#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 12 _journal_issue 4 _journal_year 2021 _journal_page_first 394 _journal_page_last 400 #============================================================================== data_test10 _audit_creation_date 2021-08-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/1' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _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 AM60 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H24 N6' _chemical_formula_sum 'C34 H24 N6' _chemical_formula_weight 516.59 _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' _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 '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 10.885(3) _cell_length_b 11.134(3) _cell_length_c 12.870(3) _cell_angle_alpha 90.122(6) _cell_angle_beta 114.141(6) _cell_angle_gamma 110.277(5) _cell_volume 1316.1(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 999 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 19.64 _cell_measurement_theta_min 1.76 _shelx_estimated_absorpt_T_max 0.985 _shelx_estimated_absorpt_T_min 0.981 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABAS 2.10 (Bruker 2003)' _exptl_absorpt_special_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 540 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7309 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 19.638 _diffrn_reflns_theta_max 19.638 _diffrn_reflns_theta_min 1.759 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1525 _reflns_number_total 2318 _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 6.45 ( Bruker, 2003)' _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _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 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.144 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.038 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 457 _refine_ls_number_reflns 2318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0416 _refine_ls_restrained_S_all 1.000 _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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.1074 _refine_special_details ? _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary ? _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 C2 C 0.2756(4) 0.9386(4) 0.5748(3) 0.0326(10) Uani 1 1 d . . . . . C3 C 0.2645(4) 1.0114(4) 0.4889(4) 0.0399(11) Uani 1 1 d . . . . . C4 C 0.2102(4) 1.1111(4) 0.4837(3) 0.0349(10) Uani 1 1 d . . . . . C5 C 0.1981(5) 1.1912(4) 0.3975(4) 0.0436(12) Uani 1 1 d . . . . . C7 C 0.1024(5) 1.3025(5) 0.4837(4) 0.0497(13) Uani 1 1 d . . . . . C8 C 0.1137(5) 1.2283(4) 0.5684(4) 0.0448(12) Uani 1 1 d . . . . . C1 C 0.2300(4) 0.9660(4) 0.6581(4) 0.0389(11) Uani 1 1 d . . . . . H1 H 0.239(3) 0.911(3) 0.722(3) 0.034(11) Uiso 1 1 d . . . . . C6 C 0.1457(5) 1.2854(5) 0.3985(4) 0.0475(12) Uani 1 1 d . . . . . C9 C 0.1686(4) 1.1318(4) 0.5711(4) 0.0377(11) Uani 1 1 d . . . . . N1 N 0.1781(3) 1.0574(3) 0.6575(3) 0.0420(9) Uani 1 1 d . . . . . C10 C 0.3307(4) 0.8368(4) 0.5795(4) 0.0369(11) Uani 1 1 d . . . . . N2 N 0.3464(3) 0.7695(3) 0.6615(3) 0.0369(9) Uani 1 1 d . . . . . N3 N 0.3995(3) 0.6743(3) 0.6455(3) 0.0385(9) Uani 1 1 d . . . . . C12 C 0.4743(4) 0.5037(4) 0.7242(3) 0.0304(10) Uani 1 1 d . . . . . C11 C 0.4216(4) 0.6080(4) 0.7287(3) 0.0324(10) Uani 1 1 d . . . . . N4 N 1.1355(4) 0.9477(3) 1.1968(3) 0.0417(9) Uani 1 1 d . . . . . C14 C 0.8846(4) 0.8382(3) 1.0538(4) 0.0332(10) Uani 1 1 d . . . . . C16 C 1.0792(4) 0.8515(4) 1.0038(3) 0.0337(10) Uani 1 1 d . . . . . C17 C 1.1788(5) 0.9193(4) 1.1166(4) 0.0343(10) Uani 1 1 d . . . . . C13 C 0.9934(5) 0.9066(4) 1.1642(4) 0.0403(12) Uani 1 1 d . . . . . C15 C 0.9289(5) 0.8113(4) 0.9735(4) 0.0338(11) Uani 1 1 d . . . . . C20 C 1.2805(5) 0.8653(4) 0.9630(4) 0.0434(12) Uani 1 1 d . . . . . C21 C 1.1336(5) 0.8243(4) 0.9275(4) 0.0427(12) Uani 1 1 d . . . . . C18 C 1.3296(5) 0.9626(4) 1.1489(4) 0.0437(12) Uani 1 1 d . . . . . C19 C 1.3788(5) 0.9356(4) 1.0733(5) 0.0451(12) Uani 1 1 d . . . . . C22 C 0.7324(5) 0.7948(4) 1.0304(4) 0.0336(11) Uani 1 1 d . . . . . N6 N 0.4928(4) 0.6900(3) 0.9309(3) 0.0371(9) Uani 1 1 d . . . . . N5 N 0.6312(4) 0.7328(3) 0.9317(3) 0.0364(9) Uani 1 1 d . . . . . C23 C 0.2409(4) 0.5603(3) 0.8186(4) 0.0335(10) Uani 1 1 d . . . . . C24 C 0.1218(5) 0.5188(4) 0.7105(4) 0.0423(12) Uani 1 1 d . . . . . H24 H 0.133(3) 0.538(3) 0.641(3) 0.029(11) Uiso 1 1 d . . . . . C28 C 0.2175(5) 0.5321(4) 0.9152(4) 0.0434(12) Uani 1 1 d . . . . . C27 C 0.0786(6) 0.4642(4) 0.9042(6) 0.0556(14) Uani 1 1 d . . . . . H27 H 0.071(4) 0.443(3) 0.975(3) 0.053(14) Uiso 1 1 d . . . . . C26 C -0.0374(6) 0.4232(5) 0.7972(6) 0.0633(16) Uani 1 1 d . . . . . C25 C -0.0176(6) 0.4504(4) 0.6999(5) 0.0564(14) Uani 1 1 d . . . . . C29 C 0.4676(4) 0.4111(4) 0.7950(4) 0.0376(11) Uani 1 1 d . . . . . C33 C 0.5301(4) 0.4950(4) 0.6457(4) 0.0417(12) Uani 1 1 d . . . . . C31 C 0.5642(4) 0.3015(5) 0.7084(4) 0.0434(12) Uani 1 1 d . . . . . C32 C 0.5738(5) 0.3938(5) 0.6382(4) 0.0480(13) Uani 1 1 d . . . . . H32 H 0.604(4) 0.387(4) 0.581(3) 0.067(15) Uiso 1 1 d . . . . . C30 C 0.5122(4) 0.3110(4) 0.7871(4) 0.0431(12) Uani 1 1 d . . . . . C34 C 0.3913(4) 0.6277(4) 0.8306(4) 0.0306(10) Uani 1 1 d . . . . . H19 H 1.483(4) 0.966(3) 1.095(3) 0.038(11) Uiso 1 1 d . . . . . H5 H 0.238(3) 1.179(3) 0.342(3) 0.037(12) Uiso 1 1 d . . . . . H31 H 0.592(4) 0.229(3) 0.701(3) 0.048(13) Uiso 1 1 d . . . . . H33 H 0.535(3) 0.559(3) 0.596(3) 0.021(10) Uiso 1 1 d . . . . . H30 H 0.509(3) 0.251(3) 0.838(3) 0.037(12) Uiso 1 1 d . . . . . H3 H 0.296(3) 0.996(3) 0.430(3) 0.040(12) Uiso 1 1 d . . . . . H8 H 0.086(4) 1.239(3) 0.628(3) 0.055(14) Uiso 1 1 d . . . . . H15 H 0.857(3) 0.764(3) 0.895(3) 0.021(10) Uiso 1 1 d . . . . . H21 H 1.059(4) 0.773(3) 0.847(3) 0.048(12) Uiso 1 1 d . . . . . H28 H 0.299(4) 0.560(3) 0.989(3) 0.040(12) Uiso 1 1 d . . . . . H6 H 0.139(4) 1.341(3) 0.338(3) 0.058(14) Uiso 1 1 d . . . . . H26 H -0.129(5) 0.377(4) 0.789(3) 0.069(16) Uiso 1 1 d . . . . . H10 H 0.366(3) 0.822(3) 0.515(3) 0.048(11) Uiso 1 1 d . . . . . H29 H 0.430(3) 0.415(3) 0.851(3) 0.041(12) Uiso 1 1 d . . . . . H13 H 0.960(3) 0.920(3) 1.219(3) 0.030(11) Uiso 1 1 d . . . . . H18 H 1.392(4) 1.008(3) 1.225(3) 0.054(14) Uiso 1 1 d . . . . . H7 H 0.066(4) 1.367(3) 0.485(3) 0.048(13) Uiso 1 1 d . . . . . H20 H 1.318(4) 0.848(3) 0.909(3) 0.048(13) Uiso 1 1 d . . . . . H25 H -0.101(4) 0.421(3) 0.619(3) 0.058(13) Uiso 1 1 d . . . . . H22 H 0.709(3) 0.808(3) 1.091(3) 0.034(12) 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 C2 0.037(3) 0.037(3) 0.031(3) 0.010(2) 0.015(2) 0.020(2) C3 0.043(3) 0.040(3) 0.036(3) 0.004(3) 0.015(2) 0.019(2) C4 0.034(3) 0.036(3) 0.030(3) 0.009(2) 0.010(2) 0.014(2) C5 0.046(3) 0.041(3) 0.035(3) 0.003(3) 0.012(2) 0.015(3) C7 0.052(3) 0.041(3) 0.050(4) 0.000(3) 0.009(3) 0.027(3) C8 0.048(3) 0.044(3) 0.043(3) 0.004(3) 0.014(3) 0.024(3) C1 0.041(3) 0.041(3) 0.034(3) 0.011(3) 0.013(2) 0.019(2) C6 0.053(3) 0.040(3) 0.040(3) 0.006(3) 0.011(3) 0.019(3) C9 0.037(3) 0.040(3) 0.030(3) 0.000(2) 0.009(2) 0.014(2) N1 0.042(2) 0.049(2) 0.034(2) 0.010(2) 0.0143(18) 0.019(2) C10 0.036(3) 0.039(3) 0.033(3) 0.008(2) 0.012(2) 0.014(2) N2 0.041(2) 0.037(2) 0.040(2) 0.0052(19) 0.0180(18) 0.0218(19) N3 0.042(2) 0.042(2) 0.036(2) 0.0106(19) 0.0183(18) 0.0195(19) C12 0.031(3) 0.041(3) 0.025(2) 0.006(2) 0.015(2) 0.017(2) C11 0.025(3) 0.035(3) 0.035(3) 0.003(2) 0.014(2) 0.009(2) N4 0.037(3) 0.048(2) 0.038(2) 0.0080(17) 0.016(2) 0.014(2) C14 0.040(3) 0.034(3) 0.030(3) 0.007(2) 0.015(3) 0.018(2) C16 0.031(3) 0.037(3) 0.035(3) 0.008(2) 0.015(3) 0.015(2) C17 0.027(3) 0.036(3) 0.040(3) 0.011(2) 0.014(3) 0.013(2) C13 0.045(4) 0.048(3) 0.037(3) 0.010(2) 0.024(3) 0.020(3) C15 0.034(3) 0.036(3) 0.029(3) 0.004(2) 0.012(3) 0.012(2) C20 0.045(4) 0.048(3) 0.050(4) 0.015(3) 0.030(3) 0.022(3) C21 0.033(3) 0.051(3) 0.043(3) 0.002(2) 0.017(3) 0.014(3) C18 0.036(4) 0.044(3) 0.040(3) 0.015(3) 0.009(3) 0.012(3) C19 0.032(3) 0.049(3) 0.063(4) 0.025(3) 0.025(3) 0.020(3) C22 0.028(3) 0.044(3) 0.034(3) 0.008(2) 0.017(3) 0.016(2) N6 0.028(2) 0.048(2) 0.042(2) 0.0087(19) 0.019(2) 0.0172(19) N5 0.027(2) 0.050(2) 0.033(2) 0.0056(19) 0.013(2) 0.0157(19) C23 0.032(3) 0.037(3) 0.042(3) 0.011(2) 0.020(3) 0.019(2) C24 0.033(3) 0.051(3) 0.047(4) 0.011(3) 0.022(3) 0.016(3) C28 0.038(4) 0.052(3) 0.049(4) 0.015(3) 0.024(3) 0.021(3) C27 0.053(4) 0.056(3) 0.087(5) 0.035(3) 0.051(4) 0.029(3) C26 0.033(4) 0.049(4) 0.111(6) 0.029(4) 0.032(4) 0.019(3) C25 0.046(4) 0.056(3) 0.066(4) 0.020(3) 0.020(4) 0.024(3) C29 0.039(3) 0.046(3) 0.042(3) 0.016(3) 0.025(2) 0.023(2) C33 0.055(3) 0.046(3) 0.037(3) 0.020(3) 0.022(3) 0.031(3) C31 0.037(3) 0.045(3) 0.053(3) 0.006(3) 0.018(3) 0.023(3) C32 0.056(3) 0.063(4) 0.043(3) 0.016(3) 0.028(3) 0.034(3) C30 0.040(3) 0.041(3) 0.053(3) 0.017(3) 0.021(3) 0.019(3) C34 0.029(3) 0.034(3) 0.035(3) 0.008(2) 0.015(2) 0.018(2) _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 C2 C3 1.363(5) . ? C2 C1 1.424(5) . ? C2 C10 1.446(5) . ? C3 C4 1.417(5) . ? C4 C5 1.418(5) . ? C4 C9 1.418(5) . ? C5 C6 1.360(6) . ? C7 C8 1.361(6) . ? C7 C6 1.393(6) . ? C8 C9 1.394(5) . ? C1 N1 1.323(5) . ? C9 N1 1.380(5) . ? C10 N2 1.284(4) . ? N2 N3 1.422(4) . ? N3 C11 1.290(4) . ? C12 C11 1.473(5) . ? C12 C29 1.379(5) . ? C12 C33 1.393(5) . ? C11 C34 1.510(5) . ? N4 C17 1.374(5) . ? N4 C13 1.325(5) . ? C14 C13 1.412(5) . ? C14 C15 1.377(5) . ? C14 C22 1.451(5) . ? C16 C17 1.412(5) . ? C16 C15 1.414(5) . ? C16 C21 1.416(5) . ? C17 C18 1.411(5) . ? C20 C21 1.368(5) . ? C20 C19 1.395(6) . ? C18 C19 1.364(6) . ? C22 N5 1.276(4) . ? N6 N5 1.410(4) . ? N6 C34 1.291(4) . ? C23 C24 1.392(5) . ? C23 C28 1.383(5) . ? C23 C34 1.486(5) . ? C24 C25 1.389(6) . ? C28 C27 1.382(6) . ? C27 C26 1.369(6) . ? C26 C25 1.371(6) . ? C29 C30 1.379(5) . ? C33 C32 1.384(5) . ? C31 C32 1.375(5) . ? C31 C30 1.367(5) . ? 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 C3 C2 C1 117.6(4) . . ? C3 C2 C10 120.6(4) . . ? C1 C2 C10 121.8(4) . . ? C2 C3 C4 120.8(4) . . ? C3 C4 C5 123.4(4) . . ? C3 C4 C9 117.4(4) . . ? C5 C4 C9 119.2(4) . . ? C6 C5 C4 120.0(5) . . ? C8 C7 C6 121.6(5) . . ? C7 C8 C9 120.0(5) . . ? N1 C1 C2 124.3(4) . . ? C5 C6 C7 120.0(5) . . ? C8 C9 C4 119.1(4) . . ? N1 C9 C4 122.0(4) . . ? N1 C9 C8 118.9(4) . . ? C1 N1 C9 117.9(4) . . ? N2 C10 C2 121.8(4) . . ? C10 N2 N3 111.1(3) . . ? C11 N3 N2 112.6(3) . . ? C29 C12 C11 121.6(4) . . ? C29 C12 C33 118.2(4) . . ? C33 C12 C11 120.2(4) . . ? N3 C11 C12 119.4(4) . . ? N3 C11 C34 123.6(3) . . ? C12 C11 C34 116.9(4) . . ? C13 N4 C17 116.7(4) . . ? C13 C14 C22 119.6(4) . . ? C15 C14 C13 117.8(4) . . ? C15 C14 C22 122.6(4) . . ? C17 C16 C15 117.9(4) . . ? C17 C16 C21 118.9(4) . . ? C15 C16 C21 123.1(4) . . ? N4 C17 C16 122.8(4) . . ? N4 C17 C18 117.9(4) . . ? C16 C17 C18 119.3(4) . . ? N4 C13 C14 125.1(4) . . ? C14 C15 C16 119.6(4) . . ? C21 C20 C19 121.0(5) . . ? C20 C21 C16 120.0(5) . . ? C19 C18 C17 120.4(5) . . ? C18 C19 C20 120.3(5) . . ? N5 C22 C14 121.3(4) . . ? C34 N6 N5 111.3(3) . . ? C22 N5 N6 111.9(3) . . ? C24 C23 C34 121.1(4) . . ? C28 C23 C24 118.6(4) . . ? C28 C23 C34 120.2(4) . . ? C25 C24 C23 120.7(5) . . ? C23 C28 C27 120.5(5) . . ? C26 C27 C28 120.2(5) . . ? C27 C26 C25 120.6(5) . . ? C26 C25 C24 119.4(5) . . ? C30 C29 C12 121.2(5) . . ? C32 C33 C12 120.1(4) . . ? C30 C31 C32 119.4(5) . . ? C31 C32 C33 120.7(5) . . ? C31 C30 C29 120.4(5) . . ? N6 C34 C11 122.8(3) . . ? N6 C34 C23 118.3(3) . . ? C23 C34 C11 118.5(4) . . ? _shelx_res_file ; TITL TEST10 OLEX2: imported from CIF test10.res created by SHELXL-2018/1 at 22:19:43 on 21-Aug-2021 CELL 0.71073 10.885 11.134 12.87 90.122 114.141 110.277 ZERR 2 0.003 0.003 0.003 0.006 0.006 0.005 LATT 1 SFAC C H N DISP C 0.0033 0.0016 DISP H 0 0 DISP N 0.0061 0.0033 UNIT 68 48 12 L.S. 20 PLAN 5 SIZE 0.24 0.2 0.19 TEMP -173(2) fmap 2 53 acta OMIT -1 1 1 REM REM REM WGHT 0.052200 FVAR 0.59074 C2 1 0.275638 0.938648 0.574829 11.00000 0.03665 0.03674 = 0.03061 0.00997 0.01504 0.02037 C3 1 0.264490 1.011438 0.488874 11.00000 0.04330 0.04018 = 0.03640 0.00434 0.01515 0.01880 C4 1 0.210249 1.111139 0.483703 11.00000 0.03426 0.03613 = 0.03046 0.00877 0.01031 0.01385 C5 1 0.198130 1.191176 0.397452 11.00000 0.04625 0.04144 = 0.03527 0.00310 0.01186 0.01518 C7 1 0.102450 1.302491 0.483676 11.00000 0.05211 0.04117 = 0.04975 0.00027 0.00942 0.02651 C8 1 0.113687 1.228287 0.568444 11.00000 0.04779 0.04386 = 0.04256 0.00372 0.01395 0.02415 C1 1 0.229987 0.965967 0.658137 11.00000 0.04063 0.04110 = 0.03441 0.01124 0.01308 0.01887 H1 2 0.239173 0.910515 0.721658 11.00000 0.03417 C6 1 0.145688 1.285406 0.398523 11.00000 0.05338 0.04045 = 0.03955 0.00620 0.01091 0.01913 C9 1 0.168642 1.131784 0.571077 11.00000 0.03676 0.03964 = 0.02999 -0.00001 0.00871 0.01408 N1 3 0.178108 1.057363 0.657532 11.00000 0.04198 0.04891 = 0.03439 0.01010 0.01431 0.01936 C10 1 0.330671 0.836774 0.579535 11.00000 0.03583 0.03869 = 0.03274 0.00799 0.01213 0.01387 N2 3 0.346361 0.769480 0.661476 11.00000 0.04086 0.03700 = 0.03965 0.00518 0.01804 0.02183 N3 3 0.399518 0.674264 0.645470 11.00000 0.04159 0.04230 = 0.03627 0.01060 0.01832 0.01949 C12 1 0.474323 0.503658 0.724223 11.00000 0.03065 0.04145 = 0.02472 0.00635 0.01459 0.01712 C11 1 0.421588 0.607990 0.728676 11.00000 0.02500 0.03522 = 0.03512 0.00311 0.01378 0.00866 N4 3 1.135533 0.947660 1.196838 11.00000 0.03694 0.04841 = 0.03780 0.00801 0.01624 0.01424 C14 1 0.884614 0.838210 1.053842 11.00000 0.03971 0.03370 = 0.02991 0.00741 0.01525 0.01801 C16 1 1.079153 0.851454 1.003816 11.00000 0.03104 0.03748 = 0.03536 0.00799 0.01505 0.01542 C17 1 1.178765 0.919326 1.116573 11.00000 0.02656 0.03647 = 0.03966 0.01068 0.01356 0.01286 C13 1 0.993445 0.906574 1.164222 11.00000 0.04508 0.04753 = 0.03711 0.00957 0.02432 0.01978 C15 1 0.928886 0.811331 0.973517 11.00000 0.03361 0.03576 = 0.02877 0.00392 0.01152 0.01199 C20 1 1.280476 0.865278 0.962951 11.00000 0.04464 0.04834 = 0.05050 0.01530 0.02979 0.02183 C21 1 1.133557 0.824272 0.927543 11.00000 0.03301 0.05095 = 0.04291 0.00223 0.01691 0.01440 C18 1 1.329562 0.962577 1.148938 11.00000 0.03630 0.04403 = 0.04003 0.01519 0.00895 0.01240 C19 1 1.378781 0.935574 1.073346 11.00000 0.03153 0.04948 = 0.06292 0.02525 0.02459 0.02026 C22 1 0.732433 0.794766 1.030413 11.00000 0.02821 0.04410 = 0.03393 0.00813 0.01678 0.01590 N6 3 0.492803 0.689996 0.930932 11.00000 0.02808 0.04765 = 0.04215 0.00867 0.01920 0.01722 N5 3 0.631217 0.732795 0.931687 11.00000 0.02718 0.04971 = 0.03325 0.00562 0.01327 0.01570 C23 1 0.240880 0.560255 0.818639 11.00000 0.03205 0.03654 = 0.04158 0.01079 0.02046 0.01876 C24 1 0.121751 0.518787 0.710546 11.00000 0.03314 0.05107 = 0.04742 0.01123 0.02198 0.01592 H24 2 0.132734 0.538486 0.640774 11.00000 0.02913 C28 1 0.217470 0.532132 0.915162 11.00000 0.03787 0.05199 = 0.04897 0.01495 0.02422 0.02052 C27 1 0.078556 0.464220 0.904165 11.00000 0.05270 0.05562 = 0.08748 0.03459 0.05082 0.02873 H27 2 0.070774 0.443486 0.974845 11.00000 0.05254 C26 1 -0.037368 0.423214 0.797164 11.00000 0.03294 0.04917 = 0.11129 0.02924 0.03211 0.01868 C25 1 -0.017639 0.450362 0.699920 11.00000 0.04639 0.05592 = 0.06555 0.02044 0.01963 0.02364 C29 1 0.467631 0.411096 0.794959 11.00000 0.03941 0.04594 = 0.04163 0.01640 0.02499 0.02322 C33 1 0.530058 0.494962 0.645745 11.00000 0.05513 0.04595 = 0.03668 0.02023 0.02173 0.03140 C31 1 0.564156 0.301503 0.708414 11.00000 0.03709 0.04478 = 0.05257 0.00594 0.01787 0.02263 C32 1 0.573826 0.393796 0.638220 11.00000 0.05556 0.06265 = 0.04299 0.01565 0.02772 0.03420 H32 2 0.603887 0.386851 0.581266 11.00000 0.06654 C30 1 0.512194 0.311030 0.787145 11.00000 0.03976 0.04059 = 0.05290 0.01677 0.02090 0.01880 C34 1 0.391300 0.627665 0.830612 11.00000 0.02890 0.03386 = 0.03463 0.00812 0.01451 0.01751 H19 2 1.482768 0.965518 1.095206 11.00000 0.03793 H5 2 0.238051 1.179232 0.342406 11.00000 0.03684 H31 2 0.591923 0.229472 0.700563 11.00000 0.04791 H33 2 0.534713 0.558727 0.595747 11.00000 0.02067 H30 2 0.508670 0.251234 0.837600 11.00000 0.03735 H3 2 0.296392 0.995871 0.430223 11.00000 0.04031 H8 2 0.085669 1.238562 0.627555 11.00000 0.05460 H15 2 0.857347 0.763534 0.895114 11.00000 0.02070 H21 2 1.058915 0.773380 0.847374 11.00000 0.04772 H28 2 0.298782 0.560472 0.989091 11.00000 0.03956 H6 2 0.139482 1.340791 0.338270 11.00000 0.05843 H26 2 -0.128534 0.376523 0.789370 11.00000 0.06949 H10 2 0.366358 0.821896 0.514629 11.00000 0.04835 H29 2 0.430377 0.414811 0.851055 11.00000 0.04059 H13 2 0.960125 0.920035 1.219199 11.00000 0.02991 H18 2 1.391819 1.007508 1.225006 11.00000 0.05361 H7 2 0.066236 1.367457 0.484782 11.00000 0.04802 H20 2 1.317619 0.848062 0.909419 11.00000 0.04776 H25 2 -0.100857 0.420536 0.618734 11.00000 0.05842 H22 2 0.708856 0.808060 1.091110 11.00000 0.03446 HKLF 4 REM TEST10 OLEX2: imported from CIF REM R1 = 0.0416 for 1525 Fo > 4sig(Fo) and 0.0747 for all 2318 data REM 457 parameters refined using 0 restraints END WGHT 0.0538 0.0000 REM Highest difference peak 0.144, deepest hole -0.203, 1-sigma level 0.038 Q1 1 0.2036 0.5176 0.5798 11.00000 0.05 0.14 Q2 1 0.5990 0.6575 0.8461 11.00000 0.05 0.14 Q3 1 0.3064 0.4241 0.9946 11.00000 0.05 0.14 Q4 1 0.1691 0.7000 0.7361 11.00000 0.05 0.14 Q5 1 -0.0226 1.3478 0.3590 11.00000 0.05 0.13 ; _shelx_res_checksum 51129 _shelx_hkl_file ; -1 0 0 2.42 0.93 -1 0 0 3.19 1.18 1 0 0 4.97 0.99 2 0 0 9.73 2.16 -2 0 0 13.23 3.34 -2 0 0 8.06 2.56 -3 0 0 607.75 23.66 3 0 0 598.34 22.69 -3 0 0 603.91 21.29 -4 0 0 71.47 8.18 4 0 0 74.29 7.69 -4 0 0 82.46 7.04 -4 0 0 70.33 5.48 5 0 0 16.20 5.34 -5 0 0 22.93 4.20 -5 0 0 16.10 5.43 -5 0 0 15.60 4.91 -6 0 0 5.72 5.17 -6 0 0 1.91 3.17 6 0 0 0.52 4.11 7 0 0 -0.80 3.93 -7 0 0 -0.01 6.18 7 0 0 -1.76 5.39 -8 0 0 64.67 13.86 8 0 0 46.74 10.64 8 -1 0 38.87 9.55 -8 1 0 8.83 7.63 -8 1 0 17.59 7.66 7 -1 0 4.80 5.82 -7 1 0 -0.43 5.18 -7 1 0 0.07 5.30 6 -1 0 83.88 10.00 -6 1 0 64.39 5.89 -6 1 0 68.35 8.81 -6 1 0 63.46 10.32 5 -1 0 16.46 5.13 -5 1 0 29.44 5.84 -5 1 0 15.09 5.42 4 -1 0 37.33 3.78 4 -1 0 28.50 5.39 -4 1 0 35.27 5.50 -4 1 0 43.15 6.58 -3 1 0 1.26 2.72 3 -1 0 3.28 2.72 3 -1 0 -0.25 1.68 -3 1 0 -3.95 2.27 -2 1 0 215.66 10.02 -2 1 0 223.89 9.43 2 -1 0 214.02 7.45 1 -1 0 674.65 18.75 -1 1 0 532.53 19.65 -1 1 0 673.55 19.53 0 -1 0 30.68 2.12 0 1 0 25.71 2.07 -1 -1 0 1053.72 32.84 -1 -1 0 1105.91 33.68 -2 -1 0 9961.40 284.25 2 1 0 9998.10 280.80 -2 -1 0 9405.82 275.50 -3 -1 0 297.84 14.65 3 1 0 284.74 12.22 3 1 0 293.07 13.94 4 1 0 68.35 6.36 4 1 0 69.55 7.76 -4 -1 0 73.61 6.50 -4 -1 0 65.52 8.46 5 1 0 22.84 4.96 5 1 0 20.06 5.96 -5 -1 0 16.35 6.00 -5 -1 0 20.82 4.45 6 1 0 47.93 7.09 -6 -1 0 44.78 6.58 -6 -1 0 56.61 10.59 6 1 0 54.73 9.17 7 1 0 6.27 6.08 -7 -1 0 -0.65 6.36 7 1 0 13.91 5.33 8 1 0 5.77 6.66 -8 -1 0 -3.62 5.88 9 -2 0 -1.12 5.91 -9 2 0 -5.80 5.77 8 -2 0 12.74 8.41 -8 2 0 17.11 8.35 -8 2 0 25.92 8.59 -7 2 0 8.69 6.23 -7 2 0 9.33 5.79 7 -2 0 10.48 6.24 -6 2 0 123.29 12.31 6 -2 0 127.52 12.10 -6 2 0 103.77 10.57 -5 2 0 541.64 25.14 5 -2 0 565.75 24.32 5 -2 0 563.97 18.51 -5 2 0 551.48 23.31 -4 2 0 0.48 3.23 -4 2 0 3.52 3.42 4 -2 0 5.18 1.94 4 -2 0 3.57 3.32 3 -2 0 19.71 2.38 -3 2 0 25.35 4.36 -3 2 0 27.09 4.45 3 -2 0 13.98 3.74 -2 2 0 93.71 6.59 2 -2 0 85.70 4.55 -2 2 0 89.28 5.98 1 -2 0 294.20 10.95 -1 2 0 311.25 10.42 -1 2 0 315.35 11.90 0 -2 0 214.56 9.18 0 2 0 218.21 9.19 0 -2 0 210.47 7.27 1 2 0 4.00 2.82 -1 -2 0 4.52 2.46 -1 -2 0 -0.63 2.01 -2 -2 0 61.59 5.83 2 2 0 52.10 5.62 -2 -2 0 55.56 5.34 3 2 0 86.01 6.50 -3 -2 0 113.61 7.76 -3 -2 0 96.49 8.58 3 2 0 105.39 8.70 -4 -2 0 1271.85 46.02 4 2 0 1245.98 44.76 -4 -2 0 1246.26 42.63 4 2 0 1286.80 41.89 5 2 0 10.50 5.42 -5 -2 0 6.30 3.39 5 2 0 21.44 5.50 -5 -2 0 13.35 5.92 -6 -2 0 84.38 12.55 6 2 0 50.06 9.12 6 2 0 56.93 8.16 -6 -2 0 50.63 7.49 -7 -2 0 19.26 6.34 7 2 0 8.49 6.28 7 2 0 6.88 7.01 -7 -2 0 22.01 9.05 9 -3 0 84.97 13.65 -9 3 0 85.19 13.05 -9 3 0 75.00 14.45 8 -3 0 11.66 7.48 -8 3 0 15.40 8.02 -8 3 0 12.81 8.15 -7 3 0 365.93 19.68 -7 3 0 264.19 19.35 7 -3 0 286.61 19.05 -6 3 0 4.83 4.71 -6 3 0 11.26 5.07 6 -3 0 4.60 4.24 5 -3 0 139.44 11.06 -5 3 0 134.15 11.40 -5 3 0 134.85 10.27 5 -3 0 128.85 6.31 4 -3 0 124.32 9.11 -4 3 0 121.31 9.18 -4 3 0 109.14 8.50 4 -3 0 109.74 5.72 3 -3 0 19.60 3.99 -3 3 0 25.84 4.57 -3 3 0 22.89 4.05 3 -3 0 24.17 3.00 -2 3 0 23.54 4.31 -2 3 0 25.08 3.43 -2 3 0 25.49 4.53 2 -3 0 11.01 3.05 1 -3 0 6190.11 175.93 -1 3 0 6102.27 179.51 -1 3 0 6257.83 179.80 -1 3 0 6182.54 176.06 0 -3 0 215.65 10.81 0 3 0 202.41 10.27 0 3 0 202.86 10.32 0 -3 0 230.45 7.76 -1 -3 0 -0.06 1.98 -1 -3 0 1.00 2.11 1 3 0 0.11 2.53 1 3 0 1.76 2.60 -2 -3 0 71.98 6.66 -2 -3 0 57.65 6.25 2 3 0 97.37 7.95 2 3 0 65.14 6.51 -3 -3 0 19.02 4.59 -3 -3 0 35.71 6.23 3 3 0 34.86 6.19 4 3 0 0.15 3.86 4 3 0 5.11 3.89 -4 -3 0 11.40 5.24 -4 -3 0 1.91 3.46 5 3 0 64.25 9.62 -5 -3 0 44.69 7.48 -5 -3 0 54.93 9.81 5 3 0 69.12 8.49 -6 -3 0 -2.24 3.85 -6 -3 0 13.76 6.87 6 3 0 5.27 6.29 6 3 0 6.27 4.99 -7 -3 0 19.45 6.53 7 3 0 34.75 9.35 -7 -3 0 7.50 7.52 -9 4 0 31.02 10.72 9 -4 0 38.95 10.08 -9 4 0 12.72 7.88 -8 4 0 66.78 12.39 8 -4 0 88.44 12.83 -8 4 0 107.38 12.43 7 -4 0 22.42 7.30 -7 4 0 25.17 7.90 -7 4 0 20.52 7.12 -6 4 0 109.71 10.81 -6 4 0 132.32 12.32 6 -4 0 128.58 11.58 -5 4 0 488.46 22.54 5 -4 0 502.94 17.24 -5 4 0 490.80 22.04 5 -4 0 485.35 22.85 4 -4 0 101.96 6.62 4 -4 0 106.92 9.05 -4 4 0 104.85 8.99 -4 4 0 106.41 8.28 -3 4 0 61.14 7.02 -3 4 0 51.69 6.50 3 -4 0 51.78 4.81 -3 4 0 61.67 5.69 -2 4 0 20.96 4.76 2 -4 0 21.59 3.99 -2 4 0 19.16 2.86 -2 4 0 18.97 4.63 1 -4 0 63.67 6.24 -1 4 0 78.53 7.03 -1 4 0 62.19 6.64 0 -4 0 39.21 5.69 0 4 0 52.80 5.88 0 4 0 42.74 5.62 1 4 0 2.60 2.76 -1 -4 0 3.40 2.40 -1 -4 0 6.05 3.22 1 4 0 -5.06 2.98 -2 -4 0 65.80 7.58 2 4 0 88.48 8.34 2 4 0 87.99 8.58 -2 -4 0 79.87 7.23 -3 -4 0 -4.47 3.22 3 4 0 -4.01 3.56 3 4 0 -2.87 3.37 -3 -4 0 0.92 3.38 -4 -4 0 5.55 4.56 4 4 0 4.84 4.05 -4 -4 0 16.84 5.30 4 4 0 11.21 5.43 -5 -4 0 15.68 6.48 -5 -4 0 20.82 7.31 5 4 0 13.48 6.72 5 4 0 33.05 8.45 -6 -4 0 7.93 6.50 6 4 0 1.89 5.99 6 4 0 0.81 5.76 -6 -4 0 1.36 5.49 -9 5 0 10.11 8.52 9 -5 0 4.27 6.68 -9 5 0 13.86 7.26 8 -5 0 5.29 6.55 -8 5 0 1.23 5.88 -8 5 0 4.32 5.68 -7 5 0 -0.77 4.74 -7 5 0 1.17 5.25 7 -5 0 3.07 4.39 6 -5 0 299.94 18.12 -6 5 0 309.29 17.92 -6 5 0 313.00 18.10 5 -5 0 -0.23 2.86 -5 5 0 2.51 3.43 5 -5 0 -4.97 2.19 -5 5 0 -1.56 3.41 -4 5 0 14.01 4.00 -4 5 0 13.31 5.06 4 -5 0 12.56 3.57 -4 5 0 13.80 5.07 -3 5 0 1245.28 44.41 -3 5 0 1260.27 43.17 3 -5 0 1191.07 40.27 -3 5 0 1257.75 40.25 -2 5 0 514.72 22.09 -2 5 0 499.31 16.95 -2 5 0 498.80 21.51 2 -5 0 494.76 20.41 -1 5 0 47.28 6.45 1 -5 0 37.56 6.08 -1 5 0 41.21 6.54 0 5 0 33.31 6.00 0 5 0 29.19 5.70 0 -5 0 25.22 5.79 -1 -5 0 79.86 8.83 1 5 0 86.69 8.47 1 5 0 83.23 8.83 -1 -5 0 87.18 6.32 -2 -5 0 -2.63 2.88 -2 -5 0 2.89 3.39 2 5 0 5.68 4.69 2 5 0 0.43 3.59 3 5 0 4.54 5.78 3 5 0 9.99 5.52 -3 -5 0 15.34 5.25 -3 -5 0 7.26 5.18 4 5 0 8.87 6.39 4 5 0 7.67 5.11 -4 -5 0 4.77 5.20 -4 -5 0 5.19 5.21 5 5 0 1.20 6.75 -5 -5 0 0.90 5.56 -5 -5 0 -1.72 4.70 5 5 0 5.15 6.38 -9 6 0 -2.89 5.84 -9 6 0 -1.39 5.96 9 -6 0 0.82 6.09 -8 6 0 4.24 5.87 -8 6 0 -6.79 4.92 8 -6 0 3.15 5.07 -7 6 0 1.90 5.15 -7 6 0 -1.65 4.80 7 -6 0 1.73 4.13 6 -6 0 67.67 9.45 -6 6 0 72.28 9.81 -6 6 0 51.59 8.27 5 -6 0 6.51 3.46 -5 6 0 7.56 4.86 -5 6 0 2.35 3.76 4 -6 0 1.07 3.24 -4 6 0 5.97 3.53 -4 6 0 6.99 4.44 -4 6 0 11.67 5.11 -3 6 0 440.44 22.03 3 -6 0 430.72 19.49 -3 6 0 443.44 21.48 -3 6 0 448.66 16.88 2 -6 0 77.41 8.48 -2 6 0 75.33 8.54 -2 6 0 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