# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Lukes, Ivan' 'Jurecka, Petr' 'Novotny, Karel' 'Rohovec, Jan' 'Vojtisek, Pavel' _publ_contact_author_name 'Prof Ivan Lukes' _publ_contact_author_address ; Department of Inorganic Chemistry Universita Karlova (Charles University) Hlavova 2030 Prague 2 CZ-128 40 CZECH REPUBLIC ; _publ_contact_author_email 'LUKES@NATUR.CUNI.CZ' _publ_section_title ; Synthesis, Characterisation and Extraction Behaviour of Calix[4]Arene-Based Phosphonic Acids ; data_dpcfix4 #in paper label 1a _database_code_CSD 179147 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54H78O10P2*CH3OH*0.33H2O ( three indep. mol.)' _chemical_formula_sum 'C168 H243 O31 P6' _chemical_formula_weight 2944.44 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.8560(10) _cell_length_b 20.9620(10) _cell_length_c 23.9120(10) _cell_angle_alpha 71.093(4) _cell_angle_beta 75.343(4) _cell_angle_gamma 88.723(4) _cell_volume 8632.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 29.41 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ---- _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3178 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; measured in frozen drop of Apiezon fat (highly instable in air do to loss of solvent molecules ; _diffrn_ambient_temperature 180(1) _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 'KUMA (Poland)' _diffrn_measurement_method '.omega.-scan (0.5.degree)' _diffrn_detector_area_resol_mean '16.7 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75773 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 29.41 _reflns_number_total 40373 _reflns_number_gt 19038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA (Poland)' _computing_cell_refinement 'KUMA (Poland)' _computing_data_reduction 'KUMA (Poland)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 40373 _refine_ls_number_parameters 1873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1961 _refine_ls_R_factor_gt 0.1305 _refine_ls_wR_factor_ref 0.4005 _refine_ls_wR_factor_gt 0.3750 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.836 _refine_ls_shift/su_mean 0.046 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 C1A C 0.5262(3) 0.3096(2) 0.34982(18) 0.0516(10) Uani 1 1 d . . . C2A C 0.6060(3) 0.2976(2) 0.32436(19) 0.0568(11) Uani 1 1 d . . . H2X H 0.6106 0.2500 0.3294 0.068 Uiso 1 1 calc R . . H2Y H 0.6364 0.3100 0.3469 0.068 Uiso 1 1 calc R . . C3A C 0.6327(2) 0.3394(2) 0.25647(19) 0.0499(10) Uani 1 1 d . . . C4A C 0.6012(2) 0.3253(2) 0.21512(19) 0.0519(10) Uani 1 1 d . . . H4X H 0.5655 0.2899 0.2291 0.062 Uiso 1 1 calc R . . C5A C 0.6216(2) 0.3629(2) 0.15316(19) 0.0511(10) Uani 1 1 d . . . C6A C 0.6730(2) 0.4169(2) 0.13451(18) 0.0488(10) Uani 1 1 d . . . H6X H 0.6870 0.4428 0.0933 0.059 Uiso 1 1 calc R . . C7A C 0.7044(2) 0.4338(2) 0.17474(18) 0.0489(10) Uani 1 1 d . . . C8A C 0.7550(2) 0.4978(2) 0.15240(19) 0.0521(10) Uani 1 1 d . . . H8X H 0.7718 0.5027 0.1860 0.063 Uiso 1 1 calc R . . H8Y H 0.7975 0.4951 0.1206 0.063 Uiso 1 1 calc R . . C9A C 0.7125(2) 0.5574(2) 0.12756(18) 0.0497(10) Uani 1 1 d . . . C10A C 0.7172(3) 0.5854(2) 0.06515(19) 0.0534(10) Uani 1 1 d . . . H10X H 0.7533 0.5714 0.0379 0.064 Uiso 1 1 calc R . . C11A C 0.6714(3) 0.6324(2) 0.04187(18) 0.0513(10) Uani 1 1 d . A . C12A C 0.6199(3) 0.6531(2) 0.08439(19) 0.0520(10) Uani 1 1 d . . . H12X H 0.5884 0.6854 0.0700 0.062 Uiso 1 1 calc R . . C13A C 0.6128(3) 0.6286(2) 0.14650(18) 0.0499(10) Uani 1 1 d . . . C14A C 0.5513(3) 0.6496(2) 0.19056(19) 0.0571(11) Uani 1 1 d . . . H14X H 0.5705 0.6587 0.2214 0.069 Uiso 1 1 calc R . . H14Y H 0.5324 0.6909 0.1684 0.069 Uiso 1 1 calc R . . C15A C 0.4896(2) 0.5954(2) 0.22142(18) 0.0485(10) Uani 1 1 d . . . C16A C 0.4455(3) 0.5815(2) 0.1881(2) 0.0545(11) Uani 1 1 d . . . H16X H 0.4538 0.6071 0.1470 0.065 Uiso 1 1 calc R . . C17A C 0.3893(3) 0.5309(3) 0.2135(2) 0.0616(12) Uani 1 1 d . . . C18A C 0.3798(3) 0.4921(2) 0.2757(2) 0.0592(11) Uani 1 1 d . . . H18X H 0.3424 0.4580 0.2939 0.071 Uiso 1 1 calc R . . C19A C 0.4241(3) 0.5029(2) 0.31101(19) 0.0528(11) Uani 1 1 d . . . C20A C 0.4154(3) 0.4555(2) 0.3753(2) 0.0606(12) Uani 1 1 d . . . H20X H 0.3651 0.4542 0.3991 0.073 Uiso 1 1 calc R . . H20Y H 0.4474 0.4717 0.3945 0.073 Uiso 1 1 calc R . . C21A C 0.4343(3) 0.3852(2) 0.37469(17) 0.0538(11) Uani 1 1 d . . . C22A C 0.3784(3) 0.3354(2) 0.38866(18) 0.0575(11) Uani 1 1 d . . . H22X H 0.3296 0.3446 0.4012 0.069 Uiso 1 1 calc R . . C23A C 0.3956(3) 0.2713(2) 0.3839(2) 0.0624(12) Uani 1 1 d . . . C24A C 0.4699(3) 0.2605(2) 0.36436(18) 0.0560(11) Uani 1 1 d . . . H24X H 0.4823 0.2185 0.3609 0.067 Uiso 1 1 calc R . . C25A C 0.5082(3) 0.3720(2) 0.35616(17) 0.0521(10) Uani 1 1 d . . . C26A C 0.6838(2) 0.3935(2) 0.23556(18) 0.0498(10) Uani 1 1 d . . . C27A C 0.6610(2) 0.5806(2) 0.16820(18) 0.0499(10) Uani 1 1 d . . . C28A C 0.4771(2) 0.5558(2) 0.28286(18) 0.0497(10) Uani 1 1 d . . . O1A O 0.71129(17) 0.41052(15) 0.27844(13) 0.0558(7) Uani 1 1 d . . . O2A O 0.65680(18) 0.55258(16) 0.22930(12) 0.0572(8) Uani 1 1 d . . . H2A H 0.6175 0.5605 0.2493 0.069 Uiso 1 1 calc R . . O3A O 0.52293(17) 0.56877(14) 0.31646(12) 0.0524(7) Uani 1 1 d . . . O4A O 0.55895(18) 0.42247(15) 0.34425(13) 0.0572(8) Uani 1 1 d . . . H4A H 0.5448 0.4438 0.3679 0.069 Uiso 1 1 calc R . . C30A C 0.5862(3) 0.3490(2) 0.1062(2) 0.0579(11) Uani 1 1 d . . . C31A C 0.5248(4) 0.2948(3) 0.1360(3) 0.0890(18) Uani 1 1 d . . . H31X H 0.5059 0.2866 0.1050 0.107 Uiso 1 1 calc R . . H31Y H 0.4863 0.3092 0.1633 0.107 Uiso 1 1 calc R . . H31Z H 0.5429 0.2540 0.1586 0.107 Uiso 1 1 calc R . . C32A C 0.5594(4) 0.4135(3) 0.0689(3) 0.0838(17) Uani 1 1 d . . . H32X H 0.5097 0.4184 0.0892 0.101 Uiso 1 1 calc R . . H32Y H 0.5612 0.4114 0.0291 0.101 Uiso 1 1 calc R . . H32Z H 0.5902 0.4514 0.0649 0.101 Uiso 1 1 calc R . . C33A C 0.6465(4) 0.3239(4) 0.0621(3) 0.096(2) Uani 1 1 d . . . H33X H 0.6260 0.3150 0.0323 0.115 Uiso 1 1 calc R . . H33Y H 0.6645 0.2832 0.0850 0.115 Uiso 1 1 calc R . . H33Z H 0.6862 0.3579 0.0418 0.115 Uiso 1 1 calc R . . C40A C 0.6724(3) 0.6565(2) -0.02633(18) 0.0564(11) Uani 1 1 d . . . C41A C 0.7462(5) 0.6316(6) -0.0650(3) 0.054(2) Uani 0.574(11) 1 d P A 1 H41X H 0.7466 0.6460 -0.1075 0.065 Uiso 0.574(11) 1 calc PR A 1 H41Y H 0.7460 0.5833 -0.0497 0.065 Uiso 0.574(11) 1 calc PR A 1 H71Z H 0.7891 0.6511 -0.0604 0.065 Uiso 0.574(11) 1 calc PR A 1 C42A C 0.6781(6) 0.7306(4) -0.0519(3) 0.062(3) Uani 0.574(11) 1 d P A 1 H42X H 0.7241 0.7476 -0.0503 0.075 Uiso 0.574(11) 1 calc PR A 1 H42Y H 0.6384 0.7483 -0.0285 0.075 Uiso 0.574(11) 1 calc PR A 1 H42Z H 0.6754 0.7442 -0.0937 0.075 Uiso 0.574(11) 1 calc PR A 1 C43A C 0.6126(6) 0.6194(6) -0.0328(4) 0.051(2) Uani 0.574(11) 1 d P A 1 H43X H 0.6216 0.6208 -0.0746 0.061 Uiso 0.574(11) 1 calc PR A 1 H43Y H 0.5673 0.6396 -0.0216 0.061 Uiso 0.574(11) 1 calc PR A 1 H43Z H 0.6092 0.5733 -0.0066 0.061 Uiso 0.574(11) 1 calc PR A 1 C44A C 0.6066(8) 0.7170(7) -0.0396(5) 0.073(4) Uani 0.426(11) 1 d P A 2 H44X H 0.6172 0.7542 -0.0272 0.088 Uiso 0.426(11) 1 calc PR A 2 H44Y H 0.5585 0.6966 -0.0163 0.088 Uiso 0.426(11) 1 calc PR A 2 H44Z H 0.6083 0.7330 -0.0823 0.088 Uiso 0.426(11) 1 calc PR A 2 C45A C 0.7394(7) 0.6863(11) -0.0636(6) 0.087(6) Uani 0.426(11) 1 d P A 2 H45X H 0.7775 0.6573 -0.0530 0.105 Uiso 0.426(11) 1 calc PR A 2 H45Y H 0.7475 0.7288 -0.0583 0.105 Uiso 0.426(11) 1 calc PR A 2 H45Z H 0.7401 0.6937 -0.1055 0.105 Uiso 0.426(11) 1 calc PR A 2 C46A C 0.6441(10) 0.6006(10) -0.0429(7) 0.073(5) Uani 0.426(11) 1 d P A 2 H46X H 0.6318 0.6192 -0.0814 0.087 Uiso 0.426(11) 1 calc PR A 2 H46Y H 0.6010 0.5779 -0.0117 0.087 Uiso 0.426(11) 1 calc PR A 2 H46Z H 0.6812 0.5690 -0.0463 0.087 Uiso 0.426(11) 1 calc PR A 2 C50A C 0.3392(3) 0.5157(4) 0.1776(3) 0.0845(18) Uani 1 1 d . . . C51A C 0.3662(5) 0.5500(5) 0.1120(3) 0.150(4) Uani 1 1 d . . . H51X H 0.3258 0.5559 0.0935 0.080 Uiso 1 1 calc R . . H51Y H 0.4014 0.5234 0.0945 0.080 Uiso 1 1 calc R . . H51Z H 0.3890 0.5934 0.1048 0.080 Uiso 1 1 calc R . . C52A C 0.3377(6) 0.4386(5) 0.1868(4) 0.144(4) Uani 1 1 d . . . H52X H 0.2881 0.4193 0.2048 0.080 Uiso 1 1 calc R . . H52Y H 0.3679 0.4169 0.2135 0.080 Uiso 1 1 calc R . . H52Z H 0.3561 0.4320 0.1480 0.080 Uiso 1 1 calc R . . C53A C 0.2611(5) 0.5264(8) 0.2083(5) 0.191(6) Uani 1 1 d . . . H53X H 0.2300 0.4869 0.2168 0.229 Uiso 1 1 calc R . . H53Y H 0.2438 0.5648 0.1817 0.229 Uiso 1 1 calc R . . H53Z H 0.2600 0.5341 0.2460 0.229 Uiso 1 1 calc R . . C60A C 0.3361(3) 0.2157(3) 0.3997(3) 0.0822(16) Uani 1 1 d . . . C61A C 0.3487(6) 0.1761(6) 0.3608(5) 0.194(6) Uani 1 1 d . . . H61X H 0.3794 0.2019 0.3215 0.080 Uiso 1 1 calc R . . H61Y H 0.3027 0.1629 0.3562 0.080 Uiso 1 1 calc R . . H61Z H 0.3727 0.1365 0.3783 0.080 Uiso 1 1 calc R . . C62A C 0.3342(7) 0.1669(6) 0.4636(4) 0.213(7) Uani 1 1 d . . . H62X H 0.3576 0.1267 0.4600 0.080 Uiso 1 1 calc R . . H62Y H 0.2842 0.1553 0.4872 0.080 Uiso 1 1 calc R . . H62Z H 0.3598 0.1881 0.4836 0.080 Uiso 1 1 calc R . . C63A C 0.2589(5) 0.2347(6) 0.4214(6) 0.174(5) Uani 1 1 d . . . H63X H 0.2405 0.2577 0.3867 0.209 Uiso 1 1 calc R . . H63Y H 0.2589 0.2638 0.4452 0.209 Uiso 1 1 calc R . . H63Z H 0.2280 0.1945 0.4461 0.209 Uiso 1 1 calc R . . C70A C 0.7741(3) 0.3749(3) 0.2922(2) 0.0668(13) Uani 1 1 d . B . H70X H 0.8183 0.3962 0.2608 0.080 Uiso 1 1 calc R . . H70Y H 0.7685 0.3285 0.2935 0.080 Uiso 1 1 calc R . . P1A P 0.78083(10) 0.37683(11) 0.36427(7) 0.0880(5) Uani 1 1 d . . . O11A O 0.7136(3) 0.3556(3) 0.41270(19) 0.1147(17) Uani 1 1 d . B . O12A O 0.8473(2) 0.3359(3) 0.37547(17) 0.1084(16) Uani 1 1 d . B . O13A O 0.8043(8) 0.4445(4) 0.3524(4) 0.204(5) Uani 1 1 d . B . C80A C 0.4945(3) 0.6153(2) 0.34820(19) 0.0584(12) Uani 1 1 d . . . H80X H 0.4474 0.5975 0.3770 0.070 Uiso 1 1 calc R . . H80Y H 0.4879 0.6583 0.3194 0.070 Uiso 1 1 calc R . . P2A P 0.55978(11) 0.62561(8) 0.38757(7) 0.0853(5) Uani 1 1 d . . . O21A O 0.6306(4) 0.6577(3) 0.3464(3) 0.155(3) Uani 1 1 d . . . O22A O 0.5139(4) 0.6671(2) 0.4264(2) 0.140(2) Uani 1 1 d . . . O23A O 0.5629(2) 0.5566(2) 0.43663(16) 0.0858(12) Uani 1 1 d . . . C71A C 0.8181(13) 0.4863(19) 0.3266(11) 0.32(3) Uani 0.550(13) 1 d P B 1 H71X H 0.7834 0.4943 0.3015 0.080 Uiso 0.550(13) 1 calc PR B 1 H71Y H 0.8643 0.4805 0.3001 0.080 Uiso 0.550(13) 1 calc PR B 1 C72A C 0.8309(13) 0.5573(12) 0.3317(12) 0.196(11) Uani 0.550(13) 1 d P B 1 H72X H 0.8776 0.5776 0.3050 0.236 Uiso 0.550(13) 1 calc PR B 1 H72Y H 0.8303 0.5524 0.3731 0.236 Uiso 0.550(13) 1 calc PR B 1 H72Z H 0.7926 0.5854 0.3200 0.236 Uiso 0.550(13) 1 calc PR B 1 C73A C 0.8396(12) 0.4820(13) 0.3897(11) 0.141(9) Uani 0.450(13) 1 d P B 2 H73X H 0.8101 0.5201 0.3917 0.170 Uiso 0.450(13) 1 calc PR B 2 H73Y H 0.8298 0.4508 0.4313 0.170 Uiso 0.450(13) 1 calc PR B 2 C74A C 0.9133(14) 0.5070(14) 0.3744(13) 0.191(13) Uani 0.450(13) 1 d P B 2 H74X H 0.9348 0.5158 0.3314 0.080 Uiso 0.450(13) 1 calc PR B 2 H74Y H 0.9403 0.4740 0.3975 0.080 Uiso 0.450(13) 1 calc PR B 2 H74Z H 0.9150 0.5480 0.3837 0.080 Uiso 0.450(13) 1 calc PR B 2 C75A C 0.8349(6) 0.2603(8) 0.4100(5) 0.242(10) Uani 1 1 d . . . H75X H 0.8592 0.2547 0.4423 0.290 Uiso 1 1 calc R B . H75Y H 0.7828 0.2552 0.4303 0.290 Uiso 1 1 calc R . . C76A C 0.8450(15) 0.2109(7) 0.3990(8) 0.40(2) Uani 1 1 d . B . H76X H 0.8642 0.2211 0.3556 0.476 Uiso 1 1 calc R . . H76Y H 0.7996 0.1839 0.4125 0.476 Uiso 1 1 calc R . . H76Z H 0.8797 0.1864 0.4197 0.476 Uiso 1 1 calc R . . C81A C 0.6158(4) 0.5103(4) 0.4248(3) 0.095(2) Uani 1 1 d . . . H81X H 0.6586 0.5347 0.3934 0.114 Uiso 1 1 calc R . . H81Y H 0.5953 0.4792 0.4095 0.114 Uiso 1 1 calc R . . C82A C 0.6379(5) 0.4718(4) 0.4805(3) 0.114(3) Uani 1 1 d . . . H82X H 0.6868 0.4579 0.4693 0.137 Uiso 1 1 calc R . . H82Y H 0.6046 0.4326 0.5030 0.137 Uiso 1 1 calc R . . H82Z H 0.6366 0.4998 0.5055 0.137 Uiso 1 1 calc R . . C83A C 0.5371(9) 0.6835(5) 0.4736(5) 0.246(9) Uani 1 1 d . . . H83X H 0.5153 0.6485 0.5122 0.080 Uiso 1 1 calc R . . H83Y H 0.5899 0.6803 0.4656 0.080 Uiso 1 1 calc R . . C84A C 0.5237(5) 0.7374(3) 0.4808(3) 0.111(3) Uani 1 1 d . . . H84X H 0.5648 0.7546 0.4897 0.080 Uiso 1 1 calc R . . H84Y H 0.4809 0.7316 0.5143 0.080 Uiso 1 1 calc R . . H84Z H 0.5149 0.7686 0.4442 0.080 Uiso 1 1 calc R . . C1B C 0.8167(2) 0.1177(2) 0.28847(17) 0.0456(9) Uani 1 1 d . . . C2B C 0.8724(2) 0.0773(2) 0.31959(19) 0.0543(11) Uani 1 1 d . . . H2T H 0.8486 0.0360 0.3510 0.065 Uiso 1 1 calc R . . H2U H 0.8939 0.1035 0.3387 0.065 Uiso 1 1 calc R . . C3B C 0.9321(2) 0.0609(2) 0.27015(17) 0.0451(9) Uani 1 1 d . . . C4B C 0.9129(2) 0.0256(2) 0.23630(18) 0.0475(9) Uani 1 1 d . . . H4T H 0.8651 0.0066 0.2479 0.057 Uiso 1 1 calc R . . C5B C 0.9617(2) 0.0170(2) 0.18567(18) 0.0473(9) Uani 1 1 d . . . C6B C 1.0328(2) 0.0451(2) 0.17070(18) 0.0454(9) Uani 1 1 d . . . H6T H 1.0670 0.0391 0.1375 0.054 Uiso 1 1 calc R . . C7B C 1.05504(19) 0.0820(2) 0.20307(18) 0.0433(9) Uani 1 1 d . . . C8B C 1.1308(2) 0.1180(2) 0.17997(19) 0.0481(10) Uani 1 1 d . . . H8T H 1.1679 0.0852 0.1848 0.058 Uiso 1 1 calc R . . H8U H 1.1348 0.1472 0.2035 0.058 Uiso 1 1 calc R . . C9B C 1.14341(19) 0.1598(2) 0.1130(2) 0.0479(10) Uani 1 1 d . . . C10B C 1.1853(2) 0.1369(3) 0.0682(2) 0.0550(11) Uani 1 1 d . . . H10T H 1.2105 0.0981 0.0795 0.066 Uiso 1 1 calc R . . C11B C 1.1910(2) 0.1705(3) 0.0057(2) 0.0616(12) Uani 1 1 d . . . C12B C 1.1523(2) 0.2289(3) -0.0087(2) 0.0588(12) Uani 1 1 d . . . H12T H 1.1555 0.2528 -0.0496 0.071 Uiso 1 1 calc R . . C13B C 1.1088(2) 0.2523(2) 0.0364(2) 0.0551(11) Uani 1 1 d . . . C14B C 1.0649(2) 0.3140(3) 0.0176(2) 0.0637(12) Uani 1 1 d . . . H14T H 1.0736 0.3460 0.0372 0.076 Uiso 1 1 calc R . . H14U H 1.0812 0.3360 -0.0264 0.076 Uiso 1 1 calc R . . C15B C 0.9833(2) 0.2936(2) 0.0359(2) 0.0526(10) Uani 1 1 d . . . C16B C 0.9555(2) 0.2601(2) 0.0030(2) 0.0562(11) Uani 1 1 d . . . H16T H 0.9873 0.2528 -0.0308 0.067 Uiso 1 1 calc R . . C17B C 0.8816(2) 0.2372(2) 0.0193(2) 0.0560(11) Uani 1 1 d . . . C18B C 0.8373(2) 0.2463(2) 0.0723(2) 0.0549(11) Uani 1 1 d . . . H18T H 0.7884 0.2300 0.0850 0.066 Uiso 1 1 calc R . . C19B C 0.8617(2) 0.2778(2) 0.10657(19) 0.0484(10) Uani 1 1 d . . . C20B C 0.8111(2) 0.2850(2) 0.1650(2) 0.0521(10) Uani 1 1 d . . . H20T H 0.8365 0.3127 0.1803 0.063 Uiso 1 1 calc R . . H20U H 0.7679 0.3075 0.1557 0.063 Uiso 1 1 calc R . . C21B C 0.7879(2) 0.2172(2) 0.21327(19) 0.0456(9) Uani 1 1 d . . . C22B C 0.7197(2) 0.1834(2) 0.2239(2) 0.0495(10) Uani 1 1 d . . . H22T H 0.6864 0.2059 0.2027 0.059 Uiso 1 1 calc R . . C23B C 0.6992(2) 0.1178(2) 0.2644(2) 0.0472(10) Uani 1 1 d . . . C24B C 0.7491(2) 0.0862(2) 0.29674(19) 0.0468(9) Uani 1 1 d . . . H24T H 0.7368 0.0428 0.3247 0.056 Uiso 1 1 calc R . . C25B C 0.8355(2) 0.1828(2) 0.24738(18) 0.0430(9) Uani 1 1 d . . . C26B C 1.0043(2) 0.0874(2) 0.25396(18) 0.0432(9) Uani 1 1 d . . . C27B C 1.1057(2) 0.2183(2) 0.0966(2) 0.0486(10) Uani 1 1 d . . . C28B C 0.9349(2) 0.3030(2) 0.08597(19) 0.0478(9) Uani 1 1 d . . . O1B O 1.02360(14) 0.12471(15) 0.28688(13) 0.0511(7) Uani 1 1 d . . . O2B O 1.06689(15) 0.23862(15) 0.14450(13) 0.0534(7) Uani 1 1 d . . . H2B H 1.0547 0.2772 0.1310 0.064 Uiso 1 1 calc R . . O3B O 0.96189(16) 0.33735(14) 0.11851(14) 0.0543(7) Uani 1 1 d . . . O4B O 0.90192(14) 0.21638(15) 0.23834(13) 0.0501(7) Uani 1 1 d . . . H4B H 0.9217 0.2319 0.2016 0.060 Uiso 1 1 calc R . . C30B C 0.9386(2) -0.0196(3) 0.1458(2) 0.0638(13) Uani 1 1 d . . . C31B C 0.8562(3) -0.0363(4) 0.1636(3) 0.104(2) Uani 1 1 d . . . H31T H 0.8447 -0.0596 0.1381 0.124 Uiso 1 1 calc R . . H31U H 0.8312 0.0048 0.1581 0.124 Uiso 1 1 calc R . . H31V H 0.8408 -0.0645 0.2056 0.124 Uiso 1 1 calc R . . C32B C 0.9748(6) -0.0856(5) 0.1547(6) 0.191(6) Uani 1 1 d . . . H32T H 0.9548 -0.1120 0.1355 0.229 Uiso 1 1 calc R . . H32U H 0.9661 -0.1099 0.1976 0.229 Uiso 1 1 calc R . . H32V H 1.0268 -0.0768 0.1365 0.229 Uiso 1 1 calc R . . C33B C 0.9590(4) 0.0298(5) 0.0790(3) 0.129(3) Uani 1 1 d . . . H33T H 0.9405 0.0109 0.0535 0.155 Uiso 1 1 calc R . . H33U H 1.0115 0.0371 0.0642 0.155 Uiso 1 1 calc R . . H33V H 0.9378 0.0721 0.0779 0.155 Uiso 1 1 calc R . . C40B C 1.2372(3) 0.1432(3) -0.0422(2) 0.0738(15) Uani 1 1 d . . . C41B C 1.2328(4) 0.1827(5) -0.1062(3) 0.116(3) Uani 1 1 d . . . H41T H 1.2583 0.2263 -0.1192 0.140 Uiso 1 1 calc R . . H41U H 1.1823 0.1883 -0.1067 0.140 Uiso 1 1 calc R . . H41V H 1.2551 0.1586 -0.1335 0.140 Uiso 1 1 calc R . . C42B C 1.3181(2) 0.1448(3) -0.0410(3) 0.0799(16) Uani 1 1 d . . . H42T H 1.3378 0.1908 -0.0560 0.096 Uiso 1 1 calc R . . H42U H 1.3454 0.1206 -0.0664 0.096 Uiso 1 1 calc R . . H42V H 1.3217 0.1240 0.0003 0.096 Uiso 1 1 calc R . . C43B C 1.2082(3) 0.0689(4) -0.0280(3) 0.101(2) Uani 1 1 d . . . H43T H 1.2356 0.0515 -0.0590 0.121 Uiso 1 1 calc R . . H43U H 1.1571 0.0680 -0.0276 0.121 Uiso 1 1 calc R . . H43V H 1.2139 0.0414 0.0112 0.121 Uiso 1 1 calc R . . C50B C 0.8490(3) 0.2065(3) -0.0190(2) 0.0700(14) Uani 1 1 d . . . C51B C 0.8012(3) 0.1418(3) 0.0214(3) 0.0890(18) Uani 1 1 d . . . H51T H 0.7824 0.1227 -0.0038 0.107 Uiso 1 1 calc R . . H51U H 0.7610 0.1524 0.0501 0.107 Uiso 1 1 calc R . . H51V H 0.8302 0.1099 0.0432 0.107 Uiso 1 1 calc R . . C52B C 0.8004(3) 0.2567(3) -0.0512(3) 0.0822(16) Uani 1 1 d . . . H52T H 0.7626 0.2681 -0.0212 0.099 Uiso 1 1 calc R . . H52U H 0.7783 0.2368 -0.0741 0.099 Uiso 1 1 calc R . . H52V H 0.8297 0.2969 -0.0784 0.099 Uiso 1 1 calc R . . C53B C 0.9078(3) 0.1896(4) -0.0683(3) 0.106(2) Uani 1 1 d . . . H53T H 0.9315 0.2307 -0.0989 0.127 Uiso 1 1 calc R . . H53U H 0.8852 0.1641 -0.0868 0.127 Uiso 1 1 calc R . . H53V H 0.9435 0.1634 -0.0500 0.127 Uiso 1 1 calc R . . C60B C 0.6256(2) 0.0827(2) 0.2722(2) 0.0570(11) Uani 1 1 d . . . C61B C 0.5631(2) 0.1225(2) 0.2955(2) 0.0583(11) Uani 1 1 d . . . H61T H 0.5170 0.0981 0.3039 0.070 Uiso 1 1 calc R . . H61U H 0.5644 0.1658 0.2650 0.070 Uiso 1 1 calc R . . H61V H 0.5686 0.1286 0.3323 0.070 Uiso 1 1 calc R . . C62B C 0.6148(3) 0.0106(3) 0.3193(3) 0.0828(17) Uani 1 1 d . . . H62T H 0.6509 -0.0172 0.3044 0.099 Uiso 1 1 calc R . . H62U H 0.5666 -0.0083 0.3251 0.099 Uiso 1 1 calc R . . H62V H 0.6203 0.0125 0.3576 0.099 Uiso 1 1 calc R . . C63B C 0.6221(3) 0.0794(4) 0.2102(3) 0.0859(18) Uani 1 1 d . . . H63T H 0.6620 0.0548 0.1955 0.103 Uiso 1 1 calc R . . H63U H 0.6259 0.1244 0.1817 0.103 Uiso 1 1 calc R . . H63V H 0.5763 0.0570 0.2145 0.103 Uiso 1 1 calc R . . C70B C 1.0595(3) 0.0843(3) 0.3324(2) 0.0678(13) Uani 1 1 d . . . H70T H 1.0973 0.0600 0.3135 0.081 Uiso 1 1 calc R . . H70U H 1.0238 0.0513 0.3648 0.081 Uiso 1 1 calc R . . P1B P 1.09957(16) 0.13486(13) 0.36410(10) 0.1187(7) Uani 1 1 d . . . O11B O 1.1368(5) 0.0907(3) 0.4071(3) 0.189(3) Uani 1 1 d . . . O12B O 1.1518(3) 0.1901(3) 0.3132(2) 0.1042(14) Uani 1 1 d . . . O13B O 1.0385(4) 0.1675(4) 0.3913(3) 0.148(2) Uani 1 1 d . . . C80B C 0.9543(3) 0.4085(2) 0.0963(3) 0.0744(15) Uani 1 1 d . . . H80T H 0.9028 0.4179 0.1033 0.089 Uiso 1 1 calc R . . H80U H 0.9774 0.4266 0.0528 0.089 Uiso 1 1 calc R . . P2B P 0.99829(9) 0.44582(8) 0.13727(9) 0.0851(5) Uani 1 1 d . . . O21B O 1.0767(2) 0.4374(2) 0.1262(2) 0.1017(14) Uani 1 1 d . . . O22B O 0.9719(3) 0.5180(3) 0.1185(3) 0.129(2) Uani 1 1 d . . . O23B O 0.9568(2) 0.4171(3) 0.2048(2) 0.1039(14) Uani 1 1 d . . . C71B C 1.1266(6) 0.2496(4) 0.2719(6) 0.155(4) Uani 1 1 d . . . H71T H 1.1084 0.2367 0.2424 0.186 Uiso 1 1 calc R . . H71U H 1.0869 0.2682 0.2953 0.186 Uiso 1 1 calc R . . C72B C 1.1871(5) 0.2995(6) 0.2406(5) 0.156(4) Uani 1 1 d . . . H72T H 1.1686 0.3435 0.2284 0.187 Uiso 1 1 calc R . . H72U H 1.2154 0.2901 0.2050 0.187 Uiso 1 1 calc R . . H72V H 1.2177 0.2981 0.2675 0.187 Uiso 1 1 calc R . . C73B C 1.0389 0.2082 0.4350 0.100 Uiso 1 1 d . . . H73T H 0.9877 0.1984 0.4579 0.080 Uiso 1 1 calc R . . H73U H 1.0648 0.1770 0.4615 0.080 Uiso 1 1 calc R . . C74B C 1.0505(4) 0.2588(3) 0.4474(3) 0.100 Uiso 1 1 d . . . H74T H 1.0079 0.2847 0.4483 0.080 Uiso 1 1 calc R . . H74U H 1.0917 0.2856 0.4168 0.080 Uiso 1 1 calc R . . H74V H 1.0609 0.2455 0.4867 0.080 Uiso 1 1 calc R . . C81B C 0.9904(7) 0.5679(6) 0.1428(7) 0.178(5) Uani 1 1 d . . . H81T H 1.0163 0.5462 0.1736 0.080 Uiso 1 1 calc R . . H81U H 1.0245 0.6020 0.1100 0.080 Uiso 1 1 calc R . . C82B C 0.9371(8) 0.5985(6) 0.1670(5) 0.193(6) Uani 1 1 d . . . H82T H 0.9135 0.5699 0.2078 0.080 Uiso 1 1 calc R . . H82U H 0.9021 0.6083 0.1429 0.080 Uiso 1 1 calc R . . H82V H 0.9561 0.6399 0.1684 0.080 Uiso 1 1 calc R . . C83B C 0.9857(4) 0.3639(5) 0.2478(4) 0.114(2) Uani 1 1 d . . . H83T H 1.0235 0.3421 0.2259 0.136 Uiso 1 1 calc R . . H83U H 0.9468 0.3301 0.2745 0.136 Uiso 1 1 calc R . . C84B C 1.0172(5) 0.3964(6) 0.2844(5) 0.157(4) Uani 1 1 d . . . H84T H 0.9825 0.4253 0.2989 0.188 Uiso 1 1 calc R . . H84U H 1.0618 0.4226 0.2590 0.188 Uiso 1 1 calc R . . H84V H 1.0277 0.3620 0.3186 0.188 Uiso 1 1 calc R . . C1C C 0.2461(2) 0.8706(2) 0.15094(17) 0.0424(9) Uani 1 1 d . . . C2C C 0.1869(2) 0.9151(2) 0.17110(19) 0.0459(9) Uani 1 1 d . . . H2P H 0.1807 0.9512 0.1355 0.055 Uiso 1 1 calc R . . H2R H 0.1406 0.8884 0.1908 0.055 Uiso 1 1 calc R . . C3C C 0.20699(19) 0.94529(19) 0.21506(16) 0.0375(8) Uani 1 1 d . . . C4C C 0.26507(19) 0.9933(2) 0.19437(16) 0.0394(8) Uani 1 1 d . . . H4P H 0.2914 1.0057 0.1535 0.047 Uiso 1 1 calc R . . C5C C 0.2860(2) 1.0241(2) 0.23223(16) 0.0435(9) Uani 1 1 d . . . C6C C 0.2472(2) 1.0008(2) 0.29434(17) 0.0454(9) Uani 1 1 d . . . H6P H 0.2601 1.0198 0.3208 0.054 Uiso 1 1 calc R . . C7C C 0.1909(2) 0.9511(2) 0.31771(17) 0.0457(9) Uani 1 1 d . . . C8C C 0.1576(3) 0.9242(2) 0.38691(17) 0.0587(12) Uani 1 1 d . . . H8P H 0.1421 0.9615 0.4018 0.070 Uiso 1 1 calc R . . H8R H 0.1148 0.8940 0.3963 0.070 Uiso 1 1 calc R . . C9C C 0.2136(2) 0.8869(2) 0.41801(17) 0.0551(12) Uani 1 1 d . . . C10C C 0.2527(3) 0.9173(2) 0.44580(17) 0.0594(12) Uani 1 1 d . . . H10P H 0.2407 0.9600 0.4477 0.071 Uiso 1 1 calc R . . C11C C 0.3089(3) 0.8869(3) 0.47077(19) 0.0631(13) Uani 1 1 d . . . C12C C 0.3242(3) 0.8227(2) 0.46757(18) 0.0596(12) Uani 1 1 d . . . H12P H 0.3611 0.8007 0.4844 0.071 Uiso 1 1 calc R . . C13C C 0.2868(3) 0.7899(2) 0.44034(18) 0.0574(12) Uani 1 1 d . . . C14C C 0.3087(3) 0.7227(2) 0.43235(19) 0.0610(12) Uani 1 1 d . . . H14P H 0.3383 0.7007 0.4601 0.073 Uiso 1 1 calc R . . H14R H 0.2651 0.6934 0.4419 0.073 Uiso 1 1 calc R . . C15C C 0.3521(3) 0.7344(2) 0.36694(19) 0.0539(11) Uani 1 1 d . . . C16C C 0.4154(3) 0.7752(2) 0.34185(19) 0.0581(12) Uani 1 1 d . . . H16P H 0.4345 0.7915 0.3672 0.070 Uiso 1 1 calc R . . C17C C 0.4531(3) 0.7938(2) 0.27946(18) 0.0533(11) Uani 1 1 d . . . C18C C 0.4223(3) 0.7678(2) 0.2435(2) 0.0560(11) Uani 1 1 d . . . H18P H 0.4457 0.7790 0.2021 0.067 Uiso 1 1 calc R . . C19C C 0.3590(3) 0.7263(2) 0.2664(2) 0.0569(11) Uani 1 1 d . . . C20C C 0.3238(3) 0.7053(3) 0.2228(2) 0.0670(13) Uani 1 1 d . . . H20P H 0.3562 0.6775 0.2034 0.080 Uiso 1 1 calc R . . H20R H 0.2776 0.6793 0.2455 0.080 Uiso 1 1 calc R . . C21C C 0.3110(2) 0.7687(2) 0.1751(2) 0.0547(11) Uani 1 1 d . . . C22C C 0.3588(2) 0.7937(2) 0.1170(2) 0.0536(11) Uani 1 1 d . . . H22P H 0.3964 0.7673 0.1057 0.064 Uiso 1 1 calc R . . C23C C 0.3532(2) 0.8565(2) 0.07459(18) 0.0479(10) Uani 1 1 d . . . C24C C 0.2953(2) 0.8934(2) 0.09346(17) 0.0439(9) Uani 1 1 d . . . H24P H 0.2893 0.9353 0.0664 0.053 Uiso 1 1 calc R . . C25C C 0.2535(2) 0.8068(2) 0.19135(19) 0.0496(10) Uani 1 1 d . . . C26C C 0.1704(2) 0.9251(2) 0.27788(18) 0.0441(9) Uani 1 1 d . . . C27C C 0.2306(3) 0.8221(2) 0.41577(18) 0.0551(11) Uani 1 1 d . . . C28C C 0.3243(3) 0.7099(2) 0.3285(2) 0.0574(11) Uani 1 1 d . . . O1C O 0.11268(15) 0.87428(14) 0.30078(13) 0.0541(7) Uani 1 1 d . . . O2C O 0.19165(17) 0.79051(15) 0.39041(14) 0.0584(8) Uani 1 1 d . . . H2C H 0.2125 0.7572 0.3856 0.070 Uiso 1 1 calc R . . O3C O 0.25776(18) 0.67047(17) 0.35242(16) 0.0698(9) Uani 1 1 d . . . O4C O 0.20606(16) 0.78308(15) 0.24867(13) 0.0547(7) Uani 1 1 d . . . H4C H 0.2187 0.7466 0.2679 0.066 Uiso 1 1 calc R . . C30C C 0.3455(2) 1.0812(2) 0.20902(19) 0.0515(10) Uani 1 1 d . . . C31C C 0.4000(3) 1.0665(3) 0.2483(3) 0.0810(16) Uani 1 1 d . . . H31P H 0.4329 1.0342 0.2376 0.097 Uiso 1 1 calc R . . H31R H 0.3739 1.0484 0.2907 0.097 Uiso 1 1 calc R . . H31S H 0.4276 1.1075 0.2413 0.097 Uiso 1 1 calc R . . C32C C 0.3103(3) 1.1458(2) 0.2149(2) 0.0652(12) Uani 1 1 d . . . H32P H 0.2701 1.1348 0.2510 0.078 Uiso 1 1 calc R . . H32R H 0.2926 1.1677 0.1795 0.078 Uiso 1 1 calc R . . H32S H 0.3462 1.1755 0.2178 0.078 Uiso 1 1 calc R . . C33C C 0.3867(3) 1.0932(3) 0.1431(2) 0.0807(16) Uani 1 1 d . . . H33P H 0.4208 1.1318 0.1291 0.097 Uiso 1 1 calc R . . H33R H 0.3525 1.1011 0.1182 0.097 Uiso 1 1 calc R . . H33S H 0.4130 1.0542 0.1400 0.097 Uiso 1 1 calc R . . C40C C 0.3555(4) 0.9247(3) 0.4971(2) 0.0792(16) Uani 1 1 d . . . C41C C 0.3861(8) 0.8757(5) 0.5440(6) 0.249(9) Uani 1 1 d . . . H41P H 0.3724 0.8863 0.5813 0.080 Uiso 1 1 calc R . . H41R H 0.4387 0.8783 0.5297 0.080 Uiso 1 1 calc R . . H41S H 0.3669 0.8308 0.5514 0.080 Uiso 1 1 calc R . . C42C C 0.3065(5) 0.9683(4) 0.5281(4) 0.120(3) Uani 1 1 d . . . H42P H 0.2896 1.0034 0.4981 0.144 Uiso 1 1 calc R . . H42R H 0.3337 0.9882 0.5479 0.144 Uiso 1 1 calc R . . H42S H 0.2650 0.9410 0.5580 0.144 Uiso 1 1 calc R . . C43C C 0.4140(5) 0.9658(6) 0.4460(4) 0.163(5) Uani 1 1 d . . . H43P H 0.4303 0.9424 0.4170 0.196 Uiso 1 1 calc R . . H43R H 0.4544 0.9741 0.4609 0.196 Uiso 1 1 calc R . . H43S H 0.3958 1.0081 0.4264 0.196 Uiso 1 1 calc R . . C50C C 0.5208(3) 0.8427(2) 0.2513(2) 0.0686(14) Uani 1 1 d . . . C51C C 0.5841(5) 0.8102(5) 0.2207(5) 0.163(5) Uani 1 1 d . . . H51P H 0.5774 0.8096 0.1823 0.196 Uiso 1 1 calc R . . H51R H 0.5860 0.7647 0.2466 0.196 Uiso 1 1 calc R . . H51S H 0.6292 0.8355 0.2135 0.196 Uiso 1 1 calc R . . C52C C 0.5475(5) 0.8601(5) 0.3004(3) 0.151(4) Uani 1 1 d . . . H52P H 0.5993 0.8547 0.2940 0.080 Uiso 1 1 calc R . . H52R H 0.5220 0.8304 0.3402 0.080 Uiso 1 1 calc R . . H52S H 0.5379 0.9060 0.2977 0.080 Uiso 1 1 calc R . . C53C C 0.5042(7) 0.9047(4) 0.2083(5) 0.193(5) Uani 1 1 d . . . H53P H 0.5243 0.9046 0.1672 0.080 Uiso 1 1 calc R . . H53R H 0.5256 0.9429 0.2134 0.080 Uiso 1 1 calc R . . H53S H 0.4520 0.9075 0.2158 0.080 Uiso 1 1 calc R . . C60C C 0.4100(2) 0.8820(3) 0.0130(2) 0.0597(12) Uani 1 1 d . . . C61C C 0.4135(3) 0.8293(3) -0.0207(2) 0.0755(15) Uani 1 1 d . . . H61P H 0.4509 0.8443 -0.0587 0.091 Uiso 1 1 calc R . . H61R H 0.3669 0.8246 -0.0287 0.091 Uiso 1 1 calc R . . H61S H 0.4249 0.7865 0.0046 0.091 Uiso 1 1 calc R . . C62C C 0.3942(3) 0.9492(3) -0.0286(2) 0.0780(15) Uani 1 1 d . . . H62P H 0.3911 0.9823 -0.0083 0.094 Uiso 1 1 calc R . . H62R H 0.3484 0.9447 -0.0381 0.094 Uiso 1 1 calc R . . H62S H 0.4330 0.9633 -0.0657 0.094 Uiso 1 1 calc R . . C63C C 0.4861(3) 0.8888(4) 0.0237(2) 0.0869(19) Uani 1 1 d . . . H63P H 0.4840 0.9168 0.0489 0.104 Uiso 1 1 calc R . . H63R H 0.5213 0.9091 -0.0149 0.104 Uiso 1 1 calc R . . H63S H 0.5005 0.8449 0.0439 0.104 Uiso 1 1 calc R . . C70C C 0.0411(2) 0.8997(2) 0.3063(2) 0.0616(12) Uani 1 1 d . . . H70P H 0.0344 0.9243 0.2662 0.074 Uiso 1 1 calc R . . H70R H 0.0346 0.9299 0.3302 0.074 Uiso 1 1 calc R . . P1C P -0.02368(9) 0.82813(11) 0.34363(15) 0.1326(11) Uani 1 1 d . . . O11C O -0.0155(4) 0.7818(4) 0.3047(5) 0.192(4) Uani 1 1 d . . . O12C O -0.0983(2) 0.8631(2) 0.3459(3) 0.124(2) Uani 1 1 d . . . O13C O -0.0158(3) 0.7921(3) 0.4059(3) 0.159(3) Uani 1 1 d . . . C80C C 0.2672(4) 0.5990(3) 0.3727(3) 0.0941(19) Uani 1 1 d . . . H80P H 0.2879 0.5868 0.4078 0.113 Uiso 1 1 calc R . . H80R H 0.3002 0.5864 0.3403 0.113 Uiso 1 1 calc R . . P2C P 0.17945(19) 0.55740(15) 0.3929(2) 0.1838(18) Uani 1 1 d . . . O21C C 0.1303(6) 0.5773(4) 0.4430(5) 0.173(5) Uani 1 1 d . . . O22C C 0.1498(5) 0.5793(7) 0.3329(9) 0.173(5) Uani 1 1 d . . . O23C C 0.1982(6) 0.4862(4) 0.4050(8) 0.237(9) Uani 1 1 d . . . C71C C -0.1689(4) 0.8256(6) 0.3763(7) 0.229(8) Uani 1 1 d . . . H71P H -0.1727 0.8035 0.4195 0.274 Uiso 1 1 calc R . . H71R H -0.1750 0.7914 0.3583 0.274 Uiso 1 1 calc R . . C72C C -0.2256(4) 0.8752(6) 0.3680(6) 0.209(7) Uani 1 1 d . . . H72P H -0.2323 0.8855 0.3275 0.251 Uiso 1 1 calc R . . H72R H -0.2101 0.9158 0.3732 0.251 Uiso 1 1 calc R . . H72S H -0.2711 0.8565 0.3977 0.251 Uiso 1 1 calc R . . C73C C 0.0119(10) 0.7369(9) 0.4217(7) 0.296(12) Uani 1 1 d . . . H73P H 0.0603 0.7388 0.3946 0.080 Uiso 1 1 calc R . . H73R H -0.0185 0.7015 0.4193 0.080 Uiso 1 1 calc R . . C74C C 0.9832(4) 0.2766(4) 0.5216(3) 0.100 Uiso 1 1 d . . . H74P H 0.9364 0.2943 0.5183 0.080 Uiso 1 1 calc R . . H74R H 0.9877 0.2360 0.5111 0.080 Uiso 1 1 calc R . . H74S H 1.0218 0.3094 0.4942 0.080 Uiso 1 1 calc R . . C81C C 0.1241(14) 0.6361(11) 0.2930(10) 0.338(14) Uiso 1 1 d . . . H81P H 0.1631 0.6716 0.2781 0.080 Uiso 1 1 calc R . . H81R H 0.0835 0.6510 0.3189 0.080 Uiso 1 1 calc R . . C82C C 0.0989(10) 0.6366(12) 0.2383(8) 0.57(4) Uani 1 1 d . . . H82P H 0.1012 0.5922 0.2348 0.080 Uiso 1 1 calc R . . H82R H 0.1302 0.6681 0.2020 0.080 Uiso 1 1 calc R . . H82C H 0.0492 0.6498 0.2429 0.080 Uiso 1 1 calc R . . C83C C 0.1500(17) 0.4360(16) 0.4382(14) 1.45(16) Uani 1 1 d . . . H83P H 0.1034 0.4511 0.4564 0.080 Uiso 1 1 calc R . . H83R H 0.1679 0.4031 0.4698 0.080 Uiso 1 1 calc R . . C84C C 0.1456(8) 0.4087(10) 0.3834(7) 0.350(15) Uani 1 1 d . . . H84P H 0.1024 0.4239 0.3700 0.080 Uiso 1 1 calc R . . H84R H 0.1433 0.3602 0.3977 0.080 Uiso 1 1 calc R . . H84S H 0.1884 0.4257 0.3498 0.080 Uiso 1 1 calc R . . O1SS O 0.8475(5) 0.4931(5) 0.9911(3) 0.184(3) Uani 1 1 d . . . C1SS C 0.8327(5) 0.4324(5) 0.9867(4) 0.128(3) Uani 1 1 d . . . H1S1 H 0.8778 0.4137 0.9723 0.080 Uiso 1 1 calc R . . H1S2 H 0.8029 0.4379 0.9586 0.080 Uiso 1 1 calc R . . H1S3 H 0.8068 0.4024 1.0263 0.080 Uiso 1 1 calc R . . O2SS O 0.2449(10) 0.2864(15) 0.6786(10) 0.55(2) Uani 1 1 d . . . C2SS C 0.2259(11) 0.2580(12) 0.7297(8) 0.70(6) Uani 1 1 d . . . H2S1 H 0.2479 0.2800 0.7513 0.080 Uiso 1 1 calc R . . H2S2 H 0.2404 0.2124 0.7378 0.080 Uiso 1 1 calc R . . H2S3 H 0.1734 0.2577 0.7431 0.080 Uiso 1 1 calc R . . O3SS O 1.0908(6) 0.0348(13) 0.5446(6) 0.449(18) Uani 1 1 d . . . C3SS C 1.1238(12) 0.0355(8) 0.5207(7) 0.37(2) Uani 1 1 d . . . H3S5 H 1.1441 0.0812 0.5003 0.080 Uiso 1 1 calc R . . H3S6 H 1.1117 0.0178 0.4917 0.080 Uiso 1 1 calc R . . H3S7 H 1.1592 0.0084 0.5386 0.080 Uiso 1 1 calc R . . O99 O 0.2306(13) 0.3493(8) 0.5374(7) 0.387(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.076(3) 0.045(2) 0.040(2) -0.0155(18) -0.024(2) 0.008(2) C2A 0.085(3) 0.043(2) 0.049(2) -0.0158(19) -0.030(2) 0.017(2) C3A 0.064(3) 0.042(2) 0.049(2) -0.0175(18) -0.0242(19) 0.024(2) C4A 0.062(3) 0.043(2) 0.057(2) -0.0213(19) -0.022(2) 0.020(2) C5A 0.065(3) 0.051(3) 0.050(2) -0.024(2) -0.028(2) 0.022(2) C6A 0.056(2) 0.056(3) 0.040(2) -0.0182(18) -0.0185(17) 0.017(2) C7A 0.052(2) 0.056(3) 0.049(2) -0.0261(19) -0.0201(18) 0.022(2) C8A 0.053(2) 0.060(3) 0.050(2) -0.024(2) -0.0168(18) 0.008(2) C9A 0.059(2) 0.054(3) 0.045(2) -0.0231(19) -0.0194(18) 0.002(2) C10A 0.069(3) 0.052(3) 0.044(2) -0.0194(19) -0.0167(19) -0.009(2) C11A 0.078(3) 0.040(2) 0.040(2) -0.0103(17) -0.024(2) -0.013(2) C12A 0.071(3) 0.040(2) 0.049(2) -0.0105(18) -0.028(2) -0.002(2) C13A 0.074(3) 0.036(2) 0.048(2) -0.0180(18) -0.024(2) 0.008(2) C14A 0.088(3) 0.045(2) 0.048(2) -0.0201(19) -0.030(2) 0.025(2) C15A 0.071(3) 0.039(2) 0.046(2) -0.0236(18) -0.0239(19) 0.021(2) C16A 0.075(3) 0.053(3) 0.048(2) -0.028(2) -0.026(2) 0.026(2) C17A 0.076(3) 0.074(3) 0.056(3) -0.041(2) -0.028(2) 0.024(3) C18A 0.075(3) 0.061(3) 0.054(3) -0.035(2) -0.017(2) 0.007(2) C19A 0.072(3) 0.048(2) 0.048(2) -0.029(2) -0.015(2) 0.018(2) C20A 0.084(3) 0.060(3) 0.047(2) -0.030(2) -0.018(2) 0.013(2) C21A 0.083(3) 0.048(3) 0.035(2) -0.0230(18) -0.0122(19) 0.003(2) C22A 0.073(3) 0.062(3) 0.041(2) -0.021(2) -0.017(2) 0.003(2) C23A 0.095(4) 0.053(3) 0.050(2) -0.025(2) -0.026(2) 0.000(3) C24A 0.084(3) 0.048(3) 0.044(2) -0.0207(19) -0.025(2) 0.012(2) C25A 0.079(3) 0.050(3) 0.0320(19) -0.0167(18) -0.0177(19) 0.001(2) C26A 0.060(3) 0.056(3) 0.045(2) -0.0263(19) -0.0249(19) 0.028(2) C27A 0.068(3) 0.049(2) 0.041(2) -0.0207(18) -0.0223(19) 0.007(2) C28A 0.068(3) 0.047(2) 0.047(2) -0.0292(19) -0.0226(19) 0.020(2) O1A 0.0666(19) 0.0603(19) 0.0514(16) -0.0241(14) -0.0276(14) 0.0176(15) O2A 0.081(2) 0.0613(19) 0.0406(15) -0.0235(14) -0.0278(14) 0.0253(17) O3A 0.079(2) 0.0458(16) 0.0472(15) -0.0246(13) -0.0306(14) 0.0221(14) O4A 0.079(2) 0.0469(18) 0.0505(17) -0.0248(13) -0.0145(14) 0.0040(16) C30A 0.071(3) 0.063(3) 0.053(2) -0.026(2) -0.031(2) 0.018(2) C31A 0.110(5) 0.086(4) 0.085(4) -0.024(3) -0.054(4) -0.010(4) C32A 0.099(4) 0.084(4) 0.084(4) -0.022(3) -0.059(3) 0.012(3) C33A 0.094(4) 0.139(6) 0.099(4) -0.086(4) -0.045(3) 0.033(4) C40A 0.073(3) 0.056(3) 0.036(2) -0.0086(19) -0.0156(19) -0.015(2) C41A 0.067(5) 0.065(6) 0.034(4) -0.020(4) -0.016(3) 0.014(4) C42A 0.086(8) 0.051(5) 0.040(4) -0.001(3) -0.016(4) -0.009(4) C43A 0.061(6) 0.065(6) 0.031(4) -0.019(4) -0.017(4) -0.007(5) C44A 0.098(11) 0.070(8) 0.055(7) -0.008(6) -0.041(7) 0.010(7) C45A 0.051(7) 0.135(17) 0.054(7) -0.005(8) -0.008(5) -0.017(9) C46A 0.086(12) 0.111(13) 0.044(7) -0.051(7) -0.023(7) 0.020(9) C50A 0.089(4) 0.118(5) 0.088(4) -0.074(4) -0.046(3) 0.028(3) C51A 0.179(8) 0.205(9) 0.073(4) -0.026(5) -0.066(5) -0.069(7) C52A 0.186(9) 0.167(8) 0.103(6) -0.058(5) -0.054(6) -0.058(7) C53A 0.095(6) 0.389(19) 0.174(9) -0.179(11) -0.072(6) 0.050(8) C60A 0.083(4) 0.082(4) 0.101(4) -0.052(4) -0.028(3) -0.004(3) C61A 0.186(10) 0.214(11) 0.194(10) -0.158(9) 0.058(8) -0.116(9) C62A 0.304(17) 0.187(11) 0.117(7) -0.025(7) -0.015(9) -0.174(12) C63A 0.124(7) 0.181(10) 0.257(13) -0.156(10) -0.007(8) -0.026(7) C70A 0.070(3) 0.088(4) 0.060(3) -0.036(3) -0.034(2) 0.027(3) P1A 0.1083(12) 0.1151(15) 0.0640(9) -0.0460(9) -0.0442(9) 0.0386(11) O11A 0.102(3) 0.188(5) 0.070(2) -0.060(3) -0.031(2) 0.062(3) O12A 0.084(3) 0.180(5) 0.058(2) -0.024(3) -0.034(2) 0.028(3) O13A 0.416(18) 0.123(6) 0.125(6) -0.057(4) -0.139(9) 0.052(8) C80A 0.100(4) 0.046(2) 0.044(2) -0.0275(19) -0.031(2) 0.023(2) P2A 0.1455(15) 0.0639(9) 0.0760(9) -0.0307(7) -0.0705(10) 0.0142(10) O21A 0.174(5) 0.145(5) 0.137(4) -0.004(4) -0.071(4) -0.087(4) O22A 0.304(7) 0.088(3) 0.111(3) -0.072(3) -0.151(4) 0.088(4) O23A 0.133(3) 0.082(3) 0.059(2) -0.0320(18) -0.047(2) 0.048(2) C71A 0.19(2) 0.62(7) 0.20(3) -0.31(4) 0.092(19) -0.28(4) C72A 0.17(2) 0.162(19) 0.21(2) -0.031(18) -0.006(17) 0.009(16) C73A 0.138(17) 0.19(2) 0.153(18) -0.138(19) -0.042(13) 0.042(15) C74A 0.20(3) 0.24(3) 0.27(3) -0.19(3) -0.16(2) 0.05(2) C75A 0.145(8) 0.269(16) 0.129(8) 0.111(10) 0.043(7) 0.098(10) C76A 0.65(4) 0.172(12) 0.242(16) -0.168(13) 0.25(2) -0.207(19) C81A 0.124(5) 0.105(5) 0.090(4) -0.055(4) -0.060(4) 0.042(4) C82A 0.157(7) 0.112(5) 0.065(4) -0.022(3) -0.031(4) 0.065(5) C83A 0.56(3) 0.142(8) 0.198(10) -0.132(8) -0.301(15) 0.178(12) C84A 0.202(8) 0.095(5) 0.090(4) -0.061(4) -0.096(5) 0.049(5) C1B 0.037(2) 0.065(3) 0.044(2) -0.029(2) -0.0126(16) 0.0109(18) C2B 0.039(2) 0.072(3) 0.050(2) -0.017(2) -0.0140(17) 0.012(2) C3B 0.039(2) 0.052(2) 0.043(2) -0.0127(18) -0.0142(16) 0.0095(17) C4B 0.039(2) 0.054(3) 0.050(2) -0.0131(19) -0.0162(17) -0.0024(18) C5B 0.036(2) 0.060(3) 0.051(2) -0.0206(19) -0.0181(17) 0.0062(18) C6B 0.039(2) 0.053(2) 0.045(2) -0.0171(18) -0.0116(16) 0.0119(17) C7B 0.0327(18) 0.045(2) 0.054(2) -0.0155(18) -0.0159(16) 0.0081(16) C8B 0.0308(19) 0.059(3) 0.059(2) -0.024(2) -0.0132(16) 0.0081(17) C9B 0.0273(18) 0.052(2) 0.068(3) -0.024(2) -0.0117(17) 0.0011(16) C10B 0.031(2) 0.073(3) 0.070(3) -0.034(2) -0.0142(18) 0.0090(19) C11B 0.031(2) 0.090(4) 0.068(3) -0.032(3) -0.0111(19) 0.006(2) C12B 0.033(2) 0.080(3) 0.060(3) -0.017(2) -0.0129(18) 0.002(2) C13B 0.033(2) 0.064(3) 0.063(3) -0.016(2) -0.0096(18) -0.0010(19) C14B 0.041(2) 0.068(3) 0.072(3) -0.012(2) -0.011(2) 0.002(2) C15B 0.043(2) 0.053(3) 0.060(3) -0.015(2) -0.0171(19) 0.0102(19) C16B 0.052(2) 0.067(3) 0.056(2) -0.026(2) -0.0186(19) 0.019(2) C17B 0.044(2) 0.070(3) 0.067(3) -0.035(2) -0.024(2) 0.019(2) C18B 0.038(2) 0.064(3) 0.072(3) -0.033(2) -0.0180(19) 0.0143(19) C19B 0.047(2) 0.043(2) 0.059(2) -0.0183(19) -0.0186(18) 0.0150(18) C20B 0.048(2) 0.050(3) 0.066(3) -0.030(2) -0.0163(19) 0.0156(19) C21B 0.040(2) 0.051(2) 0.060(2) -0.036(2) -0.0136(17) 0.0135(18) C22B 0.039(2) 0.059(3) 0.066(3) -0.037(2) -0.0211(18) 0.0163(19) C23B 0.038(2) 0.051(3) 0.067(3) -0.037(2) -0.0150(18) 0.0088(18) C24B 0.0347(19) 0.054(2) 0.061(2) -0.032(2) -0.0114(17) 0.0087(17) C25B 0.0360(19) 0.054(2) 0.050(2) -0.032(2) -0.0128(16) 0.0074(17) C26B 0.037(2) 0.046(2) 0.053(2) -0.0192(18) -0.0198(16) 0.0144(17) C27B 0.0314(19) 0.054(3) 0.061(2) -0.022(2) -0.0077(17) 0.0050(17) C28B 0.046(2) 0.043(2) 0.055(2) -0.0141(19) -0.0179(18) 0.0063(18) O1B 0.0414(15) 0.0565(18) 0.0681(18) -0.0329(15) -0.0205(13) 0.0123(13) O2B 0.0461(15) 0.0531(18) 0.0599(17) -0.0192(14) -0.0121(13) 0.0134(14) O3B 0.0538(17) 0.0437(17) 0.0727(19) -0.0219(14) -0.0262(14) 0.0090(13) O4B 0.0370(14) 0.0625(19) 0.0564(16) -0.0260(15) -0.0133(12) -0.0006(13) C30B 0.044(2) 0.096(4) 0.068(3) -0.047(3) -0.018(2) 0.007(2) C31B 0.057(3) 0.171(7) 0.123(5) -0.099(5) -0.026(3) -0.002(4) C32B 0.186(9) 0.211(10) 0.352(16) -0.243(12) -0.191(11) 0.129(8) C33B 0.106(5) 0.218(9) 0.077(4) -0.061(5) -0.025(4) -0.042(6) C40B 0.049(3) 0.118(5) 0.074(3) -0.055(3) -0.021(2) 0.024(3) C41B 0.083(4) 0.213(9) 0.069(4) -0.069(5) -0.021(3) 0.054(5) C42B 0.041(2) 0.128(5) 0.082(3) -0.055(3) -0.010(2) 0.023(3) C43B 0.060(3) 0.161(7) 0.122(5) -0.098(5) -0.025(3) 0.020(4) C50B 0.048(3) 0.103(4) 0.081(3) -0.057(3) -0.024(2) 0.019(3) C51B 0.087(4) 0.101(5) 0.111(5) -0.055(4) -0.054(4) 0.011(4) C52B 0.083(4) 0.105(5) 0.077(3) -0.044(3) -0.038(3) 0.019(3) C53B 0.077(4) 0.158(7) 0.127(5) -0.104(5) -0.032(4) 0.033(4) C60B 0.045(2) 0.058(3) 0.089(3) -0.045(2) -0.029(2) 0.013(2) C61B 0.042(2) 0.063(3) 0.081(3) -0.037(2) -0.018(2) 0.005(2) C62B 0.054(3) 0.060(3) 0.146(5) -0.044(3) -0.031(3) -0.001(2) C63B 0.056(3) 0.135(5) 0.101(4) -0.086(4) -0.019(3) -0.006(3) C70B 0.068(3) 0.081(4) 0.069(3) -0.037(3) -0.029(2) 0.021(3) P1B 0.159(2) 0.1341(18) 0.0935(13) -0.0674(13) -0.0457(14) -0.0090(16) O11B 0.341(10) 0.161(5) 0.146(5) -0.064(4) -0.187(6) 0.033(6) O12B 0.096(3) 0.114(4) 0.123(4) -0.053(3) -0.045(3) -0.001(3) O13B 0.159(5) 0.162(5) 0.140(5) -0.072(4) -0.035(4) -0.016(4) C80B 0.070(3) 0.046(3) 0.109(4) -0.024(3) -0.031(3) 0.011(2) P2B 0.0667(9) 0.0704(10) 0.1271(14) -0.0513(9) -0.0152(9) -0.0047(7) O21B 0.071(3) 0.098(3) 0.126(4) -0.043(3) 0.000(2) -0.006(2) O22B 0.111(4) 0.091(3) 0.232(6) -0.100(4) -0.066(4) 0.022(3) O23B 0.074(3) 0.139(4) 0.125(4) -0.082(3) -0.020(3) 0.009(3) C71B 0.173(10) 0.085(6) 0.237(12) -0.058(7) -0.102(9) 0.016(6) C72B 0.098(6) 0.182(10) 0.153(8) -0.045(7) 0.013(5) -0.011(6) C81B 0.208(13) 0.101(7) 0.242(14) -0.066(8) -0.073(11) 0.015(7) C82B 0.325(18) 0.152(10) 0.161(9) -0.098(8) -0.110(11) 0.098(11) C83B 0.089(5) 0.138(7) 0.123(6) -0.059(5) -0.023(4) 0.012(5) C84B 0.128(7) 0.233(12) 0.132(7) -0.100(8) -0.023(6) 0.037(7) C1C 0.0368(19) 0.050(2) 0.050(2) -0.0255(18) -0.0154(16) 0.0090(17) C2C 0.0342(19) 0.056(3) 0.054(2) -0.0243(19) -0.0138(16) 0.0095(17) C3C 0.0338(18) 0.042(2) 0.0376(18) -0.0130(16) -0.0120(14) 0.0111(15) C4C 0.0313(18) 0.050(2) 0.0359(18) -0.0138(16) -0.0091(14) 0.0140(16) C5C 0.0358(19) 0.057(2) 0.0389(19) -0.0142(17) -0.0139(15) 0.0154(17) C6C 0.050(2) 0.053(2) 0.042(2) -0.0230(18) -0.0190(17) 0.0207(19) C7C 0.045(2) 0.053(2) 0.0361(19) -0.0136(17) -0.0083(16) 0.0187(19) C8C 0.065(3) 0.065(3) 0.035(2) -0.0110(19) -0.0027(18) 0.028(2) C9C 0.065(3) 0.056(3) 0.0325(19) -0.0081(18) -0.0017(18) 0.026(2) C10C 0.095(3) 0.049(3) 0.032(2) -0.0142(18) -0.016(2) 0.025(2) C11C 0.086(3) 0.065(3) 0.036(2) -0.015(2) -0.015(2) 0.022(3) C12C 0.071(3) 0.065(3) 0.039(2) -0.015(2) -0.013(2) 0.028(2) C13C 0.070(3) 0.051(3) 0.039(2) -0.0064(19) -0.0059(19) 0.022(2) C14C 0.079(3) 0.049(3) 0.046(2) -0.008(2) -0.012(2) 0.020(2) C15C 0.069(3) 0.038(2) 0.051(2) -0.0098(19) -0.016(2) 0.020(2) C16C 0.093(4) 0.038(2) 0.047(2) -0.0160(19) -0.023(2) 0.019(2) C17C 0.082(3) 0.030(2) 0.045(2) -0.0145(17) -0.011(2) 0.011(2) C18C 0.084(3) 0.038(2) 0.047(2) -0.0183(19) -0.016(2) 0.024(2) C19C 0.075(3) 0.044(2) 0.058(3) -0.022(2) -0.023(2) 0.025(2) C20C 0.080(3) 0.061(3) 0.072(3) -0.033(2) -0.027(3) 0.025(3) C21C 0.061(3) 0.057(3) 0.060(3) -0.033(2) -0.023(2) 0.018(2) C22C 0.047(2) 0.072(3) 0.058(3) -0.041(2) -0.0189(19) 0.019(2) C23C 0.043(2) 0.065(3) 0.048(2) -0.034(2) -0.0135(17) 0.0026(19) C24C 0.039(2) 0.056(2) 0.045(2) -0.0237(18) -0.0162(16) 0.0006(17) C25C 0.046(2) 0.056(3) 0.051(2) -0.024(2) -0.0105(18) 0.0047(19) C26C 0.039(2) 0.039(2) 0.048(2) -0.0092(17) -0.0089(16) 0.0128(17) C27C 0.068(3) 0.054(3) 0.034(2) -0.0107(18) -0.0032(18) 0.015(2) C28C 0.069(3) 0.046(3) 0.058(3) -0.017(2) -0.019(2) 0.023(2) O1C 0.0432(15) 0.0410(16) 0.0632(17) -0.0054(13) -0.0034(13) 0.0055(12) O2C 0.0649(19) 0.0496(18) 0.0568(17) -0.0162(15) -0.0115(15) 0.0153(15) O3C 0.062(2) 0.060(2) 0.084(2) -0.0206(17) -0.0181(17) 0.0165(16) O4C 0.0604(18) 0.0461(17) 0.0493(16) -0.0121(13) -0.0047(13) 0.0102(14) C30C 0.035(2) 0.067(3) 0.058(2) -0.022(2) -0.0188(17) 0.0053(19) C31C 0.056(3) 0.103(4) 0.103(4) -0.041(3) -0.046(3) 0.013(3) C32C 0.054(3) 0.057(3) 0.084(3) -0.023(2) -0.016(2) 0.001(2) C33C 0.054(3) 0.106(4) 0.077(3) -0.045(3) 0.012(2) -0.025(3) C40C 0.119(5) 0.072(3) 0.058(3) -0.027(3) -0.038(3) 0.032(3) C41C 0.47(2) 0.144(8) 0.313(16) -0.135(10) -0.346(18) 0.129(12) C42C 0.170(8) 0.114(6) 0.110(5) -0.079(5) -0.041(5) 0.021(5) C43C 0.135(7) 0.268(12) 0.103(6) -0.103(7) 0.004(5) -0.079(8) C50C 0.103(4) 0.046(3) 0.052(3) -0.022(2) -0.004(2) -0.008(3) C51C 0.130(7) 0.172(8) 0.191(9) -0.133(8) 0.055(6) -0.072(6) C52C 0.173(8) 0.165(8) 0.098(5) -0.057(5) 0.019(5) -0.110(7) C53C 0.237(12) 0.069(5) 0.203(11) 0.042(6) -0.042(9) -0.038(6) C60C 0.046(2) 0.086(4) 0.053(2) -0.038(2) -0.0035(18) -0.001(2) C61C 0.062(3) 0.117(5) 0.066(3) -0.061(3) -0.011(2) 0.010(3) C62C 0.063(3) 0.101(4) 0.060(3) -0.022(3) -0.003(2) -0.014(3) C63C 0.046(3) 0.157(6) 0.067(3) -0.059(4) 0.000(2) -0.016(3) C70C 0.039(2) 0.053(3) 0.073(3) -0.005(2) -0.001(2) 0.0044(19) P1C 0.0528(9) 0.0689(12) 0.214(3) 0.0226(15) -0.0157(12) -0.0076(8) O11C 0.139(5) 0.124(5) 0.309(11) -0.033(6) -0.100(6) -0.035(4) O12C 0.043(2) 0.093(3) 0.170(5) 0.028(3) -0.003(2) -0.0105(19) O13C 0.098(3) 0.101(4) 0.170(6) 0.070(4) 0.005(3) 0.002(3) C80C 0.102(5) 0.059(3) 0.104(4) -0.023(3) -0.001(4) 0.009(3) P2C 0.133(2) 0.120(2) 0.255(4) -0.099(2) 0.078(3) -0.0444(18) O21C 0.155(8) 0.092(5) 0.167(8) -0.015(5) 0.105(7) -0.004(5) O22C 0.087(6) 0.190(12) 0.301(17) -0.166(12) -0.042(8) 0.006(6) O23C 0.143(8) 0.063(5) 0.40(2) -0.094(8) 0.135(11) -0.058(5) C71C 0.065(5) 0.167(9) 0.300(16) 0.085(10) 0.009(7) 0.004(5) C72C 0.058(4) 0.179(10) 0.248(13) 0.059(9) 0.037(6) 0.023(5) C73C 0.276(19) 0.28(2) 0.195(15) 0.101(15) -0.046(13) -0.144(18) C82C 0.47(4) 1.02(9) 0.194(18) -0.18(3) -0.11(2) 0.52(5) C83C 2.0(2) 1.37(17) 0.40(5) 0.03(8) 0.18(9) 1.5(2) C84C 0.193(14) 0.49(3) 0.257(19) 0.03(2) -0.052(13) -0.21(2) O1SS 0.224(8) 0.171(7) 0.127(5) -0.057(5) 0.017(5) 0.019(6) C1SS 0.117(6) 0.108(6) 0.146(7) -0.032(6) -0.019(5) -0.014(5) O2SS 0.276(17) 0.74(4) 0.34(2) 0.27(3) -0.113(16) -0.18(2) C2SS 0.28(3) 1.11(11) 0.29(3) 0.39(5) -0.12(2) -0.14(4) O3SS 0.162(8) 0.72(4) 0.184(10) 0.155(16) 0.029(8) 0.104(14) C3SS 0.86(6) 0.225(17) 0.209(17) -0.150(15) -0.35(3) 0.27(3) O99 0.61(3) 0.276(14) 0.234(13) -0.051(11) -0.082(16) 0.066(18) _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 C1A C25A 1.389(6) . ? C1A C24A 1.393(6) . ? C1A C2A 1.523(7) . ? C2A C3A 1.530(6) . ? C3A C4A 1.381(6) . ? C3A C26A 1.381(6) . ? C4A C5A 1.390(6) . ? C5A C6A 1.387(6) . ? C5A C30A 1.545(6) . ? C6A C7A 1.386(6) . ? C7A C26A 1.382(6) . ? C7A C8A 1.526(6) . ? C8A C9A 1.507(6) . ? C9A C27A 1.390(6) . ? C9A C10A 1.396(6) . ? C10A C11A 1.370(6) . ? C11A C12A 1.390(6) . ? C11A C40A 1.538(5) . ? C12A C13A 1.377(6) . ? C13A C27A 1.403(6) . ? C13A C14A 1.519(6) . ? C14A C15A 1.505(7) . ? C15A C16A 1.381(6) . ? C15A C28A 1.395(6) . ? C16A C17A 1.386(7) . ? C17A C18A 1.411(7) . ? C17A C50A 1.527(7) . ? C18A C19A 1.398(6) . ? C19A C28A 1.382(6) . ? C19A C20A 1.506(6) . ? C20A C21A 1.511(6) . ? C21A C22A 1.399(7) . ? C21A C25A 1.401(6) . ? C22A C23A 1.408(7) . ? C23A C24A 1.398(7) . ? C23A C60A 1.521(8) . ? C25A O4A 1.352(5) . ? C26A O1A 1.401(5) . ? C27A O2A 1.369(5) . ? C28A O3A 1.403(5) . ? O1A C70A 1.437(5) . ? O3A C80A 1.436(5) . ? C30A C31A 1.502(8) . ? C30A C32A 1.515(7) . ? C30A C33A 1.552(7) . ? C40A C45A 1.372(12) . ? C40A C43A 1.452(11) . ? C40A C42A 1.469(9) . ? C40A C46A 1.500(17) . ? C40A C41A 1.639(9) . ? C40A C44A 1.766(13) . ? C50A C51A 1.454(9) . ? C50A C53A 1.518(10) . ? C50A C52A 1.560(11) . ? C60A C61A 1.411(9) . ? C60A C63A 1.508(11) . ? C60A C62A 1.531(12) . ? C70A P1A 1.772(5) . ? P1A O13A 1.411(9) . ? P1A O11A 1.447(5) . ? P1A O12A 1.533(4) . ? P1A C71A 2.23(3) . ? O12A C75A 1.522(14) . ? O13A C71A 0.89(3) . ? O13A C73A 1.62(2) . ? C80A P2A 1.783(5) . ? P2A O21A 1.467(6) . ? P2A O23A 1.550(4) . ? P2A O22A 1.564(5) . ? O22A C83A 1.446(7) . ? O23A C81A 1.418(7) . ? C71A C72A 1.56(3) . ? C73A C74A 1.41(3) . ? C75A C76A 1.149(18) . ? C81A C82A 1.473(8) . ? C83A C84A 1.209(9) . ? C1B C25B 1.389(6) . ? C1B C24B 1.388(6) . ? C1B C2B 1.522(5) . ? C2B C3B 1.535(5) . ? C3B C4B 1.372(6) . ? C3B C26B 1.394(5) . ? C4B C5B 1.384(6) . ? C5B C6B 1.388(6) . ? C5B C30B 1.545(6) . ? C6B C7B 1.392(6) . ? C7B C26B 1.380(5) . ? C7B C8B 1.516(5) . ? C8B C9B 1.516(6) . ? C9B C10B 1.374(6) . ? C9B C27B 1.397(6) . ? C10B C11B 1.407(7) . ? C11B C12B 1.402(7) . ? C11B C40B 1.514(7) . ? C12B C13B 1.398(6) . ? C13B C27B 1.370(6) . ? C13B C14B 1.524(6) . ? C14B C15B 1.520(6) . ? C15B C28B 1.377(6) . ? C15B C16B 1.404(6) . ? C16B C17B 1.399(6) . ? C17B C18B 1.398(6) . ? C17B C50B 1.522(6) . ? C18B C19B 1.368(6) . ? C19B C28B 1.396(6) . ? C19B C20B 1.529(6) . ? C20B C21B 1.501(6) . ? C21B C25B 1.396(5) . ? C21B C22B 1.408(6) . ? C22B C23B 1.396(6) . ? C23B C24B 1.389(6) . ? C23B C60B 1.524(6) . ? C25B O4B 1.384(5) . ? C26B O1B 1.385(5) . ? C27B O2B 1.381(5) . ? C28B O3B 1.401(5) . ? O1B C70B 1.453(5) . ? O3B C80B 1.429(5) . ? C30B C32B 1.504(9) . ? C30B C31B 1.519(7) . ? C30B C33B 1.553(9) . ? C40B C41B 1.508(8) . ? C40B C42B 1.535(7) . ? C40B C43B 1.564(9) . ? C50B C51B 1.532(9) . ? C50B C52B 1.527(7) . ? C50B C53B 1.527(7) . ? C60B C63B 1.524(7) . ? C60B C61B 1.523(6) . ? C60B C62B 1.546(8) . ? C70B P1B 1.765(5) . ? P1B O13B 1.446(7) . ? P1B O11B 1.458(6) . ? P1B O12B 1.524(5) . ? O12B C71B 1.473(10) . ? O13B C73B 1.549(6) . ? C80B P2B 1.787(6) . ? P2B O21B 1.452(4) . ? P2B O23B 1.528(5) . ? P2B O22B 1.542(5) . ? O22B C81B 1.437(12) . ? O23B C83B 1.453(9) . ? C71B C72B 1.438(12) . ? C73B C74B 1.228(7) . ? C81B C82B 1.293(13) . ? C83B C84B 1.501(12) . ? C1C C24C 1.389(5) . ? C1C C25C 1.402(6) . ? C1C C2C 1.523(5) . ? C2C C3C 1.513(5) . ? C3C C4C 1.382(5) . ? C3C C26C 1.410(5) . ? C4C C5C 1.401(5) . ? C5C C6C 1.405(5) . ? C5C C30C 1.521(6) . ? C6C C7C 1.378(6) . ? C7C C26C 1.373(6) . ? C7C C8C 1.528(5) . ? C8C C9C 1.504(6) . ? C9C C10C 1.390(7) . ? C9C C27C 1.403(6) . ? C10C C11C 1.389(7) . ? C11C C12C 1.393(7) . ? C11C C40C 1.559(8) . ? C12C C13C 1.390(7) . ? C13C C27C 1.397(6) . ? C13C C14C 1.518(6) . ? C14C C15C 1.513(6) . ? C15C C16C 1.366(7) . ? C15C C28C 1.397(7) . ? C16C C17C 1.408(6) . ? C17C C18C 1.395(6) . ? C17C C50C 1.518(7) . ? C18C C19C 1.373(7) . ? C19C C28C 1.392(6) . ? C19C C20C 1.545(7) . ? C20C C21C 1.505(7) . ? C21C C25C 1.384(6) . ? C21C C22C 1.390(6) . ? C22C C23C 1.398(6) . ? C23C C24C 1.391(5) . ? C23C C60C 1.523(6) . ? C25C O4C 1.372(5) . ? C26C O1C 1.411(5) . ? C27C O2C 1.362(6) . ? C28C O3C 1.400(6) . ? O1C C70C 1.431(5) . ? O3C C80C 1.439(6) . ? C30C C33C 1.512(6) . ? C30C C31C 1.523(6) . ? C30C C32C 1.526(6) . ? C40C C43C 1.459(10) . ? C40C C41C 1.483(9) . ? C40C C42C 1.516(8) . ? C50C C53C 1.458(10) . ? C50C C51C 1.507(10) . ? C50C C52C 1.532(9) . ? C60C C62C 1.512(8) . ? C60C C63C 1.537(7) . ? C60C C61C 1.555(7) . ? C70C P1C 1.789(5) . ? P1C O13C 1.479(7) . ? P1C O11C 1.530(10) . ? P1C O12C 1.568(4) . ? O12C C71C 1.452(9) . ? O13C C73C 1.242(18) . ? C80C P2C 1.767(8) . ? P2C O23C 1.479(10) . ? P2C O21C 1.487(8) . ? P2C O22C 1.597(16) . ? O22C C81C 1.43(2) . ? O23C C83C 1.30(3) . ? C71C C72C 1.479(12) . ? C73C C74C 1.319(16) 2_666 ? C74C C73C 1.319(16) 2_666 ? C81C C82C 1.50(2) . ? C83C C84C 1.61(3) . ? O1SS C1SS 1.350(10) . ? O2SS C2SS 1.136(18) . ? O3SS C3SS 0.73(2) . ? 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 C25A C1A C24A 118.7(4) . . ? C25A C1A C2A 119.7(4) . . ? C24A C1A C2A 121.5(4) . . ? C1A C2A C3A 110.4(3) . . ? C4A C3A C26A 118.7(4) . . ? C4A C3A C2A 119.1(4) . . ? C26A C3A C2A 122.1(4) . . ? C3A C4A C5A 121.7(4) . . ? C4A C5A C6A 117.4(4) . . ? C4A C5A C30A 122.6(4) . . ? C6A C5A C30A 119.9(4) . . ? C7A C6A C5A 122.8(4) . . ? C26A C7A C6A 117.4(4) . . ? C26A C7A C8A 122.3(4) . . ? C6A C7A C8A 120.1(4) . . ? C9A C8A C7A 108.4(3) . . ? C27A C9A C10A 118.5(4) . . ? C27A C9A C8A 119.2(4) . . ? C10A C9A C8A 121.9(4) . . ? C11A C10A C9A 123.5(4) . . ? C10A C11A C12A 115.9(4) . . ? C10A C11A C40A 122.2(4) . . ? C12A C11A C40A 121.8(4) . . ? C13A C12A C11A 124.0(4) . . ? C12A C13A C27A 118.1(4) . . ? C12A C13A C14A 120.8(4) . . ? C27A C13A C14A 120.9(4) . . ? C15A C14A C13A 111.5(3) . . ? C16A C15A C28A 117.9(4) . . ? C16A C15A C14A 120.1(4) . . ? C28A C15A C14A 122.0(4) . . ? C17A C16A C15A 122.8(4) . . ? C16A C17A C18A 116.8(4) . . ? C16A C17A C50A 123.3(5) . . ? C18A C17A C50A 119.9(5) . . ? C19A C18A C17A 122.8(5) . . ? C28A C19A C18A 116.7(4) . . ? C28A C19A C20A 123.3(4) . . ? C18A C19A C20A 119.9(4) . . ? C19A C20A C21A 110.3(3) . . ? C22A C21A C25A 120.6(4) . . ? C22A C21A C20A 120.2(4) . . ? C25A C21A C20A 119.1(4) . . ? C21A C22A C23A 120.5(5) . . ? C24A C23A C22A 117.2(4) . . ? C24A C23A C60A 121.1(4) . . ? C22A C23A C60A 121.7(5) . . ? C1A C24A C23A 123.1(4) . . ? O4A C25A C1A 123.1(4) . . ? O4A C25A C21A 117.0(4) . . ? C1A C25A C21A 119.9(4) . . ? C3A C26A C7A 122.0(4) . . ? C3A C26A O1A 118.3(4) . . ? C7A C26A O1A 119.5(4) . . ? O2A C27A C9A 117.9(4) . . ? O2A C27A C13A 122.0(4) . . ? C9A C27A C13A 120.0(4) . . ? C19A C28A C15A 122.9(4) . . ? C19A C28A O3A 118.9(4) . . ? C15A C28A O3A 118.1(4) . . ? C26A O1A C70A 114.3(3) . . ? C28A O3A C80A 113.5(3) . . ? C31A C30A C32A 110.4(4) . . ? C31A C30A C5A 112.4(4) . . ? C32A C30A C5A 110.4(4) . . ? C31A C30A C33A 107.5(5) . . ? C32A C30A C33A 108.3(5) . . ? C5A C30A C33A 107.6(4) . . ? C45A C40A C43A 135.2(8) . . ? C45A C40A C42A 63.4(10) . . ? C43A C40A C42A 118.8(6) . . ? C45A C40A C46A 114.2(11) . . ? C43A C40A C46A 28.9(6) . . ? C42A C40A C46A 134.7(8) . . ? C45A C40A C11A 112.4(6) . . ? C43A C40A C11A 107.6(5) . . ? C42A C40A C11A 111.3(4) . . ? C46A C40A C11A 110.6(7) . . ? C45A C40A C41A 44.2(9) . . ? C43A C40A C41A 103.7(6) . . ? C42A C40A C41A 105.7(6) . . ? C46A C40A C41A 75.8(7) . . ? C11A C40A C41A 109.3(4) . . ? C45A C40A C44A 107.4(10) . . ? C43A C40A C44A 76.2(7) . . ? C42A C40A C44A 47.1(6) . . ? C46A C40A C44A 102.1(9) . . ? C11A C40A C44A 109.5(5) . . ? C41A C40A C44A 139.1(6) . . ? C51A C50A C53A 117.7(7) . . ? C51A C50A C17A 112.4(6) . . ? C53A C50A C17A 107.6(5) . . ? C51A C50A C52A 106.1(6) . . ? C53A C50A C52A 103.7(8) . . ? C17A C50A C52A 108.7(5) . . ? C61A C60A C63A 118.5(7) . . ? C61A C60A C23A 114.8(6) . . ? C63A C60A C23A 114.8(6) . . ? C61A C60A C62A 105.7(8) . . ? C63A C60A C62A 91.8(8) . . ? C23A C60A C62A 107.4(5) . . ? O1A C70A P1A 108.4(3) . . ? O13A P1A O11A 112.2(6) . . ? O13A P1A O12A 105.1(6) . . ? O11A P1A O12A 115.8(3) . . ? O13A P1A C70A 103.9(4) . . ? O11A P1A C70A 114.6(3) . . ? O12A P1A C70A 104.2(2) . . ? O13A P1A C71A 11.3(7) . . ? O11A P1A C71A 118.5(7) . . ? O12A P1A C71A 108.2(9) . . ? C70A P1A C71A 92.6(6) . . ? C75A O12A P1A 118.8(5) . . ? C71A O13A P1A 150.8(16) . . ? C71A O13A C73A 74.8(18) . . ? P1A O13A C73A 133.4(11) . . ? O3A C80A P2A 107.0(3) . . ? O21A P2A O23A 115.9(3) . . ? O21A P2A O22A 116.3(4) . . ? O23A P2A O22A 102.8(2) . . ? O21A P2A C80A 113.3(3) . . ? O23A P2A C80A 107.8(2) . . ? O22A P2A C80A 98.9(3) . . ? C83A O22A P2A 123.5(6) . . ? C81A O23A P2A 121.7(4) . . ? O13A C71A C72A 137(2) . . ? O13A C71A P1A 18.0(10) . . ? C72A C71A P1A 154.0(16) . . ? C74A C73A O13A 126.1(15) . . ? C76A C75A O12A 137.6(13) . . ? O23A C81A C82A 111.2(5) . . ? C84A C83A O22A 119.6(7) . . ? C25B C1B C24B 119.7(4) . . ? C25B C1B C2B 120.9(4) . . ? C24B C1B C2B 119.0(4) . . ? C1B C2B C3B 107.5(3) . . ? C4B C3B C26B 118.6(4) . . ? C4B C3B C2B 119.6(4) . . ? C26B C3B C2B 121.4(4) . . ? C3B C4B C5B 122.7(4) . . ? C4B C5B C6B 116.7(4) . . ? C4B C5B C30B 122.4(4) . . ? C6B C5B C30B 120.9(4) . . ? C5B C6B C7B 123.0(4) . . ? C26B C7B C6B 117.5(3) . . ? C26B C7B C8B 122.1(4) . . ? C6B C7B C8B 120.2(3) . . ? C7B C8B C9B 109.2(3) . . ? C10B C9B C27B 119.7(4) . . ? C10B C9B C8B 120.5(4) . . ? C27B C9B C8B 119.5(4) . . ? C9B C10B C11B 121.8(4) . . ? C12B C11B C10B 116.7(4) . . ? C12B C11B C40B 123.2(4) . . ? C10B C11B C40B 120.2(4) . . ? C13B C12B C11B 122.1(4) . . ? C27B C13B C12B 119.0(4) . . ? C27B C13B C14B 121.7(4) . . ? C12B C13B C14B 119.3(4) . . ? C15B C14B C13B 110.6(4) . . ? C28B C15B C16B 117.4(4) . . ? C28B C15B C14B 123.0(4) . . ? C16B C15B C14B 119.5(4) . . ? C17B C16B C15B 122.2(4) . . ? C16B C17B C18B 116.4(4) . . ? C16B C17B C50B 122.9(4) . . ? C18B C17B C50B 120.7(4) . . ? C19B C18B C17B 123.9(4) . . ? C18B C19B C28B 117.1(4) . . ? C18B C19B C20B 121.6(4) . . ? C28B C19B C20B 121.3(4) . . ? C21B C20B C19B 111.1(3) . . ? C25B C21B C22B 116.7(4) . . ? C25B C21B C20B 121.0(4) . . ? C22B C21B C20B 122.2(4) . . ? C23B C22B C21B 123.6(4) . . ? C24B C23B C22B 116.8(4) . . ? C24B C23B C60B 122.0(4) . . ? C22B C23B C60B 121.2(4) . . ? C1B C24B C23B 121.8(4) . . ? O4B C25B C1B 121.7(3) . . ? O4B C25B C21B 117.0(4) . . ? C1B C25B C21B 121.3(4) . . ? C7B C26B O1B 119.6(3) . . ? C7B C26B C3B 121.3(4) . . ? O1B C26B C3B 118.9(3) . . ? C13B C27B O2B 123.7(4) . . ? C13B C27B C9B 120.7(4) . . ? O2B C27B C9B 115.6(4) . . ? C15B C28B C19B 122.9(4) . . ? C15B C28B O3B 117.8(4) . . ? C19B C28B O3B 119.2(4) . . ? C26B O1B C70B 111.6(3) . . ? C28B O3B C80B 112.3(3) . . ? C32B C30B C31B 107.1(6) . . ? C32B C30B C5B 108.8(4) . . ? C31B C30B C5B 112.6(4) . . ? C32B C30B C33B 114.6(7) . . ? C31B C30B C33B 106.9(5) . . ? C5B C30B C33B 107.0(5) . . ? C41B C40B C11B 112.9(5) . . ? C41B C40B C42B 108.0(5) . . ? C11B C40B C42B 110.2(4) . . ? C41B C40B C43B 107.3(6) . . ? C11B C40B C43B 108.5(5) . . ? C42B C40B C43B 109.8(5) . . ? C17B C50B C51B 111.0(4) . . ? C17B C50B C52B 109.4(4) . . ? C51B C50B C52B 107.9(4) . . ? C17B C50B C53B 112.6(4) . . ? C51B C50B C53B 108.3(5) . . ? C52B C50B C53B 107.6(5) . . ? C63B C60B C61B 109.8(4) . . ? C63B C60B C23B 108.5(4) . . ? C61B C60B C23B 109.8(3) . . ? C63B C60B C62B 109.6(4) . . ? C61B C60B C62B 107.1(4) . . ? C23B C60B C62B 112.1(4) . . ? O1B C70B P1B 111.6(4) . . ? O13B P1B O11B 115.0(5) . . ? O13B P1B O12B 107.4(4) . . ? O11B P1B O12B 112.3(4) . . ? O13B P1B C70B 104.2(3) . . ? O11B P1B C70B 107.8(3) . . ? O12B P1B C70B 109.8(3) . . ? C71B O12B P1B 123.3(6) . . ? P1B O13B C73B 126.8(5) . . ? O3B C80B P2B 107.0(3) . . ? O21B P2B O23B 113.3(3) . . ? O21B P2B O22B 118.5(3) . . ? O23B P2B O22B 102.2(3) . . ? O21B P2B C80B 113.6(3) . . ? O23B P2B C80B 107.1(3) . . ? O22B P2B C80B 100.5(3) . . ? C81B O22B P2B 121.9(7) . . ? C83B O23B P2B 121.2(4) . . ? C72B C71B O12B 109.0(8) . . ? C74B C73B O13B 154.7(4) . . ? C82B C81B O22B 117.5(11) . . ? O23B C83B C84B 107.1(7) . . ? C24C C1C C25C 118.9(3) . . ? C24C C1C C2C 120.8(4) . . ? C25C C1C C2C 120.2(3) . . ? C3C C2C C1C 111.2(3) . . ? C4C C3C C26C 117.2(3) . . ? C4C C3C C2C 119.8(3) . . ? C26C C3C C2C 122.9(3) . . ? C3C C4C C5C 122.9(3) . . ? C4C C5C C6C 116.3(4) . . ? C4C C5C C30C 123.5(3) . . ? C6C C5C C30C 120.1(4) . . ? C7C C6C C5C 122.9(4) . . ? C26C C7C C6C 118.1(3) . . ? C26C C7C C8C 123.0(4) . . ? C6C C7C C8C 118.7(4) . . ? C9C C8C C7C 109.8(3) . . ? C10C C9C C27C 118.9(4) . . ? C10C C9C C8C 121.0(4) . . ? C27C C9C C8C 120.0(5) . . ? C11C C10C C9C 123.0(4) . . ? C10C C11C C12C 116.4(5) . . ? C10C C11C C40C 121.6(4) . . ? C12C C11C C40C 121.8(4) . . ? C13C C12C C11C 123.0(4) . . ? C12C C13C C27C 118.9(4) . . ? C12C C13C C14C 122.2(4) . . ? C27C C13C C14C 118.8(5) . . ? C15C C14C C13C 109.4(3) . . ? C16C C15C C28C 117.9(4) . . ? C16C C15C C14C 121.2(4) . . ? C28C C15C C14C 120.6(4) . . ? C15C C16C C17C 123.2(4) . . ? C18C C17C C16C 116.1(4) . . ? C18C C17C C50C 121.2(4) . . ? C16C C17C C50C 122.7(4) . . ? C19C C18C C17C 123.2(4) . . ? C18C C19C C28C 118.0(4) . . ? C18C C19C C20C 120.2(4) . . ? C28C C19C C20C 121.4(5) . . ? C21C C20C C19C 107.9(4) . . ? C25C C21C C22C 118.5(4) . . ? C25C C21C C20C 118.8(4) . . ? C22C C21C C20C 122.4(4) . . ? C21C C22C C23C 123.5(4) . . ? C24C C23C C22C 115.8(4) . . ? C24C C23C C60C 123.8(4) . . ? C22C C23C C60C 120.3(4) . . ? C1C C24C C23C 122.9(4) . . ? O4C C25C C21C 119.3(4) . . ? O4C C25C C1C 120.2(3) . . ? C21C C25C C1C 120.4(4) . . ? C7C C26C O1C 119.1(3) . . ? C7C C26C C3C 122.4(4) . . ? O1C C26C C3C 118.5(4) . . ? O2C C27C C13C 120.2(4) . . ? O2C C27C C9C 119.9(4) . . ? C13C C27C C9C 119.8(5) . . ? C19C C28C C15C 121.7(5) . . ? C19C C28C O3C 119.2(4) . . ? C15C C28C O3C 119.0(4) . . ? C26C O1C C70C 113.9(3) . . ? C28C O3C C80C 113.2(4) . . ? C33C C30C C31C 109.0(4) . . ? C33C C30C C5C 112.0(4) . . ? C31C C30C C5C 110.9(4) . . ? C33C C30C C32C 109.4(4) . . ? C31C C30C C32C 106.4(4) . . ? C5C C30C C32C 109.0(3) . . ? C43C C40C C41C 111.1(9) . . ? C43C C40C C42C 111.0(7) . . ? C41C C40C C42C 107.5(7) . . ? C43C C40C C11C 107.6(5) . . ? C41C C40C C11C 110.5(5) . . ? C42C C40C C11C 109.1(5) . . ? C53C C50C C51C 111.3(8) . . ? C53C C50C C17C 109.9(6) . . ? C51C C50C C17C 110.2(4) . . ? C53C C50C C52C 109.0(7) . . ? C51C C50C C52C 104.8(7) . . ? C17C C50C C52C 111.5(4) . . ? C62C C60C C23C 113.6(4) . . ? C62C C60C C63C 108.7(5) . . ? C23C C60C C63C 109.1(4) . . ? C62C C60C C61C 108.2(4) . . ? C23C C60C C61C 109.4(4) . . ? C63C C60C C61C 107.6(4) . . ? O1C C70C P1C 106.9(3) . . ? O13C P1C O11C 112.1(4) . . ? O13C P1C O12C 111.4(4) . . ? O11C P1C O12C 110.8(4) . . ? O13C P1C C70C 110.5(4) . . ? O11C P1C C70C 110.4(4) . . ? O12C P1C C70C 101.2(2) . . ? C71C O12C P1C 122.4(5) . . ? C73C O13C P1C 125.4(11) . . ? O3C C80C P2C 107.0(4) . . ? O23C P2C O21C 119.2(7) . . ? O23C P2C O22C 107.4(9) . . ? O21C P2C O22C 111.5(7) . . ? O23C P2C C80C 101.3(5) . . ? O21C P2C C80C 109.2(6) . . ? O22C P2C C80C 107.2(5) . . ? C81C O22C P2C 141.4(12) . . ? C83C O23C P2C 122.0(15) . . ? O12C C71C C72C 106.6(7) . . ? O13C C73C C74C 108.8(17) . 2_666 ? O22C C81C C82C 126(2) . . ? O23C C83C C84C 96(2) . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 1.002 _refine_diff_density_min -2.467 _refine_diff_density_rms 0.103 data_end3a #in paper label 3a _database_code_CSD 179148 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H86 O10 P2' _chemical_formula_weight 1005.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.994(2) _cell_length_b 12.123(2) _cell_length_c 21.235(5) _cell_angle_alpha 102.455(16) _cell_angle_beta 93.036(18) _cell_angle_gamma 93.847(15) _cell_volume 3001.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 0.98 _cell_measurement_theta_max 22.98 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas --- _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KUMA (Poland)' _diffrn_measurement_method '.omega.-scan (0.5.degree)' _diffrn_detector_area_resol_mean '16.7 pixels/mm' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8325 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 22.98 _reflns_number_total 8323 _reflns_number_gt 5692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA (Poland)' _computing_cell_refinement 'KUMA (Poland)' _computing_data_reduction 'KUMA (Poland)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8323 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1578 _refine_ls_R_factor_gt 0.1241 _refine_ls_wR_factor_ref 0.3884 _refine_ls_wR_factor_gt 0.3681 _refine_ls_goodness_of_fit_ref 1.565 _refine_ls_restrained_S_all 1.565 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.46169(16) 0.19465(17) 0.24771(12) 0.0549(7) Uani 1 1 d . . . P2 P -0.05921(18) -0.02068(17) 0.24347(13) 0.0598(7) Uani 1 1 d . . . O1 O 0.2390(3) 0.4253(3) 0.3282(2) 0.0306(10) Uani 1 1 d . . . O2 O 0.0221(4) 0.3425(4) 0.3193(2) 0.0428(12) Uani 1 1 d . . . H2AO H 0.0819 0.3543 0.3412 0.064 Uiso 1 1 calc R . . O3 O -0.0029(3) 0.2828(3) 0.1726(2) 0.0315(10) Uani 1 1 d . . . O4 O 0.2064(3) 0.3836(3) 0.1842(2) 0.0367(11) Uani 1 1 d . . . H4AO H 0.1565 0.3395 0.1628 0.055 Uiso 1 1 calc R . . O11 O 0.5366(5) 0.2899(6) 0.2736(4) 0.101(3) Uani 1 1 d . . . O12 O 0.4854(5) 0.0790(6) 0.2664(4) 0.083(2) Uani 1 1 d . . . O13 O 0.4586(8) 0.1552(6) 0.1733(4) 0.110(3) Uani 1 1 d . . . O21 O -0.1672(6) -0.0238(6) 0.2124(5) 0.110(3) Uani 1 1 d . . . O22 O -0.0020(5) -0.1293(4) 0.2363(3) 0.080(2) Uani 1 1 d . . . O23 O -0.0631(7) 0.0067(7) 0.3206(4) 0.104(2) Uani 1 1 d . . . C1 C 0.2985(5) 0.5657(5) 0.1925(3) 0.0263(13) Uani 1 1 d . . . C2 C 0.3669(5) 0.5542(5) 0.2526(3) 0.0285(14) Uani 1 1 d . . . H2A H 0.4414 0.5912 0.2535 0.034 Uiso 1 1 calc R . . H2B H 0.3742 0.4747 0.2517 0.034 Uiso 1 1 calc R . . C3 C 0.3101(5) 0.6079(5) 0.3132(3) 0.0275(14) Uani 1 1 d . . . C4 C 0.3179(5) 0.7233(5) 0.3346(3) 0.0367(16) Uani 1 1 d . . . H4A H 0.3634 0.7673 0.3138 0.044 Uiso 1 1 calc R . . C5 C 0.2596(6) 0.7781(6) 0.3867(4) 0.0446(18) Uani 1 1 d . . . C6 C 0.1933(6) 0.7109(5) 0.4163(3) 0.0366(16) Uani 1 1 d . . . H6 H 0.1534 0.7457 0.4505 0.044 Uiso 1 1 calc R . . C7 C 0.1827(5) 0.5924(5) 0.3977(3) 0.0285(14) Uani 1 1 d . . . C8 C 0.1036(5) 0.5233(5) 0.4288(3) 0.0283(14) Uani 1 1 d . . . H8A H 0.1020 0.5593 0.4742 0.034 Uiso 1 1 calc R . . H8B H 0.1305 0.4488 0.4262 0.034 Uiso 1 1 calc R . . C9 C -0.0139(5) 0.5103(5) 0.3971(3) 0.0258(13) Uani 1 1 d . . . C10 C -0.0909(5) 0.5894(6) 0.4188(3) 0.0382(16) Uani 1 1 d . . . H10 H -0.0693 0.6480 0.4543 0.046 Uiso 1 1 calc R . . C11 C -0.1981(6) 0.5843(7) 0.3896(3) 0.0466(19) Uani 1 1 d . . . C12 C -0.2278(5) 0.4959(6) 0.3380(3) 0.0375(16) Uani 1 1 d . . . H12 H -0.3001 0.4895 0.3187 0.045 Uiso 1 1 calc R . . C13 C -0.1548(5) 0.4147(5) 0.3130(3) 0.0264(13) Uani 1 1 d . . . C14 C -0.1892(5) 0.3267(5) 0.2515(3) 0.0286(14) Uani 1 1 d . . . H14A H -0.1447 0.2622 0.2494 0.034 Uiso 1 1 calc R . . H14B H -0.2673 0.3003 0.2516 0.034 Uiso 1 1 calc R . . C15 C -0.1724(5) 0.3765(5) 0.1935(3) 0.0257(13) Uani 1 1 d . . . C16 C -0.2489(5) 0.4475(5) 0.1747(3) 0.0305(14) Uani 1 1 d . . . H16 H -0.3143 0.4571 0.1962 0.037 Uiso 1 1 calc R . . C17 C -0.2319(5) 0.5028(5) 0.1267(3) 0.0332(15) Uani 1 1 d . . . C18 C -0.1325(5) 0.4905(5) 0.0957(3) 0.0276(14) Uani 1 1 d . . . H18 H -0.1182 0.5314 0.0643 0.033 Uiso 1 1 calc R . . C19 C -0.0534(5) 0.4181(5) 0.1107(3) 0.0234(13) Uani 1 1 d . . . C20 C 0.0547(5) 0.4066(5) 0.0771(3) 0.0252(13) Uani 1 1 d . . . H20A H 0.0407 0.4126 0.0326 0.030 Uiso 1 1 calc R . . H20B H 0.0799 0.3321 0.0766 0.030 Uiso 1 1 calc R . . C21 C 0.1468(4) 0.4964(5) 0.1098(3) 0.0225(13) Uani 1 1 d . . . C22 C 0.1638(5) 0.5969(5) 0.0885(3) 0.0273(14) Uani 1 1 d . . . H22 H 0.1175 0.6076 0.0541 0.033 Uiso 1 1 calc R . . C23 C 0.2460(5) 0.6811(5) 0.1161(3) 0.0306(14) Uani 1 1 d . . . C24 C 0.3125(5) 0.6620(5) 0.1687(3) 0.0268(13) Uani 1 1 d . . . H24 H 0.3686 0.7173 0.1882 0.032 Uiso 1 1 calc R . . C25 C 0.2153(5) 0.4805(5) 0.1612(3) 0.0250(13) Uani 1 1 d . . . C26 C 0.2452(5) 0.5436(5) 0.3466(3) 0.0256(13) Uani 1 1 d . . . C27 C -0.0483(5) 0.4237(5) 0.3440(3) 0.0272(14) Uani 1 1 d . . . C28 C -0.0766(5) 0.3597(5) 0.1584(3) 0.0264(14) Uani 1 1 d . . . C30 C 0.2721(8) 0.9071(6) 0.4095(4) 0.063(2) Uani 1 1 d . . . C31 C 0.1738(11) 0.9500(8) 0.4408(8) 0.127(5) Uani 1 1 d . . . H31A H 0.1077 0.9190 0.4136 0.191 Uiso 1 1 calc R . . H31B H 0.1788 1.0312 0.4478 0.191 Uiso 1 1 calc R . . H31C H 0.1701 0.9282 0.4815 0.191 Uiso 1 1 calc R . . C32 C 0.3799(11) 0.9436(9) 0.4415(11) 0.229(13) Uani 1 1 d . . . H32A H 0.4364 0.9099 0.4150 0.343 Uiso 1 1 calc R . . H32B H 0.3846 0.9210 0.4821 0.343 Uiso 1 1 calc R . . H32C H 0.3914 1.0247 0.4489 0.343 Uiso 1 1 calc R . . C33 C 0.2566(15) 0.9616(9) 0.3485(7) 0.139(6) Uani 1 1 d . . . H33A H 0.1843 0.9362 0.3268 0.208 Uiso 1 1 calc R . . H33B H 0.3137 0.9388 0.3195 0.208 Uiso 1 1 calc R . . H33C H 0.2625 1.0427 0.3623 0.208 Uiso 1 1 calc R . . C40 C -0.2775(8) 0.6756(9) 0.4142(4) 0.080(3) Uani 1 1 d . . . C41 C -0.2199(13) 0.7962(10) 0.4017(7) 0.126(5) Uani 1 1 d . . . H41A H -0.1478 0.8135 0.4249 0.189 Uiso 1 1 calc R . . H41B H -0.2671 0.8560 0.4166 0.189 Uiso 1 1 calc R . . H41C H -0.2115 0.7892 0.3563 0.189 Uiso 1 1 calc R . . C42 C -0.3747(12) 0.6726(13) 0.3742(6) 0.152(7) Uani 1 1 d . . . H42A H -0.3566 0.6570 0.3299 0.227 Uiso 1 1 calc R . . H42B H -0.4063 0.7445 0.3846 0.227 Uiso 1 1 calc R . . H42C H -0.4280 0.6142 0.3809 0.227 Uiso 1 1 calc R . . C43 C -0.2761(9) 0.7048(9) 0.4836(4) 0.080(3) Uani 1 1 d . . . H43A H -0.2013 0.7035 0.5017 0.121 Uiso 1 1 calc R . . H43B H -0.3251 0.6510 0.4982 0.121 Uiso 1 1 calc R . . H43C H -0.3011 0.7793 0.4972 0.121 Uiso 1 1 calc R . . C50 C -0.3249(7) 0.5769(7) 0.1066(4) 0.056(2) Uani 1 1 d . . . C51 C -0.4367(7) 0.5020(8) 0.0901(5) 0.071(3) Uani 1 1 d . . . H51A H -0.4553 0.4711 0.1266 0.107 Uiso 1 1 calc R . . H51B H -0.4290 0.4413 0.0536 0.107 Uiso 1 1 calc R . . H51C H -0.4951 0.5471 0.0800 0.107 Uiso 1 1 calc R . . C52 C -0.3437(8) 0.6704(7) 0.1640(5) 0.068(2) Uani 1 1 d . . . H52A H -0.3581 0.6382 0.2006 0.103 Uiso 1 1 calc R . . H52B H -0.4068 0.7096 0.1538 0.103 Uiso 1 1 calc R . . H52C H -0.2782 0.7226 0.1741 0.103 Uiso 1 1 calc R . . C53 C -0.2958(4) 0.6225(4) 0.0483(3) 0.098(4) Uani 1 1 d . . . H53A H -0.3541 0.6671 0.0376 0.147 Uiso 1 1 calc R . . H53B H -0.2885 0.5605 0.0125 0.147 Uiso 1 1 calc R . . H53C H -0.2263 0.6688 0.0579 0.147 Uiso 1 1 calc R . . C60 C 0.2658(4) 0.7903(4) 0.0926(3) 0.0399(16) Uani 1 1 d R . . C61 C 0.3799(4) 0.7944(4) 0.0655(3) 0.097(4) Uani 1 1 d R . . H61A H 0.4359 0.7831 0.0970 0.145 Uiso 1 1 calc R . . H61B H 0.3959 0.8669 0.0552 0.145 Uiso 1 1 calc R . . H61C H 0.3802 0.7358 0.0270 0.145 Uiso 1 1 calc R . . C62 C 0.2673(10) 0.8938(6) 0.1523(5) 0.081(3) Uani 1 1 d . . . H62A H 0.3271 0.8892 0.1833 0.122 Uiso 1 1 calc R . . H62B H 0.1972 0.8920 0.1720 0.122 Uiso 1 1 calc R . . H62C H 0.2787 0.9633 0.1379 0.122 Uiso 1 1 calc R . . C63 C 0.1730(5) 0.8050(5) 0.0447(3) 0.085(3) Uani 1 1 d . . . H63A H 0.1021 0.7991 0.0633 0.128 Uiso 1 1 calc R . . H63B H 0.1732 0.7470 0.0060 0.128 Uiso 1 1 calc R . . H63C H 0.1846 0.8781 0.0346 0.128 Uiso 1 1 calc R . . C70 C 0.3316(5) 0.3805(5) 0.3628(3) 0.0521(19) Uani 1 1 d R . . H70A H 0.4037 0.4050 0.3497 0.063 Uiso 1 1 calc R . . H70B H 0.3301 0.4073 0.4092 0.063 Uiso 1 1 calc R . . C71 C 0.3124(7) 0.2551(6) 0.3447(4) 0.053(2) Uani 1 1 d . . . H71A H 0.2383 0.2327 0.3561 0.064 Uiso 1 1 calc R . . H71B H 0.3666 0.2223 0.3693 0.064 Uiso 1 1 calc R . . C72 C 0.3228(6) 0.2059(7) 0.2689(5) 0.062(2) Uani 1 1 d . . . H72A H 0.2874 0.2550 0.2448 0.074 Uiso 1 1 calc R . . H72B H 0.2825 0.1316 0.2565 0.074 Uiso 1 1 calc R . . C73 C 0.5919(9) 0.0321(11) 0.2603(8) 0.123(5) Uani 1 1 d . . . H73A H 0.6081 0.0164 0.2151 0.147 Uiso 1 1 calc R . . H73B H 0.6493 0.0881 0.2839 0.147 Uiso 1 1 calc R . . C74 C 0.5977(9) -0.0670(10) 0.2830(7) 0.109(4) Uani 1 1 d . . . H74A H 0.6723 -0.0908 0.2802 0.163 Uiso 1 1 calc R . . H74B H 0.5460 -0.1253 0.2573 0.163 Uiso 1 1 calc R . . H74C H 0.5786 -0.0532 0.3273 0.163 Uiso 1 1 calc R . . C75 C 0.4640(16) 0.2352(14) 0.1351(7) 0.164(8) Uani 1 1 d . . . H75A H 0.5390 0.2427 0.1208 0.197 Uiso 1 1 calc R . . H75B H 0.4475 0.3083 0.1603 0.197 Uiso 1 1 calc R . . C76 C 0.372(3) 0.195(3) 0.0706(13) 0.33(2) Uani 1 1 d . . . H76A H 0.3730 0.2530 0.0458 0.497 Uiso 1 1 calc R . . H76B H 0.2977 0.1849 0.0848 0.497 Uiso 1 1 calc R . . H76C H 0.3910 0.1256 0.0442 0.497 Uiso 1 1 calc R . . C80 C -0.0384(7) 0.1639(6) 0.1339(4) 0.053(2) Uani 1 1 d . . . H80A H -0.1138 0.1405 0.1428 0.063 Uiso 1 1 calc R . . H80B H -0.0368 0.1610 0.0879 0.063 Uiso 1 1 calc R . . C81 C 0.0443(8) 0.0876(7) 0.1545(4) 0.065(2) Uani 1 1 d . . . H81A H 0.1192 0.1151 0.1468 0.078 Uiso 1 1 calc R . . H81B H 0.0289 0.0120 0.1276 0.078 Uiso 1 1 calc R . . C82 C 0.0418(7) 0.0803(7) 0.2264(5) 0.068(3) Uani 1 1 d . . . H82A H 0.0283 0.1543 0.2516 0.082 Uiso 1 1 calc R . . H82B H 0.1153 0.0627 0.2408 0.082 Uiso 1 1 calc R . . C83 C -0.0405(12) -0.2371(9) 0.2331(9) 0.135(6) Uani 1 1 d . . . H83A H -0.1108 -0.2329 0.2537 0.162 Uiso 1 1 calc R . . H83B H -0.0596 -0.2696 0.1876 0.162 Uiso 1 1 calc R . . C84 C 0.0128(8) -0.3146(7) 0.2553(4) 0.067(2) Uani 1 1 d . . . H84A H -0.0300 -0.3866 0.2425 0.100 Uiso 1 1 calc R . . H84B H 0.0221 -0.2932 0.3016 0.100 Uiso 1 1 calc R . . H84C H 0.0850 -0.3202 0.2379 0.100 Uiso 1 1 calc R . . C85 C -0.1200(12) 0.0954(11) 0.3555(6) 0.111(4) Uani 1 1 d . . . H85A H -0.1878 0.0642 0.3702 0.133 Uiso 1 1 calc R . . H85B H -0.1413 0.1449 0.3273 0.133 Uiso 1 1 calc R . . C86 C -0.0476(13) 0.1631(14) 0.4128(7) 0.135(5) Uani 1 1 d . . . H86A H -0.0877 0.2239 0.4353 0.203 Uiso 1 1 calc R . . H86B H 0.0197 0.1939 0.3983 0.203 Uiso 1 1 calc R . . H86C H -0.0287 0.1148 0.4415 0.203 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0337(11) 0.0461(12) 0.0836(16) 0.0100(11) -0.0004(10) 0.0119(9) P2 0.0510(13) 0.0404(12) 0.0929(18) 0.0238(11) 0.0014(12) 0.0106(9) O1 0.030(2) 0.019(2) 0.045(3) 0.0096(18) 0.0001(19) 0.0079(17) O2 0.028(2) 0.030(2) 0.060(3) -0.009(2) -0.014(2) 0.0104(19) O3 0.024(2) 0.028(2) 0.048(3) 0.0189(19) 0.0006(19) 0.0057(18) O4 0.030(2) 0.032(2) 0.054(3) 0.027(2) -0.013(2) -0.0027(19) O11 0.047(4) 0.091(5) 0.151(7) -0.009(5) 0.024(4) 0.007(3) O12 0.059(4) 0.091(5) 0.118(6) 0.050(4) 0.024(4) 0.036(3) O13 0.151(7) 0.089(5) 0.091(5) 0.017(4) 0.055(5) -0.012(5) O21 0.069(5) 0.095(5) 0.173(8) 0.063(5) -0.027(5) -0.017(4) O22 0.091(5) 0.023(3) 0.126(6) 0.018(3) -0.018(4) 0.009(3) O23 0.122(6) 0.102(6) 0.101(6) 0.040(5) 0.031(5) 0.035(5) C1 0.024(3) 0.030(3) 0.025(3) 0.005(3) 0.000(2) 0.008(3) C2 0.018(3) 0.031(3) 0.036(3) 0.009(3) -0.006(3) 0.001(2) C3 0.026(3) 0.029(3) 0.027(3) 0.009(3) -0.010(3) 0.000(3) C4 0.038(4) 0.031(4) 0.040(4) 0.011(3) -0.004(3) -0.008(3) C5 0.051(4) 0.029(4) 0.048(4) 0.000(3) -0.007(3) 0.001(3) C6 0.047(4) 0.027(3) 0.034(4) 0.004(3) 0.000(3) -0.001(3) C7 0.032(3) 0.025(3) 0.027(3) 0.002(3) -0.009(3) 0.005(3) C8 0.034(3) 0.025(3) 0.027(3) 0.006(2) -0.002(3) 0.003(3) C9 0.027(3) 0.027(3) 0.028(3) 0.014(3) 0.001(2) 0.004(3) C10 0.040(4) 0.044(4) 0.026(3) -0.005(3) -0.001(3) 0.014(3) C11 0.041(4) 0.066(5) 0.027(4) -0.008(3) -0.005(3) 0.027(4) C12 0.030(4) 0.050(4) 0.031(4) 0.004(3) 0.000(3) 0.010(3) C13 0.022(3) 0.028(3) 0.029(3) 0.009(3) 0.001(3) -0.003(2) C14 0.019(3) 0.027(3) 0.039(4) 0.008(3) 0.000(3) -0.003(2) C15 0.023(3) 0.021(3) 0.029(3) -0.002(2) -0.004(2) -0.003(2) C16 0.024(3) 0.038(4) 0.029(3) 0.004(3) -0.001(3) 0.013(3) C17 0.033(4) 0.039(4) 0.028(3) 0.005(3) 0.003(3) 0.014(3) C18 0.035(3) 0.026(3) 0.025(3) 0.010(3) 0.002(3) 0.007(3) C19 0.022(3) 0.025(3) 0.021(3) 0.002(2) -0.004(2) 0.000(2) C20 0.031(3) 0.025(3) 0.020(3) 0.004(2) 0.001(2) 0.003(3) C21 0.018(3) 0.027(3) 0.022(3) 0.002(2) 0.003(2) 0.007(2) C22 0.028(3) 0.026(3) 0.030(3) 0.013(3) -0.005(3) 0.006(3) C23 0.024(3) 0.031(3) 0.039(4) 0.011(3) 0.003(3) 0.009(3) C24 0.023(3) 0.021(3) 0.037(3) 0.005(3) 0.005(3) 0.005(2) C25 0.021(3) 0.027(3) 0.029(3) 0.008(3) 0.004(2) 0.007(2) C26 0.025(3) 0.019(3) 0.030(3) 0.002(2) -0.012(3) 0.005(2) C27 0.032(3) 0.017(3) 0.035(3) 0.006(3) 0.008(3) 0.007(2) C28 0.026(3) 0.017(3) 0.033(3) 0.000(2) -0.009(3) 0.000(2) C30 0.094(7) 0.024(4) 0.063(5) -0.008(4) 0.014(5) -0.009(4) C31 0.127(11) 0.031(5) 0.201(15) -0.020(7) 0.000(10) 0.001(6) C32 0.116(11) 0.034(6) 0.46(3) -0.084(11) -0.156(16) 0.014(6) C33 0.245(19) 0.039(6) 0.126(11) 0.012(6) -0.023(11) 0.016(8) C40 0.064(6) 0.106(8) 0.057(5) -0.024(5) -0.014(4) 0.057(6) C41 0.163(13) 0.085(9) 0.151(12) 0.048(8) 0.042(10) 0.065(9) C42 0.146(12) 0.188(14) 0.093(8) -0.061(9) -0.043(8) 0.144(11) C43 0.098(7) 0.098(7) 0.047(5) 0.002(5) 0.015(5) 0.062(6) C50 0.062(5) 0.063(5) 0.050(5) 0.015(4) 0.008(4) 0.043(4) C51 0.046(5) 0.086(7) 0.084(6) 0.023(5) -0.023(4) 0.025(5) C52 0.067(6) 0.056(5) 0.090(7) 0.020(5) 0.016(5) 0.040(4) C53 0.092(7) 0.140(10) 0.104(8) 0.087(8) 0.046(6) 0.083(7) C60 0.044(4) 0.030(4) 0.050(4) 0.021(3) -0.003(3) 0.001(3) C61 0.099(8) 0.084(7) 0.139(10) 0.079(7) 0.050(7) 0.032(6) C62 0.119(8) 0.025(4) 0.101(7) 0.019(4) -0.005(6) 0.003(5) C63 0.098(7) 0.047(5) 0.116(8) 0.054(5) -0.053(6) -0.019(5) C70 0.050(5) 0.053(5) 0.057(5) 0.018(4) -0.004(4) 0.011(4) C71 0.050(5) 0.053(5) 0.064(5) 0.024(4) 0.005(4) 0.015(4) C72 0.033(4) 0.046(5) 0.112(7) 0.030(5) 0.000(4) 0.007(3) C73 0.058(6) 0.125(10) 0.218(16) 0.096(11) 0.021(8) 0.044(7) C74 0.079(7) 0.088(8) 0.182(13) 0.065(9) 0.042(8) 0.035(6) C75 0.24(2) 0.165(15) 0.083(9) 0.043(10) 0.024(11) -0.086(14) C76 0.53(6) 0.34(4) 0.17(2) 0.14(3) 0.09(3) 0.03(4) C80 0.058(5) 0.042(4) 0.059(5) 0.015(4) 0.001(4) 0.000(4) C81 0.066(6) 0.050(5) 0.083(6) 0.019(4) 0.015(5) 0.009(4) C82 0.051(5) 0.044(5) 0.116(8) 0.028(5) -0.002(5) 0.013(4) C83 0.128(11) 0.052(7) 0.229(18) 0.048(9) -0.008(11) 0.007(7) C84 0.086(6) 0.043(5) 0.070(6) 0.013(4) -0.017(5) 0.013(4) C85 0.133(11) 0.112(10) 0.099(9) 0.034(8) 0.033(9) 0.045(9) C86 0.138(13) 0.172(15) 0.099(10) 0.042(10) 0.013(9) -0.012(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O11 1.407(7) . ? P1 O13 1.547(8) . ? P1 O12 1.576(6) . ? P1 C72 1.755(8) . ? P2 O21 1.417(7) . ? P2 O22 1.508(6) . ? P2 O23 1.602(8) . ? P2 C82 1.771(9) . ? O1 C26 1.398(7) . ? O1 C70 1.494(7) . ? O2 C27 1.376(7) . ? O2 H2AO 0.8200 . ? O3 C28 1.394(7) . ? O3 C80 1.518(8) . ? O4 C25 1.366(7) . ? O4 H4AO 0.8200 . ? O12 C73 1.433(11) . ? O13 C75 1.392(15) . ? O22 C83 1.343(12) . ? O23 C85 1.407(13) . ? C1 C24 1.374(8) . ? C1 C25 1.414(8) . ? C1 C2 1.518(8) . ? C2 C3 1.527(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.370(9) . ? C3 C26 1.391(8) . ? C4 C5 1.408(10) . ? C4 H4A 0.9300 . ? C5 C6 1.370(10) . ? C5 C30 1.529(10) . ? C6 C7 1.401(9) . ? C6 H6 0.9300 . ? C7 C26 1.399(8) . ? C7 C8 1.497(8) . ? C8 C9 1.512(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C27 1.389(8) . ? C9 C10 1.399(8) . ? C10 C11 1.390(9) . ? C10 H10 0.9300 . ? C11 C12 1.370(9) . ? C11 C40 1.532(10) . ? C12 C13 1.399(9) . ? C12 H12 0.9300 . ? C13 C27 1.392(8) . ? C13 C14 1.515(8) . ? C14 C15 1.502(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.398(8) . ? C15 C28 1.404(8) . ? C16 C17 1.352(9) . ? C16 H16 0.9300 . ? C17 C18 1.393(9) . ? C17 C50 1.576(9) . ? C18 C19 1.404(8) . ? C18 H18 0.9300 . ? C19 C28 1.386(8) . ? C19 C20 1.512(8) . ? C20 C21 1.524(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C25 1.385(8) . ? C21 C22 1.395(8) . ? C22 C23 1.380(8) . ? C22 H22 0.9300 . ? C23 C24 1.406(8) . ? C23 C60 1.520(7) . ? C24 H24 0.9300 . ? C30 C32 1.424(14) . ? C30 C31 1.455(15) . ? C30 C33 1.584(15) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C40 C42 1.399(13) . ? C40 C43 1.440(12) . ? C40 C41 1.654(17) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C50 C53 1.507(9) . ? C50 C52 1.513(11) . ? C50 C51 1.548(12) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C60 C63 1.513(7) . ? C60 C61 1.5151 . ? C60 C62 1.578(11) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C70 C71 1.484(9) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.606(12) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.392(14) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C76 1.68(3) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C80 C81 1.511(11) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82 1.550(13) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.325(13) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 C86 1.508(18) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 P1 O13 114.3(5) . . ? O11 P1 O12 118.1(5) . . ? O13 P1 O12 98.8(4) . . ? O11 P1 C72 115.7(4) . . ? O13 P1 C72 107.5(5) . . ? O12 P1 C72 100.3(4) . . ? O21 P2 O22 118.7(4) . . ? O21 P2 O23 111.5(5) . . ? O22 P2 O23 97.7(4) . . ? O21 P2 C82 115.5(4) . . ? O22 P2 C82 105.5(4) . . ? O23 P2 C82 105.9(5) . . ? C26 O1 C70 110.3(4) . . ? C27 O2 H2AO 109.5 . . ? C28 O3 C80 110.8(4) . . ? C25 O4 H4AO 109.5 . . ? C73 O12 P1 122.9(6) . . ? C75 O13 P1 119.8(9) . . ? C83 O22 P2 132.6(8) . . ? C85 O23 P2 123.6(8) . . ? C24 C1 C25 118.1(5) . . ? C24 C1 C2 120.6(5) . . ? C25 C1 C2 121.3(5) . . ? C1 C2 C3 110.1(5) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C26 117.7(6) . . ? C4 C3 C2 120.1(5) . . ? C26 C3 C2 122.1(5) . . ? C3 C4 C5 122.6(6) . . ? C3 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? C6 C5 C4 117.3(6) . . ? C6 C5 C30 121.9(7) . . ? C4 C5 C30 120.8(7) . . ? C5 C6 C7 123.2(6) . . ? C5 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C26 C7 C6 116.5(6) . . ? C26 C7 C8 122.4(5) . . ? C6 C7 C8 121.0(6) . . ? C7 C8 C9 112.1(5) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C27 C9 C10 117.2(5) . . ? C27 C9 C8 122.1(5) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 123.0(6) . . ? C11 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C12 C11 C10 117.0(6) . . ? C12 C11 C40 122.4(6) . . ? C10 C11 C40 120.6(6) . . ? C11 C12 C13 123.2(6) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C27 C13 C12 117.4(5) . . ? C27 C13 C14 122.2(5) . . ? C12 C13 C14 120.3(5) . . ? C15 C14 C13 110.2(5) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C28 117.4(5) . . ? C16 C15 C14 120.8(5) . . ? C28 C15 C14 121.6(5) . . ? C17 C16 C15 122.9(6) . . ? C17 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 C17 C18 118.4(6) . . ? C16 C17 C50 119.6(6) . . ? C18 C17 C50 122.0(6) . . ? C17 C18 C19 121.8(5) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C28 C19 C18 117.6(5) . . ? C28 C19 C20 121.1(5) . . ? C18 C19 C20 121.2(5) . . ? C19 C20 C21 112.5(4) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C25 C21 C22 118.6(5) . . ? C25 C21 C20 121.1(5) . . ? C22 C21 C20 120.3(5) . . ? C23 C22 C21 123.0(5) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C22 C23 C24 116.5(5) . . ? C22 C23 C60 123.3(5) . . ? C24 C23 C60 120.3(5) . . ? C1 C24 C23 123.2(6) . . ? C1 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? O4 C25 C21 122.5(5) . . ? O4 C25 C1 116.8(5) . . ? C21 C25 C1 120.7(5) . . ? C3 C26 O1 119.7(5) . . ? C3 C26 C7 122.6(5) . . ? O1 C26 C7 117.7(5) . . ? O2 C27 C9 121.1(5) . . ? O2 C27 C13 116.8(5) . . ? C9 C27 C13 122.1(5) . . ? C19 C28 O3 119.5(5) . . ? C19 C28 C15 121.6(5) . . ? O3 C28 C15 118.9(5) . . ? C32 C30 C31 118.7(11) . . ? C32 C30 C5 110.5(8) . . ? C31 C30 C5 111.7(7) . . ? C32 C30 C33 109.6(13) . . ? C31 C30 C33 96.5(11) . . ? C5 C30 C33 108.6(7) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C42 C40 C43 122.6(9) . . ? C42 C40 C11 115.1(7) . . ? C43 C40 C11 112.6(7) . . ? C42 C40 C41 95.9(11) . . ? C43 C40 C41 99.1(9) . . ? C11 C40 C41 106.8(8) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C53 C50 C52 112.1(7) . . ? C53 C50 C51 108.7(6) . . ? C52 C50 C51 106.3(7) . . ? C53 C50 C17 111.8(6) . . ? C52 C50 C17 109.1(6) . . ? C51 C50 C17 108.5(6) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C63 C60 C61 112.3(3) . . ? C63 C60 C23 112.1(5) . . ? C61 C60 C23 109.5(3) . . ? C63 C60 C62 106.8(5) . . ? C61 C60 C62 107.2(5) . . ? C23 C60 C62 108.8(5) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C71 C70 O1 106.3(5) . . ? C71 C70 H70A 110.5 . . ? O1 C70 H70A 110.5 . . ? C71 C70 H70B 110.5 . . ? O1 C70 H70B 110.5 . . ? H70A C70 H70B 108.7 . . ? C70 C71 C72 112.3(6) . . ? C70 C71 H71A 109.1 . . ? C72 C71 H71A 109.1 . . ? C70 C71 H71B 109.1 . . ? C72 C71 H71B 109.1 . . ? H71A C71 H71B 107.9 . . ? C71 C72 P1 113.5(6) . . ? C71 C72 H72A 108.9 . . ? P1 C72 H72A 108.9 . . ? C71 C72 H72B 108.9 . . ? P1 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? C74 C73 O12 113.9(10) . . ? C74 C73 H73A 108.8 . . ? O12 C73 H73A 108.8 . . ? C74 C73 H73B 108.8 . . ? O12 C73 H73B 108.8 . . ? H73A C73 H73B 107.7 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O13 C75 C76 110.2(14) . . ? O13 C75 H75A 109.6 . . ? C76 C75 H75A 109.6 . . ? O13 C75 H75B 109.6 . . ? C76 C75 H75B 109.6 . . ? H75A C75 H75B 108.1 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C81 C80 O3 106.3(6) . . ? C81 C80 H80A 110.5 . . ? O3 C80 H80A 110.5 . . ? C81 C80 H80B 110.5 . . ? O3 C80 H80B 110.5 . . ? H80A C80 H80B 108.7 . . ? C80 C81 C82 114.1(7) . . ? C80 C81 H81A 108.7 . . ? C82 C81 H81A 108.7 . . ? C80 C81 H81B 108.7 . . ? C82 C81 H81B 108.7 . . ? H81A C81 H81B 107.6 . . ? C81 C82 P2 115.9(6) . . ? C81 C82 H82A 108.3 . . ? P2 C82 H82A 108.3 . . ? C81 C82 H82B 108.3 . . ? P2 C82 H82B 108.3 . . ? H82A C82 H82B 107.4 . . ? C84 C83 O22 126.6(12) . . ? C84 C83 H83A 105.7 . . ? O22 C83 H83A 105.7 . . ? C84 C83 H83B 105.7 . . ? O22 C83 H83B 105.7 . . ? H83A C83 H83B 106.1 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O23 C85 C86 111.1(12) . . ? O23 C85 H85A 109.4 . . ? C86 C85 H85A 109.4 . . ? O23 C85 H85B 109.4 . . ? C86 C85 H85B 109.4 . . ? H85A C85 H85B 108.0 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.445 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.120 data_end3b #in paper label 3b _database_code_CSD 179149 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50H70O10P2 * 2.5H2O * 4.5MeOH (some H-atoms not found)' _chemical_formula_sum 'C436 H572 O132 P16' _chemical_formula_weight 8420.46 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.454(10) _cell_length_b 17.486(3) _cell_length_c 21.540(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.03(2) _cell_angle_gamma 90.00 _cell_volume 12459(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 29.34 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4484 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; measured in frozen drop of Apiezon fat (highly instable in air do to loss of solvent molecules ; _diffrn_ambient_temperature 180(1) _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 'KUMA (Poland)' _diffrn_measurement_method '.omega.-scan (0.5.degree)' _diffrn_detector_area_resol_mean '16.7 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34044 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 29.34 _reflns_number_total 14684 _reflns_number_gt 6230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA (Poland)' _computing_cell_refinement 'KUMA (Poland)' _computing_data_reduction 'KUMA (Poland)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON-92 (Spek, 1992)' _computing_publication_material 'WORD' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14684 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1946 _refine_ls_R_factor_gt 0.1175 _refine_ls_wR_factor_ref 0.3693 _refine_ls_wR_factor_gt 0.3381 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.38678(4) -0.12703(9) 0.68338(7) 0.0715(4) Uani 1 1 d . . . P2 P 0.40996(4) 0.00694(9) 0.54525(7) 0.0693(4) Uani 1 1 d . . . O1 O 0.24966(9) -0.06484(17) 0.44346(15) 0.0513(7) Uani 1 1 d . . . O2 O 0.27170(10) 0.07484(17) 0.42102(16) 0.0562(8) Uani 1 1 d . . . O3 O 0.29386(8) 0.04073(15) 0.30989(14) 0.0462(7) Uani 1 1 d . . . O4 O 0.25951(9) -0.09336(16) 0.31363(15) 0.0523(7) Uani 1 1 d . . . O11 O 0.40383(10) -0.1609(3) 0.6412(2) 0.0838(11) Uani 1 1 d . . . O12 O 0.40071(13) -0.1791(3) 0.75150(19) 0.0996(14) Uani 1 1 d . . . O13 O 0.39825(15) -0.0439(3) 0.6999(2) 0.1132(17) Uani 1 1 d . . . O21 O 0.40846(13) 0.0442(3) 0.6091(2) 0.0974(13) Uani 1 1 d . . . O22 O 0.41059(11) -0.0775(2) 0.5498(2) 0.0803(11) Uani 1 1 d . . . O23 O 0.44675(12) 0.0334(3) 0.5459(2) 0.0959(13) Uani 1 1 d . . . C1 C 0.19669(14) -0.1562(2) 0.2541(2) 0.0507(10) Uani 1 1 d . . . C2 C 0.20455(14) -0.1781(2) 0.3286(2) 0.0525(10) Uani 1 1 d . . . H2A H 0.2334 -0.1803 0.3649 0.063 Uiso 1 1 calc R . . H2B H 0.1933 -0.2283 0.3255 0.063 Uiso 1 1 calc R . . C3 C 0.18534(13) -0.1195(3) 0.3526(2) 0.0498(10) Uani 1 1 d . . . C4 C 0.14350(14) -0.1181(3) 0.3170(2) 0.0575(11) Uani 1 1 d . . . H4 H 0.1283 -0.1573 0.2844 0.069 Uiso 1 1 calc R . . C5 C 0.12348(16) -0.0594(3) 0.3288(3) 0.0657(13) Uani 1 1 d . . . C6 C 0.14693(16) -0.0023(3) 0.3783(3) 0.0626(13) Uani 1 1 d . . . H6 H 0.1341 0.0376 0.3863 0.075 Uiso 1 1 calc R . . C7 C 0.18942(14) -0.0022(3) 0.4170(2) 0.0544(11) Uani 1 1 d . . . C8 C 0.21366(16) 0.0642(3) 0.4658(3) 0.0591(12) Uani 1 1 d . . . H8A H 0.2410 0.0474 0.5019 0.071 Uiso 1 1 calc R . . H8B H 0.2017 0.0820 0.4924 0.071 Uiso 1 1 calc R . . C9 C 0.21491(15) 0.1302(2) 0.4202(2) 0.0539(11) Uani 1 1 d . . . C10 C 0.18690(15) 0.1900(3) 0.3958(2) 0.0589(12) Uani 1 1 d . . . H10 H 0.1680 0.1892 0.4089 0.071 Uiso 1 1 calc R . . C11 C 0.18590(15) 0.2504(3) 0.3532(2) 0.0582(12) Uani 1 1 d . . . C12 C 0.21622(14) 0.2505(2) 0.3386(2) 0.0526(11) Uani 1 1 d . . . H12 H 0.2177 0.2921 0.3133 0.063 Uiso 1 1 calc R . . C13 C 0.24398(13) 0.1928(2) 0.3592(2) 0.0459(10) Uani 1 1 d . . . C14 C 0.27364(13) 0.1923(2) 0.3347(2) 0.0486(10) Uani 1 1 d . . . H14A H 0.2816 0.2443 0.3328 0.058 Uiso 1 1 calc R . . H14B H 0.2977 0.1639 0.3702 0.058 Uiso 1 1 calc R . . C15 C 0.25431(13) 0.1559(2) 0.2592(2) 0.0470(10) Uani 1 1 d . . . C16 C 0.22359(13) 0.1948(2) 0.1968(2) 0.0477(10) Uani 1 1 d . . . H16 H 0.2182 0.2454 0.2020 0.057 Uiso 1 1 calc R . . C17 C 0.20085(13) 0.1607(2) 0.1271(2) 0.0457(9) Uani 1 1 d . . . C18 C 0.21012(13) 0.0849(2) 0.1209(2) 0.0457(10) Uani 1 1 d . . . H18 H 0.1951 0.0608 0.0751 0.055 Uiso 1 1 calc R . . C19 C 0.24089(12) 0.0444(2) 0.1807(2) 0.0434(9) Uani 1 1 d . . . C20 C 0.24530(13) -0.0406(2) 0.1723(2) 0.0442(9) Uani 1 1 d . . . H20A H 0.2411 -0.0497 0.1241 0.053 Uiso 1 1 calc R . . H20B H 0.2727 -0.0562 0.2096 0.053 Uiso 1 1 calc R . . C21 C 0.21608(14) -0.0886(2) 0.1796(2) 0.0481(10) Uani 1 1 d . . . C22 C 0.17909(13) -0.1091(2) 0.1167(2) 0.0489(10) Uani 1 1 d . . . H22 H 0.1732 -0.0925 0.0708 0.059 Uiso 1 1 calc R . . C23 C 0.15062(14) -0.1533(3) 0.1194(2) 0.0515(10) Uani 1 1 d . . . C24 C 0.16051(13) -0.1767(2) 0.1885(2) 0.0499(10) Uani 1 1 d . . . H24 H 0.1423 -0.2075 0.1917 0.060 Uiso 1 1 calc R . . C25 C 0.22428(12) -0.1117(2) 0.2483(2) 0.0444(9) Uani 1 1 d . . . C26 C 0.20751(14) -0.0625(3) 0.4048(2) 0.0504(10) Uani 1 1 d . . . C27 C 0.24353(14) 0.1312(2) 0.4010(2) 0.0489(10) Uani 1 1 d . . . C28 C 0.26325(13) 0.0814(2) 0.2493(2) 0.0457(10) Uani 1 1 d . . . C30 C 0.07756(17) -0.0580(4) 0.2876(3) 0.0854(18) Uani 1 1 d . . . C31 C 0.0589(2) -0.0684(7) 0.2089(4) 0.149(4) Uani 1 1 d . . . H31A H 0.0669 -0.1170 0.2000 0.223 Uiso 1 1 calc R . . H31B H 0.0675 -0.0283 0.1900 0.223 Uiso 1 1 calc R . . H31C H 0.0301 -0.0669 0.1844 0.223 Uiso 1 1 calc R . . C32 C 0.0651(2) -0.1115(12) 0.3204(8) 0.316(13) Uani 1 1 d . . . H32A H 0.0381 -0.1285 0.2843 0.474 Uiso 1 1 calc R . . H32B H 0.0655 -0.0879 0.3611 0.474 Uiso 1 1 calc R . . H32C H 0.0831 -0.1546 0.3381 0.474 Uiso 1 1 calc R . . C33 C 0.0630(3) 0.0189(10) 0.2991(8) 0.253(10) Uani 1 1 d . . . H33A H 0.0347 0.0156 0.2805 0.380 Uiso 1 1 calc R . . H33B H 0.0672 0.0583 0.2730 0.380 Uiso 1 1 calc R . . H33C H 0.0778 0.0309 0.3509 0.380 Uiso 1 1 calc R . . C40 C 0.15492(15) 0.3153(3) 0.3275(3) 0.0607(12) Uani 1 1 d . . . C41 C 0.11709(18) 0.2899(3) 0.3228(4) 0.0851(17) Uani 1 1 d . . . H41A H 0.1067 0.2446 0.2930 0.128 Uiso 1 1 calc R . . H41B H 0.0972 0.3298 0.3008 0.128 Uiso 1 1 calc R . . H41C H 0.1233 0.2792 0.3717 0.128 Uiso 1 1 calc R . . C42 C 0.1740(2) 0.3832(4) 0.3750(5) 0.123(3) Uani 1 1 d . . . H42A H 0.1760 0.3758 0.4211 0.184 Uiso 1 1 calc R . . H42B H 0.1578 0.4275 0.3505 0.184 Uiso 1 1 calc R . . H42C H 0.2005 0.3903 0.3843 0.184 Uiso 1 1 calc R . . C43 C 0.1405(3) 0.3385(4) 0.2463(4) 0.119(3) Uani 1 1 d . . . H43A H 0.1623 0.3629 0.2463 0.178 Uiso 1 1 calc R . . H43B H 0.1181 0.3732 0.2271 0.178 Uiso 1 1 calc R . . H43C H 0.1323 0.2936 0.2158 0.178 Uiso 1 1 calc R . . C50 C 0.16571(13) 0.2012(2) 0.0600(2) 0.0498(10) Uani 1 1 d . . . C51 C 0.16001(15) 0.2836(3) 0.0774(2) 0.0614(12) Uani 1 1 d . . . H51A H 0.1368 0.3058 0.0344 0.092 Uiso 1 1 calc R . . H51B H 0.1836 0.3132 0.0911 0.092 Uiso 1 1 calc R . . H51C H 0.1560 0.2834 0.1175 0.092 Uiso 1 1 calc R . . C52 C 0.17265(15) 0.2030(3) -0.0030(2) 0.0597(12) Uani 1 1 d . . . H52A H 0.1754 0.1516 -0.0154 0.090 Uiso 1 1 calc R . . H52B H 0.1968 0.2312 0.0123 0.090 Uiso 1 1 calc R . . H52C H 0.1500 0.2271 -0.0455 0.090 Uiso 1 1 calc R . . C53 C 0.12704(15) 0.1562(3) 0.0353(3) 0.0719(14) Uani 1 1 d . . . H53A H 0.1043 0.1818 -0.0058 0.108 Uiso 1 1 calc R . . H53B H 0.1232 0.1529 0.0756 0.108 Uiso 1 1 calc R . . H53C H 0.1293 0.1056 0.0205 0.108 Uiso 1 1 calc R . . C60 C 0.11004(15) -0.1741(3) 0.0479(3) 0.0616(12) Uani 1 1 d . . . C61 C 0.0851(2) -0.2278(5) 0.0631(4) 0.111(2) Uani 1 1 d . . . H61A H 0.0580 -0.2303 0.0202 0.166 Uiso 1 1 calc R . . H61B H 0.0847 -0.2092 0.1045 0.166 Uiso 1 1 calc R . . H61C H 0.0970 -0.2779 0.0741 0.166 Uiso 1 1 calc R . . C62 C 0.11771(19) -0.2108(4) -0.0081(3) 0.0894(18) Uani 1 1 d . . . H62A H 0.0924 -0.2260 -0.0514 0.134 Uiso 1 1 calc R . . H62B H 0.1347 -0.2549 0.0138 0.134 Uiso 1 1 calc R . . H62C H 0.1308 -0.1745 -0.0217 0.134 Uiso 1 1 calc R . . C63 C 0.0868(2) -0.0992(4) 0.0175(4) 0.106(2) Uani 1 1 d . . . H63A H 0.1000 -0.0677 0.0004 0.160 Uiso 1 1 calc R . . H63B H 0.0861 -0.0730 0.0559 0.160 Uiso 1 1 calc R . . H63C H 0.0597 -0.1099 -0.0229 0.160 Uiso 1 1 calc R . . C70 C 0.26786(13) -0.1044(3) 0.5129(2) 0.0495(10) Uani 1 1 d . . . H70A H 0.2611 -0.1584 0.5043 0.059 Uiso 1 1 calc R . . H70B H 0.2577 -0.0840 0.5416 0.059 Uiso 1 1 calc R . . C71 C 0.31244(14) -0.0944(3) 0.5543(2) 0.0515(10) Uani 1 1 d . . . H71A H 0.3191 -0.0405 0.5637 0.062 Uiso 1 1 calc R . . H71B H 0.3224 -0.1135 0.5248 0.062 Uiso 1 1 calc R . . C72 C 0.33306(14) -0.1383(3) 0.6289(2) 0.0586(12) Uani 1 1 d . . . H72A H 0.3267 -0.1923 0.6189 0.070 Uiso 1 1 calc R . . H72B H 0.3221 -0.1202 0.6571 0.070 Uiso 1 1 calc R . . C80 C 0.33294(14) 0.0496(3) 0.3203(3) 0.0596(12) Uani 1 1 d . . . H80A H 0.3398 0.1034 0.3239 0.072 Uiso 1 1 calc R . . H80B H 0.3327 0.0278 0.2786 0.072 Uiso 1 1 calc R . . C81 C 0.36396(13) 0.0081(3) 0.3919(2) 0.0579(11) Uani 1 1 d . . . H81A H 0.3565 -0.0454 0.3873 0.070 Uiso 1 1 calc R . . H81B H 0.3902 0.0109 0.3981 0.070 Uiso 1 1 calc R . . C82 C 0.36749(17) 0.0405(3) 0.4605(3) 0.0723(14) Uani 1 1 d . . . H82A H 0.3431 0.0278 0.4591 0.087 Uiso 1 1 calc R . . H82B H 0.3690 0.0958 0.4593 0.087 Uiso 1 1 calc R . . O99M O 0.13609(13) 0.1155(2) 0.2197(2) 0.0922(12) Uani 1 1 d . . . C99M C 0.15703(17) 0.0500(3) 0.2188(3) 0.0672(13) Uani 1 1 d . . . H99A H 0.1817 0.0656 0.2236 0.101 Uiso 1 1 calc R . . H99B H 0.1404 0.0231 0.1730 0.101 Uiso 1 1 calc R . . H99C H 0.1632 0.0171 0.2594 0.101 Uiso 1 1 calc R . . O98M O 0.0627(2) 0.4869(4) 0.1638(4) 0.125(2) Uani 0.75 1 d P . . C98M C 0.0422(3) 0.5578(10) 0.1101(4) 0.163(5) Uani 1 1 d . . . O98X O 0.0424(7) 0.631(2) 0.1285(7) 0.182(17) Uani 0.25 1 d P . . O97M O 0.0341(3) 0.6721(5) 0.4535(4) 0.100(4) Uani 0.526(12) 1 d P . . C97M C 0.0514(5) 0.6619(9) 0.5427(10) 0.221(7) Uani 1 1 d . . . O97X O 0.0341(3) 0.6908(5) 0.5761(7) 0.115(5) Uani 0.474(12) 1 d P . . O96M O 0.0587(2) 0.1542(4) 0.1184(3) 0.155(2) Uani 1 1 d . . . C96M C 0.0405(3) 0.1046(5) 0.0610(5) 0.128(3) Uani 1 1 d . . . H96A H 0.0186 0.1298 0.0183 0.192 Uiso 1 1 calc R . . H96B H 0.0304 0.0618 0.0739 0.192 Uiso 1 1 calc R . . H96C H 0.0598 0.0870 0.0501 0.192 Uiso 1 1 calc R . . O95M O 0.0082(3) 0.2336(5) 0.1411(5) 0.100(3) Uani 0.50 1 d P . . C95M C 0.0013(5) 0.1946(10) 0.3113(8) 0.114(5) Uani 0.50 1 d P . . H95A H 0.0213 0.2232 0.3089 0.171 Uiso 0.50 1 calc PR . . H95B H -0.0227 0.1901 0.2626 0.171 Uiso 0.50 1 calc PR . . H95C H 0.0116 0.1445 0.3308 0.171 Uiso 0.50 1 calc PR . . O99W O -0.0192(4) 0.3481(7) 0.1033(9) 0.061(4) Uani 0.25 1 d P . . O98W O -0.0481(5) 0.4661(8) 0.2341(7) 0.086(5) Uani 0.25 1 d P . . O97W O 0.0164(5) 0.6568(9) 0.2717(9) 0.086(5) Uani 0.25 1 d P . . O96W O 0.0216(3) 0.7247(6) 0.1774(6) 0.121(3) Uani 0.50 1 d P . . O95W O 0.0000 0.567(2) 0.2500 0.232(13) Uani 0.50 2 d SP . . O94W O 0.0043(3) 0.3905(6) 0.1470(6) 0.046(3) Uani 0.25 1 d P . . O93W O -0.0086(8) 0.7400(11) 0.1042(10) 0.124(8) Uani 0.25 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 P1 0.0717(9) 0.0783(10) 0.0403(7) 0.0035(6) 0.0149(6) -0.0174(7) P2 0.0618(8) 0.0941(11) 0.0383(6) 0.0021(6) 0.0183(6) -0.0076(7) O1 0.0607(19) 0.0566(18) 0.0401(15) 0.0103(13) 0.0299(15) 0.0037(14) O2 0.073(2) 0.0561(19) 0.0475(17) 0.0085(14) 0.0376(16) 0.0071(15) O3 0.0497(17) 0.0489(17) 0.0326(13) 0.0061(12) 0.0177(13) 0.0009(12) O4 0.0563(18) 0.0587(18) 0.0336(14) 0.0036(13) 0.0192(14) -0.0036(14) O11 0.058(2) 0.120(3) 0.061(2) 0.025(2) 0.0239(18) -0.001(2) O12 0.096(3) 0.133(4) 0.0424(19) 0.015(2) 0.020(2) -0.019(3) O13 0.107(3) 0.097(3) 0.067(2) 0.002(2) 0.004(2) -0.040(3) O21 0.095(3) 0.117(3) 0.056(2) -0.014(2) 0.026(2) 0.006(2) O22 0.081(3) 0.093(3) 0.061(2) 0.0155(19) 0.034(2) 0.004(2) O23 0.079(3) 0.138(4) 0.056(2) -0.008(2) 0.028(2) -0.031(2) C1 0.062(3) 0.051(2) 0.044(2) 0.0037(19) 0.032(2) 0.006(2) C2 0.060(3) 0.050(3) 0.046(2) 0.0066(19) 0.028(2) 0.002(2) C3 0.062(3) 0.055(3) 0.036(2) 0.0138(19) 0.029(2) 0.006(2) C4 0.061(3) 0.071(3) 0.040(2) 0.013(2) 0.026(2) 0.002(2) C5 0.068(3) 0.097(4) 0.039(2) 0.016(3) 0.034(2) 0.013(3) C6 0.074(3) 0.075(3) 0.052(3) 0.019(2) 0.042(3) 0.023(3) C7 0.071(3) 0.060(3) 0.043(2) 0.018(2) 0.038(2) 0.015(2) C8 0.085(3) 0.057(3) 0.053(3) 0.009(2) 0.049(3) 0.011(2) C9 0.080(3) 0.051(3) 0.039(2) 0.0022(19) 0.038(2) 0.003(2) C10 0.079(3) 0.058(3) 0.048(2) -0.004(2) 0.040(2) 0.006(2) C11 0.079(3) 0.058(3) 0.039(2) -0.004(2) 0.033(2) 0.003(2) C12 0.073(3) 0.047(2) 0.033(2) -0.0007(18) 0.027(2) -0.003(2) C13 0.065(3) 0.037(2) 0.034(2) -0.0051(17) 0.026(2) -0.0060(19) C14 0.062(3) 0.043(2) 0.032(2) -0.0019(17) 0.0201(19) -0.0056(19) C15 0.062(3) 0.045(2) 0.034(2) -0.0019(17) 0.027(2) -0.0044(19) C16 0.065(3) 0.047(2) 0.032(2) 0.0010(17) 0.027(2) 0.000(2) C17 0.059(3) 0.047(2) 0.0316(19) 0.0058(17) 0.0250(19) -0.0023(19) C18 0.063(3) 0.046(2) 0.0276(18) -0.0017(16) 0.0241(19) -0.0076(19) C19 0.055(2) 0.045(2) 0.036(2) 0.0050(17) 0.029(2) 0.0006(18) C20 0.058(2) 0.043(2) 0.036(2) 0.0009(17) 0.029(2) -0.0019(18) C21 0.064(3) 0.041(2) 0.044(2) -0.0025(18) 0.032(2) 0.0016(19) C22 0.061(3) 0.050(2) 0.034(2) 0.0016(18) 0.024(2) 0.003(2) C23 0.063(3) 0.049(2) 0.046(2) -0.0008(19) 0.032(2) -0.001(2) C24 0.056(3) 0.048(2) 0.046(2) -0.0010(19) 0.028(2) -0.003(2) C25 0.049(2) 0.040(2) 0.037(2) -0.0026(17) 0.0186(19) -0.0038(18) C26 0.061(3) 0.056(3) 0.041(2) 0.019(2) 0.032(2) 0.008(2) C27 0.068(3) 0.045(2) 0.035(2) -0.0005(18) 0.030(2) 0.000(2) C28 0.059(3) 0.047(2) 0.034(2) 0.0033(17) 0.028(2) -0.0067(19) C30 0.063(3) 0.136(5) 0.055(3) 0.024(3) 0.031(3) 0.025(3) C31 0.081(5) 0.263(12) 0.070(4) -0.002(6) 0.021(4) 0.005(6) C32 0.046(4) 0.61(3) 0.241(13) 0.307(18) 0.046(6) 0.033(9) C33 0.083(7) 0.36(2) 0.212(13) -0.128(14) 0.013(7) 0.086(9) C40 0.074(3) 0.053(3) 0.061(3) -0.001(2) 0.040(3) 0.004(2) C41 0.080(4) 0.080(4) 0.089(4) 0.010(3) 0.042(3) 0.016(3) C42 0.106(5) 0.081(5) 0.167(8) -0.049(5) 0.065(6) 0.005(4) C43 0.153(7) 0.106(5) 0.131(6) 0.061(5) 0.099(6) 0.068(5) C50 0.056(3) 0.054(3) 0.035(2) -0.0002(18) 0.022(2) 0.001(2) C51 0.070(3) 0.060(3) 0.042(2) 0.005(2) 0.023(2) 0.016(2) C52 0.079(3) 0.063(3) 0.034(2) 0.010(2) 0.029(2) 0.010(2) C53 0.060(3) 0.082(4) 0.057(3) 0.010(3) 0.021(2) -0.002(3) C60 0.065(3) 0.070(3) 0.043(2) -0.004(2) 0.025(2) -0.002(2) C61 0.090(5) 0.156(7) 0.069(4) -0.012(4) 0.033(4) -0.046(5) C62 0.081(4) 0.107(5) 0.065(3) -0.028(3) 0.030(3) -0.013(3) C63 0.084(4) 0.096(5) 0.082(4) -0.013(4) 0.009(3) 0.012(4) C70 0.063(3) 0.053(2) 0.038(2) 0.0107(19) 0.030(2) 0.002(2) C71 0.067(3) 0.049(2) 0.039(2) 0.0045(18) 0.029(2) 0.000(2) C72 0.075(3) 0.064(3) 0.038(2) 0.000(2) 0.032(2) -0.004(2) C80 0.058(3) 0.072(3) 0.045(2) 0.001(2) 0.026(2) -0.005(2) C81 0.048(3) 0.070(3) 0.041(2) 0.002(2) 0.015(2) 0.002(2) C82 0.081(4) 0.070(3) 0.048(3) 0.004(2) 0.024(3) 0.010(3) O99M 0.099(3) 0.088(3) 0.070(2) -0.004(2) 0.034(2) 0.028(2) C99M 0.086(4) 0.059(3) 0.060(3) 0.007(2) 0.042(3) 0.005(3) O98M 0.135(6) 0.110(5) 0.110(5) -0.013(4) 0.053(5) 0.006(4) C98M 0.084(5) 0.345(17) 0.040(4) -0.005(7) 0.022(4) 0.050(8) O98X 0.123(16) 0.39(4) 0.006(6) -0.037(13) 0.018(8) -0.16(2) O97M 0.140(8) 0.119(7) 0.055(5) 0.022(4) 0.061(5) 0.047(5) C97M 0.233(14) 0.207(12) 0.29(2) -0.083(14) 0.186(15) -0.042(11) O97X 0.099(7) 0.093(7) 0.174(11) -0.042(7) 0.088(8) -0.029(5) O96M 0.131(5) 0.185(6) 0.108(4) -0.011(4) 0.040(4) 0.078(4) C96M 0.108(6) 0.133(7) 0.125(7) 0.006(6) 0.052(5) -0.017(5) O95M 0.099(6) 0.079(6) 0.116(7) 0.004(5) 0.056(6) 0.000(5) C95M 0.106(11) 0.136(13) 0.083(9) -0.003(9) 0.042(8) 0.010(9) O99W 0.057(8) 0.046(7) 0.104(11) 0.052(8) 0.059(8) 0.034(6) O98W 0.124(13) 0.078(10) 0.046(7) 0.020(7) 0.040(8) 0.034(9) O97W 0.101(14) 0.066(8) 0.073(12) -0.022(8) 0.036(9) -0.015(7) O96W 0.080(6) 0.139(8) 0.097(7) 0.032(6) 0.018(5) 0.020(6) O95W 0.126(16) 0.38(4) 0.084(12) 0.000 -0.011(10) 0.000 O94W 0.032(6) 0.030(6) 0.043(6) -0.002(5) -0.002(5) 0.020(5) O93W 0.20(2) 0.100(13) 0.070(11) 0.024(10) 0.072(13) 0.069(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O13 1.507(5) . ? P1 O11 1.514(4) . ? P1 O12 1.551(4) . ? P1 C72 1.788(5) . ? P2 O22 1.479(4) . ? P2 O23 1.516(4) . ? P2 O21 1.552(4) . ? P2 C82 1.775(5) . ? O1 C26 1.397(5) . ? O1 C70 1.435(5) . ? O2 C27 1.368(5) . ? O3 C28 1.397(5) . ? O3 C80 1.441(5) . ? O4 C25 1.373(5) . ? C1 C25 1.398(6) . ? C1 C24 1.402(6) . ? C1 C2 1.508(6) . ? C2 C3 1.522(6) . ? C3 C4 1.391(6) . ? C3 C26 1.397(6) . ? C4 C5 1.399(7) . ? C5 C6 1.384(8) . ? C5 C30 1.522(8) . ? C6 C7 1.408(7) . ? C7 C26 1.376(6) . ? C7 C8 1.508(7) . ? C8 C9 1.532(6) . ? C9 C27 1.399(6) . ? C9 C10 1.400(6) . ? C10 C11 1.386(6) . ? C11 C12 1.393(6) . ? C11 C40 1.534(7) . ? C12 C13 1.372(6) . ? C13 C27 1.410(5) . ? C13 C14 1.525(6) . ? C14 C15 1.508(5) . ? C15 C28 1.396(6) . ? C15 C16 1.402(6) . ? C16 C17 1.395(5) . ? C17 C18 1.400(6) . ? C17 C50 1.527(6) . ? C18 C19 1.389(5) . ? C19 C28 1.398(5) . ? C19 C20 1.519(6) . ? C20 C21 1.503(6) . ? C21 C25 1.390(6) . ? C21 C22 1.392(6) . ? C22 C23 1.390(6) . ? C23 C24 1.379(6) . ? C23 C60 1.542(6) . ? C30 C32 1.414(11) . ? C30 C31 1.445(9) . ? C30 C33 1.536(13) . ? C40 C42 1.476(8) . ? C40 C41 1.507(8) . ? C40 C43 1.570(8) . ? C50 C52 1.524(6) . ? C50 C53 1.532(7) . ? C50 C51 1.536(6) . ? C60 C61 1.518(8) . ? C60 C62 1.536(7) . ? C60 C63 1.526(8) . ? C70 C71 1.487(6) . ? C71 C72 1.551(6) . ? C80 C81 1.532(6) . ? C81 C82 1.516(7) . ? O99M C99M 1.418(6) . ? O98M C98M 1.585(14) . ? C98M O98X 1.33(4) . ? O97M O93W 1.61(2) 2 ? O97M C97M 1.661(18) . ? C97M O97X 1.332(15) . ? O96M C96M 1.352(10) . ? O95M C95M 1.439(17) 2 ? C95M O95M 1.439(17) 2 ? O99W O94W 1.159(16) . ? O97W O97W 1.11(3) 2 ? O97W O95W 1.66(4) . ? O96W O93W 1.39(2) . ? O95W O97W 1.66(4) 2 ? O93W O97M 1.61(2) 2 ? 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 O13 P1 O11 110.2(3) . . ? O13 P1 O12 115.9(3) . . ? O11 P1 O12 107.0(3) . . ? O13 P1 C72 111.0(3) . . ? O11 P1 C72 108.5(2) . . ? O12 P1 C72 103.8(2) . . ? O22 P2 O23 108.8(3) . . ? O22 P2 O21 111.6(2) . . ? O23 P2 O21 111.3(3) . . ? O22 P2 C82 111.8(2) . . ? O23 P2 C82 105.7(3) . . ? O21 P2 C82 107.6(2) . . ? C26 O1 C70 113.1(3) . . ? C28 O3 C80 113.4(3) . . ? C25 C1 C24 117.8(4) . . ? C25 C1 C2 121.2(4) . . ? C24 C1 C2 120.9(4) . . ? C1 C2 C3 109.8(3) . . ? C4 C3 C26 117.7(4) . . ? C4 C3 C2 119.1(4) . . ? C26 C3 C2 123.0(4) . . ? C3 C4 C5 122.1(5) . . ? C6 C5 C4 117.6(5) . . ? C6 C5 C30 121.4(5) . . ? C4 C5 C30 121.1(5) . . ? C5 C6 C7 122.4(4) . . ? C26 C7 C6 117.5(5) . . ? C26 C7 C8 121.7(4) . . ? C6 C7 C8 120.7(4) . . ? C7 C8 C9 111.3(4) . . ? C27 C9 C10 118.6(4) . . ? C27 C9 C8 120.8(4) . . ? C10 C9 C8 120.6(4) . . ? C11 C10 C9 123.3(4) . . ? C10 C11 C12 115.7(4) . . ? C10 C11 C40 122.1(4) . . ? C12 C11 C40 122.1(4) . . ? C13 C12 C11 123.9(4) . . ? C12 C13 C27 118.9(4) . . ? C12 C13 C14 121.3(4) . . ? C27 C13 C14 119.7(4) . . ? C15 C14 C13 110.1(3) . . ? C28 C15 C16 117.7(4) . . ? C28 C15 C14 122.5(4) . . ? C16 C15 C14 119.6(4) . . ? C17 C16 C15 122.5(4) . . ? C16 C17 C18 117.4(4) . . ? C16 C17 C50 122.6(4) . . ? C18 C17 C50 119.9(4) . . ? C19 C18 C17 122.3(4) . . ? C18 C19 C28 118.3(4) . . ? C18 C19 C20 119.1(4) . . ? C28 C19 C20 122.1(4) . . ? C21 C20 C19 112.9(3) . . ? C25 C21 C22 118.2(4) . . ? C25 C21 C20 121.8(4) . . ? C22 C21 C20 119.9(4) . . ? C23 C22 C21 123.0(4) . . ? C24 C23 C22 116.7(4) . . ? C24 C23 C60 122.4(4) . . ? C22 C23 C60 120.9(4) . . ? C23 C24 C1 123.1(4) . . ? O4 C25 C21 122.8(4) . . ? O4 C25 C1 116.1(3) . . ? C21 C25 C1 121.1(4) . . ? C7 C26 O1 118.8(4) . . ? C7 C26 C3 122.6(4) . . ? O1 C26 C3 118.6(4) . . ? O2 C27 C9 123.0(4) . . ? O2 C27 C13 117.5(4) . . ? C9 C27 C13 119.5(4) . . ? O3 C28 C15 119.5(3) . . ? O3 C28 C19 118.6(4) . . ? C15 C28 C19 121.8(4) . . ? C32 C30 C31 114.2(10) . . ? C32 C30 C5 109.0(5) . . ? C31 C30 C5 111.4(5) . . ? C32 C30 C33 103.6(11) . . ? C31 C30 C33 107.7(8) . . ? C5 C30 C33 110.6(7) . . ? C42 C40 C41 113.3(5) . . ? C42 C40 C11 109.9(5) . . ? C41 C40 C11 111.8(4) . . ? C42 C40 C43 107.6(6) . . ? C41 C40 C43 104.9(5) . . ? C11 C40 C43 109.1(4) . . ? C52 C50 C17 110.0(3) . . ? C52 C50 C53 109.2(4) . . ? C17 C50 C53 108.0(4) . . ? C52 C50 C51 108.6(4) . . ? C17 C50 C51 112.5(3) . . ? C53 C50 C51 108.5(4) . . ? C61 C60 C62 109.8(5) . . ? C61 C60 C63 108.4(6) . . ? C62 C60 C63 110.5(5) . . ? C61 C60 C23 111.9(4) . . ? C62 C60 C23 109.9(4) . . ? C63 C60 C23 106.2(4) . . ? O1 C70 C71 108.9(3) . . ? C70 C71 C72 110.1(3) . . ? C71 C72 P1 113.0(3) . . ? O3 C80 C81 107.7(3) . . ? C82 C81 C80 113.8(4) . . ? C81 C82 P2 114.4(4) . . ? O98X C98M O98M 127.7(11) . . ? O93W O97M C97M 131.3(10) 2 . ? O97X C97M O97M 125.3(14) . . ? O97W O97W O95W 70.5(7) 2 . ? O97W O95W O97W 38.9(14) . 2 ? O96W O93W O97M 121.4(13) . 2 ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 29.34 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 0.774 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.091