data_6042 _audit_creation_date 2019-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelxl_version_number 2013-2 _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _audit_update_record ; ???? ; _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H30 O3' _chemical_formula_sum 'C24 H30 O3' _chemical_formula_weight 366.48 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _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, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.220(4) _cell_length_b 12.600(5) _cell_length_c 12.894(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1985.2(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1648 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 71.9 _cell_measurement_theta_min 27.1 _shelx_estimated_absorpt_T_max 0.865 _shelx_estimated_absorpt_T_min 0.682 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ? _exptl_crystal_colour 'Colorless' _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'Unknown' _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.666 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.24 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10399 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.354 _diffrn_reflns_theta_min 4.907 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'MicroMax 002+' _diffrn_measurement_method \f\k _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _reflns_Friedel_coverage 0.716 _reflns_Friedel_fraction_full 0.973 _reflns_Friedel_fraction_max 0.935 _reflns_number_gt 3305 _reflns_number_total 3785 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution ' SHELXL-2018/3 (Sheldrick, 2018)' _refine_diff_density_max 0.122 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.030 _refine_ls_abs_structure_details ; Flack x determined using 1209 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.09(13) _refine_ls_extinction_coef 0.0040(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 3785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0355 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0618P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.0987 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B) 2.c Aromatic/amide H refined with riding coordinates: C4(H4) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.27229(16) -0.60897(17) -0.00511(16) 0.0464(4) Uani 1 1 d . . . . . H1A H -0.3026 -0.6362 -0.0694 0.056 Uiso 1 1 calc R . . . . H1B H -0.2435 -0.5387 -0.0190 0.056 Uiso 1 1 calc R . . . . C2 C -0.17858(19) -0.6804(2) 0.0284(2) 0.0613(6) Uani 1 1 d . . . . . H2A H -0.2030 -0.7537 0.0268 0.074 Uiso 1 1 calc R . . . . H2B H -0.1190 -0.6733 -0.0208 0.074 Uiso 1 1 calc R . . . . C3 C -0.13743(18) -0.6555(2) 0.1339(2) 0.0637(6) Uani 1 1 d . . . . . C4 C -0.20994(17) -0.59691(17) 0.20217(17) 0.0501(5) Uani 1 1 d . . . . . H4 H -0.1824 -0.5750 0.2659 0.060 Uiso 1 1 calc R . . . . C5 C -0.31443(16) -0.57201(15) 0.17959(15) 0.0402(4) Uani 1 1 d . . . . . C6 C -0.37839(17) -0.51212(18) 0.25663(15) 0.0488(5) Uani 1 1 d . . . . . H6 H -0.3341 -0.4677 0.3028 0.059 Uiso 1 1 calc R . . . . C7 C -0.48861(17) -0.46517(19) 0.22926(16) 0.0508(5) Uani 1 1 d . . . . . H7 H -0.5037 -0.3949 0.2586 0.061 Uiso 1 1 calc R . . . . C8 C -0.53417(15) -0.48478(16) 0.12118(14) 0.0412(4) Uani 1 1 d . . . . . H8 H -0.5843 -0.5455 0.1231 0.049 Uiso 1 1 calc R . . . . C9 C -0.44146(15) -0.50722(14) 0.04256(14) 0.0378(4) Uani 1 1 d . . . . . H9 H -0.3957 -0.4434 0.0420 0.045 Uiso 1 1 calc R . . . . C10 C -0.36488(14) -0.59958(14) 0.07515(14) 0.0377(4) Uani 1 1 d . . . . . C11 C -0.48630(17) -0.51859(17) -0.06815(15) 0.0460(4) Uani 1 1 d . . . . . H11A H -0.4257 -0.5293 -0.1155 0.055 Uiso 1 1 calc R . . . . H11B H -0.5327 -0.5809 -0.0715 0.055 Uiso 1 1 calc R . . . . C12 C -0.55209(18) -0.42154(17) -0.10329(16) 0.0470(5) Uani 1 1 d . . . . . H12A H -0.5049 -0.3597 -0.1053 0.056 Uiso 1 1 calc R . . . . H12B H -0.5806 -0.4334 -0.1725 0.056 Uiso 1 1 calc R . . . . C13 C -0.64676(16) -0.40214(15) -0.02777(15) 0.0432(4) Uani 1 1 d . . . . . C14 C -0.59539(16) -0.38692(16) 0.08095(15) 0.0453(4) Uani 1 1 d . . . . . H14 H -0.5380 -0.3337 0.0703 0.054 Uiso 1 1 calc R . . . . C15 C -0.6814(2) -0.3299(2) 0.1454(2) 0.0639(6) Uani 1 1 d . . . . . H15 H -0.6567 -0.2906 0.2067 0.077 Uiso 1 1 calc R . . . . C16 C -0.7538(2) -0.2721(2) 0.06785(19) 0.0690(7) Uani 1 1 d . . . . . H16 H -0.7733 -0.1984 0.0836 0.083 Uiso 1 1 calc R . . . . C17 C -0.70919(17) -0.29502(18) -0.03811(17) 0.0510(5) Uani 1 1 d . . . . . C18 C -0.72661(18) -0.49667(18) -0.03994(19) 0.0564(5) Uani 1 1 d . . . . . H18A H -0.7165 -0.5453 0.0165 0.085 Uiso 1 1 calc GR . . . . H18B H -0.7123 -0.5324 -0.1043 0.085 Uiso 1 1 calc GR . . . . H18C H -0.8006 -0.4710 -0.0396 0.085 Uiso 1 1 calc GR . . . . C19 C -0.42570(17) -0.70625(16) 0.08108(17) 0.0489(5) Uani 1 1 d . . . . . H19A H -0.3771 -0.7599 0.1071 0.073 Uiso 1 1 calc GR . . . . H19B H -0.4506 -0.7259 0.0131 0.073 Uiso 1 1 calc GR . . . . H19C H -0.4874 -0.6996 0.1267 0.073 Uiso 1 1 calc GR . . . . C20 C -0.48314(19) -0.5538(2) 0.30555(17) 0.0632(6) Uani 1 1 d . . . . . H20A H -0.5092 -0.6229 0.2836 0.076 Uiso 1 1 calc R . . . . H20B H -0.4964 -0.5371 0.3779 0.076 Uiso 1 1 calc R . . . . C21 C -0.8001(2) -0.3576(3) 0.1380(2) 0.0802(9) Uani 1 1 d . . . . . H21A H -0.8476 -0.3354 0.1943 0.096 Uiso 1 1 calc R . . . . H21B H -0.8192 -0.4251 0.1067 0.096 Uiso 1 1 calc R . . . . C22 C -0.6402(2) -0.20149(17) -0.0778(2) 0.0610(6) Uani 1 1 d . . . . . H22A H -0.6653 -0.1351 -0.0481 0.073 Uiso 1 1 calc R . . . . H22B H -0.5636 -0.2112 -0.0607 0.073 Uiso 1 1 calc R . . . . C23 C -0.6575(2) -0.20298(19) -0.1938(2) 0.0616(6) Uani 1 1 d . . . . . H23A H -0.6594 -0.1315 -0.2218 0.074 Uiso 1 1 calc R . . . . H23B H -0.6000 -0.2427 -0.2283 0.074 Uiso 1 1 calc R . . . . C24 C -0.7655(2) -0.25642(18) -0.20618(19) 0.0584(6) Uani 1 1 d . . . . . O25 O -0.79656(12) -0.30211(14) -0.11629(12) 0.0580(4) Uani 1 1 d . . . . . O26 O -0.82220(17) -0.26134(18) -0.28198(15) 0.0834(6) Uani 1 1 d . . . . . O27 O -0.04701(17) -0.6844(3) 0.16198(19) 0.1155(10) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0443(10) 0.0558(10) 0.0391(10) -0.0035(8) 0.0000(8) 0.0072(9) C2 0.0515(11) 0.0762(15) 0.0563(14) -0.0082(11) -0.0020(10) 0.0205(11) C3 0.0480(11) 0.0795(15) 0.0636(15) -0.0017(13) -0.0097(11) 0.0167(11) C4 0.0483(10) 0.0582(11) 0.0439(11) -0.0036(9) -0.0127(9) 0.0011(9) C5 0.0441(9) 0.0424(9) 0.0341(10) 0.0012(7) -0.0033(7) -0.0041(8) C6 0.0482(10) 0.0640(11) 0.0342(10) -0.0052(9) -0.0052(8) 0.0012(9) C7 0.0509(11) 0.0684(13) 0.0329(11) -0.0082(9) -0.0015(8) 0.0099(10) C8 0.0412(8) 0.0510(9) 0.0314(9) -0.0021(8) -0.0005(7) 0.0049(8) C9 0.0408(8) 0.0406(8) 0.0319(9) -0.0004(7) 0.0006(7) 0.0020(7) C10 0.0391(8) 0.0412(8) 0.0329(9) -0.0010(7) -0.0019(7) -0.0018(7) C11 0.0525(10) 0.0545(10) 0.0308(9) -0.0026(8) -0.0011(8) 0.0123(9) C12 0.0545(11) 0.0521(10) 0.0343(10) -0.0005(8) -0.0030(8) 0.0099(9) C13 0.0442(9) 0.0481(9) 0.0375(10) -0.0015(8) -0.0051(8) 0.0066(8) C14 0.0478(10) 0.0509(10) 0.0371(10) -0.0065(8) -0.0013(8) 0.0079(9) C15 0.0667(13) 0.0797(15) 0.0452(13) -0.0120(11) -0.0012(10) 0.0289(13) C16 0.0686(14) 0.0830(16) 0.0554(14) -0.0080(13) 0.0002(12) 0.0327(13) C17 0.0488(10) 0.0567(11) 0.0474(12) -0.0021(9) -0.0094(9) 0.0135(9) C18 0.0548(11) 0.0591(11) 0.0553(13) 0.0031(10) -0.0118(10) -0.0026(10) C19 0.0541(11) 0.0442(10) 0.0483(11) 0.0010(9) -0.0095(9) -0.0057(8) C20 0.0573(12) 0.1003(18) 0.0322(11) 0.0075(11) 0.0044(9) 0.0047(12) C21 0.0629(14) 0.119(2) 0.0591(16) -0.0018(16) 0.0133(12) 0.0322(16) C22 0.0645(13) 0.0472(10) 0.0715(16) -0.0052(11) -0.0140(12) 0.0090(10) C23 0.0630(13) 0.0535(11) 0.0684(15) 0.0124(11) -0.0060(12) 0.0059(11) C24 0.0627(13) 0.0569(11) 0.0557(14) 0.0071(10) -0.0099(11) 0.0108(10) O25 0.0492(8) 0.0697(9) 0.0550(9) 0.0070(8) -0.0114(7) 0.0073(7) O26 0.0851(12) 0.0975(14) 0.0677(12) 0.0193(10) -0.0286(10) -0.0069(11) O27 0.0694(12) 0.187(3) 0.0901(15) -0.0321(17) -0.0302(11) 0.0626(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.519(3) . ? C1 C10 1.538(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.484(3) . ? C3 C4 1.451(3) . ? C3 O27 1.218(3) . ? C4 H4 0.9300 . ? C4 C5 1.347(3) . ? C5 C6 1.472(3) . ? C5 C10 1.521(2) . ? C6 H6 0.9800 . ? C6 C7 1.513(3) . ? C6 C20 1.520(3) . ? C7 H7 0.9800 . ? C7 C8 1.521(3) . ? C7 C20 1.489(4) . ? C8 H8 0.9800 . ? C8 C9 1.546(3) . ? C8 C14 1.533(3) . ? C9 H9 0.9800 . ? C9 C10 1.551(2) . ? C9 C11 1.536(3) . ? C10 C19 1.538(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.532(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.532(3) . ? C13 C14 1.548(3) . ? C13 C17 1.556(3) . ? C13 C18 1.548(3) . ? C14 H14 0.9800 . ? C14 C15 1.520(3) . ? C15 H15 0.9800 . ? C15 C16 1.521(3) . ? C15 C21 1.496(4) . ? C16 H16 0.9800 . ? C16 C17 1.499(3) . ? C16 C21 1.515(4) . ? C17 C22 1.536(3) . ? C17 O25 1.471(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.512(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.490(4) . ? C24 O25 1.349(3) . ? C24 O26 1.200(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1A C1 H1B 107.6 . . ? C2 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? C2 C1 C10 114.13(18) . . ? C10 C1 H1A 108.7 . . ? C10 C1 H1B 108.7 . . ? C1 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C3 C2 C1 112.98(19) . . ? C3 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C4 C3 C2 117.20(19) . . ? O27 C3 C2 121.1(2) . . ? O27 C3 C4 121.7(2) . . ? C3 C4 H4 117.8 . . ? C5 C4 C3 124.5(2) . . ? C5 C4 H4 117.8 . . ? C4 C5 C6 118.48(18) . . ? C4 C5 C10 121.50(18) . . ? C6 C5 C10 119.95(16) . . ? C5 C6 H6 114.2 . . ? C5 C6 C7 121.04(17) . . ? C5 C6 C20 123.4(2) . . ? C7 C6 H6 114.2 . . ? C7 C6 C20 58.81(15) . . ? C20 C6 H6 114.2 . . ? C6 C7 H7 115.5 . . ? C6 C7 C8 118.44(16) . . ? C8 C7 H7 115.5 . . ? C20 C7 C6 60.85(15) . . ? C20 C7 H7 115.5 . . ? C20 C7 C8 120.0(2) . . ? C7 C8 H8 109.4 . . ? C7 C8 C9 111.23(16) . . ? C7 C8 C14 110.99(16) . . ? C9 C8 H8 109.4 . . ? C14 C8 H8 109.4 . . ? C14 C8 C9 106.42(15) . . ? C8 C9 H9 105.9 . . ? C8 C9 C10 113.67(15) . . ? C10 C9 H9 105.9 . . ? C11 C9 C8 111.41(15) . . ? C11 C9 H9 105.9 . . ? C11 C9 C10 113.39(14) . . ? C1 C10 C9 108.62(15) . . ? C5 C10 C1 108.37(15) . . ? C5 C10 C9 108.24(14) . . ? C5 C10 C19 110.58(15) . . ? C19 C10 C1 108.77(15) . . ? C19 C10 C9 112.19(14) . . ? C9 C11 H11A 109.0 . . ? C9 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C12 C11 C9 112.81(16) . . ? C12 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C11 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C13 C12 C11 109.61(16) . . ? C13 C12 H12A 109.7 . . ? C13 C12 H12B 109.7 . . ? C12 C13 C14 106.81(16) . . ? C12 C13 C17 117.01(17) . . ? C12 C13 C18 106.79(17) . . ? C14 C13 C17 99.72(15) . . ? C18 C13 C14 116.29(17) . . ? C18 C13 C17 110.48(16) . . ? C8 C14 C13 113.88(16) . . ? C8 C14 H14 104.4 . . ? C13 C14 H14 104.4 . . ? C15 C14 C8 122.20(18) . . ? C15 C14 C13 105.86(17) . . ? C15 C14 H14 104.4 . . ? C14 C15 H15 117.9 . . ? C14 C15 C16 105.6(2) . . ? C16 C15 H15 117.9 . . ? C21 C15 C14 121.7(2) . . ? C21 C15 H15 117.9 . . ? C21 C15 C16 60.30(19) . . ? C15 C16 H16 117.3 . . ? C17 C16 C15 107.16(18) . . ? C17 C16 H16 117.3 . . ? C17 C16 C21 122.9(2) . . ? C21 C16 C15 59.04(18) . . ? C21 C16 H16 117.3 . . ? C16 C17 C13 105.50(18) . . ? C16 C17 C22 110.8(2) . . ? C22 C17 C13 115.15(17) . . ? O25 C17 C13 111.21(17) . . ? O25 C17 C16 111.84(18) . . ? O25 C17 C22 102.51(17) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C6 C20 H20A 117.7 . . ? C6 C20 H20B 117.7 . . ? C7 C20 C6 60.34(15) . . ? C7 C20 H20A 117.7 . . ? C7 C20 H20B 117.7 . . ? H20A C20 H20B 114.9 . . ? C15 C21 C16 60.67(19) . . ? C15 C21 H21A 117.7 . . ? C15 C21 H21B 117.7 . . ? C16 C21 H21A 117.7 . . ? C16 C21 H21B 117.7 . . ? H21A C21 H21B 114.8 . . ? C17 C22 H22A 110.9 . . ? C17 C22 H22B 110.9 . . ? H22A C22 H22B 109.0 . . ? C23 C22 C17 104.09(19) . . ? C23 C22 H22A 110.9 . . ? C23 C22 H22B 110.9 . . ? C22 C23 H23A 111.0 . . ? C22 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C24 C23 C22 103.6(2) . . ? C24 C23 H23A 111.0 . . ? C24 C23 H23B 111.0 . . ? O25 C24 C23 110.5(2) . . ? O26 C24 C23 128.5(2) . . ? O26 C24 O25 121.0(2) . . ? C24 O25 C17 111.00(17) . . ? _shelx_res_file ; TITL 6042 in P212121 #19 REM reset to P212121 #19 CELL 1.54178 12.2196 12.6 12.8935 90 90 90 ZERR 4 0.0038 0.0045 0.0043 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 96 120 12 L.S. 24 PLAN 5 SIZE 0.312 0.24 0.666 BOND HTAB BOND $H fmap 2 53 acta REM REM REM WGHT 0.061800 EXTI 0.003953 FVAR 0.77954 C1 1 -0.272294 -0.608974 -0.005107 11.00000 0.04428 0.05578 = 0.03907 -0.00347 0.00000 0.00723 AFIX 23 H1A 2 -0.302603 -0.636178 -0.069357 11.00000 -1.20000 H1B 2 -0.243530 -0.538654 -0.019047 11.00000 -1.20000 AFIX 0 C2 1 -0.178583 -0.680450 0.028377 11.00000 0.05153 0.07617 = 0.05635 -0.00822 -0.00203 0.02053 AFIX 23 H2A 2 -0.203048 -0.753668 0.026767 11.00000 -1.20000 H2B 2 -0.118974 -0.673335 -0.020816 11.00000 -1.20000 AFIX 0 C3 1 -0.137431 -0.655529 0.133866 11.00000 0.04801 0.07950 = 0.06363 -0.00172 -0.00969 0.01666 C4 1 -0.209941 -0.596914 0.202172 11.00000 0.04827 0.05823 = 0.04395 -0.00359 -0.01269 0.00109 AFIX 43 H4 2 -0.182357 -0.575049 0.265912 11.00000 -1.20000 AFIX 0 C5 1 -0.314432 -0.572013 0.179585 11.00000 0.04408 0.04237 = 0.03407 0.00120 -0.00330 -0.00408 C6 1 -0.378388 -0.512118 0.256630 11.00000 0.04822 0.06404 = 0.03415 -0.00521 -0.00521 0.00124 AFIX 13 H6 2 -0.334124 -0.467690 0.302806 11.00000 -1.20000 AFIX 0 C7 1 -0.488609 -0.465173 0.229260 11.00000 0.05089 0.06843 = 0.03294 -0.00821 -0.00150 0.00994 AFIX 13 H7 2 -0.503709 -0.394914 0.258553 11.00000 -1.20000 AFIX 0 C8 1 -0.534171 -0.484780 0.121183 11.00000 0.04118 0.05101 = 0.03143 -0.00208 -0.00045 0.00486 AFIX 13 H8 2 -0.584264 -0.545487 0.123143 11.00000 -1.20000 AFIX 0 C9 1 -0.441460 -0.507216 0.042559 11.00000 0.04076 0.04057 = 0.03194 -0.00037 0.00057 0.00200 AFIX 13 H9 2 -0.395656 -0.443374 0.041984 11.00000 -1.20000 AFIX 0 C10 1 -0.364881 -0.599581 0.075151 11.00000 0.03909 0.04121 = 0.03292 -0.00104 -0.00189 -0.00180 C11 1 -0.486297 -0.518587 -0.068148 11.00000 0.05253 0.05452 = 0.03082 -0.00263 -0.00107 0.01229 AFIX 23 H11A 2 -0.425653 -0.529333 -0.115542 11.00000 -1.20000 H11B 2 -0.532743 -0.580922 -0.071524 11.00000 -1.20000 AFIX 0 C12 1 -0.552088 -0.421537 -0.103292 11.00000 0.05454 0.05207 = 0.03433 -0.00054 -0.00296 0.00985 AFIX 23 H12A 2 -0.504919 -0.359654 -0.105343 11.00000 -1.20000 H12B 2 -0.580644 -0.433408 -0.172522 11.00000 -1.20000 AFIX 0 C13 1 -0.646762 -0.402143 -0.027770 11.00000 0.04416 0.04805 = 0.03746 -0.00148 -0.00513 0.00657 C14 1 -0.595385 -0.386918 0.080946 11.00000 0.04782 0.05089 = 0.03710 -0.00648 -0.00133 0.00786 AFIX 13 H14 2 -0.537956 -0.333736 0.070281 11.00000 -1.20000 AFIX 0 C15 1 -0.681350 -0.329853 0.145381 11.00000 0.06675 0.07968 = 0.04522 -0.01201 -0.00116 0.02894 AFIX 13 H15 2 -0.656714 -0.290567 0.206684 11.00000 -1.20000 AFIX 0 C16 1 -0.753836 -0.272122 0.067855 11.00000 0.06864 0.08296 = 0.05538 -0.00797 0.00019 0.03268 AFIX 13 H16 2 -0.773344 -0.198411 0.083557 11.00000 -1.20000 AFIX 0 C17 1 -0.709187 -0.295021 -0.038109 11.00000 0.04876 0.05672 = 0.04743 -0.00214 -0.00941 0.01348 C18 1 -0.726606 -0.496674 -0.039938 11.00000 0.05484 0.05907 = 0.05532 0.00311 -0.01183 -0.00258 AFIX 137 H18A 2 -0.716479 -0.545331 0.016547 11.00000 -1.50000 H18B 2 -0.712306 -0.532358 -0.104312 11.00000 -1.50000 H18C 2 -0.800562 -0.470968 -0.039596 11.00000 -1.50000 AFIX 0 C19 1 -0.425699 -0.706253 0.081077 11.00000 0.05410 0.04415 = 0.04834 0.00097 -0.00953 -0.00573 AFIX 137 H19A 2 -0.377101 -0.759854 0.107129 11.00000 -1.50000 H19B 2 -0.450552 -0.725936 0.013114 11.00000 -1.50000 H19C 2 -0.487411 -0.699565 0.126687 11.00000 -1.50000 AFIX 0 C20 1 -0.483138 -0.553760 0.305549 11.00000 0.05726 0.10026 = 0.03220 0.00746 0.00443 0.00473 AFIX 23 H20A 2 -0.509225 -0.622901 0.283568 11.00000 -1.20000 H20B 2 -0.496446 -0.537089 0.377905 11.00000 -1.20000 AFIX 0 C21 1 -0.800127 -0.357551 0.137969 11.00000 0.06286 0.11859 = 0.05913 -0.00181 0.01327 0.03219 AFIX 23 H21A 2 -0.847568 -0.335374 0.194259 11.00000 -1.20000 H21B 2 -0.819246 -0.425066 0.106690 11.00000 -1.20000 AFIX 0 C22 1 -0.640232 -0.201493 -0.077765 11.00000 0.06446 0.04716 = 0.07148 -0.00521 -0.01403 0.00897 AFIX 23 H22A 2 -0.665302 -0.135066 -0.048078 11.00000 -1.20000 H22B 2 -0.563567 -0.211230 -0.060734 11.00000 -1.20000 AFIX 0 C23 1 -0.657492 -0.202979 -0.193849 11.00000 0.06299 0.05350 = 0.06837 0.01242 -0.00596 0.00595 AFIX 23 H23A 2 -0.659373 -0.131510 -0.221755 11.00000 -1.20000 H23B 2 -0.600027 -0.242681 -0.228322 11.00000 -1.20000 AFIX 0 C24 1 -0.765454 -0.256421 -0.206180 11.00000 0.06267 0.05687 = 0.05573 0.00713 -0.00990 0.01081 O25 3 -0.796562 -0.302107 -0.116292 11.00000 0.04920 0.06974 = 0.05503 0.00701 -0.01140 0.00728 O26 3 -0.822205 -0.261344 -0.281980 11.00000 0.08514 0.09748 = 0.06768 0.01930 -0.02865 -0.00693 O27 3 -0.047014 -0.684411 0.161977 11.00000 0.06938 0.18705 = 0.09009 -0.03211 -0.03017 0.06261 HKLF 4 REM 6042 in P212121 #19 REM R1 = 0.0355 for 3305 Fo > 4sig(Fo) and 0.0398 for all 3785 data REM 247 parameters refined using 0 restraints END WGHT 0.0618 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x-1/2, -y-1, z-1/2 HTAB C23 O27_$1 REM Highest difference peak 0.122, deepest hole -0.134, 1-sigma level 0.030 Q1 1 -0.0371 -0.6147 0.1402 11.00000 0.05 0.12 Q2 1 -0.7263 -0.3816 0.1630 11.00000 0.05 0.12 Q3 1 -0.3230 -0.5999 0.0366 11.00000 0.05 0.11 Q4 1 -0.3831 -0.6451 0.0631 11.00000 0.05 0.11 Q5 1 -0.5188 -0.4795 0.1805 11.00000 0.05 0.11 ; _shelx_res_checksum 58387 _shelx_hkl_file ; 0 0 -1 0.07 0.16 0 0 1 0.68 0.18 0 0 2 837.23 15.27 0 0 4 42.40 2.62 0 0 5 1.25 0.78 0 0 6 646.74 16.42 0 0 7 2.67 3.00 0 0 8 162.60 9.69 0 0 -8 145.91 6.64 0 0 9 0.04 0.91 0 0 -9 0.50 0.44 0 0 -9 0.07 0.50 0 0 10 16.83 3.38 0 0 -10 19.58 2.59 0 0 -10 14.36 1.86 0 0 11 0.12 1.24 0 0 -11 3.83 2.28 0 0 -11 -0.01 0.82 0 0 -12 58.85 4.89 0 0 -14 5.64 5.61 0 0 -15 0.10 0.48 0 -1 0 0.50 0.44 0 -1 0 0.04 0.04 0 -1 -1 1169.60 20.52 0 -1 1 1211.80 19.65 0 -1 1 1192.01 20.10 0 -1 -2 2490.07 138.92 0 -1 2 2067.96 34.87 0 1 2 2366.06 131.69 0 -1 -3 317.49 8.68 0 -1 3 319.84 7.66 0 1 3 338.37 8.30 0 -1 -4 587.40 14.43 0 -1 4 669.75 14.56 0 1 4 666.41 14.77 0 -1 5 784.94 17.51 0 1 5 858.20 19.28 0 -1 6 51.32 3.86 0 1 6 84.25 4.88 0 -1 7 142.28 7.26 0 1 7 145.14 7.17 0 -1 8 4.71 1.54 0 1 8 0.41 1.57 0 1 -8 0.53 0.52 0 -1 -8 0.35 0.49 0 -1 -8 0.29 0.38 0 1 9 2.34 1.38 0 -1 9 3.45 1.94 0 1 -9 3.16 2.08 0 -1 -9 6.22 3.66 0 1 -9 1.25 0.78 0 -1 -9 2.16 1.25 0 -1 10 9.16 6.23 0 1 10 7.97 6.49 0 1 -10 12.67 2.73 0 -1 -10 11.66 4.59 0 1 -10 6.95 4.38 0 -1 -10 10.29 5.08 0 -1 11 26.45 4.33 0 1 11 28.83 4.54 0 1 -11 30.85 6.68 0 -1 -11 34.47 5.24 0 -1 -11 24.02 8.14 0 -1 -12 80.47 5.72 0 -1 -12 67.45 6.31 0 1 -13 41.13 3.89 0 -1 -13 50.13 4.47 0 -1 -14 1.02 1.19 0 1 -14 0.89 1.05 0 -1 -15 0.36 0.82 0 -2 0 283.05 6.32 0 -2 0 277.34 5.92 0 -2 -1 1572.92 28.05 0 -2 1 1498.38 25.23 0 -2 1 1501.77 25.60 0 -2 -2 55.52 2.86 0 -2 2 59.94 1.69 0 -2 -3 81.97 4.33 0 -2 3 71.99 1.99 0 -2 3 72.47 3.15 0 2 3 83.98 3.71 0 -2 -4 501.63 13.69 0 -2 4 544.86 12.74 0 2 4 551.06 13.17 0 -2 -5 9.41 6.99 0 -2 5 10.09 1.58 0 2 5 9.84 1.69 0 -2 6 50.43 4.66 0 2 6 54.86 5.02 0 -2 7 210.14 9.03 0 2 7 214.54 9.14 0 -2 8 30.68 3.71 0 2 8 29.86 3.72 0 2 -8 31.14 2.76 0 -2 -8 29.88 2.23 0 -2 -8 28.52 2.20 0 -2 9 0.45 1.48 0 2 9 0.92 1.03 0 2 -9 3.63 2.15 0 -2 -9 2.02 1.21 0 -2 -9 1.13 0.94 0 -2 10 33.08 4.73 0 2 10 31.09 4.48 0 -2 -10 34.81 3.53 0 -2 -10 33.41 3.09 0 -2 11 181.55 13.58 0 2 11 165.39 12.73 0 -2 -11 181.31 11.21 0 -2 -11 164.64 9.98 0 2 -12 1.50 1.49 0 -2 -12 1.38 1.05 0 -2 -12 0.73 0.91 0 -2 -13 27.36 3.58 0 -2 -13 21.66 2.30 0 -2 -14 90.35 5.59 0 -2 -15 16.69 2.43 0 -3 0 0.16 0.17 0 -3 -1 297.41 8.43 0 -3 1 281.11 7.13 0 -3 -2 5190.74 289.26 0 -3 2 4758.33 263.98 0 -3 2 5339.17 296.52 0 -3 -3 19.27 2.11 0 -3 3 22.81 1.13 0 -3 3 22.00 1.88 0 -3 -4 26.58 2.95 0 -3 4 29.28 1.20 0 -3 4 31.42 2.54 0 3 4 31.61 2.60 0 -3 -5 29.22 3.36 0 -3 5 33.84 2.82 0 3 5 36.48 3.20 0 -3 6 145.82 6.70 0 3 6 160.66 7.48 0 -3 7 22.75 3.25 0 3 7 19.96 3.10 0 -3 -7 21.31 2.00 0 -3 8 2.82 2.44 0 3 8 3.47 1.88 0 -3 -8 6.61 3.44 0 -3 9 126.24 9.07 0 3 9 123.39 9.05 0 -3 -9 128.57 6.64 0 -3 -9 124.24 6.55 0 -3 10 287.28 18.36 0 3 10 278.85 17.76 0 -3 -10 331.81 17.56 0 -3 -10 300.17 16.13 0 -3 11 33.98 5.11 0 3 11 32.77 4.96 0 -3 -11 34.57 3.66 0 -3 -11 33.54 3.38 0 -3 -12 88.13 6.09 0 -3 -12 68.41 4.58 0 -3 -13 0.44 0.68 0 -3 -13 0.18 0.53 0 -3 -14 10.24 2.11 0 -3 -14 11.38 2.00 0 -3 -15 82.60 4.22 0 -4 0 2073.49 37.37 0 -4 -1 254.89 8.57 0 -4 1 216.09 6.15 0 -4 1 214.68 6.16 0 -4 -2 315.84 10.31 0 -4 2 305.55 7.28 0 -4 2 275.48 7.44 0 -4 -3 297.84 10.38 0 -4 3 331.69 7.35 0 -4 3 324.33 8.90 0 -4 -4 766.47 20.75 0 -4 4 769.15 17.44 0 4 4 757.42 17.72 0 -4 -5 12.85 2.63 0 -4 5 16.84 2.39 0 4 5 15.96 2.42 0 -4 6 726.47 18.54 0 4 6 694.37 18.27 0 -4 7 199.52 10.88 0 4 7 188.37 10.67 0 -4 -7 181.39 7.49 0 -4 8 71.11 6.39 0 4 8 64.25 5.89 0 -4 -8 74.40 4.71 0 -4 9 259.69 17.91 0 4 9 243.00 17.01 0 -4 -9 268.60 16.17 0 -4 -9 258.54 15.64 0 -4 10 52.36 5.95 0 4 10 52.36 5.86 0 -4 -10 69.83 5.24 0 -4 -10 58.74 4.51 0 4 11 0.85 1.60 0 -4 -11 2.25 1.20 0 -4 -11 2.13 1.53 0 -4 -12 97.65 8.00 0 -4 -12 90.87 7.33 0 -4 -13 4.26 1.84 0 -4 -13 2.54 2.26 0 -4 -14 31.52 3.73 0 -4 -14 32.87 3.64 0 -4 -15 0.98 3.88 0 -5 0 0.26 0.49 0 -5 1 43.28 4.03 0 -5 -1 30.35 3.17 0 -5 1 28.98 2.32 0 -5 -2 190.19 8.49 0 -5 2 161.90 5.30 0 -5 2 166.04 5.86 0 -5 -3 2.09 1.83 0 -5 3 1.21 1.63 0 -5 3 1.89 1.51 0 -5 -4 20.91 3.60 0 -5 4 20.14 2.74 0 -5 -5 33.65 4.78 0 -5 5 30.62 3.34 0 5 5 35.67 3.94 0 -5 6 8.37 6.73 0 5 6 7.98 1.85 0 -5 -6 7.79 3.26 0 -5 7 5.60 4.52 0 5 7 5.18 1.58 0 -5 7 3.97 1.79 0 -5 -7 5.58 0.91 0 -5 8 37.34 4.45 0 5 8 38.58 4.59 0 -5 -8 37.52 2.80 0 -5 9 81.78 7.53 0 5 9 72.75 6.91 0 -5 -9 89.02 5.82 0 -5 10 50.09 6.00 0 5 10 51.74 6.30 0 -5 -10 55.47 5.96 0 -5 -10 55.92 4.96 0 -5 -11 2.01 1.12 0 -5 -11 1.46 1.76 0 -5 -12 14.98 2.10 0 -5 -12 13.74 1.88 0 -5 -13 17.70 2.41 0 -5 -13 13.71 1.78 0 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447.85 20.51 5 -4 -6 381.31 17.72 -5 4 -6 450.77 19.55 -5 -4 -6 447.63 19.14 5 -4 -6 420.48 19.78 5 -4 -7 201.73 15.29 5 -4 7 209.50 13.94 5 -4 7 216.69 15.06 -5 4 7 226.52 16.57 -5 -4 7 231.11 14.56 -5 -4 -7 226.57 15.22 -5 -4 -7 219.96 13.10 5 -4 -7 210.35 12.39 -5 4 -7 244.74 15.48 -5 -4 -7 234.59 14.56 5 -4 -8 166.68 13.38 5 -4 8 169.97 11.91 -5 4 8 166.20 12.71 -5 -4 8 194.24 11.52 -5 -4 -8 226.94 14.80 -5 -4 -8 175.36 9.93 5 -4 -8 181.26 10.00 -5 4 -8 201.97 12.12 -5 -4 -8 197.80 11.70 5 -4 9 110.96 9.10 -5 4 9 110.64 10.19 -5 -4 9 115.60 7.17 -5 4 9 113.96 6.86 -5 -4 -9 165.50 12.44 -5 -4 -9 148.33 9.28 5 -4 -9 110.84 6.76 -5 4 -9 134.20 9.00 -5 -4 -9 125.19 8.32 -5 -4 10 47.15 3.11 -5 -4 -10 63.70 6.52 -5 -4 -10 54.54 4.27 5 -4 -10 48.83 3.34 -5 4 -10 53.69 4.39 -5 -4 -10 49.20 4.26 -5 -4 11 61.88 3.65 -5 -4 -11 71.12 6.53 -5 -4 -11 69.17 4.70 5 -4 -11 58.34 3.72 -5 4 -11 70.31 8.01 -5 -4 -11 70.57 5.48 -5 -4 -12 25.52 3.97 -5 -4 -12 23.24 3.21 -5 -4 -13 7.15 1.84 -5 -4 -13 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244.43 15.58 -8 4 -3 249.23 15.52 -8 -4 -3 269.18 17.13 8 -4 -3 254.71 14.96 8 -4 3 259.28 15.16 -8 4 3 258.22 17.11 8 -4 -4 8.80 5.16 8 -4 4 6.77 5.59 -8 -4 4 9.69 1.58 -8 4 4 9.70 2.57 -8 4 -4 7.83 1.67 -8 -4 -4 10.20 5.50 8 -4 -4 9.31 3.94 -8 4 4 8.14 4.28 8 -4 -5 84.90 7.78 8 -4 5 88.30 7.54 -8 4 5 90.59 8.32 -8 -4 5 97.93 6.23 -8 4 5 104.35 6.76 -8 4 -5 100.93 7.09 -8 -4 -5 110.77 8.23 8 -4 -5 101.41 6.03 -8 4 5 103.23 6.95 8 -4 -6 61.34 6.78 8 -4 6 57.15 5.78 -8 4 6 52.90 6.03 -8 -4 6 71.95 5.27 -8 4 6 70.01 5.28 -8 4 -6 64.33 5.26 -8 -4 -6 68.52 7.33 -8 -4 -6 63.69 4.66 -8 4 6 71.92 5.51 8 -4 7 70.41 6.24 -8 4 7 75.66 7.31 -8 -4 7 98.49 6.32 -8 4 -7 87.64 6.05 -8 -4 -7 93.24 7.31 -8 -4 -7 94.84 5.97 -8 4 7 89.42 5.57 -8 -4 8 0.84 0.83 -8 4 8 0.38 0.94 -8 4 -8 0.35 0.86 -8 -4 -8 -0.29 1.28 -8 -4 -8 0.31 0.85 -8 -4 9 18.18 2.03 -8 4 9 18.11 1.99 -8 -4 -9 22.84 13.32 -8 -4 -9 18.96 2.46 -8 -4 10 6.78 4.03 -8 4 10 4.99 2.13 -8 -4 -10 6.35 3.92 -8 -4 -10 5.70 3.97 -8 -4 11 11.86 1.57 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183.47 10.49 -8 5 5 179.43 10.91 8 -5 -6 12.08 16.00 8 -5 6 22.64 3.70 -8 5 6 22.61 4.02 -8 -5 6 29.54 3.08 -8 5 6 25.87 2.80 -8 -5 -6 27.52 3.91 8 -5 -6 29.90 2.83 -8 5 6 27.65 3.06 -8 -5 7 53.54 3.85 -8 -5 -7 47.85 4.94 -8 -5 -7 44.08 3.42 -8 -5 8 6.68 4.90 -8 5 8 7.05 1.25 -8 -5 -8 9.42 8.14 -8 -5 -8 6.56 5.13 -8 -5 9 8.66 3.86 -8 5 9 6.81 4.54 -8 -5 -9 10.62 6.24 -8 -5 -9 7.85 4.01 -8 -5 10 21.20 2.11 -8 5 10 15.77 1.56 -8 -5 -10 22.32 3.27 -8 -5 -10 18.04 3.34 -8 -5 11 13.13 1.46 -8 -5 -11 15.48 2.73 -8 -5 -11 13.28 1.94 -8 -5 -12 8.08 1.48 -8 -5 -12 7.91 1.14 8 -6 0 6.36 4.59 -8 6 0 5.76 3.09 8 -6 0 7.64 2.58 8 -6 1 165.62 12.44 8 -6 -1 159.02 12.39 -8 -6 1 155.22 8.34 -8 6 1 152.87 8.92 -8 6 -1 168.91 9.80 8 -6 -1 162.70 8.96 8 -6 1 160.41 8.99 8 -6 -2 135.66 10.83 8 -6 2 126.17 10.12 -8 -6 2 133.99 7.56 -8 6 2 149.94 8.82 8 -6 -2 146.25 8.25 8 -6 2 136.59 7.82 8 -6 -3 388.46 24.66 8 -6 3 357.04 22.29 -8 -6 3 407.89 25.54 -8 6 3 382.21 20.79 -8 -6 -3 364.07 20.86 8 -6 -3 413.49 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8.29 3.95 -10 -7 2 2.90 2.23 -10 7 2 2.75 2.12 10 -7 -2 3.37 1.87 10 -7 2 3.02 1.36 -10 7 2 3.90 2.66 -10 -7 3 19.47 3.11 -10 7 3 21.53 2.14 10 -7 -3 20.64 2.01 10 -7 3 19.69 1.82 -10 7 3 20.63 2.52 -10 -7 4 2.24 1.33 10 -7 -4 1.98 1.69 10 -7 4 2.51 1.43 -10 7 4 2.06 1.18 -10 -7 5 28.51 2.94 10 -7 5 27.17 2.83 -10 7 5 25.26 2.83 -10 -7 6 2.00 1.27 10 -7 6 1.80 1.34 -10 -7 7 5.85 3.70 -10 7 7 4.66 1.01 10 -7 7 4.32 0.70 -10 -7 8 8.20 1.23 -10 7 8 7.75 1.21 -10 7 -8 6.81 1.11 -10 -7 9 8.38 0.92 -10 7 9 5.11 0.66 10 -8 0 3.95 2.38 -10 8 0 4.28 2.96 10 -8 1 32.95 3.24 10 -8 -1 31.54 3.22 -10 8 1 32.77 3.75 10 -8 -2 11.48 1.54 10 -8 2 12.38 1.64 -10 8 2 12.84 4.50 -10 -8 3 1.01 0.87 10 -8 -3 1.26 1.07 10 -8 3 0.53 0.28 -10 8 3 0.54 0.80 -10 -8 4 10.90 1.56 10 -8 -4 9.96 1.29 10 -8 4 9.98 1.87 -10 8 4 10.03 1.80 -10 -8 5 4.30 2.31 10 -8 5 3.82 2.00 -10 -8 6 3.07 2.15 10 -8 6 2.27 0.85 -10 -8 7 34.69 4.31 -10 8 7 31.53 3.25 10 -8 7 27.67 2.79 -10 -8 8 0.63 1.07 -10 8 8 0.36 1.09 10 -9 0 3.05 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0.08 0.54 -13 -1 -8 0.15 0.30 -13 -2 0 4.71 3.40 -13 2 0 6.00 4.29 -13 2 0 4.95 3.98 -13 2 -1 25.12 2.72 -13 -2 1 25.75 2.74 -13 2 1 26.43 2.87 -13 -2 -1 26.49 3.31 -13 2 1 24.41 2.73 -13 2 -1 25.11 2.75 -13 2 2 3.11 0.76 -13 -2 2 3.52 2.17 -13 2 2 3.90 2.52 -13 -2 -2 3.76 2.09 -13 2 -2 3.62 2.54 -13 2 2 3.77 2.65 -13 2 -2 3.49 2.66 -13 -2 3 16.27 1.84 -13 2 3 14.93 1.91 -13 -2 3 14.10 1.85 -13 2 3 14.60 2.04 -13 -2 -3 14.39 2.36 -13 2 -3 14.43 4.45 -13 2 3 14.37 2.22 -13 -2 4 9.94 1.39 -13 2 4 8.31 1.28 -13 2 4 9.55 1.58 -13 -2 4 8.07 1.28 -13 -2 -4 9.12 5.72 -13 2 -4 7.97 4.79 -13 2 4 10.43 6.92 -13 -2 5 7.59 1.20 -13 2 5 6.93 1.15 -13 2 5 6.69 2.35 -13 -2 -5 6.90 5.56 -13 2 -5 7.41 1.46 -13 -2 6 6.89 1.09 -13 2 6 7.05 1.10 -13 -2 -6 6.02 1.26 -13 2 -6 7.38 3.67 -13 -2 7 1.07 0.72 -13 2 7 0.47 1.07 -13 -2 -7 0.80 1.41 -13 2 -7 0.52 1.30 -13 -3 0 4.08 3.70 -13 3 0 6.50 3.81 -13 3 0 4.37 2.88 -13 3 1 4.12 0.76 -13 3 -1 6.44 2.91 -13 -3 1 5.50 3.78 -13 3 1 5.69 4.11 -13 -3 -1 6.00 3.79 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4 -3 6.08 1.10 -13 -4 -3 5.78 2.89 -13 4 3 8.39 4.90 -13 4 -3 6.99 5.01 -13 -4 4 9.62 1.14 -13 4 4 10.30 1.47 -13 4 4 10.67 1.56 -13 4 -4 10.04 1.48 -13 -4 -4 8.99 1.43 -13 4 4 10.91 1.65 -13 4 -4 11.83 1.69 -13 -4 5 1.57 1.95 -13 4 5 3.56 0.77 -13 4 -5 1.44 2.19 -13 -4 -5 1.91 2.13 -13 4 5 1.26 2.46 -13 -4 6 1.12 2.12 -13 4 6 2.41 0.74 -13 -4 -6 0.83 2.31 -13 4 7 15.72 1.17 -13 5 0 3.76 3.24 -13 5 0 3.97 2.95 -13 5 1 0.25 0.74 -13 5 1 0.83 0.66 -13 5 -1 0.64 1.01 -13 5 -1 0.95 0.74 -13 5 1 0.52 0.52 -13 5 2 7.31 1.02 -13 5 2 9.09 1.34 -13 5 -2 6.37 2.21 -13 5 -2 7.88 5.13 -13 5 2 10.17 5.77 -13 5 3 5.29 0.84 -13 5 3 5.08 0.93 -13 5 -3 5.07 0.86 -13 5 3 5.15 3.65 -13 5 -3 5.10 4.66 -13 5 4 7.53 1.15 -13 5 -4 6.69 1.10 -13 5 4 8.37 1.37 -13 5 5 21.45 1.42 -13 5 6 7.97 0.82 -13 6 0 4.43 1.82 -13 6 0 7.02 1.38 -13 6 1 3.50 0.61 -13 6 -1 5.30 0.78 -13 6 1 4.73 0.79 -13 6 -1 5.58 1.29 -13 6 1 6.03 4.01 -13 6 2 4.18 0.70 -13 6 2 4.49 0.74 -13 6 -2 4.03 3.69 -13 6 2 4.48 2.76 -13 6 3 2.41 0.54 -13 6 3 2.30 2.88 -13 6 -3 2.49 2.82 -13 6 4 1.93 1.31 -13 6 4 0.79 2.60 -13 6 -4 0.94 2.18 -13 6 5 0.36 0.92 -13 7 0 14.74 1.48 -13 7 -1 1.14 2.04 -13 7 1 1.23 2.10 -13 7 2 11.58 1.21 -13 7 -2 11.74 1.34 -13 7 3 0.79 1.83 -13 7 -3 0.58 1.94 -14 0 0 24.14 2.70 -14 0 -1 3.60 1.93 -14 0 1 4.01 2.21 -14 0 2 14.96 1.89 -14 0 -2 14.85 2.06 -14 0 3 -0.12 0.43 -14 0 -3 -0.15 0.74 -14 0 4 4.34 0.63 -14 0 4 4.96 0.82 -14 0 -4 6.01 3.38 -14 0 -5 1.28 1.47 -14 -1 0 10.29 3.97 -14 1 0 9.57 3.79 -14 1 0 10.61 1.59 -14 -1 -1 2.49 2.20 -14 1 -1 2.47 1.69 -14 1 1 2.34 2.29 -14 -1 1 2.57 1.71 -14 1 -1 1.10 2.34 -14 1 1 2.16 3.00 -14 1 2 6.65 1.27 -14 -1 2 6.11 1.18 -14 -1 -2 6.21 3.78 -14 1 -2 6.81 4.34 -14 1 -2 5.68 0.93 -14 1 2 5.87 1.19 -14 1 3 8.84 1.24 -14 1 3 15.66 1.99 -14 -1 3 17.39 2.15 -14 1 -3 16.79 2.65 -14 -1 -3 16.18 2.61 -14 1 4 1.79 1.29 -14 1 4 3.55 0.76 -14 -1 -4 3.64 2.56 -14 1 -4 3.38 3.35 -14 -1 -5 16.71 1.60 -14 1 -5 17.44 1.61 -14 -2 0 0.91 1.18 -14 2 0 1.06 0.91 -14 2 0 0.43 0.82 -14 -2 -1 10.77 1.67 -14 2 -1 11.99 1.88 -14 -2 1 11.93 1.73 -14 2 1 12.87 1.89 -14 2 -1 12.02 1.72 -14 2 1 10.31 1.60 -14 2 2 1.26 0.98 -14 -2 2 0.42 0.95 -14 -2 -2 0.57 0.69 -14 2 -2 0.66 0.63 -14 2 -2 0.29 0.83 -14 2 2 0.77 0.62 -14 2 3 14.95 1.89 -14 2 -3 14.50 2.04 -14 -2 -3 17.09 2.35 -14 2 3 16.47 2.15 -14 2 4 17.66 1.11 -14 2 4 21.97 1.56 -14 2 -4 19.88 1.63 -14 -2 -4 22.81 1.97 -14 2 -5 7.26 0.92 -14 -2 -5 7.23 1.00 -14 -3 0 0.27 0.36 -14 3 0 0.11 0.34 -14 3 0 0.11 0.25 -14 -3 1 3.75 0.66 -14 3 1 6.26 1.14 -14 -3 -1 5.33 0.90 -14 3 -1 5.32 3.87 -14 3 -1 5.54 0.98 -14 3 1 6.32 1.26 -14 3 2 4.78 3.20 -14 -3 -2 1.64 2.72 -14 3 -2 3.70 3.20 -14 3 -2 2.22 3.08 -14 3 2 4.47 0.99 -14 3 3 4.97 0.84 -14 -3 -3 1.30 2.87 -14 3 -3 4.32 0.86 -14 3 3 4.27 2.54 -14 3 -4 6.45 0.91 -14 -3 -4 7.04 0.98 -14 4 0 3.68 1.88 -14 4 0 3.60 2.49 -14 4 -1 0.69 0.77 -14 4 1 0.96 1.31 -14 4 -1 0.58 0.75 -14 4 1 0.50 0.93 -14 4 2 2.94 0.66 -14 4 -2 1.19 2.04 -14 4 -2 1.36 2.17 -14 4 2 1.43 2.94 -14 4 -3 0.89 1.53 -14 4 3 1.24 3.42 -14 5 0 10.83 1.04 -14 5 0 11.09 1.28 -14 5 1 0.18 0.94 -14 5 -1 0.56 0.95 -14 5 1 0.37 0.88 -14 5 2 4.91 0.83 -15 0 0 0.04 0.20 -15 0 -1 0.57 0.85 -15 1 0 0.08 0.23 -15 1 1 1.85 1.59 -15 1 -1 0.77 2.14 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 34920 _olex2_submission_special_instructions 'No special instructions were received'