# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/483 data_MGB44 #------------------------------------------------------------------------------ _audit_creation_date '2000-08-21' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1999 data collection and refinement by dcrh 2000-08-21 minor issue fixed-up by acwillis, and cif produced 2000-08-21 passes checkcif with minor alerts ; #------------------------------------------------------------------------------ _publ_requested_journal ' test ' _publ_requested_category ' FO ' _publ_contact_author_name ' David C. R. Hockless ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6249 4109 ' _publ_contact_author_fax ' 61 2 6249 0750 ' _publ_contact_author_email ' willis@rsc.anu.edu.au ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; mgb44 ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 6.423(3) _cell_length_b 11.868(3) _cell_length_c 14.006(3) _cell_angle_alpha 90 _cell_angle_beta 93.30(3) _cell_angle_gamma 90 _cell_volume 1065.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.3 _cell_measurement_theta_max 28.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 390.55 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H30 O5 Si ' _chemical_formula_moiety 'C21 H30 O5 Si ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 420.00 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.88 _exptl_special_details ; The scan width was (1.30+0.30tan\q)\% with an \w scan speed of 8\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1C. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 1852 _reflns_number_total 1680 _reflns_number_gt 1209 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03315 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 60.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.14802 _diffrn_orient_matrix_UB_12 -0.00496 _diffrn_orient_matrix_UB_13 0.02599 _diffrn_orient_matrix_UB_21 0.04757 _diffrn_orient_matrix_UB_22 -0.00598 _diffrn_orient_matrix_UB_23 -0.06655 _diffrn_orient_matrix_UB_31 0.01213 _diffrn_orient_matrix_UB_32 0.08390 _diffrn_orient_matrix_UB_33 -0.00321 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 42 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 60 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 10 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si 0 2 0.244 0.330 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Si(1) 0.2077(4) 0.8543 0.4002(2) 0.0458(8) 1.000 . Uani d ? O(1') -0.1551(9) 0.5685(8) 0.1908(5) 0.067(3) 1.000 . Uani d ? O(2) -0.1821(8) 0.5795(6) 0.0329(4) 0.039(2) 1.000 . Uani d ? O(3') -0.1668(8) 0.5424(8) -0.1224(5) 0.060(2) 1.000 . Uani d ? O(6') 0.3565(8) 0.8523(7) -0.0491(4) 0.042(2) 1.000 . Uani d ? O(8) 0.3269(9) 0.7561(7) 0.3422(4) 0.043(2) 1.000 . Uani d ? C(1) -0.084(1) 0.5486(9) 0.1179(7) 0.041(3) 1.000 . Uani d ? C(3) -0.088(1) 0.5373(9) -0.0437(6) 0.038(3) 1.000 . Uani d ? C(3a) 0.120(1) 0.4806(8) -0.0112(6) 0.027(2) 1.000 . Uani d ? C(3b) 0.305(1) 0.5492(9) -0.0500(5) 0.027(2) 1.000 . Uani d ? C(4) 0.291(1) 0.579(1) -0.1588(6) 0.040(3) 1.000 . Uani d ? C(5) 0.370(2) 0.699(1) -0.1641(7) 0.064(4) 1.000 . Uani d ? C(6) 0.350(1) 0.7519(9) -0.0662(5) 0.028(3) 1.000 . Uani d ? C(6a) 0.333(1) 0.6588(8) 0.0015(5) 0.024(2) 1.000 . Uani d ? C(6b) 0.343(1) 0.6606(8) 0.0976(5) 0.027(2) 1.000 . Uani d ? C(7) 0.375(1) 0.7522(8) 0.1689(5) 0.027(2) 1.000 . Uani d ? C(8) 0.258(1) 0.7032(9) 0.2549(5) 0.032(2) 1.000 . Uani d ? C(9) 0.305(1) 0.579(1) 0.2528(6) 0.034(3) 1.000 . Uani d ? C(9a) 0.310(1) 0.5489(8) 0.1462(6) 0.028(2) 1.000 . Uani d ? C(9b) 0.120(1) 0.4875(8) 0.0991(6) 0.031(2) 1.000 . Uani d ? C(10) -0.071(1) 0.863(1) 0.3633(6) 0.056(3) 1.000 . Uani d ? C(11) 0.328(2) 0.996(1) 0.3705(9) 0.079(5) 1.000 . Uani d ? C(12) 0.257(2) 0.823(1) 0.5272(7) 0.051(3) 1.000 . Uani d ? C(13) 0.489(2) 0.817(1) 0.5562(6) 0.062(4) 1.000 . Uani d ? C(14) 0.156(2) 0.912(1) 0.5915(7) 0.072(4) 1.000 . Uani d ? C(15) 0.160(2) 0.706(1) 0.5484(8) 0.081(5) 1.000 . Uani d ? C(31a) 0.124(1) 0.360(1) -0.0516(6) 0.046(3) 1.000 . Uani d ? H(3b) 0.4281 0.5064 -0.0375 0.032 1.000 . Uiso c ? H(4a) 0.3757 0.5297 -0.1930 0.048 1.000 . Uiso c ? H(4b) 0.1506 0.5742 -0.1841 0.048 1.000 . Uiso c ? H(5a) 0.2882 0.7400 -0.2110 0.077 1.000 . Uiso c ? H(5b) 0.5115 0.6992 -0.1801 0.077 1.000 . Uiso c ? H(7a) 0.3140 0.8209 0.1464 0.033 1.000 . Uiso c ? H(7b) 0.5189 0.7638 0.1855 0.033 1.000 . Uiso c ? H(8) 0.1127 0.7146 0.2438 0.038 1.000 . Uiso c ? H(9a) 0.4297 0.5036 0.1383 0.034 1.000 . Uiso c ? H(9b) 0.1151 0.4133 0.1244 0.037 1.000 . Uiso c ? H(10a) -0.0867 0.8889 0.2992 0.067 1.000 . Uiso c ? H(10b) -0.1319 0.7899 0.3674 0.067 1.000 . Uiso c ? H(10c) -0.1381 0.9132 0.4041 0.067 1.000 . Uiso c ? H(11a) 0.2201 1.0481 0.3524 0.095 1.000 . Uiso c ? H(11b) 0.4168 0.9870 0.3191 0.095 1.000 . Uiso c ? H(11c) 0.4064 1.0239 0.4250 0.095 1.000 . Uiso c ? H(13a) 0.5550 0.7667 0.5148 0.075 1.000 . Uiso c ? H(13b) 0.5488 0.8899 0.5517 0.075 1.000 . Uiso c ? H(13c) 0.5070 0.7907 0.6202 0.075 1.000 . Uiso c ? H(14a) 0.2153 0.9843 0.5804 0.086 1.000 . Uiso c ? H(14b) 0.0101 0.9151 0.5765 0.086 1.000 . Uiso c ? H(14c) 0.1816 0.8925 0.6568 0.086 1.000 . Uiso c ? H(15a) 0.2434 0.6481 0.5233 0.098 1.000 . Uiso c ? H(15b) 0.0229 0.7018 0.5193 0.098 1.000 . Uiso c ? H(15c) 0.1547 0.6962 0.6156 0.098 1.000 . Uiso c ? H(31aa) 0.0743 0.3610 -0.1168 0.056 1.000 . Uiso c ? H(31ab) 0.2634 0.3328 -0.0470 0.056 1.000 . Uiso c ? H(31ac) 0.0383 0.3128 -0.0161 0.056 1.000 . Uiso c ? H(91) 0.1987 0.5375 0.2817 0.041 1.000 . Uiso c ? H(92) 0.4357 0.5635 0.2852 0.041 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si(1) 0.044(1) 0.059(2) 0.034(1) 0.009(2) 0.002(1) -0.012(2) O(1') 0.032(3) 0.101(7) 0.069(5) -0.009(4) 0.020(3) -0.043(5) O(2) 0.024(3) 0.032(4) 0.063(4) 0.002(3) 0.008(3) -0.008(4) O(3') 0.027(3) 0.079(6) 0.074(5) 0.005(4) -0.003(3) 0.023(5) O(6') 0.042(3) 0.034(5) 0.052(4) -0.006(4) 0.009(3) 0.009(4) O(8) 0.041(3) 0.056(5) 0.032(3) 0.002(4) 0.000(3) -0.016(3) C(1) 0.027(4) 0.035(6) 0.063(6) -0.020(5) 0.017(4) -0.021(6) C(3) 0.021(4) 0.039(6) 0.054(6) -0.007(5) -0.005(4) 0.008(5) C(3a) 0.028(4) 0.022(5) 0.032(4) -0.004(4) 0.001(3) 0.000(4) C(3b) 0.020(4) 0.032(6) 0.029(4) -0.002(4) 0.002(3) -0.005(4) C(4) 0.040(5) 0.052(7) 0.027(5) -0.009(5) 0.005(4) -0.009(5) C(5) 0.092(9) 0.059(9) 0.042(6) -0.006(7) 0.007(6) 0.001(6) C(6) 0.030(4) 0.031(6) 0.022(4) 0.004(4) 0.004(3) 0.009(4) C(6a) 0.015(4) 0.028(6) 0.029(4) 0.002(4) 0.003(3) 0.000(4) C(6b) 0.013(4) 0.034(6) 0.033(5) 0.005(4) -0.001(3) -0.010(5) C(7) 0.025(4) 0.031(6) 0.024(4) 0.001(4) -0.007(3) -0.002(4) C(8) 0.022(4) 0.047(6) 0.026(5) 0.007(4) 0.005(3) 0.002(5) C(9) 0.025(4) 0.044(6) 0.033(5) 0.007(4) 0.004(3) 0.002(5) C(9a) 0.025(4) 0.027(5) 0.032(4) 0.009(4) 0.002(3) 0.003(5) C(9b) 0.028(4) 0.024(5) 0.043(5) 0.002(4) 0.009(4) 0.002(5) C(10) 0.043(5) 0.074(8) 0.052(6) 0.015(7) 0.009(4) -0.010(7) C(11) 0.085(9) 0.06(1) 0.09(1) -0.013(8) 0.022(7) 0.009(8) C(12) 0.054(6) 0.059(9) 0.039(5) 0.010(6) 0.006(4) -0.007(5) C(13) 0.053(6) 0.08(1) 0.051(6) 0.002(6) -0.010(5) -0.011(6) C(14) 0.075(8) 0.10(1) 0.042(6) 0.002(8) 0.016(6) -0.013(7) C(15) 0.083(9) 0.10(1) 0.060(8) -0.010(8) 0.003(6) 0.021(8) C(31a) 0.034(4) 0.038(6) 0.068(6) -0.001(5) 0.006(4) -0.005(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^] ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000018(5) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ; Absolute configuration assigned to match known chirality of synthetic precursors. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1209 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_all 0.0538 _refine_ls_wR_factor_ref 0.0501 _refine_ls_goodness_of_fit_all 1.964 _refine_ls_goodness_of_fit_ref 2.227 _refine_ls_shift/su_max 0.0018 _refine_ls_shift/su_mean 0.0013 _refine_diff_density_min -0.24 _refine_diff_density_max 0.46 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si(1) O(8) 1.636(7) . . yes Si(1) C(10) 1.837(9) . . yes Si(1) C(11) 1.91(1) . . yes Si(1) C(12) 1.826(9) . . yes O(1') C(1) 1.17(1) . . yes O(2) C(1) 1.37(1) . . yes O(2) C(3) 1.36(1) . . yes O(3') C(3) 1.19(1) . . yes O(6') C(6) 1.22(1) . . yes O(8) C(8) 1.42(1) . . yes C(1) C(9b) 1.53(1) . . yes C(3) C(3a) 1.54(1) . . yes C(3a) C(3b) 1.56(1) . . yes C(3a) C(9b) 1.55(1) . . yes C(3a) C(31a) 1.54(1) . . yes C(3b) C(4) 1.56(1) . . yes C(3b) C(6a) 1.49(1) . . yes C(3b) H(3b) 0.95 . . no C(4) C(5) 1.51(1) . . yes C(4) H(4a) 0.95 . . no C(4) H(4b) 0.95 . . no C(5) C(6) 1.52(1) . . yes C(5) H(5a) 0.95 . . no C(5) H(5b) 0.95 . . no C(6) C(6a) 1.46(1) . . yes C(6a) C(6b) 1.34(1) . . yes C(6b) C(7) 1.48(1) . . yes C(6b) C(9a) 1.51(1) . . yes C(7) C(8) 1.57(1) . . yes C(7) H(7a) 0.95 . . no C(7) H(7b) 0.95 . . no C(8) C(9) 1.51(1) . . yes C(8) H(8) 0.95 . . no C(9) C(9a) 1.54(1) . . yes C(9) H(91) 0.95 . . no C(9) H(92) 0.95 . . no C(9a) C(9b) 1.53(1) . . yes C(9a) H(9a) 0.95 . . no C(9b) H(9b) 0.95 . . no C(10) H(10a) 0.95 . . no C(10) H(10b) 0.95 . . no C(10) H(10c) 0.95 . . no C(11) H(11a) 0.95 . . no C(11) H(11b) 0.95 . . no C(11) H(11c) 0.95 . . no C(12) C(13) 1.52(1) . . yes C(12) C(14) 1.55(1) . . yes C(12) C(15) 1.56(2) . . yes C(13) H(13a) 0.95 . . no C(13) H(13b) 0.95 . . no C(13) H(13c) 0.95 . . no C(14) H(14a) 0.95 . . no C(14) H(14b) 0.95 . . no C(14) H(14c) 0.95 . . no C(15) H(15a) 0.95 . . no C(15) H(15b) 0.95 . . no C(15) H(15c) 0.95 . . no C(31a) H(31aa) 0.95 . . no C(31a) H(31ab) 0.95 . . no C(31a) H(31ac) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(8) Si(1) C(10) 112.0(4) . . . yes O(8) Si(1) C(11) 108.3(4) . . . yes O(8) Si(1) C(12) 106.3(4) . . . yes C(10) Si(1) C(11) 106.9(6) . . . yes C(10) Si(1) C(12) 113.3(4) . . . yes C(11) Si(1) C(12) 110.0(6) . . . yes C(1) O(2) C(3) 112.6(7) . . . yes Si(1) O(8) C(8) 127.7(5) . . . yes O(1') C(1) O(2) 121.5(9) . . . yes O(1') C(1) C(9b) 129(1) . . . yes O(2) C(1) C(9b) 109.5(7) . . . yes O(2) C(3) O(3') 121.8(8) . . . yes O(2) C(3) C(3a) 110.3(7) . . . yes O(3') C(3) C(3a) 127.8(9) . . . yes C(3) C(3a) C(3b) 109.4(7) . . . yes C(3) C(3a) C(9b) 103.0(7) . . . yes C(3) C(3a) C(31a) 109.5(7) . . . yes C(3b) C(3a) C(9b) 111.1(6) . . . yes C(3b) C(3a) C(31a) 108.9(7) . . . yes C(9b) C(3a) C(31a) 114.7(7) . . . yes C(3a) C(3b) C(4) 117.0(6) . . . yes C(3a) C(3b) C(6a) 111.0(6) . . . yes C(3a) C(3b) H(3b) 107.5 . . . no C(4) C(3b) C(6a) 105.8(7) . . . yes C(4) C(3b) H(3b) 107.5 . . . no C(6a) C(3b) H(3b) 107.5 . . . no C(3b) C(4) C(5) 105.1(8) . . . yes C(3b) C(4) H(4a) 110.6 . . . no C(3b) C(4) H(4b) 110.6 . . . no C(5) C(4) H(4a) 110.6 . . . no C(5) C(4) H(4b) 110.6 . . . no H(4a) C(4) H(4b) 109.5 . . . no C(4) C(5) C(6) 107.4(9) . . . yes C(4) C(5) H(5a) 110.0 . . . no C(4) C(5) H(5b) 110.0 . . . no C(6) C(5) H(5a) 110.0 . . . no C(6) C(5) H(5b) 110.0 . . . no H(5a) C(5) H(5b) 109.5 . . . no O(6') C(6) C(5) 125.4(9) . . . yes O(6') C(6) C(6a) 127.9(8) . . . yes C(5) C(6) C(6a) 106.7(9) . . . yes C(3b) C(6a) C(6) 110.8(7) . . . yes C(3b) C(6a) C(6b) 119.7(8) . . . yes C(6) C(6a) C(6b) 129.5(9) . . . yes C(6a) C(6b) C(7) 133.1(9) . . . yes C(6a) C(6b) C(9a) 115.9(8) . . . yes C(7) C(6b) C(9a) 111.0(7) . . . yes C(6b) C(7) C(8) 101.0(7) . . . yes C(6b) C(7) H(7a) 111.5 . . . no C(6b) C(7) H(7b) 111.5 . . . no C(8) C(7) H(7a) 111.5 . . . no C(8) C(7) H(7b) 111.5 . . . no H(7a) C(7) H(7b) 109.5 . . . no O(8) C(8) C(7) 111.1(7) . . . yes O(8) C(8) C(9) 113.4(7) . . . yes O(8) C(8) H(8) 109.3 . . . no C(7) C(8) C(9) 104.2(7) . . . yes C(7) C(8) H(8) 109.3 . . . no C(9) C(8) H(8) 109.3 . . . no C(8) C(9) C(9a) 105.2(7) . . . yes C(8) C(9) H(91) 110.5 . . . no C(8) C(9) H(92) 110.5 . . . no C(9a) C(9) H(91) 110.5 . . . no C(9a) C(9) H(92) 110.5 . . . no H(91) C(9) H(92) 109.5 . . . no C(6b) C(9a) C(9) 104.2(8) . . . yes C(6b) C(9a) C(9b) 110.5(6) . . . yes C(6b) C(9a) H(9a) 108.0 . . . no C(9) C(9a) C(9b) 117.8(6) . . . yes C(9) C(9a) H(9a) 108.0 . . . no C(9b) C(9a) H(9a) 108.0 . . . no C(1) C(9b) C(3a) 104.0(7) . . . yes C(1) C(9b) C(9a) 111.5(7) . . . yes C(1) C(9b) H(9b) 108.9 . . . no C(3a) C(9b) C(9a) 114.3(7) . . . yes C(3a) C(9b) H(9b) 108.9 . . . no C(9a) C(9b) H(9b) 108.9 . . . no Si(1) C(10) H(10a) 109.5 . . . no Si(1) C(10) H(10b) 109.5 . . . no Si(1) C(10) H(10c) 109.5 . . . no H(10a) C(10) H(10b) 109.5 . . . no H(10a) C(10) H(10c) 109.5 . . . no H(10b) C(10) H(10c) 109.5 . . . no Si(1) C(11) H(11a) 109.5 . . . no Si(1) C(11) H(11b) 109.5 . . . no Si(1) C(11) H(11c) 109.5 . . . no H(11a) C(11) H(11b) 109.5 . . . no H(11a) C(11) H(11c) 109.5 . . . no H(11b) C(11) H(11c) 109.5 . . . no Si(1) C(12) C(13) 112.4(7) . . . yes Si(1) C(12) C(14) 111.8(8) . . . yes Si(1) C(12) C(15) 108.5(8) . . . yes C(13) C(12) C(14) 108.2(9) . . . yes C(13) C(12) C(15) 107(1) . . . yes C(14) C(12) C(15) 108.3(9) . . . yes C(12) C(13) H(13a) 109.5 . . . no C(12) C(13) H(13b) 109.5 . . . no C(12) C(13) H(13c) 109.5 . . . no H(13a) C(13) H(13b) 109.5 . . . no H(13a) C(13) H(13c) 109.5 . . . no H(13b) C(13) H(13c) 109.5 . . . no C(12) C(14) H(14a) 109.5 . . . no C(12) C(14) H(14b) 109.5 . . . no C(12) C(14) H(14c) 109.5 . . . no H(14a) C(14) H(14b) 109.5 . . . no H(14a) C(14) H(14c) 109.5 . . . no H(14b) C(14) H(14c) 109.5 . . . no C(12) C(15) H(15a) 109.5 . . . no C(12) C(15) H(15b) 109.5 . . . no C(12) C(15) H(15c) 109.5 . . . no H(15a) C(15) H(15b) 109.5 . . . no H(15a) C(15) H(15c) 109.5 . . . no H(15b) C(15) H(15c) 109.5 . . . no C(3a) C(31a) H(31aa) 109.5 . . . no C(3a) C(31a) H(31ab) 109.5 . . . no C(3a) C(31a) H(31ac) 109.5 . . . no H(31aa C(31a) H(31ab) 109.5 . . . no H(31aa C(31a) H(31ac) 109.5 . . . no H(31ab C(31a) H(31ac) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1') O(6') 3.45(1) . 2_545 no O(1') C(9a) 3.464(9) . 1_455 no O(1') C(14) 3.57(1) . 2_546 no O(1') C(6b) 3.58(1) . 1_455 no O(2) O(6') 2.93(1) . 2_545 no O(2) C(6a) 3.262(9) . 1_455 no O(2) C(31a) 3.36(1) . 2 no O(2) C(6b) 3.373(9) . 1_455 no O(2) C(3b) 3.451(9) . 1_455 no O(3') C(4) 3.52(1) . 1_455 no O(3') C(5) 3.53(1) . 1_455 no O(3') O(6') 3.562(9) . 2_545 no O(6') C(1) 3.04(1) . 2 no O(6') C(3) 3.12(1) . 2 no O(6') C(3b) 3.43(1) . 2_655 no O(6') C(31a) 3.470(9) . 2 no O(6') C(9b) 3.49(1) . 2 no O(6') C(9a) 3.50(1) . 2_655 no O(6') C(31a) 3.55(1) . 2_655 no O(6') C(3a) 3.56(1) . 2 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Si(1) O(8) C(8) C(7) . . . . 102.1(7) no Si(1) O(8) C(8) C(9) . . . . -140.9(6) no O(1') C(1) O(2) C(3) . . . . -172.6(9) no O(1') C(1) C(9b) C(3a) . . . . 176(1) no O(1') C(1) C(9b) C(9a) . . . . -60(1) no O(2) C(1) C(9b) C(3a) . . . . -4(1) no O(2) C(1) C(9b) C(9a) . . . . 120.1(8) no O(2) C(3) C(3a) C(3b) . . . . -113.3(8) no O(2) C(3) C(3a) C(9b) . . . . 5.0(9) no O(2) C(3) C(3a) C(31a) . . . . 127.4(8) no O(3') C(3) O(2) C(1) . . . . 169.5(9) no O(3') C(3) C(3a) C(3b) . . . . 70(1) no O(3') C(3) C(3a) C(9b) . . . . -172(1) no O(3') C(3) C(3a) C(31a) . . . . -50(1) no O(6') C(6) C(5) C(4) . . . . -163.6(8) no O(6') C(6) C(6a) C(3b) . . . . 173.3(8) no O(6') C(6) C(6a) C(6b) . . . . -8(1) no O(8) Si(1) C(12) C(13) . . . . 56.7(9) no O(8) Si(1) C(12) C(14) . . . . 178.6(7) no O(8) Si(1) C(12) C(15) . . . . -62.0(8) no O(8) C(8) C(7) C(6b) . . . . 159.6(6) no O(8) C(8) C(9) C(9a) . . . . -156.3(6) no C(1) O(2) C(3) C(3a) . . . . -8(1) no C(1) C(9b) C(3a) C(3) . . . . -0.8(9) no C(1) C(9b) C(3a) C(3b) . . . . 116.3(7) no C(1) C(9b) C(3a) C(31a) . . . . -119.7(8) no C(1) C(9b) C(9a) C(6b) . . . . -68.2(9) no C(1) C(9b) C(9a) C(9) . . . . 51(1) no C(3) O(2) C(1) C(9b) . . . . 7(1) no C(3) C(3a) C(3b) C(4) . . . . -50(1) no C(3) C(3a) C(3b) C(6a) . . . . 71.5(8) no C(3) C(3a) C(9b) C(9a) . . . . -122.6(7) no C(3a) C(3b) C(4) C(5) . . . . 139.3(8) no C(3a) C(3b) C(6a) C(6) . . . . -131.5(7) no C(3a) C(3b) C(6a) C(6b) . . . . 49.9(9) no C(3a) C(9b) C(9a) C(6b) . . . . 49.4(9) no C(3a) C(9b) C(9a) C(9) . . . . 169.0(8) no C(3b) C(3a) C(9b) C(9a) . . . . -6(1) no C(3b) C(4) C(5) C(6) . . . . -21(1) no C(3b) C(6a) C(6) C(5) . . . . -9.4(9) no C(3b) C(6a) C(6b) C(7) . . . . 178.0(7) no C(3b) C(6a) C(6b) C(9a) . . . . -4(1) no C(4) C(3b) C(3a) C(9b) . . . . -163.2(8) no C(4) C(3b) C(3a) C(31a) . . . . 70(1) no C(4) C(3b) C(6a) C(6) . . . . -3.6(8) no C(4) C(3b) C(6a) C(6b) . . . . 177.8(6) no C(4) C(5) C(6) C(6a) . . . . 19(1) no C(5) C(4) C(3b) C(6a) . . . . 15.0(9) no C(5) C(6) C(6a) C(6b) . . . . 169.1(8) no C(6) C(6a) C(6b) C(7) . . . . 0(1) no C(6) C(6a) C(6b) C(9a) . . . . 177.7(7) no C(6a) C(3b) C(3a) C(9b) . . . . -41.6(9) no C(6a) C(3b) C(3a) C(31a) . . . . -168.9(7) no C(6a) C(6b) C(7) C(8) . . . . 152.4(8) no C(6a) C(6b) C(9a) C(9) . . . . -173.7(6) no C(6a) C(6b) C(9a) C(9b) . . . . -46.2(9) no C(6b) C(7) C(8) C(9) . . . . 37.1(8) no C(6b) C(9a) C(9) C(8) . . . . 19.4(8) no C(7) C(6b) C(9a) C(9) . . . . 4.8(8) no C(7) C(6b) C(9a) C(9b) . . . . 132.3(7) no C(7) C(8) C(9) C(9a) . . . . -35.4(8) no C(8) O(8) Si(1) C(10) . . . . 18.6(9) no C(8) O(8) Si(1) C(11) . . . . -99.1(8) no C(8) O(8) Si(1) C(12) . . . . 142.8(7) no C(8) C(7) C(6b) C(9a) . . . . -25.6(8) no C(8) C(9) C(9a) C(9b) . . . . -103.4(9) no C(9a) C(9b) C(3a) C(31a) . . . . 118.5(8) no C(10) Si(1) C(12) C(13) . . . . -179.9(9) no C(10) Si(1) C(12) C(14) . . . . -58(1) no C(10) Si(1) C(12) C(15) . . . . 61(1) no C(11) Si(1) C(12) C(13) . . . . -60(1) no C(11) Si(1) C(12) C(14) . . . . 61.6(9) no C(11) Si(1) C(12) C(15) . . . . -179.0(8) no #------------------------------------------------------------------------------