data_pt4s10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H45 N O9 Si' _chemical_formula_weight 567.74 _chemical_absolute_configuration ad 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6627(7) _cell_length_b 13.4490(9) _cell_length_c 12.0884(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.9610(10) _cell_angle_gamma 90.00 _cell_volume 1570.71(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 32.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9407 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26117 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 31.00 _reflns_number_total 9939 _reflns_number_gt 8837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0738P)^2^+0.1270P] 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 0.02(9) _refine_ls_number_reflns 9939 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.38545(5) 1.14024(3) 0.54296(3) 0.02714(9) Uani 1 1 d . . . N N 0.57368(13) 0.66988(10) 0.97979(11) 0.0265(3) Uani 1 1 d . . . O1 O 0.52391(11) 0.62817(8) 0.88040(8) 0.0260(2) Uani 1 1 d . . . O2 O 0.79955(14) 0.90512(11) 0.78323(14) 0.0456(3) Uani 1 1 d . . . O3 O 0.81982(12) 1.04645(10) 0.87966(11) 0.0354(3) Uani 1 1 d . . . O4 O 0.41054(12) 1.02648(8) 0.59281(8) 0.0259(2) Uani 1 1 d . . . O5 O 0.14485(11) 0.94579(9) 0.64264(9) 0.0294(2) Uani 1 1 d . . . O6 O 0.47674(10) 0.90363(8) 0.85699(8) 0.02155(19) Uani 1 1 d . . . O7 O 0.29573(11) 0.84650(8) 1.02659(8) 0.0236(2) Uani 1 1 d . . . O8 O 0.1448(2) 0.83572(17) 0.50314(17) 0.0764(6) Uani 1 1 d . . . O9 O 0.56348(12) 0.80576(9) 1.08757(9) 0.0279(2) Uani 1 1 d . . . C1 C 0.96090(19) 1.01912(19) 0.90817(19) 0.0460(5) Uani 1 1 d . . . H1A H 0.9951 1.0617 0.9684 0.069 Uiso 1 1 calc R . . H1B H 1.0194 1.0277 0.8434 0.069 Uiso 1 1 calc R . . H1C H 0.9637 0.9495 0.9320 0.069 Uiso 1 1 calc R . . C2 C -0.0485(2) 0.94584(19) 0.52293(19) 0.0507(5) Uani 1 1 d . . . H2A H -0.0708 0.9335 0.4447 0.076 Uiso 1 1 calc R . . H2B H -0.0460 1.0176 0.5366 0.076 Uiso 1 1 calc R . . H2C H -0.1193 0.9153 0.5690 0.076 Uiso 1 1 calc R . . C3 C 0.1144(3) 1.1916(2) 0.6256(2) 0.0578(6) Uani 1 1 d . . . H3A H 0.0183 1.2070 0.6048 0.087 Uiso 1 1 calc R . . H3B H 0.1555 1.2484 0.6648 0.087 Uiso 1 1 calc R . . H3C H 0.1166 1.1330 0.6739 0.087 Uiso 1 1 calc R . . C4 C 0.6250(3) 1.1171(2) 0.4174(3) 0.0687(8) Uani 1 1 d . . . H4A H 0.6638 1.1149 0.3430 0.103 Uiso 1 1 calc R . . H4B H 0.6408 1.0531 0.4544 0.103 Uiso 1 1 calc R . . H4C H 0.6700 1.1702 0.4602 0.103 Uiso 1 1 calc R . . C5 C -0.0949(2) 0.99329(17) 1.21043(18) 0.0448(5) Uani 1 1 d . . . H5A H -0.1717 1.0347 1.2260 0.054 Uiso 1 1 calc R . . C6 C -0.11651(19) 0.90034(17) 1.16537(18) 0.0432(4) Uani 1 1 d . . . H6A H -0.2079 0.8775 1.1500 0.052 Uiso 1 1 calc R . . C7 C 0.1967(2) 1.17016(16) 0.52169(19) 0.0457(5) Uani 1 1 d . . . H7A H 0.1894 1.2288 0.4724 0.055 Uiso 1 1 calc R . . H7B H 0.1524 1.1136 0.4824 0.055 Uiso 1 1 calc R . . C8 C 0.4723(3) 1.13700(18) 0.40880(15) 0.0501(5) Uani 1 1 d . . . H8A H 0.4286 1.0848 0.3622 0.060 Uiso 1 1 calc R . . H8B H 0.4575 1.2016 0.3710 0.060 Uiso 1 1 calc R . . C9 C 0.0375(2) 1.02646(16) 1.23302(17) 0.0445(4) Uani 1 1 d . . . H9A H 0.0520 1.0906 1.2641 0.053 Uiso 1 1 calc R . . C10 C 0.0897(2) 0.90169(16) 0.55106(16) 0.0417(4) Uani 1 1 d . . . C11 C 0.14994(18) 0.96559(14) 1.21013(15) 0.0357(4) Uani 1 1 d . . . H11A H 0.2411 0.9884 1.2262 0.043 Uiso 1 1 calc R . . C12 C 0.4638(2) 1.23386(13) 0.63833(15) 0.0365(4) Uani 1 1 d . . . H12A H 0.4240 1.2249 0.7126 0.044 Uiso 1 1 calc R . . H12B H 0.5645 1.2209 0.6449 0.044 Uiso 1 1 calc R . . C13 C 0.4422(3) 1.34205(15) 0.60239(19) 0.0475(5) Uani 1 1 d . . . H13A H 0.4825 1.3866 0.6584 0.071 Uiso 1 1 calc R . . H13B H 0.3429 1.3556 0.5942 0.071 Uiso 1 1 calc R . . H13C H 0.4874 1.3532 0.5315 0.071 Uiso 1 1 calc R . . C14 C 0.71929(18) 0.64927(17) 1.00223(17) 0.0423(4) Uani 1 1 d . . . H14A H 0.7452 0.6748 1.0757 0.063 Uiso 1 1 calc R . . H14B H 0.7757 0.6818 0.9462 0.063 Uiso 1 1 calc R . . H14C H 0.7351 0.5773 1.0000 0.063 Uiso 1 1 calc R . . C15 C -0.00360(18) 0.84028(14) 1.14255(16) 0.0358(4) Uani 1 1 d . . . H15A H -0.0185 0.7762 1.1115 0.043 Uiso 1 1 calc R . . C16 C 0.25133(16) 0.81008(13) 1.13181(13) 0.0296(3) Uani 1 1 d . . . H16A H 0.3271 0.8159 1.1876 0.036 Uiso 1 1 calc R . . H16B H 0.2239 0.7393 1.1259 0.036 Uiso 1 1 calc R . . C17 C 0.47031(18) 0.53028(12) 0.90124(14) 0.0314(3) Uani 1 1 d . . . H17A H 0.4417 0.4994 0.8311 0.047 Uiso 1 1 calc R . . H17B H 0.3904 0.5352 0.9499 0.047 Uiso 1 1 calc R . . H17C H 0.5423 0.4896 0.9370 0.047 Uiso 1 1 calc R . . C18 C 0.13506(17) 0.77661(13) 0.79030(15) 0.0312(3) Uani 1 1 d . . . H18A H 0.0507 0.8032 0.7552 0.047 Uiso 1 1 calc R . . H18B H 0.1137 0.7520 0.8644 0.047 Uiso 1 1 calc R . . H18C H 0.1709 0.7219 0.7455 0.047 Uiso 1 1 calc R . . C19 C 0.75279(15) 0.98302(12) 0.81241(14) 0.0279(3) Uani 1 1 d . . . C20 C 0.13059(16) 0.87226(12) 1.16432(12) 0.0267(3) Uani 1 1 d . . . C21 C 0.50839(14) 0.94660(11) 0.75280(11) 0.0216(2) Uani 1 1 d . . . H21A H 0.5485 0.8946 0.7037 0.026 Uiso 1 1 calc R . . C22 C 0.36944(14) 0.77736(10) 0.96234(11) 0.0201(2) Uani 1 1 d . . . H22A H 0.3152 0.7142 0.9569 0.024 Uiso 1 1 calc R . . C23 C 0.38204(14) 0.82234(10) 0.84717(11) 0.0206(2) Uani 1 1 d . . . H23A H 0.4214 0.7714 0.7963 0.025 Uiso 1 1 calc R . . C24 C 0.51188(15) 0.75506(10) 1.01412(12) 0.0215(2) Uani 1 1 d . . . C25 C 0.61560(15) 1.02572(11) 0.77588(13) 0.0260(3) Uani 1 1 d . . . H25A H 0.6286 1.0657 0.7081 0.031 Uiso 1 1 calc R . . H25B H 0.5814 1.0707 0.8342 0.031 Uiso 1 1 calc R . . C26 C 0.24356(14) 0.85857(10) 0.79943(12) 0.0220(2) Uani 1 1 d . . . H26A H 0.2074 0.9115 0.8493 0.026 Uiso 1 1 calc R . . C27 C 0.27182(15) 0.90549(11) 0.68709(12) 0.0233(3) Uani 1 1 d . . . H27A H 0.3077 0.8536 0.6357 0.028 Uiso 1 1 calc R . . C28 C 0.37712(14) 0.98924(10) 0.69820(11) 0.0212(2) Uani 1 1 d . . . H28A H 0.3391 1.0438 0.7449 0.025 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 Si 0.0404(2) 0.02067(18) 0.02030(17) 0.00270(15) -0.00176(15) -0.00075(16) N 0.0240(6) 0.0237(6) 0.0316(6) -0.0030(5) -0.0044(5) 0.0060(5) O1 0.0332(5) 0.0201(5) 0.0246(5) -0.0007(4) -0.0003(4) 0.0028(4) O2 0.0321(6) 0.0384(7) 0.0663(9) -0.0083(7) -0.0025(6) 0.0094(6) O3 0.0227(5) 0.0380(7) 0.0452(7) -0.0007(5) -0.0058(5) -0.0004(5) O4 0.0349(6) 0.0213(5) 0.0215(5) 0.0027(4) 0.0014(4) 0.0004(4) O5 0.0276(5) 0.0290(6) 0.0314(5) 0.0044(5) -0.0098(4) -0.0001(4) O6 0.0228(4) 0.0194(4) 0.0225(5) 0.0036(4) -0.0005(3) -0.0021(4) O7 0.0260(5) 0.0201(5) 0.0249(5) 0.0029(4) 0.0054(4) 0.0045(4) O8 0.0834(13) 0.0780(14) 0.0663(11) -0.0357(10) -0.0411(10) 0.0183(11) O9 0.0283(5) 0.0261(5) 0.0292(5) -0.0029(4) -0.0035(4) 0.0005(4) C1 0.0253(8) 0.0575(13) 0.0549(12) 0.0055(10) -0.0092(7) 0.0013(8) C2 0.0405(10) 0.0580(13) 0.0527(12) 0.0152(10) -0.0234(9) -0.0095(9) C3 0.0486(12) 0.0465(12) 0.0787(16) 0.0080(12) 0.0113(11) 0.0159(10) C4 0.0802(17) 0.0454(13) 0.0820(18) -0.0083(12) 0.0482(15) -0.0098(12) C5 0.0380(9) 0.0479(11) 0.0490(11) -0.0014(9) 0.0103(8) 0.0155(8) C6 0.0281(8) 0.0462(11) 0.0556(12) 0.0019(9) 0.0054(7) 0.0013(7) C7 0.0491(11) 0.0337(9) 0.0539(11) 0.0099(8) -0.0110(9) 0.0043(8) C8 0.0843(15) 0.0357(9) 0.0310(8) 0.0037(8) 0.0182(9) -0.0035(10) C9 0.0514(11) 0.0370(9) 0.0450(10) -0.0129(8) 0.0021(8) 0.0099(8) C10 0.0424(9) 0.0432(10) 0.0388(9) 0.0043(8) -0.0183(8) -0.0079(8) C11 0.0313(8) 0.0387(9) 0.0371(8) -0.0064(7) -0.0003(6) 0.0013(7) C12 0.0549(11) 0.0222(7) 0.0321(8) -0.0008(6) -0.0060(7) 0.0001(7) C13 0.0698(14) 0.0229(8) 0.0495(11) 0.0014(7) -0.0080(10) -0.0051(8) C14 0.0273(8) 0.0468(11) 0.0523(10) -0.0104(9) -0.0087(7) 0.0144(8) C15 0.0302(8) 0.0310(8) 0.0462(10) -0.0003(7) 0.0047(7) -0.0008(6) C16 0.0301(7) 0.0300(7) 0.0289(7) 0.0089(6) 0.0071(6) 0.0083(6) C17 0.0391(8) 0.0215(7) 0.0334(8) -0.0005(6) -0.0022(6) -0.0001(6) C18 0.0269(7) 0.0275(7) 0.0390(8) 0.0066(6) -0.0042(6) -0.0058(6) C19 0.0231(6) 0.0284(7) 0.0323(7) 0.0063(6) 0.0023(5) -0.0007(5) C20 0.0269(7) 0.0306(7) 0.0228(6) 0.0046(5) 0.0051(5) 0.0050(5) C21 0.0211(6) 0.0208(6) 0.0229(6) 0.0030(5) 0.0019(4) -0.0003(5) C22 0.0210(6) 0.0162(6) 0.0230(6) 0.0015(4) 0.0011(4) 0.0010(4) C23 0.0223(6) 0.0159(6) 0.0235(6) 0.0020(4) -0.0007(5) 0.0008(4) C24 0.0227(6) 0.0182(6) 0.0236(6) 0.0038(5) 0.0022(5) 0.0011(5) C25 0.0217(6) 0.0226(6) 0.0338(7) 0.0054(5) -0.0001(5) -0.0014(5) C26 0.0206(6) 0.0195(6) 0.0259(6) 0.0030(5) -0.0019(5) -0.0008(5) C27 0.0246(6) 0.0194(6) 0.0256(6) 0.0016(5) -0.0046(5) 0.0009(5) C28 0.0241(6) 0.0183(6) 0.0212(6) 0.0011(5) -0.0005(5) 0.0009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si O4 1.6606(11) . ? Si C8 1.8388(19) . ? Si C12 1.8598(18) . ? Si C7 1.881(2) . ? N C24 1.3600(18) . ? N O1 1.4036(17) . ? N C14 1.455(2) . ? O1 C17 1.4385(19) . ? O2 C19 1.196(2) . ? O3 C19 1.338(2) . ? O3 C1 1.448(2) . ? O4 C28 1.4114(17) . ? O5 C10 1.357(2) . ? O5 C27 1.4373(17) . ? O6 C21 1.4236(16) . ? O6 C23 1.4293(16) . ? O7 C22 1.4120(17) . ? O7 C16 1.4353(18) . ? O8 C10 1.190(3) . ? O9 C24 1.2194(18) . ? C2 C10 1.495(3) . ? C3 C7 1.525(3) . ? C4 C8 1.502(4) . ? C5 C9 1.378(3) . ? C5 C6 1.378(3) . ? C6 C15 1.389(3) . ? C9 C11 1.392(3) . ? C11 C20 1.383(2) . ? C12 C13 1.532(3) . ? C15 C20 1.387(2) . ? C16 C20 1.493(2) . ? C18 C26 1.524(2) . ? C19 C25 1.504(2) . ? C21 C25 1.508(2) . ? C21 C28 1.5315(19) . ? C22 C23 1.5247(18) . ? C22 C24 1.5321(19) . ? C23 C26 1.5281(18) . ? C26 C27 1.526(2) . ? C27 C28 1.522(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 O4 Si C8 103.43(9) . . ? O4 Si C12 110.08(7) . . ? C8 Si C12 112.07(10) . . ? O4 Si C7 112.46(8) . . ? C8 Si C7 109.88(11) . . ? C12 Si C7 108.89(10) . . ? C24 N O1 116.87(12) . . ? C24 N C14 122.12(14) . . ? O1 N C14 113.57(12) . . ? N O1 C17 109.57(11) . . ? C19 O3 C1 115.28(15) . . ? C28 O4 Si 128.34(9) . . ? C10 O5 C27 117.46(14) . . ? C21 O6 C23 112.57(10) . . ? C22 O7 C16 115.07(11) . . ? C9 C5 C6 120.42(18) . . ? C5 C6 C15 119.44(18) . . ? C3 C7 Si 116.46(16) . . ? C4 C8 Si 113.94(17) . . ? C5 C9 C11 119.70(19) . . ? O8 C10 O5 123.40(18) . . ? O8 C10 C2 126.17(19) . . ? O5 C10 C2 110.41(19) . . ? C20 C11 C9 120.83(17) . . ? C13 C12 Si 114.53(13) . . ? C20 C15 C6 121.12(18) . . ? O7 C16 C20 106.77(12) . . ? O2 C19 O3 123.78(15) . . ? O2 C19 C25 125.67(16) . . ? O3 C19 C25 110.50(14) . . ? C11 C20 C15 118.49(15) . . ? C11 C20 C16 120.83(15) . . ? C15 C20 C16 120.55(15) . . ? O6 C21 C25 106.25(11) . . ? O6 C21 C28 110.16(11) . . ? C25 C21 C28 112.15(12) . . ? O7 C22 C23 106.84(10) . . ? O7 C22 C24 111.23(11) . . ? C23 C22 C24 111.46(11) . . ? O6 C23 C22 106.77(10) . . ? O6 C23 C26 110.05(10) . . ? C22 C23 C26 112.86(11) . . ? O9 C24 N 121.13(13) . . ? O9 C24 C22 122.79(13) . . ? N C24 C22 115.87(12) . . ? C19 C25 C21 112.60(13) . . ? C18 C26 C27 111.58(12) . . ? C18 C26 C23 113.19(12) . . ? C27 C26 C23 107.41(11) . . ? O5 C27 C28 108.60(11) . . ? O5 C27 C26 108.92(12) . . ? C28 C27 C26 110.90(11) . . ? O4 C28 C27 110.22(11) . . ? O4 C28 C21 108.75(11) . . ? C27 C28 C21 107.97(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.458 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.046