data_CCDC-778900 _audit_creation_method SHELXL-97 _publ_section_references ; CrystalClear, Rigaku Corp., (1999) Altomare, A., M. Burla, M. Camalli, G. Cascarano, C. Giacovazzo A. Guagliardi, A. Moliterni, G. Polidori & R. Spagna. (1999) J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C123 H132 O27' _chemical_formula_weight 2042.29 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.374(4) _cell_length_b 11.9732(17) _cell_length_c 22.305(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.010(4) _cell_angle_gamma 90.00 _cell_volume 5328.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details ; Shape and scale corrections using equivalent reflections. Shape function based on spherical harmonics. Highest even and odd order for spherical harmonics: 4 and 3 Laue group: 2/m Friedel opposites are equivalent. ; _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7115 _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method 'phi and omega rotations' _diffrn_reflns_number 27444 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9345 _reflns_number_gt 5768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 1999)' _computing_data_reduction 'CrystalClear (Rigaku, 1999)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1664P)^2^+3.5471P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9345 _refine_ls_number_parameters 688 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.2902 _refine_ls_wR_factor_gt 0.2323 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.28693(18) 0.3251(3) 0.31539(18) 0.0375(9) Uani 1 1 d . . . H1A H 0.3261 0.2772 0.3289 0.050 Uiso 1 1 calc R . . H1B H 0.2495 0.2821 0.2872 0.050 Uiso 1 1 calc R . . C2 C 0.29944(17) 0.4239(3) 0.27867(17) 0.0359(8) Uani 1 1 d . . . C3 C 0.36411(17) 0.4696(3) 0.29874(18) 0.0381(9) Uani 1 1 d . . . H3 H 0.3983 0.4347 0.3317 0.051 Uiso 1 1 calc R . . C4 C 0.37869(16) 0.5642(3) 0.27134(18) 0.0366(9) Uani 1 1 d . . . C5 C 0.32790(17) 0.6195(3) 0.22239(18) 0.0361(8) Uani 1 1 d . . . C6 C 0.26460(17) 0.5718(3) 0.20039(18) 0.0378(9) Uani 1 1 d . . . H6 H 0.2311 0.6058 0.1663 0.050 Uiso 1 1 calc R . . C7 C 0.24878(17) 0.4757(3) 0.22671(17) 0.0353(8) Uani 1 1 d . . . C8 C 0.17698(17) 0.4332(3) 0.19905(18) 0.0390(9) Uani 1 1 d . . . H8A H 0.1609 0.4391 0.1526 0.052 Uiso 1 1 calc R . . H8B H 0.1762 0.3549 0.2099 0.052 Uiso 1 1 calc R . . C9 C 0.13033(16) 0.4979(3) 0.22413(18) 0.0373(9) Uani 1 1 d . . . C10 C 0.09996(17) 0.5942(3) 0.19138(18) 0.0401(9) Uani 1 1 d . . . H10 H 0.1066 0.6134 0.1537 0.053 Uiso 1 1 calc R . . C11 C 0.06001(17) 0.6625(3) 0.21327(18) 0.0399(9) Uani 1 1 d . . . C12 C 0.05215(17) 0.6351(3) 0.27126(19) 0.0386(9) Uani 1 1 d . . . C13 C 0.08045(17) 0.5378(3) 0.30262(19) 0.0408(9) Uani 1 1 d . . . H13 H 0.0740 0.5193 0.3405 0.054 Uiso 1 1 calc R . . C14 C 0.11842(17) 0.4660(3) 0.27982(18) 0.0373(9) Uani 1 1 d . . . C15 C 0.14419(18) 0.3575(3) 0.31580(19) 0.0406(9) Uani 1 1 d . . . H15A H 0.1092 0.3252 0.3285 0.054 Uiso 1 1 calc R . . H15B H 0.1537 0.3053 0.2870 0.054 Uiso 1 1 calc R . . C16 C 0.20659(18) 0.3721(3) 0.37490(19) 0.0371(8) Uani 1 1 d . . . C17 C 0.19901(19) 0.4013(3) 0.4325(2) 0.0435(9) Uani 1 1 d . . . H17 H 0.1559 0.4065 0.4333 0.058 Uiso 1 1 calc R . . C18 C 0.25241(19) 0.4228(3) 0.4881(2) 0.0431(9) Uani 1 1 d . . . C19 C 0.31702(19) 0.4205(3) 0.48607(19) 0.0411(9) Uani 1 1 d . . . C20 C 0.32569(19) 0.3862(3) 0.43056(19) 0.0418(9) Uani 1 1 d . . . H20 H 0.3690 0.3793 0.4305 0.056 Uiso 1 1 calc R . . C21 C 0.27173(18) 0.3614(3) 0.37422(18) 0.0386(9) Uani 1 1 d . . . C22 C 0.32251(18) 0.9870(4) 0.54232(18) 0.0435(9) Uani 1 1 d . . . H22A H 0.3339 0.9789 0.5883 0.058 Uiso 1 1 calc R . . H22B H 0.3243 1.0660 0.5333 0.058 Uiso 1 1 calc R . . C23 C 0.37529(17) 0.9258(4) 0.52278(18) 0.0404(9) Uani 1 1 d . . . C24 C 0.40583(18) 0.8316(4) 0.55683(19) 0.0431(10) Uani 1 1 d . . . H24 H 0.3940 0.8082 0.5911 0.057 Uiso 1 1 calc R . . C25 C 0.45364(18) 0.7707(4) 0.54164(19) 0.0447(10) Uani 1 1 d . . . C26 C 0.47255(18) 0.8051(3) 0.49111(18) 0.0417(9) Uani 1 1 d . . . C27 C 0.44389(17) 0.9015(4) 0.45737(18) 0.0420(9) Uani 1 1 d . . . H27 H 0.4573 0.9258 0.4243 0.056 Uiso 1 1 calc R . . C28 C 0.39505(17) 0.9631(3) 0.47213(18) 0.0396(9) Uani 1 1 d . . . C29 C 0.36791(18) 1.0669(3) 0.43248(18) 0.0396(9) Uani 1 1 d . . . H29A H 0.4035 1.1008 0.4214 0.053 Uiso 1 1 calc R . . H29B H 0.3547 1.1200 0.4586 0.053 Uiso 1 1 calc R . . C30 C 0.30851(17) 1.0454(3) 0.37125(17) 0.0368(8) Uani 1 1 d . . . C31 C 0.32072(17) 1.0047(3) 0.31738(18) 0.0393(9) Uani 1 1 d . . . H31 H 0.3647 0.9902 0.3211 0.052 Uiso 1 1 calc R . . C32 C 0.27023(17) 0.9854(3) 0.25941(18) 0.0355(8) Uani 1 1 d . . . C33 C 0.20358(17) 1.0117(3) 0.25259(18) 0.0356(8) Uani 1 1 d . . . C34 C 0.19139(17) 1.0507(3) 0.30535(18) 0.0354(8) Uani 1 1 d . . . H34 H 0.1475 1.0672 0.3012 0.047 Uiso 1 1 calc R . . C35 C 0.24250(17) 1.0664(3) 0.36514(17) 0.0332(8) Uani 1 1 d . . . C36 C 0.22247(19) 1.0997(3) 0.42193(18) 0.0391(9) Uani 1 1 d . . . H36A H 0.2590 1.1404 0.4531 0.052 Uiso 1 1 calc R . . H36B H 0.1838 1.1487 0.4071 0.052 Uiso 1 1 calc R . . C37 C 0.20582(17) 0.9979(3) 0.45381(17) 0.0369(8) Uani 1 1 d . . . C38 C 0.14155(18) 0.9523(3) 0.42510(18) 0.0385(9) Uani 1 1 d . . . H38 H 0.1117 0.9862 0.3885 0.051 Uiso 1 1 calc R . . C39 C 0.12100(17) 0.8579(3) 0.44965(17) 0.0385(9) Uani 1 1 d . . . C40 C 0.16604(18) 0.8081(3) 0.50585(18) 0.0406(9) Uani 1 1 d . . . C41 C 0.23014(18) 0.8514(3) 0.53355(17) 0.0386(9) Uani 1 1 d . . . H41 H 0.2601 0.8170 0.5699 0.051 Uiso 1 1 calc R . . C42 C 0.25112(18) 0.9457(4) 0.50840(17) 0.0399(9) Uani 1 1 d . . . C43 C 0.47835(19) 0.5869(4) 0.2488(2) 0.0486(10) Uani 1 1 d . . . H43A H 0.4516 0.6145 0.2065 0.065 Uiso 1 1 calc R . . H43B H 0.4861 0.5076 0.2456 0.065 Uiso 1 1 calc R . . C44 C 0.54359(19) 0.6480(4) 0.2743(2) 0.0507(11) Uani 1 1 d . . . H44 H 0.5708 0.6379 0.3171 0.067 Uiso 1 1 calc R . . C45 C 0.5638(3) 0.7156(5) 0.2385(3) 0.0732(15) Uani 1 1 d . . . H45A H 0.5373 0.7267 0.1957 0.097 Uiso 1 1 calc R . . H45B H 0.6048 0.7522 0.2561 0.097 Uiso 1 1 calc R . . C46 C 0.36938(19) 0.8071(3) 0.2383(2) 0.0422(9) Uani 1 1 d . . . H46A H 0.4177 0.8046 0.2500 0.056 Uiso 1 1 calc R . . H46B H 0.3592 0.7989 0.2770 0.056 Uiso 1 1 calc R . . C47 C 0.34297(18) 0.9159(3) 0.2067(2) 0.0430(9) Uani 1 1 d . . . H47A H 0.3734 0.9748 0.2295 0.057 Uiso 1 1 calc R . . H47B H 0.3427 0.9142 0.1632 0.057 Uiso 1 1 calc R . . C48 C 0.0166(2) 0.7718(4) 0.1166(2) 0.0511(11) Uani 1 1 d . . . H48A H 0.0591 0.7635 0.1106 0.068 Uiso 1 1 calc R . . H48B H 0.0004 0.8470 0.1038 0.068 Uiso 1 1 calc R . . C49 C -0.0316(2) 0.6917(4) 0.0755(2) 0.0551(12) Uani 1 1 d . . . H49 H -0.0701 0.6772 0.0844 0.073 Uiso 1 1 calc R . . C50 C -0.0240(3) 0.6386(5) 0.0266(3) 0.0810(17) Uani 1 1 d . . . H50A H 0.0139 0.6511 0.0164 0.108 Uiso 1 1 calc R . . H50B H -0.0567 0.5887 0.0024 0.108 Uiso 1 1 calc R . . C51 C 0.03188(18) 0.8151(3) 0.30879(19) 0.0415(9) Uani 1 1 d . . . H51A H 0.0077 0.8598 0.2714 0.055 Uiso 1 1 calc R . . H51B H 0.0796 0.8247 0.3184 0.055 Uiso 1 1 calc R . . C52 C 0.01382(17) 0.8507(4) 0.36541(19) 0.0427(9) Uani 1 1 d . . . H52A H 0.0136 0.9317 0.3673 0.057 Uiso 1 1 calc R . . H52B H -0.0311 0.8248 0.3592 0.057 Uiso 1 1 calc R . . C53 C 0.2084(3) 0.3846(5) 0.5703(3) 0.0716(14) Uani 1 1 d D . . H53A H 0.1695 0.3545 0.5365 0.095 Uiso 1 1 calc R . . H53B H 0.1933 0.4259 0.6000 0.095 Uiso 1 1 calc R . . C54 C 0.2531(6) 0.2945(9) 0.6038(5) 0.175(5) Uani 1 1 d D . . H54 H 0.2920 0.3202 0.6356 0.233 Uiso 1 1 calc R . . C55 C 0.2508(10) 0.1890(9) 0.5993(7) 0.263(11) Uani 1 1 d D . . H55A H 0.2140 0.1545 0.5691 0.350 Uiso 1 1 calc R . . H55B H 0.2858 0.1461 0.6263 0.350 Uiso 1 1 calc R . . C56 C 0.4171(2) 0.5245(5) 0.5293(3) 0.0691(14) Uani 1 1 d . . . H56A H 0.3952 0.5711 0.4921 0.092 Uiso 1 1 calc R . . H56B H 0.4519 0.4814 0.5215 0.092 Uiso 1 1 calc R . . C57 C 0.4465(2) 0.5944(4) 0.5872(3) 0.0653(14) Uani 1 1 d . . . H57A H 0.4107 0.6276 0.5983 0.087 Uiso 1 1 calc R . . H57B H 0.4728 0.5477 0.6228 0.087 Uiso 1 1 calc R . . C58 C 0.5356(2) 0.7741(4) 0.4226(2) 0.0555(11) Uani 1 1 d . . . H58A H 0.4967 0.7643 0.3845 0.083 Uiso 1 1 calc R . . H58B H 0.5713 0.7280 0.4200 0.083 Uiso 1 1 calc R . . H58C H 0.5492 0.8510 0.4262 0.083 Uiso 1 1 calc R . . C59 C 0.0920(2) 1.0405(4) 0.1833(2) 0.0560(12) Uani 1 1 d . . . H59A H 0.0719 0.9984 0.2083 0.084 Uiso 1 1 calc R . . H59B H 0.0646 1.0351 0.1386 0.084 Uiso 1 1 calc R . . H59C H 0.0958 1.1174 0.1964 0.084 Uiso 1 1 calc R . . C60 C 0.1839(2) 0.6681(4) 0.5863(2) 0.0523(11) Uani 1 1 d . . . H60A H 0.2244 0.6448 0.5807 0.078 Uiso 1 1 calc R . . H60B H 0.1620 0.6042 0.5959 0.078 Uiso 1 1 calc R . . H60C H 0.1945 0.7205 0.6211 0.078 Uiso 1 1 calc R . . O1 O 0.44418(11) 0.6061(2) 0.29328(13) 0.0433(7) Uani 1 1 d . . . O2 O 0.33863(12) 0.7169(2) 0.19400(12) 0.0400(6) Uani 1 1 d . . . O3 O 0.27740(12) 0.9431(3) 0.20463(13) 0.0464(7) Uani 1 1 d . . . O4 O 0.02671(13) 0.7568(2) 0.18288(13) 0.0487(7) Uani 1 1 d . . . O5 O 0.01362(12) 0.6983(2) 0.29660(14) 0.0448(7) Uani 1 1 d . . . O6 O 0.05910(12) 0.8084(3) 0.42474(13) 0.0459(7) Uani 1 1 d . . . O7 O 0.24439(15) 0.4551(3) 0.54408(15) 0.0559(8) Uani 1 1 d . . . O8 O 0.36911(14) 0.4511(3) 0.54077(14) 0.0571(8) Uani 1 1 d . . . O9 O 0.48731(13) 0.6795(3) 0.57799(14) 0.0515(8) Uani 1 1 d . . . O10 O 0.51998(13) 0.7425(3) 0.47829(13) 0.0484(7) Uani 1 1 d . . . O11 O 0.15676(12) 0.9972(2) 0.19302(12) 0.0430(7) Uani 1 1 d . . . O12 O 0.14026(13) 0.7198(3) 0.52848(13) 0.0487(7) Uani 1 1 d . . . C61 C 0.2531(4) 0.7105(7) 0.3684(4) 0.154(3) Uani 0.50 1 d P A 1 H61A H 0.2309 0.7565 0.3316 0.231 Uiso 0.50 1 calc PR A 1 H61B H 0.2430 0.7375 0.4045 0.231 Uiso 0.50 1 calc PR A 1 H61C H 0.2377 0.6349 0.3592 0.231 Uiso 0.50 1 calc PR A 1 O13 O 0.3208(3) 0.7145(7) 0.3824(4) 0.140(3) Uani 0.50 1 d P A 1 H13a H 0.3317 0.6646 0.3629 0.210 Uiso 0.50 1 calc PR A 1 C61' C 0.3208(3) 0.7145(7) 0.3824(4) 0.140(3) Uani 0.50 1 d P B 2 H61X H 0.3429 0.6685 0.4192 0.210 Uiso 0.50 1 calc PR B 2 H61Y H 0.3361 0.7901 0.3916 0.210 Uiso 0.50 1 calc PR B 2 H61Z H 0.3308 0.6875 0.3463 0.210 Uiso 0.50 1 calc PR B 2 O13' O 0.2531(4) 0.7105(7) 0.3684(4) 0.154(3) Uani 0.50 1 d P B 2 H13' H 0.2370 0.6590 0.3434 0.231 Uiso 0.50 1 calc PR B 2 C62 C 0.0205(7) 0.5277(13) 0.4924(6) 0.095(4) Uani 0.50 1 d P . . H62A H -0.0206 0.5694 0.4768 0.142 Uiso 0.50 1 calc PR . . H62B H 0.0485 0.5567 0.5333 0.142 Uiso 0.50 1 calc PR . . H62C H 0.0107 0.4505 0.4969 0.142 Uiso 0.50 1 calc PR . . O14 O 0.0522(4) 0.5366(7) 0.4506(4) 0.079(2) Uani 0.50 1 d P . . H14 H 0.0831 0.5812 0.4643 0.118 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(2) 0.030(2) 0.045(2) 0.0038(17) 0.0215(16) 0.0056(15) C2 0.0356(18) 0.036(2) 0.039(2) -0.0017(16) 0.0172(16) 0.0045(14) C3 0.0364(19) 0.041(2) 0.039(2) 0.0024(17) 0.0165(16) 0.0033(15) C4 0.0275(17) 0.042(2) 0.041(2) -0.0056(17) 0.0132(15) -0.0018(14) C5 0.0404(19) 0.033(2) 0.040(2) -0.0005(17) 0.0209(16) -0.0001(15) C6 0.0356(19) 0.042(2) 0.0360(19) 0.0010(17) 0.0130(15) 0.0012(15) C7 0.0407(19) 0.036(2) 0.0330(18) -0.0053(16) 0.0180(15) -0.0010(15) C8 0.040(2) 0.038(2) 0.040(2) -0.0076(17) 0.0155(16) -0.0049(15) C9 0.0300(17) 0.039(2) 0.042(2) -0.0058(17) 0.0117(15) -0.0052(14) C10 0.0343(18) 0.047(2) 0.037(2) 0.0002(18) 0.0100(15) -0.0031(16) C11 0.0348(19) 0.037(2) 0.045(2) -0.0003(18) 0.0108(16) -0.0024(15) C12 0.0322(18) 0.036(2) 0.049(2) -0.0050(18) 0.0166(16) -0.0044(15) C13 0.0338(19) 0.043(2) 0.048(2) 0.0009(18) 0.0177(17) -0.0053(15) C14 0.0318(18) 0.035(2) 0.044(2) -0.0007(17) 0.0124(16) -0.0049(14) C15 0.041(2) 0.037(2) 0.051(2) 0.0002(18) 0.0259(18) -0.0020(15) C16 0.045(2) 0.024(2) 0.048(2) 0.0059(16) 0.0234(17) 0.0005(14) C17 0.045(2) 0.036(2) 0.054(2) 0.0052(19) 0.0236(19) 0.0028(16) C18 0.051(2) 0.034(2) 0.052(2) -0.0022(18) 0.0275(19) 0.0006(16) C19 0.047(2) 0.030(2) 0.045(2) 0.0022(17) 0.0160(17) -0.0055(16) C20 0.042(2) 0.040(2) 0.049(2) 0.0025(18) 0.0219(18) 0.0002(16) C21 0.046(2) 0.029(2) 0.044(2) 0.0061(17) 0.0197(17) 0.0034(15) C22 0.045(2) 0.052(3) 0.034(2) -0.0028(18) 0.0156(16) -0.0048(17) C23 0.0352(19) 0.050(3) 0.0335(19) -0.0068(18) 0.0087(15) -0.0101(16) C24 0.038(2) 0.049(3) 0.038(2) 0.0024(18) 0.0083(16) -0.0093(17) C25 0.036(2) 0.048(3) 0.044(2) -0.0005(19) 0.0060(17) -0.0082(17) C26 0.0361(19) 0.043(2) 0.040(2) -0.0051(18) 0.0068(16) -0.0058(16) C27 0.0335(19) 0.052(3) 0.038(2) -0.0069(18) 0.0097(16) -0.0086(16) C28 0.0347(19) 0.043(2) 0.037(2) -0.0073(17) 0.0071(16) -0.0117(15) C29 0.0395(19) 0.038(2) 0.040(2) -0.0030(17) 0.0115(16) -0.0099(15) C30 0.0397(19) 0.034(2) 0.037(2) -0.0011(16) 0.0135(16) -0.0026(15) C31 0.0345(18) 0.042(2) 0.044(2) 0.0053(18) 0.0162(16) 0.0030(15) C32 0.0400(19) 0.035(2) 0.0369(19) -0.0021(16) 0.0205(16) 0.0018(15) C33 0.0381(18) 0.031(2) 0.038(2) 0.0015(16) 0.0133(15) 0.0030(14) C34 0.0359(18) 0.029(2) 0.045(2) 0.0018(16) 0.0193(16) 0.0034(14) C35 0.0407(19) 0.0245(19) 0.0370(19) 0.0019(15) 0.0171(16) -0.0003(14) C36 0.046(2) 0.034(2) 0.039(2) -0.0033(17) 0.0163(16) 0.0006(16) C37 0.0422(19) 0.038(2) 0.0349(19) -0.0005(16) 0.0188(16) -0.0003(15) C38 0.0394(19) 0.047(2) 0.0322(19) 0.0053(17) 0.0162(16) 0.0014(16) C39 0.0374(19) 0.047(2) 0.0344(19) 0.0017(17) 0.0167(16) 0.0019(16) C40 0.043(2) 0.045(2) 0.038(2) 0.0061(18) 0.0198(17) 0.0004(16) C41 0.0395(19) 0.046(2) 0.0325(19) 0.0040(17) 0.0151(15) 0.0027(16) C42 0.042(2) 0.050(3) 0.0292(18) -0.0054(17) 0.0157(16) 0.0012(17) C43 0.039(2) 0.055(3) 0.055(2) -0.001(2) 0.0221(18) 0.0011(17) C44 0.043(2) 0.054(3) 0.062(3) 0.009(2) 0.027(2) 0.0052(18) C45 0.061(3) 0.075(4) 0.094(4) 0.024(3) 0.040(3) 0.003(2) C46 0.043(2) 0.034(2) 0.053(2) -0.0032(18) 0.0212(18) -0.0001(15) C47 0.041(2) 0.041(2) 0.054(2) -0.0057(19) 0.0258(18) -0.0013(16) C48 0.048(2) 0.057(3) 0.051(3) 0.014(2) 0.0216(19) 0.0091(19) C49 0.054(2) 0.061(3) 0.052(3) 0.006(2) 0.020(2) -0.004(2) C50 0.088(4) 0.089(5) 0.068(3) -0.001(3) 0.031(3) -0.012(3) C51 0.0361(19) 0.041(2) 0.046(2) 0.0007(18) 0.0129(16) -0.0005(15) C52 0.0312(18) 0.046(2) 0.048(2) 0.0012(18) 0.0107(16) 0.0033(15) C53 0.108(4) 0.064(4) 0.056(3) 0.004(3) 0.046(3) -0.001(3) C54 0.298(15) 0.129(9) 0.161(9) 0.031(7) 0.157(11) 0.069(9) C55 0.56(3) 0.107(9) 0.302(18) 0.036(10) 0.37(2) 0.069(13) C56 0.060(3) 0.071(4) 0.072(3) 0.005(3) 0.019(2) -0.007(2) C57 0.056(3) 0.053(3) 0.075(3) 0.016(3) 0.009(2) -0.007(2) C58 0.055(2) 0.062(3) 0.050(3) -0.003(2) 0.020(2) 0.005(2) C59 0.040(2) 0.074(3) 0.050(2) 0.001(2) 0.0113(18) 0.010(2) C60 0.056(2) 0.049(3) 0.052(2) 0.007(2) 0.020(2) 0.0025(19) O1 0.0317(13) 0.0506(18) 0.0497(15) 0.0020(13) 0.0173(11) 0.0000(11) O2 0.0413(14) 0.0373(16) 0.0434(15) 0.0026(12) 0.0176(11) -0.0011(11) O3 0.0397(14) 0.060(2) 0.0412(15) -0.0017(13) 0.0170(12) 0.0093(12) O4 0.0489(16) 0.0492(18) 0.0482(16) 0.0120(14) 0.0176(13) 0.0102(12) O5 0.0393(14) 0.0403(17) 0.0607(17) 0.0007(13) 0.0253(13) -0.0003(11) O6 0.0340(13) 0.0578(19) 0.0443(15) 0.0098(13) 0.0119(11) -0.0048(11) O7 0.0695(19) 0.054(2) 0.0573(18) -0.0090(15) 0.0384(16) -0.0085(14) O8 0.0517(17) 0.070(2) 0.0489(17) 0.0012(15) 0.0177(14) -0.0166(14) O9 0.0480(16) 0.0484(19) 0.0526(17) 0.0127(14) 0.0112(13) -0.0032(13) O10 0.0406(14) 0.0557(19) 0.0492(16) -0.0018(14) 0.0166(12) 0.0009(12) O11 0.0351(13) 0.0574(19) 0.0345(14) -0.0043(12) 0.0101(11) 0.0112(11) O12 0.0431(15) 0.057(2) 0.0449(16) 0.0152(14) 0.0147(12) -0.0045(12) C61 0.113(6) 0.127(7) 0.214(9) -0.040(6) 0.050(5) -0.022(4) O13 0.100(5) 0.144(7) 0.162(7) -0.017(5) 0.030(4) -0.021(4) C61' 0.100(5) 0.144(7) 0.162(7) -0.017(5) 0.030(4) -0.021(4) O13' 0.113(6) 0.127(7) 0.214(9) -0.040(6) 0.050(5) -0.022(4) C62 0.105(10) 0.128(13) 0.060(7) -0.015(7) 0.040(6) -0.032(8) O14 0.078(5) 0.086(6) 0.076(5) -0.019(4) 0.033(4) -0.025(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.516(5) . ? C1 C21 1.524(5) . ? C2 C3 1.403(5) . ? C2 C7 1.415(5) . ? C3 C4 1.375(5) . ? C4 C5 1.400(5) . ? C4 O1 1.400(4) . ? C5 O2 1.385(5) . ? C5 C6 1.386(5) . ? C6 C7 1.387(5) . ? C7 C8 1.522(5) . ? C8 C9 1.519(5) . ? C9 C10 1.394(6) . ? C9 C14 1.407(5) . ? C10 C11 1.391(5) . ? C11 O4 1.377(5) . ? C11 C12 1.401(5) . ? C12 O5 1.380(5) . ? C12 C13 1.382(6) . ? C13 C14 1.397(5) . ? C14 C15 1.523(5) . ? C15 C16 1.512(5) . ? C16 C17 1.396(6) . ? C16 C21 1.403(5) . ? C17 C18 1.375(6) . ? C18 O7 1.375(5) . ? C18 C19 1.398(5) . ? C19 O8 1.374(5) . ? C19 C20 1.379(6) . ? C20 C21 1.399(5) . ? C22 C42 1.523(5) . ? C22 C23 1.534(6) . ? C23 C24 1.386(6) . ? C23 C28 1.413(5) . ? C24 C25 1.393(6) . ? C25 C26 1.389(6) . ? C25 O9 1.396(5) . ? C26 O10 1.371(5) . ? C26 C27 1.394(6) . ? C27 C28 1.410(5) . ? C28 C29 1.515(6) . ? C29 C30 1.516(5) . ? C30 C35 1.391(5) . ? C30 C31 1.405(5) . ? C31 C32 1.374(5) . ? C32 O3 1.381(4) . ? C32 C33 1.413(5) . ? C33 O11 1.358(4) . ? C33 C34 1.375(5) . ? C34 C35 1.401(5) . ? C35 C36 1.528(5) . ? C36 C37 1.515(5) . ? C37 C38 1.402(5) . ? C37 C42 1.402(5) . ? C38 C39 1.394(5) . ? C39 O6 1.372(4) . ? C39 C40 1.410(5) . ? C40 O12 1.369(5) . ? C40 C41 1.386(5) . ? C41 C42 1.404(6) . ? C43 O1 1.445(5) . ? C43 C44 1.495(6) . ? C44 C45 1.314(6) . ? C46 O2 1.451(5) . ? C46 C47 1.492(6) . ? C47 O3 1.423(4) . ? C48 O4 1.425(5) . ? C48 C49 1.464(6) . ? C49 C50 1.321(7) . ? C51 O5 1.451(5) . ? C51 C52 1.509(6) . ? C52 O6 1.423(5) . ? C53 O7 1.403(6) . ? C53 C54 1.457(8) . ? C54 C55 1.267(8) . ? C56 O8 1.442(6) . ? C56 C57 1.477(8) . ? C57 O9 1.403(5) . ? C58 O10 1.449(5) . ? C59 O11 1.420(5) . ? C60 O12 1.434(5) . ? C61 O13 1.367(8) . ? C62 O14 1.340(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 112.1(3) . . ? C3 C2 C7 117.9(4) . . ? C3 C2 C1 118.5(3) . . ? C7 C2 C1 123.6(3) . . ? C4 C3 C2 122.3(3) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 O1 119.8(3) . . ? C5 C4 O1 120.1(3) . . ? O2 C5 C6 119.1(3) . . ? O2 C5 C4 123.1(3) . . ? C6 C5 C4 117.8(4) . . ? C5 C6 C7 123.2(3) . . ? C6 C7 C2 118.7(3) . . ? C6 C7 C8 118.0(3) . . ? C2 C7 C8 123.3(3) . . ? C9 C8 C7 112.3(3) . . ? C10 C9 C14 119.3(3) . . ? C10 C9 C8 118.2(3) . . ? C14 C9 C8 122.5(3) . . ? C11 C10 C9 122.1(4) . . ? O4 C11 C10 125.7(4) . . ? O4 C11 C12 115.7(3) . . ? C10 C11 C12 118.6(4) . . ? O5 C12 C13 118.2(4) . . ? O5 C12 C11 122.5(3) . . ? C13 C12 C11 119.3(3) . . ? C12 C13 C14 122.7(4) . . ? C13 C14 C9 117.8(4) . . ? C13 C14 C15 118.7(3) . . ? C9 C14 C15 123.4(3) . . ? C16 C15 C14 113.6(3) . . ? C17 C16 C21 118.4(3) . . ? C17 C16 C15 118.3(3) . . ? C21 C16 C15 123.3(4) . . ? C18 C17 C16 122.9(3) . . ? C17 C18 O7 122.5(3) . . ? C17 C18 C19 118.5(4) . . ? O7 C18 C19 118.8(4) . . ? O8 C19 C20 123.4(3) . . ? O8 C19 C18 117.4(4) . . ? C20 C19 C18 119.2(4) . . ? C19 C20 C21 122.5(3) . . ? C20 C21 C16 118.2(4) . . ? C20 C21 C1 118.2(3) . . ? C16 C21 C1 123.6(3) . . ? C42 C22 C23 114.3(3) . . ? C24 C23 C28 118.6(4) . . ? C24 C23 C22 118.9(4) . . ? C28 C23 C22 122.5(4) . . ? C23 C24 C25 122.4(4) . . ? C26 C25 C24 119.6(4) . . ? C26 C25 O9 117.6(4) . . ? C24 C25 O9 122.6(4) . . ? O10 C26 C25 117.3(4) . . ? O10 C26 C27 123.7(4) . . ? C25 C26 C27 119.0(4) . . ? C26 C27 C28 121.7(4) . . ? C27 C28 C23 118.7(4) . . ? C27 C28 C29 116.9(4) . . ? C23 C28 C29 124.3(4) . . ? C28 C29 C30 114.1(3) . . ? C35 C30 C31 118.2(3) . . ? C35 C30 C29 123.4(3) . . ? C31 C30 C29 118.5(3) . . ? C32 C31 C30 122.6(3) . . ? C31 C32 O3 126.5(3) . . ? C31 C32 C33 119.0(3) . . ? O3 C32 C33 114.4(3) . . ? O11 C33 C34 125.6(3) . . ? O11 C33 C32 115.9(3) . . ? C34 C33 C32 118.5(3) . . ? C33 C34 C35 122.6(3) . . ? C30 C35 C34 119.1(3) . . ? C30 C35 C36 122.8(3) . . ? C34 C35 C36 118.0(3) . . ? C37 C36 C35 111.3(3) . . ? C38 C37 C42 118.8(4) . . ? C38 C37 C36 117.1(3) . . ? C42 C37 C36 124.1(3) . . ? C39 C38 C37 122.1(3) . . ? O6 C39 C38 125.8(3) . . ? O6 C39 C40 115.4(3) . . ? C38 C39 C40 118.8(3) . . ? O12 C40 C41 126.1(3) . . ? O12 C40 C39 114.7(3) . . ? C41 C40 C39 119.3(4) . . ? C40 C41 C42 121.9(3) . . ? C37 C42 C41 119.1(3) . . ? C37 C42 C22 122.9(4) . . ? C41 C42 C22 118.0(3) . . ? O1 C43 C44 107.0(3) . . ? C45 C44 C43 122.4(5) . . ? O2 C46 C47 109.1(3) . . ? O3 C47 C46 114.7(3) . . ? O4 C48 C49 112.3(4) . . ? C50 C49 C48 124.5(5) . . ? O5 C51 C52 107.3(3) . . ? O6 C52 C51 112.6(3) . . ? O7 C53 C54 107.6(6) . . ? C55 C54 C53 134.2(15) . . ? O8 C56 C57 107.2(4) . . ? O9 C57 C56 112.0(4) . . ? C4 O1 C43 113.0(3) . . ? C5 O2 C46 115.1(3) . . ? C32 O3 C47 118.3(3) . . ? C11 O4 C48 118.3(3) . . ? C12 O5 C51 116.4(3) . . ? C39 O6 C52 117.3(3) . . ? C18 O7 C53 118.4(4) . . ? C19 O8 C56 114.0(3) . . ? C25 O9 C57 115.7(3) . . ? C26 O10 C58 116.8(3) . . ? C33 O11 C59 116.0(3) . . ? C40 O12 C60 116.6(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14 O12 0.82 2.25 3.006(8) 154.4 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.688 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.078