# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2008 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Alexander Katz' 'Kathleen A. Durkin' 'Justin M. Notestein' 'Andrew Solovyov' _publ_contact_author_name 'Alexander Katz' _publ_contact_author_email KATZ@CCHEM.BERKELEY.EDU _publ_section_title ; Graftable Chiral Ligands for Bioinspired Catalytic Materials: Calixarenes Bearing Asymmetric Centers Directly Attached to the Lower Rim ; # Attachment 'B801434P_calix2.cif' data_Solovyov_SOL150 _database_code_depnum_ccdc_archive 'CCDC 685846' # CHEMICAL DATA _chemical_formula_sum 'C70 H79 N O4 ' _chemical_formula_moiety 'C70 H79 N O4' _chemical_formula_weight 998.40 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 12.305(1) _cell_length_b 12.911(1) _cell_length_c 19.409(2) _cell_angle_alpha 90 _cell_angle_beta 105.578(2) _cell_angle_gamma 90 _cell_volume 2970.3(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2430 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 19.5 _cell_measurement_temperature 163.2 #------------------------------------------------------------------------------ _exptl_crystal_description tabular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076.00 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.995 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 12310 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 21.27 _diffrn_measured_fraction_theta_max 0.9937 _diffrn_reflns_theta_full 21.27 _diffrn_measured_fraction_theta_full 0.9937 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Due to the rapid drop-off in intensity with increasing sin(theta)/lambda only the t-butyl carbons, acetonitrile molecule and oxygen atoms were refined with anisotropic thermal parameters. The rapid drop-off in intensity is in part due to the significant thermal motion of the t-butyl carbons (hence why they were allowed to refine anisotropically) and the disorder of one of the napthalene rings. The disordered napthalene moiety was modeled as two rigid bodies (C48-C57, C71-C80) with a 60:40 occupancy. This value was arrived at through refinement of the site occupancy factors of the two components. The refined occupancy was very close to 60:40 and it was decided that the occupancy should be set to 60:40. The thermal parameters of the atoms of the two components are satisfactory and comparable at this ratio. Due to the disorder, the hydrogen atoms on the disordered naphthalene moiety were omitted from the calculation. This disorder also made locating the hydrogen on the bridging carbon (C46) unreliable and it too was omitted. Due to the relatively low resolution of the dataset, the locations of the hydroxyl hydrogens could not be determined, hence they were not included in the calculations. The enantiomorph of the space group and the enantiomer of the molecule were determined by inspection of the known chiral centers. ; _reflns_number_total 3479 _reflns_number_gt 2890 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.0847 _refine_ls_R_factor_all 0.1010 _refine_ls_wR_factor_all 0.0865 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2890 _refine_ls_number_parameters 427 _refine_ls_goodness_of_fit_ref 3.182 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0155 _refine_diff_density_max 0.53 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details . _refine_ls_abs_structure_Flack . _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.631' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution SIR97 _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics ? #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2754(5) 0.2333 0.6158(3) 0.054(2) Uani 1.00 d . . . O2 O 0.3272(5) 0.1321(6) 0.7461(3) 0.053(2) Uani 1.00 d . . . O3 O 0.5773(5) 0.1018(6) 0.7751(3) 0.054(2) Uani 1.00 d . . . O4 O 0.5381(5) 0.2270(6) 0.6620(3) 0.061(2) Uani 1.00 d . . . N1 N 0.494(1) 0.593(1) 0.9037(6) 0.121(5) Uani 1.00 d . . . C1 C 0.2607(7) 0.3367(8) 0.6361(4) 0.046(2) Uiso 1.00 d . . . C2 C 0.3257(7) 0.4133(8) 0.6152(4) 0.052(2) Uiso 1.00 d . . . C3 C 0.3079(7) 0.5152(8) 0.6348(5) 0.055(3) Uiso 1.00 d . . . C4 C 0.2322(7) 0.5428(8) 0.6727(5) 0.050(2) Uiso 1.00 d . . . C5 C 0.1751(7) 0.4626(8) 0.6938(5) 0.052(2) Uiso 1.00 d . . . C6 C 0.1885(7) 0.3574(8) 0.6773(4) 0.048(2) Uiso 1.00 d . . . C7 C 0.2112(8) 0.6553(7) 0.6873(5) 0.054(3) Uani 1.00 d . . . C8 C 0.118(1) 0.6950(10) 0.6278(7) 0.126(5) Uani 1.00 d . . . C9 C 0.178(1) 0.6670(10) 0.7558(7) 0.109(5) Uani 1.00 d . . . C10 C 0.315(1) 0.721(1) 0.694(1) 0.154(7) Uani 1.00 d . . . C11 C 0.1341(7) 0.2736(8) 0.7101(4) 0.049(2) Uiso 1.00 d . . . C12 C 0.1894(9) 0.1978(8) 0.5542(5) 0.062(3) Uani 1.00 d . . . C13 C 0.171(1) 0.2688(9) 0.4912(5) 0.082(4) Uani 1.00 d . . . C14 C 0.2314(8) 0.0893(9) 0.5372(5) 0.062(3) Uiso 1.00 d . . . C15 C 0.3438(9) 0.0663(9) 0.5550(5) 0.069(3) Uiso 1.00 d . . . C16 C 0.3818(9) -0.0319(10) 0.5373(6) 0.076(3) Uiso 1.00 d . . . C17 C 0.3023(8) -0.1029(8) 0.5025(5) 0.062(3) Uiso 1.00 d . . . C18 C 0.3403(9) -0.2036(10) 0.4845(5) 0.074(3) Uiso 1.00 d . . . C19 C 0.2598(9) -0.2712(9) 0.4460(5) 0.073(3) Uiso 1.00 d . . . C20 C 0.149(1) -0.247(1) 0.4263(6) 0.088(4) Uiso 1.00 d . . . C21 C 0.1067(9) -0.151(1) 0.4418(6) 0.087(4) Uiso 1.00 d . . . C22 C 0.1895(8) -0.0801(9) 0.4813(5) 0.061(3) Uiso 1.00 d . . . C23 C 0.1519(8) 0.0212(9) 0.5000(5) 0.068(3) Uiso 1.00 d . . . C24 C 0.2967(7) 0.1831(8) 0.8008(5) 0.049(2) Uiso 1.00 d . . . C25 C 0.2013(7) 0.2485(8) 0.7856(4) 0.046(2) Uiso 1.00 d . . . C26 C 0.1750(7) 0.2966(8) 0.8430(5) 0.054(3) Uiso 1.00 d . . . C27 C 0.2332(8) 0.2815(8) 0.9125(5) 0.055(2) Uiso 1.00 d . . . C28 C 0.3246(7) 0.2112(8) 0.9251(5) 0.056(3) Uiso 1.00 d . . . C29 C 0.3566(7) 0.1622(8) 0.8710(4) 0.046(2) Uiso 1.00 d . . . C30 C 0.2049(9) 0.3390(10) 0.9746(6) 0.075(4) Uani 1.00 d . . . C31 C 0.199(2) 0.268(2) 1.0317(9) 0.25(1) Uani 1.00 d . . . C32 C 0.096(1) 0.398(1) 0.9530(7) 0.135(6) Uani 1.00 d . . . C33 C 0.299(2) 0.417(2) 1.004(1) 0.22(1) Uani 1.00 d . . . C34 C 0.4599(7) 0.0926(8) 0.8867(5) 0.051(2) Uiso 1.00 d . . . C35 C 0.6165(7) 0.1641(8) 0.8361(5) 0.050(2) Uiso 1.00 d . . . C36 C 0.5666(7) 0.1568(8) 0.8910(5) 0.053(2) Uiso 1.00 d . . . C37 C 0.6097(8) 0.2150(8) 0.9519(5) 0.055(3) Uiso 1.00 d . . . C38 C 0.7030(8) 0.2816(8) 0.9586(5) 0.058(3) Uiso 1.00 d . . . C39 C 0.7452(7) 0.2897(9) 0.9005(5) 0.059(3) Uiso 1.00 d . . . C40 C 0.7048(8) 0.2323(9) 0.8372(5) 0.056(3) Uiso 1.00 d . . . C41 C 0.7533(8) 0.3422(8) 1.0273(5) 0.063(4) Uani 1.00 d . . . C42 C 0.6744(9) 0.3463(9) 1.0752(6) 0.084(4) Uani 1.00 d . . . C43 C 0.782(1) 0.4541(9) 1.0120(6) 0.097(4) Uani 1.00 d . . . C44 C 0.8626(9) 0.288(1) 1.0680(6) 0.087(4) Uani 1.00 d . . . C45 C 0.7507(8) 0.2504(8) 0.7739(5) 0.062(3) Uiso 1.00 d . . . C46 C 0.6181(8) -0.0057(7) 0.7832(6) 0.064(3) Uani 1.00 d . . . C47 C 0.5233(9) -0.0690(8) 0.7361(7) 0.084(4) Uani 1.00 d . . . C48 C 0.7093(8) -0.016(1) 0.7372(7) 0.029(3) Uiso 0.40 d G . . C49 C 0.6873(7) -0.017(1) 0.6628(7) 0.029(3) Uiso 0.40 d G . . C50 C 0.7764(8) -0.016(1) 0.6311(5) 0.054(3) Uiso 0.40 d G . . C51 C 0.8875(8) -0.0156(10) 0.6736(5) 0.050(3) Uiso 0.40 d G . . C52 C 0.9767(9) -0.015(2) 0.6419(6) 0.070(3) Uiso 0.40 d G . . C53 C 1.0878(8) -0.014(2) 0.6845(8) 0.082(3) Uiso 0.40 d G . . C54 C 1.1098(7) -0.014(1) 0.7588(8) 0.082(3) Uiso 0.40 d G . . C55 C 1.0207(8) -0.014(1) 0.7906(6) 0.066(3) Uiso 0.40 d G . . C56 C 0.9095(8) -0.0149(9) 0.7480(5) 0.045(3) Uiso 0.40 d G . . C57 C 0.8204(9) -0.015(1) 0.7798(5) 0.056(3) Uiso 0.40 d G . . C58 C 0.5909(7) 0.3242(8) 0.6765(5) 0.048(2) Uiso 1.00 d . . . C59 C 0.6889(7) 0.3380(8) 0.7258(5) 0.050(2) Uiso 1.00 d . . . C60 C 0.7355(8) 0.4397(9) 0.7375(5) 0.060(3) Uiso 1.00 d . . . C61 C 0.6806(8) 0.5214(9) 0.6940(5) 0.060(3) Uiso 1.00 d . . . C62 C 0.5832(8) 0.5031(9) 0.6449(5) 0.064(3) Uiso 1.00 d . . . C63 C 0.5314(7) 0.4054(8) 0.6318(5) 0.057(3) Uiso 1.00 d . . . C64 C 0.7345(10) 0.6298(8) 0.7096(8) 0.086(5) Uani 1.00 d . . . C65 C 0.847(1) 0.632(1) 0.6952(9) 0.147(7) Uani 1.00 d . . . C66 C 0.668(1) 0.7101(10) 0.6492(8) 0.129(6) Uani 1.00 d . . . C67 C 0.719(2) 0.672(1) 0.7748(7) 0.135(6) Uani 1.00 d . . . C68 C 0.4207(8) 0.3904(9) 0.5811(5) 0.067(3) Uiso 1.00 d . . . C69 C 0.4686(9) 0.4291(9) 0.8228(6) 0.075(4) Uani 1.00 d . . . C70 C 0.4834(9) 0.520(1) 0.8700(6) 0.075(4) Uani 1.00 d . . . C71 C 0.7385(6) -0.0068(8) 0.7769(5) 0.037(3) Uiso 0.60 d G . . C72 C 0.8307(7) 0.0098(8) 0.8359(4) 0.052(3) Uiso 0.60 d G . . C73 C 0.9396(6) 0.0125(8) 0.8271(3) 0.061(3) Uiso 0.60 d G . . C74 C 0.9562(5) -0.0013(7) 0.7594(3) 0.050(3) Uiso 0.60 d G . . C75 C 1.0651(5) 0.0015(9) 0.7507(4) 0.058(3) Uiso 0.60 d G . . C76 C 1.0817(6) -0.012(1) 0.6829(5) 0.068(3) Uiso 0.60 d G . . C77 C 0.9895(7) -0.0289(10) 0.6240(4) 0.060(3) Uiso 0.60 d G . . C78 C 0.8807(7) -0.0317(9) 0.6327(3) 0.059(3) Uiso 0.60 d G . . C79 C 0.8640(5) -0.0178(6) 0.7004(3) 0.040(3) Uiso 0.60 d G . . C80 C 0.7552(5) -0.0206(8) 0.7091(4) 0.035(3) Uiso 0.60 d G . . H1 H 0.3508 0.5688 0.6210 0.0660 Uiso 1.00 calc . . . H2 H 0.1237 0.4787 0.7210 0.0622 Uiso 1.00 calc . . . H3 H 0.1039 0.7654 0.6366 0.1517 Uiso 1.00 calc . . . H4 H 0.1394 0.6901 0.5843 0.1517 Uiso 1.00 calc . . . H5 H 0.0523 0.6551 0.6244 0.1517 Uiso 1.00 calc . . . H6 H 0.1627 0.7379 0.7628 0.1305 Uiso 1.00 calc . . . H7 H 0.1119 0.6271 0.7533 0.1305 Uiso 1.00 calc . . . H8 H 0.2374 0.6436 0.7947 0.1305 Uiso 1.00 calc . . . H9 H 0.3738 0.6970 0.7331 0.1853 Uiso 1.00 calc . . . H10 H 0.3377 0.7168 0.6512 0.1853 Uiso 1.00 calc . . . H11 H 0.2978 0.7911 0.7023 0.1853 Uiso 1.00 calc . . . H12 H 0.0608 0.2958 0.7110 0.0587 Uiso 1.00 calc . . . H13 H 0.1280 0.2129 0.6817 0.0587 Uiso 1.00 calc . . . H14 H 0.1205 0.1897 0.5670 0.0750 Uiso 1.00 calc . . . H15 H 0.2379 0.2738 0.4764 0.0981 Uiso 1.00 calc . . . H16 H 0.1116 0.2422 0.4531 0.0981 Uiso 1.00 calc . . . H17 H 0.1501 0.3355 0.5042 0.0981 Uiso 1.00 calc . . . H18 H 0.3972 0.1161 0.5795 0.0831 Uiso 1.00 calc . . . H19 H 0.4599 -0.0479 0.5491 0.0911 Uiso 1.00 calc . . . H20 H 0.4178 -0.2221 0.4987 0.0893 Uiso 1.00 calc . . . H21 H 0.2829 -0.3370 0.4331 0.0870 Uiso 1.00 calc . . . H22 H 0.0976 -0.2965 0.4004 0.1052 Uiso 1.00 calc . . . H23 H 0.0285 -0.1353 0.4272 0.1048 Uiso 1.00 calc . . . H24 H 0.0741 0.0392 0.4867 0.0813 Uiso 1.00 calc . . . H25 H 0.1126 0.3428 0.8332 0.0648 Uiso 1.00 calc . . . H26 H 0.3655 0.1972 0.9731 0.0669 Uiso 1.00 calc . . . H27 H 0.1840 0.3051 1.0701 0.3010 Uiso 1.00 calc . . . H28 H 0.1412 0.2184 1.0141 0.3010 Uiso 1.00 calc . . . H29 H 0.2696 0.2326 1.0482 0.3010 Uiso 1.00 calc . . . H30 H 0.0879 0.4384 0.9924 0.1617 Uiso 1.00 calc . . . H31 H 0.0971 0.4431 0.9143 0.1617 Uiso 1.00 calc . . . H32 H 0.0349 0.3515 0.9387 0.1617 Uiso 1.00 calc . . . H33 H 0.3682 0.3813 1.0212 0.2635 Uiso 1.00 calc . . . H34 H 0.3036 0.4636 0.9673 0.2635 Uiso 1.00 calc . . . H35 H 0.2823 0.4543 1.0423 0.2635 Uiso 1.00 calc . . . H36 H 0.4673 0.0583 0.9311 0.0609 Uiso 1.00 calc . . . H37 H 0.4511 0.0427 0.8497 0.0609 Uiso 1.00 calc . . . H38 H 0.5757 0.2101 0.9903 0.0664 Uiso 1.00 calc . . . H39 H 0.8054 0.3368 0.9031 0.0709 Uiso 1.00 calc . . . H40 H 0.7095 0.3834 1.1177 0.1014 Uiso 1.00 calc . . . H41 H 0.6065 0.3803 1.0508 0.1014 Uiso 1.00 calc . . . H42 H 0.6578 0.2779 1.0872 0.1014 Uiso 1.00 calc . . . H43 H 0.8144 0.4887 1.0559 0.1160 Uiso 1.00 calc . . . H44 H 0.8335 0.4539 0.9835 0.1160 Uiso 1.00 calc . . . H45 H 0.7146 0.4890 0.9871 0.1160 Uiso 1.00 calc . . . H46 H 0.8464 0.2187 1.0783 0.1039 Uiso 1.00 calc . . . H47 H 0.9145 0.2881 1.0395 0.1039 Uiso 1.00 calc . . . H48 H 0.8947 0.3239 1.1115 0.1039 Uiso 1.00 calc . . . H49 H 0.8283 0.2678 0.7907 0.0744 Uiso 1.00 calc . . . H50 H 0.7428 0.1884 0.7466 0.0744 Uiso 1.00 calc . . . H51 H 0.8029 0.4521 0.7742 0.0719 Uiso 1.00 calc . . . H52 H 0.5466 0.5599 0.6171 0.0772 Uiso 1.00 calc . . . H53 H 0.8969 0.5876 0.7278 0.1766 Uiso 1.00 calc . . . H54 H 0.8398 0.6094 0.6476 0.1766 Uiso 1.00 calc . . . H55 H 0.8754 0.7008 0.7008 0.1766 Uiso 1.00 calc . . . H56 H 0.7035 0.7761 0.6577 0.1549 Uiso 1.00 calc . . . H57 H 0.6703 0.6857 0.6034 0.1549 Uiso 1.00 calc . . . H58 H 0.5921 0.7156 0.6510 0.1549 Uiso 1.00 calc . . . H59 H 0.7567 0.6292 0.8138 0.1626 Uiso 1.00 calc . . . H60 H 0.7497 0.7398 0.7817 0.1626 Uiso 1.00 calc . . . H61 H 0.6409 0.6743 0.7720 0.1626 Uiso 1.00 calc . . . H62 H 0.4145 0.3207 0.5650 0.0799 Uiso 1.00 calc . . . H63 H 0.4141 0.4356 0.5415 0.0799 Uiso 1.00 calc . . . H64 H 0.4570 -0.0604 0.7517 0.1010 Uiso 1.00 calc . . . H65 H 0.5092 -0.0462 0.6880 0.1010 Uiso 1.00 calc . . . H66 H 0.5441 -0.1400 0.7391 0.1010 Uiso 1.00 calc . . . H67 H 0.4720 0.4501 0.7765 0.0897 Uiso 1.00 calc . . . H68 H 0.3974 0.3982 0.8197 0.0897 Uiso 1.00 calc . . . H69 H 0.5268 0.3804 0.8417 0.0897 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.079(4) 0.030(3) 0.054(4) 0.006(3) 0.021(4) -0.007(3) O2 0.063(4) 0.035(3) 0.066(4) 0.003(3) 0.026(3) -0.008(3) O3 0.062(4) 0.029(4) 0.079(4) 0.003(3) 0.031(4) 0.006(3) O4 0.080(4) 0.022(3) 0.091(5) -0.013(3) 0.041(4) -0.008(3) N1 0.131(10) 0.100(9) 0.12(1) 0.017(8) 0.014(8) -0.045(8) C7 0.070(7) 0.021(5) 0.074(7) 0.010(5) 0.025(6) -0.003(5) C8 0.19(1) 0.057(8) 0.11(1) 0.055(9) -0.01(1) -0.006(7) C9 0.16(1) 0.053(7) 0.13(1) 0.003(8) 0.06(1) -0.029(7) C10 0.13(1) 0.055(8) 0.32(2) -0.039(9) 0.13(1) -0.06(1) C12 0.093(8) 0.040(6) 0.056(7) 0.002(6) 0.023(7) -0.017(5) C13 0.118(9) 0.055(7) 0.059(7) 0.019(6) -0.000(7) -0.004(6) C30 0.073(8) 0.090(9) 0.062(8) 0.003(7) 0.020(6) -0.022(7) C31 0.48(4) 0.22(2) 0.13(1) 0.20(3) 0.21(2) 0.08(2) C32 0.13(1) 0.17(2) 0.11(1) 0.05(1) 0.047(10) -0.04(1) C33 0.19(2) 0.27(3) 0.24(2) -0.11(2) 0.13(2) -0.19(2) C41 0.056(7) 0.047(7) 0.077(8) -0.003(5) 0.005(6) 0.004(6) C42 0.081(8) 0.071(8) 0.096(9) -0.002(6) 0.015(7) -0.021(7) C43 0.121(10) 0.062(8) 0.081(8) -0.007(7) -0.017(8) -0.008(7) C44 0.080(8) 0.079(8) 0.090(8) 0.003(7) 0.003(7) 0.002(7) C46 0.072(7) 0.006(5) 0.121(9) 0.002(5) 0.038(7) -0.003(5) C47 0.087(8) 0.040(6) 0.14(1) -0.001(6) 0.052(8) -0.024(6) C64 0.100(9) 0.020(6) 0.16(1) -0.014(5) 0.074(9) -0.009(7) C65 0.16(1) 0.09(1) 0.21(2) -0.07(1) 0.10(1) -0.02(1) C66 0.23(2) 0.040(7) 0.14(1) -0.025(10) 0.09(1) -0.009(8) C67 0.26(2) 0.062(8) 0.094(9) -0.06(1) 0.07(1) -0.031(7) C69 0.092(8) 0.055(7) 0.074(7) 0.014(6) 0.016(7) -0.009(6) C70 0.067(8) 0.086(10) 0.069(8) 0.012(7) 0.015(7) 0.011(8) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.42(1) . . yes O1 C12 1.44(1) . . yes O2 C24 1.38(1) . . yes O3 C35 1.41(1) . . yes O3 C46 1.47(1) . . yes O4 C58 1.41(1) . . yes N1 C70 1.13(2) . . yes C1 C2 1.40(1) . . yes C1 C6 1.37(1) . . yes C2 C3 1.40(2) . . yes C2 C68 1.52(2) . . yes C3 C4 1.38(1) . . yes C4 C5 1.37(1) . . yes C4 C7 1.52(1) . . yes C5 C6 1.41(1) . . yes C6 C11 1.50(1) . . yes C7 C8 1.48(2) . . yes C7 C9 1.50(2) . . yes C7 C10 1.51(2) . . yes C11 C25 1.51(1) . . yes C12 C13 1.50(1) . . yes C12 C14 1.56(2) . . yes C14 C15 1.37(1) . . yes C14 C23 1.37(1) . . yes C15 C16 1.42(2) . . yes C16 C17 1.38(1) . . yes C17 C18 1.46(2) . . yes C17 C22 1.37(1) . . yes C18 C19 1.38(2) . . yes C19 C20 1.35(2) . . yes C20 C21 1.40(2) . . yes C21 C22 1.43(2) . . yes C22 C23 1.47(2) . . yes C24 C25 1.41(1) . . yes C24 C29 1.39(1) . . yes C25 C26 1.39(1) . . yes C26 C27 1.36(1) . . yes C27 C28 1.41(1) . . yes C27 C30 1.53(2) . . yes C28 C29 1.37(1) . . yes C29 C34 1.52(1) . . yes C30 C31 1.46(2) . . yes C30 C32 1.50(2) . . yes C30 C33 1.52(2) . . yes C34 C36 1.54(1) . . yes C35 C36 1.37(1) . . yes C35 C40 1.39(1) . . yes C36 C37 1.38(1) . . yes C37 C38 1.41(1) . . yes C38 C39 1.37(1) . . yes C38 C41 1.53(1) . . yes C39 C40 1.41(1) . . yes C40 C45 1.50(1) . . yes C41 C42 1.52(2) . . yes C41 C43 1.53(2) . . yes C41 C44 1.53(1) . . yes C45 C59 1.53(1) . . yes C46 C47 1.51(1) . . yes C46 C48 1.62(2) . . yes C46 C71 1.52(1) . . yes C58 C59 1.33(1) . . yes C58 C63 1.43(1) . . yes C59 C60 1.43(1) . . yes C60 C61 1.41(1) . . yes C61 C62 1.34(1) . . yes C61 C64 1.54(2) . . yes C62 C63 1.41(2) . . yes C63 C68 1.46(1) . . yes C64 C65 1.48(2) . . yes C64 C66 1.61(2) . . yes C64 C67 1.43(2) . . yes C69 C70 1.47(2) . . yes C51 C50 1.39(1) . . yes C51 C56 1.39(1) . . yes C51 C52 1.39(2) . . yes C50 C49 1.39(2) . . yes C49 C48 1.39(2) . . yes C48 C57 1.39(1) . . yes C57 C56 1.39(2) . . yes C56 C55 1.39(1) . . yes C52 C53 1.39(1) . . yes C53 C54 1.39(2) . . yes C54 C55 1.39(2) . . yes C74 C73 1.395(9) . . yes C74 C79 1.395(7) . . yes C74 C75 1.395(9) . . yes C73 C72 1.39(1) . . yes C72 C71 1.39(1) . . yes C71 C80 1.39(1) . . yes C80 C79 1.395(9) . . yes C79 C78 1.395(9) . . yes C75 C76 1.39(1) . . yes C76 C77 1.39(1) . . yes C77 C78 1.39(1) . . yes C3 H1 0.950 . . no C5 H2 0.950 . . no C8 H3 0.950 . . no C8 H4 0.950 . . no C8 H5 0.950 . . no C9 H6 0.950 . . no C9 H7 0.950 . . no C9 H8 0.950 . . no C10 H9 0.950 . . no C10 H10 0.950 . . no C10 H11 0.950 . . no C11 H12 0.950 . . no C11 H13 0.950 . . no C12 H14 0.950 . . no C13 H15 0.950 . . no C13 H16 0.950 . . no C13 H17 0.950 . . no C15 H18 0.950 . . no C16 H19 0.950 . . no C18 H20 0.950 . . no C19 H21 0.950 . . no C20 H22 0.950 . . no C21 H23 0.950 . . no C23 H24 0.950 . . no C26 H25 0.950 . . no C28 H26 0.950 . . no C31 H27 0.950 . . no C31 H28 0.950 . . no C31 H29 0.950 . . no C32 H30 0.950 . . no C32 H31 0.950 . . no C32 H32 0.950 . . no C33 H33 0.950 . . no C33 H34 0.950 . . no C33 H35 0.950 . . no C34 H36 0.950 . . no C34 H37 0.950 . . no C37 H38 0.950 . . no C39 H39 0.950 . . no C42 H40 0.950 . . no C42 H41 0.950 . . no C42 H42 0.950 . . no C43 H43 0.950 . . no C43 H44 0.950 . . no C43 H45 0.950 . . no C44 H46 0.950 . . no C44 H47 0.950 . . no C44 H48 0.950 . . no C45 H49 0.950 . . no C45 H50 0.950 . . no C47 H64 0.950 . . no C47 H65 0.950 . . no C47 H66 0.950 . . no C60 H51 0.950 . . no C62 H52 0.950 . . no C65 H53 0.950 . . no C65 H54 0.950 . . no C65 H55 0.950 . . no C66 H56 0.950 . . no C66 H57 0.950 . . no C66 H58 0.950 . . no C67 H59 0.950 . . no C67 H60 0.950 . . no C67 H61 0.950 . . no C68 H62 0.950 . . no C68 H63 0.950 . . no C69 H67 0.950 . . no C69 H68 0.950 . . no C69 H69 0.950 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C12 114.2(5) . . . ? C35 O3 C46 114.9(7) . . . ? O1 C1 C2 117.4(8) . . . ? O1 C1 C6 119.7(8) . . . ? C2 C1 C6 122.8(9) . . . ? C1 C2 C3 116.2(9) . . . ? C1 C2 C68 123.8(10) . . . ? C3 C2 C68 119.6(9) . . . ? C2 C3 C4 124.3(10) . . . ? C3 C4 C5 115.9(10) . . . ? C3 C4 C7 121.3(9) . . . ? C5 C4 C7 122.7(9) . . . ? C4 C5 C6 123.8(9) . . . ? C1 C6 C5 116.8(9) . . . ? C1 C6 C11 122.7(9) . . . ? C5 C6 C11 120.2(9) . . . ? C4 C7 C8 108.7(8) . . . ? C4 C7 C9 111.3(9) . . . ? C4 C7 C10 112.0(9) . . . ? C8 C7 C9 108(1) . . . ? C8 C7 C10 109(1) . . . ? C9 C7 C10 106(1) . . . ? C6 C11 C25 112.0(7) . . . ? O1 C12 C13 113.6(8) . . . ? O1 C12 C14 104.5(7) . . . ? C13 C12 C14 111.4(9) . . . ? C12 C14 C15 120.9(9) . . . ? C12 C14 C23 117.3(9) . . . ? C15 C14 C23 121(1) . . . ? C14 C15 C16 120.5(10) . . . ? C15 C16 C17 118.4(10) . . . ? C16 C17 C18 118.8(9) . . . ? C16 C17 C22 122(1) . . . ? C18 C17 C22 119.0(9) . . . ? C17 C18 C19 117.7(9) . . . ? C18 C19 C20 121(1) . . . ? C19 C20 C21 123(1) . . . ? C20 C21 C22 115.2(10) . . . ? C17 C22 C21 122(1) . . . ? C17 C22 C23 118.7(9) . . . ? C21 C22 C23 118.7(9) . . . ? C14 C23 C22 118.4(9) . . . ? O2 C24 C25 120.4(7) . . . ? O2 C24 C29 118.5(8) . . . ? C25 C24 C29 120.9(9) . . . ? C11 C25 C24 122.6(8) . . . ? C11 C25 C26 119.8(8) . . . ? C24 C25 C26 117.4(7) . . . ? C25 C26 C27 123.9(9) . . . ? C26 C27 C28 116.4(9) . . . ? C26 C27 C30 122.7(9) . . . ? C28 C27 C30 120.9(8) . . . ? C27 C28 C29 122.8(8) . . . ? C24 C29 C28 118.4(8) . . . ? C24 C29 C34 120.4(8) . . . ? C28 C29 C34 121.0(7) . . . ? C27 C30 C31 111(1) . . . ? C27 C30 C32 113.7(9) . . . ? C27 C30 C33 107(1) . . . ? C31 C30 C32 108(1) . . . ? C31 C30 C33 108(1) . . . ? C32 C30 C33 107(1) . . . ? C29 C34 C36 110.4(8) . . . ? O3 C35 C36 119.5(8) . . . ? O3 C35 C40 117.6(9) . . . ? C36 C35 C40 122.9(9) . . . ? C34 C36 C35 123.4(8) . . . ? C34 C36 C37 117.8(9) . . . ? C35 C36 C37 118.6(9) . . . ? C36 C37 C38 121.8(9) . . . ? C37 C38 C39 116.8(9) . . . ? C37 C38 C41 121.4(9) . . . ? C39 C38 C41 121.7(9) . . . ? C38 C39 C40 123.9(9) . . . ? C35 C40 C39 115.9(9) . . . ? C35 C40 C45 123.3(8) . . . ? C39 C40 C45 120.7(9) . . . ? C38 C41 C42 112.2(8) . . . ? C38 C41 C43 111.9(9) . . . ? C38 C41 C44 108.1(9) . . . ? C42 C41 C43 107.6(10) . . . ? C42 C41 C44 108.5(9) . . . ? C43 C41 C44 108.4(9) . . . ? C40 C45 C59 112.3(8) . . . ? O3 C46 C47 105.1(7) . . . ? O3 C46 C48 106.7(9) . . . ? O3 C46 C71 108.2(8) . . . ? C47 C46 C48 99.1(9) . . . ? C47 C46 C71 123.8(10) . . . ? C48 C46 C71 28.1(5) . . . ? O4 C58 C59 122.9(8) . . . ? O4 C58 C63 113.5(7) . . . ? C59 C58 C63 123.6(9) . . . ? C45 C59 C58 122.9(9) . . . ? C45 C59 C60 118.1(7) . . . ? C58 C59 C60 119.0(9) . . . ? C59 C60 C61 119.1(8) . . . ? C60 C61 C62 119.4(10) . . . ? C60 C61 C64 116.7(8) . . . ? C62 C61 C64 123.8(10) . . . ? C61 C62 C63 124.4(10) . . . ? C58 C63 C62 114.5(7) . . . ? C58 C63 C68 122.9(9) . . . ? C62 C63 C68 122.4(9) . . . ? C61 C64 C65 110(1) . . . ? C61 C64 C66 109.5(9) . . . ? C61 C64 C67 111(1) . . . ? C65 C64 C66 99(1) . . . ? C65 C64 C67 120(1) . . . ? C66 C64 C67 103(1) . . . ? C2 C68 C63 111.5(8) . . . ? N1 C70 C69 176(1) . . . ? C50 C51 C56 120.0(9) . . . ? C50 C51 C52 120.0(9) . . . ? C56 C51 C52 120.0(8) . . . ? C51 C50 C49 120.0(9) . . . ? C50 C49 C48 120.0(8) . . . ? C46 C48 C49 127.0(8) . . . ? C46 C48 C57 112(1) . . . ? C49 C48 C57 120(1) . . . ? C48 C57 C56 120.0(9) . . . ? C51 C56 C57 120.0(8) . . . ? C51 C56 C55 120.0(10) . . . ? C57 C56 C55 120.0(9) . . . ? C51 C52 C53 120(1) . . . ? C52 C53 C54 120(1) . . . ? C53 C54 C55 120.0(9) . . . ? C56 C55 C54 119(1) . . . ? C73 C74 C79 120.0(6) . . . ? C73 C74 C75 120.0(6) . . . ? C79 C74 C75 120.0(6) . . . ? C74 C73 C72 120.0(6) . . . ? C73 C72 C71 120.0(7) . . . ? C46 C71 C72 121.9(8) . . . ? C46 C71 C80 118.1(7) . . . ? C72 C71 C80 120.0(7) . . . ? C71 C80 C79 120.0(6) . . . ? C74 C79 C80 120.0(6) . . . ? C74 C79 C78 120.0(6) . . . ? C80 C79 C78 120.0(6) . . . ? C74 C75 C76 120.0(6) . . . ? C75 C76 C77 120.0(7) . . . ? C76 C77 C78 120.0(8) . . . ? C79 C78 C77 120.0(6) . . . ? C2 C3 H1 117.871 . . . no C4 C3 H1 117.873 . . . no C4 C5 H2 118.091 . . . no C6 C5 H2 118.091 . . . no C7 C8 H3 109.472 . . . no C7 C8 H4 109.470 . . . no C7 C8 H5 109.470 . . . no H3 C8 H4 109.473 . . . no H3 C8 H5 109.472 . . . no H4 C8 H5 109.470 . . . no C7 C9 H6 109.470 . . . no C7 C9 H7 109.471 . . . no C7 C9 H8 109.472 . . . no H6 C9 H7 109.472 . . . no H6 C9 H8 109.471 . . . no H7 C9 H8 109.472 . . . no C7 C10 H9 109.471 . . . no C7 C10 H10 109.470 . . . no C7 C10 H11 109.471 . . . no H9 C10 H10 109.471 . . . no H9 C10 H11 109.471 . . . no H10 C10 H11 109.473 . . . no C6 C11 H12 108.832 . . . no C6 C11 H13 108.832 . . . no C25 C11 H12 108.832 . . . no C25 C11 H13 108.831 . . . no H12 C11 H13 109.459 . . . no O1 C12 H14 109.059 . . . no C13 C12 H14 109.060 . . . no C14 C12 H14 109.059 . . . no C12 C13 H15 109.470 . . . no C12 C13 H16 109.469 . . . no C12 C13 H17 109.470 . . . no H15 C13 H16 109.473 . . . no H15 C13 H17 109.473 . . . no H16 C13 H17 109.471 . . . no C14 C15 H18 119.742 . . . no C16 C15 H18 119.742 . . . no C15 C16 H19 120.804 . . . no C17 C16 H19 120.804 . . . no C17 C18 H20 121.126 . . . no C19 C18 H20 121.127 . . . no C18 C19 H21 119.109 . . . no C20 C19 H21 119.112 . . . no C19 C20 H22 118.175 . . . no C21 C20 H22 118.176 . . . no C20 C21 H23 122.421 . . . no C22 C21 H23 122.421 . . . no C14 C23 H24 120.803 . . . no C22 C23 H24 120.803 . . . no C25 C26 H25 118.051 . . . no C27 C26 H25 118.051 . . . no C27 C28 H26 118.585 . . . no C29 C28 H26 118.585 . . . no C30 C31 H27 109.471 . . . no C30 C31 H28 109.471 . . . no C30 C31 H29 109.470 . . . no H27 C31 H28 109.472 . . . no H27 C31 H29 109.472 . . . no H28 C31 H29 109.471 . . . no C30 C32 H30 109.470 . . . no C30 C32 H31 109.469 . . . no C30 C32 H32 109.471 . . . no H30 C32 H31 109.473 . . . no H30 C32 H32 109.472 . . . no H31 C32 H32 109.472 . . . no C30 C33 H33 109.468 . . . no C30 C33 H34 109.470 . . . no C30 C33 H35 109.469 . . . no H33 C33 H34 109.474 . . . no H33 C33 H35 109.471 . . . no H34 C33 H35 109.475 . . . no C29 C34 H36 109.244 . . . no C29 C34 H37 109.243 . . . no C36 C34 H36 109.242 . . . no C36 C34 H37 109.241 . . . no H36 C34 H37 109.459 . . . no C36 C37 H38 119.125 . . . no C38 C37 H38 119.125 . . . no C38 C39 H39 118.067 . . . no C40 C39 H39 118.066 . . . no C41 C42 H40 109.470 . . . no C41 C42 H41 109.469 . . . no C41 C42 H42 109.469 . . . no H40 C42 H41 109.473 . . . no H40 C42 H42 109.474 . . . no H41 C42 H42 109.472 . . . no C41 C43 H43 109.469 . . . no C41 C43 H44 109.470 . . . no C41 C43 H45 109.470 . . . no H43 C43 H44 109.473 . . . no H43 C43 H45 109.471 . . . no H44 C43 H45 109.475 . . . no C41 C44 H46 109.471 . . . no C41 C44 H47 109.470 . . . no C41 C44 H48 109.471 . . . no H46 C44 H47 109.472 . . . no H46 C44 H48 109.473 . . . no H47 C44 H48 109.471 . . . no C40 C45 H49 108.764 . . . no C40 C45 H50 108.764 . . . no C59 C45 H49 108.762 . . . no C59 C45 H50 108.762 . . . no H49 C45 H50 109.460 . . . no C46 C47 H64 109.472 . . . no C46 C47 H65 109.470 . . . no C46 C47 H66 109.470 . . . no H64 C47 H65 109.472 . . . no H64 C47 H66 109.473 . . . no H65 C47 H66 109.471 . . . no C59 C60 H51 120.432 . . . no C61 C60 H51 120.433 . . . no C61 C62 H52 117.820 . . . no C63 C62 H52 117.821 . . . no C64 C65 H53 109.470 . . . no C64 C65 H54 109.471 . . . no C64 C65 H55 109.471 . . . no H53 C65 H54 109.472 . . . no H53 C65 H55 109.472 . . . no H54 C65 H55 109.472 . . . no C64 C66 H56 109.471 . . . no C64 C66 H57 109.470 . . . no C64 C66 H58 109.468 . . . no H56 C66 H57 109.475 . . . no H56 C66 H58 109.473 . . . no H57 C66 H58 109.471 . . . no C64 C67 H59 109.472 . . . no C64 C67 H60 109.471 . . . no C64 C67 H61 109.468 . . . no H59 C67 H60 109.475 . . . no H59 C67 H61 109.470 . . . no H60 C67 H61 109.470 . . . no C2 C68 H62 108.953 . . . no C2 C68 H63 108.953 . . . no C63 C68 H62 108.953 . . . no C63 C68 H63 108.953 . . . no H62 C68 H63 109.459 . . . no C70 C69 H67 109.470 . . . no C70 C69 H68 109.470 . . . no C70 C69 H69 109.470 . . . no H67 C69 H68 109.473 . . . no H67 C69 H69 109.473 . . . no H68 C69 H69 109.473 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.8(6) 1_555 1_555 1_555 1_555 yes O1 C1 C2 C68 -8(1) 1_555 1_555 1_555 1_555 yes O1 C1 C6 C5 -178.1(6) 1_555 1_555 1_555 1_555 yes O1 C1 C6 C11 7(1) 1_555 1_555 1_555 1_555 yes O1 C12 C14 C15 -27(1) 1_555 1_555 1_555 1_555 yes O1 C12 C14 C23 156.4(9) 1_555 1_555 1_555 1_555 yes O2 C24 C25 C11 -5(1) 1_555 1_555 1_555 1_555 yes O2 C24 C25 C26 179.5(9) 1_555 1_555 1_555 1_555 yes O2 C24 C29 C28 -178.6(9) 1_555 1_555 1_555 1_555 yes O2 C24 C29 C34 5(1) 1_555 1_555 1_555 1_555 yes O3 C35 C36 C34 -7(1) 1_555 1_555 1_555 1_555 yes O3 C35 C36 C37 177.0(8) 1_555 1_555 1_555 1_555 yes O3 C35 C40 C39 -177.1(8) 1_555 1_555 1_555 1_555 yes O3 C35 C40 C45 6(1) 1_555 1_555 1_555 1_555 yes O3 C46 C48 C49 -71(1) 1_555 1_555 1_555 1_555 yes O3 C46 C48 C57 102(1) 1_555 1_555 1_555 1_555 yes O3 C46 C71 C72 86(1) 1_555 1_555 1_555 1_555 yes O3 C46 C71 C80 -90(1) 1_555 1_555 1_555 1_555 yes O4 C58 C59 C45 -2(1) 1_555 1_555 1_555 1_555 yes O4 C58 C59 C60 -179.2(9) 1_555 1_555 1_555 1_555 yes O4 C58 C63 C62 -179.5(9) 1_555 1_555 1_555 1_555 yes O4 C58 C63 C68 5(1) 1_555 1_555 1_555 1_555 yes C1 O1 C12 C13 51(1) 1_555 1_555 1_555 1_555 yes C1 O1 C12 C14 173.3(7) 1_555 1_555 1_555 1_555 yes C1 C2 C3 C4 0(1) 1_555 1_555 1_555 1_555 yes C1 C2 C68 C63 -104(1) 1_555 1_555 1_555 1_555 yes C1 C6 C5 C4 -1(1) 1_555 1_555 1_555 1_555 yes C1 C6 C11 C25 93.6(10) 1_555 1_555 1_555 1_555 yes C2 C1 O1 C12 -100.3(8) 1_555 1_555 1_555 1_555 yes C2 C1 C6 C5 4(1) 1_555 1_555 1_555 1_555 yes C2 C1 C6 C11 -169.2(7) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C5 2(1) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C7 -175.5(8) 1_555 1_555 1_555 1_555 yes C2 C68 C63 C58 90(1) 1_555 1_555 1_555 1_555 yes C2 C68 C63 C62 -83(1) 1_555 1_555 1_555 1_555 yes C3 C2 C1 C6 -4(1) 1_555 1_555 1_555 1_555 yes C3 C2 C68 C63 67(1) 1_555 1_555 1_555 1_555 yes C3 C4 C5 C6 -1(1) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C8 89(1) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C9 -150.8(9) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C10 -31(1) 1_555 1_555 1_555 1_555 yes C4 C3 C2 C68 -172.9(8) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C11 172.2(7) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C8 -87(1) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C9 31(1) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C10 151(1) 1_555 1_555 1_555 1_555 yes C5 C6 C11 C25 -80.2(10) 1_555 1_555 1_555 1_555 yes C6 C1 O1 C12 82.4(9) 1_555 1_555 1_555 1_555 yes C6 C1 C2 C68 168.8(7) 1_555 1_555 1_555 1_555 yes C6 C5 C4 C7 176.3(7) 1_555 1_555 1_555 1_555 yes C6 C11 C25 C24 -80(1) 1_555 1_555 1_555 1_555 yes C6 C11 C25 C26 94(1) 1_555 1_555 1_555 1_555 yes C11 C25 C24 C29 179.8(9) 1_555 1_555 1_555 1_555 yes C11 C25 C26 C27 -177.7(9) 1_555 1_555 1_555 1_555 yes C12 C14 C15 C16 -178.0(10) 1_555 1_555 1_555 1_555 yes C12 C14 C23 C22 178.0(9) 1_555 1_555 1_555 1_555 yes C13 C12 C14 C15 95(1) 1_555 1_555 1_555 1_555 yes C13 C12 C14 C23 -80(1) 1_555 1_555 1_555 1_555 yes C14 C15 C16 C17 0(1) 1_555 1_555 1_555 1_555 yes C14 C23 C22 C17 0(1) 1_555 1_555 1_555 1_555 yes C14 C23 C22 C21 -179(1) 1_555 1_555 1_555 1_555 yes C15 C14 C23 C22 2(1) 1_555 1_555 1_555 1_555 yes C15 C16 C17 C18 -179.7(10) 1_555 1_555 1_555 1_555 yes C15 C16 C17 C22 3(1) 1_555 1_555 1_555 1_555 yes C16 C15 C14 C23 -2(1) 1_555 1_555 1_555 1_555 yes C16 C17 C18 C19 -176(1) 1_555 1_555 1_555 1_555 yes C16 C17 C22 C21 176(1) 1_555 1_555 1_555 1_555 yes C16 C17 C22 C23 -3(1) 1_555 1_555 1_555 1_555 yes C17 C18 C19 C20 0(1) 1_555 1_555 1_555 1_555 yes C17 C22 C21 C20 0(1) 1_555 1_555 1_555 1_555 yes C18 C17 C22 C21 0(1) 1_555 1_555 1_555 1_555 yes C18 C17 C22 C23 179.7(10) 1_555 1_555 1_555 1_555 yes C18 C19 C20 C21 0(1) 1_555 1_555 1_555 1_555 yes C19 C18 C17 C22 0(1) 1_555 1_555 1_555 1_555 yes C19 C20 C21 C22 0(1) 1_555 1_555 1_555 1_555 yes C20 C21 C22 C23 -179(1) 1_555 1_555 1_555 1_555 yes C24 C25 C26 C27 -2(1) 1_555 1_555 1_555 1_555 yes C24 C29 C28 C27 0(1) 1_555 1_555 1_555 1_555 yes C24 C29 C34 C36 89(1) 1_555 1_555 1_555 1_555 yes C25 C24 C29 C28 -3(1) 1_555 1_555 1_555 1_555 yes C25 C24 C29 C34 -179.3(9) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C28 0(1) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C30 177.6(10) 1_555 1_555 1_555 1_555 yes C26 C25 C24 C29 4(1) 1_555 1_555 1_555 1_555 yes C26 C27 C28 C29 1(1) 1_555 1_555 1_555 1_555 yes C26 C27 C30 C31 132(1) 1_555 1_555 1_555 1_555 yes C26 C27 C30 C32 9(1) 1_555 1_555 1_555 1_555 yes C26 C27 C30 C33 -108(1) 1_555 1_555 1_555 1_555 yes C27 C28 C29 C34 176.0(9) 1_555 1_555 1_555 1_555 yes C28 C27 C30 C31 -49(1) 1_555 1_555 1_555 1_555 yes C28 C27 C30 C32 -171(1) 1_555 1_555 1_555 1_555 yes C28 C27 C30 C33 69(1) 1_555 1_555 1_555 1_555 yes C28 C29 C34 C36 -86(1) 1_555 1_555 1_555 1_555 yes C29 C28 C27 C30 -176.5(10) 1_555 1_555 1_555 1_555 yes C29 C34 C36 C35 -100(1) 1_555 1_555 1_555 1_555 yes C29 C34 C36 C37 75(1) 1_555 1_555 1_555 1_555 yes C34 C36 C35 C40 171.9(9) 1_555 1_555 1_555 1_555 yes C34 C36 C37 C38 -175.8(9) 1_555 1_555 1_555 1_555 yes C35 O3 C46 C47 148.0(9) 1_555 1_555 1_555 1_555 yes C35 O3 C46 C48 -107.4(9) 1_555 1_555 1_555 1_555 yes C35 O3 C46 C71 -78.0(10) 1_555 1_555 1_555 1_555 yes C35 C36 C37 C38 0(1) 1_555 1_555 1_555 1_555 yes C35 C40 C39 C38 0(1) 1_555 1_555 1_555 1_555 yes C35 C40 C45 C59 89(1) 1_555 1_555 1_555 1_555 yes C36 C35 O3 C46 -79(1) 1_555 1_555 1_555 1_555 yes C36 C35 C40 C39 3(1) 1_555 1_555 1_555 1_555 yes C36 C35 C40 C45 -172.3(9) 1_555 1_555 1_555 1_555 yes C36 C37 C38 C39 3(1) 1_555 1_555 1_555 1_555 yes C36 C37 C38 C41 -177.4(9) 1_555 1_555 1_555 1_555 yes C37 C36 C35 C40 -3(1) 1_555 1_555 1_555 1_555 yes C37 C38 C39 C40 -3(1) 1_555 1_555 1_555 1_555 yes C37 C38 C41 C42 -16(1) 1_555 1_555 1_555 1_555 yes C37 C38 C41 C43 -137(1) 1_555 1_555 1_555 1_555 yes C37 C38 C41 C44 103(1) 1_555 1_555 1_555 1_555 yes C38 C39 C40 C45 176.1(9) 1_555 1_555 1_555 1_555 yes C39 C38 C41 C42 163.2(10) 1_555 1_555 1_555 1_555 yes C39 C38 C41 C43 42(1) 1_555 1_555 1_555 1_555 yes C39 C38 C41 C44 -77(1) 1_555 1_555 1_555 1_555 yes C39 C40 C45 C59 -86(1) 1_555 1_555 1_555 1_555 yes C40 C35 O3 C46 101(1) 1_555 1_555 1_555 1_555 yes C40 C39 C38 C41 177.3(9) 1_555 1_555 1_555 1_555 yes C40 C45 C59 C58 -82(1) 1_555 1_555 1_555 1_555 yes C40 C45 C59 C60 94(1) 1_555 1_555 1_555 1_555 yes C45 C59 C58 C63 179.1(10) 1_555 1_555 1_555 1_555 yes C45 C59 C60 C61 179.9(10) 1_555 1_555 1_555 1_555 yes C46 C48 C49 C50 173(1) 1_555 1_555 1_555 1_555 yes C46 C48 C57 C56 -174(1) 1_555 1_555 1_555 1_555 yes C46 C71 C72 C73 -177.2(9) 1_555 1_555 1_555 1_555 yes C46 C71 C80 C79 177.3(9) 1_555 1_555 1_555 1_555 yes C47 C46 C48 C49 37(1) 1_555 1_555 1_555 1_555 yes C47 C46 C48 C57 -148(1) 1_555 1_555 1_555 1_555 yes C47 C46 C71 C72 -149(1) 1_555 1_555 1_555 1_555 yes C47 C46 C71 C80 32(1) 1_555 1_555 1_555 1_555 yes C58 C59 C60 C61 -3(1) 1_555 1_555 1_555 1_555 yes C58 C63 C62 C61 0(1) 1_555 1_555 1_555 1_555 yes C59 C58 C63 C62 -1(1) 1_555 1_555 1_555 1_555 yes C59 C58 C63 C68 -176(1) 1_555 1_555 1_555 1_555 yes C59 C60 C61 C62 3(1) 1_555 1_555 1_555 1_555 yes C59 C60 C61 C64 179(1) 1_555 1_555 1_555 1_555 yes C60 C59 C58 C63 2(1) 1_555 1_555 1_555 1_555 yes C60 C61 C62 C63 -1(1) 1_555 1_555 1_555 1_555 yes C60 C61 C64 C65 64(1) 1_555 1_555 1_555 1_555 yes C60 C61 C64 C66 173(1) 1_555 1_555 1_555 1_555 yes C60 C61 C64 C67 -72(1) 1_555 1_555 1_555 1_555 yes C61 C62 C63 C68 175(1) 1_555 1_555 1_555 1_555 yes C62 C61 C64 C65 -118(1) 1_555 1_555 1_555 1_555 yes C62 C61 C64 C66 -10(1) 1_555 1_555 1_555 1_555 yes C62 C61 C64 C67 104(1) 1_555 1_555 1_555 1_555 yes C63 C62 C61 C64 -177(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O2 C54 3.33(2) . 1_455 ? O2 C53 3.43(2) . 1_455 ? O2 C76 3.48(1) . 1_455 ? O3 C80 3.23(1) . 1_555 ? O3 C49 3.24(1) . 1_555 ? O3 C72 3.25(1) . 1_555 ? O3 C57 3.33(1) . 1_555 ? C13 C78 3.46(1) . 2_656 ? C18 C63 3.39(2) . 2_646 ? C18 C58 3.47(1) . 2_646 ? C19 C50 3.48(2) . 2_646 ? C19 C58 3.59(2) . 2_646 ? C23 C77 3.57(2) . 1_455 ? C24 C54 3.38(2) . 1_455 ? C25 C54 3.56(2) . 1_455 ? C25 C75 3.58(1) . 1_455 ? C66 C49 3.54(2) . 1_565 ? #------------------------------------------------------------------------------ # Attachment 'B801434P_calix7.cif' data_Andrei_Solovyov_chiral_cal _database_code_depnum_ccdc_archive 'CCDC 685847' # CHEMICAL DATA _chemical_formula_sum 'C78 H110 N2 O12 ' _chemical_formula_moiety 'C70 H86 N2 O8, 4(C2 H6 O) ' _chemical_formula_weight 1267.73 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 13.170(1) _cell_length_b 19.498(2) _cell_length_c 14.880(2) _cell_angle_alpha 90 _cell_angle_beta 107.687(2) _cell_angle_gamma 90 _cell_volume 3640.3(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2822 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 23.5 _cell_measurement_temperature 180.2 #------------------------------------------------------------------------------ _exptl_crystal_description bladelike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376.00 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 20876 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 26.38 _diffrn_measured_fraction_theta_max 0.9857 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.9857 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). One of the t-butyl groups was disordered. Adjustment of the occupancies to give approximately equal Biso gave 60:40 occupancy ratio. This disorder accounts for many of the nominally unlikely bond distances in the CIF. Three of the four ethanol molecules were ordered but the last was grossly disordered. It appears to have (at least) three different orientations in the same region of space. Hydrogen atoms were included in calculated positions for all atoms in the molecule, including the disordered t-butyl group and for the three ordered ethanol molecules. Hydroxyl hydrogen atoms were included in locations picked from a difference Fourier map and not adjusted. No hydrogen atoms were included for the disordered ethanol. ; _reflns_number_total 7590 _reflns_number_gt 5585 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.0587 _refine_ls_R_factor_all 0.0896 _refine_ls_wR_factor_all 0.0634 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5585 _refine_ls_number_parameters 826 _refine_ls_goodness_of_fit_ref 1.674 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0079 _refine_diff_density_max 0.36 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details . _refine_ls_abs_structure_Flack . _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.631' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution SIR97 _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics teXsan #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0088(2) 0.2754 -0.0266(2) 0.0249(7) Uani 1.00 d . . . O2 O -0.1577(2) 0.1895(2) 0.0167(2) 0.0304(8) Uani 1.00 d . . . O3 O -0.0932(2) 0.0544(2) 0.0153(2) 0.0272(8) Uani 1.00 d . . . O4 O 0.0208(2) 0.1411(2) -0.0803(2) 0.0317(8) Uani 1.00 d . . . O5 O -0.1136(3) 0.2491(2) 0.2316(2) 0.048(1) Uani 1.00 d . . . O6 O 0.0178(3) 0.3264(3) 0.2925(3) 0.088(2) Uani 1.00 d . . . O7 O 0.2615(2) 0.0943(2) 0.0453(2) 0.0442(10) Uani 1.00 d . . . O8 O 0.2845(3) 0.0151(2) 0.1608(3) 0.051(1) Uani 1.00 d . . . O9 O -0.3837(3) 0.1683(3) -0.3007(3) 0.084(2) Uani 1.00 d . . . O10 O -0.5183(5) 0.1650(5) -0.4889(4) 0.162(3) Uani 1.00 d . . . O11 O 0.4854(3) -0.0432(3) 0.2282(3) 0.084(2) Uani 1.00 d . . . O12 O 0.0456(9) 0.3097(6) 0.4944(8) 0.113(4) Uiso 0.50 d P . . O13 O 0.137(1) 0.402(1) 0.419(1) 0.090(5) Uiso 0.25 d P . . O14 O 0.226(3) 0.307(2) 0.475(2) 0.18(1) Uiso 0.25 d P . . N1 N 0.0064(3) 0.2666(2) 0.1587(2) 0.035(1) Uani 1.00 d . . . N2 N 0.1240(3) 0.0658(2) 0.0918(2) 0.033(1) Uani 1.00 d . . . C1 C -0.0552(3) 0.3006(2) -0.1137(3) 0.025(1) Uani 1.00 d . . . C2 C -0.0221(3) 0.2910(2) -0.1933(3) 0.025(1) Uani 1.00 d . . . C3 C -0.0852(3) 0.3163(2) -0.2796(3) 0.028(1) Uani 1.00 d . . . C4 C -0.1814(3) 0.3498(2) -0.2894(3) 0.028(1) Uani 1.00 d . . . C5 C -0.2145(3) 0.3552(2) -0.2089(3) 0.029(1) Uani 1.00 d . . . C6 C -0.1548(3) 0.3300(2) -0.1215(3) 0.024(1) Uani 1.00 d . . . C7 C -0.2519(3) 0.3785(3) -0.3842(3) 0.037(1) Uani 1.00 d . . . C8 C -0.2545(4) 0.4565(3) -0.3774(3) 0.049(2) Uani 1.00 d . . . C9 C -0.3654(4) 0.3497(3) -0.4061(4) 0.054(2) Uani 1.00 d . . . C10 C -0.2083(4) 0.3593(3) -0.4650(3) 0.050(2) Uani 1.00 d . . . C11 C -0.2043(3) 0.3277(2) -0.0418(3) 0.027(1) Uani 1.00 d . . . C12 C -0.2630(3) 0.2039(2) -0.0294(3) 0.028(1) Uani 1.00 d . . . C13 C -0.2892(3) 0.2719(3) -0.0587(3) 0.027(1) Uani 1.00 d . . . C14 C -0.3941(3) 0.2869(3) -0.1068(3) 0.031(1) Uani 1.00 d . . . C15 C -0.4746(3) 0.2378(3) -0.1288(3) 0.033(1) Uani 1.00 d . . . C16 C -0.4458(3) 0.1715(3) -0.0959(3) 0.031(1) Uani 1.00 d . . . C17 C -0.3414(3) 0.1536(2) -0.0449(3) 0.028(1) Uani 1.00 d . . . C18 C -0.5870(3) 0.2575(3) -0.1884(3) 0.039(1) Uani 1.00 d . . . C19 C -0.6615(4) 0.1967(3) -0.2112(4) 0.061(2) Uani 1.00 d . . . C20 C -0.6315(4) 0.3119(3) -0.1355(4) 0.057(2) Uani 1.00 d . . . C21 C -0.5829(4) 0.2887(3) -0.2813(4) 0.060(2) Uani 1.00 d . . . C22 C -0.3152(3) 0.0806(2) -0.0106(3) 0.030(1) Uani 1.00 d . . . C23 C -0.1673(3) 0.0307(2) -0.0677(3) 0.026(1) Uani 1.00 d . . . C24 C -0.2751(3) 0.0386(2) -0.0787(3) 0.029(1) Uani 1.00 d . . . C25 C -0.3484(3) 0.0120(3) -0.1600(3) 0.035(1) Uani 1.00 d . . . C26 C -0.3183(4) -0.0202(3) -0.2311(3) 0.037(1) Uani 1.00 d . . . C27 C -0.2089(4) -0.0219(3) -0.2194(3) 0.034(1) Uani 1.00 d . . . C28 C -0.1325(3) 0.0034(2) -0.1401(3) 0.030(1) Uani 1.00 d . . . C29 C -0.3993(4) -0.0524(3) -0.3180(3) 0.046(2) Uani 1.00 d . . . C30 C -0.4099(8) -0.1256(4) -0.2996(7) 0.155(4) Uani 1.00 d . . . C31 C -0.5096(6) -0.0188(5) -0.3366(6) 0.123(3) Uani 1.00 d . . . C32 C -0.3702(7) -0.0406(8) -0.4057(5) 0.195(5) Uani 1.00 d . . . C33 C -0.0171(4) 0.0037(3) -0.1393(3) 0.033(1) Uani 1.00 d . . . C34 C 0.0250(3) 0.1271(3) -0.1697(3) 0.028(1) Uani 1.00 d . . . C35 C 0.0063(3) 0.0591(3) -0.2010(3) 0.029(1) Uani 1.00 d . . . C36 C 0.0085(4) 0.0442(3) -0.2915(3) 0.036(1) Uani 1.00 d . . . C37 C 0.0313(3) 0.0927(3) -0.3507(3) 0.036(1) Uani 1.00 d . . . C38 C 0.0528(3) 0.1584(3) -0.3154(3) 0.034(1) Uani 1.00 d . . . C39 C 0.0516(3) 0.1774(2) -0.2258(3) 0.026(1) Uani 1.00 d . . . C40 C 0.0317(4) 0.0747(3) -0.4506(3) 0.050(2) Uani 1.00 d . . . C41 C -0.0001(9) -0.0003(6) -0.4767(8) 0.073(3) Uiso 0.60 d P . . C42 C 0.086(1) 0.0148(9) -0.460(1) 0.073(4) Uiso 0.40 d P . . C43 C 0.1478(10) 0.0841(7) -0.4533(9) 0.092(4) Uiso 0.60 d P . . C44 C 0.064(1) 0.1387(8) -0.503(1) 0.068(4) Uiso 0.40 d P . . C45 C -0.0392(9) 0.1189(6) -0.5175(8) 0.079(3) Uiso 0.60 d P . . C46 C -0.092(1) 0.0690(7) -0.5109(10) 0.056(4) Uiso 0.40 d P . . C47 C 0.0763(3) 0.2497(2) -0.1910(3) 0.027(1) Uani 1.00 d . . . C48 C 0.0686(3) 0.3270(2) 0.0382(3) 0.028(1) Uani 1.00 d . . . C49 C 0.1775(3) 0.3395(2) 0.0265(3) 0.032(1) Uani 1.00 d . . . C50 C 0.2445(4) 0.2766(3) 0.0736(3) 0.042(1) Uani 1.00 d . . . C51 C 0.1896(3) 0.2485(3) 0.1432(3) 0.039(1) Uani 1.00 d . . . C52 C 0.0972(3) 0.2971(2) 0.1379(3) 0.031(1) Uani 1.00 d . . . C53 C -0.0247(4) 0.2844(3) 0.2333(3) 0.048(2) Uani 1.00 d . . . C54 C -0.1593(4) 0.2646(4) 0.3056(4) 0.066(2) Uani 1.00 d . . . C55 C -0.2711(4) 0.2370(3) 0.2782(3) 0.047(2) Uani 1.00 d . . . C56 C -0.3341(5) 0.2336(3) 0.1852(4) 0.057(2) Uani 1.00 d . . . C57 C -0.4398(5) 0.2125(3) 0.1628(4) 0.062(2) Uani 1.00 d . . . C58 C -0.4825(5) 0.1960(3) 0.2328(4) 0.061(2) Uani 1.00 d . . . C59 C -0.4206(5) 0.1980(3) 0.3264(4) 0.066(2) Uani 1.00 d . . . C60 C -0.3157(5) 0.2169(3) 0.3470(4) 0.056(2) Uani 1.00 d . . . C61 C -0.0401(3) 0.0007(2) 0.0820(3) 0.029(1) Uani 1.00 d . . . C62 C -0.1001(4) -0.0169(3) 0.1505(3) 0.039(1) Uani 1.00 d . . . C63 C -0.0705(4) 0.0397(3) 0.2264(3) 0.051(2) Uani 1.00 d . . . C64 C 0.0268(4) 0.0755(3) 0.2135(3) 0.041(1) Uani 1.00 d . . . C65 C 0.0628(4) 0.0313(2) 0.1446(3) 0.032(1) Uani 1.00 d . . . C66 C 0.2274(4) 0.0546(3) 0.1049(3) 0.038(1) Uani 1.00 d . . . C67 C 0.3652(4) 0.0770(3) 0.0353(4) 0.047(2) Uani 1.00 d . . . C68 C 0.3575(4) 0.0192(3) -0.0324(4) 0.042(1) Uani 1.00 d . . . C69 C 0.2801(4) 0.0199(3) -0.1201(4) 0.056(2) Uani 1.00 d . . . C70 C 0.2733(4) -0.0318(4) -0.1848(4) 0.066(2) Uani 1.00 d . . . C71 C 0.3438(5) -0.0863(4) -0.1607(5) 0.069(2) Uani 1.00 d . . . C72 C 0.4208(5) -0.0876(3) -0.0747(5) 0.066(2) Uani 1.00 d . . . C73 C 0.4272(4) -0.0350(3) -0.0097(4) 0.051(2) Uani 1.00 d . . . C74 C -0.2726(4) 0.1652(3) -0.2793(3) 0.048(2) Uani 1.00 d . . . C75 C -0.2457(4) 0.1524(4) -0.3681(4) 0.060(2) Uani 1.00 d . . . C76 C -0.6160(7) 0.1547(7) -0.5067(6) 0.151(4) Uani 1.00 d . . . C77 C -0.6803(6) 0.1586(6) -0.6025(6) 0.124(3) Uani 1.00 d . . . C78 C 0.5528(6) -0.0082(4) 0.3060(6) 0.095(3) Uani 1.00 d . . . C79 C 0.6521(9) 0.0104(6) 0.290(1) 0.175(5) Uani 1.00 d . . . C80 C 0.130(1) 0.3406(9) 0.549(1) 0.142(5) Uiso 0.75 d P . . C81 C 0.198(1) 0.3640(8) 0.505(1) 0.144(5) Uiso 0.75 d P . . C83 C 0.132(3) 0.383(2) 0.618(2) 0.11(1) Uiso 0.25 d P . . C84 C 0.140(4) 0.281(3) 0.507(3) 0.15(1) Uiso 0.25 d P . . H1 H -0.0668 -0.0100 -0.4728 0.0863 Uiso 0.60 calc P . . H2 H 0.0076 -0.0110 -0.5360 0.0863 Uiso 0.60 calc P . . H3 H 0.0522 -0.0300 -0.4301 0.0863 Uiso 0.60 calc P . . H4 H 0.1970 0.0623 -0.4156 0.1140 Uiso 0.60 calc P . . H5 H 0.1464 0.0811 -0.5211 0.1140 Uiso 0.60 calc P . . H6 H 0.1605 0.1370 -0.4439 0.1140 Uiso 0.60 calc P . . H7 H -0.0234 0.1621 -0.5016 0.1012 Uiso 0.60 calc P . . H8 H -0.0383 0.1060 -0.5784 0.1012 Uiso 0.60 calc P . . H9 H -0.1117 0.1071 -0.5142 0.1012 Uiso 0.60 calc P . . H10 H 0.0513 -0.0236 -0.4448 0.0855 Uiso 0.40 calc P . . H11 H 0.0742 0.0110 -0.5306 0.0855 Uiso 0.40 calc P . . H12 H 0.1552 0.0182 -0.4307 0.0855 Uiso 0.40 calc P . . H13 H 0.1342 0.1537 -0.4786 0.0922 Uiso 0.40 calc P . . H14 H 0.0467 0.1333 -0.5708 0.0922 Uiso 0.40 calc P . . H15 H 0.0185 0.1802 -0.4976 0.0922 Uiso 0.40 calc P . . H16 H -0.1282 0.1073 -0.5002 0.0710 Uiso 0.40 calc P . . H17 H -0.0990 0.0629 -0.5753 0.0710 Uiso 0.40 calc P . . H18 H -0.1226 0.0281 -0.4899 0.0710 Uiso 0.40 calc P . . H19 H -0.0620 0.3104 -0.3337 0.0340 Uiso 1.00 calc . . . H20 H -0.2802 0.3772 -0.2142 0.0353 Uiso 1.00 calc . . . H21 H -0.1843 0.4740 -0.3654 0.0594 Uiso 1.00 calc . . . H22 H -0.2990 0.4746 -0.4352 0.0594 Uiso 1.00 calc . . . H23 H -0.2816 0.4692 -0.3276 0.0594 Uiso 1.00 calc . . . H24 H -0.3946 0.3622 -0.3575 0.0647 Uiso 1.00 calc . . . H25 H -0.4087 0.3675 -0.4646 0.0647 Uiso 1.00 calc . . . H26 H -0.3633 0.3009 -0.4101 0.0647 Uiso 1.00 calc . . . H27 H -0.2070 0.3105 -0.4704 0.0598 Uiso 1.00 calc . . . H28 H -0.2528 0.3779 -0.5223 0.0598 Uiso 1.00 calc . . . H29 H -0.1381 0.3766 -0.4526 0.0598 Uiso 1.00 calc . . . H30 H -0.1501 0.3184 0.0157 0.0317 Uiso 1.00 calc . . . H31 H -0.2361 0.3707 -0.0377 0.0317 Uiso 1.00 calc . . . H32 H -0.4121 0.3327 -0.1256 0.0369 Uiso 1.00 calc . . . H33 H -0.4993 0.1370 -0.1086 0.0376 Uiso 1.00 calc . . . H34 H -0.7302 0.2111 -0.2487 0.0727 Uiso 1.00 calc . . . H35 H -0.6348 0.1633 -0.2447 0.0727 Uiso 1.00 calc . . . H36 H -0.6667 0.1770 -0.1541 0.0727 Uiso 1.00 calc . . . H37 H -0.5874 0.3512 -0.1245 0.0688 Uiso 1.00 calc . . . H38 H -0.7019 0.3241 -0.1721 0.0688 Uiso 1.00 calc . . . H39 H -0.6335 0.2934 -0.0767 0.0688 Uiso 1.00 calc . . . H40 H -0.5388 0.3280 -0.2689 0.0716 Uiso 1.00 calc . . . H41 H -0.5549 0.2557 -0.3146 0.0716 Uiso 1.00 calc . . . H42 H -0.6529 0.3010 -0.3184 0.0716 Uiso 1.00 calc . . . H43 H -0.2619 0.0813 0.0490 0.0367 Uiso 1.00 calc . . . H44 H -0.3778 0.0594 -0.0041 0.0367 Uiso 1.00 calc . . . H45 H -0.4223 0.0163 -0.1669 0.0425 Uiso 1.00 calc . . . H46 H -0.1856 -0.0414 -0.2681 0.0412 Uiso 1.00 calc . . . H47 H -0.4358 -0.1309 -0.2473 0.1835 Uiso 1.00 calc . . . H48 H -0.4596 -0.1459 -0.3541 0.1835 Uiso 1.00 calc . . . H49 H -0.3431 -0.1475 -0.2879 0.1835 Uiso 1.00 calc . . . H50 H -0.5040 0.0288 -0.3476 0.1453 Uiso 1.00 calc . . . H51 H -0.5583 -0.0392 -0.3908 0.1453 Uiso 1.00 calc . . . H52 H -0.5341 -0.0253 -0.2837 0.1453 Uiso 1.00 calc . . . H53 H -0.3026 -0.0595 -0.3989 0.2360 Uiso 1.00 calc . . . H54 H -0.4224 -0.0615 -0.4570 0.2360 Uiso 1.00 calc . . . H55 H -0.3693 0.0075 -0.4163 0.2360 Uiso 1.00 calc . . . H56 H 0.0269 0.0106 -0.0763 0.0403 Uiso 1.00 calc . . . H57 H -0.0011 -0.0396 -0.1611 0.0403 Uiso 1.00 calc . . . H58 H -0.0060 -0.0016 -0.3138 0.0429 Uiso 1.00 calc . . . H59 H 0.0696 0.1923 -0.3544 0.0407 Uiso 1.00 calc . . . H60 H 0.1120 0.2719 -0.2296 0.0326 Uiso 1.00 calc . . . H61 H 0.1220 0.2481 -0.1278 0.0326 Uiso 1.00 calc . . . H62 H 0.0296 0.3684 0.0333 0.0337 Uiso 1.00 calc . . . H63 H 0.1730 0.3418 -0.0384 0.0379 Uiso 1.00 calc . . . H64 H 0.2080 0.3805 0.0572 0.0379 Uiso 1.00 calc . . . H65 H 0.2451 0.2429 0.0275 0.0505 Uiso 1.00 calc . . . H66 H 0.3155 0.2899 0.1059 0.0505 Uiso 1.00 calc . . . H67 H 0.1639 0.2033 0.1255 0.0467 Uiso 1.00 calc . . . H68 H 0.2382 0.2477 0.2052 0.0467 Uiso 1.00 calc . . . H69 H 0.1234 0.3332 0.1816 0.0367 Uiso 1.00 calc . . . H70 H -0.1183 0.2433 0.3626 0.0793 Uiso 1.00 calc . . . H71 H -0.1605 0.3125 0.3142 0.0793 Uiso 1.00 calc . . . H72 H -0.3049 0.2459 0.1365 0.0684 Uiso 1.00 calc . . . H73 H -0.4819 0.2090 0.0988 0.0742 Uiso 1.00 calc . . . H74 H -0.5551 0.1830 0.2174 0.0728 Uiso 1.00 calc . . . H75 H -0.4498 0.1862 0.3757 0.0788 Uiso 1.00 calc . . . H76 H -0.2722 0.2164 0.4109 0.0663 Uiso 1.00 calc . . . H77 H -0.0270 -0.0391 0.0502 0.0348 Uiso 1.00 calc . . . H78 H -0.1746 -0.0171 0.1196 0.0462 Uiso 1.00 calc . . . H79 H -0.0787 -0.0607 0.1782 0.0462 Uiso 1.00 calc . . . H80 H -0.1278 0.0712 0.2175 0.0608 Uiso 1.00 calc . . . H81 H -0.0541 0.0202 0.2877 0.0608 Uiso 1.00 calc . . . H82 H 0.0082 0.1200 0.1884 0.0490 Uiso 1.00 calc . . . H83 H 0.0813 0.0784 0.2721 0.0490 Uiso 1.00 calc . . . H84 H 0.1051 -0.0051 0.1791 0.0382 Uiso 1.00 calc . . . H85 H 0.3933 0.1159 0.0133 0.0562 Uiso 1.00 calc . . . H86 H 0.4117 0.0637 0.0954 0.0562 Uiso 1.00 calc . . . H87 H 0.2305 0.0565 -0.1359 0.0663 Uiso 1.00 calc . . . H88 H 0.2211 -0.0302 -0.2453 0.0783 Uiso 1.00 calc . . . H89 H 0.3386 -0.1233 -0.2037 0.0824 Uiso 1.00 calc . . . H90 H 0.4700 -0.1246 -0.0593 0.0791 Uiso 1.00 calc . . . H91 H 0.4800 -0.0369 0.0502 0.0606 Uiso 1.00 calc . . . H92 H -0.2424 0.2074 -0.2524 0.0576 Uiso 1.00 calc . . . H93 H -0.2453 0.1290 -0.2358 0.0576 Uiso 1.00 calc . . . H94 H -0.2768 0.1101 -0.3952 0.0722 Uiso 1.00 calc . . . H95 H -0.2731 0.1886 -0.4114 0.0722 Uiso 1.00 calc . . . H96 H -0.1707 0.1499 -0.3547 0.0722 Uiso 1.00 calc . . . H97 H -0.6230 0.1095 -0.4848 0.1801 Uiso 1.00 calc . . . H98 H -0.6420 0.1869 -0.4718 0.1801 Uiso 1.00 calc . . . H99 H -0.6864 0.2051 -0.6224 0.1488 Uiso 1.00 calc . . . H100 H -0.6481 0.1328 -0.6411 0.1488 Uiso 1.00 calc . . . H101 H -0.7487 0.1405 -0.6084 0.1488 Uiso 1.00 calc . . . H102 H 0.5181 0.0325 0.3167 0.1134 Uiso 1.00 calc . . . H103 H 0.5676 -0.0366 0.3603 0.1134 Uiso 1.00 calc . . . H104 H 0.6882 -0.0296 0.2805 0.2119 Uiso 1.00 calc . . . H105 H 0.6385 0.0395 0.2366 0.2119 Uiso 1.00 calc . . . H106 H 0.6961 0.0345 0.3441 0.2119 Uiso 1.00 calc . . . H112 H -0.0311 0.2341 0.1195 0.0416 Uiso 1.00 calc . . . H113 H 0.0902 0.0964 0.0477 0.0396 Uiso 1.00 calc . . . H114 H -0.1494 0.1449 0.0172 0.0620 Uiso 1.00 calc . . . H115 H 0.0468 0.1874 -0.0650 0.0620 Uiso 1.00 calc . . . H116 H -0.4238 0.1502 -0.2497 0.0620 Uiso 1.00 calc . . . H117 H 0.4182 -0.0189 0.1879 0.0620 Uiso 1.00 calc . . . H118 H -0.4698 0.1875 -0.4387 0.0620 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.023(1) 0.023(1) 0.023(1) -0.002(1) 0.000(1) 0.000(1) O2 0.026(2) 0.025(2) 0.035(2) -0.000(1) 0.001(1) 0.000(1) O3 0.031(2) 0.024(2) 0.023(2) -0.002(1) 0.003(1) -0.002(1) O4 0.046(2) 0.026(2) 0.023(2) 0.001(1) 0.010(1) -0.001(1) O5 0.054(2) 0.059(2) 0.039(2) -0.016(2) 0.024(2) -0.010(2) O6 0.082(3) 0.140(4) 0.050(2) -0.055(3) 0.030(2) -0.048(3) O7 0.041(2) 0.039(2) 0.056(2) 0.001(2) 0.021(2) 0.008(2) O8 0.040(2) 0.055(2) 0.056(2) 0.011(2) 0.011(2) 0.023(2) O9 0.062(3) 0.136(4) 0.059(3) 0.019(3) 0.028(2) 0.006(3) O10 0.090(4) 0.31(1) 0.076(4) -0.047(5) 0.011(3) 0.013(5) O11 0.063(3) 0.094(3) 0.079(3) 0.025(2) -0.001(2) -0.002(3) N1 0.046(2) 0.033(2) 0.026(2) -0.010(2) 0.012(2) -0.004(2) N2 0.032(2) 0.032(2) 0.032(2) 0.005(2) 0.004(2) 0.010(2) C1 0.026(2) 0.016(2) 0.028(2) -0.003(2) 0.001(2) -0.000(2) C2 0.021(2) 0.026(2) 0.028(2) -0.003(2) 0.007(2) -0.001(2) C3 0.028(2) 0.032(2) 0.026(2) -0.002(2) 0.009(2) -0.001(2) C4 0.028(2) 0.026(2) 0.028(2) -0.005(2) 0.005(2) 0.003(2) C5 0.022(2) 0.023(2) 0.042(3) -0.003(2) 0.007(2) -0.003(2) C6 0.022(2) 0.015(2) 0.032(2) -0.003(2) 0.003(2) -0.000(2) C7 0.034(3) 0.038(3) 0.031(3) 0.001(2) -0.002(2) 0.010(2) C8 0.063(3) 0.045(3) 0.033(3) 0.011(3) 0.004(2) 0.008(2) C9 0.035(3) 0.065(4) 0.048(3) -0.000(3) -0.008(2) 0.018(3) C10 0.058(3) 0.054(3) 0.033(3) 0.008(3) 0.006(3) 0.008(2) C11 0.024(2) 0.021(2) 0.032(2) 0.003(2) 0.004(2) -0.001(2) C12 0.028(2) 0.029(2) 0.026(2) -0.001(2) 0.009(2) -0.005(2) C13 0.026(2) 0.032(2) 0.026(2) -0.002(2) 0.011(2) -0.005(2) C14 0.032(2) 0.031(3) 0.034(2) 0.006(2) 0.016(2) -0.002(2) C15 0.025(2) 0.044(3) 0.035(3) 0.000(2) 0.014(2) -0.004(2) C16 0.027(2) 0.035(3) 0.035(3) -0.007(2) 0.014(2) -0.005(2) C17 0.033(2) 0.027(2) 0.028(2) -0.003(2) 0.013(2) 0.001(2) C18 0.025(2) 0.050(3) 0.040(3) 0.002(2) 0.007(2) -0.002(2) C19 0.028(3) 0.056(4) 0.090(4) -0.000(2) 0.003(3) -0.001(3) C20 0.036(3) 0.061(4) 0.073(4) 0.010(3) 0.014(3) -0.006(3) C21 0.036(3) 0.079(4) 0.059(4) 0.008(3) 0.004(3) -0.002(3) C22 0.031(2) 0.033(2) 0.026(2) -0.009(2) 0.007(2) 0.002(2) C23 0.036(3) 0.019(2) 0.019(2) -0.004(2) 0.003(2) -0.000(2) C24 0.035(3) 0.021(2) 0.030(2) -0.007(2) 0.010(2) 0.006(2) C25 0.032(3) 0.036(3) 0.037(3) -0.003(2) 0.008(2) 0.004(2) C26 0.047(3) 0.034(3) 0.027(2) -0.015(2) 0.007(2) 0.000(2) C27 0.049(3) 0.027(2) 0.028(3) -0.004(2) 0.013(2) -0.002(2) C28 0.037(3) 0.019(2) 0.032(3) -0.003(2) 0.007(2) -0.000(2) C29 0.053(3) 0.047(3) 0.031(3) -0.011(2) 0.002(2) -0.005(2) C30 0.192(9) 0.045(4) 0.132(8) -0.044(5) -0.092(7) 0.007(5) C31 0.090(5) 0.152(8) 0.077(5) 0.012(5) -0.047(4) -0.047(5) C32 0.136(7) 0.41(2) 0.042(4) -0.17(1) 0.026(5) -0.070(7) C33 0.045(3) 0.027(2) 0.029(2) 0.003(2) 0.012(2) -0.005(2) C34 0.020(2) 0.036(3) 0.026(2) 0.002(2) 0.004(2) -0.000(2) C35 0.028(2) 0.033(3) 0.027(2) 0.001(2) 0.009(2) -0.004(2) C36 0.035(3) 0.036(3) 0.037(3) -0.002(2) 0.013(2) -0.007(2) C37 0.029(2) 0.051(3) 0.028(2) 0.001(2) 0.010(2) -0.006(2) C38 0.028(2) 0.044(3) 0.032(3) -0.000(2) 0.012(2) -0.001(2) C39 0.019(2) 0.033(2) 0.025(2) 0.003(2) 0.005(2) -0.000(2) C40 0.061(3) 0.056(3) 0.039(3) -0.001(3) 0.025(3) -0.011(3) C47 0.022(2) 0.032(2) 0.026(2) -0.002(2) 0.005(2) 0.002(2) C48 0.027(2) 0.022(2) 0.033(2) -0.001(2) 0.006(2) -0.005(2) C49 0.030(2) 0.027(2) 0.033(2) -0.001(2) 0.001(2) -0.001(2) C50 0.034(3) 0.040(3) 0.042(3) 0.004(2) -0.003(2) -0.003(2) C51 0.033(3) 0.035(3) 0.043(3) 0.000(2) -0.000(2) 0.008(2) C52 0.036(3) 0.025(2) 0.029(2) -0.006(2) 0.007(2) -0.006(2) C53 0.049(3) 0.067(4) 0.024(3) -0.009(3) 0.004(2) -0.002(3) C54 0.060(4) 0.102(5) 0.039(3) -0.009(3) 0.020(3) -0.013(3) C55 0.047(3) 0.062(3) 0.031(3) 0.000(3) 0.014(2) -0.009(3) C56 0.060(4) 0.077(4) 0.041(3) -0.007(3) 0.025(3) -0.006(3) C57 0.060(4) 0.077(4) 0.044(3) -0.008(3) 0.010(3) -0.015(3) C58 0.059(4) 0.072(4) 0.057(4) -0.007(3) 0.027(3) -0.012(3) C59 0.071(4) 0.078(4) 0.060(4) -0.011(3) 0.036(3) -0.007(3) C60 0.065(4) 0.072(4) 0.034(3) 0.002(3) 0.021(3) -0.006(3) C61 0.040(3) 0.017(2) 0.028(2) 0.002(2) 0.006(2) 0.001(2) C62 0.044(3) 0.040(3) 0.031(3) -0.005(2) 0.010(2) 0.005(2) C63 0.053(3) 0.063(4) 0.034(3) -0.003(3) 0.011(3) -0.000(3) C64 0.050(3) 0.037(3) 0.031(3) -0.001(2) 0.007(2) -0.003(2) C65 0.042(3) 0.024(2) 0.030(2) 0.002(2) 0.009(2) 0.004(2) C66 0.040(3) 0.033(3) 0.038(3) -0.005(2) 0.009(2) 0.001(2) C67 0.040(3) 0.043(3) 0.060(3) -0.007(2) 0.020(3) 0.006(3) C68 0.039(3) 0.036(3) 0.054(3) -0.004(2) 0.018(3) 0.007(2) C69 0.038(3) 0.048(3) 0.076(4) 0.010(2) 0.012(3) -0.000(3) C70 0.050(3) 0.073(4) 0.066(4) 0.009(3) 0.006(3) -0.012(3) C71 0.072(4) 0.062(4) 0.076(5) 0.010(3) 0.025(4) -0.007(3) C72 0.074(4) 0.061(4) 0.063(4) 0.029(3) 0.021(4) 0.014(3) C73 0.047(3) 0.052(3) 0.057(3) 0.007(3) 0.021(3) 0.009(3) C74 0.048(3) 0.048(3) 0.043(3) -0.006(3) 0.005(2) 0.002(2) C75 0.044(3) 0.081(4) 0.056(3) -0.003(3) 0.016(3) -0.006(3) C76 0.069(5) 0.28(1) 0.088(6) -0.048(7) -0.000(5) 0.035(8) C77 0.077(5) 0.20(1) 0.078(5) -0.042(6) 0.001(4) 0.024(6) C78 0.075(5) 0.097(6) 0.092(6) -0.010(4) -0.006(4) 0.002(5) C79 0.110(8) 0.125(9) 0.27(2) -0.029(7) 0.032(9) -0.037(9) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.402(4) . . yes O1 C48 1.449(4) . . yes O2 C12 1.376(5) . . yes O3 C23 1.400(4) . . yes O3 C61 1.467(5) . . yes O4 C34 1.376(5) . . yes O5 C53 1.352(7) . . yes O5 C54 1.439(7) . . yes O6 C53 1.209(7) . . yes O7 C66 1.352(7) . . yes O7 C67 1.459(6) . . yes O8 C66 1.213(6) . . yes O9 C74 1.401(7) . . yes O10 C76 1.25(1) . . yes O11 C78 1.404(9) . . yes O12 C80 1.31(2) . . yes O12 C84 1.33(5) . . yes O13 C81 1.48(2) . . yes O14 C81 1.28(4) . . yes O14 C84 1.45(7) . . yes N1 C52 1.451(6) . . yes N1 C53 1.339(7) . . yes N2 C65 1.450(7) . . yes N2 C66 1.334(6) . . yes C1 C2 1.394(7) . . yes C1 C6 1.404(6) . . yes C2 C3 1.390(5) . . yes C2 C47 1.518(6) . . yes C3 C4 1.393(6) . . yes C4 C5 1.397(7) . . yes C4 C7 1.538(6) . . yes C5 C6 1.390(6) . . yes C6 C11 1.517(7) . . yes C7 C8 1.526(8) . . yes C7 C9 1.536(7) . . yes C7 C10 1.529(8) . . yes C11 C13 1.526(6) . . yes C12 C13 1.405(7) . . yes C12 C17 1.391(6) . . yes C13 C14 1.380(5) . . yes C14 C15 1.391(7) . . yes C15 C16 1.393(7) . . yes C15 C18 1.526(6) . . yes C16 C17 1.398(5) . . yes C17 C22 1.516(7) . . yes C18 C19 1.511(8) . . yes C18 C20 1.539(8) . . yes C18 C21 1.525(8) . . yes C22 C24 1.517(7) . . yes C23 C24 1.388(6) . . yes C23 C28 1.398(7) . . yes C24 C25 1.398(6) . . yes C25 C26 1.388(7) . . yes C26 C27 1.398(7) . . yes C26 C29 1.538(6) . . yes C27 C28 1.387(6) . . yes C28 C33 1.517(7) . . yes C29 C30 1.468(10) . . yes C29 C31 1.54(1) . . yes C29 C32 1.49(1) . . yes C33 C35 1.509(7) . . yes C34 C35 1.402(7) . . yes C34 C39 1.399(7) . . yes C35 C36 1.387(7) . . yes C36 C37 1.386(7) . . yes C37 C38 1.380(7) . . yes C37 C40 1.528(7) . . yes C38 C39 1.388(6) . . yes C39 C47 1.503(7) . . yes C40 C41 1.54(1) . . yes C40 C42 1.40(2) . . yes C40 C43 1.55(1) . . yes C40 C44 1.60(2) . . yes C40 C45 1.43(1) . . yes C40 C46 1.61(1) . . yes C41 C42 1.12(2) . . yes C41 C46 1.78(2) . . yes C42 C43 1.57(2) . . yes C43 C44 1.55(2) . . yes C44 C45 1.37(2) . . yes C45 C46 1.22(2) . . yes C48 C49 1.516(6) . . yes C48 C52 1.532(6) . . yes C49 C50 1.548(7) . . yes C50 C51 1.532(8) . . yes C51 C52 1.525(7) . . yes C54 C55 1.502(8) . . yes C55 C56 1.383(7) . . yes C55 C60 1.384(9) . . yes C56 C57 1.391(9) . . yes C57 C58 1.363(10) . . yes C58 C59 1.384(8) . . yes C59 C60 1.372(9) . . yes C61 C62 1.507(7) . . yes C61 C65 1.514(6) . . yes C62 C63 1.542(7) . . yes C63 C64 1.522(8) . . yes C64 C65 1.521(7) . . yes C67 C68 1.494(8) . . yes C68 C69 1.391(7) . . yes C68 C73 1.373(8) . . yes C69 C70 1.378(9) . . yes C70 C71 1.385(9) . . yes C71 C72 1.370(8) . . yes C72 C73 1.394(9) . . yes C74 C75 1.489(8) . . yes C76 C77 1.42(1) . . yes C78 C79 1.45(2) . . yes C80 C81 1.34(3) . . yes C80 C83 1.32(4) . . yes C80 C84 1.34(5) . . yes C81 C84 1.79(5) . . yes O2 H114 0.877 . . no O4 H115 0.967 . . no O9 H116 1.105 . . no O10 H118 0.932 . . no O11 H117 1.023 . . no N1 H112 0.901 . . no N2 H113 0.898 . . no C3 H19 0.951 . . no C5 H20 0.947 . . no C8 H21 0.950 . . no C8 H22 0.950 . . no C8 H23 0.949 . . no C9 H24 0.948 . . no C9 H25 0.951 . . no C9 H26 0.954 . . no C10 H27 0.955 . . no C10 H28 0.949 . . no C10 H29 0.948 . . no C11 H30 0.951 . . no C11 H31 0.947 . . no C14 H32 0.946 . . no C16 H33 0.952 . . no C19 H34 0.950 . . no C19 H35 0.950 . . no C19 H36 0.953 . . no C20 H37 0.946 . . no C20 H38 0.951 . . no C20 H39 0.954 . . no C21 H40 0.946 . . no C21 H41 0.953 . . no C21 H42 0.950 . . no C22 H43 0.950 . . no C22 H44 0.952 . . no C25 H45 0.951 . . no C27 H46 0.950 . . no C30 H47 0.944 . . no C30 H48 0.960 . . no C30 H49 0.946 . . no C31 H50 0.949 . . no C31 H51 0.952 . . no C31 H52 0.947 . . no C32 H53 0.940 . . no C32 H54 0.950 . . no C32 H55 0.952 . . no C33 H56 0.950 . . no C33 H57 0.951 . . no C36 H58 0.951 . . no C38 H59 0.949 . . no C41 H1 0.919 . . no C41 H2 0.942 . . no C41 H3 1.000 . . no C42 H10 0.936 . . no C42 H11 1.022 . . no C42 H12 0.888 . . no C43 H4 0.834 . . no C43 H5 1.005 . . no C43 H6 1.046 . . no C44 H13 0.927 . . no C44 H14 0.974 . . no C44 H15 1.026 . . no C45 H7 0.883 . . no C45 H8 0.944 . . no C45 H9 0.998 . . no C46 H16 0.926 . . no C46 H17 0.942 . . no C46 H18 0.985 . . no C47 H60 0.950 . . no C47 H61 0.951 . . no C48 H62 0.947 . . no C49 H63 0.951 . . no C49 H64 0.948 . . no C50 H65 0.952 . . no C50 H66 0.949 . . no C51 H67 0.952 . . no C51 H68 0.950 . . no C52 H69 0.950 . . no C54 H70 0.952 . . no C54 H71 0.943 . . no C56 H72 0.949 . . no C57 H73 0.948 . . no C58 H74 0.947 . . no C59 H75 0.954 . . no C60 H76 0.950 . . no C61 H77 0.951 . . no C62 H78 0.950 . . no C62 H79 0.952 . . no C63 H80 0.950 . . no C63 H81 0.950 . . no C64 H82 0.947 . . no C64 H83 0.948 . . no C65 H84 0.952 . . no C67 H85 0.946 . . no C67 H86 0.953 . . no C69 H87 0.948 . . no C70 H88 0.953 . . no C71 H89 0.954 . . no C72 H90 0.950 . . no C73 H91 0.951 . . no C74 H92 0.948 . . no C74 H93 0.952 . . no C75 H94 0.954 . . no C75 H95 0.950 . . no C75 H96 0.948 . . no C76 H97 0.953 . . no C76 H98 0.944 . . no C77 H99 0.951 . . no C77 H100 0.954 . . no C77 H101 0.946 . . no C78 H102 0.953 . . no C78 H103 0.950 . . no C79 H104 0.946 . . no C79 H105 0.947 . . no C79 H106 0.959 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C48 115.1(2) . . . ? C23 O3 C61 115.0(3) . . . ? C53 O5 C54 116.1(4) . . . ? C66 O7 C67 116.2(4) . . . ? C80 O12 C84 61(2) . . . ? C81 O14 C84 81(3) . . . ? C52 N1 C53 123.3(4) . . . ? C65 N2 C66 123.8(4) . . . ? O1 C1 C2 118.9(3) . . . ? O1 C1 C6 120.2(4) . . . ? C2 C1 C6 120.6(3) . . . ? C1 C2 C3 119.0(4) . . . ? C1 C2 C47 122.5(3) . . . ? C3 C2 C47 118.4(4) . . . ? C2 C3 C4 122.2(4) . . . ? C3 C4 C5 117.1(4) . . . ? C3 C4 C7 122.9(4) . . . ? C5 C4 C7 119.9(4) . . . ? C4 C5 C6 122.7(4) . . . ? C1 C6 C5 118.1(4) . . . ? C1 C6 C11 122.4(3) . . . ? C5 C6 C11 119.2(4) . . . ? C4 C7 C8 108.8(4) . . . ? C4 C7 C9 109.8(4) . . . ? C4 C7 C10 111.4(4) . . . ? C8 C7 C9 109.8(4) . . . ? C8 C7 C10 108.5(4) . . . ? C9 C7 C10 108.5(4) . . . ? C6 C11 C13 111.1(3) . . . ? O2 C12 C13 117.5(4) . . . ? O2 C12 C17 121.6(4) . . . ? C13 C12 C17 120.9(4) . . . ? C11 C13 C12 121.6(3) . . . ? C11 C13 C14 120.1(4) . . . ? C12 C13 C14 118.3(4) . . . ? C13 C14 C15 123.2(4) . . . ? C14 C15 C16 116.6(4) . . . ? C14 C15 C18 120.0(4) . . . ? C16 C15 C18 123.4(4) . . . ? C15 C16 C17 122.7(4) . . . ? C12 C17 C16 118.1(4) . . . ? C12 C17 C22 121.7(3) . . . ? C16 C17 C22 120.2(4) . . . ? C15 C18 C19 112.5(4) . . . ? C15 C18 C20 109.2(4) . . . ? C15 C18 C21 109.4(4) . . . ? C19 C18 C20 109.4(4) . . . ? C19 C18 C21 108.0(4) . . . ? C20 C18 C21 108.3(5) . . . ? C17 C22 C24 111.8(4) . . . ? O3 C23 C24 118.8(4) . . . ? O3 C23 C28 120.1(4) . . . ? C24 C23 C28 121.0(4) . . . ? C22 C24 C23 122.2(4) . . . ? C22 C24 C25 119.3(4) . . . ? C23 C24 C25 118.2(4) . . . ? C24 C25 C26 123.1(4) . . . ? C25 C26 C27 115.9(4) . . . ? C25 C26 C29 122.7(4) . . . ? C27 C26 C29 121.4(5) . . . ? C26 C27 C28 123.5(5) . . . ? C23 C28 C27 117.9(4) . . . ? C23 C28 C33 123.7(4) . . . ? C27 C28 C33 118.4(4) . . . ? C26 C29 C30 108.7(5) . . . ? C26 C29 C31 110.7(5) . . . ? C26 C29 C32 112.1(6) . . . ? C30 C29 C31 108.0(7) . . . ? C30 C29 C32 112.3(8) . . . ? C31 C29 C32 104.9(6) . . . ? C28 C33 C35 112.8(4) . . . ? O4 C34 C35 117.0(4) . . . ? O4 C34 C39 121.9(4) . . . ? C35 C34 C39 121.0(4) . . . ? C33 C35 C34 121.5(4) . . . ? C33 C35 C36 120.6(4) . . . ? C34 C35 C36 117.9(4) . . . ? C35 C36 C37 123.1(5) . . . ? C36 C37 C38 116.8(4) . . . ? C36 C37 C40 121.8(5) . . . ? C38 C37 C40 121.5(5) . . . ? C37 C38 C39 123.5(5) . . . ? C34 C39 C38 117.6(4) . . . ? C34 C39 C47 121.2(4) . . . ? C38 C39 C47 121.1(4) . . . ? C37 C40 C41 112.5(6) . . . ? C37 C40 C42 116.0(8) . . . ? C37 C40 C43 107.0(6) . . . ? C37 C40 C44 112.0(7) . . . ? C37 C40 C45 110.2(7) . . . ? C37 C40 C46 104.9(7) . . . ? C41 C40 C43 107.4(8) . . . ? C41 C40 C45 109.1(7) . . . ? C42 C40 C44 112(1) . . . ? C42 C40 C46 110.4(9) . . . ? C43 C40 C45 110.5(8) . . . ? C44 C40 C46 99.2(8) . . . ? C2 C47 C39 113.3(3) . . . ? O1 C48 C49 112.1(4) . . . ? O1 C48 C52 107.7(3) . . . ? C49 C48 C52 102.1(3) . . . ? C48 C49 C50 104.5(4) . . . ? C49 C50 C51 105.5(4) . . . ? C50 C51 C52 106.1(4) . . . ? N1 C52 C48 112.8(3) . . . ? N1 C52 C51 115.6(4) . . . ? C48 C52 C51 104.1(4) . . . ? O5 C53 O6 124.4(5) . . . ? O5 C53 N1 109.5(4) . . . ? O6 C53 N1 126.1(5) . . . ? O5 C54 C55 108.7(4) . . . ? C54 C55 C56 122.0(5) . . . ? C54 C55 C60 120.1(4) . . . ? C56 C55 C60 117.8(5) . . . ? C55 C56 C57 120.4(6) . . . ? C56 C57 C58 120.1(5) . . . ? C57 C58 C59 120.6(6) . . . ? C58 C59 C60 118.5(6) . . . ? C55 C60 C59 122.4(5) . . . ? O3 C61 C62 112.4(4) . . . ? O3 C61 C65 106.8(3) . . . ? C62 C61 C65 103.2(4) . . . ? C61 C62 C63 105.4(4) . . . ? C62 C63 C64 105.6(5) . . . ? C63 C64 C65 105.8(4) . . . ? N2 C65 C61 113.0(4) . . . ? N2 C65 C64 116.1(4) . . . ? C61 C65 C64 103.5(4) . . . ? O7 C66 O8 123.6(5) . . . ? O7 C66 N2 109.8(4) . . . ? O8 C66 N2 126.6(5) . . . ? O7 C67 C68 111.7(4) . . . ? C67 C68 C69 120.4(5) . . . ? C67 C68 C73 120.8(4) . . . ? C69 C68 C73 118.9(5) . . . ? C68 C69 C70 121.5(5) . . . ? C69 C70 C71 118.9(5) . . . ? C70 C71 C72 120.3(6) . . . ? C71 C72 C73 120.4(6) . . . ? C68 C73 C72 120.0(5) . . . ? O9 C74 C75 108.6(4) . . . ? O10 C76 C77 117.8(9) . . . ? O11 C78 C79 111.3(9) . . . ? O12 C80 C81 114(1) . . . ? O12 C80 C83 125(2) . . . ? O12 C80 C84 59(2) . . . ? C81 C80 C83 108(2) . . . ? C81 C80 C84 83(2) . . . ? C83 C80 C84 157(2) . . . ? O13 C81 O14 105(1) . . . ? O13 C81 C80 109(1) . . . ? O13 C81 C84 110(1) . . . ? O14 C81 C80 100(2) . . . ? O14 C81 C84 53(2) . . . ? C80 C81 C84 48(1) . . . ? O12 C84 O14 126(3) . . . ? O12 C84 C80 58(2) . . . ? O12 C84 C81 90(2) . . . ? O14 C84 C80 92(3) . . . ? O14 C84 C81 45(2) . . . ? C80 C84 C81 48(1) . . . ? C12 O2 H114 108.105 . . . no C34 O4 H115 107.269 . . . no C74 O9 H116 120.919 . . . no C76 O10 H118 131.055 . . . no C78 O11 H117 118.441 . . . no C52 N1 H112 118.371 . . . no C53 N1 H112 118.295 . . . no C65 N2 H113 118.062 . . . no C66 N2 H113 118.162 . . . no C2 C3 H19 118.901 . . . no C4 C3 H19 118.938 . . . no C4 C5 H20 118.551 . . . no C6 C5 H20 118.701 . . . no C7 C8 H21 109.372 . . . no C7 C8 H22 109.378 . . . no C7 C8 H23 109.415 . . . no H21 C8 H22 109.524 . . . no H21 C8 H23 109.558 . . . no H22 C8 H23 109.581 . . . no C7 C9 H24 109.798 . . . no C7 C9 H25 109.598 . . . no C7 C9 H26 109.437 . . . no H24 C9 H25 109.599 . . . no H24 C9 H26 109.326 . . . no H25 C9 H26 109.066 . . . no C7 C10 H27 109.317 . . . no C7 C10 H28 109.648 . . . no C7 C10 H29 109.703 . . . no H27 C10 H28 109.173 . . . no H27 C10 H29 109.236 . . . no H28 C10 H29 109.748 . . . no C6 C11 H30 109.072 . . . no C6 C11 H31 109.172 . . . no C13 C11 H30 108.891 . . . no C13 C11 H31 108.982 . . . no H30 C11 H31 109.634 . . . no C13 C14 H32 118.421 . . . no C15 C14 H32 118.374 . . . no C15 C16 H33 118.742 . . . no C17 C16 H33 118.532 . . . no C18 C19 H34 109.712 . . . no C18 C19 H35 109.653 . . . no C18 C19 H36 109.539 . . . no H34 C19 H35 109.460 . . . no H34 C19 H36 109.242 . . . no H35 C19 H36 109.220 . . . no C18 C20 H37 109.683 . . . no C18 C20 H38 109.512 . . . no C18 C20 H39 109.330 . . . no H37 C20 H38 109.749 . . . no H37 C20 H39 109.504 . . . no H38 C20 H39 109.048 . . . no C18 C21 H40 109.546 . . . no C18 C21 H41 109.229 . . . no C18 C21 H42 109.432 . . . no H40 C21 H41 109.595 . . . no H40 C21 H42 109.810 . . . no H41 C21 H42 109.215 . . . no C17 C22 H43 109.135 . . . no C17 C22 H44 109.059 . . . no C24 C22 H43 108.856 . . . no C24 C22 H44 108.723 . . . no H43 C22 H44 109.285 . . . no C24 C25 H45 118.417 . . . no C26 C25 H45 118.474 . . . no C26 C27 H46 118.275 . . . no C28 C27 H46 118.237 . . . no C29 C30 H47 109.773 . . . no C29 C30 H48 108.843 . . . no C29 C30 H49 109.758 . . . no H47 C30 H48 109.130 . . . no H47 C30 H49 110.334 . . . no H48 C30 H49 108.975 . . . no C29 C31 H50 109.242 . . . no C29 C31 H51 109.255 . . . no C29 C31 H52 109.522 . . . no H50 C31 H51 109.375 . . . no H50 C31 H52 109.827 . . . no H51 C31 H52 109.604 . . . no C29 C32 H53 109.508 . . . no C29 C32 H54 108.854 . . . no C29 C32 H55 108.574 . . . no H53 C32 H54 110.338 . . . no H53 C32 H55 110.195 . . . no H54 C32 H55 109.336 . . . no C28 C33 H56 108.531 . . . no C28 C33 H57 108.562 . . . no C35 C33 H56 108.855 . . . no C35 C33 H57 108.745 . . . no H56 C33 H57 109.301 . . . no C35 C36 H58 118.370 . . . no C37 C36 H58 118.540 . . . no C37 C38 H59 118.210 . . . no C39 C38 H59 118.265 . . . no C40 C41 H1 111.857 . . . no C40 C41 H2 110.461 . . . no C40 C41 H3 107.396 . . . no H1 C41 H2 112.970 . . . no H1 C41 H3 107.810 . . . no H2 C41 H3 105.981 . . . no C40 C42 H10 110.389 . . . no C40 C42 H11 103.981 . . . no C40 C42 H12 111.770 . . . no H10 C42 H11 104.732 . . . no H10 C42 H12 116.527 . . . no H11 C42 H12 108.413 . . . no C40 C43 H4 119.485 . . . no C40 C43 H5 107.555 . . . no C40 C43 H6 103.419 . . . no H4 C43 H5 114.738 . . . no H4 C43 H6 110.718 . . . no H5 C43 H6 98.296 . . . no C40 C44 H13 116.175 . . . no C40 C44 H14 113.974 . . . no C40 C44 H15 109.128 . . . no H13 C44 H14 109.393 . . . no H13 C44 H15 105.087 . . . no H14 C44 H15 101.707 . . . no C40 C45 H7 109.767 . . . no C40 C45 H8 108.225 . . . no C40 C45 H9 104.970 . . . no H7 C45 H8 116.180 . . . no H7 C45 H9 111.042 . . . no H8 C45 H9 106.005 . . . no C40 C46 H16 109.590 . . . no C40 C46 H17 110.305 . . . no C40 C46 H18 108.766 . . . no H16 C46 H17 112.341 . . . no H16 C46 H18 108.501 . . . no H17 C46 H18 107.235 . . . no C2 C47 H60 108.708 . . . no C2 C47 H61 108.631 . . . no C39 C47 H60 108.329 . . . no C39 C47 H61 108.398 . . . no H60 C47 H61 109.411 . . . no O1 C48 H62 111.527 . . . no C49 C48 H62 111.415 . . . no C52 C48 H62 111.558 . . . no C48 C49 H63 110.821 . . . no C48 C49 H64 110.902 . . . no C50 C49 H63 110.490 . . . no C50 C49 H64 110.524 . . . no H63 C49 H64 109.535 . . . no C49 C50 H65 110.381 . . . no C49 C50 H66 110.523 . . . no C51 C50 H65 110.451 . . . no C51 C50 H66 110.559 . . . no H65 C50 H66 109.353 . . . no C50 C51 H67 110.180 . . . no C50 C51 H68 110.199 . . . no C52 C51 H67 110.448 . . . no C52 C51 H68 110.630 . . . no H67 C51 H68 109.286 . . . no N1 C52 H69 108.060 . . . no C48 C52 H69 108.186 . . . no C51 C52 H69 107.851 . . . no O5 C54 H70 109.466 . . . no O5 C54 H71 109.847 . . . no C55 C54 H70 109.261 . . . no C55 C54 H71 109.695 . . . no H70 C54 H71 109.898 . . . no C55 C56 H72 119.541 . . . no C57 C56 H72 120.018 . . . no C56 C57 H73 119.865 . . . no C58 C57 H73 120.008 . . . no C57 C58 H74 119.884 . . . no C59 C58 H74 119.545 . . . no C58 C59 H75 121.014 . . . no C60 C59 H75 120.441 . . . no C55 C60 H76 118.771 . . . no C59 C60 H76 118.821 . . . no O3 C61 H77 111.527 . . . no C62 C61 H77 111.259 . . . no C65 C61 H77 111.350 . . . no C61 C62 H78 110.559 . . . no C61 C62 H79 110.509 . . . no C63 C62 H78 110.619 . . . no C63 C62 H79 110.425 . . . no H78 C62 H79 109.273 . . . no C62 C63 H80 110.326 . . . no C62 C63 H81 110.477 . . . no C64 C63 H80 110.428 . . . no C64 C63 H81 110.493 . . . no H80 C63 H81 109.427 . . . no C63 C64 H82 110.072 . . . no C63 C64 H83 110.004 . . . no C65 C64 H82 110.508 . . . no C65 C64 H83 110.518 . . . no H82 C64 H83 109.840 . . . no N2 C65 H84 107.947 . . . no C61 C65 H84 107.840 . . . no C64 C65 H84 108.058 . . . no O7 C67 H85 109.036 . . . no O7 C67 H86 108.822 . . . no C68 C67 H85 108.975 . . . no C68 C67 H86 108.698 . . . no H85 C67 H86 109.554 . . . no C68 C69 H87 119.552 . . . no C70 C69 H87 118.962 . . . no C69 C70 H88 120.739 . . . no C71 C70 H88 120.344 . . . no C70 C71 H89 120.053 . . . no C72 C71 H89 119.647 . . . no C71 C72 H90 119.776 . . . no C73 C72 H90 119.856 . . . no C68 C73 H91 120.281 . . . no C72 C73 H91 119.679 . . . no O9 C74 H92 109.530 . . . no O9 C74 H93 109.799 . . . no C75 C74 H92 109.773 . . . no C75 C74 H93 109.653 . . . no H92 C74 H93 109.454 . . . no C74 C75 H94 109.428 . . . no C74 C75 H95 109.498 . . . no C74 C75 H96 109.664 . . . no H94 C75 H95 109.211 . . . no H94 C75 H96 109.334 . . . no H95 C75 H96 109.690 . . . no O10 C76 H97 106.129 . . . no O10 C76 H98 107.370 . . . no C77 C76 H97 107.625 . . . no C77 C76 H98 108.105 . . . no H97 C76 H98 109.698 . . . no C76 C77 H99 109.368 . . . no C76 C77 H100 109.633 . . . no C76 C77 H101 109.512 . . . no H99 C77 H100 109.036 . . . no H99 C77 H101 109.795 . . . no H100 C77 H101 109.482 . . . no O11 C78 H102 109.095 . . . no O11 C78 H103 109.388 . . . no C79 C78 H102 108.825 . . . no C79 C78 H103 109.002 . . . no H102 C78 H103 109.223 . . . no C78 C79 H104 109.716 . . . no C78 C79 H105 109.805 . . . no C78 C79 H106 109.191 . . . no H104 C79 H105 110.118 . . . no H104 C79 H106 109.033 . . . no H105 C79 H106 108.956 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.7(4) 1_555 1_555 1_555 1_555 yes O1 C1 C2 C47 4.7(6) 1_555 1_555 1_555 1_555 yes O1 C1 C6 C5 178.9(4) 1_555 1_555 1_555 1_555 yes O1 C1 C6 C11 -8.1(6) 1_555 1_555 1_555 1_555 yes O1 C48 C49 C50 -75.6(4) 1_555 1_555 1_555 1_555 yes O1 C48 C52 N1 -48.9(5) 1_555 1_555 1_555 1_555 yes O1 C48 C52 C51 77.1(4) 1_555 1_555 1_555 1_555 yes O2 C12 C13 C11 1.0(6) 1_555 1_555 1_555 1_555 yes O2 C12 C13 C14 178.6(4) 1_555 1_555 1_555 1_555 yes O2 C12 C17 C16 -177.3(4) 1_555 1_555 1_555 1_555 yes O2 C12 C17 C22 1.0(7) 1_555 1_555 1_555 1_555 yes O3 C23 C24 C22 8.6(7) 1_555 1_555 1_555 1_555 yes O3 C23 C24 C25 -177.3(4) 1_555 1_555 1_555 1_555 yes O3 C23 C28 C27 177.6(4) 1_555 1_555 1_555 1_555 yes O3 C23 C28 C33 -6.2(7) 1_555 1_555 1_555 1_555 yes O3 C61 C62 C63 -80.0(4) 1_555 1_555 1_555 1_555 yes O3 C61 C65 N2 -48.7(5) 1_555 1_555 1_555 1_555 yes O3 C61 C65 C64 77.7(4) 1_555 1_555 1_555 1_555 yes O4 C34 C35 C33 -0.2(6) 1_555 1_555 1_555 1_555 yes O4 C34 C35 C36 179.0(4) 1_555 1_555 1_555 1_555 yes O4 C34 C39 C38 -179.5(3) 1_555 1_555 1_555 1_555 yes O4 C34 C39 C47 -0.3(6) 1_555 1_555 1_555 1_555 yes O5 C53 N1 C52 177.7(4) 1_555 1_555 1_555 1_555 yes O5 C54 C55 C56 -31.9(8) 1_555 1_555 1_555 1_555 yes O5 C54 C55 C60 151.1(5) 1_555 1_555 1_555 1_555 yes O6 C53 O5 C54 0.9(8) 1_555 1_555 1_555 1_555 yes O6 C53 N1 C52 -0.9(8) 1_555 1_555 1_555 1_555 yes O7 C66 N2 C65 180.0(4) 1_555 1_555 1_555 1_555 yes O7 C67 C68 C69 48.0(7) 1_555 1_555 1_555 1_555 yes O7 C67 C68 C73 -132.7(5) 1_555 1_555 1_555 1_555 yes O8 C66 O7 C67 13.5(7) 1_555 1_555 1_555 1_555 yes O8 C66 N2 C65 0.1(8) 1_555 1_555 1_555 1_555 yes O12 C80 C81 O13 47(2) 1_555 1_555 1_555 1_555 yes O12 C80 C81 O14 -62(2) 1_555 1_555 1_555 1_555 yes O12 C80 C81 C84 -52(2) 1_555 1_555 1_555 1_555 yes O12 C80 C84 O14 132(3) 1_555 1_555 1_555 1_555 yes O12 C80 C84 C81 123(1) 1_555 1_555 1_555 1_555 yes O12 C84 O14 C81 42(4) 1_555 1_555 1_555 1_555 yes O12 C84 C80 C81 -123(1) 1_555 1_555 1_555 1_555 yes O12 C84 C80 C83 111(7) 1_555 1_555 1_555 1_555 yes O12 C84 C81 O13 -52(2) 1_555 1_555 1_555 1_555 yes O12 C84 C81 O14 -146(3) 1_555 1_555 1_555 1_555 yes O12 C84 C81 C80 45(1) 1_555 1_555 1_555 1_555 yes O13 C81 O14 C84 -104(2) 1_555 1_555 1_555 1_555 yes O13 C81 C80 C83 -98(2) 1_555 1_555 1_555 1_555 yes O13 C81 C80 C84 100(2) 1_555 1_555 1_555 1_555 yes O13 C81 C84 O14 94(2) 1_555 1_555 1_555 1_555 yes O13 C81 C84 C80 -97(2) 1_555 1_555 1_555 1_555 yes O14 C81 C80 C83 150(2) 1_555 1_555 1_555 1_555 yes O14 C81 C80 C84 -10(2) 1_555 1_555 1_555 1_555 yes O14 C81 C84 C80 167(3) 1_555 1_555 1_555 1_555 yes O14 C84 O12 C80 -67(4) 1_555 1_555 1_555 1_555 yes O14 C84 C80 C81 8(2) 1_555 1_555 1_555 1_555 yes O14 C84 C80 C83 -116(7) 1_555 1_555 1_555 1_555 yes O14 C84 C81 C80 -167(3) 1_555 1_555 1_555 1_555 yes N1 C52 C48 C49 -167.1(4) 1_555 1_555 1_555 1_555 yes N1 C52 C51 C50 151.2(4) 1_555 1_555 1_555 1_555 yes N1 C53 O5 C54 -177.7(4) 1_555 1_555 1_555 1_555 yes N2 C65 C61 C62 -167.3(4) 1_555 1_555 1_555 1_555 yes N2 C65 C64 C63 156.0(4) 1_555 1_555 1_555 1_555 yes N2 C66 O7 C67 -166.3(4) 1_555 1_555 1_555 1_555 yes C1 O1 C48 C49 -90.1(4) 1_555 1_555 1_555 1_555 yes C1 O1 C48 C52 158.3(3) 1_555 1_555 1_555 1_555 yes C1 C2 C3 C4 -1.3(7) 1_555 1_555 1_555 1_555 yes C1 C2 C47 C39 98.6(5) 1_555 1_555 1_555 1_555 yes C1 C6 C5 C4 3.0(7) 1_555 1_555 1_555 1_555 yes C1 C6 C11 C13 -101.0(4) 1_555 1_555 1_555 1_555 yes C2 C1 O1 C48 105.1(4) 1_555 1_555 1_555 1_555 yes C2 C1 C6 C5 -6.3(6) 1_555 1_555 1_555 1_555 yes C2 C1 C6 C11 166.6(4) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C5 -2.0(7) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C7 179.6(4) 1_555 1_555 1_555 1_555 yes C2 C47 C39 C34 -76.3(5) 1_555 1_555 1_555 1_555 yes C2 C47 C39 C38 102.9(5) 1_555 1_555 1_555 1_555 yes C3 C2 C1 C6 5.5(7) 1_555 1_555 1_555 1_555 yes C3 C2 C47 C39 -77.1(5) 1_555 1_555 1_555 1_555 yes C3 C4 C5 C6 1.0(7) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C8 -113.9(5) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C9 125.9(5) 1_555 1_555 1_555 1_555 yes C3 C4 C7 C10 5.6(6) 1_555 1_555 1_555 1_555 yes C4 C3 C2 C47 174.6(4) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C11 -170.2(4) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C8 67.6(6) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C9 -52.6(6) 1_555 1_555 1_555 1_555 yes C5 C4 C7 C10 -172.8(4) 1_555 1_555 1_555 1_555 yes C5 C6 C11 C13 71.9(5) 1_555 1_555 1_555 1_555 yes C6 C1 O1 C48 -80.1(4) 1_555 1_555 1_555 1_555 yes C6 C1 C2 C47 -170.1(4) 1_555 1_555 1_555 1_555 yes C6 C5 C4 C7 179.6(4) 1_555 1_555 1_555 1_555 yes C6 C11 C13 C12 87.0(5) 1_555 1_555 1_555 1_555 yes C6 C11 C13 C14 -90.5(5) 1_555 1_555 1_555 1_555 yes C11 C13 C12 C17 179.8(4) 1_555 1_555 1_555 1_555 yes C11 C13 C14 C15 176.7(4) 1_555 1_555 1_555 1_555 yes C12 C13 C14 C15 -0.9(7) 1_555 1_555 1_555 1_555 yes C12 C17 C16 C15 -2.0(7) 1_555 1_555 1_555 1_555 yes C12 C17 C22 C24 -83.1(5) 1_555 1_555 1_555 1_555 yes C13 C12 C17 C16 4.1(7) 1_555 1_555 1_555 1_555 yes C13 C12 C17 C22 -177.7(4) 1_555 1_555 1_555 1_555 yes C13 C14 C15 C16 2.9(7) 1_555 1_555 1_555 1_555 yes C13 C14 C15 C18 -175.5(5) 1_555 1_555 1_555 1_555 yes C14 C13 C12 C17 -2.7(7) 1_555 1_555 1_555 1_555 yes C14 C15 C16 C17 -1.3(7) 1_555 1_555 1_555 1_555 yes C14 C15 C18 C19 175.7(5) 1_555 1_555 1_555 1_555 yes C14 C15 C18 C20 -62.6(6) 1_555 1_555 1_555 1_555 yes C14 C15 C18 C21 55.7(6) 1_555 1_555 1_555 1_555 yes C15 C16 C17 C22 179.7(4) 1_555 1_555 1_555 1_555 yes C16 C15 C18 C19 -2.6(7) 1_555 1_555 1_555 1_555 yes C16 C15 C18 C20 119.1(5) 1_555 1_555 1_555 1_555 yes C16 C15 C18 C21 -122.6(5) 1_555 1_555 1_555 1_555 yes C16 C17 C22 C24 95.1(5) 1_555 1_555 1_555 1_555 yes C17 C16 C15 C18 177.0(5) 1_555 1_555 1_555 1_555 yes C17 C22 C24 C23 94.8(5) 1_555 1_555 1_555 1_555 yes C17 C22 C24 C25 -79.2(5) 1_555 1_555 1_555 1_555 yes C22 C24 C23 C28 -167.5(4) 1_555 1_555 1_555 1_555 yes C22 C24 C25 C26 172.6(5) 1_555 1_555 1_555 1_555 yes C23 O3 C61 C62 -89.5(4) 1_555 1_555 1_555 1_555 yes C23 O3 C61 C65 158.1(4) 1_555 1_555 1_555 1_555 yes C23 C24 C25 C26 -1.7(7) 1_555 1_555 1_555 1_555 yes C23 C28 C27 C26 1.2(7) 1_555 1_555 1_555 1_555 yes C23 C28 C33 C35 -101.8(5) 1_555 1_555 1_555 1_555 yes C24 C23 O3 C61 105.8(5) 1_555 1_555 1_555 1_555 yes C24 C23 C28 C27 -6.4(7) 1_555 1_555 1_555 1_555 yes C24 C23 C28 C33 169.8(4) 1_555 1_555 1_555 1_555 yes C24 C25 C26 C27 -3.1(7) 1_555 1_555 1_555 1_555 yes C24 C25 C26 C29 176.9(5) 1_555 1_555 1_555 1_555 yes C25 C24 C23 C28 6.6(7) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C28 3.4(7) 1_555 1_555 1_555 1_555 yes C25 C26 C29 C30 -94.3(7) 1_555 1_555 1_555 1_555 yes C25 C26 C29 C31 24.2(8) 1_555 1_555 1_555 1_555 yes C25 C26 C29 C32 140.9(8) 1_555 1_555 1_555 1_555 yes C26 C27 C28 C33 -175.2(4) 1_555 1_555 1_555 1_555 yes C27 C26 C29 C30 85.8(7) 1_555 1_555 1_555 1_555 yes C27 C26 C29 C31 -155.7(6) 1_555 1_555 1_555 1_555 yes C27 C26 C29 C32 -39.0(9) 1_555 1_555 1_555 1_555 yes C27 C28 C33 C35 74.4(5) 1_555 1_555 1_555 1_555 yes C28 C23 O3 C61 -78.1(5) 1_555 1_555 1_555 1_555 yes C28 C27 C26 C29 -176.7(5) 1_555 1_555 1_555 1_555 yes C28 C33 C35 C34 81.2(5) 1_555 1_555 1_555 1_555 yes C28 C33 C35 C36 -98.0(5) 1_555 1_555 1_555 1_555 yes C33 C35 C34 C39 177.0(4) 1_555 1_555 1_555 1_555 yes C33 C35 C36 C37 -178.8(4) 1_555 1_555 1_555 1_555 yes C34 C35 C36 C37 2.0(6) 1_555 1_555 1_555 1_555 yes C34 C39 C38 C37 -1.2(6) 1_555 1_555 1_555 1_555 yes C35 C34 C39 C38 3.5(6) 1_555 1_555 1_555 1_555 yes C35 C34 C39 C47 -177.4(3) 1_555 1_555 1_555 1_555 yes C35 C36 C37 C38 0.3(6) 1_555 1_555 1_555 1_555 yes C35 C36 C37 C40 -179.2(4) 1_555 1_555 1_555 1_555 yes C36 C35 C34 C39 -3.9(6) 1_555 1_555 1_555 1_555 yes C36 C37 C38 C39 -0.7(6) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C41 2.4(7) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C42 -46(1) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C43 -115.4(7) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C44 -177.9(7) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C45 124.4(7) 1_555 1_555 1_555 1_555 yes C36 C37 C40 C46 75.5(7) 1_555 1_555 1_555 1_555 yes C37 C38 C39 C47 179.7(4) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C41 -177.1(6) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C42 134.0(9) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C43 65.2(7) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C44 2.6(8) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C45 -55.0(8) 1_555 1_555 1_555 1_555 yes C38 C37 C40 C46 -104.0(7) 1_555 1_555 1_555 1_555 yes C39 C38 C37 C40 178.8(4) 1_555 1_555 1_555 1_555 yes C48 C49 C50 C51 -23.0(4) 1_555 1_555 1_555 1_555 yes C48 C52 N1 C53 -125.2(5) 1_555 1_555 1_555 1_555 yes C48 C52 C51 C50 27.0(4) 1_555 1_555 1_555 1_555 yes C49 C48 C52 C51 -41.1(4) 1_555 1_555 1_555 1_555 yes C49 C50 C51 C52 -2.6(4) 1_555 1_555 1_555 1_555 yes C50 C49 C48 C52 39.4(4) 1_555 1_555 1_555 1_555 yes C51 C52 N1 C53 115.2(5) 1_555 1_555 1_555 1_555 yes C53 O5 C54 C55 164.1(5) 1_555 1_555 1_555 1_555 yes C54 C55 C56 C57 -175.2(6) 1_555 1_555 1_555 1_555 yes C54 C55 C60 C59 173.2(6) 1_555 1_555 1_555 1_555 yes C55 C56 C57 C58 0(1) 1_555 1_555 1_555 1_555 yes C55 C60 C59 C58 3(1) 1_555 1_555 1_555 1_555 yes C56 C55 C60 C59 -3.9(10) 1_555 1_555 1_555 1_555 yes C56 C57 C58 C59 -1(1) 1_555 1_555 1_555 1_555 yes C57 C56 C55 C60 1.9(9) 1_555 1_555 1_555 1_555 yes C57 C58 C59 C60 0(1) 1_555 1_555 1_555 1_555 yes C61 C62 C63 C64 -15.1(5) 1_555 1_555 1_555 1_555 yes C61 C65 N2 C66 -129.9(5) 1_555 1_555 1_555 1_555 yes C61 C65 C64 C63 31.6(5) 1_555 1_555 1_555 1_555 yes C62 C61 C65 C64 -40.9(4) 1_555 1_555 1_555 1_555 yes C62 C63 C64 C65 -10.2(5) 1_555 1_555 1_555 1_555 yes C63 C62 C61 C65 34.6(4) 1_555 1_555 1_555 1_555 yes C64 C65 N2 C66 110.7(5) 1_555 1_555 1_555 1_555 yes C66 O7 C67 C68 81.6(5) 1_555 1_555 1_555 1_555 yes C67 C68 C69 C70 178.1(6) 1_555 1_555 1_555 1_555 yes C67 C68 C73 C72 -178.2(6) 1_555 1_555 1_555 1_555 yes C68 C69 C70 C71 1(1) 1_555 1_555 1_555 1_555 yes C68 C73 C72 C71 -1(1) 1_555 1_555 1_555 1_555 yes C69 C68 C73 C72 1.1(9) 1_555 1_555 1_555 1_555 yes C69 C70 C71 C72 -1(1) 1_555 1_555 1_555 1_555 yes C70 C69 C68 C73 -1.3(9) 1_555 1_555 1_555 1_555 yes C70 C71 C72 C73 1(1) 1_555 1_555 1_555 1_555 yes C80 O12 C84 C81 -38(1) 1_555 1_555 1_555 1_555 yes C80 C81 O14 C84 9(2) 1_555 1_555 1_555 1_555 yes C80 C84 O14 C81 -9(2) 1_555 1_555 1_555 1_555 yes C81 C80 O12 C84 66(2) 1_555 1_555 1_555 1_555 yes C81 C84 C80 C83 -125(7) 1_555 1_555 1_555 1_555 yes C83 C80 O12 C84 -154(3) 1_555 1_555 1_555 1_555 yes C83 C80 C81 C84 160(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O6 O13 2.53(2) . . ? O6 O12 2.93(1) . . ? O6 C84 3.24(4) . . ? O6 O14 3.24(3) . . ? O6 C81 3.40(1) . . ? O8 O11 2.772(5) . . ? O8 C5 3.388(6) . 2_545 ? O8 C8 3.553(7) . 2_545 ? O8 C78 3.566(8) . . ? O9 O10 2.823(6) . . ? O9 C16 3.388(7) . . ? O9 C15 3.417(7) . . ? O9 C21 3.597(8) . . ? O10 C59 3.430(10) . 1_554 ? O10 C75 3.501(7) . . ? O11 C73 3.391(7) . . ? O11 C21 3.522(8) . 2_545 ? O12 C44 3.34(2) . 1_556 ? O12 C54 3.37(1) . . ? O13 C41 2.92(2) . 2_555 ? O13 C32 3.33(2) . 2_555 ? O13 C36 3.57(2) . 2_555 ? O14 C77 3.49(4) . 1_656 ? O14 C76 3.60(4) . 1_656 ? C32 C81 3.58(2) . 2_545 ? C41 C83 3.22(3) . 2_545 ? C41 C80 3.55(2) . 2_545 ? C44 C84 2.94(5) . 1_554 ? C56 C71 3.529(10) . 2_555 ? #------------------------------------------------------------------------------