_publ_contact_author T.Hanna _publ_contact_author_email T.Hanna@tcu.edu _publ_author_name ' Tracy A.Hanna, Lihua Liu, Alfredo M.Angeles-Boza, Xiaodi Kou, C.David Gutsche, Krzystof Ejsmont, Lev N. Zakharov, Christofer D. Incarvito, A.L.Rheingold ' _journal_name_full Journal of American Chemical Society data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H33 Li O7' _chemical_formula_weight 524.51 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' 'Li' 'Li' -0.0003 0.0001 '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 P2(1)/c 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 10.7535(5) _cell_length_b 14.7011(7) _cell_length_c 18.2911(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.9860(10) _cell_angle_gamma 90.00 _cell_volume 2765.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min O.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.088 _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 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14288 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4863 _reflns_number_gt 3698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0457P)^2^+0.1736P] 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 SHELXL _refine_ls_extinction_coef 0.0022(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4863 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.1456(2) 0.14300(17) 1.10416(13) 0.0370(5) Uani 1 1 d . . . O1 O 0.18024(8) 0.20434(6) 1.01923(5) 0.0284(2) Uani 1 1 d . . . O2 O 0.00227(9) 0.13397(6) 0.91005(5) 0.0344(2) Uani 1 1 d . . . O3 O 0.15582(10) -0.01321(6) 0.87557(6) 0.0344(2) Uani 1 1 d . . . O4 O 0.32711(9) 0.09343(7) 0.97796(5) 0.0342(2) Uani 1 1 d . . . O5 O 0.13230(12) 0.01969(8) 1.06338(6) 0.0434(3) Uani 1 1 d . . . O6 O -0.01961(11) 0.17023(9) 1.12075(8) 0.0510(3) Uani 1 1 d . . . O7 O 0.29170(11) 0.14546(8) 1.19708(6) 0.0547(3) Uani 1 1 d . . . C1 C 0.20918(12) 0.29087(9) 1.00537(7) 0.0270(3) Uani 1 1 d . . . C2 C 0.10891(13) 0.35250(9) 0.97014(7) 0.0296(3) Uani 1 1 d . . . C3 C 0.14143(15) 0.44173(10) 0.95831(8) 0.0391(4) Uani 1 1 d . . . C4 C 0.27013(15) 0.47033(11) 0.97983(10) 0.0463(4) Uani 1 1 d . . . C5 C 0.36794(15) 0.40911(10) 1.01378(9) 0.0404(4) Uani 1 1 d . . . C6 C 0.33981(12) 0.31962(9) 1.02704(7) 0.0302(3) Uani 1 1 d . . . C7 C -0.03303(13) 0.32308(11) 0.94781(8) 0.0315(3) Uani 1 1 d . . . C8 C -0.06323(12) 0.19154(9) 0.85314(7) 0.0278(3) Uani 1 1 d . . . C9 C -0.08552(12) 0.28262(9) 0.86792(7) 0.0288(3) Uani 1 1 d . . . C10 C -0.16071(13) 0.33502(11) 0.80769(8) 0.0355(3) Uani 1 1 d . . . C11 C -0.21314(14) 0.29825(11) 0.73548(8) 0.0387(4) Uani 1 1 d . . . C12 C -0.18743(13) 0.20867(11) 0.72192(8) 0.0362(3) Uani 1 1 d . . . C13 C -0.11038(12) 0.15379(9) 0.77975(7) 0.0302(3) Uani 1 1 d . . . C14 C -0.07105(13) 0.05868(10) 0.76314(8) 0.0335(3) Uani 1 1 d . . . C15 C 0.17397(13) 0.02762(9) 0.81109(7) 0.0293(3) Uani 1 1 d . . . C16 C 0.06527(13) 0.05902(9) 0.75401(7) 0.0302(3) Uani 1 1 d . . . C17 C 0.08542(15) 0.09493(10) 0.68805(8) 0.0357(3) Uani 1 1 d . . . C18 C 0.20848(16) 0.10076(11) 0.67916(9) 0.0426(4) Uani 1 1 d . . . C19 C 0.31499(15) 0.07155(10) 0.73714(8) 0.0399(4) Uani 1 1 d . . . C20 C 0.29976(13) 0.03437(9) 0.80411(7) 0.0320(3) Uani 1 1 d . . . C21 C 0.41789(14) 0.00361(10) 0.86766(9) 0.0364(3) Uani 1 1 d . . . C22 C 0.43946(12) 0.12745(9) 0.96751(7) 0.0296(3) Uani 1 1 d . . . C23 C 0.48948(13) 0.08276(10) 0.91448(8) 0.0335(3) Uani 1 1 d . . . C24 C 0.60523(14) 0.11465(12) 0.90429(9) 0.0432(4) Uani 1 1 d . . . C25 C 0.67107(16) 0.18681(12) 0.94637(10) 0.0501(4) Uani 1 1 d . . . C26 C 0.61995(14) 0.23036(11) 0.99821(9) 0.0411(4) Uani 1 1 d . . . C27 C 0.50324(12) 0.20237(10) 1.00951(7) 0.0310(3) Uani 1 1 d . . . C28 C 0.44782(13) 0.25310(10) 1.06531(8) 0.0329(3) Uani 1 1 d . . . C29 C 0.32643(17) 0.16268(12) 1.26502(9) 0.0523(4) Uani 1 1 d . . . C30 C 0.2370(3) 0.19799(19) 1.30618(13) 0.0686(6) Uani 1 1 d . . . C31 C 0.4642(3) 0.1488(5) 1.30981(19) 0.1387(17) Uani 1 1 d . . . H3 H 0.0683(15) 0.4853(11) 0.9323(9) 0.053(5) Uiso 1 1 d . . . H4 H 0.2928(15) 0.5326(12) 0.9716(9) 0.057(5) Uiso 1 1 d . . . H5 H 0.4610(14) 0.4295(10) 1.0308(8) 0.042(4) Uiso 1 1 d . . . H10 H -0.1773(13) 0.3980(11) 0.8187(8) 0.041(4) Uiso 1 1 d . . . H11 H -0.2678(14) 0.3366(11) 0.6941(9) 0.044(4) Uiso 1 1 d . . . H12 H -0.2222(13) 0.1809(10) 0.6704(9) 0.040(4) Uiso 1 1 d . . . H17 H 0.0074(14) 0.1172(10) 0.6480(9) 0.044(4) Uiso 1 1 d . . . H18 H 0.2201(14) 0.1245(11) 0.6333(9) 0.051(4) Uiso 1 1 d . . . H19 H 0.4052(15) 0.0758(10) 0.7312(9) 0.048(4) Uiso 1 1 d . . . H24 H 0.6406(13) 0.0833(10) 0.8647(8) 0.041(4) Uiso 1 1 d . . . H25 H 0.7550(18) 0.2103(12) 0.9407(10) 0.068(5) Uiso 1 1 d . . . H26 H 0.6666(15) 0.2833(11) 1.0293(9) 0.048(4) Uiso 1 1 d . . . H2A H 0.0608(18) 0.1639(12) 0.9488(11) 0.069(6) Uiso 1 1 d . . . H3A H 0.2140(19) 0.0136(14) 0.9161(12) 0.082(7) Uiso 1 1 d . . . H4A H 0.2840(17) 0.1398(13) 0.9998(10) 0.069(6) Uiso 1 1 d . . . H5A H 0.0848(19) -0.0238(15) 1.0695(12) 0.079(7) Uiso 1 1 d . . . H6A H -0.070(2) 0.1218(16) 1.1199(12) 0.084(7) Uiso 1 1 d . . . H7A H -0.0478(12) 0.2772(9) 0.9853(7) 0.031(4) Uiso 1 1 d . . . H14A H -0.1332(13) 0.0375(9) 0.7152(8) 0.034(4) Uiso 1 1 d . . . H21A H 0.4791(13) -0.0272(9) 0.8437(8) 0.036(4) Uiso 1 1 d . . . H28A H 0.5188(14) 0.2879(10) 1.1008(8) 0.035(4) Uiso 1 1 d . . . H30A H 0.246(2) 0.1665(19) 1.3508(17) 0.124(9) Uiso 1 1 d . . . H31A H 0.519(3) 0.137(2) 1.278(2) 0.170(14) Uiso 1 1 d . . . H5B H 0.202(2) -0.0057(17) 1.0530(14) 0.110(9) Uiso 1 1 d . . . H6B H -0.035(2) 0.2059(18) 1.1535(15) 0.116(10) Uiso 1 1 d . . . H7B H -0.0836(12) 0.3775(10) 0.9499(7) 0.030(4) Uiso 1 1 d . . . H14B H -0.0769(12) 0.0158(10) 0.8034(8) 0.034(4) Uiso 1 1 d . . . H21B H 0.3883(13) -0.0406(10) 0.9012(8) 0.041(4) Uiso 1 1 d . . . H28B H 0.4161(12) 0.2086(9) 1.0963(7) 0.030(3) Uiso 1 1 d . . . H30B H 0.258(3) 0.253(3) 1.3235(19) 0.153(13) Uiso 1 1 d . . . H31B H 0.488(3) 0.194(2) 1.342(2) 0.169(15) Uiso 1 1 d . . . H30C H 0.150(3) 0.200(2) 1.2764(18) 0.140(12) Uiso 1 1 d . . . H31C H 0.462(4) 0.105(3) 1.351(3) 0.196(19) Uiso 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 Li1 0.0415(13) 0.0389(14) 0.0321(12) 0.0029(10) 0.0129(10) -0.0051(11) O1 0.0301(5) 0.0294(5) 0.0260(5) 0.0021(4) 0.0084(4) -0.0052(4) O2 0.0398(6) 0.0289(5) 0.0278(5) 0.0016(4) -0.0006(4) -0.0013(4) O3 0.0413(6) 0.0333(6) 0.0277(5) 0.0039(4) 0.0087(4) -0.0047(4) O4 0.0323(5) 0.0346(6) 0.0382(6) -0.0042(4) 0.0144(4) -0.0054(4) O5 0.0473(7) 0.0354(7) 0.0480(7) 0.0030(5) 0.0148(5) -0.0071(6) O6 0.0492(7) 0.0454(7) 0.0674(8) -0.0029(6) 0.0310(6) -0.0085(6) O7 0.0581(7) 0.0736(9) 0.0308(6) -0.0067(6) 0.0103(5) -0.0100(6) C1 0.0341(7) 0.0273(7) 0.0215(6) -0.0028(6) 0.0110(6) -0.0054(6) C2 0.0343(7) 0.0300(8) 0.0254(7) -0.0039(6) 0.0102(6) -0.0029(6) C3 0.0431(9) 0.0304(8) 0.0428(9) 0.0000(7) 0.0110(7) -0.0004(7) C4 0.0492(10) 0.0292(9) 0.0592(10) 0.0011(8) 0.0136(8) -0.0106(7) C5 0.0359(9) 0.0375(9) 0.0468(9) -0.0041(7) 0.0107(7) -0.0111(7) C6 0.0313(7) 0.0341(8) 0.0259(7) -0.0040(6) 0.0096(6) -0.0058(6) C7 0.0306(8) 0.0309(8) 0.0342(8) -0.0015(6) 0.0112(6) 0.0019(6) C8 0.0235(7) 0.0308(8) 0.0282(7) 0.0041(6) 0.0063(5) -0.0027(5) C9 0.0239(7) 0.0321(8) 0.0318(7) 0.0010(6) 0.0101(6) -0.0033(6) C10 0.0329(8) 0.0322(9) 0.0412(8) 0.0041(7) 0.0105(6) 0.0021(6) C11 0.0369(8) 0.0393(9) 0.0352(8) 0.0084(7) 0.0034(7) 0.0038(7) C12 0.0328(8) 0.0426(9) 0.0288(8) 0.0013(7) 0.0024(6) -0.0024(6) C13 0.0253(7) 0.0338(8) 0.0299(7) 0.0012(6) 0.0055(6) -0.0049(6) C14 0.0355(8) 0.0330(8) 0.0271(7) -0.0019(7) 0.0016(6) -0.0060(6) C15 0.0414(8) 0.0228(7) 0.0236(7) -0.0006(6) 0.0095(6) -0.0022(6) C16 0.0374(8) 0.0250(7) 0.0266(7) -0.0041(6) 0.0066(6) -0.0032(6) C17 0.0460(9) 0.0314(8) 0.0269(7) 0.0007(6) 0.0060(7) 0.0008(7) C18 0.0586(11) 0.0425(9) 0.0298(8) 0.0044(7) 0.0180(8) -0.0021(7) C19 0.0445(9) 0.0430(9) 0.0366(8) -0.0019(7) 0.0187(7) -0.0023(7) C20 0.0387(8) 0.0268(8) 0.0304(7) -0.0030(6) 0.0102(6) 0.0008(6) C21 0.0368(8) 0.0365(9) 0.0365(8) -0.0010(7) 0.0115(7) 0.0063(7) C22 0.0241(7) 0.0340(8) 0.0288(7) 0.0062(6) 0.0047(6) 0.0013(6) C23 0.0294(8) 0.0365(8) 0.0325(7) 0.0039(6) 0.0061(6) 0.0068(6) C24 0.0335(8) 0.0550(10) 0.0436(9) -0.0022(8) 0.0152(7) 0.0039(7) C25 0.0320(9) 0.0654(12) 0.0562(10) -0.0033(9) 0.0183(8) -0.0083(8) C26 0.0309(8) 0.0483(10) 0.0423(8) -0.0016(8) 0.0076(7) -0.0078(7) C27 0.0260(7) 0.0364(8) 0.0274(7) 0.0053(6) 0.0030(5) -0.0002(6) C28 0.0300(8) 0.0380(9) 0.0277(7) -0.0022(7) 0.0037(6) -0.0090(6) C29 0.0584(11) 0.0607(11) 0.0349(9) -0.0052(8) 0.0092(8) -0.0113(9) C30 0.0952(19) 0.0730(16) 0.0434(11) 0.0009(11) 0.0292(12) 0.0122(13) C31 0.0687(18) 0.270(5) 0.0617(18) -0.051(3) -0.0052(14) 0.008(2) _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 Li1 O1 1.924(2) . ? Li1 O6 1.930(3) . ? Li1 O7 1.949(3) . ? Li1 O5 1.950(3) . ? O1 C1 1.3510(15) . ? O2 C8 1.3665(15) . ? O3 C15 1.3871(15) . ? O4 C22 1.3716(15) . ? O7 C29 1.2151(18) . ? C1 C6 1.4084(17) . ? C1 C2 1.4117(19) . ? C2 C3 1.391(2) . ? C2 C7 1.5230(19) . ? C3 C4 1.389(2) . ? C4 C5 1.386(2) . ? C5 C6 1.387(2) . ? C6 C28 1.5232(19) . ? C7 C9 1.5250(18) . ? C8 C9 1.4005(18) . ? C8 C13 1.4033(18) . ? C9 C10 1.3931(19) . ? C10 C11 1.385(2) . ? C11 C12 1.383(2) . ? C12 C13 1.3945(19) . ? C13 C14 1.517(2) . ? C14 C16 1.5230(19) . ? C15 C16 1.3987(18) . ? C15 C20 1.3989(18) . ? C16 C17 1.3906(19) . ? C17 C18 1.382(2) . ? C18 C19 1.383(2) . ? C19 C20 1.3939(19) . ? C20 C21 1.5188(19) . ? C21 C23 1.515(2) . ? C22 C27 1.4020(19) . ? C22 C23 1.4023(19) . ? C23 C24 1.393(2) . ? C24 C25 1.379(2) . ? C25 C26 1.384(2) . ? C26 C27 1.3924(19) . ? C27 C28 1.5194(19) . ? C29 C30 1.478(3) . ? C29 C31 1.483(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 O1 Li1 O6 115.71(13) . . ? O1 Li1 O7 113.51(12) . . ? O6 Li1 O7 113.80(12) . . ? O1 Li1 O5 97.87(11) . . ? O6 Li1 O5 106.54(12) . . ? O7 Li1 O5 107.54(12) . . ? C1 O1 Li1 134.60(10) . . ? C29 O7 Li1 145.54(14) . . ? O1 C1 C6 119.68(11) . . ? O1 C1 C2 120.19(11) . . ? C6 C1 C2 120.12(12) . . ? C3 C2 C1 118.89(13) . . ? C3 C2 C7 120.26(13) . . ? C1 C2 C7 120.81(12) . . ? C4 C3 C2 121.10(15) . . ? C5 C4 C3 119.57(15) . . ? C4 C5 C6 121.24(14) . . ? C5 C6 C1 119.07(13) . . ? C5 C6 C28 120.88(12) . . ? C1 C6 C28 120.04(12) . . ? C2 C7 C9 115.41(11) . . ? O2 C8 C9 121.61(11) . . ? O2 C8 C13 116.46(12) . . ? C9 C8 C13 121.90(12) . . ? C10 C9 C8 117.94(12) . . ? C10 C9 C7 120.59(13) . . ? C8 C9 C7 121.44(12) . . ? C11 C10 C9 121.24(14) . . ? C12 C11 C10 119.71(14) . . ? C11 C12 C13 121.36(13) . . ? C12 C13 C8 117.74(13) . . ? C12 C13 C14 121.33(12) . . ? C8 C13 C14 120.81(12) . . ? C13 C14 C16 110.65(11) . . ? O3 C15 C16 118.88(12) . . ? O3 C15 C20 119.23(11) . . ? C16 C15 C20 121.87(12) . . ? C17 C16 C15 117.69(13) . . ? C17 C16 C14 119.69(12) . . ? C15 C16 C14 122.57(12) . . ? C18 C17 C16 121.52(14) . . ? C17 C18 C19 119.83(14) . . ? C18 C19 C20 120.82(14) . . ? C19 C20 C15 118.22(12) . . ? C19 C20 C21 120.17(13) . . ? C15 C20 C21 121.60(12) . . ? C23 C21 C20 112.16(12) . . ? O4 C22 C27 121.32(12) . . ? O4 C22 C23 117.20(12) . . ? C27 C22 C23 121.46(12) . . ? C24 C23 C22 118.25(13) . . ? C24 C23 C21 120.62(13) . . ? C22 C23 C21 121.11(12) . . ? C25 C24 C23 121.17(15) . . ? C24 C25 C26 119.76(15) . . ? C25 C26 C27 121.37(15) . . ? C26 C27 C22 117.95(13) . . ? C26 C27 C28 120.14(13) . . ? C22 C27 C28 121.91(12) . . ? C27 C28 C6 113.73(11) . . ? O7 C29 C30 122.87(18) . . ? O7 C29 C31 119.7(2) . . ? C30 C29 C31 117.4(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.177 _refine_diff_density_min -0.133 _refine_diff_density_rms 0.030 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H64 Na2 O11' _chemical_formula_weight 1067.14 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 29.155(4) _cell_length_b 37.198(4) _cell_length_c 10.5835(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11478(2) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14856 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.33 _reflns_number_total 4124 _reflns_number_gt 3040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0759P)^2^+29.4309P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.3(11) _refine_ls_number_reflns 4124 _refine_ls_number_parameters 366 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.2236 _refine_ls_wR_factor_gt 0.2087 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.006 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 Na1 Na 0.45160(9) 0.03662(7) 0.7200(4) 0.0879(10) Uani 1 1 d . . . O1 O 0.44383(17) -0.00727(11) 0.8723(6) 0.0842(16) Uani 1 1 d . . . O2 O 0.38447(18) 0.00468(16) 0.6664(8) 0.100(2) Uani 1 1 d . . . O3 O 0.42198(18) -0.05512(16) 0.5897(6) 0.0919(17) Uani 1 1 d . . . O4 O 0.47825(14) -0.06168(11) 0.7685(5) 0.0734(14) Uani 1 1 d . . . O5 O 0.5000 0.0000 0.5827(10) 0.087(2) Uani 1 2 d S . . O6 O 0.42130(19) 0.09043(15) 0.6861(9) 0.132(3) Uani 1 1 d . . . C1 C 0.4411(5) -0.0386(4) 1.0646(12) 0.122(4) Uani 1 1 d . . . C2 C 0.4209(8) -0.0483(5) 1.1744(16) 0.187(7) Uani 1 1 d . . . H2A H 0.4328 -0.0661 1.2267 0.224 Uiso 1 1 calc R . . C3 C 0.3846(9) -0.0315(7) 1.200(2) 0.217(11) Uani 1 1 d . . . H3B H 0.3717 -0.0377 1.2779 0.260 Uiso 1 1 calc R . . C4 C 0.3599(6) -0.0050(5) 1.134(2) 0.188(8) Uani 1 1 d . . . H4A H 0.3339 0.0066 1.1647 0.226 Uiso 1 1 calc R . . C5 C 0.3811(4) 0.0023(3) 1.0060(13) 0.137(5) Uani 1 1 d . . . C6 C 0.4219(4) -0.0142(3) 0.9819(12) 0.104(3) Uani 1 1 d . . . C7 C 0.3592(5) 0.0264(3) 0.9100(18) 0.187(8) Uani 1 1 d . . . H7A H 0.3419 0.0452 0.9525 0.225 Uiso 1 1 calc R . . H7B H 0.3827 0.0378 0.8588 0.225 Uiso 1 1 calc R . . C8 C 0.3282(3) 0.0052(3) 0.8287(18) 0.143(6) Uani 1 1 d . . . C9 C 0.2842(4) -0.0054(3) 0.8648(18) 0.163(6) Uani 1 1 d . . . H9A H 0.2722 0.0013 0.9426 0.195 Uiso 1 1 calc R . . C10 C 0.2585(4) -0.0267(4) 0.780(2) 0.161(8) Uani 1 1 d . . . H10A H 0.2283 -0.0319 0.8023 0.193 Uiso 1 1 calc R . . C11 C 0.2739(5) -0.0397(5) 0.6726(17) 0.173(8) Uani 1 1 d . . . H11A H 0.2565 -0.0551 0.6226 0.207 Uiso 1 1 calc R . . C12 C 0.3167(3) -0.0292(4) 0.6397(18) 0.151(6) Uani 1 1 d . . . C13 C 0.3430(3) -0.0065(3) 0.7114(13) 0.106(4) Uani 1 1 d . . . C14 C 0.3302(5) -0.0398(5) 0.5128(17) 0.192(8) Uani 1 1 d . . . H14A H 0.3526 -0.0230 0.4796 0.230 Uiso 1 1 calc R . . H14B H 0.3037 -0.0397 0.4575 0.230 Uiso 1 1 calc R . . C15 C 0.3514(3) -0.0785(4) 0.5182(9) 0.134(4) Uani 1 1 d . . . C16 C 0.3295(5) -0.1093(5) 0.4832(15) 0.177(6) Uani 1 1 d . . . H16A H 0.2998 -0.1070 0.4516 0.212 Uiso 1 1 calc R . . C17 C 0.3473(6) -0.1432(5) 0.4907(16) 0.169(6) Uani 1 1 d . . . H17A H 0.3296 -0.1627 0.4648 0.203 Uiso 1 1 calc R . . C18 C 0.3919(4) -0.1491(4) 0.5368(14) 0.171(6) Uani 1 1 d . . . H18A H 0.4041 -0.1720 0.5455 0.205 Uiso 1 1 calc R . . C19 C 0.4167(3) -0.1185(3) 0.5687(11) 0.118(4) Uani 1 1 d . . . C20 C 0.3968(3) -0.0856(3) 0.5619(9) 0.099(3) Uani 1 1 d . . . C21 C 0.4649(3) -0.1237(3) 0.6197(12) 0.131(5) Uani 1 1 d . . . H21A H 0.4842 -0.1042 0.5906 0.157 Uiso 1 1 calc R . . H21B H 0.4774 -0.1460 0.5863 0.157 Uiso 1 1 calc R . . C22 C 0.4661(2) -0.12505(18) 0.7647(13) 0.105(4) Uani 1 1 d . . . C23 C 0.4629(4) -0.1559(3) 0.833(2) 0.147(6) Uani 1 1 d . . . H23A H 0.4600 -0.1775 0.7895 0.176 Uiso 1 1 calc R . . C24 C 0.4639(5) -0.1573(4) 0.960(2) 0.170(8) Uani 1 1 d . . . H24A H 0.4593 -0.1787 1.0036 0.205 Uiso 1 1 calc R . . C25 C 0.4717(3) -0.1264(3) 1.0202(16) 0.166(7) Uani 1 1 d . . . H25A H 0.4736 -0.1269 1.1079 0.199 Uiso 1 1 calc R . . C26 C 0.4772(3) -0.0936(2) 0.9598(12) 0.111(4) Uani 1 1 d . . . C27 C 0.4742(2) -0.09261(16) 0.8296(10) 0.076(2) Uani 1 1 d . . . C28 C 0.4846(4) -0.0595(3) 1.0366(10) 0.117(4) Uani 1 1 d . . . H28A H 0.5056 -0.0440 0.9910 0.140 Uiso 1 1 calc R . . H28B H 0.4990 -0.0659 1.1160 0.140 Uiso 1 1 calc R . . C29 C 0.5000 0.0000 0.4690(16) 0.091(4) Uani 1 2 d S . . C30 C 0.4706(4) 0.0252(3) 0.4018(12) 0.159(5) Uani 1 1 d . . . H30A H 0.4744 0.0219 0.3124 0.239 Uiso 1 1 calc R . . H30B H 0.4788 0.0493 0.4244 0.239 Uiso 1 1 calc R . . H30C H 0.4392 0.0209 0.4243 0.239 Uiso 1 1 calc R . . C31 C 0.4124(3) 0.1206(2) 0.7206(14) 0.105(3) Uani 1 1 d . . . C32 C 0.4041(4) 0.1492(2) 0.6282(15) 0.155(5) Uani 1 1 d . . . H32A H 0.4071 0.1396 0.5443 0.232 Uiso 1 1 calc R . . H32B H 0.4261 0.1681 0.6403 0.232 Uiso 1 1 calc R . . H32C H 0.3737 0.1585 0.6395 0.232 Uiso 1 1 calc R . . C33 C 0.4091(4) 0.1286(4) 0.8555(18) 0.180(6) Uani 1 1 d . . . H33A H 0.4155 0.1072 0.9034 0.270 Uiso 1 1 calc R . . H33B H 0.3787 0.1369 0.8747 0.270 Uiso 1 1 calc R . . H33C H 0.4309 0.1469 0.8772 0.270 Uiso 1 1 calc R . . H1O H 0.465(3) -0.033(2) 0.817(7) 0.10(2) Uiso 1 1 d . . . H2O H 0.3805(16) -0.0126(13) 0.599(5) 0.026(15) Uiso 1 1 d . . . H3O H 0.444(2) -0.0605(14) 0.661(6) 0.053(17) Uiso 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 Na1 0.0629(16) 0.0579(15) 0.143(3) 0.0299(17) 0.0188(18) 0.0058(12) O1 0.087(3) 0.044(2) 0.121(5) 0.008(3) 0.031(3) 0.000(2) O2 0.066(4) 0.087(4) 0.148(6) 0.040(4) 0.008(4) -0.008(3) O3 0.067(3) 0.119(4) 0.089(4) 0.013(3) -0.029(3) -0.012(3) O4 0.060(3) 0.042(2) 0.118(4) 0.000(3) -0.019(3) 0.006(2) O5 0.063(4) 0.092(5) 0.107(7) 0.000 0.000 -0.016(3) O6 0.087(4) 0.063(3) 0.247(9) 0.034(5) 0.008(4) 0.015(3) C1 0.166(12) 0.136(10) 0.065(7) -0.003(7) 0.007(8) -0.084(9) C2 0.25(2) 0.200(18) 0.114(14) -0.027(12) -0.017(14) -0.080(17) C3 0.27(3) 0.23(3) 0.155(17) -0.039(16) 0.058(19) -0.01(2) C4 0.147(13) 0.174(14) 0.24(2) -0.088(14) 0.094(14) -0.033(10) C5 0.133(9) 0.075(7) 0.201(13) -0.044(7) 0.101(9) -0.027(6) C6 0.105(7) 0.088(6) 0.119(9) -0.014(7) 0.032(7) -0.047(6) C7 0.146(10) 0.048(5) 0.37(2) 0.003(10) 0.158(13) 0.022(7) C8 0.078(7) 0.055(6) 0.296(18) 0.040(8) 0.060(10) 0.008(5) C9 0.093(8) 0.112(8) 0.284(18) 0.087(11) 0.058(10) 0.035(7) C10 0.055(7) 0.129(10) 0.30(2) 0.127(13) -0.022(10) -0.006(6) C11 0.103(12) 0.203(16) 0.211(17) 0.144(15) -0.025(10) 0.013(10) C12 0.047(6) 0.179(11) 0.227(15) 0.175(12) -0.036(8) -0.022(6) C13 0.034(5) 0.092(6) 0.193(12) 0.079(7) 0.015(6) 0.011(5) C14 0.115(10) 0.260(17) 0.199(16) 0.179(15) -0.062(10) -0.045(10) C15 0.082(6) 0.236(13) 0.085(7) 0.018(8) -0.055(5) -0.079(8) C16 0.125(10) 0.262(18) 0.144(12) 0.020(14) -0.079(9) -0.061(13) C17 0.149(13) 0.221(15) 0.138(11) -0.062(13) 0.001(10) -0.107(12) C18 0.117(9) 0.179(12) 0.216(15) -0.103(11) -0.009(9) -0.053(8) C19 0.098(7) 0.119(8) 0.136(9) -0.078(7) 0.004(6) -0.028(6) C20 0.076(6) 0.131(8) 0.089(6) -0.038(6) 0.004(5) -0.034(6) C21 0.096(7) 0.107(8) 0.188(14) -0.091(8) -0.033(8) 0.004(5) C22 0.047(4) 0.036(4) 0.230(13) -0.020(6) -0.047(6) 0.006(3) C23 0.088(7) 0.045(6) 0.31(2) 0.015(10) -0.012(11) 0.005(4) C24 0.139(10) 0.078(8) 0.29(2) 0.095(14) -0.029(13) -0.017(7) C25 0.100(7) 0.107(8) 0.289(19) 0.097(11) -0.076(9) -0.035(6) C26 0.083(6) 0.081(6) 0.168(11) 0.045(7) -0.071(7) -0.021(4) C27 0.061(4) 0.041(4) 0.126(8) 0.019(4) -0.035(5) 0.009(3) C28 0.120(8) 0.133(9) 0.097(8) 0.006(6) -0.042(7) -0.052(7) C29 0.077(8) 0.125(11) 0.072(9) 0.000 0.000 -0.024(7) C30 0.181(12) 0.174(11) 0.123(9) 0.051(9) -0.011(9) 0.003(9) C31 0.061(5) 0.064(5) 0.189(12) 0.037(7) 0.022(6) 0.009(4) C32 0.112(8) 0.081(6) 0.270(16) 0.067(9) -0.005(9) 0.009(5) C33 0.119(10) 0.206(15) 0.215(17) 0.033(13) 0.042(11) 0.050(9) _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 Na1 O6 2.217(6) . ? Na1 O1 2.305(6) . ? Na1 O4 2.306(5) 2_655 ? Na1 O2 2.359(6) . ? Na1 O5 2.441(7) . ? Na1 Na1 3.923(5) 2_655 ? O1 C6 1.350(12) . ? O1 H1O 1.26(9) . ? O2 C13 1.365(10) . ? O2 H2O 0.97(5) . ? O3 C20 1.382(10) . ? O3 H3O 1.02(7) . ? O4 C27 1.325(8) . ? O4 Na1 2.306(5) 2_655 ? O4 H1O 1.26(9) . ? O5 C29 1.203(14) . ? O5 Na1 2.441(7) 2_655 ? O6 C31 1.207(10) . ? C1 C2 1.352(19) . ? C1 C6 1.379(15) . ? C1 C28 1.519(16) . ? C2 C3 1.26(2) . ? C2 H2A 0.9300 . ? C3 C4 1.41(3) . ? C3 H3B 0.9300 . ? C4 C5 1.51(2) . ? C4 H4A 0.9300 . ? C5 C6 1.362(14) . ? C5 C7 1.499(19) . ? C7 C8 1.475(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.384(17) . ? C8 C9 1.397(14) . ? C9 C10 1.41(2) . ? C9 H9A 0.9300 . ? C10 C11 1.32(2) . ? C10 H10A 0.9300 . ? C11 C12 1.355(16) . ? C11 H11A 0.9300 . ? C12 C13 1.369(18) . ? C12 C14 1.45(2) . ? C14 C15 1.565(19) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.363(18) . ? C15 C20 1.427(13) . ? C16 C17 1.367(18) . ? C16 H16A 0.9300 . ? C17 C18 1.406(19) . ? C17 H17A 0.9300 . ? C18 C19 1.388(13) . ? C18 H18A 0.9300 . ? C19 C20 1.358(13) . ? C19 C21 1.519(13) . ? C21 C22 1.536(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.362(15) . ? C22 C27 1.409(11) . ? C23 C24 1.34(2) . ? C23 H23A 0.9300 . ? C24 C25 1.33(2) . ? C24 H24A 0.9300 . ? C25 C26 1.384(13) . ? C25 H25A 0.9300 . ? C26 C27 1.382(12) . ? C26 C28 1.522(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.455(12) 2_655 ? C29 C30 1.455(12) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.462(19) . ? C31 C32 1.466(14) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 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 O6 Na1 O1 135.5(3) . . ? O6 Na1 O4 91.4(2) . 2_655 ? O1 Na1 O4 102.6(2) . 2_655 ? O6 Na1 O2 94.9(2) . . ? O1 Na1 O2 74.4(2) . . ? O4 Na1 O2 173.3(2) 2_655 . ? O6 Na1 O5 129.6(3) . . ? O1 Na1 O5 94.5(2) . . ? O4 Na1 O5 81.11(16) 2_655 . ? O2 Na1 O5 93.2(2) . . ? O6 Na1 Na1 156.0(2) . 2_655 ? O1 Na1 Na1 65.09(14) . 2_655 ? O4 Na1 Na1 69.06(13) 2_655 2_655 ? O2 Na1 Na1 104.31(18) . 2_655 ? O5 Na1 Na1 36.6(2) . 2_655 ? C6 O1 Na1 141.5(6) . . ? C6 O1 H1O 119(3) . . ? Na1 O1 H1O 99(3) . . ? C13 O2 Na1 143.6(9) . . ? C13 O2 H2O 87(3) . . ? Na1 O2 H2O 128(3) . . ? C20 O3 H3O 110(3) . . ? C27 O4 Na1 122.6(4) . 2_655 ? C27 O4 H1O 121(3) . . ? Na1 O4 H1O 91(3) 2_655 . ? C29 O5 Na1 126.6(2) . 2_655 ? C29 O5 Na1 126.6(2) . . ? Na1 O5 Na1 106.9(4) 2_655 . ? C31 O6 Na1 151.0(9) . . ? C2 C1 C6 123.0(17) . . ? C2 C1 C28 113.2(17) . . ? C6 C1 C28 123.6(10) . . ? C3 C2 C1 115(2) . . ? C3 C2 H2A 122.5 . . ? C1 C2 H2A 122.6 . . ? C2 C3 C4 132(2) . . ? C2 C3 H3B 114.1 . . ? C4 C3 H3B 114.1 . . ? C3 C4 C5 111.3(15) . . ? C3 C4 H4A 124.3 . . ? C5 C4 H4A 124.3 . . ? C6 C5 C7 121.0(11) . . ? C6 C5 C4 116.4(15) . . ? C7 C5 C4 122.6(13) . . ? O1 C6 C5 119.3(12) . . ? O1 C6 C1 118.6(10) . . ? C5 C6 C1 122.1(12) . . ? C8 C7 C5 109.6(9) . . ? C8 C7 H7A 109.7 . . ? C5 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C5 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 116.2(15) . . ? C13 C8 C7 120.1(10) . . ? C9 C8 C7 123.7(17) . . ? C8 C9 C10 118.4(16) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? C11 C10 C9 125.0(15) . . ? C11 C10 H10A 117.5 . . ? C9 C10 H10A 117.5 . . ? C10 C11 C12 115.5(19) . . ? C10 C11 H11A 122.3 . . ? C12 C11 H11A 122.3 . . ? C11 C12 C13 123.5(18) . . ? C11 C12 C14 114.0(17) . . ? C13 C12 C14 121.9(10) . . ? O2 C13 C12 119.3(13) . . ? O2 C13 C8 119.5(12) . . ? C12 C13 C8 121.2(10) . . ? C12 C14 C15 108.8(10) . . ? C12 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? C12 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C20 111.6(13) . . ? C16 C15 C14 125.3(11) . . ? C20 C15 C14 123.2(10) . . ? C15 C16 C17 125.6(13) . . ? C15 C16 H16A 117.2 . . ? C17 C16 H16A 117.2 . . ? C16 C17 C18 120.9(12) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C19 C18 C17 116.1(13) . . ? C19 C18 H18A 122.0 . . ? C17 C18 H18A 122.0 . . ? C20 C19 C18 120.3(11) . . ? C20 C19 C21 122.0(7) . . ? C18 C19 C21 117.6(11) . . ? C19 C20 O3 120.1(8) . . ? C19 C20 C15 125.4(9) . . ? O3 C20 C15 114.3(10) . . ? C19 C21 C22 112.3(9) . . ? C19 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C19 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 118.3(12) . . ? C23 C22 C21 123.9(10) . . ? C27 C22 C21 117.6(9) . . ? C24 C23 C22 124.3(13) . . ? C24 C23 H23A 117.9 . . ? C22 C23 H23A 117.9 . . ? C25 C24 C23 116.6(13) . . ? C25 C24 H24A 121.7 . . ? C23 C24 H24A 121.7 . . ? C24 C25 C26 123.9(16) . . ? C24 C25 H25A 118.0 . . ? C26 C25 H25A 118.1 . . ? C27 C26 C25 118.5(11) . . ? C27 C26 C28 121.2(8) . . ? C25 C26 C28 120.2(12) . . ? O4 C27 C26 120.4(7) . . ? O4 C27 C22 121.4(9) . . ? C26 C27 C22 118.2(8) . . ? C26 C28 C1 114.5(7) . . ? C26 C28 H28A 108.6 . . ? C1 C28 H28A 108.6 . . ? C26 C28 H28B 108.6 . . ? C1 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? O5 C29 C30 119.3(8) . 2_655 ? O5 C29 C30 119.3(8) . . ? C30 C29 C30 121.5(16) 2_655 . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C31 C33 120.0(10) . . ? O6 C31 C32 120.5(13) . . ? C33 C31 C32 119.5(11) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 O3 H3O O4 1.02(7) 1.51(7) 2.516(7) 170(5) . O2 H2O O3 0.97(5) 1.99(5) 2.608(9) 119(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.171 _refine_diff_density_min -0.164 _refine_diff_density_rms 0.044 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H31 O5 Rb' _chemical_formula_weight 581.04 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' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 18.1392(7) _cell_length_b 18.9515(7) _cell_length_c 7.4377(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2556.82(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.979 _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 100(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16078 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4839 _reflns_number_gt 4177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0367P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.084(6) _refine_ls_number_reflns 4839 _refine_ls_number_parameters 471 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.811549(12) 0.850022(12) 0.42058(6) 0.03405(9) Uani 1 1 d . . . O1 O 0.96264(13) 0.77117(11) 0.1005(3) 0.0322(5) Uani 1 1 d . . . O2 O 0.92228(9) 0.88629(9) -0.0388(3) 0.0205(4) Uani 1 1 d . . . O3 O 0.81220(10) 0.83193(10) -0.1864(3) 0.0312(5) Uani 1 1 d . . . O4 O 0.84168(10) 0.69170(10) -0.0654(3) 0.0243(4) Uani 1 1 d . . . O5 O 0.68761(9) 0.93596(10) 0.4300(4) 0.0407(5) Uani 1 1 d . . . C1 C 0.94333(13) 0.71336(13) 0.3776(4) 0.0182(6) Uani 1 1 d . . . C2 C 0.95161(16) 0.71187(16) 0.5630(4) 0.0242(6) Uani 1 1 d . . . C3 C 0.98083(18) 0.76928(17) 0.6529(4) 0.0278(7) Uani 1 1 d . . . C4 C 1.00223(16) 0.82863(16) 0.5583(4) 0.0245(7) Uani 1 1 d . . . C5 C 0.99634(13) 0.83153(14) 0.3726(4) 0.0182(6) Uani 1 1 d . . . C6 C 0.96760(14) 0.77268(14) 0.2823(4) 0.0192(6) Uani 1 1 d . . . C7 C 1.01652(14) 0.89782(14) 0.2698(4) 0.0214(6) Uani 1 1 d . . . C8 C 0.95027(13) 0.94560(13) 0.2363(4) 0.0186(6) Uani 1 1 d . . . C9 C 0.93124(14) 0.99672(14) 0.3623(4) 0.0214(6) Uani 1 1 d . . . C10 C 0.87236(15) 1.04230(14) 0.3332(4) 0.0238(6) Uani 1 1 d . . . C11 C 0.83403(15) 1.03784(14) 0.1722(4) 0.0216(6) Uani 1 1 d . . . C12 C 0.85074(14) 0.98715(13) 0.0439(4) 0.0186(6) Uani 1 1 d . . . C13 C 0.90766(13) 0.93844(13) 0.0784(4) 0.0188(6) Uani 1 1 d . . . C14 C 0.80821(15) 0.98325(14) -0.1311(4) 0.0217(6) Uani 1 1 d . . . C15 C 0.74079(13) 0.93580(12) -0.1176(4) 0.0200(6) Uani 1 1 d . . . C16 C 0.67260(12) 0.96396(12) -0.0767(6) 0.0250(6) Uani 1 1 d . . . C17 C 0.61051(14) 0.92232(14) -0.0609(5) 0.0311(7) Uani 1 1 d . . . C18 C 0.61686(12) 0.85030(13) -0.0807(6) 0.0264(5) Uani 1 1 d . . . C19 C 0.68472(12) 0.81908(13) -0.1184(3) 0.0187(6) Uani 1 1 d . . . C20 C 0.74673(14) 0.86239(13) -0.1400(4) 0.0203(6) Uani 1 1 d . . . C21 C 0.69278(16) 0.73941(14) -0.1199(4) 0.0235(7) Uani 1 1 d . . . C22 C 0.72211(16) 0.71380(13) 0.0604(4) 0.0190(6) Uani 1 1 d . . . C23 C 0.67581(15) 0.71354(13) 0.2094(4) 0.0209(6) Uani 1 1 d . . . C24 C 0.70153(15) 0.69418(14) 0.3775(4) 0.0243(7) Uani 1 1 d . . . C25 C 0.77462(14) 0.67403(13) 0.3961(5) 0.0227(6) Uani 1 1 d . . . C26 C 0.82293(14) 0.67388(13) 0.2499(4) 0.0191(6) Uani 1 1 d . . . C27 C 0.79536(14) 0.69366(12) 0.0812(4) 0.0195(6) Uani 1 1 d . . . C28 C 0.90358(15) 0.65470(14) 0.2787(5) 0.0237(6) Uani 1 1 d . . . C29 C 0.67335(16) 1.01001(17) 0.4483(6) 0.0374(9) Uani 1 1 d . . . C30 C 0.59778(17) 1.02102(16) 0.3771(6) 0.0429(10) Uani 1 1 d . . . C31 C 0.55853(16) 0.95403(16) 0.4294(9) 0.0471(9) Uani 1 1 d . . . C32 C 0.61892(18) 0.89836(16) 0.4284(7) 0.0394(7) Uani 1 1 d . . . H2 H 0.9370(19) 0.6768(17) 0.629(5) 0.039(10) Uiso 1 1 d . . . H3 H 0.9840(17) 0.7677(15) 0.769(5) 0.025(9) Uiso 1 1 d . . . H4 H 1.0191(16) 0.8646(14) 0.612(5) 0.021(8) Uiso 1 1 d . . . H7A H 1.0383(14) 0.8813(13) 0.151(4) 0.014(7) Uiso 1 1 d . . . H7B H 1.0509(15) 0.9232(14) 0.356(4) 0.030(8) Uiso 1 1 d . . . H9 H 0.9561(14) 1.0021(14) 0.468(5) 0.019(8) Uiso 1 1 d . . . H10 H 0.8602(12) 1.0756(12) 0.415(5) 0.016(6) Uiso 1 1 d . . . H11 H 0.7949(15) 1.0726(14) 0.151(4) 0.021(8) Uiso 1 1 d . . . H14A H 0.7933(13) 1.0303(14) -0.171(4) 0.015(7) Uiso 1 1 d . . . H14B H 0.8419(19) 0.9697(16) -0.230(5) 0.038(10) Uiso 1 1 d . . . H16 H 0.6673(14) 1.0163(14) -0.068(5) 0.031(7) Uiso 1 1 d . . . H17 H 0.5636(14) 0.9433(12) -0.037(4) 0.021(7) Uiso 1 1 d . . . H18 H 0.5759(13) 0.8230(12) -0.057(5) 0.018(6) Uiso 1 1 d . . . H21A H 0.6502(16) 0.7167(14) -0.137(4) 0.026(8) Uiso 1 1 d . . . H21B H 0.7230(16) 0.7253(14) -0.206(4) 0.008(7) Uiso 1 1 d . . . H23 H 0.6264(15) 0.7259(12) 0.204(4) 0.008(6) Uiso 1 1 d . . . H24 H 0.6734(14) 0.6918(14) 0.478(4) 0.016(8) Uiso 1 1 d . . . H25 H 0.7930(15) 0.6658(14) 0.496(4) 0.013(8) Uiso 1 1 d . . . H28A H 0.9039(13) 0.6142(14) 0.361(4) 0.018(7) Uiso 1 1 d . . . H28B H 0.9287(17) 0.6465(14) 0.172(4) 0.022(8) Uiso 1 1 d . . . H29A H 0.7112(17) 1.0376(16) 0.416(7) 0.052(9) Uiso 1 1 d . . . H29B H 0.671(2) 1.0217(19) 0.582(6) 0.056(11) Uiso 1 1 d . . . H30A H 0.5740(14) 1.0641(14) 0.405(6) 0.034(7) Uiso 1 1 d . . . H30B H 0.603(2) 1.025(2) 0.230(8) 0.094(17) Uiso 1 1 d . . . H31A H 0.523(2) 0.9452(19) 0.352(6) 0.055(13) Uiso 1 1 d . . . H31B H 0.537(2) 0.958(2) 0.551(7) 0.062(14) Uiso 1 1 d . . . H32A H 0.611(2) 0.871(2) 0.529(6) 0.038(11) Uiso 1 1 d . . . H32B H 0.617(2) 0.868(2) 0.327(7) 0.061(14) Uiso 1 1 d . . . H01 H 0.9534(18) 0.8104(17) 0.060(5) 0.038(10) Uiso 1 1 d . . . H03 H 0.876(2) 0.870(2) -0.088(10) 0.097(14) Uiso 1 1 d . . . H04 H 0.837(2) 0.726(2) -0.097(8) 0.015(13) Uiso 0.65 1 d P . . H04A H 0.886(4) 0.709(4) -0.041(12) 0.01(2) Uiso 0.35 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 Rb1 0.02295(12) 0.02553(13) 0.0537(2) 0.00113(19) 0.01343(18) 0.00209(10) O1 0.0640(16) 0.0192(11) 0.0134(11) 0.0019(9) -0.0017(11) -0.0046(11) O2 0.0200(8) 0.0195(8) 0.0220(12) -0.0012(8) 0.0011(8) 0.0004(7) O3 0.0219(10) 0.0201(10) 0.0517(15) -0.0043(9) 0.0083(9) -0.0006(8) O4 0.0240(9) 0.0251(11) 0.0238(12) -0.0027(11) 0.0038(10) 0.0031(8) O5 0.0298(9) 0.0493(11) 0.0431(14) -0.0010(15) 0.0011(12) 0.0148(9) C1 0.0145(10) 0.0201(12) 0.0199(17) 0.0009(11) -0.0002(11) 0.0028(9) C2 0.0232(14) 0.0283(16) 0.0211(16) 0.0087(14) 0.0075(12) 0.0086(12) C3 0.0321(17) 0.0361(18) 0.0153(17) -0.0022(14) -0.0008(13) 0.0147(14) C4 0.0213(14) 0.0276(15) 0.0246(17) -0.0071(14) -0.0075(13) 0.0071(12) C5 0.0116(10) 0.0217(12) 0.0213(16) -0.0004(11) 0.0007(11) 0.0025(9) C6 0.0177(12) 0.0215(14) 0.0184(15) 0.0000(12) 0.0030(11) 0.0030(10) C7 0.0158(12) 0.0196(13) 0.0287(17) -0.0015(13) -0.0011(12) -0.0038(11) C8 0.0147(11) 0.0156(12) 0.0255(16) 0.0032(11) 0.0019(11) -0.0039(10) C9 0.0193(13) 0.0207(13) 0.0240(17) -0.0008(11) -0.0033(12) -0.0061(11) C10 0.0261(14) 0.0150(13) 0.0304(17) -0.0052(12) -0.0011(12) -0.0011(11) C11 0.0177(13) 0.0167(13) 0.0305(17) 0.0038(11) -0.0013(12) -0.0024(10) C12 0.0201(13) 0.0163(12) 0.0194(15) 0.0031(11) 0.0017(11) -0.0035(10) C13 0.0185(12) 0.0180(12) 0.0200(15) 0.0038(11) 0.0030(11) -0.0060(10) C14 0.0294(13) 0.0159(12) 0.0199(17) 0.0036(10) 0.0013(12) 0.0027(11) C15 0.0232(11) 0.0188(11) 0.0179(16) 0.0004(11) -0.0025(12) 0.0010(9) C16 0.0250(12) 0.0218(12) 0.0282(15) -0.0087(17) -0.0096(17) 0.0071(9) C17 0.0192(11) 0.0361(15) 0.038(2) -0.0060(17) -0.0028(15) 0.0077(10) C18 0.0190(10) 0.0306(12) 0.0296(15) -0.0044(16) -0.0030(17) -0.0020(10) C19 0.0210(11) 0.0214(11) 0.0136(16) -0.0018(10) -0.0060(12) -0.0005(9) C20 0.0185(12) 0.0240(13) 0.0183(15) 0.0000(10) -0.0011(10) 0.0025(10) C21 0.0219(12) 0.0210(12) 0.028(2) -0.0039(12) -0.0022(13) -0.0042(11) C22 0.0224(13) 0.0111(12) 0.0235(16) -0.0032(11) -0.0027(12) -0.0014(10) C23 0.0183(14) 0.0158(13) 0.0286(17) -0.0005(11) -0.0015(12) -0.0025(10) C24 0.0244(13) 0.0227(13) 0.0259(19) -0.0019(12) 0.0067(13) -0.0067(11) C25 0.0277(13) 0.0187(11) 0.0218(17) 0.0056(13) -0.0042(15) -0.0045(10) C26 0.0197(13) 0.0107(11) 0.0269(16) -0.0010(11) 0.0006(12) -0.0018(10) C27 0.0248(13) 0.0101(11) 0.0235(16) -0.0025(11) 0.0033(12) -0.0024(10) C28 0.0240(14) 0.0136(13) 0.0334(18) 0.0027(13) -0.0023(13) 0.0034(11) C29 0.0222(13) 0.0444(17) 0.046(3) 0.0093(19) 0.0057(16) -0.0032(12) C30 0.0302(15) 0.0292(16) 0.069(3) -0.0101(18) -0.0056(18) 0.0050(12) C31 0.0266(14) 0.0380(16) 0.077(3) 0.005(3) -0.007(2) -0.0012(13) C32 0.0493(17) 0.0318(15) 0.037(2) 0.000(2) -0.001(2) 0.0066(13) _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 Rb1 O5 2.7770(17) . ? Rb1 O3 2.943(3) 1_556 ? Rb1 C6 3.349(3) . ? Rb1 C5 3.389(2) . ? Rb1 C8 3.390(2) . ? Rb1 C25 3.407(3) . ? Rb1 C20 3.481(3) 1_556 ? Rb1 C13 3.511(3) . ? Rb1 C1 3.539(2) . ? Rb1 C9 3.554(3) . ? Rb1 C26 3.577(3) . ? Rb1 C24 3.579(3) . ? O1 C6 1.355(4) . ? O1 H01 0.82(3) . ? O2 C13 1.344(3) . ? O2 H03 0.97(5) . ? O3 C20 1.365(3) . ? O3 Rb1 2.943(3) 1_554 ? O4 C27 1.377(4) . ? O4 H04 0.69(4) . ? O4 H04A 0.88(8) . ? O5 C29 1.433(4) . ? O5 C32 1.435(4) . ? C1 C2 1.387(4) . ? C1 C6 1.400(4) . ? C1 C28 1.515(4) . ? C2 C3 1.383(4) . ? C2 H2 0.87(3) . ? C3 C4 1.382(4) . ? C3 H3 0.87(3) . ? C4 C5 1.386(4) . ? C4 H4 0.85(3) . ? C5 C6 1.403(4) . ? C5 C7 1.516(4) . ? C7 C8 1.525(4) . ? C7 H7A 1.02(3) . ? C7 H7B 1.01(3) . ? C8 C9 1.392(4) . ? C8 C13 1.412(4) . ? C9 C10 1.391(4) . ? C9 H9 0.91(3) . ? C10 C11 1.387(4) . ? C10 H10 0.91(3) . ? C11 C12 1.387(4) . ? C11 H11 0.98(3) . ? C12 C13 1.408(4) . ? C12 C14 1.515(4) . ? C14 C15 1.521(3) . ? C14 H14A 0.98(3) . ? C14 H14B 0.99(4) . ? C15 C16 1.381(3) . ? C15 C20 1.405(3) . ? C16 C17 1.380(3) . ? C16 H16 1.00(3) . ? C17 C18 1.378(3) . ? C17 H17 0.96(3) . ? C18 C19 1.394(3) . ? C18 H18 0.92(2) . ? C19 C20 1.402(3) . ? C19 C21 1.517(4) . ? C20 Rb1 3.481(3) 1_554 ? C21 C22 1.522(4) . ? C21 H21A 0.89(3) . ? C21 H21B 0.88(3) . ? C22 C23 1.390(4) . ? C22 C27 1.391(4) . ? C23 C24 1.384(4) . ? C23 H23 0.93(3) . ? C24 C25 1.387(4) . ? C24 H24 0.91(3) . ? C25 C26 1.397(4) . ? C25 H25 0.83(3) . ? C26 C27 1.402(4) . ? C26 C28 1.523(4) . ? C28 H28A 0.98(3) . ? C28 H28B 0.93(3) . ? C29 C30 1.484(4) . ? C29 H29A 0.90(3) . ? C29 H29B 1.02(4) . ? C30 C31 1.507(5) . ? C30 H30A 0.95(3) . ? C30 H30B 1.10(6) . ? C31 C32 1.521(4) . ? C31 H31A 0.87(4) . ? C31 H31B 0.99(5) . ? C32 H32A 0.93(4) . ? C32 H32B 0.95(5) . ? 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 O5 Rb1 O3 92.66(8) . 1_556 ? O5 Rb1 C6 161.54(8) . . ? O3 Rb1 C6 104.52(6) 1_556 . ? O5 Rb1 C5 149.77(6) . . ? O3 Rb1 C5 95.08(6) 1_556 . ? C6 Rb1 C5 24.02(6) . . ? O5 Rb1 C8 107.32(6) . . ? O3 Rb1 C8 117.44(6) 1_556 . ? C6 Rb1 C8 58.83(6) . . ? C5 Rb1 C8 43.83(6) . . ? O5 Rb1 C25 114.61(6) . . ? O3 Rb1 C25 86.55(7) 1_556 . ? C6 Rb1 C25 73.82(6) . . ? C5 Rb1 C25 95.03(6) . . ? C8 Rb1 C25 130.35(7) . . ? O5 Rb1 C20 70.33(8) . 1_556 ? O3 Rb1 C20 22.60(5) 1_556 1_556 ? C6 Rb1 C20 127.10(6) . 1_556 ? C5 Rb1 C20 116.09(6) . 1_556 ? C8 Rb1 C20 126.47(7) . 1_556 ? C25 Rb1 C20 92.85(7) . 1_556 ? O5 Rb1 C13 98.07(7) . . ? O3 Rb1 C13 140.68(6) 1_556 . ? C6 Rb1 C13 64.31(6) . . ? C5 Rb1 C13 58.79(6) . . ? C8 Rb1 C13 23.54(6) . . ? C25 Rb1 C13 121.75(7) . . ? C20 Rb1 C13 144.71(6) 1_556 . ? O5 Rb1 C1 168.05(6) . . ? O3 Rb1 C1 90.10(6) 1_556 . ? C6 Rb1 C1 23.24(6) . . ? C5 Rb1 C1 41.13(6) . . ? C8 Rb1 C1 81.56(6) . . ? C25 Rb1 C1 53.95(6) . . ? C20 Rb1 C1 111.24(6) 1_556 . ? C13 Rb1 C1 87.04(6) . . ? O5 Rb1 C9 92.23(6) . . ? O3 Rb1 C9 102.11(6) 1_556 . ? C6 Rb1 C9 77.80(6) . . ? C5 Rb1 C9 57.58(6) . . ? C8 Rb1 C9 22.96(6) . . ? C25 Rb1 C9 151.58(7) . . ? C20 Rb1 C9 105.55(7) 1_556 . ? C13 Rb1 C9 40.08(7) . . ? C1 Rb1 C9 98.56(6) . . ? O5 Rb1 C26 127.08(6) . . ? O3 Rb1 C26 104.10(6) 1_556 . ? C6 Rb1 C26 55.52(6) . . ? C5 Rb1 C26 78.99(6) . . ? C8 Rb1 C26 108.19(6) . . ? C25 Rb1 C26 22.91(7) . . ? C20 Rb1 C26 114.55(6) 1_556 . ? C13 Rb1 C26 99.17(6) . . ? C1 Rb1 C26 41.07(6) . . ? C9 Rb1 C26 130.65(6) . . ? O5 Rb1 C24 92.00(6) . . ? O3 Rb1 C24 89.71(6) 1_556 . ? C6 Rb1 C24 94.74(6) . . ? C5 Rb1 C24 117.18(6) . . ? C8 Rb1 C24 144.96(7) . . ? C25 Rb1 C24 22.73(6) . . ? C20 Rb1 C24 87.20(7) 1_556 . ? C13 Rb1 C24 127.30(7) . . ? C1 Rb1 C24 76.39(6) . . ? C9 Rb1 C24 167.24(7) . . ? C26 Rb1 C24 39.68(6) . . ? C6 O1 H01 111(2) . . ? C13 O2 H03 108(3) . . ? C20 O3 Rb1 101.45(17) . 1_554 ? C27 O4 H04 99(4) . . ? C27 O4 H04A 112(5) . . ? H04 O4 H04A 81(5) . . ? C29 O5 C32 109.3(2) . . ? C29 O5 Rb1 136.27(16) . . ? C32 O5 Rb1 114.29(15) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 C28 121.3(3) . . ? C6 C1 C28 119.5(2) . . ? C2 C1 Rb1 89.90(16) . . ? C6 C1 Rb1 70.76(13) . . ? C28 C1 Rb1 105.03(14) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 H2 117(2) . . ? C1 C2 H2 123(2) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 121(2) . . ? C2 C3 H3 119(2) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 Rb1 88.11(19) . . ? C5 C4 Rb1 68.97(16) . . ? C3 C4 H4 121(2) . . ? C5 C4 H4 118(2) . . ? Rb1 C4 H4 113(2) . . ? C4 C5 C6 118.3(3) . . ? C4 C5 C7 121.1(3) . . ? C6 C5 C7 120.5(2) . . ? C4 C5 Rb1 88.59(18) . . ? C6 C5 Rb1 76.41(14) . . ? C7 C5 Rb1 101.90(14) . . ? O1 C6 C1 117.9(2) . . ? O1 C6 C5 121.3(2) . . ? C1 C6 C5 120.9(2) . . ? O1 C6 Rb1 105.04(16) . . ? C1 C6 Rb1 85.99(14) . . ? C5 C6 Rb1 79.58(14) . . ? C5 C7 C8 112.6(2) . . ? C5 C7 H7A 106.1(15) . . ? C8 C7 H7A 110.2(15) . . ? C5 C7 H7B 103.0(16) . . ? C8 C7 H7B 107.8(15) . . ? H7A C7 H7B 117(2) . . ? C9 C8 C13 119.4(2) . . ? C9 C8 C7 119.9(3) . . ? C13 C8 C7 120.7(2) . . ? C9 C8 Rb1 85.15(15) . . ? C13 C8 Rb1 83.03(14) . . ? C7 C8 Rb1 101.63(15) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 Rb1 92.05(16) . . ? C8 C9 Rb1 71.89(14) . . ? C10 C9 H9 116.5(17) . . ? C8 C9 H9 122.3(18) . . ? Rb1 C9 H9 106.6(17) . . ? C11 C10 C9 118.8(3) . . ? C11 C10 H10 120.2(18) . . ? C9 C10 H10 121.0(18) . . ? C12 C11 C10 121.8(3) . . ? C12 C11 H11 120.8(17) . . ? C10 C11 H11 117.5(17) . . ? C11 C12 C13 119.3(3) . . ? C11 C12 C14 120.9(2) . . ? C13 C12 C14 119.8(2) . . ? O2 C13 C12 120.6(2) . . ? O2 C13 C8 120.1(2) . . ? C12 C13 C8 119.3(2) . . ? O2 C13 Rb1 102.53(14) . . ? C12 C13 Rb1 94.63(16) . . ? C8 C13 Rb1 73.43(14) . . ? C12 C14 C15 112.4(2) . . ? C12 C14 H14A 110.8(16) . . ? C15 C14 H14A 109.7(15) . . ? C12 C14 H14B 110(2) . . ? C15 C14 H14B 113.2(18) . . ? H14A C14 H14B 101(2) . . ? C16 C15 C20 118.5(2) . . ? C16 C15 C14 120.4(2) . . ? C20 C15 C14 121.0(2) . . ? C17 C16 C15 121.9(2) . . ? C17 C16 H16 118.9(15) . . ? C15 C16 H16 119.0(15) . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17 120.4(15) . . ? C16 C17 H17 120.3(14) . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 117.9(15) . . ? C19 C18 H18 120.8(14) . . ? C18 C19 C20 118.9(2) . . ? C18 C19 C21 120.6(2) . . ? C20 C19 C21 120.3(2) . . ? O3 C20 C19 118.7(2) . . ? O3 C20 C15 121.0(2) . . ? C19 C20 C15 120.3(2) . . ? O3 C20 Rb1 55.96(15) . 1_554 ? C19 C20 Rb1 109.82(17) . 1_554 ? C15 C20 Rb1 101.76(17) . 1_554 ? C19 C21 C22 110.1(2) . . ? C19 C21 H21A 113.4(17) . . ? C22 C21 H21A 105.7(19) . . ? C19 C21 H21B 111.5(18) . . ? C22 C21 H21B 108.9(18) . . ? H21A C21 H21B 107(3) . . ? C23 C22 C27 119.2(3) . . ? C23 C22 C21 119.5(3) . . ? C27 C22 C21 121.3(3) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H23 115.6(17) . . ? C22 C23 H23 123.3(17) . . ? C23 C24 C25 119.0(3) . . ? C23 C24 Rb1 92.87(16) . . ? C25 C24 Rb1 71.66(15) . . ? C23 C24 H24 124.7(17) . . ? C25 C24 H24 116.2(17) . . ? Rb1 C24 H24 106.3(17) . . ? C24 C25 C26 121.5(3) . . ? C24 C25 Rb1 85.62(16) . . ? C26 C25 Rb1 85.42(15) . . ? C24 C25 H25 122(2) . . ? C26 C25 H25 117(2) . . ? Rb1 C25 H25 93.3(19) . . ? C25 C26 C27 118.2(2) . . ? C25 C26 C28 119.6(3) . . ? C27 C26 C28 122.2(3) . . ? C25 C26 Rb1 71.68(14) . . ? C27 C26 Rb1 92.73(15) . . ? C28 C26 Rb1 103.19(15) . . ? O4 C27 C22 120.1(3) . . ? O4 C27 C26 118.9(2) . . ? C22 C27 C26 120.9(3) . . ? C1 C28 C26 110.5(2) . . ? C1 C28 H28A 105.6(15) . . ? C26 C28 H28A 106.3(14) . . ? C1 C28 H28B 107.7(18) . . ? C26 C28 H28B 113.0(19) . . ? H28A C28 H28B 114(2) . . ? O5 C29 C30 105.7(3) . . ? O5 C29 H29A 114(2) . . ? C30 C29 H29A 122(3) . . ? O5 C29 H29B 108(2) . . ? C30 C29 H29B 106(2) . . ? H29A C29 H29B 100(4) . . ? C29 C30 C31 103.0(3) . . ? C29 C30 H30A 117.5(19) . . ? C31 C30 H30A 117.0(18) . . ? C29 C30 H30B 107(2) . . ? C31 C30 H30B 111(2) . . ? H30A C30 H30B 101(3) . . ? C30 C31 C32 104.1(3) . . ? C30 C31 H31A 110(3) . . ? C32 C31 H31A 113(3) . . ? C30 C31 H31B 111(2) . . ? C32 C31 H31B 110(2) . . ? H31A C31 H31B 109(3) . . ? O5 C32 C31 106.3(2) . . ? O5 C32 Rb1 44.48(12) . . ? C31 C32 Rb1 150.8(2) . . ? O5 C32 H32A 114(2) . . ? C31 C32 H32A 106(2) . . ? Rb1 C32 H32A 91(2) . . ? O5 C32 H32B 110(3) . . ? C31 C32 H32B 114(3) . . ? Rb1 C32 H32B 82(3) . . ? H32A C32 H32B 107(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.692 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.057 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H29 Cs O5' _chemical_formula_weight 614.45 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' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 7.4016(7) _cell_length_b 19.4783(17) _cell_length_c 18.4508(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.882(2) _cell_angle_gamma 90.00 _cell_volume 2634.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.445 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14834 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5156 _reflns_number_gt 4625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 5156 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.010 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 Cs1 Cs -0.28245(3) 0.758943(11) 0.366627(11) 0.04554(12) Uani 1 1 d . . . O1 O 0.2658(4) 0.6301(2) 0.38015(11) 0.0780(10) Uani 1 1 d . . . O2 O 0.4667(3) 0.65031(12) 0.50533(12) 0.0482(5) Uani 1 1 d . . . O3 O 0.3628(4) 0.77374(14) 0.52028(18) 0.0669(8) Uani 1 1 d . . . O4 O 0.1401(4) 0.76324(12) 0.38665(15) 0.0546(6) Uani 1 1 d . . . O5 O -0.1763(4) 0.87890(17) 0.2836(2) 0.1026(12) Uani 1 1 d . . . C1 C 0.3761(4) 0.62081(16) 0.32785(14) 0.0391(6) Uani 1 1 d . . . C2 C 0.3317(4) 0.65400(15) 0.26003(15) 0.0399(6) Uani 1 1 d . . . C3 C 0.4434(5) 0.64371(17) 0.20609(17) 0.0520(8) Uani 1 1 d . . . H3A H 0.4129 0.6647 0.1595 0.062 Uiso 1 1 calc R . . C4 C 0.5991(6) 0.60311(18) 0.21955(19) 0.0616(10) Uani 1 1 d . . . H4A H 0.6774 0.5979 0.1832 0.074 Uiso 1 1 calc R . . C5 C 0.6389(5) 0.57010(16) 0.28705(17) 0.0507(8) Uani 1 1 d . . . H5A H 0.7438 0.5416 0.2959 0.061 Uiso 1 1 calc R . . C6 C 0.5284(4) 0.57810(14) 0.34132(15) 0.0392(6) Uani 1 1 d . . . C7 C 0.5774(4) 0.54349(15) 0.41521(15) 0.0435(7) Uani 1 1 d . . . H7A H 0.4650 0.5361 0.4377 0.052 Uiso 1 1 calc R . . H7B H 0.6322 0.4980 0.4082 0.052 Uiso 1 1 calc R . . C8 C 0.6490(3) 0.63902(15) 0.50870(14) 0.0343(6) Uani 1 1 d . . . C9 C 0.7097(4) 0.58600(15) 0.46603(15) 0.0387(6) Uani 1 1 d . . . C10 C 0.8983(4) 0.57721(18) 0.46840(17) 0.0515(8) Uani 1 1 d . . . H10A H 0.9423 0.5420 0.4397 0.062 Uiso 1 1 calc R . . C11 C 1.0215(4) 0.6181(2) 0.51113(18) 0.0560(9) Uani 1 1 d . . . H11A H 1.1488 0.6109 0.5122 0.067 Uiso 1 1 calc R . . C12 C 0.9593(4) 0.66948(19) 0.55228(17) 0.0486(8) Uani 1 1 d . . . H12A H 1.0448 0.6981 0.5812 0.058 Uiso 1 1 calc R . . C13 C 0.7736(4) 0.68053(16) 0.55261(15) 0.0372(6) Uani 1 1 d . . . C14 C 0.7109(4) 0.73711(16) 0.59940(17) 0.0410(7) Uani 1 1 d . . . H14A H 0.8050 0.7449 0.6422 0.049 Uiso 1 1 calc R . . H14B H 0.5973 0.7227 0.6178 0.049 Uiso 1 1 calc R . . C15 C 0.5028(4) 0.81835(16) 0.51866(16) 0.0421(7) Uani 1 1 d . . . C16 C 0.6764(4) 0.80396(16) 0.55671(14) 0.0388(6) Uani 1 1 d . . . C17 C 0.8191(4) 0.85003(17) 0.55207(16) 0.0451(7) Uani 1 1 d . . . H17A H 0.9373 0.8398 0.5767 0.054 Uiso 1 1 calc R . . C18 C 0.7921(4) 0.90975(17) 0.51276(16) 0.0476(7) Uani 1 1 d . . . H18A H 0.8905 0.9405 0.5102 0.057 Uiso 1 1 calc R . . C19 C 0.6173(5) 0.92498(17) 0.47634(17) 0.0484(7) Uani 1 1 d . . . H19A H 0.5972 0.9668 0.4499 0.058 Uiso 1 1 calc R . . C20 C 0.4743(4) 0.87972(16) 0.47863(15) 0.0426(7) Uani 1 1 d . . . C21 C 0.2886(4) 0.89463(18) 0.43416(17) 0.0530(8) Uani 1 1 d . . . H21A H 0.2658 0.9447 0.4329 0.064 Uiso 1 1 calc R . . H21B H 0.1912 0.8723 0.4575 0.064 Uiso 1 1 calc R . . C22 C 0.2183(3) 0.80142(16) 0.33664(15) 0.0371(6) Uani 1 1 d . . . C23 C 0.2854(4) 0.86731(16) 0.35585(18) 0.0420(7) Uani 1 1 d . . . C24 C 0.3568(4) 0.90580(17) 0.30378(18) 0.0524(8) Uani 1 1 d . . . H24A H 0.4010 0.9507 0.3161 0.063 Uiso 1 1 calc R . . C25 C 0.3661(5) 0.88117(19) 0.23461(19) 0.0540(8) Uani 1 1 d . . . H25A H 0.4147 0.9090 0.1997 0.065 Uiso 1 1 calc R . . C26 C 0.3047(4) 0.81619(17) 0.21615(16) 0.0453(7) Uani 1 1 d . . . H26A H 0.3134 0.7988 0.1687 0.054 Uiso 1 1 calc R . . C27 C 0.2293(4) 0.77522(17) 0.26686(16) 0.0393(6) Uani 1 1 d . . . C28 C 0.1710(4) 0.70210(18) 0.24662(18) 0.0495(8) Uani 1 1 d . . . H28A H 0.0759 0.6874 0.2762 0.059 Uiso 1 1 calc R . . H28B H 0.1181 0.7002 0.1944 0.059 Uiso 1 1 calc R . . C29 C -0.1307(5) 0.9537(2) 0.18870(19) 0.0636(9) Uani 1 1 d . . . H29A H -0.1609 0.9129 0.1583 0.095 Uiso 1 1 calc R . . H29B H -0.0074 0.9692 0.1831 0.095 Uiso 1 1 calc R . . H29C H -0.2184 0.9903 0.1733 0.095 Uiso 1 1 calc R . . C30 C -0.1387(4) 0.93650(18) 0.2659(2) 0.0539(9) Uani 1 1 d . . . C31 C -0.0989(6) 0.9927(2) 0.3210(2) 0.0756(12) Uani 1 1 d . . . H31A H -0.1092 0.9749 0.3699 0.113 Uiso 1 1 calc R . . H31B H -0.1866 1.0302 0.3093 0.113 Uiso 1 1 calc R . . H31C H 0.0250 1.0100 0.3197 0.113 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 Cs1 0.04466(17) 0.04513(17) 0.04861(17) -0.00164(7) 0.01279(11) -0.00810(7) O1 0.0814(18) 0.122(3) 0.0330(13) 0.0072(13) 0.0146(12) 0.0514(19) O2 0.0277(10) 0.0556(14) 0.0605(13) -0.0177(11) 0.0030(9) -0.0013(9) O3 0.0446(14) 0.0484(14) 0.098(2) 0.0024(14) -0.0256(13) -0.0077(11) O4 0.0563(16) 0.0597(16) 0.0499(15) 0.0013(10) 0.0154(12) -0.0056(11) O5 0.0507(16) 0.073(2) 0.183(3) 0.062(2) 0.0106(18) -0.0013(14) C1 0.0454(16) 0.0405(15) 0.0311(14) -0.0089(11) 0.0041(12) -0.0028(12) C2 0.0468(16) 0.0345(14) 0.0352(14) -0.0074(11) -0.0054(12) -0.0055(12) C3 0.074(2) 0.0416(17) 0.0416(17) 0.0072(13) 0.0123(15) 0.0011(16) C4 0.086(3) 0.052(2) 0.0538(19) 0.0135(16) 0.0341(18) 0.0153(19) C5 0.063(2) 0.0375(16) 0.0541(19) 0.0053(13) 0.0182(16) 0.0128(15) C6 0.0536(17) 0.0265(13) 0.0371(14) -0.0026(10) 0.0047(12) -0.0022(12) C7 0.0592(18) 0.0303(14) 0.0409(15) 0.0023(11) 0.0061(13) 0.0055(13) C8 0.0292(13) 0.0405(15) 0.0333(13) 0.0035(11) 0.0041(10) 0.0025(11) C9 0.0430(16) 0.0389(15) 0.0351(14) 0.0089(11) 0.0090(11) 0.0057(12) C10 0.0506(18) 0.056(2) 0.0516(18) 0.0098(15) 0.0206(15) 0.0164(15) C11 0.0289(15) 0.074(2) 0.067(2) 0.0175(18) 0.0127(14) 0.0045(15) C12 0.0303(14) 0.061(2) 0.0528(18) 0.0125(15) -0.0023(13) -0.0054(13) C13 0.0302(13) 0.0460(16) 0.0343(14) 0.0106(11) 0.0003(11) -0.0026(11) C14 0.0368(17) 0.0544(18) 0.0284(14) -0.0009(12) -0.0079(11) -0.0059(12) C15 0.0405(16) 0.0419(16) 0.0420(16) -0.0151(12) -0.0013(12) -0.0005(12) C16 0.0426(15) 0.0433(16) 0.0288(13) -0.0095(11) -0.0008(11) -0.0012(12) C17 0.0412(16) 0.0521(18) 0.0394(15) -0.0079(13) -0.0033(12) -0.0050(14) C18 0.0528(18) 0.0464(17) 0.0445(17) -0.0070(13) 0.0102(14) -0.0044(14) C19 0.064(2) 0.0390(16) 0.0434(16) -0.0070(13) 0.0108(14) 0.0109(15) C20 0.0484(16) 0.0384(15) 0.0396(15) -0.0131(12) 0.0014(12) 0.0127(13) C21 0.0524(18) 0.0477(18) 0.0567(19) -0.0130(15) -0.0004(15) 0.0233(15) C22 0.0260(12) 0.0448(16) 0.0389(14) 0.0033(12) -0.0015(10) 0.0079(11) C23 0.0343(15) 0.0395(16) 0.0488(17) -0.0007(13) -0.0065(12) 0.0146(12) C24 0.0481(18) 0.0423(17) 0.061(2) 0.0097(15) -0.0117(15) 0.0024(14) C25 0.0482(18) 0.056(2) 0.057(2) 0.0202(16) 0.0024(15) 0.0057(15) C26 0.0386(15) 0.058(2) 0.0364(15) 0.0065(13) -0.0036(12) 0.0131(14) C27 0.0278(13) 0.0458(16) 0.0398(16) 0.0005(12) -0.0117(11) 0.0084(12) C28 0.0432(17) 0.054(2) 0.0450(17) -0.0083(14) -0.0164(13) -0.0018(14) C29 0.061(2) 0.066(2) 0.063(2) -0.0128(18) 0.0034(17) 0.0044(19) C30 0.0280(14) 0.0496(19) 0.083(2) 0.0171(17) 0.0019(14) 0.0083(13) C31 0.085(3) 0.089(3) 0.050(2) 0.000(2) 0.0029(19) 0.030(2) _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 Cs1 O5 2.959(3) . ? Cs1 O4 3.100(3) . ? O1 C1 1.359(3) . ? O2 C8 1.360(3) . ? O3 C15 1.356(4) . ? O4 C22 1.373(4) . ? O5 C30 1.211(4) . ? C1 C6 1.396(4) . ? C1 C2 1.407(4) . ? C1 Cs1 3.693(3) 1_655 ? C2 C3 1.393(4) . ? C2 C28 1.508(4) . ? C2 Cs1 3.829(3) 1_655 ? C3 C4 1.392(5) . ? C4 C5 1.397(4) . ? C5 C6 1.386(4) . ? C6 C7 1.520(4) . ? C6 Cs1 3.796(3) 1_655 ? C7 C9 1.507(4) . ? C8 C13 1.398(4) . ? C8 C9 1.409(4) . ? C8 Cs1 3.599(3) 1_655 ? C9 C10 1.402(4) . ? C9 Cs1 3.840(3) 1_655 ? C10 C11 1.375(5) . ? C11 C12 1.373(5) . ? C12 C13 1.392(4) . ? C13 C14 1.512(4) . ? C13 Cs1 3.727(3) 1_655 ? C14 C16 1.525(4) . ? C15 C20 1.406(4) . ? C15 C16 1.405(4) . ? C15 Cs1 3.600(3) 1_655 ? C16 C17 1.397(4) . ? C16 Cs1 3.668(3) 1_655 ? C17 C18 1.371(5) . ? C17 Cs1 3.836(3) 1_655 ? C18 C19 1.405(5) . ? C19 C20 1.383(5) . ? C20 C21 1.529(4) . ? C20 Cs1 3.751(3) 1_655 ? C21 C23 1.537(4) . ? C22 C27 1.398(4) . ? C22 C23 1.404(4) . ? C22 Cs1 3.753(3) 1_655 ? C23 C24 1.380(5) . ? C23 Cs1 3.815(3) 1_655 ? C24 C25 1.374(5) . ? C25 C26 1.372(5) . ? C26 C27 1.403(4) . ? C27 C28 1.520(5) . ? C27 Cs1 3.838(3) 1_655 ? C29 C30 1.473(5) . ? C30 C31 1.495(6) . ? 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 O5 Cs1 O4 72.85(7) . . ? C22 O4 Cs1 116.48(19) . . ? C30 O5 Cs1 163.3(4) . . ? O1 C1 C6 120.1(3) . . ? O1 C1 C2 118.7(3) . . ? C6 C1 C2 121.1(3) . . ? O1 C1 Cs1 103.2(2) . 1_655 ? C6 C1 Cs1 83.41(17) . 1_655 ? C2 C1 Cs1 84.70(17) . 1_655 ? C3 C2 C1 118.7(3) . . ? C3 C2 C28 120.3(3) . . ? C1 C2 C28 120.9(3) . . ? C3 C2 Cs1 88.29(19) . 1_655 ? C1 C2 Cs1 73.84(15) . 1_655 ? C28 C2 Cs1 105.59(17) . 1_655 ? C4 C3 C2 120.8(3) . . ? C5 C4 C3 119.3(3) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C7 120.4(3) . . ? C1 C6 C7 120.8(3) . . ? C5 C6 Cs1 87.08(18) . 1_655 ? C1 C6 Cs1 75.17(16) . 1_655 ? C7 C6 Cs1 105.24(16) . 1_655 ? C9 C7 C6 111.7(2) . . ? O2 C8 C13 120.3(3) . . ? O2 C8 C9 118.9(3) . . ? C13 C8 C9 120.8(3) . . ? O2 C8 Cs1 95.73(16) . 1_655 ? C13 C8 Cs1 84.21(16) . 1_655 ? C9 C8 Cs1 88.92(16) . 1_655 ? C10 C9 C8 117.7(3) . . ? C10 C9 C7 120.8(3) . . ? C8 C9 C7 121.4(3) . . ? C10 C9 Cs1 92.40(19) . 1_655 ? C8 C9 Cs1 69.56(15) . 1_655 ? C7 C9 Cs1 103.65(16) . 1_655 ? C11 C10 C9 121.8(3) . . ? C12 C11 C10 119.5(3) . . ? C11 C12 C13 121.4(3) . . ? C8 C13 C12 118.8(3) . . ? C8 C13 C14 121.5(3) . . ? C12 C13 C14 119.7(3) . . ? C8 C13 Cs1 73.88(15) . 1_655 ? C12 C13 Cs1 92.56(17) . 1_655 ? C14 C13 Cs1 102.88(16) . 1_655 ? C13 C14 C16 111.7(2) . . ? O3 C15 C20 119.8(3) . . ? O3 C15 C16 120.7(3) . . ? C20 C15 C16 119.6(3) . . ? O3 C15 Cs1 103.4(2) . 1_655 ? C20 C15 Cs1 85.10(17) . 1_655 ? C16 C15 Cs1 81.60(17) . 1_655 ? C17 C16 C15 119.2(3) . . ? C17 C16 C14 120.4(3) . . ? C15 C16 C14 120.3(3) . . ? C17 C16 Cs1 86.13(17) . 1_655 ? C15 C16 Cs1 76.12(16) . 1_655 ? C14 C16 Cs1 105.06(18) . 1_655 ? C18 C17 C16 121.4(3) . . ? C18 C17 Cs1 85.64(17) . 1_655 ? C16 C17 Cs1 72.56(15) . 1_655 ? C17 C18 C19 119.4(3) . . ? C20 C19 C18 120.6(3) . . ? C19 C20 C15 119.8(3) . . ? C19 C20 C21 119.9(3) . . ? C15 C20 C21 120.2(3) . . ? C19 C20 Cs1 87.45(17) . 1_655 ? C15 C20 Cs1 72.97(16) . 1_655 ? C21 C20 Cs1 106.71(17) . 1_655 ? C20 C21 C23 109.6(2) . . ? O4 C22 C27 120.3(3) . . ? O4 C22 C23 119.5(3) . . ? C27 C22 C23 120.2(3) . . ? O4 C22 Cs1 106.19(18) . 1_655 ? C27 C22 Cs1 82.81(16) . 1_655 ? C23 C22 Cs1 81.79(16) . 1_655 ? O4 C22 Cs1 45.20(15) . . ? C27 C22 Cs1 103.24(18) . . ? C23 C22 Cs1 117.84(19) . . ? Cs1 C22 Cs1 149.96(8) 1_655 . ? C24 C23 C22 118.5(3) . . ? C24 C23 C21 120.6(3) . . ? C22 C23 C21 120.9(3) . . ? C24 C23 Cs1 86.46(19) . 1_655 ? C22 C23 Cs1 76.85(15) . 1_655 ? C21 C23 Cs1 103.75(16) . 1_655 ? C25 C24 C23 122.0(3) . . ? C24 C25 C26 119.7(3) . . ? C25 C26 C27 120.5(3) . . ? C22 C27 C26 119.0(3) . . ? C22 C27 C28 121.2(3) . . ? C26 C27 C28 119.7(3) . . ? C22 C27 Cs1 76.00(15) . 1_655 ? C26 C27 Cs1 86.10(17) . 1_655 ? C28 C27 Cs1 104.91(17) . 1_655 ? C2 C28 C27 110.5(2) . . ? O5 C30 C29 120.8(4) . . ? O5 C30 C31 121.8(4) . . ? C29 C30 C31 117.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.753 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.096 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H95 O9 Rb1' _chemical_formula_weight 1093.87 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' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 13.0013(6) _cell_length_b 13.0013(6) _cell_length_c 18.2767(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3089.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.85 _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 128(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19742 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3726 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1049P)^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 3726 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.2500 0.2500 0.48368(3) 0.0520(2) Uani 1 4 d S . . O1 O 0.31377(17) 0.12290(15) 0.62144(11) 0.0597(5) Uani 1 1 d . . . O2 O 0.42699(18) 0.18391(18) 0.41059(13) 0.0758(7) Uani 1 1 d . . . C1 C 0.3394(2) 0.07019(19) 0.68275(14) 0.0443(6) Uani 1 1 d . . . C2 C 0.2698(2) 0.00163(19) 0.71417(15) 0.0464(6) Uani 1 1 d . . . C3 C 0.2994(2) -0.0535(2) 0.77526(15) 0.0510(6) Uani 1 1 d . . . H3A H 0.2518 -0.1003 0.7964 0.061 Uiso 1 1 calc R . . C4 C 0.3955(2) -0.0433(2) 0.80686(15) 0.0526(7) Uani 1 1 d . . . C5 C 0.4625(2) 0.0262(2) 0.77510(14) 0.0495(6) Uani 1 1 d . . . H5A H 0.5290 0.0347 0.7959 0.059 Uiso 1 1 calc R . . C6 C 0.4367(2) 0.08389(19) 0.71430(15) 0.0464(6) Uani 1 1 d . . . C7 C 0.5123(2) 0.1617(2) 0.68404(17) 0.0559(7) Uani 1 1 d . . . H7A H 0.5051 0.1640 0.6301 0.067 Uiso 1 1 calc R . . H7B H 0.5830 0.1382 0.6952 0.067 Uiso 1 1 calc R . . C8 C 0.4251(3) -0.1108(3) 0.87355(17) 0.0702(9) Uani 1 1 d . . . C9 C 0.4216(3) -0.2250(3) 0.8516(2) 0.0877(12) Uani 1 1 d . . . H9A H 0.4719 -0.2378 0.8127 0.132 Uiso 1 1 calc R . . H9B H 0.3526 -0.2422 0.8340 0.132 Uiso 1 1 calc R . . H9C H 0.4383 -0.2677 0.8942 0.132 Uiso 1 1 calc R . . C10 C 0.3438(4) -0.0943(4) 0.9350(2) 0.1010(14) Uani 1 1 d . . . H10A H 0.3443 -0.0220 0.9502 0.151 Uiso 1 1 calc R . . H10B H 0.3605 -0.1381 0.9769 0.151 Uiso 1 1 calc R . . H10C H 0.2754 -0.1123 0.9164 0.151 Uiso 1 1 calc R . . C11 C 0.5294(4) -0.0835(5) 0.9042(2) 0.1190(18) Uani 1 1 d . . . H11A H 0.5304 -0.0106 0.9178 0.178 Uiso 1 1 calc R . . H11B H 0.5823 -0.0965 0.8671 0.178 Uiso 1 1 calc R . . H11C H 0.5433 -0.1257 0.9475 0.178 Uiso 1 1 calc R . . C12 C 0.4812(3) 0.1027(3) 0.4426(2) 0.0758(10) Uani 1 1 d . . . H12A H 0.4743 0.0395 0.4127 0.091 Uiso 1 1 calc R . . H12B H 0.4549 0.0885 0.4924 0.091 Uiso 1 1 calc R . . C13 C 0.5906(3) 0.1363(3) 0.44558(18) 0.0694(9) Uani 1 1 d . . . H13A H 0.6377 0.0776 0.4374 0.083 Uiso 1 1 calc R . . H13B H 0.6068 0.1682 0.4934 0.083 Uiso 1 1 calc R . . C14 C 0.5993(3) 0.2143(3) 0.38411(19) 0.0704(9) Uani 1 1 d . . . H14A H 0.6229 0.2818 0.4028 0.085 Uiso 1 1 calc R . . H14B H 0.6474 0.1903 0.3458 0.085 Uiso 1 1 calc R . . C15 C 0.4915(3) 0.2209(4) 0.3553(2) 0.0934(13) Uani 1 1 d . . . H15A H 0.4739 0.2930 0.3432 0.112 Uiso 1 1 calc R . . H15B H 0.4842 0.1786 0.3106 0.112 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 Rb1 0.0625(3) 0.0625(3) 0.0311(3) 0.000 0.000 0.000 O1 0.0662(13) 0.0460(11) 0.0668(12) 0.0062(9) 0.0040(10) 0.0161(9) O2 0.0725(15) 0.0741(15) 0.0808(15) 0.0127(13) 0.0189(12) 0.0120(12) C1 0.0495(14) 0.0368(12) 0.0466(13) -0.0097(10) 0.0082(11) 0.0089(11) C2 0.0450(14) 0.0392(13) 0.0552(15) -0.0199(11) 0.0053(12) -0.0021(11) C3 0.0476(15) 0.0512(15) 0.0543(15) -0.0096(13) 0.0133(12) -0.0073(12) C4 0.0535(16) 0.0596(17) 0.0447(14) -0.0089(12) 0.0086(12) -0.0054(13) C5 0.0418(14) 0.0552(16) 0.0515(15) -0.0100(12) 0.0048(11) -0.0016(12) C6 0.0425(14) 0.0405(13) 0.0563(15) -0.0107(11) 0.0181(12) 0.0043(11) C7 0.0444(15) 0.0505(16) 0.0727(18) -0.0053(14) 0.0275(13) 0.0010(12) C8 0.077(2) 0.084(2) 0.0502(17) 0.0079(15) 0.0029(15) -0.0092(18) C9 0.103(3) 0.084(3) 0.076(2) 0.019(2) 0.004(2) 0.012(2) C10 0.138(4) 0.113(3) 0.0519(19) 0.009(2) 0.027(2) -0.003(3) C11 0.109(4) 0.160(5) 0.088(3) 0.039(3) -0.037(3) -0.027(3) C12 0.091(3) 0.0601(19) 0.076(2) 0.0093(17) 0.024(2) 0.0038(18) C13 0.089(2) 0.0614(19) 0.0577(18) -0.0066(15) -0.0064(17) 0.0157(17) C14 0.080(2) 0.0580(19) 0.073(2) -0.0033(16) 0.0164(18) -0.0054(17) C15 0.106(3) 0.108(3) 0.066(2) 0.026(2) 0.022(2) 0.033(3) _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 Rb1 O2 2.796(2) 2 ? Rb1 O2 2.796(2) 4 ? Rb1 O2 2.796(2) 3 ? Rb1 O2 2.796(2) . ? Rb1 O1 3.124(2) 3 ? Rb1 O1 3.124(2) 2 ? Rb1 O1 3.124(2) . ? Rb1 O1 3.124(2) 4 ? Rb1 C12 3.643(4) 4 ? Rb1 C12 3.643(4) 3 ? Rb1 C12 3.643(4) . ? Rb1 C12 3.643(4) 2 ? O1 C1 1.355(3) . ? O2 C15 1.398(4) . ? O2 C12 1.398(4) . ? C1 C2 1.394(4) . ? C1 C6 1.401(4) . ? C2 C3 1.381(4) . ? C2 C7 1.520(4) 4 ? C3 C4 1.383(4) . ? C4 C5 1.384(4) . ? C4 C8 1.550(4) . ? C5 C6 1.382(4) . ? C6 C7 1.515(4) . ? C7 C2 1.520(4) 3 ? C8 C11 1.509(6) . ? C8 C9 1.538(5) . ? C8 C10 1.556(5) . ? C12 C13 1.489(5) . ? C13 C14 1.518(5) . ? C14 C15 1.500(5) . ? 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 O2 Rb1 O2 76.81(4) 2 4 ? O2 Rb1 O2 76.81(4) 2 3 ? O2 Rb1 O2 122.93(10) 4 3 ? O2 Rb1 O2 122.93(10) 2 . ? O2 Rb1 O2 76.81(4) 4 . ? O2 Rb1 O2 76.81(4) 3 . ? O2 Rb1 O1 137.64(6) 2 3 ? O2 Rb1 O1 140.00(7) 4 3 ? O2 Rb1 O1 90.23(6) 3 3 ? O2 Rb1 O1 91.79(6) . 3 ? O2 Rb1 O1 90.23(6) 2 2 ? O2 Rb1 O1 137.64(6) 4 2 ? O2 Rb1 O1 91.79(6) 3 2 ? O2 Rb1 O1 140.00(7) . 2 ? O1 Rb1 O1 49.48(4) 3 2 ? O2 Rb1 O1 140.00(7) 2 . ? O2 Rb1 O1 91.79(6) 4 . ? O2 Rb1 O1 137.64(6) 3 . ? O2 Rb1 O1 90.23(6) . . ? O1 Rb1 O1 49.48(4) 3 . ? O1 Rb1 O1 72.58(7) 2 . ? O2 Rb1 O1 91.79(6) 2 4 ? O2 Rb1 O1 90.23(6) 4 4 ? O2 Rb1 O1 140.00(7) 3 4 ? O2 Rb1 O1 137.64(6) . 4 ? O1 Rb1 O1 72.58(7) 3 4 ? O1 Rb1 O1 49.48(4) 2 4 ? O1 Rb1 O1 49.48(4) . 4 ? O2 Rb1 C12 73.88(8) 2 4 ? O2 Rb1 C12 20.07(7) 4 4 ? O2 Rb1 C12 137.92(8) 3 4 ? O2 Rb1 C12 94.62(7) . 4 ? O1 Rb1 C12 131.56(7) 3 4 ? O1 Rb1 C12 117.60(7) 2 4 ? O1 Rb1 C12 82.49(8) . 4 ? O1 Rb1 C12 70.68(7) 4 4 ? O2 Rb1 C12 94.62(7) 2 3 ? O2 Rb1 C12 137.92(8) 4 3 ? O2 Rb1 C12 20.07(7) 3 3 ? O2 Rb1 C12 73.88(8) . 3 ? O1 Rb1 C12 70.68(7) 3 3 ? O1 Rb1 C12 82.49(8) 2 3 ? O1 Rb1 C12 117.60(7) . 3 ? O1 Rb1 C12 131.56(7) 4 3 ? C12 Rb1 C12 156.19(12) 4 3 ? O2 Rb1 C12 137.92(8) 2 . ? O2 Rb1 C12 73.88(8) 4 . ? O2 Rb1 C12 94.62(7) 3 . ? O2 Rb1 C12 20.07(7) . . ? O1 Rb1 C12 82.49(8) 3 . ? O1 Rb1 C12 131.56(7) 2 . ? O1 Rb1 C12 70.68(7) . . ? O1 Rb1 C12 117.60(7) 4 . ? C12 Rb1 C12 87.56(2) 4 . ? C12 Rb1 C12 87.56(2) 3 . ? O2 Rb1 C12 20.07(7) 2 2 ? O2 Rb1 C12 94.62(7) 4 2 ? O2 Rb1 C12 73.88(8) 3 2 ? O2 Rb1 C12 137.92(8) . 2 ? O1 Rb1 C12 117.60(7) 3 2 ? O1 Rb1 C12 70.68(7) 2 2 ? O1 Rb1 C12 131.56(7) . 2 ? O1 Rb1 C12 82.49(8) 4 2 ? C12 Rb1 C12 87.56(2) 4 2 ? C12 Rb1 C12 87.56(2) 3 2 ? C12 Rb1 C12 156.19(12) . 2 ? C1 O1 Rb1 177.89(15) . . ? C15 O2 C12 105.0(3) . . ? C15 O2 Rb1 137.1(2) . . ? C12 O2 Rb1 116.60(18) . . ? O1 C1 C2 120.3(2) . . ? O1 C1 C6 119.9(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C7 119.3(2) . 4 ? C1 C2 C7 121.8(3) . 4 ? C2 C3 C4 122.7(3) . . ? C3 C4 C5 117.2(3) . . ? C3 C4 C8 119.9(3) . . ? C5 C4 C8 122.9(3) . . ? C6 C5 C4 122.6(3) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C7 119.8(3) . . ? C1 C6 C7 121.4(3) . . ? C6 C7 C2 114.0(2) . 3 ? C11 C8 C9 110.4(4) . . ? C11 C8 C4 112.4(3) . . ? C9 C8 C4 109.5(3) . . ? C11 C8 C10 108.1(3) . . ? C9 C8 C10 107.5(3) . . ? C4 C8 C10 108.7(3) . . ? O2 C12 C13 106.0(3) . . ? O2 C12 Rb1 43.33(14) . . ? C13 C12 Rb1 128.8(2) . . ? C12 C13 C14 103.9(3) . . ? C15 C14 C13 103.2(3) . . ? O2 C15 C14 106.7(3) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.375 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.078 #===END data_11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H54 Cl3 Li O9' _chemical_formula_weight 936.24 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' 'Li' 'Li' -0.0003 0.0001 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.0435(8) _cell_length_b 18.8487(12) _cell_length_c 22.2687(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.4370(10) _cell_angle_gamma 90.00 _cell_volume 4895.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2905 _exptl_absorpt_correction_T_max 0.3300 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20515 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6395 _reflns_number_gt 3289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1326P)^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 SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6395 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1441 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2339 _refine_ls_wR_factor_gt 0.2017 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 3.914 _refine_ls_shift/su_mean 0.015 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 Cl1 Cl 0.8320(3) 0.80547(12) 0.49281(12) 0.1358(11) Uani 1 1 d . . . Cl2 Cl 0.76347(18) 0.95050(12) 0.47784(10) 0.0989(8) Uani 1 1 d . . . Cl3 Cl 0.9836(2) 0.91387(17) 0.55145(12) 0.1469(12) Uani 1 1 d . . . Li1 Li 0.2652(8) 0.8754(5) 0.2199(4) 0.050(3) Uani 1 1 d . . . O1 O 0.3033(3) 0.86709(19) 0.14083(16) 0.0466(10) Uani 1 1 d . . . O2 O 0.4574(3) 0.9534(2) 0.12060(18) 0.0491(11) Uani 1 1 d . . . H2 H 0.3989 0.9346 0.1268 0.074 Uiso 1 1 calc R . . O3 O 0.6526(3) 0.95791(19) 0.20892(17) 0.0507(11) Uani 1 1 d . . . H3A H 0.5869 0.9609 0.1860 0.076 Uiso 1 1 calc R . . O4 O 0.6741(3) 0.8750(2) 0.32288(17) 0.0503(11) Uani 1 1 d . . . H4A H 0.6589 0.8568 0.3538 0.075 Uiso 1 1 calc R . . O5 O 0.6507(3) 0.7838(2) 0.22454(18) 0.0542(11) Uani 1 1 d . . . H5A H 0.5933 0.7845 0.1948 0.081 Uiso 1 1 calc R . . O6 O 0.4568(3) 0.7769(2) 0.13844(18) 0.0531(11) Uani 1 1 d . . . H6 H 0.4006 0.8039 0.1323 0.080 Uiso 1 1 calc R . . O7 O 0.3429(5) 0.9581(3) 0.2560(3) 0.1030(19) Uani 1 1 d . . . O8 O 0.3253(6) 0.8018(3) 0.2748(3) 0.134(3) Uani 1 1 d . . . O9 O 0.1035(5) 0.8843(4) 0.2014(2) 0.120(2) Uani 1 1 d . . . C1 C 0.2228(5) 0.8666(3) 0.0858(3) 0.0422(15) Uani 1 1 d . . . C2 C 0.1824(5) 0.8015(4) 0.0592(3) 0.0503(16) Uani 1 1 d . . . C3 C 0.1043(5) 0.8032(4) 0.0008(3) 0.0577(18) Uani 1 1 d . . . H3 H 0.0768 0.7601 -0.0185 0.069 Uiso 1 1 calc R . . C4 C 0.0670(5) 0.8652(4) -0.0291(3) 0.0614(19) Uani 1 1 d . . . H4 H 0.0159 0.8646 -0.0686 0.074 Uiso 1 1 calc R . . C5 C 0.1051(5) 0.9287(4) -0.0007(3) 0.0527(17) Uani 1 1 d . . . H5 H 0.0785 0.9715 -0.0207 0.063 Uiso 1 1 calc R . . C6 C 0.1825(5) 0.9302(3) 0.0572(3) 0.0453(15) Uani 1 1 d . . . C7 C 0.2186(5) 1.0002(3) 0.0895(3) 0.0549(17) Uani 1 1 d . . . H7A H 0.1513 1.0314 0.0819 0.066 Uiso 1 1 calc R . . H7B H 0.2428 0.9915 0.1342 0.066 Uiso 1 1 calc R . . C8 C 0.4277(5) 1.0139(3) 0.0859(2) 0.0412(15) Uani 1 1 d . . . C9 C 0.3138(5) 1.0393(3) 0.0704(2) 0.0473(16) Uani 1 1 d . . . C10 C 0.2943(6) 1.1015(4) 0.0368(3) 0.0620(19) Uani 1 1 d . . . H10 H 0.2198 1.1205 0.0264 0.074 Uiso 1 1 calc R . . C11 C 0.3799(7) 1.1370(3) 0.0180(3) 0.064(2) Uani 1 1 d . . . H11 H 0.3633 1.1789 -0.0055 0.077 Uiso 1 1 calc R . . C12 C 0.4901(6) 1.1105(3) 0.0339(3) 0.0559(17) Uani 1 1 d . . . H12 H 0.5485 1.1346 0.0210 0.067 Uiso 1 1 calc R . . C13 C 0.5162(5) 1.0491(3) 0.0684(2) 0.0447(15) Uani 1 1 d . . . C14 C 0.6371(5) 1.0208(3) 0.0862(3) 0.0499(16) Uani 1 1 d . . . H14A H 0.6746 1.0323 0.0531 0.060 Uiso 1 1 calc R . . H14B H 0.6341 0.9690 0.0893 0.060 Uiso 1 1 calc R . . C15 C 0.7120(5) 1.0183(3) 0.2042(3) 0.0400(14) Uani 1 1 d . . . C16 C 0.7100(5) 1.0501(3) 0.1473(3) 0.0410(14) Uani 1 1 d . . . C17 C 0.7766(5) 1.1097(3) 0.1472(3) 0.0510(17) Uani 1 1 d . . . H17 H 0.7762 1.1317 0.1093 0.061 Uiso 1 1 calc R . . C18 C 0.8433(5) 1.1376(3) 0.2012(3) 0.0618(19) Uani 1 1 d . . . H18 H 0.8881 1.1782 0.2003 0.074 Uiso 1 1 calc R . . C19 C 0.8437(5) 1.1049(3) 0.2570(3) 0.0534(17) Uani 1 1 d . . . H19 H 0.8889 1.1241 0.2941 0.064 Uiso 1 1 calc R . . C20 C 0.7803(5) 1.0456(3) 0.2597(3) 0.0393(14) Uani 1 1 d . . . C21 C 0.7827(5) 1.0089(3) 0.3203(3) 0.0510(16) Uani 1 1 d . . . H21A H 0.8174 1.0411 0.3544 0.061 Uiso 1 1 calc R . . H21B H 0.7035 1.0002 0.3224 0.061 Uiso 1 1 calc R . . C22 C 0.7911(5) 0.8749(3) 0.3302(2) 0.0399(14) Uani 1 1 d . . . C23 C 0.8466(5) 0.9398(3) 0.3305(2) 0.0409(14) Uani 1 1 d . . . C24 C 0.9651(5) 0.9383(3) 0.3391(2) 0.0495(16) Uani 1 1 d . . . H24 H 1.0043 0.9814 0.3384 0.059 Uiso 1 1 calc R . . C25 C 1.0266(5) 0.8766(4) 0.3483(3) 0.0531(16) Uani 1 1 d . . . H25 H 1.1068 0.8773 0.3549 0.064 Uiso 1 1 calc R . . C26 C 0.9692(5) 0.8133(3) 0.3479(2) 0.0495(16) Uani 1 1 d . . . H26 H 1.0110 0.7706 0.3540 0.059 Uiso 1 1 calc R . . C27 C 0.8505(5) 0.8112(3) 0.3386(2) 0.0420(15) Uani 1 1 d . . . C28 C 0.7901(5) 0.7403(3) 0.3376(2) 0.0473(16) Uani 1 1 d . . . H28A H 0.8316 0.7117 0.3728 0.057 Uiso 1 1 calc R . . H28B H 0.7126 0.7486 0.3427 0.057 Uiso 1 1 calc R . . C29 C 0.7133(5) 0.7235(3) 0.2217(3) 0.0391(14) Uani 1 1 d . . . C30 C 0.7818(5) 0.6991(3) 0.2784(3) 0.0437(15) Uani 1 1 d . . . C31 C 0.8431(5) 0.6373(3) 0.2779(3) 0.0563(17) Uani 1 1 d . . . H31 H 0.8881 0.6191 0.3154 0.068 Uiso 1 1 calc R . . C32 C 0.8395(5) 0.6018(3) 0.2234(3) 0.0612(18) Uani 1 1 d . . . H32 H 0.8806 0.5593 0.2241 0.073 Uiso 1 1 calc R . . C33 C 0.7752(5) 0.6286(3) 0.1674(3) 0.0517(16) Uani 1 1 d . . . H33 H 0.7749 0.6049 0.1302 0.062 Uiso 1 1 calc R . . C34 C 0.7115(5) 0.6902(3) 0.1659(3) 0.0430(15) Uani 1 1 d . . . C35 C 0.6463(5) 0.7204(3) 0.1047(3) 0.0511(16) Uani 1 1 d . . . H35A H 0.6422 0.7720 0.1090 0.061 Uiso 1 1 calc R . . H35B H 0.6904 0.7110 0.0740 0.061 Uiso 1 1 calc R . . C36 C 0.4341(5) 0.7225(3) 0.0970(3) 0.0434(15) Uani 1 1 d . . . C37 C 0.5273(5) 0.6928(3) 0.0797(3) 0.0454(15) Uani 1 1 d . . . C38 C 0.5047(6) 0.6373(3) 0.0379(3) 0.0617(19) Uani 1 1 d . . . H38 H 0.5662 0.6160 0.0256 0.074 Uiso 1 1 calc R . . C39 C 0.3964(7) 0.6121(3) 0.0138(3) 0.070(2) Uani 1 1 d . . . H39 H 0.3842 0.5746 -0.0149 0.084 Uiso 1 1 calc R . . C40 C 0.3056(6) 0.6416(3) 0.0314(3) 0.0610(18) Uani 1 1 d . . . H40 H 0.2315 0.6233 0.0152 0.073 Uiso 1 1 calc R . . C41 C 0.3205(5) 0.6978(3) 0.0727(3) 0.0499(16) Uani 1 1 d . . . C42 C 0.2207(5) 0.7317(3) 0.0914(3) 0.0578(18) Uani 1 1 d . . . H42A H 0.2420 0.7397 0.1363 0.069 Uiso 1 1 calc R . . H42B H 0.1558 0.6987 0.0822 0.069 Uiso 1 1 calc R . . C43 C 0.4092(6) 0.9950(4) 0.2905(3) 0.066(2) Uani 1 1 d . . . C44 C 0.4524(8) 0.9786(4) 0.3579(3) 0.100(3) Uani 1 1 d . . . H44A H 0.3939 0.9530 0.3722 0.150 Uiso 1 1 calc R . . H44B H 0.4703 1.0225 0.3811 0.150 Uiso 1 1 calc R . . H44C H 0.5209 0.9497 0.3643 0.150 Uiso 1 1 calc R . . C45 C 0.4544(6) 1.0586(4) 0.2670(4) 0.083(2) Uani 1 1 d . . . H45A H 0.5228 1.0464 0.2537 0.125 Uiso 1 1 calc R . . H45B H 0.4733 1.0940 0.2996 0.125 Uiso 1 1 calc R . . H45C H 0.3970 1.0776 0.2321 0.125 Uiso 1 1 calc R . . C46 C 0.3861(7) 0.7642(4) 0.3135(4) 0.081(2) Uani 1 1 d . . . C47 C 0.3991(11) 0.7772(5) 0.3796(4) 0.169(5) Uani 1 1 d . . . H47A H 0.3363 0.8066 0.3852 0.253 Uiso 1 1 calc R . . H47B H 0.4713 0.8014 0.3966 0.253 Uiso 1 1 calc R . . H47C H 0.3985 0.7324 0.4009 0.253 Uiso 1 1 calc R . . C48 C 0.4430(6) 0.7026(4) 0.2956(4) 0.098(3) Uani 1 1 d . . . H48A H 0.4571 0.7107 0.2551 0.148 Uiso 1 1 calc R . . H48B H 0.3945 0.6612 0.2939 0.148 Uiso 1 1 calc R . . H48C H 0.5153 0.6948 0.3258 0.148 Uiso 1 1 calc R . . C49 C 0.0127(7) 0.8693(4) 0.1815(3) 0.064(2) Uani 1 1 d . . . C50 C -0.0184(13) 0.7937(6) 0.1768(5) 0.214(7) Uani 1 1 d . . . H50A H -0.0640 0.7835 0.1352 0.321 Uiso 1 1 calc R . . H50B H -0.0624 0.7826 0.2066 0.321 Uiso 1 1 calc R . . H50C H 0.0508 0.7651 0.1854 0.321 Uiso 1 1 calc R . . C51 C -0.0802(14) 0.9145(9) 0.1606(6) 0.307(12) Uani 1 1 d . . . H51A H -0.1467 0.8955 0.1723 0.460 Uiso 1 1 calc R . . H51B H -0.0966 0.9186 0.1158 0.460 Uiso 1 1 calc R . . H51C H -0.0620 0.9610 0.1792 0.460 Uiso 1 1 calc R . . C52 C 0.8760(6) 0.8918(4) 0.4874(3) 0.071(2) Uani 1 1 d . . . H52 H 0.9074 0.8953 0.4504 0.085 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 Cl1 0.207(3) 0.0947(17) 0.148(2) 0.0069(15) 0.125(2) 0.0017(18) Cl2 0.0766(14) 0.1168(17) 0.1057(17) 0.0173(13) 0.0269(12) 0.0246(13) Cl3 0.107(2) 0.206(3) 0.1024(19) -0.0383(19) -0.0211(15) 0.043(2) Li1 0.038(6) 0.060(7) 0.050(6) -0.002(5) 0.010(5) 0.003(5) O1 0.032(2) 0.069(3) 0.035(2) -0.0046(19) 0.0007(19) 0.004(2) O2 0.033(2) 0.056(3) 0.057(3) 0.016(2) 0.009(2) 0.009(2) O3 0.050(3) 0.048(3) 0.050(3) 0.009(2) 0.003(2) -0.011(2) O4 0.037(3) 0.061(3) 0.056(3) 0.008(2) 0.018(2) 0.001(2) O5 0.046(3) 0.056(3) 0.053(3) 0.000(2) -0.003(2) 0.010(2) O6 0.035(2) 0.058(3) 0.061(3) -0.010(2) 0.002(2) 0.007(2) O7 0.110(4) 0.078(4) 0.110(5) -0.046(3) 0.006(4) -0.022(3) O8 0.158(6) 0.090(4) 0.123(5) 0.061(4) -0.023(4) -0.006(4) O9 0.047(4) 0.250(8) 0.066(4) -0.014(4) 0.022(3) -0.009(4) C1 0.023(3) 0.070(5) 0.033(4) -0.005(3) 0.005(3) 0.006(3) C2 0.026(3) 0.084(5) 0.040(4) -0.009(4) 0.006(3) -0.006(3) C3 0.038(4) 0.084(5) 0.048(4) -0.018(4) 0.006(3) -0.009(4) C4 0.031(4) 0.106(6) 0.040(4) -0.008(4) -0.005(3) 0.007(4) C5 0.024(3) 0.095(5) 0.036(4) -0.006(4) 0.003(3) 0.009(3) C6 0.028(3) 0.071(5) 0.036(4) -0.008(3) 0.006(3) 0.010(3) C7 0.035(4) 0.077(5) 0.050(4) -0.002(4) 0.006(3) 0.023(3) C8 0.047(4) 0.041(4) 0.031(3) 0.000(3) 0.003(3) 0.009(3) C9 0.056(4) 0.050(4) 0.031(3) -0.005(3) 0.001(3) 0.022(3) C10 0.068(5) 0.058(5) 0.049(4) -0.008(4) -0.005(4) 0.023(4) C11 0.088(6) 0.050(4) 0.044(4) 0.006(3) -0.003(4) 0.010(4) C12 0.077(5) 0.046(4) 0.040(4) -0.002(3) 0.007(3) -0.004(4) C13 0.051(4) 0.050(4) 0.030(3) -0.010(3) 0.002(3) -0.001(3) C14 0.062(4) 0.053(4) 0.040(4) -0.005(3) 0.023(3) -0.006(3) C15 0.032(3) 0.039(4) 0.052(4) -0.006(3) 0.016(3) -0.002(3) C16 0.038(4) 0.041(4) 0.049(4) -0.003(3) 0.020(3) 0.003(3) C17 0.038(4) 0.055(4) 0.064(5) 0.012(3) 0.020(3) -0.002(3) C18 0.049(4) 0.054(4) 0.079(5) 0.011(4) 0.009(4) -0.022(3) C19 0.042(4) 0.055(4) 0.057(4) -0.004(3) -0.001(3) -0.011(3) C20 0.030(3) 0.039(4) 0.048(4) -0.002(3) 0.008(3) -0.003(3) C21 0.048(4) 0.056(4) 0.049(4) -0.007(3) 0.010(3) 0.001(3) C22 0.029(3) 0.055(4) 0.036(3) 0.005(3) 0.007(3) -0.001(3) C23 0.030(4) 0.054(4) 0.037(3) -0.001(3) 0.004(3) -0.001(3) C24 0.042(4) 0.061(5) 0.045(4) 0.000(3) 0.009(3) -0.010(4) C25 0.035(4) 0.065(5) 0.059(4) 0.002(3) 0.011(3) 0.000(4) C26 0.044(4) 0.061(4) 0.038(4) 0.003(3) 0.000(3) 0.011(4) C27 0.040(4) 0.052(4) 0.031(3) 0.005(3) 0.004(3) 0.003(3) C28 0.039(4) 0.056(4) 0.042(4) 0.008(3) 0.002(3) -0.004(3) C29 0.031(3) 0.035(4) 0.051(4) 0.012(3) 0.010(3) 0.005(3) C30 0.033(4) 0.044(4) 0.054(4) 0.004(3) 0.012(3) -0.002(3) C31 0.041(4) 0.054(4) 0.067(5) 0.011(4) 0.001(3) 0.007(3) C32 0.042(4) 0.056(4) 0.077(5) -0.013(4) 0.000(4) 0.015(3) C33 0.035(4) 0.066(4) 0.058(4) -0.005(3) 0.020(3) 0.004(4) C34 0.033(4) 0.055(4) 0.045(4) 0.005(3) 0.016(3) 0.000(3) C35 0.053(4) 0.060(4) 0.047(4) 0.007(3) 0.025(3) 0.002(3) C36 0.049(4) 0.043(4) 0.038(4) 0.007(3) 0.011(3) 0.000(3) C37 0.056(4) 0.047(4) 0.035(4) 0.004(3) 0.013(3) -0.001(3) C38 0.065(5) 0.076(5) 0.045(4) 0.001(4) 0.017(4) 0.003(4) C39 0.090(6) 0.063(5) 0.056(5) -0.019(4) 0.019(4) -0.007(4) C40 0.060(5) 0.069(5) 0.050(4) -0.006(4) 0.007(4) -0.014(4) C41 0.046(4) 0.054(4) 0.050(4) 0.005(3) 0.012(3) -0.004(3) C42 0.049(4) 0.069(5) 0.056(4) -0.004(4) 0.014(3) -0.017(4) C43 0.072(5) 0.045(5) 0.078(6) -0.020(4) 0.016(4) 0.008(4) C44 0.133(8) 0.095(6) 0.067(6) -0.005(5) 0.014(5) 0.005(5) C45 0.079(6) 0.069(5) 0.111(6) 0.001(5) 0.040(5) 0.015(4) C46 0.104(7) 0.045(5) 0.084(6) 0.015(4) 0.002(5) -0.018(5) C47 0.298(16) 0.086(7) 0.088(8) -0.019(6) -0.014(8) 0.028(8) C48 0.076(6) 0.092(6) 0.135(8) 0.007(5) 0.040(5) -0.010(5) C49 0.042(4) 0.100(6) 0.055(5) -0.002(4) 0.020(4) 0.010(5) C50 0.34(2) 0.187(12) 0.128(10) -0.038(8) 0.079(11) -0.161(13) C51 0.34(2) 0.44(2) 0.128(11) 0.006(13) 0.033(12) 0.32(2) C52 0.067(5) 0.088(5) 0.059(5) 0.001(4) 0.016(4) 0.011(4) _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 Cl1 C52 1.726(7) . ? Cl2 C52 1.720(7) . ? Cl3 C52 1.723(7) . ? Li1 O8 1.872(11) . ? Li1 O7 1.891(11) . ? Li1 O9 1.895(11) . ? Li1 O1 1.933(10) . ? O1 C1 1.360(6) . ? O2 C8 1.375(6) . ? O3 C15 1.363(6) . ? O4 C22 1.377(6) . ? O5 C29 1.375(6) . ? O6 C36 1.360(6) . ? O7 C43 1.185(7) . ? O8 C46 1.211(8) . ? O9 C49 1.110(7) . ? C1 C6 1.386(7) . ? C1 C2 1.396(7) . ? C2 C3 1.403(8) . ? C2 C42 1.513(8) . ? C3 C4 1.364(8) . ? C4 C5 1.378(8) . ? C5 C6 1.391(7) . ? C6 C7 1.513(7) . ? C7 C9 1.510(8) . ? C8 C13 1.391(8) . ? C8 C9 1.411(8) . ? C9 C10 1.381(8) . ? C10 C11 1.379(9) . ? C11 C12 1.379(9) . ? C12 C13 1.382(8) . ? C13 C14 1.508(8) . ? C14 C16 1.527(7) . ? C15 C16 1.395(7) . ? C15 C20 1.402(7) . ? C16 C17 1.381(7) . ? C17 C18 1.373(8) . ? C18 C19 1.387(8) . ? C19 C20 1.363(7) . ? C20 C21 1.511(7) . ? C21 C23 1.501(7) . ? C22 C27 1.387(7) . ? C22 C23 1.392(7) . ? C23 C24 1.392(7) . ? C24 C25 1.366(7) . ? C25 C26 1.379(8) . ? C26 C27 1.393(8) . ? C27 C28 1.518(7) . ? C28 C30 1.512(7) . ? C29 C34 1.386(7) . ? C29 C30 1.403(7) . ? C30 C31 1.381(7) . ? C31 C32 1.377(8) . ? C32 C33 1.388(8) . ? C33 C34 1.388(7) . ? C34 C35 1.505(7) . ? C35 C37 1.495(8) . ? C36 C37 1.392(8) . ? C36 C41 1.419(8) . ? C37 C38 1.383(8) . ? C38 C39 1.365(9) . ? C39 C40 1.369(9) . ? C40 C41 1.384(8) . ? C41 C42 1.509(8) . ? C43 C45 1.467(9) . ? C43 C44 1.494(9) . ? C46 C48 1.454(10) . ? C46 C47 1.462(11) . ? C49 C51 1.391(12) . ? C49 C50 1.471(11) . ? 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 O8 Li1 O7 105.3(5) . . ? O8 Li1 O9 114.6(6) . . ? O7 Li1 O9 113.1(5) . . ? O8 Li1 O1 113.2(5) . . ? O7 Li1 O1 104.5(5) . . ? O9 Li1 O1 105.9(5) . . ? C1 O1 Li1 122.9(4) . . ? C43 O7 Li1 160.2(6) . . ? C46 O8 Li1 164.9(7) . . ? C49 O9 Li1 157.1(8) . . ? O1 C1 C6 119.8(5) . . ? O1 C1 C2 118.8(5) . . ? C6 C1 C2 121.4(5) . . ? C1 C2 C3 117.1(6) . . ? C1 C2 C42 122.1(5) . . ? C3 C2 C42 120.9(6) . . ? C4 C3 C2 122.4(6) . . ? C3 C4 C5 119.2(6) . . ? C4 C5 C6 120.9(6) . . ? C1 C6 C5 118.9(6) . . ? C1 C6 C7 120.7(5) . . ? C5 C6 C7 120.3(6) . . ? C9 C7 C6 116.1(5) . . ? O2 C8 C13 116.3(5) . . ? O2 C8 C9 121.3(5) . . ? C13 C8 C9 122.4(5) . . ? C10 C9 C8 116.3(6) . . ? C10 C9 C7 121.9(6) . . ? C8 C9 C7 121.8(5) . . ? C11 C10 C9 122.6(6) . . ? C12 C11 C10 119.3(6) . . ? C11 C12 C13 121.2(6) . . ? C12 C13 C8 118.1(6) . . ? C12 C13 C14 120.9(6) . . ? C8 C13 C14 121.0(5) . . ? C13 C14 C16 114.3(4) . . ? O3 C15 C16 122.6(5) . . ? O3 C15 C20 116.2(5) . . ? C16 C15 C20 121.1(5) . . ? C17 C16 C15 118.2(5) . . ? C17 C16 C14 119.8(5) . . ? C15 C16 C14 122.0(5) . . ? C18 C17 C16 121.5(6) . . ? C17 C18 C19 119.0(6) . . ? C20 C19 C18 121.8(6) . . ? C19 C20 C15 118.3(5) . . ? C19 C20 C21 121.9(5) . . ? C15 C20 C21 119.8(5) . . ? C23 C21 C20 115.3(5) . . ? O4 C22 C27 119.6(5) . . ? O4 C22 C23 118.4(5) . . ? C27 C22 C23 121.9(5) . . ? C22 C23 C24 117.3(5) . . ? C22 C23 C21 122.2(5) . . ? C24 C23 C21 120.5(5) . . ? C25 C24 C23 122.4(6) . . ? C24 C25 C26 118.9(6) . . ? C25 C26 C27 121.4(6) . . ? C22 C27 C26 118.1(5) . . ? C22 C27 C28 122.1(5) . . ? C26 C27 C28 119.8(5) . . ? C30 C28 C27 113.1(5) . . ? O5 C29 C34 122.0(5) . . ? O5 C29 C30 115.8(5) . . ? C34 C29 C30 122.2(5) . . ? C31 C30 C29 117.6(6) . . ? C31 C30 C28 121.5(5) . . ? C29 C30 C28 120.9(5) . . ? C32 C31 C30 121.2(6) . . ? C31 C32 C33 120.2(6) . . ? C34 C33 C32 120.5(6) . . ? C29 C34 C33 118.2(5) . . ? C29 C34 C35 121.9(5) . . ? C33 C34 C35 119.9(5) . . ? C37 C35 C34 116.1(5) . . ? O6 C36 C37 116.8(5) . . ? O6 C36 C41 121.2(5) . . ? C37 C36 C41 122.0(6) . . ? C38 C37 C36 117.0(6) . . ? C38 C37 C35 121.5(6) . . ? C36 C37 C35 121.5(5) . . ? C39 C38 C37 122.4(6) . . ? C38 C39 C40 120.0(6) . . ? C39 C40 C41 121.3(6) . . ? C40 C41 C36 117.3(6) . . ? C40 C41 C42 121.8(6) . . ? C36 C41 C42 121.0(6) . . ? C41 C42 C2 114.1(5) . . ? O7 C43 C45 119.9(7) . . ? O7 C43 C44 122.7(7) . . ? C45 C43 C44 117.4(7) . . ? O8 C46 C48 120.9(8) . . ? O8 C46 C47 120.9(9) . . ? C48 C46 C47 118.1(8) . . ? O9 C49 C51 127.5(12) . . ? O9 C49 C50 118.9(9) . . ? C51 C49 C50 113.6(12) . . ? Cl2 C52 Cl3 110.8(4) . . ? Cl2 C52 Cl1 111.6(4) . . ? Cl3 C52 Cl1 110.5(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.481 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.066 #===END data_15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H45 Cs O9' _chemical_formula_weight 862.72 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' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.693(2) _cell_length_b 20.271(3) _cell_length_c 24.076(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7659.0(18) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'elongated p' _exptl_crystal_colour colorless _exptl_crystal_size_max .34 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type integration (Face indexed) _exptl_absorpt_correction_T_min 0.8237 _exptl_absorpt_correction_T_max 0.9549 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27538 _diffrn_reflns_av_R_equivalents 0.1970 _diffrn_reflns_av_sigmaI/netI 0.1518 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 21.50 _reflns_number_total 4396 _reflns_number_gt 2095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1004P)^2^+138.0530P] 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 SHELXL _refine_ls_extinction_coef 0.00000(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4396 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2912 _refine_ls_wR_factor_gt 0.2290 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 4.422 _refine_ls_shift/su_mean 0.023 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 Cs1 Cs 0.69668(10) 0.15089(7) 0.70656(6) 0.0652(7) Uani 1 1 d . . . O1 O 0.8799(12) 0.1088(7) 0.6367(8) 0.075(6) Uani 1 1 d . . . O2 O 0.9548(8) 0.1929(6) 0.7091(6) 0.040(4) Uani 1 1 d . . . O3 O 0.8832(9) 0.1197(7) 0.7847(6) 0.038(4) Uani 1 1 d . . . O4 O 0.6047(11) 0.0397(6) 0.7688(6) 0.036(4) Uani 1 1 d . . . O5 O 0.4790(9) 0.0263(6) 0.6959(5) 0.037(3) Uani 1 1 d . . . O6 O 0.6058(10) 0.0410(7) 0.6288(5) 0.062(5) Uani 1 1 d . . . O7 O 0.6063(11) 0.2473(9) 0.6337(8) 0.084(6) Uani 1 1 d . . . O8 O 0.004(3) 0.046(2) 0.531(2) 0.29(2) Uani 1 1 d . . . O9 O 0.912(5) 0.964(5) 0.530(4) 0.60(6) Uani 1 1 d . . . C1 C 0.8412(15) 0.1357(9) 0.5939(9) 0.045(6) Uani 1 1 d . . . C2 C 0.7801(12) 0.0946(9) 0.5676(7) 0.035(5) Uani 1 1 d . . . C3 C 0.7337(12) 0.1201(10) 0.5237(7) 0.037(5) Uani 1 1 d . . . H3 H 0.6898 0.0953 0.5083 0.044 Uiso 1 1 calc R . . C4 C 0.7513(14) 0.1802(9) 0.5033(7) 0.039(5) Uani 1 1 d . . . H4 H 0.7240 0.1955 0.4715 0.047 Uiso 1 1 calc R . . C5 C 0.8097(14) 0.2182(9) 0.5298(8) 0.041(5) Uani 1 1 d . . . H5 H 0.8175 0.2612 0.5173 0.049 Uiso 1 1 calc R . . C6 C 0.8580(13) 0.1973(9) 0.5741(8) 0.037(5) Uani 1 1 d . . . C7 C 0.9246(14) 0.2421(10) 0.6028(8) 0.050(6) Uani 1 1 d . . . H7A H 0.9738 0.2160 0.6133 0.061 Uiso 1 1 calc R . . H7B H 0.9434 0.2758 0.5769 0.061 Uiso 1 1 calc R . . C8 C 0.8869(13) 0.2748(10) 0.6542(8) 0.046(6) Uani 1 1 d . . . C9 C 0.8429(13) 0.3315(9) 0.6501(9) 0.047(6) Uani 1 1 d . . . H9 H 0.8345 0.3506 0.6155 0.056 Uiso 1 1 calc R . . C10 C 0.8098(15) 0.3619(10) 0.6977(9) 0.067(7) Uani 1 1 d . . . H10 H 0.7777 0.4003 0.6941 0.081 Uiso 1 1 calc R . . C11 C 0.8243(11) 0.3353(9) 0.7500(8) 0.034(5) Uani 1 1 d . . . H11 H 0.8010 0.3549 0.7815 0.041 Uiso 1 1 calc R . . C12 C 0.8738(11) 0.2793(9) 0.7546(8) 0.033(5) Uani 1 1 d . . . C13 C 0.9045(12) 0.2491(10) 0.7066(9) 0.046(5) Uani 1 1 d . . . C14 C 0.8948(12) 0.2533(9) 0.8120(7) 0.035(5) Uiso 1 1 d . . . H14A H 0.9485 0.2297 0.8104 0.042 Uiso 1 1 calc R . . H14B H 0.9021 0.2904 0.8370 0.042 Uiso 1 1 calc R . . C15 C 0.8273(11) 0.2081(9) 0.8352(7) 0.028(5) Uani 1 1 d . . . C16 C 0.8235(11) 0.1403(9) 0.8216(6) 0.022(4) Uani 1 1 d . . . C17 C 0.7586(13) 0.1002(9) 0.8403(7) 0.030(5) Uani 1 1 d . . . C18 C 0.6985(16) 0.1245(8) 0.8720(9) 0.052(6) Uani 1 1 d . . . H18 H 0.6541 0.0973 0.8834 0.063 Uiso 1 1 calc R . . C19 C 0.6996(13) 0.1937(9) 0.8900(7) 0.035(5) Uiso 1 1 d . . . H19 H 0.6586 0.2102 0.9142 0.042 Uiso 1 1 calc R . . C20 C 0.7644(12) 0.2335(9) 0.8694(7) 0.037(5) Uani 1 1 d . . . H20 H 0.7655 0.2780 0.8787 0.044 Uiso 1 1 calc R . . C21 C 0.7584(12) 0.0295(9) 0.8230(8) 0.037(5) Uani 1 1 d . . . H21A H 0.7633 0.0277 0.7829 0.044 Uiso 1 1 calc R . . H21B H 0.8088 0.0086 0.8384 0.044 Uiso 1 1 calc R . . C22 C 0.6826(12) -0.0102(8) 0.8397(7) 0.028(5) Uani 1 1 d . . . C23 C 0.6044(12) -0.0051(8) 0.8130(6) 0.021(4) Uiso 1 1 d . . . C24 C 0.5332(12) -0.0409(8) 0.8265(7) 0.027(5) Uani 1 1 d . . . C25 C 0.5412(13) -0.0840(9) 0.8723(8) 0.039(5) Uani 1 1 d . . . H25 H 0.4947 -0.1090 0.8837 0.047 Uiso 1 1 calc R . . C26 C 0.6200(15) -0.0891(10) 0.9009(8) 0.047(6) Uani 1 1 d . . . H26 H 0.6252 -0.1174 0.9311 0.056 Uiso 1 1 calc R . . C27 C 0.6873(14) -0.0528(9) 0.8842(8) 0.043(5) Uani 1 1 d . . . H27 H 0.7386 -0.0567 0.9033 0.051 Uiso 1 1 calc R . . C28 C 0.4488(13) -0.0341(10) 0.8012(7) 0.046(6) Uani 1 1 d . . . H28A H 0.4366 0.0124 0.7961 0.055 Uiso 1 1 calc R . . H28B H 0.4065 -0.0517 0.8267 0.055 Uiso 1 1 calc R . . C29 C 0.4397(13) -0.0701(10) 0.7438(9) 0.040(5) Uani 1 1 d . . . C30 C 0.4546(13) -0.0380(9) 0.6947(9) 0.044(6) Uani 1 1 d . . . C31 C 0.4431(12) -0.0683(9) 0.6433(7) 0.030(5) Uiso 1 1 d . . . C32 C 0.4198(12) -0.1351(9) 0.6432(9) 0.040(5) Uani 1 1 d . . . H32 H 0.4138 -0.1574 0.6097 0.048 Uiso 1 1 calc R . . C33 C 0.4059(13) -0.1683(10) 0.6926(8) 0.048(6) Uani 1 1 d . . . H33 H 0.3895 -0.2124 0.6923 0.058 Uiso 1 1 calc R . . C34 C 0.4166(11) -0.1353(9) 0.7423(8) 0.033(5) Uani 1 1 d . . . H34 H 0.4078 -0.1578 0.7754 0.040 Uiso 1 1 calc R . . C35 C 0.4570(13) -0.0312(10) 0.5900(7) 0.040(5) Uani 1 1 d . . . H35A H 0.4161 -0.0467 0.5627 0.048 Uiso 1 1 calc R . . H35B H 0.4457 0.0152 0.5965 0.048 Uiso 1 1 calc R . . C36 C 0.5441(16) -0.0382(9) 0.5666(8) 0.043(6) Uani 1 1 d . . . C37 C 0.6152(17) -0.0049(10) 0.5863(9) 0.051(6) Uani 1 1 d . . . C38 C 0.6998(17) -0.0129(10) 0.5642(8) 0.049(6) Uani 1 1 d . . . C39 C 0.7075(15) -0.0578(10) 0.5199(8) 0.046(6) Uani 1 1 d . . . H39 H 0.7611 -0.0663 0.5051 0.055 Uiso 1 1 calc R . . C40 C 0.6394(17) -0.0887(10) 0.4985(8) 0.044(6) Uani 1 1 d . . . H40 H 0.6464 -0.1158 0.4677 0.053 Uiso 1 1 calc R . . C41 C 0.5598(17) -0.0813(10) 0.5210(9) 0.055(7) Uani 1 1 d . . . H41 H 0.5147 -0.1051 0.5060 0.066 Uiso 1 1 calc R . . C42 C 0.7709(16) 0.0248(9) 0.5904(8) 0.052(7) Uani 1 1 d . . . H42A H 0.8238 0.0011 0.5844 0.063 Uiso 1 1 calc R . . H42B H 0.7612 0.0271 0.6301 0.063 Uiso 1 1 calc R . . C43 C 0.5861(16) 0.2600(12) 0.5893(10) 0.056(7) Uani 1 1 d . . . C44 C 0.527(2) 0.2239(19) 0.5594(14) 0.162(18) Uani 1 1 d . . . H44A H 0.5229 0.1801 0.5744 0.242 Uiso 1 1 calc R . . H44B H 0.5438 0.2217 0.5212 0.242 Uiso 1 1 calc R . . H44C H 0.4720 0.2450 0.5620 0.242 Uiso 1 1 calc R . . C45 C 0.629(2) 0.3176(15) 0.5623(15) 0.157(18) Uani 1 1 d . . . H45A H 0.6300 0.3542 0.5877 0.236 Uiso 1 1 calc R . . H45B H 0.5986 0.3298 0.5294 0.236 Uiso 1 1 calc R . . H45C H 0.6866 0.3058 0.5527 0.236 Uiso 1 1 calc R . . H1O H 0.906(9) 0.128(7) 0.656(6) 0.00(5) Uiso 1 1 d . . . H2O H 0.928(9) 0.179(6) 0.738(6) 0.00(4) Uiso 1 1 d . . . H3O H 0.908(9) 0.087(7) 0.786(6) 0.00(5) Uiso 1 1 d . . . H4O H 0.556(11) 0.041(9) 0.763(8) 0.03(7) Uiso 1 1 d . . . H6O H 0.531(10) 0.038(7) 0.680(6) 0.01(5) Uiso 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 Cs1 0.0805(12) 0.0604(10) 0.0547(9) 0.0203(8) -0.0197(9) -0.0215(10) O1 0.122(17) 0.037(10) 0.066(12) 0.009(9) -0.044(12) -0.049(10) O2 0.044(9) 0.032(8) 0.045(9) 0.003(8) 0.018(8) 0.004(7) O3 0.046(10) 0.014(7) 0.055(10) 0.007(7) 0.004(8) 0.016(7) O4 0.045(12) 0.021(8) 0.043(9) 0.001(6) 0.004(8) -0.011(8) O5 0.040(10) 0.027(8) 0.045(9) -0.001(7) -0.003(8) 0.003(7) O6 0.106(14) 0.048(9) 0.032(8) -0.001(8) -0.004(8) -0.031(9) O7 0.084(14) 0.093(14) 0.074(13) -0.018(11) 0.004(12) 0.006(11) O8 0.21(4) 0.26(4) 0.39(6) 0.14(4) -0.16(4) -0.11(4) O9 0.39(10) 0.73(16) 0.67(15) 0.30(13) -0.07(10) 0.08(10) C1 0.074(17) 0.023(13) 0.037(13) 0.004(11) 0.000(12) 0.000(12) C2 0.041(15) 0.038(13) 0.027(11) -0.004(10) 0.008(10) 0.020(11) C3 0.042(14) 0.052(14) 0.016(10) 0.009(10) -0.010(9) -0.017(11) C4 0.080(17) 0.022(11) 0.015(10) 0.015(10) -0.001(11) 0.005(12) C5 0.064(16) 0.023(11) 0.035(12) 0.015(10) 0.010(12) -0.006(12) C6 0.034(14) 0.027(13) 0.051(14) 0.016(11) 0.016(11) -0.011(11) C7 0.061(16) 0.048(14) 0.042(13) 0.021(11) 0.025(12) 0.010(13) C8 0.055(16) 0.044(14) 0.038(14) 0.017(11) 0.021(11) -0.008(12) C9 0.064(16) 0.013(12) 0.064(16) 0.008(10) -0.006(12) 0.005(11) C10 0.089(19) 0.039(14) 0.074(18) -0.013(13) 0.027(17) 0.007(14) C11 0.031(13) 0.026(12) 0.047(13) 0.000(10) 0.006(10) -0.004(10) C12 0.020(12) 0.018(11) 0.060(14) 0.005(10) 0.002(10) 0.003(9) C13 0.042(14) 0.042(13) 0.053(14) 0.007(13) 0.015(12) -0.015(11) C15 0.024(13) 0.034(12) 0.027(11) -0.025(9) 0.000(9) 0.015(9) C16 0.023(12) 0.034(13) 0.009(8) -0.005(9) 0.001(8) 0.010(10) C17 0.040(14) 0.021(11) 0.028(11) -0.006(10) 0.004(11) -0.007(11) C18 0.074(17) 0.010(10) 0.073(16) -0.019(10) -0.010(15) -0.007(12) C20 0.042(14) 0.022(11) 0.046(12) -0.015(10) -0.026(11) 0.010(10) C21 0.024(12) 0.046(14) 0.040(12) -0.008(11) -0.004(10) 0.013(11) C22 0.024(13) 0.028(11) 0.032(11) -0.002(9) 0.007(10) 0.019(10) C24 0.033(13) 0.013(10) 0.034(11) -0.008(9) 0.017(10) 0.000(9) C25 0.040(15) 0.043(13) 0.033(12) -0.009(11) 0.009(11) 0.001(11) C26 0.074(19) 0.035(13) 0.032(13) 0.012(10) 0.008(13) -0.008(13) C27 0.049(15) 0.043(13) 0.037(12) -0.001(10) 0.014(12) -0.006(13) C28 0.052(15) 0.056(14) 0.030(12) -0.010(11) -0.003(11) 0.002(12) C29 0.034(14) 0.038(13) 0.047(14) -0.001(12) 0.008(10) -0.010(11) C30 0.049(14) 0.018(12) 0.065(17) -0.014(11) -0.013(12) -0.006(10) C32 0.028(13) 0.039(14) 0.054(14) -0.007(11) -0.011(10) -0.005(10) C33 0.055(15) 0.034(13) 0.054(16) 0.000(11) -0.007(12) -0.006(11) C34 0.030(13) 0.026(13) 0.044(13) 0.007(10) 0.006(10) 0.007(9) C35 0.041(15) 0.041(13) 0.038(12) 0.005(10) -0.006(11) 0.004(11) C36 0.080(19) 0.020(12) 0.028(12) 0.015(10) -0.033(13) 0.000(12) C37 0.08(2) 0.024(13) 0.048(15) 0.008(11) -0.009(15) -0.024(13) C38 0.065(18) 0.046(15) 0.036(12) 0.030(12) -0.018(14) -0.013(14) C39 0.055(17) 0.046(14) 0.036(13) 0.007(11) 0.002(12) 0.007(13) C40 0.068(18) 0.033(13) 0.031(13) 0.006(10) -0.013(13) -0.004(14) C41 0.08(2) 0.047(15) 0.035(14) 0.009(12) -0.013(13) -0.015(14) C42 0.10(2) 0.014(11) 0.041(13) 0.003(10) -0.016(13) 0.001(12) C43 0.062(18) 0.068(18) 0.038(15) -0.024(14) 0.002(14) 0.013(15) C44 0.10(3) 0.23(5) 0.15(3) -0.12(3) -0.02(2) 0.01(3) C45 0.17(4) 0.11(3) 0.20(4) 0.02(3) 0.15(3) 0.04(3) _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 Cs1 O7 2.99(2) . ? Cs1 O4 3.067(13) . ? Cs1 O6 3.242(13) . ? Cs1 C16 3.417(15) . ? Cs1 O1 3.44(2) . ? Cs1 C17 3.516(17) . ? Cs1 O3 3.537(14) . ? Cs1 C1 3.55(2) . ? Cs1 C2 3.769(17) . ? Cs1 C13 3.822(18) . ? Cs1 C21 3.854(19) . ? Cs1 C15 3.890(16) . ? O1 C1 1.31(2) . ? O2 C13 1.39(2) . ? O3 C16 1.356(19) . ? O4 C23 1.40(2) . ? O5 C30 1.36(2) . ? O6 C37 1.39(2) . ? O7 C43 1.14(2) . ? C1 C6 1.36(2) . ? C1 C2 1.42(3) . ? C2 C3 1.38(2) . ? C2 C42 1.52(2) . ? C3 C4 1.34(2) . ? C4 C5 1.36(3) . ? C5 C6 1.38(3) . ? C6 C7 1.55(3) . ? C7 C8 1.52(3) . ? C8 C9 1.34(3) . ? C8 C13 1.39(3) . ? C9 C10 1.40(3) . ? C10 C11 1.39(3) . ? C11 C12 1.38(2) . ? C12 C13 1.39(3) . ? C12 C14 1.51(2) . ? C14 C15 1.51(2) . ? C15 C20 1.38(2) . ? C15 C16 1.41(2) . ? C16 C17 1.38(2) . ? C17 C18 1.31(3) . ? C17 C21 1.49(2) . ? C18 C19 1.47(2) . ? C19 C20 1.39(2) . ? C21 C22 1.49(2) . ? C22 C27 1.38(2) . ? C22 C23 1.39(2) . ? C23 C24 1.37(2) . ? C24 C25 1.41(2) . ? C24 C28 1.46(2) . ? C25 C26 1.42(3) . ? C26 C27 1.35(3) . ? C28 C29 1.57(3) . ? C29 C34 1.37(2) . ? C29 C30 1.37(3) . ? C30 C31 1.39(2) . ? C31 C32 1.40(2) . ? C31 C35 1.50(2) . ? C32 C33 1.38(2) . ? C33 C34 1.38(3) . ? C35 C36 1.48(3) . ? C36 C37 1.39(3) . ? C36 C41 1.43(3) . ? C37 C38 1.44(3) . ? C38 C39 1.41(3) . ? C38 C42 1.49(3) . ? C39 C40 1.34(3) . ? C40 C41 1.37(3) . ? C43 C44 1.39(3) . ? C43 C45 1.50(4) . ? 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 O7 Cs1 O4 123.0(5) . . ? O7 Cs1 O6 84.3(4) . . ? O4 Cs1 O6 64.5(3) . . ? O7 Cs1 C16 142.6(5) . . ? O4 Cs1 C16 80.3(4) . . ? O6 Cs1 C16 133.0(4) . . ? O7 Cs1 O1 105.8(4) . . ? O4 Cs1 O1 116.8(4) . . ? O6 Cs1 O1 85.1(4) . . ? C16 Cs1 O1 83.9(4) . . ? O7 Cs1 C17 149.4(5) . . ? O4 Cs1 C17 57.9(4) . . ? O6 Cs1 C17 116.7(4) . . ? C16 Cs1 C17 22.9(4) . . ? O1 Cs1 C17 98.3(5) . . ? O7 Cs1 O3 145.4(4) . . ? O4 Cs1 O3 89.9(4) . . ? O6 Cs1 O3 123.3(4) . . ? C16 Cs1 O3 22.4(3) . . ? O1 Cs1 O3 61.6(4) . . ? C17 Cs1 O3 39.8(4) . . ? O7 Cs1 C1 84.9(5) . . ? O4 Cs1 C1 127.6(4) . . ? O6 Cs1 C1 77.3(4) . . ? C16 Cs1 C1 104.0(5) . . ? O1 Cs1 C1 21.6(4) . . ? C17 Cs1 C1 119.8(5) . . ? O3 Cs1 C1 82.1(4) . . ? O7 Cs1 C2 80.9(4) . . ? O4 Cs1 C2 112.0(4) . . ? O6 Cs1 C2 55.4(4) . . ? C16 Cs1 C2 119.9(4) . . ? O1 Cs1 C2 36.9(4) . . ? C17 Cs1 C2 128.9(4) . . ? O3 Cs1 C2 97.5(4) . . ? C1 Cs1 C2 22.1(4) . . ? O7 Cs1 C13 93.7(5) . . ? O4 Cs1 C13 141.7(5) . . ? O6 Cs1 C13 137.2(4) . . ? C16 Cs1 C13 62.3(4) . . ? O1 Cs1 C13 54.3(4) . . ? C17 Cs1 C13 85.2(5) . . ? O3 Cs1 C13 52.1(4) . . ? C1 Cs1 C13 60.0(5) . . ? C2 Cs1 C13 82.1(5) . . ? O7 Cs1 C21 164.8(4) . . ? O4 Cs1 C21 45.1(4) . . ? O6 Cs1 C21 95.3(4) . . ? C16 Cs1 C21 39.1(4) . . ? O1 Cs1 C21 89.3(4) . . ? C17 Cs1 C21 22.8(4) . . ? O3 Cs1 C21 44.8(4) . . ? C1 Cs1 C21 109.9(4) . . ? C2 Cs1 C21 111.4(4) . . ? C13 Cs1 C21 96.8(4) . . ? O7 Cs1 C15 121.6(4) . . ? O4 Cs1 C15 94.5(4) . . ? O6 Cs1 C15 153.7(4) . . ? C16 Cs1 C15 21.0(4) . . ? O1 Cs1 C15 91.3(4) . . ? C17 Cs1 C15 38.1(4) . . ? O3 Cs1 C15 36.3(3) . . ? C1 Cs1 C15 107.3(5) . . ? C2 Cs1 C15 127.9(4) . . ? C13 Cs1 C15 52.7(4) . . ? C21 Cs1 C15 58.6(4) . . ? C1 O1 Cs1 84.0(13) . . ? C16 O3 Cs1 73.8(8) . . ? C23 O4 Cs1 148.2(12) . . ? C37 O6 Cs1 146.9(14) . . ? C43 O7 Cs1 145.9(17) . . ? O1 C1 C6 124(2) . . ? O1 C1 C2 114.7(17) . . ? C6 C1 C2 121(2) . . ? O1 C1 Cs1 74.5(12) . . ? C6 C1 Cs1 108.1(13) . . ? C2 C1 Cs1 87.7(12) . . ? C3 C2 C1 118.5(18) . . ? C3 C2 C42 124.8(19) . . ? C1 C2 C42 116.7(17) . . ? C3 C2 Cs1 112.4(12) . . ? C1 C2 Cs1 70.2(11) . . ? C42 C2 Cs1 85.9(10) . . ? C4 C3 C2 120.7(19) . . ? C3 C4 C5 118.8(18) . . ? C4 C5 C6 124.1(17) . . ? C1 C6 C5 117(2) . . ? C1 C6 C7 121(2) . . ? C5 C6 C7 122.4(17) . . ? C8 C7 C6 110.8(17) . . ? C9 C8 C13 119(2) . . ? C9 C8 C7 120.7(18) . . ? C13 C8 C7 119.8(19) . . ? C8 C9 C10 121(2) . . ? C11 C10 C9 121(2) . . ? C12 C11 C10 119.0(19) . . ? C11 C12 C13 119.3(18) . . ? C11 C12 C14 118.8(18) . . ? C13 C12 C14 121.9(17) . . ? O2 C13 C12 121.5(18) . . ? O2 C13 C8 117(2) . . ? C12 C13 C8 121.2(19) . . ? O2 C13 Cs1 93.2(10) . . ? C12 C13 Cs1 86.2(11) . . ? C8 C13 Cs1 91.4(12) . . ? C15 C14 C12 113.3(15) . . ? C20 C15 C16 118.0(17) . . ? C20 C15 C14 119.6(16) . . ? C16 C15 C14 122.3(15) . . ? C20 C15 Cs1 102.1(11) . . ? C16 C15 Cs1 60.3(9) . . ? C14 C15 Cs1 104.9(10) . . ? O3 C16 C17 122.9(16) . . ? O3 C16 C15 114.9(16) . . ? C17 C16 C15 121.9(16) . . ? O3 C16 Cs1 83.8(9) . . ? C17 C16 Cs1 82.6(10) . . ? C15 C16 Cs1 98.7(10) . . ? C18 C17 C16 120.1(18) . . ? C18 C17 C21 121.5(18) . . ? C16 C17 C21 118.5(18) . . ? C18 C17 Cs1 103.0(14) . . ? C16 C17 Cs1 74.5(9) . . ? C21 C17 Cs1 91.5(10) . . ? C17 C18 C19 122(2) . . ? C20 C19 C18 117.2(19) . . ? C19 C20 C15 121.2(17) . . ? C22 C21 C17 116.4(16) . . ? C22 C21 Cs1 109.9(11) . . ? C17 C21 Cs1 65.8(10) . . ? C27 C22 C23 117.0(18) . . ? C27 C22 C21 120.3(18) . . ? C23 C22 C21 122.6(16) . . ? C24 C23 C22 124.8(17) . . ? C24 C23 O4 121.7(17) . . ? C22 C23 O4 113.5(17) . . ? C23 C24 C25 116.1(18) . . ? C23 C24 C28 126.1(17) . . ? C25 C24 C28 117.5(17) . . ? C24 C25 C26 120.1(19) . . ? C27 C26 C25 119.8(19) . . ? C26 C27 C22 122(2) . . ? C24 C28 C29 113.8(16) . . ? C34 C29 C30 118.6(18) . . ? C34 C29 C28 119.8(18) . . ? C30 C29 C28 121.6(17) . . ? O5 C30 C29 119.1(17) . . ? O5 C30 C31 118.5(19) . . ? C29 C30 C31 122.4(17) . . ? C30 C31 C32 117.4(18) . . ? C30 C31 C35 121.3(17) . . ? C32 C31 C35 121.3(17) . . ? C33 C32 C31 120.7(18) . . ? C34 C33 C32 119.3(18) . . ? C29 C34 C33 121.5(18) . . ? C36 C35 C31 114.2(16) . . ? C37 C36 C41 115(2) . . ? C37 C36 C35 124(2) . . ? C41 C36 C35 121(2) . . ? C36 C37 O6 119(2) . . ? C36 C37 C38 124(2) . . ? O6 C37 C38 116.5(19) . . ? C39 C38 C37 116(2) . . ? C39 C38 C42 126(2) . . ? C37 C38 C42 118(2) . . ? C40 C39 C38 122(2) . . ? C39 C40 C41 122(2) . . ? C40 C41 C36 122(2) . . ? C38 C42 C2 113.2(16) . . ? O7 C43 C44 124(3) . . ? O7 C43 C45 117(3) . . ? C44 C43 C45 119(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 21.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.157 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.143 #===END data_33 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H65 K2 O12' _chemical_formula_weight 984.26 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.6363(12) _cell_length_b 24.9037(19) _cell_length_c 15.0403(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.0120(10) _cell_angle_gamma 90.00 _cell_volume 5213.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2499 _exptl_absorpt_correction_T_max 0.4442 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21918 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6814 _reflns_number_gt 4903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0842P)^2^+1.6521P] 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 SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6814 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 3.653 _refine_ls_shift/su_mean 0.064 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 K1 K 0.40129(6) 0.36857(3) 0.29635(5) 0.0464(3) Uani 1 1 d . . . K2 K 0.51818(6) 0.22175(3) 0.41090(6) 0.0502(3) Uani 1 1 d . . . O1 O 0.3374(2) 0.27670(12) 0.3572(2) 0.0553(7) Uani 1 1 d . . . O2 O 0.5379(2) 0.33383(13) 0.4511(2) 0.0633(8) Uani 1 1 d . . . O3 O 0.4884(2) 0.28581(11) 0.2368(2) 0.0520(8) Uani 1 1 d . . . O4 O 0.3898(2) 0.32351(14) 0.0192(2) 0.0455(8) Uani 1 1 d . . . O5 O 0.57694(17) 0.40593(9) 0.28196(17) 0.0418(6) Uani 1 1 d . . . O6 O 0.70068(15) 0.36044(8) 0.41744(16) 0.0379(6) Uani 1 1 d . . . H6 H 0.7044 0.3279 0.4068 0.057 Uiso 1 1 calc R . . O7 O 0.67805(15) 0.26525(8) 0.35540(15) 0.0381(6) Uani 1 1 d . . . O8 O 0.48208(15) 0.19560(9) 0.09924(15) 0.0401(6) Uani 1 1 d . . . H8 H 0.4232 0.2009 0.0802 0.060 Uiso 1 1 calc R . . O9 O 0.31649(16) 0.22908(9) 0.03159(16) 0.0414(6) Uani 1 1 d . . . H9 H 0.3256 0.2609 0.0200 0.062 Uiso 1 1 calc R . . O10 O 0.3422(3) 0.45600(13) 0.3802(2) 0.0916(11) Uani 1 1 d . . . O11 O 0.6806(2) 0.18200(11) 0.5463(2) 0.0695(8) Uani 1 1 d . . . O12 O 0.0497(5) 0.3737(3) 0.2259(5) 0.210(3) Uani 1 1 d . . . C1 C 0.3544(2) 0.36477(13) 0.0580(2) 0.0351(8) Uani 1 1 d . . . C2 C 0.4161(2) 0.40801(13) 0.0920(2) 0.0339(8) Uani 1 1 d . . . C3 C 0.3821(3) 0.45197(13) 0.1285(2) 0.0393(9) Uani 1 1 d . . . H3 H 0.4207 0.4853 0.1412 0.047 Uiso 1 1 calc R . . C4 C 0.2889(3) 0.45309(14) 0.1332(3) 0.0458(9) Uani 1 1 d . . . H4 H 0.2623 0.4868 0.1500 0.055 Uiso 1 1 calc R . . C5 C 0.2300(3) 0.40930(15) 0.1021(3) 0.0475(10) Uani 1 1 d . . . H5 H 0.1626 0.4111 0.1027 0.057 Uiso 1 1 calc R . . C6 C 0.2601(2) 0.36428(14) 0.0636(2) 0.0407(9) Uani 1 1 d . . . C7 C 0.5180(2) 0.40492(13) 0.0862(2) 0.0386(8) Uani 1 1 d . . . H7A H 0.5424 0.3687 0.1051 0.046 Uiso 1 1 calc R . . H7B H 0.5145 0.4092 0.0205 0.046 Uiso 1 1 calc R . . C8 C 0.6222(2) 0.44164(12) 0.2407(2) 0.0345(8) Uani 1 1 d . . . C9 C 0.6976(2) 0.47389(12) 0.2950(2) 0.0342(8) Uani 1 1 d . . . C10 C 0.7431(2) 0.50769(13) 0.2487(3) 0.0416(9) Uani 1 1 d . . . H10 H 0.7954 0.5286 0.2836 0.050 Uiso 1 1 calc R . . C11 C 0.7130(3) 0.51129(14) 0.1521(3) 0.0466(9) Uani 1 1 d . . . H11 H 0.7443 0.5347 0.1220 0.056 Uiso 1 1 calc R . . C12 C 0.6370(2) 0.48054(13) 0.1002(3) 0.0421(9) Uani 1 1 d . . . H12 H 0.6157 0.4841 0.0348 0.051 Uiso 1 1 calc R . . C13 C 0.5910(2) 0.44427(13) 0.1427(2) 0.0357(8) Uani 1 1 d . . . C14 C 0.7265(2) 0.47323(13) 0.4011(2) 0.0420(9) Uani 1 1 d . . . H14A H 0.6695 0.4642 0.4191 0.050 Uiso 1 1 calc R . . H14B H 0.7457 0.5097 0.4235 0.050 Uiso 1 1 calc R . . C15 C 0.7891(2) 0.38015(13) 0.4580(2) 0.0355(8) Uani 1 1 d . . . C16 C 0.8641(2) 0.34569(14) 0.5087(2) 0.0389(8) Uani 1 1 d . . . C17 C 0.9539(3) 0.36744(16) 0.5543(3) 0.0520(10) Uani 1 1 d . . . H17 H 1.0038 0.3448 0.5884 0.062 Uiso 1 1 calc R . . C18 C 0.9708(3) 0.42132(17) 0.5504(3) 0.0613(11) Uani 1 1 d . . . H18 H 1.0316 0.4355 0.5824 0.074 Uiso 1 1 calc R . . C19 C 0.8980(3) 0.45486(15) 0.4990(3) 0.0543(10) Uani 1 1 d . . . H19 H 0.9105 0.4917 0.4957 0.065 Uiso 1 1 calc R . . C20 C 0.8069(2) 0.43525(14) 0.4524(2) 0.0397(9) Uani 1 1 d . . . C21 C 0.8458(3) 0.28631(13) 0.5144(2) 0.0422(9) Uani 1 1 d . . . H21A H 0.7829 0.2815 0.5235 0.051 Uiso 1 1 calc R . . H21B H 0.8943 0.2717 0.5696 0.051 Uiso 1 1 calc R . . C22 C 0.7645(2) 0.24293(13) 0.3553(2) 0.0350(8) Uani 1 1 d . . . C23 C 0.7657(2) 0.21012(13) 0.2806(2) 0.0372(8) Uani 1 1 d . . . C24 C 0.8536(3) 0.18969(15) 0.2789(3) 0.0492(10) Uani 1 1 d . . . H24 H 0.8561 0.1672 0.2295 0.059 Uiso 1 1 calc R . . C25 C 0.9380(3) 0.20220(17) 0.3495(3) 0.0597(11) Uani 1 1 d . . . H25 H 0.9973 0.1894 0.3463 0.072 Uiso 1 1 calc R . . C26 C 0.9345(3) 0.23318(16) 0.4233(3) 0.0534(10) Uani 1 1 d . . . H26 H 0.9916 0.2408 0.4713 0.064 Uiso 1 1 calc R . . C27 C 0.8479(2) 0.25378(14) 0.4291(2) 0.0401(9) Uani 1 1 d . . . C28 C 0.6743(2) 0.19816(14) 0.2040(2) 0.0396(8) Uani 1 1 d . . . H28A H 0.6905 0.1790 0.1539 0.048 Uiso 1 1 calc R . . H28B H 0.6443 0.2323 0.1781 0.048 Uiso 1 1 calc R . . C29 C 0.5045(2) 0.16538(13) 0.1786(2) 0.0352(8) Uani 1 1 d . . . C30 C 0.4346(3) 0.13588(13) 0.2031(2) 0.0404(9) Uani 1 1 d . . . C31 C 0.4642(3) 0.10487(14) 0.2847(3) 0.0478(10) Uani 1 1 d . . . H31 H 0.4183 0.0794 0.2981 0.057 Uiso 1 1 calc R . . C32 C 0.5590(3) 0.10343(14) 0.3389(3) 0.0462(9) Uani 1 1 d . . . H32 H 0.5806 0.0742 0.3853 0.055 Uiso 1 1 calc R . . C33 C 0.6277(3) 0.13286(13) 0.3134(2) 0.0420(9) Uani 1 1 d . . . H33 H 0.6966 0.1250 0.3439 0.050 Uiso 1 1 calc R . . C34 C 0.6009(2) 0.16494(13) 0.2330(2) 0.0365(8) Uani 1 1 d . . . C35 C 0.3307(2) 0.13416(14) 0.1406(3) 0.0454(9) Uani 1 1 d . . . H35A H 0.3308 0.1309 0.0757 0.054 Uiso 1 1 calc R . . H35B H 0.3010 0.1016 0.1556 0.054 Uiso 1 1 calc R . . C36 C 0.2623(2) 0.22720(14) 0.0895(2) 0.0395(9) Uani 1 1 d . . . C37 C 0.2677(2) 0.18160(14) 0.1465(2) 0.0403(9) Uani 1 1 d . . . C38 C 0.2121(3) 0.18013(16) 0.2060(3) 0.0503(10) Uani 1 1 d . . . H38 H 0.2153 0.1500 0.2446 0.060 Uiso 1 1 calc R . . C39 C 0.1518(3) 0.22237(17) 0.2094(3) 0.0544(11) Uani 1 1 d . . . H39 H 0.1148 0.2209 0.2505 0.065 Uiso 1 1 calc R . . C40 C 0.1458(2) 0.26685(16) 0.1525(3) 0.0487(10) Uani 1 1 d . . . H40 H 0.1041 0.2951 0.1550 0.058 Uiso 1 1 calc R . . C41 C 0.2005(2) 0.27022(14) 0.0919(2) 0.0417(9) Uani 1 1 d . . . C42 C 0.1912(2) 0.31789(14) 0.0270(3) 0.0461(9) Uani 1 1 d . . . H42A H 0.1255 0.3317 0.0115 0.055 Uiso 1 1 calc R . . H42B H 0.2004 0.3051 -0.0313 0.055 Uiso 1 1 calc R . . C43 C 0.3560(4) 0.50335(19) 0.3725(3) 0.0657(12) Uani 1 1 d . . . C44 C 0.4523(4) 0.5235(2) 0.3795(4) 0.1013(17) Uani 1 1 d . . . H44A H 0.4721 0.5495 0.4298 0.152 Uiso 1 1 calc R . . H44B H 0.4509 0.5404 0.3210 0.152 Uiso 1 1 calc R . . H44C H 0.4974 0.4938 0.3923 0.152 Uiso 1 1 calc R . . C45 C 0.2770(4) 0.5433(2) 0.3533(4) 0.1040(19) Uani 1 1 d . . . H45A H 0.2173 0.5252 0.3501 0.156 Uiso 1 1 calc R . . H45B H 0.2704 0.5610 0.2942 0.156 Uiso 1 1 calc R . . H45C H 0.2915 0.5697 0.4030 0.156 Uiso 1 1 calc R . . C46 C 0.7505(3) 0.15889(15) 0.5953(3) 0.0512(10) Uani 1 1 d . . . C47 C 0.8193(3) 0.1306(2) 0.5557(3) 0.0822(15) Uani 1 1 d . . . H47A H 0.8030 0.0928 0.5480 0.123 Uiso 1 1 calc R . . H47B H 0.8841 0.1347 0.5979 0.123 Uiso 1 1 calc R . . H47C H 0.8154 0.1461 0.4954 0.123 Uiso 1 1 calc R . . C48 C 0.7732(3) 0.15652(17) 0.6989(3) 0.0658(12) Uani 1 1 d . . . H48A H 0.8300 0.1779 0.7280 0.099 Uiso 1 1 calc R . . H48B H 0.7851 0.1196 0.7196 0.099 Uiso 1 1 calc R . . H48C H 0.7194 0.1705 0.7165 0.099 Uiso 1 1 calc R . . C49 C 0.0152(10) 0.4297(4) 0.3190(7) 0.272(7) Uani 1 1 d . . . H49A H 0.0600 0.4561 0.3557 0.408 Uiso 1 1 calc R . . H49B H -0.0323 0.4213 0.3498 0.408 Uiso 1 1 calc R . . H49C H -0.0167 0.4442 0.2573 0.408 Uiso 1 1 calc R . . C50 C 0.0671(6) 0.3813(4) 0.3103(6) 0.133(3) Uani 1 1 d . . . C51 C 0.1171(9) 0.3546(6) 0.3858(7) 0.306(10) Uani 1 1 d . . . H51A H 0.0989 0.3170 0.3790 0.458 Uiso 1 1 calc R . . H51B H 0.1038 0.3693 0.4403 0.458 Uiso 1 1 calc R . . H51C H 0.1851 0.3580 0.3935 0.458 Uiso 1 1 calc R . . C52 C 0.0234(6) 0.0620(3) 0.3245(6) 0.159(3) Uani 1 1 d . . . H52A H 0.0879 0.0745 0.3568 0.239 Uiso 1 1 calc R . . H52B H -0.0110 0.0893 0.2812 0.239 Uiso 1 1 calc R . . H52C H 0.0268 0.0294 0.2903 0.239 Uiso 1 1 calc R . . C53 C -0.0303(6) 0.0502(3) 0.3969(6) 0.161(3) Uani 1 1 d . . . H53A H -0.0292 0.0822 0.4351 0.193 Uiso 1 1 calc R . . H53B H -0.0975 0.0412 0.3641 0.193 Uiso 1 1 calc R . . C54 C 0.0183(6) 0.0027(4) 0.4608(6) 0.163(4) Uani 1 1 d . . . H54A H 0.0066 -0.0306 0.4243 0.196 Uiso 1 1 calc R . . H54B H 0.0879 0.0087 0.4838 0.196 Uiso 1 1 calc R . . H1A H 0.308(4) 0.278(2) 0.404(4) 0.12(2) Uiso 1 1 d . . . H2A H 0.523(5) 0.336(3) 0.502(5) 0.16(3) Uiso 1 1 d . . . H3A H 0.483(4) 0.277(2) 0.190(3) 0.08(2) Uiso 1 1 d . . . H4A H 0.370(3) 0.3016(14) 0.020(3) 0.028(14) Uiso 1 1 d . . . H5A H 0.617(3) 0.3914(16) 0.335(3) 0.066(13) Uiso 1 1 d . . . H1B H 0.289(4) 0.268(2) 0.313(4) 0.12(2) Uiso 1 1 d . . . H2B H 0.591(6) 0.356(3) 0.468(6) 0.20(4) Uiso 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 K1 0.0557(5) 0.0420(5) 0.0406(5) 0.0060(4) 0.0138(4) 0.0008(4) K2 0.0487(5) 0.0445(5) 0.0589(6) 0.0048(4) 0.0189(4) 0.0040(4) O1 0.0539(18) 0.0707(19) 0.0371(16) 0.0035(14) 0.0080(16) -0.0166(14) O2 0.0502(18) 0.104(2) 0.0348(16) 0.0045(16) 0.0116(14) -0.0167(16) O3 0.0564(18) 0.0549(17) 0.0422(18) -0.0112(15) 0.0116(14) 0.0003(12) O4 0.0431(17) 0.0445(19) 0.0495(18) -0.0093(15) 0.0149(13) -0.0071(15) O5 0.0385(14) 0.0475(15) 0.0365(15) 0.0112(12) 0.0074(12) -0.0076(11) O6 0.0339(13) 0.0332(12) 0.0425(14) -0.0024(12) 0.0059(11) -0.0031(10) O7 0.0290(13) 0.0443(14) 0.0389(14) -0.0006(11) 0.0075(11) 0.0033(10) O8 0.0353(13) 0.0508(15) 0.0332(14) 0.0027(12) 0.0089(11) -0.0018(11) O9 0.0430(14) 0.0416(14) 0.0400(14) -0.0001(12) 0.0136(12) -0.0064(11) O10 0.139(3) 0.057(2) 0.096(3) -0.0019(18) 0.060(2) 0.000(2) O11 0.0516(18) 0.0678(19) 0.080(2) 0.0222(16) 0.0068(16) 0.0033(15) O12 0.205(6) 0.260(7) 0.169(6) -0.057(5) 0.062(5) 0.093(5) C1 0.040(2) 0.035(2) 0.0272(19) 0.0006(16) 0.0070(16) 0.0044(16) C2 0.039(2) 0.035(2) 0.0244(18) 0.0045(15) 0.0060(16) 0.0005(15) C3 0.046(2) 0.035(2) 0.034(2) 0.0075(16) 0.0071(17) 0.0023(16) C4 0.045(2) 0.043(2) 0.047(2) 0.0026(18) 0.0113(19) 0.0123(18) C5 0.034(2) 0.055(2) 0.049(2) -0.001(2) 0.0072(18) 0.0070(18) C6 0.036(2) 0.045(2) 0.036(2) -0.0001(17) 0.0040(16) 0.0037(16) C7 0.044(2) 0.040(2) 0.033(2) -0.0025(16) 0.0143(17) -0.0035(16) C8 0.035(2) 0.0311(19) 0.040(2) 0.0036(16) 0.0155(17) 0.0004(15) C9 0.0341(19) 0.0290(18) 0.038(2) -0.0004(16) 0.0091(16) 0.0000(15) C10 0.038(2) 0.034(2) 0.051(2) -0.0028(17) 0.0111(18) -0.0034(16) C11 0.052(2) 0.038(2) 0.055(3) 0.0053(19) 0.024(2) -0.0061(17) C12 0.050(2) 0.042(2) 0.039(2) 0.0014(17) 0.0209(18) -0.0033(18) C13 0.039(2) 0.0339(19) 0.036(2) 0.0008(16) 0.0128(17) 0.0010(15) C14 0.046(2) 0.0348(19) 0.042(2) -0.0043(17) 0.0093(18) -0.0067(16) C15 0.033(2) 0.043(2) 0.0283(19) -0.0039(16) 0.0064(16) -0.0055(16) C16 0.037(2) 0.048(2) 0.0273(19) -0.0004(16) 0.0035(16) -0.0019(16) C17 0.042(2) 0.058(3) 0.043(2) 0.0071(19) -0.0051(18) -0.0049(18) C18 0.042(2) 0.066(3) 0.059(3) 0.008(2) -0.008(2) -0.016(2) C19 0.053(3) 0.049(2) 0.052(2) -0.001(2) 0.003(2) -0.0195(19) C20 0.039(2) 0.043(2) 0.035(2) -0.0022(17) 0.0081(17) -0.0053(16) C21 0.038(2) 0.048(2) 0.032(2) 0.0049(17) -0.0012(16) 0.0040(16) C22 0.034(2) 0.0344(19) 0.036(2) 0.0069(16) 0.0089(17) 0.0014(15) C23 0.041(2) 0.0353(19) 0.034(2) 0.0045(16) 0.0094(16) 0.0028(15) C24 0.047(2) 0.055(2) 0.047(2) -0.0045(19) 0.015(2) 0.0108(18) C25 0.036(2) 0.078(3) 0.062(3) -0.003(2) 0.011(2) 0.016(2) C26 0.039(2) 0.065(3) 0.045(2) -0.003(2) -0.0028(19) 0.0123(18) C27 0.037(2) 0.044(2) 0.034(2) 0.0050(17) 0.0029(17) 0.0036(16) C28 0.043(2) 0.043(2) 0.031(2) 0.0005(16) 0.0095(17) 0.0016(16) C29 0.047(2) 0.0316(19) 0.0278(19) -0.0026(16) 0.0119(17) -0.0010(15) C30 0.051(2) 0.0322(19) 0.040(2) -0.0052(17) 0.0170(18) -0.0047(16) C31 0.064(3) 0.036(2) 0.049(2) -0.0036(18) 0.026(2) -0.0083(18) C32 0.066(3) 0.034(2) 0.038(2) 0.0038(17) 0.016(2) 0.0018(18) C33 0.054(2) 0.036(2) 0.035(2) -0.0018(17) 0.0112(18) 0.0026(17) C34 0.047(2) 0.0335(19) 0.030(2) -0.0050(16) 0.0129(18) 0.0010(16) C35 0.050(2) 0.040(2) 0.048(2) -0.0068(18) 0.0175(19) -0.0143(17) C36 0.0300(19) 0.053(2) 0.035(2) -0.0131(18) 0.0104(17) -0.0120(17) C37 0.037(2) 0.045(2) 0.038(2) -0.0057(17) 0.0106(17) -0.0133(16) C38 0.043(2) 0.062(3) 0.047(2) -0.0071(19) 0.014(2) -0.016(2) C39 0.043(2) 0.076(3) 0.048(3) -0.014(2) 0.020(2) -0.018(2) C40 0.030(2) 0.063(3) 0.051(2) -0.017(2) 0.0100(19) -0.0057(17) C41 0.0284(19) 0.052(2) 0.040(2) -0.0102(18) 0.0045(17) -0.0092(16) C42 0.032(2) 0.053(2) 0.048(2) -0.0066(19) 0.0056(18) 0.0022(16) C43 0.105(4) 0.057(3) 0.045(3) 0.004(2) 0.038(3) 0.008(3) C44 0.110(5) 0.103(4) 0.090(4) 0.029(3) 0.029(3) -0.010(3) C45 0.139(5) 0.094(4) 0.105(4) 0.022(3) 0.074(4) 0.037(4) C46 0.050(3) 0.046(2) 0.054(3) 0.009(2) 0.011(2) -0.0068(19) C47 0.078(3) 0.113(4) 0.057(3) 0.010(3) 0.023(3) 0.025(3) C48 0.070(3) 0.065(3) 0.061(3) -0.005(2) 0.017(2) 0.000(2) C49 0.53(2) 0.151(8) 0.137(8) -0.024(7) 0.103(11) 0.055(12) C50 0.158(7) 0.163(7) 0.092(5) -0.044(5) 0.060(5) 0.026(5) C51 0.295(14) 0.48(2) 0.166(9) 0.140(12) 0.106(10) 0.294(16) C52 0.156(7) 0.152(7) 0.183(8) -0.021(6) 0.073(7) 0.032(5) C53 0.156(7) 0.120(6) 0.192(9) 0.022(6) 0.033(7) 0.059(5) C54 0.109(6) 0.160(7) 0.213(11) -0.098(8) 0.039(6) -0.033(5) _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 K1 O2 2.699(3) . ? K1 O3 2.717(3) . ? K1 O1 2.735(3) . ? K1 O10 2.784(3) . ? K1 O5 2.805(2) . ? K1 C3 3.214(3) . ? K1 C4 3.265(4) . ? K1 C2 3.298(3) . ? K1 C5 3.364(4) . ? K1 C1 3.436(3) . ? K1 C6 3.473(3) . ? K1 K2 4.1764(11) . ? K2 O11 2.790(3) . ? K2 O2 2.852(3) . ? K2 O1 2.865(3) . ? K2 O7 2.925(2) . ? K2 O3 2.981(3) . ? K2 O4 3.056(3) 4_566 ? K2 C32 3.258(3) . ? K2 C33 3.327(3) . ? K2 C31 3.431(4) . ? O4 C1 1.362(4) . ? O4 K2 3.056(3) 4_565 ? O5 C8 1.367(4) . ? O6 C15 1.342(4) . ? O7 C22 1.382(4) . ? O8 C29 1.362(4) . ? O9 C36 1.348(4) . ? O10 C43 1.208(5) . ? O11 C46 1.206(4) . ? O12 C50 1.230(8) . ? C1 C2 1.397(5) . ? C1 C6 1.408(5) . ? C2 C3 1.385(5) . ? C2 C7 1.523(4) . ? C3 C4 1.387(5) . ? C4 C5 1.380(5) . ? C5 C6 1.395(5) . ? C6 C42 1.520(5) . ? C7 C13 1.504(4) . ? C8 C13 1.404(5) . ? C8 C9 1.405(4) . ? C9 C10 1.387(5) . ? C9 C14 1.519(5) . ? C10 C11 1.385(5) . ? C11 C12 1.376(5) . ? C12 C13 1.394(5) . ? C14 C20 1.520(5) . ? C15 C20 1.404(5) . ? C15 C16 1.416(5) . ? C16 C17 1.391(5) . ? C16 C21 1.510(5) . ? C17 C18 1.369(5) . ? C18 C19 1.387(5) . ? C19 C20 1.389(5) . ? C21 C27 1.526(5) . ? C22 C23 1.394(5) . ? C22 C27 1.399(5) . ? C23 C24 1.391(5) . ? C23 C28 1.501(5) . ? C24 C25 1.393(5) . ? C25 C26 1.367(5) . ? C26 C27 1.394(5) . ? C28 C34 1.523(5) . ? C29 C34 1.395(5) . ? C29 C30 1.399(5) . ? C30 C31 1.400(5) . ? C30 C35 1.521(5) . ? C31 C32 1.375(5) . ? C32 C33 1.390(5) . ? C33 C34 1.400(5) . ? C35 C37 1.518(5) . ? C36 C41 1.410(5) . ? C36 C37 1.410(5) . ? C37 C38 1.384(5) . ? C38 C39 1.385(5) . ? C39 C40 1.386(5) . ? C40 C41 1.390(5) . ? C41 C42 1.517(5) . ? C43 C44 1.468(7) . ? C43 C45 1.485(6) . ? C46 C48 1.490(6) . ? C46 C47 1.495(6) . ? C49 C50 1.453(11) . ? C50 C51 1.324(10) . ? C52 C53 1.555(10) . ? C53 C54 1.549(11) . ? C54 C54 1.446(16) 3_556 ? 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 O2 K1 O3 75.11(10) . . ? O2 K1 O1 71.46(10) . . ? O3 K1 O1 73.72(9) . . ? O2 K1 O10 96.38(11) . . ? O3 K1 O10 170.27(11) . . ? O1 K1 O10 108.44(10) . . ? O2 K1 O5 73.78(9) . . ? O3 K1 O5 72.03(8) . . ? O1 K1 O5 136.06(9) . . ? O10 K1 O5 101.30(9) . . ? O2 K1 C3 138.25(10) . . ? O3 K1 C3 99.63(9) . . ? O1 K1 C3 147.99(10) . . ? O10 K1 C3 83.47(10) . . ? O5 K1 C3 65.45(8) . . ? O2 K1 C4 157.12(10) . . ? O3 K1 C4 114.83(9) . . ? O1 K1 C4 130.25(10) . . ? O10 K1 C4 71.42(10) . . ? O5 K1 C4 89.35(8) . . ? C3 K1 C4 24.71(8) . . ? O2 K1 C2 130.89(9) . . ? O3 K1 C2 75.28(9) . . ? O1 K1 C2 133.58(9) . . ? O10 K1 C2 107.95(9) . . ? O5 K1 C2 60.20(8) . . ? C3 K1 C2 24.52(8) . . ? C4 K1 C2 43.15(9) . . ? O2 K1 C5 178.86(10) . . ? O3 K1 C5 104.03(9) . . ? O1 K1 C5 107.62(9) . . ? O10 K1 C5 84.53(10) . . ? O5 K1 C5 106.73(9) . . ? C3 K1 C5 42.48(9) . . ? C4 K1 C5 23.96(9) . . ? C2 K1 C5 49.24(8) . . ? O2 K1 C1 138.29(9) . . ? O3 K1 C1 66.30(9) . . ? O1 K1 C1 110.34(9) . . ? O10 K1 C1 120.26(9) . . ? O5 K1 C1 79.68(8) . . ? C3 K1 C1 42.06(8) . . ? C4 K1 C1 48.86(8) . . ? C2 K1 C1 23.83(8) . . ? C5 K1 C1 41.22(8) . . ? O2 K1 C6 155.57(9) . . ? O3 K1 C6 80.67(9) . . ? O1 K1 C6 98.82(9) . . ? O10 K1 C6 108.01(10) . . ? O5 K1 C6 101.90(8) . . ? C3 K1 C6 49.30(8) . . ? C4 K1 C6 42.09(9) . . ? C2 K1 C6 42.24(8) . . ? C5 K1 C6 23.48(8) . . ? C1 K1 C6 23.51(8) . . ? O2 K1 K2 42.60(7) . . ? O3 K1 K2 45.38(7) . . ? O1 K1 K2 42.97(7) . . ? O10 K1 K2 130.01(8) . . ? O5 K1 K2 93.09(6) . . ? C3 K1 K2 144.59(7) . . ? C4 K1 K2 157.12(7) . . ? C2 K1 K2 120.58(6) . . ? C5 K1 K2 136.26(7) . . ? C1 K1 K2 109.30(6) . . ? C6 K1 K2 115.40(6) . . ? O11 K2 O2 100.66(9) . . ? O11 K2 O1 151.57(10) . . ? O2 K2 O1 67.43(9) . . ? O11 K2 O7 76.33(7) . . ? O2 K2 O7 70.15(8) . . ? O1 K2 O7 119.57(7) . . ? O11 K2 O3 133.74(8) . . ? O2 K2 O3 68.91(8) . . ? O1 K2 O3 68.00(8) . . ? O7 K2 O3 57.56(7) . . ? O11 K2 O4 90.31(8) . 4_566 ? O2 K2 O4 106.65(9) . 4_566 ? O1 K2 O4 70.11(8) . 4_566 ? O7 K2 O4 165.10(8) . 4_566 ? O3 K2 O4 135.91(8) . 4_566 ? O11 K2 C32 73.72(9) . . ? O2 K2 C32 159.87(10) . . ? O1 K2 C32 125.92(10) . . ? O7 K2 C32 89.72(8) . . ? O3 K2 C32 100.61(9) . . ? O4 K2 C32 92.85(9) 4_566 . ? O11 K2 C33 70.62(9) . . ? O2 K2 C33 135.53(9) . . ? O1 K2 C33 136.25(10) . . ? O7 K2 C33 65.41(8) . . ? O3 K2 C33 85.90(8) . . ? O4 K2 C33 116.66(9) 4_566 . ? C32 K2 C33 24.35(8) . . ? O11 K2 C31 95.83(9) . . ? O2 K2 C31 159.81(9) . . ? O1 K2 C31 102.40(9) . . ? O7 K2 C31 102.94(8) . . ? O3 K2 C31 91.25(9) . . ? O4 K2 C31 84.70(9) 4_566 . ? C32 K2 C31 23.54(9) . . ? C33 K2 C31 41.55(9) . . ? O11 K2 K1 139.43(6) . . ? O2 K2 K1 39.85(6) . . ? O1 K2 K1 40.59(6) . . ? O7 K2 K1 79.62(5) . . ? O3 K2 K1 40.45(6) . . ? O4 K2 K1 107.56(7) 4_566 . ? C32 K2 K1 138.46(7) . . ? C33 K2 K1 126.32(6) . . ? C31 K2 K1 121.30(7) . . ? K1 O1 K2 96.44(9) . . ? K1 O2 K2 97.55(9) . . ? K1 O3 K2 94.17(10) . . ? C1 O4 K2 152.3(2) . 4_565 ? C8 O5 K1 146.6(2) . . ? C22 O7 K2 131.65(18) . . ? C43 O10 K1 129.4(3) . . ? C46 O11 K2 170.2(3) . . ? O4 C1 C2 116.7(3) . . ? O4 C1 C6 122.0(3) . . ? C2 C1 C6 121.3(3) . . ? O4 C1 K1 119.2(2) . . ? C2 C1 K1 72.50(18) . . ? C6 C1 K1 79.70(19) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 122.8(3) . . ? C1 C2 C7 118.3(3) . . ? C3 C2 K1 74.35(18) . . ? C1 C2 K1 83.67(19) . . ? C7 C2 K1 112.7(2) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 K1 81.14(18) . . ? C4 C3 K1 79.7(2) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 K1 82.1(2) . . ? C3 C4 K1 75.58(19) . . ? C4 C5 C6 122.0(3) . . ? C4 C5 K1 74.0(2) . . ? C6 C5 K1 82.6(2) . . ? C5 C6 C1 117.4(3) . . ? C5 C6 C42 120.1(3) . . ? C1 C6 C42 122.5(3) . . ? C5 C6 K1 73.9(2) . . ? C1 C6 K1 76.79(19) . . ? C42 C6 K1 120.7(2) . . ? C13 C7 C2 118.2(3) . . ? O5 C8 C13 117.5(3) . . ? O5 C8 C9 120.8(3) . . ? C13 C8 C9 121.7(3) . . ? C10 C9 C8 117.9(3) . . ? C10 C9 C14 120.9(3) . . ? C8 C9 C14 121.2(3) . . ? C11 C10 C9 121.3(3) . . ? C12 C11 C10 119.8(3) . . ? C11 C12 C13 121.4(3) . . ? C12 C13 C8 117.8(3) . . ? C12 C13 C7 121.5(3) . . ? C8 C13 C7 120.4(3) . . ? C9 C14 C20 117.4(3) . . ? O6 C15 C20 120.0(3) . . ? O6 C15 C16 120.1(3) . . ? C20 C15 C16 119.9(3) . . ? C17 C16 C15 119.1(3) . . ? C17 C16 C21 120.7(3) . . ? C15 C16 C21 120.2(3) . . ? C18 C17 C16 121.1(3) . . ? C17 C18 C19 119.7(3) . . ? C18 C19 C20 121.5(3) . . ? C19 C20 C15 118.7(3) . . ? C19 C20 C14 120.6(3) . . ? C15 C20 C14 120.7(3) . . ? C16 C21 C27 115.0(3) . . ? O7 C22 C23 118.5(3) . . ? O7 C22 C27 119.8(3) . . ? C23 C22 C27 121.8(3) . . ? C24 C23 C22 118.2(3) . . ? C24 C23 C28 121.5(3) . . ? C22 C23 C28 120.3(3) . . ? C23 C24 C25 120.8(3) . . ? C26 C25 C24 119.9(3) . . ? C25 C26 C27 121.5(3) . . ? C26 C27 C22 117.8(3) . . ? C26 C27 C21 120.2(3) . . ? C22 C27 C21 122.0(3) . . ? C23 C28 C34 115.4(3) . . ? O8 C29 C34 116.4(3) . . ? O8 C29 C30 121.6(3) . . ? C34 C29 C30 122.0(3) . . ? C29 C30 C31 117.9(3) . . ? C29 C30 C35 121.6(3) . . ? C31 C30 C35 120.4(3) . . ? C32 C31 C30 121.1(3) . . ? C32 C31 K2 71.1(2) . . ? C30 C31 K2 88.4(2) . . ? C31 C32 C33 120.4(3) . . ? C31 C32 K2 85.3(2) . . ? C33 C32 K2 80.6(2) . . ? C32 C33 C34 120.4(3) . . ? C32 C33 K2 75.01(19) . . ? C34 C33 K2 87.5(2) . . ? C29 C34 C33 118.3(3) . . ? C29 C34 C28 120.2(3) . . ? C33 C34 C28 121.6(3) . . ? C37 C35 C30 116.8(3) . . ? O9 C36 C41 120.1(3) . . ? O9 C36 C37 119.1(3) . . ? C41 C36 C37 120.8(3) . . ? C38 C37 C36 118.7(3) . . ? C38 C37 C35 120.4(3) . . ? C36 C37 C35 120.8(3) . . ? C37 C38 C39 120.9(4) . . ? C38 C39 C40 120.3(4) . . ? C39 C40 C41 120.9(4) . . ? C40 C41 C36 118.4(3) . . ? C40 C41 C42 121.0(3) . . ? C36 C41 C42 120.5(3) . . ? C41 C42 C6 116.4(3) . . ? O10 C43 C44 120.8(5) . . ? O10 C43 C45 121.9(5) . . ? C44 C43 C45 117.3(5) . . ? O11 C46 C48 122.0(4) . . ? O11 C46 C47 122.0(4) . . ? C48 C46 C47 116.0(4) . . ? O12 C50 C51 133.7(9) . . ? O12 C50 C49 105.9(8) . . ? C51 C50 C49 120.3(8) . . ? C54 C53 C52 110.1(6) . . ? C54 C54 C53 111.3(10) 3_556 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.530 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.050 #===END data_34 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H65 O12 Rb2' _chemical_formula_weight 1077.00 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' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.3918(8) _cell_length_b 25.2018(15) _cell_length_c 15.1928(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.4530(10) _cell_angle_gamma 90.00 _cell_volume 5256.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21996 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6874 _reflns_number_gt 5165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0692P)^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 SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6874 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 13.538 _refine_ls_shift/su_mean 0.290 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 Rb1 Rb 0.37779(3) 0.627633(15) 0.79915(3) 0.04958(16) Uani 1 1 d . . . Rb2 Rb 0.51745(3) 0.776729(16) 0.91980(3) 0.04847(16) Uani 1 1 d . . . O1 O 0.3251(2) 0.72497(12) 0.8649(2) 0.0587(8) Uani 1 1 d . . . O2 O 0.4835(2) 0.71058(13) 0.7413(3) 0.0537(9) Uani 1 1 d . . . O3 O 0.5310(3) 0.6567(2) 0.9581(3) 0.0787(12) Uani 1 1 d . . . O4 O 0.3900(2) 0.67594(13) 0.5269(2) 0.0444(8) Uani 1 1 d . . . O5 O 0.56997(19) 0.59300(11) 0.77949(18) 0.0420(7) Uani 1 1 d . . . O6 O 0.69540(17) 0.63733(10) 0.91527(15) 0.0368(6) Uani 1 1 d . . . H6 H 0.6600 0.6343 0.9492 0.055 Uiso 1 1 calc R . . O7 O 0.67839(16) 0.73052(9) 0.85781(15) 0.0359(6) Uani 1 1 d . . . O8 O 0.4888(3) 0.80091(15) 0.6072(2) 0.0432(10) Uani 1 1 d . . . O9 O 0.31798(17) 0.76776(10) 0.53883(16) 0.0410(7) Uani 1 1 d . . . H9 H 0.3736 0.7790 0.5651 0.061 Uiso 1 1 calc R . . O10 O 0.3200(3) 0.53412(14) 0.8814(3) 0.1052(13) Uani 1 1 d . . . O11 O 0.6901(2) 0.81753(13) 1.0556(2) 0.0748(10) Uani 1 1 d . . . O12 O 0.1178(7) 0.6211(3) 0.7611(5) 0.272(4) Uani 1 1 d . . . C1 C 0.3514(3) 0.63420(14) 0.5613(2) 0.0346(9) Uani 1 1 d . . . C2 C 0.2554(3) 0.63508(15) 0.5651(2) 0.0394(10) Uani 1 1 d . . . C3 C 0.2212(3) 0.58963(17) 0.5980(3) 0.0468(10) Uani 1 1 d . . . H3 H 0.1511 0.5870 0.5926 0.056 Uiso 1 1 calc R . . C4 C 0.2799(3) 0.54570(16) 0.6264(2) 0.0456(10) Uani 1 1 d . . . H4 H 0.2508 0.5119 0.6383 0.055 Uiso 1 1 calc R . . C5 C 0.3754(3) 0.54665(15) 0.6236(2) 0.0378(9) Uani 1 1 d . . . H5 H 0.4144 0.5136 0.6362 0.045 Uiso 1 1 calc R . . C6 C 0.4122(3) 0.59065(14) 0.5914(2) 0.0328(9) Uani 1 1 d . . . C7 C 0.5164(3) 0.59392(15) 0.5877(2) 0.0379(9) Uani 1 1 d . . . H7A H 0.5149 0.5900 0.5230 0.045 Uiso 1 1 calc R . . H7B H 0.5408 0.6297 0.6072 0.045 Uiso 1 1 calc R . . C8 C 0.6180(2) 0.55720(14) 0.7406(2) 0.0333(9) Uani 1 1 d . . . C9 C 0.5890(3) 0.55495(14) 0.6436(2) 0.0343(9) Uani 1 1 d . . . C10 C 0.6366(3) 0.51919(15) 0.6033(3) 0.0430(10) Uani 1 1 d . . . H10 H 0.6171 0.5159 0.5387 0.052 Uiso 1 1 calc R . . C11 C 0.7119(3) 0.48825(15) 0.6555(3) 0.0464(10) Uani 1 1 d . . . H11 H 0.7448 0.4651 0.6265 0.056 Uiso 1 1 calc R . . C12 C 0.7389(3) 0.49128(14) 0.7507(3) 0.0420(10) Uani 1 1 d . . . H12 H 0.7903 0.4701 0.7861 0.050 Uiso 1 1 calc R . . C13 C 0.6911(3) 0.52508(14) 0.7945(2) 0.0349(9) Uani 1 1 d . . . C14 C 0.7173(3) 0.52527(15) 0.8993(2) 0.0425(10) Uani 1 1 d . . . H14A H 0.6588 0.5349 0.9160 0.051 Uiso 1 1 calc R . . H14B H 0.7347 0.4889 0.9211 0.051 Uiso 1 1 calc R . . C15 C 0.7839(3) 0.61628(15) 0.9578(2) 0.0357(9) Uani 1 1 d . . . C16 C 0.7992(3) 0.56159(15) 0.9516(2) 0.0378(9) Uani 1 1 d . . . C17 C 0.8897(3) 0.54126(17) 0.9996(3) 0.0499(11) Uani 1 1 d . . . H17 H 0.9005 0.5046 0.9965 0.060 Uiso 1 1 calc R . . C18 C 0.9640(3) 0.57239(19) 1.0514(3) 0.0575(12) Uani 1 1 d . . . H18 H 1.0247 0.5575 1.0832 0.069 Uiso 1 1 calc R . . C19 C 0.9476(3) 0.62611(18) 1.0558(3) 0.0513(11) Uani 1 1 d . . . H19 H 0.9981 0.6478 1.0914 0.062 Uiso 1 1 calc R . . C20 C 0.8593(3) 0.64900(15) 1.0094(2) 0.0371(9) Uani 1 1 d . . . C21 C 0.8442(3) 0.70794(15) 1.0162(2) 0.0418(10) Uani 1 1 d . . . H21A H 0.8934 0.7215 1.0712 0.050 Uiso 1 1 calc R . . H21B H 0.7802 0.7138 1.0248 0.050 Uiso 1 1 calc R . . C22 C 0.7665(3) 0.75149(14) 0.8596(2) 0.0330(9) Uani 1 1 d . . . C23 C 0.8500(3) 0.73972(14) 0.9331(2) 0.0371(9) Uani 1 1 d . . . C24 C 0.9378(3) 0.75962(17) 0.9283(3) 0.0510(11) Uani 1 1 d . . . H24 H 0.9949 0.7515 0.9758 0.061 Uiso 1 1 calc R . . C25 C 0.9443(3) 0.79079(18) 0.8565(3) 0.0570(12) Uani 1 1 d . . . H25 H 1.0053 0.8033 0.8549 0.068 Uiso 1 1 calc R . . C26 C 0.8613(3) 0.80388(16) 0.7865(3) 0.0475(11) Uani 1 1 d . . . H26 H 0.8657 0.8261 0.7383 0.057 Uiso 1 1 calc R . . C27 C 0.7715(3) 0.78444(14) 0.7869(2) 0.0341(9) Uani 1 1 d . . . C28 C 0.6804(2) 0.79729(14) 0.7109(2) 0.0354(9) Uani 1 1 d . . . H28A H 0.6491 0.7639 0.6849 0.042 Uiso 1 1 calc R . . H28B H 0.6987 0.8159 0.6620 0.042 Uiso 1 1 calc R . . C29 C 0.5095(3) 0.83085(14) 0.6851(2) 0.0343(9) Uani 1 1 d . . . C30 C 0.6065(3) 0.83089(13) 0.7387(2) 0.0329(9) Uani 1 1 d . . . C31 C 0.6331(3) 0.86273(14) 0.8162(2) 0.0402(10) Uani 1 1 d . . . H31 H 0.7030 0.8702 0.8459 0.048 Uiso 1 1 calc R . . C32 C 0.5641(3) 0.89312(15) 0.8411(3) 0.0482(11) Uani 1 1 d . . . H32 H 0.5865 0.9228 0.8851 0.058 Uiso 1 1 calc R . . C33 C 0.4680(3) 0.89179(15) 0.7869(3) 0.0481(11) Uani 1 1 d . . . H33 H 0.4218 0.9180 0.7986 0.058 Uiso 1 1 calc R . . C34 C 0.4382(3) 0.86050(14) 0.7079(3) 0.0399(10) Uani 1 1 d . . . C35 C 0.3335(3) 0.86213(15) 0.6464(3) 0.0486(11) Uani 1 1 d . . . H35A H 0.3342 0.8652 0.5823 0.058 Uiso 1 1 calc R . . H35B H 0.3034 0.8945 0.6610 0.058 Uiso 1 1 calc R . . C36 C 0.2636(3) 0.77097(15) 0.5963(3) 0.0386(10) Uani 1 1 d . . . C37 C 0.2688(3) 0.81573(16) 0.6523(3) 0.0434(10) Uani 1 1 d . . . C38 C 0.2103(3) 0.81816(19) 0.7087(3) 0.0561(12) Uani 1 1 d . . . H38 H 0.2135 0.8481 0.7463 0.067 Uiso 1 1 calc R . . C39 C 0.1459(3) 0.7772(2) 0.7116(3) 0.0648(14) Uani 1 1 d . . . H39 H 0.1062 0.7796 0.7505 0.078 Uiso 1 1 calc R . . C40 C 0.1413(3) 0.73267(19) 0.6562(3) 0.0550(12) Uani 1 1 d . . . H40 H 0.0987 0.7048 0.6586 0.066 Uiso 1 1 calc R . . C41 C 0.1989(3) 0.72906(16) 0.5975(3) 0.0442(10) Uani 1 1 d . . . C42 C 0.1882(3) 0.68199(15) 0.5323(3) 0.0453(10) Uani 1 1 d . . . H42A H 0.1210 0.6692 0.5174 0.054 Uiso 1 1 calc R . . H42B H 0.1977 0.6949 0.4748 0.054 Uiso 1 1 calc R . . C43 C 0.3377(4) 0.4889(2) 0.8683(3) 0.0684(14) Uani 1 1 d . . . C44 C 0.4389(5) 0.4722(3) 0.8785(4) 0.114(2) Uani 1 1 d . . . H44A H 0.4823 0.5023 0.8979 0.170 Uiso 1 1 calc R . . H44B H 0.4433 0.4591 0.8199 0.170 Uiso 1 1 calc R . . H44C H 0.4576 0.4443 0.9245 0.170 Uiso 1 1 calc R . . C45 C 0.2633(4) 0.4477(2) 0.8414(4) 0.0981(19) Uani 1 1 d . . . H45A H 0.1993 0.4637 0.8289 0.147 Uiso 1 1 calc R . . H45B H 0.2728 0.4222 0.8911 0.147 Uiso 1 1 calc R . . H45C H 0.2682 0.4299 0.7864 0.147 Uiso 1 1 calc R . . C46 C 0.7600(3) 0.84073(17) 1.1035(3) 0.0532(11) Uani 1 1 d . . . C47 C 0.8337(4) 0.8645(3) 1.0644(3) 0.102(2) Uani 1 1 d . . . H47A H 0.8229 0.8518 1.0019 0.153 Uiso 1 1 calc R . . H47B H 0.8985 0.8544 1.1020 0.153 Uiso 1 1 calc R . . H47C H 0.8277 0.9029 1.0639 0.153 Uiso 1 1 calc R . . C48 C 0.7781(3) 0.84763(19) 1.2038(3) 0.0640(13) Uani 1 1 d . . . H48A H 0.7245 0.8324 1.2217 0.096 Uiso 1 1 calc R . . H48B H 0.7833 0.8851 1.2188 0.096 Uiso 1 1 calc R . . H48C H 0.8382 0.8299 1.2369 0.096 Uiso 1 1 calc R . . C49 C 0.0884(6) 0.6126(3) 0.8244(5) 0.115(2) Uani 1 1 d . . . C50 C 0.1304(6) 0.6342(4) 0.9108(6) 0.214(6) Uani 1 1 d . . . H50A H 0.1955 0.6465 0.9155 0.321 Uiso 1 1 calc R . . H50B H 0.1337 0.6074 0.9575 0.321 Uiso 1 1 calc R . . H50C H 0.0913 0.6638 0.9200 0.321 Uiso 1 1 calc R . . C51 C 0.0142(5) 0.5701(3) 0.8159(4) 0.136(3) Uani 1 1 d . . . H51A H -0.0225 0.5655 0.7514 0.205 Uiso 1 1 calc R . . H51B H -0.0298 0.5802 0.8505 0.205 Uiso 1 1 calc R . . H51C H 0.0465 0.5371 0.8402 0.205 Uiso 1 1 calc R . . C52 C 0.0178(5) 0.5053(3) 0.4562(5) 0.141(3) Uani 1 1 d . . . H52A H 0.0890 0.5086 0.4761 0.169 Uiso 1 1 calc R . . H52B H 0.0003 0.4749 0.4143 0.169 Uiso 1 1 calc R . . C53 C -0.0259(5) 0.5549(3) 0.4049(5) 0.130(3) Uani 1 1 d . . . H53A H -0.0181 0.5846 0.4481 0.156 Uiso 1 1 calc R . . H53B H -0.0957 0.5496 0.3746 0.156 Uiso 1 1 calc R . . C54 C 0.0265(5) 0.5676(3) 0.3314(5) 0.140(3) Uani 1 1 d . . . H54A H 0.0926 0.5791 0.3621 0.210 Uiso 1 1 calc R . . H54B H -0.0084 0.5955 0.2910 0.210 Uiso 1 1 calc R . . H54C H 0.0280 0.5360 0.2954 0.210 Uiso 1 1 calc R . . H1A H 0.327(7) 0.729(4) 0.938(8) 0.34(5) Uiso 1 1 d . . . H1B H 0.261(4) 0.742(3) 0.821(4) 0.15(2) Uiso 1 1 d . . . H2B H 0.490(4) 0.716(2) 0.705(4) 0.09(3) Uiso 1 1 d . . . H3A H 0.535(5) 0.667(3) 1.007(5) 0.18(4) Uiso 1 1 d . . . H3B H 0.539(2) 0.6233(13) 0.975(2) 0.014(10) Uiso 1 1 d . . . H4A H 0.367(3) 0.6999(15) 0.530(3) 0.027(14) Uiso 1 1 d . . . H5A H 0.607(3) 0.6078(17) 0.825(3) 0.061(14) Uiso 1 1 d . . . H8 H 0.450(2) 0.7988(16) 0.595(3) 0.000(13) Uiso 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 Rb1 0.0642(3) 0.0423(3) 0.0417(2) -0.00676(18) 0.0152(2) -0.0057(2) Rb2 0.0470(3) 0.0435(3) 0.0605(3) -0.0080(2) 0.0247(2) -0.00482(19) O1 0.056(2) 0.068(2) 0.0453(18) -0.0052(15) 0.0052(15) 0.0106(16) O2 0.061(2) 0.053(2) 0.046(2) 0.0077(16) 0.0140(17) -0.0016(15) O3 0.068(2) 0.123(4) 0.044(2) -0.010(2) 0.0143(17) 0.015(2) O4 0.0420(18) 0.0403(19) 0.0545(18) 0.0118(16) 0.0197(14) 0.0076(16) O5 0.0371(16) 0.0489(18) 0.0370(15) -0.0106(14) 0.0064(13) 0.0092(14) O6 0.0318(15) 0.0413(15) 0.0385(14) 0.0034(12) 0.0122(12) 0.0039(12) O7 0.0243(14) 0.0431(16) 0.0385(14) 0.0021(12) 0.0068(11) -0.0019(12) O8 0.033(2) 0.051(2) 0.045(2) 0.0009(14) 0.0098(18) 0.0026(19) O9 0.0330(15) 0.0499(17) 0.0389(15) 0.0033(13) 0.0091(12) 0.0006(13) O10 0.168(4) 0.048(2) 0.124(3) 0.007(2) 0.082(3) 0.007(2) O11 0.056(2) 0.071(2) 0.088(2) -0.0215(19) 0.0097(18) -0.0118(18) O12 0.546(12) 0.163(6) 0.220(6) 0.008(5) 0.288(8) -0.044(6) C1 0.035(2) 0.038(2) 0.029(2) 0.0009(17) 0.0066(17) -0.0061(19) C2 0.034(2) 0.047(3) 0.034(2) 0.0002(19) 0.0057(18) -0.0059(19) C3 0.030(2) 0.057(3) 0.050(2) -0.002(2) 0.0060(19) -0.010(2) C4 0.050(3) 0.042(3) 0.044(2) -0.0044(19) 0.012(2) -0.016(2) C5 0.043(3) 0.032(2) 0.035(2) -0.0085(17) 0.0077(18) -0.0028(18) C6 0.036(2) 0.036(2) 0.0254(19) -0.0040(17) 0.0066(16) -0.0052(18) C7 0.040(2) 0.043(2) 0.033(2) 0.0011(18) 0.0135(18) 0.0018(19) C8 0.031(2) 0.032(2) 0.040(2) -0.0033(18) 0.0155(18) 0.0002(18) C9 0.035(2) 0.034(2) 0.035(2) -0.0011(17) 0.0131(17) 0.0014(18) C10 0.047(3) 0.044(2) 0.042(2) -0.006(2) 0.019(2) 0.001(2) C11 0.046(3) 0.039(2) 0.059(3) -0.007(2) 0.024(2) 0.006(2) C12 0.038(2) 0.030(2) 0.057(3) 0.0014(19) 0.014(2) 0.0036(18) C13 0.036(2) 0.027(2) 0.041(2) 0.0015(18) 0.0121(18) 0.0005(18) C14 0.048(3) 0.034(2) 0.046(2) 0.0060(19) 0.0139(19) 0.0056(19) C15 0.030(2) 0.044(3) 0.030(2) 0.0060(18) 0.0061(17) 0.0080(19) C16 0.037(2) 0.041(2) 0.033(2) 0.0072(18) 0.0080(18) 0.0081(19) C17 0.052(3) 0.047(3) 0.046(2) 0.004(2) 0.008(2) 0.016(2) C18 0.045(3) 0.068(3) 0.049(3) 0.003(2) -0.002(2) 0.018(2) C19 0.038(3) 0.064(3) 0.043(2) -0.003(2) -0.001(2) 0.002(2) C20 0.036(2) 0.047(2) 0.0250(19) 0.0017(18) 0.0051(17) 0.004(2) C21 0.038(2) 0.050(3) 0.029(2) -0.0042(18) -0.0028(17) -0.0036(19) C22 0.031(2) 0.034(2) 0.031(2) -0.0067(17) 0.0065(17) -0.0009(18) C23 0.034(2) 0.040(2) 0.035(2) -0.0034(18) 0.0055(18) -0.0050(18) C24 0.031(2) 0.065(3) 0.047(3) 0.000(2) -0.0040(19) -0.010(2) C25 0.032(3) 0.078(3) 0.059(3) -0.001(3) 0.011(2) -0.018(2) C26 0.048(3) 0.055(3) 0.041(2) 0.001(2) 0.015(2) -0.010(2) C27 0.032(2) 0.039(2) 0.031(2) -0.0032(17) 0.0091(17) -0.0049(18) C28 0.036(2) 0.037(2) 0.032(2) 0.0009(17) 0.0084(17) -0.0024(18) C29 0.048(3) 0.028(2) 0.028(2) 0.0012(17) 0.0137(19) 0.0008(19) C30 0.042(2) 0.028(2) 0.031(2) 0.0048(17) 0.0145(18) 0.0003(18) C31 0.046(2) 0.037(2) 0.038(2) 0.0023(19) 0.0130(19) -0.005(2) C32 0.068(3) 0.033(2) 0.044(2) -0.0033(19) 0.018(2) -0.004(2) C33 0.066(3) 0.034(2) 0.052(3) 0.006(2) 0.029(2) 0.012(2) C34 0.046(3) 0.032(2) 0.044(2) 0.0065(19) 0.016(2) 0.0053(19) C35 0.052(3) 0.039(2) 0.057(3) 0.006(2) 0.020(2) 0.017(2) C36 0.025(2) 0.049(3) 0.041(2) 0.013(2) 0.0084(18) 0.0110(19) C37 0.034(2) 0.048(3) 0.048(2) 0.005(2) 0.012(2) 0.016(2) C38 0.055(3) 0.063(3) 0.052(3) 0.005(2) 0.019(2) 0.018(3) C39 0.053(3) 0.089(4) 0.060(3) 0.012(3) 0.028(2) 0.024(3) C40 0.033(2) 0.075(3) 0.057(3) 0.020(3) 0.014(2) 0.009(2) C41 0.026(2) 0.058(3) 0.045(2) 0.012(2) 0.0041(19) 0.012(2) C42 0.026(2) 0.059(3) 0.047(2) 0.010(2) 0.0045(18) -0.001(2) C43 0.115(5) 0.055(3) 0.051(3) 0.003(2) 0.048(3) 0.004(3) C44 0.130(6) 0.112(5) 0.095(5) -0.028(4) 0.029(4) 0.000(4) C45 0.130(5) 0.090(4) 0.100(4) -0.019(4) 0.072(4) -0.021(4) C46 0.053(3) 0.045(3) 0.062(3) -0.007(2) 0.018(2) 0.004(2) C47 0.105(5) 0.144(6) 0.067(3) -0.031(4) 0.041(3) -0.050(4) C48 0.067(3) 0.063(3) 0.063(3) 0.006(2) 0.021(2) -0.003(2) C49 0.182(8) 0.100(5) 0.089(5) 0.000(4) 0.081(5) -0.028(5) C50 0.218(10) 0.291(14) 0.174(8) -0.129(9) 0.123(8) -0.184(10) C51 0.159(7) 0.136(7) 0.088(5) 0.018(4) -0.003(4) -0.021(6) C52 0.093(6) 0.119(6) 0.180(9) -0.028(7) -0.005(5) -0.027(5) C53 0.115(6) 0.105(6) 0.146(7) 0.016(5) 0.001(5) 0.013(5) C54 0.147(7) 0.132(7) 0.135(6) -0.008(5) 0.033(5) 0.046(5) _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 Rb1 O3 2.835(4) . ? Rb1 O1 2.837(3) . ? Rb1 O2 2.874(4) . ? Rb1 O10 2.904(4) . ? Rb1 O5 2.999(3) . ? Rb1 C4 3.304(4) . ? Rb1 C3 3.347(4) . ? Rb1 C5 3.350(3) . ? Rb1 O12 3.614(9) . ? Rb1 C6 3.466(3) . ? Rb1 C2 3.467(3) . ? Rb1 C1 3.522(3) . ? Rb2 O11 2.900(3) . ? Rb2 O1 2.945(3) . ? Rb2 O7 2.986(2) . ? Rb2 O4 3.037(3) 4_576 ? Rb2 O3 3.074(6) . ? Rb2 O2 3.095(4) . ? Rb2 C32 3.312(4) . ? Rb2 C31 3.393(4) . ? Rb2 C33 3.483(4) . ? Rb2 O8 3.579(4) 4_576 ? Rb2 C30 3.632(3) . ? Rb2 C34 3.731(4) . ? O4 C1 1.365(4) . ? O4 Rb2 3.037(3) 4_575 ? O5 C8 1.373(4) . ? O6 C15 1.351(4) . ? O7 C22 1.367(4) . ? O8 C29 1.359(5) . ? O8 Rb2 3.579(4) 4_575 ? O9 C36 1.338(4) . ? O10 C43 1.197(5) . ? O11 C46 1.202(5) . ? O12 C49 1.180(7) . ? C1 C6 1.393(5) . ? C1 C2 1.401(5) . ? C2 C3 1.396(5) . ? C2 C42 1.514(5) . ? C3 C4 1.381(5) . ? C4 C5 1.388(5) . ? C5 C6 1.381(5) . ? C6 C7 1.520(5) . ? C7 C9 1.498(5) . ? C8 C13 1.384(5) . ? C8 C9 1.406(5) . ? C9 C10 1.382(5) . ? C10 C11 1.377(5) . ? C11 C12 1.382(5) . ? C12 C13 1.384(5) . ? C13 C14 1.523(5) . ? C14 C16 1.515(5) . ? C15 C20 1.401(5) . ? C15 C16 1.404(5) . ? C16 C17 1.386(5) . ? C17 C18 1.368(6) . ? C18 C19 1.379(6) . ? C19 C20 1.381(5) . ? C20 C21 1.509(5) . ? C21 C23 1.518(5) . ? C22 C27 1.400(5) . ? C22 C23 1.405(5) . ? C23 C24 1.382(5) . ? C24 C25 1.370(6) . ? C25 C26 1.380(5) . ? C26 C27 1.384(5) . ? C27 C28 1.499(5) . ? C28 C30 1.515(5) . ? C29 C34 1.394(5) . ? C29 C30 1.390(5) . ? C30 C31 1.381(5) . ? C31 C32 1.392(5) . ? C32 C33 1.382(5) . ? C33 C34 1.392(5) . ? C34 C35 1.516(5) . ? C35 C37 1.514(5) . ? C36 C37 1.401(5) . ? C36 C41 1.412(5) . ? C37 C38 1.372(6) . ? C38 C39 1.397(6) . ? C39 C40 1.391(6) . ? C40 C41 1.392(6) . ? C41 C42 1.523(5) . ? C43 C45 1.460(7) . ? C43 C44 1.478(7) . ? C46 C48 1.478(6) . ? C46 C47 1.488(6) . ? C49 C50 1.382(9) . ? C49 C51 1.491(9) . ? C52 C53 1.506(10) . ? C52 C52 1.586(14) 3_566 ? C53 C54 1.557(9) . ? 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 O3 Rb1 O1 72.42(12) . . ? O3 Rb1 O2 74.01(12) . . ? O1 Rb1 O2 72.58(10) . . ? O3 Rb1 O10 95.36(13) . . ? O1 Rb1 O10 114.13(10) . . ? O2 Rb1 O10 165.53(11) . . ? O3 Rb1 O5 69.83(10) . . ? O1 Rb1 O5 129.69(9) . . ? O2 Rb1 O5 65.97(9) . . ? O10 Rb1 O5 101.44(10) . . ? O3 Rb1 C4 151.13(13) . . ? O1 Rb1 C4 136.46(10) . . ? O2 Rb1 C4 110.52(10) . . ? O10 Rb1 C4 74.07(11) . . ? O5 Rb1 C4 85.73(9) . . ? O3 Rb1 C3 172.04(11) . . ? O1 Rb1 C3 113.03(10) . . ? O2 Rb1 C3 101.66(10) . . ? O10 Rb1 C3 87.68(11) . . ? O5 Rb1 C3 102.37(9) . . ? C4 Rb1 C3 23.95(9) . . ? O3 Rb1 C5 130.95(11) . . ? O1 Rb1 C5 150.15(9) . . ? O2 Rb1 C5 94.58(10) . . ? O10 Rb1 C5 84.96(10) . . ? O5 Rb1 C5 62.17(8) . . ? C4 Rb1 C5 24.07(9) . . ? C3 Rb1 C5 41.88(10) . . ? O3 Rb1 O12 130.65(13) . . ? O1 Rb1 O12 73.89(12) . . ? O2 Rb1 O12 127.00(12) . . ? O10 Rb1 O12 67.39(14) . . ? O5 Rb1 O12 155.80(12) . . ? C4 Rb1 O12 70.73(13) . . ? C3 Rb1 O12 57.30(12) . . ? C5 Rb1 O12 94.69(12) . . ? O3 Rb1 C6 123.93(10) . . ? O1 Rb1 C6 132.82(9) . . ? O2 Rb1 C6 71.57(9) . . ? O10 Rb1 C6 108.14(10) . . ? O5 Rb1 C6 56.16(8) . . ? C4 Rb1 C6 41.60(9) . . ? C3 Rb1 C6 48.13(9) . . ? C5 Rb1 C6 23.29(8) . . ? O12 Rb1 C6 105.42(12) . . ? O3 Rb1 C2 152.33(11) . . ? O1 Rb1 C2 101.96(9) . . ? O2 Rb1 C2 78.45(9) . . ? O10 Rb1 C2 111.24(11) . . ? O5 Rb1 C2 96.54(8) . . ? C4 Rb1 C2 41.84(9) . . ? C3 Rb1 C2 23.56(9) . . ? C5 Rb1 C2 48.39(9) . . ? O12 Rb1 C2 69.83(12) . . ? C6 Rb1 C2 41.26(9) . . ? O3 Rb1 C1 132.74(10) . . ? O1 Rb1 C1 111.28(9) . . ? O2 Rb1 C1 63.65(9) . . ? O10 Rb1 C1 121.54(10) . . ? O5 Rb1 C1 74.36(8) . . ? C4 Rb1 C1 47.59(9) . . ? C3 Rb1 C1 40.61(9) . . ? C5 Rb1 C1 40.52(9) . . ? O12 Rb1 C1 92.87(12) . . ? C6 Rb1 C1 22.97(8) . . ? C2 Rb1 C1 23.11(8) . . ? O11 Rb2 O1 152.89(9) . . ? O11 Rb2 O7 77.44(8) . . ? O1 Rb2 O7 119.35(7) . . ? O11 Rb2 O4 90.34(9) . 4_576 ? O1 Rb2 O4 70.00(8) . 4_576 ? O7 Rb2 O4 166.50(7) . 4_576 ? O11 Rb2 O3 102.81(10) . . ? O1 Rb2 O3 67.60(9) . . ? O7 Rb2 O3 70.42(8) . . ? O4 Rb2 O3 107.41(10) 4_576 . ? O11 Rb2 O2 133.69(9) . . ? O1 Rb2 O2 68.00(9) . . ? O7 Rb2 O2 56.44(8) . . ? O4 Rb2 O2 135.96(9) 4_576 . ? O3 Rb2 O2 67.70(9) . . ? O11 Rb2 C32 73.72(10) . . ? O1 Rb2 C32 124.42(10) . . ? O7 Rb2 C32 88.34(9) . . ? O4 Rb2 C32 93.79(10) 4_576 . ? O3 Rb2 C32 158.63(10) . . ? O2 Rb2 C32 99.01(10) . . ? O11 Rb2 C31 70.67(9) . . ? O1 Rb2 C31 134.56(9) . . ? O7 Rb2 C31 64.42(8) . . ? O4 Rb2 C31 117.16(9) 4_576 . ? O3 Rb2 C31 134.74(10) . . ? O2 Rb2 C31 84.73(9) . . ? C32 Rb2 C31 23.93(9) . . ? O11 Rb2 C33 95.73(10) . . ? O1 Rb2 C33 101.14(10) . . ? O7 Rb2 C33 100.66(8) . . ? O4 Rb2 C33 86.11(9) 4_576 . ? O3 Rb2 C33 156.77(10) . . ? O2 Rb2 C33 89.39(9) . . ? C32 Rb2 C33 23.30(9) . . ? C31 Rb2 C33 40.77(10) . . ? O11 Rb2 O8 84.62(9) . 4_576 ? O1 Rb2 O8 70.14(9) . 4_576 ? O7 Rb2 O8 108.84(8) . 4_576 ? O4 Rb2 O8 63.68(9) 4_576 4_576 ? O3 Rb2 O8 47.74(9) . 4_576 ? O2 Rb2 O8 112.15(9) . 4_576 ? C32 Rb2 O8 148.84(9) . 4_576 ? C31 Rb2 O8 155.18(9) . 4_576 ? C33 Rb2 O8 149.79(9) . 4_576 ? O11 Rb2 C30 89.09(9) . . ? O1 Rb2 C30 117.86(8) . . ? O7 Rb2 C30 54.86(7) . . ? O4 Rb2 C30 131.69(9) 4_576 . ? O3 Rb2 C30 119.75(9) . . ? O2 Rb2 C30 62.45(9) . . ? C32 Rb2 C30 40.33(9) . . ? C31 Rb2 C30 22.34(8) . . ? C33 Rb2 C30 45.98(9) . . ? O8 Rb2 C30 163.56(9) 4_576 . ? O11 Rb2 C34 112.84(9) . . ? O1 Rb2 C34 89.33(9) . . ? O7 Rb2 C34 90.80(7) . . ? O4 Rb2 C34 99.34(8) 4_576 . ? O3 Rb2 C34 134.88(9) . . ? O2 Rb2 C34 67.77(9) . . ? C32 Rb2 C34 39.63(9) . . ? C31 Rb2 C34 45.88(9) . . ? C33 Rb2 C34 21.90(8) . . ? O8 Rb2 C34 156.56(9) 4_576 . ? C30 Rb2 C34 38.71(8) . . ? Rb1 O1 Rb2 98.91(9) . . ? Rb1 O2 Rb2 94.75(11) . . ? Rb1 O3 Rb2 95.98(12) . . ? C1 O4 Rb2 152.7(3) . 4_575 ? C8 O5 Rb1 146.3(2) . . ? C22 O7 Rb2 130.24(19) . . ? C29 O8 Rb2 161.6(3) . 4_575 ? C43 O10 Rb1 126.7(3) . . ? C46 O11 Rb2 170.4(3) . . ? C49 O12 Rb1 119.0(7) . . ? O4 C1 C6 116.4(3) . . ? O4 C1 C2 121.6(3) . . ? C6 C1 C2 122.0(3) . . ? O4 C1 Rb1 119.9(2) . . ? C6 C1 Rb1 76.29(19) . . ? C2 C1 Rb1 76.3(2) . . ? C3 C2 C1 117.3(4) . . ? C3 C2 C42 120.0(4) . . ? C1 C2 C42 122.6(3) . . ? C3 C2 Rb1 73.4(2) . . ? C1 C2 Rb1 80.6(2) . . ? C42 C2 Rb1 117.3(2) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 Rb1 76.3(2) . . ? C2 C3 Rb1 83.0(2) . . ? C3 C4 C5 119.6(4) . . ? C3 C4 Rb1 79.8(2) . . ? C5 C4 Rb1 79.8(2) . . ? C6 C5 C4 120.9(4) . . ? C6 C5 Rb1 83.1(2) . . ? C4 C5 Rb1 76.1(2) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C7 123.0(3) . . ? C1 C6 C7 118.4(3) . . ? C5 C6 Rb1 73.6(2) . . ? C1 C6 Rb1 80.7(2) . . ? C7 C6 Rb1 115.6(2) . . ? C9 C7 C6 118.1(3) . . ? O5 C8 C13 121.4(3) . . ? O5 C8 C9 116.6(3) . . ? C13 C8 C9 122.0(3) . . ? C10 C9 C8 117.4(3) . . ? C10 C9 C7 122.0(3) . . ? C8 C9 C7 120.4(3) . . ? C11 C10 C9 121.5(4) . . ? C10 C11 C12 119.8(4) . . ? C11 C12 C13 120.8(4) . . ? C8 C13 C12 118.3(3) . . ? C8 C13 C14 121.5(3) . . ? C12 C13 C14 120.1(3) . . ? C16 C14 C13 117.4(3) . . ? O6 C15 C20 119.8(3) . . ? O6 C15 C16 119.9(3) . . ? C20 C15 C16 120.3(3) . . ? C17 C16 C15 118.0(4) . . ? C17 C16 C14 120.9(3) . . ? C15 C16 C14 121.0(3) . . ? C18 C17 C16 122.6(4) . . ? C17 C18 C19 118.4(4) . . ? C18 C19 C20 122.0(4) . . ? C19 C20 C15 118.7(4) . . ? C19 C20 C21 120.4(3) . . ? C15 C20 C21 120.9(3) . . ? C20 C21 C23 114.7(3) . . ? O7 C22 C27 118.7(3) . . ? O7 C22 C23 120.0(3) . . ? C27 C22 C23 121.3(3) . . ? C24 C23 C22 117.3(3) . . ? C24 C23 C21 121.0(3) . . ? C22 C23 C21 121.7(3) . . ? C25 C24 C23 122.2(4) . . ? C24 C25 C26 120.0(4) . . ? C25 C26 C27 120.4(4) . . ? C26 C27 C22 118.8(3) . . ? C26 C27 C28 121.4(3) . . ? C22 C27 C28 119.7(3) . . ? C27 C28 C30 115.5(3) . . ? O8 C29 C34 122.0(3) . . ? O8 C29 C30 115.4(4) . . ? C34 C29 C30 122.6(3) . . ? C31 C30 C29 118.2(3) . . ? C31 C30 C28 121.6(3) . . ? C29 C30 C28 120.2(3) . . ? C31 C30 Rb2 69.1(2) . . ? C29 C30 Rb2 85.6(2) . . ? C28 C30 Rb2 116.0(2) . . ? C30 C31 C32 120.9(4) . . ? C30 C31 Rb2 88.6(2) . . ? C32 C31 Rb2 74.8(2) . . ? C33 C32 C31 119.5(4) . . ? C33 C32 Rb2 85.3(2) . . ? C31 C32 Rb2 81.3(2) . . ? C32 C33 C34 121.5(4) . . ? C32 C33 Rb2 71.4(2) . . ? C34 C33 Rb2 89.1(2) . . ? C33 C34 C29 117.3(4) . . ? C33 C34 C35 120.5(3) . . ? C29 C34 C35 122.0(3) . . ? C33 C34 Rb2 69.0(2) . . ? C29 C34 Rb2 81.6(2) . . ? C35 C34 Rb2 122.5(2) . . ? C34 C35 C37 117.2(3) . . ? O9 C36 C37 120.6(4) . . ? O9 C36 C41 118.7(4) . . ? C37 C36 C41 120.7(4) . . ? C38 C37 C36 119.0(4) . . ? C38 C37 C35 120.4(4) . . ? C36 C37 C35 120.5(4) . . ? C37 C38 C39 121.6(4) . . ? C40 C39 C38 119.3(4) . . ? C41 C40 C39 120.7(4) . . ? C40 C41 C36 118.8(4) . . ? C40 C41 C42 120.3(4) . . ? C36 C41 C42 120.9(4) . . ? C2 C42 C41 117.7(3) . . ? O10 C43 C45 123.3(6) . . ? O10 C43 C44 120.3(6) . . ? C45 C43 C44 116.4(5) . . ? O10 C43 Rb1 38.4(3) . . ? C45 C43 Rb1 138.4(4) . . ? C44 C43 Rb1 93.8(4) . . ? O11 C46 C48 122.5(4) . . ? O11 C46 C47 121.5(4) . . ? C48 C46 C47 116.0(4) . . ? O12 C49 C50 122.8(8) . . ? O12 C49 C51 118.8(8) . . ? C50 C49 C51 117.6(6) . . ? C53 C52 C52 112.6(9) . 3_566 ? C52 C53 C54 108.9(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.050 #===END data_35 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H58 Cl2 Cs2 O12' _chemical_formula_weight 1259.74 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' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.4144(11) _cell_length_b 25.3537(19) _cell_length_c 15.1924(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.7150(10) _cell_angle_gamma 90.00 _cell_volume 5288.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19950 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 21.50 _reflns_number_total 6063 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6063 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1306 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.3379 _refine_ls_wR_factor_gt 0.3185 _refine_ls_goodness_of_fit_ref 1.315 _refine_ls_restrained_S_all 1.315 _refine_ls_shift/su_max 3.851 _refine_ls_shift/su_mean 0.048 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 Cs1 Cs 1.12431(10) 0.12702(5) 0.20119(9) 0.0625(6) Uani 1 1 d . . . Cs2 Cs 0.98677(10) 0.27646(5) 0.08109(9) 0.0648(6) Uani 1 1 d . . . Cl1 Cl 0.518(5) 0.994(3) 0.437(5) 0.42(4) Uiso 0.45(3) 1 d P . . Cl2 Cl 0.4946(12) 1.0160(7) 0.3291(12) 0.136(9) Uiso 0.55(3) 1 d P . . O1 O 1.1793(7) 0.2234(4) 0.1339(7) 0.039(3) Uani 1 1 d . . . O2 O 1.0209(7) 0.2109(3) 0.2598(6) 0.023(2) Uani 1 1 d . . . O3 O 0.9707(8) 0.1577(5) 0.0416(7) 0.047(3) Uani 1 1 d . . . O4 O 1.0178(6) 0.3004(3) 0.3935(5) 0.015(2) Uani 1 1 d . . . O5 O 0.8254(6) 0.2304(3) 0.1433(5) 0.013(2) Uani 1 1 d . . . O6 O 0.8083(6) 0.1372(3) 0.0840(6) 0.015(2) Uani 1 1 d . . . O7 O 0.9355(9) 0.0925(5) 0.2235(8) 0.021(3) Uani 1 1 d . . . O8 O 1.1160(6) 0.1762(3) 0.4736(6) 0.019(2) Uani 1 1 d . . . O9 O 1.1885(10) 0.2675(4) 0.4615(8) 0.023(3) Uani 1 1 d . . . O10 O 0.8170(9) 0.3168(4) -0.0541(8) 0.044(3) Uani 1 1 d . . . O11 O 1.1737(12) 0.0317(5) 0.1189(10) 0.078(4) Uani 1 1 d . . . O12 O 1.384(3) 0.1204(9) 0.233(2) 0.24(2) Uani 1 1 d . . . C1 C 0.9932(9) 0.3298(5) 0.3149(9) 0.014(3) Uiso 1 1 d . . . C2 C 0.8997(9) 0.3301(5) 0.2620(9) 0.016(3) Uiso 1 1 d . . . C3 C 0.8722(11) 0.3627(5) 0.1832(9) 0.021(3) Uani 1 1 d . . . H23 H 0.8072 0.3639 0.1475 0.025 Uiso 1 1 calc R . . C4 C 0.9365(11) 0.3913(5) 0.1591(10) 0.024(3) Uiso 1 1 d . . . H24 H 0.9170 0.4119 0.1061 0.029 Uiso 1 1 calc R . . C5 C 1.0345(13) 0.3908(5) 0.2133(11) 0.038(5) Uani 1 1 d . . . H25 H 1.0793 0.4114 0.1959 0.046 Uiso 1 1 calc R . . C6 C 1.0661(10) 0.3599(5) 0.2929(9) 0.020(3) Uiso 1 1 d . . . C7 C 0.8222(9) 0.2964(5) 0.2883(8) 0.011(3) Uani 1 1 d . . . H21A H 0.8528 0.2638 0.3156 0.014 Uiso 1 1 calc R . . H21B H 0.8030 0.3152 0.3356 0.014 Uiso 1 1 calc R . . C8 C 0.7336(10) 0.2831(5) 0.2133(9) 0.019(3) Uani 1 1 d . . . C9 C 0.7371(10) 0.2516(5) 0.1402(9) 0.016(3) Uani 1 1 d . . . C10 C 0.6539(10) 0.2389(5) 0.0650(8) 0.019(3) Uani 1 1 d . . . C11 C 0.5661(10) 0.2604(6) 0.0714(10) 0.034(4) Uani 1 1 d . . . H16 H 0.5095 0.2541 0.0231 0.041 Uiso 1 1 calc R . . C12 C 0.5591(12) 0.2891(7) 0.1415(11) 0.045(5) Uani 1 1 d . . . H17 H 0.4980 0.2997 0.1435 0.054 Uiso 1 1 calc R . . C13 C 0.6405(10) 0.3035(6) 0.2116(10) 0.031(4) Uani 1 1 d . . . H18 H 0.6352 0.3263 0.2578 0.037 Uiso 1 1 calc R . . C14 C 0.6610(10) 0.2082(5) -0.0159(8) 0.023(4) Uani 1 1 d . . . H14A H 0.7253 0.2134 -0.0223 0.027 Uiso 1 1 calc R . . H14B H 0.6139 0.2220 -0.0712 0.027 Uiso 1 1 calc R . . C15 C 0.6432(10) 0.1488(5) -0.0097(8) 0.019(3) Uani 1 1 d . . . C16 C 0.7195(10) 0.1157(5) 0.0425(8) 0.020(3) Uani 1 1 d . . . C17 C 0.7031(10) 0.0618(5) 0.0497(9) 0.024(4) Uani 1 1 d . . . C18 C 0.6094(12) 0.0411(6) 0.0039(10) 0.037(4) Uani 1 1 d . . . H9 H 0.5968 0.0053 0.0082 0.045 Uiso 1 1 calc R . . C19 C 0.5376(12) 0.0741(7) -0.0467(11) 0.045(5) Uani 1 1 d . . . H10 H 0.4762 0.0606 -0.0769 0.054 Uiso 1 1 calc R . . C20 C 0.5551(11) 0.1263(6) -0.0532(10) 0.034(4) Uani 1 1 d . . . H11 H 0.5051 0.1476 -0.0886 0.041 Uiso 1 1 calc R . . C21 C 0.7837(10) 0.0262(5) 0.1012(9) 0.020(3) Uani 1 1 d . . . H7A H 0.8413 0.0355 0.0842 0.024 Uiso 1 1 calc R . . H7B H 0.7661 -0.0095 0.0797 0.024 Uiso 1 1 calc R . . C22 C 0.8119(9) 0.0259(4) 0.2077(9) 0.013(3) Uani 1 1 d . . . C23 C 0.8864(9) 0.0573(5) 0.2618(9) 0.014(3) Uiso 1 1 d . . . C24 C 0.9157(9) 0.0551(5) 0.3567(8) 0.013(3) Uani 1 1 d . . . C25 C 0.8678(10) 0.0191(5) 0.3978(9) 0.020(3) Uani 1 1 d . . . H3 H 0.8876 0.0157 0.4618 0.025 Uiso 1 1 calc R . . C26 C 0.7933(10) -0.0108(5) 0.3462(11) 0.025(4) Uani 1 1 d . . . H4 H 0.7611 -0.0337 0.3749 0.030 Uiso 1 1 calc R . . C27 C 0.7651(10) -0.0075(5) 0.2514(10) 0.021(3) Uani 1 1 d . . . H5 H 0.7137 -0.0281 0.2164 0.025 Uiso 1 1 calc R . . C28 C 0.9891(9) 0.0949(5) 0.4133(8) 0.015(3) Uani 1 1 d . . . H42A H 0.9650 0.1299 0.3929 0.018 Uiso 1 1 calc R . . H42B H 0.9904 0.0916 0.4773 0.018 Uiso 1 1 calc R . . C29 C 1.0929(9) 0.0913(5) 0.4104(8) 0.011(3) Uiso 1 1 d . . . C30 C 1.1534(9) 0.1345(5) 0.4404(8) 0.014(3) Uiso 1 1 d . . . C31 C 1.2480(10) 0.1355(5) 0.4358(9) 0.023(4) Uani 1 1 d . . . C32 C 1.2832(10) 0.0901(6) 0.4015(9) 0.024(4) Uani 1 1 d . . . H37 H 1.3462 0.0899 0.3970 0.029 Uiso 1 1 calc R . . C33 C 1.2245(12) 0.0464(6) 0.3747(9) 0.031(4) Uani 1 1 d . . . H38 H 1.2489 0.0163 0.3545 0.037 Uiso 1 1 calc R . . C34 C 1.1286(10) 0.0470(5) 0.3779(9) 0.018(3) Uiso 1 1 d . . . H39 H 1.0888 0.0178 0.3582 0.021 Uiso 1 1 calc R . . C35 C 1.3159(9) 0.1822(6) 0.4687(9) 0.025(4) Uani 1 1 d . . . H35A H 1.3824 0.1696 0.4835 0.030 Uiso 1 1 calc R . . H35B H 1.3068 0.1953 0.5255 0.030 Uiso 1 1 calc R . . C36 C 1.3038(10) 0.2289(5) 0.4012(9) 0.020(3) Uiso 1 1 d . . . C37 C 1.2403(10) 0.2695(5) 0.4031(9) 0.021(3) Uiso 1 1 d . . . C38 C 1.2356(11) 0.3137(6) 0.3466(10) 0.029(4) Uiso 1 1 d . . . C39 C 1.2916(11) 0.3163(6) 0.2909(10) 0.031(4) Uani 1 1 d . . . H30 H 1.2878 0.3459 0.2539 0.037 Uiso 1 1 calc R . . C40 C 1.3537(12) 0.2770(7) 0.2869(11) 0.042(5) Uani 1 1 d . . . H31 H 1.3916 0.2794 0.2473 0.051 Uiso 1 1 calc R . . C41 C 1.3599(11) 0.2320(6) 0.3440(10) 0.032(4) Uani 1 1 d . . . H32 H 1.4024 0.2047 0.3422 0.038 Uiso 1 1 calc R . . C42 C 1.1688(11) 0.3608(5) 0.3523(10) 0.032(4) Uani 1 1 d . . . H28A H 1.1686 0.3637 0.4160 0.038 Uiso 1 1 calc R . . H28B H 1.1985 0.3927 0.3381 0.038 Uiso 1 1 calc R . . C43 C 1.390(5) 0.147(3) 0.104(3) 0.45(7) Uani 1 1 d . . . H43A H 1.3256 0.1419 0.0631 0.676 Uiso 1 1 calc R . . H43B H 1.4367 0.1393 0.0721 0.676 Uiso 1 1 calc R . . H43C H 1.3982 0.1823 0.1263 0.676 Uiso 1 1 calc R . . C44 C 1.404(2) 0.1163(10) 0.170(2) 0.098(9) Uani 1 1 d . . . C45 C 1.483(6) 0.072(2) 0.179(3) 0.43(7) Uani 1 1 d . . . H45A H 1.4529 0.0383 0.1706 0.645 Uiso 1 1 calc R . . H45B H 1.5309 0.0745 0.2384 0.645 Uiso 1 1 calc R . . H45C H 1.5145 0.0778 0.1317 0.645 Uiso 1 1 calc R . . C46 C 1.0518(18) -0.0315(8) 0.1187(14) 0.077(7) Uani 1 1 d . . . H48A H 1.0400 -0.0636 0.0834 0.115 Uiso 1 1 calc R . . H48B H 1.0066 -0.0049 0.0865 0.115 Uiso 1 1 calc R . . H48C H 1.0433 -0.0377 0.1781 0.115 Uiso 1 1 calc R . . C47 C 1.1545(15) -0.0130(7) 0.1312(11) 0.047(5) Uani 1 1 d . . . C48 C 1.2305(16) -0.0534(8) 0.1532(14) 0.068(6) Uani 1 1 d . . . H46A H 1.2244 -0.0747 0.2034 0.102 Uiso 1 1 calc R . . H46B H 1.2933 -0.0368 0.1708 0.102 Uiso 1 1 calc R . . H46C H 1.2237 -0.0752 0.1000 0.102 Uiso 1 1 calc R . . C49 C 0.7306(12) 0.3488(6) -0.2022(12) 0.046(5) Uani 1 1 d . . . H49A H 0.7850 0.3356 -0.2196 0.069 Uiso 1 1 calc R . . H49B H 0.7236 0.3859 -0.2147 0.069 Uiso 1 1 calc R . . H49C H 0.6724 0.3309 -0.2371 0.069 Uiso 1 1 calc R . . C50 C 0.7477(13) 0.3394(6) -0.1009(11) 0.033(4) Uani 1 1 d . . . C51 C 0.6707(16) 0.3645(9) -0.0648(13) 0.079(7) Uani 1 1 d . . . H51A H 0.6776 0.3515 -0.0038 0.119 Uiso 1 1 calc R . . H51B H 0.6072 0.3557 -0.1051 0.119 Uiso 1 1 calc R . . H51C H 0.6788 0.4021 -0.0628 0.119 Uiso 1 1 calc R . . C52 C 0.5335(19) 0.9193(10) 0.2899(18) 0.070(7) Uiso 1 1 d . . . C53 C 0.521(3) 0.9456(14) 0.363(2) 0.131(11) Uiso 1 1 d . . . C54 C 0.444(3) 0.9251(15) 0.430(3) 0.074(14) Uiso 1 1 d . . . C55 C 0.5715(15) 0.9098(7) 0.3200(14) 0.040(5) Uiso 1 1 d . . . C56 C 0.448(3) 0.9373(17) 0.423(3) 0.083(16) Uiso 1 1 d . . . H1O H 0.904(11) 0.103(6) 0.198(10) 0.00(5) Uiso 1 1 d . . . H5O H 1.150(10) 0.271(6) 0.444(11) 0.00(5) Uiso 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 Cs1 0.0840(11) 0.0521(9) 0.0532(9) 0.0070(6) 0.0233(7) 0.0039(6) Cs2 0.0711(11) 0.0565(9) 0.0752(11) 0.0087(7) 0.0349(8) 0.0060(6) O1 0.036(7) 0.052(7) 0.023(6) 0.011(5) -0.001(5) -0.011(5) O2 0.027(6) 0.023(5) 0.016(5) -0.005(4) 0.002(4) -0.001(4) O3 0.034(7) 0.093(9) 0.014(5) 0.014(6) 0.009(5) -0.007(6) O4 0.022(5) 0.017(5) 0.010(5) -0.004(4) 0.011(4) -0.008(4) O5 0.011(5) 0.018(5) 0.009(5) -0.001(4) 0.001(4) 0.002(4) O6 0.016(5) 0.010(4) 0.018(5) -0.006(4) 0.000(4) -0.008(4) O7 0.010(7) 0.032(7) 0.012(6) 0.017(5) -0.010(5) 0.002(5) O8 0.019(5) 0.023(5) 0.016(5) -0.007(4) 0.008(4) -0.001(4) O9 0.009(7) 0.032(7) 0.023(7) 0.000(5) -0.004(6) -0.002(6) O10 0.040(7) 0.045(7) 0.047(7) 0.023(6) 0.012(6) 0.017(6) O11 0.131(14) 0.029(8) 0.089(11) -0.001(7) 0.056(10) 0.007(8) O12 0.53(6) 0.110(18) 0.18(3) 0.010(17) 0.27(4) 0.08(2) C3 0.035(9) 0.013(7) 0.015(7) -0.006(6) 0.006(7) 0.003(6) C5 0.078(14) 0.006(7) 0.056(11) -0.010(7) 0.057(10) -0.010(7) C7 0.012(8) 0.018(7) 0.003(7) -0.001(6) 0.001(6) 0.006(6) C8 0.028(9) 0.016(7) 0.017(8) 0.006(6) 0.013(7) 0.011(6) C9 0.022(9) 0.013(7) 0.014(8) 0.011(6) 0.007(6) 0.004(6) C10 0.020(9) 0.026(8) 0.006(7) 0.009(6) -0.002(6) 0.006(6) C11 0.015(9) 0.060(11) 0.017(9) 0.011(8) -0.011(7) 0.013(8) C12 0.020(10) 0.080(13) 0.032(10) 0.009(10) 0.005(8) 0.040(9) C13 0.025(10) 0.045(10) 0.024(9) -0.001(7) 0.009(8) 0.007(7) C14 0.024(9) 0.032(8) 0.000(7) 0.009(6) -0.014(6) 0.006(7) C15 0.026(9) 0.028(8) 0.000(6) -0.005(6) -0.001(6) -0.012(7) C16 0.023(9) 0.032(9) 0.004(7) -0.002(6) 0.005(6) 0.002(7) C17 0.027(9) 0.032(9) 0.010(7) -0.005(7) 0.002(7) -0.011(7) C18 0.042(11) 0.039(10) 0.026(9) -0.011(8) 0.004(8) -0.022(8) C19 0.029(10) 0.062(13) 0.030(10) -0.006(9) -0.011(8) -0.027(9) C20 0.025(10) 0.048(11) 0.021(9) 0.005(8) -0.006(7) 0.003(8) C21 0.027(9) 0.009(7) 0.025(8) -0.005(6) 0.010(7) -0.013(6) C22 0.017(8) 0.002(6) 0.021(8) 0.002(6) 0.007(6) 0.004(6) C24 0.016(8) 0.008(7) 0.019(8) 0.000(6) 0.008(6) 0.003(6) C25 0.031(9) 0.018(7) 0.015(8) 0.008(6) 0.011(7) 0.005(7) C26 0.031(9) 0.006(7) 0.046(11) 0.002(7) 0.025(8) -0.011(6) C27 0.019(8) 0.002(7) 0.044(10) 0.002(6) 0.013(7) 0.005(6) C28 0.026(8) 0.010(7) 0.011(7) 0.002(6) 0.008(6) 0.000(6) C31 0.034(9) 0.021(8) 0.008(7) 0.003(6) -0.003(7) 0.008(7) C32 0.011(8) 0.042(10) 0.017(8) 0.010(7) 0.001(6) 0.011(7) C33 0.050(11) 0.027(9) 0.013(8) 0.007(7) 0.005(7) 0.020(8) C35 0.000(7) 0.045(9) 0.021(8) -0.024(7) -0.010(6) -0.010(6) C39 0.025(9) 0.041(10) 0.029(9) -0.009(7) 0.012(7) -0.017(8) C40 0.026(10) 0.070(13) 0.033(10) -0.017(9) 0.011(8) -0.034(10) C41 0.019(9) 0.045(10) 0.028(9) -0.026(8) 0.001(7) -0.014(7) C42 0.058(11) 0.011(7) 0.038(9) -0.009(7) 0.032(8) -0.023(7) C43 0.45(10) 0.76(15) 0.24(5) 0.29(8) 0.26(6) 0.56(11) C44 0.18(3) 0.065(16) 0.079(19) -0.014(14) 0.08(2) 0.007(17) C45 0.66(13) 0.25(6) 0.17(4) -0.13(4) -0.19(6) 0.30(8) C46 0.11(2) 0.070(15) 0.054(13) 0.034(11) 0.030(13) 0.012(13) C47 0.100(17) 0.034(11) 0.022(9) 0.002(8) 0.041(10) 0.002(11) C48 0.084(16) 0.067(14) 0.068(14) 0.001(11) 0.046(12) 0.011(12) C49 0.033(10) 0.035(10) 0.070(14) -0.006(9) 0.014(9) 0.003(8) C50 0.045(11) 0.028(9) 0.034(10) -0.008(8) 0.024(9) -0.023(8) C51 0.088(17) 0.118(19) 0.038(12) 0.043(12) 0.029(12) 0.048(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 Cs1 O3 2.850(10) . ? Cs1 O1 2.853(10) . ? Cs1 O2 2.888(9) . ? Cs1 O11 2.907(12) . ? Cs1 O7 2.975(12) . ? Cs1 C33 3.301(13) . ? Cs1 C32 3.338(12) . ? Cs1 C34 3.350(13) . ? Cs1 C29 3.464(12) . ? Cs1 C31 3.473(12) . ? Cs1 C30 3.534(13) . ? Cs1 O12 3.63(4) . ? Cs2 O10 2.863(11) . ? Cs2 O1 2.967(11) . ? Cs2 O5 3.000(8) . ? Cs2 O3 3.064(13) . ? Cs2 O8 3.071(9) 4_565 ? Cs2 O2 3.093(9) . ? Cs2 C4 3.306(14) . ? Cs2 C3 3.387(13) . ? Cs2 C5 3.474(14) . ? Cs2 O4 3.590(8) 4_565 ? Cs2 C2 3.617(13) . ? Cs2 C6 3.728(13) . ? Cl1 C53 1.66(7) . ? Cl1 Cl2 1.66(7) . ? Cl1 C56 1.72(8) . ? Cl1 Cl1 2.17(14) 3_676 ? Cl1 C54 2.03(8) . ? Cl2 C53 1.87(4) . ? O4 C1 1.360(15) . ? O4 Cs2 3.590(8) 4_566 ? O5 C9 1.369(15) . ? O6 C16 1.358(16) . ? O7 C23 1.374(17) . ? O8 C30 1.353(15) . ? O8 Cs2 3.071(8) 4_566 ? O9 C37 1.323(19) . ? O10 C50 1.183(18) . ? O11 C47 1.19(2) . ? O12 C44 1.09(3) . ? C1 C2 1.343(17) . ? C1 C6 1.420(19) . ? C2 C3 1.408(18) . ? C2 C7 1.551(18) . ? C3 C4 1.31(2) . ? C4 C5 1.40(2) . ? C5 C6 1.39(2) . ? C6 C42 1.48(2) . ? C7 C8 1.469(18) . ? C8 C9 1.382(18) . ? C8 C13 1.43(2) . ? C9 C10 1.419(18) . ? C10 C11 1.41(2) . ? C10 C14 1.485(19) . ? C11 C12 1.32(2) . ? C12 C13 1.37(2) . ? C14 C15 1.535(19) . ? C15 C20 1.37(2) . ? C15 C16 1.418(19) . ? C16 C17 1.396(19) . ? C17 C18 1.42(2) . ? C17 C21 1.491(19) . ? C18 C19 1.37(2) . ? C19 C20 1.36(2) . ? C21 C22 1.544(18) . ? C22 C27 1.373(18) . ? C22 C23 1.388(18) . ? C23 C24 1.374(17) . ? C24 C25 1.401(18) . ? C24 C28 1.523(17) . ? C25 C26 1.354(19) . ? C26 C27 1.375(19) . ? C28 C29 1.514(18) . ? C29 C34 1.388(18) . ? C29 C30 1.386(17) . ? C30 C31 1.387(19) . ? C31 C32 1.42(2) . ? C31 C35 1.520(19) . ? C32 C33 1.38(2) . ? C33 C34 1.40(2) . ? C35 C36 1.541(19) . ? C36 C41 1.36(2) . ? C36 C37 1.382(19) . ? C37 C38 1.402(19) . ? C38 C39 1.34(2) . ? C38 C42 1.55(2) . ? C39 C40 1.35(2) . ? C40 C41 1.42(2) . ? C43 C44 1.23(5) . ? C44 C45 1.58(5) . ? C46 C47 1.51(3) . ? C47 C48 1.46(3) . ? C49 C50 1.50(2) . ? C50 C51 1.52(3) . ? C52 C55 0.64(3) . ? C52 C53 1.36(4) . ? C53 C55 1.44(4) . ? C53 C56 1.61(5) . ? C53 C54 1.80(5) . ? 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 O3 Cs1 O1 71.9(3) . . ? O3 Cs1 O2 73.8(3) . . ? O1 Cs1 O2 72.9(3) . . ? O3 Cs1 O11 95.2(4) . . ? O1 Cs1 O11 115.3(4) . . ? O2 Cs1 O11 164.0(4) . . ? O3 Cs1 O7 71.1(3) . . ? O1 Cs1 O7 131.0(3) . . ? O2 Cs1 O7 66.8(3) . . ? O11 Cs1 O7 99.0(4) . . ? O3 Cs1 C33 152.5(4) . . ? O1 Cs1 C33 135.6(3) . . ? O2 Cs1 C33 110.6(3) . . ? O11 Cs1 C33 73.9(4) . . ? O7 Cs1 C33 85.4(4) . . ? O3 Cs1 C32 172.9(3) . . ? O1 Cs1 C32 112.2(3) . . ? O2 Cs1 C32 101.6(3) . . ? O11 Cs1 C32 88.2(4) . . ? O7 Cs1 C32 102.2(3) . . ? C33 Cs1 C32 24.0(4) . . ? O3 Cs1 C34 131.9(3) . . ? O1 Cs1 C34 150.1(3) . . ? O2 Cs1 C34 94.8(3) . . ? O11 Cs1 C34 83.9(4) . . ? O7 Cs1 C34 61.7(3) . . ? C33 Cs1 C34 24.3(4) . . ? C32 Cs1 C34 42.2(3) . . ? O3 Cs1 C29 124.6(3) . . ? O1 Cs1 C29 132.9(3) . . ? O2 Cs1 C29 71.7(3) . . ? O11 Cs1 C29 107.1(3) . . ? O7 Cs1 C29 55.9(3) . . ? C33 Cs1 C29 41.7(3) . . ? C32 Cs1 C29 48.3(3) . . ? C34 Cs1 C29 23.4(3) . . ? O3 Cs1 C31 151.6(3) . . ? O1 Cs1 C31 101.7(3) . . ? O2 Cs1 C31 77.9(3) . . ? O11 Cs1 C31 112.1(4) . . ? O7 Cs1 C31 95.9(3) . . ? C33 Cs1 C31 41.9(3) . . ? C32 Cs1 C31 23.9(3) . . ? C34 Cs1 C31 48.4(3) . . ? C29 Cs1 C31 40.9(3) . . ? O3 Cs1 C30 132.7(3) . . ? O1 Cs1 C30 111.3(3) . . ? O2 Cs1 C30 63.5(3) . . ? O11 Cs1 C30 121.2(3) . . ? O7 Cs1 C30 74.0(3) . . ? C33 Cs1 C30 47.6(3) . . ? C32 Cs1 C30 40.9(3) . . ? C34 Cs1 C30 40.6(3) . . ? C29 Cs1 C30 22.8(3) . . ? C31 Cs1 C30 22.8(3) . . ? O3 Cs1 O12 129.0(5) . . ? O1 Cs1 O12 72.6(4) . . ? O2 Cs1 O12 126.9(4) . . ? O11 Cs1 O12 69.0(5) . . ? O7 Cs1 O12 156.0(5) . . ? C33 Cs1 O12 71.4(5) . . ? C32 Cs1 O12 58.0(5) . . ? C34 Cs1 O12 95.6(5) . . ? C29 Cs1 O12 106.4(5) . . ? C31 Cs1 O12 71.2(5) . . ? C30 Cs1 O12 94.0(5) . . ? O10 Cs2 O1 151.8(3) . . ? O10 Cs2 O5 77.9(3) . . ? O1 Cs2 O5 119.3(2) . . ? O10 Cs2 O3 102.3(3) . . ? O1 Cs2 O3 67.4(3) . . ? O5 Cs2 O3 70.1(2) . . ? O10 Cs2 O8 90.2(3) . 4_565 ? O1 Cs2 O8 69.6(2) . 4_565 ? O5 Cs2 O8 166.7(2) . 4_565 ? O3 Cs2 O8 107.6(3) . 4_565 ? O10 Cs2 O2 134.0(3) . . ? O1 Cs2 O2 68.5(3) . . ? O5 Cs2 O2 56.4(2) . . ? O3 Cs2 O2 68.0(2) . . ? O8 Cs2 O2 135.8(2) 4_565 . ? O10 Cs2 C4 73.2(3) . . ? O1 Cs2 C4 126.3(3) . . ? O5 Cs2 C4 87.4(3) . . ? O3 Cs2 C4 157.4(3) . . ? O8 Cs2 C4 94.7(3) 4_565 . ? O2 Cs2 C4 98.8(3) . . ? O10 Cs2 C3 70.7(3) . . ? O1 Cs2 C3 135.7(3) . . ? O5 Cs2 C3 64.8(3) . . ? O3 Cs2 C3 134.9(3) . . ? O8 Cs2 C3 116.8(3) 4_565 . ? O2 Cs2 C3 85.1(3) . . ? C4 Cs2 C3 22.6(3) . . ? O10 Cs2 C5 95.3(4) . . ? O1 Cs2 C5 102.6(4) . . ? O5 Cs2 C5 100.3(3) . . ? O3 Cs2 C5 157.3(3) . . ? O8 Cs2 C5 86.3(3) 4_565 . ? O2 Cs2 C5 89.4(3) . . ? C4 Cs2 C5 23.7(4) . . ? C3 Cs2 C5 40.1(4) . . ? O10 Cs2 O4 84.8(3) . 4_565 ? O1 Cs2 O4 68.7(2) . 4_565 ? O5 Cs2 O4 109.5(2) . 4_565 ? O3 Cs2 O4 48.1(2) . 4_565 ? O8 Cs2 O4 63.1(2) 4_565 4_565 ? O2 Cs2 O4 112.3(2) . 4_565 ? C4 Cs2 O4 148.9(3) . 4_565 ? C3 Cs2 O4 155.4(3) . 4_565 ? C5 Cs2 O4 149.4(3) . 4_565 ? O10 Cs2 C2 89.6(3) . . ? O1 Cs2 C2 118.5(3) . . ? O5 Cs2 C2 54.9(2) . . ? O3 Cs2 C2 119.7(3) . . ? O8 Cs2 C2 131.6(3) 4_565 . ? O2 Cs2 C2 62.3(3) . . ? C4 Cs2 C2 39.8(3) . . ? C3 Cs2 C2 22.9(3) . . ? C5 Cs2 C2 45.6(3) . . ? O4 Cs2 C2 164.4(2) 4_565 . ? O10 Cs2 C6 112.8(3) . . ? O1 Cs2 C6 90.5(3) . . ? O5 Cs2 C6 90.7(3) . . ? O3 Cs2 C6 135.4(3) . . ? O8 Cs2 C6 99.3(3) 4_565 . ? O2 Cs2 C6 67.8(3) . . ? C4 Cs2 C6 40.0(3) . . ? C3 Cs2 C6 45.8(3) . . ? C5 Cs2 C6 22.0(3) . . ? O4 Cs2 C6 156.0(3) 4_565 . ? C2 Cs2 C6 38.5(3) . . ? C53 Cl1 Cl2 68(3) . . ? C53 Cl1 C56 57(3) . . ? Cl2 Cl1 C56 103(4) . . ? C53 Cl1 Cl1 140(7) . 3_676 ? Cl2 Cl1 Cl1 142(6) . 3_676 ? C56 Cl1 Cl1 86(5) . 3_676 ? C53 Cl1 C54 57(3) . . ? Cl2 Cl1 C54 107(4) . . ? C56 Cl1 C54 4(2) . . ? Cl1 Cl1 C54 85(4) 3_676 . ? Cl1 Cl2 C53 56(3) . . ? Cs1 O1 Cs2 98.4(3) . . ? Cs1 O2 Cs2 94.8(3) . . ? Cs1 O3 Cs2 96.3(3) . . ? C1 O4 Cs2 158.8(7) . 4_566 ? C9 O5 Cs2 129.7(7) . . ? C23 O7 Cs1 147.8(9) . . ? C30 O8 Cs2 151.5(7) . 4_566 ? C50 O10 Cs2 170.2(11) . . ? C47 O11 Cs1 128.5(12) . . ? C44 O12 Cs1 115(3) . . ? C2 C1 O4 118.3(11) . . ? C2 C1 C6 122.4(12) . . ? O4 C1 C6 119.2(11) . . ? C2 C1 Cs2 72.9(7) . . ? O4 C1 Cs2 123.8(7) . . ? C6 C1 Cs2 77.3(7) . . ? C1 C2 C3 118.9(12) . . ? C1 C2 C7 120.9(11) . . ? C3 C2 C7 120.2(11) . . ? C1 C2 Cs2 86.3(8) . . ? C3 C2 Cs2 69.3(7) . . ? C7 C2 Cs2 115.6(7) . . ? C4 C3 C2 121.4(13) . . ? C4 C3 Cs2 75.3(8) . . ? C2 C3 Cs2 87.8(8) . . ? C3 C4 C5 120.0(14) . . ? C3 C4 Cs2 82.1(8) . . ? C5 C4 Cs2 84.9(8) . . ? C6 C5 C4 121.3(14) . . ? C6 C5 Cs2 89.3(8) . . ? C4 C5 Cs2 71.4(8) . . ? C5 C6 C1 115.8(12) . . ? C5 C6 C42 121.5(13) . . ? C1 C6 C42 122.6(12) . . ? C5 C6 Cs2 68.7(8) . . ? C1 C6 Cs2 80.9(7) . . ? C42 C6 Cs2 121.5(8) . . ? C8 C7 C2 116.8(10) . . ? C9 C8 C13 117.3(12) . . ? C9 C8 C7 121.3(12) . . ? C13 C8 C7 121.4(12) . . ? O5 C9 C8 117.4(11) . . ? O5 C9 C10 119.2(11) . . ? C8 C9 C10 123.3(12) . . ? C11 C10 C9 114.5(13) . . ? C11 C10 C14 123.4(12) . . ? C9 C10 C14 122.0(12) . . ? C12 C11 C10 124.1(13) . . ? C11 C12 C13 121.1(14) . . ? C12 C13 C8 119.5(14) . . ? C10 C14 C15 114.1(11) . . ? C20 C15 C16 118.1(13) . . ? C20 C15 C14 121.9(12) . . ? C16 C15 C14 120.0(12) . . ? O6 C16 C17 120.9(12) . . ? O6 C16 C15 118.9(12) . . ? C17 C16 C15 120.2(13) . . ? C16 C17 C18 118.8(13) . . ? C16 C17 C21 120.7(12) . . ? C18 C17 C21 120.4(13) . . ? C19 C18 C17 119.4(14) . . ? C20 C19 C18 120.8(14) . . ? C19 C20 C15 122.6(14) . . ? C17 C21 C22 117.9(11) . . ? C27 C22 C23 118.2(12) . . ? C27 C22 C21 119.9(11) . . ? C23 C22 C21 121.9(11) . . ? O7 C23 C24 115.9(11) . . ? O7 C23 C22 121.8(11) . . ? C24 C23 C22 122.3(12) . . ? C23 C24 C25 117.3(12) . . ? C23 C24 C28 120.3(11) . . ? C25 C24 C28 122.1(11) . . ? C26 C25 C24 121.3(12) . . ? C25 C26 C27 120.1(12) . . ? C26 C27 C22 120.8(12) . . ? C29 C28 C24 117.8(10) . . ? C34 C29 C30 119.4(12) . . ? C34 C29 C28 122.4(11) . . ? C30 C29 C28 118.1(11) . . ? C34 C29 Cs1 73.7(7) . . ? C30 C29 Cs1 81.5(7) . . ? C28 C29 Cs1 114.7(7) . . ? O8 C30 C31 120.9(11) . . ? O8 C30 C29 117.3(11) . . ? C31 C30 C29 121.8(12) . . ? O8 C30 Cs1 119.3(7) . . ? C31 C30 Cs1 76.1(7) . . ? C29 C30 Cs1 75.7(7) . . ? C30 C31 C32 118.1(12) . . ? C30 C31 C35 122.8(12) . . ? C32 C31 C35 119.1(13) . . ? C30 C31 Cs1 81.1(7) . . ? C32 C31 Cs1 72.7(7) . . ? C35 C31 Cs1 117.6(8) . . ? C33 C32 C31 120.3(14) . . ? C33 C32 Cs1 76.5(7) . . ? C31 C32 Cs1 83.4(7) . . ? C32 C33 C34 120.3(13) . . ? C32 C33 Cs1 79.5(8) . . ? C34 C33 Cs1 79.8(7) . . ? C29 C34 C33 120.0(12) . . ? C29 C34 Cs1 82.9(7) . . ? C33 C34 Cs1 75.9(7) . . ? C31 C35 C36 116.7(10) . . ? C41 C36 C37 119.8(13) . . ? C41 C36 C35 120.1(13) . . ? C37 C36 C35 120.0(12) . . ? O9 C37 C36 119.9(13) . . ? O9 C37 C38 120.6(12) . . ? C36 C37 C38 119.5(13) . . ? C39 C38 C37 120.0(14) . . ? C39 C38 C42 120.2(13) . . ? C37 C38 C42 119.8(13) . . ? C38 C39 C40 121.8(16) . . ? C39 C40 C41 119.0(15) . . ? C36 C41 C40 119.9(15) . . ? C6 C42 C38 118.5(11) . . ? O12 C44 C43 130(4) . . ? O12 C44 C45 112(4) . . ? C43 C44 C45 116(4) . . ? O11 C47 C48 121(2) . . ? O11 C47 C46 122.7(19) . . ? C48 C47 C46 116.6(17) . . ? O11 C47 Cs1 37.1(9) . . ? C48 C47 Cs1 137.6(14) . . ? C46 C47 Cs1 97.8(12) . . ? O10 C50 C49 122.5(15) . . ? O10 C50 C51 124.2(15) . . ? C49 C50 C51 113.2(15) . . ? C55 C52 C53 84(4) . . ? C52 C53 C55 26.4(13) . . ? C52 C53 C56 133(3) . . ? C55 C53 C56 133(3) . . ? C52 C53 Cl1 162(4) . . ? C55 C53 Cl1 153(4) . . ? C56 C53 Cl1 64(3) . . ? C52 C53 C54 125(3) . . ? C55 C53 C54 124(3) . . ? C56 C53 C54 9(2) . . ? Cl1 C53 C54 72(3) . . ? C52 C53 Cl2 108(2) . . ? C55 C53 Cl2 124(2) . . ? C56 C53 Cl2 100(2) . . ? Cl1 C53 Cl2 56(3) . . ? C54 C53 Cl2 109(2) . . ? C53 C54 Cl1 51(2) . . ? C52 C55 C53 69(3) . . ? C53 C56 Cl1 60(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.561 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.246 #===END data_36 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H72 K1 O12 Rb1' _chemical_formula_weight 1073.72 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.5123(8) _cell_length_b 24.7889(13) _cell_length_c 14.8909(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.9540(10) _cell_angle_gamma 90.00 _cell_volume 5096.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(0.1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.118 _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 100.0(0.1) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32715 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.31 _reflns_number_total 11905 _reflns_number_gt 8901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0934P)^2^+13.5677P] 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 11905 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.49145(3) 0.222388(14) 0.08478(3) 0.02814(11) Uani 1 1 d . . . K1 K 0.60422(5) 0.37219(3) 0.20275(5) 0.01868(15) Uani 1 1 d . . . O1 O 0.52600(19) 0.19777(10) 0.40164(17) 0.0198(5) Uani 1 1 d . . . O2 O 0.69389(17) 0.23141(9) 0.46856(16) 0.0201(5) Uani 1 1 d . . . O3 O 0.61917(19) 0.32404(11) 0.47917(18) 0.0223(5) Uani 1 1 d . . . O4 O 0.42718(18) 0.40812(10) 0.21660(18) 0.0203(5) Uani 1 1 d . . . O5 O 0.30262(15) 0.36118(9) 0.08034(15) 0.0177(5) Uani 1 1 d . . . O6 O 0.32740(17) 0.26666(10) 0.14617(17) 0.0185(5) Uani 1 1 d . . . O7 O 0.5179(2) 0.28781(11) 0.2628(2) 0.0237(6) Uani 1 1 d . . . O8 O 0.6771(2) 0.28474(12) 0.1425(2) 0.0323(6) Uani 1 1 d . . . O9 O 0.4688(2) 0.34117(16) 0.0462(2) 0.0411(8) Uani 1 1 d . . . O10 O 0.3204(2) 0.18096(12) -0.0507(2) 0.0382(7) Uani 1 1 d . . . O11 O 0.6620(3) 0.45987(12) 0.1176(2) 0.0490(8) Uani 1 1 d . . . C1 C 0.5029(2) 0.16688(13) 0.3226(2) 0.0175(6) Uani 1 1 d . . . C2 C 0.4051(2) 0.16597(13) 0.2685(2) 0.0170(6) Uani 1 1 d . . . C3 C 0.3776(3) 0.13351(13) 0.1885(2) 0.0209(7) Uani 1 1 d . . . H3A H 0.3072 0.1260 0.1577 0.025 Uiso 1 1 calc R . . C4 C 0.4456(3) 0.10311(13) 0.1620(2) 0.0233(7) Uani 1 1 d . . . H4A H 0.4227 0.0730 0.1158 0.028 Uiso 1 1 calc R . . C5 C 0.5426(3) 0.10496(14) 0.2161(2) 0.0238(7) Uani 1 1 d . . . H5A H 0.5888 0.0784 0.2033 0.029 Uiso 1 1 calc R . . C6 C 0.5728(3) 0.13665(13) 0.2970(2) 0.0212(7) Uani 1 1 d . . . C7 C 0.6785(2) 0.13527(14) 0.3601(3) 0.0229(7) Uani 1 1 d . . . H7A H 0.6791 0.1327 0.4266 0.028 Uiso 1 1 calc R . . H7B H 0.7089 0.1020 0.3454 0.028 Uiso 1 1 calc R . . C8 C 0.7402(2) 0.18262(14) 0.3516(2) 0.0212(7) Uani 1 1 d . . . C9 C 0.7463(2) 0.22871(14) 0.4089(2) 0.0201(7) Uani 1 1 d . . . C10 C 0.8083(2) 0.27166(14) 0.4041(2) 0.0215(7) Uani 1 1 d . . . C11 C 0.8628(2) 0.26819(15) 0.3421(3) 0.0238(7) Uani 1 1 d . . . H11A H 0.9049 0.2969 0.3390 0.029 Uiso 1 1 calc R . . C12 C 0.8564(3) 0.22287(16) 0.2842(3) 0.0280(8) Uani 1 1 d . . . H12A H 0.8934 0.2211 0.2416 0.034 Uiso 1 1 calc R . . C13 C 0.7956(3) 0.18085(15) 0.2896(2) 0.0255(7) Uani 1 1 d . . . H13A H 0.7914 0.1501 0.2504 0.031 Uiso 1 1 calc R . . C14 C 0.8183(2) 0.32010(14) 0.4692(3) 0.0241(7) Uani 1 1 d . . . H14A H 0.8104 0.3075 0.5295 0.029 Uiso 1 1 calc R . . H14B H 0.8850 0.3344 0.4833 0.029 Uiso 1 1 calc R . . C15 C 0.7479(2) 0.36623(13) 0.4325(2) 0.0204(7) Uani 1 1 d . . . C16 C 0.6537(2) 0.36603(13) 0.4399(2) 0.0177(6) Uani 1 1 d . . . C17 C 0.5900(2) 0.40937(13) 0.4068(2) 0.0169(6) Uani 1 1 d . . . C18 C 0.6233(2) 0.45410(13) 0.3696(2) 0.0193(6) Uani 1 1 d . . . H18A H 0.5833 0.4878 0.3572 0.023 Uiso 1 1 calc R . . C19 C 0.7166(3) 0.45577(14) 0.3638(3) 0.0237(7) Uani 1 1 d . . . H19A H 0.7426 0.4901 0.3460 0.028 Uiso 1 1 calc R . . C20 C 0.7775(3) 0.41204(15) 0.3942(3) 0.0254(7) Uani 1 1 d . . . H20A H 0.8457 0.4142 0.3923 0.031 Uiso 1 1 calc R . . C21 C 0.4883(2) 0.40511(13) 0.4136(2) 0.0189(6) Uani 1 1 d . . . H21A H 0.4643 0.3683 0.3935 0.023 Uiso 1 1 calc R . . H21B H 0.4926 0.4087 0.4810 0.023 Uiso 1 1 calc R . . C22 C 0.4132(2) 0.44443(13) 0.3585(2) 0.0174(6) Uani 1 1 d . . . C23 C 0.3807(2) 0.44250(12) 0.2595(2) 0.0174(6) Uani 1 1 d . . . C24 C 0.3025(2) 0.47414(12) 0.2064(2) 0.0180(6) Uani 1 1 d . . . C25 C 0.2558(2) 0.50713(13) 0.2546(2) 0.0213(7) Uani 1 1 d . . . H25A H 0.2012 0.5278 0.2199 0.026 Uiso 1 1 calc R . . C26 C 0.2876(2) 0.51036(13) 0.3526(3) 0.0222(7) Uani 1 1 d . . . H26A H 0.2557 0.5333 0.3846 0.027 Uiso 1 1 calc R . . C27 C 0.3666(2) 0.47968(13) 0.4032(2) 0.0198(6) Uani 1 1 d . . . H27A H 0.3895 0.4828 0.4701 0.024 Uiso 1 1 calc R . . C28 C 0.2718(2) 0.47420(13) 0.0991(2) 0.0213(7) Uani 1 1 d . . . H28A H 0.2503 0.5111 0.0770 0.026 Uiso 1 1 calc R . . H28B H 0.3296 0.4661 0.0794 0.026 Uiso 1 1 calc R . . C29 C 0.1921(2) 0.43519(14) 0.0490(2) 0.0202(7) Uani 1 1 d . . . C30 C 0.2123(2) 0.38008(13) 0.0411(2) 0.0186(6) Uani 1 1 d . . . C31 C 0.1378(2) 0.34511(13) -0.0102(2) 0.0191(6) Uani 1 1 d . . . C32 C 0.0459(3) 0.36523(16) -0.0541(3) 0.0278(8) Uani 1 1 d . . . H32A H -0.0038 0.3416 -0.0890 0.033 Uiso 1 1 calc R . . C33 C 0.0258(3) 0.41915(17) -0.0479(3) 0.0340(9) Uani 1 1 d . . . H33A H -0.0372 0.4327 -0.0788 0.041 Uiso 1 1 calc R . . C34 C 0.0981(3) 0.45353(16) 0.0038(3) 0.0315(9) Uani 1 1 d . . . H34A H 0.0834 0.4906 0.0086 0.038 Uiso 1 1 calc R . . C35 C 0.1584(3) 0.28548(13) -0.0168(2) 0.0207(7) Uani 1 1 d . . . H35A H 0.2228 0.2814 -0.0259 0.025 Uiso 1 1 calc R . . H35B H 0.1097 0.2703 -0.0732 0.025 Uiso 1 1 calc R . . C36 C 0.1568(2) 0.25298(13) 0.0690(2) 0.0200(7) Uani 1 1 d . . . C37 C 0.2410(2) 0.24394(13) 0.1442(2) 0.0174(6) Uani 1 1 d . . . C38 C 0.2396(2) 0.21083(13) 0.2203(2) 0.0195(6) Uani 1 1 d . . . C39 C 0.1519(3) 0.18864(15) 0.2215(3) 0.0250(7) Uani 1 1 d . . . H39A H 0.1499 0.1662 0.2725 0.030 Uiso 1 1 calc R . . C40 C 0.0673(3) 0.19908(17) 0.1487(3) 0.0304(8) Uani 1 1 d . . . H40A H 0.0074 0.1844 0.1506 0.036 Uiso 1 1 calc R . . C41 C 0.0703(3) 0.23061(16) 0.0739(3) 0.0270(8) Uani 1 1 d . . . H41A H 0.0122 0.2374 0.0243 0.032 Uiso 1 1 calc R . . C42 C 0.3326(2) 0.19978(13) 0.2983(2) 0.0170(6) Uani 1 1 d . . . H42A H 0.3168 0.1811 0.3504 0.020 Uiso 1 1 calc R . . H42B H 0.3632 0.2347 0.3231 0.020 Uiso 1 1 calc R . . C43 C 0.2497(3) 0.15688(15) -0.0980(3) 0.0270(8) Uani 1 1 d . . . C44 C 0.1829(3) 0.1288(2) -0.0544(3) 0.0396(10) Uani 1 1 d . . . H44A H 0.2062 0.1337 0.0142 0.059 Uiso 1 1 calc R . . H44B H 0.1810 0.0902 -0.0693 0.059 Uiso 1 1 calc R . . H44C H 0.1177 0.1440 -0.0796 0.059 Uiso 1 1 calc R . . C45 C 0.2243(3) 0.15332(16) -0.2030(3) 0.0318(8) Uani 1 1 d . . . H45A H 0.2724 0.1731 -0.2240 0.048 Uiso 1 1 calc R . . H45B H 0.1600 0.1691 -0.2321 0.048 Uiso 1 1 calc R . . H45C H 0.2237 0.1154 -0.2219 0.048 Uiso 1 1 calc R . . C46 C 0.6425(4) 0.50707(17) 0.1250(3) 0.0386(10) Uani 1 1 d . . . C47 C 0.7172(4) 0.55008(18) 0.1411(4) 0.0453(11) Uani 1 1 d . . . H47A H 0.7796 0.5340 0.1437 0.068 Uiso 1 1 calc R . . H47B H 0.7231 0.5684 0.2010 0.068 Uiso 1 1 calc R . . H47C H 0.6982 0.5763 0.0894 0.068 Uiso 1 1 calc R . . C48 C 0.5433(4) 0.5241(2) 0.1190(3) 0.0454(11) Uani 1 1 d . . . H48A H 0.5009 0.4925 0.1086 0.068 Uiso 1 1 calc R . . H48B H 0.5191 0.5494 0.0663 0.068 Uiso 1 1 calc R . . H48C H 0.5440 0.5418 0.1780 0.068 Uiso 1 1 calc R . . H1O H 0.577(3) 0.2032(16) 0.422(3) 0.015(10) Uiso 1 1 d . . . H3O H 0.648(3) 0.3030(18) 0.480(3) 0.019(12) Uiso 1 1 d . . . H4O H 0.392(3) 0.3963(16) 0.181(3) 0.014(11) Uiso 1 1 d . . . H6O H 0.317(3) 0.2919(17) 0.126(3) 0.016(11) Uiso 1 1 d . . . H7C H 0.531(4) 0.2799(19) 0.309(4) 0.031(14) Uiso 1 1 d . . . H7D H 0.467(4) 0.288(2) 0.245(4) 0.037(15) Uiso 1 1 d . . . H8D H 0.721(4) 0.271(2) 0.179(4) 0.049(16) Uiso 1 1 d . . . H8C H 0.693(3) 0.2801(17) 0.089(3) 0.032(12) Uiso 1 1 d . . . H9D H 0.423(4) 0.349(2) 0.037(4) 0.06(2) Uiso 1 1 d . . . H9C H 0.480(4) 0.337(2) -0.002(4) 0.047(15) Uiso 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 Rb1 0.0297(2) 0.02362(18) 0.0333(2) -0.00402(14) 0.01293(15) -0.00279(14) K1 0.0296(4) 0.0131(3) 0.0137(3) -0.0027(2) 0.0071(3) -0.0003(3) O1 0.0168(13) 0.0238(12) 0.0171(11) -0.0004(9) 0.0027(10) 0.0006(10) O2 0.0210(12) 0.0215(12) 0.0179(11) 0.0018(9) 0.0060(9) 0.0024(9) O3 0.0229(13) 0.0180(12) 0.0268(13) 0.0049(10) 0.0088(10) 0.0051(11) O4 0.0181(12) 0.0231(12) 0.0172(12) -0.0069(10) 0.0018(10) 0.0019(10) O5 0.0138(10) 0.0171(11) 0.0196(11) 0.0004(9) 0.0017(9) 0.0019(8) O6 0.0154(11) 0.0168(12) 0.0217(12) 0.0036(10) 0.0031(9) -0.0005(9) O7 0.0243(16) 0.0257(14) 0.0192(14) 0.0041(11) 0.0037(11) 0.0003(11) O8 0.0296(15) 0.0442(17) 0.0193(13) -0.0004(12) 0.0022(12) 0.0142(13) O9 0.0238(16) 0.081(3) 0.0184(14) -0.0086(14) 0.0065(12) 0.0116(16) O10 0.0260(14) 0.0345(16) 0.0510(18) -0.0118(13) 0.0074(13) -0.0028(12) O11 0.081(3) 0.0249(15) 0.0492(19) 0.0020(13) 0.0325(18) 0.0003(15) C1 0.0247(16) 0.0145(14) 0.0143(14) 0.0036(11) 0.0073(12) -0.0021(12) C2 0.0221(16) 0.0153(14) 0.0140(14) 0.0029(11) 0.0061(12) 0.0006(12) C3 0.0294(18) 0.0161(15) 0.0169(15) 0.0005(12) 0.0068(13) -0.0047(13) C4 0.036(2) 0.0134(15) 0.0210(16) -0.0006(12) 0.0101(14) -0.0028(13) C5 0.0331(19) 0.0156(15) 0.0260(17) 0.0031(13) 0.0142(15) 0.0029(14) C6 0.0263(17) 0.0175(15) 0.0217(16) 0.0035(13) 0.0104(13) 0.0005(13) C7 0.0231(17) 0.0189(16) 0.0269(18) 0.0039(13) 0.0080(14) 0.0067(13) C8 0.0196(16) 0.0215(16) 0.0215(16) 0.0028(13) 0.0048(13) 0.0079(13) C9 0.0153(15) 0.0250(17) 0.0174(15) 0.0061(13) 0.0015(12) 0.0075(13) C10 0.0145(15) 0.0238(17) 0.0222(17) 0.0053(13) -0.0001(12) 0.0070(13) C11 0.0138(15) 0.0294(18) 0.0265(18) 0.0081(14) 0.0037(13) 0.0039(13) C12 0.0215(17) 0.042(2) 0.0225(17) 0.0076(15) 0.0098(14) 0.0068(16) C13 0.0267(18) 0.0290(19) 0.0211(17) 0.0028(14) 0.0077(14) 0.0079(14) C14 0.0168(16) 0.0265(18) 0.0258(18) 0.0002(14) 0.0018(13) 0.0009(13) C15 0.0175(15) 0.0192(16) 0.0216(16) 0.0001(13) 0.0019(12) -0.0005(12) C16 0.0186(15) 0.0179(15) 0.0151(14) -0.0020(12) 0.0031(12) -0.0026(12) C17 0.0159(15) 0.0201(15) 0.0128(14) -0.0038(12) 0.0018(11) -0.0007(12) C18 0.0227(16) 0.0127(14) 0.0204(16) -0.0033(12) 0.0035(13) -0.0002(12) C19 0.0232(17) 0.0195(16) 0.0276(18) -0.0027(13) 0.0066(14) -0.0060(13) C20 0.0204(17) 0.0256(18) 0.0294(18) -0.0016(14) 0.0064(14) -0.0040(14) C21 0.0220(16) 0.0192(16) 0.0170(15) 0.0010(12) 0.0080(13) 0.0041(12) C22 0.0156(15) 0.0154(15) 0.0205(16) 0.0013(12) 0.0045(12) -0.0010(12) C23 0.0167(15) 0.0135(14) 0.0226(16) -0.0035(12) 0.0070(12) -0.0014(11) C24 0.0190(15) 0.0112(14) 0.0221(16) 0.0009(12) 0.0040(12) -0.0008(12) C25 0.0191(16) 0.0146(15) 0.0301(18) 0.0022(13) 0.0074(13) 0.0011(12) C26 0.0244(17) 0.0161(15) 0.0296(18) -0.0043(13) 0.0135(14) 0.0030(13) C27 0.0221(16) 0.0173(15) 0.0211(16) -0.0030(12) 0.0083(13) -0.0021(12) C28 0.0256(17) 0.0170(15) 0.0202(16) 0.0020(12) 0.0054(13) 0.0041(13) C29 0.0201(16) 0.0238(17) 0.0150(15) -0.0035(12) 0.0027(12) 0.0020(13) C30 0.0193(16) 0.0215(16) 0.0148(15) 0.0022(12) 0.0049(12) 0.0026(13) C31 0.0202(16) 0.0203(16) 0.0158(15) 0.0005(12) 0.0040(12) 0.0018(12) C32 0.0225(17) 0.034(2) 0.0221(17) -0.0068(15) -0.0011(14) 0.0000(15) C33 0.0205(18) 0.041(2) 0.033(2) -0.0080(17) -0.0035(15) 0.0102(16) C34 0.030(2) 0.0261(19) 0.032(2) -0.0067(15) -0.0011(16) 0.0125(15) C35 0.0219(16) 0.0228(17) 0.0141(15) -0.0033(12) 0.0007(12) -0.0022(13) C36 0.0224(16) 0.0189(16) 0.0172(15) -0.0013(12) 0.0041(13) -0.0008(13) C37 0.0158(15) 0.0190(15) 0.0162(15) -0.0044(12) 0.0034(12) -0.0028(12) C38 0.0170(15) 0.0201(16) 0.0194(16) -0.0022(12) 0.0029(12) 0.0006(12) C39 0.0245(18) 0.0267(18) 0.0249(18) -0.0004(14) 0.0092(14) -0.0059(14) C40 0.0205(18) 0.039(2) 0.031(2) -0.0005(16) 0.0065(15) -0.0107(16) C41 0.0165(16) 0.036(2) 0.0232(18) -0.0004(15) -0.0021(13) -0.0042(14) C42 0.0169(15) 0.0189(15) 0.0138(14) -0.0004(12) 0.0029(12) -0.0007(12) C43 0.0246(18) 0.0226(17) 0.033(2) -0.0038(15) 0.0074(15) 0.0035(14) C44 0.035(2) 0.055(3) 0.030(2) -0.0056(19) 0.0112(17) -0.011(2) C45 0.036(2) 0.030(2) 0.030(2) 0.0009(16) 0.0111(16) 0.0018(16) C46 0.071(3) 0.028(2) 0.0246(19) -0.0021(16) 0.027(2) -0.003(2) C47 0.064(3) 0.033(2) 0.054(3) -0.001(2) 0.040(2) -0.003(2) C48 0.056(3) 0.043(3) 0.038(2) -0.011(2) 0.016(2) -0.003(2) _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 Rb1 O10 2.863(3) . ? Rb1 O8 2.993(3) . ? Rb1 O9 2.999(4) . ? Rb1 O3 3.005(3) 4_565 ? Rb1 O6 3.008(2) . ? Rb1 O7 3.029(3) . ? Rb1 C4 3.314(3) . ? Rb1 C3 3.398(3) . ? Rb1 C5 3.457(3) . ? Rb1 O1 3.528(2) 4_565 ? Rb1 C2 3.623(3) . ? Rb1 C6 3.688(3) . ? Rb1 H6O 3.28(4) . ? Rb1 H7D 3.00(5) . ? Rb1 H8C 3.24(5) . ? Rb1 H9C 3.12(5) . ? K1 O9 2.658(3) . ? K1 O8 2.685(3) . ? K1 O7 2.727(3) . ? K1 O11 2.773(3) . ? K1 O4 2.786(3) . ? K1 C18 3.154(3) . ? K1 C19 3.208(3) . ? K1 C17 3.242(3) . ? K1 C20 3.318(4) . ? K1 C16 3.384(3) . ? K1 C15 3.417(3) . ? K1 H4O 3.05(4) . ? K1 H7D 3.07(5) . ? K1 H9D 3.06(6) . ? O1 C1 1.357(4) . ? O1 Rb1 3.528(2) 4_566 ? O1 H1O 0.72(4) . ? O2 C9 1.338(4) . ? O3 C16 1.362(4) . ? O3 Rb1 3.005(3) 4_566 ? O3 H3O 0.66(4) . ? O4 C23 1.362(4) . ? O4 H4O 0.67(4) . ? O5 C30 1.345(4) . ? O6 C37 1.366(4) . ? O6 H6O 0.69(4) . ? O7 H7C 0.68(5) . ? O7 H7D 0.70(5) . ? O8 H8D 0.78(6) . ? O8 H8C 0.90(5) . ? O9 H9D 0.66(6) . ? O9 H9C 0.79(6) . ? O10 C43 1.208(4) . ? O11 C46 1.217(5) . ? C1 C2 1.400(5) . ? C1 C6 1.404(5) . ? C2 C3 1.390(4) . ? C2 C42 1.514(4) . ? C3 C4 1.391(5) . ? C3 H3A 1.0000 . ? C4 C5 1.390(5) . ? C4 H4A 1.0000 . ? C5 C6 1.391(5) . ? C5 H5A 1.0000 . ? C6 C7 1.533(5) . ? C7 C8 1.505(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.399(5) . ? C8 C9 1.412(5) . ? C9 C10 1.410(5) . ? C10 C11 1.391(5) . ? C10 C14 1.522(5) . ? C11 C12 1.402(5) . ? C11 H11A 0.9500 . ? C12 C13 1.383(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.518(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.397(5) . ? C15 C16 1.406(5) . ? C16 C17 1.404(4) . ? C17 C18 1.391(5) . ? C17 C21 1.513(4) . ? C18 C19 1.384(5) . ? C18 H18A 1.0000 . ? C19 C20 1.384(5) . ? C19 H19A 1.0000 . ? C20 H20A 1.0000 . ? C21 C22 1.503(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.394(4) . ? C22 C23 1.404(5) . ? C23 C24 1.405(4) . ? C24 C25 1.393(5) . ? C24 C28 1.521(5) . ? C25 C26 1.391(5) . ? C25 H25A 0.9500 . ? C26 C27 1.389(5) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.516(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.399(5) . ? C29 C30 1.410(5) . ? C30 C31 1.412(5) . ? C31 C32 1.385(5) . ? C31 C35 1.517(5) . ? C32 C33 1.377(6) . ? C32 H32A 0.9500 . ? C33 C34 1.386(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.517(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.394(5) . ? C36 C37 1.398(4) . ? C37 C38 1.404(5) . ? C38 C39 1.392(5) . ? C38 C42 1.510(4) . ? C39 C40 1.390(5) . ? C39 H39A 0.9500 . ? C40 C41 1.372(5) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C45 1.494(5) . ? C43 C44 1.495(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.477(7) . ? C46 C47 1.486(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 O10 Rb1 O8 153.59(9) . . ? O10 Rb1 O9 101.38(9) . . ? O8 Rb1 O9 65.39(9) . . ? O10 Rb1 O3 91.98(8) . 4_565 ? O8 Rb1 O3 72.68(8) . 4_565 ? O9 Rb1 O3 108.93(8) . 4_565 ? O10 Rb1 O6 75.50(7) . . ? O8 Rb1 O6 116.80(7) . . ? O9 Rb1 O6 69.52(8) . . ? O3 Rb1 O6 166.49(7) 4_565 . ? O10 Rb1 O7 131.07(8) . . ? O8 Rb1 O7 67.19(8) . . ? O9 Rb1 O7 67.60(8) . . ? O3 Rb1 O7 136.95(8) 4_565 . ? O6 Rb1 O7 55.76(7) . . ? O10 Rb1 C4 72.62(9) . . ? O8 Rb1 C4 128.35(9) . . ? O9 Rb1 C4 157.06(9) . . ? O3 Rb1 C4 93.57(8) 4_565 . ? O6 Rb1 C4 87.56(8) . . ? O7 Rb1 C4 99.13(8) . . ? O10 Rb1 C3 69.54(9) . . ? O8 Rb1 C3 136.47(8) . . ? O9 Rb1 C3 133.17(9) . . ? O3 Rb1 C3 117.03(8) 4_565 . ? O6 Rb1 C3 63.71(8) . . ? O7 Rb1 C3 84.11(8) . . ? C4 Rb1 C3 23.89(8) . . ? O10 Rb1 C5 94.87(9) . . ? O8 Rb1 C5 104.78(8) . . ? O9 Rb1 C5 157.96(8) . . ? O3 Rb1 C5 85.07(8) 4_565 . ? O6 Rb1 C5 100.79(8) . . ? O7 Rb1 C5 90.49(8) . . ? C4 Rb1 C5 23.58(9) . . ? C3 Rb1 C5 41.10(9) . . ? O10 Rb1 O1 87.45(8) . 4_565 ? O8 Rb1 O1 66.57(7) . 4_565 ? O9 Rb1 O1 48.25(7) . 4_565 ? O3 Rb1 O1 63.44(7) 4_565 4_565 ? O6 Rb1 O1 110.16(7) . 4_565 ? O7 Rb1 O1 111.48(7) . 4_565 ? C4 Rb1 O1 149.37(7) . 4_565 ? C3 Rb1 O1 156.94(7) . 4_565 ? C5 Rb1 O1 148.50(7) . 4_565 ? O10 Rb1 C2 88.11(8) . . ? O8 Rb1 C2 118.22(8) . . ? O9 Rb1 C2 118.75(8) . . ? O3 Rb1 C2 131.31(7) 4_565 . ? O6 Rb1 C2 54.61(7) . . ? O7 Rb1 C2 61.70(7) . . ? C4 Rb1 C2 40.55(8) . . ? C3 Rb1 C2 22.54(7) . . ? C5 Rb1 C2 46.51(8) . . ? O1 Rb1 C2 164.77(7) 4_565 . ? O10 Rb1 C6 112.09(8) . . ? O8 Rb1 C6 91.69(8) . . ? O9 Rb1 C6 135.85(8) . . ? O3 Rb1 C6 98.14(7) 4_565 . ? O6 Rb1 C6 91.38(7) . . ? O7 Rb1 C6 68.77(8) . . ? C4 Rb1 C6 39.98(8) . . ? C3 Rb1 C6 46.26(8) . . ? C5 Rb1 C6 22.16(8) . . ? O1 Rb1 C6 154.35(7) 4_565 . ? C2 Rb1 C6 39.13(7) . . ? O10 Rb1 H6O 76.7(7) . . ? O8 Rb1 H6O 110.7(7) . . ? O9 Rb1 H6O 58.3(7) . . ? O3 Rb1 H6O 159.7(7) 4_565 . ? O6 Rb1 H6O 11.6(7) . . ? O7 Rb1 H6O 56.6(7) . . ? C4 Rb1 H6O 98.8(7) . . ? C3 Rb1 H6O 75.1(7) . . ? C5 Rb1 H6O 112.3(7) . . ? O1 Rb1 H6O 98.9(7) 4_565 . ? C2 Rb1 H6O 65.9(7) . . ? C6 Rb1 H6O 101.7(7) . . ? O10 Rb1 H7D 117.8(11) . . ? O8 Rb1 H7D 78.8(10) . . ? O9 Rb1 H7D 65.4(10) . . ? O3 Rb1 H7D 150.1(11) 4_565 . ? O6 Rb1 H7D 42.4(11) . . ? O7 Rb1 H7D 13.4(10) . . ? C4 Rb1 H7D 97.2(10) . . ? C3 Rb1 H7D 78.4(10) . . ? C5 Rb1 H7D 93.9(10) . . ? O1 Rb1 H7D 112.8(10) 4_565 . ? C2 Rb1 H7D 57.2(10) . . ? C6 Rb1 H7D 73.7(10) . . ? H6O Rb1 H7D 43.6(13) . . ? O10 Rb1 H8C 139.0(9) . . ? O8 Rb1 H8C 15.9(9) . . ? O9 Rb1 H8C 67.3(8) . . ? O3 Rb1 H8C 58.8(9) 4_565 . ? O6 Rb1 H8C 128.8(8) . . ? O7 Rb1 H8C 82.8(9) . . ? C4 Rb1 H8C 131.6(8) . . ? C3 Rb1 H8C 147.1(8) . . ? C5 Rb1 H8C 109.0(8) . . ? O1 Rb1 H8C 55.0(8) 4_565 . ? C2 Rb1 H8C 132.5(9) . . ? C6 Rb1 H8C 100.8(8) . . ? H6O Rb1 H8C 120.6(11) . . ? H7D Rb1 H8C 93.9(14) . . ? O10 Rb1 H9C 96.5(10) . . ? O8 Rb1 H9C 64.8(9) . . ? O9 Rb1 H9C 14.7(11) . . ? O3 Rb1 H9C 95.4(11) 4_565 . ? O6 Rb1 H9C 81.2(11) . . ? O7 Rb1 H9C 81.4(11) . . ? C4 Rb1 H9C 166.1(10) . . ? C3 Rb1 H9C 144.3(10) . . ? C5 Rb1 H9C 168.6(10) . . ? O1 Rb1 H9C 33.6(11) 4_565 . ? C2 Rb1 H9C 132.9(11) . . ? C6 Rb1 H9C 147.7(10) . . ? H6O Rb1 H9C 69.7(13) . . ? H7D Rb1 H9C 80.0(14) . . ? H8C Rb1 H9C 62.3(12) . . ? O9 K1 O8 74.56(10) . . ? O9 K1 O7 77.03(11) . . ? O8 K1 O7 76.00(9) . . ? O9 K1 O11 94.10(11) . . ? O8 K1 O11 105.92(10) . . ? O7 K1 O11 170.19(11) . . ? O9 K1 O4 73.04(9) . . ? O8 K1 O4 138.58(9) . . ? O7 K1 O4 72.15(8) . . ? O11 K1 O4 101.48(9) . . ? O9 K1 C18 137.65(10) . . ? O8 K1 C18 146.63(9) . . ? O7 K1 C18 99.98(9) . . ? O11 K1 C18 83.70(9) . . ? O4 K1 C18 66.11(8) . . ? O9 K1 C19 155.60(11) . . ? O8 K1 C19 127.55(9) . . ? O7 K1 C19 115.44(9) . . ? O11 K1 C19 71.34(10) . . ? O4 K1 C19 90.36(8) . . ? C18 K1 C19 25.11(9) . . ? O9 K1 C17 131.38(10) . . ? O8 K1 C17 133.49(9) . . ? O7 K1 C17 75.07(8) . . ? O11 K1 C17 108.75(9) . . ? O4 K1 C17 60.86(8) . . ? C18 K1 C17 25.07(8) . . ? C19 K1 C17 43.99(9) . . ? O9 K1 C20 178.21(11) . . ? O8 K1 C20 104.79(9) . . ? O7 K1 C20 104.48(9) . . ? O11 K1 C20 84.47(10) . . ? O4 K1 C20 108.27(9) . . ? C18 K1 C20 43.31(9) . . ? C19 K1 C20 24.41(9) . . ? C17 K1 C20 50.26(9) . . ? O9 K1 C16 139.84(10) . . ? O8 K1 C16 109.49(9) . . ? O7 K1 C16 66.06(9) . . ? O11 K1 C16 121.06(9) . . ? O4 K1 C16 80.85(8) . . ? C18 K1 C16 42.94(8) . . ? C19 K1 C16 49.72(8) . . ? C17 K1 C16 24.35(8) . . ? C20 K1 C16 41.92(8) . . ? O9 K1 C15 157.49(10) . . ? O8 K1 C15 96.78(9) . . ? O7 K1 C15 80.73(9) . . ? O11 K1 C15 108.33(10) . . ? O4 K1 C15 103.41(8) . . ? C18 K1 C15 50.28(8) . . ? C19 K1 C15 42.84(8) . . ? C17 K1 C15 43.08(8) . . ? C20 K1 C15 23.88(8) . . ? C16 K1 C15 23.86(8) . . ? O9 K1 Rb1 44.98(9) . . ? O8 K1 Rb1 44.91(7) . . ? O7 K1 Rb1 45.77(6) . . ? O11 K1 Rb1 129.26(7) . . ? O4 K1 Rb1 93.67(6) . . ? C18 K1 Rb1 145.45(7) . . ? C19 K1 Rb1 157.33(7) . . ? C17 K1 Rb1 120.80(6) . . ? C20 K1 Rb1 135.58(7) . . ? C16 K1 Rb1 108.98(6) . . ? C15 K1 Rb1 114.69(6) . . ? O9 K1 H4O 61.1(8) . . ? O8 K1 H4O 127.7(8) . . ? O7 K1 H4O 68.5(8) . . ? O11 K1 H4O 103.7(8) . . ? O4 K1 H4O 12.2(8) . . ? C18 K1 H4O 78.3(8) . . ? C19 K1 H4O 102.4(8) . . ? C17 K1 H4O 71.8(8) . . ? C20 K1 H4O 120.3(8) . . ? C16 K1 H4O 90.0(8) . . ? C15 K1 H4O 113.4(8) . . ? Rb1 K1 H4O 83.1(8) . . ? O9 K1 H7D 68.5(10) . . ? O8 K1 H7D 82.5(10) . . ? O7 K1 H7D 12.1(10) . . ? O11 K1 H7D 158.3(10) . . ? O4 K1 H7D 62.0(10) . . ? C18 K1 H7D 100.3(10) . . ? C19 K1 H7D 119.7(10) . . ? C17 K1 H7D 76.6(10) . . ? C20 K1 H7D 113.2(10) . . ? C16 K1 H7D 72.5(10) . . ? C15 K1 H7D 90.0(10) . . ? Rb1 K1 H7D 45.3(9) . . ? H4O K1 H7D 57.2(12) . . ? O9 K1 H9D 10.6(12) . . ? O8 K1 H9D 84.6(12) . . ? O7 K1 H9D 75.8(12) . . ? O11 K1 H9D 94.7(11) . . ? O4 K1 H9D 62.5(12) . . ? C18 K1 H9D 127.1(12) . . ? C19 K1 H9D 147.0(12) . . ? C17 K1 H9D 121.7(12) . . ? C20 K1 H9D 170.4(12) . . ? C16 K1 H9D 133.6(12) . . ? C15 K1 H9D 155.4(12) . . ? Rb1 K1 H9D 51.0(11) . . ? H4O K1 H9D 50.7(14) . . ? H7D K1 H9D 65.7(15) . . ? C1 O1 Rb1 158.6(2) . 4_566 ? C1 O1 H1O 115(3) . . ? Rb1 O1 H1O 87(3) 4_566 . ? C16 O3 Rb1 152.2(2) . 4_566 ? C16 O3 H3O 107(4) . . ? Rb1 O3 H3O 100(4) 4_566 . ? C23 O4 K1 146.7(2) . . ? C23 O4 H4O 106(3) . . ? K1 O4 H4O 107(3) . . ? C37 O6 Rb1 130.5(2) . . ? C37 O6 H6O 106(3) . . ? Rb1 O6 H6O 107(3) . . ? K1 O7 Rb1 94.07(9) . . ? K1 O7 H7C 122(4) . . ? Rb1 O7 H7C 130(4) . . ? K1 O7 H7D 113(4) . . ? Rb1 O7 H7D 81(4) . . ? H7C O7 H7D 109(6) . . ? K1 O8 Rb1 95.78(9) . . ? K1 O8 H8D 116(4) . . ? Rb1 O8 H8D 117(4) . . ? K1 O8 H8C 129(3) . . ? Rb1 O8 H8C 98(3) . . ? H8D O8 H8C 101(5) . . ? K1 O9 Rb1 96.22(11) . . ? K1 O9 H9D 122(5) . . ? Rb1 O9 H9D 112(5) . . ? K1 O9 H9C 122(4) . . ? Rb1 O9 H9C 91(4) . . ? H9D O9 H9C 108(6) . . ? C43 O10 Rb1 169.7(3) . . ? C46 O11 K1 126.9(3) . . ? O1 C1 C2 116.3(3) . . ? O1 C1 C6 122.0(3) . . ? C2 C1 C6 121.6(3) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 C42 122.0(3) . . ? C1 C2 C42 119.7(3) . . ? C3 C2 Rb1 69.58(18) . . ? C1 C2 Rb1 84.40(18) . . ? C42 C2 Rb1 116.16(19) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 Rb1 87.87(19) . . ? C4 C3 Rb1 74.68(19) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? Rb1 C3 H3A 118.9 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 Rb1 84.0(2) . . ? C3 C4 Rb1 81.43(19) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? Rb1 C4 H4A 119.0 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 Rb1 72.42(19) . . ? C6 C5 Rb1 88.3(2) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? Rb1 C5 H5A 119.1 . . ? C5 C6 C1 118.3(3) . . ? C5 C6 C7 120.5(3) . . ? C1 C6 C7 121.1(3) . . ? C5 C6 Rb1 69.57(19) . . ? C1 C6 Rb1 81.81(18) . . ? C7 C6 Rb1 122.3(2) . . ? C8 C7 C6 116.1(3) . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 118.9(3) . . ? C13 C8 C7 120.6(3) . . ? C9 C8 C7 120.5(3) . . ? O2 C9 C10 119.8(3) . . ? O2 C9 C8 120.0(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 119.3(3) . . ? C11 C10 C14 120.6(3) . . ? C9 C10 C14 120.1(3) . . ? C10 C11 C12 121.0(3) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C8 121.4(3) . . ? C12 C13 H13A 119.3 . . ? C8 C13 H13A 119.3 . . ? C15 C14 C10 116.4(3) . . ? C15 C14 H14A 108.2 . . ? C10 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C10 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C20 C15 C16 117.7(3) . . ? C20 C15 C14 120.1(3) . . ? C16 C15 C14 122.1(3) . . ? C20 C15 K1 74.1(2) . . ? C16 C15 K1 76.72(18) . . ? C14 C15 K1 121.9(2) . . ? O3 C16 C17 116.5(3) . . ? O3 C16 C15 122.1(3) . . ? C17 C16 C15 121.4(3) . . ? O3 C16 K1 119.64(19) . . ? C17 C16 K1 72.16(17) . . ? C15 C16 K1 79.42(19) . . ? C18 C17 C16 118.5(3) . . ? C18 C17 C21 123.2(3) . . ? C16 C17 C21 118.2(3) . . ? C18 C17 K1 73.94(18) . . ? C16 C17 K1 83.50(19) . . ? C21 C17 K1 112.85(19) . . ? C19 C18 C17 121.0(3) . . ? C19 C18 K1 79.6(2) . . ? C17 C18 K1 80.99(18) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? K1 C18 H18A 119.1 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 K1 82.2(2) . . ? C18 C19 K1 75.26(19) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? K1 C19 H19A 119.9 . . ? C19 C20 C15 121.6(3) . . ? C19 C20 K1 73.4(2) . . ? C15 C20 K1 82.1(2) . . ? C19 C20 H20A 119.1 . . ? C15 C20 H20A 119.1 . . ? K1 C20 H20A 119.1 . . ? C22 C21 C17 118.4(3) . . ? C22 C21 H21A 107.7 . . ? C17 C21 H21A 107.7 . . ? C22 C21 H21B 107.7 . . ? C17 C21 H21B 107.7 . . ? H21A C21 H21B 107.1 . . ? C27 C22 C23 117.9(3) . . ? C27 C22 C21 121.5(3) . . ? C23 C22 C21 120.2(3) . . ? O4 C23 C22 117.3(3) . . ? O4 C23 C24 121.1(3) . . ? C22 C23 C24 121.5(3) . . ? C25 C24 C23 118.4(3) . . ? C25 C24 C28 120.6(3) . . ? C23 C24 C28 121.0(3) . . ? C26 C25 C24 121.1(3) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C22 121.6(3) . . ? C26 C27 H27A 119.2 . . ? C22 C27 H27A 119.2 . . ? C29 C28 C24 116.6(3) . . ? C29 C28 H28A 108.1 . . ? C24 C28 H28A 108.1 . . ? C29 C28 H28B 108.1 . . ? C24 C28 H28B 108.1 . . ? H28A C28 H28B 107.3 . . ? C34 C29 C30 118.1(3) . . ? C34 C29 C28 120.9(3) . . ? C30 C29 C28 120.9(3) . . ? O5 C30 C29 120.1(3) . . ? O5 C30 C31 120.1(3) . . ? C29 C30 C31 119.8(3) . . ? C32 C31 C30 120.0(3) . . ? C32 C31 C35 120.0(3) . . ? C30 C31 C35 120.0(3) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C33 C34 C29 121.8(3) . . ? C33 C34 H34A 119.1 . . ? C29 C34 H34A 119.1 . . ? C31 C35 C36 114.1(3) . . ? C31 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C31 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C41 C36 C37 118.2(3) . . ? C41 C36 C35 120.2(3) . . ? C37 C36 C35 121.6(3) . . ? O6 C37 C36 121.4(3) . . ? O6 C37 C38 117.7(3) . . ? C36 C37 C38 120.9(3) . . ? C39 C38 C37 118.8(3) . . ? C39 C38 C42 121.5(3) . . ? C37 C38 C42 119.7(3) . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C41 C40 C39 119.8(3) . . ? C41 C40 H40A 120.1 . . ? C39 C40 H40A 120.1 . . ? C40 C41 C36 121.6(3) . . ? C40 C41 H41A 119.2 . . ? C36 C41 H41A 119.2 . . ? C38 C42 C2 114.3(3) . . ? C38 C42 H42A 108.7 . . ? C2 C42 H42A 108.7 . . ? C38 C42 H42B 108.7 . . ? C2 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O10 C43 C45 122.1(4) . . ? O10 C43 C44 121.7(4) . . ? C45 C43 C44 116.3(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O11 C46 C48 121.3(4) . . ? O11 C46 C47 121.8(5) . . ? C48 C46 C47 117.0(4) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.895 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.104 #===END data_40 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H78 Li2 O10' _chemical_formula_weight 925.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Li' 'Li' -0.0003 0.0001 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.668(3) _cell_length_b 22.379(5) _cell_length_c 20.881(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.354(4) _cell_angle_gamma 90.00 _cell_volume 6283(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .63 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21748 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 21.00 _reflns_number_total 6735 _reflns_number_gt 3959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 SHELXL _refine_ls_extinction_coef 0.0053(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6735 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1601 _refine_ls_R_factor_gt 0.1052 _refine_ls_wR_factor_ref 0.3187 _refine_ls_wR_factor_gt 0.2777 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 4.020 _refine_ls_shift/su_mean 0.132 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 Li1 Li 0.5750(8) 0.5100(4) 0.9799(5) 0.042(3) Uani 1 1 d . . . Li2 Li 0.5710(9) 0.5864(5) 1.1202(5) 0.050(3) Uani 1 1 d . . . O1 O 0.5862(3) 0.59470(18) 0.9669(2) 0.0431(12) Uani 1 1 d . . . O2 O 0.5019(3) 0.63952(18) 1.05499(18) 0.0397(11) Uani 1 1 d . . . O3 O 0.3590(3) 0.56631(19) 1.02638(19) 0.0426(12) Uani 1 1 d . . . O4 O 0.4433(3) 0.49017(17) 0.92835(17) 0.0380(11) Uani 1 1 d . . . O5 O 0.7042(4) 0.6178(2) 1.1470(3) 0.0673(15) Uani 1 1 d . . . O6 O 0.5171(4) 0.5919(2) 1.2029(2) 0.0717(16) Uani 1 1 d . . . O7 O 0.7634(5) 0.7116(3) 0.3159(3) 0.103(2) Uani 1 1 d . . . O8 O 0.9407(11) 0.5072(7) 0.7795(8) 0.304(10) Uani 1 1 d . . . O9 O 0.168(5) 0.0996(11) 0.020(2) 0.90(6) Uani 1 1 d . . . O10 O 0.970(4) 0.9349(16) 0.075(3) 0.78(5) Uani 1 1 d . . . C1 C 0.6045(5) 0.6338(3) 0.9196(3) 0.0417(17) Uani 1 1 d . . . C2 C 0.5948(5) 0.6117(3) 0.8550(3) 0.0481(19) Uani 1 1 d . . . C3 C 0.6183(5) 0.6493(4) 0.8075(4) 0.065(2) Uani 1 1 d . . . H3 H 0.6125 0.6351 0.7652 0.078 Uiso 1 1 calc R . . C4 C 0.6504(6) 0.7077(4) 0.8208(4) 0.074(3) Uani 1 1 d . . . C5 C 0.6559(5) 0.7291(4) 0.8848(4) 0.068(2) Uani 1 1 d . . . H5 H 0.6756 0.7684 0.8942 0.081 Uiso 1 1 calc R . . C6 C 0.6327(5) 0.6930(3) 0.9348(3) 0.0474(18) Uani 1 1 d . . . C7 C 0.6389(5) 0.7177(3) 1.0041(3) 0.0501(19) Uani 1 1 d . . . H7A H 0.6851 0.7510 1.0101 0.060 Uiso 1 1 calc R . . H7B H 0.6657 0.6868 1.0350 0.060 Uiso 1 1 calc R . . C8 C 0.5386(5) 0.7388(3) 1.0199(3) 0.0441(17) Uani 1 1 d . . . C9 C 0.4759(5) 0.6985(3) 1.0456(3) 0.0383(16) Uani 1 1 d . . . C10 C 0.3845(5) 0.7188(3) 1.0609(3) 0.0410(17) Uani 1 1 d . . . C11 C 0.3578(5) 0.7787(3) 1.0474(3) 0.0528(19) Uani 1 1 d . . . H11 H 0.2975 0.7921 1.0569 0.063 Uiso 1 1 calc R . . C12 C 0.4165(6) 0.8193(3) 1.0206(3) 0.054(2) Uani 1 1 d . . . C13 C 0.5072(6) 0.7980(3) 1.0088(3) 0.057(2) Uani 1 1 d . . . H13 H 0.5492 0.8245 0.9926 0.069 Uiso 1 1 calc R . . C14 C 0.3177(5) 0.6768(3) 1.0903(3) 0.0425(17) Uani 1 1 d . . . H14A H 0.2835 0.6999 1.1189 0.051 Uiso 1 1 calc R . . H14B H 0.3595 0.6480 1.1172 0.051 Uiso 1 1 calc R . . C15 C 0.2390(5) 0.6422(3) 1.0422(3) 0.0368(16) Uani 1 1 d . . . C16 C 0.2646(5) 0.5904(3) 1.0115(3) 0.0343(16) Uani 1 1 d . . . C17 C 0.1948(5) 0.5603(3) 0.9653(3) 0.0362(16) Uani 1 1 d . . . C18 C 0.0966(5) 0.5808(3) 0.9533(3) 0.0416(17) Uani 1 1 d . . . H18 H 0.0497 0.5602 0.9235 0.050 Uiso 1 1 calc R . . C19 C 0.0662(5) 0.6312(3) 0.9845(3) 0.0408(17) Uani 1 1 d . . . C20 C 0.1403(5) 0.6613(3) 1.0280(3) 0.0447(18) Uani 1 1 d . . . H20 H 0.1226 0.6956 1.0483 0.054 Uiso 1 1 calc R . . C21 C 0.2278(5) 0.5088(3) 0.9253(3) 0.0374(16) Uani 1 1 d . . . H21A H 0.2687 0.4811 0.9542 0.045 Uiso 1 1 calc R . . H21B H 0.1698 0.4874 0.9031 0.045 Uiso 1 1 calc R . . C22 C 0.2870(5) 0.5330(3) 0.8752(3) 0.0349(16) Uani 1 1 d . . . C23 C 0.3899(5) 0.5243(3) 0.8802(3) 0.0342(16) Uani 1 1 d . . . C24 C 0.4381(5) 0.5507(3) 0.8322(3) 0.0378(16) Uani 1 1 d . . . C25 C 0.3791(6) 0.5793(3) 0.7785(3) 0.0505(19) Uani 1 1 d . . . H25 H 0.4110 0.5944 0.7462 0.061 Uiso 1 1 calc R . . C26 C 0.2769(5) 0.5864(3) 0.7705(3) 0.0429(17) Uani 1 1 d . . . C27 C 0.2338(5) 0.5630(3) 0.8206(3) 0.0409(17) Uani 1 1 d . . . H27 H 0.1655 0.5674 0.8179 0.049 Uiso 1 1 calc R . . C28 C 0.5510(5) 0.5508(3) 0.8367(3) 0.0500(19) Uani 1 1 d . . . H28A H 0.5805 0.5218 0.8691 0.060 Uiso 1 1 calc R . . H28B H 0.5669 0.5389 0.7951 0.060 Uiso 1 1 calc R . . C29 C 0.6801(9) 0.7476(6) 0.7659(5) 0.122(5) Uani 1 1 d . . . C30 C 0.7363(16) 0.7995(6) 0.7878(6) 0.233(11) Uani 1 1 d . . . H30A H 0.7350 0.8266 0.7521 0.349 Uiso 1 1 calc R . . H30B H 0.8038 0.7883 0.8048 0.349 Uiso 1 1 calc R . . H30C H 0.7080 0.8185 0.8215 0.349 Uiso 1 1 calc R . . C31 C 0.7731(10) 0.7083(8) 0.7362(8) 0.201(9) Uani 1 1 d . . . H31A H 0.7530 0.6674 0.7286 0.302 Uiso 1 1 calc R . . H31B H 0.8337 0.7099 0.7675 0.302 Uiso 1 1 calc R . . H31C H 0.7835 0.7260 0.6961 0.302 Uiso 1 1 calc R . . C32 C 0.6008(8) 0.7501(5) 0.7077(4) 0.119(4) Uani 1 1 d . . . H32A H 0.5428 0.7687 0.7188 0.178 Uiso 1 1 calc R . . H32B H 0.5845 0.7103 0.6923 0.178 Uiso 1 1 calc R . . H32C H 0.6234 0.7728 0.6743 0.178 Uiso 1 1 calc R . . C33 C 0.3812(6) 0.8843(3) 1.0062(4) 0.072(2) Uani 1 1 d . . . C34 C 0.2777(7) 0.8859(4) 0.9644(5) 0.107(3) Uani 1 1 d . . . H34A H 0.2313 0.8670 0.9874 0.161 Uiso 1 1 calc R . . H34B H 0.2784 0.8651 0.9243 0.161 Uiso 1 1 calc R . . H34C H 0.2581 0.9267 0.9553 0.161 Uiso 1 1 calc R . . C35 C 0.3800(11) 0.9167(4) 1.0706(6) 0.154(6) Uani 1 1 d . . . H35A H 0.3465 0.9544 1.0621 0.231 Uiso 1 1 calc R . . H35B H 0.4470 0.9234 1.0926 0.231 Uiso 1 1 calc R . . H35C H 0.3456 0.8927 1.0975 0.231 Uiso 1 1 calc R . . C36 C 0.4482(9) 0.9184(4) 0.9679(7) 0.146(5) Uani 1 1 d . . . H36A H 0.4580 0.8951 0.9309 0.219 Uiso 1 1 calc R . . H36B H 0.5113 0.9258 0.9953 0.219 Uiso 1 1 calc R . . H36C H 0.4176 0.9557 0.9533 0.219 Uiso 1 1 calc R . . C37 C -0.0420(5) 0.6516(3) 0.9705(4) 0.059(2) Uani 1 1 d . . . C38 C -0.0795(9) 0.6548(8) 0.9001(6) 0.208(9) Uani 1 1 d . . . H38A H -0.0420 0.6840 0.8810 0.311 Uiso 1 1 calc R . . H38B H -0.1484 0.6661 0.8926 0.311 Uiso 1 1 calc R . . H38C H -0.0725 0.6164 0.8808 0.311 Uiso 1 1 calc R . . C39 C -0.1051(8) 0.6053(6) 0.9978(8) 0.175(7) Uani 1 1 d . . . H39A H -0.1702 0.6214 0.9980 0.263 Uiso 1 1 calc R . . H39B H -0.0743 0.5953 1.0415 0.263 Uiso 1 1 calc R . . H39C H -0.1107 0.5700 0.9712 0.263 Uiso 1 1 calc R . . C40 C -0.0606(9) 0.7078(6) 1.0039(8) 0.171(6) Uani 1 1 d . . . H40A H -0.0299 0.7405 0.9854 0.256 Uiso 1 1 calc R . . H40B H -0.0330 0.7046 1.0495 0.256 Uiso 1 1 calc R . . H40C H -0.1309 0.7146 0.9987 0.256 Uiso 1 1 calc R . . C41 C 0.2164(6) 0.6138(3) 0.7076(3) 0.058(2) Uani 1 1 d . . . C42 C 0.1123(7) 0.6363(5) 0.7187(4) 0.099(3) Uani 1 1 d . . . H42A H 0.0715 0.6026 0.7249 0.148 Uiso 1 1 calc R . . H42B H 0.0810 0.6586 0.6813 0.148 Uiso 1 1 calc R . . H42C H 0.1207 0.6614 0.7565 0.148 Uiso 1 1 calc R . . C43 C 0.2051(8) 0.5664(4) 0.6541(3) 0.107(4) Uani 1 1 d . . . H43A H 0.2697 0.5546 0.6467 0.160 Uiso 1 1 calc R . . H43B H 0.1674 0.5827 0.6147 0.160 Uiso 1 1 calc R . . H43C H 0.1711 0.5323 0.6672 0.160 Uiso 1 1 calc R . . C44 C 0.2705(7) 0.6686(4) 0.6848(4) 0.102(3) Uani 1 1 d . . . H44A H 0.2862 0.6966 0.7200 0.154 Uiso 1 1 calc R . . H44B H 0.2281 0.6874 0.6489 0.154 Uiso 1 1 calc R . . H44C H 0.3308 0.6558 0.6714 0.154 Uiso 1 1 calc R . . C45 C 0.7777(6) 0.6186(3) 1.1913(4) 0.064(2) Uani 1 1 d . . . C46 C 0.7841(8) 0.5789(4) 1.2491(4) 0.095(3) Uani 1 1 d . . . H46A H 0.7756 0.6023 1.2863 0.143 Uiso 1 1 calc R . . H46B H 0.8480 0.5598 1.2575 0.143 Uiso 1 1 calc R . . H46C H 0.7329 0.5491 1.2408 0.143 Uiso 1 1 calc R . . C47 C 0.8630(8) 0.6574(5) 1.1876(5) 0.116(4) Uani 1 1 d . . . H47A H 0.8459 0.6848 1.1521 0.174 Uiso 1 1 calc R . . H47B H 0.9185 0.6334 1.1808 0.174 Uiso 1 1 calc R . . H47C H 0.8806 0.6793 1.2276 0.174 Uiso 1 1 calc R . . C48 C 0.5201(6) 0.6309(4) 1.2435(4) 0.069(2) Uani 1 1 d . . . C49 C 0.5323(8) 0.6951(4) 1.2286(5) 0.101(3) Uani 1 1 d . . . H49A H 0.5972 0.7083 1.2490 0.151 Uiso 1 1 calc R . . H49B H 0.4827 0.7182 1.2448 0.151 Uiso 1 1 calc R . . H49C H 0.5247 0.7004 1.1823 0.151 Uiso 1 1 calc R . . C50 C 0.5152(9) 0.6150(5) 1.3140(4) 0.130(4) Uani 1 1 d . . . H50A H 0.5222 0.5726 1.3199 0.195 Uiso 1 1 calc R . . H50B H 0.4523 0.6275 1.3237 0.195 Uiso 1 1 calc R . . H50C H 0.5679 0.6350 1.3426 0.195 Uiso 1 1 calc R . . C51 C 0.8739(8) 0.7849(4) 0.3690(5) 0.115(4) Uani 1 1 d . . . H51A H 0.9074 0.7734 0.4116 0.172 Uiso 1 1 calc R . . H51B H 0.8618 0.8272 0.3681 0.172 Uiso 1 1 calc R . . H51C H 0.9146 0.7750 0.3375 0.172 Uiso 1 1 calc R . . C52 C 0.7800(6) 0.7534(4) 0.3534(4) 0.063(2) Uani 1 1 d . . . C53 C 0.6989(8) 0.7750(4) 0.3863(4) 0.104(3) Uani 1 1 d . . . H53A H 0.6360 0.7614 0.3628 0.156 Uiso 1 1 calc R . . H53B H 0.6995 0.8179 0.3874 0.156 Uiso 1 1 calc R . . H53C H 0.7088 0.7597 0.4300 0.156 Uiso 1 1 calc R . . C54 C 0.7378(9) 0.4912(6) 0.7205(5) 0.136(4) Uani 1 1 d . . . H54A H 0.7093 0.5300 0.7103 0.203 Uiso 1 1 calc R . . H54B H 0.6887 0.4652 0.7331 0.203 Uiso 1 1 calc R . . H54C H 0.7598 0.4750 0.6829 0.203 Uiso 1 1 calc R . . C55 C 0.851(3) 0.4980(15) 0.7923(18) 0.43(3) Uani 1 1 d . . . C56 C 0.8196(10) 0.4597(4) 0.8485(4) 0.104(4) Uani 1 1 d . . . H56A H 0.8762 0.4380 0.8709 0.157 Uiso 1 1 calc R . . H56B H 0.7684 0.4320 0.8302 0.157 Uiso 1 1 calc R . . H56C H 0.7949 0.4857 0.8785 0.157 Uiso 1 1 calc R . . H1O H 0.561(6) 0.603(3) 1.005(4) 0.09(3) Uiso 1 1 d . . . H3O H 0.419(7) 0.595(4) 1.039(4) 0.10(3) Uiso 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 Li1 0.039(7) 0.044(6) 0.038(6) 0.006(5) -0.007(5) 0.009(5) Li2 0.055(8) 0.053(7) 0.037(6) 0.002(5) -0.009(6) 0.008(6) O1 0.052(3) 0.044(3) 0.035(2) 0.008(2) 0.011(2) 0.003(2) O2 0.041(3) 0.033(3) 0.041(2) 0.0045(19) -0.004(2) 0.007(2) O3 0.035(3) 0.046(3) 0.041(2) -0.003(2) -0.010(2) 0.009(2) O4 0.038(3) 0.043(3) 0.029(2) -0.0011(19) -0.006(2) 0.008(2) O5 0.058(4) 0.067(4) 0.067(3) -0.007(3) -0.014(3) 0.006(3) O6 0.084(4) 0.080(4) 0.048(3) -0.013(3) 0.002(3) 0.005(3) O7 0.101(5) 0.099(5) 0.100(4) -0.046(4) -0.005(4) 0.003(4) O8 0.257(14) 0.372(19) 0.344(17) -0.222(15) 0.218(14) -0.212(14) O9 2.00(16) 0.24(2) 0.73(6) -0.18(3) 0.95(9) -0.32(5) O10 1.16(11) 0.47(4) 0.96(9) 0.08(5) 0.84(10) -0.16(6) C1 0.031(4) 0.048(5) 0.045(4) 0.015(4) 0.003(3) 0.005(3) C2 0.029(4) 0.072(5) 0.043(4) 0.020(4) 0.004(3) 0.004(4) C3 0.036(5) 0.104(7) 0.052(5) 0.029(5) 0.001(4) -0.013(5) C4 0.045(5) 0.110(8) 0.059(6) 0.046(5) -0.014(4) -0.017(5) C5 0.038(5) 0.075(5) 0.081(6) 0.036(5) -0.011(4) -0.011(4) C6 0.036(4) 0.046(5) 0.057(4) 0.019(4) 0.000(4) 0.004(3) C7 0.035(4) 0.037(4) 0.075(5) 0.007(4) 0.000(4) -0.002(3) C8 0.039(5) 0.035(4) 0.053(4) -0.002(3) -0.009(4) -0.001(3) C9 0.036(4) 0.038(4) 0.035(4) -0.010(3) -0.010(3) 0.009(3) C10 0.044(5) 0.039(4) 0.033(3) -0.010(3) -0.011(3) 0.008(4) C11 0.043(5) 0.048(5) 0.059(4) -0.016(4) -0.014(4) 0.012(4) C12 0.051(5) 0.036(4) 0.065(5) -0.007(4) -0.019(4) 0.010(4) C13 0.060(6) 0.034(4) 0.068(5) 0.005(3) -0.016(4) 0.000(4) C14 0.044(4) 0.047(4) 0.033(3) -0.005(3) -0.003(3) 0.012(3) C15 0.033(4) 0.050(4) 0.026(3) 0.005(3) 0.001(3) 0.011(3) C16 0.028(4) 0.042(4) 0.031(3) 0.007(3) 0.000(3) 0.012(3) C17 0.036(5) 0.042(4) 0.027(3) 0.003(3) -0.002(3) 0.002(3) C18 0.032(4) 0.044(4) 0.043(4) 0.010(3) -0.009(3) 0.003(3) C19 0.033(4) 0.044(4) 0.044(4) 0.007(3) -0.001(3) 0.008(3) C20 0.045(5) 0.051(4) 0.036(4) 0.004(3) 0.001(4) 0.011(4) C21 0.031(4) 0.041(4) 0.035(3) 0.002(3) -0.008(3) 0.004(3) C22 0.029(4) 0.036(4) 0.032(3) -0.006(3) -0.013(3) 0.007(3) C23 0.037(4) 0.033(4) 0.027(3) 0.002(3) -0.009(3) 0.012(3) C24 0.034(4) 0.049(4) 0.026(3) -0.001(3) -0.007(3) 0.009(3) C25 0.058(6) 0.059(5) 0.031(4) 0.002(3) -0.001(4) -0.003(4) C26 0.039(5) 0.046(4) 0.035(4) 0.004(3) -0.016(4) 0.001(3) C27 0.038(4) 0.036(4) 0.042(4) -0.004(3) -0.012(4) 0.005(3) C28 0.047(5) 0.070(5) 0.032(4) 0.005(3) 0.001(3) 0.016(4) C29 0.100(9) 0.173(12) 0.084(7) 0.078(7) -0.010(7) -0.056(8) C30 0.44(3) 0.153(13) 0.114(9) 0.028(9) 0.068(14) -0.186(17) C31 0.127(12) 0.29(2) 0.203(15) 0.158(15) 0.082(12) 0.043(13) C32 0.094(8) 0.163(10) 0.091(7) 0.086(7) -0.006(6) 0.005(7) C33 0.067(6) 0.039(4) 0.094(6) -0.010(4) -0.027(5) 0.013(4) C34 0.084(8) 0.066(6) 0.150(9) 0.008(6) -0.039(7) 0.023(5) C35 0.208(15) 0.073(7) 0.148(10) -0.045(7) -0.060(10) 0.070(8) C36 0.124(11) 0.051(6) 0.260(15) 0.043(8) 0.027(10) 0.007(6) C37 0.034(5) 0.068(5) 0.073(5) -0.004(4) 0.001(4) 0.016(4) C38 0.090(10) 0.40(3) 0.112(10) 0.033(12) -0.028(8) 0.143(13) C39 0.056(8) 0.170(12) 0.307(19) 0.105(13) 0.049(10) 0.021(8) C40 0.070(8) 0.164(12) 0.267(16) -0.055(12) 0.002(9) 0.054(8) C41 0.064(6) 0.061(5) 0.038(4) 0.011(4) -0.017(4) 0.005(4) C42 0.076(7) 0.127(8) 0.076(6) 0.031(5) -0.032(5) 0.028(6) C43 0.155(10) 0.099(7) 0.041(4) -0.008(4) -0.049(6) 0.026(7) C44 0.104(8) 0.116(8) 0.069(6) 0.054(5) -0.034(6) -0.013(6) C45 0.053(6) 0.064(5) 0.066(5) -0.029(4) -0.012(5) 0.010(4) C46 0.125(9) 0.077(6) 0.067(6) -0.010(5) -0.031(6) 0.020(6) C47 0.074(7) 0.157(10) 0.115(8) -0.053(7) 0.010(6) -0.044(7) C48 0.062(6) 0.085(7) 0.055(5) -0.005(5) -0.004(4) 0.006(5) C49 0.096(8) 0.088(7) 0.104(7) -0.027(6) -0.021(6) -0.007(6) C50 0.154(11) 0.175(11) 0.064(6) -0.020(6) 0.029(7) -0.003(9) C51 0.087(8) 0.110(8) 0.123(8) 0.046(6) -0.048(7) -0.033(7) C52 0.070(6) 0.061(5) 0.049(4) -0.014(4) -0.015(4) 0.003(5) C53 0.135(10) 0.103(8) 0.070(6) -0.018(5) 0.005(6) 0.011(7) C54 0.119(10) 0.184(12) 0.102(8) -0.046(8) 0.017(7) 0.025(9) C55 0.41(4) 0.43(4) 0.54(5) -0.39(4) 0.28(4) -0.32(4) C56 0.195(11) 0.070(6) 0.061(5) 0.034(5) 0.055(7) -0.014(6) _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 Li1 O1 1.925(11) . ? Li1 O3 1.947(11) 3_667 ? Li1 O4 1.975(11) . ? Li1 O4 1.975(10) 3_667 ? Li1 Li1 2.39(2) 3_667 ? Li1 Li2 3.392(15) 3_667 ? Li1 Li2 3.400(14) . ? Li2 O2 1.923(11) . ? Li2 O5 1.938(13) . ? Li2 O4 1.983(11) 3_667 ? Li2 O6 1.999(12) . ? Li2 C23 2.535(12) 3_667 ? Li2 Li1 3.392(15) 3_667 ? O1 C1 1.376(7) . ? O2 C9 1.371(7) . ? O3 C16 1.381(7) . ? O3 Li1 1.947(11) 3_667 ? O4 C23 1.366(7) . ? O4 Li1 1.975(10) 3_667 ? O4 Li2 1.983(11) 3_667 ? O5 C45 1.237(8) . ? O6 C48 1.211(9) . ? O7 C52 1.213(8) . ? O8 C55 1.31(3) . ? C1 C6 1.400(9) . ? C1 C2 1.420(9) . ? C2 C3 1.382(9) . ? C2 C28 1.509(10) . ? C3 C4 1.390(11) . ? C4 C5 1.410(11) . ? C4 C29 1.563(11) . ? C5 C6 1.400(9) . ? C6 C7 1.538(9) . ? C7 C8 1.541(9) . ? C8 C13 1.399(9) . ? C8 C9 1.416(9) . ? C9 C10 1.419(9) . ? C10 C11 1.406(9) . ? C10 C14 1.514(9) . ? C11 C12 1.394(10) . ? C12 C13 1.391(10) . ? C12 C33 1.547(10) . ? C14 C15 1.543(9) . ? C15 C20 1.396(9) . ? C15 C16 1.400(8) . ? C16 C17 1.401(8) . ? C17 C18 1.397(8) . ? C17 C21 1.537(8) . ? C18 C19 1.402(9) . ? C19 C20 1.405(9) . ? C19 C37 1.526(9) . ? C21 C22 1.531(8) . ? C22 C23 1.405(8) . ? C22 C27 1.407(8) . ? C23 C24 1.422(8) . ? C23 Li2 2.535(12) 3_667 ? C24 C25 1.412(9) . ? C24 C28 1.530(9) . ? C25 C26 1.385(9) . ? C26 C27 1.393(9) . ? C26 C41 1.547(9) . ? C29 C30 1.421(16) . ? C29 C32 1.476(13) . ? C29 C31 1.748(18) . ? C33 C34 1.523(11) . ? C33 C36 1.524(14) . ? C33 C35 1.531(13) . ? C37 C38 1.468(13) . ? C37 C40 1.483(13) . ? C37 C39 1.523(13) . ? C41 C43 1.528(10) . ? C41 C44 1.552(11) . ? C41 C42 1.565(12) . ? C45 C47 1.467(12) . ? C45 C46 1.488(11) . ? C48 C49 1.487(12) . ? C48 C50 1.527(12) . ? C51 C52 1.450(11) . ? C52 C53 1.486(12) . ? C54 C55 1.96(4) . ? C55 C56 1.58(4) . ? 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 O1 Li1 O3 143.6(6) . 3_667 ? O1 Li1 O4 103.4(5) . . ? O3 Li1 O4 98.9(5) 3_667 . ? O1 Li1 O4 99.6(5) . 3_667 ? O3 Li1 O4 101.8(5) 3_667 3_667 ? O4 Li1 O4 105.5(5) . 3_667 ? O1 Li1 Li1 109.2(7) . 3_667 ? O3 Li1 Li1 107.2(7) 3_667 3_667 ? O4 Li1 Li1 52.7(4) . 3_667 ? O4 Li1 Li1 52.7(4) 3_667 3_667 ? O1 Li1 Li2 126.3(5) . 3_667 ? O3 Li1 Li2 68.2(4) 3_667 3_667 ? O4 Li1 Li2 31.1(3) . 3_667 ? O4 Li1 Li2 115.7(5) 3_667 3_667 ? Li1 Li1 Li2 69.6(5) 3_667 3_667 ? O1 Li1 Li2 69.0(4) . . ? O3 Li1 Li2 125.3(4) 3_667 . ? O4 Li1 Li2 115.4(5) . . ? O4 Li1 Li2 30.8(3) 3_667 . ? Li1 Li1 Li2 69.2(5) 3_667 . ? Li2 Li1 Li2 138.8(4) 3_667 . ? O2 Li2 O5 107.3(6) . . ? O2 Li2 O4 100.4(5) . 3_667 ? O5 Li2 O4 117.5(6) . 3_667 ? O2 Li2 O6 111.3(6) . . ? O5 Li2 O6 101.6(5) . . ? O4 Li2 O6 118.5(6) 3_667 . ? O2 Li2 C23 132.8(5) . 3_667 ? O5 Li2 C23 99.6(5) . 3_667 ? O4 Li2 C23 32.4(2) 3_667 3_667 ? O6 Li2 C23 100.0(5) . 3_667 ? O2 Li2 Li1 78.3(4) . 3_667 ? O5 Li2 Li1 145.8(5) . 3_667 ? O4 Li2 Li1 30.9(3) 3_667 3_667 ? O6 Li2 Li1 107.7(5) . 3_667 ? C23 Li2 Li1 58.5(3) 3_667 3_667 ? O2 Li2 Li1 77.5(4) . . ? O5 Li2 Li1 105.8(5) . . ? O4 Li2 Li1 30.7(3) 3_667 . ? O6 Li2 Li1 147.2(6) . . ? C23 Li2 Li1 58.0(3) 3_667 . ? Li1 Li2 Li1 41.2(4) 3_667 . ? C1 O1 Li1 139.3(5) . . ? C9 O2 Li2 141.0(5) . . ? C16 O3 Li1 138.8(5) . 3_667 ? C23 O4 Li1 126.2(5) . . ? C23 O4 Li1 124.8(4) . 3_667 ? Li1 O4 Li1 74.5(5) . 3_667 ? C23 O4 Li2 96.7(4) . 3_667 ? Li1 O4 Li2 118.0(5) . 3_667 ? Li1 O4 Li2 118.4(5) 3_667 3_667 ? C45 O5 Li2 144.7(6) . . ? C48 O6 Li2 132.6(7) . . ? O1 C1 C6 121.2(6) . . ? O1 C1 C2 117.5(6) . . ? C6 C1 C2 121.3(6) . . ? C3 C2 C1 118.3(7) . . ? C3 C2 C28 120.1(7) . . ? C1 C2 C28 121.4(6) . . ? C2 C3 C4 122.4(8) . . ? C3 C4 C5 118.0(7) . . ? C3 C4 C29 120.3(9) . . ? C5 C4 C29 121.7(9) . . ? C6 C5 C4 122.0(8) . . ? C5 C6 C1 117.9(7) . . ? C5 C6 C7 120.9(7) . . ? C1 C6 C7 121.2(6) . . ? C6 C7 C8 114.3(5) . . ? C13 C8 C9 118.6(6) . . ? C13 C8 C7 120.9(6) . . ? C9 C8 C7 120.5(5) . . ? O2 C9 C8 120.6(6) . . ? O2 C9 C10 119.4(6) . . ? C8 C9 C10 120.0(6) . . ? C11 C10 C9 117.9(6) . . ? C11 C10 C14 121.3(6) . . ? C9 C10 C14 120.8(6) . . ? C12 C11 C10 123.6(7) . . ? C13 C12 C11 116.5(6) . . ? C13 C12 C33 122.9(8) . . ? C11 C12 C33 120.6(7) . . ? C12 C13 C8 123.4(7) . . ? C10 C14 C15 116.6(5) . . ? C20 C15 C16 117.9(6) . . ? C20 C15 C14 121.3(6) . . ? C16 C15 C14 120.8(5) . . ? O3 C16 C15 121.3(5) . . ? O3 C16 C17 117.4(5) . . ? C15 C16 C17 121.2(6) . . ? C18 C17 C16 118.7(6) . . ? C18 C17 C21 120.9(6) . . ? C16 C17 C21 120.2(5) . . ? C17 C18 C19 122.4(6) . . ? C18 C19 C20 116.6(6) . . ? C18 C19 C37 120.6(6) . . ? C20 C19 C37 122.8(6) . . ? C15 C20 C19 123.2(6) . . ? C22 C21 C17 110.4(5) . . ? C23 C22 C27 119.4(6) . . ? C23 C22 C21 123.1(5) . . ? C27 C22 C21 117.5(6) . . ? O4 C23 C22 121.8(5) . . ? O4 C23 C24 119.8(5) . . ? C22 C23 C24 118.4(5) . . ? O4 C23 Li2 51.0(3) . 3_667 ? C22 C23 Li2 110.1(5) . 3_667 ? C24 C23 Li2 106.3(4) . 3_667 ? C25 C24 C23 118.5(6) . . ? C25 C24 C28 118.3(6) . . ? C23 C24 C28 123.2(5) . . ? C26 C25 C24 124.5(6) . . ? C25 C26 C27 114.9(6) . . ? C25 C26 C41 121.4(7) . . ? C27 C26 C41 123.6(6) . . ? C26 C27 C22 124.1(6) . . ? C2 C28 C24 111.5(5) . . ? C30 C29 C32 120.6(11) . . ? C30 C29 C4 115.2(10) . . ? C32 C29 C4 112.0(8) . . ? C30 C29 C31 98.1(13) . . ? C32 C29 C31 101.6(10) . . ? C4 C29 C31 105.9(9) . . ? C34 C33 C36 105.8(8) . . ? C34 C33 C35 109.6(8) . . ? C36 C33 C35 109.1(9) . . ? C34 C33 C12 111.0(6) . . ? C36 C33 C12 112.2(8) . . ? C35 C33 C12 109.0(7) . . ? C38 C37 C40 111.8(10) . . ? C38 C37 C39 106.8(11) . . ? C40 C37 C39 104.1(10) . . ? C38 C37 C19 111.0(7) . . ? C40 C37 C19 113.9(7) . . ? C39 C37 C19 108.7(7) . . ? C43 C41 C26 108.4(6) . . ? C43 C41 C44 108.4(7) . . ? C26 C41 C44 111.3(6) . . ? C43 C41 C42 110.8(7) . . ? C26 C41 C42 111.3(6) . . ? C44 C41 C42 106.7(7) . . ? O5 C45 C47 121.1(9) . . ? O5 C45 C46 121.3(8) . . ? C47 C45 C46 117.6(9) . . ? O6 C48 C49 122.8(7) . . ? O6 C48 C50 120.3(9) . . ? C49 C48 C50 116.9(9) . . ? O7 C52 C51 125.1(9) . . ? O7 C52 C53 118.7(8) . . ? C51 C52 C53 116.2(8) . . ? O8 C55 C56 129(4) . . ? O8 C55 C54 120(3) . . ? C56 C55 C54 104.0(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.699 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.094 #===END data_41 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Cl3 O4' _chemical_formula_weight 557.87 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2184(10) _cell_length_b 11.3149(8) _cell_length_c 16.9918(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.4050(10) _cell_angle_gamma 90.00 _cell_volume 2725.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description CUBIC _exptl_crystal_colour COLORLESS _exptl_crystal_size_max .46 _exptl_crystal_size_mid .41 _exptl_crystal_size_min .32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11264 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3558 _reflns_number_gt 2810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1379P)^2^+5.9339P] 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 SHELXL _refine_ls_extinction_coef 0.0011(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3558 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2633 _refine_ls_wR_factor_gt 0.2477 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.002 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 C1 C 0.2873(3) 0.5752(4) 0.1897(3) 0.0466(12) Uani 1 1 d . . . C2 C 0.2193(4) 0.5290(4) 0.1339(3) 0.0524(13) Uani 1 1 d . . . C3 C 0.2462(5) 0.4340(5) 0.0888(3) 0.0677(16) Uani 1 1 d . . . H3 H 0.2031 0.4018 0.0508 0.081 Uiso 1 1 calc R . . C4 C 0.3348(5) 0.3872(5) 0.0994(4) 0.0739(17) Uani 1 1 d . . . H4 H 0.3517 0.3248 0.0678 0.089 Uiso 1 1 calc R . . C5 C 0.3992(4) 0.4313(5) 0.1564(4) 0.0692(16) Uani 1 1 d . . . H5 H 0.4588 0.3972 0.1638 0.083 Uiso 1 1 calc R . . C6 C 0.3761(4) 0.5265(4) 0.2030(3) 0.0531(13) Uani 1 1 d . . . C7 C 0.2789(5) 0.7854(5) 0.2070(4) 0.0718(17) Uani 1 1 d . . . H7A H 0.3450 0.7951 0.2011 0.108 Uiso 1 1 calc R . . H7B H 0.2587 0.8431 0.2435 0.108 Uiso 1 1 calc R . . H7C H 0.2442 0.7958 0.1567 0.108 Uiso 1 1 calc R . . C8 C 0.1195(4) 0.5775(5) 0.1241(3) 0.0619(14) Uani 1 1 d . . . H8A H 0.1196 0.6581 0.1435 0.074 Uiso 1 1 calc R . . H8B H 0.0988 0.5792 0.0684 0.074 Uiso 1 1 calc R . . C9 C 0.0381(3) 0.5252(4) 0.2475(3) 0.0503(12) Uani 1 1 d . . . C10 C 0.0502(4) 0.5055(5) 0.1675(3) 0.0520(13) Uani 1 1 d . . . C11 C -0.0007(4) 0.4142(5) 0.1308(3) 0.0611(14) Uani 1 1 d . . . H11 H 0.0056 0.3992 0.0777 0.073 Uiso 1 1 calc R . . C12 C -0.0607(4) 0.3449(6) 0.1712(3) 0.0688(16) Uani 1 1 d . . . H12 H -0.0954 0.2853 0.1448 0.083 Uiso 1 1 calc R . . C13 C -0.0691(4) 0.3637(5) 0.2503(3) 0.0583(14) Uani 1 1 d . . . H13 H -0.1087 0.3156 0.2774 0.070 Uiso 1 1 calc R . . C14 C -0.0194(3) 0.4535(4) 0.2900(3) 0.0495(12) Uani 1 1 d . . . C15 C -0.0273(3) 0.4710(5) 0.3779(3) 0.0545(13) Uani 1 1 d . . . H15A H -0.0236 0.5548 0.3900 0.065 Uiso 1 1 calc R . . H15B H -0.0884 0.4428 0.3917 0.065 Uiso 1 1 calc R . . C16 C 0.1337(3) 0.4621(4) 0.4540(3) 0.0470(12) Uani 1 1 d . . . C17 C 0.0495(3) 0.4066(4) 0.4276(3) 0.0488(12) Uani 1 1 d . . . C18 C 0.0391(4) 0.2886(5) 0.4464(3) 0.0615(14) Uani 1 1 d . . . H18 H -0.0168 0.2498 0.4303 0.074 Uiso 1 1 calc R . . C19 C 0.1096(4) 0.2279(5) 0.4883(3) 0.0702(16) Uani 1 1 d . . . H19 H 0.1012 0.1485 0.5003 0.084 Uiso 1 1 calc R . . C20 C 0.1926(4) 0.2834(5) 0.5129(3) 0.0633(15) Uani 1 1 d . . . H20 H 0.2402 0.2410 0.5409 0.076 Uiso 1 1 calc R . . C21 C 0.2066(3) 0.4018(4) 0.4965(3) 0.0487(12) Uani 1 1 d . . . C22 C 0.2994(4) 0.4616(5) 0.5226(3) 0.0561(13) Uani 1 1 d . . . H22A H 0.2884 0.5455 0.5289 0.067 Uiso 1 1 calc R . . H22B H 0.3224 0.4303 0.5736 0.067 Uiso 1 1 calc R . . C23 C 0.3795(3) 0.5163(4) 0.3984(3) 0.0504(12) Uani 1 1 d . . . C24 C 0.3742(3) 0.4443(5) 0.4649(3) 0.0502(12) Uani 1 1 d . . . C25 C 0.4402(4) 0.3547(5) 0.4761(3) 0.0587(14) Uani 1 1 d . . . H25 H 0.4391 0.3067 0.5204 0.070 Uiso 1 1 calc R . . C26 C 0.5074(4) 0.3347(5) 0.4236(3) 0.0648(15) Uani 1 1 d . . . H26 H 0.5518 0.2750 0.4329 0.078 Uiso 1 1 calc R . . C27 C 0.5083(4) 0.4042(5) 0.3569(3) 0.0611(14) Uani 1 1 d . . . H27 H 0.5524 0.3889 0.3205 0.073 Uiso 1 1 calc R . . C28 C 0.4450(3) 0.4964(5) 0.3431(3) 0.0551(13) Uani 1 1 d . . . C29 C 0.4453(4) 0.5708(5) 0.2684(3) 0.0641(15) Uani 1 1 d . . . H29A H 0.4298 0.6519 0.2807 0.077 Uiso 1 1 calc R . . H29B H 0.5083 0.5703 0.2500 0.077 Uiso 1 1 calc R . . C30 C 0.2224(5) 0.4045(7) 0.8151(4) 0.093(2) Uani 1 1 d . . . H30 H 0.1613 0.4408 0.8231 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.2229(3) 0.3575(5) 0.72320(15) 0.271(3) Uani 1 1 d . . . Cl2 Cl 0.24341(19) 0.2866(3) 0.88188(15) 0.1361(10) Uani 1 1 d . . . Cl3 Cl 0.3102(3) 0.5049(4) 0.8353(5) 0.282(3) Uani 1 1 d . . . O1 O 0.2619(3) 0.6685(3) 0.23642(18) 0.0543(9) Uani 1 1 d . . . O2 O 0.0841(3) 0.6182(4) 0.2853(2) 0.0727(12) Uani 1 1 d . . . H2 H 0.1370 0.6248 0.2695 0.109 Uiso 1 1 calc R . . O3 O 0.1447(3) 0.5812(3) 0.4388(2) 0.0603(10) Uani 1 1 d . . . H3A H 0.1221 0.5962 0.3940 0.090 Uiso 1 1 calc R . . O4 O 0.3181(3) 0.6097(4) 0.3896(2) 0.0714(11) Uani 1 1 d . . . H4A H 0.3054 0.6225 0.3425 0.107 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 0.065(3) 0.036(3) 0.039(2) 0.005(2) 0.011(2) -0.003(2) C2 0.071(3) 0.048(3) 0.040(3) 0.007(2) 0.009(2) 0.000(2) C3 0.095(5) 0.061(3) 0.047(3) -0.006(3) 0.006(3) -0.008(3) C4 0.104(5) 0.054(3) 0.066(4) -0.010(3) 0.021(4) 0.009(3) C5 0.075(4) 0.064(4) 0.072(4) 0.007(3) 0.024(3) 0.013(3) C6 0.062(3) 0.050(3) 0.049(3) 0.006(2) 0.017(2) -0.004(2) C7 0.107(5) 0.039(3) 0.072(4) 0.007(3) 0.027(3) -0.004(3) C8 0.078(4) 0.065(3) 0.041(3) 0.012(2) -0.006(3) 0.003(3) C9 0.051(3) 0.051(3) 0.047(3) -0.003(2) -0.006(2) 0.004(2) C10 0.054(3) 0.060(3) 0.041(3) 0.003(2) -0.005(2) 0.012(2) C11 0.065(3) 0.072(4) 0.045(3) -0.010(3) -0.007(3) 0.003(3) C12 0.063(3) 0.079(4) 0.062(4) -0.020(3) -0.006(3) -0.007(3) C13 0.052(3) 0.066(3) 0.057(3) -0.008(3) 0.002(2) -0.003(3) C14 0.041(3) 0.058(3) 0.049(3) -0.007(2) -0.002(2) 0.010(2) C15 0.048(3) 0.067(3) 0.050(3) -0.008(2) 0.007(2) 0.002(2) C16 0.054(3) 0.051(3) 0.038(2) -0.007(2) 0.013(2) -0.001(2) C17 0.050(3) 0.057(3) 0.040(3) -0.008(2) 0.010(2) -0.004(2) C18 0.056(3) 0.071(4) 0.057(3) 0.001(3) 0.004(3) -0.015(3) C19 0.079(4) 0.060(3) 0.071(4) 0.014(3) 0.002(3) -0.014(3) C20 0.066(4) 0.068(4) 0.055(3) 0.012(3) 0.000(3) -0.002(3) C21 0.054(3) 0.058(3) 0.034(2) -0.003(2) 0.008(2) -0.002(2) C22 0.061(3) 0.067(3) 0.038(3) -0.004(2) -0.005(2) -0.006(3) C23 0.045(3) 0.056(3) 0.048(3) -0.001(2) -0.002(2) -0.005(2) C24 0.047(3) 0.057(3) 0.046(3) -0.005(2) -0.008(2) -0.009(2) C25 0.060(3) 0.061(3) 0.053(3) 0.001(3) -0.007(3) -0.009(3) C26 0.055(3) 0.062(3) 0.076(4) -0.002(3) -0.005(3) 0.004(3) C27 0.046(3) 0.071(4) 0.066(3) -0.008(3) 0.004(3) -0.003(3) C28 0.044(3) 0.064(3) 0.057(3) -0.002(2) 0.002(2) -0.011(2) C29 0.052(3) 0.075(4) 0.066(3) 0.009(3) 0.011(3) -0.013(3) C30 0.077(4) 0.113(6) 0.093(5) 0.008(4) 0.027(4) 0.029(4) Cl1 0.314(5) 0.420(7) 0.0779(16) -0.020(2) -0.004(2) 0.282(5) Cl2 0.137(2) 0.159(2) 0.1179(18) 0.0283(16) 0.0421(15) 0.0215(17) Cl3 0.153(3) 0.157(3) 0.550(10) -0.017(4) 0.122(5) -0.043(2) O1 0.080(2) 0.0393(19) 0.0458(19) 0.0016(15) 0.0191(17) -0.0030(16) O2 0.087(3) 0.075(3) 0.058(2) -0.016(2) 0.016(2) -0.026(2) O3 0.070(2) 0.047(2) 0.063(2) -0.0046(17) 0.0038(19) 0.0009(17) O4 0.076(3) 0.078(3) 0.062(2) 0.016(2) 0.015(2) 0.018(2) _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 C1 C6 1.381(7) . ? C1 O1 1.385(6) . ? C1 C2 1.401(7) . ? C2 C3 1.391(8) . ? C2 C8 1.519(8) . ? C3 C4 1.366(9) . ? C4 C5 1.374(9) . ? C5 C6 1.392(8) . ? C6 C29 1.512(8) . ? C7 O1 1.441(6) . ? C8 C10 1.513(7) . ? C9 O2 1.372(6) . ? C9 C14 1.393(7) . ? C9 C10 1.402(7) . ? C10 C11 1.382(7) . ? C11 C12 1.379(8) . ? C12 C13 1.376(8) . ? C13 C14 1.383(7) . ? C14 C15 1.520(7) . ? C15 C17 1.514(7) . ? C16 O3 1.383(6) . ? C16 C21 1.395(7) . ? C16 C17 1.396(7) . ? C17 C18 1.383(8) . ? C18 C19 1.369(8) . ? C19 C20 1.375(8) . ? C20 C21 1.385(7) . ? C21 C22 1.518(7) . ? C22 C24 1.515(7) . ? C23 O4 1.371(6) . ? C23 C28 1.392(7) . ? C23 C24 1.398(7) . ? C24 C25 1.384(7) . ? C25 C26 1.375(8) . ? C26 C27 1.380(8) . ? C27 C28 1.387(8) . ? C28 C29 1.524(8) . ? C30 Cl1 1.649(8) . ? C30 Cl3 1.704(9) . ? C30 Cl2 1.762(8) . ? 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 C6 C1 O1 119.1(4) . . ? C6 C1 C2 122.4(5) . . ? O1 C1 C2 118.4(4) . . ? C3 C2 C1 117.2(5) . . ? C3 C2 C8 120.9(5) . . ? C1 C2 C8 122.0(5) . . ? C4 C3 C2 121.1(6) . . ? C3 C4 C5 120.7(5) . . ? C4 C5 C6 120.5(6) . . ? C1 C6 C5 118.0(5) . . ? C1 C6 C29 121.6(5) . . ? C5 C6 C29 120.4(5) . . ? C10 C8 C2 113.0(4) . . ? O2 C9 C14 118.8(4) . . ? O2 C9 C10 119.1(5) . . ? C14 C9 C10 122.1(5) . . ? C11 C10 C9 117.2(5) . . ? C11 C10 C8 121.4(5) . . ? C9 C10 C8 121.3(5) . . ? C12 C11 C10 121.5(5) . . ? C13 C12 C11 120.1(5) . . ? C12 C13 C14 120.7(5) . . ? C13 C14 C9 118.3(5) . . ? C13 C14 C15 120.1(5) . . ? C9 C14 C15 121.6(4) . . ? C17 C15 C14 112.3(4) . . ? O3 C16 C21 118.9(4) . . ? O3 C16 C17 119.0(4) . . ? C21 C16 C17 122.1(5) . . ? C18 C17 C16 117.6(5) . . ? C18 C17 C15 120.6(5) . . ? C16 C17 C15 121.8(5) . . ? C19 C18 C17 121.2(5) . . ? C18 C19 C20 120.4(5) . . ? C19 C20 C21 121.0(5) . . ? C20 C21 C16 117.7(5) . . ? C20 C21 C22 120.5(5) . . ? C16 C21 C22 121.8(5) . . ? C24 C22 C21 113.0(4) . . ? O4 C23 C28 120.2(5) . . ? O4 C23 C24 117.7(4) . . ? C28 C23 C24 122.1(5) . . ? C25 C24 C23 117.4(5) . . ? C25 C24 C22 120.5(5) . . ? C23 C24 C22 122.1(5) . . ? C26 C25 C24 121.9(5) . . ? C25 C26 C27 119.3(5) . . ? C26 C27 C28 121.4(5) . . ? C27 C28 C23 117.9(5) . . ? C27 C28 C29 120.9(5) . . ? C23 C28 C29 121.3(5) . . ? C6 C29 C28 112.7(4) . . ? Cl1 C30 Cl3 110.5(5) . . ? Cl1 C30 Cl2 110.7(5) . . ? Cl3 C30 Cl2 106.8(5) . . ? C1 O1 C7 116.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.019 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.069 #===END