data_mo_CHEM0372_a _publ_contact_author_name "Vivian Wing Wah Yam" _publ_contact_author_address "Department of Chemistry, The University of Hong Kong, Pokfulam Road, Hong Kong" _publ_contact_author_email "wwyam@hku.hk; chanmym@hku.hk" _publ_contact_author_fax "+(852) 2857-1586" _publ_contact_author_phone "+(852) 2859-2153" _publ_requested_journal "Journal of the American Chemical Society" _publ_section_title "Realization of Thermally Stimulated Delay Phosphorescence in Arylgold(III) Complexes and Efficient Gold(III) Based Blue-Emitting OLEDs" _publ_author_name "Vivian Wing-Wah Yam" _publ_author_address "Department of Chemistry, The University of Hong Kong, Pokfulam Road, Hong Kong" _publ_section_abstract "To address and overcome the difficulties associated with the increased reactivity and susceptibility of blue emitters to deactivation pathways arising from the high-lying triplet excited states, we have successfully demonstrated an innovative strategy of harvesting triplet emission via the thermally stimulated delayed phosphorescence mechanism, where thermal up-conversion of excitons from the lower-energy triplet excited states (T1) to higher-energy triplet excited states (T1') are observed to generate blue emission. The lower-lying T1 excited state could serve as a mediator to populate the emissive T1' state by up-conversion via reverse internal conversion, which could enhance the photoluminescence quantum yield by over 20-folds. Organic light-emitting devices with a respectable external quantum efficiency of up to 7.7 % and sky-blue emission with CIE coordinates of (0.17, 0.37) have been realized. The operational stability for the device based on complex 1 has also been explored and the device is found to show fairly respectable lifetime. This work opens up a new avenue to the design and synthesis of blue phosphorescent emitters." _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H50 Au N3' _chemical_formula_sum 'C43 H50 Au N3' _chemical_formula_weight 805.82 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 10.6434(14) _cell_length_b 11.5563(14) _cell_length_c 15.779(2) _cell_angle_alpha 101.439(3) _cell_angle_beta 98.369(4) _cell_angle_gamma 104.009(3) _cell_volume 1807.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 347 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 22.5 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_F_000 816 _exptl_transmission_factor_min 0.3699 _exptl_transmission_factor_max 0.4899 _exptl_crystal_size_max 0.371 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.027 _exptl_absorpt_coefficient_mu 4.104 _shelx_estimated_absorpt_T_min 0.311 _shelx_estimated_absorpt_T_max 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 149(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'I\mS HB micro-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 62245 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.014 _diffrn_reflns_theta_max 25.038 _diffrn_reflns_theta_full 25.038 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 6350 _reflns_number_gt 5685 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _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^)+(0.0132P)^2^+0.7273P] 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_number_reflns 6350 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0444 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Au1 Au 0.74169(2) 0.46105(2) 0.54837(2) 0.01576(5) Uani 1 1 d . . . . . C1 C 0.5613(3) 0.3484(2) 0.46950(19) 0.0177(7) Uani 1 1 d . . . . . N2 N 0.7424(2) 0.5249(2) 0.43845(15) 0.0169(6) Uani 1 1 d . . . . . C2 C 0.4688(3) 0.2478(2) 0.48175(19) 0.0186(7) Uani 1 1 d . . . . . H2 H 0.4859 0.2203 0.5340 0.022 Uiso 1 1 calc R U . . . N3 N 0.8528(2) 0.6525(2) 0.36034(15) 0.0172(5) Uani 1 1 d . . . . . C3 C 0.3517(3) 0.1861(3) 0.41967(19) 0.0187(7) Uani 1 1 d . . . . . C4 C 0.3254(3) 0.2278(3) 0.3439(2) 0.0222(7) Uani 1 1 d . . . . . H4 H 0.2445 0.1891 0.3024 0.027 Uiso 1 1 calc R U . . . N4 N 0.6343(2) 0.5183(2) 0.29770(15) 0.0181(6) Uani 1 1 d . . . . . C6 C 0.5334(3) 0.3833(2) 0.38924(19) 0.0171(6) Uani 1 1 d . . . . . C5 C 0.4167(3) 0.3257(3) 0.3286(2) 0.0221(7) Uani 1 1 d . . . . . H5 H 0.3989 0.3531 0.2763 0.027 Uiso 1 1 calc R U . . . C7 C 0.6372(3) 0.4795(3) 0.37193(19) 0.0163(6) Uani 1 1 d . . . . . C8 C 0.7446(3) 0.6028(3) 0.29457(19) 0.0156(6) Uani 1 1 d . . . . . C9 C 0.8481(3) 0.6111(2) 0.43250(19) 0.0167(7) Uani 1 1 d . . . . . C10 C 0.9219(3) 0.5988(2) 0.58455(19) 0.0172(6) Uani 1 1 d . . . . . C11 C 1.0130(3) 0.6475(3) 0.66456(19) 0.0183(7) Uani 1 1 d . . . . . H11 H 0.9958 0.6156 0.7141 0.022 Uiso 1 1 calc R U . . . C12 C 1.1295(3) 0.7424(2) 0.67425(19) 0.0180(7) Uani 1 1 d . . . . . C13 C 1.1572(3) 0.7838(3) 0.60029(19) 0.0212(7) Uani 1 1 d . . . . . H13 H 1.2386 0.8431 0.6046 0.025 Uiso 1 1 calc R U . . . C14 C 1.0681(3) 0.7398(3) 0.52066(19) 0.0195(7) Uani 1 1 d . . . . . H14 H 1.0871 0.7705 0.4710 0.023 Uiso 1 1 calc R U . . . C15 C 0.9509(3) 0.6509(2) 0.51337(18) 0.0155(6) Uani 1 1 d . . . . . C16 C 0.7396(3) 0.3948(2) 0.65765(19) 0.0158(6) Uani 1 1 d . . . . . C17 C 0.6265(3) 0.3682(3) 0.69193(19) 0.0183(7) Uani 1 1 d . . . . . H17 H 0.5488 0.3832 0.6640 0.022 Uiso 1 1 calc R U . . . C18 C 0.6227(3) 0.3206(3) 0.76536(19) 0.0192(7) Uani 1 1 d . . . . . H18 H 0.5429 0.3038 0.7867 0.023 Uiso 1 1 calc R U . . . C19 C 0.7335(3) 0.2969(3) 0.80867(19) 0.0190(7) Uani 1 1 d . . . . . C20 C 0.8481(3) 0.3252(3) 0.77498(19) 0.0211(7) Uani 1 1 d . . . . . H20 H 0.9261 0.3113 0.8035 0.025 Uiso 1 1 calc R U . . . C21 C 0.8519(3) 0.3730(3) 0.70132(19) 0.0189(7) Uani 1 1 d . . . . . H21 H 0.9319 0.3912 0.6803 0.023 Uiso 1 1 calc R U . . . C36 C 1.2170(3) 0.8022(3) 0.7661(2) 0.0242(7) Uani 1 1 d . . . . . C37 C 1.3440(4) 0.8960(4) 0.7630(3) 0.0604(13) Uani 1 1 d . . . . . H01V H 1.3938 0.8556 0.7251 0.091 Uiso 1 1 calc R U . . . H01W H 1.3979 0.9304 0.8228 0.091 Uiso 1 1 calc R U . . . H01X H 1.3216 0.9623 0.7392 0.091 Uiso 1 1 calc R U . . . C38 C 1.1374(4) 0.8650(4) 0.8228(2) 0.0501(11) Uani 1 1 d . . . . . H01Y H 1.1111 0.9274 0.7961 0.075 Uiso 1 1 calc R U . . . H01Z H 1.1914 0.9044 0.8821 0.075 Uiso 1 1 calc R U . . . H011 H 1.0582 0.8038 0.8270 0.075 Uiso 1 1 calc R U . . . C39 C 1.2571(4) 0.7066(3) 0.8093(2) 0.0377(9) Uani 1 1 d . . . . . H00J H 1.1777 0.6434 0.8107 0.057 Uiso 1 1 calc R U . . . H00L H 1.3065 0.7463 0.8698 0.057 Uiso 1 1 calc R U . . . H00M H 1.3129 0.6684 0.7753 0.057 Uiso 1 1 calc R U . . . C40 C 0.2591(3) 0.0694(3) 0.4335(2) 0.0203(7) Uani 1 1 d . . . . . C41 C 0.3231(3) -0.0350(3) 0.4124(2) 0.0332(8) Uani 1 1 d . . . . . H01M H 0.3339 -0.0478 0.3509 0.050 Uiso 1 1 calc R U . . . H01N H 0.2666 -0.1106 0.4210 0.050 Uiso 1 1 calc R U . . . H01O H 0.4099 -0.0134 0.4517 0.050 Uiso 1 1 calc R U . . . C42 C 0.2399(3) 0.0883(3) 0.5294(2) 0.0341(9) Uani 1 1 d . . . . . H01J H 0.2063 0.1599 0.5445 0.051 Uiso 1 1 calc R U . . . H01K H 0.3248 0.1019 0.5690 0.051 Uiso 1 1 calc R U . . . H01L H 0.1764 0.0150 0.5358 0.051 Uiso 1 1 calc R U . . . C43 C 0.1226(3) 0.0329(3) 0.3734(2) 0.0340(8) Uani 1 1 d . . . . . H01G H 0.1311 0.0120 0.3116 0.051 Uiso 1 1 calc R U . . . H01H H 0.0835 0.1018 0.3831 0.051 Uiso 1 1 calc R U . . . H01I H 0.0656 -0.0385 0.3870 0.051 Uiso 1 1 calc R U . . . C35 C 0.6379(3) 0.7793(3) -0.0686(2) 0.0272(8) Uani 1 1 d . . . . . H00N H 0.6406 0.8030 -0.1247 0.041 Uiso 1 1 calc R U . . . H00O H 0.6271 0.8471 -0.0246 0.041 Uiso 1 1 calc R U . . . H00S H 0.5633 0.7063 -0.0770 0.041 Uiso 1 1 calc R U . . . C34 C 0.8818(3) 0.8642(3) -0.0282(2) 0.0227(7) Uani 1 1 d . . . . . H01A H 0.8821 0.8829 -0.0862 0.034 Uiso 1 1 calc R U . . . H01B H 0.9656 0.8482 -0.0069 0.034 Uiso 1 1 calc R U . . . H01C H 0.8711 0.9344 0.0136 0.034 Uiso 1 1 calc R U . . . C33 C 0.7849(3) 0.6441(3) -0.1048(2) 0.0277(8) Uani 1 1 d . . . . . H00C H 0.7073 0.5728 -0.1165 0.041 Uiso 1 1 calc R U . . . H00E H 0.8642 0.6220 -0.0819 0.041 Uiso 1 1 calc R U . . . H00I H 0.7945 0.6696 -0.1597 0.041 Uiso 1 1 calc R U . . . C32 C 0.7671(3) 0.7505(3) -0.03639(19) 0.0195(7) Uani 1 1 d . . . . . C31 C 0.6642(3) 0.5726(3) 0.1335(2) 0.0230(7) Uani 1 1 d . . . . . H31 H 0.6006 0.4990 0.1333 0.028 Uiso 1 1 calc R U . . . C30 C 0.6724(3) 0.6076(3) 0.0556(2) 0.0232(7) Uani 1 1 d . . . . . H30 H 0.6151 0.5564 0.0025 0.028 Uiso 1 1 calc R U . . . C29 C 0.7623(3) 0.7159(2) 0.05212(19) 0.0165(6) Uani 1 1 d . . . . . C28 C 0.8440(3) 0.7875(3) 0.13157(19) 0.0204(7) Uani 1 1 d . . . . . H28 H 0.9057 0.8624 0.1319 0.025 Uiso 1 1 calc R U . . . C27 C 0.8377(3) 0.7525(3) 0.2102(2) 0.0221(7) Uani 1 1 d . . . . . H27 H 0.8955 0.8032 0.2633 0.027 Uiso 1 1 calc R U . . . C26 C 0.7476(3) 0.6436(3) 0.21252(19) 0.0161(6) Uani 1 1 d . . . . . C25 C 0.8456(3) 0.3269(3) 0.9656(2) 0.0341(9) Uani 1 1 d . . . . . H01D H 0.9304 0.3366 0.9465 0.051 Uiso 1 1 calc R U . . . H01E H 0.8482 0.2902 1.0165 0.051 Uiso 1 1 calc R U . . . H01F H 0.8294 0.4075 0.9822 0.051 Uiso 1 1 calc R U . . . C24 C 0.7569(4) 0.1150(3) 0.8660(2) 0.0384(9) Uani 1 1 d . . . . . H01S H 0.6848 0.0605 0.8184 0.058 Uiso 1 1 calc R U . . . H01T H 0.7595 0.0808 0.9181 0.058 Uiso 1 1 calc R U . . . H01U H 0.8412 0.1222 0.8465 0.058 Uiso 1 1 calc R U . . . C23 C 0.6035(3) 0.2280(3) 0.9213(2) 0.0356(9) Uani 1 1 d . . . . . H01P H 0.5879 0.3088 0.9384 0.053 Uiso 1 1 calc R U . . . H01Q H 0.6080 0.1915 0.9723 0.053 Uiso 1 1 calc R U . . . H01R H 0.5310 0.1743 0.8736 0.053 Uiso 1 1 calc R U . . . C22 C 0.7338(3) 0.2426(3) 0.8895(2) 0.0255(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01571(7) 0.01631(7) 0.01374(7) 0.00582(4) 0.00169(4) 0.00067(4) C1 0.0165(16) 0.0148(15) 0.0199(17) 0.0019(13) 0.0032(13) 0.0031(12) N2 0.0185(14) 0.0164(13) 0.0130(14) 0.0022(11) 0.0018(11) 0.0015(11) C2 0.0212(16) 0.0189(15) 0.0147(16) 0.0049(13) 0.0032(13) 0.0032(13) N3 0.0180(13) 0.0188(13) 0.0139(13) 0.0058(11) 0.0023(11) 0.0028(11) C3 0.0166(16) 0.0175(15) 0.0206(17) 0.0038(13) 0.0043(13) 0.0023(13) C4 0.0181(16) 0.0228(16) 0.0198(17) 0.0053(14) -0.0032(13) -0.0012(13) N4 0.0179(13) 0.0192(13) 0.0177(14) 0.0070(11) 0.0019(11) 0.0048(11) C6 0.0167(16) 0.0171(15) 0.0178(16) 0.0070(13) 0.0044(13) 0.0024(12) C5 0.0199(17) 0.0266(17) 0.0186(17) 0.0098(14) 0.0000(13) 0.0034(14) C7 0.0161(16) 0.0172(15) 0.0181(17) 0.0056(13) 0.0061(13) 0.0068(12) C8 0.0142(16) 0.0175(15) 0.0172(16) 0.0039(13) 0.0043(13) 0.0076(13) C9 0.0172(16) 0.0145(15) 0.0196(17) 0.0047(13) 0.0071(13) 0.0045(13) C10 0.0179(16) 0.0162(15) 0.0182(17) 0.0065(13) 0.0043(13) 0.0039(12) C11 0.0216(16) 0.0191(15) 0.0137(16) 0.0045(13) 0.0022(13) 0.0051(13) C12 0.0191(16) 0.0155(15) 0.0181(17) 0.0021(13) 0.0018(13) 0.0050(13) C13 0.0183(16) 0.0207(16) 0.0218(18) 0.0060(14) 0.0020(14) 0.0007(13) C14 0.0192(16) 0.0226(16) 0.0177(17) 0.0086(13) 0.0051(13) 0.0039(13) C15 0.0180(16) 0.0151(14) 0.0124(15) 0.0013(12) 0.0027(12) 0.0046(12) C16 0.0192(16) 0.0103(14) 0.0157(16) 0.0019(12) 0.0044(13) 0.0003(12) C17 0.0179(16) 0.0190(15) 0.0171(16) 0.0039(13) 0.0011(13) 0.0054(13) C18 0.0182(16) 0.0225(16) 0.0172(16) 0.0057(13) 0.0056(13) 0.0041(13) C19 0.0225(17) 0.0150(15) 0.0174(17) 0.0036(13) 0.0032(13) 0.0022(13) C20 0.0201(17) 0.0234(16) 0.0197(17) 0.0058(13) 0.0014(13) 0.0073(13) C21 0.0160(16) 0.0211(16) 0.0194(17) 0.0063(13) 0.0047(13) 0.0030(13) C36 0.0263(18) 0.0231(16) 0.0170(17) 0.0009(14) -0.0015(14) 0.0021(14) C37 0.050(3) 0.067(3) 0.031(2) 0.011(2) -0.0189(19) -0.029(2) C38 0.056(3) 0.053(2) 0.032(2) -0.0167(19) -0.0085(19) 0.031(2) C39 0.044(2) 0.041(2) 0.0220(19) -0.0004(16) -0.0072(16) 0.0163(18) C40 0.0183(16) 0.0160(15) 0.0233(18) 0.0045(13) 0.0036(13) -0.0005(13) C41 0.0313(19) 0.0199(17) 0.046(2) 0.0077(16) 0.0088(17) 0.0016(15) C42 0.042(2) 0.0235(18) 0.031(2) 0.0053(15) 0.0144(17) -0.0043(16) C43 0.0241(18) 0.0305(19) 0.041(2) 0.0112(16) 0.0042(16) -0.0049(15) C35 0.0250(18) 0.0341(19) 0.0258(19) 0.0169(15) 0.0036(15) 0.0072(15) C34 0.0256(18) 0.0231(16) 0.0195(17) 0.0106(14) 0.0053(14) 0.0025(14) C33 0.038(2) 0.0250(17) 0.0175(17) 0.0059(14) 0.0031(15) 0.0055(15) C32 0.0228(17) 0.0176(15) 0.0167(16) 0.0075(13) 0.0008(13) 0.0023(13) C31 0.0223(17) 0.0186(16) 0.0232(18) 0.0094(14) -0.0001(14) -0.0038(13) C30 0.0209(17) 0.0226(16) 0.0173(17) 0.0052(13) -0.0051(13) -0.0050(13) C29 0.0170(16) 0.0167(15) 0.0172(16) 0.0070(13) 0.0029(13) 0.0053(12) C28 0.0214(17) 0.0169(15) 0.0196(17) 0.0054(13) 0.0040(14) -0.0015(13) C27 0.0214(17) 0.0212(16) 0.0182(17) 0.0025(13) -0.0011(13) 0.0004(13) C26 0.0149(15) 0.0197(15) 0.0165(16) 0.0082(13) 0.0037(13) 0.0069(13) C25 0.036(2) 0.048(2) 0.0200(18) 0.0161(16) 0.0018(15) 0.0093(17) C24 0.057(2) 0.0327(19) 0.033(2) 0.0191(17) 0.0109(18) 0.0160(18) C23 0.038(2) 0.048(2) 0.0247(19) 0.0215(17) 0.0111(16) 0.0071(17) C22 0.0275(18) 0.0316(18) 0.0177(17) 0.0104(14) 0.0041(14) 0.0057(15) _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 Au1 N2 2.015(2) . ? Au1 C16 2.021(3) . ? Au1 C10 2.093(3) . ? Au1 C1 2.094(3) . ? C1 C2 1.395(4) . ? C1 C6 1.417(4) . ? N2 C7 1.337(4) . ? N2 C9 1.339(3) . ? C2 C3 1.399(4) . ? C2 H2 0.9500 . ? N3 C9 1.323(4) . ? N3 C8 1.352(4) . ? C3 C4 1.391(4) . ? C3 C40 1.542(4) . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? N4 C7 1.333(4) . ? N4 C8 1.347(3) . ? C6 C5 1.379(4) . ? C6 C7 1.464(4) . ? C5 H5 0.9500 . ? C8 C26 1.464(4) . ? C9 C15 1.467(4) . ? C10 C11 1.396(4) . ? C10 C15 1.414(4) . ? C11 C12 1.408(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 C36 1.531(4) . ? C13 C14 1.380(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C16 C17 1.383(4) . ? C16 C21 1.393(4) . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 C20 1.394(4) . ? C19 C22 1.529(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C36 C38 1.519(5) . ? C36 C39 1.520(4) . ? C36 C37 1.528(5) . ? C37 H01V 0.9800 . ? C37 H01W 0.9800 . ? C37 H01X 0.9800 . ? C38 H01Y 0.9800 . ? C38 H01Z 0.9800 . ? C38 H011 0.9800 . ? C39 H00J 0.9800 . ? C39 H00L 0.9800 . ? C39 H00M 0.9800 . ? C40 C43 1.527(4) . ? C40 C41 1.528(4) . ? C40 C42 1.536(4) . ? C41 H01M 0.9800 . ? C41 H01N 0.9800 . ? C41 H01O 0.9800 . ? C42 H01J 0.9800 . ? C42 H01K 0.9800 . ? C42 H01L 0.9800 . ? C43 H01G 0.9800 . ? C43 H01H 0.9800 . ? C43 H01I 0.9800 . ? C35 C32 1.531(4) . ? C35 H00N 0.9800 . ? C35 H00O 0.9800 . ? C35 H00S 0.9800 . ? C34 C32 1.531(4) . ? C34 H01A 0.9800 . ? C34 H01B 0.9800 . ? C34 H01C 0.9800 . ? C33 C32 1.536(4) . ? C33 H00C 0.9800 . ? C33 H00E 0.9800 . ? C33 H00I 0.9800 . ? C32 C29 1.532(4) . ? C31 C30 1.376(4) . ? C31 C26 1.391(4) . ? C31 H31 0.9500 . ? C30 C29 1.396(4) . ? C30 H30 0.9500 . ? C29 C28 1.391(4) . ? C28 C27 1.385(4) . ? C28 H28 0.9500 . ? C27 C26 1.397(4) . ? C27 H27 0.9500 . ? C25 C22 1.538(4) . ? C25 H01D 0.9800 . ? C25 H01E 0.9800 . ? C25 H01F 0.9800 . ? C24 C22 1.536(5) . ? C24 H01S 0.9800 . ? C24 H01T 0.9800 . ? C24 H01U 0.9800 . ? C23 C22 1.525(4) . ? C23 H01P 0.9800 . ? C23 H01Q 0.9800 . ? C23 H01R 0.9800 . ? 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 N2 Au1 C16 179.26(10) . . ? N2 Au1 C10 79.05(10) . . ? C16 Au1 C10 101.59(11) . . ? N2 Au1 C1 79.36(10) . . ? C16 Au1 C1 100.00(11) . . ? C10 Au1 C1 158.41(11) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 Au1 131.9(2) . . ? C6 C1 Au1 111.33(19) . . ? C7 N2 C9 120.8(2) . . ? C7 N2 Au1 119.30(18) . . ? C9 N2 Au1 119.88(19) . . ? C1 C2 C3 122.2(3) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C9 N3 C8 115.7(2) . . ? C4 C3 C2 118.9(3) . . ? C4 C3 C40 121.3(3) . . ? C2 C3 C40 119.6(3) . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C7 N4 C8 115.4(2) . . ? C5 C6 C1 121.6(3) . . ? C5 C6 C7 121.6(3) . . ? C1 C6 C7 116.7(3) . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? N4 C7 N2 121.2(2) . . ? N4 C7 C6 125.8(3) . . ? N2 C7 C6 113.0(2) . . ? N4 C8 N3 125.6(3) . . ? N4 C8 C26 117.0(2) . . ? N3 C8 C26 117.3(2) . . ? N3 C9 N2 121.2(3) . . ? N3 C9 C15 126.6(2) . . ? N2 C9 C15 112.2(2) . . ? C11 C10 C15 116.7(2) . . ? C11 C10 Au1 131.8(2) . . ? C15 C10 Au1 111.5(2) . . ? C10 C11 C12 122.1(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 118.5(3) . . ? C13 C12 C36 121.9(3) . . ? C11 C12 C36 119.5(3) . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 121.7(3) . . ? C14 C15 C9 121.2(3) . . ? C10 C15 C9 117.0(2) . . ? C17 C16 C21 117.1(3) . . ? C17 C16 Au1 121.5(2) . . ? C21 C16 Au1 121.4(2) . . ? C18 C17 C16 122.2(3) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 116.7(3) . . ? C18 C19 C22 123.2(3) . . ? C20 C19 C22 120.1(3) . . ? C21 C20 C19 122.1(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C16 120.7(3) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C38 C36 C39 108.4(3) . . ? C38 C36 C37 109.8(3) . . ? C39 C36 C37 107.4(3) . . ? C38 C36 C12 107.9(3) . . ? C39 C36 C12 111.2(2) . . ? C37 C36 C12 112.2(3) . . ? C36 C37 H01V 109.5 . . ? C36 C37 H01W 109.5 . . ? H01V C37 H01W 109.5 . . ? C36 C37 H01X 109.5 . . ? H01V C37 H01X 109.5 . . ? H01W C37 H01X 109.5 . . ? C36 C38 H01Y 109.5 . . ? C36 C38 H01Z 109.5 . . ? H01Y C38 H01Z 109.5 . . ? C36 C38 H011 109.5 . . ? H01Y C38 H011 109.5 . . ? H01Z C38 H011 109.5 . . ? C36 C39 H00J 109.5 . . ? C36 C39 H00L 109.5 . . ? H00J C39 H00L 109.5 . . ? C36 C39 H00M 109.5 . . ? H00J C39 H00M 109.5 . . ? H00L C39 H00M 109.5 . . ? C43 C40 C41 108.8(3) . . ? C43 C40 C42 107.7(3) . . ? C41 C40 C42 109.6(3) . . ? C43 C40 C3 112.3(3) . . ? C41 C40 C3 107.6(2) . . ? C42 C40 C3 110.8(2) . . ? C40 C41 H01M 109.5 . . ? C40 C41 H01N 109.5 . . ? H01M C41 H01N 109.5 . . ? C40 C41 H01O 109.5 . . ? H01M C41 H01O 109.5 . . ? H01N C41 H01O 109.5 . . ? C40 C42 H01J 109.5 . . ? C40 C42 H01K 109.5 . . ? H01J C42 H01K 109.5 . . ? C40 C42 H01L 109.5 . . ? H01J C42 H01L 109.5 . . ? H01K C42 H01L 109.5 . . ? C40 C43 H01G 109.5 . . ? C40 C43 H01H 109.5 . . ? H01G C43 H01H 109.5 . . ? C40 C43 H01I 109.5 . . ? H01G C43 H01I 109.5 . . ? H01H C43 H01I 109.5 . . ? C32 C35 H00N 109.5 . . ? C32 C35 H00O 109.5 . . ? H00N C35 H00O 109.5 . . ? C32 C35 H00S 109.5 . . ? H00N C35 H00S 109.5 . . ? H00O C35 H00S 109.5 . . ? C32 C34 H01A 109.5 . . ? C32 C34 H01B 109.5 . . ? H01A C34 H01B 109.5 . . ? C32 C34 H01C 109.5 . . ? H01A C34 H01C 109.5 . . ? H01B C34 H01C 109.5 . . ? C32 C33 H00C 109.5 . . ? C32 C33 H00E 109.5 . . ? H00C C33 H00E 109.5 . . ? C32 C33 H00I 109.5 . . ? H00C C33 H00I 109.5 . . ? H00E C33 H00I 109.5 . . ? C34 C32 C35 108.1(2) . . ? C34 C32 C29 111.9(2) . . ? C35 C32 C29 108.8(2) . . ? C34 C32 C33 107.8(2) . . ? C35 C32 C33 109.9(2) . . ? C29 C32 C33 110.2(2) . . ? C30 C31 C26 121.0(3) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C31 C30 C29 122.0(3) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C28 C29 C30 116.8(3) . . ? C28 C29 C32 123.4(2) . . ? C30 C29 C32 119.8(3) . . ? C27 C28 C29 121.7(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C27 C26 120.8(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C31 C26 C27 117.7(3) . . ? C31 C26 C8 121.1(3) . . ? C27 C26 C8 121.2(3) . . ? C22 C25 H01D 109.5 . . ? C22 C25 H01E 109.5 . . ? H01D C25 H01E 109.5 . . ? C22 C25 H01F 109.5 . . ? H01D C25 H01F 109.5 . . ? H01E C25 H01F 109.5 . . ? C22 C24 H01S 109.5 . . ? C22 C24 H01T 109.5 . . ? H01S C24 H01T 109.5 . . ? C22 C24 H01U 109.5 . . ? H01S C24 H01U 109.5 . . ? H01T C24 H01U 109.5 . . ? C22 C23 H01P 109.5 . . ? C22 C23 H01Q 109.5 . . ? H01P C23 H01Q 109.5 . . ? C22 C23 H01R 109.5 . . ? H01P C23 H01R 109.5 . . ? H01Q C23 H01R 109.5 . . ? C23 C22 C19 112.5(3) . . ? C23 C22 C24 108.0(3) . . ? C19 C22 C24 109.3(3) . . ? C23 C22 C25 108.3(3) . . ? C19 C22 C25 109.5(2) . . ? C24 C22 C25 109.3(3) . . ? _refine_diff_density_max 0.604 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.090 _shelx_res_file ; mo_CHEM0372_a.res created by SHELXL-2014/7 TITL 260\mo_CHEM0372_a.res in P-1 REM Old TITL mo_CHEM0372_0m in P-1 REM SHELXT solution in P-1 REM R1 0.064, Rweak 0.012, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C43 N3 Au CELL 0.71073 10.6434 11.5563 15.7795 101.439 98.369 104.009 ZERR 2.000 0.0014 0.0014 0.0021 0.003 0.004 0.003 LATT 1 SFAC C H N AU UNIT 86 100 6 2 TEMP -123.630 SIZE 0.027 0.063 0.371 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 20 ACTA WGHT 0.013200 0.727300 FVAR 0.23348 AU1 4 0.741690 0.461053 0.548371 11.00000 0.01571 0.01631 = 0.01374 0.00582 0.00169 0.00067 C1 1 0.561267 0.348351 0.469504 11.00000 0.01654 0.01476 = 0.01991 0.00191 0.00321 0.00307 N2 3 0.742409 0.524883 0.438451 11.00000 0.01850 0.01643 = 0.01303 0.00219 0.00181 0.00153 C2 1 0.468818 0.247797 0.481746 11.00000 0.02118 0.01885 = 0.01469 0.00488 0.00322 0.00317 AFIX 43 H2 2 0.485936 0.220255 0.533988 11.00000 -1.20000 AFIX 0 N3 3 0.852782 0.652527 0.360337 11.00000 0.01804 0.01881 = 0.01394 0.00580 0.00232 0.00283 C3 1 0.351729 0.186147 0.419666 11.00000 0.01662 0.01752 = 0.02056 0.00376 0.00431 0.00235 C4 1 0.325406 0.227827 0.343905 11.00000 0.01806 0.02284 = 0.01976 0.00525 -0.00319 -0.00120 AFIX 43 H4 2 0.244538 0.189098 0.302449 11.00000 -1.20000 AFIX 0 N4 3 0.634309 0.518294 0.297703 11.00000 0.01788 0.01921 = 0.01766 0.00703 0.00191 0.00477 C6 1 0.533383 0.383326 0.389236 11.00000 0.01666 0.01705 = 0.01777 0.00697 0.00438 0.00244 C5 1 0.416731 0.325742 0.328579 11.00000 0.01993 0.02663 = 0.01864 0.00975 -0.00002 0.00340 AFIX 43 H5 2 0.398858 0.353058 0.276320 11.00000 -1.20000 AFIX 0 C7 1 0.637179 0.479532 0.371927 11.00000 0.01608 0.01721 = 0.01812 0.00560 0.00607 0.00684 C8 1 0.744564 0.602848 0.294565 11.00000 0.01419 0.01748 = 0.01721 0.00390 0.00429 0.00765 C9 1 0.848136 0.611108 0.432499 11.00000 0.01723 0.01445 = 0.01964 0.00472 0.00708 0.00446 C10 1 0.921873 0.598832 0.584554 11.00000 0.01789 0.01617 = 0.01822 0.00650 0.00432 0.00392 C11 1 1.012961 0.647509 0.664557 11.00000 0.02163 0.01907 = 0.01373 0.00454 0.00221 0.00511 AFIX 43 H11 2 0.995804 0.615629 0.714066 11.00000 -1.20000 AFIX 0 C12 1 1.129501 0.742378 0.674248 11.00000 0.01907 0.01550 = 0.01808 0.00211 0.00176 0.00500 C13 1 1.157202 0.783757 0.600289 11.00000 0.01826 0.02075 = 0.02183 0.00602 0.00200 0.00067 AFIX 43 H13 2 1.238628 0.843100 0.604614 11.00000 -1.20000 AFIX 0 C14 1 1.068058 0.739830 0.520656 11.00000 0.01916 0.02256 = 0.01769 0.00860 0.00511 0.00386 AFIX 43 H14 2 1.087069 0.770499 0.470985 11.00000 -1.20000 AFIX 0 C15 1 0.950856 0.650948 0.513367 11.00000 0.01801 0.01510 = 0.01243 0.00127 0.00267 0.00458 C16 1 0.739619 0.394844 0.657650 11.00000 0.01917 0.01028 = 0.01565 0.00192 0.00442 0.00031 C17 1 0.626483 0.368232 0.691933 11.00000 0.01791 0.01902 = 0.01710 0.00393 0.00114 0.00540 AFIX 43 H17 2 0.548772 0.383240 0.663966 11.00000 -1.20000 AFIX 0 C18 1 0.622737 0.320640 0.765356 11.00000 0.01818 0.02245 = 0.01717 0.00567 0.00560 0.00408 AFIX 43 H18 2 0.542901 0.303775 0.786693 11.00000 -1.20000 AFIX 0 C19 1 0.733457 0.296921 0.808665 11.00000 0.02250 0.01504 = 0.01741 0.00363 0.00321 0.00221 C20 1 0.848073 0.325238 0.774977 11.00000 0.02005 0.02344 = 0.01974 0.00575 0.00143 0.00731 AFIX 43 H20 2 0.926078 0.311285 0.803483 11.00000 -1.20000 AFIX 0 C21 1 0.851864 0.373037 0.701319 11.00000 0.01603 0.02107 = 0.01937 0.00634 0.00472 0.00301 AFIX 43 H21 2 0.931881 0.391175 0.680308 11.00000 -1.20000 AFIX 0 C36 1 1.217014 0.802215 0.766130 11.00000 0.02633 0.02310 = 0.01696 0.00095 -0.00145 0.00212 C37 1 1.343969 0.896025 0.763031 11.00000 0.04988 0.06736 = 0.03053 0.01102 -0.01888 -0.02874 AFIX 137 H01V 2 1.393826 0.855583 0.725068 11.00000 -1.50000 H01W 2 1.397911 0.930376 0.822807 11.00000 -1.50000 H01X 2 1.321598 0.962285 0.739229 11.00000 -1.50000 AFIX 0 C38 1 1.137370 0.865033 0.822844 11.00000 0.05588 0.05350 = 0.03218 -0.01675 -0.00854 0.03141 AFIX 137 H01Y 2 1.111109 0.927412 0.796060 11.00000 -1.50000 H01Z 2 1.191447 0.904377 0.882104 11.00000 -1.50000 H011 2 1.058171 0.803837 0.826956 11.00000 -1.50000 AFIX 0 C39 1 1.257105 0.706578 0.809308 11.00000 0.04403 0.04139 = 0.02201 -0.00037 -0.00716 0.01633 AFIX 137 H00J 2 1.177725 0.643382 0.810669 11.00000 -1.50000 H00L 2 1.306517 0.746260 0.869756 11.00000 -1.50000 H00M 2 1.312923 0.668428 0.775339 11.00000 -1.50000 AFIX 0 C40 1 0.259100 0.069385 0.433536 11.00000 0.01835 0.01598 = 0.02330 0.00454 0.00361 -0.00053 C41 1 0.323134 -0.034985 0.412409 11.00000 0.03132 0.01993 = 0.04553 0.00768 0.00882 0.00162 AFIX 137 H01M 2 0.333939 -0.047849 0.350916 11.00000 -1.50000 H01N 2 0.266621 -0.110594 0.421041 11.00000 -1.50000 H01O 2 0.409907 -0.013448 0.451719 11.00000 -1.50000 AFIX 0 C42 1 0.239900 0.088257 0.529393 11.00000 0.04181 0.02354 = 0.03124 0.00533 0.01439 -0.00434 AFIX 137 H01J 2 0.206288 0.159906 0.544515 11.00000 -1.50000 H01K 2 0.324804 0.101878 0.569048 11.00000 -1.50000 H01L 2 0.176355 0.015030 0.535791 11.00000 -1.50000 AFIX 0 C43 1 0.122630 0.032894 0.373444 11.00000 0.02406 0.03055 = 0.04095 0.01120 0.00423 -0.00489 AFIX 137 H01G 2 0.131137 0.011987 0.311643 11.00000 -1.50000 H01H 2 0.083547 0.101768 0.383099 11.00000 -1.50000 H01I 2 0.065602 -0.038498 0.387014 11.00000 -1.50000 AFIX 0 C35 1 0.637865 0.779334 -0.068552 11.00000 0.02502 0.03407 = 0.02581 0.01695 0.00364 0.00717 AFIX 137 H00N 2 0.640566 0.802955 -0.124718 11.00000 -1.50000 H00O 2 0.627066 0.847148 -0.024554 11.00000 -1.50000 H00S 2 0.563270 0.706326 -0.076964 11.00000 -1.50000 AFIX 0 C34 1 0.881812 0.864238 -0.028246 11.00000 0.02561 0.02307 = 0.01953 0.01059 0.00525 0.00249 AFIX 137 H01A 2 0.882142 0.882888 -0.086163 11.00000 -1.50000 H01B 2 0.965601 0.848179 -0.006934 11.00000 -1.50000 H01C 2 0.871122 0.934416 0.013575 11.00000 -1.50000 AFIX 0 C33 1 0.784876 0.644087 -0.104826 11.00000 0.03813 0.02500 = 0.01755 0.00590 0.00309 0.00553 AFIX 137 H00C 2 0.707288 0.572817 -0.116525 11.00000 -1.50000 H00E 2 0.864151 0.621993 -0.081863 11.00000 -1.50000 H00I 2 0.794537 0.669552 -0.159738 11.00000 -1.50000 AFIX 0 C32 1 0.767088 0.750539 -0.036393 11.00000 0.02279 0.01760 = 0.01667 0.00747 0.00080 0.00231 C31 1 0.664168 0.572630 0.133502 11.00000 0.02227 0.01862 = 0.02323 0.00940 -0.00013 -0.00377 AFIX 43 H31 2 0.600578 0.498951 0.133320 11.00000 -1.20000 AFIX 0 C30 1 0.672380 0.607585 0.055583 11.00000 0.02087 0.02265 = 0.01734 0.00518 -0.00506 -0.00500 AFIX 43 H30 2 0.615100 0.556439 0.002533 11.00000 -1.20000 AFIX 0 C29 1 0.762307 0.715898 0.052125 11.00000 0.01705 0.01673 = 0.01723 0.00697 0.00292 0.00530 C28 1 0.843990 0.787495 0.131568 11.00000 0.02143 0.01694 = 0.01957 0.00535 0.00401 -0.00152 AFIX 43 H28 2 0.905705 0.862378 0.131883 11.00000 -1.20000 AFIX 0 C27 1 0.837733 0.752500 0.210243 11.00000 0.02139 0.02115 = 0.01816 0.00250 -0.00107 0.00041 AFIX 43 H27 2 0.895456 0.803212 0.263267 11.00000 -1.20000 AFIX 0 C26 1 0.747573 0.643555 0.212522 11.00000 0.01494 0.01970 = 0.01649 0.00822 0.00370 0.00695 C25 1 0.845602 0.326880 0.965565 11.00000 0.03560 0.04758 = 0.02003 0.01614 0.00180 0.00926 AFIX 137 H01D 2 0.930366 0.336622 0.946497 11.00000 -1.50000 H01E 2 0.848224 0.290229 1.016501 11.00000 -1.50000 H01F 2 0.829448 0.407515 0.982182 11.00000 -1.50000 AFIX 0 C24 1 0.756929 0.114967 0.865972 11.00000 0.05728 0.03268 = 0.03255 0.01908 0.01092 0.01601 AFIX 137 H01S 2 0.684810 0.060458 0.818382 11.00000 -1.50000 H01T 2 0.759532 0.080763 0.918071 11.00000 -1.50000 H01U 2 0.841196 0.122242 0.846462 11.00000 -1.50000 AFIX 0 C23 1 0.603546 0.227982 0.921316 11.00000 0.03848 0.04798 = 0.02467 0.02148 0.01106 0.00708 AFIX 137 H01P 2 0.587919 0.308765 0.938441 11.00000 -1.50000 H01Q 2 0.607978 0.191523 0.972315 11.00000 -1.50000 H01R 2 0.531041 0.174285 0.873649 11.00000 -1.50000 AFIX 0 C22 1 0.733816 0.242570 0.889478 11.00000 0.02747 0.03161 = 0.01767 0.01040 0.00410 0.00568 REM ##### HKLF 4 REM 260\mo_CHEM0372_a.res in P-1 REM R1 = 0.0215 for 5685 Fo > 4sig(Fo) and 0.0298 for all 6350 data REM 436 parameters refined using 0 restraints END WGHT 0.0132 0.7273 REM Highest difference peak 0.604, deepest hole -1.035, 1-sigma level 0.090 Q1 1 0.6556 0.4085 0.5480 11.00000 0.05 0.60 Q2 1 0.6714 0.4661 0.5917 11.00000 0.05 0.49 Q3 1 0.6090 0.4747 0.5523 11.00000 0.05 0.46 Q4 1 0.8745 0.4566 0.5509 11.00000 0.05 0.45 Q5 1 0.7771 0.5766 0.6263 11.00000 0.05 0.45 Q6 1 0.8260 0.5045 0.5453 11.00000 0.05 0.43 Q7 1 0.8411 0.3902 0.5589 11.00000 0.05 0.43 Q8 1 0.8163 0.4631 0.4971 11.00000 0.05 0.42 Q9 1 0.5599 0.4540 0.3945 11.00000 0.05 0.42 Q10 1 0.7090 0.5358 0.5956 11.00000 0.05 0.39 Q11 1 0.8533 0.4487 0.6115 11.00000 0.05 0.39 Q12 1 0.6399 0.3397 0.4831 11.00000 0.05 0.37 Q13 1 0.2406 0.0610 0.4735 11.00000 0.05 0.36 Q14 1 0.7275 0.3521 0.4680 11.00000 0.05 0.35 Q15 1 0.8106 0.7003 0.2125 11.00000 0.05 0.35 Q16 1 0.9030 0.6034 0.4828 11.00000 0.05 0.35 Q17 1 0.9833 0.7828 0.3745 11.00000 0.05 0.35 Q18 1 0.7802 0.6174 0.3557 11.00000 0.05 0.35 Q19 1 0.6814 0.2408 0.9063 11.00000 0.05 0.35 Q20 1 0.9329 0.7294 0.3429 11.00000 0.05 0.34 ; _shelx_res_checksum 41113 _shelx_hkl_file ; 1 0 0 -1.50 3.10 1 0 0 0.30 0.60 1 0 0 0.00 0.70 -2 0 0 3729.73 247.28 -2 0 0 3859.71 247.48 -2 0 0 4402.06 249.28 -2 0 0 3862.81 247.68 2 0 0 3965.50 247.18 2 0 0 3817.32 247.68 2 0 0 3835.02 247.18 2 0 0 4321.77 249.18 2 0 0 3561.74 247.18 2 0 0 4442.96 249.97 2 0 0 3925.11 247.48 -3 0 0 4.90 3.00 -3 0 0 5.60 1.50 -3 0 0 4.60 2.40 -3 0 0 12.70 6.40 -3 0 0 6.50 2.00 3 0 0 5.60 1.70 3 0 0 9.00 7.20 3 0 0 3.20 1.60 3 0 0 6.50 2.40 3 0 0 4.30 1.80 3 0 0 13.30 6.70 3 0 0 5.10 2.40 -4 0 0 377.26 25.20 -4 0 0 367.86 23.90 -4 0 0 350.46 28.70 -4 0 0 363.26 24.60 -4 0 0 372.16 23.70 4 0 0 364.36 23.80 4 0 0 364.96 24.80 4 0 0 390.76 24.00 4 0 0 351.86 30.40 4 0 0 359.16 29.10 4 0 0 374.86 24.60 4 0 0 346.17 23.80 -5 0 0 30.10 12.20 -5 0 0 45.80 6.50 -5 0 0 51.79 5.40 -5 0 0 62.79 7.40 -5 0 0 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58.29 7.30 -5 3 0 65.19 18.70 -5 3 0 79.99 14.70 -5 3 0 55.49 5.90 4 -3 0 179.98 21.70 4 -3 0 181.38 12.40 4 -3 0 175.08 12.80 4 -3 0 196.58 13.30 4 -3 0 200.58 13.70 4 -3 0 181.78 12.80 4 -3 0 180.48 21.50 4 -3 0 183.68 12.50 -4 3 0 171.58 13.70 -4 3 0 178.58 22.60 -4 3 0 177.38 20.80 -4 3 0 173.88 12.80 -4 3 0 162.28 13.50 -4 3 0 173.48 12.60 3 -3 0 81.49 7.20 3 -3 0 82.19 13.50 3 -3 0 81.29 6.30 3 -3 0 70.19 5.60 3 -3 0 74.59 6.30 3 -3 0 70.89 13.00 -3 3 0 79.59 7.50 -3 3 0 83.89 14.40 -3 3 0 72.49 6.30 -3 3 0 81.19 11.80 -3 3 0 72.19 6.10 -3 3 0 74.09 6.80 2 -3 0 1414.16 90.09 2 -3 0 1476.55 86.79 2 -3 0 1384.76 85.89 2 -3 0 1261.67 86.39 2 -3 0 1407.66 90.29 2 -3 0 1379.86 86.49 2 -3 0 1491.75 87.49 -2 3 0 1306.67 86.39 -2 3 0 1368.16 87.29 -2 3 0 1312.17 85.89 -2 3 0 1518.85 90.89 -2 3 0 1298.07 86.69 -2 3 0 1281.37 86.39 -2 3 0 1459.55 89.89 1 -3 0 60.99 4.70 1 -3 0 56.29 3.80 1 -3 0 43.00 4.20 1 -3 0 58.49 8.50 1 -3 0 49.90 4.30 1 -3 0 58.79 5.30 -1 3 0 44.70 4.10 -1 3 0 62.29 9.10 -1 3 0 61.49 6.00 -1 3 0 46.40 4.30 -1 3 0 55.79 8.30 -1 3 0 61.39 4.70 0 -3 0 86.29 8.60 0 -3 0 98.19 7.20 0 -3 0 77.69 5.60 0 -3 0 78.69 6.00 0 -3 0 89.59 8.50 0 -3 0 78.89 5.70 0 3 0 70.49 8.50 0 3 0 84.19 5.80 0 3 0 83.79 6.00 0 3 0 67.99 8.40 0 3 0 87.29 7.30 0 3 0 82.69 5.70 -1 -3 0 437.96 28.70 -1 -3 0 442.96 29.10 -1 -3 0 482.85 29.10 -1 -3 0 411.96 27.80 -1 -3 0 454.15 29.10 -1 -3 0 441.26 27.90 1 3 0 452.95 28.70 1 3 0 466.95 29.20 1 3 0 418.46 27.90 1 3 0 463.75 28.40 1 3 0 412.06 29.40 1 3 0 444.96 29.20 1 3 0 436.66 27.90 1 3 0 453.15 28.70 -2 -3 0 180.48 11.30 -2 -3 0 166.78 12.70 -2 -3 0 190.78 12.70 -2 -3 0 176.88 13.00 -2 -3 0 187.98 13.50 2 3 0 162.78 13.00 2 3 0 181.88 12.70 2 3 0 175.58 11.30 2 3 0 172.08 11.20 2 3 0 186.68 12.80 2 3 0 177.28 12.50 2 3 0 158.88 12.40 -3 -3 0 692.63 43.70 -3 -3 0 652.03 42.20 -3 -3 0 652.93 43.60 -3 -3 0 730.93 44.80 -3 -3 0 660.53 44.40 -3 -3 0 712.03 42.10 3 3 0 693.23 43.40 3 3 0 622.44 43.40 3 3 0 659.23 43.90 3 3 0 662.13 43.50 3 3 0 658.33 42.10 3 3 0 616.34 42.10 3 3 0 716.83 43.20 3 3 0 672.63 45.10 -4 -3 0 278.87 19.40 -4 -3 0 322.57 21.60 -4 -3 0 312.37 24.20 -4 -3 0 335.27 19.30 -4 -3 0 289.77 23.80 -4 -3 0 303.27 21.40 4 3 0 293.57 20.60 4 3 0 289.57 25.20 4 3 0 326.27 20.40 4 3 0 317.07 23.10 4 3 0 292.17 19.20 4 3 0 279.17 19.40 4 3 0 292.37 20.80 4 3 0 280.17 21.00 -5 -3 0 299.17 26.60 -5 -3 0 357.96 20.20 -5 -3 0 297.87 20.40 -5 -3 0 311.77 27.10 -5 -3 0 345.37 23.10 -5 -3 0 284.47 22.40 5 3 0 331.67 21.00 5 3 0 293.27 22.20 5 3 0 297.87 21.50 5 3 0 324.17 26.80 5 3 0 285.17 28.70 5 3 0 300.17 22.10 5 3 0 306.17 20.10 5 3 0 287.87 20.20 -6 -3 0 122.39 19.60 -6 -3 0 125.79 8.20 -6 -3 0 108.19 10.70 -6 -3 0 100.19 16.80 -6 -3 0 109.59 8.90 -6 -3 0 112.79 13.30 6 3 0 108.59 11.40 6 3 0 112.59 8.20 6 3 0 104.99 10.00 6 3 0 120.69 9.10 6 3 0 111.09 16.40 6 3 0 98.69 10.10 6 3 0 141.89 21.20 6 3 0 99.89 8.50 -7 -3 0 51.19 7.00 -7 -3 0 71.19 19.30 -7 -3 0 54.59 16.70 -7 -3 0 74.99 10.80 -7 -3 0 66.79 8.40 -7 -3 0 69.29 5.70 7 3 0 61.79 6.00 7 3 0 68.49 17.10 7 3 0 44.20 21.90 7 3 0 53.59 9.20 7 3 0 68.99 6.40 7 3 0 55.59 6.00 7 3 0 52.39 8.60 7 3 0 48.40 7.90 -8 -3 0 98.09 14.70 -8 -3 0 108.79 10.60 -8 -3 0 130.59 24.20 -8 -3 0 127.99 26.90 8 3 0 95.39 8.70 8 3 0 112.59 9.00 8 3 0 101.19 8.80 8 3 0 102.39 15.00 8 3 0 121.89 29.40 -9 -3 0 191.38 31.80 -9 -3 0 169.68 34.60 -9 -3 0 219.38 22.60 9 3 0 196.78 19.50 9 3 0 222.58 22.50 9 3 0 221.68 15.90 9 3 0 216.58 15.80 9 3 0 234.78 40.40 -10 -3 0 3.60 12.00 -10 -3 0 -55.99 31.80 10 3 0 15.60 5.60 10 3 0 20.20 9.30 12 -4 0 132.99 93.49 12 -4 0 129.79 15.00 12 -4 0 90.09 14.30 -12 4 0 75.89 14.50 -12 4 0 10.30 54.69 11 -4 0 1.20 6.90 11 -4 0 26.90 53.59 11 -4 0 10.50 8.70 11 -4 0 12.70 9.30 11 -4 0 63.49 56.69 11 -4 0 14.40 11.20 -11 4 0 8.50 7.00 -11 4 0 5.00 8.60 -11 4 0 3.30 9.10 -11 4 0 33.00 55.49 -11 4 0 -57.09 42.60 10 -4 0 110.99 12.70 10 -4 0 129.99 13.90 10 -4 0 114.19 15.30 10 -4 0 169.98 44.70 10 -4 0 96.69 45.00 10 -4 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33.70 -2 -4 0 477.75 29.80 -2 -4 0 490.95 31.40 -2 -4 0 472.95 31.30 -2 -4 0 484.25 31.20 -2 -4 0 418.36 29.70 2 4 0 472.95 31.20 2 4 0 466.15 29.80 2 4 0 459.35 31.30 2 4 0 497.65 29.80 2 4 0 465.75 31.60 2 4 0 528.15 31.90 2 4 0 445.56 31.00 2 4 0 490.85 31.50 -3 -4 0 879.91 55.49 -3 -4 0 839.82 53.29 -3 -4 0 905.61 55.09 -3 -4 0 864.71 55.19 -3 -4 0 821.82 55.09 3 4 0 784.82 54.69 3 4 0 907.41 55.19 3 4 0 910.11 54.89 3 4 0 811.42 53.19 3 4 0 846.62 54.99 3 4 0 795.02 53.29 3 4 0 911.01 55.89 3 4 0 798.32 55.59 -4 -4 0 175.98 12.20 -4 -4 0 194.48 12.10 -4 -4 0 191.58 14.70 -4 -4 0 169.28 14.40 -4 -4 0 201.88 17.60 -4 -4 0 197.88 17.50 4 4 0 162.18 18.70 4 4 0 173.78 12.10 4 4 0 190.18 12.00 4 4 0 203.88 16.30 4 4 0 177.98 14.30 4 4 0 169.28 14.50 4 4 0 185.38 14.20 4 4 0 194.88 13.90 -5 -4 0 832.32 51.99 -5 -4 0 759.92 49.40 -5 -4 0 765.02 51.69 -5 -4 0 766.32 53.79 -5 -4 0 845.82 54.39 -5 -4 0 865.51 49.30 5 4 0 764.82 51.09 5 4 0 690.63 51.29 5 4 0 753.32 55.19 5 4 0 804.82 52.89 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332.77 45.40 8 -5 0 314.87 22.20 -8 5 0 316.17 47.10 -8 5 0 350.06 43.30 -8 5 0 290.77 22.20 -8 5 0 287.87 24.70 -8 5 0 268.07 22.90 7 -5 0 255.07 18.60 7 -5 0 301.67 20.80 7 -5 0 248.58 19.50 7 -5 0 268.77 38.60 7 -5 0 240.58 19.00 7 -5 0 272.07 36.10 7 -5 0 297.67 20.70 7 -5 0 266.47 18.80 -7 5 0 240.78 20.90 -7 5 0 256.07 41.50 -7 5 0 237.38 19.00 -7 5 0 257.77 19.70 -7 5 0 287.87 34.00 6 -5 0 318.67 36.50 6 -5 0 369.46 25.00 6 -5 0 363.26 22.90 6 -5 0 347.97 39.20 6 -5 0 339.47 22.70 6 -5 0 325.27 23.40 6 -5 0 360.56 23.70 6 -5 0 373.26 24.60 -6 5 0 292.77 24.00 -6 5 0 374.36 35.10 -6 5 0 325.97 23.50 -6 5 0 316.97 25.10 -6 5 0 351.46 41.30 -6 5 0 316.87 23.10 5 -5 0 527.65 45.60 5 -5 0 486.35 45.80 5 -5 0 520.75 33.30 5 -5 0 462.05 33.00 5 -5 0 514.35 32.40 5 -5 0 530.55 32.30 5 -5 0 531.45 34.00 -5 5 0 464.75 33.90 -5 5 0 499.55 33.30 -5 5 0 551.64 48.20 -5 5 0 486.25 33.00 -5 5 0 494.75 34.70 -5 5 0 476.15 43.40 4 -5 0 507.55 31.90 4 -5 0 565.74 33.60 4 -5 0 526.35 42.40 4 -5 0 550.34 34.50 4 -5 0 504.85 33.00 4 -5 0 521.65 42.50 -4 5 0 485.05 34.50 -4 5 0 473.45 33.30 -4 5 0 456.15 32.70 -4 5 0 456.85 40.80 -4 5 0 547.95 43.80 -4 5 0 465.15 32.90 3 -5 0 473.45 28.90 3 -5 0 467.85 36.50 3 -5 0 502.25 30.10 3 -5 0 392.86 28.30 3 -5 0 430.46 28.50 3 -5 0 426.86 27.30 3 -5 0 469.35 27.30 3 -5 0 446.86 36.50 -3 5 0 402.56 29.80 -3 5 0 406.06 28.40 -3 5 0 418.26 28.50 -3 5 0 386.16 34.80 -3 5 0 426.26 37.80 2 -5 0 147.99 9.90 2 -5 0 115.59 9.20 2 -5 0 145.19 11.40 2 -5 0 127.29 9.30 2 -5 0 128.99 8.40 2 -5 0 122.09 16.60 -2 5 0 124.49 9.40 -2 5 0 136.39 8.30 -2 5 0 115.59 16.50 -2 5 0 120.39 10.90 -2 5 0 116.39 9.30 -2 5 0 122.39 9.80 -2 5 0 117.69 17.80 1 -5 0 459.95 30.00 1 -5 0 450.05 34.70 1 -5 0 530.05 32.00 1 -5 0 448.86 30.20 1 -5 0 480.65 34.50 1 -5 0 459.05 29.90 1 -5 0 495.85 30.20 -1 5 0 488.25 30.30 -1 5 0 449.16 31.70 -1 5 0 425.96 29.90 -1 5 0 447.26 30.00 -1 5 0 468.05 35.90 -1 5 0 487.75 29.70 -1 5 0 456.55 34.60 0 -5 0 33.80 7.80 0 -5 0 37.60 4.50 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247.98 50.39 9 -6 0 226.78 19.00 9 -6 0 243.98 18.70 9 -6 0 255.97 19.10 -9 6 0 224.08 21.90 -9 6 0 226.68 18.60 -9 6 0 198.48 19.30 -9 6 0 216.08 19.40 -9 6 0 267.37 49.80 8 -6 0 139.69 13.50 8 -6 0 106.99 13.20 8 -6 0 130.89 13.80 8 -6 0 108.89 10.70 8 -6 0 123.29 11.20 8 -6 0 72.59 33.90 8 -6 0 101.79 11.70 8 -6 0 123.79 37.70 -8 6 0 122.59 11.90 -8 6 0 92.39 11.90 -8 6 0 106.49 14.20 -8 6 0 82.59 39.80 -8 6 0 96.79 12.00 -8 6 0 58.49 31.20 7 -6 0 253.67 20.20 7 -6 0 289.57 19.60 7 -6 0 286.87 19.20 7 -6 0 295.17 21.80 7 -6 0 263.77 42.00 7 -6 0 271.87 41.40 7 -6 0 283.57 20.80 7 -6 0 305.67 22.30 -7 6 0 323.97 44.80 -7 6 0 259.17 21.10 -7 6 0 274.07 20.10 -7 6 0 268.67 38.50 -7 6 0 268.07 20.80 -7 6 0 238.08 22.30 6 -6 0 49.99 6.40 6 -6 0 32.00 24.80 6 -6 0 48.90 5.40 6 -6 0 55.89 5.70 6 -6 0 53.49 8.50 6 -6 0 51.39 6.60 6 -6 0 45.90 7.50 6 -6 0 26.00 24.60 -6 6 0 38.60 6.80 -6 6 0 39.30 7.90 -6 6 0 33.30 21.90 -6 6 0 39.90 25.60 -6 6 0 41.60 9.10 -6 6 0 38.30 6.40 5 -6 0 620.24 51.59 5 -6 0 643.34 39.90 5 -6 0 588.24 39.30 5 -6 0 608.44 38.00 5 -6 0 646.74 37.90 5 -6 0 629.44 53.29 5 -6 0 658.83 41.00 5 -6 0 553.14 39.00 -5 6 0 605.94 50.49 -5 6 0 573.04 39.30 -5 6 0 536.15 39.90 -5 6 0 542.55 54.29 -5 6 0 560.84 41.20 -5 6 0 593.64 39.20 4 -6 0 13.60 1.60 4 -6 0 41.10 17.20 4 -6 0 18.10 4.20 4 -6 0 11.60 3.30 4 -6 0 15.80 5.30 4 -6 0 25.00 17.20 4 -6 0 18.80 3.70 -4 6 0 9.40 4.90 -4 6 0 16.20 3.80 -4 6 0 -8.30 17.30 -4 6 0 15.00 14.70 -4 6 0 12.30 4.50 -4 6 0 14.70 3.70 3 -6 0 596.34 48.20 3 -6 0 630.04 40.00 3 -6 0 674.03 42.10 3 -6 0 702.83 40.50 -3 6 0 584.74 41.80 -3 6 0 571.94 39.90 -3 6 0 580.34 40.30 -3 6 0 625.24 49.80 -3 6 0 592.84 39.90 2 -6 0 19.20 2.40 2 -6 0 28.60 3.60 2 -6 0 15.40 11.60 2 -6 0 14.10 2.90 2 -6 0 26.10 11.50 -2 6 0 18.30 4.70 -2 6 0 17.40 3.30 -2 6 0 16.20 14.00 -2 6 0 21.10 3.90 -2 6 0 14.30 3.00 -2 6 0 22.50 11.90 1 -6 0 865.11 55.49 1 -6 0 843.12 55.59 1 -6 0 858.31 60.59 1 -6 0 850.51 55.39 1 -6 0 874.81 55.89 1 -6 0 914.01 60.59 1 -6 0 1018.90 57.99 -1 6 0 842.92 57.79 -1 6 0 897.41 55.39 -1 6 0 872.81 61.69 -1 6 0 885.51 60.39 -1 6 0 860.11 55.59 -1 6 0 820.72 55.49 -1 6 0 900.51 55.99 0 -6 0 10.80 8.30 0 -6 0 0.10 1.50 0 -6 0 0.90 2.40 0 -6 0 -3.10 6.60 0 -6 0 0.90 2.70 0 -6 0 2.10 3.10 0 -6 0 4.00 1.60 0 6 0 2.60 1.80 0 6 0 2.50 4.20 0 6 0 3.50 2.20 0 6 0 -1.00 2.30 0 6 0 17.80 9.70 0 6 0 -0.40 1.60 0 6 0 4.90 8.10 -1 -6 0 866.21 53.79 -1 -6 0 829.12 56.79 -1 -6 0 965.40 56.59 -1 -6 0 837.92 55.19 -1 -6 0 905.61 56.59 -1 -6 0 854.31 53.89 1 6 0 793.52 54.69 1 6 0 839.02 56.49 1 6 0 918.41 57.49 1 6 0 865.71 55.19 1 6 0 867.81 55.09 1 6 0 777.72 53.99 1 6 0 874.71 57.59 1 6 0 859.11 53.99 -2 -6 0 1.00 1.20 -2 -6 0 3.50 1.00 -2 -6 0 3.70 6.30 -2 -6 0 -2.70 3.20 -2 -6 0 4.60 5.20 2 6 0 3.90 4.20 2 6 0 5.40 6.20 2 6 0 -0.90 6.60 2 6 0 1.70 1.20 2 6 0 0.70 4.50 2 6 0 4.50 3.10 2 6 0 -0.60 3.30 2 6 0 0.80 1.30 -3 -6 0 591.94 37.20 -3 -6 0 549.65 37.80 -3 -6 0 561.24 37.10 3 6 0 575.24 38.30 3 6 0 530.65 35.20 3 6 0 590.14 36.70 3 6 0 576.44 37.30 3 6 0 575.04 37.50 3 6 0 589.04 38.50 3 6 0 526.75 35.30 3 6 0 522.45 37.40 -4 -6 0 83.79 9.10 -4 -6 0 90.19 10.80 -4 -6 0 89.59 9.30 4 6 0 79.09 9.60 4 6 0 90.59 10.80 4 6 0 91.29 10.50 4 6 0 86.09 9.30 4 6 0 81.99 5.90 4 6 0 95.79 10.20 4 6 0 71.79 9.50 4 6 0 80.59 5.90 -5 -6 0 176.28 15.20 -5 -6 0 164.38 16.20 5 6 0 155.78 16.20 5 6 0 133.49 16.30 5 6 0 168.08 10.50 5 6 0 171.98 15.10 5 6 0 136.89 10.90 5 6 0 168.38 14.60 5 6 0 139.59 14.80 -6 -6 0 17.80 10.90 -6 -6 0 34.40 3.00 -6 -6 0 26.60 8.40 -6 -6 0 20.70 11.80 -6 -6 0 23.30 2.70 -6 -6 0 13.50 8.20 6 6 0 29.50 13.30 6 6 0 29.50 3.70 6 6 0 25.10 7.20 6 6 0 6.00 10.20 6 6 0 29.90 3.70 6 6 0 29.90 8.40 6 6 0 26.30 6.70 -7 -6 0 331.47 30.40 -7 -6 0 215.28 31.80 -7 -6 0 262.77 29.40 -7 -6 0 295.17 18.90 7 6 0 295.47 19.40 7 6 0 301.17 28.30 7 6 0 260.77 24.20 7 6 0 309.67 19.20 7 6 0 316.47 23.00 7 6 0 260.87 28.20 7 6 0 294.87 24.50 -8 -6 0 34.70 18.30 -8 -6 0 21.00 20.00 -8 -6 0 12.00 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