data_CCDC-778902 _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 'C60 H54 O12' _chemical_formula_weight 967.03 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 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 11.8090(13) _cell_length_b 12.9971(15) _cell_length_c 17.8807(19) _cell_angle_alpha 89.531(4) _cell_angle_beta 89.764(4) _cell_angle_gamma 88.396(3) _cell_volume 2743.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.081 _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: -1 Friedel opposites are equivalent. ; _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9235 _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 42110 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9641 _reflns_number_gt 8202 _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^)+(0.0988P)^2^+0.6407P] 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 9641 _refine_ls_number_parameters 698 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 -0.15531(15) 0.37279(14) 0.31606(10) 0.0309(4) Uani 1 1 d . . . H1a H -0.1997 0.3446 0.3567 0.041 Uiso 1 1 calc R . . H1b H -0.2016 0.4254 0.2912 0.041 Uiso 1 1 calc R . . C2 C -0.05096(14) 0.42194(13) 0.34814(9) 0.0282(4) Uani 1 1 d . . . C3 C 0.00032(15) 0.49945(14) 0.30626(9) 0.0312(4) Uani 1 1 d . . . H3 H -0.0324 0.5205 0.2613 0.042 Uiso 1 1 calc R . . C4 C 0.09770(15) 0.54569(13) 0.32941(9) 0.0294(4) Uani 1 1 d . . . C5 C 0.14763(14) 0.51572(13) 0.39705(9) 0.0262(4) Uani 1 1 d . . . C6 C 0.09636(14) 0.44067(13) 0.43957(9) 0.0270(4) Uani 1 1 d . . . H6 H 0.1281 0.4218 0.4854 0.036 Uiso 1 1 calc R . . C7 C -0.00173(14) 0.39204(13) 0.41613(9) 0.0258(4) Uani 1 1 d . . . C8 C -0.04781(15) 0.30771(13) 0.46627(9) 0.0282(4) Uani 1 1 d . . . H8a H -0.0375 0.3267 0.5181 0.038 Uiso 1 1 calc R . . H8b H -0.1285 0.3027 0.4576 0.038 Uiso 1 1 calc R . . C9 C 0.00918(14) 0.20307(13) 0.45316(9) 0.0261(4) Uani 1 1 d . . . C10 C 0.10836(14) 0.17903(13) 0.49310(9) 0.0284(4) Uani 1 1 d . . . H10 H 0.1361 0.2274 0.5258 0.038 Uiso 1 1 calc R . . C11 C 0.16626(14) 0.08603(14) 0.48557(9) 0.0285(4) Uani 1 1 d . . . C12 C 0.12561(14) 0.01265(13) 0.43552(9) 0.0267(4) Uani 1 1 d . . . C13 C 0.02704(14) 0.03563(13) 0.39698(9) 0.0268(4) Uani 1 1 d . . . H13 H -0.0008 -0.0132 0.3646 0.036 Uiso 1 1 calc R . . C14 C -0.03276(14) 0.12966(13) 0.40465(9) 0.0260(4) Uani 1 1 d . . . C15 C -0.14041(14) 0.14452(14) 0.35932(9) 0.0285(4) Uani 1 1 d . . . H15a H -0.1783 0.0794 0.3569 0.038 Uiso 1 1 calc R . . H15b H -0.1906 0.1930 0.3850 0.038 Uiso 1 1 calc R . . C16 C -0.12057(13) 0.18359(14) 0.28022(9) 0.0276(4) Uani 1 1 d . . . C17 C -0.09514(15) 0.11103(14) 0.22449(10) 0.0306(4) Uani 1 1 d . . . H17 H -0.0930 0.0414 0.2370 0.041 Uiso 1 1 calc R . . C18 C -0.07313(15) 0.14051(15) 0.15118(10) 0.0327(4) Uani 1 1 d . . . C19 C -0.07605(15) 0.24513(15) 0.13276(10) 0.0334(4) Uani 1 1 d . . . C20 C -0.10360(15) 0.31648(14) 0.18682(10) 0.0325(4) Uani 1 1 d . . . H20 H -0.1072 0.3859 0.1737 0.043 Uiso 1 1 calc R . . C21 C -0.12639(14) 0.28795(14) 0.26090(10) 0.0295(4) Uani 1 1 d . . . C22 C 0.51120(16) 0.13845(14) 0.08252(10) 0.0344(4) Uani 1 1 d . A . H22a H 0.5905 0.1477 0.0940 0.046 Uiso 1 1 calc R . . H22b H 0.5070 0.1105 0.0325 0.046 Uiso 1 1 calc R . . C23 C 0.44958(16) 0.24229(15) 0.08400(9) 0.0336(4) Uani 1 1 d . . . C24 C 0.3643(7) 0.2573(8) 0.0368(5) 0.0300(15) Uani 0.55 1 d PU A 1 H24 H 0.3454 0.2037 0.0055 0.040 Uiso 0.55 1 calc PR A 1 C25 C 0.3042(6) 0.3457(7) 0.0319(4) 0.0314(14) Uani 0.55 1 d PU A 1 C24' C 0.3327(9) 0.2521(11) 0.0515(6) 0.0329(19) Uani 0.45 1 d PU A 2 H24' H 0.2985 0.1944 0.0324 0.044 Uiso 0.45 1 calc PR A 2 C25' C 0.2730(7) 0.3509(8) 0.0498(5) 0.0309(16) Uani 0.45 1 d PU A 2 C26 C 0.33235(17) 0.43322(15) 0.07571(10) 0.0362(4) Uani 1 1 d . . . C27 C 0.42794(16) 0.42033(15) 0.11893(10) 0.0344(4) Uani 1 1 d . A . H27 H 0.4540 0.4764 0.1451 0.046 Uiso 1 1 calc R . . C28 C 0.48717(15) 0.32642(14) 0.12490(9) 0.0307(4) Uani 1 1 d . A . C29 C 0.58908(15) 0.32110(15) 0.17642(10) 0.0339(4) Uani 1 1 d . . . H29a H 0.6429 0.2698 0.1575 0.045 Uiso 1 1 calc R A . H29b H 0.6256 0.3870 0.1750 0.045 Uiso 1 1 calc R . . C30 C 0.56100(14) 0.29476(14) 0.25702(10) 0.0303(4) Uani 1 1 d . A . C31 C 0.51980(14) 0.37388(14) 0.30341(10) 0.0311(4) Uani 1 1 d . . . H31 H 0.5059 0.4388 0.2827 0.041 Uiso 1 1 calc R A . C32 C 0.49909(14) 0.35899(14) 0.37885(10) 0.0295(4) Uani 1 1 d . A . C33 C 0.52442(14) 0.26297(14) 0.41098(9) 0.0299(4) Uani 1 1 d . . . C34 C 0.55876(14) 0.18228(14) 0.36479(10) 0.0311(4) Uani 1 1 d . A . H34 H 0.5710 0.1172 0.3857 0.041 Uiso 1 1 calc R . . C35 C 0.57544(14) 0.19598(14) 0.28803(10) 0.0304(4) Uani 1 1 d . . . C36 C 0.60532(15) 0.10201(14) 0.24163(10) 0.0318(4) Uani 1 1 d . A . H36a H 0.6486 0.0532 0.2721 0.042 Uiso 1 1 calc R . . H36b H 0.6530 0.1224 0.2001 0.042 Uiso 1 1 calc R . . C37 C 0.50185(14) 0.04930(13) 0.21115(9) 0.0271(4) Uani 1 1 d . . . C38 C 0.44226(14) -0.01555(13) 0.25924(9) 0.0286(4) Uani 1 1 d . A . H38 H 0.4659 -0.0224 0.3086 0.038 Uiso 1 1 calc R . . C39 C 0.35035(14) -0.06946(13) 0.23655(9) 0.0283(4) Uani 1 1 d . . . C40 C 0.31666(14) -0.06349(14) 0.16154(9) 0.0301(4) Uani 1 1 d . A . C41 C 0.37170(15) 0.00346(14) 0.11412(9) 0.0304(4) Uani 1 1 d . . . H41 H 0.3476 0.0099 0.0648 0.040 Uiso 1 1 calc R A . C42 C 0.46241(14) 0.06176(14) 0.13792(9) 0.0289(4) Uani 1 1 d . A . O1 O 0.15020(12) 0.62385(10) 0.29060(7) 0.0391(3) Uani 1 1 d . . . C43 C 0.14702(17) 0.62069(17) 0.21118(10) 0.0405(5) Uani 1 1 d . . . H43a H 0.1553 0.5496 0.1955 0.054 Uiso 1 1 calc R . . H43b H 0.2111 0.6574 0.1914 0.054 Uiso 1 1 calc R . . C44 C 0.04327(18) 0.66520(16) 0.17888(10) 0.0397(5) Uani 1 1 d . . . C45 C -0.0394(2) 0.70071(19) 0.15082(12) 0.0499(5) Uani 1 1 d . . . H45 H -0.1045 0.7287 0.1287 0.066 Uiso 1 1 calc R . . O2 O 0.24404(10) 0.56590(9) 0.41594(7) 0.0311(3) Uani 1 1 d . . . C46 C 0.30583(15) 0.52967(14) 0.48016(9) 0.0314(4) Uani 1 1 d . . . H46a H 0.2536 0.5231 0.5219 0.042 Uiso 1 1 calc R . . H46b H 0.3607 0.5805 0.4934 0.042 Uiso 1 1 calc R . . C47 C 0.36710(15) 0.42753(15) 0.46854(10) 0.0338(4) Uani 1 1 d . A . H47a H 0.3928 0.3996 0.5162 0.045 Uiso 1 1 calc R . . H47b H 0.3163 0.3790 0.4464 0.045 Uiso 1 1 calc R . . O3 O 0.46220(10) 0.44302(9) 0.41995(7) 0.0330(3) Uani 1 1 d . . . O4 O 0.26126(11) 0.05559(10) 0.52556(7) 0.0358(3) Uani 1 1 d . . . C48 C 0.30214(17) 0.12687(16) 0.57895(11) 0.0402(5) Uani 1 1 d . . . H48a H 0.3142 0.1922 0.5540 0.053 Uiso 1 1 calc R . . H48b H 0.3748 0.1015 0.5975 0.053 Uiso 1 1 calc R . . C49 C 0.22600(19) 0.14398(16) 0.64221(11) 0.0438(5) Uani 1 1 d . . . C50 C 0.1667(3) 0.1623(2) 0.69445(13) 0.0606(7) Uani 1 1 d . . . H50 H 0.1203 0.1767 0.7354 0.081 Uiso 1 1 calc R . . O5 O 0.18758(10) -0.07791(9) 0.43103(6) 0.0310(3) Uani 1 1 d . . . C51 C 0.15232(15) -0.15185(13) 0.37727(9) 0.0292(4) Uani 1 1 d . A . H51a H 0.0713 -0.1606 0.3821 0.039 Uiso 1 1 calc R . . H51b H 0.1897 -0.2177 0.3880 0.039 Uiso 1 1 calc R . . C52 C 0.17943(14) -0.12003(14) 0.29797(9) 0.0305(4) Uani 1 1 d . . . H52a H 0.1389 -0.1619 0.2629 0.041 Uiso 1 1 calc R A . H52b H 0.1571 -0.0485 0.2897 0.041 Uiso 1 1 calc R . . O6 O 0.29996(10) -0.13433(10) 0.28761(6) 0.0325(3) Uani 1 1 d . A . O7 O -0.04750(12) 0.07487(11) 0.09244(7) 0.0411(3) Uani 1 1 d . . . C53 C -0.06278(18) -0.03235(15) 0.10378(11) 0.0405(5) Uani 1 1 d . . . H53a H -0.0203 -0.0549 0.1475 0.054 Uiso 1 1 calc R . . H53b H -0.0323 -0.0695 0.0610 0.054 Uiso 1 1 calc R . . C54 C -0.18174(18) -0.05827(15) 0.11403(11) 0.0391(5) Uani 1 1 d . . . C55 C -0.2769(2) -0.08182(17) 0.12235(13) 0.0515(6) Uani 1 1 d . . . H55 H -0.3518 -0.1004 0.1289 0.068 Uiso 1 1 calc R . . O8 O -0.05446(12) 0.27286(11) 0.05926(7) 0.0437(3) Uani 1 1 d . . . C56 C 0.0640(3) 0.2650(3) 0.0402(2) 0.0429(8) Uani 0.55 1 d P A 1 H56a H 0.0751 0.2172 -0.0007 0.057 Uiso 0.55 1 calc PR A 1 H56b H 0.1066 0.2387 0.0829 0.057 Uiso 0.55 1 calc PR A 1 C57 C 0.1067(5) 0.3675(3) 0.0179(3) 0.0383(10) Uani 0.55 1 d P A 1 H57a H 0.0526 0.4016 -0.0153 0.051 Uiso 0.55 1 calc PR A 1 H57b H 0.1140 0.4098 0.0620 0.051 Uiso 0.55 1 calc PR A 1 O9 O 0.2140(3) 0.3578(2) -0.01883(17) 0.0394(7) Uani 0.55 1 d P A 1 C56' C -0.0320(4) 0.3698(4) 0.0374(2) 0.0391(10) Uani 0.45 1 d P A 2 H56a' H -0.0904 0.4164 0.0570 0.052 Uiso 0.45 1 calc PR A 2 H56b' H -0.0345 0.3740 -0.0167 0.052 Uiso 0.45 1 calc PR A 2 C57' C 0.0807(4) 0.4034(4) 0.0634(3) 0.0384(10) Uani 0.45 1 d P A 2 H57a' H 0.0848 0.4777 0.0594 0.051 Uiso 0.45 1 calc PR A 2 H57b' H 0.0916 0.3839 0.1154 0.051 Uiso 0.45 1 calc PR A 2 O9' O 0.1699(4) 0.3541(3) 0.0167(2) 0.0380(9) Uani 0.45 1 d P A 2 O10 O 0.27835(12) 0.52905(11) 0.06941(7) 0.0426(3) Uani 1 1 d . A . C58 C 0.3068(3) 0.5821(2) 0.00402(16) 0.0834(10) Uani 1 1 d . . . H58a H 0.3854 0.5988 0.0053 0.125 Uiso 1 1 calc R A . H58b H 0.2614 0.6443 0.0003 0.125 Uiso 1 1 calc R . . H58c H 0.2931 0.5396 -0.0385 0.125 Uiso 1 1 calc R . . O11 O 0.51517(11) 0.25360(10) 0.48769(7) 0.0351(3) Uani 1 1 d . A . C59 C 0.5784(2) 0.17100(19) 0.52112(11) 0.0510(6) Uani 1 1 d . . . H59a H 0.5454 0.1069 0.5082 0.077 Uiso 1 1 calc R A . H59b H 0.5775 0.1785 0.5745 0.077 Uiso 1 1 calc R . . H59c H 0.6552 0.1717 0.5033 0.077 Uiso 1 1 calc R . . O12 O 0.23134(11) -0.12657(11) 0.14030(7) 0.0374(3) Uani 1 1 d . . . C60 C 0.20832(18) -0.13149(19) 0.06222(11) 0.0468(5) Uani 1 1 d . A . H60a H 0.1818 -0.0652 0.0446 0.070 Uiso 1 1 calc R . . H60b H 0.1514 -0.1813 0.0536 0.070 Uiso 1 1 calc R . . H60c H 0.2764 -0.1513 0.0358 0.070 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 C1 0.0267(9) 0.0284(9) 0.0377(9) 0.0019(7) -0.0080(7) 0.0003(7) C2 0.0264(9) 0.0246(9) 0.0335(9) -0.0017(7) -0.0046(7) 0.0013(7) C3 0.0353(10) 0.0275(9) 0.0308(9) 0.0012(7) -0.0106(7) -0.0002(7) C4 0.0342(9) 0.0231(9) 0.0309(8) 0.0006(7) -0.0022(7) -0.0013(7) C5 0.0258(8) 0.0226(9) 0.0301(8) -0.0049(7) -0.0024(6) 0.0000(7) C6 0.0284(9) 0.0264(9) 0.0258(8) -0.0036(7) -0.0034(6) 0.0039(7) C7 0.0260(8) 0.0232(9) 0.0281(8) -0.0027(7) 0.0002(6) 0.0032(7) C8 0.0278(9) 0.0273(9) 0.0296(8) -0.0010(7) 0.0009(7) 0.0003(7) C9 0.0264(9) 0.0249(9) 0.0270(8) 0.0038(7) 0.0040(6) -0.0033(7) C10 0.0310(9) 0.0279(9) 0.0264(8) 0.0012(7) -0.0016(7) -0.0030(7) C11 0.0263(9) 0.0326(10) 0.0265(8) 0.0038(7) -0.0034(6) -0.0020(7) C12 0.0290(9) 0.0244(9) 0.0265(8) 0.0021(7) 0.0018(6) 0.0007(7) C13 0.0296(9) 0.0262(9) 0.0248(8) 0.0001(7) 0.0001(6) -0.0030(7) C14 0.0250(8) 0.0270(9) 0.0261(8) 0.0043(7) 0.0025(6) -0.0023(7) C15 0.0238(8) 0.0260(9) 0.0360(9) 0.0007(7) -0.0021(7) -0.0032(7) C16 0.0197(8) 0.0290(9) 0.0344(9) 0.0023(7) -0.0059(6) -0.0034(7) C17 0.0287(9) 0.0266(9) 0.0366(9) 0.0020(7) -0.0072(7) -0.0029(7) C18 0.0308(9) 0.0340(10) 0.0335(9) -0.0018(8) -0.0041(7) -0.0043(8) C19 0.0304(9) 0.0369(11) 0.0331(9) 0.0067(8) -0.0075(7) -0.0055(8) C20 0.0319(10) 0.0265(9) 0.0394(10) 0.0046(7) -0.0117(7) -0.0051(7) C21 0.0215(8) 0.0307(10) 0.0365(9) 0.0023(7) -0.0081(7) -0.0030(7) C22 0.0407(10) 0.0347(10) 0.0279(8) -0.0031(7) 0.0053(7) -0.0055(8) C23 0.0425(11) 0.0324(10) 0.0262(8) 0.0029(7) 0.0019(7) -0.0073(8) C24 0.037(4) 0.027(2) 0.027(3) 0.002(2) 0.001(2) -0.013(3) C25 0.023(4) 0.043(3) 0.028(3) -0.003(2) 0.002(2) -0.001(3) C24' 0.035(5) 0.033(3) 0.031(5) 0.011(3) -0.005(3) -0.013(4) C25' 0.021(4) 0.036(3) 0.035(5) 0.007(3) -0.001(3) 0.004(3) C26 0.0419(11) 0.0313(10) 0.0354(9) 0.0056(8) -0.0004(8) -0.0022(8) C27 0.0372(10) 0.0326(10) 0.0337(9) -0.0013(8) 0.0033(7) -0.0082(8) C28 0.0320(9) 0.0329(10) 0.0276(8) 0.0022(7) 0.0053(7) -0.0078(7) C29 0.0300(9) 0.0312(10) 0.0409(10) 0.0003(8) 0.0015(7) -0.0075(8) C30 0.0212(8) 0.0339(10) 0.0362(9) -0.0021(7) -0.0039(7) -0.0056(7) C31 0.0268(9) 0.0283(9) 0.0384(9) 0.0004(7) -0.0073(7) -0.0039(7) C32 0.0220(8) 0.0298(10) 0.0369(9) -0.0045(7) -0.0061(7) -0.0016(7) C33 0.0240(8) 0.0316(10) 0.0341(9) -0.0028(7) -0.0061(7) -0.0007(7) C34 0.0268(9) 0.0289(9) 0.0377(9) -0.0014(7) -0.0073(7) 0.0017(7) C35 0.0205(8) 0.0332(10) 0.0376(9) -0.0037(8) -0.0042(7) -0.0010(7) C36 0.0266(9) 0.0325(10) 0.0363(9) -0.0026(7) -0.0025(7) 0.0020(7) C37 0.0252(8) 0.0255(9) 0.0303(8) -0.0040(7) -0.0008(6) 0.0045(7) C38 0.0290(9) 0.0295(9) 0.0272(8) -0.0009(7) -0.0038(7) 0.0034(7) C39 0.0288(9) 0.0266(9) 0.0293(8) 0.0011(7) 0.0025(7) 0.0026(7) C40 0.0275(9) 0.0305(10) 0.0325(9) -0.0044(7) -0.0030(7) -0.0018(7) C41 0.0331(9) 0.0331(10) 0.0248(8) -0.0012(7) -0.0013(7) 0.0010(8) C42 0.0287(9) 0.0287(9) 0.0291(8) -0.0030(7) 0.0037(7) 0.0031(7) O1 0.0481(8) 0.0368(8) 0.0331(7) 0.0072(5) -0.0107(6) -0.0157(6) C43 0.0392(11) 0.0483(12) 0.0339(9) 0.0027(8) 0.0011(8) -0.0037(9) C44 0.0464(12) 0.0415(11) 0.0316(9) 0.0043(8) -0.0015(8) -0.0105(9) C45 0.0484(13) 0.0516(14) 0.0499(12) 0.0109(10) -0.0087(10) -0.0040(11) O2 0.0288(6) 0.0281(7) 0.0366(6) -0.0003(5) -0.0090(5) -0.0032(5) C46 0.0296(9) 0.0322(10) 0.0324(9) -0.0046(7) -0.0081(7) 0.0015(7) C47 0.0305(9) 0.0347(10) 0.0360(9) 0.0002(8) -0.0023(7) 0.0022(8) O3 0.0321(7) 0.0286(7) 0.0384(7) -0.0060(5) -0.0014(5) -0.0010(5) O4 0.0355(7) 0.0340(7) 0.0376(7) -0.0011(5) -0.0128(5) 0.0033(6) C48 0.0411(11) 0.0350(11) 0.0450(11) 0.0008(8) -0.0156(8) -0.0067(9) C49 0.0595(13) 0.0360(11) 0.0367(11) 0.0012(8) -0.0168(10) -0.0120(10) C50 0.0905(19) 0.0533(15) 0.0391(12) -0.0054(10) -0.0016(12) -0.0195(13) O5 0.0334(7) 0.0286(7) 0.0309(6) -0.0008(5) -0.0028(5) 0.0051(5) C51 0.0325(9) 0.0241(9) 0.0309(8) -0.0020(7) 0.0011(7) -0.0016(7) C52 0.0291(9) 0.0313(10) 0.0312(9) -0.0007(7) 0.0010(7) -0.0016(7) O6 0.0303(7) 0.0328(7) 0.0342(6) 0.0074(5) 0.0037(5) 0.0007(5) O7 0.0507(8) 0.0356(8) 0.0371(7) -0.0022(6) 0.0015(6) -0.0061(6) C53 0.0456(11) 0.0324(11) 0.0433(10) -0.0027(8) -0.0016(8) 0.0034(9) C54 0.0465(12) 0.0316(10) 0.0390(10) -0.0053(8) -0.0016(8) 0.0010(9) C55 0.0488(14) 0.0429(13) 0.0630(14) -0.0155(11) 0.0035(10) -0.0029(10) O8 0.0499(8) 0.0472(9) 0.0342(7) 0.0103(6) -0.0057(6) -0.0075(7) C56 0.048(2) 0.041(2) 0.0394(18) 0.0028(16) 0.0039(15) 0.0019(17) C57 0.039(3) 0.035(2) 0.041(3) -0.0024(18) -0.002(2) -0.002(2) O9 0.0342(16) 0.0520(17) 0.0317(14) 0.0026(13) -0.0009(12) 0.0006(13) C56' 0.044(2) 0.038(2) 0.036(2) 0.0065(18) -0.0059(18) -0.0041(19) C57' 0.035(2) 0.039(2) 0.041(2) -0.004(2) -0.0039(19) -0.0006(19) O9' 0.032(2) 0.045(2) 0.037(2) -0.0030(16) -0.007(2) 0.005(2) O10 0.0464(8) 0.0354(8) 0.0458(8) 0.0062(6) 0.0019(6) 0.0010(6) C58 0.132(3) 0.0485(16) 0.0670(17) 0.0268(13) 0.0303(17) 0.0260(17) O11 0.0368(7) 0.0368(7) 0.0314(6) 0.0002(5) -0.0059(5) 0.0076(6) C59 0.0557(13) 0.0567(14) 0.0392(11) 0.0076(10) -0.0029(9) 0.0228(11) O12 0.0387(7) 0.0443(8) 0.0300(6) -0.0037(6) -0.0027(5) -0.0129(6) C60 0.0445(12) 0.0627(14) 0.0343(10) -0.0093(9) -0.0036(8) -0.0171(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 C21 1.516(2) . ? C1 C2 1.520(2) . ? C2 C7 1.397(2) . ? C2 C3 1.400(3) . ? C3 C4 1.379(3) . ? C4 O1 1.385(2) . ? C4 C5 1.395(2) . ? C5 O2 1.372(2) . ? C5 C6 1.383(2) . ? C6 C7 1.402(2) . ? C7 C8 1.521(2) . ? C8 C9 1.520(2) . ? C9 C14 1.397(2) . ? C9 C10 1.401(2) . ? C10 C11 1.379(2) . ? C11 O4 1.380(2) . ? C11 C12 1.409(2) . ? C12 O5 1.371(2) . ? C12 C13 1.379(2) . ? C13 C14 1.402(2) . ? C14 C15 1.517(2) . ? C15 C16 1.518(2) . ? C16 C21 1.397(3) . ? C16 C17 1.404(2) . ? C17 C18 1.388(3) . ? C18 O7 1.386(2) . ? C18 C19 1.396(3) . ? C19 C20 1.377(3) . ? C19 O8 1.384(2) . ? C20 C21 1.400(3) . ? C22 C23 1.516(3) . ? C22 C42 1.522(2) . ? C23 C24 1.326(11) . ? C23 C28 1.404(3) . ? C23 C24' 1.501(13) . ? C24 C25 1.336(15) . ? C25 O9 1.407(9) . ? C25 C26 1.433(9) . ? C24' C25' 1.447(18) . ? C25' O9' 1.355(11) . ? C25' C26 1.379(12) . ? C26 C27 1.376(3) . ? C26 O10 1.387(2) . ? C27 C28 1.393(3) . ? C28 C29 1.518(3) . ? C29 C30 1.516(2) . ? C30 C35 1.401(3) . ? C30 C31 1.402(2) . ? C31 C32 1.383(3) . ? C32 O3 1.381(2) . ? C32 C33 1.395(3) . ? C33 O11 1.380(2) . ? C33 C34 1.391(2) . ? C34 C35 1.396(3) . ? C35 C36 1.515(2) . ? C36 C37 1.522(2) . ? C37 C42 1.398(2) . ? C37 C38 1.400(2) . ? C38 C39 1.373(2) . ? C39 O6 1.382(2) . ? C39 C40 1.402(2) . ? C40 O12 1.373(2) . ? C40 C41 1.383(3) . ? C41 C42 1.399(3) . ? O1 C43 1.422(2) . ? C43 C44 1.459(3) . ? C44 C45 1.180(3) . ? O2 C46 1.432(2) . ? C46 C47 1.509(2) . ? C47 O3 1.435(2) . ? O4 C48 1.430(2) . ? C48 C49 1.457(3) . ? C49 C50 1.186(3) . ? O5 C51 1.436(2) . ? C51 C52 1.509(2) . ? C52 O6 1.442(2) . ? O7 C53 1.423(2) . ? C53 C54 1.464(3) . ? C54 C55 1.182(3) . ? O8 C56' 1.349(5) . ? O8 C56 1.440(4) . ? C56 C57 1.488(6) . ? C57 O9 1.428(5) . ? C56' C57' 1.490(6) . ? C57' O9' 1.477(6) . ? O10 C58 1.397(3) . ? O11 C59 1.420(2) . ? O12 C60 1.426(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 C21 C1 C2 112.87(14) . . ? C7 C2 C3 118.26(16) . . ? C7 C2 C1 123.57(16) . . ? C3 C2 C1 118.14(15) . . ? C4 C3 C2 122.30(16) . . ? C3 C4 O1 124.33(16) . . ? C3 C4 C5 119.70(16) . . ? O1 C4 C5 115.96(15) . . ? O2 C5 C6 125.66(15) . . ? O2 C5 C4 115.88(15) . . ? C6 C5 C4 118.46(15) . . ? C5 C6 C7 122.37(16) . . ? C2 C7 C6 118.90(16) . . ? C2 C7 C8 123.50(15) . . ? C6 C7 C8 117.60(15) . . ? C9 C8 C7 113.16(13) . . ? C14 C9 C10 118.62(15) . . ? C14 C9 C8 123.70(15) . . ? C10 C9 C8 117.67(15) . . ? C11 C10 C9 122.26(16) . . ? C10 C11 O4 125.24(15) . . ? C10 C11 C12 119.31(16) . . ? O4 C11 C12 115.41(15) . . ? O5 C12 C13 125.52(15) . . ? O5 C12 C11 115.99(15) . . ? C13 C12 C11 118.47(15) . . ? C12 C13 C14 122.60(15) . . ? C9 C14 C13 118.72(15) . . ? C9 C14 C15 124.17(15) . . ? C13 C14 C15 117.11(15) . . ? C16 C15 C14 113.83(14) . . ? C21 C16 C17 119.01(16) . . ? C21 C16 C15 122.91(15) . . ? C17 C16 C15 118.08(16) . . ? C18 C17 C16 121.69(17) . . ? O7 C18 C17 125.92(17) . . ? O7 C18 C19 115.14(16) . . ? C17 C18 C19 118.93(16) . . ? C20 C19 O8 122.36(17) . . ? C20 C19 C18 119.60(16) . . ? O8 C19 C18 118.01(16) . . ? C19 C20 C21 122.13(17) . . ? C16 C21 C20 118.60(16) . . ? C16 C21 C1 123.57(16) . . ? C20 C21 C1 117.83(16) . . ? C23 C22 C42 112.79(14) . . ? C24 C23 C28 118.6(5) . . ? C28 C23 C24' 116.7(6) . . ? C24 C23 C22 117.4(5) . . ? C28 C23 C22 123.45(17) . . ? C24' C23 C22 119.0(6) . . ? C23 C24 C25 123.2(9) . . ? C24 C25 O9 121.1(8) . . ? C24 C25 C26 121.3(8) . . ? O9 C25 C26 117.5(6) . . ? C25' C24' C23 120.4(10) . . ? O9' C25' C26 127.1(8) . . ? O9' C25' C24' 116.7(10) . . ? C26 C25' C24' 115.9(8) . . ? C27 C26 C25' 122.2(4) . . ? C27 C26 O10 120.45(17) . . ? C25' C26 O10 116.1(4) . . ? C27 C26 C25 115.1(4) . . ? O10 C26 C25 124.0(4) . . ? C26 C27 C28 122.48(17) . . ? C27 C28 C23 118.85(17) . . ? C27 C28 C29 117.48(16) . . ? C23 C28 C29 123.67(17) . . ? C30 C29 C28 114.21(14) . . ? C35 C30 C31 118.13(16) . . ? C35 C30 C29 123.63(15) . . ? C31 C30 C29 118.24(17) . . ? C32 C31 C30 122.48(17) . . ? O3 C32 C31 117.75(16) . . ? O3 C32 C33 123.00(16) . . ? C31 C32 C33 119.05(16) . . ? O11 C33 C34 123.37(17) . . ? O11 C33 C32 117.77(15) . . ? C34 C33 C32 118.85(16) . . ? C33 C34 C35 122.05(18) . . ? C34 C35 C30 118.98(16) . . ? C34 C35 C36 118.08(17) . . ? C30 C35 C36 122.91(16) . . ? C35 C36 C37 113.14(14) . . ? C42 C37 C38 117.84(16) . . ? C42 C37 C36 123.97(16) . . ? C38 C37 C36 118.19(15) . . ? C39 C38 C37 122.75(16) . . ? C38 C39 O6 118.26(15) . . ? C38 C39 C40 119.29(16) . . ? O6 C39 C40 122.25(16) . . ? O12 C40 C41 124.66(16) . . ? O12 C40 C39 116.82(16) . . ? C41 C40 C39 118.51(16) . . ? C40 C41 C42 122.15(16) . . ? C37 C42 C41 119.14(16) . . ? C37 C42 C22 123.23(16) . . ? C41 C42 C22 117.60(15) . . ? C4 O1 C43 117.32(14) . . ? O1 C43 C44 114.00(16) . . ? C45 C44 C43 178.2(2) . . ? C5 O2 C46 117.94(14) . . ? O2 C46 C47 113.70(13) . . ? O3 C47 C46 108.68(15) . . ? C32 O3 C47 116.29(14) . . ? C11 O4 C48 116.79(14) . . ? O4 C48 C49 113.79(17) . . ? C50 C49 C48 176.7(2) . . ? C12 O5 C51 117.36(13) . . ? O5 C51 C52 112.46(14) . . ? O6 C52 C51 107.36(14) . . ? C39 O6 C52 116.35(13) . . ? C18 O7 C53 118.00(14) . . ? O7 C53 C54 112.95(16) . . ? C55 C54 C53 178.3(2) . . ? C56' O8 C19 123.5(2) . . ? C56' O8 C56 77.6(3) . . ? C19 O8 C56 112.81(19) . . ? O8 C56 C57 110.5(4) . . ? O9 C57 C56 111.2(4) . . ? C25 O9 C57 112.4(4) . . ? O8 C56' C57' 112.6(4) . . ? O9' C57' C56' 109.0(4) . . ? C25' O9' C57' 113.2(5) . . ? C26 O10 C58 113.28(16) . . ? C33 O11 C59 116.07(14) . . ? C40 O12 C60 116.72(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.265 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.228 0.238 0.272 86.3 8.3 2 0.415 0.342 0.760 156.0 22.8 3 0.585 0.658 0.240 156.1 22.8 4 0.771 0.762 0.728 86.4 8.4