# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2088 #=============================================================================== data_global #=============================================================================== _audit_creation_date 14-03-00 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; ; _publ_contact_author_address # Address of author for correspondance ; ; _publ_contact_author_phone 'xxxxxxxxxx' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email xxx@xx.xx.xx _publ_requested_journal 'Acta Crystallographica C' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dupont Karl' #<--'Last name, first name' ; Research School of Chemistry National Laboratory Ouchnock Islandia ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st343 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C87 H94 Cl6 O8 Si2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C87 H94 Cl6 O8 Si2' _chemical_formula_weight 1536.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 11.4684(5) _cell_length_b 17.5630(7) _cell_length_c 20.4767(5) _cell_angle_alpha 97.489(2) _cell_angle_beta 101.974(2) _cell_angle_gamma 97.733(2) _cell_volume 3944.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 30386 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 32.6 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.29 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.305 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 103 frames,246 sec/frame, delta phi = 1.7 deg. Each frame measured 2 times. Detector to crystal distance 29 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30386 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 32.55 _reflns_number_total 21194 _reflns_number_gt 10852 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10852 _refine_ls_number_parameters 930 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.137 _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_all 0.108 _refine_ls_wR_factor_ref 0.092 _refine_ls_goodness_of_fit_all 1.920 _refine_ls_goodness_of_fit_ref 1.618 _refine_ls_shift/su_max 0.043 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.758 _refine_diff_density_min -0.096 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol SI1 0.45930(7) -0.10558(5) 0.66451(4) 0.0242(3) 1.000 Uani ? ? Si O1 0.4902(2) -0.1390(1) 0.59303(9) 0.0288(9) 1.000 Uani ? ? O O2 0.3369(2) -0.0690(1) 0.65131(9) 0.0262(9) 1.000 Uani ? ? O O3 0.4433(2) -0.1756(1) 0.70660(9) 0.0292(9) 1.000 Uani ? ? O O4 0.5658(2) -0.0382(1) 0.7056(1) 0.030(1) 1.000 Uani ? ? O SI2 0.46895(7) 0.05007(5) 0.81179(3) 0.0233(3) 1.000 Uani ? ? Si O5 0.4140(2) -0.0411(1) 0.79392(9) 0.0266(9) 1.000 Uani ? ? O O6 0.4032(2) 0.0906(1) 0.86725(9) 0.0261(9) 1.000 Uani ? ? O O7 0.6125(2) 0.0609(1) 0.84364(8) 0.0251(9) 1.000 Uani ? ? O O8 0.4507(2) 0.0896(1) 0.74491(9) 0.0266(9) 1.000 Uani ? ? O C1 0.4182(3) -0.2088(2) 0.5573(1) 0.029(1) 1.000 Uani ? ? C C2 0.4545(3) -0.2789(2) 0.5697(1) 0.034(1) 1.000 Uani ? ? C C3 0.3860(3) -0.3470(2) 0.5299(1) 0.037(2) 1.000 Uani ? ? C C4 0.2824(3) -0.3471(2) 0.4800(1) 0.035(2) 1.000 Uani ? ? C C5 0.2466(3) -0.2749(2) 0.4730(1) 0.035(2) 1.000 Uani ? ? C C6 0.3121(3) -0.2055(2) 0.5117(1) 0.030(1) 1.000 Uani ? ? C C7 0.2096(4) -0.4214(2) 0.4344(2) 0.047(2) 1.000 Uani ? ? C C8 0.1886(4) -0.4102(2) 0.3603(2) 0.051(2) 1.000 Uani ? ? C C9 0.2737(5) -0.4922(2) 0.4405(2) 0.059(3) 1.000 Uani ? ? C C10 0.0866(4) -0.4380(3) 0.4534(2) 0.084(3) 1.000 Uani ? ? C C11 0.5654(3) -0.2799(2) 0.6247(1) 0.035(1) 1.000 Uani ? ? C C12 0.5444(3) -0.2880(2) 0.6944(1) 0.028(1) 1.000 Uani ? ? C C13 0.5828(3) -0.3512(2) 0.7237(2) 0.031(1) 1.000 Uani ? ? C C14 0.5779(3) -0.3605(2) 0.7896(1) 0.033(2) 1.000 Uani ? ? C C15 0.5380(3) -0.3026(2) 0.8273(1) 0.032(1) 1.000 Uani ? ? C C16 0.4993(3) -0.2386(2) 0.8011(1) 0.026(1) 1.000 Uani ? ? C C17 0.4980(3) -0.2342(2) 0.7334(1) 0.026(1) 1.000 Uani ? ? C C18 0.6152(3) -0.4315(2) 0.8213(2) 0.044(2) 1.000 Uani ? ? C C19 0.7013(4) -0.4048(2) 0.8906(2) 0.062(2) 1.000 Uani ? ? C C20 0.6797(4) -0.4797(2) 0.7773(2) 0.072(2) 1.000 Uani ? ? C C21 0.5002(5) -0.4822(2) 0.8274(2) 0.073(3) 1.000 Uani ? ? C C22 0.4669(3) -0.1748(2) 0.8482(1) 0.028(1) 1.000 Uani ? ? C C23 0.3389(3) -0.1588(2) 0.8272(1) 0.026(1) 1.000 Uani ? ? C C24 0.2415(3) -0.2111(2) 0.8333(1) 0.029(1) 1.000 Uani ? ? C C25 0.1223(3) -0.2005(2) 0.8126(1) 0.029(1) 1.000 Uani ? ? C C26 0.1030(3) -0.1361(2) 0.7811(1) 0.029(1) 1.000 Uani ? ? C C27 0.1983(3) -0.0828(2) 0.7724(1) 0.025(1) 1.000 Uani ? ? C C28 0.3156(3) -0.0923(2) 0.7993(1) 0.025(1) 1.000 Uani ? ? C C29 0.0190(3) -0.2556(2) 0.8278(2) 0.037(2) 1.000 Uani ? ? C C30 -0.1045(3) -0.2456(2) 0.7890(2) 0.053(2) 1.000 Uani ? ? C C31 0.0322(4) -0.3406(2) 0.8087(2) 0.056(2) 1.000 Uani ? ? C C32 0.0240(4) -0.2374(3) 0.9036(2) 0.064(2) 1.000 Uani ? ? C C33 0.1711(3) -0.0221(2) 0.7283(1) 0.025(1) 1.000 Uani ? ? C C34 0.1329(3) -0.0590(2) 0.6539(1) 0.025(1) 1.000 Uani ? ? C C35 0.0117(3) -0.0691(2) 0.6211(1) 0.029(1) 1.000 Uani ? ? C C36 -0.0304(3) -0.1015(2) 0.5534(1) 0.030(1) 1.000 Uani ? ? C C37 0.0564(3) -0.1219(2) 0.5186(1) 0.029(1) 1.000 Uani ? ? C C38 0.1793(3) -0.1119(2) 0.5489(1) 0.027(1) 1.000 Uani ? ? C C39 0.2159(3) -0.0824(2) 0.6181(1) 0.024(1) 1.000 Uani ? ? C C40 -0.1653(3) -0.1162(2) 0.5189(1) 0.033(2) 1.000 Uani ? ? C C41 -0.2347(3) -0.0628(3) 0.5554(2) 0.052(2) 1.000 Uani ? ? C C42 -0.2165(4) -0.2005(2) 0.5220(2) 0.054(2) 1.000 Uani ? ? C C43 -0.1851(3) -0.1029(2) 0.4460(2) 0.047(2) 1.000 Uani ? ? C C44 0.2680(3) -0.1292(2) 0.5058(1) 0.030(1) 1.000 Uani ? ? C C45 0.6776(3) 0.0298(2) 0.8959(1) 0.026(1) 1.000 Uani ? ? C C46 0.7559(3) -0.0203(2) 0.8793(1) 0.029(1) 1.000 Uani ? ? C C47 0.8242(3) -0.0501(2) 0.9316(2) 0.034(1) 1.000 Uani ? ? C C48 0.8172(3) -0.0318(2) 0.9986(1) 0.034(2) 1.000 Uani ? ? C C49 0.7393(3) 0.0191(2) 1.0128(1) 0.033(2) 1.000 Uani ? ? C C50 0.6687(3) 0.0510(2) 0.9630(1) 0.028(1) 1.000 Uani ? ? C C51 0.8864(3) -0.0688(2) 1.0533(2) 0.048(2) 1.000 Uani ? ? C C52 0.8325(3) -0.1517(2) 1.0541(2) 0.052(2) 1.000 Uani ? ? C C53 0.7425(4) -0.1947(2) 1.0104(2) 0.065(2) 1.000 Uani ? ? C C54 0.5799(3) 0.0995(2) 0.9863(1) 0.031(1) 1.000 Uani ? ? C C55 0.5542(3) 0.1715(2) 0.9568(1) 0.029(1) 1.000 Uani ? ? C C56 0.6123(3) 0.2456(2) 0.9871(1) 0.035(2) 1.000 Uani ? ? C C57 0.5841(3) 0.3122(2) 0.9613(1) 0.036(2) 1.000 Uani ? ? C C58 0.4949(3) 0.3025(2) 0.9019(1) 0.037(2) 1.000 Uani ? ? C C59 0.4344(3) 0.2291(2) 0.8689(1) 0.029(1) 1.000 Uani ? ? C C60 0.4633(3) 0.1650(2) 0.8980(1) 0.026(1) 1.000 Uani ? ? C C61 0.6528(4) 0.3924(2) 0.9953(2) 0.050(2) 1.000 Uani ? ? C C62 0.7710(4) 0.4081(2) 0.9771(2) 0.060(2) 1.000 Uani ? ? C C63 0.8750(5) 0.4179(3) 1.0175(3) 0.089(4) 1.000 Uani ? ? C C64 0.3420(3) 0.2177(2) 0.8021(1) 0.032(1) 1.000 Uani ? ? C C65 0.4017(3) 0.2193(2) 0.7420(1) 0.028(1) 1.000 Uani ? ? C C66 0.4032(3) 0.2846(2) 0.7096(1) 0.032(1) 1.000 Uani ? ? C C67 0.4537(3) 0.2890(2) 0.6537(1) 0.032(1) 1.000 Uani ? ? C C68 0.5026(3) 0.2263(2) 0.6302(1) 0.031(1) 1.000 Uani ? ? C C69 0.5033(2) 0.1595(2) 0.6606(1) 0.025(1) 1.000 Uani ? ? C C70 0.4542(2) 0.1578(2) 0.7175(1) 0.024(1) 1.000 Uani ? ? C C71 0.4503(3) 0.3598(2) 0.6182(2) 0.045(2) 1.000 Uani ? ? C C72 0.3326(4) 0.3881(2) 0.6072(2) 0.052(2) 1.000 Uani ? ? C C73 0.3150(5) 0.4569(3) 0.6264(2) 0.081(3) 1.000 Uani ? ? C C74 0.5504(3) 0.0903(2) 0.6300(1) 0.028(1) 1.000 Uani ? ? C C75 0.6664(3) 0.0758(2) 0.6745(1) 0.027(1) 1.000 Uani ? ? C C76 0.7737(3) 0.1273(2) 0.6830(1) 0.033(1) 1.000 Uani ? ? C C77 0.8795(3) 0.1210(2) 0.7279(1) 0.035(2) 1.000 Uani ? ? C C78 0.8745(3) 0.0616(2) 0.7672(1) 0.032(1) 1.000 Uani ? ? C C79 0.7701(3) 0.0096(2) 0.7608(1) 0.028(1) 1.000 Uani ? ? C C80 0.6677(2) 0.0148(2) 0.7111(1) 0.025(1) 1.000 Uani ? ? C C81 0.9973(4) 0.1766(3) 0.7372(2) 0.060(2) 1.000 Uani ? ? C C82 0.9962(6) 0.2457(4) 0.7077(3) 0.038(3) 0.500 Uani ? ? C C82A 1.0396(7) 0.1932(5) 0.6847(4) 0.050(4) 0.500 Uani ? ? C C83 1.0670(4) 0.2709(3) 0.6679(2) 0.063(2) 1.000 Uani ? ? C C84 0.7646(3) -0.0498(2) 0.8074(1) 0.032(1) 1.000 Uani ? ? C C85 0.1697(4) -0.2883(2) 0.6454(2) 0.057(2) 1.000 Uani ? ? C CL1 0.0147(1) -0.30129(8) 0.61059(7) 0.0879(8) 1.000 Uani ? ? Cl CL2 0.2145(1) -0.36941(7) 0.67518(6) 0.0794(7) 1.000 Uani ? ? Cl C86 0.7455(3) 0.2320(2) 0.8387(2) 0.049(2) 1.000 Uani ? ? C CL3 0.8816(1) 0.23009(7) 0.89584(6) 0.0723(7) 1.000 Uani ? ? Cl CL4 0.7556(1) 0.31124(6) 0.79432(5) 0.0631(5) 1.000 Uani ? ? Cl C87 0.0903(6) 0.4048(4) 0.8609(3) 0.113(2) 1.000 Uiso ? ? C CL5 0.1954(4) 0.3699(2) 0.9073(2) 0.129(1) 0.500 Uiso ? ? Cl CL6 0.1490(3) 0.4646(2) 0.7969(2) 0.110(1) 0.500 Uiso ? ? Cl Cl5a 0.2408(3) 0.3935(2) 0.9027(2) 0.109(1) 0.500 Uiso ? ? Cl Cl6a 0.0754(5) 0.4564(3) 0.8076(2) 0.168(2) 0.500 Uiso ? ? Cl H1 0.4107 -0.3954 0.5370 0.0487 1.000 Uiso calc C3 H H2 0.1748 -0.2733 0.4407 0.0470 1.000 Uiso calc C5 H H3 0.1434 -0.4566 0.3323 0.0723 1.000 Uiso calc C8 H H4 0.1452 -0.3684 0.3539 0.0723 1.000 Uiso calc C8 H H5 0.2643 -0.3988 0.3486 0.0723 1.000 Uiso calc C8 H H6 0.2247 -0.5366 0.4112 0.0923 1.000 Uiso calc C9 H H7 0.3490 -0.4822 0.4281 0.0923 1.000 Uiso calc C9 H H8 0.2870 -0.5017 0.4858 0.0923 1.000 Uiso calc C9 H H9 0.0400 -0.4840 0.4255 0.1181 1.000 Uiso calc C10 H H10 0.0992 -0.4447 0.4995 0.1181 1.000 Uiso calc C10 H H11 0.0448 -0.3954 0.4469 0.1181 1.000 Uiso calc C10 H H12 0.6191 -0.2325 0.6289 0.0453 1.000 Uiso calc C11 H H13 0.6023 -0.3224 0.6104 0.0453 1.000 Uiso calc C11 H H14 0.6133 -0.3891 0.6974 0.0435 1.000 Uiso calc C13 H H15 0.5369 -0.3066 0.8730 0.0417 1.000 Uiso calc C15 H H16 0.7233 -0.4489 0.9093 0.0811 1.000 Uiso calc C19 H H17 0.7718 -0.3728 0.8859 0.0811 1.000 Uiso calc C19 H H18 0.6624 -0.3760 0.9197 0.0811 1.000 Uiso calc C19 H H19 0.7013 -0.5227 0.7981 0.0946 1.000 Uiso calc C20 H H20 0.6274 -0.4982 0.7340 0.0946 1.000 Uiso calc C20 H H21 0.7505 -0.4483 0.7724 0.0946 1.000 Uiso calc C20 H H22 0.5205 -0.5263 0.8468 0.1004 1.000 Uiso calc C21 H H23 0.4602 -0.4529 0.8555 0.1004 1.000 Uiso calc C21 H H24 0.4483 -0.4989 0.7838 0.1004 1.000 Uiso calc C21 H H25 0.5210 -0.1280 0.8503 0.0362 1.000 Uiso calc C22 H H26 0.4772 -0.1894 0.8918 0.0362 1.000 Uiso calc C22 H H27 0.2569 -0.2562 0.8525 0.0368 1.000 Uiso calc C24 H H28 0.0224 -0.1281 0.7651 0.0365 1.000 Uiso calc C26 H H29 -0.1653 -0.2807 0.8000 0.0728 1.000 Uiso calc C30 H H30 -0.1168 -0.1936 0.8009 0.0728 1.000 Uiso calc C30 H H31 -0.1088 -0.2561 0.7418 0.0728 1.000 Uiso calc C30 H H32 -0.0324 -0.3737 0.8185 0.0753 1.000 Uiso calc C31 H H33 0.0302 -0.3514 0.7618 0.0753 1.000 Uiso calc C31 H H34 0.1070 -0.3496 0.8341 0.0753 1.000 Uiso calc C31 H H35 -0.0392 -0.2709 0.9142 0.0808 1.000 Uiso calc C32 H H36 0.0998 -0.2454 0.9286 0.0808 1.000 Uiso calc C32 H H37 0.0147 -0.1848 0.9151 0.0808 1.000 Uiso calc C32 H H38 0.2414 0.0160 0.7350 0.0331 1.000 Uiso calc C33 H H39 0.1075 0.0020 0.7404 0.0331 1.000 Uiso calc C33 H H40 -0.0445 -0.0531 0.6461 0.0363 1.000 Uiso calc C35 H H41 0.0305 -0.1436 0.4720 0.0399 1.000 Uiso calc C37 H H42 -0.3177 -0.0733 0.5328 0.0754 1.000 Uiso calc C41 H H43 -0.2267 -0.0718 0.6008 0.0754 1.000 Uiso calc C41 H H44 -0.2028 -0.0100 0.5554 0.0754 1.000 Uiso calc C41 H H45 -0.3002 -0.2111 0.5009 0.0767 1.000 Uiso calc C42 H H46 -0.1753 -0.2349 0.4991 0.0767 1.000 Uiso calc C42 H H47 -0.2056 -0.2077 0.5679 0.0767 1.000 Uiso calc C42 H H48 -0.2693 -0.1124 0.4260 0.0641 1.000 Uiso calc C43 H H49 -0.1524 -0.0506 0.4447 0.0641 1.000 Uiso calc C43 H H50 -0.1461 -0.1374 0.4217 0.0641 1.000 Uiso calc C43 H H51 0.2296 -0.1301 0.4598 0.0400 1.000 Uiso calc C44 H H52 0.3361 -0.0886 0.5190 0.0400 1.000 Uiso calc C44 H H53 0.8776 -0.0842 0.9210 0.0441 1.000 Uiso calc C47 H H54 0.7341 0.0327 1.0584 0.0447 1.000 Uiso calc C49 H H55 0.8890 -0.0387 1.0958 0.0618 1.000 Uiso calc C51 H H56 0.9662 -0.0682 1.0470 0.0618 1.000 Uiso calc C51 H H57 0.8687 -0.1750 1.0909 0.0660 1.000 Uiso calc C52 H H58 0.7161 -0.2466 1.0161 0.0816 1.000 Uiso calc C53 H H59 0.7028 -0.1745 0.9726 0.0816 1.000 Uiso calc C53 H H60 0.6091 0.1158 1.0337 0.0423 1.000 Uiso calc C54 H H61 0.5046 0.0656 0.9778 0.0423 1.000 Uiso calc C54 H H62 0.6740 0.2514 1.0272 0.0473 1.000 Uiso calc C56 H H63 0.4748 0.3471 0.8833 0.0473 1.000 Uiso calc C58 H H64 0.6659 0.3952 1.0430 0.0723 1.000 Uiso calc C61 H H65 0.6060 0.4306 0.9814 0.0723 1.000 Uiso calc C61 H H66 0.7695 0.4112 0.9309 0.0869 1.000 Uiso calc C62 H H67 0.9461 0.4277 1.0009 0.1275 1.000 Uiso calc C63 H H68 0.8813 0.4153 1.0641 0.1275 1.000 Uiso calc C63 H H69 0.2950 0.2583 0.8032 0.0401 1.000 Uiso calc C64 H H70 0.2910 0.1689 0.7963 0.0401 1.000 Uiso calc C64 H H71 0.3688 0.3273 0.7262 0.0412 1.000 Uiso calc C66 H H72 0.5370 0.2285 0.5920 0.0411 1.000 Uiso calc C68 H H73 0.4684 0.3467 0.5754 0.0576 1.000 Uiso calc C71 H H74 0.5104 0.4009 0.6449 0.0576 1.000 Uiso calc C71 H H75 0.2635 0.3513 0.5835 0.0671 1.000 Uiso calc C72 H H76 0.2356 0.4692 0.6168 0.1056 1.000 Uiso calc C73 H H77 0.3812 0.4958 0.6503 0.1056 1.000 Uiso calc C73 H H78 0.5658 0.0993 0.5875 0.0372 1.000 Uiso calc C74 H H79 0.4905 0.0453 0.6234 0.0372 1.000 Uiso calc C74 H H80 0.7747 0.1683 0.6571 0.0422 1.000 Uiso calc C76 H H81 0.9452 0.0570 0.7992 0.0425 1.000 Uiso calc C78 H H82 0.6956 -0.0885 0.7875 0.0412 1.000 Uiso calc C84 H H83 0.8356 -0.0727 0.8103 0.0412 1.000 Uiso calc C84 H H84 0.1900 -0.2459 0.6819 0.0759 1.000 Uiso calc C85 H H85 0.2116 -0.2766 0.6116 0.0759 1.000 Uiso calc C85 H H86 0.6839 0.2358 0.8630 0.0632 1.000 Uiso calc C86 H H87 0.7250 0.1850 0.8070 0.0632 1.000 Uiso calc C86 H 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 _atom_site_aniso_type_symbol SI1 0.0256(4) 0.0243(4) 0.0229(3) 0.0046(3) 0.0058(3) 0.0015(3) Si O1 0.028(1) 0.031(1) 0.0277(9) 0.0031(8) 0.0089(7) 0.0011(8) O O2 0.0256(9) 0.028(1) 0.0250(9) 0.0048(8) 0.0044(7) 0.0027(7) O O3 0.038(1) 0.0249(9) 0.0260(8) 0.0115(8) 0.0088(7) 0.0056(7) O O4 0.028(1) 0.031(1) 0.0331(9) 0.0006(9) 0.0056(8) 0.0003(8) O SI2 0.0256(4) 0.0228(4) 0.0216(3) 0.0041(3) 0.0048(3) 0.0021(3) Si O5 0.028(1) 0.0240(9) 0.0285(9) 0.0026(8) 0.0071(7) 0.0034(7) O O6 0.031(1) 0.0229(9) 0.0250(8) 0.0027(8) 0.0092(7) -0.0000(7) O O7 0.0262(9) 0.0274(9) 0.0220(8) 0.0059(8) 0.0018(7) 0.0047(7) O O8 0.033(1) 0.0247(9) 0.0233(8) 0.0062(8) 0.0068(7) 0.0054(7) O C1 0.033(1) 0.028(1) 0.026(1) 0.001(1) 0.012(1) -0.003(1) C C2 0.036(1) 0.035(2) 0.030(1) 0.007(1) 0.015(1) 0.001(1) C C3 0.050(2) 0.033(2) 0.031(1) 0.009(1) 0.016(1) 0.002(1) C C4 0.044(2) 0.034(2) 0.029(1) -0.000(1) 0.011(1) -0.003(1) C C5 0.037(2) 0.047(2) 0.024(1) 0.005(1) 0.011(1) 0.002(1) C C6 0.034(1) 0.036(2) 0.023(1) 0.005(1) 0.013(1) 0.004(1) C C7 0.057(2) 0.045(2) 0.040(2) -0.007(2) 0.015(1) -0.006(2) C C8 0.065(2) 0.051(2) 0.041(2) 0.009(2) 0.004(2) -0.014(2) C C9 0.111(4) 0.035(2) 0.052(2) -0.003(2) 0.002(2) -0.002(2) C C10 0.086(3) 0.077(3) 0.091(3) -0.045(2) 0.044(2) -0.033(2) C C11 0.034(1) 0.034(2) 0.038(1) 0.013(1) 0.012(1) -0.000(1) C C12 0.026(1) 0.027(1) 0.030(1) 0.006(1) 0.004(1) 0.002(1) C C13 0.031(2) 0.023(1) 0.042(2) 0.006(1) 0.004(1) -0.001(1) C C14 0.035(2) 0.027(1) 0.038(1) 0.006(1) 0.003(1) 0.005(1) C C15 0.034(2) 0.032(1) 0.031(1) 0.006(1) 0.006(1) 0.010(1) C C16 0.024(1) 0.025(1) 0.029(1) 0.003(1) 0.004(1) 0.003(1) C C17 0.027(1) 0.020(1) 0.032(1) 0.004(1) 0.004(1) 0.003(1) C C18 0.055(2) 0.031(2) 0.050(2) 0.015(1) 0.007(1) 0.009(1) C C19 0.082(3) 0.051(2) 0.057(2) 0.031(2) 0.002(2) 0.022(2) C C20 0.110(3) 0.051(2) 0.066(2) 0.051(2) 0.015(2) 0.015(2) C C21 0.088(3) 0.042(2) 0.106(3) 0.003(2) 0.022(2) 0.036(2) C C22 0.032(1) 0.028(1) 0.024(1) 0.008(1) 0.004(1) 0.007(1) C C23 0.029(1) 0.027(1) 0.022(1) 0.006(1) 0.004(1) 0.001(1) C C24 0.037(1) 0.026(1) 0.025(1) 0.008(1) 0.009(1) 0.009(1) C C25 0.033(1) 0.027(1) 0.028(1) 0.005(1) 0.010(1) 0.004(1) C C26 0.027(1) 0.033(1) 0.027(1) 0.009(1) 0.008(1) 0.005(1) C C27 0.032(1) 0.027(1) 0.018(1) 0.006(1) 0.006(1) 0.003(1) C C28 0.031(1) 0.022(1) 0.022(1) 0.002(1) 0.0081(9) -0.001(1) C C29 0.032(2) 0.034(2) 0.048(2) 0.004(1) 0.014(1) 0.013(1) C C30 0.038(2) 0.045(2) 0.086(2) 0.001(2) 0.013(2) 0.023(2) C C31 0.053(2) 0.036(2) 0.091(2) 0.001(2) 0.029(2) 0.017(2) C C32 0.057(2) 0.075(3) 0.062(2) 0.003(2) 0.034(1) 0.015(2) C C33 0.028(1) 0.023(1) 0.024(1) 0.007(1) 0.004(1) 0.001(1) C C34 0.029(1) 0.024(1) 0.023(1) 0.007(1) 0.007(1) 0.006(1) C C35 0.030(1) 0.029(1) 0.027(1) 0.007(1) 0.008(1) 0.009(1) C C36 0.029(1) 0.028(1) 0.031(1) 0.004(1) 0.005(1) 0.010(1) C C37 0.035(2) 0.030(1) 0.024(1) 0.003(1) 0.002(1) 0.003(1) C C38 0.029(1) 0.027(1) 0.026(1) 0.004(1) 0.006(1) 0.004(1) C C39 0.024(1) 0.024(1) 0.023(1) 0.002(1) 0.002(1) 0.005(1) C C40 0.028(1) 0.039(2) 0.034(1) 0.001(1) 0.001(1) 0.005(1) C C41 0.031(2) 0.079(3) 0.058(2) 0.018(2) -0.001(2) -0.002(2) C C42 0.040(2) 0.055(2) 0.073(2) -0.008(2) -0.004(2) 0.021(2) C C43 0.034(2) 0.067(2) 0.045(2) 0.007(2) -0.001(1) 0.017(2) C C44 0.032(1) 0.039(2) 0.021(1) 0.006(1) 0.007(1) 0.004(1) C C45 0.026(1) 0.025(1) 0.027(1) 0.002(1) 0.002(1) 0.005(1) C C46 0.027(1) 0.027(1) 0.032(1) 0.003(1) 0.004(1) 0.007(1) C C47 0.029(1) 0.032(1) 0.040(1) 0.008(1) 0.004(1) 0.010(1) C C48 0.035(2) 0.035(2) 0.033(1) 0.000(1) -0.002(1) 0.009(1) C C49 0.041(2) 0.035(2) 0.025(1) 0.001(1) 0.002(1) 0.008(1) C C50 0.030(1) 0.028(1) 0.026(1) -0.001(1) 0.002(1) 0.003(1) C C51 0.046(2) 0.054(2) 0.044(2) 0.017(2) 0.001(1) 0.020(1) C C52 0.049(2) 0.064(2) 0.045(2) 0.013(2) 0.010(1) 0.028(1) C C53 0.069(2) 0.058(2) 0.068(2) 0.009(2) 0.023(2) 0.024(2) C C54 0.043(2) 0.035(2) 0.019(1) 0.007(1) 0.006(1) 0.005(1) C C55 0.034(1) 0.029(1) 0.024(1) 0.007(1) 0.010(1) 0.003(1) C C56 0.045(2) 0.034(2) 0.027(1) 0.004(1) 0.007(1) -0.002(1) C C57 0.046(2) 0.030(2) 0.033(1) 0.002(1) 0.011(1) -0.001(1) C C58 0.047(2) 0.029(1) 0.036(1) 0.011(1) 0.014(1) 0.006(1) C C59 0.034(1) 0.030(1) 0.025(1) 0.008(1) 0.013(1) 0.003(1) C C60 0.031(1) 0.025(1) 0.022(1) 0.003(1) 0.009(1) 0.001(1) C C61 0.076(3) 0.033(2) 0.051(2) 0.005(2) 0.006(2) -0.000(2) C C62 0.085(3) 0.038(2) 0.067(2) -0.011(2) 0.015(2) -0.001(2) C C63 0.086(4) 0.064(3) 0.128(4) -0.013(3) 0.007(3) 0.011(3) C C64 0.033(1) 0.028(1) 0.034(1) 0.012(1) 0.009(1) 0.004(1) C C65 0.027(1) 0.027(1) 0.028(1) 0.006(1) 0.004(1) 0.004(1) C C66 0.030(1) 0.031(1) 0.035(1) 0.008(1) 0.004(1) 0.009(1) C C67 0.030(2) 0.032(1) 0.034(1) 0.002(1) 0.003(1) 0.012(1) C C68 0.029(1) 0.040(2) 0.025(1) 0.003(1) 0.005(1) 0.011(1) C C69 0.021(1) 0.032(1) 0.024(1) 0.004(1) 0.001(1) 0.004(1) C C70 0.022(1) 0.027(1) 0.024(1) 0.002(1) 0.001(1) 0.003(1) C C71 0.055(2) 0.037(2) 0.045(2) 0.005(2) 0.014(1) 0.018(1) C C72 0.061(2) 0.044(2) 0.052(2) 0.014(2) 0.005(2) 0.024(1) C C73 0.095(3) 0.062(2) 0.090(3) 0.040(2) 0.008(3) 0.021(2) C C74 0.029(1) 0.035(2) 0.021(1) 0.001(1) 0.006(1) 0.004(1) C C75 0.025(1) 0.033(1) 0.023(1) 0.008(1) 0.007(1) 0.000(1) C C76 0.031(1) 0.039(2) 0.029(1) 0.004(1) 0.010(1) 0.009(1) C C77 0.028(1) 0.045(2) 0.034(1) 0.001(1) 0.006(1) 0.010(1) C C78 0.026(1) 0.043(2) 0.029(1) 0.009(1) 0.005(1) 0.004(1) C C79 0.027(1) 0.031(1) 0.026(1) 0.009(1) 0.008(1) 0.004(1) C C80 0.023(1) 0.028(1) 0.026(1) 0.004(1) 0.006(1) -0.001(1) C C81 0.033(2) 0.086(2) 0.075(2) -0.019(2) -0.004(2) 0.045(2) C C82 0.033(3) 0.034(3) 0.047(3) -0.004(3) 0.008(3) 0.000(3) C C82A 0.030(3) 0.077(5) 0.053(4) -0.003(4) 0.010(3) 0.008(4) C C83 0.047(2) 0.087(3) 0.063(2) -0.005(2) 0.005(2) 0.037(2) C C84 0.033(1) 0.029(1) 0.034(1) 0.012(1) 0.008(1) 0.004(1) C C85 0.071(2) 0.046(2) 0.056(2) -0.005(2) 0.024(2) -0.002(2) C CL1 0.0801(8) 0.1014(8) 0.0835(7) 0.0300(7) 0.0091(6) 0.0249(6) Cl CL2 0.0733(7) 0.0699(7) 0.0975(7) 0.0279(5) 0.0269(5) 0.0166(6) Cl C86 0.053(2) 0.044(2) 0.050(2) 0.005(2) 0.018(1) 0.006(2) C CL3 0.0785(7) 0.0731(7) 0.0657(6) 0.0264(6) -0.0043(5) 0.0050(5) Cl CL4 0.0759(6) 0.0530(5) 0.0626(5) 0.0133(5) 0.0205(4) 0.0186(4) Cl # 10. MOLECULAR GEOMETRY 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 SI1 O1 1.631(2) . . ? SI1 O2 1.609(2) . . ? SI1 O3 1.604(2) . . ? SI1 O4 1.590(2) . . ? O1 C1 1.401(4) . . ? O2 C39 1.386(4) . . ? O3 C17 1.390(3) . . ? O4 C80 1.368(4) . . ? SI2 O5 1.604(2) . . ? SI2 O6 1.629(2) . . ? SI2 O7 1.615(2) . . ? SI2 O8 1.602(2) . . ? O5 C28 1.378(4) . . ? O6 C60 1.393(4) . . ? O7 C45 1.390(3) . . ? O8 C70 1.387(3) . . ? C1 C2 1.389(5) . . ? C1 C6 1.385(5) . . ? C2 C3 1.393(5) . . ? C2 C11 1.517(5) . . ? C3 C4 1.397(5) . . ? C4 C5 1.400(5) . . ? C4 C7 1.529(5) . . ? C5 C6 1.390(5) . . ? C6 C44 1.505(5) . . ? C7 C8 1.529(6) . . ? C7 C9 1.533(7) . . ? C7 C10 1.540(6) . . ? C11 C12 1.517(4) . . ? C12 C13 1.408(4) . . ? C12 C17 1.388(4) . . ? C13 C14 1.392(5) . . ? C14 C15 1.381(5) . . ? C14 C18 1.549(5) . . ? C15 C16 1.394(4) . . ? C16 C17 1.394(4) . . ? C16 C22 1.517(4) . . ? C18 C19 1.527(6) . . ? C18 C20 1.523(6) . . ? C18 C21 1.527(6) . . ? C22 C23 1.516(4) . . ? C23 C24 1.386(4) . . ? C23 C28 1.399(4) . . ? C24 C25 1.390(4) . . ? C25 C26 1.395(4) . . ? C25 C29 1.536(4) . . ? C26 C27 1.396(4) . . ? C27 C28 1.385(4) . . ? C27 C33 1.509(4) . . ? C29 C30 1.519(5) . . ? C29 C31 1.530(6) . . ? C29 C32 1.531(6) . . ? C33 C34 1.524(4) . . ? C34 C35 1.388(4) . . ? C34 C39 1.389(4) . . ? C35 C36 1.388(4) . . ? C36 C37 1.396(5) . . ? C36 C40 1.533(5) . . ? C37 C38 1.394(4) . . ? C38 C39 1.399(4) . . ? C38 C44 1.514(4) . . ? C40 C41 1.529(6) . . ? C40 C42 1.532(5) . . ? C40 C43 1.515(5) . . ? C45 C46 1.399(4) . . ? C45 C50 1.405(4) . . ? C46 C47 1.393(4) . . ? C46 C84 1.524(4) . . ? C47 C48 1.388(5) . . ? C48 C49 1.393(5) . . ? C48 C51 1.506(5) . . ? C49 C50 1.391(4) . . ? C50 C54 1.523(5) . . ? C51 C52 1.507(6) . . ? C52 C53 1.291(6) . . ? C54 C55 1.508(4) . . ? C55 C56 1.382(5) . . ? C55 C60 1.401(4) . . ? C56 C57 1.393(5) . . ? C57 C58 1.393(5) . . ? C57 C61 1.519(5) . . ? C58 C59 1.392(5) . . ? C59 C60 1.387(4) . . ? C59 C64 1.519(4) . . ? C61 C62 1.479(7) . . ? C62 C63 1.279(8) . . ? C64 C65 1.527(4) . . ? C65 C66 1.398(4) . . ? C65 C70 1.394(4) . . ? C66 C67 1.392(4) . . ? C67 C68 1.378(5) . . ? C67 C71 1.521(4) . . ? C68 C69 1.397(4) . . ? C69 C70 1.398(4) . . ? C69 C74 1.511(4) . . ? C71 C72 1.483(6) . . ? C72 C73 1.278(6) . . ? C74 C75 1.521(4) . . ? C75 C76 1.390(4) . . ? C75 C80 1.386(4) . . ? C76 C77 1.389(5) . . ? C77 C78 1.402(5) . . ? C77 C81 1.517(5) . . ? C78 C79 1.376(5) . . ? C79 C80 1.407(4) . . ? C79 C84 1.507(4) . . ? C81 C82 1.425(8) . . ? C81 C82A 1.318(9) . . ? C82 C82A 1.19(1) . . ? C82 C83 1.339(8) . . ? C82A C83 1.46(1) . . ? C85 CL1 1.745(5) . . ? C85 CL2 1.720(5) . . ? C86 CL3 1.754(4) . . ? C86 CL4 1.761(4) . . ? C87 CL5 1.614(9) . . ? C87 CL6 1.952(8) . . ? C87 Cl5a 1.809(9) . . ? C87 Cl6a 1.505(8) . . ? 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 ? ? ? ? ? ? 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 O1 SI1 O2 110.7(1) . . . ? O1 SI1 O3 108.9(1) . . . ? O1 SI1 O4 109.3(1) . . . ? O2 SI1 O3 109.4(1) . . . ? O2 SI1 O4 107.8(1) . . . ? O3 SI1 O4 110.9(1) . . . ? SI1 O1 C1 116.1(2) . . . ? SI1 O2 C39 145.1(2) . . . ? SI1 O3 C17 144.5(2) . . . ? SI1 O4 C80 152.8(2) . . . ? O5 SI2 O6 108.3(1) . . . ? O5 SI2 O7 109.3(1) . . . ? O5 SI2 O8 110.8(1) . . . ? O6 SI2 O7 109.5(1) . . . ? O6 SI2 O8 111.5(1) . . . ? O7 SI2 O8 107.6(1) . . . ? SI2 O5 C28 140.3(2) . . . ? SI2 O6 C60 112.7(2) . . . ? SI2 O7 C45 131.1(2) . . . ? SI2 O8 C70 147.4(2) . . . ? O1 C1 C2 118.9(3) . . . ? O1 C1 C6 118.8(3) . . . ? C2 C1 C6 122.2(3) . . . ? C1 C2 C3 117.6(3) . . . ? C1 C2 C11 120.3(3) . . . ? C3 C2 C11 122.0(3) . . . ? C2 C3 C4 122.7(3) . . . ? C3 C4 C5 116.8(3) . . . ? C3 C4 C7 122.9(3) . . . ? C5 C4 C7 120.4(3) . . . ? C4 C5 C6 122.5(3) . . . ? C1 C6 C5 117.9(3) . . . ? C1 C6 C44 120.7(3) . . . ? C5 C6 C44 121.3(3) . . . ? C4 C7 C8 110.0(3) . . . ? C4 C7 C9 113.0(4) . . . ? C4 C7 C10 108.3(3) . . . ? C8 C7 C9 106.9(3) . . . ? C8 C7 C10 109.2(4) . . . ? C9 C7 C10 109.5(4) . . . ? C2 C11 C12 116.7(3) . . . ? C11 C12 C13 117.8(3) . . . ? C11 C12 C17 124.4(3) . . . ? C13 C12 C17 117.6(3) . . . ? C12 C13 C14 122.7(3) . . . ? C13 C14 C15 117.1(3) . . . ? C13 C14 C18 123.1(3) . . . ? C15 C14 C18 119.9(3) . . . ? C14 C15 C16 122.7(3) . . . ? C15 C16 C17 118.3(3) . . . ? C15 C16 C22 118.7(3) . . . ? C17 C16 C22 123.0(3) . . . ? O3 C17 C12 122.1(3) . . . ? O3 C17 C16 116.5(3) . . . ? C12 C17 C16 121.4(3) . . . ? C14 C18 C19 110.5(3) . . . ? C14 C18 C20 111.5(3) . . . ? C14 C18 C21 107.7(3) . . . ? C19 C18 C20 107.6(4) . . . ? C19 C18 C21 110.6(4) . . . ? C20 C18 C21 108.9(4) . . . ? C16 C22 C23 114.9(2) . . . ? C22 C23 C24 120.6(3) . . . ? C22 C23 C28 121.1(3) . . . ? C24 C23 C28 118.2(3) . . . ? C23 C24 C25 122.9(3) . . . ? C24 C25 C26 116.9(3) . . . ? C24 C25 C29 120.5(3) . . . ? C26 C25 C29 122.6(3) . . . ? C25 C26 C27 122.1(3) . . . ? C26 C27 C28 118.7(3) . . . ? C26 C27 C33 119.2(3) . . . ? C28 C27 C33 121.8(3) . . . ? O5 C28 C23 117.1(3) . . . ? O5 C28 C27 121.9(3) . . . ? C23 C28 C27 120.8(3) . . . ? C25 C29 C30 112.5(3) . . . ? C25 C29 C31 110.7(3) . . . ? C25 C29 C32 108.0(3) . . . ? C30 C29 C31 107.3(3) . . . ? C30 C29 C32 108.5(3) . . . ? C31 C29 C32 109.8(3) . . . ? C27 C33 C34 110.7(2) . . . ? C33 C34 C35 118.8(3) . . . ? C33 C34 C39 121.8(3) . . . ? C35 C34 C39 119.4(3) . . . ? C34 C35 C36 122.5(3) . . . ? C35 C36 C37 116.4(3) . . . ? C35 C36 C40 121.9(3) . . . ? C37 C36 C40 121.7(3) . . . ? C36 C37 C38 123.3(3) . . . ? C37 C38 C39 117.8(3) . . . ? C37 C38 C44 119.5(3) . . . ? C39 C38 C44 122.6(3) . . . ? O2 C39 C34 118.2(3) . . . ? O2 C39 C38 121.1(3) . . . ? C34 C39 C38 120.5(3) . . . ? C36 C40 C41 111.7(3) . . . ? C36 C40 C42 107.7(3) . . . ? C36 C40 C43 111.4(3) . . . ? C41 C40 C42 107.9(3) . . . ? C41 C40 C43 107.9(3) . . . ? C42 C40 C43 110.2(3) . . . ? C6 C44 C38 114.3(3) . . . ? O7 C45 C46 117.4(3) . . . ? O7 C45 C50 120.9(3) . . . ? C46 C45 C50 121.7(3) . . . ? C45 C46 C47 117.9(3) . . . ? C45 C46 C84 124.5(3) . . . ? C47 C46 C84 117.4(3) . . . ? C46 C47 C48 122.6(3) . . . ? C47 C48 C49 117.5(3) . . . ? C47 C48 C51 121.3(3) . . . ? C49 C48 C51 121.1(3) . . . ? C48 C49 C50 122.8(3) . . . ? C45 C50 C49 117.5(3) . . . ? C45 C50 C54 126.2(3) . . . ? C49 C50 C54 116.0(3) . . . ? C48 C51 C52 114.2(3) . . . ? C51 C52 C53 127.3(4) . . . ? C50 C54 C55 121.1(3) . . . ? C54 C55 C56 123.0(3) . . . ? C54 C55 C60 119.8(3) . . . ? C56 C55 C60 117.2(3) . . . ? C55 C56 C57 122.7(3) . . . ? C56 C57 C58 117.9(3) . . . ? C56 C57 C61 120.9(3) . . . ? C58 C57 C61 121.2(3) . . . ? C57 C58 C59 121.7(3) . . . ? C58 C59 C60 118.0(3) . . . ? C58 C59 C64 122.0(3) . . . ? C60 C59 C64 120.0(3) . . . ? O6 C60 C55 117.7(3) . . . ? O6 C60 C59 119.8(3) . . . ? C55 C60 C59 122.4(3) . . . ? C57 C61 C62 111.4(4) . . . ? C61 C62 C63 126.2(5) . . . ? C59 C64 C65 112.1(3) . . . ? C64 C65 C66 119.1(3) . . . ? C64 C65 C70 122.7(3) . . . ? C66 C65 C70 118.2(3) . . . ? C65 C66 C67 121.9(3) . . . ? C66 C67 C68 118.1(3) . . . ? C66 C67 C71 120.6(3) . . . ? C68 C67 C71 121.3(3) . . . ? C67 C68 C69 122.3(3) . . . ? C68 C69 C70 118.1(3) . . . ? C68 C69 C74 120.2(3) . . . ? C70 C69 C74 121.7(3) . . . ? O8 C70 C65 121.4(3) . . . ? O8 C70 C69 117.1(3) . . . ? C65 C70 C69 121.3(3) . . . ? C67 C71 C72 114.6(3) . . . ? C71 C72 C73 126.5(5) . . . ? C69 C74 C75 112.7(2) . . . ? C74 C75 C76 120.3(3) . . . ? C74 C75 C80 121.8(3) . . . ? C76 C75 C80 117.8(3) . . . ? C75 C76 C77 122.7(3) . . . ? C76 C77 C78 117.5(3) . . . ? C76 C77 C81 123.0(3) . . . ? C78 C77 C81 119.5(3) . . . ? C77 C78 C79 121.8(3) . . . ? C78 C79 C80 118.5(3) . . . ? C78 C79 C84 120.7(3) . . . ? C80 C79 C84 120.9(3) . . . ? O4 C80 C75 121.4(3) . . . ? O4 C80 C79 116.9(3) . . . ? C75 C80 C79 121.3(3) . . . ? C77 C81 C82 119.0(4) . . . ? C77 C81 C82A 121.1(5) . . . ? C82 C81 C82A 51.5(5) . . . ? C81 C82 C82A 59.6(6) . . . ? C81 C82 C83 127.1(7) . . . ? C82A C82 C83 70.1(6) . . . ? C81 C82A C82 68.9(6) . . . ? C81 C82A C83 125.9(8) . . . ? C82 C82A C83 59.6(6) . . . ? C82 C83 C82A 50.3(5) . . . ? C46 C84 C79 116.8(3) . . . ? CL1 C85 CL2 112.8(2) . . . ? CL3 C86 CL4 112.3(2) . . . ? CL5 C87 CL6 113.0(5) . . . ? CL5 C87 Cl5a 20.9(2) . . . ? CL5 C87 Cl6a 139.7(6) . . . ? CL6 C87 Cl5a 93.2(4) . . . ? CL6 C87 Cl6a 26.9(3) . . . ? Cl5a C87 Cl6a 119.3(5) . . . ? data_st489 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C100 H108 O8 Si2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C100 H108 O8 Si2' _chemical_formula_weight 1494.14 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 12.7530(6) _cell_length_b 14.5330(6) _cell_length_c 25.010(1) _cell_angle_alpha 100.191(5) _cell_angle_beta 98.867(5) _cell_angle_gamma 106.834(5) _cell_volume 4261.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.16 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 57465 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.8 deg 1 scans of 90 sec per frame. Data collection was divided into 5 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.50 Omega = 180.00 Kappa = 0.00 101 frames Set 2 Theta = -4.30 Kappa = -173.00 Phi = 0.00 24 frames Set 3 Theta = -8.40 Kappa = 174.00 Phi = 0.00 38 frames Set 4 Theta = 7.40 Kappa = -41.00 Phi = 0.00 56 frames Set 5 Theta = -6.40 Kappa = -68.00 Phi = 0.00 61 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 57465 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.57 _reflns_number_total 19263 _reflns_number_gt 10123 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10123 _refine_ls_number_parameters 949 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.163 _refine_ls_R_factor_gt 0.088 _refine_ls_wR_factor_all 0.240 _refine_ls_wR_factor_ref 0.110 _refine_ls_goodness_of_fit_all 2.400 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_shift/su_max 0.016 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.383 _refine_diff_density_min -0.096 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol SI1 1.08480(9) 0.12691(9) 0.77928(5) 0.0305(5) 1.000 Uani ? ? Si O1 1.2034(2) 0.1054(2) 0.7959(1) 0.039(1) 1.000 Uani ? ? O O2 1.1013(2) 0.2412(2) 0.8049(1) 0.030(1) 1.000 Uani ? ? O O3 1.0417(2) 0.0998(2) 0.7124(1) 0.034(1) 1.000 Uani ? ? O O4 0.9911(2) 0.0557(2) 0.8029(1) 0.035(1) 1.000 Uani ? ? O SI2 0.77343(9) 0.09089(8) 0.77056(5) 0.0274(5) 1.000 Uani ? ? Si O5 0.8720(2) 0.1646(2) 0.7511(1) 0.030(1) 1.000 Uani ? ? O O6 0.6564(2) 0.1133(2) 0.7527(1) 0.035(1) 1.000 Uani ? ? O O7 0.7612(2) -0.0209(2) 0.7423(1) 0.036(2) 1.000 Uani ? ? O O8 0.8100(2) 0.1130(2) 0.8377(1) 0.034(1) 1.000 Uani ? ? O C1 1.3593(3) 0.2575(3) 0.8279(2) 0.038(2) 1.000 Uani ? ? C C2 1.4545(3) 0.3221(3) 0.8180(2) 0.039(2) 1.000 Uani ? ? C C3 1.4906(3) 0.3053(4) 0.7685(2) 0.043(2) 1.000 Uani ? ? C C4 1.4243(4) 0.2221(4) 0.7272(2) 0.049(2) 1.000 Uani ? ? C C5 1.3270(3) 0.1563(3) 0.7345(2) 0.043(2) 1.000 Uani ? ? C C6 1.2978(3) 0.1734(3) 0.7861(2) 0.038(2) 1.000 Uani ? ? C C7 1.5993(4) 0.3778(4) 0.7595(2) 0.050(3) 1.000 Uani ? ? C C8 1.6350(4) 0.3343(5) 0.7074(3) 0.069(3) 1.000 Uani ? ? C C9 1.5807(5) 0.4742(5) 0.7546(3) 0.084(4) 1.000 Uani ? ? C C10 1.6963(4) 0.3974(5) 0.8086(3) 0.061(3) 1.000 Uani ? ? C C11 1.2504(4) 0.0720(4) 0.6872(2) 0.049(2) 1.000 Uani ? ? C C12 1.1707(4) 0.1063(3) 0.6500(2) 0.043(2) 1.000 Uani ? ? C C13 1.1970(4) 0.1286(4) 0.6004(2) 0.057(3) 1.000 Uani ? ? C C14 1.1271(4) 0.1562(4) 0.5629(2) 0.057(3) 1.000 Uani ? ? C C15 1.0254(4) 0.1592(4) 0.5759(2) 0.045(2) 1.000 Uani ? ? C C16 0.9953(4) 0.1390(3) 0.6253(2) 0.037(2) 1.000 Uani ? ? C C17 1.0718(4) 0.1174(3) 0.6632(2) 0.036(2) 1.000 Uani ? ? C C18 1.1580(5) 0.1824(4) 0.5089(2) 0.070(3) 1.000 Uani ? ? C C19 1.2739(7) 0.1770(8) 0.5038(3) 0.281(5) 1.000 Uani ? ? C C20 1.1596(7) 0.2854(5) 0.5082(3) 0.083(4) 1.000 Uani ? ? C C21 1.070(1) 0.1129(8) 0.4597(3) 0.142(7) 1.000 Uani ? ? C C22 0.8818(4) 0.1422(3) 0.6363(2) 0.034(2) 1.000 Uani ? ? C C23 0.8952(3) 0.2401(3) 0.6745(2) 0.028(2) 1.000 Uani ? ? C C24 0.9159(3) 0.3260(3) 0.6545(2) 0.035(2) 1.000 Uani ? ? C C25 0.9451(3) 0.4199(3) 0.6893(2) 0.033(2) 1.000 Uani ? ? C C26 0.9579(3) 0.4258(3) 0.7465(2) 0.031(2) 1.000 Uani ? ? C C27 0.9357(3) 0.3420(3) 0.7683(2) 0.026(2) 1.000 Uani ? ? C C28 0.8975(3) 0.2500(3) 0.7313(2) 0.025(2) 1.000 Uani ? ? C C29 0.9652(4) 0.5116(3) 0.6647(2) 0.048(2) 1.000 Uani ? ? C C30 0.986(2) 0.6025(6) 0.7069(4) 0.132(8) 1.000 Uani ? ? C C31 1.0650(8) 0.5267(6) 0.6407(5) 0.366(5) 1.000 Uani ? ? C C32 0.868(1) 0.5011(6) 0.6215(4) 0.165(6) 1.000 Uani ? ? C C33 0.9530(3) 0.3508(3) 0.8309(2) 0.031(2) 1.000 Uani ? ? C C34 1.0740(3) 0.3783(3) 0.8624(2) 0.027(2) 1.000 Uani ? ? C C35 1.1162(3) 0.4616(3) 0.9064(2) 0.033(2) 1.000 Uani ? ? C C36 1.2223(4) 0.4894(4) 0.9409(2) 0.036(2) 1.000 Uani ? ? C C37 1.2848(4) 0.4265(4) 0.9301(2) 0.034(2) 1.000 Uani ? ? C C38 1.2476(3) 0.3409(3) 0.8867(2) 0.031(2) 1.000 Uani ? ? C C39 1.1420(3) 0.3191(3) 0.8520(2) 0.029(2) 1.000 Uani ? ? C C40 1.2656(4) 0.5837(4) 0.9879(2) 0.044(3) 1.000 Uani ? ? C C41 1.275(1) 0.6723(6) 0.9616(4) 0.103(7) 1.000 Uani ? ? C C42 1.3730(8) 0.5944(7) 1.0236(4) 0.159(6) 1.000 Uani ? ? C C43 1.1826(6) 0.5868(7) 1.0245(3) 0.092(5) 1.000 Uani ? ? C C44 1.3208(4) 0.2748(3) 0.8823(2) 0.038(2) 1.000 Uani ? ? C C45 0.5010(4) -0.0353(4) 0.7114(2) 0.042(2) 1.000 Uani ? ? C C46 0.3990(5) -0.1018(5) 0.7153(3) 0.054(3) 1.000 Uani ? ? C C47 0.3572(5) -0.0910(5) 0.7630(3) 0.060(3) 1.000 Uani ? ? C C48 0.4201(4) -0.0145(4) 0.8088(2) 0.057(3) 1.000 Uani ? ? C C49 0.5226(4) 0.0538(4) 0.8072(2) 0.042(2) 1.000 Uani ? ? C C50 0.5575(3) 0.0430(3) 0.7576(2) 0.035(2) 1.000 Uani ? ? C C51 0.2441(6) -0.1621(7) 0.7654(4) 0.101(5) 1.000 Uani ? ? C C52 0.2344(8) -0.2078(9) 0.8054(4) 0.134(7) 1.000 Uani ? ? C C53 0.1765(7) -0.2202(9) 0.8414(4) 0.116(6) 1.000 Uani ? ? C C54 0.5941(4) 0.1328(4) 0.8576(2) 0.048(2) 1.000 Uani ? ? C C55 0.6727(4) 0.0993(3) 0.8959(2) 0.036(2) 1.000 Uani ? ? C C56 0.6452(4) 0.0757(4) 0.9454(2) 0.047(2) 1.000 Uani ? ? C C57 0.7161(4) 0.0516(4) 0.9836(2) 0.048(3) 1.000 Uani ? ? C C58 0.8217(4) 0.0551(4) 0.9737(2) 0.043(2) 1.000 Uani ? ? C C59 0.8535(4) 0.0753(3) 0.9254(2) 0.032(2) 1.000 Uani ? ? C C60 0.7758(4) 0.0937(3) 0.8855(2) 0.031(2) 1.000 Uani ? ? C C61 0.6811(6) 0.0216(5) 1.0349(2) 0.082(3) 1.000 Uani ? ? C C62 0.6438(8) -0.1549(6) 0.9915(4) 0.111(5) 1.000 Uani ? ? C C63 0.6476(6) -0.0862(5) 1.0319(3) 0.119(4) 1.000 Uani ? ? C C64 0.9672(4) 0.0728(3) 0.9150(2) 0.035(2) 1.000 Uani ? ? C C65 0.9533(3) -0.0243(3) 0.8767(2) 0.032(2) 1.000 Uani ? ? C C66 0.9216(4) -0.1120(3) 0.8947(2) 0.041(2) 1.000 Uani ? ? C C67 0.8905(5) -0.2042(4) 0.8585(2) 0.049(3) 1.000 Uani ? ? C C68 0.8878(4) -0.2082(3) 0.8029(2) 0.045(2) 1.000 Uani ? ? C C69 0.9209(4) -0.1226(3) 0.7828(2) 0.040(2) 1.000 Uani ? ? C C70 0.9584(3) -0.0314(3) 0.8207(2) 0.032(2) 1.000 Uani ? ? C C71 0.8560(7) -0.2987(4) 0.8801(3) 0.073(4) 1.000 Uani ? ? C C72 0.9213(9) -0.2969(6) 0.9312(4) 0.116(5) 1.000 Uani ? ? C C73 0.893(1) -0.3053(6) 0.9783(3) 0.104(5) 1.000 Uani ? ? C C74 0.9073(4) -0.1318(3) 0.7202(2) 0.045(2) 1.000 Uani ? ? C C75 0.7869(4) -0.1617(3) 0.6885(2) 0.037(2) 1.000 Uani ? ? C C76 0.7406(5) -0.2506(4) 0.6479(2) 0.049(3) 1.000 Uani ? ? C C77 0.6335(5) -0.2777(4) 0.6142(2) 0.049(3) 1.000 Uani ? ? C C78 0.5748(5) -0.2114(4) 0.6195(2) 0.047(3) 1.000 Uani ? ? C C79 0.6169(4) -0.1208(4) 0.6599(2) 0.040(2) 1.000 Uani ? ? C C80 0.7202(4) -0.0999(3) 0.6962(2) 0.033(2) 1.000 Uani ? ? C C81 0.5841(7) -0.3774(5) 0.5715(3) 0.069(4) 1.000 Uani ? ? C C82 0.554(1) -0.467(1) 0.6030(6) 0.073(4) 0.500 Uiso ? ? C C83 0.404(3) -0.493(2) 0.573(1) 0.20(1) 0.500 Uiso ? ? C C84 0.5492(4) -0.0499(4) 0.6604(2) 0.047(3) 1.000 Uani ? ? C C85 1.3288(4) 0.5224(4) 0.7558(3) 0.088(3) 1.000 Uani ? ? C C86 1.3742(4) 0.5777(4) 0.7187(3) 0.082(3) 1.000 Uani ? ? C C87 1.4589(5) 0.6698(4) 0.7398(3) 0.081(3) 1.000 Uani ? ? C C88 1.4988(5) 0.7111(4) 0.7974(3) 0.088(3) 1.000 Uani ? ? C C89 1.4510(5) 0.6572(5) 0.8332(3) 0.094(3) 1.000 Uani ? ? C C90 1.3675(5) 0.5641(5) 0.8135(3) 0.097(3) 1.000 Uani ? ? C C91 1.2438(5) 0.4179(5) 0.7331(3) 0.087(4) 1.000 Uani ? ? C C92 1.5922(6) 0.8117(5) 0.8193(3) 0.096(4) 1.000 Uani ? ? C C93 1.213(1) 0.772(1) 0.5581(7) 0.200(6) 1.000 Uiso ? ? C C94 1.241(1) 0.8810(9) 0.5445(5) 0.157(5) 1.000 Uiso ? ? C C95 1.3120(9) 0.8886(8) 0.5065(4) 0.130(4) 1.000 Uiso ? ? C C96 1.350(1) 0.817(1) 0.4799(6) 0.169(5) 1.000 Uiso ? ? C C97 1.325(2) 0.711(1) 0.4915(8) 0.240(8) 1.000 Uiso ? ? C C98 1.263(1) 0.7222(9) 0.5274(5) 0.145(4) 1.000 Uiso ? ? C C99 1.129(1) 0.800(1) 0.6043(7) 0.224(7) 1.000 Uiso ? ? C C100 1.410(1) 0.824(1) 0.4432(7) 0.222(7) 1.000 Uiso ? ? C C82a 0.506(1) -0.446(1) 0.5907(6) 0.079(4) 0.500 Uiso ? ? C C83a 0.467(1) -0.535(1) 0.5915(7) 0.093(5) 0.500 Uiso ? ? C H1 1.4967 0.3800 0.8462 0.0531 1.000 Uiso calc C2 H H2 1.4464 0.2098 0.6928 0.0612 1.000 Uiso calc C4 H H3 1.7015 0.3805 0.7032 0.0911 1.000 Uiso calc C8 H H4 1.6488 0.2748 0.7114 0.0911 1.000 Uiso calc C8 H H5 1.5769 0.3209 0.6756 0.0911 1.000 Uiso calc C8 H H6 1.6472 0.5186 0.7492 0.1085 1.000 Uiso calc C9 H H7 1.5207 0.4625 0.7239 0.1085 1.000 Uiso calc C9 H H8 1.5626 0.5024 0.7878 0.1085 1.000 Uiso calc C9 H H9 1.7624 0.4418 0.8028 0.0883 1.000 Uiso calc C10 H H10 1.6787 0.4258 0.8419 0.0883 1.000 Uiso calc C10 H H11 1.7084 0.3369 0.8118 0.0883 1.000 Uiso calc C10 H H12 1.2077 0.0217 0.7022 0.0623 1.000 Uiso calc C11 H H13 1.2950 0.0462 0.6656 0.0623 1.000 Uiso calc C11 H H14 1.2660 0.1245 0.5921 0.0712 1.000 Uiso calc C13 H H15 0.9746 0.1756 0.5503 0.0595 1.000 Uiso calc C15 H H16 1.2900 0.1935 0.4702 0.2690 1.000 Uiso calc C19 H H17 1.3288 0.2223 0.5346 0.2690 1.000 Uiso calc C19 H H18 1.2751 0.1118 0.5035 0.2690 1.000 Uiso calc C19 H H19 1.1787 0.3008 0.4749 0.1111 1.000 Uiso calc C20 H H20 1.0875 0.2903 0.5100 0.1111 1.000 Uiso calc C20 H H21 1.2136 0.3304 0.5393 0.1111 1.000 Uiso calc C20 H H22 1.0884 0.1285 0.4263 0.2834 1.000 Uiso calc C21 H H23 1.0670 0.0468 0.4594 0.2834 1.000 Uiso calc C21 H H24 0.9989 0.1196 0.4623 0.2834 1.000 Uiso calc C21 H H25 0.8512 0.0900 0.6532 0.0456 1.000 Uiso calc C22 H H26 0.8325 0.1344 0.6020 0.0456 1.000 Uiso calc C22 H H27 0.9097 0.3203 0.6156 0.0431 1.000 Uiso calc C24 H H28 0.9826 0.4892 0.7713 0.0436 1.000 Uiso calc C26 H H29 0.9981 0.6571 0.6899 0.2830 1.000 Uiso calc C30 H H30 0.9232 0.5970 0.7236 0.2830 1.000 Uiso calc C30 H H31 1.0509 0.6123 0.7346 0.2830 1.000 Uiso calc C30 H H32 1.0762 0.5835 0.6257 0.3905 1.000 Uiso calc C31 H H33 1.1287 0.5359 0.6689 0.3905 1.000 Uiso calc C31 H H34 1.0548 0.4704 0.6120 0.3905 1.000 Uiso calc C31 H H35 0.8821 0.5584 0.6068 0.2646 1.000 Uiso calc C32 H H36 0.8554 0.4446 0.5925 0.2646 1.000 Uiso calc C32 H H37 0.8036 0.4935 0.6371 0.2646 1.000 Uiso calc C32 H H38 0.9121 0.2889 0.8368 0.0407 1.000 Uiso calc C33 H H39 0.9235 0.4000 0.8462 0.0407 1.000 Uiso calc C33 H H40 1.0702 0.5015 0.9133 0.0433 1.000 Uiso calc C35 H H41 1.3569 0.4425 0.9534 0.0494 1.000 Uiso calc C37 H H42 1.3022 0.7316 0.9900 0.1881 1.000 Uiso calc C41 H H43 1.3263 0.6740 0.9374 0.1881 1.000 Uiso calc C41 H H44 1.2037 0.6664 0.9409 0.1881 1.000 Uiso calc C41 H H45 1.3958 0.6538 1.0519 0.2501 1.000 Uiso calc C42 H H46 1.3646 0.5396 1.0403 0.2501 1.000 Uiso calc C42 H H47 1.4282 0.5969 1.0019 0.2501 1.000 Uiso calc C42 H H48 1.2118 0.6459 1.0531 0.1415 1.000 Uiso calc C43 H H49 1.1138 0.5853 1.0027 0.1415 1.000 Uiso calc C43 H H50 1.1699 0.5313 1.0407 0.1415 1.000 Uiso calc C43 H H51 1.3858 0.3041 0.9115 0.0517 1.000 Uiso calc C44 H H52 1.2793 0.2122 0.8872 0.0517 1.000 Uiso calc C44 H H53 0.3580 -0.1555 0.6845 0.0819 1.000 Uiso calc C46 H H54 0.3928 -0.0082 0.8420 0.0754 1.000 Uiso calc C48 H H55 0.2203 -0.2119 0.7317 0.1588 1.000 Uiso calc C51 H H56 0.1938 -0.1251 0.7663 0.1588 1.000 Uiso calc C51 H H57 0.2871 -0.2423 0.8084 0.2165 1.000 Uiso calc C52 H H58 0.1892 -0.2598 0.8665 0.1872 1.000 Uiso calc C53 H H59 0.1200 -0.1900 0.8435 0.1872 1.000 Uiso calc C53 H H60 0.5457 0.1546 0.8783 0.0580 1.000 Uiso calc C54 H H61 0.6381 0.1864 0.8452 0.0580 1.000 Uiso calc C54 H H62 0.5744 0.0764 0.9527 0.0590 1.000 Uiso calc C56 H H63 0.8735 0.0432 1.0010 0.0592 1.000 Uiso calc C58 H H64 0.6192 0.0431 1.0406 0.0997 1.000 Uiso calc C61 H H65 0.7425 0.0541 1.0658 0.0997 1.000 Uiso calc C61 H H66 0.6264 -0.1063 1.0639 0.1251 1.000 Uiso calc C63 H H67 0.6207 -0.2217 0.9945 0.1457 1.000 Uiso calc C62 H H68 0.6639 -0.1393 0.9583 0.1457 1.000 Uiso calc C62 H H69 1.0160 0.0801 0.9494 0.0490 1.000 Uiso calc C64 H H70 0.9984 0.1254 0.8984 0.0490 1.000 Uiso calc C64 H H71 0.9213 -0.1084 0.9330 0.0530 1.000 Uiso calc C66 H H72 0.8628 -0.2709 0.7774 0.0608 1.000 Uiso calc C68 H H73 0.8599 -0.3516 0.8529 0.1101 1.000 Uiso calc C71 H H74 0.7807 -0.3110 0.8842 0.1101 1.000 Uiso calc C71 H H75 0.9981 -0.2882 0.9313 0.1491 1.000 Uiso calc C72 H H76 0.9474 -0.3025 1.0096 0.1560 1.000 Uiso calc C73 H H77 0.8174 -0.3142 0.9815 0.1560 1.000 Uiso calc C73 H H78 0.9388 -0.1801 0.7058 0.0567 1.000 Uiso calc C74 H H79 0.9474 -0.0696 0.7143 0.0567 1.000 Uiso calc C74 H H80 0.7834 -0.2940 0.6432 0.0691 1.000 Uiso calc C76 H H81 0.5039 -0.2272 0.5952 0.0721 1.000 Uiso calc C78 H H82 0.5970 0.0126 0.6584 0.0676 1.000 Uiso calc C84 H H83 0.4890 -0.0752 0.6286 0.0676 1.000 Uiso calc C84 H 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 _atom_site_aniso_type_symbol SI1 0.0241(5) 0.0280(5) 0.0422(6) 0.0106(4) 0.0106(4) 0.0119(5) Si O1 0.028(1) 0.035(1) 0.061(2) 0.016(1) 0.015(1) 0.018(1) O O2 0.024(1) 0.029(1) 0.038(2) 0.010(1) 0.001(1) 0.005(1) O O3 0.031(1) 0.034(1) 0.039(2) 0.010(1) 0.012(1) 0.009(1) O O4 0.030(1) 0.031(1) 0.046(2) 0.010(1) 0.011(1) 0.016(1) O SI2 0.0238(5) 0.0254(5) 0.0341(6) 0.0069(4) 0.0055(4) 0.0099(4) Si O5 0.028(1) 0.028(1) 0.037(1) 0.009(1) 0.010(1) 0.013(1) O O6 0.025(1) 0.036(1) 0.048(2) 0.009(1) 0.005(1) 0.017(1) O O7 0.036(1) 0.026(1) 0.050(2) 0.008(1) -0.003(1) 0.006(1) O O8 0.030(1) 0.039(1) 0.034(1) 0.012(1) 0.011(1) 0.014(1) O C1 0.023(2) 0.043(2) 0.056(3) 0.019(1) 0.007(2) 0.019(2) C C2 0.023(2) 0.043(2) 0.058(3) 0.014(2) 0.002(2) 0.017(2) C C3 0.024(2) 0.048(2) 0.069(3) 0.018(2) 0.016(2) 0.025(2) C C4 0.033(2) 0.051(2) 0.068(3) 0.021(2) 0.022(2) 0.020(2) C C5 0.030(2) 0.041(2) 0.063(3) 0.020(2) 0.018(2) 0.013(2) C C6 0.024(2) 0.034(2) 0.066(3) 0.015(1) 0.013(2) 0.019(2) C C7 0.028(2) 0.053(3) 0.086(3) 0.017(2) 0.023(2) 0.029(2) C C8 0.043(3) 0.082(4) 0.092(4) 0.015(3) 0.033(2) 0.030(3) C C9 0.054(3) 0.071(3) 0.155(5) 0.031(2) 0.048(3) 0.061(3) C C10 0.031(2) 0.074(4) 0.102(4) 0.010(2) 0.019(3) 0.034(3) C C11 0.041(2) 0.041(2) 0.071(3) 0.021(2) 0.029(2) 0.009(2) C C12 0.042(2) 0.033(2) 0.056(3) 0.013(2) 0.024(2) 0.005(2) C C13 0.061(2) 0.041(3) 0.074(3) 0.020(2) 0.046(2) 0.013(2) C C14 0.071(3) 0.041(3) 0.062(3) 0.018(2) 0.043(2) 0.014(2) C C15 0.059(3) 0.036(2) 0.043(2) 0.013(2) 0.021(2) 0.007(2) C C16 0.044(2) 0.028(2) 0.041(2) 0.008(2) 0.018(2) 0.006(2) C C17 0.040(2) 0.026(2) 0.042(2) 0.011(2) 0.019(2) 0.006(2) C C18 0.094(3) 0.054(3) 0.067(3) 0.021(3) 0.052(2) 0.021(3) C C19 0.265(4) 0.324(7) 0.256(4) 0.236(4) 0.238(3) 0.245(4) C C20 0.118(5) 0.070(4) 0.071(4) 0.016(4) 0.037(3) 0.031(3) C C21 0.33(1) 0.138(8) 0.062(4) -0.104(7) 0.107(4) -0.037(5) C C22 0.034(2) 0.037(2) 0.030(2) 0.008(2) 0.004(2) 0.007(2) C C23 0.022(2) 0.030(2) 0.034(2) 0.009(1) 0.007(2) 0.008(2) C C24 0.031(2) 0.039(2) 0.034(2) 0.015(2) 0.008(2) 0.014(2) C C25 0.024(2) 0.031(2) 0.048(2) 0.010(1) 0.008(2) 0.017(2) C C26 0.026(2) 0.027(2) 0.044(2) 0.009(1) 0.003(2) 0.003(2) C C27 0.017(2) 0.029(2) 0.034(2) 0.008(1) 0.003(2) 0.006(2) C C28 0.018(2) 0.027(2) 0.033(2) 0.007(1) 0.007(1) 0.012(2) C C29 0.046(2) 0.037(2) 0.064(3) 0.015(2) 0.011(2) 0.027(2) C C30 0.48(2) 0.043(4) 0.111(7) 0.059(7) 0.03(1) 0.035(4) C C31 0.287(5) 0.262(4) 0.650(7) 0.225(4) 0.378(4) 0.391(4) C C32 0.202(8) 0.092(4) 0.242(6) -0.021(4) -0.123(5) 0.116(3) C C33 0.025(2) 0.032(2) 0.036(2) 0.012(1) 0.005(2) 0.003(2) C C34 0.024(2) 0.032(2) 0.026(2) 0.007(1) 0.003(2) 0.010(2) C C35 0.031(2) 0.036(2) 0.032(2) 0.009(2) 0.007(2) 0.006(2) C C36 0.036(2) 0.041(2) 0.031(2) 0.006(2) 0.008(2) 0.006(2) C C37 0.027(2) 0.046(2) 0.033(2) 0.001(2) -0.000(2) 0.012(2) C C38 0.023(2) 0.040(2) 0.033(2) 0.009(2) 0.005(2) 0.015(2) C C39 0.027(2) 0.030(2) 0.031(2) 0.007(1) 0.007(2) 0.011(2) C C40 0.042(3) 0.050(3) 0.040(3) 0.003(2) 0.001(2) -0.001(2) C C41 0.24(1) 0.052(5) 0.089(6) -0.013(6) 0.023(7) -0.010(5) C C42 0.123(5) 0.189(7) 0.175(7) 0.092(4) -0.097(5) -0.142(5) C C43 0.068(4) 0.129(6) 0.088(5) 0.023(4) -0.000(4) -0.048(5) C C44 0.025(2) 0.046(2) 0.048(3) 0.013(2) -0.002(2) 0.018(2) C C45 0.026(2) 0.052(2) 0.053(3) 0.007(2) -0.007(2) 0.024(2) C C46 0.035(3) 0.066(3) 0.070(4) -0.002(2) -0.013(3) 0.023(3) C C47 0.031(3) 0.079(4) 0.088(4) -0.002(3) 0.003(3) 0.039(3) C C48 0.034(2) 0.075(3) 0.072(3) 0.013(2) 0.018(2) 0.036(3) C C49 0.027(2) 0.049(2) 0.055(3) 0.015(2) 0.010(2) 0.022(2) C C50 0.019(2) 0.043(2) 0.054(3) 0.009(2) 0.001(2) 0.023(2) C C51 0.059(4) 0.132(6) 0.132(6) -0.039(4) 0.003(4) 0.053(5) C C52 0.090(5) 0.194(9) 0.140(7) -0.073(5) 0.010(5) 0.061(6) C C53 0.063(4) 0.22(1) 0.113(6) -0.026(5) 0.019(4) 0.068(6) C C54 0.039(2) 0.045(2) 0.062(3) 0.021(2) 0.025(2) 0.019(2) C C55 0.039(2) 0.027(2) 0.042(2) 0.010(2) 0.015(2) 0.004(2) C C56 0.052(2) 0.041(2) 0.050(3) 0.018(2) 0.026(2) 0.010(2) C C57 0.068(3) 0.045(3) 0.035(2) 0.019(2) 0.021(2) 0.009(2) C C58 0.062(3) 0.041(2) 0.032(2) 0.013(2) 0.008(2) 0.012(2) C C59 0.037(2) 0.027(2) 0.033(2) 0.005(2) 0.004(2) 0.004(2) C C60 0.036(2) 0.026(2) 0.032(2) 0.004(2) 0.010(2) 0.007(2) C C61 0.106(4) 0.098(4) 0.053(3) 0.050(3) 0.044(3) 0.034(3) C C62 0.151(6) 0.076(5) 0.121(5) 0.024(5) 0.068(4) 0.039(4) C C63 0.139(4) 0.110(4) 0.109(3) 0.082(3) 0.089(3) 0.079(3) C C64 0.037(2) 0.032(2) 0.039(2) 0.005(2) -0.001(2) 0.011(2) C C65 0.027(2) 0.031(2) 0.042(2) 0.007(2) -0.000(2) 0.013(2) C C66 0.045(2) 0.039(2) 0.041(2) 0.012(2) 0.006(2) 0.019(2) C C67 0.062(3) 0.035(2) 0.053(3) 0.013(2) 0.005(2) 0.022(2) C C68 0.059(3) 0.028(2) 0.055(3) 0.017(2) 0.007(2) 0.013(2) C C69 0.040(2) 0.037(2) 0.044(2) 0.019(2) 0.011(2) 0.016(2) C C70 0.026(2) 0.029(2) 0.044(2) 0.012(1) 0.005(2) 0.014(2) C C71 0.132(6) 0.039(3) 0.074(4) 0.016(3) 0.004(4) 0.028(3) C C72 0.163(7) 0.083(4) 0.116(5) 0.045(4) 0.030(5) 0.062(3) C C73 0.215(9) 0.068(4) 0.077(4) 0.029(5) 0.039(5) 0.041(3) C C74 0.052(2) 0.034(2) 0.051(3) 0.019(2) 0.019(2) 0.011(2) C C75 0.055(3) 0.029(2) 0.032(2) 0.005(2) 0.015(2) 0.008(2) C C76 0.081(3) 0.037(3) 0.040(2) 0.012(2) 0.026(2) 0.007(2) C C77 0.078(4) 0.047(3) 0.033(3) -0.005(3) 0.015(2) 0.001(2) C C78 0.056(3) 0.059(3) 0.031(2) -0.005(3) -0.001(2) 0.006(2) C C79 0.046(3) 0.042(2) 0.034(2) 0.001(2) 0.003(2) 0.015(2) C C80 0.045(2) 0.028(2) 0.029(2) 0.003(2) 0.006(2) 0.007(2) C C81 0.123(5) 0.050(4) 0.052(3) -0.019(4) 0.030(3) -0.019(3) C C84 0.042(3) 0.057(3) 0.043(3) 0.004(2) -0.012(2) 0.015(2) C C85 0.061(2) 0.098(3) 0.114(4) 0.058(2) 0.054(2) 0.070(3) C C86 0.063(2) 0.087(3) 0.101(3) 0.049(2) 0.047(2) 0.060(2) C C87 0.073(3) 0.082(3) 0.090(3) 0.050(2) 0.047(2) 0.055(2) C C88 0.082(3) 0.085(3) 0.097(4) 0.061(2) 0.051(2) 0.054(3) C C89 0.093(3) 0.097(4) 0.091(4) 0.058(3) 0.054(3) 0.056(3) C C90 0.096(3) 0.098(3) 0.096(3) 0.064(2) 0.064(2) 0.065(3) C C91 0.054(3) 0.089(4) 0.140(5) 0.032(3) 0.034(3) 0.063(3) C C92 0.099(4) 0.083(4) 0.108(5) 0.036(3) 0.036(4) 0.044(4) C # 10. MOLECULAR GEOMETRY 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 SI1 O1 1.638(3) . . ? SI1 O2 1.610(3) . . ? SI1 O3 1.617(3) . . ? SI1 O4 1.602(3) . . ? O1 C6 1.405(6) . . ? O2 C39 1.392(5) . . ? O3 C17 1.389(5) . . ? O4 C70 1.388(5) . . ? SI2 O5 1.600(3) . . ? SI2 O6 1.631(3) . . ? SI2 O7 1.606(3) . . ? SI2 O8 1.618(3) . . ? O5 C28 1.387(5) . . ? O6 C50 1.413(5) . . ? O7 C80 1.384(6) . . ? O8 C60 1.381(5) . . ? C1 C2 1.390(7) . . ? C1 C6 1.392(7) . . ? C1 C44 1.521(7) . . ? C2 C3 1.393(7) . . ? C3 C4 1.393(8) . . ? C3 C7 1.554(7) . . ? C4 C5 1.391(7) . . ? C5 C6 1.397(7) . . ? C5 C11 1.514(8) . . ? C7 C8 1.537(9) . . ? C7 C9 1.509(9) . . ? C7 C10 1.525(9) . . ? C11 C12 1.521(8) . . ? C12 C13 1.402(8) . . ? C12 C17 1.397(7) . . ? C13 C14 1.385(9) . . ? C14 C15 1.395(8) . . ? C14 C18 1.544(8) . . ? C15 C16 1.403(7) . . ? C16 C17 1.396(7) . . ? C16 C22 1.526(7) . . ? C18 C19 1.53(1) . . ? C18 C20 1.49(1) . . ? C18 C21 1.51(1) . . ? C22 C23 1.515(7) . . ? C23 C24 1.396(6) . . ? C23 C28 1.396(6) . . ? C24 C25 1.394(7) . . ? C25 C26 1.398(7) . . ? C25 C29 1.537(7) . . ? C26 C27 1.395(6) . . ? C27 C28 1.389(6) . . ? C27 C33 1.525(6) . . ? C29 C30 1.47(1) . . ? C29 C31 1.47(1) . . ? C29 C32 1.46(1) . . ? C33 C34 1.522(6) . . ? C34 C35 1.391(6) . . ? C34 C39 1.407(6) . . ? C35 C36 1.393(7) . . ? C36 C37 1.396(7) . . ? C36 C40 1.533(7) . . ? C37 C38 1.404(7) . . ? C38 C39 1.401(6) . . ? C38 C44 1.524(7) . . ? C40 C41 1.53(1) . . ? C40 C42 1.47(1) . . ? C40 C43 1.51(1) . . ? C45 C46 1.408(8) . . ? C45 C50 1.397(7) . . ? C45 C84 1.506(8) . . ? C46 C47 1.38(1) . . ? C47 C48 1.393(9) . . ? C47 C51 1.528(9) . . ? C48 C49 1.405(7) . . ? C49 C50 1.381(7) . . ? C49 C54 1.505(8) . . ? C51 C52 1.30(1) . . ? C52 C53 1.25(1) . . ? C54 C55 1.521(7) . . ? C55 C56 1.410(7) . . ? C55 C60 1.401(6) . . ? C56 C57 1.374(8) . . ? C57 C58 1.394(8) . . ? C57 C61 1.516(8) . . ? C58 C59 1.386(7) . . ? C59 C60 1.412(7) . . ? C59 C64 1.521(7) . . ? C61 C63 1.48(1) . . ? C62 C63 1.27(1) . . ? C64 C65 1.505(7) . . ? C65 C66 1.396(7) . . ? C65 C70 1.399(7) . . ? C66 C67 1.389(8) . . ? C67 C68 1.375(8) . . ? C67 C71 1.535(8) . . ? C68 C69 1.401(7) . . ? C69 C70 1.390(7) . . ? C69 C74 1.525(7) . . ? C71 C72 1.40(1) . . ? C72 C73 1.30(1) . . ? C74 C75 1.514(8) . . ? C75 C76 1.398(7) . . ? C75 C80 1.415(7) . . ? C76 C77 1.395(9) . . ? C77 C78 1.382(9) . . ? C77 C81 1.534(8) . . ? C78 C79 1.413(8) . . ? C79 C80 1.397(7) . . ? C79 C84 1.524(8) . . ? C81 C82 1.62(2) . . ? C81 C82a 1.40(2) . . ? C82 C83 1.84(4) . . ? C82 C83a 1.21(2) . . ? C83 C82a 1.24(3) . . ? C83 C83a 1.22(4) . . ? C85 C86 1.415(9) . . ? C85 C90 1.41(1) . . ? C85 C91 1.53(1) . . ? C86 C87 1.41(1) . . ? C87 C88 1.41(1) . . ? C88 C89 1.390(9) . . ? C88 C92 1.54(1) . . ? C89 C90 1.41(1) . . ? C93 C94 1.63(2) . . ? C93 C98 1.32(2) . . ? C93 C99 1.77(2) . . ? C94 C95 1.41(2) . . ? C95 C96 1.38(2) . . ? C96 C97 1.57(2) . . ? C96 C98 2.16(2) . . ? C96 C100 1.27(2) . . ? C97 C98 1.30(2) . . ? C82a C83a 1.25(2) . . ? 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 ? ? ? ? ? ? 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 O1 SI1 O2 109.8(2) . . . ? O1 SI1 O3 110.3(2) . . . ? O1 SI1 O4 108.8(2) . . . ? O2 SI1 O3 110.5(2) . . . ? O2 SI1 O4 110.7(2) . . . ? O3 SI1 O4 106.8(2) . . . ? SI1 O1 C6 115.2(3) . . . ? SI1 O2 C39 146.2(3) . . . ? SI1 O3 C17 144.0(3) . . . ? SI1 O4 C70 146.0(3) . . . ? O5 SI2 O6 109.7(2) . . . ? O5 SI2 O7 108.9(2) . . . ? O5 SI2 O8 106.4(2) . . . ? O6 SI2 O7 110.8(2) . . . ? O6 SI2 O8 109.9(2) . . . ? O7 SI2 O8 111.0(2) . . . ? SI2 O5 C28 142.0(3) . . . ? SI2 O6 C50 116.5(3) . . . ? SI2 O7 C80 148.9(3) . . . ? SI2 O8 C60 145.2(3) . . . ? C2 C1 C6 118.2(5) . . . ? C2 C1 C44 122.6(5) . . . ? C6 C1 C44 119.2(4) . . . ? C1 C2 C3 122.5(5) . . . ? C2 C3 C4 117.3(5) . . . ? C2 C3 C7 121.1(5) . . . ? C4 C3 C7 121.7(5) . . . ? C3 C4 C5 122.4(5) . . . ? C4 C5 C6 118.1(5) . . . ? C4 C5 C11 121.3(5) . . . ? C6 C5 C11 120.5(4) . . . ? O1 C6 C1 119.1(5) . . . ? O1 C6 C5 119.4(5) . . . ? C1 C6 C5 121.4(5) . . . ? C3 C7 C8 111.7(5) . . . ? C3 C7 C9 109.5(4) . . . ? C3 C7 C10 110.0(5) . . . ? C8 C7 C9 110.0(6) . . . ? C8 C7 C10 106.4(5) . . . ? C9 C7 C10 109.2(6) . . . ? C5 C11 C12 111.4(4) . . . ? C11 C12 C13 119.1(5) . . . ? C11 C12 C17 122.9(5) . . . ? C13 C12 C17 118.0(5) . . . ? C12 C13 C14 123.0(5) . . . ? C13 C14 C15 116.9(5) . . . ? C13 C14 C18 122.5(5) . . . ? C15 C14 C18 120.6(6) . . . ? C14 C15 C16 122.6(5) . . . ? C15 C16 C17 118.2(5) . . . ? C15 C16 C22 119.7(5) . . . ? C17 C16 C22 122.1(4) . . . ? O3 C17 C12 121.5(5) . . . ? O3 C17 C16 117.4(4) . . . ? C12 C17 C16 121.0(5) . . . ? C14 C18 C19 111.8(7) . . . ? C14 C18 C20 110.0(5) . . . ? C14 C18 C21 109.0(6) . . . ? C19 C18 C20 107.6(7) . . . ? C19 C18 C21 110(1) . . . ? C20 C18 C21 108.0(9) . . . ? C16 C22 C23 110.4(4) . . . ? C22 C23 C24 120.1(4) . . . ? C22 C23 C28 122.1(4) . . . ? C24 C23 C28 117.5(4) . . . ? C23 C24 C25 122.6(4) . . . ? C24 C25 C26 117.1(4) . . . ? C24 C25 C29 120.1(5) . . . ? C26 C25 C29 122.7(5) . . . ? C25 C26 C27 122.3(4) . . . ? C26 C27 C28 118.0(4) . . . ? C26 C27 C33 121.1(4) . . . ? C28 C27 C33 120.9(4) . . . ? O5 C28 C23 117.9(4) . . . ? O5 C28 C27 120.0(4) . . . ? C23 C28 C27 121.8(4) . . . ? C25 C29 C30 112.3(6) . . . ? C25 C29 C31 110.5(5) . . . ? C25 C29 C32 110.8(5) . . . ? C30 C29 C31 105(1) . . . ? C30 C29 C32 107(1) . . . ? C31 C29 C32 109(1) . . . ? C27 C33 C34 115.9(4) . . . ? C33 C34 C35 118.2(4) . . . ? C33 C34 C39 123.0(4) . . . ? C35 C34 C39 118.5(4) . . . ? C34 C35 C36 123.4(4) . . . ? C35 C36 C37 115.9(4) . . . ? C35 C36 C40 121.1(5) . . . ? C37 C36 C40 123.0(4) . . . ? C36 C37 C38 123.9(4) . . . ? C37 C38 C39 117.4(4) . . . ? C37 C38 C44 118.3(4) . . . ? C39 C38 C44 124.1(4) . . . ? O2 C39 C34 117.1(4) . . . ? O2 C39 C38 122.1(4) . . . ? C34 C39 C38 120.8(4) . . . ? C36 C40 C41 108.2(5) . . . ? C36 C40 C42 113.0(6) . . . ? C36 C40 C43 111.5(5) . . . ? C41 C40 C42 110.8(9) . . . ? C41 C40 C43 105.3(8) . . . ? C42 C40 C43 107.7(8) . . . ? C1 C44 C38 116.2(4) . . . ? C46 C45 C50 117.0(6) . . . ? C46 C45 C84 121.5(5) . . . ? C50 C45 C84 121.4(5) . . . ? C45 C46 C47 121.5(6) . . . ? C46 C47 C48 118.8(5) . . . ? C46 C47 C51 120.4(7) . . . ? C48 C47 C51 120.8(7) . . . ? C47 C48 C49 122.0(6) . . . ? C48 C49 C50 116.8(5) . . . ? C48 C49 C54 122.1(5) . . . ? C50 C49 C54 121.0(4) . . . ? O6 C50 C45 117.3(5) . . . ? O6 C50 C49 119.1(5) . . . ? C45 C50 C49 123.6(5) . . . ? C47 C51 C52 121.1(8) . . . ? C51 C52 C53 139(1) . . . ? C49 C54 C55 114.2(4) . . . ? C54 C55 C56 120.1(4) . . . ? C54 C55 C60 122.8(4) . . . ? C56 C55 C60 117.0(5) . . . ? C55 C56 C57 122.9(5) . . . ? C56 C57 C58 118.0(5) . . . ? C56 C57 C61 121.3(5) . . . ? C58 C57 C61 120.7(5) . . . ? C57 C58 C59 122.2(5) . . . ? C58 C59 C60 118.2(5) . . . ? C58 C59 C64 120.3(5) . . . ? C60 C59 C64 121.5(4) . . . ? O8 C60 C55 121.8(4) . . . ? O8 C60 C59 116.7(4) . . . ? C55 C60 C59 121.3(4) . . . ? C57 C61 C63 114.9(6) . . . ? C61 C63 C62 127.7(7) . . . ? C59 C64 C65 109.6(4) . . . ? C64 C65 C66 120.2(5) . . . ? C64 C65 C70 121.5(4) . . . ? C66 C65 C70 117.9(5) . . . ? C65 C66 C67 122.1(5) . . . ? C66 C67 C68 118.2(5) . . . ? C66 C67 C71 120.4(5) . . . ? C68 C67 C71 121.4(6) . . . ? C67 C68 C69 122.1(5) . . . ? C68 C69 C70 118.3(5) . . . ? C68 C69 C74 119.4(5) . . . ? C70 C69 C74 122.2(4) . . . ? O4 C70 C65 117.9(4) . . . ? O4 C70 C69 120.6(4) . . . ? C65 C70 C69 121.1(4) . . . ? C67 C71 C72 116.0(7) . . . ? C71 C72 C73 129(1) . . . ? C69 C74 C75 114.4(4) . . . ? C74 C75 C76 119.8(5) . . . ? C74 C75 C80 122.1(4) . . . ? C76 C75 C80 118.0(5) . . . ? C75 C76 C77 122.2(6) . . . ? C76 C77 C78 118.1(5) . . . ? C76 C77 C81 120.6(7) . . . ? C78 C77 C81 121.2(7) . . . ? C77 C78 C79 122.2(5) . . . ? C78 C79 C80 118.1(5) . . . ? C78 C79 C84 118.3(5) . . . ? C80 C79 C84 123.6(5) . . . ? O7 C80 C75 116.3(4) . . . ? O7 C80 C79 122.8(5) . . . ? C75 C80 C79 120.9(5) . . . ? C77 C81 C82 110.1(7) . . . ? C77 C81 C82a 111.1(8) . . . ? C82 C81 C82a 30.2(8) . . . ? C81 C82 C83 89(1) . . . ? C81 C82 C83a 125(1) . . . ? C83 C82 C83a 40(1) . . . ? C82 C83 C82a 20(1) . . . ? C82 C83 C83a 40(1) . . . ? C82a C83 C83a 61(2) . . . ? C45 C84 C79 114.2(5) . . . ? C86 C85 C90 118.3(8) . . . ? C86 C85 C91 120.1(8) . . . ? C90 C85 C91 121.6(7) . . . ? C85 C86 C87 119.8(7) . . . ? C86 C87 C88 122.1(6) . . . ? C87 C88 C89 117.4(8) . . . ? C87 C88 C92 120.9(6) . . . ? C89 C88 C92 121.7(8) . . . ? C88 C89 C90 121.9(8) . . . ? C85 C90 C89 120.5(6) . . . ? C94 C93 C98 106(1) . . . ? C94 C93 C99 91(1) . . . ? C98 C93 C99 161(1) . . . ? C93 C94 C95 109(1) . . . ? C94 C95 C96 128(1) . . . ? C95 C96 C97 123(1) . . . ? C95 C96 C98 86(1) . . . ? C95 C96 C100 128(1) . . . ? C97 C96 C98 36.7(9) . . . ? C97 C96 C100 108(1) . . . ? C98 C96 C100 145(1) . . . ? C96 C97 C98 96(1) . . . ? C93 C98 C96 108(1) . . . ? C93 C98 C97 154(1) . . . ? C96 C98 C97 46(1) . . . ? C81 C82a C83 134(2) . . . ? C81 C82a C83a 144(1) . . . ? C83 C82a C83a 58(1) . . . ? C82 C83a C83 98(2) . . . ? C82 C83a C82a 38(1) . . . ? C83 C83a C82a 60(1) . . . ? data_st568 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C102 H104 O8 Si2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C102 H104 O8 Si2' _chemical_formula_weight 1514.13 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 15.3269(5) _cell_length_b 17.4756(6) _cell_length_c 19.0824(6) _cell_angle_alpha 65.355(5) _cell_angle_beta 72.286(5) _cell_angle_gamma 64.786(5) _cell_volume 4152.84(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 18973 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.9 deg 1 scans of 120 sec per frame. Data collection was divided into 5 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 96 frames Set 2 Theta = -3.10 Kappa = 139.00 Phi = 0.00 20 frames Set 3 Theta = -2.20 Kappa = -169.00 Phi = 0.00 25 frames Set 4 Theta = -6.40 Kappa = -82.00 Phi = 0.00 26 frames Set 5 Theta = -6.40 Kappa = -85.00 Phi = 0.00 25 frames Friedel pairs were averaged. Internal R = 0.08 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18973 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 18973 _reflns_number_gt 11390 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+0.2' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 11390 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.117 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_all 0.342 _refine_ls_wR_factor_ref 0.065 _refine_ls_goodness_of_fit_all 5.930 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_shift/su_max 0.015 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.690 _refine_diff_density_min -0.094 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol Si1 0.64026(5) 0.61822(4) 0.29285(4) 0.0185(3) Uani ? ? Si O1 0.7271(1) 0.5781(1) 0.34410(9) 0.0208(7) Uani ? ? O C1 0.7640(2) 0.6074(1) 0.3829(1) 0.0190(9) Uani ? ? C C2 0.8645(2) 0.5936(1) 0.3645(1) 0.018(1) Uani ? ? C C3 0.9013(2) 0.6277(2) 0.3989(1) 0.025(1) Uani ? ? C C4 0.8429(2) 0.6747(2) 0.4505(1) 0.027(1) Uani ? ? C C5 0.7460(2) 0.6791(2) 0.4723(1) 0.026(1) Uani ? ? C C6 0.7053(2) 0.6441(2) 0.4412(1) 0.021(1) Uani ? ? C C7 0.8867(2) 0.7173(2) 0.4813(2) 0.038(1) Uani ? ? C C8 0.9553(3) 0.6443(2) 0.5369(2) 0.082(2) Uani ? ? C C9 0.9451(3) 0.7712(2) 0.4117(2) 0.087(2) Uani ? ? C C10 0.8093(2) 0.7837(2) 0.5191(2) 0.070(2) Uani ? ? C C11 0.5994(2) 0.6494(2) 0.4708(1) 0.024(1) Uani ? ? C C12 0.5307(2) 0.7326(2) 0.4203(1) 0.022(1) Uani ? ? C C13 0.5050(2) 0.7299(1) 0.3576(1) 0.022(1) Uani ? ? C O2 0.5338(1) 0.6475(1) 0.34682(9) 0.0224(7) Uani ? ? O C14 0.4528(2) 0.8070(2) 0.3034(1) 0.022(1) Uani ? ? C C15 0.4215(2) 0.8886(2) 0.3160(1) 0.024(1) Uani ? ? C C16 0.4418(2) 0.8947(2) 0.3799(1) 0.026(1) Uani ? ? C C17 0.4976(2) 0.8157(2) 0.4306(1) 0.026(1) Uani ? ? C C18 0.4073(2) 0.9837(2) 0.3956(2) 0.032(1) Uani ? ? C C19 0.4971(3) 1.0073(2) 0.3872(2) 0.058(2) Uani ? ? C C20 0.3401(2) 1.0619(2) 0.3386(2) 0.041(1) Uani ? ? C C21 0.3511(3) 0.9732(2) 0.4787(2) 0.046(1) Uani ? ? C C22 0.4274(2) 0.7993(2) 0.2368(1) 0.025(1) Uani ? ? C C23 0.5004(2) 0.7978(2) 0.1608(1) 0.022(1) Uani ? ? C C24 0.6019(2) 0.7532(1) 0.1537(1) 0.0189(9) Uani ? ? C O3 0.6504(1) 0.7063(1) 0.21898(9) 0.0180(6) Uani ? ? O C25 0.6588(2) 0.7561(1) 0.0793(1) 0.0210(9) Uani ? ? C C26 0.6109(2) 0.8021(2) 0.0144(1) 0.026(1) Uani ? ? C C27 0.5098(2) 0.8442(2) 0.0187(1) 0.027(1) Uani ? ? C C28 0.4574(2) 0.8410(2) 0.0928(1) 0.026(1) Uani ? ? C C29 0.4607(2) 0.8901(2) -0.0554(2) 0.034(1) Uani ? ? C C30 0.4882(3) 0.8207(3) -0.0957(2) 0.084(2) Uani ? ? C C31 0.3503(3) 0.9231(4) -0.0373(2) 0.077(2) Uani ? ? C C32 0.4990(3) 0.9615(3) -0.1125(2) 0.102(2) Uani ? ? C C33 0.7684(2) 0.7044(2) 0.0640(1) 0.021(1) Uani ? ? C C34 0.8366(2) 0.6979(1) 0.1109(1) 0.0184(9) Uani ? ? C C35 0.8661(2) 0.6220(1) 0.1758(1) 0.0190(9) Uani ? ? C O4 0.8285(1) 0.5546(1) 0.19592(9) 0.0215(7) Uani ? ? O C36 0.9220(2) 0.6179(1) 0.2234(1) 0.019(1) Uani ? ? C C37 0.9592(2) 0.6869(2) 0.1990(1) 0.024(1) Uani ? ? C C38 0.9377(2) 0.7616(2) 0.1320(1) 0.023(1) Uani ? ? C C39 0.8737(2) 0.7660(2) 0.0902(1) 0.019(1) Uani ? ? C C40 0.9834(2) 0.8346(2) 0.1053(2) 0.030(1) Uani ? ? C C41 1.0105(2) 0.8390(2) 0.1743(2) 0.052(1) Uani ? ? C C42 0.9124(2) 0.9274(2) 0.0663(2) 0.040(1) Uani ? ? C C43 1.0769(2) 0.8115(2) 0.0469(2) 0.047(1) Uani ? ? C C44 0.9321(2) 0.5491(2) 0.3046(1) 0.022(1) Uani ? ? C Si2 0.85769(5) 0.44888(4) 0.21465(4) 0.0183(2) Uani ? ? Si O5 0.7988(1) 0.4338(1) 0.16648(9) 0.0220(7) Uani ? ? O C45 0.7883(2) 0.4674(1) 0.0881(1) 0.023(1) Uani ? ? C C46 0.6941(2) 0.5196(2) 0.0691(1) 0.030(1) Uani ? ? C C47 0.6836(2) 0.5536(2) -0.0099(2) 0.038(1) Uani ? ? C C48 0.7614(2) 0.5365(2) -0.0688(2) 0.040(1) Uani ? ? C C49 0.8532(2) 0.4821(2) -0.0468(2) 0.037(1) Uani ? ? C C50 0.8690(2) 0.4467(2) 0.0308(1) 0.026(1) Uani ? ? C C51 0.7487(2) 0.5773(2) -0.1541(2) 0.051(2) Uani ? ? C C52 0.7556(2) 0.6700(2) -0.1935(2) 0.050(2) Uani ? ? C C53 0.7689(2) 0.7168(2) -0.1619(2) 0.050(2) Uani ? ? C C54 0.9741(2) 0.3962(2) 0.0445(1) 0.025(1) Uani ? ? C C55 0.9970(2) 0.3126(2) 0.1152(1) 0.022(1) Uani ? ? C C56 1.0000(2) 0.3185(2) 0.1851(1) 0.022(1) Uani ? ? C O6 0.9751(1) 0.4047(1) 0.18819(9) 0.0225(7) Uani ? ? O C57 1.0214(2) 0.2438(2) 0.2516(1) 0.021(1) Uani ? ? C C58 1.0414(2) 0.1599(2) 0.2470(1) 0.023(1) Uani ? ? C C59 1.0394(2) 0.1507(2) 0.1784(1) 0.024(1) Uani ? ? C C60 1.0178(2) 0.2278(2) 0.1133(1) 0.025(1) Uani ? ? C C61 1.0617(2) 0.0600(2) 0.1727(2) 0.031(1) Uani ? ? C C62 1.1659(2) 0.0182(2) 0.1402(2) 0.032(1) Uani ? ? C C63 1.2356(2) 0.0506(2) 0.1213(2) 0.045(2) Uani ? ? C C64 1.0189(2) 0.2549(2) 0.3269(1) 0.024(1) Uani ? ? C C65 0.9246(2) 0.2532(2) 0.3831(1) 0.024(1) Uani ? ? C C66 0.8354(2) 0.3229(1) 0.3708(1) 0.022(1) Uani ? ? C O7 0.8270(1) 0.4011(1) 0.30658(9) 0.0213(7) Uani ? ? O C67 0.7498(2) 0.3195(2) 0.4250(1) 0.025(1) Uani ? ? C C68 0.7556(2) 0.2432(2) 0.4912(2) 0.029(1) Uani ? ? C C69 0.8428(2) 0.1719(2) 0.5055(2) 0.030(1) Uani ? ? C C70 0.9260(2) 0.1782(2) 0.4513(1) 0.027(1) Uani ? ? C C71 0.8458(2) 0.0907(2) 0.5792(2) 0.040(2) Uani ? ? C C72 0.8292(2) 0.1072(2) 0.6534(2) 0.045(2) Uani ? ? C C73 0.8278(3) 0.1787(3) 0.6614(2) 0.056(2) Uani ? ? C C74 0.6528(2) 0.3958(2) 0.4125(1) 0.027(1) Uani ? ? C C75 0.6153(2) 0.4046(2) 0.3439(1) 0.024(1) Uani ? ? C C76 0.6148(2) 0.4745(1) 0.2731(1) 0.022(1) Uani ? ? C O8 0.6450(1) 0.5434(1) 0.26318(9) 0.0249(7) Uani ? ? O C77 0.5938(2) 0.4753(2) 0.2062(1) 0.026(1) Uani ? ? C C78 0.5669(2) 0.4051(2) 0.2136(2) 0.036(1) Uani ? ? C C79 0.5631(2) 0.3350(2) 0.2837(2) 0.035(1) Uani ? ? C C80 0.5881(2) 0.3355(2) 0.3475(2) 0.029(1) Uani ? ? C C81 0.5325(2) 0.2601(2) 0.2903(2) 0.048(1) Uani ? ? C C82 0.4263(2) 0.2794(2) 0.3096(2) 0.049(1) Uani ? ? C C83 0.3607(2) 0.3516(2) 0.3244(2) 0.051(2) Uani ? ? C C84 0.6043(2) 0.5466(2) 0.1286(1) 0.030(1) Uani ? ? C C85 0.7665(2) 0.0582(2) 0.2511(2) 0.036(1) Uani ? ? C C86 0.7812(2) 0.0615(2) 0.3185(2) 0.048(1) Uani ? ? C C87 0.7972(2) 0.1351(2) 0.3166(2) 0.057(2) Uani ? ? C C88 0.7986(2) 0.2056(2) 0.2482(2) 0.050(1) Uani ? ? C C89 0.7853(2) 0.2028(2) 0.1811(2) 0.048(2) Uani ? ? C C90 0.7697(2) 0.1296(2) 0.1823(2) 0.044(1) Uani ? ? C C91 0.7463(2) -0.0169(2) 0.2537(2) 0.036(1) Uani ? ? C C92 0.7287(2) -0.0782(2) 0.2564(2) 0.035(1) Uani ? ? C C93 0.7072(2) -0.1541(2) 0.2597(2) 0.042(1) Uani ? ? C C94 0.2912(2) 0.5963(2) 0.2441(2) 0.053(2) Uani ? ? C C95 0.3563(3) 0.6004(2) 0.2788(2) 0.057(2) Uani ? ? C C96 0.3407(3) 0.5838(2) 0.3583(3) 0.063(2) Uani ? ? C C97 0.2601(3) 0.5625(3) 0.4049(3) 0.058(2) Uani ? ? C C98 0.1950(3) 0.5557(3) 0.3719(3) 0.059(2) Uani ? ? C C99 0.2095(3) 0.5740(3) 0.2930(3) 0.062(2) Uani ? ? C C100 0.3093(3) 0.6131(2) 0.1597(3) 0.066(2) Uani ? ? C C101 0.3244(3) 0.6257(2) 0.0918(2) 0.072(2) Uani ? ? C C102 0.3404(4) 0.6431(3) 0.0093(3) 0.104(3) Uani ? ? C H1 0.9691 0.6186 0.3868 0.0325 Uiso calc C3 H H2 0.7056 0.7070 0.5100 0.0347 Uiso calc C5 H H3 0.9823 0.6704 0.5559 0.0994 Uiso calc C8 H H4 0.9207 0.6100 0.5793 0.0994 Uiso calc C8 H H5 1.0063 0.6064 0.5104 0.0994 Uiso calc C8 H H6 0.9722 0.7976 0.4304 0.0955 Uiso calc C9 H H7 0.9961 0.7321 0.3864 0.0955 Uiso calc C9 H H8 0.9028 0.8170 0.3758 0.0955 Uiso calc C9 H H9 0.8397 0.8080 0.5371 0.0802 Uiso calc C10 H H10 0.7692 0.8307 0.4820 0.0802 Uiso calc C10 H H11 0.7705 0.7542 0.5619 0.0802 Uiso calc C10 H H12 0.5824 0.6508 0.5226 0.0328 Uiso calc C11 H H13 0.5929 0.5979 0.4706 0.0328 Uiso calc C11 H H14 0.3852 0.9417 0.2800 0.0344 Uiso calc C15 H H15 0.5136 0.8186 0.4736 0.0344 Uiso calc C17 H H16 0.4761 1.0621 0.3969 0.0730 Uiso calc C19 H H17 0.5381 0.9607 0.4238 0.0730 Uiso calc C19 H H18 0.5322 1.0135 0.3359 0.0730 Uiso calc C19 H H19 0.3207 1.1151 0.3504 0.0584 Uiso calc C20 H H20 0.3740 1.0701 0.2867 0.0584 Uiso calc C20 H H21 0.2839 1.0488 0.3435 0.0584 Uiso calc C20 H H22 0.3298 1.0279 0.4884 0.0631 Uiso calc C21 H H23 0.2961 0.9582 0.4841 0.0631 Uiso calc C21 H H24 0.3925 0.9268 0.5151 0.0631 Uiso calc C21 H H25 0.3697 0.8488 0.2226 0.0340 Uiso calc C22 H H26 0.4139 0.7451 0.2568 0.0340 Uiso calc C22 H H27 0.6491 0.8049 -0.0357 0.0345 Uiso calc C26 H H28 0.3886 0.8698 0.0977 0.0364 Uiso calc C28 H H29 0.4582 0.8485 -0.1413 0.1047 Uiso calc C30 H H30 0.5570 0.7983 -0.1098 0.1047 Uiso calc C30 H H31 0.4662 0.7726 -0.0609 0.1047 Uiso calc C30 H H32 0.3239 0.9506 -0.0846 0.1358 Uiso calc C31 H H33 0.3292 0.8738 -0.0047 0.1358 Uiso calc C31 H H34 0.3287 0.9656 -0.0114 0.1358 Uiso calc C31 H H35 0.4684 0.9891 -0.1577 0.1394 Uiso calc C32 H H36 0.4859 1.0052 -0.0898 0.1394 Uiso calc C32 H H37 0.5675 0.9361 -0.1267 0.1394 Uiso calc C32 H H38 0.7906 0.7319 0.0107 0.0279 Uiso calc C33 H H39 0.7752 0.6447 0.0725 0.0279 Uiso calc C33 H H40 1.0009 0.6827 0.2295 0.0303 Uiso calc C37 H H41 0.8548 0.8176 0.0458 0.0282 Uiso calc C39 H H42 1.0384 0.8844 0.1561 0.0619 Uiso calc C41 H H43 0.9535 0.8526 0.2112 0.0619 Uiso calc C41 H H44 1.0563 0.7828 0.1985 0.0619 Uiso calc C41 H H45 0.9420 0.9712 0.0504 0.0549 Uiso calc C42 H H46 0.8965 0.9271 0.0220 0.0549 Uiso calc C42 H H47 0.8545 0.9413 0.1023 0.0549 Uiso calc C42 H H48 1.1060 0.8559 0.0299 0.0601 Uiso calc C43 H H49 1.1214 0.7546 0.0715 0.0601 Uiso calc C43 H H50 1.0610 0.8099 0.0033 0.0601 Uiso calc C43 H H51 0.9147 0.5008 0.3094 0.0284 Uiso calc C44 H H52 0.9976 0.5269 0.3132 0.0284 Uiso calc C44 H H53 0.6205 0.5901 -0.0238 0.0484 Uiso calc C47 H H54 0.9070 0.4686 -0.0860 0.0491 Uiso calc C49 H H55 0.6863 0.5810 -0.1574 0.0662 Uiso calc C51 H H56 0.7980 0.5390 -0.1810 0.0662 Uiso calc C51 H H57 0.7498 0.6972 -0.2474 0.0662 Uiso calc C52 H H58 0.7721 0.7748 -0.1925 0.0669 Uiso calc C53 H H59 0.7752 0.6929 -0.1082 0.0669 Uiso calc C53 H H60 0.9968 0.4369 0.0483 0.0373 Uiso calc C54 H H61 1.0100 0.3791 -0.0001 0.0373 Uiso calc C54 H H62 1.0567 0.1079 0.2917 0.0335 Uiso calc C58 H H63 1.0172 0.2222 0.0660 0.0333 Uiso calc C60 H H64 1.0209 0.0673 0.1399 0.0415 Uiso calc C61 H H65 1.0476 0.0207 0.2235 0.0415 Uiso calc C61 H H66 1.1827 -0.0371 0.1326 0.0470 Uiso calc C62 H H67 1.2996 0.0190 0.1011 0.0635 Uiso calc C63 H H68 1.2223 0.1057 0.1279 0.0635 Uiso calc C63 H H69 1.0260 0.3107 0.3148 0.0326 Uiso calc C64 H H70 1.0718 0.2075 0.3517 0.0326 Uiso calc C64 H H71 0.6981 0.2397 0.5277 0.0396 Uiso calc C68 H H72 0.9861 0.1301 0.4606 0.0383 Uiso calc C70 H H73 0.9082 0.0459 0.5750 0.0612 Uiso calc C71 H H74 0.7969 0.0694 0.5820 0.0612 Uiso calc C71 H H75 0.8184 0.0608 0.7002 0.0669 Uiso calc C72 H H76 0.8165 0.1820 0.7120 0.0772 Uiso calc C73 H H77 0.8382 0.2271 0.6165 0.0772 Uiso calc C73 H H78 0.6612 0.4503 0.4030 0.0365 Uiso calc C74 H H79 0.6064 0.3846 0.4581 0.0365 Uiso calc C74 H H80 0.5507 0.4050 0.1693 0.0436 Uiso calc C78 H H81 0.5868 0.2874 0.3953 0.0421 Uiso calc C80 H H82 0.5627 0.2076 0.3301 0.0621 Uiso calc C81 H H83 0.5546 0.2496 0.2419 0.0621 Uiso calc C81 H H84 0.4032 0.2359 0.3116 0.0618 Uiso calc C82 H H85 0.2934 0.3585 0.3363 0.0654 Uiso calc C83 H H86 0.3804 0.3969 0.3231 0.0654 Uiso calc C83 H H87 0.5480 0.5664 0.1057 0.0375 Uiso calc C84 H H88 0.6065 0.5950 0.1381 0.0375 Uiso calc C84 H H89 0.7802 0.0130 0.3660 0.0609 Uiso calc C86 H H90 0.8071 0.1366 0.3628 0.0685 Uiso calc C87 H H91 0.8088 0.2561 0.2471 0.0638 Uiso calc C88 H H92 0.7869 0.2513 0.1337 0.0643 Uiso calc C89 H H93 0.7610 0.1284 0.1357 0.0556 Uiso calc C90 H H94 0.6441 -0.1331 0.2464 0.0571 Uiso calc C93 H H95 0.7545 -0.1818 0.2239 0.0571 Uiso calc C93 H H96 0.7091 -0.1966 0.3110 0.0571 Uiso calc C93 H H97 0.4123 0.6147 0.2474 0.0800 Uiso calc C95 H H98 0.3857 0.5872 0.3809 0.0888 Uiso calc C96 H H99 0.2489 0.5525 0.4593 0.0921 Uiso calc C97 H H100 0.1409 0.5386 0.4041 0.0921 Uiso calc C98 H H101 0.1636 0.5715 0.2707 0.0928 Uiso calc C99 H H102 0.3967 0.5970 -0.0038 0.1310 Uiso calc C102 H H103 0.2852 0.6447 -0.0049 0.1310 Uiso calc C102 H H104 0.3498 0.6993 -0.0179 0.1310 Uiso calc C102 H 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 _atom_site_aniso_type_symbol Si1 0.0203(3) 0.0158(2) 0.0197(3) -0.0065(2) -0.0023(2) -0.0061(2) Si O1 0.0228(7) 0.0179(6) 0.0220(7) -0.0063(5) -0.0040(5) -0.0073(5) O C1 0.026(1) 0.0164(9) 0.0164(9) -0.0081(7) -0.0072(7) -0.0017(7) C C2 0.027(1) 0.0138(9) 0.016(1) -0.0062(7) -0.0048(8) -0.0007(7) C C3 0.022(1) 0.024(1) 0.027(1) -0.0060(7) -0.0068(8) -0.0079(8) C C4 0.030(1) 0.024(1) 0.026(1) -0.0068(8) -0.0105(8) -0.0081(7) C C5 0.032(1) 0.026(1) 0.020(1) -0.0040(8) -0.0059(9) -0.0105(7) C C6 0.027(1) 0.019(1) 0.018(1) -0.0062(8) -0.0042(8) -0.0031(7) C C7 0.037(1) 0.036(1) 0.040(1) -0.0091(8) -0.0111(9) -0.0206(8) C C8 0.089(2) 0.058(2) 0.107(2) 0.002(1) -0.069(1) -0.041(1) C C9 0.097(2) 0.093(1) 0.074(2) -0.069(1) 0.005(1) -0.043(1) C C10 0.058(2) 0.067(1) 0.090(2) -0.023(1) -0.004(1) -0.0560(9) C C11 0.028(1) 0.026(1) 0.019(1) -0.0089(8) -0.0004(9) -0.0081(8) C C12 0.020(1) 0.023(1) 0.021(1) -0.0089(7) 0.0032(8) -0.0075(7) C C13 0.020(1) 0.0206(9) 0.024(1) -0.0090(7) 0.0052(8) -0.0112(7) C O2 0.0216(7) 0.0210(6) 0.0250(7) -0.0083(5) 0.0015(6) -0.0091(5) O C14 0.018(1) 0.025(1) 0.023(1) -0.0053(8) 0.0015(8) -0.0098(8) C C15 0.024(1) 0.022(1) 0.027(1) -0.0044(8) -0.0009(9) -0.0078(8) C C16 0.027(1) 0.024(1) 0.027(1) -0.0086(8) 0.0037(9) -0.0111(8) C C17 0.028(1) 0.031(1) 0.022(1) -0.0100(8) 0.0012(9) -0.0130(7) C C18 0.038(1) 0.024(1) 0.036(1) -0.0069(9) 0.000(1) -0.0155(8) C C19 0.059(2) 0.043(1) 0.079(2) -0.021(1) -0.008(1) -0.030(1) C C20 0.055(2) 0.025(1) 0.049(2) -0.009(1) -0.001(1) -0.017(1) C C21 0.062(2) 0.037(1) 0.044(1) -0.007(1) 0.000(1) -0.0264(9) C C22 0.022(1) 0.028(1) 0.026(1) -0.0053(8) -0.0031(9) -0.0103(8) C C23 0.024(1) 0.0199(9) 0.023(1) -0.0059(7) -0.0034(8) -0.0085(7) C C24 0.023(1) 0.0136(8) 0.021(1) -0.0062(7) -0.0050(8) -0.0053(7) C O3 0.0204(7) 0.0158(6) 0.0181(7) -0.0048(5) -0.0049(5) -0.0037(5) O C25 0.025(1) 0.0168(9) 0.022(1) -0.0084(7) -0.0036(8) -0.0064(7) C C26 0.030(1) 0.027(1) 0.021(1) -0.0082(8) -0.0034(9) -0.0082(8) C C27 0.029(1) 0.027(1) 0.024(1) -0.0048(8) -0.0092(9) -0.0058(8) C C28 0.021(1) 0.027(1) 0.033(1) -0.0006(8) -0.0067(9) -0.0131(8) C C29 0.033(1) 0.046(1) 0.026(1) -0.004(1) -0.013(1) -0.008(1) C C30 0.078(2) 0.098(2) 0.076(2) -0.005(2) -0.039(1) -0.046(1) C C31 0.046(2) 0.184(4) 0.054(2) 0.009(2) -0.028(1) -0.050(2) C C32 0.141(2) 0.111(3) 0.069(2) -0.079(2) -0.076(2) 0.049(2) C C33 0.025(1) 0.0195(9) 0.018(1) -0.0071(7) -0.0037(8) -0.0052(7) C C34 0.0172(9) 0.0192(9) 0.0187(9) -0.0048(7) 0.0013(8) -0.0097(7) C C35 0.0184(9) 0.0183(9) 0.021(1) -0.0080(7) 0.0032(8) -0.0097(7) C O4 0.0239(7) 0.0168(6) 0.0249(7) -0.0076(5) -0.0029(6) -0.0081(5) O C36 0.018(1) 0.0193(9) 0.020(1) -0.0038(7) -0.0005(8) -0.0083(7) C C37 0.020(1) 0.026(1) 0.026(1) -0.0086(7) -0.0045(8) -0.0089(7) C C38 0.026(1) 0.0232(9) 0.021(1) -0.0105(7) -0.0003(8) -0.0081(7) C C39 0.022(1) 0.0164(9) 0.019(1) -0.0055(7) -0.0005(8) -0.0029(7) C C40 0.032(1) 0.030(1) 0.027(1) -0.0179(8) -0.0013(9) -0.0064(8) C C41 0.071(1) 0.042(1) 0.048(1) -0.0406(8) -0.012(1) -0.0084(9) C C42 0.049(1) 0.026(1) 0.051(2) -0.0212(9) -0.010(1) -0.003(1) C C43 0.039(1) 0.049(1) 0.053(2) -0.0277(9) 0.008(1) -0.017(1) C C44 0.022(1) 0.0181(9) 0.025(1) -0.0054(7) -0.0075(8) -0.0056(7) C Si2 0.0206(3) 0.0155(2) 0.0192(3) -0.0069(2) -0.0014(2) -0.0063(2) Si O5 0.0241(7) 0.0216(6) 0.0204(7) -0.0086(5) -0.0030(6) -0.0078(5) O C45 0.034(1) 0.0168(9) 0.022(1) -0.0096(7) -0.0073(8) -0.0043(7) C C46 0.035(1) 0.026(1) 0.029(1) -0.0102(8) -0.0088(9) -0.0100(8) C C47 0.042(1) 0.034(1) 0.037(1) -0.0096(9) -0.017(1) -0.0100(9) C C48 0.055(1) 0.039(1) 0.029(1) -0.017(1) -0.014(1) -0.0088(9) C C49 0.047(1) 0.040(1) 0.027(1) -0.015(1) -0.003(1) -0.0133(9) C C50 0.038(1) 0.021(1) 0.023(1) -0.0080(8) -0.0048(9) -0.0081(7) C C51 0.067(2) 0.055(2) 0.036(1) -0.025(1) -0.017(1) -0.009(1) C C52 0.056(2) 0.061(2) 0.036(1) -0.028(1) -0.014(1) -0.003(1) C C53 0.045(2) 0.053(2) 0.051(2) -0.018(1) -0.004(1) -0.013(1) C C54 0.033(1) 0.024(1) 0.021(1) -0.0083(9) 0.004(1) -0.0071(8) C C55 0.022(1) 0.022(1) 0.023(1) -0.0059(8) 0.0015(9) -0.0073(8) C C56 0.019(1) 0.0193(9) 0.028(1) -0.0059(7) 0.0006(8) -0.0102(7) C O6 0.0218(7) 0.0187(6) 0.0281(7) -0.0062(5) -0.0008(6) -0.0102(5) O C57 0.019(1) 0.022(1) 0.023(1) -0.0042(7) -0.0025(8) -0.0081(7) C C58 0.024(1) 0.020(1) 0.025(1) -0.0043(8) -0.0031(9) -0.0040(8) C C59 0.024(1) 0.020(1) 0.028(1) -0.0049(8) -0.0011(9) -0.0107(8) C C60 0.028(1) 0.026(1) 0.022(1) -0.0068(8) -0.0005(9) -0.0110(7) C C61 0.040(1) 0.023(1) 0.033(1) -0.0091(8) -0.009(1) -0.0084(8) C C62 0.047(1) 0.021(1) 0.034(1) -0.005(1) -0.003(1) -0.0123(9) C C63 0.042(2) 0.036(1) 0.059(2) -0.003(1) 0.003(1) -0.025(1) C C64 0.024(1) 0.022(1) 0.025(1) -0.0030(8) -0.0065(9) -0.0069(8) C C65 0.029(1) 0.024(1) 0.021(1) -0.0090(7) -0.0061(8) -0.0079(7) C C66 0.031(1) 0.0196(9) 0.0172(9) -0.0110(7) -0.0060(8) -0.0045(7) C O7 0.0255(7) 0.0180(7) 0.0211(7) -0.0069(5) -0.0024(6) -0.0047(5) O C67 0.029(1) 0.0224(9) 0.024(1) -0.0103(7) -0.0019(9) -0.0081(7) C C68 0.037(1) 0.028(1) 0.023(1) -0.0150(8) 0.001(1) -0.0056(8) C C69 0.045(1) 0.025(1) 0.023(1) -0.0133(9) -0.007(1) -0.0020(9) C C70 0.035(1) 0.023(1) 0.026(1) -0.0044(9) -0.0100(9) -0.0058(8) C C71 0.055(2) 0.034(1) 0.033(2) -0.014(1) -0.005(1) 0.003(1) C C72 0.049(2) 0.053(2) 0.034(2) -0.017(1) -0.008(1) 0.003(1) C C73 0.059(2) 0.074(2) 0.041(2) -0.025(1) -0.007(1) -0.014(1) C C74 0.030(1) 0.026(1) 0.025(1) -0.0119(8) 0.005(1) -0.0092(8) C C75 0.019(1) 0.022(1) 0.034(1) -0.0060(7) 0.0022(9) -0.0128(8) C C76 0.0175(9) 0.0176(9) 0.034(1) -0.0058(7) -0.0016(8) -0.0129(7) C O8 0.0264(7) 0.0208(6) 0.0279(7) -0.0110(5) -0.0029(6) -0.0097(5) O C77 0.019(1) 0.025(1) 0.037(1) -0.0060(7) -0.0040(9) -0.0138(8) C C78 0.025(1) 0.035(1) 0.052(1) -0.0076(8) -0.0101(9) -0.0242(8) C C79 0.027(1) 0.028(1) 0.058(1) -0.0121(8) -0.003(1) -0.0187(9) C C80 0.026(1) 0.021(1) 0.046(1) -0.0093(8) 0.001(1) -0.0098(9) C C81 0.042(1) 0.034(1) 0.077(2) -0.0192(9) -0.006(1) -0.023(1) C C82 0.047(1) 0.036(1) 0.069(2) -0.0229(8) -0.016(1) -0.013(1) C C83 0.045(1) 0.056(2) 0.054(2) -0.024(1) -0.011(1) -0.012(1) C C84 0.028(1) 0.027(1) 0.036(1) -0.0048(8) -0.0123(8) -0.0139(8) C C85 0.030(1) 0.036(1) 0.043(1) -0.0138(9) 0.003(1) -0.0184(9) C C86 0.054(2) 0.047(1) 0.042(1) -0.023(1) 0.001(1) -0.018(1) C C87 0.053(2) 0.060(1) 0.060(2) -0.023(1) -0.003(1) -0.033(1) C C88 0.039(1) 0.045(1) 0.073(2) -0.0196(9) -0.002(1) -0.028(1) C C89 0.042(1) 0.043(1) 0.060(2) -0.022(1) -0.007(1) -0.008(1) C C90 0.043(1) 0.044(1) 0.046(1) -0.0206(9) -0.004(1) -0.015(1) C C91 0.036(1) 0.038(1) 0.034(1) -0.0153(9) 0.004(1) -0.0145(9) C C92 0.035(1) 0.036(1) 0.034(1) -0.0134(9) 0.004(1) -0.0125(9) C C93 0.045(1) 0.033(1) 0.051(2) -0.017(1) 0.001(1) -0.014(1) C C94 0.041(2) 0.034(1) 0.110(3) -0.006(1) -0.020(2) -0.022(1) C C95 0.044(2) 0.045(2) 0.092(2) -0.014(1) -0.007(2) -0.023(1) C C96 0.049(2) 0.048(2) 0.105(3) -0.017(1) -0.020(2) -0.017(2) C C97 0.056(2) 0.037(2) 0.094(3) -0.007(1) -0.019(2) -0.002(2) C C98 0.039(2) 0.048(2) 0.108(3) -0.012(1) -0.012(2) -0.014(2) C C99 0.041(2) 0.053(2) 0.112(3) -0.011(1) -0.022(2) -0.018(2) C C100 0.058(2) 0.049(2) 0.101(2) -0.016(1) -0.025(2) -0.021(1) C C101 0.071(2) 0.058(2) 0.090(2) -0.025(1) -0.020(2) -0.025(1) C C102 0.115(3) 0.088(2) 0.112(3) -0.053(2) -0.007(3) -0.034(2) C # 10. MOLECULAR GEOMETRY 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 Si1 O1 1.626(2) . . ? Si1 O2 1.641(2) . . ? Si1 O3 1.625(2) . . ? Si1 O8 1.597(2) . . ? O1 C1 1.396(3) . . ? C1 C2 1.406(4) . . ? C1 C6 1.398(4) . . ? C2 C3 1.394(4) . . ? C2 C44 1.522(4) . . ? C3 C4 1.399(4) . . ? C4 C5 1.393(4) . . ? C4 C7 1.542(4) . . ? C5 C6 1.401(4) . . ? C6 C11 1.523(4) . . ? C7 C8 1.505(5) . . ? C7 C9 1.552(5) . . ? C7 C10 1.509(5) . . ? C11 C12 1.515(4) . . ? C12 C13 1.392(4) . . ? C12 C17 1.398(4) . . ? C13 O2 1.400(3) . . ? C13 C14 1.396(4) . . ? C14 C15 1.398(4) . . ? C14 C22 1.509(4) . . ? C15 C16 1.401(4) . . ? C16 C17 1.399(4) . . ? C16 C18 1.543(4) . . ? C18 C19 1.543(5) . . ? C18 C20 1.534(5) . . ? C18 C21 1.533(5) . . ? C22 C23 1.541(4) . . ? C23 C24 1.405(4) . . ? C23 C28 1.403(4) . . ? C24 O3 1.404(3) . . ? C24 C25 1.416(4) . . ? C25 C26 1.393(4) . . ? C25 C33 1.533(4) . . ? C26 C27 1.396(4) . . ? C27 C28 1.389(4) . . ? C27 C29 1.549(4) . . ? C29 C30 1.545(6) . . ? C29 C31 1.514(5) . . ? C29 C32 1.480(6) . . ? C33 C34 1.512(4) . . ? C34 C35 1.400(4) . . ? C34 C39 1.393(4) . . ? C35 O4 1.391(3) . . ? C35 C36 1.389(4) . . ? O4 Si2 1.607(2) . . ? C36 C37 1.396(4) . . ? C36 C44 1.518(4) . . ? C37 C38 1.396(4) . . ? C38 C39 1.403(4) . . ? C38 C40 1.543(4) . . ? C40 C41 1.535(4) . . ? C40 C42 1.534(5) . . ? C40 C43 1.539(4) . . ? Si2 O5 1.625(2) . . ? Si2 O6 1.637(2) . . ? Si2 O7 1.614(2) . . ? O5 C45 1.393(3) . . ? C45 C46 1.404(4) . . ? C45 C50 1.408(4) . . ? C46 C47 1.404(4) . . ? C46 C84 1.533(4) . . ? C47 C48 1.390(5) . . ? C48 C49 1.395(5) . . ? C48 C51 1.518(5) . . ? C49 C50 1.400(4) . . ? C50 C54 1.515(4) . . ? C51 C52 1.510(5) . . ? C52 C53 1.306(5) . . ? C54 C55 1.512(4) . . ? C55 C56 1.396(4) . . ? C55 C60 1.392(4) . . ? C56 O6 1.410(3) . . ? C56 C57 1.388(4) . . ? C57 C58 1.400(4) . . ? C57 C64 1.516(4) . . ? C58 C59 1.395(4) . . ? C59 C60 1.393(4) . . ? C59 C61 1.517(4) . . ? C61 C62 1.500(4) . . ? C62 C63 1.305(5) . . ? C64 C65 1.519(4) . . ? C65 C66 1.395(4) . . ? C65 C70 1.408(4) . . ? C66 O7 1.391(3) . . ? C66 C67 1.409(4) . . ? C67 C68 1.395(4) . . ? C67 C74 1.518(4) . . ? C68 C69 1.390(4) . . ? C69 C70 1.388(4) . . ? C69 C71 1.521(4) . . ? C71 C72 1.486(5) . . ? C72 C73 1.311(6) . . ? C74 C75 1.510(4) . . ? C75 C76 1.393(4) . . ? C75 C80 1.407(4) . . ? C76 O8 1.389(3) . . ? C76 C77 1.401(4) . . ? C77 C78 1.396(4) . . ? C77 C84 1.503(4) . . ? C78 C79 1.392(5) . . ? C79 C80 1.387(5) . . ? C79 C81 1.516(4) . . ? C81 C82 1.474(5) . . ? C82 C83 1.313(5) . . ? C85 C86 1.398(5) . . ? C85 C90 1.388(5) . . ? C85 C91 1.450(5) . . ? C86 C87 1.394(5) . . ? C87 C88 1.374(6) . . ? C88 C89 1.378(5) . . ? C89 C90 1.388(5) . . ? C91 C92 1.191(4) . . ? C92 C93 1.470(5) . . ? C94 C95 1.393(6) . . ? C94 C99 1.412(6) . . ? C94 C100 1.469(7) . . ? C95 C96 1.384(6) . . ? C96 C97 1.379(6) . . ? C97 C98 1.396(6) . . ? C98 C99 1.369(7) . . ? C100 C101 1.186(7) . . ? C101 C102 1.435(8) . . ? 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 ? ? ? ? ? ? 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 O1 Si1 O2 109.9(1) . . . ? O1 Si1 O3 110.1(1) . . . ? O1 Si1 O8 109.8(1) . . . ? O2 Si1 O3 108.5(1) . . . ? O2 Si1 O8 108.3(1) . . . ? O3 Si1 O8 110.2(1) . . . ? Si1 O1 C1 138.5(2) . . . ? O1 C1 C2 117.3(2) . . . ? O1 C1 C6 121.7(2) . . . ? C2 C1 C6 120.8(2) . . . ? C1 C2 C3 118.0(2) . . . ? C1 C2 C44 122.5(2) . . . ? C3 C2 C44 119.4(2) . . . ? C2 C3 C4 123.0(3) . . . ? C3 C4 C5 116.4(2) . . . ? C3 C4 C7 120.3(3) . . . ? C5 C4 C7 123.2(3) . . . ? C4 C5 C6 123.0(3) . . . ? C1 C6 C5 118.0(3) . . . ? C1 C6 C11 123.0(2) . . . ? C5 C6 C11 119.1(2) . . . ? C4 C7 C8 109.4(3) . . . ? C4 C7 C9 109.1(3) . . . ? C4 C7 C10 112.5(3) . . . ? C8 C7 C9 108.6(4) . . . ? C8 C7 C10 111.2(3) . . . ? C9 C7 C10 105.9(3) . . . ? C6 C11 C12 111.7(2) . . . ? C11 C12 C13 120.5(2) . . . ? C11 C12 C17 121.6(2) . . . ? C13 C12 C17 117.7(3) . . . ? C12 C13 O2 119.5(2) . . . ? C12 C13 C14 122.4(3) . . . ? O2 C13 C14 118.1(2) . . . ? Si1 O2 C13 115.6(2) . . . ? C13 C14 C15 117.8(3) . . . ? C13 C14 C22 119.6(2) . . . ? C15 C14 C22 122.5(3) . . . ? C14 C15 C16 122.2(3) . . . ? C15 C16 C17 117.5(3) . . . ? C15 C16 C18 123.2(3) . . . ? C17 C16 C18 119.3(3) . . . ? C12 C17 C16 122.4(3) . . . ? C16 C18 C19 109.2(3) . . . ? C16 C18 C20 112.3(3) . . . ? C16 C18 C21 109.4(3) . . . ? C19 C18 C20 108.3(3) . . . ? C19 C18 C21 109.4(3) . . . ? C20 C18 C21 108.2(3) . . . ? C14 C22 C23 120.6(2) . . . ? C22 C23 C24 127.2(2) . . . ? C22 C23 C28 114.6(2) . . . ? C24 C23 C28 118.0(2) . . . ? C23 C24 O3 121.8(2) . . . ? C23 C24 C25 120.4(2) . . . ? O3 C24 C25 117.9(2) . . . ? Si1 O3 C24 129.4(2) . . . ? C24 C25 C26 118.1(2) . . . ? C24 C25 C33 125.5(2) . . . ? C26 C25 C33 116.1(2) . . . ? C25 C26 C27 123.7(3) . . . ? C26 C27 C28 116.0(3) . . . ? C26 C27 C29 121.1(3) . . . ? C28 C27 C29 122.9(3) . . . ? C23 C28 C27 123.7(3) . . . ? C27 C29 C30 109.1(3) . . . ? C27 C29 C31 112.8(3) . . . ? C27 C29 C32 110.3(3) . . . ? C30 C29 C31 105.3(4) . . . ? C30 C29 C32 106.1(4) . . . ? C31 C29 C32 112.7(4) . . . ? C25 C33 C34 120.0(2) . . . ? C33 C34 C35 120.7(2) . . . ? C33 C34 C39 121.4(2) . . . ? C35 C34 C39 117.8(2) . . . ? C34 C35 O4 117.2(2) . . . ? C34 C35 C36 121.6(2) . . . ? O4 C35 C36 120.8(2) . . . ? C35 O4 Si2 143.8(2) . . . ? C35 C36 C37 117.9(2) . . . ? C35 C36 C44 122.3(2) . . . ? C37 C36 C44 119.3(2) . . . ? C36 C37 C38 122.9(2) . . . ? C37 C38 C39 116.5(2) . . . ? C37 C38 C40 121.3(2) . . . ? C39 C38 C40 122.2(2) . . . ? C34 C39 C38 122.8(2) . . . ? C38 C40 C41 111.5(2) . . . ? C38 C40 C42 110.9(2) . . . ? C38 C40 C43 108.4(2) . . . ? C41 C40 C42 107.8(3) . . . ? C41 C40 C43 108.6(3) . . . ? C42 C40 C43 109.6(3) . . . ? C2 C44 C36 109.0(2) . . . ? O4 Si2 O5 109.2(1) . . . ? O4 Si2 O6 109.7(1) . . . ? O4 Si2 O7 109.9(1) . . . ? O5 Si2 O6 109.2(1) . . . ? O5 Si2 O7 108.1(1) . . . ? O6 Si2 O7 110.6(1) . . . ? Si2 O5 C45 133.3(2) . . . ? O5 C45 C46 117.5(2) . . . ? O5 C45 C50 120.9(2) . . . ? C46 C45 C50 121.5(3) . . . ? C45 C46 C47 117.5(3) . . . ? C45 C46 C84 123.7(3) . . . ? C47 C46 C84 118.6(3) . . . ? C46 C47 C48 123.0(3) . . . ? C47 C48 C49 117.4(3) . . . ? C47 C48 C51 121.9(3) . . . ? C49 C48 C51 120.7(3) . . . ? C48 C49 C50 122.5(3) . . . ? C45 C50 C49 118.0(3) . . . ? C45 C50 C54 125.5(3) . . . ? C49 C50 C54 116.3(3) . . . ? C48 C51 C52 113.9(3) . . . ? C51 C52 C53 127.2(3) . . . ? C50 C54 C55 118.9(2) . . . ? C54 C55 C56 120.1(3) . . . ? C54 C55 C60 122.3(3) . . . ? C56 C55 C60 117.6(3) . . . ? C55 C56 O6 117.7(2) . . . ? C55 C56 C57 122.5(3) . . . ? O6 C56 C57 119.7(2) . . . ? Si2 O6 C56 111.5(2) . . . ? C56 C57 C58 117.9(3) . . . ? C56 C57 C64 120.1(2) . . . ? C58 C57 C64 122.0(3) . . . ? C57 C58 C59 121.7(3) . . . ? C58 C59 C60 118.1(3) . . . ? C58 C59 C61 122.0(3) . . . ? C60 C59 C61 119.9(3) . . . ? C55 C60 C59 122.2(3) . . . ? C59 C61 C62 113.7(3) . . . ? C61 C62 C63 126.1(3) . . . ? C57 C64 C65 112.9(2) . . . ? C64 C65 C66 123.2(3) . . . ? C64 C65 C70 119.2(3) . . . ? C66 C65 C70 117.6(3) . . . ? C65 C66 O7 122.0(2) . . . ? C65 C66 C67 121.5(3) . . . ? O7 C66 C67 116.4(2) . . . ? Si2 O7 C66 149.0(2) . . . ? C66 C67 C68 118.2(3) . . . ? C66 C67 C74 121.7(2) . . . ? C68 C67 C74 120.1(3) . . . ? C67 C68 C69 122.1(3) . . . ? C68 C69 C70 118.0(3) . . . ? C68 C69 C71 120.2(3) . . . ? C70 C69 C71 121.8(3) . . . ? C65 C70 C69 122.5(3) . . . ? C69 C71 C72 115.5(3) . . . ? C71 C72 C73 127.1(4) . . . ? C67 C74 C75 111.5(2) . . . ? C74 C75 C76 123.0(2) . . . ? C74 C75 C80 119.6(3) . . . ? C76 C75 C80 117.1(3) . . . ? C75 C76 O8 121.0(2) . . . ? C75 C76 C77 122.7(2) . . . ? O8 C76 C77 116.1(2) . . . ? Si1 O8 C76 149.9(2) . . . ? C76 C77 C78 117.5(3) . . . ? C76 C77 C84 121.4(2) . . . ? C78 C77 C84 121.1(3) . . . ? C77 C78 C79 122.1(3) . . . ? C78 C79 C80 118.3(3) . . . ? C78 C79 C81 121.1(3) . . . ? C80 C79 C81 120.7(3) . . . ? C75 C80 C79 122.3(3) . . . ? C79 C81 C82 114.1(3) . . . ? C81 C82 C83 125.7(3) . . . ? C46 C84 C77 116.8(2) . . . ? C86 C85 C90 118.2(3) . . . ? C86 C85 C91 120.6(3) . . . ? C90 C85 C91 121.1(3) . . . ? C85 C86 C87 120.7(3) . . . ? C86 C87 C88 120.1(3) . . . ? C87 C88 C89 119.8(3) . . . ? C88 C89 C90 120.5(4) . . . ? C85 C90 C89 120.7(3) . . . ? C85 C91 C92 179.2(3) . . . ? C91 C92 C93 180.0(9) . . . ? C95 C94 C99 117.6(5) . . . ? C95 C94 C100 120.4(4) . . . ? C99 C94 C100 122.0(4) . . . ? C94 C95 C96 121.0(4) . . . ? C95 C96 C97 120.3(4) . . . ? C96 C97 C98 119.8(5) . . . ? C97 C98 C99 119.7(4) . . . ? C94 C99 C98 121.5(4) . . . ? C94 C100 C101 179.3(5) . . . ? C100 C101 C102 178.5(6) . . . ?