# Electronic Supplementary Material (ESI) for RSC Advances. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_lslt99 _database_code_depnum_ccdc_archive 'CCDC 2070473' loop_ _audit_author_name _audit_author_address 'Tao Feng' ;South Central University for Nationalities China ; _audit_update_record ; 2021-03-15 deposited with the CCDC. 2021-05-19 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 N O5' _chemical_formula_iupac ? _chemical_formula_weight 429.54 _chemical_absolute_configuration ad _chemical_melting_point ? _space_group_crystal_system hexagonal _space_group_name_H-M_alt 'P 65' _space_group_name_Hall 'P 65' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z+5/6' 'y, -x+y, z+1/6' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' _cell_length_a 17.6760(4) _cell_length_b 17.6760(4) _cell_length_c 13.1360(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3554.36(19) _cell_formula_units_Z 6 _cell_measurement_reflns_used 9847 _cell_measurement_theta_min 4.4353 _cell_measurement_theta_max 78.9492 _cell_measurement_temperature 156.(2) _exptl_crystal_description NEEDLE _exptl_crystal_colour 'light colourless' _exptl_crystal_size_max 0.153 _exptl_crystal_size_mid 0.096 _exptl_crystal_size_min 0.095 _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 _exptl_special_details ; ; _diffrn_ambient_temperature 156.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 83650 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 79.21 _diffrn_reflns_theta_full 79.21 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _refine_special_details ; ; _reflns_number_total 5041 _reflns_number_gt 4897 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.0688 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_number_reflns 5041 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.4945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.126 _refine_diff_density_min -0.153 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 2229 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.03(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_publication_material ? loop_ _atom_site_type_symbol _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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.67143(10) 0.50436(10) 0.51326(13) 0.0230(3) Uani d . . . 1 . . H H1 0.7484(13) 0.3794(13) 0.5630(17) 0.025(5) Uiso d . . . 1 . . O O2 0.53739(8) 0.40427(8) 0.42595(10) 0.0287(2) Uani d . . . 1 . . H H2 0.5136(9) 0.3629(17) 0.384(2) 0.043 Uiso calc U . R 1 . . C C2 0.73508(10) 0.48222(10) 0.56716(12) 0.0231(3) Uani d . . . 1 . . O O3 0.67282(8) 0.46285(7) 0.34544(9) 0.0283(2) Uani d . . . 1 . . C C3 0.64301(10) 0.35492(10) 0.47137(13) 0.0251(3) Uani d . . . 1 . . H H3 0.659949 0.332825 0.41043 0.03 Uiso calc U . R 1 . . C C4 0.62472(10) 0.42848(10) 0.43708(13) 0.0242(3) Uani d . . . 1 . . O O4 0.55776(8) 0.45868(8) 0.64155(10) 0.0320(3) Uani d . . . 1 . . O O5 0.55061(9) 0.29931(9) 0.62502(10) 0.0350(3) Uani d . . . 1 . . H H5A 0.5429(18) 0.3416(19) 0.6190(4) 0.053 Uiso calc U . R 1 . . C C5 0.71050(10) 0.55723(10) 0.33798(13) 0.0255(3) Uani d . . . 1 . . H H5 0.771586 0.582028 0.312127 0.031 Uiso calc U . R 1 . . N N1 0.71970(9) 0.40390(9) 0.53535(11) 0.0248(3) Uani d . . . 1 . . O O1 0.79167(7) 0.53015(7) 0.62818(9) 0.0263(2) Uani d . . . 1 . . C C6 0.71633(10) 0.58932(10) 0.44966(13) 0.0243(3) Uani d . . . 1 . . H H6 0.779196 0.623923 0.469904 0.029 Uiso calc U . R 1 . . C C7 0.66971(11) 0.64196(11) 0.47919(13) 0.0272(3) Uani d . . . 1 . . H H7 0.619836 0.624783 0.431144 0.033 Uiso calc U . R 1 . . C C11 0.82126(12) 0.80251(11) 0.73167(15) 0.0332(4) Uani d . . . 1 . . H H11A 0.868511 0.795712 0.700473 0.04 Uiso calc U . R 1 . . H H11B 0.840963 0.865681 0.733755 0.04 Uiso calc U . R 1 . . C C10 0.73916(11) 0.75585(11) 0.66491(14) 0.0300(4) Uani d . . . 1 . . H H10 0.693079 0.76627 0.694656 0.036 Uiso calc U . R 1 . . C C9 0.75648(13) 0.78971(11) 0.55740(15) 0.0341(4) Uani d . . . 1 . . H H9 0.790498 0.851164 0.548335 0.041 Uiso calc U . R 1 . . C C8 0.72801(12) 0.74054(11) 0.47386(15) 0.0325(4) Uani d . . . 1 . . C C12 0.80569(12) 0.76699(12) 0.84050(15) 0.0343(4) Uani d . . . 1 . . H H12 0.762303 0.779963 0.873095 0.041 Uiso calc U . R 1 . . C C17 0.61180(10) 0.51599(11) 0.58807(13) 0.0257(3) Uani d . . . 1 . . C C16 0.63150(11) 0.60945(11) 0.58670(14) 0.0271(3) Uani d . . . 1 . . C C15 0.70567(11) 0.65768(10) 0.66625(13) 0.0266(3) Uani d . . . 1 . . H H15 0.755425 0.649881 0.643866 0.032 Uiso calc U . R 1 . . C C14 0.68374(12) 0.62313(12) 0.77548(15) 0.0328(4) Uani d . . . 1 . . H H14A 0.639083 0.635247 0.804159 0.039 Uiso calc U . R 1 . . H H14B 0.659882 0.559143 0.776009 0.039 Uiso calc U . R 1 . . C C13 0.76664(13) 0.66802(12) 0.83951(15) 0.0350(4) Uani d . . . 1 . . H H13A 0.810111 0.65379 0.811727 0.042 Uiso calc U . R 1 . . H H13B 0.753011 0.645613 0.910133 0.042 Uiso calc U . R 1 . . C C19 0.59319(12) 0.20646(11) 0.54738(16) 0.0348(4) Uani d . . . 1 . . H H19A 0.606178 0.188087 0.482441 0.052 Uiso calc U . R 1 . . H H19B 0.544181 0.15615 0.580527 0.052 Uiso calc U . R 1 . . H H19C 0.644707 0.229878 0.591562 0.052 Uiso calc U . R 1 . . C C18 0.56912(11) 0.27675(11) 0.52815(14) 0.0290(3) Uani d . . . 1 . . H H18 0.514997 0.251455 0.485597 0.035 Uiso calc U . R 1 . . C C20 0.66120(11) 0.57860(11) 0.26173(14) 0.0278(3) Uani d . . . 1 . . H H20 0.602634 0.563311 0.276489 0.033 Uiso calc U . R 1 . . C C21 0.69597(12) 0.61788(14) 0.17476(16) 0.0398(4) Uani d . . . 1 . . H H21 0.75411 0.63114 0.161068 0.048 Uiso calc U . R 1 . . C C22 0.65195(15) 0.64342(19) 0.0957(2) 0.0582(7) Uani d . . . 1 . . H H22A 0.688571 0.705696 0.080067 0.087 Uiso calc U . R 1 . . H H22B 0.595245 0.632263 0.121498 0.087 Uiso calc U . R 1 . . H H22C 0.643188 0.609038 0.03382 0.087 Uiso calc U . R 1 . . C C23 0.75024(16) 0.78050(13) 0.36931(17) 0.0430(5) Uani d . . . 1 . . H H23A 0.783706 0.758692 0.332493 0.065 Uiso calc U . R 1 . . H H23B 0.785226 0.844215 0.375268 0.065 Uiso calc U . R 1 . . H H23C 0.696289 0.764637 0.332042 0.065 Uiso calc U . R 1 . . C C24 0.88938(14) 0.81108(15) 0.90395(18) 0.0439(5) Uani d . . . 1 . . H H24A 0.932813 0.798699 0.873969 0.066 Uiso calc U . R 1 . . H H24B 0.876479 0.788471 0.973717 0.066 Uiso calc U . R 1 . . H H24C 0.912503 0.874339 0.904851 0.066 Uiso calc U . R 1 . . C C25 0.54996(12) 0.61592(13) 0.60855(16) 0.0346(4) Uani d . . . 1 . . H H25A 0.563289 0.67628 0.598386 0.052 Uiso calc U . R 1 . . H H25B 0.531362 0.598372 0.67907 0.052 Uiso calc U . R 1 . . H H25C 0.502952 0.57724 0.562198 0.052 Uiso calc U . R 1 . . 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 0.0238(7) 0.0227(7) 0.0236(8) 0.0125(6) 0.0003(6) -0.0002(6) O2 0.0266(6) 0.0285(6) 0.0327(7) 0.0151(5) -0.0050(5) -0.0056(5) C2 0.0228(7) 0.0246(7) 0.0225(8) 0.0124(6) 0.0040(6) 0.0027(6) O3 0.0370(6) 0.0241(5) 0.0248(6) 0.0160(5) 0.0029(5) -0.0002(4) C3 0.0279(7) 0.0232(7) 0.0254(8) 0.0137(6) -0.0019(6) -0.0012(6) C4 0.0265(7) 0.0242(7) 0.0230(8) 0.0135(6) 0.0004(6) -0.0001(6) O4 0.0291(6) 0.0304(6) 0.0330(7) 0.0123(5) 0.0067(5) -0.0002(5) O5 0.0369(6) 0.0360(7) 0.0319(7) 0.0180(5) 0.0052(5) 0.0050(5) C5 0.0260(7) 0.0238(7) 0.0270(9) 0.0127(6) 0.0025(6) 0.0009(6) N1 0.0243(6) 0.0241(6) 0.0289(7) 0.0142(5) -0.0010(5) -0.0001(5) O1 0.0254(5) 0.0266(5) 0.0272(6) 0.0132(4) -0.0016(4) -0.0009(4) C6 0.0255(7) 0.0233(7) 0.0264(8) 0.0139(6) -0.0001(6) 0.0010(6) C7 0.0306(8) 0.0276(8) 0.0287(9) 0.0185(6) -0.0014(6) -0.0010(6) C11 0.0349(9) 0.0292(8) 0.0352(10) 0.0158(7) 0.0011(7) -0.0057(7) C10 0.0341(8) 0.0271(8) 0.0339(10) 0.0191(7) 0.0013(7) -0.0028(7) C9 0.0423(10) 0.0256(8) 0.0385(11) 0.0200(7) 0.0012(8) 0.0013(7) C8 0.0411(9) 0.0284(8) 0.0351(10) 0.0226(7) 0.0015(7) 0.0025(7) C12 0.0369(9) 0.0356(9) 0.0336(10) 0.0205(8) -0.0008(7) -0.0078(7) C17 0.0239(7) 0.0283(8) 0.0254(8) 0.0133(6) -0.0018(6) -0.0038(6) C16 0.0280(8) 0.0287(8) 0.0296(9) 0.0178(6) 0.0011(6) -0.0015(6) C15 0.0293(8) 0.0265(7) 0.0275(9) 0.0165(6) 0.0004(6) -0.0026(6) C14 0.0387(9) 0.0292(8) 0.0301(9) 0.0167(7) 0.0024(7) -0.0006(7) C13 0.0443(10) 0.0357(9) 0.0290(9) 0.0230(8) -0.0009(7) -0.0029(7) C19 0.0389(9) 0.0260(8) 0.0364(10) 0.0138(7) -0.0072(8) 0.0021(7) C18 0.0293(8) 0.0249(7) 0.0301(9) 0.0114(7) -0.0042(7) 0.0008(6) C20 0.0271(7) 0.0258(7) 0.0292(9) 0.0122(6) 0.0010(6) 0.0006(6) C21 0.0298(9) 0.0474(11) 0.0360(11) 0.0146(8) 0.0018(7) 0.0104(8) C22 0.0411(11) 0.0743(16) 0.0482(14) 0.0205(11) 0.0021(10) 0.0289(12) C23 0.0638(13) 0.0313(9) 0.0362(11) 0.0254(9) 0.0016(9) 0.0047(8) C24 0.0429(10) 0.0496(11) 0.0398(11) 0.0237(9) -0.0058(8) -0.0104(9) C25 0.0328(9) 0.0397(9) 0.0401(11) 0.0247(8) 0.0003(7) -0.0048(8) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C17 . 1.528(2) ? C1 C2 . 1.536(2) ? C1 C4 . 1.541(2) ? C1 C6 . 1.546(2) ? O2 C4 . 1.3881(19) ? O2 H2 . 0.84(3) ? C2 O1 . 1.230(2) ? C2 N1 . 1.337(2) ? O3 C4 . 1.423(2) ? O3 C5 . 1.4578(19) ? C3 N1 . 1.456(2) ? C3 C18 . 1.538(2) ? C3 C4 . 1.555(2) ? C3 H3 . 1.0 ? O4 C17 . 1.210(2) ? O5 C18 . 1.420(2) ? O5 H5A . 0.83(3) ? C5 C20 . 1.495(2) ? C5 C6 . 1.558(2) ? C5 H5 . 1.0 ? N1 H1 . 0.89(2) ? C6 C7 . 1.569(2) ? C6 H6 . 1.0 ? C7 C8 . 1.519(2) ? C7 C16 . 1.547(2) ? C7 H7 . 1.0 ? C11 C12 . 1.530(3) ? C11 C10 . 1.536(2) ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C10 C9 . 1.504(3) ? C10 C15 . 1.528(2) ? C10 H10 . 1.0 ? C9 C8 . 1.333(3) ? C9 H9 . 0.95 ? C8 C23 . 1.504(3) ? C12 C13 . 1.526(3) ? C12 C24 . 1.529(3) ? C12 H12 . 1.0 ? C17 C16 . 1.508(2) ? C16 C25 . 1.529(2) ? C16 C15 . 1.556(2) ? C15 C14 . 1.531(3) ? C15 H15 . 1.0 ? C14 C13 . 1.524(3) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C13 H13A . 0.99 ? C13 H13B . 0.99 ? C19 C18 . 1.522(2) ? C19 H19A . 0.98 ? C19 H19B . 0.98 ? C19 H19C . 0.98 ? C18 H18 . 1.0 ? C20 C21 . 1.318(3) ? C20 H20 . 0.95 ? C21 C22 . 1.496(3) ? C21 H21 . 0.95 ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C23 H23A . 0.98 ? C23 H23B . 0.98 ? C23 H23C . 0.98 ? C24 H24A . 0.98 ? C24 H24B . 0.98 ? C24 H24C . 0.98 ? C25 H25A . 0.98 ? C25 H25B . 0.98 ? C25 H25C . 0.98 ? 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_3 _geom_angle _geom_angle_publ_flag C17 C1 C2 . . 112.34(13) ? C17 C1 C4 . . 115.42(13) ? C2 C1 C4 . . 102.68(12) ? C17 C1 C6 . . 105.68(12) ? C2 C1 C6 . . 114.25(12) ? C4 C1 C6 . . 106.61(13) ? C4 O2 H2 . . 109.5 ? O1 C2 N1 . . 126.23(15) ? O1 C2 C1 . . 124.86(14) ? N1 C2 C1 . . 108.90(13) ? C4 O3 C5 . . 112.28(12) ? N1 C3 C18 . . 111.96(14) ? N1 C3 C4 . . 101.01(12) ? C18 C3 C4 . . 116.97(13) ? N1 C3 H3 . . 108.8 ? C18 C3 H3 . . 108.8 ? C4 C3 H3 . . 108.8 ? O2 C4 O3 . . 112.18(14) ? O2 C4 C1 . . 111.47(13) ? O3 C4 C1 . . 103.42(12) ? O2 C4 C3 . . 115.90(13) ? O3 C4 C3 . . 105.81(12) ? C1 C4 C3 . . 107.14(13) ? C18 O5 H5A . . 109.5 ? O3 C5 C20 . . 110.10(13) ? O3 C5 C6 . . 105.22(12) ? C20 C5 C6 . . 118.67(13) ? O3 C5 H5 . . 107.4 ? C20 C5 H5 . . 107.4 ? C6 C5 H5 . . 107.4 ? C2 N1 C3 . . 116.29(13) ? C2 N1 H1 . . 120.3(13) ? C3 N1 H1 . . 122.2(13) ? C1 C6 C5 . . 104.29(12) ? C1 C6 C7 . . 106.00(13) ? C5 C6 C7 . . 119.34(13) ? C1 C6 H6 . . 108.9 ? C5 C6 H6 . . 108.9 ? C7 C6 H6 . . 108.9 ? C8 C7 C16 . . 112.83(14) ? C8 C7 C6 . . 114.37(14) ? C16 C7 C6 . . 105.46(13) ? C8 C7 H7 . . 108.0 ? C16 C7 H7 . . 108.0 ? C6 C7 H7 . . 108.0 ? C12 C11 C10 . . 112.67(15) ? C12 C11 H11A . . 109.1 ? C10 C11 H11A . . 109.1 ? C12 C11 H11B . . 109.1 ? C10 C11 H11B . . 109.1 ? H11A C11 H11B . . 107.8 ? C9 C10 C15 . . 110.42(14) ? C9 C10 C11 . . 111.88(15) ? C15 C10 C11 . . 109.19(14) ? C9 C10 H10 . . 108.4 ? C15 C10 H10 . . 108.4 ? C11 C10 H10 . . 108.4 ? C8 C9 C10 . . 125.33(16) ? C8 C9 H9 . . 117.3 ? C10 C9 H9 . . 117.3 ? C9 C8 C23 . . 121.40(16) ? C9 C8 C7 . . 121.91(16) ? C23 C8 C7 . . 116.67(16) ? C13 C12 C24 . . 110.90(17) ? C13 C12 C11 . . 110.35(15) ? C24 C12 C11 . . 111.75(16) ? C13 C12 H12 . . 107.9 ? C24 C12 H12 . . 107.9 ? C11 C12 H12 . . 107.9 ? O4 C17 C16 . . 125.24(15) ? O4 C17 C1 . . 124.72(15) ? C16 C17 C1 . . 110.03(13) ? C17 C16 C25 . . 111.69(14) ? C17 C16 C7 . . 103.69(13) ? C25 C16 C7 . . 113.35(15) ? C17 C16 C15 . . 105.19(13) ? C25 C16 C15 . . 113.62(14) ? C7 C16 C15 . . 108.54(13) ? C10 C15 C14 . . 109.92(14) ? C10 C15 C16 . . 110.88(14) ? C14 C15 C16 . . 115.78(14) ? C10 C15 H15 . . 106.6 ? C14 C15 H15 . . 106.6 ? C16 C15 H15 . . 106.6 ? C13 C14 C15 . . 108.89(15) ? C13 C14 H14A . . 109.9 ? C15 C14 H14A . . 109.9 ? C13 C14 H14B . . 109.9 ? C15 C14 H14B . . 109.9 ? H14A C14 H14B . . 108.3 ? C14 C13 C12 . . 111.57(16) ? C14 C13 H13A . . 109.3 ? C12 C13 H13A . . 109.3 ? C14 C13 H13B . . 109.3 ? C12 C13 H13B . . 109.3 ? H13A C13 H13B . . 108.0 ? C18 C19 H19A . . 109.5 ? C18 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C18 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? O5 C18 C19 . . 106.16(14) ? O5 C18 C3 . . 113.18(14) ? C19 C18 C3 . . 110.82(14) ? O5 C18 H18 . . 108.9 ? C19 C18 H18 . . 108.9 ? C3 C18 H18 . . 108.9 ? C21 C20 C5 . . 122.45(16) ? C21 C20 H20 . . 118.8 ? C5 C20 H20 . . 118.8 ? C20 C21 C22 . . 125.76(18) ? C20 C21 H21 . . 117.1 ? C22 C21 H21 . . 117.1 ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? C8 C23 H23A . . 109.5 ? C8 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? C8 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? C12 C24 H24A . . 109.5 ? C12 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C12 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? C16 C25 H25A . . 109.5 ? C16 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? C16 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? 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 C17 C1 C2 O1 . . . . -62.5(2) ? C4 C1 C2 O1 . . . . 172.93(15) ? C6 C1 C2 O1 . . . . 57.9(2) ? C17 C1 C2 N1 . . . . 118.69(15) ? C4 C1 C2 N1 . . . . -5.93(16) ? C6 C1 C2 N1 . . . . -120.94(15) ? C5 O3 C4 O2 . . . . 90.26(15) ? C5 O3 C4 C1 . . . . -29.97(16) ? C5 O3 C4 C3 . . . . -142.45(13) ? C17 C1 C4 O2 . . . . 21.25(19) ? C2 C1 C4 O2 . . . . 143.81(13) ? C6 C1 C4 O2 . . . . -95.76(15) ? C17 C1 C4 O3 . . . . 141.97(13) ? C2 C1 C4 O3 . . . . -95.47(13) ? C6 C1 C4 O3 . . . . 24.96(15) ? C17 C1 C4 C3 . . . . -106.52(15) ? C2 C1 C4 C3 . . . . 16.05(15) ? C6 C1 C4 C3 . . . . 136.47(13) ? N1 C3 C4 O2 . . . . -144.84(14) ? C18 C3 C4 O2 . . . . -23.1(2) ? N1 C3 C4 O3 . . . . 90.15(14) ? C18 C3 C4 O3 . . . . -148.07(14) ? N1 C3 C4 C1 . . . . -19.71(16) ? C18 C3 C4 C1 . . . . 102.07(16) ? C4 O3 C5 C20 . . . . -106.38(15) ? C4 O3 C5 C6 . . . . 22.60(16) ? O1 C2 N1 C3 . . . . 173.48(15) ? C1 C2 N1 C3 . . . . -7.69(19) ? C18 C3 N1 C2 . . . . -107.83(16) ? C4 C3 N1 C2 . . . . 17.38(18) ? C17 C1 C6 C5 . . . . -135.32(13) ? C2 C1 C6 C5 . . . . 100.66(15) ? C4 C1 C6 C5 . . . . -12.02(15) ? C17 C1 C6 C7 . . . . -8.51(16) ? C2 C1 C6 C7 . . . . -132.54(14) ? C4 C1 C6 C7 . . . . 114.79(14) ? O3 C5 C6 C1 . . . . -5.02(15) ? C20 C5 C6 C1 . . . . 118.68(15) ? O3 C5 C6 C7 . . . . -123.02(14) ? C20 C5 C6 C7 . . . . 0.7(2) ? C1 C6 C7 C8 . . . . 148.88(14) ? C5 C6 C7 C8 . . . . -94.01(18) ? C1 C6 C7 C16 . . . . 24.32(16) ? C5 C6 C7 C16 . . . . 141.43(14) ? C12 C11 C10 C9 . . . . -178.21(14) ? C12 C11 C10 C15 . . . . -55.67(19) ? C15 C10 C9 C8 . . . . 15.0(3) ? C11 C10 C9 C8 . . . . 136.85(19) ? C10 C9 C8 C23 . . . . -178.83(18) ? C10 C9 C8 C7 . . . . 2.8(3) ? C16 C7 C8 C9 . . . . 13.0(2) ? C6 C7 C8 C9 . . . . -107.55(19) ? C16 C7 C8 C23 . . . . -165.42(16) ? C6 C7 C8 C23 . . . . 74.0(2) ? C10 C11 C12 C13 . . . . 53.2(2) ? C10 C11 C12 C24 . . . . 177.05(15) ? C2 C1 C17 O4 . . . . -64.7(2) ? C4 C1 C17 O4 . . . . 52.6(2) ? C6 C1 C17 O4 . . . . 170.10(16) ? C2 C1 C17 C16 . . . . 114.24(14) ? C4 C1 C17 C16 . . . . -128.50(15) ? C6 C1 C17 C16 . . . . -10.97(17) ? O4 C17 C16 C25 . . . . -32.7(2) ? C1 C17 C16 C25 . . . . 148.40(15) ? O4 C17 C16 C7 . . . . -155.09(17) ? C1 C17 C16 C7 . . . . 25.99(17) ? O4 C17 C16 C15 . . . . 91.00(19) ? C1 C17 C16 C15 . . . . -87.91(16) ? C8 C7 C16 C17 . . . . -155.95(13) ? C6 C7 C16 C17 . . . . -30.43(16) ? C8 C7 C16 C25 . . . . 82.75(18) ? C6 C7 C16 C25 . . . . -151.73(14) ? C8 C7 C16 C15 . . . . -44.48(18) ? C6 C7 C16 C15 . . . . 81.04(15) ? C9 C10 C15 C14 . . . . -177.05(15) ? C11 C10 C15 C14 . . . . 59.55(18) ? C9 C10 C15 C16 . . . . -47.75(19) ? C11 C10 C15 C16 . . . . -171.16(14) ? C17 C16 C15 C10 . . . . 173.98(14) ? C25 C16 C15 C10 . . . . -63.56(19) ? C7 C16 C15 C10 . . . . 63.52(16) ? C17 C16 C15 C14 . . . . -59.91(18) ? C25 C16 C15 C14 . . . . 62.55(19) ? C7 C16 C15 C14 . . . . -170.38(14) ? C10 C15 C14 C13 . . . . -61.75(18) ? C16 C15 C14 C13 . . . . 171.66(14) ? C15 C14 C13 C12 . . . . 59.44(19) ? C24 C12 C13 C14 . . . . -179.30(17) ? C11 C12 C13 C14 . . . . -54.9(2) ? N1 C3 C18 O5 . . . . 49.40(18) ? C4 C3 C18 O5 . . . . -66.47(19) ? N1 C3 C18 C19 . . . . -69.72(18) ? C4 C3 C18 C19 . . . . 174.41(14) ? O3 C5 C20 C21 . . . . -112.44(19) ? C6 C5 C20 C21 . . . . 126.31(19) ? C5 C20 C21 C22 . . . . -178.4(2) ? _shelx_res_file ; TITL LSLT99_0m_a.res in P6(5) LSLT99_0m.res created by SHELXL-2016/6 at 08:51:16 on 29-Sep-2019 CELL 1.54178 17.6760 17.6760 13.1360 90.000 90.000 120.000 ZERR 6.00 0.0004 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM x-y, x, z+5/6 SYMM y, -x+y, z+1/6 SYMM -y, x-y, z+2/3 SYMM -x+y, -x, z+1/3 SYMM -x, -y, z+1/2 SFAC C H N O UNIT 150 210 6 30 SIZE 0.096 0.153 0.095 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -116.590 SIZE 0.095 0.096 0.153 ACTA L.S. 15 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.033200 0.494500 FVAR 0.54819 C1 1 0.671431 0.504359 0.513264 11.00000 0.02378 0.02271 = 0.02357 -0.00022 0.00031 0.01247 H1 2 0.748383 0.379432 0.563020 11.00000 0.02514 O2 4 0.537390 0.404267 0.425951 11.00000 0.02663 0.02855 = 0.03266 -0.00558 -0.00499 0.01506 AFIX 148 H2 2 0.513596 0.362900 0.384459 11.00000 -1.50000 AFIX 0 C2 1 0.735085 0.482221 0.567161 11.00000 0.02279 0.02462 = 0.02246 0.00267 0.00403 0.01238 O3 4 0.672817 0.462850 0.345438 11.00000 0.03700 0.02408 = 0.02481 -0.00015 0.00290 0.01597 C3 1 0.643009 0.354925 0.471368 11.00000 0.02791 0.02324 = 0.02542 -0.00122 -0.00195 0.01375 AFIX 13 H3 2 0.659949 0.332825 0.410430 11.00000 -1.20000 AFIX 0 C4 1 0.624720 0.428475 0.437076 11.00000 0.02645 0.02419 = 0.02303 -0.00013 0.00039 0.01351 O4 4 0.557758 0.458677 0.641555 11.00000 0.02915 0.03035 = 0.03296 -0.00017 0.00671 0.01225 O5 4 0.550614 0.299309 0.625019 11.00000 0.03690 0.03601 = 0.03195 0.00500 0.00525 0.01803 AFIX 148 H5A 2 0.542897 0.341628 0.619010 11.00000 -1.50000 AFIX 0 C5 1 0.710500 0.557229 0.337975 11.00000 0.02602 0.02385 = 0.02699 0.00094 0.00246 0.01273 AFIX 13 H5 2 0.771586 0.582028 0.312127 11.00000 -1.20000 AFIX 0 N1 3 0.719700 0.403903 0.535353 11.00000 0.02426 0.02412 = 0.02894 -0.00006 -0.00096 0.01418 O1 4 0.791665 0.530150 0.628177 11.00000 0.02537 0.02665 = 0.02721 -0.00095 -0.00155 0.01321 C6 1 0.716328 0.589322 0.449663 11.00000 0.02549 0.02335 = 0.02635 0.00096 -0.00007 0.01388 AFIX 13 H6 2 0.779196 0.623923 0.469904 11.00000 -1.20000 AFIX 0 C7 1 0.669709 0.641960 0.479189 11.00000 0.03060 0.02761 = 0.02871 -0.00099 -0.00137 0.01849 AFIX 13 H7 2 0.619836 0.624783 0.431144 11.00000 -1.20000 AFIX 0 C11 1 0.821263 0.802507 0.731666 11.00000 0.03492 0.02917 = 0.03522 -0.00572 0.00115 0.01576 AFIX 23 H11A 2 0.868511 0.795712 0.700473 11.00000 -1.20000 H11B 2 0.840963 0.865681 0.733755 11.00000 -1.20000 AFIX 0 C10 1 0.739157 0.755849 0.664911 11.00000 0.03406 0.02709 = 0.03385 -0.00283 0.00131 0.01913 AFIX 13 H10 2 0.693079 0.766270 0.694656 11.00000 -1.20000 AFIX 0 C9 1 0.756481 0.789711 0.557404 11.00000 0.04225 0.02559 = 0.03848 0.00129 0.00118 0.01996 AFIX 43 H9 2 0.790498 0.851164 0.548335 11.00000 -1.20000 AFIX 0 C8 1 0.728005 0.740543 0.473859 11.00000 0.04112 0.02841 = 0.03505 0.00251 0.00154 0.02261 C12 1 0.805695 0.766994 0.840500 11.00000 0.03687 0.03565 = 0.03358 -0.00778 -0.00084 0.02053 AFIX 13 H12 2 0.762303 0.779963 0.873095 11.00000 -1.20000 AFIX 0 C17 1 0.611802 0.515987 0.588069 11.00000 0.02386 0.02829 = 0.02535 -0.00378 -0.00175 0.01327 C16 1 0.631504 0.609448 0.586701 11.00000 0.02797 0.02871 = 0.02962 -0.00152 0.00105 0.01781 C15 1 0.705675 0.657680 0.666249 11.00000 0.02926 0.02646 = 0.02748 -0.00264 0.00042 0.01646 AFIX 13 H15 2 0.755425 0.649881 0.643866 11.00000 -1.20000 AFIX 0 C14 1 0.683744 0.623128 0.775478 11.00000 0.03873 0.02921 = 0.03011 -0.00061 0.00240 0.01672 AFIX 23 H14A 2 0.639083 0.635247 0.804159 11.00000 -1.20000 H14B 2 0.659882 0.559143 0.776009 11.00000 -1.20000 AFIX 0 C13 1 0.766641 0.668018 0.839511 11.00000 0.04435 0.03567 = 0.02902 -0.00287 -0.00085 0.02301 AFIX 23 H13A 2 0.810111 0.653790 0.811727 11.00000 -1.20000 H13B 2 0.753011 0.645613 0.910133 11.00000 -1.20000 AFIX 0 C19 1 0.593191 0.206456 0.547383 11.00000 0.03890 0.02598 = 0.03640 0.00211 -0.00722 0.01381 AFIX 137 H19A 2 0.606178 0.188087 0.482441 11.00000 -1.50000 H19B 2 0.544181 0.156150 0.580527 11.00000 -1.50000 H19C 2 0.644707 0.229878 0.591562 11.00000 -1.50000 AFIX 0 C18 1 0.569124 0.276747 0.528153 11.00000 0.02926 0.02491 = 0.03006 0.00084 -0.00423 0.01139 AFIX 13 H18 2 0.514997 0.251455 0.485597 11.00000 -1.20000 AFIX 0 C20 1 0.661200 0.578601 0.261730 11.00000 0.02708 0.02580 = 0.02916 0.00060 0.00098 0.01218 AFIX 43 H20 2 0.602634 0.563311 0.276489 11.00000 -1.20000 AFIX 0 C21 1 0.695972 0.617882 0.174758 11.00000 0.02985 0.04739 = 0.03597 0.01043 0.00184 0.01460 AFIX 43 H21 2 0.754110 0.631140 0.161068 11.00000 -1.20000 AFIX 0 C22 1 0.651947 0.643423 0.095718 11.00000 0.04111 0.07425 = 0.04819 0.02889 0.00208 0.02052 AFIX 137 H22A 2 0.688571 0.705696 0.080067 11.00000 -1.50000 H22B 2 0.595245 0.632263 0.121498 11.00000 -1.50000 H22C 2 0.643188 0.609038 0.033820 11.00000 -1.50000 AFIX 0 C23 1 0.750243 0.780502 0.369309 11.00000 0.06380 0.03134 = 0.03617 0.00472 0.00158 0.02543 AFIX 137 H23A 2 0.783706 0.758692 0.332493 11.00000 -1.50000 H23B 2 0.785226 0.844215 0.375268 11.00000 -1.50000 H23C 2 0.696289 0.764637 0.332042 11.00000 -1.50000 AFIX 0 C24 1 0.889384 0.811083 0.903955 11.00000 0.04286 0.04963 = 0.03978 -0.01041 -0.00580 0.02367 AFIX 137 H24A 2 0.932813 0.798699 0.873969 11.00000 -1.50000 H24B 2 0.876479 0.788471 0.973717 11.00000 -1.50000 H24C 2 0.912503 0.874339 0.904851 11.00000 -1.50000 AFIX 0 C25 1 0.549956 0.615916 0.608550 11.00000 0.03282 0.03967 = 0.04009 -0.00478 0.00028 0.02469 AFIX 137 H25A 2 0.563289 0.676280 0.598386 11.00000 -1.50000 H25B 2 0.531362 0.598372 0.679070 11.00000 -1.50000 H25C 2 0.502952 0.577240 0.562198 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM LSLT99_0m_a.res in P6(5) REM R1 = 0.0285 for 4897 Fo > 4sig(Fo) and 0.0299 for all 5041 data REM 293 parameters refined using 1 restraints END WGHT 0.0332 0.4945 REM Instructions for potential hydrogen bonds EQIV $1 -x+y+1, -x+1, z+1/3 HTAB N1 O3_$1 EQIV $2 -y+1, x-y, z-1/3 HTAB O2 O1_$2 HTAB C3 O5_$2 HTAB O5 O4 HTAB C19 O3_$1 REM Highest difference peak 0.126, deepest hole -0.153, 1-sigma level 0.033 Q1 1 0.6462 0.4642 0.4872 11.00000 0.05 0.13 Q2 1 0.7123 0.7018 0.6707 11.00000 0.05 0.12 Q3 1 0.7007 0.6921 0.4765 11.00000 0.05 0.12 Q4 1 0.7839 0.7173 0.8379 11.00000 0.05 0.11 Q5 1 0.6986 0.4944 0.5507 11.00000 0.05 0.11 ; _shelx_res_checksum 66646 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ftxj20 _database_code_depnum_ccdc_archive 'CCDC 2070474' loop_ _audit_author_name _audit_author_address 'Tao Feng' ;South Central University for Nationalities China ; _audit_update_record ; 2021-03-15 deposited with the CCDC. 2021-05-19 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29 N O4' _chemical_formula_iupac ? _chemical_formula_weight 383.47 _chemical_absolute_configuration ad _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 6.8544(3) _cell_length_b 43.8920(19) _cell_length_c 6.7683(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2036.27(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9186 _cell_measurement_theta_min 6.0493 _cell_measurement_theta_max 79.0555 _cell_measurement_temperature 150.(2) _exptl_crystal_description BLOCK _exptl_crystal_colour 'light colourless' _exptl_crystal_size_max 0.258 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.101 _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ; _diffrn_ambient_temperature 150.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 22455 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_unetI/netI 0.0503 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 79.27 _diffrn_reflns_theta_full 79.27 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _refine_special_details ; ; _reflns_number_total 4309 _reflns_number_gt 4186 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_gt 0.1584 _refine_ls_wR_factor_ref 0.1593 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_number_reflns 4309 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.396 _refine_diff_density_min -0.372 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1619 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_publication_material ? loop_ _atom_site_type_symbol _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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.1725(3) 0.40211(5) 0.3853(4) 0.0345(5) Uani d . . . 1 . . C C1 0.8485(5) 0.47304(8) 0.2839(5) 0.0360(7) Uani d . . . 1 . . H H1A 0.803851 0.471813 0.146539 0.054 Uiso calc U . R 1 . . H H1B 0.991447 0.473198 0.287011 0.054 Uiso calc U . R 1 . . H H1C 0.79871 0.491783 0.344296 0.054 Uiso calc U . R 1 . . O O2 0.5373(3) 0.42415(5) 0.1776(3) 0.0278(5) Uani d . . . 1 . . H H2O 0.437(9) 0.4306(13) 0.113(9) 0.050(14) Uiso d . . . 1 . . C C2 0.7729(4) 0.44550(7) 0.3988(4) 0.0242(5) Uani d . . . 1 . . H H2 0.843551 0.42758 0.342169 0.029 Uiso calc U . R 1 . . O O3 0.4017(3) 0.48517(5) 0.2302(3) 0.0304(5) Uani d . . . 1 . . C C3 0.8284(4) 0.44607(7) 0.6158(4) 0.0254(5) Uani d . . . 1 . . H H3 0.908266 0.462013 0.665423 0.031 Uiso calc U . R 1 . . C C4 0.7651(4) 0.42422(7) 0.7371(4) 0.0250(5) Uani d . . . 1 . . H H4 0.804783 0.423 0.871342 0.03 Uiso calc U . R 1 . . O O4 0.3224(3) 0.44255(5) 0.8378(3) 0.0317(5) Uani d . . . 1 . . N N1 0.3525(4) 0.47075(6) 0.5537(4) 0.0259(5) Uani d . . . 1 . . H H1 0.293196 0.487287 0.596096 0.031 Uiso calc U . R 1 . . C C5 0.6268(4) 0.40172(6) 0.6460(4) 0.0222(5) Uani d . . . 1 . . H H5 0.701336 0.39003 0.544148 0.027 Uiso calc U . R 1 . . C C6 0.5073(4) 0.37843(6) 0.7672(4) 0.0247(6) Uani d . . . 1 . . H H6 0.449565 0.389504 0.882327 0.03 Uiso calc U . R 1 . . C C7 0.6243(4) 0.35195(7) 0.8478(4) 0.0282(6) Uani d . . . 1 . . C C8 0.6041(5) 0.32392(7) 0.7766(5) 0.0337(7) Uani d . . . 1 . . H H8 0.68458 0.30841 0.83086 0.04 Uiso calc U . R 1 . . C C9 0.4640(5) 0.31494(7) 0.6171(5) 0.0325(7) Uani d . . . 1 . . H H9 0.345702 0.30644 0.683661 0.039 Uiso calc U . R 1 . . C C10 0.5443(6) 0.28989(8) 0.4813(6) 0.0425(8) Uani d . . . 1 . . H H10A 0.660162 0.29775 0.41048 0.051 Uiso calc U . R 1 . . H H10B 0.586374 0.272353 0.56282 0.051 Uiso calc U . R 1 . . C C16 0.3060(4) 0.39744(6) 0.4962(4) 0.0253(5) Uani d . . . 1 . . C C15 0.3363(4) 0.36917(7) 0.6275(4) 0.0259(6) Uani d . . . 1 . . C C14 0.3964(5) 0.34201(7) 0.4919(5) 0.0281(6) Uani d . . . 1 . . H H14 0.510939 0.348873 0.41199 0.034 Uiso calc U . R 1 . . C C13 0.2388(5) 0.33179(8) 0.3467(6) 0.0369(7) Uani d . . . 1 . . H H13A 0.198754 0.349301 0.263912 0.044 Uiso calc U . R 1 . . H H13B 0.123 0.324696 0.421013 0.044 Uiso calc U . R 1 . . C C12 0.3129(6) 0.30604(8) 0.2137(6) 0.0410(8) Uani d . . . 1 . . H H12A 0.204392 0.298835 0.129172 0.049 Uiso calc U . R 1 . . H H12B 0.416395 0.314083 0.126075 0.049 Uiso calc U . R 1 . . C C11 0.3939(7) 0.27911(8) 0.3311(6) 0.0428(8) Uani d . . . 1 . . H H11 0.283019 0.269906 0.406229 0.051 Uiso calc U . R 1 . . C C19 0.4287(4) 0.46803(6) 0.3672(4) 0.0234(5) Uani d . . . 1 . . C C18 0.5504(4) 0.43889(6) 0.3615(4) 0.0218(5) Uani d . . . 1 . . C C17 0.4707(4) 0.42034(6) 0.5370(4) 0.0216(5) Uani d . . . 1 . . C C22 0.1504(5) 0.36303(8) 0.7459(6) 0.0347(7) Uani d . . . 1 . . H H22A 0.040039 0.360619 0.655105 0.052 Uiso calc U . R 1 . . H H22B 0.125268 0.380179 0.835015 0.052 Uiso calc U . R 1 . . H H22C 0.166634 0.34434 0.823403 0.052 Uiso calc U . R 1 . . C C23 0.3778(4) 0.44496(7) 0.6693(4) 0.0235(5) Uani d . . . 1 . . C C21 0.4760(9) 0.25447(11) 0.1950(8) 0.0604(12) Uani d . . . 1 . . H H21A 0.375134 0.248119 0.101014 0.091 Uiso calc U . R 1 . . H H21B 0.517007 0.236906 0.274146 0.091 Uiso calc U . R 1 . . H H21C 0.58837 0.262588 0.122671 0.091 Uiso calc U . R 1 . . C C20 0.7508(5) 0.35853(8) 1.0247(5) 0.0321(6) Uani d . . . 1 . . H H20A 0.828775 0.340473 1.056498 0.048 Uiso calc U . R 1 . . H H20B 0.668097 0.363761 1.137864 0.048 Uiso calc U . R 1 . . H H20C 0.837751 0.375645 0.99487 0.048 Uiso calc U . R 1 . . 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 O1 0.0289(11) 0.0338(11) 0.0408(12) 0.0021(8) -0.0110(10) 0.0006(9) C1 0.0291(15) 0.0399(16) 0.0390(16) -0.0030(12) 0.0002(13) 0.0139(14) O2 0.0341(11) 0.0308(10) 0.0185(9) 0.0073(8) -0.0014(8) -0.0027(8) C2 0.0199(12) 0.0285(13) 0.0243(12) 0.0034(10) 0.0014(10) 0.0033(10) O3 0.0314(10) 0.0279(10) 0.0318(10) 0.0068(8) -0.0026(9) 0.0061(8) C3 0.0205(12) 0.0297(13) 0.0261(13) 0.0033(10) -0.0025(10) -0.0019(10) C4 0.0223(12) 0.0298(13) 0.0230(12) 0.0057(10) -0.0019(10) -0.0004(10) O4 0.0322(11) 0.0408(12) 0.0222(9) 0.0111(9) 0.0025(9) -0.0020(8) N1 0.0269(12) 0.0240(11) 0.0267(11) 0.0064(9) -0.0005(9) -0.0036(9) C5 0.0202(12) 0.0263(12) 0.0200(11) 0.0048(9) 0.0012(9) 0.0023(9) C6 0.0249(13) 0.0268(13) 0.0225(12) 0.0044(10) 0.0046(10) 0.0023(10) C7 0.0275(14) 0.0331(15) 0.0239(13) 0.0052(11) 0.0061(11) 0.0079(11) C8 0.0374(16) 0.0320(15) 0.0316(15) 0.0088(12) 0.0063(13) 0.0094(12) C9 0.0387(16) 0.0249(14) 0.0340(15) 0.0020(12) 0.0063(13) 0.0040(11) C10 0.052(2) 0.0298(15) 0.0457(19) 0.0081(14) -0.0001(17) -0.0042(14) C16 0.0235(13) 0.0262(13) 0.0262(12) 0.0032(10) 0.0016(11) -0.0019(10) C15 0.0230(13) 0.0272(13) 0.0274(13) 0.0023(10) 0.0038(11) 0.0023(10) C14 0.0316(14) 0.0270(13) 0.0257(13) 0.0001(11) 0.0060(12) 0.0017(11) C13 0.0400(17) 0.0318(16) 0.0388(16) -0.0028(12) -0.0031(14) -0.0016(13) C12 0.050(2) 0.0346(17) 0.0382(17) -0.0068(14) 0.0015(16) -0.0058(13) C11 0.056(2) 0.0295(16) 0.0431(18) -0.0044(14) 0.0085(17) -0.0038(14) C19 0.0205(12) 0.0236(12) 0.0262(13) 0.0027(9) -0.0032(10) 0.0004(10) C18 0.0247(12) 0.0226(12) 0.0181(11) 0.0040(9) -0.0012(10) -0.0003(9) C17 0.0218(12) 0.0234(12) 0.0195(11) 0.0042(10) 0.0019(10) -0.0002(9) C22 0.0261(14) 0.0372(16) 0.0407(16) 0.0003(11) 0.0095(13) 0.0020(13) C23 0.0203(12) 0.0277(13) 0.0226(12) 0.0041(9) -0.0024(10) -0.0034(10) C21 0.078(3) 0.043(2) 0.060(3) 0.006(2) 0.004(3) -0.019(2) C20 0.0294(15) 0.0399(15) 0.0268(13) 0.0063(12) 0.0028(12) 0.0096(12) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C16 . 1.201(4) ? C1 C2 . 1.528(4) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? O2 C18 . 1.406(3) ? O2 H2O . 0.87(6) ? C2 C3 . 1.517(4) ? C2 C18 . 1.573(4) ? C2 H2 . 1.0 ? O3 C19 . 1.208(4) ? C3 C4 . 1.335(4) ? C3 H3 . 0.95 ? C4 C5 . 1.502(4) ? C4 H4 . 0.95 ? O4 C23 . 1.206(4) ? N1 C19 . 1.372(4) ? N1 C23 . 1.387(4) ? N1 H1 . 0.88 ? C5 C17 . 1.535(4) ? C5 C6 . 1.545(4) ? C5 H5 . 1.0 ? C6 C7 . 1.514(4) ? C6 C15 . 1.560(4) ? C6 H6 . 1.0 ? C7 C8 . 1.329(5) ? C7 C20 . 1.506(5) ? C8 C9 . 1.498(5) ? C8 H8 . 0.95 ? C9 C14 . 1.531(4) ? C9 C10 . 1.535(5) ? C9 H9 . 1.0 ? C10 C11 . 1.523(6) ? C10 H10A . 0.99 ? C10 H10B . 0.99 ? C16 C17 . 1.537(4) ? C16 C15 . 1.540(4) ? C15 C22 . 1.529(4) ? C15 C14 . 1.560(4) ? C14 C13 . 1.528(5) ? C14 H14 . 1.0 ? C13 C12 . 1.531(5) ? C13 H13A . 0.99 ? C13 H13B . 0.99 ? C12 C11 . 1.529(5) ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C11 C21 . 1.528(5) ? C11 H11 . 1.0 ? C19 C18 . 1.528(4) ? C18 C17 . 1.540(4) ? C17 C23 . 1.541(4) ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C21 H21A . 0.98 ? C21 H21B . 0.98 ? C21 H21C . 0.98 ? C20 H20A . 0.98 ? C20 H20B . 0.98 ? C20 H20C . 0.98 ? 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_3 _geom_angle _geom_angle_publ_flag C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C18 O2 H2O . . 110.(4) ? C3 C2 C1 . . 113.3(3) ? C3 C2 C18 . . 113.7(2) ? C1 C2 C18 . . 113.1(2) ? C3 C2 H2 . . 105.2 ? C1 C2 H2 . . 105.2 ? C18 C2 H2 . . 105.2 ? C4 C3 C2 . . 120.1(3) ? C4 C3 H3 . . 119.9 ? C2 C3 H3 . . 119.9 ? C3 C4 C5 . . 115.2(3) ? C3 C4 H4 . . 122.4 ? C5 C4 H4 . . 122.4 ? C19 N1 C23 . . 113.6(2) ? C19 N1 H1 . . 123.2 ? C23 N1 H1 . . 123.2 ? C4 C5 C17 . . 106.7(2) ? C4 C5 C6 . . 123.5(2) ? C17 C5 C6 . . 103.8(2) ? C4 C5 H5 . . 107.3 ? C17 C5 H5 . . 107.3 ? C6 C5 H5 . . 107.3 ? C7 C6 C5 . . 114.7(2) ? C7 C6 C15 . . 114.6(3) ? C5 C6 C15 . . 104.4(2) ? C7 C6 H6 . . 107.6 ? C5 C6 H6 . . 107.6 ? C15 C6 H6 . . 107.6 ? C8 C7 C20 . . 121.8(3) ? C8 C7 C6 . . 121.6(3) ? C20 C7 C6 . . 116.4(3) ? C7 C8 C9 . . 124.9(3) ? C7 C8 H8 . . 117.5 ? C9 C8 H8 . . 117.5 ? C8 C9 C14 . . 112.9(3) ? C8 C9 C10 . . 113.0(3) ? C14 C9 C10 . . 109.5(3) ? C8 C9 H9 . . 107.1 ? C14 C9 H9 . . 107.1 ? C10 C9 H9 . . 107.1 ? C11 C10 C9 . . 112.3(3) ? C11 C10 H10A . . 109.1 ? C9 C10 H10A . . 109.1 ? C11 C10 H10B . . 109.1 ? C9 C10 H10B . . 109.1 ? H10A C10 H10B . . 107.9 ? O1 C16 C17 . . 124.1(3) ? O1 C16 C15 . . 126.9(3) ? C17 C16 C15 . . 108.9(2) ? C22 C15 C16 . . 109.4(2) ? C22 C15 C14 . . 113.2(3) ? C16 C15 C14 . . 108.2(2) ? C22 C15 C6 . . 110.8(3) ? C16 C15 C6 . . 103.9(2) ? C14 C15 C6 . . 110.9(2) ? C13 C14 C9 . . 110.0(3) ? C13 C14 C15 . . 114.6(3) ? C9 C14 C15 . . 110.4(2) ? C13 C14 H14 . . 107.2 ? C9 C14 H14 . . 107.2 ? C15 C14 H14 . . 107.2 ? C14 C13 C12 . . 111.1(3) ? C14 C13 H13A . . 109.4 ? C12 C13 H13A . . 109.4 ? C14 C13 H13B . . 109.4 ? C12 C13 H13B . . 109.4 ? H13A C13 H13B . . 108.0 ? C11 C12 C13 . . 112.7(3) ? C11 C12 H12A . . 109.1 ? C13 C12 H12A . . 109.1 ? C11 C12 H12B . . 109.1 ? C13 C12 H12B . . 109.1 ? H12A C12 H12B . . 107.8 ? C10 C11 C21 . . 111.9(4) ? C10 C11 C12 . . 110.7(3) ? C21 C11 C12 . . 111.6(4) ? C10 C11 H11 . . 107.5 ? C21 C11 H11 . . 107.5 ? C12 C11 H11 . . 107.5 ? O3 C19 N1 . . 126.5(3) ? O3 C19 C18 . . 125.8(3) ? N1 C19 C18 . . 107.7(2) ? O2 C18 C19 . . 111.9(2) ? O2 C18 C17 . . 114.7(2) ? C19 C18 C17 . . 103.3(2) ? O2 C18 C2 . . 106.8(2) ? C19 C18 C2 . . 111.8(2) ? C17 C18 C2 . . 108.5(2) ? C5 C17 C16 . . 104.5(2) ? C5 C17 C18 . . 113.9(2) ? C16 C17 C18 . . 117.9(2) ? C5 C17 C23 . . 112.4(2) ? C16 C17 C23 . . 105.0(2) ? C18 C17 C23 . . 102.9(2) ? C15 C22 H22A . . 109.5 ? C15 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C15 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? O4 C23 N1 . . 124.4(3) ? O4 C23 C17 . . 128.1(3) ? N1 C23 C17 . . 107.2(2) ? C11 C21 H21A . . 109.5 ? C11 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C11 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? C7 C20 H20A . . 109.5 ? C7 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C7 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? 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 C1 C2 C3 C4 . . . . 176.9(3) ? C18 C2 C3 C4 . . . . 46.0(4) ? C2 C3 C4 C5 . . . . -4.8(4) ? C3 C4 C5 C17 . . . . -48.5(3) ? C3 C4 C5 C6 . . . . -168.3(3) ? C4 C5 C6 C7 . . . . -74.0(3) ? C17 C5 C6 C7 . . . . 164.9(2) ? C4 C5 C6 C15 . . . . 159.7(2) ? C17 C5 C6 C15 . . . . 38.6(3) ? C5 C6 C7 C8 . . . . -109.3(3) ? C15 C6 C7 C8 . . . . 11.5(4) ? C5 C6 C7 C20 . . . . 76.1(3) ? C15 C6 C7 C20 . . . . -163.1(2) ? C20 C7 C8 C9 . . . . 172.5(3) ? C6 C7 C8 C9 . . . . -1.8(5) ? C7 C8 C9 C14 . . . . 20.3(4) ? C7 C8 C9 C10 . . . . 145.2(3) ? C8 C9 C10 C11 . . . . 175.1(3) ? C14 C9 C10 C11 . . . . -58.2(4) ? O1 C16 C15 C22 . . . . -50.8(4) ? C17 C16 C15 C22 . . . . 126.1(3) ? O1 C16 C15 C14 . . . . 72.9(4) ? C17 C16 C15 C14 . . . . -110.2(3) ? O1 C16 C15 C6 . . . . -169.2(3) ? C17 C16 C15 C6 . . . . 7.8(3) ? C7 C6 C15 C22 . . . . 87.9(3) ? C5 C6 C15 C22 . . . . -145.7(2) ? C7 C6 C15 C16 . . . . -154.7(2) ? C5 C6 C15 C16 . . . . -28.3(3) ? C7 C6 C15 C14 . . . . -38.6(3) ? C5 C6 C15 C14 . . . . 87.8(3) ? C8 C9 C14 C13 . . . . -174.2(3) ? C10 C9 C14 C13 . . . . 59.0(4) ? C8 C9 C14 C15 . . . . -46.8(3) ? C10 C9 C14 C15 . . . . -173.6(3) ? C22 C15 C14 C13 . . . . 56.0(4) ? C16 C15 C14 C13 . . . . -65.4(3) ? C6 C15 C14 C13 . . . . -178.8(3) ? C22 C15 C14 C9 . . . . -68.8(3) ? C16 C15 C14 C9 . . . . 169.8(2) ? C6 C15 C14 C9 . . . . 56.4(3) ? C9 C14 C13 C12 . . . . -57.5(4) ? C15 C14 C13 C12 . . . . 177.5(3) ? C14 C13 C12 C11 . . . . 54.2(4) ? C9 C10 C11 C21 . . . . 179.3(3) ? C9 C10 C11 C12 . . . . 54.1(4) ? C13 C12 C11 C10 . . . . -51.8(4) ? C13 C12 C11 C21 . . . . -177.2(4) ? C23 N1 C19 O3 . . . . 168.5(3) ? C23 N1 C19 C18 . . . . -10.1(3) ? O3 C19 C18 O2 . . . . -34.3(4) ? N1 C19 C18 O2 . . . . 144.3(2) ? O3 C19 C18 C17 . . . . -158.2(3) ? N1 C19 C18 C17 . . . . 20.5(3) ? O3 C19 C18 C2 . . . . 85.4(3) ? N1 C19 C18 C2 . . . . -96.0(3) ? C3 C2 C18 O2 . . . . -150.7(2) ? C1 C2 C18 O2 . . . . 78.3(3) ? C3 C2 C18 C19 . . . . 86.6(3) ? C1 C2 C18 C19 . . . . -44.4(3) ? C3 C2 C18 C17 . . . . -26.6(3) ? C1 C2 C18 C17 . . . . -157.6(2) ? C4 C5 C17 C16 . . . . -165.1(2) ? C6 C5 C17 C16 . . . . -33.3(3) ? C4 C5 C17 C18 . . . . 64.9(3) ? C6 C5 C17 C18 . . . . -163.3(2) ? C4 C5 C17 C23 . . . . -51.7(3) ? C6 C5 C17 C23 . . . . 80.1(3) ? O1 C16 C17 C5 . . . . -167.2(3) ? C15 C16 C17 C5 . . . . 15.8(3) ? O1 C16 C17 C18 . . . . -39.5(4) ? C15 C16 C17 C18 . . . . 143.4(2) ? O1 C16 C17 C23 . . . . 74.3(4) ? C15 C16 C17 C23 . . . . -102.7(2) ? O2 C18 C17 C5 . . . . 93.9(3) ? C19 C18 C17 C5 . . . . -144.1(2) ? C2 C18 C17 C5 . . . . -25.4(3) ? O2 C18 C17 C16 . . . . -29.1(3) ? C19 C18 C17 C16 . . . . 92.9(3) ? C2 C18 C17 C16 . . . . -148.4(2) ? O2 C18 C17 C23 . . . . -144.1(2) ? C19 C18 C17 C23 . . . . -22.1(3) ? C2 C18 C17 C23 . . . . 96.6(2) ? C19 N1 C23 O4 . . . . 179.8(3) ? C19 N1 C23 C17 . . . . -4.9(3) ? C5 C17 C23 O4 . . . . -44.6(4) ? C16 C17 C23 O4 . . . . 68.5(4) ? C18 C17 C23 O4 . . . . -167.6(3) ? C5 C17 C23 N1 . . . . 140.4(2) ? C16 C17 C23 N1 . . . . -106.6(3) ? C18 C17 C23 N1 . . . . 17.3(3) ? _shelx_res_file ; TITL LSLT20_0ma_a.res in P2(1)2(1)2(1) LSLT20_0ma.res created by SHELXL-2016/6 at 15:22:53 on 07-Jan-2019 CELL 1.54178 6.8544 43.8920 6.7683 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0019 0.0003 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O UNIT 92 116 4 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! acta TEMP -123.110 SIZE 0.101 0.240 0.258 ACTA L.S. 10 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF omit 0 7 2 OMIT 2 38 0 OMIT -2 27 4 OMIT 0 41 2 OMIT -1 10 2 OMIT 1 41 0 OMIT 1 39 0 OMIT 1 1 0 WGHT 0.100000 0.593000 FVAR 0.64357 O1 4 0.172508 0.402108 0.385270 11.00000 0.02894 0.03378 = 0.04077 0.00064 -0.01098 0.00209 C1 1 0.848511 0.473044 0.283855 11.00000 0.02911 0.03994 = 0.03902 0.01387 0.00022 -0.00299 AFIX 137 H1A 2 0.803851 0.471813 0.146539 11.00000 -1.50000 H1B 2 0.991447 0.473198 0.287011 11.00000 -1.50000 H1C 2 0.798710 0.491783 0.344296 11.00000 -1.50000 AFIX 0 O2 4 0.537264 0.424153 0.177588 11.00000 0.03411 0.03083 = 0.01846 -0.00265 -0.00143 0.00728 H2O 2 0.436694 0.430644 0.112514 11.00000 0.05039 C2 1 0.772916 0.445499 0.398816 11.00000 0.01985 0.02851 = 0.02431 0.00328 0.00141 0.00336 AFIX 13 H2 2 0.843551 0.427580 0.342169 11.00000 -1.20000 AFIX 0 O3 4 0.401721 0.485170 0.230153 11.00000 0.03135 0.02791 = 0.03183 0.00608 -0.00263 0.00683 C3 1 0.828360 0.446070 0.615786 11.00000 0.02050 0.02972 = 0.02610 -0.00192 -0.00249 0.00332 AFIX 43 H3 2 0.908266 0.462013 0.665423 11.00000 -1.20000 AFIX 0 C4 1 0.765123 0.424223 0.737085 11.00000 0.02229 0.02978 = 0.02300 -0.00045 -0.00190 0.00569 AFIX 43 H4 2 0.804783 0.423000 0.871342 11.00000 -1.20000 AFIX 0 O4 4 0.322419 0.442549 0.837758 11.00000 0.03219 0.04080 = 0.02219 -0.00198 0.00250 0.01108 N1 3 0.352497 0.470747 0.553748 11.00000 0.02691 0.02398 = 0.02670 -0.00362 -0.00047 0.00640 AFIX 43 H1 2 0.293196 0.487287 0.596096 11.00000 -1.20000 AFIX 0 C5 1 0.626764 0.401716 0.646044 11.00000 0.02020 0.02633 = 0.02004 0.00228 0.00117 0.00485 AFIX 13 H5 2 0.701336 0.390030 0.544148 11.00000 -1.20000 AFIX 0 C6 1 0.507284 0.378431 0.767190 11.00000 0.02492 0.02679 = 0.02251 0.00234 0.00456 0.00439 AFIX 13 H6 2 0.449565 0.389504 0.882327 11.00000 -1.20000 AFIX 0 C7 1 0.624329 0.351950 0.847840 11.00000 0.02751 0.03308 = 0.02389 0.00793 0.00613 0.00516 C8 1 0.604121 0.323918 0.776567 11.00000 0.03743 0.03200 = 0.03161 0.00943 0.00625 0.00879 AFIX 43 H8 2 0.684580 0.308410 0.830860 11.00000 -1.20000 AFIX 0 C9 1 0.464019 0.314937 0.617064 11.00000 0.03869 0.02494 = 0.03398 0.00403 0.00629 0.00198 AFIX 13 H9 2 0.345702 0.306440 0.683661 11.00000 -1.20000 AFIX 0 C10 1 0.544253 0.289889 0.481315 11.00000 0.05205 0.02981 = 0.04573 -0.00422 -0.00007 0.00814 AFIX 23 H10A 2 0.660162 0.297750 0.410480 11.00000 -1.20000 H10B 2 0.586374 0.272353 0.562820 11.00000 -1.20000 AFIX 0 C16 1 0.305963 0.397444 0.496193 11.00000 0.02355 0.02618 = 0.02625 -0.00192 0.00158 0.00322 C15 1 0.336264 0.369171 0.627459 11.00000 0.02301 0.02722 = 0.02739 0.00228 0.00383 0.00232 C14 1 0.396391 0.342009 0.491932 11.00000 0.03161 0.02702 = 0.02574 0.00167 0.00599 0.00013 AFIX 13 H14 2 0.510939 0.348873 0.411990 11.00000 -1.20000 AFIX 0 C13 1 0.238812 0.331789 0.346694 11.00000 0.03996 0.03184 = 0.03880 -0.00164 -0.00312 -0.00279 AFIX 23 H13A 2 0.198754 0.349301 0.263912 11.00000 -1.20000 H13B 2 0.123000 0.324696 0.421013 11.00000 -1.20000 AFIX 0 C12 1 0.312860 0.306038 0.213708 11.00000 0.05024 0.03459 = 0.03820 -0.00578 0.00150 -0.00684 AFIX 23 H12A 2 0.204392 0.298835 0.129172 11.00000 -1.20000 H12B 2 0.416395 0.314083 0.126075 11.00000 -1.20000 AFIX 0 C11 1 0.393939 0.279112 0.331086 11.00000 0.05577 0.02952 = 0.04311 -0.00377 0.00846 -0.00437 AFIX 13 H11 2 0.283019 0.269906 0.406229 11.00000 -1.20000 AFIX 0 C19 1 0.428672 0.468031 0.367158 11.00000 0.02049 0.02361 = 0.02618 0.00045 -0.00325 0.00271 C18 1 0.550359 0.438887 0.361506 11.00000 0.02469 0.02260 = 0.01815 -0.00026 -0.00118 0.00399 C17 1 0.470710 0.420338 0.536987 11.00000 0.02177 0.02343 = 0.01949 -0.00021 0.00190 0.00422 C22 1 0.150356 0.363025 0.745880 11.00000 0.02610 0.03723 = 0.04066 0.00203 0.00949 0.00028 AFIX 137 H22A 2 0.040039 0.360619 0.655105 11.00000 -1.50000 H22B 2 0.125268 0.380179 0.835015 11.00000 -1.50000 H22C 2 0.166634 0.344340 0.823403 11.00000 -1.50000 AFIX 0 C23 1 0.377790 0.444961 0.669319 11.00000 0.02029 0.02766 = 0.02261 -0.00344 -0.00236 0.00413 C21 1 0.475963 0.254473 0.195037 11.00000 0.07824 0.04262 = 0.06045 -0.01885 0.00429 0.00620 AFIX 137 H21A 2 0.375134 0.248119 0.101014 11.00000 -1.50000 H21B 2 0.517007 0.236906 0.274146 11.00000 -1.50000 H21C 2 0.588370 0.262588 0.122671 11.00000 -1.50000 AFIX 0 C20 1 0.750778 0.358532 1.024710 11.00000 0.02940 0.03994 = 0.02683 0.00956 0.00281 0.00626 AFIX 137 H20A 2 0.828775 0.340473 1.056498 11.00000 -1.50000 H20B 2 0.668097 0.363761 1.137864 11.00000 -1.50000 H20C 2 0.837751 0.375645 0.994870 11.00000 -1.50000 REM ##### REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM LSLT20_0ma_a.res in P2(1)2(1)2(1) REM R1 = 0.0581 for 4186 Fo > 4sig(Fo) and 0.0596 for all 4309 data REM 261 parameters refined using 0 restraints END WGHT 0.0794 0.5657 REM Instructions for potential hydrogen bonds EQIV $1 x, y, z-1 HTAB O2 O4_$1 EQIV $2 x+1, y, z HTAB C2 O1_$2 EQIV $3 -x+1/2, -y+1, z+1/2 HTAB N1 O3_$3 REM Highest difference peak 0.396, deepest hole -0.372, 1-sigma level 0.086 Q1 1 0.6675 0.4459 0.3691 11.00000 0.05 0.40 Q2 1 0.6425 0.4221 0.6570 11.00000 0.05 0.35 Q3 1 0.5591 0.1939 0.0901 11.00000 0.05 0.28 Q4 1 0.4400 0.1014 0.8784 11.00000 0.05 0.28 Q5 1 0.6595 0.1830 0.2277 11.00000 0.05 0.27 ; _shelx_res_checksum 53167