# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Barbara Becker' 'Katarzyna Baranowska' 'Jaroslaw Chojnacki' 'Wieslaw Wojnowski' _publ_contact_author_name 'Dr Barbara Becker' _publ_contact_author_address ; Chemical Faculty Gdansk University of Technology G. Narutowicza 11/12 Gdansk 80-952 POLAND ; _publ_contact_author_email BECKERB@CHEM.PG.GDA.PL _publ_requested_journal 'Chemical Communications' _publ_section_title ; Cubane-Like Structure of a Silanethiol - Primary Amine Assembly - a Novel, Unusual Hydrogen Bond Pattern ; data_2 _database_code_depnum_ccdc_archive 'CCDC 214671' _chemical_name_common 'Tert-butylammonium triisopropoxysilanethiolate' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tert-butylammonium triisopropoxysilanethiolate ; _chemical_melting_point 128-130 _chemical_formula_moiety 'C9 H21 O3 S Si, C4 H12 N' _chemical_formula_sum 'C13 H33 N O3 S Si' _chemical_formula_weight 311.55 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 m' _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 15.974(2) _cell_length_b 15.974(2) _cell_length_c 15.974(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4076.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 200.0(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 13.3 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200.0(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 'KM4 Oxford Diffraction' _diffrn_measurement_method '\w--1.4\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 531 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.54 _reflns_number_total 531 _reflns_number_gt 440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 System (Ga\/ldecki, 1996)' _computing_cell_refinement 'KM4 System (Ga\/ldecki, 1996)' _computing_data_reduction 'DATAPROC (Ga\/ldecki, 1996)' _computing_structure_solution 'SHELXS - 97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL - 97 (Sheldrick, 1997)' _computing_molecular_graphics 'RESVIEW, (Schwenk, 1998)' _computing_publication_material 'SHELXL - 97 (Sheldrick, 1997)' _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^)+(0.1096P)^2^+3.5511P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(5) _refine_ls_number_reflns 531 _refine_ls_number_parameters 41 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 S1 S 0.39664(8) 0.60336(8) 0.60336(8) 0.0416(6) Uani 1 6 d S . . Si2 Si 0.32216(10) 0.67784(10) 0.67784(10) 0.0504(8) Uani 1 6 d S . . O1 O 0.3354(3) 0.6646(3) 0.7753(3) 0.128(3) Uani 1 2 d S . . C20 C 0.3825(4) 0.6175(4) 0.8252(5) 0.078(2) Uani 1 2 d S . . H20A H 0.4199 0.5801 0.7937 0.117 Uiso 1 2 d SR . . C21 C 0.3252(12) 0.5657(8) 0.8776(10) 0.245(9) Uani 1 1 d . . . H21A H 0.2938 0.5220 0.8487 0.367 Uiso 1 1 d R . . H21B H 0.3651 0.5311 0.9156 0.367 Uiso 1 1 d R . . H21C H 0.2959 0.6003 0.9078 0.367 Uiso 1 1 d R . . N1 N 0.4001(2) 0.4001(2) 0.5999(2) 0.0412(15) Uani 1 6 d S . . H1A H 0.3882 0.4583 0.6118 0.062 Uiso 1 2 d SR . . C1 C 0.3454(3) 0.3454(3) 0.6546(3) 0.047(2) Uani 1 6 d S . . C2 C 0.3655(4) 0.3655(4) 0.7429(5) 0.149(6) Uani 1 2 d S . . H2A H 0.3314 0.3315 0.7805 0.223 Uiso 1 2 d SR . . H2B H 0.4241 0.3512 0.7580 0.223 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0416(6) 0.0416(6) 0.0416(6) -0.0035(5) 0.0035(5) 0.0035(5) Si2 0.0504(8) 0.0504(8) 0.0504(8) -0.0082(6) 0.0082(6) 0.0082(6) O1 0.171(5) 0.171(5) 0.043(2) -0.0076(17) 0.0076(17) 0.115(6) C20 0.091(4) 0.091(4) 0.052(3) -0.011(3) 0.011(3) 0.019(5) C21 0.35(2) 0.135(9) 0.249(14) 0.040(10) 0.188(15) 0.010(10) N1 0.0412(15) 0.0412(15) 0.0412(15) 0.004(2) 0.004(2) -0.004(2) C1 0.047(2) 0.047(2) 0.047(2) 0.006(2) 0.006(2) -0.006(2) C2 0.201(9) 0.201(9) 0.045(4) 0.001(3) 0.001(3) -0.134(11) _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 S1 Si2 2.061(3) . yes Si2 O1 1.585(5) 7_665 yes Si2 O1 1.585(5) . yes Si2 O1 1.585(5) 10_656 yes O1 C20 1.329(9) . no C20 C21 1.491(12) 14_665 no C20 C21 1.491(12) . no C20 H20A 0.9834 . no C21 H21A 0.9757 . no C21 H21B 1.0386 . no C21 H21C 0.8710 . no N1 C1 1.514(11) . yes N1 H1A 0.9681 . no C1 C2 1.481(9) 8_656 no C1 C2 1.481(9) . no C1 C2 1.481(9) 11_566 no C2 H2A 0.9765 . no C2 H2B 0.9930 . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si2 O1 104.1(3) 7_665 . no O1 Si2 O1 104.1(3) 7_665 10_656 no O1 Si2 O1 104.1(3) . 10_656 no O1 Si2 S1 114.4(2) 7_665 . no O1 Si2 S1 114.4(2) . . no O1 Si2 S1 114.4(2) 10_656 . no C20 O1 Si2 137.7(5) . . no O1 C20 C21 107.7(9) . 14_665 no O1 C20 C21 107.7(9) . . no C21 C20 C21 111.5(16) 14_665 . no O1 C20 H20A 112.4 . . no C21 C20 H20A 108.8 14_665 . no C21 C20 H20A 108.8 . . no C20 C21 H21A 116.6 . . no C20 C21 H21B 104.3 . . no H21A C21 H21B 102.2 . . no C20 C21 H21C 106.8 . . no H21A C21 H21C 116.1 . . no H21B C21 H21C 110.0 . . no C1 N1 H1A 109.1 . . no C2 C1 C2 111.4(5) 8_656 . no C2 C1 C2 111.4(5) 8_656 11_566 no C2 C1 C2 111.4(5) . 11_566 no C2 C1 N1 107.4(5) 8_656 . no C2 C1 N1 107.4(5) . . no C2 C1 N1 107.4(5) 11_566 . no C1 C2 H2A 110.2 . . no C1 C2 H2B 112.7 . . no H2A C2 H2B 104.3 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A S1 0.97 2.32 3.248(4) 159.2 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.306 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.055 data_1 _database_code_depnum_ccdc_archive 'CCDC 215024' _chemical_name_common 'Tert-butylammonium tri-tert-butoxysilanethiolate' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tert-butylammonium tri-tert-butoxysilanethiolate ; _chemical_formula_moiety 'C12 H27 O3 S Si, C4 H12 N' _chemical_formula_sum 'C16 H39 N O3 S Si' _chemical_formula_weight 353.63 _chemical_melting_point 98-99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.786(6) _cell_length_b 13.892(3) _cell_length_c 26.858(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.74(3) _cell_angle_gamma 90.00 _cell_volume 9339(4) _cell_formula_units_Z 16 _cell_measurement_temperature 200.0(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200.0(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 'KM4 Oxford Diffraction' _diffrn_measurement_method '\w--1.4\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.67 _diffrn_reflns_number 14148 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.08 _reflns_number_total 7583 _reflns_number_gt 4598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 System (Ga\/ldecki, 1996)' _computing_cell_refinement 'KM4 System (Ga\/ldecki, 1996)' _computing_data_reduction 'DATAPROC (Ga\/ldecki, 1996)' _computing_structure_solution 'SHELXS - 97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL - 97 (Sheldrick, 1997)' _computing_molecular_graphics 'RESVIEW, (Schwenk, 1998)' _computing_publication_material 'SHELXL - 97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+13.9065P] 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 7583 _refine_ls_number_parameters 445 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.020 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.05647(3) 0.68154(5) 0.19950(3) 0.0370(2) Uani 1 d . . . Si1 Si 0.10483(3) 0.59174(6) 0.17994(3) 0.0328(2) Uani 1 d . . . O1 O 0.16623(8) 0.58423(17) 0.22825(9) 0.0468(6) Uani 1 d . . . O2 O 0.08075(8) 0.48348(14) 0.17442(9) 0.0438(5) Uani 1 d . . . O3 O 0.11200(8) 0.62213(16) 0.12524(9) 0.0451(5) Uani 1 d . . . C30 C 0.07754(15) 0.6564(3) 0.07067(14) 0.0537(9) Uani 1 d . . . C31 C 0.1014(2) 0.6197(4) 0.03352(17) 0.0909(16) Uani 1 d . . . H31A H 0.1368 0.6454 0.0465 0.109 Uiso 1 d R . . H31B H 0.1030 0.5507 0.0349 0.109 Uiso 1 d R . . H31C H 0.0803 0.6401 -0.0039 0.109 Uiso 1 d R . . C32 C 0.02162(17) 0.6186(4) 0.05194(16) 0.0828(14) Uani 1 d . . . H32A H 0.0063 0.6423 0.0755 0.099 Uiso 1 d R . . H32B H 0.0001 0.6390 0.0146 0.099 Uiso 1 d R . . H32C H 0.0228 0.5495 0.0534 0.099 Uiso 1 d R . . C33 C 0.0778(2) 0.7642(3) 0.07292(19) 0.0888(15) Uani 1 d . . . H33A H 0.0616 0.7858 0.0961 0.107 Uiso 1 d R . . H33B H 0.1141 0.7865 0.0877 0.107 Uiso 1 d R . . H33C H 0.0582 0.7895 0.0363 0.107 Uiso 1 d R . . C20 C 0.10047(15) 0.3902(2) 0.16856(15) 0.0506(9) Uani 1 d . . . C21 C 0.1347(2) 0.3954(3) 0.1382(2) 0.0942(17) Uani 1 d . . . H21A H 0.1137 0.4210 0.1020 0.113 Uiso 1 d R . . H21B H 0.1647 0.4369 0.1577 0.113 Uiso 1 d R . . H21C H 0.1472 0.3323 0.1351 0.113 Uiso 1 d R . . C22 C 0.1314(2) 0.3493(3) 0.22523(19) 0.0944(16) Uani 1 d . . . H22A H 0.1098 0.3454 0.2450 0.113 Uiso 1 d R . . H22B H 0.1439 0.2862 0.2222 0.113 Uiso 1 d R . . H22C H 0.1614 0.3907 0.2448 0.113 Uiso 1 d R . . C23 C 0.05169(19) 0.3300(3) 0.1367(2) 0.0937(16) Uani 1 d . . . H23A H 0.0304 0.3264 0.1568 0.112 Uiso 1 d R . . H23B H 0.0310 0.3582 0.1011 0.112 Uiso 1 d R . . H23C H 0.0627 0.2665 0.1321 0.112 Uiso 1 d R . . C10 C 0.21157(13) 0.6474(3) 0.24305(15) 0.0539(9) Uani 1 d . . . C11 C 0.23709(16) 0.6316(4) 0.20426(18) 0.0800(14) Uani 1 d . . . H11A H 0.2126 0.6510 0.1677 0.096 Uiso 1 d R . . H11B H 0.2694 0.6686 0.2160 0.096 Uiso 1 d R . . H11C H 0.2452 0.5645 0.2042 0.096 Uiso 1 d R . . C12 C 0.19561(17) 0.7516(3) 0.2417(2) 0.0837(14) Uani 1 d . . . H12A H 0.1713 0.7692 0.2047 0.100 Uiso 1 d R . . H12B H 0.1784 0.7597 0.2657 0.100 Uiso 1 d R . . H12C H 0.2267 0.7920 0.2541 0.100 Uiso 1 d R . . C13 C 0.25006(15) 0.6185(4) 0.30098(17) 0.0891(16) Uani 1 d . . . H13A H 0.2598 0.5523 0.3006 0.107 Uiso 1 d R . . H13B H 0.2815 0.6580 0.3137 0.107 Uiso 1 d R . . H13C H 0.2332 0.6258 0.3253 0.107 Uiso 1 d R . . N1 N 0.04841(11) 0.91041(18) 0.21102(11) 0.0436(7) Uani 1 d . . . H1A H 0.0621 0.8532 0.2013 0.071(12) Uiso 1 d R . . H1B H 0.0599 0.9007 0.2496 0.050(10) Uiso 1 d R . . H1C H 0.0160 0.9029 0.1994 0.055(11) Uiso 1 d R . . C1 C 0.06586(16) 1.0025(3) 0.19449(17) 0.0593(10) Uani 1 d . . . C2 C 0.0466(2) 1.0828(3) 0.21913(19) 0.0821(14) Uani 1 d . . . H2A H 0.0638 1.0775 0.2587 0.098 Uiso 1 d R . . H2B H 0.0547 1.1444 0.2083 0.098 Uiso 1 d R . . H2C H 0.0086 1.0768 0.2063 0.098 Uiso 1 d R . . C3 C 0.0382(2) 1.0085(3) 0.13090(17) 0.0817(14) Uani 1 d . . . H3A H 0.0514 0.9577 0.1159 0.098 Uiso 1 d R . . H3B H 0.0002 1.0020 0.1175 0.098 Uiso 1 d R . . H3C H 0.0463 1.0696 0.1196 0.098 Uiso 1 d R . . C4 C 0.1246(2) 1.0006(4) 0.2175(3) 0.148(3) Uani 1 d . . . H4A H 0.1393 0.9969 0.2571 0.177 Uiso 1 d R . . H4B H 0.1357 0.9454 0.2037 0.177 Uiso 1 d R . . H4C H 0.1371 1.0581 0.2071 0.177 Uiso 1 d R . . S2 S 0.08018(3) 0.87055(6) 0.34015(3) 0.0466(2) Uani 1 d . . . Si2 Si 0.12611(3) 0.96117(6) 0.40372(3) 0.0318(2) Uani 1 d D . . O4 O 0.18893(9) 0.93047(19) 0.43724(11) 0.0408(7) Uani 0.818(4) d P A 1 O5 O 0.10563(11) 0.9692(2) 0.45135(10) 0.0446(8) Uani 0.818(4) d P A 1 O6 O 0.12072(12) 1.06904(16) 0.37756(11) 0.0434(8) Uani 0.818(4) d PD A 1 O4A O 0.18363(19) 0.9663(5) 0.4025(3) 0.022(3) Uiso 0.182(4) d PD A 2 O5A O 0.1401(3) 0.9361(7) 0.4674(2) 0.027(3) Uiso 0.182(4) d PD A 2 O6A O 0.0996(4) 1.0671(4) 0.3905(4) 0.030(3) Uiso 0.182(4) d PD A 2 C40 C 0.22945(11) 0.9015(2) 0.42242(13) 0.0449(8) Uani 1 d D . . C42 C 0.22336(17) 0.7935(3) 0.41395(18) 0.0772(13) Uani 1 d D . . H42A H 0.2269 0.7636 0.4476 0.093 Uiso 1 d R . . H42B H 0.1887 0.7792 0.3849 0.093 Uiso 1 d R . . H42C H 0.2504 0.7692 0.4041 0.093 Uiso 1 d R . . C41 C 0.2237(2) 0.9496(4) 0.3692(2) 0.0777(17) Uani 0.818(4) d P A 1 H41A H 0.2277 1.0179 0.3747 0.093 Uiso 0.818(4) d PR A 1 H41B H 0.2508 0.9256 0.3593 0.093 Uiso 0.818(4) d PR A 1 H41C H 0.1891 0.9356 0.3401 0.093 Uiso 0.818(4) d PR A 1 C43 C 0.28205(17) 0.9265(4) 0.4694(2) 0.0729(16) Uani 0.818(4) d P A 1 H43A H 0.2844 0.8951 0.5022 0.088 Uiso 0.818(4) d PR A 1 H43B H 0.3109 0.9053 0.4615 0.088 Uiso 0.818(4) d PR A 1 H43C H 0.2843 0.9949 0.4749 0.088 Uiso 0.818(4) d PR A 1 C41' C 0.2668(6) 0.9355(9) 0.3964(8) 0.094(9) Uiso 0.182(4) d PD A 2 H41D H 0.2743 1.0028 0.4038 0.113 Uiso 0.182(4) d PR A 2 H41E H 0.2995 0.8996 0.4126 0.113 Uiso 0.182(4) d PR A 2 H41F H 0.2500 0.9251 0.3571 0.113 Uiso 0.182(4) d PR A 2 C43' C 0.2609(6) 0.9216(10) 0.4862(3) 0.061(6) Uiso 0.182(4) d PD A 2 H43D H 0.2391 0.9018 0.5040 0.073 Uiso 0.182(4) d PR A 2 H43E H 0.2685 0.9891 0.4924 0.073 Uiso 0.182(4) d PR A 2 H43F H 0.2937 0.8859 0.5012 0.073 Uiso 0.182(4) d PR A 2 C50 C 0.11221(13) 0.9068(3) 0.49806(13) 0.0549(9) Uani 1 d D . . C51 C 0.1115(2) 0.8027(3) 0.4845(2) 0.0930(15) Uani 1 d D . . H51A H 0.0779 0.7875 0.4540 0.112 Uiso 1 d R . . H51B H 0.1400 0.7895 0.4743 0.112 Uiso 1 d R . . H51C H 0.1160 0.7643 0.5159 0.112 Uiso 1 d R . . C52 C 0.0663(2) 0.9295(5) 0.5105(3) 0.096(2) Uani 0.818(4) d P A 1 H52A H 0.0338 0.9093 0.4800 0.115 Uiso 0.818(4) d PR A 1 H52B H 0.0699 0.8973 0.5435 0.115 Uiso 0.818(4) d PR A 1 H52C H 0.0654 0.9978 0.5153 0.115 Uiso 0.818(4) d PR A 1 C53 C 0.1644(2) 0.9363(5) 0.5460(2) 0.103(2) Uani 0.818(4) d P A 1 H53A H 0.1940 0.9201 0.5382 0.123 Uiso 0.818(4) d PR A 1 H53B H 0.1637 1.0047 0.5509 0.123 Uiso 0.818(4) d PR A 1 H53C H 0.1682 0.9041 0.5791 0.123 Uiso 0.818(4) d PR A 1 C52' C 0.0564(4) 0.9499(10) 0.4772(7) 0.070(7) Uiso 0.182(4) d PD A 2 H52D H 0.0373 0.9374 0.4383 0.084 Uiso 0.182(4) d PR A 2 H52E H 0.0375 0.9217 0.4962 0.084 Uiso 0.182(4) d PR A 2 H52F H 0.0592 1.0182 0.4834 0.084 Uiso 0.182(4) d PR A 2 C53' C 0.1437(6) 0.9260(11) 0.5599(3) 0.073(8) Uiso 0.182(4) d PD A 2 H53D H 0.1787 0.8983 0.5733 0.088 Uiso 0.182(4) d PR A 2 H53E H 0.1467 0.9942 0.5663 0.088 Uiso 0.182(4) d PR A 2 H53F H 0.1250 0.8977 0.5791 0.088 Uiso 0.182(4) d PR A 2 C60 C 0.1357(2) 1.1636(3) 0.4026(2) 0.0540(13) Uani 0.818(4) d PD A 1 C61 C 0.1497(3) 1.2220(4) 0.3620(3) 0.092(2) Uani 0.818(4) d PD A 1 H61A H 0.1196 1.2249 0.3264 0.111 Uiso 0.818(4) d PR A 1 H61B H 0.1597 1.2861 0.3762 0.111 Uiso 0.818(4) d PR A 1 H61C H 0.1791 1.1916 0.3587 0.111 Uiso 0.818(4) d PR A 1 C62 C 0.1832(2) 1.1587(4) 0.4587(2) 0.103(3) Uani 0.818(4) d PD A 1 H62A H 0.1736 1.1222 0.4834 0.124 Uiso 0.818(4) d PR A 1 H62B H 0.2127 1.1281 0.4555 0.124 Uiso 0.818(4) d PR A 1 H62C H 0.1933 1.2226 0.4730 0.124 Uiso 0.818(4) d PR A 1 C63 C 0.0875(2) 1.2078(5) 0.4066(3) 0.082(2) Uani 0.818(4) d PD A 1 H63A H 0.0783 1.1710 0.4315 0.098 Uiso 0.818(4) d PR A 1 H63B H 0.0956 1.2728 0.4199 0.098 Uiso 0.818(4) d PR A 1 H63C H 0.0579 1.2079 0.3706 0.098 Uiso 0.818(4) d PR A 1 C60' C 0.1211(6) 1.1623(7) 0.4087(7) 0.060(11) Uiso 0.182(4) d PD A 2 C61' C 0.1526(9) 1.1953(16) 0.3765(9) 0.053(7) Uiso 0.182(4) d PD A 2 H61D H 0.1631 1.2614 0.3847 0.064 Uiso 0.182(4) d PR A 2 H61E H 0.1839 1.1558 0.3874 0.064 Uiso 0.182(4) d PR A 2 H61F H 0.1307 1.1882 0.3375 0.064 Uiso 0.182(4) d PR A 2 C62' C 0.0759(9) 1.2338(11) 0.3984(13) 0.13(2) Uiso 0.182(4) d PD A 2 H62D H 0.0558 1.2147 0.4181 0.161 Uiso 0.182(4) d PR A 2 H62E H 0.0908 1.2966 0.4104 0.161 Uiso 0.182(4) d PR A 2 H62F H 0.0529 1.2352 0.3594 0.161 Uiso 0.182(4) d PR A 2 C63' C 0.1592(8) 1.1609(16) 0.4705(6) 0.063(7) Uiso 0.182(4) d PD A 2 H63D H 0.1397 1.1415 0.4908 0.075 Uiso 0.182(4) d PR A 2 H63E H 0.1880 1.1167 0.4777 0.075 Uiso 0.182(4) d PR A 2 H63F H 0.1733 1.2245 0.4818 0.075 Uiso 0.182(4) d PR A 2 N2 N 0.06636(9) 0.64108(17) 0.32355(10) 0.0364(6) Uani 1 d . . . H2D H 0.0335 0.6417 0.3204 0.043 Uiso 1 d R . . H2E H 0.0793 0.6938 0.3424 0.049 Uiso 1 d R . . H2F H 0.0663 0.6420 0.2901 0.053 Uiso 1 d R . . C5 C 0.09186(12) 0.5488(2) 0.35155(12) 0.0378(7) Uani 1 d . . . C6 C 0.09015(15) 0.5460(3) 0.40706(14) 0.0611(10) Uani 1 d . . . H6A H 0.0538 0.5460 0.4022 0.073 Uiso 1 d R . . H6B H 0.1079 0.4892 0.4269 0.073 Uiso 1 d R . . H6C H 0.1082 0.6020 0.4277 0.073 Uiso 1 d R . . C7 C 0.14865(13) 0.5480(3) 0.35726(15) 0.0545(9) Uani 1 d . . . H7A H 0.1483 0.5488 0.3214 0.065 Uiso 1 d R . . H7B H 0.1669 0.6040 0.3776 0.065 Uiso 1 d R . . H7C H 0.1667 0.4912 0.3768 0.065 Uiso 1 d R . . C8 C 0.05925(14) 0.4683(2) 0.31415(16) 0.0575(10) Uani 1 d . . . H8A H 0.0235 0.4702 0.3109 0.069 Uiso 1 d R . . H8B H 0.0584 0.4762 0.2782 0.069 Uiso 1 d R . . H8C H 0.0753 0.4075 0.3294 0.069 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0385(4) 0.0347(4) 0.0447(5) -0.0021(3) 0.0244(4) 0.0014(3) Si1 0.0347(5) 0.0336(5) 0.0343(5) -0.0017(4) 0.0189(4) 0.0002(4) O1 0.0354(12) 0.0564(14) 0.0490(14) -0.0021(11) 0.0188(10) 0.0038(11) O2 0.0506(13) 0.0310(12) 0.0585(14) -0.0007(10) 0.0319(12) 0.0019(10) O3 0.0524(13) 0.0514(14) 0.0409(13) 0.0038(10) 0.0291(11) 0.0046(11) C30 0.074(3) 0.052(2) 0.046(2) 0.0085(17) 0.035(2) 0.0086(18) C31 0.130(4) 0.110(4) 0.059(3) 0.020(3) 0.066(3) 0.034(3) C32 0.074(3) 0.116(4) 0.046(2) 0.004(2) 0.015(2) -0.008(3) C33 0.126(4) 0.059(3) 0.080(3) 0.021(2) 0.043(3) 0.010(3) C20 0.066(2) 0.033(2) 0.063(2) 0.0005(16) 0.037(2) 0.0068(16) C21 0.146(4) 0.042(3) 0.151(5) -0.007(3) 0.118(4) 0.012(3) C22 0.135(4) 0.058(3) 0.087(3) 0.013(2) 0.045(3) 0.043(3) C23 0.099(4) 0.044(3) 0.128(4) -0.018(3) 0.040(3) -0.007(2) C10 0.0327(18) 0.072(3) 0.058(2) -0.0180(19) 0.0206(16) -0.0068(17) C11 0.059(2) 0.115(4) 0.082(3) -0.028(3) 0.045(2) -0.021(2) C12 0.054(2) 0.082(3) 0.112(4) -0.039(3) 0.033(3) -0.023(2) C13 0.041(2) 0.148(5) 0.067(3) -0.007(3) 0.012(2) -0.008(3) N1 0.0464(18) 0.0369(16) 0.0519(18) 0.0014(13) 0.0254(14) -0.0033(13) C1 0.069(3) 0.038(2) 0.082(3) 0.0020(19) 0.043(2) -0.0106(18) C2 0.136(4) 0.037(2) 0.082(3) -0.002(2) 0.055(3) -0.011(2) C3 0.120(4) 0.068(3) 0.077(3) 0.010(2) 0.062(3) -0.001(3) C4 0.076(4) 0.107(5) 0.264(9) 0.057(5) 0.076(5) -0.015(3) S2 0.0482(5) 0.0328(5) 0.0379(4) -0.0019(4) -0.0008(4) 0.0015(4) Si2 0.0323(4) 0.0308(5) 0.0281(4) -0.0001(3) 0.0092(3) 0.0030(3) O4 0.0322(14) 0.0487(17) 0.0379(16) -0.0013(13) 0.0118(12) 0.0012(12) O5 0.0491(18) 0.0537(18) 0.0322(15) -0.0020(12) 0.0189(13) 0.0098(14) O6 0.0523(18) 0.0280(15) 0.0405(16) -0.0011(11) 0.0114(14) -0.0012(12) C40 0.0308(17) 0.052(2) 0.048(2) 0.0106(16) 0.0139(15) 0.0049(15) C42 0.073(3) 0.064(3) 0.078(3) 0.002(2) 0.018(2) 0.010(2) C41 0.065(3) 0.108(4) 0.079(4) 0.038(3) 0.049(3) 0.022(3) C43 0.035(3) 0.093(4) 0.077(4) 0.001(3) 0.012(3) -0.003(3) C50 0.054(2) 0.077(3) 0.0358(19) 0.0075(18) 0.0219(17) 0.0154(19) C51 0.127(4) 0.076(3) 0.086(3) 0.023(3) 0.056(3) 0.026(3) C52 0.095(4) 0.139(6) 0.081(4) 0.027(4) 0.064(4) 0.037(4) C53 0.083(4) 0.155(7) 0.044(3) 0.017(4) 0.003(3) 0.011(4) C60 0.064(3) 0.025(3) 0.059(3) -0.010(2) 0.014(3) -0.002(2) C61 0.130(6) 0.043(4) 0.116(6) 0.003(4) 0.064(5) -0.015(4) C62 0.104(5) 0.049(4) 0.092(5) -0.024(3) -0.018(4) -0.017(3) C63 0.096(5) 0.055(3) 0.098(5) -0.036(3) 0.045(4) -0.007(3) N2 0.0385(14) 0.0342(14) 0.0374(14) -0.0020(11) 0.0173(12) 0.0020(11) C5 0.0380(17) 0.0347(18) 0.0361(17) 0.0057(13) 0.0118(14) 0.0045(13) C6 0.062(2) 0.073(3) 0.048(2) 0.0182(19) 0.0233(19) 0.013(2) C7 0.0413(19) 0.061(2) 0.058(2) 0.0070(18) 0.0181(17) 0.0115(17) C8 0.062(2) 0.036(2) 0.061(2) 0.0011(17) 0.0140(19) 0.0006(17) _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 S1 Si1 2.0617(11) . ? Si1 O3 1.622(2) . ? Si1 O2 1.627(2) . ? Si1 O1 1.638(2) . ? O1 C10 1.442(4) . ? O2 C20 1.442(4) . ? O3 C30 1.440(4) . ? C30 C33 1.499(5) . ? C30 C32 1.505(5) . ? C30 C31 1.506(5) . ? C31 H31A 0.9604 . ? C31 H31B 0.9599 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9601 . ? C32 H32C 0.9601 . ? C33 H33A 0.9602 . ? C33 H33B 0.9605 . ? C33 H33C 0.9598 . ? C20 C22 1.497(5) . ? C20 C21 1.499(5) . ? C20 C23 1.503(5) . ? C21 H21A 0.9601 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9597 . ? C22 H22B 0.9602 . ? C22 H22C 0.9600 . ? C23 H23A 0.9599 . ? C23 H23B 0.9603 . ? C23 H23C 0.9601 . ? C10 C11 1.509(5) . ? C10 C13 1.510(5) . ? C10 C12 1.511(6) . ? C11 H11A 0.9599 . ? C11 H11B 0.9602 . ? C11 H11C 0.9599 . ? C12 H12A 0.9601 . ? C12 H12B 0.9602 . ? C12 H12C 0.9596 . ? C13 H13A 0.9601 . ? C13 H13B 0.9599 . ? C13 H13C 0.9601 . ? N1 C1 1.501(4) . ? N1 H1A 0.9656 . ? N1 H1B 0.9523 . ? N1 H1C 0.8227 . ? C1 C4 1.473(6) . ? C1 C2 1.510(5) . ? C1 C3 1.541(6) . ? C2 H2A 0.9598 . ? C2 H2B 0.9601 . ? C2 H2C 0.9599 . ? C3 H3A 0.9599 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9602 . ? C4 H4B 0.9600 . ? C4 H4C 0.9599 . ? S2 Si2 2.0580(12) . ? Si2 O4A 1.614(4) . ? Si2 O5 1.614(3) . ? Si2 O6A 1.614(4) . ? Si2 O5A 1.620(4) . ? Si2 O6 1.634(3) . ? Si2 O4 1.635(3) . ? O4 C40 1.406(4) . ? O5 C50 1.469(4) . ? O6 C60 1.451(3) . ? O4A C40 1.458(4) . ? O5A C50 1.413(4) . ? O6A C60' 1.446(5) . ? C40 C43 1.499(5) . ? C40 C42 1.516(5) . ? C40 C41 1.522(5) . ? C40 C41' 1.555(7) . ? C40 C43' 1.574(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9599 . ? C42 H42C 0.9601 . ? C41 H41A 0.9600 . ? C41 H41B 0.9599 . ? C41 H41C 0.9600 . ? C43 H43A 0.9601 . ? C43 H43B 0.9600 . ? C43 H43C 0.9599 . ? C41' H41D 0.9600 . ? C41' H41E 0.9600 . ? C41' H41F 0.9600 . ? C43' H43D 0.9601 . ? C43' H43E 0.9601 . ? C43' H43F 0.9598 . ? C50 C52 1.485(6) . ? C50 C51 1.490(6) . ? C50 C53 1.519(6) . ? C50 C52' 1.524(7) . ? C50 C53' 1.528(7) . ? C51 H51A 0.9601 . ? C51 H51B 0.9602 . ? C51 H51C 0.9598 . ? C52 H52A 0.9599 . ? C52 H52B 0.9601 . ? C52 H52C 0.9600 . ? C53 H53A 0.9599 . ? C53 H53B 0.9601 . ? C53 H53C 0.9601 . ? C52' H52D 0.9600 . ? C52' H52E 0.9599 . ? C52' H52F 0.9600 . ? C53' H53D 0.9600 . ? C53' H53E 0.9601 . ? C53' H53F 0.9601 . ? C60 C62 1.515(5) . ? C60 C63 1.519(6) . ? C60 C61 1.537(6) . ? C61 H61A 0.9601 . ? C61 H61B 0.9599 . ? C61 H61C 0.9599 . ? C62 H62A 0.9601 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9601 . ? C63 H63C 0.9601 . ? C60' C62' 1.528(9) . ? C60' C63' 1.533(9) . ? C60' C61' 1.543(9) . ? C61' H61D 0.9601 . ? C61' H61E 0.9603 . ? C61' H61F 0.9600 . ? C62' H62D 0.9600 . ? C62' H62E 0.9602 . ? C62' H62F 0.9599 . ? C63' H63D 0.9602 . ? C63' H63E 0.9598 . ? C63' H63F 0.9601 . ? N2 C5 1.499(4) . ? N2 H2D 0.8798 . ? N2 H2E 0.8741 . ? N2 H2F 0.8972 . ? C5 C6 1.513(4) . ? C5 C8 1.513(4) . ? C5 C7 1.517(4) . ? C6 H6A 0.9601 . ? C6 H6B 0.9599 . ? C6 H6C 0.9602 . ? C7 H7A 0.9600 . ? C7 H7B 0.9601 . ? C7 H7C 0.9599 . ? C8 H8A 0.9597 . ? C8 H8B 0.9605 . ? C8 H8C 0.9600 . ? 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 O3 Si1 O2 111.44(12) . . ? O3 Si1 O1 103.81(12) . . ? O2 Si1 O1 105.02(12) . . ? O3 Si1 S1 115.04(9) . . ? O2 Si1 S1 107.15(8) . . ? O1 Si1 S1 114.00(9) . . ? C10 O1 Si1 131.6(2) . . ? C20 O2 Si1 132.9(2) . . ? C30 O3 Si1 136.0(2) . . ? O3 C30 C33 107.5(3) . . ? O3 C30 C32 111.0(3) . . ? C33 C30 C32 110.4(4) . . ? O3 C30 C31 105.8(3) . . ? C33 C30 C31 111.7(4) . . ? C32 C30 C31 110.3(4) . . ? C30 C31 H31A 108.1 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 110.5 . . ? H31A C31 H31C 109.4 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 110.4 . . ? C30 C32 H32B 109.2 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 108.8 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 110.1 . . ? C30 C33 H33B 108.9 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C20 C22 107.9(3) . . ? O2 C20 C21 112.1(3) . . ? C22 C20 C21 110.6(4) . . ? O2 C20 C23 105.7(3) . . ? C22 C20 C23 110.2(4) . . ? C21 C20 C23 110.2(4) . . ? C20 C21 H21A 108.5 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 110.1 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 111.3 . . ? C20 C22 H22B 109.2 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 107.9 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.4 . . ? C20 C23 H23B 110.0 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 108.9 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.4 . . ? O1 C10 C11 109.7(3) . . ? O1 C10 C13 105.4(3) . . ? C11 C10 C13 109.8(3) . . ? O1 C10 C12 111.4(3) . . ? C11 C10 C12 110.1(4) . . ? C13 C10 C12 110.4(4) . . ? C10 C11 H11A 109.2 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 108.9 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.6 . . ? C10 C12 H12B 108.8 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.9 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 108.7 . . ? C10 C13 H13B 110.1 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.7 . . ? H13A C13 H13C 109.4 . . ? H13B C13 H13C 109.5 . . ? C1 N1 H1A 113.9 . . ? C1 N1 H1B 116.4 . . ? H1A N1 H1B 101.1 . . ? C1 N1 H1C 115.9 . . ? H1A N1 H1C 106.8 . . ? H1B N1 H1C 100.8 . . ? C4 C1 N1 107.6(3) . . ? C4 C1 C2 111.6(4) . . ? N1 C1 C2 106.2(3) . . ? C4 C1 C3 113.2(4) . . ? N1 C1 C3 107.7(3) . . ? C2 C1 C3 110.2(4) . . ? C1 C2 H2A 109.1 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 108.7 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.1 . . ? C1 C3 H3B 110.3 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.0 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.0 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.8 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O4A Si2 O5 134.9(3) . . ? O4A Si2 O6A 108.5(4) . . ? O5 Si2 O6A 80.0(4) . . ? O4A Si2 O5A 104.2(3) . . ? O6A Si2 O5A 107.8(4) . . ? O4A Si2 O6 81.8(2) . . ? O5 Si2 O6 106.20(15) . . ? O5A Si2 O6 125.9(3) . . ? O5 Si2 O4 103.96(14) . . ? O6A Si2 O4 129.4(4) . . ? O5A Si2 O4 69.7(3) . . ? O6 Si2 O4 110.64(14) . . ? O4A Si2 S2 105.9(3) . . ? O5 Si2 S2 113.26(11) . . ? O6A Si2 S2 108.4(4) . . ? O5A Si2 S2 121.5(3) . . ? O6 Si2 S2 107.23(10) . . ? O4 Si2 S2 115.24(10) . . ? C40 O4 Si2 135.5(2) . . ? C50 O5 Si2 132.8(2) . . ? C60 O6 Si2 132.6(3) . . ? C40 O4A Si2 132.9(5) . . ? C50 O5A Si2 137.4(5) . . ? C60' O6A Si2 132.6(8) . . ? O4 C40 C43 107.7(3) . . ? O4A C40 C43 122.8(5) . . ? O4 C40 C42 106.0(3) . . ? O4A C40 C42 122.2(4) . . ? C43 C40 C42 111.1(3) . . ? O4 C40 C41 111.7(3) . . ? O4A C40 C41 70.5(3) . . ? C43 C40 C41 110.8(4) . . ? C42 C40 C41 109.5(4) . . ? O4 C40 C41' 144.3(5) . . ? O4A C40 C41' 107.1(6) . . ? C43 C40 C41' 73.2(7) . . ? C42 C40 C41' 106.6(5) . . ? O4 C40 C43' 77.0(6) . . ? O4A C40 C43' 105.8(5) . . ? C42 C40 C43' 108.2(5) . . ? C41 C40 C43' 136.6(7) . . ? C41' C40 C43' 105.8(6) . . ? C40 C42 H42A 109.1 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.8 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.6 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41D 86.9 . . ? C40 C41 H41F 111.7 . . ? H41D C41 H41F 75.1 . . ? C40 C43 H43A 108.7 . . ? C40 C43 H43B 110.2 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C43 H43E 101.0 . . ? C40 C43 H43F 116.4 . . ? H43E C43 H43F 91.5 . . ? C40 C41' H41A 84.0 . . ? C40 C41' H41B 110.1 . . ? H41A C41' H41B 76.4 . . ? C40 C41' H41D 109.2 . . ? C40 C41' H41E 108.8 . . ? C40 C41' H41F 110.4 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C40 C43' H43A 119.7 . . ? C40 C43' H43C 89.0 . . ? H43A C43' H43C 97.1 . . ? C40 C43' H43D 108.6 . . ? C40 C43' H43E 109.8 . . ? H43D C43' H43E 109.5 . . ? C40 C43' H43F 110.0 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? O5A C50 C52 144.2(5) . . ? O5 C50 C52 105.4(3) . . ? O5A C50 C51 95.1(5) . . ? O5 C50 C51 112.4(3) . . ? C52 C50 C51 109.8(4) . . ? O5A C50 C53 81.5(4) . . ? O5 C50 C53 106.5(4) . . ? C52 C50 C53 110.5(4) . . ? C51 C50 C53 112.1(4) . . ? O5A C50 C52' 113.6(6) . . ? O5 C50 C52' 74.0(7) . . ? C51 C50 C52' 112.8(6) . . ? C53 C50 C52' 130.6(7) . . ? O5A C50 C53' 112.5(6) . . ? O5 C50 C53' 128.8(7) . . ? C52 C50 C53' 82.0(7) . . ? C51 C50 C53' 112.1(6) . . ? C52' C50 C53' 110.0(6) . . ? C50 C51 H51A 109.1 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 110.0 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.2 . . ? C50 C52 H52B 110.8 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 108.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C52 H52E 134.6 . . ? C50 C52 H52F 90.6 . . ? H52E C52 H52F 89.0 . . ? C50 C53 H53A 110.2 . . ? C50 C53 H53B 108.3 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.9 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C53 H53D 118.8 . . ? C50 C53 H53E 97.9 . . ? H53D C53 H53E 99.0 . . ? C50 C52' H52A 111.7 . . ? C50 C52' H52C 96.1 . . ? H52A C52' H52C 100.5 . . ? C50 C52' H52D 108.8 . . ? C50 C52' H52E 110.3 . . ? H52D C52' H52E 109.5 . . ? C50 C52' H52F 109.3 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? C50 C53' H53B 91.9 . . ? C50 C53' H53C 128.5 . . ? H53B C53' H53C 98.1 . . ? C50 C53' H53D 110.2 . . ? C50 C53' H53E 109.3 . . ? H53D C53' H53E 109.5 . . ? C50 C53' H53F 108.9 . . ? H53D C53' H53F 109.5 . . ? H53E C53' H53F 109.5 . . ? O6 C60 C62 111.7(3) . . ? O6 C60 C63 108.4(4) . . ? C62 C60 C63 111.1(5) . . ? O6 C60 C61 105.1(4) . . ? C62 C60 C61 110.5(5) . . ? C63 C60 C61 109.8(4) . . ? O6 C60 H61E 85.5 . . ? C62 C60 H61E 77.4 . . ? C63 C60 H61E 158.1 . . ? C60 C61 H61A 110.5 . . ? C60 C61 H61B 109.2 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 108.7 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C61 H61D 90.0 . . ? C60 C61 H61E 66.6 . . ? H61D C61 H61E 95.6 . . ? C60 C61 H61F 89.7 . . ? H61D C61 H61F 168.4 . . ? H61E C61 H61F 94.9 . . ? C60 C62 H62A 109.1 . . ? C60 C62 H62B 109.9 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.4 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C62 H63E 122.4 . . ? C60 C62 H63F 100.6 . . ? H63E C62 H63F 104.8 . . ? C60 C63 H63A 110.1 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 108.8 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C63 H62D 158.4 . . ? C60 C63 H62E 111.9 . . ? H62D C63 H62E 85.8 . . ? C60 C63 H62F 111.0 . . ? H62D C63 H62F 84.1 . . ? H62E C63 H62F 77.3 . . ? O6A C60' C62' 110.3(8) . . ? O6A C60' C63' 110.1(8) . . ? C62' C60' C63' 109.4(8) . . ? O6A C60' C61' 109.5(8) . . ? C62' C60' C61' 109.0(8) . . ? C63' C60' C61' 108.6(8) . . ? O6A C60' H63A 86.0 . . ? C61' C60' H63A 155.6 . . ? C60' C61' H61A 110.7 . . ? C60' C61' H61B 115.0 . . ? H61A C61' H61B 74.2 . . ? C60' C61' H61C 158.5 . . ? H61A C61' H61C 82.2 . . ? H61B C61' H61C 84.5 . . ? C60' C61' H61D 110.1 . . ? C60' C61' H61E 108.5 . . ? H61D C61' H61E 109.4 . . ? C60' C61' H61F 109.8 . . ? H61D C61' H61F 109.5 . . ? H61E C61' H61F 109.5 . . ? C60' C62' H63A 68.0 . . ? C60' C62' H63B 93.3 . . ? H63A C62' H63B 98.6 . . ? C60' C62' H63C 90.6 . . ? H63A C62' H63C 100.2 . . ? H63B C62' H63C 160.9 . . ? C60' C62' H62D 110.5 . . ? C60' C62' H62E 109.3 . . ? H62D C62' H62E 109.5 . . ? C60' C62' H62F 108.6 . . ? H62D C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? C60' C63' H62A 123.1 . . ? C60' C63' H62C 101.5 . . ? H62A C63' H62C 104.7 . . ? C60' C63' H63D 108.9 . . ? C60' C63' H63E 110.5 . . ? C60' C63' H63F 109.0 . . ? H63E C63' H63F 109.5 . . ? C5 N2 H2D 107.5 . . ? C5 N2 H2E 116.1 . . ? H2D N2 H2E 101.3 . . ? C5 N2 H2F 108.0 . . ? H2D N2 H2F 110.7 . . ? H2E N2 H2F 113.0 . . ? N2 C5 C6 107.8(3) . . ? N2 C5 C8 106.4(2) . . ? C6 C5 C8 111.7(3) . . ? N2 C5 C7 107.5(3) . . ? C6 C5 C7 112.1(3) . . ? C8 C5 C7 111.0(3) . . ? C5 C6 H6A 110.3 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 108.4 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 110.0 . . ? C5 C7 H7B 108.8 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.6 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.8 . . ? C5 C8 H8B 109.2 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A S1 0.97 2.39 3.212(3) 142.8 . N1 H1B S2 0.95 2.28 3.233(3) 174.9 . N1 H1C S2 0.82 2.45 3.271(3) 175.4 2 N2 H2F S1 0.90 2.39 3.271(3) 166.2 . N2 H2E S2 0.87 2.46 3.219(3) 146.0 . N2 H2D S1 0.88 2.38 3.242(3) 165.3 2 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.654 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.052 data_3 _database_code_depnum_ccdc_archive 'CCDC 215789' _chemical_name_common '3-methyl-n-butylammonium tri-tert-butoxysilanethiolate' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-methyl-n-butylammonium tri-tert-butoxysilanethiolate ; _chemical_formula_moiety '4(C12 H27 O3 S Si), C7 H8, 4(C5 H14 N)' _chemical_formula_sum 'C75 H172 N4 O12 S4 Si4' _chemical_formula_weight 1562.77 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 21.709(4) _cell_length_b 15.326(3) _cell_length_c 30.588(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.96(3) _cell_angle_gamma 90.00 _cell_volume 10171(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200.0(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200.0(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 'KM4 Oxford Diffraction' _diffrn_measurement_method '\w--2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.67 _diffrn_reflns_number 21140 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.8906 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21140 _reflns_number_gt 9864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 System (Ga\/ldecki, 1996)' _computing_cell_refinement 'KM4 System (Ga\/ldecki, 1996)' _computing_data_reduction 'DATAPROC (Ga\/ldecki, 1996)' _computing_structure_solution 'SHELXS - 97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL - 97 (Sheldrick, 1997)' _computing_molecular_graphics 'RESVIEW, (Schwenk, 1998)' _computing_publication_material 'SHELXL - 97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1247P)^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 21140 _refine_ls_number_parameters 943 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.74079(4) 0.11273(6) 0.63093(3) 0.0490(3) Uani 1 d . . . Si1 Si 0.79819(4) 0.01424(6) 0.65081(3) 0.0408(3) Uani 1 d . . . S2 S 0.85076(4) 0.36842(6) 0.66138(3) 0.0456(3) Uani 1 d . . . Si2 Si 0.91087(4) 0.45879(6) 0.63902(3) 0.0424(3) Uani 1 d . . . S3 S 0.65457(4) 0.39079(6) 0.65337(3) 0.0511(3) Uani 1 d . . . Si3 Si 0.59452(4) 0.37671(7) 0.70309(3) 0.0420(3) Uani 1 d . . . Si4 Si 0.69827(5) 0.30275(7) 0.47597(3) 0.0479(3) Uani 1 d . . . S4 S 0.75812(4) 0.27802(7) 0.52722(3) 0.0515(3) Uani 1 d . . . O1 O 0.79264(11) -0.07404(15) 0.62166(8) 0.0492(7) Uani 1 d . . . C10 C 0.78827(19) -0.0905(2) 0.57538(14) 0.0544(11) Uani 1 d . . . C11 C 0.7214(2) -0.0806(3) 0.55982(16) 0.0733(13) Uani 1 d . . . H11A H 0.6958 -0.1215 0.5758 0.110 Uiso 1 calc R . . H11B H 0.7177 -0.0931 0.5284 0.110 Uiso 1 calc R . . H11C H 0.7077 -0.0207 0.5652 0.110 Uiso 1 calc R . . C12 C 0.8097(2) -0.1826(3) 0.56944(16) 0.0711(13) Uani 1 d . . . H12A H 0.8535 -0.1870 0.5781 0.107 Uiso 1 calc R . . H12B H 0.8039 -0.1994 0.5387 0.107 Uiso 1 calc R . . H12C H 0.7858 -0.2217 0.5877 0.107 Uiso 1 calc R . . C13 C 0.8294(2) -0.0284(3) 0.55073(15) 0.0722(13) Uani 1 d . . . H13A H 0.8150 0.0317 0.5546 0.108 Uiso 1 calc R . . H13B H 0.8276 -0.0432 0.5195 0.108 Uiso 1 calc R . . H13C H 0.8719 -0.0336 0.5622 0.108 Uiso 1 calc R . . O2 O 0.86922(10) 0.05165(14) 0.64919(8) 0.0448(6) Uani 1 d . . . C20 C 0.92589(16) 0.0188(3) 0.66990(14) 0.0553(11) Uani 1 d . . . C21 C 0.9293(2) 0.0517(4) 0.71640(17) 0.0926(17) Uani 1 d . . . H21A H 0.9669 0.0295 0.7312 0.139 Uiso 1 calc R . . H21B H 0.8932 0.0314 0.7318 0.139 Uiso 1 calc R . . H21C H 0.9301 0.1157 0.7163 0.139 Uiso 1 calc R . . C22 C 0.97724(18) 0.0553(4) 0.64400(19) 0.0904(17) Uani 1 d . . . H22A H 0.9723 0.0361 0.6135 0.136 Uiso 1 calc R . . H22B H 1.0168 0.0344 0.6563 0.136 Uiso 1 calc R . . H22C H 0.9762 0.1191 0.6452 0.136 Uiso 1 calc R . . C23 C 0.9278(2) -0.0799(3) 0.66812(19) 0.0868(16) Uani 1 d . . . H23A H 0.9252 -0.0991 0.6376 0.130 Uiso 1 calc R . . H23B H 0.8930 -0.1039 0.6838 0.130 Uiso 1 calc R . . H23C H 0.9666 -0.1007 0.6819 0.130 Uiso 1 calc R . . O3 O 0.79083(11) -0.01884(16) 0.70094(8) 0.0518(7) Uani 1 d . . . C30 C 0.74660(19) -0.0735(3) 0.72126(15) 0.0585(11) Uani 1 d . . . C31 C 0.7443(3) -0.0447(4) 0.76733(18) 0.1010(18) Uani 1 d . . . H31A H 0.7858 -0.0470 0.7809 0.151 Uiso 1 calc R . . H31B H 0.7169 -0.0832 0.7832 0.151 Uiso 1 calc R . . H31C H 0.7288 0.0153 0.7684 0.151 Uiso 1 calc R . . C32 C 0.6834(2) -0.0643(5) 0.69894(19) 0.114(2) Uani 1 d . . . H32A H 0.6535 -0.0997 0.7145 0.171 Uiso 1 calc R . . H32B H 0.6851 -0.0843 0.6686 0.171 Uiso 1 calc R . . H32C H 0.6707 -0.0029 0.6994 0.171 Uiso 1 calc R . . C33 C 0.7686(3) -0.1652(3) 0.7175(3) 0.132(3) Uani 1 d . . . H33A H 0.8079 -0.1718 0.7338 0.198 Uiso 1 calc R . . H33B H 0.7742 -0.1794 0.6867 0.198 Uiso 1 calc R . . H33C H 0.7381 -0.2048 0.7296 0.198 Uiso 1 calc R . . O4 O 0.88028(10) 0.49912(16) 0.59288(8) 0.0488(7) Uani 1 d . . . C40 C 0.90810(18) 0.5419(3) 0.55537(15) 0.0617(12) Uani 1 d . . . C41 C 0.9285(2) 0.4714(3) 0.52450(16) 0.0838(15) Uani 1 d . . . H41A H 0.9436 0.4983 0.4978 0.126 Uiso 1 calc R . . H41B H 0.8935 0.4332 0.5170 0.126 Uiso 1 calc R . . H41C H 0.9616 0.4371 0.5387 0.126 Uiso 1 calc R . . C42 C 0.8566(2) 0.5950(3) 0.53431(16) 0.0782(14) Uani 1 d . . . H42A H 0.8417 0.6376 0.5554 0.117 Uiso 1 calc R . . H42B H 0.8227 0.5562 0.5251 0.117 Uiso 1 calc R . . H42C H 0.8718 0.6257 0.5088 0.117 Uiso 1 calc R . . C43 C 0.9597(2) 0.5998(4) 0.57083(19) 0.1011(19) Uani 1 d . . . H43A H 0.9442 0.6424 0.5917 0.152 Uiso 1 calc R . . H43B H 0.9764 0.6306 0.5458 0.152 Uiso 1 calc R . . H43C H 0.9921 0.5645 0.5851 0.152 Uiso 1 calc R . . O5 O 0.97757(10) 0.42140(16) 0.62580(9) 0.0517(7) Uani 1 d . . . C50 C 1.03238(19) 0.4003(3) 0.65097(17) 0.0707(13) Uani 1 d . . . C51 C 1.0167(2) 0.3572(4) 0.6939(2) 0.117(2) Uani 1 d . . . H51A H 0.9900 0.3960 0.7103 0.176 Uiso 1 calc R . . H51B H 1.0548 0.3460 0.7112 0.176 Uiso 1 calc R . . H51C H 0.9953 0.3020 0.6880 0.176 Uiso 1 calc R . . C52 C 1.0671(2) 0.4850(4) 0.6611(2) 0.0943(17) Uani 1 d . . . H52A H 1.0759 0.5150 0.6338 0.141 Uiso 1 calc R . . H52B H 1.1059 0.4717 0.6770 0.141 Uiso 1 calc R . . H52C H 1.0418 0.5227 0.6792 0.141 Uiso 1 calc R . . C53 C 1.0704(2) 0.3443(5) 0.6212(3) 0.133(3) Uani 1 d . . . H53A H 1.0496 0.2883 0.6161 0.199 Uiso 1 calc R . . H53B H 1.1112 0.3341 0.6350 0.199 Uiso 1 calc R . . H53C H 1.0750 0.3744 0.5932 0.199 Uiso 1 calc R . . O6 O 0.92618(11) 0.53865(15) 0.67263(9) 0.0516(7) Uani 1 d . . . C60 C 0.88815(19) 0.5927(3) 0.69829(16) 0.0633(12) Uani 1 d . . . C61 C 0.8785(2) 0.5460(4) 0.74142(17) 0.0849(16) Uani 1 d . . . H61A H 0.8541 0.5830 0.7604 0.127 Uiso 1 calc R . . H61B H 0.9186 0.5339 0.7558 0.127 Uiso 1 calc R . . H61C H 0.8567 0.4909 0.7358 0.127 Uiso 1 calc R . . C62 C 0.9244(3) 0.6761(3) 0.7065(2) 0.1007(19) Uani 1 d . . . H62A H 0.9287 0.7075 0.6789 0.151 Uiso 1 calc R . . H62B H 0.9654 0.6617 0.7190 0.151 Uiso 1 calc R . . H62C H 0.9026 0.7130 0.7271 0.151 Uiso 1 calc R . . C63 C 0.8267(2) 0.6113(3) 0.67587(18) 0.0843(16) Uani 1 d . . . H63A H 0.8054 0.5562 0.6694 0.126 Uiso 1 calc R . . H63B H 0.8331 0.6429 0.6485 0.126 Uiso 1 calc R . . H63C H 0.8017 0.6470 0.6951 0.126 Uiso 1 calc R . . O7 O 0.58974(11) 0.46003(17) 0.73587(8) 0.0533(7) Uani 1 d . . . C70 C 0.63426(19) 0.5169(3) 0.75661(14) 0.0606(11) Uani 1 d . . . C71 C 0.69441(19) 0.4702(3) 0.76632(16) 0.0737(13) Uani 1 d . . . H71A H 0.6868 0.4179 0.7838 0.111 Uiso 1 calc R . . H71B H 0.7226 0.5091 0.7827 0.111 Uiso 1 calc R . . H71C H 0.7129 0.4532 0.7388 0.111 Uiso 1 calc R . . C72 C 0.6433(2) 0.5933(3) 0.72701(18) 0.0843(15) Uani 1 d . . . H72A H 0.6716 0.6350 0.7413 0.126 Uiso 1 calc R . . H72B H 0.6035 0.6216 0.7207 0.126 Uiso 1 calc R . . H72C H 0.6606 0.5732 0.6996 0.126 Uiso 1 calc R . . C73 C 0.6048(2) 0.5446(3) 0.79913(16) 0.0844(15) Uani 1 d . . . H73A H 0.6330 0.5835 0.8155 0.127 Uiso 1 calc R . . H73B H 0.5965 0.4928 0.8168 0.127 Uiso 1 calc R . . H73C H 0.5660 0.5753 0.7923 0.127 Uiso 1 calc R . . O8 O 0.61644(10) 0.29021(16) 0.73141(8) 0.0495(7) Uani 1 d . . . C80 C 0.58209(18) 0.2356(3) 0.76113(14) 0.0614(12) Uani 1 d . . . C81 C 0.6304(2) 0.1911(4) 0.78969(18) 0.0913(17) Uani 1 d . . . H81A H 0.6563 0.1546 0.7716 0.137 Uiso 1 calc R . . H81B H 0.6103 0.1546 0.8113 0.137 Uiso 1 calc R . . H81C H 0.6559 0.2352 0.8048 0.137 Uiso 1 calc R . . C82 C 0.5454(2) 0.1717(4) 0.73459(17) 0.0975(19) Uani 1 d . . . H82A H 0.5148 0.2028 0.7162 0.146 Uiso 1 calc R . . H82B H 0.5243 0.1316 0.7541 0.146 Uiso 1 calc R . . H82C H 0.5728 0.1385 0.7160 0.146 Uiso 1 calc R . . C83 C 0.5420(3) 0.2913(4) 0.78971(18) 0.0988(18) Uani 1 d . . . H83A H 0.5677 0.3345 0.8054 0.148 Uiso 1 calc R . . H83B H 0.5216 0.2541 0.8109 0.148 Uiso 1 calc R . . H83C H 0.5108 0.3214 0.7713 0.148 Uiso 1 calc R . . O9 O 0.52385(10) 0.35654(18) 0.68691(9) 0.0555(7) Uani 1 d . . . C90 C 0.47666(18) 0.4097(3) 0.66665(14) 0.0634(12) Uani 1 d . . . C91 C 0.4301(3) 0.4233(6) 0.7009(3) 0.175(4) Uani 1 d . . . H91A H 0.4010 0.4689 0.6914 0.263 Uiso 1 calc R . . H91B H 0.4511 0.4410 0.7284 0.263 Uiso 1 calc R . . H91C H 0.4076 0.3687 0.7055 0.263 Uiso 1 calc R . . C92 C 0.4540(4) 0.3594(5) 0.6288(3) 0.205(5) Uani 1 d . . . H92A H 0.4885 0.3452 0.6102 0.307 Uiso 1 calc R . . H92B H 0.4234 0.3939 0.6120 0.307 Uiso 1 calc R . . H92C H 0.4349 0.3054 0.6388 0.307 Uiso 1 calc R . . C93 C 0.4994(3) 0.4968(4) 0.6515(2) 0.117(2) Uani 1 d . . . H93A H 0.5324 0.4882 0.6309 0.175 Uiso 1 calc R . . H93B H 0.5154 0.5302 0.6768 0.175 Uiso 1 calc R . . H93C H 0.4654 0.5289 0.6371 0.175 Uiso 1 calc R . . O10 O 0.70617(13) 0.39591(18) 0.45145(9) 0.0634(8) Uani 1 d . . . C100 C 0.7487(2) 0.4265(3) 0.41944(14) 0.0760(14) Uani 1 d . . . C101 C 0.7232(3) 0.3987(4) 0.37451(15) 0.1026(19) Uani 1 d . . . H10A H 0.7491 0.4228 0.3518 0.154 Uiso 1 calc R . . H10B H 0.6810 0.4207 0.3703 0.154 Uiso 1 calc R . . H10C H 0.7230 0.3349 0.3726 0.154 Uiso 1 calc R . . C102 C 0.8115(3) 0.3889(4) 0.42771(18) 0.109(2) Uani 1 d . . . H10D H 0.8401 0.4144 0.4072 0.163 Uiso 1 calc R . . H10E H 0.8099 0.3255 0.4236 0.163 Uiso 1 calc R . . H10F H 0.8256 0.4021 0.4578 0.163 Uiso 1 calc R . . C103 C 0.7485(3) 0.5245(4) 0.4232(2) 0.124(2) Uani 1 d . . . H10G H 0.7659 0.5416 0.4519 0.185 Uiso 1 calc R . . H10H H 0.7062 0.5462 0.4199 0.185 Uiso 1 calc R . . H10I H 0.7735 0.5496 0.4002 0.185 Uiso 1 calc R . . O11 O 0.69866(12) 0.23096(18) 0.43643(8) 0.0577(7) Uani 1 d . . . C110 C 0.7033(2) 0.1377(3) 0.43612(14) 0.0644(12) Uani 1 d . . . C111 C 0.7700(2) 0.1132(4) 0.44262(18) 0.0953(17) Uani 1 d . . . H11D H 0.7945 0.1445 0.4214 0.143 Uiso 1 calc R . . H11E H 0.7747 0.0502 0.4384 0.143 Uiso 1 calc R . . H11F H 0.7842 0.1290 0.4723 0.143 Uiso 1 calc R . . C112 C 0.6801(3) 0.1111(4) 0.39051(16) 0.0951(17) Uani 1 d . . . H11G H 0.6373 0.1300 0.3860 0.143 Uiso 1 calc R . . H11H H 0.6825 0.0475 0.3876 0.143 Uiso 1 calc R . . H11I H 0.7057 0.1386 0.3686 0.143 Uiso 1 calc R . . C113 C 0.6651(2) 0.0971(3) 0.47098(15) 0.0774(14) Uani 1 d . . . H11J H 0.6829 0.1120 0.4999 0.116 Uiso 1 calc R . . H11K H 0.6646 0.0336 0.4674 0.116 Uiso 1 calc R . . H11L H 0.6228 0.1195 0.4683 0.116 Uiso 1 calc R . . O12 O 0.62900(11) 0.30860(18) 0.49575(8) 0.0551(7) Uani 1 d . . . C120 C 0.57146(18) 0.3400(3) 0.47577(15) 0.0697(13) Uani 1 d . . . C121 C 0.5214(2) 0.3037(5) 0.5031(2) 0.139(3) Uani 1 d . . . H12D H 0.5213 0.2399 0.5009 0.209 Uiso 1 calc R . . H12E H 0.4815 0.3266 0.4924 0.209 Uiso 1 calc R . . H12F H 0.5288 0.3210 0.5336 0.209 Uiso 1 calc R . . C122 C 0.5721(2) 0.4403(4) 0.47711(19) 0.1011(19) Uani 1 d . . . H12G H 0.5735 0.4600 0.5076 0.152 Uiso 1 calc R . . H12H H 0.5347 0.4628 0.4622 0.152 Uiso 1 calc R . . H12I H 0.6084 0.4620 0.4624 0.152 Uiso 1 calc R . . C123 C 0.5639(2) 0.3101(4) 0.42905(17) 0.0862(15) Uani 1 d . . . H12J H 0.5986 0.3312 0.4123 0.129 Uiso 1 calc R . . H12K H 0.5253 0.3334 0.4162 0.129 Uiso 1 calc R . . H12L H 0.5628 0.2462 0.4282 0.129 Uiso 1 calc R . . N1 N 0.74432(13) 0.25147(19) 0.70799(10) 0.0469(8) Uani 1 d . . . H1A H 0.7358 0.2083 0.6883 0.056 Uiso 1 calc R . . H1B H 0.7570 0.3000 0.6937 0.056 Uiso 1 calc R . . H1C H 0.7098 0.2641 0.7228 0.056 Uiso 1 calc R . . C1 C 0.79352(17) 0.2223(3) 0.73910(13) 0.0549(10) Uani 1 d . . . H1D H 0.8312 0.2093 0.7230 0.066 Uiso 1 calc R . . H1E H 0.7805 0.1680 0.7537 0.066 Uiso 1 calc R . . C2 C 0.80772(18) 0.2916(3) 0.77332(14) 0.0605(11) Uani 1 d . . . H2A H 0.7790 0.2889 0.7978 0.073 Uiso 1 d R . . H2B H 0.8038 0.3492 0.7589 0.073 Uiso 1 d R . . C3 C 0.8647(3) 0.2741(5) 0.8009(2) 0.108(2) Uani 1 d . . . H3 H 0.8985 0.2782 0.7795 0.130 Uiso 1 calc R A 1 C4 C 0.8763(4) 0.3539(6) 0.8311(2) 0.161(3) Uani 1 d . . . H4A H 0.8477 0.3522 0.8552 0.241 Uiso 1 calc R . . H4B H 0.8698 0.4077 0.8143 0.241 Uiso 1 calc R . . H4C H 0.9188 0.3523 0.8430 0.241 Uiso 1 calc R . . C5 C 0.8742(6) 0.1977(7) 0.8196(4) 0.131(5) Uani 0.674(13) d P B 1 H5A H 0.8424 0.1871 0.8409 0.197 Uiso 0.674(13) calc PR B 1 H5B H 0.9149 0.1973 0.8345 0.197 Uiso 0.674(13) calc PR B 1 H5C H 0.8724 0.1518 0.7972 0.197 Uiso 0.674(13) calc PR B 1 C5A C 0.9205(7) 0.2596(16) 0.7866(8) 0.131(13) Uani 0.326(13) d P B 2 H5A1 H 0.9181 0.2169 0.7628 0.197 Uiso 0.326(13) calc PR B 2 H5A2 H 0.9470 0.2370 0.8106 0.197 Uiso 0.326(13) calc PR B 2 H5A3 H 0.9377 0.3144 0.7758 0.197 Uiso 0.326(13) calc PR B 2 N2 N 0.75410(12) 0.44853(19) 0.58457(10) 0.0458(8) Uani 1 d . . . H2C H 0.7586 0.3987 0.5688 0.055 Uiso 1 calc R . . H2D H 0.7435 0.4347 0.6122 0.055 Uiso 1 calc R . . H2E H 0.7903 0.4786 0.5855 0.055 Uiso 1 calc R . . C15 C 0.70532(17) 0.5029(2) 0.56369(13) 0.0520(10) Uani 1 d . . . H15A H 0.6669 0.4684 0.5606 0.062 Uiso 1 calc R . . H15B H 0.7178 0.5196 0.5340 0.062 Uiso 1 calc R . . C16 C 0.69311(17) 0.5837(2) 0.58948(14) 0.0543(10) Uani 1 d . . . H16A H 0.7310 0.6197 0.5908 0.065 Uiso 1 calc R . . H16B H 0.6840 0.5667 0.6198 0.065 Uiso 1 calc R . . C17 C 0.64066(19) 0.6386(3) 0.57129(17) 0.0702(13) Uani 1 d . . . H17 H 0.6042 0.5995 0.5666 0.084 Uiso 1 calc R . . C18 C 0.6232(2) 0.7087(3) 0.6035(2) 0.0971(18) Uani 1 d . . . H18A H 0.6118 0.6813 0.6311 0.146 Uiso 1 calc R . . H18B H 0.5881 0.7421 0.5914 0.146 Uiso 1 calc R . . H18C H 0.6583 0.7478 0.6090 0.146 Uiso 1 calc R . . C19 C 0.6555(2) 0.6779(3) 0.52766(18) 0.0912(17) Uani 1 d . . . H19A H 0.6945 0.7100 0.5305 0.137 Uiso 1 calc R . . H19B H 0.6224 0.7178 0.5182 0.137 Uiso 1 calc R . . H19C H 0.6593 0.6313 0.5060 0.137 Uiso 1 calc R . . N3 N 0.63578(12) 0.23498(19) 0.58561(10) 0.0454(8) Uani 1 d . . . H3A H 0.6383 0.2861 0.6007 0.055 Uiso 1 calc R . . H3B H 0.6277 0.2463 0.5568 0.055 Uiso 1 calc R . . H3C H 0.6721 0.2057 0.5887 0.055 Uiso 1 calc R . . C25 C 0.58584(17) 0.1812(3) 0.60285(14) 0.0547(10) Uani 1 d . . . H25A H 0.5470 0.2152 0.6014 0.066 Uiso 1 calc R . . H25B H 0.5955 0.1678 0.6340 0.066 Uiso 1 calc R . . C26 C 0.57652(19) 0.0982(3) 0.57842(16) 0.0667(12) Uani 1 d . . . H26A H 0.6157 0.0651 0.5794 0.080 Uiso 1 calc R . . H26B H 0.5662 0.1120 0.5474 0.080 Uiso 1 calc R . . C27 C 0.5259(2) 0.0404(4) 0.5961(2) 0.0904(16) Uani 1 d . . . H27 H 0.5328 0.0326 0.6283 0.108 Uiso 1 calc R . . C28 C 0.4642(3) 0.0807(5) 0.5873(3) 0.158(3) Uani 1 d . . . H28A H 0.4627 0.1378 0.6017 0.237 Uiso 1 calc R . . H28B H 0.4322 0.0428 0.5988 0.237 Uiso 1 calc R . . H28C H 0.4572 0.0880 0.5557 0.237 Uiso 1 calc R . . C29 C 0.5266(4) -0.0462(4) 0.5743(4) 0.197(5) Uani 1 d . . . H29A H 0.5639 -0.0780 0.5838 0.295 Uiso 1 calc R . . H29B H 0.5263 -0.0382 0.5425 0.295 Uiso 1 calc R . . H29C H 0.4902 -0.0796 0.5823 0.295 Uiso 1 calc R . . N4 N 0.86510(12) 0.20939(18) 0.59612(10) 0.0435(7) Uani 1 d . . . H4D H 0.8634 0.2509 0.6173 0.052 Uiso 1 calc R . . H4E H 0.8739 0.1568 0.6086 0.052 Uiso 1 calc R . . H4F H 0.8280 0.2063 0.5814 0.052 Uiso 1 calc R . . C35 C 0.91370(17) 0.2323(2) 0.56530(13) 0.0510(10) Uani 1 d . . . H35A H 0.9537 0.2369 0.5817 0.061 Uiso 1 calc R . . H35B H 0.9043 0.2901 0.5522 0.061 Uiso 1 calc R . . C36 C 0.91924(18) 0.1660(3) 0.52917(13) 0.0565(11) Uani 1 d . . . H36A H 0.8782 0.1578 0.5147 0.068 Uiso 1 calc R . . H36B H 0.9318 0.1095 0.5423 0.068 Uiso 1 calc R . . C37 C 0.9653(2) 0.1908(3) 0.49444(15) 0.0700(13) Uani 1 d . . . H37 H 0.9545 0.2501 0.4828 0.084 Uiso 1 calc R . . C38 C 1.0295(3) 0.1930(5) 0.5129(2) 0.126(2) Uani 1 d . . . H38A H 1.0326 0.2365 0.5364 0.189 Uiso 1 calc R . . H38B H 1.0578 0.2085 0.4899 0.189 Uiso 1 calc R . . H38C H 1.0405 0.1354 0.5248 0.189 Uiso 1 calc R . . C39 C 0.9614(3) 0.1256(6) 0.4568(2) 0.146(3) Uani 1 d . . . H39A H 0.9749 0.0681 0.4673 0.219 Uiso 1 calc R . . H39B H 0.9880 0.1449 0.4335 0.219 Uiso 1 calc R . . H39C H 0.9187 0.1220 0.4454 0.219 Uiso 1 calc R . . C43X C 0.8071(6) 0.8598(11) 0.3839(4) 0.308(13) Uiso 0.767(10) d PD C 1 C44 C 0.7807(5) 0.8207(7) 0.3467(3) 0.172(5) Uiso 0.767(10) d PD C 1 H44 H 0.7982 0.8273 0.3189 0.206 Uiso 0.767(10) calc PR C 1 C45 C 0.7283(5) 0.7721(7) 0.3518(4) 0.188(6) Uiso 0.767(10) d PD C 1 H45 H 0.7108 0.7427 0.3270 0.226 Uiso 0.767(10) calc PR C 1 C46 C 0.7001(6) 0.7642(12) 0.3907(5) 0.265(9) Uiso 0.767(10) d PD C 1 H46 H 0.6635 0.7306 0.3927 0.318 Uiso 0.767(10) calc PR C 1 C47 C 0.7255(8) 0.8055(16) 0.4271(5) 0.392(17) Uiso 0.767(10) d PD C 1 H47 H 0.7038 0.8095 0.4534 0.470 Uiso 0.767(10) calc PR C 1 C48 C 0.7837(6) 0.8411(9) 0.4238(3) 0.194(6) Uiso 0.767(10) d PD C 1 H48 H 0.8078 0.8528 0.4497 0.232 Uiso 0.767(10) calc PR C 1 C49 C 0.8600(5) 0.9086(8) 0.3839(4) 0.191(6) Uiso 0.767(10) d PD C 1 H49A H 0.8823 0.9020 0.4121 0.286 Uiso 0.767(10) calc PR C 1 H49B H 0.8494 0.9702 0.3793 0.286 Uiso 0.767(10) calc PR C 1 H49C H 0.8861 0.8885 0.3604 0.286 Uiso 0.767(10) calc PR C 1 C43Y C 0.8071(6) 0.8605(9) 0.3890(4) 0.041(5) Uiso 0.233(10) d PD C 2 C44A C 0.7480(8) 0.874(2) 0.3711(9) 0.25(3) Uiso 0.233(10) d PD C 2 H44A H 0.7422 0.9132 0.3472 0.304 Uiso 0.233(10) calc PR C 2 C45A C 0.6982(7) 0.832(3) 0.3876(13) 0.39(6) Uiso 0.233(10) d PD C 2 H45A H 0.6583 0.8410 0.3747 0.473 Uiso 0.233(10) calc PR C 2 C46A C 0.7058(9) 0.776(2) 0.4228(10) 0.139(13) Uiso 0.233(10) d PD C 2 H46A H 0.6711 0.7496 0.4355 0.167 Uiso 0.233(10) calc PR C 2 C47A C 0.7651(11) 0.7590(16) 0.4393(8) 0.133(12) Uiso 0.233(10) d PD C 2 H47A H 0.7718 0.7131 0.4598 0.160 Uiso 0.233(10) calc PR C 2 C48A C 0.8145(8) 0.8088(16) 0.4259(6) 0.112(10) Uiso 0.233(10) d PD C 2 H48A H 0.8528 0.8073 0.4418 0.134 Uiso 0.233(10) calc PR C 2 C49A C 0.8498(10) 0.8661(19) 0.3552(7) 0.109(10) Uiso 0.233(10) d PD C 2 H49D H 0.8918 0.8605 0.3677 0.164 Uiso 0.233(10) calc PR C 2 H49E H 0.8453 0.9226 0.3404 0.164 Uiso 0.233(10) calc PR C 2 H49F H 0.8418 0.8190 0.3340 0.164 Uiso 0.233(10) calc PR C 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 S1 0.0420(5) 0.0392(6) 0.0652(7) -0.0022(5) -0.0059(4) 0.0057(4) Si1 0.0378(6) 0.0326(5) 0.0523(7) 0.0031(5) 0.0039(4) 0.0004(4) S2 0.0432(5) 0.0425(5) 0.0515(6) 0.0007(4) 0.0059(4) -0.0096(4) Si2 0.0346(5) 0.0372(6) 0.0555(7) -0.0008(5) 0.0037(4) -0.0053(4) S3 0.0506(6) 0.0504(6) 0.0536(7) 0.0026(5) 0.0187(5) -0.0016(4) Si3 0.0344(5) 0.0475(6) 0.0443(6) 0.0070(5) 0.0061(4) 0.0025(4) Si4 0.0468(6) 0.0592(7) 0.0374(6) 0.0030(5) -0.0022(5) -0.0013(5) S4 0.0454(6) 0.0656(7) 0.0432(6) -0.0028(5) -0.0051(4) 0.0064(5) O1 0.0545(15) 0.0354(14) 0.0581(18) 0.0019(12) 0.0085(12) -0.0019(11) C10 0.069(3) 0.036(2) 0.059(3) -0.0067(19) 0.009(2) -0.0088(19) C11 0.077(3) 0.053(3) 0.088(4) -0.006(2) -0.012(3) 0.001(2) C12 0.075(3) 0.051(3) 0.088(4) -0.017(2) 0.012(3) -0.003(2) C13 0.093(3) 0.059(3) 0.065(3) -0.006(2) 0.021(2) -0.021(2) O2 0.0327(12) 0.0404(14) 0.0611(17) 0.0105(12) -0.0014(11) 0.0016(11) C20 0.038(2) 0.056(2) 0.072(3) 0.016(2) -0.0051(19) 0.0073(18) C21 0.066(3) 0.125(4) 0.084(4) -0.006(3) -0.029(3) 0.019(3) C22 0.037(2) 0.108(4) 0.126(5) 0.042(4) -0.001(3) -0.001(2) C23 0.065(3) 0.066(3) 0.130(5) 0.024(3) 0.003(3) 0.022(2) O3 0.0489(15) 0.0498(15) 0.0570(17) 0.0094(13) 0.0084(12) -0.0030(12) C30 0.063(3) 0.046(2) 0.068(3) 0.009(2) 0.019(2) -0.002(2) C31 0.106(4) 0.116(5) 0.083(4) 0.011(4) 0.026(3) -0.019(4) C32 0.076(4) 0.166(6) 0.101(4) 0.029(4) 0.015(3) -0.050(4) C33 0.166(6) 0.051(3) 0.185(7) 0.025(4) 0.087(5) 0.005(3) O4 0.0358(13) 0.0551(15) 0.0561(17) 0.0124(13) 0.0080(11) -0.0058(11) C40 0.053(2) 0.060(3) 0.074(3) 0.022(2) 0.017(2) -0.006(2) C41 0.094(4) 0.091(4) 0.068(3) 0.011(3) 0.031(3) 0.012(3) C42 0.078(3) 0.077(3) 0.080(3) 0.037(3) 0.017(3) 0.009(3) C43 0.093(4) 0.096(4) 0.115(5) 0.032(3) 0.000(3) -0.050(3) O5 0.0334(13) 0.0555(16) 0.0663(18) -0.0022(13) 0.0019(12) 0.0006(12) C50 0.041(2) 0.076(3) 0.094(4) -0.005(3) -0.003(2) -0.001(2) C51 0.077(4) 0.118(5) 0.155(6) 0.058(5) -0.037(4) -0.001(3) C52 0.055(3) 0.110(4) 0.117(5) -0.017(4) -0.008(3) -0.023(3) C53 0.057(3) 0.152(6) 0.188(7) -0.065(5) -0.015(4) 0.042(4) O6 0.0444(14) 0.0423(14) 0.0678(18) -0.0106(13) -0.0012(12) -0.0047(12) C60 0.060(3) 0.048(2) 0.081(3) -0.023(2) -0.012(2) 0.003(2) C61 0.073(3) 0.103(4) 0.079(4) -0.040(3) 0.005(3) 0.005(3) C62 0.098(4) 0.050(3) 0.152(5) -0.038(3) -0.027(4) -0.002(3) C63 0.066(3) 0.064(3) 0.121(4) -0.036(3) -0.021(3) 0.025(2) O7 0.0483(15) 0.0596(16) 0.0523(16) -0.0080(13) 0.0049(12) 0.0168(13) C70 0.062(3) 0.057(3) 0.061(3) -0.016(2) -0.010(2) 0.008(2) C71 0.056(3) 0.077(3) 0.086(3) -0.015(3) -0.012(2) 0.010(2) C72 0.099(4) 0.060(3) 0.094(4) -0.007(3) -0.003(3) -0.003(3) C73 0.095(4) 0.085(3) 0.073(3) -0.030(3) -0.005(3) 0.030(3) O8 0.0383(13) 0.0521(15) 0.0584(17) 0.0155(13) 0.0050(12) -0.0031(11) C80 0.050(2) 0.073(3) 0.061(3) 0.026(2) 0.000(2) -0.013(2) C81 0.076(3) 0.103(4) 0.094(4) 0.052(3) -0.015(3) -0.025(3) C82 0.101(4) 0.101(4) 0.089(4) 0.042(3) -0.021(3) -0.058(3) C83 0.097(4) 0.125(5) 0.077(4) 0.034(3) 0.040(3) -0.002(3) O9 0.0364(14) 0.0694(17) 0.0605(17) 0.0126(14) -0.0030(12) 0.0009(13) C90 0.041(2) 0.085(3) 0.064(3) 0.000(3) -0.005(2) 0.016(2) C91 0.119(5) 0.187(8) 0.227(9) 0.074(7) 0.102(6) 0.095(5) C92 0.240(9) 0.142(6) 0.218(9) -0.084(6) -0.181(8) 0.101(7) C93 0.091(4) 0.119(5) 0.139(6) 0.066(4) -0.016(4) 0.018(4) O10 0.0685(18) 0.0644(18) 0.0566(18) 0.0138(15) -0.0052(14) -0.0054(14) C100 0.098(4) 0.085(4) 0.045(3) 0.015(2) 0.001(3) -0.033(3) C101 0.129(5) 0.131(5) 0.047(3) 0.013(3) -0.007(3) -0.028(4) C102 0.085(4) 0.165(6) 0.077(4) 0.029(4) 0.014(3) -0.038(4) C103 0.172(7) 0.103(5) 0.096(5) 0.016(4) 0.009(4) -0.059(4) O11 0.0649(17) 0.0685(19) 0.0394(16) -0.0017(14) -0.0036(13) -0.0045(14) C110 0.072(3) 0.073(3) 0.047(3) -0.014(2) -0.004(2) -0.001(2) C111 0.088(4) 0.109(4) 0.089(4) -0.030(3) -0.002(3) 0.026(3) C112 0.125(4) 0.097(4) 0.062(3) -0.028(3) -0.022(3) -0.010(3) C113 0.095(4) 0.070(3) 0.067(3) 0.007(3) -0.001(3) -0.009(3) O12 0.0415(14) 0.0806(19) 0.0426(15) 0.0137(14) -0.0067(11) 0.0077(13) C120 0.045(2) 0.099(4) 0.064(3) 0.019(3) -0.015(2) 0.012(2) C121 0.042(3) 0.254(9) 0.123(5) 0.081(6) 0.008(3) 0.022(4) C122 0.091(4) 0.113(5) 0.098(4) -0.020(3) -0.028(3) 0.050(3) C123 0.080(3) 0.096(4) 0.080(4) 0.000(3) -0.034(3) 0.006(3) N1 0.0407(17) 0.0442(18) 0.056(2) -0.0009(15) 0.0018(14) 0.0028(14) C1 0.046(2) 0.054(2) 0.064(3) 0.006(2) -0.0067(19) 0.0027(18) C2 0.055(2) 0.069(3) 0.057(3) 0.002(2) -0.003(2) 0.006(2) C3 0.100(5) 0.128(6) 0.093(4) -0.013(4) -0.044(4) 0.002(4) C4 0.173(7) 0.182(7) 0.122(6) -0.044(6) -0.079(5) -0.005(6) C5 0.169(12) 0.099(7) 0.120(9) 0.021(6) -0.072(8) 0.012(7) C5A 0.032(9) 0.19(2) 0.18(2) -0.11(2) -0.020(10) 0.024(11) N2 0.0417(17) 0.0464(18) 0.0495(19) 0.0037(15) 0.0045(14) -0.0037(14) C15 0.045(2) 0.057(2) 0.053(2) 0.015(2) -0.0071(18) -0.0045(19) C16 0.053(2) 0.045(2) 0.065(3) 0.013(2) 0.002(2) -0.0022(18) C17 0.050(2) 0.055(3) 0.106(4) 0.017(3) -0.004(2) -0.007(2) C18 0.081(4) 0.067(3) 0.144(5) 0.011(3) 0.013(3) 0.019(3) C19 0.083(3) 0.077(3) 0.111(4) 0.033(3) -0.030(3) -0.006(3) N3 0.0375(16) 0.0518(18) 0.0468(19) 0.0013(15) -0.0002(14) 0.0024(14) C25 0.043(2) 0.065(3) 0.057(3) 0.001(2) 0.0060(18) -0.0057(19) C26 0.056(3) 0.067(3) 0.077(3) 0.001(3) 0.003(2) -0.002(2) C27 0.068(3) 0.090(4) 0.112(4) 0.009(3) -0.008(3) -0.032(3) C28 0.100(5) 0.174(7) 0.202(8) -0.015(6) 0.048(5) -0.063(5) C29 0.136(7) 0.079(5) 0.376(15) -0.017(7) 0.016(8) -0.043(4) N4 0.0404(16) 0.0372(16) 0.053(2) 0.0024(14) -0.0001(14) -0.0014(13) C35 0.044(2) 0.044(2) 0.066(3) 0.009(2) 0.0097(19) -0.0052(17) C36 0.053(2) 0.059(3) 0.058(3) 0.001(2) 0.0085(19) -0.002(2) C37 0.068(3) 0.072(3) 0.072(3) 0.015(3) 0.023(2) 0.003(2) C38 0.082(4) 0.168(6) 0.130(6) -0.018(5) 0.039(4) -0.026(4) C39 0.135(6) 0.225(9) 0.080(4) -0.048(5) 0.044(4) -0.012(6) _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 S1 Si1 2.0368(13) . ? Si1 O1 1.622(3) . ? Si1 O3 1.628(3) . ? Si1 O2 1.647(2) . ? S2 Si2 2.0371(13) . ? Si2 O5 1.621(3) . ? Si2 O6 1.626(3) . ? Si2 O4 1.659(3) . ? S3 Si3 2.0481(14) . ? Si3 O9 1.625(3) . ? Si3 O7 1.629(3) . ? Si3 O8 1.645(3) . ? Si4 O10 1.625(3) . ? Si4 O11 1.635(3) . ? Si4 O12 1.642(3) . ? Si4 S4 2.0370(15) . ? O1 C10 1.438(5) . ? C10 C12 1.500(5) . ? C10 C11 1.519(6) . ? C10 C13 1.522(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O2 C20 1.455(4) . ? C20 C22 1.498(6) . ? C20 C21 1.509(6) . ? C20 C23 1.514(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O3 C30 1.432(4) . ? C30 C31 1.479(7) . ? C30 C33 1.490(7) . ? C30 C32 1.518(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O4 C40 1.469(5) . ? C40 C43 1.493(6) . ? C40 C42 1.510(6) . ? C40 C41 1.511(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O5 C50 1.432(5) . ? C50 C53 1.516(7) . ? C50 C51 1.519(7) . ? C50 C52 1.528(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O6 C60 1.424(5) . ? C60 C63 1.506(6) . ? C60 C62 1.518(6) . ? C60 C61 1.522(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? O7 C70 1.433(5) . ? C70 C72 1.497(6) . ? C70 C71 1.510(6) . ? C70 C73 1.529(6) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? O8 C80 1.459(4) . ? C80 C82 1.486(6) . ? C80 C81 1.504(6) . ? C80 C83 1.518(7) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? O9 C90 1.434(5) . ? C90 C92 1.462(7) . ? C90 C91 1.496(7) . ? C90 C93 1.501(7) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? O10 C100 1.446(5) . ? C100 C102 1.493(7) . ? C100 C103 1.507(8) . ? C100 C101 1.525(6) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? O11 C110 1.434(5) . ? C110 C111 1.501(6) . ? C110 C113 1.508(6) . ? C110 C112 1.522(6) . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C113 H11J 0.9800 . ? C113 H11K 0.9800 . ? C113 H11L 0.9800 . ? O12 C120 1.454(4) . ? C120 C121 1.500(7) . ? C120 C123 1.504(7) . ? C120 C122 1.537(7) . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C122 H12G 0.9800 . ? C122 H12H 0.9800 . ? C122 H12I 0.9800 . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C123 H12L 0.9800 . ? N1 C1 1.475(4) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C1 C2 1.515(6) . ? C1 H1D 0.9900 . ? C1 H1E 0.9900 . ? C2 C3 1.497(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.316(10) . ? C3 C5A 1.320(17) . ? C3 C4 1.549(9) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? N2 C15 1.476(4) . ? N2 H2C 0.9100 . ? N2 H2D 0.9100 . ? N2 H2E 0.9100 . ? C15 C16 1.497(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.507(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.508(7) . ? C17 C18 1.515(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N3 C25 1.473(5) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? C25 C26 1.486(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.526(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C29 1.485(9) . ? C27 C28 1.490(9) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N4 C35 1.481(4) . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N4 H4F 0.9100 . ? C35 C36 1.509(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.532(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.486(7) . ? C37 C39 1.525(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C43X C48 1.370(8) . ? C43X C49 1.371(7) . ? C43X C44 1.391(8) . ? C44 C45 1.373(7) . ? C44 H44 0.9500 . ? C45 C46 1.361(8) . ? C45 H45 0.9500 . ? C46 C47 1.379(9) . ? C46 H46 0.9500 . ? C47 C48 1.383(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C43Y C48A 1.383(8) . ? C43Y C44A 1.394(8) . ? C43Y C49A 1.415(9) . ? C44A C45A 1.371(8) . ? C44A H44A 0.9500 . ? C45A C46A 1.381(9) . ? C45A H45A 0.9500 . ? C46A C47A 1.391(9) . ? C46A H46A 0.9500 . ? C47A C48A 1.390(9) . ? C47A H47A 0.9500 . ? C48A H48A 0.9500 . ? C49A H49D 0.9800 . ? C49A H49E 0.9800 . ? C49A H49F 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 O3 104.48(13) . . ? O1 Si1 O2 109.01(13) . . ? O3 Si1 O2 104.99(13) . . ? O1 Si1 S1 114.88(11) . . ? O3 Si1 S1 115.67(11) . . ? O2 Si1 S1 107.26(9) . . ? O5 Si2 O6 105.01(13) . . ? O5 Si2 O4 104.75(14) . . ? O6 Si2 O4 108.96(14) . . ? O5 Si2 S2 115.55(11) . . ? O6 Si2 S2 114.77(11) . . ? O4 Si2 S2 107.25(10) . . ? O9 Si3 O7 104.90(14) . . ? O9 Si3 O8 105.08(13) . . ? O7 Si3 O8 109.32(14) . . ? O9 Si3 S3 114.34(11) . . ? O7 Si3 S3 115.47(11) . . ? O8 Si3 S3 107.21(10) . . ? O10 Si4 O11 104.27(15) . . ? O10 Si4 O12 103.57(15) . . ? O11 Si4 O12 109.70(15) . . ? O10 Si4 S4 116.37(12) . . ? O11 Si4 S4 115.13(11) . . ? O12 Si4 S4 107.13(10) . . ? C10 O1 Si1 133.5(2) . . ? O1 C10 C12 105.9(3) . . ? O1 C10 C11 108.7(3) . . ? C12 C10 C11 110.7(3) . . ? O1 C10 C13 111.0(3) . . ? C12 C10 C13 109.8(4) . . ? C11 C10 C13 110.6(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 O2 Si1 130.2(2) . . ? O2 C20 C22 105.9(3) . . ? O2 C20 C21 108.0(3) . . ? C22 C20 C21 111.1(4) . . ? O2 C20 C23 110.8(3) . . ? C22 C20 C23 109.4(4) . . ? C21 C20 C23 111.6(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C30 O3 Si1 132.8(3) . . ? O3 C30 C31 106.5(4) . . ? O3 C30 C33 107.3(4) . . ? C31 C30 C33 112.1(5) . . ? O3 C30 C32 111.1(4) . . ? C31 C30 C32 110.0(4) . . ? C33 C30 C32 109.9(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C40 O4 Si2 131.9(2) . . ? O4 C40 C43 110.0(4) . . ? O4 C40 C42 104.8(3) . . ? C43 C40 C42 110.6(4) . . ? O4 C40 C41 107.8(3) . . ? C43 C40 C41 113.0(4) . . ? C42 C40 C41 110.3(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C50 O5 Si2 132.7(3) . . ? O5 C50 C53 105.3(4) . . ? O5 C50 C51 110.9(4) . . ? C53 C50 C51 114.7(5) . . ? O5 C50 C52 108.2(4) . . ? C53 C50 C52 109.2(4) . . ? C51 C50 C52 108.4(5) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C60 O6 Si2 132.6(2) . . ? O6 C60 C63 112.4(4) . . ? O6 C60 C62 105.9(4) . . ? C63 C60 C62 111.2(4) . . ? O6 C60 C61 107.6(3) . . ? C63 C60 C61 109.8(4) . . ? C62 C60 C61 109.8(4) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C70 O7 Si3 133.9(2) . . ? O7 C70 C72 107.9(3) . . ? O7 C70 C71 111.4(3) . . ? C72 C70 C71 111.1(4) . . ? O7 C70 C73 104.5(4) . . ? C72 C70 C73 111.4(4) . . ? C71 C70 C73 110.4(4) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C80 O8 Si3 130.2(2) . . ? O8 C80 C82 108.3(3) . . ? O8 C80 C81 105.1(3) . . ? C82 C80 C81 111.6(4) . . ? O8 C80 C83 110.6(4) . . ? C82 C80 C83 112.2(4) . . ? C81 C80 C83 108.8(4) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C80 C83 H83A 109.5 . . ? C80 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C80 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C90 O9 Si3 132.6(3) . . ? O9 C90 C92 105.0(4) . . ? O9 C90 C91 105.4(4) . . ? C92 C90 C91 114.2(7) . . ? O9 C90 C93 113.6(4) . . ? C92 C90 C93 109.3(6) . . ? C91 C90 C93 109.3(5) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 C93 H93A 109.5 . . ? C90 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C90 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C100 O10 Si4 132.6(3) . . ? O10 C100 C102 111.1(4) . . ? O10 C100 C103 105.6(5) . . ? C102 C100 C103 112.1(5) . . ? O10 C100 C101 107.4(4) . . ? C102 C100 C101 110.3(5) . . ? C103 C100 C101 110.2(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C100 C102 H10D 109.5 . . ? C100 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C100 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C100 C103 H10G 109.5 . . ? C100 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? C100 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C110 O11 Si4 132.7(3) . . ? O11 C110 C111 108.4(4) . . ? O11 C110 C113 111.4(4) . . ? C111 C110 C113 110.8(4) . . ? O11 C110 C112 104.6(4) . . ? C111 C110 C112 110.0(4) . . ? C113 C110 C112 111.4(4) . . ? C110 C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C110 C112 H11I 109.5 . . ? H11G C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C110 C113 H11J 109.5 . . ? C110 C113 H11K 109.5 . . ? H11J C113 H11K 109.5 . . ? C110 C113 H11L 109.5 . . ? H11J C113 H11L 109.5 . . ? H11K C113 H11L 109.5 . . ? C120 O12 Si4 130.3(2) . . ? O12 C120 C121 105.8(4) . . ? O12 C120 C123 111.3(4) . . ? C121 C120 C123 110.9(5) . . ? O12 C120 C122 108.3(4) . . ? C121 C120 C122 111.2(5) . . ? C123 C120 C122 109.3(4) . . ? C120 C121 H12D 109.5 . . ? C120 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C120 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? C120 C122 H12G 109.5 . . ? C120 C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? C120 C122 H12I 109.5 . . ? H12G C122 H12I 109.5 . . ? H12H C122 H12I 109.5 . . ? C120 C123 H12J 109.5 . . ? C120 C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? C120 C123 H12L 109.5 . . ? H12J C123 H12L 109.5 . . ? H12K C123 H12L 109.5 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 C2 111.1(3) . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? N1 C1 H1E 109.4 . . ? C2 C1 H1E 109.4 . . ? H1D C1 H1E 108.0 . . ? C3 C2 C1 114.1(4) . . ? C3 C2 H2A 95.5 . . ? C1 C2 H2A 112.0 . . ? C3 C2 H2B 118.0 . . ? C1 C2 H2B 107.7 . . ? H2A C2 H2B 109.1 . . ? C5 C3 C5A 82.1(13) . . ? C5 C3 C2 121.2(7) . . ? C5A C3 C2 126.4(12) . . ? C5 C3 C4 115.1(7) . . ? C5A C3 C4 101.4(9) . . ? C2 C3 C4 108.0(5) . . ? C5 C3 H3 103.4 . . ? C2 C3 H3 103.4 . . ? C4 C3 H3 103.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C5A H5A1 109.5 . . ? C3 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C3 C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C15 N2 H2C 109.5 . . ? C15 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C15 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? N2 C15 C16 112.1(3) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 114.4(4) . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C19 111.6(4) . . ? C16 C17 C18 111.0(4) . . ? C19 C17 C18 111.1(4) . . ? C16 C17 H17 107.7 . . ? C19 C17 H17 107.7 . . ? C18 C17 H17 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 N3 H3A 109.5 . . ? C25 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C25 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? N3 C25 C26 112.8(3) . . ? N3 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? N3 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 114.0(4) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.6 . . ? C29 C27 C28 108.3(6) . . ? C29 C27 C26 109.9(5) . . ? C28 C27 C26 110.4(5) . . ? C29 C27 H27 109.4 . . ? C28 C27 H27 109.4 . . ? C26 C27 H27 109.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 N4 H4D 109.5 . . ? C35 N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C35 N4 H4F 109.5 . . ? H4D N4 H4F 109.5 . . ? H4E N4 H4F 109.5 . . ? N4 C35 C36 112.5(3) . . ? N4 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? N4 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C37 114.3(3) . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C39 109.2(5) . . ? C38 C37 C36 111.6(4) . . ? C39 C37 C36 109.9(4) . . ? C38 C37 H37 108.7 . . ? C39 C37 H37 108.7 . . ? C36 C37 H37 108.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C48 C43X C49 116.7(8) . . ? C48 C43X C44 118.9(6) . . ? C49 C43X C44 123.9(8) . . ? C45 C44 C43X 117.5(7) . . ? C45 C44 H44 121.3 . . ? C43X C44 H44 121.3 . . ? C46 C45 C44 123.2(7) . . ? C46 C45 H45 118.4 . . ? C44 C45 H45 118.4 . . ? C45 C46 C47 118.9(7) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C46 C47 C48 117.7(8) . . ? C46 C47 H47 121.1 . . ? C48 C47 H47 121.1 . . ? C43X C48 C47 120.9(8) . . ? C43X C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48A C43Y C44A 119.1(7) . . ? C48A C43Y C49A 124.8(12) . . ? C44A C43Y C49A 108.6(11) . . ? C45A C44A C43Y 120.7(7) . . ? C45A C44A H44A 119.6 . . ? C43Y C44A H44A 119.6 . . ? C44A C45A C46A 120.4(8) . . ? C44A C45A H45A 119.8 . . ? C46A C45A H45A 119.8 . . ? C45A C46A C47A 118.9(7) . . ? C45A C46A H46A 120.6 . . ? C47A C46A H46A 120.6 . . ? C48A C47A C46A 120.2(8) . . ? C48A C47A H47A 119.9 . . ? C46A C47A H47A 119.9 . . ? C43Y C48A C47A 119.1(8) . . ? C43Y C48A H48A 120.4 . . ? C47A C48A H48A 120.4 . . ? C43Y C49A H49D 109.5 . . ? C43Y C49A H49E 109.5 . . ? H49D C49A H49E 109.5 . . ? C43Y C49A H49F 109.5 . . ? H49D C49A H49F 109.5 . . ? H49E C49A H49F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A S1 0.91 2.29 3.173(3) 163.5 . N1 H1B S2 0.91 2.52 3.288(3) 142.2 . N1 H1B S3 0.91 2.87 3.305(3) 111.2 . N1 H1C O8 0.91 2.09 2.951(4) 157.2 . N2 H2D S2 0.91 2.91 3.331(3) 109.7 . N2 H2D S3 0.91 2.43 3.192(3) 140.9 . N2 H2C S4 0.91 2.24 3.150(3) 173.2 . N2 H2E O4 0.91 1.98 2.850(4) 158.3 . N3 H3C S1 0.91 2.41 3.227(3) 150.2 . N3 H3A S3 0.91 2.29 3.179(3) 164.6 . N3 H3C S4 0.91 2.91 3.317(3) 108.5 . N3 H3B O12 0.91 2.10 2.970(4) 160.2 . N4 H4F S1 0.91 2.85 3.287(3) 110.7 . N4 H4D S2 0.91 2.27 3.172(3) 170.3 . N4 H4F S4 0.91 2.47 3.257(3) 145.4 . N4 H4E O2 0.91 2.04 2.912(4) 160.4 . _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.555 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.069