data_PhEuOEt_0m_a _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H49 Eu F9 N3 O11' _chemical_formula_weight 1298.97 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.844(8) _cell_length_b 18.882(10) _cell_length_c 20.014(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5610(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26670 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 25.1 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_F_000 2624 _exptl_transmission_factor_min 0.653400 _exptl_transmission_factor_max 0.745700 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_absorpt_coefficient_mu 1.211 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26670 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.483 _diffrn_reflns_theta_max 25.096 _diffrn_reflns_theta_full 25.096 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 9943 _reflns_number_gt 9258 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.810 _reflns_Friedel_fraction_max 0.993 _reflns_Friedel_fraction_full 0.993 _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. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.0392P)^2^+3.3203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3914 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.013(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 9943 _refine_ls_number_parameters 753 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 0.713 _refine_ls_restrained_S_all 0.715 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 C46 C -0.2847(7) 0.2397(6) 0.2499(6) 0.0502(14) Uani 0.473(7) 1 d D U P A 1 H46A H -0.263242 0.209476 0.285703 0.060 Uiso 0.473(7) 1 calc R U P A 1 H46B H -0.298175 0.211050 0.210888 0.060 Uiso 0.473(7) 1 calc R U P A 1 C47 C -0.3639(8) 0.2831(6) 0.2710(6) 0.0502(14) Uani 0.473(7) 1 d D U P A 1 H47A H -0.345711 0.315670 0.305339 0.075 Uiso 0.473(7) 1 calc R U P A 1 H47B H -0.410232 0.252580 0.287948 0.075 Uiso 0.473(7) 1 calc R U P A 1 H47C H -0.386496 0.309114 0.233354 0.075 Uiso 0.473(7) 1 calc R U P A 1 C46A C -0.3070(7) 0.2764(6) 0.2749(5) 0.0502(14) Uani 0.527(7) 1 d D . P A 2 H46C H -0.297258 0.234065 0.301305 0.060 Uiso 0.527(7) 1 calc R U P A 2 H46D H -0.324080 0.314885 0.304384 0.060 Uiso 0.527(7) 1 calc R U P A 2 C47A C -0.3777(7) 0.2641(6) 0.2229(5) 0.0502(14) Uani 0.527(7) 1 d D . P A 2 H47D H -0.395394 0.308645 0.203799 0.075 Uiso 0.527(7) 1 calc R U P A 2 H47E H -0.429118 0.241918 0.243126 0.075 Uiso 0.527(7) 1 calc R U P A 2 H47F H -0.354053 0.233977 0.188544 0.075 Uiso 0.527(7) 1 calc R U P A 2 Eu01 Eu 0.23292(2) 0.51575(2) 0.39622(2) 0.02243(6) Uani 1 1 d . . . . . O10 O 0.3645(2) 0.56883(17) 0.35199(14) 0.0318(7) Uani 1 1 d . . . . . F1 F 0.2862(2) 0.75892(15) 0.45905(19) 0.0617(9) Uani 1 1 d . . . . . O7 O 0.1296(2) 0.42613(16) 0.35786(14) 0.0284(7) Uani 1 1 d . . . . . O4 O 0.09761(19) 0.53775(14) 0.45461(14) 0.0294(7) Uani 1 1 d . . . . . O3 O 0.21236(19) 0.64159(14) 0.41190(13) 0.0304(7) Uani 1 1 d . . . . . F7 F 0.3363(3) 0.65699(17) 0.58581(15) 0.0648(9) Uani 1 1 d . . . . . F4 F 0.2621(3) 0.3236(2) 0.56899(18) 0.0866(12) Uani 1 1 d . . . . . O9 O 0.3226(2) 0.55149(16) 0.48905(13) 0.0330(7) Uani 1 1 d . . . . . O5 O -0.2346(2) 0.48606(16) 0.64010(14) 0.0413(7) Uani 1 1 d . . . . . F9 F 0.4191(2) 0.56724(18) 0.60674(14) 0.0631(8) Uani 1 1 d . . . . . O6 O 0.2184(2) 0.42652(15) 0.48370(13) 0.0321(7) Uani 1 1 d . . . . . O1 O 0.1360(2) 0.58747(19) 0.18003(15) 0.0457(8) Uani 1 1 d . . . . . O2 O 0.4224(3) 0.32949(19) 0.3225(2) 0.0568(10) Uani 1 1 d . . . . . F5 F 0.1341(3) 0.2767(2) 0.56185(18) 0.0944(15) Uani 1 1 d . . . . . F8 F 0.4785(3) 0.6620(2) 0.56844(15) 0.0850(13) Uani 1 1 d . . . . . F2 F 0.1702(3) 0.78523(17) 0.51487(17) 0.0746(12) Uani 1 1 d . . . . . F3 F 0.1685(3) 0.79180(16) 0.40917(18) 0.0733(11) Uani 1 1 d . . . . . O11 O 0.6811(2) 0.6770(2) 0.17332(18) 0.0530(10) Uani 1 1 d . . . . . O8 O -0.2216(3) 0.2957(2) 0.23472(19) 0.0681(13) Uani 1 1 d D . . . . N2 N 0.2743(2) 0.46869(17) 0.27249(16) 0.0297(8) Uani 1 1 d . . . . . C28 C -0.0200(3) 0.5637(2) 0.5285(2) 0.0264(9) Uani 1 1 d . . . . . N1 N 0.1494(2) 0.57214(19) 0.29158(16) 0.0291(8) Uani 1 1 d . . . . . C26 C 0.0947(3) 0.6549(2) 0.4915(2) 0.0274(9) Uani 1 1 d . . . . . H26 H 0.067191 0.687447 0.519854 0.033 Uiso 1 1 calc R U . . . C52 C 0.5010(3) 0.6223(2) 0.3233(2) 0.0334(10) Uani 1 1 d . . . . . N3 N 0.3542(2) 0.4142(2) 0.38315(19) 0.0316(9) Uani 1 1 d . . . . . C25 C 0.1673(3) 0.6766(2) 0.45367(19) 0.0256(9) Uani 1 1 d . . . . . C40 C -0.0013(3) 0.3570(2) 0.3480(2) 0.0289(10) Uani 1 1 d . . . . . C24 C 0.1973(3) 0.7534(2) 0.4596(2) 0.0318(10) Uani 1 1 d . . . . . C36 C 0.1771(4) 0.3370(3) 0.5571(2) 0.0453(13) Uani 1 1 d . . . . . F6 F 0.1531(3) 0.3759(2) 0.60943(17) 0.0985(14) Uani 1 1 d . . . . . C42 C -0.0792(3) 0.3331(2) 0.3797(2) 0.0393(12) Uani 1 1 d . . . . . H42 H -0.080526 0.330790 0.426112 0.047 Uiso 1 1 calc R U . . . C29 C -0.0476(3) 0.4934(2) 0.5256(2) 0.0318(10) Uani 1 1 d . . . . . H29 H -0.016898 0.462038 0.498011 0.038 Uiso 1 1 calc R U . . . C41 C -0.0016(3) 0.3599(2) 0.2782(2) 0.0299(9) Uani 1 1 d . . . . . H41 H 0.049211 0.376376 0.255894 0.036 Uiso 1 1 calc R U . . . C17 C 0.4100(3) 0.3740(3) 0.4327(3) 0.0437(12) Uani 1 1 d . . . . . H17 H 0.373106 0.359547 0.470930 0.052 Uiso 1 1 calc R U . . . C30 C -0.0699(3) 0.6097(2) 0.5680(2) 0.0345(10) Uani 1 1 d . . . . . H30 H -0.054591 0.657414 0.569209 0.041 Uiso 1 1 calc R U . . . C27 C 0.0606(3) 0.5853(2) 0.48882(19) 0.0263(9) Uani 1 1 d . . . . . C1 C -0.1638(3) 0.6002(3) 0.3911(3) 0.0513(12) Uani 1 1 d . . . . . H1 H -0.217683 0.593887 0.414015 0.062 Uiso 1 1 calc R U . . . C57 C 0.6250(3) 0.6611(2) 0.2240(2) 0.0394(11) Uani 1 1 d . . . . . C50 C 0.4453(3) 0.6174(3) 0.4421(2) 0.0370(12) Uani 1 1 d . . . . . H50 H 0.493807 0.646044 0.453693 0.044 Uiso 1 1 calc R U . . . C10 C 0.2395(3) 0.4992(2) 0.21809(18) 0.0329(10) Uani 1 1 d . . . . . C4 C -0.0401(3) 0.5523(3) 0.3298(2) 0.0401(12) Uani 1 1 d . . . . . H4 H -0.010829 0.513256 0.311488 0.048 Uiso 1 1 calc R U . . . C31 C -0.1419(3) 0.5859(2) 0.6057(2) 0.0380(10) Uani 1 1 d . . . . . H31 H -0.174486 0.617570 0.631865 0.046 Uiso 1 1 calc R U . . . C45 C -0.1522(3) 0.3147(3) 0.2748(3) 0.0450(13) Uani 1 1 d . . . . . C32 C -0.1192(3) 0.4693(2) 0.5628(2) 0.0349(11) Uani 1 1 d . . . . . H32 H -0.136605 0.422125 0.559892 0.042 Uiso 1 1 calc R U . . . C56 C 0.5456(3) 0.6269(3) 0.2078(2) 0.0413(12) Uani 1 1 d . . . . . H56 H 0.533306 0.616714 0.163222 0.050 Uiso 1 1 calc R U . . . C39 C 0.0785(3) 0.3817(2) 0.3856(2) 0.0270(9) Uani 1 1 d . . . . . C11 C 0.2637(3) 0.4802(3) 0.1536(2) 0.0490(12) Uani 1 1 d . . . . . H11 H 0.239362 0.503238 0.116726 0.059 Uiso 1 1 calc R U . . . C7 C 0.0837(3) 0.6306(2) 0.2845(2) 0.0351(11) Uani 1 1 d . . . . . H7 H 0.111773 0.675081 0.298859 0.042 Uiso 1 1 calc R U . . . C9 C 0.1731(3) 0.5548(2) 0.2330(2) 0.0322(10) Uani 1 1 d . . . . . C33 C -0.1656(2) 0.5151(2) 0.6045(2) 0.0317(8) Uani 1 1 d . . . . . C2 C -0.1205(4) 0.5434(3) 0.3635(3) 0.0493(13) Uani 1 1 d . . . . . H2 H -0.145364 0.498383 0.367481 0.059 Uiso 1 1 calc R U . . . C38 C 0.0949(3) 0.3536(2) 0.4504(2) 0.0328(10) Uani 1 1 d . . . . . H38 H 0.057368 0.317749 0.465954 0.039 Uiso 1 1 calc R U . . . C43 C -0.0750(3) 0.3389(2) 0.2423(2) 0.0370(11) Uani 1 1 d . . . . . H43 H -0.073527 0.340746 0.195899 0.044 Uiso 1 1 calc R U . . . C34 C -0.2712(3) 0.5255(3) 0.6953(2) 0.0461(11) Uani 1 1 d . . . . . H34A H -0.327290 0.503823 0.709512 0.055 Uiso 1 1 calc R U . . . H34B H -0.284373 0.573451 0.680903 0.055 Uiso 1 1 calc R U . . . C6 C -0.0030(3) 0.6194(2) 0.3231(2) 0.0330(11) Uani 1 1 d . . . . . C18 C 0.4882(3) 0.4183(3) 0.4557(2) 0.0408(12) Uani 1 1 d . . . . . C44 C -0.1540(3) 0.3127(3) 0.3441(3) 0.0468(13) Uani 1 1 d . . . . . H44 H -0.205604 0.297725 0.366320 0.056 Uiso 1 1 calc R U . . . C48 C 0.4070(4) 0.6199(3) 0.5632(2) 0.0484(13) Uani 1 1 d . . . . . C14 C 0.3336(3) 0.4165(3) 0.2639(2) 0.0373(11) Uani 1 1 d . . . . . C19 C 0.5505(3) 0.4446(3) 0.4112(3) 0.0524(14) Uani 1 1 d . . . . . H19 H 0.543105 0.436254 0.365722 0.063 Uiso 1 1 calc R U . . . C16 C 0.4379(4) 0.3087(3) 0.3912(3) 0.0613(15) Uani 1 1 d . . . . . H16A H 0.500830 0.297217 0.398437 0.074 Uiso 1 1 calc R U . . . H16B H 0.401462 0.267858 0.402872 0.074 Uiso 1 1 calc R U . . . C53 C 0.5812(4) 0.6565(3) 0.3393(3) 0.0473(13) Uani 1 1 d . . . . . H53 H 0.593744 0.666561 0.383826 0.057 Uiso 1 1 calc R U . . . C54 C 0.4848(3) 0.6079(3) 0.2557(2) 0.0384(11) Uani 1 1 d . . . . . H54 H 0.431918 0.585049 0.243328 0.046 Uiso 1 1 calc R U . . . C5 C -0.0467(4) 0.6759(3) 0.3512(3) 0.0441(13) Uani 1 1 d . . . . . H5 H -0.022190 0.721060 0.347794 0.053 Uiso 1 1 calc R U . . . C15 C 0.3685(3) 0.3874(3) 0.3269(3) 0.0388(12) Uani 1 1 d . . . . . C55 C 0.6422(4) 0.6759(3) 0.2910(3) 0.0490(13) Uani 1 1 d . . . . . H55 H 0.695138 0.698973 0.303038 0.059 Uiso 1 1 calc R U . . . C22 C 0.5736(4) 0.4714(4) 0.5448(3) 0.072(2) Uani 1 1 d . . . . . H22 H 0.580315 0.481123 0.590052 0.086 Uiso 1 1 calc R U . . . C51 C 0.4321(3) 0.6010(2) 0.3738(2) 0.0310(10) Uani 1 1 d . . . . . C49 C 0.3894(3) 0.5929(2) 0.4923(2) 0.0342(11) Uani 1 1 d . . . . . C3 C -0.1274(4) 0.6659(3) 0.3847(3) 0.0531(14) Uani 1 1 d . . . . . H3 H -0.157053 0.704697 0.403012 0.064 Uiso 1 1 calc R U . . . C37 C 0.1635(3) 0.3767(2) 0.4912(2) 0.0311(10) Uani 1 1 d . . . . . C35 C -0.2067(4) 0.5278(3) 0.7534(2) 0.0556(15) Uani 1 1 d . . . . . H35A H -0.194898 0.480409 0.768570 0.083 Uiso 1 1 calc R U . . . H35B H -0.232800 0.554767 0.789156 0.083 Uiso 1 1 calc R U . . . H35C H -0.151318 0.549508 0.739575 0.083 Uiso 1 1 calc R U . . . C20 C 0.5004(4) 0.4322(3) 0.5228(3) 0.0563(15) Uani 1 1 d . . . . . H20 H 0.459075 0.414975 0.553676 0.068 Uiso 1 1 calc R U . . . C21 C 0.6236(4) 0.4830(4) 0.4330(3) 0.0649(16) Uani 1 1 d . . . . . H21 H 0.665019 0.500373 0.402195 0.078 Uiso 1 1 calc R U . . . C23 C 0.6359(4) 0.4960(4) 0.5001(3) 0.073(2) Uani 1 1 d . . . . . H23 H 0.685942 0.521091 0.514827 0.088 Uiso 1 1 calc R U . . . C58 C 0.7726(5) 0.6973(4) 0.1885(4) 0.082(2) Uani 1 1 d . . . . . H58A H 0.797994 0.664829 0.220969 0.099 Uiso 1 1 calc R U . . . H58B H 0.773376 0.744539 0.207547 0.099 Uiso 1 1 calc R U . . . C12 C 0.3256(4) 0.4254(4) 0.1459(3) 0.0626(18) Uani 1 1 d . . . . . H12 H 0.343305 0.411168 0.103356 0.075 Uiso 1 1 calc R U . . . C8 C 0.0672(4) 0.6332(3) 0.2080(2) 0.0509(14) Uani 1 1 d . . . . . H8A H 0.007465 0.615874 0.197157 0.061 Uiso 1 1 calc R U . . . H8B H 0.073375 0.681165 0.191273 0.061 Uiso 1 1 calc R U . . . C13 C 0.3604(4) 0.3927(3) 0.2012(3) 0.0575(16) Uani 1 1 d . . . . . H13 H 0.400938 0.355381 0.197000 0.069 Uiso 1 1 calc R U . . . C59 C 0.8258(5) 0.6960(5) 0.1278(5) 0.118(3) Uani 1 1 d . . . . . H59A H 0.826927 0.648693 0.110229 0.176 Uiso 1 1 calc R U . . . H59B H 0.886118 0.711049 0.137561 0.176 Uiso 1 1 calc R U . . . H59C H 0.799495 0.727326 0.095471 0.176 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 C46 0.0494(18) 0.0504(17) 0.0509(17) 0.0010(12) 0.0002(12) -0.0036(12) C47 0.0494(18) 0.0504(17) 0.0509(17) 0.0010(12) 0.0002(12) -0.0036(12) C46A 0.0494(18) 0.0504(17) 0.0509(17) 0.0010(12) 0.0002(12) -0.0036(12) C47A 0.0494(18) 0.0504(17) 0.0509(17) 0.0010(12) 0.0002(12) -0.0036(12) Eu01 0.02448(10) 0.02425(9) 0.01854(9) -0.00177(8) 0.00160(8) -0.00196(8) O10 0.0325(18) 0.0361(18) 0.0267(16) -0.0030(14) -0.0003(14) -0.0071(15) F1 0.040(2) 0.0374(16) 0.108(3) -0.0128(16) 0.0033(17) -0.0085(13) O7 0.0328(17) 0.0274(16) 0.0251(15) -0.0017(13) 0.0026(13) -0.0064(14) O4 0.0303(16) 0.0301(16) 0.0277(15) -0.0053(12) 0.0069(12) -0.0003(12) O3 0.0365(18) 0.0279(15) 0.0267(15) -0.0034(11) 0.0050(12) -0.0020(12) F7 0.088(3) 0.057(2) 0.0491(19) -0.0207(15) 0.0091(17) -0.0057(18) F4 0.065(2) 0.109(3) 0.086(2) 0.064(2) -0.020(2) -0.002(2) O9 0.0394(19) 0.0361(17) 0.0236(15) -0.0018(13) -0.0014(13) -0.0083(15) O5 0.0355(16) 0.0495(17) 0.0391(16) -0.0051(14) 0.0139(14) -0.0073(19) F9 0.068(2) 0.094(2) 0.0279(14) 0.0029(17) -0.0125(16) -0.0042(17) O6 0.0349(18) 0.0326(16) 0.0288(15) 0.0054(12) -0.0041(13) -0.0022(14) O1 0.059(2) 0.057(2) 0.0215(16) 0.0086(15) -0.0028(15) -0.0014(18) O2 0.049(2) 0.049(2) 0.072(3) -0.020(2) 0.000(2) 0.0188(19) F5 0.121(3) 0.086(3) 0.076(2) 0.057(2) -0.047(2) -0.061(3) F8 0.091(3) 0.122(3) 0.0428(18) -0.030(2) 0.0031(17) -0.064(3) F2 0.109(3) 0.0482(19) 0.067(2) -0.0331(17) 0.041(2) -0.026(2) F3 0.099(3) 0.0376(17) 0.084(3) 0.0275(17) -0.035(2) -0.0079(16) O11 0.041(2) 0.059(2) 0.059(2) 0.0079(19) 0.0212(18) -0.0100(17) O8 0.050(2) 0.085(3) 0.069(2) 0.038(2) -0.027(2) -0.041(2) N2 0.0241(17) 0.038(2) 0.0266(17) -0.0075(14) 0.0015(15) -0.0086(16) C28 0.022(2) 0.033(2) 0.024(2) 0.0018(17) -0.0001(17) 0.0055(17) N1 0.038(2) 0.0284(19) 0.0210(18) -0.0013(14) -0.0026(15) -0.0038(16) C26 0.030(2) 0.029(2) 0.023(2) -0.0043(17) 0.0024(18) 0.0067(19) C52 0.031(3) 0.034(3) 0.035(3) 0.002(2) -0.003(2) -0.008(2) N3 0.0254(19) 0.035(2) 0.034(2) -0.0046(17) 0.0005(16) 0.0031(15) C25 0.032(2) 0.028(2) 0.0177(19) -0.0001(16) -0.0031(17) 0.0028(18) C40 0.031(2) 0.023(2) 0.033(2) -0.0010(18) 0.002(2) -0.0022(19) C24 0.038(3) 0.031(2) 0.026(2) -0.0043(18) 0.0025(19) 0.002(2) C36 0.045(3) 0.051(3) 0.040(3) 0.013(2) -0.004(2) -0.009(2) F6 0.160(4) 0.103(3) 0.0324(19) 0.012(2) 0.015(2) 0.017(3) C42 0.039(3) 0.038(3) 0.041(3) 0.013(2) 0.002(2) -0.008(2) C29 0.033(2) 0.033(3) 0.030(2) -0.0037(19) 0.0054(17) 0.0013(19) C41 0.029(2) 0.027(2) 0.034(2) 0.0004(18) 0.0009(19) -0.0047(18) C17 0.035(3) 0.041(3) 0.054(3) 0.007(2) -0.001(2) 0.009(2) C30 0.038(3) 0.030(2) 0.036(2) 0.0013(19) 0.005(2) 0.004(2) C27 0.028(2) 0.036(2) 0.016(2) -0.0002(17) -0.0024(17) 0.0036(19) C1 0.042(3) 0.060(3) 0.052(3) 0.004(3) -0.007(3) 0.003(2) C57 0.034(3) 0.036(3) 0.048(3) 0.007(2) 0.008(2) -0.003(2) C50 0.038(3) 0.042(3) 0.031(2) -0.006(2) -0.002(2) -0.017(2) C10 0.032(2) 0.045(3) 0.0218(18) -0.0069(16) 0.0034(17) -0.0140(19) C4 0.042(3) 0.030(2) 0.049(3) -0.003(2) -0.016(2) 0.001(2) C31 0.040(3) 0.039(3) 0.035(2) 0.002(2) 0.011(2) 0.0094(19) C45 0.034(3) 0.040(3) 0.061(3) 0.020(3) -0.013(2) -0.015(2) C32 0.035(3) 0.037(3) 0.032(2) -0.0023(19) 0.0017(19) -0.0024(19) C56 0.038(3) 0.052(3) 0.034(3) -0.001(2) 0.006(2) -0.003(2) C39 0.030(2) 0.0197(19) 0.031(2) -0.0030(18) 0.0027(19) -0.0008(17) C11 0.043(3) 0.078(3) 0.026(2) -0.010(2) 0.006(2) -0.008(3) C7 0.052(3) 0.025(2) 0.028(2) 0.0033(18) -0.008(2) 0.000(2) C9 0.038(3) 0.038(3) 0.020(2) 0.0034(18) -0.0037(18) -0.014(2) C33 0.0264(19) 0.041(2) 0.0282(19) 0.004(2) 0.0002(18) -0.0010(19) C2 0.042(3) 0.047(3) 0.059(3) 0.004(3) -0.020(3) -0.006(2) C38 0.041(3) 0.026(2) 0.031(2) 0.0042(19) 0.003(2) -0.009(2) C43 0.043(3) 0.030(2) 0.038(3) 0.0062(19) -0.003(2) -0.005(2) C34 0.040(2) 0.054(3) 0.044(3) 0.000(2) 0.018(2) -0.001(3) C6 0.042(3) 0.031(3) 0.026(2) 0.001(2) -0.014(2) 0.005(2) C18 0.030(3) 0.053(3) 0.039(3) 0.005(2) -0.004(2) 0.008(2) C44 0.034(3) 0.052(3) 0.054(3) 0.024(3) -0.001(2) -0.016(2) C48 0.051(3) 0.060(3) 0.034(3) -0.007(2) -0.003(2) -0.022(3) C14 0.026(2) 0.048(3) 0.037(3) -0.018(2) 0.0024(19) -0.001(2) C19 0.040(3) 0.074(4) 0.043(3) -0.001(3) -0.001(2) -0.004(3) C16 0.049(3) 0.051(3) 0.084(4) -0.003(3) -0.014(3) 0.016(2) C53 0.047(3) 0.060(3) 0.035(3) 0.004(2) -0.005(2) -0.016(3) C54 0.030(3) 0.045(3) 0.040(3) -0.005(2) 0.002(2) -0.009(2) C5 0.053(3) 0.031(3) 0.049(3) -0.001(2) -0.011(3) 0.003(2) C15 0.026(2) 0.038(3) 0.052(3) -0.009(2) 0.003(2) 0.003(2) C55 0.036(3) 0.056(3) 0.056(3) 0.008(3) -0.004(2) -0.017(2) C22 0.066(4) 0.106(6) 0.043(3) -0.004(4) -0.020(3) -0.001(4) C51 0.033(3) 0.027(2) 0.032(2) -0.0018(18) -0.0006(19) -0.0041(19) C49 0.037(3) 0.038(3) 0.027(2) -0.0024(19) -0.0051(19) -0.002(2) C3 0.055(3) 0.051(3) 0.053(3) -0.007(3) -0.005(3) 0.010(3) C37 0.038(3) 0.027(2) 0.028(2) 0.0034(18) 0.0040(19) 0.004(2) C35 0.076(4) 0.053(3) 0.038(3) 0.004(2) 0.015(2) 0.000(3) C20 0.050(3) 0.080(4) 0.039(3) 0.012(3) -0.004(3) 0.003(3) C21 0.040(3) 0.097(5) 0.057(3) 0.007(4) -0.002(2) -0.011(4) C23 0.048(3) 0.105(6) 0.067(4) 0.002(4) -0.021(3) -0.016(3) C58 0.053(4) 0.100(5) 0.093(5) 0.005(4) 0.027(4) -0.025(4) C12 0.049(3) 0.106(5) 0.033(3) -0.031(3) 0.010(3) -0.001(3) C8 0.073(4) 0.044(3) 0.037(3) 0.009(2) -0.010(3) 0.004(3) C13 0.042(3) 0.081(4) 0.049(3) -0.031(3) 0.011(3) 0.007(3) C59 0.066(5) 0.105(6) 0.182(10) 0.030(6) 0.057(6) -0.009(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 C46 O8 1.445(10) . ? C46 C47 1.494(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C46A C47A 1.495(12) . ? C46A O8 1.544(10) . ? C46A H46C 0.9700 . ? C46A H46D 0.9700 . ? C47A H47D 0.9600 . ? C47A H47E 0.9600 . ? C47A H47F 0.9600 . ? Eu01 O4 2.361(3) . ? Eu01 O10 2.367(3) . ? Eu01 O9 2.383(3) . ? Eu01 O7 2.410(3) . ? Eu01 O3 2.416(3) . ? Eu01 O6 2.439(3) . ? Eu01 N3 2.642(4) . ? Eu01 N1 2.656(4) . ? Eu01 N2 2.702(3) . ? O10 C51 1.252(5) . ? F1 C24 1.323(6) . ? O7 C39 1.259(5) . ? O4 C27 1.256(5) . ? O3 C25 1.258(5) . ? F7 C48 1.341(6) . ? F4 C36 1.308(6) . ? O9 C49 1.265(5) . ? O5 C33 1.364(5) . ? O5 C34 1.439(5) . ? F9 C48 1.333(6) . ? O6 C37 1.254(5) . ? O1 C9 1.344(5) . ? O1 C8 1.450(6) . ? O2 C15 1.357(6) . ? O2 C16 1.449(7) . ? F5 C36 1.308(6) . ? F8 C48 1.330(6) . ? F2 C24 1.322(5) . ? F3 C24 1.314(5) . ? O11 C57 1.346(6) . ? O11 C58 1.444(7) . ? O8 C45 1.354(6) . ? N2 C10 1.336(5) . ? N2 C14 1.332(6) . ? C28 C29 1.389(6) . ? C28 C30 1.389(6) . ? C28 C27 1.493(6) . ? N1 C9 1.268(5) . ? N1 C7 1.481(6) . ? C26 C25 1.379(6) . ? C26 C27 1.410(6) . ? C26 H26 0.9300 . ? C52 C53 1.391(7) . ? C52 C54 1.400(6) . ? C52 C51 1.494(6) . ? N3 C15 1.253(6) . ? N3 C17 1.500(6) . ? C25 C24 1.523(6) . ? C40 C41 1.397(6) . ? C40 C42 1.394(6) . ? C40 C39 1.480(6) . ? C36 F6 1.328(6) . ? C36 C37 1.530(6) . ? C42 C44 1.375(7) . ? C42 H42 0.9300 . ? C29 C32 1.375(6) . ? C29 H29 0.9300 . ? C41 C43 1.365(6) . ? C41 H41 0.9300 . ? C17 C18 1.502(7) . ? C17 C16 1.543(7) . ? C17 H17 0.9800 . ? C30 C31 1.383(6) . ? C30 H30 0.9300 . ? C1 C2 1.366(7) . ? C1 C3 1.360(7) . ? C1 H1 0.9300 . ? C57 C56 1.383(7) . ? C57 C55 1.393(7) . ? C50 C49 1.383(7) . ? C50 C51 1.414(6) . ? C50 H50 0.9300 . ? C10 C11 1.387(6) . ? C10 C9 1.471(6) . ? C4 C6 1.389(7) . ? C4 C2 1.381(7) . ? C4 H4 0.9300 . ? C31 C33 1.382(6) . ? C31 H31 0.9300 . ? C45 C43 1.394(7) . ? C45 C44 1.388(7) . ? C32 C33 1.384(6) . ? C32 H32 0.9300 . ? C56 C54 1.365(6) . ? C56 H56 0.9300 . ? C39 C38 1.422(6) . ? C11 C12 1.392(8) . ? C11 H11 0.9300 . ? C7 C6 1.517(7) . ? C7 C8 1.550(6) . ? C7 H7 0.9800 . ? C2 H2 0.9300 . ? C38 C37 1.377(6) . ? C38 H38 0.9300 . ? C43 H43 0.9300 . ? C34 C35 1.508(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C6 C5 1.369(7) . ? C18 C19 1.376(7) . ? C18 C20 1.381(7) . ? C44 H44 0.9300 . ? C48 C49 1.531(6) . ? C14 C13 1.390(6) . ? C14 C15 1.470(7) . ? C19 C21 1.377(8) . ? C19 H19 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C53 C55 1.375(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C5 C3 1.385(8) . ? C5 H5 0.9300 . ? C55 H55 0.9300 . ? C22 C23 1.367(9) . ? C22 C20 1.386(8) . ? C22 H22 0.9300 . ? C3 H3 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C20 H20 0.9300 . ? C21 C23 1.377(8) . ? C21 H21 0.9300 . ? C23 H23 0.9300 . ? C58 C59 1.449(10) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C12 C13 1.370(8) . ? C12 H12 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C13 H13 0.9300 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? 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 O8 C46 C47 99.6(9) . . ? O8 C46 H46A 111.8 . . ? C47 C46 H46A 111.8 . . ? O8 C46 H46B 111.8 . . ? C47 C46 H46B 111.8 . . ? H46A C46 H46B 109.6 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C47A C46A O8 104.5(7) . . ? C47A C46A H46C 110.8 . . ? O8 C46A H46C 110.8 . . ? C47A C46A H46D 110.8 . . ? O8 C46A H46D 110.8 . . ? H46C C46A H46D 108.9 . . ? C46A C47A H47D 109.5 . . ? C46A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C46A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? O4 Eu01 O10 144.35(10) . . ? O4 Eu01 O9 92.25(11) . . ? O10 Eu01 O9 73.20(10) . . ? O4 Eu01 O7 74.90(10) . . ? O10 Eu01 O7 134.71(11) . . ? O9 Eu01 O7 143.40(10) . . ? O4 Eu01 O3 69.83(9) . . ? O10 Eu01 O3 74.71(10) . . ? O9 Eu01 O3 71.98(10) . . ? O7 Eu01 O3 130.66(10) . . ? O4 Eu01 O6 72.02(10) . . ? O10 Eu01 O6 129.33(10) . . ? O9 Eu01 O6 71.65(10) . . ? O7 Eu01 O6 71.79(10) . . ? O3 Eu01 O6 125.09(9) . . ? O4 Eu01 N3 139.13(11) . . ? O10 Eu01 N3 73.04(11) . . ? O9 Eu01 N3 84.40(11) . . ? O7 Eu01 N3 83.84(11) . . ? O3 Eu01 N3 144.33(11) . . ? O6 Eu01 N3 68.29(11) . . ? O4 Eu01 N1 85.57(11) . . ? O10 Eu01 N1 85.42(11) . . ? O9 Eu01 N1 139.62(11) . . ? O7 Eu01 N1 74.53(11) . . ? O3 Eu01 N1 69.47(10) . . ? O6 Eu01 N1 143.29(10) . . ? N3 Eu01 N1 122.04(11) . . ? O4 Eu01 N2 134.85(10) . . ? O10 Eu01 N2 66.97(10) . . ? O9 Eu01 N2 132.90(11) . . ? O7 Eu01 N2 67.79(10) . . ? O3 Eu01 N2 118.12(9) . . ? O6 Eu01 N2 116.79(10) . . ? N3 Eu01 N2 61.03(11) . . ? N1 Eu01 N2 61.01(11) . . ? C51 O10 Eu01 137.4(3) . . ? C39 O7 Eu01 135.2(3) . . ? C27 O4 Eu01 140.2(3) . . ? C25 O3 Eu01 132.0(3) . . ? C49 O9 Eu01 130.8(3) . . ? C33 O5 C34 118.5(3) . . ? C37 O6 Eu01 131.4(3) . . ? C9 O1 C8 104.9(3) . . ? C15 O2 C16 104.5(4) . . ? C57 O11 C58 118.8(5) . . ? C45 O8 C46 124.3(6) . . ? C45 O8 C46A 112.3(5) . . ? C10 N2 C14 118.0(4) . . ? C10 N2 Eu01 121.1(3) . . ? C14 N2 Eu01 120.8(3) . . ? C29 C28 C30 117.6(4) . . ? C29 C28 C27 118.4(4) . . ? C30 C28 C27 124.0(4) . . ? C9 N1 C7 106.6(4) . . ? C9 N1 Eu01 119.8(3) . . ? C7 N1 Eu01 133.0(3) . . ? C25 C26 C27 122.4(4) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C53 C52 C54 117.4(4) . . ? C53 C52 C51 123.7(4) . . ? C54 C52 C51 118.9(4) . . ? C15 N3 C17 107.2(4) . . ? C15 N3 Eu01 119.9(3) . . ? C17 N3 Eu01 132.8(3) . . ? O3 C25 C26 128.7(4) . . ? O3 C25 C24 113.3(4) . . ? C26 C25 C24 117.9(4) . . ? C41 C40 C42 117.8(4) . . ? C41 C40 C39 119.9(4) . . ? C42 C40 C39 122.3(4) . . ? F1 C24 F2 106.0(4) . . ? F1 C24 F3 106.0(4) . . ? F2 C24 F3 107.0(4) . . ? F1 C24 C25 111.5(4) . . ? F2 C24 C25 114.1(4) . . ? F3 C24 C25 111.7(4) . . ? F4 C36 F5 106.8(5) . . ? F4 C36 F6 102.8(5) . . ? F5 C36 F6 107.0(5) . . ? F4 C36 C37 112.2(4) . . ? F5 C36 C37 115.1(4) . . ? F6 C36 C37 112.0(4) . . ? C44 C42 C40 121.6(4) . . ? C44 C42 H42 119.2 . . ? C40 C42 H42 119.2 . . ? C32 C29 C28 121.4(4) . . ? C32 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C43 C41 C40 121.1(4) . . ? C43 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C18 C17 N3 110.3(4) . . ? C18 C17 C16 113.8(4) . . ? N3 C17 C16 101.4(4) . . ? C18 C17 H17 110.4 . . ? N3 C17 H17 110.4 . . ? C16 C17 H17 110.4 . . ? C31 C30 C28 121.3(4) . . ? C31 C30 H30 119.3 . . ? C28 C30 H30 119.3 . . ? O4 C27 C26 122.0(4) . . ? O4 C27 C28 116.5(4) . . ? C26 C27 C28 121.5(4) . . ? C2 C1 C3 119.4(5) . . ? C2 C1 H1 120.3 . . ? C3 C1 H1 120.3 . . ? O11 C57 C56 117.0(4) . . ? O11 C57 C55 124.6(4) . . ? C56 C57 C55 118.5(4) . . ? C49 C50 C51 123.0(4) . . ? C49 C50 H50 118.5 . . ? C51 C50 H50 118.5 . . ? N2 C10 C11 123.1(4) . . ? N2 C10 C9 113.7(3) . . ? C11 C10 C9 123.2(4) . . ? C6 C4 C2 120.0(5) . . ? C6 C4 H4 120.0 . . ? C2 C4 H4 120.0 . . ? C33 C31 C30 120.0(4) . . ? C33 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? O8 C45 C43 115.9(5) . . ? O8 C45 C44 124.7(5) . . ? C43 C45 C44 119.3(5) . . ? C33 C32 C29 120.2(4) . . ? C33 C32 H32 119.9 . . ? C29 C32 H32 119.9 . . ? C57 C56 C54 121.4(5) . . ? C57 C56 H56 119.3 . . ? C54 C56 H56 119.3 . . ? O7 C39 C38 123.2(4) . . ? O7 C39 C40 117.9(4) . . ? C38 C39 C40 118.9(4) . . ? C10 C11 C12 117.8(5) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? N1 C7 C6 114.0(4) . . ? N1 C7 C8 102.9(4) . . ? C6 C7 C8 111.9(4) . . ? N1 C7 H7 109.3 . . ? C6 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? N1 C9 O1 119.8(4) . . ? N1 C9 C10 123.9(4) . . ? O1 C9 C10 116.3(4) . . ? O5 C33 C32 115.9(4) . . ? O5 C33 C31 124.8(4) . . ? C32 C33 C31 119.2(4) . . ? C1 C2 C4 120.6(5) . . ? C1 C2 H2 119.7 . . ? C4 C2 H2 119.7 . . ? C37 C38 C39 123.3(4) . . ? C37 C38 H38 118.4 . . ? C39 C38 H38 118.4 . . ? C41 C43 C45 120.4(4) . . ? C41 C43 H43 119.8 . . ? C45 C43 H43 119.8 . . ? O5 C34 C35 111.5(4) . . ? O5 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? O5 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C4 C6 C5 119.0(5) . . ? C4 C6 C7 120.9(4) . . ? C5 C6 C7 120.2(4) . . ? C19 C18 C20 118.1(5) . . ? C19 C18 C17 121.5(5) . . ? C20 C18 C17 120.4(5) . . ? C42 C44 C45 119.7(5) . . ? C42 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? F9 C48 F8 106.7(4) . . ? F9 C48 F7 105.9(4) . . ? F8 C48 F7 106.6(5) . . ? F9 C48 C49 112.4(4) . . ? F8 C48 C49 114.1(4) . . ? F7 C48 C49 110.6(4) . . ? N2 C14 C13 123.0(5) . . ? N2 C14 C15 113.5(4) . . ? C13 C14 C15 123.5(5) . . ? C21 C19 C18 121.0(5) . . ? C21 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? O2 C16 C17 104.6(4) . . ? O2 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? O2 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C52 C53 C55 121.7(5) . . ? C52 C53 H53 119.2 . . ? C55 C53 H53 119.2 . . ? C56 C54 C52 121.0(4) . . ? C56 C54 H54 119.5 . . ? C52 C54 H54 119.5 . . ? C6 C5 C3 120.2(5) . . ? C6 C5 H5 119.9 . . ? C3 C5 H5 119.9 . . ? N3 C15 O2 119.0(5) . . ? N3 C15 C14 124.0(4) . . ? O2 C15 C14 116.9(4) . . ? C53 C55 C57 120.2(5) . . ? C53 C55 H55 119.9 . . ? C57 C55 H55 119.9 . . ? C23 C22 C20 120.2(5) . . ? C23 C22 H22 119.9 . . ? C20 C22 H22 119.9 . . ? O10 C51 C50 123.7(4) . . ? O10 C51 C52 116.3(4) . . ? C50 C51 C52 120.0(4) . . ? O9 C49 C50 129.8(4) . . ? O9 C49 C48 112.8(4) . . ? C50 C49 C48 117.4(4) . . ? C1 C3 C5 120.9(5) . . ? C1 C3 H3 119.6 . . ? C5 C3 H3 119.6 . . ? O6 C37 C38 130.4(4) . . ? O6 C37 C36 112.6(4) . . ? C38 C37 C36 117.0(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C18 C20 C22 120.9(5) . . ? C18 C20 H20 119.5 . . ? C22 C20 H20 119.5 . . ? C19 C21 C23 120.4(5) . . ? C19 C21 H21 119.8 . . ? C23 C21 H21 119.8 . . ? C22 C23 C21 119.3(6) . . ? C22 C23 H23 120.4 . . ? C21 C23 H23 120.4 . . ? O11 C58 C59 109.4(6) . . ? O11 C58 H58A 109.8 . . ? C59 C58 H58A 109.8 . . ? O11 C58 H58B 109.8 . . ? C59 C58 H58B 109.8 . . ? H58A C58 H58B 108.2 . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? O1 C8 C7 104.6(4) . . ? O1 C8 H8A 110.8 . . ? C7 C8 H8A 110.8 . . ? O1 C8 H8B 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? C12 C13 C14 118.4(5) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? _refine_diff_density_max 0.675 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.046 _shelx_res_file ; TITL PhEuOEt_0m_a.res in P2(1)2(1)2(1) PhEuOEt_0m_a.res created by SHELXL-2016/6 at 17:24:45 on 25-Jun-2020 CELL 0.71073 14.8445 18.8821 20.0144 90.000 90.000 90.000 ZERR 4.000 0.0076 0.0096 0.0100 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H Eu F N O UNIT 236 196 4 36 12 44 L.S. 50 ACTA BOND $H FMAP 2 PLAN 20 EADP C46 C46A C47 C47A SADI O8 C46 O8 C46A C46 C47 C46A C47A ISOR 0.001 C46 C47 TEMP 23.000 WGHT 0.039200 3.320300 FVAR 0.18027 0.47263 PART 1 C46 1 -0.284730 0.239671 0.249879 21.00000 0.04942 0.05045 = 0.05086 0.00097 0.00022 -0.00356 AFIX 23 H46A 2 -0.263242 0.209476 0.285703 21.00000 -1.20000 H46B 2 -0.298175 0.211050 0.210888 21.00000 -1.20000 AFIX 0 C47 1 -0.363866 0.283145 0.271020 21.00000 0.04942 0.05045 = 0.05086 0.00097 0.00022 -0.00356 AFIX 137 H47A 2 -0.345711 0.315670 0.305339 21.00000 -1.50000 H47B 2 -0.410232 0.252580 0.287948 21.00000 -1.50000 H47C 2 -0.386496 0.309114 0.233354 21.00000 -1.50000 AFIX 0 PART 2 C46A 1 -0.306983 0.276429 0.274857 -21.00000 0.04942 0.05045 = 0.05086 0.00097 0.00022 -0.00356 AFIX 23 H46C 2 -0.297258 0.234065 0.301305 -21.00000 -1.20000 H46D 2 -0.324080 0.314885 0.304384 -21.00000 -1.20000 AFIX 0 C47A 1 -0.377719 0.264142 0.222934 -21.00000 0.04942 0.05045 = 0.05086 0.00097 0.00022 -0.00356 AFIX 137 H47D 2 -0.395394 0.308645 0.203799 -21.00000 -1.50000 H47E 2 -0.429118 0.241918 0.243126 -21.00000 -1.50000 H47F 2 -0.354053 0.233977 0.188544 -21.00000 -1.50000 AFIX 0 PART 0 EU01 3 0.232922 0.515749 0.396221 11.00000 0.02448 0.02425 = 0.01854 -0.00177 0.00160 -0.00196 O10 6 0.364455 0.568835 0.351990 11.00000 0.03255 0.03607 = 0.02668 -0.00299 -0.00033 -0.00712 F1 4 0.286185 0.758922 0.459054 11.00000 0.04014 0.03739 = 0.10763 -0.01278 0.00331 -0.00852 O7 6 0.129556 0.426126 0.357859 11.00000 0.03279 0.02744 = 0.02511 -0.00172 0.00256 -0.00640 O4 6 0.097609 0.537749 0.454608 11.00000 0.03027 0.03011 = 0.02770 -0.00526 0.00693 -0.00034 O3 6 0.212360 0.641593 0.411905 11.00000 0.03654 0.02794 = 0.02668 -0.00337 0.00496 -0.00199 F7 4 0.336286 0.656994 0.585806 11.00000 0.08810 0.05716 = 0.04905 -0.02072 0.00910 -0.00567 F4 4 0.262063 0.323635 0.568989 11.00000 0.06525 0.10853 = 0.08610 0.06383 -0.01980 -0.00211 O9 6 0.322559 0.551487 0.489049 11.00000 0.03942 0.03613 = 0.02361 -0.00180 -0.00135 -0.00826 O5 6 -0.234611 0.486063 0.640096 11.00000 0.03546 0.04946 = 0.03911 -0.00510 0.01386 -0.00734 F9 4 0.419088 0.567237 0.606744 11.00000 0.06769 0.09361 = 0.02788 0.00291 -0.01246 -0.00416 O6 6 0.218438 0.426520 0.483702 11.00000 0.03488 0.03257 = 0.02882 0.00541 -0.00410 -0.00216 O1 6 0.135970 0.587468 0.180034 11.00000 0.05890 0.05664 = 0.02147 0.00863 -0.00276 -0.00135 O2 6 0.422355 0.329492 0.322467 11.00000 0.04935 0.04907 = 0.07204 -0.02019 -0.00032 0.01881 F5 4 0.134107 0.276711 0.561853 11.00000 0.12131 0.08595 = 0.07581 0.05665 -0.04745 -0.06138 F8 4 0.478527 0.661951 0.568438 11.00000 0.09051 0.12171 = 0.04276 -0.03032 0.00309 -0.06444 F2 4 0.170185 0.785226 0.514872 11.00000 0.10898 0.04824 = 0.06659 -0.03309 0.04102 -0.02649 F3 4 0.168477 0.791804 0.409172 11.00000 0.09858 0.03765 = 0.08373 0.02746 -0.03477 -0.00789 O11 6 0.681051 0.676966 0.173320 11.00000 0.04066 0.05899 = 0.05935 0.00792 0.02123 -0.00997 O8 6 -0.221629 0.295654 0.234719 11.00000 0.05043 0.08528 = 0.06858 0.03839 -0.02663 -0.04110 N2 5 0.274335 0.468691 0.272495 11.00000 0.02408 0.03834 = 0.02656 -0.00751 0.00150 -0.00855 C28 1 -0.020034 0.563671 0.528503 11.00000 0.02221 0.03289 = 0.02415 0.00181 -0.00008 0.00549 N1 5 0.149438 0.572144 0.291583 11.00000 0.03778 0.02842 = 0.02104 -0.00131 -0.00261 -0.00376 C26 1 0.094655 0.654922 0.491524 11.00000 0.02970 0.02916 = 0.02334 -0.00426 0.00244 0.00670 AFIX 43 H26 2 0.067191 0.687447 0.519854 11.00000 -1.20000 AFIX 0 C52 1 0.501026 0.622325 0.323281 11.00000 0.03104 0.03373 = 0.03536 0.00197 -0.00301 -0.00810 N3 5 0.354154 0.414222 0.383146 11.00000 0.02544 0.03509 = 0.03430 -0.00464 0.00050 0.00310 C25 1 0.167265 0.676557 0.453670 11.00000 0.03154 0.02759 = 0.01775 -0.00013 -0.00306 0.00275 C40 1 -0.001328 0.357009 0.347984 11.00000 0.03081 0.02331 = 0.03255 -0.00097 0.00183 -0.00222 C24 1 0.197326 0.753427 0.459575 11.00000 0.03848 0.03095 = 0.02611 -0.00434 0.00253 0.00219 C36 1 0.177104 0.336979 0.557089 11.00000 0.04483 0.05132 = 0.03983 0.01324 -0.00378 -0.00877 F6 4 0.153123 0.375863 0.609426 11.00000 0.16047 0.10261 = 0.03238 0.01221 0.01547 0.01724 C42 1 -0.079178 0.333064 0.379706 11.00000 0.03899 0.03837 = 0.04058 0.01271 0.00220 -0.00850 AFIX 43 H42 2 -0.080526 0.330790 0.426112 11.00000 -1.20000 AFIX 0 C29 1 -0.047576 0.493444 0.525643 11.00000 0.03253 0.03258 = 0.03030 -0.00372 0.00541 0.00129 AFIX 43 H29 2 -0.016898 0.462038 0.498011 11.00000 -1.20000 AFIX 0 C41 1 -0.001558 0.359879 0.278233 11.00000 0.02894 0.02655 = 0.03430 0.00035 0.00090 -0.00469 AFIX 43 H41 2 0.049211 0.376376 0.255894 11.00000 -1.20000 AFIX 0 C17 1 0.410032 0.373982 0.432694 11.00000 0.03534 0.04128 = 0.05446 0.00694 -0.00064 0.00856 AFIX 13 H17 2 0.373106 0.359547 0.470930 11.00000 -1.20000 AFIX 0 C30 1 -0.069925 0.609675 0.568040 11.00000 0.03781 0.02980 = 0.03576 0.00126 0.00527 0.00358 AFIX 43 H30 2 -0.054591 0.657414 0.569209 11.00000 -1.20000 AFIX 0 C27 1 0.060559 0.585280 0.488823 11.00000 0.02772 0.03559 = 0.01559 -0.00025 -0.00239 0.00361 C1 1 -0.163791 0.600152 0.391070 11.00000 0.04176 0.05973 = 0.05245 0.00395 -0.00712 0.00307 AFIX 43 H1 2 -0.217683 0.593887 0.414015 11.00000 -1.20000 AFIX 0 C57 1 0.624995 0.661109 0.224020 11.00000 0.03435 0.03584 = 0.04809 0.00673 0.00784 -0.00256 C50 1 0.445286 0.617433 0.442054 11.00000 0.03808 0.04250 = 0.03054 -0.00650 -0.00191 -0.01720 AFIX 43 H50 2 0.493807 0.646044 0.453693 11.00000 -1.20000 AFIX 0 C10 1 0.239480 0.499176 0.218093 11.00000 0.03209 0.04492 = 0.02178 -0.00686 0.00342 -0.01401 C4 1 -0.040113 0.552253 0.329758 11.00000 0.04162 0.02984 = 0.04882 -0.00330 -0.01591 0.00097 AFIX 43 H4 2 -0.010829 0.513256 0.311488 11.00000 -1.20000 AFIX 0 C31 1 -0.141948 0.585909 0.605701 11.00000 0.04008 0.03912 = 0.03478 0.00151 0.01057 0.00941 AFIX 43 H31 2 -0.174486 0.617570 0.631865 11.00000 -1.20000 AFIX 0 C45 1 -0.152214 0.314683 0.274755 11.00000 0.03404 0.04013 = 0.06082 0.01972 -0.01313 -0.01450 C32 1 -0.119226 0.469345 0.562785 11.00000 0.03547 0.03674 = 0.03235 -0.00235 0.00165 -0.00240 AFIX 43 H32 2 -0.136605 0.422125 0.559892 11.00000 -1.20000 AFIX 0 C56 1 0.545587 0.626944 0.207753 11.00000 0.03766 0.05178 = 0.03440 -0.00106 0.00626 -0.00317 AFIX 43 H56 2 0.533306 0.616714 0.163222 11.00000 -1.20000 AFIX 0 C39 1 0.078529 0.381719 0.385605 11.00000 0.03044 0.01968 = 0.03080 -0.00295 0.00265 -0.00084 C11 1 0.263705 0.480162 0.153593 11.00000 0.04294 0.07785 = 0.02613 -0.01020 0.00564 -0.00819 AFIX 43 H11 2 0.239362 0.503238 0.116726 11.00000 -1.20000 AFIX 0 C7 1 0.083718 0.630644 0.284468 11.00000 0.05194 0.02508 = 0.02839 0.00327 -0.00833 0.00036 AFIX 13 H7 2 0.111773 0.675081 0.298859 11.00000 -1.20000 AFIX 0 C9 1 0.173098 0.554794 0.232970 11.00000 0.03848 0.03805 = 0.02013 0.00343 -0.00375 -0.01398 C33 1 -0.165588 0.515120 0.604469 11.00000 0.02639 0.04065 = 0.02817 0.00420 0.00024 -0.00104 C2 1 -0.120494 0.543391 0.363498 11.00000 0.04181 0.04669 = 0.05929 0.00403 -0.01967 -0.00632 AFIX 43 H2 2 -0.145364 0.498383 0.367481 11.00000 -1.20000 AFIX 0 C38 1 0.094904 0.353562 0.450381 11.00000 0.04109 0.02576 = 0.03143 0.00423 0.00275 -0.00860 AFIX 43 H38 2 0.057368 0.317749 0.465954 11.00000 -1.20000 AFIX 0 C43 1 -0.074991 0.338892 0.242320 11.00000 0.04256 0.03029 = 0.03812 0.00617 -0.00256 -0.00483 AFIX 43 H43 2 -0.073527 0.340746 0.195899 11.00000 -1.20000 AFIX 0 C34 1 -0.271231 0.525500 0.695305 11.00000 0.03985 0.05436 = 0.04405 0.00029 0.01767 -0.00143 AFIX 23 H34A 2 -0.327290 0.503823 0.709512 11.00000 -1.20000 H34B 2 -0.284373 0.573451 0.680903 11.00000 -1.20000 AFIX 0 C6 1 -0.003030 0.619415 0.323123 11.00000 0.04243 0.03053 = 0.02615 0.00112 -0.01407 0.00498 C18 1 0.488164 0.418286 0.455651 11.00000 0.03043 0.05256 = 0.03946 0.00482 -0.00407 0.00792 C44 1 -0.154012 0.312726 0.344080 11.00000 0.03376 0.05217 = 0.05436 0.02374 -0.00055 -0.01572 AFIX 43 H44 2 -0.205604 0.297725 0.366320 11.00000 -1.20000 AFIX 0 C48 1 0.407028 0.619852 0.563231 11.00000 0.05150 0.05987 = 0.03369 -0.00736 -0.00302 -0.02217 C14 1 0.333607 0.416503 0.263879 11.00000 0.02642 0.04801 = 0.03740 -0.01765 0.00239 -0.00125 C19 1 0.550497 0.444583 0.411190 11.00000 0.04046 0.07391 = 0.04285 -0.00103 -0.00089 -0.00393 AFIX 43 H19 2 0.543105 0.436254 0.365722 11.00000 -1.20000 AFIX 0 C16 1 0.437885 0.308671 0.391188 11.00000 0.04903 0.05133 = 0.08353 -0.00296 -0.01428 0.01612 AFIX 23 H16A 2 0.500830 0.297217 0.398437 11.00000 -1.20000 H16B 2 0.401462 0.267858 0.402872 11.00000 -1.20000 AFIX 0 C53 1 0.581150 0.656539 0.339301 11.00000 0.04679 0.05951 = 0.03547 0.00362 -0.00518 -0.01560 AFIX 43 H53 2 0.593744 0.666561 0.383826 11.00000 -1.20000 AFIX 0 C54 1 0.484833 0.607916 0.255715 11.00000 0.03017 0.04494 = 0.04007 -0.00493 0.00174 -0.00947 AFIX 43 H54 2 0.431918 0.585049 0.243328 11.00000 -1.20000 AFIX 0 C5 1 -0.046728 0.675886 0.351202 11.00000 0.05281 0.03082 = 0.04876 -0.00109 -0.01057 0.00339 AFIX 43 H5 2 -0.022190 0.721060 0.347794 11.00000 -1.20000 AFIX 0 C15 1 0.368514 0.387394 0.326889 11.00000 0.02618 0.03775 = 0.05244 -0.00916 0.00311 0.00308 C55 1 0.642216 0.675921 0.290977 11.00000 0.03567 0.05559 = 0.05564 0.00847 -0.00444 -0.01747 AFIX 43 H55 2 0.695138 0.698973 0.303038 11.00000 -1.20000 AFIX 0 C22 1 0.573589 0.471439 0.544766 11.00000 0.06609 0.10602 = 0.04341 -0.00398 -0.02010 -0.00067 AFIX 43 H22 2 0.580315 0.481123 0.590052 11.00000 -1.20000 AFIX 0 C51 1 0.432090 0.600963 0.373828 11.00000 0.03321 0.02741 = 0.03231 -0.00181 -0.00060 -0.00406 C49 1 0.389353 0.592949 0.492285 11.00000 0.03689 0.03830 = 0.02729 -0.00242 -0.00510 -0.00211 C3 1 -0.127383 0.665919 0.384669 11.00000 0.05526 0.05107 = 0.05297 -0.00690 -0.00492 0.01049 AFIX 43 H3 2 -0.157053 0.704697 0.403012 11.00000 -1.20000 AFIX 0 C37 1 0.163535 0.376664 0.491186 11.00000 0.03753 0.02750 = 0.02814 0.00337 0.00397 0.00382 C35 1 -0.206703 0.527750 0.753429 11.00000 0.07641 0.05278 = 0.03753 0.00353 0.01496 0.00008 AFIX 137 H35A 2 -0.194898 0.480409 0.768570 11.00000 -1.50000 H35B 2 -0.232800 0.554767 0.789156 11.00000 -1.50000 H35C 2 -0.151318 0.549508 0.739575 11.00000 -1.50000 AFIX 0 C20 1 0.500445 0.432186 0.522789 11.00000 0.04959 0.08018 = 0.03921 0.01242 -0.00412 0.00340 AFIX 43 H20 2 0.459075 0.414975 0.553676 11.00000 -1.20000 AFIX 0 C21 1 0.623620 0.483025 0.432992 11.00000 0.04039 0.09706 = 0.05736 0.00743 -0.00177 -0.01077 AFIX 43 H21 2 0.665019 0.500373 0.402195 11.00000 -1.20000 AFIX 0 C23 1 0.635867 0.495958 0.500078 11.00000 0.04797 0.10474 = 0.06721 0.00168 -0.02077 -0.01569 AFIX 43 H23 2 0.685942 0.521091 0.514827 11.00000 -1.20000 AFIX 0 C58 1 0.772575 0.697308 0.188495 11.00000 0.05339 0.10039 = 0.09341 0.00529 0.02681 -0.02490 AFIX 23 H58A 2 0.797994 0.664829 0.220969 11.00000 -1.20000 H58B 2 0.773376 0.744539 0.207547 11.00000 -1.20000 AFIX 0 C12 1 0.325633 0.425421 0.145859 11.00000 0.04890 0.10615 = 0.03267 -0.03088 0.01009 -0.00114 AFIX 43 H12 2 0.343305 0.411168 0.103356 11.00000 -1.20000 AFIX 0 C8 1 0.067199 0.633212 0.208042 11.00000 0.07278 0.04350 = 0.03653 0.00925 -0.00980 0.00443 AFIX 23 H8A 2 0.007465 0.615874 0.197157 11.00000 -1.20000 H8B 2 0.073375 0.681165 0.191273 11.00000 -1.20000 AFIX 0 C13 1 0.360397 0.392664 0.201221 11.00000 0.04241 0.08071 = 0.04943 -0.03058 0.01117 0.00666 AFIX 43 H13 2 0.400938 0.355381 0.197000 11.00000 -1.20000 AFIX 0 C59 1 0.825764 0.695982 0.127823 11.00000 0.06643 0.10475 = 0.18172 0.03007 0.05741 -0.00907 AFIX 137 H59A 2 0.826927 0.648693 0.110229 11.00000 -1.50000 H59B 2 0.886118 0.711049 0.137561 11.00000 -1.50000 H59C 2 0.799495 0.727326 0.095471 11.00000 -1.50000 AFIX 0 HKLF 4 REM PhEuOEt_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0224 for 9258 Fo > 4sig(Fo) and 0.0258 for all 9943 data REM 753 parameters refined using 18 restraints END WGHT 0.0099 0.0000 REM Highest difference peak 0.675, deepest hole -0.327, 1-sigma level 0.046 Q1 1 0.2348 0.4625 0.3972 11.00000 0.05 0.68 Q2 1 0.8368 0.6815 0.1904 11.00000 0.05 0.35 Q3 1 0.1035 0.3375 0.5983 11.00000 0.05 0.34 Q4 1 0.2273 0.2783 0.5371 11.00000 0.05 0.31 Q5 1 0.2176 0.3585 0.5990 11.00000 0.05 0.31 Q6 1 0.7416 0.7456 0.1748 11.00000 0.05 0.30 Q7 1 0.2589 0.5629 0.4100 11.00000 0.05 0.29 Q8 1 -0.3536 0.2364 0.2109 11.00000 0.05 0.28 Q9 1 0.2081 0.2639 0.5282 11.00000 0.05 0.27 Q10 1 0.2527 0.5172 0.4514 11.00000 0.05 0.25 Q11 1 0.2183 0.7573 0.5224 11.00000 0.05 0.25 Q12 1 -0.2208 0.2589 0.2253 11.00000 0.05 0.25 Q13 1 0.7008 0.6993 0.2088 11.00000 0.05 0.23 Q14 1 0.1309 0.7990 0.4519 11.00000 0.05 0.22 Q15 1 -0.2271 0.2813 0.2047 11.00000 0.05 0.22 Q16 1 0.2378 0.4782 0.4988 11.00000 0.05 0.21 Q17 1 0.2638 0.4828 0.3084 11.00000 0.05 0.21 Q18 1 0.1865 0.5559 0.3926 11.00000 0.05 0.21 Q19 1 0.2560 0.4868 0.2463 11.00000 0.05 0.20 Q20 1 -0.0183 0.3765 0.3186 11.00000 0.05 0.20 ; _shelx_res_checksum 15849 _shelx_hkl_file ; -2 0 0 2899.81 126.69 -3 0 0 -0.50 0.70 -4 0 0 23.90 2.20 -4 0 0 29.40 1.60 -5 0 0 1.10 0.50 -5 0 0 0.30 0.80 -6 0 0 184.28 9.80 -6 0 0 195.18 8.70 -7 0 0 1.20 0.60 -7 0 0 2.20 1.30 -8 0 0 577.04 27.10 -8 0 0 578.84 25.40 -9 0 0 -1.00 1.20 -10 0 0 381.66 19.20 -11 0 0 -0.70 1.50 -12 0 0 223.78 13.00 -13 0 0 -0.20 2.10 -14 0 0 82.09 7.30 -15 0 0 2.60 2.80 -16 0 0 0.10 2.80 -17 0 0 -1.40 3.00 -1 1 0 5600.94 254.47 -1 -1 0 5418.86 256.47 -2 1 0 167.28 7.70 -2 -1 0 174.08 7.90 -3 -1 0 814.52 35.60 -3 1 0 798.62 35.20 -3 1 0 809.02 35.60 -4 -1 0 16.80 1.80 -4 1 0 16.20 1.90 -4 1 0 19.60 1.50 -5 1 0 579.94 25.90 -5 -1 0 549.95 25.80 -5 1 0 578.34 25.10 -6 -1 0 1.60 1.10 -6 1 0 1.00 1.10 -6 1 0 1.80 0.70 -7 1 0 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-14 4 0 70.99 6.80 -14 -4 0 69.59 6.80 -15 4 0 46.80 6.30 -15 -4 0 36.90 5.80 -16 4 0 9.80 3.60 -16 -4 0 7.30 3.40 -17 -4 0 7.60 3.60 -17 4 0 8.90 3.70 0 5 0 0.30 0.90 0 -5 0 1.20 0.80 -1 5 0 1129.59 52.39 -1 -5 0 1205.78 52.29 -1 -5 0 1228.58 52.29 1 5 0 1208.88 52.39 -2 -5 0 473.35 20.90 2 5 0 461.55 20.70 -2 5 0 440.56 21.00 -2 -5 0 462.75 21.00 3 5 0 3444.06 147.59 -3 5 0 3421.06 148.69 -3 -5 0 3282.47 148.29 -3 -5 0 3430.06 147.49 -4 -5 0 495.95 23.70 -4 5 0 532.45 23.30 4 5 0 506.05 22.60 -4 -5 0 493.25 23.20 -5 -5 0 2508.85 112.49 -5 -5 0 2596.14 111.89 -5 5 0 2524.75 111.79 5 5 0 2620.64 111.09 6 5 0 46.40 2.60 -6 5 0 48.60 3.60 -6 -5 0 43.00 3.70 -7 5 0 642.04 30.00 -7 -5 0 677.43 30.50 -8 5 0 0.30 1.20 -8 5 0 0.10 1.20 -8 -5 0 -0.80 1.30 -9 -5 0 78.19 6.00 -9 5 0 84.29 5.40 -9 5 0 78.79 6.10 -10 5 0 51.29 4.70 -10 -5 0 44.90 4.50 -10 5 0 49.90 4.00 -11 -5 0 23.80 3.70 -11 5 0 21.50 3.70 -12 5 0 27.10 4.30 -12 -5 0 27.10 4.40 -13 -5 0 70.49 6.70 -13 5 0 67.19 6.70 -14 -5 0 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-13 6 0 100.79 8.10 -13 -6 0 104.89 8.30 -14 6 0 53.09 6.70 -14 -6 0 44.40 6.20 -15 -6 0 114.09 9.00 -15 6 0 97.69 8.90 -16 6 0 2.80 3.10 -16 -6 0 3.40 3.00 -17 6 0 60.49 8.00 -17 -6 0 76.49 7.80 0 7 0 1.80 1.10 0 -7 0 3.30 1.10 -1 7 0 788.92 35.10 -1 -7 0 769.12 34.80 1 7 0 774.22 34.90 -1 -7 0 777.22 34.80 2 7 0 560.04 25.40 -2 7 0 558.54 25.70 -2 -7 0 556.34 25.50 -2 -7 0 552.84 25.40 3 7 0 1586.84 68.79 -3 7 0 1558.84 69.29 -3 -7 0 1547.45 69.19 -3 -7 0 1578.74 68.99 -4 -7 0 100.49 6.00 -4 7 0 104.79 6.30 4 7 0 98.59 5.60 -4 -7 0 99.89 6.50 -5 -7 0 848.62 39.00 -5 7 0 862.11 39.20 5 7 0 888.41 38.30 -5 -7 0 853.11 39.70 6 7 0 189.68 9.30 -6 -7 0 188.48 11.10 -6 -7 0 192.28 10.40 -6 7 0 200.28 10.50 -7 -7 0 141.39 8.50 -7 -7 0 142.19 9.40 -7 7 0 154.48 8.50 7 7 0 144.39 7.20 -8 7 0 664.83 30.60 -8 -7 0 666.83 30.90 -8 -7 0 636.14 31.80 -9 -7 0 18.80 3.90 -9 -7 0 23.20 3.60 -9 7 0 24.30 3.30 -10 7 0 78.89 5.90 -10 -7 0 88.69 6.70 -10 7 0 80.99 6.50 -10 -7 0 83.69 7.60 -11 7 0 24.60 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490.45 23.50 -8 -10 0 135.69 8.80 -8 10 0 150.78 9.20 -8 -10 0 126.09 9.60 -9 -10 0 408.66 22.00 -9 -10 0 397.46 20.90 -9 10 0 428.46 21.00 -10 -10 0 330.57 18.60 -10 -10 0 347.57 20.20 -10 10 0 388.36 18.90 -11 10 0 203.78 12.00 -11 -10 0 200.78 13.90 -11 -10 0 202.18 12.40 -12 -10 0 16.60 4.00 -12 -10 0 26.30 5.70 -12 10 0 15.70 3.70 -13 -10 0 133.19 11.50 -13 10 0 130.49 9.60 -13 -10 0 108.69 8.90 -14 10 0 -0.90 2.20 -14 -10 0 -0.80 2.80 -14 -10 0 -1.10 3.90 -15 -10 0 95.49 11.40 -15 10 0 83.29 8.10 0 11 0 -1.50 1.40 -1 -11 0 73.19 5.20 -1 11 0 70.99 5.50 1 11 0 75.29 5.50 -2 -11 0 48.70 4.20 2 11 0 50.39 4.40 -2 11 0 48.80 4.70 -2 -11 0 50.49 4.20 -3 11 0 214.68 11.30 -3 -11 0 188.68 10.60 -3 -11 0 187.88 10.70 3 11 0 191.58 10.60 -4 11 0 323.57 16.20 -4 -11 0 298.27 15.80 4 11 0 295.47 15.30 -4 -11 0 307.47 15.60 -5 -11 0 279.67 14.60 -5 11 0 262.57 14.50 -5 -11 0 273.57 14.10 5 11 0 257.27 13.50 -6 11 0 226.28 12.80 -6 -11 0 227.88 13.10 6 11 0 227.38 11.80 -6 -11 0 227.68 12.60 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370.36 19.30 -11 -9 2 373.26 21.10 -12 -9 -2 54.99 8.00 -12 9 2 48.10 5.90 -12 -9 -2 49.40 5.80 -12 -9 2 34.60 5.30 -12 -9 2 38.40 6.40 -12 9 -2 40.40 5.50 -13 -9 -2 88.69 7.60 -13 -9 -2 82.69 9.90 -13 9 2 95.99 7.90 -13 9 -2 90.79 7.90 -13 -9 2 83.09 7.90 -13 -9 2 76.89 9.20 -14 9 2 4.80 3.00 -14 -9 -2 1.70 2.90 -14 -9 -2 2.90 4.40 -14 -9 2 5.50 3.20 -14 9 -2 3.90 2.80 -14 -9 2 7.90 4.40 -15 9 2 84.09 8.30 -15 -9 -2 76.79 7.40 -15 -9 -2 81.89 10.60 -15 -9 2 94.69 10.90 -15 9 -2 75.59 7.60 -15 -9 2 81.69 8.30 -16 -9 -2 4.80 5.40 -16 9 2 4.00 3.70 -16 -9 -2 3.60 3.20 -16 9 -2 4.40 3.40 -16 -9 2 2.30 3.60 -16 -9 2 -2.10 4.00 0 10 -2 4.10 1.90 0 10 2 2.40 1.60 0 -10 2 2.60 1.50 -1 10 2 405.16 19.50 1 10 -2 432.96 19.30 1 10 2 360.26 19.00 -1 10 -2 379.86 19.30 -1 -10 2 389.86 19.10 -2 10 2 75.59 5.30 -2 -10 -2 64.89 5.20 2 10 -2 77.89 5.10 -2 -10 -2 71.99 4.80 -2 10 -2 60.09 5.10 -2 -10 2 65.39 4.50 2 10 2 55.99 4.80 -2 -10 2 58.09 4.70 -3 -10 -2 56.29 4.10 -3 10 2 62.69 4.90 -3 -10 -2 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76.79 7.80 2 8 21 64.39 8.60 -2 -8 21 74.39 7.70 -3 8 21 42.80 6.90 3 -8 21 36.60 6.10 3 8 21 38.80 6.60 -3 -8 21 43.50 6.20 4 -8 21 47.60 7.00 -4 8 21 41.40 6.80 4 8 21 49.20 7.40 -4 -8 21 40.60 6.10 5 -8 21 16.90 4.50 -5 8 21 21.20 5.40 5 8 21 14.40 4.60 -5 -8 21 17.10 4.30 0 9 21 11.80 4.50 0 -9 21 19.40 4.80 1 -9 21 104.09 9.30 -1 9 21 96.69 9.80 -1 -9 21 120.19 9.60 1 9 21 121.29 10.90 2 -9 21 13.40 4.30 -2 9 21 9.80 4.40 2 9 21 17.00 4.80 -2 -9 21 18.40 4.70 -3 9 21 93.89 9.50 3 -9 21 83.69 8.60 -3 -9 21 77.19 7.90 3 9 21 95.99 9.70 -4 9 21 28.20 5.90 4 -9 21 25.60 5.70 -4 -9 21 36.50 5.70 4 9 21 33.40 6.40 0 10 21 67.09 9.10 0 -10 21 82.99 8.30 -1 10 21 22.50 5.90 1 -10 21 17.70 4.70 -1 -10 21 21.20 4.80 1 10 21 23.30 5.60 2 -10 21 108.69 9.60 -2 10 21 110.69 10.30 2 10 21 128.79 11.20 -2 -10 21 108.89 9.60 0 0 22 10.70 4.30 -1 0 22 336.17 19.80 1 0 22 323.77 19.70 -2 0 22 -1.60 3.00 2 0 22 0.00 3.20 3 0 22 203.08 13.80 -3 0 22 175.18 13.20 -4 0 22 5.00 3.60 4 0 22 10.10 4.20 5 0 22 163.28 12.40 -5 0 22 151.68 11.80 -6 0 22 19.30 4.80 6 0 22 14.20 4.70 0 1 22 220.28 15.10 0 -1 22 250.27 15.70 -1 1 22 -0.70 3.10 1 -1 22 1.20 3.30 -1 -1 22 -1.80 2.60 1 1 22 2.50 3.40 2 -1 22 201.88 14.00 -2 1 22 200.68 13.90 2 1 22 218.78 14.60 -2 -1 22 194.68 13.90 -3 1 22 18.80 4.80 3 -1 22 12.30 4.60 3 1 22 18.80 5.10 -3 -1 22 11.00 3.90 -4 1 22 181.98 13.00 4 -1 22 184.08 13.50 4 1 22 194.98 13.80 -4 -1 22 181.28 13.10 -5 1 22 11.10 4.10 5 -1 22 15.30 4.60 -5 -1 22 8.60 3.70 5 1 22 13.60 4.40 -6 1 22 97.39 9.30 6 -1 22 96.89 9.70 -6 -1 22 108.99 9.50 6 1 22 112.19 10.10 0 2 22 10.30 3.90 0 -2 22 8.30 3.70 1 -2 22 323.97 19.20 -1 2 22 307.47 19.10 -1 -2 22 322.87 19.30 1 2 22 332.57 19.50 -2 2 22 14.40 4.50 2 -2 22 16.40 4.90 -2 -2 22 11.80 4.30 2 2 22 8.10 4.20 3 -2 22 183.08 13.30 -3 2 22 195.98 13.70 -3 -2 22 198.18 13.50 3 2 22 189.38 13.90 4 -2 22 4.30 3.60 -4 2 22 10.60 3.90 4 2 22 2.00 3.60 -4 -2 22 5.80 3.30 5 -2 22 108.49 9.70 -5 2 22 105.59 9.80 5 2 22 118.69 10.10 -5 -2 22 104.09 9.50 -6 2 22 -0.20 3.10 6 -2 22 6.40 4.00 -6 -2 22 5.00 3.40 6 2 22 3.00 3.60 0 -3 22 189.58 13.30 0 3 22 180.98 13.20 -1 3 22 11.50 4.00 1 -3 22 8.50 3.90 -1 -3 22 9.10 4.10 1 3 22 6.00 3.80 2 -3 22 181.08 13.50 -2 3 22 196.28 13.80 -2 -3 22 187.98 13.20 2 3 22 205.68 14.10 -3 3 22 12.80 4.40 3 -3 22 10.20 4.00 3 3 22 7.30 4.10 -3 -3 22 7.60 3.90 4 -3 22 157.98 12.10 -4 3 22 167.78 12.40 4 3 22 172.18 12.70 -4 -3 22 149.59 11.50 -5 3 22 1.60 3.30 5 -3 22 3.20 3.40 -5 -3 22 5.00 3.30 5 3 22 4.70 3.80 -6 3 22 121.39 10.50 -6 -3 -22 110.39 12.90 6 -3 22 118.39 10.70 6 3 22 130.49 11.00 -6 -3 22 131.59 10.40 0 4 22 0.90 3.20 0 -4 22 -1.60 2.90 -1 4 22 193.98 13.90 1 -4 22 187.78 13.20 -1 -4 22 197.98 13.30 1 4 22 179.38 13.60 -2 4 22 9.60 4.10 2 -4 22 11.40 4.10 -2 -4 22 9.10 3.70 2 4 22 4.20 3.50 3 -4 22 204.38 14.10 -3 4 22 190.18 13.80 -3 -4 22 194.78 13.50 3 4 22 184.38 13.60 -4 4 22 17.90 4.70 4 -4 22 20.60 5.20 -4 -4 22 12.20 3.90 4 4 22 12.80 4.70 5 -4 22 120.39 10.20 -5 4 22 105.89 10.00 5 4 22 109.19 10.20 -5 -4 22 111.29 9.40 -6 -4 -22 21.10 5.70 -6 4 22 12.50 4.60 6 -4 22 20.70 5.20 -6 -4 22 26.60 5.30 6 4 22 23.40 5.60 0 -5 22 124.19 10.50 0 5 22 141.99 11.30 -1 5 22 3.30 3.20 1 -5 22 5.90 3.80 -1 -5 22 1.30 3.30 1 5 22 2.90 3.40 -2 5 22 136.39 11.20 2 -5 22 134.99 11.00 2 5 22 129.09 11.10 -2 -5 22 116.19 10.10 -3 5 22 13.20 4.30 3 -5 22 17.00 4.60 3 5 22 6.60 4.10 -3 -5 22 8.60 3.90 4 -5 22 132.79 10.90 -4 5 22 124.59 10.60 4 5 22 111.39 10.40 -4 -5 22 105.69 9.40 -5 5 22 10.90 4.10 5 -5 22 12.50 4.50 -5 -5 22 4.50 3.40 5 5 22 6.70 4.20 0 6 22 0.10 3.40 0 -6 22 3.40 3.20 1 -6 22 141.99 11.70 -1 6 22 161.58 12.40 -1 -6 22 154.08 11.80 1 6 22 159.88 12.60 -2 6 22 0.00 2.80 2 -6 22 1.20 2.90 -2 -6 22 3.40 3.40 2 6 22 1.30 3.50 3 -6 22 125.99 10.70 -3 6 22 111.69 10.30 -3 -6 22 120.39 10.30 3 6 22 149.49 11.70 -4 6 22 14.80 4.60 4 -6 22 10.90 4.20 4 6 22 8.40 4.20 -4 -6 22 1.20 2.80 0 -7 22 84.59 8.50 0 7 22 69.99 9.10 -1 7 22 3.00 3.70 1 -7 22 2.70 3.10 -1 -7 22 8.10 4.00 1 7 22 6.50 4.20 2 -7 22 101.49 9.60 -2 7 22 96.99 9.50 2 7 22 110.59 10.50 -2 -7 22 101.29 9.30 -3 7 22 6.40 4.00 3 -7 22 10.90 4.10 3 7 22 5.00 3.90 -3 -7 22 8.30 3.80 4 -7 22 101.19 9.30 -4 7 22 89.89 9.20 -4 -7 22 92.59 8.90 4 7 22 106.89 10.30 0 -8 22 8.50 3.60 0 8 22 8.40 4.30 -1 8 22 64.69 8.80 1 -8 22 63.39 8.20 -1 -8 22 70.49 7.80 1 8 22 68.29 8.80 2 -8 22 -1.40 2.80 -2 8 22 1.50 3.30 2 8 22 3.20 3.70 -2 -8 22 2.00 3.10 0 0 23 0.30 3.30 -1 0 23 6.30 3.60 1 0 23 9.60 4.20 -2 0 23 -0.20 3.10 2 0 23 1.10 3.40 -3 0 23 3.70 3.50 3 0 23 -1.30 3.30 4 0 23 38.10 6.70 -4 0 23 39.10 6.30 0 1 23 -1.50 3.20 0 -1 23 2.50 3.60 -1 1 23 3.70 3.30 1 -1 23 1.30 3.60 1 1 23 2.20 3.60 -1 -1 23 4.50 3.40 2 -1 23 5.30 3.90 -2 1 23 10.20 4.10 -2 -1 23 3.00 3.20 2 1 23 7.00 3.90 3 -1 23 19.00 5.30 -3 1 23 17.30 5.00 -3 -1 23 20.40 4.80 3 1 23 30.50 6.10 -4 1 23 14.90 4.50 4 -1 23 8.60 4.00 -4 -1 23 15.30 4.70 4 1 23 17.90 5.10 0 2 23 6.60 4.00 0 -2 23 5.10 3.40 1 -2 23 9.20 4.30 -1 2 23 5.90 3.50 -1 -2 23 6.90 4.00 1 2 23 5.00 3.80 -2 2 23 2.50 3.40 2 -2 23 0.40 3.00 2 2 23 -0.40 2.70 -2 -2 23 -5.10 2.60 3 -2 23 6.10 4.00 -3 2 23 7.60 4.00 3 2 23 7.90 4.30 -3 -2 23 10.70 4.10 4 -2 23 33.10 6.20 -4 2 23 38.20 6.50 -4 -2 23 35.30 6.10 4 2 23 51.09 7.60 0 3 23 17.90 4.70 0 -3 23 15.20 4.60 1 -3 23 4.90 3.60 -1 3 23 9.90 4.00 -1 -3 23 11.80 4.00 1 3 23 11.40 4.40 2 -3 23 5.20 3.50 -2 3 23 7.90 4.20 2 3 23 8.30 4.40 -2 -3 23 6.80 3.80 -3 3 23 8.70 4.20 3 -3 23 10.70 4.50 3 3 23 5.70 3.70 -3 -3 23 8.90 3.70 4 -3 23 7.20 3.90 -4 3 23 7.40 3.80 -4 -3 23 11.80 4.30 4 3 23 7.40 4.10 0 -4 23 17.50 4.90 0 4 23 17.30 5.00 -1 4 23 32.90 6.40 1 -4 23 34.50 6.50 1 4 23 34.80 6.60 -1 -4 23 34.90 6.20 -2 4 23 9.00 3.90 2 -4 23 6.00 3.90 -2 -4 23 5.80 3.70 2 4 23 9.40 4.00 -3 4 23 11.50 4.20 3 -4 23 12.40 4.60 -3 -4 23 18.30 4.80 3 4 23 17.00 5.10 0 -5 23 25.70 5.40 0 5 23 33.00 6.10 1 -5 23 9.10 4.10 -1 5 23 10.90 4.60 1 5 23 6.20 3.60 -1 -5 23 8.10 3.70 2 -5 23 33.60 6.20 -2 5 23 26.30 5.80 2 5 23 38.40 6.80 -2 -5 23 34.50 6.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35934