 O 0.8347(2) 0.5081(2) 0.7676(2) 0.0599(9) Uani 1 1 d . . . C4 C 0.7636(3) 0.4477(3) 0.7526(4) 0.0536(14) Uani 1 1 d . . . H4 H 0.7798 0.3946 0.7790 0.064 Uiso 1 1 calc R . . O5 O 0.6155(2) 0.3541(2) 0.6735(2) 0.0663(10) Uani 1 1 d . . . C5 C 0.7529(4) 0.4344(3) 0.6605(3) 0.0547(14) Uani 1 1 d . . . H5 H 0.8163 0.4315 0.6382 0.066 Uiso 1 1 calc R . . O6 O 0.7093(3) 0.5045(2) 0.6224(2) 0.0711(11) Uani 1 1 d . . . C6 C 0.7042(4) 0.3568(3) 0.6331(4) 0.0607(15) Uani 1 1 d . . . H6 H 0.6938 0.3602 0.5741 0.073 Uiso 1 1 calc R . . O7 O 0.6180(4) 0.6135(3) 0.6246(3) 0.1083(17) Uani 1 1 d . . . C7 C 0.7599(4) 0.2787(4) 0.6516(4) 0.0800(18) Uani 1 1 d . . . H7A H 0.7236 0.2301 0.6378 0.120 Uiso 1 1 calc R . . H7B H 0.7750 0.2773 0.7087 0.120 Uiso 1 1 calc R . . H7C H 0.8164 0.2789 0.6202 0.120 Uiso 1 1 calc R . . O8 O 0.6425(2) 0.5509(2) 0.7420(3) 0.0684(10) Uani 1 1 d . . . C8 C 0.6546(4) 0.5575(4) 0.6607(4) 0.0723(17) Uani 1 1 d . . . C9 C 0.5450(5) 0.3086(4) 0.6337(4) 0.091(2) Uani 1 1 d . . . H9A H 0.5587 0.2492 0.6363 0.109 Uiso 1 1 calc R . . H9B H 0.5422 0.3249 0.5767 0.109 Uiso 1 1 calc R . . C10 C 0.4522(5) 0.3262(4) 0.6745(4) 0.0745(18) Uani 1 1 d . . . C11 C 0.4223(5) 0.4059(6) 0.6891(5) 0.108(3) Uani 1 1 d . . . H11 H 0.4590 0.4507 0.6721 0.130 Uiso 1 1 calc R . . C12 C 0.3376(5) 0.4222(6) 0.7293(6) 0.119(3) Uani 1 1 d . . . H12 H 0.3175 0.4770 0.7373 0.143 Uiso 1 1 calc R . . C13 C 0.2868(6) 0.3585(7) 0.7557(6) 0.128(3) Uani 1 1 d . . . H13 H 0.2319 0.3682 0.7845 0.154 Uiso 1 1 calc R . . C14 C 0.3167(6) 0.2758(6) 0.7398(6) 0.116(3) Uani 1 1 d . . . H14 H 0.2796 0.2307 0.7553 0.139 Uiso 1 1 calc R . . C15 C 0.3996(5) 0.2623(5) 0.7019(4) 0.095(2) Uani 1 1 d . . . H15 H 0.4205 0.2076 0.6947 0.114 Uiso 1 1 calc R . . C16 C 0.9745(6) 0.3874(4) 0.8118(7) 0.144(4) Uani 1 1 d . . . H16A H 0.9331 0.3703 0.8548 0.216 Uiso 1 1 calc R . . H16B H 1.0379 0.3850 0.8309 0.216 Uiso 1 1 calc R . . H16C H 0.9672 0.3506 0.7660 0.216 Uiso 1 1 calc R . . C17 C 1.0057(6) 0.5227(9) 0.6616(5) 0.175(6) Uani 1 1 d . . . H17A H 1.0524 0.5656 0.6670 0.262 Uiso 1 1 calc R . . H17B H 0.9571 0.5419 0.6259 0.262 Uiso 1 1 calc R . . H17C H 1.0336 0.4730 0.6393 0.262 Uiso 1 1 calc R . . C18 C 0.9974(6) 0.5762(5) 0.8178(13) 0.240(10) Uani 1 1 d . . . C19 C 0.9780(7) 0.6611(4) 0.7807(7) 0.142(4) Uani 1 1 d . . . H19A H 0.9121 0.6671 0.7715 0.213 Uiso 1 1 calc R . . H19B H 1.0106 0.6660 0.7298 0.213 Uiso 1 1 calc R . . H19C H 0.9988 0.7042 0.8173 0.213 Uiso 1 1 calc R . . C20 C 1.1101(6) 0.5663(7) 0.8200(10) 0.225(8) Uani 1 1 d . . . H20A H 1.1334 0.5868 0.8712 0.338 Uiso 1 1 calc R . . H20B H 1.1372 0.5980 0.7763 0.338 Uiso 1 1 calc R . . H20C H 1.1263 0.5083 0.8140 0.338 Uiso 1 1 calc R . . C21 C 0.9493(8) 0.5601(8) 0.9225(5) 0.176(5) Uani 1 1 d . . . H21A H 0.8963 0.5960 0.9304 0.264 Uiso 1 1 calc R . . H21B H 0.9964 0.5733 0.9621 0.264 Uiso 1 1 calc R . . H21C H 0.9305 0.5027 0.9288 0.264 Uiso 1 1 calc R . . C22 C 0.5692(5) 0.5829(4) 0.9522(4) 0.0676(16) Uani 1 1 d . . . C23 C 0.4703(5) 0.5955(4) 0.9725(4) 0.0749(17) Uani 1 1 d . . . C24 C 0.4016(5) 0.5435(5) 0.9417(5) 0.091(2) Uani 1 1 d . . . H24 H 0.4175 0.5011 0.9053 0.109 Uiso 1 1 calc R . . C25 C 0.3096(6) 0.5539(7) 0.9644(7) 0.118(3) Uani 1 1 d . . . H25 H 0.2633 0.5190 0.9438 0.142 Uiso 1 1 calc R . . C26 C 0.2880(7) 0.6151(8) 1.0167(7) 0.127(4) Uani 1 1 d . . . H26 H 0.2258 0.6223 1.0314 0.152 Uiso 1 1 calc R . . C27 C 0.3525(9) 0.6669(7) 1.0490(6) 0.126(3) Uani 1 1 d . . . H27 H 0.3341 0.7082 1.0856 0.151 Uiso 1 1 calc R . . C28 C 0.4482(6) 0.6591(5) 1.0277(4) 0.095(2) Uani 1 1 d . . . H28 H 0.4936 0.6944 1.0494 0.114 Uiso 1 1 calc R . . C29 C 0.6644(8) 0.2947(6) 1.0673(5) 0.151(4) Uani 1 1 d . . . H29A H 0.6326 0.3403 1.0935 0.227 Uiso 1 1 calc R . . H29B H 0.7305 0.3047 1.0683 0.227 Uiso 1 1 calc R . . H29C H 0.6508 0.2434 1.0955 0.227 Uiso 1 1 calc R . . C30 C 0.4977(6) 0.2996(6) 0.9548(7) 0.145(4) Uani 1 1 d . . . H30A H 0.4690 0.2466 0.9428 0.217 Uiso 1 1 calc R . . H30B H 0.4828 0.3390 0.9125 0.217 Uiso 1 1 calc R . . H30C H 0.4747 0.3201 1.0060 0.217 Uiso 1 1 calc R . . C31 C 0.6577(5) 0.1860(4) 0.9147(5) 0.095(2) Uani 1 1 d . . . C32 C 0.6135(6) 0.1132(5) 0.9648(6) 0.130(3) Uani 1 1 d . . . H32A H 0.6378 0.1140 1.0194 0.195 Uiso 1 1 calc R . . H32B H 0.6286 0.0606 0.9395 0.195 Uiso 1 1 calc R . . H32C H 0.5469 0.1200 0.9664 0.195 Uiso 1 1 calc R . . C33 C 0.6161(7) 0.1817(5) 0.8273(5) 0.116(3) Uani 1 1 d . . . H33A H 0.6326 0.1293 0.8025 0.175 Uiso 1 1 calc R . . H33B H 0.6406 0.2269 0.7951 0.175 Uiso 1 1 calc R . . H33C H 0.5493 0.1864 0.8301 0.175 Uiso 1 1 calc R . . C34 C 0.7649(7) 0.1794(8) 0.9064(8) 0.172(5) Uani 1 1 d . . . H34A H 0.7810 0.1263 0.8827 0.258 Uiso 1 1 calc R . . H34B H 0.7932 0.1841 0.9593 0.258 Uiso 1 1 calc R . . H34C H 0.7873 0.2238 0.8720 0.258 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 0.0979(13) 0.0780(12) 0.0767(13) 0.0033(10) -0.0012(10) -0.0141(10) O1 0.150(4) 0.073(3) 0.053(3) 0.002(2) -0.013(2) -0.035(3) C1 0.078(4) 0.067(4) 0.071(4) -0.016(3) -0.010(3) -0.022(3) Si2 0.0545(10) 0.0635(12) 0.316(4) 0.0081(19) -0.0494(16) 0.0010(10) O2 0.071(2) 0.072(3) 0.079(3) -0.025(2) 0.010(2) -0.016(2) C2 0.051(3) 0.054(3) 0.078(4) -0.020(3) 0.001(3) -0.015(3) C3 0.055(3) 0.056(3) 0.051(3) -0.009(3) -0.005(2) -0.012(3) O3 0.109(4) 0.091(3) 0.083(3) -0.043(3) -0.004(3) 0.001(3) O4 0.0480(18) 0.0436(18) 0.088(3) -0.0040(19) -0.0010(17) -0.0067(16) C4 0.043(3) 0.042(3) 0.075(4) -0.004(3) -0.006(3) -0.005(2) O5 0.057(2) 0.076(3) 0.066(2) -0.011(2) 0.0022(19) -0.0164(19) C5 0.057(3) 0.051(3) 0.056(4) -0.002(3) 0.017(3) 0.004(2) O6 0.093(3) 0.059(2) 0.061(3) 0.015(2) 0.011(2) 0.010(2) C6 0.062(3) 0.055(3) 0.066(4) -0.002(3) 0.007(3) -0.006(3) O7 0.120(4) 0.090(3) 0.114(4) 0.030(3) -0.007(3) 0.040(3) C7 0.090(4) 0.054(4) 0.096(5) 0.000(3) 0.010(4) 0.005(3) O8 0.068(2) 0.061(2) 0.077(3) -0.001(2) 0.003(2) 0.0140(18) C8 0.070(4) 0.076(4) 0.071(5) 0.018(4) 0.002(3) -0.001(4) C9 0.092(5) 0.100(5) 0.079(5) -0.031(4) -0.004(4) -0.029(4) C10 0.080(4) 0.084(5) 0.060(4) -0.006(3) -0.008(3) -0.031(4) C11 0.084(5) 0.107(7) 0.134(7) 0.039(5) -0.027(5) -0.031(5) C12 0.078(5) 0.112(6) 0.168(9) 0.041(6) 0.010(5) 0.010(5) C13 0.079(5) 0.140(8) 0.166(9) 0.033(7) 0.040(6) 0.002(6) C14 0.081(5) 0.117(7) 0.148(8) 0.046(6) -0.008(5) -0.017(5) C15 0.091(5) 0.090(5) 0.103(6) 0.020(4) -0.012(4) -0.019(4) C16 0.101(5) 0.059(4) 0.271(13) -0.023(6) -0.077(7) 0.013(4) C17 0.106(6) 0.329(17) 0.089(7) -0.051(9) 0.048(5) -0.011(8) C18 0.089(6) 0.078(6) 0.55(3) 0.046(10) -0.151(11) -0.026(5) C19 0.161(8) 0.061(5) 0.204(11) 0.007(6) -0.047(7) -0.028(5) C20 0.095(6) 0.147(9) 0.43(2) -0.014(11) -0.122(10) -0.036(6) C21 0.184(10) 0.302(16) 0.041(5) -0.025(7) -0.001(5) -0.032(11) C22 0.087(5) 0.054(3) 0.062(4) -0.005(3) -0.007(3) -0.003(3) C23 0.086(5) 0.081(4) 0.058(4) 0.011(3) 0.010(3) 0.017(4) C24 0.065(4) 0.102(5) 0.105(6) 0.010(4) 0.002(4) 0.013(4) C25 0.099(7) 0.127(7) 0.129(8) 0.024(7) -0.002(6) 0.017(5) C26 0.098(7) 0.152(10) 0.131(9) 0.061(8) 0.034(6) 0.036(7) C27 0.161(9) 0.125(7) 0.092(7) 0.008(6) 0.034(6) 0.044(7) C28 0.121(6) 0.102(5) 0.062(4) -0.014(4) 0.028(4) 0.025(5) C29 0.230(11) 0.147(8) 0.077(6) 0.010(5) 0.012(6) -0.073(8) C30 0.105(6) 0.161(9) 0.169(9) -0.019(8) 0.009(6) 0.014(6) C31 0.080(5) 0.090(5) 0.114(6) 0.026(4) -0.002(4) -0.002(4) C32 0.145(7) 0.093(5) 0.152(8) 0.038(6) 0.032(6) -0.014(5) C33 0.184(8) 0.074(5) 0.091(6) 0.003(4) -0.005(6) -0.027(5) C34 0.114(7) 0.200(12) 0.202(12) 0.011(9) -0.003(7) 0.051(7) _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 O1 1.649(5) . ? Si1 C30 1.832(8) . ? Si1 C31 1.835(8) . ? Si1 C29 1.842(9) . ? O1 C1 1.379(7) . ? C1 C2 1.478(8) . ? Si2 C18 1.608(10) . ? Si2 O4 1.633(4) . ? Si2 C16 1.828(8) . ? Si2 C17 2.179(9) . ? O2 C22 1.318(7) . ? O2 C2 1.452(6) . ? C2 C3 1.513(7) . ? C3 O8 1.423(7) . ? C3 C4 1.474(7) . ? O3 C22 1.204(7) . ? O4 C4 1.424(5) . ? C4 C5 1.533(8) . ? O5 C9 1.404(7) . ? O5 C6 1.433(6) . ? C5 O6 1.424(6) . ? C5 C6 1.490(7) . ? O6 C8 1.312(8) . ? C6 C7 1.511(8) . ? O7 C8 1.193(7) . ? O8 C8 1.348(7) . ? C9 C10 1.514(10) . ? C10 C15 1.345(9) . ? C10 C11 1.363(10) . ? C11 C12 1.405(12) . ? C12 C13 1.321(11) . ? C13 C14 1.412(12) . ? C14 C15 1.357(11) . ? C18 C19 1.511(13) . ? C18 C20 1.621(12) . ? C18 C21 1.87(2) . ? C22 C23 1.469(8) . ? C23 C24 1.383(9) . ? C23 C28 1.397(9) . ? C24 C25 1.379(10) . ? C25 C26 1.335(14) . ? C26 C27 1.348(13) . ? C27 C28 1.418(13) . ? C31 C34 1.544(11) . ? C31 C33 1.555(11) . ? C31 C32 1.557(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si1 C30 110.6(4) . . ? O1 Si1 C31 105.6(3) . . ? C30 Si1 C31 109.6(4) . . ? O1 Si1 C29 108.7(3) . . ? C30 Si1 C29 110.4(5) . . ? C31 Si1 C29 111.8(5) . . ? C1 O1 Si1 130.6(4) . . ? O1 C1 C2 111.5(5) . . ? C18 Si2 O4 112.8(4) . . ? C18 Si2 C16 123.9(5) . . ? O4 Si2 C16 112.0(3) . . ? C18 Si2 C17 89.7(8) . . ? O4 Si2 C17 103.4(3) . . ? C16 Si2 C17 110.9(5) . . ? C22 O2 C2 119.1(4) . . ? O2 C2 C1 109.3(5) . . ? O2 C2 C3 105.5(4) . . ? C1 C2 C3 114.2(5) . . ? O8 C3 C4 111.8(4) . . ? O8 C3 C2 106.9(4) . . ? C4 C3 C2 113.5(4) . . ? C4 O4 Si2 129.6(3) . . ? O4 C4 C3 109.2(4) . . ? O4 C4 C5 109.6(4) . . ? C3 C4 C5 108.5(4) . . ? C9 O5 C6 116.0(4) . . ? O6 C5 C6 108.4(4) . . ? O6 C5 C4 111.5(4) . . ? C6 C5 C4 117.3(4) . . ? C8 O6 C5 123.9(5) . . ? O5 C6 C5 107.5(4) . . ? O5 C6 C7 110.4(4) . . ? C5 C6 C7 112.3(5) . . ? C8 O8 C3 120.9(5) . . ? O7 C8 O6 120.5(6) . . ? O7 C8 O8 119.5(7) . . ? O6 C8 O8 120.0(6) . . ? O5 C9 C10 109.2(5) . . ? C15 C10 C11 118.2(7) . . ? C15 C10 C9 119.9(7) . . ? C11 C10 C9 121.7(6) . . ? C10 C11 C12 121.7(7) . . ? C13 C12 C11 119.1(8) . . ? C12 C13 C14 119.5(8) . . ? C15 C14 C13 119.9(7) . . ? C10 C15 C14 121.5(8) . . ? C19 C18 Si2 119.5(10) . . ? C19 C18 C20 106.3(9) . . ? Si2 C18 C20 112.2(9) . . ? C19 C18 C21 115.2(12) . . ? Si2 C18 C21 93.8(7) . . ? C20 C18 C21 109.4(11) . . ? O3 C22 O2 122.4(6) . . ? O3 C22 C23 123.8(6) . . ? O2 C22 C23 113.7(6) . . ? C24 C23 C28 120.8(6) . . ? C24 C23 C22 121.4(6) . . ? C28 C23 C22 117.7(7) . . ? C25 C24 C23 120.5(8) . . ? C26 C25 C24 118.9(10) . . ? C25 C26 C27 122.8(10) . . ? C26 C27 C28 120.8(9) . . ? C23 C28 C27 116.2(8) . . ? C34 C31 C33 107.2(8) . . ? C34 C31 C32 113.6(7) . . ? C33 C31 C32 107.4(7) . . ? C34 C31 Si1 110.6(6) . . ? C33 C31 Si1 108.5(5) . . ? C32 C31 Si1 109.3(6) . . ? 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 Si1 O1 C1 93.7(7) . . . . ? C31 Si1 O1 C1 -147.8(6) . . . . ? C29 Si1 O1 C1 -27.7(7) . . . . ? Si1 O1 C1 C2 -128.4(5) . . . . ? C22 O2 C2 C1 89.8(6) . . . . ? C22 O2 C2 C3 -147.0(5) . . . . ? O1 C1 C2 O2 77.5(6) . . . . ? O1 C1 C2 C3 -40.4(7) . . . . ? O2 C2 C3 O8 61.7(5) . . . . ? C1 C2 C3 O8 -178.2(4) . . . . ? O2 C2 C3 C4 -174.5(4) . . . . ? C1 C2 C3 C4 -54.5(6) . . . . ? C18 Si2 O4 C4 -165.9(9) . . . . ? C16 Si2 O4 C4 -20.7(7) . . . . ? C17 Si2 O4 C4 98.7(6) . . . . ? Si2 O4 C4 C3 151.3(4) . . . . ? Si2 O4 C4 C5 -90.0(5) . . . . ? O8 C3 C4 O4 66.3(5) . . . . ? C2 C3 C4 O4 -54.7(6) . . . . ? O8 C3 C4 C5 -53.1(5) . . . . ? C2 C3 C4 C5 -174.1(4) . . . . ? O4 C4 C5 O6 -72.4(5) . . . . ? C3 C4 C5 O6 46.7(5) . . . . ? O4 C4 C5 C6 161.8(4) . . . . ? C3 C4 C5 C6 -79.1(5) . . . . ? C6 C5 O6 C8 106.6(6) . . . . ? C4 C5 O6 C8 -24.0(7) . . . . ? C9 O5 C6 C5 154.5(5) . . . . ? C9 O5 C6 C7 -82.7(6) . . . . ? O6 C5 C6 O5 -73.5(5) . . . . ? C4 C5 C6 O5 53.8(6) . . . . ? O6 C5 C6 C7 164.8(5) . . . . ? C4 C5 C6 C7 -67.8(6) . . . . ? C4 C3 O8 C8 37.3(6) . . . . ? C2 C3 O8 C8 162.1(4) . . . . ? C5 O6 C8 O7 -177.7(5) . . . . ? C5 O6 C8 O8 5.0(8) . . . . ? C3 O8 C8 O7 171.4(5) . . . . ? C3 O8 C8 O6 -11.3(8) . . . . ? C6 O5 C9 C10 -168.6(5) . . . . ? O5 C9 C10 C15 -125.4(6) . . . . ? O5 C9 C10 C11 50.4(9) . . . . ? C15 C10 C11 C12 -2.1(11) . . . . ? C9 C10 C11 C12 -177.9(7) . . . . ? C10 C11 C12 C13 2.0(14) . . . . ? C11 C12 C13 C14 -2.8(15) . . . . ? C12 C13 C14 C15 3.8(14) . . . . ? C11 C10 C15 C14 3.1(11) . . . . ? C9 C10 C15 C14 179.0(7) . . . . ? C13 C14 C15 C10 -4.0(13) . . . . ? O4 Si2 C18 C19 -47.3(17) . . . . ? C16 Si2 C18 C19 172.3(10) . . . . ? C17 Si2 C18 C19 57.1(14) . . . . ? O4 Si2 C18 C20 -172.7(10) . . . . ? C16 Si2 C18 C20 46.9(17) . . . . ? C17 Si2 C18 C20 -68.3(13) . . . . ? O4 Si2 C18 C21 74.5(6) . . . . ? C16 Si2 C18 C21 -65.8(8) . . . . ? C17 Si2 C18 C21 179.0(6) . . . . ? C2 O2 C22 O3 0.6(9) . . . . ? C2 O2 C22 C23 -177.3(5) . . . . ? O3 C22 C23 C24 -171.6(7) . . . . ? O2 C22 C23 C24 6.3(9) . . . . ? O3 C22 C23 C28 5.0(9) . . . . ? O2 C22 C23 C28 -177.2(6) . . . . ? C28 C23 C24 C25 0.6(11) . . . . ? C22 C23 C24 C25 177.0(7) . . . . ? C23 C24 C25 C26 0.0(12) . . . . ? C24 C25 C26 C27 -0.7(15) . . . . ? C25 C26 C27 C28 0.8(15) . . . . ? C24 C23 C28 C27 -0.5(10) . . . . ? C22 C23 C28 C27 -177.0(6) . . . . ? C26 C27 C28 C23 -0.2(12) . . . . ? O1 Si1 C31 C34 51.8(7) . . . . ? C30 Si1 C31 C34 171.0(7) . . . . ? C29 Si1 C31 C34 -66.3(8) . . . . ? O1 Si1 C31 C33 -65.6(5) . . . . ? C30 Si1 C31 C33 53.6(7) . . . . ? C29 Si1 C31 C33 176.3(5) . . . . ? O1 Si1 C31 C32 177.6(5) . . . . ? C30 Si1 C31 C32 -63.2(7) . . . . ? C29 Si1 C31 C32 59.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.534 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.051 data_str805m _database_code_depnum_ccdc_archive 'CCDC 762868' #TrackingRef '283_web_deposit_cif_file_1_JoseA.Martinez_1264091012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rmad _chemical_melting_point ? _chemical_formula_moiety 'C41 H59 N O7 Si2' _chemical_formula_sum 'C41 H59 N O7 Si2' _chemical_formula_weight 734.07 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' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 19 _symmetry_space_group_name_H-M P212121 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 14.2378(13) _cell_length_b 16.4937(16) _cell_length_c 19.1231(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4490.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.0015 _cell_measurement_theta_max 0.123401 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0015 _exptl_absorpt_correction_T_max 0.123401 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25922 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7906 _reflns_number_gt 3013 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+1.4056P] 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 SHELXL _refine_ls_extinction_coef 0.0008(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_number_reflns 7906 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2039 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 N1 N 0.6929(3) 0.7093(3) 1.1676(2) 0.0731(14) Uani 1 1 d . A . C1 C 0.6993(5) 0.5775(4) 0.8661(4) 0.096(2) Uani 1 1 d . A . H1A H 0.6653 0.6225 0.8453 0.116 Uiso 1 1 calc R . . H1B H 0.7177 0.5410 0.8287 0.116 Uiso 1 1 calc R . . O1 O 0.6411(3) 0.5370(3) 0.9122(2) 0.1024(14) Uani 1 1 d . . . Si2 Si 0.66808(12) 0.83583(11) 0.86844(9) 0.0773(6) Uani 1 1 d . . . O2 O 0.8472(3) 0.5406(3) 0.9144(2) 0.0915(13) Uani 1 1 d . A . C2 C 0.7852(5) 0.6089(4) 0.9018(3) 0.0783(18) Uani 1 1 d . . . H2 H 0.8166 0.6489 0.8719 0.094 Uiso 1 1 calc R A . C3 C 0.7638(4) 0.6460(3) 0.9726(3) 0.0635(15) Uani 1 1 d . A . H3 H 0.7390 0.6036 1.0034 0.076 Uiso 1 1 calc R . . O3 O 0.9633(4) 0.5989(4) 0.8536(3) 0.148(2) Uani 1 1 d . A . O4 O 0.8530(3) 0.6736(3) 1.0003(2) 0.0827(12) Uani 1 1 d . . . C4 C 0.6933(4) 0.7158(3) 0.9700(3) 0.0644(15) Uani 1 1 d . . . H4 H 0.6306 0.6958 0.9576 0.077 Uiso 1 1 calc R A . O5 O 0.9379(3) 0.7591(3) 1.0610(2) 0.1102(17) Uani 1 1 d . . . C5 C 0.6927(4) 0.7530(3) 1.0423(3) 0.0652(16) Uani 1 1 d . A . H5 H 0.6538 0.8019 1.0395 0.078 Uiso 1 1 calc R . . O6 O 0.7865(3) 0.7791(3) 1.06048(18) 0.0765(11) Uani 1 1 d . . . C6 C 0.6482(4) 0.6981(4) 1.0981(3) 0.0744(17) Uani 1 1 d . . . H6 H 0.6616 0.6422 1.0839 0.089 Uiso 1 1 calc R A . O7 O 0.7258(2) 0.7730(2) 0.91967(18) 0.0692(10) Uani 1 1 d . A . C7 C 0.5406(4) 0.7072(5) 1.0965(3) 0.102(2) Uani 1 1 d . A . H7A H 0.5134 0.6750 1.1331 0.154 Uiso 1 1 calc R . . H7B H 0.5172 0.6892 1.0521 0.154 Uiso 1 1 calc R . . H7C H 0.5242 0.7631 1.1034 0.154 Uiso 1 1 calc R . . C8 C 0.8615(6) 0.7376(5) 1.0422(3) 0.0792(19) Uani 1 1 d . A . Si1 Si 0.5838(5) 0.4571(4) 0.8925(4) 0.120(4) Uani 0.50 1 d PG A 1 C9 C 0.6717(6) 0.3738(6) 0.9051(7) 0.174(9) Uani 0.50 1 d PG A 1 H9A H 0.7173 0.3756 0.8682 0.261 Uiso 0.50 1 calc PR A 1 H9B H 0.6401 0.3223 0.9043 0.261 Uiso 0.50 1 calc PR A 1 H9C H 0.7027 0.3806 0.9493 0.261 Uiso 0.50 1 calc PR A 1 C10 C 0.5474(9) 0.4646(8) 0.7978(3) 0.165(9) Uiso 0.50 1 d PG A 1 H10A H 0.5342 0.5201 0.7864 0.247 Uiso 0.50 1 calc PR A 1 H10B H 0.4922 0.4323 0.7902 0.247 Uiso 0.50 1 calc PR A 1 H10C H 0.5974 0.4451 0.7686 0.247 Uiso 0.50 1 calc PR A 1 C11 C 0.4819(5) 0.4443(5) 0.9492(4) 0.085(5) Uani 0.50 1 d PG A 1 C12 C 0.5092(8) 0.4380(9) 1.0270(3) 0.28(2) Uani 0.50 1 d PG A 1 H12A H 0.4568 0.4174 1.0533 0.419 Uiso 0.50 1 calc PR A 1 H12B H 0.5260 0.4907 1.0443 0.419 Uiso 0.50 1 calc PR A 1 H12C H 0.5616 0.4019 1.0320 0.419 Uiso 0.50 1 calc PR A 1 C13 C 0.4278(6) 0.3636(6) 0.9278(7) 0.107(6) Uani 0.50 1 d PG A 1 H13A H 0.4722 0.3203 0.9220 0.161 Uiso 0.50 1 calc PR A 1 H13B H 0.3949 0.3722 0.8846 0.161 Uiso 0.50 1 calc PR A 1 H13C H 0.3837 0.3496 0.9637 0.161 Uiso 0.50 1 calc PR A 1 C14 C 0.4120(6) 0.5179(6) 0.9418(7) 0.115(6) Uani 0.50 1 d PG A 1 H14A H 0.3616 0.5118 0.9748 0.172 Uiso 0.50 1 calc PR A 1 H14B H 0.3870 0.5191 0.8953 0.172 Uiso 0.50 1 calc PR A 1 H14C H 0.4448 0.5676 0.9511 0.172 Uiso 0.50 1 calc PR A 1 Si1A Si 0.5586(7) 0.4701(5) 0.8930(4) 0.188(6) Uani 0.50 1 d PG A 2 C9A C 0.5801(12) 0.3993(8) 0.8176(5) 0.192(11) Uani 0.50 1 d PG A 2 H9A1 H 0.5574 0.4237 0.7752 0.288 Uiso 0.50 1 calc PR A 2 H9A2 H 0.5475 0.3492 0.8257 0.288 Uiso 0.50 1 calc PR A 2 H9A3 H 0.6462 0.3890 0.8134 0.288 Uiso 0.50 1 calc PR A 2 C10A C 0.4542(11) 0.5403(9) 0.8733(7) 0.35(3) Uani 0.50 1 d PG A 2 H10D H 0.3993 0.5205 0.8969 0.531 Uiso 0.50 1 calc PR A 2 H10E H 0.4430 0.5414 0.8238 0.531 Uiso 0.50 1 calc PR A 2 H10F H 0.4682 0.5941 0.8894 0.531 Uiso 0.50 1 calc PR A 2 C11A C 0.5397(7) 0.4148(6) 0.9746(4) 0.249(19) Uani 0.50 1 d PG A 2 C12A C 0.6220(11) 0.3575(8) 0.9958(8) 0.33(2) Uani 0.50 1 d PG A 2 H12D H 0.6611 0.3474 0.9559 0.495 Uiso 0.50 1 calc PR A 2 H12E H 0.5969 0.3071 1.0127 0.495 Uiso 0.50 1 calc PR A 2 H12F H 0.6585 0.3827 1.0320 0.495 Uiso 0.50 1 calc PR A 2 C13A C 0.4464(10) 0.3585(9) 0.9657(6) 0.234(18) Uani 0.50 1 d PG A 2 H13D H 0.4363 0.3280 1.0078 0.351 Uiso 0.50 1 calc PR A 2 H13E H 0.4550 0.3219 0.9271 0.351 Uiso 0.50 1 calc PR A 2 H13F H 0.3929 0.3924 0.9569 0.351 Uiso 0.50 1 calc PR A 2 C14A C 0.5240(11) 0.4714(9) 1.0376(4) 0.121(7) Uani 0.50 1 d PG A 2 H14D H 0.4741 0.4505 1.0661 0.182 Uiso 0.50 1 calc PR A 2 H14E H 0.5076 0.5245 1.0212 0.182 Uiso 0.50 1 calc PR A 2 H14F H 0.5806 0.4744 1.0647 0.182 Uiso 0.50 1 calc PR A 2 C15 C 0.9360(6) 0.5428(6) 0.8880(4) 0.099(2) Uani 1 1 d . . . C16 C 0.9895(6) 0.4697(7) 0.9071(4) 0.097(2) Uani 1 1 d . A . C17 C 1.0838(8) 0.4722(8) 0.8954(5) 0.163(5) Uani 1 1 d . . . H17 H 1.1104 0.5194 0.8776 0.196 Uiso 1 1 calc R A . C18 C 1.1401(13) 0.4074(14) 0.9092(8) 0.214(9) Uani 1 1 d . A . H18 H 1.2048 0.4097 0.9028 0.257 Uiso 1 1 calc R . . C19 C 1.0970(14) 0.3397(12) 0.9327(8) 0.214(8) Uani 1 1 d . . . H19 H 1.1336 0.2939 0.9406 0.257 Uiso 1 1 calc R A . C20 C 1.0026(11) 0.3345(8) 0.9457(7) 0.218(6) Uani 1 1 d . A . H20 H 0.9755 0.2871 0.9624 0.261 Uiso 1 1 calc R . . C21 C 0.9481(7) 0.4051(8) 0.9323(6) 0.157(4) Uani 1 1 d . . . H21 H 0.8839 0.4053 0.9413 0.189 Uiso 1 1 calc R A . C22 C 0.5981(5) 0.9090(4) 0.9198(4) 0.121(3) Uani 1 1 d . . . H22A H 0.5561 0.8801 0.9502 0.181 Uiso 1 1 calc R . . H22B H 0.5624 0.9426 0.8886 0.181 Uiso 1 1 calc R . . H22C H 0.6394 0.9422 0.9472 0.181 Uiso 1 1 calc R . . C23 C 0.5875(4) 0.7782(4) 0.8097(3) 0.114(3) Uani 1 1 d . . . H23A H 0.6238 0.7481 0.7763 0.171 Uiso 1 1 calc R . . H23B H 0.5470 0.8154 0.7855 0.171 Uiso 1 1 calc R . . H23C H 0.5502 0.7415 0.8370 0.171 Uiso 1 1 calc R . . C24 C 0.7626(4) 0.8843(4) 0.8169(3) 0.0799(19) Uani 1 1 d . . . C25 C 0.8296(5) 0.9317(5) 0.8663(4) 0.127(3) Uani 1 1 d . . . H25A H 0.8574 0.8950 0.8992 0.191 Uiso 1 1 calc R . . H25B H 0.7947 0.9725 0.8909 0.191 Uiso 1 1 calc R . . H25C H 0.8781 0.9571 0.8391 0.191 Uiso 1 1 calc R . . C26 C 0.7219(5) 0.9457(4) 0.7633(4) 0.120(3) Uani 1 1 d . . . H26A H 0.6768 0.9799 0.7861 0.181 Uiso 1 1 calc R . . H26B H 0.6920 0.9167 0.7259 0.181 Uiso 1 1 calc R . . H26C H 0.7719 0.9783 0.7448 0.181 Uiso 1 1 calc R . . C27 C 0.8232(5) 0.8214(4) 0.7778(4) 0.117(3) Uani 1 1 d . . . H27A H 0.8746 0.8484 0.7551 0.175 Uiso 1 1 calc R . . H27B H 0.7855 0.7941 0.7435 0.175 Uiso 1 1 calc R . . H27C H 0.8473 0.7824 0.8106 0.175 Uiso 1 1 calc R . . C28 C 0.6728(5) 0.7879(4) 1.2000(3) 0.095(2) Uani 1 1 d . . . H28A H 0.6094 0.7873 1.2185 0.114 Uiso 1 1 calc R A . H28B H 0.6759 0.8299 1.1645 0.114 Uiso 1 1 calc R . . C29 C 0.7403(6) 0.8081(4) 1.2579(4) 0.089(2) Uani 1 1 d . A . C30 C 0.7123(6) 0.8263(4) 1.3249(4) 0.111(2) Uani 1 1 d . . . H30 H 0.6486 0.8246 1.3356 0.133 Uiso 1 1 calc R A . C31 C 0.7753(9) 0.8472(5) 1.3775(5) 0.134(3) Uani 1 1 d . A . H31 H 0.7544 0.8593 1.4224 0.161 Uiso 1 1 calc R . . C32 C 0.8666(9) 0.8493(5) 1.3617(5) 0.126(3) Uani 1 1 d . . . H32 H 0.9101 0.8622 1.3963 0.151 Uiso 1 1 calc R A . C33 C 0.8966(6) 0.8329(5) 1.2966(5) 0.123(3) Uani 1 1 d . A . H33 H 0.9605 0.8359 1.2865 0.148 Uiso 1 1 calc R . . C34 C 0.8336(7) 0.8116(4) 1.2438(4) 0.108(2) Uani 1 1 d . . . H34 H 0.8555 0.7998 1.1991 0.130 Uiso 1 1 calc R A . C35 C 0.6709(5) 0.6431(5) 1.2149(3) 0.104(2) Uani 1 1 d . . . H35A H 0.6032 0.6394 1.2200 0.125 Uiso 1 1 calc R A . H35B H 0.6971 0.6551 1.2606 0.125 Uiso 1 1 calc R . . C36 C 0.7086(8) 0.5612(5) 1.1901(4) 0.099(2) Uani 1 1 d . A . C37 C 0.7952(8) 0.5530(6) 1.1564(5) 0.118(3) Uani 1 1 d . . . H37 H 0.8309 0.5989 1.1466 0.141 Uiso 1 1 calc R A . C38 C 0.8279(10) 0.4778(9) 1.1376(5) 0.174(5) Uani 1 1 d . A . H38 H 0.8860 0.4709 1.1162 0.209 Uiso 1 1 calc R . . C39 C 0.7683(17) 0.4114(13) 1.1525(9) 0.225(11) Uani 1 1 d . . . H39 H 0.7877 0.3606 1.1371 0.270 Uiso 1 1 calc R A . C40 C 0.6888(15) 0.4150(14) 1.1860(9) 0.213(11) Uani 1 1 d . A . H40 H 0.6553 0.3686 1.1978 0.256 Uiso 1 1 calc R . . C41 C 0.6566(8) 0.4926(9) 1.2031(4) 0.151(4) Uani 1 1 d . . . H41 H 0.5979 0.4980 1.2240 0.181 Uiso 1 1 calc R A . 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 N1 0.086(3) 0.086(4) 0.047(3) 0.002(3) -0.001(3) 0.016(3) C1 0.131(7) 0.073(5) 0.085(5) -0.007(4) -0.003(5) -0.003(5) O1 0.099(3) 0.104(4) 0.104(3) -0.029(3) 0.004(3) -0.037(3) Si2 0.0759(11) 0.0803(13) 0.0758(11) 0.0144(10) -0.0088(10) 0.0136(11) O2 0.091(3) 0.081(3) 0.103(3) -0.004(3) 0.033(3) 0.002(3) C2 0.088(5) 0.070(5) 0.077(4) 0.001(4) 0.015(4) -0.003(4) C3 0.068(4) 0.062(4) 0.060(4) 0.003(3) -0.001(3) -0.005(3) O3 0.150(5) 0.128(5) 0.166(6) 0.010(5) 0.075(4) -0.020(4) O4 0.069(3) 0.084(3) 0.096(3) -0.009(3) -0.011(2) 0.010(3) C4 0.067(4) 0.070(4) 0.057(4) 0.006(3) -0.001(3) 0.003(4) O5 0.072(3) 0.147(5) 0.111(4) -0.008(3) -0.016(3) -0.023(3) C5 0.062(4) 0.072(4) 0.062(4) 0.002(3) -0.009(3) 0.006(3) O6 0.077(3) 0.088(3) 0.064(3) -0.004(2) -0.002(2) -0.012(3) C6 0.058(4) 0.103(5) 0.063(4) 0.006(4) 0.002(3) 0.016(3) O7 0.077(2) 0.072(3) 0.059(2) 0.019(2) -0.010(2) 0.008(2) C7 0.064(4) 0.150(6) 0.093(5) 0.009(5) 0.000(3) 0.005(4) C8 0.081(6) 0.085(6) 0.071(5) 0.003(4) -0.005(4) -0.014(5) Si1 0.094(4) 0.128(7) 0.138(8) -0.078(6) 0.026(4) -0.032(4) C9 0.126(14) 0.087(13) 0.31(3) -0.072(16) 0.037(18) 0.044(11) C11 0.078(10) 0.112(14) 0.066(9) -0.014(9) 0.002(8) 0.011(10) C12 0.22(3) 0.20(3) 0.42(5) -0.19(3) 0.06(3) -0.14(3) C13 0.092(11) 0.083(12) 0.147(16) 0.009(11) -0.039(11) -0.040(9) C14 0.088(11) 0.086(13) 0.170(16) -0.015(11) 0.011(11) 0.005(9) Si1A 0.241(12) 0.137(8) 0.186(13) 0.005(8) -0.056(10) -0.067(8) C9A 0.33(3) 0.150(18) 0.095(12) -0.099(13) 0.073(16) -0.139(19) C10A 0.18(2) 0.21(3) 0.67(8) 0.10(4) -0.29(4) -0.02(2) C11A 0.26(4) 0.18(3) 0.31(4) -0.07(3) -0.12(4) 0.12(3) C12A 0.32(4) 0.19(3) 0.49(6) 0.05(4) -0.26(4) -0.01(3) C13A 0.135(19) 0.33(4) 0.24(3) -0.02(3) -0.07(2) -0.12(2) C14A 0.190(19) 0.119(16) 0.056(9) -0.009(10) 0.003(10) -0.062(15) C15 0.107(7) 0.103(7) 0.087(6) -0.023(5) 0.018(5) -0.005(6) C16 0.092(7) 0.120(8) 0.077(5) -0.022(5) -0.006(5) 0.005(6) C17 0.094(8) 0.232(14) 0.164(9) -0.049(9) 0.037(7) 0.027(8) C18 0.142(13) 0.35(3) 0.156(12) -0.084(15) 0.007(10) 0.057(16) C19 0.181(17) 0.29(2) 0.177(12) 0.004(13) -0.015(12) 0.148(16) C20 0.199(13) 0.195(13) 0.259(15) 0.064(11) -0.005(12) 0.073(12) C21 0.133(8) 0.133(9) 0.205(11) 0.049(8) 0.013(8) 0.042(8) C22 0.129(6) 0.101(6) 0.132(6) 0.023(5) 0.022(5) 0.039(5) C23 0.108(5) 0.127(6) 0.106(5) -0.003(5) -0.044(4) -0.015(5) C24 0.092(5) 0.069(4) 0.078(4) 0.027(4) -0.008(4) 0.007(4) C25 0.123(6) 0.117(6) 0.142(7) 0.015(6) -0.031(6) -0.027(5) C26 0.135(6) 0.113(6) 0.114(6) 0.055(5) -0.001(5) 0.010(5) C27 0.111(6) 0.128(6) 0.112(5) 0.032(5) 0.019(5) 0.024(5) C28 0.109(5) 0.103(5) 0.074(4) -0.014(4) -0.003(4) 0.042(5) C29 0.116(6) 0.086(5) 0.066(5) -0.004(4) 0.005(5) 0.023(5) C30 0.146(7) 0.112(6) 0.075(5) -0.006(5) 0.010(6) 0.035(6) C31 0.210(11) 0.118(7) 0.074(6) -0.015(5) -0.007(8) 0.019(8) C32 0.189(10) 0.103(6) 0.086(7) -0.029(5) -0.018(7) 0.026(7) C33 0.156(8) 0.102(6) 0.111(7) -0.021(6) -0.004(7) 0.015(6) C34 0.145(7) 0.108(6) 0.073(5) -0.018(4) -0.011(6) 0.005(6) C35 0.116(6) 0.128(7) 0.069(4) 0.021(5) 0.009(4) -0.011(5) C36 0.141(8) 0.077(6) 0.078(5) 0.032(5) -0.031(5) -0.017(6) C37 0.144(8) 0.100(8) 0.110(6) 0.017(5) -0.015(6) 0.016(6) C38 0.249(13) 0.103(8) 0.169(9) -0.009(8) -0.073(9) 0.062(10) C39 0.43(3) 0.097(11) 0.146(15) -0.009(11) -0.100(16) 0.016(19) C40 0.37(3) 0.120(14) 0.153(15) 0.055(13) -0.076(15) -0.065(19) C41 0.209(11) 0.141(9) 0.103(6) 0.042(7) -0.052(7) -0.026(10) _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 N1 C35 1.453(7) . ? N1 C28 1.466(7) . ? N1 C6 1.485(6) . ? C1 O1 1.383(7) . ? C1 C2 1.494(8) . ? O1 Si1 1.595(8) . ? O1 Si1A 1.653(9) . ? Si2 O7 1.646(4) . ? Si2 C22 1.847(7) . ? Si2 C24 1.849(6) . ? Si2 C23 1.866(6) . ? O2 C15 1.361(8) . ? O2 C2 1.452(7) . ? C2 C3 1.517(7) . ? C3 O4 1.449(6) . ? C3 C4 1.527(7) . ? O3 C15 1.200(9) . ? O4 C8 1.330(7) . ? C4 O7 1.426(6) . ? C4 C5 1.512(7) . ? O5 C8 1.200(7) . ? C5 O6 1.446(6) . ? C5 C6 1.536(7) . ? O6 C8 1.316(8) . ? C6 C7 1.539(7) . ? Si1 C11 1.8238 . ? Si1 C9 1.8742 . ? Si1 C10 1.8868 . ? C11 C12 1.5421 . ? C11 C14 1.5753 . ? C11 C13 1.5923 . ? Si1A C11A 1.8263 . ? Si1A C9A 1.8807 . ? Si1A C10A 1.9212 . ? C11A C14A 1.5409 . ? C11A C12A 1.5591 . ? C11A C13A 1.6297 . ? C15 C16 1.471(11) . ? C16 C21 1.310(10) . ? C16 C17 1.361(11) . ? C17 C18 1.362(19) . ? C18 C19 1.35(2) . ? C19 C20 1.369(17) . ? C20 C21 1.422(14) . ? C24 C27 1.543(8) . ? C24 C25 1.553(8) . ? C24 C26 1.554(8) . ? C28 C29 1.504(9) . ? C29 C34 1.356(9) . ? C29 C30 1.376(8) . ? C30 C31 1.390(11) . ? C31 C32 1.335(12) . ? C32 C33 1.344(10) . ? C33 C34 1.396(10) . ? C35 C36 1.528(10) . ? C36 C41 1.375(12) . ? C36 C37 1.398(10) . ? C37 C38 1.373(12) . ? C38 C39 1.41(2) . ? C39 C40 1.30(2) . ? C40 C41 1.40(2) . ? 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 C35 N1 C28 111.1(5) . . ? C35 N1 C6 111.8(5) . . ? C28 N1 C6 113.8(5) . . ? O1 C1 C2 111.5(5) . . ? C1 O1 Si1 123.7(5) . . ? C1 O1 Si1A 127.4(5) . . ? Si1 O1 Si1A 14.7(5) . . ? O7 Si2 C22 111.4(3) . . ? O7 Si2 C24 103.1(2) . . ? C22 Si2 C24 113.2(3) . . ? O7 Si2 C23 110.1(3) . . ? C22 Si2 C23 108.7(3) . . ? C24 Si2 C23 110.3(3) . . ? C15 O2 C2 118.9(6) . . ? O2 C2 C1 107.7(5) . . ? O2 C2 C3 106.7(5) . . ? C1 C2 C3 112.6(5) . . ? O4 C3 C2 106.1(5) . . ? O4 C3 C4 110.6(4) . . ? C2 C3 C4 114.0(5) . . ? C8 O4 C3 123.3(5) . . ? O7 C4 C5 110.5(4) . . ? O7 C4 C3 107.9(4) . . ? C5 C4 C3 106.3(4) . . ? O6 C5 C4 109.6(4) . . ? O6 C5 C6 112.9(4) . . ? C4 C5 C6 113.5(5) . . ? C8 O6 C5 122.0(5) . . ? N1 C6 C5 111.8(5) . . ? N1 C6 C7 115.6(5) . . ? C5 C6 C7 109.8(5) . . ? C4 O7 Si2 131.1(3) . . ? O5 C8 O6 120.2(7) . . ? O5 C8 O4 119.8(8) . . ? O6 C8 O4 119.9(6) . . ? O1 Si1 C11 111.2(4) . . ? O1 Si1 C9 103.6(5) . . ? C11 Si1 C9 111.7 . . ? O1 Si1 C10 108.3(5) . . ? C11 Si1 C10 111.1 . . ? C9 Si1 C10 110.8 . . ? C12 C11 C14 107.3 . . ? C12 C11 C13 108.2 . . ? C14 C11 C13 108.4 . . ? C12 C11 Si1 112.4 . . ? C14 C11 Si1 111.2 . . ? C13 C11 Si1 109.2 . . ? O1 Si1A C11A 104.4(5) . . ? O1 Si1A C9A 118.0(5) . . ? C11A Si1A C9A 111.6 . . ? O1 Si1A C10A 101.0(6) . . ? C11A Si1A C10A 110.8 . . ? C9A Si1A C10A 110.4 . . ? C14A C11A C12A 105.8 . . ? C14A C11A C13A 108.0 . . ? C12A C11A C13A 107.1 . . ? C14A C11A Si1A 112.7 . . ? C12A C11A Si1A 114.5 . . ? C13A C11A Si1A 108.4 . . ? O3 C15 O2 121.6(9) . . ? O3 C15 C16 126.9(9) . . ? O2 C15 C16 111.6(8) . . ? C21 C16 C17 121.9(11) . . ? C21 C16 C15 121.7(9) . . ? C17 C16 C15 116.4(11) . . ? C16 C17 C18 121.6(15) . . ? C19 C18 C17 117(2) . . ? C18 C19 C20 123.9(19) . . ? C19 C20 C21 116.9(14) . . ? C16 C21 C20 119.1(11) . . ? C27 C24 C25 106.8(6) . . ? C27 C24 C26 109.1(5) . . ? C25 C24 C26 107.5(6) . . ? C27 C24 Si2 112.0(4) . . ? C25 C24 Si2 110.0(5) . . ? C26 C24 Si2 111.2(4) . . ? N1 C28 C29 112.4(5) . . ? C34 C29 C30 117.3(8) . . ? C34 C29 C28 119.3(7) . . ? C30 C29 C28 123.3(8) . . ? C29 C30 C31 122.8(8) . . ? C32 C31 C30 118.1(9) . . ? C31 C32 C33 120.9(10) . . ? C32 C33 C34 121.1(9) . . ? C29 C34 C33 119.8(7) . . ? N1 C35 C36 113.2(6) . . ? C41 C36 C37 118.6(9) . . ? C41 C36 C35 118.8(11) . . ? C37 C36 C35 122.6(8) . . ? C38 C37 C36 120.5(10) . . ? C37 C38 C39 116.3(15) . . ? C40 C39 C38 126(2) . . ? C39 C40 C41 116(2) . . ? C36 C41 C40 122.3(14) . . ? 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 C2 C1 O1 Si1 -142.0(5) . . . . ? C2 C1 O1 Si1A -159.5(6) . . . . ? C15 O2 C2 C1 122.9(6) . . . . ? C15 O2 C2 C3 -116.0(6) . . . . ? O1 C1 C2 O2 75.1(6) . . . . ? O1 C1 C2 C3 -42.3(7) . . . . ? O2 C2 C3 O4 62.2(5) . . . . ? C1 C2 C3 O4 -179.8(5) . . . . ? O2 C2 C3 C4 -175.9(4) . . . . ? C1 C2 C3 C4 -57.9(7) . . . . ? C2 C3 O4 C8 148.9(5) . . . . ? C4 C3 O4 C8 24.8(7) . . . . ? O4 C3 C4 O7 66.6(5) . . . . ? C2 C3 C4 O7 -52.8(6) . . . . ? O4 C3 C4 C5 -51.9(5) . . . . ? C2 C3 C4 C5 -171.3(5) . . . . ? O7 C4 C5 O6 -59.2(6) . . . . ? C3 C4 C5 O6 57.6(6) . . . . ? O7 C4 C5 C6 173.6(4) . . . . ? C3 C4 C5 C6 -69.7(5) . . . . ? C4 C5 O6 C8 -37.1(7) . . . . ? C6 C5 O6 C8 90.5(6) . . . . ? C35 N1 C6 C5 -163.6(5) . . . . ? C28 N1 C6 C5 69.5(6) . . . . ? C35 N1 C6 C7 69.7(7) . . . . ? C28 N1 C6 C7 -57.1(8) . . . . ? O6 C5 C6 N1 21.9(7) . . . . ? C4 C5 C6 N1 147.4(5) . . . . ? O6 C5 C6 C7 151.7(5) . . . . ? C4 C5 C6 C7 -82.8(6) . . . . ? C5 C4 O7 Si2 -94.5(5) . . . . ? C3 C4 O7 Si2 149.8(4) . . . . ? C22 Si2 O7 C4 60.9(5) . . . . ? C24 Si2 O7 C4 -177.4(5) . . . . ? C23 Si2 O7 C4 -59.8(5) . . . . ? C5 O6 C8 O5 -176.5(5) . . . . ? C5 O6 C8 O4 6.4(8) . . . . ? C3 O4 C8 O5 -177.0(5) . . . . ? C3 O4 C8 O6 0.1(8) . . . . ? C1 O1 Si1 C11 -156.5(5) . . . . ? Si1A O1 Si1 C11 -46.9(16) . . . . ? C1 O1 Si1 C9 83.4(6) . . . . ? Si1A O1 Si1 C9 -167.0(18) . . . . ? C1 O1 Si1 C10 -34.3(6) . . . . ? Si1A O1 Si1 C10 75.3(17) . . . . ? O1 Si1 C11 C12 -59.4(6) . . . . ? C9 Si1 C11 C12 55.7 . . . . ? C10 Si1 C11 C12 180.0 . . . . ? O1 Si1 C11 C14 60.9(6) . . . . ? C9 Si1 C11 C14 176.0 . . . . ? C10 Si1 C11 C14 -59.7 . . . . ? O1 Si1 C11 C13 -179.5(6) . . . . ? C9 Si1 C11 C13 -64.4 . . . . ? C10 Si1 C11 C13 59.8 . . . . ? C1 O1 Si1A C11A 160.0(6) . . . . ? Si1 O1 Si1A C11A 79.4(18) . . . . ? C1 O1 Si1A C9A 35.4(8) . . . . ? Si1 O1 Si1A C9A -45.2(17) . . . . ? C1 O1 Si1A C10A -85.0(6) . . . . ? Si1 O1 Si1A C10A -165.6(19) . . . . ? O1 Si1A C11A C14A 50.2(6) . . . . ? C9A Si1A C11A C14A 178.8 . . . . ? C10A Si1A C11A C14A -57.7 . . . . ? O1 Si1A C11A C12A -70.8(6) . . . . ? C9A Si1A C11A C12A 57.8 . . . . ? C10A Si1A C11A C12A -178.7 . . . . ? O1 Si1A C11A C13A 169.7(6) . . . . ? C9A Si1A C11A C13A -61.7 . . . . ? C10A Si1A C11A C13A 61.8 . . . . ? C2 O2 C15 O3 -1.5(10) . . . . ? C2 O2 C15 C16 178.7(5) . . . . ? O3 C15 C16 C21 -165.7(9) . . . . ? O2 C15 C16 C21 14.0(11) . . . . ? O3 C15 C16 C17 12.7(11) . . . . ? O2 C15 C16 C17 -167.6(6) . . . . ? C21 C16 C17 C18 0.2(16) . . . . ? C15 C16 C17 C18 -178.2(11) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C17 C18 C19 C20 -3(3) . . . . ? C18 C19 C20 C21 1(3) . . . . ? C17 C16 C21 C20 -2.2(15) . . . . ? C15 C16 C21 C20 176.2(9) . . . . ? C19 C20 C21 C16 1.7(19) . . . . ? O7 Si2 C24 C27 56.5(5) . . . . ? C22 Si2 C24 C27 176.9(5) . . . . ? C23 Si2 C24 C27 -61.1(5) . . . . ? O7 Si2 C24 C25 -62.1(5) . . . . ? C22 Si2 C24 C25 58.3(5) . . . . ? C23 Si2 C24 C25 -179.7(5) . . . . ? O7 Si2 C24 C26 178.8(5) . . . . ? C22 Si2 C24 C26 -60.8(6) . . . . ? C23 Si2 C24 C26 61.2(6) . . . . ? C35 N1 C28 C29 70.2(7) . . . . ? C6 N1 C28 C29 -162.5(5) . . . . ? N1 C28 C29 C34 58.3(9) . . . . ? N1 C28 C29 C30 -124.2(7) . . . . ? C34 C29 C30 C31 -0.4(12) . . . . ? C28 C29 C30 C31 -178.0(7) . . . . ? C29 C30 C31 C32 -0.2(14) . . . . ? C30 C31 C32 C33 1.1(15) . . . . ? C31 C32 C33 C34 -1.4(14) . . . . ? C30 C29 C34 C33 0.1(11) . . . . ? C28 C29 C34 C33 177.8(6) . . . . ? C32 C33 C34 C29 0.8(12) . . . . ? C28 N1 C35 C36 -168.3(6) . . . . ? C6 N1 C35 C36 63.3(7) . . . . ? N1 C35 C36 C41 -144.7(6) . . . . ? N1 C35 C36 C37 37.1(9) . . . . ? C41 C36 C37 C38 -0.9(11) . . . . ? C35 C36 C37 C38 177.3(7) . . . . ? C36 C37 C38 C39 1.7(14) . . . . ? C37 C38 C39 C40 -4(3) . . . . ? C38 C39 C40 C41 6(3) . . . . ? C37 C36 C41 C40 2.3(14) . . . . ? C35 C36 C41 C40 -176.0(10) . . . . ? C39 C40 C41 C36 -5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.299 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.034 data_str755m _database_code_depnum_ccdc_archive 'CCDC 764882' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C46 H65 N O6 Si2' _chemical_formula_sum 'C46 H65 N O6 Si2' _exptl_crystal_recrystallization_method 'Hexane, dichloromethane, ether' _chemical_melting_point ? _exptl_crystal_description fiber _exptl_crystal_colour colorless _diffrn_ambient_temperature 273(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn _chemical_formula_weight 784.17 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.1116(10) _cell_length_b 16.5521(16) _cell_length_c 13.8615(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.705(3) _cell_angle_gamma 90.00 _cell_volume 2286.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3005 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 21.27 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9411 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details 'Bruker Sadabs' _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 12971 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7956 _reflns_number_gt 5247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0431P)^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 SHELXL _refine_ls_extinction_coef 0.0054(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.16(11) _refine_ls_number_reflns 7956 _refine_ls_number_parameters 509 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.008 _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 1.06268(8) 0.33736(5) 0.76141(6) 0.0459(2) Uani 1 1 d . . . Si2 Si 1.11355(9) 0.33069(6) 1.16974(6) 0.0548(2) Uani 1 1 d . . . O5 O 0.92870(18) 0.28604(10) 0.78057(13) 0.0413(5) Uani 1 1 d . . . O2 O 0.76807(19) 0.16504(11) 0.97023(13) 0.0458(5) Uani 1 1 d . . . O1 O 1.0796(2) 0.25909(12) 1.08655(14) 0.0519(5) Uani 1 1 d . . . O4 O 0.9814(2) 0.09226(11) 0.90874(16) 0.0526(5) Uani 1 1 d . . . H4 H 0.9108 0.0701 0.8852 0.079 Uiso 1 1 calc R . . C24 C 0.9169(3) 0.20105(16) 0.79042(19) 0.0373(7) Uani 1 1 d . . . H24 H 0.9742 0.1747 0.7494 0.045 Uiso 1 1 calc R . . C34 C 0.5463(3) 0.1436(2) 0.9945(2) 0.0486(8) Uani 1 1 d . . . C33 C 0.6593(3) 0.2002(2) 0.9972(2) 0.0482(8) Uani 1 1 d . . . O6 O 0.7581(2) 0.09291(13) 0.75861(18) 0.0706(7) Uani 1 1 d . . . H6 H 0.8178 0.0708 0.7350 0.106 Uiso 1 1 calc R . . O3 O 0.6581(2) 0.27051(15) 1.02000(18) 0.0724(7) Uani 1 1 d . . . C15 C 0.7458(3) 0.21620(19) 0.4691(2) 0.0479(8) Uani 1 1 d . . . C40 C 0.9650(3) 0.20887(18) 1.0758(2) 0.0507(8) Uani 1 1 d . . . H40A H 0.9070 0.2260 1.1210 0.061 Uiso 1 1 calc R . . H40B H 0.9923 0.1536 1.0915 0.061 Uiso 1 1 calc R . . N1 N 0.5663(2) 0.19667(14) 0.63381(16) 0.0451(6) Uani 1 1 d . . . C31 C 0.9669(3) 0.17755(16) 0.89758(19) 0.0405(7) Uani 1 1 d . . . H31 H 1.0577 0.1998 0.9140 0.049 Uiso 1 1 calc R . . C23 C 0.7714(3) 0.17875(17) 0.75188(19) 0.0438(7) Uani 1 1 d . . . H23 H 0.7174 0.2025 0.7970 0.053 Uiso 1 1 calc R . . C32 C 0.8889(3) 0.21301(17) 0.9718(2) 0.0417(7) Uani 1 1 d . . . H32 H 0.8647 0.2692 0.9546 0.050 Uiso 1 1 calc R . . C1 C 0.5045(3) 0.3410(2) 0.6493(2) 0.0494(7) Uani 1 1 d . . . C22 C 0.7131(3) 0.20983(17) 0.64937(19) 0.0428(7) Uani 1 1 d . . . H22 H 0.7261 0.2685 0.6515 0.051 Uiso 1 1 calc R . . C8 C 0.3796(3) 0.09909(18) 0.6081(2) 0.0479(7) Uani 1 1 d . . . C35 C 0.5552(3) 0.0643(2) 0.9656(2) 0.0609(9) Uani 1 1 d . . . H35 H 0.6343 0.0448 0.9484 0.073 Uiso 1 1 calc R . . C14 C 0.5160(3) 0.12100(19) 0.5860(2) 0.0578(9) Uani 1 1 d . . . H14A H 0.5786 0.0778 0.6080 0.069 Uiso 1 1 calc R . . H14B H 0.5107 0.1265 0.5157 0.069 Uiso 1 1 calc R . . C16 C 0.7878(3) 0.1786(2) 0.5695(2) 0.0510(8) Uani 1 1 d . . . H16A H 0.8830 0.1881 0.5902 0.061 Uiso 1 1 calc R . . H16B H 0.7747 0.1207 0.5637 0.061 Uiso 1 1 calc R . . C2 C 0.5047(4) 0.4161(2) 0.6056(3) 0.0688(10) Uani 1 1 d . . . H2 H 0.4969 0.4199 0.5380 0.083 Uiso 1 1 calc R . . C36 C 0.4293(3) 0.1713(2) 1.0215(2) 0.0650(9) Uani 1 1 d . . . H36 H 0.4233 0.2248 1.0409 0.078 Uiso 1 1 calc R . . C17 C 0.7120(3) 0.1689(2) 0.3870(2) 0.0651(10) Uani 1 1 d . . . H17 H 0.7140 0.1130 0.3938 0.078 Uiso 1 1 calc R . . C3 C 0.5168(4) 0.4872(2) 0.6629(4) 0.0800(12) Uani 1 1 d . . . H3 H 0.5153 0.5376 0.6332 0.096 Uiso 1 1 calc R . . C9 C 0.1271(4) 0.0571(2) 0.6484(3) 0.0641(10) Uani 1 1 d . . . H9 H 0.0431 0.0428 0.6618 0.077 Uiso 1 1 calc R . . C41 C 0.9627(4) 0.3933(2) 1.1692(3) 0.0864(12) Uani 1 1 d . . . H41A H 0.9497 0.4275 1.1124 0.130 Uiso 1 1 calc R . . H41B H 0.9739 0.4261 1.2271 0.130 Uiso 1 1 calc R . . H41C H 0.8859 0.3590 1.1677 0.130 Uiso 1 1 calc R . . C37 C 0.3201(4) 0.1201(3) 1.0198(3) 0.0834(12) Uani 1 1 d . . . H37 H 0.2419 0.1386 1.0392 0.100 Uiso 1 1 calc R . . C28 C 1.0093(3) 0.44429(19) 0.7726(3) 0.0621(9) Uani 1 1 d . . . C26 C 1.2119(3) 0.3125(2) 0.8539(3) 0.0765(11) Uani 1 1 d . . . H26A H 1.1869 0.3107 0.9177 0.115 Uiso 1 1 calc R . . H26B H 1.2795 0.3531 0.8529 0.115 Uiso 1 1 calc R . . H26C H 1.2466 0.2608 0.8390 0.115 Uiso 1 1 calc R . . C46 C 1.1706(4) 0.2869(2) 1.2948(3) 0.0704(10) Uani 1 1 d . . . C18 C 0.7423(4) 0.2988(2) 0.4559(3) 0.0662(10) Uani 1 1 d . . . H18 H 0.7659 0.3323 0.5099 0.079 Uiso 1 1 calc R . . C10 C 0.2291(4) 0.0743(2) 0.7220(3) 0.0734(11) Uani 1 1 d . . . H10 H 0.2147 0.0723 0.7865 0.088 Uiso 1 1 calc R . . C7 C 0.4865(3) 0.2651(2) 0.5892(2) 0.0563(9) Uani 1 1 d . . . H7A H 0.3925 0.2501 0.5787 0.068 Uiso 1 1 calc R . . H7B H 0.5108 0.2760 0.5257 0.068 Uiso 1 1 calc R . . C42 C 1.2525(4) 0.3885(2) 1.1303(3) 0.0869(13) Uani 1 1 d . . . H42A H 1.3261 0.3528 1.1260 0.130 Uiso 1 1 calc R . . H42B H 1.2816 0.4303 1.1771 0.130 Uiso 1 1 calc R . . H42C H 1.2217 0.4123 1.0674 0.130 Uiso 1 1 calc R . . C11 C 0.2747(3) 0.0814(2) 0.5348(2) 0.0654(10) Uani 1 1 d . . . H11 H 0.2884 0.0832 0.4701 0.078 Uiso 1 1 calc R . . C4 C 0.5187(3) 0.3391(2) 0.7495(2) 0.0577(8) Uani 1 1 d . . . H4A H 0.5188 0.2893 0.7808 0.069 Uiso 1 1 calc R . . C5 C 0.5325(4) 0.4078(2) 0.8050(3) 0.0695(10) Uani 1 1 d . . . H5 H 0.5433 0.4041 0.8728 0.083 Uiso 1 1 calc R . . C12 C 0.3533(4) 0.0945(2) 0.7026(2) 0.0706(10) Uani 1 1 d . . . H12 H 0.4220 0.1054 0.7545 0.085 Uiso 1 1 calc R . . C19 C 0.6757(4) 0.2015(3) 0.2957(3) 0.0791(11) Uani 1 1 d . . . H19 H 0.6544 0.1677 0.2418 0.095 Uiso 1 1 calc R . . C20 C 0.6704(4) 0.2827(4) 0.2833(3) 0.0892(14) Uani 1 1 d . . . H20 H 0.6441 0.3045 0.2212 0.107 Uiso 1 1 calc R . . C38 C 0.4447(4) 0.0137(3) 0.9625(3) 0.0765(11) Uani 1 1 d . . . H38 H 0.4492 -0.0396 0.9421 0.092 Uiso 1 1 calc R . . C21 C 0.7046(4) 0.3333(3) 0.3643(3) 0.0800(11) Uani 1 1 d . . . H21 H 0.7022 0.3891 0.3569 0.096 Uiso 1 1 calc R . . C39 C 0.3290(4) 0.0424(3) 0.9895(3) 0.0828(12) Uani 1 1 d . . . H39 H 0.2555 0.0083 0.9870 0.099 Uiso 1 1 calc R . . C27 C 0.8871(5) 0.4614(3) 0.6945(4) 0.1063(16) Uani 1 1 d . . . H27A H 0.8180 0.4228 0.7000 0.159 Uiso 1 1 calc R . . H27B H 0.9120 0.4574 0.6308 0.159 Uiso 1 1 calc R . . H27C H 0.8546 0.5149 0.7035 0.159 Uiso 1 1 calc R . . C6 C 0.5305(4) 0.4813(2) 0.7618(3) 0.0792(11) Uani 1 1 d . . . H6A H 0.5385 0.5278 0.7999 0.095 Uiso 1 1 calc R . . C13 C 0.1493(4) 0.0611(2) 0.5543(3) 0.0760(11) Uani 1 1 d . . . H13 H 0.0798 0.0501 0.5029 0.091 Uiso 1 1 calc R . . C29 C 0.9712(6) 0.4585(3) 0.8725(4) 0.1117(17) Uani 1 1 d . . . H29A H 0.9455 0.5139 0.8779 0.168 Uiso 1 1 calc R . . H29B H 1.0466 0.4466 0.9224 0.168 Uiso 1 1 calc R . . H29C H 0.8975 0.4240 0.8804 0.168 Uiso 1 1 calc R . . C43 C 1.2116(6) 0.3580(4) 1.3674(3) 0.140(2) Uani 1 1 d . . . H43A H 1.2513 0.3367 1.4301 0.210 Uiso 1 1 calc R . . H43B H 1.1334 0.3890 1.3742 0.210 Uiso 1 1 calc R . . H43C H 1.2752 0.3920 1.3428 0.210 Uiso 1 1 calc R . . C30 C 1.1238(5) 0.5026(3) 0.7568(5) 0.135(2) Uani 1 1 d . . . H30A H 1.0918 0.5573 0.7553 0.202 Uiso 1 1 calc R . . H30B H 1.1524 0.4902 0.6959 0.202 Uiso 1 1 calc R . . H30C H 1.1980 0.4965 0.8094 0.202 Uiso 1 1 calc R . . C45 C 1.0607(4) 0.2383(3) 1.3304(3) 0.0894(13) Uani 1 1 d . . . H45A H 1.0311 0.1960 1.2845 0.134 Uiso 1 1 calc R . . H45B H 0.9866 0.2732 1.3362 0.134 Uiso 1 1 calc R . . H45C H 1.0950 0.2151 1.3931 0.134 Uiso 1 1 calc R . . C44 C 1.2934(5) 0.2313(4) 1.2920(4) 0.132(2) Uani 1 1 d . . . H44A H 1.3174 0.2046 1.3539 0.198 Uiso 1 1 calc R . . H44B H 1.3678 0.2633 1.2791 0.198 Uiso 1 1 calc R . . H44C H 1.2712 0.1917 1.2412 0.198 Uiso 1 1 calc R . . C100 C 1.1043(4) 0.3144(2) 0.6391(3) 0.0798(11) Uani 1 1 d . . . H10A H 1.1312 0.2589 0.6370 0.120 Uiso 1 1 calc R . . H10B H 1.1763 0.3487 0.6270 0.120 Uiso 1 1 calc R . . H10C H 1.0268 0.3237 0.5899 0.120 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 0.0420(5) 0.0490(5) 0.0482(5) 0.0046(4) 0.0122(4) -0.0053(4) Si2 0.0636(6) 0.0537(5) 0.0460(5) -0.0035(5) 0.0060(4) -0.0065(5) O5 0.0378(12) 0.0406(12) 0.0453(11) 0.0036(8) 0.0062(9) -0.0033(9) O2 0.0420(12) 0.0503(12) 0.0464(11) -0.0037(9) 0.0110(9) -0.0050(10) O1 0.0505(13) 0.0557(12) 0.0488(12) -0.0087(10) 0.0067(9) -0.0080(11) O4 0.0573(13) 0.0377(11) 0.0614(14) 0.0045(10) 0.0059(11) 0.0080(10) C24 0.0366(17) 0.0373(16) 0.0402(16) -0.0003(13) 0.0123(13) 0.0021(13) C34 0.043(2) 0.068(2) 0.0351(16) 0.0082(15) 0.0067(13) 0.0024(17) C33 0.051(2) 0.058(2) 0.0370(16) 0.0047(15) 0.0100(14) 0.0075(18) O6 0.0785(18) 0.0520(14) 0.0756(17) 0.0082(12) -0.0033(13) -0.0176(13) O3 0.0687(17) 0.0646(16) 0.0884(18) -0.0102(14) 0.0265(13) 0.0065(13) C15 0.0386(18) 0.066(2) 0.0408(18) -0.0025(16) 0.0114(14) -0.0049(15) C40 0.057(2) 0.0515(18) 0.0417(17) 0.0018(14) 0.0030(15) -0.0101(16) N1 0.0372(14) 0.0489(14) 0.0469(14) -0.0099(12) 0.0004(11) -0.0045(12) C31 0.0349(16) 0.0428(17) 0.0430(17) 0.0014(13) 0.0043(13) -0.0008(14) C23 0.0434(18) 0.0460(17) 0.0421(17) -0.0033(13) 0.0078(13) -0.0048(14) C32 0.0435(18) 0.0383(15) 0.0437(17) 0.0003(13) 0.0085(13) -0.0028(14) C1 0.0352(16) 0.0555(19) 0.0564(19) 0.0042(18) 0.0049(13) 0.0046(16) C22 0.0368(17) 0.0504(17) 0.0406(16) -0.0025(13) 0.0052(13) -0.0045(14) C8 0.0446(18) 0.0553(18) 0.0426(18) -0.0099(14) 0.0039(14) -0.0042(15) C35 0.052(2) 0.071(2) 0.063(2) -0.0009(18) 0.0190(17) -0.0079(18) C14 0.054(2) 0.067(2) 0.0539(19) -0.0202(17) 0.0133(15) -0.0057(17) C16 0.0444(18) 0.0643(19) 0.0454(18) -0.0048(15) 0.0104(14) 0.0003(16) C2 0.060(2) 0.080(3) 0.066(2) 0.014(2) 0.0107(18) 0.014(2) C36 0.052(2) 0.084(2) 0.059(2) 0.0140(18) 0.0086(17) 0.015(2) C17 0.056(2) 0.091(3) 0.050(2) -0.0171(19) 0.0134(16) -0.0099(19) C3 0.080(3) 0.054(2) 0.106(4) 0.009(2) 0.014(2) 0.011(2) C9 0.052(2) 0.059(2) 0.083(3) 0.0006(19) 0.018(2) -0.0102(17) C41 0.109(3) 0.065(2) 0.090(3) 0.002(2) 0.029(3) 0.023(2) C37 0.039(2) 0.136(4) 0.076(3) 0.029(3) 0.0117(18) 0.008(3) C28 0.057(2) 0.0479(18) 0.083(3) 0.0065(18) 0.018(2) -0.0067(17) C26 0.044(2) 0.089(3) 0.092(3) 0.018(2) -0.0004(18) -0.0117(19) C46 0.062(2) 0.094(3) 0.052(2) -0.0045(18) -0.0023(18) -0.010(2) C18 0.071(2) 0.077(3) 0.052(2) 0.0010(17) 0.0138(17) -0.0047(19) C10 0.080(3) 0.088(3) 0.054(2) 0.0123(19) 0.017(2) -0.006(2) C7 0.0430(19) 0.075(2) 0.0471(19) -0.0030(17) -0.0029(14) -0.0011(17) C42 0.107(3) 0.080(3) 0.075(3) -0.008(2) 0.020(2) -0.042(2) C11 0.061(2) 0.087(3) 0.048(2) -0.0125(18) 0.0106(18) -0.013(2) C4 0.060(2) 0.0551(18) 0.061(2) 0.0040(19) 0.0188(16) 0.0023(19) C5 0.083(3) 0.065(3) 0.061(2) -0.009(2) 0.0145(19) 0.003(2) C12 0.061(2) 0.100(3) 0.049(2) -0.0030(19) 0.0004(17) -0.014(2) C19 0.079(3) 0.116(4) 0.042(2) -0.011(2) 0.0095(18) -0.019(3) C20 0.060(3) 0.160(5) 0.046(2) 0.017(3) 0.0036(19) -0.010(3) C38 0.078(3) 0.090(3) 0.063(2) 0.003(2) 0.017(2) -0.019(2) C21 0.075(2) 0.095(3) 0.074(3) 0.028(3) 0.023(2) 0.001(3) C39 0.057(3) 0.123(4) 0.068(3) 0.021(3) 0.006(2) -0.021(3) C27 0.107(4) 0.081(3) 0.127(4) 0.033(3) 0.005(3) 0.028(3) C6 0.076(3) 0.063(3) 0.099(3) -0.010(2) 0.017(2) 0.002(2) C13 0.051(2) 0.103(3) 0.073(3) -0.018(2) 0.0072(19) -0.023(2) C29 0.157(5) 0.078(3) 0.108(4) -0.026(3) 0.047(3) 0.002(3) C43 0.197(6) 0.154(5) 0.054(3) -0.016(3) -0.020(3) -0.041(4) C30 0.111(4) 0.059(3) 0.249(7) 0.012(3) 0.074(4) -0.024(3) C45 0.091(3) 0.120(3) 0.057(2) 0.032(2) 0.011(2) -0.006(3) C44 0.082(3) 0.198(6) 0.113(4) 0.055(4) 0.009(3) 0.044(4) C100 0.081(3) 0.094(3) 0.076(2) -0.001(2) 0.044(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O5 1.658(2) . ? Si1 C26 1.854(3) . ? Si1 C100 1.854(3) . ? Si1 C28 1.864(3) . ? Si2 O1 1.649(2) . ? Si2 C41 1.843(4) . ? Si2 C42 1.857(4) . ? Si2 C46 1.878(4) . ? O5 C24 1.420(3) . ? O2 C33 1.352(3) . ? O2 C32 1.454(3) . ? O1 C40 1.413(3) . ? O4 C31 1.425(3) . ? O4 H4 0.8200 . ? C24 C23 1.524(4) . ? C24 C31 1.536(4) . ? C24 H24 0.9800 . ? C34 C36 1.379(4) . ? C34 C35 1.380(4) . ? C34 C33 1.473(4) . ? C33 O3 1.206(4) . ? O6 C23 1.432(3) . ? O6 H6 0.8200 . ? C15 C17 1.376(4) . ? C15 C18 1.379(4) . ? C15 C16 1.517(4) . ? C40 C32 1.518(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N1 C7 1.465(4) . ? N1 C14 1.468(4) . ? N1 C22 1.480(4) . ? C31 C32 1.516(4) . ? C31 H31 0.9800 . ? C23 C22 1.533(4) . ? C23 H23 0.9800 . ? C32 H32 0.9800 . ? C1 C4 1.373(4) . ? C1 C2 1.383(5) . ? C1 C7 1.501(4) . ? C22 C16 1.532(4) . ? C22 H22 0.9800 . ? C8 C11 1.371(4) . ? C8 C12 1.381(4) . ? C8 C14 1.507(4) . ? C35 C38 1.391(5) . ? C35 H35 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C2 C3 1.414(5) . ? C2 H2 0.9300 . ? C36 C37 1.389(5) . ? C36 H36 0.9300 . ? C17 C19 1.368(5) . ? C17 H17 0.9300 . ? C3 C6 1.357(6) . ? C3 H3 0.9300 . ? C9 C10 1.354(5) . ? C9 C13 1.362(5) . ? C9 H9 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C37 C39 1.360(6) . ? C37 H37 0.9300 . ? C28 C29 1.517(5) . ? C28 C27 1.526(6) . ? C28 C30 1.551(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C46 C45 1.520(5) . ? C46 C44 1.551(6) . ? C46 C43 1.559(6) . ? C18 C21 1.386(5) . ? C18 H18 0.9300 . ? C10 C12 1.370(5) . ? C10 H10 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C11 C13 1.382(5) . ? C11 H11 0.9300 . ? C4 C5 1.367(5) . ? C4 H4A 0.9300 . ? C5 C6 1.354(5) . ? C5 H5 0.9300 . ? C12 H12 0.9300 . ? C19 C20 1.354(6) . ? C19 H19 0.9300 . ? C20 C21 1.397(6) . ? C20 H20 0.9300 . ? C38 C39 1.371(6) . ? C38 H38 0.9300 . ? C21 H21 0.9300 . ? C39 H39 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C6 H6A 0.9300 . ? C13 H13 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? 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 O5 Si1 C26 111.55(13) . . ? O5 Si1 C100 111.02(14) . . ? C26 Si1 C100 107.65(18) . . ? O5 Si1 C28 102.55(12) . . ? C26 Si1 C28 111.51(17) . . ? C100 Si1 C28 112.59(17) . . ? O1 Si2 C41 109.06(16) . . ? O1 Si2 C42 104.09(15) . . ? C41 Si2 C42 112.1(2) . . ? O1 Si2 C46 111.31(14) . . ? C41 Si2 C46 110.28(18) . . ? C42 Si2 C46 109.91(18) . . ? C24 O5 Si1 127.36(17) . . ? C33 O2 C32 118.8(2) . . ? C40 O1 Si2 124.52(19) . . ? C31 O4 H4 109.5 . . ? O5 C24 C23 107.3(2) . . ? O5 C24 C31 108.9(2) . . ? C23 C24 C31 114.7(2) . . ? O5 C24 H24 108.6 . . ? C23 C24 H24 108.6 . . ? C31 C24 H24 108.6 . . ? C36 C34 C35 119.7(3) . . ? C36 C34 C33 118.6(3) . . ? C35 C34 C33 121.7(3) . . ? O3 C33 O2 122.2(3) . . ? O3 C33 C34 125.4(3) . . ? O2 C33 C34 112.5(3) . . ? C23 O6 H6 109.5 . . ? C17 C15 C18 117.2(3) . . ? C17 C15 C16 121.1(3) . . ? C18 C15 C16 121.7(3) . . ? O1 C40 C32 110.4(2) . . ? O1 C40 H40A 109.6 . . ? C32 C40 H40A 109.6 . . ? O1 C40 H40B 109.6 . . ? C32 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C7 N1 C14 110.2(2) . . ? C7 N1 C22 114.5(2) . . ? C14 N1 C22 117.0(2) . . ? O4 C31 C32 111.4(2) . . ? O4 C31 C24 111.5(2) . . ? C32 C31 C24 115.7(2) . . ? O4 C31 H31 105.8 . . ? C32 C31 H31 105.8 . . ? C24 C31 H31 105.8 . . ? O6 C23 C24 108.3(2) . . ? O6 C23 C22 111.6(2) . . ? C24 C23 C22 116.2(2) . . ? O6 C23 H23 106.8 . . ? C24 C23 H23 106.8 . . ? C22 C23 H23 106.8 . . ? O2 C32 C31 108.1(2) . . ? O2 C32 C40 106.3(2) . . ? C31 C32 C40 112.9(2) . . ? O2 C32 H32 109.8 . . ? C31 C32 H32 109.8 . . ? C40 C32 H32 109.8 . . ? C4 C1 C2 117.1(3) . . ? C4 C1 C7 121.6(3) . . ? C2 C1 C7 121.3(3) . . ? N1 C22 C16 116.7(2) . . ? N1 C22 C23 107.8(2) . . ? C16 C22 C23 113.4(2) . . ? N1 C22 H22 106.0 . . ? C16 C22 H22 106.0 . . ? C23 C22 H22 106.0 . . ? C11 C8 C12 116.3(3) . . ? C11 C8 C14 121.3(3) . . ? C12 C8 C14 122.4(3) . . ? C34 C35 C38 119.3(4) . . ? C34 C35 H35 120.3 . . ? C38 C35 H35 120.3 . . ? N1 C14 C8 111.9(2) . . ? N1 C14 H14A 109.2 . . ? C8 C14 H14A 109.2 . . ? N1 C14 H14B 109.2 . . ? C8 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C15 C16 C22 115.4(2) . . ? C15 C16 H16A 108.4 . . ? C22 C16 H16A 108.4 . . ? C15 C16 H16B 108.4 . . ? C22 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C1 C2 C3 120.6(3) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C34 C36 C37 120.6(4) . . ? C34 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C19 C17 C15 122.1(4) . . ? C19 C17 H17 119.0 . . ? C15 C17 H17 119.0 . . ? C6 C3 C2 119.4(4) . . ? C6 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C10 C9 C13 119.0(3) . . ? C10 C9 H9 120.5 . . ? C13 C9 H9 120.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C37 C36 119.2(4) . . ? C39 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C29 C28 C27 108.6(4) . . ? C29 C28 C30 110.0(4) . . ? C27 C28 C30 108.6(4) . . ? C29 C28 Si1 110.2(3) . . ? C27 C28 Si1 109.2(3) . . ? C30 C28 Si1 110.2(3) . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C45 C46 C44 109.1(4) . . ? C45 C46 C43 108.6(4) . . ? C44 C46 C43 109.7(4) . . ? C45 C46 Si2 112.1(2) . . ? C44 C46 Si2 109.2(3) . . ? C43 C46 Si2 108.2(3) . . ? C15 C18 C21 121.8(4) . . ? C15 C18 H18 119.1 . . ? C21 C18 H18 119.1 . . ? C9 C10 C12 120.7(3) . . ? C9 C10 H10 119.7 . . ? C12 C10 H10 119.7 . . ? N1 C7 C1 114.0(2) . . ? N1 C7 H7A 108.8 . . ? C1 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C8 C11 C13 121.8(3) . . ? C8 C11 H11 119.1 . . ? C13 C11 H11 119.1 . . ? C5 C4 C1 122.2(3) . . ? C5 C4 H4A 118.9 . . ? C1 C4 H4A 118.9 . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C10 C12 C8 121.9(3) . . ? C10 C12 H12 119.0 . . ? C8 C12 H12 119.0 . . ? C20 C19 C17 120.5(4) . . ? C20 C19 H19 119.7 . . ? C17 C19 H19 119.7 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C39 C38 C35 120.0(4) . . ? C39 C38 H38 120.0 . . ? C35 C38 H38 120.0 . . ? C18 C21 C20 118.8(4) . . ? C18 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C37 C39 C38 121.1(4) . . ? C37 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C5 C6 C3 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C3 C6 H6A 119.9 . . ? C9 C13 C11 120.3(3) . . ? C9 C13 H13 119.9 . . ? C11 C13 H13 119.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C46 C43 H43A 109.5 . . ? C46 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C46 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C44 H44A 109.5 . . ? C46 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C46 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C100 H10A 109.5 . . ? Si1 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? Si1 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.196 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.032 data_str787m _database_code_depnum_ccdc_archive 'CCDC 764883' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C47 H63 N O7 Si2' _chemical_formula_sum 'C47 H63 N O7 Si2' _exptl_crystal_recrystallization_method 'Hexane, dichloromethane, ether' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour colorless _diffrn_ambient_temperature 293(2) _chemical_formula_weight 810.16 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_int_tables_number 1 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.734(2) _cell_length_b 11.293(2) _cell_length_c 11.423(2) _cell_angle_alpha 110.54(3) _cell_angle_beta 90.72(3) _cell_angle_gamma 108.91(3) _cell_volume 1214.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7005 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0834 _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 -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5473 _reflns_number_gt 2559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.1904P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(4) _refine_ls_number_reflns 5473 _refine_ls_number_parameters 499 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1701 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.3089 _refine_ls_wR_factor_gt 0.2259 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.007 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 -0.6755(4) -0.5628(4) -0.4303(3) 0.1063(13) Uani 1 1 d . . . O2 O -0.8696(6) -0.4087(6) -0.6192(6) 0.0647(16) Uani 1 1 d . . . Si2 Si -1.1938(4) -0.7775(4) -0.7998(4) 0.1101(14) Uani 1 1 d . . . O3 O -0.7906(6) -0.6052(7) -0.9126(6) 0.0685(18) Uani 1 1 d . . . O5 O -0.9284(7) -0.6408(7) -1.0837(6) 0.0768(19) Uani 1 1 d . . . O6 O -1.0442(7) -0.7168(7) -0.8427(6) 0.0747(19) Uani 1 1 d . . . C16 C -0.8592(8) -0.5246(9) -0.8383(8) 0.054(2) Uani 1 1 d . . . H16A H -0.8395 -0.4445 -0.8600 0.065 Uiso 1 1 calc R . . N1 N -1.0323(8) -0.4016(8) -0.9801(7) 0.066(2) Uani 1 1 d . . . O1 O -0.6858(7) -0.5248(10) -0.5530(7) 0.099(3) Uani 1 1 d . . . C30 C -0.8420(9) -0.1977(10) -0.9737(10) 0.069(3) Uani 1 1 d . . . C8 C -0.7942(9) -0.4785(10) -0.7040(8) 0.061(2) Uani 1 1 d . . . H8A H -0.7038 -0.4147 -0.6941 0.073 Uiso 1 1 calc R . . C20 C -1.1049(10) -0.5480(12) -1.0485(9) 0.075(3) Uani 1 1 d . . . H20A H -1.1899 -0.5648 -1.0152 0.090 Uiso 1 1 calc R . . C17 C -1.0075(9) -0.5994(10) -0.8708(9) 0.059(2) Uani 1 1 d . . . H17A H -1.0540 -0.5403 -0.8230 0.071 Uiso 1 1 calc R . . C19 C -1.0443(9) -0.6372(11) -1.0159(9) 0.069(3) Uani 1 1 d . . . H19A H -1.1105 -0.7288 -1.0494 0.083 Uiso 1 1 calc R . . O4 O -0.7527(9) -0.7041(9) -1.1081(8) 0.100(3) Uani 1 1 d . . . C36 C -1.2184(11) -0.3549(13) -0.8658(12) 0.085(3) Uani 1 1 d . . . C29 C -1.1245(10) -0.3267(11) -0.9614(10) 0.075(3) Uani 1 1 d . . . H29A H -1.1771 -0.3518 -1.0417 0.090 Uiso 1 1 calc R . . H29B H -1.0737 -0.2307 -0.9314 0.090 Uiso 1 1 calc R . . C37 C -1.1729(12) -0.3175(13) -0.7446(11) 0.090(3) Uani 1 1 d . . . H37A H -1.0820 -0.2770 -0.7163 0.108 Uiso 1 1 calc R . . C18 C -0.8204(11) -0.6532(11) -1.0390(10) 0.067(3) Uani 1 1 d . . . C10 C -0.8942(13) -0.2157(13) -0.4708(10) 0.081(3) Uani 1 1 d . . . C28 C -0.9227(11) -0.3442(11) -1.0465(9) 0.077(3) Uani 1 1 d . . . H28A H -0.9611 -0.3538 -1.1281 0.093 Uiso 1 1 calc R . . H28B H -0.8640 -0.3961 -1.0612 0.093 Uiso 1 1 calc R . . C9 C -0.8151(11) -0.2727(12) -0.5644(9) 0.070(3) Uani 1 1 d . . . C21 C -1.1453(12) -0.5920(11) -1.1931(10) 0.088(3) Uani 1 1 d . . . H21A H -1.1809 -0.5285 -1.2070 0.105 Uiso 1 1 calc R . . H21B H -1.0664 -0.5880 -1.2343 0.105 Uiso 1 1 calc R . . O7 O -0.7129(10) -0.2089(9) -0.5902(8) 0.109(3) Uani 1 1 d . . . C7 C -0.7869(10) -0.5885(11) -0.6602(9) 0.071(3) Uani 1 1 d . . . H7A H -0.8717 -0.6315 -0.6374 0.085 Uiso 1 1 calc R . . H7B H -0.7646 -0.6566 -0.7268 0.085 Uiso 1 1 calc R . . C31 C -0.7876(14) -0.1537(15) -0.8486(12) 0.101(4) Uani 1 1 d . . . H31A H -0.8007 -0.2151 -0.8089 0.121 Uiso 1 1 calc R . . C22 C -1.2466(15) -0.7316(16) -1.2528(14) 0.106(4) Uani 1 1 d . . . C35 C -0.8191(12) -0.1039(12) -1.0284(12) 0.089(3) Uani 1 1 d . . . H35A H -0.8530 -0.1296 -1.1124 0.106 Uiso 1 1 calc R . . C11 C -0.863(2) -0.0758(16) -0.4244(14) 0.138(6) Uani 1 1 d . . . H11A H -0.7930 -0.0252 -0.4539 0.165 Uiso 1 1 calc R . . C41 C -1.3532(13) -0.4225(17) -0.9157(14) 0.113(5) Uani 1 1 d . . . H41A H -1.3851 -0.4460 -0.9998 0.135 Uiso 1 1 calc R . . C32 C -0.7153(16) -0.0212(16) -0.7839(15) 0.120(5) Uani 1 1 d . . . H32A H -0.6817 0.0056 -0.6996 0.144 Uiso 1 1 calc R . . C38 C -1.2582(18) -0.338(2) -0.6640(16) 0.140(6) Uani 1 1 d . . . H38A H -1.2260 -0.3079 -0.5788 0.168 Uiso 1 1 calc R . . C34 C -0.7444(16) 0.0303(15) -0.957(2) 0.113(5) Uani 1 1 d . . . H34A H -0.7321 0.0927 -0.9953 0.135 Uiso 1 1 calc R . . C1 C -0.5716(14) -0.4052(16) -0.3044(13) 0.109(4) Uani 1 1 d . . . C15 C -0.9926(15) -0.2938(17) -0.4233(14) 0.112(4) Uani 1 1 d . . . H15A H -1.0111 -0.3864 -0.4509 0.135 Uiso 1 1 calc R . . C12 C -0.927(3) -0.010(2) -0.340(2) 0.162(8) Uani 1 1 d . . . H12A H -0.9055 0.0832 -0.3138 0.195 Uiso 1 1 calc R . . C6 C -0.840(2) -0.622(3) -0.386(2) 0.264(19) Uani 1 1 d . . . H6A H -0.8939 -0.7046 -0.4523 0.395 Uiso 1 1 calc R . . H6B H -0.8806 -0.5549 -0.3739 0.395 Uiso 1 1 calc R . . H6C H -0.8320 -0.6371 -0.3094 0.395 Uiso 1 1 calc R . . C2 C -0.638(3) -0.293(2) -0.277(2) 0.190(10) Uani 1 1 d . . . H2A H -0.5820 -0.2110 -0.2117 0.285 Uiso 1 1 calc R . . H2B H -0.7234 -0.3239 -0.2508 0.285 Uiso 1 1 calc R . . H2C H -0.6498 -0.2763 -0.3527 0.285 Uiso 1 1 calc R . . C33 C -0.6889(14) 0.0756(15) -0.8364(17) 0.108(4) Uani 1 1 d . . . H33A H -0.6367 0.1655 -0.7917 0.130 Uiso 1 1 calc R . . C40 C -1.4390(14) -0.453(2) -0.8246(19) 0.141(6) Uani 1 1 d . . . H40A H -1.5280 -0.5073 -0.8522 0.169 Uiso 1 1 calc R . . C43 C -1.1891(16) -0.6787(14) -0.6263(14) 0.122(5) Uani 1 1 d . . . H43A H -1.1161 -0.6801 -0.5780 0.183 Uiso 1 1 calc R . . H43B H -1.2710 -0.7188 -0.5991 0.183 Uiso 1 1 calc R . . H43C H -1.1779 -0.5870 -0.6138 0.183 Uiso 1 1 calc R . . C39 C -1.3922(18) -0.404(2) -0.7034(18) 0.141(7) Uani 1 1 d . . . H39A H -1.4500 -0.4136 -0.6448 0.170 Uiso 1 1 calc R . . C14 C -1.0643(16) -0.233(2) -0.3338(14) 0.124(5) Uani 1 1 d . . . H14A H -1.1317 -0.2846 -0.3028 0.148 Uiso 1 1 calc R . . C44 C -1.181(3) -0.911(4) -0.811(2) 0.30(2) Uani 1 1 d . . . C27 C -1.3763(19) -0.753(2) -1.227(2) 0.169(9) Uani 1 1 d . . . H27A H -1.3932 -0.6766 -1.1765 0.202 Uiso 1 1 calc R . . C42 C -1.3308(13) -0.7769(19) -0.895(2) 0.149(8) Uani 1 1 d . . . H42A H -1.3308 -0.8267 -0.9822 0.224 Uiso 1 1 calc R . . H42B H -1.3204 -0.6855 -0.8826 0.224 Uiso 1 1 calc R . . H42C H -1.4134 -0.8181 -0.8692 0.224 Uiso 1 1 calc R . . C4 C -0.548(3) -0.425(2) -0.1807(17) 0.246(16) Uani 1 1 d . . . H4A H -0.4929 -0.3409 -0.1174 0.368 Uiso 1 1 calc R . . H4B H -0.5047 -0.4903 -0.1950 0.368 Uiso 1 1 calc R . . H4C H -0.6318 -0.4573 -0.1525 0.368 Uiso 1 1 calc R . . C47 C -1.0881(18) -0.9463(16) -0.7353(18) 0.138(6) Uani 1 1 d . . . H47A H -0.9972 -0.9001 -0.7407 0.207 Uiso 1 1 calc R . . H47B H -1.1068 -1.0420 -0.7697 0.207 Uiso 1 1 calc R . . H47C H -1.1023 -0.9188 -0.6486 0.207 Uiso 1 1 calc R . . C45 C -1.203(3) -1.0268(19) -0.9641(17) 0.176(8) Uani 1 1 d . . . H45A H -1.1274 -0.9973 -1.0042 0.265 Uiso 1 1 calc R . . H45B H -1.2819 -1.0341 -1.0108 0.265 Uiso 1 1 calc R . . H45C H -1.2117 -1.1133 -0.9618 0.265 Uiso 1 1 calc R . . C13 C -1.032(3) -0.093(3) -0.2926(18) 0.173(11) Uani 1 1 d . . . H13A H -1.0781 -0.0523 -0.2329 0.207 Uiso 1 1 calc R . . C46 C -1.348(2) -1.013(2) -0.777(3) 0.206(11) Uani 1 1 d . . . H46A H -1.3602 -0.9667 -0.6921 0.309 Uiso 1 1 calc R . . H46B H -1.3474 -1.1006 -0.7862 0.309 Uiso 1 1 calc R . . H46C H -1.4188 -1.0223 -0.8352 0.309 Uiso 1 1 calc R . . C23 C -1.213(3) -0.837(2) -1.324(2) 0.166(8) Uani 1 1 d . . . H23A H -1.1261 -0.8283 -1.3376 0.199 Uiso 1 1 calc R . . C3 C -0.445(3) -0.342(4) -0.343(2) 0.255(16) Uani 1 1 d . . . H3A H -0.3937 -0.2598 -0.2745 0.383 Uiso 1 1 calc R . . H3B H -0.4625 -0.3216 -0.4150 0.383 Uiso 1 1 calc R . . H3C H -0.3963 -0.4024 -0.3642 0.383 Uiso 1 1 calc R . . C5 C -0.605(5) -0.687(2) -0.467(3) 0.34(3) Uani 1 1 d . . . H5A H -0.6635 -0.7674 -0.5327 0.510 Uiso 1 1 calc R . . H5B H -0.5914 -0.7060 -0.3935 0.510 Uiso 1 1 calc R . . H5C H -0.5212 -0.6562 -0.4957 0.510 Uiso 1 1 calc R . . C25 C -1.444(2) -0.968(2) -1.348(2) 0.171(7) Uiso 1 1 d . . . H25A H -1.5134 -1.0498 -1.3881 0.205 Uiso 1 1 calc R . . C24 C -1.330(3) -0.974(3) -1.383(2) 0.177(8) Uiso 1 1 d . . . H24A H -1.3203 -1.0522 -1.4385 0.213 Uiso 1 1 calc R . . C26 C -1.484(3) -0.873(3) -1.267(3) 0.223(11) Uiso 1 1 d . . . H26A H -1.5682 -0.8853 -1.2431 0.267 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 0.128(3) 0.114(3) 0.068(2) 0.0450(19) -0.0196(19) 0.020(2) O2 0.058(4) 0.070(5) 0.054(4) 0.015(3) 0.004(3) 0.017(4) Si2 0.075(2) 0.131(3) 0.132(3) 0.078(3) 0.015(2) 0.014(2) O3 0.061(4) 0.104(5) 0.047(4) 0.027(4) 0.016(3) 0.039(4) O5 0.083(5) 0.110(6) 0.047(4) 0.034(4) 0.015(4) 0.041(4) O6 0.068(5) 0.082(5) 0.069(4) 0.046(4) 0.005(3) 0.001(4) C16 0.055(6) 0.070(6) 0.042(5) 0.031(4) 0.008(4) 0.019(5) N1 0.063(5) 0.079(6) 0.064(5) 0.037(4) 0.017(4) 0.023(5) O1 0.059(5) 0.170(8) 0.070(5) 0.064(5) -0.001(4) 0.020(5) C30 0.054(6) 0.074(7) 0.078(7) 0.031(6) 0.014(5) 0.018(5) C8 0.054(6) 0.072(6) 0.053(6) 0.019(5) 0.016(4) 0.023(5) C20 0.056(6) 0.103(8) 0.064(6) 0.045(6) -0.011(5) 0.011(6) C17 0.052(6) 0.074(6) 0.054(6) 0.031(5) 0.006(4) 0.017(5) C19 0.052(6) 0.083(7) 0.063(6) 0.028(5) -0.008(5) 0.013(5) O4 0.108(6) 0.125(7) 0.084(6) 0.033(5) 0.035(5) 0.068(6) C36 0.057(7) 0.117(9) 0.085(8) 0.030(6) 0.008(6) 0.047(7) C29 0.062(7) 0.092(8) 0.077(7) 0.041(6) 0.010(5) 0.025(6) C37 0.078(8) 0.143(11) 0.058(7) 0.041(7) 0.016(6) 0.047(8) C18 0.066(7) 0.079(7) 0.064(7) 0.035(6) 0.007(5) 0.026(6) C10 0.090(9) 0.088(9) 0.055(6) 0.003(6) -0.017(6) 0.044(7) C28 0.079(7) 0.090(8) 0.054(6) 0.029(5) 0.020(5) 0.016(6) C9 0.065(7) 0.080(9) 0.054(6) 0.016(6) -0.007(5) 0.022(6) C21 0.097(8) 0.091(8) 0.060(7) 0.033(6) -0.026(6) 0.009(7) O7 0.105(7) 0.086(6) 0.105(6) 0.023(5) 0.021(5) 0.010(5) C7 0.071(7) 0.101(8) 0.051(6) 0.030(5) 0.004(5) 0.041(6) C31 0.117(10) 0.103(10) 0.080(9) 0.036(8) 0.011(8) 0.035(9) C22 0.086(10) 0.099(11) 0.105(10) 0.052(9) -0.039(7) -0.018(8) C35 0.093(9) 0.078(9) 0.102(9) 0.054(7) 0.007(7) 0.019(7) C11 0.186(18) 0.095(12) 0.095(11) -0.013(8) -0.011(10) 0.057(11) C41 0.066(9) 0.173(14) 0.103(10) 0.049(9) -0.002(7) 0.051(9) C32 0.118(12) 0.087(11) 0.115(12) 0.009(9) -0.020(9) 0.019(9) C38 0.110(13) 0.24(2) 0.103(11) 0.054(12) 0.025(10) 0.113(14) C34 0.106(11) 0.081(10) 0.165(17) 0.063(11) 0.032(11) 0.030(9) C1 0.090(9) 0.151(12) 0.087(9) 0.050(8) 0.004(7) 0.038(9) C15 0.090(10) 0.140(12) 0.091(10) 0.004(8) 0.011(8) 0.064(10) C12 0.23(3) 0.112(15) 0.124(16) -0.010(12) 0.010(15) 0.091(17) C6 0.18(2) 0.40(4) 0.120(16) 0.17(2) -0.034(14) -0.08(2) C2 0.27(3) 0.21(2) 0.164(19) 0.081(17) 0.031(18) 0.16(2) C33 0.083(9) 0.081(9) 0.128(13) 0.015(9) 0.018(9) 0.013(7) C40 0.054(8) 0.23(2) 0.139(15) 0.079(14) 0.007(9) 0.033(10) C43 0.131(13) 0.100(10) 0.112(12) 0.027(8) 0.035(9) 0.027(9) C39 0.097(12) 0.28(2) 0.120(14) 0.118(15) 0.048(10) 0.103(14) C14 0.105(11) 0.184(18) 0.079(9) 0.023(10) 0.008(8) 0.075(12) C44 0.39(4) 0.63(6) 0.160(19) 0.20(3) 0.11(2) 0.47(5) C27 0.106(14) 0.139(14) 0.23(2) 0.095(15) -0.094(13) -0.017(11) C42 0.066(9) 0.187(17) 0.25(2) 0.163(17) 0.028(11) 0.030(10) C4 0.41(4) 0.181(18) 0.100(13) 0.083(13) -0.098(18) 0.02(2) C47 0.146(15) 0.104(11) 0.171(16) 0.047(10) 0.005(12) 0.059(11) C45 0.24(3) 0.136(15) 0.106(13) 0.001(10) 0.005(14) 0.054(16) C13 0.22(3) 0.22(3) 0.091(12) -0.006(15) -0.009(14) 0.17(2) C46 0.125(16) 0.160(17) 0.34(3) 0.14(2) 0.100(19) 0.012(13) C23 0.20(2) 0.104(13) 0.140(16) 0.028(12) -0.072(14) 0.002(14) C3 0.17(2) 0.31(4) 0.14(2) 0.010(19) -0.005(16) -0.02(2) C5 0.64(8) 0.16(2) 0.19(2) -0.033(17) -0.19(3) 0.22(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 O1 1.615(8) . ? Si1 C5 1.73(3) . ? Si1 C6 1.82(2) . ? Si1 C1 1.832(16) . ? O2 C9 1.352(13) . ? O2 C8 1.454(10) . ? Si2 C44 1.51(3) . ? Si2 O6 1.683(7) . ? Si2 C42 1.819(15) . ? Si2 C43 1.893(15) . ? O3 C18 1.345(12) . ? O3 C16 1.414(10) . ? O5 C18 1.327(12) . ? O5 C19 1.479(12) . ? O6 C17 1.406(10) . ? C16 C17 1.509(12) . ? C16 C8 1.512(12) . ? N1 C29 1.470(12) . ? N1 C20 1.481(14) . ? N1 C28 1.501(12) . ? O1 C7 1.428(12) . ? C30 C35 1.369(13) . ? C30 C31 1.386(16) . ? C30 C28 1.505(15) . ? C8 C7 1.516(13) . ? C20 C19 1.502(14) . ? C20 C21 1.559(14) . ? C17 C19 1.570(13) . ? O4 C18 1.204(12) . ? C36 C37 1.331(15) . ? C36 C41 1.400(17) . ? C36 C29 1.540(15) . ? C37 C38 1.332(18) . ? C10 C15 1.39(2) . ? C10 C11 1.398(19) . ? C10 C9 1.474(16) . ? C9 O7 1.205(12) . ? C21 C22 1.500(18) . ? C31 C32 1.358(19) . ? C22 C23 1.35(3) . ? C22 C27 1.39(2) . ? C35 C34 1.39(2) . ? C11 C12 1.34(3) . ? C41 C40 1.46(2) . ? C32 C33 1.38(2) . ? C38 C39 1.37(2) . ? C34 C33 1.34(2) . ? C1 C3 1.47(3) . ? C1 C4 1.538(19) . ? C1 C2 1.59(2) . ? C15 C14 1.41(2) . ? C12 C13 1.47(3) . ? C40 C39 1.32(2) . ? C14 C13 1.40(3) . ? C44 C47 1.55(2) . ? C44 C45 1.73(3) . ? C44 C46 1.92(4) . ? C27 C26 1.38(3) . ? C23 C24 1.55(3) . ? C25 C24 1.30(3) . ? C25 C26 1.35(3) . ? 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 O1 Si1 C5 108.0(12) . . ? O1 Si1 C6 110.1(7) . . ? C5 Si1 C6 111(2) . . ? O1 Si1 C1 105.4(6) . . ? C5 Si1 C1 112.7(12) . . ? C6 Si1 C1 109.7(10) . . ? C9 O2 C8 117.3(7) . . ? C44 Si2 O6 95.0(13) . . ? C44 Si2 C42 119.5(15) . . ? O6 Si2 C42 113.6(5) . . ? C44 Si2 C43 107.5(9) . . ? O6 Si2 C43 109.1(6) . . ? C42 Si2 C43 110.8(9) . . ? C18 O3 C16 118.4(7) . . ? C18 O5 C19 124.0(7) . . ? C17 O6 Si2 121.4(6) . . ? O3 C16 C17 110.3(7) . . ? O3 C16 C8 104.7(6) . . ? C17 C16 C8 118.9(6) . . ? C29 N1 C20 110.5(8) . . ? C29 N1 C28 109.3(7) . . ? C20 N1 C28 112.8(7) . . ? C7 O1 Si1 129.4(7) . . ? C35 C30 C31 117.8(11) . . ? C35 C30 C28 121.4(11) . . ? C31 C30 C28 120.8(9) . . ? O2 C8 C16 108.4(7) . . ? O2 C8 C7 106.2(7) . . ? C16 C8 C7 116.3(8) . . ? N1 C20 C19 114.2(8) . . ? N1 C20 C21 115.0(8) . . ? C19 C20 C21 113.6(10) . . ? O6 C17 C16 111.1(7) . . ? O6 C17 C19 110.3(8) . . ? C16 C17 C19 107.0(7) . . ? O5 C19 C20 108.6(7) . . ? O5 C19 C17 111.7(7) . . ? C20 C19 C17 115.0(9) . . ? C37 C36 C41 123.0(11) . . ? C37 C36 C29 121.7(11) . . ? C41 C36 C29 115.3(11) . . ? N1 C29 C36 112.1(8) . . ? C36 C37 C38 119.7(13) . . ? O4 C18 O5 121.7(10) . . ? O4 C18 O3 121.9(9) . . ? O5 C18 O3 116.4(10) . . ? C15 C10 C11 119.5(14) . . ? C15 C10 C9 123.0(11) . . ? C11 C10 C9 117.5(14) . . ? N1 C28 C30 113.3(8) . . ? O7 C9 O2 122.5(10) . . ? O7 C9 C10 125.6(11) . . ? O2 C9 C10 111.9(10) . . ? C22 C21 C20 113.3(9) . . ? O1 C7 C8 106.7(9) . . ? C32 C31 C30 120.2(12) . . ? C23 C22 C27 119.6(17) . . ? C23 C22 C21 121.8(16) . . ? C27 C22 C21 118.5(17) . . ? C30 C35 C34 119.2(13) . . ? C12 C11 C10 124(2) . . ? C36 C41 C40 114.2(13) . . ? C31 C32 C33 123.6(15) . . ? C37 C38 C39 121.7(16) . . ? C33 C34 C35 124.4(12) . . ? C3 C1 C4 111.1(19) . . ? C3 C1 C2 102(2) . . ? C4 C1 C2 108.5(15) . . ? C3 C1 Si1 112.1(14) . . ? C4 C1 Si1 112.0(12) . . ? C2 C1 Si1 110.8(13) . . ? C10 C15 C14 120.1(16) . . ? C11 C12 C13 115.6(18) . . ? C34 C33 C32 114.8(14) . . ? C39 C40 C41 120.8(14) . . ? C40 C39 C38 120.0(13) . . ? C13 C14 C15 118.3(19) . . ? Si2 C44 C47 132(3) . . ? Si2 C44 C45 115.6(13) . . ? C47 C44 C45 104.0(16) . . ? Si2 C44 C46 105.4(12) . . ? C47 C44 C46 98.2(19) . . ? C45 C44 C46 93(2) . . ? C26 C27 C22 129(2) . . ? C14 C13 C12 122.1(18) . . ? C22 C23 C24 116(2) . . ? C24 C25 C26 135(3) . . ? C25 C24 C23 114(2) . . ? C25 C26 C27 107(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 C44 Si2 O6 C17 168.9(12) . . . . ? C42 Si2 O6 C17 43.5(11) . . . . ? C43 Si2 O6 C17 -80.6(8) . . . . ? C18 O3 C16 C17 55.7(9) . . . . ? C18 O3 C16 C8 -175.2(8) . . . . ? C5 Si1 O1 C7 84.7(18) . . . . ? C6 Si1 O1 C7 -36.3(16) . . . . ? C1 Si1 O1 C7 -154.6(9) . . . . ? C9 O2 C8 C16 -105.8(9) . . . . ? C9 O2 C8 C7 128.6(8) . . . . ? O3 C16 C8 O2 -172.9(6) . . . . ? C17 C16 C8 O2 -49.3(10) . . . . ? O3 C16 C8 C7 -53.4(9) . . . . ? C17 C16 C8 C7 70.3(10) . . . . ? C29 N1 C20 C19 -149.8(8) . . . . ? C28 N1 C20 C19 87.5(10) . . . . ? C29 N1 C20 C21 76.2(11) . . . . ? C28 N1 C20 C21 -46.5(12) . . . . ? Si2 O6 C17 C16 149.5(6) . . . . ? Si2 O6 C17 C19 -92.0(8) . . . . ? O3 C16 C17 O6 62.9(8) . . . . ? C8 C16 C17 O6 -57.9(11) . . . . ? O3 C16 C17 C19 -57.5(8) . . . . ? C8 C16 C17 C19 -178.3(8) . . . . ? C18 O5 C19 C20 147.7(9) . . . . ? C18 O5 C19 C17 19.7(13) . . . . ? N1 C20 C19 O5 -78.3(10) . . . . ? C21 C20 C19 O5 56.3(11) . . . . ? N1 C20 C19 C17 47.7(11) . . . . ? C21 C20 C19 C17 -177.7(8) . . . . ? O6 C17 C19 O5 -98.0(9) . . . . ? C16 C17 C19 O5 22.9(10) . . . . ? O6 C17 C19 C20 137.6(8) . . . . ? C16 C17 C19 C20 -101.5(9) . . . . ? C20 N1 C29 C36 69.7(11) . . . . ? C28 N1 C29 C36 -165.6(9) . . . . ? C37 C36 C29 N1 65.5(15) . . . . ? C41 C36 C29 N1 -114.3(12) . . . . ? C41 C36 C37 C38 -3(2) . . . . ? C29 C36 C37 C38 176.9(13) . . . . ? C19 O5 C18 O4 152.2(10) . . . . ? C19 O5 C18 O3 -28.1(13) . . . . ? C16 O3 C18 O4 168.3(9) . . . . ? C16 O3 C18 O5 -11.5(11) . . . . ? C29 N1 C28 C30 60.6(11) . . . . ? C20 N1 C28 C30 -176.0(8) . . . . ? C35 C30 C28 N1 -128.7(10) . . . . ? C31 C30 C28 N1 51.8(14) . . . . ? C8 O2 C9 O7 5.3(13) . . . . ? C8 O2 C9 C10 -173.9(7) . . . . ? C15 C10 C9 O7 -164.5(12) . . . . ? C11 C10 C9 O7 12.3(16) . . . . ? C15 C10 C9 O2 14.7(14) . . . . ? C11 C10 C9 O2 -168.5(10) . . . . ? N1 C20 C21 C22 -165.4(11) . . . . ? C19 C20 C21 C22 60.4(14) . . . . ? Si1 O1 C7 C8 147.9(8) . . . . ? O2 C8 C7 O1 -78.8(9) . . . . ? C16 C8 C7 O1 160.4(7) . . . . ? C35 C30 C31 C32 0.6(19) . . . . ? C28 C30 C31 C32 -179.9(12) . . . . ? C20 C21 C22 C23 -104.5(16) . . . . ? C20 C21 C22 C27 71.9(15) . . . . ? C31 C30 C35 C34 -0.7(16) . . . . ? C28 C30 C35 C34 179.7(11) . . . . ? C15 C10 C11 C12 -4(2) . . . . ? C9 C10 C11 C12 179.3(16) . . . . ? C37 C36 C41 C40 -2(2) . . . . ? C29 C36 C41 C40 177.7(13) . . . . ? C30 C31 C32 C33 -1(2) . . . . ? C36 C37 C38 C39 3(2) . . . . ? C30 C35 C34 C33 2(2) . . . . ? O1 Si1 C1 C3 -52.5(19) . . . . ? C5 Si1 C1 C3 65(2) . . . . ? C6 Si1 C1 C3 -171(2) . . . . ? O1 Si1 C1 C4 -178.1(15) . . . . ? C5 Si1 C1 C4 -61(2) . . . . ? C6 Si1 C1 C4 63.4(18) . . . . ? O1 Si1 C1 C2 60.6(12) . . . . ? C5 Si1 C1 C2 178(2) . . . . ? C6 Si1 C1 C2 -57.9(15) . . . . ? C11 C10 C15 C14 3.0(19) . . . . ? C9 C10 C15 C14 179.8(11) . . . . ? C10 C11 C12 C13 3(3) . . . . ? C35 C34 C33 C32 -2(2) . . . . ? C31 C32 C33 C34 2(2) . . . . ? C36 C41 C40 C39 8(2) . . . . ? C41 C40 C39 C38 -9(3) . . . . ? C37 C38 C39 C40 3(3) . . . . ? C10 C15 C14 C13 -1(2) . . . . ? O6 Si2 C44 C47 67(2) . . . . ? C42 Si2 C44 C47 -172(2) . . . . ? C43 Si2 C44 C47 -45(3) . . . . ? O6 Si2 C44 C45 -76(2) . . . . ? C42 Si2 C44 C45 45(3) . . . . ? C43 Si2 C44 C45 172.6(18) . . . . ? O6 Si2 C44 C46 -176.5(14) . . . . ? C42 Si2 C44 C46 -55.7(17) . . . . ? C43 Si2 C44 C46 71.7(18) . . . . ? C23 C22 C27 C26 -1(3) . . . . ? C21 C22 C27 C26 -177.2(19) . . . . ? C15 C14 C13 C12 0(3) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C27 C22 C23 C24 6(2) . . . . ? C21 C22 C23 C24 -177.9(13) . . . . ? C26 C25 C24 C23 -4(4) . . . . ? C22 C23 C24 C25 -4(3) . . . . ? C24 C25 C26 C27 8(4) . . . . ? C22 C27 C26 C25 -6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.443 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.081 data_p21z2 _database_code_depnum_ccdc_archive 'CCDC 766571' #TrackingRef '508_web_deposit_cif_file_0_SantiagoDiaz-Oltra_1266433730.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C40 H61 N1 O6 Si2' _chemical_formula_sum 'C80 H122 N2 O12 Si4' _exptl_crystal_recrystallization_method 'MeOH, CH2Cl2' _chemical_melting_point ? _exptl_crystal_description Fiber _exptl_crystal_colour colorless _diffrn_ambient_temperature 153(2) _chemical_formula_weight 1416.16 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.4889(15) _cell_length_b 12.379(3) _cell_length_c 45.450(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.04(3) _cell_angle_gamma 90.00 _cell_volume 4213.4(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4244 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 20.07 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31100 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.2246 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 30.51 _reflns_number_total 22377 _reflns_number_gt 8381 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1834P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_number_reflns 22377 _refine_ls_number_parameters 883 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2755 _refine_ls_R_factor_gt 0.1152 _refine_ls_wR_factor_ref 0.3674 _refine_ls_wR_factor_gt 0.2810 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.269 _refine_ls_shift/su_mean 0.020 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 -0.7120(3) -0.91695(19) -0.01227(5) 0.0488(6) Uani 1 1 d . . . O2 O -0.6779(6) -1.2421(4) -0.07773(11) 0.0370(11) Uani 1 1 d . . . Si2 Si -0.3433(3) -0.9371(2) -0.14463(6) 0.0608(7) Uani 1 1 d . . . O8 O -0.1783(6) -0.1484(3) -0.42199(11) 0.0355(11) Uani 1 1 d . . . Si3 Si -0.2122(3) -0.47097(19) -0.48771(5) 0.0515(6) Uani 1 1 d . . . O10 O 0.1688(6) -0.1835(4) -0.43051(10) 0.0397(12) Uani 1 1 d . . . H10A H 0.1694 -0.1269 -0.4211 0.060 Uiso 1 1 calc R . . O6 O -0.4642(6) -1.0370(4) -0.13152(11) 0.0375(11) Uani 1 1 d . . . Si4 Si 0.1542(3) -0.4522(2) -0.35549(6) 0.0664(8) Uani 1 1 d . . . O4 O -0.3318(6) -1.2058(4) -0.06890(10) 0.0365(11) Uani 1 1 d . . . H4A H -0.3313 -1.2629 -0.0781 0.055 Uiso 1 1 calc R . . O12 O 0.0385(6) -0.3515(4) -0.36890(10) 0.0364(11) Uani 1 1 d . . . O11 O 0.0686(7) -0.0604(4) -0.37962(11) 0.0405(12) Uani 1 1 d . . . H11A H 0.1069 -0.0731 -0.3962 0.061 Uiso 1 1 calc R . . O3 O -0.9614(6) -1.1909(4) -0.08589(14) 0.0499(14) Uani 1 1 d . . . C51 C 0.0151(9) -0.1581(5) -0.36612(15) 0.0335(15) Uani 1 1 d . . . H51A H -0.1148 -0.1648 -0.3680 0.040 Uiso 1 1 calc R . . O9 O -0.4630(6) -0.1977(4) -0.41446(13) 0.0477(13) Uani 1 1 d . . . O5 O -0.4314(6) -1.3278(4) -0.11986(11) 0.0400(12) Uani 1 1 d . . . H5A H -0.4827 -1.3331 -0.1040 0.060 Uiso 1 1 calc R . . C14 C -0.8504(9) -1.2641(6) -0.08441(15) 0.0352(16) Uani 1 1 d . . . C11 C -0.4866(9) -1.2312(5) -0.13415(15) 0.0342(16) Uani 1 1 d . . . H11B H -0.6165 -1.2247 -0.1323 0.041 Uiso 1 1 calc R . . O7 O -0.1322(8) -0.4029(4) -0.45955(12) 0.0521(14) Uani 1 1 d . . . C8 C -0.6215(9) -1.1293(5) -0.07521(15) 0.0313(15) Uani 1 1 d . . . H8A H -0.6956 -1.0836 -0.0879 0.038 Uiso 1 1 calc R . . C54 C -0.3499(9) -0.1278(6) -0.41602(15) 0.0353(16) Uani 1 1 d . . . C50 C 0.1027(8) -0.2564(6) -0.38147(14) 0.0326(15) Uani 1 1 d . . . H50A H 0.2317 -0.2530 -0.3780 0.039 Uiso 1 1 calc R . . C48 C -0.1220(9) -0.2574(6) -0.42512(15) 0.0329(15) Uani 1 1 d . . . H48A H -0.1952 -0.3039 -0.4125 0.040 Uiso 1 1 calc R . . C49 C 0.0709(9) -0.2622(5) -0.41504(15) 0.0316(15) Uani 1 1 d . . . H49A H 0.1171 -0.3324 -0.4215 0.038 Uiso 1 1 calc R . . C7 C -0.6484(11) -1.0986(6) -0.04360(16) 0.0408(18) Uani 1 1 d . . . H7A H -0.7658 -1.1218 -0.0372 0.049 Uiso 1 1 calc R . . H7B H -0.5599 -1.1344 -0.0315 0.049 Uiso 1 1 calc R . . C9 C -0.4299(8) -1.1253(5) -0.08530(15) 0.0292(15) Uani 1 1 d . . . H9A H -0.3829 -1.0550 -0.0792 0.035 Uiso 1 1 calc R . . C10 C -0.3979(9) -1.1336(5) -0.11805(15) 0.0326(15) Uani 1 1 d . . . H10B H -0.2687 -1.1371 -0.1214 0.039 Uiso 1 1 calc R . . O1 O -0.6327(7) -0.9850(4) -0.04029(11) 0.0485(13) Uani 1 1 d . . . N2 N -0.0698(9) -0.0859(5) -0.31662(13) 0.0456(16) Uani 1 1 d . . . C56 C -0.5498(10) 0.0218(6) -0.40047(18) 0.0470(19) Uani 1 1 d . . . H56A H -0.6315 -0.0304 -0.3945 0.056 Uiso 1 1 calc R . . C15 C -0.8859(9) -1.3768(5) -0.08760(16) 0.0351(16) Uani 1 1 d . . . C55 C -0.3874(10) -0.0087(6) -0.41244(17) 0.0386(17) Uani 1 1 d . . . C47 C -0.1480(11) -0.2898(6) -0.45691(17) 0.0449(19) Uani 1 1 d . . . H47A H -0.2652 -0.2670 -0.4636 0.054 Uiso 1 1 calc R . . H47B H -0.0589 -0.2547 -0.4691 0.054 Uiso 1 1 calc R . . N1 N -0.5720(9) -1.3045(5) -0.18266(15) 0.0460(17) Uani 1 1 d . . . C4 C -0.9574(12) -0.8944(6) -0.01510(18) 0.051(2) Uani 1 1 d . . . C44 C -0.4586(12) -0.4921(7) -0.4846(2) 0.058(2) Uani 1 1 d . . . C16 C -1.0488(10) -1.4096(7) -0.09943(16) 0.0440(18) Uani 1 1 d . . . H16A H -1.1308 -1.3572 -0.1052 0.053 Uiso 1 1 calc R . . C75 C -0.1884(14) 0.0995(6) -0.30888(18) 0.051(2) Uani 1 1 d . . . C60 C -0.2635(10) 0.0672(6) -0.42208(18) 0.0482(19) Uani 1 1 d . . . H60A H -0.1569 0.0470 -0.4310 0.058 Uiso 1 1 calc R . . C20 C -0.7629(11) -1.4562(6) -0.07870(17) 0.0468(18) Uani 1 1 d . . . H20A H -0.6538 -1.4365 -0.0705 0.056 Uiso 1 1 calc R . . C12 C -0.4390(11) -1.2371(7) -0.16657(16) 0.048(2) Uani 1 1 d . . . H12A H -0.4537 -1.1635 -0.1742 0.058 Uiso 1 1 calc R . . C52 C 0.0607(10) -0.1518(6) -0.33371(15) 0.0403(17) Uani 1 1 d . . . H52A H 0.0467 -0.2257 -0.3263 0.048 Uiso 1 1 calc R . . C19 C -0.8071(14) -1.5652(6) -0.0823(2) 0.065(3) Uani 1 1 d . . . H19A H -0.7268 -1.6187 -0.0767 0.078 Uiso 1 1 calc R . . C17 C -1.0920(13) -1.5151(8) -0.1029(2) 0.061(2) Uani 1 1 d . . . H17A H -1.2016 -1.5348 -0.1109 0.073 Uiso 1 1 calc R . . C66 C 0.0359(16) -0.5793(9) -0.3649(3) 0.083(3) Uani 1 1 d . . . C21 C -0.1137(11) -0.9361(9) -0.1278(2) 0.073(3) Uani 1 1 d . . . H21A H -0.1236 -0.9348 -0.1068 0.110 Uiso 1 1 calc R . . H21B H -0.0501 -0.8732 -0.1344 0.110 Uiso 1 1 calc R . . H21C H -0.0501 -0.9998 -0.1338 0.110 Uiso 1 1 calc R . . C22 C -0.3269(18) -0.9430(14) -0.1865(2) 0.113(5) Uani 1 1 d . . . H22A H -0.4447 -0.9434 -0.1948 0.170 Uiso 1 1 calc R . . H22B H -0.2649 -1.0076 -0.1922 0.170 Uiso 1 1 calc R . . H22C H -0.2628 -0.8810 -0.1935 0.170 Uiso 1 1 calc R . . C53 C 0.2530(14) -0.1221(10) -0.3271(2) 0.080(3) Uani 1 1 d . . . H53A H 0.3313 -0.1671 -0.3385 0.120 Uiso 1 1 calc R . . H53B H 0.2766 -0.1326 -0.3066 0.120 Uiso 1 1 calc R . . H53C H 0.2730 -0.0477 -0.3322 0.120 Uiso 1 1 calc R . . C57 C -0.5900(12) 0.1309(8) -0.39735(19) 0.059(2) Uani 1 1 d . . . H57A H -0.7020 0.1519 -0.3906 0.070 Uiso 1 1 calc R . . C13 C -0.2458(13) -1.2676(10) -0.1728(2) 0.081(3) Uani 1 1 d . . . H13A H -0.2258 -1.2676 -0.1937 0.121 Uiso 1 1 calc R . . H13B H -0.2222 -1.3383 -0.1651 0.121 Uiso 1 1 calc R . . H13C H -0.1677 -1.2161 -0.1636 0.121 Uiso 1 1 calc R . . C23 C -0.3785(16) -0.7155(8) -0.1519(2) 0.082(3) Uani 1 1 d . . . H23A H -0.4466 -0.6513 -0.1480 0.123 Uiso 1 1 calc R . . H23B H -0.3707 -0.7267 -0.1727 0.123 Uiso 1 1 calc R . . H23C H -0.2606 -0.7074 -0.1439 0.123 Uiso 1 1 calc R . . C73 C -0.1350(17) -0.2309(7) -0.2769(3) 0.083(4) Uani 1 1 d . . . C62 C 0.3793(13) -0.4584(9) -0.3735(2) 0.072(3) Uani 1 1 d . . . H62A H 0.3647 -0.4599 -0.3945 0.108 Uiso 1 1 calc R . . H62B H 0.4406 -0.5225 -0.3673 0.108 Uiso 1 1 calc R . . H62C H 0.4477 -0.3960 -0.3681 0.108 Uiso 1 1 calc R . . C71 C -0.161(2) -0.3992(13) -0.2540(3) 0.088(5) Uani 1 1 d . . . H71A H -0.1205 -0.4472 -0.2397 0.106 Uiso 1 1 calc R . . C26 C -0.4704(16) -0.8127(9) -0.1375(4) 0.118(6) Uani 1 1 d . . . C61 C 0.167(2) -0.4514(15) -0.3140(2) 0.130(6) Uani 1 1 d . . . H61A H 0.0491 -0.4494 -0.3060 0.196 Uiso 1 1 calc R . . H61B H 0.2327 -0.3889 -0.3076 0.196 Uiso 1 1 calc R . . H61C H 0.2274 -0.5154 -0.3074 0.196 Uiso 1 1 calc R . . C58 C -0.4680(16) 0.2054(8) -0.4040(2) 0.075(3) Uani 1 1 d . . . H58A H -0.4898 0.2775 -0.3995 0.090 Uiso 1 1 calc R . . C72 C -0.0814(17) -0.3010(11) -0.2554(2) 0.080(3) Uani 1 1 d . . . H72A H 0.0073 -0.2817 -0.2420 0.096 Uiso 1 1 calc R . . C70 C -0.282(4) -0.4293(15) -0.2702(5) 0.133(10) Uani 1 1 d . . . H70A H -0.3279 -0.4986 -0.2680 0.159 Uiso 1 1 calc R . . C18 C -0.9706(15) -1.5932(7) -0.0942(2) 0.071(3) Uani 1 1 d . . . H18A H -0.9994 -1.6658 -0.0965 0.085 Uiso 1 1 calc R . . C1 C -1.0208(16) -0.8218(9) 0.0089(2) 0.084(3) Uani 1 1 d . . . H1A H -1.1473 -0.8113 0.0071 0.126 Uiso 1 1 calc R . . H1B H -0.9613 -0.7533 0.0075 0.126 Uiso 1 1 calc R . . H1C H -0.9945 -0.8540 0.0277 0.126 Uiso 1 1 calc R . . C45 C -0.165(3) -0.3985(13) -0.5230(2) 0.151(8) Uani 1 1 d . . . H45A H -0.2316 -0.3321 -0.5235 0.227 Uiso 1 1 calc R . . H45B H -0.2007 -0.4431 -0.5393 0.227 Uiso 1 1 calc R . . H45C H -0.0401 -0.3831 -0.5243 0.227 Uiso 1 1 calc R . . C46 C -0.0917(15) -0.6028(9) -0.4841(3) 0.097(4) Uani 1 1 d . . . H46A H -0.1238 -0.6365 -0.4658 0.145 Uiso 1 1 calc R . . H46B H 0.0348 -0.5903 -0.4845 0.145 Uiso 1 1 calc R . . H46C H -0.1242 -0.6493 -0.5001 0.145 Uiso 1 1 calc R . . C5 C -0.5932(15) -0.7898(10) -0.0146(3) 0.109(5) Uani 1 1 d . . . H5B H -0.6245 -0.7537 -0.0325 0.164 Uiso 1 1 calc R . . H5C H -0.4669 -0.8032 -0.0142 0.164 Uiso 1 1 calc R . . H5D H -0.6251 -0.7451 0.0019 0.164 Uiso 1 1 calc R . . C6 C -0.657(2) -0.9865(13) 0.0218(2) 0.121(6) Uani 1 1 d . . . H6A H -0.7202 -1.0540 0.0226 0.181 Uiso 1 1 calc R . . H6B H -0.6918 -0.9425 0.0382 0.181 Uiso 1 1 calc R . . H6C H -0.5311 -0.9997 0.0226 0.181 Uiso 1 1 calc R . . C79 C -0.317(3) 0.2386(10) -0.2757(4) 0.119(5) Uani 1 1 d . . . H79A H -0.3154 0.2861 -0.2598 0.143 Uiso 1 1 calc R . . C59 C -0.3086(15) 0.1767(8) -0.4176(3) 0.077(3) Uani 1 1 d . . . H59A H -0.2305 0.2304 -0.4238 0.092 Uiso 1 1 calc R . . C41 C -0.5697(19) -0.3887(10) -0.4837(5) 0.175(10) Uani 1 1 d . . . H41A H -0.6938 -0.4069 -0.4818 0.263 Uiso 1 1 calc R . . H41B H -0.5516 -0.3485 -0.5015 0.263 Uiso 1 1 calc R . . H41C H -0.5336 -0.3457 -0.4671 0.263 Uiso 1 1 calc R . . C3 C -1.0664(18) -0.9975(11) -0.0141(5) 0.165(9) Uani 1 1 d . . . H3A H -1.1909 -0.9803 -0.0159 0.248 Uiso 1 1 calc R . . H3B H -1.0455 -1.0339 0.0042 0.248 Uiso 1 1 calc R . . H3C H -1.0317 -1.0437 -0.0301 0.248 Uiso 1 1 calc R . . C25 C -0.6582(15) -0.8230(8) -0.1504(4) 0.132(7) Uani 1 1 d . . . H25A H -0.7233 -0.7575 -0.1469 0.198 Uiso 1 1 calc R . . H25B H -0.7189 -0.8823 -0.1412 0.198 Uiso 1 1 calc R . . H25C H -0.6503 -0.8356 -0.1712 0.198 Uiso 1 1 calc R . . C64 C 0.1180(17) -0.6764(8) -0.3495(3) 0.101(4) Uani 1 1 d . . . H64A H 0.0523 -0.7403 -0.3546 0.152 Uiso 1 1 calc R . . H64B H 0.1135 -0.6658 -0.3286 0.152 Uiso 1 1 calc R . . H64C H 0.2400 -0.6844 -0.3556 0.152 Uiso 1 1 calc R . . C78 C -0.4434(19) 0.2338(8) -0.2947(3) 0.092(4) Uani 1 1 d . . . H78A H -0.5414 0.2796 -0.2933 0.110 Uiso 1 1 calc R . . C80 C -0.151(2) 0.145(2) -0.2834(3) 0.170(10) Uani 1 1 d . . . H80A H -0.0533 0.1296 -0.2716 0.204 Uiso 1 1 calc R . . C42 C -0.5207(15) -0.5663(11) -0.5095(3) 0.108(5) Uani 1 1 d . . . H42A H -0.6472 -0.5776 -0.5080 0.163 Uiso 1 1 calc R . . H42B H -0.4602 -0.6345 -0.5080 0.163 Uiso 1 1 calc R . . H42C H -0.4938 -0.5335 -0.5281 0.163 Uiso 1 1 calc R . . C65 C -0.1609(16) -0.5710(10) -0.3552(5) 0.157(8) Uani 1 1 d . . . H65A H -0.2214 -0.6374 -0.3596 0.236 Uiso 1 1 calc R . . H65B H -0.2178 -0.5126 -0.3654 0.236 Uiso 1 1 calc R . . H65C H -0.1660 -0.5579 -0.3344 0.236 Uiso 1 1 calc R . . C43 C -0.490(2) -0.5581(17) -0.4557(3) 0.152(7) Uani 1 1 d . . . H43A H -0.6157 -0.5707 -0.4531 0.228 Uiso 1 1 calc R . . H43B H -0.4453 -0.5180 -0.4392 0.228 Uiso 1 1 calc R . . H43C H -0.4289 -0.6261 -0.4569 0.228 Uiso 1 1 calc R . . C2 C -0.990(2) -0.843(2) -0.0462(4) 0.199(11) Uani 1 1 d . . . H2A H -1.1158 -0.8300 -0.0487 0.298 Uiso 1 1 calc R . . H2B H -0.9497 -0.8922 -0.0611 0.298 Uiso 1 1 calc R . . H2C H -0.9262 -0.7764 -0.0477 0.298 Uiso 1 1 calc R . . C74 C -0.049(3) 0.0275(9) -0.3216(4) 0.208(13) Uani 1 1 d . . . H74A H -0.0452 0.0395 -0.3427 0.250 Uiso 1 1 calc R . . H74B H 0.0660 0.0492 -0.3137 0.250 Uiso 1 1 calc R . . C35 C -0.6346(17) -1.1587(7) -0.2237(3) 0.075(4) Uani 1 1 d . . . C28 C -0.6833(15) -1.4877(7) -0.19173(19) 0.055(2) Uani 1 1 d . . . C39 C -0.668(2) -0.9850(10) -0.2456(3) 0.087(4) Uani 1 1 d . . . H39A H -0.6354 -0.9324 -0.2592 0.104 Uiso 1 1 calc R . . C36 C -0.759(2) -1.1372(12) -0.2045(3) 0.097(5) Uani 1 1 d . . . H36A H -0.7896 -1.1894 -0.1907 0.116 Uiso 1 1 calc R . . C40 C -0.5854(15) -1.0830(12) -0.24504(19) 0.080(3) Uani 1 1 d . . . H40A H -0.4972 -1.0994 -0.2587 0.096 Uiso 1 1 calc R . . C34 C -0.573(2) -1.2727(14) -0.2137(5) 0.183(11) Uani 1 1 d . . . H34A H -0.6463 -1.3247 -0.2240 0.220 Uiso 1 1 calc R . . H34B H -0.4517 -1.2822 -0.2209 0.220 Uiso 1 1 calc R . . C27 C -0.554(3) -1.4164(8) -0.1775(4) 0.215(13) Uani 1 1 d . . . H27A H -0.5606 -1.4285 -0.1565 0.259 Uiso 1 1 calc R . . H27B H -0.4356 -1.4380 -0.1838 0.259 Uiso 1 1 calc R . . C63 C 0.040(2) -0.5899(12) -0.3996(3) 0.123(5) Uani 1 1 d . . . H63A H -0.0202 -0.6551 -0.4053 0.184 Uiso 1 1 calc R . . H63B H 0.1613 -0.5921 -0.4062 0.184 Uiso 1 1 calc R . . H63C H -0.0198 -0.5289 -0.4082 0.184 Uiso 1 1 calc R . . C24 C -0.452(2) -0.8019(12) -0.0990(3) 0.124(5) Uani 1 1 d . . . H24A H -0.5140 -0.7383 -0.0925 0.186 Uiso 1 1 calc R . . H24B H -0.3286 -0.7970 -0.0936 0.186 Uiso 1 1 calc R . . H24C H -0.5044 -0.8645 -0.0900 0.186 Uiso 1 1 calc R . . C31 C -0.9441(19) -1.6201(7) -0.2044(3) 0.087(4) Uani 1 1 d . . . H31A H -1.0333 -1.6723 -0.2052 0.105 Uiso 1 1 calc R . . C69 C -0.340(3) -0.373(2) -0.2885(6) 0.177(12) Uani 1 1 d . . . H69A H -0.4369 -0.3985 -0.2992 0.213 Uiso 1 1 calc R . . C68 C -0.277(2) -0.2688(16) -0.2956(2) 0.111(6) Uani 1 1 d . . . H68A H -0.3222 -0.2282 -0.3111 0.134 Uiso 1 1 calc R . . C67 C -0.0683(17) -0.1161(11) -0.2839(3) 0.099(4) Uani 1 1 d . . . H67A H 0.0527 -0.1088 -0.2765 0.119 Uiso 1 1 calc R . . H67B H -0.1422 -0.0648 -0.2733 0.119 Uiso 1 1 calc R . . C38 C -0.7974(19) -0.9670(9) -0.2258(4) 0.096(4) Uani 1 1 d . . . H38A H -0.8573 -0.9013 -0.2270 0.115 Uiso 1 1 calc R . . C37 C -0.849(3) -1.0370(14) -0.2041(3) 0.131(7) Uani 1 1 d . . . H37A H -0.9360 -1.0200 -0.1902 0.157 Uiso 1 1 calc R . . C76 C -0.328(3) 0.0994(13) -0.3237(3) 0.114(5) Uani 1 1 d . . . H76A H -0.3467 0.0517 -0.3392 0.136 Uiso 1 1 calc R . . C77 C -0.433(3) 0.1620(11) -0.3169(3) 0.121(6) Uani 1 1 d . . . H77A H -0.5316 0.1635 -0.3293 0.145 Uiso 1 1 calc R . . C30 C -0.789(4) -1.6078(18) -0.2302(5) 0.237(16) Uani 1 1 d . . . H30A H -0.7866 -1.6363 -0.2491 0.284 Uiso 1 1 calc R . . C29 C -0.658(2) -1.5395(15) -0.2151(3) 0.134(7) Uani 1 1 d . . . H29A H -0.5457 -1.5341 -0.2236 0.161 Uiso 1 1 calc R . . C33 C -0.834(4) -1.481(2) -0.1766(5) 0.207(13) Uani 1 1 d . . . H33A H -0.8609 -1.4285 -0.1627 0.248 Uiso 1 1 calc R . . C32 C -0.932(3) -1.5542(11) -0.1838(3) 0.138(7) Uani 1 1 d . . . H32A H -1.0232 -1.5640 -0.1702 0.166 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 0.0446(13) 0.0579(14) 0.0438(13) -0.0217(11) -0.0062(10) 0.0055(10) O2 0.021(2) 0.029(2) 0.061(3) 0.003(2) 0.002(2) 0.0003(19) Si2 0.0457(14) 0.0610(16) 0.0757(17) 0.0139(13) -0.0088(12) -0.0167(12) O8 0.022(2) 0.028(2) 0.057(3) 0.004(2) -0.004(2) -0.0012(19) Si3 0.0449(13) 0.0599(15) 0.0498(14) -0.0221(11) 0.0060(10) -0.0081(11) O10 0.029(3) 0.049(3) 0.041(3) -0.004(2) 0.011(2) -0.010(2) O6 0.029(3) 0.037(3) 0.046(3) 0.005(2) 0.005(2) -0.003(2) Si4 0.0432(14) 0.0642(17) 0.0919(19) 0.0205(14) 0.0131(13) 0.0193(12) O4 0.027(3) 0.042(3) 0.040(3) -0.001(2) -0.002(2) 0.009(2) O12 0.033(3) 0.040(3) 0.036(3) 0.007(2) -0.003(2) 0.002(2) O11 0.037(3) 0.043(3) 0.042(3) -0.003(2) 0.011(2) -0.004(2) O3 0.020(3) 0.042(3) 0.088(4) 0.006(3) -0.004(3) 0.008(2) C51 0.025(4) 0.038(4) 0.038(4) 0.003(3) 0.005(3) -0.006(3) O9 0.025(3) 0.039(3) 0.080(4) 0.006(3) 0.001(3) -0.006(2) O5 0.033(3) 0.044(3) 0.043(3) 0.001(2) -0.002(2) 0.005(2) C14 0.025(4) 0.044(4) 0.037(4) 0.004(3) 0.005(3) 0.005(3) C11 0.019(3) 0.036(4) 0.048(4) -0.004(3) -0.006(3) 0.002(3) O7 0.056(4) 0.038(3) 0.063(3) -0.012(2) -0.018(3) 0.007(2) C8 0.024(3) 0.029(4) 0.041(4) -0.008(3) 0.005(3) -0.001(3) C54 0.028(4) 0.045(4) 0.032(4) 0.004(3) -0.003(3) -0.003(3) C50 0.014(3) 0.050(4) 0.033(4) 0.002(3) 0.002(3) 0.002(3) C48 0.022(3) 0.042(4) 0.035(4) -0.002(3) -0.002(3) -0.003(3) C49 0.025(4) 0.029(3) 0.040(4) -0.008(3) 0.010(3) -0.002(3) C7 0.046(5) 0.033(4) 0.044(4) -0.004(3) 0.014(4) 0.002(3) C9 0.020(3) 0.024(3) 0.044(4) -0.003(3) -0.003(3) -0.001(2) C10 0.018(3) 0.041(4) 0.039(4) 0.006(3) 0.003(3) -0.001(3) O1 0.050(3) 0.043(3) 0.052(3) -0.009(2) 0.022(3) -0.004(2) N2 0.063(5) 0.043(4) 0.031(3) -0.007(3) 0.014(3) -0.003(3) C56 0.033(4) 0.043(4) 0.064(5) -0.012(4) 0.003(4) 0.000(3) C15 0.028(4) 0.035(4) 0.042(4) 0.005(3) 0.002(3) -0.001(3) C55 0.030(4) 0.037(4) 0.049(4) 0.000(3) -0.005(3) 0.001(3) C47 0.043(5) 0.040(4) 0.052(5) 0.002(3) -0.012(4) -0.010(3) N1 0.053(4) 0.046(4) 0.039(4) -0.007(3) -0.017(3) 0.003(3) C4 0.057(5) 0.046(5) 0.051(5) -0.015(4) 0.012(4) -0.004(4) C44 0.055(6) 0.050(5) 0.068(6) -0.023(4) -0.010(5) -0.003(4) C16 0.033(4) 0.053(5) 0.045(4) -0.013(4) 0.001(3) -0.001(3) C75 0.076(6) 0.041(5) 0.038(5) -0.011(4) 0.005(4) -0.010(4) C60 0.039(4) 0.035(4) 0.071(5) 0.009(4) 0.006(4) 0.000(3) C20 0.041(4) 0.045(5) 0.054(5) 0.005(4) 0.006(4) 0.006(4) C12 0.048(5) 0.054(5) 0.042(4) -0.015(4) -0.010(4) 0.002(4) C52 0.038(4) 0.047(4) 0.036(4) -0.014(3) 0.013(3) 0.002(3) C19 0.084(7) 0.026(4) 0.086(7) 0.016(4) -0.006(6) -0.002(4) C17 0.054(6) 0.067(6) 0.061(6) -0.010(5) 0.003(5) -0.014(5) C66 0.079(8) 0.083(7) 0.087(8) 0.001(6) -0.005(6) 0.023(6) C21 0.035(5) 0.083(7) 0.102(7) -0.005(6) -0.012(5) -0.022(5) C22 0.101(10) 0.180(14) 0.058(6) -0.016(8) 0.006(6) -0.056(10) C53 0.067(7) 0.124(10) 0.049(6) -0.032(6) 0.005(5) -0.027(6) C57 0.047(5) 0.070(6) 0.059(5) -0.020(4) 0.006(4) 0.017(5) C13 0.063(7) 0.130(10) 0.048(5) -0.035(6) 0.007(5) 0.021(6) C23 0.105(9) 0.045(5) 0.096(8) 0.022(5) -0.003(7) -0.025(5) C73 0.102(9) 0.038(5) 0.110(9) 0.013(5) 0.085(8) 0.007(5) C62 0.058(6) 0.095(8) 0.064(6) 0.008(6) 0.010(5) 0.025(5) C71 0.103(11) 0.107(12) 0.055(7) 0.011(7) 0.031(6) 0.052(9) C26 0.066(8) 0.045(6) 0.244(19) 0.041(8) -0.017(10) -0.011(5) C61 0.132(12) 0.216(17) 0.044(6) 0.000(8) -0.004(6) 0.089(12) C58 0.080(8) 0.040(5) 0.104(8) -0.017(5) 0.018(6) 0.003(5) C72 0.099(9) 0.083(8) 0.059(7) -0.015(6) -0.004(6) 0.013(7) C70 0.19(2) 0.074(10) 0.134(17) 0.017(11) 0.103(16) 0.039(13) C18 0.086(8) 0.034(5) 0.093(7) -0.005(5) 0.002(6) -0.018(5) C1 0.088(8) 0.082(7) 0.081(7) -0.024(6) 0.008(6) 0.028(6) C45 0.25(2) 0.163(14) 0.041(6) -0.019(7) 0.020(8) -0.116(14) C46 0.067(7) 0.081(8) 0.142(11) -0.064(7) -0.007(7) 0.026(6) C5 0.057(7) 0.096(9) 0.174(13) -0.088(9) 0.015(7) -0.025(6) C6 0.147(14) 0.152(13) 0.063(7) -0.001(8) 0.006(8) 0.071(11) C79 0.165(16) 0.060(8) 0.133(13) -0.026(8) 0.012(12) -0.019(8) C59 0.072(7) 0.044(5) 0.114(9) 0.016(5) -0.005(7) -0.009(5) C41 0.078(9) 0.071(9) 0.38(3) -0.053(12) -0.090(14) 0.012(7) C3 0.072(9) 0.078(9) 0.35(3) -0.069(12) 0.079(13) -0.011(7) C25 0.057(7) 0.034(5) 0.31(2) 0.024(8) -0.032(10) 0.003(5) C64 0.090(9) 0.051(6) 0.162(12) 0.026(7) 0.032(8) 0.024(6) C78 0.106(10) 0.050(6) 0.121(10) -0.030(7) 0.003(8) 0.031(6) C80 0.065(9) 0.37(3) 0.074(9) -0.071(13) 0.008(7) -0.050(13) C42 0.059(7) 0.130(10) 0.137(11) -0.089(9) -0.005(7) -0.021(7) C65 0.048(7) 0.064(8) 0.36(3) 0.038(12) 0.025(11) -0.010(6) C43 0.104(12) 0.24(2) 0.107(11) 0.058(12) 0.029(9) -0.067(13) C2 0.092(12) 0.38(3) 0.125(13) 0.063(17) -0.036(10) 0.089(16) C74 0.33(3) 0.034(6) 0.27(2) -0.005(9) 0.23(2) -0.010(10) C35 0.087(8) 0.045(5) 0.091(9) 0.003(6) -0.068(7) 0.002(5) C28 0.084(7) 0.045(5) 0.036(5) -0.002(4) -0.003(4) 0.004(4) C39 0.118(11) 0.064(7) 0.078(8) 0.017(6) -0.061(8) -0.032(7) C36 0.145(13) 0.097(10) 0.049(7) 0.024(7) -0.034(8) -0.054(9) C40 0.068(7) 0.141(12) 0.031(5) -0.017(6) 0.008(5) -0.014(7) C34 0.105(12) 0.158(16) 0.29(3) -0.165(18) -0.080(14) 0.057(11) C27 0.35(3) 0.026(5) 0.27(2) 0.015(8) -0.26(2) -0.008(9) C63 0.148(14) 0.101(10) 0.120(11) -0.059(8) -0.010(9) -0.027(9) C24 0.107(11) 0.121(11) 0.143(13) -0.077(10) 0.011(9) 0.029(9) C31 0.147(11) 0.028(5) 0.086(8) -0.008(5) -0.040(8) -0.026(6) C69 0.117(15) 0.19(2) 0.23(3) -0.16(2) 0.083(17) -0.082(16) C68 0.096(10) 0.188(16) 0.050(7) 0.020(8) 0.005(7) 0.081(11) C67 0.069(8) 0.129(11) 0.099(9) -0.011(8) 0.028(7) 0.000(7) C38 0.096(10) 0.055(7) 0.136(12) -0.038(8) -0.045(9) 0.018(7) C37 0.23(2) 0.098(11) 0.064(8) -0.002(8) 0.018(10) -0.052(12) C76 0.166(17) 0.090(10) 0.085(9) -0.002(8) -0.004(10) 0.014(10) C77 0.22(2) 0.081(10) 0.064(8) 0.006(7) 0.012(9) 0.030(11) C30 0.32(3) 0.22(2) 0.175(19) -0.158(18) -0.14(2) 0.18(2) C29 0.089(10) 0.232(19) 0.082(9) -0.069(11) -0.004(8) 0.054(11) C33 0.24(3) 0.24(3) 0.137(16) 0.108(19) -0.060(18) -0.11(2) C32 0.24(2) 0.064(9) 0.107(12) 0.019(8) 0.004(13) -0.034(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 O1 1.638(5) . ? Si1 C5 1.811(11) . ? Si1 C6 1.819(12) . ? Si1 C4 1.863(9) . ? O2 C14 1.355(8) . ? O2 C8 1.463(8) . ? Si2 O6 1.644(5) . ? Si2 C26 1.840(14) . ? Si2 C21 1.881(8) . ? Si2 C22 1.908(10) . ? O8 C54 1.338(8) . ? O8 C48 1.421(8) . ? Si3 O7 1.645(5) . ? Si3 C45 1.871(12) . ? Si3 C44 1.869(10) . ? Si3 C46 1.873(10) . ? O10 C49 1.408(8) . ? O6 C10 1.432(8) . ? Si4 O12 1.636(5) . ? Si4 C66 1.856(13) . ? Si4 C62 1.877(10) . ? Si4 C61 1.887(10) . ? O4 C9 1.445(7) . ? O12 C50 1.394(8) . ? O11 C51 1.414(8) . ? O3 C14 1.231(8) . ? C51 C52 1.514(10) . ? C51 C50 1.549(10) . ? O9 C54 1.213(8) . ? O5 C11 1.421(8) . ? C14 C15 1.428(10) . ? C11 C12 1.518(11) . ? C11 C10 1.561(9) . ? O7 C47 1.411(9) . ? C8 C7 1.500(10) . ? C8 C9 1.507(9) . ? C54 C55 1.510(10) . ? C50 C49 1.546(9) . ? C48 C47 1.512(10) . ? C48 C49 1.517(9) . ? C7 O1 1.419(9) . ? C9 C10 1.511(10) . ? N2 C74 1.431(13) . ? N2 C52 1.491(9) . ? N2 C67 1.535(13) . ? C56 C55 1.385(11) . ? C56 C57 1.391(11) . ? C15 C16 1.393(10) . ? C15 C20 1.406(10) . ? C55 C60 1.392(10) . ? N1 C27 1.411(12) . ? N1 C34 1.46(2) . ? N1 C12 1.491(10) . ? C4 C1 1.493(12) . ? C4 C3 1.516(15) . ? C4 C2 1.567(18) . ? C44 C42 1.528(12) . ? C44 C41 1.527(15) . ? C44 C43 1.568(16) . ? C16 C17 1.355(11) . ? C75 C76 1.244(18) . ? C75 C80 1.317(15) . ? C75 C74 1.492(17) . ? C75 C77 2.02(2) . ? C60 C59 1.411(13) . ? C20 C19 1.399(12) . ? C12 C13 1.522(12) . ? C52 C53 1.516(12) . ? C19 C18 1.383(14) . ? C17 C18 1.383(14) . ? C66 C64 1.521(15) . ? C66 C65 1.543(17) . ? C66 C63 1.580(17) . ? C57 C58 1.333(14) . ? C23 C26 1.532(15) . ? C73 C72 1.368(16) . ? C73 C68 1.44(2) . ? C73 C67 1.539(16) . ? C71 C70 1.23(3) . ? C71 C72 1.354(19) . ? C26 C25 1.528(16) . ? C26 C24 1.76(2) . ? C58 C59 1.390(15) . ? C70 C69 1.17(3) . ? C79 C78 1.282(19) . ? C79 C80 1.74(3) . ? C78 C77 1.345(17) . ? C35 C36 1.306(19) . ? C35 C40 1.398(17) . ? C35 C34 1.55(2) . ? C28 C29 1.254(15) . ? C28 C33 1.33(3) . ? C28 C27 1.460(15) . ? C39 C38 1.341(18) . ? C39 C40 1.361(17) . ? C36 C37 1.41(2) . ? C31 C32 1.245(17) . ? C31 C30 1.66(3) . ? C69 C68 1.41(3) . ? C38 C37 1.37(2) . ? C76 C77 1.14(2) . ? C30 C29 1.47(3) . ? C33 C32 1.21(2) . ? 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 O1 Si1 C5 102.9(5) . . ? O1 Si1 C6 109.7(5) . . ? C5 Si1 C6 110.5(8) . . ? O1 Si1 C4 112.4(3) . . ? C5 Si1 C4 110.5(5) . . ? C6 Si1 C4 110.6(6) . . ? C14 O2 C8 119.0(5) . . ? O6 Si2 C26 106.3(5) . . ? O6 Si2 C21 111.2(4) . . ? C26 Si2 C21 113.3(5) . . ? O6 Si2 C22 111.6(5) . . ? C26 Si2 C22 103.9(8) . . ? C21 Si2 C22 110.2(5) . . ? C54 O8 C48 119.1(5) . . ? O7 Si3 C45 110.7(5) . . ? O7 Si3 C44 111.9(3) . . ? C45 Si3 C44 108.4(7) . . ? O7 Si3 C46 101.7(4) . . ? C45 Si3 C46 113.8(8) . . ? C44 Si3 C46 110.3(5) . . ? C10 O6 Si2 126.3(4) . . ? O12 Si4 C66 107.9(4) . . ? O12 Si4 C62 110.1(4) . . ? C66 Si4 C62 107.0(5) . . ? O12 Si4 C61 113.3(5) . . ? C66 Si4 C61 105.1(7) . . ? C62 Si4 C61 113.0(6) . . ? C50 O12 Si4 127.8(4) . . ? O11 C51 C52 108.3(6) . . ? O11 C51 C50 110.9(5) . . ? C52 C51 C50 112.6(6) . . ? O3 C14 O2 120.6(6) . . ? O3 C14 C15 126.0(7) . . ? O2 C14 C15 113.3(6) . . ? O5 C11 C12 109.6(6) . . ? O5 C11 C10 108.2(5) . . ? C12 C11 C10 113.1(6) . . ? C47 O7 Si3 122.9(5) . . ? O2 C8 C7 106.1(5) . . ? O2 C8 C9 106.3(5) . . ? C7 C8 C9 114.3(6) . . ? O9 C54 O8 123.2(7) . . ? O9 C54 C55 124.1(7) . . ? O8 C54 C55 112.7(6) . . ? O12 C50 C49 108.2(5) . . ? O12 C50 C51 109.4(5) . . ? C49 C50 C51 114.6(5) . . ? O8 C48 C47 108.0(5) . . ? O8 C48 C49 106.8(5) . . ? C47 C48 C49 113.6(6) . . ? O10 C49 C48 108.6(5) . . ? O10 C49 C50 112.4(5) . . ? C48 C49 C50 116.3(5) . . ? O1 C7 C8 110.0(6) . . ? O4 C9 C8 107.7(5) . . ? O4 C9 C10 112.3(5) . . ? C8 C9 C10 116.7(5) . . ? O6 C10 C9 108.0(5) . . ? O6 C10 C11 107.4(5) . . ? C9 C10 C11 116.5(5) . . ? C7 O1 Si1 124.2(5) . . ? C74 N2 C52 112.4(8) . . ? C74 N2 C67 113.1(10) . . ? C52 N2 C67 111.6(7) . . ? C55 C56 C57 119.7(8) . . ? C16 C15 C20 118.7(7) . . ? C16 C15 C14 119.1(6) . . ? C20 C15 C14 122.1(6) . . ? C56 C55 C60 121.7(7) . . ? C56 C55 C54 118.2(7) . . ? C60 C55 C54 120.1(7) . . ? O7 C47 C48 109.5(6) . . ? C27 N1 C34 115.0(11) . . ? C27 N1 C12 113.9(7) . . ? C34 N1 C12 108.9(9) . . ? C1 C4 C3 108.3(10) . . ? C1 C4 C2 111.5(11) . . ? C3 C4 C2 106.3(13) . . ? C1 C4 Si1 110.7(7) . . ? C3 C4 Si1 113.8(7) . . ? C2 C4 Si1 106.2(8) . . ? C42 C44 C41 111.1(10) . . ? C42 C44 C43 105.1(11) . . ? C41 C44 C43 109.3(14) . . ? C42 C44 Si3 109.2(7) . . ? C41 C44 Si3 115.0(8) . . ? C43 C44 Si3 106.6(8) . . ? C17 C16 C15 122.3(8) . . ? C76 C75 C80 130.6(13) . . ? C76 C75 C74 112.3(14) . . ? C80 C75 C74 116.8(15) . . ? C76 C75 C77 30.7(9) . . ? C80 C75 C77 100.6(10) . . ? C74 C75 C77 142.6(12) . . ? C55 C60 C59 116.3(8) . . ? C19 C20 C15 119.0(8) . . ? N1 C12 C11 110.2(7) . . ? N1 C12 C13 113.8(7) . . ? C11 C12 C13 114.6(6) . . ? N2 C52 C51 112.8(6) . . ? N2 C52 C53 112.8(6) . . ? C51 C52 C53 114.7(6) . . ? C18 C19 C20 119.8(8) . . ? C16 C17 C18 119.0(9) . . ? C64 C66 C65 107.8(10) . . ? C64 C66 C63 112.7(10) . . ? C65 C66 C63 108.1(12) . . ? C64 C66 Si4 111.7(8) . . ? C65 C66 Si4 109.5(8) . . ? C63 C66 Si4 107.0(9) . . ? C58 C57 C56 120.0(9) . . ? C72 C73 C68 115.6(11) . . ? C72 C73 C67 129.6(14) . . ? C68 C73 C67 114.7(13) . . ? C70 C71 C72 124.6(15) . . ? C25 C26 C23 108.4(11) . . ? C25 C26 C24 117.2(14) . . ? C23 C26 C24 109.2(11) . . ? C25 C26 Si2 109.8(9) . . ? C23 C26 Si2 110.5(10) . . ? C24 C26 Si2 101.5(8) . . ? C57 C58 C59 120.8(9) . . ? C71 C72 C73 118.3(11) . . ? C69 C70 C71 121(2) . . ? C17 C18 C19 121.2(8) . . ? C78 C79 C80 111.0(11) . . ? C58 C59 C60 121.1(9) . . ? C79 C78 C77 119.6(14) . . ? C75 C80 C79 108.3(13) . . ? N2 C74 C75 116.6(11) . . ? C36 C35 C40 121.0(11) . . ? C36 C35 C34 101.7(15) . . ? C40 C35 C34 137.2(15) . . ? C29 C28 C33 126.8(16) . . ? C29 C28 C27 125.7(16) . . ? C33 C28 C27 107.4(17) . . ? C38 C39 C40 117.7(11) . . ? C35 C36 C37 122.0(11) . . ? C39 C40 C35 119.4(11) . . ? N1 C34 C35 121.9(11) . . ? N1 C27 C28 117.2(9) . . ? C32 C31 C30 114.9(15) . . ? C70 C69 C68 126(2) . . ? C69 C68 C73 114.3(14) . . ? C73 C67 N2 115.0(10) . . ? C39 C38 C37 125.6(13) . . ? C38 C37 C36 114.3(15) . . ? C77 C76 C75 115.5(17) . . ? C76 C77 C78 134(2) . . ? C76 C77 C75 33.8(11) . . ? C78 C77 C75 99.9(12) . . ? C29 C30 C31 101.0(12) . . ? C28 C29 C30 126.1(17) . . ? C32 C33 C28 109(3) . . ? C33 C32 C31 138(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 C26 Si2 O6 C10 -145.5(7) . . . . ? C21 Si2 O6 C10 -21.7(7) . . . . ? C22 Si2 O6 C10 101.8(7) . . . . ? C66 Si4 O12 C50 -142.6(6) . . . . ? C62 Si4 O12 C50 -26.1(7) . . . . ? C61 Si4 O12 C50 101.5(8) . . . . ? C8 O2 C14 O3 -6.1(10) . . . . ? C8 O2 C14 C15 177.2(6) . . . . ? C45 Si3 O7 C47 42.4(10) . . . . ? C44 Si3 O7 C47 -78.6(7) . . . . ? C46 Si3 O7 C47 163.6(7) . . . . ? C14 O2 C8 C7 90.1(7) . . . . ? C14 O2 C8 C9 -147.7(6) . . . . ? C48 O8 C54 O9 -3.6(9) . . . . ? C48 O8 C54 C55 178.2(6) . . . . ? Si4 O12 C50 C49 107.2(5) . . . . ? Si4 O12 C50 C51 -127.3(5) . . . . ? O11 C51 C50 O12 -176.2(5) . . . . ? C52 C51 C50 O12 62.3(7) . . . . ? O11 C51 C50 C49 -54.5(7) . . . . ? C52 C51 C50 C49 -176.0(6) . . . . ? C54 O8 C48 C47 88.0(7) . . . . ? C54 O8 C48 C49 -149.4(6) . . . . ? O8 C48 C49 O10 -53.1(7) . . . . ? C47 C48 C49 O10 65.9(7) . . . . ? O8 C48 C49 C50 74.8(7) . . . . ? C47 C48 C49 C50 -166.2(6) . . . . ? O12 C50 C49 O10 -165.4(5) . . . . ? C51 C50 C49 O10 72.2(7) . . . . ? O12 C50 C49 C48 68.6(7) . . . . ? C51 C50 C49 C48 -53.7(8) . . . . ? O2 C8 C7 O1 -167.9(5) . . . . ? C9 C8 C7 O1 75.2(7) . . . . ? O2 C8 C9 O4 -52.5(6) . . . . ? C7 C8 C9 O4 64.3(7) . . . . ? O2 C8 C9 C10 75.0(7) . . . . ? C7 C8 C9 C10 -168.3(6) . . . . ? Si2 O6 C10 C9 106.0(6) . . . . ? Si2 O6 C10 C11 -127.6(5) . . . . ? O4 C9 C10 O6 -166.4(5) . . . . ? C8 C9 C10 O6 68.5(7) . . . . ? O4 C9 C10 C11 72.7(7) . . . . ? C8 C9 C10 C11 -52.4(8) . . . . ? O5 C11 C10 O6 -176.3(5) . . . . ? C12 C11 C10 O6 62.1(7) . . . . ? O5 C11 C10 C9 -55.1(7) . . . . ? C12 C11 C10 C9 -176.7(6) . . . . ? C8 C7 O1 Si1 160.3(5) . . . . ? C5 Si1 O1 C7 162.8(7) . . . . ? C6 Si1 O1 C7 45.2(9) . . . . ? C4 Si1 O1 C7 -78.3(7) . . . . ? O3 C14 C15 C16 14.6(12) . . . . ? O2 C14 C15 C16 -168.8(7) . . . . ? O3 C14 C15 C20 -164.2(8) . . . . ? O2 C14 C15 C20 12.3(10) . . . . ? C57 C56 C55 C60 -1.3(12) . . . . ? C57 C56 C55 C54 -178.8(7) . . . . ? O9 C54 C55 C56 14.7(11) . . . . ? O8 C54 C55 C56 -167.2(6) . . . . ? O9 C54 C55 C60 -162.9(7) . . . . ? O8 C54 C55 C60 15.3(9) . . . . ? Si3 O7 C47 C48 160.3(5) . . . . ? O8 C48 C47 O7 -166.9(6) . . . . ? C49 C48 C47 O7 74.8(8) . . . . ? O1 Si1 C4 C1 -173.5(7) . . . . ? C5 Si1 C4 C1 -59.2(9) . . . . ? C6 Si1 C4 C1 63.5(9) . . . . ? O1 Si1 C4 C3 64.2(11) . . . . ? C5 Si1 C4 C3 178.6(11) . . . . ? C6 Si1 C4 C3 -58.8(11) . . . . ? O1 Si1 C4 C2 -52.4(11) . . . . ? C5 Si1 C4 C2 62.0(12) . . . . ? C6 Si1 C4 C2 -175.4(12) . . . . ? O7 Si3 C44 C42 -173.6(8) . . . . ? C45 Si3 C44 C42 64.0(10) . . . . ? C46 Si3 C44 C42 -61.2(9) . . . . ? O7 Si3 C44 C41 60.8(12) . . . . ? C45 Si3 C44 C41 -61.6(12) . . . . ? C46 Si3 C44 C41 173.2(11) . . . . ? O7 Si3 C44 C43 -60.5(10) . . . . ? C45 Si3 C44 C43 177.1(10) . . . . ? C46 Si3 C44 C43 51.9(10) . . . . ? C20 C15 C16 C17 -0.6(12) . . . . ? C14 C15 C16 C17 -179.4(8) . . . . ? C56 C55 C60 C59 3.2(12) . . . . ? C54 C55 C60 C59 -179.3(8) . . . . ? C16 C15 C20 C19 0.8(11) . . . . ? C14 C15 C20 C19 179.6(8) . . . . ? C27 N1 C12 C11 -74.4(14) . . . . ? C34 N1 C12 C11 155.8(8) . . . . ? C27 N1 C12 C13 56.0(15) . . . . ? C34 N1 C12 C13 -73.8(10) . . . . ? O5 C11 C12 N1 79.0(7) . . . . ? C10 C11 C12 N1 -160.1(6) . . . . ? O5 C11 C12 C13 -51.0(9) . . . . ? C10 C11 C12 C13 69.9(9) . . . . ? C74 N2 C52 C51 -74.6(14) . . . . ? C67 N2 C52 C51 157.1(7) . . . . ? C74 N2 C52 C53 57.4(14) . . . . ? C67 N2 C52 C53 -70.9(10) . . . . ? O11 C51 C52 N2 78.3(7) . . . . ? C50 C51 C52 N2 -158.7(6) . . . . ? O11 C51 C52 C53 -52.7(9) . . . . ? C50 C51 C52 C53 70.2(9) . . . . ? C15 C20 C19 C18 -0.6(14) . . . . ? C15 C16 C17 C18 0.2(14) . . . . ? O12 Si4 C66 C64 -171.4(8) . . . . ? C62 Si4 C66 C64 70.1(9) . . . . ? C61 Si4 C66 C64 -50.3(10) . . . . ? O12 Si4 C66 C65 -52.1(10) . . . . ? C62 Si4 C66 C65 -170.6(9) . . . . ? C61 Si4 C66 C65 69.1(10) . . . . ? O12 Si4 C66 C63 64.8(9) . . . . ? C62 Si4 C66 C63 -53.7(9) . . . . ? C61 Si4 C66 C63 -174.1(9) . . . . ? C55 C56 C57 C58 -4.5(14) . . . . ? O6 Si2 C26 C25 -54.4(13) . . . . ? C21 Si2 C26 C25 -176.8(10) . . . . ? C22 Si2 C26 C25 63.5(12) . . . . ? O6 Si2 C26 C23 -174.0(9) . . . . ? C21 Si2 C26 C23 63.6(12) . . . . ? C22 Si2 C26 C23 -56.0(11) . . . . ? O6 Si2 C26 C24 70.3(8) . . . . ? C21 Si2 C26 C24 -52.1(9) . . . . ? C22 Si2 C26 C24 -171.8(8) . . . . ? C56 C57 C58 C59 8.2(16) . . . . ? C70 C71 C72 C73 -2(2) . . . . ? C68 C73 C72 C71 1.7(15) . . . . ? C67 C73 C72 C71 -179.3(11) . . . . ? C72 C71 C70 C69 -1(3) . . . . ? C16 C17 C18 C19 0.0(16) . . . . ? C20 C19 C18 C17 0.2(16) . . . . ? C57 C58 C59 C60 -6.2(17) . . . . ? C55 C60 C59 C58 0.4(14) . . . . ? C80 C79 C78 C77 0(2) . . . . ? C76 C75 C80 C79 -15(2) . . . . ? C74 C75 C80 C79 171.7(10) . . . . ? C77 C75 C80 C79 -7.2(14) . . . . ? C78 C79 C80 C75 6(2) . . . . ? C52 N2 C74 C75 171.8(14) . . . . ? C67 N2 C74 C75 -61(2) . . . . ? C76 C75 C74 N2 -78(2) . . . . ? C80 C75 C74 N2 97(2) . . . . ? C77 C75 C74 N2 -85(2) . . . . ? C40 C35 C36 C37 -0.4(18) . . . . ? C34 C35 C36 C37 176.5(12) . . . . ? C38 C39 C40 C35 -1.8(14) . . . . ? C36 C35 C40 C39 0.5(15) . . . . ? C34 C35 C40 C39 -175.2(11) . . . . ? C27 N1 C34 C35 165.5(14) . . . . ? C12 N1 C34 C35 -65.3(15) . . . . ? C36 C35 C34 N1 -33.4(16) . . . . ? C40 C35 C34 N1 142.8(14) . . . . ? C34 N1 C27 C28 -55(2) . . . . ? C12 N1 C27 C28 178.0(14) . . . . ? C29 C28 C27 N1 99(2) . . . . ? C33 C28 C27 N1 -77(2) . . . . ? C71 C70 C69 C68 4(3) . . . . ? C70 C69 C68 C73 -4(3) . . . . ? C72 C73 C68 C69 0.9(16) . . . . ? C67 C73 C68 C69 -178.3(11) . . . . ? C72 C73 C67 N2 146.3(10) . . . . ? C68 C73 C67 N2 -34.8(13) . . . . ? C74 N2 C67 C73 165.9(13) . . . . ? C52 N2 C67 C73 -66.2(11) . . . . ? C40 C39 C38 C37 3.2(18) . . . . ? C39 C38 C37 C36 -3(2) . . . . ? C35 C36 C37 C38 2(2) . . . . ? C80 C75 C76 C77 14(3) . . . . ? C74 C75 C76 C77 -171.7(14) . . . . ? C75 C76 C77 C78 -5(3) . . . . ? C79 C78 C77 C76 -1(3) . . . . ? C79 C78 C77 C75 -4.0(17) . . . . ? C80 C75 C77 C76 -169(2) . . . . ? C74 C75 C77 C76 13(2) . . . . ? C76 C75 C77 C78 177(2) . . . . ? C80 C75 C77 C78 7.6(14) . . . . ? C74 C75 C77 C78 -170.8(13) . . . . ? C32 C31 C30 C29 15.4(18) . . . . ? C33 C28 C29 C30 -3(3) . . . . ? C27 C28 C29 C30 -177.3(15) . . . . ? C31 C30 C29 C28 -14(2) . . . . ? C29 C28 C33 C32 18(3) . . . . ? C27 C28 C33 C32 -166.1(14) . . . . ? C28 C33 C32 C31 -16(4) . . . . ? C30 C31 C32 C33 -1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.743 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.087