data_CCDC-778896 _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 'C54 H54 O13.25' _chemical_formula_weight 914.97 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 22.2761(15) _cell_length_b 11.2688(6) _cell_length_c 20.5348(14) _cell_angle_alpha 90.00 _cell_angle_beta 113.8120(10) _cell_angle_gamma 90.00 _cell_volume 4715.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type 'none' _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 35655 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8293 _reflns_number_gt 7046 _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^)+(0.0675P)^2^+1.7588P] 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 SHELXL _refine_ls_extinction_coef 0.0029(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8293 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.42418(9) 0.52589(16) 0.19483(9) 0.0335(4) Uani 1 1 d . . . H1a H 0.4357 0.4679 0.1669 0.045 Uiso 1 1 calc R . . H1b H 0.4546 0.5916 0.2042 0.045 Uiso 1 1 calc R . . C2 C 0.43352(8) 0.46973(16) 0.26514(9) 0.0315(4) Uani 1 1 d . . . C3 C 0.41947(8) 0.34919(16) 0.26467(10) 0.0346(4) Uani 1 1 d . . . H3 H 0.4060 0.3079 0.2219 0.046 Uiso 1 1 calc R . . C4 C 0.42475(9) 0.28853(16) 0.32514(10) 0.0350(4) Uani 1 1 d . . . C5 C 0.44048(8) 0.35172(16) 0.38881(10) 0.0332(4) Uani 1 1 d . . . C6 C 0.45651(8) 0.47038(16) 0.38983(10) 0.0324(4) Uani 1 1 d . . . H6 H 0.4686 0.5119 0.4324 0.043 Uiso 1 1 calc R . . C7 C 0.45536(8) 0.53115(15) 0.32990(9) 0.0303(4) Uani 1 1 d . . . C8 C 0.47777(8) 0.66007(16) 0.33879(10) 0.0315(4) Uani 1 1 d . . . H8a H 0.5150 0.6690 0.3841 0.042 Uiso 1 1 calc R . . H8b H 0.4922 0.6803 0.3015 0.042 Uiso 1 1 calc R . . C9 C 0.42425(8) 0.74560(15) 0.33594(9) 0.0285(4) Uani 1 1 d . . . C10 C 0.42148(8) 0.77686(15) 0.40060(9) 0.0301(4) Uani 1 1 d . . . H10 H 0.4538 0.7491 0.4429 0.040 Uiso 1 1 calc R . . C11 C 0.37197(8) 0.84795(16) 0.40332(9) 0.0298(4) Uani 1 1 d . . . C12 C 0.32013(8) 0.88092(15) 0.33937(9) 0.0290(4) Uani 1 1 d . . . C13 C 0.32391(8) 0.85255(15) 0.27589(9) 0.0292(4) Uani 1 1 d . . . H13 H 0.2899 0.8758 0.2336 0.039 Uiso 1 1 calc R . . C14 C 0.37680(8) 0.79018(15) 0.27247(9) 0.0289(4) Uani 1 1 d . . . C15 C 0.38226(9) 0.78215(15) 0.20088(9) 0.0319(4) Uani 1 1 d . . . H15a H 0.3722 0.8594 0.1782 0.042 Uiso 1 1 calc R . . H15b H 0.4274 0.7637 0.2095 0.042 Uiso 1 1 calc R . . C16 C 0.33808(9) 0.69104(16) 0.14999(9) 0.0298(4) Uani 1 1 d . . . C17 C 0.27647(9) 0.72842(16) 0.10100(9) 0.0324(4) Uani 1 1 d . . . H17 H 0.2654 0.8083 0.0994 0.043 Uiso 1 1 calc R . . C18 C 0.23176(8) 0.65058(16) 0.05506(9) 0.0314(4) Uani 1 1 d . . . C19 C 0.24733(9) 0.53040(16) 0.05792(9) 0.0317(4) Uani 1 1 d . . . C20 C 0.30897(9) 0.49271(16) 0.10430(9) 0.0327(4) Uani 1 1 d . . . H20 H 0.3199 0.4130 0.1049 0.043 Uiso 1 1 calc R . . C21 C 0.35521(8) 0.57154(16) 0.15029(9) 0.0303(4) Uani 1 1 d . . . C22 C 0.06474(8) 0.54482(15) 0.33465(9) 0.0283(4) Uani 1 1 d . . . H22a H 0.0284 0.4903 0.3129 0.038 Uiso 1 1 calc R . . H22b H 0.0579 0.5875 0.3721 0.038 Uiso 1 1 calc R . . C23 C 0.12850(8) 0.47497(15) 0.36669(9) 0.0269(4) Uani 1 1 d . . . C24 C 0.18057(8) 0.52373(15) 0.42522(9) 0.0300(4) Uani 1 1 d . . . H24 H 0.1736 0.5934 0.4455 0.040 Uiso 1 1 calc R . . C25 C 0.24162(8) 0.47164(15) 0.45360(9) 0.0307(4) Uani 1 1 d . . . C26 C 0.25306(8) 0.36898(15) 0.42237(9) 0.0299(4) Uani 1 1 d . . . C27 C 0.20171(8) 0.31822(15) 0.36552(9) 0.0281(4) Uani 1 1 d . . . H27 H 0.2092 0.2491 0.3452 0.037 Uiso 1 1 calc R . . C28 C 0.13867(8) 0.36835(15) 0.33784(9) 0.0263(4) Uani 1 1 d . . . C29 C 0.08390(8) 0.30004(15) 0.28004(9) 0.0272(4) Uani 1 1 d . . . H29a H 0.0877 0.2169 0.2933 0.036 Uiso 1 1 calc R . . H29b H 0.0421 0.3283 0.2782 0.036 Uiso 1 1 calc R . . C30 C 0.08344(8) 0.31015(14) 0.20641(9) 0.0267(4) Uani 1 1 d . . . C31 C 0.11656(8) 0.22414(15) 0.18494(9) 0.0289(4) Uani 1 1 d . . . H31 H 0.1380 0.1635 0.2165 0.038 Uiso 1 1 calc R . . C32 C 0.11892(8) 0.22508(15) 0.11858(9) 0.0293(4) Uani 1 1 d . . . C33 C 0.08793(8) 0.31834(15) 0.07156(9) 0.0275(4) Uani 1 1 d . . . C34 C 0.05386(8) 0.40203(15) 0.09235(9) 0.0278(4) Uani 1 1 d . . . H34 H 0.0325 0.4625 0.0607 0.037 Uiso 1 1 calc R . . C35 C 0.04987(8) 0.40046(15) 0.15828(9) 0.0266(4) Uani 1 1 d . . . C36 C 0.00669(8) 0.49254(15) 0.17314(9) 0.0282(4) Uani 1 1 d . . . H36a H -0.0301 0.5105 0.1287 0.038 Uiso 1 1 calc R . . H36b H -0.0110 0.4573 0.2048 0.038 Uiso 1 1 calc R . . C37 C 0.04012(7) 0.60848(15) 0.20593(9) 0.0259(4) Uani 1 1 d . . . C38 C 0.04314(8) 0.69765(15) 0.15975(9) 0.0282(4) Uani 1 1 d . . . H38 H 0.0249 0.6833 0.1110 0.037 Uiso 1 1 calc R . . C39 C 0.07235(8) 0.80592(15) 0.18431(9) 0.0284(4) Uani 1 1 d . . . C40 C 0.10033(8) 0.82823(14) 0.25769(9) 0.0269(4) Uani 1 1 d . . . C41 C 0.09634(8) 0.74189(15) 0.30366(9) 0.0268(4) Uani 1 1 d . . . H41 H 0.1142 0.7571 0.3523 0.036 Uiso 1 1 calc R . . C42 C 0.06614(8) 0.63241(15) 0.27898(9) 0.0262(4) Uani 1 1 d . . . C43 C 0.40433(9) 0.20626(17) 0.45475(11) 0.0369(4) Uani 1 1 d . . . H43a H 0.4135 0.1884 0.5041 0.049 Uiso 1 1 calc R . . H43b H 0.4152 0.1364 0.4342 0.049 Uiso 1 1 calc R . . C44 C 0.33208(9) 0.23064(16) 0.41594(10) 0.0358(4) Uani 1 1 d . . . H44a H 0.3223 0.2555 0.3675 0.048 Uiso 1 1 calc R . . H44b H 0.3070 0.1595 0.4144 0.048 Uiso 1 1 calc R . . C45 C 0.23184(8) 0.89728(16) 0.37587(10) 0.0319(4) Uani 1 1 d . . . H45a H 0.2557 0.9074 0.4268 0.042 Uiso 1 1 calc R . . H45b H 0.2255 0.8131 0.3657 0.042 Uiso 1 1 calc R . . C46 C 0.16685(8) 0.95927(15) 0.35098(9) 0.0297(4) Uani 1 1 d . . . H46a H 0.1434 0.9317 0.3789 0.039 Uiso 1 1 calc R . . H46b H 0.1743 1.0438 0.3592 0.039 Uiso 1 1 calc R . . C47 C 0.20112(9) 0.33513(15) 0.02739(9) 0.0320(4) Uani 1 1 d . . . H47a H 0.2109 0.3247 0.0775 0.043 Uiso 1 1 calc R . . H47b H 0.2345 0.2945 0.0167 0.043 Uiso 1 1 calc R . . C48 C 0.13441(8) 0.28620(16) -0.01735(9) 0.0322(4) Uani 1 1 d . . . H48a H 0.1234 0.3065 -0.0668 0.043 Uiso 1 1 calc R . . H48b H 0.1360 0.2003 -0.0136 0.043 Uiso 1 1 calc R . . C49 C 0.39755(12) 0.1042(2) 0.26273(14) 0.0564(6) Uani 1 1 d . . . H49a H 0.3546 0.1300 0.2309 0.085 Uiso 1 1 calc R . . H49b H 0.3965 0.0209 0.2719 0.085 Uiso 1 1 calc R . . H49c H 0.4281 0.1187 0.2415 0.085 Uiso 1 1 calc R . . C50 C 0.42809(9) 0.8788(2) 0.52828(10) 0.0436(5) Uani 1 1 d . . . H50a H 0.4365 0.7961 0.5395 0.065 Uiso 1 1 calc R . . H50b H 0.4224 0.9185 0.5668 0.065 Uiso 1 1 calc R . . H50c H 0.4645 0.9132 0.5213 0.065 Uiso 1 1 calc R . . C51 C 0.11715(11) 0.6677(3) 0.01769(14) 0.0627(7) Uani 1 1 d . . . H51a H 0.1112 0.5833 0.0174 0.094 Uiso 1 1 calc R . . H51b H 0.0791 0.7033 -0.0184 0.094 Uiso 1 1 calc R . . H51c H 0.1232 0.6988 0.0634 0.094 Uiso 1 1 calc R . . C52 C 0.34110(11) 0.5788(2) 0.50237(14) 0.0596(6) Uani 1 1 d . . . H52a H 0.3606 0.5258 0.4798 0.089 Uiso 1 1 calc R . . H52b H 0.3740 0.6051 0.5470 0.089 Uiso 1 1 calc R . . H52c H 0.3229 0.6460 0.4721 0.089 Uiso 1 1 calc R . . C53 C 0.19720(10) 0.06675(18) 0.14789(12) 0.0440(5) Uani 1 1 d . . . H53a H 0.2274 0.1168 0.1842 0.066 Uiso 1 1 calc R . . H53b H 0.2206 0.0211 0.1262 0.066 Uiso 1 1 calc R . . H53c H 0.1760 0.0141 0.1688 0.066 Uiso 1 1 calc R . . C54 C 0.02876(11) 0.90497(19) 0.07193(10) 0.0466(5) Uani 1 1 d . . . H54a H 0.0193 0.8269 0.0516 0.070 Uiso 1 1 calc R . . H54b H 0.0450 0.9536 0.0442 0.070 Uiso 1 1 calc R . . H54c H -0.0106 0.9394 0.0721 0.070 Uiso 1 1 calc R . . O1 O 0.44625(6) 0.30257(12) 0.45278(7) 0.0375(3) Uani 1 1 d . . . O2 O 0.31546(6) 0.32242(11) 0.45342(7) 0.0367(3) Uani 1 1 d . . . O3 O 0.26824(6) 0.94901(10) 0.33857(6) 0.0322(3) Uani 1 1 d . . . O4 O 0.12700(6) 0.93971(10) 0.27717(6) 0.0308(3) Uani 1 1 d . . . O5 O 0.19979(6) 0.45871(11) 0.01060(7) 0.0391(3) Uani 1 1 d . . . O6 O 0.08327(6) 0.32948(11) 0.00255(6) 0.0334(3) Uani 1 1 d . . . O7 O 0.41733(8) 0.16771(12) 0.32753(8) 0.0495(4) Uani 1 1 d . . . O8 O 0.36985(6) 0.89135(12) 0.46471(6) 0.0372(3) Uani 1 1 d . . . O9 O 0.17347(6) 0.69389(12) 0.00381(7) 0.0385(3) Uani 1 1 d . . . O10 O 0.29033(6) 0.51825(12) 0.51465(7) 0.0400(3) Uani 1 1 d . . . O11 O 0.14892(6) 0.13843(11) 0.09511(7) 0.0392(3) Uani 1 1 d . . . O12 O 0.07669(7) 0.89753(12) 0.14250(7) 0.0430(3) Uani 1 1 d . . . O13a O 0.2303(15) 0.576(3) 0.2638(17) 0.124(8) Uiso 0.14 1 d P . . O13b O 0.2505(10) 0.4964(19) 0.2484(12) 0.122(5) Uiso 0.17 1 d P . . O13c O 0.2080(11) 0.523(2) 0.2105(12) 0.125(6) Uiso 0.16 1 d P . . O13d O 0.2191(16) 0.603(3) 0.232(2) 0.129(11) Uiso 0.12 1 d P . . O13e O 0.2756(14) 0.569(2) 0.3036(14) 0.126(7) Uiso 0.13 1 d P . . O13f O 0.2985(15) 0.479(3) 0.3024(16) 0.128(9) Uiso 0.11 1 d P . . O13g O 0.2614(8) 0.3836(16) 0.2351(9) 0.120(5) Uiso 0.17 1 d P . . O14 O 0.3528(5) 0.3202(9) 0.6047(5) 0.106(3) 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 C1 0.0350(9) 0.0343(10) 0.0320(9) -0.0052(8) 0.0142(8) 0.0025(7) C2 0.0269(9) 0.0339(10) 0.0315(9) -0.0015(7) 0.0095(7) 0.0046(7) C3 0.0314(9) 0.0345(10) 0.0343(10) -0.0058(8) 0.0094(8) 0.0029(7) C4 0.0323(9) 0.0280(9) 0.0422(11) -0.0003(8) 0.0123(8) 0.0018(7) C5 0.0261(9) 0.0376(10) 0.0316(9) 0.0041(8) 0.0072(7) 0.0056(7) C6 0.0289(9) 0.0344(10) 0.0309(9) -0.0023(7) 0.0090(7) 0.0037(7) C7 0.0247(8) 0.0326(9) 0.0314(9) -0.0017(7) 0.0091(7) 0.0036(7) C8 0.0283(9) 0.0351(10) 0.0295(9) -0.0031(7) 0.0101(7) -0.0017(7) C9 0.0275(8) 0.0266(9) 0.0307(9) -0.0023(7) 0.0110(7) -0.0047(7) C10 0.0272(9) 0.0320(9) 0.0275(9) -0.0003(7) 0.0073(7) -0.0001(7) C11 0.0291(9) 0.0330(9) 0.0278(9) -0.0039(7) 0.0121(7) -0.0029(7) C12 0.0264(8) 0.0262(9) 0.0331(9) 0.0005(7) 0.0107(7) -0.0020(7) C13 0.0285(9) 0.0276(9) 0.0283(9) 0.0011(7) 0.0081(7) -0.0023(7) C14 0.0318(9) 0.0234(8) 0.0301(9) -0.0019(7) 0.0110(7) -0.0054(7) C15 0.0384(10) 0.0282(9) 0.0297(9) 0.0003(7) 0.0145(8) -0.0026(7) C16 0.0359(9) 0.0314(9) 0.0238(8) -0.0002(7) 0.0140(7) -0.0011(7) C17 0.0408(10) 0.0278(9) 0.0300(9) 0.0011(7) 0.0156(8) 0.0010(7) C18 0.0332(9) 0.0353(10) 0.0248(9) 0.0034(7) 0.0108(7) 0.0017(7) C19 0.0362(10) 0.0330(10) 0.0247(8) -0.0012(7) 0.0111(7) -0.0055(7) C20 0.0401(10) 0.0285(9) 0.0300(9) 0.0001(7) 0.0147(8) 0.0016(7) C21 0.0341(9) 0.0334(9) 0.0248(8) 0.0011(7) 0.0132(7) 0.0000(7) C22 0.0322(9) 0.0288(9) 0.0273(9) 0.0019(7) 0.0155(7) 0.0011(7) C23 0.0320(9) 0.0280(9) 0.0236(8) 0.0052(7) 0.0142(7) -0.0017(7) C24 0.0367(10) 0.0262(9) 0.0282(9) 0.0008(7) 0.0143(8) -0.0008(7) C25 0.0317(9) 0.0313(9) 0.0269(9) -0.0015(7) 0.0098(7) -0.0053(7) C26 0.0281(9) 0.0316(9) 0.0295(9) 0.0049(7) 0.0111(7) 0.0007(7) C27 0.0322(9) 0.0258(8) 0.0273(9) 0.0025(7) 0.0129(7) 0.0000(7) C28 0.0300(9) 0.0271(9) 0.0239(8) 0.0054(7) 0.0131(7) -0.0030(7) C29 0.0272(8) 0.0247(8) 0.0289(9) 0.0025(7) 0.0105(7) -0.0016(6) C30 0.0236(8) 0.0258(8) 0.0284(9) 0.0006(7) 0.0081(7) -0.0035(6) C31 0.0285(9) 0.0272(9) 0.0281(9) 0.0036(7) 0.0084(7) 0.0016(7) C32 0.0305(9) 0.0250(8) 0.0318(9) -0.0028(7) 0.0119(7) 0.0008(7) C33 0.0271(8) 0.0291(9) 0.0234(8) -0.0025(7) 0.0071(7) -0.0036(7) C34 0.0266(8) 0.0270(9) 0.0245(8) 0.0017(7) 0.0048(7) 0.0004(7) C35 0.0239(8) 0.0257(9) 0.0270(9) -0.0014(7) 0.0071(7) -0.0026(6) C36 0.0237(8) 0.0306(9) 0.0280(9) 0.0009(7) 0.0079(7) -0.0006(7) C37 0.0212(8) 0.0281(9) 0.0284(9) 0.0016(7) 0.0102(7) 0.0040(6) C38 0.0263(8) 0.0335(9) 0.0225(8) 0.0013(7) 0.0075(7) 0.0024(7) C39 0.0280(9) 0.0299(9) 0.0272(9) 0.0066(7) 0.0109(7) 0.0013(7) C40 0.0240(8) 0.0264(8) 0.0290(9) 0.0007(7) 0.0093(7) 0.0015(6) C41 0.0264(8) 0.0299(9) 0.0239(8) 0.0014(7) 0.0099(7) 0.0030(7) C42 0.0241(8) 0.0280(9) 0.0279(9) 0.0024(7) 0.0120(7) 0.0044(6) C43 0.0326(10) 0.0338(10) 0.0418(11) 0.0082(8) 0.0124(8) 0.0023(7) C44 0.0330(10) 0.0313(10) 0.0406(10) -0.0016(8) 0.0123(8) 0.0013(7) C45 0.0292(9) 0.0333(10) 0.0320(9) 0.0034(7) 0.0110(7) -0.0005(7) C46 0.0295(9) 0.0285(9) 0.0280(9) -0.0015(7) 0.0084(7) -0.0009(7) C47 0.0385(10) 0.0279(9) 0.0303(9) -0.0013(7) 0.0146(8) 0.0002(7) C48 0.0376(10) 0.0320(9) 0.0275(9) -0.0034(7) 0.0135(8) 0.0007(7) C49 0.0672(15) 0.0403(12) 0.0749(16) -0.0198(11) 0.0422(13) -0.0186(10) C50 0.0338(10) 0.0647(14) 0.0285(10) -0.0072(9) 0.0087(8) 0.0057(9) C51 0.0390(12) 0.0828(18) 0.0657(16) 0.0107(14) 0.0206(11) 0.0086(11) C52 0.0473(13) 0.0633(15) 0.0631(15) -0.0198(12) 0.0170(11) -0.0228(11) C53 0.0413(11) 0.0373(11) 0.0561(13) 0.0086(9) 0.0224(10) 0.0136(8) C54 0.0626(13) 0.0396(11) 0.0281(10) 0.0089(8) 0.0086(9) 0.0027(10) O1 0.0320(7) 0.0407(7) 0.0342(7) 0.0069(6) 0.0075(5) 0.0001(5) O2 0.0284(6) 0.0392(7) 0.0366(7) -0.0033(6) 0.0071(5) 0.0040(5) O3 0.0301(6) 0.0315(7) 0.0360(7) 0.0038(5) 0.0145(5) 0.0032(5) O4 0.0313(6) 0.0271(6) 0.0288(6) 0.0022(5) 0.0067(5) -0.0020(5) O5 0.0443(7) 0.0308(7) 0.0316(7) 0.0027(5) 0.0042(6) -0.0057(5) O6 0.0344(7) 0.0402(7) 0.0240(6) -0.0012(5) 0.0102(5) 0.0040(5) O7 0.0660(10) 0.0305(7) 0.0555(9) -0.0032(6) 0.0280(8) -0.0024(6) O8 0.0295(6) 0.0519(8) 0.0274(7) -0.0064(6) 0.0085(5) 0.0036(6) O9 0.0357(7) 0.0395(7) 0.0331(7) 0.0047(6) 0.0066(6) 0.0027(6) O10 0.0354(7) 0.0441(8) 0.0328(7) -0.0086(6) 0.0060(6) -0.0044(6) O11 0.0501(8) 0.0317(7) 0.0391(7) 0.0026(6) 0.0214(6) 0.0121(6) O12 0.0487(8) 0.0419(8) 0.0290(7) 0.0117(6) 0.0061(6) -0.0102(6) O14 0.104(7) 0.118(8) 0.081(6) 0.017(5) 0.024(5) -0.006(6) 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 1.512(3) . ? C1 C21 1.525(2) . ? C2 C3 1.393(3) . ? C2 C7 1.401(2) . ? C3 C4 1.380(3) . ? C4 O7 1.375(2) . ? C4 C5 1.403(3) . ? C5 C6 1.382(3) . ? C5 O1 1.383(2) . ? C6 C7 1.399(3) . ? C7 C8 1.523(2) . ? C8 C9 1.516(2) . ? C9 C14 1.399(2) . ? C9 C10 1.399(2) . ? C10 C11 1.382(2) . ? C11 O8 1.371(2) . ? C11 C12 1.404(2) . ? C12 C13 1.377(3) . ? C12 O3 1.382(2) . ? C13 C14 1.398(2) . ? C14 C15 1.526(2) . ? C15 C16 1.511(2) . ? C16 C21 1.399(2) . ? C16 C17 1.399(2) . ? C17 C18 1.376(2) . ? C18 O9 1.389(2) . ? C18 C19 1.393(3) . ? C19 O5 1.374(2) . ? C19 C20 1.385(2) . ? C20 C21 1.399(2) . ? C22 C42 1.520(2) . ? C22 C23 1.522(2) . ? C23 C28 1.398(2) . ? C23 C24 1.402(2) . ? C24 C25 1.376(2) . ? C25 O10 1.388(2) . ? C25 C26 1.395(3) . ? C26 O2 1.378(2) . ? C26 C27 1.386(2) . ? C27 C28 1.403(2) . ? C28 C29 1.523(2) . ? C29 C30 1.512(2) . ? C30 C31 1.393(2) . ? C30 C35 1.405(2) . ? C31 C32 1.385(2) . ? C32 O11 1.376(2) . ? C32 C33 1.405(2) . ? C33 C34 1.382(2) . ? C33 O6 1.384(2) . ? C34 C35 1.392(2) . ? C35 C36 1.527(2) . ? C36 C37 1.520(2) . ? C37 C42 1.399(2) . ? C37 C38 1.402(2) . ? C38 C39 1.379(2) . ? C39 O12 1.371(2) . ? C39 C40 1.401(2) . ? C40 O4 1.378(2) . ? C40 C41 1.383(2) . ? C41 C42 1.399(2) . ? C43 O1 1.443(2) . ? C43 C44 1.505(2) . ? C44 O2 1.425(2) . ? C45 O3 1.444(2) . ? C45 C46 1.499(2) . ? C46 O4 1.431(2) . ? C47 O5 1.432(2) . ? C47 C48 1.501(2) . ? C48 O6 1.442(2) . ? C49 O7 1.415(3) . ? C50 O8 1.428(2) . ? C51 O9 1.425(3) . ? C52 O10 1.427(3) . ? C53 O11 1.429(2) . ? C54 O12 1.413(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 C2 C1 C21 115.52(15) . . ? C3 C2 C7 118.63(17) . . ? C3 C2 C1 117.24(16) . . ? C7 C2 C1 124.12(16) . . ? C4 C3 C2 122.65(17) . . ? O7 C4 C3 123.70(17) . . ? O7 C4 C5 117.23(17) . . ? C3 C4 C5 119.04(17) . . ? C6 C5 O1 116.67(16) . . ? C6 C5 C4 118.08(17) . . ? O1 C5 C4 125.05(17) . . ? C5 C6 C7 123.18(17) . . ? C6 C7 C2 117.98(17) . . ? C6 C7 C8 118.21(16) . . ? C2 C7 C8 123.82(16) . . ? C9 C8 C7 112.79(14) . . ? C14 C9 C10 119.19(16) . . ? C14 C9 C8 123.45(16) . . ? C10 C9 C8 117.32(15) . . ? C11 C10 C9 121.73(16) . . ? O8 C11 C10 124.63(15) . . ? O8 C11 C12 116.42(15) . . ? C10 C11 C12 118.94(16) . . ? C13 C12 O3 119.21(15) . . ? C13 C12 C11 118.84(16) . . ? O3 C12 C11 121.75(16) . . ? C12 C13 C14 122.61(16) . . ? C13 C14 C9 117.98(16) . . ? C13 C14 C15 118.34(15) . . ? C9 C14 C15 123.52(16) . . ? C16 C15 C14 115.06(14) . . ? C21 C16 C17 118.65(16) . . ? C21 C16 C15 123.41(15) . . ? C17 C16 C15 117.93(16) . . ? C18 C17 C16 121.96(17) . . ? C17 C18 O9 119.48(16) . . ? C17 C18 C19 119.47(16) . . ? O9 C18 C19 120.95(15) . . ? O5 C19 C20 124.98(16) . . ? O5 C19 C18 115.73(15) . . ? C20 C19 C18 119.21(16) . . ? C19 C20 C21 121.67(17) . . ? C20 C21 C16 118.90(16) . . ? C20 C21 C1 118.65(16) . . ? C16 C21 C1 122.28(16) . . ? C42 C22 C23 111.21(13) . . ? C28 C23 C24 118.72(15) . . ? C28 C23 C22 122.96(15) . . ? C24 C23 C22 118.20(15) . . ? C25 C24 C23 122.00(16) . . ? C24 C25 O10 119.98(16) . . ? C24 C25 C26 119.45(15) . . ? O10 C25 C26 120.51(15) . . ? O2 C26 C27 124.62(16) . . ? O2 C26 C25 116.13(15) . . ? C27 C26 C25 119.19(15) . . ? C26 C27 C28 121.71(16) . . ? C23 C28 C27 118.77(15) . . ? C23 C28 C29 123.28(15) . . ? C27 C28 C29 117.89(15) . . ? C30 C29 C28 114.90(13) . . ? C31 C30 C35 118.74(16) . . ? C31 C30 C29 118.25(15) . . ? C35 C30 C29 123.00(15) . . ? C32 C31 C30 122.77(16) . . ? O11 C32 C31 123.78(15) . . ? O11 C32 C33 117.61(15) . . ? C31 C32 C33 118.59(15) . . ? C34 C33 O6 115.52(15) . . ? C34 C33 C32 118.48(16) . . ? O6 C33 C32 125.74(15) . . ? C33 C34 C35 123.40(16) . . ? C34 C35 C30 117.92(16) . . ? C34 C35 C36 118.58(15) . . ? C30 C35 C36 123.42(15) . . ? C37 C36 C35 115.93(13) . . ? C42 C37 C38 118.36(15) . . ? C42 C37 C36 123.90(15) . . ? C38 C37 C36 117.72(15) . . ? C39 C38 C37 122.09(15) . . ? O12 C39 C38 125.41(16) . . ? O12 C39 C40 115.16(15) . . ? C38 C39 C40 119.43(15) . . ? O4 C40 C41 125.60(15) . . ? O4 C40 C39 115.35(14) . . ? C41 C40 C39 118.97(15) . . ? C40 C41 C42 121.82(15) . . ? C41 C42 C37 119.28(15) . . ? C41 C42 C22 116.95(15) . . ? C37 C42 C22 123.76(15) . . ? O1 C43 C44 114.43(15) . . ? O2 C44 C43 107.58(15) . . ? O3 C45 C46 107.63(14) . . ? O4 C46 C45 112.96(14) . . ? O5 C47 C48 106.90(14) . . ? O6 C48 C47 113.73(14) . . ? C5 O1 C43 120.99(14) . . ? C26 O2 C44 117.40(13) . . ? C12 O3 C45 114.56(13) . . ? C40 O4 C46 117.28(13) . . ? C19 O5 C47 117.81(13) . . ? C33 O6 C48 121.22(13) . . ? C4 O7 C49 117.60(17) . . ? C11 O8 C50 116.70(14) . . ? C18 O9 C51 113.89(15) . . ? C25 O10 C52 114.05(15) . . ? C32 O11 C53 117.30(15) . . ? C39 O12 C54 118.15(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.403 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.050