Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 207 _audit_creation_method Xtal3.7.1 _audit_creation_date 01-05-04 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Henk Hiemstra' _publ_contact_author_address ; Laboratory of Organic Chemistry, Institute of Molecular Chemistry, Nieuwe Achtergracht 129, 1018 WS Amsterdam, The Netherlands ; _publ_contact_author_email 'henkh@org.chem.uva.nl' _publ_contact_author_fax +31 20 5255670 _publ_contact_author_phone +31 20 5255941 _publ_contact_letter ; ? ; _publ_requested_journal ; Journal of the Chemical Society, Perkin Transactions 1 ; _publ_requested_category ? _publ_section_title ; Intramolecular [2+2] photocycloadditions as an approach towards the right-hand side of solanoeclepin A ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name 'Richard H. Blaauw' 'Jorg C. J. Benningshof' 'van Ginkel, Angeline E.' 'van Maarseveen, Jan H.' 'Henk Hiemstra' _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_p35bla _database_code_CSD 163621 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _chemical_formula_sum 'C18 H22 O5' _chemical_formula_moiety ? _chemical_formula_weight 318.4 _chemical_melting_point 186-187 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 6.6011(5) _cell_length_b 16.1185(10) _cell_length_c 14.5130(10) _cell_angle_alpha 90.00000 _cell_angle_beta 91.431(7) _cell_angle_gamma 90.00000 _cell_volume 1543.70(18) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.37 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 40 _cell_measurement_theta_max 43 _cell_measurement_temperature 243 _exptl_absorpt_coefficient_mu 0.82 _exptl_crystal_description ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number ? _reflns_number_total 3172 _reflns_Friedel_coverage ? _reflns_number_gt 2586 _reflns_threshold_expression 'Iobs > 2.50 sig(Iobs)' _diffrn_reflns_theta_max 75.27 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 6 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .05 _refine_ls_wR_factor_ref .053 _refine_ls_goodness_of_fit_ref .938 _refine_ls_number_reflns 2586 _refine_ls_number_parameters 297 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=[10. + 0.01(\s(Fobs)^2^) + 0.01/(\s(Fobs)]^-1^' _refine_ls_hydrogen_treatment 'restraint at 1.0 \%A' _refine_ls_shift/su_max .047 _refine_diff_density_min -.365 _refine_diff_density_max .326 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 2486(94) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack .00000 # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'CAD4 software' _computing_cell_refinement 'local program' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 72 .017 .009 'Int. Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 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 _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 .7427(4) .50872(15) .74314(17) .0263(12) Uani ? ? 1.00000 ? ? C2 .7897(4) .58032(16) .8071(2) .0342(14) Uani ? ? 1.00000 ? ? C3 .6716(5) .57189(18) .8958(2) .0407(16) Uani ? ? 1.00000 ? ? C4 .4461(5) .55759(18) .8769(2) .0426(17) Uani ? ? 1.00000 ? ? C5 .4035(4) .47630(17) .8243(2) .0337(14) Uani ? ? 1.00000 ? ? C6 .5208(4) .47728(15) .73632(18) .0276(12) Uani ? ? 1.00000 ? ? C7 .4233(4) .53172(17) .6628(2) .0374(15) Uani ? ? 1.00000 ? ? O1 .5714(3) .56435(12) .61153(14) .0401(11) Uani ? ? 1.00000 ? ? O2 .2466(3) .54714(14) .64891(18) .0554(14) Uani ? ? 1.00000 ? ? C8 .7549(4) .51789(17) .63730(19) .0339(14) Uani ? ? 1.00000 ? ? C9 .7115(5) .42802(18) .6039(2) .0377(15) Uani ? ? 1.00000 ? ? C10 .6332(4) .39677(15) .69510(17) .0277(12) Uani ? ? 1.00000 ? ? C11 .8162(4) .41832(15) .75791(17) .0256(12) Uani ? ? 1.00000 ? ? C12 .5325(4) .31511(16) .70832(19) .0325(13) Uani ? ? 1.00000 ? ? O3 .5828(3) .27552(11) .78679(13) .0332(10) Uani ? ? 1.00000 ? ? O5 .4034(4) .28641(14) .65842(17) .0623(15) Uani ? ? 1.00000 ? ? C13 .7580(4) .29819(14) .84633(17) .0263(12) Uani ? ? 1.00000 ? ? O4 .7884(3) .38602(9) .84762(12) .0262(8) Uani ? ? 1.00000 ? ? C14 .7023(4) .27334(16) .94218(19) .0307(13) Uani ? ? 1.00000 ? ? C15 .8821(5) .28139(17) 1.0095(2) .0362(15) Uani ? ? 1.00000 ? ? C16 1.0624(4) .23251(18) .9762(2) .0393(16) Uani ? ? 1.00000 ? ? C17 1.1197(4) .25897(17) .8801(2) .0360(15) Uani ? ? 1.00000 ? ? C18 .9410(4) .25075(16) .81240(19) .0300(13) Uani ? ? 1.00000 ? ? H21 .9397(17) .581(2) .821(2) .045(9) Uiso ? ? 1.00000 ? ? H22 .737(4) .6294(13) .7720(19) .046(9) Uiso ? ? 1.00000 ? ? H31 .739(5) .5259(15) .932(2) .054(10) Uiso ? ? 1.00000 ? ? H32 .698(5) .6216(13) .935(2) .059(10) Uiso ? ? 1.00000 ? ? H41 .372(4) .5540(17) .9361(11) .029(7) Uiso ? ? 1.00000 ? ? H42 .388(5) .6003(17) .834(2) .071(12) Uiso ? ? 1.00000 ? ? H51 .447(4) .4283(13) .8638(18) .048(9) Uiso ? ? 1.00000 ? ? H52 .2570(19) .4741(18) .8044(19) .039(8) Uiso ? ? 1.00000 ? ? H8 .877(3) .5461(18) .614(2) .053(10) Uiso ? ? 1.00000 ? ? H91 .613(4) .429(2) .5508(15) .051(9) Uiso ? ? 1.00000 ? ? H92 .840(3) .3993(17) .588(2) .047(9) Uiso ? ? 1.00000 ? ? H11 .949(2) .4042(16) .7305(16) .028(7) Uiso ? ? 1.00000 ? ? H141 .584(3) .3057(16) .963(2) .041(8) Uiso ? ? 1.00000 ? ? H142 .655(5) .2149(9) .941(2) .055(10) Uiso ? ? 1.00000 ? ? H151 .929(5) .3398(9) 1.016(3) .070(12) Uiso ? ? 1.00000 ? ? H152 .846(4) .2641(17) 1.0731(10) .035(8) Uiso ? ? 1.00000 ? ? H161 1.176(3) .2397(19) 1.0221(16) .043(8) Uiso ? ? 1.00000 ? ? H162 1.015(5) .1740(9) .974(2) .057(10) Uiso ? ? 1.00000 ? ? H171 1.172(5) .3170(10) .882(2) .066(11) Uiso ? ? 1.00000 ? ? H172 1.237(3) .2284(16) .8543(19) .041(8) Uiso ? ? 1.00000 ? ? H181 .983(3) .2708(14) .7502(9) .016(6) Uiso ? ? 1.00000 ? ? H182 .902(5) .1915(8) .806(2) .055(10) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 .0262(12) .0199(12) .0327(13) -.0009(9) -.0000(10) .0030(10) C2 .0405(15) .0204(12) .0414(16) -.0059(11) -.0014(12) .0008(11) C3 .0570(18) .0275(14) .0377(16) -.0059(13) .0027(13) -.0074(12) C4 .0526(18) .0293(15) .0467(18) .0050(13) .0179(14) -.0060(13) C5 .0285(13) .0281(13) .0447(16) .0010(11) .0047(11) .0002(12) C6 .0270(12) .0200(12) .0356(14) .0016(9) -.0030(10) .0001(10) C7 .0389(15) .0278(14) .0450(16) .0049(11) -.0076(12) .0010(12) O1 .0469(12) .0318(10) .0411(11) .0051(9) -.0058(9) .0120(8) O2 .0410(12) .0461(13) .0784(17) .0128(10) -.0154(11) .0096(12) C8 .0372(15) .0292(13) .0355(14) .0025(11) .0041(11) .0058(11) C9 .0503(18) .0334(15) .0296(14) .0035(13) .0007(12) -.0017(12) C10 .0296(13) .0218(12) .0315(13) .0018(10) -.0029(10) -.0020(10) C11 .0250(12) .0224(12) .0295(13) .0002(9) .0009(10) .0022(10) C12 .0353(14) .0258(13) .0361(14) -.0023(11) -.0063(11) -.0022(11) O3 .0327(10) .0253(9) .0410(11) -.0086(7) -.0104(8) .0048(8) O5 .0756(17) .0427(13) .0665(16) -.0220(12) -.0419(13) .0042(11) C13 .0267(12) .0176(11) .0344(13) -.0032(9) -.0032(10) .0003(10) O4 .0321(9) .0157(8) .0307(9) -.0013(7) -.0017(7) -.0001(7) C14 .0307(13) .0258(13) .0358(14) -.0007(10) .0057(11) .0021(11) C15 .0487(17) .0305(14) .0293(14) -.0006(12) -.0013(12) .0016(11) C16 .0386(16) .0327(15) .0458(17) .0035(12) -.0104(13) .0040(12) C17 .0264(13) .0290(14) .0527(18) .0020(11) .0007(12) .0017(12) C18 .0328(14) .0227(12) .0347(14) .0016(10) .0039(11) -.0002(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . . 1.508(4) ? C1 C8 . . 1.547(4) ? C1 C11 . . 1.549(3) ? C1 C6 . . 1.551(3) ? C2 H22 . . 1.00(2) ? C2 H21 . . 1.006(13) ? C2 C3 . . 1.528(4) ? C3 H32 . . 1.00(2) ? C3 H31 . . 1.00(3) ? C3 C4 . . 1.524(5) ? C4 H42 . . 1.00(3) ? C4 H41 . . 1.002(19) ? C4 C5 . . 1.538(4) ? C5 H51 . . 1.00(2) ? C5 H52 . . 1.003(14) ? C5 C6 . . 1.510(4) ? C6 C7 . . 1.512(4) ? C6 C10 . . 1.617(3) ? C7 O2 . . 1.205(4) ? C7 O1 . . 1.351(4) ? O1 C8 . . 1.464(3) ? C8 H8 . . 1.00(2) ? C8 C9 . . 1.552(4) ? C9 H91 . . 1.00(2) ? C9 H92 . . 1.00(2) ? C9 C10 . . 1.519(4) ? C10 C12 . . 1.489(4) ? C10 C11 . . 1.535(3) ? C11 H11 . . .999(18) ? C11 O4 . . 1.418(3) ? C12 O5 . . 1.197(4) ? C12 O3 . . 1.340(3) ? O3 C13 . . 1.472(3) ? C13 O4 . . 1.430(3) ? C13 C14 . . 1.502(4) ? C13 C18 . . 1.522(4) ? C14 H142 . . .991(17) ? C14 H141 . . .99(2) ? C14 C15 . . 1.524(4) ? C15 H151 . . .994(18) ? C15 H152 . . .999(17) ? C15 C16 . . 1.516(4) ? C16 H162 . . .994(17) ? C16 H161 . . 1.00(2) ? C16 C17 . . 1.516(4) ? C17 H172 . . 1.00(2) ? C17 H171 . . .997(19) ? C17 C18 . . 1.522(4) ? C18 H182 . . .992(15) ? C18 H181 . . 1.004(16) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 C8 . . . 121.5(2) ? C2 C1 C11 . . . 125.1(2) ? C2 C1 C6 . . . 118.0(2) ? C8 C1 C11 . . . 101.7(2) ? C8 C1 C6 . . . 92.3(2) ? C11 C1 C6 . . . 89.63(18) ? H22 C2 H21 . . . 115(2) ? H22 C2 C1 . . . 103.2(14) ? H22 C2 C3 . . . 108.8(16) ? H21 C2 C1 . . . 108.9(17) ? H21 C2 C3 . . . 110.5(17) ? C1 C2 C3 . . . 110.4(2) ? H32 C3 H31 . . . 103(2) ? H32 C3 C4 . . . 112(2) ? H32 C3 C2 . . . 109.0(17) ? H31 C3 C4 . . . 113.7(16) ? H31 C3 C2 . . . 105.8(17) ? C4 C3 C2 . . . 112.3(3) ? H42 C4 H41 . . . 113(2) ? H42 C4 C3 . . . 112(2) ? H42 C4 C5 . . . 102.3(17) ? H41 C4 C3 . . . 110.6(13) ? H41 C4 C5 . . . 106.8(15) ? C3 C4 C5 . . . 112.5(2) ? H51 C5 H52 . . . 114(2) ? H51 C5 C6 . . . 110.1(16) ? H51 C5 C4 . . . 109.2(14) ? H52 C5 C6 . . . 105.5(15) ? H52 C5 C4 . . . 109.6(17) ? C6 C5 C4 . . . 108.6(2) ? C5 C6 C7 . . . 112.6(2) ? C5 C6 C1 . . . 116.9(2) ? C5 C6 C10 . . . 123.7(2) ? C7 C6 C1 . . . 103.9(2) ? C7 C6 C10 . . . 113.3(2) ? C1 C6 C10 . . . 81.03(17) ? O2 C7 O1 . . . 122.6(3) ? O2 C7 C6 . . . 129.1(3) ? O1 C7 C6 . . . 108.3(2) ? C7 O1 C8 . . . 105.4(2) ? H8 C8 O1 . . . 110.6(15) ? H8 C8 C1 . . . 116.7(17) ? H8 C8 C9 . . . 117.6(17) ? O1 C8 C1 . . . 103.8(2) ? O1 C8 C9 . . . 104.6(2) ? C1 C8 C9 . . . 101.9(2) ? H91 C9 H92 . . . 112(2) ? H91 C9 C10 . . . 116.8(15) ? H91 C9 C8 . . . 109.8(19) ? H92 C9 C10 . . . 111.0(17) ? H92 C9 C8 . . . 110.8(15) ? C10 C9 C8 . . . 95.8(2) ? C12 C10 C9 . . . 124.6(2) ? C12 C10 C11 . . . 118.1(2) ? C12 C10 C6 . . . 116.8(2) ? C9 C10 C11 . . . 99.4(2) ? C9 C10 C6 . . . 103.0(2) ? C11 C10 C6 . . . 87.74(18) ? H11 C11 O4 . . . 114.7(14) ? H11 C11 C10 . . . 113.5(13) ? H11 C11 C1 . . . 115.7(15) ? O4 C11 C10 . . . 110.12(19) ? O4 C11 C1 . . . 115.1(2) ? C10 C11 C1 . . . 83.77(17) ? O5 C12 O3 . . . 119.2(2) ? O5 C12 C10 . . . 125.2(3) ? O3 C12 C10 . . . 115.4(2) ? C12 O3 C13 . . . 123.7(2) ? O4 C13 O3 . . . 111.18(18) ? O4 C13 C14 . . . 106.8(2) ? O4 C13 C18 . . . 112.9(2) ? O3 C13 C14 . . . 105.70(19) ? O3 C13 C18 . . . 107.7(2) ? C14 C13 C18 . . . 112.4(2) ? C11 O4 C13 . . . 111.88(18) ? H142 C14 H141 . . . 105(2) ? H142 C14 C13 . . . 109(2) ? H142 C14 C15 . . . 109.3(18) ? H141 C14 C13 . . . 110.8(16) ? H141 C14 C15 . . . 111.4(15) ? C13 C14 C15 . . . 111.5(2) ? H151 C15 H152 . . . 105(3) ? H151 C15 C16 . . . 106(2) ? H151 C15 C14 . . . 112(2) ? H152 C15 C16 . . . 110.8(16) ? H152 C15 C14 . . . 111.7(15) ? C16 C15 C14 . . . 110.9(2) ? H162 C16 H161 . . . 112(3) ? H162 C16 C17 . . . 109(2) ? H162 C16 C15 . . . 104.7(18) ? H161 C16 C17 . . . 112.4(14) ? H161 C16 C15 . . . 108.1(15) ? C17 C16 C15 . . . 111.3(2) ? H172 C17 H171 . . . 102(2) ? H172 C17 C16 . . . 114.8(16) ? H172 C17 C18 . . . 108.0(15) ? H171 C17 C16 . . . 110(2) ? H171 C17 C18 . . . 111(2) ? C16 C17 C18 . . . 111.2(2) ? H182 C18 H181 . . . 108(2) ? H182 C18 C13 . . . 107.9(18) ? H182 C18 C17 . . . 109.5(18) ? H181 C18 C13 . . . 111.5(13) ? H181 C18 C17 . . . 109.1(12) ? C13 C18 C17 . . . 110.9(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 39.3(3) ? C6 C1 C2 H21 . . . . 160.9(18) ? C6 C1 C2 H22 . . . . -76.8(17) ? C8 C1 C2 C3 . . . . 151.6(2) ? C8 C1 C2 H21 . . . . -86.8(18) ? C8 C1 C2 H22 . . . . 35.5(17) ? C11 C1 C2 C3 . . . . -72.0(3) ? C11 C1 C2 H21 . . . . 49.5(18) ? C11 C1 C2 H22 . . . . 171.9(17) ? C2 C1 C6 C5 . . . . -37.8(3) ? C2 C1 C6 C7 . . . . 87.0(3) ? C2 C1 C6 C10 . . . . -161.1(2) ? C8 C1 C6 C5 . . . . -165.6(2) ? C8 C1 C6 C7 . . . . -40.9(2) ? C8 C1 C6 C10 . . . . 71.08(18) ? C11 C1 C6 C5 . . . . 92.7(2) ? C11 C1 C6 C7 . . . . -142.6(2) ? C11 C1 C6 C10 . . . . -30.65(17) ? C2 C1 C8 O1 . . . . -75.8(3) ? C2 C1 C8 C9 . . . . 175.6(2) ? C2 C1 C8 H8 . . . . 46.1(18) ? C6 C1 C8 O1 . . . . 49.3(2) ? C6 C1 C8 C9 . . . . -59.3(2) ? C6 C1 C8 H8 . . . . 171.2(18) ? C11 C1 C8 O1 . . . . 139.4(2) ? C11 C1 C8 C9 . . . . 30.9(2) ? C11 C1 C8 H8 . . . . -98.7(18) ? C2 C1 C11 C10 . . . . 156.9(3) ? C2 C1 C11 O4 . . . . 47.6(3) ? C2 C1 C11 H11 . . . . -90.0(14) ? C6 C1 C11 C10 . . . . 32.26(18) ? C6 C1 C11 O4 . . . . -77.1(2) ? C6 C1 C11 H11 . . . . 145.4(14) ? C8 C1 C11 C10 . . . . -60.0(2) ? C8 C1 C11 O4 . . . . -169.4(2) ? C8 C1 C11 H11 . . . . 53.1(14) ? C1 C2 C3 C4 . . . . -51.2(3) ? C1 C2 C3 H31 . . . . 73.3(16) ? C1 C2 C3 H32 . . . . -176.4(18) ? H21 C2 C3 C4 . . . . -171.8(19) ? H21 C2 C3 H31 . . . . -47(2) ? H21 C2 C3 H32 . . . . 63(3) ? H22 C2 C3 C4 . . . . 61.4(16) ? H22 C2 C3 H31 . . . . -174(2) ? H22 C2 C3 H32 . . . . -64(2) ? C2 C3 C4 C5 . . . . 62.4(3) ? C2 C3 C4 H41 . . . . -178.3(16) ? C2 C3 C4 H42 . . . . -52.0(19) ? H31 C3 C4 C5 . . . . -57.6(18) ? H31 C3 C4 H41 . . . . 62(2) ? H31 C3 C4 H42 . . . . -172(3) ? H32 C3 C4 C5 . . . . -174.3(17) ? H32 C3 C4 H41 . . . . -55(2) ? H32 C3 C4 H42 . . . . 71(2) ? C3 C4 C5 C6 . . . . -55.9(3) ? C3 C4 C5 H51 . . . . 64.2(18) ? C3 C4 C5 H52 . . . . -170.7(17) ? H41 C4 C5 C6 . . . . -177.4(14) ? H41 C4 C5 H51 . . . . -57(2) ? H41 C4 C5 H52 . . . . 68(2) ? H42 C4 C5 C6 . . . . 64(2) ? H42 C4 C5 H51 . . . . -176(3) ? H42 C4 C5 H52 . . . . -51(3) ? C4 C5 C6 C1 . . . . 43.3(3) ? C4 C5 C6 C7 . . . . -76.9(3) ? C4 C5 C6 C10 . . . . 140.7(2) ? H51 C5 C6 C1 . . . . -76.2(16) ? H51 C5 C6 C7 . . . . 163.6(16) ? H51 C5 C6 C10 . . . . 21.1(16) ? H52 C5 C6 C1 . . . . 160.8(17) ? H52 C5 C6 C7 . . . . 40.6(18) ? H52 C5 C6 C10 . . . . -101.9(18) ? C1 C6 C7 O1 . . . . 20.5(3) ? C1 C6 C7 O2 . . . . -158.6(3) ? C5 C6 C7 O1 . . . . 148.0(2) ? C5 C6 C7 O2 . . . . -31.1(4) ? C10 C6 C7 O1 . . . . -65.5(3) ? C10 C6 C7 O2 . . . . 115.4(3) ? C1 C6 C10 C9 . . . . -68.1(2) ? C1 C6 C10 C11 . . . . 30.99(17) ? C1 C6 C10 C12 . . . . 151.5(2) ? C5 C6 C10 C9 . . . . 175.5(2) ? C5 C6 C10 C11 . . . . -85.5(3) ? C5 C6 C10 C12 . . . . 35.1(3) ? C7 C6 C10 C9 . . . . 33.2(3) ? C7 C6 C10 C11 . . . . 132.3(2) ? C7 C6 C10 C12 . . . . -107.1(3) ? C6 C7 O1 C8 . . . . 12.2(3) ? O2 C7 O1 C8 . . . . -168.6(3) ? C7 O1 C8 C1 . . . . -41.2(2) ? C7 O1 C8 C9 . . . . 65.4(3) ? C7 O1 C8 H8 . . . . -167.1(18) ? C1 C8 C9 C10 . . . . 13.8(2) ? C1 C8 C9 H91 . . . . 135.1(15) ? C1 C8 C9 H92 . . . . -101.3(19) ? O1 C8 C9 C10 . . . . -94.1(2) ? O1 C8 C9 H91 . . . . 27.1(15) ? O1 C8 C9 H92 . . . . 150.8(19) ? H8 C8 C9 C10 . . . . 142.8(18) ? H8 C8 C9 H91 . . . . -96(2) ? H8 C8 C9 H92 . . . . 28(3) ? C8 C9 C10 C6 . . . . 33.9(2) ? C8 C9 C10 C11 . . . . -56.0(2) ? C8 C9 C10 C12 . . . . 170.1(2) ? H91 C9 C10 C6 . . . . -82(2) ? H91 C9 C10 C11 . . . . -172(2) ? H91 C9 C10 C12 . . . . 54(2) ? H92 C9 C10 C6 . . . . 148.9(16) ? H92 C9 C10 C11 . . . . 59.0(16) ? H92 C9 C10 C12 . . . . -74.9(17) ? C6 C10 C11 C1 . . . . -30.82(17) ? C6 C10 C11 O4 . . . . 83.7(2) ? C6 C10 C11 H11 . . . . -146.2(16) ? C9 C10 C11 C1 . . . . 72.0(2) ? C9 C10 C11 O4 . . . . -173.4(2) ? C9 C10 C11 H11 . . . . -43.4(16) ? C12 C10 C11 C1 . . . . -150.2(2) ? C12 C10 C11 O4 . . . . -35.7(3) ? C12 C10 C11 H11 . . . . 94.4(16) ? C6 C10 C12 O3 . . . . -88.6(3) ? C6 C10 C12 O5 . . . . 85.9(3) ? C9 C10 C12 O3 . . . . 140.4(3) ? C9 C10 C12 O5 . . . . -45.1(4) ? C11 C10 C12 O3 . . . . 14.1(3) ? C11 C10 C12 O5 . . . . -171.5(3) ? C1 C11 O4 C13 . . . . 150.0(2) ? C10 C11 O4 C13 . . . . 57.5(2) ? H11 C11 O4 C13 . . . . -71.9(15) ? C10 C12 O3 C13 . . . . -14.4(3) ? O5 C12 O3 C13 . . . . 170.8(2) ? C12 O3 C13 O4 . . . . 35.8(3) ? C12 O3 C13 C14 . . . . 151.4(2) ? C12 O3 C13 C18 . . . . -88.4(3) ? O3 C13 O4 C11 . . . . -57.5(2) ? C14 C13 O4 C11 . . . . -172.39(18) ? C18 C13 O4 C11 . . . . 63.6(3) ? O3 C13 C14 C15 . . . . 171.6(2) ? O3 C13 C14 H141 . . . . -63.7(15) ? O3 C13 C14 H142 . . . . 51.1(18) ? O4 C13 C14 C15 . . . . -69.9(2) ? O4 C13 C14 H141 . . . . 54.8(15) ? O4 C13 C14 H142 . . . . 169.6(18) ? C18 C13 C14 C15 . . . . 54.4(3) ? C18 C13 C14 H141 . . . . 179.1(15) ? C18 C13 C14 H142 . . . . -66.1(18) ? O3 C13 C18 C17 . . . . -170.1(2) ? O3 C13 C18 H181 . . . . 68.1(13) ? O3 C13 C18 H182 . . . . -50(2) ? O4 C13 C18 C17 . . . . 66.8(3) ? O4 C13 C18 H181 . . . . -55.0(13) ? O4 C13 C18 H182 . . . . -173(2) ? C14 C13 C18 C17 . . . . -54.1(3) ? C14 C13 C18 H181 . . . . -175.9(13) ? C14 C13 C18 H182 . . . . 66(2) ? C13 C14 C15 C16 . . . . -55.0(3) ? C13 C14 C15 H151 . . . . 64(2) ? C13 C14 C15 H152 . . . . -179.1(17) ? H141 C14 C15 C16 . . . . -179.3(16) ? H141 C14 C15 H151 . . . . -61(3) ? H141 C14 C15 H152 . . . . 57(2) ? H142 C14 C15 C16 . . . . 65(2) ? H142 C14 C15 H151 . . . . -176(3) ? H142 C14 C15 H152 . . . . -59(3) ? C14 C15 C16 C17 . . . . 56.0(3) ? C14 C15 C16 H161 . . . . 179.8(17) ? C14 C15 C16 H162 . . . . -61(2) ? H151 C15 C16 C17 . . . . -66(2) ? H151 C15 C16 H161 . . . . 58(3) ? H151 C15 C16 H162 . . . . 177(3) ? H152 C15 C16 C17 . . . . -179.4(16) ? H152 C15 C16 H161 . . . . -56(2) ? H152 C15 C16 H162 . . . . 64(3) ? C15 C16 C17 C18 . . . . -56.2(3) ? C15 C16 C17 H171 . . . . 67(2) ? C15 C16 C17 H172 . . . . -179.3(15) ? H161 C16 C17 C18 . . . . -177.6(18) ? H161 C16 C17 H171 . . . . -54(3) ? H161 C16 C17 H172 . . . . 59(2) ? H162 C16 C17 C18 . . . . 58.5(19) ? H162 C16 C17 H171 . . . . -178(3) ? H162 C16 C17 H172 . . . . -65(2) ? C16 C17 C18 C13 . . . . 54.6(3) ? C16 C17 C18 H181 . . . . 177.8(14) ? C16 C17 C18 H182 . . . . -64(2) ? H171 C17 C18 C13 . . . . -68(2) ? H171 C17 C18 H181 . . . . 55(3) ? H171 C17 C18 H182 . . . . 173(3) ? H172 C17 C18 C13 . . . . -178.5(16) ? H172 C17 C18 H181 . . . . -55(2) ? H172 C17 C18 H182 . . . . 63(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag H171 H172 1.55(3) . . ? H31 H32 1.57(3) . . ? H141 H142 1.57(3) . . ? H151 H152 1.58(4) . . ? H181 H182 1.61(3) . . ? H161 H162 1.65(4) . . ? H91 H92 1.65(3) . . ? H41 H42 1.67(4) . . ? H51 H52 1.68(3) . . ? H21 H22 1.69(3) . . ? C1 H22 1.99(2) . . ? C5 H42 2.01(3) . . ? C15 H162 2.01(2) . . ? C6 H52 2.024(18) . . ? C16 H151 2.03(2) . . ? O1 H8 2.04(2) . . ? C2 H31 2.04(3) . . ? C13 H142 2.05(3) . . ? O4 H11 2.05(2) . . ? C15 H161 2.06(2) . . ? C13 H182 2.06(2) . . ? C1 C10 2.059(3) . . ? C17 H162 2.06(3) . . ? C18 H172 2.06(2) . . ? C5 H41 2.06(2) . . ? C1 H21 2.07(2) . . ? C13 H141 2.07(3) . . ? C15 H142 2.07(3) . . ? C17 H182 2.08(3) . . ? C16 H171 2.08(3) . . ? C3 H22 2.08(3) . . ? C2 H32 2.08(3) . . ? C6 H51 2.08(3) . . ? C17 H181 2.079(16) . . ? C16 H152 2.09(2) . . ? C4 H51 2.09(2) . . ? C10 H92 2.09(3) . . ? C3 H41 2.10(2) . . ? C18 H171 2.10(3) . . ? C15 H141 2.10(2) . . ? C4 H52 2.10(2) . . ? C3 H21 2.103(19) . . ? C14 H152 2.108(17) . . ? C17 H161 2.11(2) . . ? C13 H181 2.11(2) . . ? C8 H91 2.11(3) . . ? C3 H42 2.11(3) . . ? C14 H151 2.11(3) . . ? C4 H32 2.12(3) . . ? C8 H92 2.12(3) . . ? C4 H31 2.14(3) . . ? C16 H172 2.14(3) . . ? C10 H11 2.139(16) . . ? C10 H91 2.16(2) . . ? H92 H11 2.18(4) . . ? C1 H11 2.18(2) . . ? H11 H181 2.18(3) . . ? C1 H8 2.18(3) . . ? C6 C11 2.185(3) . . ? O3 O5 2.189(3) . . ? C9 H8 2.20(3) . . ? C6 C8 2.235(4) . . ? C7 C8 2.240(4) . . ? O1 O2 2.242(3) . . ? H42 H52 2.25(4) . . ? C8 C10 2.279(4) . . ? H21 H31 2.28(4) . . ? H151 H161 2.30(4) . . ? C6 O1 2.322(3) . . ? C9 C11 2.328(4) . . ? H172 H181 2.33(3) . . ? H41 H51 2.34(3) . . ? H152 H162 2.35(4) . . ? H152 H161 2.35(3) . . ? O4 C14 2.355(3) . . ? C11 C13 2.360(3) . . ? H92 H162 2.36(4) . '4 554' ? O4 H51 2.37(3) . . ? O3 C14 2.371(3) . . ? C1 O1 2.371(3) . . ? O1 H91 2.37(3) . . ? H172 H182 2.37(4) . . ? H171 H181 2.38(4) . . ? O1 C9 2.388(3) . . ? H161 H171 2.39(4) . . ? C10 O5 2.389(3) . . ? C10 O3 2.392(3) . . ? H22 H32 2.39(4) . . ? O3 O4 2.395(2) . . ? C8 C11 2.402(4) . . ? H142 H152 2.40(4) . . ? C1 C9 2.407(4) . . ? H8 H92 2.41(4) . . ? H41 H52 2.41(3) . . ? C1 C7 2.412(4) . . ? H32 H41 2.41(4) . . ? H21 H32 2.42(4) . . ? C9 H11 2.42(2) . . ? O3 C18 2.418(3) . . ? H141 H152 2.42(3) . . ? C10 O4 2.422(3) . . ? H22 H172 2.44(4) . '2 756' ? H31 H41 2.44(3) . '3 667' ? H141 H151 2.45(4) . . ? C6 C9 2.455(4) . . ? C6 O2 2.457(3) . . ? H162 H172 2.46(4) . . ? H32 H161 2.46(4) . '3 767' ? O4 C18 2.461(3) . . ? H31 H41 2.47(4) . . ? C4 C6 2.476(4) . . ? O3 H142 2.48(3) . . ? O2 H8 2.48(2) . '1 455' ? C12 C13 2.480(4) . . ? H161 H172 2.48(4) . . ? O5 H161 2.49(2) . '4 454' ? C1 C3 2.493(4) . . ? H142 H162 2.50(4) . . ? C11 H92 2.50(3) . . ? C13 C15 2.501(4) . . ? C15 C17 2.503(4) . . ? C14 C16 2.504(4) . . ? C1 O4 2.506(3) . . ? C13 C17 2.507(4) . . ? C16 C18 2.507(4) . . ? C14 C18 2.512(4) . . ? C5 C7 2.515(4) . . ? H32 H42 2.52(5) . . ? O3 H182 2.52(3) . . ? C7 H52 2.53(3) . . ? H8 H162 2.53(4) . '2 756' ? O4 H141 2.53(3) . . ? C2 C4 2.534(4) . . ? H162 H182 2.54(5) . . ? H52 H11 2.54(3) . '1 455' ? H22 H42 2.54(4) . . ? O2 H52 2.54(3) . . ? C3 C5 2.547(4) . . ? H51 H171 2.57(4) . '1 455' ? H151 H171 2.59(5) . . ? O4 H31 2.59(2) . . ? C11 C12 2.593(4) . . ? H51 H141 2.59(3) . . ? C8 H11 2.60(2) . . ? C6 H42 2.60(3) . . ? H142 H182 2.60(5) . . ? O3 H141 2.60(3) . . ? C1 C5 2.609(4) . . ? O2 H182 2.614(19) . '2 656' ? C7 C10 2.615(4) . . ? O3 H172 2.62(2) . '1 455' ? H32 H151 2.62(5) . '3 767' ? C2 C6 2.622(4) . . ? C11 H181 2.62(2) . . ? O1 H91 2.63(2) . '3 666' ? C14 H162 2.64(3) . . ? H92 H152 2.64(4) . '4 554' ? C6 C12 2.647(4) . . ? C7 H91 2.66(3) . . ? H31 H51 2.66(4) . . ? C8 H22 2.66(2) . . ? C9 C12 2.663(4) . . ? C2 C8 2.666(4) . . ? H32 H141 2.68(4) . '3 667' ? O4 H181 2.68(2) . . ? C18 H162 2.68(3) . . ? C7 C9 2.688(4) . . ? O4 H151 2.70(4) . . ? C17 H151 2.71(3) . . ? H41 H141 2.71(4) . '3 667' ? O3 H181 2.71(2) . . ? H8 H91 2.71(4) . . ? C2 H42 2.71(3) . . ? C2 C11 2.714(4) . . ? H41 H151 2.72(4) . '3 667' ? C13 H11 2.73(2) . . ? H21 H52 2.73(3) . '1 655' ? C7 H42 2.73(3) . . ? C16 H142 2.74(3) . . ? C4 H22 2.74(3) . . ? C16 H182 2.74(3) . . ? C14 H182 2.74(3) . . ? C18 H11 2.75(3) . . ? C18 H142 2.75(3) . . ? C1 H31 2.75(3) . . ? O1 H22 2.75(3) . . ? C5 C10 2.757(4) . . ? C15 H171 2.76(3) . . ? H152 H181 2.76(2) . 4 ? C13 H151 2.77(4) . . ? C3 H51 2.78(2) . . ? C6 O4 2.784(3) . . ? C13 H171 2.79(3) . . ? H21 H182 2.79(4) . '2 756' ? C5 H31 2.79(3) . . ? O4 H171 2.80(3) . . ? H21 H151 2.80(4) . '3 767' ? H151 H162 2.80(2) . . ? C11 O3 2.807(3) . . ? C10 H51 2.81(3) . . ? C10 C13 2.816(3) . . ? H52 H171 2.83(4) . '1 455' ? H91 H142 2.83(4) . '4 554' ? H42 H51 2.83(4) . . ? H22 H8 2.84(4) . . ? C12 O4 2.842(3) . . ? H22 H182 2.85(4) . '2 756' ? H22 H31 2.85(4) . . ? O3 H51 2.86(2) . . ? H162 H171 2.87(3) . . ? C6 H22 2.88(2) . . ? H8 H11 2.88(4) . . ? C6 H91 2.88(2) . . ? O5 H22 2.89(2) . '2 646' ? H171 H182 2.89(4) . . ? C11 H21 2.89(3) . . ? H142 H151 2.90(4) . . ? C1 C4 2.900(4) . . ? C11 H51 2.91(3) . . ? C13 C16 2.920(4) . . ? C3 C6 2.925(4) . . ? C11 C18 2.927(3) . . ? C14 C17 2.930(4) . . ? C2 H8 2.93(3) . . ? C15 C18 2.938(4) . . ? C5 O4 2.940(3) . . ? O1 H142 2.94(2) . '2 656' ? H32 H171 2.94(4) . '3 767' ? H141 H171 2.94(4) . '1 455' ? C1 H92 2.94(3) . . ? O4 C15 2.945(3) . . ? O2 H42 2.95(3) . . ? H31 H42 2.95(4) . . ? C13 H51 2.95(3) . . ? C1 H51 2.95(3) . . ? C5 O2 2.954(4) . . ? H22 H181 2.96(3) . '2 756' ? C12 H51 2.97(2) . . ? H11 H171 2.97(4) . . ? O1 H172 2.97(3) . '2 756' ? C11 H8 2.97(3) . . ? H21 H42 2.97(4) . '1 655' ? H8 H182 2.98(4) . '2 756' ? O1 C10 2.985(3) . . ? C12 H91 2.99(3) . . ? H42 H152 3.01(4) . '3 667' ? H142 H172 3.02(4) . '1 455' ? C7 H22 3.02(3) . . ? H141 H172 3.02(3) . '1 455' ? O4 C17 3.025(3) . . ? C12 H92 3.03(3) . . ? H41 H41 3.03(3) . '3 667' ? H141 H161 3.04(3) . '1 455' ? H92 H142 3.05(4) . '4 554' ? O5 H32 3.05(2) . '2 646' ? C5 C11 3.059(4) . . ? C6 H11 3.067(17) . . ? C2 C5 3.067(4) . . ? C16 H92 3.07(3) . 4 ? H8 H172 3.07(4) . '2 756' ? O2 H142 3.08(2) . '2 656' ? C8 H21 3.08(3) . . ? H21 H8 3.08(4) . . ? H91 H91 3.09(4) . '3 666' ? O2 H91 3.09(2) . '3 666' ? C1 H42 3.09(3) . . ? C16 H32 3.10(3) . '3 767' ? C12 H181 3.10(2) . . ? C11 H52 3.103(15) . '1 655' ? C7 H8 3.11(2) . . ? C11 H31 3.11(3) . . ? C5 H171 3.11(2) . '1 455' ? C12 H11 3.113(18) . . ? O5 H181 3.12(2) . '1 455' ? O5 H91 3.12(3) . . ? H42 H182 3.13(4) . '2 656' ? H41 H51 3.13(3) . '3 667' ? C4 C7 3.134(4) . . ? C15 H92 3.14(3) . 4 ? O3 H171 3.14(3) . '1 455' ? C10 H8 3.14(3) . . ? H21 H11 3.14(4) . . ? C12 H152 3.16(2) . '4 554' ? C18 H22 3.16(3) . '2 746' ? H31 H151 3.16(4) . '3 767' ? C10 H181 3.16(2) . . ? C2 O1 3.161(3) . . ? C7 H91 3.17(2) . '3 666' ? C9 O5 3.171(4) . . ? C1 H91 3.17(2) . . ? C3 O4 3.176(3) . . ? C13 H162 3.18(3) . . ? C6 H8 3.19(3) . . ? C2 O4 3.186(3) . . ? O2 H162 3.19(3) . '2 656' ? C3 H41 3.19(2) . '3 667' ? C2 H182 3.20(3) . '2 756' ? H32 H51 3.20(4) . '3 667' ? C17 H22 3.20(2) . '2 746' ? H42 H151 3.20(5) . '3 667' ? C14 H51 3.20(2) . . ? O4 H142 3.20(2) . . ? C4 H141 3.21(3) . '3 667' ? O5 H172 3.21(3) . '1 455' ? O1 H92 3.22(3) . . ? C5 C12 3.222(4) . . ? C12 C18 3.229(4) . . ? C10 H52 3.23(2) . . ? C3 H151 3.23(3) . '3 767' ? H21 H152 3.23(4) . '3 767' ? C2 H11 3.23(2) . . ? C12 H172 3.23(3) . '1 455' ? C9 H162 3.24(3) . '4 554' ? C6 H31 3.24(3) . . ? C15 H41 3.25(3) . '3 667' ? C2 C7 3.255(4) . . ? C9 H152 3.25(3) . '4 554' ? H92 H181 3.26(3) . . ? O3 H22 3.26(2) . '2 646' ? C15 H32 3.26(3) . '3 767' ? C11 H91 3.27(2) . . ? H41 H152 3.27(4) . '3 667' ? O2 H11 3.27(2) . '1 455' ? H21 H181 3.27(4) . '2 756' ? O2 C8 3.280(4) . '1 455' ? O4 H182 3.284(16) . . ? C17 H142 3.29(3) . . ? C15 H182 3.29(3) . . ? C18 H151 3.29(3) . . ? H21 H41 3.30(3) . '1 655' ? C6 H92 3.30(3) . . ? O5 H42 3.30(3) . '2 646' ? C16 H8 3.30(3) . '2 746' ? O2 H21 3.30(2) . '1 455' ? O5 H152 3.30(3) . '4 554' ? O3 H11 3.30(2) . . ? H92 H161 3.31(4) . '4 554' ? C9 H142 3.32(3) . '4 554' ? H42 H141 3.32(4) . '3 667' ? C14 H171 3.32(3) . . ? C6 H41 3.323(19) . . ? H31 H51 3.33(4) . '3 667' ? O4 H21 3.33(3) . . ? O3 H42 3.33(3) . '2 646' ? C3 H141 3.33(3) . '3 667' ? C3 C11 3.337(4) . . ? C14 H41 3.34(2) . '3 667' ? H91 H162 3.34(4) . '4 554' ? C2 H172 3.35(3) . '2 756' ? C11 H171 3.35(3) . . ? C4 H31 3.35(3) . '3 667' ? C1 H32 3.35(3) . . ? C7 H142 3.35(2) . '2 656' ? C17 H141 3.35(2) . '1 655' ? C14 H161 3.35(2) . . ? C13 H172 3.35(2) . . ? C6 O3 3.356(3) . . ? C7 H51 3.36(3) . . ? C6 O5 3.361(3) . . ? C16 H181 3.366(14) . . ? C17 H11 3.37(2) . . ? C16 H141 3.37(2) . . ? C17 H152 3.37(2) . . ? C8 H162 3.37(2) . '2 756' ? C18 H141 3.37(2) . . ? C13 H152 3.373(15) . . ? C14 H172 3.38(2) . '1 455' ? C4 H151 3.38(3) . '3 667' ? C14 H181 3.384(17) . . ? C2 H151 3.38(3) . '3 767' ? O3 C17 3.384(3) . '1 455' ? C18 H161 3.39(2) . . ? C7 H182 3.39(2) . '2 656' ? C1 H52 3.395(15) . . ? C8 H172 3.40(3) . '2 756' ? O2 C8 3.396(4) . . ? C15 H172 3.40(2) . . ? C4 H21 3.398(14) . . ? C3 H52 3.40(2) . . ? C2 H41 3.40(2) . . ? C3 H161 3.41(3) . '3 767' ? H91 H11 3.41(3) . . ? C5 H22 3.41(2) . . ? O2 H91 3.42(3) . . ? C5 H32 3.42(3) . . ? H142 H161 3.43(4) . '1 455' ? H32 H41 3.43(3) . '3 667' ? C17 H8 3.43(3) . '2 746' ? C12 H182 3.43(3) . . ? C7 C11 3.434(4) . . ? C6 H21 3.44(2) . . ? O5 H141 3.44(3) . '4 554' ? C4 H21 3.441(13) . '1 455' ? O5 C16 3.443(4) . '4 454' ? C2 H51 3.45(3) . . ? C1 C12 3.447(4) . . ? C4 H41 3.45(2) . '3 667' ? C11 H22 3.45(2) . . ? C18 H21 3.45(3) . '2 746' ? C12 H52 3.46(3) . . ? C10 H152 3.46(2) . '4 554' ? C5 H11 3.463(18) . '1 455' ? H31 H151 3.46(3) . . ? H152 H182 3.47(4) . 4 ? O4 H41 3.474(18) . '3 667' ? O4 H52 3.475(17) . '1 655' ? H91 H152 3.48(4) . '4 554' ? C17 H32 3.49(3) . '3 767' ? C15 H21 3.49(3) . '3 767' ? C15 H42 3.49(3) . '3 667' ? C5 O3 3.493(3) . . ? C17 H51 3.49(3) . '1 655' ? C12 H22 3.50(2) . '2 646' ? C5 H21 3.498(18) . '1 455' ? O1 H162 3.51(3) . '2 756' ? C12 H171 3.51(4) . '1 455' ? H51 H172 3.51(3) . '1 455' ? C2 C10 3.518(4) . . ? C10 C18 3.520(4) . . ? C18 H152 3.522(15) . '4 554' ? O1 H42 3.52(3) . . ? C2 H181 3.53(2) . '2 756' ? C2 H52 3.529(18) . '1 655' ? C1 H52 3.532(14) . '1 655' ? H32 H152 3.53(4) . '3 767' ? C4 O2 3.535(4) . . ? O1 C11 3.535(3) . . ? H141 H162 3.55(3) . . ? C4 H152 3.55(3) . '3 667' ? O5 C13 3.554(3) . . ? O2 C18 3.557(3) . '2 656' ? C12 H42 3.56(3) . '2 646' ? O4 C16 3.565(3) . . ? O2 C10 3.571(3) . . ? C1 O2 3.571(3) . . ? O2 H92 3.58(3) . '3 666' ? O5 H92 3.58(2) . . ? C3 O5 3.578(4) . '2 656' ? H161 H181 3.58(3) . 4 ? C5 H141 3.59(3) . . ? C3 H51 3.60(3) . '3 667' ? C14 H92 3.60(3) . 4 ? C2 O5 3.598(3) . '2 656' ? C5 O1 3.599(4) . . ? H11 H152 3.60(3) . '4 554' ? H162 H181 3.60(3) . . ? C4 O4 3.603(3) . . ? O1 C9 3.604(3) . '3 666' ? O5 H142 3.60(3) . '4 554' ? C12 C14 3.611(4) . . ? H8 H92 3.62(4) . '3 766' ? H11 H182 3.62(3) . . ? C7 C12 3.622(4) . . ? H151 H172 3.62(4) . . ? C9 O4 3.624(3) . . ? C13 H172 3.63(2) . '1 455' ? H142 H161 3.63(4) . . ? H141 H182 3.63(4) . . ? C6 C13 3.634(3) . . ? C15 H181 3.638(15) . 4 ? C14 H32 3.64(3) . '3 667' ? C11 C14 3.644(4) . . ? C12 H161 3.65(2) . '4 454' ? O3 H152 3.649(19) . '4 554' ? C16 H141 3.65(2) . '1 655' ? O5 H171 3.65(4) . '1 455' ? C14 H171 3.66(3) . '1 455' ? C18 H8 3.66(3) . '2 746' ? C7 H8 3.66(2) . '1 455' ? C7 H92 3.67(2) . . ? C14 H91 3.68(3) . 4 ? C5 C8 3.676(4) . . ? C8 H182 3.68(2) . '2 756' ? C1 O2 3.680(3) . '1 655' ? O2 H92 3.68(2) . '1 455' ? C11 C17 3.685(4) . . ? C5 H31 3.69(3) . '3 667' ? O2 C9 3.692(4) . . ? C17 H142 3.69(3) . '1 655' ? C12 H141 3.71(3) . . ? O2 C9 3.708(4) . '3 666' ? C8 H91 3.71(2) . '3 666' ? C1 C13 3.710(3) . . ? C5 C13 3.712(4) . . ? C11 O5 3.719(3) . . ? O5 H162 3.72(3) . '4 454' ? O5 H11 3.72(2) . '1 455' ? C8 O4 3.722(3) . . ? C2 C18 3.724(4) . '2 756' ? C14 H161 3.73(2) . '1 455' ? C9 O3 3.731(3) . . ? C9 H181 3.73(2) . . ? C8 C12 3.738(4) . . ? O1 C17 3.741(3) . '2 756' ? O3 C15 3.747(3) . . ? C17 H52 3.76(3) . '1 655' ? O5 H51 3.76(2) . . ? C12 H181 3.76(2) . '1 455' ? C11 H182 3.764(15) . . ? C4 C11 3.768(4) . . ? O3 C17 3.772(3) . . ? C3 C7 3.776(4) . . ? C5 H41 3.778(17) . '3 667' ? C4 C15 3.785(4) . '3 667' ? O5 C17 3.789(4) . '1 455' ? O4 H92 3.80(3) . . ? C12 H142 3.81(3) . . ? C3 H171 3.81(3) . '3 767' ? O1 H52 3.81(2) . . ? C1 H172 3.82(3) . '2 756' ? C4 H51 3.82(3) . '3 667' ? C2 H161 3.82(3) . '3 767' ? O4 H52 3.821(16) . . ? C9 C15 3.823(4) . '4 554' ? O4 H152 3.828(19) . . ? C13 H161 3.83(2) . . ? O5 H52 3.83(3) . . ? O1 H161 3.83(3) . '2 756' ? C9 H91 3.84(3) . '3 666' ? C1 H41 3.84(2) . . ? C17 H141 3.84(2) . . ? C11 H141 3.84(3) . . ? C15 H181 3.841(14) . . ? C1 H182 3.84(2) . '2 756' ? C12 C17 3.847(4) . '1 455' ? C14 H172 3.85(2) . . ? C18 H42 3.85(3) . '2 646' ? C18 H152 3.856(15) . . ? O1 H21 3.86(2) . . ? O1 O3 3.857(3) . '2 656' ? C4 O5 3.857(4) . '2 656' ? C2 H152 3.86(2) . '3 767' ? C2 C9 3.861(4) . . ? C6 H32 3.87(3) . . ? O2 H51 3.87(3) . . ? O3 H52 3.87(3) . . ? O1 C16 3.869(4) . '2 756' ? O5 C14 3.870(4) . '4 554' ? O5 C18 3.871(4) . '1 455' ? C2 O2 3.873(4) . '1 655' ? C11 H52 3.875(15) . . ? C13 H31 3.88(2) . . ? C15 H91 3.88(3) . 4 ? O2 C11 3.887(3) . '1 455' ? C7 H11 3.89(2) . '1 455' ? O2 H22 3.89(3) . . ? O1 C14 3.892(3) . '2 656' ? C5 O5 3.894(4) . . ? C14 H42 3.89(3) . '3 667' ? O2 C14 3.896(3) . '2 656' ? C7 H172 3.90(2) . '2 756' ? O4 H172 3.90(2) . . ? C5 H32 3.90(3) . '3 667' ? C3 C8 3.903(4) . . ? C2 H52 3.911(17) . . ? C5 C9 3.911(4) . . ? C4 C10 3.920(4) . . ? C5 H21 3.925(17) . . ? C4 C14 3.925(4) . '3 667' ? C13 H171 3.93(3) . '1 455' ? O3 H92 3.93(3) . . ? C14 C17 3.934(4) . '1 455' ? O5 H152 3.94(3) . '4 454' ? O1 O1 3.940(3) . '3 666' ? O1 H182 3.95(3) . '2 656' ? C6 H11 3.951(16) . '1 455' ? O2 O3 3.955(3) . '2 656' ? O1 H11 3.96(2) . . ? C7 O5 3.957(4) . . ? C1 O3 3.960(3) . . ? C4 O1 3.961(4) . . ? O1 H92 3.96(3) . '3 666' ? C9 C16 3.963(4) . '4 554' ? C10 H22 3.97(2) . . ? C2 H42 3.97(3) . '1 655' ? C16 H142 3.97(3) . '1 655' ? C8 C17 3.982(4) . '2 756' ? O3 H181 3.98(2) . '1 455' ? C11 H152 3.99(2) . '4 554' ? C3 C15 3.995(4) . '3 767' ? C3 C4 3.996(4) . '3 667' ? C7 O3 3.998(3) . '2 656' ? C7 C9 4.004(4) . '3 666' ? C7 H41 4.005(17) . . ? C9 C14 4.005(4) . '4 554' ? C11 H151 4.01(4) . . ? C10 H21 4.01(3) . . ? C12 H142 4.01(3) . '4 554' ? C2 C17 4.014(4) . '2 756' ? C8 H42 4.02(3) . . ? O5 C15 4.024(4) . '4 554' ? C16 H181 4.024(14) . 4 ? O2 C16 4.025(4) . '2 656' ? O5 O4 4.028(3) . . ? C12 H32 4.03(3) . '2 646' ? C8 C16 4.029(4) . '2 756' ? C3 C16 4.039(4) . '3 767' ? O2 C13 4.047(3) . '2 656' ? C12 C15 4.050(4) . '4 554' ? C2 C15 4.057(4) . '3 767' ? O2 C9 4.059(4) . '1 455' ? C3 C10 4.059(4) . . ? C5 C17 4.063(4) . '1 455' ? C4 C4 4.073(4) . '3 667' ? C5 C11 4.080(4) . '1 455' ? C9 C13 4.098(4) . . ? C10 C14 4.116(4) . . ? C4 C8 4.124(4) . . ? C3 O1 4.164(4) . . ? O5 C15 4.164(4) . '4 454' ? C5 C14 4.165(4) . . ? C3 C5 4.177(4) . '3 667' ? O5 C18 4.186(4) . . ? O3 C16 4.199(3) . . ? O2 C17 4.199(4) . '2 656' ? C2 O3 4.199(3) . '2 656' ? C4 O3 4.242(4) . '2 656' ? C2 O2 4.242(4) . . ? C7 C14 4.256(4) . '2 656' ? C3 C14 4.258(4) . '3 667' ? C7 O4 4.265(3) . . ? O1 C12 4.266(3) . . ? O2 C12 4.267(3) . . ? C7 O1 4.273(4) . '3 666' ? C11 C15 4.279(4) . . ? O3 C18 4.280(3) . '1 455' ? O2 C8 4.284(4) . '3 666' ? C7 C18 4.292(4) . '2 656' ? C10 C15 4.292(4) . '4 554' ? C12 C14 4.292(4) . '4 554' ? C13 C17 4.300(4) . '1 455' ? C8 C18 4.310(4) . '2 756' ? C14 C16 4.316(4) . '1 455' ? O2 O5 4.330(3) . . ? C4 C12 4.335(4) . '2 656' ? C5 O4 4.335(3) . '1 455' ? C2 C12 4.344(4) . '2 656' ? C12 C18 4.347(4) . '1 455' ? O1 C8 4.365(3) . '3 666' ? C1 O5 4.385(3) . . ? C2 C5 4.386(4) . '1 655' ? C3 C12 4.401(4) . '2 656' ? O1 C13 4.402(3) . '2 656' ? C9 C18 4.403(4) . . ? C8 O5 4.408(4) . . ? C7 C8 4.424(4) . '1 455' ? C15 C18 4.434(4) . 4 ? C3 C17 4.437(4) . '3 767' ? C2 C4 4.440(4) . '1 655' ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 680 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .797 _reflns_d_resolution_low 10.783 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 4.1 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 243 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_radiation_detector ? _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 22 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .06 _refine_ls_wR_factor_all .057 _refine_ls_goodness_of_fit_all .896 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end