# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author_name 'Filipe A. Almeida Paz' _publ_contact_author_address ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_email filipe.paz@ua.pt _publ_contact_author_fax '+351 234 370084' _publ_contact_author_phone '+351 234 370200' loop_ _publ_author_name _publ_author_footnote _publ_author_address J.A.Fernandes . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'F.Almeida Paz' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; S.S.Braga . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; P.Ribeiro-Claro . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; J.Rocha . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; # ======================================================================= _vrf_PLAT201_compound-1 ; RESPONSE: All non-hydrogen atoms of the guest molecules and the water molecules of crystallisation have been refined by assuming an isotropic displacement behaviour. ; _vrf_PLAT220_compound-1 ; RESPONSE: The crystal sructure is significantly affected by thermal disorder, in particular the guest molecules. Therefore, within the crystal contents, there is a wide dispersion of Ueq for C and O (and, consequently, H because all of these atoms have been refined by assuming a riding behaviour on their parent atoms). ; _vrf_PLAT222_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT220_compound-1 ; _vrf_PLAT241_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT220_compound-1 ; _vrf_PLAT242_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT220_compound-1 ; _vrf_PLAT306_compound-1 ; RESPONSE: As explained in the main text, all water molecules of crystallisation have been included in the structural model without the corresponsing hydrogen atoms, hence the alerts for isolated O atoms and hydrogen bonds without the involved H atom. ; _vrf_PLAT414_compound-1 ; RESPONSE: Due to the poor quality of the crystal data set, the location of the carbon and oxygen atoms of the main molecular units of the compound (i.e., cyclodextrins) are affected by a significant crystallographic error. See also our response to _vrf_PLAT340_compound-1. Thus, the geometrical placement of the attached hydrogen atoms (using appropriate HFIX instructions in SHELX) leads to short distances between C-H bonds, hence the alert. This structural limitation can not be overcome with the available data sets. ; _vrf_PLAT430_compound-1 ; RESPONSE: These short distances correspond to partially occupied oxygen atoms of water molecules of crystallisation. All these short contacts correspond to pairs of entities with total site occupancy of <= 1. ; _vrf_PLAT213_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT220_compound-1 ; _vrf_PLAT340_compound-1 ; RESPONSE: The crystals available for data collection were of poor quality and, therefore, the crystallographic data set is only of medium quality. As a consequence, the location of the heaviest atoms (e.g., C and O) reflects this higher uncertainty. ; _vrf_PLAT416_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT414_compound-1 ; _vrf_CHEMW03_compound-1 ; RESPONSE: As explained in the main text, the hydrogen atoms associated with the water molecules of crystallisation were not inlcuded in the structural model (either in calculated positions oir from preliminary locations visible from difference Fourier maps). However, the corresponding H atoms have been included in the empirical formula, hence the alert. ; _vrf_SHFSU01_compound-1 ; RESPONSE: Additional refinement cycles did not improve the overall SU. Indeed, because the guest molecules were allowed to refine and their location is significantly surrounded by a smeared out electron density, full convergence can not be achieved. ; _vrf_PLAT080_compound-1 ; RESPONSE: Please see our response to _vrf_SHFSU01_compound-1. ; _vrf_PLAT202_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT201_compound-1. ; _vrf_PLAT311_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT306_compound-1. ; _vrf_PLAT313_compound-1 ; RESPONSE: These two oxygen atoms were included in the structural model as a terminal disordered -OH group, hence the apparent presence of three covalent bonds. ; _vrf_PLAT360_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-1. ; _vrf_PLAT361_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-1. ; _vrf_PLAT366_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-1. ; _vrf_PLAT367_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-1. ; _vrf_PLAT369_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-1. ; _vrf_PLAT410_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT414_compound-1. ; _vrf_PLAT041_compound-1 ; RESPONSE: Please see our response to _vrf_CHEMW03_compound-1. ; _vrf_PLAT043_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-1. ; _vrf_PLAT044_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-1. ; _vrf_PLAT068_compound-1 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-1. ; # ======================================================================= data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 796034' #TrackingRef 'NJ-ART-10-2010-000796-Compound-1.cif' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '17 February 2011' # ======================================================================= #============================================================================== # GENERAL AND CHEMICAL DATA #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H206 K4 O103' _chemical_formula_weight 3357.17 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # CRYSTAL DATA #============================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 14.9804(15) _cell_length_b 15.6008(15) _cell_length_c 19.252(2) _cell_angle_alpha 84.728(3) _cell_angle_beta 75.560(3) _cell_angle_gamma 75.295(3) _cell_volume 4212.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4912 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 16.82 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1778 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9790 _exptl_absorpt_correction_T_max 0.9958 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1998) ; #============================================================================== # EXPERIMENTAL DATA #============================================================================== _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 X8 Kappa CCD APEX II' _diffrn_measurement_method '/w / /f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 62929 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.2166 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.35 _reflns_number_total 26365 _reflns_number_gt 10577 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT+ (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' #============================================================================== # REFINEMENT DATA #============================================================================== _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(18) _refine_ls_number_reflns 26365 _refine_ls_number_parameters 1652 _refine_ls_number_restraints 993 _refine_ls_R_factor_all 0.2978 _refine_ls_R_factor_gt 0.1384 _refine_ls_wR_factor_ref 0.3097 _refine_ls_wR_factor_gt 0.2808 _refine_ls_goodness_of_fit_ref 2.075 _refine_ls_restrained_S_all 2.091 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 #============================================================================== # 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1864(11) 1.0542(9) 0.3704(8) 0.058(4) Uani 1 1 d U . . H1 H -0.2559 1.0630 0.3743 0.069 Uiso 1 1 calc R . . O1 O -0.1512(8) 0.7172(6) 0.2328(6) 0.076(3) Uani 1 1 d U . . H1A H -0.0947 0.6949 0.2350 0.114 Uiso 1 1 calc R . . C2 C -0.1454(10) 1.0985(10) 0.3062(8) 0.057(4) Uani 1 1 d U . . H2 H -0.1771 1.1629 0.3122 0.069 Uiso 1 1 calc R . . O2 O -0.1354(7) 0.8964(7) 0.2292(6) 0.080(3) Uani 1 1 d U . . H2A H -0.1409 0.9494 0.2384 0.120 Uiso 1 1 calc R . . O3 O -0.1641(8) 1.0745(6) 0.2424(6) 0.083(4) Uani 1 1 d U . . H3 H -0.1286 1.0931 0.2064 0.124 Uiso 1 1 calc R . . C3 C -0.0417(11) 1.0916(10) 0.2978(8) 0.062(5) Uani 1 1 d U . . H3A H -0.0075 1.0277 0.2931 0.074 Uiso 1 1 calc R . . O4 O -0.0010(9) 1.1400(8) 0.2360(7) 0.109(4) Uani 1 1 d U . . H4 H -0.0006 1.1902 0.2482 0.163 Uiso 1 1 calc R . . C4 C -0.0289(11) 1.1238(10) 0.3629(8) 0.063(5) Uani 1 1 d U . . H4A H -0.0559 1.1892 0.3664 0.075 Uiso 1 1 calc R . . O5 O 0.1840(7) 1.1579(7) 0.2338(5) 0.077(3) Uani 1 1 d U . . H5 H 0.1606 1.2096 0.2202 0.115 Uiso 1 1 calc R . . C5 C -0.0705(10) 1.0744(10) 0.4335(8) 0.058(5) Uani 1 1 d U . . H5A H -0.0366 1.0103 0.4343 0.070 Uiso 1 1 calc R . . O6 O 0.3615(8) 1.0639(7) 0.2583(6) 0.079(3) Uani 1 1 d U . . H6 H 0.3995 1.0857 0.2724 0.118 Uiso 1 1 calc R . . C6 C -0.0707(12) 1.1213(10) 0.5011(9) 0.075(5) Uani 1 1 d U . . H6A H -0.1054 1.0941 0.5446 0.090 Uiso 1 1 calc R . . H6B H -0.0046 1.1141 0.5054 0.090 Uiso 1 1 calc R . . C7 C 0.1206(10) 1.1715(9) 0.3606(8) 0.045(4) Uani 1 1 d U . . H7 H 0.0758 1.2291 0.3527 0.053 Uiso 1 1 calc R . . O7 O 0.5226(8) 0.9748(8) 0.2906(6) 0.095(4) Uani 1 1 d U . . H7A H 0.4843 1.0248 0.2941 0.142 Uiso 1 1 calc R . . O8 O 0.5747(7) 0.7881(6) 0.3018(5) 0.064(3) Uani 1 1 d U . . H8 H 0.6230 0.7648 0.3177 0.096 Uiso 1 1 calc R . . C8 C 0.2043(10) 1.1603(9) 0.3005(8) 0.051(4) Uani 1 1 d U . . H8A H 0.2352 1.2103 0.2995 0.062 Uiso 1 1 calc R . . O9 O 0.6275(6) 0.6061(6) 0.3351(5) 0.059(3) Uani 1 1 d U . . H9 H 0.6755 0.6183 0.3430 0.088 Uiso 1 1 calc R . . C9 C 0.2705(10) 1.0773(9) 0.3127(8) 0.052(4) Uani 1 1 d U . . H9A H 0.2409 1.0271 0.3113 0.063 Uiso 1 1 calc R . . O10 O 0.5353(7) 0.4685(6) 0.3258(6) 0.072(3) Uani 1 1 d U . . H10 H 0.5069 0.4275 0.3377 0.109 Uiso 1 1 calc R . . C10 C 0.2955(10) 1.0746(8) 0.3876(7) 0.042(4) Uani 1 1 d U . . H10A H 0.3324 1.1200 0.3869 0.050 Uiso 1 1 calc R . . O11 O 0.4233(6) 0.3555(6) 0.3216(5) 0.061(3) Uani 1 1 d U . . H11 H 0.4131 0.3493 0.2816 0.092 Uiso 1 1 calc R . . C11 C 0.2061(9) 1.0961(7) 0.4445(7) 0.032(4) Uani 1 1 d U . . H11A H 0.1748 1.0453 0.4527 0.039 Uiso 1 1 calc R . . O12 O 0.2391(6) 0.3678(5) 0.3000(5) 0.045(3) Uani 1 1 d U . . H12 H 0.2787 0.3188 0.2918 0.068 Uiso 1 1 calc R . . C12 C 0.2277(10) 1.1155(9) 0.5132(8) 0.059(5) Uani 1 1 d U . . H12A H 0.1690 1.1214 0.5517 0.071 Uiso 1 1 calc R . . H12B H 0.2750 1.0636 0.5261 0.071 Uiso 1 1 calc R . . O13 O 0.0504(6) 0.3814(6) 0.2954(5) 0.050(3) Uani 1 1 d U . . H13 H 0.0396 0.3327 0.2892 0.076 Uiso 1 1 calc R . . C13 C 0.4386(10) 0.9806(9) 0.4136(8) 0.049(4) Uani 1 1 d U . . H13A H 0.4500 1.0412 0.4130 0.059 Uiso 1 1 calc R . . O14 O -0.0818(6) 0.5393(5) 0.2625(5) 0.052(3) Uani 1 1 d U . . H14 H -0.0756 0.5885 0.2431 0.078 Uiso 1 1 calc R . . C14 C 0.5126(10) 0.9307(10) 0.3581(8) 0.055(4) Uani 1 1 d U . . H14A H 0.5735 0.9253 0.3726 0.066 Uiso 1 1 calc R . . O15 O -0.1270(6) 0.6740(5) 0.3680(5) 0.049(3) Uani 1 1 d U . . C15 C 0.5025(10) 0.8407(9) 0.3571(7) 0.041(4) Uani 1 1 d U . . H15 H 0.4397 0.8448 0.3462 0.050 Uiso 1 1 calc R . . C16 C 0.5021(9) 0.7915(8) 0.4285(7) 0.039(4) Uani 1 1 d U . . H16 H 0.5663 0.7826 0.4385 0.047 Uiso 1 1 calc R . . O16 O -0.1406(6) 0.9605(6) 0.3640(6) 0.061(3) Uani 1 1 d U . . O17 O 0.0746(6) 1.1015(6) 0.3599(5) 0.056(3) Uani 1 1 d U . . C17 C 0.4271(10) 0.8473(9) 0.4899(8) 0.054(4) Uani 1 1 d U . . H17 H 0.3608 0.8497 0.4868 0.065 Uiso 1 1 calc R . . O18 O 0.3513(6) 0.9902(5) 0.4008(4) 0.034(2) Uani 1 1 d U . . C18 C 0.4437(8) 0.8128(8) 0.5633(7) 0.036(4) Uani 1 1 d U . . H18A H 0.3982 0.8527 0.6001 0.043 Uiso 1 1 calc R . . H18B H 0.4299 0.7535 0.5727 0.043 Uiso 1 1 calc R . . O19 O 0.4827(6) 0.7101(6) 0.4295(5) 0.045(3) Uani 1 1 d U . . C19 C 0.5372(9) 0.6322(8) 0.4572(7) 0.035(4) Uani 1 1 d U . . H19 H 0.5898 0.6493 0.4718 0.042 Uiso 1 1 calc R . . O20 O 0.3645(6) 0.4754(5) 0.4301(5) 0.041(2) Uani 1 1 d U . . C20 C 0.5822(10) 0.5716(10) 0.3932(8) 0.052(4) Uani 1 1 d U . . H20 H 0.6285 0.5199 0.4089 0.062 Uiso 1 1 calc R . . O21 O 0.0895(5) 0.4528(5) 0.4055(4) 0.035(2) Uani 1 1 d U . . C21 C 0.4985(9) 0.5343(8) 0.3767(7) 0.039(4) Uani 1 1 d U . . H21 H 0.4541 0.5844 0.3573 0.047 Uiso 1 1 calc R . . C22 C 0.4425(9) 0.4986(8) 0.4484(7) 0.039(4) Uani 1 1 d U . . H22 H 0.4841 0.4442 0.4655 0.047 Uiso 1 1 calc R . . O22 O -0.2528(7) 0.5663(7) 0.5231(6) 0.074(3) Uani 1 1 d U . . H22A H -0.2416 0.5334 0.4883 0.112 Uiso 1 1 calc R . . O23 O -0.3526(6) 0.9372(6) 0.4930(5) 0.053(3) Uani 1 1 d U . . H23 H -0.3919 0.9054 0.5057 0.080 Uiso 1 1 calc R . . C23 C 0.4113(9) 0.5648(8) 0.5033(8) 0.043(4) Uani 1 1 d U . . H23A H 0.3647 0.6162 0.4875 0.051 Uiso 1 1 calc R . . C24 C 0.3638(10) 0.5323(9) 0.5785(8) 0.053(4) Uani 1 1 d U . . H24A H 0.3430 0.5818 0.6121 0.064 Uiso 1 1 calc R . . H24B H 0.3069 0.5127 0.5756 0.064 Uiso 1 1 calc R . . O24 O -0.1125(9) 1.2078(9) 0.4962(7) 0.118(5) Uani 1 1 d U . . H24 H -0.1036 1.2246 0.4528 0.177 Uiso 1 1 calc R . . O25 O 0.2616(5) 1.1899(5) 0.5122(4) 0.037(2) Uani 1 1 d U . . H25 H 0.2343 1.2175 0.5501 0.055 Uiso 1 1 calc R . . C25 C 0.3618(10) 0.3876(9) 0.4443(8) 0.054(4) Uani 1 1 d U . . H25A H 0.4225 0.3506 0.4545 0.065 Uiso 1 1 calc R . . O26 O 0.5335(6) 0.8063(5) 0.5710(5) 0.043(3) Uani 1 1 d U . . H26 H 0.5657 0.7539 0.5641 0.065 Uiso 1 1 calc R . . C26 C 0.3396(8) 0.3558(8) 0.3762(7) 0.035(4) Uani 1 1 d U . . H26A H 0.3356 0.2926 0.3861 0.042 Uiso 1 1 calc R . . O27 O 0.4265(7) 0.4624(6) 0.6043(5) 0.059(3) Uani 1 1 d U . . H27 H 0.4594 0.4826 0.6253 0.088 Uiso 1 1 calc R . . C27 C 0.2506(9) 0.4045(8) 0.3603(7) 0.036(4) Uani 1 1 d U . . H27A H 0.2511 0.4684 0.3502 0.043 Uiso 1 1 calc R . . C28 C 0.1724(9) 0.3958(9) 0.4216(7) 0.040(4) Uani 1 1 d U . . H28 H 0.1661 0.3331 0.4284 0.048 Uiso 1 1 calc R . . O28 O 0.1070(6) 0.3271(6) 0.5640(5) 0.055(3) Uani 1 1 d U . . H28A H 0.0816 0.3146 0.5331 0.082 Uiso 1 1 calc R . . O29 O -0.0651(6) 0.4669(5) 0.4705(5) 0.042(2) Uani 1 1 d U . . C29 C 0.1842(8) 0.4289(9) 0.4906(7) 0.038(4) Uani 1 1 d U . . H29 H 0.1819 0.4937 0.4843 0.046 Uiso 1 1 calc R . . O30 O -0.2609(6) 0.7827(5) 0.4162(5) 0.036(2) Uani 1 1 d U . . C30 C 0.1149(10) 0.4150(9) 0.5530(8) 0.056(4) Uani 1 1 d U . . H30A H 0.1311 0.4332 0.5953 0.067 Uiso 1 1 calc R . . H30B H 0.0525 0.4535 0.5492 0.067 Uiso 1 1 calc R . . O31 O -0.1722(7) 1.0857(6) 0.4345(6) 0.075(3) Uani 1 1 d U . . C31 C 0.0106(9) 0.4191(8) 0.4171(7) 0.038(4) Uani 1 1 d U . . H31 H 0.0266 0.3550 0.4320 0.046 Uiso 1 1 calc R . . O32 O 0.1431(6) 1.1741(5) 0.4253(5) 0.040(2) Uani 1 1 d U . . C32 C -0.0275(9) 0.4302(7) 0.3479(6) 0.030(3) Uani 1 1 d U . . H32 H -0.0849 0.4058 0.3554 0.035 Uiso 1 1 calc R . . O33 O 0.4441(6) 0.9377(5) 0.4868(5) 0.043(3) Uani 1 1 d U . . C33 C -0.0485(10) 0.5266(9) 0.3253(8) 0.050(4) Uani 1 1 d U . . H33 H 0.0109 0.5481 0.3164 0.060 Uiso 1 1 calc R . . O34 O 0.4883(5) 0.5970(5) 0.5144(5) 0.035(2) Uani 1 1 d U . . C34 C -0.1232(10) 0.5785(8) 0.3870(7) 0.044(4) Uani 1 1 d U . . H34 H -0.1865 0.5651 0.3931 0.052 Uiso 1 1 calc R . . O35 O 0.2786(6) 0.3807(5) 0.5034(5) 0.047(3) Uani 1 1 d U . . C35 C -0.0912(8) 0.5644(8) 0.4563(6) 0.027(3) Uani 1 1 d U . . H35 H -0.0344 0.5891 0.4510 0.033 Uiso 1 1 calc R . . C36 C -0.1649(9) 0.6013(8) 0.5208(7) 0.042(4) Uani 1 1 d U . . H36A H -0.1810 0.6669 0.5175 0.051 Uiso 1 1 calc R . . H36B H -0.1414 0.5821 0.5648 0.051 Uiso 1 1 calc R . . O36 O 0.820(2) 0.3925(18) 0.7240(16) 0.132(11) Uani 0.50 1 d PU A 1 H36 H 0.8442 0.4082 0.6820 0.198 Uiso 0.50 1 calc PR A 1 O36' O 0.7175(12) 0.3829(12) 0.6780(10) 0.054(5) Uani 0.50 1 d PU A 2 H36' H 0.6607 0.3986 0.6748 0.081 Uiso 0.50 1 calc PR A 2 C55 C 0.7283(13) 0.4259(12) 0.7386(10) 0.084(6) Uani 1 1 d U . . H55A H 0.7034 0.4056 0.7016 0.101 Uiso 0.50 1 calc PR A 1 H55B H 0.7180 0.4911 0.7322 0.101 Uiso 0.50 1 calc PR A 1 H55C H 0.7956 0.4071 0.7413 0.101 Uiso 0.50 1 calc PR A 2 H55D H 0.7136 0.4908 0.7289 0.101 Uiso 0.50 1 calc PR A 2 C37 C -0.2144(8) 0.7282(8) 0.3578(7) 0.029(3) Uani 1 1 d U . . H37 H -0.2559 0.6890 0.3531 0.035 Uiso 1 1 calc R . . O37 O 0.5568(7) 0.1673(7) 0.7513(6) 0.074(3) Uani 1 1 d U . . H37A H 0.5828 0.1558 0.7861 0.111 Uiso 1 1 calc R . . O38 O 0.1945(7) 0.2977(6) 0.7221(5) 0.057(3) Uani 1 1 d U . . H38 H 0.2388 0.2580 0.7000 0.085 Uiso 1 1 calc R . . C38 C -0.1973(9) 0.7824(9) 0.2902(7) 0.044(4) Uani 1 1 d U . . H38A H -0.2599 0.8166 0.2815 0.052 Uiso 1 1 calc R . . O39 O 0.0165(6) 0.6328(6) 0.6483(5) 0.060(3) Uani 1 1 d U . . H39 H 0.0031 0.6716 0.6169 0.091 Uiso 1 1 calc R . . C39 C -0.1436(9) 0.8427(8) 0.2960(7) 0.038(4) Uani 1 1 d U . . H39A H -0.0789 0.8091 0.3006 0.045 Uiso 1 1 calc R . . O40 O 0.0749(6) 0.9964(6) 0.6244(5) 0.056(3) Uani 1 1 d U . . H40 H 0.0241 0.9860 0.6495 0.085 Uiso 1 1 calc R . . C40 C -0.1889(9) 0.8993(8) 0.3580(7) 0.041(4) Uani 1 1 d U . . H40A H -0.2527 0.9328 0.3511 0.050 Uiso 1 1 calc R . . O41 O 0.4737(6) 1.0857(6) 0.6572(5) 0.055(3) Uani 1 1 d U . . H41 H 0.5264 1.0848 0.6655 0.082 Uiso 1 1 calc R . . C41 C -0.2058(11) 0.8412(9) 0.4247(8) 0.060(5) Uani 1 1 d U . . H41A H -0.1431 0.8051 0.4317 0.072 Uiso 1 1 calc R . . O42 O 0.7783(6) 0.7942(6) 0.7191(5) 0.055(3) Uani 1 1 d U . . H42 H 0.8193 0.7961 0.6806 0.083 Uiso 1 1 calc R . . C42 C -0.2590(11) 0.8839(11) 0.4916(9) 0.076(5) Uani 1 1 d U . . H42A H -0.2641 0.8371 0.5298 0.092 Uiso 1 1 calc R . . H42B H -0.2216 0.9218 0.5040 0.092 Uiso 1 1 calc R . . O43 O 0.7511(6) 0.6339(6) 0.8018(5) 0.045(3) Uani 1 1 d U . . C43 C 0.4611(10) 0.9973(8) 0.6620(7) 0.042(4) Uani 1 1 d U . . H43A H 0.5130 0.9609 0.6262 0.050 Uiso 1 1 calc R . . H43B H 0.4005 0.9986 0.6496 0.050 Uiso 1 1 calc R . . C44 C 0.4603(9) 0.9560(8) 0.7317(7) 0.033(4) Uani 1 1 d U . . H44 H 0.4527 0.8940 0.7326 0.040 Uiso 1 1 calc R . . O44 O 0.6822(6) 0.3090(6) 0.8163(5) 0.055(3) Uani 1 1 d U . . O45 O 0.3648(6) 0.2355(5) 0.8211(5) 0.047(3) Uani 1 1 d U A . C45 C 0.3813(9) 1.0109(10) 0.7886(7) 0.048(4) Uani 1 1 d U . . H45 H 0.3763 1.0761 0.7813 0.057 Uiso 1 1 calc R . . C46 C 0.3943(10) 0.9743(10) 0.8674(8) 0.054(4) Uani 1 1 d U . . H46 H 0.3910 0.9108 0.8754 0.065 Uiso 1 1 calc R . . O46 O 0.0749(7) 0.4626(6) 0.7731(5) 0.053(3) Uani 1 1 d U . . O47 O 0.0222(6) 0.7893(5) 0.7104(5) 0.044(3) Uani 1 1 d U . . C47 C 0.4931(10) 0.9856(11) 0.8684(9) 0.069(5) Uani 1 1 d U . . H47 H 0.4976 1.0482 0.8557 0.082 Uiso 1 1 calc R . . O48 O 0.2050(6) 1.0289(5) 0.6995(5) 0.045(3) Uani 1 1 d U . . C48 C 0.5671(11) 0.9207(10) 0.8126(9) 0.063(5) Uani 1 1 d U . . H48 H 0.6323 0.9230 0.8152 0.076 Uiso 1 1 calc R . . O49 O 0.5523(6) 0.9561(6) 0.7429(5) 0.044(3) Uani 1 1 d U . . C49 C 0.7151(11) 0.7403(10) 0.7099(8) 0.061(5) Uani 1 1 d U . . H49A H 0.7504 0.6925 0.6760 0.073 Uiso 1 1 calc R . . H49B H 0.6621 0.7776 0.6906 0.073 Uiso 1 1 calc R . . O50 O 0.5571(6) 0.8343(6) 0.8296(5) 0.059(3) Uani 1 1 d U . . C50 C 0.6768(9) 0.7006(9) 0.7834(7) 0.041(4) Uani 1 1 d U . . H50 H 0.6252 0.6725 0.7797 0.049 Uiso 1 1 calc R . . O51 O 0.6602(6) 0.5386(6) 0.8670(5) 0.044(3) Uani 1 1 d U A . C51 C 0.6343(9) 0.7727(9) 0.8438(8) 0.046(4) Uani 1 1 d U . . H51 H 0.6843 0.8029 0.8475 0.056 Uiso 1 1 calc R . . O52 O 0.5345(7) 0.3215(6) 0.8898(5) 0.062(3) Uani 1 1 d U . . C52 C 0.6026(9) 0.7259(9) 0.9136(7) 0.042(4) Uani 1 1 d U . . H52 H 0.5481 0.7008 0.9117 0.051 Uiso 1 1 calc R . . O53 O 0.2428(6) 0.3492(6) 0.8798(5) 0.051(3) Uani 1 1 d U A . C53 C 0.6826(12) 0.6533(10) 0.9292(8) 0.064(5) Uani 1 1 d U . . H53 H 0.7341 0.6817 0.9324 0.076 Uiso 1 1 calc R . . O54 O 0.0406(6) 0.5942(6) 0.8290(5) 0.052(3) Uani 1 1 d U . . C54 C 0.7223(10) 0.5913(9) 0.8668(8) 0.050(4) Uani 1 1 d U . . H54 H 0.7810 0.5501 0.8769 0.060 Uiso 1 1 calc R . . O55 O 0.0614(6) 0.8718(5) 0.7903(5) 0.044(2) Uani 1 1 d U . . O56 O 0.2947(6) 0.9867(5) 0.7877(5) 0.045(3) Uani 1 1 d U . . C56 C 0.6702(11) 0.4081(10) 0.8073(8) 0.061(4) Uani 1 1 d U A . H56 H 0.6024 0.4363 0.8073 0.073 Uiso 1 1 calc R . . O57 O 0.5728(7) 0.7916(6) 0.9647(6) 0.077(3) Uani 1 1 d U . . H57 H 0.5397 0.8374 0.9488 0.116 Uiso 1 1 calc R . . C57 C 0.6947(11) 0.4448(10) 0.8659(8) 0.064(5) Uani 1 1 d U . . H57A H 0.7649 0.4279 0.8614 0.077 Uiso 1 1 calc R A . O58 O 0.6584(7) 0.6076(6) 0.9951(5) 0.067(3) Uani 1 1 d U . . H58 H 0.6174 0.5802 0.9933 0.100 Uiso 1 1 calc R . . C58 C 0.6382(10) 0.4089(9) 0.9438(7) 0.043(4) Uani 1 1 d U A . H58A H 0.5683 0.4361 0.9558 0.052 Uiso 1 1 calc R . . O59 O 0.6868(8) 0.4309(7) 0.9931(6) 0.084(3) Uani 1 1 d U . . H59 H 0.6509 0.4729 1.0184 0.126 Uiso 1 1 calc R A . C59 C 0.6607(12) 0.3161(10) 0.9393(9) 0.072(5) Uani 1 1 d U . . H59A H 0.7308 0.2925 0.9325 0.086 Uiso 1 1 calc R A . O60 O 0.6124(8) 0.2808(7) 1.0067(6) 0.087(4) Uani 1 1 d U A . H60 H 0.5557 0.2844 1.0060 0.130 Uiso 1 1 calc R . . C60 C 0.6286(10) 0.2871(9) 0.8779(8) 0.052(4) Uani 1 1 d U A . H60A H 0.6398 0.2210 0.8811 0.062 Uiso 1 1 calc R . . O61 O 0.4284(8) 0.2544(7) 1.0120(5) 0.081(3) Uani 1 1 d U A . H61 H 0.4810 0.2179 0.9999 0.121 Uiso 1 1 calc R . . C61 C 0.5161(9) 0.2610(9) 0.7469(8) 0.050(4) Uani 1 1 d U A . H61A H 0.4875 0.2760 0.7049 0.060 Uiso 1 1 calc R . . H61B H 0.5653 0.2946 0.7422 0.060 Uiso 1 1 calc R . . C62 C 0.4378(9) 0.2840(9) 0.8186(8) 0.047(4) Uani 1 1 d U . . H62 H 0.4075 0.3489 0.8168 0.057 Uiso 1 1 calc R A . O62 O 0.2401(7) 0.2507(7) 1.0064(5) 0.069(3) Uani 1 1 d U . . H62A H 0.1979 0.2897 0.9922 0.103 Uiso 1 1 calc R . . O63 O 0.0688(7) 0.3845(6) 0.9841(5) 0.070(3) Uani 1 1 d U . . H63 H 0.0795 0.3314 0.9729 0.106 Uiso 1 1 calc R . . C63 C 0.4727(9) 0.2621(8) 0.8901(6) 0.032(3) Uani 1 1 d U A . H63A H 0.5081 0.1987 0.8923 0.038 Uiso 1 1 calc R . . O64 O -0.0757(7) 0.5310(7) 0.9485(6) 0.075(3) Uani 1 1 d U A . H64 H -0.0651 0.5815 0.9381 0.113 Uiso 1 1 calc R . . C64 C 0.3890(10) 0.2814(10) 0.9500(7) 0.050(4) Uani 1 1 d U . . H64A H 0.3580 0.3463 0.9508 0.059 Uiso 1 1 calc R A . C65 C 0.3207(10) 0.2300(9) 0.9502(8) 0.051(4) Uani 1 1 d U A . H65 H 0.3510 0.1650 0.9507 0.061 Uiso 1 1 calc R . . O65 O -0.1099(7) 0.7154(6) 0.9136(5) 0.067(3) Uani 1 1 d U . . H65A H -0.0832 0.6736 0.9377 0.100 Uiso 1 1 calc R . . O66 O -0.1199(6) 0.9009(6) 0.8783(5) 0.062(3) Uani 1 1 d U . . H66 H -0.0743 0.9019 0.8959 0.092 Uiso 1 1 calc R . . C66 C 0.2853(10) 0.2585(8) 0.8813(8) 0.047(4) Uani 1 1 d U . . H66A H 0.2374 0.2250 0.8793 0.057 Uiso 1 1 calc R A . O67 O 0.0101(6) 0.9996(6) 0.8931(5) 0.065(3) Uani 1 1 d U . . H67 H 0.0189 1.0177 0.9300 0.097 Uiso 1 1 calc R . . C67 C 0.2308(11) 0.3734(10) 0.7294(8) 0.063(5) Uani 1 1 d U . . H67A H 0.2357 0.4097 0.6843 0.075 Uiso 1 1 calc R . . H67B H 0.2950 0.3526 0.7387 0.075 Uiso 1 1 calc R . . O68 O 0.1487(6) 1.1046(6) 0.8868(5) 0.058(3) Uani 1 1 d U . . H68 H 0.1940 1.0706 0.9013 0.088 Uiso 1 1 calc R . . C68 C 0.1671(10) 0.4275(9) 0.7890(7) 0.043(4) Uani 1 1 d U A . H68A H 0.1943 0.4788 0.7924 0.051 Uiso 1 1 calc R . . O69 O 0.3250(7) 1.0279(6) 0.9176(6) 0.074(3) Uani 1 1 d U . . H69 H 0.2714 1.0219 0.9162 0.111 Uiso 1 1 calc R . . C69 C 0.1485(10) 0.3840(10) 0.8617(8) 0.057(4) Uani 1 1 d U . . H69A H 0.1213 0.3326 0.8588 0.068 Uiso 1 1 calc R A . O70 O 0.5103(8) 0.9596(7) 0.9396(6) 0.088(4) Uani 1 1 d U . . H70 H 0.4888 1.0035 0.9662 0.132 Uiso 1 1 calc R . . C70 C 0.0867(10) 0.4383(9) 0.9207(8) 0.050(4) Uani 1 1 d U A . H70A H 0.1132 0.4883 0.9287 0.060 Uiso 1 1 calc R . . C71 C -0.0145(11) 0.4730(10) 0.9026(8) 0.059(5) Uani 1 1 d U . . H71 H -0.0420 0.4213 0.9010 0.071 Uiso 1 1 calc R A . C72 C 0.0052(10) 0.5177(8) 0.8261(7) 0.044(4) Uani 1 1 d U A . H72 H -0.0556 0.5368 0.8101 0.052 Uiso 1 1 calc R . . C73 C 0.0947(9) 0.6479(9) 0.6737(8) 0.049(4) Uani 1 1 d U . . H73A H 0.1362 0.6739 0.6334 0.059 Uiso 1 1 calc R . . H73B H 0.1327 0.5899 0.6872 0.059 Uiso 1 1 calc R . . C74 C 0.0670(8) 0.7072(7) 0.7362(6) 0.026(3) Uani 1 1 d U . . H74 H 0.1248 0.7122 0.7511 0.031 Uiso 1 1 calc R . . C75 C -0.0037(9) 0.6761(8) 0.8008(7) 0.040(4) Uani 1 1 d U . . H75 H -0.0584 0.6676 0.7835 0.048 Uiso 1 1 calc R . . C76 C -0.0408(9) 0.7429(8) 0.8579(7) 0.044(4) Uani 1 1 d U . . H76 H 0.0121 0.7521 0.8772 0.052 Uiso 1 1 calc R . . C77 C -0.0902(10) 0.8288(9) 0.8263(8) 0.056(4) Uani 1 1 d U . . H77 H -0.1463 0.8206 0.8106 0.068 Uiso 1 1 calc R . . C78 C -0.0171(8) 0.8592(8) 0.7602(7) 0.031(3) Uani 1 1 d U . . H78 H -0.0474 0.9152 0.7368 0.038 Uiso 1 1 calc R . . C79 C 0.1572(10) 0.9290(8) 0.6423(8) 0.053(4) Uani 1 1 d U . . H79A H 0.2154 0.9306 0.6045 0.064 Uiso 1 1 calc R . . H79B H 0.1456 0.8691 0.6440 0.064 Uiso 1 1 calc R . . C80 C 0.1711(8) 0.9478(7) 0.7137(6) 0.024(3) Uani 1 1 d U . . H80 H 0.2219 0.8987 0.7272 0.028 Uiso 1 1 calc R . . C81 C 0.0871(9) 0.9583(8) 0.7707(7) 0.035(4) Uani 1 1 d U . . H81 H 0.0336 1.0017 0.7551 0.042 Uiso 1 1 calc R . . C82 C 0.0949(10) 0.9837(9) 0.8405(8) 0.053(4) Uani 1 1 d U . . H82 H 0.1421 0.9351 0.8586 0.063 Uiso 1 1 calc R . . C83 C 0.1356(9) 1.0673(9) 0.8240(7) 0.045(4) Uani 1 1 d U . . H83 H 0.0854 1.1137 0.8070 0.054 Uiso 1 1 calc R . . C84 C 0.2248(11) 1.0545(10) 0.7586(8) 0.063(5) Uani 1 1 d U . . H84 H 0.2467 1.1108 0.7476 0.076 Uiso 1 1 calc R . . O1A O 0.6002(6) 0.6426(5) 0.6269(4) 0.039(2) Uiso 1 1 d D B -1 O2A O 0.5670(6) 0.5061(6) 0.6413(5) 0.060(3) Uiso 1 1 d D B -1 O3A O 0.0244(16) 0.8392(14) 1.1287(12) 0.248(10) Uiso 1 1 d D B -1 O4A O -0.0422(13) 0.7292(12) 1.1120(10) 0.188(7) Uiso 1 1 d D B -1 C1A C 0.5542(10) 0.5870(8) 0.6555(8) 0.0962(12) Uiso 1 1 d D B -1 C2A C 0.4695(7) 0.6160(9) 0.7206(5) 0.0962(12) Uiso 1 1 d GD B -1 C3A C 0.4437(8) 0.7035(8) 0.7415(6) 0.0962(12) Uiso 1 1 d G B -1 H3A1 H 0.4753 0.7457 0.7143 0.115 Uiso 1 1 calc R B -1 C4A C 0.3716(9) 0.7294(6) 0.8022(7) 0.0962(12) Uiso 1 1 d G B -1 H4A1 H 0.3540 0.7892 0.8165 0.115 Uiso 1 1 calc R B -1 C5A C 0.3254(7) 0.6677(9) 0.8420(5) 0.0962(12) Uiso 1 1 d G B -1 C6A C 0.3512(8) 0.5801(8) 0.8211(6) 0.0962(12) Uiso 1 1 d G B -1 H6A1 H 0.3195 0.5380 0.8483 0.115 Uiso 1 1 calc R B -1 C7A C 0.4233(9) 0.5543(6) 0.7604(7) 0.0962(12) Uiso 1 1 d G B -1 H7A1 H 0.4409 0.4945 0.7461 0.115 Uiso 1 1 calc R B -1 C8A C 0.2480(7) 0.6957(8) 0.9083(6) 0.0962(12) Uiso 1 1 d G B -1 C9A C 0.1731(9) 0.6541(7) 0.9261(6) 0.0962(12) Uiso 1 1 d G B -1 H9A1 H 0.1766 0.6027 0.9018 0.115 Uiso 1 1 calc R B -1 C10A C 0.0932(8) 0.6879(8) 0.9795(7) 0.0962(12) Uiso 1 1 d G B -1 H10B H 0.0421 0.6594 0.9917 0.115 Uiso 1 1 calc R B -1 C11A C 0.0882(7) 0.7632(8) 1.0151(6) 0.0962(12) Uiso 1 1 d GD B -1 C12A C 0.1631(9) 0.8047(7) 0.9973(6) 0.0962(12) Uiso 1 1 d G B -1 H12C H 0.1596 0.8562 1.0216 0.115 Uiso 1 1 calc R B -1 C13A C 0.2429(8) 0.7710(8) 0.9439(7) 0.0962(12) Uiso 1 1 d G B -1 H13B H 0.2941 0.7994 0.9317 0.115 Uiso 1 1 calc R B -1 C14A C 0.0052(12) 0.7888(12) 1.0873(7) 0.0962(12) Uiso 1 1 d D B -1 O1B O -0.0933(6) 0.7880(5) 0.5961(5) 0.045(2) Uiso 1 1 d D C -2 O2B O -0.0534(6) 0.9193(5) 0.5950(5) 0.049(2) Uiso 1 1 d D C -2 C1B C -0.0438(10) 0.8436(8) 0.5709(8) 0.0962(12) Uiso 1 1 d D C -2 C2B C 0.0408(7) 0.8138(9) 0.5055(5) 0.0962(12) Uiso 1 1 d GD C -2 C3B C 0.0491(8) 0.7365(8) 0.4714(7) 0.0962(12) Uiso 1 1 d G C -2 H3B H 0.0059 0.7002 0.4900 0.115 Uiso 1 1 calc R C -2 C4B C 0.1206(9) 0.7123(7) 0.4100(7) 0.0962(12) Uiso 1 1 d G C -2 H4B H 0.1262 0.6594 0.3867 0.115 Uiso 1 1 calc R C -2 C5B C 0.1838(7) 0.7654(9) 0.3827(5) 0.0962(12) Uiso 1 1 d G C -2 C6B C 0.1756(8) 0.8428(8) 0.4168(7) 0.0962(12) Uiso 1 1 d G C -2 H6B1 H 0.2188 0.8791 0.3981 0.115 Uiso 1 1 calc R C -2 C7B C 0.1041(9) 0.8670(7) 0.4782(6) 0.0962(12) Uiso 1 1 d G C -2 H7B H 0.0985 0.9199 0.5015 0.115 Uiso 1 1 calc R C -2 C8B C 0.2621(7) 0.7450(9) 0.3174(5) 0.0962(12) Uiso 1 1 d G C -2 C9B C 0.2790(8) 0.8174(7) 0.2730(6) 0.0962(12) Uiso 1 1 d G C -2 H9B H 0.2470 0.8758 0.2882 0.115 Uiso 1 1 calc R C -2 C10B C 0.3427(8) 0.8044(6) 0.2065(6) 0.0962(12) Uiso 1 1 d GD C -2 H10C H 0.3542 0.8539 0.1762 0.115 Uiso 1 1 calc R C -2 C11B C 0.3895(7) 0.7189(7) 0.1844(5) 0.0962(12) Uiso 1 1 d GD C -2 C12B C 0.3726(8) 0.6465(6) 0.2287(6) 0.0962(12) Uiso 1 1 d GD C -2 H12D H 0.4046 0.5881 0.2136 0.115 Uiso 1 1 calc R C -2 C13B C 0.3089(8) 0.6595(7) 0.2953(6) 0.0962(12) Uiso 1 1 d G C -2 H13C H 0.2973 0.6100 0.3256 0.115 Uiso 1 1 calc R C -2 C14B C 0.4182(12) 0.7068(10) 0.0992(6) 0.0962(12) Uiso 1 1 d D C -2 O3B O 0.4884(14) 0.6384(11) 0.0845(11) 0.221(8) Uiso 1 1 d D C -2 O4B O 0.4093(13) 0.7785(11) 0.0588(10) 0.203(8) Uiso 1 1 d D C -2 K1 K -0.2264(8) 0.9767(8) 0.6746(7) 0.176(4) Uani 0.55 1 d PU . . K3 K 0.6573(5) 1.0918(5) 0.5730(5) 0.122(3) Uani 0.65 1 d PU . . K4 K 0.7024(10) 0.4163(9) 0.5212(7) 0.198(5) Uani 0.55 1 d PU . . K5 K 0.7684(11) 0.1769(11) 0.6972(9) 0.296(7) Uani 0.70 1 d PU . . K6 K -0.0288(9) 1.1691(8) 0.6696(7) 0.197(5) Uani 0.60 1 d PU . . K8 K -0.2410(5) 0.5541(6) 0.1994(4) 0.092(3) Uani 0.50 1 d PU . . K9 K 0.0564(13) 0.4339(12) 0.1381(10) 0.223(7) Uani 0.45 1 d PU . . O1W O -0.2485(8) 1.3198(7) 0.4111(6) 0.0938(9) Uiso 1 1 d . . . O2W O -0.0867(8) 0.5170(8) 0.6878(6) 0.0938(9) Uiso 1 1 d . . . O3W O 0.4908(8) 0.2851(8) 0.5675(6) 0.0938(9) Uiso 1 1 d . . . O4W O -0.0954(8) 1.3345(7) 0.5792(6) 0.0938(9) Uiso 1 1 d . . . O5W O 0.6320(16) 0.1051(15) 1.0854(13) 0.0938(9) Uiso 0.50 1 d P . . O6W O 0.0077(8) 0.3176(8) 0.7213(6) 0.0938(9) Uiso 1 1 d . . . O7W O 0.5829(10) 0.8391(9) 0.1638(8) 0.0938(9) Uiso 0.85 1 d P . . O8W O -0.4093(9) 0.5248(9) 0.1736(7) 0.0938(9) Uiso 0.85 1 d P . . O9W O -0.1104(9) 1.1842(9) 0.1163(7) 0.0938(9) Uiso 0.85 1 d P . . O10W O -0.0829(9) 0.2850(9) 0.8492(8) 0.0938(9) Uiso 0.85 1 d P . . O11W O 0.3835(10) 0.3467(9) 0.1686(8) 0.0938(9) Uiso 0.85 1 d P . . O12W O 0.0015(9) 0.2291(9) 0.9681(8) 0.0938(9) Uiso 0.85 1 d P . . O13W O 0.5723(12) 0.3660(11) 1.1381(9) 0.0938(9) Uiso 0.70 1 d P . . O14W O -0.2374(11) 0.4338(11) 0.2706(9) 0.0938(9) Uiso 0.70 1 d P . . O15W O -0.1528(11) 1.1309(11) 0.8684(9) 0.0938(9) Uiso 0.70 1 d P . . O16W O -0.0028(14) 1.0177(13) 1.0299(11) 0.0938(9) Uiso 0.60 1 d P . . O17W O 0.2297(10) 0.3015(10) 0.1474(8) 0.0938(9) Uiso 0.80 1 d P . . O18W O 0.7218(16) 0.0737(15) 0.7836(13) 0.0938(9) Uiso 0.50 1 d P . . O19W O 0.3377(12) 1.2083(11) 0.6206(10) 0.0938(9) Uiso 0.65 1 d P . . O20W O 0.7063(12) 0.6931(11) 0.1132(9) 0.0938(9) Uiso 0.70 1 d P . . O21W O 0.6325(17) 0.0991(18) 1.2149(13) 0.0938(9) Uiso 0.50 1 d P . . O22W O 0.6130(16) 1.2059(15) 0.4493(13) 0.0938(9) Uiso 0.50 1 d P . . O23W O -0.2630(16) 0.8738(15) 0.9934(13) 0.0938(9) Uiso 0.50 1 d P . . O24W O 0.6945(17) -0.0551(17) 1.1836(13) 0.0938(9) Uiso 0.50 1 d P . . O25W O -0.3054(16) 0.9755(15) 0.9576(13) 0.0938(9) Uiso 0.50 1 d P . . O26W O -0.1956(17) 0.8094(15) 1.0376(13) 0.0938(9) Uiso 0.50 1 d P . . O27W O -0.0161(16) 1.3221(15) 0.1997(13) 0.0938(9) Uiso 0.50 1 d P . . O28W O -0.0548(16) 0.5481(15) 1.0908(13) 0.0938(9) Uiso 0.50 1 d P . . O29W O 0.1267(16) 0.1393(15) 1.0744(13) 0.0938(9) Uiso 0.50 1 d P . . O30W O 0.4692(16) 0.2494(17) 0.2126(13) 0.0938(9) Uiso 0.50 1 d P . . O31W O 0.4774(16) 0.1781(17) 1.1928(13) 0.0938(9) Uiso 0.50 1 d P . . O32W O 0.666(3) 0.027(4) 1.206(3) 0.0938(9) Uiso 0.25 1 d P . . O33W O 0.5788(18) 0.1901(17) 1.3164(14) 0.0938(9) Uiso 0.45 1 d P . . O34W O -0.1613(18) 1.3388(17) 0.0553(14) 0.0938(9) Uiso 0.45 1 d P . . O35W O 0.703(3) 0.286(3) 1.205(3) 0.0938(9) Uiso 0.25 1 d P . . O36W O 0.529(3) 1.089(3) 1.024(3) 0.0938(9) Uiso 0.25 1 d P . . O37W O 0.2986(16) 0.9380(15) 1.0451(13) 0.0938(9) Uiso 0.50 1 d P . . O38W O 0.343(3) 0.102(3) 1.118(2) 0.0938(9) Uiso 0.30 1 d P . . O39W O 0.6965(12) 1.2206(11) 0.5270(10) 0.0938(9) Uiso 0.70 1 d P . . O40W O 0.714(2) 1.2286(19) 0.5962(17) 0.0938(9) Uiso 0.40 1 d P . . 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 0.061(8) 0.042(8) 0.068(9) -0.008(7) -0.032(7) 0.011(7) O1 0.089(7) 0.063(6) 0.064(7) -0.010(5) -0.002(6) -0.009(5) C2 0.053(8) 0.059(8) 0.061(9) -0.009(7) -0.031(7) 0.006(6) O2 0.086(7) 0.064(6) 0.083(7) -0.009(6) 0.004(6) -0.028(5) O3 0.101(7) 0.062(6) 0.103(8) -0.004(6) -0.059(6) -0.016(5) C3 0.077(9) 0.068(8) 0.057(9) 0.001(7) -0.035(7) -0.029(7) O4 0.145(8) 0.104(8) 0.109(8) 0.010(6) -0.056(7) -0.068(7) C4 0.067(9) 0.047(8) 0.073(9) -0.008(7) -0.019(7) -0.005(7) O5 0.100(7) 0.088(7) 0.044(6) -0.034(5) -0.022(6) -0.010(6) C5 0.058(8) 0.065(8) 0.056(9) -0.010(7) -0.008(7) -0.025(7) O6 0.088(7) 0.068(6) 0.083(7) -0.014(5) -0.034(6) -0.006(5) C6 0.081(9) 0.055(8) 0.084(10) 0.000(7) -0.012(7) -0.015(7) C7 0.055(8) 0.038(7) 0.055(8) -0.004(6) -0.027(7) -0.023(6) O7 0.080(7) 0.104(7) 0.096(8) 0.025(6) -0.019(6) -0.028(6) O8 0.055(6) 0.067(6) 0.080(7) 0.003(5) -0.010(5) -0.038(5) C8 0.054(8) 0.050(8) 0.059(8) -0.016(7) -0.023(7) -0.013(7) O9 0.057(6) 0.058(6) 0.059(6) -0.020(5) 0.023(5) -0.041(5) C9 0.060(8) 0.036(7) 0.062(9) 0.000(6) -0.007(7) -0.022(7) O10 0.084(7) 0.065(6) 0.079(7) -0.035(5) 0.002(5) -0.047(5) C10 0.047(8) 0.040(7) 0.041(8) 0.007(6) -0.026(7) -0.005(6) O11 0.052(6) 0.059(6) 0.065(7) -0.015(5) 0.002(5) -0.011(5) C11 0.042(7) 0.017(6) 0.047(8) 0.004(6) -0.015(6) -0.019(6) O12 0.042(5) 0.043(5) 0.051(6) -0.007(5) 0.001(5) -0.020(4) C12 0.054(8) 0.064(8) 0.067(9) 0.011(7) -0.016(7) -0.029(7) O13 0.051(6) 0.059(6) 0.048(6) -0.020(5) -0.010(5) -0.020(5) C13 0.049(8) 0.041(7) 0.052(8) -0.005(7) -0.003(7) -0.010(6) O14 0.063(6) 0.038(5) 0.056(6) -0.025(5) -0.028(5) 0.008(4) C14 0.052(8) 0.066(8) 0.056(9) 0.022(7) -0.028(7) -0.022(7) O15 0.063(6) 0.027(5) 0.065(6) -0.009(4) -0.018(5) -0.019(5) C15 0.043(7) 0.049(7) 0.036(8) 0.002(6) -0.011(6) -0.019(6) C16 0.051(7) 0.033(7) 0.044(8) -0.013(6) -0.004(6) -0.032(6) O16 0.042(6) 0.045(6) 0.096(7) -0.017(5) -0.007(5) -0.018(5) O17 0.057(6) 0.042(5) 0.077(7) -0.010(5) -0.016(5) -0.021(5) C17 0.054(8) 0.050(8) 0.058(9) -0.008(7) -0.011(7) -0.010(6) O18 0.043(5) 0.027(5) 0.045(6) 0.016(4) -0.029(4) -0.019(4) C18 0.028(7) 0.030(7) 0.048(8) -0.011(6) 0.003(6) -0.012(6) O19 0.046(6) 0.056(6) 0.048(6) -0.003(5) -0.003(5) -0.044(5) C19 0.022(7) 0.030(7) 0.050(8) -0.017(6) -0.010(6) 0.010(6) O20 0.042(5) 0.029(5) 0.054(6) 0.004(4) -0.010(5) -0.017(4) C20 0.042(8) 0.050(8) 0.061(9) -0.008(7) -0.015(7) -0.004(6) O21 0.022(5) 0.051(5) 0.036(6) -0.006(4) -0.010(4) -0.010(4) C21 0.035(7) 0.035(7) 0.051(8) -0.014(6) -0.013(6) -0.007(6) C22 0.032(7) 0.034(7) 0.050(8) -0.003(6) -0.008(6) -0.009(6) O22 0.058(6) 0.086(7) 0.072(7) -0.019(5) -0.003(5) -0.011(5) O23 0.052(6) 0.047(5) 0.052(6) -0.015(5) -0.010(5) 0.006(5) C23 0.040(7) 0.038(7) 0.060(8) -0.016(6) -0.017(6) -0.015(6) C24 0.045(8) 0.050(8) 0.062(9) -0.008(7) -0.009(7) -0.006(6) O24 0.114(8) 0.111(8) 0.124(9) -0.029(7) -0.030(7) -0.007(7) O25 0.045(5) 0.044(5) 0.039(6) 0.014(4) -0.030(4) -0.028(4) C25 0.046(8) 0.054(8) 0.058(8) -0.006(7) 0.001(7) -0.014(6) O26 0.034(5) 0.046(5) 0.053(6) -0.010(4) -0.022(5) -0.001(4) C26 0.027(7) 0.034(7) 0.043(8) 0.003(6) 0.000(6) -0.016(6) O27 0.067(6) 0.046(6) 0.063(7) 0.004(5) -0.013(5) -0.016(5) C27 0.041(7) 0.034(7) 0.037(8) 0.013(6) -0.016(6) -0.014(6) C28 0.034(7) 0.033(7) 0.053(8) -0.013(6) -0.008(7) -0.006(6) O28 0.051(6) 0.050(6) 0.073(7) -0.012(5) -0.019(5) -0.022(5) O29 0.040(5) 0.045(5) 0.034(6) -0.007(4) 0.004(5) -0.008(4) C29 0.023(7) 0.043(7) 0.033(7) -0.005(6) 0.002(6) 0.013(6) O30 0.036(5) 0.034(5) 0.044(6) -0.009(4) -0.009(4) -0.014(4) C30 0.065(8) 0.055(8) 0.054(8) -0.004(7) -0.021(7) -0.017(7) O31 0.066(7) 0.057(6) 0.100(8) -0.011(6) -0.023(6) -0.005(5) C31 0.046(8) 0.027(7) 0.035(8) 0.002(6) 0.005(6) -0.012(6) O32 0.051(6) 0.031(5) 0.051(6) 0.005(4) -0.023(5) -0.022(4) C32 0.039(7) 0.026(7) 0.016(7) 0.005(5) 0.002(6) -0.005(6) O33 0.047(5) 0.030(5) 0.049(6) 0.005(4) -0.003(5) -0.012(4) C33 0.038(7) 0.049(8) 0.059(8) -0.020(7) -0.002(7) -0.006(6) O34 0.031(5) 0.027(5) 0.056(6) -0.002(4) -0.011(5) -0.022(4) C34 0.046(7) 0.039(7) 0.045(8) 0.007(6) -0.006(7) -0.017(6) O35 0.053(6) 0.039(5) 0.061(6) 0.007(4) -0.030(5) -0.022(4) C35 0.007(6) 0.041(7) 0.028(7) -0.010(6) 0.005(6) -0.001(5) C36 0.053(8) 0.038(7) 0.034(8) -0.017(6) -0.010(6) -0.002(6) O36 0.122(13) 0.140(14) 0.130(14) -0.021(9) -0.028(9) -0.019(9) O36' 0.042(9) 0.057(9) 0.052(9) 0.013(7) 0.012(7) -0.017(7) C55 0.068(9) 0.079(9) 0.098(10) 0.003(8) -0.007(8) -0.017(7) C37 0.026(7) 0.025(6) 0.038(8) -0.001(6) -0.006(6) -0.010(6) O37 0.074(6) 0.072(6) 0.066(7) -0.026(5) -0.004(5) -0.002(5) O38 0.082(6) 0.041(5) 0.042(6) -0.014(4) 0.000(5) -0.016(5) C38 0.039(7) 0.043(7) 0.043(8) -0.006(6) -0.005(6) -0.003(6) O39 0.064(6) 0.049(5) 0.069(6) -0.017(5) -0.018(5) -0.008(5) C39 0.041(7) 0.029(7) 0.037(8) 0.002(6) 0.007(6) -0.016(6) O40 0.040(5) 0.052(6) 0.082(7) 0.003(5) -0.026(5) -0.011(4) C40 0.040(7) 0.034(7) 0.049(8) -0.007(6) -0.001(6) -0.014(6) O41 0.062(6) 0.043(5) 0.053(6) -0.003(5) 0.010(5) -0.023(5) C41 0.060(8) 0.052(8) 0.057(9) -0.024(7) -0.008(7) 0.011(7) O42 0.039(5) 0.067(6) 0.069(6) 0.005(5) -0.014(5) -0.031(5) C42 0.087(9) 0.081(9) 0.074(9) -0.014(7) -0.029(8) -0.030(8) O43 0.027(5) 0.064(6) 0.041(6) -0.005(5) -0.004(4) -0.009(5) C43 0.051(7) 0.032(7) 0.047(8) -0.009(6) -0.020(6) -0.006(6) C44 0.039(7) 0.018(6) 0.038(8) 0.010(6) -0.004(6) -0.009(6) O44 0.050(6) 0.051(6) 0.056(6) -0.013(5) -0.003(5) -0.002(5) O45 0.059(6) 0.026(5) 0.060(6) 0.000(4) -0.015(5) -0.017(4) C45 0.048(8) 0.057(8) 0.045(8) 0.008(6) -0.021(7) -0.018(6) C46 0.057(8) 0.045(7) 0.059(8) -0.010(6) -0.003(7) -0.019(6) O46 0.064(6) 0.050(5) 0.058(6) -0.011(5) -0.017(5) -0.031(5) O47 0.041(5) 0.032(5) 0.059(6) -0.006(4) 0.001(5) -0.021(4) C47 0.056(8) 0.079(9) 0.084(9) 0.010(7) -0.031(7) -0.029(7) O48 0.050(5) 0.049(5) 0.038(6) -0.001(4) -0.009(5) -0.020(4) C48 0.061(8) 0.059(8) 0.087(9) -0.008(7) -0.019(7) -0.041(7) O49 0.040(6) 0.050(5) 0.045(6) 0.002(5) -0.001(5) -0.024(4) C49 0.065(8) 0.063(8) 0.055(9) -0.007(7) -0.012(7) -0.012(7) O50 0.046(6) 0.045(6) 0.091(7) 0.011(5) -0.020(5) -0.023(5) C50 0.031(7) 0.053(7) 0.049(8) 0.009(6) -0.019(6) -0.023(6) O51 0.031(5) 0.049(5) 0.055(6) 0.010(4) -0.016(4) -0.014(4) C51 0.032(7) 0.050(7) 0.060(8) 0.026(6) -0.020(6) -0.015(6) O52 0.048(6) 0.051(6) 0.085(7) -0.023(5) -0.011(5) -0.003(5) C52 0.039(7) 0.048(7) 0.041(8) -0.015(6) 0.004(6) -0.022(6) O53 0.052(6) 0.042(5) 0.069(6) -0.010(5) -0.015(5) -0.022(5) C53 0.078(9) 0.058(8) 0.044(8) -0.006(7) -0.004(7) -0.006(7) O54 0.047(5) 0.054(6) 0.066(6) 0.005(5) -0.029(5) -0.021(5) C54 0.050(7) 0.052(7) 0.047(8) -0.005(6) -0.008(6) -0.012(6) O55 0.033(5) 0.036(5) 0.064(6) 0.009(4) -0.005(5) -0.019(4) O56 0.044(5) 0.043(5) 0.067(6) -0.005(4) -0.030(5) -0.028(4) C56 0.055(8) 0.066(8) 0.063(9) 0.000(7) -0.013(7) -0.019(6) O57 0.081(7) 0.052(6) 0.074(7) -0.012(5) -0.006(6) 0.020(5) C57 0.071(8) 0.059(8) 0.070(9) 0.002(7) -0.025(7) -0.021(7) O58 0.077(6) 0.049(6) 0.064(7) 0.010(5) -0.015(5) -0.003(5) C58 0.049(7) 0.044(7) 0.048(8) 0.006(6) -0.022(6) -0.024(6) O59 0.101(7) 0.080(7) 0.088(7) 0.002(5) -0.057(6) -0.021(5) C59 0.076(9) 0.069(9) 0.083(9) 0.001(7) -0.025(7) -0.032(7) O60 0.116(7) 0.064(6) 0.092(8) -0.032(6) -0.045(6) -0.011(6) C60 0.055(8) 0.045(7) 0.054(8) 0.009(6) -0.024(7) -0.001(6) O61 0.099(7) 0.089(7) 0.064(7) -0.017(5) -0.054(6) -0.003(5) C61 0.046(7) 0.047(7) 0.051(8) 0.005(6) -0.010(6) -0.005(6) C62 0.043(7) 0.043(7) 0.053(8) -0.016(6) -0.010(7) -0.002(6) O62 0.079(7) 0.082(6) 0.044(6) 0.006(5) -0.006(5) -0.028(5) O63 0.078(6) 0.069(6) 0.053(6) 0.010(5) -0.008(5) -0.009(5) C63 0.036(7) 0.032(6) 0.029(7) -0.003(6) -0.013(6) -0.006(6) O64 0.065(6) 0.073(6) 0.074(7) -0.001(6) -0.006(6) -0.005(5) C64 0.055(8) 0.051(7) 0.038(8) 0.009(6) -0.024(7) 0.004(6) C65 0.056(8) 0.054(8) 0.048(8) -0.013(6) -0.023(7) -0.008(7) O65 0.063(6) 0.074(6) 0.062(6) -0.012(5) 0.000(5) -0.026(5) O66 0.054(6) 0.052(6) 0.080(7) -0.035(5) 0.008(5) -0.027(5) C66 0.061(8) 0.024(7) 0.054(8) -0.003(6) -0.008(7) -0.008(6) O67 0.045(6) 0.076(6) 0.067(7) -0.023(5) 0.017(5) -0.025(5) C67 0.070(8) 0.062(8) 0.056(8) 0.004(7) -0.007(7) -0.026(7) O68 0.063(6) 0.053(6) 0.060(6) -0.016(5) -0.010(5) -0.013(5) C68 0.059(8) 0.042(7) 0.037(8) -0.012(6) -0.024(6) -0.014(6) O69 0.072(6) 0.069(6) 0.080(7) -0.008(5) -0.011(5) -0.020(5) C69 0.051(8) 0.064(8) 0.062(9) 0.009(7) -0.021(7) -0.023(6) O70 0.121(7) 0.095(7) 0.074(7) -0.009(5) -0.052(6) -0.040(6) C70 0.054(8) 0.052(8) 0.043(8) 0.003(7) -0.009(7) -0.013(6) C71 0.062(8) 0.060(8) 0.048(8) -0.003(7) -0.010(7) -0.004(7) C72 0.038(7) 0.044(7) 0.054(8) 0.001(6) -0.016(6) -0.014(6) C73 0.045(7) 0.041(7) 0.049(8) 0.003(6) -0.004(6) 0.005(6) C74 0.029(6) 0.023(6) 0.026(7) -0.004(5) -0.005(6) -0.005(5) C75 0.041(7) 0.037(7) 0.050(8) 0.008(6) -0.014(6) -0.024(6) C76 0.039(7) 0.041(7) 0.040(8) 0.008(6) 0.019(6) -0.019(6) C77 0.049(8) 0.061(8) 0.059(8) -0.023(7) 0.003(7) -0.022(7) C78 0.028(7) 0.028(6) 0.041(7) -0.003(6) -0.006(6) -0.015(5) C79 0.064(8) 0.035(7) 0.072(9) -0.011(6) -0.023(7) -0.020(6) C80 0.019(6) 0.025(6) 0.021(7) 0.000(5) 0.010(6) -0.010(5) C81 0.039(7) 0.032(7) 0.042(8) -0.011(6) -0.021(6) -0.011(6) C82 0.048(8) 0.059(8) 0.047(8) -0.017(6) -0.002(7) -0.008(6) C83 0.042(7) 0.045(7) 0.051(8) 0.003(6) -0.007(6) -0.021(6) C84 0.063(8) 0.063(8) 0.066(9) 0.010(7) -0.013(7) -0.025(7) K1 0.167(8) 0.158(7) 0.184(8) -0.032(6) -0.006(7) -0.030(6) K3 0.081(5) 0.128(5) 0.151(6) -0.028(5) -0.021(4) -0.013(4) K4 0.206(9) 0.185(8) 0.184(9) -0.001(7) -0.030(7) -0.029(7) K5 0.281(10) 0.309(10) 0.296(10) -0.053(8) -0.094(8) -0.027(8) K6 0.210(8) 0.173(8) 0.212(9) -0.014(7) -0.063(7) -0.034(6) K8 0.063(5) 0.145(6) 0.078(6) -0.031(5) -0.004(4) -0.047(5) K9 0.223(10) 0.227(11) 0.189(10) -0.002(8) -0.051(8) 0.000(8) #============================================================================== # GEOMETRY #============================================================================== _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 C2 1.436(19) . ? C1 O16 1.450(15) . ? C1 O31 1.452(16) . ? C1 H1 1.0000 . ? O1 C38 1.485(15) . ? O1 H1A 0.8400 . ? C2 O3 1.428(16) . ? C2 C3 1.497(19) . ? C2 H2 1.0000 . ? O2 C39 1.464(15) . ? O2 H2A 0.8400 . ? O3 H3 0.8400 . ? C3 O4 1.436(17) . ? C3 C4 1.464(18) . ? C3 H3A 1.0000 . ? O4 H4 0.8400 . ? C4 O17 1.488(16) . ? C4 C5 1.567(19) . ? C4 H4A 1.0000 . ? O5 C8 1.397(15) . ? O5 H5 0.8400 . ? C5 O31 1.483(16) . ? C5 C6 1.55(2) . ? C5 H5A 1.0000 . ? O6 C9 1.478(16) . ? O6 H6 0.8400 . ? C6 O24 1.342(17) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O32 1.376(14) . ? C7 O17 1.435(14) . ? C7 C8 1.463(18) . ? C7 H7 1.0000 . ? O7 C14 1.406(16) . ? O7 H7A 0.8400 . ? O8 C15 1.454(15) . ? O8 H8 0.8400 . ? C8 C9 1.457(18) . ? C8 H8A 1.0000 . ? O9 C20 1.304(16) . ? O9 H9 0.8400 . ? C9 C10 1.571(18) . ? C9 H9A 1.0000 . ? O10 C21 1.395(14) . ? O10 H10 0.8400 . ? C10 O18 1.409(14) . ? C10 C11 1.488(17) . ? C10 H10A 1.0000 . ? O11 C26 1.420(14) . ? O11 H11 0.8400 . ? C11 O32 1.419(13) . ? C11 C12 1.511(17) . ? C11 H11A 1.0000 . ? O12 C27 1.406(14) . ? O12 H12 0.8400 . ? C12 O25 1.377(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O13 C32 1.437(14) . ? O13 H13 0.8400 . ? C13 O18 1.361(14) . ? C13 C14 1.450(19) . ? C13 O33 1.514(16) . ? C13 H13A 1.0000 . ? O14 C33 1.398(15) . ? O14 H14 0.8400 . ? C14 C15 1.451(17) . ? C14 H14A 1.0000 . ? O15 C37 1.415(13) . ? O15 C34 1.491(14) . ? C15 C16 1.511(17) . ? C15 H15 1.0000 . ? C16 O19 1.370(13) . ? C16 C17 1.563(18) . ? C16 H16 1.0000 . ? O16 C40 1.365(14) . ? C17 O33 1.490(15) . ? C17 C18 1.522(17) . ? C17 H17 1.0000 . ? C18 O26 1.367(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O19 C19 1.422(14) . ? C19 O34 1.320(15) . ? C19 C20 1.530(18) . ? C19 H19 1.0000 . ? O20 C25 1.381(15) . ? O20 C22 1.435(14) . ? C20 C21 1.617(17) . ? C20 H20 1.0000 . ? O21 C31 1.373(14) . ? O21 C28 1.417(14) . ? C21 C22 1.561(17) . ? C21 H21 1.0000 . ? C22 C23 1.454(16) . ? C22 H22 1.0000 . ? O22 C36 1.538(15) . ? O22 H22A 0.8400 . ? O23 C42 1.432(16) . ? O23 H23 0.8400 . ? C23 O34 1.437(13) . ? C23 C24 1.547(18) . ? C23 H23A 1.0000 . ? C24 O27 1.391(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O24 H24 0.8400 . ? O25 H25 0.8400 . ? C25 O35 1.483(15) . ? C25 C26 1.581(18) . ? C25 H25A 1.0000 . ? O26 H26 0.8400 . ? C26 C27 1.447(16) . ? C26 H26A 1.0000 . ? O27 H27 0.8400 . ? C27 C28 1.465(17) . ? C27 H27A 1.0000 . ? C28 C29 1.533(17) . ? C28 H28 1.0000 . ? O28 C30 1.399(14) . ? O28 H28A 0.8400 . ? O29 C31 1.423(14) . ? O29 C35 1.489(13) . ? C29 C30 1.418(17) . ? C29 O35 1.492(14) . ? C29 H29 1.0000 . ? O30 C37 1.399(14) . ? O30 C41 1.420(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.554(17) . ? C31 H31 1.0000 . ? C32 C33 1.502(16) . ? C32 H32 1.0000 . ? C33 C34 1.541(18) . ? C33 H33 1.0000 . ? C34 C35 1.507(16) . ? C34 H34 1.0000 . ? C35 C36 1.488(16) . ? C35 H35 1.0000 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O36 C55 1.31(3) . ? O36 H36 0.8400 . ? O36' C55 1.46(2) . ? O36' H36' 0.8400 . ? C55 C56 1.44(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C55 H55C 0.9900 . ? C55 H55D 0.9900 . ? C37 C38 1.488(17) . ? C37 H37 1.0000 . ? O37 C61 1.437(15) . ? O37 H37A 0.8400 . ? O38 C67 1.451(14) . ? O38 H38 0.8400 . ? C38 C39 1.411(16) . ? C38 H38A 1.0000 . ? O39 C73 1.454(14) . ? O39 H39 0.8400 . ? C39 C40 1.466(17) . ? C39 H39A 1.0000 . ? O40 C79 1.493(15) . ? O40 H40 0.8400 . ? C40 C41 1.507(19) . ? C40 H40A 1.0000 . ? O41 C43 1.430(13) . ? O41 H41 0.8400 . ? C41 C42 1.45(2) . ? C41 H41A 1.0000 . ? O42 C49 1.465(15) . ? O42 H42 0.8400 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O43 C54 1.385(15) . ? O43 C50 1.410(14) . ? C43 C44 1.434(16) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O49 1.448(14) . ? C44 C45 1.531(17) . ? C44 H44 1.0000 . ? O44 C60 1.325(15) . ? O44 C56 1.509(16) . ? O45 C66 1.437(15) . ? O45 C62 1.469(14) . ? C45 O56 1.444(14) . ? C45 C46 1.614(18) . ? C45 H45 1.0000 . ? C46 O69 1.384(15) . ? C46 C47 1.538(18) . ? C46 H46 1.0000 . ? O46 C72 1.430(15) . ? O46 C68 1.449(14) . ? O47 C74 1.396(13) . ? O47 C78 1.429(14) . ? C47 O70 1.461(17) . ? C47 C48 1.56(2) . ? C47 H47 1.0000 . ? O48 C84 1.363(16) . ? O48 C80 1.459(12) . ? C48 O50 1.394(15) . ? C48 O49 1.451(17) . ? C48 H48 1.0000 . ? C49 C50 1.527(18) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? O50 C51 1.373(14) . ? C50 C51 1.590(18) . ? C50 H50 1.0000 . ? O51 C54 1.388(14) . ? O51 C57 1.423(15) . ? C51 C52 1.497(17) . ? C51 H51 1.0000 . ? O52 C60 1.344(14) . ? O52 C63 1.465(13) . ? C52 O57 1.398(14) . ? C52 C53 1.496(18) . ? C52 H52 1.0000 . ? O53 C66 1.396(14) . ? O53 C69 1.495(15) . ? C53 O58 1.409(16) . ? C53 C54 1.516(19) . ? C53 H53 1.0000 . ? O54 C75 1.410(14) . ? O54 C72 1.434(14) . ? C54 H54 1.0000 . ? O55 C81 1.487(13) . ? O55 C78 1.495(13) . ? O56 C84 1.467(16) . ? C56 C57 1.473(19) . ? C56 H56 1.0000 . ? O57 H57 0.8400 . ? C57 C58 1.654(19) . ? C57 H57A 1.0000 . ? O58 H58 0.8400 . ? C58 C59 1.407(18) . ? C58 O59 1.441(14) . ? C58 H58A 1.0000 . ? O59 H59 0.8400 . ? C59 O60 1.454(17) . ? C59 C60 1.526(19) . ? C59 H59A 1.0000 . ? O60 H60 0.8400 . ? C60 H60A 1.0000 . ? O61 C64 1.443(14) . ? O61 H61 0.8400 . ? C61 C62 1.575(17) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.571(16) . ? C62 H62 1.0000 . ? O62 C65 1.396(15) . ? O62 H62A 0.8400 . ? O63 C70 1.423(15) . ? O63 H63 0.8400 . ? C63 C64 1.465(17) . ? C63 H63A 1.0000 . ? O64 C71 1.327(16) . ? O64 H64 0.8400 . ? C64 C65 1.450(17) . ? C64 H64A 1.0000 . ? C65 C66 1.536(17) . ? C65 H65 1.0000 . ? O65 C76 1.412(14) . ? O65 H65A 0.8400 . ? O66 C77 1.481(15) . ? O66 H66 0.8400 . ? C66 H66A 1.0000 . ? O67 C82 1.395(15) . ? O67 H67 0.8400 . ? C67 C68 1.469(18) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? O68 C83 1.464(14) . ? O68 H68 0.8400 . ? C68 C69 1.491(18) . ? C68 H68A 1.0000 . ? O69 H69 0.8400 . ? C69 C70 1.456(19) . ? C69 H69A 1.0000 . ? O70 H70 0.8400 . ? C70 C71 1.590(18) . ? C70 H70A 1.0000 . ? C71 C72 1.561(18) . ? C71 H71 1.0000 . ? C72 H72 1.0000 . ? C73 C74 1.495(16) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.548(16) . ? C74 H74 1.0000 . ? C75 C76 1.488(17) . ? C75 H75 1.0000 . ? C76 C77 1.512(18) . ? C76 H76 1.0000 . ? C77 C78 1.581(18) . ? C77 H77 1.0000 . ? C78 H78 1.0000 . ? C79 C80 1.507(16) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.433(15) . ? C80 H80 1.0000 . ? C81 C82 1.475(16) . ? C81 H81 1.0000 . ? C82 C83 1.551(17) . ? C82 H82 1.0000 . ? C83 C84 1.576(19) . ? C83 H83 1.0000 . ? C84 H84 1.0000 . ? O1A C1A 1.249(9) . ? O2A C1A 1.272(9) . ? O3A C14A 1.30(3) . ? O4A C14A 1.30(3) . ? C1A C2A 1.549(11) . ? C2A C3A 1.3900 . ? C2A C7A 1.3900 . ? C3A C4A 1.3900 . ? C3A H3A1 0.9500 . ? C4A C5A 1.3900 . ? C4A H4A1 0.9500 . ? C5A C6A 1.3900 . ? C6A C7A 1.3900 . ? C6A H6A1 0.9500 . ? C7A H7A1 0.9500 . ? C8A C9A 1.3900 . ? C8A C13A 1.3900 . ? C9A C10A 1.3900 . ? C9A H9A1 0.9500 . ? C10A C11A 1.3900 . ? C10A H10B 0.9500 . ? C11A C12A 1.3900 . ? C11A C14A 1.620(12) . ? C12A C13A 1.3900 . ? C12A H12C 0.9500 . ? C13A H13B 0.9500 . ? O1B C1B 1.268(9) . ? O2B C1B 1.269(9) . ? C1B C2B 1.556(11) . ? C2B C3B 1.3900 . ? C2B C7B 1.3900 . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C6B C7B 1.3900 . ? C6B H6B1 0.9500 . ? C7B H7B 0.9500 . ? C8B C9B 1.3900 . ? C8B C13B 1.3900 . ? C9B C10B 1.3900 . ? C9B H9B 0.9500 . ? C10B C11B 1.3900 . ? C10B H10C 0.9500 . ? C11B C12B 1.3900 . ? C11B C14B 1.605(8) . ? C12B C13B 1.3900 . ? C12B H12D 0.9500 . ? C13B H13C 0.9500 . ? C14B O3B 1.289(10) . ? C14B O4B 1.300(10) . ? K1 K3 3.091(15) 1_455 ? K3 O39W 2.276(18) . ? K3 K1 3.091(16) 1_655 ? K5 O40W 2.29(3) 1_545 ? K5 O18W 2.31(3) . ? K5 K6 2.92(2) 1_645 ? K6 K5 2.92(2) 1_465 ? K8 O14W 2.217(18) . ? K9 O27W 2.36(3) 1_545 ? K9 O28W 2.39(3) 1_554 ? O21W O32W 1.12(5) . ? O23W O26W 1.58(3) . ? O23W O25W 1.70(3) . ? O24W O32W 1.32(5) . ? O27W K9 2.36(3) 1_565 ? O28W K9 2.39(3) 1_556 ? O30W O31W 1.18(3) 1_554 ? O31W O30W 1.18(3) 1_556 ? O39W O40W 1.44(3) . ? O40W K5 2.29(3) 1_565 ? 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 C2 C1 O16 107.2(14) . . ? C2 C1 O31 112.4(14) . . ? O16 C1 O31 109.0(11) . . ? C2 C1 H1 109.4 . . ? O16 C1 H1 109.4 . . ? O31 C1 H1 109.4 . . ? C38 O1 H1A 109.5 . . ? O3 C2 C1 114.2(14) . . ? O3 C2 C3 111.4(14) . . ? C1 C2 C3 112.9(13) . . ? O3 C2 H2 105.9 . . ? C1 C2 H2 105.9 . . ? C3 C2 H2 105.9 . . ? C39 O2 H2A 109.5 . . ? C2 O3 H3 109.5 . . ? O4 C3 C4 109.9(13) . . ? O4 C3 C2 113.5(13) . . ? C4 C3 C2 108.3(14) . . ? O4 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? C3 O4 H4 109.5 . . ? C3 C4 O17 107.9(13) . . ? C3 C4 C5 113.8(13) . . ? O17 C4 C5 103.2(12) . . ? C3 C4 H4A 110.6 . . ? O17 C4 H4A 110.6 . . ? C5 C4 H4A 110.6 . . ? C8 O5 H5 109.5 . . ? O31 C5 C6 105.0(13) . . ? O31 C5 C4 105.3(12) . . ? C6 C5 C4 111.4(13) . . ? O31 C5 H5A 111.6 . . ? C6 C5 H5A 111.6 . . ? C4 C5 H5A 111.6 . . ? C9 O6 H6 109.5 . . ? O24 C6 C5 109.6(14) . . ? O24 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O24 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? O32 C7 O17 111.8(11) . . ? O32 C7 C8 112.2(12) . . ? O17 C7 C8 108.4(12) . . ? O32 C7 H7 108.1 . . ? O17 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C14 O7 H7A 109.5 . . ? C15 O8 H8 109.5 . . ? O5 C8 C9 108.5(13) . . ? O5 C8 C7 113.8(12) . . ? C9 C8 C7 108.1(14) . . ? O5 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C20 O9 H9 109.5 . . ? C8 C9 O6 112.3(12) . . ? C8 C9 C10 111.5(13) . . ? O6 C9 C10 106.4(11) . . ? C8 C9 H9A 108.9 . . ? O6 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? C21 O10 H10 109.5 . . ? O18 C10 C11 110.8(11) . . ? O18 C10 C9 109.8(11) . . ? C11 C10 C9 109.2(11) . . ? O18 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? C26 O11 H11 109.5 . . ? O32 C11 C10 110.8(11) . . ? O32 C11 C12 106.3(11) . . ? C10 C11 C12 109.7(11) . . ? O32 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? C27 O12 H12 109.5 . . ? O25 C12 C11 116.7(11) . . ? O25 C12 H12A 108.1 . . ? C11 C12 H12A 108.1 . . ? O25 C12 H12B 108.1 . . ? C11 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C32 O13 H13 109.5 . . ? O18 C13 C14 111.3(13) . . ? O18 C13 O33 111.6(11) . . ? C14 C13 O33 110.4(12) . . ? O18 C13 H13A 107.8 . . ? C14 C13 H13A 107.8 . . ? O33 C13 H13A 107.8 . . ? C33 O14 H14 109.5 . . ? O7 C14 C13 113.4(13) . . ? O7 C14 C15 114.0(13) . . ? C13 C14 C15 111.1(13) . . ? O7 C14 H14A 105.9 . . ? C13 C14 H14A 105.9 . . ? C15 C14 H14A 105.9 . . ? C37 O15 C34 117.3(9) . . ? C14 C15 O8 113.2(12) . . ? C14 C15 C16 113.0(12) . . ? O8 C15 C16 108.7(11) . . ? C14 C15 H15 107.2 . . ? O8 C15 H15 107.2 . . ? C16 C15 H15 107.2 . . ? O19 C16 C15 112.7(11) . . ? O19 C16 C17 108.6(10) . . ? C15 C16 C17 110.3(12) . . ? O19 C16 H16 108.4 . . ? C15 C16 H16 108.4 . . ? C17 C16 H16 108.4 . . ? C40 O16 C1 121.9(11) . . ? C7 O17 C4 119.4(10) . . ? O33 C17 C18 101.5(10) . . ? O33 C17 C16 109.2(11) . . ? C18 C17 C16 111.2(12) . . ? O33 C17 H17 111.5 . . ? C18 C17 H17 111.5 . . ? C16 C17 H17 111.5 . . ? C13 O18 C10 120.9(10) . . ? O26 C18 C17 114.8(11) . . ? O26 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? O26 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? C16 O19 C19 122.4(10) . . ? O34 C19 O19 113.4(11) . . ? O34 C19 C20 115.6(12) . . ? O19 C19 C20 105.2(12) . . ? O34 C19 H19 107.4 . . ? O19 C19 H19 107.4 . . ? C20 C19 H19 107.4 . . ? C25 O20 C22 114.3(10) . . ? O9 C20 C19 116.7(13) . . ? O9 C20 C21 110.5(12) . . ? C19 C20 C21 107.0(11) . . ? O9 C20 H20 107.4 . . ? C19 C20 H20 107.4 . . ? C21 C20 H20 107.4 . . ? C31 O21 C28 117.1(10) . . ? O10 C21 C22 111.2(11) . . ? O10 C21 C20 111.0(11) . . ? C22 C21 C20 108.9(11) . . ? O10 C21 H21 108.5 . . ? C22 C21 H21 108.5 . . ? C20 C21 H21 108.5 . . ? O20 C22 C23 112.6(11) . . ? O20 C22 C21 105.1(10) . . ? C23 C22 C21 111.1(11) . . ? O20 C22 H22 109.3 . . ? C23 C22 H22 109.3 . . ? C21 C22 H22 109.3 . . ? C36 O22 H22A 109.5 . . ? C42 O23 H23 109.5 . . ? O34 C23 C22 112.5(11) . . ? O34 C23 C24 104.9(11) . . ? C22 C23 C24 114.8(12) . . ? O34 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? C24 C23 H23A 108.1 . . ? O27 C24 C23 110.7(12) . . ? O27 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? O27 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C6 O24 H24 109.5 . . ? C12 O25 H25 109.5 . . ? O20 C25 O35 110.0(11) . . ? O20 C25 C26 105.9(11) . . ? O35 C25 C26 104.4(10) . . ? O20 C25 H25A 112.0 . . ? O35 C25 H25A 112.0 . . ? C26 C25 H25A 112.0 . . ? C18 O26 H26 109.5 . . ? O11 C26 C27 116.9(11) . . ? O11 C26 C25 103.7(10) . . ? C27 C26 C25 114.7(12) . . ? O11 C26 H26A 107.0 . . ? C27 C26 H26A 107.0 . . ? C25 C26 H26A 107.0 . . ? C24 O27 H27 109.5 . . ? O12 C27 C26 108.4(12) . . ? O12 C27 C28 109.1(11) . . ? C26 C27 C28 109.3(11) . . ? O12 C27 H27A 110.0 . . ? C26 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O21 C28 C27 106.0(11) . . ? O21 C28 C29 106.8(10) . . ? C27 C28 C29 111.8(11) . . ? O21 C28 H28 110.7 . . ? C27 C28 H28 110.7 . . ? C29 C28 H28 110.7 . . ? C30 O28 H28A 109.5 . . ? C31 O29 C35 114.7(9) . . ? C30 C29 O35 107.0(11) . . ? C30 C29 C28 114.3(12) . . ? O35 C29 C28 108.9(10) . . ? C30 C29 H29 108.9 . . ? O35 C29 H29 108.9 . . ? C28 C29 H29 108.9 . . ? C37 O30 C41 111.0(10) . . ? O28 C30 C29 113.7(13) . . ? O28 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? O28 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C1 O31 C5 112.9(12) . . ? O21 C31 O29 111.2(10) . . ? O21 C31 C32 110.3(10) . . ? O29 C31 C32 105.6(11) . . ? O21 C31 H31 109.9 . . ? O29 C31 H31 109.9 . . ? C32 C31 H31 109.9 . . ? C7 O32 C11 114.8(10) . . ? O13 C32 C33 109.6(10) . . ? O13 C32 C31 104.1(10) . . ? C33 C32 C31 109.1(11) . . ? O13 C32 H32 111.3 . . ? C33 C32 H32 111.3 . . ? C31 C32 H32 111.3 . . ? C17 O33 C13 109.3(10) . . ? O14 C33 C32 110.9(11) . . ? O14 C33 C34 110.5(11) . . ? C32 C33 C34 108.2(12) . . ? O14 C33 H33 109.1 . . ? C32 C33 H33 109.1 . . ? C34 C33 H33 109.1 . . ? C19 O34 C23 115.7(10) . . ? O15 C34 C35 103.8(10) . . ? O15 C34 C33 105.7(10) . . ? C35 C34 C33 112.2(12) . . ? O15 C34 H34 111.6 . . ? C35 C34 H34 111.6 . . ? C33 C34 H34 111.6 . . ? C25 O35 C29 115.7(10) . . ? C36 C35 O29 105.7(10) . . ? C36 C35 C34 115.3(11) . . ? O29 C35 C34 106.8(9) . . ? C36 C35 H35 109.6 . . ? O29 C35 H35 109.6 . . ? C34 C35 H35 109.6 . . ? C35 C36 O22 107.2(10) . . ? C35 C36 H36A 110.3 . . ? O22 C36 H36A 110.3 . . ? C35 C36 H36B 110.3 . . ? O22 C36 H36B 110.3 . . ? H36A C36 H36B 108.5 . . ? C55 O36 H36 109.5 . . ? C55 O36' H36' 109.5 . . ? O36 C55 C56 120(2) . . ? O36 C55 O36' 92.2(19) . . ? C56 C55 O36' 115.7(15) . . ? O36 C55 H55A 107.3 . . ? C56 C55 H55A 107.3 . . ? O36 C55 H55B 107.3 . . ? C56 C55 H55B 107.3 . . ? O36' C55 H55B 113.7 . . ? H55A C55 H55B 106.9 . . ? C56 C55 H55C 108.4 . . ? O36' C55 H55C 108.4 . . ? H55A C55 H55C 123.5 . . ? H55B C55 H55C 102.6 . . ? O36 C55 H55D 110.8 . . ? C56 C55 H55D 108.4 . . ? O36' C55 H55D 108.4 . . ? H55A C55 H55D 101.1 . . ? H55C C55 H55D 107.4 . . ? O30 C37 O15 111.2(10) . . ? O30 C37 C38 110.6(11) . . ? O15 C37 C38 109.6(11) . . ? O30 C37 H37 108.4 . . ? O15 C37 H37 108.4 . . ? C38 C37 H37 108.4 . . ? C61 O37 H37A 109.5 . . ? C67 O38 H38 109.5 . . ? C39 C38 O1 114.7(12) . . ? C39 C38 C37 110.4(12) . . ? O1 C38 C37 105.2(11) . . ? C39 C38 H38A 108.8 . . ? O1 C38 H38A 108.8 . . ? C37 C38 H38A 108.8 . . ? C73 O39 H39 109.5 . . ? C38 C39 O2 106.5(12) . . ? C38 C39 C40 111.8(12) . . ? O2 C39 C40 110.6(11) . . ? C38 C39 H39A 109.3 . . ? O2 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? C79 O40 H40 109.5 . . ? O16 C40 C39 113.4(11) . . ? O16 C40 C41 112.9(12) . . ? C39 C40 C41 109.0(12) . . ? O16 C40 H40A 107.1 . . ? C39 C40 H40A 107.1 . . ? C41 C40 H40A 107.1 . . ? C43 O41 H41 109.5 . . ? O30 C41 C42 103.0(13) . . ? O30 C41 C40 109.8(12) . . ? C42 C41 C40 118.0(13) . . ? O30 C41 H41A 108.5 . . ? C42 C41 H41A 108.5 . . ? C40 C41 H41A 108.5 . . ? C49 O42 H42 109.5 . . ? O23 C42 C41 117.0(13) . . ? O23 C42 H42A 108.0 . . ? C41 C42 H42A 108.0 . . ? O23 C42 H42B 108.0 . . ? C41 C42 H42B 108.0 . . ? H42A C42 H42B 107.3 . . ? C54 O43 C50 112.6(10) . . ? O41 C43 C44 113.3(11) . . ? O41 C43 H43A 108.9 . . ? C44 C43 H43A 108.9 . . ? O41 C43 H43B 108.9 . . ? C44 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 O49 103.8(10) . . ? C43 C44 C45 110.3(11) . . ? O49 C44 C45 110.2(11) . . ? C43 C44 H44 110.8 . . ? O49 C44 H44 110.8 . . ? C45 C44 H44 110.8 . . ? C60 O44 C56 111.6(11) . . ? C66 O45 C62 112.4(10) . . ? O56 C45 C44 106.7(10) . . ? O56 C45 C46 100.8(10) . . ? C44 C45 C46 109.4(11) . . ? O56 C45 H45 113.0 . . ? C44 C45 H45 113.0 . . ? C46 C45 H45 113.0 . . ? O69 C46 C47 110.2(12) . . ? O69 C46 C45 108.2(12) . . ? C47 C46 C45 103.9(11) . . ? O69 C46 H46 111.4 . . ? C47 C46 H46 111.4 . . ? C45 C46 H46 111.4 . . ? C72 O46 C68 116.0(10) . . ? C74 O47 C78 117.3(10) . . ? O70 C47 C46 108.7(13) . . ? O70 C47 C48 108.8(13) . . ? C46 C47 C48 107.0(12) . . ? O70 C47 H47 110.7 . . ? C46 C47 H47 110.7 . . ? C48 C47 H47 110.7 . . ? C84 O48 C80 111.8(10) . . ? O50 C48 O49 115.8(12) . . ? O50 C48 C47 109.8(13) . . ? O49 C48 C47 105.5(13) . . ? O50 C48 H48 108.5 . . ? O49 C48 H48 108.5 . . ? C47 C48 H48 108.5 . . ? C44 O49 C48 114.2(10) . . ? O42 C49 C50 107.6(11) . . ? O42 C49 H49A 110.2 . . ? C50 C49 H49A 110.2 . . ? O42 C49 H49B 110.2 . . ? C50 C49 H49B 110.2 . . ? H49A C49 H49B 108.5 . . ? C51 O50 C48 117.2(10) . . ? O43 C50 C49 108.1(11) . . ? O43 C50 C51 110.6(10) . . ? C49 C50 C51 112.8(11) . . ? O43 C50 H50 108.4 . . ? C49 C50 H50 108.4 . . ? C51 C50 H50 108.4 . . ? C54 O51 C57 119.2(11) . . ? O50 C51 C52 108.2(11) . . ? O50 C51 C50 111.4(11) . . ? C52 C51 C50 108.0(11) . . ? O50 C51 H51 109.8 . . ? C52 C51 H51 109.8 . . ? C50 C51 H51 109.8 . . ? C60 O52 C63 118.5(10) . . ? O57 C52 C51 104.9(11) . . ? O57 C52 C53 111.7(12) . . ? C51 C52 C53 110.4(12) . . ? O57 C52 H52 109.9 . . ? C51 C52 H52 109.9 . . ? C53 C52 H52 109.9 . . ? C66 O53 C69 121.9(10) . . ? O58 C53 C52 113.6(13) . . ? O58 C53 C54 112.2(12) . . ? C52 C53 C54 109.7(13) . . ? O58 C53 H53 107.0 . . ? C52 C53 H53 107.0 . . ? C54 C53 H53 107.0 . . ? C75 O54 C72 119.0(9) . . ? O43 C54 O51 115.1(11) . . ? O43 C54 C53 113.4(12) . . ? O51 C54 C53 109.7(12) . . ? O43 C54 H54 106.0 . . ? O51 C54 H54 106.0 . . ? C53 C54 H54 106.0 . . ? C81 O55 C78 114.7(9) . . ? C45 O56 C84 115.8(10) . . ? C55 C56 C57 111.6(14) . . ? C55 C56 O44 107.8(13) . . ? C57 C56 O44 111.8(12) . . ? C55 C56 H56 108.5 . . ? C57 C56 H56 108.5 . . ? O44 C56 H56 108.5 . . ? C52 O57 H57 109.5 . . ? O51 C57 C56 110.7(12) . . ? O51 C57 C58 104.5(12) . . ? C56 C57 C58 109.4(12) . . ? O51 C57 H57A 110.7 . . ? C56 C57 H57A 110.7 . . ? C58 C57 H57A 110.7 . . ? C53 O58 H58 109.5 . . ? C59 C58 O59 108.3(12) . . ? C59 C58 C57 105.2(13) . . ? O59 C58 C57 102.2(10) . . ? C59 C58 H58A 113.4 . . ? O59 C58 H58A 113.4 . . ? C57 C58 H58A 113.4 . . ? C58 O59 H59 109.5 . . ? C58 C59 O60 107.5(14) . . ? C58 C59 C60 112.0(13) . . ? O60 C59 C60 109.1(12) . . ? C58 C59 H59A 109.4 . . ? O60 C59 H59A 109.4 . . ? C60 C59 H59A 109.4 . . ? C59 O60 H60 109.5 . . ? O44 C60 O52 117.5(12) . . ? O44 C60 C59 108.7(12) . . ? O52 C60 C59 106.4(13) . . ? O44 C60 H60A 108.0 . . ? O52 C60 H60A 108.0 . . ? C59 C60 H60A 108.0 . . ? C64 O61 H61 109.5 . . ? O37 C61 C62 106.2(10) . . ? O37 C61 H61A 110.5 . . ? C62 C61 H61A 110.5 . . ? O37 C61 H61B 110.5 . . ? C62 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? O45 C62 C63 108.2(10) . . ? O45 C62 C61 108.1(10) . . ? C63 C62 C61 116.2(11) . . ? O45 C62 H62 108.1 . . ? C63 C62 H62 108.1 . . ? C61 C62 H62 108.1 . . ? C65 O62 H62A 109.5 . . ? C70 O63 H63 109.5 . . ? O52 C63 C64 110.3(10) . . ? O52 C63 C62 106.1(10) . . ? C64 C63 C62 107.7(10) . . ? O52 C63 H63A 110.9 . . ? C64 C63 H63A 110.9 . . ? C62 C63 H63A 110.9 . . ? C71 O64 H64 109.5 . . ? O61 C64 C65 108.5(12) . . ? O61 C64 C63 103.0(11) . . ? C65 C64 C63 113.3(13) . . ? O61 C64 H64A 110.6 . . ? C65 C64 H64A 110.6 . . ? C63 C64 H64A 110.6 . . ? O62 C65 C64 112.8(12) . . ? O62 C65 C66 105.4(11) . . ? C64 C65 C66 105.9(12) . . ? O62 C65 H65 110.9 . . ? C64 C65 H65 110.9 . . ? C66 C65 H65 110.9 . . ? C76 O65 H65A 109.5 . . ? C77 O66 H66 109.5 . . ? O53 C66 O45 111.1(10) . . ? O53 C66 C65 111.5(11) . . ? O45 C66 C65 108.1(11) . . ? O53 C66 H66A 108.7 . . ? O45 C66 H66A 108.7 . . ? C65 C66 H66A 108.7 . . ? C82 O67 H67 109.5 . . ? O38 C67 C68 110.0(11) . . ? O38 C67 H67A 109.7 . . ? C68 C67 H67A 109.7 . . ? O38 C67 H67B 109.7 . . ? C68 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? C83 O68 H68 109.5 . . ? O46 C68 C67 109.6(11) . . ? O46 C68 C69 105.8(11) . . ? C67 C68 C69 118.0(13) . . ? O46 C68 H68A 107.7 . . ? C67 C68 H68A 107.7 . . ? C69 C68 H68A 107.7 . . ? C46 O69 H69 109.5 . . ? C70 C69 C68 117.8(13) . . ? C70 C69 O53 107.4(12) . . ? C68 C69 O53 106.6(11) . . ? C70 C69 H69A 108.3 . . ? C68 C69 H69A 108.3 . . ? O53 C69 H69A 108.3 . . ? C47 O70 H70 109.5 . . ? O63 C70 C69 110.1(12) . . ? O63 C70 C71 103.7(11) . . ? C69 C70 C71 107.4(12) . . ? O63 C70 H70A 111.7 . . ? C69 C70 H70A 111.7 . . ? C71 C70 H70A 111.7 . . ? O64 C71 C72 109.8(12) . . ? O64 C71 C70 113.9(13) . . ? C72 C71 C70 105.2(12) . . ? O64 C71 H71 109.3 . . ? C72 C71 H71 109.3 . . ? C70 C71 H71 109.3 . . ? O46 C72 O54 106.0(10) . . ? O46 C72 C71 114.5(11) . . ? O54 C72 C71 109.4(11) . . ? O46 C72 H72 109.0 . . ? O54 C72 H72 109.0 . . ? C71 C72 H72 109.0 . . ? O39 C73 C74 115.6(11) . . ? O39 C73 H73A 108.4 . . ? C74 C73 H73A 108.4 . . ? O39 C73 H73B 108.4 . . ? C74 C73 H73B 108.4 . . ? H73A C73 H73B 107.4 . . ? O47 C74 C73 104.5(10) . . ? O47 C74 C75 108.9(10) . . ? C73 C74 C75 112.7(10) . . ? O47 C74 H74 110.2 . . ? C73 C74 H74 110.2 . . ? C75 C74 H74 110.2 . . ? O54 C75 C76 110.0(11) . . ? O54 C75 C74 110.0(10) . . ? C76 C75 C74 111.6(10) . . ? O54 C75 H75 108.4 . . ? C76 C75 H75 108.4 . . ? C74 C75 H75 108.4 . . ? O65 C76 C75 110.0(11) . . ? O65 C76 C77 106.8(11) . . ? C75 C76 C77 108.4(12) . . ? O65 C76 H76 110.5 . . ? C75 C76 H76 110.5 . . ? C77 C76 H76 110.5 . . ? O66 C77 C76 111.1(12) . . ? O66 C77 C78 105.9(10) . . ? C76 C77 C78 108.8(11) . . ? O66 C77 H77 110.3 . . ? C76 C77 H77 110.3 . . ? C78 C77 H77 110.3 . . ? O47 C78 O55 107.6(9) . . ? O47 C78 C77 109.5(9) . . ? O55 C78 C77 105.4(10) . . ? O47 C78 H78 111.4 . . ? O55 C78 H78 111.4 . . ? C77 C78 H78 111.4 . . ? O40 C79 C80 110.2(11) . . ? O40 C79 H79A 109.6 . . ? C80 C79 H79A 109.6 . . ? O40 C79 H79B 109.6 . . ? C80 C79 H79B 109.6 . . ? H79A C79 H79B 108.1 . . ? C81 C80 O48 111.6(9) . . ? C81 C80 C79 114.2(11) . . ? O48 C80 C79 103.5(9) . . ? C81 C80 H80 109.1 . . ? O48 C80 H80 109.1 . . ? C79 C80 H80 109.1 . . ? C80 C81 C82 116.4(11) . . ? C80 C81 O55 110.3(10) . . ? C82 C81 O55 101.1(10) . . ? C80 C81 H81 109.6 . . ? C82 C81 H81 109.6 . . ? O55 C81 H81 109.6 . . ? O67 C82 C81 114.8(12) . . ? O67 C82 C83 111.3(11) . . ? C81 C82 C83 105.4(11) . . ? O67 C82 H82 108.4 . . ? C81 C82 H82 108.4 . . ? C83 C82 H82 108.4 . . ? O68 C83 C82 114.6(11) . . ? O68 C83 C84 114.0(10) . . ? C82 C83 C84 112.2(11) . . ? O68 C83 H83 104.9 . . ? C82 C83 H83 104.9 . . ? C84 C83 H83 104.9 . . ? O48 C84 O56 113.6(12) . . ? O48 C84 C83 111.2(11) . . ? O56 C84 C83 101.6(11) . . ? O48 C84 H84 110.1 . . ? O56 C84 H84 110.1 . . ? C83 C84 H84 110.1 . . ? O1A C1A O2A 130.1(12) . . ? O1A C1A C2A 117.9(11) . . ? O2A C1A C2A 112.0(10) . . ? C3A C2A C7A 120.0 . . ? C3A C2A C1A 119.3(10) . . ? C7A C2A C1A 120.6(10) . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3A1 120.0 . . ? C4A C3A H3A1 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A1 120.0 . . ? C5A C4A H4A1 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C7A 120.0 . . ? C5A C6A H6A1 120.0 . . ? C7A C6A H6A1 120.0 . . ? C6A C7A C2A 120.0 . . ? C6A C7A H7A1 120.0 . . ? C2A C7A H7A1 120.0 . . ? C9A C8A C13A 120.0 . . ? C8A C9A C10A 120.0 . . ? C8A C9A H9A1 120.0 . . ? C10A C9A H9A1 120.0 . . ? C11A C10A C9A 120.0 . . ? C11A C10A H10B 120.0 . . ? C9A C10A H10B 120.0 . . ? C12A C11A C10A 120.0 . . ? C12A C11A C14A 120.3(11) . . ? C10A C11A C14A 118.5(11) . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12C 120.0 . . ? C11A C12A H12C 120.0 . . ? C12A C13A C8A 120.0 . . ? C12A C13A H13B 120.0 . . ? C8A C13A H13B 120.0 . . ? O4A C14A O3A 122.6(14) . . ? O4A C14A C11A 115.4(16) . . ? O3A C14A C11A 113.2(17) . . ? O1B C1B O2B 127.1(11) . . ? O1B C1B C2B 116.3(10) . . ? O2B C1B C2B 116.5(10) . . ? C3B C2B C7B 120.0 . . ? C3B C2B C1B 119.4(10) . . ? C7B C2B C1B 120.5(10) . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C5B C6B C7B 120.0 . . ? C5B C6B H6B1 120.0 . . ? C7B C6B H6B1 120.0 . . ? C6B C7B C2B 120.0 . . ? C6B C7B H7B 120.0 . . ? C2B C7B H7B 120.0 . . ? C9B C8B C13B 120.0 . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C11B C10B C9B 120.0 . . ? C11B C10B H10C 120.0 . . ? C9B C10B H10C 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B C14B 118.3(5) . . ? C10B C11B C14B 115.2(5) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12D 120.0 . . ? C13B C12B H12D 120.0 . . ? C12B C13B C8B 120.0 . . ? C12B C13B H13C 120.0 . . ? C8B C13B H13C 120.0 . . ? O3B C14B O4B 123.6(13) . . ? O3B C14B C11B 108.5(14) . . ? O4B C14B C11B 117.1(13) . . ? O39W K3 K1 117.9(5) . 1_655 ? O40W K5 O18W 129.4(11) 1_545 . ? O40W K5 K6 109.8(10) 1_545 1_645 ? O18W K5 K6 112.8(9) . 1_645 ? O27W K9 O28W 111.2(11) 1_545 1_554 ? O26W O23W O25W 151.6(19) . . ? O21W O32W O24W 167(5) . . ? O40W O39W K3 85.7(14) . . ? O39W O40W K5 155(2) . 1_565 ? 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 O16 C1 C2 O3 64.9(16) . . . . ? O31 C1 C2 O3 -175.4(11) . . . . ? O16 C1 C2 C3 -63.8(17) . . . . ? O31 C1 C2 C3 56.0(18) . . . . ? O3 C2 C3 O4 53.3(18) . . . . ? C1 C2 C3 O4 -176.6(13) . . . . ? O3 C2 C3 C4 175.7(12) . . . . ? C1 C2 C3 C4 -54.3(18) . . . . ? O4 C3 C4 O17 -65.7(16) . . . . ? C2 C3 C4 O17 169.8(12) . . . . ? O4 C3 C4 C5 -179.5(13) . . . . ? C2 C3 C4 C5 56.0(18) . . . . ? C3 C4 C5 O31 -56.9(17) . . . . ? O17 C4 C5 O31 -173.5(10) . . . . ? C3 C4 C5 C6 -170.2(14) . . . . ? O17 C4 C5 C6 73.2(15) . . . . ? O31 C5 C6 O24 -62.0(17) . . . . ? C4 C5 C6 O24 51.4(18) . . . . ? O32 C7 C8 O5 -179.7(10) . . . . ? O17 C7 C8 O5 56.3(16) . . . . ? O32 C7 C8 C9 59.7(15) . . . . ? O17 C7 C8 C9 -64.3(15) . . . . ? O5 C8 C9 O6 61.6(15) . . . . ? C7 C8 C9 O6 -174.6(11) . . . . ? O5 C8 C9 C10 -179.1(11) . . . . ? C7 C8 C9 C10 -55.3(15) . . . . ? C8 C9 C10 O18 173.8(12) . . . . ? O6 C9 C10 O18 -63.5(13) . . . . ? C8 C9 C10 C11 52.1(15) . . . . ? O6 C9 C10 C11 174.8(10) . . . . ? O18 C10 C11 O32 -170.4(9) . . . . ? C9 C10 C11 O32 -49.4(13) . . . . ? O18 C10 C11 C12 72.5(13) . . . . ? C9 C10 C11 C12 -166.4(10) . . . . ? O32 C11 C12 O25 -54.2(15) . . . . ? C10 C11 C12 O25 65.6(16) . . . . ? O18 C13 C14 O7 66.1(16) . . . . ? O33 C13 C14 O7 -169.3(11) . . . . ? O18 C13 C14 C15 -63.7(16) . . . . ? O33 C13 C14 C15 60.8(15) . . . . ? O7 C14 C15 O8 49.9(16) . . . . ? C13 C14 C15 O8 179.5(12) . . . . ? O7 C14 C15 C16 174.1(12) . . . . ? C13 C14 C15 C16 -56.4(17) . . . . ? C14 C15 C16 O19 173.6(12) . . . . ? O8 C15 C16 O19 -59.9(14) . . . . ? C14 C15 C16 C17 52.0(15) . . . . ? O8 C15 C16 C17 178.5(10) . . . . ? C2 C1 O16 C40 -113.3(15) . . . . ? O31 C1 O16 C40 124.8(13) . . . . ? O32 C7 O17 C4 107.0(14) . . . . ? C8 C7 O17 C4 -128.8(13) . . . . ? C3 C4 O17 C7 119.7(14) . . . . ? C5 C4 O17 C7 -119.6(13) . . . . ? O19 C16 C17 O33 -176.8(10) . . . . ? C15 C16 C17 O33 -52.8(14) . . . . ? O19 C16 C17 C18 72.0(14) . . . . ? C15 C16 C17 C18 -164.0(11) . . . . ? C14 C13 O18 C10 -116.3(14) . . . . ? O33 C13 O18 C10 119.9(12) . . . . ? C11 C10 O18 C13 -116.8(13) . . . . ? C9 C10 O18 C13 122.4(13) . . . . ? O33 C17 C18 O26 -62.2(13) . . . . ? C16 C17 C18 O26 53.8(14) . . . . ? C15 C16 O19 C19 133.3(13) . . . . ? C17 C16 O19 C19 -104.2(14) . . . . ? C16 O19 C19 O34 115.8(13) . . . . ? C16 O19 C19 C20 -117.0(12) . . . . ? O34 C19 C20 O9 177.2(11) . . . . ? O19 C19 C20 O9 51.4(15) . . . . ? O34 C19 C20 C21 52.9(15) . . . . ? O19 C19 C20 C21 -73.0(14) . . . . ? O9 C20 C21 O10 60.5(16) . . . . ? C19 C20 C21 O10 -171.5(12) . . . . ? O9 C20 C21 C22 -176.8(11) . . . . ? C19 C20 C21 C22 -48.7(15) . . . . ? C25 O20 C22 C23 -117.8(13) . . . . ? C25 O20 C22 C21 121.2(12) . . . . ? O10 C21 C22 O20 -63.0(13) . . . . ? C20 C21 C22 O20 174.3(10) . . . . ? O10 C21 C22 C23 175.0(10) . . . . ? C20 C21 C22 C23 52.3(14) . . . . ? O20 C22 C23 O34 -171.9(10) . . . . ? C21 C22 C23 O34 -54.3(15) . . . . ? O20 C22 C23 C24 68.2(15) . . . . ? C21 C22 C23 C24 -174.2(11) . . . . ? O34 C23 C24 O27 -63.0(14) . . . . ? C22 C23 C24 O27 61.0(15) . . . . ? C22 O20 C25 O35 112.1(12) . . . . ? C22 O20 C25 C26 -135.7(11) . . . . ? O20 C25 C26 O11 68.7(13) . . . . ? O35 C25 C26 O11 -175.2(10) . . . . ? O20 C25 C26 C27 -60.0(14) . . . . ? O35 C25 C26 C27 56.2(14) . . . . ? O11 C26 C27 O12 59.9(14) . . . . ? C25 C26 C27 O12 -178.5(10) . . . . ? O11 C26 C27 C28 178.7(11) . . . . ? C25 C26 C27 C28 -59.6(14) . . . . ? C31 O21 C28 C27 133.8(11) . . . . ? C31 O21 C28 C29 -106.9(12) . . . . ? O12 C27 C28 O21 -68.0(13) . . . . ? C26 C27 C28 O21 173.7(10) . . . . ? O12 C27 C28 C29 176.1(10) . . . . ? C26 C27 C28 C29 57.7(15) . . . . ? O21 C28 C29 C30 69.7(15) . . . . ? C27 C28 C29 C30 -174.8(12) . . . . ? O21 C28 C29 O35 -170.8(9) . . . . ? C27 C28 C29 O35 -55.3(14) . . . . ? O35 C29 C30 O28 -67.1(14) . . . . ? C28 C29 C30 O28 53.5(16) . . . . ? C2 C1 O31 C5 -58.8(15) . . . . ? O16 C1 O31 C5 60.0(16) . . . . ? C6 C5 O31 C1 173.6(12) . . . . ? C4 C5 O31 C1 55.9(15) . . . . ? C28 O21 C31 O29 117.0(12) . . . . ? C28 O21 C31 C32 -126.2(11) . . . . ? C35 O29 C31 O21 54.4(13) . . . . ? C35 O29 C31 C32 -65.2(11) . . . . ? O17 C7 O32 C11 60.7(15) . . . . ? C8 C7 O32 C11 -61.4(14) . . . . ? C10 C11 O32 C7 56.2(13) . . . . ? C12 C11 O32 C7 175.3(10) . . . . ? O21 C31 C32 O13 59.9(12) . . . . ? O29 C31 C32 O13 -180.0(9) . . . . ? O21 C31 C32 C33 -57.0(14) . . . . ? O29 C31 C32 C33 63.1(13) . . . . ? C18 C17 O33 C13 175.3(10) . . . . ? C16 C17 O33 C13 57.8(14) . . . . ? O18 C13 O33 C17 61.7(14) . . . . ? C14 C13 O33 C17 -62.7(14) . . . . ? O13 C32 C33 O14 65.9(14) . . . . ? C31 C32 C33 O14 179.2(11) . . . . ? O13 C32 C33 C34 -172.8(10) . . . . ? C31 C32 C33 C34 -59.4(14) . . . . ? O19 C19 O34 C23 63.9(14) . . . . ? C20 C19 O34 C23 -57.7(15) . . . . ? C22 C23 O34 C19 57.5(15) . . . . ? C24 C23 O34 C19 -177.1(11) . . . . ? C37 O15 C34 C35 -123.6(11) . . . . ? C37 O15 C34 C33 118.2(12) . . . . ? O14 C33 C34 O15 -69.3(13) . . . . ? C32 C33 C34 O15 169.1(10) . . . . ? O14 C33 C34 C35 178.2(10) . . . . ? C32 C33 C34 C35 56.6(14) . . . . ? O20 C25 O35 C29 58.7(14) . . . . ? C26 C25 O35 C29 -54.5(13) . . . . ? C30 C29 O35 C25 -179.4(11) . . . . ? C28 C29 O35 C25 56.6(14) . . . . ? C31 O29 C35 C36 -175.3(10) . . . . ? C31 O29 C35 C34 61.4(12) . . . . ? O15 C34 C35 C36 75.1(13) . . . . ? C33 C34 C35 C36 -171.2(11) . . . . ? O15 C34 C35 O29 -167.8(8) . . . . ? C33 C34 C35 O29 -54.1(13) . . . . ? O29 C35 C36 O22 -65.9(12) . . . . ? C34 C35 C36 O22 51.9(14) . . . . ? C41 O30 C37 O15 61.9(13) . . . . ? C41 O30 C37 C38 -60.1(14) . . . . ? C34 O15 C37 O30 104.9(12) . . . . ? C34 O15 C37 C38 -132.5(11) . . . . ? O30 C37 C38 C39 57.6(15) . . . . ? O15 C37 C38 C39 -65.4(15) . . . . ? O30 C37 C38 O1 -178.1(9) . . . . ? O15 C37 C38 O1 58.9(13) . . . . ? O1 C38 C39 O2 64.7(15) . . . . ? C37 C38 C39 O2 -176.7(11) . . . . ? O1 C38 C39 C40 -174.4(12) . . . . ? C37 C38 C39 C40 -55.7(16) . . . . ? C1 O16 C40 C39 126.9(14) . . . . ? C1 O16 C40 C41 -108.5(15) . . . . ? C38 C39 C40 O16 -177.9(12) . . . . ? O2 C39 C40 O16 -59.4(15) . . . . ? C38 C39 C40 C41 55.4(16) . . . . ? O2 C39 C40 C41 173.9(11) . . . . ? C37 O30 C41 C42 -173.4(11) . . . . ? C37 O30 C41 C40 60.0(14) . . . . ? O16 C40 C41 O30 176.7(11) . . . . ? C39 C40 C41 O30 -56.3(15) . . . . ? O16 C40 C41 C42 59.2(18) . . . . ? C39 C40 C41 C42 -173.9(13) . . . . ? O30 C41 C42 O23 -63.5(17) . . . . ? C40 C41 C42 O23 57.7(19) . . . . ? O41 C43 C44 O49 -59.9(14) . . . . ? O41 C43 C44 C45 58.2(14) . . . . ? C43 C44 C45 O56 82.7(12) . . . . ? O49 C44 C45 O56 -163.3(9) . . . . ? C43 C44 C45 C46 -169.1(10) . . . . ? O49 C44 C45 C46 -55.1(13) . . . . ? O56 C45 C46 O69 -70.8(12) . . . . ? C44 C45 C46 O69 177.0(10) . . . . ? O56 C45 C46 C47 172.1(11) . . . . ? C44 C45 C46 C47 59.9(14) . . . . ? O69 C46 C47 O70 60.7(16) . . . . ? C45 C46 C47 O70 176.3(12) . . . . ? O69 C46 C47 C48 178.0(12) . . . . ? C45 C46 C47 C48 -66.3(15) . . . . ? O70 C47 C48 O50 60.5(14) . . . . ? C46 C47 C48 O50 -56.8(16) . . . . ? O70 C47 C48 O49 -174.0(9) . . . . ? C46 C47 C48 O49 68.7(14) . . . . ? C43 C44 O49 C48 177.3(11) . . . . ? C45 C44 O49 C48 59.2(14) . . . . ? O50 C48 O49 C44 57.3(16) . . . . ? C47 C48 O49 C44 -64.4(13) . . . . ? O49 C48 O50 C51 120.7(14) . . . . ? C47 C48 O50 C51 -120.0(13) . . . . ? C54 O43 C50 C49 -177.7(10) . . . . ? C54 O43 C50 C51 58.4(13) . . . . ? O42 C49 C50 O43 -72.4(14) . . . . ? O42 C49 C50 C51 50.2(14) . . . . ? C48 O50 C51 C52 129.0(12) . . . . ? C48 O50 C51 C50 -112.5(13) . . . . ? O43 C50 C51 O50 -175.3(9) . . . . ? C49 C50 C51 O50 63.5(14) . . . . ? O43 C50 C51 C52 -56.6(13) . . . . ? C49 C50 C51 C52 -177.8(11) . . . . ? O50 C51 C52 O57 -63.6(13) . . . . ? C50 C51 C52 O57 175.8(10) . . . . ? O50 C51 C52 C53 175.9(11) . . . . ? C50 C51 C52 C53 55.3(14) . . . . ? O57 C52 C53 O58 62.2(16) . . . . ? C51 C52 C53 O58 178.6(12) . . . . ? O57 C52 C53 C54 -171.3(12) . . . . ? C51 C52 C53 C54 -55.0(16) . . . . ? C50 O43 C54 O51 68.8(15) . . . . ? C50 O43 C54 C53 -58.7(15) . . . . ? C57 O51 C54 O43 104.4(14) . . . . ? C57 O51 C54 C53 -126.3(13) . . . . ? O58 C53 C54 O43 -177.0(11) . . . . ? C52 C53 C54 O43 55.8(16) . . . . ? O58 C53 C54 O51 52.8(16) . . . . ? C52 C53 C54 O51 -74.4(15) . . . . ? C44 C45 O56 C84 -109.6(12) . . . . ? C46 C45 O56 C84 136.2(12) . . . . ? O36 C55 C56 C57 64(3) . . . . ? O36' C55 C56 C57 172.8(15) . . . . ? O36 C55 C56 O44 -60(2) . . . . ? O36' C55 C56 O44 50(2) . . . . ? C60 O44 C56 C55 -178.3(13) . . . . ? C60 O44 C56 C57 58.7(16) . . . . ? C54 O51 C57 C56 -127.3(13) . . . . ? C54 O51 C57 C58 115.0(12) . . . . ? C55 C56 C57 O51 74.3(18) . . . . ? O44 C56 C57 O51 -164.8(11) . . . . ? C55 C56 C57 C58 -171.0(13) . . . . ? O44 C56 C57 C58 -50.2(16) . . . . ? O51 C57 C58 C59 171.5(11) . . . . ? C56 C57 C58 C59 52.9(16) . . . . ? O51 C57 C58 O59 -75.4(12) . . . . ? C56 C57 C58 O59 166.0(12) . . . . ? O59 C58 C59 O60 71.4(15) . . . . ? C57 C58 C59 O60 -179.9(11) . . . . ? O59 C58 C59 C60 -168.7(12) . . . . ? C57 C58 C59 C60 -60.0(16) . . . . ? C56 O44 C60 O52 58.1(16) . . . . ? C56 O44 C60 C59 -62.6(14) . . . . ? C63 O52 C60 O44 110.5(14) . . . . ? C63 O52 C60 C59 -127.6(12) . . . . ? C58 C59 C60 O44 69.5(17) . . . . ? O60 C59 C60 O44 -171.5(12) . . . . ? C58 C59 C60 O52 -57.9(17) . . . . ? O60 C59 C60 O52 61.0(15) . . . . ? C66 O45 C62 C63 59.0(13) . . . . ? C66 O45 C62 C61 -174.5(10) . . . . ? O37 C61 C62 O45 -62.6(13) . . . . ? O37 C61 C62 C63 59.1(14) . . . . ? C60 O52 C63 C64 136.5(12) . . . . ? C60 O52 C63 C62 -107.1(13) . . . . ? O45 C62 C63 O52 -171.9(9) . . . . ? C61 C62 C63 O52 66.4(13) . . . . ? O45 C62 C63 C64 -53.8(13) . . . . ? C61 C62 C63 C64 -175.4(11) . . . . ? O52 C63 C64 O61 -67.7(12) . . . . ? C62 C63 C64 O61 176.9(10) . . . . ? O52 C63 C64 C65 175.2(11) . . . . ? C62 C63 C64 C65 59.8(14) . . . . ? O61 C64 C65 O62 67.9(15) . . . . ? C63 C64 C65 O62 -178.4(11) . . . . ? O61 C64 C65 C66 -177.3(11) . . . . ? C63 C64 C65 C66 -63.6(15) . . . . ? C69 O53 C66 O45 107.5(13) . . . . ? C69 O53 C66 C65 -131.9(13) . . . . ? C62 O45 C66 O53 58.7(14) . . . . ? C62 O45 C66 C65 -63.9(12) . . . . ? O62 C65 C66 O53 60.0(14) . . . . ? C64 C65 C66 O53 -59.7(15) . . . . ? O62 C65 C66 O45 -177.6(9) . . . . ? C64 C65 C66 O45 62.6(13) . . . . ? C72 O46 C68 C67 -179.4(11) . . . . ? C72 O46 C68 C69 52.5(13) . . . . ? O38 C67 C68 O46 -63.1(14) . . . . ? O38 C67 C68 C69 57.9(16) . . . . ? O46 C68 C69 C70 -58.1(15) . . . . ? C67 C68 C69 C70 178.9(12) . . . . ? O46 C68 C69 O53 -178.7(9) . . . . ? C67 C68 C69 O53 58.4(15) . . . . ? C66 O53 C69 C70 124.6(13) . . . . ? C66 O53 C69 C68 -108.4(13) . . . . ? C68 C69 C70 O63 173.8(11) . . . . ? O53 C69 C70 O63 -66.0(14) . . . . ? C68 C69 C70 C71 61.5(16) . . . . ? O53 C69 C70 C71 -178.3(10) . . . . ? O63 C70 C71 O64 69.9(15) . . . . ? C69 C70 C71 O64 -173.5(13) . . . . ? O63 C70 C71 C72 -169.8(11) . . . . ? C69 C70 C71 C72 -53.2(15) . . . . ? C68 O46 C72 O54 64.2(13) . . . . ? C68 O46 C72 C71 -56.5(14) . . . . ? C75 O54 C72 O46 108.3(12) . . . . ? C75 O54 C72 C71 -127.8(12) . . . . ? O64 C71 C72 O46 176.3(11) . . . . ? C70 C71 C72 O46 53.3(14) . . . . ? O64 C71 C72 O54 57.6(15) . . . . ? C70 C71 C72 O54 -65.4(14) . . . . ? C78 O47 C74 C73 176.7(9) . . . . ? C78 O47 C74 C75 56.0(12) . . . . ? O39 C73 C74 O47 -63.8(14) . . . . ? O39 C73 C74 C75 54.3(15) . . . . ? C72 O54 C75 C76 120.5(12) . . . . ? C72 O54 C75 C74 -116.2(12) . . . . ? O47 C74 C75 O54 -178.6(9) . . . . ? C73 C74 C75 O54 65.9(13) . . . . ? O47 C74 C75 C76 -56.2(13) . . . . ? C73 C74 C75 C76 -171.7(11) . . . . ? O54 C75 C76 O65 -61.8(14) . . . . ? C74 C75 C76 O65 175.8(10) . . . . ? O54 C75 C76 C77 -178.3(10) . . . . ? C74 C75 C76 C77 59.3(14) . . . . ? O65 C76 C77 O66 67.4(14) . . . . ? C75 C76 C77 O66 -174.0(10) . . . . ? O65 C76 C77 C78 -176.3(10) . . . . ? C75 C76 C77 C78 -57.8(14) . . . . ? C74 O47 C78 O55 57.6(12) . . . . ? C74 O47 C78 C77 -56.4(12) . . . . ? C81 O55 C78 O47 114.0(11) . . . . ? C81 O55 C78 C77 -129.3(10) . . . . ? O66 C77 C78 O47 174.4(10) . . . . ? C76 C77 C78 O47 54.9(13) . . . . ? O66 C77 C78 O55 59.0(12) . . . . ? C76 C77 C78 O55 -60.5(13) . . . . ? C84 O48 C80 C81 58.9(14) . . . . ? C84 O48 C80 C79 -177.9(11) . . . . ? O40 C79 C80 C81 51.8(14) . . . . ? O40 C79 C80 O48 -69.7(12) . . . . ? O48 C80 C81 C82 -58.3(15) . . . . ? C79 C80 C81 C82 -175.3(11) . . . . ? O48 C80 C81 O55 -172.7(8) . . . . ? C79 C80 C81 O55 70.3(13) . . . . ? C78 O55 C81 C80 -101.0(11) . . . . ? C78 O55 C81 C82 135.3(10) . . . . ? C80 C81 C82 O67 175.5(11) . . . . ? O55 C81 C82 O67 -65.0(13) . . . . ? C80 C81 C82 C83 52.7(15) . . . . ? O55 C81 C82 C83 172.2(10) . . . . ? O67 C82 C83 O68 54.6(16) . . . . ? C81 C82 C83 O68 179.6(11) . . . . ? O67 C82 C83 C84 -173.3(11) . . . . ? C81 C82 C83 C84 -48.3(15) . . . . ? C80 O48 C84 O56 57.1(14) . . . . ? C80 O48 C84 C83 -56.7(14) . . . . ? C45 O56 C84 O48 118.7(12) . . . . ? C45 O56 C84 C83 -121.7(11) . . . . ? O68 C83 C84 O48 -173.4(10) . . . . ? C82 C83 C84 O48 54.2(16) . . . . ? O68 C83 C84 O56 65.4(13) . . . . ? C82 C83 C84 O56 -67.0(14) . . . . ? O1A C1A C2A C3A 4.5(19) . . . . ? O2A C1A C2A C3A -177.6(10) . . . . ? O1A C1A C2A C7A -171.7(11) . . . . ? O2A C1A C2A C7A 6.2(18) . . . . ? C7A C2A C3A C4A 0.0 . . . . ? C1A C2A C3A C4A -176.2(12) . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C7A 0.0 . . . . ? C5A C6A C7A C2A 0.0 . . . . ? C3A C2A C7A C6A 0.0 . . . . ? C1A C2A C7A C6A 176.1(12) . . . . ? C13A C8A C9A C10A 0.0 . . . . ? C8A C9A C10A C11A 0.0 . . . . ? C9A C10A C11A C12A 0.0 . . . . ? C9A C10A C11A C14A -167.6(12) . . . . ? C10A C11A C12A C13A 0.0 . . . . ? C14A C11A C12A C13A 167.3(12) . . . . ? C11A C12A C13A C8A 0.0 . . . . ? C9A C8A C13A C12A 0.0 . . . . ? C12A C11A C14A O4A -158.0(13) . . . . ? C10A C11A C14A O4A 10(2) . . . . ? C12A C11A C14A O3A -10(2) . . . . ? C10A C11A C14A O3A 158.0(15) . . . . ? O1B C1B C2B C3B 10.2(19) . . . . ? O2B C1B C2B C3B -172.7(11) . . . . ? O1B C1B C2B C7B -174.2(11) . . . . ? O2B C1B C2B C7B 2.8(19) . . . . ? C7B C2B C3B C4B 0.0 . . . . ? C1B C2B C3B C4B 175.6(12) . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C7B 0.0 . . . . ? C5B C6B C7B C2B 0.0 . . . . ? C3B C2B C7B C6B 0.0 . . . . ? C1B C2B C7B C6B -175.5(12) . . . . ? C13B C8B C9B C10B 0.0 . . . . ? C8B C9B C10B C11B 0.0 . . . . ? C9B C10B C11B C12B 0.0 . . . . ? C9B C10B C11B C14B 151.2(10) . . . . ? C10B C11B C12B C13B 0.0 . . . . ? C14B C11B C12B C13B -150.3(11) . . . . ? C11B C12B C13B C8B 0.0 . . . . ? C9B C8B C13B C12B 0.0 . . . . ? C12B C11B C14B O3B -52.0(17) . . . . ? C10B C11B C14B O3B 156.3(14) . . . . ? C12B C11B C14B O4B 162.3(14) . . . . ? C10B C11B C14B O4B 10.6(19) . . . . ? K1 K3 O39W O40W -37.3(16) 1_655 . . . ? K3 O39W O40W K5 40(5) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.169 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.124 # ======================================================================= _vrf_PLAT201_compound-2 ; RESPONSE: All non-hydrogen atoms of the guest molecules, water molecules of crystallisation and one cyclodextrin have been refined by assuming an isotropic displacement behaviour. ; _vrf_PLAT202_compound-2 ; RESPONSE: All non-hydrogen atoms of the water molecules of crystallisation have been refined by assuming an isotropic displacement behaviour. ; _vrf_PLAT306_compound-2 ; RESPONSE: As explained in the main text, all water molecules of crystallisation have been included in the structural model without the corresponsing hydrogen atoms, hence the alerts for isolated O atoms and hydrogen bonds without the involved H atom. ; _vrf_PLAT410_compound-2 ; RESPONSE: Due to the poor quality of the crystal data set, the location of the carbon and oxygen atoms of the main molecular units of the compound (i.e., cyclodextrins) are affected by a significant crystallographic error. Thus, the geometrical placement of the attached hydrogen atoms (using appropriate HFIX instructions in SHELX) leads to short distances between C-H bonds, hence the alert. This structural limitation can not be overcome with the available data sets. ; _vrf_PLAT414_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT410_compound-2 ; _vrf_PLAT415_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT410_compound-2 ; _vrf_PLAT416_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT410_compound-2 ; _vrf_PLAT417_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT410_compound-2 ; _vrf_PLAT430_compound-2 ; RESPONSE: These short distances correspond to partially occupied oxygen atoms of water molecules of crystallisation. All these short contacts correspond to pairs of entities with total site occupancy of <= 1. The short interactions involving O5 may arise from the high uncertainty of the atomic positions in the structural model. ; _vrf_PLAT242_compound-2 ; RESPONSE: The crystal sructure is significantly affected by thermal disorder, in particular the guest molecules. Therefore, within the crystal contents, there is a wide dispersion of Ueq for C and O (and, consequently, H because all of these atoms have been refined by assuming a riding behaviour on their parent atoms). ; _vrf_PLAT340_compound-2 ; RESPONSE: The crystals available for data collection were of poor quality and, therefore, the crystallographic data set is only of medium quality. As a consequence, the location of the heaviest atoms (e.g., C and O) reflects this higher uncertainty. ; _vrf_PLAT360_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-2. ; _vrf_PLAT361_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-2. ; _vrf_PLAT311_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT306_compound-2. ; _vrf_PLAT369_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT340_compound-2. ; _vrf_PLAT420_compound-2 ; RESPONSE: This alert arises from a number of terminal -OH groups which are not involved in hydrogen bonds. This feature may be a natural consequence of the unusual crystal packing of cyclodextrins (which leads to a smaller number of yhydrogen bonding interactions), or to the lack of additional water molecules to establish the full hydrogen bonding connectivities. Because of the poor quality of the crystal, the latter assumption can not be discarded. ; _vrf_CHEMW03_compound-2 ; RESPONSE: As explained in the main text, the hydrogen atoms associated with the water molecules of crystallisation were not inlcuded in the structural model (either in calculated positions oir from preliminary locations visible from difference Fourier maps). However, the corresponding H atoms have been included in the empirical formula, hence the alert. ; _vrf_PLAT041_compound-2 ; RESPONSE: Please see our response to _vrf_CHEMW03_compound-2. ; _vrf_PLAT043_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-2. ; _vrf_PLAT044_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-2. ; _vrf_PLAT068_compound-2 ; RESPONSE: Please see our response to _vrf_PLAT041_compound-2. ; # ======================================================================= data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 796035' #TrackingRef 'NJ-ART-10-2010-000796-Compound-2.cif' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '17 February 2010' # ======================================================================= #============================================================================== # GENERAL AND CHEMICAL DATA #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C210 H412 K6 O206' _chemical_formula_weight 6468.00 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # CRYSTAL DATA #============================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 18.915(12) _cell_length_b 24.271(16) _cell_length_c 33.344(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.883(16) _cell_angle_gamma 90.00 _cell_volume 15080(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1067 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 17.52 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6868 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9917 _exptl_absorpt_correction_T_max 0.9979 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1998) ; #============================================================================== # EXPERIMENTAL DATA #============================================================================== _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 X8 Kappa CCD APEX II' _diffrn_measurement_method '/w / /f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 35747 _diffrn_reflns_av_R_equivalents 0.2620 _diffrn_reflns_av_sigmaI/netI 0.6786 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.35 _reflns_number_total 20478 _reflns_number_gt 4461 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT+ (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' #============================================================================== # REFINEMENT DATA #============================================================================== _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^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.3(2) _refine_ls_number_reflns 20478 _refine_ls_number_parameters 700 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.4596 _refine_ls_R_factor_gt 0.1566 _refine_ls_wR_factor_ref 0.3805 _refine_ls_wR_factor_gt 0.2844 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #============================================================================== # 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O100 O 0.7567(7) 0.2575(7) 0.9299(4) 0.0391(7) Uiso 1 1 d . . . H100 H 0.7481 0.2756 0.9500 0.059 Uiso 1 1 calc R . . O101 O 0.7779(7) 0.3752(7) 0.9343(4) 0.0391(7) Uiso 1 1 d . . . H101 H 0.7540 0.3875 0.9514 0.059 Uiso 1 1 calc R . . O102 O 0.7881(7) 0.4883(7) 0.9323(4) 0.0391(7) Uiso 1 1 d . . . H102 H 0.7902 0.4554 0.9247 0.059 Uiso 1 1 calc R . . O103 O 0.6893(7) 0.5740(7) 0.9443(4) 0.0391(7) Uiso 1 1 d . . . H103 H 0.7130 0.6013 0.9384 0.059 Uiso 1 1 calc R . . O104 O 0.5917(7) 0.6582(7) 0.9505(4) 0.0391(7) Uiso 1 1 d . . . H104 H 0.6281 0.6472 0.9415 0.059 Uiso 1 1 calc R . . O105 O 0.4500(7) 0.6523(7) 0.9662(4) 0.0391(7) Uiso 1 1 d . . . H105 H 0.4431 0.6274 0.9826 0.059 Uiso 1 1 calc R . . O106 O 0.3033(7) 0.6305(7) 0.9773(4) 0.0391(7) Uiso 1 1 d . . . H106 H 0.2791 0.6353 0.9959 0.059 Uiso 1 1 calc R . . O107 O 0.2248(7) 0.5338(7) 0.9847(4) 0.0391(7) Uiso 1 1 d . . . H107 H 0.1940 0.5086 0.9806 0.059 Uiso 1 1 calc R . . O108 O 0.1538(7) 0.4371(7) 0.9865(4) 0.0391(7) Uiso 1 1 d . . . H108 H 0.1337 0.4219 1.0043 0.059 Uiso 1 1 calc R . . O109 O 0.2026(7) 0.3271(7) 0.9867(4) 0.0391(7) Uiso 1 1 d . . . H109 H 0.1659 0.3300 0.9975 0.059 Uiso 1 1 calc R . . O110 O 0.2514(7) 0.2228(7) 0.9827(4) 0.0391(7) Uiso 1 1 d . . . H110 H 0.2239 0.2044 0.9948 0.059 Uiso 1 1 calc R . . O111 O 0.3834(7) 0.1788(7) 0.9720(4) 0.0391(7) Uiso 1 1 d . . . H111 H 0.4084 0.1542 0.9635 0.059 Uiso 1 1 calc R . . O112 O 0.5057(7) 0.1373(7) 0.9543(4) 0.0391(7) Uiso 1 1 d . . . H112 H 0.5212 0.1619 0.9712 0.059 Uiso 1 1 calc R . . O113 O 0.6321(7) 0.2013(7) 0.9482(4) 0.0391(7) Uiso 1 1 d . . . H113 H 0.6180 0.2046 0.9706 0.059 Uiso 1 1 calc R . . O114 O 0.6274(7) 0.2632(7) 0.8753(4) 0.0391(7) Uiso 1 1 d . . . O115 O 0.6889(7) 0.4347(8) 0.8702(4) 0.0391(7) Uiso 1 1 d . . . O116 O 0.5648(8) 0.5871(7) 0.8831(4) 0.0391(7) Uiso 1 1 d . . . O117 O 0.3495(8) 0.5982(7) 0.9042(4) 0.0391(7) Uiso 1 1 d . . . O118 O 0.1992(8) 0.4677(8) 0.9142(4) 0.0391(7) Uiso 1 1 d . . . O119 O 0.2343(7) 0.2870(7) 0.9140(4) 0.0391(7) Uiso 1 1 d . . . O120 O 0.4195(7) 0.1948(7) 0.8897(4) 0.0391(7) Uiso 1 1 d . . . O121 O 0.6881(7) 0.2984(7) 0.8261(4) 0.0391(7) Uiso 1 1 d . . . O122 O 0.7333(7) 0.3741(7) 0.7769(4) 0.0391(7) Uiso 1 1 d D . . H900 H 0.7604 0.3540 0.7933 0.059 Uiso 1 1 calc R . . O123 O 0.6890(8) 0.5111(7) 0.8286(4) 0.0391(7) Uiso 1 1 d . . . O124 O 0.6298(7) 0.6116(7) 0.7932(4) 0.0391(7) Uiso 1 1 d D . . H124 H 0.6286 0.6341 0.8122 0.059 Uiso 1 1 calc R . . O125 O 0.4863(8) 0.6470(7) 0.8486(4) 0.0391(7) Uiso 1 1 d . . . O126 O 0.3416(7) 0.6901(7) 0.8243(4) 0.0391(7) Uiso 1 1 d D . . H901 H 0.3747 0.7078 0.8387 0.059 Uiso 1 1 calc R . . O127 O 0.2294(7) 0.6016(7) 0.8713(4) 0.0391(7) Uiso 1 1 d . . . O128 O 0.1000(7) 0.5533(7) 0.8350(4) 0.0391(7) Uiso 1 1 d D . . H902 H 0.0940 0.5804 0.8191 0.059 Uiso 1 1 calc R . . O129 O 0.1166(7) 0.4066(7) 0.8776(4) 0.0391(7) Uiso 1 1 d . . . O130 O 0.0832(7) 0.3064(7) 0.8373(4) 0.0391(7) Uiso 1 1 d D . . H130 H 0.0679 0.3201 0.8573 0.059 Uiso 1 1 calc R . . O131 O 0.2221(7) 0.2082(7) 0.8728(4) 0.0391(7) Uiso 1 1 d . . . O132 O 0.2757(7) 0.1237(7) 0.8280(4) 0.0391(7) Uiso 1 1 d D . . H903 H 0.2484 0.1217 0.8453 0.059 Uiso 1 1 calc R . . O133 O 0.4849(7) 0.1576(7) 0.8446(4) 0.0391(7) Uiso 1 1 d . . . O134 O 0.5976(7) 0.1578(7) 0.7965(4) 0.0391(7) Uiso 1 1 d D . . H904 H 0.6082 0.1429 0.8195 0.059 Uiso 1 1 calc R . . C100 C 0.6666(9) 0.3793(10) 0.7896(5) 0.0337(8) Uiso 1 1 d D . . H10A H 0.6297 0.3606 0.7695 0.040 Uiso 1 1 calc R . . H10B H 0.6538 0.4189 0.7897 0.040 Uiso 1 1 calc R . . C101 C 0.6649(11) 0.3555(10) 0.8314(5) 0.0337(8) Uiso 1 1 d D . . H10C H 0.6157 0.3570 0.8386 0.040 Uiso 1 1 calc R . . C102 C 0.7205(12) 0.3805(10) 0.8641(6) 0.0337(8) Uiso 1 1 d . . . H10X H 0.7671 0.3850 0.8542 0.040 Uiso 1 1 calc R . . C103 C 0.7305(11) 0.3496(10) 0.9014(6) 0.0337(8) Uiso 1 1 d . . . H10D H 0.6824 0.3497 0.9100 0.040 Uiso 1 1 calc R . . C104 C 0.7483(11) 0.2897(10) 0.8974(6) 0.0337(8) Uiso 1 1 d . . . H10E H 0.7955 0.2892 0.8878 0.040 Uiso 1 1 calc R . . C105 C 0.6958(11) 0.2655(10) 0.8632(6) 0.0337(8) Uiso 1 1 d . . . H10F H 0.7114 0.2273 0.8574 0.040 Uiso 1 1 calc R . . C106 C 0.5897(10) 0.5646(8) 0.7992(5) 0.0337(8) Uiso 1 1 d D . . H10G H 0.5848 0.5414 0.7745 0.040 Uiso 1 1 calc R . . H10H H 0.5409 0.5764 0.8025 0.040 Uiso 1 1 calc R . . C107 C 0.6217(11) 0.5295(10) 0.8361(5) 0.0337(8) Uiso 1 1 d D . . H10I H 0.5896 0.4981 0.8403 0.040 Uiso 1 1 calc R . . C108 C 0.6321(11) 0.5710(10) 0.8732(5) 0.0337(8) Uiso 1 1 d . . . H10J H 0.6599 0.6041 0.8671 0.040 Uiso 1 1 calc R . . C109 C 0.6761(11) 0.5371(11) 0.9100(6) 0.0337(8) Uiso 1 1 d . . . H10K H 0.6484 0.5041 0.9164 0.040 Uiso 1 1 calc R . . C110 C 0.7430(11) 0.5212(10) 0.8990(6) 0.0337(8) Uiso 1 1 d . . . H11A H 0.7699 0.5545 0.8925 0.040 Uiso 1 1 calc R . . C111 C 0.7277(12) 0.4804(10) 0.8594(6) 0.0337(8) Uiso 1 1 d . . . H11B H 0.7740 0.4680 0.8517 0.040 Uiso 1 1 calc R . . C112 C 0.3649(10) 0.6369(8) 0.8183(5) 0.0337(8) Uiso 1 1 d D . . H11C H 0.3849 0.6360 0.7927 0.040 Uiso 1 1 calc R . . H11D H 0.3232 0.6117 0.8150 0.040 Uiso 1 1 calc R . . C113 C 0.4227(10) 0.6158(10) 0.8537(5) 0.0337(8) Uiso 1 1 d D . . H11E H 0.4305 0.5752 0.8520 0.040 Uiso 1 1 calc R . . C114 C 0.4061(11) 0.6334(10) 0.8962(6) 0.0337(8) Uiso 1 1 d . . . H114 H 0.3895 0.6726 0.8951 0.040 Uiso 1 1 calc R . . C115 C 0.4660(11) 0.6269(10) 0.9283(6) 0.0337(8) Uiso 1 1 d . . . H115 H 0.4779 0.5870 0.9328 0.040 Uiso 1 1 calc R . . C116 C 0.5317(11) 0.6588(10) 0.9186(5) 0.0337(8) Uiso 1 1 d . . . H116 H 0.5158 0.6981 0.9170 0.040 Uiso 1 1 calc R . . C117 C 0.5451(11) 0.6471(10) 0.8797(6) 0.0337(8) Uiso 1 1 d . . . H117 H 0.5852 0.6701 0.8727 0.040 Uiso 1 1 calc R . . C118 C 0.1677(8) 0.5298(9) 0.8342(5) 0.0337(8) Uiso 1 1 d D . . H11F H 0.1867 0.5435 0.8102 0.040 Uiso 1 1 calc R . . H11G H 0.1632 0.4892 0.8320 0.040 Uiso 1 1 calc R . . C119 C 0.2191(11) 0.5449(11) 0.8730(5) 0.0337(8) Uiso 1 1 d D . . H119 H 0.2662 0.5274 0.8708 0.040 Uiso 1 1 calc R . . C120 C 0.1976(12) 0.5226(10) 0.9116(6) 0.0337(8) Uiso 1 1 d . . . H120 H 0.1478 0.5354 0.9128 0.040 Uiso 1 1 calc R . . C121 C 0.2487(11) 0.5458(10) 0.9487(6) 0.0337(8) Uiso 1 1 d . . . H121 H 0.2964 0.5276 0.9498 0.040 Uiso 1 1 calc R . . C122 C 0.2589(12) 0.6076(10) 0.9427(6) 0.0337(8) Uiso 1 1 d . . . H122 H 0.2105 0.6247 0.9416 0.040 Uiso 1 1 calc R . . C123 C 0.2814(11) 0.6220(10) 0.9066(6) 0.0337(8) Uiso 1 1 d . . . H123 H 0.2849 0.6631 0.9050 0.040 Uiso 1 1 calc R . . C124 C 0.1495(9) 0.3305(9) 0.8339(5) 0.0337(8) Uiso 1 1 d D . . H12A H 0.1439 0.3587 0.8121 0.040 Uiso 1 1 calc R . . H12B H 0.1844 0.3024 0.8282 0.040 Uiso 1 1 calc R . . C125 C 0.1730(11) 0.3566(9) 0.8757(5) 0.0337(8) Uiso 1 1 d D . . H125 H 0.2206 0.3742 0.8752 0.040 Uiso 1 1 calc R . . C126 C 0.1808(12) 0.3248(10) 0.9142(6) 0.0337(8) Uiso 1 1 d . . . H126 H 0.1349 0.3048 0.9150 0.040 Uiso 1 1 calc R . . C127 C 0.1964(11) 0.3641(10) 0.9516(6) 0.0337(8) Uiso 1 1 d . . . H127 H 0.2439 0.3823 0.9517 0.040 Uiso 1 1 calc R . . C128 C 0.1383(12) 0.4095(10) 0.9519(6) 0.0337(8) Uiso 1 1 d . . . H128 H 0.0911 0.3908 0.9514 0.040 Uiso 1 1 calc R . . C129 C 0.1354(11) 0.4377(11) 0.9160(6) 0.0337(8) Uiso 1 1 d . . . H129 H 0.0967 0.4660 0.9157 0.040 Uiso 1 1 calc R . . C130 C 0.2938(11) 0.1787(8) 0.8229(5) 0.0337(8) Uiso 1 1 d D . . H13A H 0.2581 0.1964 0.8016 0.040 Uiso 1 1 calc R . . H13B H 0.3416 0.1813 0.8147 0.040 Uiso 1 1 calc R . . C131 C 0.2947(11) 0.2068(10) 0.8636(5) 0.0337(8) Uiso 1 1 d D . . H131 H 0.3091 0.2459 0.8602 0.040 Uiso 1 1 calc R . . C132 C 0.3494(11) 0.1827(10) 0.8990(5) 0.0337(8) Uiso 1 1 d . . . H132 H 0.3430 0.1419 0.8999 0.040 Uiso 1 1 calc R . . C133 C 0.3416(10) 0.2060(11) 0.9382(6) 0.0337(8) Uiso 1 1 d . . . H133 H 0.3513 0.2465 0.9390 0.040 Uiso 1 1 calc R . . C134 C 0.2608(10) 0.1933(10) 0.9437(5) 0.0337(8) Uiso 1 1 d . . . H134 H 0.2481 0.1533 0.9431 0.040 Uiso 1 1 calc R . . C135 C 0.2167(12) 0.2271(10) 0.9108(6) 0.0337(8) Uiso 1 1 d . . . H135 H 0.1654 0.2231 0.9140 0.040 Uiso 1 1 calc R . . C136 C 0.5517(10) 0.2019(9) 0.7990(5) 0.0337(8) Uiso 1 1 d D . . H13C H 0.5092 0.1988 0.7772 0.040 Uiso 1 1 calc R . . H13D H 0.5766 0.2368 0.7948 0.040 Uiso 1 1 calc R . . C137 C 0.5279(11) 0.2029(10) 0.8401(5) 0.0337(8) Uiso 1 1 d D . . H137 H 0.4980 0.2367 0.8410 0.040 Uiso 1 1 calc R . . C138 C 0.5990(11) 0.2088(10) 0.8768(6) 0.0337(8) Uiso 1 1 d . . . H138 H 0.6360 0.1804 0.8739 0.040 Uiso 1 1 calc R . . C139 C 0.5730(11) 0.2027(10) 0.9165(6) 0.0337(8) Uiso 1 1 d . . . H139 H 0.5426 0.2352 0.9205 0.040 Uiso 1 1 calc R . . C140 C 0.5273(11) 0.1474(10) 0.9196(6) 0.0337(8) Uiso 1 1 d . . . H140 H 0.5577 0.1156 0.9139 0.040 Uiso 1 1 calc R . . C141 C 0.4611(11) 0.1509(11) 0.8829(6) 0.0337(8) Uiso 1 1 d . . . H141 H 0.4321 0.1164 0.8822 0.040 Uiso 1 1 calc R . . O200 O 0.2343(9) 0.2819(9) 0.6135(5) 0.0904(12) Uiso 1 1 d . . . H852 H 0.2525 0.3111 0.6063 0.136 Uiso 1 1 calc R . . O201 O 0.2506(10) 0.4035(9) 0.6186(5) 0.0904(12) Uiso 1 1 d . . . H201 H 0.2079 0.4089 0.6216 0.136 Uiso 1 1 calc R . . O202 O 0.3576(9) 0.4777(9) 0.6053(5) 0.0904(12) Uiso 1 1 d . . . H202 H 0.3295 0.5030 0.6095 0.136 Uiso 1 1 calc R . . O203 O 0.4529(10) 0.5529(9) 0.5999(5) 0.0904(12) Uiso 1 1 d . . . H905 H 0.4495 0.5311 0.5802 0.136 Uiso 1 1 calc R . . O204 O 0.5944(9) 0.5399(9) 0.5722(5) 0.0904(12) Uiso 1 1 d . . . H204 H 0.6175 0.5160 0.5616 0.136 Uiso 1 1 calc R . . O205 O 0.7233(10) 0.4734(9) 0.5416(5) 0.0904(12) Uiso 1 1 d . . . H205 H 0.6837 0.4592 0.5441 0.136 Uiso 1 1 calc R . . O206 O 0.7962(9) 0.3697(9) 0.5491(5) 0.0904(12) Uiso 1 1 d . . . H206 H 0.7787 0.3853 0.5272 0.136 Uiso 1 1 calc R . . O207 O 0.9021(9) 0.2939(9) 0.5594(5) 0.0904(12) Uiso 1 1 d . . . H207 H 0.8742 0.3208 0.5601 0.136 Uiso 1 1 calc R . . O208 O 0.8449(9) 0.1938(9) 0.5575(5) 0.0904(12) Uiso 1 1 d . . . H208 H 0.8544 0.1608 0.5641 0.136 Uiso 1 1 calc R . . O209 O 0.7558(10) 0.1002(9) 0.5598(5) 0.0904(12) Uiso 1 1 d . . . H209 H 0.7777 0.1304 0.5627 0.136 Uiso 1 1 calc R . . O210 O 0.6152(10) 0.0702(9) 0.5636(5) 0.0904(12) Uiso 1 1 d . . . H210 H 0.6133 0.0356 0.5630 0.136 Uiso 1 1 calc R . . O211 O 0.4734(10) 0.0490(9) 0.5763(5) 0.0904(12) Uiso 1 1 d . . . H211 H 0.4918 0.0189 0.5710 0.136 Uiso 1 1 calc R . . O212 O 0.3566(10) 0.1045(8) 0.5874(5) 0.0904(12) Uiso 1 1 d . . . H212 H 0.3212 0.1053 0.5996 0.136 Uiso 1 1 calc R . . O213 O 0.2503(10) 0.1653(9) 0.6186(5) 0.0904(12) Uiso 1 1 d . . . H213 H 0.2214 0.1397 0.6211 0.136 Uiso 1 1 calc R . . O214 O 0.3354(10) 0.3364(11) 0.6700(5) 0.0904(12) Uiso 1 1 d . . . O215 O 0.4867(10) 0.4740(10) 0.6529(5) 0.0904(12) Uiso 1 1 d . . . O216 O 0.6966(11) 0.4712(9) 0.6232(5) 0.0904(12) Uiso 1 1 d . . . O217 O 0.8437(11) 0.3293(10) 0.6272(5) 0.0904(12) Uiso 1 1 d . . . O218 O 0.7833(10) 0.1584(10) 0.6288(5) 0.0904(12) Uiso 1 1 d . . . O219 O 0.5746(11) 0.0868(10) 0.6433(5) 0.0904(12) Uiso 1 1 d . . . O220 O 0.3237(10) 0.1996(10) 0.7192(6) 0.0904(12) Uiso 1 1 d . . . O221 O 0.3011(10) 0.2947(9) 0.7667(5) 0.0904(12) Uiso 1 1 d D . . H906 H 0.2704 0.2694 0.7639 0.136 Uiso 1 1 calc R . . O222 O 0.3695(11) 0.4037(9) 0.7164(5) 0.0904(12) Uiso 1 1 d . . . O223 O 0.4594(10) 0.4781(9) 0.7652(5) 0.0904(12) Uiso 1 1 d D . . H907 H 0.4870 0.5052 0.7702 0.136 Uiso 1 1 calc R . . O224 O 0.5840(11) 0.5249(9) 0.6947(5) 0.0904(12) Uiso 1 1 d . . . O225 O 0.7310(9) 0.5508(9) 0.7115(5) 0.0904(12) Uiso 1 1 d D . . H908 H 0.7254 0.5603 0.6870 0.136 Uiso 1 1 calc R . . O226 O 0.8195(10) 0.4752(10) 0.6482(5) 0.0904(12) Uiso 1 1 d . . . O227 O 0.8978(10) 0.4507(8) 0.7179(5) 0.0904(12) Uiso 1 1 d D . . H909 H 0.9348 0.4539 0.7357 0.136 Uiso 1 1 calc R . . O228 O 0.9145(10) 0.2682(10) 0.6667(5) 0.0904(12) Uiso 1 1 d . . . O231 O 0.6967(19) 0.0152(13) 0.7200(10) 0.0904(12) Uiso 0.50 1 d PD . . H837 H 0.6896 0.0052 0.7431 0.136 Uiso 0.50 1 calc PR . . O232 O 0.5053(10) 0.0506(10) 0.6842(5) 0.0904(12) Uiso 1 1 d . . . O234 O 0.3797(10) 0.1635(10) 0.6677(5) 0.0904(12) Uiso 1 1 d . . . O229 O 0.9397(10) 0.1744(9) 0.7090(5) 0.0904(12) Uiso 1 1 d D . . H910 H 0.9328 0.1493 0.6914 0.136 Uiso 1 1 calc R . . O230 O 0.7728(11) 0.0836(9) 0.6686(6) 0.0904(12) Uiso 1 1 d . . . O233 O 0.4020(10) 0.0493(9) 0.7357(5) 0.0904(12) Uiso 1 1 d D . . H911 H 0.3922 0.0496 0.7593 0.136 Uiso 1 1 calc R . . O235 O 0.7452(18) 0.0908(16) 0.7455(9) 0.0904(12) Uiso 0.50 1 d PD . . H836 H 0.7714 0.1119 0.7344 0.136 Uiso 0.50 1 calc PR . . C200 C 0.3619(11) 0.2773(11) 0.7511(7) 0.0751(15) Uiso 1 1 d D . . H20Y H 0.3903 0.2528 0.7715 0.090 Uiso 1 1 calc R . . H20H H 0.3917 0.3101 0.7483 0.090 Uiso 1 1 calc R . . C201 C 0.3486(15) 0.2473(13) 0.7105(7) 0.0751(15) Uiso 1 1 d D . . H20A H 0.3962 0.2409 0.7021 0.090 Uiso 1 1 calc R . . C202 C 0.3077(15) 0.2883(13) 0.6810(8) 0.0751(15) Uiso 1 1 d . . . H20B H 0.2614 0.2968 0.6904 0.090 Uiso 1 1 calc R . . C203 C 0.2903(15) 0.2499(11) 0.6413(8) 0.0751(15) Uiso 1 1 d D . . H203 H 0.3338 0.2429 0.6288 0.090 Uiso 1 1 calc R . . C204 C 0.2602(15) 0.1990(12) 0.6545(8) 0.0751(15) Uiso 1 1 d D . . H20C H 0.2138 0.2057 0.6642 0.090 Uiso 1 1 calc R . . C205 C 0.3135(15) 0.1677(13) 0.6863(8) 0.0751(15) Uiso 1 1 d . . . H20D H 0.2948 0.1306 0.6922 0.090 Uiso 1 1 calc R . . C206 C 0.4886(13) 0.4407(10) 0.7413(7) 0.0751(15) Uiso 1 1 d D . . H20I H 0.5115 0.4113 0.7596 0.090 Uiso 1 1 calc R . . H20J H 0.5276 0.4601 0.7306 0.090 Uiso 1 1 calc R . . C207 C 0.4420(14) 0.4121(12) 0.7049(7) 0.0751(15) Uiso 1 1 d D . . H20E H 0.4638 0.3774 0.6964 0.090 Uiso 1 1 calc R . . C208 C 0.4292(15) 0.4576(13) 0.6702(8) 0.0751(15) Uiso 1 1 d . . . H20F H 0.4125 0.4912 0.6831 0.090 Uiso 1 1 calc R . . C209 C 0.3653(13) 0.4381(13) 0.6389(7) 0.0751(15) Uiso 1 1 d D . . H20G H 0.3811 0.4028 0.6276 0.090 Uiso 1 1 calc R . . C210 C 0.2980(13) 0.4251(13) 0.6529(8) 0.0751(15) Uiso 1 1 d D . . H21A H 0.2771 0.4596 0.6624 0.090 Uiso 1 1 calc R . . C211 C 0.3137(16) 0.3849(13) 0.6877(8) 0.0751(15) Uiso 1 1 d . . . H21B H 0.2700 0.3782 0.7002 0.090 Uiso 1 1 calc R . . C212 C 0.6994(13) 0.4985(10) 0.7146(7) 0.0751(15) Uiso 1 1 d D . . H21C H 0.6839 0.4949 0.7413 0.090 Uiso 1 1 calc R . . H21D H 0.7350 0.4692 0.7124 0.090 Uiso 1 1 calc R . . C213 C 0.6343(13) 0.4920(13) 0.6802(7) 0.0751(15) Uiso 1 1 d D . . H21E H 0.6178 0.4528 0.6790 0.090 Uiso 1 1 calc R . . C214 C 0.6440(15) 0.5115(13) 0.6361(7) 0.0751(15) Uiso 1 1 d . . . H214 H 0.6697 0.5476 0.6398 0.090 Uiso 1 1 calc R . . C215 C 0.5798(14) 0.5212(12) 0.6067(8) 0.0751(15) Uiso 1 1 d D . . H215 H 0.5607 0.4834 0.5997 0.090 Uiso 1 1 calc R . . C216 C 0.5246(14) 0.5469(13) 0.6258(7) 0.0751(15) Uiso 1 1 d D . . H216 H 0.5417 0.5856 0.6312 0.090 Uiso 1 1 calc R . . C217 C 0.5072(15) 0.5260(13) 0.6684(7) 0.0751(15) Uiso 1 1 d . . . H217 H 0.4701 0.5474 0.6799 0.090 Uiso 1 1 calc R . . C219 C 0.8416(12) 0.4200(13) 0.6560(7) 0.0751(15) Uiso 1 1 d D . . H219 H 0.8064 0.4020 0.6711 0.090 Uiso 1 1 calc R . . C220 C 0.8407(15) 0.3899(13) 0.6183(8) 0.0751(15) Uiso 1 1 d . . . H220 H 0.8864 0.3993 0.6086 0.090 Uiso 1 1 calc R . . C221 C 0.7798(15) 0.4010(12) 0.5825(8) 0.0751(15) Uiso 1 1 d D . . H221 H 0.7334 0.3878 0.5896 0.090 Uiso 1 1 calc R . . C222 C 0.7786(15) 0.4609(12) 0.5796(8) 0.0751(15) Uiso 1 1 d D . . H222 H 0.8265 0.4732 0.5742 0.090 Uiso 1 1 calc R . . C223 C 0.7639(15) 0.4891(13) 0.6107(8) 0.0751(15) Uiso 1 1 d . . . H223 H 0.7631 0.5295 0.6049 0.090 Uiso 1 1 calc R . . C224 C 0.8751(12) 0.2029(11) 0.7094(7) 0.0751(15) Uiso 1 1 d D . . H22A H 0.8812 0.2321 0.7305 0.090 Uiso 1 1 calc R . . H22B H 0.8364 0.1776 0.7142 0.090 Uiso 1 1 calc R . . C225 C 0.8598(15) 0.2272(12) 0.6673(7) 0.0751(15) Uiso 1 1 d D . . H225 H 0.8139 0.2481 0.6659 0.090 Uiso 1 1 calc R . . C226 C 0.8504(15) 0.1932(13) 0.6296(8) 0.0751(15) Uiso 1 1 d . . . H226 H 0.8924 0.1677 0.6317 0.090 Uiso 1 1 calc R . . C227 C 0.8446(14) 0.2236(13) 0.5908(8) 0.0751(15) Uiso 1 1 d D . . H227 H 0.7989 0.2452 0.5870 0.090 Uiso 1 1 calc R . . C228 C 0.9039(14) 0.2625(12) 0.5938(8) 0.0751(15) Uiso 1 1 d D . . H228 H 0.9497 0.2411 0.5983 0.090 Uiso 1 1 calc R . . C229 C 0.9052(15) 0.3012(12) 0.6291(8) 0.0751(15) Uiso 1 1 d . . . H229 H 0.9462 0.3275 0.6302 0.090 Uiso 1 1 calc R . . C230 C 0.6880(15) 0.0722(13) 0.7163(7) 0.0751(15) Uiso 1 1 d D . . C231 C 0.7002(14) 0.0977(13) 0.6765(7) 0.0751(15) Uiso 1 1 d D . . H231 H 0.6934 0.1385 0.6768 0.090 Uiso 1 1 calc R . . C232 C 0.6476(14) 0.0706(14) 0.6397(7) 0.0751(15) Uiso 1 1 d . . . H232 H 0.6518 0.0295 0.6418 0.090 Uiso 1 1 calc R . . C233 C 0.6631(13) 0.0880(13) 0.6005(8) 0.0751(15) Uiso 1 1 d D . . H233 H 0.6558 0.1288 0.6007 0.090 Uiso 1 1 calc R . . C234 C 0.7388(13) 0.0825(13) 0.5987(7) 0.0751(15) Uiso 1 1 d D . . H234 H 0.7459 0.0417 0.5982 0.090 Uiso 1 1 calc R . . C235 C 0.7887(16) 0.1003(13) 0.6375(8) 0.0751(15) Uiso 1 1 d . . . H235 H 0.8385 0.0879 0.6360 0.090 Uiso 1 1 calc R . . C236 C 0.4560(13) 0.0886(11) 0.7328(6) 0.0751(15) Uiso 1 1 d D . . H23A H 0.5006 0.0769 0.7508 0.090 Uiso 1 1 calc R . . H23B H 0.4413 0.1242 0.7433 0.090 Uiso 1 1 calc R . . C237 C 0.4725(15) 0.0980(13) 0.6902(6) 0.0751(15) Uiso 1 1 d D . . H237 H 0.5068 0.1294 0.6905 0.090 Uiso 1 1 calc R . . C238 C 0.4021(15) 0.1110(13) 0.6616(7) 0.0751(15) Uiso 1 1 d . . . H238 H 0.3642 0.0838 0.6657 0.090 Uiso 1 1 calc R . . C239 C 0.4279(15) 0.1000(12) 0.6196(7) 0.0751(15) Uiso 1 1 d D . . H239 H 0.4615 0.1301 0.6146 0.090 Uiso 1 1 calc R . . C240 C 0.4590(15) 0.0473(12) 0.6125(8) 0.0751(15) Uiso 1 1 d D . . H240 H 0.4247 0.0168 0.6151 0.090 Uiso 1 1 calc R . . C241 C 0.5290(15) 0.0460(14) 0.6515(8) 0.0751(15) Uiso 1 1 d . . . H241 H 0.5539 0.0097 0.6514 0.090 Uiso 1 1 calc R . . C242 C 0.9144(10) 0.4227(9) 0.6849(5) 0.0337(8) Uiso 1 1 d D . . H24A H 0.9329 0.3853 0.6927 0.040 Uiso 1 1 calc R . . H24B H 0.9505 0.4429 0.6723 0.040 Uiso 1 1 calc R . . O1 O 0.7751(9) 0.2696(5) 0.7635(5) 0.101(3) Uiso 1 1 d D . . O2 O 0.7161(9) 0.1923(5) 0.7678(5) 0.101(3) Uiso 1 1 d D . . O3 O 0.3828(9) 0.4047(6) 0.4905(5) 0.101(3) Uiso 1 1 d D . . O4 O 0.3141(9) 0.3326(6) 0.4953(5) 0.101(3) Uiso 1 1 d D . . C1 C 0.7253(10) 0.2369(7) 0.7507(6) 0.111(3) Uiso 1 1 d D . . C14 C 0.3664(12) 0.3628(7) 0.5087(5) 0.111(3) Uiso 1 1 d D . . C2 C 0.6752(6) 0.2553(6) 0.7139(3) 0.111(3) Uiso 1 1 d G . . C3 C 0.6939(5) 0.2997(6) 0.6915(4) 0.111(3) Uiso 1 1 d GD . . H3 H 0.7396 0.3166 0.6989 0.133 Uiso 1 1 calc R . . C4 C 0.6458(5) 0.3192(5) 0.6583(3) 0.111(3) Uiso 1 1 d G . . H4 H 0.6586 0.3495 0.6430 0.133 Uiso 1 1 calc R . . C5 C 0.5790(4) 0.2945(4) 0.6475(2) 0.111(3) Uiso 1 1 d G . . C6 C 0.5602(6) 0.2501(5) 0.6699(3) 0.111(3) Uiso 1 1 d G . . H6 H 0.5146 0.2332 0.6625 0.133 Uiso 1 1 calc R . . C7 C 0.6083(7) 0.2306(6) 0.7031(3) 0.111(3) Uiso 1 1 d GD . . H7 H 0.5955 0.2003 0.7184 0.133 Uiso 1 1 calc R . . C8 C 0.5244(4) 0.3105(4) 0.6083(2) 0.111(3) Uiso 1 1 d G . . C9 C 0.5179(6) 0.3659(4) 0.5979(3) 0.111(3) Uiso 1 1 d G . . H9 H 0.5486 0.3923 0.6131 0.133 Uiso 1 1 calc R . . C10 C 0.4665(7) 0.3828(5) 0.5654(3) 0.111(3) Uiso 1 1 d GD . . H10 H 0.4621 0.4207 0.5583 0.133 Uiso 1 1 calc R . . C11 C 0.4216(6) 0.3443(6) 0.5431(3) 0.111(3) Uiso 1 1 d G . . C12 C 0.4280(6) 0.2888(6) 0.5535(3) 0.111(3) Uiso 1 1 d GD . . H12 H 0.3973 0.2624 0.5383 0.133 Uiso 1 1 calc R . . C13 C 0.4795(5) 0.2719(5) 0.5861(3) 0.111(3) Uiso 1 1 d G . . H13 H 0.4839 0.2340 0.5931 0.133 Uiso 1 1 calc R . . C15 C 0.4208(8) 0.4524(15) 0.8495(3) 0.111(3) Uiso 1 1 d D . . O5 O 0.3580(7) 0.4568(9) 0.8306(5) 0.101(3) Uiso 1 1 d D . . O6 O 0.4736(7) 0.4437(10) 0.8324(5) 0.101(3) Uiso 1 1 d D . . C16 C 0.4500(8) 0.4529(9) 0.8940(3) 0.111(3) Uiso 1 1 d G . . C17 C 0.4057(8) 0.4683(9) 0.9212(4) 0.111(3) Uiso 1 1 d GD . . H17 H 0.3596 0.4834 0.9114 0.133 Uiso 1 1 calc R . . C18 C 0.4287(11) 0.4616(9) 0.9628(4) 0.111(3) Uiso 1 1 d G . . H18 H 0.3983 0.4720 0.9814 0.133 Uiso 1 1 calc R . . C19 C 0.4961(12) 0.4395(9) 0.9771(4) 0.111(3) Uiso 1 1 d G . . C20 C 0.5405(9) 0.4241(9) 0.9499(5) 0.111(3) Uiso 1 1 d G . . H20 H 0.5865 0.4090 0.9597 0.133 Uiso 1 1 calc R . . C21 C 0.5175(8) 0.4308(9) 0.9083(5) 0.111(3) Uiso 1 1 d GD . . H21 H 0.5478 0.4204 0.8897 0.133 Uiso 1 1 calc R . . K1 K 0.9072(8) 0.2254(8) 0.4940(4) 0.103(5) Uani 0.50 1 d PU . . K2 K 0.9798(6) 0.3944(6) 0.8360(4) 0.092(4) Uani 0.60 1 d PU . . K3 K 0.8897(7) 0.2469(7) 0.9933(4) 0.084(5) Uani 0.50 1 d PU . . K4 K 0.5399(7) 0.7142(7) 0.7905(4) 0.076(4) Uani 0.50 1 d PU . . K5 K 0.0511(10) 0.1900(9) 0.6601(5) 0.152(7) Uani 0.50 1 d PU . . K6 K 0.5893(10) 0.0669(10) 0.9977(5) 0.116(7) Uani 0.40 1 d PU . . O1W O 0.958(2) 0.420(2) 0.9789(11) 0.1160(18) Uiso 0.50 1 d P . . O2W O 0.944(3) 0.483(2) 0.9570(12) 0.1160(18) Uiso 0.50 1 d P . . O3W O 0.986(2) 0.3018(18) 0.9472(12) 0.1160(18) Uiso 0.50 1 d P . . O4W O 0.9088(15) 0.3904(13) 0.9185(7) 0.1160(18) Uiso 0.75 1 d P . . O5W O 0.962(2) 0.2848(19) 0.8645(12) 0.1160(18) Uiso 0.50 1 d P . . O6W O 0.908(2) 0.2647(19) 0.8155(11) 0.1160(18) Uiso 0.50 1 d P . . O7W O 0.8504(11) 0.4368(10) 0.7963(5) 0.1160(18) Uiso 1 1 d . . . O8W O 0.922(2) 0.3259(19) 0.7711(11) 0.1160(18) Uiso 0.50 1 d P . . O9W O 0.6547(11) 0.6400(10) 0.7180(6) 0.1160(18) Uiso 1 1 d . . . O10W O 0.4079(11) 0.5710(10) 0.7363(5) 0.1160(18) Uiso 1 1 d . . . O11W O 0.4844(11) 0.0147(9) 0.8644(6) 0.1160(18) Uiso 1 1 d . . . O13W O 0.3623(11) 0.0451(10) 0.8137(6) 0.1160(18) Uiso 1 1 d . . . O14W O 0.036(2) 0.4638(19) 0.7775(11) 0.1160(18) Uiso 0.50 1 d P . . O15W O 0.1499(11) 0.4265(10) 0.7412(5) 0.1160(18) Uiso 1 1 d . . . O16W O 0.1662(11) 0.2525(10) 0.7425(6) 0.1160(18) Uiso 1 1 d . . . O17W O 0.026(2) 0.2919(19) 0.7344(11) 0.1160(18) Uiso 0.50 1 d P . . O18W O 0.091(2) 0.3453(19) 0.7006(12) 0.1160(18) Uiso 0.50 1 d P . . O19W O 0.0949(14) 0.2786(13) 0.6313(8) 0.1160(18) Uiso 0.75 1 d P . . O20W O 0.2334(18) 0.2586(17) 0.5373(11) 0.1160(18) Uiso 0.60 1 d P . . O21W O 0.126(2) 0.4010(19) 0.5167(11) 0.1160(18) Uiso 0.50 1 d P . . O22W O 0.189(2) 0.0855(19) 0.5156(11) 0.1160(18) Uiso 0.50 1 d P . . O23W O 0.363(2) 0.5128(18) 0.5270(11) 0.1160(18) Uiso 0.50 1 d P . . O24W O 0.4527(11) 0.6057(10) 0.5252(5) 0.1160(18) Uiso 1 1 d . . . O25W O 0.5000 0.4899(14) 0.5000 0.1160(18) Uiso 1 2 d S . . O26W O 0.5413(11) 0.8284(10) 0.5511(6) 0.1160(18) Uiso 1 1 d . . . O27W O 0.7516(16) 0.4804(14) 0.4641(8) 0.1160(18) Uiso 0.70 1 d P . . O28W O 0.906(2) 0.162(2) 0.4160(12) 0.1160(18) Uiso 0.50 1 d P . . O29W O 0.335(2) 0.3575(19) 0.8302(11) 0.1160(18) Uiso 0.50 1 d P . . O30W O 0.076(2) 0.3975(19) 0.6604(12) 0.1160(18) Uiso 0.50 1 d P . . O31W O 0.099(2) 0.4244(19) 0.6274(12) 0.1160(18) Uiso 0.50 1 d P . . O32W O 0.312(2) 0.0504(19) 0.7762(12) 0.1160(18) Uiso 0.50 1 d P . . O33W O 0.477(2) -0.0601(19) 0.5593(11) 0.1160(18) Uiso 0.50 1 d P . . O34W O 0.272(2) 0.3983(19) 0.7937(11) 0.1160(18) Uiso 0.50 1 d P . . O35W O 1.004(2) 0.395(2) 0.7852(11) 0.1160(18) Uiso 0.50 1 d P . . O36W O 0.852(2) 0.7282(19) 0.4645(11) 0.1160(18) Uiso 0.50 1 d P . . O37W O 0.883(2) 0.6403(19) 0.5078(11) 0.1160(18) Uiso 0.50 1 d P . . O38W O 0.260(2) 0.231(2) 0.5085(12) 0.1160(18) Uiso 0.50 1 d P . . O39W O 0.894(2) 0.264(2) 0.9619(13) 0.1160(18) Uiso 0.50 1 d P . . O40W O 0.871(2) 0.153(2) 0.4393(12) 0.1160(18) Uiso 0.50 1 d P . . O41W O 0.839(2) 0.9994(19) 0.7653(11) 0.1160(18) Uiso 0.50 1 d P . . O42W O 0.939(3) 0.506(2) 0.9409(13) 0.1160(18) Uiso 0.50 1 d P . . O43W O 0.819(2) 0.656(2) 0.5157(11) 0.1160(18) Uiso 0.50 1 d P . . O44W O 0.628(2) 0.0295(19) 0.4895(11) 0.1160(18) Uiso 0.50 1 d P . . O45W O 0.205(5) 0.338(5) 0.549(3) 0.1160(18) Uiso 0.20 1 d P . . 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 K1 0.112(9) 0.101(9) 0.094(8) -0.017(7) 0.010(7) -0.007(8) K2 0.066(7) 0.070(7) 0.127(7) -0.002(6) -0.021(6) 0.002(6) K3 0.077(8) 0.079(9) 0.100(8) 0.001(7) 0.026(7) 0.015(7) K4 0.071(7) 0.068(8) 0.082(7) -0.005(6) -0.007(6) -0.026(7) K5 0.154(10) 0.145(11) 0.155(10) -0.013(8) 0.017(8) 0.033(8) K6 0.114(10) 0.123(11) 0.117(9) 0.007(8) 0.040(8) 0.030(8) #============================================================================== # GEOMETRY #============================================================================== _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 O100 C104 1.32(2) . ? O100 H100 0.8400 . ? O101 C103 1.44(2) . ? O101 H101 0.8400 . ? O102 C110 1.51(2) . ? O102 H102 0.8400 . ? O103 C109 1.44(2) . ? O103 H103 0.8400 . ? O104 C116 1.42(2) . ? O104 H104 0.8400 . ? O105 C115 1.48(2) . ? O105 H105 0.8400 . ? O106 C122 1.42(2) . ? O106 H106 0.8400 . ? O107 C121 1.38(2) . ? O107 H107 0.8400 . ? O108 C128 1.32(2) . ? O108 H108 0.8400 . ? O109 C127 1.46(2) . ? O109 H109 0.8400 . ? O110 C134 1.52(2) . ? O110 H110 0.8400 . ? O111 C133 1.42(2) . ? O111 H111 0.8400 . ? O112 C140 1.31(2) . ? O112 H112 0.8400 . ? O113 C139 1.40(2) . ? O113 H113 0.8400 . ? O114 C105 1.42(2) . ? O114 C138 1.43(2) . ? O115 C111 1.41(2) . ? O115 C102 1.47(2) . ? O116 C108 1.42(2) . ? O116 C117 1.50(2) . ? O117 C123 1.43(2) . ? O117 C114 1.43(2) . ? O118 C120 1.33(2) . ? O118 C129 1.42(2) . ? O119 C126 1.37(2) . ? O119 C135 1.49(2) . ? O120 C141 1.37(2) . ? O120 C132 1.44(2) . ? O121 C105 1.46(2) . ? O121 C101 1.47(2) . ? O122 C100 1.404(11) . ? O122 H900 0.8400 . ? O123 C111 1.37(2) . ? O123 C107 1.41(2) . ? O124 C106 1.404(11) . ? O124 H124 0.8400 . ? O125 C117 1.39(2) . ? O125 C113 1.45(2) . ? O126 C112 1.39(3) . ? O126 H901 0.8400 . ? O127 C119 1.39(2) . ? O127 C123 1.48(2) . ? O128 C118 1.405(11) . ? O128 H902 0.8400 . ? O129 C129 1.48(2) . ? O129 C125 1.62(2) . ? O130 C124 1.406(11) . ? O130 H130 0.8400 . ? O131 C135 1.37(2) . ? O131 C131 1.46(2) . ? O132 C130 1.40(3) . ? O132 H903 0.8400 . ? O133 C137 1.39(2) . ? O133 C141 1.43(2) . ? O134 C136 1.39(3) . ? O134 H904 0.8400 . ? C100 C101 1.51(3) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.51(2) . ? C101 H10C 1.0000 . ? C102 C103 1.44(2) . ? C102 H10X 1.0000 . ? C103 C104 1.50(3) . ? C103 H10D 1.0000 . ? C104 C105 1.50(2) . ? C104 H10E 1.0000 . ? C105 H10F 1.0000 . ? C106 C107 1.53(3) . ? C106 H10G 0.9900 . ? C106 H10H 0.9900 . ? C107 C108 1.58(3) . ? C107 H10I 1.0000 . ? C108 C109 1.59(3) . ? C108 H10J 1.0000 . ? C109 C110 1.43(3) . ? C109 H10K 1.0000 . ? C110 C111 1.64(3) . ? C110 H11A 1.0000 . ? C111 H11B 1.0000 . ? C112 C113 1.55(3) . ? C112 H11C 0.9900 . ? C112 H11D 0.9900 . ? C113 C114 1.56(2) . ? C113 H11E 1.0000 . ? C114 C115 1.43(2) . ? C114 H114 1.0000 . ? C115 C116 1.54(3) . ? C115 H115 1.0000 . ? C116 C117 1.39(2) . ? C116 H116 1.0000 . ? C117 H117 1.0000 . ? C118 C119 1.523(11) . ? C118 H11F 0.9900 . ? C118 H11G 0.9900 . ? C119 C120 1.51(2) . ? C119 H119 1.0000 . ? C120 C121 1.54(2) . ? C120 H120 1.0000 . ? C121 C122 1.53(3) . ? C121 H121 1.0000 . ? C122 C123 1.39(2) . ? C122 H122 1.0000 . ? C123 H123 1.0000 . ? C124 C125 1.528(11) . ? C124 H12A 0.9900 . ? C124 H12B 0.9900 . ? C125 C126 1.48(2) . ? C125 H125 1.0000 . ? C126 C127 1.56(3) . ? C126 H126 1.0000 . ? C127 C128 1.56(3) . ? C127 H127 1.0000 . ? C128 C129 1.37(2) . ? C128 H128 1.0000 . ? C129 H129 1.0000 . ? C130 C131 1.52(3) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C131 C132 1.54(2) . ? C131 H131 1.0000 . ? C132 C133 1.45(2) . ? C132 H132 1.0000 . ? C133 C134 1.60(3) . ? C133 H133 1.0000 . ? C134 C135 1.50(3) . ? C134 H134 1.0000 . ? C135 H135 1.0000 . ? C136 C137 1.515(11) . ? C136 H13C 0.9900 . ? C136 H13D 0.9900 . ? C137 C138 1.66(2) . ? C137 H137 1.0000 . ? C138 C139 1.50(2) . ? C138 H138 1.0000 . ? C139 C140 1.61(3) . ? C139 H139 1.0000 . ? C140 C141 1.60(2) . ? C140 H140 1.0000 . ? C141 H141 1.0000 . ? O200 C203 1.50(3) . ? O200 H852 0.8400 . ? O201 C210 1.43(3) . ? O201 H201 0.8400 . ? O202 C209 1.47(3) . ? O202 H202 0.8400 . ? O203 C216 1.48(3) . ? O203 H905 0.8400 . ? O204 C215 1.31(2) . ? O204 H204 0.8400 . ? O205 C222 1.53(3) . ? O205 H205 0.8400 . ? O206 C221 1.43(3) . ? O206 H206 0.8400 . ? O207 C228 1.37(3) . ? O207 H207 0.8400 . ? O208 C227 1.33(3) . ? O208 H208 0.8400 . ? O209 C234 1.45(2) . ? O209 H209 0.8400 . ? O210 C233 1.46(3) . ? O210 H210 0.8400 . ? O211 C240 1.28(2) . ? O211 H211 0.8400 . ? O212 C239 1.58(3) . ? O212 H212 0.8400 . ? O213 C204 1.43(3) . ? O213 H213 0.8400 . ? O214 C202 1.35(3) . ? O214 C211 1.41(3) . ? O215 C208 1.37(3) . ? O215 C217 1.40(3) . ? O216 C223 1.47(3) . ? O216 C214 1.51(3) . ? O217 C229 1.34(3) . ? O217 C220 1.50(3) . ? O218 C235 1.44(3) . ? O218 C226 1.52(3) . ? O219 C241 1.37(3) . ? O219 C232 1.46(3) . ? O220 C201 1.30(3) . ? O220 C205 1.33(3) . ? O221 C200 1.41(3) . ? O221 H906 0.8400 . ? O222 C211 1.37(3) . ? O222 C207 1.50(3) . ? O223 C206 1.38(3) . ? O223 H907 0.8400 . ? O224 C213 1.39(3) . ? O224 C217 1.56(3) . ? O225 C212 1.41(3) . ? O225 H908 0.8400 . ? O226 C219 1.41(3) . ? O226 C223 1.53(3) . ? O227 C242 1.38(3) . ? O227 H909 0.8400 . ? O228 C225 1.44(3) . ? O228 C229 1.47(3) . ? O231 C230 1.396(12) . ? O231 H837 0.8400 . ? O232 C241 1.25(2) . ? O232 C237 1.34(3) . ? O234 C238 1.37(3) . ? O234 C205 1.49(3) . ? O229 C224 1.41(3) . ? O229 H910 0.8400 . ? O230 C235 1.20(3) . ? O230 C231 1.48(3) . ? O233 C236 1.41(3) . ? O233 H911 0.8400 . ? O235 C230 1.401(12) . ? O235 H836 0.8400 . ? C200 C201 1.52(3) . ? C200 H20Y 0.9900 . ? C200 H20H 0.9900 . ? C201 C202 1.52(3) . ? C201 H20A 1.0000 . ? C202 C203 1.61(3) . ? C202 H20B 1.0000 . ? C203 C204 1.46(4) . ? C203 H203 1.0000 . ? C204 C205 1.53(3) . ? C204 H20C 1.0000 . ? C205 H20D 1.0000 . ? C206 C207 1.54(3) . ? C206 H20I 0.9900 . ? C206 H20J 0.9900 . ? C207 C208 1.59(3) . ? C207 H20E 1.0000 . ? C208 C209 1.53(3) . ? C208 H20F 1.0000 . ? C209 C210 1.46(4) . ? C209 H20G 1.0000 . ? C210 C211 1.51(3) . ? C210 H21A 1.0000 . ? C211 H21B 1.0000 . ? C212 C213 1.54(3) . ? C212 H21C 0.9900 . ? C212 H21D 0.9900 . ? C213 C214 1.59(3) . ? C213 H21E 1.0000 . ? C214 C215 1.44(3) . ? C214 H214 1.0000 . ? C215 C216 1.45(4) . ? C215 H215 1.0000 . ? C216 C217 1.60(3) . ? C216 H216 1.0000 . ? C217 H217 1.0000 . ? C219 C220 1.45(3) . ? C219 C242 1.54(3) . ? C219 H219 1.0000 . ? C220 C221 1.54(3) . ? C220 H220 1.0000 . ? C221 C222 1.46(4) . ? C221 H221 1.0000 . ? C222 C223 1.31(3) . ? C222 H222 1.0000 . ? C223 H223 1.0000 . ? C224 C225 1.50(3) . ? C224 H22A 0.9900 . ? C224 H22B 0.9900 . ? C225 C226 1.49(3) . ? C225 H225 1.0000 . ? C226 C227 1.48(3) . ? C226 H226 1.0000 . ? C227 C228 1.46(4) . ? C227 H227 1.0000 . ? C228 C229 1.50(3) . ? C228 H228 1.0000 . ? C229 H229 1.0000 . ? C230 C231 1.52(4) . ? C231 C232 1.58(3) . ? C231 H231 1.0000 . ? C232 C233 1.45(3) . ? C232 H232 1.0000 . ? C233 C234 1.45(4) . ? C233 H233 1.0000 . ? C234 C235 1.53(3) . ? C234 H234 1.0000 . ? C235 H235 1.0000 . ? C236 C237 1.52(3) . ? C236 H23A 0.9900 . ? C236 H23B 0.9900 . ? C237 C238 1.53(3) . ? C237 H237 1.0000 . ? C238 C239 1.58(3) . ? C238 H238 1.0000 . ? C239 C240 1.44(4) . ? C239 H239 1.0000 . ? C240 C241 1.69(3) . ? C240 H240 1.0000 . ? C241 H241 1.0000 . ? C242 H24A 0.9900 . ? C242 H24B 0.9900 . ? O1 C1 1.25(2) . ? O2 C1 1.25(2) . ? O3 C14 1.25(2) . ? O4 C14 1.25(3) . ? C1 C2 1.49(2) . ? C14 C11 1.48(2) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 C8 1.5692 . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.3899 . ? C8 C13 1.3901 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3899 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C12 C13 1.3899 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 O6 1.25(2) . ? C15 O5 1.25(2) . ? C15 C16 1.490(11) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? K2 O35W 1.83(4) . ? K3 O39W 1.14(4) . ? O1W O2W 1.71(6) . ? O2W O42W 0.77(6) . ? O13W O32W 1.44(4) . ? O14W O35W 1.80(5) 1_455 ? O20W O38W 1.33(4) . ? O28W O40W 1.12(5) . ? O30W O31W 1.41(5) . ? O35W O14W 1.80(5) 1_655 ? O37W O43W 1.35(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 C104 O100 H100 109.5 . . ? C103 O101 H101 109.5 . . ? C110 O102 H102 109.5 . . ? C109 O103 H103 109.5 . . ? C116 O104 H104 109.5 . . ? C115 O105 H105 109.5 . . ? C122 O106 H106 109.5 . . ? C121 O107 H107 109.5 . . ? C128 O108 H108 109.5 . . ? C127 O109 H109 109.5 . . ? C134 O110 H110 109.5 . . ? C133 O111 H111 109.5 . . ? C140 O112 H112 109.5 . . ? C139 O113 H113 109.5 . . ? C105 O114 C138 114.3(18) . . ? C111 O115 C102 115.2(15) . . ? C108 O116 C117 117.9(16) . . ? C123 O117 C114 118.7(17) . . ? C120 O118 C129 120.3(18) . . ? C126 O119 C135 120.0(17) . . ? C141 O120 C132 117.0(18) . . ? C105 O121 C101 113.5(14) . . ? C100 O122 H900 109.5 . . ? C111 O123 C107 114.8(15) . . ? C106 O124 H124 109.5 . . ? C117 O125 C113 119.1(15) . . ? C112 O126 H901 109.5 . . ? C119 O127 C123 112.0(15) . . ? C118 O128 H902 109.5 . . ? C129 O129 C125 110.8(14) . . ? C124 O130 H130 109.5 . . ? C135 O131 C131 115.2(15) . . ? C130 O132 H903 109.5 . . ? C137 O133 C141 117.8(16) . . ? C136 O134 H904 109.5 . . ? O122 C100 C101 113.9(15) . . ? O122 C100 H10A 108.8 . . ? C101 C100 H10A 108.8 . . ? O122 C100 H10B 108.8 . . ? C101 C100 H10B 108.8 . . ? H10A C100 H10B 107.7 . . ? O121 C101 C102 106.4(16) . . ? O121 C101 C100 101.1(16) . . ? C102 C101 C100 112.9(17) . . ? O121 C101 H10C 112.0 . . ? C102 C101 H10C 112.0 . . ? C100 C101 H10C 112.0 . . ? C103 C102 O115 110.1(17) . . ? C103 C102 C101 112.8(19) . . ? O115 C102 C101 102.2(17) . . ? C103 C102 H10X 110.5 . . ? O115 C102 H10X 110.5 . . ? C101 C102 H10X 110.5 . . ? C102 C103 O101 114.1(19) . . ? C102 C103 C104 115.3(18) . . ? O101 C103 C104 111.5(17) . . ? C102 C103 H10D 104.9 . . ? O101 C103 H10D 104.9 . . ? C104 C103 H10D 104.9 . . ? O100 C104 C105 111.3(19) . . ? O100 C104 C103 119.7(18) . . ? C105 C104 C103 108.5(18) . . ? O100 C104 H10E 105.4 . . ? C105 C104 H10E 105.4 . . ? C103 C104 H10E 105.4 . . ? O114 C105 O121 107.3(16) . . ? O114 C105 C104 108.5(17) . . ? O121 C105 C104 112.8(19) . . ? O114 C105 H10F 109.4 . . ? O121 C105 H10F 109.4 . . ? C104 C105 H10F 109.4 . . ? O124 C106 C107 114.7(16) . . ? O124 C106 H10G 108.6 . . ? C107 C106 H10G 108.6 . . ? O124 C106 H10H 108.6 . . ? C107 C106 H10H 108.6 . . ? H10G C106 H10H 107.6 . . ? O123 C107 C106 106.2(15) . . ? O123 C107 C108 110.3(16) . . ? C106 C107 C108 104.6(16) . . ? O123 C107 H10I 111.8 . . ? C106 C107 H10I 111.8 . . ? C108 C107 H10I 111.8 . . ? O116 C108 C107 111.1(17) . . ? O116 C108 C109 109.5(15) . . ? C107 C108 C109 104.6(16) . . ? O116 C108 H10J 110.5 . . ? C107 C108 H10J 110.5 . . ? C109 C108 H10J 110.5 . . ? C110 C109 O103 109.4(18) . . ? C110 C109 C108 108.1(16) . . ? O103 C109 C108 106.6(17) . . ? C110 C109 H10K 110.9 . . ? O103 C109 H10K 110.9 . . ? C108 C109 H10K 110.9 . . ? C109 C110 O102 111.6(16) . . ? C109 C110 C111 109.3(18) . . ? O102 C110 C111 105.8(16) . . ? C109 C110 H11A 110.0 . . ? O102 C110 H11A 110.0 . . ? C111 C110 H11A 110.0 . . ? O123 C111 O115 112.6(18) . . ? O123 C111 C110 105.8(17) . . ? O115 C111 C110 107.3(15) . . ? O123 C111 H11B 110.3 . . ? O115 C111 H11B 110.3 . . ? C110 C111 H11B 110.3 . . ? O126 C112 C113 113.4(16) . . ? O126 C112 H11C 108.9 . . ? C113 C112 H11C 108.9 . . ? O126 C112 H11D 108.9 . . ? C113 C112 H11D 108.9 . . ? H11C C112 H11D 107.7 . . ? O125 C113 C112 103.1(16) . . ? O125 C113 C114 105.3(16) . . ? C112 C113 C114 112.0(16) . . ? O125 C113 H11E 112.0 . . ? C112 C113 H11E 112.0 . . ? C114 C113 H11E 112.0 . . ? O117 C114 C115 108.5(17) . . ? O117 C114 C113 106.3(16) . . ? C115 C114 C113 113.1(17) . . ? O117 C114 H114 109.6 . . ? C115 C114 H114 109.6 . . ? C113 C114 H114 109.6 . . ? C114 C115 O105 109.9(17) . . ? C114 C115 C116 110.5(17) . . ? O105 C115 C116 105.1(16) . . ? C114 C115 H115 110.4 . . ? O105 C115 H115 110.4 . . ? C116 C115 H115 110.4 . . ? C117 C116 O104 116.5(18) . . ? C117 C116 C115 112.0(18) . . ? O104 C116 C115 114.1(16) . . ? C117 C116 H116 104.2 . . ? O104 C116 H116 104.2 . . ? C115 C116 H116 104.2 . . ? O125 C117 C116 116.6(18) . . ? O125 C117 O116 102.2(17) . . ? C116 C117 O116 102.0(18) . . ? O125 C117 H117 111.7 . . ? C116 C117 H117 111.7 . . ? O116 C117 H117 111.7 . . ? O128 C118 C119 109.8(15) . . ? O128 C118 H11F 109.7 . . ? C119 C118 H11F 109.7 . . ? O128 C118 H11G 109.7 . . ? C119 C118 H11G 109.7 . . ? H11F C118 H11G 108.2 . . ? O127 C119 C120 116.7(18) . . ? O127 C119 C118 106.0(17) . . ? C120 C119 C118 114.1(18) . . ? O127 C119 H119 106.4 . . ? C120 C119 H119 106.4 . . ? C118 C119 H119 106.4 . . ? O118 C120 C119 114.0(19) . . ? O118 C120 C121 107.9(18) . . ? C119 C120 C121 109.2(17) . . ? O118 C120 H120 108.5 . . ? C119 C120 H120 108.5 . . ? C121 C120 H120 108.5 . . ? O107 C121 C122 112.8(18) . . ? O107 C121 C120 111.5(17) . . ? C122 C121 C120 109.2(18) . . ? O107 C121 H121 107.7 . . ? C122 C121 H121 107.7 . . ? C120 C121 H121 107.7 . . ? C123 C122 O106 112.3(18) . . ? C123 C122 C121 115(2) . . ? O106 C122 C121 110.5(17) . . ? C123 C122 H122 106.1 . . ? O106 C122 H122 106.1 . . ? C121 C122 H122 106.1 . . ? C122 C123 O117 111.1(18) . . ? C122 C123 O127 110.2(18) . . ? O117 C123 O127 107.5(16) . . ? C122 C123 H123 109.3 . . ? O117 C123 H123 109.3 . . ? O127 C123 H123 109.3 . . ? O130 C124 C125 102.8(14) . . ? O130 C124 H12A 111.2 . . ? C125 C124 H12A 111.2 . . ? O130 C124 H12B 111.2 . . ? C125 C124 H12B 111.2 . . ? H12A C124 H12B 109.1 . . ? C126 C125 C124 123.1(18) . . ? C126 C125 O129 108.9(14) . . ? C124 C125 O129 104.8(15) . . ? C126 C125 H125 106.3 . . ? C124 C125 H125 106.3 . . ? O129 C125 H125 106.3 . . ? O119 C126 C125 108.1(17) . . ? O119 C126 C127 112.1(17) . . ? C125 C126 C127 110.6(18) . . ? O119 C126 H126 108.6 . . ? C125 C126 H126 108.6 . . ? C127 C126 H126 108.6 . . ? O109 C127 C126 104.1(17) . . ? O109 C127 C128 112.9(16) . . ? C126 C127 C128 113.7(17) . . ? O109 C127 H127 108.7 . . ? C126 C127 H127 108.7 . . ? C128 C127 H127 108.7 . . ? O108 C128 C129 119(2) . . ? O108 C128 C127 108.3(17) . . ? C129 C128 C127 105.7(18) . . ? O108 C128 H128 107.9 . . ? C129 C128 H128 107.9 . . ? C127 C128 H128 107.9 . . ? C128 C129 O118 112.7(19) . . ? C128 C129 O129 118(2) . . ? O118 C129 O129 107.8(15) . . ? C128 C129 H129 105.9 . . ? O118 C129 H129 105.9 . . ? O129 C129 H129 105.9 . . ? O132 C130 C131 106.5(15) . . ? O132 C130 H13A 110.4 . . ? C131 C130 H13A 110.4 . . ? O132 C130 H13B 110.4 . . ? C131 C130 H13B 110.4 . . ? H13A C130 H13B 108.6 . . ? O131 C131 C130 109.4(16) . . ? O131 C131 C132 112.2(15) . . ? C130 C131 C132 114.7(17) . . ? O131 C131 H131 106.6 . . ? C130 C131 H131 106.6 . . ? C132 C131 H131 106.6 . . ? O120 C132 C133 110.6(17) . . ? O120 C132 C131 106.1(16) . . ? C133 C132 C131 112.5(17) . . ? O120 C132 H132 109.2 . . ? C133 C132 H132 109.2 . . ? C131 C132 H132 109.2 . . ? O111 C133 C132 113.7(18) . . ? O111 C133 C134 103.4(15) . . ? C132 C133 C134 105.9(17) . . ? O111 C133 H133 111.1 . . ? C132 C133 H133 111.1 . . ? C134 C133 H133 111.1 . . ? C135 C134 O110 103.6(17) . . ? C135 C134 C133 103.4(17) . . ? O110 C134 C133 105.1(16) . . ? C135 C134 H134 114.5 . . ? O110 C134 H134 114.5 . . ? C133 C134 H134 114.5 . . ? O131 C135 O119 110.0(17) . . ? O131 C135 C134 111.9(18) . . ? O119 C135 C134 113.1(18) . . ? O131 C135 H135 107.2 . . ? O119 C135 H135 107.2 . . ? C134 C135 H135 107.2 . . ? O134 C136 C137 110.5(15) . . ? O134 C136 H13C 109.5 . . ? C137 C136 H13C 109.5 . . ? O134 C136 H13D 109.5 . . ? C137 C136 H13D 109.5 . . ? H13C C136 H13D 108.1 . . ? O133 C137 C136 110.9(17) . . ? O133 C137 C138 113.7(16) . . ? C136 C137 C138 109.9(15) . . ? O133 C137 H137 107.4 . . ? C136 C137 H137 107.4 . . ? C138 C137 H137 107.4 . . ? O114 C138 C139 107.8(17) . . ? O114 C138 C137 108.3(16) . . ? C139 C138 C137 107.2(15) . . ? O114 C138 H138 111.1 . . ? C139 C138 H138 111.1 . . ? C137 C138 H138 111.1 . . ? O113 C139 C138 109.2(16) . . ? O113 C139 C140 107.5(16) . . ? C138 C139 C140 113.7(18) . . ? O113 C139 H139 108.8 . . ? C138 C139 H139 108.8 . . ? C140 C139 H139 108.8 . . ? O112 C140 C141 111.3(17) . . ? O112 C140 C139 117.7(18) . . ? C141 C140 C139 105.4(17) . . ? O112 C140 H140 107.3 . . ? C141 C140 H140 107.3 . . ? C139 C140 H140 107.3 . . ? O120 C141 O133 109.7(17) . . ? O120 C141 C140 108.2(17) . . ? O133 C141 C140 111.3(16) . . ? O120 C141 H141 109.2 . . ? O133 C141 H141 109.2 . . ? C140 C141 H141 109.2 . . ? C203 O200 H852 109.5 . . ? C210 O201 H201 109.5 . . ? C209 O202 H202 109.5 . . ? C216 O203 H905 109.5 . . ? C215 O204 H204 109.5 . . ? C222 O205 H205 109.5 . . ? C221 O206 H206 109.5 . . ? C228 O207 H207 109.5 . . ? C227 O208 H208 109.5 . . ? C234 O209 H209 109.5 . . ? C233 O210 H210 109.5 . . ? C240 O211 H211 109.5 . . ? C239 O212 H212 109.5 . . ? C204 O213 H213 109.5 . . ? C202 O214 C211 117(2) . . ? C208 O215 C217 107(2) . . ? C223 O216 C214 122(2) . . ? C229 O217 C220 121(2) . . ? C235 O218 C226 121(2) . . ? C241 O219 C232 117(2) . . ? C201 O220 C205 110(2) . . ? C200 O221 H906 109.5 . . ? C211 O222 C207 119.7(19) . . ? C206 O223 H907 109.5 . . ? C213 O224 C217 116.1(19) . . ? C212 O225 H908 109.5 . . ? C219 O226 C223 120(2) . . ? C242 O227 H909 109.5 . . ? C225 O228 C229 114(2) . . ? C230 O231 H837 109.5 . . ? C241 O232 C237 117(2) . . ? C238 O234 C205 115(2) . . ? C224 O229 H910 109.5 . . ? C235 O230 C231 117(2) . . ? C236 O233 H911 109.5 . . ? C230 O235 H836 109.5 . . ? O221 C200 C201 117(2) . . ? O221 C200 H20Y 108.1 . . ? C201 C200 H20Y 108.1 . . ? O221 C200 H20H 108.1 . . ? C201 C200 H20H 108.1 . . ? H20Y C200 H20H 107.3 . . ? O220 C201 C202 124(2) . . ? O220 C201 C200 104(2) . . ? C202 C201 C200 104(2) . . ? O220 C201 H20A 107.7 . . ? C202 C201 H20A 107.7 . . ? C200 C201 H20A 107.7 . . ? O214 C202 C201 124(3) . . ? O214 C202 C203 108(2) . . ? C201 C202 C203 99(2) . . ? O214 C202 H20B 108.0 . . ? C201 C202 H20B 108.0 . . ? C203 C202 H20B 108.0 . . ? C204 C203 O200 111(2) . . ? C204 C203 C202 106(2) . . ? O200 C203 C202 103(2) . . ? C204 C203 H203 112.0 . . ? O200 C203 H203 112.0 . . ? C202 C203 H203 112.0 . . ? O213 C204 C203 104(2) . . ? O213 C204 C205 106(2) . . ? C203 C204 C205 113(2) . . ? O213 C204 H20C 111.5 . . ? C203 C204 H20C 111.5 . . ? C205 C204 H20C 111.5 . . ? O220 C205 O234 112(2) . . ? O220 C205 C204 106(2) . . ? O234 C205 C204 104(2) . . ? O220 C205 H20D 111.7 . . ? O234 C205 H20D 111.7 . . ? C204 C205 H20D 111.7 . . ? O223 C206 C207 121(2) . . ? O223 C206 H20I 107.0 . . ? C207 C206 H20I 107.0 . . ? O223 C206 H20J 107.0 . . ? C207 C206 H20J 107.0 . . ? H20I C206 H20J 106.7 . . ? O222 C207 C206 107(2) . . ? O222 C207 C208 104(2) . . ? C206 C207 C208 105(2) . . ? O222 C207 H20E 113.4 . . ? C206 C207 H20E 113.4 . . ? C208 C207 H20E 113.4 . . ? O215 C208 C209 113(2) . . ? O215 C208 C207 118(2) . . ? C209 C208 C207 107(2) . . ? O215 C208 H20F 105.9 . . ? C209 C208 H20F 105.9 . . ? C207 C208 H20F 105.9 . . ? C210 C209 O202 114(2) . . ? C210 C209 C208 118(2) . . ? O202 C209 C208 106(2) . . ? C210 C209 H20G 105.6 . . ? O202 C209 H20G 105.6 . . ? C208 C209 H20G 105.6 . . ? O201 C210 C209 106(2) . . ? O201 C210 C211 113(2) . . ? C209 C210 C211 109(2) . . ? O201 C210 H21A 109.5 . . ? C209 C210 H21A 109.5 . . ? C211 C210 H21A 109.5 . . ? O222 C211 O214 109(2) . . ? O222 C211 C210 110(2) . . ? O214 C211 C210 105(2) . . ? O222 C211 H21B 110.9 . . ? O214 C211 H21B 110.9 . . ? C210 C211 H21B 110.9 . . ? O225 C212 C213 109(2) . . ? O225 C212 H21C 109.8 . . ? C213 C212 H21C 109.8 . . ? O225 C212 H21D 109.8 . . ? C213 C212 H21D 109.8 . . ? H21C C212 H21D 108.2 . . ? O224 C213 C212 101(2) . . ? O224 C213 C214 110(2) . . ? C212 C213 C214 117(2) . . ? O224 C213 H21E 109.4 . . ? C212 C213 H21E 109.4 . . ? C214 C213 H21E 109.4 . . ? C215 C214 O216 116(2) . . ? C215 C214 C213 117(2) . . ? O216 C214 C213 105(2) . . ? C215 C214 H214 106.0 . . ? O216 C214 H214 106.0 . . ? C213 C214 H214 106.0 . . ? O204 C215 C214 112(2) . . ? O204 C215 C216 121(2) . . ? C214 C215 C216 111(2) . . ? O204 C215 H215 103.7 . . ? C214 C215 H215 103.7 . . ? C216 C215 H215 103.7 . . ? C215 C216 O203 116(2) . . ? C215 C216 C217 122(2) . . ? O203 C216 C217 104.0(19) . . ? C215 C216 H216 104.3 . . ? O203 C216 H216 104.3 . . ? C217 C216 H216 104.3 . . ? O215 C217 O224 111(2) . . ? O215 C217 C216 93(2) . . ? O224 C217 C216 101(2) . . ? O215 C217 H217 116.2 . . ? O224 C217 H217 116.2 . . ? C216 C217 H217 116.2 . . ? O226 C219 C220 111(2) . . ? O226 C219 C242 106(2) . . ? C220 C219 C242 116(2) . . ? O226 C219 H219 107.8 . . ? C220 C219 H219 107.8 . . ? C242 C219 H219 107.8 . . ? C219 C220 O217 109(2) . . ? C219 C220 C221 119(2) . . ? O217 C220 C221 109(2) . . ? C219 C220 H220 106.5 . . ? O217 C220 H220 106.5 . . ? C221 C220 H220 106.5 . . ? O206 C221 C222 119(2) . . ? O206 C221 C220 106(2) . . ? C222 C221 C220 103(2) . . ? O206 C221 H221 109.3 . . ? C222 C221 H221 109.3 . . ? C220 C221 H221 109.3 . . ? C223 C222 C221 118(3) . . ? C223 C222 O205 110(2) . . ? C221 C222 O205 105(2) . . ? C223 C222 H222 107.8 . . ? C221 C222 H222 107.8 . . ? O205 C222 H222 107.8 . . ? C222 C223 O216 112(3) . . ? C222 C223 O226 109(2) . . ? O216 C223 O226 102(2) . . ? C222 C223 H223 111.0 . . ? O216 C223 H223 111.0 . . ? O226 C223 H223 111.0 . . ? O229 C224 C225 102.3(19) . . ? O229 C224 H22A 111.3 . . ? C225 C224 H22A 111.3 . . ? O229 C224 H22B 111.3 . . ? C225 C224 H22B 111.3 . . ? H22A C224 H22B 109.2 . . ? O228 C225 C226 111(2) . . ? O228 C225 C224 105(2) . . ? C226 C225 C224 123(2) . . ? O228 C225 H225 105.5 . . ? C226 C225 H225 105.5 . . ? C224 C225 H225 105.5 . . ? C227 C226 C225 116(2) . . ? C227 C226 O218 109(2) . . ? C225 C226 O218 108(2) . . ? C227 C226 H226 107.9 . . ? C225 C226 H226 107.9 . . ? O218 C226 H226 107.9 . . ? O208 C227 C228 107(2) . . ? O208 C227 C226 117(2) . . ? C228 C227 C226 109(2) . . ? O208 C227 H227 107.9 . . ? C228 C227 H227 107.9 . . ? C226 C227 H227 107.9 . . ? O207 C228 C227 113(2) . . ? O207 C228 C229 108(2) . . ? C227 C228 C229 112(2) . . ? O207 C228 H228 108.1 . . ? C227 C228 H228 108.1 . . ? C229 C228 H228 108.1 . . ? O217 C229 O228 107(2) . . ? O217 C229 C228 113(2) . . ? O228 C229 C228 108(2) . . ? O217 C229 H229 109.7 . . ? O228 C229 H229 109.7 . . ? C228 C229 H229 109.7 . . ? O231 C230 O235 101(3) . . ? O231 C230 C231 117(3) . . ? O235 C230 C231 105(2) . . ? O230 C231 C230 110(2) . . ? O230 C231 C232 104(2) . . ? C230 C231 C232 110(2) . . ? O230 C231 H231 110.8 . . ? C230 C231 H231 110.8 . . ? C232 C231 H231 110.8 . . ? C233 C232 O219 110(2) . . ? C233 C232 C231 112(2) . . ? O219 C232 C231 108(2) . . ? C233 C232 H232 109.1 . . ? O219 C232 H232 109.1 . . ? C231 C232 H232 109.1 . . ? C234 C233 C232 111(2) . . ? C234 C233 O210 114(2) . . ? C232 C233 O210 119(2) . . ? C234 C233 H233 103.4 . . ? C232 C233 H233 103.4 . . ? O210 C233 H233 103.4 . . ? C233 C234 O209 112(2) . . ? C233 C234 C235 114(2) . . ? O209 C234 C235 118(2) . . ? C233 C234 H234 103.2 . . ? O209 C234 H234 103.2 . . ? C235 C234 H234 103.2 . . ? O230 C235 O218 119(3) . . ? O230 C235 C234 115(3) . . ? O218 C235 C234 95(2) . . ? O230 C235 H235 108.7 . . ? O218 C235 H235 108.7 . . ? C234 C235 H235 108.7 . . ? O233 C236 C237 115(2) . . ? O233 C236 H23A 108.4 . . ? C237 C236 H23A 108.4 . . ? O233 C236 H23B 108.4 . . ? C237 C236 H23B 108.4 . . ? H23A C236 H23B 107.5 . . ? O232 C237 C236 101(2) . . ? O232 C237 C238 117(2) . . ? C236 C237 C238 108(2) . . ? O232 C237 H237 110.0 . . ? C236 C237 H237 110.0 . . ? C238 C237 H237 110.0 . . ? O234 C238 C237 111(2) . . ? O234 C238 C239 116(2) . . ? C237 C238 C239 99(2) . . ? O234 C238 H238 110.3 . . ? C237 C238 H238 110.3 . . ? C239 C238 H238 110.3 . . ? C240 C239 O212 106(2) . . ? C240 C239 C238 119(2) . . ? O212 C239 C238 104(2) . . ? C240 C239 H239 109.2 . . ? O212 C239 H239 109.2 . . ? C238 C239 H239 109.2 . . ? O211 C240 C239 107(2) . . ? O211 C240 C241 117(2) . . ? C239 C240 C241 100(2) . . ? O211 C240 H240 110.6 . . ? C239 C240 H240 110.6 . . ? C241 C240 H240 110.6 . . ? O232 C241 O219 116(3) . . ? O232 C241 C240 109(2) . . ? O219 C241 C240 106(2) . . ? O232 C241 H241 108.7 . . ? O219 C241 H241 108.7 . . ? C240 C241 H241 108.7 . . ? O227 C242 C219 102.6(17) . . ? O227 C242 H24A 111.2 . . ? C219 C242 H24A 111.2 . . ? O227 C242 H24B 111.2 . . ? C219 C242 H24B 111.2 . . ? H24A C242 H24B 109.2 . . ? O2 C1 O1 123.4(19) . . ? O2 C1 C2 121.3(10) . . ? O1 C1 C2 115.4(10) . . ? O4 C14 O3 123.4(18) . . ? O4 C14 C11 120.5(10) . . ? O3 C14 C11 115.0(13) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 119.5(12) . . ? C7 C2 C1 120.5(12) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C8 123.2 . . ? C6 C5 C8 116.5 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 C5 117.6 . . ? C13 C8 C5 122.2 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C14 119.7(13) . . ? C12 C11 C14 120.4(12) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? O6 C15 O5 123.3(13) . . ? O6 C15 C16 105.4(10) . . ? O5 C15 C16 131.3(10) . . ? C17 C16 C21 120.0 . . ? C17 C16 C15 119.4(14) . . ? C21 C16 C15 119.9(15) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 C19 106(2) . 2_657 ? C20 C19 C19 134(2) . 2_657 ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? O42W O2W O1W 161(8) . . ? O14W O35W K2 106(3) 1_655 . ? 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 C105 O121 C101 C102 58(2) . . . . ? C105 O121 C101 C100 176.5(15) . . . . ? O122 C100 C101 O121 -56(2) . . . . ? O122 C100 C101 C102 57(3) . . . . ? C111 O115 C102 C103 125.1(18) . . . . ? C111 O115 C102 C101 -114.9(17) . . . . ? O121 C101 C102 C103 -56(2) . . . . ? C100 C101 C102 C103 -166.1(19) . . . . ? O121 C101 C102 O115 -174.3(14) . . . . ? C100 C101 C102 O115 76(2) . . . . ? O115 C102 C103 O101 -61(2) . . . . ? C101 C102 C103 O101 -174.2(17) . . . . ? O115 C102 C103 C104 168.2(17) . . . . ? C101 C102 C103 C104 55(3) . . . . ? C102 C103 C104 O100 -178.4(19) . . . . ? O101 C103 C104 O100 49(3) . . . . ? C102 C103 C104 C105 -49(3) . . . . ? O101 C103 C104 C105 178.6(16) . . . . ? C138 O114 C105 O121 119.6(18) . . . . ? C138 O114 C105 C104 -118.2(19) . . . . ? C101 O121 C105 O114 61(2) . . . . ? C101 O121 C105 C104 -58(2) . . . . ? O100 C104 C105 O114 64(2) . . . . ? C103 C104 C105 O114 -69(2) . . . . ? O100 C104 C105 O121 -176.8(16) . . . . ? C103 C104 C105 O121 49(2) . . . . ? C111 O123 C107 C106 177.5(16) . . . . ? C111 O123 C107 C108 65(2) . . . . ? O124 C106 C107 O123 -62(2) . . . . ? O124 C106 C107 C108 55(2) . . . . ? C117 O116 C108 C107 -118.5(18) . . . . ? C117 O116 C108 C109 126.5(18) . . . . ? O123 C107 C108 O116 -175.9(16) . . . . ? C106 C107 C108 O116 70(2) . . . . ? O123 C107 C108 C109 -57.8(19) . . . . ? C106 C107 C108 C109 -171.6(16) . . . . ? O116 C108 C109 C110 179.5(19) . . . . ? C107 C108 C109 C110 60(2) . . . . ? O116 C108 C109 O103 -63(2) . . . . ? C107 C108 C109 O103 177.8(15) . . . . ? O103 C109 C110 O102 65(2) . . . . ? C108 C109 C110 O102 -179.6(16) . . . . ? O103 C109 C110 C111 -178.7(15) . . . . ? C108 C109 C110 C111 -63(2) . . . . ? C107 O123 C111 O115 55(2) . . . . ? C107 O123 C111 C110 -62(2) . . . . ? C102 O115 C111 O123 118.1(18) . . . . ? C102 O115 C111 C110 -125.8(17) . . . . ? C109 C110 C111 O123 62(2) . . . . ? O102 C110 C111 O123 -177.6(16) . . . . ? C109 C110 C111 O115 -58(2) . . . . ? O102 C110 C111 O115 62(2) . . . . ? C117 O125 C113 C112 167.0(16) . . . . ? C117 O125 C113 C114 49(2) . . . . ? O126 C112 C113 O125 -73(2) . . . . ? O126 C112 C113 C114 40(3) . . . . ? C123 O117 C114 C115 123.4(19) . . . . ? C123 O117 C114 C113 -114.7(17) . . . . ? O125 C113 C114 O117 -172.8(15) . . . . ? C112 C113 C114 O117 76(2) . . . . ? O125 C113 C114 C115 -54(2) . . . . ? C112 C113 C114 C115 -165.2(19) . . . . ? O117 C114 C115 O105 -71(2) . . . . ? C113 C114 C115 O105 171.2(17) . . . . ? O117 C114 C115 C116 173.3(16) . . . . ? C113 C114 C115 C116 56(3) . . . . ? C114 C115 C116 C117 -50(3) . . . . ? O105 C115 C116 C117 -168.4(18) . . . . ? C114 C115 C116 O104 175.0(18) . . . . ? O105 C115 C116 O104 56(2) . . . . ? C113 O125 C117 C116 -50(3) . . . . ? C113 O125 C117 O116 61(2) . . . . ? O104 C116 C117 O125 179.3(18) . . . . ? C115 C116 C117 O125 45(3) . . . . ? O104 C116 C117 O116 69(2) . . . . ? C115 C116 C117 O116 -65(2) . . . . ? C108 O116 C117 O125 114.8(17) . . . . ? C108 O116 C117 C116 -124.3(18) . . . . ? C123 O127 C119 C120 54(2) . . . . ? C123 O127 C119 C118 -177.6(14) . . . . ? O128 C118 C119 O127 -67(2) . . . . ? O128 C118 C119 C120 63(2) . . . . ? C129 O118 C120 C119 -118(2) . . . . ? C129 O118 C120 C121 120.7(18) . . . . ? O127 C119 C120 O118 -170.2(17) . . . . ? C118 C119 C120 O118 66(3) . . . . ? O127 C119 C120 C121 -49(2) . . . . ? C118 C119 C120 C121 -173.8(18) . . . . ? O118 C120 C121 O107 -65(2) . . . . ? C119 C120 C121 O107 170.5(18) . . . . ? O118 C120 C121 C122 169.6(18) . . . . ? C119 C120 C121 C122 45(2) . . . . ? O107 C121 C122 C123 -178.6(17) . . . . ? C120 C121 C122 C123 -54(3) . . . . ? O107 C121 C122 O106 53(2) . . . . ? C120 C121 C122 O106 177.5(15) . . . . ? O106 C122 C123 O117 66(3) . . . . ? C121 C122 C123 O117 -61(3) . . . . ? O106 C122 C123 O127 -174.6(16) . . . . ? C121 C122 C123 O127 58(3) . . . . ? C114 O117 C123 C122 -126.8(19) . . . . ? C114 O117 C123 O127 112.6(18) . . . . ? C119 O127 C123 C122 -56(2) . . . . ? C119 O127 C123 O117 65(2) . . . . ? O130 C124 C125 C126 57(3) . . . . ? O130 C124 C125 O129 -68.2(18) . . . . ? C129 O129 C125 C126 50(2) . . . . ? C129 O129 C125 C124 -176.9(15) . . . . ? C135 O119 C126 C125 -111.6(19) . . . . ? C135 O119 C126 C127 126.2(19) . . . . ? C124 C125 C126 O119 64(3) . . . . ? O129 C125 C126 O119 -173.2(15) . . . . ? C124 C125 C126 C127 -173.2(17) . . . . ? O129 C125 C126 C127 -50(2) . . . . ? O119 C126 C127 O109 -59(2) . . . . ? C125 C126 C127 O109 179.9(16) . . . . ? O119 C126 C127 C128 177.5(17) . . . . ? C125 C126 C127 C128 57(2) . . . . ? O109 C127 C128 O108 56(2) . . . . ? C126 C127 C128 O108 174.7(17) . . . . ? O109 C127 C128 C129 -175.6(18) . . . . ? C126 C127 C128 C129 -57(2) . . . . ? O108 C128 C129 O118 55(3) . . . . ? C127 C128 C129 O118 -67(2) . . . . ? O108 C128 C129 O129 -178.7(17) . . . . ? C127 C128 C129 O129 60(2) . . . . ? C120 O118 C129 C128 -117(2) . . . . ? C120 O118 C129 O129 111.4(19) . . . . ? C125 O129 C129 C128 -58(2) . . . . ? C125 O129 C129 O118 70.6(19) . . . . ? C135 O131 C131 C130 173.2(16) . . . . ? C135 O131 C131 C132 45(2) . . . . ? O132 C130 C131 O131 -67(2) . . . . ? O132 C130 C131 C132 61(2) . . . . ? C141 O120 C132 C133 122(2) . . . . ? C141 O120 C132 C131 -115.7(18) . . . . ? O131 C131 C132 O120 -167.7(16) . . . . ? C130 C131 C132 O120 67(2) . . . . ? O131 C131 C132 C133 -47(2) . . . . ? C130 C131 C132 C133 -172.4(18) . . . . ? O120 C132 C133 O111 -71(2) . . . . ? C131 C132 C133 O111 170.8(17) . . . . ? O120 C132 C133 C134 176.4(17) . . . . ? C131 C132 C133 C134 58(2) . . . . ? O111 C133 C134 C135 174.0(16) . . . . ? C132 C133 C134 C135 -66(2) . . . . ? O111 C133 C134 O110 66(2) . . . . ? C132 C133 C134 O110 -174.5(16) . . . . ? C131 O131 C135 O119 68(2) . . . . ? C131 O131 C135 C134 -58(2) . . . . ? C126 O119 C135 O131 107(2) . . . . ? C126 O119 C135 C134 -127.5(18) . . . . ? O110 C134 C135 O131 176.5(16) . . . . ? C133 C134 C135 O131 67(2) . . . . ? O110 C134 C135 O119 52(2) . . . . ? C133 C134 C135 O119 -58(2) . . . . ? C141 O133 C137 C136 176.7(16) . . . . ? C141 O133 C137 C138 52(2) . . . . ? O134 C136 C137 O133 -67(2) . . . . ? O134 C136 C137 C138 60(2) . . . . ? C105 O114 C138 C139 132.1(17) . . . . ? C105 O114 C138 C137 -112.2(17) . . . . ? O133 C137 C138 O114 -164.4(15) . . . . ? C136 C137 C138 O114 71(2) . . . . ? O133 C137 C138 C139 -48(2) . . . . ? C136 C137 C138 C139 -173.3(18) . . . . ? O114 C138 C139 O113 -70(2) . . . . ? C137 C138 C139 O113 173.6(17) . . . . ? O114 C138 C139 C140 170.0(16) . . . . ? C137 C138 C139 C140 54(2) . . . . ? O113 C139 C140 O112 55(2) . . . . ? C138 C139 C140 O112 176.4(18) . . . . ? O113 C139 C140 C141 -179.8(15) . . . . ? C138 C139 C140 C141 -59(2) . . . . ? C132 O120 C141 O133 126.8(17) . . . . ? C132 O120 C141 C140 -111.6(18) . . . . ? C137 O133 C141 O120 62(2) . . . . ? C137 O133 C141 C140 -58(2) . . . . ? O112 C140 C141 O120 64(2) . . . . ? C139 C140 C141 O120 -65(2) . . . . ? O112 C140 C141 O133 -175.4(18) . . . . ? C139 C140 C141 O133 56(2) . . . . ? C205 O220 C201 C202 65(3) . . . . ? C205 O220 C201 C200 -176(2) . . . . ? O221 C200 C201 O220 -72(3) . . . . ? O221 C200 C201 C202 60(3) . . . . ? C211 O214 C202 C201 -104(3) . . . . ? C211 O214 C202 C203 141(2) . . . . ? O220 C201 C202 O214 -175(2) . . . . ? C200 C201 C202 O214 66(3) . . . . ? O220 C201 C202 C203 -56(3) . . . . ? C200 C201 C202 C203 -174(2) . . . . ? O214 C202 C203 C204 -180(2) . . . . ? C201 C202 C203 C204 50(3) . . . . ? O214 C202 C203 O200 -63(3) . . . . ? C201 C202 C203 O200 166(2) . . . . ? O200 C203 C204 O213 72(3) . . . . ? C202 C203 C204 O213 -176(2) . . . . ? O200 C203 C204 C205 -174(2) . . . . ? C202 C203 C204 C205 -63(3) . . . . ? C201 O220 C205 O234 54(3) . . . . ? C201 O220 C205 C204 -59(3) . . . . ? C238 O234 C205 O220 127(3) . . . . ? C238 O234 C205 C204 -120(2) . . . . ? O213 C204 C205 O220 179(2) . . . . ? C203 C204 C205 O220 66(3) . . . . ? O213 C204 C205 O234 61(3) . . . . ? C203 C204 C205 O234 -51(3) . . . . ? C211 O222 C207 C206 172(2) . . . . ? C211 O222 C207 C208 61(3) . . . . ? O223 C206 C207 O222 -34(3) . . . . ? O223 C206 C207 C208 76(3) . . . . ? C217 O215 C208 C209 129(2) . . . . ? C217 O215 C208 C207 -105(3) . . . . ? O222 C207 C208 O215 -179(2) . . . . ? C206 C207 C208 O215 69(3) . . . . ? O222 C207 C208 C209 -51(3) . . . . ? C206 C207 C208 C209 -163(2) . . . . ? O215 C208 C209 C210 -173(3) . . . . ? C207 C208 C209 C210 55(4) . . . . ? O215 C208 C209 O202 -44(3) . . . . ? C207 C208 C209 O202 -175(2) . . . . ? O202 C209 C210 O201 59(3) . . . . ? C208 C209 C210 O201 -175(2) . . . . ? O202 C209 C210 C211 -179(2) . . . . ? C208 C209 C210 C211 -53(4) . . . . ? C207 O222 C211 O214 53(3) . . . . ? C207 O222 C211 C210 -62(3) . . . . ? C202 O214 C211 O222 106(3) . . . . ? C202 O214 C211 C210 -136(2) . . . . ? O201 C210 C211 O222 168(2) . . . . ? C209 C210 C211 O222 50(3) . . . . ? O201 C210 C211 O214 51(3) . . . . ? C209 C210 C211 O214 -67(3) . . . . ? C217 O224 C213 C212 -176.6(18) . . . . ? C217 O224 C213 C214 59(3) . . . . ? O225 C212 C213 O224 -76(2) . . . . ? O225 C212 C213 C214 44(3) . . . . ? C223 O216 C214 C215 105(3) . . . . ? C223 O216 C214 C213 -124(2) . . . . ? O224 C213 C214 C215 -47(3) . . . . ? C212 C213 C214 C215 -162(2) . . . . ? O224 C213 C214 O216 -177(2) . . . . ? C212 C213 C214 O216 68(3) . . . . ? O216 C214 C215 O204 -59(3) . . . . ? C213 C214 C215 O204 177(2) . . . . ? O216 C214 C215 C216 163(2) . . . . ? C213 C214 C215 C216 38(4) . . . . ? O204 C215 C216 O203 53(4) . . . . ? C214 C215 C216 O203 -173(2) . . . . ? O204 C215 C216 C217 -178(2) . . . . ? C214 C215 C216 C217 -44(4) . . . . ? C208 O215 C217 O224 115(2) . . . . ? C208 O215 C217 C216 -142(2) . . . . ? C213 O224 C217 O215 39(3) . . . . ? C213 O224 C217 C216 -58(3) . . . . ? C215 C216 C217 O215 -62(3) . . . . ? O203 C216 C217 O215 72(2) . . . . ? C215 C216 C217 O224 50(3) . . . . ? O203 C216 C217 O224 -176(2) . . . . ? C223 O226 C219 C220 33(3) . . . . ? C223 O226 C219 C242 159.6(18) . . . . ? O226 C219 C220 O217 -164(2) . . . . ? C242 C219 C220 O217 75(3) . . . . ? O226 C219 C220 C221 -38(4) . . . . ? C242 C219 C220 C221 -160(2) . . . . ? C229 O217 C220 C219 -102(3) . . . . ? C229 O217 C220 C221 127(3) . . . . ? C219 C220 C221 O206 175(2) . . . . ? O217 C220 C221 O206 -59(3) . . . . ? C219 C220 C221 C222 49(4) . . . . ? O217 C220 C221 C222 175(2) . . . . ? O206 C221 C222 C223 -180(2) . . . . ? C220 C221 C222 C223 -62(4) . . . . ? O206 C221 C222 O205 58(3) . . . . ? C220 C221 C222 O205 174.8(19) . . . . ? C221 C222 C223 O216 -53(4) . . . . ? O205 C222 C223 O216 67(3) . . . . ? C221 C222 C223 O226 59(4) . . . . ? O205 C222 C223 O226 179(2) . . . . ? C214 O216 C223 C222 -140(2) . . . . ? C214 O216 C223 O226 103(2) . . . . ? C219 O226 C223 C222 -42(3) . . . . ? C219 O226 C223 O216 77(3) . . . . ? C229 O228 C225 C226 51(3) . . . . ? C229 O228 C225 C224 -174(2) . . . . ? O229 C224 C225 O228 -69(3) . . . . ? O229 C224 C225 C226 59(3) . . . . ? O228 C225 C226 C227 -47(3) . . . . ? C224 C225 C226 C227 -173(2) . . . . ? O228 C225 C226 O218 -170(2) . . . . ? C224 C225 C226 O218 65(3) . . . . ? C235 O218 C226 C227 127(3) . . . . ? C235 O218 C226 C225 -106(3) . . . . ? C225 C226 C227 O208 172(2) . . . . ? O218 C226 C227 O208 -66(3) . . . . ? C225 C226 C227 C228 51(3) . . . . ? O218 C226 C227 C228 172(2) . . . . ? O208 C227 C228 O207 54(3) . . . . ? C226 C227 C228 O207 -178(2) . . . . ? O208 C227 C228 C229 176(2) . . . . ? C226 C227 C228 C229 -57(3) . . . . ? C220 O217 C229 O228 132(2) . . . . ? C220 O217 C229 C228 -110(3) . . . . ? C225 O228 C229 O217 64(3) . . . . ? C225 O228 C229 C228 -58(3) . . . . ? O207 C228 C229 O217 68(3) . . . . ? C227 C228 C229 O217 -57(3) . . . . ? O207 C228 C229 O228 -174(2) . . . . ? C227 C228 C229 O228 61(3) . . . . ? C235 O230 C231 C230 178(3) . . . . ? C235 O230 C231 C232 61(3) . . . . ? O231 C230 C231 O230 -56(4) . . . . ? O235 C230 C231 O230 55(3) . . . . ? O231 C230 C231 C232 58(4) . . . . ? O235 C230 C231 C232 169(3) . . . . ? C241 O219 C232 C233 124(3) . . . . ? C241 O219 C232 C231 -114(2) . . . . ? O230 C231 C232 C233 -54(3) . . . . ? C230 C231 C232 C233 -172(2) . . . . ? O230 C231 C232 O219 -175(2) . . . . ? C230 C231 C232 O219 67(3) . . . . ? O219 C232 C233 C234 169(2) . . . . ? C231 C232 C233 C234 49(4) . . . . ? O219 C232 C233 O210 -55(3) . . . . ? C231 C232 C233 O210 -175(2) . . . . ? C232 C233 C234 O209 -180(2) . . . . ? O210 C233 C234 O209 43(4) . . . . ? C232 C233 C234 C235 -41(4) . . . . ? O210 C233 C234 C235 -179(2) . . . . ? C231 O230 C235 O218 55(4) . . . . ? C231 O230 C235 C234 -57(4) . . . . ? C226 O218 C235 O230 110(3) . . . . ? C226 O218 C235 C234 -127(2) . . . . ? C233 C234 C235 O230 46(4) . . . . ? O209 C234 C235 O230 -179(3) . . . . ? C233 C234 C235 O218 -80(3) . . . . ? O209 C234 C235 O218 56(3) . . . . ? C241 O232 C237 C236 -177(2) . . . . ? C241 O232 C237 C238 66(3) . . . . ? O233 C236 C237 O232 -71(3) . . . . ? O233 C236 C237 C238 53(3) . . . . ? C205 O234 C238 C237 -111(2) . . . . ? C205 O234 C238 C239 138(2) . . . . ? O232 C237 C238 O234 -172(2) . . . . ? C236 C237 C238 O234 75(3) . . . . ? O232 C237 C238 C239 -50(3) . . . . ? C236 C237 C238 C239 -163(2) . . . . ? O234 C238 C239 C240 174(2) . . . . ? C237 C238 C239 C240 55(3) . . . . ? O234 C238 C239 O212 -69(3) . . . . ? C237 C238 C239 O212 173(2) . . . . ? O212 C239 C240 O211 62(3) . . . . ? C238 C239 C240 O211 179(2) . . . . ? O212 C239 C240 C241 -174.7(18) . . . . ? C238 C239 C240 C241 -59(3) . . . . ? C237 O232 C241 O219 54(4) . . . . ? C237 O232 C241 C240 -64(3) . . . . ? C232 O219 C241 O232 118(3) . . . . ? C232 O219 C241 C240 -121(2) . . . . ? O211 C240 C241 O232 173(3) . . . . ? C239 C240 C241 O232 58(3) . . . . ? O211 C240 C241 O219 48(3) . . . . ? C239 C240 C241 O219 -67(3) . . . . ? O226 C219 C242 O227 59(2) . . . . ? C220 C219 C242 O227 -177(2) . . . . ? O2 C1 C2 C3 -168(2) . . . . ? O1 C1 C2 C3 14(3) . . . . ? O2 C1 C2 C7 15(3) . . . . ? O1 C1 C2 C7 -162.8(19) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 -176.4(16) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C8 -174.3 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C8 C5 C6 C7 174.7 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 176.4(16) . . . . ? C4 C5 C8 C9 -39.6 . . . . ? C6 C5 C8 C9 145.9 . . . . ? C4 C5 C8 C13 145.4 . . . . ? C6 C5 C8 C13 -29.1 . . . . ? C13 C8 C9 C10 0.0 . . . . ? C5 C8 C9 C10 -175.1 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C14 179.4(14) . . . . ? O4 C14 C11 C10 -161(2) . . . . ? O3 C14 C11 C10 31(3) . . . . ? O4 C14 C11 C12 18(3) . . . . ? O3 C14 C11 C12 -149.9(18) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C14 C11 C12 C13 -179.4(15) . . . . ? C11 C12 C13 C8 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? C5 C8 C13 C12 174.8 . . . . ? O6 C15 C16 C17 172(2) . . . . ? O5 C15 C16 C17 -11(5) . . . . ? O6 C15 C16 C21 -17(3) . . . . ? O5 C15 C16 C21 160(3) . . . . ? C21 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C18 171(2) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C16 0.0 . . . . ? C17 C16 C21 C20 0.0 . . . . ? C15 C16 C21 C20 -171(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.579 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.111 #============================================================================== # END #==============================================================================