# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/420 data_1a _publ_contact_author_name ' Maarten B. Dinger and Michael J. Scott' _publ_contact_author_address ; Department of Chemistry University of Florida P.O. Box 117200 Gainesville, FL 32611-7200 ; _publ_requested_journal 'Perkin Transactions 1' _publ_section_title ; Hydroxy-substituted triarylcarbenium bromides. Synthesis, structure, derivatization and facile conversion to highly substituted xanthenes. ; _audit_creation_method SHELXL-97 _diffrn_measurement_device_type 'Siemens SMART CCD' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 O3' _chemical_formula_weight 502.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 22.3915(7) _cell_length_b 22.3915(7) _cell_length_c 10.4686(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4545.5(3) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.82 _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_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28036 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 26.36 _reflns_number_total 6209 _reflns_number_gt 4116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SMART ' _computing_data_reduction 'Bruker AXS SMART ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. The unit cell contains three independent molecules of 1a. The central carbon [C(1)] of each molecule resides on a 3-fold position. All phenolic hydrogens were located in the electron difference maps, and allowed to refine without constraint. The hydrogen bonds are tabulated below. Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A) 2sigma(I) _computing_data_collection ' Bruker AXS Smart ' _computing_cell_refinement ' Bruker AXS Smart ' _computing_data_reduction 'Bruker AXS Smart ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. Residual density associated with highly disordered solvents was located. These corresponded to two half site-occupancy chloroforms which were subsequently removed with the Platon for Windows software program (A. L. Spek, Acta Cryst., Sect. A, 1990, 46, C-34). ; _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^)+(0.0863P)^2^+11.6071P] 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 0.48(2) _refine_ls_number_reflns 6266 _refine_ls_number_parameters 368 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1973 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.154 _refine_ls_shift/su_mean 0.009 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 Br1 Br 1.24136(4) 0.29080(4) -0.97541(8) 0.0369(2) Uani 1 1 d . . . O1 O 1.3783(3) 0.3210(3) -1.1489(7) 0.0472(15) Uani 1 1 d D . . H1 H 1.3331(14) 0.326(6) -1.159(12) 0.08(4) Uiso 1 1 d D . . O2 O 1.3068(4) 0.1514(3) -0.8767(6) 0.0475(15) Uani 1 1 d D . . H2 H 1.274(5) 0.183(7) -0.860(16) 0.21(10) Uiso 1 1 d D . . O3 O 1.1863(3) 0.2108(4) -1.2434(6) 0.0474(13) Uani 1 1 d D . . H3 H 1.186(4) 0.181(4) -1.178(8) 0.09(4) Uiso 1 1 d D . . C1 C 1.3300(4) 0.1801(4) -1.1754(9) 0.0358(18) Uani 1 1 d . . . C2 C 1.3979(4) 0.1998(4) -1.1075(8) 0.0374(17) Uani 1 1 d . . . C3 C 1.4194(4) 0.2700(4) -1.1067(8) 0.0355(18) Uani 1 1 d . . . C4 C 1.4869(4) 0.2872(5) -1.0530(8) 0.045(2) Uani 1 1 d . . . C5 C 1.5103(4) 0.3619(4) -1.0398(10) 0.0433(19) Uani 1 1 d . . . C6 C 1.5845(5) 0.3682(5) -0.9864(12) 0.068(3) Uani 1 1 d . . . H6A H 1.5899 0.3406 -0.9015 0.102 Uiso 1 1 calc R . . H6B H 1.5946 0.4165 -0.9651 0.102 Uiso 1 1 calc R . . H6C H 1.6172 0.3518 -1.0581 0.102 Uiso 1 1 calc R . . C7 C 1.4582(5) 0.3989(4) -0.9400(9) 0.056(2) Uani 1 1 d . . . H7A H 1.4546 0.3732 -0.8522 0.083 Uiso 1 1 calc R . . H7B H 1.4120 0.4014 -0.9843 0.083 Uiso 1 1 calc R . . H7C H 1.4752 0.4455 -0.9206 0.083 Uiso 1 1 calc R . . C8 C 1.5082(5) 0.3975(4) -1.1860(9) 0.045(2) Uani 1 1 d . . . H8A H 1.5435 0.3767 -1.2472 0.068 Uiso 1 1 calc R . . H8B H 1.5181 0.4466 -1.1751 0.068 Uiso 1 1 calc R . . H8C H 1.4617 0.3915 -1.2275 0.068 Uiso 1 1 calc R . . C9 C 1.5288(4) 0.2314(4) -1.0029(10) 0.047(2) Uani 1 1 d . . . H9A H 1.5737 0.2412 -0.9647 0.056 Uiso 1 1 calc R . . C10 C 1.5066(4) 0.1641(4) -1.0079(9) 0.041(2) Uani 1 1 d . . . C11 C 1.5545(6) 0.1070(5) -0.9516(14) 0.073(3) Uani 1 1 d . . . H11A H 1.5628 0.0730 -1.0254 0.109 Uiso 1 1 calc R . . H11B H 1.5319 0.0846 -0.8716 0.109 Uiso 1 1 calc R . . H11C H 1.5992 0.1269 -0.9219 0.109 Uiso 1 1 calc R . . C12 C 1.4413(4) 0.1477(4) -1.0554(8) 0.0378(19) Uani 1 1 d . . . H12A H 1.4254 0.1015 -1.0530 0.045 Uiso 1 1 calc R . . C13 C 1.2927(4) 0.1186(4) -1.1175(8) 0.0373(18) Uani 1 1 d . . . C14 C 1.2905(4) 0.1024(3) -0.9790(8) 0.0354(16) Uani 1 1 d D . . C15 C 1.2673(5) 0.0383(3) -0.9291(8) 0.0373(18) Uani 1 1 d . . . C16 C 1.2638(5) 0.0209(4) -0.7748(8) 0.0399(19) Uani 1 1 d . . . C17 C 1.2409(6) -0.0534(3) -0.7509(8) 0.048(2) Uani 1 1 d . . . H17A H 1.1920 -0.0588 -0.7796 0.072 Uiso 1 1 calc R . . H17B H 1.2456 -0.0648 -0.6515 0.072 Uiso 1 1 calc R . . H17C H 1.2706 -0.0841 -0.8063 0.072 Uiso 1 1 calc R . . C18 C 1.3370(5) 0.0277(5) -0.7069(10) 0.054(2) Uani 1 1 d . . . H18A H 1.3717 0.0041 -0.7652 0.080 Uiso 1 1 calc R . . H18B H 1.3362 0.0069 -0.6136 0.080 Uiso 1 1 calc R . . H18C H 1.3494 0.0764 -0.6991 0.080 Uiso 1 1 calc R . . C19 C 1.2115(5) 0.0675(4) -0.6980(9) 0.046(2) Uani 1 1 d . . . H19A H 1.1636 0.0525 -0.7190 0.070 Uiso 1 1 calc R . . H19B H 1.2178 0.1151 -0.7291 0.070 Uiso 1 1 calc R . . H19C H 1.2197 0.0646 -0.5970 0.070 Uiso 1 1 calc R . . C20 C 1.2461(4) -0.0076(4) -1.0326(8) 0.0394(16) Uani 1 1 d . . . H20A H 1.2304 -0.0517 -1.0039 0.047 Uiso 1 1 calc R . . C21 C 1.2463(6) 0.0069(4) -1.1761(8) 0.056(3) Uani 1 1 d . . . C22 C 1.2280(9) -0.0495(5) -1.2826(9) 0.095(6) Uani 1 1 d . . . H22A H 1.1871 -0.0352 -1.3375 0.142 Uiso 1 1 calc R . . H22B H 1.2171 -0.0922 -1.2330 0.142 Uiso 1 1 calc R . . H22C H 1.2679 -0.0570 -1.3452 0.142 Uiso 1 1 calc R . . C23 C 1.2706(5) 0.0712(4) -1.2182(8) 0.044(2) Uani 1 1 d . . . H23A H 1.2721 0.0828 -1.3146 0.053 Uiso 1 1 calc R . . C24 C 1.3083(4) 0.2104(5) -1.3011(10) 0.046(2) Uani 1 1 d . . . C25 C 1.2380(4) 0.2209(3) -1.3364(7) 0.0311(15) Uani 1 1 d D . . C26 C 1.2167(4) 0.2435(4) -1.4716(9) 0.0395(17) Uani 1 1 d . . . C27 C 1.1401(4) 0.2553(4) -1.5032(8) 0.0400(19) Uani 1 1 d . . . C28 C 1.1270(5) 0.2781(5) -1.6572(10) 0.057(3) Uani 1 1 d . . . H28A H 1.1465 0.2436 -1.7210 0.086 Uiso 1 1 calc R . . H28B H 1.1499 0.3224 -1.6738 0.086 Uiso 1 1 calc R . . H28C H 1.0766 0.2825 -1.6735 0.086 Uiso 1 1 calc R . . C29 C 1.0960(5) 0.1918(5) -1.4803(10) 0.058(2) Uani 1 1 d . . . H29A H 1.1191 0.1521 -1.5234 0.086 Uiso 1 1 calc R . . H29B H 1.0498 0.1985 -1.5228 0.086 Uiso 1 1 calc R . . H29C H 1.0906 0.1837 -1.3797 0.086 Uiso 1 1 calc R . . C30 C 1.1099(5) 0.3154(5) -1.4096(10) 0.055(2) Uani 1 1 d . . . H30A H 1.1143 0.3031 -1.3106 0.083 Uiso 1 1 calc R . . H30B H 1.0605 0.3229 -1.4325 0.083 Uiso 1 1 calc R . . H30C H 1.1364 0.3577 -1.4277 0.083 Uiso 1 1 calc R . . C31 C 1.2676(5) 0.2551(4) -1.5676(7) 0.0416(19) Uani 1 1 d . . . H31A H 1.2542 0.2689 -1.6591 0.050 Uiso 1 1 calc R . . C32 C 1.3404(4) 0.2475(4) -1.5372(9) 0.0405(19) Uani 1 1 d . . . C33 C 1.3929(6) 0.2572(6) -1.6536(9) 0.061(3) Uani 1 1 d . . . H33A H 1.4404 0.2562 -1.6148 0.091 Uiso 1 1 calc R . . H33B H 1.3847 0.3016 -1.6992 0.091 Uiso 1 1 calc R . . H33C H 1.3876 0.2202 -1.7222 0.091 Uiso 1 1 calc R . . C34 C 1.3597(4) 0.2257(4) -1.4079(8) 0.0399(19) Uani 1 1 d . . . H34A H 1.4080 0.2204 -1.3871 0.048 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 Br1 0.0467(4) 0.0309(3) 0.0330(3) 0.0004(3) 0.0072(3) 0.0053(3) O1 0.049(4) 0.027(3) 0.066(4) 0.013(3) -0.008(3) 0.002(3) O2 0.083(5) 0.030(3) 0.030(3) 0.001(2) -0.002(3) -0.012(3) O3 0.043(3) 0.050(3) 0.049(3) 0.009(4) 0.004(2) 0.003(3) C1 0.036(4) 0.030(4) 0.042(5) -0.002(3) 0.002(3) -0.007(3) C2 0.053(5) 0.030(4) 0.030(4) -0.006(3) 0.004(3) -0.005(3) C3 0.043(4) 0.026(4) 0.038(4) 0.007(3) -0.012(4) 0.002(3) C4 0.054(5) 0.044(4) 0.037(5) -0.004(4) -0.008(4) 0.024(4) C5 0.053(5) 0.035(4) 0.042(5) -0.010(4) -0.008(4) 0.005(3) C6 0.081(7) 0.052(5) 0.070(7) -0.013(5) -0.022(6) 0.008(5) C7 0.092(7) 0.035(4) 0.040(5) -0.010(4) 0.006(5) 0.006(4) C8 0.061(5) 0.034(4) 0.042(5) 0.004(4) 0.010(4) 0.006(4) C9 0.042(4) 0.044(4) 0.054(6) -0.012(4) -0.023(4) 0.015(3) C10 0.046(4) 0.034(4) 0.042(5) -0.009(4) -0.014(4) 0.009(3) C11 0.077(7) 0.041(5) 0.099(9) 0.016(6) -0.038(7) 0.016(5) C12 0.050(5) 0.029(4) 0.035(5) 0.013(3) -0.007(4) 0.008(3) C13 0.051(5) 0.035(4) 0.026(4) 0.008(3) -0.001(3) 0.001(4) C14 0.069(5) 0.015(3) 0.023(3) 0.001(3) 0.003(4) 0.006(3) C15 0.050(5) 0.024(3) 0.037(4) 0.002(3) 0.004(4) 0.009(3) C16 0.060(5) 0.028(4) 0.033(4) 0.005(3) 0.006(4) 0.012(4) C17 0.081(7) 0.021(3) 0.042(4) 0.002(3) 0.005(5) -0.011(4) C18 0.064(6) 0.039(5) 0.057(6) 0.003(4) -0.011(5) 0.004(4) C19 0.053(5) 0.042(4) 0.045(5) -0.003(4) 0.012(4) 0.017(4) C20 0.053(4) 0.035(3) 0.030(3) 0.000(3) -0.008(4) -0.005(3) C21 0.110(8) 0.028(4) 0.031(4) -0.004(3) -0.002(5) -0.042(5) C22 0.215(17) 0.048(5) 0.022(4) -0.011(4) -0.020(7) -0.060(8) C23 0.076(6) 0.031(4) 0.024(4) 0.001(3) -0.008(4) -0.005(4) C24 0.035(4) 0.033(4) 0.072(6) 0.002(5) -0.003(4) -0.012(4) C25 0.043(4) 0.024(3) 0.026(3) 0.003(3) -0.003(3) 0.011(3) C26 0.047(4) 0.034(4) 0.038(4) -0.009(4) 0.008(4) -0.004(3) C27 0.051(4) 0.042(4) 0.027(5) -0.003(4) -0.008(3) 0.002(3) C28 0.053(5) 0.057(6) 0.061(6) 0.004(5) -0.025(4) 0.011(4) C29 0.065(5) 0.071(6) 0.038(5) -0.010(5) -0.010(5) -0.008(4) C30 0.065(6) 0.048(5) 0.053(6) -0.004(4) -0.002(5) 0.022(4) C31 0.069(6) 0.033(4) 0.023(4) 0.001(3) -0.007(4) -0.007(4) C32 0.034(4) 0.052(5) 0.036(4) 0.006(4) 0.014(4) 0.007(3) C33 0.084(7) 0.073(6) 0.025(4) 0.014(4) 0.006(5) -0.017(6) C34 0.043(4) 0.041(5) 0.036(4) 0.008(4) 0.002(3) -0.003(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 O1 C3 1.328(9) . ? O2 C14 1.402(9) . ? O3 C25 1.344(9) . ? C1 C24 1.402(12) . ? C1 C13 1.499(10) . ? C1 C2 1.500(11) . ? C2 C12 1.400(10) . ? C2 C3 1.427(10) . ? C3 C4 1.426(11) . ? C4 C9 1.432(11) . ? C4 C5 1.525(12) . ? C5 C6 1.511(12) . ? C5 C7 1.556(12) . ? C5 C8 1.560(12) . ? C9 C10 1.378(11) . ? C10 C12 1.365(11) . ? C10 C11 1.535(10) . ? C13 C14 1.362(11) . ? C13 C23 1.398(11) . ? C14 C15 1.406(10) . ? C15 C20 1.394(10) . ? C15 C16 1.515(11) . ? C16 C17 1.527(10) . ? C16 C19 1.535(11) . ? C16 C18 1.547(13) . ? C20 C21 1.402(10) . ? C21 C23 1.394(10) . ? C21 C22 1.537(10) . ? C24 C25 1.397(11) . ? C24 C34 1.447(12) . ? C25 C26 1.426(11) . ? C26 C31 1.355(11) . ? C26 C27 1.510(11) . ? C27 C29 1.510(11) . ? C27 C28 1.558(12) . ? C27 C30 1.583(11) . ? C31 C32 1.427(12) . ? C32 C34 1.358(11) . ? C32 C33 1.509(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 C24 C1 C13 120.8(7) . . ? C24 C1 C2 121.3(7) . . ? C13 C1 C2 117.1(7) . . ? C12 C2 C3 121.4(7) . . ? C12 C2 C1 118.7(7) . . ? C3 C2 C1 119.7(7) . . ? O1 C3 C2 123.0(7) . . ? O1 C3 C4 117.9(6) . . ? C2 C3 C4 119.1(7) . . ? C3 C4 C9 116.6(8) . . ? C3 C4 C5 121.2(7) . . ? C9 C4 C5 122.0(7) . . ? C6 C5 C4 112.4(7) . . ? C6 C5 C7 110.7(8) . . ? C4 C5 C7 107.8(7) . . ? C6 C5 C8 106.9(8) . . ? C4 C5 C8 110.0(7) . . ? C7 C5 C8 109.1(7) . . ? C10 C9 C4 122.5(7) . . ? C12 C10 C9 120.9(7) . . ? C12 C10 C11 119.4(7) . . ? C9 C10 C11 119.6(7) . . ? C10 C12 C2 119.3(7) . . ? C14 C13 C23 120.5(7) . . ? C14 C13 C1 124.0(7) . . ? C23 C13 C1 114.6(7) . . ? C13 C14 O2 120.9(6) . . ? C13 C14 C15 123.0(7) . . ? O2 C14 C15 115.9(6) . . ? C20 C15 C14 114.8(7) . . ? C20 C15 C16 122.3(7) . . ? C14 C15 C16 122.9(7) . . ? C15 C16 C17 111.7(6) . . ? C15 C16 C19 111.3(7) . . ? C17 C16 C19 107.6(7) . . ? C15 C16 C18 110.4(7) . . ? C17 C16 C18 106.0(7) . . ? C19 C16 C18 109.7(7) . . ? C15 C20 C21 124.4(7) . . ? C23 C21 C20 117.7(7) . . ? C23 C21 C22 121.7(7) . . ? C20 C21 C22 120.2(7) . . ? C21 C23 C13 119.6(7) . . ? C25 C24 C1 123.5(7) . . ? C25 C24 C34 116.7(7) . . ? C1 C24 C34 119.4(7) . . ? O3 C25 C24 121.6(6) . . ? O3 C25 C26 115.8(6) . . ? C24 C25 C26 122.6(7) . . ? C31 C26 C25 117.4(7) . . ? C31 C26 C27 122.3(8) . . ? C25 C26 C27 120.3(7) . . ? C26 C27 C29 112.7(7) . . ? C26 C27 C28 112.8(7) . . ? C29 C27 C28 106.3(7) . . ? C26 C27 C30 110.6(7) . . ? C29 C27 C30 108.7(7) . . ? C28 C27 C30 105.4(7) . . ? C26 C31 C32 122.9(7) . . ? C34 C32 C31 118.8(7) . . ? C34 C32 C33 122.0(7) . . ? C31 C32 C33 118.9(8) . . ? C32 C34 C24 121.5(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.980 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.108 #===END data_3a.CH2Cl2 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H45 Br Cl2 O2' _chemical_formula_weight 648.52 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 9.3103(5) _cell_length_b 12.5249(7) _cell_length_c 28.9201(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3372.4(3) _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 'thin flake' _exptl_crystal_colour 'dark orange ' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.66 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18656 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5935 _reflns_number_gt 5060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Smart ' _computing_cell_refinement ' Bruker AXS Smart ' _computing_data_reduction 'Bruker AXS Smart ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. Residual density associated with highly a disordered solvent was located. This corresponded to one full site-occupancy chloroform solvent which was subsequently removed with the Platon for Windows software program (A. L. Spek, Acta Cryst., Sect. A, 1990, 46, C-34). ; _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^)+(0.0552P)^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 0.017(10) _refine_ls_number_reflns 5935 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Br1 Br -0.99054(4) -0.81404(3) -0.163654(15) 0.03877(13) Uani 1 1 d . . . O1 O -1.1717(3) -1.0048(2) -0.12219(10) 0.0352(7) Uani 1 1 d . . . H1 H -1.139(6) -0.951(4) -0.1317(19) 0.068(18) Uiso 1 1 d . . . C1 C -1.3594(3) -0.8516(3) -0.16732(13) 0.0221(8) Uani 1 1 d . . . O2 O -1.2879(3) -0.71253(17) -0.23804(8) 0.0209(5) Uani 1 1 d . . . C2 C -1.4052(4) -0.9254(3) -0.12964(12) 0.0217(8) Uani 1 1 d . . . C3 C -1.3113(4) -0.9969(3) -0.10846(13) 0.0239(8) Uani 1 1 d . . . C4 C -1.3587(4) -1.0639(3) -0.07281(12) 0.0232(8) Uani 1 1 d . . . C5 C -1.2562(4) -1.1426(3) -0.04859(13) 0.0285(9) Uani 1 1 d . . . C6 C -1.1942(5) -1.2214(3) -0.08399(15) 0.0447(11) Uani 1 1 d . . . H6A H -1.2725 -1.2626 -0.0979 0.067 Uiso 1 1 calc R . . H6B H -1.1273 -1.2700 -0.0685 0.067 Uiso 1 1 calc R . . H6C H -1.1432 -1.1818 -0.1082 0.067 Uiso 1 1 calc R . . C7 C -1.3332(5) -1.2094(3) -0.01232(15) 0.0472(12) Uani 1 1 d . . . H7A H -1.3715 -1.1625 0.0118 0.071 Uiso 1 1 calc R . . H7B H -1.2655 -1.2601 0.0015 0.071 Uiso 1 1 calc R . . H7C H -1.4123 -1.2486 -0.0269 0.071 Uiso 1 1 calc R . . C8 C -1.1374(5) -1.0798(4) -0.02430(17) 0.0482(12) Uani 1 1 d . . . H8A H -1.1797 -1.0342 -0.0004 0.072 Uiso 1 1 calc R . . H8B H -1.0869 -1.0352 -0.0469 0.072 Uiso 1 1 calc R . . H8C H -1.0693 -1.1296 -0.0100 0.072 Uiso 1 1 calc R . . C9 C -1.5031(4) -1.0552(3) -0.05986(11) 0.0270(7) Uani 1 1 d . . . H9A H -1.5370 -1.1001 -0.0358 0.032 Uiso 1 1 calc R . . C10 C -1.5998(4) -0.9848(3) -0.08010(13) 0.0268(9) Uani 1 1 d . . . C11 C -1.7549(4) -0.9793(3) -0.06519(15) 0.0382(10) Uani 1 1 d . . . H11A H -1.8157 -0.9658 -0.0922 0.057 Uiso 1 1 calc R . . H11B H -1.7670 -0.9214 -0.0428 0.057 Uiso 1 1 calc R . . H11C H -1.7826 -1.0472 -0.0509 0.057 Uiso 1 1 calc R . . C12 C -1.5487(4) -0.9194(3) -0.11516(12) 0.0227(8) Uani 1 1 d . . . H12A H -1.6118 -0.8699 -0.1295 0.027 Uiso 1 1 calc R . . C13 C -1.3517(4) -0.7419(3) -0.15889(13) 0.0239(8) Uani 1 1 d . . . C14 C -1.3037(4) -0.6737(3) -0.19443(12) 0.0221(8) Uani 1 1 d . . . C15 C -1.2712(4) -0.5642(3) -0.18625(13) 0.0258(8) Uani 1 1 d . . . C16 C -1.1949(4) -0.4921(3) -0.22123(14) 0.0294(9) Uani 1 1 d . . . C17 C -1.0510(4) -0.5426(3) -0.23490(16) 0.0367(10) Uani 1 1 d . . . H17A H -1.0667 -0.6167 -0.2446 0.055 Uiso 1 1 calc R . . H17B H -0.9856 -0.5412 -0.2084 0.055 Uiso 1 1 calc R . . H17C H -1.0086 -0.5023 -0.2605 0.055 Uiso 1 1 calc R . . C18 C -1.1582(5) -0.3821(3) -0.20016(15) 0.0401(10) Uani 1 1 d . . . H18A H -1.0975 -0.3920 -0.1728 0.060 Uiso 1 1 calc R . . H18B H -1.2471 -0.3456 -0.1912 0.060 Uiso 1 1 calc R . . H18C H -1.1069 -0.3389 -0.2231 0.060 Uiso 1 1 calc R . . C19 C -1.2921(4) -0.4710(3) -0.26344(14) 0.0309(9) Uani 1 1 d . . . H19A H -1.3185 -0.5390 -0.2778 0.046 Uiso 1 1 calc R . . H19B H -1.2405 -0.4267 -0.2859 0.046 Uiso 1 1 calc R . . H19C H -1.3793 -0.4337 -0.2534 0.046 Uiso 1 1 calc R . . C20 C -1.3043(5) -0.5284(3) -0.14270(14) 0.0344(10) Uani 1 1 d . . . H20A H -1.2881 -0.4550 -0.1363 0.041 Uiso 1 1 calc R . . C21 C -1.3608(5) -0.5919(3) -0.10644(14) 0.0362(10) Uani 1 1 d . . . C22 C -1.3947(6) -0.5406(4) -0.06039(15) 0.0559(14) Uani 1 1 d . . . H22A H -1.4374 -0.5939 -0.0397 0.084 Uiso 1 1 calc R . . H22B H -1.4627 -0.4818 -0.0650 0.084 Uiso 1 1 calc R . . H22C H -1.3061 -0.5129 -0.0466 0.084 Uiso 1 1 calc R . . C23 C -1.3812(4) -0.6980(3) -0.11436(13) 0.0301(9) Uani 1 1 d . . . H23A H -1.4151 -0.7428 -0.0902 0.036 Uiso 1 1 calc R . . C24 C -1.3271(4) -0.8915(3) -0.21160(12) 0.0199(8) Uani 1 1 d . . . C25 C -1.3037(4) -0.8175(3) -0.24760(12) 0.0235(8) Uani 1 1 d . . . C26 C -1.3007(4) -0.8512(3) -0.29461(12) 0.0247(8) Uani 1 1 d . . . C27 C -1.3053(4) -0.7715(3) -0.33558(14) 0.0328(9) Uani 1 1 d . . . C28 C -1.4434(4) -0.7055(3) -0.33089(14) 0.0332(9) Uani 1 1 d . . . H28A H -1.4434 -0.6484 -0.3541 0.050 Uiso 1 1 calc R . . H28B H -1.4480 -0.6742 -0.2999 0.050 Uiso 1 1 calc R . . H28C H -1.5269 -0.7518 -0.3358 0.050 Uiso 1 1 calc R . . C29 C -1.1720(4) -0.7013(3) -0.33698(16) 0.0446(11) Uani 1 1 d . . . H29A H -1.0865 -0.7462 -0.3404 0.067 Uiso 1 1 calc R . . H29B H -1.1651 -0.6604 -0.3082 0.067 Uiso 1 1 calc R . . H29C H -1.1786 -0.6521 -0.3632 0.067 Uiso 1 1 calc R . . C30 C -1.3146(7) -0.8305(4) -0.38183(14) 0.0587(15) Uani 1 1 d . . . H30A H -1.2288 -0.8747 -0.3860 0.088 Uiso 1 1 calc R . . H30B H -1.3209 -0.7785 -0.4071 0.088 Uiso 1 1 calc R . . H30C H -1.4002 -0.8761 -0.3821 0.088 Uiso 1 1 calc R . . C31 C -1.3052(4) -0.9587(3) -0.30174(13) 0.0283(8) Uani 1 1 d . . . H31A H -1.3015 -0.9833 -0.3328 0.034 Uiso 1 1 calc R . . C32 C -1.3150(4) -1.0371(3) -0.26613(13) 0.0251(8) Uani 1 1 d . . . C33 C -1.3145(5) -1.1536(3) -0.27912(15) 0.0342(10) Uani 1 1 d . . . H33A H -1.3537 -1.1958 -0.2535 0.051 Uiso 1 1 calc R . . H33B H -1.2157 -1.1764 -0.2855 0.051 Uiso 1 1 calc R . . H33C H -1.3735 -1.1642 -0.3068 0.051 Uiso 1 1 calc R . . C34 C -1.3306(4) -1.0026(3) -0.22210(13) 0.0263(9) Uani 1 1 d . . . H34A H -1.3440 -1.0530 -0.1979 0.032 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 Br1 0.02610(19) 0.0375(2) 0.0527(2) 0.0072(2) 0.0054(2) -0.00265(19) O1 0.0233(14) 0.0372(16) 0.0452(18) 0.0156(15) 0.0037(13) 0.0004(12) C1 0.0167(17) 0.0258(17) 0.0239(19) 0.0041(17) -0.0038(17) 0.0014(13) O2 0.0222(13) 0.0185(13) 0.0221(13) 0.0026(10) 0.0024(10) 0.0012(10) C2 0.0249(19) 0.0256(19) 0.0144(18) 0.0020(16) 0.0014(15) -0.0014(16) C3 0.0209(19) 0.0265(19) 0.024(2) 0.0018(17) -0.0016(16) -0.0020(16) C4 0.0222(19) 0.0251(18) 0.022(2) -0.0018(16) -0.0037(16) -0.0013(15) C5 0.036(2) 0.0277(19) 0.022(2) 0.0046(16) -0.0052(17) -0.0017(17) C6 0.053(3) 0.038(2) 0.043(3) 0.011(2) 0.006(2) 0.011(2) C7 0.055(3) 0.046(3) 0.041(2) 0.024(2) -0.002(2) 0.002(2) C8 0.043(3) 0.052(3) 0.050(3) 0.010(2) -0.020(2) -0.004(2) C9 0.033(2) 0.0272(16) 0.0208(18) 0.0023(14) 0.006(2) -0.007(2) C10 0.026(2) 0.033(2) 0.022(2) -0.0025(17) 0.0068(16) -0.0013(16) C11 0.029(2) 0.047(3) 0.039(2) 0.007(2) 0.0101(19) 0.0025(19) C12 0.0247(19) 0.0220(18) 0.0213(19) 0.0015(16) -0.0006(15) 0.0038(14) C13 0.0170(17) 0.0328(18) 0.0217(19) 0.0049(18) 0.0000(16) -0.0012(14) C14 0.0167(16) 0.0273(19) 0.0224(19) 0.0032(17) -0.0008(14) 0.0066(16) C15 0.0237(19) 0.0239(18) 0.030(2) 0.0019(17) -0.0030(16) 0.0030(16) C16 0.026(2) 0.0231(18) 0.039(2) 0.0059(17) -0.0015(18) -0.0051(16) C17 0.021(2) 0.042(2) 0.047(3) 0.013(2) -0.0018(18) -0.0043(17) C18 0.038(2) 0.033(2) 0.050(3) 0.003(2) -0.002(2) -0.0092(18) C19 0.024(2) 0.028(2) 0.041(2) 0.0083(19) -0.0046(18) 0.0022(17) C20 0.042(2) 0.0219(19) 0.040(2) -0.0016(18) -0.004(2) 0.0025(17) C21 0.050(3) 0.030(2) 0.029(2) 0.0001(19) 0.001(2) 0.0018(19) C22 0.098(4) 0.038(3) 0.031(3) -0.008(2) 0.010(3) 0.003(3) C23 0.037(2) 0.031(2) 0.0217(19) 0.0041(18) 0.0042(17) 0.0024(19) C24 0.0160(17) 0.0216(17) 0.0220(19) 0.0043(15) -0.0009(15) 0.0018(14) C25 0.0174(17) 0.0255(18) 0.0277(19) -0.0035(18) 0.0024(14) 0.0048(17) C26 0.0246(19) 0.0309(19) 0.0185(18) 0.0025(16) 0.0036(16) 0.0053(16) C27 0.043(2) 0.0342(19) 0.0211(18) 0.0041(18) 0.005(2) 0.0083(17) C28 0.0333(19) 0.034(2) 0.033(2) 0.0088(19) -0.0053(17) 0.0074(16) C29 0.041(2) 0.045(2) 0.047(2) 0.017(2) 0.020(2) 0.012(2) C30 0.104(4) 0.049(3) 0.024(2) 0.008(2) 0.011(3) 0.022(3) C31 0.028(2) 0.035(2) 0.0219(19) -0.0020(17) 0.0028(16) 0.0030(17) C32 0.0182(18) 0.0245(19) 0.033(2) -0.0009(17) 0.0079(17) 0.0046(15) C33 0.033(2) 0.031(2) 0.039(2) -0.0061(18) 0.005(2) -0.0012(18) C34 0.0208(19) 0.028(2) 0.030(2) 0.0015(18) -0.0008(18) -0.0012(16) _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 O1 C3 1.362(5) . ? C1 C13 1.397(5) . ? C1 C24 1.407(5) . ? C1 C2 1.492(5) . ? O2 C25 1.352(4) . ? O2 C14 1.360(4) . ? C2 C3 1.394(5) . ? C2 C12 1.402(5) . ? C3 C4 1.401(5) . ? C4 C9 1.400(5) . ? C4 C5 1.541(5) . ? C5 C7 1.521(6) . ? C5 C8 1.529(6) . ? C5 C6 1.534(6) . ? C9 C10 1.390(5) . ? C10 C12 1.387(5) . ? C10 C11 1.508(5) . ? C13 C14 1.409(5) . ? C13 C23 1.427(5) . ? C14 C15 1.424(5) . ? C15 C20 1.372(5) . ? C15 C16 1.531(5) . ? C16 C17 1.533(6) . ? C16 C19 1.543(5) . ? C16 C18 1.545(5) . ? C20 C21 1.417(6) . ? C21 C23 1.362(5) . ? C21 C22 1.512(6) . ? C24 C25 1.411(5) . ? C24 C34 1.425(5) . ? C25 C26 1.424(5) . ? C26 C31 1.363(5) . ? C26 C27 1.549(5) . ? C27 C29 1.522(6) . ? C27 C30 1.531(6) . ? C27 C28 1.534(5) . ? C31 C32 1.426(5) . ? C32 C34 1.353(5) . ? C32 C33 1.506(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 C13 C1 C24 119.8(3) . . ? C13 C1 C2 119.8(3) . . ? C24 C1 C2 120.4(3) . . ? C25 O2 C14 121.8(3) . . ? C3 C2 C12 120.1(3) . . ? C3 C2 C1 122.7(3) . . ? C12 C2 C1 117.2(3) . . ? O1 C3 C2 121.2(3) . . ? O1 C3 C4 118.2(3) . . ? C2 C3 C4 120.7(3) . . ? C9 C4 C3 117.0(3) . . ? C9 C4 C5 121.5(3) . . ? C3 C4 C5 121.5(3) . . ? C7 C5 C8 107.9(3) . . ? C7 C5 C6 106.5(3) . . ? C8 C5 C6 111.4(4) . . ? C7 C5 C4 111.9(3) . . ? C8 C5 C4 109.1(3) . . ? C6 C5 C4 109.9(3) . . ? C10 C9 C4 124.0(3) . . ? C12 C10 C9 117.4(3) . . ? C12 C10 C11 120.7(3) . . ? C9 C10 C11 121.9(3) . . ? C10 C12 C2 120.9(3) . . ? C1 C13 C14 119.0(3) . . ? C1 C13 C23 121.8(3) . . ? C14 C13 C23 119.0(3) . . ? O2 C14 C13 119.6(3) . . ? O2 C14 C15 118.4(3) . . ? C13 C14 C15 122.0(3) . . ? C20 C15 C14 114.8(3) . . ? C20 C15 C16 121.2(3) . . ? C14 C15 C16 123.8(3) . . ? C15 C16 C17 109.4(3) . . ? C15 C16 C19 110.6(3) . . ? C17 C16 C19 112.3(3) . . ? C15 C16 C18 111.6(3) . . ? C17 C16 C18 106.1(3) . . ? C19 C16 C18 106.8(3) . . ? C15 C20 C21 125.4(4) . . ? C23 C21 C20 118.4(4) . . ? C23 C21 C22 122.2(4) . . ? C20 C21 C22 119.4(4) . . ? C21 C23 C13 120.1(4) . . ? C1 C24 C25 118.1(3) . . ? C1 C24 C34 122.4(3) . . ? C25 C24 C34 119.2(3) . . ? O2 C25 C24 120.3(3) . . ? O2 C25 C26 118.7(3) . . ? C24 C25 C26 120.9(3) . . ? C31 C26 C25 115.9(3) . . ? C31 C26 C27 121.3(3) . . ? C25 C26 C27 122.6(3) . . ? C29 C27 C30 107.6(4) . . ? C29 C27 C28 112.0(3) . . ? C30 C27 C28 106.8(4) . . ? C29 C27 C26 111.7(3) . . ? C30 C27 C26 111.0(3) . . ? C28 C27 C26 107.6(3) . . ? C26 C31 C32 125.0(4) . . ? C34 C32 C31 117.8(3) . . ? C34 C32 C33 123.0(4) . . ? C31 C32 C33 119.1(3) . . ? C32 C34 C24 120.7(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.366 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.103 #===END data_4a.2Me2CO _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H58 O6' _chemical_formula_weight 634.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2038(6) _cell_length_b 13.5294(8) _cell_length_c 14.9405(9) _cell_angle_alpha 96.0340(10) _cell_angle_beta 94.0770(10) _cell_angle_gamma 110.7520(10) _cell_volume 1905.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.70 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10563 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6651 _reflns_number_gt 4830 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Bruker AXS SMART ' _computing_cell_refinement 'Bruker AXS SMART ' _computing_data_reduction ' Bruker AXS SMART ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. Residual density associated with two full site-occupancy acetone solvates was located. One acetone is hydrogen-bonded to O(4). ; _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^)+(0.0789P)^2^+1.7326P] 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 0.0054(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6651 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 O1 O 0.2638(2) -0.11528(17) 0.30165(14) 0.0403(5) Uani 1 1 d . . . H1A H 0.319(4) -0.046(4) 0.331(3) 0.073(13) Uiso 1 1 d . . . O2 O 0.2842(2) 0.21625(17) 0.23854(15) 0.0380(5) Uani 1 1 d . . . H2A H 0.297(4) 0.172(3) 0.273(3) 0.055(11) Uiso 1 1 d . . . O3 O 0.6672(2) 0.16368(17) 0.34622(15) 0.0383(5) Uani 1 1 d . . . H3A H 0.732(4) 0.205(3) 0.373(3) 0.066(14) Uiso 1 1 d . . . O4 O 0.3932(2) 0.09077(16) 0.31581(13) 0.0314(5) Uani 1 1 d . . . H4A H 0.470(5) 0.136(4) 0.353(3) 0.088(15) Uiso 1 1 d . . . C1 C 0.4288(3) 0.0673(2) 0.22403(17) 0.0271(6) Uani 1 1 d . . . C2 C 0.2920(3) -0.0177(2) 0.17398(18) 0.0279(6) Uani 1 1 d . . . C3 C 0.2197(3) -0.1073(2) 0.21494(18) 0.0292(6) Uani 1 1 d . . . C4 C 0.1025(3) -0.1921(2) 0.16748(18) 0.0271(6) Uani 1 1 d . . . C5 C 0.0299(3) -0.2945(2) 0.20927(19) 0.0326(6) Uani 1 1 d . . . C6 C -0.0899(4) -0.3769(2) 0.1431(2) 0.0472(8) Uani 1 1 d . . . H6A H -0.1311 -0.4418 0.1708 0.071 Uiso 1 1 calc R . . H6B H -0.0527 -0.3940 0.0873 0.071 Uiso 1 1 calc R . . H6C H -0.1627 -0.3475 0.1288 0.071 Uiso 1 1 calc R . . C7 C -0.0330(4) -0.2677(3) 0.2945(2) 0.0455(8) Uani 1 1 d . . . H7A H -0.0745 -0.3325 0.3225 0.068 Uiso 1 1 calc R . . H7B H -0.1063 -0.2396 0.2780 0.068 Uiso 1 1 calc R . . H7C H 0.0414 -0.2140 0.3376 0.068 Uiso 1 1 calc R . . C8 C 0.1370(4) -0.3464(3) 0.2330(3) 0.0513(9) Uani 1 1 d . . . H8A H 0.0894 -0.4128 0.2574 0.077 Uiso 1 1 calc R . . H8B H 0.2122 -0.2974 0.2784 0.077 Uiso 1 1 calc R . . H8C H 0.1777 -0.3622 0.1783 0.077 Uiso 1 1 calc R . . C9 C 0.0589(3) -0.1801(2) 0.08031(18) 0.0288(6) Uani 1 1 d . . . H9A H -0.0214 -0.2355 0.0476 0.035 Uiso 1 1 calc R . . C10 C 0.1259(3) -0.0920(2) 0.03828(18) 0.0296(6) Uani 1 1 d . . . C11 C 0.0756(3) -0.0854(2) -0.0574(2) 0.0417(7) Uani 1 1 d . . . H11A H -0.0276 -0.1188 -0.0677 0.063 Uiso 1 1 calc R . . H11B H 0.1169 -0.1228 -0.1000 0.063 Uiso 1 1 calc R . . H11C H 0.1046 -0.0104 -0.0668 0.063 Uiso 1 1 calc R . . C12 C 0.2440(3) -0.0115(2) 0.08631(18) 0.0290(6) Uani 1 1 d . . . H12A H 0.2929 0.0489 0.0584 0.035 Uiso 1 1 calc R . . C13 C 0.4754(3) 0.1720(2) 0.18230(18) 0.0273(6) Uani 1 1 d . . . C14 C 0.4023(3) 0.2421(2) 0.19410(18) 0.0278(6) Uani 1 1 d . . . C15 C 0.4468(3) 0.3407(2) 0.16022(18) 0.0283(6) Uani 1 1 d . . . C16 C 0.3694(3) 0.4192(2) 0.1753(2) 0.0346(7) Uani 1 1 d . . . C17 C 0.4450(4) 0.5238(3) 0.1388(3) 0.0517(9) Uani 1 1 d . . . H17A H 0.3956 0.5731 0.1517 0.078 Uiso 1 1 calc R . . H17B H 0.4453 0.5092 0.0732 0.078 Uiso 1 1 calc R . . H17C H 0.5424 0.5559 0.1681 0.078 Uiso 1 1 calc R . . C18 C 0.2192(3) 0.3697(3) 0.1262(3) 0.0529(9) Uani 1 1 d . . . H18A H 0.1702 0.4196 0.1369 0.079 Uiso 1 1 calc R . . H18B H 0.1683 0.3031 0.1494 0.079 Uiso 1 1 calc R . . H18C H 0.2231 0.3547 0.0611 0.079 Uiso 1 1 calc R . . C19 C 0.3644(4) 0.4488(3) 0.2769(2) 0.0503(9) Uani 1 1 d . . . H19A H 0.3149 0.4988 0.2848 0.075 Uiso 1 1 calc R . . H19B H 0.4608 0.4823 0.3077 0.075 Uiso 1 1 calc R . . H19C H 0.3142 0.3841 0.3029 0.075 Uiso 1 1 calc R . . C20 C 0.5631(3) 0.3634(2) 0.11153(18) 0.0301(6) Uani 1 1 d . . . H20A H 0.5945 0.4291 0.0876 0.036 Uiso 1 1 calc R . . C21 C 0.6353(3) 0.2945(2) 0.09628(18) 0.0301(6) Uani 1 1 d . . . C22 C 0.7583(3) 0.3220(3) 0.0412(2) 0.0455(8) Uani 1 1 d . . . H22A H 0.7663 0.3866 0.0142 0.068 Uiso 1 1 calc R . . H22B H 0.7432 0.2627 -0.0070 0.068 Uiso 1 1 calc R . . H22C H 0.8453 0.3345 0.0805 0.068 Uiso 1 1 calc R . . C23 C 0.5895(3) 0.1989(2) 0.13224(18) 0.0289(6) Uani 1 1 d . . . H23A H 0.6375 0.1507 0.1223 0.035 Uiso 1 1 calc R . . C24 C 0.5486(3) 0.0228(2) 0.23024(17) 0.0269(6) Uani 1 1 d . . . C25 C 0.6700(3) 0.0762(2) 0.29128(18) 0.0282(6) Uani 1 1 d . . . C26 C 0.7857(3) 0.0423(2) 0.29546(17) 0.0274(6) Uani 1 1 d . . . C27 C 0.9230(3) 0.1030(2) 0.35887(19) 0.0324(6) Uani 1 1 d . . . C28 C 1.0303(3) 0.0479(3) 0.3494(2) 0.0439(8) Uani 1 1 d . . . H28A H 0.9912 -0.0237 0.3669 0.066 Uiso 1 1 calc R . . H28B H 1.1176 0.0898 0.3888 0.066 Uiso 1 1 calc R . . H28C H 1.0505 0.0422 0.2863 0.066 Uiso 1 1 calc R . . C29 C 0.9933(3) 0.2157(2) 0.3330(2) 0.0395(7) Uani 1 1 d . . . H29A H 1.0146 0.2099 0.2702 0.059 Uiso 1 1 calc R . . H29B H 1.0810 0.2540 0.3733 0.059 Uiso 1 1 calc R . . H29C H 0.9291 0.2547 0.3391 0.059 Uiso 1 1 calc R . . C30 C 0.8946(3) 0.1085(3) 0.4588(2) 0.0460(8) Uani 1 1 d . . . H30A H 0.8534 0.0360 0.4741 0.069 Uiso 1 1 calc R . . H30B H 0.8287 0.1456 0.4681 0.069 Uiso 1 1 calc R . . H30C H 0.9835 0.1474 0.4977 0.069 Uiso 1 1 calc R . . C31 C 0.7716(3) -0.0478(2) 0.23537(18) 0.0307(6) Uani 1 1 d . . . H31A H 0.8469 -0.0736 0.2372 0.037 Uiso 1 1 calc R . . C32 C 0.6536(3) -0.1020(2) 0.17299(19) 0.0305(6) Uani 1 1 d . . . C33 C 0.6483(3) -0.1963(2) 0.1075(2) 0.0425(8) Uani 1 1 d . . . H33A H 0.5710 -0.2124 0.0589 0.064 Uiso 1 1 calc R . . H33B H 0.6326 -0.2584 0.1395 0.064 Uiso 1 1 calc R . . H33C H 0.7379 -0.1795 0.0815 0.064 Uiso 1 1 calc R . . C34 C 0.5427(3) -0.0653(2) 0.17159(18) 0.0298(6) Uani 1 1 d . . . H34A H 0.4609 -0.1014 0.1295 0.036 Uiso 1 1 calc R . . O100 O 0.8283(3) 0.3437(2) 0.46317(19) 0.0702(8) Uani 1 1 d . . . C100 C 0.7876(4) 0.4155(3) 0.4453(3) 0.0570(9) Uani 1 1 d . . . C101 C 0.8004(6) 0.5030(4) 0.5174(3) 0.0954(16) Uani 1 1 d . . . H10A H 0.8376 0.4891 0.5751 0.143 Uiso 1 1 calc R . . H10B H 0.7073 0.5073 0.5228 0.143 Uiso 1 1 calc R . . H10C H 0.8648 0.5707 0.5022 0.143 Uiso 1 1 calc R . . C102 C 0.7315(5) 0.4191(3) 0.3540(3) 0.0731(12) Uani 1 1 d . . . H10D H 0.7646 0.3766 0.3103 0.110 Uiso 1 1 calc R . . H10E H 0.7641 0.4933 0.3418 0.110 Uiso 1 1 calc R . . H10F H 0.6282 0.3899 0.3484 0.110 Uiso 1 1 calc R . . C200 C 0.5585(4) -0.2304(3) 0.4634(3) 0.0629(10) Uani 1 1 d . . . O200 O 0.5363(4) -0.2675(3) 0.5331(2) 0.0941(11) Uani 1 1 d . . . C201 C 0.6501(7) -0.2590(4) 0.4005(4) 0.1030(18) Uani 1 1 d . . . H20B H 0.6718 -0.3193 0.4194 0.155 Uiso 1 1 calc R . . H20E H 0.7380 -0.1976 0.4020 0.155 Uiso 1 1 calc R . . H20C H 0.6010 -0.2790 0.3388 0.155 Uiso 1 1 calc R . . C202 C 0.5076(5) -0.1445(5) 0.4429(4) 0.0989(18) Uani 1 1 d . . . H20D H 0.4314 -0.1450 0.4795 0.148 Uiso 1 1 calc R . . H20H H 0.4722 -0.1563 0.3785 0.148 Uiso 1 1 calc R . . H20F H 0.5855 -0.0753 0.4573 0.148 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 O1 0.0432(12) 0.0343(12) 0.0357(11) 0.0129(9) -0.0056(9) 0.0043(10) O2 0.0301(11) 0.0374(12) 0.0528(13) 0.0158(10) 0.0161(9) 0.0152(9) O3 0.0323(12) 0.0341(12) 0.0410(12) -0.0104(10) -0.0014(10) 0.0084(10) O4 0.0310(11) 0.0320(11) 0.0299(10) 0.0037(8) 0.0043(8) 0.0099(9) C1 0.0250(13) 0.0285(14) 0.0269(13) 0.0030(11) 0.0039(11) 0.0087(11) C2 0.0228(13) 0.0273(14) 0.0338(15) 0.0058(11) 0.0044(11) 0.0085(11) C3 0.0299(14) 0.0280(14) 0.0308(14) 0.0066(11) 0.0026(11) 0.0114(12) C4 0.0247(13) 0.0255(14) 0.0337(15) 0.0056(11) 0.0086(11) 0.0111(11) C5 0.0336(15) 0.0240(14) 0.0390(16) 0.0069(12) 0.0081(12) 0.0077(12) C6 0.0482(19) 0.0286(16) 0.053(2) 0.0075(14) 0.0060(16) -0.0001(14) C7 0.0510(19) 0.0333(17) 0.0487(19) 0.0114(14) 0.0225(15) 0.0063(15) C8 0.055(2) 0.0371(18) 0.070(2) 0.0227(17) 0.0112(18) 0.0219(16) C9 0.0243(13) 0.0246(14) 0.0359(15) 0.0001(11) 0.0026(11) 0.0084(11) C10 0.0286(14) 0.0278(14) 0.0323(15) 0.0035(11) 0.0034(11) 0.0103(12) C11 0.0453(18) 0.0372(17) 0.0355(16) 0.0071(13) -0.0009(14) 0.0069(14) C12 0.0271(14) 0.0267(14) 0.0342(15) 0.0085(11) 0.0062(11) 0.0093(11) C13 0.0251(13) 0.0248(14) 0.0286(14) 0.0015(11) 0.0008(11) 0.0061(11) C14 0.0220(13) 0.0281(14) 0.0318(14) 0.0025(11) 0.0047(11) 0.0074(11) C15 0.0260(14) 0.0249(14) 0.0316(14) 0.0018(11) 0.0013(11) 0.0072(11) C16 0.0333(15) 0.0281(15) 0.0446(17) 0.0064(12) 0.0065(13) 0.0130(12) C17 0.058(2) 0.0357(18) 0.075(2) 0.0187(17) 0.0236(18) 0.0269(16) C18 0.0390(18) 0.048(2) 0.073(2) 0.0047(18) -0.0061(17) 0.0211(16) C19 0.061(2) 0.0423(19) 0.054(2) 0.0009(15) 0.0136(17) 0.0268(17) C20 0.0321(15) 0.0219(13) 0.0319(15) 0.0024(11) 0.0026(12) 0.0051(11) C21 0.0302(14) 0.0261(14) 0.0316(15) 0.0031(11) 0.0058(11) 0.0070(12) C22 0.0475(19) 0.0399(18) 0.054(2) 0.0129(15) 0.0257(16) 0.0169(15) C23 0.0272(14) 0.0257(14) 0.0331(15) 0.0000(11) 0.0039(11) 0.0099(11) C24 0.0274(14) 0.0246(13) 0.0279(14) 0.0064(11) 0.0030(11) 0.0077(11) C25 0.0289(14) 0.0253(14) 0.0283(14) 0.0039(11) 0.0037(11) 0.0072(11) C26 0.0267(14) 0.0282(14) 0.0264(14) 0.0078(11) 0.0033(11) 0.0077(11) C27 0.0269(14) 0.0389(16) 0.0305(15) 0.0045(12) -0.0005(11) 0.0115(12) C28 0.0326(16) 0.051(2) 0.0480(19) 0.0023(15) -0.0037(14) 0.0182(15) C29 0.0287(15) 0.0381(17) 0.0445(18) -0.0011(14) 0.0030(13) 0.0056(13) C30 0.0434(18) 0.063(2) 0.0308(16) 0.0054(15) -0.0031(14) 0.0201(16) C31 0.0308(15) 0.0309(15) 0.0341(15) 0.0118(12) 0.0051(12) 0.0135(12) C32 0.0327(15) 0.0231(14) 0.0353(15) 0.0062(11) 0.0030(12) 0.0092(12) C33 0.0408(17) 0.0295(16) 0.056(2) -0.0032(14) -0.0008(15) 0.0147(14) C34 0.0283(14) 0.0240(14) 0.0313(15) 0.0054(11) -0.0018(11) 0.0031(11) O100 0.0701(18) 0.0671(18) 0.0696(18) -0.0080(14) -0.0098(14) 0.0285(15) C100 0.059(2) 0.046(2) 0.060(2) -0.0039(17) 0.0051(18) 0.0157(18) C101 0.121(4) 0.086(4) 0.077(3) -0.022(3) 0.008(3) 0.045(3) C102 0.096(3) 0.047(2) 0.064(3) 0.0122(19) -0.006(2) 0.012(2) C200 0.058(2) 0.069(3) 0.049(2) 0.0097(19) 0.0050(18) 0.008(2) O200 0.115(3) 0.111(3) 0.072(2) 0.034(2) 0.023(2) 0.053(2) C201 0.136(5) 0.089(4) 0.099(4) 0.013(3) 0.059(4) 0.049(4) C202 0.082(3) 0.152(5) 0.096(4) 0.073(4) 0.027(3) 0.064(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 O1 C3 1.368(3) . ? O2 C14 1.371(3) . ? O3 C25 1.378(3) . ? O4 C1 1.474(3) . ? C1 C2 1.537(4) . ? C1 C13 1.540(4) . ? C1 C24 1.544(4) . ? C2 C12 1.387(4) . ? C2 C3 1.405(4) . ? C3 C4 1.409(4) . ? C4 C9 1.391(4) . ? C4 C5 1.542(4) . ? C5 C6 1.532(4) . ? C5 C7 1.533(4) . ? C5 C8 1.534(4) . ? C9 C10 1.388(4) . ? C10 C12 1.391(4) . ? C10 C11 1.506(4) . ? C13 C23 1.389(4) . ? C13 C14 1.404(4) . ? C14 C15 1.409(4) . ? C15 C20 1.394(4) . ? C15 C16 1.540(4) . ? C16 C17 1.530(4) . ? C16 C18 1.531(4) . ? C16 C19 1.538(4) . ? C20 C21 1.389(4) . ? C21 C23 1.390(4) . ? C21 C22 1.507(4) . ? C24 C34 1.384(4) . ? C24 C25 1.398(4) . ? C25 C26 1.409(4) . ? C26 C31 1.394(4) . ? C26 C27 1.538(4) . ? C27 C28 1.534(4) . ? C27 C30 1.540(4) . ? C27 C29 1.541(4) . ? C31 C32 1.388(4) . ? C32 C34 1.387(4) . ? C32 C33 1.507(4) . ? O100 C100 1.231(5) . ? C100 C102 1.453(5) . ? C100 C101 1.477(5) . ? C200 O200 1.204(5) . ? C200 C202 1.482(6) . ? C200 C201 1.487(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 O4 C1 C2 104.5(2) . . ? O4 C1 C13 107.8(2) . . ? C2 C1 C13 113.2(2) . . ? O4 C1 C24 109.4(2) . . ? C2 C1 C24 110.9(2) . . ? C13 C1 C24 110.8(2) . . ? C12 C2 C3 119.1(2) . . ? C12 C2 C1 121.1(2) . . ? C3 C2 C1 119.6(2) . . ? O1 C3 C2 120.6(2) . . ? O1 C3 C4 118.3(2) . . ? C2 C3 C4 121.1(2) . . ? C9 C4 C3 116.7(2) . . ? C9 C4 C5 121.9(2) . . ? C3 C4 C5 121.4(2) . . ? C6 C5 C7 107.9(2) . . ? C6 C5 C8 107.3(3) . . ? C7 C5 C8 110.1(3) . . ? C6 C5 C4 111.7(2) . . ? C7 C5 C4 110.0(2) . . ? C8 C5 C4 109.9(2) . . ? C10 C9 C4 123.8(2) . . ? C9 C10 C12 117.8(3) . . ? C9 C10 C11 121.1(2) . . ? C12 C10 C11 121.1(3) . . ? C2 C12 C10 121.4(3) . . ? C23 C13 C14 118.7(2) . . ? C23 C13 C1 121.0(2) . . ? C14 C13 C1 120.3(2) . . ? O2 C14 C13 120.8(2) . . ? O2 C14 C15 117.8(2) . . ? C13 C14 C15 121.4(2) . . ? C20 C15 C14 116.9(2) . . ? C20 C15 C16 121.5(2) . . ? C14 C15 C16 121.6(2) . . ? C17 C16 C18 108.1(3) . . ? C17 C16 C19 106.6(3) . . ? C18 C16 C19 109.8(3) . . ? C17 C16 C15 111.4(2) . . ? C18 C16 C15 109.9(2) . . ? C19 C16 C15 110.9(2) . . ? C21 C20 C15 123.2(3) . . ? C20 C21 C23 118.1(2) . . ? C20 C21 C22 120.9(3) . . ? C23 C21 C22 121.0(3) . . ? C13 C23 C21 121.6(2) . . ? C34 C24 C25 118.9(2) . . ? C34 C24 C1 120.9(2) . . ? C25 C24 C1 120.0(2) . . ? O3 C25 C24 114.8(2) . . ? O3 C25 C26 123.2(2) . . ? C24 C25 C26 122.0(2) . . ? C31 C26 C25 116.0(2) . . ? C31 C26 C27 121.1(2) . . ? C25 C26 C27 122.8(2) . . ? C28 C27 C26 111.5(2) . . ? C28 C27 C30 107.0(2) . . ? C26 C27 C30 111.0(2) . . ? C28 C27 C29 106.4(2) . . ? C26 C27 C29 109.6(2) . . ? C30 C27 C29 111.1(2) . . ? C32 C31 C26 123.6(3) . . ? C34 C32 C31 118.1(2) . . ? C34 C32 C33 121.3(3) . . ? C31 C32 C33 120.6(3) . . ? C24 C34 C32 121.4(2) . . ? O100 C100 C102 121.8(4) . . ? O100 C100 C101 119.5(4) . . ? C102 C100 C101 118.6(4) . . ? O200 C200 C202 120.0(4) . . ? O200 C200 C201 122.1(5) . . ? C202 C200 C201 117.5(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.890 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.053 #===END data_5a _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 O3' _chemical_formula_weight 500.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1823(6) _cell_length_b 12.6574(7) _cell_length_c 12.8089(7) _cell_angle_alpha 103.7790(10) _cell_angle_beta 108.4350(10) _cell_angle_gamma 111.6720(10) _cell_volume 1463.07(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.73 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9535 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6746 _reflns_number_gt 5849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART ' _computing_cell_refinement 'Bruker AXS SMART ' _computing_data_reduction 'Bruker AXS SMART ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ; _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^)+(0.0704P)^2^+0.4651P] 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 6746 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 O1 O 0.78003(13) 0.09917(10) -0.29382(8) 0.0399(3) Uani 1 1 d . . . H1A H 0.809(2) 0.0529(19) -0.2629(18) 0.055(5) Uiso 1 1 d . . . O2 O 0.90777(9) 0.09214(8) 0.19056(7) 0.02580(19) Uani 1 1 d . . . O3 O 0.88512(10) 0.02852(8) -0.13494(8) 0.0284(2) Uani 1 1 d . . . H3A H 0.876(2) -0.039(2) -0.1259(19) 0.061(6) Uiso 1 1 d . . . C1 C 0.86997(13) 0.10666(11) -0.04152(10) 0.0231(2) Uani 1 1 d . . . C2 C 0.83658(12) 0.20056(10) -0.08516(10) 0.0225(2) Uani 1 1 d . . . C3 C 0.79863(13) 0.19516(11) -0.20244(10) 0.0244(2) Uani 1 1 d . . . C4 C 0.77732(12) 0.29019(11) -0.23110(10) 0.0237(2) Uani 1 1 d . . . C5 C 0.73926(14) 0.28645(12) -0.35892(11) 0.0287(3) Uani 1 1 d . . . C6 C 0.72581(19) 0.40090(14) -0.36637(14) 0.0413(3) Uani 1 1 d . . . H6A H 0.6498 0.4035 -0.3451 0.062 Uiso 1 1 calc R . . H6B H 0.7016 0.3962 -0.4484 0.062 Uiso 1 1 calc R . . H6C H 0.8174 0.4761 -0.3103 0.062 Uiso 1 1 calc R . . C7 C 0.59405(16) 0.17141(14) -0.44888(13) 0.0411(3) Uani 1 1 d . . . H7A H 0.5203 0.1710 -0.4230 0.062 Uiso 1 1 calc R . . H7B H 0.6022 0.0963 -0.4524 0.062 Uiso 1 1 calc R . . H7C H 0.5670 0.1735 -0.5287 0.062 Uiso 1 1 calc R . . C8 C 0.85657(17) 0.28535(16) -0.39640(13) 0.0415(3) Uani 1 1 d . . . H8A H 0.8668 0.2121 -0.3945 0.062 Uiso 1 1 calc R . . H8B H 0.9482 0.3607 -0.3406 0.062 Uiso 1 1 calc R . . H8C H 0.8295 0.2825 -0.4780 0.062 Uiso 1 1 calc R . . C9 C 0.79037(12) 0.38552(11) -0.14034(11) 0.0241(2) Uani 1 1 d . . . H9A H 0.7775 0.4504 -0.1581 0.029 Uiso 1 1 calc R . . C10 C 0.82163(12) 0.39066(11) -0.02408(11) 0.0244(2) Uani 1 1 d . . . C11 C 0.82853(16) 0.49392(12) 0.06912(12) 0.0333(3) Uani 1 1 d . . . H11A H 0.9042 0.5738 0.0826 0.050 Uiso 1 1 calc R . . H11B H 0.8502 0.4822 0.1445 0.050 Uiso 1 1 calc R . . H11C H 0.7357 0.4930 0.0409 0.050 Uiso 1 1 calc R . . C12 C 0.84587(13) 0.29841(11) 0.00154(10) 0.0240(2) Uani 1 1 d . . . H12A H 0.8697 0.3015 0.0807 0.029 Uiso 1 1 calc R . . C13 C 1.01248(13) 0.17563(11) 0.07022(11) 0.0239(2) Uani 1 1 d . . . C14 C 1.02414(12) 0.17185(11) 0.18042(11) 0.0230(2) Uani 1 1 d . . . C15 C 1.15700(13) 0.24859(11) 0.28601(11) 0.0255(2) Uani 1 1 d . . . C16 C 1.17270(14) 0.26355(12) 0.41299(11) 0.0309(3) Uani 1 1 d . . . C17 C 1.07189(16) 0.31166(14) 0.43671(13) 0.0367(3) Uani 1 1 d . . . H17A H 1.1034 0.3952 0.4375 0.055 Uiso 1 1 calc R . . H17B H 1.0748 0.3146 0.5146 0.055 Uiso 1 1 calc R . . H17C H 0.9733 0.2558 0.3731 0.055 Uiso 1 1 calc R . . C18 C 1.32599(16) 0.35962(15) 0.51074(13) 0.0426(3) Uani 1 1 d . . . H18A H 1.3515 0.4399 0.5043 0.064 Uiso 1 1 calc R . . H18B H 1.3939 0.3317 0.5001 0.064 Uiso 1 1 calc R . . H18C H 1.3303 0.3685 0.5902 0.064 Uiso 1 1 calc R . . C19 C 1.14112(18) 0.14046(14) 0.42751(13) 0.0400(3) Uani 1 1 d . . . H19A H 1.2132 0.1170 0.4197 0.060 Uiso 1 1 calc R . . H19B H 1.0451 0.0754 0.3651 0.060 Uiso 1 1 calc R . . H19C H 1.1450 0.1504 0.5070 0.060 Uiso 1 1 calc R . . C20 C 1.27526(13) 0.31639(12) 0.27039(12) 0.0281(3) Uani 1 1 d . . . H20A H 1.3661 0.3658 0.3392 0.034 Uiso 1 1 calc R . . C21 C 1.26828(14) 0.31605(12) 0.15928(12) 0.0283(3) Uani 1 1 d . . . C22 C 1.40179(15) 0.39404(14) 0.15096(14) 0.0363(3) Uani 1 1 d . . . H22A H 1.4831 0.3874 0.2013 0.054 Uiso 1 1 calc R . . H22B H 1.4231 0.4810 0.1789 0.054 Uiso 1 1 calc R . . H22C H 1.3859 0.3644 0.0673 0.054 Uiso 1 1 calc R . . C23 C 1.13527(14) 0.24734(11) 0.06110(11) 0.0267(2) Uani 1 1 d . . . H23A H 1.1266 0.2486 -0.0147 0.032 Uiso 1 1 calc R . . C24 C 0.75081(13) 0.02387(11) -0.02047(11) 0.0240(2) Uani 1 1 d . . . C25 C 0.77674(13) 0.01261(11) 0.08890(11) 0.0239(2) Uani 1 1 d . . . C26 C 0.66867(13) -0.08041(11) 0.10077(11) 0.0266(2) Uani 1 1 d . . . C27 C 0.69801(14) -0.11167(12) 0.21245(12) 0.0295(3) Uani 1 1 d . . . C28 C 0.74412(17) -0.00080(14) 0.32567(12) 0.0359(3) Uani 1 1 d . . . H28A H 0.6666 0.0207 0.3147 0.054 Uiso 1 1 calc R . . H28B H 0.8311 0.0706 0.3394 0.054 Uiso 1 1 calc R . . H28C H 0.7640 -0.0230 0.3952 0.054 Uiso 1 1 calc R . . C29 C 0.81164(16) -0.15516(13) 0.22578(12) 0.0340(3) Uani 1 1 d . . . H29A H 0.7686 -0.2375 0.1620 0.051 Uiso 1 1 calc R . . H29B H 0.8460 -0.1595 0.3043 0.051 Uiso 1 1 calc R . . H29C H 0.8927 -0.0962 0.2195 0.051 Uiso 1 1 calc R . . C30 C 0.56282(17) -0.21895(15) 0.19845(14) 0.0418(3) Uani 1 1 d . . . H30A H 0.5294 -0.2929 0.1277 0.063 Uiso 1 1 calc R . . H30B H 0.4870 -0.1953 0.1884 0.063 Uiso 1 1 calc R . . H30C H 0.5858 -0.2371 0.2703 0.063 Uiso 1 1 calc R . . C31 C 0.53485(14) -0.15090(12) 0.00152(12) 0.0297(3) Uani 1 1 d . . . H31A H 0.4596 -0.2112 0.0084 0.036 Uiso 1 1 calc R . . C32 C 0.50403(14) -0.13847(12) -0.10813(12) 0.0295(3) Uani 1 1 d . . . C33 C 0.35602(15) -0.22141(14) -0.21233(13) 0.0381(3) Uani 1 1 d . . . H33A H 0.3606 -0.2200 -0.2872 0.057 Uiso 1 1 calc R . . H33B H 0.2900 -0.1916 -0.2004 0.057 Uiso 1 1 calc R . . H33C H 0.3213 -0.3066 -0.2171 0.057 Uiso 1 1 calc R . . C34 C 0.61396(14) -0.05185(12) -0.11788(11) 0.0281(3) Uani 1 1 d . . . H34A H 0.5965 -0.0434 -0.1922 0.034 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 O1 0.0690(7) 0.0348(5) 0.0243(5) 0.0128(4) 0.0189(5) 0.0341(5) O2 0.0244(4) 0.0261(4) 0.0231(4) 0.0120(3) 0.0096(3) 0.0082(4) O3 0.0391(5) 0.0255(4) 0.0282(4) 0.0125(4) 0.0176(4) 0.0196(4) C1 0.0282(6) 0.0217(5) 0.0224(5) 0.0108(4) 0.0118(5) 0.0133(5) C2 0.0232(5) 0.0207(5) 0.0244(5) 0.0111(4) 0.0104(4) 0.0105(4) C3 0.0273(6) 0.0218(5) 0.0230(5) 0.0088(4) 0.0111(5) 0.0112(5) C4 0.0216(5) 0.0240(5) 0.0239(5) 0.0114(5) 0.0095(4) 0.0091(4) C5 0.0305(6) 0.0284(6) 0.0252(6) 0.0139(5) 0.0103(5) 0.0123(5) C6 0.0561(9) 0.0382(7) 0.0355(7) 0.0241(6) 0.0176(7) 0.0251(7) C7 0.0382(8) 0.0383(8) 0.0281(7) 0.0126(6) 0.0052(6) 0.0090(6) C8 0.0451(8) 0.0547(9) 0.0303(7) 0.0207(7) 0.0209(6) 0.0237(7) C9 0.0222(5) 0.0199(5) 0.0288(6) 0.0115(5) 0.0097(5) 0.0091(4) C10 0.0220(5) 0.0214(5) 0.0260(6) 0.0075(4) 0.0099(4) 0.0088(4) C11 0.0383(7) 0.0278(6) 0.0317(6) 0.0083(5) 0.0139(6) 0.0179(6) C12 0.0251(6) 0.0249(5) 0.0216(5) 0.0096(4) 0.0103(4) 0.0116(5) C13 0.0264(6) 0.0229(5) 0.0259(6) 0.0122(5) 0.0116(5) 0.0139(5) C14 0.0235(5) 0.0225(5) 0.0265(6) 0.0125(5) 0.0119(5) 0.0122(5) C15 0.0268(6) 0.0240(6) 0.0264(6) 0.0113(5) 0.0099(5) 0.0138(5) C16 0.0305(6) 0.0316(6) 0.0237(6) 0.0111(5) 0.0080(5) 0.0117(5) C17 0.0397(7) 0.0368(7) 0.0303(7) 0.0102(6) 0.0173(6) 0.0159(6) C18 0.0359(7) 0.0455(8) 0.0278(7) 0.0117(6) 0.0055(6) 0.0111(7) C19 0.0467(8) 0.0388(7) 0.0306(7) 0.0192(6) 0.0116(6) 0.0184(7) C20 0.0242(6) 0.0263(6) 0.0296(6) 0.0102(5) 0.0089(5) 0.0115(5) C21 0.0275(6) 0.0260(6) 0.0356(7) 0.0139(5) 0.0165(5) 0.0139(5) C22 0.0288(6) 0.0353(7) 0.0422(8) 0.0154(6) 0.0181(6) 0.0114(6) C23 0.0298(6) 0.0274(6) 0.0296(6) 0.0151(5) 0.0164(5) 0.0153(5) C24 0.0265(6) 0.0218(5) 0.0257(6) 0.0119(4) 0.0115(5) 0.0123(5) C25 0.0241(6) 0.0234(5) 0.0242(6) 0.0107(5) 0.0100(5) 0.0113(5) C26 0.0283(6) 0.0259(6) 0.0279(6) 0.0137(5) 0.0137(5) 0.0126(5) C27 0.0304(6) 0.0302(6) 0.0297(6) 0.0168(5) 0.0160(5) 0.0111(5) C28 0.0445(8) 0.0379(7) 0.0315(7) 0.0178(6) 0.0221(6) 0.0194(6) C29 0.0421(7) 0.0354(7) 0.0319(7) 0.0197(6) 0.0185(6) 0.0206(6) C30 0.0378(8) 0.0412(8) 0.0404(8) 0.0241(7) 0.0188(6) 0.0077(6) C31 0.0267(6) 0.0262(6) 0.0338(6) 0.0138(5) 0.0135(5) 0.0096(5) C32 0.0264(6) 0.0265(6) 0.0309(6) 0.0120(5) 0.0086(5) 0.0114(5) C33 0.0286(7) 0.0348(7) 0.0367(7) 0.0147(6) 0.0059(6) 0.0089(6) C34 0.0300(6) 0.0277(6) 0.0264(6) 0.0139(5) 0.0096(5) 0.0144(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 O1 C3 1.3681(15) . ? O2 C14 1.3884(14) . ? O2 C25 1.3911(14) . ? O3 C1 1.4583(14) . ? C1 C24 1.5089(16) . ? C1 C13 1.5117(16) . ? C1 C2 1.5417(15) . ? C2 C12 1.3981(16) . ? C2 C3 1.4027(16) . ? C3 C4 1.4160(16) . ? C4 C9 1.3867(17) . ? C4 C5 1.5399(16) . ? C5 C6 1.5323(18) . ? C5 C7 1.5349(19) . ? C5 C8 1.536(2) . ? C9 C10 1.3970(17) . ? C10 C12 1.3801(17) . ? C10 C11 1.5045(17) . ? C13 C14 1.3900(16) . ? C13 C23 1.3980(17) . ? C14 C15 1.4204(17) . ? C15 C20 1.3914(18) . ? C15 C16 1.5364(17) . ? C16 C19 1.5362(19) . ? C16 C18 1.5370(19) . ? C16 C17 1.539(2) . ? C20 C21 1.3994(18) . ? C21 C23 1.3750(18) . ? C21 C22 1.5090(18) . ? C24 C25 1.3913(16) . ? C24 C34 1.3988(17) . ? C25 C26 1.4214(16) . ? C26 C31 1.3864(18) . ? C26 C27 1.5425(17) . ? C27 C30 1.5355(18) . ? C27 C28 1.5367(19) . ? C27 C29 1.5398(19) . ? C31 C32 1.3984(18) . ? C32 C34 1.3768(18) . ? C32 C33 1.5083(18) . ? 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 C14 O2 C25 120.01(9) . . ? O3 C1 C24 108.19(9) . . ? O3 C1 C13 107.59(9) . . ? C24 C1 C13 111.54(9) . . ? O3 C1 C2 107.74(9) . . ? C24 C1 C2 112.17(9) . . ? C13 C1 C2 109.42(9) . . ? C12 C2 C3 118.66(10) . . ? C12 C2 C1 115.78(10) . . ? C3 C2 C1 125.56(10) . . ? O1 C3 C2 122.26(10) . . ? O1 C3 C4 117.02(10) . . ? C2 C3 C4 120.73(11) . . ? C9 C4 C3 117.54(10) . . ? C9 C4 C5 121.47(10) . . ? C3 C4 C5 120.98(11) . . ? C6 C5 C7 107.49(12) . . ? C6 C5 C8 107.10(12) . . ? C7 C5 C8 109.79(12) . . ? C6 C5 C4 111.11(11) . . ? C7 C5 C4 110.11(10) . . ? C8 C5 C4 111.13(11) . . ? C4 C9 C10 123.11(11) . . ? C12 C10 C9 117.72(11) . . ? C12 C10 C11 121.72(11) . . ? C9 C10 C11 120.57(11) . . ? C10 C12 C2 122.15(11) . . ? C14 C13 C23 119.72(11) . . ? C14 C13 C1 122.37(11) . . ? C23 C13 C1 117.89(10) . . ? O2 C14 C13 121.33(11) . . ? O2 C14 C15 118.04(10) . . ? C13 C14 C15 120.62(11) . . ? C20 C15 C14 116.47(11) . . ? C20 C15 C16 120.08(11) . . ? C14 C15 C16 123.39(11) . . ? C19 C16 C15 110.79(11) . . ? C19 C16 C18 106.55(11) . . ? C15 C16 C18 112.15(11) . . ? C19 C16 C17 111.78(12) . . ? C15 C16 C17 108.85(10) . . ? C18 C16 C17 106.67(12) . . ? C15 C20 C21 123.88(12) . . ? C23 C21 C20 117.40(11) . . ? C23 C21 C22 122.22(12) . . ? C20 C21 C22 120.30(12) . . ? C21 C23 C13 121.57(11) . . ? C25 C24 C34 119.67(11) . . ? C25 C24 C1 121.83(11) . . ? C34 C24 C1 118.22(10) . . ? O2 C25 C24 121.62(10) . . ? O2 C25 C26 117.59(10) . . ? C24 C25 C26 120.79(11) . . ? C31 C26 C25 116.48(11) . . ? C31 C26 C27 120.15(11) . . ? C25 C26 C27 123.16(11) . . ? C30 C27 C28 106.03(11) . . ? C30 C27 C29 106.94(11) . . ? C28 C27 C29 112.38(11) . . ? C30 C27 C26 111.72(11) . . ? C28 C27 C26 111.50(11) . . ? C29 C27 C26 108.21(10) . . ? C26 C31 C32 123.86(12) . . ? C34 C32 C31 117.74(12) . . ? C34 C32 C33 122.03(12) . . ? C31 C32 C33 120.19(12) . . ? C32 C34 C24 121.27(11) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.320 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.053 #===END data_7b #lithium salt _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.67 H100.33 Li3 O7.67' _chemical_formula_weight 997.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? 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 20.9835(14) _cell_length_b 10.8817(7) _cell_length_c 27.2374(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.486(2) _cell_angle_gamma 90.00 _cell_volume 6151.2(7) _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 block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2187 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.85 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25905 _diffrn_reflns_av_R_equivalents 0.2046 _diffrn_reflns_av_sigmaI/netI 0.2205 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8046 _reflns_number_gt 3153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Bruker AXS SMART ' _computing_cell_refinement 'Bruker AXS SMART ' _computing_data_reduction ' Bruker AXS SMART ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1204P)^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 8046 _refine_ls_number_parameters 695 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2321 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2676 _refine_ls_wR_factor_gt 0.1949 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.978 _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 Li3 Li 0.2000(6) 0.7631(11) 0.1509(4) 0.038(3) Uani 1 1 d . . . Li2 Li 0.2937(6) 0.8654(12) 0.1277(5) 0.046(4) Uani 1 1 d . . . Li1 Li 0.1179(6) 0.6895(12) -0.0045(5) 0.048(4) Uani 1 1 d . . . O1 O 0.0886(2) 0.6450(5) 0.05010(17) 0.0431(14) Uani 1 1 d . . . O2 O 0.2866(2) 0.7224(4) 0.16706(15) 0.0297(12) Uani 1 1 d . . . O3 O 0.2073(2) 0.8359(4) 0.09000(16) 0.0329(13) Uani 1 1 d . . . C1 C 0.2195(3) 0.5601(6) 0.0844(2) 0.0224(17) Uani 1 1 d . . . C2 C 0.1676(3) 0.5816(6) 0.1185(2) 0.0255(18) Uani 1 1 d . . . C3 C 0.1045(3) 0.6209(6) 0.0979(3) 0.0296(18) Uani 1 1 d . . . C4 C 0.0561(3) 0.6299(6) 0.1303(3) 0.0309(18) Uani 1 1 d . . . C5 C -0.0104(3) 0.6843(7) 0.1105(3) 0.0336(19) Uani 1 1 d . . . C6 C -0.0467(3) 0.6040(7) 0.0693(3) 0.045(2) Uani 1 1 d . . . H6A H -0.0212 0.5951 0.0429 0.068 Uiso 1 1 calc R . . H6B H -0.0870 0.6422 0.0566 0.068 Uiso 1 1 calc R . . H6C H -0.0545 0.5246 0.0824 0.068 Uiso 1 1 calc R . . C7 C -0.0537(4) 0.6938(8) 0.1519(3) 0.060(3) Uani 1 1 d . . . H7A H -0.0940 0.7315 0.1387 0.091 Uiso 1 1 calc R . . H7B H -0.0324 0.7427 0.1788 0.091 Uiso 1 1 calc R . . H7C H -0.0616 0.6130 0.1639 0.091 Uiso 1 1 calc R . . C8 C -0.0021(4) 0.8149(8) 0.0909(3) 0.055(2) Uani 1 1 d . . . H8A H 0.0245 0.8123 0.0652 0.083 Uiso 1 1 calc R . . H8B H 0.0178 0.8661 0.1175 0.083 Uiso 1 1 calc R . . H8C H -0.0436 0.8480 0.0778 0.083 Uiso 1 1 calc R . . C9 C 0.0717(3) 0.5893(6) 0.1789(2) 0.0330(19) Uani 1 1 d . . . H9A H 0.0405 0.5955 0.1997 0.040 Uiso 1 1 calc R . . C10 C 0.1317(3) 0.5394(6) 0.1985(2) 0.0291(18) Uani 1 1 d . . . C11 C 0.1441(3) 0.4793(7) 0.2503(2) 0.0344(19) Uani 1 1 d . . . C12 C 0.0999(4) 0.5287(8) 0.2852(3) 0.063(3) Uani 1 1 d . . . H12A H 0.1135 0.4976 0.3180 0.095 Uiso 1 1 calc R . . H12B H 0.0565 0.5028 0.2739 0.095 Uiso 1 1 calc R . . H12C H 0.1019 0.6168 0.2857 0.095 Uiso 1 1 calc R . . C13 C 0.2139(3) 0.5001(8) 0.2752(3) 0.052(2) Uani 1 1 d . . . H13A H 0.2195 0.4666 0.3081 0.078 Uiso 1 1 calc R . . H13B H 0.2229 0.5867 0.2768 0.078 Uiso 1 1 calc R . . H13C H 0.2429 0.4602 0.2561 0.078 Uiso 1 1 calc R . . C14 C 0.1339(4) 0.3427(7) 0.2441(3) 0.061(3) Uani 1 1 d . . . H14A H 0.1449 0.3029 0.2757 0.091 Uiso 1 1 calc R . . H14B H 0.1608 0.3115 0.2214 0.091 Uiso 1 1 calc R . . H14C H 0.0896 0.3267 0.2314 0.091 Uiso 1 1 calc R . . C15 C 0.1790(3) 0.5390(6) 0.1673(2) 0.0299(18) Uani 1 1 d . . . H15A H 0.2166 0.4858 0.1765 0.036 Uiso 1 1 calc R . . C16 C 0.2905(3) 0.5496(6) 0.1125(2) 0.0219(17) Uani 1 1 d . . . C17 C 0.3177(3) 0.6262(7) 0.1523(2) 0.0282(18) Uani 1 1 d . . . C18 C 0.3813(3) 0.5973(6) 0.1765(2) 0.0287(18) Uani 1 1 d . . . C19 C 0.4112(3) 0.6642(7) 0.2244(3) 0.034(2) Uani 1 1 d . . . C20 C 0.4712(4) 0.5961(8) 0.2510(3) 0.068(3) Uani 1 1 d . . . H20A H 0.5050 0.5993 0.2308 0.102 Uiso 1 1 calc R . . H20B H 0.4603 0.5119 0.2563 0.102 Uiso 1 1 calc R . . H20C H 0.4855 0.6347 0.2824 0.102 Uiso 1 1 calc R . . C21 C 0.4333(4) 0.7935(7) 0.2116(3) 0.055(2) Uani 1 1 d . . . H21A H 0.4648 0.7869 0.1895 0.082 Uiso 1 1 calc R . . H21B H 0.4519 0.8347 0.2414 0.082 Uiso 1 1 calc R . . H21C H 0.3969 0.8396 0.1958 0.082 Uiso 1 1 calc R . . C22 C 0.3638(3) 0.6717(7) 0.2626(2) 0.047(2) Uani 1 1 d . . . H22A H 0.3845 0.7109 0.2923 0.070 Uiso 1 1 calc R . . H22B H 0.3507 0.5903 0.2704 0.070 Uiso 1 1 calc R . . H22C H 0.3266 0.7185 0.2489 0.070 Uiso 1 1 calc R . . C23 C 0.4180(3) 0.5146(7) 0.1548(3) 0.0323(19) Uani 1 1 d . . . H23A H 0.4601 0.5002 0.1698 0.039 Uiso 1 1 calc R . . C24 C 0.3949(3) 0.4515(6) 0.1114(2) 0.0239(17) Uani 1 1 d . . . C25 C 0.4423(3) 0.3751(7) 0.0854(3) 0.0348(19) Uani 1 1 d . . . C26 C 0.4790(4) 0.2808(7) 0.1204(3) 0.053(2) Uani 1 1 d . . . H26A H 0.5054 0.2311 0.1023 0.080 Uiso 1 1 calc R . . H26B H 0.4489 0.2293 0.1341 0.080 Uiso 1 1 calc R . . H26C H 0.5058 0.3227 0.1468 0.080 Uiso 1 1 calc R . . C27 C 0.4907(4) 0.4632(7) 0.0677(3) 0.056(2) Uani 1 1 d . . . H27A H 0.5167 0.4194 0.0474 0.084 Uiso 1 1 calc R . . H27B H 0.5177 0.4974 0.0959 0.084 Uiso 1 1 calc R . . H27C H 0.4680 0.5281 0.0487 0.084 Uiso 1 1 calc R . . C28 C 0.4081(4) 0.3065(7) 0.0403(3) 0.052(2) Uani 1 1 d . . . H28A H 0.4390 0.2590 0.0257 0.078 Uiso 1 1 calc R . . H28B H 0.3877 0.3645 0.0165 0.078 Uiso 1 1 calc R . . H28C H 0.3762 0.2527 0.0504 0.078 Uiso 1 1 calc R . . C29 C 0.3309(3) 0.4686(6) 0.0925(2) 0.0288(18) Uani 1 1 d . . . H29A H 0.3138 0.4233 0.0647 0.035 Uiso 1 1 calc R . . C30 C 0.2202(3) 0.6553(6) 0.0420(2) 0.0234(17) Uani 1 1 d . . . C31 C 0.2120(3) 0.7853(7) 0.0470(3) 0.0298(18) Uani 1 1 d . . . C32 C 0.2073(3) 0.8580(7) 0.0034(3) 0.0298(18) Uani 1 1 d . . . C33 C 0.1880(4) 0.9930(7) 0.0041(3) 0.043(2) Uani 1 1 d . . . C34 C 0.1226(4) 1.0052(8) 0.0225(3) 0.066(3) Uani 1 1 d . . . H34A H 0.1251 0.9685 0.0548 0.099 Uiso 1 1 calc R . . H34B H 0.0901 0.9642 -0.0002 0.099 Uiso 1 1 calc R . . H34C H 0.1117 1.0906 0.0245 0.099 Uiso 1 1 calc R . . C35 C 0.2390(5) 1.0667(8) 0.0377(3) 0.076(3) Uani 1 1 d . . . H35A H 0.2436 1.0342 0.0708 0.114 Uiso 1 1 calc R . . H35B H 0.2260 1.1512 0.0380 0.114 Uiso 1 1 calc R . . H35C H 0.2795 1.0610 0.0253 0.114 Uiso 1 1 calc R . . C36 C 0.1818(4) 1.0553(7) -0.0475(3) 0.054(2) Uani 1 1 d . . . H36A H 0.2225 1.0518 -0.0596 0.082 Uiso 1 1 calc R . . H36B H 0.1692 1.1395 -0.0447 0.082 Uiso 1 1 calc R . . H36C H 0.1498 1.0131 -0.0702 0.082 Uiso 1 1 calc R . . C37 C 0.2214(3) 0.8051(7) -0.0410(3) 0.0330(19) Uani 1 1 d . . . H37A H 0.2198 0.8550 -0.0689 0.040 Uiso 1 1 calc R . . C38 C 0.2376(3) 0.6827(7) -0.0452(2) 0.0290(18) Uani 1 1 d . . . C39 C 0.2594(3) 0.6276(7) -0.0920(2) 0.0327(19) Uani 1 1 d . . . C40 C 0.2170(4) 0.5183(8) -0.1106(3) 0.062(3) Uani 1 1 d . . . H40A H 0.2312 0.4847 -0.1397 0.093 Uiso 1 1 calc R . . H40B H 0.1730 0.5449 -0.1185 0.093 Uiso 1 1 calc R . . H40C H 0.2201 0.4565 -0.0852 0.093 Uiso 1 1 calc R . . C41 C 0.3291(4) 0.5858(9) -0.0793(3) 0.069(3) Uani 1 1 d . . . H41A H 0.3428 0.5485 -0.1079 0.104 Uiso 1 1 calc R . . H41B H 0.3325 0.5271 -0.0527 0.104 Uiso 1 1 calc R . . H41C H 0.3559 0.6554 -0.0691 0.104 Uiso 1 1 calc R . . C42 C 0.2572(4) 0.7211(8) -0.1339(3) 0.055(2) Uani 1 1 d . . . H42A H 0.2727 0.6837 -0.1618 0.082 Uiso 1 1 calc R . . H42B H 0.2838 0.7902 -0.1227 0.082 Uiso 1 1 calc R . . H42C H 0.2136 0.7481 -0.1436 0.082 Uiso 1 1 calc R . . C43 C 0.2339(3) 0.6108(7) -0.0036(2) 0.0283(18) Uani 1 1 d . . . H43A H 0.2401 0.5220 -0.0066 0.034 Uiso 1 1 calc R . . C44 C 0.1962(3) 0.4317(6) 0.0627(2) 0.0312(19) Uani 1 1 d . . . H44A H 0.1516 0.4367 0.0484 0.047 Uiso 1 1 calc R . . H44B H 0.2012 0.3715 0.0888 0.047 Uiso 1 1 calc R . . H44C H 0.2214 0.4081 0.0376 0.047 Uiso 1 1 calc R . . O101 O 0.0553(2) 0.7282(5) -0.05972(18) 0.0547(16) Uani 1 1 d . . . C101 C -0.0135(4) 0.7108(9) -0.0581(3) 0.063(3) Uani 1 1 d . . . H10B H -0.0288 0.7711 -0.0363 0.076 Uiso 1 1 calc R . . H10C H -0.0214 0.6294 -0.0458 0.076 Uiso 1 1 calc R . . C102 C -0.0477(4) 0.7264(9) -0.1104(3) 0.063(3) Uani 1 1 d . . . H10D H -0.0753 0.6566 -0.1203 0.075 Uiso 1 1 calc R . . H10E H -0.0735 0.8007 -0.1134 0.075 Uiso 1 1 calc R . . C103 C 0.0057(4) 0.7347(11) -0.1410(3) 0.085(4) Uani 1 1 d . . . H10F H 0.0125 0.6558 -0.1559 0.102 Uiso 1 1 calc R . . H10G H -0.0046 0.7950 -0.1672 0.102 Uiso 1 1 calc R . . C104 C 0.0610(4) 0.7704(10) -0.1086(3) 0.073(3) Uani 1 1 d . . . H10H H 0.0652 0.8592 -0.1086 0.087 Uiso 1 1 calc R . . H10I H 0.0991 0.7351 -0.1193 0.087 Uiso 1 1 calc R . . O201 O 0.3046(3) 1.0312(5) 0.1700(2) 0.0596(17) Uani 1 1 d . . . C201 C 0.3003(5) 1.1603(8) 0.1568(4) 0.079(3) Uani 1 1 d . . . H20A H 0.2561 1.1816 0.1441 0.095 Uiso 1 1 calc R . . H20B H 0.3266 1.1770 0.1310 0.095 Uiso 1 1 calc R . . C202 C 0.3233(6) 1.2343(10) 0.2014(4) 0.106(4) Uani 1 1 d . . . H20C H 0.2987 1.3094 0.2023 0.127 Uiso 1 1 calc R . . H20D H 0.3687 1.2544 0.2034 0.127 Uiso 1 1 calc R . . C203 C 0.3115(8) 1.1470(12) 0.2419(4) 0.139(5) Uani 1 1 d . . . H20E H 0.3435 1.1587 0.2711 0.167 Uiso 1 1 calc R . . H20F H 0.2692 1.1609 0.2511 0.167 Uiso 1 1 calc R . . C204 C 0.3159(6) 1.0240(10) 0.2225(3) 0.100(4) Uani 1 1 d . . . H20G H 0.3583 0.9899 0.2335 0.119 Uiso 1 1 calc R . . H20H H 0.2840 0.9711 0.2342 0.119 Uiso 1 1 calc R . . O301 O 0.1703(2) 0.8827(5) 0.19397(17) 0.0477(15) Uani 1 1 d . . . C301 C 0.1337(4) 0.9883(7) 0.1780(3) 0.051(2) Uani 1 1 d . . . H30B H 0.1118 0.9773 0.1443 0.061 Uiso 1 1 calc R . . H30C H 0.1613 1.0600 0.1788 0.061 Uiso 1 1 calc R . . C302 C 0.0855(4) 1.0036(9) 0.2134(4) 0.077(3) Uani 1 1 d . . . H30D H 0.0903 1.0833 0.2295 0.092 Uiso 1 1 calc R . . H30E H 0.0419 0.9961 0.1960 0.092 Uiso 1 1 calc R . . C303 C 0.0999(6) 0.9049(12) 0.2497(4) 0.120(5) Uani 1 1 d . . . H30F H 0.0995 0.9360 0.2830 0.144 Uiso 1 1 calc R . . H30G H 0.0682 0.8398 0.2434 0.144 Uiso 1 1 calc R . . C304 C 0.1633(6) 0.8594(9) 0.2444(3) 0.079(3) Uani 1 1 d . . . H30H H 0.1962 0.9022 0.2668 0.095 Uiso 1 1 calc R . . H30I H 0.1665 0.7721 0.2515 0.095 Uiso 1 1 calc R . . O401 O 0.3651(2) 0.8708(5) 0.08860(17) 0.0434(14) Uani 1 1 d . . . C401 C 0.4123(4) 0.9666(8) 0.0901(3) 0.054(2) Uani 1 1 d . . . H40A H 0.4453 0.9567 0.1187 0.065 Uiso 1 1 calc R . . H40B H 0.3923 1.0465 0.0919 0.065 Uiso 1 1 calc R . . C402 C 0.4407(5) 0.9549(9) 0.0431(4) 0.089(3) Uani 1 1 d . . . H40C H 0.4203 1.0120 0.0183 0.106 Uiso 1 1 calc R . . H40D H 0.4866 0.9715 0.0491 0.106 Uiso 1 1 calc R . . C403 C 0.4283(6) 0.8261(9) 0.0264(4) 0.107(4) Uani 1 1 d . . . H40E H 0.4108 0.8239 -0.0086 0.128 Uiso 1 1 calc R . . H40F H 0.4679 0.7789 0.0315 0.128 Uiso 1 1 calc R . . C404 C 0.3819(4) 0.7750(8) 0.0560(3) 0.056(2) Uani 1 1 d . . . H40G H 0.3437 0.7469 0.0345 0.067 Uiso 1 1 calc R . . H40H H 0.4007 0.7057 0.0753 0.067 Uiso 1 1 calc R . . O501 O 0.3982(8) 1.1367(18) -0.1512(5) 0.170(6) Uani 0.67 1 d PD . . C501 C 0.3786(10) 1.0394(12) -0.1191(7) 0.111(7) Uani 0.67 1 d PD . . H50C H 0.3465 0.9875 -0.1383 0.134 Uiso 0.67 1 calc PR . . H50D H 0.4156 0.9888 -0.1069 0.134 Uiso 0.67 1 calc PR . . C502 C 0.3555(9) 1.0846(17) -0.0828(6) 0.101(6) Uani 0.67 1 d PD . . H50A H 0.3879 1.0849 -0.0535 0.122 Uiso 0.67 1 calc PR . . H50B H 0.3193 1.0357 -0.0758 0.122 Uiso 0.67 1 calc PR . . C503 C 0.3348(10) 1.2086(16) -0.0953(8) 0.135(8) Uani 0.67 1 d PD . . H50E H 0.3342 1.2579 -0.0657 0.162 Uiso 0.67 1 calc PR . . H50F H 0.2922 1.2096 -0.1149 0.162 Uiso 0.67 1 calc PR . . C504 C 0.3836(13) 1.2532(13) -0.1243(8) 0.154(10) Uani 0.67 1 d PD . . H50G H 0.4214 1.2837 -0.1031 0.184 Uiso 0.67 1 calc PR . . H50H H 0.3665 1.3172 -0.1474 0.184 Uiso 0.67 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li3 0.040(8) 0.036(8) 0.038(8) -0.012(6) 0.005(6) 0.009(6) Li2 0.046(8) 0.039(9) 0.053(9) 0.002(7) 0.003(7) -0.004(7) Li1 0.052(9) 0.048(9) 0.045(8) 0.013(7) 0.004(7) 0.011(7) O1 0.036(3) 0.061(4) 0.033(3) 0.003(3) 0.007(2) 0.005(3) O2 0.028(3) 0.029(3) 0.032(3) -0.001(2) 0.004(2) 0.006(2) O3 0.041(3) 0.034(3) 0.023(3) -0.006(2) 0.002(2) 0.009(3) C1 0.026(4) 0.024(4) 0.017(4) -0.005(3) 0.004(3) 0.007(3) C2 0.020(4) 0.036(5) 0.021(4) 0.001(4) 0.002(3) 0.005(4) C3 0.031(5) 0.034(5) 0.023(4) 0.003(4) 0.001(4) -0.003(4) C4 0.031(4) 0.034(5) 0.030(5) -0.004(4) 0.011(4) 0.003(4) C5 0.016(4) 0.043(5) 0.044(5) -0.001(4) 0.012(4) 0.013(4) C6 0.030(5) 0.053(6) 0.049(5) 0.003(4) -0.004(4) 0.009(4) C7 0.034(5) 0.088(7) 0.060(6) 0.001(5) 0.008(4) 0.029(5) C8 0.030(5) 0.064(7) 0.072(6) 0.005(5) 0.010(4) 0.028(5) C9 0.033(5) 0.040(5) 0.030(5) -0.012(4) 0.014(4) -0.004(4) C10 0.028(4) 0.037(5) 0.024(4) 0.001(4) 0.009(4) -0.003(4) C11 0.033(5) 0.044(5) 0.028(5) 0.001(4) 0.010(4) -0.007(4) C12 0.059(6) 0.094(8) 0.041(5) 0.019(5) 0.025(5) 0.025(6) C13 0.056(6) 0.065(6) 0.035(5) 0.001(4) 0.004(4) -0.005(5) C14 0.078(7) 0.058(7) 0.044(5) 0.008(5) 0.001(5) -0.021(5) C15 0.025(4) 0.033(5) 0.032(5) 0.000(4) 0.004(4) 0.005(4) C16 0.026(4) 0.022(4) 0.021(4) 0.003(4) 0.011(3) 0.002(4) C17 0.027(4) 0.029(5) 0.029(4) 0.004(4) 0.007(4) 0.002(4) C18 0.028(4) 0.027(5) 0.030(4) -0.002(4) 0.000(4) 0.001(4) C19 0.029(4) 0.038(5) 0.032(5) 0.002(4) -0.008(4) -0.001(4) C20 0.058(6) 0.082(7) 0.057(6) -0.026(5) -0.015(5) 0.013(6) C21 0.065(6) 0.046(6) 0.054(6) -0.021(5) 0.013(5) -0.027(5) C22 0.040(5) 0.068(6) 0.031(5) -0.019(4) 0.002(4) -0.004(5) C23 0.018(4) 0.038(5) 0.040(5) 0.000(4) 0.001(4) 0.002(4) C24 0.022(4) 0.024(4) 0.026(4) -0.002(4) 0.006(3) 0.003(4) C25 0.026(4) 0.041(5) 0.039(5) 0.005(4) 0.009(4) 0.004(4) C26 0.048(5) 0.055(6) 0.055(5) 0.003(5) 0.004(4) 0.025(5) C27 0.041(5) 0.056(6) 0.077(6) 0.002(5) 0.032(5) 0.013(5) C28 0.048(5) 0.060(6) 0.048(5) -0.013(5) 0.008(4) 0.024(5) C29 0.030(4) 0.034(5) 0.023(4) -0.002(4) 0.005(4) -0.005(4) C30 0.014(4) 0.029(5) 0.025(4) 0.000(4) -0.003(3) -0.001(3) C31 0.031(4) 0.032(5) 0.024(4) 0.003(4) -0.003(3) 0.001(4) C32 0.028(4) 0.033(5) 0.029(5) 0.000(4) 0.005(4) 0.002(4) C33 0.055(6) 0.036(5) 0.036(5) 0.003(4) 0.001(4) -0.003(5) C34 0.084(7) 0.062(6) 0.059(6) 0.016(5) 0.033(5) 0.044(6) C35 0.105(8) 0.035(6) 0.074(7) 0.007(5) -0.030(6) 0.004(6) C36 0.059(6) 0.043(6) 0.064(6) 0.014(5) 0.020(5) 0.016(5) C37 0.022(4) 0.043(5) 0.033(5) 0.014(4) -0.001(4) 0.002(4) C38 0.025(4) 0.036(5) 0.028(4) 0.001(4) 0.009(3) 0.007(4) C39 0.032(4) 0.042(5) 0.026(4) -0.002(4) 0.012(4) 0.005(4) C40 0.088(7) 0.059(6) 0.043(5) -0.017(5) 0.022(5) -0.014(6) C41 0.060(6) 0.106(8) 0.047(5) 0.001(5) 0.023(5) 0.022(6) C42 0.074(6) 0.068(6) 0.028(5) 0.007(5) 0.025(4) -0.002(5) C43 0.025(4) 0.033(5) 0.026(4) -0.003(4) 0.002(3) -0.001(4) C44 0.031(4) 0.028(5) 0.035(4) -0.001(4) 0.005(3) 0.004(4) O101 0.039(3) 0.086(5) 0.037(3) 0.012(3) -0.001(3) 0.006(3) C101 0.043(6) 0.098(8) 0.050(6) 0.001(5) 0.011(5) 0.022(5) C102 0.042(5) 0.106(8) 0.037(5) 0.009(5) -0.001(4) 0.009(5) C103 0.051(6) 0.156(11) 0.046(6) 0.028(6) -0.002(5) -0.031(7) C104 0.055(6) 0.117(9) 0.042(6) 0.033(6) -0.005(5) -0.001(6) O201 0.083(4) 0.043(4) 0.056(4) -0.006(3) 0.020(3) 0.003(3) C201 0.108(9) 0.052(7) 0.085(8) -0.005(6) 0.038(6) -0.010(6) C202 0.189(13) 0.074(8) 0.063(7) -0.031(7) 0.045(8) -0.015(8) C203 0.233(17) 0.119(12) 0.063(8) -0.030(9) 0.015(9) -0.002(11) C204 0.153(11) 0.092(9) 0.047(7) -0.027(7) -0.008(7) 0.032(8) O301 0.070(4) 0.043(4) 0.031(3) 0.002(3) 0.011(3) 0.023(3) C301 0.054(6) 0.042(6) 0.058(6) 0.008(5) 0.010(5) 0.015(5) C302 0.063(7) 0.072(7) 0.105(8) -0.006(7) 0.043(6) 0.020(6) C303 0.154(12) 0.131(12) 0.095(9) 0.043(8) 0.088(9) 0.045(10) C304 0.139(10) 0.063(7) 0.039(6) 0.006(5) 0.025(6) 0.022(7) O401 0.046(3) 0.037(3) 0.051(3) -0.001(3) 0.022(3) -0.010(3) C401 0.057(6) 0.051(6) 0.059(6) -0.005(5) 0.022(5) -0.013(5) C402 0.111(9) 0.067(8) 0.104(8) -0.003(6) 0.067(7) -0.024(7) C403 0.146(11) 0.063(8) 0.138(10) -0.041(7) 0.111(9) -0.039(8) C404 0.053(6) 0.050(6) 0.067(6) -0.027(5) 0.017(5) -0.011(5) O501 0.199(16) 0.185(17) 0.142(13) 0.027(13) 0.075(11) 0.074(14) C501 0.18(2) 0.078(14) 0.067(13) 0.015(12) -0.027(13) -0.040(14) C502 0.136(16) 0.105(17) 0.077(13) 0.033(12) 0.065(12) -0.005(13) C503 0.18(2) 0.032(11) 0.20(2) -0.042(13) 0.063(18) 0.003(14) C504 0.25(3) 0.033(12) 0.17(2) 0.012(13) 0.01(2) -0.068(16) _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 Li3 O2 1.858(12) . ? Li3 O3 1.865(13) . ? Li3 O301 1.917(12) . ? Li3 C2 2.228(14) . ? Li3 Li2 2.423(18) . ? Li3 C15 2.530(14) . ? Li3 C3 2.765(14) . ? Li2 O2 1.908(14) . ? Li2 O401 1.963(14) . ? Li2 O3 1.974(13) . ? Li2 O201 2.135(14) . ? Li2 C17 2.716(15) . ? Li2 C31 2.725(14) . ? Li1 O1 1.758(14) . ? Li1 O101 1.894(13) . ? Li1 C30 2.355(14) . ? Li1 C31 2.475(15) . ? Li1 C43 2.577(15) . ? Li1 C32 2.609(15) . ? O1 C3 1.321(7) . ? O2 C17 1.328(7) . ? O3 C31 1.311(7) . ? C1 C2 1.547(8) . ? C1 C30 1.555(9) . ? C1 C44 1.568(8) . ? C1 C16 1.575(9) . ? C2 C15 1.395(8) . ? C2 C3 1.427(9) . ? C3 C4 1.444(9) . ? C4 C9 1.388(9) . ? C4 C5 1.537(9) . ? C5 C6 1.534(9) . ? C5 C8 1.537(10) . ? C5 C7 1.554(9) . ? C9 C10 1.403(9) . ? C10 C15 1.400(9) . ? C10 C11 1.542(9) . ? C11 C14 1.508(10) . ? C11 C12 1.520(9) . ? C11 C13 1.536(9) . ? C16 C29 1.390(9) . ? C16 C17 1.418(9) . ? C17 C18 1.433(9) . ? C18 C23 1.373(9) . ? C18 C19 1.545(9) . ? C19 C21 1.538(10) . ? C19 C22 1.543(9) . ? C19 C20 1.546(10) . ? C23 C24 1.393(8) . ? C24 C29 1.378(8) . ? C24 C25 1.544(9) . ? C25 C28 1.523(9) . ? C25 C27 1.525(10) . ? C25 C26 1.529(9) . ? C30 C43 1.401(9) . ? C30 C31 1.434(9) . ? C31 C32 1.420(9) . ? C32 C37 1.409(9) . ? C32 C33 1.525(10) . ? C33 C35 1.528(10) . ? C33 C34 1.535(10) . ? C33 C36 1.548(9) . ? C37 C38 1.383(9) . ? C38 C43 1.389(9) . ? C38 C39 1.539(9) . ? C39 C41 1.521(10) . ? C39 C42 1.525(9) . ? C39 C40 1.526(10) . ? O101 C104 1.429(8) . ? O101 C101 1.463(9) . ? C101 C102 1.506(10) . ? C102 C103 1.494(10) . ? C103 C104 1.406(10) . ? O201 C204 1.415(9) . ? O201 C201 1.450(10) . ? C201 C202 1.479(12) . ? C202 C203 1.505(14) . ? C203 C204 1.448(13) . ? O301 C301 1.415(8) . ? O301 C304 1.426(9) . ? C301 C302 1.505(10) . ? C302 C303 1.461(12) . ? C303 C304 1.446(13) . ? O401 C401 1.434(8) . ? O401 C404 1.446(8) . ? C401 C402 1.493(10) . ? C402 C403 1.485(12) . ? C403 C404 1.461(11) . ? O501 C501 1.470(18) . ? O501 C504 1.52(2) . ? C501 C502 1.263(18) . ? C502 C503 1.44(2) . ? C503 C504 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li3 O3 96.1(6) . . ? O2 Li3 O301 114.3(6) . . ? O3 Li3 O301 109.4(6) . . ? O2 Li3 C2 96.5(5) . . ? O3 Li3 C2 94.8(5) . . ? O301 Li3 C2 137.5(7) . . ? O2 Li3 Li2 50.9(4) . . ? O3 Li3 Li2 52.9(5) . . ? O301 Li3 Li2 101.4(6) . . ? C2 Li3 Li2 121.0(6) . . ? O2 Li3 C15 85.3(5) . . ? O3 Li3 C15 127.3(6) . . ? O301 Li3 C15 117.8(6) . . ? C2 Li3 C15 33.3(3) . . ? Li2 Li3 C15 131.2(6) . . ? O2 Li3 C3 126.8(6) . . ? O3 Li3 C3 85.5(4) . . ? O301 Li3 C3 115.0(6) . . ? C2 Li3 C3 30.9(3) . . ? Li2 Li3 C3 132.5(6) . . ? C15 Li3 C3 54.6(3) . . ? O2 Li2 O401 117.3(7) . . ? O2 Li2 O3 91.0(6) . . ? O401 Li2 O3 116.0(7) . . ? O2 Li2 O201 113.4(6) . . ? O401 Li2 O201 103.8(6) . . ? O3 Li2 O201 115.8(7) . . ? O2 Li2 Li3 49.0(4) . . ? O401 Li2 Li3 150.3(7) . . ? O3 Li2 Li3 48.9(4) . . ? O201 Li2 Li3 105.9(6) . . ? O2 Li2 C17 26.8(3) . . ? O401 Li2 C17 91.9(5) . . ? O3 Li2 C17 95.4(5) . . ? O201 Li2 C17 132.5(6) . . ? Li3 Li2 C17 67.9(5) . . ? O2 Li2 C31 95.7(5) . . ? O401 Li2 C31 90.7(5) . . ? O3 Li2 C31 26.8(3) . . ? O201 Li2 C31 135.3(6) . . ? Li3 Li2 C31 67.9(4) . . ? C17 Li2 C31 87.9(4) . . ? O1 Li1 O101 116.4(8) . . ? O1 Li1 C30 84.7(5) . . ? O101 Li1 C30 158.9(7) . . ? O1 Li1 C31 89.2(5) . . ? O101 Li1 C31 139.3(7) . . ? C30 Li1 C31 34.4(3) . . ? O1 Li1 C43 110.4(6) . . ? O101 Li1 C43 128.7(7) . . ? C30 Li1 C43 32.6(3) . . ? C31 Li1 C43 57.5(4) . . ? O1 Li1 C32 117.5(6) . . ? O101 Li1 C32 108.4(6) . . ? C30 Li1 C32 58.7(4) . . ? C31 Li1 C32 32.3(3) . . ? C43 Li1 C32 64.3(4) . . ? C3 O1 Li1 145.0(6) . . ? C17 O2 Li3 128.6(5) . . ? C17 O2 Li2 112.9(6) . . ? Li3 O2 Li2 80.1(6) . . ? C31 O3 Li3 130.0(6) . . ? C31 O3 Li2 110.5(6) . . ? Li3 O3 Li2 78.2(6) . . ? C2 C1 C30 115.4(5) . . ? C2 C1 C44 98.8(5) . . ? C30 C1 C44 110.4(5) . . ? C2 C1 C16 114.8(5) . . ? C30 C1 C16 107.3(5) . . ? C44 C1 C16 109.8(5) . . ? C15 C2 C3 119.5(6) . . ? C15 C2 C1 118.9(6) . . ? C3 C2 C1 120.3(6) . . ? C15 C2 Li3 85.3(5) . . ? C3 C2 Li3 95.8(5) . . ? C1 C2 Li3 99.9(5) . . ? O1 C3 C2 122.0(6) . . ? O1 C3 C4 119.5(6) . . ? C2 C3 C4 118.4(6) . . ? O1 C3 Li3 117.4(5) . . ? C2 C3 Li3 53.3(4) . . ? C4 C3 Li3 99.4(5) . . ? C9 C4 C3 118.3(6) . . ? C9 C4 C5 122.1(6) . . ? C3 C4 C5 119.6(6) . . ? C6 C5 C8 110.0(6) . . ? C6 C5 C4 111.4(6) . . ? C8 C5 C4 109.6(6) . . ? C6 C5 C7 106.8(6) . . ? C8 C5 C7 107.3(6) . . ? C4 C5 C7 111.6(6) . . ? C4 C9 C10 124.0(7) . . ? C15 C10 C9 116.5(6) . . ? C15 C10 C11 121.1(6) . . ? C9 C10 C11 122.2(6) . . ? C14 C11 C12 109.2(7) . . ? C14 C11 C13 107.8(7) . . ? C12 C11 C13 107.6(6) . . ? C14 C11 C10 108.3(6) . . ? C12 C11 C10 112.7(6) . . ? C13 C11 C10 111.2(6) . . ? C2 C15 C10 122.8(6) . . ? C2 C15 Li3 61.4(4) . . ? C10 C15 Li3 105.2(5) . . ? C29 C16 C17 118.2(6) . . ? C29 C16 C1 116.4(6) . . ? C17 C16 C1 125.0(6) . . ? O2 C17 C16 122.3(6) . . ? O2 C17 C18 120.0(6) . . ? C16 C17 C18 117.7(6) . . ? O2 C17 Li2 40.3(4) . . ? C16 C17 Li2 109.7(5) . . ? C18 C17 Li2 116.7(5) . . ? C23 C18 C17 119.3(6) . . ? C23 C18 C19 119.2(6) . . ? C17 C18 C19 121.3(6) . . ? C21 C19 C22 110.6(6) . . ? C21 C19 C18 109.7(6) . . ? C22 C19 C18 111.9(6) . . ? C21 C19 C20 107.1(6) . . ? C22 C19 C20 105.7(6) . . ? C18 C19 C20 111.8(6) . . ? C18 C23 C24 122.8(6) . . ? C29 C24 C23 116.6(6) . . ? C29 C24 C25 124.0(6) . . ? C23 C24 C25 119.2(6) . . ? C28 C25 C27 108.0(6) . . ? C28 C25 C26 107.9(6) . . ? C27 C25 C26 108.8(6) . . ? C28 C25 C24 112.0(6) . . ? C27 C25 C24 108.0(6) . . ? C26 C25 C24 112.0(6) . . ? C24 C29 C16 123.8(6) . . ? C43 C30 C31 118.0(6) . . ? C43 C30 C1 117.0(6) . . ? C31 C30 C1 124.8(6) . . ? C43 C30 Li1 82.5(5) . . ? C31 C30 Li1 77.4(5) . . ? C1 C30 Li1 113.4(5) . . ? O3 C31 C32 120.6(7) . . ? O3 C31 C30 121.7(6) . . ? C32 C31 C30 117.7(7) . . ? O3 C31 Li1 121.7(6) . . ? C32 C31 Li1 79.1(5) . . ? C30 C31 Li1 68.2(5) . . ? O3 C31 Li2 42.7(4) . . ? C32 C31 Li2 117.0(5) . . ? C30 C31 Li2 108.8(5) . . ? Li1 C31 Li2 161.1(5) . . ? C37 C32 C31 119.5(7) . . ? C37 C32 C33 119.6(6) . . ? C31 C32 C33 120.8(7) . . ? C37 C32 Li1 83.2(5) . . ? C31 C32 Li1 68.7(5) . . ? C33 C32 Li1 119.3(5) . . ? C32 C33 C35 110.5(6) . . ? C32 C33 C34 109.8(6) . . ? C35 C33 C34 109.8(7) . . ? C32 C33 C36 113.4(6) . . ? C35 C33 C36 105.8(6) . . ? C34 C33 C36 107.4(6) . . ? C38 C37 C32 123.3(7) . . ? C37 C38 C43 115.6(6) . . ? C37 C38 C39 123.4(7) . . ? C43 C38 C39 121.0(7) . . ? C41 C39 C42 107.0(6) . . ? C41 C39 C40 109.7(7) . . ? C42 C39 C40 108.7(6) . . ? C41 C39 C38 108.7(6) . . ? C42 C39 C38 112.3(6) . . ? C40 C39 C38 110.3(6) . . ? C38 C43 C30 124.8(7) . . ? C38 C43 Li1 88.3(5) . . ? C30 C43 Li1 64.9(4) . . ? C104 O101 C101 106.8(5) . . ? C104 O101 Li1 131.8(6) . . ? C101 O101 Li1 121.3(6) . . ? O101 C101 C102 106.9(6) . . ? C103 C102 C101 104.1(7) . . ? C104 C103 C102 106.4(7) . . ? C103 C104 O101 108.7(7) . . ? C204 O201 C201 107.5(7) . . ? C204 O201 Li2 119.1(6) . . ? C201 O201 Li2 133.3(6) . . ? O201 C201 C202 108.8(8) . . ? C201 C202 C203 101.0(9) . . ? C204 C203 C202 106.8(9) . . ? O201 C204 C203 108.0(9) . . ? C301 O301 C304 108.2(6) . . ? C301 O301 Li3 125.0(6) . . ? C304 O301 Li3 123.9(6) . . ? O301 C301 C302 106.1(7) . . ? C303 C302 C301 105.2(8) . . ? C304 C303 C302 106.6(8) . . ? O301 C304 C303 105.2(8) . . ? C401 O401 C404 108.1(6) . . ? C401 O401 Li2 125.8(6) . . ? C404 O401 Li2 125.9(6) . . ? O401 C401 C402 106.0(6) . . ? C403 C402 C401 105.6(7) . . ? C404 C403 C402 106.9(7) . . ? O401 C404 C403 107.9(7) . . ? C501 O501 C504 102.7(10) . . ? C502 C501 O501 111.0(12) . . ? C501 C502 C503 108.4(12) . . ? C502 C503 C504 103.2(13) . . ? C503 C504 O501 101.0(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.488 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.063 #===END data_8a.0.8Me2CO _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.40 H54.80 O3.80' _chemical_formula_weight 625.26 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9562(18) _cell_length_b 12.7398(17) _cell_length_c 13.4304(18) _cell_angle_alpha 97.043(5) _cell_angle_beta 90.828(4) _cell_angle_gamma 105.813(3) _cell_volume 1951.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 679 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.56 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4408 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4263 _reflns_number_gt 2473 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Bruker AXS SMART ' _computing_cell_refinement ' Bruker AXS SMART ' _computing_data_reduction ' Bruker AXS SMART ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. Residual density associated with highly a disordered solvent was located. This corresponded to one 0.8 site-occupancy acetone solvent which was subsequently removed with the Platon for Windows software program (A. L. Spek, Acta Cryst., Sect. A, 1990, 46, C-34). ; _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^)+(0.1059P)^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 4263 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2028 _refine_ls_wR_factor_gt 0.1752 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.010 _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 O1 O 0.3866(3) 0.1349(3) 1.2434(3) 0.0354(10) Uani 1 1 d . . . H1A H 0.325(5) 0.112(5) 1.241(4) 0.05(2) Uiso 1 1 d . . . O2 O 0.2666(3) 0.3756(3) 1.1664(3) 0.0317(10) Uani 1 1 d . . . H2A H 0.297(6) 0.354(6) 1.111(5) 0.09(3) Uiso 1 1 d . . . O3 O 0.3834(3) 0.1543(3) 0.8613(3) 0.0343(10) Uani 1 1 d . . . H3A H 0.364(4) 0.108(4) 0.908(4) 0.041(15) Uiso 1 1 d . . . C1 C 0.2737(4) 0.1638(4) 1.0552(4) 0.0252(13) Uani 1 1 d . . . C2 C 0.4026(4) 0.2291(3) 1.0954(3) 0.0254(12) Uani 1 1 d . . . C3 C 0.4476(4) 0.2118(3) 1.1873(4) 0.0290(13) Uani 1 1 d . . . C4 C 0.5608(4) 0.2721(4) 1.2250(4) 0.0286(13) Uani 1 1 d . . . C5 C 0.6115(4) 0.2504(4) 1.3246(4) 0.0402(15) Uani 1 1 d . . . C6 C 0.6169(5) 0.1305(4) 1.3157(4) 0.0520(17) Uani 1 1 d . . . H6A H 0.5382 0.0808 1.3023 0.078 Uiso 1 1 calc R . . H6B H 0.6501 0.1174 1.3786 0.078 Uiso 1 1 calc R . . H6C H 0.6658 0.1167 1.2604 0.078 Uiso 1 1 calc R . . C7 C 0.5403(5) 0.2770(5) 1.4129(4) 0.0560(18) Uani 1 1 d . . . H7A H 0.4602 0.2298 1.4023 0.084 Uiso 1 1 calc R . . H7B H 0.5401 0.3543 1.4179 0.084 Uiso 1 1 calc R . . H7C H 0.5750 0.2640 1.4752 0.084 Uiso 1 1 calc R . . C8 C 0.7384(4) 0.3240(5) 1.3483(4) 0.0548(17) Uani 1 1 d . . . H8A H 0.7691 0.3070 1.4105 0.082 Uiso 1 1 calc R . . H8B H 0.7390 0.4017 1.3562 0.082 Uiso 1 1 calc R . . H8C H 0.7870 0.3097 1.2929 0.082 Uiso 1 1 calc R . . C9 C 0.6226(4) 0.3528(4) 1.1714(4) 0.0308(13) Uani 1 1 d . . . H9A H 0.6970 0.3968 1.1981 0.037 Uiso 1 1 calc R . . C10 C 0.5817(4) 0.3729(4) 1.0805(4) 0.0289(13) Uani 1 1 d . . . C11 C 0.6542(4) 0.4570(4) 1.0206(4) 0.0414(15) Uani 1 1 d . . . H11A H 0.6731 0.5299 1.0604 0.062 Uiso 1 1 calc R . . H11B H 0.6104 0.4578 0.9586 0.062 Uiso 1 1 calc R . . H11C H 0.7263 0.4378 1.0038 0.062 Uiso 1 1 calc R . . C12 C 0.4713(4) 0.3116(3) 1.0447(4) 0.0285(13) Uani 1 1 d . . . H12A H 0.4409 0.3258 0.9836 0.034 Uiso 1 1 calc R . . C13 C 0.1936(4) 0.1762(4) 1.1437(4) 0.0222(15) Uani 1 1 d . . . C14 C 0.1993(4) 0.2805(4) 1.1964(4) 0.0248(16) Uani 1 1 d . . . C15 C 0.1353(4) 0.2931(4) 1.2825(4) 0.0258(15) Uani 1 1 d . . . C16 C 0.1453(4) 0.4058(4) 1.3422(4) 0.0340(16) Uani 1 1 d . . . C17 C 0.0743(4) 0.3976(5) 1.4345(4) 0.0511(17) Uani 1 1 d . . . H17A H 0.0988 0.3499 1.4771 0.077 Uiso 1 1 calc R . . H17B H -0.0083 0.3665 1.4141 0.077 Uiso 1 1 calc R . . H17C H 0.0864 0.4711 1.4720 0.077 Uiso 1 1 calc R . . C18 C 0.0992(5) 0.4769(4) 1.2738(5) 0.0568(17) Uani 1 1 d . . . H18A H 0.0159 0.4435 1.2574 0.085 Uiso 1 1 calc R . . H18B H 0.1414 0.4805 1.2118 0.085 Uiso 1 1 calc R . . H18C H 0.1112 0.5514 1.3093 0.085 Uiso 1 1 calc R . . C19 C 0.2720(4) 0.4642(4) 1.3769(4) 0.0463(15) Uani 1 1 d . . . H19A H 0.3001 0.4209 1.4219 0.069 Uiso 1 1 calc R . . H19B H 0.2769 0.5373 1.4127 0.069 Uiso 1 1 calc R . . H19C H 0.3201 0.4719 1.3183 0.069 Uiso 1 1 calc R . . C20 C 0.0624(4) 0.1977(4) 1.3110(4) 0.0326(15) Uani 1 1 d . . . H20A H 0.0182 0.2038 1.3685 0.039 Uiso 1 1 calc R . . C21 C 0.0512(4) 0.0934(4) 1.2593(4) 0.0351(15) Uani 1 1 d . . . C22 C -0.0322(5) -0.0074(4) 1.2907(4) 0.0558(18) Uani 1 1 d . . . H22A H -0.0121 -0.0733 1.2600 0.084 Uiso 1 1 calc R . . H22B H -0.1118 -0.0109 1.2685 0.084 Uiso 1 1 calc R . . H22C H -0.0271 -0.0036 1.3640 0.084 Uiso 1 1 calc R . . C23 C 0.1185(4) 0.0842(4) 1.1767(4) 0.0279(13) Uani 1 1 d . . . H23A H 0.1130 0.0133 1.1418 0.034 Uiso 1 1 calc R . . C24 C 0.2382(4) 0.2104(4) 0.9615(4) 0.0265(13) Uani 1 1 d . . . C25 C 0.2956(4) 0.2069(4) 0.8721(4) 0.0257(13) Uani 1 1 d . . . C26 C 0.2724(4) 0.2570(4) 0.7902(4) 0.0321(13) Uani 1 1 d . . . C27 C 0.3485(5) 0.2673(4) 0.6991(4) 0.0446(16) Uani 1 1 d . . . C28 C 0.3055(7) 0.3292(6) 0.6217(5) 0.087(2) Uani 1 1 d . . . H28A H 0.2276 0.2866 0.5945 0.131 Uiso 1 1 calc R . . H28B H 0.3592 0.3389 0.5669 0.131 Uiso 1 1 calc R . . H28C H 0.3023 0.4014 0.6543 0.131 Uiso 1 1 calc R . . C29 C 0.3463(5) 0.1534(4) 0.6438(4) 0.0538(18) Uani 1 1 d . . . H29A H 0.2673 0.1156 0.6161 0.081 Uiso 1 1 calc R . . H29B H 0.3700 0.1097 0.6911 0.081 Uiso 1 1 calc R . . H29C H 0.4001 0.1624 0.5891 0.081 Uiso 1 1 calc R . . C30 C 0.4742(5) 0.3326(5) 0.7336(5) 0.065(2) Uani 1 1 d . . . H30A H 0.5053 0.2933 0.7807 0.097 Uiso 1 1 calc R . . H30B H 0.4749 0.4056 0.7669 0.097 Uiso 1 1 calc R . . H30C H 0.5225 0.3404 0.6751 0.097 Uiso 1 1 calc R . . C31 C 0.1785(5) 0.3030(4) 0.7984(4) 0.0387(15) Uani 1 1 d . . . H31A H 0.1591 0.3368 0.7438 0.046 Uiso 1 1 calc R . . C32 C 0.1126(4) 0.3013(4) 0.8825(4) 0.0325(13) Uani 1 1 d . . . C33 C 0.0111(5) 0.3530(5) 0.8874(4) 0.0538(17) Uani 1 1 d . . . H33A H -0.0037 0.3734 0.8214 0.081 Uiso 1 1 calc R . . H33B H 0.0307 0.4189 0.9374 0.081 Uiso 1 1 calc R . . H33C H -0.0586 0.2999 0.9065 0.081 Uiso 1 1 calc R . . C34 C 0.1432(4) 0.2575(4) 0.9642(4) 0.0265(12) Uani 1 1 d . . . H34A H 0.1002 0.2588 1.0231 0.032 Uiso 1 1 calc R . . C35 C 0.2634(4) 0.0413(4) 1.0199(4) 0.0257(13) Uani 1 1 d . . . C36 C 0.3472(4) -0.0123(4) 1.0397(4) 0.0323(14) Uani 1 1 d . . . H36A H 0.4173 0.0282 1.0765 0.039 Uiso 1 1 calc R . . C37 C 0.3305(4) -0.1220(4) 1.0073(4) 0.0426(16) Uani 1 1 d . . . H37A H 0.3885 -0.1564 1.0230 0.051 Uiso 1 1 calc R . . C38 C 0.2307(4) -0.1833(4) 0.9520(4) 0.0393(15) Uani 1 1 d . . . H38A H 0.2195 -0.2594 0.9299 0.047 Uiso 1 1 calc R . . C39 C 0.1465(4) -0.1309(4) 0.9294(4) 0.0346(14) Uani 1 1 d . . . H39A H 0.0778 -0.1713 0.8905 0.042 Uiso 1 1 calc R . . C40 C 0.1629(4) -0.0212(4) 0.9631(4) 0.0332(14) Uani 1 1 d . . . H40A H 0.1046 0.0130 0.9476 0.040 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 O1 0.027(2) 0.036(2) 0.038(2) 0.0118(18) -0.0123(18) -0.0016(19) O2 0.039(2) 0.019(2) 0.037(3) 0.002(2) -0.0002(18) 0.0079(17) O3 0.034(2) 0.032(2) 0.040(2) 0.008(2) 0.0030(17) 0.0125(17) C1 0.021(3) 0.018(3) 0.038(3) 0.003(3) -0.004(2) 0.009(2) C2 0.024(3) 0.021(3) 0.032(3) -0.001(3) -0.005(2) 0.010(2) C3 0.026(3) 0.020(3) 0.040(3) 0.009(3) 0.002(2) 0.003(2) C4 0.026(3) 0.022(3) 0.036(3) -0.003(3) -0.005(2) 0.007(2) C5 0.034(3) 0.044(3) 0.038(4) 0.006(3) -0.014(3) 0.004(3) C6 0.051(4) 0.048(4) 0.060(4) 0.012(3) -0.024(3) 0.018(3) C7 0.051(4) 0.078(5) 0.036(4) 0.008(4) -0.014(3) 0.013(3) C8 0.043(3) 0.066(4) 0.049(4) 0.012(3) -0.023(3) 0.004(3) C9 0.026(3) 0.020(3) 0.045(3) -0.005(3) -0.008(2) 0.006(2) C10 0.030(3) 0.018(3) 0.041(3) 0.003(3) -0.001(2) 0.011(2) C11 0.033(3) 0.033(3) 0.056(4) 0.014(3) -0.004(3) 0.003(2) C12 0.026(3) 0.022(3) 0.036(3) 0.002(3) -0.004(2) 0.006(2) C13 0.025(3) 0.021(3) 0.024(3) -0.005(3) -0.002(2) 0.016(3) C14 0.025(3) 0.023(4) 0.029(4) 0.002(4) 0.000(2) 0.011(3) C15 0.024(3) 0.029(4) 0.025(3) 0.001(3) -0.011(2) 0.010(3) C16 0.032(3) 0.030(3) 0.039(4) -0.002(3) -0.006(3) 0.010(3) C17 0.034(3) 0.047(4) 0.069(5) -0.008(4) -0.003(3) 0.012(3) C18 0.063(4) 0.041(3) 0.077(5) 0.003(4) -0.005(3) 0.034(3) C19 0.039(3) 0.040(3) 0.052(4) -0.012(3) -0.004(3) 0.005(3) C20 0.032(3) 0.033(4) 0.031(4) -0.009(3) -0.005(2) 0.010(3) C21 0.035(3) 0.027(3) 0.040(4) 0.004(3) -0.001(3) 0.004(3) C22 0.054(4) 0.047(4) 0.059(4) 0.008(3) 0.016(3) -0.001(3) C23 0.028(3) 0.024(3) 0.029(3) -0.004(3) -0.004(2) 0.005(2) C24 0.029(3) 0.021(3) 0.028(3) -0.001(3) -0.009(2) 0.005(2) C25 0.028(3) 0.018(3) 0.029(3) -0.005(3) -0.002(2) 0.007(2) C26 0.040(3) 0.021(3) 0.033(3) -0.001(3) -0.003(3) 0.006(2) C27 0.056(4) 0.041(4) 0.038(4) 0.014(3) 0.004(3) 0.010(3) C28 0.118(6) 0.106(6) 0.061(5) 0.051(5) 0.023(4) 0.052(5) C29 0.068(4) 0.043(4) 0.041(4) -0.010(3) 0.004(3) 0.007(3) C30 0.063(4) 0.044(4) 0.070(5) 0.001(4) 0.017(3) -0.013(3) C31 0.051(4) 0.031(3) 0.032(3) 0.009(3) -0.012(3) 0.007(3) C32 0.032(3) 0.028(3) 0.039(4) 0.006(3) -0.005(3) 0.010(2) C33 0.053(4) 0.060(4) 0.061(4) 0.015(4) -0.002(3) 0.034(3) C34 0.026(3) 0.024(3) 0.029(3) -0.004(3) -0.004(2) 0.010(2) C35 0.023(3) 0.019(3) 0.036(3) 0.003(3) 0.000(2) 0.008(2) C36 0.022(3) 0.027(3) 0.049(4) 0.004(3) -0.002(2) 0.010(2) C37 0.029(3) 0.029(3) 0.074(4) 0.010(3) -0.004(3) 0.014(3) C38 0.037(3) 0.019(3) 0.061(4) -0.004(3) 0.004(3) 0.010(3) C39 0.031(3) 0.026(3) 0.044(4) 0.001(3) -0.008(2) 0.003(2) C40 0.025(3) 0.026(3) 0.048(4) 0.008(3) -0.003(2) 0.005(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 O1 C3 1.366(5) . ? O2 C14 1.370(5) . ? O3 C25 1.392(5) . ? C1 C35 1.545(6) . ? C1 C24 1.556(6) . ? C1 C13 1.558(7) . ? C1 C2 1.589(6) . ? C2 C12 1.401(6) . ? C2 C3 1.404(6) . ? C3 C4 1.413(6) . ? C4 C9 1.380(6) . ? C4 C5 1.547(6) . ? C5 C7 1.527(8) . ? C5 C6 1.537(7) . ? C5 C8 1.555(7) . ? C9 C10 1.387(6) . ? C10 C12 1.383(6) . ? C10 C11 1.507(6) . ? C13 C23 1.394(6) . ? C13 C14 1.411(6) . ? C14 C15 1.412(7) . ? C15 C20 1.389(6) . ? C15 C16 1.530(7) . ? C16 C17 1.510(7) . ? C16 C19 1.532(7) . ? C16 C18 1.559(7) . ? C20 C21 1.391(7) . ? C21 C23 1.393(7) . ? C21 C22 1.506(6) . ? C24 C25 1.392(6) . ? C24 C34 1.421(6) . ? C25 C26 1.399(6) . ? C26 C31 1.401(7) . ? C26 C27 1.533(7) . ? C27 C30 1.539(7) . ? C27 C29 1.540(7) . ? C27 C28 1.541(8) . ? C31 C32 1.385(7) . ? C32 C34 1.378(6) . ? C32 C33 1.528(7) . ? C35 C36 1.397(6) . ? C35 C40 1.401(6) . ? C36 C37 1.370(7) . ? C37 C38 1.382(7) . ? C38 C39 1.400(7) . ? C39 C40 1.375(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 C35 C1 C24 105.7(4) . . ? C35 C1 C13 111.0(4) . . ? C24 C1 C13 111.7(4) . . ? C35 C1 C2 111.4(4) . . ? C24 C1 C2 110.7(3) . . ? C13 C1 C2 106.5(4) . . ? C12 C2 C3 117.9(4) . . ? C12 C2 C1 121.2(4) . . ? C3 C2 C1 120.7(4) . . ? O1 C3 C2 122.4(4) . . ? O1 C3 C4 116.6(4) . . ? C2 C3 C4 121.0(4) . . ? C9 C4 C3 117.6(4) . . ? C9 C4 C5 121.4(4) . . ? C3 C4 C5 120.9(4) . . ? C7 C5 C6 111.2(4) . . ? C7 C5 C4 111.0(4) . . ? C6 C5 C4 109.7(4) . . ? C7 C5 C8 106.9(4) . . ? C6 C5 C8 106.6(4) . . ? C4 C5 C8 111.2(4) . . ? C4 C9 C10 123.3(4) . . ? C12 C10 C9 117.7(4) . . ? C12 C10 C11 120.2(4) . . ? C9 C10 C11 122.1(4) . . ? C10 C12 C2 122.3(4) . . ? C23 C13 C14 117.9(5) . . ? C23 C13 C1 121.0(5) . . ? C14 C13 C1 121.0(4) . . ? O2 C14 C13 121.8(4) . . ? O2 C14 C15 116.1(5) . . ? C13 C14 C15 122.1(5) . . ? C20 C15 C14 116.7(5) . . ? C20 C15 C16 121.2(5) . . ? C14 C15 C16 122.1(5) . . ? C17 C16 C15 112.3(4) . . ? C17 C16 C19 107.6(4) . . ? C15 C16 C19 110.8(4) . . ? C17 C16 C18 107.9(5) . . ? C15 C16 C18 108.7(4) . . ? C19 C16 C18 109.5(4) . . ? C15 C20 C21 123.2(5) . . ? C20 C21 C23 118.4(5) . . ? C20 C21 C22 121.4(5) . . ? C23 C21 C22 120.3(5) . . ? C21 C23 C13 121.7(5) . . ? C25 C24 C34 117.3(4) . . ? C25 C24 C1 122.4(4) . . ? C34 C24 C1 120.3(4) . . ? O3 C25 C24 120.5(4) . . ? O3 C25 C26 116.0(4) . . ? C24 C25 C26 123.4(5) . . ? C25 C26 C31 115.9(5) . . ? C25 C26 C27 122.5(5) . . ? C31 C26 C27 121.5(4) . . ? C26 C27 C30 109.5(5) . . ? C26 C27 C29 111.3(4) . . ? C30 C27 C29 110.2(5) . . ? C26 C27 C28 111.6(5) . . ? C30 C27 C28 107.6(5) . . ? C29 C27 C28 106.5(5) . . ? C32 C31 C26 123.0(4) . . ? C34 C32 C31 119.2(5) . . ? C34 C32 C33 120.0(5) . . ? C31 C32 C33 120.7(4) . . ? C32 C34 C24 120.8(5) . . ? C36 C35 C40 117.1(5) . . ? C36 C35 C1 125.0(4) . . ? C40 C35 C1 117.9(4) . . ? C37 C36 C35 121.5(5) . . ? C36 C37 C38 121.1(5) . . ? C37 C38 C39 118.5(5) . . ? C40 C39 C38 120.2(5) . . ? C39 C40 C35 121.6(5) . . ? _diffrn_measured_fraction_theta_max 0.757 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.757 _refine_diff_density_max 0.233 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.052