data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Robert Haddon' _publ_contact_author_name 'Robert Haddon' _publ_contact_author_address ; Riverside California United States CA 92521-0403 ; _publ_contact_author_email haddon@ucr.edu # Attachment '- (18)rh141_0m.cif' data_rh141_0m _database_code_depnum_ccdc_archive 'CCDC 785944' #TrackingRef '- (18)rh141_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.83 H41.74 N2.91 O12 Si' _chemical_formula_weight 913.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.357(2) _cell_length_b 12.711(2) _cell_length_c 14.644(3) _cell_angle_alpha 91.192(3) _cell_angle_beta 104.382(3) _cell_angle_gamma 101.723(3) _cell_volume 2175.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2232 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 21.79 _exptl_crystal_description 'thin plate frag' _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9741 _exptl_absorpt_correction_T_max 0.9987 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20412 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 20.39 _reflns_number_total 4292 _reflns_number_gt 2587 _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^)+(0.0641P)^2^+2.9307P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4292 _refine_ls_number_parameters 613 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.041 _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 Si1 Si 0.35367(15) 0.34288(13) 0.28001(12) 0.0321(5) Uani 1 1 d . . . O1 O 0.4471(3) 0.3500(3) 0.3926(3) 0.0309(10) Uani 1 1 d . . . C1 C 0.4979(5) 0.2737(5) 0.4309(4) 0.0302(16) Uani 1 1 d . . . C2 C 0.5425(5) 0.2816(5) 0.5289(4) 0.0326(16) Uani 1 1 d . . . H2 H 0.5351 0.3409 0.5657 0.039 Uiso 1 1 calc R . . C3 C 0.5971(5) 0.2051(5) 0.5733(4) 0.0321(16) Uani 1 1 d . . . C3A C 0.6145(5) 0.1172(5) 0.5192(4) 0.0304(16) Uani 1 1 d . . . O3" O 0.6390(3) 0.2048(3) 0.6683(3) 0.0396(11) Uani 1 1 d . . . C3" C 0.6017(6) 0.2730(5) 0.7284(4) 0.0435(18) Uani 1 1 d . . . H3"1 H 0.6320 0.3487 0.7202 0.065 Uiso 1 1 calc R . . H3"2 H 0.6297 0.2582 0.7945 0.065 Uiso 1 1 calc R . . H3"3 H 0.5179 0.2587 0.7113 0.065 Uiso 1 1 calc R . . C4 C 0.6721(5) 0.0386(5) 0.5613(5) 0.0377(17) Uani 1 1 d . . . H4 H 0.7005 0.0421 0.6280 0.045 Uiso 1 1 calc R . . C5 C 0.6875(5) -0.0436(5) 0.5059(5) 0.0366(17) Uani 1 1 d . . . H5 H 0.7255 -0.0968 0.5353 0.044 Uiso 1 1 calc R . . C6 C 0.6494(5) -0.0495(5) 0.4104(5) 0.0370(17) Uani 1 1 d . . . H6 H 0.6626 -0.1062 0.3741 0.044 Uiso 1 1 calc R . . C6A C 0.5915(5) 0.0251(5) 0.3644(5) 0.0314(16) Uani 1 1 d . . . C7 C 0.5501(5) 0.0227(5) 0.2645(5) 0.0365(17) Uani 1 1 d . . . O7" O 0.5762(4) -0.0583(3) 0.2162(3) 0.0473(12) Uani 1 1 d . . . C7" C 0.5398(8) -0.0635(6) 0.1149(5) 0.078(3) Uani 1 1 d . . . H7"1 H 0.4560 -0.0788 0.0945 0.116 Uiso 1 1 calc R . . H7"2 H 0.5678 -0.1208 0.0883 0.116 Uiso 1 1 calc R . . H7"3 H 0.5706 0.0057 0.0927 0.116 Uiso 1 1 calc R . . C8 C 0.4891(5) 0.0946(5) 0.2222(4) 0.0346(16) Uani 1 1 d . . . H8 H 0.4605 0.0888 0.1554 0.041 Uiso 1 1 calc R . . C9 C 0.4679(5) 0.1775(5) 0.2766(4) 0.0301(16) Uani 1 1 d . . . C9A C 0.5115(5) 0.1871(4) 0.3752(4) 0.0267(15) Uani 1 1 d . . . C9B C 0.5719(5) 0.1100(5) 0.4195(5) 0.0308(16) Uani 1 1 d . . . O9 O 0.4088(3) 0.2444(3) 0.2312(3) 0.0345(11) Uani 1 1 d . . . O11 O 0.2553(3) 0.2381(3) 0.3113(3) 0.0338(11) Uani 1 1 d . . . C11 C 0.1565(5) 0.2440(5) 0.3283(4) 0.0283(15) Uani 1 1 d . . . C12 C 0.0840(6) 0.1461(5) 0.3382(4) 0.0355(17) Uani 1 1 d . . . H12 H 0.1063 0.0798 0.3308 0.043 Uiso 1 1 calc R . . C13 C -0.0174(6) 0.1461(5) 0.3584(4) 0.0412(18) Uani 1 1 d . . . C13A C -0.0570(6) 0.2432(5) 0.3673(5) 0.0423(18) Uani 1 1 d . . . O13" O -0.0910(4) 0.0552(3) 0.3713(3) 0.0568(14) Uani 1 1 d . . . C13" C -0.0545(6) -0.0445(5) 0.3682(5) 0.065(2) Uani 1 1 d . . . H13A H -0.0479 -0.0611 0.3044 0.098 Uiso 1 1 calc R . . H13B H -0.1106 -0.1023 0.3844 0.098 Uiso 1 1 calc R . . H13C H 0.0200 -0.0383 0.4136 0.098 Uiso 1 1 calc R . . C14 C -0.1614(6) 0.2443(6) 0.3843(5) 0.062(2) Uani 1 1 d . . . H14 H -0.2101 0.1780 0.3900 0.074 Uiso 1 1 calc R . . C15 C -0.1969(6) 0.3383(6) 0.3932(6) 0.068(2) Uani 1 1 d . . . H15 H -0.2699 0.3369 0.4039 0.081 Uiso 1 1 calc R . . C16 C -0.1260(6) 0.4350(6) 0.3865(5) 0.063(2) Uani 1 1 d . . . H16 H -0.1497 0.5004 0.3944 0.076 Uiso 1 1 calc R . . C16A C -0.0194(5) 0.4382(5) 0.3681(5) 0.0420(18) Uani 1 1 d . . . C17 C 0.0570(6) 0.5376(5) 0.3613(5) 0.0440(18) Uani 1 1 d . . . O17" O 0.0137(4) 0.6262(3) 0.3714(4) 0.0639(15) Uani 1 1 d . . . C17" C 0.0830(6) 0.7294(5) 0.3675(6) 0.081(3) Uani 1 1 d . . . H17A H 0.1546 0.7397 0.4173 0.121 Uiso 1 1 calc R . . H17B H 0.0420 0.7855 0.3767 0.121 Uiso 1 1 calc R . . H17C H 0.1002 0.7341 0.3056 0.121 Uiso 1 1 calc R . . C18 C 0.1610(5) 0.5388(5) 0.3461(4) 0.0355(17) Uani 1 1 d . . . H18 H 0.2106 0.6059 0.3438 0.043 Uiso 1 1 calc R . . C19 C 0.1965(6) 0.4433(4) 0.3338(4) 0.0311(16) Uani 1 1 d . . . C19A C 0.1235(5) 0.3434(4) 0.3381(4) 0.0286(15) Uani 1 1 d . . . C19B C 0.0166(5) 0.3419(5) 0.3573(4) 0.0353(17) Uani 1 1 d . . . O19 O 0.2998(4) 0.4490(3) 0.3198(3) 0.0336(11) Uani 1 1 d . . . O21 O 0.4596(3) 0.4439(3) 0.2507(3) 0.0346(11) Uani 1 1 d . . . C21 C 0.4525(6) 0.4979(4) 0.1752(5) 0.0349(17) Uani 1 1 d . . . C22 C 0.5505(5) 0.5762(4) 0.1709(4) 0.0333(16) Uani 1 1 d . . . H22 H 0.6170 0.5887 0.2224 0.040 Uiso 1 1 calc R . . C23 C 0.5496(6) 0.6337(5) 0.0929(5) 0.0376(17) Uani 1 1 d . . . C23A C 0.4494(6) 0.6202(5) 0.0145(5) 0.0355(17) Uani 1 1 d . . . O23" O 0.6411(4) 0.7072(3) 0.0818(3) 0.0467(12) Uani 1 1 d . . . C23" C 0.7414(6) 0.7330(5) 0.1602(5) 0.054(2) Uani 1 1 d . . . H23A H 0.7218 0.7632 0.2146 0.082 Uiso 1 1 calc R . . H23B H 0.8008 0.7859 0.1426 0.082 Uiso 1 1 calc R . . H23C H 0.7696 0.6674 0.1770 0.082 Uiso 1 1 calc R . . C24 C 0.4467(6) 0.6767(5) -0.0658(5) 0.0427(18) Uani 1 1 d . . . H24 H 0.5134 0.7266 -0.0705 0.051 Uiso 1 1 calc R . . C25 C 0.3505(7) 0.6618(5) -0.1377(5) 0.053(2) Uani 1 1 d . . . H25 H 0.3512 0.7006 -0.1924 0.064 Uiso 1 1 calc R . . C26 C 0.2509(6) 0.5910(5) -0.1330(5) 0.0497(19) Uani 1 1 d . . . H26 H 0.1835 0.5831 -0.1831 0.060 Uiso 1 1 calc R . . C26A C 0.2502(6) 0.5313(5) -0.0543(5) 0.0409(18) Uani 1 1 d . . . C27 C 0.1498(6) 0.4525(5) -0.0471(5) 0.0452(18) Uani 1 1 d . . . O27" O 0.0556(4) 0.4491(4) -0.1184(3) 0.0591(14) Uani 1 1 d . . . C27" C -0.0479(6) 0.3766(6) -0.1112(5) 0.060(2) Uani 1 1 d . . . H27A H -0.0407 0.3019 -0.1204 0.090 Uiso 1 1 calc R . . H27B H -0.1130 0.3900 -0.1598 0.090 Uiso 1 1 calc R . . H27C H -0.0600 0.3886 -0.0485 0.090 Uiso 1 1 calc R . . C28 C 0.1548(5) 0.3894(5) 0.0276(4) 0.0368(17) Uani 1 1 d . . . H28 H 0.0893 0.3363 0.0294 0.044 Uiso 1 1 calc R . . C29 C 0.2544(5) 0.4011(5) 0.1017(4) 0.0333(16) Uani 1 1 d . . . C29A C 0.3519(5) 0.4810(4) 0.1001(4) 0.0289(15) Uani 1 1 d . . . C29B C 0.3498(6) 0.5446(4) 0.0210(4) 0.0325(16) Uani 1 1 d . . . O29 O 0.2528(3) 0.3362(3) 0.1694(3) 0.0337(11) Uani 1 1 d . . . N1# N 0.7680(6) 0.7260(5) 0.4043(5) 0.071(2) Uani 1 1 d U . . C2# C 0.7182(6) 0.6481(6) 0.4243(5) 0.0469(19) Uani 1 1 d U . . C3# C 0.6568(5) 0.5489(5) 0.4475(5) 0.0450(18) Uani 1 1 d U . . H3#1 H 0.6007 0.5120 0.3905 0.068 Uiso 1 1 calc R . . H3#2 H 0.6171 0.5636 0.4950 0.068 Uiso 1 1 calc R . . H3#3 H 0.7104 0.5031 0.4729 0.068 Uiso 1 1 calc R . . N1' N -0.0108(8) -0.0781(7) 0.1187(7) 0.126(3) Uani 1 1 d U A 2 C2' C 0.0767(9) -0.0204(7) 0.1211(6) 0.090(3) Uani 1 1 d U A 2 C3' C 0.1771(7) 0.0556(6) 0.1158(6) 0.093(3) Uani 1 1 d U A 2 H3'1 H 0.1711 0.0724 0.0500 0.140 Uiso 1 1 calc R A 2 H3'2 H 0.2445 0.0247 0.1391 0.140 Uiso 1 1 calc R A 2 H3'3 H 0.1845 0.1216 0.1547 0.140 Uiso 1 1 calc R A 2 N1* N 0.7597(8) 0.1826(7) -0.0408(6) 0.092(3) Uani 0.91 1 d PU B 2 C2* C 0.8072(10) 0.1770(9) 0.0376(8) 0.099(4) Uani 0.91 1 d PU B 2 C3* C 0.8634(13) 0.1673(12) 0.1271(8) 0.199(8) Uani 0.91 1 d PU B 2 H3*1 H 0.8382 0.0940 0.1444 0.298 Uiso 0.91 1 calc PR B 2 H3*2 H 0.8470 0.2191 0.1696 0.298 Uiso 0.91 1 calc PR B 2 H3*3 H 0.9458 0.1817 0.1326 0.298 Uiso 0.91 1 calc PR B 2 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 Si1 0.0383(12) 0.0226(10) 0.0353(11) 0.0033(8) 0.0114(9) 0.0038(8) O1 0.042(3) 0.020(2) 0.029(3) 0.005(2) 0.007(2) 0.006(2) C1 0.036(4) 0.026(4) 0.026(4) 0.005(3) 0.008(3) -0.003(3) C2 0.034(4) 0.021(4) 0.042(5) 0.003(3) 0.013(4) 0.000(3) C3 0.037(4) 0.022(4) 0.033(5) 0.003(3) 0.007(3) -0.001(3) C3A 0.024(4) 0.023(4) 0.043(5) 0.008(4) 0.008(3) 0.002(3) O3" 0.054(3) 0.032(3) 0.032(3) 0.004(2) 0.007(2) 0.013(2) C3" 0.058(5) 0.037(4) 0.036(4) -0.004(3) 0.013(4) 0.009(3) C4 0.036(4) 0.035(4) 0.041(4) 0.003(4) 0.009(3) 0.007(3) C5 0.030(4) 0.028(4) 0.048(5) 0.003(4) 0.007(4) 0.003(3) C6 0.036(4) 0.024(4) 0.048(5) 0.001(4) 0.012(4) 0.000(3) C6A 0.031(4) 0.019(4) 0.046(5) 0.006(4) 0.014(4) 0.003(3) C7 0.039(4) 0.023(4) 0.045(5) 0.000(4) 0.013(4) 0.000(3) O7" 0.073(3) 0.032(3) 0.042(3) -0.001(2) 0.017(3) 0.022(2) C7" 0.140(8) 0.058(5) 0.048(6) -0.001(4) 0.026(5) 0.052(5) C8 0.044(4) 0.022(4) 0.037(4) 0.004(4) 0.010(3) 0.005(3) C9 0.030(4) 0.019(4) 0.040(5) 0.001(4) 0.012(4) -0.002(3) C9A 0.031(4) 0.014(3) 0.032(4) 0.000(3) 0.008(3) -0.002(3) C9B 0.028(4) 0.020(4) 0.042(5) 0.002(3) 0.011(3) -0.004(3) O9 0.044(3) 0.026(2) 0.035(3) 0.001(2) 0.012(2) 0.010(2) O11 0.038(3) 0.023(2) 0.040(3) 0.0072(19) 0.013(2) -0.001(2) C11 0.025(4) 0.027(4) 0.031(4) 0.003(3) 0.007(3) 0.000(3) C12 0.044(5) 0.022(4) 0.038(4) -0.002(3) 0.011(4) 0.000(3) C13 0.040(5) 0.030(4) 0.050(5) -0.001(3) 0.019(4) -0.009(4) C13A 0.036(5) 0.031(4) 0.062(5) -0.006(3) 0.021(4) 0.001(4) O13" 0.056(3) 0.027(3) 0.089(4) 0.002(3) 0.033(3) -0.003(3) C13" 0.069(6) 0.028(4) 0.102(7) 0.001(4) 0.040(5) -0.002(4) C14 0.052(6) 0.038(5) 0.094(6) -0.017(4) 0.033(5) -0.007(4) C15 0.040(5) 0.051(5) 0.111(7) -0.023(5) 0.030(5) -0.001(5) C16 0.038(5) 0.041(5) 0.102(7) -0.026(4) 0.012(4) -0.001(4) C16A 0.029(4) 0.034(5) 0.058(5) -0.006(3) 0.009(4) -0.001(4) C17 0.039(5) 0.029(4) 0.061(5) -0.003(3) 0.000(4) 0.017(4) O17" 0.040(3) 0.032(3) 0.116(5) -0.007(3) 0.013(3) 0.010(3) C17" 0.074(6) 0.023(4) 0.140(8) -0.007(5) 0.019(6) 0.009(4) C18 0.032(5) 0.021(4) 0.048(4) 0.004(3) 0.001(3) 0.006(3) C19 0.041(5) 0.015(4) 0.031(4) 0.004(3) 0.002(3) 0.001(3) C19A 0.031(4) 0.024(4) 0.029(4) 0.003(3) 0.006(3) 0.006(3) C19B 0.035(5) 0.030(4) 0.033(4) -0.002(3) 0.001(3) 0.002(4) O19 0.037(3) 0.022(2) 0.042(3) 0.0054(19) 0.013(2) 0.002(2) O21 0.038(3) 0.031(2) 0.032(3) 0.005(2) 0.010(2) 0.000(2) C21 0.055(5) 0.017(4) 0.037(5) -0.001(3) 0.019(4) 0.007(3) C22 0.039(4) 0.021(4) 0.038(4) -0.003(3) 0.015(3) -0.003(3) C23 0.050(5) 0.021(4) 0.047(5) -0.002(4) 0.025(4) 0.003(3) C23A 0.046(5) 0.022(4) 0.043(5) 0.004(4) 0.013(4) 0.016(4) O23" 0.056(3) 0.032(3) 0.053(3) 0.000(2) 0.026(3) -0.003(2) C23" 0.060(5) 0.045(5) 0.051(5) -0.002(4) 0.019(4) -0.013(4) C24 0.060(5) 0.030(4) 0.045(5) 0.011(4) 0.017(4) 0.019(4) C25 0.065(6) 0.047(5) 0.060(6) 0.036(4) 0.026(5) 0.024(4) C26 0.047(5) 0.050(5) 0.059(5) 0.023(4) 0.017(4) 0.021(4) C26A 0.057(5) 0.028(4) 0.044(5) 0.013(4) 0.018(4) 0.017(4) C27 0.055(5) 0.041(4) 0.042(5) 0.008(4) 0.008(4) 0.021(4) O27" 0.052(3) 0.067(3) 0.052(3) 0.024(3) 0.004(3) 0.011(3) C27" 0.039(5) 0.060(5) 0.074(6) 0.019(4) 0.000(4) 0.011(4) C28 0.042(5) 0.026(4) 0.041(5) 0.004(4) 0.008(4) 0.007(3) C29 0.038(5) 0.033(4) 0.030(4) -0.004(4) 0.010(4) 0.011(4) C29A 0.031(4) 0.024(4) 0.030(4) -0.002(3) 0.003(4) 0.008(3) C29B 0.051(5) 0.018(3) 0.030(4) 0.006(3) 0.009(4) 0.010(3) O29 0.039(3) 0.024(2) 0.034(3) 0.009(2) 0.005(2) -0.0001(19) N1# 0.078(5) 0.046(4) 0.086(5) 0.010(4) 0.023(4) 0.003(4) C2# 0.055(5) 0.037(4) 0.048(5) 0.003(4) 0.013(4) 0.010(4) C3# 0.047(4) 0.034(4) 0.053(5) 0.007(3) 0.014(4) 0.005(3) N1' 0.112(7) 0.108(7) 0.154(8) -0.003(6) 0.059(7) -0.013(5) C2' 0.099(8) 0.077(7) 0.091(7) -0.028(5) 0.044(6) -0.011(5) C3' 0.067(6) 0.075(6) 0.118(8) -0.052(6) 0.028(5) -0.027(4) N1* 0.108(7) 0.088(6) 0.085(6) 0.005(6) 0.019(5) 0.038(5) C2* 0.125(10) 0.106(8) 0.073(7) -0.010(7) 0.008(7) 0.062(7) C3* 0.256(17) 0.241(16) 0.094(8) -0.050(10) -0.083(10) 0.206(14) _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 Si1 O1 1.751(4) . ? Si1 O9 1.759(4) . ? Si1 O11 1.763(4) . ? Si1 O19 1.768(4) . ? Si1 O29 1.770(4) . ? Si1 O21 1.780(4) . ? O1 C1 1.321(7) . ? C1 C2 1.398(8) . ? C1 C9A 1.417(8) . ? C2 C3 1.378(8) . ? C2 H2 0.9500 . ? C3 O3" 1.359(7) . ? C3 C3A 1.438(8) . ? C3A C4 1.408(8) . ? C3A C9B 1.417(8) . ? O3" C3" 1.439(7) . ? C3" H3"1 0.9800 . ? C3" H3"2 0.9800 . ? C3" H3"3 0.9800 . ? C4 C5 1.381(8) . ? C4 H4 0.9500 . ? C5 C6 1.355(8) . ? C5 H5 0.9500 . ? C6 C6A 1.389(8) . ? C6 H6 0.9500 . ? C6A C7 1.423(8) . ? C6A C9B 1.429(8) . ? C7 C8 1.363(8) . ? C7 O7" 1.373(7) . ? O7" C7" 1.435(8) . ? C7" H7"1 0.9800 . ? C7" H7"2 0.9800 . ? C7" H7"3 0.9800 . ? C8 C9 1.413(8) . ? C8 H8 0.9500 . ? C9 O9 1.317(7) . ? C9 C9A 1.403(8) . ? C9A C9B 1.422(8) . ? O11 C11 1.321(6) . ? C11 C12 1.411(8) . ? C11 C19A 1.419(8) . ? C12 C13 1.358(8) . ? C12 H12 0.9500 . ? C13 O13" 1.366(7) . ? C13 C13A 1.431(9) . ? C13A C14 1.375(9) . ? C13A C19B 1.426(8) . ? O13" C13" 1.433(7) . ? C13" H13A 0.9800 . ? C13" H13B 0.9800 . ? C13" H13C 0.9800 . ? C14 C15 1.368(9) . ? C14 H14 0.9500 . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 C16A 1.401(9) . ? C16 H16 0.9500 . ? C16A C19B 1.403(8) . ? C16A C17 1.437(8) . ? C17 C18 1.354(8) . ? C17 O17" 1.362(7) . ? O17" C17" 1.425(7) . ? C17" H17A 0.9800 . ? C17" H17B 0.9800 . ? C17" H17C 0.9800 . ? C18 C19 1.395(8) . ? C18 H18 0.9500 . ? C19 O19 1.331(7) . ? C19 C19A 1.413(8) . ? C19A C19B 1.414(8) . ? O21 C21 1.307(7) . ? C21 C29A 1.416(8) . ? C21 C22 1.418(8) . ? C22 C23 1.368(8) . ? C22 H22 0.9500 . ? C23 O23" 1.359(7) . ? C23 C23A 1.442(9) . ? C23A C24 1.388(8) . ? C23A C29B 1.424(8) . ? O23" C23" 1.440(7) . ? C23" H23A 0.9800 . ? C23" H23B 0.9800 . ? C23" H23C 0.9800 . ? C24 C25 1.355(9) . ? C24 H24 0.9500 . ? C25 C26 1.388(9) . ? C25 H25 0.9500 . ? C26 C26A 1.392(8) . ? C26 H26 0.9500 . ? C26A C29B 1.412(8) . ? C26A C27 1.456(9) . ? C27 O27" 1.350(7) . ? C27 C28 1.365(8) . ? O27" C27" 1.445(7) . ? C27" H27A 0.9800 . ? C27" H27B 0.9800 . ? C27" H27C 0.9800 . ? C28 C29 1.403(8) . ? C28 H28 0.9500 . ? C29 O29 1.304(7) . ? C29 C29A 1.414(8) . ? C29A C29B 1.424(8) . ? N1# C2# 1.139(8) . ? C2# C3# 1.428(9) . ? C3# H3#1 0.9800 . ? C3# H3#2 0.9800 . ? C3# H3#3 0.9800 . ? N1' C2' 1.169(10) . ? C2' C3' 1.429(11) . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? N1* C2* 1.163(11) . ? C2* C3* 1.343(13) . ? C3* H3*1 0.9800 . ? C3* H3*2 0.9800 . ? C3* H3*3 0.9800 . ? 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 Si1 O9 94.8(2) . . ? O1 Si1 O11 90.40(19) . . ? O9 Si1 O11 88.40(19) . . ? O1 Si1 O19 88.72(19) . . ? O9 Si1 O19 174.6(2) . . ? O11 Si1 O19 95.75(19) . . ? O1 Si1 O29 176.7(2) . . ? O9 Si1 O29 87.8(2) . . ? O11 Si1 O29 87.53(19) . . ? O19 Si1 O29 88.90(19) . . ? O1 Si1 O21 87.47(19) . . ? O9 Si1 O21 88.92(19) . . ? O11 Si1 O21 176.4(2) . . ? O19 Si1 O21 87.07(19) . . ? O29 Si1 O21 94.73(19) . . ? C1 O1 Si1 127.0(4) . . ? O1 C1 C2 118.3(5) . . ? O1 C1 C9A 121.9(5) . . ? C2 C1 C9A 119.7(6) . . ? C3 C2 C1 121.3(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? O3" C3 C2 124.9(6) . . ? O3" C3 C3A 114.5(5) . . ? C2 C3 C3A 120.6(6) . . ? C4 C3A C9B 119.0(6) . . ? C4 C3A C3 122.6(6) . . ? C9B C3A C3 118.4(6) . . ? C3 O3" C3" 117.8(5) . . ? O3" C3" H3"1 109.5 . . ? O3" C3" H3"2 109.5 . . ? H3"1 C3" H3"2 109.5 . . ? O3" C3" H3"3 109.5 . . ? H3"1 C3" H3"3 109.5 . . ? H3"2 C3" H3"3 109.5 . . ? C5 C4 C3A 120.3(6) . . ? C5 C4 H4 119.9 . . ? C3A C4 H4 119.9 . . ? C6 C5 C4 121.0(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C6A 121.6(6) . . ? C5 C6 H6 119.2 . . ? C6A C6 H6 119.2 . . ? C6 C6A C7 123.9(6) . . ? C6 C6A C9B 118.9(6) . . ? C7 C6A C9B 117.2(6) . . ? C8 C7 O7" 124.0(6) . . ? C8 C7 C6A 122.1(6) . . ? O7" C7 C6A 113.9(6) . . ? C7 O7" C7" 116.8(5) . . ? O7" C7" H7"1 109.5 . . ? O7" C7" H7"2 109.5 . . ? H7"1 C7" H7"2 109.5 . . ? O7" C7" H7"3 109.5 . . ? H7"1 C7" H7"3 109.5 . . ? H7"2 C7" H7"3 109.5 . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? O9 C9 C9A 122.7(5) . . ? O9 C9 C8 117.5(6) . . ? C9A C9 C8 119.8(6) . . ? C9 C9A C1 120.9(6) . . ? C9 C9A C9B 119.4(6) . . ? C1 C9A C9B 119.7(6) . . ? C3A C9B C9A 120.2(6) . . ? C3A C9B C6A 119.1(6) . . ? C9A C9B C6A 120.6(6) . . ? C9 O9 Si1 127.5(4) . . ? C11 O11 Si1 127.2(4) . . ? O11 C11 C12 117.0(5) . . ? O11 C11 C19A 122.6(5) . . ? C12 C11 C19A 120.4(6) . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 O13" 123.9(6) . . ? C12 C13 C13A 122.2(6) . . ? O13" C13 C13A 113.9(6) . . ? C14 C13A C19B 119.8(6) . . ? C14 C13A C13 122.9(6) . . ? C19B C13A C13 117.2(6) . . ? C13 O13" C13" 117.1(5) . . ? O13" C13" H13A 109.5 . . ? O13" C13" H13B 109.5 . . ? H13A C13" H13B 109.5 . . ? O13" C13" H13C 109.5 . . ? H13A C13" H13C 109.5 . . ? H13B C13" H13C 109.5 . . ? C15 C14 C13A 121.8(7) . . ? C15 C14 H14 119.1 . . ? C13A C14 H14 119.1 . . ? C14 C15 C16 119.5(7) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C16A 120.9(7) . . ? C15 C16 H16 119.5 . . ? C16A C16 H16 119.5 . . ? C16 C16A C19B 119.8(6) . . ? C16 C16A C17 122.4(6) . . ? C19B C16A C17 117.8(6) . . ? C18 C17 O17" 125.3(6) . . ? C18 C17 C16A 121.4(6) . . ? O17" C17 C16A 113.3(6) . . ? C17 O17" C17" 118.2(5) . . ? O17" C17" H17A 109.5 . . ? O17" C17" H17B 109.5 . . ? H17A C17" H17B 109.5 . . ? O17" C17" H17C 109.5 . . ? H17A C17" H17C 109.5 . . ? H17B C17" H17C 109.5 . . ? C17 C18 C19 121.1(6) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? O19 C19 C18 118.7(5) . . ? O19 C19 C19A 121.6(5) . . ? C18 C19 C19A 119.7(6) . . ? C19 C19A C19B 119.3(6) . . ? C19 C19A C11 122.0(6) . . ? C19B C19A C11 118.6(5) . . ? C16A C19B C19A 120.7(6) . . ? C16A C19B C13A 118.1(6) . . ? C19A C19B C13A 121.2(6) . . ? C19 O19 Si1 127.3(3) . . ? C21 O21 Si1 129.1(4) . . ? O21 C21 C29A 122.4(5) . . ? O21 C21 C22 117.3(6) . . ? C29A C21 C22 120.3(6) . . ? C23 C22 C21 120.2(6) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? O23" C23 C22 123.9(6) . . ? O23" C23 C23A 114.3(6) . . ? C22 C23 C23A 121.9(6) . . ? C24 C23A C29B 119.5(6) . . ? C24 C23A C23 122.9(6) . . ? C29B C23A C23 117.6(6) . . ? C23 O23" C23" 117.9(5) . . ? O23" C23" H23A 109.5 . . ? O23" C23" H23B 109.5 . . ? H23A C23" H23B 109.5 . . ? O23" C23" H23C 109.5 . . ? H23A C23" H23C 109.5 . . ? H23B C23" H23C 109.5 . . ? C25 C24 C23A 121.0(7) . . ? C25 C24 H24 119.5 . . ? C23A C24 H24 119.5 . . ? C24 C25 C26 121.2(6) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C26A 119.7(7) . . ? C25 C26 H26 120.1 . . ? C26A C26 H26 120.1 . . ? C26 C26A C29B 120.1(6) . . ? C26 C26A C27 122.2(7) . . ? C29B C26A C27 117.7(6) . . ? O27" C27 C28 124.8(6) . . ? O27" C27 C26A 114.5(6) . . ? C28 C27 C26A 120.6(7) . . ? C27 O27" C27" 116.4(5) . . ? O27" C27" H27A 109.5 . . ? O27" C27" H27B 109.5 . . ? H27A C27" H27B 109.5 . . ? O27" C27" H27C 109.5 . . ? H27A C27" H27C 109.5 . . ? H27B C27" H27C 109.5 . . ? C27 C28 C29 121.7(6) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? O29 C29 C28 117.8(6) . . ? O29 C29 C29A 122.7(6) . . ? C28 C29 C29A 119.5(6) . . ? C29 C29A C21 121.2(6) . . ? C29 C29A C29B 119.6(6) . . ? C21 C29A C29B 119.2(6) . . ? C26A C29B C29A 120.7(6) . . ? C26A C29B C23A 118.5(6) . . ? C29A C29B C23A 120.8(6) . . ? C29 O29 Si1 128.9(4) . . ? N1# C2# C3# 178.5(8) . . ? C2# C3# H3#1 109.5 . . ? C2# C3# H3#2 109.5 . . ? H3#1 C3# H3#2 109.5 . . ? C2# C3# H3#3 109.5 . . ? H3#1 C3# H3#3 109.5 . . ? H3#2 C3# H3#3 109.5 . . ? N1' C2' C3' 173.8(12) . . ? C2' C3' H3'1 109.5 . . ? C2' C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C2' C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? N1* C2* C3* 177.9(12) . . ? C2* C3* H3*1 109.5 . . ? C2* C3* H3*2 109.5 . . ? H3*1 C3* H3*2 109.5 . . ? C2* C3* H3*3 109.5 . . ? H3*1 C3* H3*3 109.5 . . ? H3*2 C3* H3*3 109.5 . . ? 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 O9 Si1 O1 C1 -25.6(5) . . . . ? O11 Si1 O1 C1 62.9(5) . . . . ? O19 Si1 O1 C1 158.6(5) . . . . ? O29 Si1 O1 C1 114(3) . . . . ? O21 Si1 O1 C1 -114.3(5) . . . . ? Si1 O1 C1 C2 -162.1(4) . . . . ? Si1 O1 C1 C9A 20.1(7) . . . . ? O1 C1 C2 C3 -179.7(5) . . . . ? C9A C1 C2 C3 -1.8(8) . . . . ? C1 C2 C3 O3" -177.5(5) . . . . ? C1 C2 C3 C3A 3.0(8) . . . . ? O3" C3 C3A C4 -1.1(8) . . . . ? C2 C3 C3A C4 178.5(5) . . . . ? O3" C3 C3A C9B 179.0(5) . . . . ? C2 C3 C3A C9B -1.4(8) . . . . ? C2 C3 O3" C3" 15.2(8) . . . . ? C3A C3 O3" C3" -165.2(5) . . . . ? C9B C3A C4 C5 0.6(8) . . . . ? C3 C3A C4 C5 -179.3(5) . . . . ? C3A C4 C5 C6 1.0(9) . . . . ? C4 C5 C6 C6A -1.3(9) . . . . ? C5 C6 C6A C7 179.8(5) . . . . ? C5 C6 C6A C9B 0.0(8) . . . . ? C6 C6A C7 C8 176.9(6) . . . . ? C9B C6A C7 C8 -3.3(8) . . . . ? C6 C6A C7 O7" -2.4(8) . . . . ? C9B C6A C7 O7" 177.4(5) . . . . ? C8 C7 O7" C7" 2.4(9) . . . . ? C6A C7 O7" C7" -178.3(6) . . . . ? O7" C7 C8 C9 -178.5(5) . . . . ? C6A C7 C8 C9 2.2(9) . . . . ? C7 C8 C9 O9 179.7(5) . . . . ? C7 C8 C9 C9A 1.0(8) . . . . ? O9 C9 C9A C1 -2.8(8) . . . . ? C8 C9 C9A C1 175.8(5) . . . . ? O9 C9 C9A C9B 178.3(5) . . . . ? C8 C9 C9A C9B -3.1(8) . . . . ? O1 C1 C9A C9 -2.0(8) . . . . ? C2 C1 C9A C9 -179.8(5) . . . . ? O1 C1 C9A C9B 176.9(5) . . . . ? C2 C1 C9A C9B -0.9(8) . . . . ? C4 C3A C9B C9A 178.8(5) . . . . ? C3 C3A C9B C9A -1.3(8) . . . . ? C4 C3A C9B C6A -1.8(8) . . . . ? C3 C3A C9B C6A 178.1(5) . . . . ? C9 C9A C9B C3A -178.7(5) . . . . ? C1 C9A C9B C3A 2.4(8) . . . . ? C9 C9A C9B C6A 2.0(8) . . . . ? C1 C9A C9B C6A -176.9(5) . . . . ? C6 C6A C9B C3A 1.6(8) . . . . ? C7 C6A C9B C3A -178.3(5) . . . . ? C6 C6A C9B C9A -179.1(5) . . . . ? C7 C6A C9B C9A 1.1(8) . . . . ? C9A C9 O9 Si1 -10.4(8) . . . . ? C8 C9 O9 Si1 171.0(4) . . . . ? O1 Si1 O9 C9 20.7(5) . . . . ? O11 Si1 O9 C9 -69.5(5) . . . . ? O19 Si1 O9 C9 151(2) . . . . ? O29 Si1 O9 C9 -157.1(4) . . . . ? O21 Si1 O9 C9 108.1(5) . . . . ? O1 Si1 O11 C11 107.4(4) . . . . ? O9 Si1 O11 C11 -157.8(4) . . . . ? O19 Si1 O11 C11 18.7(5) . . . . ? O29 Si1 O11 C11 -70.0(4) . . . . ? O21 Si1 O11 C11 161(3) . . . . ? Si1 O11 C11 C12 170.7(4) . . . . ? Si1 O11 C11 C19A -10.4(8) . . . . ? O11 C11 C12 C13 178.1(5) . . . . ? C19A C11 C12 C13 -0.8(9) . . . . ? C11 C12 C13 O13" -178.4(6) . . . . ? C11 C12 C13 C13A 2.1(10) . . . . ? C12 C13 C13A C14 177.6(7) . . . . ? O13" C13 C13A C14 -2.0(10) . . . . ? C12 C13 C13A C19B -2.1(10) . . . . ? O13" C13 C13A C19B 178.3(6) . . . . ? C12 C13 O13" C13" 3.5(9) . . . . ? C13A C13 O13" C13" -176.9(6) . . . . ? C19B C13A C14 C15 -0.8(11) . . . . ? C13 C13A C14 C15 179.6(7) . . . . ? C13A C14 C15 C16 -1.0(12) . . . . ? C14 C15 C16 C16A 1.8(12) . . . . ? C15 C16 C16A C19B -0.7(11) . . . . ? C15 C16 C16A C17 -179.6(7) . . . . ? C16 C16A C17 C18 178.1(7) . . . . ? C19B C16A C17 C18 -0.8(10) . . . . ? C16 C16A C17 O17" -1.9(10) . . . . ? C19B C16A C17 O17" 179.1(5) . . . . ? C18 C17 O17" C17" -1.1(10) . . . . ? C16A C17 O17" C17" 179.0(6) . . . . ? O17" C17 C18 C19 -178.1(6) . . . . ? C16A C17 C18 C19 1.9(10) . . . . ? C17 C18 C19 O19 -179.5(5) . . . . ? C17 C18 C19 C19A -0.7(9) . . . . ? O19 C19 C19A C19B 177.2(5) . . . . ? C18 C19 C19A C19B -1.6(8) . . . . ? O19 C19 C19A C11 0.3(9) . . . . ? C18 C19 C19A C11 -178.5(5) . . . . ? O11 C11 C19A C19 -2.4(9) . . . . ? C12 C11 C19A C19 176.5(6) . . . . ? O11 C11 C19A C19B -179.3(5) . . . . ? C12 C11 C19A C19B -0.4(8) . . . . ? C16 C16A C19B C19A 179.6(6) . . . . ? C17 C16A C19B C19A -1.5(9) . . . . ? C16 C16A C19B C13A -1.1(9) . . . . ? C17 C16A C19B C13A 177.8(6) . . . . ? C19 C19A C19B C16A 2.7(9) . . . . ? C11 C19A C19B C16A 179.7(5) . . . . ? C19 C19A C19B C13A -176.6(6) . . . . ? C11 C19A C19B C13A 0.4(8) . . . . ? C14 C13A C19B C16A 1.9(9) . . . . ? C13 C13A C19B C16A -178.5(6) . . . . ? C14 C13A C19B C19A -178.8(6) . . . . ? C13 C13A C19B C19A 0.8(9) . . . . ? C18 C19 O19 Si1 -166.7(4) . . . . ? C19A C19 O19 Si1 14.5(8) . . . . ? O1 Si1 O19 C19 -111.1(4) . . . . ? O9 Si1 O19 C19 119(2) . . . . ? O11 Si1 O19 C19 -20.8(5) . . . . ? O29 Si1 O19 C19 66.6(5) . . . . ? O21 Si1 O19 C19 161.4(4) . . . . ? O1 Si1 O21 C21 -171.3(5) . . . . ? O9 Si1 O21 C21 93.9(5) . . . . ? O11 Si1 O21 C21 135(3) . . . . ? O19 Si1 O21 C21 -82.4(5) . . . . ? O29 Si1 O21 C21 6.2(5) . . . . ? Si1 O21 C21 C29A -0.8(8) . . . . ? Si1 O21 C21 C22 178.8(4) . . . . ? O21 C21 C22 C23 178.5(5) . . . . ? C29A C21 C22 C23 -1.9(8) . . . . ? C21 C22 C23 O23" -177.6(5) . . . . ? C21 C22 C23 C23A 2.3(9) . . . . ? O23" C23 C23A C24 0.6(8) . . . . ? C22 C23 C23A C24 -179.3(6) . . . . ? O23" C23 C23A C29B -179.9(5) . . . . ? C22 C23 C23A C29B 0.2(8) . . . . ? C22 C23 O23" C23" -5.8(8) . . . . ? C23A C23 O23" C23" 174.3(5) . . . . ? C29B C23A C24 C25 0.7(9) . . . . ? C23 C23A C24 C25 -179.8(6) . . . . ? C23A C24 C25 C26 1.0(10) . . . . ? C24 C25 C26 C26A -2.0(10) . . . . ? C25 C26 C26A C29B 1.2(9) . . . . ? C25 C26 C26A C27 -177.4(6) . . . . ? C26 C26A C27 O27" -5.6(9) . . . . ? C29B C26A C27 O27" 175.8(5) . . . . ? C26 C26A C27 C28 174.8(6) . . . . ? C29B C26A C27 C28 -3.8(9) . . . . ? C28 C27 O27" C27" 3.2(9) . . . . ? C26A C27 O27" C27" -176.4(5) . . . . ? O27" C27 C28 C29 -176.8(6) . . . . ? C26A C27 C28 C29 2.8(9) . . . . ? C27 C28 C29 O29 -178.6(5) . . . . ? C27 C28 C29 C29A 0.9(9) . . . . ? O29 C29 C29A C21 -2.9(9) . . . . ? C28 C29 C29A C21 177.7(5) . . . . ? O29 C29 C29A C29B 176.1(5) . . . . ? C28 C29 C29A C29B -3.4(8) . . . . ? O21 C21 C29A C29 -2.3(9) . . . . ? C22 C21 C29A C29 178.1(5) . . . . ? O21 C21 C29A C29B 178.7(5) . . . . ? C22 C21 C29A C29B -0.9(8) . . . . ? C26 C26A C29B C29A -177.4(5) . . . . ? C27 C26A C29B C29A 1.3(8) . . . . ? C26 C26A C29B C23A 0.4(9) . . . . ? C27 C26A C29B C23A 179.1(5) . . . . ? C29 C29A C29B C26A 2.2(8) . . . . ? C21 C29A C29B C26A -178.8(6) . . . . ? C29 C29A C29B C23A -175.5(5) . . . . ? C21 C29A C29B C23A 3.5(8) . . . . ? C24 C23A C29B C26A -1.4(8) . . . . ? C23 C23A C29B C26A 179.1(5) . . . . ? C24 C23A C29B C29A 176.4(5) . . . . ? C23 C23A C29B C29A -3.1(8) . . . . ? C28 C29 O29 Si1 -169.1(4) . . . . ? C29A C29 O29 Si1 11.4(8) . . . . ? O1 Si1 O29 C29 120(3) . . . . ? O9 Si1 O29 C29 -100.3(5) . . . . ? O11 Si1 O29 C29 171.2(5) . . . . ? O19 Si1 O29 C29 75.4(5) . . . . ? O21 Si1 O29 C29 -11.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.39 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.339 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.055 # Attachment '- (18+)rh140_0m.cif' data_rh140_0m _database_code_depnum_ccdc_archive 'CCDC 785945' #TrackingRef '- (18+)rh140_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70.72 H56.44 B Cl3.44 O12 Si' _chemical_formula_weight 1259.09 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1909(2) _cell_length_b 41.2909(5) _cell_length_c 11.6570(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.1662(4) _cell_angle_gamma 90.00 _cell_volume 6128.01(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8983 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 32.43 _exptl_crystal_description 'prism frag' _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2617 _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8985 _exptl_absorpt_correction_T_max 0.9536 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 159213 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 60 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 31.51 _reflns_number_total 20371 _reflns_number_gt 15082 _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^)+(0.0747P)^2^+3.5789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20371 _refine_ls_number_parameters 862 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.02522(3) 0.367534(9) 0.13675(3) 0.01802(8) Uani 1 1 d . . . O1 O -0.07588(9) 0.38350(2) 0.02097(9) 0.0198(2) Uani 1 1 d . . . C1 C -0.07717(12) 0.41125(3) -0.03357(12) 0.0180(3) Uani 1 1 d . . . C2 C -0.17430(12) 0.42160(4) -0.10758(13) 0.0211(3) Uani 1 1 d . . . H2 H -0.2349 0.4084 -0.1166 0.025 Uiso 1 1 calc R . . C3 C -0.18159(12) 0.45054(4) -0.16648(13) 0.0214(3) Uani 1 1 d . . . C3A C -0.09031(12) 0.47067(4) -0.15815(12) 0.0198(3) Uani 1 1 d . . . O3" O -0.27156(9) 0.46261(3) -0.23570(10) 0.0279(2) Uani 1 1 d . . . C3" C -0.36627(14) 0.44480(5) -0.24092(18) 0.0363(4) Uani 1 1 d . . . H3"1 H -0.3634 0.4239 -0.2796 0.054 Uiso 1 1 calc R . . H3"2 H -0.4269 0.4572 -0.2866 0.054 Uiso 1 1 calc R . . H3"3 H -0.3731 0.4412 -0.1602 0.054 Uiso 1 1 calc R . . C4 C -0.09634(14) 0.50019(4) -0.21886(13) 0.0243(3) Uani 1 1 d . . . H4 H -0.1621 0.5075 -0.2667 0.029 Uiso 1 1 calc R . . C5 C -0.00727(14) 0.51864(4) -0.20959(14) 0.0268(3) Uani 1 1 d . . . H5 H -0.0121 0.5385 -0.2519 0.032 Uiso 1 1 calc R . . C6 C 0.08941(14) 0.50842(4) -0.13888(14) 0.0247(3) Uani 1 1 d . . . H6 H 0.1503 0.5212 -0.1338 0.030 Uiso 1 1 calc R . . C6A C 0.09747(12) 0.47938(3) -0.07521(13) 0.0198(3) Uani 1 1 d . . . C7 C 0.19542(12) 0.46851(4) 0.00285(13) 0.0206(3) Uani 1 1 d . . . O7" O 0.27578(9) 0.48924(3) 0.01280(11) 0.0267(2) Uani 1 1 d . . . C7" C 0.37561(14) 0.47990(5) 0.08923(18) 0.0341(4) Uani 1 1 d . . . H7"1 H 0.3690 0.4769 0.1704 0.051 Uiso 1 1 calc R . . H7"2 H 0.4275 0.4968 0.0888 0.051 Uiso 1 1 calc R . . H7"3 H 0.3985 0.4595 0.0607 0.051 Uiso 1 1 calc R . . C8 C 0.20276(12) 0.43949(3) 0.06233(13) 0.0196(3) Uani 1 1 d . . . H8 H 0.2686 0.4324 0.1109 0.023 Uiso 1 1 calc R . . C9 C 0.11236(12) 0.42019(3) 0.05105(12) 0.0172(2) Uani 1 1 d . . . O9 O 0.12345(8) 0.39286(2) 0.10962(9) 0.01859(19) Uani 1 1 d . . . C9A C 0.01382(11) 0.43039(3) -0.02117(12) 0.0169(2) Uani 1 1 d . . . C9B C 0.00711(12) 0.46003(3) -0.08486(12) 0.0182(3) Uani 1 1 d . . . O11 O -0.07023(9) 0.34222(2) 0.17426(10) 0.0221(2) Uani 1 1 d . . . C11 C -0.08178(12) 0.31107(4) 0.16064(13) 0.0210(3) Uani 1 1 d . . . C12 C -0.15003(13) 0.29556(4) 0.21922(15) 0.0244(3) Uani 1 1 d . . . H12 H -0.1872 0.3080 0.2636 0.029 Uiso 1 1 calc R . . C13 C -0.16231(13) 0.26253(4) 0.21161(15) 0.0253(3) Uani 1 1 d . . . C13A C -0.11000(13) 0.24318(4) 0.14138(15) 0.0251(3) Uani 1 1 d . . . O13" O -0.22268(11) 0.24548(3) 0.26630(13) 0.0342(3) Uani 1 1 d . . . C13" C -0.28264(18) 0.26276(5) 0.3329(2) 0.0421(5) Uani 1 1 d . . . H13A H -0.2349 0.2747 0.3976 0.063 Uiso 1 1 calc R . . H13B H -0.3238 0.2474 0.3663 0.063 Uiso 1 1 calc R . . H13C H -0.3301 0.2780 0.2805 0.063 Uiso 1 1 calc R . . C14 C -0.12198(15) 0.20952(4) 0.13304(18) 0.0319(4) Uani 1 1 d . . . H14 H -0.1642 0.1988 0.1760 0.038 Uiso 1 1 calc R . . C15 C -0.07250(16) 0.19173(4) 0.06227(19) 0.0345(4) Uani 1 1 d . . . H15 H -0.0804 0.1689 0.0579 0.041 Uiso 1 1 calc R . . C16 C -0.01159(14) 0.20710(4) -0.00214(17) 0.0288(3) Uani 1 1 d . . . H16 H 0.0209 0.1947 -0.0513 0.035 Uiso 1 1 calc R . . C16A C 0.00242(13) 0.24077(4) 0.00471(14) 0.0229(3) Uani 1 1 d . . . C17 C 0.06526(12) 0.25772(4) -0.06067(13) 0.0214(3) Uani 1 1 d . . . O17" O 0.10620(10) 0.23872(3) -0.13099(11) 0.0280(2) Uani 1 1 d . . . C17" C 0.17008(15) 0.25392(4) -0.19830(17) 0.0315(4) Uani 1 1 d . . . H17A H 0.1286 0.2703 -0.2511 0.047 Uiso 1 1 calc R . . H17B H 0.1945 0.2375 -0.2458 0.047 Uiso 1 1 calc R . . H17C H 0.2308 0.2643 -0.1439 0.047 Uiso 1 1 calc R . . C18 C 0.08018(12) 0.29053(4) -0.05035(13) 0.0207(3) Uani 1 1 d . . . H18 H 0.1210 0.3012 -0.0951 0.025 Uiso 1 1 calc R . . C19 C 0.03479(12) 0.30862(3) 0.02707(12) 0.0183(3) Uani 1 1 d . . . O19 O 0.05486(9) 0.33954(2) 0.03571(9) 0.0204(2) Uani 1 1 d . . . C19A C -0.03009(12) 0.29316(3) 0.08957(13) 0.0195(3) Uani 1 1 d . . . C19B C -0.04590(12) 0.25917(3) 0.07831(14) 0.0214(3) Uani 1 1 d . . . O21 O -0.00792(9) 0.39665(2) 0.23204(9) 0.0198(2) Uani 1 1 d . . . C21 C 0.00486(12) 0.39392(3) 0.34638(13) 0.0182(3) Uani 1 1 d . . . C22 C -0.05573(12) 0.41460(3) 0.39934(13) 0.0199(3) Uani 1 1 d . . . H22 H -0.1058 0.4288 0.3512 0.024 Uiso 1 1 calc R . . C23 C -0.04208(12) 0.41406(3) 0.52012(13) 0.0203(3) Uani 1 1 d . . . C23A C 0.03517(12) 0.39315(3) 0.59620(13) 0.0202(3) Uani 1 1 d . . . O23" O -0.09753(9) 0.43220(3) 0.57760(10) 0.0263(2) Uani 1 1 d . . . C23" C -0.17844(15) 0.45293(4) 0.50668(16) 0.0314(4) Uani 1 1 d . . . H23A H -0.1461 0.4695 0.4674 0.047 Uiso 1 1 calc R . . H23B H -0.2167 0.4634 0.5581 0.047 Uiso 1 1 calc R . . H23C H -0.2273 0.4399 0.4465 0.047 Uiso 1 1 calc R . . C24 C 0.05055(14) 0.39254(4) 0.71976(14) 0.0253(3) Uani 1 1 d . . . H24 H 0.0098 0.4062 0.7557 0.030 Uiso 1 1 calc R . . C25 C 0.12496(15) 0.37205(4) 0.79016(14) 0.0284(3) Uani 1 1 d . . . H25 H 0.1347 0.3718 0.8738 0.034 Uiso 1 1 calc R . . C26 C 0.18527(14) 0.35200(4) 0.73845(14) 0.0253(3) Uani 1 1 d . . . H26 H 0.2364 0.3382 0.7873 0.030 Uiso 1 1 calc R . . C26A C 0.17139(12) 0.35190(4) 0.61519(13) 0.0214(3) Uani 1 1 d . . . C27 C 0.23313(12) 0.33150(4) 0.55819(14) 0.0219(3) Uani 1 1 d . . . C27" C 0.36528(15) 0.29070(4) 0.58451(17) 0.0324(4) Uani 1 1 d . . . H27A H 0.3194 0.2758 0.5288 0.049 Uiso 1 1 calc R . . H27B H 0.4120 0.2783 0.6487 0.049 Uiso 1 1 calc R . . H27C H 0.4074 0.3033 0.5424 0.049 Uiso 1 1 calc R . . O27" O 0.30210(10) 0.31236(3) 0.63385(10) 0.0291(3) Uani 1 1 d . . . C28 C 0.21898(12) 0.33180(4) 0.43725(13) 0.0212(3) Uani 1 1 d . . . H28 H 0.2622 0.3188 0.4022 0.025 Uiso 1 1 calc R . . C29 C 0.13976(12) 0.35155(3) 0.36487(13) 0.0186(3) Uani 1 1 d . . . O29 O 0.12548(9) 0.34934(2) 0.25008(9) 0.0205(2) Uani 1 1 d . . . C29A C 0.07854(12) 0.37226(3) 0.41680(12) 0.0180(3) Uani 1 1 d . . . C29B C 0.09522(12) 0.37242(3) 0.54255(12) 0.0186(3) Uani 1 1 d . . . B1' B 0.51758(14) 0.38600(4) 0.37395(16) 0.0225(3) Uani 1 1 d . . . C1' C 0.43493(12) 0.41326(4) 0.39909(14) 0.0220(3) Uani 1 1 d . . . C2' C 0.32553(12) 0.41061(4) 0.36653(15) 0.0243(3) Uani 1 1 d . . . H2' H 0.2945 0.3920 0.3234 0.029 Uiso 1 1 calc R . . C3' C 0.25994(13) 0.43413(4) 0.39458(16) 0.0281(3) Uani 1 1 d . . . H3' H 0.1859 0.4313 0.3701 0.034 Uiso 1 1 calc R . . C4' C 0.30185(14) 0.46154(4) 0.45774(16) 0.0293(3) Uani 1 1 d . . . H4' H 0.2573 0.4775 0.4773 0.035 Uiso 1 1 calc R . . C5' C 0.41007(14) 0.46525(4) 0.49201(16) 0.0291(3) Uani 1 1 d . . . H5' H 0.4403 0.4840 0.5350 0.035 Uiso 1 1 calc R . . C6' C 0.47446(13) 0.44159(4) 0.46343(15) 0.0257(3) Uani 1 1 d . . . H6' H 0.5484 0.4446 0.4883 0.031 Uiso 1 1 calc R . . C7' C 0.58849(12) 0.40081(4) 0.28960(14) 0.0243(3) Uani 1 1 d . . . C8' C 0.58628(13) 0.43298(4) 0.25152(15) 0.0276(3) Uani 1 1 d . . . H8' H 0.5425 0.4480 0.2777 0.033 Uiso 1 1 calc R . . C9' C 0.64616(15) 0.44399(5) 0.17616(17) 0.0350(4) Uani 1 1 d . . . H9' H 0.6425 0.4661 0.1525 0.042 Uiso 1 1 calc R . . C10' C 0.71016(15) 0.42289(5) 0.13648(16) 0.0361(4) Uani 1 1 d . . . H10' H 0.7505 0.4303 0.0851 0.043 Uiso 1 1 calc R . . C11' C 0.71541(15) 0.39066(5) 0.17197(18) 0.0357(4) Uani 1 1 d . . . H11' H 0.7597 0.3759 0.1453 0.043 Uiso 1 1 calc R . . C12' C 0.65548(14) 0.38007(5) 0.24678(17) 0.0310(4) Uani 1 1 d . . . H12' H 0.6598 0.3579 0.2700 0.037 Uiso 1 1 calc R . . C13' C 0.58937(13) 0.37466(4) 0.50522(15) 0.0241(3) Uani 1 1 d . . . C14' C 0.69933(13) 0.37532(4) 0.54276(15) 0.0268(3) Uani 1 1 d . . . H14' H 0.7374 0.3829 0.4892 0.032 Uiso 1 1 calc R . . C15' C 0.75492(14) 0.36525(4) 0.65607(17) 0.0316(4) Uani 1 1 d . . . H15' H 0.8294 0.3665 0.6786 0.038 Uiso 1 1 calc R . . C16' C 0.70257(16) 0.35345(4) 0.73589(17) 0.0348(4) Uani 1 1 d . . . H16' H 0.7405 0.3460 0.8122 0.042 Uiso 1 1 calc R . . C17' C 0.59313(16) 0.35272(5) 0.70208(17) 0.0351(4) Uani 1 1 d . . . H17' H 0.5557 0.3448 0.7557 0.042 Uiso 1 1 calc R . . C18' C 0.53857(14) 0.36357(4) 0.58988(16) 0.0296(3) Uani 1 1 d . . . H18' H 0.4640 0.3635 0.5696 0.035 Uiso 1 1 calc R . . C19' C 0.45599(12) 0.35428(4) 0.30180(14) 0.0230(3) Uani 1 1 d . . . C20' C 0.47576(14) 0.32218(4) 0.33975(15) 0.0264(3) Uani 1 1 d . . . H20' H 0.5278 0.3180 0.4117 0.032 Uiso 1 1 calc R . . C21' C 0.42175(15) 0.29595(4) 0.27564(17) 0.0311(4) Uani 1 1 d . . . H21' H 0.4376 0.2745 0.3044 0.037 Uiso 1 1 calc R . . C22' C 0.34556(14) 0.30107(4) 0.17078(17) 0.0308(4) Uani 1 1 d . . . H22' H 0.3076 0.2833 0.1282 0.037 Uiso 1 1 calc R . . C23' C 0.32511(14) 0.33249(5) 0.12831(17) 0.0320(4) Uani 1 1 d . . . H23' H 0.2733 0.3364 0.0560 0.038 Uiso 1 1 calc R . . C24' C 0.38079(14) 0.35827(4) 0.19208(16) 0.0287(3) Uani 1 1 d . . . H24' H 0.3675 0.3795 0.1602 0.034 Uiso 1 1 calc R . . C1S C 0.6524(9) 0.57677(15) 0.2671(6) 0.050(2) Uani 0.61 1 d PDU A 1 H1SA H 0.7231 0.5864 0.2968 0.060 Uiso 0.61 1 calc PR A 1 H1SB H 0.6154 0.5784 0.3307 0.060 Uiso 0.61 1 calc PR A 1 Cl1S Cl 0.58115(15) 0.59784(6) 0.1390(2) 0.0534(4) Uani 0.61 1 d PDU A 1 Cl2S Cl 0.66325(14) 0.53573(4) 0.22930(17) 0.0535(4) Uani 0.61 1 d PDU A 1 C1D C 0.6441(13) 0.5787(3) 0.2568(9) 0.043(4) Uani 0.26 1 d PDU B 2 H1D1 H 0.6954 0.5954 0.2962 0.052 Uiso 0.26 1 calc PR B 2 H1D2 H 0.5959 0.5748 0.3078 0.052 Uiso 0.26 1 calc PR B 2 Cl1D Cl 0.5704(7) 0.5939(2) 0.1176(7) 0.097(3) Uani 0.26 1 d PDU B 2 Cl2D Cl 0.7123(5) 0.54237(15) 0.2462(5) 0.098(2) Uani 0.26 1 d PDU B 2 C2S C 0.5230(4) 0.17751(18) 0.5086(5) 0.0406(12) Uani 0.38 1 d PU C 3 H2SA H 0.5116 0.1543 0.4886 0.049 Uiso 0.38 1 calc PR C 3 H2SB H 0.5109 0.1810 0.5880 0.049 Uiso 0.38 1 calc PR C 3 Cl3S Cl 0.4349(3) 0.20034(14) 0.4048(3) 0.1139(19) Uani 0.38 1 d PU C 3 Cl4S Cl 0.65138(11) 0.18781(5) 0.51304(15) 0.0578(4) Uani 0.38 1 d PU C 3 C2D C 0.5410(3) 0.19777(13) 0.5248(4) 0.0362(9) Uani 0.47 1 d PU D 4 H2DA H 0.5191 0.1884 0.5928 0.043 Uiso 0.47 1 calc PR D 4 H2DB H 0.6051 0.1863 0.5180 0.043 Uiso 0.47 1 calc PR D 4 Cl3D Cl 0.56793(8) 0.23940(3) 0.54938(9) 0.0427(2) Uani 0.47 1 d PU D 4 Cl4D Cl 0.43981(18) 0.19258(6) 0.39282(19) 0.0428(4) Uani 0.47 1 d PU D 4 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 Si1 0.0259(2) 0.01429(17) 0.01668(18) 0.00137(13) 0.01061(15) 0.00146(14) O1 0.0252(5) 0.0176(5) 0.0181(5) 0.0021(4) 0.0083(4) -0.0016(4) C1 0.0257(7) 0.0163(6) 0.0138(6) -0.0010(4) 0.0083(5) 0.0004(5) C2 0.0236(7) 0.0224(7) 0.0175(6) -0.0010(5) 0.0057(5) -0.0007(5) C3 0.0253(7) 0.0224(7) 0.0158(6) -0.0011(5) 0.0043(5) 0.0035(5) C3A 0.0272(7) 0.0187(6) 0.0139(6) 0.0000(5) 0.0059(5) 0.0029(5) O3" 0.0260(6) 0.0305(6) 0.0239(5) 0.0022(4) 0.0003(4) 0.0049(5) C3" 0.0265(8) 0.0396(10) 0.0375(10) -0.0010(8) -0.0009(7) 0.0020(7) C4 0.0343(8) 0.0212(7) 0.0174(6) 0.0029(5) 0.0066(6) 0.0057(6) C5 0.0416(9) 0.0181(7) 0.0227(7) 0.0057(5) 0.0122(6) 0.0034(6) C6 0.0354(8) 0.0171(6) 0.0247(7) 0.0025(5) 0.0135(6) -0.0019(6) C6A 0.0270(7) 0.0161(6) 0.0183(6) 0.0001(5) 0.0097(5) 0.0001(5) C7 0.0252(7) 0.0177(6) 0.0215(7) -0.0016(5) 0.0107(5) -0.0023(5) O7" 0.0266(6) 0.0206(5) 0.0337(6) 0.0022(4) 0.0093(5) -0.0047(4) C7" 0.0251(8) 0.0306(9) 0.0445(10) 0.0008(7) 0.0054(7) -0.0047(7) C8 0.0220(7) 0.0182(6) 0.0193(6) -0.0003(5) 0.0068(5) 0.0004(5) C9 0.0245(7) 0.0150(6) 0.0139(6) -0.0010(4) 0.0081(5) 0.0015(5) O9 0.0239(5) 0.0150(4) 0.0179(5) 0.0024(3) 0.0072(4) 0.0015(4) C9A 0.0235(7) 0.0147(6) 0.0142(6) 0.0009(4) 0.0079(5) 0.0010(5) C9B 0.0263(7) 0.0156(6) 0.0146(6) 0.0007(4) 0.0087(5) 0.0018(5) O11 0.0316(6) 0.0152(5) 0.0247(5) 0.0012(4) 0.0167(4) 0.0012(4) C11 0.0273(7) 0.0174(6) 0.0216(7) 0.0028(5) 0.0124(6) 0.0018(5) C12 0.0298(8) 0.0208(7) 0.0283(8) 0.0035(6) 0.0178(6) 0.0022(6) C13 0.0285(8) 0.0214(7) 0.0305(8) 0.0049(6) 0.0159(6) 0.0001(6) C13A 0.0290(8) 0.0188(7) 0.0320(8) 0.0027(6) 0.0156(6) 0.0004(6) O13" 0.0389(7) 0.0250(6) 0.0481(8) 0.0063(5) 0.0284(6) -0.0012(5) C13" 0.0440(11) 0.0395(10) 0.0553(12) 0.0040(9) 0.0351(10) -0.0019(8) C14 0.0376(9) 0.0195(7) 0.0450(10) 0.0031(7) 0.0224(8) -0.0020(6) C15 0.0418(10) 0.0160(7) 0.0524(11) 0.0007(7) 0.0244(9) 0.0000(7) C16 0.0343(9) 0.0181(7) 0.0380(9) -0.0021(6) 0.0170(7) 0.0016(6) C16A 0.0268(7) 0.0164(6) 0.0282(7) -0.0003(5) 0.0121(6) 0.0009(5) C17 0.0246(7) 0.0200(6) 0.0219(7) -0.0023(5) 0.0104(5) 0.0024(5) O17" 0.0351(6) 0.0220(5) 0.0334(6) -0.0058(4) 0.0205(5) 0.0006(5) C17" 0.0364(9) 0.0312(8) 0.0339(9) -0.0066(7) 0.0214(7) -0.0021(7) C18 0.0254(7) 0.0190(6) 0.0210(7) -0.0010(5) 0.0116(5) -0.0006(5) C19 0.0235(7) 0.0158(6) 0.0174(6) 0.0008(5) 0.0083(5) 0.0000(5) O19 0.0304(6) 0.0153(4) 0.0197(5) -0.0002(4) 0.0140(4) -0.0017(4) C19A 0.0253(7) 0.0151(6) 0.0214(7) 0.0017(5) 0.0117(5) 0.0004(5) C19B 0.0252(7) 0.0164(6) 0.0254(7) 0.0014(5) 0.0116(6) 0.0017(5) O21 0.0291(5) 0.0159(5) 0.0164(5) 0.0013(3) 0.0095(4) 0.0041(4) C21 0.0232(7) 0.0149(6) 0.0188(6) 0.0000(5) 0.0097(5) -0.0006(5) C22 0.0240(7) 0.0164(6) 0.0213(7) -0.0001(5) 0.0092(5) 0.0033(5) C23 0.0232(7) 0.0174(6) 0.0228(7) -0.0031(5) 0.0103(5) 0.0003(5) C23A 0.0264(7) 0.0181(6) 0.0181(6) -0.0016(5) 0.0096(5) -0.0002(5) O23" 0.0314(6) 0.0269(6) 0.0235(5) -0.0035(4) 0.0124(5) 0.0084(5) C23" 0.0360(9) 0.0297(8) 0.0308(8) -0.0014(6) 0.0129(7) 0.0118(7) C24 0.0331(8) 0.0259(7) 0.0192(7) -0.0031(5) 0.0109(6) 0.0018(6) C25 0.0393(9) 0.0299(8) 0.0179(7) 0.0004(6) 0.0109(6) 0.0017(7) C26 0.0324(8) 0.0250(7) 0.0191(7) 0.0027(5) 0.0076(6) 0.0019(6) C26A 0.0255(7) 0.0202(6) 0.0199(7) 0.0013(5) 0.0085(5) 0.0001(5) C27 0.0248(7) 0.0195(6) 0.0224(7) 0.0040(5) 0.0081(5) 0.0027(5) C27" 0.0360(9) 0.0306(8) 0.0313(9) 0.0057(7) 0.0102(7) 0.0116(7) O27" 0.0348(6) 0.0297(6) 0.0237(5) 0.0066(4) 0.0093(5) 0.0119(5) C28 0.0259(7) 0.0187(6) 0.0218(7) 0.0028(5) 0.0115(5) 0.0043(5) C29 0.0254(7) 0.0151(6) 0.0187(6) 0.0022(5) 0.0115(5) 0.0017(5) O29 0.0300(5) 0.0184(5) 0.0165(5) 0.0028(4) 0.0120(4) 0.0057(4) C29A 0.0237(7) 0.0154(6) 0.0175(6) 0.0008(5) 0.0099(5) 0.0010(5) C29B 0.0232(7) 0.0163(6) 0.0180(6) 0.0004(5) 0.0085(5) -0.0009(5) B1' 0.0211(7) 0.0219(7) 0.0261(8) -0.0014(6) 0.0090(6) -0.0003(6) C1' 0.0235(7) 0.0207(7) 0.0234(7) 0.0017(5) 0.0087(5) 0.0000(5) C2' 0.0228(7) 0.0209(7) 0.0296(8) 0.0007(6) 0.0076(6) -0.0006(6) C3' 0.0227(7) 0.0257(8) 0.0361(9) 0.0026(6) 0.0082(6) 0.0043(6) C4' 0.0317(8) 0.0251(8) 0.0315(8) 0.0010(6) 0.0086(7) 0.0099(6) C5' 0.0351(9) 0.0236(7) 0.0282(8) -0.0040(6) 0.0075(7) 0.0000(6) C6' 0.0238(7) 0.0267(7) 0.0268(8) -0.0032(6) 0.0068(6) -0.0019(6) C7' 0.0196(7) 0.0281(8) 0.0259(7) -0.0027(6) 0.0073(6) -0.0026(6) C8' 0.0249(7) 0.0298(8) 0.0298(8) 0.0028(6) 0.0102(6) 0.0003(6) C9' 0.0346(9) 0.0387(10) 0.0335(9) 0.0071(7) 0.0119(7) -0.0057(8) C10' 0.0318(9) 0.0511(11) 0.0295(9) -0.0052(8) 0.0152(7) -0.0137(8) C11' 0.0275(8) 0.0433(10) 0.0417(10) -0.0126(8) 0.0186(7) -0.0058(7) C12' 0.0269(8) 0.0310(8) 0.0384(9) -0.0053(7) 0.0147(7) -0.0026(7) C13' 0.0256(7) 0.0200(7) 0.0281(7) -0.0022(5) 0.0093(6) 0.0007(6) C14' 0.0261(8) 0.0226(7) 0.0323(8) -0.0020(6) 0.0091(6) 0.0023(6) C15' 0.0294(8) 0.0262(8) 0.0359(9) -0.0034(7) 0.0028(7) 0.0070(6) C16' 0.0441(10) 0.0278(8) 0.0297(9) -0.0001(6) 0.0045(7) 0.0088(7) C17' 0.0454(11) 0.0326(9) 0.0300(9) 0.0015(7) 0.0142(8) 0.0011(8) C18' 0.0310(8) 0.0290(8) 0.0303(8) -0.0012(6) 0.0107(7) -0.0010(7) C19' 0.0209(7) 0.0230(7) 0.0281(7) -0.0029(6) 0.0117(6) -0.0004(5) C20' 0.0293(8) 0.0246(7) 0.0277(8) -0.0017(6) 0.0115(6) 0.0002(6) C21' 0.0386(9) 0.0228(7) 0.0369(9) -0.0035(6) 0.0188(7) -0.0015(7) C22' 0.0333(9) 0.0280(8) 0.0358(9) -0.0117(7) 0.0173(7) -0.0073(7) C23' 0.0281(8) 0.0356(9) 0.0316(9) -0.0085(7) 0.0066(7) 0.0002(7) C24' 0.0278(8) 0.0259(8) 0.0322(8) -0.0033(6) 0.0075(6) 0.0023(6) C1S 0.067(5) 0.035(3) 0.049(3) 0.008(3) 0.016(3) -0.009(3) Cl1S 0.0475(6) 0.0527(8) 0.0600(11) 0.0119(9) 0.0137(6) 0.0037(5) Cl2S 0.0844(10) 0.0427(5) 0.0413(6) -0.0066(4) 0.0306(7) 0.0086(6) C1D 0.053(8) 0.044(8) 0.047(6) -0.022(5) 0.038(6) -0.024(5) Cl1D 0.151(6) 0.087(4) 0.059(3) -0.020(2) 0.037(3) 0.009(3) Cl2D 0.152(5) 0.101(4) 0.062(3) 0.013(2) 0.068(4) 0.054(4) C2S 0.026(2) 0.064(4) 0.033(3) 0.001(3) 0.0093(19) -0.006(2) Cl3S 0.0594(17) 0.227(5) 0.059(2) 0.080(2) 0.0221(15) 0.046(2) Cl4S 0.0268(6) 0.0836(12) 0.0591(9) 0.0270(8) 0.0044(6) -0.0096(7) C2D 0.0218(17) 0.055(3) 0.0315(19) -0.0031(19) 0.0073(14) 0.0043(18) Cl3D 0.0339(5) 0.0609(7) 0.0347(5) -0.0019(4) 0.0113(4) -0.0055(4) Cl4D 0.0361(8) 0.0664(8) 0.0235(6) -0.0131(6) 0.0037(5) -0.0113(7) _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 Si1 O9 1.7570(11) . ? Si1 O1 1.7586(11) . ? Si1 O19 1.7656(11) . ? Si1 O21 1.7676(11) . ? Si1 O29 1.7734(11) . ? Si1 O11 1.7767(11) . ? O1 C1 1.3085(17) . ? C1 C2 1.411(2) . ? C1 C9A 1.413(2) . ? C2 C3 1.369(2) . ? C2 H2 0.9500 . ? C3 O3" 1.3441(18) . ? C3 C3A 1.445(2) . ? C3A C4 1.401(2) . ? C3A C9B 1.414(2) . ? O3" C3" 1.437(2) . ? C3" H3"1 0.9800 . ? C3" H3"2 0.9800 . ? C3" H3"3 0.9800 . ? C4 C5 1.381(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 C6A 1.399(2) . ? C6 H6 0.9500 . ? C6A C9B 1.415(2) . ? C6A C7 1.443(2) . ? C7 O7" 1.3437(18) . ? C7 C8 1.375(2) . ? O7" C7" 1.436(2) . ? C7" H7"1 0.9800 . ? C7" H7"2 0.9800 . ? C7" H7"3 0.9800 . ? C8 C9 1.411(2) . ? C8 H8 0.9500 . ? C9 O9 1.3073(16) . ? C9 C9A 1.415(2) . ? C9A C9B 1.4222(18) . ? O11 C11 1.3004(18) . ? C11 C19A 1.412(2) . ? C11 C12 1.417(2) . ? C12 C13 1.374(2) . ? C12 H12 0.9500 . ? C13 O13" 1.3423(18) . ? C13 C13A 1.442(2) . ? C13A C14 1.399(2) . ? C13A C19B 1.420(2) . ? O13" C13" 1.435(2) . ? C13" H13A 0.9800 . ? C13" H13B 0.9800 . ? C13" H13C 0.9800 . ? C14 C15 1.389(2) . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 H15 0.9500 . ? C16 C16A 1.402(2) . ? C16 H16 0.9500 . ? C16A C19B 1.416(2) . ? C16A C17 1.445(2) . ? C17 O17" 1.3457(17) . ? C17 C18 1.370(2) . ? O17" C17" 1.437(2) . ? C17" H17A 0.9800 . ? C17" H17B 0.9800 . ? C17" H17C 0.9800 . ? C18 C19 1.4189(19) . ? C18 H18 0.9500 . ? C19 O19 1.3024(17) . ? C19 C19A 1.4131(19) . ? C19A C19B 1.420(2) . ? O21 C21 1.3039(17) . ? C21 C29A 1.414(2) . ? C21 C22 1.4167(19) . ? C22 C23 1.372(2) . ? C22 H22 0.9500 . ? C23 O23" 1.3420(17) . ? C23 C23A 1.448(2) . ? C23A C24 1.401(2) . ? C23A C29B 1.4179(19) . ? O23" C23" 1.447(2) . ? C23" H23A 0.9800 . ? C23" H23B 0.9800 . ? C23" H23C 0.9800 . ? C24 C25 1.390(2) . ? C24 H24 0.9500 . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 C26A 1.400(2) . ? C26 H26 0.9500 . ? C26A C29B 1.414(2) . ? C26A C27 1.448(2) . ? C27 O27" 1.3457(18) . ? C27 C28 1.373(2) . ? C27" O27" 1.441(2) . ? C27" H27A 0.9800 . ? C27" H27B 0.9800 . ? C27" H27C 0.9800 . ? C28 C29 1.417(2) . ? C28 H28 0.9500 . ? C29 O29 1.3047(17) . ? C29 C29A 1.4163(19) . ? C29A C29B 1.4241(19) . ? B1' C7' 1.642(2) . ? B1' C13' 1.643(2) . ? B1' C1' 1.646(2) . ? B1' C19' 1.651(2) . ? C1' C2' 1.397(2) . ? C1' C6' 1.414(2) . ? C2' C3' 1.395(2) . ? C2' H2' 0.9500 . ? C3' C4' 1.384(2) . ? C3' H3' 0.9500 . ? C4' C5' 1.387(3) . ? C4' H4' 0.9500 . ? C5' C6' 1.391(2) . ? C5' H5' 0.9500 . ? C6' H6' 0.9500 . ? C7' C8' 1.398(2) . ? C7' C12' 1.412(2) . ? C8' C9' 1.402(2) . ? C8' H8' 0.9500 . ? C9' C10' 1.375(3) . ? C9' H9' 0.9500 . ? C10' C11' 1.390(3) . ? C10' H10' 0.9500 . ? C11' C12' 1.392(2) . ? C11' H11' 0.9500 . ? C12' H12' 0.9500 . ? C13' C14' 1.401(2) . ? C13' C18' 1.407(2) . ? C14' C15' 1.396(2) . ? C14' H14' 0.9500 . ? C15' C16' 1.384(3) . ? C15' H15' 0.9500 . ? C16' C17' 1.394(3) . ? C16' H16' 0.9500 . ? C17' C18' 1.392(3) . ? C17' H17' 0.9500 . ? C18' H18' 0.9500 . ? C19' C20' 1.400(2) . ? C19' C24' 1.408(2) . ? C20' C21' 1.400(2) . ? C20' H20' 0.9500 . ? C21' C22' 1.381(3) . ? C21' H21' 0.9500 . ? C22' C23' 1.390(3) . ? C22' H22' 0.9500 . ? C23' C24' 1.393(2) . ? C23' H23' 0.9500 . ? C24' H24' 0.9500 . ? C1S Cl2S 1.766(5) . ? C1S Cl1S 1.771(5) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C1D Cl2D 1.771(7) . ? C1D Cl1D 1.774(7) . ? C1D H1D1 0.9900 . ? C1D H1D2 0.9900 . ? C2S Cl3S 1.723(7) . ? C2S Cl4S 1.733(5) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2D Cl3D 1.763(6) . ? C2D Cl4D 1.766(5) . ? C2D H2DA 0.9900 . ? C2D H2DB 0.9900 . ? 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 O9 Si1 O1 94.91(5) . . ? O9 Si1 O19 88.12(5) . . ? O1 Si1 O19 89.38(5) . . ? O9 Si1 O21 91.35(5) . . ? O1 Si1 O21 87.98(5) . . ? O19 Si1 O21 177.26(6) . . ? O9 Si1 O29 86.84(5) . . ? O1 Si1 O29 176.91(5) . . ? O19 Si1 O29 88.13(5) . . ? O21 Si1 O29 94.52(5) . . ? O9 Si1 O11 176.26(6) . . ? O1 Si1 O11 88.02(5) . . ? O19 Si1 O11 94.24(5) . . ? O21 Si1 O11 86.43(5) . . ? O29 Si1 O11 90.33(5) . . ? C1 O1 Si1 127.74(10) . . ? O1 C1 C2 117.18(13) . . ? O1 C1 C9A 122.52(13) . . ? C2 C1 C9A 120.31(13) . . ? C3 C2 C1 120.30(14) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? O3" C3 C2 124.04(15) . . ? O3" C3 C3A 114.61(13) . . ? C2 C3 C3A 121.35(14) . . ? C4 C3A C9B 119.86(14) . . ? C4 C3A C3 122.01(14) . . ? C9B C3A C3 118.13(13) . . ? C3 O3" C3" 117.19(14) . . ? O3" C3" H3"1 109.5 . . ? O3" C3" H3"2 109.5 . . ? H3"1 C3" H3"2 109.5 . . ? O3" C3" H3"3 109.5 . . ? H3"1 C3" H3"3 109.5 . . ? H3"2 C3" H3"3 109.5 . . ? C5 C4 C3A 120.38(15) . . ? C5 C4 H4 119.8 . . ? C3A C4 H4 119.8 . . ? C4 C5 C6 120.57(14) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C6A 120.34(15) . . ? C5 C6 H6 119.8 . . ? C6A C6 H6 119.8 . . ? C6 C6A C9B 119.74(14) . . ? C6 C6A C7 122.14(14) . . ? C9B C6A C7 118.10(13) . . ? O7" C7 C8 124.17(14) . . ? O7" C7 C6A 114.34(13) . . ? C8 C7 C6A 121.47(13) . . ? C7 O7" C7" 117.20(13) . . ? O7" C7" H7"1 109.5 . . ? O7" C7" H7"2 109.5 . . ? H7"1 C7" H7"2 109.5 . . ? O7" C7" H7"3 109.5 . . ? H7"1 C7" H7"3 109.5 . . ? H7"2 C7" H7"3 109.5 . . ? C7 C8 C9 119.91(14) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? O9 C9 C8 117.54(13) . . ? O9 C9 C9A 121.83(13) . . ? C8 C9 C9A 120.63(13) . . ? C9 O9 Si1 128.37(10) . . ? C1 C9A C9 121.19(12) . . ? C1 C9A C9B 119.53(13) . . ? C9 C9A C9B 119.25(13) . . ? C3A C9B C6A 119.09(13) . . ? C3A C9B C9A 120.35(13) . . ? C6A C9B C9A 120.56(13) . . ? C11 O11 Si1 128.30(10) . . ? O11 C11 C19A 122.05(13) . . ? O11 C11 C12 117.19(13) . . ? C19A C11 C12 120.75(13) . . ? C13 C12 C11 119.77(14) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? O13" C13 C12 124.38(15) . . ? O13" C13 C13A 114.23(14) . . ? C12 C13 C13A 121.38(14) . . ? C14 C13A C19B 119.84(14) . . ? C14 C13A C13 121.84(14) . . ? C19B C13A C13 118.32(14) . . ? C13 O13" C13" 118.41(14) . . ? O13" C13" H13A 109.5 . . ? O13" C13" H13B 109.5 . . ? H13A C13" H13B 109.5 . . ? O13" C13" H13C 109.5 . . ? H13A C13" H13C 109.5 . . ? H13B C13" H13C 109.5 . . ? C15 C14 C13A 120.32(15) . . ? C15 C14 H14 119.8 . . ? C13A C14 H14 119.8 . . ? C16 C15 C14 120.52(15) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C16A 120.58(15) . . ? C15 C16 H16 119.7 . . ? C16A C16 H16 119.7 . . ? C16 C16A C19B 119.54(14) . . ? C16 C16A C17 122.38(14) . . ? C19B C16A C17 118.08(13) . . ? O17" C17 C18 123.97(14) . . ? O17" C17 C16A 114.57(13) . . ? C18 C17 C16A 121.45(13) . . ? C17 O17" C17" 117.64(13) . . ? O17" C17" H17A 109.5 . . ? O17" C17" H17B 109.5 . . ? H17A C17" H17B 109.5 . . ? O17" C17" H17C 109.5 . . ? H17A C17" H17C 109.5 . . ? H17B C17" H17C 109.5 . . ? C17 C18 C19 120.10(13) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? O19 C19 C19A 122.76(12) . . ? O19 C19 C18 117.00(12) . . ? C19A C19 C18 120.23(13) . . ? C19 O19 Si1 128.13(9) . . ? C11 C19A C19 121.10(13) . . ? C11 C19A C19B 119.35(13) . . ? C19 C19A C19B 119.53(13) . . ? C16A C19B C19A 120.52(13) . . ? C16A C19B C13A 119.17(14) . . ? C19A C19B C13A 120.31(13) . . ? C21 O21 Si1 126.61(9) . . ? O21 C21 C29A 122.24(12) . . ? O21 C21 C22 117.16(13) . . ? C29A C21 C22 120.56(13) . . ? C23 C22 C21 120.00(14) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? O23" C23 C22 124.13(14) . . ? O23" C23 C23A 114.52(13) . . ? C22 C23 C23A 121.35(13) . . ? C24 C23A C29B 119.69(14) . . ? C24 C23A C23 121.97(13) . . ? C29B C23A C23 118.33(13) . . ? C23 O23" C23" 117.50(12) . . ? O23" C23" H23A 109.5 . . ? O23" C23" H23B 109.5 . . ? H23A C23" H23B 109.5 . . ? O23" C23" H23C 109.5 . . ? H23A C23" H23C 109.5 . . ? H23B C23" H23C 109.5 . . ? C25 C24 C23A 120.52(14) . . ? C25 C24 H24 119.7 . . ? C23A C24 H24 119.7 . . ? C24 C25 C26 120.16(14) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C26A 120.71(15) . . ? C25 C26 H26 119.6 . . ? C26A C26 H26 119.6 . . ? C26 C26A C29B 119.64(14) . . ? C26 C26A C27 122.30(14) . . ? C29B C26A C27 118.06(13) . . ? O27" C27 C28 124.42(14) . . ? O27" C27 C26A 113.94(13) . . ? C28 C27 C26A 121.63(14) . . ? O27" C27" H27A 109.5 . . ? O27" C27" H27B 109.5 . . ? H27A C27" H27B 109.5 . . ? O27" C27" H27C 109.5 . . ? H27A C27" H27C 109.5 . . ? H27B C27" H27C 109.5 . . ? C27 O27" C27" 117.74(13) . . ? C27 C28 C29 119.84(13) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? O29 C29 C29A 122.36(13) . . ? O29 C29 C28 117.16(12) . . ? C29A C29 C28 120.47(13) . . ? C29 O29 Si1 127.86(9) . . ? C21 C29A C29 121.04(13) . . ? C21 C29A C29B 119.49(12) . . ? C29 C29A C29B 119.39(13) . . ? C26A C29B C23A 119.27(13) . . ? C26A C29B C29A 120.53(13) . . ? C23A C29B C29A 120.20(13) . . ? C7' B1' C13' 112.58(13) . . ? C7' B1' C1' 111.07(13) . . ? C13' B1' C1' 106.03(12) . . ? C7' B1' C19' 105.78(12) . . ? C13' B1' C19' 109.60(13) . . ? C1' B1' C19' 111.88(13) . . ? C2' C1' C6' 114.85(14) . . ? C2' C1' B1' 125.70(14) . . ? C6' C1' B1' 119.40(14) . . ? C3' C2' C1' 122.81(15) . . ? C3' C2' H2' 118.6 . . ? C1' C2' H2' 118.6 . . ? C4' C3' C2' 120.53(16) . . ? C4' C3' H3' 119.7 . . ? C2' C3' H3' 119.7 . . ? C3' C4' C5' 118.78(15) . . ? C3' C4' H4' 120.6 . . ? C5' C4' H4' 120.6 . . ? C4' C5' C6' 120.02(16) . . ? C4' C5' H5' 120.0 . . ? C6' C5' H5' 120.0 . . ? C5' C6' C1' 123.01(15) . . ? C5' C6' H6' 118.5 . . ? C1' C6' H6' 118.5 . . ? C8' C7' C12' 115.26(15) . . ? C8' C7' B1' 125.17(14) . . ? C12' C7' B1' 119.53(15) . . ? C7' C8' C9' 122.59(16) . . ? C7' C8' H8' 118.7 . . ? C9' C8' H8' 118.7 . . ? C10' C9' C8' 120.10(18) . . ? C10' C9' H9' 120.0 . . ? C8' C9' H9' 120.0 . . ? C9' C10' C11' 119.59(16) . . ? C9' C10' H10' 120.2 . . ? C11' C10' H10' 120.2 . . ? C10' C11' C12' 119.69(17) . . ? C10' C11' H11' 120.2 . . ? C12' C11' H11' 120.2 . . ? C11' C12' C7' 122.77(17) . . ? C11' C12' H12' 118.6 . . ? C7' C12' H12' 118.6 . . ? C14' C13' C18' 115.55(16) . . ? C14' C13' B1' 125.63(14) . . ? C18' C13' B1' 118.81(14) . . ? C15' C14' C13' 122.30(16) . . ? C15' C14' H14' 118.9 . . ? C13' C14' H14' 118.9 . . ? C16' C15' C14' 120.66(17) . . ? C16' C15' H15' 119.7 . . ? C14' C15' H15' 119.7 . . ? C15' C16' C17' 118.65(17) . . ? C15' C16' H16' 120.7 . . ? C17' C16' H16' 120.7 . . ? C18' C17' C16' 120.10(18) . . ? C18' C17' H17' 120.0 . . ? C16' C17' H17' 120.0 . . ? C17' C18' C13' 122.69(17) . . ? C17' C18' H18' 118.7 . . ? C13' C18' H18' 118.7 . . ? C20' C19' C24' 115.25(15) . . ? C20' C19' B1' 124.33(15) . . ? C24' C19' B1' 120.37(14) . . ? C19' C20' C21' 122.47(17) . . ? C19' C20' H20' 118.8 . . ? C21' C20' H20' 118.8 . . ? C22' C21' C20' 120.33(17) . . ? C22' C21' H21' 119.8 . . ? C20' C21' H21' 119.8 . . ? C21' C22' C23' 119.13(16) . . ? C21' C22' H22' 120.4 . . ? C23' C22' H22' 120.4 . . ? C22' C23' C24' 119.83(17) . . ? C22' C23' H23' 120.1 . . ? C24' C23' H23' 120.1 . . ? C23' C24' C19' 122.89(17) . . ? C23' C24' H24' 118.6 . . ? C19' C24' H24' 118.6 . . ? Cl2S C1S Cl1S 108.7(4) . . ? Cl2S C1S H1SA 110.0 . . ? Cl1S C1S H1SA 110.0 . . ? Cl2S C1S H1SB 110.0 . . ? Cl1S C1S H1SB 110.0 . . ? H1SA C1S H1SB 108.3 . . ? Cl2D C1D Cl1D 113.8(7) . . ? Cl2D C1D H1D1 108.8 . . ? Cl1D C1D H1D1 108.8 . . ? Cl2D C1D H1D2 108.8 . . ? Cl1D C1D H1D2 108.8 . . ? H1D1 C1D H1D2 107.7 . . ? Cl3S C2S Cl4S 111.2(4) . . ? Cl3S C2S H2SA 109.4 . . ? Cl4S C2S H2SA 109.4 . . ? Cl3S C2S H2SB 109.4 . . ? Cl4S C2S H2SB 109.4 . . ? H2SA C2S H2SB 108.0 . . ? Cl3D C2D Cl4D 109.5(3) . . ? Cl3D C2D H2DA 109.8 . . ? Cl4D C2D H2DA 109.8 . . ? Cl3D C2D H2DB 109.8 . . ? Cl4D C2D H2DB 109.8 . . ? H2DA C2D H2DB 108.2 . . ? 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 O9 Si1 O1 C1 -19.08(12) . . . . ? O19 Si1 O1 C1 -107.13(12) . . . . ? O21 Si1 O1 C1 72.11(12) . . . . ? O29 Si1 O1 C1 -143.6(9) . . . . ? O11 Si1 O1 C1 158.60(12) . . . . ? Si1 O1 C1 C2 -168.09(10) . . . . ? Si1 O1 C1 C9A 12.41(19) . . . . ? O1 C1 C2 C3 179.38(13) . . . . ? C9A C1 C2 C3 -1.1(2) . . . . ? C1 C2 C3 O3" -177.91(13) . . . . ? C1 C2 C3 C3A 2.2(2) . . . . ? O3" C3 C3A C4 -0.6(2) . . . . ? C2 C3 C3A C4 179.33(14) . . . . ? O3" C3 C3A C9B 178.62(12) . . . . ? C2 C3 C3A C9B -1.5(2) . . . . ? C2 C3 O3" C3" 4.3(2) . . . . ? C3A C3 O3" C3" -175.79(14) . . . . ? C9B C3A C4 C5 1.4(2) . . . . ? C3 C3A C4 C5 -179.43(14) . . . . ? C3A C4 C5 C6 -0.8(2) . . . . ? C4 C5 C6 C6A -0.6(2) . . . . ? C5 C6 C6A C9B 1.3(2) . . . . ? C5 C6 C6A C7 -177.50(14) . . . . ? C6 C6A C7 O7" 2.9(2) . . . . ? C9B C6A C7 O7" -175.95(12) . . . . ? C6 C6A C7 C8 -178.18(14) . . . . ? C9B C6A C7 C8 3.0(2) . . . . ? C8 C7 O7" C7" 1.1(2) . . . . ? C6A C7 O7" C7" 179.98(14) . . . . ? O7" C7 C8 C9 176.48(13) . . . . ? C6A C7 C8 C9 -2.4(2) . . . . ? C7 C8 C9 O9 -179.83(12) . . . . ? C7 C8 C9 C9A 0.1(2) . . . . ? C8 C9 O9 Si1 166.93(10) . . . . ? C9A C9 O9 Si1 -12.98(19) . . . . ? O1 Si1 O9 C9 19.49(12) . . . . ? O19 Si1 O9 C9 108.71(12) . . . . ? O21 Si1 O9 C9 -68.60(12) . . . . ? O29 Si1 O9 C9 -163.06(12) . . . . ? O11 Si1 O9 C9 -122.2(8) . . . . ? O1 C1 C9A C9 0.6(2) . . . . ? C2 C1 C9A C9 -178.93(13) . . . . ? O1 C1 C9A C9B 178.81(12) . . . . ? C2 C1 C9A C9B -0.7(2) . . . . ? O9 C9 C9A C1 -0.3(2) . . . . ? C8 C9 C9A C1 179.75(13) . . . . ? O9 C9 C9A C9B -178.59(12) . . . . ? C8 C9 C9A C9B 1.5(2) . . . . ? C4 C3A C9B C6A -0.7(2) . . . . ? C3 C3A C9B C6A -179.89(13) . . . . ? C4 C3A C9B C9A 178.89(13) . . . . ? C3 C3A C9B C9A -0.3(2) . . . . ? C6 C6A C9B C3A -0.7(2) . . . . ? C7 C6A C9B C3A 178.19(13) . . . . ? C6 C6A C9B C9A 179.78(13) . . . . ? C7 C6A C9B C9A -1.4(2) . . . . ? C1 C9A C9B C3A 1.4(2) . . . . ? C9 C9A C9B C3A 179.65(12) . . . . ? C1 C9A C9B C6A -179.08(12) . . . . ? C9 C9A C9B C6A -0.8(2) . . . . ? O9 Si1 O11 C11 -109.0(8) . . . . ? O1 Si1 O11 C11 109.16(13) . . . . ? O19 Si1 O11 C11 19.93(14) . . . . ? O21 Si1 O11 C11 -162.74(14) . . . . ? O29 Si1 O11 C11 -68.22(13) . . . . ? Si1 O11 C11 C19A -13.3(2) . . . . ? Si1 O11 C11 C12 167.51(11) . . . . ? O11 C11 C12 C13 -177.62(15) . . . . ? C19A C11 C12 C13 3.2(2) . . . . ? C11 C12 C13 O13" 178.11(16) . . . . ? C11 C12 C13 C13A -2.3(3) . . . . ? O13" C13 C13A C14 -0.4(3) . . . . ? C12 C13 C13A C14 180.00(18) . . . . ? O13" C13 C13A C19B 178.83(15) . . . . ? C12 C13 C13A C19B -0.8(3) . . . . ? C12 C13 O13" C13" 3.1(3) . . . . ? C13A C13 O13" C13" -176.57(17) . . . . ? C19B C13A C14 C15 -0.8(3) . . . . ? C13 C13A C14 C15 178.41(18) . . . . ? C13A C14 C15 C16 -0.8(3) . . . . ? C14 C15 C16 C16A 1.1(3) . . . . ? C15 C16 C16A C19B 0.2(3) . . . . ? C15 C16 C16A C17 179.91(17) . . . . ? C16 C16A C17 O17" 1.9(2) . . . . ? C19B C16A C17 O17" -178.29(14) . . . . ? C16 C16A C17 C18 -178.29(16) . . . . ? C19B C16A C17 C18 1.5(2) . . . . ? C18 C17 O17" C17" 0.5(2) . . . . ? C16A C17 O17" C17" -179.70(15) . . . . ? O17" C17 C18 C19 -179.35(15) . . . . ? C16A C17 C18 C19 0.9(2) . . . . ? C17 C18 C19 O19 177.79(14) . . . . ? C17 C18 C19 C19A -3.0(2) . . . . ? C19A C19 O19 Si1 9.7(2) . . . . ? C18 C19 O19 Si1 -171.11(11) . . . . ? O9 Si1 O19 C19 159.07(13) . . . . ? O1 Si1 O19 C19 -105.99(13) . . . . ? O21 Si1 O19 C19 -122.0(12) . . . . ? O29 Si1 O19 C19 72.17(13) . . . . ? O11 Si1 O19 C19 -18.02(13) . . . . ? O11 C11 C19A C19 -1.7(2) . . . . ? C12 C11 C19A C19 177.45(15) . . . . ? O11 C11 C19A C19B 179.96(15) . . . . ? C12 C11 C19A C19B -0.9(2) . . . . ? O19 C19 C19A C11 3.5(2) . . . . ? C18 C19 C19A C11 -175.61(14) . . . . ? O19 C19 C19A C19B -178.17(14) . . . . ? C18 C19 C19A C19B 2.7(2) . . . . ? C16 C16A C19B C19A 177.99(16) . . . . ? C17 C16A C19B C19A -1.8(2) . . . . ? C16 C16A C19B C13A -1.7(2) . . . . ? C17 C16A C19B C13A 178.58(15) . . . . ? C11 C19A C19B C16A 178.06(15) . . . . ? C19 C19A C19B C16A -0.3(2) . . . . ? C11 C19A C19B C13A -2.3(2) . . . . ? C19 C19A C19B C13A 179.38(15) . . . . ? C14 C13A C19B C16A 2.0(3) . . . . ? C13 C13A C19B C16A -177.24(15) . . . . ? C14 C13A C19B C19A -177.68(17) . . . . ? C13 C13A C19B C19A 3.1(2) . . . . ? O9 Si1 O21 C21 -113.29(12) . . . . ? O1 Si1 O21 C21 151.84(12) . . . . ? O19 Si1 O21 C21 167.9(11) . . . . ? O29 Si1 O21 C21 -26.35(13) . . . . ? O11 Si1 O21 C21 63.70(12) . . . . ? Si1 O21 C21 C29A 22.2(2) . . . . ? Si1 O21 C21 C22 -160.20(11) . . . . ? O21 C21 C22 C23 -176.71(14) . . . . ? C29A C21 C22 C23 1.0(2) . . . . ? C21 C22 C23 O23" -178.39(14) . . . . ? C21 C22 C23 C23A 1.3(2) . . . . ? O23" C23 C23A C24 -0.8(2) . . . . ? C22 C23 C23A C24 179.48(15) . . . . ? O23" C23 C23A C29B 178.16(13) . . . . ? C22 C23 C23A C29B -1.6(2) . . . . ? C22 C23 O23" C23" 1.6(2) . . . . ? C23A C23 O23" C23" -178.10(14) . . . . ? C29B C23A C24 C25 0.7(2) . . . . ? C23 C23A C24 C25 179.65(15) . . . . ? C23A C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C26A -0.6(3) . . . . ? C25 C26 C26A C29B 0.0(2) . . . . ? C25 C26 C26A C27 179.60(16) . . . . ? C26 C26A C27 O27" 1.6(2) . . . . ? C29B C26A C27 O27" -178.77(14) . . . . ? C26 C26A C27 C28 -179.66(15) . . . . ? C29B C26A C27 C28 -0.1(2) . . . . ? C28 C27 O27" C27" 0.0(2) . . . . ? C26A C27 O27" C27" 178.63(14) . . . . ? O27" C27 C28 C29 176.26(15) . . . . ? C26A C27 C28 C29 -2.3(2) . . . . ? C27 C28 C29 O29 -175.82(14) . . . . ? C27 C28 C29 C29A 3.2(2) . . . . ? C29A C29 O29 Si1 -5.9(2) . . . . ? C28 C29 O29 Si1 173.14(10) . . . . ? O9 Si1 O29 C29 109.37(13) . . . . ? O1 Si1 O29 C29 -125.9(10) . . . . ? O19 Si1 O29 C29 -162.41(13) . . . . ? O21 Si1 O29 C29 18.26(13) . . . . ? O11 Si1 O29 C29 -68.19(13) . . . . ? O21 C21 C29A C29 -2.3(2) . . . . ? C22 C21 C29A C29 -179.82(14) . . . . ? O21 C21 C29A C29B 174.59(13) . . . . ? C22 C21 C29A C29B -3.0(2) . . . . ? O29 C29 C29A C21 -5.9(2) . . . . ? C28 C29 C29A C21 175.07(14) . . . . ? O29 C29 C29A C29B 177.23(13) . . . . ? C28 C29 C29A C29B -1.8(2) . . . . ? C26 C26A C29B C23A 0.9(2) . . . . ? C27 C26A C29B C23A -178.67(14) . . . . ? C26 C26A C29B C29A -178.87(14) . . . . ? C27 C26A C29B C29A 1.5(2) . . . . ? C24 C23A C29B C26A -1.3(2) . . . . ? C23 C23A C29B C26A 179.73(14) . . . . ? C24 C23A C29B C29A 178.51(14) . . . . ? C23 C23A C29B C29A -0.5(2) . . . . ? C21 C29A C29B C26A -177.51(14) . . . . ? C29 C29A C29B C26A -0.6(2) . . . . ? C21 C29A C29B C23A 2.7(2) . . . . ? C29 C29A C29B C23A 179.58(14) . . . . ? C7' B1' C1' C2' 118.90(16) . . . . ? C13' B1' C1' C2' -118.49(16) . . . . ? C19' B1' C1' C2' 0.9(2) . . . . ? C7' B1' C1' C6' -64.04(19) . . . . ? C13' B1' C1' C6' 58.56(18) . . . . ? C19' B1' C1' C6' 178.00(14) . . . . ? C6' C1' C2' C3' 0.3(2) . . . . ? B1' C1' C2' C3' 177.48(15) . . . . ? C1' C2' C3' C4' -0.3(3) . . . . ? C2' C3' C4' C5' 0.3(3) . . . . ? C3' C4' C5' C6' -0.4(3) . . . . ? C4' C5' C6' C1' 0.4(3) . . . . ? C2' C1' C6' C5' -0.3(2) . . . . ? B1' C1' C6' C5' -177.71(15) . . . . ? C13' B1' C7' C8' -113.76(17) . . . . ? C1' B1' C7' C8' 5.0(2) . . . . ? C19' B1' C7' C8' 126.57(16) . . . . ? C13' B1' C7' C12' 68.51(19) . . . . ? C1' B1' C7' C12' -172.75(15) . . . . ? C19' B1' C7' C12' -51.16(19) . . . . ? C12' C7' C8' C9' 0.0(3) . . . . ? B1' C7' C8' C9' -177.81(16) . . . . ? C7' C8' C9' C10' 0.1(3) . . . . ? C8' C9' C10' C11' -0.3(3) . . . . ? C9' C10' C11' C12' 0.3(3) . . . . ? C10' C11' C12' C7' -0.2(3) . . . . ? C8' C7' C12' C11' 0.0(3) . . . . ? B1' C7' C12' C11' 177.96(16) . . . . ? C7' B1' C13' C14' -3.5(2) . . . . ? C1' B1' C13' C14' -125.18(16) . . . . ? C19' B1' C13' C14' 113.90(17) . . . . ? C7' B1' C13' C18' 175.67(14) . . . . ? C1' B1' C13' C18' 54.02(18) . . . . ? C19' B1' C13' C18' -66.90(18) . . . . ? C18' C13' C14' C15' 0.8(2) . . . . ? B1' C13' C14' C15' -179.98(15) . . . . ? C13' C14' C15' C16' 1.3(3) . . . . ? C14' C15' C16' C17' -1.9(3) . . . . ? C15' C16' C17' C18' 0.3(3) . . . . ? C16' C17' C18' C13' 1.9(3) . . . . ? C14' C13' C18' C17' -2.4(2) . . . . ? B1' C13' C18' C17' 178.30(16) . . . . ? C7' B1' C19' C20' 112.20(16) . . . . ? C13' B1' C19' C20' -9.4(2) . . . . ? C1' B1' C19' C20' -126.73(16) . . . . ? C7' B1' C19' C24' -65.16(18) . . . . ? C13' B1' C19' C24' 173.22(14) . . . . ? C1' B1' C19' C24' 55.91(19) . . . . ? C24' C19' C20' C21' -2.4(2) . . . . ? B1' C19' C20' C21' -179.87(15) . . . . ? C19' C20' C21' C22' -0.1(3) . . . . ? C20' C21' C22' C23' 1.6(3) . . . . ? C21' C22' C23' C24' -0.5(3) . . . . ? C22' C23' C24' C19' -2.2(3) . . . . ? C20' C19' C24' C23' 3.6(2) . . . . ? B1' C19' C24' C23' -178.85(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.927 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.070