#============================================================================= data_global _publ_requested_journal J.Med.Chem. #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Robert N. Young' _publ_contact_author_address ;Young, Robert Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada, V5A 1S6 ; _publ_contact_author_email roberty@sfu.ca _publ_contact_author_phone +1-778-782-3351 _publ_contact_author_fax +1-778-782-3765 loop_ _publ_author_name _publ_author_address 'Hamilton, C. Michael' ;Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada, V5A 1S6 ; #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _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 ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Design and synthesis of a photoaffinity labelling analogue of ivacaftor to probe its putative binding site on mutant CFTR ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; ## -------------------REFERENCES ----------------------## _publ_section_references ; Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G. M. (2015).Acta Cryst. C71, 3-8 Bruker (2013). SAINT, Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2014). APEX2, Bruker AXS Inc., Madison, Wisconsin, USA. H\"ubschle, C. B., Sheldrick, G. M. & Dittrich, B. (2011). J. Appl. Cryst. 44, 1281-1284. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _exptl_absorpt_process_details ; Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_CMH-04-045amidine #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C20 H29 F3 N3 O4' _chemical_formula_moiety 'C20 H29 F3 N3 O4' _chemical_formula_weight 432.46 #============================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' #------------------------------------------------ _cell_length_a 9.6508(3) _cell_length_b 10.7941(4) _cell_length_c 11.6332(3) _cell_angle_alpha 68.832(2) _cell_angle_beta 87.760(2) _cell_angle_gamma 87.527(3) _cell_volume 1128.67(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3146 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 66.21 _exptl_crystal_description plate _exptl_crystal_colour 'colourless' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 458 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrick , 1996)' _exptl_absorpt_correction_T_min 0.5452 _exptl_absorpt_correction_T_max 0.7531 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\f and \w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 10993 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_theta_min 4.076 _diffrn_reflns_theta_max 68.406 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measured_fraction_theta_full 0.954 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 3923 _reflns_number_gt 2461 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; 'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+0.1775P] where P=(Fo^2^+2Fc^2^)/3' ; _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3923 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.283 _refine_diff_density_min -0.231 #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker SAINT (Bruker, 2013)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2013)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015), Shelxle (H\"ubschle et al., 2011)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS 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' 'F' 'F' 0.0727 0.0534 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 O 0.24637(18) 0.3601(3) 0.2189(2) 0.0712(7) Uani 1 1 d . . . . . H1 H 0.517(4) 0.308(3) 0.346(3) 0.068(10) Uiso 1 1 d . . . . . F1 F 0.0313(2) 0.7959(2) 0.7199(2) 0.0850(6) Uani 1 1 d . . . . . N1 N 0.2436(2) 0.5927(2) 0.6505(2) 0.0486(6) Uani 1 1 d . . . . . C1 C 0.3019(3) 0.5851(3) 0.4494(3) 0.0473(6) Uani 1 1 d . . . . . O2 O 0.2909(2) 0.7224(2) 0.39784(19) 0.0623(6) Uani 1 1 d . . . . . F2 F 0.0471(2) 0.6252(2) 0.88219(18) 0.0880(7) Uani 1 1 d . . . . . N2 N 0.4296(2) 0.3163(3) 0.3446(2) 0.0518(6) Uani 1 1 d . . . . . C2 C 0.2680(2) 0.5175(3) 0.5727(2) 0.0434(6) Uani 1 1 d . . . . . F3 F 0.22943(18) 0.7270(2) 0.7955(2) 0.0873(7) Uani 1 1 d . . . . . O3 O 0.0889(2) 0.7436(2) 0.28836(19) 0.0635(6) Uani 1 1 d . . . . . N3 N 0.0047(2) 0.5495(3) 0.6841(2) 0.0679(8) Uani 1 1 d . . . . . H3A H 0.0020 0.5018 0.6390 0.082 Uiso 1 1 calc R U . . . H3B H -0.0695 0.5640 0.7214 0.082 Uiso 1 1 calc R U . . . C3 C 0.2743(3) 0.3805(3) 0.6167(2) 0.0459(6) Uani 1 1 d . . . . . H3 H 0.2464 0.3357 0.6982 0.055 Uiso 1 1 calc R U . . . O4 O 0.45229(17) 0.2828(2) 0.16817(16) 0.0543(5) Uani 1 1 d . . . . . C4 C 0.3200(2) 0.3045(3) 0.5463(2) 0.0439(6) Uani 1 1 d . . . . . C5 C 0.3670(2) 0.3778(3) 0.4254(2) 0.0463(6) Uani 1 1 d . . . . . C6 C 0.3535(3) 0.5145(3) 0.3789(2) 0.0499(7) Uani 1 1 d . . . . . H6 H 0.3802 0.5603 0.2973 0.060 Uiso 1 1 calc R U . . . C7 C 0.3171(3) 0.1516(3) 0.6001(3) 0.0508(7) Uani 1 1 d . . . . . C8 C 0.2505(4) 0.1011(3) 0.7302(3) 0.0713(9) Uani 1 1 d . . . . . H8A H 0.1575 0.1372 0.7274 0.107 Uiso 1 1 calc R U . . . H8B H 0.3038 0.1288 0.7842 0.107 Uiso 1 1 calc R U . . . H8C H 0.2487 0.0058 0.7605 0.107 Uiso 1 1 calc R U . . . C9 C 0.4632(3) 0.0886(3) 0.6099(3) 0.0688(9) Uani 1 1 d . . . . . H9A H 0.5057 0.1127 0.5292 0.103 Uiso 1 1 calc R U . . . H9B H 0.4579 -0.0063 0.6463 0.103 Uiso 1 1 calc R U . . . H9C H 0.5177 0.1199 0.6606 0.103 Uiso 1 1 calc R U . . . C10 C 0.2289(3) 0.1009(3) 0.5200(3) 0.0688(9) Uani 1 1 d . . . . . H10A H 0.1370 0.1400 0.5146 0.103 Uiso 1 1 calc R U . . . H10B H 0.2241 0.0059 0.5566 0.103 Uiso 1 1 calc R U . . . H10C H 0.2705 0.1250 0.4389 0.103 Uiso 1 1 calc R U . . . C11 C 0.1233(3) 0.6009(3) 0.6962(2) 0.0457(6) Uani 1 1 d . . . . . C12 C 0.1101(3) 0.6879(3) 0.7738(3) 0.0556(8) Uani 1 1 d . . . . . C13 C 0.3653(3) 0.3247(3) 0.2403(2) 0.0481(7) Uani 1 1 d . . . . . C14 C 0.4016(3) 0.2631(3) 0.0582(2) 0.0534(7) Uani 1 1 d . . . . . C15 C 0.2982(4) 0.1550(4) 0.0987(4) 0.0868(11) Uani 1 1 d . . . . . H15A H 0.2756 0.1313 0.0298 0.130 Uiso 1 1 calc R U . . . H15B H 0.2156 0.1857 0.1302 0.130 Uiso 1 1 calc R U . . . H15C H 0.3371 0.0785 0.1622 0.130 Uiso 1 1 calc R U . . . C16 C 0.5328(4) 0.2194(5) 0.0072(3) 0.0944(14) Uani 1 1 d . . . . . H16A H 0.5131 0.2051 -0.0672 0.142 Uiso 1 1 calc R U . . . H16B H 0.5687 0.1382 0.0668 0.142 Uiso 1 1 calc R U . . . H16C H 0.6004 0.2870 -0.0103 0.142 Uiso 1 1 calc R U . . . C17 C 0.3425(5) 0.3903(4) -0.0322(3) 0.0886(12) Uani 1 1 d . . . . . H17A H 0.4093 0.4587 -0.0502 0.133 Uiso 1 1 calc R U . . . H17B H 0.2595 0.4164 0.0025 0.133 Uiso 1 1 calc R U . . . H17C H 0.3211 0.3773 -0.1069 0.133 Uiso 1 1 calc R U . . . C18 C 0.1530(3) 0.7738(3) 0.3790(3) 0.0648(8) Uani 1 1 d . . . . . H18A H 0.1000 0.7380 0.4557 0.078 Uiso 1 1 calc R U . . . H18B H 0.1533 0.8696 0.3558 0.078 Uiso 1 1 calc R U . . . C19 C 0.1376(4) 0.8162(5) 0.1677(3) 0.0942(13) Uani 1 1 d . . . . . H19A H 0.2358 0.7958 0.1613 0.113 Uiso 1 1 calc R U . . . H19B H 0.1269 0.9104 0.1531 0.113 Uiso 1 1 calc R U . . . C20 C 0.0678(6) 0.7888(7) 0.0756(4) 0.139(2) Uani 1 1 d . . . . . H20A H -0.0027 0.7279 0.0975 0.166 Uiso 1 1 calc R U . . . H20B H 0.0924 0.8317 -0.0070 0.166 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0379(10) 0.119(2) 0.0782(15) -0.0625(14) -0.0104(9) 0.0111(11) F1 0.0868(13) 0.0670(12) 0.1164(17) -0.0518(12) -0.0232(11) 0.0231(11) N1 0.0392(11) 0.0621(15) 0.0561(14) -0.0351(12) -0.0040(9) 0.0003(10) C1 0.0389(12) 0.0513(17) 0.0550(17) -0.0224(14) -0.0048(11) -0.0041(12) O2 0.0602(12) 0.0523(12) 0.0741(14) -0.0216(10) -0.0053(10) -0.0075(10) F2 0.1093(15) 0.1046(16) 0.0639(13) -0.0479(12) 0.0140(11) -0.0112(13) N2 0.0411(12) 0.0751(17) 0.0486(14) -0.0343(13) -0.0025(10) 0.0052(12) C2 0.0329(11) 0.0551(17) 0.0511(16) -0.0296(13) -0.0049(10) -0.0002(12) F3 0.0576(10) 0.1182(17) 0.1289(17) -0.0947(15) -0.0123(10) -0.0034(11) O3 0.0572(11) 0.0698(14) 0.0588(13) -0.0177(11) -0.0003(9) -0.0026(10) N3 0.0453(13) 0.088(2) 0.096(2) -0.0631(17) 0.0081(12) -0.0117(13) C3 0.0440(13) 0.0557(17) 0.0418(15) -0.0224(13) -0.0011(10) -0.0010(13) O4 0.0419(9) 0.0857(14) 0.0459(11) -0.0372(10) -0.0021(7) 0.0049(9) C4 0.0371(12) 0.0555(16) 0.0434(15) -0.0234(13) -0.0062(10) 0.0053(12) C5 0.0348(12) 0.0633(18) 0.0486(16) -0.0296(14) -0.0021(10) 0.0014(12) C6 0.0431(13) 0.0634(19) 0.0439(15) -0.0199(14) -0.0003(11) -0.0053(13) C7 0.0485(14) 0.0542(17) 0.0527(17) -0.0231(14) -0.0053(12) 0.0029(13) C8 0.085(2) 0.0601(19) 0.063(2) -0.0175(16) 0.0043(16) 0.0012(18) C9 0.0609(18) 0.0597(19) 0.088(2) -0.0304(18) -0.0102(16) 0.0085(16) C10 0.0700(19) 0.068(2) 0.072(2) -0.0270(17) -0.0110(16) -0.0146(17) C11 0.0437(14) 0.0490(16) 0.0498(16) -0.0242(13) -0.0074(11) 0.0017(12) C12 0.0494(15) 0.0621(19) 0.067(2) -0.0374(16) -0.0093(14) 0.0047(15) C13 0.0393(13) 0.0659(18) 0.0472(16) -0.0300(14) 0.0044(11) -0.0057(13) C14 0.0511(14) 0.071(2) 0.0440(16) -0.0281(15) -0.0078(12) 0.0019(14) C15 0.091(3) 0.097(3) 0.087(3) -0.049(2) -0.007(2) -0.016(2) C16 0.072(2) 0.162(4) 0.077(3) -0.079(3) -0.0033(18) 0.019(2) C17 0.117(3) 0.090(3) 0.057(2) -0.023(2) -0.021(2) 0.009(2) C18 0.077(2) 0.0566(19) 0.062(2) -0.0229(16) -0.0045(15) 0.0090(17) C19 0.086(2) 0.124(4) 0.063(2) -0.022(2) 0.0056(19) -0.017(3) C20 0.144(4) 0.212(6) 0.065(3) -0.052(3) -0.003(3) -0.047(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C13 1.200(3) . ? F1 C12 1.328(3) . ? N1 C11 1.270(3) . ? N1 C2 1.426(3) . ? C1 C6 1.374(4) . ? C1 O2 1.385(3) . ? C1 C2 1.388(4) . ? O2 C18 1.414(4) . ? F2 C12 1.333(4) . ? N2 C13 1.356(3) . ? N2 C5 1.436(3) . ? N2 H1 0.84(3) . ? C2 C3 1.378(4) . ? F3 C12 1.307(3) . ? O3 C18 1.385(3) . ? O3 C19 1.411(4) . ? N3 C11 1.327(3) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C3 C4 1.402(4) . ? C3 H3 0.9300 . ? O4 C13 1.342(3) . ? O4 C14 1.476(3) . ? C4 C5 1.409(4) . ? C4 C7 1.541(4) . ? C5 C6 1.378(4) . ? C6 H6 0.9300 . ? C7 C9 1.529(4) . ? C7 C8 1.537(4) . ? C7 C10 1.537(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.519(4) . ? C14 C15 1.499(5) . ? C14 C17 1.501(5) . ? C14 C16 1.507(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.411(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9300 . ? C20 H20B 0.9300 . ? 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 C11 N1 C2 120.7(2) . . ? C6 C1 O2 119.5(3) . . ? C6 C1 C2 119.1(3) . . ? O2 C1 C2 121.3(2) . . ? C1 O2 C18 114.2(2) . . ? C13 N2 C5 120.2(2) . . ? C13 N2 H1 118(2) . . ? C5 N2 H1 116(2) . . ? C3 C2 C1 118.3(2) . . ? C3 C2 N1 123.0(2) . . ? C1 C2 N1 118.2(2) . . ? C18 O3 C19 113.7(3) . . ? C11 N3 H3A 120.0 . . ? C11 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C2 C3 C4 124.1(3) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C13 O4 C14 120.6(2) . . ? C3 C4 C5 115.4(3) . . ? C3 C4 C7 121.0(2) . . ? C5 C4 C7 123.6(2) . . ? C6 C5 C4 120.5(2) . . ? C6 C5 N2 116.6(2) . . ? C4 C5 N2 122.9(3) . . ? C1 C6 C5 122.0(3) . . ? C1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C9 C7 C8 107.1(3) . . ? C9 C7 C10 109.7(3) . . ? C8 C7 C10 106.5(3) . . ? C9 C7 C4 111.6(2) . . ? C8 C7 C4 111.5(2) . . ? C10 C7 C4 110.2(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 N3 130.7(2) . . ? N1 C11 C12 115.4(2) . . ? N3 C11 C12 113.8(2) . . ? F3 C12 F1 107.6(3) . . ? F3 C12 F2 107.8(2) . . ? F1 C12 F2 105.2(2) . . ? F3 C12 C11 113.2(2) . . ? F1 C12 C11 111.3(2) . . ? F2 C12 C11 111.4(3) . . ? O1 C13 O4 125.5(2) . . ? O1 C13 N2 124.4(2) . . ? O4 C13 N2 110.0(2) . . ? O4 C14 C15 108.8(2) . . ? O4 C14 C17 111.3(2) . . ? C15 C14 C17 112.3(3) . . ? O4 C14 C16 101.6(2) . . ? C15 C14 C16 111.3(3) . . ? C17 C14 C16 111.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 O2 112.6(2) . . ? O3 C18 H18A 109.1 . . ? O2 C18 H18A 109.1 . . ? O3 C18 H18B 109.1 . . ? O2 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O3 C19 C20 113.4(4) . . ? O3 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? O3 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C19 C20 H20A 120.0 . . ? C19 C20 H20B 120.0 . . ? H20A C20 H20B 120.0 . . ? _shelx_res_file ; cu_CMH_03_045sp_run_0m_a.res created by SHELXL-2014/7 TITL cu_CMH_03_045sp_run_0m_a.res in P-1 REM Old TITL cu_CMH_03_045sp_run_0m in P-1 REM SHELXT solution in P-1 REM R1 0.206, Rweak 0.018, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C20 F3 N4 O3 CELL 1.54178 9.6508 10.7941 11.6332 68.832 87.760 87.527 ZERR 2.000 0.0003 0.0004 0.0003 0.002 0.002 0.003 LATT 1 SFAC C F N O H UNIT 40 6 6 8 58 TEMP 23.000 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 20 acta WGHT 0.077000 0.177500 EXTI 0.003621 FVAR 0.80196 O1 4 0.246374 0.360053 0.218904 11.00000 0.03787 0.11937 = 0.07818 -0.06254 -0.01037 0.01107 H1 5 0.516919 0.308449 0.345662 11.00000 0.06840 F1 2 0.031260 0.795890 0.719931 11.00000 0.08676 0.06698 = 0.11636 -0.05182 -0.02319 0.02311 N1 3 0.243566 0.592743 0.650518 11.00000 0.03922 0.06211 = 0.05613 -0.03508 -0.00403 0.00033 C1 1 0.301867 0.585099 0.449367 11.00000 0.03887 0.05126 = 0.05502 -0.02242 -0.00482 -0.00414 O2 4 0.290901 0.722408 0.397835 11.00000 0.06021 0.05231 = 0.07413 -0.02157 -0.00530 -0.00752 F2 2 0.047067 0.625183 0.882190 11.00000 0.10926 0.10462 = 0.06395 -0.04787 0.01397 -0.01124 N2 3 0.429631 0.316341 0.344553 11.00000 0.04111 0.07512 = 0.04859 -0.03429 -0.00251 0.00515 C2 1 0.267978 0.517486 0.572727 11.00000 0.03290 0.05509 = 0.05109 -0.02963 -0.00489 -0.00018 F3 2 0.229434 0.727010 0.795471 11.00000 0.05760 0.11821 = 0.12885 -0.09470 -0.01227 -0.00343 O3 4 0.088867 0.743550 0.288360 11.00000 0.05720 0.06983 = 0.05882 -0.01773 -0.00027 -0.00257 N3 3 0.004696 0.549543 0.684120 11.00000 0.04533 0.08779 = 0.09577 -0.06312 0.00810 -0.01170 AFIX 93 H3A 5 0.001976 0.501790 0.638995 11.00000 -1.20000 H3B 5 -0.069450 0.564020 0.721401 11.00000 -1.20000 AFIX 0 C3 1 0.274250 0.380504 0.616702 11.00000 0.04400 0.05567 = 0.04185 -0.02238 -0.00109 -0.00097 AFIX 43 H3 5 0.246424 0.335697 0.698192 11.00000 -1.20000 AFIX 0 O4 4 0.452293 0.282840 0.168174 11.00000 0.04189 0.08570 = 0.04593 -0.03725 -0.00210 0.00486 C4 1 0.319951 0.304548 0.546250 11.00000 0.03712 0.05548 = 0.04341 -0.02336 -0.00615 0.00525 C5 1 0.367013 0.377770 0.425432 11.00000 0.03477 0.06328 = 0.04856 -0.02959 -0.00214 0.00143 C6 1 0.353513 0.514454 0.378921 11.00000 0.04308 0.06344 = 0.04393 -0.01986 -0.00026 -0.00532 AFIX 43 H6 5 0.380183 0.560309 0.297321 11.00000 -1.20000 AFIX 0 C7 1 0.317102 0.151624 0.600056 11.00000 0.04848 0.05424 = 0.05270 -0.02306 -0.00528 0.00285 C8 1 0.250516 0.101131 0.730231 11.00000 0.08547 0.06006 = 0.06347 -0.01751 0.00432 0.00125 AFIX 137 H8A 5 0.157465 0.137159 0.727355 11.00000 -1.50000 H8B 5 0.303753 0.128843 0.784193 11.00000 -1.50000 H8C 5 0.248731 0.005849 0.760469 11.00000 -1.50000 AFIX 0 C9 1 0.463194 0.088636 0.609940 11.00000 0.06093 0.05971 = 0.08846 -0.03037 -0.01020 0.00853 AFIX 137 H9A 5 0.505725 0.112732 0.529168 11.00000 -1.50000 H9B 5 0.457892 -0.006312 0.646258 11.00000 -1.50000 H9C 5 0.517710 0.119931 0.660600 11.00000 -1.50000 AFIX 0 C10 1 0.228917 0.100872 0.520015 11.00000 0.07003 0.06800 = 0.07188 -0.02703 -0.01096 -0.01457 AFIX 137 H10A 5 0.137039 0.140022 0.514612 11.00000 -1.50000 H10B 5 0.224145 0.005898 0.556560 11.00000 -1.50000 H10C 5 0.270482 0.124995 0.438875 11.00000 -1.50000 AFIX 0 C11 1 0.123331 0.600900 0.696224 11.00000 0.04374 0.04904 = 0.04981 -0.02422 -0.00737 0.00175 C12 1 0.110080 0.687920 0.773842 11.00000 0.04944 0.06207 = 0.06725 -0.03743 -0.00926 0.00469 C13 1 0.365259 0.324733 0.240345 11.00000 0.03927 0.06587 = 0.04716 -0.02997 0.00440 -0.00569 C14 1 0.401569 0.263098 0.058175 11.00000 0.05111 0.07138 = 0.04397 -0.02815 -0.00778 0.00192 C15 1 0.298163 0.154951 0.098739 11.00000 0.09073 0.09739 = 0.08681 -0.04871 -0.00678 -0.01617 AFIX 137 H15A 5 0.275642 0.131349 0.029784 11.00000 -1.50000 H15B 5 0.215571 0.185713 0.130194 11.00000 -1.50000 H15C 5 0.337054 0.078533 0.162215 11.00000 -1.50000 AFIX 0 C16 1 0.532845 0.219365 0.007220 11.00000 0.07245 0.16152 = 0.07703 -0.07885 -0.00328 0.01879 AFIX 137 H16A 5 0.513108 0.205105 -0.067221 11.00000 -1.50000 H16B 5 0.568689 0.138175 0.066758 11.00000 -1.50000 H16C 5 0.600363 0.286955 -0.010336 11.00000 -1.50000 AFIX 0 C17 1 0.342545 0.390342 -0.032229 11.00000 0.11658 0.08993 = 0.05670 -0.02281 -0.02116 0.00950 AFIX 137 H17A 5 0.409265 0.458679 -0.050159 11.00000 -1.50000 H17B 5 0.259546 0.416382 0.002543 11.00000 -1.50000 H17C 5 0.321073 0.377345 -0.106892 11.00000 -1.50000 AFIX 0 C18 1 0.153001 0.773814 0.378960 11.00000 0.07679 0.05662 = 0.06164 -0.02288 -0.00447 0.00895 AFIX 23 H18A 5 0.099956 0.737976 0.455715 11.00000 -1.20000 H18B 5 0.153278 0.869612 0.355831 11.00000 -1.20000 AFIX 0 C19 1 0.137625 0.816189 0.167723 11.00000 0.08634 0.12410 = 0.06290 -0.02177 0.00560 -0.01713 AFIX 23 H19A 5 0.235843 0.795802 0.161271 11.00000 -1.20000 H19B 5 0.126909 0.910385 0.153118 11.00000 -1.20000 AFIX 0 C20 1 0.067820 0.788822 0.075604 11.00000 0.14394 0.21229 = 0.06534 -0.05202 -0.00280 -0.04736 AFIX 93 H20A 5 -0.002714 0.727890 0.097542 11.00000 -1.20000 H20B 5 0.092353 0.831720 -0.007038 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM cu_CMH_03_045sp_run_0m_a.res in P-1 REM R1 = 0.0566 for 2461 Fo > 4sig(Fo) and 0.0913 for all 3923 data REM 282 parameters refined using 0 restraints END WGHT 0.0770 0.1775 REM Highest difference peak 0.283, deepest hole -0.231, 1-sigma level 0.048 Q1 1 0.0714 0.8934 0.0877 11.00000 0.05 0.28 Q2 1 0.1428 0.6424 0.8843 11.00000 0.05 0.27 Q3 1 0.1520 0.7261 0.1670 11.00000 0.05 0.23 Q4 1 -0.0288 0.7834 0.0841 11.00000 0.05 0.23 Q5 1 0.1442 0.8133 0.6982 11.00000 0.05 0.21 Q6 1 0.2452 0.8603 0.1776 11.00000 0.05 0.20 Q7 1 0.1686 0.6554 0.1150 11.00000 0.05 0.20 Q8 1 0.4409 0.3936 -0.0399 11.00000 0.05 0.20 Q9 1 0.2756 0.5830 0.6826 11.00000 0.05 0.17 Q10 1 0.5423 0.1206 0.5707 11.00000 0.05 0.16 Q11 1 0.1755 0.6773 0.5828 11.00000 0.05 0.16 Q12 1 0.0306 0.9609 0.1598 11.00000 0.05 0.16 Q13 1 0.3209 0.2390 0.5641 11.00000 0.05 0.15 Q14 1 0.2095 0.8023 0.2669 11.00000 0.05 0.15 Q15 1 0.4369 0.2055 0.3884 11.00000 0.05 0.15 Q16 1 -0.0442 0.8937 0.0421 11.00000 0.05 0.15 Q17 1 0.2492 0.5267 0.3626 11.00000 0.05 0.15 Q18 1 0.3781 0.4422 0.5982 11.00000 0.05 0.15 Q19 1 0.1808 0.5912 0.6773 11.00000 0.05 0.14 Q20 1 0.2070 0.3711 -0.0424 11.00000 0.05 0.14 ; _shelx_res_checksum 31615 _shelx_hkl_file ; 1 0 0 36.90 2.70 2 0 0 1029.90 62.29 3 0 0 1005.60 61.19 -4 0 0 648.84 39.30 4 0 0 655.63 40.60 -5 0 0 203.68 12.70 5 0 0 206.58 14.40 -6 0 0 170.18 10.60 6 0 0 158.18 12.50 -7 0 0 32.30 3.00 7 0 0 33.00 5.00 7 0 0 36.80 5.30 7 0 0 27.10 4.90 -8 0 0 73.99 7.00 -8 0 0 60.79 4.90 8 0 0 62.79 7.80 8 0 0 63.59 7.40 8 0 0 53.19 6.80 8 0 0 65.79 7.30 -9 0 0 48.10 4.20 9 0 0 45.30 7.00 9 0 0 49.30 6.60 9 0 0 49.70 7.30 -10 0 0 18.30 2.80 -10 0 0 20.70 3.10 10 0 0 23.80 4.70 10 0 0 26.20 4.80 10 0 0 27.20 5.30 -11 0 0 4.00 1.70 11 0 0 1.70 2.40 11 0 0 2.80 2.60 11 -1 0 36.60 4.60 -11 1 0 32.50 3.30 10 -1 0 -0.10 2.90 10 -1 0 -2.70 2.70 -10 1 0 -0.10 1.80 9 -1 0 5.60 3.30 9 -1 0 -0.30 3.20 9 -1 0 3.50 3.40 -9 1 0 1.90 1.70 -9 1 0 1.40 2.00 8 -1 0 90.39 8.30 8 -1 0 75.99 7.90 8 -1 0 86.29 8.60 -8 1 0 98.19 6.50 7 -1 0 -0.20 2.30 7 -1 0 0.80 2.60 7 -1 0 -2.80 2.50 7 -1 0 2.60 2.40 -7 1 0 0.50 1.10 -7 1 0 0.60 2.10 6 -1 0 12.20 3.20 -6 1 0 7.10 1.30 5 -1 0 48.10 5.20 -5 1 0 54.09 3.80 4 -1 0 274.77 18.20 -4 1 0 279.47 17.00 3 -1 0 2435.46 146.39 2 -1 0 5251.57 313.97 1 -1 0 0.90 0.60 1 1 0 34.90 2.60 1 1 0 28.90 2.40 1 1 0 32.60 2.20 2 1 0 9999.00 597.24 3 1 0 331.47 21.20 4 1 0 351.36 22.70 -5 -1 0 9.20 1.30 5 1 0 10.00 2.60 -6 -1 0 22.00 2.10 6 1 0 23.30 3.60 -7 -1 0 18.80 2.20 7 1 0 22.80 4.70 7 1 0 24.40 4.70 7 1 0 18.20 4.00 7 1 0 17.50 4.10 -8 -1 0 43.70 3.60 8 1 0 49.99 8.90 8 1 0 35.00 6.40 8 1 0 31.60 5.90 8 1 0 43.90 6.70 -9 -1 0 0.10 1.20 9 1 0 5.90 3.90 9 1 0 -1.10 3.50 9 1 0 -1.30 3.50 -10 -1 0 9.60 1.90 -10 -1 0 7.20 2.10 10 1 0 8.00 4.00 10 1 0 6.20 3.60 10 1 0 6.20 3.70 -11 -1 0 -1.30 1.50 11 1 0 2.10 2.90 11 1 0 -0.30 2.20 11 1 0 -0.80 2.70 11 -2 0 28.90 3.70 -11 2 0 20.60 3.60 -11 2 0 15.50 2.10 10 -2 0 3.10 3.10 -10 2 0 2.50 1.80 9 -2 0 21.30 4.60 -9 2 0 27.80 3.50 8 -2 0 31.70 5.50 8 -2 0 25.20 5.10 -8 2 0 28.60 3.20 -8 2 0 29.30 3.60 7 -2 0 4.50 2.80 7 -2 0 2.80 2.90 7 -2 0 3.40 2.90 -7 2 0 0.60 1.20 -7 2 0 1.30 1.80 6 -2 0 0.60 2.00 -6 2 0 0.50 1.00 5 -2 0 128.19 9.80 -5 2 0 134.39 8.50 4 -2 0 344.47 23.10 -4 2 0 376.86 22.10 3 -2 0 44.10 4.00 2 -2 0 47.50 3.70 1 -2 0 107.89 6.80 0 -2 0 5179.28 316.67 0 2 0 5427.46 316.77 1 2 0 332.17 20.10 1 2 0 327.77 20.40 2 2 0 1220.98 74.69 2 2 0 1121.29 74.39 2 2 0 1383.46 74.99 3 2 0 1189.28 67.99 3 2 0 1043.00 67.59 4 2 0 12.90 2.50 4 2 0 14.30 3.00 -5 -2 0 0.20 0.60 5 2 0 3.80 1.90 5 2 0 3.60 2.20 -6 -2 0 193.68 12.20 6 2 0 197.68 14.30 -7 -2 0 1.00 0.90 7 2 0 -2.00 3.10 7 2 0 -2.00 2.60 7 2 0 1.60 2.40 7 2 0 2.10 2.90 -8 -2 0 55.39 4.30 8 2 0 57.09 7.20 8 2 0 59.19 7.00 8 2 0 44.90 7.20 -9 -2 0 -0.60 1.20 9 2 0 0.30 3.60 9 2 0 2.40 4.30 9 2 0 1.70 3.80 -10 -2 0 23.30 2.60 10 2 0 24.20 4.80 10 2 0 10.50 3.60 10 2 0 22.00 4.80 -11 -2 0 2.50 1.60 11 2 0 -0.80 2.70 11 2 0 1.50 2.10 11 2 0 3.50 3.00 11 -3 0 -0.70 1.50 -11 3 0 -1.50 1.80 10 -3 0 23.80 4.40 -10 3 0 12.80 2.20 -10 3 0 5.70 3.10 9 -3 0 27.00 5.60 -9 3 0 29.60 3.40 8 -3 0 13.60 3.90 -8 3 0 13.10 2.60 7 -3 0 18.40 4.10 7 -3 0 23.60 4.50 -7 3 0 22.10 3.10 6 -3 0 92.49 10.50 -6 3 0 128.69 7.90 -5 3 0 40.70 3.30 4 -3 0 2.60 1.50 -4 3 0 1.90 0.90 3 -3 0 211.68 13.70 2 -3 0 27.60 2.50 1 -3 0 178.68 11.10 0 -3 0 85.69 6.20 0 3 0 100.19 6.30 1 3 0 2894.91 170.78 1 3 0 2813.52 171.18 2 3 0 275.27 17.80 2 3 0 304.77 18.40 3 3 0 100.89 7.40 4 3 0 161.58 11.40 5 3 0 26.30 3.60 -6 -3 0 146.79 9.60 6 3 0 168.08 12.00 -7 -3 0 -0.20 0.80 7 3 0 -3.30 2.90 7 3 0 -1.80 2.50 7 3 0 1.90 2.50 7 3 0 -0.30 3.90 -8 -3 0 17.40 2.20 8 3 0 16.80 4.80 8 3 0 13.90 3.70 8 3 0 26.50 5.90 -9 -3 0 1.60 1.10 9 3 0 -1.30 3.10 9 3 0 0.50 3.50 9 3 0 1.60 4.50 10 3 0 2.20 3.50 10 3 0 7.60 3.90 10 3 0 0.60 2.70 -11 -3 0 -3.00 1.20 11 3 0 2.20 2.90 11 3 0 0.60 2.40 10 -4 0 9.40 2.50 -10 4 0 0.10 2.50 9 -4 0 24.80 4.90 -9 4 0 21.00 2.80 -9 4 0 22.10 4.40 8 -4 0 7.50 3.60 -8 4 0 4.00 1.80 -8 4 0 6.30 4.10 7 -4 0 26.20 5.00 7 -4 0 32.90 5.90 -7 4 0 29.60 3.40 6 -4 0 -4.30 3.50 6 -4 0 0.00 2.70 -6 4 0 0.90 1.70 3 -4 0 31.70 2.90 2 -4 0 165.48 10.50 0 -4 0 96.99 7.20 0 4 0 124.39 7.60 1 4 0 321.37 20.00 2 4 0 784.52 48.20 3 4 0 312.57 20.30 4 4 0 9.90 2.40 5 4 0 25.20 3.70 -6 -4 0 0.30 0.60 6 4 0 0.20 2.80 6 4 0 2.00 2.00 6 4 0 2.80 3.50 -7 -4 0 3.10 1.00 7 4 0 4.30 3.40 7 4 0 -0.30 2.40 7 4 0 5.50 4.40 -8 -4 0 8.00 1.40 8 4 0 13.00 4.50 8 4 0 5.30 4.30 -9 -4 0 28.80 2.80 9 4 0 37.00 6.30 9 4 0 32.10 6.70 10 4 0 0.80 3.30 10 4 0 2.50 3.30 11 4 0 17.10 3.10 11 4 0 8.60 2.70 -10 5 0 1.20 2.00 -9 5 0 10.50 3.20 8 -5 0 12.00 5.00 -8 5 0 7.50 3.70 7 -5 0 15.80 5.40 -7 5 0 4.00 3.80 6 -5 0 24.50 5.20 -6 5 0 32.80 6.20 5 -5 0 0.60 3.70 -5 5 0 -1.90 3.50 3 -5 0 387.66 24.00 2 -5 0 192.18 12.30 -1 5 0 91.79 7.20 0 -5 0 24.30 2.10 0 5 0 27.30 2.90 -1 -5 0 2582.34 154.28 3 5 0 114.49 8.80 4 5 0 88.39 7.60 5 5 0 1.20 2.00 5 5 0 0.90 4.20 6 5 0 6.60 4.10 6 5 0 3.40 2.40 6 5 0 1.90 3.10 6 5 0 2.80 4.90 -7 -5 0 2.00 0.90 7 5 0 3.00 4.60 7 5 0 -0.50 3.10 -8 -5 0 0.90 1.00 8 5 0 0.90 4.50 8 5 0 -3.00 3.40 -9 -5 0 14.90 2.00 9 5 0 10.70 4.20 9 5 0 22.50 5.30 10 5 0 1.10 3.10 10 5 0 2.20 3.10 -9 6 0 2.40 2.50 8 -6 0 5.90 4.40 -8 6 0 2.20 3.10 7 -6 0 71.29 9.70 -7 6 0 65.29 7.60 6 -6 0 21.70 5.70 -6 6 0 17.60 4.80 5 -6 0 7.90 4.80 -5 6 0 -1.00 3.70 4 -6 0 2.90 2.10 4 -6 0 1.00 3.70 -4 6 0 1.20 3.20 3 -6 0 43.40 3.90 -3 6 0 36.70 5.00 2 -6 0 17.70 2.30 -2 6 0 14.20 3.10 1 -6 0 7.70 1.50 0 -6 0 127.29 8.10 -1 -6 0 19.90 1.80 -2 -6 0 31.60 2.50 -3 -6 0 345.77 21.00 4 6 0 92.89 8.90 4 6 0 83.49 9.90 5 6 0 21.50 5.30 5 6 0 17.50 5.60 5 6 0 12.40 3.50 -6 -6 0 24.20 2.80 6 6 0 16.50 4.20 6 6 0 16.00 5.80 6 6 0 20.40 5.60 7 6 0 22.00 6.10 7 6 0 32.60 6.10 7 6 0 33.70 5.80 -8 -6 0 1.80 1.20 8 6 0 -0.40 3.70 8 6 0 -4.90 4.00 9 6 0 3.80 3.60 9 6 0 2.00 3.40 10 6 0 1.10 2.20 10 6 0 4.90 2.80 -9 7 0 -0.10 1.70 8 -7 0 19.90 4.50 -8 7 0 24.30 4.00 7 -7 0 20.70 5.40 -7 7 0 10.40 3.50 6 -7 0 13.10 5.10 -6 7 0 11.20 4.10 5 -7 0 45.90 8.60 -5 7 0 44.40 6.50 4 -7 0 0.60 2.20 4 -7 0 2.70 4.10 -4 7 0 4.70 3.70 3 -7 0 11.00 2.90 3 -7 0 14.30 4.10 -3 7 0 12.00 4.20 -3 7 0 17.20 5.30 2 -7 0 12.80 2.70 2 -7 0 10.50 2.10 -2 7 0 16.60 5.50 -2 7 0 16.70 4.10 -2 7 0 7.70 5.00 1 -7 0 37.80 3.50 -1 7 0 35.30 9.70 -1 7 0 41.60 8.20 -1 -7 0 50.39 3.70 1 7 0 47.90 8.30 1 7 0 44.70 8.80 -2 -7 0 95.49 6.10 2 7 0 88.79 10.70 2 7 0 77.19 10.00 2 7 0 96.89 8.90 -3 -7 0 3.70 1.10 3 7 0 -2.60 3.40 3 7 0 -8.20 3.80 3 7 0 4.90 4.50 -4 -7 0 3.90 1.10 4 7 0 3.60 4.90 4 7 0 9.00 4.00 4 7 0 -2.70 4.20 -5 -7 0 20.80 2.10 5 7 0 15.20 5.70 5 7 0 14.40 5.00 -6 -7 0 4.90 1.30 6 7 0 2.30 4.80 6 7 0 3.80 4.80 -7 -7 0 1.50 1.20 7 7 0 7.40 4.70 7 7 0 -2.00 4.70 8 7 0 7.60 4.10 9 7 0 9.90 3.10 8 -8 0 8.80 2.90 -8 8 0 17.00 2.80 7 -8 0 11.20 4.30 -7 8 0 8.60 2.90 6 -8 0 -0.40 4.40 -6 8 0 9.30 3.70 5 -8 0 18.30 5.30 -5 8 0 7.50 3.90 4 -8 0 5.10 4.30 4 -8 0 0.50 2.30 -4 8 0 1.60 3.50 3 -8 0 26.10 4.10 3 -8 0 33.10 6.20 -3 8 0 31.40 6.90 -3 8 0 39.10 6.00 2 -8 0 79.29 7.10 2 -8 0 100.59 6.80 -2 8 0 81.99 11.50 -2 8 0 85.59 10.80 -2 8 0 80.59 8.20 1 -8 0 30.90 3.10 1 -8 0 20.30 3.50 -1 8 0 17.70 5.80 -1 8 0 16.60 4.10 -1 8 0 17.60 6.40 0 -8 0 49.40 3.90 0 8 0 27.70 6.90 0 8 0 35.70 8.10 0 8 0 39.00 6.00 1 8 0 23.30 6.70 1 8 0 19.70 4.70 1 8 0 24.90 6.90 -2 -8 0 11.20 1.70 2 8 0 22.20 6.90 2 8 0 10.60 4.20 2 8 0 7.20 5.40 -3 -8 0 33.80 2.90 3 8 0 21.20 6.50 3 8 0 35.00 6.10 3 8 0 21.60 6.30 -4 -8 0 1.40 1.20 4 8 0 -3.50 5.00 4 8 0 0.70 3.80 4 8 0 -1.00 4.90 -5 -8 0 5.40 1.50 5 8 0 12.10 5.00 5 8 0 -0.50 4.70 -6 -8 0 18.20 2.40 6 8 0 11.90 4.70 6 8 0 21.70 6.90 7 8 0 40.60 8.10 7 8 0 34.40 6.70 8 8 0 -2.70 2.80 7 -9 0 -0.20 2.30 -7 9 0 2.20 1.90 6 -9 0 3.50 3.70 -6 9 0 2.20 2.40 5 -9 0 8.80 4.70 -5 9 0 11.10 3.50 4 -9 0 9.80 2.60 4 -9 0 16.70 5.50 -4 9 0 12.40 4.20 3 -9 0 23.20 5.40 3 -9 0 19.20 3.30 -3 9 0 17.80 4.40 -3 9 0 22.80 6.50 2 -9 0 33.90 6.80 2 -9 0 37.60 4.30 2 -9 0 33.90 4.50 -2 9 0 33.90 7.50 -2 9 0 44.90 8.70 -2 9 0 39.60 6.10 1 -9 0 19.50 2.90 1 -9 0 2.80 3.90 1 -9 0 18.50 3.20 -1 9 0 16.60 4.70 -1 9 0 13.30 6.90 -1 9 0 12.60 6.20 0 -9 0 30.80 3.30 0 -9 0 20.00 3.40 0 9 0 23.50 5.00 0 9 0 20.30 6.70 0 9 0 20.80 7.30 -1 -9 0 3.00 1.50 1 9 0 -3.70 5.10 1 9 0 -0.70 4.20 1 9 0 2.10 5.70 2 9 0 18.50 5.20 2 9 0 11.90 7.30 2 9 0 6.40 5.50 -3 -9 0 0.20 1.20 3 9 0 -1.30 5.50 3 9 0 7.60 5.80 3 9 0 2.60 4.60 -4 -9 0 1.30 1.20 4 9 0 0.10 5.60 4 9 0 -2.50 4.70 4 9 0 -1.80 4.00 -5 -9 0 40.00 3.30 5 9 0 35.80 6.60 5 9 0 33.40 7.90 6 9 0 -2.00 4.30 6 9 0 6.50 3.70 7 9 0 -0.50 2.80 7 9 0 1.50 3.60 6 -10 0 -2.20 2.60 5 -10 0 -0.30 3.50 -5 10 0 0.20 2.10 4 -10 0 15.50 4.80 -4 10 0 9.40 3.00 3 -10 0 3.00 2.00 3 -10 0 2.40 4.00 -3 10 0 -0.30 7.20 -3 10 0 -0.20 3.00 2 -10 0 -1.50 2.00 2 -10 0 -1.40 3.90 -2 10 0 8.60 5.50 -2 10 0 0.00 5.30 -2 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1.10 3.10 1 -7 1 4.70 1.50 1 -7 1 0.50 2.10 -2 7 -1 56.89 8.10 -2 7 -1 54.29 6.90 -2 7 -1 57.09 9.00 2 -7 1 69.59 5.10 2 -7 1 56.59 5.60 2 -7 1 45.20 7.60 -3 7 -1 84.49 7.80 3 -7 1 61.79 8.60 3 -7 1 66.29 6.30 -4 7 -1 4.40 3.80 4 -7 1 3.10 4.60 4 -7 1 5.70 2.40 -5 7 -1 1.30 3.30 5 -7 1 -1.70 4.50 -6 7 -1 1.40 3.60 6 -7 1 2.70 5.30 -7 7 -1 1.40 2.90 7 -7 1 13.70 5.40 -8 7 -1 2.20 2.40 8 -7 1 1.00 3.00 -9 7 -1 3.90 2.90 10 6 -1 3.10 2.60 9 6 -1 22.50 4.60 9 6 -1 27.70 5.10 8 6 -1 2.90 4.00 8 6 -1 5.80 4.70 8 6 -1 2.80 4.70 -8 -6 1 5.60 1.40 7 6 -1 17.50 5.20 7 6 -1 12.90 5.50 7 6 -1 22.40 5.40 -7 -6 1 23.70 2.60 6 6 -1 4.20 4.00 6 6 -1 -9.30 4.10 6 6 -1 8.20 5.00 -6 -6 1 0.60 1.10 5 6 -1 0.00 2.30 5 6 -1 10.40 4.50 5 6 -1 -2.90 4.00 -5 -6 1 0.80 1.00 4 6 -1 7.70 5.10 4 6 -1 -0.30 3.50 -4 -6 1 3.50 1.00 3 6 -1 -3.70 3.70 3 6 -1 -0.60 4.00 -3 -6 1 -0.30 0.90 -2 -6 1 155.88 9.90 -1 -6 1 278.17 17.10 0 -6 1 53.59 3.90 1 -6 1 28.00 2.80 2 -6 1 5.90 1.60 -3 6 -1 26.40 5.10 3 -6 1 30.10 3.90 3 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17.10 2.30 3 7 -4 -2.50 4.30 3 7 -4 0.10 5.10 3 7 -4 -11.40 4.00 -3 -7 4 1.60 2.30 -3 -7 4 1.50 1.40 2 7 -4 33.70 6.10 2 7 -4 25.20 7.10 2 7 -4 32.30 7.20 -2 -7 4 28.10 3.20 -2 -7 4 24.70 3.90 1 7 -4 0.30 5.30 1 7 -4 14.70 4.60 1 7 -4 18.20 6.60 -1 -7 4 10.80 2.90 0 7 -4 -2.00 3.60 0 7 -4 -4.30 5.20 0 -7 4 -1.80 2.20 0 -7 4 0.20 1.70 -1 7 -4 3.00 5.60 -1 7 -4 -1.30 3.50 1 -7 4 0.20 2.30 -2 7 -4 0.20 3.80 -2 7 -4 3.00 6.10 2 -7 4 2.10 2.30 -3 7 -4 -2.60 3.70 3 -7 4 3.20 2.70 3 -7 4 -0.40 3.80 -4 7 -4 13.10 4.20 4 -7 4 26.10 6.00 -5 7 -4 -3.10 3.20 5 -7 4 -8.70 4.10 -6 7 -4 -0.60 2.90 6 -7 4 -4.70 4.00 -7 7 -4 -1.20 2.10 7 -7 4 4.50 3.70 8 6 -4 1.70 3.50 8 6 -4 5.50 3.00 8 6 -4 6.00 3.00 -8 -6 4 14.30 2.30 7 6 -4 1.80 3.70 7 6 -4 -1.80 4.60 7 6 -4 -0.90 3.50 -7 -6 4 -0.50 2.20 6 6 -4 45.60 9.10 6 6 -4 37.30 7.50 6 6 -4 18.40 5.00 5 6 -4 1.60 5.20 5 6 -4 2.70 4.50 5 6 -4 1.10 4.10 -5 -6 4 -0.40 1.40 4 6 -4 32.10 7.50 4 6 -4 39.30 6.70 -4 -6 4 41.10 3.70 3 6 -4 213.38 16.00 3 6 -4 206.88 17.40 3 6 -4 203.28 17.60 -3 -6 4 236.98 13.70 -3 -6 4 191.58 14.70 2 6 -4 22.90 4.80 2 6 -4 16.60 6.10 2 6 -4 16.70 6.70 -2 -6 4 18.60 2.60 -2 -6 4 14.20 3.00 1 6 -4 120.49 12.60 1 6 -4 90.29 11.70 1 6 -4 108.89 9.70 -1 -6 4 101.39 8.30 -1 -6 4 118.59 7.60 0 6 -4 6.40 5.70 0 6 -4 6.10 3.40 0 -6 4 6.50 2.60 -1 6 -4 3.90 5.60 -1 6 -4 7.50 4.00 1 -6 4 6.50 2.60 -2 6 -4 94.79 11.60 -2 6 -4 105.19 9.30 2 -6 4 94.69 7.50 2 -6 4 74.79 9.70 -3 6 -4 -2.10 3.20 3 -6 4 0.10 3.70 3 -6 4 0.10 2.20 -4 6 -4 10.40 4.60 4 -6 4 9.40 4.70 -5 6 -4 -0.10 3.70 5 -6 4 -2.50 4.40 -6 6 -4 1.90 3.30 6 -6 4 1.20 4.90 -7 6 -4 -3.30 2.70 7 -6 4 -5.40 3.70 -8 6 -4 3.10 2.10 8 -6 4 -2.40 2.70 9 5 -4 3.10 2.90 9 5 -4 0.80 2.50 -9 -5 4 2.90 1.70 8 5 -4 4.70 4.50 8 5 -4 3.00 3.60 8 5 -4 5.20 3.90 -8 -5 4 6.10 2.30 7 5 -4 18.30 5.40 7 5 -4 0.20 4.90 7 5 -4 7.80 4.20 -7 -5 4 7.30 1.70 -7 -5 4 11.90 4.60 6 5 -4 93.39 11.00 6 5 -4 73.79 9.10 6 5 -4 56.59 7.80 -6 -5 4 57.59 5.00 5 5 -4 41.10 7.50 5 5 -4 41.10 7.60 5 5 -4 40.50 8.40 -5 -5 4 34.70 3.60 4 5 -4 19.00 4.90 4 5 -4 8.00 4.90 4 5 -4 9.10 5.90 4 5 -4 11.20 4.70 -4 -5 4 9.40 1.90 -4 -5 4 13.70 4.70 3 5 -4 59.19 6.80 3 5 -4 50.99 9.00 3 5 -4 53.59 9.00 3 5 -4 44.40 7.50 -3 -5 4 45.50 4.00 -3 -5 4 44.40 6.60 2 5 -4 63.89 9.00 2 5 -4 82.09 9.80 2 5 -4 75.69 7.90 -2 -5 4 73.79 6.20 -2 -5 4 59.09 7.60 -2 -5 4 72.09 5.30 1 5 -4 399.06 29.00 1 5 -4 400.46 27.00 -1 -5 4 439.36 25.70 0 5 -4 11.00 3.30 0 5 -4 11.20 5.30 0 -5 4 10.40 1.90 0 -5 4 7.20 2.40 -1 5 -4 34.40 5.20 -1 5 -4 34.40 7.10 1 -5 4 45.30 3.80 1 -5 4 30.00 4.10 -2 5 -4 19.30 6.00 -2 5 -4 23.70 4.60 2 -5 4 21.20 3.30 2 -5 4 14.20 4.40 -3 5 -4 10.00 3.90 3 -5 4 4.00 2.20 3 -5 4 9.90 4.30 -4 5 -4 26.00 5.20 4 -5 4 16.40 4.80 -5 5 -4 -2.60 3.90 5 -5 4 -2.30 4.00 -6 5 -4 0.00 3.50 6 -5 4 -2.70 5.00 -7 5 -4 -0.90 3.10 7 -5 4 -3.20 4.40 -8 5 -4 3.20 2.90 8 -5 4 2.60 3.50 -9 5 -4 -0.90 1.80 9 -5 4 5.80 2.60 9 4 -4 -2.80 3.00 9 4 -4 0.70 3.10 -9 -4 4 3.10 2.00 8 4 -4 36.00 6.60 8 4 -4 20.50 5.90 8 4 -4 44.10 7.50 -8 -4 4 42.50 4.30 -8 -4 4 26.80 3.10 7 4 -4 89.89 11.10 7 4 -4 74.99 9.30 7 4 -4 72.09 8.70 -7 -4 4 63.89 5.30 6 4 -4 14.00 5.30 6 4 -4 2.70 4.40 6 4 -4 7.10 4.10 -6 -4 4 3.10 1.50 5 4 -4 -1.00 3.40 5 4 -4 1.50 4.50 5 4 -4 -1.50 3.90 5 4 -4 2.20 2.80 -5 -4 4 0.50 3.10 -5 -4 4 -1.30 1.20 4 4 -4 21.40 4.80 4 4 -4 15.50 5.50 4 4 -4 12.40 3.80 4 4 -4 12.20 3.40 -4 -4 4 8.70 1.80 -4 -4 4 16.80 4.50 3 4 -4 105.59 11.40 3 4 -4 96.69 7.90 -3 -4 4 82.79 8.50 -3 -4 4 75.69 5.90 -2 -4 4 168.28 13.50 -2 -4 4 176.58 11.20 -1 -4 4 21.90 2.40 -1 -4 4 26.30 4.40 0 -4 4 77.49 5.50 0 -4 4 78.69 7.30 1 -4 4 155.48 11.80 2 -4 4 -0.60 1.90 -3 4 -4 8.60 4.90 -4 4 -4 19.80 4.70 4 -4 4 34.20 6.40 -5 4 -4 6.80 4.00 5 -4 4 -0.60 4.00 -6 4 -4 12.50 4.70 -6 4 -4 5.70 2.20 6 -4 4 7.20 5.60 -7 4 -4 53.79 7.50 7 -4 4 69.19 9.70 -8 4 -4 9.50 3.90 8 -4 4 7.70 4.50 -9 4 -4 16.10 3.40 9 -4 4 11.40 3.70 10 3 -4 5.60 3.10 10 3 -4 2.50 2.30 -10 -3 4 1.10 1.40 9 3 -4 3.00 3.20 9 3 -4 -5.70 2.90 -9 -3 4 2.80 2.20 8 3 -4 52.19 7.60 8 3 -4 29.20 6.70 8 3 -4 39.30 8.00 -8 -3 4 48.20 4.80 -8 -3 4 43.60 3.70 7 3 -4 4.20 4.20 7 3 -4 0.20 5.00 7 3 -4 -1.70 3.60 -7 -3 4 -0.40 1.30 6 3 -4 5.00 3.80 6 3 -4 -1.80 4.10 6 3 -4 14.30 4.70 -6 -3 4 10.60 1.80 5 3 -4 348.17 21.50 5 3 -4 274.27 20.40 5 3 -4 271.67 20.20 5 3 -4 282.07 21.90 -5 -3 4 294.87 18.40 -5 -3 4 308.97 21.60 4 3 -4 52.79 5.70 -4 -3 4 56.29 6.70 -4 -3 4 46.50 3.90 3 3 -4 -0.80 1.40 -3 -3 4 -1.10 2.30 -3 -3 4 0.10 1.10 2 3 -4 43.80 4.40 -2 -3 4 45.00 5.40 -2 -3 4 34.20 3.10 -1 -3 4 2.90 2.30 -1 -3 4 6.50 1.30 0 -3 4 137.49 10.60 0 -3 4 134.39 8.70 1 -3 4 337.97 22.80 1 -3 4 346.27 21.10 2 -3 4 54.39 5.70 3 -3 4 87.89 7.90 4 -3 4 10.50 3.50 -5 3 -4 8.60 2.30 -5 3 -4 11.80 4.30 5 -3 4 4.30 4.40 -6 3 -4 41.20 6.80 -6 3 -4 38.00 4.30 6 -3 4 42.20 7.80 -7 3 -4 47.70 4.80 -7 3 -4 48.80 7.10 7 -3 4 63.39 9.40 -8 3 -4 2.50 1.90 -8 3 -4 6.90 4.30 8 -3 4 3.50 4.70 -9 3 -4 79.49 7.30 -9 3 -4 68.89 5.40 9 -3 4 100.09 9.30 -10 3 -4 -2.80 1.70 10 2 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4.30 3.70 -3 -7 -13 2.50 1.10 3 7 13 6.00 2.50 3 7 13 2.30 3.00 -4 -7 -13 0.60 0.90 4 7 13 0.80 1.50 2 -8 -13 -0.10 2.00 1 -8 -13 3.60 2.00 -1 8 13 9.40 3.40 0 -8 -13 2.20 1.00 0 -8 -13 1.80 2.00 0 8 13 8.80 3.80 -1 -8 -13 -0.80 2.00 -1 -8 -13 0.70 1.00 1 8 13 1.10 3.30 -2 -8 -13 1.70 1.00 2 8 13 4.50 2.80 2 8 13 2.10 3.30 -3 -8 -13 -0.90 0.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87048