data_UP1327 _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H45 N O5 S Si' _chemical_formula_weight 547.81 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' 'S' 'S' 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.9222(4) _cell_length_b 9.8530(4) _cell_length_c 20.0514(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.404(2) _cell_angle_gamma 90.00 _cell_volume 1563.78(13) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Sheldrick, 2007)' _exptl_absorpt_correction_T_min 0.6977 _exptl_absorpt_correction_T_max 0.7452 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 26518 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.07 _reflns_number_total 5405 _reflns_number_gt 5055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0675P)^2^+0.6644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _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 0.02(8) _refine_ls_number_reflns 5405 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.005 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6869(3) 0.5587(3) 0.31046(12) 0.0315(5) Uani 1 1 d . . . C2 C 0.5299(3) 0.5016(3) 0.27326(12) 0.0325(5) Uani 1 1 d . . . H2a H 0.5042 0.4127 0.2910 0.043 Uiso 1 1 calc R . . H2b H 0.4342 0.5605 0.2804 0.043 Uiso 1 1 calc R . . C3 C 0.5569(3) 0.4901(3) 0.19894(12) 0.0360(5) Uani 1 1 d . . . H3 H 0.6405 0.4194 0.1907 0.048 Uiso 1 1 calc R . . C4 C 0.6172(3) 0.6261(3) 0.17233(12) 0.0409(6) Uani 1 1 d . . . H4a H 0.6448 0.6160 0.1259 0.054 Uiso 1 1 calc R . . H4b H 0.5269 0.6923 0.1745 0.054 Uiso 1 1 calc R . . C5 C 0.7712(4) 0.6773(3) 0.21214(13) 0.0418(6) Uani 1 1 d . . . H5 H 0.8666 0.6161 0.2057 0.056 Uiso 1 1 calc R . . C6 C 0.6587(3) 0.5935(3) 0.38480(11) 0.0314(5) Uani 1 1 d . . . H6 H 0.7663 0.6255 0.4050 0.042 Uiso 1 1 calc R . . C7 C 0.5264(3) 0.7026(3) 0.39484(13) 0.0358(6) Uani 1 1 d . . . H7a H 0.5102 0.7568 0.3547 0.048 Uiso 1 1 calc R . . H7b H 0.5620 0.7621 0.4314 0.048 Uiso 1 1 calc R . . C8 C 0.4421(3) 0.4643(3) 0.43650(12) 0.0325(5) Uani 1 1 d . . . C9 C 0.7289(3) 0.3800(3) 0.45318(12) 0.0325(5) Uani 1 1 d . . . H9a H 0.8036 0.3464 0.4198 0.043 Uiso 1 1 calc R . . H9b H 0.6693 0.3029 0.4709 0.043 Uiso 1 1 calc R . . C10 C 0.8331(3) 0.4465(3) 0.50883(12) 0.0320(5) Uani 1 1 d . . . C11 C 0.7676(3) 0.5479(3) 0.54818(13) 0.0365(6) Uani 1 1 d . . . H11 H 0.6562 0.5754 0.5403 0.049 Uiso 1 1 calc R . . C12 C 0.8636(3) 0.6091(3) 0.59870(12) 0.0409(6) Uani 1 1 d . . . H12 H 0.8173 0.6770 0.6245 0.054 Uiso 1 1 calc R . . C13 C 1.0306(4) 0.5684(3) 0.61088(13) 0.0405(6) Uani 1 1 d . . . C14 C 1.0981(3) 0.4688(3) 0.57227(14) 0.0435(6) Uani 1 1 d . . . H14 H 1.2094 0.4413 0.5802 0.058 Uiso 1 1 calc R . . C15 C 0.9997(3) 0.4091(3) 0.52132(14) 0.0420(6) Uani 1 1 d . . . H15 H 1.0469 0.3424 0.4950 0.056 Uiso 1 1 calc R . . C16 C 1.2910(4) 0.6057(5) 0.67301(19) 0.0701(10) Uani 1 1 d . . . H16a H 1.3025 0.5117 0.6849 0.105 Uiso 1 1 calc R . . H16b H 1.3368 0.6611 0.7088 0.105 Uiso 1 1 calc R . . H16c H 1.3511 0.6231 0.6333 0.105 Uiso 1 1 calc R . . C17 C 0.9785(3) 0.4936(4) 0.32871(14) 0.0489(7) Uani 1 1 d . . . H17a H 1.0023 0.5855 0.3163 0.073 Uiso 1 1 calc R . . H17b H 1.0590 0.4339 0.3095 0.073 Uiso 1 1 calc R . . H17c H 0.9860 0.4854 0.3764 0.073 Uiso 1 1 calc R . . C18 C 0.4860(6) 0.1885(6) 0.1243(4) 0.133(3) Uani 1 1 d . . . H18a H 0.6041 0.2065 0.1197 0.199 Uiso 1 1 calc R . . H18b H 0.4498 0.1196 0.0931 0.199 Uiso 1 1 calc R . . H18c H 0.4677 0.1580 0.1689 0.199 Uiso 1 1 calc R . . C19 C 0.4358(8) 0.4235(10) 0.0279(2) 0.156(3) Uani 1 1 d . . . H19a H 0.3771 0.5076 0.0200 0.234 Uiso 1 1 calc R . . H19b H 0.4118 0.3626 -0.0086 0.234 Uiso 1 1 calc R . . H19c H 0.5552 0.4404 0.0318 0.234 Uiso 1 1 calc R . . C20 C 0.1316(4) 0.3187(3) 0.10072(17) 0.0551(8) Uani 1 1 d . . . C21 C 0.0397(5) 0.4497(4) 0.0842(2) 0.0777(11) Uani 1 1 d . . . H21a H 0.0748 0.4833 0.0420 0.117 Uiso 1 1 calc R . . H21b H 0.0659 0.5156 0.1183 0.117 Uiso 1 1 calc R . . H21c H -0.0798 0.4334 0.0817 0.117 Uiso 1 1 calc R . . C22 C 0.0881(6) 0.2134(4) 0.0460(3) 0.0930(16) Uani 1 1 d . . . H22a H -0.0323 0.2041 0.0408 0.140 Uiso 1 1 calc R . . H22b H 0.1372 0.1275 0.0584 0.140 Uiso 1 1 calc R . . H22c H 0.1325 0.2430 0.0046 0.140 Uiso 1 1 calc R . . C23 C 0.0746(6) 0.2688(6) 0.1686(3) 0.0969(16) Uani 1 1 d . . . H23a H 0.1106 0.3323 0.2027 0.145 Uiso 1 1 calc R . . H23b H 0.1239 0.1817 0.1782 0.145 Uiso 1 1 calc R . . H23c H -0.0463 0.2614 0.1674 0.145 Uiso 1 1 calc R . . C24 C 0.8193(4) 0.8216(4) 0.19183(15) 0.0541(8) Uani 1 1 d . . . H24a H 0.8449 0.8210 0.1449 0.072 Uiso 1 1 calc R . . H24b H 0.7220 0.8800 0.1967 0.072 Uiso 1 1 calc R . . C25 C 0.9666(4) 0.8823(3) 0.23067(17) 0.0567(8) Uani 1 1 d . . . H25a H 0.9464 0.8737 0.2779 0.075 Uiso 1 1 calc R . . H25b H 0.9711 0.9785 0.2205 0.075 Uiso 1 1 calc R . . C26 C 1.1380(4) 0.8203(4) 0.21775(15) 0.0545(8) Uani 1 1 d . . . H26 H 1.1359 0.7239 0.2297 0.072 Uiso 1 1 calc R . . C27 C 1.1823(4) 0.8330(4) 0.14723(16) 0.0579(8) Uani 1 1 d . . . C28 C 1.2173(5) 0.8403(5) 0.09099(18) 0.0688(10) Uani 1 1 d . . . H28 H 1.2449 0.8461 0.0465 0.091 Uiso 1 1 calc R . . C29 C 1.2800(5) 0.8929(4) 0.26179(17) 0.0674(10) Uani 1 1 d . . . H29a H 1.3860 0.8482 0.2561 0.101 Uiso 1 1 calc R . . H29b H 1.2521 0.8888 0.3079 0.101 Uiso 1 1 calc R . . H29c H 1.2885 0.9861 0.2483 0.101 Uiso 1 1 calc R . . N1 N 0.6068(2) 0.4732(2) 0.42160(10) 0.0304(4) Uani 1 1 d . . . O1 O 0.7363(2) 0.68346(19) 0.28261(8) 0.0362(4) Uani 1 1 d . . . O2 O 0.3745(2) 0.3684(2) 0.46237(10) 0.0438(5) Uani 1 1 d . . . O3 O 1.1170(3) 0.6373(2) 0.66120(11) 0.0562(6) Uani 1 1 d . . . O4 O 0.8117(2) 0.4579(2) 0.30462(9) 0.0393(4) Uani 1 1 d . . . O5 O 0.3974(2) 0.4546(2) 0.16727(9) 0.0442(5) Uani 1 1 d . . . S1 S 0.33204(7) 0.61662(7) 0.41375(3) 0.03750(16) Uani 1 1 d . . . Si1 Si 0.36412(11) 0.34500(10) 0.10758(5) 0.0584(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0279(12) 0.0357(13) 0.0307(12) -0.0005(10) -0.0031(10) -0.0015(10) C2 0.0296(12) 0.0336(14) 0.0340(12) -0.0026(10) -0.0032(10) -0.0062(10) C3 0.0322(12) 0.0404(14) 0.0350(12) -0.0068(11) -0.0049(10) -0.0018(11) C4 0.0434(14) 0.0510(16) 0.0280(12) 0.0005(12) -0.0028(10) -0.0025(14) C5 0.0416(15) 0.0536(16) 0.0303(13) 0.0000(12) 0.0038(11) -0.0106(13) C6 0.0261(11) 0.0364(15) 0.0311(11) 0.0002(10) -0.0041(8) -0.0078(10) C7 0.0394(14) 0.0325(14) 0.0353(13) -0.0002(10) -0.0017(10) -0.0045(11) C8 0.0294(12) 0.0370(14) 0.0310(12) -0.0019(10) -0.0013(9) -0.0040(11) C9 0.0330(12) 0.0315(13) 0.0332(12) 0.0034(10) 0.0021(10) 0.0019(10) C10 0.0302(12) 0.0334(13) 0.0323(12) 0.0072(10) 0.0012(9) 0.0011(10) C11 0.0300(13) 0.0415(15) 0.0378(13) 0.0023(11) -0.0013(10) 0.0054(11) C12 0.0481(15) 0.0387(15) 0.0354(13) -0.0014(12) -0.0025(11) 0.0048(13) C13 0.0454(15) 0.0405(15) 0.0347(13) 0.0066(11) -0.0087(11) -0.0063(11) C14 0.0304(13) 0.0519(18) 0.0474(15) 0.0051(13) -0.0091(11) 0.0045(12) C15 0.0371(14) 0.0437(16) 0.0451(15) 0.0009(12) 0.0017(11) 0.0090(12) C16 0.063(2) 0.072(2) 0.071(2) 0.010(2) -0.0357(17) -0.012(2) C17 0.0294(13) 0.075(2) 0.0421(15) 0.0022(14) -0.0003(11) 0.0029(14) C18 0.079(3) 0.089(4) 0.225(7) -0.087(4) -0.066(4) 0.037(3) C19 0.162(6) 0.256(9) 0.053(3) -0.041(4) 0.039(3) -0.094(6) C20 0.0540(17) 0.0479(18) 0.0615(19) -0.0112(15) -0.0199(15) 0.0003(15) C21 0.068(2) 0.056(2) 0.106(3) -0.002(2) -0.027(2) 0.0090(19) C22 0.082(3) 0.069(3) 0.123(4) -0.042(3) -0.053(3) 0.001(2) C23 0.077(3) 0.115(4) 0.099(3) 0.023(3) 0.010(2) -0.032(3) C24 0.0574(18) 0.062(2) 0.0437(16) 0.0097(15) 0.0062(13) -0.0108(16) C25 0.070(2) 0.0450(18) 0.0562(18) 0.0028(14) 0.0106(15) -0.0072(15) C26 0.0636(19) 0.0537(19) 0.0457(16) 0.0038(14) -0.0023(14) 0.0061(16) C27 0.0525(17) 0.068(2) 0.0526(19) -0.0064(16) -0.0026(14) 0.0046(16) C28 0.070(2) 0.086(3) 0.050(2) 0.0036(19) 0.0045(16) -0.005(2) C29 0.063(2) 0.084(3) 0.0532(19) -0.0055(18) -0.0113(16) 0.0132(19) N1 0.0272(9) 0.0339(11) 0.0301(10) 0.0039(8) -0.0003(8) -0.0040(8) O1 0.0372(9) 0.0418(10) 0.0297(9) -0.0003(8) 0.0017(7) -0.0128(8) O2 0.0370(10) 0.0429(12) 0.0519(11) 0.0064(9) 0.0047(8) -0.0103(8) O3 0.0598(13) 0.0542(14) 0.0525(12) -0.0010(10) -0.0221(10) -0.0100(11) O4 0.0290(9) 0.0507(12) 0.0381(9) -0.0030(8) -0.0006(7) 0.0033(8) O5 0.0380(10) 0.0517(12) 0.0420(10) -0.0131(9) -0.0092(8) -0.0014(9) S1 0.0290(3) 0.0408(3) 0.0425(3) -0.0030(3) -0.0007(2) 0.0005(3) Si1 0.0450(5) 0.0675(6) 0.0622(5) -0.0332(5) -0.0043(4) -0.0038(4) 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 O4 1.410(3) . ? C1 O1 1.412(3) . ? C1 C2 1.531(3) . ? C1 C6 1.555(3) . ? C2 C3 1.519(3) . ? C3 O5 1.433(3) . ? C3 C4 1.527(4) . ? C4 C5 1.516(4) . ? C5 O1 1.452(3) . ? C5 C24 1.532(5) . ? C6 N1 1.464(3) . ? C6 C7 1.521(4) . ? C7 S1 1.812(3) . ? C8 O2 1.213(3) . ? C8 N1 1.354(3) . ? C8 S1 1.785(3) . ? C9 N1 1.459(3) . ? C9 C10 1.509(3) . ? C10 C15 1.383(3) . ? C10 C11 1.387(4) . ? C11 C12 1.380(4) . ? C12 C13 1.394(4) . ? C13 C14 1.373(4) . ? C13 O3 1.374(3) . ? C14 C15 1.389(4) . ? C16 O3 1.424(4) . ? C17 O4 1.431(3) . ? C18 Si1 1.843(5) . ? C19 Si1 1.884(6) . ? C20 C21 1.511(5) . ? C20 C23 1.533(6) . ? C20 C22 1.538(5) . ? C20 Si1 1.860(3) . ? C24 C25 1.500(5) . ? C25 C26 1.521(5) . ? C26 C27 1.476(4) . ? C26 C29 1.573(5) . ? C27 C28 1.175(5) . ? O5 Si1 1.6252(19) . ? 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 O4 C1 O1 111.90(19) . . ? O4 C1 C2 105.0(2) . . ? O1 C1 C2 111.1(2) . . ? O4 C1 C6 111.37(19) . . ? O1 C1 C6 103.92(19) . . ? C2 C1 C6 113.70(19) . . ? C3 C2 C1 111.15(19) . . ? O5 C3 C2 107.18(19) . . ? O5 C3 C4 110.0(2) . . ? C2 C3 C4 109.7(2) . . ? C5 C4 C3 111.4(2) . . ? O1 C5 C4 110.2(2) . . ? O1 C5 C24 106.2(2) . . ? C4 C5 C24 111.9(3) . . ? N1 C6 C7 107.20(19) . . ? N1 C6 C1 111.07(19) . . ? C7 C6 C1 114.22(19) . . ? C6 C7 S1 107.07(17) . . ? O2 C8 N1 126.3(2) . . ? O2 C8 S1 123.00(19) . . ? N1 C8 S1 110.74(18) . . ? N1 C9 C10 112.3(2) . . ? C15 C10 C11 117.8(2) . . ? C15 C10 C9 120.4(2) . . ? C11 C10 C9 121.8(2) . . ? C12 C11 C10 121.6(2) . . ? C11 C12 C13 119.6(3) . . ? C14 C13 O3 125.0(3) . . ? C14 C13 C12 119.7(2) . . ? O3 C13 C12 115.2(3) . . ? C13 C14 C15 119.9(2) . . ? C10 C15 C14 121.5(3) . . ? C21 C20 C23 108.2(4) . . ? C21 C20 C22 109.1(3) . . ? C23 C20 C22 110.6(4) . . ? C21 C20 Si1 111.3(3) . . ? C23 C20 Si1 107.8(2) . . ? C22 C20 Si1 109.7(3) . . ? C25 C24 C5 115.4(3) . . ? C24 C25 C26 115.6(3) . . ? C27 C26 C25 112.3(3) . . ? C27 C26 C29 107.8(3) . . ? C25 C26 C29 110.1(3) . . ? C28 C27 C26 178.7(4) . . ? C8 N1 C9 119.4(2) . . ? C8 N1 C6 117.2(2) . . ? C9 N1 C6 122.21(18) . . ? C1 O1 C5 114.6(2) . . ? C13 O3 C16 117.6(3) . . ? C1 O4 C17 116.1(2) . . ? C3 O5 Si1 126.97(17) . . ? C8 S1 C7 92.09(12) . . ? O5 Si1 C18 110.72(19) . . ? O5 Si1 C20 106.06(13) . . ? C18 Si1 C20 114.0(2) . . ? O5 Si1 C19 107.8(2) . . ? C18 Si1 C19 108.9(4) . . ? C20 Si1 C19 109.1(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.653 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.043