# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1702 data_global _publ_requested_journal ChemComm _publ_contact_author ; Henk Hiemstra Institute of Molecular Chemistry Laboratory of Organic Chemistry Nieuwe Achtergracht 129 1018 WS Amsterdam The Netherlands ; _publ_contact_author_email henkh@org.chem.uva.nl _publ_section_title ; ? ; _publ_section_references ; ? ; data_o11bla #------------------------------------------------------------------------------ _audit_creation_date 00-04-28 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Enraf-Nonius CAD4 software' _computing_cell_refinement 'CELCON prog. comparable with xtal_LATCON' _computing_data_reduction 'xtal_ADDREF (Davenport &Hall, 1992)' _computing_structure_solution 'CRUNCH (de Gelder et al., 1993)' _computing_structure_refinement 'xtal_CRYLSQ (Olthof_Hazekamp, 1992)' _computing_publication_material 'xtal_BONDLA_(Dreissig,Doherty,Stewart&Hall,1992)_CIFIO (Hall,1992)' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_weight 292.3 #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_sum ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural 'C16 H20 O5' #ActaC _chemical_melting_point 177-178 #ActaC #------------------------------------------------------------------------------ _cell_length_a 14.2190(10) #ActaC _cell_length_b 7.3084(7) #ActaC _cell_length_c 14.697(2) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 111.047(10) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 1425.4(3) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 270 #ActaC _cell_measurement_reflns_used 23 #ActaC _cell_measurement_theta_min 40.02 #ActaC _cell_measurement_theta_max 44.84 #ActaC #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/c_1 #ActaC _symmetry_space_group_name_Hall -p_2ybc #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description block #ActaC _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.50 #ActaC _exptl_crystal_size_mid 0.45 #ActaC _exptl_crystal_size_min 0.40 #ActaC _exptl_crystal_density_diffrn 1.362 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 624 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 0.83 #ActaC _exptl_absorpt_correction_type none #ActaC _exptl_absorpt_correction_T_min ? #ActaC _exptl_absorpt_correction_T_max ? #ActaC _exptl_special_details #ActaC ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 270 #ActaC _diffrn_radiation_wavelength 1.5418 #ActaC _diffrn_radiation_type 'Cu K\a' #ActaC _diffrn_radiation_source Xray-tube #ActaC _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'ENRAF NONIUS CAD4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 20 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 2 -2 1 3 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 2924 #ActaC _diffrn_reflns_av_R_equivalents ? #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min -17 #ActaC _diffrn_reflns_limit_h_max 0 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 9 #ActaC _diffrn_reflns_limit_l_min -16 #ActaC _diffrn_reflns_limit_l_max 18 #ActaC _diffrn_reflns_theta_min 3.33 #ActaC _diffrn_reflns_theta_max 75.12 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC #----------------------------------------------------------------------------- loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 64 .017 .009 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 80 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 20 .047 .032 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 #----------------------------------------------------------------------------- loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC C1 .32099(17) .0964(3) .43535(16) .0334(10) Uani ? ? C2 .20246(18) .1117(3) .36777(16) .0374(11) Uani ? ? C3 .21311(18) .2897(3) .42795(16) .0361(10) Uani ? ? C4 .29611(17) .2003(3) .51605(16) .0320(10) Uani ? ? C5 .36152(18) -.0933(3) .45439(17) .0362(11) Uani ? ? C6 .31604(19) -.0857(3) .60213(16) .0364(10) Uani ? ? C7 .4154(2) -.0516(4) .6823(2) .0509(14) Uani ? ? C8 .2499(2) -.2147(4) .6329(2) .0500(14) Uani ? ? C9 .3686(2) .3335(3) .58714(19) .0425(12) Uani ? ? C10 .1225(2) -.0236(4) .36925(19) .0462(12) Uani ? ? C11 .0266(2) .0843(5) .3597(2) .0579(15) Uani ? ? C12 .0436(2) .2316(4) .4372(2) .0549(15) Uani ? ? C13 .1187(2) .3777(4) .4315(2) .0470(13) Uani ? ? C14 .3668(2) .2494(4) .3946(2) .0436(12) Uani ? ? C15 .2764(2) .3821(3) .37329(19) .0440(12) Uani ? ? C16 .1834(2) .1768(4) .26514(18) .0493(13) Uani ? ? O1 .34063(14) -.1830(2) .52454(12) .0440(8) Uani ? ? O2 .25611(12) .0706(2) .56555(11) .0343(7) Uani ? ? O3 .40110(15) -.1729(2) .40640(13) .0522(10) Uani ? ? O4 .21690(15) .3540(2) .27094(13) .0541(10) Uani ? ? O5 .14415(18) .1012(3) .18939(13) .0721(12) Uani ? ? H71 .448(2) -.169(2) .712(2) .077(10) Uiso ? ? H72 .4646(18) .013(4) .659(2) .072(10) Uiso ? ? H73 .399(2) .014(4) .7346(16) .067(9) Uiso ? ? H81 .1860(14) -.238(5) .5768(16) .079(11) Uiso ? ? H82 .296(2) -.320(3) .663(2) .078(10) Uiso ? ? H83 .231(2) -.156(4) .6855(16) .071(10) Uiso ? ? H91 .345(2) .350(4) .6423(15) .062(9) Uiso ? ? H92 .4387(11) .288(4) .609(2) .069(9) Uiso ? ? H93 .378(2) .445(3) .5521(18) .061(9) Uiso ? ? H101 .1108(18) -.105(3) .3105(12) .045(7) Uiso ? ? H102 .144(2) -.091(4) .4322(13) .067(9) Uiso ? ? H111 .003(2) .143(4) .2939(12) .079(11) Uiso ? ? H112 -.0243(18) .001(4) .371(2) .076(10) Uiso ? ? H121 -.0188(15) .299(4) .433(2) .073(10) Uiso ? ? H122 .070(2) .173(4) .5028(12) .068(9) Uiso ? ? H131 .089(2) .448(4) .3689(13) .068(9) Uiso ? ? H132 .134(2) .461(4) .4891(15) .077(10) Uiso ? ? H141 .4302(12) .293(4) .4461(14) .050(8) Uiso ? ? H142 .3777(18) .220(3) .3325(11) .042(7) Uiso ? ? H15 .298(2) .5128(18) .384(2) .077(10) Uiso ? ? #----------------------------------------------------------------------------- loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC C1 .0427(12) .0235(11) .0346(11) .0042(9) .0145(10) .0002(9) C2 .0496(14) .0277(11) .0320(11) .0012(10) .0112(10) -.0008(9) C3 .0458(13) .0225(11) .0369(12) .0029(9) .0110(10) .0003(9) C4 .0404(12) .0199(10) .0354(11) .0002(9) .0132(10) -.0011(9) C5 .0443(13) .0266(11) .0389(12) .0056(10) .0162(10) -.0011(9) C6 .0533(14) .0235(11) .0339(11) .0089(10) .0174(10) .0031(9) C7 .0581(17) .0433(16) .0463(15) .0135(13) .0129(13) .0084(12) C8 .073(2) .0295(13) .0561(17) .0017(13) .0333(15) .0057(12) C9 .0507(15) .0271(12) .0423(14) -.0018(11) .0079(11) -.0061(11) C10 .0532(15) .0366(14) .0399(14) -.0088(12) .0059(12) -.0056(11) C11 .0467(16) .0586(18) .0573(17) -.0085(14) .0052(13) .0005(15) C12 .0442(15) .0585(18) .0597(18) .0060(13) .0158(13) .0004(15) C13 .0523(15) .0345(13) .0491(15) .0112(11) .0121(12) .0013(12) C14 .0546(16) .0332(13) .0480(15) .0002(11) .0245(12) .0063(11) C15 .0574(16) .0271(12) .0442(14) .0003(11) .0142(12) .0077(10) C16 .0635(17) .0446(15) .0351(13) .0029(13) .0118(12) .0042(11) O1 .0738(12) .0212(8) .0440(9) .0108(8) .0296(9) .0021(7) O2 .0463(9) .0225(7) .0355(8) .0049(6) .0164(7) .0022(6) O3 .0733(13) .0359(10) .0586(11) .0139(9) .0374(10) -.0024(8) O4 .0765(13) .0411(10) .0414(10) .0030(9) .0171(9) .0122(8) O5 .1037(18) .0657(14) .0358(10) -.0016(13) .0114(11) -.0067(10) #----------------------------------------------------------------------------- _atom_sites_solution_primary 'Direct Methods' _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens calculated #----------------------------------------------------------------------------- _refine_special_details sfls:_F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme '1/[0.5+0.01*\s(Fobs)^2^+0.01/\s(Fobs)]' _refine_ls_hydrogen_treatment 'H-atom x,y,z,U refined, restrained at 1.0 \%A' _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 3138(188) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 2510 #ActaC _refine_ls_number_parameters 271 #ActaC _refine_ls_number_restraints 20 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .061 #ActaC _refine_ls_R_factor_obs .056 #ActaC _refine_ls_wR_factor_all .055 #ActaC _refine_ls_wR_factor_obs .053 #ActaC _refine_ls_goodness_of_fit_all 1.031 #ActaC _refine_ls_goodness_of_fit_obs 1.09 #ActaC _refine_ls_shift/esd_max .621 #ActaC _refine_ls_shift/esd_mean .057 #ActaC _refine_diff_density_min -.296 #ActaC _refine_diff_density_max .261 #ActaC #----------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC C1 C5 1.489(3) . . ? C1 C14 1.521(4) . . ? C1 C4 1.552(4) . . ? C1 C2 1.624(3) . . ? C2 C16 1.510(4) . . ? C2 C10 1.513(4) . . ? C2 C3 1.550(3) . . ? C3 C13 1.507(4) . . ? C3 C4 1.549(3) . . ? C3 C15 1.559(4) . . ? C4 O2 1.431(3) . . ? C4 C9 1.526(3) . . ? C5 O3 1.199(4) . . ? C5 O1 1.342(3) . . ? C6 O2 1.410(3) . . ? C6 O1 1.488(3) . . ? C6 C7 1.500(3) . . ? C6 C8 1.511(4) . . ? C7 H71 1.00(2) . . ? C7 H72 1.00(3) . . ? C7 H73 1.00(3) . . ? C8 H81 .998(18) . . ? C8 H83 1.00(3) . . ? C8 H82 1.00(2) . . ? C9 H92 .989(17) . . ? C9 H91 .99(3) . . ? C9 H93 1.00(2) . . ? C10 H102 1.00(2) . . ? C10 H101 1.01(2) . . ? C10 C11 1.537(4) . . ? C11 H111 1.00(2) . . ? C11 H112 1.00(3) . . ? C11 C12 1.522(5) . . ? C12 H122 1.00(2) . . ? C12 H121 1.00(2) . . ? C12 C13 1.534(4) . . ? C13 H132 1.00(2) . . ? C13 H131 1.00(2) . . ? C14 H141 .998(17) . . ? C14 H142 1.00(2) . . ? C14 C15 1.550(4) . . ? C15 H15 .998(15) . . ? C15 O4 1.451(3) . . ? C16 O5 1.188(3) . . ? C16 O4 1.372(3) . . ? #----------------------------------------------------------------------------- #----------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC H92 H93 1.50(3) . . ? H71 H72 1.60(4) . . ? H121 H122 1.60(3) . . ? H71 H73 1.60(4) . . ? H81 H83 1.61(3) . . ? H82 H83 1.62(4) . . ? H91 H92 1.64(4) . . ? H131 H132 1.65(3) . . ? H141 H142 1.65(3) . . ? H111 H112 1.68(4) . . ? H101 H102 1.68(3) . . ? H72 H73 1.69(5) . . ? H91 H93 1.71(4) . . ? H81 H82 1.73(3) . . ? C6 H82 2.00(3) . . ? C12 H112 2.01(3) . . ? C6 H73 2.01(2) . . ? O4 H15 2.02(2) . . ? C3 H131 2.02(3) . . ? C2 H101 2.03(2) . . ? C13 H121 2.05(2) . . ? C4 H91 2.05(2) . . ? C1 C3 2.059(3) . . ? C10 H111 2.06(3) . . ? C6 H83 2.07(3) . . ? C11 H102 2.07(3) . . ? C11 H122 2.072(18) . . ? C6 H81 2.07(3) . . ? C1 H141 2.08(2) . . ? C12 H111 2.08(2) . . ? C6 H71 2.08(2) . . ? C12 H132 2.08(3) . . ? C13 H122 2.08(3) . . ? C2 H102 2.09(3) . . ? C3 H132 2.09(3) . . ? C4 H93 2.09(2) . . ? C12 H131 2.10(3) . . ? C4 H92 2.099(17) . . ? C10 H112 2.10(3) . . ? C6 H72 2.10(2) . . ? C15 H142 2.11(3) . . ? C11 H101 2.12(2) . . ? H72 H92 2.12(4) . . ? C11 H121 2.13(3) . . ? C14 H15 2.141(19) . . ? C1 H142 2.15(2) . . ? C15 H141 2.162(17) . . ? O1 O3 2.198(3) . . ? C2 C4 2.204(3) . . ? C2 C15 2.226(3) . . ? C15 C16 2.240(3) . . ? O4 O5 2.243(3) . . ? H93 H141 2.24(4) . . ? C3 H15 2.25(3) . . ? H81 H102 2.26(3) . . ? C1 C15 2.275(3) . . ? H112 H122 2.30(3) . . ? H71 H82 2.30(4) . . ? C8 O2 2.323(3) . . ? H122 H132 2.32(4) . . ? C2 O4 2.327(3) . . ? H102 H112 2.33(4) . . ? H101 H111 2.33(4) . . ? H121 H131 2.34(4) . . ? H121 H132 2.34(4) . . ? O4 H142 2.35(2) . . ? H112 H121 2.35(4) . . ? O2 H102 2.36(2) . . ? H92 H141 2.36(4) . . ? C4 C14 2.369(4) . . ? H93 H15 2.37(4) . . ? H81 H121 2.37(3) . 3_556 ? C3 O4 2.375(3) . . ? C14 O4 2.377(3) . . ? C7 O1 2.379(3) . . ? C1 O3 2.388(3) . . ? C1 O1 2.388(3) . . ? H141 H15 2.39(3) . . ? C8 O1 2.394(4) . . ? O1 O2 2.400(2) . . ? C4 C6 2.406(3) . . ? C1 O2 2.412(3) . . ? C4 C15 2.413(4) . . ? C3 C16 2.421(4) . . ? C3 C14 2.423(4) . . ? C2 C14 2.443(4) . . ? C9 O2 2.447(3) . . ? O2 H91 2.45(3) . . ? C2 O5 2.450(3) . . ? H111 H121 2.46(4) . . ? C7 O2 2.466(3) . . ? C2 C11 2.470(4) . . ? C3 O2 2.478(3) . . ? C5 C6 2.479(4) . . ? C10 C16 2.488(4) . . ? O2 H81 2.49(3) . . ? C3 C12 2.499(4) . . ? C16 H101 2.50(2) . . ? C7 C8 2.501(4) . . ? H73 H142 2.50(4) . 4 ? O5 H101 2.50(2) . . ? H101 H112 2.51(4) . . ? O3 H92 2.51(2) . 3_656 ? H112 H122 2.52(4) . 3_556 ? H81 H132 2.53(4) . 1_545 ? O2 H83 2.53(3) . . ? C11 C13 2.536(4) . . ? O1 H82 2.54(3) . . ? C9 H141 2.54(2) . . ? C7 H82 2.54(2) . . ? C15 H93 2.55(2) . . ? H73 H83 2.55(4) . . ? H82 H91 2.56(4) . 1_545 ? C10 C12 2.557(5) . . ? C4 H141 2.56(2) . . ? H71 H92 2.56(4) . 2_646 ? O1 H72 2.57(3) . . ? H101 H111 2.57(3) . 2_545 ? O4 H83 2.58(3) . 4_554 ? O2 H122 2.58(3) . . ? H102 H122 2.59(4) . . ? H111 H131 2.59(4) . . ? C16 H142 2.60(2) . . ? C3 C9 2.598(3) . . ? O1 H81 2.61(2) . . ? O2 H73 2.61(2) . . ? C3 C10 2.617(3) . . ? C2 C13 2.622(4) . . ? O1 H71 2.63(3) . . ? C4 C5 2.626(3) . . ? C2 C5 2.629(3) . . ? C1 C16 2.630(3) . . ? C3 H93 2.65(2) . . ? C8 H71 2.66(3) . . ? C2 H111 2.66(3) . . ? H142 H15 2.66(4) . . ? C5 C14 2.664(4) . . ? C13 C15 2.672(5) . . ? C14 C16 2.672(3) . . ? C14 H93 2.67(3) . . ? C15 H131 2.68(3) . . ? O3 H15 2.68(2) . 1_545 ? H111 H131 2.69(3) . 2_545 ? C8 H73 2.69(3) . . ? O3 H72 2.70(3) . 3_656 ? C4 C13 2.709(3) . . ? H91 H142 2.71(3) . 4 ? C1 C9 2.711(3) . . ? C13 H111 2.71(2) . . ? O1 H102 2.72(3) . . ? C9 H72 2.72(3) . . ? O3 H141 2.736(17) . 3_656 ? C7 H83 2.74(3) . . ? C2 O2 2.744(3) . . ? C10 H122 2.74(3) . . ? C16 H111 2.76(3) . . ? C12 H102 2.77(3) . . ? C7 H92 2.77(3) . . ? C3 H122 2.77(3) . . ? H73 H91 2.78(4) . . ? O1 H93 2.776(19) . 1_545 ? C1 C10 2.777(4) . . ? O4 H131 2.78(3) . . ? H72 H142 2.78(4) . 3_656 ? C11 H131 2.79(3) . . ? H71 H142 2.80(4) . 3_656 ? C6 H102 2.80(2) . . ? C1 C6 2.812(3) . . ? O2 H72 2.82(2) . . ? C2 H142 2.83(3) . . ? C5 O2 2.847(3) . . ? H73 H82 2.85(3) . . ? H102 H111 2.85(3) . . ? C1 H102 2.86(3) . . ? C4 O1 2.864(3) . . ? C1 H92 2.87(3) . . ? H111 H122 2.88(2) . . ? H82 H93 2.88(4) . 1_545 ? C9 C14 2.886(4) . . ? H122 H131 2.89(4) . . ? C3 C11 2.896(4) . . ? H121 H132 2.90(4) . 3_566 ? C4 H72 2.90(2) . . ? C4 H132 2.91(3) . . ? C10 O2 2.910(3) . . ? H73 H92 2.91(4) . . ? O2 H92 2.91(2) . . ? C10 O5 2.915(4) . . ? H83 H15 2.92(4) . 4 ? C2 C12 2.927(5) . . ? O5 H132 2.93(2) . 4_554 ? H131 H15 2.93(4) . . ? C8 H102 2.931(18) . . ? C2 H131 2.94(3) . . ? C5 H72 2.94(3) . . ? O1 H15 2.94(2) . 1_545 ? O5 H111 2.95(3) . . ? H72 H91 2.95(4) . . ? H71 H91 2.96(3) . 2_646 ? C14 H92 2.96(3) . . ? C9 C15 2.960(4) . . ? C3 H102 2.96(3) . . ? C5 H142 2.96(2) . . ? H71 H83 2.97(4) . . ? H71 H72 2.97(3) . 2_646 ? C4 H102 2.97(3) . . ? O4 H112 2.98(2) . 2 ? O4 H73 2.98(3) . 4_554 ? H83 H112 2.98(4) . 3_556 ? C5 H102 3.00(3) . . ? O5 H121 3.00(3) . 2_545 ? C4 H15 3.00(3) . . ? C1 O4 3.001(3) . . ? C3 H141 3.001(19) . . ? C5 H141 3.00(3) . . ? C1 H93 3.01(2) . . ? H73 H15 3.03(5) . 4 ? C13 H15 3.04(3) . . ? O3 H142 3.04(2) . . ? C4 C7 3.043(3) . . ? O5 H122 3.04(2) . 4_554 ? C3 H91 3.06(2) . . ? C9 H15 3.08(3) . . ? C10 C13 3.078(4) . . ? H83 H121 3.08(3) . 3_556 ? H71 H73 3.08(4) . 2_646 ? C14 H73 3.08(3) . 4_554 ? C5 H15 3.083(16) . 1_545 ? C16 H131 3.08(3) . . ? C9 H82 3.09(3) . 1_565 ? H73 H92 3.09(3) . 2_646 ? C7 H91 3.09(3) . . ? C11 C16 3.097(5) . . ? C4 C10 3.099(3) . . ? O5 H82 3.10(3) . 4_544 ? C7 C9 3.107(4) . . ? C9 H73 3.11(3) . . ? C16 H15 3.11(2) . . ? C14 O3 3.120(3) . . ? C3 H111 3.12(3) . . ? C1 H15 3.123(15) . . ? H101 H131 3.13(3) . 2_545 ? C15 H132 3.13(3) . . ? C8 H121 3.14(2) . 3_556 ? H91 H132 3.14(3) . . ? C13 O4 3.149(4) . . ? C5 H141 3.150(19) . 3_656 ? O2 H82 3.15(2) . . ? C4 H122 3.16(3) . . ? C13 O2 3.158(3) . . ? C12 O2 3.159(3) . . ? C9 H71 3.16(2) . 2_656 ? C5 C7 3.172(4) . . ? C3 H142 3.17(3) . . ? C6 C9 3.179(3) . . ? O5 H91 3.19(3) . 4_554 ? H82 H132 3.19(3) . 1_545 ? H81 H112 3.19(4) . 3_556 ? C12 H81 3.20(2) . 3_556 ? C2 H15 3.202(18) . . ? H122 H122 3.21(4) . 3_556 ? C15 H73 3.21(3) . 4_554 ? C8 H132 3.21(2) . 1_545 ? C5 C10 3.213(4) . . ? C6 H92 3.22(3) . . ? C2 H122 3.22(3) . . ? O4 H141 3.228(16) . . ? O1 H141 3.231(19) . 3_656 ? O1 H73 3.23(2) . . ? C6 H91 3.24(3) . . ? C7 H92 3.24(2) . 2_646 ? C1 H101 3.24(2) . . ? H132 H15 3.25(5) . . ? C1 H72 3.25(3) . . ? C2 O1 3.249(3) . . ? C10 H81 3.26(3) . . ? C13 C16 3.255(4) . . ? C9 H132 3.26(3) . . ? H93 H132 3.26(4) . . ? C7 H142 3.27(3) . 3_656 ? O1 H83 3.27(3) . . ? C15 H83 3.28(3) . 4_554 ? O2 H93 3.28(2) . . ? O5 H81 3.29(3) . 4_544 ? H73 H141 3.30(3) . 4 ? C2 H141 3.299(19) . . ? C4 H142 3.30(2) . . ? O2 H71 3.31(2) . . ? C4 H73 3.31(2) . . ? O2 O4 3.307(3) . 4 ? O5 H131 3.31(3) . 2_545 ? O2 H132 3.32(3) . . ? C11 H131 3.320(19) . 2_545 ? C3 H121 3.33(2) . . ? H93 H141 3.33(4) . 3_666 ? H112 H131 3.33(4) . 2_545 ? C10 O1 3.332(3) . . ? O5 H112 3.34(3) . 2 ? C2 H112 3.34(3) . . ? O5 H142 3.34(2) . . ? C16 H102 3.35(3) . . ? C13 H112 3.35(3) . . ? O3 H82 3.35(3) . 4_544 ? C3 H92 3.355(17) . . ? C7 H81 3.36(2) . . ? C4 C12 3.362(4) . . ? H72 H141 3.36(4) . 3_656 ? O3 H71 3.37(3) . 4_544 ? C8 H72 3.38(3) . . ? C15 O5 3.377(3) . . ? C11 H132 3.38(2) . . ? C14 H72 3.38(3) . 3_656 ? C16 H112 3.39(2) . 2 ? C2 O3 3.388(3) . . ? C12 H112 3.39(3) . 3_556 ? C11 H122 3.39(3) . 3_556 ? H102 H132 3.39(4) . 1_545 ? C16 H91 3.40(3) . 4_554 ? O4 H91 3.40(3) . 4_554 ? H72 H91 3.41(3) . 2_646 ? C3 H101 3.41(2) . . ? H83 H101 3.41(4) . 4_545 ? H101 H121 3.41(3) . 2_545 ? H81 H122 3.41(4) . . ? H101 H131 3.42(3) . 1_545 ? C12 H101 3.42(2) . . ? C11 H101 3.42(2) . 2 ? C5 H101 3.43(2) . . ? H72 H82 3.43(4) . . ? H81 H122 3.43(3) . 3_556 ? C10 H111 3.44(2) . 2_545 ? C10 H121 3.44(3) . . ? C8 O5 3.439(4) . 4_545 ? C8 H91 3.44(3) . 1_545 ? C7 H71 3.44(2) . 2_656 ? C3 C5 3.442(3) . . ? C13 H102 3.45(3) . . ? C9 O3 3.447(4) . 3_656 ? C2 H132 3.45(3) . . ? C7 H142 3.45(2) . 4 ? H102 H121 3.45(4) . 3_556 ? C13 H81 3.45(3) . 1_565 ? O3 H141 3.45(3) . . ? H83 H111 3.45(5) . 3_556 ? C4 C16 3.457(3) . . ? C8 O4 3.459(4) . 4 ? C4 H131 3.47(2) . . ? H121 H121 3.47(4) . 3_566 ? C1 H91 3.47(2) . . ? H71 H141 3.47(4) . 3_656 ? C15 H92 3.48(2) . . ? C11 O5 3.477(5) . . ? C10 H131 3.48(3) . . ? C9 C13 3.483(4) . . ? O5 H83 3.49(3) . 4_544 ? C5 H72 3.50(3) . 3_656 ? H112 H121 3.50(4) . 3_556 ? H102 H131 3.50(4) . 1_545 ? H83 H102 3.51(3) . . ? C13 H93 3.51(3) . . ? O3 H83 3.51(2) . 4_544 ? C5 H92 3.51(3) . . ? C1 C13 3.520(4) . . ? C11 H83 3.52(3) . 3_556 ? C7 H91 3.53(2) . 2_646 ? H91 H141 3.53(4) . . ? C8 H93 3.53(3) . 1_545 ? O4 H111 3.54(3) . . ? O3 H73 3.54(3) . 4_544 ? H72 H93 3.54(3) . . ? C2 C6 3.544(3) . . ? H102 H122 3.55(4) . 3_556 ? C4 O4 3.549(3) . . ? C8 H112 3.55(3) . 3_556 ? C6 O3 3.556(4) . . ? C1 C7 3.557(4) . . ? C14 H71 3.56(4) . 3_656 ? H71 H93 3.56(3) . 2_646 ? C3 O5 3.561(3) . . ? C11 O2 3.567(3) . . ? C6 C10 3.568(3) . . ? H71 H81 3.57(3) . . ? C5 H71 3.57(3) . . ? H71 H93 3.58(3) . 1_545 ? O3 H93 3.58(3) . 3_656 ? H72 H92 3.58(4) . 2_646 ? C13 H91 3.58(2) . . ? C14 O3 3.581(3) . 3_656 ? C9 H142 3.582(19) . 4 ? C1 O5 3.586(3) . . ? C5 H92 3.59(2) . 3_656 ? H73 H81 3.59(3) . . ? H92 H15 3.59(4) . . ? C10 O4 3.592(4) . . ? O4 H111 3.60(3) . 2 ? C5 C16 3.604(3) . . ? H73 H93 3.61(3) . 2_646 ? O3 H93 3.61(2) . 1_545 ? H112 H112 3.61(5) . 3_556 ? H93 H142 3.62(3) . . ? H72 H141 3.62(4) . . ? C2 C9 3.624(3) . . ? C12 H122 3.63(3) . 3_556 ? C5 C8 3.630(5) . . ? C9 O1 3.638(3) . 1_565 ? C5 H93 3.64(2) . 1_545 ? C11 H81 3.65(3) . 3_556 ? C9 H73 3.65(2) . 2_656 ? C14 O2 3.652(4) . . ? C15 O3 3.652(3) . 1_565 ? C16 H82 3.65(3) . 4_544 ? C4 C8 3.659(4) . . ? C5 C9 3.661(3) . . ? C16 H141 3.661(16) . . ? C14 O5 3.666(3) . . ? C12 O5 3.670(4) . 4 ? C10 C15 3.673(4) . . ? O1 H101 3.676(18) . . ? C6 O4 3.677(4) . 4 ? C3 C6 3.678(3) . . ? C13 O5 3.679(4) . 4 ? C14 H91 3.68(2) . 4_554 ? C6 H93 3.68(2) . 1_545 ? C13 H111 3.69(2) . 2 ? C13 H121 3.69(3) . 3_566 ? C7 O3 3.694(4) . 3_656 ? O2 O5 3.699(3) . 4 ? C11 O4 3.705(3) . 2_545 ? C12 H101 3.709(17) . 2 ? C12 H83 3.71(3) . 3_556 ? C10 H131 3.714(19) . 2_545 ? C5 H81 3.72(3) . . ? O5 H121 3.72(3) . 4_554 ? C15 O2 3.720(3) . . ? C15 H91 3.72(2) . . ? C5 C15 3.731(3) . . ? C4 O3 3.741(3) . . ? O4 H122 3.745(16) . 4_554 ? O3 H72 3.75(3) . . ? O1 H92 3.75(3) . . ? C12 C16 3.758(5) . . ? C7 C9 3.761(3) . 2_646 ? C16 H122 3.768(17) . 4_554 ? O2 H112 3.77(3) . 3_556 ? C14 O1 3.779(3) . . ? C6 H122 3.78(3) . . ? C12 O5 3.784(4) . 2 ? C4 C11 3.790(3) . . ? C7 O4 3.793(4) . 4 ? O2 H101 3.795(17) . . ? C5 O3 3.795(3) . 3_656 ? C15 O1 3.798(3) . 1_565 ? C7 H141 3.80(2) . 3_656 ? O1 H142 3.81(2) . 3_656 ? C8 H15 3.81(3) . 4 ? O4 H101 3.81(2) . . ? C4 H81 3.81(3) . . ? C3 H112 3.81(3) . . ? C12 H132 3.81(3) . 3_566 ? O1 H91 3.82(3) . 1_545 ? O1 H132 3.82(3) . 1_545 ? C2 H93 3.83(2) . . ? C16 H83 3.83(3) . 4_554 ? C14 H91 3.84(3) . . ? C8 H122 3.84(3) . . ? C1 O3 3.839(3) . 3_656 ? O5 H102 3.84(2) . . ? C2 H121 3.85(3) . . ? C9 H72 3.86(3) . 2_656 ? O3 H102 3.86(3) . . ? C1 H72 3.86(3) . 3_656 ? O2 H141 3.87(2) . . ? C13 H101 3.870(18) . 2 ? C9 O1 3.871(3) . . ? C13 C14 3.872(5) . . ? C5 C14 3.872(3) . 3_656 ? C11 H111 3.87(3) . 2_545 ? O4 H132 3.87(3) . . ? C13 O5 3.875(4) . 2 ? C8 C9 3.876(4) . 1_545 ? C5 H82 3.88(3) . . ? C9 H142 3.88(2) . . ? O3 H101 3.88(2) . . ? C10 H131 3.89(3) . 1_545 ? C13 H102 3.90(3) . 1_565 ? C8 C10 3.899(4) . . ? C8 O3 3.905(3) . 4_545 ? C7 H15 3.90(4) . 4 ? C10 C14 3.906(4) . . ? C16 O2 3.906(4) . 4_554 ? C12 C15 3.909(5) . . ? O4 H81 3.91(3) . 4_554 ? C4 H101 3.915(19) . . ? C5 C5 3.921(3) . 3_656 ? C3 O1 3.923(3) . . ? C8 C12 3.925(5) . 3_556 ? C14 O1 3.925(3) . 3_656 ? C7 O3 3.927(4) . 4_545 ? C1 C11 3.928(4) . . ? C10 H132 3.93(3) . . ? C11 O4 3.931(4) . . ? C4 H83 3.93(3) . . ? O5 H131 3.93(3) . . ? C7 C14 3.934(5) . 3_656 ? C13 H101 3.93(2) . . ? C12 H102 3.93(3) . 3_556 ? C7 H72 3.95(3) . 2_646 ? O3 H141 3.95(3) . 1_545 ? C7 H93 3.95(2) . 2_646 ? C10 O3 3.954(4) . . ? C16 H73 3.96(3) . 4_554 ? C11 H81 3.96(3) . . ? C4 H71 3.97(2) . . ? C16 O3 3.976(3) . . ? O2 H142 3.982(17) . 4 ? C16 H132 3.99(2) . 4_554 ? C10 H122 3.99(3) . 3_556 ? O4 H93 4.00(2) . . ? C12 H121 4.00(3) . 3_566 ? O5 H111 4.00(3) . 2_545 ? O3 H142 4.008(16) . 3_656 ? C5 H142 4.008(19) . 3_656 ? C16 H112 4.01(3) . . ? C1 H131 4.01(3) . . ? C9 O5 4.015(4) . 4 ? C14 H72 4.02(3) . . ? C8 H101 4.02(3) . 4_545 ? C11 H112 4.02(3) . 3_556 ? C16 H131 4.03(3) . 2_545 ? C7 H73 4.03(3) . 2_646 ? C15 H111 4.04(3) . . ? C5 H73 4.04(2) . . ? C9 H81 4.04(3) . 1_565 ? C1 H132 4.04(3) . . ? O3 O3 4.039(2) . 3_656 ? C4 O3 4.044(3) . 3_656 ? O2 O3 4.044(3) . . ? C5 C15 4.068(3) . 1_545 ? C1 C12 4.076(4) . . ? C7 C14 4.079(4) . 4 ? C8 C11 4.084(5) . 3_556 ? C7 O3 4.084(4) . . ? C1 C8 4.090(4) . . ? C11 C15 4.109(4) . . ? C8 C13 4.142(4) . 1_545 ? C12 O4 4.144(4) . . ? C11 C16 4.149(4) . 2_545 ? C4 O5 4.149(4) . 4 ? C7 C15 4.160(5) . 4 ? C11 C12 4.167(5) . 3_556 ? C6 C14 4.171(4) . . ? C8 C16 4.171(4) . 4_545 ? C8 C15 4.192(4) . 4 ? C11 O5 4.198(4) . 2_545 ? C1 C5 4.213(3) . 3_656 ? C13 O5 4.219(4) . . ? C16 O2 4.229(3) . . ? C9 O4 4.245(4) . 4 ? C14 O3 4.246(3) . 1_565 ? C12 C12 4.248(5) . 3_556 ? C5 O5 4.254(3) . . ? C5 O4 4.266(3) . . ? C3 O1 4.279(3) . 1_565 ? C4 O4 4.300(3) . 4 ? C11 C13 4.303(4) . 2_545 ? O1 O3 4.313(3) . 3_656 ? C9 C16 4.328(5) . 4 ? C6 C9 4.330(3) . 1_545 ? C10 C11 4.348(4) . 2_545 ? O3 O4 4.362(3) . 1_545 ? C13 O1 4.364(3) . 1_565 ? C3 O5 4.367(4) . 4 ? C9 O4 4.367(3) . . ? O3 O5 4.378(3) . . ? C15 O3 4.384(3) . . ? C3 O3 4.392(3) . . ? C11 O5 4.407(4) . 2 ? C2 C8 4.409(4) . . ? C9 C12 4.411(4) . . ? C6 C12 4.418(4) . . ? C7 C7 4.434(4) . 2_656 ? C7 C7 4.434(4) . 2_646 ? #----------------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC C5 C1 C14 124.5(2) . . . ? C5 C1 C4 119.4(2) . . . ? C5 C1 C2 115.18(17) . . . ? C14 C1 C4 100.87(19) . . . ? C14 C1 C2 101.89(17) . . . ? C4 C1 C2 87.85(17) . . . ? C16 C2 C10 110.74(19) . . . ? C16 C2 C3 104.6(2) . . . ? C16 C2 C1 114.0(2) . . . ? C10 C2 C3 117.4(2) . . . ? C10 C2 C1 124.53(19) . . . ? C3 C2 C1 80.87(15) . . . ? C13 C3 C4 124.9(2) . . . ? C13 C3 C2 118.2(2) . . . ? C13 C3 C15 121.3(2) . . . ? C4 C3 C2 90.69(16) . . . ? C4 C3 C15 101.9(2) . . . ? C2 C3 C15 91.5(2) . . . ? O2 C4 C9 111.63(19) . . . ? O2 C4 C3 112.44(18) . . . ? O2 C4 C1 107.80(17) . . . ? C9 C4 C3 115.34(18) . . . ? C9 C4 C1 123.5(2) . . . ? C3 C4 C1 83.21(16) . . . ? O3 C5 O1 119.6(2) . . . ? O3 C5 C1 125.0(2) . . . ? O1 C5 C1 114.9(2) . . . ? O2 C6 O1 111.76(17) . . . ? O2 C6 C7 115.8(2) . . . ? O2 C6 C8 105.3(2) . . . ? O1 C6 C7 105.5(2) . . . ? O1 C6 C8 105.9(2) . . . ? C7 C6 C8 112.3(2) . . . ? H71 C7 H72 106(2) . . . ? H71 C7 H73 106(2) . . . ? H71 C7 C6 111.1(14) . . . ? H72 C7 H73 115(2) . . . ? H72 C7 C6 112.9(14) . . . ? H73 C7 C6 105.4(15) . . . ? H81 C8 H83 107(2) . . . ? H81 C8 H82 119(2) . . . ? H81 C8 C6 109.8(17) . . . ? H83 C8 H82 108(2) . . . ? H83 C8 C6 109.0(17) . . . ? H82 C8 C6 103.3(18) . . . ? H92 C9 H91 112(2) . . . ? H92 C9 H93 98(2) . . . ? H92 C9 C4 111.4(17) . . . ? H91 C9 H93 118(2) . . . ? H91 C9 C4 106.9(16) . . . ? H93 C9 C4 110.5(13) . . . ? H102 C10 H101 113.7(19) . . . ? H102 C10 C2 111.2(16) . . . ? H102 C10 C11 107.5(18) . . . ? H101 C10 C2 105.4(15) . . . ? H101 C10 C11 110.9(13) . . . ? C2 C10 C11 108.1(2) . . . ? H111 C11 H112 114(2) . . . ? H111 C11 C12 109.3(17) . . . ? H111 C11 C10 107(2) . . . ? H112 C11 C12 104.0(18) . . . ? H112 C11 C10 109.9(15) . . . ? C12 C11 C10 113.4(2) . . . ? H122 C12 H121 107(3) . . . ? H122 C12 C11 109.0(16) . . . ? H122 C12 C13 108.8(16) . . . ? H121 C12 C11 113.8(15) . . . ? H121 C12 C13 105.9(16) . . . ? C11 C12 C13 112.2(3) . . . ? H132 C13 H131 111(2) . . . ? H132 C13 C3 111.4(18) . . . ? H132 C13 C12 108.5(18) . . . ? H131 C13 C3 105.7(17) . . . ? H131 C13 C12 109.8(16) . . . ? C3 C13 C12 110.6(2) . . . ? H141 C14 H142 111.5(19) . . . ? H141 C14 C1 109.5(14) . . . ? H141 C14 C15 114.4(14) . . . ? H142 C14 C1 115.2(15) . . . ? H142 C14 C15 109.9(13) . . . ? C1 C14 C15 95.6(2) . . . ? H15 C15 O4 109.5(17) . . . ? H15 C15 C14 112.5(17) . . . ? H15 C15 C3 122(2) . . . ? O4 C15 C14 104.7(2) . . . ? O4 C15 C3 104.1(2) . . . ? C14 C15 C3 102.4(2) . . . ? O5 C16 O4 122.3(3) . . . ? O5 C16 C2 130.1(3) . . . ? O4 C16 C2 107.6(2) . . . ? C5 O1 C6 122.21(17) . . . ? C6 O2 C4 115.7(2) . . . ? C16 O4 C15 104.94(18) . . . ? #----------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC C4 C1 C2 C3 30.49(17) . . . . ? C4 C1 C2 C10 -86.6(3) . . . . ? C4 C1 C2 C16 132.4(2) . . . . ? C5 C1 C2 C3 152.2(2) . . . . ? C5 C1 C2 C10 35.1(4) . . . . ? C5 C1 C2 C16 -105.9(3) . . . . ? C14 C1 C2 C3 -70.2(2) . . . . ? C14 C1 C2 C10 172.8(2) . . . . ? C14 C1 C2 C16 31.8(3) . . . . ? C2 C1 C4 C3 -30.31(16) . . . . ? C2 C1 C4 C9 -146.3(2) . . . . ? C2 C1 C4 O2 81.13(17) . . . . ? C5 C1 C4 C3 -148.2(2) . . . . ? C5 C1 C4 C9 95.8(3) . . . . ? C5 C1 C4 O2 -36.7(2) . . . . ? C14 C1 C4 C3 71.38(18) . . . . ? C14 C1 C4 C9 -44.6(2) . . . . ? C14 C1 C4 O2 -177.18(16) . . . . ? C2 C1 C5 O1 -79.9(2) . . . . ? C2 C1 C5 O3 92.5(3) . . . . ? C4 C1 C5 O1 22.6(3) . . . . ? C4 C1 C5 O3 -164.9(2) . . . . ? C14 C1 C5 O1 153.2(2) . . . . ? C14 C1 C5 O3 -34.3(3) . . . . ? C2 C1 C14 C15 35.8(2) . . . . ? C2 C1 C14 H141 154.1(15) . . . . ? C2 C1 C14 H142 -79.4(14) . . . . ? C4 C1 C14 C15 -54.33(19) . . . . ? C4 C1 C14 H141 64.0(15) . . . . ? C4 C1 C14 H142 -169.4(14) . . . . ? C5 C1 C14 C15 168.0(2) . . . . ? C5 C1 C14 H141 -73.6(15) . . . . ? C5 C1 C14 H142 52.9(14) . . . . ? C1 C2 C3 C4 -30.54(18) . . . . ? C1 C2 C3 C13 -161.5(2) . . . . ? C1 C2 C3 C15 71.38(17) . . . . ? C10 C2 C3 C4 93.7(2) . . . . ? C10 C2 C3 C13 -37.3(3) . . . . ? C10 C2 C3 C15 -164.34(19) . . . . ? C16 C2 C3 C4 -143.1(2) . . . . ? C16 C2 C3 C13 85.9(3) . . . . ? C16 C2 C3 C15 -41.2(2) . . . . ? C1 C2 C10 C11 140.8(2) . . . . ? C1 C2 C10 H101 -100.6(12) . . . . ? C1 C2 C10 H102 23.0(18) . . . . ? C3 C2 C10 C11 42.7(3) . . . . ? C3 C2 C10 H101 161.4(12) . . . . ? C3 C2 C10 H102 -75.0(18) . . . . ? C16 C2 C10 C11 -77.2(3) . . . . ? C16 C2 C10 H101 41.4(12) . . . . ? C16 C2 C10 H102 165.1(18) . . . . ? C1 C2 C16 O4 -65.8(3) . . . . ? C1 C2 C16 O5 116.8(4) . . . . ? C3 C2 C16 O4 20.5(3) . . . . ? C3 C2 C16 O5 -156.9(3) . . . . ? C10 C2 C16 O4 147.9(2) . . . . ? C10 C2 C16 O5 -29.6(4) . . . . ? C2 C3 C4 C1 31.91(18) . . . . ? C2 C3 C4 C9 155.9(2) . . . . ? C2 C3 C4 O2 -74.6(2) . . . . ? C13 C3 C4 C1 157.7(2) . . . . ? C13 C3 C4 C9 -78.4(3) . . . . ? C13 C3 C4 O2 51.2(3) . . . . ? C15 C3 C4 C1 -59.74(18) . . . . ? C15 C3 C4 C9 64.2(3) . . . . ? C15 C3 C4 O2 -166.23(18) . . . . ? C2 C3 C13 C12 38.4(3) . . . . ? C2 C3 C13 H131 -80.3(15) . . . . ? C2 C3 C13 H132 159.2(17) . . . . ? C4 C3 C13 C12 -74.6(3) . . . . ? C4 C3 C13 H131 166.7(15) . . . . ? C4 C3 C13 H132 46.1(17) . . . . ? C15 C3 C13 C12 149.5(2) . . . . ? C15 C3 C13 H131 30.8(15) . . . . ? C15 C3 C13 H132 -89.8(17) . . . . ? C2 C3 C15 C14 -58.42(18) . . . . ? C2 C3 C15 O4 50.4(2) . . . . ? C2 C3 C15 H15 174.7(17) . . . . ? C4 C3 C15 C14 32.6(2) . . . . ? C4 C3 C15 O4 141.44(18) . . . . ? C4 C3 C15 H15 -94.3(17) . . . . ? C13 C3 C15 C14 176.9(2) . . . . ? C13 C3 C15 O4 -74.2(3) . . . . ? C13 C3 C15 H15 50.1(18) . . . . ? C1 C4 C9 H91 -162.6(16) . . . . ? C1 C4 C9 H92 -40(2) . . . . ? C1 C4 C9 H93 67.4(19) . . . . ? C3 C4 C9 H91 98.4(16) . . . . ? C3 C4 C9 H92 -139(2) . . . . ? C3 C4 C9 H93 -31.6(19) . . . . ? O2 C4 C9 H91 -31.6(16) . . . . ? O2 C4 C9 H92 91(2) . . . . ? O2 C4 C9 H93 -161.5(19) . . . . ? C1 C4 O2 C6 53.6(2) . . . . ? C3 C4 O2 C6 143.47(18) . . . . ? C9 C4 O2 C6 -85.1(2) . . . . ? C1 C5 O1 C6 -22.8(3) . . . . ? O3 C5 O1 C6 164.3(2) . . . . ? C8 C6 C7 H71 50(2) . . . . ? C8 C6 C7 H72 169.0(19) . . . . ? C8 C6 C7 H73 -65.1(17) . . . . ? O1 C6 C7 H71 -65(2) . . . . ? O1 C6 C7 H72 54.1(19) . . . . ? O1 C6 C7 H73 180.0(16) . . . . ? O2 C6 C7 H71 171(2) . . . . ? O2 C6 C7 H72 -70.1(19) . . . . ? O2 C6 C7 H73 55.8(17) . . . . ? C7 C6 C8 H81 -177.5(19) . . . . ? C7 C6 C8 H82 -49.5(17) . . . . ? C7 C6 C8 H83 65.1(15) . . . . ? O1 C6 C8 H81 -62.9(19) . . . . ? O1 C6 C8 H82 65.1(17) . . . . ? O1 C6 C8 H83 179.7(15) . . . . ? O2 C6 C8 H81 55.6(19) . . . . ? O2 C6 C8 H82 -176.4(17) . . . . ? O2 C6 C8 H83 -61.8(15) . . . . ? C7 C6 O1 C5 -88.2(2) . . . . ? C8 C6 O1 C5 152.5(2) . . . . ? O2 C6 O1 C5 38.4(3) . . . . ? C7 C6 O2 C4 65.8(3) . . . . ? C8 C6 O2 C4 -169.54(18) . . . . ? O1 C6 O2 C4 -55.1(2) . . . . ? C2 C10 C11 C12 -55.6(3) . . . . ? C2 C10 C11 H111 64.8(17) . . . . ? C2 C10 C11 H112 -171.5(18) . . . . ? H101 C10 C11 C12 -170.7(14) . . . . ? H101 C10 C11 H111 -50(2) . . . . ? H101 C10 C11 H112 73(2) . . . . ? H102 C10 C11 C12 64.5(15) . . . . ? H102 C10 C11 H111 -175(2) . . . . ? H102 C10 C11 H112 -51(2) . . . . ? C10 C11 C12 C13 61.9(3) . . . . ? C10 C11 C12 H121 -178(2) . . . . ? C10 C11 C12 H122 -58.8(19) . . . . ? H111 C11 C12 C13 -57(2) . . . . ? H111 C11 C12 H121 63(3) . . . . ? H111 C11 C12 H122 -178(3) . . . . ? H112 C11 C12 C13 -178.8(14) . . . . ? H112 C11 C12 H121 -59(2) . . . . ? H112 C11 C12 H122 61(2) . . . . ? C11 C12 C13 C3 -50.1(3) . . . . ? C11 C12 C13 H131 66.1(17) . . . . ? C11 C12 C13 H132 -172.5(16) . . . . ? H121 C12 C13 C3 -174.8(18) . . . . ? H121 C12 C13 H131 -59(2) . . . . ? H121 C12 C13 H132 63(2) . . . . ? H122 C12 C13 C3 70.7(18) . . . . ? H122 C12 C13 H131 -173(2) . . . . ? H122 C12 C13 H132 -52(2) . . . . ? C1 C14 C15 C3 12.0(2) . . . . ? C1 C14 C15 O4 -96.4(2) . . . . ? C1 C14 C15 H15 145(2) . . . . ? H141 C14 C15 C3 -102.3(15) . . . . ? H141 C14 C15 O4 149.3(15) . . . . ? H141 C14 C15 H15 30(3) . . . . ? H142 C14 C15 C3 131.5(15) . . . . ? H142 C14 C15 O4 23.1(15) . . . . ? H142 C14 C15 H15 -96(3) . . . . ? C3 C15 O4 C16 -42.5(3) . . . . ? C14 C15 O4 C16 64.7(3) . . . . ? H15 C15 O4 C16 -174(2) . . . . ? C2 C16 O4 C15 13.2(3) . . . . ? O5 C16 O4 C15 -169.2(3) . . . . ? #----------------------------------------------------------------------------- _reflns_limit_h_min -17 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min -16 _reflns_limit_l_max 18 _reflns_number_total 2924 #ActaC _reflns_number_observed 2521 #ActaC _reflns_observed_criterion refl_observed_if_I_obs>2.50*sigma(I_obs) _reflns_d_resolution_high .798 _reflns_d_resolution_low 13.235 #----------------------------------------------------------------------------- loop_ _reflns_scale_group_code _reflns_scale_meas_F ? .157213 #----------------------------------------------------------------------------- loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? #==END