data_CCDC-778897 _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 O12 Xe' _chemical_formula_weight 1026.27 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' 'Xe' 'Xe' -0.4205 1.9578 '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 22.0490(9) _cell_length_b 11.4109(5) _cell_length_c 20.7802(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.599(2) _cell_angle_gamma 90.00 _cell_volume 4633.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.810 _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_min 0.9181 _exptl_absorpt_correction_T_max 1.0000 _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 36314 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _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 2.56 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8203 _reflns_number_gt 6581 _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^)+(0.0202P)^2^+7.4179P] 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 8203 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Xe1 Xe 0.255322(14) 0.45729(3) 0.516353(15) 0.06885(10) Uani 1 1 d . . . C1 C 0.41182(13) 0.7006(2) 0.70072(14) 0.0229(6) Uani 1 1 d . . . H1a H 0.4080 0.7833 0.7090 0.031 Uiso 1 1 calc R . . H1b H 0.4554 0.6735 0.7388 0.031 Uiso 1 1 calc R . . C2 C 0.41220(12) 0.6868(2) 0.62830(13) 0.0215(5) Uani 1 1 d . . . C3 C 0.37499(13) 0.7679(2) 0.57359(14) 0.0259(6) Uani 1 1 d . . . H3 H 0.3508 0.8263 0.5831 0.034 Uiso 1 1 calc R . . C4 C 0.37275(13) 0.7650(2) 0.50583(14) 0.0261(6) Uani 1 1 d . . . C5 C 0.40742(13) 0.6750(2) 0.49051(14) 0.0237(6) Uani 1 1 d . . . C6 C 0.44462(12) 0.5953(2) 0.54490(14) 0.0222(5) Uani 1 1 d . . . H6 H 0.4679 0.5359 0.5349 0.029 Uiso 1 1 calc R . . C7 C 0.44892(12) 0.6000(2) 0.61424(13) 0.0210(5) Uani 1 1 d . . . C8 C 0.49504(12) 0.5111(2) 0.67039(14) 0.0223(5) Uani 1 1 d . . . H8a H 0.5343 0.4957 0.6623 0.030 Uiso 1 1 calc R . . H8b H 0.5119 0.5454 0.7183 0.030 Uiso 1 1 calc R . . C9 C 0.46059(12) 0.3955(2) 0.66914(13) 0.0197(5) Uani 1 1 d . . . C10 C 0.45946(12) 0.3095(2) 0.62081(14) 0.0232(6) Uani 1 1 d . . . H10 H 0.4803 0.3250 0.5917 0.031 Uiso 1 1 calc R . . C11 C 0.42848(13) 0.2026(2) 0.61488(14) 0.0248(6) Uani 1 1 d . . . C12 C 0.39606(12) 0.1789(2) 0.65790(13) 0.0212(5) Uani 1 1 d . . . C13 C 0.39819(12) 0.2623(2) 0.70662(13) 0.0209(5) Uani 1 1 d . . . H13 H 0.3778 0.2462 0.7360 0.028 Uiso 1 1 calc R . . C14 C 0.43028(12) 0.3713(2) 0.71327(13) 0.0198(5) Uani 1 1 d . . . C15 C 0.43009(13) 0.4555(2) 0.76970(13) 0.0221(5) Uani 1 1 d . . . H15a H 0.4685 0.5089 0.7844 0.029 Uiso 1 1 calc R . . H15b H 0.4362 0.4115 0.8122 0.029 Uiso 1 1 calc R . . C16 C 0.36404(13) 0.5265(2) 0.74181(13) 0.0222(5) Uani 1 1 d . . . C17 C 0.30912(13) 0.4777(2) 0.74899(14) 0.0248(6) Uani 1 1 d . . . H17 H 0.3151 0.4058 0.7723 0.033 Uiso 1 1 calc R . . C18 C 0.24658(13) 0.5326(2) 0.72276(14) 0.0247(6) Uani 1 1 d . . . C19 C 0.23660(13) 0.6404(2) 0.68748(13) 0.0236(6) Uani 1 1 d . . . C20 C 0.29069(13) 0.6896(2) 0.68046(13) 0.0224(5) Uani 1 1 d . . . H20 H 0.2842 0.7613 0.6569 0.030 Uiso 1 1 calc R . . C21 C 0.35474(12) 0.6352(2) 0.70754(13) 0.0207(5) Uani 1 1 d . . . C22 C 0.10605(14) 0.2103(2) 0.32146(14) 0.0254(6) Uani 1 1 d . . . H22a H 0.1167 0.1331 0.3100 0.034 Uiso 1 1 calc R . . H22b H 0.0591 0.2279 0.2866 0.034 Uiso 1 1 calc R . . C23 C 0.15257(13) 0.2987(2) 0.31180(13) 0.0239(6) Uani 1 1 d . . . C24 C 0.21912(14) 0.2639(2) 0.32867(14) 0.0262(6) Uani 1 1 d . . . H24 H 0.2318 0.1863 0.3414 0.035 Uiso 1 1 calc R . . C25 C 0.26641(14) 0.3411(2) 0.32705(14) 0.0273(6) Uani 1 1 d . . . C26 C 0.24787(14) 0.4580(2) 0.30912(14) 0.0264(6) Uani 1 1 d . . . C27 C 0.18079(13) 0.4914(2) 0.28714(14) 0.0256(6) Uani 1 1 d . . . H27 H 0.1677 0.5681 0.2718 0.034 Uiso 1 1 calc R . . C28 C 0.13233(13) 0.4130(2) 0.28742(13) 0.0234(6) Uani 1 1 d . . . C29 C 0.05991(13) 0.4581(2) 0.26327(13) 0.0257(6) Uani 1 1 d . . . H29a H 0.0468 0.5102 0.2221 0.034 Uiso 1 1 calc R . . H29b H 0.0282 0.3927 0.2482 0.034 Uiso 1 1 calc R . . C30 C 0.05620(12) 0.5229(2) 0.32481(13) 0.0224(5) Uani 1 1 d . . . C31 C 0.07761(13) 0.6394(2) 0.33395(14) 0.0260(6) Uani 1 1 d . . . H31 H 0.0865 0.6743 0.2987 0.035 Uiso 1 1 calc R . . C32 C 0.08610(13) 0.7047(2) 0.39334(14) 0.0263(6) Uani 1 1 d . . . C33 C 0.07515(13) 0.6505(2) 0.44743(14) 0.0254(6) Uani 1 1 d . . . C34 C 0.05043(12) 0.5369(2) 0.43656(14) 0.0247(6) Uani 1 1 d . . . H34 H 0.0408 0.5028 0.4714 0.033 Uiso 1 1 calc R . . C35 C 0.03933(12) 0.4710(2) 0.37501(13) 0.0231(6) Uani 1 1 d . . . C36 C 0.01003(13) 0.3478(2) 0.36585(14) 0.0262(6) Uani 1 1 d . . . H36a H -0.0280 0.3487 0.3771 0.035 Uiso 1 1 calc R . . H36b H -0.0075 0.3243 0.3155 0.035 Uiso 1 1 calc R . . C37 C 0.06220(13) 0.2577(2) 0.41396(14) 0.0241(6) Uani 1 1 d . . . C38 C 0.06256(13) 0.2293(2) 0.47944(14) 0.0274(6) Uani 1 1 d . . . H38 H 0.0290 0.2604 0.4897 0.036 Uiso 1 1 calc R . . C39 C 0.11189(13) 0.1554(3) 0.52965(14) 0.0277(6) Uani 1 1 d . . . C40 C 0.16607(13) 0.1194(2) 0.51802(14) 0.0240(6) Uani 1 1 d . . . C41 C 0.16384(13) 0.1428(2) 0.45165(14) 0.0241(6) Uani 1 1 d . . . H41 H 0.1991 0.1152 0.4431 0.032 Uiso 1 1 calc R . . C42 C 0.11079(13) 0.2061(2) 0.39701(14) 0.0225(5) Uani 1 1 d . . . C43 C 0.36323(13) 0.7061(2) 0.35880(14) 0.0272(6) Uani 1 1 d . . . H43a H 0.3783 0.6912 0.3225 0.036 Uiso 1 1 calc R . . H43b H 0.3591 0.7902 0.3621 0.036 Uiso 1 1 calc R . . C44 C 0.29430(14) 0.6512(2) 0.33448(14) 0.0260(6) Uani 1 1 d . . . H44a H 0.2823 0.6511 0.3739 0.035 Uiso 1 1 calc R . . H44b H 0.2597 0.6949 0.2941 0.035 Uiso 1 1 calc R . . C45 C 0.32306(13) 0.0478(2) 0.68025(14) 0.0244(6) Uani 1 1 d . . . H45a H 0.3447 0.0754 0.7301 0.033 Uiso 1 1 calc R . . H45b H 0.3158 -0.0359 0.6810 0.033 Uiso 1 1 calc R . . C46 C 0.25529(13) 0.1071(2) 0.63943(14) 0.0260(6) Uani 1 1 d . . . H46a H 0.2286 0.0985 0.6654 0.035 Uiso 1 1 calc R . . H46b H 0.2618 0.1900 0.6345 0.035 Uiso 1 1 calc R . . C47 C 0.15700(14) 0.7960(2) 0.62332(14) 0.0268(6) Uani 1 1 d . . . H47a H 0.1943 0.8513 0.6470 0.036 Uiso 1 1 calc R . . H47b H 0.1163 0.8308 0.6221 0.036 Uiso 1 1 calc R . . C48 C 0.14492(13) 0.7777(2) 0.54706(14) 0.0284(6) Uani 1 1 d . . . H48a H 0.1390 0.8525 0.5227 0.038 Uiso 1 1 calc R . . H48b H 0.1838 0.7380 0.5470 0.038 Uiso 1 1 calc R . . C49 C 0.30262(15) 0.9364(3) 0.46705(17) 0.0375(7) Uani 1 1 d . . . H49a H 0.2680 0.9019 0.4767 0.056 Uiso 1 1 calc R . . H49b H 0.2815 0.9871 0.4256 0.056 Uiso 1 1 calc R . . H49c H 0.3336 0.9810 0.5085 0.056 Uiso 1 1 calc R . . C50 C 0.48165(19) 0.1033(3) 0.5537(2) 0.0495(9) Uani 1 1 d . . . H50a H 0.5176 0.1560 0.5841 0.074 Uiso 1 1 calc R . . H50b H 0.4667 0.1228 0.5036 0.074 Uiso 1 1 calc R . . H50c H 0.4985 0.0244 0.5626 0.074 Uiso 1 1 calc R . . C51 C 0.14361(16) 0.4263(3) 0.67163(18) 0.0443(8) Uani 1 1 d . . . H51a H 0.1260 0.4794 0.6312 0.067 Uiso 1 1 calc R . . H51b H 0.1070 0.4008 0.6811 0.067 Uiso 1 1 calc R . . H51c H 0.1635 0.3596 0.6604 0.067 Uiso 1 1 calc R . . C52 C 0.38212(17) 0.3243(4) 0.4117(2) 0.0613(11) Uani 1 1 d . . . H52a H 0.3857 0.4072 0.4205 0.092 Uiso 1 1 calc R . . H52b H 0.4251 0.2947 0.4174 0.092 Uiso 1 1 calc R . . H52c H 0.3705 0.2861 0.4457 0.092 Uiso 1 1 calc R . . C53 C 0.12818(16) 0.8685(3) 0.35447(16) 0.0367(7) Uani 1 1 d . . . H53a H 0.1653 0.8212 0.3572 0.055 Uiso 1 1 calc R . . H53b H 0.1439 0.9471 0.3691 0.055 Uiso 1 1 calc R . . H53c H 0.0919 0.8688 0.3055 0.055 Uiso 1 1 calc R . . C54 C 0.04806(16) 0.1296(4) 0.59461(19) 0.0564(11) Uani 1 1 d . . . H54a H 0.0420 0.2111 0.6017 0.085 Uiso 1 1 calc R . . H54b H 0.0496 0.0850 0.6345 0.085 Uiso 1 1 calc R . . H54c H 0.0105 0.1031 0.5501 0.085 Uiso 1 1 calc R . . O1 O 0.41422(9) 0.66265(17) 0.42794(9) 0.0278(4) Uani 1 1 d . . . O2 O 0.29806(10) 0.53335(17) 0.31257(11) 0.0343(5) Uani 1 1 d . . . O3 O 0.36800(9) 0.06883(15) 0.64921(10) 0.0250(4) Uani 1 1 d . . . O4 O 0.21972(9) 0.05323(16) 0.56838(9) 0.0263(4) Uani 1 1 d . . . O5 O 0.17318(9) 0.69109(16) 0.66579(10) 0.0268(4) Uani 1 1 d . . . O6 O 0.08390(9) 0.70719(16) 0.50990(10) 0.0280(4) Uani 1 1 d . . . O7 O 0.33923(11) 0.84672(18) 0.45274(10) 0.0377(5) Uani 1 1 d . . . O8 O 0.42620(11) 0.11380(18) 0.56963(12) 0.0407(5) Uani 1 1 d . . . O9 O 0.19464(9) 0.48424(17) 0.73437(10) 0.0326(5) Uani 1 1 d . . . O10 O 0.33048(10) 0.30184(18) 0.34003(11) 0.0358(5) Uani 1 1 d . . . O11 O 0.10357(11) 0.82146(16) 0.40136(10) 0.0346(5) Uani 1 1 d . . . O12 O 0.11057(10) 0.1143(2) 0.59095(11) 0.0404(5) 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 Xe1 0.05838(16) 0.07244(19) 0.06453(17) -0.02212(14) 0.01897(13) -0.00870(13) C1 0.0246(13) 0.0196(13) 0.0239(13) -0.0029(11) 0.0107(11) -0.0008(10) C2 0.0200(12) 0.0200(13) 0.0243(13) -0.0031(11) 0.0101(11) -0.0043(10) C3 0.0270(14) 0.0202(14) 0.0325(15) -0.0010(11) 0.0154(12) 0.0019(11) C4 0.0265(14) 0.0248(14) 0.0260(14) 0.0045(11) 0.0114(12) 0.0032(11) C5 0.0232(13) 0.0248(14) 0.0251(13) 0.0004(11) 0.0129(11) -0.0024(11) C6 0.0201(12) 0.0218(13) 0.0292(14) -0.0017(11) 0.0154(11) 0.0000(10) C7 0.0169(12) 0.0212(13) 0.0240(13) -0.0001(11) 0.0086(11) -0.0040(10) C8 0.0179(12) 0.0261(14) 0.0238(13) -0.0004(11) 0.0103(11) -0.0002(10) C9 0.0139(12) 0.0223(13) 0.0183(12) 0.0020(10) 0.0035(10) 0.0034(10) C10 0.0214(13) 0.0269(14) 0.0248(13) 0.0026(11) 0.0136(11) 0.0020(11) C11 0.0246(13) 0.0274(14) 0.0222(13) -0.0040(11) 0.0107(11) 0.0004(11) C12 0.0191(12) 0.0197(13) 0.0226(13) 0.0013(10) 0.0079(11) 0.0024(10) C13 0.0209(13) 0.0245(14) 0.0201(12) 0.0030(11) 0.0118(11) 0.0045(10) C14 0.0183(12) 0.0210(13) 0.0163(12) 0.0020(10) 0.0047(10) 0.0057(10) C15 0.0261(13) 0.0225(13) 0.0174(12) 0.0003(10) 0.0099(11) -0.0001(11) C16 0.0272(13) 0.0232(14) 0.0164(12) -0.0047(10) 0.0104(11) -0.0001(11) C17 0.0344(15) 0.0213(14) 0.0220(13) 0.0018(11) 0.0158(12) 0.0013(11) C18 0.0295(14) 0.0262(14) 0.0229(13) -0.0012(11) 0.0159(11) -0.0037(11) C19 0.0230(13) 0.0269(14) 0.0200(13) -0.0047(11) 0.0092(11) 0.0007(11) C20 0.0282(14) 0.0176(13) 0.0210(13) -0.0016(10) 0.0111(11) -0.0009(11) C21 0.0239(13) 0.0215(13) 0.0165(12) -0.0050(10) 0.0092(11) -0.0014(10) C22 0.0307(14) 0.0215(14) 0.0239(13) -0.0034(11) 0.0125(12) -0.0017(11) C23 0.0297(14) 0.0270(14) 0.0169(12) -0.0056(11) 0.0124(11) -0.0033(11) C24 0.0340(15) 0.0227(14) 0.0242(13) -0.0025(11) 0.0155(12) 0.0007(11) C25 0.0292(14) 0.0308(15) 0.0262(14) -0.0031(12) 0.0164(12) 0.0029(12) C26 0.0348(15) 0.0256(14) 0.0250(14) -0.0045(11) 0.0190(12) -0.0060(12) C27 0.0339(15) 0.0223(14) 0.0249(14) 0.0005(11) 0.0174(12) 0.0021(11) C28 0.0295(14) 0.0243(14) 0.0176(12) -0.0031(11) 0.0118(11) -0.0023(11) C29 0.0276(14) 0.0273(14) 0.0200(13) 0.0032(11) 0.0093(11) -0.0006(12) C30 0.0176(12) 0.0264(14) 0.0200(12) 0.0030(11) 0.0059(10) 0.0057(10) C31 0.0240(13) 0.0310(15) 0.0226(13) 0.0060(11) 0.0104(11) 0.0035(11) C32 0.0258(14) 0.0240(14) 0.0261(14) 0.0014(11) 0.0096(12) 0.0030(11) C33 0.0190(13) 0.0312(15) 0.0244(13) 0.0000(12) 0.0088(11) 0.0047(11) C34 0.0193(12) 0.0321(15) 0.0234(13) 0.0040(11) 0.0105(11) 0.0026(11) C35 0.0166(12) 0.0276(14) 0.0219(13) 0.0044(11) 0.0064(10) 0.0048(11) C36 0.0222(13) 0.0312(15) 0.0232(13) 0.0034(12) 0.0088(11) -0.0004(11) C37 0.0214(13) 0.0241(14) 0.0239(13) -0.0010(11) 0.0080(11) -0.0049(11) C38 0.0225(13) 0.0317(15) 0.0301(15) 0.0018(12) 0.0139(12) 0.0016(11) C39 0.0265(14) 0.0352(16) 0.0236(14) 0.0046(12) 0.0134(12) -0.0014(12) C40 0.0202(13) 0.0241(14) 0.0240(13) -0.0011(11) 0.0071(11) -0.0013(11) C41 0.0240(13) 0.0211(13) 0.0285(14) -0.0033(11) 0.0132(12) -0.0018(11) C42 0.0266(13) 0.0190(13) 0.0222(13) -0.0023(11) 0.0115(11) -0.0054(11) C43 0.0309(14) 0.0288(15) 0.0249(14) 0.0063(12) 0.0154(12) 0.0007(12) C44 0.0316(15) 0.0241(14) 0.0249(13) 0.0037(11) 0.0153(12) 0.0029(11) C45 0.0253(13) 0.0220(14) 0.0263(13) 0.0037(11) 0.0122(11) -0.0023(11) C46 0.0259(14) 0.0286(15) 0.0243(13) -0.0042(11) 0.0122(12) -0.0025(11) C47 0.0277(14) 0.0237(14) 0.0278(14) -0.0018(11) 0.0117(12) 0.0025(11) C48 0.0257(14) 0.0307(15) 0.0267(14) 0.0000(12) 0.0103(12) -0.0031(12) C49 0.0384(17) 0.0271(16) 0.0373(16) 0.0021(13) 0.0093(14) 0.0102(13) C50 0.071(2) 0.0382(19) 0.063(2) -0.0070(17) 0.052(2) 0.0050(17) C51 0.0349(17) 0.047(2) 0.050(2) 0.0032(16) 0.0187(15) -0.0105(15) C52 0.0319(18) 0.084(3) 0.057(2) -0.001(2) 0.0110(17) 0.0061(18) C53 0.0415(17) 0.0304(16) 0.0328(16) -0.0005(13) 0.0126(14) -0.0088(13) C54 0.0351(18) 0.100(3) 0.0441(19) 0.038(2) 0.0266(16) 0.0210(19) O1 0.0286(10) 0.0356(11) 0.0241(9) 0.0058(8) 0.0165(8) 0.0062(8) O2 0.0402(11) 0.0277(11) 0.0490(12) -0.0083(9) 0.0326(10) -0.0066(9) O3 0.0261(9) 0.0207(9) 0.0314(10) -0.0028(8) 0.0162(8) -0.0021(7) O4 0.0256(9) 0.0260(10) 0.0229(9) -0.0010(8) 0.0075(8) 0.0024(8) O5 0.0249(9) 0.0272(10) 0.0310(10) 0.0037(8) 0.0152(8) 0.0031(8) O6 0.0254(9) 0.0337(11) 0.0268(10) -0.0064(8) 0.0136(8) -0.0020(8) O7 0.0517(13) 0.0332(11) 0.0310(11) 0.0104(9) 0.0215(10) 0.0210(10) O8 0.0503(13) 0.0385(12) 0.0516(13) -0.0217(10) 0.0392(11) -0.0127(10) O9 0.0323(10) 0.0353(11) 0.0370(11) 0.0058(9) 0.0218(9) -0.0022(9) O10 0.0314(11) 0.0399(12) 0.0416(12) -0.0016(9) 0.0215(10) 0.0044(9) O11 0.0508(12) 0.0236(10) 0.0316(10) 0.0009(8) 0.0210(10) 0.0004(9) O12 0.0284(11) 0.0637(15) 0.0340(11) 0.0224(10) 0.0186(9) 0.0137(10) 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 1.517(4) . ? C1 C21 1.525(3) . ? C2 C7 1.393(4) . ? C2 C3 1.400(4) . ? C3 C4 1.386(4) . ? C4 O7 1.370(3) . ? C4 C5 1.402(4) . ? C5 O1 1.383(3) . ? C5 C6 1.385(4) . ? C6 C7 1.400(4) . ? C7 C8 1.525(3) . ? C8 C9 1.516(3) . ? C9 C14 1.390(4) . ? C9 C10 1.396(4) . ? C10 C11 1.375(4) . ? C11 O8 1.368(3) . ? C11 C12 1.406(4) . ? C12 O3 1.375(3) . ? C12 C13 1.375(4) . ? C13 C14 1.405(4) . ? C14 C15 1.518(3) . ? C15 C16 1.526(3) . ? C16 C21 1.398(4) . ? C16 C17 1.402(4) . ? C17 C18 1.376(4) . ? C18 O9 1.389(3) . ? C18 C19 1.396(4) . ? C19 O5 1.382(3) . ? C19 C20 1.386(4) . ? C20 C21 1.400(3) . ? C22 C23 1.517(4) . ? C22 C42 1.525(4) . ? C23 C28 1.395(4) . ? C23 C24 1.399(4) . ? C24 C25 1.377(4) . ? C25 O10 1.384(3) . ? C25 C26 1.394(4) . ? C26 O2 1.377(3) . ? C26 C27 1.384(4) . ? C27 C28 1.396(4) . ? C28 C29 1.524(4) . ? C29 C30 1.512(4) . ? C30 C35 1.392(4) . ? C30 C31 1.394(4) . ? C31 C32 1.378(4) . ? C32 O11 1.375(3) . ? C32 C33 1.399(4) . ? C33 O6 1.382(3) . ? C33 C34 1.383(4) . ? C34 C35 1.404(4) . ? C35 C36 1.522(4) . ? C36 C37 1.521(4) . ? C37 C38 1.395(4) . ? C37 C42 1.403(4) . ? C38 C39 1.389(4) . ? C39 O12 1.370(3) . ? C39 C40 1.386(4) . ? C40 C41 1.383(4) . ? C40 O4 1.385(3) . ? C41 C42 1.396(4) . ? C43 O1 1.441(3) . ? C43 C44 1.498(4) . ? C44 O2 1.434(3) . ? C45 O3 1.431(3) . ? C45 C46 1.495(4) . ? C46 O4 1.449(3) . ? C47 O5 1.431(3) . ? C47 C48 1.495(4) . ? C48 O6 1.446(3) . ? C49 O7 1.418(3) . ? C50 O8 1.413(4) . ? C51 O9 1.430(4) . ? C52 O10 1.417(4) . ? C53 O11 1.422(3) . ? C54 O12 1.426(3) . ? 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 115.2(2) . . ? C7 C2 C3 118.6(2) . . ? C7 C2 C1 123.6(2) . . ? C3 C2 C1 117.8(2) . . ? C4 C3 C2 122.7(2) . . ? O7 C4 C3 123.6(2) . . ? O7 C4 C5 117.6(2) . . ? C3 C4 C5 118.8(2) . . ? O1 C5 C6 114.8(2) . . ? O1 C5 C4 126.6(2) . . ? C6 C5 C4 118.3(2) . . ? C5 C6 C7 123.2(2) . . ? C2 C7 C6 118.3(2) . . ? C2 C7 C8 124.0(2) . . ? C6 C7 C8 117.7(2) . . ? C9 C8 C7 114.5(2) . . ? C14 C9 C10 118.8(2) . . ? C14 C9 C8 123.5(2) . . ? C10 C9 C8 117.7(2) . . ? C11 C10 C9 122.0(2) . . ? O8 C11 C10 125.3(2) . . ? O8 C11 C12 115.3(2) . . ? C10 C11 C12 119.4(2) . . ? O3 C12 C13 126.1(2) . . ? O3 C12 C11 115.0(2) . . ? C13 C12 C11 118.8(2) . . ? C12 C13 C14 121.9(2) . . ? C9 C14 C13 119.0(2) . . ? C9 C14 C15 123.9(2) . . ? C13 C14 C15 117.1(2) . . ? C14 C15 C16 112.71(19) . . ? C21 C16 C17 118.5(2) . . ? C21 C16 C15 123.6(2) . . ? C17 C16 C15 117.9(2) . . ? C18 C17 C16 122.2(2) . . ? C17 C18 O9 120.4(2) . . ? C17 C18 C19 119.6(2) . . ? O9 C18 C19 119.9(2) . . ? O5 C19 C20 125.9(2) . . ? O5 C19 C18 115.4(2) . . ? C20 C19 C18 118.6(2) . . ? C19 C20 C21 122.4(2) . . ? C16 C21 C20 118.7(2) . . ? C16 C21 C1 123.3(2) . . ? C20 C21 C1 117.9(2) . . ? C23 C22 C42 115.4(2) . . ? C28 C23 C24 118.6(2) . . ? C28 C23 C22 123.2(2) . . ? C24 C23 C22 118.2(2) . . ? C25 C24 C23 122.0(3) . . ? C24 C25 O10 120.3(2) . . ? C24 C25 C26 119.1(2) . . ? O10 C25 C26 120.5(2) . . ? O2 C26 C27 123.7(2) . . ? O2 C26 C25 117.0(2) . . ? C27 C26 C25 119.2(2) . . ? C26 C27 C28 121.7(2) . . ? C23 C28 C27 118.9(2) . . ? C23 C28 C29 123.0(2) . . ? C27 C28 C29 118.0(2) . . ? C30 C29 C28 110.2(2) . . ? C35 C30 C31 119.7(2) . . ? C35 C30 C29 124.3(2) . . ? C31 C30 C29 115.7(2) . . ? C32 C31 C30 122.3(2) . . ? O11 C32 C31 123.1(2) . . ? O11 C32 C33 118.3(2) . . ? C31 C32 C33 118.5(2) . . ? O6 C33 C34 117.7(2) . . ? O6 C33 C32 123.1(2) . . ? C34 C33 C32 119.0(2) . . ? C33 C34 C35 122.7(2) . . ? C30 C35 C34 117.4(2) . . ? C30 C35 C36 123.0(2) . . ? C34 C35 C36 119.6(2) . . ? C37 C36 C35 113.2(2) . . ? C38 C37 C42 119.2(2) . . ? C38 C37 C36 117.3(2) . . ? C42 C37 C36 123.5(2) . . ? C39 C38 C37 121.5(2) . . ? O12 C39 C40 116.9(2) . . ? O12 C39 C38 124.0(2) . . ? C40 C39 C38 119.1(2) . . ? C41 C40 O4 118.8(2) . . ? C41 C40 C39 118.8(2) . . ? O4 C40 C39 122.2(2) . . ? C40 C41 C42 122.7(2) . . ? C41 C42 C37 117.5(2) . . ? C41 C42 C22 119.1(2) . . ? C37 C42 C22 123.3(2) . . ? O1 C43 C44 113.2(2) . . ? O2 C44 C43 107.5(2) . . ? O3 C45 C46 112.8(2) . . ? O4 C46 C45 108.2(2) . . ? O5 C47 C48 114.0(2) . . ? O6 C48 C47 108.0(2) . . ? C5 O1 C43 121.9(2) . . ? C26 O2 C44 116.0(2) . . ? C12 O3 C45 117.23(19) . . ? C40 O4 C46 114.11(19) . . ? C19 O5 C47 118.5(2) . . ? C33 O6 C48 116.9(2) . . ? C4 O7 C49 118.0(2) . . ? C11 O8 C50 117.7(2) . . ? C18 O9 C51 112.9(2) . . ? C25 O10 C52 113.4(2) . . ? C32 O11 C53 117.2(2) . . ? C39 O12 C54 116.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.806 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.057