data_testm1 _audit_creation_date 2017-07-04 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _shelxl_version_number 2013-4 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H19 N O2' _chemical_formula_sum 'C18 H19 N O2' _chemical_formula_weight 281.34 _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' 0.0033 0.0016 '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' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.46160(10) _cell_length_b 10.9738(2) _cell_length_c 20.6916(5) _cell_angle_alpha 90 _cell_angle_beta 98.3310(10) _cell_angle_gamma 90 _cell_volume 1451.72(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2553 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.59 _cell_measurement_theta_min 2.72 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.5970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0734 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.8008. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.293 _exptl_crystal_size_min 0.171 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_unetI/netI 0.0365 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 12091 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.160 _diffrn_reflns_theta_min 1.989 _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker area detector' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2481 _reflns_number_total 3224 _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 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'Bruker Apex suite' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.464 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.045 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 195 _refine_ls_number_reflns 3224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0439 _refine_ls_restrained_S_all 1.026 _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^)+(0.0493P)^2^+0.4964P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1014 _refine_ls_wR_factor_ref 0.1104 _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: C11(H11) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B) 2.c Aromatic/amide H refined with riding coordinates: C5(H5), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) 2.d Idealised Me refined as rotating group: C10(H10A,H10B,H10C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _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 O1 O 1.04624(16) 0.34515(10) 0.23381(5) 0.0216(3) Uani 1 1 d . . . . . O2 O 0.73969(16) 0.62787(9) 0.25501(5) 0.0214(3) Uani 1 1 d . . . . . N1 N 0.76698(19) 0.52436(11) 0.15990(6) 0.0200(3) Uani 1 1 d . . . . . C1 C 0.8901(3) 0.60910(15) 0.12627(8) 0.0251(4) Uani 1 1 d . . . . . H1A H 0.9351 0.6807 0.1539 0.030 Uiso 1 1 calc R . . . . H1B H 0.8104 0.6373 0.0845 0.030 Uiso 1 1 calc R . . . . C2 C 1.0766(3) 0.53062(15) 0.11490(8) 0.0275(4) Uani 1 1 d . . . . . H2A H 1.1840 0.5290 0.1542 0.033 Uiso 1 1 calc R . . . . H2B H 1.1409 0.5614 0.0775 0.033 Uiso 1 1 calc R . . . . C3 C 0.9816(3) 0.40380(15) 0.10039(8) 0.0251(4) Uani 1 1 d . . . . . H3A H 1.0854 0.3396 0.1150 0.030 Uiso 1 1 calc R . . . . H3B H 0.9342 0.3938 0.0530 0.030 Uiso 1 1 calc R . . . . C4 C 0.7934(2) 0.39634(14) 0.13908(7) 0.0191(3) Uani 1 1 d . . . . . C5 C 0.6008(2) 0.34875(15) 0.09648(7) 0.0226(3) Uani 1 1 d . . . . . H5 H 0.5274 0.4015 0.0647 0.027 Uiso 1 1 calc R . . . . C6 C 0.5291(2) 0.23495(15) 0.10166(8) 0.0230(4) Uani 1 1 d . . . . . C7 C 0.6314(2) 0.15495(15) 0.15355(8) 0.0228(3) Uani 1 1 d . . . . . H7 H 0.5955 0.0710 0.1528 0.027 Uiso 1 1 calc R . . . . C8 C 0.7726(2) 0.19647(14) 0.20148(8) 0.0205(3) Uani 1 1 d . . . . . H8 H 0.8362 0.1415 0.2339 0.025 Uiso 1 1 calc R . . . . C9 C 0.8337(2) 0.32826(14) 0.20545(7) 0.0176(3) Uani 1 1 d . . . . . C10 C 0.3507(3) 0.18209(16) 0.05615(8) 0.0294(4) Uani 1 1 d . . . . . H10A H 0.2897 0.2451 0.0256 0.044 Uiso 1 1 calc GR . . . . H10B H 0.2441 0.1519 0.0813 0.044 Uiso 1 1 calc GR . . . . H10C H 0.4015 0.1146 0.0316 0.044 Uiso 1 1 calc GR . . . . C11 C 0.6954(2) 0.40522(13) 0.24647(7) 0.0169(3) Uani 1 1 d . . . . . H11 H 0.5456 0.3848 0.2309 0.020 Uiso 1 1 calc R . . . . C12 C 0.7359(2) 0.53350(14) 0.22294(7) 0.0183(3) Uani 1 1 d . . . . . C13 C 0.7352(2) 0.38537(13) 0.31913(7) 0.0182(3) Uani 1 1 d . . . . . C14 C 0.9142(2) 0.43103(14) 0.35736(7) 0.0213(3) Uani 1 1 d . . . . . H14 H 1.0120 0.4775 0.3375 0.026 Uiso 1 1 calc R . . . . C15 C 0.9506(3) 0.40909(15) 0.42411(8) 0.0251(4) Uani 1 1 d . . . . . H15 H 1.0730 0.4406 0.4496 0.030 Uiso 1 1 calc R . . . . C16 C 0.8096(3) 0.34161(15) 0.45379(8) 0.0282(4) Uani 1 1 d . . . . . H16 H 0.8345 0.3269 0.4995 0.034 Uiso 1 1 calc R . . . . C17 C 0.6321(3) 0.29590(16) 0.41627(8) 0.0284(4) Uani 1 1 d . . . . . H17 H 0.5346 0.2496 0.4364 0.034 Uiso 1 1 calc R . . . . C18 C 0.5952(2) 0.31717(14) 0.34940(8) 0.0229(3) Uani 1 1 d . . . . . H18 H 0.4731 0.2848 0.3241 0.028 Uiso 1 1 calc R . . . . H1 H 1.111(3) 0.271(2) 0.2366(10) 0.046(6) Uiso 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 O1 0.0181(5) 0.0180(6) 0.0275(6) -0.0025(5) -0.0006(4) 0.0001(4) O2 0.0225(5) 0.0154(6) 0.0258(6) -0.0026(4) 0.0019(4) 0.0002(4) N1 0.0246(6) 0.0154(6) 0.0198(7) 0.0013(5) 0.0029(5) -0.0019(5) C1 0.0324(9) 0.0206(8) 0.0221(8) 0.0046(6) 0.0028(7) -0.0068(7) C2 0.0308(9) 0.0276(9) 0.0255(9) -0.0002(7) 0.0087(7) -0.0081(7) C3 0.0292(8) 0.0263(9) 0.0210(8) -0.0030(7) 0.0079(7) -0.0052(7) C4 0.0233(7) 0.0161(8) 0.0180(8) -0.0018(6) 0.0033(6) -0.0028(6) C5 0.0248(8) 0.0259(9) 0.0167(8) -0.0014(6) 0.0014(6) -0.0003(6) C6 0.0226(8) 0.0257(9) 0.0214(8) -0.0078(6) 0.0058(6) -0.0035(6) C7 0.0247(8) 0.0166(8) 0.0286(8) -0.0039(6) 0.0090(7) -0.0039(6) C8 0.0220(7) 0.0151(7) 0.0248(8) -0.0004(6) 0.0053(6) 0.0018(6) C9 0.0175(7) 0.0166(7) 0.0183(7) -0.0010(6) 0.0008(6) -0.0012(6) C10 0.0281(8) 0.0321(10) 0.0277(9) -0.0078(7) 0.0024(7) -0.0057(7) C11 0.0175(7) 0.0144(7) 0.0184(7) -0.0009(6) 0.0010(6) -0.0014(5) C12 0.0155(7) 0.0177(8) 0.0203(8) 0.0011(6) -0.0018(6) 0.0011(6) C13 0.0227(7) 0.0145(7) 0.0176(7) -0.0007(6) 0.0031(6) 0.0024(6) C14 0.0243(8) 0.0171(8) 0.0221(8) -0.0009(6) 0.0018(6) 0.0002(6) C15 0.0308(8) 0.0205(8) 0.0220(8) -0.0031(7) -0.0035(7) 0.0012(6) C16 0.0446(10) 0.0230(9) 0.0164(8) 0.0000(6) 0.0029(7) 0.0046(7) C17 0.0389(10) 0.0242(9) 0.0239(9) 0.0007(7) 0.0108(7) -0.0043(7) C18 0.0264(8) 0.0198(8) 0.0228(8) -0.0033(6) 0.0043(6) -0.0030(6) _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 C9 1.4251(17) . ? O1 H1 0.91(2) . ? O2 C12 1.2282(18) . ? N1 C1 1.4637(19) . ? N1 C4 1.4864(19) . ? N1 C12 1.3520(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.527(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.533(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.552(2) . ? C4 C5 1.510(2) . ? C4 C9 1.552(2) . ? C5 H5 0.9500 . ? C5 C6 1.342(2) . ? C6 C7 1.468(2) . ? C6 C10 1.496(2) . ? C7 H7 0.9500 . ? C7 C8 1.327(2) . ? C8 H8 0.9500 . ? C8 C9 1.498(2) . ? C9 C11 1.566(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 1.0000 . ? C11 C12 1.524(2) . ? C11 C13 1.504(2) . ? C13 C14 1.396(2) . ? C13 C18 1.391(2) . ? C14 H14 0.9500 . ? C14 C15 1.388(2) . ? C15 H15 0.9500 . ? C15 C16 1.385(2) . ? C16 H16 0.9500 . ? C16 C17 1.383(2) . ? C17 H17 0.9500 . ? C17 C18 1.389(2) . ? C18 H18 0.9500 . ? 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 C9 O1 H1 108.3(13) . . ? C1 N1 C4 111.69(12) . . ? C12 N1 C1 125.35(13) . . ? C12 N1 C4 112.90(12) . . ? N1 C1 H1A 111.3 . . ? N1 C1 H1B 111.3 . . ? N1 C1 C2 102.14(13) . . ? H1A C1 H1B 109.2 . . ? C2 C1 H1A 111.3 . . ? C2 C1 H1B 111.3 . . ? C1 C2 H2A 111.0 . . ? C1 C2 H2B 111.0 . . ? C1 C2 C3 103.87(13) . . ? H2A C2 H2B 109.0 . . ? C3 C2 H2A 111.0 . . ? C3 C2 H2B 111.0 . . ? C2 C3 H3A 110.6 . . ? C2 C3 H3B 110.6 . . ? C2 C3 C4 105.57(13) . . ? H3A C3 H3B 108.8 . . ? C4 C3 H3A 110.6 . . ? C4 C3 H3B 110.6 . . ? N1 C4 C3 103.35(12) . . ? N1 C4 C5 112.13(12) . . ? N1 C4 C9 102.13(11) . . ? C3 C4 C9 115.98(13) . . ? C5 C4 C3 110.98(12) . . ? C5 C4 C9 111.64(12) . . ? C4 C5 H5 118.7 . . ? C6 C5 C4 122.68(15) . . ? C6 C5 H5 118.7 . . ? C5 C6 C7 119.42(14) . . ? C5 C6 C10 123.64(16) . . ? C7 C6 C10 116.92(14) . . ? C6 C7 H7 119.0 . . ? C8 C7 C6 121.94(15) . . ? C8 C7 H7 119.0 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.32(15) . . ? C9 C8 H8 119.3 . . ? O1 C9 C4 109.28(12) . . ? O1 C9 C8 112.26(12) . . ? O1 C9 C11 107.35(11) . . ? C4 C9 C11 100.60(11) . . ? C8 C9 C4 114.01(12) . . ? C8 C9 C11 112.57(12) . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11 107.9 . . ? C12 C11 C9 100.79(11) . . ? C12 C11 H11 107.9 . . ? C13 C11 C9 115.80(12) . . ? C13 C11 H11 107.9 . . ? C13 C11 C12 116.14(12) . . ? O2 C12 N1 126.13(14) . . ? O2 C12 C11 126.66(14) . . ? N1 C12 C11 107.21(12) . . ? C14 C13 C11 121.46(13) . . ? C18 C13 C11 119.99(13) . . ? C18 C13 C14 118.52(14) . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.54(15) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.45(15) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 120.3 . . ? C17 C16 C15 119.37(15) . . ? C17 C16 H16 120.3 . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.46(15) . . ? C18 C17 H17 119.8 . . ? C13 C18 H18 119.7 . . ? C17 C18 C13 120.65(15) . . ? C17 C18 H18 119.7 . . ? _shelx_res_file ; TITL testm1_a.res in P2(1)/c REM Old TITL testm1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.122, Rweak 0.005, Alpha 0.022, Orientation as input REM Formula found by SHELXT: C18 N O2 CELL 0.71073 6.4616 10.9738 20.6916 90 98.331 90 ZERR 4 0.0001 0.0002 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 76 4 8 L.S. 4 PLAN 5 TEMP -173.23 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.049300 0.496400 FVAR 0.72897 O1 4 1.046244 0.345149 0.233812 11.00000 0.01809 0.01800 = 0.02753 -0.00246 -0.00064 0.00009 O2 4 0.739694 0.627873 0.255007 11.00000 0.02255 0.01539 = 0.02577 -0.00263 0.00194 0.00022 N1 3 0.766981 0.524355 0.159903 11.00000 0.02455 0.01541 = 0.01985 0.00128 0.00292 -0.00188 C1 1 0.890102 0.609097 0.126266 11.00000 0.03238 0.02059 = 0.02205 0.00461 0.00282 -0.00681 AFIX 23 H1A 2 0.935143 0.680660 0.153898 11.00000 -1.20000 H1B 2 0.810367 0.637263 0.084461 11.00000 -1.20000 AFIX 0 C2 1 1.076570 0.530620 0.114898 11.00000 0.03076 0.02762 = 0.02549 -0.00016 0.00871 -0.00811 AFIX 23 H2A 2 1.183962 0.529040 0.154216 11.00000 -1.20000 H2B 2 1.140871 0.561406 0.077461 11.00000 -1.20000 AFIX 0 C3 1 0.981566 0.403804 0.100391 11.00000 0.02924 0.02634 = 0.02104 -0.00303 0.00791 -0.00522 AFIX 23 H3A 2 1.085434 0.339551 0.114988 11.00000 -1.20000 H3B 2 0.934233 0.393780 0.053005 11.00000 -1.20000 AFIX 0 C4 1 0.793354 0.396337 0.139082 11.00000 0.02329 0.01615 = 0.01797 -0.00178 0.00333 -0.00283 C5 1 0.600790 0.348750 0.096475 11.00000 0.02475 0.02590 = 0.01665 -0.00140 0.00143 -0.00032 AFIX 43 H5 2 0.527401 0.401546 0.064700 11.00000 -1.20000 AFIX 0 C6 1 0.529123 0.234952 0.101665 11.00000 0.02259 0.02570 = 0.02136 -0.00782 0.00584 -0.00349 C7 1 0.631401 0.154947 0.153552 11.00000 0.02474 0.01657 = 0.02859 -0.00387 0.00904 -0.00391 AFIX 43 H7 2 0.595465 0.070963 0.152803 11.00000 -1.20000 AFIX 0 C8 1 0.772584 0.196472 0.201476 11.00000 0.02198 0.01515 = 0.02483 -0.00035 0.00532 0.00178 AFIX 43 H8 2 0.836153 0.141544 0.233908 11.00000 -1.20000 AFIX 0 C9 1 0.833726 0.328256 0.205455 11.00000 0.01753 0.01662 = 0.01825 -0.00101 0.00078 -0.00119 C10 1 0.350705 0.182089 0.056147 11.00000 0.02808 0.03208 = 0.02765 -0.00776 0.00239 -0.00566 AFIX 137 H10A 2 0.289684 0.245120 0.025633 11.00000 -1.50000 H10B 2 0.244089 0.151869 0.081341 11.00000 -1.50000 H10C 2 0.401464 0.114649 0.031650 11.00000 -1.50000 AFIX 0 C11 1 0.695416 0.405222 0.246467 11.00000 0.01755 0.01438 = 0.01835 -0.00092 0.00095 -0.00142 AFIX 13 H11 2 0.545639 0.384839 0.230911 11.00000 -1.20000 AFIX 0 C12 1 0.735903 0.533499 0.222945 11.00000 0.01554 0.01765 = 0.02029 0.00106 -0.00176 0.00112 C13 1 0.735205 0.385370 0.319130 11.00000 0.02271 0.01445 = 0.01760 -0.00069 0.00314 0.00245 C14 1 0.914246 0.431033 0.357365 11.00000 0.02435 0.01709 = 0.02208 -0.00087 0.00185 0.00019 AFIX 43 H14 2 1.011990 0.477500 0.337529 11.00000 -1.20000 AFIX 0 C15 1 0.950564 0.409087 0.424111 11.00000 0.03076 0.02046 = 0.02198 -0.00311 -0.00353 0.00125 AFIX 43 H15 2 1.072987 0.440571 0.449607 11.00000 -1.20000 AFIX 0 C16 1 0.809554 0.341606 0.453793 11.00000 0.04459 0.02305 = 0.01641 0.00003 0.00288 0.00456 AFIX 43 H16 2 0.834547 0.326860 0.499501 11.00000 -1.20000 AFIX 0 C17 1 0.632051 0.295898 0.416273 11.00000 0.03892 0.02423 = 0.02389 0.00074 0.01079 -0.00429 AFIX 43 H17 2 0.534642 0.249628 0.436357 11.00000 -1.20000 AFIX 0 C18 1 0.595163 0.317171 0.349400 11.00000 0.02643 0.01976 = 0.02283 -0.00330 0.00428 -0.00299 AFIX 43 H18 2 0.473105 0.284826 0.324095 11.00000 -1.20000 AFIX 0 H1 2 1.111003 0.270804 0.236597 11.00000 0.04636 HKLF 4 REM testm1_a.res in P2(1)/c REM R1 = 0.0439 for 2481 Fo > 4sig(Fo) and 0.0620 for all 3224 data REM 195 parameters refined using 0 restraints END WGHT 0.0493 0.4964 REM Highest difference peak 0.464, deepest hole -0.220, 1-sigma level 0.045 Q1 1 0.8176 0.1415 0.1328 11.00000 0.05 0.46 Q2 1 0.8119 0.3569 0.1692 11.00000 0.05 0.29 Q3 1 0.7902 0.2660 0.2026 11.00000 0.05 0.26 Q4 1 0.7155 0.3980 0.2819 11.00000 0.05 0.25 Q5 1 0.7025 0.3637 0.1203 11.00000 0.05 0.23 ; _shelx_res_checksum 76798 _shelx_hkl_file ; 1 0 0 1230.38 17.80 1 0 0 1219.18 17.60 1 0 0 1237.38 18.20 2 0 0 948.01 17.30 2 0 0 955.90 16.30 2 0 0 956.10 16.50 3 0 0 198.18 7.10 3 0 0 181.88 7.00 3 0 0 200.68 8.00 4 0 0 213.18 8.70 4 0 0 193.08 8.30 4 0 0 208.08 10.00 5 0 0 79.89 8.30 5 0 0 75.29 7.00 5 0 0 71.89 6.70 6 0 0 285.07 13.90 6 0 0 273.77 12.10 6 0 0 277.57 12.70 7 0 0 87.29 9.40 8 0 0 23.10 6.40 0 -1 0 0.10 0.40 0 1 0 0.40 0.30 1 -1 0 3817.12 49.99 1 -1 0 3728.33 50.19 1 -1 0 3742.73 52.59 1 -1 0 3810.22 51.29 -1 -1 0 3723.83 52.59 1 1 0 3717.93 52.29 2 -1 0 401.26 9.70 -2 -1 0 401.36 6.90 2 -1 0 399.06 8.70 2 -1 0 389.66 9.70 2 1 0 408.56 8.70 -2 1 0 407.86 6.70 2 1 0 393.86 9.30 3 -1 0 171.08 7.40 3 -1 0 163.68 6.30 3 -1 0 170.88 7.20 -3 -1 0 170.58 3.30 3 1 0 172.88 6.40 3 1 0 169.28 7.60 -3 1 0 167.18 3.60 3 1 0 165.28 6.90 4 -1 0 797.72 17.50 4 -1 0 787.72 19.40 4 -1 0 775.52 18.20 4 1 0 771.12 17.20 4 1 0 753.52 18.00 5 -1 0 11.70 4.70 5 -1 0 15.40 4.20 5 -1 0 18.70 4.70 5 1 0 20.60 4.80 5 1 0 10.40 3.60 6 -1 0 66.99 7.50 6 -1 0 55.39 8.00 6 1 0 59.09 7.50 6 1 0 66.19 7.00 7 -1 0 5.60 5.40 7 -1 0 5.70 4.10 7 1 0 7.60 4.90 -7 1 0 7.10 3.70 8 -1 0 3.60 4.60 8 1 0 6.70 5.10 0 -2 0 219.28 5.30 0 2 0 218.08 4.90 -1 -2 0 3578.24 48.20 1 -2 0 3589.14 50.89 -1 2 0 3671.53 49.20 2 -2 0 143.39 6.10 2 -2 0 151.68 6.10 2 -2 0 145.39 4.50 2 -2 0 148.69 4.90 -2 -2 0 151.08 4.50 2 2 0 147.29 5.60 -2 2 0 151.98 5.50 3 -2 0 27.70 3.80 -3 -2 0 32.40 2.60 3 -2 0 32.30 3.30 3 -2 0 32.80 2.30 3 -2 0 32.20 4.20 3 2 0 26.70 3.50 3 2 0 29.80 3.30 -3 2 0 28.30 2.30 4 -2 0 241.38 10.00 4 -2 0 236.18 10.30 4 -2 0 236.68 8.80 -4 -2 0 237.98 5.40 4 2 0 236.38 9.60 4 2 0 233.18 8.40 -4 2 0 243.08 5.50 5 -2 0 150.48 8.40 5 -2 0 158.48 9.80 5 2 0 161.68 8.20 5 2 0 147.79 8.90 -5 2 0 148.59 8.00 6 -2 0 115.79 8.60 6 -2 0 149.59 10.70 -6 2 0 140.29 8.40 6 2 0 136.89 9.50 6 2 0 137.09 8.20 7 -2 0 -2.70 4.60 7 -2 0 10.70 4.60 7 2 0 4.20 4.20 -7 2 0 -1.10 2.90 8 -2 0 1.60 5.80 8 -2 0 6.30 5.00 8 2 0 -0.10 4.90 0 -3 0 0.10 1.70 0 3 0 1.40 1.30 -1 -3 0 77.39 4.20 1 -3 0 72.89 4.10 -1 3 0 75.09 4.00 -2 -3 0 158.68 5.40 2 -3 0 163.18 4.90 2 -3 0 160.48 5.50 2 -3 0 161.48 6.30 2 3 0 167.48 6.20 -2 3 0 161.98 6.20 3 -3 0 173.18 7.60 -3 -3 0 160.18 5.70 3 -3 0 156.18 5.50 3 -3 0 165.28 6.00 3 3 0 163.38 7.20 3 3 0 160.88 6.00 -3 3 0 147.79 6.70 3 3 0 161.38 5.60 -4 -3 0 248.68 7.30 4 -3 0 267.27 11.30 4 -3 0 256.97 9.20 4 3 0 246.08 8.60 -4 3 0 256.57 9.80 4 3 0 250.57 10.60 5 -3 0 1.10 3.00 -5 -3 0 0.60 1.50 5 -3 0 0.60 3.80 -5 3 0 -2.60 2.70 5 3 0 -5.80 2.60 5 3 0 3.30 2.90 6 -3 0 34.30 5.50 6 -3 0 46.70 7.60 -6 3 0 38.70 5.50 6 3 0 25.60 5.50 7 -3 0 62.79 7.90 7 -3 0 63.89 9.50 7 3 0 63.69 8.60 -7 3 0 54.39 7.10 8 -3 0 6.40 6.60 8 -3 0 8.50 4.80 8 3 0 11.50 5.90 0 -4 0 5739.63 77.39 0 4 0 5604.14 76.19 1 -4 0 718.93 14.60 -1 -4 0 716.33 14.60 -1 4 0 728.33 14.80 2 -4 0 101.19 5.00 -2 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-1 -1 24.10 5.40 6 -1 -1 17.10 5.60 6 -1 -1 29.80 5.80 -6 1 1 19.00 4.00 6 1 -1 18.00 4.60 6 1 -1 18.40 5.10 5 -1 -1 80.99 8.50 5 -1 -1 97.09 7.40 5 -1 -1 104.69 7.80 5 1 -1 101.69 7.20 5 1 -1 85.89 7.70 -5 1 1 92.99 6.10 4 -1 -1 47.80 4.80 4 -1 -1 38.40 5.10 4 -1 -1 40.90 5.60 4 1 -1 36.80 4.60 4 1 -1 47.10 5.00 3 -1 -1 477.55 12.40 3 -1 -1 476.25 11.40 3 -1 -1 479.35 12.70 3 1 -1 470.85 11.60 3 1 -1 479.35 11.90 -3 1 1 459.55 7.00 -3 1 1 469.75 7.30 2 -1 -1 10.50 2.30 -2 -1 1 7.20 1.00 2 -1 -1 3.70 2.00 2 -1 -1 7.90 2.00 -2 1 1 8.10 1.10 2 1 -1 6.20 1.90 2 1 -1 5.30 2.00 1 -1 -1 4098.29 57.79 1 -1 -1 4053.69 58.99 1 -1 -1 4090.09 58.09 1 -1 -1 4012.10 57.59 -1 -1 1 4038.40 57.89 -1 1 1 4145.99 61.59 1 1 -1 4062.19 59.59 0 -1 -1 59.79 1.60 0 -1 1 61.99 1.90 0 -1 -1 60.69 2.00 0 1 1 62.09 1.60 1 -1 1 9999.00 133.59 1 -1 1 9946.80 141.69 1 -1 1 9903.21 135.39 -1 -1 -1 9683.83 136.79 1 1 1 9906.51 136.59 1 1 1 9960.70 131.69 2 -1 1 10.10 1.30 2 -1 1 13.20 2.50 2 -1 1 12.30 2.10 -2 -1 -1 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5 23.30 6.90 -7 5 -5 28.30 6.60 7 -6 -5 10.60 5.90 -7 6 5 20.80 6.30 7 6 -5 4.10 4.60 6 -6 -5 11.50 5.10 -6 6 5 8.70 4.40 6 6 -5 9.90 5.10 5 -6 -5 -0.90 3.60 -5 -6 5 0.60 2.60 5 -6 -5 3.30 4.20 5 6 -5 4.00 4.00 -5 6 5 5.80 3.80 -5 6 5 -2.50 3.50 4 -6 -5 113.49 10.00 4 -6 -5 104.59 7.90 -4 -6 5 109.39 7.00 4 6 -5 118.49 7.90 -4 6 5 105.29 8.10 -4 6 5 116.99 8.40 3 -6 -5 3.30 3.40 3 -6 -5 1.00 2.80 -3 -6 5 -3.50 2.70 3 -6 -5 -0.90 3.00 -3 6 5 2.90 3.50 -3 6 5 1.70 4.00 3 6 -5 1.30 2.70 2 -6 -5 1121.39 23.80 2 -6 -5 1104.69 23.70 -2 -6 5 1126.69 23.30 -2 6 5 1175.68 25.00 2 6 -5 1137.39 21.20 -2 6 5 1120.69 24.50 -1 -6 5 29.70 4.60 1 -6 -5 24.10 4.60 1 6 -5 27.80 3.20 -1 6 5 30.50 5.10 1 6 -5 27.20 2.90 0 -6 5 -0.80 3.20 0 -6 -5 2.80 3.30 0 6 -5 3.40 1.10 0 6 -5 4.40 2.10 0 6 5 -1.30 3.00 1 -6 5 14.30 3.90 -1 -6 -5 9.60 3.60 -1 6 -5 9.40 2.90 1 6 5 7.80 3.80 -2 -6 -5 31.10 5.10 2 -6 5 32.60 5.20 2 6 5 29.30 5.30 -2 6 -5 24.80 4.30 -3 -6 -5 187.68 10.10 3 -6 5 182.18 9.70 3 -6 5 190.58 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360.06 13.30 1 -7 5 361.46 13.00 -1 7 -5 376.76 12.40 1 7 5 338.47 13.50 -2 -7 -5 3.80 4.20 2 -7 5 3.10 3.50 2 7 5 -0.60 4.60 -2 7 -5 11.20 3.60 -3 -7 -5 20.10 5.10 3 -7 5 21.50 4.80 -3 7 -5 15.70 4.40 3 7 5 22.80 5.80 4 -7 5 4.60 4.30 -4 -7 -5 1.40 3.70 -4 7 -5 0.60 3.20 -5 -7 -5 0.20 3.50 5 -7 5 3.80 4.50 -5 7 -5 -1.20 3.50 5 7 5 0.20 4.00 6 -7 5 15.20 6.00 6 7 5 3.00 5.00 -6 7 -5 4.10 4.00 6 -8 -5 2.80 4.60 -6 -8 5 7.00 6.00 -6 8 5 0.60 4.50 6 8 -5 6.10 5.00 -6 8 5 5.00 4.90 -5 -8 5 29.50 5.30 5 -8 -5 22.40 5.60 5 8 -5 31.90 6.60 -5 8 5 35.60 7.20 -5 8 5 24.00 6.20 4 -8 -5 28.90 5.30 -4 -8 5 33.40 5.60 -4 8 5 25.00 5.90 4 8 -5 33.70 5.60 -4 8 5 24.00 5.70 3 -8 -5 393.26 14.80 3 -8 -5 403.76 13.60 -3 -8 5 398.46 14.20 -3 8 5 408.66 16.10 -3 8 5 422.26 16.10 3 8 -5 407.16 13.20 -2 -8 5 2.90 3.80 2 -8 -5 5.20 4.10 -2 8 5 4.40 4.20 2 8 -5 0.40 2.50 1 -8 -5 5.00 4.00 -1 -8 5 0.80 3.90 1 8 -5 3.40 2.80 1 8 -5 -1.60 1.80 0 -8 -5 125.39 9.10 0 -8 5 120.49 8.50 0 8 5 131.59 9.80 0 8 -5 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0 9 -5 94.79 7.10 0 9 5 94.09 9.70 -1 -9 -5 337.37 14.40 1 -9 5 304.57 13.50 1 9 5 319.67 14.80 -1 9 -5 309.57 12.60 2 -9 5 26.80 5.80 -2 -9 -5 30.30 6.10 -2 9 -5 28.30 5.60 2 9 5 22.10 6.30 -3 -9 -5 60.39 7.70 3 -9 5 61.79 7.90 -3 9 -5 63.69 7.80 3 9 5 50.79 8.90 -4 -9 -5 46.40 7.30 4 -9 5 28.70 6.00 -4 9 -5 28.80 6.20 -5 -9 -5 66.49 8.80 5 -9 5 60.69 9.10 5 9 5 70.99 9.40 -5 9 -5 82.89 9.90 -5 -10 5 2.90 4.60 5 -10 -5 2.40 4.40 5 10 -5 -5.50 4.00 -5 10 5 7.20 5.50 -5 10 5 8.40 5.70 4 -10 -5 147.39 9.90 -4 -10 5 154.38 10.70 -4 10 5 159.48 12.30 -4 10 5 175.58 13.10 4 10 -5 147.29 9.90 -3 -10 5 -0.40 3.80 3 -10 -5 5.40 3.40 3 -10 -5 0.30 4.10 3 10 -5 -0.80 3.30 -3 10 5 0.80 4.90 -3 10 5 -2.40 4.40 -2 -10 5 -1.90 3.80 2 -10 -5 -2.70 4.00 -2 10 5 -3.50 4.30 -1 -10 5 55.99 7.90 1 -10 -5 46.30 8.00 1 10 -5 60.69 6.70 0 -10 5 5.60 4.30 0 -10 -5 2.50 4.40 0 10 -5 -0.50 3.10 0 10 5 3.50 4.90 -1 -10 -5 30.50 6.60 1 -10 5 29.60 6.10 -1 10 -5 30.60 5.40 1 10 5 37.40 7.50 2 -10 5 187.28 12.00 -2 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5.70 4 -12 -5 4.80 4.50 -4 12 5 -4.10 6.40 -4 12 5 9.80 7.20 -3 -12 5 45.60 8.40 3 -12 -5 45.10 6.70 -3 12 5 27.50 8.20 -2 -12 5 0.30 5.80 2 -12 -5 -5.40 4.40 -2 12 5 -1.00 5.10 1 -12 -5 -3.90 4.70 -1 -12 5 1.60 5.60 -1 12 5 -5.40 4.70 0 -12 5 5.10 5.60 0 -12 -5 1.60 5.60 0 12 5 3.90 5.80 0 12 -5 4.80 4.30 1 -12 5 106.99 11.30 -1 -12 -5 102.79 11.90 1 12 5 96.39 12.10 -1 12 -5 125.09 11.30 2 -12 5 7.90 5.70 -2 -12 -5 3.30 5.20 2 12 5 8.80 6.00 -2 12 -5 3.90 4.00 -3 -12 -5 107.99 12.00 -3 12 -5 100.99 11.40 3 -13 -5 13.30 4.70 -2 -13 5 22.10 7.60 2 -13 -5 15.60 7.10 -2 13 5 16.40 8.30 1 -13 -5 9.60 6.60 -1 -13 5 9.10 6.20 -1 13 5 3.80 6.10 0 -13 5 70.89 10.20 0 -13 -5 53.19 9.50 0 13 5 72.09 11.10 0 13 -5 62.89 9.30 -1 -13 -5 123.59 13.80 1 -13 5 120.99 12.80 1 13 5 98.19 12.80 -1 13 -5 113.09 11.50 -2 -13 -5 5.40 6.90 2 -13 5 -2.50 5.40 -2 13 -5 -2.60 3.80 2 13 5 -0.50 7.40 8 0 -6 10.60 5.20 8 0 -6 0.30 4.40 7 0 -6 -1.70 4.00 7 0 -6 6.90 4.80 6 0 -6 0.10 3.60 6 0 -6 0.20 3.50 5 0 -6 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6.00 0 -5 24 54.09 9.60 0 -5 -24 47.30 10.20 0 5 -24 35.90 8.20 0 5 24 30.40 8.70 -1 -6 24 35.60 8.40 1 -6 -24 45.20 10.00 -1 6 24 54.79 11.10 -3 0 25 5.80 6.40 2 0 -25 -1.80 4.00 -2 0 25 -0.80 4.50 -1 0 25 0.90 5.20 1 0 -25 0.30 4.60 0 0 25 -0.20 6.10 0 0 -25 12.50 6.60 -1 0 -25 2.00 5.50 1 0 25 -2.20 5.30 -3 -1 25 9.90 6.50 -3 1 25 13.20 6.90 -2 -1 25 -3.60 4.40 2 -1 -25 5.20 5.60 -2 1 25 2.50 5.80 2 1 -25 2.00 4.70 -1 -1 25 19.60 6.80 1 -1 -25 16.40 7.30 1 1 -25 13.70 6.50 -1 1 25 19.20 7.60 0 -1 -25 1.10 5.20 0 -1 25 -0.80 5.20 0 1 25 6.70 5.90 0 1 -25 13.90 6.20 -1 -1 -25 65.89 11.90 1 -1 25 54.89 10.00 1 1 25 62.99 10.40 -1 1 -25 61.29 10.70 -3 -2 25 71.89 10.00 -3 2 25 50.59 8.80 -2 -2 25 26.50 7.50 2 -2 -25 31.50 8.10 2 2 -25 29.40 7.50 -2 2 25 21.60 6.90 -1 -2 25 66.69 10.10 1 -2 -25 68.59 11.00 -1 2 25 68.19 10.20 1 2 -25 66.39 10.40 0 -2 -25 4.70 5.60 0 -2 25 2.80 5.70 0 2 25 -1.70 5.00 0 2 -25 -1.80 4.40 -1 -2 -25 2.60 5.70 1 -2 25 9.80 6.50 -1 2 -25 1.50 5.30 1 2 25 8.20 6.40 -3 -3 25 3.80 6.30 -3 3 25 0.50 5.40 -2 -3 25 0.60 5.20 2 -3 -25 5.60 6.10 -2 3 25 -9.70 5.20 2 3 -25 5.10 4.90 1 -3 -25 46.30 9.40 -1 -3 25 47.30 9.00 -1 3 25 51.59 9.70 1 3 -25 74.69 10.90 0 -3 -25 54.39 10.50 0 -3 25 54.89 9.40 0 3 -25 26.90 7.60 0 3 25 33.90 8.40 1 -3 25 77.69 11.00 -1 -3 -25 96.69 13.70 -1 3 -25 98.89 13.00 1 3 25 89.29 12.20 -2 -4 25 28.70 7.40 2 -4 -25 50.89 9.60 2 4 -25 30.40 7.70 -2 4 25 39.10 8.90 -1 -4 25 22.80 7.10 1 -4 -25 38.10 9.40 1 4 -25 9.70 5.90 -1 4 25 10.80 7.90 0 -4 25 6.40 6.00 0 -4 -25 -0.50 5.50 0 4 25 7.10 6.90 0 4 -25 19.00 7.30 2 0 -26 5.10 5.40 -2 0 26 1.10 6.40 1 0 -26 2.60 5.40 -1 0 26 10.70 6.30 0 0 -26 9.40 6.20 0 0 26 0.30 5.50 2 -1 -26 99.49 12.50 -2 -1 26 91.89 11.40 2 1 -26 128.69 13.60 -2 1 26 76.79 11.00 -1 -1 26 4.60 5.90 1 -1 -26 21.10 7.50 -1 1 26 6.60 6.70 1 1 -26 9.50 6.30 0 -1 -26 16.20 7.10 0 -1 26 1.20 5.80 0 1 -26 9.60 6.10 0 1 26 23.00 7.50 -2 -2 26 8.00 6.10 2 -2 -26 -2.70 4.40 -2 2 26 -5.60 5.40 2 2 -26 -0.20 4.20 1 -2 -26 1.80 5.30 -1 -2 26 0.30 6.50 1 2 -26 3.30 4.90 -1 2 26 -9.80 4.90 0 -2 26 12.50 6.50 0 -2 -26 13.30 6.70 0 2 26 5.60 6.50 0 2 -26 20.70 7.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 81916 _olex2_submission_special_instructions 'No special instructions were received'