# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Chiu, Chien-Yang' 'Kim, Bumjung' 'Gorodetsky, Alon' 'Sattler, Wesley' 'Wei, Sujun' 'Sattler, Aaron' 'Steigerwald, Michael' 'Nuckolls, Colin' _publ_contact_author_name 'Nuckolls, Colin' _publ_contact_author_email cn37@columbia.edu _publ_section_title ; Shape-Shifting in Contorted Dibenzotetrathienocoronenes ; # Attachment '- 1a.cif' data_2s10 _database_code_depnum_ccdc_archive 'CCDC 817721' #TrackingRef '- 1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H16 S4' _chemical_formula_weight 624.77 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' S S 0.1246 0.1234 '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' _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 3.8220(7) _cell_length_b 13.266(2) _cell_length_c 13.858(2) _cell_angle_alpha 118.434(2) _cell_angle_beta 93.312(3) _cell_angle_gamma 94.220(3) _cell_volume 612.75(18) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 5500 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 32.43 _exptl_crystal_description NEEDLE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7643 _exptl_absorpt_correction_T_max 0.9916 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10530 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 32.55 _reflns_number_total 4150 _reflns_number_gt 3249 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Excess electron density (Q1 = 1.52) was found 0.563A away from C1 suggesting the possibility of a small fractional disorder between carbon and sulfur. However, this disorder was not modeled based on synthetic chemists knowledge of the synthetic route and spectroscopic data, which makes this disorder highly unlikely. ; _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^)+(0.0787P)^2^+1.0429P] 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 4150 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.71169(17) 0.53644(5) 0.40672(5) 0.01795(15) Uani 1 1 d . . . S2 S 0.01709(16) 0.68848(5) -0.24732(5) 0.01681(15) Uani 1 1 d . . . C1 C 0.0583(6) 0.8427(2) -0.03941(18) 0.0151(4) Uani 1 1 d . . . H1A H 0.0437 0.9128 0.0262 0.018 Uiso 1 1 calc R . . C2 C 0.2112(5) 0.74113(18) -0.04437(18) 0.0106(4) Uani 1 1 d . . . C3 C 0.3676(6) 0.72683(17) 0.04399(17) 0.0104(4) Uani 1 1 d . . . C4 C 0.4844(6) 0.82334(18) 0.15268(17) 0.0109(4) Uani 1 1 d . . . C5 C 0.5359(6) 0.94431(19) 0.17679(19) 0.0123(4) Uani 1 1 d . . . H5A H 0.4652 0.9623 0.1204 0.015 Uiso 1 1 calc R . . C6 C 0.6754(7) 1.0285(2) 0.2730(2) 0.0191(5) Uani 1 1 d . . . H6A H 0.6926 1.1059 0.2860 0.023 Uiso 1 1 calc R . . C7 C 0.7970(7) 1.0058(2) 0.3553(2) 0.0193(5) Uani 1 1 d . . . H7A H 0.9067 1.0672 0.4234 0.023 Uiso 1 1 calc R . . C8 C 0.7614(6) 0.8965(2) 0.33993(18) 0.0153(4) Uani 1 1 d . . . H8A H 0.8489 0.8827 0.3977 0.018 Uiso 1 1 calc R . . C9 C 0.5959(6) 0.80146(18) 0.23914(17) 0.0120(4) Uani 1 1 d . . . C10 C 0.5760(6) 0.68472(18) 0.22053(17) 0.0110(4) Uani 1 1 d . . . C11 C 0.6089(6) 0.65852(18) 0.30945(18) 0.0125(4) Uani 1 1 d . . . C12 C 0.5569(6) 0.7304(2) 0.42428(18) 0.0148(4) Uani 1 1 d . . . H12A H 0.4979 0.8071 0.4539 0.018 Uiso 1 1 calc R . . C13 C 0.6022(7) 0.6752(2) 0.4848(2) 0.0201(5) Uani 1 1 d . . . H13A H 0.5766 0.7090 0.5614 0.024 Uiso 1 1 calc R . . C14 C 0.6832(6) 0.54846(18) 0.28769(17) 0.0114(4) Uani 1 1 d . . . C15 C 0.7007(5) 0.45843(17) 0.17824(17) 0.0103(4) Uani 1 1 d . . . C16 C 0.1917(6) 0.65073(18) -0.15272(17) 0.0110(4) Uani 1 1 d . . . C17 C -0.0596(6) 0.82008(19) -0.1445(2) 0.0154(4) Uani 1 1 d . . . H17A H -0.1745 0.8735 -0.1587 0.019 Uiso 1 1 calc R . . C18 C 0.6027(5) 0.47899(17) 0.08948(16) 0.0094(3) Uani 1 1 d . . . C19 C 0.5390(5) 0.59315(17) 0.11145(17) 0.0097(4) Uani 1 1 d . . . C20 C 0.4348(5) 0.61493(17) 0.02196(17) 0.0094(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0237(3) 0.0172(3) 0.0139(3) 0.0084(2) -0.0001(2) 0.0031(2) S2 0.0190(3) 0.0157(3) 0.0169(3) 0.0092(2) -0.0020(2) 0.0026(2) C1 0.0125(9) 0.0289(12) 0.0139(9) 0.0159(9) 0.0078(7) 0.0155(8) C2 0.0102(8) 0.0094(8) 0.0133(9) 0.0064(7) 0.0015(7) 0.0013(7) C3 0.0125(9) 0.0077(8) 0.0107(9) 0.0040(7) 0.0016(7) 0.0017(7) C4 0.0110(9) 0.0095(8) 0.0113(9) 0.0043(7) 0.0016(7) 0.0022(7) C5 0.0114(9) 0.0188(10) 0.0177(10) 0.0158(8) 0.0083(7) 0.0094(7) C6 0.0207(11) 0.0140(10) 0.0211(11) 0.0069(9) 0.0051(9) 0.0028(8) C7 0.0186(11) 0.0117(9) 0.0210(11) 0.0027(9) 0.0016(9) 0.0007(8) C8 0.0166(10) 0.0161(10) 0.0118(9) 0.0061(8) -0.0012(8) 0.0016(8) C9 0.0146(9) 0.0090(8) 0.0109(9) 0.0036(7) 0.0013(7) 0.0021(7) C10 0.0136(9) 0.0087(8) 0.0094(8) 0.0034(7) 0.0000(7) 0.0014(7) C11 0.0152(9) 0.0110(9) 0.0100(9) 0.0043(7) -0.0003(7) 0.0014(7) C12 0.0163(10) 0.0147(9) 0.0117(9) 0.0048(8) 0.0008(7) 0.0041(8) C13 0.0221(11) 0.0258(12) 0.0114(10) 0.0080(9) 0.0013(8) 0.0038(9) C14 0.0142(9) 0.0109(9) 0.0089(8) 0.0051(7) -0.0014(7) 0.0004(7) C15 0.0116(9) 0.0091(8) 0.0099(8) 0.0048(7) -0.0010(7) 0.0001(7) C16 0.0114(9) 0.0111(9) 0.0114(9) 0.0066(7) -0.0005(7) 0.0006(7) C17 0.0142(10) 0.0151(10) 0.0216(11) 0.0125(9) 0.0010(8) 0.0036(8) C18 0.0094(8) 0.0094(8) 0.0092(8) 0.0045(7) 0.0007(7) 0.0009(6) C19 0.0105(8) 0.0089(8) 0.0099(8) 0.0046(7) 0.0011(7) 0.0023(7) C20 0.0091(8) 0.0090(8) 0.0097(8) 0.0041(7) 0.0010(6) 0.0013(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 C14 1.729(2) . ? S1 C13 1.733(3) . ? S2 C17 1.708(2) . ? S2 C16 1.729(2) . ? C1 C17 1.379(3) . ? C1 C2 1.481(3) . ? C2 C16 1.399(3) . ? C2 C3 1.430(3) . ? C3 C20 1.413(3) . ? C3 C4 1.452(3) . ? C4 C9 1.411(3) . ? C4 C5 1.470(3) . ? C5 C6 1.312(3) . ? C6 C7 1.376(4) . ? C7 C8 1.357(3) . ? C8 C9 1.430(3) . ? C9 C10 1.439(3) . ? C10 C19 1.408(3) . ? C10 C11 1.432(3) . ? C11 C14 1.398(3) . ? C11 C12 1.449(3) . ? C12 C13 1.363(3) . ? C14 C15 1.425(3) . ? C15 C16 1.417(3) 2_665 ? C15 C18 1.417(3) . ? C16 C15 1.417(3) 2_665 ? C18 C19 1.438(3) . ? C18 C20 1.440(3) 2_665 ? C19 C20 1.443(3) . ? C20 C18 1.440(3) 2_665 ? 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 C14 S1 C13 91.83(11) . . ? C17 S2 C16 91.59(11) . . ? C17 C1 C2 109.7(2) . . ? C16 C2 C3 119.41(18) . . ? C16 C2 C1 111.75(18) . . ? C3 C2 C1 128.84(19) . . ? C20 C3 C2 118.38(18) . . ? C20 C3 C4 118.69(18) . . ? C2 C3 C4 122.77(18) . . ? C9 C4 C3 119.28(18) . . ? C9 C4 C5 116.29(18) . . ? C3 C4 C5 124.01(19) . . ? C6 C5 C4 122.7(2) . . ? C5 C6 C7 120.6(2) . . ? C8 C7 C6 120.5(2) . . ? C7 C8 C9 121.8(2) . . ? C4 C9 C8 117.97(19) . . ? C4 C9 C10 119.97(19) . . ? C8 C9 C10 121.71(19) . . ? C19 C10 C11 118.66(19) . . ? C19 C10 C9 119.14(19) . . ? C11 C10 C9 122.14(19) . . ? C14 C11 C10 119.34(19) . . ? C14 C11 C12 111.89(19) . . ? C10 C11 C12 128.68(19) . . ? C13 C12 C11 112.2(2) . . ? C12 C13 S1 112.60(18) . . ? C11 C14 C15 121.88(19) . . ? C11 C14 S1 111.35(16) . . ? C15 C14 S1 126.57(16) . . ? C16 C15 C18 117.99(18) 2_665 . ? C16 C15 C14 123.94(19) 2_665 . ? C18 C15 C14 118.07(18) . . ? C2 C16 C15 122.41(19) . 2_665 ? C2 C16 S2 112.02(15) . . ? C15 C16 S2 125.55(16) 2_665 . ? C1 C17 S2 114.80(17) . . ? C15 C18 C19 119.79(18) . . ? C15 C18 C20 119.64(18) . 2_665 ? C19 C18 C20 120.57(18) . 2_665 ? C10 C19 C18 120.38(18) . . ? C10 C19 C20 119.27(18) . . ? C18 C19 C20 120.35(18) . . ? C3 C20 C18 120.72(18) . 2_665 ? C3 C20 C19 120.19(18) . . ? C18 C20 C19 119.09(18) 2_665 . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 32.55 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.525 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.123 # Attachment '- 1b.cif' data_fbu2s10 _database_code_depnum_ccdc_archive 'CCDC 817722' #TrackingRef '- 1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58.33 H50.67 S4' _chemical_formula_weight 879.90 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' 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 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 27.5560(11) _cell_length_b 16.5467(7) _cell_length_c 28.5253(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.4150(10) _cell_angle_gamma 90.00 _cell_volume 12967.8(9) _cell_formula_units_Z 12 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9364 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.50 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5576 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9070 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 207430 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 30.54 _reflns_number_total 39675 _reflns_number_gt 27222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The butyl groups are disordered and have been restrained using SAME and SADI restraints. As such, bond lengths and bond angles are not reliable. ; _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^)+(0.0766P)^2^+5.8966P] 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 39675 _refine_ls_number_parameters 1697 _refine_ls_number_restraints 2179 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_restrained_S_all 1.295 _refine_ls_shift/su_max 0.032 _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 S101 S 0.42588(3) 0.42798(4) 1.10758(2) 0.02784(14) Uani 1 1 d U . . S102 S 0.49978(2) 0.30418(4) 1.07715(2) 0.03087(15) Uani 1 1 d U . . S103 S 0.31186(2) 0.28020(4) 0.75486(2) 0.02387(12) Uani 1 1 d U . . S104 S 0.23342(2) 0.39314(4) 0.79056(2) 0.02346(12) Uani 1 1 d U . . S201 S 0.03198(2) 0.69613(4) 0.43831(2) 0.02478(13) Uani 1 1 d U . . S202 S 0.06881(2) 0.70507(4) 0.54166(2) 0.02518(13) Uani 1 1 d U . . S203 S -0.27168(2) 0.59487(4) 0.63463(2) 0.02502(13) Uani 1 1 d U . . S204 S -0.31305(2) 0.60572(4) 0.53332(2) 0.02768(14) Uani 1 1 d U . . S302 S 0.12756(2) 0.47782(4) 0.65418(2) 0.02579(13) Uani 1 1 d U . . S303 S -0.03341(2) 0.45492(4) 0.31141(2) 0.02558(13) Uani 1 1 d U . . S402 S 0.33487(2) 0.66463(4) 1.03145(2) 0.02379(12) Uani 1 1 d U . . S403 S 0.58174(2) 0.25283(4) 0.90855(2) 0.02305(12) Uani 1 1 d U . . C101 C 0.37769(8) 0.31194(14) 0.98734(8) 0.0190(4) Uani 1 1 d U . . C102 C 0.39271(8) 0.25663(14) 0.95262(8) 0.0183(4) Uani 1 1 d U . . C103 C 0.36595(8) 0.25292(14) 0.90731(8) 0.0173(4) Uani 1 1 d U . . C104 C 0.32396(8) 0.30333(13) 0.89749(8) 0.0173(4) Uani 1 1 d U . . C105 C 0.30316(8) 0.34314(13) 0.93566(8) 0.0180(4) Uani 1 1 d U . . C106 C 0.33010(8) 0.34848(14) 0.98098(8) 0.0191(4) Uani 1 1 d U . . C107 C 0.40794(9) 0.32740(15) 1.02861(8) 0.0211(4) Uani 1 1 d U . . C108 C 0.45366(9) 0.28732(15) 1.03340(8) 0.0223(5) Uani 1 1 d U . . C109 C 0.46711(9) 0.22885(15) 1.00140(9) 0.0226(5) Uani 1 1 d U . . C110 C 0.43430(8) 0.20826(14) 0.96175(8) 0.0200(4) Uani 1 1 d U . . C111 C 0.44013(8) 0.13843(15) 0.93177(8) 0.0218(5) Uani 1 1 d U . . C112 C 0.41318(8) 0.13462(14) 0.88735(8) 0.0209(4) Uani 1 1 d U . . C113 C 0.38161(8) 0.20141(14) 0.87242(8) 0.0190(4) Uani 1 1 d U . . C114 C 0.36383(8) 0.21543(14) 0.82458(8) 0.0196(4) Uani 1 1 d U . . C115 C 0.32523(8) 0.26939(14) 0.81485(8) 0.0190(4) Uani 1 1 d U . . C116 C 0.30221(8) 0.31014(14) 0.85109(8) 0.0178(4) Uani 1 1 d U . . C117 C 0.26067(8) 0.36070(14) 0.84403(8) 0.0189(4) Uani 1 1 d U . . C118 C 0.23798(8) 0.39452(14) 0.88156(8) 0.0196(4) Uani 1 1 d U . . C119 C 0.25739(8) 0.38023(14) 0.92881(8) 0.0191(4) Uani 1 1 d U . . C120 C 0.23242(9) 0.40256(14) 0.96965(8) 0.0207(4) Uani 1 1 d U . . C121 C 0.25947(9) 0.41177(14) 1.01352(8) 0.0220(5) Uani 1 1 d U . . C122 C 0.31118(9) 0.39345(14) 1.01727(8) 0.0212(4) Uani 1 1 d U . . C123 C 0.34427(9) 0.41779(15) 1.05595(8) 0.0222(5) Uani 1 1 d U . . C124 C 0.39141(9) 0.38518(15) 1.06067(8) 0.0225(5) Uani 1 1 d U . . C125 C 0.53794(10) 0.23608(18) 1.05246(10) 0.0336(6) Uani 1 1 d DU . . C126 C 0.51627(9) 0.20064(17) 1.01333(9) 0.0277(5) Uani 1 1 d U . . H12A H 0.5318 0.1612 0.9955 0.033 Uiso 1 1 calc R . . C127 C 0.46772(9) 0.06956(16) 0.94688(9) 0.0269(5) Uani 1 1 d U . . H12B H 0.4862 0.0710 0.9764 0.032 Uiso 1 1 calc R . . C128 C 0.46844(10) 0.00094(17) 0.92002(10) 0.0311(6) Uani 1 1 d U . . H12C H 0.4877 -0.0440 0.9308 0.037 Uiso 1 1 calc R . . C129 C 0.44103(10) -0.00308(16) 0.87700(10) 0.0300(6) Uani 1 1 d U . . H12D H 0.4412 -0.0510 0.8587 0.036 Uiso 1 1 calc R . . C130 C 0.41370(9) 0.06247(15) 0.86097(9) 0.0254(5) Uani 1 1 d U . . H13A H 0.3949 0.0590 0.8317 0.030 Uiso 1 1 calc R . . C131 C 0.38290(9) 0.18627(15) 0.78200(8) 0.0229(5) Uani 1 1 d U . . H13B H 0.4095 0.1497 0.7818 0.027 Uiso 1 1 calc R . . C132 C 0.35906(9) 0.21632(15) 0.74201(9) 0.0253(5) Uani 1 1 d DU . . C133 C 0.19259(9) 0.45405(15) 0.81778(9) 0.0254(5) Uani 1 1 d DU . . C134 C 0.19894(9) 0.44829(15) 0.86522(9) 0.0230(5) Uani 1 1 d U . . H13C H 0.1796 0.4769 0.8858 0.028 Uiso 1 1 calc R . . C135 C 0.18124(9) 0.40921(15) 0.96745(9) 0.0248(5) Uani 1 1 d U . . H13D H 0.1629 0.4004 0.9383 0.030 Uiso 1 1 calc R . . C136 C 0.15746(10) 0.42813(17) 1.00665(10) 0.0297(6) Uani 1 1 d U . . H13E H 0.1230 0.4328 1.0045 0.036 Uiso 1 1 calc R . . C137 C 0.18405(10) 0.44041(17) 1.04940(10) 0.0314(6) Uani 1 1 d U . . H13F H 0.1677 0.4551 1.0763 0.038 Uiso 1 1 calc R . . C138 C 0.23378(10) 0.43151(16) 1.05319(9) 0.0266(5) Uani 1 1 d U . . H13G H 0.2513 0.4387 1.0829 0.032 Uiso 1 1 calc R . . C139 C 0.33848(10) 0.47932(16) 1.09130(9) 0.0266(5) Uani 1 1 d U . . H13H H 0.3090 0.5083 1.0937 0.032 Uiso 1 1 calc R . . C140 C 0.37859(11) 0.49176(16) 1.12037(9) 0.0295(6) Uani 1 1 d DU . . C141 C 0.59016(11) 0.2244(2) 1.07118(12) 0.0475(8) Uani 1 1 d DU . . H14A H 0.5991 0.1673 1.0664 0.057 Uiso 1 1 calc R . . H14B H 0.6110 0.2580 1.0522 0.057 Uiso 1 1 calc R . . C142 C 0.60149(14) 0.2448(3) 1.12158(15) 0.0627(11) Uani 1 1 d DU . . H14C H 0.5832 0.2080 1.1411 0.075 Uiso 1 1 calc R . . H14D H 0.5904 0.3006 1.1273 0.075 Uiso 1 1 calc R . . C143 C 0.65588(15) 0.2383(3) 1.13698(19) 0.0762(15) Uani 1 1 d DU . . H14E H 0.6738 0.2765 1.1180 0.091 Uiso 1 1 calc R . . H14F H 0.6609 0.2556 1.1702 0.091 Uiso 1 1 calc R . . C144 C 0.67755(16) 0.1559(3) 1.13257(19) 0.0777(14) Uani 1 1 d DU . . H14G H 0.7116 0.1567 1.1454 0.117 Uiso 1 1 calc R . . H14H H 0.6760 0.1403 1.0993 0.117 Uiso 1 1 calc R . . H14I H 0.6593 0.1169 1.1501 0.117 Uiso 1 1 calc R . . C145 C 0.37063(11) 0.20185(17) 0.69228(9) 0.0307(6) Uani 1 1 d DU . . H14J H 0.3415 0.1791 0.6745 0.037 Uiso 1 1 calc R . . H14K H 0.3969 0.1610 0.6922 0.037 Uiso 1 1 calc R . . C146 C 0.38656(10) 0.27740(17) 0.66694(9) 0.0289(5) Uani 1 1 d DU . . H14L H 0.3918 0.2633 0.6340 0.035 Uiso 1 1 calc R . . H14M H 0.3601 0.3179 0.6663 0.035 Uiso 1 1 calc R . . C147 C 0.43299(11) 0.3150(2) 0.68980(11) 0.0390(7) Uani 1 1 d DU . . H14N H 0.4274 0.3311 0.7224 0.047 Uiso 1 1 calc R . . H14O H 0.4591 0.2739 0.6915 0.047 Uiso 1 1 calc R . . C148 C 0.44983(16) 0.3882(3) 0.66360(14) 0.0650(12) Uani 1 1 d DU . . H14P H 0.4795 0.4100 0.6801 0.098 Uiso 1 1 calc R . . H14Q H 0.4243 0.4295 0.6621 0.098 Uiso 1 1 calc R . . H14R H 0.4566 0.3724 0.6316 0.098 Uiso 1 1 calc R . . C149 C 0.15808(10) 0.50776(17) 0.78874(10) 0.0317(6) Uani 1 1 d DU . . H14S H 0.1339 0.5302 0.8091 0.038 Uiso 1 1 calc R . . H14T H 0.1403 0.4749 0.7641 0.038 Uiso 1 1 calc R . . C150 C 0.18351(12) 0.57732(18) 0.76549(10) 0.0379(7) Uani 1 1 d DU . . H15A H 0.2079 0.5546 0.7454 0.046 Uiso 1 1 calc R . . H15B H 0.1591 0.6070 0.7448 0.046 Uiso 1 1 calc R . . C151 C 0.20882(15) 0.6366(2) 0.79970(13) 0.0523(9) Uani 1 1 d DU . . H15C H 0.2335 0.6074 0.8204 0.063 Uiso 1 1 calc R . . H15D H 0.1846 0.6599 0.8198 0.063 Uiso 1 1 calc R . . C152 C 0.23356(16) 0.7047(3) 0.77480(18) 0.0704(12) Uani 1 1 d DU . . H15E H 0.2470 0.7439 0.7981 0.106 Uiso 1 1 calc R . . H15F H 0.2097 0.7315 0.7528 0.106 Uiso 1 1 calc R . . H15G H 0.2599 0.6825 0.7575 0.106 Uiso 1 1 calc R . . C153 C 0.38631(12) 0.55450(18) 1.15822(9) 0.0354(6) Uani 1 1 d DU . . H15H H 0.3574 0.5901 1.1571 0.042 Uiso 1 1 calc R . . H15I H 0.4146 0.5882 1.1515 0.042 Uiso 1 1 calc R . . C154 C 0.3949(2) 0.5206(2) 1.20727(12) 0.0780(15) Uani 1 1 d DU . . H15J H 0.4261 0.4906 1.2101 0.094 Uiso 1 1 calc R . . H15K H 0.3684 0.4826 1.2135 0.094 Uiso 1 1 calc R . . C155 C 0.3968(3) 0.5966(5) 1.24710(17) 0.137(3) Uani 1 1 d DU . . H15L H 0.3743 0.6414 1.2375 0.164 Uiso 1 1 calc R . . H15M H 0.3908 0.5777 1.2791 0.164 Uiso 1 1 calc R . . C156 C 0.4427(3) 0.6154(5) 1.2430(2) 0.126(2) Uani 1 1 d DU . . H15N H 0.4532 0.6558 1.2668 0.188 Uiso 1 1 calc R . . H15O H 0.4463 0.6375 1.2116 0.188 Uiso 1 1 calc R . . H15P H 0.4628 0.5668 1.2477 0.188 Uiso 1 1 calc R . . C201 C -0.07905(8) 0.72042(13) 0.52362(8) 0.0181(4) Uani 1 1 d U . . C202 C -0.08876(8) 0.72665(13) 0.57214(8) 0.0176(4) Uani 1 1 d U . . C203 C -0.13727(8) 0.71216(13) 0.58562(8) 0.0176(4) Uani 1 1 d U . . C204 C -0.17569(8) 0.69461(13) 0.55014(8) 0.0178(4) Uani 1 1 d U . . C205 C -0.16798(8) 0.70835(14) 0.50138(8) 0.0182(4) Uani 1 1 d U . . C206 C -0.11895(8) 0.71931(13) 0.48810(8) 0.0185(4) Uani 1 1 d U . . C207 C -0.03044(8) 0.71862(14) 0.51081(8) 0.0192(4) Uani 1 1 d U . . C208 C 0.00738(8) 0.71971(14) 0.54767(8) 0.0205(4) Uani 1 1 d U . . C209 C -0.00184(8) 0.73259(14) 0.59481(8) 0.0200(4) Uani 1 1 d U . . C210 C -0.05078(8) 0.74162(14) 0.60701(8) 0.0188(4) Uani 1 1 d U . . C211 C -0.06407(9) 0.76636(14) 0.65310(8) 0.0204(4) Uani 1 1 d U . . C212 C -0.11102(9) 0.74895(14) 0.66679(8) 0.0209(4) Uani 1 1 d U . . C213 C -0.14619(8) 0.70999(14) 0.63340(8) 0.0194(4) Uani 1 1 d U . . C214 C -0.18923(8) 0.67032(15) 0.64636(8) 0.0206(4) Uani 1 1 d U . . C215 C -0.22532(8) 0.64870(14) 0.61127(8) 0.0199(4) Uani 1 1 d U . . C216 C -0.22100(8) 0.66589(14) 0.56311(8) 0.0195(4) Uani 1 1 d U . . C217 C -0.25789(8) 0.65174(15) 0.52648(8) 0.0216(5) Uani 1 1 d U . . C218 C -0.25256(8) 0.67328(15) 0.47952(8) 0.0223(5) Uani 1 1 d U . . C219 C -0.20725(9) 0.70634(15) 0.46706(8) 0.0212(4) Uani 1 1 d U . . C220 C -0.19936(9) 0.73614(15) 0.42043(8) 0.0227(5) Uani 1 1 d U . . C221 C -0.15138(9) 0.74460(15) 0.40698(8) 0.0237(5) Uani 1 1 d U . . C222 C -0.11048(9) 0.72450(14) 0.44023(8) 0.0207(4) Uani 1 1 d U . . C223 C -0.06179(9) 0.71294(14) 0.42726(8) 0.0213(4) Uani 1 1 d U . . C224 C -0.02323(9) 0.71112(14) 0.46205(8) 0.0207(4) Uani 1 1 d U . . C225 C 0.08268(9) 0.71356(16) 0.60166(9) 0.0262(5) Uani 1 1 d DU . . C226 C 0.04278(9) 0.72840(15) 0.62524(9) 0.0225(5) Uani 1 1 d U . . H22A H 0.0439 0.7354 0.6584 0.027 Uiso 1 1 calc R . . C227 C -0.03274(9) 0.81484(15) 0.68332(8) 0.0242(5) Uani 1 1 d U . . H22B H -0.0015 0.8289 0.6740 0.029 Uiso 1 1 calc R . . C228 C -0.04679(10) 0.84192(16) 0.72594(9) 0.0280(5) Uani 1 1 d U . . H22C H -0.0254 0.8747 0.7455 0.034 Uiso 1 1 calc R . . C229 C -0.09223(10) 0.82126(16) 0.74032(9) 0.0275(5) Uani 1 1 d U . . H22D H -0.1013 0.8382 0.7702 0.033 Uiso 1 1 calc R . . C230 C -0.12424(9) 0.77614(16) 0.71124(8) 0.0254(5) Uani 1 1 d U . . H23A H -0.1555 0.7632 0.7211 0.030 Uiso 1 1 calc R . . C231 C -0.20028(9) 0.64022(16) 0.69199(9) 0.0245(5) Uani 1 1 d U . . H23B H -0.1801 0.6489 0.7200 0.029 Uiso 1 1 calc R . . C232 C -0.24275(9) 0.59826(17) 0.69029(9) 0.0279(5) Uani 1 1 d DU . . C233 C -0.33006(9) 0.61289(17) 0.47424(9) 0.0281(5) Uani 1 1 d DU . . C234 C -0.29570(9) 0.64963(16) 0.44891(9) 0.0264(5) Uani 1 1 d U . . H23C H -0.2993 0.6586 0.4159 0.032 Uiso 1 1 calc R . . C235 C -0.23831(10) 0.76436(16) 0.38928(9) 0.0282(5) Uani 1 1 d U . . H23E H -0.2707 0.7612 0.3985 0.034 Uiso 1 1 calc R . . C236 C -0.23012(11) 0.79621(18) 0.34598(9) 0.0345(6) Uani 1 1 d U . . H23F H -0.2568 0.8124 0.3250 0.041 Uiso 1 1 calc R . . C237 C -0.18258(12) 0.80473(19) 0.33292(9) 0.0369(7) Uani 1 1 d U . . H23G H -0.1769 0.8273 0.3032 0.044 Uiso 1 1 calc R . . C238 C -0.14421(11) 0.78050(17) 0.36303(9) 0.0309(6) Uani 1 1 d U . . H23H H -0.1120 0.7880 0.3542 0.037 Uiso 1 1 calc R . . C239 C -0.04489(9) 0.69822(15) 0.38097(9) 0.0238(5) Uani 1 1 d U . . H23I H -0.0659 0.6958 0.3530 0.029 Uiso 1 1 calc R . . C240 C 0.00429(10) 0.68835(15) 0.38213(9) 0.0259(5) Uani 1 1 d DU . . C241 C 0.13453(10) 0.70352(18) 0.62116(11) 0.0350(6) Uani 1 1 d DU . . H24A H 0.1478 0.6534 0.6081 0.042 Uiso 1 1 calc R . . H24B H 0.1350 0.6968 0.6557 0.042 Uiso 1 1 calc R . . C242 C 0.16732(11) 0.7733(2) 0.61058(15) 0.0519(9) Uani 1 1 d DU . . H24C H 0.1572 0.8217 0.6277 0.062 Uiso 1 1 calc R . . H24D H 0.1631 0.7854 0.5765 0.062 Uiso 1 1 calc R . . C243 C 0.22092(12) 0.7568(3) 0.62413(19) 0.0733(14) Uani 1 1 d DU . . H24E H 0.2390 0.8086 0.6257 0.088 Uiso 1 1 calc R . . H24F H 0.2244 0.7316 0.6557 0.088 Uiso 1 1 calc R . . C244 C 0.24273(19) 0.7011(3) 0.5888(2) 0.0932(18) Uani 1 1 d DU . . H24G H 0.2783 0.7026 0.5936 0.140 Uiso 1 1 calc R . . H24H H 0.2326 0.7192 0.5568 0.140 Uiso 1 1 calc R . . H24I H 0.2313 0.6458 0.5932 0.140 Uiso 1 1 calc R . . C245 C -0.26321(11) 0.5521(2) 0.73003(11) 0.0403(7) Uani 1 1 d DU . . H24J H -0.2975 0.5372 0.7212 0.048 Uiso 1 1 calc R . . H24K H -0.2624 0.5866 0.7585 0.048 Uiso 1 1 calc R . . C246 C -0.23195(16) 0.4732(2) 0.74086(12) 0.0541(9) Uani 1 1 d DU . . H24L H -0.2349 0.4376 0.7129 0.065 Uiso 1 1 calc R . . H24M H -0.1973 0.4886 0.7465 0.065 Uiso 1 1 calc R . . C247 C -0.24699(19) 0.4263(2) 0.78287(14) 0.0649(11) Uani 1 1 d DU . . H24N H -0.2813 0.4093 0.7767 0.078 Uiso 1 1 calc R . . H24O H -0.2269 0.3768 0.7865 0.078 Uiso 1 1 calc R . . C248 C -0.2420(2) 0.4728(3) 0.82820(14) 0.0713(13) Uani 1 1 d DU . . H24P H -0.2437 0.4354 0.8547 0.107 Uiso 1 1 calc R . . H24Q H -0.2685 0.5123 0.8286 0.107 Uiso 1 1 calc R . . H24R H -0.2107 0.5010 0.8309 0.107 Uiso 1 1 calc R . . C249 C -0.37775(10) 0.5772(2) 0.45549(10) 0.0391(7) Uani 1 1 d DU . . H24S H -0.3966 0.6187 0.4369 0.047 Uiso 1 1 calc R . . H24T H -0.3967 0.5617 0.4822 0.047 Uiso 1 1 calc R . . C250 C -0.37134(14) 0.5041(2) 0.42506(14) 0.0585(10) Uani 1 1 d DU . . H25A H -0.3570 0.5217 0.3960 0.070 Uiso 1 1 calc R . . H25B H -0.4038 0.4810 0.4159 0.070 Uiso 1 1 calc R . . C251 C -0.33895(16) 0.4372(2) 0.44846(15) 0.0617(10) Uani 1 1 d DU . . H25C H -0.3363 0.3928 0.4256 0.074 Uiso 1 1 calc R . . H25D H -0.3059 0.4594 0.4558 0.074 Uiso 1 1 calc R . . C252 C -0.3562(2) 0.4039(3) 0.49125(17) 0.0846(15) Uani 1 1 d DU . . H25E H -0.3381 0.3544 0.4998 0.127 Uiso 1 1 calc R . . H25F H -0.3909 0.3914 0.4861 0.127 Uiso 1 1 calc R . . H25G H -0.3511 0.4434 0.5167 0.127 Uiso 1 1 calc R . . C253 C 0.03362(10) 0.67203(18) 0.34080(9) 0.0320(6) Uani 1 1 d DU . . H25H H 0.0383 0.6129 0.3382 0.038 Uiso 1 1 calc R . . H25I H 0.0146 0.6901 0.3119 0.038 Uiso 1 1 calc R . . C254 C 0.08152(16) 0.7113(3) 0.34295(15) 0.0733(14) Uani 1 1 d DU . . H25J H 0.0999 0.6958 0.3728 0.088 Uiso 1 1 calc R . . H25K H 0.0768 0.7706 0.3436 0.088 Uiso 1 1 calc R . . C255 C 0.11392(16) 0.6892(3) 0.29984(14) 0.0648(11) Uani 1 1 d DU . . H25L H 0.1483 0.7052 0.3069 0.078 Uiso 1 1 calc R . . H25M H 0.1125 0.6306 0.2927 0.078 Uiso 1 1 calc R . . C256 C 0.09153(16) 0.7355(3) 0.26177(18) 0.0765(13) Uani 1 1 d DU . . H25N H 0.1084 0.7254 0.2333 0.115 Uiso 1 1 calc R . . H25O H 0.0936 0.7931 0.2696 0.115 Uiso 1 1 calc R . . H25P H 0.0573 0.7198 0.2563 0.115 Uiso 1 1 calc R . . C302 C 0.05241(9) 0.49804(13) 0.50831(8) 0.0183(4) Uani 1 1 d U . . C303 C 0.03012(9) 0.49329(13) 0.46091(8) 0.0186(4) Uani 1 1 d U . . C304 C -0.02197(8) 0.49616(13) 0.45284(7) 0.0184(4) Uani 1 1 d U . . C308 C 0.09473(9) 0.49321(14) 0.60046(8) 0.0212(5) Uani 1 1 d U . . C309 C 0.12470(9) 0.48710(14) 0.56335(8) 0.0203(4) Uani 1 1 d U . . C310 C 0.10343(9) 0.49743(14) 0.51612(8) 0.0189(4) Uani 1 1 d U . . C311 C 0.13282(9) 0.51171(14) 0.47705(8) 0.0206(4) Uani 1 1 d U . . C312 C 0.11104(9) 0.50407(14) 0.43029(8) 0.0205(4) Uani 1 1 d U . . C313 C 0.05964(9) 0.48592(14) 0.42283(8) 0.0198(4) Uani 1 1 d U . . C314 C 0.03663(9) 0.46767(14) 0.37722(8) 0.0214(5) Uani 1 1 d U . . C315 C -0.01368(9) 0.47569(14) 0.36956(8) 0.0211(4) Uani 1 1 d U . . C316 C -0.04393(9) 0.49332(14) 0.40629(8) 0.0201(4) Uani 1 1 d U . . C325 C 0.18062(9) 0.46029(15) 0.62750(9) 0.0248(5) Uani 1 1 d DU . . C326 C 0.17405(9) 0.46697(15) 0.57983(9) 0.0239(5) Uani 1 1 d U . . H32A H 0.1994 0.4592 0.5595 0.029 Uiso 1 1 calc R . . C327 C 0.18112(9) 0.54034(15) 0.48345(9) 0.0252(5) Uani 1 1 d U . . H32B H 0.1955 0.5475 0.5145 0.030 Uiso 1 1 calc R . . C328 C 0.20813(10) 0.55821(16) 0.44611(10) 0.0288(5) Uani 1 1 d U . . H32C H 0.2409 0.5760 0.4515 0.035 Uiso 1 1 calc R . . C329 C 0.18708(10) 0.55008(16) 0.40036(9) 0.0282(5) Uani 1 1 d U . . H32D H 0.2055 0.5620 0.3744 0.034 Uiso 1 1 calc R . . C330 C 0.13959(9) 0.52477(15) 0.39283(9) 0.0251(5) Uani 1 1 d U . . H33A H 0.1254 0.5210 0.3615 0.030 Uiso 1 1 calc R . . C331 C 0.05767(10) 0.43845(15) 0.33545(8) 0.0249(5) Uani 1 1 d U . . H33B H 0.0914 0.4273 0.3344 0.030 Uiso 1 1 calc R . . C332 C 0.02475(10) 0.42851(16) 0.29801(8) 0.0259(5) Uani 1 1 d DU . . C341 C 0.22739(10) 0.44375(17) 0.65683(9) 0.0305(6) Uani 1 1 d DU . . H34C H 0.2448 0.3987 0.6425 0.037 Uiso 1 1 calc R . . H34D H 0.2197 0.4266 0.6887 0.037 Uiso 1 1 calc R . . C342 C 0.26030(10) 0.51686(19) 0.66090(10) 0.0338(6) Uani 1 1 d DU . . H34E H 0.2415 0.5632 0.6719 0.041 Uiso 1 1 calc R . . H34F H 0.2703 0.5305 0.6292 0.041 Uiso 1 1 calc R . . C343 C 0.30595(11) 0.5062(2) 0.69409(11) 0.0411(7) Uani 1 1 d DU . . H34G H 0.2962 0.4919 0.7257 0.049 Uiso 1 1 calc R . . H34H H 0.3253 0.4608 0.6828 0.049 Uiso 1 1 calc R . . C344 C 0.33732(13) 0.5807(3) 0.69787(13) 0.0552(10) Uani 1 1 d DU . . H34I H 0.3659 0.5705 0.7197 0.083 Uiso 1 1 calc R . . H34J H 0.3186 0.6258 0.7095 0.083 Uiso 1 1 calc R . . H34K H 0.3479 0.5943 0.6668 0.083 Uiso 1 1 calc R . . C345 C 0.03274(11) 0.39322(17) 0.25047(9) 0.0321(6) Uani 1 1 d DU . . H34A H 0.0411 0.3353 0.2545 0.038 Uiso 1 1 calc R . . H34B H 0.0018 0.3965 0.2304 0.038 Uiso 1 1 calc R . . C346 C 0.07205(11) 0.43387(19) 0.22526(10) 0.0365(6) Uani 1 1 d DU . . H34L H 0.0789 0.4008 0.1976 0.044 Uiso 1 1 calc R . . H34M H 0.1022 0.4358 0.2465 0.044 Uiso 1 1 calc R . . C347 C 0.05934(11) 0.51900(19) 0.20883(10) 0.0357(6) Uani 1 1 d DU . . H34N H 0.0547 0.5530 0.2367 0.043 Uiso 1 1 calc R . . H34O H 0.0280 0.5176 0.1893 0.043 Uiso 1 1 calc R . . C348 C 0.09773(13) 0.5582(3) 0.18045(13) 0.0534(9) Uani 1 1 d DU . . H34P H 0.0867 0.6121 0.1702 0.080 Uiso 1 1 calc R . . H34Q H 0.1027 0.5248 0.1529 0.080 Uiso 1 1 calc R . . H34R H 0.1284 0.5628 0.2001 0.080 Uiso 1 1 calc R . . C402 C 0.45341(8) 0.51199(13) 0.97452(8) 0.0168(4) Uani 1 1 d U . . C403 C 0.48769(8) 0.45557(13) 0.95703(8) 0.0168(4) Uani 1 1 d U . . C404 C 0.53401(8) 0.44350(13) 0.98294(8) 0.0170(4) Uani 1 1 d U . . C408 C 0.38448(8) 0.61327(14) 1.01163(8) 0.0202(4) Uani 1 1 d U . . C409 C 0.37084(8) 0.56646(14) 0.97216(8) 0.0195(4) Uani 1 1 d U . . C410 C 0.40735(8) 0.52233(13) 0.95000(8) 0.0189(4) Uani 1 1 d U . . C411 C 0.39960(8) 0.49253(14) 0.90232(8) 0.0192(4) Uani 1 1 d U . . C412 C 0.43368(8) 0.43837(14) 0.88457(8) 0.0190(4) Uani 1 1 d U . . C413 C 0.47546(8) 0.41245(14) 0.91516(8) 0.0182(4) Uani 1 1 d U . . C414 C 0.50597(8) 0.34644(14) 0.90352(8) 0.0190(4) Uani 1 1 d U . . C415 C 0.55138(8) 0.33660(14) 0.92828(8) 0.0187(4) Uani 1 1 d U . . C416 C 0.56757(8) 0.38735(14) 0.96635(8) 0.0185(4) Uani 1 1 d U . . C425 C 0.29519(8) 0.61794(15) 0.98970(9) 0.0243(5) Uani 1 1 d DU . . C426 C 0.31884(8) 0.56863(15) 0.96126(9) 0.0234(5) Uani 1 1 d U . . H42A H 0.3027 0.5383 0.9364 0.028 Uiso 1 1 calc R . . C427 C 0.36185(9) 0.52302(15) 0.87057(9) 0.0247(5) Uani 1 1 d U . . H42B H 0.3396 0.5611 0.8816 0.030 Uiso 1 1 calc R . . C428 C 0.35651(10) 0.49911(16) 0.82434(9) 0.0275(5) Uani 1 1 d U . . H42C H 0.3301 0.5190 0.8042 0.033 Uiso 1 1 calc R . . C429 C 0.38977(10) 0.44590(16) 0.80699(9) 0.0272(5) Uani 1 1 d U . . H42D H 0.3862 0.4292 0.7750 0.033 Uiso 1 1 calc R . . C430 C 0.42812(9) 0.41732(15) 0.83642(9) 0.0240(5) Uani 1 1 d U . . H43A H 0.4514 0.3826 0.8240 0.029 Uiso 1 1 calc R . . C431 C 0.49649(9) 0.28205(14) 0.87014(8) 0.0217(5) Uani 1 1 d U . . H43B H 0.4671 0.2779 0.8506 0.026 Uiso 1 1 calc R . . C432 C 0.53336(9) 0.22771(15) 0.86907(8) 0.0227(5) Uani 1 1 d DU . . C441 C 0.24137(9) 0.63324(17) 0.98829(10) 0.0286(5) Uani 1 1 d DU . . H44A H 0.2322 0.6429 1.0207 0.034 Uiso 1 1 calc R . . H44B H 0.2239 0.5844 0.9762 0.034 Uiso 1 1 calc R . . C442 C 0.22532(10) 0.70497(19) 0.95775(14) 0.0449(8) Uani 1 1 d DU . . H44C H 0.2336 0.6945 0.9251 0.054 Uiso 1 1 calc R . . H44D H 0.2436 0.7534 0.9693 0.054 Uiso 1 1 calc R . . C443 C 0.17073(10) 0.72242(19) 0.95741(15) 0.0476(9) Uani 1 1 d DU . . H44E H 0.1629 0.7358 0.9898 0.057 Uiso 1 1 calc R . . H44F H 0.1630 0.7704 0.9375 0.057 Uiso 1 1 calc R . . C444 C 0.13927(11) 0.6540(2) 0.93977(13) 0.0453(8) Uani 1 1 d DU . . H44G H 0.1051 0.6713 0.9373 0.068 Uiso 1 1 calc R . . H44H H 0.1434 0.6085 0.9617 0.068 Uiso 1 1 calc R . . H44I H 0.1486 0.6373 0.9087 0.068 Uiso 1 1 calc R . . C445 C 0.53441(9) 0.15270(16) 0.83961(9) 0.0278(5) Uani 1 1 d DU . . H44J H 0.5060 0.1186 0.8457 0.033 Uiso 1 1 calc R . . H44K H 0.5642 0.1216 0.8494 0.033 Uiso 1 1 calc R . . C446 C 0.53346(11) 0.16950(19) 0.78744(10) 0.0372(7) Uani 1 1 d DU . . H44L H 0.5648 0.1944 0.7805 0.045 Uiso 1 1 calc R . . H44M H 0.5073 0.2091 0.7788 0.045 Uiso 1 1 calc R . . C447 C 0.52505(13) 0.0943(2) 0.75695(12) 0.0533(10) Uani 1 1 d DU . . H44N H 0.5497 0.0530 0.7671 0.064 Uiso 1 1 calc R . . H44O H 0.4926 0.0717 0.7619 0.064 Uiso 1 1 calc R . . C448 C 0.5280(2) 0.1112(3) 0.70542(13) 0.093(2) Uani 1 1 d DU . . H44P H 0.5208 0.0617 0.6874 0.139 Uiso 1 1 calc R . . H44Q H 0.5608 0.1301 0.7000 0.139 Uiso 1 1 calc R . . H44R H 0.5042 0.1530 0.6954 0.139 Uiso 1 1 calc R . . C993 C 0.03131(13) 1.0512(2) 0.57900(14) 0.0501(8) Uani 1 1 d U . . H99A H 0.0603 1.0771 0.5710 0.060 Uiso 1 1 calc R . . C994 C 0.00043(13) 1.0911(2) 0.60714(14) 0.0484(8) Uani 1 1 d U . . H99B H 0.0082 1.1441 0.6180 0.058 Uiso 1 1 calc R . . C995 C -0.04192(13) 1.0538(2) 0.61959(13) 0.0464(8) Uani 1 1 d U . . H99C H -0.0629 1.0808 0.6394 0.056 Uiso 1 1 calc R . . C996 C -0.05331(12) 0.9771(2) 0.60286(13) 0.0458(8) Uani 1 1 d U . . H99D H -0.0823 0.9512 0.6109 0.055 Uiso 1 1 calc R . . C997 C -0.02230(13) 0.93836(19) 0.57444(13) 0.0463(8) Uani 1 1 d U . . H99E H -0.0306 0.8859 0.5629 0.056 Uiso 1 1 calc R . . C998 C 0.02065(13) 0.9738(2) 0.56226(14) 0.0489(8) Uani 1 1 d U . . C999 C 0.05459(17) 0.9294(2) 0.53230(18) 0.0695(13) Uani 1 1 d U . . H99F H 0.0627 0.9640 0.5062 0.104 Uiso 1 1 calc R . . H99G H 0.0387 0.8800 0.5199 0.104 Uiso 1 1 calc R . . H99H H 0.0844 0.9151 0.5514 0.104 Uiso 1 1 calc 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 S101 0.0334(3) 0.0322(3) 0.0174(3) 0.0027(2) -0.0013(2) -0.0037(3) S102 0.0275(3) 0.0354(4) 0.0280(3) 0.0064(3) -0.0087(3) 0.0000(3) S103 0.0264(3) 0.0266(3) 0.0184(3) -0.0013(2) 0.0000(2) 0.0033(2) S104 0.0220(3) 0.0276(3) 0.0202(3) 0.0014(2) -0.0024(2) 0.0038(2) S201 0.0248(3) 0.0261(3) 0.0241(3) -0.0019(2) 0.0060(2) -0.0031(2) S202 0.0186(3) 0.0271(3) 0.0298(3) -0.0015(2) 0.0017(2) -0.0019(2) S203 0.0178(3) 0.0318(3) 0.0256(3) 0.0003(2) 0.0025(2) 0.0013(2) S204 0.0184(3) 0.0393(4) 0.0252(3) -0.0099(3) 0.0006(2) -0.0004(2) S302 0.0270(3) 0.0341(3) 0.0157(3) 0.0002(2) -0.0019(2) -0.0042(3) S303 0.0334(3) 0.0294(3) 0.0138(2) -0.0018(2) 0.0006(2) -0.0008(3) S402 0.0169(3) 0.0250(3) 0.0292(3) -0.0008(2) 0.0004(2) 0.0036(2) S403 0.0212(3) 0.0230(3) 0.0248(3) -0.0024(2) 0.0011(2) 0.0032(2) C101 0.0193(10) 0.0185(10) 0.0193(10) 0.0047(8) 0.0018(8) -0.0012(8) C102 0.0154(10) 0.0203(11) 0.0193(10) 0.0048(8) 0.0017(8) 0.0003(8) C103 0.0152(10) 0.0175(10) 0.0194(10) 0.0034(8) 0.0017(8) -0.0008(8) C104 0.0156(10) 0.0166(10) 0.0197(10) 0.0018(8) 0.0014(8) 0.0001(8) C105 0.0182(10) 0.0174(10) 0.0183(10) 0.0026(8) 0.0015(8) 0.0003(8) C106 0.0187(10) 0.0186(11) 0.0200(10) 0.0045(8) 0.0020(8) 0.0005(8) C107 0.0222(11) 0.0225(11) 0.0184(10) 0.0058(9) 0.0007(8) -0.0020(9) C108 0.0211(11) 0.0269(12) 0.0183(10) 0.0073(9) -0.0023(8) -0.0015(9) C109 0.0193(11) 0.0243(12) 0.0240(11) 0.0085(9) 0.0008(9) 0.0006(9) C110 0.0177(10) 0.0202(11) 0.0222(11) 0.0070(8) 0.0024(8) 0.0017(8) C111 0.0193(11) 0.0237(11) 0.0230(11) 0.0051(9) 0.0047(9) 0.0034(9) C112 0.0168(10) 0.0211(11) 0.0254(11) 0.0049(9) 0.0057(9) 0.0017(8) C113 0.0153(10) 0.0205(11) 0.0215(10) 0.0021(8) 0.0028(8) -0.0006(8) C114 0.0183(10) 0.0200(11) 0.0206(10) -0.0002(8) 0.0019(8) -0.0003(8) C115 0.0191(10) 0.0192(11) 0.0185(10) 0.0001(8) 0.0009(8) -0.0014(8) C116 0.0159(10) 0.0183(10) 0.0191(10) 0.0011(8) 0.0008(8) -0.0005(8) C117 0.0163(10) 0.0218(11) 0.0182(10) 0.0025(8) -0.0008(8) -0.0006(8) C118 0.0165(10) 0.0199(11) 0.0222(11) 0.0029(9) -0.0007(8) 0.0013(8) C119 0.0187(10) 0.0176(10) 0.0211(10) 0.0011(8) 0.0028(8) 0.0008(8) C120 0.0214(11) 0.0182(11) 0.0231(11) 0.0033(9) 0.0055(9) 0.0033(9) C121 0.0257(11) 0.0194(11) 0.0214(11) 0.0037(9) 0.0051(9) 0.0030(9) C122 0.0244(11) 0.0211(11) 0.0183(10) 0.0046(8) 0.0025(8) 0.0025(9) C123 0.0279(12) 0.0235(11) 0.0155(10) 0.0043(9) 0.0036(9) 0.0013(9) C124 0.0276(12) 0.0240(12) 0.0155(10) 0.0067(9) -0.0012(9) -0.0026(9) C125 0.0255(13) 0.0380(15) 0.0363(15) 0.0140(12) -0.0052(11) 0.0042(11) C126 0.0224(12) 0.0308(13) 0.0297(13) 0.0088(10) 0.0004(10) 0.0047(10) C127 0.0239(12) 0.0287(13) 0.0285(12) 0.0079(10) 0.0057(10) 0.0078(10) C128 0.0306(13) 0.0268(13) 0.0369(14) 0.0096(11) 0.0094(11) 0.0116(11) C129 0.0310(13) 0.0218(12) 0.0382(14) -0.0002(11) 0.0094(11) 0.0046(10) C130 0.0231(12) 0.0236(12) 0.0299(13) -0.0002(10) 0.0054(10) 0.0018(9) C131 0.0225(11) 0.0230(11) 0.0235(11) -0.0010(9) 0.0036(9) 0.0010(9) C132 0.0282(12) 0.0247(12) 0.0234(11) -0.0038(9) 0.0041(10) -0.0004(10) C133 0.0231(12) 0.0257(12) 0.0268(12) 0.0016(10) -0.0015(9) 0.0049(9) C134 0.0193(11) 0.0235(12) 0.0257(12) 0.0015(9) -0.0007(9) 0.0047(9) C135 0.0225(11) 0.0233(12) 0.0291(12) 0.0044(10) 0.0055(9) 0.0032(9) C136 0.0248(12) 0.0295(13) 0.0360(14) 0.0042(11) 0.0097(10) 0.0061(10) C137 0.0340(14) 0.0328(14) 0.0294(13) 0.0042(11) 0.0147(11) 0.0081(11) C138 0.0334(13) 0.0257(12) 0.0214(11) 0.0038(9) 0.0067(10) 0.0048(10) C139 0.0345(13) 0.0248(12) 0.0204(11) 0.0020(9) 0.0024(10) 0.0018(10) C140 0.0427(15) 0.0276(13) 0.0184(11) 0.0012(9) 0.0045(10) -0.0008(11) C141 0.0270(14) 0.056(2) 0.057(2) 0.0189(17) -0.0135(14) 0.0029(14) C142 0.045(2) 0.064(2) 0.073(3) -0.009(2) -0.0331(19) 0.0077(18) C143 0.048(2) 0.069(3) 0.104(4) -0.013(3) -0.046(2) 0.011(2) C144 0.053(2) 0.071(3) 0.102(4) 0.002(3) -0.038(2) 0.016(2) C145 0.0369(15) 0.0340(14) 0.0218(12) -0.0050(10) 0.0066(10) 0.0025(11) C146 0.0301(13) 0.0358(14) 0.0208(11) -0.0010(10) 0.0024(10) 0.0011(11) C147 0.0307(14) 0.0537(19) 0.0321(15) 0.0032(13) -0.0006(12) -0.0016(13) C148 0.062(2) 0.081(3) 0.052(2) 0.009(2) 0.0056(19) -0.035(2) C149 0.0293(13) 0.0364(15) 0.0280(13) 0.0024(11) -0.0066(10) 0.0107(11) C150 0.0453(17) 0.0362(15) 0.0314(14) 0.0035(12) -0.0029(12) 0.0122(13) C151 0.065(2) 0.0364(17) 0.053(2) 0.0058(15) -0.0114(17) 0.0015(16) C152 0.055(2) 0.056(2) 0.100(4) 0.008(2) 0.003(2) -0.0069(19) C153 0.0531(18) 0.0324(14) 0.0207(12) -0.0012(10) 0.0029(12) -0.0030(13) C154 0.158(5) 0.047(2) 0.0260(16) 0.0043(15) -0.011(2) -0.007(3) C155 0.155(6) 0.217(7) 0.036(2) 0.031(3) -0.019(3) -0.083(6) C156 0.139(6) 0.148(6) 0.087(4) 0.013(4) -0.011(4) 0.033(5) C201 0.0201(10) 0.0156(10) 0.0186(10) -0.0007(8) 0.0009(8) -0.0004(8) C202 0.0189(10) 0.0166(10) 0.0171(10) 0.0004(8) -0.0006(8) 0.0003(8) C203 0.0191(10) 0.0166(10) 0.0167(10) -0.0019(8) -0.0013(8) 0.0013(8) C204 0.0176(10) 0.0175(10) 0.0178(10) -0.0027(8) -0.0006(8) 0.0018(8) C205 0.0187(10) 0.0184(10) 0.0173(10) -0.0028(8) -0.0009(8) 0.0013(8) C206 0.0205(10) 0.0166(10) 0.0183(10) -0.0027(8) 0.0004(8) -0.0013(8) C207 0.0202(10) 0.0167(10) 0.0207(10) -0.0017(8) 0.0013(8) -0.0022(8) C208 0.0166(10) 0.0209(11) 0.0239(11) -0.0003(9) 0.0009(8) -0.0002(8) C209 0.0188(10) 0.0186(11) 0.0220(11) 0.0011(8) -0.0017(8) -0.0032(8) C210 0.0200(10) 0.0176(10) 0.0186(10) -0.0003(8) -0.0002(8) -0.0011(8) C211 0.0218(11) 0.0196(11) 0.0190(10) 0.0006(8) -0.0030(8) 0.0000(8) C212 0.0226(11) 0.0209(11) 0.0184(10) -0.0021(8) -0.0027(8) 0.0025(9) C213 0.0181(10) 0.0214(11) 0.0184(10) -0.0014(8) 0.0001(8) 0.0035(8) C214 0.0178(10) 0.0240(11) 0.0200(10) -0.0021(9) 0.0011(8) 0.0052(9) C215 0.0161(10) 0.0225(11) 0.0213(10) -0.0006(9) 0.0022(8) 0.0032(8) C216 0.0169(10) 0.0207(11) 0.0209(10) -0.0043(9) 0.0006(8) 0.0029(8) C217 0.0158(10) 0.0241(12) 0.0247(11) -0.0074(9) -0.0002(8) 0.0026(9) C218 0.0191(10) 0.0266(12) 0.0205(11) -0.0072(9) -0.0026(8) 0.0035(9) C219 0.0211(11) 0.0231(11) 0.0190(10) -0.0047(9) -0.0010(8) 0.0014(9) C220 0.0272(12) 0.0216(11) 0.0184(10) -0.0037(9) -0.0047(9) 0.0011(9) C221 0.0291(12) 0.0231(12) 0.0185(11) -0.0025(9) -0.0018(9) 0.0001(10) C222 0.0238(11) 0.0192(11) 0.0188(10) -0.0017(8) 0.0013(8) -0.0022(9) C223 0.0256(11) 0.0183(11) 0.0201(10) -0.0026(8) 0.0029(9) -0.0045(9) C224 0.0223(11) 0.0184(11) 0.0219(11) -0.0001(9) 0.0044(9) -0.0030(9) C225 0.0210(11) 0.0247(12) 0.0321(13) 0.0015(10) -0.0032(10) -0.0038(9) C226 0.0201(11) 0.0236(12) 0.0232(11) 0.0009(9) -0.0019(9) -0.0017(9) C227 0.0241(12) 0.0264(12) 0.0210(11) -0.0012(9) -0.0052(9) -0.0022(9) C228 0.0331(13) 0.0278(13) 0.0217(11) -0.0054(10) -0.0067(10) -0.0002(10) C229 0.0325(13) 0.0312(13) 0.0181(11) -0.0059(10) -0.0027(10) 0.0064(11) C230 0.0242(12) 0.0316(13) 0.0200(11) -0.0031(10) -0.0007(9) 0.0057(10) C231 0.0184(11) 0.0315(13) 0.0237(11) 0.0031(10) 0.0027(9) 0.0037(9) C232 0.0233(12) 0.0384(15) 0.0222(12) 0.0030(10) 0.0034(9) 0.0052(10) C233 0.0184(11) 0.0425(15) 0.0227(12) -0.0119(11) -0.0016(9) 0.0005(10) C234 0.0162(10) 0.0329(13) 0.0303(13) -0.0132(10) 0.0036(9) -0.0021(9) C235 0.0314(13) 0.0283(13) 0.0234(12) -0.0042(10) -0.0078(10) 0.0011(10) C236 0.0442(16) 0.0352(15) 0.0219(12) -0.0009(11) -0.0123(11) 0.0045(12) C237 0.0490(17) 0.0419(16) 0.0187(12) 0.0035(11) -0.0038(11) 0.0010(13) C238 0.0377(15) 0.0342(14) 0.0206(12) 0.0018(10) 0.0001(10) -0.0002(12) C239 0.0265(12) 0.0237(12) 0.0218(11) -0.0045(9) 0.0053(9) -0.0068(9) C240 0.0316(13) 0.0244(12) 0.0226(11) -0.0045(9) 0.0073(10) -0.0094(10) C241 0.0218(12) 0.0364(15) 0.0451(16) 0.0006(13) -0.0081(11) 0.0018(11) C242 0.0247(14) 0.062(2) 0.069(2) -0.0067(19) 0.0001(15) -0.0080(14) C243 0.0265(17) 0.080(3) 0.112(4) -0.032(3) -0.007(2) -0.0060(18) C244 0.067(3) 0.101(4) 0.115(4) 0.030(3) 0.028(3) 0.030(3) C245 0.0295(14) 0.061(2) 0.0310(14) 0.0130(14) 0.0051(11) -0.0032(13) C246 0.075(3) 0.054(2) 0.0349(17) 0.0038(15) 0.0145(17) -0.0049(19) C247 0.093(3) 0.049(2) 0.055(2) 0.0058(18) 0.020(2) -0.001(2) C248 0.108(4) 0.063(3) 0.046(2) 0.0073(19) 0.027(2) 0.015(3) C249 0.0207(12) 0.065(2) 0.0311(14) -0.0158(14) -0.0006(11) -0.0048(13) C250 0.047(2) 0.073(3) 0.055(2) -0.0202(19) 0.0017(17) -0.0136(18) C251 0.067(3) 0.049(2) 0.071(3) -0.0180(19) 0.018(2) -0.0143(18) C252 0.106(4) 0.075(3) 0.072(3) -0.013(2) 0.003(3) -0.042(3) C253 0.0379(15) 0.0342(14) 0.0257(12) -0.0055(11) 0.0138(11) -0.0083(12) C254 0.074(3) 0.086(3) 0.066(3) -0.039(2) 0.040(2) -0.039(2) C255 0.070(3) 0.067(3) 0.054(2) 0.0100(19) -0.0137(19) -0.028(2) C256 0.048(2) 0.077(3) 0.101(3) -0.014(3) -0.016(2) 0.005(2) C302 0.0252(11) 0.0155(10) 0.0145(9) -0.0004(8) 0.0025(8) -0.0008(8) C303 0.0256(11) 0.0161(10) 0.0143(9) -0.0005(8) 0.0020(8) -0.0014(8) C304 0.0245(11) 0.0170(10) 0.0136(9) -0.0012(8) 0.0020(8) -0.0017(8) C308 0.0267(12) 0.0217(11) 0.0145(10) -0.0014(8) -0.0027(8) -0.0038(9) C309 0.0237(11) 0.0189(11) 0.0181(10) -0.0017(8) -0.0007(8) -0.0028(9) C310 0.0237(11) 0.0171(10) 0.0159(10) -0.0006(8) 0.0021(8) -0.0008(8) C311 0.0258(11) 0.0173(10) 0.0189(10) -0.0007(8) 0.0039(9) 0.0016(9) C312 0.0270(11) 0.0172(10) 0.0179(10) 0.0001(8) 0.0048(9) 0.0041(9) C313 0.0256(11) 0.0179(10) 0.0161(10) 0.0006(8) 0.0032(8) 0.0029(9) C314 0.0316(12) 0.0187(11) 0.0141(10) 0.0007(8) 0.0024(9) 0.0012(9) C315 0.0294(12) 0.0207(11) 0.0130(9) -0.0002(8) -0.0001(8) -0.0016(9) C316 0.0268(11) 0.0194(11) 0.0143(10) 0.0003(8) 0.0021(8) -0.0043(9) C325 0.0278(12) 0.0252(12) 0.0208(11) 0.0003(9) -0.0018(9) -0.0032(10) C326 0.0266(12) 0.0236(12) 0.0212(11) -0.0020(9) -0.0003(9) -0.0016(9) C327 0.0262(12) 0.0233(12) 0.0261(12) -0.0007(10) 0.0030(10) -0.0002(10) C328 0.0253(12) 0.0283(13) 0.0335(14) 0.0014(11) 0.0063(10) -0.0007(10) C329 0.0279(12) 0.0309(13) 0.0273(12) 0.0038(10) 0.0115(10) 0.0041(10) C330 0.0279(12) 0.0271(12) 0.0210(11) 0.0015(9) 0.0067(9) 0.0061(10) C331 0.0348(13) 0.0242(12) 0.0160(10) 0.0003(9) 0.0041(9) 0.0075(10) C332 0.0356(14) 0.0248(12) 0.0178(11) -0.0008(9) 0.0043(10) 0.0048(10) C341 0.0308(13) 0.0361(15) 0.0236(12) -0.0016(11) -0.0049(10) 0.0020(11) C342 0.0295(14) 0.0434(16) 0.0276(13) 0.0054(12) -0.0031(11) -0.0048(12) C343 0.0276(14) 0.063(2) 0.0317(15) 0.0066(14) -0.0057(11) -0.0071(14) C344 0.0377(18) 0.078(3) 0.048(2) 0.0079(19) -0.0057(15) -0.0207(18) C345 0.0488(17) 0.0318(14) 0.0156(11) -0.0029(10) 0.0022(11) 0.0100(12) C346 0.0387(15) 0.0479(17) 0.0230(13) -0.0043(12) 0.0035(11) 0.0154(13) C347 0.0334(14) 0.0447(17) 0.0291(14) -0.0026(12) 0.0024(11) 0.0039(13) C348 0.046(2) 0.067(2) 0.048(2) 0.0052(17) 0.0094(16) -0.0017(18) C402 0.0150(10) 0.0164(10) 0.0188(10) 0.0018(8) -0.0002(8) -0.0012(8) C403 0.0152(9) 0.0171(10) 0.0180(10) 0.0027(8) 0.0004(8) -0.0021(8) C404 0.0151(10) 0.0177(10) 0.0182(10) 0.0027(8) 0.0006(8) -0.0011(8) C408 0.0179(10) 0.0192(11) 0.0236(11) 0.0027(9) 0.0014(8) 0.0022(8) C409 0.0162(10) 0.0177(10) 0.0238(11) 0.0028(8) -0.0027(8) 0.0000(8) C410 0.0175(10) 0.0158(10) 0.0227(11) 0.0014(8) -0.0029(8) -0.0011(8) C411 0.0179(10) 0.0178(10) 0.0210(10) 0.0011(8) -0.0035(8) -0.0021(8) C412 0.0171(10) 0.0196(11) 0.0199(10) 0.0014(8) -0.0011(8) -0.0041(8) C413 0.0156(10) 0.0186(10) 0.0203(10) 0.0024(8) 0.0005(8) -0.0029(8) C414 0.0186(10) 0.0201(11) 0.0182(10) 0.0007(8) 0.0020(8) -0.0026(8) C415 0.0191(10) 0.0182(10) 0.0191(10) 0.0011(8) 0.0031(8) 0.0014(8) C416 0.0170(10) 0.0193(10) 0.0190(10) 0.0026(8) -0.0007(8) -0.0003(8) C425 0.0150(10) 0.0244(12) 0.0329(13) 0.0027(10) -0.0018(9) -0.0001(9) C426 0.0161(10) 0.0220(11) 0.0313(13) 0.0014(9) -0.0029(9) -0.0009(9) C427 0.0201(11) 0.0247(12) 0.0282(12) 0.0009(10) -0.0058(9) 0.0002(9) C428 0.0255(12) 0.0297(13) 0.0258(12) 0.0037(10) -0.0079(10) -0.0018(10) C429 0.0301(13) 0.0286(13) 0.0217(11) -0.0009(10) -0.0063(10) -0.0047(10) C430 0.0252(12) 0.0230(12) 0.0234(11) -0.0011(9) -0.0018(9) -0.0029(9) C431 0.0196(11) 0.0216(11) 0.0240(11) -0.0009(9) 0.0025(9) -0.0040(9) C432 0.0228(11) 0.0236(11) 0.0223(11) -0.0017(9) 0.0041(9) -0.0024(9) C441 0.0153(10) 0.0318(13) 0.0384(14) 0.0006(11) -0.0009(10) 0.0028(10) C442 0.0230(13) 0.0346(16) 0.076(2) 0.0131(15) -0.0061(14) 0.0018(12) C443 0.0223(13) 0.0333(16) 0.085(3) 0.0009(16) -0.0076(15) 0.0075(12) C444 0.0234(14) 0.0467(19) 0.064(2) -0.0009(16) -0.0078(14) 0.0039(13) C445 0.0245(12) 0.0273(13) 0.0324(13) -0.0080(10) 0.0066(10) -0.0014(10) C446 0.0395(16) 0.0417(16) 0.0289(13) -0.0125(12) -0.0062(12) 0.0152(13) C447 0.0421(18) 0.064(2) 0.0504(19) -0.0357(17) -0.0192(15) 0.0257(16) C448 0.128(4) 0.103(4) 0.041(2) -0.035(2) -0.035(2) 0.082(3) C993 0.0435(18) 0.0335(16) 0.073(2) 0.0116(16) 0.0026(17) -0.0054(14) C994 0.0490(19) 0.0307(16) 0.064(2) 0.0055(15) -0.0063(16) -0.0034(14) C995 0.0414(17) 0.0436(18) 0.053(2) 0.0099(15) -0.0033(15) 0.0072(14) C996 0.0375(17) 0.0384(17) 0.060(2) 0.0137(15) -0.0043(15) -0.0016(13) C997 0.0459(18) 0.0259(15) 0.066(2) 0.0112(14) 0.0014(16) -0.0046(13) C998 0.0481(19) 0.0303(16) 0.069(2) 0.0130(15) 0.0066(17) 0.0002(14) C999 0.074(3) 0.038(2) 0.101(4) 0.009(2) 0.036(3) 0.0056(19) _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 S101 C124 1.732(2) . ? S101 C140 1.737(3) . ? S102 C125 1.728(3) . ? S102 C108 1.734(2) . ? S103 C115 1.732(2) . ? S103 C132 1.737(3) . ? S104 C117 1.733(2) . ? S104 C133 1.737(3) . ? S201 C240 1.726(3) . ? S201 C224 1.730(2) . ? S202 C225 1.730(3) . ? S202 C208 1.732(2) . ? S203 C232 1.722(3) . ? S203 C215 1.732(2) . ? S204 C233 1.718(3) . ? S204 C217 1.724(2) . ? S302 C325 1.724(3) . ? S302 C308 1.737(2) . ? S303 C332 1.732(3) . ? S303 C315 1.740(2) . ? S402 C425 1.735(3) . ? S402 C408 1.741(2) . ? S403 C432 1.728(2) . ? S403 C415 1.735(2) . ? C101 C107 1.413(3) . ? C101 C102 1.433(3) . ? C101 C106 1.443(3) . ? C102 C110 1.406(3) . ? C102 C103 1.439(3) . ? C103 C113 1.403(3) . ? C103 C104 1.436(3) . ? C104 C116 1.415(3) . ? C104 C105 1.430(3) . ? C105 C119 1.403(3) . ? C105 C106 1.443(3) . ? C106 C122 1.407(3) . ? C107 C108 1.421(3) . ? C107 C124 1.422(3) . ? C108 C109 1.400(4) . ? C109 C110 1.433(3) . ? C109 C126 1.448(3) . ? C110 C111 1.454(3) . ? C111 C127 1.418(3) . ? C111 C112 1.420(3) . ? C112 C130 1.412(3) . ? C112 C113 1.450(3) . ? C113 C114 1.433(3) . ? C114 C115 1.400(3) . ? C114 C131 1.443(3) . ? C115 C116 1.424(3) . ? C116 C117 1.420(3) . ? C117 C118 1.397(3) . ? C118 C119 1.431(3) . ? C118 C134 1.445(3) . ? C119 C120 1.446(3) . ? C120 C135 1.411(3) . ? C120 C121 1.415(3) . ? C121 C138 1.418(3) . ? C121 C122 1.453(3) . ? C122 C123 1.434(3) . ? C123 C124 1.403(3) . ? C123 C139 1.450(3) . ? C125 C126 1.358(4) . ? C125 C141 1.508(4) . ? C127 C128 1.371(4) . ? C128 C129 1.392(4) . ? C129 C130 1.378(4) . ? C131 C132 1.366(3) . ? C132 C145 1.497(3) . ? C133 C134 1.354(3) . ? C133 C149 1.503(3) . ? C135 C136 1.375(4) . ? C136 C137 1.388(4) . ? C137 C138 1.374(4) . ? C139 C140 1.346(4) . ? C140 C153 1.501(4) . ? C141 C142 1.486(5) . ? C142 C143 1.533(5) . ? C143 C144 1.497(6) . ? C145 C146 1.525(4) . ? C146 C147 1.523(4) . ? C147 C148 1.514(5) . ? C149 C150 1.525(4) . ? C150 C151 1.515(4) . ? C151 C152 1.521(5) . ? C153 C154 1.509(4) . ? C154 C155 1.693(7) . ? C155 C156 1.317(8) . ? C201 C207 1.416(3) . ? C201 C202 1.434(3) . ? C201 C206 1.437(3) . ? C202 C210 1.409(3) . ? C202 C203 1.439(3) . ? C203 C213 1.404(3) . ? C203 C204 1.437(3) . ? C204 C216 1.412(3) . ? C204 C205 1.441(3) . ? C205 C219 1.403(3) . ? C205 C206 1.442(3) . ? C206 C222 1.406(3) . ? C207 C208 1.422(3) . ? C207 C224 1.425(3) . ? C208 C209 1.404(3) . ? C209 C210 1.426(3) . ? C209 C226 1.451(3) . ? C210 C211 1.451(3) . ? C211 C212 1.410(3) . ? C211 C227 1.421(3) . ? C212 C230 1.419(3) . ? C212 C213 1.456(3) . ? C213 C214 1.429(3) . ? C214 C215 1.402(3) . ? C214 C231 1.448(3) . ? C215 C216 1.417(3) . ? C216 C217 1.420(3) . ? C217 C218 1.405(3) . ? C218 C219 1.433(3) . ? C218 C234 1.473(3) . ? C219 C220 1.450(3) . ? C220 C221 1.412(4) . ? C220 C235 1.419(3) . ? C221 C238 1.415(4) . ? C221 C222 1.455(3) . ? C222 C223 1.432(3) . ? C223 C224 1.397(3) . ? C223 C239 1.454(3) . ? C225 C226 1.355(4) . ? C225 C241 1.502(3) . ? C227 C228 1.379(4) . ? C228 C229 1.390(4) . ? C229 C230 1.382(4) . ? C231 C232 1.358(4) . ? C232 C245 1.511(4) . ? C233 C234 1.376(4) . ? C233 C249 1.501(3) . ? C235 C236 1.377(4) . ? C236 C237 1.396(4) . ? C237 C238 1.370(4) . ? C239 C240 1.363(4) . ? C240 C253 1.504(3) . ? C241 C242 1.511(4) . ? C242 C243 1.522(5) . ? C243 C244 1.522(6) . ? C245 C246 1.582(5) . ? C246 C247 1.512(5) . ? C247 C248 1.501(5) . ? C249 C250 1.507(5) . ? C250 C251 1.541(6) . ? C251 C252 1.452(6) . ? C253 C254 1.468(4) . ? C254 C255 1.616(5) . ? C255 C256 1.430(6) . ? C302 C310 1.407(3) . ? C302 C303 1.444(3) . ? C302 C304 1.444(3) 3_566 ? C303 C313 1.411(3) . ? C303 C304 1.437(3) . ? C304 C316 1.417(3) . ? C304 C302 1.444(3) 3_566 ? C308 C309 1.396(3) . ? C308 C316 1.416(3) 3_566 ? C309 C310 1.437(3) . ? C309 C326 1.443(3) . ? C310 C311 1.447(3) . ? C311 C327 1.411(3) . ? C311 C312 1.426(3) . ? C312 C330 1.417(3) . ? C312 C313 1.447(3) . ? C313 C314 1.435(3) . ? C314 C315 1.393(3) . ? C314 C331 1.448(3) . ? C315 C316 1.418(3) . ? C316 C308 1.416(3) 3_566 ? C325 C326 1.363(3) . ? C325 C341 1.507(3) . ? C327 C328 1.378(4) . ? C328 C329 1.393(4) . ? C329 C330 1.375(4) . ? C331 C332 1.357(4) . ? C332 C345 1.508(3) . ? C341 C342 1.511(4) . ? C342 C343 1.525(4) . ? C343 C344 1.504(5) . ? C345 C346 1.504(4) . ? C346 C347 1.517(4) . ? C347 C348 1.526(4) . ? C402 C410 1.412(3) . ? C402 C404 1.439(3) 3_667 ? C402 C403 1.444(3) . ? C403 C413 1.410(3) . ? C403 C404 1.439(3) . ? C404 C416 1.418(3) . ? C404 C402 1.439(3) 3_667 ? C408 C409 1.394(3) . ? C408 C416 1.419(3) 3_667 ? C409 C410 1.429(3) . ? C409 C426 1.443(3) . ? C410 C411 1.447(3) . ? C411 C427 1.419(3) . ? C411 C412 1.419(3) . ? C412 C430 1.414(3) . ? C412 C413 1.455(3) . ? C413 C414 1.433(3) . ? C414 C415 1.398(3) . ? C414 C431 1.439(3) . ? C415 C416 1.417(3) . ? C416 C408 1.419(3) 3_667 ? C425 C426 1.353(4) . ? C425 C441 1.502(3) . ? C427 C428 1.374(4) . ? C428 C429 1.389(4) . ? C429 C430 1.381(3) . ? C431 C432 1.359(3) . ? C432 C445 1.500(3) . ? C441 C442 1.518(4) . ? C442 C443 1.531(4) . ? C443 C444 1.489(4) . ? C445 C446 1.512(4) . ? C446 C447 1.526(4) . ? C447 C448 1.505(5) . ? C993 C994 1.382(5) . ? C993 C998 1.390(5) . ? C994 C995 1.390(5) . ? C995 C996 1.384(5) . ? C996 C997 1.380(5) . ? C997 C998 1.389(5) . ? C998 C999 1.506(5) . ? 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 C124 S101 C140 92.00(13) . . ? C125 S102 C108 92.12(13) . . ? C115 S103 C132 92.28(12) . . ? C117 S104 C133 92.19(12) . . ? C240 S201 C224 91.99(12) . . ? C225 S202 C208 91.94(12) . . ? C232 S203 C215 92.01(12) . . ? C233 S204 C217 91.99(12) . . ? C325 S302 C308 92.12(12) . . ? C332 S303 C315 91.94(12) . . ? C425 S402 C408 91.65(12) . . ? C432 S403 C415 92.09(11) . . ? C107 C101 C102 120.6(2) . . ? C107 C101 C106 120.1(2) . . ? C102 C101 C106 119.3(2) . . ? C110 C102 C101 120.7(2) . . ? C110 C102 C103 119.8(2) . . ? C101 C102 C103 119.5(2) . . ? C113 C103 C104 120.1(2) . . ? C113 C103 C102 119.9(2) . . ? C104 C103 C102 120.0(2) . . ? C116 C104 C105 120.7(2) . . ? C116 C104 C103 120.4(2) . . ? C105 C104 C103 118.9(2) . . ? C119 C105 C104 120.3(2) . . ? C119 C105 C106 119.5(2) . . ? C104 C105 C106 120.1(2) . . ? C122 C106 C101 120.9(2) . . ? C122 C106 C105 119.8(2) . . ? C101 C106 C105 119.1(2) . . ? C101 C107 C108 117.2(2) . . ? C101 C107 C124 117.4(2) . . ? C108 C107 C124 125.3(2) . . ? C109 C108 C107 122.5(2) . . ? C109 C108 S102 111.37(18) . . ? C107 C108 S102 126.1(2) . . ? C108 C109 C110 119.7(2) . . ? C108 C109 C126 111.1(2) . . ? C110 C109 C126 129.1(2) . . ? C102 C110 C109 117.8(2) . . ? C102 C110 C111 118.0(2) . . ? C109 C110 C111 124.2(2) . . ? C127 C111 C112 117.8(2) . . ? C127 C111 C110 122.7(2) . . ? C112 C111 C110 119.1(2) . . ? C130 C112 C111 119.1(2) . . ? C130 C112 C113 121.2(2) . . ? C111 C112 C113 119.3(2) . . ? C103 C113 C114 118.4(2) . . ? C103 C113 C112 117.7(2) . . ? C114 C113 C112 123.8(2) . . ? C115 C114 C113 119.4(2) . . ? C115 C114 C131 111.5(2) . . ? C113 C114 C131 128.9(2) . . ? C114 C115 C116 122.2(2) . . ? C114 C115 S103 111.25(17) . . ? C116 C115 S103 126.57(18) . . ? C104 C116 C117 117.3(2) . . ? C104 C116 C115 117.5(2) . . ? C117 C116 C115 125.1(2) . . ? C118 C117 C116 122.1(2) . . ? C118 C117 S104 111.17(17) . . ? C116 C117 S104 126.70(18) . . ? C117 C118 C119 119.9(2) . . ? C117 C118 C134 111.4(2) . . ? C119 C118 C134 128.3(2) . . ? C105 C119 C118 118.1(2) . . ? C105 C119 C120 118.6(2) . . ? C118 C119 C120 123.4(2) . . ? C135 C120 C121 119.2(2) . . ? C135 C120 C119 121.3(2) . . ? C121 C120 C119 119.3(2) . . ? C120 C121 C138 118.0(2) . . ? C120 C121 C122 119.3(2) . . ? C138 C121 C122 122.4(2) . . ? C106 C122 C123 117.7(2) . . ? C106 C122 C121 118.2(2) . . ? C123 C122 C121 124.1(2) . . ? C124 C123 C122 119.7(2) . . ? C124 C123 C139 110.7(2) . . ? C122 C123 C139 129.4(2) . . ? C123 C124 C107 122.5(2) . . ? C123 C124 S101 111.45(19) . . ? C107 C124 S101 126.01(19) . . ? C126 C125 C141 125.7(3) . . ? C126 C125 S102 112.0(2) . . ? C141 C125 S102 122.2(2) . . ? C125 C126 C109 113.5(3) . . ? C128 C127 C111 121.8(2) . . ? C127 C128 C129 120.1(2) . . ? C130 C129 C128 120.0(3) . . ? C129 C130 C112 121.1(2) . . ? C132 C131 C114 113.5(2) . . ? C131 C132 C145 127.6(2) . . ? C131 C132 S103 111.41(18) . . ? C145 C132 S103 121.0(2) . . ? C134 C133 C149 128.3(2) . . ? C134 C133 S104 111.54(18) . . ? C149 C133 S104 120.1(2) . . ? C133 C134 C118 113.7(2) . . ? C136 C135 C120 121.3(2) . . ? C135 C136 C137 119.7(2) . . ? C138 C137 C136 120.6(2) . . ? C137 C138 C121 121.2(2) . . ? C140 C139 C123 114.0(2) . . ? C139 C140 C153 127.8(3) . . ? C139 C140 S101 111.8(2) . . ? C153 C140 S101 120.3(2) . . ? C142 C141 C125 115.9(3) . . ? C141 C142 C143 112.9(4) . . ? C144 C143 C142 115.3(4) . . ? C132 C145 C146 114.1(2) . . ? C147 C146 C145 113.3(2) . . ? C148 C147 C146 113.2(3) . . ? C133 C149 C150 113.2(2) . . ? C151 C150 C149 114.4(3) . . ? C150 C151 C152 112.3(3) . . ? C140 C153 C154 114.4(3) . . ? C153 C154 C155 109.9(3) . . ? C156 C155 C154 95.5(6) . . ? C207 C201 C202 120.1(2) . . ? C207 C201 C206 120.4(2) . . ? C202 C201 C206 119.5(2) . . ? C210 C202 C201 120.7(2) . . ? C210 C202 C203 119.7(2) . . ? C201 C202 C203 119.5(2) . . ? C213 C203 C204 120.3(2) . . ? C213 C203 C202 119.9(2) . . ? C204 C203 C202 119.6(2) . . ? C216 C204 C203 120.1(2) . . ? C216 C204 C205 120.3(2) . . ? C203 C204 C205 119.5(2) . . ? C219 C205 C204 120.5(2) . . ? C219 C205 C206 120.5(2) . . ? C204 C205 C206 118.94(19) . . ? C222 C206 C201 120.6(2) . . ? C222 C206 C205 119.4(2) . . ? C201 C206 C205 119.9(2) . . ? C201 C207 C208 117.6(2) . . ? C201 C207 C224 117.3(2) . . ? C208 C207 C224 125.0(2) . . ? C209 C208 C207 122.3(2) . . ? C209 C208 S202 111.49(17) . . ? C207 C208 S202 126.24(18) . . ? C208 C209 C210 119.6(2) . . ? C208 C209 C226 111.0(2) . . ? C210 C209 C226 129.2(2) . . ? C202 C210 C209 118.3(2) . . ? C202 C210 C211 117.6(2) . . ? C209 C210 C211 124.1(2) . . ? C212 C211 C227 118.4(2) . . ? C212 C211 C210 119.6(2) . . ? C227 C211 C210 121.7(2) . . ? C211 C212 C230 119.1(2) . . ? C211 C212 C213 119.2(2) . . ? C230 C212 C213 121.4(2) . . ? C203 C213 C214 118.3(2) . . ? C203 C213 C212 117.8(2) . . ? C214 C213 C212 123.9(2) . . ? C215 C214 C213 119.3(2) . . ? C215 C214 C231 111.6(2) . . ? C213 C214 C231 128.8(2) . . ? C214 C215 C216 122.2(2) . . ? C214 C215 S203 111.12(18) . . ? C216 C215 S203 126.56(18) . . ? C204 C216 C215 117.6(2) . . ? C204 C216 C217 117.4(2) . . ? C215 C216 C217 124.9(2) . . ? C218 C217 C216 122.6(2) . . ? C218 C217 S204 112.20(17) . . ? C216 C217 S204 125.23(19) . . ? C217 C218 C219 119.4(2) . . ? C217 C218 C234 111.0(2) . . ? C219 C218 C234 129.3(2) . . ? C205 C219 C218 118.4(2) . . ? C205 C219 C220 118.0(2) . . ? C218 C219 C220 123.5(2) . . ? C221 C220 C235 118.4(2) . . ? C221 C220 C219 119.5(2) . . ? C235 C220 C219 121.8(2) . . ? C220 C221 C238 118.7(2) . . ? C220 C221 C222 119.7(2) . . ? C238 C221 C222 121.3(2) . . ? C206 C222 C223 118.1(2) . . ? C206 C222 C221 118.0(2) . . ? C223 C222 C221 123.8(2) . . ? C224 C223 C222 119.7(2) . . ? C224 C223 C239 111.2(2) . . ? C222 C223 C239 129.0(2) . . ? C223 C224 C207 122.4(2) . . ? C223 C224 S201 111.63(18) . . ? C207 C224 S201 125.95(18) . . ? C226 C225 C241 128.4(3) . . ? C226 C225 S202 112.33(19) . . ? C241 C225 S202 119.2(2) . . ? C225 C226 C209 113.2(2) . . ? C228 C227 C211 121.3(2) . . ? C227 C228 C229 120.0(2) . . ? C230 C229 C228 120.2(2) . . ? C229 C230 C212 120.8(2) . . ? C232 C231 C214 112.6(2) . . ? C231 C232 C245 127.0(2) . . ? C231 C232 S203 112.72(19) . . ? C245 C232 S203 120.1(2) . . ? C234 C233 C249 127.3(2) . . ? C234 C233 S204 113.51(19) . . ? C249 C233 S204 119.2(2) . . ? C233 C234 C218 111.3(2) . . ? C236 C235 C220 121.3(3) . . ? C235 C236 C237 120.0(3) . . ? C238 C237 C236 119.9(3) . . ? C237 C238 C221 121.6(3) . . ? C240 C239 C223 112.7(2) . . ? C239 C240 C253 126.6(2) . . ? C239 C240 S201 112.42(18) . . ? C253 C240 S201 121.0(2) . . ? C225 C241 C242 114.1(2) . . ? C241 C242 C243 113.3(3) . . ? C244 C243 C242 111.4(4) . . ? C232 C245 C246 109.5(2) . . ? C247 C246 C245 113.6(3) . . ? C248 C247 C246 114.1(3) . . ? C233 C249 C250 112.5(3) . . ? C249 C250 C251 114.6(3) . . ? C252 C251 C250 114.9(4) . . ? C254 C253 C240 115.0(2) . . ? C253 C254 C255 114.5(3) . . ? C256 C255 C254 103.0(4) . . ? C310 C302 C303 119.7(2) . . ? C310 C302 C304 120.8(2) . 3_566 ? C303 C302 C304 119.5(2) . 3_566 ? C313 C303 C304 120.5(2) . . ? C313 C303 C302 119.8(2) . . ? C304 C303 C302 119.7(2) . . ? C316 C304 C303 119.9(2) . . ? C316 C304 C302 119.3(2) . 3_566 ? C303 C304 C302 120.77(19) . 3_566 ? C309 C308 C316 123.0(2) . 3_566 ? C309 C308 S302 111.10(18) . . ? C316 C308 S302 125.82(18) 3_566 . ? C308 C309 C310 118.7(2) . . ? C308 C309 C326 111.6(2) . . ? C310 C309 C326 129.7(2) . . ? C302 C310 C309 118.7(2) . . ? C302 C310 C311 119.3(2) . . ? C309 C310 C311 122.0(2) . . ? C327 C311 C312 118.4(2) . . ? C327 C311 C310 122.2(2) . . ? C312 C311 C310 119.1(2) . . ? C330 C312 C311 117.8(2) . . ? C330 C312 C313 122.2(2) . . ? C311 C312 C313 119.5(2) . . ? C303 C313 C314 118.4(2) . . ? C303 C313 C312 119.0(2) . . ? C314 C313 C312 122.4(2) . . ? C315 C314 C313 119.1(2) . . ? C315 C314 C331 111.1(2) . . ? C313 C314 C331 129.7(2) . . ? C314 C315 C316 122.5(2) . . ? C314 C315 S303 111.39(17) . . ? C316 C315 S303 125.93(19) . . ? C308 C316 C304 118.0(2) 3_566 . ? C308 C316 C315 124.3(2) 3_566 . ? C304 C316 C315 117.8(2) . . ? C326 C325 C341 127.7(2) . . ? C326 C325 S302 112.02(19) . . ? C341 C325 S302 120.25(19) . . ? C325 C326 C309 113.2(2) . . ? C328 C327 C311 122.2(2) . . ? C327 C328 C329 119.5(2) . . ? C330 C329 C328 119.9(2) . . ? C329 C330 C312 122.2(2) . . ? C332 C331 C314 113.7(2) . . ? C331 C332 C345 128.3(2) . . ? C331 C332 S303 111.68(18) . . ? C345 C332 S303 119.9(2) . . ? C325 C341 C342 112.3(2) . . ? C341 C342 C343 114.6(2) . . ? C344 C343 C342 113.1(3) . . ? C346 C345 C332 114.7(2) . . ? C345 C346 C347 113.9(2) . . ? C346 C347 C348 113.9(3) . . ? C410 C402 C404 120.3(2) . 3_667 ? C410 C402 C403 119.6(2) . . ? C404 C402 C403 120.05(19) 3_667 . ? C413 C403 C404 120.6(2) . . ? C413 C403 C402 120.0(2) . . ? C404 C403 C402 119.4(2) . . ? C416 C404 C402 119.7(2) . 3_667 ? C416 C404 C403 119.7(2) . . ? C402 C404 C403 120.6(2) 3_667 . ? C409 C408 C416 122.5(2) . 3_667 ? C409 C408 S402 111.34(17) . . ? C416 C408 S402 125.99(18) 3_667 . ? C408 C409 C410 119.1(2) . . ? C408 C409 C426 111.2(2) . . ? C410 C409 C426 129.7(2) . . ? C402 C410 C409 118.6(2) . . ? C402 C410 C411 119.1(2) . . ? C409 C410 C411 122.1(2) . . ? C427 C411 C412 118.0(2) . . ? C427 C411 C410 121.8(2) . . ? C412 C411 C410 119.8(2) . . ? C430 C412 C411 118.5(2) . . ? C430 C412 C413 122.1(2) . . ? C411 C412 C413 119.1(2) . . ? C403 C413 C414 118.4(2) . . ? C403 C413 C412 119.0(2) . . ? C414 C413 C412 122.5(2) . . ? C415 C414 C413 119.3(2) . . ? C415 C414 C431 111.0(2) . . ? C413 C414 C431 129.6(2) . . ? C414 C415 C416 122.3(2) . . ? C414 C415 S403 111.37(17) . . ? C416 C415 S403 126.20(18) . . ? C415 C416 C404 118.0(2) . . ? C415 C416 C408 124.2(2) . 3_667 ? C404 C416 C408 117.8(2) . 3_667 ? C426 C425 C441 127.3(2) . . ? C426 C425 S402 111.90(18) . . ? C441 C425 S402 120.8(2) . . ? C425 C426 C409 113.7(2) . . ? C428 C427 C411 122.0(2) . . ? C427 C428 C429 120.0(2) . . ? C430 C429 C428 119.7(2) . . ? C429 C430 C412 121.8(2) . . ? C432 C431 C414 114.0(2) . . ? C431 C432 C445 127.3(2) . . ? C431 C432 S403 111.52(18) . . ? C445 C432 S403 121.11(19) . . ? C425 C441 C442 113.0(2) . . ? C441 C442 C443 113.2(3) . . ? C444 C443 C442 113.9(3) . . ? C432 C445 C446 113.6(2) . . ? C445 C446 C447 113.6(3) . . ? C448 C447 C446 112.8(4) . . ? C994 C993 C998 121.1(3) . . ? C993 C994 C995 120.2(3) . . ? C996 C995 C994 119.4(4) . . ? C997 C996 C995 119.6(3) . . ? C996 C997 C998 121.9(3) . . ? C997 C998 C993 117.7(4) . . ? C997 C998 C999 120.9(3) . . ? C993 C998 C999 121.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.211 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.093 # Attachment '- 1b_TCNQ.cif' data_cocrs10 _database_code_depnum_ccdc_archive 'CCDC 817723' #TrackingRef '- 1b_TCNQ.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 N4 S4' _chemical_formula_weight 1053.38 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' S S 0.1246 0.1234 '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' _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 13.742(2) _cell_length_b 21.483(4) _cell_length_c 17.611(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.049(3) _cell_angle_gamma 90.00 _cell_volume 5170.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.45 _exptl_crystal_description BLOCK _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8803 _exptl_absorpt_correction_T_max 0.9636 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 79510 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.54 _reflns_number_total 15748 _reflns_number_gt 10534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0700P)^2^+4.3833P] 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 15748 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.287 _refine_ls_restrained_S_all 1.287 _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 S1 S 0.45089(6) 0.59264(4) 1.47002(4) 0.03058(17) Uani 1 1 d . . . S2 S 0.24199(6) 0.59382(4) 1.40304(4) 0.02991(17) Uani 1 1 d . . . S3 S 0.46909(5) 0.55316(3) 0.86461(4) 0.02101(14) Uani 1 1 d . . . S4 S 0.67996(5) 0.55399(3) 0.93581(4) 0.02089(14) Uani 1 1 d . . . C1 C 0.4265(2) 0.61410(12) 1.23791(14) 0.0194(5) Uani 1 1 d . . . C2 C 0.35466(19) 0.61507(11) 1.17201(14) 0.0182(5) Uani 1 1 d . . . C3 C 0.38681(18) 0.61042(11) 1.09679(14) 0.0170(5) Uani 1 1 d . . . C4 C 0.48971(18) 0.60364(11) 1.08873(14) 0.0172(5) Uani 1 1 d . . . C5 C 0.56067(18) 0.61424(12) 1.15374(14) 0.0176(5) Uani 1 1 d . . . C6 C 0.52861(19) 0.61943(12) 1.22893(14) 0.0187(5) Uani 1 1 d . . . C7 C 0.3960(2) 0.60951(12) 1.31231(14) 0.0210(5) Uani 1 1 d . . . C8 C 0.2942(2) 0.60445(13) 1.31887(15) 0.0231(5) Uani 1 1 d . . . C9 C 0.2233(2) 0.60801(13) 1.25538(15) 0.0229(5) Uani 1 1 d . . . C10 C 0.25338(19) 0.61782(12) 1.18082(15) 0.0202(5) Uani 1 1 d . . . C11 C 0.18606(19) 0.63256(12) 1.11366(15) 0.0205(5) Uani 1 1 d . . . C12 C 0.21831(19) 0.62843(12) 1.03960(15) 0.0203(5) Uani 1 1 d . . . C13 C 0.31728(18) 0.60814(11) 1.03176(14) 0.0172(5) Uani 1 1 d . . . C14 C 0.34821(19) 0.58735(12) 0.96075(14) 0.0180(5) Uani 1 1 d . . . C15 C 0.44815(19) 0.57944(11) 0.95447(13) 0.0176(5) Uani 1 1 d . . . C16 C 0.52125(18) 0.58951(11) 1.01664(14) 0.0174(5) Uani 1 1 d . . . C17 C 0.62386(18) 0.58157(12) 1.01294(14) 0.0183(5) Uani 1 1 d . . . C18 C 0.69288(19) 0.59456(12) 1.07505(15) 0.0200(5) Uani 1 1 d . . . C19 C 0.66059(19) 0.61665(12) 1.14436(14) 0.0197(5) Uani 1 1 d . . . C20 C 0.72646(19) 0.64334(13) 1.20594(15) 0.0229(5) Uani 1 1 d . . . C21 C 0.6965(2) 0.64721(13) 1.28021(15) 0.0236(5) Uani 1 1 d . . . C22 C 0.5991(2) 0.62629(13) 1.29285(15) 0.0222(5) Uani 1 1 d . . . C23 C 0.5696(2) 0.61468(12) 1.36728(15) 0.0227(5) Uani 1 1 d . . . C24 C 0.4702(2) 0.60702(12) 1.37558(14) 0.0234(5) Uani 1 1 d . . . C25 C 0.1245(2) 0.59160(14) 1.35545(17) 0.0291(6) Uani 1 1 d . . . C26 C 0.1263(2) 0.59894(14) 1.27890(16) 0.0284(6) Uani 1 1 d . . . H26A H 0.0689 0.5982 1.2438 0.034 Uiso 1 1 calc R . . C27 C 0.0910(2) 0.65678(14) 1.11914(17) 0.0266(6) Uani 1 1 d . . . H27A H 0.0688 0.6613 1.1682 0.032 Uiso 1 1 calc R . . C28 C 0.0299(2) 0.67388(14) 1.05561(18) 0.0295(6) Uani 1 1 d . . . H28A H -0.0345 0.6880 1.0611 0.035 Uiso 1 1 calc R . . C29 C 0.0621(2) 0.67053(14) 0.98328(17) 0.0276(6) Uani 1 1 d . . . H29A H 0.0202 0.6829 0.9395 0.033 Uiso 1 1 calc R . . C30 C 0.1555(2) 0.64912(13) 0.97561(16) 0.0229(5) Uani 1 1 d . . . H30A H 0.1780 0.6483 0.9264 0.027 Uiso 1 1 calc R . . C31 C 0.28973(19) 0.56785(12) 0.89163(14) 0.0202(5) Uani 1 1 d . . . H31A H 0.2202 0.5686 0.8856 0.024 Uiso 1 1 calc R . . C32 C 0.34486(19) 0.54818(12) 0.83591(14) 0.0195(5) Uani 1 1 d . . . C33 C 0.79526(19) 0.55639(12) 0.98745(15) 0.0213(5) Uani 1 1 d . . . C34 C 0.79037(19) 0.57879(12) 1.05896(15) 0.0219(5) Uani 1 1 d . . . H34A H 0.8462 0.5836 1.0951 0.026 Uiso 1 1 calc R . . C35 C 0.8151(2) 0.67211(14) 1.19092(18) 0.0293(6) Uani 1 1 d . . . H35A H 0.8340 0.6712 1.1406 0.035 Uiso 1 1 calc R . . C36 C 0.8747(2) 0.70144(16) 1.2480(2) 0.0360(7) Uani 1 1 d . . . H36A H 0.9343 0.7201 1.2371 0.043 Uiso 1 1 calc R . . C37 C 0.8467(2) 0.70352(16) 1.32211(19) 0.0362(7) Uani 1 1 d . . . H37A H 0.8879 0.7230 1.3619 0.043 Uiso 1 1 calc R . . C38 C 0.7596(2) 0.67745(14) 1.33723(17) 0.0300(6) Uani 1 1 d . . . H38A H 0.7411 0.6798 1.3876 0.036 Uiso 1 1 calc R . . C39 C 0.6284(2) 0.60528(13) 1.43958(16) 0.0285(6) Uani 1 1 d . . . H39A H 0.6978 0.6073 1.4451 0.034 Uiso 1 1 calc R . . C40 C 0.5752(3) 0.59332(13) 1.49889(16) 0.0304(6) Uani 1 1 d . . . C41 C 0.0391(2) 0.58326(17) 1.40058(18) 0.0354(7) Uani 1 1 d . . . H41A H 0.0392 0.5400 1.4201 0.042 Uiso 1 1 calc R . . H41B H -0.0221 0.5893 1.3664 0.042 Uiso 1 1 calc R . . C42 C 0.0398(2) 0.62807(16) 1.46752(18) 0.0333(7) Uani 1 1 d . . . H42A H 0.0356 0.6712 1.4476 0.040 Uiso 1 1 calc R . . H42B H 0.1029 0.6239 1.4999 0.040 Uiso 1 1 calc R . . C43 C -0.0433(2) 0.61737(17) 1.51661(19) 0.0379(7) Uani 1 1 d . . . H43A H -0.1064 0.6252 1.4855 0.045 Uiso 1 1 calc R . . H43B H -0.0426 0.5733 1.5332 0.045 Uiso 1 1 calc R . . C44 C -0.0363(4) 0.6589(2) 1.5864(2) 0.0578(11) Uani 1 1 d . . . H44A H -0.0920 0.6508 1.6155 0.087 Uiso 1 1 calc R . . H44B H -0.0371 0.7026 1.5704 0.087 Uiso 1 1 calc R . . H44C H 0.0248 0.6501 1.6185 0.087 Uiso 1 1 calc R . . C45 C 0.3111(2) 0.52444(13) 0.75757(15) 0.0238(5) Uani 1 1 d . . . H45A H 0.2475 0.5030 0.7589 0.029 Uiso 1 1 calc R . . H45B H 0.3588 0.4935 0.7425 0.029 Uiso 1 1 calc R . . C46 C 0.2995(2) 0.57601(13) 0.69770(15) 0.0244(5) Uani 1 1 d . . . H46A H 0.2441 0.6030 0.7083 0.029 Uiso 1 1 calc R . . H46B H 0.3594 0.6019 0.7026 0.029 Uiso 1 1 calc R . . C47 C 0.2814(2) 0.55225(14) 0.61588(15) 0.0287(6) Uani 1 1 d . . . H47A H 0.2776 0.5883 0.5807 0.034 Uiso 1 1 calc R . . H47B H 0.3379 0.5265 0.6047 0.034 Uiso 1 1 calc R . . C48 C 0.1889(2) 0.51408(16) 0.59992(17) 0.0332(7) Uani 1 1 d . . . H48A H 0.1788 0.5038 0.5454 0.050 Uiso 1 1 calc R . . H48B H 0.1330 0.5381 0.6141 0.050 Uiso 1 1 calc R . . H48C H 0.1951 0.4756 0.6299 0.050 Uiso 1 1 calc R . . C49 C 0.8843(2) 0.53237(14) 0.95516(16) 0.0241(5) Uani 1 1 d . . . H49A H 0.8828 0.4863 0.9567 0.029 Uiso 1 1 calc R . . H49B H 0.9427 0.5461 0.9887 0.029 Uiso 1 1 calc R . . C50 C 0.8964(2) 0.55252(15) 0.87370(16) 0.0279(6) Uani 1 1 d . . . H50A H 0.8942 0.5985 0.8703 0.033 Uiso 1 1 calc R . . H50B H 0.8418 0.5357 0.8385 0.033 Uiso 1 1 calc R . . C51 C 0.9935(2) 0.52916(17) 0.84972(17) 0.0339(7) Uani 1 1 d . . . H51A H 1.0472 0.5434 0.8877 0.041 Uiso 1 1 calc R . . H51B H 0.9933 0.4831 0.8503 0.041 Uiso 1 1 calc R . . C52 C 1.0140(3) 0.5513(2) 0.7709(2) 0.0546(11) Uani 1 1 d . . . H52A H 1.0772 0.5348 0.7592 0.082 Uiso 1 1 calc R . . H52B H 1.0157 0.5969 0.7701 0.082 Uiso 1 1 calc R . . H52C H 0.9622 0.5363 0.7327 0.082 Uiso 1 1 calc R . . C53 C 0.6064(3) 0.58046(16) 1.58240(18) 0.0427(9) Uani 1 1 d . . . H53A H 0.5674 0.6070 1.6138 0.051 Uiso 1 1 calc R . . H53B H 0.5918 0.5365 1.5935 0.051 Uiso 1 1 calc R . . C54 C 0.7119(3) 0.5923(2) 1.6047(2) 0.0498(10) Uani 1 1 d . . . H54A H 0.7278 0.6352 1.5898 0.060 Uiso 1 1 calc R . . H54B H 0.7510 0.5633 1.5765 0.060 Uiso 1 1 calc R . . C55 C 0.7412(3) 0.5841(2) 1.6915(2) 0.0557(11) Uani 1 1 d . . . H55A H 0.7191 0.5427 1.7073 0.067 Uiso 1 1 calc R . . H55B H 0.8134 0.5852 1.7014 0.067 Uiso 1 1 calc R . . C56 C 0.6992(3) 0.63296(19) 1.73966(18) 0.0465(9) Uani 1 1 d . . . H56A H 0.7226 0.6261 1.7935 0.070 Uiso 1 1 calc R . . H56B H 0.6276 0.6304 1.7329 0.070 Uiso 1 1 calc R . . H56C H 0.7198 0.6743 1.7240 0.070 Uiso 1 1 calc R . . N104 N 0.7691(2) 0.72187(15) 0.97800(18) 0.0440(7) Uani 1 1 d . . . N103 N 0.5516(2) 0.76565(13) 1.12924(16) 0.0386(6) Uani 1 1 d . . . N101 N 0.1022(2) 0.73256(16) 0.78642(19) 0.0463(8) Uani 1 1 d . . . N102 N 0.3045(2) 0.72365(13) 0.61091(16) 0.0384(6) Uani 1 1 d . . . C101 C 0.3571(2) 0.73712(12) 0.81215(16) 0.0234(5) Uani 1 1 d . . . C102 C 0.4573(2) 0.72973(12) 0.79667(16) 0.0248(5) Uani 1 1 d . . . H10A H 0.4720 0.7250 0.7455 0.030 Uiso 1 1 calc R . . C103 C 0.5309(2) 0.72950(13) 0.85432(16) 0.0255(6) Uani 1 1 d . . . H10B H 0.5963 0.7233 0.8431 0.031 Uiso 1 1 calc R . . C104 C 0.5116(2) 0.73847(12) 0.93222(16) 0.0248(6) Uani 1 1 d . . . C105 C 0.4113(2) 0.74705(13) 0.94738(16) 0.0257(6) Uani 1 1 d . . . H10C H 0.3970 0.7539 0.9983 0.031 Uiso 1 1 calc R . . C106 C 0.3374(2) 0.74557(13) 0.89038(16) 0.0256(6) Uani 1 1 d . . . H10D H 0.2718 0.7501 0.9019 0.031 Uiso 1 1 calc R . . C107 C 0.2809(2) 0.73487(13) 0.75386(17) 0.0267(6) Uani 1 1 d . . . C108 C 0.1812(2) 0.73490(15) 0.77113(18) 0.0330(7) Uani 1 1 d . . . C109 C 0.2952(2) 0.72910(13) 0.67499(17) 0.0288(6) Uani 1 1 d . . . C110 C 0.5858(2) 0.74016(13) 0.99157(17) 0.0274(6) Uani 1 1 d . . . C111 C 0.5661(2) 0.75387(14) 1.06825(17) 0.0302(6) Uani 1 1 d . . . C112 C 0.6874(2) 0.72965(14) 0.98277(18) 0.0314(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0447(5) 0.0306(4) 0.0161(3) 0.0010(3) 0.0017(3) -0.0026(3) S2 0.0322(4) 0.0397(4) 0.0189(3) 0.0002(3) 0.0078(3) -0.0079(3) S3 0.0200(3) 0.0266(3) 0.0164(3) -0.0012(2) 0.0016(2) 0.0003(2) S4 0.0178(3) 0.0273(3) 0.0179(3) -0.0009(2) 0.0033(2) -0.0004(2) C1 0.0240(13) 0.0185(11) 0.0160(11) -0.0014(9) 0.0024(9) 0.0003(9) C2 0.0205(12) 0.0188(11) 0.0153(11) -0.0005(9) 0.0023(9) -0.0018(9) C3 0.0170(11) 0.0199(11) 0.0144(10) 0.0003(9) 0.0025(9) -0.0012(9) C4 0.0171(11) 0.0191(11) 0.0154(11) -0.0004(9) 0.0019(9) 0.0004(9) C5 0.0172(11) 0.0207(11) 0.0148(11) -0.0006(9) 0.0006(9) 0.0011(9) C6 0.0202(12) 0.0204(12) 0.0153(11) -0.0023(9) 0.0003(9) 0.0025(9) C7 0.0281(14) 0.0203(12) 0.0149(11) -0.0009(9) 0.0041(10) -0.0004(10) C8 0.0269(14) 0.0262(13) 0.0170(11) -0.0009(10) 0.0058(10) -0.0051(10) C9 0.0239(13) 0.0254(13) 0.0199(12) -0.0020(10) 0.0046(10) -0.0054(10) C10 0.0195(12) 0.0221(12) 0.0193(12) -0.0016(9) 0.0034(9) -0.0020(9) C11 0.0157(12) 0.0251(12) 0.0209(12) -0.0014(10) 0.0023(9) -0.0026(9) C12 0.0159(12) 0.0237(12) 0.0211(12) -0.0016(10) 0.0017(9) -0.0028(9) C13 0.0162(11) 0.0203(11) 0.0148(11) 0.0015(9) 0.0010(9) -0.0014(9) C14 0.0191(12) 0.0200(11) 0.0151(11) 0.0023(9) 0.0020(9) -0.0016(9) C15 0.0202(12) 0.0190(11) 0.0131(10) 0.0001(9) -0.0003(9) -0.0021(9) C16 0.0194(12) 0.0173(11) 0.0156(11) 0.0004(9) 0.0028(9) -0.0008(9) C17 0.0169(12) 0.0215(12) 0.0169(11) -0.0007(9) 0.0045(9) -0.0012(9) C18 0.0177(12) 0.0220(12) 0.0206(12) -0.0001(9) 0.0028(9) 0.0015(9) C19 0.0168(12) 0.0234(12) 0.0184(11) -0.0009(9) -0.0003(9) 0.0008(9) C20 0.0183(12) 0.0266(13) 0.0225(12) -0.0057(10) -0.0041(10) 0.0053(10) C21 0.0197(13) 0.0286(13) 0.0212(12) -0.0066(10) -0.0043(10) 0.0067(10) C22 0.0217(13) 0.0256(13) 0.0186(12) -0.0056(10) -0.0013(10) 0.0050(10) C23 0.0283(14) 0.0230(12) 0.0158(11) -0.0040(9) -0.0030(10) 0.0059(10) C24 0.0341(15) 0.0207(12) 0.0153(11) -0.0006(9) 0.0023(10) 0.0027(11) C25 0.0256(14) 0.0354(15) 0.0274(14) -0.0037(12) 0.0073(11) -0.0087(12) C26 0.0278(15) 0.0358(16) 0.0228(13) -0.0030(11) 0.0078(11) -0.0110(12) C27 0.0207(13) 0.0339(15) 0.0258(13) -0.0045(11) 0.0062(11) -0.0026(11) C28 0.0169(13) 0.0346(15) 0.0371(16) -0.0013(13) 0.0031(11) 0.0008(11) C29 0.0183(13) 0.0337(15) 0.0300(15) 0.0009(12) -0.0017(11) 0.0011(11) C30 0.0191(12) 0.0256(13) 0.0239(13) 0.0002(10) 0.0019(10) -0.0007(10) C31 0.0184(12) 0.0246(12) 0.0174(11) -0.0011(9) 0.0013(9) -0.0039(9) C32 0.0187(12) 0.0226(12) 0.0165(11) 0.0004(9) -0.0011(9) 0.0000(9) C33 0.0157(11) 0.0244(12) 0.0235(12) 0.0025(10) 0.0003(9) 0.0012(10) C34 0.0169(12) 0.0254(13) 0.0228(12) -0.0009(10) -0.0006(10) 0.0009(10) C35 0.0195(13) 0.0363(16) 0.0319(15) -0.0082(12) 0.0011(11) 0.0021(11) C36 0.0182(14) 0.0450(18) 0.0433(18) -0.0146(15) -0.0035(12) -0.0013(12) C37 0.0234(15) 0.0446(18) 0.0381(17) -0.0153(14) -0.0083(12) 0.0023(13) C38 0.0254(14) 0.0374(16) 0.0253(14) -0.0113(12) -0.0065(11) 0.0065(12) C39 0.0342(16) 0.0297(14) 0.0197(12) -0.0047(11) -0.0055(11) 0.0111(12) C40 0.0468(19) 0.0238(13) 0.0185(12) -0.0020(10) -0.0063(12) 0.0067(12) C41 0.0323(16) 0.0485(19) 0.0270(15) 0.0001(13) 0.0111(12) -0.0133(14) C42 0.0291(16) 0.0409(17) 0.0315(15) 0.0022(13) 0.0108(12) -0.0025(13) C43 0.0299(16) 0.050(2) 0.0353(17) 0.0037(15) 0.0100(13) -0.0013(14) C44 0.070(3) 0.055(2) 0.055(2) -0.0069(19) 0.035(2) -0.007(2) C45 0.0282(14) 0.0254(13) 0.0172(12) -0.0028(10) -0.0006(10) 0.0006(11) C46 0.0290(14) 0.0262(13) 0.0173(12) 0.0006(10) -0.0002(10) -0.0022(11) C47 0.0351(16) 0.0351(15) 0.0165(12) -0.0009(11) 0.0046(11) -0.0020(12) C48 0.0338(16) 0.0431(18) 0.0217(13) -0.0024(12) -0.0015(12) -0.0028(13) C49 0.0175(12) 0.0304(14) 0.0250(13) -0.0022(11) 0.0042(10) 0.0011(10) C50 0.0213(13) 0.0404(16) 0.0224(13) 0.0006(12) 0.0043(10) 0.0011(12) C51 0.0240(15) 0.0522(19) 0.0267(15) -0.0053(13) 0.0084(12) -0.0006(13) C52 0.042(2) 0.088(3) 0.0360(19) -0.002(2) 0.0182(17) -0.001(2) C53 0.067(3) 0.0320(17) 0.0250(15) -0.0004(13) -0.0117(15) 0.0041(16) C54 0.044(2) 0.076(3) 0.0300(17) 0.0018(17) 0.0058(15) 0.0168(19) C55 0.047(2) 0.087(3) 0.0312(18) 0.0055(19) -0.0033(16) 0.020(2) C56 0.056(2) 0.060(2) 0.0210(15) -0.0023(15) -0.0093(15) 0.0138(19) N104 0.0333(16) 0.0515(18) 0.0461(17) 0.0230(14) -0.0016(13) -0.0024(13) N103 0.0451(17) 0.0409(16) 0.0286(14) 0.0016(11) -0.0017(12) -0.0096(13) N101 0.0278(15) 0.062(2) 0.0483(18) 0.0126(15) -0.0005(13) 0.0039(14) N102 0.0451(17) 0.0373(15) 0.0317(14) 0.0009(11) -0.0008(12) 0.0007(12) C101 0.0261(14) 0.0197(12) 0.0243(13) 0.0005(10) 0.0027(10) 0.0000(10) C102 0.0302(15) 0.0229(13) 0.0218(13) -0.0003(10) 0.0052(11) 0.0001(11) C103 0.0265(14) 0.0240(13) 0.0264(13) 0.0012(10) 0.0042(11) -0.0009(11) C104 0.0314(15) 0.0204(12) 0.0227(13) 0.0045(10) 0.0036(11) -0.0026(11) C105 0.0321(15) 0.0231(13) 0.0229(13) 0.0008(10) 0.0068(11) -0.0019(11) C106 0.0263(14) 0.0237(13) 0.0279(14) 0.0021(11) 0.0075(11) -0.0014(11) C107 0.0263(14) 0.0236(13) 0.0295(14) 0.0024(11) 0.0003(11) 0.0006(11) C108 0.0307(16) 0.0349(16) 0.0321(16) 0.0055(12) -0.0022(12) 0.0019(13) C109 0.0298(15) 0.0255(14) 0.0295(15) 0.0019(11) -0.0046(12) 0.0010(11) C110 0.0307(15) 0.0243(13) 0.0267(14) 0.0060(11) 0.0009(11) -0.0046(11) C111 0.0350(16) 0.0292(15) 0.0249(14) 0.0059(11) -0.0041(12) -0.0082(12) C112 0.0329(17) 0.0320(15) 0.0283(15) 0.0110(12) -0.0018(12) -0.0048(12) _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 C40 1.730(3) . ? S1 C24 1.739(3) . ? S2 C8 1.729(3) . ? S2 C25 1.740(3) . ? S3 C32 1.732(3) . ? S3 C15 1.733(2) . ? S4 C17 1.735(2) . ? S4 C33 1.743(3) . ? C1 C7 1.421(3) . ? C1 C6 1.433(4) . ? C1 C2 1.442(4) . ? C2 C10 1.418(4) . ? C2 C3 1.443(3) . ? C3 C13 1.413(3) . ? C3 C4 1.443(3) . ? C4 C16 1.417(3) . ? C4 C5 1.441(3) . ? C5 C19 1.401(4) . ? C5 C6 1.443(3) . ? C6 C22 1.414(3) . ? C7 C8 1.420(4) . ? C7 C24 1.430(4) . ? C8 C9 1.406(4) . ? C9 C10 1.433(4) . ? C9 C26 1.449(4) . ? C10 C11 1.457(4) . ? C11 C27 1.419(4) . ? C11 C12 1.424(4) . ? C12 C30 1.417(4) . ? C12 C13 1.449(4) . ? C13 C14 1.434(3) . ? C14 C15 1.400(4) . ? C14 C31 1.448(3) . ? C15 C16 1.422(3) . ? C16 C17 1.429(3) . ? C17 C18 1.398(4) . ? C18 C19 1.423(3) . ? C18 C34 1.439(4) . ? C19 C20 1.455(4) . ? C20 C21 1.415(4) . ? C20 C35 1.416(4) . ? C21 C38 1.414(4) . ? C21 C22 1.450(4) . ? C22 C23 1.434(4) . ? C23 C24 1.399(4) . ? C23 C39 1.448(4) . ? C25 C26 1.360(4) . ? C25 C41 1.495(4) . ? C27 C28 1.376(4) . ? C28 C29 1.394(4) . ? C29 C30 1.383(4) . ? C31 C32 1.368(4) . ? C32 C45 1.498(4) . ? C33 C34 1.356(4) . ? C33 C49 1.495(4) . ? C35 C36 1.380(4) . ? C36 C37 1.399(5) . ? C37 C38 1.372(5) . ? C39 C40 1.361(4) . ? C40 C53 1.513(4) . ? C41 C42 1.521(4) . ? C42 C43 1.521(4) . ? C43 C44 1.513(5) . ? C45 C46 1.526(4) . ? C46 C47 1.524(4) . ? C47 C48 1.513(4) . ? C49 C50 1.524(4) . ? C50 C51 1.526(4) . ? C51 C52 1.520(5) . ? C53 C54 1.484(6) . ? C54 C55 1.549(5) . ? C55 C56 1.502(5) . ? N104 C112 1.148(4) . ? N103 C111 1.141(4) . ? N101 C108 1.147(4) . ? N102 C109 1.155(4) . ? C101 C107 1.387(4) . ? C101 C102 1.441(4) . ? C101 C106 1.443(4) . ? C102 C103 1.356(4) . ? C103 C104 1.438(4) . ? C104 C110 1.382(4) . ? C104 C105 1.443(4) . ? C105 C106 1.351(4) . ? C107 C109 1.428(4) . ? C107 C108 1.435(4) . ? C110 C111 1.435(4) . ? C110 C112 1.439(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 S1 C24 91.97(14) . . ? C8 S2 C25 92.20(14) . . ? C32 S3 C15 91.90(12) . . ? C17 S4 C33 92.06(13) . . ? C7 C1 C6 119.7(2) . . ? C7 C1 C2 120.0(2) . . ? C6 C1 C2 120.3(2) . . ? C10 C2 C1 120.6(2) . . ? C10 C2 C3 120.1(2) . . ? C1 C2 C3 119.2(2) . . ? C13 C3 C2 120.0(2) . . ? C13 C3 C4 120.2(2) . . ? C2 C3 C4 119.7(2) . . ? C16 C4 C5 120.0(2) . . ? C16 C4 C3 120.3(2) . . ? C5 C4 C3 119.6(2) . . ? C19 C5 C4 120.1(2) . . ? C19 C5 C6 120.2(2) . . ? C4 C5 C6 119.6(2) . . ? C22 C6 C1 121.2(2) . . ? C22 C6 C5 119.3(2) . . ? C1 C6 C5 119.5(2) . . ? C1 C7 C8 118.0(2) . . ? C1 C7 C24 117.7(2) . . ? C8 C7 C24 124.2(2) . . ? C9 C8 C7 122.5(2) . . ? C9 C8 S2 111.9(2) . . ? C7 C8 S2 125.5(2) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 C26 110.3(2) . . ? C10 C9 C26 130.1(3) . . ? C2 C10 C9 118.4(2) . . ? C2 C10 C11 117.8(2) . . ? C9 C10 C11 123.7(2) . . ? C27 C11 C12 117.6(2) . . ? C27 C11 C10 122.3(2) . . ? C12 C11 C10 119.8(2) . . ? C30 C12 C11 119.1(2) . . ? C30 C12 C13 121.2(2) . . ? C11 C12 C13 119.5(2) . . ? C3 C13 C14 118.7(2) . . ? C3 C13 C12 118.3(2) . . ? C14 C13 C12 123.0(2) . . ? C15 C14 C13 119.4(2) . . ? C15 C14 C31 111.1(2) . . ? C13 C14 C31 129.3(2) . . ? C14 C15 C16 122.7(2) . . ? C14 C15 S3 111.75(18) . . ? C16 C15 S3 125.5(2) . . ? C4 C16 C15 117.7(2) . . ? C4 C16 C17 117.6(2) . . ? C15 C16 C17 124.6(2) . . ? C18 C17 C16 122.1(2) . . ? C18 C17 S4 111.08(19) . . ? C16 C17 S4 126.77(19) . . ? C17 C18 C19 119.4(2) . . ? C17 C18 C34 111.6(2) . . ? C19 C18 C34 128.9(2) . . ? C5 C19 C18 119.1(2) . . ? C5 C19 C20 117.8(2) . . ? C18 C19 C20 123.0(2) . . ? C21 C20 C35 119.2(2) . . ? C21 C20 C19 119.6(2) . . ? C35 C20 C19 120.8(3) . . ? C38 C21 C20 117.8(3) . . ? C38 C21 C22 122.7(3) . . ? C20 C21 C22 119.1(2) . . ? C6 C22 C23 118.2(2) . . ? C6 C22 C21 118.4(2) . . ? C23 C22 C21 123.3(2) . . ? C24 C23 C22 119.3(2) . . ? C24 C23 C39 110.6(3) . . ? C22 C23 C39 130.0(3) . . ? C23 C24 C7 122.6(2) . . ? C23 C24 S1 111.7(2) . . ? C7 C24 S1 125.7(2) . . ? C26 C25 C41 129.7(3) . . ? C26 C25 S2 111.2(2) . . ? C41 C25 S2 119.2(2) . . ? C25 C26 C9 114.4(3) . . ? C28 C27 C11 122.0(3) . . ? C27 C28 C29 120.2(3) . . ? C30 C29 C28 119.6(3) . . ? C29 C30 C12 121.4(3) . . ? C32 C31 C14 113.1(2) . . ? C31 C32 C45 128.6(2) . . ? C31 C32 S3 112.02(19) . . ? C45 C32 S3 119.4(2) . . ? C34 C33 C49 126.7(2) . . ? C34 C33 S4 111.3(2) . . ? C49 C33 S4 121.8(2) . . ? C33 C34 C18 113.9(2) . . ? C36 C35 C20 121.3(3) . . ? C35 C36 C37 119.6(3) . . ? C38 C37 C36 119.9(3) . . ? C37 C38 C21 122.2(3) . . ? C40 C39 C23 114.0(3) . . ? C39 C40 C53 131.3(3) . . ? C39 C40 S1 111.7(2) . . ? C53 C40 S1 117.0(3) . . ? C25 C41 C42 113.3(3) . . ? C41 C42 C43 113.6(3) . . ? C44 C43 C42 112.6(3) . . ? C32 C45 C46 112.9(2) . . ? C47 C46 C45 113.9(2) . . ? C48 C47 C46 114.0(2) . . ? C33 C49 C50 115.8(2) . . ? C49 C50 C51 110.6(2) . . ? C52 C51 C50 113.6(3) . . ? C54 C53 C40 113.3(3) . . ? C53 C54 C55 112.8(3) . . ? C56 C55 C54 113.8(3) . . ? C107 C101 C102 121.2(3) . . ? C107 C101 C106 120.5(3) . . ? C102 C101 C106 118.3(3) . . ? C103 C102 C101 120.8(3) . . ? C102 C103 C104 121.0(3) . . ? C110 C104 C103 121.9(3) . . ? C110 C104 C105 120.0(3) . . ? C103 C104 C105 118.0(3) . . ? C106 C105 C104 121.2(3) . . ? C105 C106 C101 120.7(3) . . ? C101 C107 C109 123.5(3) . . ? C101 C107 C108 120.4(3) . . ? C109 C107 C108 116.0(3) . . ? N101 C108 C107 177.1(4) . . ? N102 C109 C107 178.2(3) . . ? C104 C110 C111 121.3(3) . . ? C104 C110 C112 124.2(3) . . ? C111 C110 C112 114.5(3) . . ? N103 C111 C110 178.8(3) . . ? N104 C112 C110 177.9(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.677 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.099 # Attachment '- 1b_c60.cif' data_fw60s10 _database_code_depnum_ccdc_archive 'CCDC 817724' #TrackingRef '- 1b_c60.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C310 H64 S4' _chemical_formula_weight 3915.85 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' 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 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 22.514(5) _cell_length_b 19.373(4) _cell_length_c 19.548(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.901(3) _cell_angle_gamma 90.00 _cell_volume 8066(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6907 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 20.40 _exptl_crystal_description PLATE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9721 _exptl_absorpt_correction_T_max 0.9972 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 111637 _diffrn_reflns_av_R_equivalents 0.2303 _diffrn_reflns_av_sigmaI/netI 0.1915 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.28 _reflns_number_total 20019 _reflns_number_gt 7325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The C60's were modeled using the FRAG command, with bond lengths fixed at 1.458 (bonds fusing 5 and 6) and 1.401 (bonds fusing 6 and 6). SIMU and DELU restraints were applied to all atoms in the crystal structure. ; _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^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20019 _refine_ls_number_parameters 1066 _refine_ls_number_restraints 5004 _refine_ls_R_factor_all 0.3184 _refine_ls_R_factor_gt 0.1623 _refine_ls_wR_factor_ref 0.4275 _refine_ls_wR_factor_gt 0.3811 _refine_ls_goodness_of_fit_ref 1.724 _refine_ls_restrained_S_all 1.634 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6857(2) 1.1754(3) -0.28329(10) 0.123(5) Uani 1 1 d GU . . C2 C 0.6300(2) 1.2036(3) -0.27086(14) 0.143(6) Uani 1 1 d GU . . C3 C 0.59844(16) 1.1474(3) -0.24684(18) 0.148(6) Uani 1 1 d GU . . C4 C 0.6347(2) 1.0845(3) -0.24445(19) 0.114(5) Uani 1 1 d GU . . C5 C 0.6886(2) 1.1018(3) -0.26697(15) 0.140(5) Uani 1 1 d GU . . C6 C 0.6224(2) 1.2651(3) -0.2369(2) 0.127(5) Uani 1 1 d GU . . C7 C 0.6776(2) 1.3095(2) -0.2190(2) 0.155(6) Uani 1 1 d GU . . C8 C 0.6842(2) 1.34301(14) -0.1501(3) 0.148(6) Uani 1 1 d GU . . C9 C 0.6331(2) 1.31927(18) -0.1255(3) 0.163(6) Uani 1 1 d GU . . C10 C 0.59493(16) 1.2711(2) -0.1792(3) 0.153(6) Uani 1 1 d GU . . C11 C 0.7332(2) 1.2253(3) -0.26260(15) 0.145(5) Uani 1 1 d GU . . C12 C 0.7356(3) 1.2912(2) -0.2258(2) 0.141(6) Uani 1 1 d GU . . C13 C 0.7988(2) 1.2999(2) -0.1749(3) 0.151(6) Uani 1 1 d GU . . C14 C 0.8355(2) 1.2392(3) -0.1802(2) 0.115(4) Uani 1 1 d GU . . C15 C 0.7949(2) 1.1932(3) -0.2344(2) 0.142(5) Uani 1 1 d GU . . C16 C 0.8040(2) 1.1225(3) -0.2197(2) 0.128(5) Uani 1 1 d GU . . C17 C 0.84950(18) 1.0980(2) -0.1525(3) 0.116(5) Uani 1 1 d GU . . C18 C 0.8235(2) 1.0368(2) -0.1293(3) 0.109(4) Uani 1 1 d GU . . C19 C 0.7619(2) 1.02350(18) -0.1822(3) 0.104(4) Uani 1 1 d GU . . C20 C 0.7499(2) 1.0765(2) -0.2380(2) 0.118(5) Uani 1 1 d GU . . C21 C 0.87842(15) 1.2203(3) -0.1133(3) 0.100(4) Uani 1 1 d GU . . C22 C 0.88593(13) 1.1459(3) -0.1029(3) 0.119(4) Uani 1 1 d GU . . C23 C 0.89348(10) 1.1309(3) -0.0274(3) 0.111(4) Uani 1 1 d GU . . C24 C 0.89065(11) 1.1960(3) 0.0088(2) 0.123(5) Uani 1 1 d GU . . C25 C 0.88134(14) 1.2513(2) -0.0443(3) 0.099(4) Uani 1 1 d GU . . C26 C 0.7285(3) 1.0555(2) 0.0467(2) 0.141(6) Uani 1 1 d GU . . C27 C 0.7276(2) 1.1217(3) 0.08178(15) 0.149(6) Uani 1 1 d GU . . C28 C 0.6651(2) 1.1513(3) 0.0508(2) 0.146(5) Uani 1 1 d GU . . C29 C 0.6273(2) 1.1033(3) -0.0033(3) 0.117(5) Uani 1 1 d GU . . C30 C 0.6665(2) 1.0441(2) -0.0058(3) 0.159(6) Uani 1 1 d GU . . C31 C 0.7777(2) 1.1686(3) 0.10202(10) 0.104(4) Uani 1 1 d GU . . C32 C 0.8336(2) 1.1414(3) 0.08922(14) 0.138(5) Uani 1 1 d GU . . C33 C 0.86391(16) 1.1981(3) 0.06426(18) 0.129(5) Uani 1 1 d GU . . C34 C 0.8268(2) 1.2603(2) 0.06164(18) 0.113(5) Uani 1 1 d GU . . C35 C 0.7735(2) 1.2420(3) 0.08497(15) 0.131(5) Uani 1 1 d GU . . C36 C 0.7092(2) 1.00051(14) -0.1655(3) 0.114(4) Uani 1 1 d GU . . C37 C 0.6463(2) 1.0295(2) -0.1953(3) 0.116(5) Uani 1 1 d GU . . C38 C 0.62042(19) 1.0371(2) -0.1363(3) 0.143(5) Uani 1 1 d GU . . C39 C 0.6673(2) 1.01270(15) -0.0701(3) 0.129(5) Uani 1 1 d GU . . C40 C 0.7222(3) 0.99010(10) -0.0882(3) 0.140(5) Uani 1 1 d GU . . C41 C 0.84215(19) 1.30600(19) -0.0397(3) 0.131(5) Uani 1 1 d GU . . C42 C 0.8011(2) 1.33085(15) -0.1094(3) 0.133(5) Uani 1 1 d GU . . C43 C 0.7434(3) 1.35601(10) -0.0995(3) 0.150(6) Uani 1 1 d GU . . C44 C 0.7488(2) 1.34672(13) -0.0237(3) 0.124(5) Uani 1 1 d GU . . C45 C 0.8098(2) 1.31581(19) 0.0133(2) 0.113(4) Uani 1 1 d GU . . C46 C 0.56986(10) 1.2141(3) -0.1540(3) 0.130(5) Uani 1 1 d GU . . C47 C 0.57222(11) 1.1492(3) -0.1909(2) 0.135(5) Uani 1 1 d GU . . C48 C 0.58081(14) 1.0934(3) -0.1386(3) 0.124(5) Uani 1 1 d GU . . C49 C 0.58378(15) 1.1237(3) -0.0693(3) 0.128(5) Uani 1 1 d GU . . C50 C 0.57701(13) 1.1983(3) -0.0788(3) 0.127(5) Uani 1 1 d GU . . C51 C 0.61212(18) 1.2489(3) -0.0317(3) 0.131(5) Uani 1 1 d GU . . C52 C 0.6573(2) 1.2218(3) 0.0344(2) 0.125(5) Uani 1 1 d GU . . C53 C 0.7121(2) 1.2668(2) 0.0544(2) 0.124(5) Uani 1 1 d GU . . C54 C 0.7008(2) 1.32182(18) 0.0008(3) 0.123(5) Uani 1 1 d GU . . C55 C 0.6390(2) 1.3107(2) -0.0524(3) 0.133(5) Uani 1 1 d GU . . C56 C 0.8390(2) 1.0809(2) 0.0525(2) 0.117(5) Uani 1 1 d GU . . C57 C 0.7843(2) 1.0358(2) 0.0350(2) 0.148(6) Uani 1 1 d GU . . C58 C 0.7791(2) 1.00032(13) -0.0325(3) 0.131(5) Uani 1 1 d GU . . C59 C 0.8306(2) 1.02345(18) -0.0567(3) 0.139(5) Uani 1 1 d GU . . C60 C 0.86767(16) 1.0732(2) -0.0041(3) 0.144(6) Uani 1 1 d GU . . C101 C 0.24401(19) 1.2648(3) -0.18844(16) 0.133(5) Uani 1 1 d GU . . C102 C 0.19571(14) 1.2926(3) -0.16134(19) 0.120(5) Uani 1 1 d GU . . C103 C 0.18995(15) 1.2465(3) -0.1049(3) 0.118(5) Uani 1 1 d GU . . C104 C 0.2347(2) 1.1903(2) -0.0970(3) 0.161(6) Uani 1 1 d GU . . C105 C 0.2681(2) 1.2016(2) -0.1487(2) 0.129(5) Uani 1 1 d GU . . C106 C 0.18476(14) 1.3608(3) -0.14483(19) 0.128(5) Uani 1 1 d GU . . C107 C 0.2243(2) 1.4107(3) -0.16563(18) 0.142(5) Uani 1 1 d GU . . C108 C 0.2411(2) 1.4648(2) -0.1109(2) 0.136(5) Uani 1 1 d GU . . C109 C 0.2120(2) 1.4483(2) -0.0562(3) 0.143(5) Uani 1 1 d GU . . C110 C 0.17721(13) 1.3840(3) -0.0772(2) 0.125(5) Uani 1 1 d GU . . C111 C 0.2768(2) 1.3203(3) -0.20504(10) 0.118(5) Uani 1 1 d GU . . C112 C 0.2737(2) 1.3940(3) -0.19143(15) 0.136(5) Uani 1 1 d GU . . C113 C 0.3373(3) 1.4216(3) -0.1707(2) 0.147(5) Uani 1 1 d GU . . C114 C 0.3798(2) 1.3650(3) -0.17156(19) 0.129(5) Uani 1 1 d GU . . C115 C 0.3424(2) 1.3024(3) -0.19276(13) 0.106(4) Uani 1 1 d GU . . C116 C 0.3704(2) 1.2416(3) -0.15826(19) 0.128(5) Uani 1 1 d GU . . C117 C 0.43185(19) 1.2428(3) -0.1026(2) 0.119(5) Uani 1 1 d GU . . C118 C 0.4315(2) 1.1921(2) -0.0476(3) 0.189(7) Uani 1 1 d GU . . C119 C 0.3698(3) 1.15957(16) -0.0693(3) 0.134(5) Uani 1 1 d GU . . C120 C 0.3320(2) 1.1902(2) -0.1377(2) 0.165(6) Uani 1 1 d GU . . C121 C 0.4378(2) 1.3712(3) -0.1168(3) 0.153(6) Uani 1 1 d GU . . C122 C 0.46420(16) 1.3055(3) -0.0847(2) 0.138(5) Uani 1 1 d GU . . C123 C 0.49500(11) 1.3165(3) -0.0075(3) 0.155(6) Uani 1 1 d GU . . C124 C 0.48766(14) 1.3890(3) 0.0081(3) 0.154(6) Uani 1 1 d GU . . C125 C 0.4523(2) 1.4228(3) -0.0595(3) 0.159(6) Uani 1 1 d GU . . C126 C 0.3994(2) 1.2628(3) 0.16326(14) 0.129(5) Uani 1 1 d GU . . C127 C 0.3930(2) 1.3361(3) 0.17645(10) 0.123(5) Uani 1 1 d GU . . C128 C 0.3266(2) 1.3506(3) 0.16267(13) 0.108(4) Uani 1 1 d GU . . C129 C 0.2919(2) 1.2864(3) 0.14097(18) 0.133(5) Uani 1 1 d GU . . C130 C 0.3369(3) 1.2321(3) 0.1413(2) 0.142(5) Uani 1 1 d GU . . C131 C 0.42848(19) 1.3887(3) 0.15933(17) 0.142(5) Uani 1 1 d GU . . C132 C 0.47662(14) 1.3618(3) 0.1315(2) 0.141(6) Uani 1 1 d GU . . C133 C 0.48101(15) 1.4079(3) 0.0744(3) 0.141(6) Uani 1 1 d GU . . C134 C 0.4356(2) 1.4634(2) 0.0670(3) 0.161(6) Uani 1 1 d GU . . C135 C 0.4031(2) 1.4515(2) 0.1195(2) 0.143(6) Uani 1 1 d GU . . C136 C 0.3370(3) 1.14112(10) -0.0222(3) 0.152(6) Uani 1 1 d GU . . C137 C 0.2708(3) 1.15560(15) -0.0344(3) 0.180(7) Uani 1 1 d GU . . C138 C 0.2645(3) 1.1807(2) 0.0332(3) 0.164(6) Uani 1 1 d GU . . C139 C 0.3269(3) 1.18180(19) 0.0873(3) 0.163(6) Uani 1 1 d GU . . C140 C 0.3716(3) 1.15731(15) 0.0530(3) 0.141(6) Uani 1 1 d GU . . C141 C 0.4090(3) 1.4736(2) -0.0563(3) 0.168(6) Uani 1 1 d GU . . C142 C 0.3503(3) 1.4721(2) -0.1166(3) 0.172(6) Uani 1 1 d GU . . C143 C 0.3004(3) 1.49618(15) -0.0902(3) 0.145(5) Uani 1 1 d GU . . C144 C 0.3282(3) 1.51257(10) -0.0136(3) 0.171(6) Uani 1 1 d GU . . C145 C 0.3953(3) 1.49861(15) 0.0073(3) 0.177(7) Uani 1 1 d GU . . C146 C 0.17722(11) 1.3378(3) -0.0220(2) 0.149(6) Uani 1 1 d GU . . C147 C 0.18388(13) 1.2653(3) -0.0382(3) 0.143(5) Uani 1 1 d GU . . C148 C 0.2186(2) 1.2308(3) 0.0291(3) 0.146(6) Uani 1 1 d GU . . C149 C 0.2333(2) 1.2819(3) 0.0869(2) 0.165(6) Uani 1 1 d GU . . C150 C 0.20779(16) 1.3480(3) 0.0553(2) 0.140(5) Uani 1 1 d GU . . C151 C 0.2377(2) 1.4123(3) 0.0703(2) 0.118(5) Uani 1 1 d GU . . C152 C 0.2993(2) 1.4107(3) 0.12590(19) 0.128(5) Uani 1 1 d GU . . C153 C 0.3389(2) 1.4619(2) 0.1071(2) 0.178(6) Uani 1 1 d GU . . C154 C 0.3018(3) 1.49510(16) 0.0399(3) 0.136(5) Uani 1 1 d GU . . C155 C 0.2393(2) 1.4645(2) 0.0172(3) 0.178(6) Uani 1 1 d GU . . C156 C 0.48486(13) 1.2935(3) 0.1127(2) 0.135(5) Uani 1 1 d GU . . C157 C 0.4460(2) 1.2432(3) 0.13400(18) 0.139(5) Uani 1 1 d GU . . C158 C 0.4311(2) 1.1877(2) 0.0807(2) 0.151(6) Uani 1 1 d GU . . C159 C 0.4608(2) 1.2038(2) 0.0265(3) 0.143(6) Uani 1 1 d GU . . C160 C 0.49400(12) 1.2691(3) 0.0462(2) 0.131(5) Uani 1 1 d GU . . C201 C 0.4527(4) 0.5628(5) 0.3303(6) 0.079(3) Uani 1 1 d U . . H20A H 0.4955 0.5508 0.3606 0.118 Uiso 1 1 calc R . . H20B H 0.4417 0.6085 0.3442 0.118 Uiso 1 1 calc R . . H20C H 0.4505 0.5635 0.2794 0.118 Uiso 1 1 calc R . . C202 C 0.4069(3) 0.5094(4) 0.3409(5) 0.0418(18) Uani 1 1 d U . . H20D H 0.4109 0.5074 0.3928 0.050 Uiso 1 1 calc R . . H20E H 0.4182 0.4634 0.3267 0.050 Uiso 1 1 calc R . . C203 C 0.3388(3) 0.5252(4) 0.2970(4) 0.0357(16) Uani 1 1 d U . . H20F H 0.3346 0.5276 0.2451 0.043 Uiso 1 1 calc R . . H20G H 0.3271 0.5708 0.3116 0.043 Uiso 1 1 calc R . . C204 C 0.2271(3) 0.4746(4) 0.2594(4) 0.0283(14) Uani 1 1 d U . . C205 C 0.0484(3) 0.8803(3) 0.3448(4) 0.0274(15) Uani 1 1 d U . . H20H H 0.0512 0.8521 0.3880 0.033 Uiso 1 1 calc R . . H20I H 0.0056 0.9002 0.3267 0.033 Uiso 1 1 calc R . . C206 C -0.0785(3) 0.8003(4) -0.0787(4) 0.0296(14) Uani 1 1 d U . . H20J H -0.0758 0.8491 -0.0737 0.036 Uiso 1 1 calc R . . C207 C 0.2937(3) 0.4700(4) 0.3082(4) 0.0321(15) Uani 1 1 d U . . H20K H 0.3103 0.4240 0.3016 0.039 Uiso 1 1 calc R . . H20L H 0.2940 0.4728 0.3588 0.039 Uiso 1 1 calc R . . C208 C 0.1229(3) 0.5203(3) 0.1802(3) 0.0190(12) Uani 1 1 d U . . C209 C -0.1118(3) 0.7722(3) -0.1448(4) 0.0262(13) Uani 1 1 d U . . H20M H -0.1326 0.8015 -0.1842 0.031 Uiso 1 1 calc R . . C210 C 0.0959(4) 0.9387(4) 0.3666(4) 0.0390(19) Uani 1 1 d U . . H21A H 0.0878 0.9664 0.4045 0.059 Uiso 1 1 calc R . . H21B H 0.0922 0.9678 0.3245 0.059 Uiso 1 1 calc R . . H21C H 0.1384 0.9193 0.3848 0.059 Uiso 1 1 calc R . . C211 C -0.0204(3) 0.6406(3) 0.0306(3) 0.0153(10) Uani 1 1 d U . . C212 C -0.1337(3) 0.5489(3) -0.1651(3) 0.0165(12) Uani 1 1 d U . . C213 C 0.0583(3) 0.8342(3) 0.2871(4) 0.0245(13) Uani 1 1 d U . . H21D H 0.1014 0.8150 0.3047 0.029 Uiso 1 1 calc R . . H21E H 0.0544 0.8621 0.2435 0.029 Uiso 1 1 calc R . . C214 C 0.0112(3) 0.7750(3) 0.2669(4) 0.0241(13) Uani 1 1 d U . . H21F H 0.0136 0.7495 0.3116 0.029 Uiso 1 1 calc R . . H21G H -0.0315 0.7949 0.2477 0.029 Uiso 1 1 calc R . . C215 C -0.1148(3) 0.7027(3) -0.1537(3) 0.0207(12) Uani 1 1 d U . . H21H H -0.1358 0.6844 -0.2004 0.025 Uiso 1 1 calc R . . C216 C -0.0453(3) 0.5413(3) -0.0532(3) 0.0162(11) Uani 1 1 d U . . C217 C -0.0539(3) 0.6849(3) -0.0269(3) 0.0180(11) Uani 1 1 d U . . C218 C 0.0710(3) 0.5584(3) 0.1356(3) 0.0167(11) Uani 1 1 d U . . C219 C -0.0506(3) 0.7615(3) -0.0226(3) 0.0129(11) Uani 1 1 d U . . H21I H -0.0278 0.7829 0.0219 0.016 Uiso 1 1 calc R . . C220 C -0.1941(3) 0.5729(3) -0.2122(3) 0.0175(13) Uani 1 1 d U . . H22A H -0.2091 0.6183 -0.2099 0.021 Uiso 1 1 calc R . . C221 C 0.0192(3) 0.7243(3) 0.2127(3) 0.0197(12) Uani 1 1 d U . . C222 C 0.0359(3) 0.5297(3) 0.0679(3) 0.0150(11) Uani 1 1 d U . . C223 C -0.0141(3) 0.7250(3) 0.1398(3) 0.0113(11) Uani 1 1 d U . . H22B H -0.0443 0.7586 0.1156 0.014 Uiso 1 1 calc R . . C224 C 0.0510(3) 0.6230(3) 0.1542(3) 0.0172(11) Uani 1 1 d U . . C225 C -0.0893(3) 0.5832(3) -0.1055(3) 0.0163(11) Uani 1 1 d U . . C226 C -0.0094(3) 0.5714(3) 0.0157(3) 0.0160(11) Uani 1 1 d U . . C227 C 0.0057(3) 0.6629(3) 0.1044(3) 0.0174(11) Uani 1 1 d U . . C228 C -0.0876(3) 0.6565(3) -0.0960(3) 0.0166(10) Uani 1 1 d U . . C301 C 0.0785(4) 1.0895(4) -0.0965(5) 0.044(2) Uani 1 1 d . . . H30A H 0.1066 1.1246 -0.0715 0.053 Uiso 1 1 calc R . . C302 C -0.0076(4) 1.0116(4) -0.1052(5) 0.039(2) Uani 1 1 d . . . H30B H -0.0379 0.9937 -0.0857 0.047 Uiso 1 1 calc R . . C303 C -0.0480(4) 0.9306(4) -0.2081(5) 0.052(2) Uani 1 1 d . . . H30C H -0.0768 0.9196 -0.1812 0.078 Uiso 1 1 calc R . . H30D H -0.0239 0.8893 -0.2113 0.078 Uiso 1 1 calc R . . H30E H -0.0722 0.9461 -0.2569 0.078 Uiso 1 1 calc R . . C304 C 0.0334(4) 1.0633(4) -0.0686(4) 0.049(2) Uani 1 1 d . . . H30F H 0.0307 1.0808 -0.0244 0.058 Uiso 1 1 calc R . . C305 C 0.0412(4) 1.0126(4) -0.1974(4) 0.041(2) Uani 1 1 d . . . H30G H 0.0442 0.9950 -0.2415 0.049 Uiso 1 1 calc R . . C306 C 0.0815(4) 1.0632(4) -0.1613(5) 0.050(2) Uani 1 1 d . . . H30H H 0.1120 1.0807 -0.1809 0.060 Uiso 1 1 calc R . . C307 C -0.0043(4) 0.9865(4) -0.1700(4) 0.0323(18) Uani 1 1 d . . . S1 S 0.18495(9) 0.55279(9) 0.25093(9) 0.0291(5) Uani 1 1 d . . . S2 S 0.07438(9) 0.65923(9) 0.23965(9) 0.0278(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.179(13) 0.156(12) 0.024(6) -0.013(7) 0.019(8) -0.035(10) C2 0.176(13) 0.184(13) 0.030(7) 0.015(8) -0.019(8) 0.003(12) C3 0.095(10) 0.215(14) 0.070(9) 0.002(10) -0.061(7) -0.007(10) C4 0.117(10) 0.131(10) 0.073(8) -0.067(7) 0.002(7) -0.069(8) C5 0.198(13) 0.149(11) 0.059(8) -0.065(8) 0.021(9) -0.007(11) C6 0.113(10) 0.164(12) 0.073(8) 0.072(8) -0.013(8) 0.057(9) C7 0.203(14) 0.116(11) 0.118(11) 0.081(9) 0.016(11) 0.042(11) C8 0.210(14) 0.063(8) 0.152(12) 0.063(8) 0.035(11) 0.055(9) C9 0.180(13) 0.118(11) 0.193(13) 0.007(10) 0.062(11) 0.129(9) C10 0.122(11) 0.173(13) 0.134(12) 0.041(10) -0.001(9) 0.107(9) C11 0.165(12) 0.229(14) 0.048(7) 0.056(9) 0.047(8) -0.005(11) C12 0.190(13) 0.123(10) 0.109(10) 0.090(8) 0.045(10) -0.023(10) C13 0.159(12) 0.135(12) 0.177(13) 0.067(10) 0.077(11) -0.050(10) C14 0.110(10) 0.148(11) 0.124(10) 0.013(9) 0.087(8) -0.043(8) C15 0.139(11) 0.244(14) 0.078(9) 0.007(10) 0.083(8) -0.026(11) C16 0.177(12) 0.151(11) 0.109(10) -0.040(9) 0.121(9) -0.027(10) C17 0.072(8) 0.160(11) 0.137(10) -0.080(9) 0.064(8) 0.008(8) C18 0.112(10) 0.076(8) 0.151(11) -0.042(8) 0.058(9) 0.040(7) C19 0.131(10) 0.060(7) 0.140(11) -0.061(7) 0.068(9) -0.003(7) C20 0.150(11) 0.144(11) 0.073(8) -0.086(7) 0.055(8) -0.011(9) C21 0.064(8) 0.123(10) 0.130(10) -0.007(9) 0.054(7) -0.017(7) C22 0.049(7) 0.165(11) 0.159(11) -0.033(10) 0.055(8) 0.000(8) C23 0.039(6) 0.134(11) 0.157(11) 0.038(9) 0.026(8) 0.045(7) C24 0.032(6) 0.215(13) 0.098(9) -0.007(10) -0.013(6) -0.026(8) C25 0.049(7) 0.111(9) 0.136(10) -0.007(8) 0.028(7) -0.053(6) C26 0.173(12) 0.118(10) 0.132(11) 0.103(9) 0.049(10) -0.001(10) C27 0.209(14) 0.200(13) 0.037(7) 0.054(8) 0.038(9) -0.013(12) C28 0.145(11) 0.262(14) 0.069(8) 0.042(9) 0.087(8) 0.000(11) C29 0.112(10) 0.144(11) 0.129(10) 0.030(9) 0.087(8) -0.041(8) C30 0.147(12) 0.162(12) 0.186(13) 0.105(10) 0.079(10) -0.041(10) C31 0.140(11) 0.137(11) 0.029(6) 0.010(7) 0.018(7) 0.006(9) C32 0.185(13) 0.142(12) 0.047(8) 0.028(8) -0.018(9) 0.003(11) C33 0.081(9) 0.199(13) 0.055(7) 0.002(9) -0.048(6) -0.021(9) C34 0.125(11) 0.122(10) 0.063(8) -0.043(7) -0.007(8) -0.053(9) C35 0.166(12) 0.187(12) 0.039(7) -0.054(8) 0.032(8) -0.005(11) C36 0.164(12) 0.051(7) 0.135(10) -0.035(7) 0.060(10) -0.027(8) C37 0.130(10) 0.078(8) 0.144(11) -0.067(8) 0.051(9) -0.046(8) C38 0.095(10) 0.110(10) 0.223(14) -0.045(10) 0.047(10) -0.086(8) C39 0.181(13) 0.050(7) 0.168(12) 0.028(8) 0.071(10) -0.057(8) C40 0.174(13) 0.022(6) 0.217(14) 0.003(9) 0.052(11) -0.004(8) C41 0.110(10) 0.083(9) 0.176(12) -0.033(9) 0.012(9) -0.065(7) C42 0.181(12) 0.038(7) 0.186(12) 0.013(8) 0.070(11) -0.053(8) C43 0.213(14) 0.030(6) 0.206(14) -0.007(9) 0.067(12) 0.011(9) C44 0.171(12) 0.044(7) 0.165(12) -0.043(8) 0.065(11) -0.011(8) C45 0.134(11) 0.077(8) 0.141(11) -0.079(7) 0.060(9) -0.048(8) C46 0.035(6) 0.197(13) 0.156(12) 0.059(10) 0.028(8) 0.062(8) C47 0.028(6) 0.253(14) 0.096(9) 0.003(10) -0.018(6) -0.023(9) C48 0.053(8) 0.134(11) 0.172(12) 0.012(10) 0.021(8) -0.059(7) C49 0.071(8) 0.198(13) 0.142(11) 0.014(11) 0.072(8) -0.027(9) C50 0.066(8) 0.188(12) 0.154(11) -0.014(10) 0.074(9) 0.007(9) C51 0.063(8) 0.185(13) 0.159(12) -0.067(10) 0.053(8) 0.041(8) C52 0.156(11) 0.154(11) 0.129(10) -0.042(9) 0.133(9) -0.013(9) C53 0.153(11) 0.154(11) 0.073(8) -0.078(8) 0.047(8) 0.027(9) C54 0.152(11) 0.072(9) 0.175(13) -0.053(8) 0.093(10) 0.001(8) C55 0.131(11) 0.107(10) 0.180(13) -0.034(10) 0.079(10) 0.041(9) C56 0.087(9) 0.154(11) 0.080(8) 0.066(8) -0.012(7) 0.067(8) C57 0.191(13) 0.099(10) 0.121(10) 0.094(8) 0.006(10) 0.024(10) C58 0.183(13) 0.040(7) 0.163(12) 0.029(8) 0.046(11) 0.039(8) C59 0.144(12) 0.084(9) 0.189(13) -0.006(9) 0.056(11) 0.073(8) C60 0.101(10) 0.132(11) 0.167(13) 0.008(10) -0.003(9) 0.089(8) C101 0.113(10) 0.202(13) 0.053(7) -0.078(8) -0.015(7) -0.024(10) C102 0.040(7) 0.214(13) 0.072(8) -0.039(9) -0.030(6) 0.017(8) C103 0.044(7) 0.153(11) 0.130(10) -0.080(9) -0.007(7) -0.039(7) C104 0.182(13) 0.098(10) 0.167(13) -0.050(9) 0.009(11) -0.107(9) C105 0.095(9) 0.112(9) 0.142(11) -0.113(8) -0.014(8) 0.006(8) C106 0.067(8) 0.223(13) 0.063(8) 0.010(9) -0.021(6) 0.078(9) C107 0.120(11) 0.177(12) 0.106(10) 0.078(9) 0.007(8) 0.093(10) C108 0.166(12) 0.096(9) 0.160(12) 0.102(8) 0.073(10) 0.093(8) C109 0.119(11) 0.148(11) 0.165(12) 0.016(10) 0.049(9) 0.115(9) C110 0.051(7) 0.203(13) 0.114(10) 0.002(10) 0.019(7) 0.066(8) C111 0.125(10) 0.187(13) 0.021(5) 0.005(8) -0.006(7) 0.011(10) C112 0.154(11) 0.208(12) 0.064(7) 0.107(8) 0.061(8) 0.106(10) C113 0.240(14) 0.129(11) 0.110(10) 0.074(8) 0.110(10) 0.001(11) C114 0.132(11) 0.204(13) 0.092(9) 0.031(10) 0.092(8) 0.001(10) C115 0.129(10) 0.157(11) 0.044(6) -0.007(7) 0.046(7) 0.063(9) C116 0.138(11) 0.155(11) 0.118(10) -0.074(9) 0.078(9) 0.017(9) C117 0.120(10) 0.137(11) 0.134(11) 0.012(9) 0.090(9) 0.083(8) C118 0.165(13) 0.148(12) 0.242(15) -0.035(11) 0.048(12) 0.115(10) C119 0.154(12) 0.040(7) 0.197(13) -0.042(8) 0.044(10) 0.039(8) C120 0.232(14) 0.108(11) 0.154(12) -0.087(9) 0.059(12) 0.015(11) C121 0.128(11) 0.229(14) 0.153(12) 0.029(11) 0.117(9) -0.002(11) C122 0.098(10) 0.243(14) 0.106(10) -0.015(11) 0.076(8) 0.022(10) C123 0.027(6) 0.249(15) 0.189(13) -0.021(12) 0.037(9) 0.002(9) C124 0.075(9) 0.231(14) 0.169(12) -0.004(11) 0.056(9) -0.093(10) C125 0.170(12) 0.181(13) 0.186(13) -0.010(11) 0.141(11) -0.096(10) C126 0.108(9) 0.247(14) 0.034(6) 0.064(8) 0.024(7) 0.088(10) C127 0.114(10) 0.203(13) 0.030(6) -0.023(8) -0.008(7) -0.006(10) C128 0.093(9) 0.200(12) 0.038(6) -0.019(8) 0.031(6) 0.058(9) C129 0.115(10) 0.252(14) 0.050(7) 0.055(9) 0.049(7) -0.003(10) C130 0.232(14) 0.149(12) 0.064(8) 0.072(8) 0.071(10) 0.028(11) C131 0.108(11) 0.227(14) 0.077(9) -0.095(9) 0.009(8) -0.025(10) C132 0.044(7) 0.227(14) 0.116(11) -0.091(10) -0.024(7) -0.011(9) C133 0.053(8) 0.189(13) 0.176(12) -0.107(10) 0.031(9) -0.080(8) C134 0.161(13) 0.093(10) 0.210(14) -0.064(10) 0.036(11) -0.095(9) C135 0.106(10) 0.136(10) 0.160(11) -0.140(9) 0.006(9) -0.018(9) C136 0.181(13) 0.031(7) 0.229(14) -0.008(9) 0.048(12) -0.030(8) C137 0.218(14) 0.072(9) 0.225(15) -0.007(10) 0.035(13) -0.089(10) C138 0.170(12) 0.123(11) 0.215(14) 0.049(10) 0.085(11) -0.096(10) C139 0.211(14) 0.112(11) 0.152(12) 0.106(9) 0.041(11) -0.027(10) C140 0.200(13) 0.060(8) 0.161(12) 0.067(8) 0.056(11) 0.068(9) C141 0.180(13) 0.080(10) 0.263(15) 0.017(11) 0.099(12) -0.079(9) C142 0.253(15) 0.105(11) 0.183(13) 0.091(9) 0.106(12) -0.006(11) C143 0.231(14) 0.055(8) 0.192(13) 0.059(9) 0.128(11) 0.048(9) C144 0.226(15) 0.041(7) 0.263(15) -0.002(10) 0.102(13) 0.003(10) C145 0.249(15) 0.039(8) 0.254(15) -0.027(10) 0.096(13) -0.050(10) C146 0.032(7) 0.250(15) 0.180(13) -0.020(12) 0.055(8) 0.001(9) C147 0.055(8) 0.239(14) 0.136(11) 0.000(11) 0.030(8) -0.093(9) C148 0.120(11) 0.233(14) 0.114(10) 0.008(10) 0.077(9) -0.104(10) C149 0.122(11) 0.270(16) 0.136(12) 0.030(12) 0.088(10) -0.014(12) C150 0.115(10) 0.256(15) 0.089(9) -0.021(10) 0.086(8) 0.024(11) C151 0.130(10) 0.161(11) 0.102(9) 0.028(8) 0.090(8) 0.103(9) C152 0.145(11) 0.162(12) 0.118(10) -0.082(9) 0.098(9) 0.001(9) C153 0.240(14) 0.125(11) 0.175(13) -0.116(9) 0.073(12) 0.026(11) C154 0.197(13) 0.034(7) 0.197(13) -0.016(8) 0.093(11) 0.048(8) C155 0.197(14) 0.150(13) 0.208(14) -0.024(11) 0.093(12) 0.094(11) C156 0.032(6) 0.244(14) 0.088(9) -0.046(10) -0.036(6) 0.042(8) C157 0.124(11) 0.173(12) 0.079(9) 0.039(9) -0.023(8) 0.097(9) C158 0.126(11) 0.121(11) 0.192(14) 0.071(10) 0.033(10) 0.097(9) C159 0.088(10) 0.162(12) 0.159(12) -0.058(10) 0.011(9) 0.078(9) C160 0.034(7) 0.222(14) 0.129(11) 0.016(10) 0.017(7) 0.051(8) C201 0.043(5) 0.064(6) 0.112(7) 0.007(6) 0.000(5) -0.015(5) C202 0.030(3) 0.031(3) 0.055(4) 0.000(3) 0.001(3) -0.002(3) C203 0.031(3) 0.030(3) 0.043(3) 0.001(3) 0.008(3) 0.002(3) C204 0.022(3) 0.034(3) 0.027(3) 0.004(3) 0.006(3) 0.001(3) C205 0.029(3) 0.026(3) 0.028(3) -0.009(3) 0.010(3) -0.002(3) C206 0.028(3) 0.025(3) 0.031(3) -0.003(2) 0.003(2) -0.001(2) C207 0.028(3) 0.030(3) 0.034(3) 0.000(3) 0.004(3) 0.001(3) C208 0.019(3) 0.022(3) 0.015(3) -0.002(2) 0.005(2) -0.002(2) C209 0.025(3) 0.023(3) 0.026(3) 0.002(2) 0.003(2) -0.001(2) C210 0.040(4) 0.026(4) 0.046(4) -0.007(3) 0.006(4) -0.005(3) C211 0.0131(19) 0.0158(19) 0.0163(19) -0.0043(17) 0.0037(17) -0.0028(17) C212 0.019(3) 0.017(3) 0.013(2) 0.001(2) 0.005(2) -0.001(2) C213 0.025(3) 0.026(3) 0.026(3) -0.005(3) 0.013(2) -0.004(2) C214 0.022(3) 0.027(3) 0.025(3) -0.009(2) 0.011(2) -0.007(2) C215 0.022(2) 0.021(2) 0.017(2) -0.002(2) 0.004(2) -0.001(2) C216 0.016(2) 0.017(2) 0.017(2) -0.0019(19) 0.0068(19) -0.004(2) C217 0.017(2) 0.018(2) 0.020(2) -0.0013(18) 0.0060(18) -0.0005(18) C218 0.017(2) 0.017(2) 0.016(2) -0.004(2) 0.005(2) -0.002(2) C219 0.012(2) 0.016(2) 0.010(2) -0.007(2) 0.0038(19) -0.003(2) C220 0.023(3) 0.016(3) 0.013(3) -0.002(2) 0.004(2) 0.002(2) C221 0.018(2) 0.018(2) 0.025(2) -0.006(2) 0.009(2) -0.003(2) C222 0.015(2) 0.017(2) 0.014(2) -0.0023(19) 0.0066(19) -0.0018(19) C223 0.009(2) 0.016(2) 0.012(2) -0.007(2) 0.0065(19) -0.005(2) C224 0.016(2) 0.017(2) 0.018(2) -0.0024(19) 0.0050(19) -0.0021(19) C225 0.018(2) 0.017(2) 0.014(2) -0.0011(19) 0.0054(19) -0.0005(19) C226 0.015(2) 0.016(2) 0.018(2) -0.0013(18) 0.0066(18) -0.0033(18) C227 0.016(2) 0.017(2) 0.019(2) -0.003(2) 0.0058(19) -0.0027(19) C228 0.015(2) 0.017(2) 0.017(2) -0.0015(18) 0.0049(18) -0.0018(18) C301 0.036(5) 0.028(4) 0.061(6) 0.000(4) 0.007(5) -0.006(4) C302 0.032(5) 0.030(4) 0.059(6) 0.001(4) 0.020(4) 0.001(4) C303 0.041(5) 0.041(5) 0.070(6) 0.009(5) 0.011(5) 0.002(4) C304 0.059(6) 0.048(5) 0.039(5) -0.007(4) 0.017(5) 0.017(5) C305 0.052(5) 0.031(4) 0.045(5) -0.003(4) 0.024(4) 0.001(4) C306 0.036(5) 0.039(5) 0.078(7) 0.009(5) 0.023(5) 0.003(4) C307 0.040(5) 0.021(4) 0.039(5) 0.004(3) 0.017(4) 0.008(3) S1 0.0334(11) 0.0239(9) 0.0243(9) -0.0027(8) 0.0013(8) -0.0013(8) S2 0.0351(11) 0.0255(10) 0.0214(9) -0.0036(8) 0.0071(8) 0.0028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C11 1.4011 . ? C1 C5 1.4579 . ? C1 C2 1.4580 . ? C2 C6 1.4008 . ? C2 C3 1.4583 . ? C3 C47 1.4006 . ? C3 C4 1.4581 . ? C4 C37 1.4009 . ? C4 C5 1.4580 . ? C5 C20 1.4014 . ? C6 C10 1.4580 . ? C6 C7 1.4580 . ? C7 C12 1.4007 . ? C7 C8 1.4580 . ? C8 C43 1.4007 . ? C8 C9 1.4581 . ? C9 C55 1.4011 . ? C9 C10 1.4580 . ? C10 C46 1.4009 . ? C11 C12 1.4579 . ? C11 C15 1.4580 . ? C12 C13 1.4580 . ? C13 C42 1.4010 . ? C13 C14 1.4582 . ? C14 C21 1.4004 . ? C14 C15 1.4578 . ? C15 C16 1.4011 . ? C16 C20 1.4579 . ? C16 C17 1.4579 . ? C17 C22 1.4007 . ? C17 C18 1.4579 . ? C18 C59 1.4011 . ? C18 C19 1.4579 . ? C19 C36 1.4007 . ? C19 C20 1.4581 . ? C21 C22 1.4580 . ? C21 C25 1.4581 . ? C22 C23 1.4579 . ? C23 C60 1.4011 . ? C23 C24 1.4580 . ? C24 C33 1.4011 . ? C24 C25 1.4580 . ? C25 C41 1.4007 . ? C26 C57 1.4007 . ? C26 C30 1.4579 . ? C26 C27 1.4581 . ? C27 C31 1.4008 . ? C27 C28 1.4581 . ? C28 C52 1.4008 . ? C28 C29 1.4580 . ? C29 C49 1.4007 . ? C29 C30 1.4581 . ? C30 C39 1.4010 . ? C31 C32 1.4579 . ? C31 C35 1.4580 . ? C32 C56 1.4009 . ? C32 C33 1.4580 . ? C33 C34 1.4581 . ? C34 C45 1.4008 . ? C34 C35 1.4579 . ? C35 C53 1.4011 . ? C36 C40 1.4578 . ? C36 C37 1.4580 . ? C37 C38 1.4581 . ? C38 C48 1.4010 . ? C38 C39 1.4579 . ? C39 C40 1.4579 . ? C40 C58 1.4010 . ? C41 C42 1.4580 . ? C41 C45 1.4583 . ? C42 C43 1.4580 . ? C43 C44 1.4581 . ? C44 C54 1.4007 . ? C44 C45 1.4580 . ? C46 C50 1.4579 . ? C46 C47 1.4581 . ? C47 C48 1.4581 . ? C48 C49 1.4579 . ? C49 C50 1.4580 . ? C50 C51 1.4007 . ? C51 C55 1.4580 . ? C51 C52 1.4581 . ? C52 C53 1.4580 . ? C53 C54 1.4579 . ? C54 C55 1.4581 . ? C56 C57 1.4577 . ? C56 C60 1.4580 . ? C57 C58 1.4581 . ? C58 C59 1.4581 . ? C59 C60 1.4581 . ? C101 C111 1.4008 . ? C101 C102 1.4579 . ? C101 C105 1.4583 . ? C102 C106 1.4009 . ? C102 C103 1.4576 . ? C103 C147 1.4011 . ? C103 C104 1.4580 . ? C104 C137 1.4010 . ? C104 C105 1.4580 . ? C105 C120 1.4011 . ? C106 C110 1.4579 . ? C106 C107 1.4582 . ? C107 C112 1.4007 . ? C107 C108 1.4580 . ? C108 C143 1.4010 . ? C108 C109 1.4584 . ? C109 C155 1.4008 . ? C109 C110 1.4579 . ? C110 C146 1.4008 . ? C111 C115 1.4580 . ? C111 C112 1.4581 . ? C112 C113 1.4581 . ? C113 C142 1.4008 . ? C113 C114 1.4580 . ? C114 C121 1.4006 . ? C114 C115 1.4581 . ? C115 C116 1.4010 . ? C116 C117 1.4579 . ? C116 C120 1.4581 . ? C117 C122 1.4007 . ? C117 C118 1.4579 . ? C118 C159 1.4008 . ? C118 C119 1.4582 . ? C119 C136 1.4005 . ? C119 C120 1.4581 . ? C121 C125 1.4580 . ? C121 C122 1.4581 . ? C122 C123 1.4579 . ? C123 C160 1.4009 . ? C123 C124 1.4581 . ? C124 C133 1.4010 . ? C124 C125 1.4579 . ? C125 C141 1.4008 . ? C126 C157 1.4010 . ? C126 C130 1.4578 . ? C126 C127 1.4579 . ? C127 C131 1.4005 . ? C127 C128 1.4580 . ? C128 C152 1.4008 . ? C128 C129 1.4580 . ? C129 C149 1.4003 . ? C129 C130 1.4582 . ? C130 C139 1.4008 . ? C131 C135 1.4580 . ? C131 C132 1.4582 . ? C132 C156 1.4007 . ? C132 C133 1.4580 . ? C133 C134 1.4576 . ? C134 C145 1.4010 . ? C134 C135 1.4585 . ? C135 C153 1.4009 . ? C136 C140 1.4580 . ? C136 C137 1.4581 . ? C137 C138 1.4578 . ? C138 C148 1.4010 . ? C138 C139 1.4580 . ? C139 C140 1.4581 . ? C140 C158 1.4008 . ? C141 C145 1.4579 . ? C141 C142 1.4580 . ? C142 C143 1.4577 . ? C143 C144 1.4580 . ? C144 C154 1.4011 . ? C144 C145 1.4579 . ? C146 C147 1.4581 . ? C146 C150 1.4581 . ? C147 C148 1.4581 . ? C148 C149 1.4581 . ? C149 C150 1.4580 . ? C150 C151 1.4009 . ? C151 C155 1.4580 . ? C151 C152 1.4580 . ? C152 C153 1.4581 . ? C153 C154 1.4579 . ? C154 C155 1.4580 . ? C156 C157 1.4580 . ? C156 C160 1.4581 . ? C157 C158 1.4579 . ? C158 C159 1.4580 . ? C159 C160 1.4582 . ? C201 C202 1.523(11) . ? C202 C203 1.526(10) . ? C203 C207 1.538(10) . ? C204 C220 1.344(9) 3_565 ? C204 C207 1.496(9) . ? C204 S1 1.766(7) . ? C205 C213 1.510(9) . ? C205 C210 1.521(9) . ? C206 C219 1.311(9) . ? C206 C209 1.378(9) . ? C208 C212 1.410(8) 3_565 ? C208 C218 1.418(8) . ? C208 S1 1.734(6) . ? C209 C215 1.357(9) . ? C211 C226 1.412(8) . ? C211 C217 1.421(8) . ? C211 C227 1.436(8) . ? C212 C208 1.410(8) 3_565 ? C212 C225 1.430(8) . ? C212 C220 1.448(8) . ? C213 C214 1.525(9) . ? C214 C221 1.499(9) . ? C215 C228 1.415(8) . ? C216 C225 1.424(8) . ? C216 C222 1.436(8) 3_565 ? C216 C226 1.450(8) . ? C217 C228 1.427(8) . ? C217 C219 1.488(8) . ? C218 C224 1.416(8) . ? C218 C222 1.417(8) . ? C220 C204 1.344(9) 3_565 ? C221 C223 1.378(8) . ? C221 S2 1.728(7) . ? C222 C226 1.434(8) . ? C222 C216 1.436(8) 3_565 ? C223 C227 1.522(8) . ? C224 C227 1.394(8) . ? C224 S2 1.729(6) . ? C225 C228 1.432(8) . ? C301 C306 1.388(12) . ? C301 C304 1.393(11) . ? C302 C307 1.381(10) . ? C302 C304 1.392(11) . ? C303 C307 1.491(11) . ? C305 C306 1.367(11) . ? C305 C307 1.394(10) . ? 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 C11 C1 C5 129.4 . . ? C11 C1 C2 108.2 . . ? C5 C1 C2 108.0 . . ? C6 C2 C1 129.8 . . ? C6 C2 C3 109.7 . . ? C1 C2 C3 108.0 . . ? C47 C3 C4 111.7 . . ? C47 C3 C2 127.1 . . ? C4 C3 C2 108.0 . . ? C37 C4 C5 113.2 . . ? C37 C4 C3 129.4 . . ? C5 C4 C3 108.0 . . ? C20 C5 C1 113.6 . . ? C20 C5 C4 127.2 . . ? C1 C5 C4 108.0 . . ? C2 C6 C10 125.6 . . ? C2 C6 C7 113.1 . . ? C10 C6 C7 108.0 . . ? C12 C7 C6 125.1 . . ? C12 C7 C8 112.4 . . ? C6 C7 C8 108.0 . . ? C43 C8 C7 121.4 . . ? C43 C8 C9 119.7 . . ? C7 C8 C9 108.0 . . ? C55 C9 C10 119.8 . . ? C55 C9 C8 123.3 . . ? C10 C9 C8 108.0 . . ? C46 C10 C6 122.0 . . ? C46 C10 C9 117.6 . . ? C6 C10 C9 108.0 . . ? C1 C11 C12 130.5 . . ? C1 C11 C15 111.1 . . ? C12 C11 C15 108.0 . . ? C7 C12 C11 112.5 . . ? C7 C12 C13 129.8 . . ? C11 C12 C13 108.0 . . ? C42 C13 C12 114.3 . . ? C42 C13 C14 123.8 . . ? C12 C13 C14 108.0 . . ? C21 C14 C15 126.8 . . ? C21 C14 C13 112.3 . . ? C15 C14 C13 108.0 . . ? C16 C15 C14 115.7 . . ? C16 C15 C11 123.6 . . ? C14 C15 C11 108.0 . . ? C15 C16 C20 119.5 . . ? C15 C16 C17 121.1 . . ? C20 C16 C17 108.0 . . ? C22 C17 C16 119.4 . . ? C22 C17 C18 121.8 . . ? C16 C17 C18 108.0 . . ? C59 C18 C17 122.7 . . ? C59 C18 C19 117.1 . . ? C17 C18 C19 108.0 . . ? C36 C19 C18 125.1 . . ? C36 C19 C20 115.6 . . ? C18 C19 C20 108.0 . . ? C5 C20 C16 121.4 . . ? C5 C20 C19 118.0 . . ? C16 C20 C19 108.0 . . ? C14 C21 C22 113.8 . . ? C14 C21 C25 124.6 . . ? C22 C21 C25 108.0 . . ? C17 C22 C23 114.8 . . ? C17 C22 C21 122.9 . . ? C23 C22 C21 108.0 . . ? C60 C23 C22 124.3 . . ? C60 C23 C24 116.4 . . ? C22 C23 C24 108.0 . . ? C33 C24 C25 122.0 . . ? C33 C24 C23 119.9 . . ? C25 C24 C23 108.0 . . ? C41 C25 C24 117.3 . . ? C41 C25 C21 122.0 . . ? C24 C25 C21 108.0 . . ? C57 C26 C30 123.2 . . ? C57 C26 C27 117.8 . . ? C30 C26 C27 108.0 . . ? C31 C27 C28 116.4 . . ? C31 C27 C26 124.8 . . ? C28 C27 C26 108.0 . . ? C52 C28 C29 117.1 . . ? C52 C28 C27 120.6 . . ? C29 C28 C27 108.0 . . ? C49 C29 C28 123.9 . . ? C49 C29 C30 116.2 . . ? C28 C29 C30 108.0 . . ? C39 C30 C26 114.2 . . ? C39 C30 C29 123.8 . . ? C26 C30 C29 108.0 . . ? C27 C31 C32 112.2 . . ? C27 C31 C35 125.5 . . ? C32 C31 C35 108.0 . . ? C56 C32 C31 127.8 . . ? C56 C32 C33 109.3 . . ? C31 C32 C33 108.0 . . ? C24 C33 C32 127.0 . . ? C24 C33 C34 112.5 . . ? C32 C33 C34 108.0 . . ? C45 C34 C35 109.0 . . ? C45 C34 C33 133.3 . . ? C35 C34 C33 108.0 . . ? C53 C35 C34 125.5 . . ? C53 C35 C31 114.5 . . ? C34 C35 C31 108.0 . . ? C19 C36 C40 112.6 . . ? C19 C36 C37 124.9 . . ? C40 C36 C37 108.0 . . ? C4 C37 C36 120.5 . . ? C4 C37 C38 115.7 . . ? C36 C37 C38 108.0 . . ? C48 C38 C39 123.5 . . ? C48 C38 C37 117.8 . . ? C39 C38 C37 108.0 . . ? C30 C39 C38 116.0 . . ? C30 C39 C40 127.3 . . ? C38 C39 C40 108.0 . . ? C58 C40 C36 127.8 . . ? C58 C40 C39 113.7 . . ? C36 C40 C39 108.0 . . ? C25 C41 C42 114.3 . . ? C25 C41 C45 127.9 . . ? C42 C41 C45 108.0 . . ? C13 C42 C41 122.5 . . ? C13 C42 C43 119.7 . . ? C41 C42 C43 108.0 . . ? C8 C43 C42 122.0 . . ? C8 C43 C44 116.3 . . ? C42 C43 C44 108.0 . . ? C54 C44 C45 113.4 . . ? C54 C44 C43 124.7 . . ? C45 C44 C43 108.0 . . ? C34 C45 C44 131.0 . . ? C34 C45 C41 106.8 . . ? C44 C45 C41 108.0 . . ? C10 C46 C50 126.4 . . ? C10 C46 C47 115.0 . . ? C50 C46 C47 108.0 . . ? C3 C47 C46 120.1 . . ? C3 C47 C48 122.3 . . ? C46 C47 C48 108.0 . . ? C38 C48 C49 116.5 . . ? C38 C48 C47 122.6 . . ? C49 C48 C47 108.0 . . ? C29 C49 C48 123.3 . . ? C29 C49 C50 114.3 . . ? C48 C49 C50 108.0 . . ? C51 C50 C46 111.8 . . ? C51 C50 C49 126.5 . . ? C46 C50 C49 108.0 . . ? C50 C51 C55 126.0 . . ? C50 C51 C52 114.4 . . ? C55 C51 C52 108.0 . . ? C28 C52 C53 119.4 . . ? C28 C52 C51 123.6 . . ? C53 C52 C51 108.0 . . ? C35 C53 C54 118.4 . . ? C35 C53 C52 122.8 . . ? C54 C53 C52 108.0 . . ? C44 C54 C53 121.5 . . ? C44 C54 C55 118.1 . . ? C53 C54 C55 108.0 . . ? C9 C55 C51 118.1 . . ? C9 C55 C54 117.6 . . ? C51 C55 C54 108.0 . . ? C32 C56 C57 114.4 . . ? C32 C56 C60 127.4 . . ? C57 C56 C60 108.0 . . ? C26 C57 C56 122.2 . . ? C26 C57 C58 117.5 . . ? C56 C57 C58 108.0 . . ? C40 C58 C59 114.5 . . ? C40 C58 C57 123.8 . . ? C59 C58 C57 108.0 . . ? C18 C59 C58 122.9 . . ? C18 C59 C60 116.3 . . ? C58 C59 C60 108.0 . . ? C23 C60 C56 119.8 . . ? C23 C60 C59 120.1 . . ? C56 C60 C59 108.0 . . ? C111 C101 C102 108.2 . . ? C111 C101 C105 129.4 . . ? C102 C101 C105 108.0 . . ? C106 C102 C103 109.7 . . ? C106 C102 C101 129.7 . . ? C103 C102 C101 108.0 . . ? C147 C103 C102 127.1 . . ? C147 C103 C104 111.7 . . ? C102 C103 C104 108.0 . . ? C137 C104 C103 129.4 . . ? C137 C104 C105 113.2 . . ? C103 C104 C105 108.0 . . ? C120 C105 C104 127.2 . . ? C120 C105 C101 113.6 . . ? C104 C105 C101 108.0 . . ? C102 C106 C110 125.5 . . ? C102 C106 C107 113.1 . . ? C110 C106 C107 108.0 . . ? C112 C107 C108 112.5 . . ? C112 C107 C106 125.1 . . ? C108 C107 C106 108.0 . . ? C143 C108 C107 121.4 . . ? C143 C108 C109 119.7 . . ? C107 C108 C109 108.0 . . ? C155 C109 C110 119.8 . . ? C155 C109 C108 123.3 . . ? C110 C109 C108 108.0 . . ? C146 C110 C109 117.6 . . ? C146 C110 C106 122.0 . . ? C109 C110 C106 108.0 . . ? C101 C111 C115 111.1 . . ? C101 C111 C112 130.5 . . ? C115 C111 C112 108.0 . . ? C107 C112 C113 129.7 . . ? C107 C112 C111 112.5 . . ? C113 C112 C111 108.0 . . ? C142 C113 C114 123.8 . . ? C142 C113 C112 114.3 . . ? C114 C113 C112 108.0 . . ? C121 C114 C113 112.3 . . ? C121 C114 C115 126.8 . . ? C113 C114 C115 108.0 . . ? C116 C115 C111 123.6 . . ? C116 C115 C114 115.7 . . ? C111 C115 C114 108.0 . . ? C115 C116 C117 121.1 . . ? C115 C116 C120 119.5 . . ? C117 C116 C120 108.0 . . ? C122 C117 C118 121.8 . . ? C122 C117 C116 119.4 . . ? C118 C117 C116 108.0 . . ? C159 C118 C117 122.7 . . ? C159 C118 C119 117.1 . . ? C117 C118 C119 108.0 . . ? C136 C119 C120 115.6 . . ? C136 C119 C118 125.1 . . ? C120 C119 C118 108.0 . . ? C105 C120 C119 118.0 . . ? C105 C120 C116 121.4 . . ? C119 C120 C116 108.0 . . ? C114 C121 C125 124.5 . . ? C114 C121 C122 113.8 . . ? C125 C121 C122 108.0 . . ? C117 C122 C123 114.8 . . ? C117 C122 C121 122.9 . . ? C123 C122 C121 108.0 . . ? C160 C123 C122 124.2 . . ? C160 C123 C124 116.3 . . ? C122 C123 C124 108.0 . . ? C133 C124 C125 122.0 . . ? C133 C124 C123 119.9 . . ? C125 C124 C123 108.0 . . ? C141 C125 C124 117.3 . . ? C141 C125 C121 122.0 . . ? C124 C125 C121 108.0 . . ? C157 C126 C130 123.2 . . ? C157 C126 C127 117.8 . . ? C130 C126 C127 108.0 . . ? C131 C127 C126 124.8 . . ? C131 C127 C128 116.4 . . ? C126 C127 C128 108.0 . . ? C152 C128 C127 120.6 . . ? C152 C128 C129 117.0 . . ? C127 C128 C129 108.0 . . ? C149 C129 C128 123.9 . . ? C149 C129 C130 116.2 . . ? C128 C129 C130 108.0 . . ? C139 C130 C126 114.2 . . ? C139 C130 C129 123.8 . . ? C126 C130 C129 108.0 . . ? C127 C131 C135 125.5 . . ? C127 C131 C132 112.2 . . ? C135 C131 C132 108.0 . . ? C156 C132 C133 109.3 . . ? C156 C132 C131 127.8 . . ? C133 C132 C131 108.0 . . ? C124 C133 C134 112.5 . . ? C124 C133 C132 127.0 . . ? C134 C133 C132 108.0 . . ? C145 C134 C133 133.3 . . ? C145 C134 C135 109.0 . . ? C133 C134 C135 108.0 . . ? C153 C135 C131 114.5 . . ? C153 C135 C134 125.5 . . ? C131 C135 C134 108.0 . . ? C119 C136 C140 112.6 . . ? C119 C136 C137 124.9 . . ? C140 C136 C137 108.0 . . ? C104 C137 C138 115.6 . . ? C104 C137 C136 120.5 . . ? C138 C137 C136 108.0 . . ? C148 C138 C137 117.8 . . ? C148 C138 C139 123.5 . . ? C137 C138 C139 108.0 . . ? C130 C139 C138 116.0 . . ? C130 C139 C140 127.3 . . ? C138 C139 C140 108.0 . . ? C158 C140 C136 127.8 . . ? C158 C140 C139 113.7 . . ? C136 C140 C139 108.0 . . ? C125 C141 C145 127.9 . . ? C125 C141 C142 114.3 . . ? C145 C141 C142 108.0 . . ? C113 C142 C143 119.7 . . ? C113 C142 C141 122.5 . . ? C143 C142 C141 108.0 . . ? C108 C143 C142 122.0 . . ? C108 C143 C144 116.3 . . ? C142 C143 C144 108.0 . . ? C154 C144 C145 113.4 . . ? C154 C144 C143 124.7 . . ? C145 C144 C143 108.0 . . ? C134 C145 C144 131.0 . . ? C134 C145 C141 106.8 . . ? C144 C145 C141 108.0 . . ? C110 C146 C147 115.0 . . ? C110 C146 C150 126.4 . . ? C147 C146 C150 108.0 . . ? C103 C147 C146 120.0 . . ? C103 C147 C148 122.3 . . ? C146 C147 C148 108.0 . . ? C138 C148 C147 122.6 . . ? C138 C148 C149 116.5 . . ? C147 C148 C149 108.0 . . ? C129 C149 C150 114.3 . . ? C129 C149 C148 123.3 . . ? C150 C149 C148 108.0 . . ? C151 C150 C149 126.5 . . ? C151 C150 C146 111.8 . . ? C149 C150 C146 108.0 . . ? C150 C151 C155 126.0 . . ? C150 C151 C152 114.4 . . ? C155 C151 C152 108.0 . . ? C128 C152 C151 123.6 . . ? C128 C152 C153 119.4 . . ? C151 C152 C153 108.0 . . ? C135 C153 C154 118.4 . . ? C135 C153 C152 122.7 . . ? C154 C153 C152 108.0 . . ? C144 C154 C153 121.5 . . ? C144 C154 C155 118.1 . . ? C153 C154 C155 108.0 . . ? C109 C155 C154 117.6 . . ? C109 C155 C151 118.1 . . ? C154 C155 C151 108.0 . . ? C132 C156 C157 114.5 . . ? C132 C156 C160 127.4 . . ? C157 C156 C160 108.0 . . ? C126 C157 C158 117.6 . . ? C126 C157 C156 122.2 . . ? C158 C157 C156 108.0 . . ? C140 C158 C157 123.8 . . ? C140 C158 C159 114.5 . . ? C157 C158 C159 108.0 . . ? C118 C159 C158 123.0 . . ? C118 C159 C160 116.3 . . ? C158 C159 C160 108.0 . . ? C123 C160 C156 119.8 . . ? C123 C160 C159 120.1 . . ? C156 C160 C159 108.0 . . ? C201 C202 C203 112.8(7) . . ? C202 C203 C207 111.6(6) . . ? C220 C204 C207 127.9(6) 3_565 . ? C220 C204 S1 111.2(5) 3_565 . ? C207 C204 S1 120.6(5) . . ? C213 C205 C210 112.8(6) . . ? C219 C206 C209 121.7(7) . . ? C204 C207 C203 116.0(6) . . ? C212 C208 C218 122.1(5) 3_565 . ? C212 C208 S1 111.3(5) 3_565 . ? C218 C208 S1 126.2(5) . . ? C215 C209 C206 120.2(6) . . ? C226 C211 C217 119.6(5) . . ? C226 C211 C227 116.8(5) . . ? C217 C211 C227 123.6(5) . . ? C208 C212 C225 119.3(5) 3_565 . ? C208 C212 C220 111.2(5) 3_565 . ? C225 C212 C220 129.3(6) . . ? C205 C213 C214 112.3(5) . . ? C221 C214 C213 116.4(5) . . ? C209 C215 C228 122.3(6) . . ? C225 C216 C222 121.0(5) . 3_565 ? C225 C216 C226 119.2(5) . . ? C222 C216 C226 119.8(5) 3_565 . ? C211 C217 C228 120.0(5) . . ? C211 C217 C219 123.6(5) . . ? C228 C217 C219 116.1(5) . . ? C224 C218 C222 117.3(5) . . ? C224 C218 C208 124.8(5) . . ? C222 C218 C208 117.9(5) . . ? C206 C219 C217 121.6(6) . . ? C204 C220 C212 114.4(6) 3_565 . ? C223 C221 C214 125.1(6) . . ? C223 C221 S2 114.8(5) . . ? C214 C221 S2 120.1(5) . . ? C218 C222 C226 119.8(5) . . ? C218 C222 C216 119.3(5) . 3_565 ? C226 C222 C216 120.9(5) . 3_565 ? C221 C223 C227 108.7(5) . . ? C227 C224 C218 122.2(5) . . ? C227 C224 S2 112.0(4) . . ? C218 C224 S2 125.7(5) . . ? C216 C225 C212 117.5(5) . . ? C216 C225 C228 119.2(5) . . ? C212 C225 C228 123.3(5) . . ? C211 C226 C222 121.3(5) . . ? C211 C226 C216 119.4(5) . . ? C222 C226 C216 119.3(5) . . ? C224 C227 C211 120.2(5) . . ? C224 C227 C223 112.1(5) . . ? C211 C227 C223 127.5(5) . . ? C215 C228 C217 118.2(6) . . ? C215 C228 C225 122.5(5) . . ? C217 C228 C225 119.2(5) . . ? C306 C301 C304 118.7(8) . . ? C307 C302 C304 120.0(8) . . ? C301 C304 C302 120.5(8) . . ? C306 C305 C307 120.6(8) . . ? C305 C306 C301 120.9(8) . . ? C302 C307 C305 119.3(7) . . ? C302 C307 C303 119.4(7) . . ? C305 C307 C303 121.3(7) . . ? C208 S1 C204 91.9(3) . . ? C221 S2 C224 92.1(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.285 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.150