# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 _publ_requested_journal ' Chemical Communications ' loop_ _publ_author_name 'Tsutsui, Shinobu' 'Sakamoto, Kenkichi' _publ_contact_author_name ' Dr Shinobu Tsutsui ' _publ_contact_author_address ; Photodynamics Research Center, The Institute of Physical and Chemical Research (RIKEN), 519-1399 Aoba, Aramaki, Aoba-ku, Sendai 980-0845, JAPAN ; _publ_contact_author_email ' stsutsui@postman.riken.go.jp ' _publ_section_title ; Preparation and Structures of Novel Silamacrocyclic Compounds: Silacalix[4]quinone and Silacalix[4]hydroquinone Octamethyl Ether ; _publ_section_references ; ? ; data_tetrasilacalix4arene_2 _database_code_CSD 213339 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H56 O8 Si4' _chemical_formula_weight 777.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.569(11) _cell_length_b 16.408(16) _cell_length_c 23.63(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.093(17) _cell_angle_gamma 90.00 _cell_volume 4369(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3907 _cell_measurement_theta_min 2.207 _cell_measurement_theta_max 26.797 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9388 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 82 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.38 _diffrn_reflns_number 21757 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.1432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7676 _reflns_number_gt 4197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7676 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3258(3) 0.2114(2) 0.12156(14) 0.0188(8) Uani 1 1 d . . . C2 C 0.2855(3) 0.2058(2) 0.06042(14) 0.0196(8) Uani 1 1 d . . . C3 C 0.3189(3) 0.1346(2) 0.03422(15) 0.0212(8) Uani 1 1 d . . . H3 H 0.2918 0.1278 -0.0066 0.025 Uiso 1 1 calc R . . C4 C 0.3899(3) 0.0743(2) 0.06584(14) 0.0198(8) Uani 1 1 d . . . C5 C 0.4329(3) 0.0846(2) 0.12562(14) 0.0190(8) Uani 1 1 d . . . H5 H 0.4859 0.0453 0.1469 0.023 Uiso 1 1 calc R . . C6 C 0.3987(3) 0.1526(2) 0.15503(14) 0.0192(8) Uani 1 1 d . . . C7 C 0.3486(3) 0.3456(2) 0.16457(16) 0.0329(10) Uani 1 1 d . . . H7A H 0.4214 0.3306 0.1928 0.049 Uiso 1 1 calc R . . H7B H 0.3051 0.3865 0.1818 0.049 Uiso 1 1 calc R . . H7C H 0.3691 0.3683 0.1297 0.049 Uiso 1 1 calc R . . C8 C 0.4880(3) -0.0563(2) 0.06646(15) 0.0265(9) Uani 1 1 d . . . H8A H 0.5679 -0.0335 0.0794 0.040 Uiso 1 1 calc R . . H8B H 0.4905 -0.1028 0.0407 0.040 Uiso 1 1 calc R . . H8C H 0.4593 -0.0745 0.1003 0.040 Uiso 1 1 calc R . . C9 C 0.6010(3) 0.1998(2) 0.25861(15) 0.0306(9) Uani 1 1 d . . . H9A H 0.6306 0.1968 0.3008 0.046 Uiso 1 1 calc R . . H9B H 0.5937 0.2571 0.2465 0.046 Uiso 1 1 calc R . . H9C H 0.6565 0.1720 0.2394 0.046 Uiso 1 1 calc R . . C10 C 0.4730(3) 0.0397(2) 0.26129(15) 0.0329(10) Uani 1 1 d . . . H10A H 0.5402 0.0167 0.2479 0.049 Uiso 1 1 calc R . . H10B H 0.4010 0.0087 0.2445 0.049 Uiso 1 1 calc R . . H10C H 0.4889 0.0366 0.3038 0.049 Uiso 1 1 calc R . . C11 C 0.2365(3) 0.16888(19) 0.28703(14) 0.0183(8) Uani 1 1 d . . . C12 C 0.3460(3) 0.2001(2) 0.27863(13) 0.0182(8) Uani 1 1 d . . . C13 C 0.3855(3) 0.2737(2) 0.30778(14) 0.0202(8) Uani 1 1 d . . . H13 H 0.4575 0.2972 0.3027 0.024 Uiso 1 1 calc R . . C14 C 0.3225(3) 0.3137(2) 0.34399(14) 0.0206(8) Uani 1 1 d . . . C15 C 0.2137(3) 0.2824(2) 0.35024(14) 0.0203(8) Uani 1 1 d . . . H15 H 0.1702 0.3099 0.3741 0.024 Uiso 1 1 calc R . . C16 C 0.1679(3) 0.2094(2) 0.32097(13) 0.0177(8) Uani 1 1 d . . . C17 C 0.1610(3) 0.0789(2) 0.20528(14) 0.0310(9) Uani 1 1 d . . . H17A H 0.1010 0.1191 0.1877 0.046 Uiso 1 1 calc R . . H17B H 0.1285 0.0239 0.1971 0.046 Uiso 1 1 calc R . . H17C H 0.2312 0.0851 0.1890 0.046 Uiso 1 1 calc R . . C18 C 0.3218(3) 0.4234(2) 0.41206(16) 0.0340(10) Uani 1 1 d . . . H18A H 0.2415 0.4405 0.3927 0.051 Uiso 1 1 calc R . . H18B H 0.3685 0.4712 0.4284 0.051 Uiso 1 1 calc R . . H18C H 0.3177 0.3851 0.4434 0.051 Uiso 1 1 calc R . . C19 C 0.0253(3) 0.0716(2) 0.36528(15) 0.0290(9) Uani 1 1 d . . . H19A H 0.0721 0.0806 0.4049 0.044 Uiso 1 1 calc R . . H19B H 0.0640 0.0302 0.3461 0.044 Uiso 1 1 calc R . . H19C H -0.0544 0.0529 0.3668 0.044 Uiso 1 1 calc R . . C20 C -0.0630(3) 0.2479(2) 0.36039(15) 0.0251(9) Uani 1 1 d . . . H20A H -0.1430 0.2286 0.3608 0.038 Uiso 1 1 calc R . . H20B H -0.0684 0.2998 0.3395 0.038 Uiso 1 1 calc R . . H20C H -0.0175 0.2555 0.4004 0.038 Uiso 1 1 calc R . . C21 C -0.1143(3) 0.2159(2) 0.20532(14) 0.0184(8) Uani 1 1 d . . . C22 C -0.0801(3) 0.1530(2) 0.24645(14) 0.0171(8) Uani 1 1 d . . . C23 C -0.1231(3) 0.0731(2) 0.23055(14) 0.0211(8) Uani 1 1 d . . . H23 H -0.1023 0.0296 0.2575 0.025 Uiso 1 1 calc R . . C24 C -0.1958(3) 0.0580(2) 0.17568(15) 0.0204(8) Uani 1 1 d . . . C25 C -0.2296(3) 0.1224(2) 0.13663(15) 0.0222(8) Uani 1 1 d . . . H25 H -0.2806 0.1115 0.0999 0.027 Uiso 1 1 calc R . . C26 C -0.1904(3) 0.2028(2) 0.15000(14) 0.0189(8) Uani 1 1 d . . . C27 C 0.0381(3) 0.3189(2) 0.20697(15) 0.0278(9) Uani 1 1 d . . . H27A H 0.0619 0.2762 0.1829 0.042 Uiso 1 1 calc R . . H27B H 0.0989 0.3245 0.2431 0.042 Uiso 1 1 calc R . . H27C H 0.0293 0.3707 0.1858 0.042 Uiso 1 1 calc R . . C28 C -0.1938(4) -0.0875(2) 0.19239(17) 0.0381(10) Uani 1 1 d . . . H28A H -0.1069 -0.0872 0.2008 0.057 Uiso 1 1 calc R . . H28B H -0.2235 -0.1379 0.1720 0.057 Uiso 1 1 calc R . . H28C H -0.2204 -0.0842 0.2288 0.057 Uiso 1 1 calc R . . C29 C -0.3312(3) 0.3642(2) 0.13177(16) 0.0331(10) Uani 1 1 d . . . H29A H -0.3650 0.4067 0.1037 0.050 Uiso 1 1 calc R . . H29B H -0.2766 0.3891 0.1651 0.050 Uiso 1 1 calc R . . H29C H -0.3952 0.3363 0.1450 0.050 Uiso 1 1 calc R . . C30 C -0.3554(3) 0.2449(2) 0.03155(16) 0.0326(10) Uani 1 1 d . . . H30A H -0.3867 0.2887 0.0042 0.049 Uiso 1 1 calc R . . H30B H -0.4209 0.2183 0.0444 0.049 Uiso 1 1 calc R . . H30C H -0.3145 0.2048 0.0123 0.049 Uiso 1 1 calc R . . C31 C -0.0352(3) 0.3003(2) 0.05126(13) 0.0185(8) Uani 1 1 d . . . C32 C -0.1217(3) 0.3435(2) 0.07371(13) 0.0178(8) Uani 1 1 d . . . C33 C -0.1022(3) 0.4275(2) 0.08447(13) 0.0180(8) Uani 1 1 d . . . H33 H -0.1598 0.4585 0.0980 0.022 Uiso 1 1 calc R . . C34 C 0.0003(3) 0.4664(2) 0.07564(13) 0.0165(8) Uani 1 1 d . . . C35 C 0.0865(3) 0.4207(2) 0.05689(13) 0.0184(8) Uani 1 1 d . . . H35 H 0.1575 0.4469 0.0529 0.022 Uiso 1 1 calc R . . C36 C 0.0715(3) 0.3362(2) 0.04357(13) 0.0180(8) Uani 1 1 d . . . C37 C 0.0085(3) 0.1540(2) 0.06181(17) 0.0313(10) Uani 1 1 d . . . H37A H 0.0560 0.1345 0.0351 0.047 Uiso 1 1 calc R . . H37B H -0.0399 0.1091 0.0712 0.047 Uiso 1 1 calc R . . H37C H 0.0614 0.1739 0.0976 0.047 Uiso 1 1 calc R . . C38 C 0.1188(3) 0.5889(2) 0.08360(14) 0.0227(8) Uani 1 1 d . . . H38A H 0.1851 0.5628 0.1107 0.034 Uiso 1 1 calc R . . H38B H 0.1156 0.6467 0.0936 0.034 Uiso 1 1 calc R . . H38C H 0.1302 0.5838 0.0439 0.034 Uiso 1 1 calc R . . C39 C 0.1220(3) 0.2390(2) -0.06041(14) 0.0289(9) Uani 1 1 d . . . H39A H 0.0785 0.2808 -0.0864 0.043 Uiso 1 1 calc R . . H39B H 0.0670 0.1959 -0.0548 0.043 Uiso 1 1 calc R . . H39C H 0.1840 0.2157 -0.0777 0.043 Uiso 1 1 calc R . . C40 C 0.2961(3) 0.3672(2) -0.00364(16) 0.0300(9) Uani 1 1 d . . . H40A H 0.3522 0.3429 -0.0242 0.045 Uiso 1 1 calc R . . H40B H 0.3398 0.3908 0.0331 0.045 Uiso 1 1 calc R . . H40C H 0.2505 0.4100 -0.0277 0.045 Uiso 1 1 calc R . . O1 O 0.27618(19) 0.27502(14) 0.14918(10) 0.0228(6) Uani 1 1 d . . . O2 O 0.4093(2) 0.00511(14) 0.03562(10) 0.0276(6) Uani 1 1 d . . . O3 O 0.1939(2) 0.09129(14) 0.26715(9) 0.0236(6) Uani 1 1 d . . . O4 O 0.3777(2) 0.38408(14) 0.37048(10) 0.0250(6) Uani 1 1 d . . . O5 O -0.0753(2) 0.29668(13) 0.22060(10) 0.0252(6) Uani 1 1 d . . . O6 O -0.2386(2) -0.01887(14) 0.15648(10) 0.0313(6) Uani 1 1 d . . . O7 O -0.0676(2) 0.21896(13) 0.03494(10) 0.0247(6) Uani 1 1 d . . . O8 O 0.0091(2) 0.54981(13) 0.08745(9) 0.0217(6) Uani 1 1 d . . . Si1 Si 0.45170(9) 0.14934(6) 0.23782(4) 0.0208(2) Uani 1 1 d . . . Si2 Si 0.01360(8) 0.17045(6) 0.32292(4) 0.0189(2) Uani 1 1 d . . . Si3 Si -0.24816(8) 0.28843(6) 0.09611(4) 0.0203(2) Uani 1 1 d . . . Si4 Si 0.19176(8) 0.28619(6) 0.01166(4) 0.0200(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0195(19) 0.0165(19) 0.0227(19) -0.0053(15) 0.0096(15) 0.0012(16) C2 0.0199(19) 0.026(2) 0.0149(18) 0.0014(15) 0.0075(15) 0.0010(16) C3 0.0178(19) 0.028(2) 0.0190(19) 0.0037(16) 0.0069(15) 0.0008(16) C4 0.024(2) 0.020(2) 0.0171(19) 0.0001(15) 0.0074(15) 0.0025(16) C5 0.0201(19) 0.019(2) 0.0180(18) 0.0024(15) 0.0045(15) 0.0034(16) C6 0.0187(19) 0.020(2) 0.0195(19) 0.0033(15) 0.0052(15) -0.0012(16) C7 0.046(3) 0.023(2) 0.030(2) -0.0026(17) 0.0089(19) 0.000(2) C8 0.028(2) 0.025(2) 0.026(2) 0.0007(16) 0.0061(17) 0.0057(18) C9 0.029(2) 0.045(3) 0.0181(19) -0.0070(17) 0.0058(16) 0.0044(19) C10 0.048(3) 0.035(2) 0.017(2) 0.0001(17) 0.0100(18) 0.012(2) C11 0.027(2) 0.0119(19) 0.0138(18) 0.0025(14) -0.0010(15) 0.0005(16) C12 0.0220(19) 0.020(2) 0.0119(17) 0.0023(14) 0.0031(14) 0.0021(16) C13 0.0191(19) 0.023(2) 0.0182(18) 0.0034(15) 0.0037(15) -0.0005(16) C14 0.025(2) 0.018(2) 0.0170(19) -0.0010(15) 0.0019(16) 0.0012(16) C15 0.0197(19) 0.021(2) 0.0195(19) 0.0022(16) 0.0028(15) 0.0035(16) C16 0.0207(19) 0.0194(19) 0.0135(17) 0.0027(15) 0.0046(14) 0.0063(16) C17 0.038(2) 0.037(2) 0.019(2) -0.0122(17) 0.0079(17) -0.0058(19) C18 0.040(3) 0.030(2) 0.033(2) -0.0156(18) 0.0128(19) -0.0038(19) C19 0.038(2) 0.026(2) 0.022(2) 0.0016(16) 0.0049(17) -0.0058(18) C20 0.021(2) 0.031(2) 0.024(2) -0.0047(17) 0.0050(16) 0.0012(17) C21 0.0191(19) 0.0168(19) 0.0213(19) -0.0038(16) 0.0089(15) -0.0030(16) C22 0.0127(18) 0.021(2) 0.0174(18) -0.0017(15) 0.0031(14) 0.0011(15) C23 0.023(2) 0.019(2) 0.0210(19) 0.0011(15) 0.0049(16) -0.0026(16) C24 0.0179(19) 0.019(2) 0.025(2) -0.0001(16) 0.0045(15) -0.0022(16) C25 0.019(2) 0.028(2) 0.0183(19) -0.0007(16) 0.0012(15) -0.0029(17) C26 0.0163(18) 0.026(2) 0.0172(18) 0.0022(15) 0.0091(15) -0.0005(16) C27 0.026(2) 0.026(2) 0.027(2) 0.0038(17) -0.0020(17) -0.0121(17) C28 0.052(3) 0.019(2) 0.039(2) -0.0032(18) 0.001(2) -0.005(2) C29 0.031(2) 0.036(2) 0.036(2) 0.0066(19) 0.0160(19) 0.0054(19) C30 0.030(2) 0.034(2) 0.029(2) 0.0071(18) -0.0024(18) -0.0003(19) C31 0.025(2) 0.017(2) 0.0109(17) 0.0031(14) -0.0013(14) 0.0028(16) C32 0.0216(19) 0.022(2) 0.0085(17) 0.0068(14) 0.0000(14) 0.0053(16) C33 0.023(2) 0.021(2) 0.0098(17) 0.0025(14) 0.0022(14) 0.0052(16) C34 0.023(2) 0.017(2) 0.0068(16) 0.0010(14) -0.0019(14) 0.0034(16) C35 0.0192(19) 0.023(2) 0.0118(17) 0.0024(15) 0.0007(14) 0.0013(16) C36 0.024(2) 0.019(2) 0.0091(17) 0.0039(14) 0.0010(14) 0.0045(16) C37 0.032(2) 0.021(2) 0.042(2) 0.0063(18) 0.0112(19) 0.0034(18) C38 0.028(2) 0.017(2) 0.0193(19) -0.0011(15) -0.0013(15) -0.0018(17) C39 0.031(2) 0.041(2) 0.0146(19) 0.0036(17) 0.0038(16) 0.0136(19) C40 0.031(2) 0.032(2) 0.029(2) 0.0066(17) 0.0116(18) 0.0065(18) O1 0.0240(14) 0.0222(14) 0.0223(13) -0.0082(11) 0.0058(11) 0.0018(11) O2 0.0397(16) 0.0216(14) 0.0200(14) -0.0021(11) 0.0035(11) 0.0113(12) O3 0.0320(15) 0.0220(14) 0.0159(13) -0.0010(10) 0.0039(11) -0.0047(11) O4 0.0262(14) 0.0210(14) 0.0291(14) -0.0079(11) 0.0091(11) -0.0017(11) O5 0.0317(15) 0.0184(14) 0.0263(14) -0.0038(11) 0.0085(11) -0.0053(11) O6 0.0396(16) 0.0171(14) 0.0307(15) 0.0023(11) -0.0057(12) -0.0070(12) O7 0.0318(15) 0.0155(14) 0.0267(14) 0.0014(11) 0.0064(11) 0.0035(11) O8 0.0263(14) 0.0193(14) 0.0194(13) -0.0016(10) 0.0049(10) -0.0028(11) Si1 0.0237(6) 0.0255(6) 0.0131(5) -0.0006(4) 0.0041(4) 0.0037(5) Si2 0.0206(5) 0.0198(6) 0.0162(5) 0.0000(4) 0.0037(4) -0.0008(4) Si3 0.0204(5) 0.0243(6) 0.0165(5) 0.0028(4) 0.0047(4) 0.0015(5) Si4 0.0237(6) 0.0224(6) 0.0143(5) 0.0018(4) 0.0052(4) 0.0046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.402(5) . ? C1 C2 1.417(5) . ? C1 O1 1.419(4) . ? C2 C3 1.416(5) . ? C2 Si4 1.918(4) . ? C3 C4 1.390(5) . ? C4 O2 1.387(4) . ? C4 C5 1.398(5) . ? C5 C6 1.418(5) . ? C6 Si1 1.914(4) . ? C7 O1 1.428(4) . ? C8 O2 1.441(4) . ? C9 Si1 1.878(4) . ? C10 Si1 1.882(4) . ? C11 O3 1.407(4) . ? C11 C16 1.415(5) . ? C11 C12 1.422(5) . ? C12 C13 1.414(5) . ? C12 Si1 1.911(4) . ? C13 C14 1.405(5) . ? C14 O4 1.397(4) . ? C14 C15 1.398(5) . ? C15 C16 1.424(5) . ? C16 Si2 1.907(4) . ? C17 O3 1.439(4) . ? C18 O4 1.445(4) . ? C19 Si2 1.895(4) . ? C20 Si2 1.881(4) . ? C21 C22 1.412(5) . ? C21 C26 1.418(5) . ? C21 O5 1.420(4) . ? C22 C23 1.422(5) . ? C22 Si2 1.907(4) . ? C23 C24 1.399(5) . ? C24 O6 1.392(4) . ? C24 C25 1.400(5) . ? C25 C26 1.408(5) . ? C26 Si3 1.912(4) . ? C27 O5 1.466(4) . ? C28 O6 1.434(4) . ? C29 Si3 1.883(4) . ? C30 Si3 1.876(4) . ? C31 C36 1.416(5) . ? C31 O7 1.416(4) . ? C31 C32 1.423(5) . ? C32 C33 1.411(5) . ? C32 Si3 1.894(4) . ? C33 C34 1.403(5) . ? C34 O8 1.396(4) . ? C34 C35 1.398(4) . ? C35 C36 1.424(5) . ? C36 Si4 1.911(4) . ? C37 O7 1.436(4) . ? C38 O8 1.444(4) . ? C39 Si4 1.878(4) . ? C40 Si4 1.885(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 123.2(3) . . ? C6 C1 O1 120.1(3) . . ? C2 C1 O1 116.3(3) . . ? C3 C2 C1 116.1(3) . . ? C3 C2 Si4 118.6(2) . . ? C1 C2 Si4 125.3(3) . . ? C4 C3 C2 122.6(3) . . ? O2 C4 C3 116.8(3) . . ? O2 C4 C5 123.8(3) . . ? C3 C4 C5 119.3(3) . . ? C4 C5 C6 121.0(3) . . ? C1 C6 C5 117.7(3) . . ? C1 C6 Si1 127.5(3) . . ? C5 C6 Si1 114.7(2) . . ? O3 C11 C16 114.5(3) . . ? O3 C11 C12 122.4(3) . . ? C16 C11 C12 122.8(3) . . ? C13 C12 C11 116.1(3) . . ? C13 C12 Si1 116.5(3) . . ? C11 C12 Si1 127.3(3) . . ? C14 C13 C12 122.7(3) . . ? O4 C14 C15 126.0(3) . . ? O4 C14 C13 114.3(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 120.1(3) . . ? C11 C16 C15 118.4(3) . . ? C11 C16 Si2 120.3(3) . . ? C15 C16 Si2 121.1(2) . . ? C22 C21 C26 122.9(3) . . ? C22 C21 O5 119.0(3) . . ? C26 C21 O5 118.1(3) . . ? C21 C22 C23 117.8(3) . . ? C21 C22 Si2 123.6(2) . . ? C23 C22 Si2 118.6(2) . . ? C24 C23 C22 120.7(3) . . ? O6 C24 C23 123.9(3) . . ? O6 C24 C25 116.3(3) . . ? C23 C24 C25 119.7(3) . . ? C24 C25 C26 122.2(3) . . ? C25 C26 C21 116.8(3) . . ? C25 C26 Si3 119.5(2) . . ? C21 C26 Si3 123.6(3) . . ? C36 C31 O7 122.8(3) . . ? C36 C31 C32 123.2(3) . . ? O7 C31 C32 113.9(3) . . ? C33 C32 C31 117.1(3) . . ? C33 C32 Si3 121.2(3) . . ? C31 C32 Si3 121.3(3) . . ? C34 C33 C32 121.6(3) . . ? O8 C34 C35 124.3(3) . . ? O8 C34 C33 116.2(3) . . ? C35 C34 C33 119.5(3) . . ? C34 C35 C36 122.1(3) . . ? C31 C36 C35 116.3(3) . . ? C31 C36 Si4 127.3(3) . . ? C35 C36 Si4 116.2(3) . . ? C1 O1 C7 116.0(3) . . ? C4 O2 C8 118.0(3) . . ? C11 O3 C17 117.3(2) . . ? C14 O4 C18 116.4(3) . . ? C21 O5 C27 115.1(2) . . ? C24 O6 C28 117.6(3) . . ? C31 O7 C37 118.8(3) . . ? C34 O8 C38 116.7(3) . . ? C9 Si1 C10 107.06(18) . . ? C9 Si1 C12 109.34(16) . . ? C10 Si1 C12 108.90(16) . . ? C9 Si1 C6 108.51(15) . . ? C10 Si1 C6 108.58(15) . . ? C12 Si1 C6 114.22(15) . . ? C20 Si2 C19 108.30(18) . . ? C20 Si2 C22 108.66(16) . . ? C19 Si2 C22 109.23(16) . . ? C20 Si2 C16 109.20(16) . . ? C19 Si2 C16 110.15(16) . . ? C22 Si2 C16 111.23(15) . . ? C30 Si3 C29 107.77(18) . . ? C30 Si3 C32 111.39(17) . . ? C29 Si3 C32 108.35(17) . . ? C30 Si3 C26 109.19(17) . . ? C29 Si3 C26 108.89(17) . . ? C32 Si3 C26 111.16(15) . . ? C39 Si4 C40 106.21(17) . . ? C39 Si4 C36 109.43(16) . . ? C40 Si4 C36 109.14(17) . . ? C39 Si4 C2 109.24(17) . . ? C40 Si4 C2 107.53(17) . . ? C36 Si4 C2 114.92(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.421 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.071 #===END data_tetrasilacalix4quinone_1 _database_code_CSD 213340 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H94 O16 Si8' _chemical_formula_weight 1632.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.866(4) _cell_length_b 13.099(2) _cell_length_c 16.060(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.575(3) _cell_angle_gamma 90.00 _cell_volume 4407.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3417 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.27 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9298 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 109 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.13 _diffrn_reflns_number 13196 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5135 _reflns_number_gt 3185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+2.9113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5135 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.24607(13) 0.2794(2) 0.2806(2) 0.0250(6) Uani 1 1 d . . . C2 C 0.17508(13) 0.2738(2) 0.2155(2) 0.0259(6) Uani 1 1 d . . . C3 C 0.14931(14) 0.2612(2) 0.1184(2) 0.0310(7) Uani 1 1 d . . . H3 H 0.1042 0.2567 0.0764 0.037 Uiso 1 1 calc R . . C4 C 0.18756(14) 0.2539(2) 0.0736(2) 0.0324(7) Uani 1 1 d . . . C5 C 0.25742(14) 0.2642(2) 0.1390(2) 0.0296(6) Uani 1 1 d . . . H5 H 0.2826 0.2631 0.1109 0.036 Uiso 1 1 calc R . . C6 C 0.28660(13) 0.2751(2) 0.2376(2) 0.0254(6) Uani 1 1 d . . . C7 C 0.14799(17) 0.1675(3) 0.3593(3) 0.0424(8) Uani 1 1 d . . . H7A H 0.1173 0.1627 0.3796 0.064 Uiso 1 1 calc R . . H7B H 0.1911 0.1760 0.4179 0.064 Uiso 1 1 calc R . . H7C H 0.1462 0.1050 0.3244 0.064 Uiso 1 1 calc R . . C8 C 0.04147(15) 0.2803(3) 0.1769(3) 0.0443(8) Uani 1 1 d . . . H8A H 0.0297 0.2145 0.1424 0.066 Uiso 1 1 calc R . . H8B H 0.0330 0.3351 0.1299 0.066 Uiso 1 1 calc R . . H8C H 0.0162 0.2918 0.2065 0.066 Uiso 1 1 calc R . . C9 C 0.1365(2) 0.5000 0.2981(3) 0.0322(9) Uani 1 2 d S . . C10 C 0.14953(14) 0.4004(2) 0.3511(2) 0.0305(7) Uani 1 1 d . . . C11 C 0.17690(15) 0.4034(2) 0.4495(2) 0.0343(7) Uani 1 1 d . . . H11 H 0.1863 0.3408 0.4845 0.041 Uiso 1 1 calc R . . C12 C 0.1931(2) 0.5000 0.5055(3) 0.0373(10) Uani 1 2 d S . . C13 C 0.37786(18) 0.5000 0.3452(3) 0.0266(8) Uani 1 2 d S . . C14 C 0.39712(12) 0.4012(2) 0.3995(2) 0.0251(6) Uani 1 1 d . . . C15 C 0.43039(13) 0.4042(2) 0.4985(2) 0.0285(6) Uani 1 1 d . . . H15 H 0.4425 0.3415 0.5338 0.034 Uiso 1 1 calc R . . C16 C 0.44908(19) 0.5000 0.5549(3) 0.0291(9) Uani 1 2 d S . . C17 C 0.40134(16) 0.1685(2) 0.4125(2) 0.0386(7) Uani 1 1 d . . . H17A H 0.3812 0.1059 0.3752 0.058 Uiso 1 1 calc R . . H17B H 0.3885 0.1803 0.4598 0.058 Uiso 1 1 calc R . . H17C H 0.4478 0.1616 0.4483 0.058 Uiso 1 1 calc R . . C18 C 0.41559(14) 0.2767(3) 0.2564(2) 0.0356(7) Uani 1 1 d . . . H18A H 0.4619 0.2779 0.3032 0.053 Uiso 1 1 calc R . . H18B H 0.4026 0.3367 0.2132 0.053 Uiso 1 1 calc R . . H18C H 0.4035 0.2145 0.2164 0.053 Uiso 1 1 calc R . . C19 C 0.0364(4) 1.0000 -0.0451(5) 0.079(2) Uani 1 2 d S . . C20 C 0.0661(5) 1.0000 0.0561(5) 0.092(3) Uani 1 2 d S . . H20 H 0.1114 1.0000 0.0969 0.110 Uiso 1 2 calc SR . . C21 C 0.0291(4) 1.0000 0.1002(5) 0.085(2) Uani 1 2 d S . . H21 H 0.0508 1.0000 0.1702 0.102 Uiso 1 2 calc SR . . C22 C 0.0759(4) 1.0000 -0.0924(5) 0.098(3) Uani 1 2 d S . . H22A H 0.1117 0.9525 -0.0567 0.147 Uiso 0.50 1 calc PR . . H22B H 0.0922 1.0689 -0.0893 0.147 Uiso 0.50 1 calc PR . . H22C H 0.0489 0.9786 -0.1616 0.147 Uiso 0.50 1 calc PR . . C23 C 0.2084(6) 0.5000 0.8886(7) 0.129(5) Uani 1 2 d S . . C24 C 0.2318(7) 0.5000 0.9869(10) 0.143(6) Uani 1 2 d S . . H24 H 0.2766 0.5000 1.0332 0.171 Uiso 1 2 calc SR . . C25 C 0.1908(7) 0.5000 1.0194(7) 0.147(6) Uani 1 2 d S . . H25 H 0.2075 0.5000 1.0883 0.176 Uiso 1 2 calc SR . . C26 C 0.1231(6) 0.5000 0.9504(6) 0.114(4) Uani 1 2 d S . . C27 C 0.1023(6) 0.5000 0.8523(5) 0.118(4) Uani 1 2 d S . . H27 H 0.0577 0.5000 0.8040 0.142 Uiso 1 2 calc SR . . C28 C 0.1461(6) 0.5000 0.8217(7) 0.114(4) Uani 1 2 d S . . H28 H 0.1309 0.5000 0.7533 0.137 Uiso 1 2 calc SR . . C29 C 0.2560(6) 0.5000 0.8540(9) 0.141(4) Uani 1 2 d S . . H29A H 0.2357 0.4683 0.7885 0.211 Uiso 0.50 1 calc PR . . H29B H 0.2943 0.4613 0.9011 0.211 Uiso 0.50 1 calc PR . . H29C H 0.2679 0.5704 0.8504 0.211 Uiso 0.50 1 calc PR . . C30 C 0.0776(7) 0.5000 0.9865(6) 0.149(5) Uani 1 2 d S . . H30A H 0.0368 0.5303 0.9358 0.224 Uiso 0.50 1 calc PR . . H30B H 0.0961 0.5400 1.0475 0.224 Uiso 0.50 1 calc PR . . H30C H 0.0705 0.4297 0.9993 0.224 Uiso 0.50 1 calc PR . . O1 O 0.27146(9) 0.28711(16) 0.37008(14) 0.0333(5) Uani 1 1 d . . . O2 O 0.16234(11) 0.2375(2) -0.01517(16) 0.0465(6) Uani 1 1 d . . . O3 O 0.11512(19) 0.5000 0.2091(2) 0.0503(9) Uani 1 2 d S . . O4 O 0.21825(18) 0.5000 0.5960(2) 0.0478(9) Uani 1 2 d S . . O5 O 0.34525(15) 0.5000 0.2538(2) 0.0385(7) Uani 1 2 d S . . O6 O 0.47939(16) 0.5000 0.6454(2) 0.0446(8) Uani 1 2 d S . . Si1 Si 0.12777(4) 0.27928(6) 0.27578(6) 0.0298(2) Uani 1 1 d . . . Si2 Si 0.37539(4) 0.27896(6) 0.32535(6) 0.0264(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0298(14) 0.0214(13) 0.0236(15) -0.0012(11) 0.0142(12) -0.0020(11) C2 0.0283(14) 0.0235(14) 0.0266(15) 0.0005(11) 0.0152(12) 0.0005(11) C3 0.0281(15) 0.0343(16) 0.0297(16) -0.0038(13) 0.0149(13) -0.0034(12) C4 0.0342(16) 0.0374(17) 0.0244(16) -0.0050(12) 0.0150(13) -0.0016(13) C5 0.0315(15) 0.0352(16) 0.0267(15) -0.0027(12) 0.0188(13) -0.0017(12) C6 0.0273(14) 0.0252(14) 0.0238(14) -0.0004(11) 0.0137(12) 0.0003(11) C7 0.053(2) 0.0353(18) 0.052(2) 0.0064(15) 0.0368(19) 0.0008(15) C8 0.0362(17) 0.045(2) 0.056(2) -0.0004(17) 0.0282(17) 0.0005(15) C9 0.041(2) 0.032(2) 0.033(2) 0.000 0.026(2) 0.000 C10 0.0377(16) 0.0280(15) 0.0378(17) 0.0019(12) 0.0282(15) 0.0025(12) C11 0.0446(18) 0.0328(16) 0.0354(17) 0.0046(13) 0.0280(16) 0.0033(13) C12 0.041(3) 0.040(3) 0.039(3) 0.000 0.027(2) 0.000 C13 0.024(2) 0.032(2) 0.024(2) 0.000 0.0127(18) 0.000 C14 0.0204(13) 0.0305(15) 0.0236(14) 0.0002(11) 0.0114(12) -0.0003(11) C15 0.0267(14) 0.0331(16) 0.0257(15) 0.0043(12) 0.0140(13) 0.0024(12) C16 0.027(2) 0.037(2) 0.019(2) 0.000 0.0091(18) 0.000 C17 0.0388(18) 0.0354(18) 0.0367(18) 0.0058(14) 0.0171(15) 0.0048(14) C18 0.0323(15) 0.0433(18) 0.0356(17) -0.0095(14) 0.0211(14) -0.0058(14) C19 0.120(6) 0.031(3) 0.038(3) 0.000 0.010(4) 0.000 C20 0.123(7) 0.055(4) 0.047(4) 0.000 0.012(4) 0.000 C21 0.123(7) 0.045(4) 0.040(4) 0.000 0.013(4) 0.000 C22 0.150(8) 0.068(5) 0.055(4) 0.000 0.041(5) 0.000 C23 0.164(10) 0.029(3) 0.065(6) 0.000 -0.023(6) 0.000 C24 0.185(14) 0.048(5) 0.101(10) 0.000 0.016(9) 0.000 C25 0.200(13) 0.032(4) 0.050(5) 0.000 -0.037(7) 0.000 C26 0.194(11) 0.030(3) 0.048(5) 0.000 0.019(6) 0.000 C27 0.186(10) 0.034(4) 0.042(4) 0.000 0.001(5) 0.000 C28 0.202(12) 0.049(4) 0.067(6) 0.000 0.057(8) 0.000 C29 0.182(11) 0.041(5) 0.178(12) 0.000 0.082(10) 0.000 C30 0.255(15) 0.056(5) 0.047(5) 0.000 0.022(7) 0.000 O1 0.0339(11) 0.0438(13) 0.0231(11) 0.0004(9) 0.0160(9) 0.0002(9) O2 0.0379(12) 0.0720(17) 0.0245(12) -0.0117(11) 0.0135(10) -0.0089(12) O3 0.086(3) 0.0352(18) 0.036(2) 0.000 0.037(2) 0.000 O4 0.070(2) 0.047(2) 0.0313(19) 0.000 0.0303(18) 0.000 O5 0.0489(19) 0.0339(17) 0.0216(16) 0.000 0.0117(15) 0.000 O6 0.051(2) 0.047(2) 0.0250(17) 0.000 0.0137(16) 0.000 Si1 0.0338(5) 0.0271(4) 0.0364(5) 0.0009(4) 0.0240(4) -0.0001(3) Si2 0.0253(4) 0.0291(4) 0.0252(4) -0.0011(3) 0.0139(3) -0.0001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.224(3) . ? C1 C2 1.492(4) . ? C1 C6 1.498(4) . ? C2 C3 1.339(4) . ? C2 Si1 1.885(3) . ? C3 C4 1.472(4) . ? C4 O2 1.229(4) . ? C4 C5 1.475(4) . ? C5 C6 1.347(4) . ? C6 Si2 1.874(3) . ? C7 Si1 1.863(3) . ? C8 Si1 1.859(3) . ? C9 O3 1.228(5) . ? C9 C10 1.494(4) 6_565 ? C9 C10 1.494(4) . ? C10 C11 1.343(4) . ? C10 Si1 1.889(3) . ? C11 C12 1.478(4) . ? C12 O4 1.234(5) . ? C12 C11 1.478(4) 6_565 ? C13 O5 1.237(5) . ? C13 C14 1.489(3) 6_565 ? C13 C14 1.489(3) . ? C14 C15 1.340(4) . ? C14 Si2 1.892(3) . ? C15 C16 1.469(4) . ? C16 O6 1.225(5) . ? C16 C15 1.469(4) 6_565 ? C17 Si2 1.870(3) . ? C18 Si2 1.848(3) . ? C19 C21 1.374(11) 5_575 ? C19 C20 1.376(9) . ? C19 C22 1.530(11) . ? C20 C21 1.431(12) . ? C21 C19 1.374(11) 5_575 ? C23 C28 1.327(14) . ? C23 C24 1.357(15) . ? C23 C29 1.556(15) . ? C24 C25 1.374(17) . ? C25 C26 1.432(16) . ? C26 C27 1.368(11) . ? C26 C30 1.524(15) . ? C27 C28 1.416(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.6(2) . . ? O1 C1 C6 119.7(2) . . ? C2 C1 C6 120.7(2) . . ? C3 C2 C1 117.8(2) . . ? C3 C2 Si1 124.3(2) . . ? C1 C2 Si1 117.91(19) . . ? C2 C3 C4 123.1(3) . . ? O2 C4 C3 121.2(3) . . ? O2 C4 C5 120.8(3) . . ? C3 C4 C5 118.0(3) . . ? C6 C5 C4 122.0(3) . . ? C5 C6 C1 118.3(2) . . ? C5 C6 Si2 123.9(2) . . ? C1 C6 Si2 117.70(19) . . ? O3 C9 C10 119.21(18) . 6_565 ? O3 C9 C10 119.21(18) . . ? C10 C9 C10 121.6(4) 6_565 . ? C11 C10 C9 117.5(3) . . ? C11 C10 Si1 124.5(2) . . ? C9 C10 Si1 118.0(2) . . ? C10 C11 C12 122.7(3) . . ? O4 C12 C11 121.09(19) . . ? O4 C12 C11 121.09(19) . 6_565 ? C11 C12 C11 117.8(4) . 6_565 ? O5 C13 C14 119.62(17) . 6_565 ? O5 C13 C14 119.62(17) . . ? C14 C13 C14 120.8(3) 6_565 . ? C15 C14 C13 117.9(3) . . ? C15 C14 Si2 123.8(2) . . ? C13 C14 Si2 118.3(2) . . ? C14 C15 C16 123.0(3) . . ? O6 C16 C15 121.33(17) . . ? O6 C16 C15 121.33(17) . 6_565 ? C15 C16 C15 117.3(3) . 6_565 ? C21 C19 C20 117.1(8) 5_575 . ? C21 C19 C22 122.5(7) 5_575 . ? C20 C19 C22 120.5(8) . . ? C19 C20 C21 120.4(8) . . ? C19 C21 C20 122.5(7) 5_575 . ? C28 C23 C24 121.7(15) . . ? C28 C23 C29 119.4(11) . . ? C24 C23 C29 118.9(12) . . ? C23 C24 C25 120.0(14) . . ? C24 C25 C26 120.6(11) . . ? C27 C26 C25 116.8(13) . . ? C27 C26 C30 122.6(11) . . ? C25 C26 C30 120.6(10) . . ? C26 C27 C28 120.9(11) . . ? C23 C28 C27 120.0(11) . . ? C8 Si1 C7 111.11(16) . . ? C8 Si1 C2 108.33(14) . . ? C7 Si1 C2 109.82(13) . . ? C8 Si1 C10 109.97(15) . . ? C7 Si1 C10 109.03(14) . . ? C2 Si1 C10 108.54(12) . . ? C18 Si2 C17 110.89(15) . . ? C18 Si2 C6 110.32(13) . . ? C17 Si2 C6 109.52(14) . . ? C18 Si2 C14 109.10(13) . . ? C17 Si2 C14 108.45(14) . . ? C6 Si2 C14 108.52(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 C14 C15 C16 -0.7(4) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C4 C5 C6 C1 -1.5(4) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.601 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.071 #===END